Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bigoli, Francesco' 'Curreli, Simona' 'Deplano, Paola' 'Leoni, Laura' 'Mercuri, Maria Laura' 'Pellinghelli, Maria Angela' 'Serpe, Angela' 'Trogu, Emanuele F.' _publ_contact_author_name 'Prof Paola Deplano' _publ_contact_author_address ; Dipartimento di Chimica Inorganica ed Analitica Universitą di Cagliari Cittadella di Monserrato Monserrato- Cagliari I090042 ITALY ; _publ_contact_author_email 'DEPLANO@VAXCA1.UNICA.IT' _publ_section_title ; NICKEL DITHIOLENE COMPLEXES AS SOURCE OF A NEW FAMILY OF S,S-DINEGATIVE CHIRAL LIGANDS 5,5'-bis(1,3-dialkyl-4-imidazolidine-2-thione-4-thiolate (R4btimdt). ; data_[Ni(tp)(Bu4btimdt)] _database_code_CSD 102390 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H69 N4 Ni P3 S4' _chemical_formula_weight 1174.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 '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 11.057(4) _cell_length_b 12.973(6) _cell_length_c 23.023(9) _cell_angle_alpha 78.69(2) _cell_angle_beta 75.88(2) _cell_angle_gamma 69.89(2) _cell_volume 2985(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 18 _cell_measurement_theta_max 30 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 2.866 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' -diffrn_measurement_method '\q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 11289 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 70.00 _reflns_number_total 11289 _reflns_number_gt 4884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf_Nonius CAD4 local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP' _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^)+(0.1507P)^2^+2.8699P] 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 0.00005(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11289 _refine_ls_number_parameters 610 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1907 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.3316 _refine_ls_wR_factor_gt 0.2243 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 1.972 _refine_ls_shift/su_mean 0.006 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.31869(13) 0.20773(10) 0.22109(6) 0.0521(4) Uani 1 1 d . . . S11 S 0.0115(3) 0.7693(2) 0.21345(15) 0.0961(9) Uani 1 1 d . . . S21 S 0.3706(2) 0.35573(17) 0.23352(11) 0.0648(6) Uani 1 1 d . . . S12 S 0.1150(3) 0.2457(3) 0.51601(11) 0.0965(9) Uani 1 1 d . . . S22 S 0.1051(2) 0.24522(17) 0.27806(9) 0.0577(5) Uani 1 1 d . . . P1 P 0.2868(2) 0.26344(16) 0.12344(9) 0.0519(5) Uani 1 1 d . . . P2 P 0.3057(2) 0.05100(16) 0.20742(9) 0.0536(5) Uani 1 1 d . . . P3 P 0.5174(2) 0.10871(17) 0.23625(9) 0.0547(5) Uani 1 1 d . . . N11 N 0.0449(7) 0.5811(6) 0.2939(3) 0.0678(19) Uani 1 1 d . . . N21 N 0.2019(7) 0.5680(5) 0.2160(3) 0.0613(17) Uani 1 1 d . . . N12 N 0.1258(7) 0.3863(6) 0.4103(3) 0.0657(19) Uani 1 1 d . . . N22 N 0.1012(7) 0.2306(6) 0.4013(3) 0.0620(18) Uani 1 1 d . . . C11 C 0.0875(10) 0.6380(7) 0.2413(4) 0.070(2) Uani 1 1 d . . . C21 C 0.2332(8) 0.4654(6) 0.2518(4) 0.0544(19) Uani 1 1 d . . . C31 C 0.1352(8) 0.4764(6) 0.3020(4) 0.061(2) Uani 1 1 d . . . C12 C 0.1130(9) 0.2870(8) 0.4414(4) 0.068(2) Uani 1 1 d . . . C22 C 0.1079(8) 0.2907(7) 0.3441(3) 0.056(2) Uani 1 1 d . . . C32 C 0.1208(8) 0.3879(7) 0.3497(3) 0.061(2) Uani 1 1 d . . . C1A C 0.1772(8) 0.4000(6) 0.0996(4) 0.0548(19) Uani 1 1 d . . . C2A C 0.0783(9) 0.4534(7) 0.1426(4) 0.064(2) Uani 1 1 d . . . H2A H 0.0707 0.4220 0.1827 0.077 Uiso 1 1 calc R . . C3A C -0.0101(10) 0.5539(8) 0.1263(4) 0.075(3) Uani 1 1 d . . . H3A H -0.0788 0.5886 0.1555 0.091 Uiso 1 1 calc R . . C4A C 0.0022(12) 0.6031(8) 0.0680(5) 0.085(3) Uani 1 1 d . . . H4A H -0.0569 0.6713 0.0574 0.102 Uiso 1 1 calc R . . C5A C 0.1030(11) 0.5503(8) 0.0249(5) 0.081(3) Uani 1 1 d . . . H5A H 0.1119 0.5836 -0.0149 0.097 Uiso 1 1 calc R . . C6A C 0.1900(9) 0.4500(7) 0.0397(4) 0.070(2) Uani 1 1 d . . . H6A H 0.2575 0.4151 0.0102 0.084 Uiso 1 1 calc R . . C1B C 0.4342(8) 0.2481(7) 0.0651(3) 0.058(2) Uani 1 1 d . . . C2B C 0.4924(9) 0.3297(8) 0.0515(4) 0.072(3) Uani 1 1 d . . . H2B H 0.4509 0.3954 0.0685 0.087 Uiso 1 1 calc R . . C3B C 0.6147(10) 0.3149(10) 0.0119(4) 0.083(3) Uani 1 1 d . . . H3B H 0.6529 0.3713 0.0026 0.100 Uiso 1 1 calc R . . C4B C 0.6768(11) 0.2193(10) -0.0126(5) 0.091(3) Uani 1 1 d . . . H4B H 0.7578 0.2096 -0.0384 0.109 Uiso 1 1 calc R . . C5B C 0.6196(11) 0.1365(10) 0.0010(5) 0.091(3) Uani 1 1 d . . . H5B H 0.6623 0.0705 -0.0156 0.109 Uiso 1 1 calc R . . C6B C 0.4971(9) 0.1513(7) 0.0399(4) 0.070(2) Uani 1 1 d . . . H6B H 0.4583 0.0954 0.0485 0.084 Uiso 1 1 calc R . . C1C C 0.2124(8) 0.1684(7) 0.1068(3) 0.057(2) Uani 1 1 d . . . C2C C 0.1507(9) 0.1882(8) 0.0575(4) 0.071(2) Uani 1 1 d . . . H2C H 0.1512 0.2502 0.0293 0.085 Uiso 1 1 calc R . . C3C C 0.0890(10) 0.1161(8) 0.0503(4) 0.076(3) Uani 1 1 d . . . H3C H 0.0480 0.1306 0.0174 0.092 Uiso 1 1 calc R . . C4C C 0.0876(10) 0.0224(8) 0.0915(4) 0.078(3) Uani 1 1 d . . . H4C H 0.0451 -0.0254 0.0870 0.094 Uiso 1 1 calc R . . C5C C 0.1526(9) 0.0013(7) 0.1408(4) 0.068(2) Uani 1 1 d . . . H5C H 0.1554 -0.0622 0.1682 0.081 Uiso 1 1 calc R . . C6C C 0.2117(8) 0.0743(6) 0.1485(3) 0.0523(18) Uani 1 1 d . . . C1D C 0.2478(10) -0.0440(7) 0.2669(4) 0.067(2) Uani 1 1 d . . . C2D C 0.3370(12) -0.1274(9) 0.2962(5) 0.093(3) Uani 1 1 d . . . H2D H 0.4266 -0.1384 0.2837 0.112 Uiso 1 