# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1 _database_code_depnum_ccdc_archive 'CCDC 895612' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(MedoenH)]ClO4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H17 Cl N4 Ni O6' _chemical_formula_weight 383.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.3309(2) _cell_length_b 16.9368(5) _cell_length_c 12.1796(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.4410(10) _cell_angle_gamma 90.00 _cell_volume 1505.43(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9441 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 39.79 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6701 _exptl_absorpt_correction_T_max 0.7534 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2001)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 77236 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 45.38 _reflns_number_total 12451 _reflns_number_gt 9137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054 (Bruker, 2007)' _computing_cell_refinement 'SAINT V7.68A (Bruker, 2007)' _computing_data_reduction 'SAINT V7.68A (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.8549P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12451 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.426001(16) 0.092430(7) 0.909106(10) 0.01047(3) Uani 1 1 d . . . Cl1 Cl 0.86044(3) 0.198561(13) 0.480761(19) 0.01296(4) Uani 1 1 d . . . N1 N 0.21203(10) 0.04579(5) 0.85078(7) 0.01155(11) Uani 1 1 d . . . N2 N 0.47155(11) 0.10700(5) 0.76639(7) 0.01290(12) Uani 1 1 d . . . C1 C 0.18868(12) 0.04415(6) 0.74214(8) 0.01250(13) Uani 1 1 d . . . C2 C 0.34464(13) 0.08161(6) 0.69338(8) 0.01297(14) Uani 1 1 d . . . N3 N 0.40570(11) 0.08627(5) 1.05979(7) 0.01178(11) Uani 1 1 d . . . N4 N 0.64985(11) 0.13659(5) 0.95158(7) 0.01274(12) Uani 1 1 d . . . C3 C 0.53708(13) 0.11930(6) 1.12234(8) 0.01296(13) Uani 1 1 d . . . C4 C 0.68757(12) 0.14707(6) 1.05598(8) 0.01330(14) Uani 1 1 d . . . C5 C 0.02499(14) 0.00877(6) 0.67763(9) 0.01580(15) Uani 1 1 d . . . H5A H -0.0633 -0.0085 0.7283 0.024 Uiso 1 1 calc R . . H5B H 0.0633 -0.0367 0.6357 0.024 Uiso 1 1 calc R . . H5C H -0.0323 0.0483 0.6267 0.024 Uiso 1 1 calc R . . C6 C 0.34695(15) 0.08739(7) 0.57139(9) 0.01886(17) Uani 1 1 d . . . H6A H 0.4667 0.1069 0.5539 0.028 Uiso 1 1 calc R . . H6B H 0.2510 0.1239 0.5417 0.028 Uiso 1 1 calc R . . H6C H 0.3247 0.0351 0.5383 0.028 Uiso 1 1 calc R . . C7 C 0.53772(17) 0.13072(7) 1.24299(9) 0.02024(18) Uani 1 1 d . . . H7A H 0.4265 0.1075 1.2682 0.030 Uiso 1 1 calc R . . H7B H 0.5414 0.1873 1.2599 0.030 Uiso 1 1 calc R . . H7C H 0.6457 0.1049 1.2807 0.030 Uiso 1 1 calc R . . C8 C 0.85904(15) 0.18207(7) 1.11071(10) 0.01960(18) Uani 1 1 d . . . H8A H 0.9344 0.2022 1.0545 0.029 Uiso 1 1 calc R . . H8B H 0.9275 0.1416 1.1549 0.029 Uiso 1 1 calc R . . H8C H 0.8282 0.2255 1.1587 0.029 Uiso 1 1 calc R . . C9 C 0.63800(13) 0.15347(7) 0.75158(9) 0.01589(15) Uani 1 1 d . . . H9A H 0.6043 0.2087 0.7323 0.019 Uiso 1 1 calc R . . H9B H 0.7023 0.1308 0.6910 0.019 Uiso 1 1 calc R . . C10 C 0.76440(13) 0.15128(7) 0.86057(9) 0.01587(15) Uani 1 1 d . . . H10A H 0.8566 0.1088 0.8577 0.019 Uiso 1 1 calc R . . H10B H 0.8297 0.2022 0.8721 0.019 Uiso 1 1 calc R . . O1 O 0.09442(10) 0.01614(5) 0.91381(6) 0.01490(12) Uani 1 1 d . . . O2 O 0.25670(11) 0.05782(5) 1.10563(6) 0.01578(12) Uani 1 1 d . . . O3 O 0.76278(12) 0.12432(5) 0.48446(7) 0.01777(13) Uani 1 1 d . . . O4 O 0.98729(14) 0.19399(6) 0.39717(8) 0.02494(18) Uani 1 1 d . . . O5 O 0.73245(14) 0.26191(6) 0.45491(10) 0.0291(2) Uani 1 1 d . . . O6 O 0.96142(12) 0.21248(5) 0.58714(7) 0.02026(15) Uani 1 1 d . . . H1 H 0.183(3) 0.0391(13) 1.0487(18) 0.035(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00902(4) 0.01222(5) 0.00997(4) -0.00026(4) -0.00017(3) -0.00071(3) Cl1 0.01503(8) 0.01211(8) 0.01164(8) -0.00101(6) 0.00074(6) -0.00217(6) N1 0.0103(2) 0.0122(3) 0.0120(3) -0.0001(2) 0.0000(2) -0.0006(2) N2 0.0106(3) 0.0162(3) 0.0120(3) -0.0005(2) 0.0018(2) 0.0003(2) C1 0.0120(3) 0.0132(3) 0.0120(3) -0.0016(3) -0.0003(3) 0.0002(2) C2 0.0123(3) 0.0154(4) 0.0112(3) -0.0014(3) 0.0013(3) 0.0023(2) N3 0.0112(3) 0.0125(3) 0.0114(3) 0.0013(2) -0.0003(2) -0.0010(2) N4 0.0099(3) 0.0133(3) 0.0148(3) 0.0001(2) -0.0001(2) -0.0004(2) C3 0.0138(3) 0.0124(3) 0.0121(3) 0.0010(3) -0.0018(3) -0.0004(3) C4 0.0120(3) 0.0114(3) 0.0157(4) 0.0003(3) -0.0026(3) 0.0000(2) C5 0.0154(3) 0.0164(4) 0.0149(4) -0.0032(3) -0.0024(3) -0.0008(3) C6 0.0168(4) 0.0281(5) 0.0118(3) -0.0015(3) 0.0020(3) 0.0011(3) C7 0.0248(5) 0.0231(5) 0.0120(4) -0.0001(3) -0.0024(3) -0.0036(4) C8 0.0157(4) 0.0205(4) 0.0212(4) -0.0005(3) -0.0057(3) -0.0039(3) C9 0.0116(3) 0.0203(4) 0.0160(4) 0.0021(3) 0.0025(3) -0.0010(3) C10 0.0100(3) 0.0200(4) 0.0177(4) 0.0004(3) 0.0018(3) -0.0013(3) O1 0.0126(3) 0.0178(3) 0.0143(3) 0.0021(2) 0.0011(2) -0.0041(2) O2 0.0144(3) 0.0200(3) 0.0129(3) 0.0018(2) 0.0013(2) -0.0045(2) O3 0.0214(3) 0.0166(3) 0.0153(3) -0.0011(2) 0.0017(3) -0.0089(3) O4 0.0317(4) 0.0256(4) 0.0196(4) -0.0029(3) 0.0134(3) -0.0090(3) O5 0.0269(4) 0.0180(4) 0.0401(6) -0.0039(4) -0.0091(4) 0.0063(3) O6 0.0245(4) 0.0211(4) 0.0141(3) -0.0015(3) -0.0038(3) -0.0076(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.8177(9) . ? Ni1 N4 1.8328(8) . ? Ni1 N1 1.8379(8) . ? Ni1 N3 1.8582(8) . ? Cl1 O5 1.4404(10) . ? Cl1 O4 1.4445(9) . ? Cl1 O6 1.4493(8) . ? Cl1 O3 1.4498(8) . ? N1 O1 1.3078(11) . ? N1 C1 1.3182(12) . ? N2 C2 1.2978(12) . ? N2 C9 1.4774(13) . ? C1 C2 1.4803(14) . ? C1 C5 1.4958(13) . ? C2 C6 1.4907(14) . ? N3 C3 1.2969(12) . ? N3 O2 1.3612(11) . ? N4 C4 1.2877(13) . ? N4 C10 1.4739(13) . ? C3 C7 1.4818(14) . ? C3 C4 1.5035(14) . ? C4 C8 1.4889(13) . ? C9 C10 1.5456(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N4 88.50(4) . . ? N2 Ni1 N1 85.19(4) . . ? N4 Ni1 N1 173.23(4) . . ? N2 Ni1 N3 172.43(4) . . ? N4 Ni1 N3 84.12(4) . . ? N1 Ni1 N3 102.26(4) . . ? O5 Cl1 O4 109.60(7) . . ? O5 Cl1 O6 109.95(6) . . ? O4 Cl1 O6 109.30(6) . . ? O5 Cl1 O3 109.84(6) . . ? O4 Cl1 O3 109.16(5) . . ? O6 Cl1 O3 108.98(5) . . ? O1 N1 C1 123.44(8) . . ? O1 N1 Ni1 121.61(6) . . ? C1 N1 Ni1 114.95(7) . . ? C2 N2 C9 129.76(9) . . ? C2 N2 Ni1 115.18(7) . . ? C9 N2 Ni1 114.69(6) . . ? N1 C1 C2 111.22(8) . . ? N1 C1 C5 123.85(9) . . ? C2 C1 C5 124.93(9) . . ? N2 C2 C1 113.44(8) . . ? N2 C2 C6 125.87(9) . . ? C1 C2 C6 120.68(9) . . ? C3 N3 O2 119.47(8) . . ? C3 N3 Ni1 115.56(7) . . ? O2 N3 Ni1 124.58(6) . . ? C4 N4 C10 129.43(8) . . ? C4 N4 Ni1 115.95(7) . . ? C10 N4 Ni1 114.54(6) . . ? N3 C3 C7 124.84(9) . . ? N3 C3 C4 111.17(8) . . ? C7 C3 C4 123.97(9) . . ? N4 C4 C8 126.16(10) . . ? N4 C4 C3 112.82(8) . . ? C8 C4 C3 121.02(9) . . ? N2 C9 C10 108.50(8) . . ? N4 C10 C9 108.18(7) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.890 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.115 data_complex5 _database_code_depnum_ccdc_archive 'CCDC 895613' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(Medoen)Zn(Me3TACN)(MeCN)](ClO4)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 Cl2 N8.50 Ni O10 Zn' _chemical_formula_weight 778.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5005(4) _cell_length_b 20.8961(7) _cell_length_c 14.2514(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.6370(10) _cell_angle_gamma 90.00 _cell_volume 3225.65(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9777 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.26 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1614 _exptl_absorpt_coefficient_mu 1.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6041 _exptl_absorpt_correction_T_max 0.6609 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 138960 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 37.48 _reflns_number_total 16269 _reflns_number_gt 10456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+2.9759P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16269 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.01631(2) 0.349091(13) 0.775177(17) 0.02771(6) Uani 1 1 d . . . Ni1 Ni 0.08250(2) 0.401822(14) 0.558575(19) 0.02701(7) Uani 1 1 d . . . O2 O -0.09645(14) 0.40400(8) 0.65925(11) 0.0303(3) Uani 1 1 d . . . O1 O 0.17785(15) 0.38995(10) 0.77191(12) 0.0365(4) Uani 1 1 d . . . N3 N -0.07266(16) 0.40821(9) 0.57561(12) 0.0263(3) Uani 1 1 d . . . N2 N 0.2187(2) 0.39857(10) 0.51905(16) 0.0356(4) Uani 1 1 d . . . N1 N 0.19992(17) 0.39293(10) 0.68703(14) 0.0314(4) Uani 1 1 d . . . C3 C -0.1649(2) 0.42075(11) 0.49289(16) 0.0307(4) Uani 1 1 d . . . N4 N -0.0068(2) 0.41681(10) 0.42708(13) 0.0347(4) Uani 1 1 d . . . C2 C 0.3241(2) 0.39730(14) 0.5886(2) 0.0416(5) Uani 1 1 d . . . C4 C -0.1242(2) 0.42536(11) 0.40555(16) 0.0347(4) Uani 1 1 d . . . C1 C 0.3153(2) 0.39475(14) 0.6894(2) 0.0405(5) Uani 1 1 d . . . C7 C -0.2930(2) 0.43019(14) 0.4927(2) 0.0423(5) Uani 1 1 d . . . H7A H -0.3241 0.3899 0.5105 0.064 Uiso 1 1 calc R . . H7B H -0.3460 0.4436 0.4262 0.064 Uiso 1 1 calc R . . H7C H -0.2934 0.4633 0.5414 0.064 Uiso 1 1 calc R . . C5 C 0.4233(3) 0.3908(2) 0.7823(3) 0.0662(10) Uani 1 1 d . . . H5A H 0.4520 0.3464 0.7935 0.099 Uiso 1 1 calc R . . H5B H 0.3994 0.4054 0.8386 0.099 Uiso 1 1 calc R . . H5C H 0.4898 0.4181 0.7762 0.099 Uiso 1 1 calc R . . C9 C 0.1916(3) 0.39461(16) 0.4109(2) 0.0495(7) Uani 1 1 d . . . H9A H 0.1887 0.3493 0.3899 0.059 Uiso 1 1 calc R . . H9B H 0.2565 0.4168 0.3921 0.059 Uiso 1 1 calc R . . C6 C 0.4468(3) 0.3974(2) 0.5744(3) 0.0638(9) Uani 1 1 d . . . H6A H 0.4874 0.3560 0.5953 0.096 Uiso 1 1 calc R . . H6B H 0.4982 0.4316 0.6145 0.096 Uiso 1 1 calc R . . H6C H 0.4354 0.4046 0.5039 0.096 Uiso 1 1 calc R . . C10 C 0.0681(3) 0.42615(14) 0.36134(18) 0.0440(6) Uani 1 1 d . . . H10A H 0.0793 0.4724 0.3518 0.053 Uiso 1 1 calc R . . H10B H 0.0262 0.4065 0.2953 0.053 Uiso 1 1 calc R . . C8 C -0.2109(3) 0.43929(15) 0.30328(18) 0.0503(7) Uani 1 1 d . . . H8A H -0.2116 0.4854 0.2906 0.076 Uiso 1 1 calc R . . H8B H -0.2942 0.4252 0.2979 0.076 Uiso 1 1 calc R . . H8C H -0.1839 0.4164 0.2542 0.076 Uiso 1 1 calc R . . Cl1 Cl 0.38261(7) 0.43241(4) 0.23020(5) 0.04759(15) Uani 1 1 d . . . N5 N 0.00368(18) 0.41414(10) 0.88872(13) 0.0320(4) Uani 1 1 d . . . N8 N 0.0293(2) 0.27578(12) 0.66592(18) 0.0469(5) Uani 1 1 d . . . N6 N 0.1128(2) 0.28924(11) 0.90332(17) 0.0416(5) Uani 1 1 d . . . N7 N -0.1447(2) 0.30640(12) 0.79778(18) 0.0438(5) Uani 1 1 d . . . C11 C 0.1135(3) 0.39831(16) 0.97407(19) 0.0496(7) Uani 1 1 d . . . H11A H 0.1072 0.4197 1.0341 0.060 Uiso 1 1 calc R . . H11B H 0.1873 0.4156 0.9618 0.060 Uiso 1 1 calc R . . C16 C -0.1132(3) 0.40073(17) 0.9093(2) 0.0510(7) Uani 1 1 d . . . H16A H -0.1527 0.4418 0.9159 0.061 Uiso 1 1 calc R . . H16B H -0.0933 0.3776 0.9733 0.061 Uiso 1 1 calc R . . C17 C 0.0087(4) 0.48115(14) 0.8589(2) 0.0521(7) Uani 1 1 d . . . H17A H 0.0139 0.5093 0.9152 0.078 Uiso 1 1 calc R . . H17B H -0.0660 0.4913 0.8029 0.078 Uiso 1 1 calc R . . H17C H 0.0814 0.4875 0.8389 0.078 Uiso 1 1 calc R . . C12 C 0.1311(3) 0.32855(18) 0.9941(2) 0.0585(8) Uani 1 1 d . . . H12A H 0.0723 0.3140 1.0269 0.070 Uiso 1 1 calc R . . H12B H 0.2156 0.3212 1.0411 0.070 Uiso 1 1 calc R . . C15 C -0.2027(3) 0.36151(18) 0.8282(3) 0.0539(7) Uani 1 1 d . . . H15A H -0.2694 0.3460 0.8519 0.065 Uiso 1 1 calc R . . H15B H -0.2408 0.3892 0.7695 0.065 Uiso 1 1 calc R . . C13 C 0.0266(4) 0.23624(18) 0.8961(3) 0.0712(11) Uani 1 1 d . . . H13A H 0.0546 0.2118 0.9593 0.085 Uiso 1 1 calc R . . H13B H 0.0297 0.2071 0.8423 0.085 Uiso 1 1 calc R . . C20 C 0.0451(3) 0.2431(2) 0.6101(3) 0.0697(11) Uani 1 1 d . . . C14 C -0.1024(3) 0.25601(18) 0.8761(3) 0.0663(10) Uani 1 1 d . . . H14A H -0.1113 0.2723 0.9386 0.080 Uiso 1 1 calc R . . H14B H -0.1566 0.2181 0.8550 0.080 Uiso 1 1 calc R . . C19 C -0.2296(4) 0.2777(2) 0.7058(3) 0.0731(11) Uani 1 1 d . . . H19A H -0.3042 0.2627 0.7177 0.110 Uiso 1 1 calc R . . H19B H -0.1890 0.2415 0.6860 0.110 Uiso 1 1 calc R . . H19C H -0.2522 0.3098 0.6526 0.110 Uiso 1 1 calc R . . C18 C 0.2301(4) 0.2638(2) 0.8996(3) 0.0719(12) Uani 1 1 d . . . H18A H 0.2644 0.2335 0.9544 0.108 Uiso 1 1 calc R . . H18B H 0.2884 0.2991 0.9059 0.108 Uiso 1 1 calc R . . H18C H 0.2159 0.2419 0.8359 0.108 Uiso 1 1 calc R . . O4 O 0.9428(9) 0.3437(3) 0.1527(3) 0.109(3) Uani 0.719(6) 1 d P . . O5 O 0.8338(9) 0.3002(4) 0.2310(7) 0.133(4) Uani 0.719(6) 1 d P . . O3 O 0.9030(11) 0.2394(3) 0.1191(4) 0.125(3) Uani 0.719(6) 1 d P . . O6 O 1.0129(5) 0.2697(3) 0.2845(4) 0.113(2) Uani 0.719(6) 1 d P . . Cl2 Cl 0.92202(14) 0.28362(10) 0.19313(10) 0.0409(3) Uani 0.719(6) 1 d P A . O4B O 0.9967(10) 0.2959(12) 0.1601(10) 0.121(8) Uani 0.281(6) 1 d P A 2 O3B O 0.8294(17) 0.3613(6) 0.1144(10) 0.089(4) Uani 0.281(6) 1 d P A 2 O6B O 0.807(2) 0.2499(9) 0.089(2) 0.174(13) Uani 0.281(6) 1 d P A 2 O5B O 0.8117(11) 0.2732(12) 0.2106(16) 0.135(11) Uani 0.281(6) 1 d P A 2 Cl2B Cl 0.8754(8) 0.29973(17) 0.1542(7) 0.0629(18) Uani 0.281(6) 1 d P A 2 O10 O 0.4661(11) 0.3979(6) 0.2089(13) 0.194(7) Uani 0.622(5) 1 d P B 1 O9 O 0.4203(8) 0.4571(6) 0.3224(5) 0.157(4) Uani 0.622(5) 1 d P B 1 O7 O 0.3446(5) 0.4824(3) 0.1595(5) 0.103(2) Uani 0.622(5) 1 d P B 1 O8 O 0.2704(5) 0.3938(2) 0.2187(3) 0.0740(17) Uani 0.622(5) 1 d P B 1 O7B O 0.4938(8) 0.4818(5) 0.2514(6) 0.087(3) Uani 0.378(5) 1 d P B 2 O8B O 0.2846(9) 0.4622(6) 0.2153(7) 0.107(5) Uani 0.378(5) 1 d P B 2 O10B O 0.4069(9) 0.3931(5) 0.1567(7) 0.065(2) Uani 0.378(5) 1 d P B 2 O9B O 0.4314(6) 0.3987(5) 0.3245(5) 0.066(2) Uani 0.378(5) 1 d P B 2 C99 C 0.445(2) 0.5140(10) -0.0044(8) 0.080(5) Uani 0.491(7) 1 d P . . N9 N 0.3491(10) 0.5373(6) -0.0349(9) 0.106(4) Uani 0.491(7) 1 d P . . C97 C 0.571(2) 0.4842(11) 0.0400(11) 0.087(5) Uani 0.491(7) 1 d P . . C21 C 0.0629(6) 0.1983(4) 0.5369(5) 0.172(5) Uani 1 1 d . . . H21A H 0.0037 0.1631 0.5263 0.258 Uiso 1 1 calc R . . H21B H 0.1471 0.1812 0.5617 0.258 Uiso 1 1 calc R . . H21C H 0.0499 0.2207 0.4738 0.258 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02252(11) 0.03660(13) 0.02266(10) -0.00038(8) 0.00581(8) 0.00071(9) Ni1 0.02581(12) 0.03450(14) 0.02257(11) -0.00136(9) 0.01056(9) 0.00346(9) O2 0.0224(6) 0.0453(8) 0.0235(6) 0.0014(6) 0.0082(5) 0.0053(6) O1 0.0225(7) 0.0622(11) 0.0242(6) -0.0019(7) 0.0070(5) -0.0030(7) N3 0.0237(7) 0.0319(8) 0.0219(6) -0.0023(6) 0.0059(5) 0.0019(6) N2 0.0389(10) 0.0393(10) 0.0372(9) -0.0011(8) 0.0240(8) 0.0018(8) N1 0.0232(8) 0.0431(10) 0.0295(8) -0.0026(7) 0.0111(6) 0.0004(7) C3 0.0283(9) 0.0330(10) 0.0262(8) -0.0009(7) 0.0029(7) 0.0018(7) N4 0.0473(11) 0.0359(9) 0.0221(7) -0.0004(6) 0.0132(7) 0.0046(8) C2 0.0329(11) 0.0505(14) 0.0501(14) -0.0047(11) 0.0254(10) -0.0006(10) C4 0.0451(12) 0.0300(10) 0.0229(8) -0.0006(7) 0.0033(8) 0.0024(8) C1 0.0232(9) 0.0579(15) 0.0428(12) -0.0037(11) 0.0143(9) 0.0006(9) C7 0.0229(9) 0.0490(14) 0.0452(13) 0.0067(11) -0.0017(9) 0.0017(9) C5 0.0220(11) 0.126(3) 0.0489(16) -0.0090(18) 0.0095(11) -0.0062(15) C9 0.0624(18) 0.0588(17) 0.0409(13) -0.0049(12) 0.0352(13) 0.0004(13) C6 0.0369(14) 0.097(3) 0.070(2) -0.0049(19) 0.0354(15) -0.0018(15) C10 0.0640(17) 0.0460(13) 0.0284(10) -0.0022(9) 0.0240(11) -0.0023(12) C8 0.0624(18) 0.0504(15) 0.0253(10) 0.0045(10) -0.0022(10) 0.0071(13) Cl1 0.0534(4) 0.0525(4) 0.0391(3) 0.0102(3) 0.0185(3) -0.0007(3) N5 0.0335(9) 0.0412(10) 0.0217(7) 0.0010(7) 0.0099(6) 0.0004(7) N8 0.0525(13) 0.0419(11) 0.0395(11) -0.0040(9) 0.0064(10) 0.0081(10) N6 0.0396(11) 0.0472(12) 0.0364(10) 0.0100(9) 0.0106(8) 0.0111(9) N7 0.0323(10) 0.0491(12) 0.0473(12) 0.0054(10) 0.0097(9) -0.0108(9) C11 0.0489(15) 0.0626(17) 0.0265(10) -0.0057(11) -0.0017(10) 0.0048(13) C16 0.0477(15) 0.0686(19) 0.0441(14) -0.0006(13) 0.0251(12) 0.0066(13) C17 0.087(2) 0.0398(13) 0.0343(12) -0.0024(10) 0.0265(14) -0.0039(14) C12 0.0614(19) 0.071(2) 0.0309(12) 0.0086(13) -0.0009(12) 0.0096(16) C15 0.0354(13) 0.073(2) 0.0608(18) 0.0078(15) 0.0262(13) -0.0026(13) C13 0.073(2) 0.0527(19) 0.079(3) 0.0294(18) 0.014(2) 0.0010(17) C20 0.0562(19) 0.076(2) 0.0595(19) -0.0296(18) -0.0040(15) 0.0220(17) C14 0.060(2) 0.060(2) 0.076(2) 0.0266(18) 0.0187(17) -0.0150(16) C19 0.0534(19) 0.089(3) 0.064(2) -0.0025(19) 0.0036(16) -0.0399(19) C18 0.062(2) 0.096(3) 0.0582(19) 0.0316(19) 0.0198(16) 0.048(2) O4 0.217(9) 0.081(3) 0.046(2) -0.021(2) 0.067(4) -0.066(4) O5 0.180(8) 0.114(5) 0.176(7) -0.042(5) 0.152(7) -0.028(5) O3 0.259(10) 0.057(3) 0.073(3) -0.030(2) 0.074(5) -0.033(5) O6 0.102(4) 0.141(5) 0.071(3) 0.011(3) -0.005(3) -0.006(3) Cl2 0.0420(6) 0.0471(7) 0.0404(5) -0.0056(4) 0.0227(5) -0.0071(4) O4B 0.038(5) 0.26(2) 0.081(8) 0.025(12) 0.039(5) 0.031(9) O3B 0.130(12) 0.072(7) 0.070(7) -0.021(6) 0.041(8) -0.034(8) O6B 0.148(17) 0.078(11) 0.32(3) -0.113(16) 0.11(2) -0.061(12) O5B 0.036(5) 0.22(2) 0.165(16) 0.153(17) 0.058(7) 0.037(8) Cl2B 0.086(4) 0.0395(14) 0.097(4) 0.0000(18) 0.075(4) -0.0014(17) O10 0.148(10) 0.150(10) 0.35(2) -0.006(11) 0.166(12) 0.023(8) O9 0.153(7) 0.240(10) 0.078(4) -0.048(5) 0.038(4) -0.150(7) O7 0.068(3) 0.111(4) 0.110(4) 0.076(4) 0.002(3) -0.013(3) O8 0.092(3) 0.098(4) 0.0314(15) -0.0092(18) 0.0195(18) -0.059(3) O7B 0.081(5) 0.108(7) 0.068(4) 0.011(4) 0.021(4) -0.048(5) O8B 0.084(6) 0.157(11) 0.075(5) 0.026(6) 0.021(4) 0.087(7) O10B 0.069(5) 0.071(5) 0.071(5) -0.017(4) 0.047(4) -0.011(4) O9B 0.036(3) 0.110(6) 0.050(3) 0.034(4) 0.012(2) 0.010(3) C99 0.099(9) 0.090(8) 0.042(5) 0.000(6) 0.012(7) -0.038(7) N9 0.084(6) 0.126(9) 0.093(7) 0.034(6) 0.007(6) -0.019(6) C97 0.110(14) 0.100(10) 0.062(8) -0.020(9) 0.041(10) -0.031(9) C21 0.115(5) 0.225(9) 0.137(5) -0.138(6) -0.010(4) 0.066(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.0593(17) . ? Zn1 O2 2.0707(15) . ? Zn1 N5 2.1552(19) . ? Zn1 N7 2.175(2) . ? Zn1 N6 2.184(2) . ? Zn1 N8 2.225(2) . ? Ni1 N2 1.8351(19) . ? Ni1 N4 1.8361(19) . ? Ni1 N1 1.8836(19) . ? Ni1 N3 1.8848(17) . ? O2 N3 1.312(2) . ? O1 N1 1.318(2) . ? N3 C3 1.320(3) . ? N2 C2 1.283(4) . ? N2 C9 1.468(3) . ? N1 C1 1.316(3) . ? C3 C4 1.473(3) . ? C3 C7 1.486(3) . ? N4 C4 1.291(3) . ? N4 C10 1.484(3) . ? C2 C1 1.474(4) . ? C2 C6 1.492(4) . ? C4 C8 1.492(3) . ? C1 C5 1.482(4) . ? C9 C10 1.509(5) . ? Cl1 O8B 1.242(7) . ? Cl1 O10 1.316(10) . ? Cl1 O9 1.341(6) . ? Cl1 O7 1.414(4) . ? Cl1 O10B 1.431(9) . ? Cl1 O9B 1.453(6) . ? Cl1 O8 1.484(4) . ? Cl1 O7B 1.591(7) . ? N5 C11 1.467(3) . ? N5 C17 1.470(3) . ? N5 C16 1.496(4) . ? N8 C20 1.110(4) . ? N6 C13 1.467(5) . ? N6 C18 1.467(4) . ? N6 C12 1.487(4) . ? N7 C15 1.467(4) . ? N7 C19 1.473(4) . ? N7 C14 1.493(4) . ? C11 C12 1.486(5) . ? C16 C15 1.505(5) . ? C13 C14 1.473(6) . ? C20 C21 1.466(5) . ? O4 O4B 1.161(18) . ? O4 Cl2B 1.207(6) . ? O4 O3B 1.287(17) . ? O4 Cl2 1.435(5) . ? O5 O5B 0.65(3) . ? O5 Cl2B 1.333(8) . ? O5 Cl2 1.344(6) . ? O3 O6B 1.06(2) . ? O3 Cl2 1.363(5) . ? O3 Cl2B 1.431(7) . ? O3 O4B 1.57(2) . ? O6 Cl2 1.399(5) . ? O6 O4B 1.804(14) . ? O6 Cl2B 2.090(11) . ? Cl2 Cl2B 0.713(8) . ? Cl2 O4B 1.139(11) . ? Cl2 O5B 1.390(10) . ? Cl2 O6B 1.77(2) . ? Cl2 O3B 2.056(16) . ? O4B Cl2B 1.372(11) . ? O3B Cl2B 1.434(16) . ? O6B Cl2B 1.442(18) . ? O6B O5B 1.79(3) . ? O5B Cl2B 1.373(11) . ? C99 C97 0.479(16) 3_665 ? C99 N9 1.14(3) . ? C99 C99 1.37(5) 3_665 ? C99 C97 1.511(18) . ? N9 C97 1.05(2) 3_665 ? C97 C99 0.479(16) 3_665 ? C97 N9 1.05(2) 3_665 ? C97 C97 1.77(5) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 94.59(7) . . ? O1 Zn1 N5 92.55(7) . . ? O2 Zn1 N5 93.86(7) . . ? O1 Zn1 N7 173.20(8) . . ? O2 Zn1 N7 90.53(8) . . ? N5 Zn1 N7 82.64(9) . . ? O1 Zn1 N6 92.73(8) . . ? O2 Zn1 N6 172.13(8) . . ? N5 Zn1 N6 82.92(8) . . ? N7 Zn1 N6 81.94(9) . . ? O1 Zn1 N8 89.80(9) . . ? O2 Zn1 N8 89.68(8) . . ? N5 Zn1 N8 175.58(9) . . ? N7 Zn1 N8 94.70(10) . . ? N6 Zn1 N8 93.22(9) . . ? N2 Ni1 N4 86.31(10) . . ? N2 Ni1 N1 83.55(9) . . ? N4 Ni1 N1 168.90(9) . . ? N2 Ni1 N3 170.00(9) . . ? N4 Ni1 N3 83.69(8) . . ? N1 Ni1 N3 106.40(7) . . ? N3 O2 Zn1 119.73(12) . . ? N1 O1 Zn1 119.58(13) . . ? O2 N3 C3 118.32(18) . . ? O2 N3 Ni1 127.42(13) . . ? C3 N3 Ni1 114.21(15) . . ? C2 N2 C9 128.5(2) . . ? C2 N2 Ni1 116.46(17) . . ? C9 N2 Ni1 114.98(19) . . ? C1 N1 O1 118.8(2) . . ? C1 N1 Ni1 114.14(16) . . ? O1 N1 Ni1 126.89(14) . . ? N3 C3 C4 112.3(2) . . ? N3 C3 C7 121.8(2) . . ? C4 C3 C7 125.9(2) . . ? C4 N4 C10 127.9(2) . . ? C4 N4 Ni1 116.60(16) . . ? C10 N4 Ni1 114.99(18) . . ? N2 C2 C1 113.4(2) . . ? N2 C2 C6 125.9(3) . . ? C1 C2 C6 120.7(3) . . ? N4 C4 C3 113.16(19) . . ? N4 C4 C8 124.1(2) . . ? C3 C4 C8 122.7(2) . . ? N1 C1 C2 112.0(2) . . ? N1 C1 C5 123.8(2) . . ? C2 C1 C5 124.1(2) . . ? N2 C9 C10 107.5(2) . . ? N4 C10 C9 107.6(2) . . ? O8B Cl1 O10 157.9(8) . . ? O8B Cl1 O9 87.2(7) . . ? O10 Cl1 O9 114.6(9) . . ? O8B Cl1 O7 57.5(6) . . ? O10 Cl1 O7 108.4(7) . . ? O9 Cl1 O7 109.6(6) . . ? O8B Cl1 O10B 123.5(6) . . ? O10 Cl1 O10B 34.8(7) . . ? O9 Cl1 O10B 149.3(7) . . ? O7 Cl1 O10B 89.6(6) . . ? O8B Cl1 O9B 116.6(5) . . ? O10 Cl1 O9B 82.1(8) . . ? O9 Cl1 O9B 51.9(5) . . ? O7 Cl1 O9B 161.4(5) . . ? O10B Cl1 O9B 106.8(6) . . ? O8B Cl1 O8 63.2(7) . . ? O10 Cl1 O8 110.5(6) . . ? O9 Cl1 O8 107.5(3) . . ? O7 Cl1 O8 105.9(3) . . ? O10B Cl1 O8 89.0(4) . . ? O9B Cl1 O8 83.7(4) . . ? O8B Cl1 O7B 109.4(8) . . ? O10 Cl1 O7B 78.3(7) . . ? O9 Cl1 O7B 65.8(4) . . ? O7 Cl1 O7B 72.1(4) . . ? O10B Cl1 O7B 99.7(5) . . ? O9B Cl1 O7B 95.9(5) . . ? O8 Cl1 O7B 171.0(4) . . ? C11 N5 C17 110.4(2) . . ? C11 N5 C16 112.1(2) . . ? C17 N5 C16 111.1(2) . . ? C11 N5 Zn1 102.93(16) . . ? C17 N5 Zn1 111.41(14) . . ? C16 N5 Zn1 108.71(17) . . ? C20 N8 Zn1 172.7(3) . . ? C13 N6 C18 109.4(3) . . ? C13 N6 C12 111.9(3) . . ? C18 N6 C12 111.6(3) . . ? C13 N6 Zn1 103.44(19) . . ? C18 N6 Zn1 113.07(19) . . ? C12 N6 Zn1 107.15(17) . . ? C15 N7 C19 110.6(3) . . ? C15 N7 C14 113.5(3) . . ? C19 N7 C14 109.3(3) . . ? C15 N7 Zn1 102.47(17) . . ? C19 N7 Zn1 112.2(2) . . ? C14 N7 Zn1 108.70(18) . . ? N5 C11 C12 113.8(2) . . ? N5 C16 C15 112.3(2) . . ? C11 C12 N6 113.9(2) . . ? N7 C15 C16 113.1(2) . . ? N6 C13 C14 114.5(3) . . ? N8 C20 C21 178.0(7) . . ? C13 C14 N7 113.4(3) . . ? O4B O4 Cl2B 70.8(8) . . ? O4B O4 O3B 135.9(12) . . ? Cl2B O4 O3B 70.1(8) . . ? O4B O4 Cl2 50.7(7) . . ? Cl2B O4 Cl2 29.8(4) . . ? O3B O4 Cl2 98.0(7) . . ? O5B O5 Cl2B 79.7(16) . . ? O5B O5 Cl2 80.3(15) . . ? Cl2B O5 Cl2 30.9(3) . . ? O6B O3 Cl2 92.8(13) . . ? O6B O3 Cl2B 68.8(11) . . ? Cl2 O3 Cl2B 29.4(4) . . ? O6B O3 O4B 118.9(13) . . ? Cl2 O3 O4B 44.9(4) . . ? Cl2B O3 O4B 54.1(6) . . ? Cl2 O6 O4B 39.1(4) . . ? Cl2 O6 Cl2B 5.92(17) . . ? O4B O6 Cl2B 40.4(3) . . ? Cl2B Cl2 O4B 92.7(8) . . ? Cl2B Cl2 O5 73.7(5) . . ? O4B Cl2 O5 152.0(13) . . ? Cl2B Cl2 O3 80.5(6) . . ? O4B Cl2 O3 77.3(11) . . ? O5 Cl2 O3 122.6(6) . . ? Cl2B Cl2 O5B 73.7(6) . . ? O4B Cl2 O5B 166.0(9) . . ? O5 Cl2 O5B 27.2(12) . . ? O3 Cl2 O5B 96.6(13) . . ? Cl2B Cl2 O6 162.4(6) . . ? O4B Cl2 O6 90.0(7) . . ? O5 Cl2 O6 96.2(5) . . ? O3 Cl2 O6 117.0(5) . . ? O5B Cl2 O6 104.0(7) . . ? Cl2B Cl2 O4 57.2(5) . . ? O4B Cl2 O4 52.1(10) . . ? O5 Cl2 O4 100.7(5) . . ? O3 Cl2 O4 106.7(3) . . ? O5B Cl2 O4 119.6(9) . . ? O6 Cl2 O4 112.5(4) . . ? Cl2B Cl2 O6B 51.7(10) . . ? O4B Cl2 O6B 101.4(12) . . ? O5 Cl2 O6B 89.3(8) . . ? O3 Cl2 O6B 36.9(7) . . ? O5B Cl2 O6B 67.6(13) . . ? O6 Cl2 O6B 144.3(9) . . ? O4 Cl2 O6B 100.9(10) . . ? Cl2B Cl2 O3B 24.0(5) . . ? O4B Cl2 O3B 85.4(10) . . ? O5 Cl2 O3B 72.2(6) . . ? O3 Cl2 O3B 101.2(5) . . ? O5B Cl2 O3B 83.4(7) . . ? O6 Cl2 O3B 139.5(5) . . ? O4 Cl2 O3B 38.3(5) . . ? O6B Cl2 O3B 75.7(9) . . ? Cl2 O4B O4 77.2(7) . . ? Cl2 O4B Cl2B 31.3(4) . . ? O4 O4B Cl2B 56.2(5) . . ? Cl2 O4B O3 57.7(9) . . ? O4 O4B O3 109.5(9) . . ? Cl2B O4B O3 57.7(7) . . ? Cl2 O4B O6 50.9(6) . . ? O4 O4B O6 103.1(9) . . ? Cl2B O4B O6 81.1(7) . . ? O3 O4B O6 88.2(10) . . ? O4 O3B Cl2B 52.3(7) . . ? O4 O3B Cl2 43.7(5) . . ? Cl2B O3B Cl2 11.7(4) . . ? O3 O6B Cl2B 67.7(12) . . ? O3 O6B Cl2 50.3(11) . . ? Cl2B O6B Cl2 22.8(5) . . ? O3 O6B O5B 88(2) . . ? Cl2B O6B O5B 48.9(10) . . ? Cl2 O6B O5B 46.0(8) . . ? O5 O5B Cl2B 72.8(13) . . ? O5 O5B Cl2 72.5(13) . . ? Cl2B O5B Cl2 29.9(4) . . ? O5 O5B O6B 123.6(18) . . ? Cl2B O5B O6B 52.3(9) . . ? Cl2 O5B O6B 66.4(10) . . ? Cl2 Cl2B O4 93.1(9) . . ? Cl2 Cl2B O5 75.4(7) . . ? O4 Cl2B O5 114.8(5) . . ? Cl2 Cl2B O4B 56.0(8) . . ? O4 Cl2B O4B 53.1(9) . . ? O5 Cl2B O4B 126.0(10) . . ? Cl2 Cl2B O5B 76.4(6) . . ? O4 Cl2B O5B 142.2(12) . . ? O5 Cl2B O5B 27.6(13) . . ? O4B Cl2B O5B 132.3(12) . . ? Cl2 Cl2B O3 70.0(4) . . ? O4 Cl2B O3 116.4(6) . . ? O5 Cl2B O3 118.4(6) . . ? O4B Cl2B O3 68.3(11) . . ? O5B Cl2B O3 94.2(12) . . ? Cl2 Cl2B O3B 144.4(9) . . ? O4 Cl2B O3B 57.5(7) . . ? O5 Cl2B O3B 97.6(7) . . ? O4B Cl2B O3B 108.0(11) . . ? O5B Cl2B O3B 113.3(11) . . ? O3 Cl2B O3B 138.4(8) . . ? Cl2 Cl2B O6B 105.4(13) . . ? O4 Cl2B O6B 138.8(13) . . ? O5 Cl2B O6B 105.5(11) . . ? O4B Cl2B O6B 108.7(12) . . ? O5B Cl2B O6B 78.8(15) . . ? O3 Cl2B O6B 43.5(8) . . ? O3B Cl2B O6B 110.1(14) . . ? Cl2 Cl2B O6 11.7(4) . . ? O4 Cl2B O6 86.9(7) . . ? O5 Cl2B O6 69.3(6) . . ? O4B Cl2B O6 58.5(7) . . ? O5B Cl2B O6 75.7(7) . . ? O3 Cl2B O6 81.7(5) . . ? O3B Cl2B O6 133.6(7) . . ? O6B Cl2B O6 116.3(12) . . ? C97 C99 N9 66(5) 3_665 . ? C97 C99 C99 98(6) 3_665 3_665 ? N9 C99 C99 164.0(19) . 