# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Perrotin, Philippe' 'McCahill, Jenny' 'Wu, Guang' 'Scott, Susannah' _publ_contact_author_name 'Prof. Susannah Scott' _publ_contact_author_email sscott@engineering.ucsb.edu _publ_section_title ; Linear, High Molecular Weight Polyethylene from a Discrete, Mononuclear Phosphinoarenesulfonate Complex of Nickel(II) ; # Attachment '- 2a.CIF' data_a052810 _database_code_depnum_ccdc_archive 'CCDC 806742' #TrackingRef '- 2a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H47 Ni O7 P S' _chemical_formula_weight 869.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.165(7) _cell_length_b 11.531(7) _cell_length_c 17.445(11) _cell_angle_alpha 72.330(9) _cell_angle_beta 90.064(10) _cell_angle_gamma 83.002(10) _cell_volume 2122(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.648 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15376 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.71 _reflns_number_total 7172 _reflns_number_gt 5523 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7172 _refine_ls_number_parameters 539 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1855 _refine_ls_goodness_of_fit_ref 2.054 _refine_ls_restrained_S_all 2.075 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9579(7) 0.1543(5) 0.4464(4) 0.0456(16) Uani 1 1 d . . . H1A H 0.8763 0.1342 0.4444 0.055 Uiso 1 1 calc R . . H1B H 1.0187 0.0938 0.4361 0.055 Uiso 1 1 calc R . . C2 C 0.9855(8) 0.2009(6) 0.5066(4) 0.0510(18) Uani 1 1 d . . . H2 H 1.066(6) 0.172(6) 0.532(4) 0.061 Uiso 1 1 calc . . . C3 C 0.9347(7) 0.3056(5) 0.5149(3) 0.0439(16) Uani 1 1 d . . . H3A H 0.9815 0.3445 0.5446 0.053 Uiso 1 1 calc R . . H3B H 0.8494 0.3115 0.5257 0.053 Uiso 1 1 calc R . . C4 C 0.9184(6) 0.4886(6) 0.1942(3) 0.0447(17) Uani 1 1 d D . . C5 C 0.8933(4) 0.5766(5) 0.2239(3) 0.0302(13) Uani 1 1 d D . . C6 C 0.8737(5) 0.6938(5) 0.1666(3) 0.0318(13) Uani 1 1 d D . . H6 H 0.8515 0.7626 0.1831 0.038 Uiso 1 1 calc R . . C7 C 0.8874(5) 0.7061(5) 0.0866(3) 0.0345(14) Uani 1 1 d D . . H7 H 0.8734 0.7835 0.0488 0.041 Uiso 1 1 calc R . . C8 C 0.9212(5) 0.6065(5) 0.0622(3) 0.0375(15) Uani 1 1 d D . . H8 H 0.9288 0.6161 0.0076 0.045 Uiso 1 1 calc R . . C9 C 0.9446(5) 0.4910(5) 0.1174(3) 0.0347(14) Uani 1 1 d D . . H9 H 0.9752 0.4216 0.1036 0.042 Uiso 1 1 calc R . . C10 C 1.1284(4) 0.2794(4) 0.2324(3) 0.0175(10) Uani 1 1 d . . . C11 C 1.2372(4) 0.2890(4) 0.2692(3) 0.0192(11) Uani 1 1 d . . . C12 C 1.3456(5) 0.2621(5) 0.2348(3) 0.0271(12) Uani 1 1 d . . . H12 H 1.4179 0.2680 0.2590 0.032 Uiso 1 1 calc R . . C13 C 1.3485(5) 0.2269(5) 0.1656(3) 0.0280(12) Uani 1 1 d . . . H13 H 1.4218 0.2115 0.1430 0.034 Uiso 1 1 calc R . . C14 C 1.2419(5) 0.2150(5) 0.1304(3) 0.0251(12) Uani 1 1 d . . . H14 H 1.2433 0.1904 0.0843 0.030 Uiso 1 1 calc R . . C15 C 1.1332(5) 0.2393(4) 0.1636(3) 0.0211(11) Uani 1 1 d . . . H15 H 1.0619 0.2291 0.1402 0.025 Uiso 1 1 calc R . . C16 C 1.2434(4) 0.3347(5) 0.3409(3) 0.0225(12) Uani 1 1 d . . . C17 C 1.2391(4) 0.4602(5) 0.3286(3) 0.0250(12) Uani 1 1 d . . . C18 C 1.2604(5) 0.5056(5) 0.3920(3) 0.0297(13) Uani 1 1 d . . . H18 H 1.2592 0.5894 0.3831 0.036 Uiso 1 1 calc R . . C19 C 1.2832(5) 0.4239(6) 0.4685(4) 0.0360(15) Uani 1 1 d . . . H19 H 1.2960 0.4539 0.5112 0.043 Uiso 1 1 calc R . . C20 C 1.2875(5) 0.2987(6) 0.4830(3) 0.0342(14) Uani 1 1 d . . . H20 H 1.3025 0.2452 0.5350 0.041 Uiso 1 1 calc R . . C21 C 1.2690(5) 0.2536(5) 0.4188(3) 0.0283(13) Uani 1 1 d . . . C22 C 1.2006(7) 0.6624(5) 0.2355(4) 0.0506(18) Uani 1 1 d . . . H22A H 1.1412 0.6859 0.2696 0.076 Uiso 1 1 calc R . . H22B H 1.1757 0.7027 0.1801 0.076 Uiso 1 1 calc R . . H22C H 1.2768 0.6860 0.2464 0.076 Uiso 1 1 calc R . . C23 C 1.3175(6) 0.0452(6) 0.5029(4) 0.0493(17) Uani 1 1 d . . . H23A H 1.3944 0.0635 0.5175 0.074 Uiso 1 1 calc R . . H23B H 1.3261 -0.0366 0.4991 0.074 Uiso 1 1 calc R . . H23C H 1.2609 0.0517 0.5433 0.074 Uiso 1 1 calc R . . C24 C 0.8964(4) 0.2011(4) 0.2543(3) 0.0175(11) Uani 1 1 d . . . C25 C 0.7769(4) 0.2163(4) 0.2261(3) 0.0189(11) Uani 1 1 d . . . C26 C 0.7244(5) 0.1104(5) 0.2268(3) 0.0275(12) Uani 1 1 d . . . H26 H 0.6449 0.1198 0.2077 0.033 Uiso 1 1 calc R . . C27 C 0.7865(5) -0.0059(5) 0.2547(3) 0.0274(12) Uani 1 1 d . . . H27 H 0.7490 -0.0737 0.2550 0.033 Uiso 1 1 calc R . . C28 C 0.9045(5) -0.0208(5) 0.2822(3) 0.0240(12) Uani 1 1 d . . . H28 H 0.9476 -0.0989 0.3007 0.029 Uiso 1 1 calc R . . C29 C 0.9588(5) 0.0807(4) 0.2823(3) 0.0222(11) Uani 1 1 d . . . H29 H 1.0386 0.0695 0.3013 0.027 Uiso 1 1 calc R . . C30 C 0.6987(4) 0.3369(4) 0.1985(3) 0.0204(11) Uani 1 1 d . . . C31 C 0.6828(5) 0.4046(5) 0.1169(3) 0.0288(13) Uani 1 1 d . . . C32 C 0.6058(5) 0.5141(5) 0.0919(4) 0.0362(14) Uani 1 1 d . . . H32 H 0.5957 0.5593 0.0377 0.043 Uiso 1 1 calc R . . C33 C 0.5436(5) 0.5548(5) 0.1509(4) 0.0337(14) Uani 1 1 d . . . H33 H 0.4926 0.6287 0.1349 0.040 Uiso 1 1 calc R . . C34 C 0.5553(5) 0.4897(5) 0.2310(3) 0.0276(13) Uani 1 1 d . . . H34 H 0.5123 0.5183 0.2686 0.033 Uiso 1 1 calc R . . C35 C 0.6330(4) 0.3792(5) 0.2553(3) 0.0222(11) Uani 1 1 d . . . C36 C 0.7372(6) 0.4195(6) -0.0190(3) 0.0445(16) Uani 1 1 d . . . H36A H 0.6556 0.4250 -0.0384 0.067 Uiso 1 1 calc R . . H36B H 0.7907 0.3769 -0.0475 0.067 Uiso 1 1 calc R . . H36C H 0.7584 0.5006 -0.0277 0.067 Uiso 1 1 calc R . . C38 C 0.5786(5) 0.3352(6) 0.3928(3) 0.0396(15) Uani 1 1 d . . . H38A H 0.6034 0.4076 0.4009 0.059 Uiso 1 1 calc R . . H38B H 0.5903 0.2689 0.4422 0.059 Uiso 1 1 calc R . . H38C H 0.4948 0.3507 0.3759 0.059 Uiso 1 1 calc R . . C40 C 0.5084(5) 0.8156(5) 0.2452(4) 0.0362(14) Uani 1 1 d . . . H40 H 0.5654 0.8041 0.2085 0.043 Uiso 1 1 calc R . . C41 C 0.4096(6) 0.9034(5) 0.2200(4) 0.0445(16) Uani 1 1 d . . . H41 H 0.4004 0.9512 0.1663 0.053 Uiso 1 1 calc R . . C42 C 0.3239(6) 0.9209(6) 0.2739(4) 0.0464(17) Uani 1 1 d . . . H42 H 0.2572 0.9803 0.2567 0.056 Uiso 1 1 calc R . . C43 C 0.3386(6) 0.8496(6) 0.3532(4) 0.0446(17) Uani 1 1 d . . . H43 H 0.2816 0.8609 0.3900 0.054 Uiso 1 1 calc R . . C44 C 0.4376(6) 0.7611(6) 0.3783(4) 0.0423(16) Uani 1 1 d . . . H44 H 0.4464 0.7123 0.4318 0.051 Uiso 1 1 calc R . . C45 C 0.5233(6) 0.7447(6) 0.3246(4) 0.0390(15) Uani 1 1 d . . . H45 H 0.5907 0.6862 0.3419 0.047 Uiso 1 1 calc R . . C46 C 0.6092(6) 0.9777(7) 0.0422(4) 0.0508(18) Uani 1 1 d . . . H46 H 0.6828 0.9624 0.0707 0.061 Uiso 1 1 calc R . . C47 C 0.5620(6) 0.8841(6) 0.0244(4) 0.0505(18) Uani 1 1 d . . . H47 H 0.6041 0.8054 0.0408 0.061 Uiso 1 1 calc R . . C48 C 0.4530(7) 0.9056(7) -0.0175(4) 0.0513(18) Uani 1 1 d . . . H48 H 0.4213 0.8416 -0.0292 0.062 Uiso 1 1 calc R . . C49 C 0.1089(6) 0.9305(6) 0.0298(4) 0.0466(17) Uani 1 1 d . . . H49 H 0.1825 0.8836 0.0495 0.056 Uiso 1 1 calc R . . C50 C 0.0409(6) 0.9878(6) 0.0775(4) 0.0451(16) Uani 1 1 d . . . H50 H 0.0685 0.9795 0.1294 0.054 Uiso 1 1 calc R . . C51 C -0.0668(6) 1.0565(6) 0.0478(4) 0.0457(17) Uani 1 1 d . . . H51 H -0.1126 1.0952 0.0797 0.055 Uiso 1 1 calc R . . Ni Ni 0.97972(6) 0.32511(6) 0.39685(4) 0.0254(2) Uani 1 1 d . . . O1 O 0.9827(3) 0.5001(3) 0.3718(2) 0.0266(8) Uani 1 1 d . . . O2 O 0.8647(4) 0.6997(3) 0.3272(2) 0.0428(11) Uani 1 1 d . . . O3 O 0.7661(3) 0.5146(4) 0.3506(2) 0.0345(9) Uani 1 1 d . . . O4 O 1.2127(3) 0.5317(3) 0.2510(2) 0.0325(9) Uani 1 1 d . . . O5 O 1.2743(3) 0.1312(3) 0.4262(2) 0.0349(10) Uani 1 1 d . . . O6 O 0.7475(3) 0.3538(3) 0.0657(2) 0.0350(9) Uani 1 1 d . . . O7 O 0.6490(3) 0.3031(3) 0.3322(2) 0.0305(9) Uani 1 1 d . . . P P 0.98083(11) 0.31978(11) 0.27151(7) 0.0181(3) Uani 1 1 d . . . S S 0.87319(11) 0.57488(11) 0.32639(7) 0.0199(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.072(5) 0.032(3) 0.033(4) -0.012(3) 0.003(3) 0.000(3) C2 0.091(6) 0.035(4) 0.022(3) -0.001(3) 0.007(3) -0.006(4) C3 0.075(5) 0.036(4) 0.021(3) -0.010(3) 0.020(3) -0.005(3) C4 0.045(4) 0.059(5) 0.018(3) 0.006(3) -0.002(3) -0.008(3) C5 0.018(3) 0.032(3) 0.028(3) 0.011(3) -0.004(2) -0.006(2) C6 0.041(3) 0.020(3) 0.033(3) -0.008(3) -0.002(3) 0.000(2) C7 0.044(4) 0.026(3) 0.028(3) -0.001(3) -0.004(3) -0.001(3) C8 0.045(4) 0.037(4) 0.019(3) 0.005(3) 0.006(3) 0.001(3) C9 0.032(3) 0.030(3) 0.043(4) -0.018(3) -0.007(3) 0.009(3) C10 0.021(3) 0.013(2) 0.019(3) -0.007(2) 0.002(2) -0.001(2) C11 0.021(3) 0.015(3) 0.023(3) -0.008(2) -0.001(2) -0.001(2) C12 0.020(3) 0.032(3) 0.034(3) -0.018(3) -0.002(2) -0.002(2) C13 0.023(3) 0.032(3) 0.033(3) -0.016(3) 0.010(2) -0.003(2) C14 0.034(3) 0.023(3) 0.019(3) -0.009(2) 0.005(2) 0.000(2) C15 0.024(3) 0.018(3) 0.020(3) -0.005(2) -0.003(2) 0.000(2) C16 0.015(3) 0.029(3) 0.030(3) -0.017(2) 0.002(2) -0.004(2) C17 0.019(3) 0.028(3) 0.032(3) -0.017(3) -0.001(2) -0.001(2) C18 0.026(3) 0.032(3) 0.043(4) -0.026(3) 0.000(3) -0.007(2) C19 0.030(3) 0.056(4) 0.036(4) -0.032(3) 0.001(3) -0.011(3) C20 0.036(3) 0.047(4) 0.025(3) -0.019(3) 0.000(3) -0.008(3) C21 0.024(3) 0.035(3) 0.031(3) -0.017(3) -0.001(2) -0.004(2) C22 0.078(5) 0.023(3) 0.051(4) -0.014(3) -0.008(4) -0.002(3) C23 0.064(5) 0.038(4) 0.040(4) -0.004(3) -0.011(3) 0.000(3) C24 0.022(3) 0.017(3) 0.015(3) -0.007(2) 0.005(2) -0.005(2) C25 0.024(3) 0.021(3) 0.014(3) -0.008(2) 0.004(2) -0.003(2) C26 0.024(3) 0.033(3) 0.031(3) -0.018(3) -0.001(2) -0.009(2) C27 0.035(3) 0.022(3) 0.032(3) -0.015(2) 0.004(3) -0.010(2) C28 0.033(3) 0.016(3) 0.023(3) -0.007(2) 0.000(2) 0.001(2) C29 0.025(3) 0.021(3) 0.021(3) -0.008(2) -0.002(2) -0.001(2) C30 0.018(3) 0.020(3) 0.027(3) -0.012(2) 0.000(2) -0.002(2) C31 0.025(3) 0.033(3) 0.030(3) -0.013(3) 0.001(2) -0.001(2) C32 0.036(3) 0.033(3) 0.033(3) -0.003(3) -0.007(3) 0.002(3) C33 0.025(3) 0.027(3) 0.049(4) -0.014(3) -0.006(3) 0.006(2) C34 0.024(3) 0.025(3) 0.038(3) -0.016(3) -0.002(2) 0.001(2) C35 0.021(3) 0.024(3) 0.027(3) -0.013(2) -0.001(2) -0.005(2) C36 0.048(4) 0.059(4) 0.025(3) -0.014(3) -0.002(3) 0.002(3) C38 0.043(4) 0.048(4) 0.030(3) -0.018(3) 0.008(3) 0.004(3) C40 0.037(3) 0.035(3) 0.042(4) -0.020(3) 0.011(3) -0.006(3) C41 0.058(4) 0.024(3) 0.042(4) 0.002(3) 0.006(3) -0.003(3) C42 0.047(4) 0.030(3) 0.059(5) -0.011(3) 0.013(3) 0.003(3) C43 0.055(4) 0.044(4) 0.046(4) -0.029(3) 0.023(3) -0.013(3) C44 0.057(4) 0.044(4) 0.027(3) -0.012(3) -0.003(3) -0.009(3) C45 0.039(4) 0.039(4) 0.040(4) -0.017(3) -0.006(3) 0.004(3) C46 0.046(4) 0.059(5) 0.038(4) -0.001(3) 0.013(3) -0.010(4) C47 0.053(5) 0.039(4) 0.050(4) -0.001(3) 0.030(4) 0.000(3) C48 0.064(5) 0.053(5) 0.046(4) -0.022(3) 0.031(4) -0.022(4) C49 0.046(4) 