# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1731 data_jd3_6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H29 Br N Ni P S' _chemical_formula_weight 677.25 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.8322(5) _cell_length_b 14.8477(7) _cell_length_c 19.7415(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.8990(10) _cell_angle_gamma 90.00 _cell_volume 3095.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method ? _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 2.063 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17906 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6929 _reflns_number_observed 4866 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6929 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_obs 0.0525 _refine_ls_wR_factor_all 0.1568 _refine_ls_wR_factor_obs 0.1363 _refine_ls_goodness_of_fit_all 0.971 _refine_ls_goodness_of_fit_obs 1.018 _refine_ls_restrained_S_all 0.971 _refine_ls_restrained_S_obs 1.018 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.43203(4) 0.28509(3) 0.12413(2) 0.03748(15) Uani 1 d . . Br1 Br 1.05952(5) 0.67542(4) 0.75715(2) 0.0750(2) Uani 1 d . . P1 P 0.26839(8) 0.35731(6) 0.06957(4) 0.0382(2) Uani 1 d . . S1 S 0.36761(10) 0.29383(8) 0.22112(5) 0.0539(3) Uani 1 d . . N1 N 0.7306(3) 0.4756(2) 0.4555(2) 0.0538(8) Uani 1 d . . C1 C 0.9527(4) 0.6128(3) 0.6826(2) 0.0489(9) Uani 1 d . . C2 C 0.9856(5) 0.6073(4) 0.6193(2) 0.0688(14) Uani 1 d . . H2 H 1.0527(41) 0.6372(30) 0.6136(21) 0.055(12) Uiso 1 d . . C3 C 0.9046(5) 0.5653(3) 0.5646(2) 0.0613(12) Uani 1 d . . H3 H 0.9297(38) 0.5554(28) 0.5229(23) 0.058(12) Uiso 1 d . . C4 C 0.7937(4) 0.5277(3) 0.5729(2) 0.0453(8) Uani 1 d . . C5 C 0.7641(5) 0.5316(4) 0.6374(2) 0.0625(12) Uani 1 d . . H5 H 0.6904(45) 0.5129(34) 0.6449(24) 0.074(15) Uiso 1 d . . C6 C 0.8444(5) 0.5750(3) 0.6920(2) 0.0633(12) Uani 1 d . . H6 H 0.8193(41) 0.5829(31) 0.7313(25) 0.067(13) Uiso 1 d . . C7 C 0.7056(4) 0.4842(3) 0.5145(2) 0.0496(9) Uani 1 d . . H7 H 0.6268(43) 0.4645(30) 0.5223(23) 0.067(14) Uiso 1 d . . C8 C 0.6420(4) 0.4319(3) 0.4010(2) 0.0462(9) Uani 1 d . . C9 C 0.6514(4) 0.4493(3) 0.3334(2) 0.0578(11) Uani 1 d . . H9 H 0.7053(52) 0.4959(40) 0.3254(28) 0.096(18) Uiso 1 d . . C10 C 0.5701(4) 0.4093(3) 0.2776(2) 0.0552(11) Uani 1 d . . H10 H 0.5723(37) 0.4235(27) 0.2379(22) 0.050(11) Uiso 1 d . . C11 C 0.4791(4) 0.3487(3) 0.2872(2) 0.0450(8) Uani 1 d . . C12 C 0.4729(4) 0.3290(3) 0.3556(2) 0.0532(10) Uani 1 d . . H12 H 0.4115(44) 0.2904(31) 0.3610(24) 0.063(13) Uiso 1 d . . C13 C 0.5519(4) 0.3708(3) 0.4110(2) 0.0526(10) Uani 1 d . . H13 H 0.5415(38) 0.3575(28) 0.4578(22) 0.057(11) Uiso 1 d . . C14 C 0.6202(4) 0.2959(4) 0.1116(3) 0.0659(12) Uani 1 d . . H14 H 0.6635(45) 0.3507(35) 0.1210(24) 0.071(15) Uiso 1 d . . C15 C 0.6123(4) 0.2327(4) 0.1620(3) 0.0663(13) Uani 1 d . . H15 H 0.6545(41) 0.2344(30) 0.2080(24) 0.060(12) Uiso 1 d . . C16 C 0.5349(5) 0.1600(4) 0.1307(3) 0.0688(13) Uani 1 d . . H16 H 0.5130(54) 0.1145(39) 0.1552(28) 0.093(19) Uiso 1 d . . C17 C 0.4878(5) 0.1801(4) 0.0631(3) 0.0645(13) Uani 1 d . . H17 H 0.4361(41) 0.1462(31) 0.0301(24) 0.062(12) Uiso 1 d . . C18 C 0.5369(4) 0.2656(4) 0.0498(3) 0.0650(13) Uani 1 d . . H18 H 0.5219(49) 0.2908(34) 0.0121(28) 0.075(17) Uiso 1 d . . C191 C 0.2650(4) 0.4695(3) 0.1069(2) 0.0475(9) Uani 1 d . . C192 C 0.3734(5) 0.5209(3) 0.1148(3) 0.0691(13) Uani 1 d . . H192 H 0.4377(48) 0.5004(37) 0.1046(28) 0.081(18) Uiso 1 d . . C193 C 0.3829(5) 0.6050(3) 0.1454(3) 0.0777(15) Uani 1 d . . H193 H 0.4622(52) 0.6399(40) 0.1531(28) 0.094(17) Uiso 1 d . . C194 C 0.2839(5) 0.6358(4) 0.1716(3) 0.0775(15) Uani 1 d . . H194 H 0.2863(49) 0.6953(37) 0.1982(28) 0.088(16) Uiso 1 d . . C195 C 0.1749(6) 0.5875(3) 0.1633(3) 0.0719(14) Uani 1 d . . H195 H 0.1050(49) 0.6091(36) 0.1776(26) 0.082(16) Uiso 1 d . . C196 C 0.1642(5) 0.5028(3) 0.1303(2) 0.0599(11) Uani 1 d . . H196 H 0.0840(44) 0.4714(32) 0.1236(23) 0.068(14) Uiso 1 d . . C201 C 0.1163(3) 0.3019(3) 0.0678(2) 0.0425(8) Uani 1 d . . C202 C 0.1123(4) 0.2237(3) 0.1052(2) 0.0504(9) Uani 1 d . . H202 H 0.1851(37) 0.2011(25) 0.1364(20) 0.042(10) Uiso 1 d . . C203 C -0.0021(5) 0.1791(3) 0.1012(3) 0.0600(11) Uani 1 d . . H203 H -0.0015(41) 0.1257(31) 0.1322(21) 0.059(12) Uiso 1 d . . C204 C -0.1118(4) 