# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_whh20 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common MesDPBPhHNiSiH2Ph _chemical_formula_moiety 'C26.50 H26 B0.50 Ni0.50 O0.25 P Si0.50' _chemical_formula_sum 'C26.50 H26 B0.50 Ni0.50 O0.25 P Si0.50' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 428.25 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6097(8) _cell_length_b 13.0379(9) _cell_length_c 17.3875(12) _cell_angle_alpha 68.361(4) _cell_angle_beta 72.030(4) _cell_angle_gamma 64.875(4) _cell_volume 2178.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9836 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 30.59 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8577 _exptl_absorpt_correction_T_max 0.9385 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 105776 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 30.51 _reflns_number_total 13243 _reflns_number_gt 11307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.7491P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13243 _refine_ls_number_parameters 564 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Ni Ni 0.694411(16) 0.088420(14) 0.258331(10) 0.01290(5) Uani 1 1 d . . . P1 P 0.62094(3) 0.24179(3) 0.16006(2) 0.01330(7) Uani 1 1 d . . . P2 P 0.76322(3) -0.07997(3) 0.34858(2) 0.01350(7) Uani 1 1 d . . . Si Si 0.77626(4) 0.18772(3) 0.29490(2) 0.01699(8) Uani 1 1 d . . . H101 H 0.796(2) 0.1432(19) 0.3786(13) 0.032(5) Uiso 1 1 d . . . H102 H 0.698(2) 0.3053(19) 0.2900(14) 0.035(6) Uiso 1 1 d . . . B B 0.66722(15) -0.02306(13) 0.18334(10) 0.0152(3) Uani 1 1 d . . . H100 H 0.6091(18) 0.0335(17) 0.2414(12) 0.021(5) Uiso 1 1 d . . . C1 C 0.45689(13) 0.32938(11) 0.19953(9) 0.0156(2) Uani 1 1 d . . . C2 C 0.41870(15) 0.31605(13) 0.28602(9) 0.0216(3) Uani 1 1 d . . . H2A H 0.4758 0.2585 0.3231 0.026 Uiso 1 1 calc R . . C3 C 0.29758(16) 0.38649(14) 0.31825(10) 0.0255(3) Uani 1 1 d . . . H3A H 0.2723 0.3769 0.3772 0.031 Uiso 1 1 calc R . . C4 C 0.21361(15) 0.47064(13) 0.26467(10) 0.0236(3) Uani 1 1 d . . . H4A H 0.1310 0.5189 0.2868 0.028 Uiso 1 1 calc R . . C5 C 0.25043(14) 0.48417(13) 0.17878(10) 0.0222(3) Uani 1 1 d . . . H5A H 0.1930 0.5421 0.1421 0.027 Uiso 1 1 calc R . . C6 C 0.37085(14) 0.41350(13) 0.14607(9) 0.0186(3) Uani 1 1 d . . . H6A H 0.3948 0.4223 0.0872 0.022 Uiso 1 1 calc R . . C7 C 0.70103(13) 0.34862(12) 0.10414(8) 0.0149(2) Uani 1 1 d . . . C8 C 0.65087(13) 0.46255(12) 0.11334(9) 0.0177(3) Uani 1 1 d . . . H8A H 0.5696 0.4883 0.1484 0.021 Uiso 1 1 calc R . . C9 C 0.72031(14) 0.53807(13) 0.07103(10) 0.0214(3) Uani 1 1 d . . . H9A H 0.6859 0.6157 0.0769 0.026 Uiso 1 1 calc R . . C10 C 0.83929(14) 0.50069(13) 0.02044(10) 0.0217(3) Uani 1 1 d . . . H10A H 0.8863 0.5527 -0.0083 0.026 Uiso 1 1 calc R . . C11 C 0.89019(14) 0.38718(14) 0.01154(9) 0.0206(3) Uani 1 1 d . . . H11A H 0.9720 0.3615 -0.0231 0.025 Uiso 1 1 calc R . . C12 C 0.82170(13) 0.31172(12) 0.05308(9) 0.0173(2) Uani 1 1 d . . . H12A H 0.8568 0.2342 0.0469 0.021 Uiso 1 1 calc R . . C13 C 0.61415(12) 0.19236(12) 0.07695(8) 0.0141(2) Uani 1 1 d . . . C14 C 0.59282(13) 0.27097(12) -0.00232(9) 0.0170(2) Uani 1 1 d . . . H14A H 0.5855 0.3504 -0.0141 0.020 Uiso 1 1 calc R . . C15 C 0.58234(13) 0.23263(13) -0.06360(9) 0.0184(3) Uani 1 1 d . . . H15A H 0.5676 0.2858 -0.1173 0.022 Uiso 1 1 calc R . . C16 C 0.59344(14) 0.11660(13) -0.04609(9) 0.0193(3) Uani 1 1 d . . . H16A H 0.5850 0.0903 -0.0876 0.023 Uiso 1 1 calc R . . C17 C 0.61692(14) 0.03854(13) 0.03212(9) 0.0189(3) Uani 1 1 d . . . H17A H 0.6247 -0.0408 0.0429 0.023 Uiso 1 1 calc R . . C18 C 0.62957(13) 0.07330(12) 0.09583(8) 0.0151(2) Uani 1 1 d . . . C19 C 0.59487(14) -0.11957(12) 0.21663(9) 0.0171(2) Uani 1 1 d . . . C20 C 0.65520(15) -0.23755(13) 0.21221(10) 0.0211(3) Uani 1 1 d . . . C21 C 0.58545(18) -0.31455(14) 0.24552(10) 0.0267(3) Uani 1 1 d . . . H21A H 0.6286 -0.3938 0.2428 0.032 Uiso 1 1 calc R . . C22 C 0.45598(18) -0.27902(16) 0.28216(10) 0.0290(4) Uani 1 1 d . . . C23 C 0.39453(16) -0.16232(16) 0.28279(10) 0.0262(3) Uani 1 1 d . . . H23A H 0.3047 -0.1351 0.3053 0.031 Uiso 1 1 calc R . . C24 C 0.46078(14) -0.08315(13) 0.25120(9) 0.0199(3) Uani 1 1 d . . . C25 C 0.79467(16) -0.28874(14) 0.17112(12) 0.0280(3) Uani 1 1 d . . . H25A H 0.8120 -0.3680 0.1687 0.042 Uiso 1 1 calc R . . H25B H 0.8523 -0.2932 0.2042 0.042 Uiso 1 1 calc R . . H25C H 0.8099 -0.2382 0.1140 0.042 Uiso 1 1 calc R . . C26 C 0.3850(2) -0.3650(2) 0.32062(14) 0.0438(5) Uani 1 1 d . . . H26A H 0.2930 -0.3227 0.3177 0.066 Uiso 1 1 calc R . . H26B H 0.3950 -0.4038 0.3795 0.066 Uiso 1 1 calc R . . H26C H 0.4210 -0.4245 0.2896 0.066 Uiso 1 1 calc R . . C27 C 0.38346(15) 0.04152(14) 0.25640(10) 0.0239(3) Uani 1 1 d . . . H27A H 0.2910 0.0533 0.2710 0.036 Uiso 1 1 calc R . . H27B H 0.4010 0.0968 0.2019 0.036 Uiso 1 1 calc R . . H27C H 0.4081 0.0555 0.2997 0.036 Uiso 1 1 calc R . . C28 C 0.82201(13) -0.07784(11) 0.18395(8) 0.0138(2) Uani 1 1 d . . . C29 C 0.91411(14) -0.08250(12) 0.10944(9) 0.0174(3) Uani 1 1 d . . . H29A H 0.8857 -0.0418 0.0570 0.021 Uiso 1 1 calc R . . C30 C 1.04548(14) -0.14473(13) 0.10990(9) 0.0205(3) Uani 1 1 d . . . H30A H 1.1052 -0.1439 0.0583 0.025 Uiso 1 1 calc R . . C31 C 1.08951(14) -0.20789(13) 0.18532(10) 0.0211(3) Uani 1 1 d . . . H31A H 1.1782 -0.2552 0.1855 0.025 Uiso 1 1 calc R . . C32 C 1.00302(13) -0.20160(12) 0.26068(9) 0.0176(3) Uani 1 1 d . . . H32A H 1.0330 -0.2430 0.3126 0.021 Uiso 1 1 calc R . . C33 C 0.87186(13) -0.13435(11) 0.26023(8) 0.0139(2) Uani 1 1 d . . . C34 C 0.64677(14) -0.15289(12) 0.40338(9) 0.0178(3) Uani 1 1 d . . . C35 C 0.67638(16) -0.27206(14) 0.41507(11) 0.0271(3) Uani 1 1 d . . . H35A H 0.7599 -0.3184 0.3925 0.033 Uiso 1 1 calc R . . C36 C 0.58289(17) -0.32330(15) 0.46014(12) 0.0322(4) Uani 1 1 d . . . H36A H 0.6024 -0.4045 0.4676 0.039 Uiso 1 1 calc R . . C37 C 0.46151(17) -0.25599(16) 0.49403(11) 0.0300(4) Uani 1 1 d . . . H37A H 0.3989 -0.2918 0.5259 0.036 Uiso 1 1 calc R . . C38 C 0.43114(16) -0.13751(16) 0.48174(10) 0.0265(3) Uani 1 1 d . . . H38A H 0.3475 -0.0914 0.5044 0.032 Uiso 1 1 calc R . . C39 C 0.52346(14) -0.08573(14) 0.43610(9) 0.0203(3) Uani 1 1 d . . . H39A H 0.5023 -0.0039 0.4271 0.024 Uiso 1 1 calc R . . C40 C 0.85773(14) -0.11756(12) 0.42759(9) 0.0171(2) Uani 1 1 d . . . C41 C 0.97230(16) -0.09358(14) 0.40521(9) 0.0228(3) Uani 1 1 d . . . H41A H 1.0036 -0.0611 0.3478 0.027 Uiso 1 1 calc R . . C42 C 1.0402(2) -0.11704(19) 0.46646(12) 0.0386(5) Uani 1 1 d . . . H42A H 1.1191 -0.1028 0.4508 0.046 Uiso 1 1 calc R . . C43 C 0.9928(3) -0.1614(2) 0.55070(12) 0.0514(7) Uani 1 1 d . . . H43A H 1.0391 -0.1766 0.5926 0.062 Uiso 1 1 calc R . . C44 C 0.8785(2) -0.18339(19) 0.57368(10) 0.0369(4) Uani 1 1 d . . . H44A H 0.8457 -0.2127 0.6314 0.044 Uiso 1 1 calc R . . C45 C 0.81177(16) -0.16270(14) 0.51250(9) 0.0225(3) Uani 1 1 d . . . H45A H 0.7342 -0.1794 0.5285 0.027 Uiso 1 1 calc R . . C46 C 0.93675(15) 0.19123(13) 0.22655(9) 0.0204(3) Uani 1 1 d . . . C47 C 0.98201(19) 0.27974(16) 0.21732(10) 0.0304(4) Uani 1 1 d . . . H47A H 0.9322 0.3378 0.2469 0.036 Uiso 1 1 calc R . . C48 C 1.0994(2) 0.2837(2) 0.16524(12) 0.0405(5) Uani 1 1 d . . . H48A H 1.1299 0.3431 0.1609 0.049 Uiso 1 1 calc R . . C49 C 1.17166(18) 0.2025(2) 0.12018(12) 0.0400(5) Uani 1 1 d . . . H49A H 1.2501 0.2075 0.0834 0.048 Uiso 1 1 calc R . . C50 C 1.12990(16) 0.11371(17) 0.12862(11) 0.0339(4) Uani 1 1 d . . . H50A H 1.1802 0.0566 0.0984 0.041 Uiso 1 1 calc R . . C51 C 1.01370(15) 0.10807(14) 0.18169(10) 0.0242(3) Uani 1 1 d . . . H51A H 0.9861 0.0462 0.1875 0.029 Uiso 1 1 calc R . . O1S O 0.0234(2) 0.5029(2) 0.55651(17) 0.0262(5) Uani 0.50 1 d P A -1 C1S C -0.0164(4) 0.5077(4) 0.4857(2) 0.0276(8) Uani 0.50 1 d P A -1 H1S1 H 0.0598 0.4709 0.4468 0.033 Uiso 0.50 1 calc PR A -1 H1S2 H -0.0584 0.5909 0.4553 0.033 Uiso 0.50 1 calc PR A -1 C2S C -0.1091(3) 0.4441(3) 0.51405(16) 0.0310(7) Uani 0.50 1 d P A -1 H2S1 H -0.0667 0.3615 0.5434 0.046 Uiso 0.50 1 calc PR A -1 H2S2 H -0.1370 0.4476 0.4651 0.046 Uiso 0.50 1 calc PR A -1 H2S3 H -0.1845 0.4811 0.5523 0.046 Uiso 0.50 1 calc PR A -1 C3S C 0.1085(3) 0.5657(3) 0.53320(16) 0.0277(7) Uani 0.50 1 d PR A -1 H3S1 H 0.0665 0.6485 0.5021 0.033 Uiso 0.50 1 calc PR A -1 H3S2 H 0.1880 0.5297 0.4959 0.033 Uiso 0.50 1 calc PR A -1 C4S C 0.1425(4) 0.5622(3) 0.6114(3) 0.0377(8) Uani 0.50 1 d P A -1 H4S1 H 0.0631 0.5941 0.6494 0.057 Uiso 0.50 1 calc PR A -1 H4S2 H 0.1970 0.6098 0.5959 0.057 Uiso 0.50 1 calc PR A -1 H4S3 H 0.1896 0.4806 0.6398 0.057 Uiso 0.50 1 calc PR 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 Ni 0.01505(8) 0.01285(8) 0.01171(8) -0.00207(6) -0.00327(6) -0.00626(6) P1 0.01476(15) 0.01273(14) 0.01234(15) -0.00279(11) -0.00243(11) -0.00536(12) P2 0.01531(15) 0.01405(14) 0.01148(14) -0.00214(11) -0.00237(12) -0.00666(12) Si 0.02398(19) 0.01825(17) 0.01290(17) -0.00436(13) -0.00269(14) -0.01161(15) B 0.0175(7) 0.0155(6) 0.0152(6) -0.0033(5) -0.0051(5) -0.0075(5) C1 0.0152(6) 0.0137(5) 0.0169(6) -0.0039(5) -0.0010(5) -0.0059(5) C2 0.0229(7) 0.0178(6) 0.0160(6) -0.0010(5) -0.0014(5) -0.0042(5) C3 0.0252(7) 0.0224(7) 0.0177(7) -0.0037(5) 0.0028(6) -0.0043(6) C4 0.0191(7) 0.0198(6) 0.0256(7) -0.0068(6) 0.0013(6) -0.0043(5) C5 0.0189(7) 0.0213(7) 0.0247(7) -0.0067(6) -0.0060(6) -0.0038(5) C6 0.0177(6) 0.0213(6) 0.0179(6) -0.0054(5) -0.0037(5) -0.0074(5) C7 0.0160(6) 0.0158(6) 0.0129(6) -0.0018(4) -0.0030(5) -0.0073(5) C8 0.0157(6) 0.0161(6) 0.0211(6) -0.0044(5) -0.0033(5) -0.0060(5) C9 0.0208(7) 0.0165(6) 0.0281(7) -0.0022(5) -0.0087(6) -0.0082(5) C10 0.0208(7) 0.0235(7) 0.0217(7) 0.0026(5) -0.0082(5) -0.0131(6) C11 0.0173(6) 0.0282(7) 0.0158(6) -0.0029(5) -0.0025(5) -0.0106(6) C12 0.0170(6) 0.0198(6) 0.0152(6) -0.0055(5) -0.0026(5) -0.0061(5) C13 0.0134(6) 0.0164(6) 0.0127(6) -0.0036(4) -0.0029(4) -0.0053(5) C14 0.0171(6) 0.0169(6) 0.0151(6) -0.0022(5) -0.0041(5) -0.0054(5) C15 0.0158(6) 0.0233(6) 0.0142(6) -0.0034(5) -0.0049(5) -0.0052(5) C16 0.0188(6) 0.0255(7) 0.0178(6) -0.0069(5) -0.0068(5) -0.0084(5) C17 0.0211(7) 0.0207(6) 0.0196(6) -0.0052(5) -0.0072(5) -0.0094(5) C18 0.0142(6) 0.0176(6) 0.0156(6) -0.0044(5) -0.0040(5) -0.0067(5) C19 0.0209(6) 0.0197(6) 0.0156(6) -0.0018(5) -0.0068(5) -0.0119(5) C20 0.0270(7) 0.0206(6) 0.0220(7) -0.0033(5) -0.0097(6) -0.0126(6) C21 0.0398(9) 0.0223(7) 0.0274(8) -0.0016(6) -0.0134(7) -0.0189(7) C22 0.0399(9) 0.0358(9) 0.0225(7) 0.0024(6) -0.0113(7) -0.0284(8) C23 0.0259(8) 0.0390(9) 0.0206(7) -0.0020(6) -0.0057(6) -0.0220(7) C24 0.0210(7) 0.0269(7) 0.0158(6) -0.0021(5) -0.0064(5) -0.0133(6) C25 0.0298(8) 0.0213(7) 0.0406(9) -0.0142(7) -0.0081(7) -0.0099(6) C26 0.0567(13) 0.0491(12) 0.0405(11) 0.0031(9) -0.0113(9) -0.0434(11) C27 0.0177(7) 0.0298(8) 0.0242(7) -0.0057(6) -0.0053(5) -0.0088(6) C28 0.0171(6) 0.0127(5) 0.0144(6) -0.0039(4) -0.0037(5) -0.0071(5) C29 