3_665 ? C97 C99 C97 116(6) 3_665 . ? N9 C99 C97 177.7(19) . . ? C99 C99 C97 18.3(6) 3_665 . ? C97 N9 C99 24.7(8) 3_665 . ? C99 C97 N9 89(5) 3_665 3_665 ? C99 C97 C99 64(6) 3_665 . ? N9 C97 C99 153(2) 3_665 . ? C99 C97 C97 50(5) 3_665 3_665 ? N9 C97 C97 138.9(18) 3_665 3_665 ? C99 C97 C97 14.0(10) . 3_665 ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.477 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.118 data_complex6 _database_code_depnum_ccdc_archive 'CCDC 895614' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(Medopn)Zn(Me3TACN)(MeCN)](ClO4)2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H42 Cl2 N8 Ni O10 Zn' _chemical_formula_weight 773.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5533(5) _cell_length_b 22.0368(8) _cell_length_c 12.9726(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.810(2) _cell_angle_gamma 90.00 _cell_volume 3193.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9985 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 37.42 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.572 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6015 _exptl_absorpt_correction_T_max 0.6947 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 126335 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 39.21 _reflns_number_total 18185 _reflns_number_gt 13961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+8.0533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18185 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1802 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.06328(2) 0.137082(13) 0.72278(2) 0.01765(6) Uani 1 1 d . . . Ni1 Ni -0.04613(3) 0.078008(14) 0.94018(3) 0.01974(7) Uani 1 1 d . . . Cl1 Cl 0.61630(16) 0.23798(7) 0.80181(12) 0.0191(2) Uani 0.717(8) 1 d P A 1 O4 O 0.5614(3) 0.20713(14) 0.8760(3) 0.0297(7) Uani 0.717(8) 1 d P A 1 O6 O 0.7159(3) 0.2728(2) 0.8628(3) 0.0453(11) Uani 0.717(8) 1 d P A 1 O5 O 0.6507(5) 0.1943(2) 0.7326(5) 0.0379(11) Uani 0.717(8) 1 d P A 1 Cl1A Cl 0.6348(6) 0.2478(4) 0.7895(6) 0.0454(14) Uani 0.283(8) 1 d P A 2 O4A O 0.7295(11) 0.2756(6) 0.7660(17) 0.079(6) Uani 0.283(8) 1 d P A 2 O6A O 0.6553(19) 0.2257(8) 0.8938(9) 0.082(6) Uani 0.283(8) 1 d P A 2 O5A O 0.6026(16) 0.1920(9) 0.7203(16) 0.058(4) Uani 0.283(8) 1 d P A 2 Cl2 Cl 0.59331(6) 0.09147(3) 0.30977(5) 0.02558(11) Uani 1 1 d . . . O9 O 0.5931(3) 0.06424(18) 0.2095(3) 0.0558(9) Uani 1 1 d . . . O10 O 0.7124(3) 0.10760(15) 0.3645(3) 0.0489(7) Uani 1 1 d . . . N1 N 0.11819(19) 0.08513(9) 0.93502(16) 0.0199(3) Uani 1 1 d . . . O1 O 0.15919(16) 0.08869(9) 0.84948(15) 0.0225(3) Uani 1 1 d . . . N3 N -0.12084(18) 0.07185(9) 0.79102(17) 0.0205(3) Uani 1 1 d . . . O2 O -0.06524(17) 0.07148(9) 0.71481(15) 0.0234(3) Uani 1 1 d . . . N4 N -0.2092(2) 0.07350(10) 0.9486(2) 0.0273(4) Uani 1 1 d . . . N2 N 0.0244(3) 0.07971(10) 1.08994(19) 0.0268(4) Uani 1 1 d . . . C1 C 0.1962(3) 0.08726(12) 1.0284(2) 0.0254(5) Uani 1 1 d . . . C2 C 0.1397(3) 0.08391(12) 1.1173(2) 0.0288(5) Uani 1 1 d . . . C3 C -0.2371(2) 0.06356(12) 0.7649(2) 0.0245(4) Uani 1 1 d . . . C4 C -0.2870(2) 0.06589(12) 0.8565(3) 0.0276(5) Uani 1 1 d . . . C5 C 0.3268(3) 0.09467(17) 1.0392(3) 0.0381(7) Uani 1 1 d . . . H5A H 0.3406 0.1021 0.9688 0.057 Uiso 1 1 calc R . . H5B H 0.3689 0.0577 1.0698 0.057 Uiso 1 1 calc R . . H5C H 0.3569 0.1291 1.0861 0.057 Uiso 1 1 calc R . . C7 C -0.3104(3) 0.05499(14) 0.6522(3) 0.0313(6) Uani 1 1 d . . . H7A H -0.3560 0.0921 0.6278 0.047 Uiso 1 1 calc R . . H7B H -0.3657 0.0210 0.6494 0.047 Uiso 1 1 calc R . . H7C H -0.2572 0.0464 0.6061 0.047 Uiso 1 1 calc R . . C8 C -0.4196(3) 0.06136(16) 0.8408(3) 0.0375(7) Uani 1 1 d . . . H8A H -0.4369 0.0477 0.9072 0.056 Uiso 1 1 calc R . . H8B H -0.4525 0.0322 0.7838 0.056 Uiso 1 1 calc R . . H8C H -0.4561 0.1012 0.8211 0.056 Uiso 1 1 calc R . . C9 C -0.0439(4) 0.07778(15) 1.1708(3) 0.0361(7) Uani 1 1 d . . . H9A H 0.0039 0.0964 1.2377 0.043 Uiso 1 1 calc R . . H9B H -0.0599 0.0350 1.1861 0.043 Uiso 1 1 calc R . . C10 C -0.1614(3) 0.11137(14) 1.1335(3) 0.0334(6) Uani 1 1 d . . . H10A H -0.1965 0.1171 1.1949 0.040 Uiso 1 1 calc R . . H10B H -0.1455 0.1521 1.1079 0.040 Uiso 1 1 calc R . . C11 C -0.2512(3) 0.07919(17) 1.0456(3) 0.0383(7) Uani 1 1 d . . . H11A H -0.2667 0.0382 1.0704 0.046 Uiso 1 1 calc R . . H11B H -0.3276 0.1020 1.0290 0.046 Uiso 1 1 calc R . . N5 N 0.1346(2) 0.08954(11) 0.60532(18) 0.0252(4) Uani 1 1 d . . . N6 N 0.20513(19) 0.20106(11) 0.71578(17) 0.0233(4) Uani 1 1 d . . . N7 N -0.03415(19) 0.18757(11) 0.58681(17) 0.0227(4) Uani 1 1 d . . . C12 C 0.2427(3) 0.12169(16) 0.5913(2) 0.0304(5) Uani 1 1 d . . . H12A H 0.2208 0.1472 0.5264 0.037 Uiso 1 1 calc R . . H12B H 0.3029 0.0916 0.5819 0.037 Uiso 1 1 calc R . . C13 C 0.2961(2) 0.16126(15) 0.6875(2) 0.0296(5) Uani 1 1 d . . . H13A H 0.3327 0.1350 0.7491 0.035 Uiso 1 1 calc R . . H13B H 0.3603 0.1867 0.6722 0.035 Uiso 1 1 calc R . . C14 C 0.1559(3) 0.24647(13) 0.6301(2) 0.0288(5) Uani 1 1 d . . . H14A H 0.1808 0.2355 0.5649 0.035 Uiso 1 1 calc R . . H14B H 0.1888 0.2871 0.6536 0.035 Uiso 1 1 calc R . . C15 C 0.0204(3) 0.24862(13) 0.6048(2) 0.0274(5) Uani 1 1 d . . . H15A H -0.0039 0.2683 0.6645 0.033 Uiso 1 1 calc R . . H15B H -0.0103 0.2737 0.5402 0.033 Uiso 1 1 calc R . . C16 C -0.0137(3) 0.15809(15) 0.4885(2) 0.0281(5) Uani 1 1 d . . . H16A H 0.0450 0.1823 0.4622 0.034 Uiso 1 1 calc R . . H16B H -0.0898 0.1577 0.4321 0.034 Uiso 1 1 calc R . . C17 C 0.0322(3) 0.09358(15) 0.5099(2) 0.0292(5) Uani 1 1 d . . . H17A H -0.0334 0.0673 0.5200 0.035 Uiso 1 1 calc R . . H17B H 0.0573 0.0784 0.4471 0.035 Uiso 1 1 calc R . . C18 C 0.1633(3) 0.02581(14) 0.6338(3) 0.0333(6) Uani 1 1 d . . . H18A H 0.0934 0.0058 0.6484 0.050 Uiso 1 1 calc R . . H18B H 0.2306 0.0239 0.6975 0.050 Uiso 1 1 calc R . . H18C H 0.1852 0.0052 0.5746 0.050 Uiso 1 1 calc R . . C19 C 0.2586(3) 0.23236(14) 0.8176(2) 0.0294(5) Uani 1 1 d . . . H19A H 0.2833 0.2023 0.8746 0.044 Uiso 1 1 calc R . . H19B H 0.1994 0.2599 0.8346 0.044 Uiso 1 1 calc R . . H19C H 0.3286 0.2557 0.8110 0.044 Uiso 1 1 calc R . . C20 C -0.1630(2) 0.19152(16) 0.5817(2) 0.0311(6) Uani 1 1 d . . . H20A H -0.1732 0.2030 0.6518 0.047 Uiso 1 1 calc R . . H20B H -0.2008 0.1520 0.5610 0.047 Uiso 1 1 calc R . . H20C H -0.2005 0.2222 0.5290 0.047 Uiso 1 1 calc R . . N8 N -0.0035(2) 0.19690(10) 0.83546(18) 0.0239(4) Uani 1 1 d . . . C21 C -0.0131(2) 0.23133(12) 0.8986(2) 0.0243(4) Uani 1 1 d . . . O3 O 0.5292(2) 0.27997(12) 0.7418(2) 0.0413(6) Uani 1 1 d . . . O7 O 0.5179(4) 0.14398(17) 0.2888(4) 0.0731(12) Uani 1 1 d . . . O8 O 0.5473(4) 0.0493(2) 0.3702(3) 0.0839(15) Uani 1 1 d . . . C6 C 0.2138(4) 0.08684(17) 1.2299(3) 0.0431(8) Uani 1 1 d . . . H6A H 0.2025 0.1264 1.2605 0.065 Uiso 1 1 calc R . . H6B H 0.2984 0.0815 1.2314 0.065 Uiso 1 1 calc R . . H6C H 0.1890 0.0545 1.2716 0.065 Uiso 1 1 calc R . . C22 C -0.0215(4) 0.27472(19) 0.9805(3) 0.0413(8) Uani 1 1 d . . . H22A H -0.0480 0.2539 1.0372 0.062 Uiso 1 1 calc R . . H22B H -0.0793 0.3064 0.9492 0.062 Uiso 1 1 calc R . . H22C H 0.0571 0.2931 1.0103 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01653(11) 0.02088(11) 0.01371(11) -0.00001(8) 0.00051(8) -0.00414(8) Ni1 0.02349(14) 0.01659(12) 0.01948(13) 0.00282(9) 0.00612(10) 0.00157(10) Cl1 0.0170(5) 0.0182(4) 0.0212(4) -0.0016(3) 0.0030(3) 0.0001(3) O4 0.0388(17) 0.0295(13) 0.0248(13) -0.0018(10) 0.0156(12) -0.0041(11) O6 0.0284(16) 0.059(2) 0.042(2) -0.0005(17) -0.0041(14) -0.0204(15) O5 0.057(3) 0.0295(17) 0.038(2) 0.0007(15) 0.031(2) 0.012(2) Cl1A 0.029(2) 0.047(3) 0.061(3) 0.011(2) 0.0132(17) 0.0079(17) O4A 0.036(6) 0.054(7) 0.140(17) -0.008(9) 0.011(7) -0.004(5) O6A 0.142(18) 0.078(10) 0.020(4) -0.001(5) 0.010(7) 0.022(11) O5A 0.059(9) 0.060(8) 0.050(7) 0.001(6) 0.007(8) -0.006(8) Cl2 0.0229(2) 0.0249(2) 0.0282(3) 0.0017(2) 0.0054(2) -0.00415(19) O9 0.0362(13) 0.083(2) 0.0460(16) -0.0278(16) 0.0069(12) -0.0073(14) O10 0.0352(13) 0.0524(16) 0.0509(16) -0.0111(13) -0.0039(11) -0.0184(12) N1 0.0206(8) 0.0189(7) 0.0169(8) 0.0013(6) -0.0013(6) 0.0026(6) O1 0.0189(7) 0.0292(8) 0.0183(7) 0.0022(6) 0.0029(6) 0.0028(6) N3 0.0181(8) 0.0192(8) 0.0229(9) 0.0042(6) 0.0028(6) -0.0033(6) O2 0.0220(8) 0.0279(8) 0.0186(7) 0.0001(6) 0.0022(6) -0.0085(6) N4 0.0318(11) 0.0213(9) 0.0335(12) 0.0021(8) 0.0171(9) -0.0005(8) N2 0.0416(13) 0.0200(8) 0.0196(9) 0.0029(7) 0.0092(8) 0.0067(8) C1 0.0281(11) 0.0221(10) 0.0196(10) 0.0006(8) -0.0053(8) 0.0039(8) C2 0.0460(16) 0.0199(9) 0.0160(9) 0.0016(7) -0.0005(9) 0.0071(9) C3 0.0190(9) 0.0218(9) 0.0309(12) 0.0062(8) 0.0029(8) -0.0031(7) C4 0.0241(11) 0.0213(10) 0.0392(14) 0.0055(9) 0.0114(10) -0.0004(8) C5 0.0244(12) 0.0442(17) 0.0368(16) 0.0100(13) -0.0083(11) 0.0004(11) C7 0.0224(11) 0.0314(12) 0.0354(14) 0.0051(10) -0.0012(10) -0.0079(9) C8 0.0244(12) 0.0340(14) 0.057(2) 0.0049(14) 0.0154(13) -0.0026(10) C9 0.059(2) 0.0298(13) 0.0246(12) 0.0057(10) 0.0201(13) 0.0101(13) C10 0.0491(17) 0.0243(11) 0.0334(14) -0.0002(10) 0.0227(13) 0.0020(11) C11 0.0429(17) 0.0379(15) 0.0428(18) -0.0047(13) 0.0267(15) -0.0071(13) N5 0.0269(10) 0.0289(10) 0.0194(9) -0.0045(7) 0.0052(7) -0.0050(8) N6 0.0205(8) 0.0286(9) 0.0190(8) -0.0039(7) 0.0017(7) -0.0083(7) N7 0.0212(8) 0.0285(9) 0.0166(8) 0.0035(7) 0.0014(6) -0.0056(7) C12 0.0270(12) 0.0394(14) 0.0256(12) -0.0058(10) 0.0080(9) -0.0039(10) C13 0.0209(10) 0.0411(15) 0.0261(12) -0.0056(10) 0.0050(9) -0.0074(10) C14 0.0305(12) 0.0294(12) 0.0261(12) 0.0028(9) 0.0061(9) -0.0119(10) C15 0.0299(12) 0.0265(11) 0.0249(11) 0.0068(9) 0.0054(9) -0.0037(9) C16 0.0275(11) 0.0384(14) 0.0160(10) 0.0015(9) 0.0010(8) -0.0096(10) C17 0.0316(12) 0.0375(13) 0.0165(10) -0.0055(9) 0.0026(9) -0.0121(10) C18 0.0408(15) 0.0281(12) 0.0314(14) -0.0078(10) 0.0097(12) 0.0000(11) C19 0.0248(11) 0.0321(12) 0.0283(12) -0.0088(10) 0.0011(9) -0.0105(9) C20 0.0203(10) 0.0445(16) 0.0258(12) 0.0118(11) 0.0012(9) -0.0011(10) N8 0.0263(9) 0.0236(9) 0.0212(9) 0.0014(7) 0.0049(7) 0.0018(7) C21 0.0256(10) 0.0267(10) 0.0191(10) 0.0009(8) 0.0030(8) 0.0003(8) O3 0.0347(12) 0.0353(12) 0.0488(15) 0.0093(11) 0.0014(10) 0.0065(9) O7 0.080(3) 0.0521(19) 0.075(3) -0.0069(18) -0.003(2) 0.0339(19) O8 0.079(3) 0.108(3) 0.059(2) 0.033(2) 0.0066(19) -0.055(2) C6 0.061(2) 0.0391(16) 0.0202(12) 0.0005(11) -0.0059(13) 0.0087(15) C22 0.049(2) 0.0447(18) 0.0292(15) -0.0128(13) 0.0091(13) 0.0017(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.0335(18) . ? Zn1 O2 2.0559(18) . ? Zn1 N7 2.145(2) . ? Zn1 N5 2.177(2) . ? Zn1 N6 2.181(2) . ? Zn1 N8 2.246(2) . ? Ni1 N2 1.905(2) . ? Ni1 N3 1.911(2) . ? Ni1 N4 1.917(2) . ? Ni1 N1 1.923(2) . ? Cl1 O5 1.439(5) . ? Cl1 O6 1.440(4) . ? Cl1 O3 1.441(3) . ? Cl1 O4 1.450(3) . ? Cl1A O4A 1.355(16) . ? Cl1A O6A 1.400(14) . ? Cl1A O3 1.411(7) . ? Cl1A O5A 1.51(2) . ? Cl2 O8 1.405(3) . ? Cl2 O10 1.423(3) . ? Cl2 O9 1.432(3) . ? Cl2 O7 1.432(3) . ? N1 C1 1.313(3) . ? N1 O1 1.316(3) . ? N3 O2 1.310(3) . ? N3 C3 1.311(3) . ? N4 C4 1.309(4) . ? N4 C11 1.466(4) . ? N2 C2 1.292(4) . ? N2 C9 1.466(4) . ? C1 C2 1.464(4) . ? C1 C5 1.488(4) . ? C2 C6 1.493(4) . ? C3 C4 1.448(4) . ? C3 C7 1.501(4) . ? C4 C8 1.497(4) . ? C9 C10 1.513(5) . ? C10 C11 1.508(5) . ? N5 C18 1.469(4) . ? N5 C17 1.480(4) . ? N5 C12 1.487(4) . ? N6 C19 1.478(3) . ? N6 C13 1.485(4) . ? N6 C14 1.496(4) . ? N7 C20 1.476(4) . ? N7 C15 1.479(4) . ? N7 C16 1.503(4) . ? C12 C13 1.519(4) . ? C14 C15 1.515(4) . ? C16 C17 1.518(5) . ? N8 C21 1.143(3) . ? C21 C22 1.451(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 84.79(8) . . ? O1 Zn1 N7 178.40(8) . . ? O2 Zn1 N7 95.91(8) . . ? O1 Zn1 N5 95.04(9) . . ? O2 Zn1 N5 91.38(8) . . ? N7 Zn1 N5 83.51(9) . . ? O1 Zn1 N6 96.47(8) . . ? O2 Zn1 N6 173.24(8) . . ? N7 Zn1 N6 82.67(8) . . ? N5 Zn1 N6 81.90(9) . . ? O1 Zn1 N8 89.35(8) . . ? O2 Zn1 N8 94.67(8) . . ? N7 Zn1 N8 92.03(9) . . ? N5 Zn1 N8 172.83(9) . . ? N6 Zn1 N8 91.99(9) . . ? N2 Ni1 N3 176.69(10) . . ? N2 Ni1 N4 96.51(12) . . ? N3 Ni1 N4 81.83(10) . . ? N2 Ni1 N1 82.25(10) . . ? N3 Ni1 N1 99.49(9) . . ? N4 Ni1 N1 177.90(10) . . ? O5 Cl1 O6 112.9(3) . . ? O5 Cl1 O3 111.0(3) . . ? O6 Cl1 O3 107.7(2) . . ? O5 Cl1 O4 109.8(3) . . ? O6 Cl1 O4 108.0(2) . . ? O3 Cl1 O4 107.2(2) . . ? O4A Cl1A O6A 115.4(13) . . ? O4A Cl1A O3 109.3(8) . . ? O6A Cl1A O3 120.9(9) . . ? O4A Cl1A O5A 109.0(12) . . ? O6A Cl1A O5A 104.2(11) . . ? O3 Cl1A O5A 95.4(9) . . ? O8 Cl2 O10 110.0(2) . . ? O8 Cl2 O9 108.5(3) . . ? O10 Cl2 O9 109.54(19) . . ? O8 Cl2 O7 110.0(3) . . ? O10 Cl2 O7 110.9(2) . . ? O9 Cl2 O7 107.9(2) . . ? C1 N1 O1 117.8(2) . . ? C1 N1 Ni1 114.9(2) . . ? O1 N1 Ni1 127.28(15) . . ? N1 O1 Zn1 118.28(14) . . ? O2 N3 C3 118.1(2) . . ? O2 N3 Ni1 125.66(16) . . ? C3 N3 Ni1 116.07(19) . . ? N3 O2 Zn1 116.42(15) . . ? C4 N4 C11 119.6(3) . . ? C4 N4 Ni1 114.2(2) . . ? C11 N4 Ni1 126.2(2) . . ? C2 N2 C9 120.8(3) . . ? C2 N2 Ni1 115.1(2) . . ? C9 N2 Ni1 124.1(2) . . ? N1 C1 C2 112.7(3) . . ? N1 C1 C5 122.0(3) . . ? C2 C1 C5 125.2(3) . . ? N2 C2 C1 115.1(2) . . ? N2 C2 C6 124.3(3) . . ? C1 C2 C6 120.6(3) . . ? N3 C3 C4 112.2(2) . . ? N3 C3 C7 123.7(3) . . ? C4 C3 C7 124.0(2) . . ? N4 C4 C3 115.4(2) . . ? N4 C4 C8 124.9(3) . . ? C3 C4 C8 119.6(3) . . ? N2 C9 C10 111.1(2) . . ? C11 C10 C9 113.6(3) . . ? N4 C11 C10 112.0(3) . . ? C18 N5 C17 110.4(2) . . ? C18 N5 C12 110.1(3) . . ? C17 N5 C12 112.7(2) . . ? C18 N5 Zn1 112.68(18) . . ? C17 N5 Zn1 101.09(18) . . ? C12 N5 Zn1 109.67(17) . . ? C19 N6 C13 109.6(2) . . ? C19 N6 C14 110.2(2) . . ? C13 N6 C14 111.7(2) . . ? C19 N6 Zn1 114.29(17) . . ? C13 N6 Zn1 102.43(16) . . ? C14 N6 Zn1 108.42(15) . . ? C20 N7 C15 109.8(2) . . ? C20 N7 C16 111.3(2) . . ? C15 N7 C16 112.0(2) . . ? C20 N7 Zn1 112.25(16) . . ? C15 N7 Zn1 103.26(15) . . ? C16 N7 Zn1 108.09(17) . . ? N5 C12 C13 110.5(2) . . ? N6 C13 C12 112.2(2) . . ? N6 C14 C15 111.0(2) . . ? N7 C15 C14 112.4(2) . . ? N7 C16 C17 111.9(2) . . ? N5 C17 C16 112.1(2) . . ? C21 N8 Zn1 165.6(2) . . ? N8 C21 C22 178.3(3) . . ? Cl1A O3 Cl1 14.8(3) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.034 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.154 data_complex7 _database_code_depnum_ccdc_archive 'CCDC 895615' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(OAc)Ni(Medoen)Zn(Me3TACN)]ClO4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H40 Cl N7 Ni O8 Zn' _chemical_formula_weight 678.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.853(4) _cell_length_b 18.337(4) _cell_length_c 16.409(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.05(3) _cell_angle_gamma 90.00 _cell_volume 5673(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9863 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.72 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5287 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2001)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 51719 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 29.13 _reflns_number_total 7185 _reflns_number_gt 5416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054 (Bruker, 2007)' _computing_cell_refinement 'SAINT V7.68A (Bruker, 2007)' _computing_data_reduction 'SAINT V7.68A (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+31.8882P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7185 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.217913(18) 1.035366(18) 0.940792(19) 0.02218(9) Uani 1 1 d . A . Ni2 Ni 0.31629(2) 0.89675(2) 1.03083(2) 0.03061(12) Uani 1 1 d . A . Cl1 Cl 0.5000 0.23877(6) 0.2500 0.0262(2) Uani 1 2 d S . . N1 N 0.34784(14) 0.95033(14) 0.93835(15) 0.0274(6) Uani 1 1 d . . . C1 C 0.41612(18) 0.94421(19) 0.9230(2) 0.0341(7) Uani 1 1 d . . . C2 C 0.45170(19) 0.8978(2) 0.9833(2) 0.0390(8) Uani 1 1 d . . . N2 N 0.41057(18) 0.87226(17) 1.0379(2) 0.0416(7) Uani 1 1 d . . . N3 N 0.21682(16) 0.89267(14) 1.02154(15) 0.0292(6) Uani 1 1 d . . . N4 N 0.30125(19) 0.81565(15) 1.09638(16) 0.0388(7) Uani 1 1 d . . . O1 O 0.30836(12) 0.99106(13) 0.88992(12) 0.0294(5) Uani 1 1 d . . . O2 O 0.17600(13) 0.93964(13) 0.98473(14) 0.0350(5) Uani 1 1 d . . . C3 C 0.1861(2) 0.83786(17) 1.06083(18) 0.0343(8) Uani 1 1 d . . . C4 C 0.2369(2) 0.79196(17) 1.10208(19) 0.0365(8) Uani 1 1 d . . . C5 C 0.4508(2) 0.9800(2) 0.8518(2) 0.0449(9) Uani 1 1 d . . . H5A H 0.4494 0.9478 0.8058 0.067 Uiso 1 1 calc R . . H5B H 0.4992 0.9911 0.8651 0.067 Uiso 1 1 calc R . . H5C H 0.4261 1.0243 0.8388 0.067 Uiso 1 1 calc R . . C6 C 0.5296(2) 0.8844(3) 0.9774(3) 0.0590(12) Uani 1 1 d . . . H6A H 0.5455 0.8589 1.0252 0.088 Uiso 1 1 calc R . . H6B H 0.5541 0.9301 0.9733 0.088 Uiso 1 1 calc R . . H6C H 0.5394 0.8554 0.9300 0.088 Uiso 1 1 calc R . . C7 C 0.1078(2) 0.8278(2) 1.0635(2) 0.0441(9) Uani 1 1 d . . . H7A H 0.0885 0.8556 1.1078 0.066 Uiso 1 1 calc R . . H7B H 0.0971 0.7771 1.0713 0.066 Uiso 1 1 calc R . . H7C H 0.0874 0.8441 1.0131 0.066 Uiso 1 1 calc R . . C8 C 0.2164(3) 0.72325(19) 1.1448(2) 0.0528(12) Uani 1 1 d . . . H8A H 0.2056 0.6863 1.1052 0.079 Uiso 1 1 calc R . . H8B H 0.1755 0.7320 1.1781 0.079 Uiso 1 1 calc R . . H8C H 0.2551 0.7072 1.1785 0.079 Uiso 1 1 calc R . . C9 C 0.4279(3) 0.8263(2) 1.1093(3) 0.0575(12) Uani 1 1 d . . . H9A H 0.4378 0.8566 1.1563 0.069 Uiso 1 1 calc R . . H9B H 0.4695 0.7968 1.0980 0.069 Uiso 1 1 calc R . . C10 C 0.3648(3) 0.7781(2) 1.1256(2) 0.0517(11) Uani 1 1 d . . . H10A H 0.3702 0.7319 1.0975 0.062 Uiso 1 1 calc R . . H10B H 0.3608 0.7685 1.1836 0.062 Uiso 1 1 calc R . . N5 N 0.15997(16) 1.01859(16) 0.82509(17) 0.0354(7) Uani 1 1 d . . . N6 N 0.23657(17) 1.14194(16) 0.88311(19) 0.0394(7) Uani 1 1 d . . . N7 N 0.11718(17) 1.0887(2) 0.97123(19) 0.0458(8) Uani 1 1 d . . . C17 C 0.1686(2) 0.9432(2) 0.7962(2) 0.0480(10) Uani 1 1 d . A . H17A H 0.1440 0.9106 0.8323 0.072 Uiso 1 1 calc R . . H17B H 0.2181 0.9309 0.7954 0.072 Uiso 1 1 calc R . . H17C H 0.1493 0.9388 0.7423 0.072 Uiso 1 1 calc R . . C18 C 0.3109(2) 1.1646(2) 0.8902(3) 0.0483(10) Uani 1 1 d . A . H18A H 0.3406 1.1305 0.8618 0.072 Uiso 1 1 calc R . . H18B H 0.3243 1.1659 0.9466 0.072 Uiso 1 1 calc R . . H18C H 0.3166 1.2122 0.8668 0.072 Uiso 1 1 calc R . . C19 C 0.0984(2) 1.0782(3) 1.0569(2) 0.0552(11) Uani 1 1 d . A . H19A H 0.1336 1.1007 1.0908 0.083 Uiso 1 1 calc R . . H19B H 0.0962 1.0270 1.0687 0.083 Uiso 1 1 calc R . . H19C H 0.0530 1.1001 1.0673 0.083 Uiso 1 1 calc R . . O3 O 0.26625(12) 1.07233(13) 1.04557(13) 0.0322(5) Uani 1 1 d . . . O4 O 0.32239(16) 0.98639(14) 1.11717(15) 0.0436(6) Uani 1 1 d . . . C20 C 0.30083(18) 1.04943(18) 1.10613(19) 0.0301(7) Uani 1 1 d . A . Cl2 Cl 0.5000 0.68755(11) 0.2500 0.1032(10) Uani 1 2 d S . . O9 O 0.4841(7) 0.6303(9) 0.2128(9) 0.113(7) Uani 0.534(17) 1 d P . 1 O10 O 0.5338(8) 0.7441(5) 0.2271(7) 0.103(5) Uani 0.534(17) 1 d P . 1 O9A O 0.4722(4) 0.6633(4) 0.1596(8) 0.053(3) Uani 0.466(17) 1 d P . 2 O10A O 0.5768(9) 0.7072(10) 0.2100(5) 0.100(6) Uani 0.466(17) 1 d P . 2 C21 C 0.3171(2) 1.1059(2) 1.1713(2) 0.0414(9) Uani 1 1 d . . . H21A H 0.3301 1.0816 1.2210 0.062 Uiso 1 1 calc R A . H21B H 0.2759 1.1355 1.1806 0.062 Uiso 1 1 calc R . . H21C H 0.3557 1.1362 1.1536 0.062 Uiso 1 1 calc R . . O5 O 0.4793(4) 0.3137(3) 0.2576(6) 0.071(3) Uani 0.525(5) 1 d P . . O7 O 0.4548(4) 0.1956(3) 0.3023(4) 0.0603(18) Uani 0.525(5) 1 d P . . O6 O 0.4907(5) 0.2172(5) 0.1682(4) 0.087(3) Uani 0.525(5) 1 d P . . O8 O 0.5688(3) 0.2337(4) 0.2757(5) 0.085(3) Uani 0.525(5) 1 d P . . C11 C 0.2023(4) 1.0659(4) 0.7676(3) 0.0440(15) Uani 0.758(9) 1 d P A 1 H11A H 0.2492 1.0451 0.7601 0.053 Uiso 0.758(9) 1 calc PR A 1 H11B H 0.1790 1.0674 0.7148 0.053 Uiso 0.758(9) 1 calc PR A 1 C12 C 0.2092(4) 1.1420(3) 0.8004(3) 0.0450(15) Uani 0.758(9) 1 d P A 1 H12A H 0.2407 1.1698 0.7657 0.054 Uiso 0.758(9) 1 calc PR A 1 H12B H 0.1631 1.1655 0.7996 0.054 Uiso 0.758(9) 1 calc PR A 1 C13 C 0.1902(4) 1.1902(4) 0.9393(5) 0.0457(17) Uani 0.758(9) 1 d P A 1 H13A H 0.2119 1.1923 0.9929 0.055 Uiso 0.758(9) 1 calc PR A 1 H13B H 0.1891 1.2394 0.9176 0.055 Uiso 0.758(9) 1 calc PR A 1 C14 C 0.1155(4) 1.1629(3) 0.9478(4) 0.0474(16) Uani 0.758(9) 1 d P A 1 H14A H 0.0905 1.1913 0.9886 0.057 Uiso 0.758(9) 1 calc PR A 1 H14B H 0.0906 1.1681 0.8964 0.057 Uiso 0.758(9) 1 calc PR A 1 C15 C 0.0646(3) 1.0417(4) 0.9193(4) 0.0452(16) Uani 0.758(9) 1 d P A 1 H15A H 0.0626 0.9927 0.9414 0.054 Uiso 0.758(9) 1 calc PR A 1 H15B H 0.0175 1.0626 0.9227 0.054 Uiso 0.758(9) 1 calc PR A 1 C16 C 0.0873(4) 1.0384(4) 0.8313(5) 0.0416(16) Uani 0.758(9) 1 d P A 1 H16A H 0.0584 1.0029 0.8026 0.050 Uiso 0.758(9) 1 calc PR A 1 H16B H 0.0799 1.0856 0.8060 0.050 Uiso 0.758(9) 1 calc PR A 1 C12A C 0.2411(10) 1.1119(12) 0.7861(9) 0.036(4) Uani 0.242(9) 1 d P A 2 C11A C 0.1673(10) 1.0790(12) 0.7693(10) 0.036(4) Uani 0.242(9) 1 d P A 2 C14A C 0.1540(9) 1.1776(7) 0.9757(11) 0.029(4) Uani 0.242(9) 1 d P A 2 C13A C 0.1929(11) 1.1944(10) 0.8957(15) 0.038(5) Uani 0.242(9) 1 d P A 2 C15A C 0.0679(8) 1.0932(9) 0.9131(9) 0.033(4) Uani 0.242(9) 1 d P A 2 C16A C 0.0783(9) 1.0252(14) 0.8635(11) 0.032(5) Uani 0.242(9) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02554(18) 0.02232(17) 0.01867(16) 0.00364(13) -0.00134(12) -0.00110(13) Ni2 0.0433(3) 0.0244(2) 0.0241(2) 0.00166(15) -0.00964(17) 0.00376(18) Cl1 0.0290(5) 0.0262(5) 0.0234(5) 0.000 -0.0051(4) 0.000 N1 0.0314(14) 0.0279(13) 0.0230(12) -0.0058(10) -0.0059(10) 0.0021(11) C1 0.0321(17) 0.0345(17) 0.0357(17) -0.0133(14) -0.0036(14) 0.0009(14) C2 0.0352(19) 0.0321(18) 0.050(2) -0.0165(16) -0.0164(16) 0.0081(15) N2 0.0475(18) 0.0346(16) 0.0427(17) -0.0036(13) -0.0159(15) 0.0074(14) N3 0.0469(16) 0.0241(13) 0.0167(11) 0.0020(10) -0.0030(11) -0.0027(12) N4 0.071(2) 0.0252(14) 0.0200(13) -0.0002(11) -0.0085(13) 0.0125(14) O1 0.0338(12) 0.0347(12) 0.0197(10) 0.0018(9) 0.0013(9) 0.0040(10) O2 0.0383(13) 0.0334(12) 0.0334(12) 0.0151(10) -0.0085(10) -0.0087(10) C3 0.062(2) 0.0224(15) 0.0182(14) -0.0023(12) 0.0037(14) -0.0055(15) C4 0.072(3) 0.0192(15) 0.0182(14) -0.0032(12) 0.0021(15) -0.0016(16) C5 0.0355(19) 0.057(2) 0.042(2) -0.0142(18) 0.0057(16) -0.0045(17) C6 0.037(2) 0.058(3) 0.082(3) -0.021(2) -0.021(2) 0.0120(19) C7 0.063(3) 0.0356(19) 0.0338(18) 0.0009(15) 0.0112(17) -0.0182(18) C8 0.112(4) 0.0195(16) 0.0269(17) 0.0002(13) 0.012(2) 0.001(2) C9 0.070(3) 0.043(2) 0.059(3) 0.002(2) -0.035(2) 0.014(2) C10 0.086(3) 0.036(2) 0.0325(19) 0.0027(16) -0.011(2) 0.023(2) N5 0.0441(17) 0.0352(16) 0.0269(14) 0.0060(12) -0.0114(12) -0.0029(13) N6 0.0428(17) 0.0281(15) 0.0474(18) 0.0149(13) -0.0067(14) -0.0084(13) N7 0.0407(18) 0.061(2) 0.0352(16) 0.0044(15) 0.0052(13) 0.0151(16) C17 0.059(3) 0.047(2) 0.038(2) -0.0135(17) -0.0170(18) 0.0007(19) C18 0.046(2) 0.034(2) 0.065(3) 0.0128(18) 0.0057(19) -0.0123(17) C19 0.039(2) 0.087(3) 0.040(2) -0.004(2) 0.0145(17) 0.003(2) O3 0.0372(13) 0.0351(13) 0.0242(11) -0.0026(9) -0.0038(9) -0.0008(10) O4 0.0694(18) 0.0336(13) 0.0279(12) -0.0047(10) -0.0159(12) 0.0036(13) C20 0.0373(18) 0.0320(17) 0.0211(14) -0.0029(12) 0.0007(12) -0.0067(14) Cl2 0.0774(13) 0.0460(10) 0.186(3) 0.000 -0.0915(16) 0.000 O9 0.094(9) 0.140(10) 0.105(10) -0.077(9) 0.053(8) -0.065(8) O10 0.169(13) 0.062(5) 0.077(8) 0.005(4) -0.092(8) -0.009(5) O9A 0.042(4) 0.040(4) 0.078(7) -0.031(4) -0.031(4) 0.015(3) O10A 0.125(11) 0.135(12) 0.042(4) 0.018(6) -0.018(6) -0.104(10) C21 0.059(2) 0.0374(19) 0.0275(17) -0.0073(14) -0.0063(16) -0.0057(17) O5 0.096(8) 0.044(3) 0.074(5) 0.022(3) 0.007(5) 0.032(3) O7 0.088(5) 0.049(3) 0.045(3) 0.005(3) 0.012(3) -0.021(3) O6 0.127(7) 0.097(6) 0.036(3) -0.021(4) 0.007(4) -0.068(5) O8 0.041(4) 0.096(6) 0.118(7) 0.016(5) -0.034(4) 0.006(4) C11 0.054(4) 0.055(4) 0.023(2) 0.014(2) -0.003(3) 0.005(4) C12 0.056(4) 0.037(3) 0.041(3) 0.022(2) 0.001(3) 0.003(3) C13 0.049(4) 0.022(3) 0.067(5) -0.001(3) -0.005(4) 0.000(2) C14 0.043(4) 0.038(3) 0.061(4) -0.006(3) 0.006(3) 0.013(3) C15 0.024(2) 0.054(4) 0.057(4) 0.002(3) -0.008(2) -0.003(2) C16 0.042(4) 0.042(3) 0.041(4) 0.003(3) -0.016(3) -0.002(3) C12A 0.038(9) 0.049(11) 0.021(7) 0.018(7) -0.003(6) -0.005(8) C11A 0.023(8) 0.068(13) 0.018(6) 0.019(7) 0.000(6) 0.000(8) C14A 0.014(7) 0.014(6) 0.059(10) 0.000(6) -0.004(7) -0.001(5) C13A 0.039(9) 0.015(7) 0.060(12) 0.009(9) -0.010(10) 0.002(6) C15A 0.031(7) 0.028(9) 0.040(8) -0.004(6) -0.009(6) 0.006(6) C16A 0.014(6) 0.069(14) 0.014(9) -0.001(8) -0.004(6) -0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 2.056(2) . ? Zn1 O3 2.060(2) . ? Zn1 O1 2.066(2) . ? Zn1 N7 2.194(3) . ? Zn1 N6 2.200(3) . ? Zn1 N5 2.211(3) . ? Ni2 N2 1.837(3) . ? Ni2 N4 1.857(3) . ? Ni2 N3 1.883(3) . ? Ni2 N1 1.904(3) . ? Ni2 O4 2.173(2) . ? Cl1 O8 1.366(6) 2_655 ? Cl1 O8 1.366(6) . ? Cl1 O6 1.409(6) 2_655 ? Cl1 O6 1.410(6) . ? Cl1 O5 1.433(6) 2_655 ? Cl1 O5 1.433(6) . ? Cl1 O7 1.445(6) 2_655 ? Cl1 O7 1.445(6) . ? N1 C1 1.317(4) . ? N1 O1 1.320(3) . ? C1 C2 1.467(5) . ? C1 C5 1.491(5) . ? C2 N2 1.275(5) . ? C2 C6 1.493(5) . ? N2 C9 1.479(5) . ? N3 O2 1.303(3) . ? N3 C3 1.327(4) . ? N4 C4 1.293(5) . ? N4 C10 1.462(5) . ? C3 C4 1.443(5) . ? C3 C7 1.488(5) . ? C4 C8 1.492(5) . ? C9 C10 1.507(7) . ? N5 C16 1.421(8) . ? N5 C11A 1.444(18) . ? N5 C17 1.471(5) . ? N5 C11 1.511(7) . ? N5 C16A 1.669(18) . ? N6 C13A 1.28(2) . ? N6 C12 1.451(6) . ? N6 C18 1.467(5) . ? N6 C13 1.549(8) . ? N6 C12A 1.686(18) . ? N7 C15A 1.333(14) . ? N7 C14 1.415(6) . ? N7 C19 1.462(5) . ? N7 C15 1.565(7) . ? N7 C14A 1.774(15) . ? O3 C20 1.260(4) . ? O4 C20 1.239(4) . ? C20 C21 1.520(4) . ? Cl2 O9 1.251(8) 2_655 ? Cl2 O9 1.251(8) . ? Cl2 O10 1.274(11) . ? Cl2 O10 1.274(11) 2_655 ? Cl2 O10A 1.631(12) . ? Cl2 O10A 1.631(12) 2_655 ? Cl2 O9A 1.634(9) 2_655 ? Cl2 O9A 1.634(9) . ? O9 O9 1.36(4) 2_655 ? O10 O10 1.48(4) 2_655 ? O5 O5 0.818(13) 2_655 ? O5 O8 1.808(11) 2_655 ? O7 O6 1.202(10) 2_655 ? O7 O8 1.524(10) 2_655 ? O6 O7 1.202(10) 2_655 ? O6 O8 1.483(11) 2_655 ? O8 O6 1.483(11) 2_655 ? O8 O7 1.524(10) 2_655 ? O8 O5 1.808(11) 2_655 ? C11 C12 1.501(9) . ? C13 C14 1.501(9) . ? C15 C16 1.507(9) . ? C12A C11A 1.54(2) . ? C14A C13A 1.53(3) . ? C15A C16A 1.50(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O3 99.10(9) . . ? O2 Zn1 O1 97.10(10) . . ? O3 Zn1 O1 95.85(9) . . ? O2 Zn1 N7 88.14(12) . . ? O3 Zn1 N7 92.62(11) . . ? O1 Zn1 N7 169.19(10) . . ? O2 Zn1 N6 166.18(10) . . ? O3 Zn1 N6 89.77(11) . . ? O1 Zn1 N6 92.47(11) . . ? N7 Zn1 N6 80.84(13) . . ? O2 Zn1 N5 89.57(10) . . ? O3 Zn1 N5 168.62(10) . . ? O1 Zn1 N5 90.32(10) . . ? N7 Zn1 N5 80.23(12) . . ? N6 Zn1 N5 80.40(11) . . ? N2 Ni2 N4 85.17(15) . . ? N2 Ni2 N3 163.55(13) . . ? N4 Ni2 N3 82.10(13) . . ? N2 Ni2 N1 82.73(14) . . ? N4 Ni2 N1 157.36(12) . . ? N3 Ni2 N1 105.54(11) . . ? N2 Ni2 O4 95.34(13) . . ? N4 Ni2 O4 103.66(11) . . ? N3 Ni2 O4 97.76(11) . . ? N1 Ni2 O4 96.49(11) . . ? O8 Cl1 O8 172.2(7) 2_655 . ? O8 Cl1 O6 113.1(5) 2_655 2_655 ? O8 Cl1 O6 64.6(5) . 