0.2126(4) 0.0597(3) 0.0647(13) Uani 1 d . . H204 H -0.1830(40) 0.1808(25) 0.0573(19) 0.043(10) Uiso 1 d . . C205 C -0.1082(4) 0.2900(4) 0.0223(3) 0.0669(13) Uani 1 d . . H205 H -0.1784(45) 0.3128(30) -0.0080(24) 0.065(13) Uiso 1 d . . C206 C 0.0041(4) 0.3348(3) 0.0255(2) 0.0560(10) Uani 1 d . . H206 H 0.0116(49) 0.3994(36) 0.0026(26) 0.089(16) Uiso 1 d . . C211 C 0.2548(3) 0.3789(3) -0.0232(2) 0.0448(8) Uani 1 d . . C212 C 0.2323(6) 0.4616(4) -0.0538(3) 0.0752(14) Uani 1 d . . H212 H 0.2129(35) 0.5051(27) -0.0278(20) 0.041(10) Uiso 1 d . . C213 C 0.2140(7) 0.4719(5) -0.1256(3) 0.102(2) Uani 1 d . . H213 H 0.1900(64) 0.5329(50) -0.1360(36) 0.128(24) Uiso 1 d . . C214 C 0.2239(6) 0.3997(5) -0.1657(3) 0.095(2) Uani 1 d . . H214 H 0.2360(56) 0.4026(40) -0.2097(34) 0.108(20) Uiso 1 d . . C215 C 0.2463(6) 0.3161(4) -0.1374(2) 0.0777(15) Uani 1 d . . H215 H 0.2569(52) 0.2565(45) -0.1667(30) 0.111(21) Uiso 1 d . . C216 C 0.2608(5) 0.3058(3) -0.0658(2) 0.0604(11) Uani 1 d . . H216 H 0.2652(49) 0.2442(40) -0.0472(27) 0.089(17) Uiso 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 Ni 0.0348(3) 0.0437(3) 0.0315(2) -0.0038(2) 0.0025(2) 0.0006(2) Br1 0.0821(4) 0.0819(4) 0.0486(3) -0.0140(2) -0.0116(2) -0.0113(3) P1 0.0359(5) 0.0390(5) 0.0375(4) -0.0056(4) 0.0035(3) 0.0000(4) S1 0.0506(6) 0.0761(7) 0.0340(5) -0.0076(4) 0.0072(4) -0.0174(5) N1 0.061(2) 0.060(2) 0.037(2) -0.0021(15) 0.0014(14) -0.012(2) C1 0.054(2) 0.052(2) 0.034(2) -0.006(2) -0.004(2) -0.001(2) C2 0.071(3) 0.084(3) 0.052(2) -0.012(2) 0.014(2) -0.038(3) C3 0.077(3) 0.074(3) 0.034(2) -0.007(2) 0.016(2) -0.026(2) C4 0.049(2) 0.045(2) 0.039(2) -0.002(2) 0.006(2) -0.002(2) C5 0.053(3) 0.084(3) 0.053(2) -0.013(2) 0.017(2) -0.012(2) C6 0.072(3) 0.084(3) 0.035(2) -0.012(2) 0.014(2) -0.002(2) C7 0.049(2) 0.052(2) 0.044(2) -0.003(2) 0.001(2) -0.003(2) C8 0.053(2) 0.049(2) 0.032(2) -0.003(2) 0.0008(15) -0.003(2) C9 0.068(3) 0.060(3) 0.044(2) -0.002(2) 0.010(2) -0.023(2) C10 0.070(3) 0.064(3) 0.030(2) -0.001(2) 0.007(2) -0.017(2) C11 0.047(2) 0.054(2) 0.032(2) -0.004(2) 0.0053(15) 0.001(2) C12 0.055(2) 0.068(3) 0.038(2) 0.000(2) 0.012(2) -0.020(2) C13 0.060(2) 0.066(3) 0.030(2) 0.003(2) 0.007(2) -0.015(2) C14 0.039(2) 0.078(3) 0.082(3) -0.009(3) 0.015(2) -0.001(2) C15 0.047(3) 0.085(4) 0.057(3) -0.004(2) -0.007(2) 0.017(2) C16 0.064(3) 0.060(3) 0.078(3) 0.000(3) 0.007(3) 0.019(2) C17 0.059(3) 0.070(3) 0.061(3) -0.026(2) 0.007(2) 0.012(2) C18 0.051(3) 0.099(4) 0.050(3) -0.003(3) 0.023(2) 0.017(3) C191 0.047(2) 0.041(2) 0.051(2) -0.009(2) 0.004(2) 0.006(2) C192 0.050(3) 0.057(3) 0.095(4) -0.024(2) 0.004(2) 0.002(2) C193 0.061(3) 0.052(3) 0.113(4) -0.029(3) 0.003(3) -0.007(2) C194 0.083(4) 0.058(3) 0.083(4) -0.023(3) 0.001(3) 0.000(3) C195 0.082(4) 0.059(3) 0.081(3) -0.010(2) 0.031(3) 0.016(3) C196 0.063(3) 0.057(3) 0.061(3) -0.011(2) 0.016(2) 0.001(2) C201 0.033(2) 0.049(2) 0.044(2) -0.011(2) 0.0068(15) -0.0013(15) C202 0.045(2) 0.053(2) 0.050(2) -0.011(2) 0.005(2) -0.004(2) C203 0.063(3) 0.056(3) 0.066(3) -0.014(2) 0.025(2) -0.015(2) C204 0.035(2) 0.073(3) 0.088(3) -0.031(3) 0.018(2) -0.011(2) C205 0.038(2) 0.079(3) 0.080(3) -0.016(3) 0.004(2) 0.005(2) C206 0.040(2) 0.060(3) 0.065(3) -0.007(2) 0.005(2) 0.003(2) C211 0.044(2) 0.046(2) 0.041(2) 0.000(2) 0.0009(15) -0.005(2) C212 0.105(4) 0.051(3) 0.061(3) 0.000(2) -0.002(3) -0.008(3) C213 0.147(6) 0.072(4) 0.069(4) 0.027(3) -0.013(3) -0.030(4) C214 0.123(5) 0.107(5) 0.044(3) 0.007(3) -0.002(3) -0.048(4) C215 0.096(4) 0.088(4) 0.042(2) -0.010(3) 0.000(2) -0.011(3) C216 0.076(3) 0.062(3) 0.037(2) -0.005(2) 0.001(2) -0.001(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 C18 2.067(4) . ? Ni C15 2.080(4) . ? Ni C14 2.114(5) . ? Ni C17 2.138(4) . ? Ni P1 2.1447(10) . ? Ni C16 2.156(5) . ? Ni S1 2.1834(10) . ? Br1 C1 1.900(4) . ? P1 C191 1.826(4) . ? P1 C211 1.833(4) . ? P1 C201 1.835(4) . ? S1 C11 1.766(4) . ? N1 C7 1.261(5) . ? N1 C8 1.427(4) . ? C1 C6 1.350(6) . ? C1 C2 1.376(6) . ? C2 C3 1.380(6) . ? C3 C4 1.368(6) . ? C4 C5 1.382(6) . ? C4 C7 1.471(5) . ? C5 C6 1.383(6) . ? C8 C13 1.379(5) . ? C8 C9 1.385(5) . ? C9 C10 1.383(6) . ? C10 C11 1.379(6) . ? C11 C12 1.398(5) . ? C12 C13 1.377(5) . ? C14 C15 1.384(7) . ? C14 C18 1.419(7) . ? C15 C16 1.420(7) . ? C16 C17 1.353(7) . ? C17 C18 1.422(8) . ? C191 