# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jonas Peters' _publ_contact_author_email JCPETERS@MIT.EDU _publ_section_title ; Redox rich dicobalt macrocycles as templates for multi-electron transformations ; loop_ _publ_author_name 'Louise A. Berben' 'Nathaniel Szymczak' # Attachment 'Nate combined cif.cif' data_nks3-51 _database_code_depnum_ccdc_archive 'CCDC 740044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H25 B2 Cl Co2 F4 N11 O8' _chemical_formula_weight 822.46 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' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 '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 20.2112(12) _cell_length_b 13.9739(8) _cell_length_c 12.7646(7) _cell_angle_alpha 90.00 _cell_angle_beta 120.5490(10) _cell_angle_gamma 90.00 _cell_volume 3104.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 31.50 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7461 _exptl_absorpt_correction_T_max 0.8353 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35757 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.51 _reflns_number_total 4730 _reflns_number_gt 4280 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Suspect C-C Bond in CIF: C12 -- C12 .. 1.71 Ang. Alert level A is due to apparently close coordinated acetonitrile molecules. Each C12 atom is half occupancy, so they are not really in close proximity although they appear crystallographically to be so. ; _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^)+(0.0455P)^2^+4.7314P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4730 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Co1 Co 0.271127(13) 0.636379(15) 0.94461(2) 0.02497(8) Uani 1 1 d . . . N1 N 0.29907(7) 0.76560(9) 0.92883(10) 0.0194(2) Uani 1 1 d . . . N2 N 0.22169(7) 0.65222(9) 1.04013(10) 0.0181(2) Uani 1 1 d . . . N3 N 0.25843(7) 0.50501(9) 0.96779(11) 0.0212(2) Uani 1 1 d . A . N4 N 0.32916(7) 0.60718(10) 0.86948(11) 0.0222(2) Uani 1 1 d . A . C1 C 0.33866(8) 0.76990(11) 0.86817(13) 0.0214(3) Uani 1 1 d . . . C2 C 0.35688(9) 0.67787(11) 0.83737(13) 0.0233(3) Uani 1 1 d . A . C3 C 0.22209(8) 0.48320(11) 1.02382(13) 0.0215(3) Uani 1 1 d . . . C4 C 0.20066(8) 0.56713(11) 1.06685(12) 0.0209(3) Uani 1 1 d . A . C5 C 0.35916(9) 0.85597(12) 0.83753(15) 0.0250(3) Uani 1 1 d . . . H5 H 0.3852 0.8569 0.7949 0.030 Uiso 1 1 calc R . . C6 C 0.16017(9) 0.56099(12) 1.12813(14) 0.0256(3) Uani 1 1 d . . . H6 H 0.1466 0.5019 1.1452 0.031 Uiso 1 1 calc R A . C7 C 0.20106(10) 0.38360(12) 1.03857(15) 0.0284(3) Uani 1 1 d . A . H7A H 0.1468 0.3745 0.9861 0.043 Uiso 1 1 calc R . . H7B H 0.2145 0.3737 1.1215 0.043 Uiso 1 1 calc R . . H7C H 0.2284 0.3386 1.0176 0.043 Uiso 1 1 calc R . . C8 C 0.40305(11) 0.66352(14) 0.77660(19) 0.0351(4) Uani 1 1 d . . . H8A H 0.4481 0.6267 0.8288 0.053 Uiso 1 1 calc R A . H8B H 0.4180 0.7246 0.7610 0.053 Uiso 1 1 calc R . . H8C H 0.3726 0.6301 0.7012 0.053 Uiso 1 1 calc R . . O1 O 0.33939(8) 0.51959(8) 0.83186(11) 0.0298(3) Uani 1 1 d . . . O2 O 0.27393(8) 0.42850(8) 0.91679(11) 0.0289(2) Uani 1 1 d . . . B1 B 0.34351(12) 0.43690(14) 0.90760(18) 0.0308(4) Uani 1 1 d . A . F1 F 0.34376(8) 0.35702(8) 0.84435(12) 0.0402(3) Uani 1 1 d . . . F2 F 0.40863(7) 0.44257(10) 1.02184(11) 0.0438(3) Uani 1 1 d . . . N5 N 0.16483(8) 0.65578(9) 0.78378(11) 0.0219(2) Uani 1 1 d . A . C9 C 0.03284(10) 0.69626(15) 0.59466(17) 0.0360(4) Uani 1 1 d . A . H9A H 0.0258 0.6571 0.5279 0.054 Uiso 1 1 calc R . . H9B H 0.0313 0.7625 0.5737 0.054 Uiso 1 1 calc R . . H9C H -0.0074 0.6833 0.6118 0.054 Uiso 1 1 calc R . . C11 C 0.10687(9) 0.67477(11) 0.70166(14) 0.0225(3) Uani 1 1 d . . . Cl1 Cl 0.0000 0.46363(4) 0.7500 0.03011(12) Uani 1 2 d S . . O3 O 0.07579(14) 0.4910(2) 0.7825(3) 0.0327(5) Uani 0.50 1 d P . . O4 O 0.0000 0.36345(16) 0.7500 0.0797(11) Uani 1 2 d S . . O5 O -0.00059(18) 0.4779(2) 0.8709(3) 0.0419(6) Uani 0.50 1 d P . . O6 O 0.05598(18) 0.5218(3) 0.8340(3) 0.0494(8) Uani 0.50 1 d P . . N6 N 0.39079(15) 0.63967(18) 1.1282(2) 0.0223(5) Uani 0.50 1 d P A 2 C12 C 0.4530(3) 0.6172(4) 1.1929(5) 0.0317(9) Uani 0.50 1 d P . 2 C10 C 0.5340(4) 0.5881(5) 1.2745(7) 0.0545(16) Uani 0.50 1 d P . 1 H10A H 0.5527 0.6526 1.2949 0.082 Uiso 0.50 1 calc PR . 1 H10B H 0.5494 0.5614 1.2209 0.082 Uiso 0.50 1 calc PR . 1 H10C H 0.5550 0.5504 1.3473 0.082 Uiso 0.50 1 calc PR . 1 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 Co1 0.03724(14) 0.01995(11) 0.03099(13) 0.00750(7) 0.02701(11) 0.00842(8) N1 0.0174(5) 0.0260(6) 0.0152(5) -0.0018(4) 0.0085(4) -0.0001(4) N2 0.0176(5) 0.0227(5) 0.0139(5) 0.0004(4) 0.0078(4) -0.0001(4) N3 0.0255(6) 0.0196(5) 0.0202(5) 0.0012(4) 0.0127(5) 0.0039(4) N4 0.0242(6) 0.0241(6) 0.0200(5) -0.0017(4) 0.0124(5) 0.0041(5) C1 0.0186(6) 0.0290(7) 0.0178(6) -0.0030(5) 0.0102(5) -0.0030(5) C2 0.0227(6) 0.0289(7) 0.0219(6) -0.0035(5) 0.0138(5) -0.0006(5) C3 0.0233(6) 0.0222(6) 0.0181(6) 0.0005(5) 0.0098(5) 0.0009(5) C4 0.0195(6) 0.0256(7) 0.0168(6) -0.0009(5) 0.0088(5) -0.0020(5) C5 0.0245(7) 0.0309(8) 0.0254(7) -0.0041(6) 0.0170(6) -0.0062(6) C6 0.0269(7) 0.0281(7) 0.0267(7) -0.0021(6) 0.0170(6) -0.0065(6) C7 0.0360(8) 0.0256(7) 0.0275(7) 0.0004(6) 0.0191(7) -0.0035(6) C8 0.0398(9) 0.0381(9) 0.0439(10) -0.0096(8) 0.0332(8) -0.0053(7) O1 0.0445(7) 0.0237(5) 0.0337(6) -0.0004(4) 0.0289(6) 0.0062(5) O2 0.0434(7) 0.0200(5) 0.0346(6) 0.0000(4) 0.0281(5) 0.0051(5) B1 0.0408(10) 0.0268(8) 0.0326(9) 0.0045(7) 0.0243(8) 0.0116(7) F1 0.0620(8) 0.0269(5) 0.0494(7) 0.0024(4) 0.0413(6) 0.0127(5) F2 0.0413(6) 0.0497(7) 0.0383(6) 0.0076(5) 0.0186(5) 0.0202(5) N5 0.0253(6) 0.0224(5) 0.0195(5) 0.0004(4) 0.0124(5) 0.0006(5) C9 0.0244(7) 0.0395(9) 0.0306(8) 0.0024(7) 0.0041(6) 0.0026(7) C11 0.0233(6) 0.0212(6) 0.0232(6) -0.0017(5) 0.0120(5) -0.0003(5) Cl1 0.0218(2) 0.0247(2) 0.0472(3) 0.000 0.0200(2) 0.000 O3 0.0247(11) 0.0377(13) 0.0417(14) -0.0029(11) 0.0213(11) -0.0075(10) O4 0.110(2) 0.0250(10) 0.172(4) 0.000 0.122(3) 0.000 O5 0.0495(16) 0.0497(16) 0.0428(15) -0.0061(13) 0.0355(14) -0.0101(13) O6 0.0363(15) 0.0512(18) 0.0432(16) -0.0026(14) 0.0074(13) -0.0131(13) N6 0.0227(11) 0.0242(12) 0.0187(11) 0.0010(9) 0.0096(9) 0.0013(9) C12 0.034(2) 0.025(2) 0.031(2) -0.0016(15) 0.013(2) -0.0005(16) C10 0.039(3) 0.056(4) 0.051(4) 0.010(3) 0.009(3) 0.016(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 Co1 N3 1.8976(13) . ? Co1 N4 1.8988(13) . ? Co1 N1 1.9329(13) . ? Co1 N2 1.9423(12) . ? Co1 N5 2.1023(13) . ? Co1 N6 2.363(3) . ? N1 N2 1.3494(17) 7_567 ? N1 C1 1.3686(18) . ? N2 N1 1.3494(17) 7_567 ? N2 C4 1.3630(19) . ? N3 C3 1.2953(19) . ? N3 O2 1.3682(16) . ? N4 C2 1.300(2) . ? N4 O1 1.3684(17) . ? C1 C5 1.391(2) . ? C1 C2 1.446(2) . ? C2 C8 1.500(2) . ? C3 C4 1.451(2) . ? C3 C7 1.495(2) . ? C4 C6 1.393(2) . ? C5 C6 1.366(2) 7_567 ? C6 C5 1.366(2) 7_567 ? O1 B1 1.482(2) . ? O2 B1 1.474(2) . ? B1 F1 1.379(2) . ? B1 F2 1.383(2) . ? N5 C11 1.137(2) . ? C9 C11 1.455(2) . ? Cl1 O6 1.363(3) . ? Cl1 O6 1.363(3) 2_556 ? Cl1 O4 1.400(2) . ? Cl1 O3 1.421(2) 2_556 ? Cl1 O3 1.421(2) . ? Cl1 O5 1.563(3) . ? Cl1 O5 1.563(3) 2_556 ? O3 O6 1.023(4) . ? O3 O5 1.776(4) 2_556 ? O5 O6 1.566(4) . ? O5 O3 1.776(4) 2_556 ? N6 C12 1.143(6) . ? C12 C12 1.708(12) 2_657 ? C10 C10 1.186(14) 2_657 ? 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 N3 Co1 N4 92.18(6) . . ? N3 Co1 N1 171.86(5) . . ? N4 Co1 N1 81.95(6) . . ? N3 Co1 N2 81.88(5) . . ? N4 Co1 N2 171.30(5) . . ? N1 Co1 N2 103.28(5) . . ? N3 Co1 N5 97.18(5) . . ? N4 Co1 N5 96.98(5) . . ? N1 Co1 N5 89.17(5) . . ? N2 Co1 N5 90.11(5) . . ? N3 Co1 N6 90.89(7) . . ? N4 Co1 N6 85.49(8) . . ? N1 Co1 N6 83.06(7) . . ? N2 Co1 N6 88.22(7) . . ? N5 Co1 N6 171.44(7) . . ? N2 N1 C1 119.16(13) 7_567 . ? N2 N1 Co1 127.85(9) 7_567 . ? C1 N1 Co1 112.69(10) . . ? N1 N2 C4 119.07(12) 7_567 . ? N1 N2 Co1 128.12(10) 7_567 . ? C4 N2 Co1 112.52(10) . . ? C3 N3 O2 114.21(12) . . ? C3 N3 Co1 118.25(10) . . ? O2 N3 Co1 126.87(10) . . ? C2 N4 O1 113.74(12) . . ? C2 N4 Co1 118.14(11) . . ? O1 N4 Co1 127.72(10) . . ? N1 C1 C5 122.70(14) . . ? N1 C1 C2 114.69(13) . . ? C5 C1 C2 122.61(13) . . ? N4 C2 C1 112.32(13) . . ? N4 C2 C8 122.86(15) . . ? C1 C2 C8 124.81(14) . . ? N3 C3 C4 112.39(13) . . ? N3 C3 C7 124.46(14) . . ? C4 C3 C7 123.10(13) . . ? N2 C4 C6 122.76(14) . . ? N2 C4 C3 114.79(12) . . ? C6 C4 C3 122.43(14) . . ? C6 C5 C1 118.01(14) 7_567 . ? C5 C6 C4 118.26(14) 7_567 . ? N4 O1 B1 115.91(12) . . ? N3 O2 B1 115.72(13) . . ? F1 B1 F2 112.27(15) . . ? F1 B1 O2 105.64(16) . . ? F2 B1 O2 110.83(14) . . ? F1 B1 O1 105.36(14) . . ? F2 B1 O1 110.55(17) . . ? O2 B1 O1 112.00(14) . . ? C11 N5 Co1 173.12(13) . . ? N5 C11 C9 178.15(17) . . ? O6 Cl1 O6 106.8(3) . 2_556 ? O6 Cl1 O4 126.61(15) . . ? O6 Cl1 O4 126.61(15) 2_556 . ? O6 Cl1 O3 114.2(2) . 2_556 ? O6 Cl1 O3 43.04(18) 2_556 2_556 ? O4 Cl1 O3 105.60(12) . 2_556 ? O6 Cl1 O3 43.04(18) . . ? O6 Cl1 O3 114.2(2) 2_556 . ? O4 Cl1 O3 105.60(12) . . ? O3 Cl1 O3 148.8(2) 2_556 . ? O6 Cl1 O5 64.31(19) . . ? O6 Cl1 O5 106.3(2) 2_556 . ? O4 Cl1 O5 97.34(12) . . ? O3 Cl1 O5 72.89(16) 2_556 . ? O3 Cl1 O5 103.03(16) . . ? O6 Cl1 O5 106.3(2) . 2_556 ? O6 Cl1 O5 64.31(19) 2_556 2_556 ? O4 Cl1 O5 97.34(12) . 2_556 ? O3 Cl1 O5 103.03(16) 2_556 2_556 ? O3 Cl1 O5 72.89(16) . 2_556 ? O5 Cl1 O5 165.3(2) . 2_556 ? O6 O3 Cl1 65.5(2) . . ? O6 O3 O5 110.9(3) . 2_556 ? Cl1 O3 O5 57.25(13) . 2_556 ? Cl1 O5 O6 51.64(15) . . ? Cl1 O5 O3 49.86(12) . 2_556 ? O6 O5 O3 88.52(19) . 2_556 ? O3 O6 Cl1 71.5(2) . . ? O3 O6 O5 127.8(3) . . ? Cl1 O6 O5 64.05(17) . . ? C12 N6 Co1 155.1(3) . . ? N6 C12 C12 162.6(4) . 2_657 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.699 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.074 #===END data_nks4-44p _database_code_depnum_ccdc_archive 'CCDC 740045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H46 B2 Br4 Co2 F4 N12 O8' _chemical_formula_weight 1213.89 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _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 9.9295(7) _cell_length_b 11.0421(7) _cell_length_c 11.0924(7) _cell_angle_alpha 110.2380(10) _cell_angle_beta 99.6700(10) _cell_angle_gamma 102.1900(10) _cell_volume 1076.18(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9024 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 30.61 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 4.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 0.65 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19848 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 30.61 _reflns_number_total 6407 _reflns_number_gt 4840 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0438P)^2^+1.6829P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6407 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _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 Co1 Co 0.63679(4) 0.17281(4) 0.07426(3) 0.00761(9) Uani 1 1 d . . . Br1 Br 0.81135(3) 0.06533(3) 0.00999(3) 0.01677(8) Uani 1 1 d . . . Br2 Br 0.46655(3) 0.28531(3) 0.13996(3) 0.01712(8) Uani 1 1 d . . . N1 N 0.5132(3) 0.0746(2) -0.1079(2) 0.0082(4) Uani 1 1 d . . . N2 N 0.6947(3) 0.3041(2) 0.0054(2) 0.0110(5) Uani 1 1 d . . . N3 N 0.5802(3) 0.0481(2) 0.1604(2) 0.0086(4) Uani 1 1 d . . . N4 N 0.7645(3) 0.2781(3) 0.2460(2) 0.0102(5) Uani 1 1 d . . . N5 N -0.0151(3) 0.8584(3) 0.2230(3) 0.0206(6) Uani 1 1 d . . . N6 N 0.2991(3) 0.3010(3) 0.4134(3) 0.0228(6) Uani 1 1 d . . . C1 C 0.6349(3) 0.2799(3) -0.1160(3) 0.0106(5) Uani 1 1 d . . . C2 C 0.5342(3) 0.1455(3) -0.1848(3) 0.0100(5) Uani 1 1 d . . . C3 C 0.6527(3) 0.1003(3) 0.2906(3) 0.0094(5) Uani 1 1 d . . . C4 C 0.7569(3) 0.2325(3) 0.3381(3) 0.0101(5) Uani 1 1 d . . . C5 C 0.4626(3) 0.0937(3) -0.3204(3) 0.0110(5) Uani 1 1 d . . . H5 H 0.4798 0.1446 -0.3729 0.013 Uiso 1 1 calc R . . C6 C 0.6324(3) 0.0319(3) 0.3743(3) 0.0114(5) Uani 1 1 d . . . H6 H 0.6832 0.0717 0.4657 0.014 Uiso 1 1 calc R . . C7 C 0.8436(3) 0.3038(3) 0.4792(3) 0.0139(6) Uani 1 1 d . . . H7A H 0.9026 0.2494 0.5006 0.021 Uiso 1 1 calc R . . H7B H 0.7799 0.3173 0.5381 0.021 Uiso 1 1 calc R . . H7C H 0.9053 0.3915 0.4918 0.021 Uiso 1 1 calc R . . C8 C 0.6602(4) 0.3824(3) -0.1753(3) 0.0160(6) Uani 1 1 d . . . H8A H 0.6072 0.4473 -0.1437 0.024 Uiso 1 1 calc R . . H8B H 0.6276 0.3373 -0.2727 0.024 Uiso 1 1 calc R . . H8C H 0.7624 0.4300 -0.1486 0.024 Uiso 1 1 calc R . . C9 C -0.0256(5) 0.9780(5) 0.3246(4) 0.0428(12) Uani 1 1 d . . . H9A H 0.0683 1.0277 0.3878 0.064 Uiso 1 1 calc R . . H9B H -0.0940 0.9517 0.3717 0.064 Uiso 1 1 calc R . . H9C H -0.0581 1.0355 0.2830 0.064 Uiso 1 1 calc R . . C10 C -0.1433(4) 0.7749(4) 0.1161(4) 0.0268(8) Uani 1 1 d . . . H10A H -0.1198 0.7043 0.0482 0.040 Uiso 1 1 calc R . . H10B H -0.1817 0.8310 0.0759 0.040 Uiso 1 1 calc R . . H10C H -0.2149 0.7333 0.1521 0.040 Uiso 1 1 calc R . . C11 C 0.3336(5) 0.4246(5) 0.5315(4) 0.0426(11) Uani 1 1 d . . . H11A H 0.4171 0.4299 0.5965 0.064 Uiso 1 1 calc R . . H11B H 0.2521 0.4248 0.5706 0.064 Uiso 1 1 calc R . . H11C H 0.3548 0.5024 0.5071 0.064 Uiso 1 1 calc R . . C12 C 0.1828(5) 0.2801(6) 0.3029(4) 0.0423(12) Uani 1 1 d . . . H12A H 0.1724 0.1958 0.2282 0.063 Uiso 1 1 calc R . . H12B H 0.2034 0.3556 0.2751 0.063 Uiso 1 1 calc R . . H12C H 0.0939 0.2747 0.3309 0.063 Uiso 1 1 calc R . . C13 C 0.1057(3) 0.8243(4) 0.2292(3) 0.0181(6) Uani 1 1 d . . . H13 H 0.1057 0.7461 0.1575 0.022 Uiso 1 1 calc R . . C14 C 0.3828(4) 0.2204(3) 0.4016(3) 0.0170(6) Uani 1 1 d . . . H14 H 0.3558 0.1413 0.3219 0.020 Uiso 1 1 calc R . . B1 B 0.9014(4) 0.4515(4) 0.1854(3) 0.0190(8) Uani 1 1 d . . . F1 F 0.9966(2) 0.3906(2) 0.1310(2) 0.0276(5) Uani 1 1 d . . . F2 F 0.9589(2) 0.5885(2) 0.25394(19) 0.0295(5) Uani 1 1 d . . . O1 O 0.8574(2) 0.4013(2) 0.2852(2) 0.0146(4) Uani 1 1 d . . . O2 O 0.7772(3) 0.4326(2) 0.0799(2) 0.0178(5) Uani 1 1 d . . . O3 O 0.2179(3) 0.8837(3) 0.3184(2) 0.0242(5) Uani 1 1 d . . . O4 O 0.4925(2) 0.2397(2) 0.4854(2) 0.0177(5) 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 Co1 0.00914(18) 0.00676(18) 0.00530(15) 0.00277(14) -0.00034(12) 0.00014(14) Br1 0.01701(16) 0.01877(17) 0.01627(14) 0.00868(12) 0.00468(11) 0.00545(13) Br2 0.01817(17) 0.01790(17) 0.01424(14) 0.00511(12) 0.00276(11) 0.00646(13) N1 0.0088(11) 0.0077(12) 0.0073(9) 0.0038(9) 0.0004(8) 0.0003(9) N2 0.0122(12) 0.0047(11) 0.0111(10) 0.0013(9) -0.0009(9) -0.0009(9) N3 0.0077(11) 0.0084(12) 0.0073(9) 0.0021(9) 0.0001(8) 0.0007(9) N4 0.0108(12) 0.0077(12) 0.0103(10) 0.0039(9) 0.0008(9) 0.0001(9) N5 0.0172(14) 0.0249(16) 0.0211(13) 0.0109(12) 0.0031(11) 0.0072(12) N6 0.0242(16) 0.0306(18) 0.0199(13) 0.0114(13) 0.0078(11) 0.0164(14) C1 0.0119(14) 0.0081(14) 0.0106(12) 0.0044(11) 0.0009(10) 0.0008(11) C2 0.0115(13) 0.0090(14) 0.0087(11) 0.0042(10) 0.0013(10) 0.0016(11) C3 0.0105(13) 0.0095(14) 0.0071(11) 0.0029(10) 0.0009(9) 0.0026(11) C4 0.0099(13) 0.0092(14) 0.0084(11) 0.0030(10) -0.0009(9) 0.0006(11) C5 0.0133(14) 0.0139(15) 0.0063(11) 0.0051(11) 0.0009(10) 0.0042(12) C6 0.0138(14) 0.0125(15) 0.0068(11) 0.0033(11) 0.0016(10) 0.0037(12) C7 0.0157(15) 0.0130(15) 0.0069(11) 0.0035(11) -0.0024(10) -0.0029(12) C8 0.0209(16) 0.0107(15) 0.0135(12) 0.0072(12) -0.0008(11) -0.0013(12) C9 0.033(2) 0.050(3) 0.032(2) -0.001(2) 0.0008(17) 0.022(2) C10 0.0164(17) 0.027(2) 0.0339(19) 0.0142(16) -0.0025(14) 0.0030(15) C11 0.054(3) 0.037(3) 0.041(2) 0.008(2) 0.017(2) 0.031(2) C12 0.028(2) 0.081(4) 0.033(2) 0.033(2) 0.0089(17) 0.029(2) C13 0.0173(16) 0.0221(18) 0.0191(14) 0.0141(13) 0.0043(12) 0.0047(13) C14 0.0213(17) 0.0193(17) 0.0128(13) 0.0071(12) 0.0079(12) 0.0070(14) B1 0.0196(18) 0.0171(19) 0.0134(14) 0.0084(14) -0.0045(13) -0.0052(15) F1 0.0166(10) 0.0392(14) 0.0249(10) 0.0159(10) 0.0032(8) 0.0005(9) F2 0.0362(13) 0.0158(11) 0.0194(9) 0.0093(8) -0.0141(8) -0.0138(9) O1 0.0166(11) 0.0098(11) 0.0107(9) 0.0038(8) -0.0021(8) -0.0051(9) O2 0.0239(12) 0.0085(11) 0.0125(9) 0.0042(8) -0.0065(8) -0.0036(9) O3 0.0173(12) 0.0352(15) 0.0186(11) 0.0142(11) -0.0010(9) 0.0031(11) O4 0.0207(12) 0.0203(12) 0.0150(10) 0.0107(9) 0.0030(9) 0.0067(10) _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 Co1 N2 1.891(2) . ? Co1 N4 1.903(2) . ? Co1 N1 1.964(2) . ? Co1 N3 1.972(2) . ? Co1 Br2 2.3677(5) . ? Co1 Br1 2.3706(5) . ? N1 N3 1.333(3) 2_655 ? N1 C2 1.354(3) . ? N2 C1 1.286(3) . ? N2 O2 1.355(3) . ? N3 N1 1.333(3) 2_655 ? N3 C3 1.355(3) . ? N4 C4 1.292(3) . ? N4 O1 1.348(3) . ? N5 C13 1.330(4) . ? N5 C9 1.446(5) . ? N5 C10 1.455(4) . ? N6 C14 1.330(4) . ? N6 C12 1.451(5) . ? N6 C11 1.454(5) . ? C1 C2 1.455(4) . ? C1 C8 1.493(4) . ? C2 C5 1.403(4) . ? C3 C6 1.398(4) . ? C3 C4 1.458(4) . ? C4 C7 1.490(4) . ? C5 C6 1.362(4) 2_655 ? C5 H5 0.9500 . ? C6 C5 1.362(4) 2_655 ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O3 1.234(4) . ? C13 H13 0.9500 . ? C14 O4 1.234(4) . ? C14 H14 0.9500 . ? B1 F2 1.373(4) . ? B1 F1 1.374(5) . ? B1 O2 1.474(4) . ? B1 O1 1.486(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 N2 Co1 N4 93.81(10) . . ? N2 Co1 N1 81.68(10) . . ? N4 Co1 N1 175.40(10) . . ? N2 Co1 N3 175.31(10) . . ? N4 Co1 N3 82.14(10) . . ? N1 Co1 N3 102.41(10) . . ? N2 Co1 Br2 85.97(8) . . ? N4 Co1 Br2 89.42(8) . . ? N1 Co1 Br2 91.14(7) . . ? N3 Co1 Br2 91.60(7) . . ? N2 Co1 Br1 92.95(8) . . ? N4 Co1 Br1 89.78(8) . . ? N1 Co1 Br1 89.58(7) . . ? N3 Co1 Br1 89.41(7) . . ? Br2 Co1 Br1 178.61(2) . . ? N3 N1 C2 119.9(2) 2_655 . ? N3 N1 Co1 128.25(17) 2_655 . ? C2 N1 Co1 111.87(19) . . ? C1 N2 O2 115.4(2) . . ? C1 N2 Co1 118.8(2) . . ? O2 N2 Co1 124.72(17) . . ? N1 N3 C3 119.2(2) 2_655 . ? N1 N3 Co1 129.28(17) 2_655 . ? C3 N3 Co1 111.47(19) . . ? C4 N4 O1 115.5(2) . . ? C4 N4 Co1 117.8(2) . . ? O1 N4 Co1 126.62(17) . . ? C13 N5 C9 121.3(3) . . ? C13 N5 C10 121.4(3) . . ? C9 N5 C10 117.3(3) . . ? C14 N6 C12 121.7(3) . . ? C14 N6 C11 120.7(3) . . ? C12 N6 C11 117.0(3) . . ? N2 C1 C2 112.3(2) . . ? N2 C1 C8 123.1(3) . . ? C2 C1 C8 124.5(2) . . ? N1 C2 C5 122.4(3) . . ? N1 C2 C1 115.1(2) . . ? C5 C2 C1 122.4(3) . . ? N3 C3 C6 122.9(3) . . ? N3 C3 C4 115.5(2) . . ? C6 C3 C4 121.6(2) . . ? N4 C4 C3 113.0(2) . . ? N4 C4 C7 125.1(3) . . ? C3 C4 C7 121.8(2) . . ? C6 C5 C2 117.8(3) 2_655 . ? C6 C5 H5 121.1 2_655 . ? C2 C5 H5 121.1 . . ? C5 C6 C3 117.9(2) 2_655 . ? C5 C6 H6 121.1 2_655 . ? C3 C6 H6 121.1 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 H8A 109.5 . . ? C1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 H9A 109.5 . . ? N5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 H11A 109.5 . . ? N6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 N5 126.7(3) . . ? O3 C13 H13 116.6 . . ? N5 C13 H13 116.6 . . ? O4 C14 N6 125.5(3) . . ? O4 C14 H14 117.3 . . ? N6 C14 H14 117.3 . . ? F2 B1 F1 112.7(3) . . ? F2 B1 O2 105.9(3) . . ? F1 B1 O2 110.5(3) . . ? F2 B1 O1 104.8(3) . . ? F1 B1 O1 111.2(3) . . ? O2 B1 O1 111.6(3) . . ? N4 O1 B1 120.6(2) . . ? N2 O2 B1 116.8(2) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.61 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.981 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.135 #===END data_nks5 _database_code_depnum_ccdc_archive 'CCDC 740046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Cl3 Co2 N11 O10' _chemical_formula_weight 856.80 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' Co Co 0.3494 0.9721 '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 11.599(2) _cell_length_b 11.925(2) _cell_length_c 12.693(2) _cell_angle_alpha 74.162(3) _cell_angle_beta 82.285(3) _cell_angle_gamma 73.895(2) _cell_volume 1619.