0.037(4) 0.050(4) -0.001(3) 0.008(3) -0.010(3) C50 0.063(5) 0.044(4) 0.032(4) -0.012(3) 0.008(3) -0.022(4) C51 0.061(5) 0.036(4) 0.046(4) -0.017(3) 0.026(3) -0.016(3) Ni 0.0312(4) 0.0218(4) 0.0226(4) -0.0068(3) 0.0008(3) -0.0013(3) O1 0.031(2) 0.024(2) 0.027(2) -0.0127(16) -0.0036(16) 0.0002(16) O2 0.063(3) 0.029(2) 0.042(3) -0.0225(19) -0.007(2) 0.004(2) O3 0.033(2) 0.045(2) 0.029(2) -0.0165(18) 0.0023(17) -0.0032(18) O4 0.041(2) 0.022(2) 0.038(2) -0.0167(18) -0.0053(18) 0.0000(17) O5 0.047(3) 0.027(2) 0.030(2) -0.0084(17) -0.0072(19) -0.0016(18) O6 0.043(2) 0.039(2) 0.019(2) -0.0073(17) 0.0008(17) 0.0066(19) O7 0.035(2) 0.033(2) 0.024(2) -0.0118(18) 0.0069(17) 0.0022(17) P 0.0207(7) 0.0155(7) 0.0204(7) -0.0089(5) 0.0027(5) -0.0019(5) S 0.0276(7) 0.0150(6) 0.0175(7) -0.0067(5) 0.0002(5) 0.0006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.367(9) . ? C1 Ni 1.941(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.319(9) . ? C2 Ni 2.009(6) . ? C2 H2 0.98(7) . ? C3 Ni 2.072(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.275(7) . ? C4 C9 1.365(7) . ? C4 P 2.042(6) . ? C5 C6 1.407(7) . ? C5 S 1.797(6) . ? C6 C7 1.370(8) . ? C6 H6 0.9300 . ? C7 C8 1.355(8) . ? C7 H7 0.9300 . ? C8 C9 1.381(8) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.405(7) . ? C10 C15 1.410(7) . ? C10 P 1.846(5) . ? C11 C12 1.394(7) . ? C11 C16 1.502(7) . ? C12 C13 1.385(7) . ? C12 H12 0.9300 . ? C13 C14 1.378(7) . ? C13 H13 0.9300 . ? C14 C15 1.380(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.392(7) . ? C16 C21 1.402(7) . ? C17 O4 1.365(6) . ? C17 C18 1.391(7) . ? C18 C19 1.381(8) . ? C18 H18 0.9300 . ? C19 C20 1.383(8) . ? C19 H19 0.9300 . ? C20 C21 1.395(7) . ? C20 H20 0.9300 . ? C21 O5 1.372(6) . ? C22 O4 1.438(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O5 1.443(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.394(7) . ? C24 C29 1.416(7) . ? C24 P 1.847(5) . ? C25 C26 1.414(7) . ? C25 C30 1.492(7) . ? C26 C27 1.376(7) . ? C26 H26 0.9300 . ? C27 C28 1.374(7) . ? C27 H27 0.9300 . ? C28 C29 1.383(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.400(7) . ? C30 C35 1.402(7) . ? C31 O6 1.371(6) . ? C31 C32 1.387(8) . ? C32 C33 1.407(8) . ? C32 H32 0.9300 . ? C33 C34 1.368(8) . ? C33 H33 0.9300 . ? C34 C35 1.399(7) . ? C34 H34 0.9300 . ? C35 O7 1.360(6) . ? C36 O6 1.439(7) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C38 O7 1.428(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C40 C41 1.376(9) . ? C40 C45 1.376(8) . ? C40 H40 0.9300 . ? C41 C42 1.382(9) . ? C41 H41 0.9300 . ? C42 C43 1.377(9) . ? C42 H42 0.9300 . ? C43 C44 1.381(9) . ? C43 H43 0.9300 . ? C44 C45 1.376(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.371(9) . ? C46 C48 1.378(10) 2_675 ? C46 H46 0.9300 . ? C47 C48 1.376(10) . ? C47 H47 0.9300 . ? C48 C46 1.378(10) 2_675 ? C48 H48 0.9300 . ? C49 C50 1.386(9) . ? C49 C51 1.389(9) 2_575 ? C49 H49 0.9300 . ? C50 C51 1.364(10) . ? C50 H50 0.9300 . ? C51 C49 1.389(9) 2_575 ? C51 H51 0.9300 . ? Ni O1 1.935(4) . ? Ni P 2.206(2) . ? O1 S 1.481(4) . ? O2 S 1.435(4) . ? O3 S 1.455(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Ni 72.4(4) . . ? C2 C1 H1A 116.3 . . ? Ni C1 H1A 116.3 . . ? C2 C1 H1B 116.3 . . ? Ni C1 H1B 116.3 . . ? H1A C1 H1B 113.3 . . ? C3 C2 C1 125.3(7) . . ? C3 C2 Ni 73.8(4) . . ? C1 C2 Ni 67.1(4) . . ? C3 C2 H2 115(4) . . ? C1 C2 H2 115(4) . . ? Ni C2 H2 115(4) . . ? C2 C3 Ni 68.6(4) . . ? C2 C3 H3A 116.8 . . ? Ni C3 H3A 116.8 . . ? C2 C3 H3B 116.8 . . ? Ni C3 H3B 116.8 . . ? H3A C3 H3B 113.8 . . ? C5 C4 C9 130.1(6) . . ? C5 C4 P 117.7(4) . . ? C9 C4 P 109.3(5) . . ? C4 C5 C6 114.6(6) . . ? C4 C5 S 130.5(4) . . ? C6 C5 S 114.8(4) . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C6 120.6(5) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 120.7(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C4 C9 C8 113.4(5) . . ? C4 C9 H9 123.3 . . ? C8 C9 H9 123.3 . . ? C11 C10 C15 118.8(4) . . ? C11 C10 P 121.4(4) . . ? C15 C10 P 119.8(4) . . ? C12 C11 C10 118.6(4) . . ? C12 C11 C16 117.6(4) . . ? C10 C11 C16 123.6(4) . . ? C13 C12 C11 121.8(5) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C14 C13 C12 119.5(5) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 121.0(4) . . ? C14 C15 H15 119.5 . . ? C10 C15 H15 119.5 . . ? C17 C16 C21 118.9(4) . . ? C17 C16 C11 119.1(5) . . ? C21 C16 C11 121.5(5) . . ? O4 C17 C18 124.2(5) . . ? O4 C17 C16 114.6(4) . . ? C18 C17 C16 121.1(5) . . ? C19 C18 C17 118.8(5) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 121.7(5) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C21 119.2(5) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? O5 C21 C20 123.9(5) . . ? O5 C21 C16 115.8(4) . . ? C20 C21 C16 120.3(5) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 118.4(4) . . ? C25 C24 P 127.2(4) . . ? C29 C24 P 114.0(3) . . ? C24 C25 C26 118.2(5) . . ? C24 C25 C30 124.1(4) . . ? C26 C25 C30 117.7(4) . . ? C27 C26 C25 122.5(5) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C28 C27 C26 119.3(5) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 119.8(5) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C24 121.8(5) . . ? C28 C29 H29 119.1 . . ? C24 C29 H29 119.1 . . ? C31 C30 C35 119.2(5) . . ? C31 C30 C25 121.7(4) . . ? C35 C30 C25 119.0(4) . . ? O6 C31 C32 124.0(5) . . ? O6 C31 C30 115.0(5) . . ? C32 C31 C30 121.0(5) . . ? C31 C32 C33 118.1(5) . . ? C31 C32 H32 121.0 . . ? C33 C32 H32 121.0 . . ? C34 C33 C32 122.4(5) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 118.9(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? O7 C35 C34 124.9(5) . . ? O7 C35 C30 114.6(4) . . ? C34 C35 C30 120.4(5) . . ? O6 C36 H36A 109.5 . . ? O6 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O6 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O7 C38 H38A 109.5 . . ? O7 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O7 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C40 C45 120.3(6) . . ? C41 C40 H40 119.9 . . ? C45 C40 H40 119.9 . . ? C40 C41 C42 120.4(6) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 119.3(6) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C44 120.2(6) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.4(6) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C40 C45 C44 119.4(6) . . ? C40 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 C48 119.7(7) . 2_675 ? C47 C46 H46 120.2 . . ? C48 C46 H46 120.2 2_675 . ? C46 C47 C48 120.6(7) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C46 119.7(6) . 2_675 ? C47 C48 H48 120.1 . . ? C46 C48 H48 120.1 2_675 . ? C50 C49 C51 119.8(6) . 2_575 ? C50 C49 H49 120.1 . . ? C51 C49 H49 120.1 2_575 . ? C51 C50 C49 119.5(6) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C49 120.7(6) . 2_575 ? C50 C51 H51 119.7 . . ? C49 C51 H51 119.7 2_575 . ? O1 Ni C1 165.5(2) . . ? O1 Ni C2 127.2(2) . . ? C1 Ni C2 40.5(3) . . ? O1 Ni C3 92.93(19) . . ? C1 Ni C3 72.9(2) . . ? C2 Ni C3 37.7(2) . . ? O1 Ni P 96.67(11) . . ? C1 Ni P 96.47(18) . . ? C2 Ni P 136.0(2) . . ? C3 Ni P 163.5(2) . . ? S O1 Ni 113.61(19) . . ? C17 O4 C22 117.1(4) . . ? C21 O5 C23 117.0(4) . . ? C31 O6 C36 118.0(4) . . ? C35 O7 C38 118.1(4) . . ? C10 P C24 100.2(2) . . ? C10 P C4 104.0(2) . . ? C24 P C4 110.6(2) . . ? C10 P Ni 117.10(16) . . ? C24 P Ni 113.80(15) . . ? C4 P Ni 110.26(18) . . ? O2 S O3 115.6(2) . . ? O2 S O1 111.5(2) . . ? O3 S O1 111.3(2) . . ? O2 S C5 107.1(2) . . ? O3 S C5 105.1(2) . . ? O1 S C5 105.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni C1 C2 C3 47.8(7) . . . . ? C1 C2 C3 Ni -45.3(7) . . . . ? C9 C4 C5 C6 9.6(9) . . . . ? P C4 C5 C6 168.1(4) . . . . ? C9 C4 C5 S -173.1(5) . . . . ? P C4 C5 S -14.5(7) . . . . ? C4 C5 C6 C7 -2.8(7) . . . . ? S C5 C6 C7 179.5(4) . . . . ? C5 C6 C7 C8 -0.8(8) . . . . ? C6 C7 C8 C9 -1.2(9) . . . . ? C5 C4 C9 C8 -11.4(10) . . . . ? P C4 C9 C8 -171.3(4) . . . . ? C7 C8 C9 C4 6.2(8) . . . . ? C15 C10 C11 C12 2.0(7) . . . . ? P C10 C11 C12 -177.3(4) . . . . ? C15 C10 C11 C16 177.8(4) . . . . ? P C10 C11 C16 -1.5(7) . . . . ? C10 C11 C12 C13 0.2(8) . . . . ? C16 C11 C12 C13 -175.8(5) . . . . ? C11 C12 C13 C14 -1.6(8) . . . . ? C12 C13 C14 C15 0.7(8) . . . . ? C13 C14 C15 C10 1.5(7) . . . . ? C11 C10 C15 C14 -2.9(7) . . . . ? P C10 C15 C14 176.4(4) . . . . ? C12 C11 C16 C17 88.7(6) . . . . ? C10 C11 C16 C17 -87.1(6) . . . . ? C12 C11 C16 C21 -82.8(6) . . . . ? C10 C11 C16 C21 101.4(6) . . . . ? C21 C16 C17 O4 -179.6(4) . . . . ? C11 C16 C17 O4 8.7(6) . . . . ? C21 C16 C17 C18 0.3(7) . . . . ? C11 C16 C17 C18 -171.5(5) . . . . ? O4 C17 C18 C19 178.3(5) . . . . ? C16 C17 C18 C19 -1.5(8) . . . . ? C17 C18 C19 C20 1.2(8) . . . . ? C18 C19 C20 C21 0.4(8) . . . . ? C19 C20 C21 O5 178.3(5) . . . . ? C19 C20 C21 C16 -1.7(8) . . . . ? C17 C16 C21 O5 -178.7(4) . . . . ? C11 C16 C21 O5 -7.2(7) . . . . ? C17 C16 C21 C20 1.3(7) . . . . ? C11 C16 C21 C20 172.9(5) . . . . ? C29 C24 C25 C26 -0.1(7) . . . . ? P C24 C25 C26 -172.1(4) . . . . ? C29 C24 C25 C30 177.0(4) . . . . ? P C24 C25 C30 5.1(7) . . . . ? C24 C25 C26 C27 0.5(7) . . . . ? C30 C25 C26 C27 -176.8(5) . . . . ? C25 C26 C27 C28 -0.8(8) . . . . ? C26 C27 C28 C29 0.7(8) . . . . ? C27 C28 C29 C24 -0.3(8) . . . . ? C25 C24 C29 C28 0.0(7) . . . . ? P C24 C29 C28 173.0(4) . . . . ? C24 C25 C30 C31 97.3(6) . . . . ? C26 C25 C30 C31 -85.5(6) . . . . ? C24 C25 C30 C35 -87.2(6) . . . . ? C26 C25 C30 C35 89.9(5) . . . . ? C35 C30 C31 O6 -177.8(4) . . . . ? C25 C30 C31 O6 -2.3(7) . . . . ? C35 C30 C31 C32 1.8(7) . . . . ? C25 C30 C31 C32 177.2(5) . . . . ? O6 C31 C32 C33 179.1(5) . . . . ? C30 C31 C32 C33 -0.4(8) . . . . ? C31 C32 C33 C34 -0.9(8) . . . . ? C32 C33 C34 C35 0.8(8) . . . . ? C33 C34 C35 O7 -177.0(4) . . . . ? C33 C34 C35 C30 0.7(7) . . . . ? C31 C30 C35 O7 175.9(4) . . . . ? C25 C30 C35 O7 0.4(6) . . . . ? C31 C30 C35 C34 -1.9(7) . . . . ? C25 C30 C35 C34 -177.5(4) . . . . ? C45 C40 C41 C42 -0.4(9) . . . . ? C40 C41 C42 C43 0.0(10) . . . . ? C41 C42 C43 C44 -0.3(9) . . . . ? C42 C43 C44 C45 0.9(9) . . . . ? C41 C40 C45 C44 1.0(9) . . . . ? C43 C44 C45 C40 -1.3(9) . . . . ? C48 C46 C47 C48 -0.3(11) 2_675 . . . ? C46 C47 C48 C46 0.3(11) . . . 2_675 ? C51 C49 C50 C51 -0.1(10) 2_575 . . . ? C49 C50 C51 C49 0.1(10) . . . 