C196 1.370(6) . ? C191 C192 1.380(6) . ? C192 C193 1.381(6) . ? C193 C194 1.369(7) . ? C194 C195 1.359(7) . ? C195 C196 1.408(7) . ? C201 C202 1.382(6) . ? C201 C206 1.400(5) . ? C202 C203 1.393(6) . ? C203 C204 1.377(7) . ? C204 C205 1.372(8) . ? C205 C206 1.375(6) . ? C211 C212 1.367(6) . ? C211 C216 1.384(6) . ? C212 C213 1.394(8) . ? C213 C214 1.351(9) . ? C214 C215 1.362(8) . ? C215 C216 1.394(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 Ni C15 65.3(2) . . ? C18 Ni C14 39.7(2) . . ? C15 Ni C14 38.5(2) . . ? C18 Ni C17 39.5(2) . . ? C15 Ni C17 64.5(2) . . ? C14 Ni C17 65.7(2) . . ? C18 Ni P1 103.7(2) . . ? C15 Ni P1 166.4(2) . . ? C14 Ni P1 127.9(2) . . ? C17 Ni P1 112.77(14) . . ? C18 Ni C16 64.1(2) . . ? C15 Ni C16 39.1(2) . . ? C14 Ni C16 64.7(2) . . ? C17 Ni C16 36.7(2) . . ? P1 Ni C16 145.04(14) . . ? C18 Ni S1 164.79(15) . . ? C15 Ni S1 99.53(15) . . ? C14 Ni S1 127.14(15) . . ? C17 Ni S1 136.4(2) . . ? P1 Ni S1 91.18(4) . . ? C16 Ni S1 105.1(2) . . ? C191 P1 C211 103.8(2) . . ? C191 P1 C201 108.5(2) . . ? C211 P1 C201 100.8(2) . . ? C191 P1 Ni 110.04(12) . . ? C211 P1 Ni 117.55(13) . . ? C201 P1 Ni 115.06(13) . . ? C11 S1 Ni 112.04(13) . . ? C7 N1 C8 119.8(4) . . ? C6 C1 C2 120.6(4) . . ? C6 C1 Br1 119.7(3) . . ? C2 C1 Br1 119.7(3) . . ? C1 C2 C3 119.3(4) . . ? C4 C3 C2 120.8(4) . . ? C3 C4 C5 119.0(4) . . ? C3 C4 C7 121.2(3) . . ? C5 C4 C7 119.8(4) . . ? C4 C5 C6 120.1(4) . . ? C1 C6 C5 120.1(4) . . ? N1 C7 C4 122.3(4) . . ? C13 C8 C9 117.9(3) . . ? C13 C8 N1 124.7(3) . . ? C9 C8 N1 117.4(4) . . ? C10 C9 C8 121.1(4) . . ? C11 C10 C9 121.2(4) . . ? C10 C11 C12 117.3(3) . . ? C10 C11 S1 126.3(3) . . ? C12 C11 S1 116.4(3) . . ? C13 C12 C11 121.2(4) . . ? C12 C13 C8 121.1(3) . . ? C15 C14 C18 105.9(5) . . ? C15 C14 Ni 69.4(3) . . ? C18 C14 Ni 68.4(3) . . ? C14 C15 C16 109.2(5) . . ? C14 C15 Ni 72.1(3) . . ? C16 C15 Ni 73.3(3) . . ? C17 C16 C15 108.4(5) . . ? C17 C16 Ni 70.9(3) . . ? C15 C16 Ni 67.5(3) . . ? C16 C17 C18 107.8(5) . . ? C16 C17 Ni 72.3(3) . . ? C18 C17 Ni 67.6(2) . . ? C14 C18 C17 108.4(5) . . ? C14 C18 Ni 71.9(3) . . ? C17 C18 Ni 72.9(3) . . ? C196 C191 C192 119.0(4) . . ? C196 C191 P1 123.7(3) . . ? C192 C191 P1 117.2(3) . . ? C191 C192 C193 121.9(5) . . ? C194 C193 C192 118.6(5) . . ? C195 C194 C193 120.7(5) . . ? C194 C195 C196 120.4(5) . . ? C191 C196 C195 119.2(5) . . ? C202 C201 C206 119.0(4) . . ? C202 C201 P1 120.1(3) . . ? C206 C201 P1 120.8(3) . . ? C201 C202 C203 120.2(4) . . ? C204 C203 C202 120.0(5) . . ? C205 C204 C203 119.9(4) . . ? C204 C205 C206 120.8(5) . . ? C205 C206 C201 120.0(5) . . ? C212 C211 C216 117.7(4) . . ? C212 C211 P1 124.5(3) . . ? C216 C211 P1 117.8(3) . . ? C211 C212 C213 121.2(5) . . ? C214 C213 C212 119.8(6) . . ? C213 C214 C215 120.8(5) . . ? C214 C215 C216 119.1(5) . . ? C211 C216 C215 121.3(5) . . ? _refine_diff_density_max 0.584 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.067 #============================================================================== data_4c #============================================================================== _audit_creation_date 'Oct 6 17:51:34 1999' _audit_creation_method 'PLATON option' #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. James Darkwa' _publ_contact_author_address ; Department of Chemistry University of the Western Cape South Africa ; _publ_contact_author_email 'Jdarkwa@uwc.ac.za' _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal ? _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ? #=============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address ? ; ? ; #=============================================================================== _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H44 N Ni P S' _chemical_formula_structural ? _chemical_formula_sum 'C31 H44 N Ni P S' _chemical_formula_weight 552.40 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 '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' N N 0.0061 0.0033 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.8090(3) _cell_length_b 10.9160(4) _cell_length_c 14.4300(6) _cell_angle_alpha 80.813(2) _cell_angle_beta 73.796(2) _cell_angle_gamma 68.446(2) _cell_volume 1517.53(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 333 _cell_measurement_theta_min 2 _cell_measurement_theta_max 18 _cell_special_details ; ? ; _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_size_rad 0.13 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.78 _exptl_crystal_density_meas_temp 'Not Measured' _exptl_absorpt_correction_type 'Semi-empirical' _exptl_absorpt_process_details ; A data set with a high redundancy was collected. Variation in intensity due to absorption were corrected by allow the scale factor to vary. ; _exptl_absorpt_correction_T_min 'Not Measured' _exptl_absorpt_correction_T_max 'Not Measured' #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 207 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number_diffrn_reflns_number 6774 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6774 _reflns_number_gt 5710 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_full ? _diffrn_reflns_reduction_process ; The 4 sets of data were scaled using Denzo-SMN. Unit cell dimensions were refined on all data. ; _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo-SMN (Z.Otwinowski and W.Minor,1997)' _computing_data_reduction 'Denzo-SMN (Z.Otwinowski and W.Minor,1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.1131P)^2^+4.1902P] 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 SHELXL _refine_ls_extinction_coef 0.002(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6774 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 1.450 _refine_ls_shift/su_mean 0.113 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.53 _refine_diff_density_max 3.270 _refine_diff_density_min -3.048 _refine_diff_density_rms 0.089 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Ni1 Ni Uani 0.18810 0.55000 0.23360 1.000 0.0292 S1B S Uani 0.26673 0.68028 0.12344 1.000 0.0370 P1 P Uani 0.37820 0.39115 0.20291 1.000 0.0301 N1B N Uani 0.00278 0.81296 -0.21178 1.000 0.0390 C1 C Uani 0.00178 0.69044 0.30181 1.000 0.0555 C2 C Uani -0.02989 0.60758 0.25101 1.000 0.0490 C3 C Uani 0.01903 0.47851 0.28885 1.000 0.0422 C4 C Uani 0.08084 0.48142 0.36358 1.000 0.0424 C5 C Uani 0.06169 0.61309 0.37558 1.000 0.0507 C6 C Uani 0.18182 0.71666 0.02908 1.000 0.0324 C7 C Uani 0.13448 0.63023 -0.00025 1.000 0.0371 C8 C Uani 0.07684 0.66201 -0.07916 1.000 0.0380 C9 C Uani 0.06150 0.78447 -0.13071 1.000 0.0355 C10 C Uani 0.10998 0.87112 -0.10287 1.000 0.0392 C11 C Uani 0.16930 0.83756 -0.02451 1.000 0.0385 C12 C Uani -0.07342 0.93082 -0.22768 1.000 0.0393 C13 C Uani -0.12579 0.97579 -0.31490 1.000 0.0367 C14 C Uani -0.09456 0.89377 -0.38931 1.000 0.0392 C15 C Uani -0.13950 0.94403 -0.47295 1.000 0.0432 C16 C Uani -0.21518 1.07780 -0.48542 1.000 0.0429 C17 C Uani -0.24775 1.15763 -0.41137 1.000 0.0455 C18 C Uani -0.20440 1.10873 -0.32689 1.000 0.0444 C19 C Uani -0.26039 1.13264 -0.57785 1.000 0.0641 C20 C Uani 0.38747 0.24448 0.28593 1.000 0.0383 C21 C Uani 0.51885 0.12413 0.26487 1.000 0.0488 C22 C Uani 0.51274 0.01079 0.33841 1.000 0.0802 C23 C Uani 0.35004 0.23213 -0.03359 1.000 0.0749 C24 C Uani 0.42054 0.33213 0.08262 1.000 0.0413 C25 C Uani 0.32861 0.26084 0.07150 1.000 0.0454 C26 C Uani 0.64214 -0.11048 0.31977 1.000 0.1166 C27 C Uani 0.28240 0.14342 -0.04426 1.000 0.1473 C28 C Uani 0.52763 0.43164 0.20367 1.000 0.0352 C29 C Uani 0.52270 0.47338 0.30142 1.000 0.0392 C30 C Uani 0.64790 0.50523 0.30207 1.000 0.0446 C31 C Uani 0.64805 0.53600 0.40046 1.000 0.0530 H1 H Uiso -0.01466 0.78043 0.28811 1.000 0.0666 H2 H Uiso -0.07532 0.63535 0.20132 1.000 0.0589 H3 H Uiso 0.01272 0.40434 0.26923 1.000 0.0506 H4 H Uiso 0.12654 0.40788 0.39878 1.000 0.0509 H5 H Uiso 0.08441 0.64296 0.42326 1.000 0.0609 H6 H Uiso 0.23104 0.31202 0.09932 1.000 0.0439 H7 H Uiso 0.14172 0.54912 0.03398 1.000 0.0446 H8 H Uiso 0.04808 0.60140 -0.09807 1.000 0.0456 H10 H Uiso 0.10256 0.95226 -0.13707 1.000 0.0470 H11 H Uiso 0.20146 0.89668 -0.00718 1.000 0.0462 H12 H Uiso -0.09698 0.99134 -0.18163 1.000 0.0472 H14 H Uiso -0.04321 0.80478 -0.38258 1.000 0.0470 H15 H Uiso -0.11908 0.88808 -0.52155 1.000 0.0518 H17 H Uiso -0.29999 1.24635 -0.41811 1.000 0.0546 H18 H Uiso -0.22777 1.16475 -0.27778 1.000 0.0533 H19A H Uiso -0.22363 1.20126 -0.60720 1.000 0.0961 H19B H Uiso -0.22770 1.06350 -0.62142 1.000 0.0961 H19C H Uiso -0.35863 1.16813 -0.56381 1.000 0.0961 H20A H Uiso 0.31101 0.21746 0.28699 1.000 0.0460 H20B H Uiso 