1 calc R . . C3D C 0.2891(18) -0.1954(11) 0.3457(6) 0.123(5) Uani 1 1 d . . . H3D H 0.3477 -0.2489 0.3674 0.148 Uiso 1 1 calc R . . C4D C 0.1583(16) -0.1843(11) 0.3622(6) 0.113(5) Uani 1 1 d . . . H4D H 0.1291 -0.2332 0.3931 0.136 Uiso 1 1 calc R . . C5D C 0.0718(14) -0.1022(11) 0.3336(5) 0.100(4) Uani 1 1 d . . . H5D H -0.0172 -0.0948 0.3451 0.120 Uiso 1 1 calc R . . C6D C 0.1136(11) -0.0279(8) 0.2867(4) 0.079(3) Uani 1 1 d . . . H6D H 0.0527 0.0314 0.2690 0.095 Uiso 1 1 calc R . . C1E C 0.5730(8) -0.0036(6) 0.1896(4) 0.057(2) Uani 1 1 d . . . C2E C 0.7032(8) -0.0614(7) 0.1674(4) 0.070(2) Uani 1 1 d . . . H2E H 0.7709 -0.0463 0.1778 0.084 Uiso 1 1 calc R . . C3E C 0.7319(10) -0.1421(8) 0.1294(5) 0.082(3) Uani 1 1 d . . . H3E H 0.8186 -0.1789 0.1134 0.099 Uiso 1 1 calc R . . C4E C 0.6332(11) -0.1664(8) 0.1161(5) 0.085(3) Uani 1 1 d . . . H4E H 0.6536 -0.2209 0.0912 0.101 Uiso 1 1 calc R . . C5E C 0.5021(10) -0.1127(7) 0.1382(4) 0.071(2) Uani 1 1 d . . . H5E H 0.4356 -0.1311 0.1287 0.085 Uiso 1 1 calc R . . C6E C 0.4721(9) -0.0295(7) 0.1756(4) 0.060(2) Uani 1 1 d . . . C1F C 0.5277(8) 0.0408(7) 0.3124(4) 0.059(2) Uani 1 1 d . . . C2F C 0.6338(10) -0.0511(8) 0.3258(4) 0.083(3) Uani 1 1 d . . . H2F H 0.7030 -0.0794 0.2950 0.100 Uiso 1 1 calc R . . C3F C 0.6354(13) -0.0987(9) 0.3835(5) 0.098(4) Uani 1 1 d . . . H3F H 0.7061 -0.1598 0.3921 0.117 Uiso 1 1 calc R . . C4F C 0.5366(13) -0.0593(11) 0.4289(5) 0.103(4) Uani 1 1 d . . . H4F H 0.5388 -0.0951 0.4680 0.124 Uiso 1 1 calc R . . C5F C 0.4326(11) 0.0328(11) 0.4184(4) 0.106(4) Uani 1 1 d . . . H5F H 0.3651 0.0612 0.4497 0.127 Uiso 1 1 calc R . . C6F C 0.4323(10) 0.0824(9) 0.3584(4) 0.084(3) Uani 1 1 d . . . H6F H 0.3641 0.1459 0.3502 0.100 Uiso 1 1 calc R . . C1G C 0.6499(8) 0.1686(7) 0.2162(4) 0.064(2) Uani 1 1 d . . . C2G C 0.6992(10) 0.1929(9) 0.2581(5) 0.088(3) Uani 1 1 d . . . H2G H 0.6668 0.1765 0.2989 0.105 Uiso 1 1 calc R . . C3G C 0.7989(12) 0.2425(12) 0.2407(7) 0.112(4) Uani 1 1 d . . . H3G H 0.8328 0.2587 0.2698 0.134 Uiso 1 1 calc R . . C4G C 0.8460(13) 0.2671(11) 0.1810(8) 0.116(5) Uani 1 1 d . . . H4G H 0.9132 0.2990 0.1695 0.140 Uiso 1 1 calc R . . C5G C 0.7956(11) 0.2455(10) 0.1380(6) 0.098(4) Uani 1 1 d . . . H5G H 0.8274 0.2628 0.0973 0.118 Uiso 1 1 calc R . . C6G C 0.6983(10) 0.1985(8) 0.1556(5) 0.080(3) Uani 1 1 d . . . H6G H 0.6625 0.1856 0.1262 0.096 Uiso 1 1 calc R . . C41 C -0.0782(10) 0.6217(9) 0.3362(5) 0.091(3) Uiso 1 1 d D . . H41A H -0.0861 0.6948 0.3439 0.109 Uiso 1 1 calc R . . H41B H -0.0742 0.5735 0.3741 0.109 Uiso 1 1 calc R . . C51 C -0.2009(15) 0.6282(12) 0.3147(10) 0.207(9) Uiso 1 1 d D . . H51A H -0.2781 0.6644 0.3427 0.249 Uiso 1 1 calc R . . H51B H -0.2030 0.6723 0.2755 0.249 Uiso 1 1 calc R . . C61 C -0.2039(16) 0.5149(13) 0.3100(10) 0.204(9) Uiso 1 1 d D . . H61A H -0.1769 0.4642 0.3449 0.245 Uiso 1 1 calc R . . H61B H -0.1434 0.4872 0.2741 0.245 Uiso 1 1 calc R . . C71 C -0.345(2) 0.522(2) 0.3068(17) 0.39(2) Uiso 1 1 d D . . H71A H -0.3408 0.4770 0.2773 0.582 Uiso 1 1 calc R . . H71B H -0.3937 0.5971 0.2956 0.582 Uiso 1 1 calc R . . H71C H -0.3873 0.4951 0.3456 0.582 Uiso 1 1 calc R . . C81 C 0.2808(9) 0.5984(8) 0.1585(4) 0.078(3) Uiso 1 1 d D . . H81A H 0.2237 0.6385 0.1301 0.093 Uiso 1 1 calc R . . H81B H 0.3411 0.5319 0.1421 0.093 Uiso 1 1 calc R . . C91 C 0.3580(9) 0.6701(8) 0.1666(6) 0.105(4) Uiso 1 1 d D . . H91A H 0.3846 0.7094 0.1278 0.126 Uiso 1 1 calc R . . H91B H 0.3021 0.7244 0.1932 0.126 Uiso 1 1 calc R . . C101 C 0.4784(10) 0.6020(11) 0.1926(6) 0.136(5) Uiso 1 1 d D . . H10A H 0.4562 0.5480 0.2253 0.163 Uiso 1 1 calc R . . H10B H 0.5097 0.6498 0.2086 0.163 Uiso 1 1 calc R . . C111 C 0.5874(13) 0.5421(14) 0.1429(8) 0.183(7) Uiso 1 1 d D . . H11A H 0.5767 0.4726 0.1410 0.275 Uiso 1 1 calc R . . H11B H 0.6717 0.5295 0.1522 0.275 Uiso 1 1 calc R . . H11C H 0.5814 0.5872 0.1046 0.275 Uiso 1 1 calc R . . C42 C 0.1600(10) 0.4637(9) 0.4354(5) 0.086(3) Uiso 1 1 d D . . H42A H 0.1289 0.4579 0.4787 0.104 Uiso 1 1 calc R . . H42B H 0.1186 0.5386 0.4182 0.104 Uiso 1 1 calc R . . C52 C 0.3117(12) 0.4376(15) 0.4209(8) 0.174(7) Uiso 1 1 d D . . H52A H 0.3543 0.3588 0.4293 0.209 Uiso 1 1 calc R . . H52B H 0.3410 0.4607 0.3786 0.209 Uiso 1 1 calc R . . C62 C 0.346(2) 0.502(2) 0.4610(15) 0.41(2) Uiso 1 1 d D . . H62A H 0.2879 0.5771 0.4601 0.491 Uiso 1 1 calc R . . H62B H 0.4358 0.5035 0.4464 0.491 Uiso 1 1 calc R . . C72 C 0.332(5) 0.442(4) 0.5261(12) 0.60(4) Uiso 1 1 d D . . H72A H 0.2739 0.3984 0.5312 0.900 Uiso 1 1 calc R . . H72B H 0.2961 0.4952 0.5543 0.900 Uiso 1 1 calc R . . H72C H 0.4162 0.3938 0.5335 0.900 Uiso 1 1 calc R . . C82 C 0.0836(9) 0.1216(9) 0.4152(5) 0.088(3) Uiso 1 1 d D . . H82A H 0.1423 0.0760 0.4420 0.105 Uiso 1 1 calc R . . H82B H 0.1101 0.0881 0.3781 0.105 Uiso 1 1 calc R . . C92 C -0.0532(11) 0.1191(14) 0.4438(7) 0.163(6) Uiso 1 1 d D . . H92A H -0.0515 0.0424 0.4531 0.196 Uiso 1 1 calc R . . H92B H -0.0780 0.1496 0.4818 0.196 Uiso 1 1 calc R . . C102 C -0.1561(13) 0.179(2) 0.4080(9) 0.255(12) Uiso 1 1 d D . . H10C H -0.1358 0.1475 0.3706 0.306 Uiso 1 1 calc R . . H10D H -0.1598 0.2562 0.3982 0.306 Uiso 1 1 calc R . . C112 C -0.2925(12) 0.1702(18) 0.4455(9) 0.228(10) Uiso 1 1 d D . . H11D H -0.2931 0.1644 0.4878 0.342 Uiso 1 1 calc R . . H11E H -0.3063 0.1058 0.4373 0.342 Uiso 1 1 calc R . . H11F H -0.3612 0.2350 0.4343 