0.0214(6) 0.0193(6) 0.0131(6) -0.0043(5) -0.0033(5) -0.0086(5) C30 0.0201(7) 0.0222(6) 0.0175(6) -0.0072(5) 0.0011(5) -0.0077(5) C31 0.0157(6) 0.0204(6) 0.0229(7) -0.0066(5) -0.0021(5) -0.0029(5) C32 0.0174(6) 0.0163(6) 0.0170(6) -0.0027(5) -0.0050(5) -0.0043(5) C33 0.0159(6) 0.0131(5) 0.0130(6) -0.0026(4) -0.0026(4) -0.0064(5) C34 0.0192(6) 0.0198(6) 0.0145(6) -0.0011(5) -0.0032(5) -0.0100(5) C35 0.0231(7) 0.0198(7) 0.0345(9) -0.0019(6) -0.0041(6) -0.0095(6) C36 0.0314(9) 0.0220(7) 0.0411(10) 0.0026(7) -0.0079(7) -0.0161(7) C37 0.0293(8) 0.0390(9) 0.0240(8) 0.0004(7) -0.0029(6) -0.0231(7) C38 0.0219(7) 0.0378(9) 0.0202(7) -0.0080(6) 0.0019(6) -0.0149(7) C39 0.0212(7) 0.0251(7) 0.0157(6) -0.0058(5) -0.0025(5) -0.0098(6) C40 0.0232(7) 0.0171(6) 0.0136(6) -0.0030(5) -0.0058(5) -0.0089(5) C41 0.0299(8) 0.0275(7) 0.0167(6) -0.0005(5) -0.0078(6) -0.0175(6) C42 0.0523(11) 0.0558(12) 0.0260(8) 0.0051(8) -0.0172(8) -0.0424(10) C43 0.0808(16) 0.0825(17) 0.0217(9) 0.0078(9) -0.0251(10) -0.0648(15) C44 0.0619(13) 0.0527(11) 0.0135(7) -0.0005(7) -0.0094(7) -0.0414(10) C45 0.0318(8) 0.0253(7) 0.0148(6) -0.0037(5) -0.0035(6) -0.0160(6) C46 0.0255(7) 0.0265(7) 0.0134(6) 0.0018(5) -0.0076(5) -0.0163(6) C47 0.0477(10) 0.0376(9) 0.0196(7) 0.0022(6) -0.0128(7) -0.0314(8) C48 0.0512(12) 0.0557(12) 0.0289(9) 0.0128(8) -0.0188(8) -0.0447(10) C49 0.0255(8) 0.0559(12) 0.0303(9) 0.0130(8) -0.0094(7) -0.0247(8) C50 0.0192(7) 0.0395(9) 0.0281(8) 0.0027(7) -0.0028(6) -0.0079(7) C51 0.0211(7) 0.0268(7) 0.0219(7) 0.0000(6) -0.0052(6) -0.0106(6) O1S 0.0320(13) 0.0261(11) 0.0204(12) -0.0063(10) -0.0022(10) -0.0119(10) C1S 0.030(2) 0.0354(19) 0.020(3) -0.0073(19) -0.0053(15) -0.0133(18) C2S 0.0366(19) 0.0264(16) 0.0312(18) -0.0085(14) -0.0074(15) -0.0108(14) C3S 0.0266(16) 0.0210(14) 0.0324(18) -0.0073(13) -0.0029(13) -0.0073(12) C4S 0.043(2) 0.0289(17) 0.045(2) -0.0144(16) -0.0157(17) -0.0070(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni P1 2.1393(4) . ? Ni P2 2.1596(4) . ? Ni Si 2.2379(4) . ? Ni B 2.4401(15) . ? Ni H100 1.586(19) . ? P1 C7 1.8147(13) . ? P1 C13 1.8193(14) . ? P1 C1 1.8241(14) . ? P2 C34 1.8078(14) . ? P2 C33 1.8169(14) . ? P2 C40 1.8189(14) . ? Si C46 1.8848(15) . ? Si H101 1.41(2) . ? Si H102 1.40(2) . ? B C18 1.618(2) . ? B C28 1.630(2) . ? B C19 1.638(2) . ? B H100 1.314(19) . ? C1 C2 1.396(2) . ? C1 C6 1.3984(19) . ? C2 C3 1.390(2) . ? C2 H2A 0.9500 . ? C3 C4 1.386(2) . ? C3 H3A 0.9500 . ? C4 C5 1.386(2) . ? C4 H4A 0.9500 . ? C5 C6 1.389(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.3980(19) . ? C7 C12 1.3990(19) . ? C8 C9 1.3908(19) . ? C8 H8A 0.9500 . ? C9 C10 1.383(2) . ? C9 H9A 0.9500 . ? C10 C11 1.390(2) . ? C10 H10A 0.9500 . ? C11 C12 1.381(2) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.4017(18) . ? C13 C18 1.4050(18) . ? C14 C15 1.387(2) . ? C14 H14A 0.9500 . ? C15 C16 1.385(2) . ? C15 H15A 0.9500 . ? C16 C17 1.390(2) . ? C16 H16A 0.9500 . ? C17 C18 1.4075(19) . ? C17 H17A 0.9500 . ? C19 C20 1.415(2) . ? C19 C24 1.420(2) . ? C20 C21 1.404(2) . ? C20 C25 1.516(2) . ? C21 C22 1.384(3) . ? C21 H21A 0.9500 . ? C22 C23 1.382(3) . ? C22 C26 1.508(2) . ? C23 C24 1.398(2) . ? C23 H23A 0.9500 . ? C24 C27 1.509(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.4048(19) . ? C28 C33 1.4240(18) . ? C29 C30 1.392(2) . ? C29 H29A 0.9500 . ? C30 C31 1.385(2) . ? C30 H30A 0.9500 . ? C31 C32 1.389(2) . ? C31 H31A 0.9500 . ? C32 C33 1.3986(19) . ? C32 H32A 0.9500 . ? C34 C35 1.389(2) . ? C34 C39 1.393(2) . ? C35 C36 1.394(2) . ? C35 H35A 0.9500 . ? C36 C37 1.386(3) . ? C36 H36A 0.9500 . ? C37 C38 1.377(3) . ? C37 H37A 0.9500 . ? C38 C39 1.389(2) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C45 1.3967(19) . ? C40 C41 1.401(2) . ? C41 C42 1.386(2) . ? C41 H41A 0.9500 . ? C42 C43 1.389(3) . ? C42 H42A 0.9500 . ? C43 C44 1.384(3) . ? C43 H43A 0.9500 . ? C44 C45 1.387(2) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C51 1.398(2) . ? C46 C47 1.400(2) . ? C47 C48 1.395(3) . ? C47 H47A 0.9500 . ? C48 C49 1.375(3) . ? C48 H48A 0.9500 . ? C49 C50 1.380(3) . ? C49 H49A 0.9500 . ? C50 C51 1.394(2) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? O1S C1S 1.415(5) . ? O1S C3S 1.415(4) . ? C1S C2S 1.490(5) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C3S C4S 1.510(5) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? 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 P1 Ni P2 171.813(15) . . ? P1 Ni Si 89.826(16) . . ? P2 Ni Si 98.101(16) . . ? P1 Ni B 86.56(4) . . ? P2 Ni B 85.27(4) . . ? Si Ni B 161.50(4) . . ? P1 Ni H100 87.2(7) . . ? P2 Ni H100 85.4(7) . . ? Si Ni H100 168.3(7) . . ? B Ni H100 29.4(7) . . ? C7 P1 C13 103.47(6) . . ? C7 P1 C1 104.20(6) . . ? C13 P1 C1 108.15(6) . . ? C7 P1 Ni 122.92(5) . . ? C13 P1 Ni 107.59(4) . . ? C1 P1 Ni 109.69(5) . . ? C34 P2 C33 113.24(6) . . ? C34 P2 C40 103.62(6) . . ? C33 P2 C40 108.32(6) . . ? C34 P2 Ni 115.80(5) . . ? C33 P2 Ni 87.12(4) . . ? C40 P2 Ni 127.53(5) . . ? C46 Si Ni 111.96(5) . . ? C46 Si H101 106.6(8) . . ? Ni Si H101 114.6(8) . . ? C46 Si H102 105.9(9) . . ? Ni Si H102 114.5(9) . . ? H101 Si H102 102.5(12) . . ? C18 B C28 113.40(11) . . ? C18 B C19 112.59(11) . . ? C28 B C19 115.49(11) . . ? C18 B Ni 103.66(8) . . ? C28 B Ni 76.29(7) . . ? C19 B Ni 130.62(10) . . ? C18 B H100 105.8(8) . . ? C28 B H100 108.1(8) . . ? C19 B H100 100.0(8) . . ? Ni B H100 36.4(8) . . ? C2 C1 C6 119.01(13) . . ? C2 C1 P1 118.50(11) . . ? C6 C1 P1 122.39(11) . . ? C3 C2 C1 120.39(14) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C4 C3 C2 120.17(14) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 119.85(14) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 120.38(14) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 120.18(13) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? C8 C7 C12 119.26(12) . . ? C8 C7 P1 123.07(10) . . ? C12 C7 P1 117.59(10) . . ? C9 C8 C7 119.84(13) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C10 C9 C8 120.34(14) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C9 C10 C11 120.11(13) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 119.95(14) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 120.49(13) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? C14 C13 C18 121.69(12) . . ? C14 C13 P1 120.90(10) . . ? C18 C13 P1 117.40(10) . . ? C15 C14 C13 119.95(13) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 119.70(13) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C16 C17 120.08(13) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C18 122.14(13) . . ? C16 C17 H17A 118.9 . . ? C18 C17 H17A 118.9 . . ? C13 C18 C17 116.40(12) . . ? C13 C18 B 123.34(12) . . ? C17 C18 B 120.19(12) . . ? C20 C19 C24 116.51(13) . . ? C20 C19 B 125.00(13) . . ? C24 C19 B 118.48(12) . . ? C21 C20 C19 120.47(15) . . ? C21 C20 C25 115.79(14) . . ? C19 C20 C25 123.73(13) . . ? C22 C21 C20 122.29(16) . . ? C22 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C23 C22 C21 117.62(14) . . ? C23 C22 C26 121.31(18) . . ? C21 C22 C26 121.07(18) . . ? C22 C23 C24 121.85(15) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C23 C24 C19 121.12(15) . . ? C23 C24 C27 116.90(14) . . ? C19 C24 C27 121.98(13) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 115.96(12) . . ? C29 C28 B 121.81(12) . . ? C33 C28 B 121.94(12) . . ? C30 C29 C28 122.23(13) . . ? C30 C29 H29A 118.9 . . ? C28 C29 H29A 118.9 . . ? C31 C30 C29 120.29(13) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C30 C31 C32 119.54(13) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C31 C32 C33 120.10(13) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C32 C33 C28 121.45(12) . . ? C32 C33 P2 122.85(10) . . ? C28 C33 P2 113.73(10) . . ? C35 C34 C39 119.55(13) . . ? C35 C34 P2 122.74(12) . . ? C39 C34 P2 117.70(11) . . ? C34 C35 C36 119.67(15) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C37 C36 C35 120.15(16) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C38 C37 C36 120.40(15) . . ? C38 C37 H37A 119.8 . . ? C36 C37 H37A 119.8 . . ? C37 C38 C39 119.67(15) . . ? C37 C38 H38A 120.2 . . ? C39 C38 H38A 120.2 . . ? C38 C39 C34 120.53(15) . . ? C38 C39 H39A 119.7 . . ? C34 C39 H39A 119.7 . . ? C45 C40 C41 118.94(13) . . ? C45 C40 P2 120.17(11) . . ? C41 C40 P2 120.71(10) . . ? C42 C41 C40 120.27(14) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 120.09(17) . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C44 C43 C42 120.13(16) . . ? C44 C43 H43A 119.9 . . ? C42 C43 H43A 119.9 . . ? C43 C44 C45 120.04(16) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 C40 120.50(15) . . ? C44 C45 H45A 119.8 . . ? C40 C45 H45A 119.7 . . ? C51 C46 C47 117.36(15) . . ? C51 C46 Si 121.79(11) . . ? C47 C46 Si 120.83(13) . . ? C48 C47 C46 120.74(19) . . ? C48 C47 H47A 119.6 . . ? C46 C47 H47A 119.6 . . ? C49 C48 C47 120.67(17) . . ? C49 C48 H48A 119.7 . . ? C47 C48 H48A 119.7 . . ? C48 C49 C50 119.78(17) . . ? C48 C49 H49A 120.1 . . ? C50 C49 H49A 120.1 . . ? C49 C50 C51 119.80(19) . . ? C49 C50 H50A 120.1 . . ? C51 C50 H50A 120.1 . . ? C50 C51 C46 121.60(16) . . ? C50 C51 H51A 119.2 . . ? C46 C51 H51A 119.2 . . ? C1S O1S C3S 111.7(3) . . ? O1S C1S C2S 109.4(3) . . ? O1S C1S H1S1 109.8 . . ? C2S C1S H1S1 109.8 . . ? O1S C1S H1S2 109.8 . . ? C2S C1S H1S2 109.8 . . ? H1S1 C1S H1S2 108.2 . . ? O1S C3S C4S 109.2(3) . . ? O1S C3S H3S1 109.8 . . ? C4S C3S H3S1 109.8 . . ? O1S C3S H3S2 109.8 . . ? C4S C3S H3S2 109.8 . . ? H3S1 C3S H3S2 108.3 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.479 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.064 _database_code_depnum_ccdc_archive 'CCDC 961588' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_snm12 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common MesDPBPhHNiSiHPh2 _chemical_formula_moiety 'C60 H54 B Ni P2 Si' _chemical_formula_sum 'C60 H54 B Ni P2 Si' _chemical_melting_point ? _exptl_crystal_description blade _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 934.58 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1452(6) _cell_length_b 20.3316(10) _cell_length_c 21.4335(11) _cell_angle_alpha 69.986(3) _cell_angle_beta 77.017(3) _cell_angle_gamma 82.180(3) _cell_volume 4835.