0.37462 0.26963 0.35038 1.000 0.0460 H22A H Uiso 0.49814 0.03925 0.40213 1.000 0.0963 H22B H Uiso 0.43492 -0.01330 0.33821 1.000 0.0963 H23A H Uiso 0.44754 0.19365 -0.06146 1.000 0.0899 H23B H Uiso 0.31602 0.31491 -0.07007 1.000 0.0899 H24A H Uiso 0.51478 0.27269 0.06844 1.000 0.0495 H24B H Uiso 0.41395 0.40680 0.03540 1.000 0.0495 H26A H Uiso 0.63302 -0.17868 0.36943 1.000 0.1750 H26B H Uiso 0.65523 -0.14154 0.25795 1.000 0.1750 H26C H Uiso 0.71966 -0.08760 0.32019 1.000 0.1750 H27A H Uiso 0.29802 0.13187 -0.11164 1.000 0.2209 H27B H Uiso 0.31891 0.05946 -0.01131 1.000 0.2209 H27C H Uiso 0.18575 0.18053 -0.01685 1.000 0.2209 H28 H Uiso 0.33708 0.18037 0.11108 1.000 0.0582 H28A H Uiso 0.53498 0.50265 0.15498 1.000 0.0423 H28B H Uiso 0.60931 0.35530 0.18592 1.000 0.0423 H29 H Uiso 0.60117 0.14766 0.26012 1.000 0.0481 H29A H Uiso 0.51419 0.40286 0.35030 1.000 0.0471 H29B H Uiso 0.44170 0.55046 0.31879 1.000 0.0471 H30 H Uiso 0.53893 0.09861 0.20301 1.000 0.0754 H30A H Uiso 0.65229 0.58040 0.25690 1.000 0.0535 H30B H Uiso 0.72944 0.43070 0.27973 1.000 0.0535 H31A H Uiso 0.72928 0.55546 0.39605 1.000 0.0794 H31B H Uiso 0.56867 0.61090 0.42257 1.000 0.0794 H31C H Uiso 0.64630 0.46118 0.44528 1.000 0.0794 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 0.0254 0.0294 0.0283 -0.0020 -0.0020 -0.0074 S1B 0.0406 0.0403 0.0338 0.0046 -0.0105 -0.0196 P1 0.0242 0.0313 0.0313 -0.0044 -0.0015 -0.0083 N1B 0.0434 0.0401 0.0338 0.0026 -0.0098 -0.0162 C1 0.0280 0.0357 0.0824 -0.0136 0.0106 -0.0011 C2 0.0237 0.0566 0.0570 0.0021 -0.0066 -0.0071 C3 0.0308 0.0468 0.0468 -0.0054 0.0045 -0.0200 C4 0.0362 0.0477 0.0328 0.0050 0.0057 -0.0156 C5 0.0458 0.0625 0.0375 -0.0198 0.0108 -0.0197 C6 0.0329 0.0313 0.0279 -0.0005 -0.0030 -0.0088 C7 0.0415 0.0315 0.0375 0.0042 -0.0101 -0.0136 C8 0.0439 0.0339 0.0375 -0.0014 -0.0091 -0.0157 C9 0.0367 0.0352 0.0308 -0.0005 -0.0055 -0.0104 C10 0.0443 0.0313 0.0397 0.0068 -0.0097 -0.0142 C11 0.0437 0.0317 0.0408 0.0010 -0.0100 -0.0152 C12 0.0421 0.0398 0.0353 -0.0045 -0.0083 -0.0130 C13 0.0388 0.0350 0.0367 -0.0010 -0.0105 -0.0124 C14 0.0449 0.0316 0.0421 0.0002 -0.0124 -0.0138 C15 0.0493 0.0426 0.0426 -0.0044 -0.0146 -0.0180 C16 0.0448 0.0452 0.0439 0.0052 -0.0192 -0.0182 C17 0.0461 0.0325 0.0589 -0.0004 -0.0216 -0.0091 C18 0.0482 0.0361 0.0501 -0.0096 -0.0173 -0.0090 C19 0.0709 0.0658 0.0606 0.0065 -0.0371 -0.0178 C20 0.0321 0.0328 0.0488 0.0025 -0.0099 -0.0116 C21 0.0430 0.0365 0.0644 -0.0084 -0.0190 -0.0042 C22 0.0547 0.0387 0.1464 0.0272 -0.0389 -0.0177 C23 0.0909 0.0876 0.0594 -0.0300 -0.0059 -0.0441 C24 0.0331 0.0488 0.0366 -0.0144 0.0028 -0.0114 C25 0.0495 0.0428 0.0461 -0.0124 -0.0080 -0.0169 C26 0.1110 0.0366 0.2066 -0.0016 -0.0869 0.0033 C27 0.1411 0.1990 0.1319 -0.0812 -0.0013 -0.0866 C28 0.0286 0.0366 0.0376 -0.0032 -0.0032 -0.0109 C29 0.0320 0.0429 0.0414 -0.0070 -0.0035 -0.0134 C30 0.0405 0.0524 0.0434 -0.0025 -0.0056 -0.0222 C31 0.0478 0.0671 0.0529 -0.0099 -0.0097 -0.0292 #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1B 2.1642 . . yes Ni1 P1 2.1318 . . yes Ni1 C1 2.1170 . . yes Ni1 C2 2.1545 . . yes Ni1 C3 2.1495 . . yes Ni1 C4 2.0972 . . yes Ni1 C5 2.1761 . . yes S1B C6 1.7639 . . yes P1 C20 1.8289 . . yes P1 C24 1.8261 . . yes P1 C28 1.8277 . . yes N1B C9 1.4217 . . yes N1B C12 1.2724 . . yes C1 C2 1.4325 . . no C1 C5 1.4006 . . no C2 C3 1.3896 . . no C3 C4 1.4280 . . no C4 C5 1.4069 . . no C6 C7 1.3907 . . no C6 C11 1.3997 . . no C7 C8 1.3842 . . no C8 C9 1.3987 . . no C9 C10 1.3906 . . no C10 C11 1.3870 . . no C12 C13 1.4634 . . no C13 C14 1.3968 . . no C13 C18 1.3978 . . no C14 C15 1.3834 . . no C15 C16 1.3979 . . no C16 C17 1.3738 . . no C16 C19 1.5065 . . no C17 C18 1.3848 . . no C20 C21 1.5332 . . no C21 C22 1.5043 . . no C22 C26 1.5246 . . no C23 C25 1.5342 . . no C23 C27 1.4583 . . no C24 C25 1.5217 . . no C28 C29 1.5316 . . no C29 C30 1.5187 . . no C30 C31 1.5107 . . no C1 H1 0.9300 . . no C2 H2 0.9300 . . no C3 H3 0.9300 . . no C4 H4 0.9300 . . no C5 H5 0.9300 . . no C7 H7 0.9300 . . no C8 H8 0.9300 . . no C10 H10 0.9300 . . no C11 H11 0.9300 . . no C12 H12 0.9300 . . no C14 H14 0.9300 . . no C15 H15 0.9300 . . no C17 H17 0.9300 . . no C18 H18 0.9300 . . no C19 H19A 0.9600 . . no C19 H19B 0.9600 . . no C19 H19C 0.9600 . . no C20 H20A 0.9700 . . no C20 H20B 0.9700 . . no C21 H29 0.9953 . . no C21 H30 0.9210 . . no C22 H22A 0.9700 . . no C22 H22B 0.9700 . . no C23 H23A 0.9700 . . no C23 H23B 0.9700 . . no C24 H24A 0.9700 . . no C24 H24B 0.9700 . . no C25 H6 0.9940 . . no C25 H28 0.9572 . . no C26 H26A 0.9600 . . no C26 H26B 0.9600 . . no C26 H26C 0.9600 . . no C27 H27A 0.9600 . . no C27 H27B 0.9600 . . no C27 H27C 0.9600 . . no C28 H28A 0.9700 . . no C28 H28B 0.9700 . . no C29 H29A 0.9700 . . no C29 H29B 0.9700 . . no C30 H30A 0.9700 . . no C30 H30B 0.9700 . . no C31 H31A 0.9600 . . no C31 H31B 0.9600 . . no C31 H31C 0.9600 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1B Ni1 P1 92.00 . . . yes S1B Ni1 C1 98.89 . . . yes S1B Ni1 C2 109.29 . . . yes S1B Ni1 C3 143.72 . . . yes S1B Ni1 C4 161.17 . . . yes S1B Ni1 C5 122.85 . . . yes P1 Ni1 C1 165.02 . . . yes P1 Ni1 C2 144.65 . . . yes P1 Ni1 C3 111.27 . . . yes P1 Ni1 C4 102.78 . . . yes P1 Ni1 C5 126.99 . . . yes C1 Ni1 C2 39.18 . . . yes C1 Ni1 C3 64.78 . . . yes C1 Ni1 C4 64.62 . . . yes C1 Ni1 C5 38.05 . . . yes C2 Ni1 C3 37.67 . . . yes C2 Ni1 C4 64.34 . . . yes C2 Ni1 C5 64.13 . . . yes C3 Ni1 C4 39.27 . . . yes C3 Ni1 C5 64.61 . . . yes C4 Ni1 C5 38.39 . . . yes Ni1 S1B C6 109.40 . . . yes Ni1 P1 C20 114.80 . . . yes Ni1 P1 C24 113.02 . . . yes Ni1 P1 C28 114.64 . . . yes C20 P1 C24 105.10 . . . yes C20 P1 C28 104.64 . . . yes C24 P1 C28 103.46 . . . yes C9 N1B C12 118.20 . . . yes Ni1 C1 C2 71.83 . . . yes Ni1 C1 C5 73.26 . . . yes C2 C1 C5 108.49 . . . no Ni1 C2 C1 69.00 . . . yes Ni1 C2 C3 70.97 . . . yes C1 C2 C3 108.16 . . . no Ni1 C3 C2 71.36 . . . yes Ni1 C3 C4 68.39 . . . yes C2 C3 C4 106.96 . . . no Ni1 C4 C3 72.34 . . . yes Ni1 C4 C5 73.84 . . . yes C3 C4 C5 109.26 . . . no Ni1 C5 C1 68.69 . . . yes Ni1 C5 C4 67.77 . . . yes C1 C5 C4 106.71 . . . no S1B C6 C7 124.68 . . . yes S1B C6 C11 117.76 . . . yes C7 C6 C11 117.41 . . . no C6 C7 C8 121.59 . . . no C7 C8 C9 120.57 . . . no N1B C9 C8 118.86 . . . yes N1B C9 C10 122.70 . . . yes C8 C9 C10 118.38 . . . no C9 C10 C11 120.56 . . . no C6 C11 C10 121.46 . . . no N1B C12 C13 123.19 . . . yes C12 C13 C14 123.05 . . . no C12 C13 C18 118.53 . . . no C14 C13 C18 118.33 . . . no C13 C14 C15 120.44 . . . no C14 C15 C16 120.90 . . . no C15 C16 C17 118.46 . . . no C15 C16 C19 120.62 . . . no C17 C16 C19 120.91 . . . no C16 C17 C18 121.36 . . . no C13 C18 C17 120.49 . . . no P1 C20 C21 117.40 . . . yes C20 C21 C22 111.87 . . . no C21 C22 C26 113.22 . . . no C25 C23 C27 114.02 . . . no P1 C24 C25 113.83 . . . yes C23 C25 C24 112.99 . . . no P1 C28 C29 113.77 . . . yes C28 C29 C30 113.59 . . . no C29 C30 C31 113.50 . . . no Ni1 C1 H1 120.89 . . . no C2 C1 H1 125.76 . . . no C5 C1 H1 125.76 . . . no Ni1 C2 H2 125.69 . . . no C1 C2 H2 125.92 . . . no C3 C2 H2 125.92 . . . no Ni1 C3 H3 125.31 . . . no C2 C3 H3 126.52 . . . no C4 C3 H3 126.52 . . . no Ni1 C4 H4 120.16 . . . no C3 C4 H4 125.37 . . . no C5 C4 H4 125.37 . . . no Ni1 C5 H5 128.42 . . . no C1 C5 H5 126.65 . . . no C4 C5 H5 126.65 . . . no C6 C7 H7 119.21 . . . no C8 C7 H7 119.21 . . . no C7 C8 H8 119.71 . . . no C9 C8 H8 119.71 . . . no C9 C10 H10 119.72 . . . no C11 C10 H10 119.72 . . . no C6 C11 H11 119.27 . . . no C10 C11 H11 119.27 . . . no N1B C12 H12 118.40 . . . no C13 C12 H12 118.40 . . . no C13 C14 H14 119.78 . . . no C15 C14 H14 119.78 . . . no C14 C15 H15 119.55 . . . no C16 C15 H15 119.55 . . . no C16 C17 H17 119.32 . . . no C18 C17 H17 119.32 . . . no C13 C18 H18 119.76 . . . no C17 C18 H18 119.76 . . . no C16 C19 H19A 109.47 . . . no C16 C19 H19B 109.47 . . . no C16 C19 H19C 109.47 . . . no H19A C19 H19B 109.47 . . . no H19A C19 H19C 109.47 . . . no H19B C19 H19C 109.47 . . . no P1 C20 H20A 107.95 . . . no P1 C20 H20B 107.95 . . . no C21 C20 H20A 107.95 . . . no C21 C20 H20B 107.95 . . . no H20A C20 H20B 107.22 . . . no C20 C21 H29 111.16 . . . no C20 C21 H30 111.79 . . . no C22 C21 H29 111.06 . . . no C22 C21 H30 111.11 . . . no H29 C21 H30 99.24 . . . no C21 C22 H22A 108.93 . . . no C21 C22 H22B 108.93 . . . no C26 C22 H22A 108.93 . . . no C26 C22 H22B 108.93 . . . no H22A C22 H22B 107.75 . . . no C25 C23 H23A 108.75 . . . no C25 C23 H23B 108.75 . . . no C27 C23 H23A 108.75 . . . no C27 C23 H23B 108.75 . . . no H23A C23 H23B 107.65 . . . no P1 C24 H24A 