0.342 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 Ni 0.0553(8) 0.0426(7) 0.0516(8) -0.0036(5) -0.0056(6) -0.0113(6) S11 0.109(2) 0.0499(13) 0.120(2) 0.0050(14) -0.0441(18) -0.0060(13) S21 0.0610(13) 0.0491(11) 0.0797(15) -0.0128(10) -0.0045(11) -0.0149(10) S12 0.115(2) 0.117(2) 0.0483(13) 0.0030(14) -0.0142(14) -0.0333(18) S22 0.0550(12) 0.0610(12) 0.0516(11) -0.0048(9) -0.0038(9) -0.0167(9) P1 0.0567(12) 0.0458(10) 0.0470(11) 0.0011(8) -0.0048(9) -0.0153(9) P2 0.0627(13) 0.0440(10) 0.0487(11) 0.0002(8) -0.0070(9) -0.0156(9) P3 0.0551(12) 0.0478(11) 0.0538(12) -0.0046(9) -0.0101(9) -0.0078(9) N11 0.069(5) 0.058(4) 0.068(5) -0.020(4) -0.006(4) -0.006(4) N21 0.072(5) 0.050(4) 0.060(4) 0.001(3) -0.011(4) -0.022(3) N12 0.069(5) 0.072(5) 0.052(4) -0.014(3) -0.012(3) -0.013(4) N22 0.071(5) 0.057(4) 0.046(4) 0.008(3) -0.002(3) -0.018(3) C11 0.082(6) 0.046(5) 0.073(6) -0.004(4) -0.021(5) -0.008(4) C21 0.060(5) 0.039(4) 0.061(5) -0.006(3) -0.013(4) -0.010(3) C31 0.057(5) 0.049(4) 0.067(5) -0.008(4) -0.016(4) -0.001(4) C12 0.078(6) 0.069(6) 0.046(5) -0.007(4) -0.005(4) -0.014(5) C22 0.054(5) 0.060(5) 0.043(4) 0.000(4) -0.004(3) -0.013(4) C32 0.064(5) 0.063(5) 0.044(4) -0.001(4) -0.007(4) -0.010(4) C1A 0.055(5) 0.055(5) 0.051(4) 0.006(4) -0.014(4) -0.018(4) C2A 0.078(6) 0.063(5) 0.048(5) 0.007(4) -0.024(4) -0.019(5) C3A 0.077(6) 0.068(6) 0.070(6) -0.010(5) -0.028(5) 0.002(5) C4A 0.115(9) 0.057(6) 0.079(7) 0.000(5) -0.043(6) -0.011(6) C5A 0.111(8) 0.063(6) 0.068(6) 0.016(5) -0.026(6) -0.034(6) C6A 0.069(6) 0.063(5) 0.068(6) 0.005(4) -0.016(5) -0.014(4) C1B 0.068(5) 0.057(5) 0.046(4) 0.001(4) -0.004(4) -0.025(4) C2B 0.069(6) 0.076(6) 0.062(5) -0.004(5) -0.003(5) -0.019(5) C3B 0.080(7) 0.101(8) 0.068(6) 0.002(6) -0.004(5) -0.040(6) C4B 0.074(7) 0.110(9) 0.069(7) -0.006(6) 0.016(5) -0.029(7) C5B 0.090(8) 0.092(8) 0.067(6) -0.016(6) 0.007(6) -0.010(6) C6B 0.081(6) 0.062(5) 0.054(5) 0.003(4) -0.003(4) -0.018(5) C1C 0.067(5) 0.063(5) 0.039(4) 0.002(3) -0.007(4) -0.025(4) C2C 0.081(6) 0.071(6) 0.062(5) 0.002(4) -0.021(5) -0.026(5) C3C 0.085(7) 0.078(6) 0.064(6) -0.011(5) -0.017(5) -0.020(5) C4C 0.082(7) 0.079(7) 0.077(7) -0.021(5) -0.015(5) -0.025(5) C5C 0.075(6) 0.047(5) 0.077(6) -0.005(4) -0.004(5) -0.022(4) C6C 0.058(5) 0.042(4) 0.056(5) -0.006(3) -0.007(4) -0.017(4) C1D 0.087(7) 0.056(5) 0.055(5) -0.004(4) -0.005(5) -0.025(5) C2D 0.103(8) 0.085(7) 0.079(7) 0.027(6) -0.015(6) -0.035(6) C3D 0.183(15) 0.093(9) 0.084(8) 0.031(7) -0.022(9) -0.058(10) C4D 0.142(13) 0.102(10) 0.085(9) 0.014(7) 0.011(8) -0.061(10) C5D 0.126(10) 0.109(9) 0.076(7) -0.013(7) 0.022(7) -0.075(9) C6D 0.092(7) 0.066(6) 0.078(7) -0.010(5) -0.001(6) -0.033(5) C1E 0.055(5) 0.052(4) 0.057(5) -0.001(4) -0.009(4) -0.011(4) C2E 0.049(5) 0.059(5) 0.092(7) -0.019(5) -0.010(5) -0.002(4) C3E 0.067(6) 0.078(7) 0.091(7) -0.035(6) 0.001(5) -0.006(5) C4E 0.087(7) 0.065(6) 0.092(8) -0.031(5) -0.006(6) -0.009(5) C5E 0.079(6) 0.064(5) 0.066(6) -0.012(4) -0.006(5) -0.021(5) C6E 0.069(5) 0.050(4) 0.050(5) 0.001(4) -0.007(4) -0.012(4) C1F 0.054(5) 0.054(5) 0.059(5) -0.006(4) -0.017(4) -0.002(4) C2F 0.088(7) 0.081(7) 0.063(6) -0.009(5) -0.029(5) 0.007(5) C3F 0.120(9) 0.079(7) 0.072(7) 0.008(5) -0.046(7) 0.006(6) C4F 0.118(10) 0.106(9) 0.069(7) 0.002(6) -0.015(7) -0.023(8) C5F 0.089(8) 0.144(11) 0.051(6) -0.002(6) -0.012(5) 0.000(7) C6F 0.086(7) 0.087(7) 0.056(6) -0.008(5) -0.006(5) -0.006(6) C1G 0.053(5) 0.061(5) 0.071(6) -0.015(4) -0.017(4) -0.002(4) C2G 0.076(7) 0.093(8) 0.103(8) -0.005(6) -0.026(6) -0.035(6) C3G 0.085(9) 0.133(11) 0.139(12) -0.019(9) -0.045(8) -0.045(8) C4G 0.091(9) 0.089(9) 0.171(15) -0.009(9) -0.016(10) -0.040(7) C5G 0.079(8) 0.095(8) 0.115(10) 0.012(7) -0.009(7) -0.040(7) C6G 0.083(7) 0.072(6) 0.079(7) -0.002(5) -0.012(5) -0.024(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 Ni P2 2.174(3) . ? Ni P3 2.204(3) . ? Ni S21 2.270(3) . ? Ni P1 2.297(3) . ? Ni S22 2.341(3) . ? S11 C11 1.693(8) . ? S21 C21 1.716(8) . ? S12 C12 1.701(9) . ? S22 C22 1.746(8) . ? P1 C1B 1.820(8) . ? P1 C1A 1.837(8) . ? P1 C1C 1.838(9) . ? P2 C1D 1.805(9) . ? P2 C6C 1.823(8) . ? P2 C6E 1.825(9) . ? P3 C1G 1.810(10) . ? P3 C1F 1.813(8) . ? P3 C1E 1.825(9) . ? N11 C11 1.359(11) . ? N11 C31 1.391(10) . ? N11 C41 1.462(12) . ? N21 C11 1.350(11) . ? N21 C21 1.401(9) . ? N21 C81 1.461(11) . ? N12 C12 1.380(11) . ? N12 C32 1.407(10) . ? N12 C42 1.441(12) . ? N22 C12 1.340(11) . ? N22 C22 1.392(9) . ? N22 C82 1.456(12) . ? C21 C31 1.371(11) . ? C31 C32 1.446(11) . ? C22 C32 1.350(11) . ? C1A C2A 1.369(11) . ? C1A C6A 1.400(11) . ? C2A C3A 1.380(11) . ? C2A H2A 0.9300 . ? C3A C4A 1.366(13) . ? C3A H3A 0.9300 . ? C4A C5A 1.377(14) . ? C4A H4A 0.9300 . ? C5A C6A 1.364(12) . ? C5A H5A 0.9300 . ? C6A H6A 0.9300 . ? C1B C2B 1.368(12) . ? C1B C6B 1.374(11) . ? C2B C3B 1.408(13) . ? C2B H2B 0.9300 . ? C3B C4B 1.352(14) . ? C3B H3B 0.9300 . ? C4B C5B 1.375(15) . ? C4B H4B 0.9300 . ? C5B C6B 1.404(13) . ? C5B H5B 0.9300 . ? C6B H6B 0.9300 . ? C1C C6C 1.398(10) . ? C1C C2C 1.401(11) . ? C2C C3C 1.387(13) . ? C2C H2C 0.9300 . ? C3C C4C 1.390(13) . ? C3C H3C 0.9300 . ? C4C C5C 1.422(13) . ? C4C H4C 0.9300 . ? C5C C6C 1.379(11) . ? C5C H5C 0.9300 . ? C1D C2D 1.380(13) . ? C1D C6D 1.396(13) . ? C2D C3D 1.410(14) . ? C2D H2D 0.9300 . ? C3D C4D 1.367(18) . ? C3D H3D 0.9300 . ? C4D C5D 1.347(17) . ? C4D H4D 0.9300 . ? C5D C6D 1.401(13) . ? C5D H5D 0.9300 . ? C6D H6D 0.9300 . ? C1E C6E 1.393(12) . ? C1E C2E 1.394(11) . ? C2E C3E 1.399(12) . ? C2E H2E 0.9300 . ? C3E C4E 1.350(14) . ? C3E H3E 0.9300 . ? C4E C5E 1.390(13) . ? C4E H4E 0.9300 . ? C5E C6E 1.411(12) . ? C5E H5E 0.9300 . ? C1F C6F 1.346(12) . ? C1F C2F 1.402(11) . ? C2F C3F 1.354(13) . ? C2F H2F 0.9300 . ? C3F C4F 1.347(15) . ? C3F H3F 0.9300 . ? C4F C5F 1.373(15) . ? C4F H4F 0.9300 . ? C5F C6F 1.405(13) . ? C5F H5F 0.9300 . ? C6F H6F 0.9300 . ? C1G C2G 1.351(13) . ? C1G C6G 1.396(13) . ? C2G C3G 1.400(15) . ? C2G H2G 0.9300 . ? C3G C4G 1.361(18) . ? C3G H3G 0.9300 . ? C4G C5G 1.362(18) . ? C4G H4G 0.9300 . ? C5G C6G 1.354(14) . ? C5G H5G 0.9300 . ? C6G H6G 0.9300 . ? C41 C51 1.525(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C51 C61 1.507(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C61 C71 1.549(10) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C81 C91 1.523(8) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C91 C101 1.511(8) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C101 C111 1.548(9) . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C111 H11A 0.9600 . ? C111 H11B 0.9600 . ? C111 H11C 0.9600 . ? C42 C52 1.556(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C52 C62 1.545(10) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C62 C72 1.546(10) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C72 H72A 1.1116 . ? C72 H72B 1.1116 . ? C72 H72C 1.1117 . ? C82 C92 1.504(9) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C92 C102 1.476(9) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C102 C112 1.574(9) . ? C102 H10C 0.9700 . ? C102 H10D 0.9700 . ? C112 H11D 0.9600 . ? C112 H11E 0.9600 . ? C112 H11F 0.9600 . ? 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 P2 Ni P3 84.33(9) . . ? P2 Ni S21 169.94(10) . . ? P3 Ni S21 85.95(10) . . ? P2 Ni P1 84.74(9) . . ? P3 Ni P1 118.37(9) . . ? S21 Ni P1 97.65(9) . . ? P2 Ni S22 88.36(9) . . ? P3 Ni S22 136.46(10) . . ? S21 Ni S22 100.50(9) . . ? P1 Ni S22 103.51(9) . . ? C21 S21 Ni 111.8(3) . . ? C22 S22 Ni 106.6(3) . . ? C1B P1 C1A 103.5(4) . . ? C1B P1 C1C 103.1(4) . . ? C1A P1 C1C 102.7(4) . . ? C1B P1 Ni 116.2(3) . . ? C1A P1 Ni 122.7(3) . . ? C1C P1 Ni 106.2(2) . . ? C1D P2 C6C 106.2(4) . . ? C1D P2 C6E 104.4(4) . . ? C6C P2 C6E 104.9(4) . . ? C1D P2 Ni 124.2(3) . . ? C6C P2 Ni 109.5(2) . . ? C6E P2 Ni 106.0(3) . . ? C1G P3 C1F 103.8(4) . . ? C1G P3 C1E 103.8(4) . . ? C1F P3 C1E 105.0(4) . . ? C1G P3 Ni 120.9(3) . . ? C1F P3 Ni 115.6(3) . . ? C1E P3 Ni 106.2(3) . . ? C11 N11 C31 110.1(7) . . ? C11 N11 C41 125.8(8) . . ? C31 N11 C41 124.1(8) . . ? C11 N21 C21 111.4(7) . . ? C11 N21 C81 122.9(7) . . ? C21 N21 C81 125.7(7) . . ? C12 N12 C32 107.9(7) . . ? C12 N12 C42 123.9(8) . . ? C32 N12 C42 127.4(8) . . ? C12 N22 C22 110.5(7) . . ? C12 N22 C82 125.1(8) . . ? C22 N22 C82 124.4(8) . . ? N21 C11 N11 105.7(7) . . ? N21 C11 S11 127.6(7) . . ? N11 C11 S11 126.8(7) . . ? C31 C21 N21 105.1(7) . . ? C31 C21 S21 130.4(6) . . ? N21 C21 S21 124.4(6) . . ? C21 C31 N11 107.6(7) . . ? C21 C31 C32 124.8(7) . . ? N11 C31 C32 127.0(8) . . ? N22 C12 N12 106.9(7) . . ? N22 C12 S12 127.5(7) . . ? N12 C12 S12 125.6(7) . . ? C32 C22 N22 106.9(7) . . ? C32 C22 S22 127.4(6) . . ? N22 C22 S22 125.7(7) . . ? C22 C32 N12 107.8(7) . . ? C22 C32 C31 127.2(8) . . ? N12 C32 C31 125.0(8) . . ? C2A C1A C6A 119.4(7) . . ? C2A C1A P1 117.9(6) . . ? C6A C1A P1 122.7(7) . . ? C1A C2A C3A 120.0(8) . . ? C1A C2A H2A 120.0 . . ? C3A C2A H2A 120.0 . . ? C4A C3A C2A 120.8(9) . . ? C4A C3A H3A 119.6 . . ? C2A C3A H3A 119.6 . . ? C3A C4A C5A 119.2(9) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C6A C5A C4A 121.0(9) . . ? C6A C5A H5A 119.5 . . ? C4A C5A H5A 119.5 . . ? C5A C6A C1A 119.6(9) . . ? C5A C6A H6A 120.2 . . ? C1A C6A H6A 120.2 . . ? C2B C1B C6B 119.0(8) . . ? C2B C1B P1 119.0(7) . . ? C6B C1B P1 121.5(7) . . ? C1B C2B C3B 120.5(9) . . ? C1B C2B H2B 119.7 . . ? C3B C2B H2B 119.7 . . ? C4B C3B C2B 120.3(10) . . ? C4B C3B H3B 119.8 . . ? C2B C3B H3B 119.8 . . ? C3B C4B C5B 119.7(10) . . ? C3B C4B H4B 120.2 . . ? C5B C4B H4B 120.2 . . ? C4B C5B C6B 120.2(10) . . ? C4B C5B H5B 119.9 . . ? C6B C5B H5B 119.9 . . ? C1B C6B C5B 120.2(9) . . ? C1B C6B H6B 119.9 . . ? C5B C6B H6B 119.9 . . ? C6C C1C C2C 119.0(8) . . ? C6C C1C P1 116.9(6) . . ? C2C C1C P1 124.1(6) . . ? C3C C2C C1C 120.6(9) . . ? C3C C2C H2C 119.7 . . ? C1C C2C H2C 119.7 . . ? C2C C3C C4C 120.8(9) . . ? C2C C3C H3C 119.6 . . ? C4C C3C H3C 119.6 . . ? C3C C4C C5C 118.4(9) . . ? C3C C4C H4C 120.8 . . ? C5C C4C H4C 120.8 . . ? C6C C5C C4C 120.6(8) . . ? C6C C5C H5C 119.7 . . ? C4C C5C H5C 119.7 . . ? C5C C6C C1C 120.6(8) . . ? C5C C6C P2 124.0(6) . . ? C1C C6C P2 115.2(6) . . ? C2D C1D C6D 120.0(9) . . ? C2D C1D P2 119.2(8) . . ? C6D C1D P2 120.5(7) . . ? C1D C2D C3D 118.5(12) . . ? C1D C2D H2D 120.8 . . ? C3D C2D H2D 120.8 . . ? C4D C3D C2D 121.2(13) . . ? C4D C3D H3D 119.4 . . ? C2D C3D H3D 119.4 . . ? C5D C4D C3D 119.8(12) . . ? C5D C4D H4D 120.1 . . ? C3D C4D H4D 120.1 . . ? C4D C5D C6D 121.1(12) . . ? C4D C5D H5D 119.4 . . ? C6D C5D H5D 119.4 . . ? C1D C6D C5D 119.1(11) . . ? C1D C6D H6D 120.5 . . ? C5D C6D H6D 120.5 . . ? C6E C1E C2E 119.6(8) . . ? C6E C1E P3 114.3(6) . . ? C2E C1E P3 126.1(7) . . ? C1E C2E C3E 120.1(9) . . ? C1E C2E H2E 119.9 . . ? C3E