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9330 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.39 _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 0.532 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8114 _exptl_absorpt_correction_T_max 0.9607 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 107064 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.02 _reflns_number_total 19001 _reflns_number_gt 14294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+5.1190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19001 _refine_ls_number_parameters 1193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Ni1 Ni 0.32528(2) 0.480325(16) 0.285402(16) 0.01253(8) Uani 1 1 d . . . Ni2 Ni 0.31022(3) -0.014218(17) 0.291277(17) 0.01430(8) Uani 1 1 d . . . P11 P 0.29474(5) 0.47906(3) 0.18909(3) 0.01397(14) Uani 1 1 d . . . P12 P 0.38319(5) 0.49051(3) 0.36944(3) 0.01264(14) Uani 1 1 d . . . P21 P 0.27549(5) -0.01839(3) 0.19771(3) 0.01502(14) Uani 1 1 d . . . P22 P 0.37771(5) -0.01766(3) 0.37668(3) 0.01497(14) Uani 1 1 d . . . Si1 Si 0.14489(5) 0.48429(4) 0.34023(4) 0.01391(15) Uani 1 1 d . . . H101 H 0.138(2) 0.4587(14) 0.4101(14) 0.020(7) Uiso 1 1 d . . . Si2 Si 0.13246(6) -0.00186(4) 0.34726(4) 0.01603(15) Uani 1 1 d . . . H201 H 0.131(2) 0.0337(15) 0.3936(15) 0.026(8) Uiso 1 1 d . . . B1 B 0.5217(2) 0.50678(16) 0.22124(15) 0.0165(6) Uani 1 1 d . . . B2 B 0.5120(2) -0.04213(15) 0.24183(15) 0.0162(6) Uani 1 1 d . . . H100 H 0.455(2) 0.4587(14) 0.2543(14) 0.017(7) Uiso 1 1 d . . . H200 H 0.436(2) 0.0058(14) 0.2473(14) 0.021(7) Uiso 1 1 d . . . C11 C 0.1631(2) 0.49004(14) 0.15773(13) 0.0188(6) Uani 1 1 d . . . C12 C 0.1357(2) 0.44127(16) 0.13228(16) 0.0279(7) Uani 1 1 d . . . H12A H 0.1848 0.4007 0.1320 0.033 Uiso 1 1 calc R . . C13 C 0.0358(3) 0.45199(18) 0.10714(19) 0.0387(8) Uani 1 1 d . . . H13A H 0.0171 0.4184 0.0900 0.046 Uiso 1 1 calc R . . C14 C -0.0356(2) 0.51061(18) 0.10691(18) 0.0365(8) Uani 1 1 d . . . H14A H -0.1028 0.5179 0.0891 0.044 Uiso 1 1 calc R . . C15 C -0.0092(2) 0.55901(17) 0.13274(16) 0.0297(7) Uani 1 1 d . . . H15A H -0.0584 0.5996 0.1327 0.036 Uiso 1 1 calc R . . C16 C 0.0886(2) 0.54835(15) 0.15852(14) 0.0218(6) Uani 1 1 d . . . H16A H 0.1053 0.5813 0.1771 0.026 Uiso 1 1 calc R . . C17 C 0.3754(2) 0.41006(14) 0.15937(14) 0.0175(5) Uani 1 1 d . . . C18 C 0.3745(2) 0.34191(14) 0.20386(14) 0.0219(6) Uani 1 1 d . . . H18A H 0.3323 0.3324 0.2487 0.026 Uiso 1 1 calc R . . C19 C 0.4349(2) 0.28764(16) 0.18319(16) 0.0298(7) Uani 1 1 d . . . H19A H 0.4336 0.2410 0.2136 0.036 Uiso 1 1 calc R . . C21 C 0.3385(2) 0.05401(14) 0.12801(14) 0.0189(6) Uani 1 1 d . . . C22 C 0.3158(2) 0.11917(15) 0.13748(15) 0.0250(6) Uani 1 1 d . . . H22A H 0.2707 0.1230 0.1786 0.030 Uiso 1 1 calc R . . C23 C 0.3586(3) 0.17849(17) 0.08709(17) 0.0334(7) Uani 1 1 d . . . H23A H 0.3417 0.2233 0.0930 0.040 Uiso 1 1 calc R . . C24 C 0.4261(3) 0.17174(18) 0.02819(17) 0.0372(8) Uani 1 1 d . . . H24A H 0.4565 0.2122 -0.0063 0.045 Uiso 1 1 calc R . . C25 C 0.4500(2) 0.10760(19) 0.01864(16) 0.0354(8) Uani 1 1 d . . . H25A H 0.4972 0.1039 -0.0220 0.042 Uiso 1 1 calc R . . C26 C 0.4053(2) 0.04794(16) 0.06832(14) 0.0258(6) Uani 1 1 d . . . H26A H 0.4203 0.0036 0.0615 0.031 Uiso 1 1 calc R . . C27 C 0.1459(2) -0.02735(14) 0.17185(14) 0.0185(6) Uani 1 1 d . . . C28 C 0.1105(2) 0.02301(15) 0.11670(15) 0.0239(6) Uani 1 1 d . . . H28A H 0.1542 0.0623 0.0916 0.029 Uiso 1 1 calc R . . C29 C 0.0110(2) 0.01654(17) 0.09765(16) 0.0306(7) Uani 1 1 d . . . H29A H -0.0131 0.0517 0.0600 0.037 Uiso 1 1 calc R . . C110 C 0.4967(2) 0.30162(16) 0.11846(16) 0.0281(7) Uani 1 1 d . . . H11A H 0.5384 0.2645 0.1043 0.034 Uiso 1 1 calc R . . C111 C 0.4987(2) 0.36920(16) 0.07396(15) 0.0256(6) Uani 1 1 d . . . H11B H 0.5420 0.3785 0.0294 0.031 Uiso 1 1 calc R . . C112 C 0.4376(2) 0.42361(15) 0.09403(14) 0.0208(6) Uani 1 1 d . . . H11C H 0.4384 0.4701 0.0631 0.025 Uiso 1 1 calc R . . C113 C 0.3618(2) 0.56179(13) 0.14637(13) 0.0152(5) Uani 1 1 d . . . C114 C 0.3179(2) 0.61679(14) 0.09717(13) 0.0197(6) Uani 1 1 d . . . H11D H 0.2653 0.6080 0.0746 0.024 Uiso 1 1 calc R . . C115 C 0.3502(2) 0.68432(15) 0.08085(14) 0.0240(6) Uani 1 1 d . . . H11E H 0.3230 0.7216 0.0457 0.029 Uiso 1 1 calc R . . C116 C 0.4224(2) 0.69679(14) 0.11633(14) 0.0242(6) Uani 1 1 d . . . H11F H 0.4391 0.7435 0.1087 0.029 Uiso 1 1 calc R . . C117 C 0.4707(2) 0.64181(14) 0.16280(14) 0.0211(6) Uani 1 1 d . . . H11G H 0.5218 0.6518 0.1855 0.025 Uiso 1 1 calc R . . C118 C 0.4475(2) 0.57187(13) 0.17779(13) 0.0159(5) Uani 1 1 d . . . C120 C 0.6436(2) 0.39249(14) 0.21036(14) 0.0181(6) Uani 1 1 d . . . C121 C 0.7151(2) 0.35213(15) 0.17494(15) 0.0227(6) Uani 1 1 d . . . H12B H 0.7343 0.3046 0.1985 0.027 Uiso 1 1 calc R . . C122 C 0.7592(2) 0.37923(16) 0.10618(15) 0.0250(6) Uani 1 1 d . . . C123 C 0.7338(2) 0.44938(15) 0.07486(14) 0.0226(6) Uani 1 1 d . . . H12C H 0.7651 0.4697 0.0283 0.027 Uiso 1 1 calc R . . C124 C 0.6637(2) 0.49200(14) 0.10878(14) 0.0191(6) Uani 1 1 d . . . C119 C 0.61222(19) 0.46348(14) 0.17766(13) 0.0159(5) Uani 1 1 d . . . C125 C 0.6012(2) 0.35700(14) 0.28490(14) 0.0230(6) Uani 1 1 d . . . H12D H 0.6405 0.3105 0.2994 0.034 Uiso 1 1 calc R . . H12E H 0.5196 0.3521 0.2931 0.034 Uiso 1 1 calc R . . H12F H 0.6161 0.3854 0.3106 0.034 Uiso 1 1 calc R . . C126 C 0.8308(3) 0.33400(18) 0.06748(17) 0.0364(8) Uani 1 1 d . . . H12G H 0.8747 0.3638 0.0255 0.055 Uiso 1 1 calc R . . H12H H 0.7818 0.3066 0.0566 0.055 Uiso 1 1 calc R . . H12I H 0.8826 0.3021 0.0951 0.055 Uiso 1 1 calc R . . C127 C 0.6505(2) 0.56886(15) 0.06824(14) 0.0244(6) Uani 1 1 d . . . H12J H 0.6711 0.5973 0.0921 0.037 Uiso 1 1 calc R . . H12K H 0.5716 0.5812 0.0626 0.037 Uiso 1 1 calc R . . H12L H 0.7001 0.5778 0.0237 0.037 Uiso 1 1 calc R . . C128 C 0.5183(2) 0.53123(13) 0.33636(13) 0.0150(5) Uani 1 1 d . . . C129 C 0.5612(2) 0.56231(14) 0.37449(14) 0.0184(6) Uani 1 1 d . . . H12M H 0.5195 0.5627 0.4176 0.022 Uiso 1 1 calc R . . C130 C 0.6648(2) 0.59255(14) 0.34910(14) 0.0192(6) Uani 1 1 d . . . H13B H 0.6935 0.6147 0.3741 0.023 Uiso 1 1 calc R . . C131 C 0.7260(2) 0.59016(14) 0.28688(14) 0.0205(6) Uani 1 1 d . . . H13C H 0.7976 0.6098 0.2697 0.025 Uiso 1 1 calc R . . C132 C 0.6833(2) 0.55922(14) 0.24947(14) 0.0194(6) Uani 1 1 d . . . H13D H 0.7274 0.5573 0.2074 0.023 Uiso 1 1 calc R . . C133 C 0.5764(2) 0.53062(13) 0.27221(13) 0.0160(5) Uani 1 1 d . . . C134 C 0.4113(2) 0.40560(13) 0.43142(13) 0.0162(5) Uani 1 1 d . . . C135 C 0.5112(2) 0.38825(14) 0.45611(15) 0.0236(6) Uani 1 1 d . . . H13E H 0.5683 0.4209 0.4399 0.028 Uiso 1 1 calc R . . C136 C 0.5287(3) 0.32418(16) 0.50391(16) 0.0308(7) Uani 1 1 d . . . H13F H 0.5980 0.3129 0.5199 0.037 Uiso 1 1 calc R . . C137 C 0.4455(2) 0.27599(15) 0.52889(15) 0.0252(6) Uani 1 1 d . . . H13G H 0.4571 0.2321 0.5623 0.030 Uiso 1 1 calc R . . C138 C 0.3460(2) 0.29282(14) 0.50448(15) 0.0256(6) Uani 1 1 d . . . H13H H 0.2886 0.2603 0.5213 0.031 Uiso 1 1 calc R . . C139 C 0.3290(2) 0.35606(14) 0.45618(15) 0.0222(6) Uani 1 1 d . . . H13I H 0.2606 0.3664 0.4393 0.027 Uiso 1 1 calc R . . C140 C 0.30410(19) 0.54358(13) 0.42022(13) 0.0150(5) Uani 1 1 d . . . C141 C 0.2850(2) 0.61482(14) 0.38648(14) 0.0183(6) Uani 1 1 d . . . H14B H 0.3115 0.6332 0.3390 0.022 Uiso 1 1 calc R . . C142 C 0.2278(2) 0.65881(14) 0.42157(15) 0.0234(6) Uani 1 1 d . . . H14C H 0.2157 0.7074 0.3983 0.028 Uiso 1 1 calc R . . C143 C 0.1878(2) 0.63229(15) 0.49092(15) 0.0241(6) Uani 1 1 d . . . H14D H 0.1476 0.6625 0.5150 0.029 Uiso 1 1 calc R . . C144 C 0.2070(2) 0.56181(15) 0.52452(15) 0.0236(6) Uani 1 1 d . . . H14E H 0.1804 0.5436 0.5720 0.028 Uiso 1 1 calc R . . C145 C 0.2649(2) 0.51735(14) 0.48955(14) 0.0187(6) Uani 1 1 d . . . H14F H 0.2777 0.4689 0.5131 0.022 Uiso 1 1 calc R . . C146 C 0.0772(2) 0.57619(13) 0.32648(14) 0.0176(6) Uani 1 1 d . . . C147 C -0.0156(2) 0.58833(15) 0.37423(16) 0.0245(6) Uani 1 1 d . . . H14G H -0.0457 0.5498 0.4114 0.029 Uiso 1 1 calc R . . C148 C -0.0644(2) 0.65481(16) 0.36866(18) 0.0322(7) Uani 1 1 d . . . H14H H -0.1274 0.6616 0.4018 0.039 Uiso 1 1 calc R . . C149 C -0.0220(3) 0.71171(16) 0.31506(18) 0.0341(8) Uani 1 1 d . . . H14I H -0.0562 0.7575 0.3110 0.041 Uiso 1 1 calc R . . C150 C 0.0703(3) 0.70169(15) 0.26742(16) 0.0283(7) Uani 1 1 d . . . H15B H 0.1002 0.7407 0.2307 0.034 Uiso 1 1 calc R . . C151 C 0.1194(2) 0.63458(14) 0.27325(14) 0.0205(6) Uani 1 1 d . . . H15C H 0.1830 0.6283 0.2403 0.025 Uiso 1 1 calc R . . C152 C 0.0522(2) 0.42560(13) 0.32525(13) 0.0160(5) Uani 1 1 d . . . C153 C 0.0846(2) 0.35458(14) 0.33872(15) 0.0224(6) Uani 1 1 d . . . H15D H 0.1529 0.3369 0.3550 0.027 Uiso 1 1 calc R . . C154 C 0.0197(2) 0.30863(15) 0.32900(17) 0.0295(7) Uani 1 1 d . . . H15E H 0.0432 0.2602 0.3392 0.035 Uiso 1 1 calc R . . C155 C -0.0793(2) 0.33417(16) 0.30440(17) 0.0304(7) Uani 1 1 d . . . H15F H -0.1236 0.3033 0.2972 0.037 Uiso 1 1 calc R . . C156 C -0.1133(2) 0.40423(16) 0.29044(16) 0.0268(7) Uani 1 1 d . . . H15G H -0.1810 0.4218 0.2733 0.032 Uiso 1 1 calc R . . C157 C -0.0486(2) 0.44935(14) 0.30137(14) 0.0197(6) Uani 1 1 d . . . H15H H -0.0738 0.4974 0.2923 0.024 Uiso 1 1 calc R . . C210 C -0.0525(2) -0.04070(17) 0.13326(17) 0.0316(7) Uani 1 1 d . . . H21A H -0.1195 -0.0454 0.1197 0.038 Uiso 1 1 calc R . . C211 C -0.0186(2) -0.09075(16) 0.18835(16) 0.0279(7) Uani 1 1 d . . . H21B H -0.0622 -0.1303 0.2127 0.033 Uiso 1 1 calc R . . C212 C 0.0789(2) -0.08420(14) 0.20893(15) 0.0211(6) Uani 1 1 d . . . H21C H 0.1002 -0.1183 0.2481 0.025 Uiso 1 1 calc R . . C213 C 0.3585(2) -0.10230(13) 0.21082(13) 0.0164(5) Uani 1 1 d . . . C214 C 0.3192(2) -0.16102(14) 0.20499(14) 0.0191(6) Uani 1 1 d . . . H21D H 0.2618 -0.1551 0.1795 0.023 Uiso 1 1 calc R . . C215 C 0.3633(2) -0.22759(15) 0.23602(15) 0.0230(6) Uani 1 1 d . . . H21E H 0.3367 -0.2673 0.2315 0.028 Uiso 1 1 calc R . . C216 C 0.4463(2) -0.23643(15) 0.27376(15) 0.0242(6) Uani 1 1 d . . . H21F H 0.4740 -0.2822 0.2971 0.029 Uiso 1 1 calc R . . C217 C 0.4887(2) -0.17803(14) 0.27726(15) 0.0219(6) Uani 1 1 d . . . H21G H 0.5468 -0.1849 0.3025 0.026 Uiso 1 1 calc R . . C218 C 0.4492(2) -0.10941(14) 0.24510(13) 0.0174(5) Uani 1 1 d . . . C219 C 0.5922(2) -0.00215(14) 0.16978(14) 0.0171(5) Uani 1 1 d . . . C220 C 0.6429(2) -0.03285(15) 0.11931(14) 0.0204(6) Uani 1 1 d . . . C221 C 0.7043(2) 0.00710(16) 0.05755(14) 0.0245(6) Uani 1 1 d . . . H22B H 0.7355 -0.0145 0.0240 0.029 Uiso 1 1 calc R . . C222 C 0.7211(2) 0.07696(16) 0.04365(15) 0.0250(6) Uani 1 1 d . . . C223 C 0.6784(2) 0.10613(15) 0.09435(14) 0.0230(6) Uani 1 1 d . . . H22C H 0.6926 0.1533 0.0869 0.028 Uiso 1 1 calc R . . C224 C 0.6148(2) 0.06823(14) 0.15654(14) 0.0184(6) Uani 1 1 d . . . C225 C 0.6406(2) -0.11007(16) 0.12895(16) 0.0285(7) Uani 1 1 d . . . H22D H 0.6893 -0.1209 0.0901 0.043 Uiso 1 1 calc R . . H22E H 0.5628 -0.1211 0.1326 0.043 Uiso 1 1 calc R . . H22F H 0.6681 -0.1382 0.1704 0.043 Uiso 1 1 calc R . . C226 C 0.7821(3) 0.11982(18) -0.02495(16) 0.0380(8) Uani 1 1 d . . . H22G H 0.8355 0.0890 -0.0455 0.057 Uiso 1 1 calc R . . H22H H 0.8234 0.1553 -0.0198 0.057 Uiso 1 1 calc R . . H22I H 0.7269 0.1431 -0.0540 0.057 Uiso 1 1 calc R . . C227 C 0.5719(2) 0.10549(14) 0.20826(14) 0.0207(6) Uani 1 1 d . . . H22J H 0.5897 0.0758 0.2520 0.031 Uiso 1 1 calc R . . H22K H 0.4897 0.1150 0.2127 0.031 Uiso 1 1 calc R . . H22L H 0.6084 0.1498 0.1936 0.031 Uiso 1 1 calc R . . C228 C 0.5760(2) -0.06134(13) 0.30516(14) 0.0167(5) Uani 1 1 d . . . C229 