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 29.01 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5829 _exptl_absorpt_correction_T_max 0.8773 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32839 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 29.07 _reflns_number_total 8592 _reflns_number_gt 6460 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1373P)^2^+3.1120P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8592 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.2321 _refine_ls_wR_factor_gt 0.2102 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 Co1 Co 0.22339(5) 0.59911(5) 0.30490(4) 0.01810(16) Uani 1 1 d . . . Co2 Co 0.09138(5) 0.62820(5) 0.58566(5) 0.01851(16) Uani 1 1 d . . . N1 N 0.0084(3) 0.6542(3) 0.4567(3) 0.0202(7) Uani 1 1 d . . . N2 N 0.1555(3) 0.5725(3) 0.7267(3) 0.0242(7) Uani 1 1 d . . . N3 N 0.0570(3) 0.6537(3) 0.3527(3) 0.0193(6) Uani 1 1 d . . . N4 N 0.2845(3) 0.5080(3) 0.4441(3) 0.0187(6) Uani 1 1 d . . . N5 N -0.0678(3) 0.6705(3) 0.6489(3) 0.0238(7) Uani 1 1 d . . . N6 N 0.2427(3) 0.5272(3) 0.5453(3) 0.0193(7) Uani 1 1 d . . . N7 N 0.3586(3) 0.4919(3) 0.2511(3) 0.0224(7) Uani 1 1 d . . . N8 N 0.1598(3) 0.6577(3) 0.1643(3) 0.0231(7) Uani 1 1 d . . . C1 C 0.1004(4) 0.6113(4) 0.8261(4) 0.0261(2) Uani 1 1 d . . . H1A H 0.1017 0.6960 0.8173 0.031 Uiso 1 1 calc R . . H1B H 0.1474 0.5609 0.8896 0.031 Uiso 1 1 calc R . . C2 C -0.1070(4) 0.6894(4) 0.7598(4) 0.0261(2) Uani 1 1 d . . . H2A H -0.1908 0.6821 0.7778 0.031 Uiso 1 1 calc R . . H2B H -0.1062 0.7722 0.7599 0.031 Uiso 1 1 calc R . . C3 C 0.2318(4) 0.6635(4) 0.0599(4) 0.0261(2) Uani 1 1 d . . . H3A H 0.2848 0.7180 0.0524 0.031 Uiso 1 1 calc R . . H3B H 0.1782 0.6962 -0.0017 0.031 Uiso 1 1 calc R . . C4 C 0.4045(4) 0.4929(4) 0.1368(4) 0.0261(2) Uani 1 1 d . . . H4A H 0.4490 0.4099 0.1334 0.031 Uiso 1 1 calc R . . H4B H 0.4621 0.5441 0.1146 0.031 Uiso 1 1 calc R . . C5 C -0.0280(4) 0.6003(4) 0.8475(4) 0.0261(2) Uani 1 1 d . . . H5A H -0.0597 0.6154 0.9202 0.031 Uiso 1 1 calc R . . H5B H -0.0300 0.5174 0.8491 0.031 Uiso 1 1 calc R . . C6 C -0.1524(4) 0.7004(4) 0.5813(4) 0.0261(2) Uani 1 1 d . . . H6 H -0.2351 0.7238 0.6042 0.031 Uiso 1 1 calc R . . C7 C 0.4279(4) 0.4169(4) 0.3263(4) 0.0261(2) Uani 1 1 d . . . H7 H 0.4981 0.3599 0.3086 0.031 Uiso 1 1 calc R . . C8 C 0.0448(4) 0.7019(4) 0.1632(4) 0.0261(2) Uani 1 1 d . . . H8 H 0.0047 0.7345 0.0968 0.031 Uiso 1 1 calc R . . C9 C 0.3074(4) 0.5386(4) 0.0555(4) 0.0261(2) Uani 1 1 d . . . H9A H 0.2549 0.4824 0.0719 0.031 Uiso 1 1 calc R . . H9B H 0.3452 0.5407 -0.0195 0.031 Uiso 1 1 calc R . . C10 C 0.2628(4) 0.5023(4) 0.7307(4) 0.0261(2) Uani 1 1 d . . . H10 H 0.3048 0.4731 0.7961 0.031 Uiso 1 1 calc R . . C11 C 0.3141(4) 0.4716(4) 0.6303(4) 0.0261(2) Uani 1 1 d . . . C12 C 0.3926(4) 0.4248(4) 0.4360(4) 0.0261(2) Uani 1 1 d . . . C13 C -0.0183(4) 0.6986(4) 0.2684(4) 0.0261(2) Uani 1 1 d . . . C14 C -0.1139(4) 0.6960(4) 0.4713(4) 0.0261(2) Uani 1 1 d . . . C15 C 0.4257(4) 0.3881(4) 0.6234(4) 0.0261(2) Uani 1 1 d . . . H15 H 0.4726 0.3510 0.6854 0.031 Uiso 1 1 calc R . . C16 C -0.1432(4) 0.7419(4) 0.2818(4) 0.0261(2) Uani 1 1 d . . . H16 H -0.1920 0.7714 0.2208 0.031 Uiso 1 1 calc R . . C17 C -0.1918(4) 0.7399(4) 0.3858(4) 0.0261(2) Uani 1 1 d . . . H17 H -0.2760 0.7675 0.3999 0.031 Uiso 1 1 calc R . . C18 C 0.4639(4) 0.3624(4) 0.5245(4) 0.0261(2) Uani 1 1 d . . . H18 H 0.5368 0.3038 0.5159 0.031 Uiso 1 1 calc R . . N9 N 0.1300(3) 0.7869(3) 0.5506(3) 0.0271(8) Uani 1 1 d . . . N10 N 0.2868(3) 0.7439(3) 0.2881(3) 0.0219(7) Uani 1 1 d . . . N11 N 0.6796(4) 0.2528(4) 0.2129(4) 0.0407(10) Uani 1 1 d . . . C29 C 0.6496(7) 0.0671(6) 0.1627(8) 0.070(2) Uani 1 1 d . . . H29A H 0.5811 0.0930 0.1165 0.106 Uiso 1 1 calc R . . H29B H 0.6340 0.0068 0.2291 0.106 Uiso 1 1 calc R . . H29C H 0.7224 0.0319 0.1221 0.106 Uiso 1 1 calc R . . C30 C 0.1461(9) 1.0026(9) 0.5529(9) 0.0261(2) Uani 0.50 1 d P . . C30A C 0.1692(11) 1.0003(10) 0.4980(12) 0.044(3) Uani 0.50 1 d P . . C31 C 0.3755(12) 0.9299(10) 0.2102(10) 0.0261(2) Uani 0.50 1 d P . . C31A C 0.3965(18) 0.9191(17) 0.2446(17) 0.015(4) Uiso 0.25 1 d P . . C31B C 0.364(3) 0.941(2) 0.241(2) 0.029(6) Uiso 0.25 1 d P . . C32 C 0.1377(13) 0.8847(13) 0.5570(11) 0.0261(2) Uani 0.50 1 d P . . C32A C 0.1516(10) 0.8764(10) 0.5254(9) 0.024(2) Uani 0.50 1 d P . . C33 C 0.3257(4) 0.8248(4) 0.2619(4) 0.0269(9) Uani 1 1 d . . . C34 C 0.6661(4) 0.1700(4) 0.1931(4) 0.0327(10) Uani 1 1 d . . . Cl1 Cl 0.65289(12) 0.76633(10) 0.02322(10) 0.0331(3) Uani 1 1 d . . . O1 O 0.6401(5) 0.8796(4) 0.0465(5) 0.0672(14) Uani 1 1 d . . . O2 O 0.6388(4) 0.7810(4) -0.0898(3) 0.0524(11) Uani 1 1 d . . . O3 O 0.7707(4) 0.6898(4) 0.0505(3) 0.0459(10) Uani 1 1 d . . . O4 O 0.5618(4) 0.7100(4) 0.0880(4) 0.0488(10) Uani 1 1 d . . . Cl2 Cl 0.0372(2) 0.02045(18) 0.1493(2) 0.0751(6) Uani 1 1 d . . . O5 O 0.0649(6) 0.0111(5) 0.2608(7) 0.099(2) Uani 1 1 d . . . O6 O 0.1224(6) -0.0416(8) 0.0867(5) 0.099(2) Uani 1 1 d . . . O7 O -0.0720(8) -0.0202(12) 0.1654(10) 0.167(5) Uani 1 1 d . . . O8 O 0.0097(11) 0.1422(7) 0.0860(8) 0.157(4) Uani 1 1 d . . . Cl3 Cl 0.5000 0.0000 0.5000 0.0741(9) Uani 1 2 d S . . O9 O 0.4067(8) 0.0978(9) 0.4122(9) 0.066(3) Uani 0.50 1 d P . . O10 O 0.5800(8) -0.0343(10) 0.4124(9) 0.057(3) Uani 0.50 1 d P . . O11 O 0.5716(12) 0.0976(11) 0.4678(13) 0.096(5) Uani 0.50 1 d P . . O12 O 0.510(3) -0.0714(14) 0.4556(16) 0.203(15) Uani 0.50 1 d P . . 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 Co1 0.0160(3) 0.0156(3) 0.0247(3) -0.0066(2) -0.0011(2) -0.00553(19) Co2 0.0168(3) 0.0155(3) 0.0261(3) -0.0075(2) 0.0002(2) -0.0070(2) N1 0.0152(15) 0.0163(15) 0.0327(18) -0.0092(13) -0.0029(13) -0.0061(12) N2 0.0258(18) 0.0229(17) 0.0274(18) -0.0083(14) -0.0006(14) -0.0101(14) N3 0.0171(15) 0.0163(15) 0.0274(17) -0.0079(13) -0.0020(13) -0.0063(12) N4 0.0150(15) 0.0157(15) 0.0275(17) -0.0065(13) -0.0004(13) -0.0065(12) N5 0.0223(17) 0.0191(17) 0.034(2) -0.0120(14) 0.0075(15) -0.0113(14) N6 0.0197(16) 0.0174(15) 0.0233(16) -0.0048(13) -0.0010(13) -0.0094(12) N7 0.0210(17) 0.0207(17) 0.0278(18) -0.0098(14) 0.0030(14) -0.0076(13) N8 0.0252(18) 0.0206(17) 0.0261(18) -0.0097(14) -0.0007(14) -0.0067(13) C1 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C2 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C3 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C4 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C5 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C6 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C7 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C8 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C9 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C10 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C11 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C12 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C13 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C14 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C15 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C16 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C17 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C18 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) N9 0.0263(19) 0.0185(17) 0.038(2) -0.0049(15) -0.0069(16) -0.0082(14) N10 0.0213(17) 0.0184(16) 0.0268(18) -0.0044(13) -0.0029(14) -0.0067(13) N11 0.035(2) 0.040(2) 0.052(3) -0.021(2) 0.006(2) -0.0119(19) C29 0.053(4) 0.029(3) 0.137(8) -0.023(4) -0.034(4) -0.008(3) C30 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C30A 0.051(7) 0.029(5) 0.062(8) -0.020(5) 0.006(6) -0.025(5) C31 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C32 0.0242(5) 0.0232(5) 0.0335(6) -0.0095(4) -0.0003(4) -0.0085(4) C32A 0.025(5) 0.020(4) 0.035(6) -0.011(4) -0.005(4) -0.010(3) C33 0.021(2) 0.022(2) 0.036(2) -0.0067(18) -0.0005(17) -0.0053(16) C34 0.025(2) 0.028(2) 0.043(3) -0.005(2) -0.004(2) -0.0072(18) Cl1 0.0416(7) 0.0255(5) 0.0329(6) -0.0111(4) -0.0026(5) -0.0056(5) O1 0.072(3) 0.046(3) 0.096(4) -0.046(3) 0.013(3) -0.016(2) O2 0.061(3) 0.051(3) 0.037(2) -0.0119(19) -0.0113(19) 0.004(2) O3 0.036(2) 0.055(3) 0.041(2) -0.0117(19) -0.0056(17) -0.0024(18) O4 0.041(2) 0.047(2) 0.053(3) -0.0022(19) -0.0056(19) -0.0110(18) Cl2 0.0658(12) 0.0493(10) 0.1092(18) -0.0198(11) -0.0048(12) -0.0132(9) O5 0.101(5) 0.052(3) 0.142(6) -0.020(4) -0.069(5) 0.009(3) O6 0.066(4) 0.183(8) 0.065(4) -0.049(4) 0.013(3) -0.047(4) O7 0.117(7) 0.229(12) 0.222(12) -0.131(10) 0.052(7) -0.105(8) O8 0.247(12) 0.067(5) 0.111(7) 0.002(4) -0.003(7) 0.007(6) Cl3 0.0320(11) 0.130(3) 0.0795(18) -0.0678(19) 0.0184(11) -0.0199(13) O9 0.038(5) 0.064(6) 0.083(7) -0.013(5) -0.022(5) 0.009(4) O10 0.037(5) 0.075(7) 0.068(6) -0.044(6) 0.008(4) -0.006(4) O11 0.075(8) 0.065(7) 0.123(12) -0.012(7) 0.033(8) -0.005(6) O12 0.40(4) 0.063(9) 0.138(16) -0.070(10) 0.15(2) -0.074(16) _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 Co1 N8 1.899(4) . ? Co1 N7 1.907(4) . ? Co1 N4 1.914(4) . ? Co1 N3 1.929(3) . ? Co1 N10 2.007(3) . ? Co2 N5 1.901(4) . ? Co2 N2 1.906(4) . ? Co2 N1 1.918(4) . ? Co2 N6 1.927(4) . ? Co2 N9 1.985(4) . ? N1 N3 1.365(5) . ? N1 C14 1.373(6) . ? N2 C10 1.292(6) . ? N2 C1 1.467(6) . ? N3 C13 1.369(6) . ? N4 N6 1.367(5) . ? N4 C12 1.378(5) . ? N5 C6 1.301(6) . ? N5 C2 1.477(6) . ? N6 C11 1.355(6) . ? N7 C7 1.303(6) . ? N7 C4 1.475(6) . ? N8 C8 1.292(6) . ? N8 C3 1.464(6) . ? C1 C5 1.513(6) . ? C2 C5 1.516(6) . ? C3 C9 1.516(6) . ? C4 C9 1.515(6) . ? C6 C14 1.418(6) . ? C7 C12 1.419(6) . ? C8 C13 1.431(6) . ? C10 C11 1.429(6) . ? C11 C15 1.406(6) . ? C12 C18 1.397(6) . ? C13 C16 1.401(6) . ? C14 C17 1.400(6) . ? C15 C18 1.361(6) . ? C16 C17 1.361(6) . ? N9 C32A 1.115(11) . ? N9 C32 1.219(14) . ? N10 C33 1.128(6) . ? N11 C34 1.137(7) . ? C29 C34 1.449(8) . ? C30 C30A 0.716(14) . ? C30 C32 1.422(17) . ? C30 C32A 1.618(14) . ? C30A C32A 1.488(14) . ? C30A C32 1.495(18) . ? C31 C33 1.478(11) . ? C31A C33 1.521(18) . ? C31B C33 1.52(3) . ? Cl1 O2 1.423(4) . ? Cl1 O1 1.425(4) . ? Cl1 O3 1.443(4) . ? Cl1 O4 1.449(4) . ? Cl2 O6 1.364(7) . ? Cl2 O8 1.425(8) . ? Cl2 O7 1.449(8) . ? Cl2 O5 1.460(8) . ? Cl3 O12 1.117(16) 2_656 ? Cl3 O12 1.117(16) . ? Cl3 O10 1.423(9) 2_656 ? Cl3 O10 1.423(9) . ? Cl3 O11 1.549(14) 2_656 ? Cl3 O11 1.549(14) . ? Cl3 O9 1.639(9) 2_656 ? Cl3 O9 1.639(9) . ? O10 O12 1.05(2) . ? O11 O12 1.30(2) 2_656 ? O12 O11 1.30(2) 2_656 ? 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 N8 Co1 N7 91.30(16) . . ? N8 Co1 N4 167.91(15) . . ? N7 Co1 N4 82.72(15) . . ? N8 Co1 N3 82.34(16) . . ? N7 Co1 N3 155.01(14) . . ? N4 Co1 N3 98.68(15) . . ? N8 Co1 N10 93.05(15) . . ? N7 Co1 N10 101.70(15) . . ? N4 Co1 N10 98.44(14) . . ? N3 Co1 N10 102.75(14) . . ? N5 Co2 N2 91.41(17) . . ? N5 Co2 N1 82.59(16) . . ? N2 Co2 N1 166.55(15) . . ? N5 Co2 N6 158.71(15) . . ? N2 Co2 N6 82.31(15) . . ? N1 Co2 N6 98.97(15) . . ? N5 Co2 N9 99.53(16) . . ? N2 Co2 N9 95.22(16) . . ? N1 Co2 N9 97.63(15) . . ? N6 Co2 N9 101.28(15) . . ? N3 N1 C14 118.1(4) . . ? N3 N1 Co2 127.8(3) . . ? C14 N1 Co2 113.3(3) . . ? C10 N2 C1 117.8(4) . . ? C10 N2 Co2 115.5(3) . . ? C1 N2 Co2 126.4(3) . . ? N1 N3 C13 118.3(3) . . ? N1 N3 Co1 128.4(3) . . ? C13 N3 Co1 113.3(3) . . ? N6 N4 C12 118.0(4) . . ? N6 N4 Co1 127.9(3) . . ? C12 N4 Co1 113.5(3) . . ? C6 N5 C2 115.8(4) . . ? C6 N5 Co2 115.1(3) . . ? C2 N5 Co2 128.5(3) . . ? C11 N6 N4 118.4(3) . . ? C11 N6 Co2 113.4(3) . . ? N4 N6 Co2 128.2(3) . . ? C7 N7 C4 115.5(4) . . ? C7 N7 Co1 114.7(3) . . ? C4 N7 Co1 129.2(3) . . ? C8 N8 C3 119.0(4) . . ? C8 N8 Co1 115.9(3) . . ? C3 N8 Co1 124.9(3) . . ? N2 C1 C5 110.6(4) . . ? N5 C2 C5 112.8(4) . . ? N8 C3 C9 109.7(4) . . ? N7 C4 C9 114.0(4) . . ? C1 C5 C2 111.1(4) . . ? N5 C6 C14 116.0(4) . . ? N7 C7 C12 116.3(4) . . ? N8 C8 C13 115.6(4) . . ? C4 C9 C3 111.6(4) . . ? N2 C10 C11 115.5(4) . . ? N6 C11 C15 124.2(4) . . ? N6 C11 C10 113.3(4) . . ? C15 C11 C10 122.5(4) . . ? N4 C12 C18 123.7(4) . . ? N4 C12 C7 112.4(4) . . ? C18 C12 C7 123.7(4) . . ? N3 C13 C16 124.4(4) . . ? N3 C13 C8 112.7(4) . . ? C16 C13 C8 122.9(4) . . ? N1 C14 C17 124.0(4) . . ? N1 C14 C6 112.7(4) . . ? C17 C14 C6 123.1(4) . . ? C18 C15 C11 117.5(4) . . ? C17 C16 C13 117.3(4) . . ? C16 C17 C14 118.0(4) . . ? C15 C18 C12 117.8(4) . . ? C32A N9 C32 21.1(7) . . ? C32A N9 Co2 176.4(6) . . ? C32 N9 Co2 162.1(7) . . ? C33 N10 Co1 169.2(4) . . ? C30A C30 C32 81.6(13) . . ? C30A C30 C32A 66.7(12) . . ? C32 C30 C32A 14.9(6) . . ? C30 C30A C32A 87.1(14) . . ? C30 C30A C32 70.1(13) . . ? C32A C30A C32 16.9(5) . . ? N9 C32 C30 174.2(13) . . ? N9 C32 C30A 146.4(12) . . ? C30 C32 C30A 28.3(6) . . ? N9 C32A C30A 174.3(11) . . ? N9 C32A C30 149.1(10) . . ? C30A C32A C30 26.2(6) . . ? N10 C33 C31 171.2(7) . . ? N10 C33 C31A 168.1(9) . . ? C31 C33 C31A 19.0(8) . . ? N10 C33 C31B 170.6(10) . . ? C31 C33 C31B 16.9(10) . . ? C31A C33 C31B 15.0(11) . . ? N11 C34 C29 177.5(7) . . ? O2 Cl1 O1 111.0(3) . . ? O2 Cl1 O3 109.0(3) . . ? O1 Cl1 O3 109.4(3) . . ? O2 Cl1 O4 108.6(3) . . ? O1 Cl1 O4 109.4(3) . . ? O3 Cl1 O4 109.5(3) . . ? O6 Cl2 O8 105.3(6) . . ? O6 Cl2 O7 110.8(5) . . ? O8 Cl2 O7 107.3(8) . . ? O6 Cl2 O5 117.9(4) . . ? O8 Cl2 O5 111.8(5) . . ? O7 Cl2 O5 103.5(6) . . ? O12 Cl3 O12 180.000(5) 2_656 . ? O12 Cl3 O10 47.1(13) 2_656 2_656 ? O12 Cl3 O10 132.9(13) . 2_656 ? O12 Cl3 O10 132.9(13) 2_656 . ? O12 Cl3 O10 47.1(13) . . ? O10 Cl3 O10 180.000(1) 2_656 . ? O12 Cl3 O11 124.5(12) 2_656 2_656 ? O12 Cl3 O11 55.5(12) . 2_656 ? O10 Cl3 O11 77.6(7) 2_656 2_656 ? O10 Cl3 O11 102.4(7) . 2_656 ? O12 Cl3 O11 55.5(12) 2_656 . ? O12 Cl3 O11 124.5(12) . . ? O10 Cl3 O11 102.4(7) 2_656 . ? O10 Cl3 O11 77.6(7) . . ? O11 Cl3 O11 180.0(6) 2_656 . ? O12 Cl3 O9 91.6(16) 2_656 2_656 ? O12 Cl3 O9 88.4(16) . 2_656 ? O10 Cl3 O9 90.6(6) 2_656 2_656 ? O10 Cl3 O9 89.4(6) . 2_656 ? O11 Cl3 O9 83.6(7) 2_656 2_656 ? O11 Cl3 O9 96.4(7) . 2_656 ? O12 Cl3 O9 88.4(16) 2_656 . ? O12 Cl3 O9 91.6(16) . . ? O10 Cl3 O9 89.4(6) 2_656 . ? O10 Cl3 O9 90.6(6) . . ? O11 Cl3 O9 96.4(7) 2_656 . ? O11 Cl3 O9 83.6(7) . . ? O9 Cl3 O9 180.0(7) 2_656 . ? O12 O10 Cl3 51.0(9) . . ? O12 O11 Cl3 45.1(9) 2_656 . ? O10 O12 Cl3 81.9(18) . . ? O10 O12 O11 160(2) . 2_656 ? Cl3 O12 O11 79.4(12) . 2_656 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.157 _refine_diff_density_min -3.010 _refine_diff_density_rms 0.178 #===END data_nks3297a _database_code_depnum_ccdc_archive 'CCDC 740047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 B2 Cl4 Co2 F4 N12 O20' _chemical_formula_weight 1161.86 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' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 '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 11.3016(10) _cell_length_b 12.7344(11) _cell_length_c 19.140(2) _cell_angle_alpha 103.927(2) _cell_angle_beta 94.988(2) _cell_angle_gamma 113.2930(10) _cell_volume 2403.