2_575 ? C2 C1 Ni O1 -35.9(12) . . . . ? C2 C1 Ni C3 -23.7(5) . . . . ? C2 C1 Ni P 169.2(4) . . . . ? C3 C2 Ni O1 28.4(6) . . . . ? C1 C2 Ni O1 169.4(4) . . . . ? C3 C2 Ni C1 -141.0(7) . . . . ? C1 C2 Ni C3 141.0(7) . . . . ? C3 C2 Ni P -156.6(4) . . . . ? C1 C2 Ni P -15.6(6) . . . . ? C2 C3 Ni O1 -157.7(5) . . . . ? C2 C3 Ni C1 25.3(5) . . . . ? C2 C3 Ni P 76.7(8) . . . . ? C1 Ni O1 S -90.1(9) . . . . ? C2 Ni O1 S -118.7(4) . . . . ? C3 Ni O1 S -101.7(3) . . . . ? P Ni O1 S 64.8(2) . . . . ? C18 C17 O4 C22 -3.2(7) . . . . ? C16 C17 O4 C22 176.7(5) . . . . ? C20 C21 O5 C23 -8.7(8) . . . . ? C16 C21 O5 C23 171.3(5) . . . . ? C32 C31 O6 C36 1.6(8) . . . . ? C30 C31 O6 C36 -178.9(4) . . . . ? C34 C35 O7 C38 2.2(7) . . . . ? C30 C35 O7 C38 -175.5(4) . . . . ? C11 C10 P C24 -142.9(4) . . . . ? C15 C10 P C24 37.8(4) . . . . ? C11 C10 P C4 102.7(4) . . . . ? C15 C10 P C4 -76.7(4) . . . . ? C11 C10 P Ni -19.3(4) . . . . ? C15 C10 P Ni 161.4(3) . . . . ? C25 C24 P C10 -139.1(4) . . . . ? C29 C24 P C10 48.7(4) . . . . ? C25 C24 P C4 -29.7(5) . . . . ? C29 C24 P C4 158.0(4) . . . . ? C25 C24 P Ni 95.1(4) . . . . ? C29 C24 P Ni -77.2(4) . . . . ? C5 C4 P C10 -122.6(5) . . . . ? C9 C4 P C10 40.2(5) . . . . ? C5 C4 P C24 130.6(5) . . . . ? C9 C4 P C24 -66.6(5) . . . . ? C5 C4 P Ni 3.8(5) . . . . ? C9 C4 P Ni 166.6(4) . . . . ? O1 Ni P C10 96.3(2) . . . . ? C1 Ni P C10 -89.8(3) . . . . ? C2 Ni P C10 -79.7(4) . . . . ? C3 Ni P C10 -138.5(7) . . . . ? O1 Ni P C24 -147.3(2) . . . . ? C1 Ni P C24 26.6(3) . . . . ? C2 Ni P C24 36.7(4) . . . . ? C3 Ni P C24 -22.1(7) . . . . ? O1 Ni P C4 -22.3(2) . . . . ? C1 Ni P C4 151.6(3) . . . . ? C2 Ni P C4 161.7(4) . . . . ? C3 Ni P C4 102.8(7) . . . . ? Ni O1 S O2 165.0(2) . . . . ? Ni O1 S O3 34.3(3) . . . . ? Ni O1 S C5 -79.1(3) . . . . ? C4 C5 S O2 171.2(5) . . . . ? C6 C5 S O2 -11.5(4) . . . . ? C4 C5 S O3 -65.3(6) . . . . ? C6 C5 S O3 112.0(4) . . . . ? C4 C5 S O1 52.4(6) . . . . ? C6 C5 S O1 -130.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.430 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.111 # Attachment '- 2b.CIF' data_gniallym _database_code_depnum_ccdc_archive 'CCDC 806743' #TrackingRef '- 2b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H33 Ni O5 P S' _chemical_formula_weight 655.35 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.848(4) _cell_length_b 11.461(4) _cell_length_c 22.104(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.795(5) _cell_angle_gamma 90.00 _cell_volume 3116.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24608 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.83 _reflns_number_total 6423 _reflns_number_gt 5162 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6423 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _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 C1 C 0.3014(3) 0.8237(3) 0.19912(13) 0.0553(10) Uani 1 1 d . . . C2A C 0.2544(4) 0.7184(4) 0.18383(17) 0.0335(14) Uani 0.692(11) 1 d P . . C2B C 0.2114(9) 0.7800(9) 0.1905(4) 0.0335(14) Uani 0.31 1 d P . . C3 C 0.1701(2) 0.6724(3) 0.20422(12) 0.0367(7) Uani 1 1 d . . . C4 C 0.28564(18) 0.7041(2) 0.42785(11) 0.0180(5) Uani 1 1 d . . . C5 C 0.34230(19) 0.8101(2) 0.43941(10) 0.0191(5) Uani 1 1 d . . . C6 C 0.3885(2) 0.8489(2) 0.50085(11) 0.0252(6) Uani 1 1 d . . . H6 H 0.4261 0.9193 0.5081 0.030 Uiso 1 1 calc R . . C7 C 0.3785(2) 0.7827(2) 0.55139(12) 0.0281(6) Uani 1 1 d . . . H7 H 0.4099 0.8085 0.5925 0.034 Uiso 1 1 calc R . . C8 C 0.3224(2) 0.6794(2) 0.54092(12) 0.0285(6) Uani 1 1 d . . . H8 H 0.3160 0.6353 0.5750 0.034 Uiso 1 1 calc R . . C9 C 0.2751(2) 0.6402(2) 0.47945(11) 0.0248(5) Uani 1 1 d . . . H9 H 0.2361 0.5707 0.4728 0.030 Uiso 1 1 calc R . . C10 C 0.24602(19) 0.4882(2) 0.35609(11) 0.0196(5) Uani 1 1 d . . . C11 C 0.33327(19) 0.4347(2) 0.34087(10) 0.0204(5) Uani 1 1 d . . . C12 C 0.3487(2) 0.3147(2) 0.35063(12) 0.0264(6) Uani 1 1 d . . . H12 H 0.4063 0.2785 0.3405 0.032 Uiso 1 1 calc R . . C13 C 0.2802(3) 0.2486(2) 0.37496(13) 0.0319(6) Uani 1 1 d . . . H13 H 0.2922 0.1690 0.3816 0.038 Uiso 1 1 calc R . . C14 C 0.1937(2) 0.3017(2) 0.38944(12) 0.0309(6) Uani 1 1 d . . . H14 H 0.1470 0.2576 0.4055 0.037 Uiso 1 1 calc R . . C15 C 0.1765(2) 0.4204(2) 0.38002(12) 0.0249(5) Uani 1 1 d . . . H15 H 0.1181 0.4555 0.3897 0.030 Uiso 1 1 calc R . . C16 C 0.41615(19) 0.4991(2) 0.31812(11) 0.0205(5) Uani 1 1 d . . . C17 C 0.5008(2) 0.5598(2) 0.36074(11) 0.0230(5) Uani 1 1 d . . . C18 C 0.5839(2) 0.6109(2) 0.34131(13) 0.0285(6) Uani 1 1 d . . . H18 H 0.6405 0.6498 0.3701 0.034 Uiso 1 1 calc R . . C19 C 0.5811(2) 0.6030(2) 0.27873(13) 0.0298(6) Uani 1 1 d . . . H19 H 0.6359 0.6385 0.2655 0.036 Uiso 1 1 calc R . . C20 C 0.4995(2) 0.5440(2) 0.23491(13) 0.0273(6) Uani 1 1 d . . . H20 H 0.4993 0.5397 0.1929 0.033 Uiso 1 1 calc R . . C21 C 0.41758(19) 0.4913(2) 0.25485(11) 0.0229(5) Uani 1 1 d . . . C22 C 0.5731(2) 0.6296(3) 0.46673(13) 0.0360(7) Uani 1 1 d . . . H22A H 0.6447 0.6012 0.4698 0.054 Uiso 1 1 calc R . . H22B H 0.5599 0.6234 0.5072 0.054 Uiso 1 1 calc R . . H22C H 0.5674 0.7098 0.4536 0.054 Uiso 1 1 calc R . . C23 C 0.3365(2) 0.4122(2) 0.15180(12) 0.0298(6) Uani 1 1 d . . . H23A H 0.3303 0.4859 0.1304 0.045 Uiso 1 1 calc R . . H23B H 0.2773 0.3626 0.1300 0.045 Uiso 1 1 calc R . . H23C H 0.4041 0.3760 0.1524 0.045 Uiso 1 1 calc R . . C24 C 0.08131(19) 0.6712(2) 0.33164(11) 0.0206(5) Uani 