2_655 ? O8 Cl1 O6 64.6(5) 2_655 . ? O8 Cl1 O6 113.1(5) . . ? O6 Cl1 O6 147.5(7) 2_655 . ? O8 Cl1 O5 107.2(5) 2_655 2_655 ? O8 Cl1 O5 80.4(5) . 2_655 ? O6 Cl1 O5 108.5(6) 2_655 2_655 ? O6 Cl1 O5 102.6(5) . 2_655 ? O8 Cl1 O5 80.4(5) 2_655 . ? O8 Cl1 O5 107.2(5) . . ? O6 Cl1 O5 102.7(5) 2_655 . ? O6 Cl1 O5 108.5(6) . . ? O5 Cl1 O5 33.2(5) 2_655 . ? O8 Cl1 O7 109.8(5) 2_655 2_655 ? O8 Cl1 O7 65.6(5) . 2_655 ? O6 Cl1 O7 109.8(4) 2_655 2_655 ? O6 Cl1 O7 49.8(4) . 2_655 ? O5 Cl1 O7 108.2(4) 2_655 2_655 ? O5 Cl1 O7 137.4(4) . 2_655 ? O8 Cl1 O7 65.6(5) 2_655 . ? O8 Cl1 O7 109.8(5) . . ? O6 Cl1 O7 49.8(4) 2_655 . ? O6 Cl1 O7 109.8(4) . . ? O5 Cl1 O7 137.4(4) 2_655 . ? O5 Cl1 O7 108.2(4) . . ? O7 Cl1 O7 113.6(5) 2_655 . ? C1 N1 O1 118.9(3) . . ? C1 N1 Ni2 114.5(2) . . ? O1 N1 Ni2 126.6(2) . . ? N1 C1 C2 111.5(3) . . ? N1 C1 C5 122.8(3) . . ? C2 C1 C5 125.7(3) . . ? N2 C2 C1 114.2(3) . . ? N2 C2 C6 125.7(4) . . ? C1 C2 C6 120.1(4) . . ? C2 N2 C9 129.2(4) . . ? C2 N2 Ni2 117.1(3) . . ? C9 N2 Ni2 113.7(3) . . ? O2 N3 C3 117.9(3) . . ? O2 N3 Ni2 126.8(2) . . ? C3 N3 Ni2 115.2(2) . . ? C4 N4 C10 125.9(3) . . ? C4 N4 Ni2 117.0(2) . . ? C10 N4 Ni2 116.2(3) . . ? N1 O1 Zn1 116.39(17) . . ? N3 O2 Zn1 119.99(19) . . ? N3 C3 C4 112.3(3) . . ? N3 C3 C7 122.8(3) . . ? C4 C3 C7 124.8(3) . . ? N4 C4 C3 113.1(3) . . ? N4 C4 C8 124.1(4) . . ? C3 C4 C8 122.8(4) . . ? N2 C9 C10 107.5(3) . . ? N4 C10 C9 108.2(3) . . ? C16 N5 C11A 86.7(8) . . ? C16 N5 C17 111.7(4) . . ? C11A N5 C17 120.4(9) . . ? C16 N5 C11 114.1(4) . . ? C11A N5 C11 27.4(6) . . ? C17 N5 C11 106.3(4) . . ? C16 N5 C16A 20.6(6) . . ? C11A N5 C16A 105.8(11) . . ? C17 N5 C16A 107.0(9) . . ? C11 N5 C16A 133.0(9) . . ? C16 N5 Zn1 112.2(4) . . ? C11A N5 Zn1 113.0(8) . . ? C17 N5 Zn1 110.6(2) . . ? C11 N5 Zn1 101.3(3) . . ? C16A N5 Zn1 96.9(6) . . ? C13A N6 C12 85.6(10) . . ? C13A N6 C18 112.9(10) . . ? C12 N6 C18 114.4(4) . . ? C13A N6 C13 27.5(9) . . ? C12 N6 C13 110.8(4) . . ? C18 N6 C13 109.3(4) . . ? C13A N6 C12A 115.5(12) . . ? C12 N6 C12A 30.3(6) . . ? C18 N6 C12A 96.7(6) . . ? C13 N6 C12A 141.1(7) . . ? C13A N6 Zn1 119.6(10) . . ? C12 N6 Zn1 110.2(3) . . ? C18 N6 Zn1 111.8(2) . . ? C13 N6 Zn1 99.2(3) . . ? C12A N6 Zn1 97.2(6) . . ? C15A N7 C14 74.4(8) . . ? C15A N7 C19 121.7(7) . . ? C14 N7 C19 112.4(4) . . ? C15A N7 C15 37.3(7) . . ? C14 N7 C15 111.6(4) . . ? C19 N7 C15 107.3(4) . . ? C15A N7 C14A 104.2(9) . . ? C14 N7 C14A 30.2(5) . . ? C19 N7 C14A 100.1(7) . . ? C15 N7 C14A 140.9(6) . . ? C15A N7 Zn1 117.9(7) . . ? C14 N7 Zn1 112.7(3) . . ? C19 N7 Zn1 111.8(3) . . ? C15 N7 Zn1 100.3(3) . . ? C14A N7 Zn1 94.6(5) . . ? C20 O3 Zn1 141.0(2) . . ? C20 O4 Ni2 126.4(2) . . ? O4 C20 O3 126.6(3) . . ? O4 C20 C21 117.8(3) . . ? O3 C20 C21 115.6(3) . . ? O9 Cl2 O9 66(2) 2_655 . ? O9 Cl2 O10 135.1(12) 2_655 . ? O9 Cl2 O10 131.2(11) . . ? O9 Cl2 O10 131.2(11) 2_655 2_655 ? O9 Cl2 O10 135.1(12) . 2_655 ? O10 Cl2 O10 71.0(16) . 2_655 ? O9 Cl2 O10A 99.8(10) 2_655 . ? O9 Cl2 O10A 101.6(7) . . ? O10 Cl2 O10A 42.0(5) . . ? O10 Cl2 O10A 112.5(14) 2_655 . ? O9 Cl2 O10A 101.6(7) 2_655 2_655 ? O9 Cl2 O10A 99.8(10) . 2_655 ? O10 Cl2 O10A 112.5(14) . 2_655 ? O10 Cl2 O10A 42.0(5) 2_655 2_655 ? O10A Cl2 O10A 154.4(15) . 2_655 ? O9 Cl2 O9A 41.6(8) 2_655 2_655 ? O9 Cl2 O9A 106.9(13) . 2_655 ? O10 Cl2 O9A 109.2(4) . 2_655 ? O10 Cl2 O9A 96.5(7) 2_655 2_655 ? O10A Cl2 O9A 98.1(4) . 2_655 ? O10A Cl2 O9A 88.8(5) 2_655 2_655 ? O9 Cl2 O9A 106.9(13) 2_655 . ? O9 Cl2 O9A 41.6(8) . . ? O10 Cl2 O9A 96.5(7) . . ? O10 Cl2 O9A 109.2(4) 2_655 . ? O10A Cl2 O9A 88.8(5) . . ? O10A Cl2 O9A 98.1(4) 2_655 . ? O9A Cl2 O9A 148.4(7) 2_655 . ? Cl2 O9 O9 57.1(11) . 2_655 ? Cl2 O10 O10 54.5(8) . 2_655 ? O5 O5 Cl1 73.4(3) 2_655 . ? O5 O5 O8 112.7(8) 2_655 2_655 ? Cl1 O5 O8 48.2(3) . 2_655 ? O6 O7 Cl1 63.6(4) 2_655 . ? O6 O7 O8 115.8(6) 2_655 2_655 ? Cl1 O7 O8 54.7(3) . 2_655 ? O7 O6 Cl1 66.7(4) 2_655 . ? O7 O6 O8 117.6(6) 2_655 2_655 ? Cl1 O6 O8 56.3(4) . 2_655 ? Cl1 O8 O6 59.1(4) . 2_655 ? Cl1 O8 O7 59.7(4) . 2_655 ? O6 O8 O7 102.0(6) 2_655 2_655 ? Cl1 O8 O5 51.4(3) . 2_655 ? O6 O8 O5 88.5(5) 2_655 2_655 ? O7 O8 O5 88.4(5) 2_655 2_655 ? C12 C11 N5 110.8(5) . . ? N6 C12 C11 111.5(5) . . ? C14 C13 N6 113.3(5) . . ? N7 C14 C13 108.9(5) . . ? C16 C15 N7 111.4(5) . . ? N5 C16 C15 110.7(5) . . ? C11A C12A N6 104.5(13) . . ? N5 C11A C12A 105.9(13) . . ? C13A C14A N7 109.6(12) . . ? N6 C13A C14A 107.2(14) . . ? N7 C15A C16A 104.2(12) . . ? C15A C16A N5 112.7(14) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.049 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.097 data_complex8 _database_code_depnum_ccdc_archive 'CCDC 895616' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(NO2)Ni(Medoen)Zn(Me3TACN)]ClO4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H37 Cl N8 Ni O8 Zn' _chemical_formula_weight 665.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.5274(4) _cell_length_b 12.4106(5) _cell_length_c 13.0776(5) _cell_angle_alpha 98.7540(10) _cell_angle_beta 96.0040(10) _cell_angle_gamma 90.074(2) _cell_volume 1360.17(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 29.60 _exptl_crystal_description blade _exptl_crystal_colour black _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 1.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5165 _exptl_absorpt_correction_T_max 0.7937 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 42058 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 33.19 _reflns_number_total 19253 _reflns_number_gt 15193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.7167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.467(9) _refine_ls_number_reflns 19253 _refine_ls_number_parameters 699 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn01 Zn 0.79746(4) 0.78472(3) 0.05716(3) 0.01801(10) Uani 1 1 d . . . Zn1 Zn 0.43325(4) 0.28093(3) 0.68779(3) 0.01755(10) Uani 1 1 d . . . Ni03 Ni 0.59867(5) 0.83214(3) 0.27360(3) 0.01786(11) Uani 1 1 d . . . Ni1 Ni 0.63463(5) 0.25404(3) 0.47035(3) 0.01733(10) Uani 1 1 d . . . Cl1 Cl 0.16490(13) 0.79139(8) 0.65143(9) 0.0276(2) Uani 1 1 d . . . Cl06 Cl 0.07463(15) 0.27092(11) 0.09688(10) 0.0377(3) Uani 1 1 d . . . O6 O 0.8895(3) 0.7498(2) 0.2029(2) 0.0208(6) Uani 1 1 d . . . N1 N 0.4414(4) 0.3269(2) 0.4764(3) 0.0173(6) Uani 1 1 d . . . O2 O 0.5226(4) 0.1338(2) 0.6201(2) 0.0201(6) Uani 1 1 d . . . O7 O 0.5737(4) 0.7051(2) 0.0580(2) 0.0275(7) Uani 1 1 d . . . N7 N 0.5016(4) 0.2373(3) 0.8425(3) 0.0247(7) Uani 1 1 d . . . N15 N 0.8872(4) 0.6337(3) -0.0229(3) 0.0253(7) Uani 1 1 d . . . N5 N 0.2124(4) 0.2035(3) 0.7100(3) 0.0230(7) Uani 1 1 d . . . C20 C 0.5302(5) 1.0245(3) 0.2033(3) 0.0197(7) Uani 1 1 d . . . O4 O 0.8315(4) 0.4328(2) 0.6159(3) 0.0341(7) Uani 1 1 d . . . O9 O 0.1690(6) 0.8800(3) 0.7365(3) 0.0609(11) Uani 1 1 d . . . O5 O 0.7256(4) 0.9380(2) 0.1196(2) 0.0222(6) Uani 1 1 d . . . C21 C 0.4277(5) 1.0154(3) 0.2837(3) 0.0220(8) Uani 1 1 d . . . N10 N 0.4439(4) 0.9239(3) 0.3219(3) 0.0219(7) Uani 1 1 d . . . C30 C 0.9666(6) 0.9245(3) -0.0521(4) 0.0302(10) Uani 1 1 d . . . H30A H 1.0592 0.9495 -0.0824 0.036 Uiso 1 1 calc R . . H30B H 0.9176 0.9896 -0.0155 0.036 Uiso 1 1 calc R . . N3 N 0.6166(4) 0.1381(2) 0.5468(2) 0.0166(6) Uani 1 1 d . . . N9 N 0.6267(4) 0.9416(2) 0.1898(3) 0.0182(6) Uani 1 1 d . . . C15 C 0.4011(5) 0.1360(3) 0.8391(3) 0.0265(7) Uani 1 1 d . . . H15A H 0.4413 0.0759 0.7905 0.032 Uiso 1 1 calc R . . H15B H 0.4105 0.1140 0.9091 0.032 Uiso 1 1 calc R . . C19 C 0.6692(6) 0.2108(4) 0.8587(4) 0.0308(10) Uani 1 1 d . . . H19A H 0.7336 0.2770 0.8621 0.046 Uiso 1 1 calc R . . H19B H 0.6959 0.1566 0.8008 0.046 Uiso 1 1 calc R . . H19C H 0.6901 0.1813 0.9240 0.046 Uiso 1 1 calc R . . C33 C 0.8288(6) 0.6249(4) -0.1361(4) 0.0300(9) Uani 1 1 d . . . H33A H 0.9159 0.6454 -0.1741 0.036 Uiso 1 1 calc R . . H33B H 0.7990 0.5480 -0.1633 0.036 Uiso 1 1 calc R . . N12 N 0.5732(4) 0.7612(3) 0.3846(3) 0.0230(7) Uani 1 1 d . . . C14 C 0.4555(5) 0.3271(3) 0.9227(3) 0.0281(8) Uani 1 1 d . . . H14A H 0.5386 0.3381 0.9823 0.034 Uiso 1 1 calc R . . H14B H 0.3564 0.3062 0.9486 0.034 Uiso 1 1 calc R . . O11 O 0.3202(5) 0.7459(4) 0.6497(3) 0.0514(10) Uani 1 1 d . . . O12 O 0.0589(4) 0.7089(3) 0.6693(3) 0.0434(8) Uani 1 1 d . . . N8 N 0.7200(4) 0.3680(2) 0.6120(3) 0.0214(7) Uani 1 1 d . . . N16 N 0.5010(4) 0.7181(3) 0.1406(3) 0.0218(7) Uani 1 1 d . . . N13 N 1.0196(5) 0.8518(3) 0.0238(3) 0.0258(8) Uani 1 1 d . . . C12 C 0.1623(5) 0.3895(3) 0.7920(3) 0.0295(8) Uani 1 1 d . . . H12A H 0.1588 0.3716 0.8630 0.035 Uiso 1 1 calc R . . H12B H 0.0936 0.4527 0.7848 0.035 Uiso 1 1 calc R . . C11 C 0.1000(5) 0.2936(3) 0.7138(3) 0.0294(8) Uani 1 1 d . . . H11A H -0.0018 0.2684 0.7327 0.035 Uiso 1 1 calc R . . H11B H 0.0809 0.3161 0.6442 0.035 Uiso 1 1 calc R . . C38 C 0.8343(6) 0.5363(3) 0.0191(4) 0.0360(10) Uani 1 1 d . . . H38A H 0.8813 0.4708 -0.0163 0.054 Uiso 1 1 calc R . . H38B H 0.7191 0.5295 0.0072 0.054 Uiso 1 1 calc R . . H38C H 0.8678 0.5445 0.0939 0.054 Uiso 1 1 calc R . . O10 O 0.1192(5) 0.8266(3) 0.5536(3) 0.0493(10) Uani 1 1 d . . . N2 N 0.6546(5) 0.3324(3) 0.3631(3) 0.0233(7) Uani 1 1 d . . . N4 N 0.7950(4) 0.1702(3) 0.4173(3) 0.0208(7) Uani 1 1 d . . . O1 O 0.3390(4) 0.3210(2) 0.5452(2) 0.0220(6) Uani 1 1 d . . . C1 C 0.4116(5) 0.3921(3) 0.4062(3) 0.0227(8) Uani 1 1 d . . . C2 C 0.5349(5) 0.3924(3) 0.3379(3) 0.0221(8) Uani 1 1 d . . . C3 C 0.7198(5) 0.0591(3) 0.5296(3) 0.0186(7) Uani 1 1 d . . . C4 C 0.8182(5) 0.0781(3) 0.4494(3) 0.0189(7) Uani 1 1 d . . . C5 C 0.2677(5) 0.4617(4) 0.4026(4) 0.0317(10) Uani 1 1 d . . . H5A H 0.1844 0.4288 0.4346 0.048 Uiso 1 1 calc R . . H5B H 0.2306 0.4670 0.3300 0.048 Uiso 1 1 calc R . . H5C H 0.2941 0.5348 0.4407 0.048 Uiso 1 1 calc R . . C6 C 0.5197(7) 0.4552(4) 0.2481(4) 0.0374(11) Uani 1 1 d . . . H6A H 0.6156 0.4470 0.2126 0.056 Uiso 1 1 calc R . . H6B H 0.5049 0.5325 0.2738 0.056 Uiso 1 1 calc R . . H6C H 0.4287 0.4272 0.1992 0.056 Uiso 1 1 calc R . . C7 C 0.7342(6) -0.0325(3) 0.5924(3) 0.0262(8) Uani 1 1 d . . . H7A H 0.7180 -0.0049 0.6647 0.039 Uiso 1 1 calc R . . H7B H 0.8395 -0.0636 0.5899 0.039 Uiso 1 1 calc R . . H7C H 0.6544 -0.0890 0.5636 0.039 Uiso 1 1 calc R . . C9 C 0.8034(6) 0.3199(4) 0.3168(4) 0.0291(9) Uani 1 1 d . . . H9A H 0.8801 0.3770 0.3523 0.035 Uiso 1 1 calc R . . H9B H 0.7862 0.3275 0.2422 0.035 Uiso 1 1 calc R . . C10 C 0.8675(6) 0.2061(3) 0.3291(4) 0.0288(9) Uani 1 1 d . . . H10A H 0.8392 0.1542 0.2644 0.035 Uiso 1 1 calc R . . H10B H 0.9839 0.2094 0.3438 0.035 Uiso 1 1 calc R . . O3 O 0.6488(4) 0.3722(2) 0.6927(2) 0.0247(6) Uani 1 1 d . . . C8 C 0.9322(5) -0.0040(3) 0.4046(3) 0.0235(8) Uani 1 1 d . . . H8A H 0.8912 -0.0350 0.3334 0.035 Uiso 1 1 calc R . . H8B H 0.9453 -0.0624 0.4474 0.035 Uiso 1 1 calc R . . H8C H 1.0344 0.0319 0.4039 0.035 Uiso 1 1 calc R . . N6 N 0.3292(5) 0.4201(3) 0.7784(3) 0.0263(7) Uani 1 1 d . . . C13 C 0.4317(6) 0.4343(3) 0.8781(3) 0.0302(10) Uani 1 1 d . . . H13A H 0.3842 0.4883 0.9292 0.036 Uiso 1 1 calc R . . H13B H 0.5357 0.4637 0.8673 0.036 Uiso 1 1 calc R . . C16 C 0.2334(6) 0.1525(3) 0.8058(3) 0.0299(10) Uani 1 1 d . . . H16A H 0.1863 0.1995 0.8623 0.036 Uiso 1 1 calc R . . H16B H 0.1767 0.0812 0.7930 0.036 Uiso 1 1 calc R . . C17 C 0.1594(5) 0.1184(4) 0.6186(3) 0.0307(9) Uani 1 1 d . . . H17A H 0.2376 0.0606 0.6124 0.046 Uiso 1 1 calc R . . H17B H 0.1485 0.1517 0.5550 0.046 Uiso 1 1 calc R . . H17C H 0.0576 0.0872 0.6287 0.046 Uiso 1 1 calc R . . C18 C 0.3326(6) 0.5186(3) 0.7284(4) 0.0364(10) Uani 1 1 d . . . H18A H 0.3005 0.5816 0.7760 0.055 Uiso 1 1 calc R . . H18B H 0.2598 0.5086 0.6644 0.055 Uiso 1 1 calc R . . H18C H 0.4398 0.5313 0.7115 0.055 Uiso 1 1 calc R . . N11 N 0.7913(4) 0.7540(2) 0.2733(3) 0.0173(6) Uani 1 1 d . . . C22 C 0.8176(5) 0.6951(3) 0.3483(3) 0.0212(8) Uani 1 1 d . . . C23 C 0.6859(5) 0.7026(3) 0.4158(3) 0.0233(8) Uani 1 1 d . . . C24 C 0.5281(6) 1.1165(3) 0.1405(4) 0.0307(10) Uani 1 1 d . . . H24A H 0.6328 1.1254 0.1180 0.046 Uiso 1 1 calc R . . H24B H 0.4997 1.1841 0.1832 0.046 Uiso 1 1 calc R . . H24C H 0.4504 1.0999 0.0793 0.046 Uiso 1 1 calc R . . C25 C 0.3128(5) 1.1025(3) 0.3169(3) 0.0290(9) Uani 1 1 d . . . H25A H 0.2097 1.0854 0.2770 0.043 Uiso 1 1 calc R . . H25B H 0.3514 1.1732 0.3041 0.043 Uiso 1 1 calc R . . H25C H 0.3026 1.1057 0.3912 0.043 Uiso 1 1 calc R . . C26 C 0.9597(6) 0.6278(3) 0.3596(4) 0.0311(10) Uani 1 1 d . . . H26A H 0.9535 0.5662 0.3026 0.047 Uiso 1 1 calc R . . H26B H 0.9656 0.6002 0.4262 0.047 Uiso 1 1 calc R . . H26C H 1.0539 0.6722 0.3574 0.047 Uiso 1 1 calc R . . C27 C 0.6909(6) 0.6431(4) 0.5084(4) 0.0326(10) Uani 1 1 d . . . H27A H 0.5896 0.6505 0.5377 0.049 Uiso 1 1 calc R . . H27B H 0.7753 0.6744 0.5613 0.049 Uiso 1 1 calc R . . H27C H 0.7110 0.5658 0.4865 0.049 Uiso 1 1 calc R . . C28 C 0.3670(5) 0.8947(4) 0.4085(3) 0.0273(8) Uani 1 1 d . . . H28A H 0.2510 0.8963 0.3926 0.033 Uiso 1 1 calc R . . H28B H 0.3977 0.9476 0.4722 0.033 Uiso 1 1 calc R . . C29 C 0.4170(6) 0.7818(4) 0.4254(4) 0.0323(10) Uani 1 1 d . . . H29A H 0.4257 0.7761 0.5005 0.039 Uiso 1 1 calc R . . H29B H 0.3380 0.7271 0.3883 0.039 Uiso 1 1 calc R . . O8 O 0.3832(4) 0.6596(3) 0.1370(3) 0.0381(8) Uani 1 1 d . . . N14 N 0.7201(5) 0.8101(3) -0.1020(3) 0.0248(7) Uani 1 1 d . . . C31 C 0.8459(5) 0.8672(3) -0.1411(3) 0.0303(8) Uani 1 1 d . . . H31A H 0.7987 0.9224 -0.1818 0.036 Uiso 1 1 calc R . . H31B H 0.9018 0.8144 -0.1885 0.036 Uiso 1 1 calc R . . C32 C 0.6924(5) 0.6939(3) -0.1576(3) 0.0295(8) Uani 1 1 d . . . H32A H 0.5975 0.6628 -0.1347 0.035 Uiso 1 1 calc R . . H32B H 0.6729 0.6944 -0.2335 0.035 Uiso 1 1 calc R . . C34 C 1.0575(4) 0.6495(3) 0.0010(3) 0.0289(8) Uani 1 1 d . . . H34A H 1.1120 0.5891 -0.0388 0.035 Uiso 1 1 calc R . . H34B H 1.0869 0.6479 0.0760 0.035 Uiso 1 1 calc R . . C35 C 1.1105(5) 0.7568(4) -0.0261(3) 0.0304(8) Uani 1 1 d . . . H35A H 1.0960 0.7537 -0.1026 0.036 Uiso 1 1 calc R . . H35B H 1.2243 0.7686 -0.0028 0.036 Uiso 1 1 calc R . . C36 C 1.1063(5) 0.9121(4) 0.1148(3) 0.0354(10) Uani 1 1 d . . . H36A H 1.1992 0.9470 0.0948 0.053 Uiso 1 1 calc R . . H36B H 1.1399 0.8623 0.1640 0.053 Uiso 1 1 calc R . . H36C H 1.0388 0.9680 0.1477 0.053 Uiso 1 1 calc R . . C37 C 0.5687(6) 0.8668(4) -0.1110(4) 0.0292(10) Uani 1 1 d . . . H37A H 0.5810 0.9406 -0.0716 0.044 Uiso 1 1 calc R . . H37B H 0.4884 0.8264 -0.0830 0.044 Uiso 1 1 calc R . . H37C H 0.5358 0.8710 -0.1843 0.044 Uiso 1 1 calc R . . O13 O 0.1216(10) 0.3479(6) 0.0403(6) 0.154(4) Uani 1 1 d . . . O14 O 0.1256(6) 0.2978(5) 0.2031(4) 0.0740(14) Uani 1 1 d . . . O15 O 0.1579(7) 0.1719(4) 0.0596(4) 0.0816(14) Uani 1 1 d . . . O16 O -0.0872(6) 0.2558(9) 0.0864(4) 0.151(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn01 0.0174(2) 0.0225(2) 0.0146(2) 0.00290(16) 0.00372(17) 0.00321(16) Zn1 0.0176(2) 0.02090(19) 0.0147(2) 0.00364(15) 0.00283(17) 0.00435(16) Ni03 0.0164(2) 0.0232(2) 0.0166(2) 0.00902(18) 0.00561(19) 0.00624(17) Ni1 0.0163(2) 0.0199(2) 0.0181(3) 0.00819(17) 0.00445(19) 0.00578(17) Cl1 0.0329(6) 0.0289(5) 0.0242(5) 0.0084(4) 0.0112(4) 0.0025(4) Cl06 0.0325(7) 0.0579(7) 0.0286(6) 0.0205(5) 0.0107(5) 0.0088(5) O6 0.0150(15) 0.0317(14) 0.0153(14) 0.0024(11) 0.0012(11) 0.0067(11) N1 0.0184(17) 0.0164(13) 0.0181(16) 0.0052(11) 0.0023(13) 0.0030(11) O2 0.0255(15) 0.0186(11) 0.0185(14) 0.0057(10) 0.0095(11) 0.0035(10) O7 0.0296(18) 0.0280(14) 0.0240(16) 0.0051(12) -0.0031(13) -0.0050(12) N7 0.0241(17) 0.0330(17) 0.0173(16) 0.0042(13) 0.0032(13) 0.0109(13) N15 0.0200(16) 0.0319(17) 0.0222(17) -0.0002(13) 0.0006(13) 0.0071(13) N5 0.0185(17) 0.0283(16) 0.0250(18) 0.0077(13) 0.0102(13) 0.0035(12) C20 0.0242(19) 0.0178(15) 0.0156(17) 0.0000(12) -0.0007(14) 0.0046(13) O4 0.0319(18) 0.0308(15) 0.0405(19) 0.0150(13) -0.0065(14) -0.0098(12) O9 0.100(3) 0.0407(19) 0.044(2) -0.0062(16) 0.034(2) -0.016(2) O5 0.0283(16) 0.0208(12) 0.0195(14) 0.0053(10) 0.0094(12) 0.0032(11) C21 0.0170(18) 0.0229(16) 0.0241(19) -0.0002(14) -0.0010(14) 0.0071(13) N10 0.0167(16) 0.0308(16) 0.0184(16) 0.0020(13) 0.0050(12) 0.0042(12) C30 0.045(3) 0.0246(18) 0.021(2) 0.0033(15) 0.0049(18) -0.0066(17) N3 0.0194(16) 0.0174(13) 0.0131(14) 0.0025(11) 0.0024(12) 0.0019(11) N9 0.0198(16) 0.0212(14) 0.0145(15) 0.0047(11) 0.0022(12) 0.0045(12) C15 0.039(2) 0.0228(16) 0.0196(16) 0.0086(13) 0.0045(14) 0.0036(14) C19 0.025(2) 0.041(2) 0.028(2) 0.0111(18) -0.0009(19) 0.0041(18) C33 0.034(2) 0.031(2) 0.022(2) -0.0010(16) -0.0018(17) -0.0075(17) N12 0.0182(17) 0.0308(16) 0.0224(17) 0.0086(13) 0.0064(13) 0.0025(12) C14 0.038(2) 0.0270(17) 0.0174(16) 0.0006(13) -0.0020(14) -0.0005(15) O11 0.0339(19) 0.082(3) 0.048(2) 0.036(2) 0.0111(16) 0.0139(18) O12 0.0418(19) 0.0393(17) 0.052(2) 0.0097(15) 0.0138(16) -0.0126(14) N8 0.0185(16) 0.0200(14) 0.0265(18) 0.0096(12) -0.0025(13) 0.0034(11) N16 0.0166(16) 0.0232(14) 0.0277(18) 0.0129(13) -0.0008(13) 0.0002(11) N13 0.0248(19) 0.0350(18) 0.0195(17) 0.0094(13) 0.0045(14) -0.0018(14) C12 0.0272(19) 0.033(2) 0.030(2) 0.0038(16) 0.0103(15) 0.0109(15) C11 0.0213(18) 0.034(2) 0.034(2) 0.0075(16) 0.0051(15) 0.0023(15) C38 0.044(3) 0.0251(18) 0.037(2) 0.0069(16) -0.005(2) 0.0068(17) O10 0.050(2) 0.072(2) 0.0368(19) 0.0345(18) 0.0157(16) 0.0278(19) N2 0.0268(19) 0.0266(15) 0.0201(17) 0.0135(13) 0.0051(14) 0.0004(13) N4 0.0174(16) 0.0282(15) 0.0183(16) 0.0061(12) 0.0054(12) 0.0075(12) O1 0.0193(15) 0.0276(13) 0.0227(15) 0.0107(11) 0.0092(12) 0.0077(11) C1 0.022(2) 0.0197(16) 0.026(2) 0.0076(14) -0.0017(16) 0.0030(14) C2 0.0234(19) 0.0227(16) 0.0204(18) 0.0091(14) -0.0042(14) 0.0002(14) C3 0.0206(18) 0.0177(15) 0.0163(17) 0.0014(12) -0.0018(13) 0.0060(12) C4 0.0153(17) 0.0214(16) 0.0178(17) -0.0026(13) 0.0000(13) 0.0025(12) C5 0.021(2) 0.031(2) 0.045(3) 0.0186(19) -0.0041(18) 0.0075(15) C6 0.048(3) 0.035(2) 0.034(2) 0.0208(19) 0.002(2) 0.0041(19) C7 0.035(2) 0.0206(16) 0.0232(19) 0.0041(14) 0.0024(16) 0.0089(15) C9 0.028(2) 0.033(2) 0.032(2) 0.0149(17) 0.0116(17) 0.0022(16) C10 0.029(2) 0.035(2) 0.026(2) 0.0108(16) 0.0142(17) 0.0028(16) O3 0.0241(16) 0.0280(14) 0.0219(15) 0.0036(11) 0.0020(12) 0.0004(11) C8 0.0181(17) 0.0190(16) 0.032(2) -0.0002(14) 0.0014(14) 0.0058(13) N6 0.033(2) 0.0232(15) 0.0212(17) -0.0016(12) 0.0009(14) 0.0076(13) C13 0.043(3) 0.0286(19) 0.0171(19) -0.0012(15) 0.0003(17) -0.0100(17) C16 0.049(3) 0.0262(18) 0.0156(18) 0.0053(14) 0.0055(17) -0.0043(17) C17 0.028(2) 0.041(2) 0.0226(19) 0.0024(16) 0.0012(15) -0.0120(17) C18 0.058(3) 0.0207(17) 0.031(2) 0.0044(15) 0.002(2) 0.0102(18) N11 0.0154(16) 0.0203(14) 0.0159(16) 0.0027(11) 0.0001(12) 0.0021(11) C22 0.020(2) 0.0230(17) 0.0205(18) 0.0093(14) -0.0052(14) 0.0001(14) C23 0.030(2) 0.0213(16) 0.0205(18) 0.0088(14) 0.0041(15) -0.0023(14) C24 0.047(3) 0.0212(17) 0.024(2) 0.0091(15) -0.0041(18) 0.0068(17) C25 0.028(2) 0.0250(18) 0.031(2) -0.0051(15) 0.0033(16) 0.0084(15) C26 0.031(2) 0.0249(18) 0.037(2) 0.0107(16) -0.0034(18) 0.0098(16) C27 0.036(2) 0.040(2) 0.026(2) 0.0215(18) -0.0017(17) -0.0013(18) C28 0.0180(19) 0.044(2) 0.0223(19) 0.0081(16) 0.0087(14) 0.0032(16) C29 0.023(2) 0.045(2) 0.034(2) 0.0128(19) 0.0153(17) 0.0008(17) O8 0.0261(17) 0.0447(18) 0.048(2) 0.0245(15) -0.0034(14) -0.0117(13) N14 0.0274(18) 0.0313(17) 0.0161(16) 0.0066(13) 0.0000(13) 0.0053(13) C31 0.035(2) 0.037(2) 0.0206(17) 0.0101(15) 0.0035(15) -0.0009(16) C32 0.034(2) 0.035(2) 0.0185(17) 0.0020(14) -0.0014(14) 0.0003(16) C34 0.0228(18) 0.0317(19) 0.030(2) -0.0031(15) 0.0031(15) 0.0083(14) C35 0.0189(18) 0.042(2) 0.030(2) 0.0052(17) 0.0059(15) 0.0078(16) C36 0.033(2) 0.050(3) 0.024(2) 0.0070(18) -0.0007(17) -0.018(2) C37 0.029(3) 0.036(2) 0.024(2) 0.0115(17) -0.0022(19) 0.0083(17) O13 0.227(8) 0.139(5) 0.159(6) 0.129(5) 0.160(6) 0.127(6) O14 0.052(3) 0.119(4) 0.049(2) 0.005(3) 0.006(2) -0.014(3) O15 0.114(4) 0.057(3) 0.071(3) -0.003(2) 0.013(3) 0.008(3) O16 0.037(3) 0.370(12) 0.032(2) -0.010(4) 0.0043(19) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn01 O5 2.072(3) . ? Zn01 O6 2.092(3) . ? Zn01 O7 2.149(3) . ? Zn01 N13 2.180(4) . ? Zn01 N15 2.184(3) . ? Zn01 N14 2.186(3) . ? Zn1 O1 2.083(3) . ? Zn1 O2 2.086(3) . ? Zn1 O3 2.148(3) . ? Zn1 N5 2.179(4) . ? Zn1 N6 2.185(3) . ? Zn1 N7 2.194(3) . ? Ni03 N12 1.840(3) . ? Ni03 N10 1.843(3) . ? Ni03 N9 1.900(3) . ? Ni03 N11 1.908(3) . ? Ni03 N16 2.160(4) . ? Ni1 N2 1.846(3) . ? Ni1 N4 1.848(3) . ? Ni1 N1 1.883(3) . ? Ni1 N3 1.888(3) . ? Ni1 N8 2.209(4) . ? Cl1 O12 1.426(3) . ? Cl1 O10 1.430(3) . ? Cl1 O9 1.438(4) . ? Cl1 O11 1.441(4) . ? Cl06 O13 1.377(5) . ? Cl06 O16 1.382(5) . ? Cl06 O14 1.400(5) . ? Cl06 O15 1.464(5) . ? O6 N11 1.303(4) . ? N1 C1 1.319(5) . ? N1 O1 1.328(4) . ? O2 N3 1.319(4) . ? O7 N16 1.290(5) . ? N7 C19 1.468(6) . ? N7 C14 1.493(5) . ? N7 C15 1.513(5) . ? N15 C34 1.460(5) . ? N15 C38 1.489(5) . ? N15 C33 1.499(6) . ? N5 C11 1.472(5) . ? N5 C16 1.482(5) . ? N5 C17 1.500(6) . ? C20 N9 1.321(5) . ? C20 C21 1.452(6) . ? C20 C24 1.504(5) . ? O4 N8 1.237(5) . ? O5 N9 1.306(4) . ? C21 N10 1.310(5) . ? C21 C25 1.506(6) . ? N10 C28 1.457(5) . ? C30 N13 1.477(6) . ? C30 C31 1.554(6) . ? N3 C3 1.328(5) . ? C15 C16 1.474(7) . ? C33 C32 1.473(6) . ? N12 C23 1.276(5) . ? N12 C29 1.494(6) . ? C14 C13 1.538(6) . ? N8 O3 1.265(5) . ? N16 O8 1.232(5) . ? N13 C36 1.437(6) . ? N13 C35 1.513(6) . ? C12 C11 1.503(6) . ? C12 N6 1.508(6) . ? N2 C2 1.309(5) . ? N2 C9 1.461(6) . ? N4 C4 1.284(5) . ? N4 C10 1.489(5) . ? C1 C2 1.449(6) . ? C1 C5 1.502(6) . ? C2 C6 1.500(6) . ? C3 C4 1.456(5) . ? C3 C7 1.498(5) . ? C4 C8 1.506(5) . ? C9 C10 