C 0.6901(2) -0.08756(14) 0.29958(14) 0.0202(6) Uani 1 1 d . . . H22M H 0.7312 -0.0895 0.2569 0.024 Uiso 1 1 calc R . . C230 C 0.7444(2) -0.11069(14) 0.35456(14) 0.0204(6) Uani 1 1 d . . . H23B H 0.8214 -0.1280 0.3490 0.024 Uiso 1 1 calc R . . C231 C 0.6868(2) -0.10861(13) 0.41732(14) 0.0198(6) Uani 1 1 d . . . H23C H 0.7236 -0.1249 0.4551 0.024 Uiso 1 1 calc R . . C232 C 0.5747(2) -0.08245(13) 0.42471(14) 0.0183(6) Uani 1 1 d . . . H23D H 0.5344 -0.0808 0.4677 0.022 Uiso 1 1 calc R . . C233 C 0.5210(2) -0.05859(13) 0.36909(13) 0.0157(5) Uani 1 1 d . . . C234 C 0.3953(2) 0.07034(14) 0.37662(13) 0.0190(6) Uani 1 1 d . . . C235 C 0.3163(2) 0.12436(15) 0.35469(17) 0.0296(7) Uani 1 1 d . . . H23E H 0.2545 0.1154 0.3389 0.036 Uiso 1 1 calc R . . C236 C 0.3256(3) 0.19108(16) 0.35526(19) 0.0389(9) Uani 1 1 d . . . H23F H 0.2695 0.2273 0.3409 0.047 Uiso 1 1 calc R . . C237 C 0.4169(3) 0.20545(15) 0.37679(15) 0.0323(7) Uani 1 1 d . . . H23G H 0.4222 0.2509 0.3787 0.039 Uiso 1 1 calc R . . C238 C 0.4989(3) 0.15330(16) 0.39519(16) 0.0356(8) Uani 1 1 d . . . H23H H 0.5634 0.1632 0.4078 0.043 Uiso 1 1 calc R . . C239 C 0.4882(3) 0.08594(15) 0.39548(16) 0.0312(7) Uani 1 1 d . . . H23I H 0.5453 0.0501 0.4088 0.037 Uiso 1 1 calc R . . C240 C 0.3092(2) -0.06546(14) 0.46221(14) 0.0182(6) Uani 1 1 d . . . C241 C 0.2700(2) -0.03480(15) 0.51222(14) 0.0246(6) Uani 1 1 d . . . H24B H 0.2813 0.0131 0.5033 0.030 Uiso 1 1 calc R . . C242 C 0.2142(3) -0.07418(18) 0.57555(16) 0.0345(7) Uani 1 1 d . . . H24C H 0.1884 -0.0532 0.6101 0.041 Uiso 1 1 calc R . . C243 C 0.1962(3) -0.14346(18) 0.58840(16) 0.0364(8) Uani 1 1 d . . . H24D H 0.1570 -0.1699 0.6315 0.044 Uiso 1 1 calc R . . C244 C 0.2351(2) -0.17442(16) 0.53882(16) 0.0293(7) Uani 1 1 d . . . H24E H 0.2231 -0.2223 0.5480 0.035 Uiso 1 1 calc R . . C245 C 0.2913(2) -0.13600(15) 0.47578(15) 0.0227(6) Uani 1 1 d . . . H24F H 0.3178 -0.1575 0.4417 0.027 Uiso 1 1 calc R . . C246 C 0.0333(2) 0.05702(14) 0.29203(14) 0.0189(6) Uani 1 1 d . . . C247 C 0.0454(2) 0.12905(15) 0.26356(15) 0.0249(6) Uani 1 1 d . . . H24G H 0.1050 0.1485 0.2722 0.030 Uiso 1 1 calc R . . C248 C -0.0266(3) 0.17297(16) 0.22324(17) 0.0344(7) Uani 1 1 d . . . H24H H -0.0160 0.2218 0.2045 0.041 Uiso 1 1 calc R . . C249 C -0.1146(2) 0.14583(17) 0.21006(17) 0.0330(7) Uani 1 1 d . . . H24I H -0.1643 0.1759 0.1824 0.040 Uiso 1 1 calc R . . C250 C -0.1291(2) 0.07498(16) 0.23734(16) 0.0288(7) Uani 1 1 d . . . H25B H -0.1886 0.0560 0.2282 0.035 Uiso 1 1 calc R . . C251 C -0.0571(2) 0.03135(15) 0.27803(15) 0.0227(6) Uani 1 1 d . . . H25C H -0.0691 -0.0173 0.2971 0.027 Uiso 1 1 calc R . . C252 C 0.0602(2) -0.08400(13) 0.40313(14) 0.0165(5) Uani 1 1 d . . . C253 C -0.0155(2) -0.08028(15) 0.46157(15) 0.0222(6) Uani 1 1 d . . . H25D H -0.0287 -0.0371 0.4709 0.027 Uiso 1 1 calc R . . C254 C -0.0719(2) -0.13829(16) 0.50653(16) 0.0283(7) Uani 1 1 d . . . H25E H -0.1213 -0.1349 0.5467 0.034 Uiso 1 1 calc R . . C255 C -0.0560(2) -0.20087(15) 0.49278(15) 0.0264(7) Uani 1 1 d . . . H25F H -0.0959 -0.2403 0.5228 0.032 Uiso 1 1 calc R . . C256 C 0.0177(2) -0.20591(15) 0.43547(15) 0.0247(6) Uani 1 1 d . . . H25G H 0.0284 -0.2488 0.4257 0.030 Uiso 1 1 calc R . . C257 C 0.0771(2) -0.14816(14) 0.39149(15) 0.0218(6) Uani 1 1 d . . . H25H H 0.1299 -0.1528 0.3529 0.026 Uiso 1 1 calc R . . C1S C -0.1063(5) 0.7633(3) -0.0002(5) 0.111(2) Uani 1 1 d . . . H1SA H -0.0989 0.7722 -0.0474 0.133 Uiso 1 1 calc R . . C2S C -0.1972(7) 0.7357(3) 0.0481(4) 0.114(3) Uani 1 1 d . . . H2SA H -0.2565 0.7207 0.0349 0.137 Uiso 1 1 calc R . . C3S C -0.2067(4) 0.7284(3) 0.1183(3) 0.0859(17) Uani 1 1 d . . . H3SA H -0.2740 0.7101 0.1482 0.103 Uiso 1 1 calc R . . C4S C -0.1279(4) 0.7453(2) 0.1459(3) 0.0719(14) Uani 1 1 d . . . H4S H -0.1356 0.7407 0.1923 0.086 Uiso 1 1 calc R . . C5S C -0.0323(5) 0.7711(4) 0.0943(3) 0.108(2) Uani 1 1 d . . . H5SA H 0.0304 0.7852 0.1053 0.129 Uiso 1 1 calc R . . C6S C -0.0313(6) 0.7755(3) 0.0288(3) 0.0909(17) Uani 1 1 d . . . H6SA H 0.0377 0.7904 -0.0013 0.109 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 Ni1 0.00692(15) 0.01693(17) 0.01411(18) -0.00491(13) -0.00042(12) -0.00496(12) Ni2 0.00846(15) 0.01844(17) 0.01602(18) -0.00549(14) -0.00107(12) -0.00328(12) P11 0.0088(3) 0.0189(3) 0.0148(3) -0.0054(3) -0.0009(2) -0.0054(2) P12 0.0088(3) 0.0158(3) 0.0133(3) -0.0038(3) -0.0006(2) -0.0053(2) P21 0.0100(3) 0.0181(3) 0.0178(4) -0.0063(3) -0.0023(3) -0.0030(2) P22 0.0125(3) 0.0167(3) 0.0160(4) -0.0057(3) -0.0015(3) -0.0027(2) Si1 0.0080(3) 0.0170(3) 0.0168(4) -0.0055(3) 0.0001(3) -0.0050(3) Si2 0.0096(3) 0.0190(4) 0.0186(4) -0.0057(3) -0.0001(3) -0.0035(3) B1 0.0077(13) 0.0235(16) 0.0173(16) -0.0054(12) 0.0026(11) -0.0096(11) B2 0.0101(13) 0.0198(15) 0.0180(16) -0.0060(12) 0.0001(11) -0.0039(11) C11 0.0096(12) 0.0292(15) 0.0166(14) -0.0044(11) -0.0015(10) -0.0079(10) C12 0.0203(14) 0.0310(16) 0.0370(18) -0.0137(14) -0.0078(13) -0.0063(12) C13 0.0260(16) 0.047(2) 0.056(2) -0.0236(18) -0.0181(16) -0.0104(14) C14 0.0171(14) 0.052(2) 0.046(2) -0.0151(17) -0.0149(14) -0.0065(14) C15 0.0130(13) 0.0388(18) 0.0354(18) -0.0106(14) -0.0028(12) -0.0025(12) C16 0.0125(12) 0.0319(16) 0.0216(15) -0.0096(12) -0.0009(11) -0.0046(11) C17 0.0098(11) 0.0232(14) 0.0232(15) -0.0110(12) -0.0035(10) -0.0038(10) C18 0.0181(13) 0.0254(15) 0.0219(15) -0.0085(12) 0.0013(11) -0.0063(11) C19 0.0296(16) 0.0241(15) 0.0363(19) -0.0115(14) -0.0040(14) -0.0036(12) C21 0.0108(12) 0.0250(14) 0.0208(15) -0.0036(12) -0.0064(11) -0.0055(10) C22 0.0224(14) 0.0270(15) 0.0243(16) -0.0046(13) -0.0046(12) -0.0070(12) C23 0.0307(16) 0.0287(17) 0.040(2) -0.0025(14) -0.0126(15) -0.0118(13) C24 0.0232(16) 0.044(2) 0.0329(19) 0.0088(15) -0.0078(14) -0.0151(14) C25 0.0179(14) 0.061(2) 0.0189(16) -0.0012(15) -0.0015(12) -0.0070(14) C26 0.0165(13) 0.0398(17) 0.0217(16) -0.0092(13) -0.0060(12) -0.0018(12) C27 0.0088(12) 0.0256(14) 0.0234(15) -0.0105(12) -0.0030(11) -0.0022(10) C28 0.0155(13) 0.0282(15) 0.0274(16) -0.0070(13) -0.0051(12) -0.0029(11) C29 0.0192(14) 0.0377(18) 0.0337(18) -0.0058(14) -0.0122(13) -0.0009(12) C110 0.0191(14) 0.0334(17) 0.0398(19) -0.0233(15) -0.0052(13) 0.0015(12) C111 0.0163(13) 0.0406(18) 0.0243(16) -0.0176(14) -0.0003(12) -0.0045(12) C112 0.0154(13) 0.0299(15) 0.0196(15) -0.0101(12) -0.0031(11) -0.0047(11) C113 0.0094(11) 0.0213(13) 0.0143(13) -0.0073(11) 0.0033(10) -0.0040(10) C114 0.0139(12) 0.0267(15) 0.0156(14) -0.0047(11) 0.0007(10) -0.0037(11) C115 0.0253(14) 0.0218(14) 0.0183(15) -0.0017(12) 0.0003(12) 0.0000(11) C116 0.0297(15) 0.0196(14) 0.0192(15) -0.0053(12) 0.0059(12) -0.0080(11) C117 0.0188(13) 0.0233(14) 0.0221(15) -0.0091(12) 0.0023(11) -0.0094(11) C118 0.0101(11) 0.0217(14) 0.0154(14) -0.0070(11) 0.0028(10) -0.0048(10) C120 0.0096(12) 0.0262(14) 0.0212(15) -0.0091(12) -0.0025(10) -0.0069(10) C121 0.0149(13) 0.0255(15) 0.0293(16) -0.0101(13) -0.0042(11) -0.0038(11) C122 0.0155(13) 0.0367(17) 0.0282(17) -0.0183(14) -0.0001(12) -0.0059(12) C123 0.0143(13) 0.0369(17) 0.0188(15) -0.0111(13) 0.0010(11) -0.0107(11) C124 0.0082(11) 0.0314(15) 0.0201(15) -0.0101(12) -0.0007(10) -0.0076(10) C119 0.0068(11) 0.0235(14) 0.0195(14) -0.0076(11) -0.0022(10) -0.0065(10) C125 0.0189(13) 0.0212(14) 0.0256(16) -0.0036(12) -0.0023(12) -0.0045(11) C126 0.0331(17) 0.0425(19) 0.037(2) -0.0221(16) -0.0012(15) -0.0006(14) C127 0.0171(13) 0.0332(16) 0.0190(15) -0.0061(12) 0.0041(11) -0.0077(11) C128 0.0101(11) 0.0169(13) 0.0168(14) -0.0025(10) -0.0016(10) -0.0059(9) C129 0.0155(12) 0.0229(14) 0.0173(14) -0.0057(11) -0.0026(11) -0.0063(10) C130 0.0164(13) 0.0215(14) 0.0224(15) -0.0049(12) -0.0082(11) -0.0085(10) C131 0.0116(12) 0.0221(14) 0.0262(16) -0.0016(12) -0.0048(11) -0.0096(10) C132 0.0104(12) 0.0274(15) 0.0203(15) -0.0067(12) -0.0006(10) -0.0081(10) C133 0.0112(12) 0.0157(13) 0.0195(14) -0.0026(11) -0.0028(10) -0.0042(10) C134 0.0142(12) 0.0180(13) 0.0173(14) -0.0071(11) -0.0011(10) -0.0043(10) C135 0.0211(14) 0.0216(14) 0.0279(16) -0.0026(12) -0.0087(12) -0.0083(11) C136 0.0280(16) 0.0285(16) 0.0378(19) -0.0033(14) -0.0205(14) -0.0038(12) C137 0.0314(16) 0.0184(14) 0.0251(16) -0.0033(12) -0.0098(13) -0.0017(12) C138 0.0219(14) 0.0175(14) 0.0338(17) -0.0018(12) -0.0044(12) -0.0083(11) C139 0.0161(13) 0.0210(14) 0.0291(16) -0.0034(12) -0.0081(12) -0.0062(11) C140 0.0082(11) 0.0201(13) 0.0187(14) -0.0065(11) -0.0022(10) -0.0071(9) C141 0.0138(12) 0.0221(14) 0.0193(14) -0.0050(11) -0.0029(10) -0.0070(10) C142 0.0199(13) 0.0187(14) 0.0339(17) -0.0094(12) -0.0069(12) -0.0037(11) C143 0.0164(13) 0.0292(16) 0.0323(17) -0.0176(13) -0.0013(12) -0.0054(11) C144 0.0192(13) 0.0323(16) 0.0202(15) -0.0105(13) 0.0023(11) -0.0100(12) C145 0.0160(13) 0.0195(13) 0.0200(14) -0.0053(11) -0.0007(11) -0.0068(10) C146 0.0114(12) 0.0201(13) 0.0255(15) -0.0110(12) -0.0042(11) -0.0042(10) C147 0.0148(13) 0.0277(15) 0.0351(18) -0.0161(13) 0.0015(12) -0.0101(11) C148 0.0161(14) 0.0384(18) 0.052(2) -0.0303(17) -0.0034(14) -0.0005(12) C149 0.0313(17) 0.0254(16) 0.055(2) -0.0206(16) -0.0187(16) 0.0053(13) C150 0.0314(16) 0.0226(15) 0.0341(18) -0.0076(13) -0.0143(14) -0.0037(12) C151 0.0161(13) 0.0250(14) 0.0230(15) -0.0094(12) -0.0051(11) -0.0036(11) C152 0.0099(11) 0.0203(13) 0.0173(14) -0.0066(11) 0.0035(10) -0.0083(10) C153 0.0152(13) 0.0236(14) 0.0288(16) -0.0063(12) -0.0062(11) -0.0049(11) C154 0.0283(15) 0.0193(14) 0.043(2) -0.0082(13) -0.0097(14) -0.0077(12) C155 0.0246(15) 0.0293(16) 0.043(2) -0.0130(14) -0.0088(14) -0.0142(12) C156 0.0154(13) 0.0329(16) 0.0342(18) -0.0094(14) -0.0073(12) -0.0077(12) C157 0.0114(12) 0.0212(14) 0.0247(15) -0.0059(12) 0.0002(11) -0.0052(10) C210 0.0127(13) 0.0426(19) 0.044(2) -0.0146(16) -0.0113(13) -0.0043(12) C211 0.0137(13) 0.0355(17) 0.0360(18) -0.0133(14) -0.0012(12) -0.0083(12) C212 0.0131(12) 0.0248(14) 0.0260(16) -0.0091(12) -0.0028(11) -0.0021(10) C213 0.0130(12) 0.0183(13) 0.0178(14) -0.0066(11) -0.0001(10) -0.0032(10) C214 0.0130(12) 0.0245(14) 0.0223(15) -0.0109(12) -0.0018(11) -0.0036(10) C215 0.0207(14) 0.0234(14) 0.0270(16) -0.0113(12) -0.0001(12) -0.0075(11) C216 0.0217(14) 0.0196(14) 0.0286(17) -0.0047(12) -0.0042(12) -0.0017(11) C217 0.0164(13) 0.0229(14) 0.0272(16) -0.0068(12) -0.0066(11) -0.0032(11) C218 0.0111(12) 0.0223(14) 0.0190(14) -0.0079(11) 0.0005(10) -0.0038(10) C219 0.0066(11) 0.0234(14) 0.0208(15) -0.0054(11) -0.0038(10) -0.0019(10) C220 0.0089(12) 0.0311(15) 0.0216(15) -0.0092(12) -0.0047(11) 0.0016(10) C221 0.0125(13) 0.0403(17) 0.0204(15) -0.0124(13) -0.0028(11) 0.0058(12) C222 0.0113(12) 0.0357(17) 0.0213(16) -0.0037(13) -0.0004(11) 0.0012(11) C223 0.0128(12) 0.0261(15) 0.0254(16) -0.0021(12) -0.0031(11) -0.0032(11) C224 0.0095(12) 0.0249(14) 0.0191(14) -0.0046(11) -0.0032(10) -0.0017(10) C225 0.0239(15) 0.0340(17) 0.0308(17) -0.0183(14) 0.0004(13) -0.0009(12) C226 0.0311(17) 