1 1 d . . . C25 C 0.0047(2) 0.6009(2) 0.28959(11) 0.0257(6) Uani 1 1 d . . . H25 H 0.0267 0.5319 0.2747 0.031 Uiso 1 1 calc R . . C26 C -0.1034(2) 0.6332(3) 0.26998(13) 0.0322(6) Uani 1 1 d . . . H26 H -0.1541 0.5858 0.2423 0.039 Uiso 1 1 calc R . . C27 C -0.1364(2) 0.7361(3) 0.29146(14) 0.0345(7) Uani 1 1 d . . . H27 H -0.2089 0.7588 0.2773 0.041 Uiso 1 1 calc R . . C28 C -0.0623(2) 0.8047(3) 0.33369(14) 0.0334(6) Uani 1 1 d . . . H28 H -0.0852 0.8727 0.3489 0.040 Uiso 1 1 calc R . . C29 C 0.0474(2) 0.7733(2) 0.35404(13) 0.0254(6) Uani 1 1 d . . . H29 H 0.0974 0.8204 0.3824 0.030 Uiso 1 1 calc R . . C30 C 0.9742(3) 0.6144(3) 0.48418(17) 0.0563(9) Uani 1 1 d . . . H30 H 0.9568 0.6917 0.4731 0.068 Uiso 1 1 calc R . . C31 C 0.9265(3) 0.5260(4) 0.44303(17) 0.0592(10) Uani 1 1 d . . . H31 H 0.8763 0.5438 0.4045 0.071 Uiso 1 1 calc R . . C32 C 0.9535(3) 0.4113(3) 0.45911(17) 0.0553(10) Uani 1 1 d . . . H32 H 0.9223 0.3517 0.4312 0.066 Uiso 1 1 calc R . . C33 C 0.0892(3) 0.5662(3) 0.0266(2) 0.0663(12) Uani 1 1 d . . . H33 H 0.1498 0.6123 0.0446 0.080 Uiso 1 1 calc R . . C34 C 0.0028(4) 0.5691(4) 0.05011(17) 0.0620(11) Uani 1 1 d . . . H34 H 0.0054 0.6161 0.0848 0.074 Uiso 1 1 calc R . . C35 C -0.0874(3) 0.5046(3) 0.02373(18) 0.0554(9) Uani 1 1 d . . . H35 H -0.1471 0.5082 0.0395 0.067 Uiso 1 1 calc R . . Ni Ni 0.28727(3) 0.73383(3) 0.277228(14) 0.02034(12) Uani 1 1 d . . . O1 O 0.40014(13) 0.82090(15) 0.33608(8) 0.0227(4) Uani 1 1 d . . . O2 O 0.25159(15) 0.94544(15) 0.34514(8) 0.0286(4) Uani 1 1 d . . . O3 O 0.43947(16) 0.98744(16) 0.40569(8) 0.0321(4) Uani 1 1 d . . . O4 O 0.49462(14) 0.56188(16) 0.42153(8) 0.0287(4) Uani 1 1 d . . . O5 O 0.33315(14) 0.43042(15) 0.21557(8) 0.0265(4) Uani 1 1 d . . . P P 0.22653(5) 0.64564(5) 0.34743(3) 0.01698(15) Uani 1 1 d . . . S S 0.35850(5) 0.90079(5) 0.37736(3) 0.02110(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.086(3) 0.061(2) 0.0168(14) 0.0013(14) 0.0121(15) -0.029(2) C2A 0.047(3) 0.039(3) 0.0127(17) -0.0013(16) 0.0062(16) -0.0012(19) C2B 0.047(3) 0.039(3) 0.0127(17) -0.0013(16) 0.0062(16) -0.0012(19) C3 0.0417(17) 0.0451(18) 0.0184(13) -0.0038(12) 0.0011(12) -0.0083(14) C4 0.0141(11) 0.0202(12) 0.0193(11) -0.0014(9) 0.0041(9) 0.0032(10) C5 0.0186(12) 0.0202(12) 0.0183(11) -0.0002(9) 0.0050(9) 0.0020(10) C6 0.0224(13) 0.0282(14) 0.0240(13) -0.0050(10) 0.0051(10) -0.0017(11) C7 0.0269(14) 0.0385(16) 0.0166(12) -0.0036(11) 0.0028(11) 0.0050(12) C8 0.0347(15) 0.0302(15) 0.0215(12) 0.0046(11) 0.0098(11) 0.0049(12) C9 0.0300(14) 0.0227(13) 0.0229(12) 0.0013(10) 0.0096(11) -0.0001(11) C10 0.0215(12) 0.0178(12) 0.0184(11) -0.0009(9) 0.0042(9) -0.0007(10) C11 0.0209(12) 0.0198(13) 0.0178(11) -0.0026(9) 0.0014(9) -0.0020(10) C12 0.0262(14) 0.0211(14) 0.0298(13) -0.0046(11) 0.0046(11) 0.0038(11) C13 0.0430(17) 0.0176(13) 0.0326(15) 0.0002(11) 0.0066(13) -0.0014(12) C14 0.0365(16) 0.0246(14) 0.0323(14) 0.0041(11) 0.0111(12) -0.0086(12) C15 0.0244(13) 0.0206(13) 0.0300(13) -0.0002(10) 0.0081(11) -0.0023(11) C16 0.0163(12) 0.0167(12) 0.0273(12) -0.0004(10) 0.0045(10) 0.0020(10) C17 0.0209(13) 0.0198(13) 0.0272(13) -0.0028(10) 0.0055(10) 0.0040(10) C18 0.0188(13) 0.0219(14) 0.0415(15) -0.0041(11) 0.0037(11) -0.0002(11) C19 0.0215(14) 0.0247(14) 0.0462(16) -0.0013(12) 0.0148(12) -0.0023(11) C20 0.0276(14) 0.0251(14) 0.0327(14) -0.0011(11) 0.0143(11) 0.0014(11) C21 0.0189(13) 0.0197(13) 0.0298(13) -0.0029(10) 0.0062(10) 0.0016(10) C22 0.0343(16) 0.0359(16) 0.0301(14) -0.0088(12) -0.0027(12) -0.0033(13) C23 0.0330(15) 0.0317(15) 0.0261(13) -0.0079(11) 0.0108(11) -0.0030(12) C24 0.0184(12) 0.0209(13) 0.0219(12) -0.0004(10) 0.0049(9) 0.0000(10) C25 0.0233(13) 0.0257(14) 0.0259(13) -0.0046(10) 0.0034(11) 0.0002(11) C26 0.0194(13) 0.0353(16) 0.0361(15) -0.0052(12) -0.0011(11) -0.0064(12) C27 0.0149(13) 0.0370(17) 0.0469(18) 0.0002(13) 0.0014(12) 0.0022(12) C28 0.0240(14) 0.0276(15) 0.0474(17) -0.0060(13) 0.0084(13) 0.0052(12) C29 0.0189(13) 0.0221(14) 0.0327(14) -0.0071(10) 0.0036(11) -0.0013(10) C30 0.065(2) 0.056(2) 0.056(2) 0.0063(19) 0.031(2) -0.002(2) C31 0.049(2) 0.088(3) 0.0409(18) 0.0039(19) 0.0141(16) -0.001(2) C32 0.055(2) 0.059(2) 0.059(2) -0.0114(19) 0.0274(19) -0.0147(19) C33 0.042(2) 0.0306(19) 0.104(3) -0.002(2) -0.014(2) -0.0052(16) C34 0.070(3) 0.058(2) 0.0428(19) -0.0104(17) -0.0080(18) 0.024(2) C35 0.052(2) 0.053(2) 0.063(2) 0.0184(19) 0.0185(19) 0.0145(18) Ni 0.0247(2) 0.0192(2) 0.01705(18) -0.00114(11) 0.00588(14) -0.00158(13) O1 0.0238(9) 0.0219(9) 0.0235(9) -0.0021(7) 0.0087(7) -0.0043(7) O2 0.0290(10) 0.0230(10) 0.0309(10) 0.0040(8) 0.0040(8) 0.0060(8) O3 0.0386(11) 0.0284(10) 0.0291(10) -0.0072(8) 0.0096(8) -0.0159(9) O4 0.0267(10) 0.0303(10) 0.0267(9) -0.0062(8) 0.0037(8) -0.0049(8) O5 0.0246(9) 0.0313(10) 0.0242(9) -0.0071(7) 0.0079(7) -0.0050(8) P 0.0159(3) 0.0162(3) 0.0178(3) -0.0010(2) 0.0032(2) -0.0003(2) S 0.0240(3) 0.0177(3) 0.0207(3) -0.0019(2) 0.0051(2) -0.0042(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 C1 C2B 1.223(11) . ? C1 C2A 1.348(5) . ? C1 Ni 2.063(3) . ? C2A C2B 0.934(11) . ? C2A C3 1.391(5) . ? C2A Ni 1.992(4) . ? C2B C3 1.410(11) . ? C2B Ni 1.956(9) . ? C3 Ni 1.990(3) . ? C4 C9 1.394(3) . ? C4 