# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email abya@iitk.ac.in _publ_contact_author_name 'Sabyasachi Sarkar' loop_ _publ_author_name 'Sabyasachi Sarkar' 'Ameerunisha Begum' 'Sumit Sonkar' 'Manav Saxena' data_13maycm _database_code_depnum_ccdc_archive 'CCDC 834592' #TrackingRef '- 13maycm.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H32 Ni O8.25 P S4' _chemical_formula_sum 'C36 H32 Ni O8.25 P S4' _chemical_formula_weight 814.54 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 10.844(5) _cell_length_b 10.972(5) _cell_length_c 15.617(5) _cell_angle_alpha 85.742(5) _cell_angle_beta 82.695(5) _cell_angle_gamma 82.424(5) _cell_volume 1823.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 811 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.96 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.652 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _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 scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8593 _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_av_sigmaI/netI 0.2270 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6251 _reflns_number_gt 2786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1620P)^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 6251 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2066 _refine_ls_R_factor_gt 0.0999 _refine_ls_wR_factor_ref 0.3109 _refine_ls_wR_factor_gt 0.2311 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 1.0000 0.0000 0.0280(6) Uani 1 2 d S . . Ni2 Ni 0.0000 0.5000 0.5000 0.0302(6) Uani 1 2 d S . . S1 S 0.3754(3) 0.9059(3) 0.0915(2) 0.0329(8) Uani 1 1 d . . . S2 S 0.6430(3) 0.9747(3) 0.0841(2) 0.0335(8) Uani 1 1 d . . . S3 S 0.1857(3) 0.4393(3) 0.4417(2) 0.0364(8) Uani 1 1 d . . . S4 S -0.0643(3) 0.3320(3) 0.4749(2) 0.0388(8) Uani 1 1 d . . . O1 O 0.7255(9) 0.9383(10) 0.2659(7) 0.064(3) Uani 1 1 d . . . O2 O 0.6369(8) 0.7625(7) 0.2885(5) 0.034(2) Uani 1 1 d . . . O3 O 0.3264(9) 0.7303(9) 0.2562(6) 0.053(3) Uani 1 1 d . . . O4 O 0.3907(9) 0.8763(8) 0.3260(6) 0.047(2) Uani 1 1 d . . . O5 O 0.3623(10) 0.1607(10) 0.4177(7) 0.063(3) Uani 1 1 d . . . O6 O 0.3239(9) 0.2482(8) 0.2891(6) 0.049(2) Uani 1 1 d . . . O7 O 0.1371(9) 0.0634(8) 0.3487(6) 0.051(3) Uani 1 1 d . . . O8 O -0.0608(9) 0.0925(8) 0.4160(6) 0.051(3) Uani 1 1 d . . . O9 O 0.410(4) 0.979(5) 0.554(3) 0.085(15) Uani 0.25 1 d P . . P1 P 0.8080(3) 0.4618(3) 0.1536(2) 0.0304(8) Uani 1 1 d . . . C1 C 0.4557(11) 0.8716(10) 0.1775(7) 0.030(3) Uani 1 1 d . . . C2 C 0.5770(11) 0.8979(10) 0.1753(8) 0.032(3) Uani 1 1 d . . . C3 C 0.3849(11) 0.8176(12) 0.2555(9) 0.036(3) Uani 1 1 d . . . C4 C 0.3256(17) 0.8313(15) 0.4070(9) 0.083(6) Uani 1 1 d . . . H4A H 0.3370 0.8814 0.4526 0.124 Uiso 1 1 calc R . . H4B H 0.3590 0.7475 0.4201 0.124 Uiso 1 1 calc R . . H4C H 0.2379 0.8355 0.4019 0.124 Uiso 1 1 calc R . . C5 C 0.6550(12) 0.8684(13) 0.2467(9) 0.042(3) Uani 1 1 d . . . C6 C 0.6954(13) 0.7322(13) 