1.541(6) . ? N6 C18 1.474(5) . ? N6 C13 1.478(6) . ? N11 C22 1.312(5) . ? C22 C26 1.481(6) . ? C22 C23 1.493(6) . ? C23 C27 1.509(5) . ? C28 C29 1.508(6) . ? N14 C31 1.462(5) . ? N14 C37 1.474(6) . ? N14 C32 1.519(5) . ? C34 C35 1.511(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn01 O6 92.57(12) . . ? O5 Zn01 O7 95.35(12) . . ? O6 Zn01 O7 94.90(12) . . ? O5 Zn01 N13 91.31(13) . . ? O6 Zn01 N13 93.99(13) . . ? O7 Zn01 N13 168.64(14) . . ? O5 Zn01 N15 172.65(12) . . ? O6 Zn01 N15 92.16(12) . . ? O7 Zn01 N15 89.84(13) . . ? N13 Zn01 N15 82.76(14) . . ? O5 Zn01 N14 92.62(13) . . ? O6 Zn01 N14 174.01(13) . . ? O7 Zn01 N14 87.60(13) . . ? N13 Zn01 N14 82.91(14) . . ? N15 Zn01 N14 82.38(13) . . ? O1 Zn1 O2 93.29(12) . . ? O1 Zn1 O3 94.53(12) . . ? O2 Zn1 O3 94.93(12) . . ? O1 Zn1 N5 91.81(13) . . ? O2 Zn1 N5 92.38(12) . . ? O3 Zn1 N5 170.03(13) . . ? O1 Zn1 N6 93.88(13) . . ? O2 Zn1 N6 170.61(12) . . ? O3 Zn1 N6 90.54(13) . . ? N5 Zn1 N6 81.35(14) . . ? O1 Zn1 N7 172.75(14) . . ? O2 Zn1 N7 89.69(12) . . ? O3 Zn1 N7 91.80(13) . . ? N5 Zn1 N7 81.46(14) . . ? N6 Zn1 N7 82.50(13) . . ? N12 Ni03 N10 85.79(15) . . ? N12 Ni03 N9 163.20(16) . . ? N10 Ni03 N9 82.92(15) . . ? N12 Ni03 N11 82.54(15) . . ? N10 Ni03 N11 159.45(15) . . ? N9 Ni03 N11 104.26(14) . . ? N12 Ni03 N16 103.59(14) . . ? N10 Ni03 N16 109.99(15) . . ? N9 Ni03 N16 91.97(13) . . ? N11 Ni03 N16 89.23(14) . . ? N2 Ni1 N4 85.20(15) . . ? N2 Ni1 N1 82.92(15) . . ? N4 Ni1 N1 160.19(16) . . ? N2 Ni1 N3 162.49(15) . . ? N4 Ni1 N3 82.61(14) . . ? N1 Ni1 N3 104.98(14) . . ? N2 Ni1 N8 104.20(14) . . ? N4 Ni1 N8 112.04(15) . . ? N1 Ni1 N8 86.30(14) . . ? N3 Ni1 N8 92.03(13) . . ? O12 Cl1 O10 110.7(2) . . ? O12 Cl1 O9 108.7(2) . . ? O10 Cl1 O9 111.8(2) . . ? O12 Cl1 O11 108.2(2) . . ? O10 Cl1 O11 108.9(2) . . ? O9 Cl1 O11 108.4(3) . . ? O13 Cl06 O16 112.5(5) . . ? O13 Cl06 O14 112.1(5) . . ? O16 Cl06 O14 108.0(3) . . ? O13 Cl06 O15 105.0(3) . . ? O16 Cl06 O15 112.8(5) . . ? O14 Cl06 O15 106.3(3) . . ? N11 O6 Zn01 116.3(2) . . ? C1 N1 O1 118.8(3) . . ? C1 N1 Ni1 114.8(3) . . ? O1 N1 Ni1 126.4(2) . . ? N3 O2 Zn1 117.2(2) . . ? N16 O7 Zn01 120.6(3) . . ? C19 N7 C14 112.5(4) . . ? C19 N7 C15 109.9(3) . . ? C14 N7 C15 111.0(3) . . ? C19 N7 Zn1 112.7(3) . . ? C14 N7 Zn1 108.7(2) . . ? C15 N7 Zn1 101.4(2) . . ? C34 N15 C38 110.0(3) . . ? C34 N15 C33 114.8(3) . . ? C38 N15 C33 109.9(3) . . ? C34 N15 Zn01 102.2(2) . . ? C38 N15 Zn01 112.0(3) . . ? C33 N15 Zn01 107.7(3) . . ? C11 N5 C16 114.4(3) . . ? C11 N5 C17 108.9(3) . . ? C16 N5 C17 109.5(3) . . ? C11 N5 Zn1 103.4(2) . . ? C16 N5 Zn1 109.7(3) . . ? C17 N5 Zn1 110.9(2) . . ? N9 C20 C21 112.6(3) . . ? N9 C20 C24 122.7(4) . . ? C21 C20 C24 124.8(4) . . ? N9 O5 Zn01 116.6(2) . . ? N10 C21 C20 113.3(3) . . ? N10 C21 C25 124.2(4) . . ? C20 C21 C25 122.5(3) . . ? C21 N10 C28 126.2(4) . . ? C21 N10 Ni03 116.5(3) . . ? C28 N10 Ni03 116.7(3) . . ? N13 C30 C31 112.3(3) . . ? O2 N3 C3 118.5(3) . . ? O2 N3 Ni1 126.3(2) . . ? C3 N3 Ni1 114.9(3) . . ? O5 N9 C20 119.7(3) . . ? O5 N9 Ni03 125.7(2) . . ? C20 N9 Ni03 114.5(3) . . ? C16 C15 N7 112.6(3) . . ? C32 C33 N15 114.0(4) . . ? C23 N12 C29 129.2(4) . . ? C23 N12 Ni03 118.0(3) . . ? C29 N12 Ni03 112.9(3) . . ? N7 C14 C13 111.3(3) . . ? O4 N8 O3 117.1(4) . . ? O4 N8 Ni1 123.2(3) . . ? O3 N8 Ni1 119.7(3) . . ? O8 N16 O7 115.6(4) . . ? O8 N16 Ni03 125.7(3) . . ? O7 N16 Ni03 118.6(3) . . ? C36 N13 C30 110.9(3) . . ? C36 N13 C35 112.8(4) . . ? C30 N13 C35 111.2(3) . . ? C36 N13 Zn01 112.4(3) . . ? C30 N13 Zn01 102.3(3) . . ? C35 N13 Zn01 106.6(2) . . ? C11 C12 N6 112.2(3) . . ? N5 C11 C12 110.9(3) . . ? C2 N2 C9 127.8(3) . . ? C2 N2 Ni1 116.5(3) . . ? C9 N2 Ni1 115.6(3) . . ? C4 N4 C10 125.2(3) . . ? C4 N4 Ni1 116.8(3) . . ? C10 N4 Ni1 117.2(3) . . ? N1 O1 Zn1 115.6(2) . . ? N1 C1 C2 112.8(3) . . ? N1 C1 C5 122.5(4) . . ? C2 C1 C5 124.7(3) . . ? N2 C2 C1 112.8(3) . . ? N2 C2 C6 125.6(4) . . ? C1 C2 C6 121.6(4) . . ? N3 C3 C4 111.6(3) . . ? N3 C3 C7 121.9(4) . . ? C4 C3 C7 126.4(3) . . ? N4 C4 C3 113.8(3) . . ? N4 C4 C8 122.7(4) . . ? C3 C4 C8 123.4(3) . . ? N2 C9 C10 108.2(3) . . ? N4 C10 C9 107.2(3) . . ? N8 O3 Zn1 120.2(3) . . ? C18 N6 C13 111.0(3) . . ? C18 N6 C12 110.8(3) . . ? C13 N6 C12 111.8(3) . . ? C18 N6 Zn1 111.9(3) . . ? C13 N6 Zn1 102.7(3) . . ? C12 N6 Zn1 108.3(2) . . ? N6 C13 C14 112.6(3) . . ? C15 C16 N5 112.0(4) . . ? O6 N11 C22 119.3(3) . . ? O6 N11 Ni03 125.8(2) . . ? C22 N11 Ni03 114.8(3) . . ? N11 C22 C26 122.5(4) . . ? N11 C22 C23 111.7(3) . . ? C26 C22 C23 125.8(3) . . ? N12 C23 C22 112.8(3) . . ? N12 C23 C27 125.8(4) . . ? C22 C23 C27 121.3(4) . . ? N10 C28 C29 108.4(3) . . ? N12 C29 C28 108.1(3) . . ? C31 N14 C37 112.2(3) . . ? C31 N14 C32 112.9(3) . . ? C37 N14 C32 107.6(3) . . ? C31 N14 Zn01 108.8(3) . . ? C37 N14 Zn01 113.0(3) . . ? C32 N14 Zn01 102.0(2) . . ? N14 C31 C30 112.4(3) . . ? C33 C32 N14 111.5(3) . . ? N15 C34 C35 111.0(3) . . ? C34 C35 N13 112.2(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.119 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.112 data_complex10 _database_code_depnum_ccdc_archive 'CCDC 895617' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(TMFdoen)Zn(Me3TACN)(MeCN)](ClO4)(BPh4)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H150 B2 Cl2 N18 Ni2 O16 Zn2' _chemical_formula_weight 2321.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7327(7) _cell_length_b 15.5512(9) _cell_length_c 17.9328(10) _cell_angle_alpha 67.784(3) _cell_angle_beta 71.146(3) _cell_angle_gamma 77.960(3) _cell_volume 2852.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9369 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 37.89 _exptl_crystal_description blade _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7365 _exptl_absorpt_correction_T_max 0.9116 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 342149 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 45.86 _reflns_number_total 48552 _reflns_number_gt 30734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 48552 _refine_ls_number_parameters 753 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.121836(7) 0.655771(5) 0.230202(5) 0.01093(2) Uani 1 1 d . A . Ni1 Ni 0.076173(7) 0.875157(5) 0.284752(5) 0.01016(2) Uani 1 1 d . . . Cl1 Cl 0.862825(17) 0.818014(13) 0.504629(11) 0.02055(3) Uani 1 1 d . . . N4 N -0.02643(5) 0.98540(4) 0.27141(3) 0.01254(9) Uani 1 1 d . . . O3 O 0.35809(5) 0.77485(4) 0.44608(3) 0.01757(9) Uani 1 1 d . . . N1 N 0.17994(5) 0.76499(4) 0.32040(3) 0.01151(8) Uani 1 1 d . . . N2 N 0.14171(5) 0.92484(4) 0.33931(3) 0.01217(9) Uani 1 1 d . . . O1 O 0.19377(5) 0.68468(3) 0.30865(3) 0.01581(9) Uani 1 1 d . . . N3 N -0.01969(5) 0.83966(4) 0.23483(3) 0.01201(9) Uani 1 1 d . . . C1 C 0.23755(6) 0.77481(4) 0.36756(4) 0.01203(10) Uani 1 1 d . . . C6 C 0.28418(6) 0.86380(5) 0.43586(4) 0.01360(10) Uani 1 1 d . . . C2 C 0.21495(6) 0.86512(4) 0.37772(4) 0.01175(9) Uani 1 1 d . . . C3 C -0.11080(6) 0.90280(4) 0.22267(4) 0.01429(10) Uani 1 1 d . . . C4 C -0.11473(6) 0.98296(4) 0.24511(4) 0.01396(10) Uani 1 1 d . . . C17 C 0.10441(6) 1.02274(4) 0.33386(4) 0.01464(11) Uani 1 1 d . . . H17A H 0.1682 1.0625 0.2925 0.018 Uiso 1 1 calc R . . H17B H 0.0913 1.0294 0.3889 0.018 Uiso 1 1 calc R . . C44 C 0.69871(6) 0.87125(5) 0.87052(4) 0.01435(10) Uani 1 1 d . . . C38 C 0.60859(6) 0.72388(5) 0.86720(4) 0.01556(11) Uani 1 1 d . . . O2 O -0.01412(5) 0.76287(3) 0.21915(3) 0.01626(9) Uani 1 1 d . . . N5 N 0.00178(6) 0.56135(4) 0.33434(4) 0.01995(11) Uani 1 1 d . . . C49 C 0.60825(6) 0.93470(5) 0.83773(4) 0.01610(11) Uani 1 1 d . . . H49 H 0.5535 0.9123 0.8218 0.019 Uiso 1 1 calc R . . N7 N 0.05403(6) 0.60159(4) 0.15740(4) 0.01900(11) Uani 1 1 d . . . C43 C 0.59485(6) 0.76047(5) 0.78519(5) 0.01775(12) Uani 1 1 d . . . H43 H 0.6424 0.8088 0.7449 0.021 Uiso 1 1 calc R . . O4 O -0.28168(5) 0.99881(4) 0.19730(4) 0.02371(11) Uani 1 1 d . . . C39 C 0.53067(7) 0.65547(5) 0.92351(5) 0.01928(12) Uani 1 1 d . . . H39 H 0.5342 0.6293 0.9800 0.023 Uiso 1 1 calc R . . C55 C 0.63124(6) 0.75782(5) 1.05147(4) 0.01700(11) Uani 1 1 d . . . H55 H 0.6069 0.8225 1.0296 0.020 Uiso 1 1 calc R . . C28 C 0.29515(7) 0.79229(5) 0.05654(5) 0.01925(12) Uani 1 1 d . A . C50 C 0.68981(6) 0.70908(5) 0.99545(4) 0.01577(11) Uani 1 1 d . . . C5 C 0.31982(6) 0.71078(5) 0.41889(4) 0.01386(10) Uani 1 1 d . . . C37 C 0.88376(6) 0.73258(4) 0.75876(4) 0.01555(11) Uani 1 1 d . . . H37 H 0.8233 0.7524 0.7294 0.019 Uiso 1 1 calc R . . C45 C 0.77831(7) 0.91056(5) 0.89002(4) 0.01703(11) Uani 1 1 d . . . H45 H 0.8427 0.8710 0.9107 0.020 Uiso 1 1 calc R . . C47 C 0.67422(7) 1.06525(5) 0.84928(4) 0.01974(13) Uani 1 1 d . . . H47 H 0.6651 1.1295 0.8431 0.024 Uiso 1 1 calc R . . C52 C 0.70041(7) 0.57027(5) 1.11918(5) 0.02185(14) Uani 1 1 d . . . H52 H 0.7252 0.5057 1.1415 0.026 Uiso 1 1 calc R . . C10 C 0.43370(7) 0.66880(6) 0.36949(5) 0.02163(14) Uani 1 1 d . . . H10A H 0.4758 0.7188 0.3220 0.032 Uiso 1 1 calc R . . H10B H 0.4119 0.6262 0.3488 0.032 Uiso 1 1 calc R . . H10C H 0.4870 0.6343 0.4057 0.032 Uiso 1 1 calc R . . C35 C 1.09327(7) 0.68091(5) 0.75657(5) 0.02259(14) Uani 1 1 d . . . H35 H 1.1741 0.6658 0.7278 0.027 Uiso 1 1 calc R . . C18 C -0.01325(7) 1.05267(5) 0.30698(5) 0.01885(12) Uani 1 1 d . . . H18D H -0.0830 1.0538 0.3558 0.023 Uiso 1 1 calc R . . H18E H -0.0106 1.1161 0.2647 0.023 Uiso 1 1 calc R . . C32 C 0.84957(6) 0.72581(5) 0.84339(4) 0.01465(11) Uani 1 1 d . . . C51 C 0.72280(7) 0.61370(5) 1.03316(5) 0.02066(13) Uani 1 1 d . . . H51 H 0.7623 0.5772 0.9981 0.025 Uiso 1 1 calc R . . C12 C 0.36914(7) 0.94016(5) 0.39942(5) 0.02096(13) Uani 1 1 d . . . H12F H 0.4192 0.9296 0.4371 0.031 Uiso 1 1 calc R . . H12G H 0.3216 1.0011 0.3931 0.031 Uiso 1 1 calc R . . H12H H 0.4214 0.9390 0.3446 0.031 Uiso 1 1 calc R . . C33 C 0.94470(7) 0.69572(5) 0.88158(5) 0.01958(12) Uani 1 1 d . . . H33 H 0.9274 0.6907 0.9385 0.023 Uiso 1 1 calc R . . C46 C 0.76700(7) 1.00497(5) 0.88030(4) 0.01896(12) Uani 1 1 d . . . H46 H 0.8225 1.0282 0.8948 0.023 Uiso 1 1 calc R . . C8 C -0.23036(7) 1.04433(5) 0.23447(5) 0.02048(13) Uani 1 1 d . . . C48 C 0.59578(7) 1.02956(5) 0.82770(4) 0.01890(12) Uani 1 1 d . . . H48 H 0.5327 1.0699 0.8058 0.023 Uiso 1 1 calc R . . C42 C 0.51478(7) 0.72883(6) 0.76073(5) 0.02191(14) Uani 1 1 d . . . H42 H 0.5106 0.7543 0.7044 0.026 Uiso 1 1 calc R . . C40 C 0.44862(7) 0.62439(5) 0.90013(5) 0.02351(15) Uani 1 1 d . . . H40 H 0.3976 0.5784 0.9406 0.028 Uiso 1 1 calc R . . C29 C 0.36620(7) 0.85446(5) -0.01944(5) 0.02118(13) Uani 1 1 d . . . H29A H 0.4000 0.8973 -0.0056 0.032 Uiso 1 1 calc R . . H29B H 0.3145 0.8903 -0.0565 0.032 Uiso 1 1 calc R . . H29C H 0.4323 0.8178 -0.0476 0.032 Uiso 1 1 calc R . . C7 C -0.22336(7) 0.90569(5) 0.19909(5) 0.01971(13) Uani 1 1 d . . . C53 C 0.64195(7) 0.62090(6) 1.17266(5) 0.02201(14) Uani 1 1 d . . . H53 H 0.6260 0.5917 1.2316 0.026 Uiso 1 1 calc R . . C41 C 0.44099(7) 0.66014(6) 0.81838(6) 0.02433(15) Uani 1 1 d . . . H41 H 0.3864 0.6382 0.8020 0.029 Uiso 1 1 calc R . . C36 C 1.00230(7) 0.71153(5) 0.71609(5) 0.01899(13) Uani 1 1 d . . . H36 H 1.0210 0.7182 0.6586 0.023 Uiso 1 1 calc R . . C11 C 0.19760(7) 0.86501(6) 0.51991(4) 0.02083(13) Uani 1 1 d . . . H11A H 0.1369 0.8214 0.5378 0.031 Uiso 1 1 calc R . . H11B H 0.1572 0.9281 0.5143 0.031 Uiso 1 1 calc R . . H11C H 0.2431 0.8463 0.5617 0.031 Uiso 1 1 calc R . . N8 N 0.24007(7) 0.74277(5) 0.11712(4) 0.02601(14) Uani 1 1 d . . . C9 C 0.25125(7) 0.63567(5) 0.49406(5) 0.02189(14) Uani 1 1 d . . . H9D H 0.3038 0.6005 0.5307 0.033 Uiso 1 1 calc R . . H9E H 0.2266 0.5932 0.4747 0.033 Uiso 1 1 calc R . . H9F H 0.1793 0.6651 0.5251 0.033 Uiso 1 1 calc R . . C34 C 1.06315(7) 0.67284(6) 0.84019(5) 0.02292(14) Uani 1 1 d . . . H34 H 1.1238 0.6516 0.8694 0.028 Uiso 1 1 calc R . . C54 C 0.60739(7) 0.71502(6) 1.13800(4) 0.02135(13) Uani 1 1 d . . . H54 H 0.5670 0.7508 1.1735 0.026 Uiso 1 1 calc R . . N6 N 0.24391(6) 0.53039(5) 0.23786(5) 0.02531(14) Uani 1 1 d . . . C14 C -0.20158(9) 0.90128(6) 0.11259(6) 0.02986(18) Uani 1 1 d . . . H14G H -0.2785 0.9158 0.0978 0.045 Uiso 1 1 calc R . . H14H H -0.1667 0.8384 0.1121 0.045 Uiso 1 1 calc R . . H14I H -0.1455 0.9468 0.0719 0.045 Uiso 1 1 calc R . . B1 B 0.71062(7) 0.75689(5) 0.89350(5) 0.01462(12) Uani 1 1 d . . . O5 O 0.90185(7) 0.90422(5) 0.49454(5) 0.04166(18) Uani 1 1 d . . . O6 O 0.76875(7) 0.79051(7) 0.57994(4) 0.0521(2) Uani 1 1 d . . . O7 O 0.82174(7) 0.82799(6) 0.43439(4) 0.04075(17) Uani 1 1 d . . . O8 O 0.96461(7) 0.74791(5) 0.50879(5) 0.04332(18) Uani 1 1 d . . . C13 C -0.30392(7) 0.83199(6) 0.26665(6) 0.02830(17) Uani 1 1 d . . . H13A H -0.3125 0.8354 0.3217 0.042 Uiso 1 1 calc R . . H13B H -0.2670 0.7698 0.2651 0.042 Uiso 1 1 calc R . . H13C H -0.3838 0.8434 0.2565 0.042 Uiso 1 1 calc R . . C15 C -0.31757(8) 1.04543(7) 0.31862(6) 0.0329(2) Uani 1 1 d . . . H15A H -0.3977 1.0733 0.3109 0.049 Uiso 1 1 calc R . . H15B H -0.2875 1.0823 0.3409 0.049 Uiso 1 1 calc R . . H15C H -0.3233 0.9814 0.3580 0.049 Uiso 1 1 calc R . . C16 C -0.20724(9) 1.14187(6) 0.17299(7) 0.0321(2) Uani 1 1 d . . . H16A H -0.1497 1.1377 0.1206 0.048 Uiso 1 1 calc R . . H16B H -0.1735 1.1748 0.1968 0.048 Uiso 1 1 calc R . . H16C H -0.2835 1.1761 0.1619 0.048 Uiso 1 1 calc R . . C19 C 0.0726(2) 0.46944(14) 0.35986(14) 0.0243(4) Uani 0.4432(18) 1 d P A 1 H19A H 0.0548 0.4275 0.3359 0.029 Uiso 0.4432(18) 1 calc PR A 1 H19B H 0.0476 0.4410 0.4216 0.029 Uiso 0.4432(18) 1 calc PR A 1 C20 C 0.20734(18) 0.47804(12) 0.33091(13) 0.0239(4) Uani 0.4432(18) 1 d P A 1 H20A H 0.2277 0.5118 0.3612 0.029 Uiso 0.4432(18) 1 calc PR A 1 H20B H 0.2522 0.4151 0.3433 0.029 Uiso 0.4432(18) 1 calc PR A 1 C21 C 0.2365(3) 0.4830(2) 0.1875(2) 0.0270(6) Uani 0.4432(18) 1 d P A 1 H21A H 0.1895 0.4287 0.2225 0.032 Uiso 0.4432(18) 1 calc PR A 1 H21B H 0.3189 0.4594 0.1611 0.032 Uiso 0.4432(18) 1 calc PR A 1 C22 C 0.1761(2) 0.54691(15) 0.12020(13) 0.0262(4) Uani 0.4432(18) 1 d P A 1 H22A H 0.1584 0.5094 0.0920 0.031 Uiso 0.4432(18) 1 calc PR A 1 H22B H 0.2324 0.5924 0.0778 0.031 Uiso 0.4432(18) 1 calc PR A 1 C23 C -0.03110(16) 0.53640(12) 0.21107(11) 0.0201(3) Uani 0.4432(18) 1 d P A 1 H23A H 0.0101 0.4722 0.2228 0.024 Uiso 0.4432(18) 1 calc PR A 1 H23B H -0.0940 0.5410 0.1836 0.024 Uiso 0.4432(18) 1 calc PR A 1 C24 C -0.0890(2) 0.55668(16) 0.29189(17) 0.0218(4) Uani 0.4432(18) 1 d P A 1 H24A H -0.1425 0.5075 0.3309 0.026 Uiso 0.4432(18) 1 calc PR A 1 H24B H -0.1402 0.6169 0.2803 0.026 Uiso 0.4432(18) 1 calc PR A 1 C19A C 0.0902(2) 0.48919(12) 0.37482(11) 0.0358(5) Uani 0.5568(18) 1 d P A 2 H19C H 0.0466 0.4373 0.4201 0.043 Uiso 0.5568(18) 1 calc PR A 2 H19D H 0.1298 0.5172 0.4001 0.043 Uiso 0.5568(18) 1 calc PR A 2 C20A C 0.18534(18) 0.45161(10) 0.31170(12) 0.0346(4) Uani 0.5568(18) 1 d P A 2 H20C H 0.2476 0.4092 0.3382 0.041 Uiso 0.5568(18) 1 calc PR A 2 H20D H 0.1476 0.4153 0.2926 0.041 Uiso 0.5568(18) 1 calc PR A 2 C21A C 0.2471(2) 0.51180(17) 0.15773(16) 0.0289(5) Uani 0.5568(18) 1 d P A 2 H21C H 0.2942 0.5582 0.1081 0.035 Uiso 0.5568(18) 1 calc PR A 2 H21D H 0.2894 0.4491 0.1599 0.035 Uiso 0.5568(18) 1 calc PR A 2 C22A C 0.12271(14) 0.51708(10) 0.14773(9) 0.0194(3) Uani 0.5568(18) 1 d P A 2 H22C H 0.1298 0.5156 0.0917 0.023 Uiso 0.5568(18) 1 calc PR A 2 H22D H 0.0810 0.4627 0.1903 0.023 Uiso 0.5568(18) 1 calc PR A 2 C23A C -0.07534(12) 0.58149(10) 0.21644(9) 0.0207(3) Uani 0.5568(18) 1 d P A 2 H23C H -0.1252 0.6414 0.2161 0.025 Uiso 0.5568(18) 1 calc PR A 2 H23D H -0.1139 0.5480 0.1952 0.025 Uiso 0.5568(18) 1 calc PR A 2 C24A C -0.0719(2) 0.52341(14) 0.30525(13) 0.0245(4) Uani 0.5568(18) 1 d P A 2 H24C H -0.1553 0.5214 0.3426 0.029 Uiso 0.5568(18) 1 calc PR A 2 H24D H -0.0386 0.4587 0.3078 0.029 Uiso 0.5568(18) 1 calc PR A 2 C25 C -0.06568(10) 0.60408(7) 0.39812(5) 0.0371(2) Uani 1 1 d . A . H25A H -0.1174 0.6591 0.3741 0.056 Uiso 1 1 calc R . . H25B H -0.0087 0.6228 0.4176 0.056 Uiso 1 1 calc R . . H25C H -0.1160 0.5589 0.4454 0.056 Uiso 1 1 calc R . . C26 C 0.36909(9) 0.54654(8) 0.22583(9) 0.0486(3) Uani 1 1 d . A . H26A H 0.3710 0.5704 0.2687 0.073 Uiso 1 1 calc R . . H26B H 0.3982 0.5923 0.1703 0.073 Uiso 1 1 calc R . . H26C H 0.4212 0.4877 0.2305 0.073 Uiso 1 1 calc R . . C27 C 0.02683(10) 0.67053(6) 0.08172(5) 0.0333(2) Uani 1 1 d . A . H27A H -0.0074 0.6405 0.0557 0.050 Uiso 1 1 calc R . . H27B H 0.1014 0.6968 0.0425 0.050 Uiso 1 1 calc R . . H27C H -0.0318 0.7206 0.0962 0.050 Uiso 1 1 calc R . . C30 C 0.49538(11) 0.63329(9) 0.59449(7) 0.0452(3) Uani 1 1 d . . . C31 C 0.58554(10) 0.69275(9) 0.53168(7) 0.0464(3) Uani 1 1 d . . . H31A H 0.5484 0.7403 0.4897 0.070 Uiso 1 1 calc R . . H31B H 0.6513 0.6550 0.5046 0.070 Uiso 1 1 calc R . . H31C H 0.6180 0.7233 0.5582 0.070 Uiso 1 1 calc R . . N9 N 0.42368(13) 0.58761(10) 0.64421(8) 0.0729(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01331(3) 0.00887(3) 0.01225(3) -0.00519(2) -0.00355(2) -0.00119(2) Ni1 0.01217(3) 0.00891(3) 0.01144(3) -0.00518(3) -0.00391(2) -0.00074(2) Cl1 0.02374(8) 0.02073(8) 0.01558(7) -0.00459(6) -0.00193(6) -0.00715(6) N4 0.0152(2) 0.0100(2) 0.0140(2) -0.00567(17) -0.00404(17) -0.00150(17) O3 0.0211(2) 0.0165(2) 0.0223(2) -0.00984(19) -0.01254(19) 0.00021(18) N1 0.0135(2) 0.0103(2) 0.0130(2) -0.00577(17) -0.00396(17) -0.00182(17) N2 0.0144(2) 0.0112(2) 0.0124(2) -0.00564(17) -0.00276(17) -0.00267(17) O1 0.0204(2) 0.01094(19) 0.0224(2) -0.00980(17) -0.01078(18) 0.00123(16) N3 0.0154(2) 0.0088(2) 0.0137(2) -0.00496(17) -0.00529(17) -0.00076(17) C1 0.0137(2) 0.0121(2) 0.0117(2) -0.00463(19) -0.00353(18) -0.00284(19) C6 0.0165(3) 0.0141(3) 0.0131(2) -0.0061(2) -0.0048(2) -0.0032(2) C2 0.0132(2) 0.0129(2) 0.0106(2) -0.00553(19) -0.00172(18) -0.00376(19) C3 0.0164(3) 0.0110(2) 0.0189(3) -0.0065(2) -0.0086(2) 0.0004(2) C4 0.0161(3) 0.0100(2) 0.0172(3) -0.0057(2) -0.0062(2) 0.0007(2) C17 0.0190(3) 0.0110(2) 0.0167(3) -0.0063(2) -0.0056(2) -0.0028(2) C44 0.0172(3) 0.0140(3) 0.0114(2) -0.0054(2) -0.0008(2) -0.0032(2) C38 0.0173(3) 0.0134(3) 0.0171(3) -0.0086(2) -0.0025(2) -0.0006(2) O2 0.0216(2) 0.01040(19) 0.0234(2) -0.00983(18) -0.01198(19) 0.00200(16) N5 0.0286(3) 0.0160(3) 0.0152(2) -0.0033(2) -0.0043(2) -0.0085(2) C49 0.0179(3) 0.0152(3) 0.0143(3) -0.0051(2) -0.0020(2) -0.0032(2) N7 0.0310(3) 0.0137(2) 0.0175(2) -0.0058(2) -0.0127(2) -0.0023(2) C43 0.0190(3) 0.0176(3) 0.0198(3) -0.0098(2) -0.0061(2) -0.0002(2) O4 0.0248(3) 0.0144(2) 0.0424(3) -0.0147(2) -0.0221(2) 0.00692(19) C39 0.0201(3) 0.0164(3) 0.0220(3) -0.0100(3) -0.0016(2) -0.0029(2) C55 0.0212(3) 0.0165(3) 0.0140(3) -0.0063(2) -0.0031(2) -0.0038(2) C28 0.0190(3) 0.0198(3) 0.0195(3) -0.0095(3) -0.0013(2) -0.0036(2) C50 0.0200(3) 0.0145(3) 0.0138(2) -0.0058(2) -0.0034(2) -0.0035(2) C5 0.0157(3) 0.0137(3) 0.0150(2) -0.0057(2) -0.0063(2) -0.0021(2) C37 0.0211(3) 0.0110(3) 0.0145(3) -0.0046(2) -0.0029(2) -0.0040(2) C45 0.0198(3) 0.0168(3) 0.0155(3) -0.0069(2) -0.0033(2) -0.0034(2) C47 0.0288(4) 0.0134(3) 0.0147(3) -0.0048(2) -0.0003(2) -0.0061(3) C52 0.0256(3) 0.0170(3) 0.0205(3) -0.0012(3) -0.0076(3) -0.0047(3) C10 0.0173(3) 0.0262(4) 0.0276(4) -0.0162(3) -0.0085(3) 0.0027(3) C35 0.0192(3) 0.0180(3) 0.0288(4) -0.0115(3) 0.0004(3) -0.0022(2) C18 0.0221(3) 0.0154(3) 0.0268(3) -0.0141(3) -0.0112(3) 0.0026(2) C32 0.0185(3) 0.0120(3) 0.0147(3) -0.0061(2) -0.0038(2) -0.0020(2) C51 0.0274(3) 0.0159(3) 0.0181(3) -0.0062(2) -0.0048(3) -0.0023(3) C12 0.0236(3) 0.0206(3) 0.0229(3) -0.0059(3) -0.0086(3) -0.0095(3) C33 0.0214(3) 0.0205(3) 0.0193(3) -0.0090(3) -0.0071(2) -0.0002(2) C46 0.0240(3) 0.0183(3) 0.0155(3) -0.0078(2) -0.0004(2) -0.0078(3) C8 0.0205(3) 0.0149(3) 0.0332(4) -0.0131(3) -0.0146(3) 0.0047(2) C48 0.0234(3) 0.0148(3) 0.0157(3) -0.0043(2) -0.0032(2) -0.0009(2) C42 0.0225(3) 0.0223(3) 0.0279(4) -0.0150(3) -0.0119(3) 0.0041(3) C40 0.0195(3) 0.0194(3) 0.0342(4) -0.0146(3) -0.0027(3) -0.0038(3) C29 0.0232(3) 0.0184(3) 0.0167(3) -0.0044(2) 0.0000(2) -0.0027(3) C7 0.0211(3) 0.0126(3) 0.0328(4) -0.0104(3) -0.0169(3) 0.0038(2) C53 0.0250(3) 0.0257(4) 0.0142(3) -0.0022(3) -0.0053(2) -0.0089(3) C41 0.0192(3) 0.0229(4) 0.0399(4) -0.0201(3) -0.0108(3) 0.0020(3) C36 0.0234(3) 0.0135(3) 0.0184(3) -0.0075(2) 0.0015(2) -0.0056(2) C11 0.0264(3) 0.0250(3) 0.0129(3) -0.0093(3) -0.0037(2) -0.0030(3) N8 0.0283(3) 0.0266(3) 0.0231(3) -0.0115(3) 0.0030(3) -0.0126(3) C9 0.0267(3) 0.0182(3) 0.0198(3) 0.0003(3) -0.0102(3) -0.0067(3) C34 0.0204(3) 0.0211(3) 0.0291(4) -0.0103(3) -0.0088(3) 0.0012(3) C54 0.0261(3) 0.0248(4) 0.0139(3) -0.0083(3) -0.0021(2) -0.0060(3) N6 0.0217(3) 0.0180(3) 0.0435(4) -0.0177(3) -0.0148(3) 0.0064(2) C14 0.0403(5) 0.0248(4) 0.0372(5) -0.0163(3) -0.0274(4) 0.0086(3) B1 0.0184(3) 0.0132(3) 0.0131(3) -0.0061(2) -0.0031(2) -0.0021(2) O5 0.0459(4) 0.0230(3) 0.0559(5) -0.0201(3) -0.0012(4) -0.0101(3) O6 0.0439(4) 0.0937(7) 0.0202(3) -0.0172(4) 0.0084(3) -0.0405(4) O7 0.0502(4) 0.0519(5) 0.0206(3) -0.0071(3) -0.0159(3) -0.0054(4) O8 0.0486(4) 0.0255(3) 0.0624(5) -0.0176(3) -0.0271(4) 0.0077(3) C13 0.0198(3) 0.0194(3) 0.0483(5) -0.0091(3) -0.0156(3) -0.0012(3) C15 0.0201(4) 0.0413(5) 0.0453(5) -0.0280(4) -0.0102(3) 0.0085(3) C16 0.0400(5) 0.0132(3) 0.0497(5) -0.0070(3) -0.0283(4) 0.0026(3) C19 0.0340(10) 0.0136(8) 0.0251(9) 0.0039(6) -0.0164(8) -0.0086(7) C20 0.0320(9) 0.0115(7) 0.0348(9) -0.0051(6) -0.0232(8) 0.0016(6) C21 0.0254(12) 0.0264(14) 0.0442(17) -0.0266(11) -0.0187(13) 0.0098(10) C22 0.0279(9) 0.0312(10) 0.0310(9) -0.0257(8) -0.0079(8) 0.0025(8) C23 0.0228(8) 0.0145(7) 0.0293(8) -0.0074(6) -0.0138(6) -0.0039(6) C24 0.0196(8) 0.0196(10) 0.0266(10) -0.0018(9) -0.0084(7) -0.0108(8) C19A 0.0791(15) 0.0126(6) 0.0254(7) 0.0018(5) -0.0322(9) -0.0111(8) C20A 0.0590(11) 0.0120(6) 0.0499(10) -0.0108(6) -0.0434(9) 0.0076(6) C21A 0.0215(7) 0.0300(12) 0.0461(14) -0.0310(10) -0.0042(10) 0.0019(9) C22A 0.0240(6) 0.0185(6) 0.0219(6) -0.0137(5) -0.0062(5) -0.0015(5) C23A 0.0169(5) 0.0210(6) 0.0320(7) -0.0153(5) -0.0099(5) -0.0004(5) C24A 0.0305(9) 0.0234(8) 0.0212(8) -0.0097(7) 0.0021(6) -0.0166(8) C25 0.0525(6) 0.0400(5) 0.0185(3) -0.0150(3) 0.0112(4) -0.0271(5) C26 0.0252(4) 0.0521(6) 0.1032(10) -0.0614(7) -0.0350(5) 0.0203(4) C27 0.0628(6) 0.0232(4) 0.0231(4) -0.0067(3) -0.0270(4) -0.0007(4) C30 0.0526(7) 0.0489(6) 0.0422(6) -0.0043(5) -0.0331(5) -0.0104(5) C31 0.0358(5) 0.0657(8) 0.0418(6) -0.0121(5) -0.0193(5) -0.0107(5) N9 0.0851(9) 0.0776(9) 0.0541(7) 0.0189(6) -0.0437(7) -0.0424(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 2.0504(5) . ? Zn1 O1 2.0729(5) . ? Zn1 N6 2.1522(6) . ? Zn1 N5 2.1718(6) . ? Zn1 N8 2.1811(7) . ? Zn1 N7 2.1977(6) . ? Ni1 N2 1.8577(5) . ? Ni1 N4 1.8603(6) . ? Ni1 N1 1.9054(5) . ? Ni1 N3 1.9117(5) . ? Cl1 O6 1.4219(7) . ? Cl1 O7 1.4340(7) . ? Cl1 O5 1.4348(7) . ? Cl1 O8 1.4399(7) . ? N4 C4 1.2817(8) . ? N4 C18 1.4700(8) . ? O3 C6 1.4525(8) . ? O3 C5 1.4587(8) . ? N1 C1 1.3061(8) . ? N1 O1 1.3127(7) . ? N2 C2 1.2811(8) . ? N2 C17 1.4684(8) . ? N3 C3 1.3058(8) . ? N3 O2 1.3111(7) . ? C1 C2 1.4432(9) . ? C1 C5 1.5003(9) . ? C6 C2 1.5072(9) . ? C6 C12 1.5221(10) . ? C6 C11 1.5257(9) . ? C3 C4 1.4357(9) . ? C3 C7 1.4989(9) . ? C4 C8 1.5090(9) . ? C17 C18 1.5321(10) . ? C44 C49 1.4048(10) . ? C44 C45 1.4068(10) . ? C44 B1 1.6528(10) . ? C38 C39 1.4086(10) . ? C38 C43 1.4124(10) . ? C38 B1 1.6500(10) . ? N5 C24A 1.450(2) . ? N5 C25 1.4651(11) . ? N5 C19 1.483(2) . ? N5 C19A 1.500(2) . ? N5 C24 1.522(3) . ? C49 C48 1.3986(10) . ? N7 C23 1.4195(18) . ? N7 C22A 1.4307(14) . ? N7 C27 1.4595(10) . ? N7 C23A 1.5594(16) . ? N7 C22 1.588(2) . ? C43 C42 1.3927(10) . ? O4 C8 1.4498(9) . ? O4 C7 1.4601(8) . ? C39 C40 1.3943(11) . ? C55 C54 1.3947(10) . ? C55 C50 1.4030(9) . ? C28 N8 1.1455(10) . ? C28 C29 1.4464(10) . ? C50 C51 1.4065(10) . ? C50 B1 1.6475(10) . ? C5 C10 1.5181(10) . ? C5 C9 1.5261(10) . ? C37 C36 1.3924(10) . ? C37 C32 1.4066(9) . ? C45 C46 1.3942(10) . ? C47 C48 1.3822(11) . ? C47 C46 1.3944(11) . ? C52 C51 1.3888(10) . ? C52 C53 1.3895(12) . ? C35 C36 1.3857(12) . ? C35 C34 1.3868(12) . ? C32 C33 1.4028(10) . ? C32 B1 1.6589(10) . ? C33 C34 1.3912(11) . ? C8 C16 1.5179(12) . ? C8 C15 1.5292(12) . ? C42 C41 1.3899(12) . ? C40 C41 1.3836(12) . ? C7 C14 1.5143(12) . ? C7 C13 1.5286(12) . ? C53 C54 1.3858(11) . ? N6 C21 1.395(3) . ? N6 C26 1.4747(12) . ? N6 C20A 1.504(2) . ? N6 C20 1.512(2) . ? N6 C21A 1.557(3) . ? C19 C20 1.514(3) . ? C21 C22 1.516(4) . ? C23 C24 1.511(3) . ? C19A C20A 1.510(3) . ? C21A C22A 