C5 1.402(3) . ? C4 P 1.845(2) . ? C5 C6 1.389(3) . ? C5 S 1.780(2) . ? C6 C7 1.387(4) . ? C6 H6 0.9300 . ? C7 C8 1.371(4) . ? C7 H7 0.9300 . ? C8 C9 1.393(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C15 1.398(3) . ? C10 C11 1.402(3) . ? C10 P 1.824(2) . ? C11 C12 1.397(4) . ? C11 C16 1.497(3) . ? C12 C13 1.383(4) . ? C12 H12 0.9300 . ? C13 C14 1.384(4) . ? C13 H13 0.9300 . ? C14 C15 1.385(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.401(3) . ? C16 C21 1.407(3) . ? C17 O4 1.369(3) . ? C17 C18 1.391(4) . ? C18 C19 1.376(4) . ? C18 H18 0.9300 . ? C19 C20 1.381(4) . ? C19 H19 0.9300 . ? C20 C21 1.391(3) . ? C20 H20 0.9300 . ? C21 O5 1.369(3) . ? C22 O4 1.426(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O5 1.438(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C29 1.388(3) . ? C24 C25 1.398(3) . ? C24 P 1.820(2) . ? C25 C26 1.382(4) . ? C25 H25 0.9300 . ? C26 C27 1.383(4) . ? C26 H26 0.9300 . ? C27 C28 1.373(4) . ? C27 H27 0.9300 . ? C28 C29 1.397(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C32 1.360(5) 3_766 ? C30 C31 1.381(6) . ? C30 H30 0.9300 . ? C31 C32 1.380(5) . ? C31 H31 0.9300 . ? C32 C30 1.360(5) 3_766 ? C32 H32 0.9300 . ? C33 C34 1.356(6) . ? C33 C35 1.371(5) 3_565 ? C33 H33 0.9300 . ? C34 C35 1.357(6) . ? C34 H34 0.9300 . ? C35 C33 1.371(5) 3_565 ? C35 H35 0.9300 . ? Ni O1 1.9237(17) . ? Ni P 2.1768(8) . ? O1 S 1.4965(17) . ? O2 S 1.4459(19) . ? O3 S 1.4437(18) . ? 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 C2B C1 C2A 42.2(5) . . ? C2B C1 Ni 67.6(4) . . ? C2A C1 Ni 67.8(2) . . ? C2B C2A C1 61.7(7) . . ? C2B C2A C3 71.6(7) . . ? C1 C2A C3 126.3(4) . . ? C2B C2A Ni 74.2(6) . . ? C1 C2A Ni 73.5(2) . . ? C3 C2A Ni 69.49(18) . . ? C2A C2B C1 76.0(9) . . ? C2A C2B C3 69.5(7) . . ? C1 C2B C3 136.2(9) . . ? C2A C2B Ni 78.5(7) . . ? C1 C2B Ni 77.1(5) . . ? C3 C2B Ni 70.4(4) . . ? C2A C3 C2B 38.9(4) . . ? C2A C3 Ni 69.6(2) . . ? C2B C3 Ni 67.8(4) . . ? C9 C4 C5 118.3(2) . . ? C9 C4 P 119.17(19) . . ? C5 C4 P 122.53(17) . . ? C6 C5 C4 120.6(2) . . ? C6 C5 S 117.01(19) . . ? C4 C5 S 122.40(17) . . ? C7 C6 C5 120.0(2) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 120.2(2) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.2(2) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C4 C9 C8 120.7(2) . . ? C4 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C15 C10 C11 119.3(2) . . ? C15 C10 P 120.43(18) . . ? C11 C10 P 120.22(18) . . ? C12 C11 C10 118.8(2) . . ? C12 C11 C16 117.0(2) . . ? C10 C11 C16 124.1(2) . . ? C13 C12 C11 121.4(2) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 119.6(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 120.1(2) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.8(2) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C17 C16 C21 118.0(2) . . ? C17 C16 C11 120.6(2) . . ? C21 C16 C11 121.1(2) . . ? O4 C17 C18 124.3(2) . . ? O4 C17 C16 114.5(2) . . ? C18 C17 C16 121.2(2) . . ? C19 C18 C17 118.9(2) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 122.1(2) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C19 C20 C21 118.7(2) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? O5 C21 C20 123.6(2) . . ? O5 C21 C16 115.3(2) . . ? C20 C21 C16 121.0(2) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 119.3(2) . . ? C29 C24 P 118.50(18) . . ? C25 C24 P 121.36(18) . . ? C26 C25 C24 120.3(2) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.6(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C24 C29 C28 119.6(2) . . ? C24 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C32 C30 C31 120.2(4) 3_766 . ? C32 C30 H30 119.9 3_766 . ? C31 C30 H30 119.9 . . ? C32 C31 C30 119.9(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C30 C32 C31 119.8(4) 3_766 . ? C30 C32 H32 120.1 3_766 . ? C31 C32 H32 120.1 . . ? C34 C33 C35 120.2(4) . 3_565 ? C34 C33 H33 119.9 . . ? C35 C33 H33 119.9 3_565 . ? C33 C34 C35 121.0(4) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C33 118.9(4) . 3_565 ? C34 C35 H35 120.6 . . ? C33 C35 H35 120.6 3_565 . ? O1 Ni C2B 126.0(3) . . ? O1 Ni C3 167.80(10) . . ? C2B Ni C3 41.8(3) . . ? O1 Ni C2A 129.76(14) . . ? C2B Ni C2A 27.3(3) . . ? C3 Ni C2A 40.90(15) . . ? O1 Ni C1 94.33(11) . . ? C2B Ni C1 35.3(3) . . ? C3 Ni C1 74.15(13) . . ? C2A Ni C1 38.79(15) . . ? O1 Ni P 96.56(6) . . ? C2B Ni P 130.1(3) . . ? C3 Ni P 94.06(9) . . ? C2A Ni P 133.26(13) . . ? C1 Ni P 164.75(12) . . ? S O1 Ni 113.41(10) . . ? C17 O4 C22 117.9(2) . . ? C21 O5 C23 116.95(19) . . ? C24 P C10 106.34(11) . . ? C24 P C4 103.89(10) . . ? C10 P C4 104.60(11) . . ? C24 P Ni 110.32(8) . . ? C10 P Ni 117.87(8) . . ? C4 P Ni 112.69(8) . . ? O3 S O2 115.67(12) . . ? O3 S O1 110.22(10) . . ? O2 S O1 111.86(10) . . ? O3 S C5 107.30(11) . . ? O2 S C5 106.28(11) . . ? O1 S C5 104.74(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni C1 C2A C2B 80.6(6) . . . . ? C2B C1 C2A C3 -32.8(7) . . . . ? Ni C1 C2A C3 47.8(4) . . . . ? C2B C1 C2A Ni -80.6(6) . . . . ? C3 C2A C2B C1 152.6(5) . . . . ? Ni C2A C2B C1 79.4(3) . . . . ? C1 C2A C2B C3 -152.6(5) . . . . ? Ni C2A C2B C3 -73.2(2) . . . . ? C1 C2A C2B Ni -79.4(3) . . . . ? C3 C2A C2B Ni 73.2(2) . . . . ? Ni C1 C2B C2A -81.1(6) . . . . ? C2A