C2E H2E 120.0 . . ? C4E C3E C2E 119.7(9) . . ? C4E C3E H3E 120.2 . . ? C2E C3E H3E 120.2 . . ? C3E C4E C5E 122.2(9) . . ? C3E C4E H4E 118.9 . . ? C5E C4E H4E 118.9 . . ? C4E C5E C6E 118.5(10) . . ? C4E C5E H5E 120.8 . . ? C6E C5E H5E 120.8 . . ? C1E C6E C5E 119.9(8) . . ? C1E C6E P2 115.8(6) . . ? C5E C6E P2 124.3(8) . . ? C6F C1F C2F 118.4(8) . . ? C6F C1F P3 119.0(7) . . ? C2F C1F P3 122.6(7) . . ? C3F C2F C1F 119.8(10) . . ? C3F C2F H2F 120.1 . . ? C1F C2F H2F 120.1 . . ? C4F C3F C2F 121.3(10) . . ? C4F C3F H3F 119.4 . . ? C2F C3F H3F 119.4 . . ? C3F C4F C5F 121.1(11) . . ? C3F C4F H4F 119.4 . . ? C5F C4F H4F 119.4 . . ? C4F C5F C6F 117.3(10) . . ? C4F C5F H5F 121.4 . . ? C6F C5F H5F 121.4 . . ? C1F C6F C5F 122.1(10) . . ? C1F C6F H6F 119.0 . . ? C5F C6F H6F 119.0 . . ? C2G C1G C6G 117.7(10) . . ? C2G C1G P3 122.2(8) . . ? C6G C1G P3 120.0(8) . . ? C1G C2G C3G 120.5(12) . . ? C1G C2G H2G 119.8 . . ? C3G C2G H2G 119.8 . . ? C4G C3G C2G 119.8(13) . . ? C4G C3G H3G 120.1 . . ? C2G C3G H3G 120.1 . . ? C3G C4G C5G 120.6(13) . . ? C3G C4G H4G 119.7 . . ? C5G C4G H4G 119.7 . . ? C6G C5G C4G 118.9(13) . . ? C6G C5G H5G 120.5 . . ? C4G C5G H5G 120.5 . . ? C5G C6G C1G 122.4(11) . . ? C5G C6G H6G 118.8 . . ? C1G C6G H6G 118.8 . . ? N11 C41 C51 114.7(11) . . ? N11 C41 H41A 108.6 . . ? C51 C41 H41A 108.6 . . ? N11 C41 H41B 108.6 . . ? C51 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C61 C51 C41 111.4(9) . . ? C61 C51 H51A 109.3 . . ? C41 C51 H51A 109.3 . . ? C61 C51 H51B 109.3 . . ? C41 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? C51 C61 C71 109.5(9) . . ? C51 C61 H61A 109.8 . . ? C71 C61 H61A 109.8 . . ? C51 C61 H61B 109.8 . . ? C71 C61 H61B 109.8 . . ? H61A C61 H61B 108.2 . . ? C61 C71 H71A 109.5 . . ? C61 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C61 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N21 C81 C91 111.1(8) . . ? N21 C81 H81A 109.4 . . ? C91 C81 H81A 109.4 . . ? N21 C81 H81B 109.4 . . ? C91 C81 H81B 109.4 . . ? H81A C81 H81B 108.0 . . ? C101 C91 C81 111.8(7) . . ? C101 C91 H91A 109.3 . . ? C81 C91 H91A 109.3 . . ? C101 C91 H91B 109.3 . . ? C81 C91 H91B 109.3 . . ? H91A C91 H91B 107.9 . . ? C91 C101 C111 109.9(8) . . ? C91 C101 H10A 109.7 . . ? C111 C101 H10A 109.7 . . ? C91 C101 H10B 109.7 . . ? C111 C101 H10B 109.7 . . ? H10A C101 H10B 108.2 . . ? C101 C111 H11A 109.5 . . ? C101 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C101 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? N12 C42 C52 109.2(10) . . ? N12 C42 H42A 109.8 . . ? C52 C42 H42A 109.8 . . ? N12 C42 H42B 109.8 . . ? C52 C42 H42B 109.8 . . ? H42A C42 H42B 108.3 . . ? C62 C52 C42 107.4(9) . . ? C62 C52 H52A 110.2 . . ? C42 C52 H52A 110.2 . . ? C62 C52 H52B 110.2 . . ? C42 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? C52 C62 C72 107.9(9) . . ? C52 C62 H62A 110.1 . . ? C72 C62 H62A 110.1 . . ? C52 C62 H62B 110.1 . . ? C72 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? C62 C72 H72A 124.2 . . ? C62 C72 H72B 124.2 . . ? H72A C72 H72B 91.5 . . ? C62 C72 H72C 124.2 . . ? H72A C72 H72C 91.5 . . ? H72B C72 H72C 91.5 . . ? N22 C82 C92 115.8(10) . . ? N22 C82 H82A 108.3 . . ? C92 C82 H82A 108.3 . . ? N22 C82 H82B 108.3 . . ? C92 C82 H82B 108.3 . . ? H82A C82 H82B 107.4 . . ? C102 C92 C82 116.4(9) . . ? C102 C92 H92A 108.2 . . ? C82 C92 H92A 108.2 . . ? C102 C92 H92B 108.2 . . ? C82 C92 H92B 108.2 . . ? H92A C92 H92B 107.3 . . ? C92 C102 C112 109.4(9) . . ? C92 C102 H10C 109.8 . . ? C112 C102 H10C 109.8 . . ? C92 C102 H10D 109.8 . . ? C112 C102 H10D 109.8 . . ? H10C C102 H10D 108.3 . . ? C102 C112 H11D 109.5 . . ? C102 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C102 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.990 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.105 #=END data_Compound2 #[Ni(QP)(Bu4btimdt)] (2) _database_code_CSD 171252 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ni(QP)(Bu4btimdt)]' _chemical_formula_sum 'C76 H78 N4 Ni P4 S4' _chemical_formula_weight 1358.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pca21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 16.689(5) _cell_length_b 23.461(5) _cell_length_c 18.253(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7147(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 19 _cell_measurement_theta_max 38 _exptl_crystal_description 'truncated pyramid' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 _exptl_absorpt_coefficient_mu 2.672 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED diffractometer' _diffrn_measurement_method '\q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none' _diffrn_reflns_number 7015 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 70.02 _reflns_number_total 7015 _reflns_number_gt 3513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens AED local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP' _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^)+(0.1457P)^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 SHELXL _refine_ls_extinction_coef 0.00033(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_number_reflns 7015 _refine_ls_number_parameters 622 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1925 _refine_ls_wR_factor_gt 0.1712 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 1.549 _refine_ls_shift/su_mean 0.051 