1.510(3) . ? C23A C24A 1.514(3) . ? C30 N9 1.1372(16) . ? C30 C31 1.4467(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 98.930(19) . . ? O2 Zn1 N6 169.80(2) . . ? O1 Zn1 N6 90.11(2) . . ? O2 Zn1 N5 92.01(2) . . ? O1 Zn1 N5 92.64(2) . . ? N6 Zn1 N5 82.81(3) . . ? O2 Zn1 N8 89.33(3) . . ? O1 Zn1 N8 93.21(2) . . ? N6 Zn1 N8 94.91(3) . . ? N5 Zn1 N8 173.73(2) . . ? O2 Zn1 N7 88.82(2) . . ? O1 Zn1 N7 170.82(2) . . ? N6 Zn1 N7 81.79(3) . . ? N5 Zn1 N7 82.11(2) . . ? N8 Zn1 N7 91.79(3) . . ? N2 Ni1 N4 83.85(2) . . ? N2 Ni1 N1 85.85(2) . . ? N4 Ni1 N1 167.73(2) . . ? N2 Ni1 N3 168.55(2) . . ? N4 Ni1 N3 85.76(2) . . ? N1 Ni1 N3 103.85(2) . . ? O6 Cl1 O7 110.27(5) . . ? O6 Cl1 O5 109.90(5) . . ? O7 Cl1 O5 110.24(5) . . ? O6 Cl1 O8 109.42(6) . . ? O7 Cl1 O8 108.78(5) . . ? O5 Cl1 O8 108.19(5) . . ? C4 N4 C18 128.04(6) . . ? C4 N4 Ni1 112.05(4) . . ? C18 N4 Ni1 118.53(4) . . ? C6 O3 C5 114.29(5) . . ? C1 N1 O1 119.47(5) . . ? C1 N1 Ni1 110.23(4) . . ? O1 N1 Ni1 130.15(4) . . ? C2 N2 C17 129.37(5) . . ? C2 N2 Ni1 112.41(4) . . ? C17 N2 Ni1 118.22(4) . . ? N1 O1 Zn1 126.26(4) . . ? C3 N3 O2 118.42(5) . . ? C3 N3 Ni1 109.90(4) . . ? O2 N3 Ni1 131.36(4) . . ? N1 C1 C2 115.31(6) . . ? N1 C1 C5 134.31(6) . . ? C2 C1 C5 110.29(5) . . ? O3 C6 C2 102.65(5) . . ? O3 C6 C12 107.66(6) . . ? C2 C6 C12 114.14(5) . . ? O3 C6 C11 110.03(5) . . ? C2 C6 C11 110.43(6) . . ? C12 C6 C11 111.49(6) . . ? N2 C2 C1 115.99(5) . . ? N2 C2 C6 135.33(6) . . ? C1 C2 C6 108.65(5) . . ? N3 C3 C4 115.56(6) . . ? N3 C3 C7 133.44(6) . . ? C4 C3 C7 110.54(6) . . ? N4 C4 C3 116.26(6) . . ? N4 C4 C8 134.96(6) . . ? C3 C4 C8 108.72(6) . . ? N2 C17 C18 108.02(5) . . ? C49 C44 C45 115.14(6) . . ? C49 C44 B1 125.30(6) . . ? C45 C44 B1 119.39(6) . . ? C39 C38 C43 114.50(6) . . ? C39 C38 B1 123.13(6) . . ? C43 C38 B1 122.35(6) . . ? N3 O2 Zn1 125.58(4) . . ? C24A N5 C25 115.05(11) . . ? C24A N5 C19 91.24(12) . . ? C25 N5 C19 118.78(11) . . ? C24A N5 C19A 113.21(11) . . ? C25 N5 C19A 103.49(10) . . ? C19 N5 C19A 22.32(8) . . ? C24A N5 C24 19.54(9) . . ? C25 N5 C24 106.49(12) . . ? C19 N5 C24 110.44(13) . . ? C19A N5 C24 132.60(12) . . ? C24A N5 Zn1 111.14(9) . . ? C25 N5 Zn1 111.34(5) . . ? C19 N5 Zn1 107.68(9) . . ? C19A N5 Zn1 101.58(9) . . ? C24 N5 Zn1 100.60(10) . . ? C48 C49 C44 122.46(7) . . ? C23 N7 C22A 79.82(10) . . ? C23 N7 C27 118.26(9) . . ? C22A N7 C27 115.37(8) . . ? C23 N7 C23A 30.63(8) . . ? C22A N7 C23A 110.39(9) . . ? C27 N7 C23A 101.66(8) . . ? C23 N7 C22 108.87(12) . . ? C22A N7 C22 29.13(9) . . ? C27 N7 C22 101.95(10) . . ? C23A N7 C22 139.49(11) . . ? C23 N7 Zn1 110.73(8) . . ? C22A N7 Zn1 112.00(7) . . ? C27 N7 Zn1 115.62(5) . . ? C23A N7 Zn1 99.96(6) . . ? C22 N7 Zn1 98.85(8) . . ? C42 C43 C38 122.97(7) . . ? C8 O4 C7 114.42(5) . . ? C40 C39 C38 123.03(7) . . ? C54 C55 C50 122.60(7) . . ? N8 C28 C29 179.15(9) . . ? C55 C50 C51 114.91(6) . . ? C55 C50 B1 123.18(6) . . ? C51 C50 B1 121.77(6) . . ? O3 C5 C1 101.77(5) . . ? O3 C5 C10 106.75(5) . . ? C1 C5 C10 114.45(6) . . ? O3 C5 C9 110.60(5) . . ? C1 C5 C9 111.16(6) . . ? C10 C5 C9 111.57(6) . . ? C36 C37 C32 122.90(7) . . ? C46 C45 C44 122.99(7) . . ? C48 C47 C46 118.65(7) . . ? C51 C52 C53 120.25(7) . . ? C36 C35 C34 118.20(7) . . ? N4 C18 C17 108.30(5) . . ? C33 C32 C37 114.51(6) . . ? C33 C32 B1 121.88(6) . . ? C37 C32 B1 123.49(6) . . ? C52 C51 C50 123.14(7) . . ? C34 C33 C32 123.24(7) . . ? C45 C46 C47 120.03(7) . . ? O4 C8 C4 102.91(5) . . ? O4 C8 C16 107.56(6) . . ? C4 C8 C16 112.43(7) . . ? O4 C8 C15 109.34(7) . . ? C4 C8 C15 111.69(7) . . ? C16 C8 C15 112.36(7) . . ? C47 C48 C49 120.70(7) . . ? C41 C42 C43 120.33(7) . . ? C41 C40 C39 120.45(7) . . ? O4 C7 C3 101.92(5) . . ? O4 C7 C14 106.98(6) . . ? C3 C7 C14 114.69(7) . . ? O4 C7 C13 109.76(6) . . ? C3 C7 C13 110.64(6) . . ? C14 C7 C13 112.21(7) . . ? C54 C53 C52 118.41(7) . . ? C40 C41 C42 118.67(7) . . ? C35 C36 C37 120.67(7) . . ? C28 N8 Zn1 175.28(7) . . ? C35 C34 C33 120.46(7) . . ? C53 C54 C55 120.69(7) . . ? C21 N6 C26 112.77(15) . . ? C21 N6 C20A 87.05(15) . . ? C26 N6 C20A 120.08(10) . . ? C21 N6 C20 115.16(15) . . ? C26 N6 C20 100.85(10) . . ? C20A N6 C20 28.81(8) . . ? C21 N6 C21A 20.50(12) . . ? C26 N6 C21A 104.92(12) . . ? C20A N6 C21A 107.05(11) . . ? C20 N6 C21A 135.51(12) . . ? C21 N6 Zn1 113.76(13) . . ? C26 N6 Zn1 112.20(5) . . ? C20A N6 Zn1 108.78(8) . . ? C20 N6 Zn1 100.87(8) . . ? C21A N6 Zn1 102.05(10) . . ? C50 B1 C38 108.64(5) . . ? C50 B1 C44 107.42(5) . . ? C38 B1 C44 112.34(6) . . ? C50 B1 C32 110.50(6) . . ? C38 B1 C32 110.84(5) . . ? C44 B1 C32 107.04(5) . . ? N5 C19 C20 111.84(14) . . ? N6 C20 C19 109.53(13) . . ? N6 C21 C22 110.7(2) . . ? C21 C22 N7 111.96(18) . . ? N7 C23 C24 109.39(14) . . ? C23 C24 N5 113.70(18) . . ? N5 C19A C20A 110.86(12) . . ? N6 C20A C19A 110.37(12) . . ? C22A C21A N6 112.99(17) . . ? N7 C22A C21A 109.48(13) . . ? C24A C23A N7 111.69(12) . . ? N5 C24A C23A 111.48(13) . . ? N9 C30 C31 179.02(17) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 45.86 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.840 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.070 data_complex11 _database_code_depnum_ccdc_archive 'CCDC 895618' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(TMFdoen)Zn(Me3TACN)(THF)]BPh4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H178 B2 N14 Ni2 O13 Zn2' _chemical_formula_weight 2318.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9784(8) _cell_length_b 19.7901(14) _cell_length_c 26.2940(18) _cell_angle_alpha 104.912(4) _cell_angle_beta 91.396(4) _cell_angle_gamma 98.300(4) _cell_volume 5947.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9849 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.62 _exptl_crystal_description blade _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2476 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7363 _exptl_absorpt_correction_T_max 0.9405 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 288123 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 35.75 _reflns_number_total 51564 _reflns_number_gt 30294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+3.6073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 51564 _refine_ls_number_parameters 1446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1235 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.23335(2) 0.725934(12) 0.107421(9) 0.01646(5) Uani 1 1 d . . . Zn2 Zn 0.278848(19) 0.214542(11) 0.429608(8) 0.01356(5) Uani 1 1 d . . . Ni1 Ni -0.00902(2) 0.754364(13) 0.191982(9) 0.01329(5) Uani 1 1 d . . . Ni2 Ni 0.26230(2) 0.343664(13) 0.352694(9) 0.01733(5) Uani 1 1 d . . . N12 N 0.10891(15) 0.18651(9) 0.45304(6) 0.0194(3) Uani 1 1 d . . . O4 O 0.08056(13) 0.60763(8) 0.29967(6) 0.0228(3) Uani 1 1 d . . . O8 O 0.17383(14) 0.17469(8) 0.18724(5) 0.0237(3) Uani 1 1 d . . . C32 C 0.21622(17) 0.22399(10) 0.27605(7) 0.0155(3) Uani 1 1 d . . . N14 N 0.32146(14) 0.21591(8) 0.51259(6) 0.0153(3) Uani 1 1 d . . . O9 O 0.26156(15) 0.54384(8) 0.49788(6) 0.0280(4) Uani 1 1 d . . . O1 O 0.11359(12) 0.78574(8) 0.10280(5) 0.0193(3) Uani 1 1 d . . . N8 N 0.23657(14) 0.24397(8) 0.32792(6) 0.0150(3) Uani 1 1 d . . . C59 C 0.4930(2) 0.20971(12) 0.35146(8) 0.0241(4) Uani 1 1 d . . . H59A H 0.4279 0.1796 0.3287 0.029 Uiso 1 1 calc R . . H59B H 0.5533 0.1807 0.3526 0.029 Uiso 1 1 calc R . . N6 N 0.29940(16) 0.75323(10) 0.03508(7) 0.0226(4) Uani 1 1 d . . . C8 C -0.02475(17) 0.63640(10) 0.30181(7) 0.0171(4) Uani 1 1 d . . . C75 C 0.63788(16) 0.51496(10) 0.12039(7) 0.0154(3) Uani 1 1 d . . . N5 N 0.14692(16) 0.63257(10) 0.04789(7) 0.0251(4) Uani 1 1 d . . . C18 C -0.18548(17) 0.73635(10) 0.25998(8) 0.0169(4) Uani 1 1 d . . . H18A H -0.1921 0.7475 0.2986 0.020 Uiso 1 1 calc R . . H18B H -0.2415 0.6941 0.2430 0.020 Uiso 1 1 calc R . . N1 N 0.02954(14) 0.79348(9) 0.13520(6) 0.0156(3) Uani 1 1 d . . . N7 N 0.37396(15) 0.66275(9) 0.09424(7) 0.0197(3) Uani 1 1 d . . . N3 N 0.10544(14) 0.70043(8) 0.19757(6) 0.0151(3) Uani 1 1 d . . . O10 O 0.45886(13) 0.23922(8) 0.40431(6) 0.0220(3) Uani 1 1 d . . . O2 O 0.19868(12) 0.69036(8) 0.17118(5) 0.0195(3) Uani 1 1 d . . . C6 C -0.21287(17) 0.88345(11) 0.14682(8) 0.0187(4) Uani 1 1 d . . . O6 O 0.22566(12) 0.19321(7) 0.35327(5) 0.0169(3) Uani 1 1 d . . . C3 C 0.08825(17) 0.67013(10) 0.23681(7) 0.0159(3) Uani 1 1 d . . . N13 N 0.28165(15) 0.09927(9) 0.42032(6) 0.0186(3) Uani 1 1 d . . . C4 C -0.01164(17) 0.68046(10) 0.26271(7) 0.0163(3) Uani 1 1 d . . . N10 N 0.27007(14) 0.36229(8) 0.42666(6) 0.0162(3) Uani 1 1 d . . . C99 C 0.16556(16) 1.03291(10) 0.64513(7) 0.0154(3) Uani 1 1 d . . . N2 N -0.13333(14) 0.79971(9) 0.19515(6) 0.0161(3) Uani 1 1 d . . . O7 O 0.27626(13) 0.31956(7) 0.45810(5) 0.0182(3) Uani 1 1 d . . . O5 O 0.34351(13) 0.82507(8) 0.16462(6) 0.0236(3) Uani 1 1 d . . . C69 C 0.46000(17) 0.41887(10) 0.12314(7) 0.0163(4) Uani 1 1 d . . . C100 C 0.14168(18) 1.08789(11) 0.62365(7) 0.0188(4) Uani 1 1 d . . . H100 H 0.1923 1.1027 0.5999 0.023 Uiso 1 1 calc R . . N4 N -0.07102(14) 0.72317(8) 0.24711(6) 0.0154(3) Uani 1 1 d . . . C80 C 0.60408(16) 0.51172(10) 0.06815(7) 0.0152(3) Uani 1 1 d . . . H80 H 0.5465 0.4745 0.0499 0.018 Uiso 1 1 calc R . . C39 C 0.25258(18) 0.54638(10) 0.44304(8) 0.0197(4) Uani 1 1 d . . . C33 C 0.22668(17) 0.27943(10) 0.25130(7) 0.0171(4) Uani 1 1 d . . . O3 O -0.16212(14) 0.90318(9) 0.10216(6) 0.0281(4) Uani 1 1 d . . . C78 C 0.73448(18) 0.61600(11) 0.06716(8) 0.0210(4) Uani 1 1 d . . . H78 H 0.7665 0.6498 0.0496 0.025 Uiso 1 1 calc R . . B2 B 0.27752(19) 0.99364(12) 0.62854(8) 0.0154(4) Uani 1 1 d . . . C37 C 0.20945(18) 0.24968(11) 0.19263(7) 0.0194(4) Uani 1 1 d . . . C104 C 0.08689(17) 1.01510(10) 0.68022(7) 0.0173(4) Uani 1 1 d . . . H104 H 0.0979 0.9782 0.6959 0.021 Uiso 1 1 calc R . . C35 C 0.26671(18) 0.47286(10) 0.41364(8) 0.0187(4) Uani 1 1 d . . . C105 C 0.38366(17) 1.05323(10) 0.62252(7) 0.0160(3) Uani 1 1 d . . . C36 C 0.18716(19) 0.15368(10) 0.23594(7) 0.0194(4) Uani 1 1 d . . . C74 C 0.36167(18) 0.44672(10) 0.13869(8) 0.0188(4) Uani 1 1 d . . . H74 H 0.3671 0.4864 0.1685 0.023 Uiso 1 1 calc R . . C2 C -0.13614(17) 0.83595(10) 0.16010(7) 0.0168(4) Uani 1 1 d . . . C17 C -0.20597(17) 0.79912(11) 0.23919(7) 0.0170(4) Uani 1 1 d . . . H17A H -0.2864 0.7939 0.2270 0.020 Uiso 1 1 calc R . . H17B H -0.1867 0.8439 0.2673 0.020 Uiso 1 1 calc R . . B1 B 0.58632(19) 0.45590(12) 0.15109(8) 0.0165(4) Uani 1 1 d . . . C52 C 0.36400(19) 0.09883(11) 0.46321(8) 0.0212(4) Uani 1 1 d . . . H52A H 0.4410 0.1169 0.4549 0.025 Uiso 1 1 calc R . . H52B H 0.3632 0.0496 0.4655 0.025 Uiso 1 1 calc R . . C5 C -0.05933(18) 0.87396(11) 0.08705(8) 0.0206(4) Uani 1 1 d . . . C63 C 0.57734(17) 0.49396(11) 0.21435(7) 0.0189(4) Uani 1 1 d . . . C81 C 0.67204(19) 0.39711(11) 0.14656(8) 0.0210(4) Uani 1 1 d . . . C106 C 0.46216(17) 1.03929(10) 0.58410(7) 0.0172(4) Uani 1 1 d . . . H106 H 0.4514 0.9942 0.5592 0.021 Uiso 1 1 calc R . . C93 C 0.31316(17) 0.95586(10) 0.67409(7) 0.0167(4) Uani 1 1 d . . . C87 C 0.24854(17) 0.93411(11) 0.57128(7) 0.0181(4) Uani 1 1 d . . . C34 C 0.26947(17) 0.43040(10) 0.44880(7) 0.0170(4) Uani 1 1 d . . . C1 C -0.04698(17) 0.83152(10) 0.12601(7) 0.0164(3) Uani 1 1 d . . . C88 C 0.18739(18) 0.94725(12) 0.52957(8) 0.0207(4) Uani 1 1 d . . . H88 H 0.1603 0.9912 0.5352 0.025 Uiso 1 1 calc R . . C7 C 0.15055(18) 0.62202(11) 0.25812(8) 0.0204(4) Uani 1 1 d . . . C79 C 0.65134(17) 0.56070(10) 0.04189(7) 0.0172(4) Uani 1 1 d . . . H79 H 0.6263 0.5560 0.0064 0.021 Uiso 1 1 calc R . . C70 C 0.44450(18) 0.36020(11) 0.07877(7) 0.0192(4) Uani 1 1 d . . . H70 H 0.5086 0.3392 0.0664 0.023 Uiso 1 1 calc R . . C94 C 0.24378(18) 0.89687(11) 0.68303(8) 0.0206(4) Uani 1 1 d . . . H94 H 0.1766 0.8776 0.6610 0.025 Uiso 1 1 calc R . . C110 C 0.40513(18) 1.12106(11) 0.65778(8) 0.0207(4) Uani 1 1 d . . . H110 H 0.3547 1.1331 0.6848 0.025 Uiso 1 1 calc R . . C55 C 0.11120(18) 0.19355(12) 0.51070(8) 0.0223(4) Uani 1 1 d . . . H55A H 0.1038 0.1459 0.5170 0.027 Uiso 1 1 calc R . . H55B H 0.0460 0.2157 0.5255 0.027 Uiso 1 1 calc R . . C24 C 0.42142(19) 0.74786(13) 0.04035(9) 0.0264(5) Uani 1 1 d . . . H24A H 0.4586 0.7873 0.0698 0.032 Uiso 1 1 calc R . . H24B H 0.4571 0.7527 0.0076 0.032 Uiso 1 1 calc R . . C92 C 0.28825(19) 0.86890(12) 0.55951(8) 0.0237(4) Uani 1 1 d . . . H92 H 0.3326 0.8579 0.5859 0.028 Uiso 1 1 calc R . . C72 C 0.24457(19) 0.36076(11) 0.06880(8) 0.0213(4) Uani 1 1 d . . . H72 H 0.1728 0.3415 0.0507 0.026 Uiso 1 1 calc R . . C62 C 0.5346(2) 0.30505(12) 0.42500(9) 0.0269(5) Uani 1 1 d . . . H62A H 0.6064 0.2964 0.4398 0.032 Uiso 1 1 calc R . . H62B H 0.4996 0.3374 0.4531 0.032 Uiso 1 1 calc R . . C98 C 0.41229(18) 0.97954(11) 0.70740(8) 0.0201(4) Uani 1 1 d . . . H98 H 0.4631 1.0188 0.7029 0.024 Uiso 1 1 calc R . . N9 N 0.24991(17) 0.34314(9) 0.28268(7) 0.0222(4) Uani 1 1 d . . . C101 C 0.04808(18) 1.12149(11) 0.63537(8) 0.0211(4) Uani 1 1 d . . . H101 H 0.0351 1.1576 0.6192 0.025 Uiso 1 1 calc R . . C54 C 0.22065(17) 0.23834(11) 0.53896(7) 0.0191(4) Uani 1 1 d . . . H54A H 0.2191 0.2886 0.5401 0.023 Uiso 1 1 calc R . . H54B H 0.2255 0.2345 0.5757 0.023 Uiso 1 1 calc R . . C89 C 0.16447(19) 0.89848(13) 0.48009(8) 0.0259(5) Uani 1 1 d . . . H89 H 0.1229 0.9098 0.4530 0.031 Uiso 1 1 calc R . . C102 C -0.02666(18) 1.10265(11) 0.67062(8) 0.0221(4) Uani 1 1 d . . . H102 H -0.0904 1.1259 0.6793 0.027 Uiso 1 1 calc R . . C108 C 0.57296(18) 1.15504(11) 0.61615(8) 0.0219(4) Uani 1 1 d . . . H108 H 0.6361 1.1890 0.6140 0.026 Uiso 1 1 calc R . . C73 C 0.25625(19) 0.41895(11) 0.11240(8) 0.0219(4) Uani 1 1 d . . . H73 H 0.1919 0.4399 0.1244 0.026 Uiso 1 1 calc R . . C15 C -0.0309(2) 0.68002(13) 0.35811(8) 0.0288(5) Uani 1 1 d . . . H15A H -0.0267 0.6500 0.3823 0.043 Uiso 1 1 calc R . . H15B H -0.1024 0.6989 0.3615 0.043 Uiso 1 1 calc R . . H15C H 0.0324 0.7193 0.3669 0.043 Uiso 1 1 calc R . . C53 C 0.33656(19) 0.14394(10) 0.51577(7) 0.0192(4) Uani 1 1 d . . . H53A H 0.2664 0.1208 0.5272 0.023 Uiso 1 1 calc R . . H53B H 0.3985 0.1478 0.5425 0.023 Uiso 1 1 calc R . . C77 C 0.77020(19) 0.62111(12) 0.11883(8) 0.0234(4) Uani 1 1 d . . . H77 H 0.8273 0.6588 0.1368 0.028 Uiso 1 1 calc R . . N11 N 0.27262(17) 0.44011(9) 0.36367(7) 0.0225(4) Uani 1 1 d . . . C57 C 0.3176(2) 0.05945(11) 0.36931(8) 0.0262(5) Uani 1 1 d . . . H57A H 0.3952 0.0793 0.3645 0.039 Uiso 1 1 calc R . . H57B H 0.2671 0.0630 0.3406 0.039 Uiso 1 1 calc R . . H57C H 0.3144 0.0096 0.3691 0.039 Uiso 1 1 calc R . . C58 C 0.42241(18) 0.26700(11) 0.53687(8) 0.0214(4) Uani 1 1 d . . . H58A H 0.4151 0.3136 0.5318 0.032 Uiso 1 1 calc R . . H58B H 0.4898 0.2511 0.5203 0.032 Uiso 1 1 calc R . . H58C H 0.4295 0.2704 0.5747 0.032 Uiso 1 1 calc R . . C82 C 0.78881(19) 0.41309(13) 0.14290(8) 0.0251(4) Uani 1 1 d . . . H82 H 0.8191 0.4587 0.1396 0.030 Uiso 1 1 calc R . . C90 C 0.2022(2) 0.83400(13) 0.47071(8) 0.0296(5) Uani 1 1 d . . . H90 H 0.1854 0.8001 0.4375 0.036 Uiso 1 1 calc R . . C68 C 0.5934(2) 0.45924(13) 0.25352(8) 0.0286(5) Uani 1 1 d . . . H68 H 0.6097 0.4122 0.2433 0.034 Uiso 1 1 calc R . . C31 C 0.3791(2) 0.82497(13) 0.21750(8) 0.0272(5) Uani 1 1 d . . . H31A H 0.4572 0.8504 0.2271 0.033 Uiso 1 1 calc R . . H31B H 0.3761 0.7759 0.2205 0.033 Uiso 1 1 calc R . . C48 C 0.2770(2) 0.41095(11) 0.26945(8) 0.0306(5) Uani 1 1 d . . . H48A H 0.2280 0.4118 0.2388 0.037 Uiso 1 1 calc R . . H48B H 0.3569 0.4187 0.2606 0.037 Uiso 1 1 calc R . . C30 C 0.2966(2) 0.86255(12) 0.25280(9) 0.0281(5) Uani 1 1 d . . . H30A H 0.3345 0.8901 0.2873 0.034 Uiso 1 1 calc R . . H30B H 0.2328 0.8283 0.2588 0.034 Uiso 1 1 calc R . . C38 C 0.2604(2) 0.47283(10) 0.50437(8) 0.0215(4) Uani 1 1 d . . . C13 C 0.2665(2) 0.65780(15) 0.28357(10) 0.0337(6) Uani 1 1 d . . . H13A H 0.2596 0.7025 0.3092 0.051 Uiso 1 1 calc R . . H13B H 0.3163 0.6673 0.2564 0.051 Uiso 1 1 calc R . . H13C H 0.2986 0.6267 0.3016 0.051 Uiso 1 1 calc R . . C76 C 0.72327(18) 0.57179(11) 0.14435(8) 0.0212(4) Uani 1 1 d . . . H76 H 0.7499 0.5765 0.1796 0.025 Uiso 1 1 calc R . . C97 C 0.4392(2) 0.94794(12) 0.74674(8) 0.0251(4) Uani 1 1 d . . . H97 H 0.5075 0.9656 0.7681 0.030 Uiso 1 1 calc R . . C10 C -0.0796(2) 0.82876(13) 0.03004(8) 0.0289(5) Uani 1 1 d . . . H10A H -0.1432 0.7906 0.0275 0.043 Uiso 1 1 calc R . . H10B H -0.0115 0.8083 0.0189 0.043 Uiso 1 1 calc R . . H10C H -0.0970 0.8584 0.0071 0.043 Uiso 1 1 calc R . . C40 C 0.0755(2) 0.11232(13) 0.24453(9) 0.0324(5) Uani 1 1 d . . . H40A H 0.0158 0.1416 0.2459 0.049 Uiso 1 1 calc R . . H40B H 0.0818 0.0992 0.2779 0.049 Uiso 1 1 calc R . . H40C H 0.0568 0.0694 0.2154 0.049 Uiso 1 1 calc R . . C64 C 0.55211(18) 0.56260(12) 0.23275(8) 0.0237(4) Uani 1 1 d . . . H64 H 0.5388 0.5882 0.2078 0.028 Uiso 1 1 calc R . . C96 C 0.3673(2) 0.89116(13) 0.75489(8) 0.0279(5) Uani 1 1 d . . . H96 H 0.3849 0.8700 0.7821 0.034 Uiso 1 1 calc R . . C47 C 0.3468(2) 0.60258(11) 0.43611(9) 0.0268(5) Uani 1 1 d . . . H47A H 0.3382 0.6484 0.4598 0.040 Uiso 1 1 calc R . . H47B H 0.3431 0.6057 0.3995 0.040 Uiso 1 1 calc R . . H47C H 0.4199 0.5900 0.4445 0.040 Uiso 1 1 calc R . . C71 C 0.33996(19) 0.33140(11) 0.05220(8) 0.0215(4) Uani 1 1 d . . . H71 H 0.3338 0.2914 0.0225 0.026 Uiso 1 1 calc R . . C27 C 0.4514(2) 0.67066(13) 0.14031(8) 0.0268(5) Uani 1 1 d . . . H27A H 0.4078 0.6620 0.1697 0.040 Uiso 1 1 calc R . . H27B H 0.4939 0.7188 0.1506 0.040 Uiso 1 1 calc R . . H27C H 0.5041 0.6365 0.1314 0.040 Uiso 1 1 calc R . . C95 C 0.2692(2) 0.86556(12) 0.72271(9) 0.0263(5) Uani 1 1 d . . . H95 H 0.2189 0.8264 0.7277 0.032 Uiso 1 1 calc R . . C49 C 0.2563(2) 0.46784(11) 0.31792(8) 0.0286(5) Uani 1 1 d . . . H49A H 0.3101 0.5119 0.3210 0.034 Uiso 1 1 calc R . . H49B H 0.1784 0.4785 0.3154 0.034 Uiso 1 1 calc R . . C28 C 0.3128(2) 0.89434(12) 0.17044(9) 0.0296(5) Uani 1 1 d . . . H28A H 0.2600 0.8942 0.1408 0.035 Uiso 1 1 calc R . . H28B H 0.3807 0.9298 0.1714 0.035 Uiso 1 1 calc R . . C107 C 0.55559(18) 1.08874(11) 0.58076(8) 0.0203(4) Uani 1 1 d . . . H107 H 0.6072 1.0769 0.5542 0.024 Uiso 1 1 calc R . . C50 C 0.07766(19) 0.11281(12) 0.42099(8) 0.0250(5) Uani 1 1 d . . . H50A H 0.0698 0.1123 0.3833 0.030 Uiso 1 1 calc R . . H50B H 0.0035 0.0927 0.4310 0.030 Uiso 1 1 calc R . . C91 C 0.2650(2) 0.81940(13) 0.51042(9) 0.0292(5) Uani 1 1 d . . . H91 H 0.2924 0.7755 0.5043 0.035 Uiso 1 1 calc R . . C43 C 0.3186(2) 0.26074(12) 0.16579(9) 0.0283(5) Uani 1 1 d . . . H43A H 0.3779 0.2429 0.1825 0.042 Uiso 1 1 calc R . . H43B H 0.3414 0.3114 0.1691 0.042 Uiso 1 1 calc R . . H43C H 0.3071 0.2351 0.1284 0.042 Uiso 1 1 calc R . . C60 C 0.5365(2) 0.27291(13) 0.33042(10) 0.0350(6) Uani 1 1 d . . . H60A H 0.6081 0.2662 0.3131 0.042 Uiso 1 1 calc R . . H60B H 0.4802 0.2793 0.3045 0.042 Uiso 1 1 calc R . . C25 C 0.0359(2) 0.60864(14) 0.06542(10) 0.0340(6) Uani 1 1 d . . . H25A H -0.0057 0.5702 0.0372 0.051 Uiso 1 1 calc R . . H25B H -0.0071 0.6482 0.0740 0.051 Uiso 1 1 calc R . . H25C H 0.0465 0.5915 0.0968 0.051 Uiso 1 1 calc R . . C26 C 0.2906(2) 0.82479(13) 0.03059(9) 0.0305(5) Uani 1 1 d . . . H26A H 0.3353 0.8599 0.0599 0.046 Uiso 1 1 calc R . . H26B H 0.2112 0.8318 0.0318 0.046 Uiso 1 1 calc R . . H26C H 0.3193 0.8304 -0.0029 0.046 Uiso 1 1 calc R . . C109 C 0.49695(19) 1.17126(11) 0.65481(8) 0.0229(4) Uani 1 1 d . . . H109 H 0.5077 1.2167 0.6792 0.027 Uiso 1 1 calc R . . C65 C 0.5456(2) 0.59520(14) 0.28617(8) 0.0290(5) Uani 1 1 d . . . H65 H 0.5293 0.6422 0.2969 0.035 Uiso 1 1 calc R . . C86 C 0.6341(2) 0.32854(12) 0.15096(9) 0.0280(5) Uani 1 1 d . . . H86 H 0.5556 0.3149 0.1536 0.034 Uiso 1 1 calc R . . C21 C 0.2195(2) 0.57684(13) 0.03710(11) 0.0348(6) Uani 1 1 d . . . H21A H 0.2534 0.5751 0.0029 0.042 Uiso 1 1 calc R . . H21B H 0.1724 0.5304 0.0341 0.042 Uiso 1 1 calc R . . C11 C -0.2143(2) 0.95008(12) 0.19111(9) 0.0289(5) Uani 1 1 d . . . H11A H -0.1368 0.9747 0.2012 0.043 Uiso 1 1 calc R . . H11B H -0.2477 0.9372 0.2216 0.043 Uiso 1 1 calc R . . H11C H -0.2593 0.9813 0.1791 0.043 Uiso 1 1 calc R . . C20 C 0.1321(2) 0.66110(16) 0.00151(9) 0.0358(6) Uani 1 1 d . . . H20A H 0.0754 0.6936 0.0087 0.043 Uiso 1 1 calc R . . H20B H 0.1022 0.6215 -0.0294 0.043 Uiso 1 1 calc R . . C103 C -0.00612(18) 1.04910(11) 0.69290(8) 0.0218(4) Uani 1 1 d . . . H103 H -0.0563 1.0354 0.7172 0.026 Uiso 1 1 calc R . . C9 C 0.0371(2) 0.93493(12) 0.09289(9) 0.0287(5) Uani 1 1 d . . . H9A H 0.0200 0.9645 0.0699 0.043 Uiso 1 1 calc R . . H9B H 0.1071 0.9161 0.0829 0.043 Uiso 1 1 calc R . . H9C H 0.0465 0.9635 0.1296 0.043 Uiso 1 1 calc R . . C16 C -0.1236(2) 0.57582(12) 0.28616(10) 0.0290(5) Uani 1 1 d . . . H16A H -0.1166 0.5478 0.2501 0.044 Uiso 1 1 calc R . . H16B H -0.1947 0.5951 0.2879 0.044 Uiso 1 1 calc R . . H16C H -0.1230 0.5456 0.3104 0.044 Uiso 1 1 calc R . . C51 C 0.1646(2) 0.06713(11) 0.42820(8) 0.0241(4) Uani 1 1 d . . . H51A H 0.1622 0.0603 0.4642 0.029 Uiso 1 1 calc R . . H51B H 0.1453 0.0200 0.4027 0.029 Uiso 1 1 calc R . . C14 C 0.1557(2) 0.55271(13) 0.21703(9) 0.0333(6) Uani 1 1 d . . . H14A H 0.1901 0.5209 0.2335 0.050 Uiso 1 1 calc R . . H14B H 0.2014 0.5622 0.1885 0.050 Uiso 1 1 calc R . . H14C H 0.0791 0.5305 0.2027 0.050 Uiso 1 1 calc R . . C83 C 0.8626(2) 0.36498(14) 0.14389(10) 0.0330(5) Uani 1 1 d . . . H83 H 0.9414 0.3784 0.1417 0.040 Uiso 1 1 calc R . . C42 C 0.1142(2) 0.27597(13) 0.16828(9) 0.0300(5) Uani 1 1 d . . . H42A H 0.1004 0.2500 0.1310 0.045 Uiso 1 1 calc R . . H42B H 0.1351 0.3266 0.1712 0.045 Uiso 1 1 calc R . . H42C H 0.0455 0.2683 0.1868 0.045 Uiso 1 1 calc R . . C66 C 0.5629(2) 0.55906(15) 0.32342(8) 0.0342(6) Uani 1 1 d . . . H66 H 0.5585 0.5808 0.3599 0.041 Uiso 1 1 calc R . . C45 C 0.3592(2) 0.47540(13) 0.54189(9) 0.0335(6) Uani 1 1 d . . . H45A H 0.4295 0.4926 0.5278 0.050 Uiso 1 1 calc R . . H45B H 0.3620 0.4278 0.5460 0.050 Uiso 1 1 calc R . . H45C H 0.3502 0.5074 0.5763 0.050 Uiso 1 1 calc R . . C22 C 0.3121(2) 0.58934(12) 0.07953(10) 0.0304(5) Uani 1 1 d . . . H22A H 0.2790 0.5786 0.1112 0.036 Uiso 1 1 calc R . . H22B H 0.3664 0.5563 0.0673 0.036 Uiso 1 1 calc R . . C41 C 0.2821(2) 0.10949(13) 0.23066(9) 0.0322(5) Uani 1 1 d . . . H41A H 0.2635 0.0680 0.2004 0.048 Uiso 1 1 calc R . . H41B H 0.2913 0.0940 0.2628 0.048 Uiso 1 1 calc R . . H41C H 0.3526 0.1380 0.2253 0.048 Uiso 1 1 calc R . . C61 C 0.5554(3) 0.33639(15) 0.37854(11) 0.0426(7) Uani 1 1 d . . . H61A H 0.6335 0.3620 0.3813 0.051 Uiso 1 1 calc R . . H61B H 0.5018 0.3695 0.3767 0.051 Uiso 1 1 calc R . . C56 C 0.0320(2) 0.23111(14) 0.43791(9) 0.0289(5) Uani 1 1 d . . . H56A H 0.0375 0.2292 0.4004 0.043 Uiso 1 1 calc R . . H56B H 0.0535 0.2801 0.4591 0.043 Uiso 1 1 calc R . . H56C H -0.0458 0.2136 0.4442 0.043 Uiso 1 1 calc R . . C19 C 0.2403(2) 0.70014(14) -0.01177(9) 0.0333(5) Uani 1 1 d . . . H19A H 0.2909 0.6657 -0.0267 0.040 Uiso 1 1 calc R . . H19B H 0.2230 0.7243 -0.0390 0.040 Uiso 1 1 calc R . . C67 C 0.5864(2) 0.49129(15) 0.30693(9) 0.0380(6) Uani 1 1 d . . . H67 H 0.5980 0.4659 0.3322 0.046 Uiso 1 1 calc R . . C29 C 0.2562(3) 0.91105(14) 0.22251(10) 0.0373(6) Uani 1 1 d . . . H29A H 0.2792 0.9613 0.2420 0.045 Uiso 1 1 calc R . . H29B H 0.1729 0.9014 0.2164 0.045 Uiso 1 1 calc R . . C84 C 0.8214(2) 0.29819(15) 0.14800(10) 0.0380(6) Uani 1 1 d . . . H84 H 0.8713 0.2651 0.1484 0.046 Uiso 1 1 calc R . . C44 C 0.1487(2) 0.44961(14) 0.52602(11) 0.0366(6) Uani 1 1 d . . . H44A H 0.1409 0.4825 0.5602 0.055 Uiso 1 1 calc R . . H44B H 0.1473 0.4018 0.5305 0.055 Uiso 1 1 calc R . . H44C H 0.0861 0.4495 0.5013 0.055 Uiso 1 1 calc R . . C12 C -0.3321(2) 0.84522(14) 0.12839(11) 0.0338(5) Uani 1 1 d . . . H12A H -0.3719 0.8740 0.1111 0.051 Uiso 1 1 calc R . . H12B H -0.3727 0.8376 0.1588 0.051 Uiso 1 1 calc R . . H12C H -0.3285 0.7995 0.1034 0.051 Uiso 1 1 calc R . . C46 C 0.1377(2) 0.56453(14) 0.43039(10) 0.0322(5) Uani 1 1 d . . . H46A H 0.0780 0.5276 0.4350 0.048 Uiso 1 1 calc R . . H46B H 0.1330 0.5677 0.3938 0.048 Uiso 1 1 calc R . . H46C H 0.1282 0.6101 0.4542 0.048 Uiso 1 1 calc R . . C85 C 0.7062(3) 0.27957(14) 0.15163(11) 0.0384(6) Uani 1 1 d . . . H85 H 0.6767 0.2336 0.1545 0.046 Uiso 1 1 calc R . . C23 C 0.4400(2) 0.67891(13) 0.05030(9) 0.0262(5) Uani 1 1 d . . . H23A H 0.4178 0.6403 0.0178 0.031 Uiso 1 1 calc R . . H23B H 0.5215 0.6808 0.0590 0.031 Uiso 1 1 calc R . . O11 O 0.3323(3) 0.01305(17) 0.08348(14) 0.0931(10) Uani 1 1 d . . . C111 C 0.4446(5) 0.0378(4) 0.0907(3) 0.123(2) Uani 1 1 d . . . H11D H 0.4874 0.0017 0.0703 0.148 Uiso 1 1 calc R . . H11E