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.52 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6595 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66218 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 30.52 _reflns_number_total 14390 _reflns_number_gt 10927 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0854P)^2^+4.0362P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14390 _refine_ls_number_parameters 670 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1772 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 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 Co1 Co 0.06424(3) 0.05615(3) 0.100069(19) 0.02033(9) Uani 1 1 d . . . Co2 Co 0.43367(4) 0.58906(4) 0.46129(2) 0.03322(11) Uani 1 1 d . A . N1 N 0.3769(3) 0.5841(3) 0.35534(15) 0.0405(6) Uani 1 1 d . . . N2 N 0.4662(3) 0.4481(2) 0.39896(14) 0.0319(5) Uani 1 1 d . . . N3 N 0.4994(3) 0.6233(2) 0.57271(13) 0.0316(5) Uani 1 1 d . . . N4 N 0.4024(3) 0.7375(3) 0.50860(16) 0.0383(6) Uani 1 1 d . . . N5 N 0.0459(4) 0.3417(5) 0.4437(3) 0.0947(19) Uani 1 1 d . . . N7 N 0.1531(2) 0.0005(2) 0.17020(12) 0.0259(5) Uani 1 1 d . . . N8 N -0.0237(2) 0.1322(2) 0.04169(12) 0.0221(4) Uani 1 1 d . . . N9 N 0.0698(2) 0.1956(2) 0.17930(12) 0.0250(4) Uani 1 1 d . . . N10 N -0.2872(3) -0.1777(2) 0.15028(15) 0.0314(5) Uani 1 1 d . . . N11 N 0.4339(2) 0.2197(2) 0.03630(13) 0.0239(4) Uani 1 1 d . . . N30 N 0.8887(4) 0.6671(3) 0.2601(3) 0.0685(12) Uani 1 1 d . . . N40 N 0.0751(2) -0.0885(2) 0.03033(12) 0.0227(4) Uani 1 1 d . . . B1 B 0.1313(4) 0.1303(3) 0.27897(19) 0.0335(7) Uani 1 1 d . . . B2 B 0.2855(5) 0.7257(5) 0.3928(3) 0.0549(12) Uani 1 1 d . . . Cl3 Cl 0.76550(7) 0.49033(6) 0.95171(4) 0.03119(15) Uani 1 1 d . . . Cl4 Cl 0.65477(7) 0.15728(6) 0.17540(4) 0.03009(15) Uani 1 1 d . . . O1 O 0.3721(3) 0.8021(3) 0.46710(16) 0.0495(6) Uani 1 1 d . . . O2 O 0.3516(3) 0.6744(3) 0.33897(15) 0.0495(6) Uani 1 1 d . . . O3 O 0.6197(4) 0.7159(4) 0.4611(2) 0.0657(9) Uani 1 1 d . . . O4 O 0.2608(3) 0.4674(2) 0.47616(14) 0.0483(6) Uani 1 1 d . . . O5 O 0.6948(3) 0.1348(3) 0.24084(15) 0.0562(8) Uani 1 1 d . . . O6 O 0.7115(2) 0.1124(2) 0.11726(14) 0.0388(5) Uani 1 1 d . . . O7 O 0.6972(3) 0.2835(2) 0.1881(2) 0.0641(9) Uani 1 1 d . . . O8 O 0.5134(2) 0.0988(2) 0.15370(14) 0.0451(6) Uani 1 1 d . . . O9 O 0.6259(3) 0.4187(3) 0.92728(16) 0.0553(8) Uani 1 1 d . . . O10 O 0.8053(3) 0.4876(2) 1.02450(13) 0.0428(6) Uani 1 1 d . . . O11 O 0.7952(2) 0.6106(2) 0.95140(15) 0.0392(5) Uani 1 1 d . . . O12 O 0.8343(3) 0.4432(3) 0.90193(15) 0.0499(7) Uani 1 1 d . . . O13 O 0.25235(19) 0.17328(17) 0.08780(11) 0.0247(4) Uani 1 1 d . . . O14 O -0.12177(19) -0.07485(18) 0.10055(11) 0.0269(4) Uani 1 1 d . . . O15 O 0.2042(2) 0.06259(19) 0.24342(11) 0.0319(4) Uani 1 1 d . . . O16 O 0.1352(2) 0.23083(19) 0.25114(11) 0.0304(4) Uani 1 1 d . . . O30 O 0.7024(5) 0.6231(5) 0.3011(3) 0.1199(19) Uani 1 1 d . . . F1 F 0.2009(2) 0.18706(19) 0.35075(10) 0.0417(5) Uani 1 1 d . . . F2 F 0.00208(19) 0.05159(19) 0.27429(11) 0.0414(5) Uani 1 1 d . . . F3 F 0.1746(2) 0.6360(3) 0.40081(15) 0.0628(7) Uani 1 1 d . . . F4 F 0.2590(3) 0.8056(3) 0.36349(17) 0.0735(8) Uani 1 1 d . . . C1 C 0.4370(3) 0.4269(3) 0.32588(16) 0.0327(6) Uani 1 1 d . . . C2 C 0.4442(3) 0.3281(3) 0.27783(16) 0.0373(7) Uani 1 1 d . . . H2 H 0.4248 0.3128 0.2261 0.045 Uiso 1 1 calc R . . C3 C 0.3974(3) 0.5132(3) 0.30247(16) 0.0364(7) Uani 1 1 d . . . C4 C 0.3863(4) 0.5143(4) 0.22455(18) 0.0444(8) Uani 1 1 d . . . H4A H 0.3521 0.5720 0.2184 0.067 Uiso 1 1 calc R . . H4B H 0.3262 0.4342 0.1922 0.067 Uiso 1 1 calc R . . H4C H 0.4733 0.5376 0.2118 0.067 Uiso 1 1 calc R . . C6 C 0.4793(5) 0.9187(3) 0.6160(2) 0.0529(10) Uani 1 1 d . . . H6A H 0.4566 0.9554 0.5805 0.079 Uiso 1 1 calc R . . H6B H 0.5727 0.9644 0.6393 0.079 Uiso 1 1 calc R . . H6C H 0.4259 0.9191 0.6537 0.079 Uiso 1 1 calc R . . C7 C 0.4527(3) 0.7924(3) 0.57698(19) 0.0389(7) Uani 1 1 d . . . C8 C 0.5201(3) 0.7458(3) 0.69301(18) 0.0385(7) Uani 1 1 d . . . H8 H 0.5147 0.8135 0.7241 0.046 Uiso 1 1 calc R . . C9 C 0.4918(3) 0.7199(3) 0.61648(17) 0.0331(6) Uani 1 1 d . . . C10 C 0.1558(4) 0.4073(5) 0.4326(3) 0.0638(13) Uani 1 1 d . A . H10 H 0.1569 0.4104 0.3835 0.077 Uiso 1 1 calc R . . C11 C 0.0601(10) 0.3069(9) 0.5202(6) 0.141(3) Uiso 1 1 d . . . H11A H 0.0439 0.2225 0.5085 0.212 Uiso 1 1 calc R . . H11B H -0.0042 0.3199 0.5481 0.212 Uiso 1 1 calc R . . H11C H 0.1492 0.3576 0.5497 0.212 Uiso 1 1 calc R . . C12 C -0.0741(9) 0.2830(8) 0.3873(5) 0.124(3) Uiso 1 1 d . . . H12A H -0.1382 0.3124 0.4036 0.186 Uiso 1 1 calc R . . H12B H -0.1108 0.1962 0.3788 0.186 Uiso 1 1 calc R . . H12C H -0.0539 0.3010 0.3416 0.186 Uiso 1 1 calc R . . C14 C 0.0306(3) 0.2700(2) 0.16123(16) 0.0265(5) Uani 1 1 d . . . C15 C 0.0430(3) 0.3848(3) 0.21120(19) 0.0368(7) Uani 1 1 d . . . H15A H -0.0445 0.3777 0.2180 0.055 Uiso 1 1 calc R . . H15B H 0.0837 0.4496 0.1896 0.055 Uiso 1 1 calc R . . H15C H 0.0980 0.4028 0.2589 0.055 Uiso 1 1 calc R . . C16 C -0.0302(3) 0.2308(2) 0.08216(16) 0.0245(5) Uani 1 1 d . . . C17 C 0.1397(3) -0.2473(3) 0.02319(17) 0.0286(6) Uani 1 1 d . . . H17 H 0.1796 -0.2862 0.0468 0.034 Uiso 1 1 calc R . . C18 C 0.1315(3) -0.1440(2) 0.06336(15) 0.0253(5) Uani 1 1 d . . . C19 C 0.0895(3) -0.2910(3) -0.05054(17) 0.0283(5) Uani 1 1 d . . . H19 H 0.0945 -0.3604 -0.0797 0.034 Uiso 1 1 calc R . . C20 C 0.1837(3) -0.0864(3) 0.14383(16) 0.0282(5) Uani 1 1 d . . . C21 C 0.2654(3) -0.1264(3) 0.18715(19) 0.0389(7) Uani 1 1 d . . . H21A H 0.3574 -0.0877 0.1827 0.058 Uiso 1 1 calc R . . H21B H 0.2329 -0.2136 0.1681 0.058 Uiso 1 1 calc R . . H21C H 0.2595 -0.1041 0.2390 0.058 Uiso 1 1 calc R . . C22 C 0.3218(3) 0.1445(2) 0.04623(15) 0.0233(5) Uani 1 1 d . . . H22 H 0.2909 0.0620 0.0200 0.028 Uiso 1 1 calc R . . C23 C 0.4904(3) 0.3481(3) 0.07573(18) 0.0321(6) Uani 1 1 d . . . H23A H 0.4193 0.3717 0.0856 0.048 Uiso 1 1 calc R . . H23B H 0.5419 0.3937 0.0456 0.048 Uiso 1 1 calc R . . H23C H 0.5476 0.3647 0.1224 0.048 Uiso 1 1 calc R . . C24 C -0.1976(3) -0.0773(2) 0.14439(15) 0.0257(5) Uani 1 1 d . . . H24 H -0.1904 -0.0033 0.1750 0.031 Uiso 1 1 calc R . . C25 C -0.2994(3) -0.2944(3) 0.1075(2) 0.0412(8) Uani 1 1 d . . . H25A H -0.2440 -0.2839 0.0707 0.062 Uiso 1 1 calc R . . H25B H -0.3913 -0.3457 0.0827 0.062 Uiso 1 1 calc R . . H25C H -0.2709 -0.3320 0.1404 0.062 Uiso 1 1 calc R . . C26 C -0.3741(4) -0.1767(4) 0.2023(2) 0.0465(8) Uani 1 1 d . . . H26A H -0.3585 -0.2153 0.2384 0.070 Uiso 1 1 calc R . . H26B H -0.4659 -0.2204 0.1758 0.070 Uiso 1 1 calc R . . H26C H -0.3561 -0.0937 0.2277 0.070 Uiso 1 1 calc R . . C30 C 0.6628(6) 0.7952(5) 0.4295(3) 0.0416(14) Uani 0.639(8) 1 d P A 1 H30 H 0.6244 0.7693 0.3787 0.050 Uiso 0.639(8) 1 calc PR A 1 N12 N 0.7509(5) 0.9070(4) 0.4538(3) 0.0361(11) Uani 0.639(8) 1 d P A 1 C31 C 0.7879(7) 0.9792(6) 0.4043(4) 0.058(2) Uani 0.639(8) 1 d P A 1 H31A H 0.7267 0.9368 0.3566 0.087 Uiso 0.639(8) 1 calc PR A 1 H31B H 0.8775 0.9937 0.3977 0.087 Uiso 0.639(8) 1 calc PR A 1 H31C H 0.7847 1.0560 0.4252 0.087 Uiso 0.639(8) 1 calc PR A 1 C30A C 0.7018(12) 0.7715(11) 0.4884(6) 0.040(2) Uani 0.361(8) 1 d P A 2 N12A N 0.7386(9) 0.8863(8) 0.4923(5) 0.042(2) Uani 0.361(8) 1 d P A 2 C31A C 0.6752(16) 0.9219(12) 0.4378(9) 0.068(4) Uani 0.361(8) 1 d P A 2 C32 C 0.8216(7) 0.9712(5) 0.5354(3) 0.0838(19) Uani 1 1 d . . . C33 C 0.9567(6) 0.6272(7) 0.2072(4) 0.094(2) Uani 1 1 d . . . H33A H 0.9108 0.5398 0.1861 0.142 Uiso 1 1 calc R . . H33B H 1.0470 0.6498 0.2314 0.142 Uiso 1 1 calc R . . H33C H 0.9587 0.6648 0.1679 0.142 Uiso 1 1 calc R . . C34 C 0.9393(6) 0.7915(4) 0.3027(7) 0.156(5) Uani 1 1 d . . . C35 C 0.7737(6) 0.5878(5) 0.2674(5) 0.099(2) Uani 1 1 d . . . H35 H 0.7472 0.5043 0.2465 0.118 Uiso 1 1 calc R . . C45 C 0.5145(3) 0.1764(3) -0.00725(17) 0.0301(6) Uani 1 1 d . . . H45A H 0.5964 0.1935 0.0249 0.045 Uiso 1 1 calc R . . H45B H 0.5349 0.2168 -0.0452 0.045 Uiso 1 1 calc R . . H45C H 0.4660 0.0897 -0.0307 0.045 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 Co1 0.01775(16) 0.02003(16) 0.02186(17) 0.00540(12) 0.00254(12) 0.00761(13) Co2 0.0396(2) 0.0338(2) 0.02335(19) 0.00397(16) 0.00246(16) 0.01625(18) N1 0.0421(16) 0.0487(16) 0.0315(13) 0.0119(12) 0.0011(11) 0.0217(13) N2 0.0317(13) 0.0327(13) 0.0241(11) 0.0034(9) 0.0019(9) 0.0104(10) N3 0.0339(13) 0.0289(12) 0.0243(11) 0.0015(9) 0.0031(9) 0.0101(10) N4 0.0397(15) 0.0365(14) 0.0396(14) 0.0093(12) 0.0066(11) 0.0187(12) N5 0.045(2) 0.081(3) 0.096(4) -0.027(3) 0.032(2) -0.007(2) N7 0.0236(11) 0.0259(11) 0.0231(10) 0.0081(9) 0.0010(8) 0.0058(9) N8 0.0168(10) 0.0224(10) 0.0242(10) 0.0066(8) 0.0051(8) 0.0056(8) N9 0.0198(10) 0.0277(11) 0.0215(10) 0.0038(8) 0.0037(8) 0.0065(9) N10 0.0269(12) 0.0279(12) 0.0411(14) 0.0151(10) 0.0084(10) 0.0106(10) N11 0.0209(10) 0.0230(10) 0.0276(11) 0.0082(8) 0.0057(8) 0.0086(8) N30 0.047(2) 0.0453(19) 0.124(4) 0.042(2) 0.014(2) 0.0207(17) N40 0.0191(10) 0.0218(10) 0.0243(10) 0.0077(8) 0.0029(8) 0.0057(8) B1 0.0310(17) 0.0364(17) 0.0257(15) 0.0072(13) 0.0001(12) 0.0094(14) B2 0.052(3) 0.067(3) 0.055(3) 0.016(2) 0.002(2) 0.038(2) Cl3 0.0315(3) 0.0284(3) 0.0371(4) 0.0171(3) 0.0051(3) 0.0124(3) Cl4 0.0268(3) 0.0265(3) 0.0393(4) 0.0105(3) 0.0074(3) 0.0133(3) O1 0.0577(17) 0.0484(15) 0.0521(15) 0.0165(12) 0.0080(13) 0.0325(13) O2 0.0557(16) 0.0601(17) 0.0428(14) 0.0208(12) 0.0025(12) 0.0334(14) O3 0.0472(18) 0.086(2) 0.091(3) 0.065(2) 0.0286(18) 0.0302(18) O4 0.0484(15) 0.0389(13) 0.0368(13) -0.0036(10) 0.0110(11) 0.0062(11) O5 0.076(2) 0.079(2) 0.0354(13) 0.0181(13) 0.0088(13) 0.0557(18) O6 0.0368(12) 0.0464(13) 0.0497(13) 0.0255(11) 0.0226(10) 0.0250(11) O7 0.0589(19) 0.0267(12) 0.106(3) 0.0167(15) 0.0166(18) 0.0191(13) O8 0.0271(11) 0.0567(15) 0.0422(13) 0.0043(11) 0.0115(10) 0.0142(11) O9 0.0361(14) 0.0519(16) 0.0594(17) 0.0328(14) -0.0020(12) -0.0064(12) O10 0.0546(15) 0.0510(14) 0.0341(12) 0.0167(11) 0.0059(10) 0.0324(13) O11 0.0308(11) 0.0317(11) 0.0643(16) 0.0262(11) 0.0169(11) 0.0143(9) O12 0.076(2) 0.0519(15) 0.0457(14) 0.0246(12) 0.0235(13) 0.0437(15) O13 0.0214(9) 0.0256(9) 0.0298(9) 0.0107(7) 0.0091(7) 0.0106(7) O14 0.0214(9) 0.0244(9) 0.0327(10) 0.0081(8) 0.0057(7) 0.0080(7) O15 0.0330(11) 0.0329(11) 0.0229(9) 0.0059(8) -0.0043(8) 0.0106(9) O16 0.0298(10) 0.0326(10) 0.0211(9) 0.0001(8) 0.0003(7) 0.0112(8) O30 0.080(3) 0.118(4) 0.127(4) 0.024(3) 0.024(3) 0.014(3) F1 0.0406(11) 0.0521(12) 0.0231(8) 0.0056(8) -0.0005(7) 0.0157(9) F2 0.0334(10) 0.0483(11) 0.0356(10) 0.0169(9) 0.0057(8) 0.0083(9) F3 0.0469(14) 0.0744(17) 0.0667(16) 0.0157(13) 0.0048(12) 0.0303(13) F4 0.087(2) 0.087(2) 0.0757(19) 0.0338(16) 0.0082(15) 0.0620(18) C1 0.0253(13) 0.0396(16) 0.0221(12) 0.0052(11) 0.0022(10) 0.0058(12) C2 0.0298(15) 0.0434(17) 0.0221(13) -0.0001(12) 0.0048(11) 0.0051(13) C3 0.0290(15) 0.0462(18) 0.0247(13) 0.0097(12) 0.0016(11) 0.0084(13) C4 0.0389(18) 0.059(2) 0.0285(15) 0.0168(15) 0.0040(13) 0.0127(16) C6 0.067(3) 0.0369(18) 0.052(2) 0.0013(16) 0.0126(19) 0.0261(18) C7 0.0391(17) 0.0318(15) 0.0407(17) 0.0024(13) 0.0100(13) 0.0147(13) C8 0.0320(15) 0.0384(16) 0.0300(15) -0.0037(12) 0.0094(12) 0.0076(13) C9 0.0307(15) 0.0308(14) 0.0288(14) 0.0014(11) 0.0059(11) 0.0087(12) C10 0.038(2) 0.077(3) 0.050(2) -0.011(2) 0.0032(17) 0.016(2) C14 0.0197(12) 0.0259(12) 0.0310(13) 0.0040(10) 0.0076(10) 0.0089(10) C15 0.0353(16) 0.0332(15) 0.0375(16) -0.0012(12) 0.0057(12) 0.0176(13) C16 0.0171(11) 0.0221(11) 0.0326(13) 0.0083(10) 0.0082(9) 0.0062(9) C17 0.0239(13) 0.0255(13) 0.0414(15) 0.0155(11) 0.0091(11) 0.0119(11) C18 0.0184(12) 0.0246(12) 0.0305(13) 0.0109(10) 0.0039(9) 0.0057(10) C19 0.0241(13) 0.0251(12) 0.0383(15) 0.0102(11) 0.0103(11) 0.0117(10) C20 0.0239(13) 0.0269(13) 0.0304(13) 0.0125(11) 0.0004(10) 0.0064(10) C21 0.0387(17) 0.0337(15) 0.0415(17) 0.0136(13) -0.0067(13) 0.0144(13) C22 0.0212(12) 0.0230(11) 0.0271(12) 0.0093(10) 0.0039(9) 0.0101(10) C23 0.0277(14) 0.0245(13) 0.0379(15) 0.0066(11) 0.0078(11) 0.0063(11) C24 0.0224(12) 0.0243(12) 0.0301(13) 0.0077(10) 0.0029(10) 0.0104(10) C25 0.0342(17) 0.0218(13) 0.060(2) 0.0101(14) 0.0037(15) 0.0067(12) C26 0.045(2) 0.052(2) 0.053(2) 0.0302(18) 0.0233(16) 0.0206(17) C30 0.045(3) 0.037(3) 0.033(3) 0.008(2) 0.005(2) 0.010(2) N12 0.036(2) 0.032(2) 0.036(3) 0.0134(19) 0.0002(18) 0.0094(18) C31 0.051(4) 0.054(4) 0.067(4) 0.039(3) 0.000(3) 0.011(3) C30A 0.047(6) 0.053(6) 0.040(5) 0.022(4) 0.018(4) 0.033(5) N12A 0.046(5) 0.034(4) 0.036(5) 0.002(4) 0.003(4) 0.014(4) C31A 0.070(9) 0.052(7) 0.080(9) 0.025(7) -0.008(7) 0.025(7) C32 0.136(5) 0.047(3) 0.055(3) 0.011(2) 0.036(3) 0.026(3) C33 0.060(3) 0.126(6) 0.119(5) 0.054(5) 0.023(3) 0.051(4) C34 0.055(3) 0.024(2) 0.332(14) 0.016(4) -0.051(5) 0.000(2) C35 0.068(4) 0.045(3) 0.151(7) -0.001(3) 0.041(4) 0.007(2) C45 0.0266(14) 0.0328(14) 0.0355(14) 0.0127(12) 0.0123(11) 0.0147(12) _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 Co1 N9 2.014(2) . ? Co1 N7 2.025(2) . ? Co1 N40 2.053(2) . ? Co1 N8 2.064(2) . ? Co1 O14 2.107(2) . ? Co1 O13 2.1325(19) . ? Co2 N1 2.051(3) . ? Co2 O4 2.052(3) . ? Co2 N4 2.069(3) . ? Co2 N3 2.076(3) . ? Co2 O3 2.085(4) . ? Co2 N2 2.085(3) . ? N1 C3 1.287(5) . ? N1 O2 1.386(4) . ? N2 N3 1.324(4) 2_666 ? N2 C1 1.344(4) . ? N3 N2 1.324(4) 2_666 ? N3 C9 1.349(4) . ? N4 C7 1.281(4) . ? N4 O1 1.383(4) . ? N5 C10 1.264(6) . ? N5 C12 1.455(10) . ? N5 C11 1.641(11) . ? N7 C20 1.289(4) . ? N7 O15 1.374(3) . ? N8 N40 1.335(3) 2 ? N8 C16 1.341(3) . ? N9 C14 1.295(4) . ? N9 O16 1.380(3) . ? N10 C24 1.319(4) . ? N10 C25 1.460(4) . ? N10 C26 1.459(4) . ? N11 C22 1.315(3) . ? N11 C45 1.462(4) . ? N11 C23 1.465(4) . ? N30 C35 1.338(7) . ? N30 C33 1.440(8) . ? N30 C34 1.443(7) . ? N40 N8 1.335(3) 2 ? N40 C18 1.344(4) . ? B1 F1 1.383(4) . ? B1 F2 1.386(4) . ? B1 O16 1.487(4) . ? B1 O15 1.504(4) . ? B2 F3 1.373(6) . ? B2 F4 1.388(6) . ? B2 O2 1.498(6) . ? B2 O1 1.505(6) . ? Cl3 O11 1.434(2) . ? Cl3 O9 1.438(3) . ? Cl3 O10 1.439(2) . ? Cl3 O12 1.448(3) . ? Cl4 O5 1.426(3) . ? Cl4 O7 1.433(3) . ? Cl4 O8 1.440(2) . ? Cl4 O6 1.444(2) . ? O3 C30A 0.924(12) . ? O3 C30 1.256(6) . ? O4 C10 1.221(5) . ? O13 C22 1.257(3) . ? O14 C24 1.247(3) . ? O30 C35 1.227(8) . ? C1 C2 1.405(5) . ? C1 C3 1.483(5) . ? C2 C8 1.368(5) 2_666 ? C3 C4 1.490(4) . ? C6 C7 1.495(5) . ? C7 C9 1.491(5) . ? C8 C2 1.368(5) 2_666 ? C8 C9 1.400(4) . ? C14 C16 1.482(4) . ? C14 C15 1.487(4) . ? C16 C19 1.401(4) 2 ? C17 C19 1.362(4) . ? C17 C18 1.397(4) . ? C18 C20 1.488(4) . ? C19 C16 1.401(4) 2 ? C20 C21 1.498(4) . ? C30 N12 1.309(7) . ? N12 C31 1.450(8) . ? N12 C32 1.549(8) . ? C30A N12A 1.333(15) . ? N12A C32 1.168(10) . ? N12A C31A 1.470(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 N9 Co1 N7 94.27(10) . . ? N9 Co1 N40 172.03(9) . . ? N7 Co1 N40 77.86(9) . . ? N9 Co1 N8 77.53(9) . . ? N7 Co1 N8 171.80(9) . . ? N40 Co1 N8 110.33(9) . . ? N9 Co1 O14 99.24(9) . . ? N7 Co1 O14 90.78(9) . . ? N40 Co1 O14 82.34(8) . . ? N8 Co1 O14 90.54(8) . . ? N9 Co1 O13 87.68(8) . . ? N7 Co1 O13 89.78(9) . . ? N40 Co1 O13 90.95(8) . . ? N8 Co1 O13 89.89(8) . . ? O14 Co1 O13 172.99(8) . . ? N1 Co2 O4 100.24(12) . . ? N1 Co2 N4 94.52(12) . . ? O4 Co2 N4 94.93(12) . . ? N1 Co2 N3 170.82(12) . . ? O4 Co2 N3 84.87(11) . . ? N4 Co2 N3 77.36(11) . . ? N1 Co2 O3 87.62(14) . . ? O4 Co2 O3 172.13(13) . . ? N4 Co2 O3 84.06(14) . . ? N3 Co2 O3 87.29(13) . . ? N1 Co2 N2 77.09(11) . . ? O4 Co2 N2 89.64(11) . . ? N4 Co2 N2 171.07(11) . . ? N3 Co2 N2 110.77(10) . . ? O3 Co2 N2 92.45(14) . . ? C3 N1 O2 116.7(3) . . ? C3 N1 Co2 118.7(2) . . ? O2 N1 Co2 122.3(2) . . ? N3 N2 C1 121.4(3) 2_666 . ? N3 N2 Co2 123.72(19) 2_666 . ? C1 N2 Co2 114.6(2) . . ? N2 N3 C9 120.9(3) 2_666 . ? N2 N3 Co2 124.36(19) 2_666 . ? C9 N3 Co2 114.4(2) . . ? C7 N4 O1 116.7(3) . . ? C7 N4 Co2 117.6(2) . . ? O1 N4 Co2 121.9(2) . . ? C10 N5 C12 122.7(7) . . ? C10 N5 C11 112.4(6) . . ? C12 N5 C11 123.6(6) . . ? C20 N7 O15 116.4(2) . . ? C20 N7 Co1 118.99(19) . . ? O15 N7 Co1 123.64(18) . . ? N40 N8 C16 120.2(2) 2 . ? N40 N8 Co1 124.96(17) 2 . ? C16 N8 Co1 114.84(18) . . ? C14 N9 O16 115.8(2) . . ? C14 N9 Co1 119.41(19) . . ? O16 N9 Co1 123.67(18) . . ? C24 N10 C25 121.3(3) . . ? C24 N10 C26 121.4(3) . . ? C25 N10 C26 117.2(3) . . ? C22 N11 C45 120.9(2) . . ? C22 N11 C23 121.2(2) . . ? C45 N11 C23 117.4(2) . . ? C35 N30 C33 119.0(5) . . ? C35 N30 C34 119.7(6) . . ? C33 N30 C34 121.2(6) . . ? N8 N40 C18 120.6(2) 2 . ? N8 N40 Co1 124.53(17) 2 . ? C18 N40 Co1 114.77(18) . . ? F1 B1 F2 112.7(3) . . ? F1 B1 O16 103.5(3) . . ? F2 B1 O16 110.2(3) . . ? F1 B1 O15 104.6(3) . . ? F2 B1 O15 110.0(3) . . ? O16 B1 O15 115.6(3) . . ? F3 B2 F4 113.2(4) . . ? F3 B2 O2 110.4(4) . . ? F4 B2 O2 104.3(4) . . ? F3 B2 O1 109.8(4) . . ? F4 B2 O1 104.2(4) . . ? O2 B2 O1 114.8(3) . . ? O11 Cl3 O9 108.79(16) . . ? O11 Cl3 O10 110.80(16) . . ? O9 Cl3 O10 109.08(16) . . ? O11 Cl3 O12 108.70(16) . . ? O9 Cl3 O12 109.7(2) . . ? O10 Cl3 O12 109.72(15) . . ? O5 Cl4 O7 110.1(2) . . ? O5 Cl4 O8 109.66(19) . . ? O7 Cl4 O8 108.44(18) . . ? O5 Cl4 O6 109.74(15) . . ? O7 Cl4 O6 109.33(18) . . ? O8 Cl4 O6 109.59(15) . . ? N4 O1 B2 113.7(3) . . ? N1 O2 B2 113.4(3) . . ? C30A O3 C30 72.6(7) . . ? C30A O3 Co2 146.9(7) . . ? C30 O3 Co2 135.0(4) . . ? C10 O4 Co2 129.0(3) . . ? C22 O13 Co1 126.16(18) . . ? C24 O14 Co1 132.06(18) . . ? N7 O15 B1 114.8(2) . . ? N9 O16 B1 114.3(2) . . ? N2 C1 C2 120.0(3) . . ? N2 C1 C3 115.1(3) . . ? C2 C1 C3 124.9(3) . . ? C8 C2 C1 118.7(3) 2_666 . ? N1 C3 C1 113.5(3) . . ? N1 C3 C4 125.7(3) . . ? C1 C3 C4 120.8(3) . . ? N4 C7 C9 113.3(3) . . ? N4 C7 C6 126.0(4) . . ? C9 C7 C6 120.6(3) . . ? C2 C8 C9 118.8(3) 2_666 . ? N3 C9 C8 120.2(3) . . ? N3 C9 C7 115.0(3) . . ? C8 C9 C7 124.8(3) . . ? O4 C10 N5 129.0(5) . . ? N9 C14 C16 113.0(2) . . ? N9 C14 C15 126.3(3) . . ? C16 C14 C15 120.7(3) . . ? N8 C16 C19 121.5(3) . 