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.54487(7) 0.22878(5) 0.30468(8) 0.0590(3) Uani 1 1 d . . . P1 P 0.48004(12) 0.22571(9) 0.19691(13) 0.0679(5) Uani 1 1 d . . . P2 P 0.63964(11) 0.27314(8) 0.24464(11) 0.0572(4) Uani 1 1 d . . . P3 P 0.63869(13) 0.16758(8) 0.33571(13) 0.0645(5) Uani 1 1 d . . . P4 P 0.73296(13) 0.34685(9) 0.38037(13) 0.0680(5) Uani 1 1 d . . . S11 S 0.4228(3) 0.13997(16) 0.64759(19) 0.1245(12) Uani 1 1 d . . . S21 S 0.44857(15) 0.16824(10) 0.34882(15) 0.0801(6) Uani 1 1 d . . . S12 S 0.22645(16) 0.40579(13) 0.3862(2) 0.1111(10) Uani 1 1 d . . . S22 S 0.52560(12) 0.30749(8) 0.38174(14) 0.0692(5) Uani 1 1 d . . . N11 N 0.3864(4) 0.2202(3) 0.5465(5) 0.076(2) Uani 1 1 d . . . N21 N 0.4390(5) 0.1435(3) 0.4980(5) 0.086(2) Uani 1 1 d . . . N12 N 0.2964(4) 0.3069(3) 0.4320(5) 0.083(2) Uani 1 1 d . . . N22 N 0.3802(4) 0.3649(3) 0.3791(4) 0.0718(18) Uani 1 1 d . . . C11 C 0.4142(6) 0.1681(4) 0.5629(6) 0.086(3) Uani 1 1 d . . . C21 C 0.4230(6) 0.1830(4) 0.4402(5) 0.077(2) Uani 1 1 d . . . C31 C 0.3905(5) 0.2287(4) 0.4692(5) 0.069(2) Uani 1 1 d . . . C12 C 0.3024(6) 0.3592(4) 0.3997(6) 0.083(3) Uani 1 1 d . . . C22 C 0.4241(5) 0.3161(4) 0.3988(5) 0.071(2) Uani 1 1 d . . . C32 C 0.3716(5) 0.2813(4) 0.4348(5) 0.068(2) Uani 1 1 d . . . C1A C 0.4159(4) 0.2857(3) 0.1731(4) 0.076(2) Uani 1 1 d G . . C2A C 0.3554(4) 0.2997(3) 0.2223(3) 0.098(3) Uani 1 1 d G . . H2A H 0.3486 0.2783 0.2648 0.117 Uiso 1 1 calc R . . C3A C 0.3051(4) 0.3456(4) 0.2081(5) 0.120(4) Uani 1 1 d G . . H3A H 0.2646 0.3549 0.2410 0.144 Uiso 1 1 calc R . . C4A C 0.3152(5) 0.3775(3) 0.1446(6) 0.126(5) Uani 1 1 d G . . H4A H 0.2815 0.4082 0.1351 0.151 Uiso 1 1 calc R . . C5A C 0.3757(6) 0.3636(3) 0.0954(4) 0.118(4) Uani 1 1 d G . . H5A H 0.3824 0.3850 0.0529 0.142 Uiso 1 1 calc R . . C6A C 0.4260(4) 0.3177(3) 0.1096(4) 0.096(3) Uani 1 1 d G . . H6A H 0.4664 0.3084 0.0767 0.116 Uiso 1 1 calc R . . C1B C 0.4211(4) 0.1636(3) 0.1725(5) 0.088(3) Uani 1 1 d G . . C2B C 0.4576(4) 0.1104(4) 0.1766(5) 0.116(4) Uani 1 1 d G . . H2B H 0.5106 0.1074 0.1919 0.139 Uiso 1 1 calc R . . C3B C 0.4149(7) 0.0617(3) 0.1578(7) 0.162(7) Uani 1 1 d G . . H3B H 0.4393 0.0261 0.1606 0.194 Uiso 1 1 calc R . . C4B C 0.3357(7) 0.0662(4) 0.1349(8) 0.205(11) Uani 1 1 d G . . H4B H 0.3071 0.0336 0.1224 0.246 Uiso 1 1 calc R . . C5B C 0.2992(4) 0.1193(5) 0.1309(9) 0.29(2) Uani 1 1 d G . . H5B H 0.2462 0.1223 0.1155 0.353 Uiso 1 1 calc R . . C6B C 0.3419(5) 0.1681(4) 0.1496(7) 0.169(8) Uani 1 1 d G . . H6B H 0.3175 0.2036 0.1469 0.203 Uiso 1 1 calc R . . C1C C 0.5576(3) 0.2275(3) 0.1280(3) 0.071(2) Uani 1 1 d G . . C2C C 0.6285(3) 0.2549(2) 0.1471(2) 0.066(2) Uani 1 1 d G . . C3C C 0.6899(3) 0.2602(3) 0.0961(3) 0.080(2) Uani 1 1 d G . . H3C H 0.7373 0.2785 0.1089 0.096 Uiso 1 1 calc R . . C4C C 0.6804(4) 0.2382(3) 0.0259(3) 0.088(3) Uani 1 1 d G . . H4C H 0.7215 0.2417 -0.0082 0.105 Uiso 1 1 calc R . . C5C C 0.6096(4) 0.2108(3) 0.0068(2) 0.093(3) Uani 1 1 d G . . H5C H 0.6032 0.1961 -0.0402 0.111 Uiso 1 1 calc R . . C6C C 0.5482(3) 0.2055(3) 0.0578(3) 0.090(3) Uani 1 1 d G . . H6C H 0.5008 0.1872 0.0450 0.107 Uiso 1 1 calc R . . C1D C 0.7378(2) 0.2441(2) 0.2664(3) 0.0638(19) Uani 1 1 d G . . C2D C 0.7383(3) 0.1939(2) 0.3069(3) 0.0615(17) Uani 1 1 d G . . C3D C 0.8104(3) 0.1663(2) 0.3212(3) 0.084(3) Uani 1 1 d G . . H3D H 0.8107 0.1327 0.3482 0.101 Uiso 1 1 calc R . . C4D C 0.8818(3) 0.1889(3) 0.2950(4) 0.090(3) Uani 1 1 d G . . H4D H 0.9300 0.1704 0.3045 0.108 Uiso 1 1 calc R . . C5D C 0.8813(2) 0.2390(3) 0.2545(3) 0.085(3) Uani 1 1 d G . . H5D H 0.9291 0.2541 0.2370 0.103 Uiso 1 1 calc R . . C6D C 0.8093(3) 0.2667(2) 0.2402(3) 0.071(2) Uani 1 1 d G . . H6D H 0.8089 0.3002 0.2132 0.085 Uiso 1 1 calc R . . C1E C 0.6361(5) 0.1001(2) 0.2867(4) 0.088(3) Uani 1 1 d G . . C2E C 0.6687(5) 0.0968(3) 0.2167(5) 0.124(5) Uani 1 1 d G . . H2E H 0.6951 0.1281 0.1969 0.149 Uiso 1 1 calc R . . C3E C 0.6619(6) 0.0468(4) 0.1765(5) 0.177(8) Uani 1 1 d G . . H3E H 0.6837 0.0446 0.1297 0.213 Uiso 1 1 calc R . . C4E C 0.6224(7) 0.0000(3) 0.2061(7) 0.189(9) Uani 1 1 d G . . H4E H 0.6178 -0.0335 0.1792 0.227 Uiso 1 1 calc R . . C5E C 0.5898(6) 0.0033(3) 0.2761(7) 0.178(8) Uani 1 1 d G . . H5E H 0.5634 -0.0280 0.2959 0.214 Uiso 1 1 calc R . . C6E C 0.5966(5) 0.0533(3) 0.3163(5) 0.123(5) Uani 1 1 d G . . H6E H 0.5748 0.0555 0.3631 0.148 Uiso 1 1 calc R . . C1F C 0.6510(4) 0.1513(3) 0.4321(3) 0.078(2) Uani 1 1 d G . . C2F C 0.6196(4) 0.1890(3) 0.4834(4) 0.081(3) Uani 1 1 d G . . H2F H 0.5947 0.2224 0.4679 0.097 Uiso 1 1 calc R . . C3F C 0.6253(5) 0.1769(4) 0.5577(3) 0.112(4) Uani 1 1 d G . . H3F H 0.6043 0.2021 0.5920 0.134 Uiso 1 1 calc R . . C4F C 0.6625(6) 0.1270(5) 0.5808(3) 0.147(6) Uani 1 1 d G . . H4F H 0.6663 0.1188 0.6306 0.176 Uiso 1 1 calc R . . C5F C 0.6939(6) 0.0893(4) 0.5296(5) 0.176(8) Uani 1 1 d G . . H5F H 0.7188 0.0559 0.5451 0.211 Uiso 1 1 calc R . . C6F C 0.6882(5) 0.1014(3) 0.4553(4) 0.133(5) Uani 1 1 d G . . H6F H 0.7092 0.0762 0.4210 0.160 Uiso 1 1 calc R . . C1G C 0.6453(3) 0.35153(15) 0.2473(3) 0.0597(17) Uani 1 1 d G . . C2G C 0.6784(3) 0.3830(2) 0.3043(3) 0.0628(18) Uani 1 1 d G . . C3G C 0.6720(4) 0.44209(19) 0.3044(3) 0.078(2) Uani 1 1 d G . . H3G H 0.6941 0.4632 0.3425 0.094 Uiso 1 1 calc R . . C4G C 0.6327(4) 0.46968(15) 0.2474(4) 0.096(3) Uani 1 1 d G . . H4G H 0.6284 0.5092 0.2474 0.115 