0.045(2) 0.0240(18) -0.0012(15) 0.0052(14) -0.0017(14) C227 0.0154(13) 0.0200(14) 0.0257(16) -0.0057(12) -0.0003(11) -0.0075(10) C228 0.0115(12) 0.0146(12) 0.0235(15) -0.0048(11) -0.0023(10) -0.0043(9) C229 0.0120(12) 0.0249(14) 0.0227(15) -0.0067(12) -0.0012(11) -0.0043(10) C230 0.0107(12) 0.0198(14) 0.0305(16) -0.0058(12) -0.0054(11) -0.0039(10) C231 0.0196(13) 0.0158(13) 0.0256(16) -0.0038(11) -0.0104(12) -0.0044(10) C232 0.0195(13) 0.0180(13) 0.0187(14) -0.0060(11) -0.0046(11) -0.0035(10) C233 0.0115(12) 0.0148(12) 0.0211(14) -0.0050(11) -0.0023(10) -0.0048(9) C234 0.0205(13) 0.0194(13) 0.0159(14) -0.0057(11) 0.0012(11) -0.0047(11) C235 0.0149(13) 0.0216(15) 0.045(2) -0.0054(14) 0.0033(13) -0.0068(11) C236 0.0220(15) 0.0208(15) 0.059(2) -0.0047(15) 0.0125(15) -0.0053(12) C237 0.0457(19) 0.0209(15) 0.0255(17) -0.0091(13) 0.0130(14) -0.0155(14) C238 0.056(2) 0.0257(16) 0.0310(18) -0.0066(14) -0.0180(16) -0.0146(15) C239 0.0457(19) 0.0226(15) 0.0320(18) -0.0086(13) -0.0213(15) -0.0022(13) C240 0.0101(12) 0.0237(14) 0.0189(14) -0.0040(11) -0.0032(10) -0.0018(10) C241 0.0246(14) 0.0273(15) 0.0204(15) -0.0080(12) -0.0024(12) 0.0010(12) C242 0.0355(17) 0.0426(19) 0.0190(16) -0.0091(14) 0.0022(13) 0.0041(14) C243 0.0274(16) 0.044(2) 0.0237(17) 0.0017(15) 0.0043(13) -0.0050(14) C244 0.0269(15) 0.0272(16) 0.0289(17) 0.0012(13) -0.0069(13) -0.0101(12) C245 0.0191(13) 0.0257(15) 0.0244(16) -0.0079(12) -0.0041(12) -0.0054(11) C246 0.0112(12) 0.0233(14) 0.0196(14) -0.0068(11) 0.0015(10) -0.0005(10) C247 0.0185(14) 0.0245(15) 0.0303(17) -0.0071(13) -0.0044(12) -0.0017(11) C248 0.0323(17) 0.0233(16) 0.039(2) -0.0024(14) -0.0056(14) 0.0032(13) C249 0.0226(15) 0.0377(18) 0.0337(19) -0.0063(15) -0.0093(13) 0.0073(13) C250 0.0150(13) 0.0388(18) 0.0328(18) -0.0129(14) -0.0041(12) 0.0004(12) C251 0.0142(13) 0.0277(15) 0.0250(16) -0.0090(12) 0.0001(11) -0.0024(11) C252 0.0093(11) 0.0206(13) 0.0203(14) -0.0057(11) -0.0051(10) -0.0020(10) C253 0.0156(13) 0.0242(14) 0.0285(16) -0.0117(12) -0.0004(11) -0.0044(11) C254 0.0200(14) 0.0338(17) 0.0272(17) -0.0070(13) 0.0043(12) -0.0103(12) C255 0.0177(13) 0.0273(15) 0.0303(17) -0.0001(13) -0.0059(12) -0.0105(11) C256 0.0235(14) 0.0197(14) 0.0332(17) -0.0067(13) -0.0130(13) -0.0012(11) C257 0.0184(13) 0.0246(15) 0.0229(15) -0.0089(12) -0.0040(11) 0.0002(11) C1S 0.070(4) 0.080(4) 0.199(8) -0.056(5) -0.040(5) -0.004(3) C2S 0.138(6) 0.064(4) 0.159(7) -0.010(4) -0.109(6) 0.000(4) C3S 0.064(3) 0.061(3) 0.127(5) -0.012(3) -0.042(3) 0.009(2) C4S 0.069(3) 0.051(3) 0.094(4) -0.006(3) -0.032(3) -0.022(2) C5S 0.109(5) 0.146(6) 0.083(4) -0.046(4) 0.009(3) -0.084(4) C6S 0.106(5) 0.110(5) 0.072(4) -0.046(4) -0.025(3) -0.001(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 Ni1 P12 2.1556(7) . ? Ni1 P11 2.1869(7) . ? Ni1 Si1 2.2466(7) . ? Ni1 B1 2.498(3) . ? Ni1 H100 1.64(3) . ? Ni2 P22 2.1444(8) . ? Ni2 P21 2.1711(8) . ? Ni2 Si2 2.2491(7) . ? Ni2 B2 2.514(3) . ? Ni2 H200 1.63(3) . ? P11 C17 1.814(3) . ? P11 C113 1.821(3) . ? P11 C11 1.828(3) . ? P12 C140 1.823(3) . ? P12 C128 1.824(2) . ? P12 C134 1.826(3) . ? P21 C21 1.809(3) . ? P21 C213 1.827(3) . ? P21 C27 1.833(3) . ? P22 C240 1.820(3) . ? P22 C233 1.822(3) . ? P22 C234 1.830(3) . ? Si1 C146 1.889(3) . ? Si1 C152 1.894(2) . ? Si1 H101 1.39(3) . ? Si2 C252 1.885(3) . ? Si2 C246 1.888(3) . ? Si2 H201 1.41(3) . ? B1 C118 1.625(4) . ? B1 C133 1.627(4) . ? B1 C119 1.641(4) . ? B1 H100 1.26(3) . ? B2 C228 1.621(4) . ? B2 C218 1.629(4) . ? B2 C219 1.635(4) . ? B2 H200 1.27(3) . ? C11 C12 1.391(4) . ? C11 C16 1.393(4) . ? C12 C13 1.396(4) . ? C12 H12A 0.9500 . ? C13 C14 1.375(5) . ? C13 H13A 0.9500 . ? C14 C15 1.384(4) . ? C14 H14A 0.9500 . ? C15 C16 1.381(4) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.387(4) . ? C17 C112 1.388(4) . ? C18 C19 1.386(4) . ? C18 H18A 0.9500 . ? C19 C110 1.374(4) . ? C19 H19A 0.9500 . ? C21 C26 1.387(4) . ? C21 C22 1.390(4) . ? C22 C23 1.385(4) . ? C22 H22A 0.9500 . ? C23 C24 1.381(5) . ? C23 H23A 0.9500 . ? C24 C25 1.371(5) . ? C24 H24A 0.9500 . ? C25 C26 1.391(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.382(4) . ? C27 C212 1.402(4) . ? C28 C29 1.394(4) . ? C28 H28A 0.9500 . ? C29 C210 1.380(4) . ? C29 H29A 0.9500 . ? C110 C111 1.378(4) . ? C110 H11A 0.9500 . ? C111 C112 1.385(4) . ? C111 H11B 0.9500 . ? C112 H11C 0.9500 . ? C113 C114 1.389(4) . ? C113 C118 1.430(4) . ? C114 C115 1.385(4) . ? C114 H11D 0.9500 . ? C115 C116 1.380(4) . ? C115 H11E 0.9500 . ? C116 C117 1.381(4) . ? C116 H11F 0.9500 . ? C117 C118 1.400(4) . ? C117 H11G 0.9500 . ? C120 C121 1.393(4) . ? C120 C119 1.413(4) . ? C120 C125 1.510(4) . ? C121 C122 1.390(4) . ? C121 H12B 0.9500 . ? C122 C123 1.378(4) . ? C122 C126 1.507(4) . ? C123 C124 1.399(4) . ? C123 H12C 0.9500 . ? C124 C119 1.416(4) . ? C124 C127 1.512(4) . ? C125 H12D 0.9800 . ? C125 H12E 0.9800 . ? C125 H12F 0.9800 . ? C126 H12G 0.9800 . ? C126 H12H 0.9800 . ? C126 H12I 0.9800 . ? C127 H12J 0.9800 . ? C127 H12K 0.9800 . ? C127 H12L 0.9800 . ? C128 C133 1.401(4) . ? C128 C129 1.405(4) . ? C129 C130 1.390(3) . ? C129 H12M 0.9500 . ? C130 C131 1.386(4) . ? C130 H13B 0.9500 . ? C131 C132 1.388(4) . ? C131 H13C 0.9500 . ? C132 C133 1.411(3) . ? C132 H13D 0.9500 . ? C134 C135 1.386(4) . ? C134 C139 1.401(3) . ? C135 C136 1.379(4) . ? C135 H13E 0.9500 . ? C136 C137 1.391(4) . ? C136 H13F 0.9500 . ? C137 C138 1.379(4) . ? C137 H13G 0.9500 . ? C138 C139 1.371(4) . ? C138 H13H 0.9500 . ? C139 H13I 0.9500 . ? C140 C145 1.389(4) . ? C140 C141 1.393(4) . ? C141 C142 1.380(4) . ? C141 H14B 0.9500 . ? C142 C143 1.391(4) . ? C142 H14C 0.9500 . ? C143 C144 1.380(4) . ? C143 H14D 0.9500 . ? C144 C145 1.388(4) . ? C144 H14E 0.9500 . ? C145 H14F 0.9500 . ? C146 C151 1.396(4) . ? C146 C147 1.399(4) . ? C147 C148 1.377(4) . ? C147 H14G 0.9500 . ? C148 C149 1.382(5) . ? C148 H14H 0.9500 . ? C149 C150 1.381(5) . ? C149 H14I 0.9500 . ? C150 C151 1.389(4) . ? C150 H15B 0.9500 . ? C151 H15C 0.9500 . ? C152 C153 1.391(4) . ? C152 C157 1.395(4) . ? C153 C154 1.394(4) . ? C153 H15D 0.9500 . ? C154 C155 1.386(4) . ? C154 H15E 0.9500 . ? C155 C156 1.376(4) . ? C155 H15F 0.9500 . ? C156 C157 1.393(4) . ? C156 H15G 0.9500 . ? C157 H15H 0.9500 . ? C210 C211 1.372(4) . ? C210 H21A 0.9500 . ? C211 C212 1.390(4) . ? C211 H21B 0.9500 . ? C212 H21C 0.9500 . ? C213 C214 1.397(3) . ? C213 C218 1.422(4) . ? C214 C215 1.381(4) . ? C214 H21D 0.9500 . ? C215 C216 1.386(4) . ? C215 H21E 0.9500 . ? C216 C217 1.388(4) . ? C216 H21F 0.9500 . ? C217 C218 1.400(4) . ? C217 H21G 0.9500 . ? C219 C224 1.413(4) . ? C219 C220 1.413(4) . ? C220 C221 1.398(4) . ? C220 C225 1.515(4) . ? C221 C222 1.382(4) . ? C221 H22B 0.9500 . ? C222 C223 1.381(4) . ? C222 C226 1.510(4) . ? C223 C224 1.401(4) . ? C223 H22C 0.9500 . ? C224 C227 1.511(4) . ? C225 H22D 0.9800 . ? C225 H22E 0.9800 . ? C225 H22F 0.9800 . ? C226 H22G 0.9800 . ? C226 H22H 0.9800 . ? C226 H22I 0.9800 . ? C227 H22J 0.9800 . ? C227 H22K 0.9800 . ? C227 H22L 0.9800 . ? C228 C233 1.399(4) . ? C228 C229 1.410(3) . ? C229 C230 1.389(4) . ? C229 H22M 0.9500 . ? C230 C231 1.382(4) . ? C230 H23B 0.9500 . ? C231 C232 1.388(4) . ? C231 H23C 0.9500 . ? C232 C233 1.396(4) . ? C232 H23D 0.9500 . ? C234 C235 1.382(4) . ? C234 C239 1.389(4) . ? C235 C236 1.381(4) . ? C235 H23E 0.9500 . ? C236 C237 1.392(5) . ? C236 H23F 0.9500 . ? C237 C238 1.369(5) . ? C237 H23G 0.9500 . ? C238 C239 1.391(4) . ? C238 H23H 0.9500 . ? C239 H23I 0.9500 . ? C240 C241 1.382(4) . ? C240 C245 1.400(4) . ? C241 C242 1.391(4) . ? C241 H24B 0.9500 . ? C242 C243 1.378(5) . ? C242 H24C 0.9500 . ? C243 C244 1.378(5) . ? C243 H24D 0.9500 . ? C244 C245 1.382(4) . ? C244 H24E 0.9500 . ? C245 H24F 0.9500 . ? C246 C247 1.395(4) . ? C246 C251 1.407(4) . ? C247 C248 1.382(4) . ? C247 H24G 0.9500 . ? C248 C249 1.388(4) . ? C248 H24H 0.9500 . ? C249 C250 1.376(4) . ? C249 H24I 0.9500 . ? C250 C251 1.383(4) . ? C250 H25B 0.9500 . ? C251 H25C 0.9500 . ? C252 C257 1.390(4) . ? C252 C253 1.396(4) . ? C253 C254 1.391(4) . ? C253 H25D 0.9500 . ? C254 C255 1.381(4) . ? C254 H25E 0.9500 . ? C255 C256 1.374(4) . ? C255 H25F 0.9500 . ? C256 C257 1.398(4) . ? C256 H25G 0.9500 . ? C257 H25H 0.9500 . ? C1S C6S 1.304(8) . ? C1S C2S 1.364(10) . ? C1S H1SA 0.9500 . ? C2S C3S 1.439(9) . ? C2S H2SA 0.9500 . ? C3S C4S 1.366(7) . ? C3S H3SA 0.9500 . ? C4S C5S 1.427(7) . ? C4S H4S 0.9500 . ? C5S C6S 1.373(7) . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? 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 P12 Ni1 P11 169.56(3) . . ? P12 Ni1 Si1 90.34(3) . . ? P11 Ni1 Si1 98.91(3) . . ? P12 Ni1 B1 85.60(7) . . ? P11 Ni1 B1 84.28(7) . . ? Si1 Ni1 B1 166.12(7) . . ? P12 Ni1 H100 89.4(9) . . ? P11 Ni1 H100 82.7(9) . . ? Si1 Ni1 H100 167.2(9) . . ? B1 Ni1 H100 26.3(9) . . ? P22 Ni2 P21 168.63(3) . . ? P22 Ni2 Si2 90.95(3) . . ? P21 Ni2 Si2 100.08(3) . . ? P22 Ni2 B2 84.63(7) . . ? P21 Ni2 B2 84.11(7) . . ? Si2 Ni2 B2 172.46(7) . . ? P22 Ni2 H200 85.7(10) . . ? P21 Ni2 H200 84.8(10) . . ? Si2 Ni2 H200 160.0(10) . . ? B2 Ni2 H200 25.8(10) . . ? C17 P11 C113 110.47(11) . . ? C17 P11 C11 103.28(12) . . ? C113 P11 C11 105.74(12) . . ? C17 P11 Ni1 114.58(9) . . ? C113 P11 Ni1 89.65(9) . . ? C11 P11 Ni1 130.86(9) . . ? C140 P12 C128 102.53(11) . . ? C140 P12 C134 104.35(12) . . ? C128 P12 C134 106.16(11) . . ? C140 P12 Ni1 122.48(8) . . ? C128 P12 Ni1 107.56(9) . . ? C134 P12 Ni1 112.36(8) . . ? C21 P21 C213 115.30(12) . . ? C21 P21 C27 102.75(12) . . ? C213 P21 C27 107.57(12) . . ? C21 P21 Ni2 109.10(9) . . ? C213 P21 Ni2 88.90(9) . . ? C27 P21 Ni2 133.19(9) . . ? C240 P22 C233 103.88(12) . . ? C240 P22 C234 106.37(12) . . ? C233 P22 C234 104.33(12) . . ? C240 P22 Ni2 120.53(9) . . ? C233 P22 Ni2 108.59(9) . . ? C234 P22 Ni2 111.74(9) . . ? C146 Si1 C152 111.54(11) . . ? C146 Si1 Ni1 113.77(8) . . ? C152 Si1 Ni1 113.68(8) . . ? C146 Si1 H101 102.4(11) . . ? C152 Si1 H101 103.0(11) . . ? Ni1 Si1 H101 111.2(11) . . ? C252 Si2 C246 108.89(11) . . ? C252 Si2 Ni2 117.73(8) . . ? C246 Si2 Ni2 114.00(8) . . ? C252 Si2 H201 102.2(12) . . ? C246 Si2 H201 102.3(12) . . ? Ni2 Si2 H201 109.9(12) . . ? C118 B1 C133 110.7(2) . . ? C118 B1 C119 115.9(2) . . ? C133 B1 C119 113.8(2) . . ? C118 B1 Ni1 78.49(13) . . ? C133 B1 Ni1 102.83(16) . . ? C119 B1 Ni1 129.91(17) . . ? C118 B1 H100 106.9(12) . . ? C133 B1 H100 110.4(12) . . ? C119 B1 H100 98.2(12) . . ? Ni1 B1 H100 35.1(12) . . ? C228 B2 C218 110.7(2) . . ? C228 B2 C219 112.4(2) . . ? C218 B2 C219 116.9(2) . . ? C228 B2 Ni2 103.32(16) . . ? C218 B2 Ni2 77.82(13) . . ? C219 B2 Ni2 130.70(18) . . ? C228 B2 H200 107.4(13) . . ? C218 B2 H200 107.3(13) . . ? C219 B2 H200 101.1(13) . . ? Ni2 B2 H200 34.0(13) . . ? C12 C11 C16 118.8(2) . . ? C12 C11 P11 121.2(2) . . ? C16 C11 P11 120.0(2) . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C11 121.0(3) . . ? C15 C16 H16A 119.5 . . ? C11 C16 H16A 119.5 . . ? C18 C17 C112 119.5(2) . . ? C18 C17 P11 118.4(2) . . ? C112 C17 P11 122.0(2) . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C110 C19 C18 119.7(3) . . ? C110 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C26 C21 C22 120.1(3) . . ? C26 C21 P21 124.6(2) . . ? C22 C21 P21 115.2(2) . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 119.2(3) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C25 C24 C23 121.1(3) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C21 C26 C25 119.2(3) . . ? C21 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C28 C27 C212 118.8(2) . . ? C28 C27 P21 120.6(2) . . ? C212 C27 P21 120.6(2) . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C210 C29 C28 120.3(3) . . ? C210 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C19 C110 C111 120.4(3) . . ? C19 C110 H11A 119.8 . . ? C111 C110 H11A 119.8 . . ? C110 C111 C112 120.2(3) . . ? C110 C111 H11B 119.9 . . ? C112 C111 H11B 119.9 . . ? C111 C112 C17 119.8(3) . . ? C111 C112 H11C 120.1 . . ? C17 C112 H11C 120.1 . . ? C114 C113 C118 121.4(2) . . ? C114 C113 P11 122.89(19) . . ? C118 C113 P11 114.23(19) . . ? C115 C114 C113 120.4(3) . . ? C115 C114 H11D 119.8 . . ? C113 C114 H11D 119.8 . . ? C116 C115 C114 119.1(3) . . ? C116 C115 H11E 120.5 . . ? C114 C115 H11E 120.5 . . ? C115 C116 C117 120.5(3) . . ? C115 C116 H11F 119.8 . . ? C117 C116 H11F 119.8 . . ? C116 C117 C118 122.7(3) . . ? C116 C117 H11G 118.6 . . ? C118 C117 H11G 118.6 . . ? C117 C118 C113 115.1(2) . . ? C117 C118 B1 122.1(2) . . ? C113 C118 B1 122.4(2) . . ? C121 C120 C119 121.2(3) . . ? C121 C120 C125 117.1(2) . . ? C119 C120 C125 121.7(2) . . ? C122 C121 C120 122.1(3) . . ? C122 C121 H12B 118.9 . . ? C120 C121 H12B 118.9 . . ? C123 C122 C121 116.9(3) . . ? C123 C122 C126 121.5(3) . . ? C121 C122 C126 121.7(3) . . ? C122 C123 C124 122.8(3) . . ? C122 C123 H12C 118.6 . . ? C124 C123 H12C 118.6 . . ? C123 C124 C119 120.5(3) . . ? C123 C124 C127 116.1(2) . . ? C119 C124 C127 123.4(2) . . ? C120 C119 C124 116.3(2) . . ? C120 C119 B1 118.8(2) . . ? C124 C119 B1 124.9(2) . . ? C120 C125 H12D 109.5 . . ? C120 C125 H12E 109.5 . . ? H12D C125 H12E 109.5 . . ? C120 C125 H12F 109.5 . . ? H12D C125 H12F 109.5 . . ? H12E C125 H12F 109.5 . . ? C122 C126 H12G 109.5 . . ? C122 C126 H12H 109.5 . . ? H12G C126 H12H 109.5 . . ? C122 C126 H12I 109.5 . . ? H12G C126 H12I 109.5 . . ? H12H C126 H12I 109.5 . . ? C124 C127 H12J 109.5 . . ? C124 C127 H12K 109.5 . . ? H12J C127 H12K 109.5 . . ? C124 C127 H12L 109.5 . . ? H12J C127 H12L 109.5 . . ? H12K C127 H12L 109.5 . . ? C133 C128 C129 121.8(2) . . ? C133 C128 P12 117.85(18) . . ? C129 C128 P12 120.37(19) . . ? C130 C129 C128 119.9(2) . . ? C130 C129 H12M 120.1 . . ? C128 C129 H12M 120.1 . . ? C131 C130 C129 119.4(2) . . ? C131 C130 H13B 120.3 . . ? C129 C130 H13B 120.3 . . ? C130 C131 C132 120.5(2) . . ? C130 C131 H13C 119.8 . . ? C132 C131 H13C 119.8 . . ? C131 C132 C133 121.8(2) . . ? C131 C132 H13D 119.1 . . ? C133 C132 H13D 119.1 . . ? C128 C133 C132 116.5(2) . . ? C128 C133 B1 123.5(2) . . ? C132 C133 B1 119.6(2) . . ? C135 C134 C139 118.1(2) . . ? C135 C134 P12 122.35(19) . . ? C139 C134 P12 119.5(2) . . ? C136 C135 C134 120.8(3) . . ? C136 C135 H13E 119.6 . . ? C134 C135 H13E 119.6 . . ? C135 C136 C137 120.4(3) . . ? C135 C136 H13F 119.8 . . ? C137 C136 H13F 119.8 . . ? C138 C137 C136 119.1(3) . . ? C138 C137 H13G 120.5 . . ? C136 C137 H13G 120.5 . . ? C139 C138 C137 120.6(3) . . ? C139 C138 H13H 119.7 . . ? C137 C138 H13H 119.7 . . ? C138 C139 C134 120.9(3) . . ? C138 C139 H13I 119.5 . . ? C134 C139 H13I 119.5 . . ? C145 C140 C141 119.2(2) . . ? C145 C140 P12 123.9(2) . . ? C141 C140 P12 116.8(2) . . ? C142 C141 C140 120.4(3) . . ? C142 C141 H14B 119.8 . . ? C140 C141 H14B 119.8 . . ? C141 C142 C143 120.3(3) . . ? C141 C142 H14C 119.9 . . ? C143 C142 H14C 119.9 . . ? C144 C143 C142 119.5(3) . . ? C144 C143 H14D 120.3 . . ? C142 C143 H14D 120.3 . . ? C143 C144 C145 120.5(3) . . ? C143 C144 H14E 119.7 . . ? C145 C144 H14E 119.7 . . ? C144 C145 C140 120.1(3) . . ? C144 C145 H14F 119.9 . . ? C140 C145 H14F 119.9 . . ? C151 C146 C147 117.1(2) . . ? C151 C146 Si1 123.6(2) . . ? C147 C146 Si1 119.1(2) . . ? C148 C147 C146 121.6(3) . . ? C148 C147 H14G 119.2 . . ? C146 C147 H14G 119.2 . . ? C147 C148 C149 120.2(3) . . ? C147 C148 H14H 119.9 . . ? C149 C148 H14H 119.9 . . ? C150 C149 C148 119.7(3) . . ? C150 C149 H14I 120.2 . . ? C148 C149 H14I 120.2 . . ? C149 C150 C151 119.9(3) . . ? C149 C150 H15B 120.0 . . ? C151 C150 H15B 120.0 . . ? C150 C151 C146 121.4(3) . . ? C150 C151 H15C 119.3 . . ? C146 C151 H15C 119.3 . . ? C153 C152 C157 117.1(2) . . ? C153 C152 Si1 119.16(19) . . ? C157 C152 Si1 123.7(2) . . ? C152 C153 C154 121.9(3) . . ? C152 C153 H15D 119.1 . . ? C154 C153 H15D 119.1 . . ? C155 C154 C153 119.5(3) . . ? C155 C154 H15E 120.3 . . ? C153 C154 H15E 120.3 . . ? C156 C155 C154 119.9(3) . . ? C156 C155 H15F 120.0 . . ? C154 C155 H15F 120.0 . . ? C155 C156 C157 120.0(3) . . ? C155 C156 H15G 120.0 . . ? C157 C156 H15G 120.0 . . ? C156 C157 C152 121.6(3) . . ? C156 C157 H15H 119.2 . . ? C152 C157 H15H 119.2 . . ? C211 C210 C29 119.7(3) . . ? C211 C210 H21A 120.1 . . ? C29 C210 H21A 120.1 . . ? C210 C211 C212 120.7(3) . . ? C210 C211 H21B 119.7 . . ? C212 C211 H21B 119.7 . . ? C211 C212 C27 120.0(3) . . ? C211 C212 H21C 120.0 . . ? C27 C212 H21C 120.0 . . ? C214 C213 C218 120.8(2) . . ? C214 C213 P21 122.40(19) . . ? C218 C213 P21 114.60(19) . . ? C215 C214 C213 120.5(2) . . ? C215 C214 H21D 119.8 . . ? C213 C214 H21D 119.8 . . ? C214 C215 C216 119.9(3) . . ? C214 C215 H21E 120.0 . . ? C216 C215 H21E 120.0 . . ? C215 C216 C217 119.7(3) . . ? C215 C216 H21F 120.2 . . ? C217 C216 H21F 120.2 . . ? C216 C217 C218 122.6(3) . . ? C216 C217 H21G 118.7 . . ? C218 C217 H21G 118.7 . . ? C217 C218 C213 116.3(2) . . ? C217 C218 B2 121.1(2) . . ? C213 C218 B2 122.3(2) . . ? C224 C219 C220 116.6(2) . . ? C224 C219 B2 118.3(2) . . ? C220 C219 B2 125.0(2) . . ? C221 C220 C219 120.7(3) . . ? C221 C220 C225 115.8(2) . . ? C219 C220 C225 123.5(2) . . ? C222 C221 C220 122.2(3) . . ? C222 C221 H22B 118.9 . . ? C220 C221 H22B 118.9 . . ? C223 C222 C221 117.5(3) . . ? C223 C222 C226 121.5(3) . . ? C221 C222 C226 121.0(3) . . ? C222 C223 C224 122.0(3) . . ? C222 C223 H22C 119.0 . . ? C224 C223 H22C 119.0 . . ? C223 C224 C219 120.8(3) . . ? C223 C224 C227 117.4(2) . . ? C219 C224 C227 121.8(2) . . ? C220 C225 H22D 109.5 . . ? C220 C225 H22E 109.5 . . ? H22D C225 H22E 109.5 . . ? C220 C225 H22F 109.5 . . ? H22D C225 H22F 109.5 . . ? H22E C225 H22F 109.5 . . ? C222 C226 H22G 109.5 . . ? C222 C226 H22H 109.5 . . ? H22G C226 H22H 109.5 . . ? C222 C226 H22I 109.5 . . ? H22G C226 H22I 109.5 . . ? H22H C226 H22I 109.5 . . ? C224 C227 H22J 109.5 . . ? C224 C227 H22K 109.5 . . ? H22J C227 H22K 109.5 . . ? C224 C227 H22L 109.5 . . ? H22J C227 H22L 109.5 . . ? H22K C227 H22L 109.5 . . ? C233 C228 C229 116.1(2) . . ? C233 C228 B2 123.1(2) . . ? C229 C228 B2 120.6(2) . . ? C230 C229 C228 122.1(3) . . ? C230 C229 H22M 119.0 . . ? C228 C229 H22M 119.0 . . ? C231 C230 C229 120.3(2) . . ? C231 C230 H23B 119.9 . . ? C229 C230 H23B 119.9 . . ? C230 C231 C232 119.4(3) . . ? C230 C231 H23C 120.3 . . ? C232 C231 H23C 120.3 . . ? C231 C232 C233 120.1(3) . . ? C231 C232 H23D 120.0 . . ? C233 C232 H23D 120.0 . . ? C232 C233 C228 122.0(2) . . ? C232 C233 P22 120.4(2) . . ? C228 C233 P22 117.50(19) . . ? C235 C234 C239 118.1(3) . . ? C235 C234 P22 119.6(2) . . ? C239 C234 P22 122.3(2) . . ? C236 C235 C234 121.2(3) . . ? C236 C235 H23E 119.4 . . ? C234 C235 H23E 119.4 . . ? C235 C236 C237 120.2(3) . . ? C235 C236 H23F 119.9 . . ? C237 C236 H23F 119.9 . . ? C238 C237 C236 119.2(3) . . ? C238 C237 H23G 120.4 . . ? C236 C237 H23G 120.4 . . ? C237 C238 C239 120.3(3) . . ? C237 C238 H23H 119.8 . . ? C239 C238 H23H 119.8 . . ? C234 C239 C238 120.9(3) . . ? C234 C239 H23I 119.5 . . ? C238 C239 H23I 119.5 . . ? C241 C240 C245 119.5(3) . . ? C241 C240 P22 123.4(2) . . ? C245 C240 P22 117.0(2) . . ? C240 C241 C242 120.0(3) . . ? C240 C241 H24B 120.0 . . ? C242 C241 H24B 120.0 . . ? C243 C242 C241 120.2(3) . . ? C243 C242 H24C 119.9 . . ? C241 C242 H24C 119.9 . . ? C242 C243 C244 120.1(3) . . ? C242 C243 H24D 119.9 . . ? C244 C243 H24D 119.9 . . ? C243 C244 C245 120.2(3) . . ? C243 C244 H24E 119.9 . . ? C245 C244 H24E 119.9 . . ? C244 C245 C240 120.0(3) . . ? C244 C245 H24F 120.0 . . ? C240 C245 H24F 120.0 . . ? C247 C246 C251 116.4(3) . . ? C247 C246 Si2 121.2(2) . . ? C251 C246 Si2 122.4(2) . . ? C248 C247 C246 122.0(3) . . ? C248 C247 H24G 119.0 . . ? C246 C247 H24G 119.0 . . ? C247 C248 C249 120.1(3) . . ? C247 C248 H24H 120.0 . . ? C249 C248 H24H 120.0 . . ? C250 C249 C248 119.5(3) . . ? C250 C249 H24I 120.3 . . ? C248 C249 H24I 120.3 . . ? C249 C250 C251 120.2(3) . . ? C249 C250 H25B 119.9 . . ? C251 C250 H25B 119.9 . . ? C250 C251 C246 121.8(3) . . ? C250 C251 H25C 119.1 . . ? C246 C251 H25C 119.1 . . ? C257 C252 C253 117.3(2) . . ? C257 C252 Si2 125.5(2) . . ? C253 C252 Si2 117.16(19) . . ? C254 C253 C252 121.5(3) . . ? C254 C253 H25D 119.2 . . ? C252 C253 H25D 119.2 . . ? C255 C254 C253 119.9(3) . . ? C255 C254 H25E 120.0 . . ? C253 C254 H25E 120.0 . . ? C256 C255 C254 119.7(3) . . ? C256 C255 H25F 120.2 . . ? C254 C255 H25F 120.2 . . ? C255 C256 C257 120.2(3) . . ? C255 C256 H25G 119.9 . . ? C257 C256 H25G 119.9 . . ? C252 C257 C256 121.2(3) . . ? C252 C257 H25H 119.4 . . ? C256 C257 H25H 119.4 . . ? C6S C1S C2S 109.2(8) . . ? C6S C1S H1SA 125.4 . . ? C2S C1S H1SA 125.4 . . ? C1S C2S C3S 122.5(6) . . ? C1S C2S H2SA 118.7 . . ? C3S C2S H2SA 118.7 . . ? C4S C3S C2S 126.1(6) . . ? C4S C3S H3SA 116.9 . . ? C2S C3S H3SA 116.9 . . ? C3S C4S C5S 109.5(5) . . ? C3S C4S H4S 125.2 . . ? C5S C4S H4S 125.2 . . ? C6S C5S C4S 119.8(5) . . ? C6S C5S H5SA 120.1 . . ? C4S C5S H5SA 120.1 . . ? C1S C6S C5S 132.6(7) . . ? C1S C6S H6SA 113.7 . . ? C5S C6S H6SA 113.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.754 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 961589' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_snm21 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common MesDPBPhNiCHOC6H5 _chemical_formula_moiety 'C55.50 H45 B Ni O P2' _chemical_formula_sum 'C55.50 H45 B Ni O P2' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour red _diffrn_ambient_temperature 100(2) _chemical_formula_weight 859.38 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9166(8) _cell_length_b 15.2418(9) _cell_length_c 22.8933(15) _cell_angle_alpha 90.00 _cell_angle_beta 105.256(3) _cell_angle_gamma 90.00 _cell_volume 4348.