2 ? N8 C16 C14 114.8(2) . . ? C19 C16 C14 123.7(3) 2 . ? C19 C17 C18 118.7(3) . . ? N40 C18 C17 121.0(3) . . ? N40 C18 C20 114.9(2) . . ? C17 C18 C20 124.1(3) . . ? C17 C19 C16 118.1(3) . 2 ? N7 C20 C18 113.0(2) . . ? N7 C20 C21 125.2(3) . . ? C18 C20 C21 121.8(3) . . ? O13 C22 N11 125.0(2) . . ? O14 C24 N10 123.1(3) . . ? O3 C30 N12 131.8(6) . . ? C30 N12 C31 120.9(5) . . ? C30 N12 C32 123.6(5) . . ? C31 N12 C32 115.5(5) . . ? O3 C30A N12A 118.4(10) . . ? C32 N12A C30A 128.3(10) . . ? C32 N12A C31A 110.0(10) . . ? C30A N12A C31A 121.6(10) . . ? N12A C32 N12 32.5(5) . . ? O30 C35 N30 119.9(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.782 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.107 #===END data_nks3-213 _database_code_depnum_ccdc_archive 'CCDC 740048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H36 B4 Co2 F12 N14 O4' _chemical_formula_weight 1213.97 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 17.2357(12) _cell_length_b 24.1048(17) _cell_length_c 13.4470(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.8100(10) _cell_angle_gamma 90.00 _cell_volume 5534.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9533 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 30.41 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116404 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.28 _reflns_number_total 13710 _reflns_number_gt 10779 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0559P)^2^+7.2191P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13710 _refine_ls_number_parameters 790 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.043 _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 Co1 Co 0.102846(19) 0.507608(13) 0.06621(2) 0.01821(9) Uani 1 1 d . . . Co2 Co 0.58194(2) 0.519796(15) 0.42685(3) 0.02264(9) Uani 1 1 d . . . N1 N 0.02092(12) 0.56572(9) 0.04186(15) 0.0199(4) Uani 1 1 d . . . N2 N 0.16110(12) 0.56922(9) 0.12760(15) 0.0201(4) Uani 1 1 d . . . N3 N 0.18963(12) 0.45685(9) 0.09396(15) 0.0202(4) Uani 1 1 d . . . N4 N 0.05312(12) 0.44076(9) -0.00028(15) 0.0198(4) Uani 1 1 d . . . N5 N 0.49423(12) 0.46839(9) 0.38613(15) 0.0202(4) Uani 1 1 d . . . N6 N 0.56384(12) 0.54502(9) 0.56222(15) 0.0206(4) Uani 1 1 d . . . N7 N 0.67078(14) 0.56833(10) 0.45505(17) 0.0286(5) Uani 1 1 d . . . N8 N 0.60865(14) 0.49860(10) 0.29895(17) 0.0282(5) Uani 1 1 d . . . N9 N 0.51112(15) 0.58759(10) 0.35916(17) 0.0304(5) Uani 1 1 d . . . N10 N 0.64762(14) 0.45156(10) 0.49609(18) 0.0298(5) Uani 1 1 d . . . N11 N 0.14525(13) 0.53088(9) -0.07366(17) 0.0249(5) Uani 1 1 d . . . N12 N 0.05289(14) 0.49049(10) 0.19995(17) 0.0272(5) Uani 1 1 d . . . N13 N 0.9754(3) 0.6312(2) 0.3010(3) 0.0816(13) Uani 1 1 d . . . N14 N 0.8830(3) 0.40599(19) 0.4786(4) 0.0910(15) Uani 1 1 d . . . O1 O 0.23828(10) 0.56830(7) 0.16442(14) 0.0233(4) Uani 1 1 d . . . O2 O 0.26211(10) 0.46856(8) 0.14216(14) 0.0237(4) Uani 1 1 d . . . O3 O 0.72764(13) 0.57748(11) 0.39603(15) 0.0418(6) Uani 1 1 d . . . O4 O 0.67590(13) 0.51226(11) 0.26287(16) 0.0431(6) Uani 1 1 d . . . B1 B 0.7082(3) 0.5661(2) 0.2873(3) 0.0513(11) Uani 1 1 d . . . B2 B 0.26638(18) 0.51586(12) 0.2155(2) 0.0241(6) Uani 1 1 d . . . F1 F 0.77754(15) 0.56924(12) 0.24717(17) 0.0705(8) Uani 1 1 d . . . F2 F 0.65432(16) 0.60605(11) 0.24652(17) 0.0667(7) Uani 1 1 d . . . F3 F 0.34442(9) 0.52410(7) 0.24712(11) 0.0277(3) Uani 1 1 d . . . F4 F 0.22413(10) 0.50371(7) 0.29256(12) 0.0319(4) Uani 1 1 d . . . C1 C 0.04556(15) 0.61568(10) 0.08041(19) 0.0222(5) Uani 1 1 d . . . C2 C 0.12845(15) 0.61770(10) 0.12263(19) 0.0217(5) Uani 1 1 d . . . C3 C 0.17169(15) 0.66958(11) 0.1534(2) 0.0257(5) Uani 1 1 d . . . C4 C 0.10337(15) 0.39753(10) 0.00184(19) 0.0216(5) Uani 1 1 d . . . C5 C 0.18213(15) 0.40830(10) 0.05347(18) 0.0211(5) Uani 1 1 d . . . C6 C 0.24657(15) 0.36717(11) 0.0566(2) 0.0239(5) Uani 1 1 d . . . C7 C 0.0255(2) 0.49285(15) 0.2703(3) 0.0444(8) Uani 1 1 d . . . C8 C 0.16867(16) 0.55300(12) -0.1376(2) 0.0297(6) Uani 1 1 d . . . C9 C 0.08069(16) 0.34595(11) -0.0396(2) 0.0281(6) Uani 1 1 d . . . H9 H 0.1174 0.3165 -0.0395 0.034 Uiso 1 1 calc R . . C10 C 0.25066(17) 0.32279(12) 0.1238(2) 0.0289(6) Uani 1 1 d . . . H10 H 0.2113 0.3177 0.1660 0.035 Uiso 1 1 calc R . . C11 C 0.36481(18) 0.33598(14) -0.0026(3) 0.0391(7) Uani 1 1 d . . . H11 H 0.4034 0.3400 -0.0463 0.047 Uiso 1 1 calc R . . C12 C 0.36997(18) 0.29277(14) 0.0655(3) 0.0404(8) Uani 1 1 d . . . H12 H 0.4126 0.2676 0.0692 0.048 Uiso 1 1 calc R . . C13 C 0.31368(19) 0.28597(13) 0.1281(2) 0.0370(7) Uani 1 1 d . . . H13 H 0.3177 0.2560 0.1745 0.044 Uiso 1 1 calc R . . C14 C 0.30315(17) 0.37352(12) -0.0071(2) 0.0312(6) Uani 1 1 d . . . H14 H 0.2997 0.4034 -0.0536 0.037 Uiso 1 1 calc R . . C15 C -0.00431(16) 0.66104(11) 0.0803(2) 0.0278(6) Uani 1 1 d . . . H15 H 0.0141 0.6957 0.1077 0.033 Uiso 1 1 calc R . . C16 C 0.23119(16) 0.68602(12) 0.0992(2) 0.0324(6) Uani 1 1 d . . . H16 H 0.2413 0.6654 0.0421 0.039 Uiso 1 1 calc R . . C17 C 0.27576(19) 0.73281(13) 0.1291(3) 0.0431(8) Uani 1 1 d . . . H17 H 0.3162 0.7443 0.0922 0.052 Uiso 1 1 calc R . . C18 C 0.2018(2) 0.74655(13) 0.2658(3) 0.0430(8) Uani 1 1 d . . . H18 H 0.1920 0.7673 0.3229 0.052 Uiso 1 1 calc R . . C19 C 0.26123(19) 0.76234(13) 0.2118(3) 0.0478(9) Uani 1 1 d . . . H19 H 0.2922 0.7940 0.2324 0.057 Uiso 1 1 calc R . . C20 C 0.15622(17) 0.69996(12) 0.2360(2) 0.0317(6) Uani 1 1 d . . . H20 H 0.1150 0.6892 0.2721 0.038 Uiso 1 1 calc R . . C21 C 0.1988(3) 0.5834(2) -0.2187(3) 0.0694(6) Uani 1 1 d . . . H21A H 0.1612 0.6122 -0.2446 0.104 Uiso 1 1 calc R . . H21B H 0.2064 0.5576 -0.2729 0.104 Uiso 1 1 calc R . . H21C H 0.2490 0.6007 -0.1929 0.104 Uiso 1 1 calc R . . C22 C -0.0108(3) 0.4962(2) 0.3624(3) 0.0694(6) Uani 1 1 d . . . H22A H 0.0259 0.5134 0.4156 0.104 Uiso 1 1 calc R . . H22B H -0.0242 0.4589 0.3831 0.104 Uiso 1 1 calc R . . H22C H -0.0585 0.5188 0.3500 0.104 Uiso 1 1 calc R . . C23 C 0.9168(3) 0.30169(16) 0.4789(3) 0.0539(10) Uani 1 1 d . . . H23A H 0.8688 0.2800 0.4800 0.081 Uiso 1 1 calc R . . H23B H 0.9544 0.2925 0.5380 0.081 Uiso 1 1 calc R . . H23C H 0.9396 0.2929 0.4179 0.081 Uiso 1 1 calc R . . C24 C 0.8540(2) 0.68101(17) 0.3507(3) 0.0519(9) Uani 1 1 d . . . H24A H 0.8429 0.6668 0.4156 0.078 Uiso 1 1 calc R . . H24B H 0.8086 0.6746 0.2997 0.078 Uiso 1 1 calc R . . H24C H 0.8647 0.7209 0.3563 0.078 Uiso 1 1 calc R . . C25 C 0.7141(3) 0.3689(2) 0.5965(3) 0.0694(6) Uani 1 1 d . . . H25A H 0.7702 0.3688 0.5911 0.104 Uiso 1 1 calc R . . H25B H 0.6906 0.3340 0.5699 0.104 Uiso 1 1 calc R . . H25C H 0.7066 0.3727 0.6672 0.104 Uiso 1 1 calc R . . C26 C 0.4629(3) 0.68350(19) 0.2879(3) 0.0694(6) Uani 1 1 d . . . H26A H 0.4567 0.7085 0.3438 0.104 Uiso 1 1 calc R . . H26B H 0.4125 0.6794 0.2451 0.104 Uiso 1 1 calc R . . H26C H 0.5015 0.6989 0.2485 0.104 Uiso 1 1 calc R . . C27 C 0.49611(15) 0.44698(10) 0.29333(18) 0.0212(5) Uani 1 1 d . . . C28 C 0.67646(19) 0.41528(13) 0.5391(2) 0.0365(7) Uani 1 1 d . . . C29 C 0.57844(15) 0.44241(13) 0.1464(2) 0.0280(6) Uani 1 1 d . . . C30 C 0.68032(15) 0.59337(11) 0.54062(19) 0.0239(5) Uani 1 1 d . . . C31 C 0.62030(15) 0.58002(10) 0.60369(19) 0.0214(5) Uani 1 1 d . . . C32 C 0.74482(16) 0.63299(12) 0.57471(19) 0.0272(6) Uani 1 1 d . . . C33 C 0.58062(17) 0.38567(14) 0.1283(2) 0.0354(7) Uani 1 1 d . . . H33 H 0.5727 0.3599 0.1795 0.043 Uiso 1 1 calc R . . C34 C 0.6059(2) 0.40514(18) -0.0405(3) 0.0468(9) Uani 1 1 d . . . H34 H 0.6155 0.3923 -0.1045 0.056 Uiso 1 1 calc R . . C35 C 0.5947(2) 0.36695(17) 0.0339(3) 0.0477(9) Uani 1 1 d . . . H35 H 0.5966 0.3283 0.0206 0.057 Uiso 1 1 calc R . . C36 C 0.60329(19) 0.46134(17) -0.0226(2) 0.0421(8) Uani 1 1 d . . . H36 H 0.6108 0.4869 -0.0741 0.051 Uiso 1 1 calc R . . C37 C 0.58970(17) 0.48048(14) 0.0707(2) 0.0326(6) Uani 1 1 d . . . H37 H 0.5880 0.5192 0.0834 0.039 Uiso 1 1 calc R . . C38 C 0.86309(18) 0.70722(13) 0.6403(2) 0.0352(7) Uani 1 1 d . . . H38 H 0.9037 0.7327 0.6632 0.042 Uiso 1 1 calc R . . C39 C 0.82136(17) 0.61391(13) 0.5987(2) 0.0328(6) Uani 1 1 d . . . H39 H 0.8331 0.5757 0.5924 0.039 Uiso 1 1 calc R . . C40 C 0.78714(18) 0.72610(12) 0.6156(2) 0.0332(6) Uani 1 1 d . . . H40 H 0.7757 0.7645 0.6206 0.040 Uiso 1 1 calc R . . C41 C 0.72739(17) 0.68868(12) 0.5834(2) 0.0295(6) Uani 1 1 d . . . H41 H 0.6750 0.7013 0.5674 0.035 Uiso 1 1 calc R . . C42 C 0.88036(18) 0.65153(13) 0.6320(2) 0.0368(7) Uani 1 1 d . . . H42 H 0.9327 0.6389 0.6492 0.044 Uiso 1 1 calc R . . C43 C 0.62235(15) 0.60158(10) 0.69998(19) 0.0228(5) Uani 1 1 d . . . H43 H 0.6638 0.6252 0.7280 0.027 Uiso 1 1 calc R . . C44 C 0.56276(15) 0.58770(11) 0.75320(19) 0.0237(5) Uani 1 1 d . . . H44 H 0.5616 0.6012 0.8194 0.028 Uiso 1 1 calc R . . C17A C 0.9203(3) 0.65313(18) 0.3225(3) 0.0534(9) Uani 1 1 d . . . C18A C 0.8985(3) 0.35983(19) 0.4801(3) 0.0569(10) Uani 1 1 d . . . C27A C 0.4896(2) 0.62886(13) 0.3277(2) 0.0363(7) Uani 1 1 d . . . C28A C 0.56370(16) 0.46363(11) 0.24557(19) 0.0247(5) Uani 1 1 d . . . B3 B 0.4777(2) 0.70587(16) 0.5837(3) 0.0433(9) Uani 1 1 d . . . F5 F 0.44139(17) 0.68382(15) 0.6558(3) 0.1088(14) Uani 1 1 d . . . F6 F 0.4268(2) 0.73143(18) 0.5135(3) 0.1340(19) Uani 1 1 d . . . F7 F 0.5319(4) 0.6781(3) 0.5347(6) 0.0420(14) Uani 0.50 1 d P . . F7A F 0.5035(6) 0.6602(4) 0.5410(6) 0.109(4) Uani 0.50 1 d P . . F8 F 0.5072(5) 0.7566(3) 0.6092(5) 0.084(2) Uani 0.50 1 d P . . F8A F 0.5467(4) 0.7274(3) 0.6419(7) 0.100(2) Uani 0.50 1 d P . . B4 B 0.9690(2) 0.32022(15) 0.1670(3) 0.0334(7) Uani 1 1 d . . . F9 F 0.90369(12) 0.31955(10) 0.09335(14) 0.0485(5) Uani 1 1 d . . . F10 F 0.9974(3) 0.37181(18) 0.1611(4) 0.0332(10) Uani 0.50 1 d P . . F10A F 1.0318(4) 0.3527(3) 0.1513(4) 0.073(2) Uani 0.50 1 d P . . F11 F 0.9887(3) 0.2682(2) 0.1916(6) 0.085(2) Uani 0.50 1 d P . . F11A F 1.0249(2) 0.28077(15) 0.1362(3) 0.0348(8) Uani 0.50 1 d P . . F12 F 0.9443(3) 0.3451(4) 0.2573(4) 0.082(2) Uani 0.50 1 d P . . F12A F 0.9531(2) 0.30601(19) 0.2585(3) 0.0335(9) Uani 0.50 1 d P . . 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 Co1 0.01747(16) 0.01900(16) 0.01744(16) -0.00164(12) -0.00024(12) 0.00062(12) Co2 0.02183(18) 0.02914(19) 0.01624(16) -0.00220(13) -0.00002(13) -0.00818(13) N1 0.0177(10) 0.0222(10) 0.0189(10) -0.0004(8) -0.0001(8) -0.0005(8) N2 0.0174(10) 0.0235(10) 0.0185(10) -0.0005(8) -0.0007(8) -0.0001(8) N3 0.0195(10) 0.0231(10) 0.0170(9) -0.0002(8) -0.0009(8) -0.0004(8) N4 0.0190(10) 0.0222(10) 0.0179(10) -0.0012(8) 0.0015(8) 0.0005(8) N5 0.0197(10) 0.0232(10) 0.0163(9) 0.0014(8) -0.0021(8) -0.0024(8) N6 0.0195(10) 0.0236(10) 0.0177(10) 0.0024(8) -0.0014(8) -0.0030(8) N7 0.0262(12) 0.0389(13) 0.0207(11) -0.0015(9) 0.0030(9) -0.0114(10) N8 0.0234(11) 0.0386(13) 0.0227(11) -0.0030(9) 0.0032(9) -0.0093(9) N9 0.0341(13) 0.0320(13) 0.0235(11) 0.0006(10) -0.0015(10) -0.0071(10) N10 0.0272(12) 0.0350(13) 0.0254(11) -0.0047(10) -0.0030(9) -0.0015(10) N11 0.0251(11) 0.0264(11) 0.0232(11) -0.0002(9) 0.0030(9) 0.0011(9) N12 0.0268(12) 0.0315(12) 0.0230(11) -0.0001(9) 0.0022(9) -0.0030(9) N13 0.074(3) 0.099(3) 0.071(3) -0.017(2) 0.006(2) 0.012(2) N14 0.138(4) 0.061(3) 0.077(3) 0.013(2) 0.028(3) 0.013(3) O1 0.0173(8) 0.0247(9) 0.0260(9) -0.0015(7) -0.0040(7) 0.0008(7) O2 0.0184(9) 0.0250(9) 0.0255(9) -0.0042(7) -0.0049(7) 0.0012(7) O3 0.0383(12) 0.0638(15) 0.0248(10) -0.0094(10) 0.0093(9) -0.0297(11) O4 0.0310(11) 0.0700(16) 0.0304(11) -0.0167(11) 0.0122(9) -0.0246(11) B1 0.049(2) 0.070(3) 0.036(2) -0.003(2) 0.0108(18) -0.020(2) B2 0.0250(14) 0.0244(14) 0.0218(14) -0.0010(11) -0.0014(11) 0.0007(11) F1 0.0641(15) 0.104(2) 0.0484(13) -0.0224(13) 0.0245(11) -0.0430(14) F2 0.0815(18) 0.0720(17) 0.0480(13) 0.0070(11) 0.0139(12) -0.0192(14) F3 0.0238(8) 0.0310(8) 0.0264(8) -0.0017(6) -0.0040(6) 0.0006(6) F4 0.0322(9) 0.0390(9) 0.0241(8) 0.0002(7) 0.0021(7) -0.0035(7) C1 0.0219(12) 0.0216(12) 0.0226(12) -0.0027(9) 0.0017(10) -0.0017(9) C2 0.0204(12) 0.0233(12) 0.0207(12) -0.0030(9) 0.0002(9) -0.0006(9) C3 0.0195(12) 0.0218(12) 0.0331(14) -0.0033(10) -0.0063(10) 0.0009(9) C4 0.0210(12) 0.0210(12) 0.0223(12) -0.0008(9) 0.0013(9) 0.0013(9) C5 0.0214(12) 0.0217(11) 0.0197(11) 0.0006(9) 0.0010(9) 0.0008(9) C6 0.0215(12) 0.0222(12) 0.0260(13) -0.0073(10) -0.0047(10) 0.0022(9) C7 0.053(2) 0.051(2) 0.0317(17) -0.0022(14) 0.0115(15) -0.0143(16) C8 0.0249(13) 0.0348(15) 0.0290(14) 0.0011(11) 0.0021(11) 0.0047(11) C9 0.0236(13) 0.0227(12) 0.0366(15) -0.0058(11) -0.0008(11) 0.0034(10) C10 0.0306(14) 0.0283(13) 0.0252(13) -0.0024(10) -0.0056(11) 0.0033(11) C11 0.0238(14) 0.0474(18) 0.0461(18) -0.0175(15) 0.0050(13) 0.0029(13) C12 0.0258(15) 0.0405(17) 0.0497(19) -0.0202(15) -0.0135(13) 0.0125(12) C13 0.0406(17) 0.0288(14) 0.0365(16) -0.0038(12) -0.0138(13) 0.0096(12) C14 0.0255(14) 0.0329(15) 0.0351(15) -0.0066(12) 0.0037(11) -0.0004(11) C15 0.0257(13) 0.0213(12) 0.0348(15) -0.0060(11) -0.0020(11) 0.0011(10) C16 0.0235(13) 0.0282(14) 0.0437(17) 0.0004(12) -0.0020(12) 0.0000(11) C17 0.0265(15) 0.0300(15) 0.071(2) 0.0034(15) -0.0007(15) -0.0038(12) C18 0.0382(17) 0.0302(15) 0.055(2) -0.0197(14) -0.0140(15) 0.0081(13) C19 0.0292(16) 0.0255(15) 0.082(3) -0.0099(16) -0.0148(17) -0.0033(12) C20 0.0267(14) 0.0279(14) 0.0379(16) -0.0081(12) -0.0049(12) 0.0047(11) C21 0.0955(19) 0.0626(14) 0.0527(13) 0.0093(10) 0.0191(12) 0.0033(12) C22 0.0955(19) 0.0626(14) 0.0527(13) 0.0093(10) 0.0191(12) 0.0033(12) C23 0.068(3) 0.045(2) 0.045(2) 0.0038(16) -0.0076(18) -0.0085(18) C24 0.052(2) 0.056(2) 0.050(2) -0.0002(17) 0.0144(18) -0.0051(18) C25 0.0955(19) 0.0626(14) 0.0527(13) 0.0093(10) 0.0191(12) 0.0033(12) C26 0.0955(19) 0.0626(14) 0.0527(13) 0.0093(10) 0.0191(12) 0.0033(12) C27 0.0228(12) 0.0223(12) 0.0172(11) 0.0005(9) -0.0024(9) 0.0011(9) C28 0.0389(17) 0.0374(17) 0.0321(15) -0.0041(13) 0.0015(13) -0.0005(13) C29 0.0195(12) 0.0417(16) 0.0223(13) -0.0071(11) 0.0013(10) -0.0041(11) C30 0.0227(12) 0.0280(13) 0.0196(12) 0.0021(10) -0.0019(10) -0.0074(10) C31 0.0211(12) 0.0214(12) 0.0201(12) 0.0023(9) -0.0032(9) -0.0026(9) C32 0.0282(14) 0.0339(14) 0.0175(12) 0.0025(10) -0.0034(10) -0.0123(11) C33 0.0270(14) 0.0429(17) 0.0367(16) -0.0106(13) 0.0054(12) -0.0035(12) C34 0.0334(17) 0.076(3) 0.0325(16) -0.0208(17) 0.0095(13) -0.0062(16) C35 0.0340(17) 0.056(2) 0.054(2) -0.0276(18) 0.0103(15) -0.0048(15) C36 0.0326(16) 0.068(2) 0.0265(15) -0.0030(15) 0.0062(12) -0.0058(15) C37 0.0273(14) 0.0461(17) 0.0247(14) -0.0040(12) 0.0042(11) -0.0052(12) C38 0.0336(15) 0.0381(16) 0.0309(15) 0.0041(12) -0.0065(12) -0.0194(13) C39 0.0304(15) 0.0333(15) 0.0328(15) 0.0010(12) -0.0028(12) -0.0080(12) C40 0.0383(16) 0.0294(14) 0.0300(14) 0.0071(11) -0.0030(12) -0.0122(12) C41 0.0296(14) 0.0331(14) 0.0242(13) 0.0058(11) -0.0027(11) -0.0081(11) C42 0.0291(15) 0.0415(17) 0.0369(16) 0.0049(13) -0.0065(12) -0.0105(13) C43 0.0231(12) 0.0227(12) 0.0204(12) 0.0001(9) -0.0046(9) -0.0030(9) C44 0.0252(13) 0.0247(12) 0.0195(12) -0.0022(9) -0.0028(10) -0.0005(10) C17A 0.059(2) 0.055(2) 0.046(2) -0.0038(17) 0.0054(18) -0.0075(19) C18A 0.069(3) 0.056(2) 0.047(2) 0.0070(18) 0.0151(19) -0.007(2) C27A 0.0426(18) 0.0363(16) 0.0277(15) -0.0014(12) -0.0035(13) -0.0061(13) C28A 0.0243(13) 0.0301(13) 0.0190(12) -0.0011(10) 0.0005(10) -0.0017(10) B3 0.045(2) 0.0327(18) 0.053(2) -0.0051(16) 0.0084(18) 0.0044(15) F5 0.0642(18) 0.127(3) 0.140(3) 0.097(2) 0.0312(19) 0.0171(18) F6 0.145(3) 0.156(3) 0.115(3) 0.083(3) 0.066(3) 0.115(3) F7 0.030(2) 0.043(3) 0.053(3) 0.001(2) 0.005(2) 0.0087(19) F7A 0.189(11) 0.078(6) 0.045(4) -0.029(4) -0.043(6) 0.090(6) F8 0.134(6) 0.052(3) 0.071(4) -0.022(3) 0.039(4) -0.025(4) F8A 0.067(4) 0.080(5) 0.146(7) -0.045(5) -0.005(4) -0.013(3) B4 0.0276(16) 0.0410(19) 0.0307(16) 0.0056(14) 0.0005(13) -0.0031(13) F9 0.0419(11) 0.0715(14) 0.0289(9) 0.0013(9) -0.0062(8) 0.0046(10) F10 0.042(3) 0.0272(19) 0.030(2) -0.0010(14) 0.0053(19) -0.0028(17) F10A 0.071(4) 0.117(6) 0.031(3) 0.007(3) 0.002(3) -0.057(4) F11 0.058(3) 0.051(3) 0.129(6) 0.011(3) -0.043(4) -0.003(3) F11A 0.038(2) 0.0301(18) 0.0346(19) 0.0007(15) -0.0004(16) 0.0098(15) F12 0.040(3) 0.167(7) 0.035(3) -0.023(4) -0.003(2) 0.013(4) F12A 0.0274(19) 0.051(2) 0.0213(17) 0.0048(18) 0.0003(14) -0.0155(18) _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 Co1 N2 1.916(2) . ? Co1 N3 1.929(2) . ? Co1 N4 1.981(2) . ? Co1 N1 1.984(2) . ? Co1 N12 2.137(2) . ? Co1 N11 2.182(2) . ? Co2 N8 1.910(2) . ? Co2 N7 1.923(2) . ? Co2 N5 1.974(2) . ? Co2 N6 1.984(2) . ? Co2 N10 2.137(3) . ? Co2 N9 2.165(3) . ? N1 N4 1.331(3) 3_565 ? N1 C1 1.356(3) . ? N2 C2 1.295(3) . ? N2 O1 1.355(3) . ? N3 C5 1.290(3) . ? N3 O2 1.357(3) . ? N4 N1 1.331(3) 3_565 ? N4 C4 1.353(3) . ? N5 N6 1.333(3) 3_666 ? N5 C27 1.355(3) . ? N6 N5 1.333(3) 3_666 ? N6 C31 1.350(3) . ? N7 C30 1.290(3) . ? N7 O3 1.360(3) . ? N8 C28A 1.294(3) . ? N8 O4 1.356(3) . ? N9 C27A 1.124(4) . ? N10 C28 1.126(4) . ? N11 C8 1.132(4) . ? N12 C7 1.114(4) . ? N13 C17A 1.157(6) . ? N14 C18A 1.144(6) . ? O1 B2 1.488(3) . ? O2 B2 1.502(3) . ? O3 B1 1.480(5) . ? O4 B1 1.433(5) . ? B1 F1 1.379(5) . ? B1 F2 1.397(6) . ? B2 F3 1.369(3) . ? B2 F4 1.377(4) . ? C1 C15 1.391(4) . ? C1 C2 1.465(3) . ? C2 C3 1.486(3) . ? C3 C20 1.386(4) . ? C3 C16 1.394(4) . ? C4 C9 1.396(4) . ? C4 C5 1.462(3) . ? C5 C6 1.485(3) . ? C6 C14 1.391(4) . ? C6 C10 1.396(4) . ? C7 C22 1.464(6) . ? C8 C21 1.467(5) . ? C9 C15 1.366(4) 3_565 ? C10 C13 1.398(4) . ? C11 C12 1.382(5) . ? C11 C14 1.391(4) . ? C12 C13 1.378(5) . ? C15 C9 1.366(4) 3_565 ? C16 C17 1.393(4) . ? C17 C19 1.373(5) . ? C18 C19 1.388(5) . ? C18 C20 1.397(4) . ? C23 C18A 1.437(6) . ? C24 C17A 1.421(6) . ? C25 C28 1.460(6) . ? C26 C27A 1.472(5) . ? C27 C44 1.396(3) 3_666 ? C27 C28A 1.461(4) . ? C29 C33 1.391(4) . ? C29 C37 1.403(4) . ? C29 C28A 1.482(4) . ? C30 C31 1.460(4) . ? C30 C32 1.490(3) . ? C31 C43 1.391(4) . ? C32 C41 1.384(4) . ? C32 C39 1.393(4) . ? C33 C35 1.400(5) . ? C34 C36 1.378(5) . ? C34 C35 1.392(6) . ? C36 C37 1.386(4) . ? C38 C42 1.383(5) . ? C38 C40 1.383(4) . ? C39 C42 1.390(4) . ? C40 C41 1.393(4) . ? C43 C44 1.371(4) . ? C44 C27 1.396(3) 3_666 ? B3 F5 1.333(5) . ? B3 F7A 1.345(9) . ? B3 F6 1.348(5) . ? B3 F8 1.350(7) . ? B3 F7 1.387(8) . ? B3 F8A 1.429(8) . ? F7 F7A 0.666(13) . ? F8 F8A 1.033(9) . ? B4 F11 1.330(6) . ? B4 F12A 1.340(5) . ? B4 F10 1.343(6) . ? B4 F10A 1.376(6) . ? B4 F9 1.394(4) . ? B4 F11A 1.454(5) . ? B4 F12 1.468(6) . ? F10 F10A 0.776(7) . ? F10A F11A 1.748(9) . ? F11 F11A 1.078(8) . ? F11 F12A 1.473(8) . ? F12 F12A 0.954(8) . ? 