Uiso 1 1 calc R . . C5G C 0.5996(4) 0.4382(2) 0.1904(3) 0.094(3) Uani 1 1 d G . . H5G H 0.5733 0.4567 0.1523 0.112 Uiso 1 1 calc R . . C6G C 0.6060(4) 0.3791(2) 0.1904(3) 0.080(2) Uani 1 1 d G . . H6G H 0.5839 0.3581 0.1522 0.095 Uiso 1 1 calc R . . C1H C 0.7165(4) 0.3910(2) 0.4625(3) 0.072(2) Uani 1 1 d G . . C2H C 0.6671(4) 0.3683(2) 0.5164(4) 0.081(2) Uani 1 1 d G . . H2H H 0.6407 0.3340 0.5082 0.097 Uiso 1 1 calc R . . C3H C 0.6572(4) 0.3969(3) 0.5824(3) 0.095(3) Uani 1 1 d G . . H3H H 0.6241 0.3817 0.6185 0.114 Uiso 1 1 calc R . . C4H C 0.6966(5) 0.4482(3) 0.5946(3) 0.106(4) Uani 1 1 d G . . H4H H 0.6900 0.4674 0.6388 0.128 Uiso 1 1 calc R . . C5H C 0.7460(5) 0.4709(3) 0.5407(4) 0.113(4) Uani 1 1 d G . . H5H H 0.7724 0.5053 0.5488 0.135 Uiso 1 1 calc R . . C6H C 0.7560(4) 0.4423(3) 0.4746(3) 0.100(3) Uani 1 1 d G . . H6H H 0.7891 0.4575 0.4386 0.120 Uiso 1 1 calc R . . C1I C 0.8371(3) 0.3669(3) 0.3574(3) 0.069(2) Uani 1 1 d G . . C2I C 0.8952(4) 0.3450(3) 0.4041(3) 0.094(3) Uani 1 1 d G . . H2I H 0.8801 0.3242 0.4452 0.113 Uiso 1 1 calc R . . C3I C 0.9759(3) 0.3540(4) 0.3893(5) 0.116(4) Uani 1 1 d G . . H3I H 1.0148 0.3393 0.4205 0.139 Uiso 1 1 calc R . . C4I C 0.9985(3) 0.3850(4) 0.3277(5) 0.118(4) Uani 1 1 d G . . H4I H 1.0525 0.3911 0.3178 0.142 Uiso 1 1 calc R . . C5I C 0.9404(4) 0.4070(3) 0.2810(4) 0.102(3) Uani 1 1 d G . . H5I H 0.9555 0.4277 0.2399 0.123 Uiso 1 1 calc R . . C6I C 0.8597(4) 0.3979(3) 0.2958(3) 0.084(3) Uani 1 1 d G . . H6I H 0.8208 0.4126 0.2646 0.100 Uiso 1 1 calc R . . C41 C 0.3563(6) 0.2597(4) 0.5995(7) 0.095(3) Uiso 1 1 d D . . H41A H 0.3176 0.2401 0.6302 0.114 Uiso 1 1 calc R . . H41B H 0.3280 0.2898 0.5739 0.114 Uiso 1 1 calc R . . C51 C 0.4191(10) 0.2867(6) 0.6488(9) 0.159(6) Uiso 1 1 d D . . H51A H 0.3930 0.3040 0.6908 0.191 Uiso 1 1 calc R . . H51B H 0.4552 0.2575 0.6666 0.191 Uiso 1 1 calc R . . C61 C 0.4642(9) 0.3295(6) 0.6099(12) 0.168(7) Uiso 1 1 d D . . H61A H 0.4722 0.3175 0.5596 0.201 Uiso 1 1 calc R . . H61B H 0.5163 0.3341 0.6326 0.201 Uiso 1 1 calc R . . C71 C 0.4181(13) 0.3879(7) 0.6113(14) 0.200(8) Uiso 1 1 d D . . H71A H 0.3819 0.3896 0.5705 0.299 Uiso 1 1 calc R . . H71B H 0.4559 0.4186 0.6081 0.299 Uiso 1 1 calc R . . H71C H 0.3884 0.3910 0.6562 0.299 Uiso 1 1 calc R . . C81 C 0.4651(7) 0.0855(5) 0.4915(7) 0.102(3) Uiso 1 1 d D . . H81A H 0.4960 0.0751 0.5345 0.123 Uiso 1 1 calc R . . H81B H 0.4996 0.0817 0.4490 0.123 Uiso 1 1 calc R . . C91 C 0.3947(10) 0.0457(7) 0.4839(11) 0.162(6) Uiso 1 1 d D . . H91A H 0.3491 0.0665 0.4647 0.195 Uiso 1 1 calc R . . H91B H 0.3801 0.0310 0.5318 0.195 Uiso 1 1 calc R . . C101 C 0.415(3) -0.0050(14) 0.432(3) 0.66(6) Uiso 1 1 d D . . H10A H 0.3993 -0.0410 0.4541 0.790 Uiso 1 1 calc R . . H10B H 0.4712 -0.0060 0.4206 0.790 Uiso 1 1 calc R . . C111 C 0.363(5) 0.007(3) 0.361(2) 0.74(7) Uiso 1 1 d D . . H11A H 0.3099 0.0176 0.3753 1.103 Uiso 1 1 calc R . . H11B H 0.3618 -0.0264 0.3314 1.103 Uiso 1 1 calc R . . H11C H 0.3874 0.0379 0.3343 1.103 Uiso 1 1 calc R . . C42 C 0.2229(6) 0.2800(4) 0.4493(7) 0.098(3) Uiso 1 1 d D . . H42A H 0.1816 0.3084 0.4576 0.118 Uiso 1 1 calc R . . H42B H 0.2287 0.2573 0.4934 0.118 Uiso 1 1 calc R . . C52 C 0.1996(10) 0.2412(7) 0.3835(10) 0.163(6) Uiso 1 1 d D . . H52A H 0.1850 0.2644 0.3416 0.196 Uiso 1 1 calc R . . H52B H 0.2445 0.2173 0.3699 0.196 Uiso 1 1 calc R . . C62 C 0.1279(14) 0.2040(10) 0.4071(15) 0.251(13) Uiso 1 1 d D . . H62A H 0.0796 0.2267 0.4108 0.301 Uiso 1 1 calc R . . H62B H 0.1383 0.1862 0.4541 0.301 Uiso 1 1 calc R . . C72 C 0.1191(18) 0.1580(11) 0.3460(18) 0.322(18) Uiso 1 1 d D . . H72A H 0.0686 0.1628 0.3216 0.482 Uiso 1 1 calc R . . H72B H 0.1216 0.1207 0.3675 0.482 Uiso 1 1 calc R . . H72C H 0.1618 0.1623 0.3111 0.482 Uiso 1 1 calc R . . C82 C 0.4115(7) 0.4143(4) 0.3418(6) 0.091(3) Uiso 1 1 d D . . H82A H 0.3733 0.4271 0.3054 0.109 Uiso 1 1 calc R . . H82B H 0.4608 0.4043 0.3168 0.109 Uiso 1 1 calc R . . C92 C 0.4280(11) 0.4627(7) 0.3965(10) 0.184(7) Uiso 1 1 d D . . H92A H 0.4324 0.4982 0.3697 0.220 Uiso 1 1 calc R . . H92B H 0.3827 0.4659 0.4295 0.220 Uiso 1 1 calc R . . C102 C 0.4990(11) 0.4546(7) 0.4386(10) 0.180(7) Uiso 1 1 d D . . H10C H 0.5447 0.4499 0.4063 0.216 Uiso 1 1 calc R . . H10D H 0.4941 0.4206 0.4685 0.216 Uiso 1 1 calc R . . C112 C 0.5120(9) 0.5109(6) 0.4912(8) 0.146(5) Uiso 1 1 d D . . H11D H 0.5433 0.5388 0.4655 0.219 Uiso 1 1 calc R . . H11E H 0.5394 0.4998 0.5352 0.219 Uiso 1 1 calc R . . H11F H 0.4608 0.5268 0.5035 0.219 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 Ni 0.0593(7) 0.0547(6) 0.0630(7) 0.0034(6) 0.0019(6) -0.0036(5) P1 0.0636(11) 0.0733(13) 0.0668(13) -0.0036(11) -0.0051(10) -0.0099(10) P2 0.0576(10) 0.0559(9) 0.0579(10) 0.0035(9) 0.0000(9) -0.0028(9) P3 0.0684(12) 0.0540(10) 0.0711(12) 0.0049(10) 0.0051(10) 0.0020(9) P4 0.0794(13) 0.0650(11) 0.0597(11) 0.0005(10) 0.0007(11) -0.0072(10) S11 0.154(3) 0.120(2) 0.100(2) 0.0430(19) 0.015(2) -0.001(2) S21 0.0814(14) 0.0663(12) 0.0926(16) 0.0005(12) 0.0178(12) -0.0167(11) S12 0.0937(18) 0.1050(18) 0.135(2) -0.003(2) -0.0074(19) 0.0372(15) S22 0.0660(11) 0.0622(11) 0.0793(13) -0.0068(11) 0.0100(11) -0.0053(9) N11 0.070(4) 0.073(4) 0.086(5) 0.011(4) 0.015(4) 0.000(4) N21 0.096(6) 0.061(4) 0.101(6) 0.028(4) 0.020(5) 0.003(4) N12 0.066(4) 0.088(5) 0.095(6) 0.011(5) 0.014(4) 0.006(4) N22 0.076(4) 0.060(4) 0.080(5) 