H 0.4694 0.0482 0.1284 0.148 Uiso 1 1 calc R . . C112 C 0.4678(5) 0.1054(4) 0.0719(4) 0.167(4) Uani 1 1 d . . . H11F H 0.4882 0.1476 0.1022 0.201 Uiso 1 1 calc R . . H11G H 0.5302 0.1030 0.0478 0.201 Uiso 1 1 calc R . . C113 C 0.3612(5) 0.1087(2) 0.0441(2) 0.0912(16) Uani 1 1 d . . . H11H H 0.3602 0.0858 0.0059 0.109 Uiso 1 1 calc R . . H11I H 0.3475 0.1581 0.0494 0.109 Uiso 1 1 calc R . . C114 C 0.2759(4) 0.0673(2) 0.07119(18) 0.0787(13) Uani 1 1 d . . . H11J H 0.2533 0.0988 0.1038 0.094 Uiso 1 1 calc R . . H11K H 0.2075 0.0458 0.0475 0.094 Uiso 1 1 calc R . . O12 O 0.9313(8) 0.4284(2) 0.3461(2) 0.121(4) Uani 0.637(7) 1 d P A 1 C117 C 0.9504(6) 0.3772(3) 0.3723(3) 0.062(2) Uani 0.637(7) 1 d P A 1 H11L H 1.0307 0.3853 0.3854 0.074 Uiso 0.637(7) 1 calc PR A 1 H11M H 0.9032 0.3808 0.4030 0.074 Uiso 0.637(7) 1 calc PR A 1 C119 C 0.9261(8) 0.3909(3) 0.2934(3) 0.081(3) Uani 0.637(7) 1 d P A 1 H11N H 0.8749 0.4102 0.2726 0.097 Uiso 0.637(7) 1 calc PR A 1 H11O H 1.0022 0.3964 0.2797 0.097 Uiso 0.637(7) 1 calc PR A 1 O12A O 0.8167(8) 0.4034(5) 0.3521(3) 0.065(3) Uani 0.363(7) 1 d P A 2 C17A C 0.8767(14) 0.3626(7) 0.3776(4) 0.064(4) Uani 0.363(7) 1 d P A 2 H17C H 0.8249 0.3384 0.3984 0.077 Uiso 0.363(7) 1 calc PR A 2 H17D H 0.9383 0.3940 0.4019 0.077 Uiso 0.363(7) 1 calc PR A 2 C19A C 0.8357(8) 0.3810(4) 0.2984(3) 0.034(2) Uani 0.363(7) 1 d P A 2 H19C H 0.7624 0.3690 0.2774 0.041 Uiso 0.363(7) 1 calc PR A 2 H19D H 0.8818 0.4202 0.2877 0.041 Uiso 0.363(7) 1 calc PR A 2 C116 C 0.9236(6) 0.3106(3) 0.3378(2) 0.123(2) Uani 1 1 d . . . H11R H 0.8609 0.2818 0.3503 0.147 Uiso 1 1 calc R A 1 H11S H 0.9898 0.2854 0.3338 0.147 Uiso 1 1 calc R A 1 C118 C 0.8895(8) 0.3242(3) 0.28801(19) 0.140(3) Uani 1 1 d . A . H11P H 0.9239 0.2945 0.2582 0.169 Uiso 1 1 calc R B 1 H11Q H 0.8062 0.3141 0.2816 0.169 Uiso 1 1 calc R B 1 O13 O 0.8739(4) 0.1044(2) 0.13044(16) 0.1265(15) Uani 1 1 d . . . C120 C 0.7550(4) 0.0877(3) 0.10671(18) 0.0798(13) Uani 1 1 d . . . H12F H 0.7050 0.0595 0.1257 0.096 Uiso 1 1 calc R . . H12G H 0.7238 0.1313 0.1064 0.096 Uiso 1 1 calc R . . C121 C 0.7700(7) 0.0478(3) 0.0550(3) 0.145(3) Uani 1 1 d . . . H12D H 0.7180 0.0591 0.0296 0.173 Uiso 1 1 calc R . . H12E H 0.7511 -0.0033 0.0528 0.173 Uiso 1 1 calc R . . C123 C 0.8911(6) 0.0638(2) 0.04035(14) 0.0935(18) Uani 1 1 d . . . H12H H 0.9272 0.0206 0.0327 0.112 Uiso 1 1 calc R . . H12I H 0.8937 0.0830 0.0091 0.112 Uiso 1 1 calc R . . C122 C 0.9435(4) 0.1132(2) 0.08400(14) 0.0725(12) Uani 1 1 d . . . H12J H 0.9458 0.1615 0.0795 0.087 Uiso 1 1 calc R . . H12K H 1.0219 0.1052 0.0899 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01691(11) 0.01874(11) 0.01406(9) 0.00319(8) 0.00487(8) 0.00535(8) Zn2 0.01682(11) 0.01391(10) 0.01042(9) 0.00457(7) 0.00257(7) 0.00113(8) Ni1 0.01390(12) 0.01445(11) 0.01194(10) 0.00323(8) 0.00286(8) 0.00368(9) Ni2 0.02727(15) 0.01341(11) 0.01171(10) 0.00494(8) 0.00137(9) 0.00144(10) N12 0.0170(8) 0.0257(9) 0.0145(7) 0.0055(6) 0.0012(6) -0.0008(7) O4 0.0254(8) 0.0299(8) 0.0205(7) 0.0142(6) 0.0087(6) 0.0132(6) O8 0.0392(9) 0.0194(7) 0.0115(6) 0.0063(5) -0.0019(6) -0.0021(6) C32 0.0182(9) 0.0155(8) 0.0136(7) 0.0058(6) 0.0032(6) 0.0018(7) N14 0.0175(8) 0.0151(7) 0.0136(7) 0.0051(6) 0.0012(6) 0.0015(6) O9 0.0498(11) 0.0160(7) 0.0183(7) 0.0027(5) 0.0023(7) 0.0091(7) O1 0.0177(7) 0.0253(7) 0.0173(6) 0.0067(5) 0.0082(5) 0.0077(6) N8 0.0181(8) 0.0152(7) 0.0130(6) 0.0068(6) 0.0029(6) 0.0010(6) C59 0.0236(11) 0.0281(11) 0.0189(9) 0.0042(8) 0.0062(8) 0.0013(9) N6 0.0264(10) 0.0265(9) 0.0169(7) 0.0067(7) 0.0056(7) 0.0080(7) C8 0.0195(10) 0.0195(9) 0.0149(8) 0.0065(7) 0.0044(7) 0.0071(7) C75 0.0147(9) 0.0194(9) 0.0119(7) 0.0026(6) 0.0021(6) 0.0050(7) N5 0.0220(10) 0.0259(9) 0.0223(8) -0.0029(7) 0.0047(7) 0.0031(7) C18 0.0143(9) 0.0189(9) 0.0182(8) 0.0057(7) 0.0042(7) 0.0031(7) N1 0.0157(8) 0.0174(7) 0.0139(7) 0.0037(6) 0.0045(6) 0.0040(6) N7 0.0198(9) 0.0213(8) 0.0195(8) 0.0055(6) 0.0076(6) 0.0065(7) N3 0.0157(8) 0.0162(7) 0.0133(7) 0.0025(6) 0.0044(6) 0.0037(6) O10 0.0230(8) 0.0230(7) 0.0173(6) 0.0028(5) 0.0055(6) -0.0017(6) O2 0.0181(7) 0.0249(7) 0.0191(6) 0.0084(6) 0.0088(5) 0.0092(6) C6 0.0173(10) 0.0233(9) 0.0179(8) 0.0078(7) 0.0033(7) 0.0066(8) O6 0.0252(8) 0.0144(6) 0.0126(6) 0.0072(5) 0.0006(5) 0.0010(5) C3 0.0179(9) 0.0160(8) 0.0145(8) 0.0036(6) 0.0031(7) 0.0051(7) N13 0.0271(9) 0.0158(7) 0.0130(7) 0.0045(6) 0.0024(6) 0.0015(7) C4 0.0189(10) 0.0159(8) 0.0131(7) 0.0028(6) 0.0015(7) 0.0016(7) N10 0.0209(9) 0.0150(7) 0.0136(7) 0.0055(6) 0.0021(6) 0.0025(6) C99 0.0146(9) 0.0194(9) 0.0107(7) 0.0028(6) 0.0010(6) -0.0007(7) N2 0.0168(8) 0.0177(7) 0.0143(7) 0.0038(6) 0.0036(6) 0.0043(6) O7 0.0271(8) 0.0159(6) 0.0136(6) 0.0066(5) 0.0031(5) 0.0050(6) O5 0.0288(9) 0.0241(7) 0.0158(6) 0.0010(6) 0.0017(6) 0.0048(6) C69 0.0185(10) 0.0189(9) 0.0134(7) 0.0080(7) 0.0028(7) 0.0018(7) C100 0.0205(10) 0.0229(9) 0.0133(8) 0.0057(7) 0.0015(7) 0.0025(8) N4 0.0161(8) 0.0159(7) 0.0146(7) 0.0037(6) 0.0052(6) 0.0033(6) C80 0.0150(9) 0.0175(8) 0.0119(7) 0.0020(6) 0.0005(6) 0.0023(7) C39 0.0232(11) 0.0168(9) 0.0191(9) 0.0037(7) -0.0016(7) 0.0054(8) C33 0.0210(10) 0.0181(9) 0.0134(8) 0.0067(7) 0.0016(7) 0.0023(7) O3 0.0300(9) 0.0403(9) 0.0254(7) 0.0196(7) 0.0121(6) 0.0203(7) C78 0.0217(10) 0.0221(9) 0.0185(9) 0.0061(7) 0.0045(7) -0.0008(8) B2 0.0146(10) 0.0185(10) 0.0132(8) 0.0045(7) 0.0015(7) 0.0020(8) C37 0.0267(11) 0.0191(9) 0.0131(8) 0.0070(7) 0.0014(7) 0.0012(8) C104 0.0184(10) 0.0172(8) 0.0153(8) 0.0039(7) 0.0026(7) -0.0003(7) C35 0.0208(10) 0.0157(8) 0.0194(8) 0.0052(7) -0.0009(7) 0.0020(7) C105 0.0163(9) 0.0191(9) 0.0130(7) 0.0056(7) 0.0013(6) 0.0016(7) C36 0.0290(11) 0.0176(9) 0.0116(7) 0.0052(7) 0.0006(7) 0.0011(8) C74 0.0216(10) 0.0173(9) 0.0177(8) 0.0051(7) 0.0018(7) 0.0025(7) C2 0.0169(9) 0.0179(9) 0.0148(8) 0.0028(7) 0.0007(7) 0.0037(7) C17 0.0156(9) 0.0211(9) 0.0159(8) 0.0060(7) 0.0048(7) 0.0060(7) B1 0.0176(11) 0.0208(10) 0.0114(8) 0.0050(7) 0.0013(7) 0.0027(8) C52 0.0302(12) 0.0186(9) 0.0171(8) 0.0075(7) 0.0026(8) 0.0064(8) C5 0.0234(11) 0.0240(10) 0.0171(8) 0.0077(7) 0.0055(7) 0.0084(8) C63 0.0166(10) 0.0275(10) 0.0123(8) 0.0054(7) 0.0011(7) 0.0019(8) C81 0.0239(11) 0.0259(10) 0.0147(8) 0.0060(7) 0.0004(7) 0.0077(8) C106 0.0173(10) 0.0165(8) 0.0179(8) 0.0049(7) 0.0034(7) 0.0023(7) C93 0.0175(10) 0.0196(9) 0.0134(8) 0.0038(7) 0.0044(7) 0.0048(7) C87 0.0142(9) 0.0229(9) 0.0156(8) 0.0046(7) 0.0050(7) -0.0024(7) C34 0.0196(10) 0.0155(8) 0.0160(8) 0.0038(7) 0.0008(7) 0.0032(7) C1 0.0181(10) 0.0185(9) 0.0130(7) 0.0037(6) 0.0022(7) 0.0046(7) C88 0.0185(10) 0.0264(10) 0.0154(8) 0.0052(7) 0.0029(7) -0.0028(8) C7 0.0220(10) 0.0245(10) 0.0191(9) 0.0093(8) 0.0060(7) 0.0110(8) C79 0.0180(10) 0.0202(9) 0.0131(8) 0.0035(7) 0.0015(7) 0.0034(7) C70 0.0224(10) 0.0211(9) 0.0149(8) 0.0061(7) 0.0051(7) 0.0029(8) C94 0.0210(10) 0.0211(9) 0.0213(9) 0.0076(7) 0.0047(7) 0.0038(8) C110 0.0188(10) 0.0247(10) 0.0156(8) 0.0021(7) 0.0036(7) -0.0006(8) C55 0.0201(10) 0.0310(11) 0.0146(8) 0.0055(8) 0.0065(7) 0.0000(8) C24 0.0241(11) 0.0315(12) 0.0260(10) 0.0101(9) 0.0108(8) 0.0062(9) C92 0.0206(11) 0.0252(10) 0.0217(9) 0.0000(8) 0.0027(8) 0.0027(8) C72 0.0221(11) 0.0237(10) 0.0173(8) 0.0071(7) -0.0018(7) -0.0019(8) C62 0.0252(12) 0.0270(11) 0.0226(10) 0.0011(8) 0.0028(8) -0.0055(9) C98 0.0219(10) 0.0213(9) 0.0170(8) 0.0033(7) 0.0019(7) 0.0056(8) N9 0.0359(11) 0.0171(8) 0.0152(7) 0.0082(6) 0.0015(7) 0.0017(7) C101 0.0221(11) 0.0215(9) 0.0186(9) 0.0034(7) -0.0032(7) 0.0040(8) C54 0.0224(10) 0.0223(9) 0.0119(8) 0.0034(7) 0.0044(7) 0.0028(8) C89 0.0198(11) 0.0384(12) 0.0143(8) 0.0040(8) 0.0013(7) -0.0076(9) C102 0.0160(10) 0.0242(10) 0.0229(9) -0.0001(8) 0.0008(7) 0.0040(8) C108 0.0174(10) 0.0246(10) 0.0237(9) 0.0094(8) 0.0005(8) -0.0022(8) C73 0.0201(10) 0.0239(10) 0.0231(9) 0.0085(8) 0.0016(8) 0.0039(8) C15 0.0407(14) 0.0354(12) 0.0149(9) 0.0070(8) 0.0068(9) 0.0191(11) C53 0.0288(11) 0.0160(8) 0.0141(8) 0.0064(7) 0.0007(7) 0.0032(8) C77 0.0227(11) 0.0249(10) 0.0175(9) 0.0015(8) -0.0013(8) -0.0053(8) N11 0.0361(11) 0.0146(7) 0.0167(7) 0.0057(6) -0.0014(7) 0.0009(7) C57 0.0450(14) 0.0197(10) 0.0151(8) 0.0047(7) 0.0066(9) 0.0077(9) C58 0.0218(11) 0.0215(9) 0.0182(9) 0.0036(7) -0.0030(7) -0.0017(8) C82 0.0239(11) 0.0311(11) 0.0192(9) 0.0028(8) -0.0018(8) 0.0081(9) C90 0.0227(11) 0.0372(13) 0.0180(9) -0.0048(9) 0.0066(8) -0.0102(9) C68 0.0394(14) 0.0322(12) 0.0152(9) 0.0103(8) 0.0009(8) 0.0019(10) C31 0.0292(12) 0.0308(11) 0.0198(9) 0.0015(8) -0.0017(8) 0.0085(9) C48 0.0574(17) 0.0182(10) 0.0175(9) 0.0099(8) 0.0007(10) 0.0005(10) C30 0.0336(13) 0.0277(11) 0.0202(9) 0.0008(8) 0.0071(9) 0.0043(9) C38 0.0323(12) 0.0153(9) 0.0174(8) 0.0039(7) 0.0041(8) 0.0057(8) C13 0.0238(12) 0.0520(16) 0.0341(12) 0.0247(12) 0.0009(9) 0.0100(11) C76 0.0200(10) 0.0272(10) 0.0132(8) 0.0028(7) -0.0021(7) -0.0023(8) C97 0.0280(12) 0.0302(11) 0.0183(9) 0.0052(8) -0.0012(8) 0.0115(9) C10 0.0330(13) 0.0373(13) 0.0166(9) 0.0060(9) -0.0003(8) 0.0088(10) C40 0.0413(15) 0.0302(12) 0.0202(10) 0.0077(9) -0.0022(9) -0.0131(10) C64 0.0208(11) 0.0351(12) 0.0158(8) 0.0046(8) 0.0000(7) 0.0100(9) C96 0.0394(14) 0.0318(12) 0.0190(9) 0.0117(9) 0.0059(9) 0.0166(10) C47 0.0304(12) 0.0185(10) 0.0281(11) 0.0034(8) -0.0016(9) -0.0016(9) C71 0.0277(11) 0.0211(9) 0.0146(8) 0.0053(7) 0.0020(7) -0.0009(8) C27 0.0274(12) 0.0348(12) 0.0221(10) 0.0083(9) 0.0050(8) 0.0157(10) C95 0.0321(13) 0.0246(10) 0.0278(10) 0.0141(9) 0.0107(9) 0.0087(9) C49 0.0505(15) 0.0175(9) 0.0187(9) 0.0085(8) -0.0043(9) 0.0028(9) C28 0.0419(14) 0.0196(10) 0.0252(10) 0.0049(8) -0.0007(10) 0.0011(9) C107 0.0176(10) 0.0237(10) 0.0214(9) 0.0082(8) 0.0063(7) 0.0042(8) C50 0.0225(11) 0.0312(11) 0.0171(9) 0.0068(8) -0.0004(8) -0.0103(9) C91 0.0274(12) 0.0271(11) 0.0260(10) -0.0050(9) 0.0085(9) 0.0022(9) C43 0.0381(14) 0.0280(11) 0.0227(10) 0.0117(9) 0.0121(9) 0.0072(10) C60 0.0422(15) 0.0339(13) 0.0271(11) 0.0086(10) 0.0126(10) -0.0030(11) C25 0.0256(13) 0.0331(13) 0.0337(12) -0.0033(10) 0.0077(10) -0.0056(10) C26 0.0361(14) 0.0341(12) 0.0286(11) 0.0154(10) 0.0144(10) 0.0144(10) C109 0.0237(11) 0.0219(10) 0.0190(9) 0.0017(7) -0.0013(8) -0.0021(8) C65 0.0243(12) 0.0409(13) 0.0185(9) -0.0013(9) 0.0026(8) 0.0110(10) C86 0.0285(12) 0.0278(11) 0.0314(11) 0.0121(9) 0.0007(9) 0.0085(9) C21 0.0322(14) 0.0242(11) 0.0405(14) -0.0042(10) 0.0094(11) 0.0021(10) C11 0.0404(14) 0.0248(11) 0.0248(10) 0.0061(9) 0.0066(9) 0.0162(10) C20 0.0263(13) 0.0550(17) 0.0197(10) 0.0004(10) -0.0010(9) 0.0032(11) C103 0.0183(10) 0.0233(10) 0.0209(9) 0.0027(8) 0.0056(7) -0.0008(8) C9 0.0304(13) 0.0280(11) 0.0303(11) 0.0123(9) 0.0049(9) 0.0041(9) C16 0.0276(12) 0.0271(11) 0.0351(12) 0.0168(10) -0.0004(9) -0.0020(9) C51 0.0332(12) 0.0196(9) 0.0162(8) 0.0055(7) 0.0012(8) -0.0086(8) C14 0.0568(17) 0.0267(11) 0.0246(10) 0.0109(9) 0.0151(11) 0.0239(11) C83 0.0250(12) 0.0435(14) 0.0295(11) 0.0034(10) -0.0064(9) 0.0150(11) C42 0.0350(14) 0.0331(12) 0.0241(10) 0.0120(9) -0.0058(9) 0.0055(10) C66 0.0330(13) 0.0543(16) 0.0122(9) 0.0044(10) 0.0047(8) 0.0045(12) C45 0.0523(17) 0.0240(11) 0.0210(10) 0.0008(8) -0.0110(10) 0.0067(11) C22 0.0338(13) 0.0193(10) 0.0389(13) 0.0061(9) 0.0115(10) 0.0080(9) C41 0.0541(16) 0.0274(11) 0.0171(9) 0.0032(8) 0.0026(10) 0.0177(11) C61 0.0520(18) 0.0324(13) 0.0384(14) 0.0075(11) 0.0086(13) -0.0070(12) C56 0.0198(11) 0.0443(14) 0.0245(10) 0.0106(10) 0.0016(8) 0.0083(10) C19 0.0379(14) 0.0428(14) 0.0176(10) 0.0047(9) 0.0022(9) 0.0073(11) C67 0.0514(17) 0.0481(16) 0.0148(9) 0.0131(10) 0.0016(10) 0.0001(13) C29 0.0450(16) 0.0318(13) 0.0332(13) -0.0005(10) 0.0035(11) 0.0166(12) C84 0.0395(15) 0.0427(15) 0.0331(13) 0.0039(11) -0.0083(11) 0.0238(12) C44 0.0443(16) 0.0297(12) 0.0371(13) 0.0074(10) 0.0215(11) 0.0095(11) C12 0.0217(12) 0.0395(14) 0.0433(14) 0.0192(11) -0.0074(10) 0.0017(10) C46 0.0269(13) 0.0334(13) 0.0384(13) 0.0097(10) 0.0012(10) 0.0117(10) C85 0.0459(17) 0.0300(13) 0.0428(14) 0.0131(11) -0.0071(12) 0.0130(11) C23 0.0215(11) 0.0361(12) 0.0243(10) 0.0117(9) 0.0089(8) 0.0070(9) O11 0.105(3) 0.067(2) 0.109(3) 0.0250(18) 0.019(2) 0.0114(18) C111 0.071(4) 0.183(7) 0.124(5) 0.082(5) 0.007(3) -0.030(4) C112 0.056(4) 0.119(5) 0.319(12) 0.057(7) 0.005(5) -0.009(3) C113 0.122(4) 0.059(3) 0.090(3) 0.014(2) 0.041(3) 0.010(3) C114 0.094(3) 0.063(3) 0.074(3) 0.009(2) 0.026(2) 0.009(2) O12 0.234(10) 0.044(3) 0.080(4) 0.011(2) -0.045(5) 0.029(4) C117 0.058(4) 0.051(3) 0.071(4) 0.027(3) -0.036(3) -0.020(3) C119 0.114(7) 0.053(4) 0.061(4) 0.012(3) 0.013(4) -0.032(4) O12A 0.079(6) 0.076(5) 0.049(4) 0.014(4) 0.012(4) 0.047(5) C17A 0.108(11) 0.064(7) 0.035(4) 0.019(5) 0.009(6) 0.051(8) C19A 0.045(5) 0.031(4) 0.033(4) 0.013(3) 0.001(3) 0.015(3) C116 0.203(7) 0.102(4) 0.074(3) 0.036(3) -0.043(4) 0.045(4) C118 0.263(9) 0.122(5) 0.047(3) 0.035(3) 0.006(4) 0.042(6) O13 0.151(4) 0.135(3) 0.102(3) 0.063(3) -0.017(3) -0.006(3) C120 0.083(3) 0.085(3) 0.073(3) 0.031(2) -0.029(2) 0.007(2) C121 0.218(8) 0.078(4) 0.118(5) 0.045(3) -0.104(5) -0.055(4) C123 0.194(6) 0.050(2) 0.0287(16) 0.0095(15) -0.003(2) -0.001(3) C122 0.119(4) 0.052(2) 0.050(2) 0.0215(17) 0.013(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.0073(15) . ? Zn1 O2 2.0090(14) . ? Zn1 N5 2.1947(18) . ? Zn1 N7 2.2212(17) . ? Zn1 N6 2.2394(17) . ? Zn1 O5 2.3431(15) . ? Zn2 O6 2.0091(13) . ? Zn2 O7 2.0248(14) . ? Zn2 N12 2.1776(17) . ? Zn2 N14 2.2212(15) . ? Zn2 N13 2.2361(17) . ? Zn2 O10 2.2942(15) . ? Ni1 N2 1.8394(17) . ? Ni1 N4 1.8479(15) . ? Ni1 N3 1.8799(17) . ? Ni1 N1 1.8886(16) . ? Ni2 N9 1.8406(16) . ? Ni2 N11 1.8407(17) . ? Ni2 N10 1.8813(15) . ? Ni2 N8 1.8882(16) . ? N12 C50 1.474(3) . ? N12 C56 1.478(3) . ? N12 C55 1.485(2) . ? O4 C8 1.454(2) . ? O4 C7 1.454(2) . ? O8 C37 1.453(2) . ? O8 C36 1.456(2) . ? C32 N8 1.324(2) . ? C32 C33 1.405(3) . ? C32 C36 1.502(3) . ? N14 C58 1.473(3) . ? N14 C54 1.474(3) . ? N14 C53 1.484(2) . ? O9 C38 1.457(2) . ? O9 C39 1.457(2) . ? O1 N1 1.335(2) . ? N8 O6 1.3348(19) . ? C59 O10 1.456(2) . ? C59 C60 1.524(3) . ? N6 C26 1.470(3) . ? N6 C19 1.483(3) . ? N6 C24 1.486(3) . ? C8 C4 1.507(3) . ? C8 C15 1.519(3) . ? C8 C16 1.523(3) . ? C75 C80 1.405(2) . ? C75 C76 1.407(3) . ? C75 B1 1.643(3) . ? N5 C25 1.472(3) . ? N5 C21 1.476(3) . ? N5 C20 1.487(3) . ? C18 N4 1.464(3) . ? C18 C17 1.527(3) . ? N1 C1 1.322(3) . ? N7 C27 1.469(3) . ? N7 C22 1.482(3) . ? N7 C23 1.492(3) . ? N3 C3 1.326(2) . ? N3 O2 1.341(2) . ? O10 C62 1.444(3) . ? C6 O3 1.450(2) . ? C6 C2 1.501(3) . ? C6 C12 1.521(3) . ? C6 C11 1.521(3) . ? C3 C4 1.406(3) . ? C3 C7 1.496(3) . ? N13 C57 1.479(3) . ? N13 C52 1.483(3) . ? N13 C51 1.496(3) . ? C4 N4 1.314(3) . ? N10 C34 1.325(2) . ? N10 O7 1.334(2) . ? C99 C104 1.406(3) . ? C99 C100 1.408(3) . ? C99 B2 1.658(3) . ? N2 C2 1.308(2) . ? N2 C17 1.467(2) . ? O5 C28 1.442(3) . ? O5 C31 1.445(3) . ? C69 C74 1.398(3) . ? C69 C70 1.405(3) . ? C69 B1 1.648(3) . ? C100 C101 1.386(3) . ? C80 C79 1.393(3) . ? C39 C35 1.497(3) . ? C39 C47 1.515(3) . ? C39 C46 1.521(3) . ? C33 N9 1.304(3) . ? C33 C37 1.500(3) . ? O3 C5 1.456(3) . ? C78 C79 1.382(3) . ? C78 C77 1.388(3) . ? B2 C93 1.644(3) . ? B2 C105 1.645(3) . ? B2 C87 1.649(3) . ? C37 C42 1.513(3) . ? C37 C43 1.516(3) . ? C104 C103 1.387(3) . ? C35 N11 1.316(3) . ? C35 C34 1.403(3) . ? C105 C106 1.399(3) . ? C105 C110 1.406(3) . ? C36 C40 1.518(3) . ? C36 C41 1.519(3) . ? C74 C73 1.391(3) . ? C2 C1 1.409(3) . ? B1 C81 1.644(3) . ? B1 C63 1.653(3) . ? C52 C53 1.512(3) . ? C5 C1 1.499(3) . ? C5 C9 1.519(3) . ? C5 C10 1.528(3) . ? C63 C64 1.399(3) . ? C63 C68 1.401(3) . ? C81 C82 1.400(3) . ? C81 C86 1.402(3) . ? C106 C107 1.397(3) . ? C93 C98 1.405(3) . ? C93 C94 1.407(3) . ? C87 C92 1.402(3) . ? C87 C88 1.404(3) . ? C34 C38 1.502(3) . ? C88 C89 1.400(3) . ? C7 C13 1.519(3) . ? C7 C14 1.522(3) . ? C70 C71 1.388(3) . ? C94 C95 1.392(3) . ? C110 C109 1.390(3) . ? C55 C54 1.528(3) . ? C24 C23 1.500(3) . ? C92 C91 1.399(3) . ? C72 C71 1.385(3) . ? C72 C73 1.388(3) . ? C62 C61 1.516(4) . ? C98 C97 1.393(3) . ? N9 C48 1.465(3) . ? C101 C102 1.386(3) . ? C89 C90 1.380(4) . ? C102 C103 1.384(3) . ? C108 C107 1.384(3) . ? C108 C109 1.388(3) . ? C77 C76 1.384(3) . ? N11 C49 1.465(3) . ? C82 C83 1.394(3) . ? C90 C91 1.385(4) . ? C68 C67 1.394(3) . ? C31 C30 1.514(3) . ? C48 C49 1.520(3) . ? C30 C29 1.516(4) . ? C38 C45 1.509(3) . ? C38 C44 1.523(3) . ? C97 C96 1.379(3) . ? C64 C65 1.396(3) . ? C96 C95 1.383(3) . ? C28 C29 1.523(4) . ? C50 C51 1.512(3) . ? C60 C61 1.522(4) . ? C65 C66 1.381(3) . ? C86 C85 1.391(3) . ? C21 C22 1.502(4) . ? C20 C19 1.507(4) . ? C83 C84 1.375(4) . ? C66 C67 1.372(4) . ? C84 C85 1.389(4) . ? O11 C111 1.355(6) . ? O11 C114 1.447(5) . ? C111 C112 1.533(9) . ? C112 C113 1.473(8) . ? C113 C114 1.521(6) . ? O12 C119 1.387(8) . ? O12 C117 1.406(7) . ? C117 C116 1.383(8) . ? C119 C118 1.299(8) . ? O12A C19A 1.400(10) . ? O12A C17A 1.430(12) . ? C17A C116 1.453(11) . ? C19A C118 1.346(9) . ? C116 C118 1.463(6) . ? O13 C120 1.497(6) . ? O13 C122 1.527(6) . ? C120 C121 1.416(8) . ? C121 C123 1.519(9) . ? C123 C122 1.370(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 104.23(6) . . ? O1 Zn1 N5 94.64(7) . . ? O2 Zn1 N5 97.42(7) . . ? O1 Zn1 N7 166.83(6) . . ? O2 Zn1 N7 88.71(6) . . ? N5 Zn1 N7 81.05(7) . . ? O1 Zn1 N6 86.88(6) . . ? O2 Zn1 N6 168.88(6) . . ? N5 Zn1 N6 81.25(7) . . ? N7 Zn1 N6 80.17(6) . . ? O1 Zn1 O5 88.94(6) . . ? O2 Zn1 O5 87.18(6) . . ? N5 Zn1 O5 173.28(6) . . ? N7 Zn1 O5 94.22(6) . . ? N6 Zn1 O5 93.29(6) . . ? O6 Zn2 O7 104.33(5) . . ? O6 Zn2 N12 92.49(6) . . ? O7 Zn2 N12 92.66(6) . . ? O6 Zn2 N14 168.47(6) . . ? O7 Zn2 N14 85.64(6) . . ? N12 Zn2 N14 81.11(6) . . ? O6 Zn2 N13 89.78(6) . . ? O7 Zn2 N13 165.11(6) . . ? N12 Zn2 N13 81.82(7) . . ? N14 Zn2 N13 79.86(6) . . ? O6 Zn2 O10 87.43(6) . . ? O7 Zn2 O10 89.67(6) . . ? N12 Zn2 O10 177.61(6) . . ? N14 Zn2 O10 98.55(6) . . ? N13 Zn2 O10 95.79(6) . . ? N2 Ni1 N4 83.77(7) . . ? N2 Ni1 N3 169.77(7) . . ? N4 Ni1 N3 86.08(7) . . ? N2 Ni1 N1 85.67(7) . . ? N4 Ni1 N1 169.39(7) . . ? N3 Ni1 N1 104.45(7) . . ? N9 Ni2 N11 83.51(8) . . ? N9 Ni2 N10 168.99(7) . . ? N11 Ni2 N10 85.78(7) . . ? N9 Ni2 N8 85.54(7) . . ? N11 Ni2 N8 168.12(7) . . ? N10 Ni2 N8 104.92(7) . . ? C50 N12 C56 109.70(17) . . ? C50 N12 C55 113.25(16) . . ? C56 N12 C55 111.00(17) . . ? C50 N12 Zn2 102.01(13) . . ? C56 N12 Zn2 110.43(13) . . ? C55 N12 Zn2 110.13(12) . . ? C8 O4 C7 113.80(14) . . ? C37 O8 C36 114.09(14) . . ? N8 C32 C33 115.06(17) . . ? N8 C32 C36 134.36(17) . . ? C33 C32 C36 110.55(16) . . ? C58 N14 C54 109.51(15) . . ? C58 N14 C53 109.76(16) . . ? C54 N14 C53 111.69(15) . . ? C58 N14 Zn2 113.68(12) . . ? C54 N14 Zn2 102.02(11) . . ? C53 N14 Zn2 110.02(11) . . ? C38 O9 C39 113.91(15) . . ? N1 O1 Zn1 123.99(11) . . ? C32 N8 O6 117.21(15) . . ? C32 N8 Ni2 110.69(12) . . ? O6 N8 Ni2 131.77(12) . . ? O10 C59 C60 105.92(18) . . ? C26 N6 C19 109.49(19) . . ? C26 N6 C24 107.89(18) . . ? C19 N6 C24 112.22(18) . . ? C26 N6 Zn1 116.32(13) . . ? C19 N6 Zn1 108.22(14) . . ? C24 N6 Zn1 102.62(12) . . ? O4 C8 C4 102.99(15) . . ? O4 C8 C15 107.05(16) . . ? C4 C8 C15 113.21(17) . . ? O4 C8 C16 109.33(17) . . ? C4 C8 C16 112.67(17) . . ? C15 C8 C16 111.07(18) . . ? C80 C75 C76 114.76(17) . . ? C80 C75 B1 123.37(17) . . ? C76 C75 B1 121.83(16) . . ? C25 N5 C21 112.7(2) . . ? C25 N5 C20 110.1(2) . . ? C21 N5 C20 111.68(19) . . ? C25 N5 Zn1 109.80(13) . . ? C21 N5 Zn1 109.77(14) . . ? C20 N5 Zn1 102.33(14) . . ? N4 C18 C17 106.72(15) . . ? C1 N1 O1 117.67(15) . . ? C1 N1 Ni1 110.63(12) . . ? O1 N1 Ni1 131.58(13) . . ? C27 N7 C22 108.00(18) . . ? C27 N7 C23 109.37(17) . . ? C22 N7 C23 111.70(17) . . ? C27 N7 Zn1 116.15(13) . . ? C22 N7 Zn1 101.89(13) . . ? C23 N7 Zn1 109.56(13) . . ? C3 N3 O2 117.49(16) . . ? C3 N3 Ni1 110.38(13) . . ? O2 N3 Ni1 132.07(12) . . ? C62 O10 C59 105.83(15) . . ? C62 O10 Zn2 125.01(13) . . ? C59 O10 Zn2 123.21(12) . . ? N3 O2 Zn1 123.25(11) . . ? O3 C6 C2 102.90(15) . . ? O3 C6 C12 107.44(17) . . ? C2 C6 C12 112.96(18) . . ? O3 C6 C11 108.89(17) . . ? C2 C6 C11 112.91(17) . . ? C12 C6 C11 111.20(19) . . ? N8 O6 Zn2 120.81(11) . . ? N3 C3 C4 115.86(17) . . ? N3 C3 C7 133.07(18) . . ? C4 C3 C7 110.93(16) . . ? C57 N13 C52 109.22(17) . . ? C57 N13 C51 109.17(16) . . ? C52 N13 C51 112.15(15) . . ? C57 N13 Zn2 116.05(12) . . ? C52 N13 Zn2 103.41(12) . . ? C51 N13 Zn2 106.81(13) . . ? N4 C4 C3 115.15(17) . . ? N4 C4 C8 135.67(18) . . ? C3 C4 C8 109.16(17) . . ? C34 N10 O7 118.21(15) . . ? C34 N10 Ni2 110.68(12) . . ? O7 N10 Ni2 131.11(12) . . ? C104 C99 C100 114.39(18) . . ? C104 C99 B2 124.65(17) . . ? C100 C99 B2 120.96(16) . . ? C2 N2 C17 128.40(17) . . ? C2 N2 Ni1 112.99(13) . . ? C17 N2 Ni1 118.05(12) . . ? N10 O7 Zn2 122.38(11) . . ? C28 O5 C31 104.19(16) . . ? C28 O5 Zn1 119.79(13) . . ? C31 O5 Zn1 121.48(13) . . ? C74 C69 C70 114.85(18) . . ? C74 C69 B1 122.84(17) . . ? C70 C69 B1 122.10(18) . . ? C101 C100 C99 123.27(18) . . ? C4 N4 C18 128.50(16) . . ? C4 N4 Ni1 112.36(13) . . ? C18 N4 Ni1 117.86(12) . . ? C79 C80 C75 122.84(18) . . ? O9 C39 C35 102.54(15) . . ? O9 C39 C47 107.40(17) . . ? C35 C39 C47 113.42(18) . . ? O9 C39 C46 109.77(18) . . ? C35 C39 C46 112.56(18) . . ? C47 C39 C46 110.68(18) . . ? N9 C33 C32 115.69(17) . . ? N9 C33 C37 134.50(17) . . ? C32 C33 C37 109.80(17) . . ? C6 O3 C5 114.53(15) . . ? C79 C78 C77 118.56(19) . . ? C93 B2 C105 109.29(16) . . ? C93 B2 C87 110.20(16) . . ? C105 B2 C87 108.56(15) . . ? C93 B2 C99 110.27(15) . . ? C105 B2 C99 109.08(16) . . ? C87 B2 C99 109.41(16) . . ? O8 C37 C33 102.51(14) . . ? O8 C37 C42 107.01(17) . . ? C33 C37 C42 113.33(18) . . ? O8 C37 C43 110.01(17) . . ? C33 C37 C43 111.50(18) . . ? C42 C37 C43 111.94(17) . . ? C103 C104 C99 122.87(19) . . ? N11 C35 C34 115.21(18) . . ? N11 C35 C39 134.79(18) . . ? C34 C35 C39 109.94(17) . . ? C106 C105 C110 115.19(18) . . ? C106 C105 B2 122.91(17) . . ? C110 C105 B2 121.81(17) . . ? O8 C36 C32 102.02(15) . . ? O8 C36 C40 108.17(17) . . ? C32 C36 C40 112.77(18) . . ? O8 C36 C41 108.28(16) . . ? C32 C36 C41 113.03(18) . . ? C40 C36 C41 111.89(19) . . ? C73 C74 C69 122.94(19) . . ? N2 C2 C1 115.19(18) . . ? N2 C2 C6 135.20(18) . . ? C1 C2 C6 109.61(16) . . ? N2 C17 C18 106.99(15) . . ? C75 B1 C81 109.08(16) . . ? C75 B1 C69 107.78(15) . . ? C81 B1 C69 111.38(16) . . ? C75 B1 C63 110.44(16) . . ? C81 B1 C63 107.91(15) . . ? C69 B1 C63 110.25(16) . . ? N13 C52 C53 111.43(17) . . ? O3 C5 C1 102.16(15) . . ? O3 C5 C9 108.42(18) . . ? C1 C5 C9 112.87(18) . . ? O3 C5 C10 107.83(18) . . ? C1 C5 C10 113.32(18) . . ? C9 C5 C10 111.59(18) . . ? C64 C63 C68 115.04(19) . . ? C64 C63 B1 122.79(17) . . ? C68 C63 B1 122.17(19) . . ? C82 C81 C86 115.0(2) . . ? C82 C81 B1 123.05(19) . . ? C86 C81 B1 121.73(19) . . ? C107 C106 C105 122.86(18) . . ? C98 C93 C94 114.71(18) . . ? C98 C93 B2 123.80(17) . . ? C94 C93 B2 121.49(18) . . ? C92 C87 C88 115.10(18) . . ? C92 C87 B2 122.98(18) . . ? C88 C87 B2 121.81(18) . . ? N10 C34 C35 115.39(17) . . ? N10 C34 C38 133.71(17) . . ? C35 C34 C38 110.62(17) . . ? N1 C1 C2 115.49(17) . . ? N1 C1 C5 133.72(18) . . ? C2 C1 C5 110.77(17) . . ? C89 C88 C87 123.0(2) . . ? O4 C7 C3 102.57(16) . . ? O4 C7 C13 107.54(17) . . ? C3 C7 C13 112.88(18) . . ? O4 C7 C14 109.06(18) . . ? C3 C7 C14 112.06(17) . . ? C13 C7 C14 112.1(2) . . ? C78 C79 C80 120.37(18) . . ? C71 C70 C69 123.1(2) . . ? C95 C94 C93 122.9(2) . . ? C109 C110 C105 122.85(19) . . ? N12 C55 C54 111.58(16) . . ? N6 C24 C23 112.25(18) . . ? C91 C92 C87 122.5(2) . . ? C71 C72 C73 118.5(2) . . ? O10 C62 C61 105.57(18) . . ? C97 C98 C93 122.8(2) . . ? C33 N9 C48 129.14(17) . . ? C33 N9 Ni2 112.82(13) . . ? C48 N9 Ni2 117.76(14) . . ? C100 C101 C102 120.3(2) . . ? N14 C54 C55 112.10(16) . . ? C90 C89 C88 120.0(2) . . ? C103 C102 C101 118.3(2) . . ? C107 C108 C109 119.16(19) . . ? C72 C73 C74 120.4(2) . . ? N14 C53 C52 111.55(15) . . ? C76 C77 C78 120.53(19) . . ? C35 N11 C49 127.29(18) . . ? C35 N11 Ni2 112.30(13) . . ? C49 N11 Ni2 118.22(13) . . ? C83 C82 C81 122.9(2) . . ? C89 C90 C91 119.0(2) . . ? C67 C68 C63 122.3(2) . . ? O5 C31 C30 105.40(18) . . ? N9 C48 C49 106.45(17) . . ? C31 C30 C29 104.02(19) . . ? O9 C38 C34 102.05(15) . . ? O9 C38 C45 107.75(18) . . ? C34 C38 C45 114.53(19) . . ? O9 C38 C44 108.99(18) . . ? C34 C38 C44 111.70(19) . . ? C45 C38 C44 111.2(2) . . ? C77 C76 C75 122.92(18) . . ? C96 C97 C98 120.5(2) . . ? C65 C64 C63 123.0(2) . . ? C97 C96 C95 118.7(2) . . ? C72 C71 C70 120.23(19) . . ? C96 C95 C94 120.3(2) . . ? N11 C49 C48 106.92(17) . . ? O5 C28 C29 105.39(18) . . ? C108 C107 C106 119.93(19) . . ? N12 C50 C51 112.07(17) . . ? C90 C91 C92 120.4(2) . . ? C61 C60 C59 105.31(19) . . ? C108 C109 C110 120.0(2) . . ? C66 C65 C64 119.9(2) . . ? C85 C86 C81 123.0(2) . . ? N5 C21 C22 112.25(19) . . ? N5 C20 C19 113.0(2) . . ? C102 C103 C104 120.80(19) . . ? N13 C51 C50 112.14(16) . . ? C84 C83 C82 120.0(2) . . ? C67 C66 C65 118.9(2) . . ? N7 C22 C21 113.3(2) . . ? C62 C61 C60 104.6(2) . . ? N6 C19 C20 112.11(19) . . ? C66 C67 C68 120.9(2) . . ? C30 C29 C28 104.9(2) . . ? C83 C84 C85 119.4(2) . . ? C84 C85 C86 119.7(3) . . ? N7 C23 C24 112.13(18) . . ? C111 O11 C114 107.9(4) . . ? O11 C111 C112 108.8(5) . . ? C113 C112 C111 105.0(5) . . ? C112 C113 C114 101.1(5) . . ? O11 C114 C113 105.9(4) . . ? C119 O12 C117 102.5(6) . . ? C116 C117 O12 109.2(5) . . ? C118 C119 O12 110.5(6) . . ? C19A O12A C17A 105.9(6) . . ? O12A C17A C116 108.9(7) . . ? C118 C19A O12A 111.6(6) . . ? C117 C116 C17A 37.5(6) . . ? C117 C116 C118 104.3(5) . . ? C17A C116 C118 104.0(6) . . ? C119 C118 C19A 48.6(5) . . ? C119 C118 C116 105.3(6) . . ? C19A C118 C116 109.0(5) . . ? C120 O13 C122 103.0(3) . . ? C121 C120 O13 101.2(5) . . ? C120 C121 C123 111.1(4) . . ? C122 C123 C121 104.3(4) . . ? C123 C122 O13 106.4(4) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.305 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.095 data_complex12 _database_code_depnum_ccdc_archive 'CCDC 895619' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(PPh3)Ni(TMFdoen)Zn(Me3TACN)]BPh4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H100 B N7 Ni O6 P Zn' _chemical_formula_weight 1385.