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9739 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 44.10 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8772 _exptl_absorpt_correction_T_max 0.9132 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 250827 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 42.16 _reflns_number_total 30670 _reflns_number_gt 21811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.8439P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30670 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.004 _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 Ni Ni 0.524544(8) 0.857811(6) 0.148442(4) 0.01161(2) Uani 1 1 d . . . P1 P 0.377812(15) 0.804384(12) 0.159419(8) 0.01055(3) Uani 1 1 d . . . P2 P 0.651139(15) 0.857286(12) 0.235447(9) 0.01040(3) Uani 1 1 d . . . O O 0.60135(5) 0.88124(5) 0.09116(3) 0.01939(11) Uani 1 1 d . . . B B 0.45027(7) 0.98182(5) 0.22142(4) 0.01342(13) Uani 1 1 d . . . C1 C 0.78984(6) 0.84449(5) 0.23066(4) 0.01330(11) Uani 1 1 d . . . C2 C 0.81637(6) 0.87699(5) 0.17931(4) 0.01582(12) Uani 1 1 d . . . H2 H 0.7622 0.9017 0.1471 0.019 Uiso 1 1 calc R . . C3 C 0.92204(7) 0.87322(6) 0.17531(4) 0.01924(14) Uani 1 1 d . . . H3 H 0.9397 0.8961 0.1405 0.023 Uiso 1 1 calc R . . C4 C 1.00179(7) 0.83634(6) 0.22172(5) 0.02032(15) Uani 1 1 d . . . H4 H 1.0736 0.8333 0.2185 0.024 Uiso 1 1 calc R . . C5 C 0.97596(7) 0.80408(5) 0.27272(4) 0.01927(14) Uani 1 1 d . . . H5 H 1.0303 0.7789 0.3046 0.023 Uiso 1 1 calc R . . C6 C 0.87095(6) 0.80842(5) 0.27750(4) 0.01617(13) Uani 1 1 d . . . H6 H 0.8542 0.7868 0.3128 0.019 Uiso 1 1 calc R . . C7 C 0.64155(6) 0.77334(5) 0.29063(3) 0.01254(11) Uani 1 1 d . . . C8 C 0.59447(7) 0.79048(5) 0.33778(4) 0.01667(13) Uani 1 1 d . . . H8 H 0.5718 0.8483 0.3438 0.020 Uiso 1 1 calc R . . C9 C 0.58052(8) 0.72299(6) 0.37615(4) 0.02259(16) Uani 1 1 d . . . H9 H 0.5475 0.7348 0.4078 0.027 Uiso 1 1 calc R . . C10 C 0.61483(8) 0.63867(6) 0.36818(4) 0.02433(17) Uani 1 1 d . . . H10 H 0.6055 0.5928 0.3944 0.029 Uiso 1 1 calc R . . C11 C 0.66271(7) 0.62132(6) 0.32191(4) 0.02122(15) Uani 1 1 d . . . H11 H 0.6871 0.5637 0.3168 0.025 Uiso 1 1 calc R . . C12 C 0.67515(6) 0.68792(5) 0.28293(4) 0.01636(13) Uani 1 1 d . . . H12 H 0.7067 0.6754 0.2508 0.020 Uiso 1 1 calc R . . C13 C 0.65701(6) 0.96096(5) 0.27605(3) 0.01248(11) Uani 1 1 d . . . C14 C 0.75192(7) 0.99167(5) 0.31545(4) 0.01659(13) Uani 1 1 d . . . H14 H 0.8148 0.9565 0.3235 0.020 Uiso 1 1 calc R . . C15 C 0.75488(8) 1.07319(5) 0.34290(4) 0.02056(15) Uani 1 1 d . . . H15 H 0.8195 1.0937 0.3698 0.025 Uiso 1 1 calc R . . C16 C 0.66294(8) 1.12459(5) 0.33090(4) 0.02076(15) Uani 1 1 d . . . H16 H 0.6643 1.1802 0.3498 0.025 Uiso 1 1 calc R . . C17 C 0.56892(7) 1.09442(5) 0.29123(4) 0.01817(14) Uani 1 1 d . . . H17 H 0.5066 1.1302 0.2832 0.022 Uiso 1 1 calc R . . C18 C 0.56355(6) 1.01244(4) 0.26264(3) 0.01322(11) Uani 1 1 d . . . C19 C 0.39283(6) 0.91390(5) 0.25508(3) 0.01260(11) Uani 1 1 d . . . C20 C 0.37883(7) 0.93866(5) 0.31160(4) 0.01703(13) Uani 1 1 d . . . H20 H 0.4083 0.9926 0.3292 0.020 Uiso 1 1 calc R . . C21 C 0.32292(7) 0.88609(6) 0.34239(4) 0.01931(14) Uani 1 1 d . . . H21 H 0.3135 0.9046 0.3803 0.023 Uiso 1 1 calc R . . C22 C 0.28080(7) 0.80646(6) 0.31772(4) 0.01847(14) Uani 1 1 d . . . H22 H 0.2413 0.7709 0.3383 0.022 Uiso 1 1 calc R . . C23 C 0.29660(6) 0.77881(5) 0.26283(4) 0.01533(12) Uani 1 1 d . . . H23 H 0.2693 0.7237 0.2464 0.018 Uiso 1 1 calc R . . C24 C 0.35249(6) 0.83187(5) 0.23172(3) 0.01182(11) Uani 1 1 d . . . C25 C 0.24918(6) 0.83000(5) 0.10571(3) 0.01349(11) Uani 1 1 d . . . C26 C 0.24110(7) 0.90028(5) 0.06599(3) 0.01543(12) Uani 1 1 d . . . H26 H 0.3035 0.9328 0.0652 0.019 Uiso 1 1 calc R . . C27 C 0.14231(7) 0.92330(5) 0.02729(4) 0.01951(14) Uani 1 1 d . . . H27 H 0.1375 0.9715 0.0004 0.023 Uiso 1 1 calc R . . C29 C 0.05825(7) 0.80546(6) 0.06750(4) 0.02112(15) Uani 1 1 d . . . H29 H -0.0042 0.7730 0.0681 0.025 Uiso 1 1 calc R . . C28 C 0.05099(7) 0.87585(6) 0.02796(4) 0.02241(16) Uani 1 1 d . . . H28 H -0.0163 0.8914 0.0015 0.027 Uiso 1 1 calc R . . C30 C 0.15654(6) 0.78263(5) 0.10611(4) 0.01741(13) Uani 1 1 d . . . H30 H 0.1610 0.7345 0.1330 0.021 Uiso 1 1 calc R . . C31 C 0.38185(6) 0.68503(5) 0.15544(3) 0.01272(11) Uani 1 1 d . . . C37 C 0.38716(6) 1.04280(5) 0.16831(3) 0.01257(11) Uani 1 1 d . . . C36 C 0.43475(6) 0.63587(5) 0.20587(4) 0.01526(12) Uani 1 1 d . . . H36 H 0.4603 0.6639 0.2440 0.018 Uiso 1 1 calc R . . C38 C 0.44331(6) 1.08840(5) 0.13159(3) 0.01400(12) Uani 1 1 d . . . C35 C 0.45038(7) 0.54635(5) 0.20072(4) 0.01888(14) Uani 1 1 d . . . H35 H 0.4869 0.5136 0.2353 0.023 Uiso 1 1 calc R . . C39 C 0.38899(7) 1.14350(5) 0.08516(4) 0.01735(13) Uani 1 1 d . . . H39 H 0.4282 1.1721 0.0609 0.021 Uiso 1 1 calc R . . C34 C 0.41305(7) 0.50455(5) 0.14540(4) 0.02035(15) Uani 1 1 d . . . H34 H 0.4242 0.4434 0.1420 0.024 Uiso 1 1 calc R . . C40 C 0.27933(7) 1.15794(5) 0.07311(4) 0.01750(13) Uani 1 1 d . . . C33 C 0.35939(8) 0.55251(5) 0.09515(4) 0.02176(15) Uani 1 1 d . . . H33 H 0.3331 0.5240 0.0572 0.026 Uiso 1 1 calc R . . C41 C 0.22413(6) 1.11523(5) 0.10927(4) 0.01493(12) Uani 1 1 d . . . H41 H 0.1492 1.1250 0.1020 0.018 Uiso 1 1 calc R . . C32 C 0.34378(7) 0.64224(5) 0.09988(4) 0.01800(13) Uani 1 1 d . . . H32 H 0.3070 0.6747 0.0652 0.022 Uiso 1 1 calc R . . C42 C 0.27465(6) 1.05865(5) 0.15584(3) 0.01339(11) Uani 1 1 d . . . C43 C 0.56277(7) 1.08135(6) 0.13998(4) 0.01866(14) Uani 1 1 d . . . H43A H 0.5807 1.1019 0.1033 0.028 Uiso 1 1 calc R . . H43B H 0.5850 1.0200 0.1476 0.028 Uiso 1 1 calc R . . H43C H 0.6002 1.1175 0.1745 0.028 Uiso 1 1 calc R . . C44 C 0.22334(8) 1.21987(8) 0.02371(5) 0.0290(2) Uani 1 1 d . . . H44A H 0.1531 1.2357 0.0294 0.044 Uiso 1 1 calc R . . H44B H 0.2137 1.1913 -0.0157 0.044 Uiso 1 1 calc R . . H44C H 0.2668 1.2730 0.0253 0.044 Uiso 1 1 calc R . . C45 C 0.20229(7) 1.01926(6) 0.19101(4) 0.01902(14) Uani 1 1 d . . . H45A H 0.1300 1.0439 0.1764 0.029 Uiso 1 1 calc R . . H45B H 0.2307 1.0328 0.2341 0.029 Uiso 1 1 calc R . . H45C H 0.1992 0.9555 0.1853 0.029 Uiso 1 1 calc R . . C46 C 0.50283(7) 0.86489(5) 0.05920(4) 0.01642(13) Uani 1 1 d . . . C47 C 0.47828(6) 0.78114(6) 0.02617(3) 0.01616(13) Uani 1 1 d . . . C52 C 0.38281(7) 0.77007(6) -0.01935(4) 0.01969(14) Uani 1 1 d . . . H52 H 0.3311 0.8158 -0.0277 0.024 Uiso 1 1 calc R . . C51 C 0.36321(8) 0.69265(7) -0.05243(4) 0.02498(17) Uani 1 1 d . . . H51 H 0.2981 0.6857 -0.0832 0.030 Uiso 1 1 calc R . . C49 C 0.53306(9) 0.63553(7) 0.00460(4) 0.02506(17) Uani 1 1 d . . . H49 H 0.5845 0.5896 0.0128 0.030 Uiso 1 1 calc R . . C48 C 0.55274(7) 0.71247(6) 0.03789(4) 0.01940(14) Uani 1 1 d . . . H48 H 0.6175 0.7187 0.0690 0.023 Uiso 1 1 calc R . . C50 C 0.43824(9) 0.62532(7) -0.04083(5) 0.02772(19) Uani 1 1 d . . . H50 H 0.4249 0.5726 -0.0638 0.033 Uiso 1 1 calc R . . H46 H 0.4575(11) 0.9148(9) 0.0412(6) 0.025(3) Uiso 1 1 d . . . C1S C -0.0528(2) 0.49231(14) 0.01803(11) 0.0311(4) Uani 0.50 1 d P . 1 C2S C 0.0009(7) 0.5713(7) 0.0217(5) 0.049(2) Uani 0.50 1 d P . 1 C3S C 0.0792(3) 0.58323(19) -0.00863(15) 0.0483(7) Uani 0.50 1 d P . 1 C4S C 0.1182(10) 0.5140(7) -0.0451(3) 0.076(3) Uani 0.50 1 d P . 1 C5S C 0.0538(4) 0.4361(2) -0.04577(15) 0.0568(9) Uani 0.50 1 d P . 1 C6S C -0.0248(7) 0.4254(7) -0.0163(4) 0.0424(17) Uani 0.50 1 d P . 1 C7S C -0.1277(8) 0.4784(7) 0.0485(4) 0.068(3) Uani 0.50 1 d P . 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 Ni 0.01082(4) 0.01330(4) 0.01046(4) 0.00148(3) 0.00234(3) -0.00220(3) P1 0.00961(7) 0.01031(7) 0.01140(7) 0.00139(5) 0.00217(6) 0.00014(5) P2 0.00951(7) 0.01028(7) 0.01134(7) -0.00017(5) 0.00261(6) -0.00044(5) O 0.0169(3) 0.0281(3) 0.0141(2) 0.0012(2) 0.0057(2) -0.0072(2) B 0.0141(3) 0.0116(3) 0.0151(3) 0.0008(2) 0.0047(3) 0.0002(2) C1 0.0105(3) 0.0125(3) 0.0169(3) -0.0016(2) 0.0037(2) -0.0011(2) C2 0.0136(3) 0.0143(3) 0.0206(3) -0.0005(2) 0.0065(3) -0.0009(2) C3 0.0153(3) 0.0180(3) 0.0271(4) -0.0009(3) 0.0104(3) -0.0019(3) C4 0.0121(3) 0.0169(3) 0.0332(4) -0.0034(3) 0.0080(3) -0.0007(2) C5 0.0115(3) 0.0163(3) 0.0282(4) -0.0021(3) 0.0019(3) 0.0001(2) C6 0.0117(3) 0.0156(3) 0.0201(3) -0.0006(2) 0.0023(2) -0.0009(2) C7 0.0106(3) 0.0124(2) 0.0136(3) 0.0014(2) 0.0014(2) -0.0004(2) C8 0.0167(3) 0.0189(3) 0.0145(3) 0.0018(2) 0.0042(2) -0.0002(2) C9 0.0231(4) 0.0277(4) 0.0171(3) 0.0065(3) 0.0054(3) -0.0029(3) C10 0.0235(4) 0.0233(4) 0.0231(4) 0.0116(3) 0.0007(3) -0.0037(3) C11 0.0166(3) 0.0151(3) 0.0286(4) 0.0070(3) 0.0000(3) 0.0006(3) C12 0.0137(3) 0.0128(3) 0.0218(3) 0.0017(2) 0.0033(3) 0.0010(2) C13 0.0141(3) 0.0108(2) 0.0122(3) -0.00056(19) 0.0027(2) -0.0011(2) C14 0.0168(3) 0.0150(3) 0.0158(3) -0.0011(2) 0.0005(2) -0.0016(2) C15 0.0239(4) 0.0164(3) 0.0184(3) -0.0036(2) 0.0002(3) -0.0040(3) C16 0.0282(4) 0.0128(3) 0.0201(3) -0.0037(2) 0.0044(3) -0.0024(3) C17 0.0224(4) 0.0110(3) 0.0211(3) -0.0012(2) 0.0056(3) 0.0009(2) C18 0.0154(3) 0.0099(2) 0.0145(3) 0.0010(2) 0.0042(2) -0.0001(2) C19 0.0129(3) 0.0124(2) 0.0128(3) 0.0014(2) 0.0039(2) 0.0015(2) C20 0.0198(3) 0.0168(3) 0.0159(3) 0.0000(2) 0.0071(3) 0.0021(3) C21 0.0209(4) 0.0239(4) 0.0157(3) 0.0032(3) 0.0094(3) 0.0051(3) C22 0.0171(3) 0.0215(3) 0.0198(3) 0.0076(3) 0.0101(3) 0.0032(3) C23 0.0132(3) 0.0152(3) 0.0189(3) 0.0045(2) 0.0064(2) 0.0010(2) C24 0.0105(3) 0.0122(2) 0.0130(3) 0.0027(2) 0.0035(2) 0.0015(2) C25 0.0118(3) 0.0139(3) 0.0136(3) 0.0000(2) 0.0011(2) 0.0018(2) C26 0.0169(3) 0.0145(3) 0.0137(3) 0.0004(2) 0.0020(2) 0.0037(2) C27 0.0220(4) 0.0180(3) 0.0151(3) -0.0008(2) -0.0010(3) 0.0074(3) C29 0.0122(3) 0.0236(4) 0.0244(4) -0.0046(3) -0.0007(3) 0.0012(3) C28 0.0178(4) 0.0233(4) 0.0207(4) -0.0047(3) -0.0044(3) 0.0074(3) C30 0.0124(3) 0.0185(3) 0.0196(3) -0.0003(2) 0.0012(2) 0.0002(2) C31 0.0115(3) 0.0112(2) 0.0159(3) 0.0009(2) 0.0044(2) -0.0001(2) C37 0.0128(3) 0.0110(2) 0.0143(3) 0.0009(2) 0.0044(2) 0.0001(2) C36 0.0130(3) 0.0134(3) 0.0183(3) 0.0021(2) 0.0021(2) 0.0007(2) C38 0.0135(3) 0.0131(3) 0.0156(3) 0.0016(2) 0.0043(2) -0.0010(2) C35 0.0183(3) 0.0131(3) 0.0243(4) 0.0038(2) 0.0039(3) 0.0023(2) C39 0.0158(3) 0.0197(3) 0.0164(3) 0.0055(2) 0.0039(2) -0.0008(3) C34 0.0235(4) 0.0123(3) 0.0265(4) 0.0005(3) 0.0088(3) 0.0015(3) C40 0.0163(3) 0.0186(3) 0.0160(3) 0.0039(2) 0.0014(3) -0.0002(2) C33 0.0305(4) 0.0143(3) 0.0208(4) -0.0030(3) 0.0074(3) -0.0005(3) C41 0.0132(3) 0.0142(3) 0.0166(3) 0.0007(2) 0.0026(2) 0.0010(2) C32 0.0237(4) 0.0143(3) 0.0160(3) 0.0003(2) 0.0052(3) 0.0006(3) C42 0.0133(3) 0.0115(2) 0.0162(3) 0.0002(2) 0.0053(2) 0.0008(2) C43 0.0143(3) 0.0191(3) 0.0234(4) 0.0067(3) 0.0064(3) 0.0002(3) C44 0.0193(4) 0.0369(5) 0.0278(5) 0.0168(4) 0.0007(3) 0.0023(4) C45 0.0153(3) 0.0196(3) 0.0249(4) 0.0059(3) 0.0101(3) 0.0039(3) C46 0.0162(3) 0.0216(3) 0.0116(3) 0.0034(2) 0.0040(2) -0.0011(3) C47 0.0149(3) 0.0237(3) 0.0099(3) 0.0020(2) 0.0034(2) -0.0005(3) C52 0.0159(3) 0.0306(4) 0.0116(3) 0.0016(3) 0.0018(2) -0.0005(3) C51 0.0230(4) 0.0371(5) 0.0129(3) -0.0031(3) 0.0014(3) -0.0052(4) C49 0.0281(5) 