108.79 . . . no P1 C24 H24B 108.79 . . . no C25 C24 H24A 108.79 . . . no C25 C24 H24B 108.79 . . . no H24A C24 H24B 107.67 . . . no C23 C25 H6 110.84 . . . no C23 C25 H28 108.78 . . . no C24 C25 H6 110.02 . . . no C24 C25 H28 113.66 . . . no H6 C25 H28 99.81 . . . no C22 C26 H26A 109.47 . . . no C22 C26 H26B 109.47 . . . no C22 C26 H26C 109.47 . . . no H26A C26 H26B 109.47 . . . no H26A C26 H26C 109.47 . . . no H26B C26 H26C 109.47 . . . no C23 C27 H27A 109.47 . . . no C23 C27 H27B 109.47 . . . no C23 C27 H27C 109.47 . . . no H27A C27 H27B 109.47 . . . no H27A C27 H27C 109.47 . . . no H27B C27 H27C 109.47 . . . no P1 C28 H28A 108.81 . . . no P1 C28 H28B 108.81 . . . no C29 C28 H28A 108.80 . . . no C29 C28 H28B 108.81 . . . no H28A C28 H28B 107.68 . . . no C28 C29 H29A 108.85 . . . no C28 C29 H29B 108.85 . . . no C30 C29 H29A 108.85 . . . no C30 C29 H29B 108.85 . . . no H29A C29 H29B 107.70 . . . no C29 C30 H30A 108.87 . . . no C29 C30 H30B 108.87 . . . no C31 C30 H30A 108.87 . . . no C31 C30 H30B 108.87 . . . no H30A C30 H30B 107.71 . . . no C30 C31 H31A 109.47 . . . no C30 C31 H31B 109.47 . . . no C30 C31 H31C 109.47 . . . no H31A C31 H31B 109.47 . . . no H31A C31 H31C 109.47 . . . no H31B C31 H31C 109.47 . . . no 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 P1 Ni1 S1B C6 112.60 . . . . no C1 Ni1 S1B C6 -77.72 . . . . no C2 Ni1 S1B C6 -38.67 . . . . no C3 Ni1 S1B C6 -18.77 . . . . no C5 Ni1 S1B C6 -109.75 . . . . no S1B Ni1 P1 C20 173.46 . . . . no C2 Ni1 P1 C20 -58.19 . . . . no C3 Ni1 P1 C20 -35.01 . . . . no C4 Ni1 P1 C20 5.21 . . . . no C5 Ni1 P1 C20 38.56 . . . . no S1B Ni1 P1 C24 -66.00 . . . . no C2 Ni1 P1 C24 62.35 . . . . no C3 Ni1 P1 C24 85.53 . . . . no C4 Ni1 P1 C24 125.76 . . . . no C5 Ni1 P1 C24 159.10 . . . . no S1B Ni1 P1 C28 52.24 . . . . no C2 Ni1 P1 C28 -179.40 . . . . no C3 Ni1 P1 C28 -156.22 . . . . no C4 Ni1 P1 C28 -116.00 . . . . no C5 Ni1 P1 C28 -82.65 . . . . no S1B Ni1 C1 C2 109.72 . . . . no C3 Ni1 C1 C2 -36.19 . . . . no C4 Ni1 C1 C2 -79.84 . . . . no C5 Ni1 C1 C2 -116.57 . . . . no S1B Ni1 C1 C5 -133.71 . . . . no C2 Ni1 C1 C5 116.57 . . . . no C3 Ni1 C1 C5 80.37 . . . . no C4 Ni1 C1 C5 36.73 . . . . no C5 Ni1 C2 C3 -81.27 . . . . no P1 Ni1 C4 C3 -108.08 . . . . no C1 Ni1 C4 C3 80.51 . . . . no C2 Ni1 C4 C3 36.89 . . . . no C5 Ni1 C4 C3 116.92 . . . . no P1 Ni1 C4 C5 135.00 . . . . no S1B Ni1 C2 C1 -80.19 . . . . no P1 Ni1 C2 C1 155.95 . . . . no C3 Ni1 C2 C1 119.05 . . . . no C4 Ni1 C2 C1 80.60 . . . . no C5 Ni1 C2 C1 37.78 . . . . no S1B Ni1 C2 C3 160.76 . . . . no P1 Ni1 C2 C3 36.89 . . . . no C1 Ni1 C2 C3 -119.05 . . . . no C4 Ni1 C2 C3 -38.45 . . . . no C2 Ni1 C5 C1 -38.90 . . . . no C4 Ni1 C5 C1 -119.53 . . . . no S1B Ni1 C5 C4 177.75 . . . . no P1 Ni1 C5 C4 -59.68 . . . . no S1B Ni1 C3 C2 -31.71 . . . . no P1 Ni1 C3 C2 -158.11 . . . . no C1 Ni1 C3 C2 37.62 . . . . no C4 Ni1 C3 C2 117.69 . . . . no C5 Ni1 C3 C2 79.89 . . . . no S1B Ni1 C3 C4 -149.40 . . . . no P1 Ni1 C3 C4 84.20 . . . . no C1 Ni1 C3 C4 -80.07 . . . . no C2 Ni1 C3 C4 -117.69 . . . . no C5 Ni1 C3 C4 -37.80 . . . . no P1 Ni1 C5 C1 -179.21 . . . . no C1 Ni1 C4 C5 -36.41 . . . . no C3 Ni1 C5 C1 -80.86 . . . . no C3 Ni1 C4 C5 -116.92 . . . . no C2 Ni1 C5 C4 80.63 . . . . no S1B Ni1 C5 C1 58.22 . . . . no C1 Ni1 C5 C4 119.53 . . . . no C3 Ni1 C5 C4 38.67 . . . . no C2 Ni1 C4 C5 -80.03 . . . . no Ni1 S1B C6 C7 -32.69 . . . . no Ni1 S1B C6 C11 151.87 . . . . no C28 P1 C24 C25 165.95 . . . . no C20 P1 C28 C29 -65.29 . . . . no C24 P1 C28 C29 -175.13 . . . . no Ni1 P1 C24 C25 -69.47 . . . . no Ni1 P1 C28 C29 61.34 . . . . no C20 P1 C24 C25 56.46 . . . . no Ni1 P1 C20 C21 177.00 . . . . no C24 P1 C20 C21 52.19 . . . . no C28 P1 C20 C21 -56.46 . . . . no C9 N1B C12 C13 172.25 . . . . no C12 N1B C9 C8 144.50 . . . . no C12 N1B C9 C10 -38.39 . . . . no C2 C1 C5 C4 6.40 . . . . no C5 C1 C2 C3 -4.15 . . . . no C2 C1 C5 Ni1 63.64 . . . . no Ni1 C1 C2 C3 60.43 . . . . no C5 C1 C2 Ni1 -64.57 . . . . no Ni1 C1 C5 C4 -57.24 . . . . no C1 C2 C3 Ni1 -59.19 . . . . no C1 C2 C3 C4 0.20 . . . . no Ni1 C2 C3 C4 59.39 . . . . no C2 C3 C4 Ni1 -61.30 . . . . no Ni1 C3 C4 C5 65.12 . . . . no C2 C3 C4 C5 3.82 . . . . no C3 C4 C5 C1 -6.34 . . . . no C3 C4 C5 Ni1 -64.16 . . . . no Ni1 C4 C5 C1 57.82 . . . . no S1B C6 