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 Co1 N3 93.51(9) . . ? N2 Co1 N4 174.05(9) . . ? N3 Co1 N4 81.25(9) . . ? N2 Co1 N1 80.99(9) . . ? N3 Co1 N1 174.41(9) . . ? N4 Co1 N1 104.20(8) . . ? N2 Co1 N12 91.98(9) . . ? N3 Co1 N12 96.04(9) . . ? N4 Co1 N12 91.36(9) . . ? N1 Co1 N12 85.19(9) . . ? N2 Co1 N11 87.41(9) . . ? N3 Co1 N11 89.31(9) . . ? N4 Co1 N11 89.72(8) . . ? N1 Co1 N11 89.45(8) . . ? N12 Co1 N11 174.64(9) . . ? N8 Co2 N7 93.30(10) . . ? N8 Co2 N5 81.46(9) . . ? N7 Co2 N5 174.75(9) . . ? N8 Co2 N6 174.74(9) . . ? N7 Co2 N6 81.54(9) . . ? N5 Co2 N6 103.71(9) . . ? N8 Co2 N10 90.47(10) . . ? N7 Co2 N10 91.25(10) . . ? N5 Co2 N10 88.74(9) . . ? N6 Co2 N10 88.64(9) . . ? N8 Co2 N9 90.83(10) . . ? N7 Co2 N9 90.69(10) . . ? N5 Co2 N9 89.45(9) . . ? N6 Co2 N9 90.25(9) . . ? N10 Co2 N9 177.60(9) . . ? N4 N1 C1 119.8(2) 3_565 . ? N4 N1 Co1 127.34(16) 3_565 . ? C1 N1 Co1 112.64(16) . . ? C2 N2 O1 115.6(2) . . ? C2 N2 Co1 118.60(17) . . ? O1 N2 Co1 125.15(16) . . ? C5 N3 O2 115.1(2) . . ? C5 N3 Co1 117.59(17) . . ? O2 N3 Co1 126.85(16) . . ? N1 N4 C4 119.5(2) 3_565 . ? N1 N4 Co1 128.06(16) 3_565 . ? C4 N4 Co1 112.38(16) . . ? N6 N5 C27 120.1(2) 3_666 . ? N6 N5 Co2 127.49(16) 3_666 . ? C27 N5 Co2 112.42(17) . . ? N5 N6 C31 119.1(2) 3_666 . ? N5 N6 Co2 128.79(16) 3_666 . ? C31 N6 Co2 112.09(17) . . ? C30 N7 O3 115.5(2) . . ? C30 N7 Co2 117.52(18) . . ? O3 N7 Co2 126.94(17) . . ? C28A N8 O4 115.8(2) . . ? C28A N8 Co2 118.33(19) . . ? O4 N8 Co2 125.41(17) . . ? C27A N9 Co2 164.7(3) . . ? C28 N10 Co2 172.8(3) . . ? C8 N11 Co1 166.4(2) . . ? C7 N12 Co1 165.9(3) . . ? N2 O1 B2 115.12(19) . . ? N3 O2 B2 115.55(19) . . ? N7 O3 B1 117.5(2) . . ? N8 O4 B1 117.5(3) . . ? F1 B1 F2 112.0(4) . . ? F1 B1 O4 106.8(4) . . ? F2 B1 O4 108.5(3) . . ? F1 B1 O3 106.5(3) . . ? F2 B1 O3 108.0(4) . . ? O4 B1 O3 115.0(3) . . ? F3 B2 F4 113.2(2) . . ? F3 B2 O1 105.3(2) . . ? F4 B2 O1 110.8(2) . . ? F3 B2 O2 105.8(2) . . ? F4 B2 O2 110.4(2) . . ? O1 B2 O2 111.0(2) . . ? N1 C1 C15 122.4(2) . . ? N1 C1 C2 114.6(2) . . ? C15 C1 C2 123.0(2) . . ? N2 C2 C1 112.6(2) . . ? N2 C2 C3 123.2(2) . . ? C1 C2 C3 124.2(2) . . ? C20 C3 C16 120.3(3) . . ? C20 C3 C2 121.6(3) . . ? C16 C3 C2 118.1(2) . . ? N4 C4 C9 122.3(2) . . ? N4 C4 C5 115.1(2) . . ? C9 C4 C5 122.6(2) . . ? N3 C5 C4 113.3(2) . . ? N3 C5 C6 124.2(2) . . ? C4 C5 C6 122.5(2) . . ? C14 C6 C10 120.4(3) . . ? C14 C6 C5 119.6(2) . . ? C10 C6 C5 120.1(2) . . ? N12 C7 C22 179.5(5) . . ? N11 C8 C21 178.1(4) . . ? C15 C9 C4 118.2(2) 3_565 . ? C13 C10 C6 118.9(3) . . ? C12 C11 C14 120.0(3) . . ? C13 C12 C11 120.5(3) . . ? C12 C13 C10 120.5(3) . . ? C11 C14 C6 119.8(3) . . ? C9 C15 C1 117.7(2) 3_565 . ? C17 C16 C3 119.7(3) . . ? C19 C17 C16 120.0(3) . . ? C19 C18 C20 119.8(3) . . ? C17 C19 C18 120.8(3) . . ? C3 C20 C18 119.5(3) . . ? N5 C27 C44 122.3(2) . 3_666 ? N5 C27 C28A 114.9(2) . . ? C44 C27 C28A 122.8(2) 3_666 . ? N10 C28 C25 179.0(4) . . ? C33 C29 C37 120.5(3) . . ? C33 C29 C28A 120.6(3) . . ? C37 C29 C28A 119.0(3) . . ? N7 C30 C31 113.6(2) . . ? N7 C30 C32 125.0(2) . . ? C31 C30 C32 121.4(2) . . ? N6 C31 C43 122.9(2) . . ? N6 C31 C30 115.2(2) . . ? C43 C31 C30 121.9(2) . . ? C41 C32 C39 120.7(3) . . ? C41 C32 C30 119.1(3) . . ? C39 C32 C30 120.2(3) . . ? C29 C33 C35 119.2(3) . . ? C36 C34 C35 120.9(3) . . ? C34 C35 C33 119.8(3) . . ? C34 C36 C37 119.9(3) . . ? C36 C37 C29 119.7(3) . . ? C42 C38 C40 120.5(3) . . ? C42 C39 C32 119.2(3) . . ? C38 C40 C41 119.8(3) . . ? C32 C41 C40 119.6(3) . . ? C38 C42 C39 120.2(3) . . ? C44 C43 C31 118.0(2) . . ? C43 C44 C27 117.6(2) . 3_666 ? N13 C17A C24 178.4(5) . . ? N14 C18A C23 178.2(5) . . ? N9 C27A C26 178.7(4) . . ? N8 C28A C27 112.8(2) . . ? N8 C28A C29 124.1(2) . . ? C27 C28A C29 123.0(2) . . ? F5 B3 F7A 101.5(6) . . ? F5 B3 F6 111.5(4) . . ? F7A B3 F6 107.2(5) . . ? F5 B3 F8 112.0(4) . . ? F7A B3 F8 135.6(7) . . ? F6 B3 F8 87.2(5) . . ? F5 B3 F7 124.5(4) . . ? F7A B3 F7 28.1(5) . . ? F6 B3 F7 107.7(5) . . ? F8 B3 F7 107.7(5) . . ? F5 B3 F8A 100.7(5) . . ? F7A B3 F8A 103.5(6) . . ? F6 B3 F8A 129.1(5) . . ? F8 B3 F8A 43.5(4) . . ? F7 B3 F8A 82.7(5) . . ? F7A F7 B3 72.4(12) . . ? F7 F7A B3 79.4(13) . . ? F8A F8 B3 72.3(5) . . ? F8 F8A B3 64.1(5) . . ? F11 B4 F12A 66.9(4) . . ? F11 B4 F10 143.6(4) . . ? F12A B4 F10 114.4(4) . . ? F11 B4 F10A 113.2(5) . . ? F12A B4 F10A 123.3(4) . . ? F10 B4 F10A 33.1(3) . . ? F11 B4 F9 108.7(3) . . ? F12A B4 F9 113.8(3) . . ? F10 B4 F9 103.5(3) . . ? F10A B4 F9 118.2(4) . . ? F11 B4 F11A 45.3(4) . . ? F12A B4 F11A 108.7(3) . . ? F10 B4 F11A 109.1(3) . . ? F10A B4 F11A 76.2(4) . . ? F9 B4 F11A 107.0(3) . . ? F11 B4 F12 105.8(5) . . ? F12A B4 F12 39.4(3) . . ? F10 B4 F12 79.6(4) . . ? F10A B4 F12 102.5(5) . . ? F9 B4 F12 107.2(3) . . ? F11A B4 F12 141.3(4) . . ? F10A F10 B4 75.7(7) . . ? F10 F10A B4 71.1(6) . . ? F10 F10A F11A 124.6(8) . . ? B4 F10A F11A 53.9(3) . . ? F11A F11 B4 73.5(4) . . ? F11A F11 F12A 125.2(5) . . ? B4 F11 F12A 56.9(3) . . ? F11 F11A B4 61.3(4) . . ? F11 F11A F10A 103.6(5) . . ? B4 F11A F10A 49.9(3) . . ? F12A F12 B4 63.1(4) . . ? F12 F12A B4 77.5(5) . . ? F12 F12A F11 132.8(6) . . ? B4 F12A F11 56.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.908 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.083 #===END data_nks3-115 _database_code_depnum_ccdc_archive 'CCDC 740049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H21 B6 F12 N12 O4 Zn2' _chemical_formula_weight 917.09 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' F F 0.0171 0.0103 '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 12.0885(9) _cell_length_b 12.2379(10) _cell_length_c 22.2619(18) _cell_angle_alpha 90.00 _cell_angle_beta 103.5470(10) _cell_angle_gamma 90.00 _cell_volume 3201.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9641 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 29.95 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.73 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _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 BrukerP4 _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77302 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.57 _reflns_number_total 8967 _reflns_number_gt 7292 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0547P)^2^+6.2757P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8967 _refine_ls_number_parameters 479 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.053 _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 0.48710(2) 0.09295(2) 0.226695(13) 0.02120(8) Uani 1 1 d . . . Zn2 Zn 0.65661(3) 0.02722(2) 0.384035(14) 0.02178(8) Uani 1 1 d . . . N1 N 0.31422(19) 0.08263(18) 0.18818(10) 0.0229(4) Uani 1 1 d . . . N2 N 0.42007(18) 0.01326(17) 0.29557(10) 0.0207(4) Uani 1 1 d . . . N3 N 0.48178(19) -0.01632(18) 0.35047(10) 0.0217(4) Uani 1 1 d . . . N4 N 0.6094(2) -0.04759(18) 0.45932(10) 0.0233(4) Uani 1 1 d . . . N5 N 0.8074(2) -0.0599(2) 0.41347(10) 0.0248(4) Uani 1 1 d . . . N6 N 0.69339(18) -0.03703(18) 0.30089(10) 0.0212(4) Uani 1 1 d . . . N7 N 0.63229(18) -0.01396(17) 0.24468(10) 0.0210(4) Uani 1 1 d . . . N8 N 0.51360(19) 0.05565(19) 0.14035(10) 0.0225(4) Uani 1 1 d . . . C1 C 0.8479(2) -0.1167(2) 0.37444(12) 0.0239(5) Uani 1 1 d . . . C2 C 0.7853(2) -0.1012(2) 0.30915(12) 0.0222(5) Uani 1 1 d . . . C3 C 0.6619(2) -0.0523(2) 0.19445(12) 0.0218(5) Uani 1 1 d . . . C4 C 0.5887(2) -0.0153(2) 0.13454(12) 0.0230(5) Uani 1 1 d . . . C5 C 0.5141(2) -0.0993(2) 0.45035(12) 0.0230(5) Uani 1 1 d . . . C6 C 0.4352(2) -0.0722(2) 0.39011(12) 0.0225(5) Uani 1 1 d . . . C7 C 0.3087(2) -0.0088(2) 0.27876(12) 0.0222(5) Uani 1 1 d . . . C8 C 0.2498(2) 0.0285(2) 0.21577(12) 0.0238(5) Uani 1 1 d . . . C9 C 0.8173(2) -0.1481(2) 0.25831(13) 0.0270(5) Uani 1 1 d . . . H9 H 0.8806 -0.1961 0.2640 0.032 Uiso 1 1 calc R . . C10 C 0.7552(2) -0.1231(2) 0.20024(13) 0.0274(5) Uani 1 1 d . . . H10 H 0.7748 -0.1529 0.1647 0.033 Uiso 1 1 calc R . . C11 C 0.2552(2) -0.0672(2) 0.31841(13) 0.0266(5) Uani 1 1 d . . . H11 H 0.1761 -0.0828 0.3067 0.032 Uiso 1 1 calc R . . C12 C 0.3202(2) -0.1012(2) 0.37459(12) 0.0272(5) Uani 1 1 d . . . H12 H 0.2878 -0.1432 0.4020 0.033 Uiso 1 1 calc R . . C13 C 0.1295(3) -0.0020(3) 0.18846(15) 0.0357(7) Uani 1 1 d . . . H13A H 0.1044 0.0321 0.1477 0.054 Uiso 1 1 calc R . . H13B H 0.0814 0.0235 0.2155 0.054 Uiso 1 1 calc R . . H13C H 0.1234 -0.0816 0.1842 0.054 Uiso 1 1 calc R . . C14 C 0.6016(3) -0.0603(3) 0.07451(13) 0.0340(6) Uani 1 1 d . . . H14A H 0.5281 -0.0884 0.0512 0.051 Uiso 1 1 calc R . . H14B H 0.6575 -0.1197 0.0821 0.051 Uiso 1 1 calc R . . H14C H 0.6276 -0.0024 0.0507 0.051 Uiso 1 1 calc R . . C15 C 0.9458(2) -0.1926(3) 0.39323(14) 0.0311(6) Uani 1 1 d . . . H15A H 1.0077 -0.1557 0.4225 0.047 Uiso 1 1 calc R . . H15B H 0.9723 -0.2148 0.3567 0.047 Uiso 1 1 calc R . . H15C H 0.9220 -0.2573 0.4129 0.047 Uiso 1 1 calc R . . C16 C 0.4817(3) -0.1807(2) 0.49307(12) 0.0274(5) Uani 1 1 d . . . H16A H 0.4761 -0.2534 0.4741 0.041 Uiso 1 1 calc R . . H16B H 0.4081 -0.1605 0.5011 0.041 Uiso 1 1 calc R . . H16C H 0.5397 -0.1817 0.5321 0.041 Uiso 1 1 calc R . . O1 O 0.26732(17) 0.11290(17) 0.12832(9) 0.0275(4) Uani 1 1 d . . . O2 O 0.43974(17) 0.08870(16) 0.08679(9) 0.0259(4) Uani 1 1 d . . . O3 O 0.68616(17) -0.06708(16) 0.51422(8) 0.0262(4) Uani 1 1 d . . . O4 O 0.86016(17) -0.07418(17) 0.47418(9) 0.0277(4) Uani 1 1 d . . . B1 B 0.3521(3) 0.1666(3) 0.09886(15) 0.0266(6) Uani 1 1 d . . . B2 B 0.7987(3) -0.0153(3) 0.51487(14) 0.0263(6) Uani 1 1 d . . . B3 B 0.5761(3) 0.2527(2) 0.33177(14) 0.0243(6) Uani 1 1 d . . . F1 F 0.29331(15) 0.20268(15) 0.04255(8) 0.0347(4) Uani 1 1 d . . . F2 F 0.40671(15) 0.24976(13) 0.13792(8) 0.0303(3) Uani 1 1 d . . . F3 F 0.78107(14) 0.09366(13) 0.49549(8) 0.0285(3) Uani 1 1 d . . . F4 F 0.86296(15) -0.02375(14) 0.57421(8) 0.0322(4) Uani 1 1 d . . . F5 F 0.46800(14) 0.23731(14) 0.34251(8) 0.0294(3) Uani 1 1 d . . . F6 F 0.56929(16) 0.21958(16) 0.26711(9) 0.0374(4) Uani 1 1 d . . . F7 F 0.60997(15) 0.36148(13) 0.33927(8) 0.0301(3) Uani 1 1 d . . . F8 F 0.65896(16) 0.18456(16) 0.37576(9) 0.0389(4) Uani 1 1 d . . . O5 O 0.8604(2) 0.2850(2) 0.41489(13) 0.0459(6) Uani 1 1 d . . . C17 C 0.9495(3) 0.2100(3) 0.40756(19) 0.0483(9) Uani 1 1 d . . . H17A H 0.9215 0.1642 0.3704 0.058 Uiso 1 1 calc R . . H17B H 0.9692 0.1611 0.4439 0.058 Uiso 1 1 calc R . . C18 C 1.0551(4) 0.2723(4) 0.4010(3) 0.0678(13) Uani 1 1 d . . . H18A H 1.0375 0.3149 0.3627 0.102 Uiso 1 1 calc R . . H18B H 1.1163 0.2204 0.3998 0.102 Uiso 1 1 calc R . . H18C H 1.0796 0.3216 0.4363 0.102 Uiso 1 1 calc R . . C19 C 0.8856(5) 0.3456(5) 0.4726(2) 0.0796(17) Uani 1 1 d D . . C20 C 0.7895(10) 0.4026(9) 0.4865(5) 0.039(3) Uiso 0.50 1 d P . . C20A C 0.7494(16) 0.341(2) 0.4779(10) 0.066(5) Uiso 0.25 1 d PD . . C20B C 0.7760(15) 0.3854(11) 0.4858(9) 0.033(5) Uani 0.25 1 d P . . B4 B 0.8618(3) 0.1706(3) 0.22287(18) 0.0357(7) Uani 1 1 d . . . F9 F 0.9094(2) 0.08288(19) 0.25714(13) 0.0613(6) Uani 1 1 d . . . F10 F 0.7844(5) 0.2301(6) 0.2587(3) 0.0289(14) Uiso 0.33 1 d P . . F10A F 0.7831(6) 0.1965(6) 0.2553(4) 0.0332(16) Uiso 0.33 1 d P . . F10B F 0.7576(6) 0.2041(6) 0.2274(4) 0.0495(16) Uiso 0.33 1 d P . . F11 F 0.93974(17) 0.25371(17) 0.22525(11) 0.0472(5) Uani 1 1 d . . . F12 F 0.8180(12) 0.1528(12) 0.1609(6) 0.067(4) Uiso 0.33 1 d P . . F12A F 0.8446(8) 0.1206(8) 0.1640(4) 0.056(2) Uiso 0.33 1 d P . . F12B F 0.7905(7) 0.1500(7) 0.1672(4) 0.042(2) Uiso 0.33 1 d P . . 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 0.02152(14) 0.02386(15) 0.02058(14) 0.00314(11) 0.00970(11) 0.00229(11) Zn2 0.02417(15) 0.02305(15) 0.02055(14) 0.00157(11) 0.01017(11) 0.00474(11) N1 0.0245(10) 0.0244(10) 0.0209(10) 0.0035(8) 0.0073(8) 0.0042(8) N2 0.0235(10) 0.0200(10) 0.0209(10) 0.0017(8) 0.0102(8) 0.0023(8) N3 0.0258(10) 0.0214(10) 0.0209(10) 0.0021(8) 0.0113(8) 0.0035(8) N4 0.0301(11) 0.0233(10) 0.0175(10) -0.0003(8) 0.0077(8) 0.0055(9) N5 0.0259(11) 0.0280(11) 0.0207(10) -0.0010(8) 0.0059(8) 0.0029(9) N6 0.0214(10) 0.0233(10) 0.0210(10) 0.0005(8) 0.0093(8) 0.0012(8) N7 0.0228(10) 0.0217(10) 0.0205(10) 0.0015(8) 0.0094(8) 0.0002(8) N8 0.0229(10) 0.0251(10) 0.0208(10) 0.0039(8) 0.0078(8) -0.0021(8) C1 0.0215(11) 0.0268(12) 0.0243(12) -0.0020(10) 0.0070(9) 0.0013(9) C2 0.0209(11) 0.0236(12) 0.0241(12) -0.0021(9) 0.0093(9) -0.0002(9) C3 0.0232(12) 0.0231(11) 0.0216(11) -0.0015(9) 0.0104(9) -0.0024(9) C4 0.0257(12) 0.0245(12) 0.0215(11) 0.0000(9) 0.0107(9) -0.0030(9) C5 0.0322(13) 0.0207(11) 0.0191(11) -0.0007(9) 0.0120(10) 0.0038(10) C6 0.0301(13) 0.0201(11) 0.0206(11) -0.0012(9) 0.0124(10) 0.0013(9) C7 0.0249(12) 0.0212(11) 0.0231(11) -0.0004(9) 0.0109(9) 0.0001(9) C8 0.0250(12) 0.0246(12) 0.0236(12) 0.0010(10) 0.0091(10) 0.0018(10) C9 0.0220(12) 0.0317(14) 0.0289(13) -0.0054(11) 0.0092(10) 0.0048(10) C10 0.0246(12) 0.0335(14) 0.0266(13) -0.0069(11) 0.0109(10) 0.0022(10) C11 0.0266(13) 0.0314(13) 0.0241(12) -0.0014(10) 0.0109(10) -0.0067(10) C12 0.0342(14) 0.0288(13) 0.0226(12) -0.0009(10) 0.0146(11) -0.0058(11) C13 0.0282(14) 0.0461(17) 0.0320(15) 0.0058(13) 0.0055(11) -0.0063(13) C14 0.0463(17) 0.0357(15) 0.0233(13) -0.0006(11) 0.0148(12) 0.0052(13) C15 0.0279(13) 0.0350(15) 0.0304(14) -0.0029(12) 0.0068(11) 0.0089(11) C16 0.0376(15) 0.0248(12) 0.0233(12) 0.0039(10) 0.0142(11) 0.0022(11) O1 0.0256(9) 0.0348(10) 0.0221(9) 0.0084(8) 0.0055(7) 0.0021(8) O2 0.0289(9) 0.0297(10) 0.0197(8) 0.0058(7) 0.0067(7) 0.0022(8) O3 0.0327(10) 0.0279(9) 0.0181(8) 0.0022(7) 0.0061(7) 0.0049(8) O4 0.0298(10) 0.0322(10) 0.0203(9) -0.0010(7) 0.0043(7) 0.0071(8) B1 0.0304(15) 0.0250(14) 0.0262(14) 0.0057(11) 0.0102(12) 0.0010(11) B2 0.0326(15) 0.0271(14) 0.0193(13) -0.0016(11) 0.0063(11) 0.0050(12) B3 0.0259(14) 0.0207(13) 0.0284(14) 0.0014(11) 0.0106(11) 0.0022(10) F1 0.0379(9) 0.0377(9) 0.0284(9) 0.0128(7) 0.0072(7) 0.0061(8) F2 0.0372(9) 0.0250(8) 0.0302(8) 0.0040(6) 0.0111(7) 0.0000(7) F3 0.0333(9) 0.0254(8) 0.0276(8) 0.0006(6) 0.0087(7) 0.0043(6) F4 0.0374(9) 0.0350(9) 0.0224(8) -0.0020(7) 0.0036(7) 0.0072(7) F5 0.0281(8) 0.0285(8) 0.0363(9) 0.0007(7) 0.0172(7) 0.0041(6) F6 0.0399(10) 0.0377(10) 0.0374(10) 0.0014(8) 0.0145(8) 0.0002(8) F7 0.0351(9) 0.0210(7) 0.0352(9) 0.0007(7) 0.0101(7) 0.0024(6) F8 0.0420(10) 0.0363(10) 0.0384(10) -0.0002(8) 0.0096(8) 0.0046(8) O5 0.0367(12) 0.0465(14) 0.0526(15) 0.0058(12) 0.0066(11) 0.0006(11) C17 0.0367(17) 0.058(2) 0.054(2) 0.0209(18) 0.0184(16) 0.0125(16) C18 0.049(2) 0.068(3) 0.087(3) 0.034(3) 0.016(2) 0.026(2) C19 0.072(3) 0.089(4) 0.064(3) -0.026(3) -0.015(2) 0.016(3) C20B 0.043(8) 0.007(5) 0.054(9) -0.035(6) 0.022(6) -0.029(5) B4 0.0300(16) 0.0375(18) 0.0427(19) 0.0022(15) 0.0148(14) -0.0072(14) F9 0.0762(17) 0.0401(12) 0.0659(16) 0.0101(11) 0.0135(13) -0.0006(11) F11 0.0321(10) 0.0448(11) 0.0689(14) 0.0059(10) 0.0199(9) -0.0114(8) _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 F6 1.944(2) . ? Zn1 N1 2.069(2) . ? Zn1 N8 2.072(2) . ? Zn1 N2 2.131(2) . ? Zn1 N7 2.150(2) . ? Zn2 F8 1.935(2) . ? Zn2 N5 2.080(2) . ? Zn2 N4 2.103(2) . ? Zn2 N3 2.137(2) . ? Zn2 N6 2.151(2) . ? N1 C8 1.284(3) . ? N1 O1 1.371(3) . ? N2 N3 1.324(3) . ? N2 C7 1.337(3) . ? N3 C6 1.340(3) . ? N4 C5 1.288(4) . ? N4 O3 1.371(3) . ? N5 C1 1.295(3) . ? N5 O4 1.364(3) . ? N6 N7 1.326(3) . ? N6 C2 1.337(3) . ? N7 C3 1.336(3) . ? N8 C4 1.284(3) . ? N8 O2 1.372(3) . ? C1 C15 1.485(4) . ? C1 C2 1.485(4) . ? C2 C9 1.402(4) . ? C3 C10 1.405(4) . ? C3 C4 1.488(4) . ? C4 C14 1.487(4) . ? C5 C6 1.489(4) . ? C5 C16 1.491(4) . ? C6 C12 1.397(4) . ? C7 C11 1.405(3) . ? C7 C8 1.488(4) . ? C8 C13 1.486(4) . ? C9 C10 1.368(4) . ? C11 C12 1.377(4) . ? O1 B1 1.492(4) . ? O2 B1 1.496(4) . ? O3 B2 1.498(4) . ? O4 B2 1.486(4) . ? B1 F1 1.362(4) . ? B1 F2 1.399(4) . ? B2 F4 1.370(3) . ? B2 F3 1.402(4) . ? B3 F7 1.391(3) . ? B3 F5 1.395(3) . ? B3 F6 1.479(4) . ? B3 F8 1.483(4) . ? O5 C19 1.453(6) . ? O5 C17 1.453(4) . ? C17 C18 1.524(6) . ? C19 C20 1.450(13) . ? C19 C20B 1.505(19) . ? C19 C20A 1.680(19) . ? C20 C20A 0.89(2) . ? C20A C20B 0.64(2) . ? B4 F10B 1.351(8) . ? B4 F12B 1.358(9) . ? B4 F10A 1.360(8) . ? B4 F9 1.364(5) . ? B4 F12 1.374(14) . ? B4 F11 1.379(4) . ? B4 F12A 1.417(10) . ? B4 F10 1.545(7) . ? F10 F10B 0.765(9) . ? F10A F10B 0.633(9) . ? F10B F12B 1.627(11) . ? F12 F12A 0.503(17) . ? F12A F12B 0.764(13) . ? 