0.3685(8) 0.045(3) Uani 1 1 d . . . H6A H 0.6756 0.6532 0.3928 0.068 Uiso 1 1 calc R . . H6B H 0.6642 0.7937 0.4092 0.068 Uiso 1 1 calc R . . H6C H 0.7846 0.7299 0.3558 0.068 Uiso 1 1 calc R . . C7 C 0.1756(10) 0.2975(10) 0.4080(7) 0.027(3) Uani 1 1 d . . . C8 C 0.0640(11) 0.2494(10) 0.4208(8) 0.030(3) Uani 1 1 d . . . C9 C 0.0534(12) 0.1277(12) 0.3909(8) 0.039(3) Uani 1 1 d . . . C10 C -0.0768(15) -0.0283(12) 0.3907(10) 0.060(4) Uani 1 1 d . . . H10A H -0.1603 -0.0459 0.4110 0.090 Uiso 1 1 calc R . . H10B H -0.0176 -0.0892 0.4157 0.090 Uiso 1 1 calc R . . H10C H -0.0631 -0.0300 0.3289 0.090 Uiso 1 1 calc R . . C11 C 0.2953(14) 0.2251(14) 0.3716(9) 0.047(4) Uani 1 1 d . . . C12 C 0.4384(14) 0.1742(13) 0.2542(10) 0.064(5) Uani 1 1 d . . . H12A H 0.4555 0.1947 0.1934 0.096 Uiso 1 1 calc R . . H12B H 0.4282 0.0885 0.2632 0.096 Uiso 1 1 calc R . . H12C H 0.5070 0.1907 0.2831 0.096 Uiso 1 1 calc R . . C13 C 0.7341(10) 0.5015(11) 0.0580(7) 0.031(3) Uani 1 1 d . . . C14 C 0.6613(11) 0.6170(10) 0.0483(8) 0.031(3) Uani 1 1 d . . . H14 H 0.6516 0.6727 0.0915 0.037 Uiso 1 1 calc R . . C15 C 0.6041(11) 0.6467(10) -0.0267(8) 0.031(3) Uani 1 1 d . . . H15 H 0.5552 0.7223 -0.0333 0.038 Uiso 1 1 calc R . . C16 C 0.6191(11) 0.5663(11) -0.0903(9) 0.037(3) Uani 1 1 d . . . H16 H 0.5808 0.5881 -0.1401 0.044 Uiso 1 1 calc R . . C17 C 0.6917(12) 0.4503(11) -0.0824(8) 0.037(3) Uani 1 1 d . . . H17 H 0.7020 0.3959 -0.1264 0.044 Uiso 1 1 calc R . . C18 C 0.7461(11) 0.4206(10) -0.0091(7) 0.033(3) Uani 1 1 d . . . H18 H 0.7930 0.3438 -0.0028 0.039 Uiso 1 1 calc R . . C19 C 0.9083(11) 0.3185(11) 0.1436(7) 0.031(3) Uani 1 1 d . . . C20 C 0.8578(12) 0.2117(11) 0.1434(9) 0.042(3) Uani 1 1 d . . . H20 H 0.7712 0.2135 0.1490 0.050 Uiso 1 1 calc R . . C21 C 0.9323(12) 0.1017(13) 0.1350(9) 0.048(4) Uani 1 1 d . . . H21 H 0.8965 0.0290 0.1360 0.057 Uiso 1 1 calc R . . C22 C 1.0609(11) 0.0991(11) 0.1250(8) 0.038(3) Uani 1 1 d . . . H22 H 1.1120 0.0245 0.1189 0.045 Uiso 1 1 calc R . . C23 C 1.1130(11) 0.2059(11) 0.1241(9) 0.042(3) Uani 1 1 d . . . H23 H 1.1998 0.2032 0.1161 0.050 Uiso 1 1 calc R . . C24 C 1.0403(11) 0.3174(11) 0.1347(8) 0.034(3) Uani 1 1 d . . . H24 H 1.0763 0.3895 0.1360 0.041 Uiso 1 1 calc R . . C25 C 0.8991(11) 0.5814(10) 0.1694(8) 0.034(3) Uani 1 1 d . . . C26 C 0.9219(11) 0.6750(10) 0.1080(8) 0.033(3) Uani 1 1 d . . . H26 H 0.8855 0.6811 0.0568 0.039 Uiso 1 1 calc R . . C27 C 0.9987(11) 0.7593(11) 0.1230(8) 0.032(3) Uani 1 1 d . . . H27 H 1.0160 0.8204 0.0803 0.039 Uiso 1 1 calc R . . C28 C 1.0501(11) 0.7565(11) 0.1978(8) 0.036(3) Uani 1 1 d . . . H28 H 1.0969 0.8182 0.2074 0.043 Uiso 1 1 calc R . . C29 C 1.0329(12) 0.6609(12) 0.2607(8) 0.042(3) Uani 1 1 d . . . H29 H 1.0728 0.6557 0.3104 0.050 Uiso 1 1 calc R . . C30 C 0.9553(12) 0.5733(13) 0.2486(9) 0.045(3) Uani 1 1 d . . . H30 H 0.9403 0.5109 0.2909 0.053 Uiso 1 1 calc R . . C31 C 0.6949(12) 0.4414(11) 0.2441(7) 0.034(3) Uani 1 1 d . . . C32 C 0.5743(10) 0.5025(11) 