C11 C10 176.82 . . . . no C7 C6 C11 C10 1.05 . . . . no C11 C6 C7 C8 -0.14 . . . . no S1B C6 C7 C8 -175.59 . . . . no C6 C7 C8 C9 -1.54 . . . . no C7 C8 C9 N1B 179.53 . . . . no C7 C8 C9 C10 2.28 . . . . no C8 C9 C10 C11 -1.39 . . . . no N1B C9 C10 C11 -178.52 . . . . no C9 C10 C11 C6 -0.28 . . . . no N1B C12 C13 C14 -1.25 . . . . no N1B C12 C13 C18 -177.55 . . . . no C12 C13 C18 C17 175.34 . . . . no C14 C13 C18 C17 -1.14 . . . . no C18 C13 C14 C15 0.68 . . . . no C12 C13 C14 C15 -175.62 . . . . no C13 C14 C15 C16 0.91 . . . . no C14 C15 C16 C17 -2.03 . . . . no C14 C15 C16 C19 178.26 . . . . no C19 C16 C17 C18 -178.71 . . . . no C15 C16 C17 C18 1.58 . . . . no C16 C17 C18 C13 -0.02 . . . . no P1 C20 C21 C22 -179.92 . . . . no C20 C21 C22 C26 -179.80 . . . . no C27 C23 C25 C24 169.35 . . . . no P1 C24 C25 C23 170.59 . . . . no P1 C28 C29 C30 179.26 . . . . no C28 C29 C30 C31 -175.48 . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni1 H6 3.3072 . . no Ni1 H7 3.0606 . . no Ni1 H29B 3.3043 . . no Ni1 H18 3.4719 . 2_575 no S1B H24B 3.1066 . . no S1B H28A 2.9493 . . no S1B H18 2.8557 . 2_575 no N1B H14 2.6675 . . no N1B H3 2.7090 . 2_565 no C2 C7 3.5784 . . no C7 C2 3.5784 . . no C14 C15 3.5842 . 2_574 no C14 C16 3.4321 . 2_574 no C15 C15 3.5050 . 2_574 no C15 C14 3.5842 . 2_574 no C16 C14 3.4321 . 2_574 no C1 H26C 3.0928 . 1_465 no C2 H31A 3.0245 . 1_455 no C3 H31A 2.9471 . 1_455 no C8 H27C 2.8127 . 2_565 no C9 H27C 2.8559 . 2_565 no C10 H12 2.6084 . . no C11 H24A 3.0866 . 2_665 no C12 H10 2.6824 . . no C14 H20A 2.9521 . 2_565 no C16 H22B 2.9299 . 2_565 no C17 H22B 2.8824 . 2_565 no C18 H22B 3.0836 . 2_565 no C19 H29 3.0633 . 1_464 no C20 H4 2.9078 . . no C20 H28 2.9603 . . no C20 H29A 2.9480 . . no C21 H24A 3.0356 . . no C21 H28B 2.9825 . . no C24 H30 2.9297 . . no C25 H20A 3.0324 . . no C26 H19B 3.0742 . 1_646 no C26 H27A 2.9192 . 2_655 no C27 H11 3.0522 . 1_545 no C27 H26B 2.9687 . 2_655 no C28 H29 2.9411 . . no C29 H20B 3.0806 . . no C31 H26A 3.0250 . 1_565 no H3 N1B 2.7090 . 2_565 no H3 H14 2.5594 . 2_565 no H4 C20 2.9078 . . no H4 H20B 2.5047 . . no H6 Ni1 3.3072 . . no H6 H7 2.5324 . . no H7 Ni1 3.0606 . . no H7 H6 2.5324 . . no H10 C12 2.6824 . . no H10 H12 2.2929 . . no H11 C27 3.0522 . 1_565 no H11 H27B 2.5207 . 1_565 no H12 C10 2.6084 . . no H12 H10 2.2929 . . no H12 H18 2.4076 . . no H14 N1B 2.6675 . . no H14 H3 2.5594 . 2_565 no H15 H19B 2.3523 . . no H17 H29B 2.5716 . 2_575 no H18 H12 2.4076 . . no H18 Ni1 3.4719 . 2_575 no H18 S1B 2.8557 . 2_575 no H19B C26 3.0742 . 1_464 no H19B H15 2.3523 . . no H19B H26C 2.2704 . 1_464 no H20A C25 3.0324 . . no H20A H22B 2.4828 . . no H20A H28 2.5557 . . no H20A C14 2.9521 . 2_565 no H20B C29 3.0806 . . no H20B H4 2.5047 . . no H20B H22A 2.4809 . . no H20B H29A 2.4498 . . no H22A H20B 2.4809 . . no H22B H20A 2.4828 . . no H22B C16 2.9299 . 2_565 no H22B C17 2.8824 . 2_565 no H22B C18 3.0836 . 2_565 no H23A H24A 2.5541 . . no H23B H24B 2.5710 . . no H24A C21 3.0356 . . no H24A H23A 2.5541 . . no H24A H30 2.4879 . . no H24A C11 3.0866 . 2_665 no H24B S1B 3.1066 . . no H24B H23B 2.5710 . . no H26A C31 3.0250 . 1_545 no H26A H31B 2.5809 . 1_545 no H26B H30 2.5597 . . no H26B C27 2.9687 . 2_655 no H26B H27A 2.0240 . 2_655 no H26C C1 3.0928 . 1_645 no H26C H19B 2.2704 . 1_646 no H26C H29 2.5453 . . no H27A C26 2.9192 . 2_655 no H27A H26B 2.0240 . 2_655 no H27B H11 2.5207 . 1_545 no H27B H28 2.4552 . . no H27C C8 2.8127 . 2_565 no H27C C9 2.8559 . 2_565 no H28 C20 2.9603 . . no H28 H20A 2.5557 . . no H28 H27B 2.4552 . . no H28A S1B 2.9493 . . no H28A H30A 2.5926 . . no H28B C21 2.9825 . . no H28B H29 2.3688 . . no H28B H30B 2.5136 . . no H29 C19 3.0633 . 1_646 no H29 C28 2.9411 . . no H29 H26C 2.5453 . . no H29 H28B 2.3688 . . no H29A C20 2.9480 . . no H29A H20B 2.4498 . . no H29A H31C 2.5222 . . no H29B Ni1 3.3043 . . no H29B H31B 2.5863 . . no H29B H17 2.5716 . 2_575 no H30 C24 2.9297 . . no H30 H24A 2.4879 . . no H30 H26B 2.5597 . . no H30A H28A 2.5926 . . no H30B H28B 2.5136 . . no H31A C2 3.0245 . 1_655 no H31A C3 2.9471 . 1_655 no H31B H26A 2.5809 . 1_565 no H31B H29B 2.5863 . . no H31C H29A 2.5222 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C18 H18 S1B 0.9300 2.8557 3.7805 173.00 2_575 yes # End of Crystallographic Information File