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 F6 Zn1 N1 126.70(9) . . ? F6 Zn1 N8 115.57(8) . . ? N1 Zn1 N8 87.87(9) . . ? F6 Zn1 N2 105.73(8) . . ? N1 Zn1 N2 75.69(9) . . ? N8 Zn1 N2 137.23(9) . . ? F6 Zn1 N7 95.31(8) . . ? N1 Zn1 N7 137.85(9) . . ? N8 Zn1 N7 75.04(8) . . ? N2 Zn1 N7 91.09(8) . . ? F8 Zn2 N5 120.55(9) . . ? F8 Zn2 N4 121.46(8) . . ? N5 Zn2 N4 84.69(9) . . ? F8 Zn2 N3 104.49(8) . . ? N5 Zn2 N3 134.75(9) . . ? N4 Zn2 N3 74.89(8) . . ? F8 Zn2 N6 105.73(8) . . ? N5 Zn2 N6 75.01(8) . . ? N4 Zn2 N6 132.54(9) . . ? N3 Zn2 N6 89.70(8) . . ? C8 N1 O1 116.4(2) . . ? C8 N1 Zn1 120.04(18) . . ? O1 N1 Zn1 122.27(16) . . ? N3 N2 C7 121.0(2) . . ? N3 N2 Zn1 124.20(16) . . ? C7 N2 Zn1 114.72(17) . . ? N2 N3 C6 121.0(2) . . ? N2 N3 Zn2 123.47(16) . . ? C6 N3 Zn2 115.49(18) . . ? C5 N4 O3 116.5(2) . . ? C5 N4 Zn2 119.35(18) . . ? O3 N4 Zn2 122.19(16) . . ? C1 N5 O4 115.7(2) . . ? C1 N5 Zn2 120.32(19) . . ? O4 N5 Zn2 123.35(16) . . ? N7 N6 C2 121.1(2) . . ? N7 N6 Zn2 123.54(16) . . ? C2 N6 Zn2 115.39(17) . . ? N6 N7 C3 121.1(2) . . ? N6 N7 Zn1 123.72(16) . . ? C3 N7 Zn1 115.13(17) . . ? C4 N8 O2 116.3(2) . . ? C4 N8 Zn1 120.58(18) . . ? O2 N8 Zn1 122.04(16) . . ? N5 C1 C15 123.3(3) . . ? N5 C1 C2 113.7(2) . . ? C15 C1 C2 123.1(2) . . ? N6 C2 C9 120.5(2) . . ? N6 C2 C1 115.2(2) . . ? C9 C2 C1 124.3(2) . . ? N7 C3 C10 120.4(2) . . ? N7 C3 C4 115.1(2) . . ? C10 C3 C4 124.5(2) . . ? N8 C4 C14 124.5(3) . . ? N8 C4 C3 113.7(2) . . ? C14 C4 C3 121.8(2) . . ? N4 C5 C6 113.0(2) . . ? N4 C5 C16 126.0(3) . . ? C6 C5 C16 121.0(2) . . ? N3 C6 C12 120.9(2) . . ? N3 C6 C5 115.3(2) . . ? C12 C6 C5 123.8(2) . . ? N2 C7 C11 120.5(2) . . ? N2 C7 C8 115.5(2) . . ? C11 C7 C8 124.0(2) . . ? N1 C8 C13 125.4(3) . . ? N1 C8 C7 113.5(2) . . ? C13 C8 C7 121.0(2) . . ? C10 C9 C2 118.5(2) . . ? C9 C10 C3 118.4(2) . . ? C12 C11 C7 118.4(3) . . ? C11 C12 C6 118.1(2) . . ? N1 O1 B1 112.1(2) . . ? N8 O2 B1 112.1(2) . . ? N4 O3 B2 111.0(2) . . ? N5 O4 B2 110.9(2) . . ? F1 B1 F2 113.9(2) . . ? F1 B1 O1 106.5(2) . . ? F2 B1 O1 108.6(2) . . ? F1 B1 O2 106.3(2) . . ? F2 B1 O2 108.9(2) . . ? O1 B1 O2 112.7(2) . . ? F4 B2 F3 112.3(2) . . ? F4 B2 O4 107.4(2) . . ? F3 B2 O4 109.6(2) . . ? F4 B2 O3 106.6(2) . . ? F3 B2 O3 109.1(2) . . ? O4 B2 O3 111.8(2) . . ? F7 B3 F5 111.7(2) . . ? F7 B3 F6 109.1(2) . . ? F5 B3 F6 106.8(2) . . ? F7 B3 F8 108.9(2) . . ? F5 B3 F8 109.0(2) . . ? F6 B3 F8 111.3(2) . . ? B3 F6 Zn1 125.08(16) . . ? B3 F8 Zn2 126.86(17) . . ? C19 O5 C17 114.5(3) . . ? O5 C17 C18 110.8(3) . . ? C20 C19 O5 115.0(6) . . ? C20 C19 C20B 10.1(6) . . ? O5 C19 C20B 109.1(6) . . ? C20 C19 C20A 32.1(9) . . ? O5 C19 C20A 92.2(9) . . ? C20B C19 C20A 22.2(9) . . ? C20A C20 C19 88.3(16) . . ? C20B C20A C20 5(2) . . ? C20B C20A C19 63(2) . . ? C20 C20A C19 59.6(14) . . ? C20A C20B C19 95(2) . . ? F10B B4 F12B 73.8(5) . . ? F10B B4 F10A 27.0(4) . . ? F12B B4 F10A 98.9(5) . . ? F10B B4 F9 118.4(4) . . ? F12B B4 F9 117.3(5) . . ? F10A B4 F9 98.2(4) . . ? F10B B4 F12 88.7(7) . . ? F12B B4 F12 16.4(7) . . ? F10A B4 F12 114.7(7) . . ? F9 B4 F12 116.7(7) . . ? F10B B4 F11 114.5(4) . . ? F12B B4 F11 117.0(5) . . ? F10A B4 F11 111.4(4) . . ? F9 B4 F11 111.4(3) . . ? F12 B4 F11 104.8(6) . . ? F10B B4 F12A 105.3(6) . . ? F12B B4 F12A 31.9(6) . . ? F10A B4 F12A 128.5(6) . . ? F9 B4 F12A 97.4(5) . . ? F12 B4 F12A 20.7(7) . . ? F11 B4 F12A 107.7(5) . . ? F10B B4 F10 29.6(4) . . ? F12B B4 F10 103.1(5) . . ? F10A B4 F10 14.8(4) . . ? F9 B4 F10 108.0(4) . . ? F12 B4 F10 117.1(7) . . ? F11 B4 F10 97.1(4) . . ? F12A B4 F10 134.8(5) . . ? F10B F10 B4 60.9(7) . . ? F10B F10A B4 75.7(10) . . ? F10A F10B F10 33.1(9) . . ? F10A F10B B4 77.3(10) . . ? F10 F10B B4 89.4(8) . . ? F10A F10B F12B 126.4(13) . . ? F10 F10B F12B 141.8(9) . . ? B4 F10B F12B 53.3(4) . . ? F12A F12 B4 84(2) . . ? F12 F12A F12B 27(2) . . ? F12 F12A B4 75(2) . . ? F12B F12A B4 69.8(8) . . ? F12A F12B B4 78.4(9) . . ? F12A F12B F10B 130.4(10) . . ? B4 F12B F10B 52.9(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.113 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.102 #===END data_nks3-79 _database_code_depnum_ccdc_archive 'CCDC 740050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 B2 Cl2 Co2 F4 N9 O7' _chemical_formula_weight 822.90 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _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 36.625(3) _cell_length_b 10.9319(9) _cell_length_c 20.0900(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.1350(10) _cell_angle_gamma 90.00 _cell_volume 8022.6(11) _cell_formula_units_Z 10 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9835 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.16 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 1.15 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'Blessing, Acta Cryst.' _exptl_special_details ; ? ; _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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72610 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.36 _reflns_number_total 9997 _reflns_number_gt 6807 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Short Inter D...A Contact O12A .. O21 .. shortcontact between a solvent water and solvent acetonitrile molecule present. However, both molecules are half occupancy so not necessarily there at the same time Solvent acetonitrile molecules and perchlorate counter-anions are modelled isotropically because the displacement parameters were too big when refined using an anisotropic model. ; _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^)+(0.1281P)^2^+55.1563P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9997 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2438 _refine_ls_wR_factor_gt 0.2116 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.094 _refine_ls_shift/su_mean 0.001 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 Co1 Co 0.090457(17) 0.72935(5) 0.00749(3) 0.02679(18) Uani 1 1 d . . . Co2 Co 0.140120(16) 0.78218(5) 0.17401(3) 0.02577(17) Uani 1 1 d . . . N1 N 0.05736(11) 0.6051(3) -0.0259(2) 0.0294(8) Uani 1 1 d . . . N2 N 0.08610(10) 0.6359(3) 0.09050(19) 0.0263(8) Uani 1 1 d . . . N3 N 0.09960(10) 0.6670(3) 0.15141(19) 0.0268(8) Uani 1 1 d . . . N4 N 0.13310(11) 0.7210(4) 0.2614(2) 0.0304(8) Uani 1 1 d . . . N5 N 0.18162(11) 0.8814(4) 0.2031(2) 0.0337(9) Uani 1 1 d . . . N6 N 0.14908(10) 0.8604(3) 0.0881(2) 0.0280(8) Uani 1 1 d . . . N7 N 0.12912(11) 0.8507(3) 0.0305(2) 0.0303(8) Uani 1 1 d . . . N8 N 0.08999(13) 0.8138(4) -0.0763(2) 0.0380(10) Uani 1 1 d . . . N9 N 0.13414(12) 0.6100(4) -0.0220(2) 0.0370(9) Uani 1 1 d . . . N10 N 0.17535(12) 0.6307(4) 0.1498(2) 0.0373(10) Uani 1 1 d . . . N11 N 0.10254(11) 0.9318(3) 0.18832(19) 0.0283(8) Uani 1 1 d . . . N12 N 0.04582(12) 0.8424(3) 0.0431(2) 0.0314(9) Uani 1 1 d . . . C1 C 0.05177(13) 0.5133(4) 0.0121(3) 0.0316(10) Uani 1 1 d . . . C2 C 0.06407(12) 0.5381(4) 0.0823(2) 0.0291(9) Uani 1 1 d . . . C3 C 0.05261(14) 0.4714(4) 0.1364(3) 0.0368(11) Uani 1 1 d . . . H3 H 0.0370 0.4025 0.1296 0.044 Uiso 1 1 calc R . . C4 C 0.06444(14) 0.5076(5) 0.1990(3) 0.0371(11) Uani 1 1 d . . . H4 H 0.0564 0.4676 0.2372 0.045 Uiso 1 1 calc R . . C5 C 0.08901(13) 0.6062(4) 0.2051(3) 0.0321(10) Uani 1 1 d . . . C6 C 0.10644(14) 0.6470(5) 0.2688(3) 0.0344(10) Uani 1 1 d . . . C7 C 0.09418(17) 0.6020(6) 0.3335(3) 0.0522(15) Uani 1 1 d . . . H7A H 0.1012 0.5160 0.3396 0.078 Uiso 1 1 calc R . . H7B H 0.0675 0.6096 0.3334 0.078 Uiso 1 1 calc R . . H7C H 0.1058 0.6508 0.3701 0.078 Uiso 1 1 calc R . . C8 C 0.19674(14) 0.9460(5) 0.1596(3) 0.0393(12) Uani 1 1 d . . . C9 C 0.17823(13) 0.9366(4) 0.0928(3) 0.0348(11) Uani 1 1 d . . . C10 C 0.18857(15) 1.0040(5) 0.0382(3) 0.0426(13) Uani 1 1 d . . . H10 H 0.2097 1.0548 0.0418 0.051 Uiso 1 1 calc R . . C11 C 0.16789(16) 0.9953(5) -0.0198(3) 0.0442(13) Uani 1 1 d . . . H11 H 0.1738 1.0406 -0.0579 0.053 Uiso 1 1 calc R . . C12 C 0.13754(16) 0.9182(5) -0.0225(3) 0.0389(12) Uani 1 1 d . . . C13 C 0.11316(18) 0.9008(6) -0.0820(3) 0.0501(15) Uani 1 1 d . . . C14 C 0.1153(3) 0.9753(8) -0.1436(4) 0.088(3) Uani 1 1 d . . . H14A H 0.1309 0.9336 -0.1741 0.132 Uiso 1 1 calc R . . H14B H 0.1257 1.0557 -0.1319 0.132 Uiso 1 1 calc R . . H14C H 0.0907 0.9858 -0.1654 0.132 Uiso 1 1 calc R . . C15 C 0.15561(16) 0.5451(5) -0.0388(3) 0.0407(12) Uani 1 1 d . . . C16 C 0.1832(2) 0.4604(7) -0.0608(4) 0.0656(19) Uani 1 1 d . . . H16A H 0.1786 0.3782 -0.0439 0.098 Uiso 1 1 calc R . . H16B H 0.2076 0.4876 -0.0436 0.098 Uiso 1 1 calc R . . H16C H 0.1821 0.4587 -0.1097 0.098 Uiso 1 1 calc R . . C17 C 0.01769(15) 0.8753(4) 0.0576(2) 0.0341(11) Uani 1 1 d . . . C18 C -0.01845(17) 0.9165(5) 0.0738(3) 0.0481(14) Uani 1 1 d . . . H18A H -0.0176 1.0042 0.0838 0.072 Uiso 1 1 calc R . . H18B H -0.0259 0.8715 0.1128 0.072 Uiso 1 1 calc R . . H18C H -0.0361 0.9014 0.0357 0.072 Uiso 1 1 calc R . . C19 C 0.08194(14) 1.0079(4) 0.1921(2) 0.0334(10) Uani 1 1 d . . . C20 C 0.0552(2) 1.1058(7) 0.1984(4) 0.080(3) Uani 1 1 d . . . H20A H 0.0335 1.0729 0.2176 0.119 Uiso 1 1 calc R . . H20B H 0.0483 1.1401 0.1542 0.119 Uiso 1 1 calc R . . H20C H 0.0660 1.1702 0.2275 0.119 Uiso 1 1 calc R . . C21 C 0.19256(17) 0.5486(6) 0.1424(3) 0.0511(15) Uani 1 1 d . . . C55 C 0.03533(15) 0.3944(4) -0.0115(3) 0.0396(12) Uani 1 1 d . . . H55A H 0.0220 0.4060 -0.0551 0.059 Uiso 1 1 calc R . . H55B H 0.0184 0.3653 0.0207 0.059 Uiso 1 1 calc R . . H55C H 0.0548 0.3339 -0.0155 0.059 Uiso 1 1 calc R . . C56 C 0.22923(17) 1.0270(7) 0.1722(4) 0.0586(17) Uani 1 1 d . . . H56A H 0.2216 1.1127 0.1679 0.088 Uiso 1 1 calc R . . H56B H 0.2472 1.0091 0.1397 0.088 Uiso 1 1 calc R . . H56C H 0.2403 1.0125 0.2174 0.088 Uiso 1 1 calc R . . C57 C 0.2151(3) 0.4401(10) 0.1341(6) 0.121(5) Uani 1 1 d . . . H57A H 0.2170 0.3931 0.1758 0.182 Uiso 1 1 calc R . . H57B H 0.2397 0.4653 0.1230 0.182 Uiso 1 1 calc R . . H57C H 0.2039 0.3892 0.0980 0.182 Uiso 1 1 calc R . . B1 B 0.03684(19) 0.7068(5) -0.1267(3) 0.0382(13) Uani 1 1 d . . . B2 B 0.19043(16) 0.7898(6) 0.3127(3) 0.0383(13) Uani 1 1 d . . . F1 F 0.02536(10) 0.6737(3) -0.19122(15) 0.0489(8) Uani 1 1 d . . . F2 F 0.01003(9) 0.7676(3) -0.09520(15) 0.0382(7) Uani 1 1 d . . . F3 F 0.20793(9) 0.6873(4) 0.29079(17) 0.0542(9) Uani 1 1 d . . . F4 F 0.20379(9) 0.8272(3) 0.37529(16) 0.0485(8) Uani 1 1 d . . . O1 O 0.04662(10) 0.5900(3) -0.09191(17) 0.0369(8) Uani 1 1 d . . . O2 O 0.06881(12) 0.7888(4) -0.13368(19) 0.0484(10) Uani 1 1 d . . . O3 O 0.15113(10) 0.7637(3) 0.31897(18) 0.0370(8) Uani 1 1 d . . . O4 O 0.19587(10) 0.8945(4) 0.26793(19) 0.0437(9) Uani 1 1 d . . . Cl1 Cl 0.0000 0.7748(2) 0.2500 0.0501(5) Uani 1 2 d S . . O5 O 0.0029(2) 0.7034(7) 0.1892(4) 0.121(3) Uani 1 1 d . . . O6 O 0.0305(3) 0.8399(13) 0.2613(4) 0.194(6) Uani 1 1 d . . . Cl2 Cl 0.12505(7) 0.24335(19) 0.06486(16) 0.0934(8) Uani 1 1 d . . . O7 O 0.1639(7) 0.218(2) 0.1001(13) 0.155(8) Uiso 0.50 1 d P . . O8 O 0.1253(3) 0.3713(11) 0.0610(6) 0.074(3) Uiso 0.50 1 d P . . O9 O 0.1203(4) 0.2173(13) -0.0133(8) 0.100(4) Uiso 0.50 1 d P . . O10 O 0.1126(4) 0.3462(14) 0.0898(8) 0.098(4) Uiso 0.50 1 d P . . O7A O 0.1484(4) 0.1847(12) 0.1182(7) 0.079(3) Uiso 0.50 1 d P . . O8A O 0.0862(8) 0.212(2) 0.0833(14) 0.189(10) Uiso 0.50 1 d P . . O9A O 0.1578(6) 0.2669(19) 0.0273(11) 0.151(7) Uiso 0.50 1 d P . . O10A O 0.1054(3) 0.1486(12) 0.0511(6) 0.083(3) Uiso 0.50 1 d P . . Cl3 Cl 0.2500 0.7500 0.0000 0.347(9) Uani 1 2 d S . . O11 O 0.2851(5) 0.7624(17) -0.0019(9) 0.265(8) Uiso 1 1 d . . . O12 O 0.2508(5) 0.6174(18) 0.0373(9) 0.133(6) Uiso 0.50 1 d P . . O12A O 0.2504(5) 0.8188(18) 0.0698(10) 0.134(6) Uiso 0.50 1 d P . . N80 N 0.3506(6) 0.869(2) 0.2202(11) 0.120(7) Uiso 0.50 1 d P A . C80 C 0.3104(9) 0.769(3) 0.1893(16) 0.130(9) Uiso 0.50 1 d P . . C81 C 0.3301(7) 0.819(2) 0.2089(12) 0.100(6) Uiso 0.50 1 d P A . O20 O 0.2500 1.2500 0.0000 0.174(12) Uiso 0.50 2 d SP . . O21 O 0.2787(7) 0.709(2) 0.1678(12) 0.175(9) Uiso 0.50 1 d P A 1 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 Co1 0.0305(3) 0.0198(3) 0.0309(3) 0.0003(2) 0.0082(2) -0.0025(2) Co2 0.0225(3) 0.0205(3) 0.0351(3) -0.0022(2) 0.0074(2) 0.0014(2) N1 0.033(2) 0.0216(18) 0.034(2) -0.0031(15) 0.0035(16) -0.0003(15) N2 0.0291(19) 0.0174(16) 0.0332(19) 0.0017(14) 0.0071(15) 0.0007(14) N3 0.0254(18) 0.0214(17) 0.034(2) 0.0043(15) 0.0033(15) 0.0025(14) N4 0.029(2) 0.029(2) 0.033(2) 0.0003(16) 0.0005(16) 0.0054(16) N5 0.026(2) 0.032(2) 0.044(2) -0.0072(18) 0.0047(17) 0.0004(16) N6 0.0248(18) 0.0219(17) 0.038(2) -0.0018(15) 0.0096(16) -0.0014(14) N7 0.036(2) 0.0202(17) 0.036(2) -0.0007(15) 0.0112(17) -0.0018(15) N8 0.047(3) 0.037(2) 0.031(2) 0.0012(18) 0.0087(18) -0.011(2) N9 0.037(2) 0.034(2) 0.042(2) -0.0064(18) 0.0120(19) 0.0001(18) N10 0.034(2) 0.035(2) 0.044(2) -0.0070(19) 0.0062(18) 0.0082(18) N11 0.0283(19) 0.0251(18) 0.0318(19) -0.0048(15) 0.0053(15) 0.0020(15) N12 0.042(2) 0.0219(18) 0.030(2) 0.0006(15) 0.0039(17) 0.0002(17) C1 0.027(2) 0.021(2) 0.047(3) -0.0020(19) 0.006(2) 0.0010(17) C2 0.027(2) 0.020(2) 0.039(2) 0.0015(18) -0.0006(19) 0.0019(17) C3 0.034(3) 0.025(2) 0.052(3) 0.011(2) 0.001(2) -0.0058(19) C4 0.036(3) 0.031(2) 0.045(3) 0.016(2) 0.003(2) -0.006(2) C5 0.028(2) 0.030(2) 0.039(3) 0.009(2) 0.0040(19) 0.0041(18) C6 0.032(2) 0.033(2) 0.039(3) 0.007(2) 0.007(2) 0.004(2) C7 0.050(3) 0.065(4) 0.042(3) 0.018(3) 0.004(3) -0.010(3) C8 0.030(2) 0.036(3) 0.053(3) -0.009(2) 0.010(2) -0.004(2) C9 0.030(2) 0.026(2) 0.051(3) -0.007(2) 0.018(2) -0.0047(18) C10 0.041(3) 0.034(3) 0.055(3) -0.008(2) 0.022(2) -0.015(2) C11 0.052(3) 0.033(3) 0.050(3) 0.001(2) 0.019(3) -0.014(2) C12 0.049(3) 0.030(2) 0.040(3) 0.003(2) 0.014(2) -0.010(2) C13 0.064(4) 0.047(3) 0.040(3) 0.010(2) 0.010(3) -0.021(3) C14 0.105(7) 0.095(6) 0.062(5) 0.036(4) -0.004(4) -0.053(5) C15 0.044(3) 0.036(3) 0.043(3) -0.005(2) 0.011(2) -0.007(2) C16 0.060(4) 0.056(4) 0.083(5) -0.019(4) 0.020(4) 0.008(3) C17 0.050(3) 0.020(2) 0.032(2) -0.0001(18) 0.005(2) 0.002(2) C18 0.057(4) 0.031(3) 0.059(4) 0.006(2) 0.021(3) 0.013(2) C19 0.041(3) 0.029(2) 0.031(2) -0.0026(19) 0.002(2) 0.006(2) C20 0.096(6) 0.073(5) 0.068(5) -0.015(4) -0.006(4) 0.059(5) C21 0.048(3) 0.054(4) 0.051(3) -0.013(3) -0.001(3) 0.019(3) C55 0.039(3) 0.024(2) 0.056(3) -0.005(2) 0.006(2) -0.006(2) C56 0.045(3) 0.065(4) 0.067(4) -0.007(3) 0.009(3) -0.023(3) C57 0.108(8) 0.112(8) 0.138(9) -0.054(7) -0.030(7) 0.082(7) B1 0.051(4) 0.033(3) 0.031(3) 0.002(2) 0.002(2) -0.006(3) B2 0.029(3) 0.044(3) 0.041(3) -0.007(3) 0.002(2) 0.009(2) F1 0.067(2) 0.0479(19) 0.0315(16) -0.0008(14) -0.0009(14) -0.0058(17) F2 0.0481(18) 0.0305(14) 0.0354(15) 0.0028(12) -0.0003(13) 0.0027(13) F3 0.0477(19) 0.064(2) 0.0496(19) -0.0118(17) -0.0038(15) 0.0312(17) F4 0.0357(17) 0.064(2) 0.0447(18) -0.0125(16) -0.0017(14) 0.0043(15) O1 0.048(2) 0.0280(17) 0.0342(18) -0.0071(14) 0.0009(15) 0.0028(15) O2 0.060(3) 0.056(2) 0.0297(18) 0.0066(17) 0.0006(17) -0.022(2) O3 0.0327(18) 0.040(2) 0.0381(19) -0.0030(15) 0.0015(15) 0.0021(15) O4 0.0342(19) 0.051(2) 0.046(2) -0.0117(18) 0.0012(16) -0.0103(17) Cl1 0.0423(11) 0.0548(12) 0.0541(12) 0.000 0.0087(9) 0.000 O5 0.176(8) 0.104(5) 0.082(4) -0.023(4) -0.004(5) 0.071(5) O6 0.145(7) 0.328(15) 0.111(6) 0.000(8) 0.027(5) -0.169(9) Cl2 0.0911(16) 0.0453(10) 0.149(2) 0.0168(12) 0.0468(16) 0.0162(10) Cl3 0.213(7) 0.075(3) 0.80(3) -0.151(7) 0.318(13) -0.035(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 Co1 N1 1.909(4) . ? Co1 N8 1.919(4) . ? Co1 N7 1.971(4) . ? Co1 N2 1.972(4) . ? Co1 N9 2.179(4) . ? Co1 N12 2.209(4) . ? Co2 N4 1.914(4) . ? Co2 N5 1.924(4) . ? Co2 N3 1.974(4) . ? Co2 N6 1.974(4) . ? Co2 N11 2.170(4) . ? Co2 N10 2.176(4) . ? N1 C1 1.286(6) . ? N1 O1 1.366(5) . ? N2 N3 1.330(5) . ? N2 C2 1.343(6) . ? N3 C5 1.347(6) . ? N4 C6 1.284(6) . ? N4 O3 1.371(5) . ? N5 C8 1.279(7) . ? N5 O4 1.376(6) . ? N6 N7 1.329(6) . ? N6 C9 1.352(6) . ? N7 C12 1.348(6) . ? N8 C13 1.285(7) . ? N8 O2 1.370(6) . ? N9 C15 1.129(7) . ? N10 C21 1.113(7) . ? N11 C19 1.130(6) . ? N12 C17 1.149(6) . ? C1 C2 1.476(7) . ? C1 C55 1.495(6) . ? C2 C3 1.398(7) . ? C3 C4 1.358(8) . ? C4 C5 1.404(7) . ? C5 C6 1.459(7) . ? C6 C7 1.490(7) . ? C8 C9 1.462(8) . ? C8 C56 1.491(7) . ? C9 C10 1.398(7) . ? C10 C11 1.346(9) . ? C11 C12 1.393(7) . ? C12 C13 1.452(8) . ? C13 C14 1.489(8) . ? C15 C16 1.463(8) . ? C17 C18 1.457(8) . ? C19 C20 1.462(8) . ? C21 C57 1.462(9) . ? B1 F2 1.377(7) . ? B1 F1 1.381(7) . ? B1 O1 1.487(7) . ? B1 O2 1.489(7) . ? B2 F4 1.377(7) . ? B2 F3 1.379(7) . ? B2 O4 1.479(8) . ? B2 O3 1.482(7) . ? Cl1 O6 1.329(7) 2 ? Cl1 O6 1.329(7) . ? Cl1 O5 1.460(7) 2 ? Cl1 O5 1.460(7) . ? Cl2 O10A 1.279(13) . ? Cl2 O10 1.325(15) . ? Cl2 O8 1.401(12) . ? Cl2 O7A 1.470(13) . ? Cl2 O9A 1.49(2) . ? Cl2 O8A 1.54(3) . ? Cl2 O7 1.57(2) . ? Cl2 O9 1.593(15) . ? O7 O7A 0.79(2) . ? O7 O9A 1.56(3) . ? O8 O10 0.817(16) . ? O8 O9A 1.82(2) . ? O9 O10A 1.623(19) . ? O9 O9A 1.64(2) . ? O10 O8A 1.76(3) . ? O8A O10A 1.21(3) . ? Cl3 O11 1.30(2) 7_565 ? Cl3 O11 1.30(2) . ? Cl3 O12A 1.59(2) . ? Cl3 O12A 1.59(2) 7_565 ? Cl3 O12 1.632(19) . ? Cl3 O12 1.63(2) 7_565 ? N80 C81 0.94(3) . ? N80 C80 1.90(4) . ? C80 C81 0.96(3) . ? C80 O21 1.38(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 N1 Co1 N8 93.94(18) . . ? N1 Co1 N7 