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.7065(12) _cell_length_b 13.6234(7) _cell_length_c 24.0450(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.533(3) _cell_angle_gamma 90.00 _cell_volume 7110.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9705 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 35.66 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2884 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7419 _exptl_absorpt_correction_T_max 0.9734 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 217603 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 37.58 _reflns_number_total 34190 _reflns_number_gt 20225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+3.4407P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 34190 _refine_ls_number_parameters 858 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.681702(9) 0.287235(15) 0.131179(7) 0.01226(4) Uani 1 1 d . . . Ni2 Ni 0.849644(10) 0.274101(17) 0.110398(8) 0.01291(5) Uani 1 1 d . . . P1 P 0.85436(2) 0.11167(3) 0.119679(18) 0.01497(8) Uani 1 1 d . . . N6 N 0.63519(7) 0.21611(12) 0.20025(6) 0.0168(3) Uani 1 1 d . . . N7 N 0.60263(7) 0.21752(11) 0.08540(6) 0.0158(3) Uani 1 1 d . . . N5 N 0.61791(7) 0.40091(12) 0.14198(6) 0.0172(3) Uani 1 1 d . . . N1 N 0.80571(6) 0.33287(11) 0.17448(6) 0.0134(3) Uani 1 1 d . . . O2 O 0.72178(5) 0.30848(11) 0.05911(5) 0.0189(3) Uani 1 1 d . . . N3 N 0.78338(6) 0.30804(11) 0.05448(6) 0.0130(3) Uani 1 1 d . . . C52 C 0.55315(8) 0.78038(13) 0.06099(7) 0.0145(3) Uani 1 1 d . . . O1 O 0.74585(5) 0.32790(10) 0.18779(5) 0.0178(2) Uani 1 1 d . . . N2 N 0.92085(7) 0.34036(12) 0.14764(6) 0.0160(3) Uani 1 1 d . . . N4 N 0.90237(6) 0.30896(11) 0.04579(6) 0.0146(3) Uani 1 1 d . . . C58 C 0.57867(8) 0.76506(12) 0.17136(7) 0.0147(3) Uani 1 1 d . . . C46 C 0.47179(8) 0.84478(12) 0.13635(6) 0.0132(3) Uani 1 1 d . . . C64 C 0.48956(8) 0.65258(12) 0.12359(7) 0.0140(3) Uani 1 1 d . . . C8 C 0.88856(8) 0.37845(14) -0.05372(7) 0.0181(3) Uani 1 1 d . . . C63 C 0.56344(8) 0.77016(13) 0.22808(7) 0.0177(3) Uani 1 1 d . . . H63 H 0.5211 0.7739 0.2376 0.021 Uiso 1 1 calc R . . C3 C 0.80574(7) 0.33451(12) 0.00629(6) 0.0131(3) Uani 1 1 d . . . C23 C 0.55225(8) 0.29137(14) 0.08386(7) 0.0193(3) Uani 1 1 d . . . H23A H 0.5222 0.2765 0.1134 0.023 Uiso 1 1 calc R . . H23B H 0.5304 0.2876 0.0476 0.023 Uiso 1 1 calc R . . C1 C 0.84299(8) 0.37518(14) 0.21034(7) 0.0162(3) Uani 1 1 d . . . C51 C 0.48664(8) 0.93455(13) 0.16234(7) 0.0165(3) Uani 1 1 d . . . H51 H 0.5282 0.9462 0.1731 0.020 Uiso 1 1 calc R . . C4 C 0.87164(8) 0.33711(13) 0.00258(7) 0.0145(3) Uani 1 1 d . . . C34 C 0.80003(8) 0.05057(13) 0.07315(7) 0.0174(3) Uani 1 1 d . . . C56 C 0.61355(9) 0.72200(14) -0.01846(8) 0.0218(4) Uani 1 1 d . . . H56 H 0.6383 0.6721 -0.0345 0.026 Uiso 1 1 calc R . . C20 C 0.61724(8) 0.30566(15) 0.23140(7) 0.0198(4) Uani 1 1 d . . . H20C H 0.6547 0.3364 0.2475 0.024 Uiso 1 1 calc R . . H20D H 0.5901 0.2867 0.2625 0.024 Uiso 1 1 calc R . . C53 C 0.54355(8) 0.86692(14) 0.03040(7) 0.0172(3) Uani 1 1 d . . . H53 H 0.5202 0.9182 0.0466 0.021 Uiso 1 1 calc R . . C2 C 0.90601(8) 0.38177(14) 0.19416(7) 0.0176(3) Uani 1 1 d . . . C57 C 0.58922(9) 0.70885(14) 0.03426(7) 0.0197(3) Uani 1 1 d . . . H57 H 0.5973 0.6489 0.0531 0.024 Uiso 1 1 calc R . . O3 O 0.89203(7) 0.47393(13) 0.27478(6) 0.0304(3) Uani 1 1 d . . . C65 C 0.46229(8) 0.61303(14) 0.07534(7) 0.0185(3) Uani 1 1 d . . . H65 H 0.4679 0.6465 0.0411 0.022 Uiso 1 1 calc R . . C68 C 0.44471(8) 0.51190(13) 0.17298(7) 0.0181(3) Uani 1 1 d . . . H68 H 0.4391 0.4776 0.2070 0.022 Uiso 1 1 calc R . . C24 C 0.57734(8) 0.39446(15) 0.09221(7) 0.0202(3) Uani 1 1 d . . . H24A H 0.6009 0.4141 0.0589 0.024 Uiso 1 1 calc R . . H24B H 0.5426 0.4408 0.0963 0.024 Uiso 1 1 calc R . . C7 C 0.77668(8) 0.37352(14) -0.04623(7) 0.0169(3) Uani 1 1 d . . . C40 C 0.92813(8) 0.05594(14) 0.10069(7) 0.0183(3) Uani 1 1 d . . . C67 C 0.41784(9) 0.47685(14) 0.12453(8) 0.0204(3) Uani 1 1 d . . . H67 H 0.3932 0.4192 0.1250 0.024 Uiso 1 1 calc R . . C47 C 0.40963(8) 0.83375(14) 0.12120(7) 0.0166(3) Uani 1 1 d . . . H47 H 0.3971 0.7748 0.1033 0.020 Uiso 1 1 calc R . . C17 C 0.97649(8) 0.36105(16) 0.11578(7) 0.0209(4) Uani 1 1 d . . . H17C H 1.0129 0.3320 0.1346 0.025 Uiso 1 1 calc R . . H17D H 0.9828 0.4328 0.1128 0.025 Uiso 1 1 calc R . . C21 C 0.58113(8) 0.15887(14) 0.18069(7) 0.0183(3) Uani 1 1 d . . . H21E H 0.5433 0.1982 0.1859 0.022 Uiso 1 1 calc R . . H21F H 0.5774 0.0985 0.2033 0.022 Uiso 1 1 calc R . . C69 C 0.48008(8) 0.59759(13) 0.17220(7) 0.0161(3) Uani 1 1 d . . . H69 H 0.4985 0.6196 0.2060 0.019 Uiso 1 1 calc R . . C39 C 0.80499(9) 0.07462(14) 0.01663(7) 0.0201(3) Uani 1 1 d . . . H39 H 0.8367 0.1177 0.0049 0.024 Uiso 1 1 calc R . . C49 C 0.38174(8) 0.99256(14) 0.15784(7) 0.0188(3) Uani 1 1 d . . . H49 H 0.3516 1.0411 0.1655 0.023 Uiso 1 1 calc R . . C18 C 0.96805(8) 0.31563(15) 0.05701(7) 0.0178(3) Uani 1 1 d . . . H18A H 0.9881 0.3575 0.0288 0.021 Uiso 1 1 calc R . . H18B H 0.9870 0.2496 0.0557 0.021 Uiso 1 1 calc R . . C5 C 0.83262(9) 0.42760(16) 0.26434(7) 0.0219(4) Uani 1 1 d . . . C28 C 0.84482(8) 0.05368(14) 0.18771(7) 0.0190(3) Uani 1 1 d . . . C55 C 0.60188(9) 0.80758(15) -0.04777(7) 0.0213(4) Uani 1 1 d . . . H55 H 0.6175 0.8161 -0.0842 0.026 Uiso 1 1 calc R . . C59 C 0.64205(9) 0.76214(15) 0.16050(8) 0.0233(4) Uani 1 1 d . . . H59 H 0.6553 0.7589 0.1230 0.028 Uiso 1 1 calc R . . C66 C 0.42754(9) 0.52742(14) 0.07524(8) 0.0213(4) Uani 1 1 d . . . H66 H 0.4104 0.5034 0.0414 0.026 Uiso 1 1 calc R . . C62 C 0.60683(10) 0.76997(15) 0.27084(8) 0.0253(4) Uani 1 1 d . . . H62 H 0.5941 0.7721 0.3085 0.030 Uiso 1 1 calc R . . C6 C 0.94080(9) 0.43828(16) 0.23908(8) 0.0245(4) Uani 1 1 d . . . O4 O 0.82968(6) 0.39667(13) -0.07986(6) 0.0321(4) Uani 1 1 d . . . C50 C 0.44297(8) 1.00700(13) 0.17296(7) 0.0185(3) Uani 1 1 d . . . H50 H 0.4551 1.0664 0.1906 0.022 Uiso 1 1 calc R . . C48 C 0.36559(8) 0.90569(15) 0.13134(7) 0.0197(3) Uani 1 1 d . . . H48 H 0.3241 0.8952 0.1200 0.024 Uiso 1 1 calc R . . C35 C 0.75256(9) -0.01205(15) 0.08948(8) 0.0227(4) Uani 1 1 d . . . H35 H 0.7483 -0.0290 0.1276 0.027 Uiso 1 1 calc R . . C22 C 0.58689(9) 0.13110(14) 0.11963(7) 0.0200(3) Uani 1 1 d . . . H22A H 0.6193 0.0805 0.1156 0.024 Uiso 1 1 calc R . . H22B H 0.5475 0.1028 0.1062 0.024 Uiso 1 1 calc R . . C26 C 0.67490(9) 0.15396(16) 0.23631(8) 0.0257(4) Uani 1 1 d . . . H26C H 0.7119 0.1908 0.2472 0.038 Uiso 1 1 calc R . . H26D H 0.6869 0.0948 0.2159 0.038 Uiso 1 1 calc R . . H26E H 0.6522 0.1352 0.2697 0.038 Uiso 1 1 calc R . . C25 C 0.64776(10) 0.49771(15) 0.14433(9) 0.0252(4) Uani 1 1 d . . . H25F H 0.6717 0.5080 0.1105 0.038 Uiso 1 1 calc R . . H25G H 0.6752 0.5008 0.1769 0.038 Uiso 1 1 calc R . . H25H H 0.6162 0.5489 0.1472 0.038 Uiso 1 1 calc R . . C27 C 0.61733(9) 0.18534(16) 0.02840(7) 0.0244(4) Uani 1 1 d . . . H27I H 0.5826 0.1479 0.0130 0.037 Uiso 1 1 calc R . . H27J H 0.6542 0.1439 0.0293 0.037 Uiso 1 1 calc R . . H27K H 0.6249 0.2429 0.0050 0.037 Uiso 1 1 calc R . . C45 C 0.98121(9) 0.09552(16) 0.12547(8) 0.0242(4) Uani 1 1 d . . . H45 H 0.9777 0.1509 0.1493 0.029 Uiso 1 1 calc R . . C19 C 0.58388(9) 0.38056(15) 0.19497(7) 0.0210(4) Uani 1 1 d . . . H19A H 0.5422 0.3557 0.1858 0.025 Uiso 1 1 calc R . . H19B H 0.5792 0.4426 0.2160 0.025 Uiso 1 1 calc R . . C41 C 0.93414(10) -0.02519(16) 0.06581(8) 0.0246(4) Uani 1 1 d . . . H41 H 0.8987 -0.0531 0.0486 0.030 Uiso 1 1 calc R . . C54 C 0.56703(9) 0.88065(15) -0.02311(7) 0.0202(3) Uani 1 1 d . . . H54 H 0.5591 0.9401 -0.0425 0.024 Uiso 1 1 calc R . . C38 C 0.76423(10) 0.03622(16) -0.02201(8) 0.0259(4) Uani 1 1 d . . . H38 H 0.7684 0.0523 -0.0602 0.031 Uiso 1 1 calc R . . C36 C 0.71150(10) -0.04968(16) 0.05034(10) 0.0290(4) Uani 1 1 d . . . H36 H 0.6793 -0.0922 0.0618 0.035 Uiso 1 1 calc R . . C33 C 0.85394(11) -0.04670(16) 0.19546(8) 0.0277(4) Uani 1 1 d . . . H33 H 0.8633 -0.0873 0.1646 0.033 Uiso 1 1 calc R . . C44 C 1.03871(10) 0.05515(18) 0.11585(9) 0.0299(5) Uani 1 1 d . . . H44 H 1.0744 0.0824 0.1331 0.036 Uiso 1 1 calc R . . C29 C 0.83258(9) 0.11225(16) 0.23363(7) 0.0235(4) Uani 1 1 d . . . H29 H 0.8267 0.1809 0.2289 0.028 Uiso 1 1 calc R . . C14 C 0.73800(11) 0.29833(18) -0.07717(8) 0.0294(5) Uani 1 1 d . . . H14C H 0.7222 0.3272 -0.1118 0.044 Uiso 1 1 calc R . . H14D H 0.7034 0.2782 -0.0539 0.044 Uiso 1 1 calc R . . H14E H 0.7634 0.2409 -0.0858 0.044 Uiso 1 1 calc R . . C31 C 0.83697(10) -0.02836(18) 0.29386(8) 0.0310(5) Uani 1 1 d . . . H31 H 0.8341 -0.0564 0.3299 0.037 Uiso 1 1 calc R . . C11 C 0.97640(11) 0.52732(19) 0.21893(10) 0.0361(5) Uani 1 1 d . . . H11A H 0.9499 0.5671 0.1946 0.054 Uiso 1 1 calc R . . H11B H 1.0126 0.5056 0.1982 0.054 Uiso 1 1 calc R . . H11C H 0.9897 0.5667 0.2510 0.054 Uiso 1 1 calc R . . C30 C 0.82880(11) 0.07095(18) 0.28673(8) 0.0297(5) Uani 1 1 d . . . H30 H 0.8206 0.1115 0.3179 0.036 Uiso 1 1 calc R . . C61 C 0.66879(11) 0.7667(2) 0.25819(10) 0.0367(5) Uani 1 1 d . . . H61 H 0.6990 0.7664 0.2870 0.044 Uiso 1 1 calc R . . C32 C 0.84940(12) -0.08763(17) 0.24829(9) 0.0331(5) Uani 1 1 d . . . H32 H 0.8548 -0.1563 0.2532 0.040 Uiso 1 1 calc R . . C43 C 1.04390(10) -0.02493(19) 0.08106(9) 0.0342(5) Uani 1 1 d . . . H43 H 1.0833 -0.0525 0.0742 0.041 Uiso 1 1 calc R . . C42 C 0.99219(11) -0.06541(18) 0.05612(9) 0.0326(5) Uani 1 1 d . . . H42 H 0.9962 -0.1207 0.0324 0.039 Uiso 1 1 calc R . . C10 C 0.81785(11) 0.35755(19) 0.31176(8) 0.0315(5) Uani 1 1 d . . . H10D H 0.8489 0.3054 0.3133 0.047 Uiso 1 1 calc R . . H10E H 0.7771 0.3285 0.3055 0.047 Uiso 1 1 calc R . . H10F H 0.8180 0.3937 0.3470 0.047 Uiso 1 1 calc R . . C12 C 0.98231(10) 0.3678(2) 0.27142(9) 0.0333(5) Uani 1 1 d . . . H12G H 1.0009 0.4022 0.3032 0.050 Uiso 1 1 calc R . . H12H H 1.0149 0.3435 0.2470 0.050 Uiso 1 1 calc R . . H12I H 0.9578 0.3123 0.2848 0.050 Uiso 1 1 calc R . . C15 C 0.92280(11) 0.47566(17) -0.04962(9) 0.0333(5) Uani 1 1 d . . . H15J H 0.9199 0.5101 -0.0853 0.050 Uiso 1 1 calc R . . H15K H 0.9662 0.4633 -0.0404 0.050 Uiso 1 1 calc R . . H15L H 0.9043 0.5161 -0.0205 0.050 Uiso 1 1 calc R . . C16 C 0.92376(12) 0.30536(19) -0.08880(9) 0.0350(5) Uani 1 1 d . . . H16M H 0.9006 0.2437 -0.0911 0.052 Uiso 1 1 calc R . . H16N H 0.9642 0.2931 -0.0717 0.052 Uiso 1 1 calc R . . H16O H 0.9292 0.3321 -0.1263 0.052 Uiso 1 1 calc R . . C37 C 0.71732(10) -0.02549(17) -0.00533(10) 0.0306(5) Uani 1 1 d . . . H37 H 0.6891 -0.0513 -0.0320 0.037 Uiso 1 1 calc R . . C60 C 0.68613(10) 0.7638(2) 0.20294(10) 0.0368(5) Uani 1 1 d . . . H60 H 0.7286 0.7629 0.1939 0.044 Uiso 1 1 calc R . . C9 C 0.78474(11) 0.50897(18) 0.26056(9) 0.0336(5) Uani 1 1 d . . . H9A H 0.7857 0.5478 0.2949 0.050 Uiso 1 1 calc R . . H9B H 0.7437 0.4800 0.2555 0.050 Uiso 1 1 calc R . . H9C H 0.7939 0.5515 0.2288 0.050 Uiso 1 1 calc R . . C13 C 0.74065(12) 0.46751(19) -0.03667(9) 0.0367(6) Uani 1 1 d . . . H13D H 0.7670 0.5154 -0.0175 0.055 Uiso 1 1 calc R . . H13E H 0.7046 0.4533 -0.0138 0.055 Uiso 1 1 calc R . . H13F H 0.7271 0.4945 -0.0725 0.055 Uiso 1 1 calc R . . B1 B 0.52431(9) 0.76066(14) 0.12304(7) 0.0135(3) Uani 1 1 d . . . C73 C 0.79864(13) 0.6349(2) 0.09604(13) 0.0450(6) Uani 1 1 d . . . H73A H 0.7657 0.6169 0.1224 0.054 Uiso 1 1 calc R . . H73B H 0.7803 0.6450 0.0586 0.054 Uiso 1 1 calc R . . C72 C 0.83340(14) 0.7246(2) 0.11542(17) 0.0590(9) Uani 1 1 d . . . H72C H 0.8152 0.7850 0.0994 0.071 Uiso 1 1 calc R . . H72D H 0.8332 0.7296 0.1565 0.071 Uiso 1 1 calc R . . C71 C 0.89750(13) 0.7088(2) 0.09452(14) 0.0476(7) Uani 1 1 d . . . H71E H 0.9051 0.7511 0.0618 0.057 Uiso 1 1 calc R . . H71F H 0.9280 0.7255 0.1239 0.057 Uiso 1 1 calc R . . O5 O 0.90289(9) 0.60901(15) 0.07967(9) 0.0530(5) Uani 1 1 d . . . C74 C 0.84767(13) 0.55976(18) 0.09497(12) 0.0432(6) Uani 1 1 d . . . H74G H 0.8525 0.5290 0.1321 0.052 Uiso 1 1 calc R . . H74H H 0.8374 0.5079 0.0676 0.052 Uiso 1 1 calc R . . O6 O 0.12789(10) 0.27360(17) 0.11672(10) 0.0596(6) Uani 1 1 d . . . C76 C 0.17887(17) 0.2298(3) 0.14398(16) 0.0664(10) Uani 1 1 d . . . H76A H 0.2047 0.2811 0.1617 0.080 Uiso 1 1 calc R . . H76B H 0.1643 0.1848 0.1734 0.080 Uiso 1 1 calc R . . C77 C 0.2138(2) 0.1771(5) 0.10478(17) 0.123(2) Uani 1 1 d . . . H77A H 0.2002 0.1079 0.1023 0.148 Uiso 1 1 calc R . . H77B H 0.2583 0.1790 0.1142 0.148 Uiso 1 1 calc R . . C78 C 0.2000(2) 0.2335(4) 0.0496(2) 0.1013(17) Uani 1 1 d . . . H78A H 0.2265 0.2922 0.0458 0.122 Uiso 1 1 calc R . . H78B H 0.2049 0.1908 0.0166 0.122 Uiso 1 1 calc R . . C79 C 0.13623(18) 0.2600(3) 0.05799(16) 0.0757(12) Uani 1 1 d . . . H79A H 0.1263 0.3213 0.0377 0.091 Uiso 1 1 calc R . . H79B H 0.1088 0.2073 0.0440 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.00882(8) 0.01747(9) 0.01051(8) 0.00000(7) 0.00140(6) -0.00089(7) Ni2 0.01010(9) 0.01805(11) 0.01060(8) -0.00049(8) 0.00114(7) -0.00174(8) P1 0.01472(19) 0.0168(2) 0.01339(17) 0.00133(15) 0.00144(15) -0.00012(16) N6 0.0124(6) 0.0244(8) 0.0137(6) 0.0023(6) -0.0004(5) -0.0028(6) N7 0.0132(6) 0.0220(7) 0.0122(5) -0.0004(5) 0.0022(5) -0.0034(6) N5 0.0143(6) 0.0199(7) 0.0174(6) 0.0004(5) 0.0013(5) 0.0000(6) N1 0.0111(6) 0.0164(7) 0.0127(5) -0.0001(5) 0.0008(5) -0.0018(5) O2 0.0085(5) 0.0351(8) 0.0131(5) 0.0006(5) 0.0012(4) -0.0020(5) N3 0.0093(6) 0.0169(7) 0.0127(5) -0.0015(5) 0.0017(5) -0.0026(5) C52 0.0145(7) 0.0144(7) 0.0147(6) -0.0020(6) 0.0011(5) -0.0034(6) O1 0.0097(5) 0.0300(7) 0.0136(5) -0.0034(5) 0.0022(4) -0.0025(5) N2 0.0113(6) 0.0213(7) 0.0154(6) 0.0007(5) 0.0010(5) -0.0029(5) N4 0.0102(6) 0.0199(7) 0.0136(6) 0.0014(5) 0.0014(5) -0.0018(5) C58 0.0143(7) 0.0120(7) 0.0177(7) -0.0016(6) 0.0003(6) 0.0002(6) C46 0.0143(7) 0.0144(7) 0.0109(6) 0.0024(5) 0.0016(5) -0.0012(6) C64 0.0142(7) 0.0132(7) 0.0147(6) 0.0008(6) 0.0000(6) 0.0003(6) C8 0.0133(7) 0.0264(9) 0.0145(7) 0.0041(6) 0.0022(6) -0.0036(7) C63 0.0187(8) 0.0174(8) 0.0169(7) -0.0025(6) -0.0014(6) -0.0009(7) C3 0.0127(7) 0.0150(7) 0.0117(6) 0.0008(6) 0.0014(5) -0.0027(6) C23 0.0125(7) 0.0290(10) 0.0162(7) 0.0032(7) -0.0019(6) -0.0027(7) C1 0.0152(7) 0.0216(9) 0.0119(6) -0.0019(6) 0.0001(6) -0.0042(6) C51 0.0139(7) 0.0165(8) 0.0193(7) 0.0013(6) 0.0011(6) -0.0014(6) C4 0.0122(7) 0.0181(8) 0.0131(6) 0.0013(6) 0.0025(5) -0.0023(6) C34 0.0163(8) 0.0158(8) 0.0200(7) 0.0006(6) -0.0006(6) -0.0004(6) C56 0.0240(9) 0.0208(9) 0.0207(8) -0.0058(7) 0.0070(7) -0.0038(7) C20 0.0158(8) 0.0305(10) 0.0131(7) -0.0033(7) 0.0033(6) -0.0038(7) C53 0.0161(8) 0.0194(8) 0.0159(7) 0.0012(6) 0.0006(6) -0.0019(6) C2 0.0138(7) 0.0234(9) 0.0155(7) -0.0003(6) -0.0015(6) -0.0038(6) C57 0.0236(9) 0.0167(8) 0.0188(7) -0.0011(6) 0.0039(7) -0.0016(7) O3 0.0222(7) 0.0454(10) 0.0236(7) -0.0163(6) -0.0003(5) -0.0101(7) C65 0.0213(8) 0.0172(8) 0.0169(7) 0.0036(6) -0.0047(6) -0.0026(7) C68 0.0199(8) 0.0157(8) 0.0187(7) 0.0021(6) 0.0043(6) -0.0006(6) C24 0.0155(8) 0.0251(9) 0.0201(8) 0.0054(7) 0.0002(6) 0.0025(7) C7 0.0130(7) 0.0238(9) 0.0140(7) 0.0019(6) 0.0014(6) -0.0019(6) C40 0.0168(8) 0.0213(9) 0.0169(7) 0.0049(6) 0.0026(6) 0.0026(7) C67 0.0192(8) 0.0150(8) 0.0269(9) 0.0022(7) -0.0005(7) -0.0038(7) C47 0.0158(7) 0.0196(8) 0.0143(7) -0.0003(6) -0.0018(6) -0.0013(6) C17 0.0126(7) 0.0316(10) 0.0187(7) -0.0001(7) 0.0029(6) -0.0059(7) C21 0.0156(8) 0.0238(9) 0.0154(7) 0.0034(6) 0.0011(6) -0.0055(7) C69 0.0177(8) 0.0164(8) 0.0144(7) 0.0002(6) 0.0020(6) -0.0002(6) C39 0.0224(9) 0.0201(9) 0.0178(7) 0.0010(7) -0.0006(7) -0.0030(7) C49 0.0180(8) 0.0198(9) 0.0185(7) 0.0036(6) 0.0033(6) 0.0050(7) C18 0.0085(7) 0.0288(9) 0.0160(7) 0.0032(7) 0.0012(6) -0.0014(6) C5 0.0192(8) 0.0315(10) 0.0150(7) -0.0079(7) -0.0003(6) -0.0051(8) C28 0.0181(8) 0.0233(9) 0.0156(7) 0.0038(6) 0.0016(6) 0.0013(7) C55 0.0212(8) 0.0272(10) 0.0154(7) -0.0009(7) 0.0030(6) -0.0084(7) C59 0.0153(8) 0.0286(10) 0.0260(9) -0.0032(8) 0.0010(7) -0.0001(7) C66 0.0226(9) 0.0190(9) 0.0220(8) 0.0018(7) -0.0079(7) -0.0040(7) C62 0.0299(10) 0.0253(10) 0.0206(8) -0.0042(7) -0.0062(7) 0.0030(8) C6 0.0184(8) 0.0364(11) 0.0186(8) -0.0076(8) -0.0019(7) -0.0090(8) O4 0.0129(6) 0.0627(11) 0.0208(6) 0.0218(7) -0.0003(5) -0.0058(7) C50 0.0204(8) 0.0142(8) 0.0209(8) 0.0018(6) 0.0030(6) -0.0004(6) C48 0.0133(7) 0.0258(9) 0.0200(8) 0.0041(7) -0.0013(6) 0.0022(7) C35 0.0212(9) 0.0219(9) 0.0251(9) 0.0042(7) 0.0022(7) -0.0016(7) C22 0.0199(8) 0.0206(9) 0.0193(7) -0.0003(7) 0.0006(6) -0.0072(7) C26 0.0206(9) 0.0312(11) 0.0251(9) 0.0117(8) -0.0041(7) -0.0039(8) C25 0.0252(10) 0.0189(9) 0.0316(10) -0.0007(8) 0.0005(8) -0.0004(7) C27 0.0229(9) 0.0349(11) 0.0153(7) -0.0068(7) 0.0027(7) -0.0082(8) C45 0.0202(9) 0.0277(10) 0.0247(9) 0.0068(8) -0.0023(7) 0.0023(8) C19 0.0174(8) 0.0264(10) 0.0192(7) -0.0041(7) 0.0056(6) 0.0025(7) C41 0.0246(9) 0.0261(10) 0.0231(8) -0.0005(7) 0.0013(7) 0.0044(8) C54 0.0195(8) 0.0237(9) 0.0174(7) 0.0053(7) 0.0006(6) -0.0045(7) C38 0.0297(10) 0.0256(10) 0.0221(8) -0.0009(7) -0.0060(8) -0.0031(8) C36 0.0217(9) 0.0262(10) 0.0391(11) 0.0030(9) -0.0023(8) -0.0077(8) C33 0.0366(11) 0.0249(10) 0.0217(9) 0.0048(8) 0.0038(8) 0.0037(9) C44 0.0176(9) 0.0396(13) 0.0324(10) 0.0128(9) -0.0023(8) 0.0038(8) C29 0.0280(10) 0.0270(10) 0.0155(7) 0.0031(7) 0.0011(7) 0.0018(8) C14 0.0331(11) 0.0413(13) 0.0137(7) 0.0012(8) -0.0033(7) -0.0164(9) C31 0.0324(11) 0.0409(13) 0.0196(8) 0.0120(8) 0.0023(8) 0.0017(10) C11 0.0330(12) 0.0417(14) 0.0336(11) -0.0083(10) -0.0006(9) -0.0206(10) C30 0.0348(11) 0.0385(12) 0.0158(8) 0.0040(8) 0.0031(8) 0.0005(9) C61 0.0252(10) 0.0498(15) 0.0349(11) -0.0088(10) -0.0163(9) 0.0069(10) C32 0.0443(13) 0.0276(11) 0.0274(10) 0.0128(9) 0.0036(9) 0.0041(10) C43 0.0242(10) 0.0449(14) 0.0337(11) 0.0163(10) 0.0077(9) 0.0138(10) C42 0.0347(12) 0.0345(12) 0.0287(10) 0.0001(9) 0.0075(9) 0.0143(10) C10 0.0324(11) 0.0476(14) 0.0147(8) -0.0040(8) 0.0032(8) -0.0080(10) C12 0.0237(10) 0.0505(15) 0.0254(9) -0.0039(9) -0.0069(8) -0.0025(10) C15 0.0392(12) 0.0341(12) 0.0265(10) 0.0130(9) -0.0039(9) -0.0178(10) C16 0.0387(13) 0.0481(14) 0.0182(8) -0.0016(9) 0.0074(8) 0.0103(11) C37 0.0265(10) 0.0297(11) 0.0354(11) -0.0021(9) -0.0113(9) -0.0079(9) C60 0.0141(9) 0.0554(16) 0.0407(12) -0.0085(11) -0.0049(8) 0.0025(10) C9 0.0324(11) 0.0368(12) 0.0315(11) -0.0161(9) 0.0004(9) 0.0036(10) C13 0.0466(14) 0.0385(13) 0.0248(10) 0.0043(9) -0.0053(9) 0.0193(11) B1 0.0143(8) 0.0142(8) 0.0120(7) -0.0001(6) 0.0004(6) -0.0023(6) C73 0.0382(14) 0.0370(14) 0.0598(17) -0.0112(12) 0.0001(12) -0.0080(11) C72 0.0414(15) 0.0359(15) 0.100(3) -0.0238(16) 0.0105(16) -0.0048(12) C71 0.0416(15) 0.0345(14) 0.0669(19) -0.0037(13) 0.0084(13) -0.0084(11) O5 0.0430(11) 0.0427(11) 0.0736(14) -0.0147(10) 0.0137(10) 0.0042(9) C74 0.0550(17) 0.0232(11) 0.0512(15) -0.0008(11) -0.0055(13) -0.0040(11) O6 0.0403(11) 0.0683(15) 0.0701(15) -0.0086(12) 0.0003(10) 0.0143(10) C76 0.066(2) 0.059(2) 0.074(2) -0.0049(17) -0.0174(18) 0.0250(18) C77 0.127(4) 0.188(6) 0.055(2) -0.012(3) -0.005(2) 0.115(4) C78 0.074(3) 0.144(5) 0.086(3) 0.022(3) 0.026(2) 0.050(3) C79 0.065(2) 0.103(3) 0.060(2) 0.022(2) 0.0110(18) 0.033(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.9676(12) . ? Zn1 O1 2.0158(12) . ? Zn1 N5 2.0953(15) . ? Zn1 N6 2.1790(14) . ? Zn1 N7 2.2416(15) . ? Ni2 N1 1.9880(14) . ? Ni2 N2 1.9950(15) . ? Ni2 N4 1.9955(14) . ? Ni2 N3 2.0136(14) . ? Ni2 P1 2.2263(5) . ? P1 C34 1.8196(19) . ? P1 C28 1.8301(18) . ? P1 C40 1.8338(18) . ? N6 C21 1.482(2) . ? N6 C26 1.482(2) . ? N6 C20 1.485(2) . ? N7 C27 1.477(2) . ? N7 C22 1.478(2) . ? N7 C23 1.486(2) . ? N5 C25 1.470(3) . ? N5 C24 1.482(2) . ? N5 C19 1.504(2) . ? N1 C1 1.311(2) . ? N1 O1 1.3426(18) . ? O2 N3 1.3428(18) . ? N3 C3 1.311(2) . ? C52 C53 1.404(2) . ? C52 C57 1.409(2) . ? C52 B1 1.645(2) . ? N2 C2 1.296(2) . ? N2 C17 1.463(2) . ? N4 C4 1.288(2) . ? N4 C18 1.451(2) . ? C58 C59 1.403(2) . ? C58 C63 1.408(2) . ? C58 B1 1.649(3) . ? C46 C47 1.402(2) . ? C46 C51 1.409(2) . ? C46 B1 1.650(3) . ? C64 C69 1.405(2) . ? C64 C65 1.405(2) . ? C64 B1 1.654(3) . ? C8 O4 1.441(2) . ? C8 C4 1.515(2) . ? C8 C16 1.516(3) . ? C8 C15 1.521(3) . ? C63 C62 1.388(3) . ? C3 C4 1.435(2) . ? C3 C7 1.503(2) . ? C23 C24 1.519(3) . ? C1 C2 1.429(2) . ? C1 C5 1.501(2) . ? C51 C50 1.394(3) . ? C34 C35 1.397(3) . ? C34 C39 1.403(2) . ? C56 C55 1.385(3) . ? C56 C57 1.389(2) . ? C20 C19 1.523(3) . ? C53 C54 1.401(2) . ? C2 C6 1.521(2) . ? O3 C6 1.453(2) . ? O3 C5 1.456(2) . ? C65 C66 1.389(3) . ? C68 C67 1.383(3) . ? C68 C69 1.397(3) . ? C7 O4 1.447(2) . ? C7 C14 1.515(3) . ? C7 C13 1.519(3) . ? C40 C41 1.394(3) . ? C40 C45 1.400(3) . ? C67 C66 1.389(3) . ? C47 C48 1.392(3) . ? C17 C18 1.552(3) . ? C21 C22 1.522(2) . ? C39 C38 1.380(3) . ? C49 C48 1.388(3) . ? C49 C50 1.389(3) . ? C5 C9 1.522(3) . ? C5 C10 1.523(3) . ? C28 C29 1.390(3) . ? C28 C33 1.394(3) . ? C55 C54 1.387(3) . ? C59 C60 1.393(3) . ? C62 C61 1.382(3) . ? C6 C11 1.520(3) . ? C6 C12 1.525(3) . ? C35 C36 1.388(3) . ? C45 C44 1.385(3) . ? C41 C42 1.395(3) . ? C38 C37 1.383(3) . ? C36 C37 1.385(3) . ? C33 C32 1.392(3) . ? C44 C43 1.380(4) . ? C29 C30 1.398(3) . ? C31 C30 1.375(3) . ? C31 C32 1.390(3) . ? C61 C60 1.385(3) . ? C43 C42 1.382(4) . ? C73 C74 1.477(4) . ? C73 C72 1.508(4) . ? C72 C71 1.499(4) . ? C71 O5 1.410(3) . ? O5 C74 1.425(3) . ? O6 C76 1.413(4) . ? O6 C79 1.437(4) . ? C76 C77 1.411(5) . ? C77 C78 1.560(6) . ? C78 C79 1.446(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 104.24(5) . . ? O2 Zn1 N5 107.37(6) . . ? O1 Zn1 N5 99.58(6) . . ? O2 Zn1 N6 161.54(6) . . ? O1 Zn1 N6 85.96(5) . . ? N5 Zn1 N6 85.57(6) . . ? O2 Zn1 N7 88.43(5) . . ? O1 Zn1 N7 165.70(5) . . ? N5 Zn1 N7 82.54(6) . . ? N6 Zn1 N7 80.09(5) . . ? N1 Ni2 N2 81.09(6) . . ? N1 Ni2 N4 142.22(6) . . ? N2 Ni2 N4 78.12(6) . . ? N1 Ni2 N3 94.60(6) . . ? N2 Ni2 N3 137.86(6) . . ? N4 Ni2 N3 80.61(6) . . ? N1 Ni2 P1 110.15(4) . . ? N2 Ni2 P1 111.72(5) . . ? N4 Ni2 P1 106.76(5) . . ? N3 Ni2 P1 109.09(4) . . ? C34 P1 C28 105.90(8) . . ? C34 P1 C40 102.71(8) . . ? C28 P1 C40 98.63(8) . . ? C34 P1 Ni2 111.35(6) . . ? C28 P1 Ni2 120.88(7) . . ? C40 P1 Ni2 115.21(6) . . ? C21 N6 C26 109.84(15) . . ? C21 N6 C20 112.43(14) . . ? C26 N6 C20 109.15(15) . . ? C21 N6 Zn1 111.29(10) . . ? C26 N6 Zn1 115.38(11) . . ? C20 N6 Zn1 98.32(10) . . ? C27 N7 C22 109.48(15) . . ? C27 N7 C23 110.07(15) . . ? C22 N7 C23 112.28(14) . . ? C27 N7 Zn1 114.24(11) . . ? C22 N7 Zn1 104.11(10) . . ? C23 N7 Zn1 106.57(11) . . ? C25 N5 C24 110.03(15) . . ? C25 N5 C19 110.64(15) . . ? C24 N5 C19 112.36(14) . . ? C25 N5 Zn1 112.10(12) . . ? C24 N5 Zn1 104.15(11) . . ? C19 N5 Zn1 107.40(11) . . ? C1 N1 O1 117.28(13) . . ? C1 N1 Ni2 112.91(11) . . ? O1 N1 Ni2 129.54(10) . . ? N3 O2 Zn1 121.41(10) . . ? C3 N3 O2 116.69(14) . . ? C3 N3 Ni2 112.67(11) . . ? O2 