0.0267(4) 0.0204(4) -0.0011(3) 0.0064(3) 0.0039(3) C48 0.0178(3) 0.0254(4) 0.0143(3) 0.0017(3) 0.0028(3) 0.0019(3) C50 0.0334(5) 0.0309(4) 0.0186(4) -0.0061(3) 0.0063(3) -0.0035(4) C1S 0.0355(11) 0.0258(9) 0.0273(10) -0.0047(7) 0.0002(8) -0.0017(8) C2S 0.043(3) 0.026(2) 0.072(5) -0.017(3) 0.005(2) -0.0040(17) C3S 0.0487(16) 0.0383(13) 0.0464(16) 0.0003(11) -0.0076(13) -0.0113(12) C4S 0.152(8) 0.040(3) 0.0176(16) 0.0020(15) -0.007(3) 0.003(3) C5S 0.095(3) 0.0428(16) 0.0407(16) 0.0019(12) 0.0311(18) 0.0064(17) C6S 0.073(5) 0.0248(14) 0.0307(16) -0.0070(11) 0.015(3) -0.006(3) C7S 0.068(4) 0.044(3) 0.072(5) 0.001(3) -0.018(3) 0.005(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 Ni O 1.8752(6) . ? Ni C46 1.9906(8) . ? Ni P1 2.1375(2) . ? Ni P2 2.2197(2) . ? P1 C24 1.8186(8) . ? P1 C31 1.8229(7) . ? P1 C25 1.8302(8) . ? P2 C13 1.8248(7) . ? P2 C7 1.8251(7) . ? P2 C1 1.8339(8) . ? O C46 1.3141(10) . ? B C37 1.5764(11) . ? B C19 1.5864(11) . ? B C18 1.5882(11) . ? C1 C2 1.3988(11) . ? C1 C6 1.3994(11) . ? C2 C3 1.3931(11) . ? C2 H2 0.9500 . ? C3 C4 1.3892(13) . ? C3 H3 0.9500 . ? C4 C5 1.3862(14) . ? C4 H4 0.9500 . ? C5 C6 1.3906(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.3959(11) . ? C7 C12 1.3980(10) . ? C8 C9 1.3948(12) . ? C8 H8 0.9500 . ? C9 C10 1.3871(14) . ? C9 H9 0.9500 . ? C10 C11 1.3852(15) . ? C10 H10 0.9500 . ? C11 C12 1.3887(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.3977(11) . ? C13 C18 1.4044(10) . ? C14 C15 1.3884(11) . ? C14 H14 0.9500 . ? C15 C16 1.3885(13) . ? C15 H15 0.9500 . ? C16 C17 1.3895(12) . ? C16 H16 0.9500 . ? C17 C18 1.4037(10) . ? C17 H17 0.9500 . ? C19 C20 1.4043(11) . ? C19 C24 1.4051(10) . ? C20 C21 1.3887(12) . ? C20 H20 0.9500 . ? C21 C22 1.3879(13) . ? C21 H21 0.9500 . ? C22 C23 1.3906(12) . ? C22 H22 0.9500 . ? C23 C24 1.3974(10) . ? C23 H23 0.9500 . ? C25 C26 1.3912(11) . ? C25 C30 1.3996(11) . ? C26 C27 1.3933(11) . ? C26 H26 0.9500 . ? C27 C28 1.3871(14) . ? C27 H27 0.9500 . ? C29 C30 1.3869(12) . ? C29 C28 1.3910(14) . ? C29 H29 0.9500 . ? C28 H28 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.3948(10) . ? C31 C32 1.3987(11) . ? C37 C42 1.4260(10) . ? C37 C38 1.4271(10) . ? C36 C35 1.3889(11) . ? C36 H36 0.9500 . ? C38 C39 1.3910(11) . ? C38 C43 1.5079(11) . ? C35 C34 1.3860(13) . ? C35 H35 0.9500 . ? C39 C40 1.3875(12) . ? C39 H39 0.9500 . ? C34 C33 1.3851(13) . ? C34 H34 0.9500 . ? C40 C41 1.3886(12) . ? C40 C44 1.5041(12) . ? C33 C32 1.3907(11) . ? C33 H33 0.9500 . ? C41 C42 1.3928(11) . ? C41 H41 0.9500 . ? C32 H32 0.9500 . ? C42 C45 1.5095(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.4750(12) . ? C46 H46 0.982(14) . ? C47 C48 1.3988(12) . ? C47 C52 1.3996(11) . ? C52 C51 1.3890(14) . ? C52 H52 0.9500 . ? C51 C50 1.3883(16) . ? C51 H51 0.9500 . ? C49 C48 1.3852(13) . ? C49 C50 1.3912(15) . ? C49 H49 0.9500 . ? C48 H48 0.9500 . ? C50 H50 0.9500 . ? C1S C4S 1.176(13) 3_565 ? C1S C3S 1.204(3) 3_565 ? C1S C5S 1.265(4) 3_565 ? C1S C7S 1.350(12) . ? C1S C2S 1.382(10) . ? C1S C6S 1.393(10) . ? C1S C2S 1.593(10) 3_565 ? C1S C6S 1.613(9) 3_565 ? C1S C1S 1.786(5) 3_565 ? C2S C6S 0.364(15) 3_565 ? C2S C5S 1.010(9) 3_565 ? C2S C3S 1.381(8) . ? C2S C1S 1.593(10) 3_565 ? C3S C6S 1.024(9) 3_565 ? C3S C1S 1.204(3) 3_565 ? C3S C4S 1.513(11) . ? C3S C7S 1.552(11) 3_565 ? C4S C7S 0.20(2) 3_565 ? C4S C1S 1.176(13) 3_565 ? C4S C5S 1.448(13) . ? C5S C2S 1.010(9) 3_565 ? C5S C1S 1.264(4) 3_565 ? C5S C6S 1.368(8) . ? C5S C7S 1.626(12) 3_565 ? C6S C2S 0.364(15) 3_565 ? C6S C3S 1.024(9) 3_565 ? C6S C1S 1.613(9) 3_565 ? C7S C4S 0.20(2) 3_565 ? C7S C3S 1.552(11) 3_565 ? C7S C5S 1.626(12) 3_565 ? 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 O Ni C46 39.60(3) . . ? O Ni P1 143.46(2) . . ? C46 Ni P1 104.56(3) . . ? O Ni P2 103.17(2) . . ? C46 Ni P2 142.44(3) . . ? P1 Ni P2 111.084(9) . . ? C24 P1 C31 106.84(3) . . ? C24 P1 C25 102.32(3) . . ? C31 P1 C25 102.25(3) . . ? C24 P1 Ni 113.37(2) . . ? C31 P1 Ni 109.66(3) . . ? C25 P1 Ni 121.07(3) . . ? C13 P2 C7 104.82(3) . . ? C13 P2 C1 102.25(3) . . ? C7 P2 C1 102.24(3) . . ? C13 P2 Ni 112.09(2) . . ? C7 P2 Ni 117.10(2) . . ? C1 P2 Ni 116.57(3) . . ? C46 O Ni 74.94(4) . . ? C37 B C19 123.11(7) . . ? C37 B C18 119.58(6) . . ? C19 B C18 112.25(6) . . ? C2 C1 C6 118.91(7) . . ? C2 C1 P2 118.14(6) . . ? C6 C1 P2 122.83(6) . . ? C3 C2 C1 120.11(8) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.56(8) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.57(8) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.34(8) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.50(8) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 119.00(7) . . ? C8 C7 P2 121.78(6) . . ? C12 C7 P2 119.06(6) . . ? C9 C8 C7 120.24(8) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.12(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 119.99(8) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.15(8) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.49(8) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C14 C13 C18 120.76(7) . . ? C14 C13 P2 122.05(6) . . ? C18 C13 P2 117.02(5) . . ? C15 C14 C13 120.45(8) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.68(8) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 119.84(7) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 121.79(8) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C13 117.47(7) . . ? C17 C18 B 117.60(7) . . ? C13 C18 B 124.77(6) . . ? C20 C19 C24 117.71(7) . . ? C20 C19 B 117.53(7) . . ? C24 C19 B 124.74(7) . . ? C21 C20 C19 121.53(8) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C20 119.91(8) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 119.85(7) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.23(7) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.71(7) . . ? C23 C24 P1 124.84(6) . . ? C19 C24 P1 114.45(5) . . ? C26 C25 C30 118.96(7) . . ? C26 C25 P1 120.13(6) . . ? C30 C25 P1 120.81(6) . . ? C25 C26 C27 120.54(8) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 120.06(8) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C30 C29 C28 120.13(8) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C27 C28 C29 119.83(8) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C29 C30 C25 120.48(8) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C36 C31 C32 118.73(7) . . ? C36 C31 P1 120.59(6) . . ? C32 C31 P1 120.20(6) . . ? C42 C37 C38 116.65(7) . . ? C42 C37 B 123.18(7) . . ? C38 C37 B 120.11(7) . . ? C35 C36 C31 120.53(8) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C39 C38 C37 120.79(7) . . ? C39 C38 C43 115.71(7) . . ? C37 C38 C43 123.50(7) . . ? C34 C35 C36 120.37(8) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C40 C39 C38 122.07(7) . . ? C40 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? C33 C34 C35 119.61(8) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C39 C40 C41 117.67(7) . . ? C39 C40 C44 120.85(8) . . ? C41 C40 C44 121.45(8) . . ? C34 C33 C32 120.36(8) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C40 C41 C42 122.41(7) . . ? C40 C41 H41 118.8 . . ? C42 C41 H41 118.8 . . ? C33 C32 C31 120.39(8) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C41 C42 C37 120.38(7) . . ? C41 C42 C45 115.05(7) . . ? C37 C42 C45 124.55(7) . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O C46 C47 119.71(7) . . ? O C46 Ni 65.46(4) . . ? C47 C46 Ni 115.63(5) . . ? O C46 H46 118.0(8) . . ? C47 C46 H46 115.5(8) . . ? Ni C46 H46 112.3(8) . . ? C48 C47 C52 118.64(8) . . ? C48 C47 C46 120.33(7) . . ? C52 C47 C46 120.96(8) . . ? C51 C52 C47 120.45(9) . . ? C51 C52 H52 119.8 . . ? C47 C52 H52 119.8 . . ? C50 C51 C52 120.38(9) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C48 C49 C50 120.27(9) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C48 C47 120.70(8) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C51 C50 C49 119.55(9) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C4S C1S C3S 78.9(5) 3_565 3_565 ? C4S C1S C5S 72.7(5) 3_565 3_565 ? C3S C1S C5S 151.1(4) 3_565 3_565 ? C4S C1S C7S 4.4(9) 3_565 . ? C3S C1S C7S 74.6(5) 3_565 . ? C5S C1S C7S 76.9(5) 3_565 . ? C4S C1S C2S 117.3(6) 3_565 . ? C3S C1S C2S 163.5(5) 3_565 . ? C5S C1S C2S 44.6(4) 3_565 . ? C7S C1S C2S 121.5(6) . . ? C4S C1S C6S 124.6(6) 3_565 . ? C3S C1S C6S 45.7(4) 3_565 . ? C5S C1S C6S 162.6(4) 3_565 . ? C7S C1S C6S 120.3(6) . . ? C2S C1S C6S 118.2(5) . . ? C4S C1S C2S 136.0(6) 3_565 3_565 ? C3S C1S C2S 57.1(4) 3_565 3_565 ? C5S C1S C2S 150.9(4) 3_565 3_565 ? C7S C1S C2S 131.7(6) . 3_565 ? C2S C1S C2S 106.6(5) . 3_565 ? C6S C1S C2S 11.7(6) . 3_565 ? C4S C1S C6S 127.8(6) 3_565 3_565 ? C3S C1S C6S 152.6(4) 3_565 3_565 ? C5S C1S C6S 55.2(4) 3_565 3_565 ? C7S C1S C6S 132.0(6) . 3_565 ? C2S C1S C6S 10.8(7) . 3_565 ? C6S C1S C6S 107.5(5) . 3_565 ? C2S C1S C6S 95.9(4) 3_565 3_565 ? C4S C1S C1S 175.1(5) 3_565 3_565 ? C3S C1S C1S 104.9(3) 3_565 3_565 ? C5S C1S C1S 103.2(3) 3_565 3_565 ? C7S C1S C1S 176.2(4) . 3_565 ? C2S C1S C1S 58.7(4) . 3_565 ? C6S C1S C1S 59.5(4) . 3_565 ? C2S C1S C1S 47.9(3) 3_565 3_565 ? C6S C1S C1S 48.1(4) 3_565 3_565 ? C6S C2S C5S 167(4) 3_565 3_565 ? C6S C2S C3S 10(3) 3_565 . ? C5S C2S C3S 177.1(11) 3_565 . ? C6S C2S C1S 124(4) 3_565 . ? C5S C2S C1S 61.5(5) 3_565 . ? C3S C2S C1S 120.4(8) . . ? C6S C2S C1S 51(3) 3_565 3_565 ? C5S C2S C1S 134.6(9) 3_565 3_565 ? C3S C2S C1S 47.1(3) . 3_565 ? C1S C2S C1S 73.4(5) . 3_565 ? C6S C3S C1S 76.9(6) 3_565 3_565 ? C6S C3S C2S 3.6(9) 3_565 . ? C1S C3S C2S 75.8(5) 3_565 . ? C6S C3S C4S 126.6(8) 3_565 . ? C1S C3S C4S 49.7(5) 3_565 . ? C2S C3S C4S 125.5(7) . . ? C6S C3S C7S 133.8(8) 3_565 3_565 ? C1S C3S C7S 57.0(5) 3_565 3_565 ? C2S C3S C7S 132.7(7) . 3_565 ? C4S C3S C7S 7.3(9) . 3_565 ? C7S C4S C1S 149(6) 3_565 3_565 ? C7S C4S C5S 153(5) 3_565 . ? C1S C4S C5S 56.5(6) 3_565 . ? C7S C4S C3S 98(6) 3_565 . ? C1S C4S C3S 51.4(4) 3_565 . ? C5S C4S C3S 107.7(8) . . ? C2S C5S C1S 73.9(7) 3_565 3_565 ? C2S C5S C6S 3.4(10) 3_565 . ? C1S C5S C6S 75.5(5) 3_565 . ? C2S C5S C4S 124.7(8) 3_565 . ? C1S C5S C4S 50.9(5) 3_565 . ? C6S C5S C4S 126.3(7) . . ? C2S C5S C7S 127.8(8) 3_565 3_565 ? C1S C5S C7S 53.9(4) 3_565 3_565 ? C6S C5S C7S 129.3(6) . 3_565 ? C4S C5S C7S 3.2(7) . 3_565 ? C2S C6S C3S 166(3) 3_565 3_565 ? C2S C6S C5S 9(3) 3_565 . ? C3S C6S C5S 175.7(9) 3_565 . ? C2S C6S C1S 117(3) 3_565 . ? C3S C6S C1S 57.4(5) 3_565 . ? C5S C6S C1S 121.8(7) . . ? C2S C6S C1S 45(3) 3_565 3_565 ? C3S C6S C1S 129.4(8) 3_565 3_565 ? C5S C6S C1S 49.4(3) . 3_565 ? C1S C6S C1S 72.5(5) . 3_565 ? C4S C7S C1S 27(5) 3_565 . ? C4S C7S C3S 75(6) 3_565 3_565 ? C1S C7S C3S 48.4(4) . 3_565 ? C4S C7S C5S 24(5) 3_565 3_565 ? C1S C7S C5S 49.2(4) . 3_565 ? C3S C7S C5S 97.5(7) 3_565 3_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 42.16 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.688 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 961590'