0.2514(8) 0.031(3) Uani 1 1 d . . . H32 H 0.5480 0.5557 0.2063 0.038 Uiso 1 1 calc R . . C33 C 0.4912(12) 0.4844(12) 0.3270(8) 0.040(3) Uani 1 1 d . . . H33 H 0.4100 0.5251 0.3311 0.048 Uiso 1 1 calc R . . C34 C 0.5282(12) 0.4087(13) 0.3934(8) 0.043(3) Uani 1 1 d . . . H34 H 0.4730 0.4003 0.4436 0.052 Uiso 1 1 calc R . . C35 C 0.6512(13) 0.3407(16) 0.3881(9) 0.068(5) Uani 1 1 d . . . H35 H 0.6759 0.2870 0.4335 0.081 Uiso 1 1 calc R . . C36 C 0.7335(12) 0.3580(15) 0.3120(10) 0.059(4) Uani 1 1 d . . . H36 H 0.8134 0.3145 0.3063 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0216(12) 0.0264(12) 0.0369(12) -0.0060(10) -0.0044(10) -0.0035(9) Ni2 0.0235(12) 0.0323(13) 0.0359(12) -0.0079(10) -0.0043(10) -0.0039(9) S1 0.0255(17) 0.0303(17) 0.0421(18) -0.0003(14) -0.0060(14) -0.0001(13) S2 0.0288(17) 0.0349(18) 0.0385(17) -0.0043(14) -0.0070(14) -0.0063(13) S3 0.0282(18) 0.0339(18) 0.0471(19) -0.0094(15) 0.0000(15) -0.0040(13) S4 0.0294(18) 0.0395(19) 0.049(2) -0.0088(16) -0.0025(15) -0.0069(14) O1 0.051(6) 0.075(8) 0.077(7) 0.035(6) -0.042(6) -0.039(6) O2 0.044(5) 0.028(5) 0.032(4) -0.004(4) -0.020(4) 0.000(4) O3 0.051(6) 0.051(6) 0.059(6) 0.013(5) -0.004(5) -0.030(5) O4 0.057(6) 0.035(5) 0.042(5) 0.000(4) 0.011(5) 0.002(4) O5 0.052(7) 0.074(8) 0.064(7) -0.035(6) -0.005(6) 0.006(6) O6 0.050(6) 0.045(6) 0.052(6) -0.029(5) 0.012(5) -0.006(4) O7 0.060(7) 0.031(5) 0.062(6) -0.019(5) -0.002(5) -0.001(5) O8 0.044(6) 0.048(6) 0.065(6) -0.026(5) -0.007(5) -0.012(5) O9 0.05(3) 0.14(4) 0.07(3) 0.01(3) -0.02(3) -0.04(3) P1 0.0249(17) 0.0299(18) 0.0369(18) -0.0041(14) -0.0052(14) -0.0023(13) C1 0.024(6) 0.032(7) 0.032(6) -0.012(5) 0.005(5) 0.002(5) C2 0.036(7) 0.025(6) 0.036(7) -0.016(5) 0.002(6) -0.007(5) C3 0.019(7) 0.036(8) 0.049(8) -0.006(7) -0.003(6) 0.010(6) C4 0.118(15) 0.057(11) 0.054(10) 0.014(8) 0.050(11) -0.009(10) C5 0.030(8) 0.051(9) 0.042(8) -0.008(7) 0.001(6) 0.002(6) C6 0.048(9) 0.046(8) 0.048(8) -0.003(7) -0.024(7) -0.010(7) C7 0.017(6) 0.025(6) 0.037(7) -0.007(5) -0.003(5) 0.006(5) C8 0.034(7) 0.016(6) 0.042(7) -0.010(5) -0.010(6) -0.002(5) C9 0.034(8) 0.046(8) 0.039(7) -0.001(7) -0.016(6) -0.003(6) C10 0.081(12) 0.036(8) 0.070(10) -0.018(8) -0.012(9) -0.022(8) C11 0.046(9) 0.054(10) 0.045(9) -0.014(7) -0.011(8) -0.005(7) C12 0.063(11) 0.049(9) 0.077(11) -0.038(9) 0.021(9) -0.002(8) C13 0.021(6) 0.037(7) 0.034(7) 0.001(6) -0.002(5) 0.003(5) C14 0.030(7) 0.028(7) 0.035(7) -0.008(5) -0.007(6) 0.005(5) C15 0.028(7) 0.020(6) 0.046(7) -0.006(6) -0.007(6) 0.000(5) C16 0.035(8) 0.026(7) 0.050(8) -0.005(6) -0.005(6) -0.008(6) C17 0.040(8) 0.036(7) 0.037(7) -0.016(6) -0.014(6) -0.002(6) C18 0.039(8) 0.022(6) 0.037(7) -0.015(6) 0.002(6) -0.003(5) C19 0.028(7) 0.030(7) 0.035(7) 0.003(5) -0.011(6) 0.002(5) C20 0.031(8) 0.034(8) 0.061(9) -0.001(7) -0.018(7) 0.000(6) C21 0.024(7) 0.043(8) 0.071(10) 0.013(7) -0.003(7) 0.005(6) C22 0.032(7) 0.019(6) 0.063(9) 0.004(6) -0.013(7) -0.001(5) C23 0.022(7) 0.034(8) 0.068(9) 