171.19(17) . . ? N8 Co1 N7 80.92(18) . . ? N1 Co1 N2 80.84(16) . . ? N8 Co1 N2 174.27(18) . . ? N7 Co1 N2 104.55(16) . . ? N1 Co1 N9 86.48(17) . . ? N8 Co1 N9 90.58(19) . . ? N7 Co1 N9 86.43(16) . . ? N2 Co1 N9 91.45(16) . . ? N1 Co1 N12 92.62(16) . . ? N8 Co1 N12 93.13(18) . . ? N7 Co1 N12 94.79(15) . . ? N2 Co1 N12 84.79(15) . . ? N9 Co1 N12 176.23(16) . . ? N4 Co2 N5 94.26(18) . . ? N4 Co2 N3 80.76(17) . . ? N5 Co2 N3 173.73(17) . . ? N4 Co2 N6 174.35(17) . . ? N5 Co2 N6 80.99(17) . . ? N3 Co2 N6 104.18(16) . . ? N4 Co2 N11 90.77(16) . . ? N5 Co2 N11 91.69(16) . . ? N3 Co2 N11 92.17(15) . . ? N6 Co2 N11 86.35(15) . . ? N4 Co2 N10 93.43(17) . . ? N5 Co2 N10 91.65(17) . . ? N3 Co2 N10 84.89(16) . . ? N6 Co2 N10 89.78(16) . . ? N11 Co2 N10 174.43(16) . . ? C1 N1 O1 115.7(4) . . ? C1 N1 Co1 118.1(3) . . ? O1 N1 Co1 123.9(3) . . ? N3 N2 C2 119.7(4) . . ? N3 N2 Co1 126.8(3) . . ? C2 N2 Co1 113.2(3) . . ? N2 N3 C5 120.1(4) . . ? N2 N3 Co2 126.7(3) . . ? C5 N3 Co2 112.7(3) . . ? C6 N4 O3 116.2(4) . . ? C6 N4 Co2 118.6(3) . . ? O3 N4 Co2 124.5(3) . . ? C8 N5 O4 115.8(4) . . ? C8 N5 Co2 118.4(4) . . ? O4 N5 Co2 125.7(3) . . ? N7 N6 C9 119.5(4) . . ? N7 N6 Co2 127.7(3) . . ? C9 N6 Co2 112.7(3) . . ? N6 N7 C12 120.1(4) . . ? N6 N7 Co1 126.8(3) . . ? C12 N7 Co1 112.6(3) . . ? C13 N8 O2 114.2(4) . . ? C13 N8 Co1 118.0(4) . . ? O2 N8 Co1 127.6(3) . . ? C15 N9 Co1 176.9(5) . . ? C21 N10 Co2 174.0(5) . . ? C19 N11 Co2 175.8(4) . . ? C17 N12 Co1 162.9(4) . . ? N1 C1 C2 111.9(4) . . ? N1 C1 C55 124.7(5) . . ? C2 C1 C55 123.4(4) . . ? N2 C2 C3 122.1(4) . . ? N2 C2 C1 113.8(4) . . ? C3 C2 C1 124.0(4) . . ? C4 C3 C2 118.3(4) . . ? C3 C4 C5 117.7(5) . . ? N3 C5 C4 121.9(5) . . ? N3 C5 C6 114.7(4) . . ? C4 C5 C6 123.3(5) . . ? N4 C6 C5 112.4(4) . . ? N4 C6 C7 126.0(5) . . ? C5 C6 C7 121.6(5) . . ? N5 C8 C9 113.1(4) . . ? N5 C8 C56 126.3(5) . . ? C9 C8 C56 120.6(5) . . ? N6 C9 C10 121.8(5) . . ? N6 C9 C8 114.8(4) . . ? C10 C9 C8 123.4(5) . . ? C11 C10 C9 118.4(5) . . ? C10 C11 C12 118.3(5) . . ? N7 C12 C11 121.9(5) . . ? N7 C12 C13 114.6(4) . . ? C11 C12 C13 123.5(5) . . ? N8 C13 C12 113.2(5) . . ? N8 C13 C14 123.6(6) . . ? C12 C13 C14 123.1(5) . . ? N9 C15 C16 179.6(7) . . ? N12 C17 C18 178.2(6) . . ? N11 C19 C20 178.9(6) . . ? N10 C21 C57 178.8(9) . . ? F2 B1 F1 112.3(5) . . ? F2 B1 O1 110.7(4) . . ? F1 B1 O1 105.2(4) . . ? F2 B1 O2 110.1(5) . . ? F1 B1 O2 105.0(4) . . ? O1 B1 O2 113.4(5) . . ? F4 B2 F3 113.0(5) . . ? F4 B2 O4 105.7(5) . . ? F3 B2 O4 110.4(5) . . ? F4 B2 O3 105.3(4) . . ? F3 B2 O3 110.3(5) . . ? O4 B2 O3 112.0(4) . . ? N1 O1 B1 113.3(4) . . ? N8 O2 B1 116.3(4) . . ? N4 O3 B2 114.0(4) . . ? N5 O4 B2 115.9(4) . . ? O6 Cl1 O6 115.3(13) 2 . ? O6 Cl1 O5 108.6(6) 2 2 ? O6 Cl1 O5 104.7(5) . 2 ? O6 Cl1 O5 104.7(5) 2 . ? O6 Cl1 O5 108.6(6) . . ? O5 Cl1 O5 115.3(7) 2 . ? O10A Cl2 O10 124.4(9) . . ? O10A Cl2 O8 143.4(8) . . ? O10 Cl2 O8 34.7(7) . . ? O10A Cl2 O7A 95.4(8) . . ? O10 Cl2 O7A 107.1(9) . . ? O8 Cl2 O7A 118.0(7) . . ? O10A Cl2 O9A 119.5(10) . . ? O10 Cl2 O9A 111.0(11) . . ? O8 Cl2 O9A 77.8(10) . . ? O7A Cl2 O9A 89.7(10) . . ? O10A Cl2 O8A 49.7(10) . . ? O10 Cl2 O8A 75.5(12) . . ? O8 Cl2 O8A 104.5(12) . . ? O7A Cl2 O8A 103.1(12) . . ? O9A Cl2 O8A 163.4(13) . . ? O10A Cl2 O7 115.7(10) . . ? O10 Cl2 O7 107.7(11) . . ? O8 Cl2 O7 100.9(10) . . ? O7A Cl2 O7 29.8(9) . . ? O9A Cl2 O7 61.2(11) . . ? O8A Cl2 O7 132.7(14) . . ? O10A Cl2 O9 67.8(8) . . ? O10 Cl2 O9 120.6(9) . . ? O8 Cl2 O9 97.2(7) . . ? O7A Cl2 O9 131.0(8) . . ? O9A Cl2 O9 64.2(10) . . ? O8A Cl2 O9 99.3(11) . . ? O7 Cl2 O9 116.3(11) . . ? O7A O7 O9A 122(3) . . ? O7A O7 Cl2 68(2) . . ? O9A O7 Cl2 56.8(12) . . ? O10 O8 Cl2 67.6(15) . . ? O10 O8 O9A 118.5(18) . . ? Cl2 O8 O9A 53.2(8) . . ? Cl2 O9 O10A 46.9(6) . . ? Cl2 O9 O9A 54.7(9) . . ? O10A O9 O9A 94.3(12) . . ? O8 O10 Cl2 77.7(15) . . ? O8 O10 O8A 125(2) . . ? Cl2 O10 O8A 57.7(11) . . ? O7 O7A Cl2 82(2) . . ? O10A O8A Cl2 54.0(13) . . ? O10A O8A O10 100.3(19) . . ? Cl2 O8A O10 46.8(9) . . ? Cl2 O9A O7 62.0(12) . . ? Cl2 O9A O9 61.1(10) . . ? O7 O9A O9 114.4(17) . . ? Cl2 O9A O8 49.0(8) . . ? O7 O9A O8 85.3(14) . . ? O9 O9A O8 81.1(11) . . ? O8A O10A Cl2 76.2(15) . . ? O8A O10A O9 114.0(17) . . ? Cl2 O10A O9 65.3(8) . . ? O11 Cl3 O11 180.0(17) 7_565 . ? O11 Cl3 O12A 88.3(10) 7_565 . ? O11 Cl3 O12A 91.7(10) . . ? O11 Cl3 O12A 91.7(10) 7_565 7_565 ? O11 Cl3 O12A 88.3(10) . 7_565 ? O12A Cl3 O12A 180.0(7) . 7_565 ? O11 Cl3 O12 83.0(10) 7_565 . ? O11 Cl3 O12 97.0(10) . . ? O12A Cl3 O12 90.9(9) . . ? O12A Cl3 O12 89.1(9) 7_565 . ? O11 Cl3 O12 97.0(10) 7_565 7_565 ? O11 Cl3 O12 83.0(10) . 7_565 ? O12A Cl3 O12 89.1(9) . 7_565 ? O12A Cl3 O12 90.9(9) 7_565 7_565 ? O12 Cl3 O12 180.0(11) . 7_565 ? C81 N80 C80 5(2) . . ? C81 C80 O21 171(4) . . ? C81 C80 N80 5(2) . . ? O21 C80 N80 174(3) . . ? N80 C81 C80 170(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.004 _refine_diff_density_min -1.858 _refine_diff_density_rms 0.140 #===END data_nks3-55d _database_code_depnum_ccdc_archive 'CCDC 740051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 B4 Co2 F12 N12 O4' _chemical_formula_weight 911.65 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 15.033(3) _cell_length_b 20.805(4) _cell_length_c 11.395(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3564.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9000 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 28.5 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32921 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 29.57 _reflns_number_total 5000 _reflns_number_gt 3485 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0821P)^2^+3.2671P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5000 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Co1 Co 0.11626(2) 0.509362(19) 0.56005(3) 0.02562(13) Uani 1 1 d . . . C1 C 0.1215(2) 0.61646(16) 0.7008(3) 0.0393(7) Uani 1 1 d . . . H1 H 0.1420 0.6477 0.7525 0.047 Uiso 1 1 calc R . . C2 C 0.2175(2) 0.40757(15) 0.4860(3) 0.0338(6) Uani 1 1 d . . . H2 H 0.2652 0.3794 0.4785 0.041 Uiso 1 1 calc R . . C3 C -0.0316(2) 0.66211(17) 0.6867(4) 0.0509(9) Uani 1 1 d . . . H3 H -0.0173 0.6957 0.7372 0.061 Uiso 1 1 calc R . . C4 C 0.1143(2) 0.34289(16) 0.3613(3) 0.0442(8) Uani 1 1 d . . . H4 H 0.1577 0.3120 0.3469 0.053 Uiso 1 1 calc R . . C5 C 0.0308(2) 0.61526(15) 0.6577(3) 0.0369(7) Uani 1 1 d . . . C6 C 0.13152(19) 0.39560(15) 0.4326(3) 0.0326(6) Uani 1 1 d . . . C7 C 0.1727(2) 0.60722(16) 0.3500(3) 0.0390(7) Uani 1 1 d . . . C8 C 0.04560(19) 0.42610(15) 0.7854(3) 0.0343(6) Uani 1 1 d . . . C9 C 0.2101(4) 0.6588(2) 0.2781(4) 0.0806(17) Uani 1 1 d . . . H9A H 0.1674 0.6929 0.2708 0.121 Uiso 1 1 calc R . . H9B H 0.2244 0.6424 0.2016 0.121 Uiso 1 1 calc R . . H9C H 0.2631 0.6750 0.3146 0.121 Uiso 1 1 calc R . . C10 C 0.0030(2) 0.38899(19) 0.8785(3) 0.0451(8) Uani 1 1 d . . . H10A H -0.0566 0.4043 0.8899 0.068 Uiso 1 1 calc R . . H10B H 0.0361 0.3939 0.9500 0.068 Uiso 1 1 calc R . . H10C H 0.0015 0.3444 0.8567 0.068 Uiso 1 1 calc R . . N1 N 0.17130(16) 0.57093(12) 0.6619(2) 0.0324(5) Uani 1 1 d . . . N2 N 0.01212(15) 0.56526(11) 0.5864(2) 0.0269(5) Uani 1 1 d . . . N3 N 0.06940(15) 0.44041(11) 0.4574(2) 0.0265(5) Uani 1 1 d . . . N4 N 0.22265(15) 0.45985(13) 0.5441(2) 0.0310(5) Uani 1 1 d . . . N5 N 0.14551(18) 0.56824(13) 0.4079(2) 0.0345(5) Uani 1 1 d . . . N6 N 0.07767(16) 0.45393(12) 0.7115(2) 0.0326(5) Uani 1 1 d . . . O1 O 0.30153(14) 0.47083(12) 0.5992(2) 0.0396(5) Uani 1 1 d . . . O2 O 0.25505(14) 0.56880(11) 0.70580(19) 0.0400(5) Uani 1 1 d . . . B1 B 0.3211(2) 0.5390(2) 0.6253(3) 0.0418(8) Uani 1 1 d . . . F1 F 0.32455(13) 0.57444(11) 0.52273(19) 0.0515(5) Uani 1 1 d . . . F2 F 0.40056(12) 0.53880(12) 0.68409(19) 0.0527(5) Uani 1 1 d . . . B2 B 0.4287(5) 0.7500 0.1555(6) 0.0573(16) Uani 1 2 d S . . F3 F 0.3981(3) 0.7500 0.2685(4) 0.0921(13) Uani 1 2 d S . . F4 F 0.4697(5) 0.6942(2) 0.1220(4) 0.1101(18) Uani 0.75 1 d P . . F4A F 0.3877(14) 0.7118(11) 0.0906(19) 0.129(6) Uiso 0.25 1 d P . . F5 F 0.3588(13) 0.7500 0.0694(13) 0.049(4) Uani 0.25 2 d SP . . F5A F 0.5267(15) 0.7500 0.206(2) 0.184(16) Uani 0.25 2 d SP . . F5B F 0.3401(17) 0.7298(12) 0.096(2) 0.052(7) Uiso 0.13 1 d P . . F5C F 0.5046(13) 0.7171(11) 0.1587(17) 0.043(4) Uiso 0.13 1 d P . . B3 B 0.1279(3) 0.7500 0.9422(4) 0.0347(10) Uani 1 2 d S . . F6 F 0.2005(2) 0.7500 0.8625(3) 0.0653(9) Uani 1 2 d S . . F7 F 0.1180(3) 0.6863(2) 0.9617(4) 0.0504(10) Uani 0.50 1 d P . . F8 F 0.1428(4) 0.7163(3) 1.0416(5) 0.0831(19) Uani 0.50 1 d P . . F9 F 0.0512(3) 0.7280(2) 0.8885(4) 0.0625(14) Uani 0.50 1 d P . . N13 N 0.1658(6) 0.7500 0.5759(6) 0.090(2) Uani 1 2 d S . . C13 C 0.2439(5) 0.7500 0.5633(5) 0.0634(16) Uani 1 2 d S . . C14 C 0.3359(5) 0.7500 0.5481(7) 0.081(2) Uani 1 2 d S . . H14A H 0.3589 0.7921 0.5646 0.122 Uiso 0.50 1 calc PR . . H14B H 0.3498 0.7385 0.4687 0.122 Uiso 0.50 1 calc PR . . H14C H 0.3623 0.7194 0.6008 0.122 Uiso 0.50 1 calc PR . . 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 Co1 0.0276(2) 0.0218(2) 0.0275(2) 0.00068(14) 0.00299(14) 0.00141(14) C1 0.0388(16) 0.0311(18) 0.0480(18) -0.0114(14) -0.0003(13) -0.0031(12) C2 0.0317(14) 0.0303(17) 0.0395(15) 0.0010(12) 0.0019(11) 0.0091(12) C3 0.0425(17) 0.0293(19) 0.081(3) -0.0199(17) 0.0030(17) 0.0018(14) C4 0.0405(17) 0.0253(18) 0.067(2) -0.0106(15) 0.0072(15) 0.0054(13) C5 0.0384(15) 0.0264(17) 0.0458(17) -0.0074(13) 0.0045(13) -0.0016(12) C6 0.0341(15) 0.0236(16) 0.0402(16) 0.0025(12) 0.0063(12) 0.0045(11) C7 0.0491(18) 0.0342(18) 0.0337(15) 0.0020(13) -0.0046(13) -0.0089(14) C8 0.0321(14) 0.0357(18) 0.0351(15) -0.0003(12) 0.0016(11) 0.0046(12) C9 0.148(5) 0.052(3) 0.043(2) 0.0104(19) 0.000(3) -0.046(3) C10 0.0393(17) 0.052(2) 0.0439(18) 0.0105(15) 0.0045(14) -0.0049(15) N1 0.0312(12) 0.0300(14) 0.0361(13) -0.0019(10) 0.0002(9) -0.0024(10) N2 0.0290(11) 0.0188(12) 0.0329(12) 0.0008(9) 0.0042(9) -0.0003(9) N3 0.0311(11) 0.0165(12) 0.0317(11) 0.0019(8) 0.0038(9) 0.0017(9) N4 0.0273(11) 0.0321(15) 0.0335(12) 0.0025(10) 0.0019(9) 0.0040(10) N5 0.0382(13) 0.0285(14) 0.0368(13) 0.0042(10) 0.0033(11) 0.0015(11) N6 0.0340(12) 0.0304(14) 0.0333(12) 0.0036(10) 0.0048(10) 0.0045(10) O1 0.0306(10) 0.0432(14) 0.0449(12) -0.0033(10) -0.0053(9) 0.0057(9) O2 0.0323(10) 0.0480(14) 0.0396(12) -0.0073(10) -0.0056(9) 0.0010(9) B1 0.0334(17) 0.051(2) 0.0408(19) -0.0007(17) 0.0000(14) 0.0001(16) F1 0.0401(11) 0.0622(15) 0.0522(12) 0.0083(10) 0.0020(9) -0.0079(9) F2 0.0368(10) 0.0657(15) 0.0556(12) -0.0084(11) -0.0073(9) 0.0013(9) B2 0.076(5) 0.044(4) 0.052(4) 0.000 -0.016(3) 0.000 F3 0.100(3) 0.114(4) 0.063(2) 0.000 0.000(2) 0.000 F4 0.198(6) 0.048(3) 0.085(3) -0.013(2) -0.017(3) 0.029(3) F5 0.048(8) 0.079(13) 0.019(6) 0.000 -0.013(6) 0.000 F5A 0.075(14) 0.38(5) 0.092(17) 0.000 -0.031(12) 0.000 B3 0.043(3) 0.028(3) 0.033(2) 0.000 -0.005(2) 0.000 F6 0.0512(18) 0.090(3) 0.0543(19) 0.000 0.0070(14) 0.000 F7 0.058(3) 0.022(2) 0.072(3) 0.0091(19) 0.014(2) 0.0044(17) F8 0.071(3) 0.100(5) 0.078(4) 0.061(3) -0.020(3) -0.013(3) F9 0.056(2) 0.065(4) 0.066(3) -0.016(2) -0.018(2) -0.0128(19) N13 0.115(6) 0.075(5) 0.080(4) 0.000 0.013(4) 0.000 C13 0.076(4) 0.063(4) 0.052(3) 0.000 0.007(3) 0.000 C14 0.079(5) 0.085(6) 0.080(5) 0.000 -0.024(4) 0.000 _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 Co1 N4 1.911(2) . ? Co1 N1 1.917(2) . ? Co1 N2 1.973(2) . ? Co1 N3 1.980(2) . ? Co1 N6 2.155(2) . ? Co1 N5 2.168(3) . ? C1 N1 1.286(4) . ? C1 C5 1.449(4) . ? C2 N4 1.276(4) . ? C2 C6 1.451(4) . ? C3 C4 1.361(5) 5_566 ? C3 C5 1.393(4) . ? C4 C3 1.361(5) 5_566 ? C4 C6 1.389(5) . ? C5 N2 1.349(4) . ? C6 N3 1.350(4) . ? C7 N5 1.122(4) . ? C7 C9 1.464(5) . ? C8 N6 1.130(4) . ? C8 C10 1.460(4) . ? N1 O2 1.355(3) . ? N2 N3 1.329(3) 5_566 ? N3 N2 1.329(3) 5_566 ? N4 O1 1.361(3) . ? O1 B1 1.478(5) . ? O2 B1 1.488(4) . ? B1 F2 1.370(4) . ? B1 F1 1.383(5) . ? B2 F4A 1.25(2) 7_575 ? B2 F4A 1.25(2) . ? B2 F5C 1.33(2) 7_575 ? B2 F5C 1.33(2) . ? B2 F3 1.368(8) . ? B2 F4 1.369(6) 7_575 ? B2 F4 1.369(6) . ? B2 F5 1.437(15) . ? B2 F5B 1.55(3) 7_575 ? B2 F5B 1.55(3) . ? B2 F5A 1.58(2) . ? F4 F5C 0.82(2) . ? F4 F4A 1.33(2) . ? F4 F5A 1.731(16) . ? F4A F5B 0.81(3) . ? F4A F5 0.94(2) . ? F4A F5B 1.41(3) 7_575 ? F4A F4A 1.59(5) 7_575 ? F5 F5B 0.59(2) 7_575 ? F5 F5B 0.59(2) . ? F5 F4A 0.94(2) 7_575 ? F5A F5C 0.93(2) . ? F5A F5C 0.93(2) 7_575 ? F5A F4 1.731(16) 7_575 ? F5B F5B 0.84(5) 7_575 ? F5B F4A 1.41(3) 7_575 ? F5C F5C 1.37(4) 7_575 ? B3 F8 1.350(6) 7_575 ? B3 F8 1.350(6) . ? B3 F7 1.351(4) 7_575 ? B3 F7 1.351(4) . ? B3 F9 1.384(6) 7_575 ? B3 F9 1.384(6) . ? B3 F6 1.420(6) . ? F7 F8 1.165(7) . ? F7 F9 1.566(6) . ? F8 F8 1.401(14) 7_575 ? F9 F9 0.917(9) 7_575 ? N13 C13 1.183(10) . ? C13 C14 1.394(11) . ? 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 N4 Co1 N1 93.24(11) . . ? N4 Co1 N2 174.96(10) . . ? N1 Co1 N2 81.74(10) . . ? N4 Co1 N3 81.44(10) . . ? N1 Co1 N3 174.52(10) . . ? N2 Co1 N3 103.57(10) . . ? N4 Co1 N6 90.74(10) . . ? N1 Co1 N6 89.36(10) . . ? N2 Co1 N6 88.84(9) . . ? N3 Co1 N6 89.39(10) . . ? N4 Co1 N5 93.37(10) . . ? N1 Co1 N5 91.11(11) . . ? N2 Co1 N5 87.12(10) . . ? N3 Co1 N5 90.53(10) . . ? N6 Co1 N5 175.83(10) . . ? N1 C1 C5 114.8(3) . . ? N4 C2 C6 114.7(3) . . ? C4 C3 C5 117.8(3) 5_566 . ? C3 C4 C6 117.8(3) 5_566 . ? N2 C5 C3 122.8(3) . . ? N2 C5 C1 114.4(3) . . ? C3 C5 C1 122.8(3) . . ? N3 C6 C4 122.6(3) . . ? N3 C6 C2 114.2(3) . . ? C4 C6 C2 123.2(3) . . ? N5 C7 C9 178.0(4) . . ? N6 C8 C10 178.4(4) . . ? C1 N1 O2 116.0(3) . . ? C1 N1 Co1 116.7(2) . . ? O2 N1 Co1 127.05(19) . . ? N3 N2 C5 119.1(2) 5_566 . ? N3 N2 Co1 128.47(18) 5_566 . ? C5 N2 Co1 112.41(19) . . ? N2 N3 C6 119.9(2) 5_566 . ? N2 N3 Co1 127.92(18) 5_566 . ? C6 N3 Co1 112.2(2) . . ? C2 N4 O1 115.8(2) . . ? C2 N4 Co1 117.3(2) . . ? O1 N4 Co1 126.50(19) . . ? C7 N5 Co1 162.2(3) . . ? C8 N6 Co1 170.3(2) . . ? N4 O1 B1 115.3(2) . . ? N1 O2 B1 114.0(2) . . ? F2 B1 F1 112.5(3) . . ? F2 B1 O1 105.6(3) . . ? F1 B1 O1 110.5(3) . . ? F2 B1 O2 106.3(3) . . ? F1 B1 O2 108.9(3) . . ? O1 B1 O2 113.0(3) . . ? F4A B2 F4A 79(2) 7_575 . ? F4A B2 F5C 96.4(13) 7_575 7_575 ? F4A B2 F5C 140.0(14) . 7_575 ? F4A B2 F5C 140.0(14) 7_575 . ? F4A B2 F5C 96.4(13) . . ? F5C B2 F5C 61.8(19) 7_575 . ? F4A B2 F3 113.1(11) 7_575 . ? F4A B2 F3 113.1(11) . . ? F5C B2 F3 105.2(10) 7_575 . ? F5C B2 F3 105.2(10) . . ? F4A B2 F4 61.1(10) 7_575 7_575 ? F4A B2 F4 126.7(12) . 7_575 ? F5C B2 F4 35.5(9) 7_575 7_575 ? F5C B2 F4 93.3(11) . 7_575 ? F3 B2 F4 114.4(4) . 7_575 ? F4A B2 F4 126.7(12) 7_575 . ? F4A B2 F4 61.1(10) . . ? F5C B2 F4 93.3(11) 7_575 . ? F5C B2 F4 35.5(9) . . ? F3 B2 F4 114.4(4) . . ? F4 B2 F4 116.1(8) 7_575 . ? F4A B2 F5 40.1(11) 7_575 . ? F4A B2 F5 40.1(11) . . ? F5C B2 F5 130.2(12) 7_575 . ? F5C B2 F5 130.2(12) . . ? F3 B2 F5 113.4(10) . . ? F4 B2 F5 98.0(6) 7_575 . ? F4 B2 F5 98.0(6) . . ? F4A B2 F5B 31.3(14) 7_575 7_575 ? F4A B2 F5B 59.4(13) . 7_575 ? F5C B2 F5B 127.5(14) 7_575 7_575 ? F5C B2 F5B 152.6(13) . 7_575 ? F3 B2 F5B 97.0(10) . 7_575 ? F4 B2 F5B 92.0(11) 7_575 7_575 ? F4 B2 F5B 119.7(10) . 7_575 ? F5 B2 F5B 22.4(8) . 7_575 ? F4A B2 F5B 59.4(13) 7_575 . ? F4A B2 F5B 31.3(14) . . ? F5C B2 F5B 152.6(13) 7_575 . ? F5C B2 F5B 127.5(14) . . ? F3 B2 F5B 97.0(10) . . ? F4 B2 F5B 119.7(10) 7_575 . ? F4 B2 F5B 92.0(11) . . ? F5 B2 F5B 22.4(8) . . ? F5B B2 F5B 31(2) 7_575 . ? F4A B2 F5A 132.4(12) 7_575 . ? F4A B2 F5A 132.4(12) . . ? F5C B2 F5A 36.0(10) 7_575 . ? F5C B2 F5A 36.0(10) . . ? F3 B2 F5A 88.4(10) . . ? F4 B2 F5A 71.4(6) 7_575 . ? F4 B2 F5A 71.4(6) . . ? F5 B2 F5A 158.2(14) . . ? F5B B2 F5A 163.3(11) 7_575 . ? F5B B2 F5A 163.3(11) . . ? F5C F4 F4A 124.4(19) . . ? F5C F4 B2 69.8(15) . . ? F4A F4 B2 55.0(9) . . ? F5C F4 F5A 10.1(18) . . ? F4A F4 F5A 114.9(11) . . ? B2 F4 F5A 60.0(7) . . ? F5B F4A F5 38.7(19) . . ? F5B F4A B2 95(3) . . ? F5 F4A B2 80.9(19) . . ? F5B F4A F4 157(3) . . ? F5 F4A F4 137(3) . . ? B2 F4A F4 63.9(10) . . ? F5B F4A F5B 32(3) . 7_575 ? F5 F4A F5B 17.7(16) . 7_575 ? B2 F4A F5B 71.0(16) . 7_575 ? F4 F4A F5B 134(2) . 7_575 ? F5B F4A F4A 62(3) . 7_575 ? F5 F4A F4A 32.0(16) . 7_575 ? B2 F4A F4A 50.5(11) . 7_575 ? F4 F4A F4A 106.0(10) . 7_575 ? F5B F4A F4A 30.6(12) 7_575 7_575 ? F5B F5 F5B 91(7) 7_575 . ? F5B F5 F4A 59(3) 7_575 7_575 ? F5B F5 F4A 134(4) . 7_575 ? F5B F5 F4A 134(4) 7_575 . ? F5B F5 F4A 59(3) . . ? F4A F5 F4A 116(3) 7_575 . ? F5B F5 B2 90(3) 7_575 . ? F5B F5 B2 90(3) . . ? F4A F5 B2 59.1(15) 7_575 . ? F4A F5 B2 59.1(15) . . ? F5C F5A F5C 95(3) . 7_575 ? F5C F5A B2 57.2(18) . . ? F5C F5A B2 57.2(18) 7_575 . ? F5C F5A F4 90(2) . 7_575 ? F5C F5A F4 8.9(15) 7_575 7_575 ? B2 F5A F4 48.6(6) . 7_575 ? F5C F5A F4 8.9(15) . . ? F5C F5A F4 90(2) 7_575 . ? B2 F5A F4 48.6(6) . . ? F4 F5A F4 84.3(10) 7_575 . ? F5 F5B F4A 82(4) . . ? F5 F5B F5B 45(3) . 7_575 ? F4A F5B F5B 118(3) . 7_575 ? F5 F5B F4A 29(3) . 7_575 ? F4A F5B F4A 87(3) . 7_575 ? F5B F5B F4A 30.6(12) 7_575 7_575 ? F5 F5B B2 68(3) . . ? F4A F5B B2 53(2) . . ? F5B F5B B2 74.3(10) 7_575 . ? F4A F5B B2 49.6(12) 7_575 . ? F4 F5C F5A 161(3) . . ? F4 F5C B2 74.7(15) . . ? F5A F5C B2 87(2) . . ? F4 F5C F5C 125.4(15) . 7_575 ? F5A F5C F5C 42.7(16) . 7_575 ? B2 F5C F5C 59.1(10) . 7_575 ? F8 B3 F8 62.5(7) 7_575 . ? F8 B3 F7 51.1(3) 7_575 7_575 ? F8 B3 F7 112.9(6) . 7_575 ? F8 B3 F7 112.9(6) 7_575 . ? F8 B3 F7 51.1(3) . . ? F7 B3 F7 157.1(6) 7_575 . ? F8 B3 F9 109.7(4) 7_575 7_575 ? F8 B3 F9 132.9(5) . 