C1 C2B C3 38.6(8) . . . . ? Ni C1 C2B C3 -42.5(9) . . . . ? C2A C1 C2B Ni 81.1(6) . . . . ? C1 C2A C3 C2B 30.2(6) . . . . ? Ni C2A C3 C2B 79.5(6) . . . . ? C2B C2A C3 Ni -79.5(6) . . . . ? C1 C2A C3 Ni -49.3(4) . . . . ? C1 C2B C3 C2A -40.3(9) . . . . ? Ni C2B C3 C2A -84.6(6) . . . . ? C2A C2B C3 Ni 84.6(6) . . . . ? C1 C2B C3 Ni 44.4(9) . . . . ? C9 C4 C5 C6 1.3(3) . . . . ? P C4 C5 C6 -177.90(18) . . . . ? C9 C4 C5 S -178.60(18) . . . . ? P C4 C5 S 2.2(3) . . . . ? C4 C5 C6 C7 -0.2(4) . . . . ? S C5 C6 C7 179.7(2) . . . . ? C5 C6 C7 C8 -0.5(4) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C5 C4 C9 C8 -1.8(4) . . . . ? P C4 C9 C8 177.4(2) . . . . ? C7 C8 C9 C4 1.2(4) . . . . ? C15 C10 C11 C12 -0.5(3) . . . . ? P C10 C11 C12 177.24(18) . . . . ? C15 C10 C11 C16 -176.7(2) . . . . ? P C10 C11 C16 1.1(3) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C16 C11 C12 C13 176.3(2) . . . . ? C11 C12 C13 C14 0.7(4) . . . . ? C12 C13 C14 C15 -0.5(4) . . . . ? C13 C14 C15 C10 -0.2(4) . . . . ? C11 C10 C15 C14 0.7(4) . . . . ? P C10 C15 C14 -177.0(2) . . . . ? C12 C11 C16 C17 -98.0(3) . . . . ? C10 C11 C16 C17 78.3(3) . . . . ? C12 C11 C16 C21 75.9(3) . . . . ? C10 C11 C16 C21 -107.9(3) . . . . ? C21 C16 C17 O4 -179.0(2) . . . . ? C11 C16 C17 O4 -4.9(3) . . . . ? C21 C16 C17 C18 -0.1(3) . . . . ? C11 C16 C17 C18 174.0(2) . . . . ? O4 C17 C18 C19 -180.0(2) . . . . ? C16 C17 C18 C19 1.2(4) . . . . ? C17 C18 C19 C20 -1.3(4) . . . . ? C18 C19 C20 C21 0.1(4) . . . . ? C19 C20 C21 O5 -179.8(2) . . . . ? C19 C20 C21 C16 1.1(4) . . . . ? C17 C16 C21 O5 179.7(2) . . . . ? C11 C16 C21 O5 5.7(3) . . . . ? C17 C16 C21 C20 -1.1(4) . . . . ? C11 C16 C21 C20 -175.1(2) . . . . ? C29 C24 C25 C26 0.7(4) . . . . ? P C24 C25 C26 -168.8(2) . . . . ? C24 C25 C26 C27 0.6(4) . . . . ? C25 C26 C27 C28 -1.8(4) . . . . ? C26 C27 C28 C29 1.8(5) . . . . ? C25 C24 C29 C28 -0.7(4) . . . . ? P C24 C29 C28 169.1(2) . . . . ? C27 C28 C29 C24 -0.5(4) . . . . ? C32 C30 C31 C32 -0.9(6) 3_766 . . . ? C30 C31 C32 C30 0.9(6) . . . 3_766 ? C35 C33 C34 C35 -1.4(6) 3_565 . . . ? C33 C34 C35 C33 1.4(6) . . . 3_565 ? C2A C2B Ni O1 108.5(7) . . . . ? C1 C2B Ni O1 30.4(7) . . . . ? C3 C2B Ni O1 -179.4(2) . . . . ? C2A C2B Ni C3 -72.1(7) . . . . ? C1 C2B Ni C3 -150.2(8) . . . . ? C1 C2B Ni C2A -78.1(8) . . . . ? C3 C2B Ni C2A 72.1(7) . . . . ? C2A C2B Ni C1 78.1(8) . . . . ? C3 C2B Ni C1 150.2(8) . . . . ? C2A C2B Ni P -108.7(7) . . . . ? C1 C2B Ni P 173.2(3) . . . . ? C3 C2B Ni P -36.6(6) . . . . ? C2A C3 Ni O1 44.2(6) . . . . ? C2B C3 Ni O1 2.3(7) . . . . ? C2A C3 Ni C2B 41.9(5) . . . . ? C2B C3 Ni C2A -41.9(5) . . . . ? C2A C3 Ni C1 24.5(3) . . . . ? C2B C3 Ni C1 -17.4(5) . . . . ? C2A C3 Ni P -165.3(2) . . . . ? C2B C3 Ni P 152.8(5) . . . . ? C2B C2A Ni O1 -93.1(8) . . . . ? C1 C2A Ni O1 -28.6(3) . . . . ? C3 C2A Ni O1 -168.96(17) . . . . ? C1 C2A Ni C2B 64.5(7) . . . . ? C3 C2A Ni C2B -75.9(8) . . . . ? C2B C2A Ni C3 75.9(8) . . . . ? C1 C2A Ni C3 140.4(4) . . . . ? C2B C2A Ni C1 -64.5(7) . . . . ? C3 C2A Ni C1 -140.4(4) . . . . ? C2B C2A Ni P 96.2(7) . . . . ? C1 C2A Ni P 160.7(2) . . . . ? C3 C2A Ni P 20.3(3) . . . . ? C2B C1 Ni O1 -155.8(6) . . . . ? C2A C1 Ni O1 158.4(3) . . . . ? C2A C1 Ni C2B -45.9(5) . . . . ? C2B C1 Ni C3 20.1(6) . . . . ? C2A C1 Ni C3 -25.7(3) . . . . ? C2B C1 Ni C2A 45.9(5) . . . . ? C2B C1 Ni P -20.2(8) . . . . ? C2A C1 Ni P -66.1(5) . . . . ? C2B Ni O1 S 92.6(4) . . . . ? C3 Ni O1 S 90.8(5) . . . . ? C2A Ni O1 S 127.16(19) . . . . ? C1 Ni O1 S 109.68(15) . . . . ? P Ni O1 S -59.63(10) . . . . ? C18 C17 O4 C22 5.9(4) . . . . ? C16 C17 O4 C22 -175.2(2) . . . . ? C20 C21 O5 C23 5.8(3) . . . . ? C16 C21 O5 C23 -175.0(2) . . . . ? C29 C24 P C10 147.3(2) . . . . ? C25 C24 P C10 -43.1(2) . . . . ? C29 C24 P C4 37.2(2) . . . . ? C25 C24 P C4 -153.2(2) . . . . ? C29 C24 P Ni -83.8(2) . . . . ? C25 C24 P Ni 85.8(2) . . . . ? C15 C10 P C24 -30.6(2) . . . . ? C11 C10 P C24 151.60(19) . . . . ? C15 C10 P C4 78.9(2) . . . . ? C11 C10 P C4 -98.8(2) . . . . ? C15 C10 P Ni -155.02(17) . . . . ? C11 C10 P Ni 27.2(2) . . . . ? C9 C4 P C24 75.5(2) . . . . ? C5 C4 P C24 -105.3(2) . . . . ? C9 C4 P C10 -35.8(2) . . . . ? C5 C4 P C10 143.4(2) . . . . ? C9 C4 P Ni -165.06(17) . . . . ? C5 C4 P Ni 14.1(2) . . . . ? O1 Ni P C24 125.21(10) . . . . ? C2B Ni P C24 -25.3(4) . . . . ? C3 Ni P C24 -48.78(13) . . . . ? C2A Ni P C24 -62.0(2) . . . . ? C1 Ni P C24 -10.1(4) . . . . ? O1 Ni P C10 -112.42(10) . . . . ? C2B Ni P C10 97.1(4) . . . . ? C3 Ni P C10 73.59(13) . . . . ? C2A Ni P C10 60.4(2) . . . . ? C1 Ni P C10 112.2(4) . . . . ? O1 Ni P C4 9.60(10) . . . . ? C2B Ni P C4 -140.9(4) . . . . ? C3 Ni P C4 -164.39(12) . . . . ? C2A Ni P C4 -177.6(2) . . . . ? C1 Ni P C4 -125.7(4) . . . . ? Ni O1 S O3 -162.39(10) . . . . ? Ni O1 S O2 -32.21(14) . . . . ? Ni O1 S C5 82.49(12) . . . . ? C6 C5 S O3 12.5(2) . . . . ? C4 C5 S O3 -167.6(2) . . . . ? C6 C5 S O2 -111.8(2) . . . . ? C4 C5 S O2 68.1(2) . . . . ? C6 C5 S O1 129.65(19) . . . . ? C4 C5 S O1 -50.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.83 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.266 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.097