0.011(7) -0.008(7) 0.001(6) C24 0.030(7) 0.032(7) 0.042(7) 0.004(6) -0.012(6) -0.006(5) C25 0.031(7) 0.024(7) 0.049(8) -0.008(6) -0.015(6) 0.000(5) C26 0.023(6) 0.028(7) 0.043(7) 0.003(6) 0.000(6) 0.006(5) C27 0.025(7) 0.027(7) 0.047(8) -0.007(6) -0.004(6) -0.004(5) C28 0.028(7) 0.029(7) 0.056(8) -0.013(6) -0.010(6) -0.009(5) C29 0.040(8) 0.049(9) 0.042(8) -0.004(7) -0.018(6) -0.015(6) C30 0.039(8) 0.047(9) 0.048(8) -0.009(7) -0.002(7) -0.005(6) C31 0.041(8) 0.032(7) 0.031(6) 0.004(5) -0.017(6) -0.005(6) C32 0.020(6) 0.036(7) 0.041(7) -0.006(6) -0.006(6) -0.008(5) C33 0.029(7) 0.055(9) 0.040(7) -0.023(7) 0.008(6) -0.022(6) C34 0.029(8) 0.065(10) 0.035(7) 0.003(7) 0.005(6) -0.015(7) C35 0.037(9) 0.116(15) 0.042(8) 0.027(9) -0.006(7) 0.005(9) C36 0.022(8) 0.086(12) 0.065(10) 0.020(9) -0.005(7) -0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S2 2.135(3) . ? Ni1 S2 2.135(3) 2_675 ? Ni1 S1 2.143(3) . ? Ni1 S1 2.143(3) 2_675 ? Ni2 S4 2.133(3) 2_566 ? Ni2 S4 2.133(3) . ? Ni2 S3 2.144(3) . ? Ni2 S3 2.144(3) 2_566 ? S1 C1 1.684(12) . ? S2 C2 1.723(12) . ? S3 C7 1.700(12) . ? S4 C8 1.718(12) . ? O1 C5 1.229(16) . ? O2 C5 1.315(15) . ? O2 C6 1.469(14) . ? O3 C3 1.216(14) . ? O4 C3 1.327(15) . ? O4 C4 1.455(14) . ? O5 C11 1.211(16) . ? O6 C11 1.301(16) . ? O6 C12 1.458(15) . ? O7 C9 1.227(15) . ? O8 C9 1.348(15) . ? O8 C10 1.449(15) . ? P1 C31 1.772(12) . ? P1 C13 1.781(12) . ? P1 C25 1.792(12) . ? P1 C19 1.795(12) . ? C1 C2 1.379(16) . ? C1 C3 1.484(16) . ? C2 C5 1.476(18) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.370(15) . ? C7 C11 1.498(17) . ? C8 C9 1.470(16) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.406(16) . ? C13 C14 1.411(16) . ? C14 C15 1.393(16) . ? C14 H14 0.9300 . ? C15 C16 1.357(16) . ? C15 H15 0.9300 . ? C16 C17 1.411(17) . ? C16 H16 0.9300 . ? C17 C18 1.353(16) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.358(16) . ? C19 C24 1.419(16) . ? C20 C21 1.365(17) . ? C20 H20 0.9300 . ? C21 C22 1.380(16) . ? C21 H21 0.9300 . ? C22 C23 1.365(16) . ? C22 H22 0.9300 . ? C23 C24 1.374(16) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.376(16) . ? C25 C30 1.440(18) . ? C26 C27 1.375(16) . ? C26 H26 0.9300 . ? C27 C28 1.354(17) . ? C27 H27 0.9300 . ? C28 C29 1.397(17) . ? C28 H28 0.9300 . ? C29 C30 1.396(17) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.384(16) . ? C31 C36 1.415(17) . ? C32 C33 1.410(15) . ? C32 H32 0.9300 . ? C33 C34 1.348(17) . ? C33 H33 0.9300 . ? C34 C35 1.436(19) . ? C34 H34 0.9300 . ? C35 C36 1.409(18) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? 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 S2 Ni1 S2 180.0 . 2_675 ? S2 Ni1 S1 92.08(12) . . ? S2 Ni1 S1 87.92(12) 2_675 . ? S2 Ni1 S1 87.92(12) . 2_675 ? S2 Ni1 S1 92.08(12) 2_675 2_675 ? S1 Ni1 S1 180.00(14) . 2_675 ? S4 Ni2 S4 180.000(1) 2_566 . ? S4 Ni2 S3 88.47(12) 2_566 . ? S4 Ni2 S3 91.53(12) . . ? S4 Ni2 S3 91.53(12) 2_566 2_566 ? S4 Ni2 S3 88.47(12) . 2_566 ? S3 Ni2 S3 180.000(1) . 