N3 Ni2 130.64(10) . . ? C53 C52 C57 114.98(15) . . ? C53 C52 B1 123.79(15) . . ? C57 C52 B1 121.23(15) . . ? N1 O1 Zn1 121.12(9) . . ? C2 N2 C17 125.51(15) . . ? C2 N2 Ni2 112.73(11) . . ? C17 N2 Ni2 119.47(11) . . ? C4 N4 C18 129.18(14) . . ? C4 N4 Ni2 113.73(11) . . ? C18 N4 Ni2 116.09(11) . . ? C59 C58 C63 114.90(16) . . ? C59 C58 B1 124.34(15) . . ? C63 C58 B1 120.75(15) . . ? C47 C46 C51 115.07(16) . . ? C47 C46 B1 122.68(15) . . ? C51 C46 B1 122.22(15) . . ? C69 C64 C65 114.75(16) . . ? C69 C64 B1 123.48(15) . . ? C65 C64 B1 121.54(14) . . ? O4 C8 C4 103.46(13) . . ? O4 C8 C16 108.67(16) . . ? C4 C8 C16 112.38(17) . . ? O4 C8 C15 108.01(17) . . ? C4 C8 C15 112.83(15) . . ? C16 C8 C15 111.06(18) . . ? C62 C63 C58 123.62(18) . . ? N3 C3 C4 116.06(14) . . ? N3 C3 C7 133.15(15) . . ? C4 C3 C7 110.48(13) . . ? N7 C23 C24 111.08(14) . . ? N1 C1 C2 115.81(15) . . ? N1 C1 C5 132.99(16) . . ? C2 C1 C5 110.95(15) . . ? C50 C51 C46 122.86(17) . . ? N4 C4 C3 116.86(14) . . ? N4 C4 C8 134.73(15) . . ? C3 C4 C8 108.35(14) . . ? C35 C34 C39 118.58(17) . . ? C35 C34 P1 125.60(14) . . ? C39 C34 P1 115.69(14) . . ? C55 C56 C57 120.24(18) . . ? N6 C20 C19 112.68(14) . . ? C54 C53 C52 122.66(17) . . ? N2 C2 C1 117.01(15) . . ? N2 C2 C6 135.00(16) . . ? C1 C2 C6 107.98(15) . . ? C56 C57 C52 122.99(18) . . ? C6 O3 C5 113.73(14) . . ? C66 C65 C64 123.22(16) . . ? C67 C68 C69 120.29(16) . . ? N5 C24 C23 111.80(15) . . ? O4 C7 C3 102.54(13) . . ? O4 C7 C14 108.23(15) . . ? C3 C7 C14 113.56(16) . . ? O4 C7 C13 108.29(17) . . ? C3 C7 C13 112.55(15) . . ? C14 C7 C13 111.12(18) . . ? C41 C40 C45 118.69(18) . . ? C41 C40 P1 124.39(15) . . ? C45 C40 P1 116.85(15) . . ? C68 C67 C66 118.79(17) . . ? C48 C47 C46 122.66(17) . . ? N2 C17 C18 107.99(14) . . ? N6 C21 C22 111.41(14) . . ? C68 C69 C64 122.78(16) . . ? C38 C39 C34 120.60(18) . . ? C48 C49 C50 118.56(17) . . ? N4 C18 C17 107.55(14) . . ? O3 C5 C1 102.47(14) . . ? O3 C5 C9 107.33(17) . . ? C1 C5 C9 113.76(16) . . ? O3 C5 C10 109.56(16) . . ? C1 C5 C10 112.57(17) . . ? C9 C5 C10 110.65(17) . . ? C29 C28 C33 119.00(17) . . ? C29 C28 P1 119.10(15) . . ? C33 C28 P1 121.73(14) . . ? C56 C55 C54 119.01(16) . . ? C60 C59 C58 122.09(19) . . ? C67 C66 C65 120.12(17) . . ? C61 C62 C63 119.47(19) . . ? O3 C6 C11 107.28(18) . . ? O3 C6 C2 103.24(14) . . ? C11 C6 C2 115.35(17) . . ? O3 C6 C12 109.85(16) . . ? C11 C6 C12 111.44(18) . . ? C2 C6 C12 109.28(18) . . ? C8 O4 C7 115.16(13) . . ? C49 C50 C51 120.18(17) . . ? C49 C48 C47 120.66(17) . . ? C36 C35 C34 120.37(18) . . ? N7 C22 C21 111.14(15) . . ? C44 C45 C40 121.0(2) . . ? N5 C19 C20 112.09(14) . . ? C40 C41 C42 120.1(2) . . ? C55 C54 C53 120.09(18) . . ? C39 C38 C37 120.29(19) . . ? C37 C36 C35 120.22(19) . . ? C32 C33 C28 120.3(2) . . ? C43 C44 C45 119.6(2) . . ? C28 C29 C30 120.5(2) . . ? C30 C31 C32 119.96(19) . . ? C31 C30 C29 120.1(2) . . ? C62 C61 C60 119.1(2) . . ? C31 C32 C33 120.2(2) . . ? C44 C43 C42 120.5(2) . . ? C43 C42 C41 120.1(2) . . ? C38 C37 C36 119.93(19) . . ? C61 C60 C59 120.8(2) . . ? C52 B1 C58 110.92(14) . . ? C52 B1 C46 109.39(14) . . ? C58 B1 C46 109.22(13) . . ? C52 B1 C64 109.27(13) . . ? C58 B1 C64 110.48(14) . . ? C46 B1 C64 107.50(13) . . ? C74 C73 C72 102.0(2) . . ? C71 C72 C73 104.1(2) . . ? O5 C71 C72 107.6(2) . . ? C71 O5 C74 108.4(2) . . ? O5 C74 C73 106.6(2) . . ? C76 O6 C79 107.2(3) . . ? C77 C76 O6 109.2(3) . . ? C76 C77 C78 102.5(3) . . ? C79 C78 C77 100.4(3) . . ? O6 C79 C78 107.4(3) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.924 _refine_diff_density_min -1.123 _refine_diff_density_rms 0.100 data_complex13 _database_code_depnum_ccdc_archive 'CCDC 895620' #TrackingRef 'web_deposit_cif_file_0_ChristopherUyeda_1344540614.X-ray_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common complex13 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H74 B N7 Ni O5 Zn' _chemical_formula_weight 1048.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.2117(13) _cell_length_b 12.9449(10) _cell_length_c 24.7109(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.430(3) _cell_angle_gamma 90.00 _cell_volume 5396.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9971 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.51 _exptl_crystal_description leaf _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6869 _exptl_absorpt_correction_T_max 0.9589 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 72415 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.57 _reflns_number_total 14374 _reflns_number_gt 7797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+4.7723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14374 _refine_ls_number_parameters 659 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1534 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1929 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn01 Zn 0.25888(2) 0.74270(3) 0.095079(17) 0.02963(13) Uani 1 1 d . A 4 Ni02 Ni 0.04294(3) 0.77422(4) 0.03877(2) 0.03625(16) Uani 1 1 d . A 4 O1 O 0.20487(14) 0.7932(2) 0.01997(10) 0.0325(6) Uani 1 1 d . A 4 C004 C 0.3935(2) 0.2628(2) 0.15452(15) 0.0233(7) Uani 1 1 d . B 4 O2 O 0.16914(16) 0.7356(3) 0.13691(12) 0.0511(8) Uani 1 1 d . A 4 N4 N -0.0528(2) 0.7519(3) 0.06277(15) 0.0493(10) Uani 1 1 d . A 4 N3 N 0.0930(2) 0.7377(3) 0.11270(14) 0.0445(9) Uani 1 1 d . A 4 B1 B 0.4638(2) 0.2592(3) 0.11801(16) 0.0209(8) Uani 1 1 d . B 4 C009 C 0.3451(2) 0.2373(3) -0.03627(15) 0.0308(8) Uani 1 1 d . B 4 H009 H 0.3142 0.1863 -0.0583 0.037 Uiso 1 1 calc R B 4 C010 C 0.5170(2) 0.0819(3) 0.16944(14) 0.0249(7) Uani 1 1 d . B 4 H010 H 0.4951 0.1045 0.1998 0.030 Uiso 1 1 calc R B 4 C011 C 0.5217(2) 0.4321(3) 0.17141(14) 0.0259(8) Uani 1 1 d . B 4 H011 H 0.4699 0.4444 0.1779 0.031 Uiso 1 1 calc R B 4 C012 C 0.42573(19) 0.2880(2) 0.05319(14) 0.0211(7) Uani 1 1 d . B 4 N1 N 0.12668(17) 0.8036(3) 0.00229(13) 0.0347(8) Uani 1 1 d . A 4 C014 C 0.5352(2) 0.3430(2) 0.14269(13) 0.0223(7) Uani 1 1 d . B 4 O3 O 0.07756(15) 0.8944(3) -0.13626(10) 0.0447(8) Uani 1 1 d . A 4 C016 C 0.3564(2) 0.3328(3) -0.05859(15) 0.0306(8) Uani 1 1 d . B 4 H016 H 0.3340 0.3475 -0.0961 0.037 Uiso 1 1 calc R B 4 C017 C 0.5814(2) 0.5036(3) 0.19093(15) 0.0284(8) Uani 1 1 d . B 4 H017 H 0.5697 0.5629 0.2106 0.034 Uiso 1 1 calc R B 4 C018 C 0.50500(19) 0.1429(2) 0.12182(14) 0.0224(7) Uani 1 1 d . B 4 N2 N -0.02254(18) 0.8112(3) -0.02678(13) 0.0425(9) Uani 1 1 d . A 4 C020 C 0.3790(2) 0.2159(3) 0.01815(15) 0.0268(8) Uani 1 1 d . B 4 H020 H 0.3703 0.1498 0.0326 0.032 Uiso 1 1 calc R B 4 C021 C 0.43412(19) 0.3842(3) 0.02882(15) 0.0251(7) Uani 1 1 d . B 4 H021 H 0.4641 0.4364 0.0506 0.030 Uiso 1 1 calc R B 4 C022 C 0.3127(2) 0.2632(3) 0.13136(18) 0.0374(9) Uani 1 1 d . B 4 H022 H 0.2970 0.2640 0.0923 0.045 Uiso 1 1 calc R B 4 C023 C 0.6570(2) 0.4889(3) 0.18183(15) 0.0288(8) Uani 1 1 d . B 4 H023 H 0.6978 0.5372 0.1952 0.035 Uiso 1 1 calc R B 4 C024 C 0.5595(2) -0.0105(3) 0.17466(15) 0.0281(8) Uani 1 1 d . B 4 H024 H 0.5670 -0.0483 0.2082 0.034 Uiso 1 1 calc R B 4 N7 N 0.37255(18) 0.7309(3) 0.06851(13) 0.0348(8) Uani 1 1 d . A 4 C026 C 0.6723(2) 0.4026(3) 0.15298(16) 0.0330(9) Uani 1 1 d . B 4 H026 H 0.7239 0.3918 0.1458 0.040 Uiso 1 1 calc R B 4 C027 C 0.4109(2) 0.2629(3) 0.21254(16) 0.0309(8) Uani 1 1 d . B 4 H027 H 0.4649 0.2648 0.2308 0.037 Uiso 1 1 calc R B 4 C028 C 0.5906(2) -0.0468(3) 0.13093(15) 0.0305(8) Uani 1 1 d . B 4 H028 H 0.6201 -0.1092 0.1341 0.037 Uiso 1 1 calc R B 4 C029 C 0.5778(2) 0.0092(3) 0.08256(16) 0.0309(8) Uani 1 1 d . B 4 H029 H 0.5976 -0.0158 0.0518 0.037 Uiso 1 1 calc R B 4 C030 C 0.6127(2) 0.3311(3) 0.13435(15) 0.0291(8) Uani 1 1 d . B 4 H030 H 0.6252 0.2717 0.1152 0.035 Uiso 1 1 calc R B 4 C031 C 0.4005(2) 0.4064(3) -0.02568(15) 0.0302(8) Uani 1 1 d . B 4 H031 H 0.4078 0.4726 -0.0404 0.036 Uiso 1 1 calc R B 4 C032 C 0.3534(3) 0.2605(3) 0.24446(18) 0.0380(10) Uani 1 1 d . B 4 H032 H 0.3682 0.2598 0.2836 0.046 Uiso 1 1 calc R B 4 C033 C 0.2742(3) 0.2591(3) 0.2192(2) 0.0516(12) Uani 1 1 d . B 4 H033 H 0.2341 0.2560 0.2406 0.062 Uiso 1 1 calc R B 4 N5 N 0.3020(2) 0.8965(3) 0.11927(13) 0.0389(8) Uani 1 1 d . A 4 C035 C 0.5366(2) 0.1015(3) 0.07846(15) 0.0290(8) Uani 1 1 d . B 4 H035 H 0.5293 0.1385 0.0446 0.035 Uiso 1 1 calc R B 4 C036 C 0.4138(3) 0.6737(4) 0.16541(17) 0.0465(11) Uani 1 1 d . A 4 H03A H 0.4530 0.7268 0.1815 0.056 Uiso 1 1 calc R A 4 H03B H 0.4293 0.6084 0.1855 0.056 Uiso 1 1 calc R A 4 N6 N 0.3365(2) 0.7047(3) 0.17598(14) 0.0450(9) Uani 1 1 d . A 4 O5 O 0.2225(2) 0.5787(3) 0.06401(18) 0.0718(11) Uani 1 1 d . A 4 C17 C -0.1006(3) 0.8075(5) -0.02468(19) 0.0602(14) Uani 1 1 d . A 4 H039 H -0.1403 0.8283 -0.0552 0.072 Uiso 1 1 calc R A 4 C040 C 0.2546(3) 0.2624(4) 0.1625(2) 0.0549(13) Uani 1 1 d . B 4 H040 H 0.2004 0.2641 0.1446 0.066 Uiso 1 1 calc R B 4 C5 C 0.1449(2) 0.8697(4) -0.09173(16) 0.0434(11) Uani 1 1 d . A 4 C042 C 0.3578(3) 0.9194(4) 0.0829(2) 0.0523(12) Uani 1 1 d . A 4 H04A H 0.3271 0.9448 0.0472 0.063 Uiso 1 1 calc R A 4 H04B H 0.3930 0.9763 0.0996 0.063 Uiso 1 1 calc R A 4 C18 C -0.1198(3) 0.7728(4) 0.02282(19) 0.0571(14) Uani 1 1 d . A 4 H043 H -0.1726 0.7640 0.0281 0.068 Uiso 1 1 calc R A 4 C3 C 0.0398(3) 0.7175(5) 0.1419(2) 0.0671(17) Uani 1 1 d . A 4 C55 C 0.3696(3) 0.6859(5) 0.0138(2) 0.0617(14) Uani 1 1 d . A 4 H55A H 0.3391 0.7312 -0.0144 0.093 Uiso 1 1 calc R A 4 H55B H 0.3441 0.6179 0.0120 0.093 Uiso 1 1 calc R A 4 H55C H 0.4236 0.6784 0.0072 0.093 Uiso 1 1 calc R A 4 C1 C 0.1026(2) 0.8384(5) -0.04658(18) 0.0564(14) Uani 1 1 d . A 4 C047 C 0.2359(3) 0.9706(4) 0.1111(3) 0.0812(19) Uani 1 1 d . A 4 H04D H 0.2565 1.0401 0.1212 0.122 Uiso 1 1 calc R A 4 H04E H 0.1983 0.9511 0.1343 0.122 Uiso 1 1 calc R A 4 H04F H 0.2090 0.9701 0.0722 0.122 Uiso 1 1 calc R A 4 C4 C -0.0417(3) 0.7250(5) 0.1137(2) 0.0711(18) Uani 1 1 d . A 4 C7 C 0.0446(3) 0.6922(7) 0.2023(2) 0.098(3) Uani 1 1 d . A 4 C8 C -0.0940(3) 0.7007(7) 0.1535(2) 0.096(3) Uani 1 1 d . A 4 O4 O -0.0389(2) 0.6900(5) 0.20600(15) 0.1130(19) Uani 1 1 d . A 4 C21 C 0.3453(4) 0.8917(5) 0.1778(2) 0.085(2) Uani 1 1 d . A 4 H21A H 0.4024 0.9026 0.1785 0.102 Uiso 1 1 calc R A 4 H21B H 0.3270 0.9498 0.1982 0.102 Uiso 1 1 calc R A 4 C22 C 0.3366(4) 0.7980(5) 0.2069(2) 0.0743(19) Uani 1 1 d . A 4 H22A H 0.3804 0.7942 0.2396 0.089 Uiso 1 1 calc R A 4 H22B H 0.2864 0.8018 0.2205 0.089 Uiso 1 1 calc R A 4 C24 C 0.4201(3) 0.6586(6) 0.1084(2) 0.089(2) Uani 1 1 d . A 4 H24A H 0.4035 0.5871 0.0975 0.107 Uiso 1 1 calc R A 4 H24B H 0.4765 0.6655 0.1057 0.107 Uiso 1 1 calc R A 4 C25 C 0.4072(4) 0.8342(5) 0.0717(3) 0.085(2) Uani 1 1 d . A 4 H25A H 0.4557 0.8335 0.1009 0.102 Uiso 1 1 calc R A 4 H25B H 0.4238 0.8484 0.0363 0.102 Uiso 1 1 calc R A 4 C31 C 0.1971(4) 0.5494(5) 0.0068(3) 0.091(2) Uani 1 1 d . A 4 H31A H 0.2286 0.4903 -0.0024 0.109 Uiso 1 1 calc R A 4 H31B H 0.2030 0.6079 -0.0179 0.109 Uiso 1 1 calc R A 4 C32 C 0.1100(4) 0.5194(6) 0.0010(4) 0.115(3) Uani 1 1 d . A 4 H32A H 0.0751 0.5798 -0.0101 0.137 Uiso 1 1 calc R A 4 H32B H 0.0955 0.4640 -0.0267 0.137 Uiso 1 1 calc R A 4 C33 C 0.1032(5) 0.4825(6) 0.0571(5) 0.138(4) Uani 1 1 d . A 4 H33A H 0.0914 0.4076 0.0564 0.165 Uiso 1 1 calc R A 4 H33B H 0.0605 0.5199 0.0705 0.165 Uiso 1 1 calc R A 4 C34 C 0.1851(4) 0.5051(5) 0.0948(4) 0.126(3) Uani 1 1 d . A 4 H34A H 0.1784 0.5349 0.1305 0.151 Uiso 1 1 calc R A 4 H34B H 0.2170 0.4412 0.1021 0.151 Uiso 1 1 calc R A 4 C13 C 0.0787(4) 0.5857(7) 0.2182(3) 0.130(4) Uani 1 1 d . A 4 H13A H 0.0718 0.5688 0.2556 0.195 Uiso 1 1 calc R A 4 H13B H 0.1353 0.5853 0.2171 0.195 Uiso 1 1 calc R A 4 H13C H 0.0511 0.5344 0.1922 0.195 Uiso 1 1 calc R A 4 C14 C 0.0847(5) 0.7778(8) 0.2396(2) 0.140(4) Uani 1 1 d . A 4 H14A H 0.0566 0.8430 0.2296 0.210 Uiso 1 1 calc R A 4 H14B H 0.1398 0.7848 0.2352 0.210 Uiso 1 1 calc R A 4 H14C H 0.0836 0.7610 0.2781 0.210 Uiso 1 1 calc R A 4 C15 C -0.1397(4) 0.6008(8) 0.1409(4) 0.154(5) Uani 1 1 d . A 4 H15A H -0.1029 0.5445 0.1376 0.231 Uiso 1 1 calc R A 4 H15B H -0.1782 0.6079 0.1061 0.231 Uiso 1 1 calc R A 4 H15C H -0.1678 0.5852 0.1708 0.231 Uiso 1 1 calc R A 4 C16 C -0.1489(4) 0.7895(9) 0.1597(3) 0.147(4) Uani 1 1 d . A 4 H16A H -0.1817 0.7707 0.1865 0.221 Uiso 1 1 calc R A 4 H16B H -0.1832 0.8043 0.1239 0.221 Uiso 1 1 calc R A 4 H16C H -0.1174 0.8509 0.1728 0.221 Uiso 1 1 calc R A 4 C27 C 0.3084(4) 0.6194(7) 0.2073(3) 0.122(3) Uani 1 1 d . . . H27A H 0.3429 0.6140 0.2438 0.183 Uiso 1 1 calc R A 4 H27B H 0.3098 0.5543 0.1872 0.183 Uiso 1 1 calc R A 4 H27C H 0.2540 0.6335 0.2115 0.183 Uiso 1 1 calc R A 4 C6 C 0.0028(3) 0.8762(6) -0.1200(2) 0.088(2) Uani 1 1 d . . . C9 C 0.1960(3) 0.9629(5) -0.0785(2) 0.0715(17) Uani 1 1 d . . . H9A H 0.2125 0.9873 -0.1121 0.107 Uiso 1 1 calc R A 4 H9B H 0.2430 0.9452 -0.0507 0.107 Uiso 1 1 calc R A 4 H9C H 0.1662 1.0175 -0.0642 0.107 Uiso 1 1 calc R A 4 C10 C 0.1913(3) 0.7813(5) -0.1119(2) 0.0739(17) Uani 1 1 d . . . C11 C -0.0620(3) 0.9030(6) -0.1611(2) 0.083(2) Uani 1 1 d . A . H11A H -0.0615 0.8613 -0.1942 0.124 Uiso 1 1 calc R . . H11B H -0.0587 0.9764 -0.1701 0.124 Uiso 1 1 calc R . . H11C H -0.1111 0.8901 -0.1479 0.124 Uiso 1 1 calc R . . C12 C -0.0101(5) 0.7413(7) -0.1376(4) 0.045(3) Uani 0.474(9) 1 d P A 1 H12A H -0.0645 0.7136 -0.1491 0.054 Uiso 0.474(9) 1 calc PR A 1 H12B H 0.0322 0.7047 -0.1518 0.054 Uiso 0.474(9) 1 calc PR A 1 C2 C 0.0152(6) 0.8107(12) -0.0735(5) 0.050(3) Uani 0.474(9) 1 d P A 1 C12A C -0.0040(6) 1.0023(9) -0.0865(5) 0.088(5) Uani 0.526(9) 1 d P A 2 H12C H 0.0404 1.0518 -0.0840 0.105 Uiso 0.526(9) 1 calc PR A 2 H12D H -0.0570 1.0323 -0.0868 0.105 Uiso 0.526(9) 1 calc PR A 2 C2A C 0.0159(5) 0.8776(8) -0.0618(3) 0.033(2) Uani 0.526(9) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn01 0.0225(2) 0.0397(3) 0.0248(2) 0.00571(19) -0.00003(17) -0.00095(17) Ni02 0.0217(3) 0.0625(4) 0.0241(3) 0.0106(2) 0.0036(2) 0.0026(2) O1 0.0216(13) 0.0536(16) 0.0208(13) 0.0033(12) 0.0004(10) 0.0036(11) C004 0.0281(18) 0.0168(16) 0.0257(19) -0.0016(14) 0.0068(15) -0.0013(13) O2 0.0237(15) 0.092(2) 0.0339(16) 0.0277(16) -0.0021(12) -0.0019(14) N4 0.0261(18) 0.086(3) 0.036(2) 0.021(2) 0.0084(15) 0.0036(17) N3 0.0265(18) 0.076(3) 0.0292(19) 0.0204(18) 0.0022(14) -0.0012(16) B1 0.0219(19) 0.0203(18) 0.0196(19) 0.0024(15) 0.0017(15) 0.0005(14) C009 0.031(2) 0.032(2) 0.027(2) -0.0041(16) -0.0012(16) 0.0008(15) C010 0.0279(19) 0.0238(17) 0.0213(19) -0.0019(14) 0.0011(15) -0.0037(14) C011 0.0214(18) 0.0264(18) 0.029(2) 0.0024(15) 0.0016(15) 0.0006(13) C012 0.0208(16) 0.0222(16) 0.0204(17) -0.0005(14) 0.0044(13) 0.0021(13) N1 0.0194(16) 0.058(2) 0.0251(17) 0.0041(16) 0.0002(13) 0.0035(14) C014 0.0260(18) 0.0231(17) 0.0161(17) 0.0043(14) 0.0002(14) -0.0019(13) O3 0.0246(14) 0.090(2) 0.0189(14) 0.0097(14) 0.0034(11) 0.0114(14) C016 0.0259(19) 0.046(2) 0.0196(19) 0.0073(17) 0.0028(15) 0.0071(16) C017 0.035(2) 0.0218(17) 0.027(2) 0.0005(15) 0.0020(16) 0.0005(14) C018 0.0236(18) 0.0208(16) 0.0216(18) 0.0005(14) 0.0017(14) -0.0030(13) N2 0.0224(17) 0.080(3) 0.0241(18) 0.0088(18) 0.0032(13) 0.0101(17) C020 0.032(2) 0.0201(16) 0.028(2) 0.0038(15) 0.0032(16) -0.0006(14) C021 0.0214(17) 0.0232(17) 0.030(2) 0.0037(15) 0.0043(15) -0.0016(13) C022 0.031(2) 0.047(2) 0.035(2) -0.0013(18) 0.0089(17) -0.0032(17) C023 0.0288(19) 0.0302(19) 0.025(2) 0.0077(16) -0.0014(15) -0.0086(15) C024 0.033(2) 0.0264(18) 0.0217(19) 0.0036(15) -0.0031(15) -0.0023(15) N7 0.0257(17) 0.052(2) 0.0248(17) 0.0004(15) 0.0020(13) 0.0037(14) C026 0.027(2) 0.039(2) 0.034(2) -0.0006(18) 0.0089(16) -0.0052(16) C027 0.043(2) 0.0244(18) 0.027(2) -0.0019(15) 0.0115(17) 0.0017(15) C028 0.034(2) 0.0239(18) 0.033(2) 0.0016(16) 0.0054(17) 0.0023(15) C029 0.038(2) 0.0294(19) 0.028(2) 0.0004(16) 0.0129(17) 0.0022(16) C030 0.034(2) 0.0297(19) 0.026(2) -0.0046(16) 0.0123(16) -0.0052(15) C031 0.029(2) 0.0297(19) 0.032(2) 0.0122(16) 0.0057(16) 0.0025(15) C032 0.059(3) 0.028(2) 0.032(2) -0.0047(17) 0.020(2) -0.0011(18) C033 0.056(3) 0.057(3) 0.053(3) -0.008(2) 0.037(3) -0.012(2) N5 0.044(2) 0.045(2) 0.0268(18) -0.0065(15) 0.0034(15) -0.0031(16) C035 0.038(2) 0.0248(18) 0.026(2) 0.0057(15) 0.0089(16) 0.0016(15) C036 0.044(3) 0.060(3) 0.033(2) 0.007(2) 0.0028(19) 0.022(2) N6 0.032(2) 0.067(2) 0.034(2) 0.0215(18) 0.0025(16) 0.0069(17) O5 0.063(2) 0.048(2) 0.102(3) 0.001(2) 0.009(2) -0.0143(17) C17 0.024(2) 0.118(5) 0.037(3) 0.018(3) 0.0020(19) 0.009(2) C040 0.031(2) 0.081(4) 0.055(3) -0.008(3) 0.014(2) -0.007(2) C5 0.023(2) 0.084(3) 0.022(2) 0.009(2) 0.0019(16) 0.008(2) C042 0.060(3) 0.046(3) 0.052(3) 0.011(2) 0.013(2) -0.011(2) C18 0.026(2) 0.108(4) 0.038(3) 0.018(3) 0.0063(19) 0.003(2) C3 0.033(3) 0.128(5) 0.039(3) 0.041(3) 0.006(2) 0.004(3) C55 0.038(3) 0.095(4) 0.052(3) -0.030(3) 0.008(2) 0.010(3) C1 0.023(2) 0.113(4) 0.032(2) 0.021(3) 0.0005(18) 0.007(2) C047 0.067(4) 0.052(3) 0.123(5) -0.032(3) 0.015(4) 0.018(3) C4 0.033(3) 0.137(5) 0.043(3) 0.043(3) 0.008(2) 0.002(3) C7 0.041(3) 0.204(8) 0.051(4) 0.065(5) 0.016(3) 0.009(4) C8 0.036(3) 0.200(8) 0.055(4) 0.071(4) 0.018(3) 0.014(4) O4 0.043(2) 0.247(6) 0.054(2) 0.076(3) 0.0219(19) 0.015(3) C21 0.131(6) 0.091(4) 0.034(3) -0.026(3) 0.015(3) -0.061(4) C22 0.085(4) 0.098(5) 0.032(3) -0.014(3) -0.008(3) 0.049(4) C24 0.052(3) 0.168(7) 0.047(3) 0.035(4) 0.011(3) 0.056(4) C25 0.086(4) 0.086(4) 0.104(5) -0.031(4) 0.066(4) -0.039(4) C31 0.068(4) 0.060(4) 0.139(6) -0.041(4) 0.008(4) -0.011(3) C32 0.068(5) 0.076(5) 0.192(9) -0.023(5) 0.007(5) -0.027(4) C33 0.103(6) 0.087(6) 0.229(12) -0.033(6) 0.048(7) -0.055(5) C34 0.085(5) 0.068(4) 0.226(10) 0.071(5) 0.031(6) -0.012(4) C13 0.056(4) 0.230(10) 0.112(6) 0.127(7) 0.033(4) 0.032(5) C14 0.085(5) 0.310(13) 0.027(3) 0.023(5) 0.017(3) -0.034(7) C15 0.063(5) 0.257(12) 0.141(7) 0.121(8) 0.015(5) -0.036(6) C16 0.075(5) 0.321(13) 0.057(4) 0.070(6) 0.039(4) 0.082(6) C27 0.057(4) 0.201(9) 0.099(5) 0.113(6) -0.005(3) -0.013(4) C6 0.020(2) 0.203(8) 0.042(3) 0.055(4) 0.003(2) 0.013(3) C9 0.042(3) 0.121(5) 0.050(3) 0.007(3) 0.006(2) -0.023(3) C10 0.036(3) 0.124(5) 0.062(3) 0.002(3) 0.011(2) 0.035(3) C11 0.033(3) 0.177(7) 0.038(3) 0.022(4) 0.006(2) 0.017(3) C12 0.030(5) 0.063(6) 0.045(6) -0.021(5) 0.015(4) -0.007(4) C2 0.028(5) 0.087(10) 0.038(6) 0.009(6) 0.015(4) 0.010(6) C12A 0.040(6) 0.080(8) 0.150(13) -0.059(8) 0.035(7) -0.007(5) C2A 0.027(4) 0.055(6) 0.018(4) -0.001(4) 0.007(3) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn01 O1 2.013(2) . ? Zn01 O2 2.024(3) . ? Zn01 N5 2.167(3) . ? Zn01 N7 2.189(3) . ? Zn01 N6 2.228(3) . ? Zn01 O5 2.302(3) . ? Ni02 N2 1.844(3) . ? Ni02 N4 1.882(3) . ? Ni02 N1 1.884(3) . ? Ni02 N3 1.918(3) . ? O1 N1 1.337(4) . ? C004 C022 1.396(5) . ? C004 C027 1.405(5) . ? C004 B1 1.647(5) . ? O2 N3 1.329(4) . ? N4 C4 1.284(6) . ? N4 C18 1.388(6) . ? N3 C3 1.298(5) . ? B1 C012 1.648(5) . ? B1 C018 1.659(5) . ? B1 C014 1.662(5) . ? C009 C016 1.382(5) . ? C009 C020 1.383(5) . ? C010 C024 1.394(5) . ? C010 C018 1.398(5) . ? C011 C017 1.396(5) . ? C011 C014 1.398(5) . ? C012 C021 1.403(5) . ? C012 C020 1.411(5) . ? N1 C1 1.279(5) . ? C014 C030 1.398(5) . ? O3 C6 1.442(5) . ? O3 C5 1.466(4) . ? C016 C031 1.378(5) . ? C017 C023 1.378(5) . ? C018 C035 1.401(5) . ? N2 C17 1.356(5) . ? C021 C031 1.386(5) . ? C022 C040 1.377(6) . ? C023 C026 1.378(5) . ? C024 C028 1.380(5) . ? N7 C25 1.459(6) . ? N7 C55 1.464(5) . ? N7 C24 1.483(6) . ? C026 C030 1.390(5) . ? C027 C032 1.383(5) . ? C028 C029 1.378(5) . ? C029 C035 1.383(5) . ? C032 C033 1.382(7) . ? C033 C040 1.375(7) . ? N5 C042 1.470(5) . ? N5 C047 1.471(6) . ? N5 C21 1.492(6) . ? C036 C24 1.447(7) . ? C036 N6 1.463(5) . ? N6 C22 1.429(7) . ? N6 C27 1.483(7) . ? O5 C31 1.444(7) . ? O5 C34 1.448(7) . ? C17 C18 1.357(6) . ? C5 C9 1.490(7) . ? C5 C1 1.503(6) . ? C5 C10 1.534(7) . ? C042 C25 1.451(7) . ? C3 C4 1.441(7) . ? C3 C7 1.516(7) . ? C4 C8 1.493(7) . ? C7 O4 1.459(6) . ? C7 C14 1.517(12) . ? C7 C13 1.519(11) . ? C8 O4 1.453(7) . ? C8 C15 1.514(12) . ? C8 C16 1.515(11) . ? C21 C22 1.432(8) . ? C31 C32 1.529(8) . ? C32 C33 1.492(12) . ? C33 C34 1.556(11) . ? C6 C11 1.395(6) . ? C6 C2 1.410(12) . ? C6 C2A 1.411(9) . ? C6 C12 1.803(12) . ? C6 C12A 1.844(12) . ? C12 C2 1.797(16) . ? C12A C2A 1.736(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn01 O2 103.05(10) . . ? O1 Zn01 N5 91.51(12) . . ? O2 Zn01 N5 98.92(13) . . ? O1 Zn01 N7 91.32(11) . . ? O2 Zn01 N7 165.49(12) . . ? N5 Zn01 N7 82.49(13) . . ? O1 Zn01 N6 169.78(12) . . ? O2 Zn01 N6 85.08(12) . . ? N5 Zn01 N6 81.00(14) . . ? N7 Zn01 N6 80.86(12) . . ? O1 Zn01 O5 86.94(13) . . ? O2 Zn01 O5 86.80(14) . . ? N5 Zn01 O5 174.28(13) . . ? N7 Zn01 O5 92.04(13) . . ? N6 Zn01 O5 99.83(15) . . ? N2 Ni02 N4 84.00(15) . . ? N2 Ni02 N1 85.39(13) . . ? N4 Ni02 N1 169.39(14) . . ? N2 Ni02 N3 169.00(14) . . ? N4 Ni02 N3 85.30(15) . . ? N1 Ni02 N3 105.30(14) . . ? N1 O1 Zn01 125.8(2) . . ? C022 C004 C027 114.3(3) . . ? C022 C004 B1 123.8(3) . . ? C027 C004 B1 121.9(3) . . ? N3 O2 Zn01 123.6(2) . . ? C4 N4 C18 133.8(4) . . ? C4 N4 Ni02 112.4(3) . . ? C18 N4 Ni02 113.7(3) . . ? C3 N3 O2 119.1(3) . . ? C3 N3 Ni02 110.2(3) . . ? O2 N3 Ni02 130.6(3) . . ? C004 B1 C012 109.4(3) . . ? C004 B1 C018 110.3(3) . . ? C012 B1 C018 110.1(3) . . ? C004 B1 C014 110.6(3) . . ? C012 B1 C014 109.4(3) . . ? C018 B1 C014 107.1(3) . . ? C016 C009 C020 120.1(3) . . ? C024 C010 C018 123.4(3) . . ? C017 C011 C014 122.5(3) . . ? C021 C012 C020 114.7(3) . . ? C021 C012 B1 124.2(3) . . ? C020 C012 B1 121.0(3) . . ? C1 N1 O1 117.4(3) . . ? C1 N1 Ni02 112.8(3) . . ? O1 N1 Ni02 129.7(2) . . ? C030 C014 C011 115.2(3) . . ? C030 C014 B1 122.2(3) . . ? C011 C014 B1 122.6(3) . . ? C6 O3 C5 111.8(3) . . ? C031 C016 C009 119.1(3) . . ? C023 C017 C011 120.4(3) . . ? C010 C018 C035 114.3(3) . . ? C010 C018 B1 123.4(3) . . ? C035 C018 B1 122.0(3) . . ? C17 N2 Ni02 113.3(3) . . ? C009 C020 C012 122.9(3) . . ? C031 C021 C012 122.8(3) . . ? C040 C022 C004 123.1(4) . . ? C017 C023 C026 118.7(3) . . ? C028 C024 C010 119.8(3) . . ? C25 N7 C55 110.7(4) . . ? C25 N7 C24 112.1(5) . . ? C55 N7 C24 106.0(4) . . ? C25 N7 Zn01 107.4(3) . . ? C55 N7 Zn01 115.8(3) . . ? C24 N7 Zn01 104.7(3) . . ? C023 C026 C030 120.5(3) . . ? C032 C027 C004 123.4(4) . . ? C029 C028 C024 118.7(3) . . ? C028 C029 C035 120.6(3) . . ? C026 C030 C014 122.7(3) . . ? C016 C031 C021 120.4(3) . . ? C033 C032 C027 119.7(4) . . ? C040 C033 C032 118.8(4) . . ? C042 N5 C047 111.4(4) . . ? C042 N5 C21 109.9(4) . . ? C047 N5 C21 112.6(4) . . ? C042 N5 Zn01 104.2(3) . . ? C047 N5 Zn01 110.4(3) . . ? C21 N5 Zn01 107.9(3) . . ? C029 C035 C018 123.1(3) . . ? C24 C036 N6 117.2(4) . . ? C22 N6 C036 115.0(4) . . ? C22 N6 C27 108.5(5) . . ? C036 N6 C27 106.9(4) . . ? C22 N6 Zn01 103.3(3) . . ? C036 N6 Zn01 107.8(2) . . ? C27 N6 Zn01 115.7(3) . . ? C31 O5 C34 105.2(5) . . ? C31 O5 Zn01 125.3(3) . . ? C34 O5 Zn01 123.4(5) . . ? N2 C17 C18 117.2(4) . . ? C033 C040 C022 120.7(4) . . ? O3 C5 C9 109.4(4) . . ? O3 C5 C1 100.9(3) . . ? C9 C5 C1 114.0(4) . . ? O3 C5 C10 107.7(4) . . ? C9 C5 C10 110.6(4) . . ? C1 C5 C10 113.5(4) . . ? C25 C042 N5 116.2(4) . . ? C17 C18 N4 111.7(4) . . ? N3 C3 C4 116.4(4) . . ? N3 C3 C7 133.2(4) . . ? C4 C3 C7 110.3(4) . . ? N1 C1 C5 133.0(4) . . ? N4 C4 C3 115.6(4) . . ? N4 C4 C8 135.4(4) . . ? C3 C4 C8 109.0(4) . . ? O4 C7 C3 101.8(4) . . ? O4 C7 C14 108.2(6) . . ? C3 C7 C14 111.7(6) . . ? O4 C7 C13 107.5(6) . . ? C3 C7 C13 113.2(7) . . ? C14 C7 C13 113.6(6) . . ? O4 C8 C4 103.6(4) . . ? O4 C8 C15 108.9(6) . . ? C4 C8 C15 113.6(7) . . ? O4 C8 C16 107.0(6) . . ? C4 C8 C16 112.1(6) . . ? C15 C8 C16 111.1(6) . . ? C8 O4 C7 114.8(4) . . ? C22 C21 N5 116.1(4) . . ? N6 C22 C21 115.9(4) . . ? C036 C24 N7 115.1(4) . . ? C042 C25 N7 117.3(4) . . ? O5 C31 C32 105.0(6) . . ? C33 C32 C31 104.5(7) . . ? C32 C33 C34 105.6(6) . . ? O5 C34 C33 104.7(7) . . ? C11 C6 C2 135.5(6) . . ? C11 C6 C2A 133.1(6) . . ? C2 C6 C2A 37.8(5) . . ? C11 C6 O3 112.7(4) . . ? C2 C6 O3 109.0(5) . . ? C2A C6 O3 108.1(5) . . ? C11 C6 C12 91.3(6) . . ? C2 C6 C12 66.7(7) . . ? C2A C6 C12 104.2(6) . . ? O3 C6 C12 99.5(5) . . ? C11 C6 C12A 89.7(6) . . ? C2 C6 C12A 100.4(8) . . ? C2A C6 C12A 62.8(7) . . ? O3 C6 C12A 96.9(5) . . ? C12 C6 C12A 161.8(5) . . ? C2 C12 C6 46.1(5) . . ? C6 C2 C12 67.2(6) . . ? C2A C12A C6 46.3(4) . . ? C6 C2A C12A 70.9(6) . . ? _diffrn_measured_fraction_theta_max 0.867 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.964 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.088