7_575 ? F7 B3 F9 69.9(3) 7_575 7_575 ? F7 B3 F9 107.8(4) . 7_575 ? F8 B3 F9 132.9(5) 7_575 . ? F8 B3 F9 109.7(4) . . ? F7 B3 F9 107.8(4) 7_575 . ? F7 B3 F9 69.9(3) . . ? F9 B3 F9 38.7(4) 7_575 . ? F8 B3 F6 114.2(4) 7_575 . ? F8 B3 F6 114.2(4) . . ? F7 B3 F6 101.0(3) 7_575 . ? F7 B3 F6 101.0(3) . . ? F9 B3 F6 110.9(4) 7_575 . ? F9 B3 F6 110.9(4) . . ? F8 F7 B3 64.4(4) . . ? F8 F7 F9 109.0(4) . . ? B3 F7 F9 56.1(3) . . ? F7 F8 B3 64.5(3) . . ? F7 F8 F8 122.4(3) . 7_575 ? B3 F8 F8 58.8(3) . 7_575 ? F9 F9 B3 70.6(2) 7_575 . ? F9 F9 F7 123.5(2) 7_575 . ? B3 F9 F7 54.1(2) . . ? N13 C13 C14 179.8(7) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.878 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.098 #===END data_nks6 _database_code_depnum_ccdc_archive 'CCDC 740052' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H29 Cl3 Co2 N11 O12' _chemical_formula_weight 887.79 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' Co Co 0.3494 0.9721 '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 11.556(3) _cell_length_b 29.721(8) _cell_length_c 11.189(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.96 _cell_angle_gamma 90.00 _cell_volume 3362.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.35 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 1.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5619 _exptl_absorpt_correction_T_max 0.7806 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _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 P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53463 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5741 _reflns_number_gt 4428 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0714P)^2^+7.1897P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5741 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.005 _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 Co1 Co 0.26873(6) 0.101416(19) 0.60836(6) 0.01893(17) Uani 1 1 d . . . Co2 Co 0.04578(6) 0.14201(2) 0.24327(6) 0.02119(18) Uani 1 1 d . . . N1 N 0.1267(3) 0.17600(12) 0.4109(3) 0.0178(8) Uani 1 1 d . . . N2 N 0.2191(3) 0.16273(12) 0.5381(4) 0.0180(8) Uani 1 1 d . . . N3 N 0.3856(4) 0.13190(13) 0.7758(4) 0.0233(8) Uani 1 1 d . . . N4 N 0.2997(4) 0.04363(13) 0.6997(4) 0.0238(9) Uani 1 1 d . . . N5 N 0.1438(3) 0.06712(12) 0.4481(4) 0.0195(8) Uani 1 1 d . . . N6 N 0.0682(3) 0.08178(12) 0.3182(4) 0.0207(8) Uani 1 1 d . . . N7 N -0.0673(4) 0.11134(15) 0.0776(4) 0.0291(9) Uani 1 1 d . . . N8 N -0.0393(4) 0.19813(14) 0.1688(4) 0.0267(9) Uani 1 1 d . . . N9 N 0.2010(4) 0.14424(12) 0.2149(4) 0.0219(5) Uani 1 1 d . . . C24 C 0.7813(5) 0.17458(17) 0.3571(6) 0.0360(12) Uani 1 1 d . . . H24A H 0.7393 0.1962 0.2821 0.054 Uiso 1 1 calc R . . H24B H 0.8765 0.1805 0.4084 0.054 Uiso 1 1 calc R . . H24C H 0.7429 0.1776 0.4180 0.054 Uiso 1 1 calc R . . C1 C 0.4816(5) 0.10999(17) 0.9038(5) 0.0313(11) Uani 1 1 d . . . H1A H 0.5166 0.1323 0.9789 0.038 Uiso 1 1 calc R . . H1B H 0.5567 0.0982 0.8939 0.038 Uiso 1 1 calc R . . C2 C 0.4167(5) 0.07192(16) 0.9381(5) 0.0310(11) Uani 1 1 d . . . H2A H 0.4748 0.0624 1.0337 0.037 Uiso 1 1 calc R . . H2B H 0.3323 0.0826 0.9306 0.037 Uiso 1 1 calc R . . C3 C 0.3900(5) 0.03243(16) 0.8453(5) 0.0309(11) Uani 1 1 d . . . H3A H 0.4748 0.0213 0.8549 0.037 Uiso 1 1 calc R . . H3B H 0.3503 0.0079 0.8736 0.037 Uiso 1 1 calc R . . C4 C -0.1411(6) 0.1324(2) -0.0586(5) 0.0450(15) Uani 1 1 d . . . H4A H -0.2000 0.1098 -0.1254 0.054 Uiso 1 1 calc R . . H4B H -0.0782 0.1431 -0.0886 0.054 Uiso 1 1 calc R . . C5 C -0.2225(5) 0.1714(2) -0.0546(5) 0.0432(14) Uani 1 1 d . . . H5A H -0.2837 0.1813 -0.1491 0.052 Uiso 1 1 calc R . . H5B H -0.2762 0.1616 -0.0124 0.052 Uiso 1 1 calc R . . C6 C -0.1368(5) 0.21024(19) 0.0248(5) 0.0374(13) Uani 1 1 d . . . H6A H -0.0883 0.2214 -0.0218 0.045 Uiso 1 1 calc R . . H6B H -0.1938 0.2350 0.0258 0.045 Uiso 1 1 calc R . . C7 C 0.2294(5) 0.01227(15) 0.6203(5) 0.0262(11) Uani 1 1 d . . . H7 H 0.2334 -0.0174 0.6537 0.031 Uiso 1 1 calc R . . C8 C 0.0672(5) -0.00961(16) 0.3802(5) 0.0329(12) Uani 1 1 d . . . H8 H 0.0661 -0.0401 0.4052 0.039 Uiso 1 1 calc R . . C9 C -0.0056(5) 0.00460(17) 0.2466(5) 0.0339(12) Uani 1 1 d . . . H9 H -0.0561 -0.0161 0.1755 0.041 Uiso 1 1 calc R . . C10 C -0.0748(5) 0.06859(19) 0.0854(5) 0.0332(12) Uani 1 1 d . . . H10 H -0.1249 0.0505 0.0070 0.040 Uiso 1 1 calc R . . C11 C 0.0019(5) 0.23163(17) 0.2545(5) 0.0282(11) Uani 1 1 d . . . H11 H -0.0305 0.2613 0.2269 0.034 Uiso 1 1 calc R . . C12 C 0.1555(5) 0.25354(16) 0.4947(5) 0.0291(11) Uani 1 1 d . . . H12 H 0.1317 0.2844 0.4774 0.035 Uiso 1 1 calc R . . C13 C 0.2481(5) 0.23926(16) 0.6228(5) 0.0279(11) Uani 1 1 d . . . H13 H 0.2901 0.2597 0.6970 0.033 Uiso 1 1 calc R . . C14 C 0.3736(4) 0.17455(15) 0.7698(5) 0.0244(10) Uani 1 1 d . . . H14 H 0.4248 0.1931 0.8468 0.029 Uiso 1 1 calc R . . C15 C 0.1428(5) 0.02298(15) 0.4770(5) 0.0239(10) Uani 1 1 d . . . C16 C -0.0030(4) 0.04975(16) 0.2193(5) 0.0255(11) Uani 1 1 d . . . C17 C 0.0978(4) 0.22163(15) 0.3914(5) 0.0233(10) Uani 1 1 d . . . C18 C 0.2772(4) 0.19350(14) 0.6387(4) 0.0205(9) Uani 1 1 d . . . C19 C 0.2948(5) 0.14720(15) 0.2051(5) 0.0255(10) Uani 1 1 d . . . C21 C 0.7587(5) 0.12872(17) 0.3013(5) 0.0309(11) Uani 1 1 d . . . C23 C 0.4130(5) 0.15164(18) 0.1948(6) 0.0406(14) Uani 1 1 d . . . H23A H 0.3919 0.1658 0.1075 0.061 Uiso 1 1 calc R . . H23B H 0.4513 0.1218 0.1999 0.061 Uiso 1 1 calc R . . H23C H 0.4768 0.1704 0.2700 0.061 Uiso 1 1 calc R . . N11 N 0.7385(4) 0.09367(13) 0.2563(4) 0.0219(5) Uani 1 1 d . . . Cl1 Cl 0.31710(12) 0.01646(4) 0.20682(12) 0.0298(3) Uani 1 1 d . . . Cl2 Cl 0.54792(12) 0.23253(4) 0.56262(12) 0.0309(3) Uani 1 1 d . . . Cl3 Cl 0.04599(11) 0.13233(4) 0.73157(12) 0.0276(3) Uani 1 1 d . . . O1 O 0.2033(4) 0.03396(14) 0.0878(4) 0.0574(12) Uani 1 1 d . . . O2 O 0.3344(3) -0.03012(12) 0.1847(3) 0.0355(8) Uani 1 1 d . . . O3 O 0.4329(4) 0.04119(13) 0.2315(4) 0.0482(10) Uani 1 1 d . . . O4 O 0.2994(4) 0.02039(14) 0.3243(4) 0.0447(10) Uani 1 1 d . . . O5 O 0.6410(5) 0.20126(16) 0.5666(5) 0.0720(15) Uani 1 1 d . . . O6 O 0.5864(4) 0.27758(13) 0.5513(4) 0.0452(10) Uani 1 1 d . . . O7 O 0.5415(4) 0.23002(15) 0.6877(4) 0.0466(10) Uani 1 1 d . . . O8 O 0.4171(4) 0.22386(14) 0.4475(4) 0.0492(10) Uani 1 1 d . . . O10 O 0.1537(7) 0.1623(3) 0.8196(9) 0.038(2) Uani 0.50 1 d P . . O10A O -0.0857(7) 0.1207(3) 0.6854(8) 0.0432(19) Uani 0.50 1 d P . . O11 O 0.0495(9) 0.0950(2) 0.8260(7) 0.046(2) Uani 0.50 1 d P . . O11A O -0.0756(6) 0.1547(3) 0.6848(7) 0.0310(16) Uani 0.50 1 d P . . O12 O 0.0621(14) 0.1125(5) 0.6294(16) 0.027(3) Uani 0.50 1 d P . . O9 O 0.0998(14) 0.1009(5) 0.6684(16) 0.028(3) Uani 0.50 1 d P . . O9A O 0.1309(18) 0.1476(7) 0.8546(19) 0.026(5) Uiso 0.25 1 d P . . O12A O 0.0235(16) 0.1751(5) 0.6346(18) 0.029(4) Uiso 0.25 1 d P . . O9B O 0.0589(19) 0.1779(6) 0.685(2) 0.044(5) Uiso 0.25 1 d P . . O12B O 0.1251(16) 0.1326(7) 0.8736(18) 0.035(5) Uiso 0.25 1 d P . . N10 N 0.4081(4) 0.09475(12) 0.5619(4) 0.0219(5) Uani 1 1 d . . . C25 C 0.5084(5) 0.09089(16) 0.5505(4) 0.0306(12) Uani 1 1 d . . . C26 C 0.6290(5) 0.08492(19) 0.5361(5) 0.0353(12) Uani 1 1 d . . . H26A H 0.6853 0.0616 0.5996 0.053 Uiso 1 1 calc R . . H26B H 0.6779 0.1134 0.5569 0.053 Uiso 1 1 calc R . . H26C H 0.6031 0.0759 0.4423 0.053 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 Co1 0.0217(3) 0.0164(3) 0.0199(3) 0.0007(2) 0.0110(3) -0.0008(2) Co2 0.0189(3) 0.0294(4) 0.0173(3) 0.0009(3) 0.0104(3) 0.0009(3) N1 0.0200(18) 0.0191(19) 0.0174(19) 0.0042(15) 0.0115(16) 0.0032(15) N2 0.0194(18) 0.0172(19) 0.0212(19) -0.0008(15) 0.0128(16) -0.0015(15) N3 0.023(2) 0.025(2) 0.0188(19) 0.0007(16) 0.0075(16) -0.0044(16) N4 0.032(2) 0.022(2) 0.026(2) 0.0025(17) 0.0209(18) 0.0017(17) N5 0.0219(19) 0.020(2) 0.024(2) -0.0034(16) 0.0169(17) -0.0013(15) N6 0.0192(19) 0.024(2) 0.022(2) -0.0064(16) 0.0125(16) -0.0028(16) N7 0.022(2) 0.047(3) 0.020(2) -0.0045(19) 0.0111(17) -0.0004(19) N8 0.020(2) 0.040(3) 0.024(2) 0.0114(19) 0.0144(17) 0.0054(18) N9 0.0285(12) 0.0173(11) 0.0206(11) 0.0022(9) 0.0123(10) 0.0057(9) C24 0.041(3) 0.030(3) 0.042(3) 0.000(2) 0.023(3) -0.002(2) C1 0.029(3) 0.037(3) 0.022(2) 0.002(2) 0.008(2) 0.001(2) C2 0.037(3) 0.032(3) 0.024(3) 0.009(2) 0.015(2) 0.008(2) C3 0.039(3) 0.029(3) 0.029(3) 0.012(2) 0.020(2) 0.009(2) C4 0.040(3) 0.074(4) 0.019(3) -0.002(3) 0.013(2) -0.002(3) C5 0.028(3) 0.072(4) 0.025(3) 0.015(3) 0.010(2) 0.005(3) C6 0.024(3) 0.056(4) 0.028(3) 0.019(3) 0.010(2) 0.008(2) C7 0.039(3) 0.016(2) 0.036(3) 0.001(2) 0.028(2) 0.000(2) C8 0.042(3) 0.022(3) 0.050(3) -0.010(2) 0.034(3) -0.006(2) C9 0.031(3) 0.032(3) 0.044(3) -0.022(2) 0.023(3) -0.009(2) C10 0.021(2) 0.053(4) 0.024(3) -0.019(2) 0.010(2) -0.005(2) C11 0.027(3) 0.028(3) 0.034(3) 0.012(2) 0.019(2) 0.006(2) C12 0.031(3) 0.017(2) 0.044(3) 0.003(2) 0.022(2) 0.001(2) C13 0.033(3) 0.021(2) 0.033(3) -0.005(2) 0.019(2) -0.005(2) C14 0.027(2) 0.025(3) 0.022(2) -0.0053(19) 0.012(2) -0.010(2) C15 0.032(3) 0.018(2) 0.031(3) -0.006(2) 0.023(2) -0.0042(19) C16 0.020(2) 0.035(3) 0.027(3) -0.013(2) 0.015(2) -0.003(2) C17 0.023(2) 0.023(2) 0.030(3) 0.008(2) 0.018(2) 0.0021(19) C18 0.024(2) 0.018(2) 0.024(2) -0.0011(18) 0.015(2) -0.0035(18) C19 0.032(3) 0.020(2) 0.032(3) 0.005(2) 0.021(2) 0.006(2) C21 0.028(3) 0.035(3) 0.034(3) 0.010(2) 0.019(2) 0.002(2) C23 0.040(3) 0.028(3) 0.072(4) 0.005(3) 0.042(3) 0.002(2) N11 0.0285(12) 0.0173(11) 0.0206(11) 0.0022(9) 0.0123(10) 0.0057(9) Cl1 0.0336(6) 0.0305(7) 0.0262(6) -0.0061(5) 0.0153(5) 0.0020(5) Cl2 0.0345(7) 0.0319(7) 0.0299(6) 0.0102(5) 0.0183(5) 0.0058(5) Cl3 0.0232(6) 0.0229(6) 0.0386(7) -0.0103(5) 0.0164(5) -0.0013(5) O1 0.063(3) 0.050(3) 0.036(2) -0.0027(19) 0.007(2) 0.025(2) O2 0.034(2) 0.035(2) 0.036(2) -0.0090(16) 0.0153(17) 0.0013(16) O3 0.059(3) 0.039(2) 0.060(3) -0.0060(19) 0.040(2) -0.0103(19) O4 0.050(2) 0.056(3) 0.040(2) -0.0079(19) 0.031(2) 0.0024(19) O5 0.086(3) 0.063(3) 0.098(4) 0.024(3) 0.069(3) 0.036(3) O6 0.046(2) 0.040(2) 0.036(2) 0.0100(17) 0.0094(18) -0.0060(18) O7 0.039(2) 0.072(3) 0.032(2) 0.017(2) 0.0205(18) 0.002(2) O8 0.055(3) 0.058(3) 0.031(2) -0.0022(19) 0.0179(19) -0.014(2) O10 0.032(4) 0.044(5) 0.051(5) -0.027(4) 0.029(4) -0.019(4) O10A 0.030(4) 0.054(6) 0.054(5) -0.021(4) 0.027(4) -0.011(4) O11 0.101(7) 0.018(4) 0.038(4) 0.015(3) 0.048(5) 0.020(4) O11A 0.023(4) 0.039(4) 0.031(4) 0.003(3) 0.013(3) 0.009(3) O12 0.027(8) 0.027(8) 0.032(7) -0.007(5) 0.019(6) -0.004(5) O9 0.030(8) 0.021(7) 0.046(9) -0.013(5) 0.030(7) 0.000(4) N10 0.0285(12) 0.0173(11) 0.0206(11) 0.0022(9) 0.0123(10) 0.0057(9) C25 0.045(3) 0.021(2) 0.014(2) 0.0029(19) 0.005(2) -0.001(2) C26 0.028(3) 0.049(3) 0.036(3) 0.005(2) 0.021(2) 0.008(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 Co1 N3 1.924(4) . ? Co1 N10 1.926(4) . ? Co1 N4 1.941(4) . ? Co1 N2 1.957(4) . ? Co1 N5 1.958(4) . ? Co1 O9 2.352(17) . ? Co2 N7 1.905(4) . ? Co2 N8 1.910(4) . ? Co2 N1 1.927(4) . ? Co2 N6 1.940(4) . ? Co2 N9 1.968(4) . ? N1 N2 1.360(5) . ? N1 C17 1.389(6) . ? N2 C18 1.350(5) . ? N3 C14 1.274(6) . ? N3 C1 1.472(6) . ? N4 C7 1.272(6) . ? N4 C3 1.486(6) . ? N5 C15 1.353(6) . ? N5 N6 1.355(5) . ? N6 C16 1.388(6) . ? N7 C10 1.279(7) . ? N7 C4 1.477(6) . ? N8 C11 1.303(6) . ? N8 C6 1.495(6) . ? N9 C19 1.145(6) . ? C24 C21 1.469(7) . ? C1 C2 1.506(7) . ? C2 C3 1.497(7) . ? C4 C5 1.508(8) . ? C5 C6 1.499(8) . ? C7 C15 1.457(7) . ? C8 C9 1.379(7) . ? C8 C15 1.399(7) . ? C9 C16 1.380(7) . ? C10 C16 1.429(7) . ? C11 C17 1.420(7) . ? C12 C13 1.376(7) . ? C12 C17 1.391(7) . ? C13 C18 1.391(6) . ? C14 C18 1.458(6) . ? C19 C23 1.431(7) . ? C21 N11 1.131(6) . ? Cl1 O4 1.430(4) . ? Cl1 O3 1.431(4) . ? Cl1 O2 1.437(4) . ? Cl1 O1 1.442(4) . ? Cl2 O5 1.406(4) . ? Cl2 O6 1.435(4) . ? Cl2 O7 1.439(4) . ? Cl2 O8 1.458(4) . ? Cl3 O9A 1.325(18) . ? Cl3 O12 1.376(18) . ? Cl3 O10A 1.393(7) . ? Cl3 O12B 1.398(17) . ? Cl3 O11A 1.406(7) . ? Cl3 O10 1.458(7) . ? Cl3 O9 1.478(15) . ? Cl3 O9B 1.488(18) . ? Cl3 O11 1.518(7) . ? Cl3 O12A 1.609(16) . ? O10 O9A 0.718(19) . ? O10 O12B 1.20(2) . ? O10 O9B 1.45(2) . ? O10A O11A 1.015(10) . ? O10A O11 1.766(11) . ? O11 O12B 1.357(19) . ? O11 O9A 1.77(2) . ? O11A O12A 1.618(16) . ? O11A O9B 1.702(19) . ? O12 O9 0.561(14) . ? O9A O12B 0.51(2) . ? O12A O9B 0.51(2) . ? N10 C25 1.232(6) . ? C25 C26 1.488(7) . ? 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 N3 Co1 N10 91.51(16) . . ? N3 Co1 N4 92.33(16) . . ? N10 Co1 N4 94.92(15) . . ? N3 Co1 N2 83.33(15) . . ? N10 Co1 N2 96.21(15) . . ? N4 Co1 N2 168.15(15) . . ? N3 Co1 N5 174.57(15) . . ? N10 Co1 N5 92.37(15) . . ? N4 Co1 N5 83.55(16) . . ? N2 Co1 N5 100.02(15) . . ? N3 Co1 O9 90.8(4) . . ? N10 Co1 O9 173.7(4) . . ? N4 Co1 O9 79.1(3) . . ? N2 Co1 O9 89.9(3) . . ? N5 Co1 O9 85.0(4) . . ? N7 Co2 N8 91.57(18) . . ? N7 Co2 N1 168.18(16) . . ? N8 Co2 N1 82.63(16) . . ? N7 Co2 N6 82.19(17) . . ? N8 Co2 N6 157.96(15) . . ? N1 Co2 N6 99.37(15) . . ? N7 Co2 N9 96.23(16) . . ? N8 Co2 N9 102.54(15) . . ? N1 Co2 N9 95.09(15) . . ? N6 Co2 N9 99.16(14) . . ? N2 N1 C17 117.1(4) . . ? N2 N1 Co2 129.2(3) . . ? C17 N1 Co2 113.1(3) . . ? C18 N2 N1 119.8(4) . . ? C18 N2 Co1 111.4(3) . . ? N1 N2 Co1 128.3(3) . . ? C14 N3 C1 120.2(4) . . ? C14 N3 Co1 114.2(3) . . ? C1 N3 Co1 125.6(3) . . ? C7 N4 C3 118.3(4) . . ? C7 N4 Co1 112.8(3) . . ? C3 N4 Co1 128.9(3) . . ? C15 N5 N6 119.5(4) . . ? C15 N5 Co1 112.0(3) . . ? N6 N5 Co1 128.4(3) . . ? N5 N6 C16 117.4(4) . . ? N5 N6 Co2 129.9(3) . . ? C16 N6 Co2 112.6(3) . . ? C10 N7 C4 117.8(4) . . ? C10 N7 Co2 116.5(3) . . ? C4 N7 Co2 125.6(4) . . ? C11 N8 C6 115.2(4) . . ? C11 N8 Co2 114.7(3) . . ? C6 N8 Co2 129.8(4) . . ? C19 N9 Co2 175.9(4) . . ? N3 C1 C2 110.3(4) . . ? C3 C2 C1 111.9(4) . . ? N4 C3 C2 112.6(4) . . ? N7 C4 C5 110.7(4) . . ? C6 C5 C4 111.5(5) . . ? N8 C6 C5 113.0(4) . . ? N4 C7 C15 118.3(4) . . ? C9 C8 C15 116.9(5) . . ? C16 C9 C8 118.1(4) . . ? N7 C10 C16 115.9(4) . . ? N8 C11 C17 116.8(4) . . ? C13 C12 C17 118.3(4) . . ? C12 C13 C18 116.9(4) . . ? N3 C14 C18 116.6(4) . . ? N5 C15 C8 124.1(4) . . ? N5 C15 C7 113.2(4) . . ? C8 C15 C7 122.7(4) . . ? C9 C16 N6 124.0(4) . . ? C9 C16 C10 123.3(4) . . ? N6 C16 C10 112.7(4) . . ? N1 C17 C12 123.6(4) . . ? N1 C17 C11 112.1(4) . . ? C12 C17 C11 124.3(4) . . ? N2 C18 C13 124.3(4) . . ? N2 C18 C14 114.0(4) . . ? C13 C18 C14 121.7(4) . . ? N9 C19 C23 178.8(6) . . ? N11 C21 C24 178.4(6) . . ? O4 Cl1 O3 108.5(2) . . ? O4 Cl1 O2 109.3(2) . . ? O3 Cl1 O2 109.5(2) . . ? O4 Cl1 O1 110.3(2) . . ? O3 Cl1 O1 110.0(3) . . ? O2 Cl1 O1 109.2(2) . . ? O5 Cl2 O6 110.8(3) . . ? O5 Cl2 O7 109.5(3) . . ? O6 Cl2 O7 107.3(2) . . ? O5 Cl2 O8 111.2(3) . . ? O6 Cl2 O8 108.7(2) . . ? O7 Cl2 O8 109.3(2) . . ? O9A Cl3 O12 132.8(10) . . ? O9A Cl3 O10A 126.6(9) . . ? O12 Cl3 O10A 98.6(8) . . ? O9A Cl3 O12B 21.4(10) . . ? O12 Cl3 O12B 132.0(8) . . ? O10A Cl3 O12B 114.8(8) . . ? O9A Cl3 O11A 109.2(9) . . ? O12 Cl3 O11A 113.9(6) . . ? O10A Cl3 O11A 42.5(4) . . ? O12B Cl3 O11A 114.0(7) . . ? O9A Cl3 O10 29.4(9) . . ? O12 Cl3 O10 114.1(8) . . ? O10A Cl3 O10 145.5(4) . . ? O12B Cl3 O10 49.8(8) . . ? O11A Cl3 O10 109.6(5) . . ? O9A Cl3 O9 116.2(10) . . ? O12 Cl3 O9 22.3(6) . . ? O10A Cl3 O9 107.7(7) . . ? O12B Cl3 O9 110.6(9) . . ? O11A Cl3 O9 134.2(6) . . ? O10 Cl3 O9 106.8(7) . . ? O9A Cl3 O9B 84.6(12) . . ? O12 Cl3 O9B 91.1(10) . . ? O10A Cl3 O9B 111.9(8) . . ? O12B Cl3 O9B 106.0(11) . . ? O11A Cl3 O9B 72.0(8) . . ? O10 Cl3 O9B 58.9(8) . . ? O9 Cl3 O9B 105.6(9) . . ? O9A Cl3 O11 76.7(11) . . ? O12 Cl3 O11 107.3(6) . . ? O10A Cl3 O11 74.6(5) . . ? O12B Cl3 O11 55.3(8) . . ? O11A Cl3 O11 106.8(4) . . ? O10 Cl3 O11 104.5(5) . . ? O9 Cl3 O11 89.8(6) . . ? O9B Cl3 O11 159.7(8) . . ? O9A Cl3 O12A 103.1(12) . . ? O12 Cl3 O12A 79.7(8) . . ? O10A Cl3 O12A 98.9(7) . . ? O12B Cl3 O12A 124.4(10) . . ? O11A Cl3 O12A 64.5(6) . . ? O10 Cl3 O12A 77.2(7) . . ? O9 Cl3 O12A 98.3(8) . . ? O9B Cl3 O12A 18.6(8) . . ? O11 Cl3 O12A 170.9(6) . . ? O9A O10 O12B 10(2) . . ? O9A O10 O9B 118(2) . . ? O12B O10 O9B 120.4(12) . . ? O9A O10 Cl3 64.9(16) . . ? O12B O10 Cl3 62.5(8) . . ? O9B O10 Cl3 61.6(8) . . ? O11A O10A Cl3 69.4(6) . . ? O11A O10A O11 112.4(7) . . ? Cl3 O10A O11 56.0(4) . . ? O12B O11 Cl3 57.9(8) . . ? O12B O11 O10A 96.8(9) . . ? Cl3 O11 O10A 49.5(3) . . ? O12B O11 O9A 11.2(10) . . ? Cl3 O11 O9A 46.7(6) . . ? O10A O11 O9A 86.7(7) . . ? O10A O11A Cl3 68.0(6) . . ? O10A O11A O12A 118.5(9) . . ? Cl3 O11A O12A 63.8(6) . . ? O10A O11A O9B 120.8(9) . . ? Cl3 O11A O9B 56.2(7) . . ? O12A O11A O9B 17.6(8) . . ? O9 O12 Cl3 89(4) . . ? O12 O9 Cl3 69(3) . . ? O12 O9 Co1 102(4) . . ? Cl3 O9 Co1 137.1(10) . . ? O12B O9A O10 156(5) . . ? O12B O9A Cl3 87(4) . . ? O10 O9A Cl3 85.7(19) . . ? O12B O9A O11 31(3) . . ? O10 O9A O11 138(2) . . ? Cl3 O9A O11 56.6(8) . . ? O9B O12A Cl3 67(3) . . ? O9B O12A O11A 90(3) . . ? Cl3 O12A O11A 51.6(5) . . ? O12A O9B O10 152(4) . . ? O12A O9B Cl3 94(3) . . ? O10 O9B Cl3 59.6(8) . . ? O12A O9B O11A 72(3) . . ? O10 O9B O11A 95.6(11) . . ? Cl3 O9B O11A 51.8(6) . . ? O9A O12B O10 14(3) . . ? O9A O12B O11 138(4) . . ? O10 O12B O11 133.4(14) . . ? O9A O12B Cl3 71(3) . . ? O10 O12B Cl3 67.7(9) . . ? O11 O12B Cl3 66.9(8) . . ? C25 N10 Co1 171.5(3) . . ? N10 C25 C26 178.5(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.677 _refine_diff_density_min -1.935 _refine_diff_density_rms 0.095 #===END