2_566 ? C1 S1 Ni1 103.9(4) . . ? C2 S2 Ni1 104.1(4) . . ? C7 S3 Ni2 104.3(4) . . ? C8 S4 Ni2 104.6(4) . . ? C5 O2 C6 117.3(10) . . ? C3 O4 C4 117.7(11) . . ? C11 O6 C12 112.7(12) . . ? C9 O8 C10 115.0(11) . . ? C31 P1 C13 110.6(5) . . ? C31 P1 C25 110.8(6) . . ? C13 P1 C25 108.7(6) . . ? C31 P1 C19 106.9(5) . . ? C13 P1 C19 110.4(6) . . ? C25 P1 C19 109.5(6) . . ? C2 C1 C3 123.2(11) . . ? C2 C1 S1 121.4(9) . . ? C3 C1 S1 115.4(9) . . ? C1 C2 C5 124.9(11) . . ? C1 C2 S2 118.5(10) . . ? C5 C2 S2 116.6(9) . . ? O3 C3 O4 122.8(12) . . ? O3 C3 C1 124.7(12) . . ? O4 C3 C1 112.5(11) . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 O2 124.4(13) . . ? O1 C5 C2 122.9(13) . . ? O2 C5 C2 112.7(11) . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C11 122.3(11) . . ? C8 C7 S3 120.5(8) . . ? C11 C7 S3 117.0(9) . . ? C7 C8 C9 121.1(11) . . ? C7 C8 S4 119.0(8) . . ? C9 C8 S4 119.9(9) . . ? O7 C9 O8 122.7(12) . . ? O7 C9 C8 125.3(12) . . ? O8 C9 C8 112.0(11) . . ? O8 C10 H10A 109.5 . . ? O8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 124.6(14) . . ? O5 C11 C7 121.7(13) . . ? O6 C11 C7 113.4(13) . . ? O6 C12 H12A 109.5 . . ? O6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.3(11) . . ? C18 C13 P1 121.8(9) . . ? C14 C13 P1 119.8(10) . . ? C15 C14 C13 119.2(11) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 120.6(11) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 121.4(13) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 118.1(12) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C17 C18 C13 122.4(11) . . ? C17 C18 H18 118.8 . . ? C13 C18 H18 118.8 . . ? C20 C19 C24 120.1(11) . . ? C20 C19 P1 120.0(9) . . ? C24 C19 P1 119.9(9) . . ? C19 C20 C21 121.0(12) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C22 119.6(13) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.0(12) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 121.5(12) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C19 117.6(11) . . ? C23 C24 H24 121.2 . . ? C19 C24 H24 121.2 . . ? C26 C25 C30 119.7(11) . . ? C26 C25 P1 123.0(10) . . ? C30 C25 P1 117.2(9) . . ? C27 C26 C25 119.5(12) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C28 C27 C26 122.3(12) . . ? C28 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C27 C28 C29 120.1(11) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 119.6(12) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C25 118.6(12) . . ? C29 C30 H30 120.7 . . ? C25 C30 H30 120.7 . . ? C32 C31 C36 119.7(11) . . ? C32 C31 P1 123.7(9) . . ? C36 C31 P1 116.6(10) . . ? C31 C32 C33 120.3(12) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 120.7(12) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 121.2(12) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 117.9(13) . . ? C36 C35 H35 121.1 . . ? C34 C35 H35 121.1 . . ? C35 C36 C31 120.3(13) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.263 _refine_diff_density_min -1.491 _refine_diff_density_rms 0.187