0.012(4) -0.002(4) 0.007(3) C11 0.087(7) 0.085(6) 0.085(7) 0.025(6) 0.004(5) 0.002(5) C21 0.081(6) 0.077(6) 0.072(6) 0.010(5) 0.012(5) 0.000(5) C31 0.058(4) 0.065(5) 0.086(6) 0.002(5) 0.009(4) -0.005(4) C12 0.079(6) 0.083(6) 0.089(7) -0.007(5) -0.013(5) 0.009(5) C22 0.066(5) 0.070(5) 0.076(6) -0.001(4) 0.014(4) 0.011(4) C32 0.057(5) 0.072(5) 0.074(5) 0.012(4) 0.012(4) 0.010(4) C1A 0.075(5) 0.083(6) 0.070(5) -0.014(5) -0.018(5) 0.007(5) C2A 0.105(8) 0.100(7) 0.088(7) -0.006(6) -0.014(6) 0.033(6) C3A 0.094(8) 0.150(12) 0.116(10) -0.023(9) -0.022(7) 0.030(8) C4A 0.127(11) 0.122(10) 0.130(12) 0.004(9) -0.027(10) 0.036(9) C5A 0.124(10) 0.118(9) 0.113(10) 0.037(8) -0.034(9) 0.001(8) C6A 0.108(8) 0.085(7) 0.097(8) 0.012(6) -0.002(7) -0.008(6) C1B 0.074(6) 0.102(8) 0.088(7) -0.018(6) 0.004(5) -0.027(5) C2B 0.125(10) 0.086(7) 0.135(11) -0.029(7) -0.007(8) -0.020(7) C3B 0.181(16) 0.113(11) 0.191(18) -0.038(12) 0.020(14) -0.026(11) C4B 0.107(11) 0.150(14) 0.36(3) -0.090(19) -0.004(15) -0.060(11) C5B 0.090(10) 0.203(19) 0.59(6) -0.17(3) -0.064(19) -0.038(12) C6B 0.070(7) 0.147(12) 0.29(2) -0.095(14) -0.036(11) -0.006(7) C1C 0.084(6) 0.068(5) 0.063(5) -0.004(4) -0.007(4) -0.014(4) C2C 0.074(5) 0.064(4) 0.059(5) -0.009(4) 0.008(4) -0.007(4) C3C 0.066(5) 0.096(6) 0.078(6) 0.007(5) -0.003(5) 0.002(5) C4C 0.082(6) 0.116(8) 0.065(5) 0.006(5) 0.005(5) 0.013(6) C5C 0.116(9) 0.102(7) 0.061(5) -0.004(5) 0.003(6) 0.001(6) C6C 0.089(7) 0.098(7) 0.081(6) -0.016(6) -0.002(6) -0.023(6) C1D 0.058(4) 0.067(4) 0.066(5) -0.010(4) -0.005(4) -0.003(4) C2D 0.065(4) 0.061(4) 0.058(4) -0.009(4) 0.010(4) 0.003(3) C3D 0.070(5) 0.090(6) 0.092(7) 0.016(5) -0.008(5) 0.009(5) C4D 0.059(5) 0.124(8) 0.087(7) 0.004(6) 0.004(5) 0.019(5) C5D 0.068(5) 0.116(8) 0.073(6) -0.011(6) -0.002(4) 0.002(5) C6D 0.060(4) 0.088(6) 0.066(5) -0.008(5) -0.001(4) -0.011(4) C1E 0.093(6) 0.054(4) 0.118(9) -0.010(5) 0.022(6) 0.005(4) C2E 0.124(9) 0.084(7) 0.164(13) -0.046(8) 0.044(9) -0.026(7) C3E 0.174(14) 0.118(10) 0.24(2) -0.113(13) 0.064(15) -0.035(10) C4E 0.188(15) 0.095(9) 0.28(3) -0.078(13) 0.074(17) -0.054(10) C5E 0.187(15) 0.092(9) 0.26(2) -0.041(12) 0.079(16) -0.053(10) C6E 0.130(9) 0.048(4) 0.191(14) -0.003(7) 0.034(10) -0.010(5) C1F 0.077(6) 0.088(6) 0.070(5) 0.020(5) 0.002(5) 0.011(5) C2F 0.075(6) 0.088(6) 0.079(6) 0.012(5) -0.005(5) 0.000(5) C3F 0.114(9) 0.154(11) 0.068(6) 0.006(7) -0.001(6) -0.010(8) C4F 0.121(11) 0.217(17) 0.102(10) 0.079(11) -0.002(8) 0.003(11) C5F 0.164(14) 0.24(2) 0.128(13) 0.104(14) 0.013(11) 0.074(14) C6F 0.176(13) 0.124(10) 0.101(9) 0.052(8) 0.029(9) 0.068(9) C1G 0.057(4) 0.058(4) 0.064(4) 0.011(4) 0.004(4) -0.004(3) C2G 0.070(5) 0.055(4) 0.064(4) 0.004(4) 0.004(4) -0.010(3) C3G 0.102(6) 0.063(5) 0.070(5) -0.002(5) 0.005(5) -0.007(4) C4G 0.129(9) 0.056(5) 0.103(8) 0.020(6) 0.016(7) 0.001(5) C5G 0.115(8) 0.073(6) 0.094(7) 0.019(6) -0.016(6) 0.005(6) C6G 0.090(6) 0.070(5) 0.078(6) 0.014(5) -0.011(5) 0.000(5) C1H 0.080(6) 0.074(5) 0.062(5) 0.000(4) -0.001(4) -0.003(4) C2H 0.086(6) 0.076(5) 0.080(6) 0.012(5) -0.002(5) -0.001(5) C3H 0.111(8) 0.116(8) 0.058(5) 0.012(6) 0.011(5) 0.010(7) C4H 0.131(9) 0.123(9) 0.065(6) -0.008(6) -0.012(7) 0.015(8) C5H 0.161(10) 0.094(7) 0.083(7) -0.015(6) 0.012(8) -0.031(8) C6H 0.140(9) 0.088(6) 0.071(6) -0.006(5) 0.013(6) -0.022(7) C1I 0.066(5) 0.069(5) 0.072(5) -0.004(4) -0.001(4) -0.009(4) C2I 0.082(6) 0.092(7) 0.109(8) 0.006(6) -0.020(6) -0.007(5) C3I 0.088(7) 0.128(9) 0.131(11) 0.000(10) -0.018(7) 0.003(7) C4I 0.104(9) 0.128(10) 0.123(11) -0.012(8) 0.006(8) -0.024(8) C5I 0.081(7) 0.124(9) 0.101(8) 0.003(7) 0.012(6) -0.020(6) C6I 0.090(6) 0.084(6) 0.077(6) -0.005(5) 0.003(5) -0.026(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 Ni P2 2.188(2) . ? Ni P3 2.199(3) . ? Ni P1 2.246(3) . ? Ni S21 2.291(2) . ? Ni S22 2.344(3) . ? P1 C1C 1.806(5) . ? P1 C1B 1.813(6) . ? P1 C1A 1.822(6) . ? P2 C1D 1.819(4) . ? P2 C2C 1.840(5) . ? P2 C1G 1.842(4) . ? P3 C1F 1.813(6) . ? P3 C1E 1.819(5) . ? P3 C2D 1.850(5) . ? P4 C1H 1.842(5) . ? P4 C1I 1.849(5) . ? P4 C2G 1.864(5) . ? S11 C11 1.686(11) . ? S21 C21 1.757(10) . ? S12 C12 1.693(10) . ? S22 C22 1.734(9) . ? N11 C11 1.343(12) . ? N11 C31 1.425(12) . ? N11 C41 1.431(13) . ? N21 C11 1.381(14) . ? N21 C21 1.431(12) . ? N21 C81 1.434(13) . ? N12 C12 1.365(12) . ? N12 C32 1.392(10) . ? N12 C42 1.414(12) . ? N22 C12 1.358(12) . ? N22 C22 1.407(10) . ? N22 C82 1.442(12) . ? C21 C31 1.312(12) . ? C31 C32 1.421(12) . ? C22 C32 1.365(12) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A H2A 0.9300 . ? C3A C4A 1.3900 . ? C3A H3A 0.9300 . ? C4A C5A 1.3900 . ? C4A H4A 0.9300 . ? C5A C6A 1.3900 . ? C5A H5A 0.9300 . ? C6A H6A 0.9300 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C2B H2B 0.9300 . ? C3B C4B 1.3900 . ? C3B H3B 0.9300 . ? C4B C5B 1.3900 . ? C4B H4B 0.9300 . ? C5B C6B 1.3900 . ? C5B H5B 0.9300 . ? C6B H6B 0.9300 . ? C1C C2C 1.3900 . ? C1C C6C 1.3900 . ? C2C C3C 1.3900 . ? C3C C4C 1.3900 . ? C3C H3C 0.9300 . ? C4C C5C 1.3900 . ? C4C H4C 0.9300 . ? C5C C6C 1.3900 . ? C5C H5C 0.9300 . ? C6C H6C 0.9300 . ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C2D C3D 1.3900 . ? C3D C4D 1.3900 . ? C3D H3D 0.9300 . ? C4D C5D 1.3900 . ? C4D H4D 0.9300 . ? C5D C6D 1.3900 . ? C5D H5D 0.9300 . ? C6D H6D 0.9300 . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C2E C3E 1.3900 . ? C2E H2E 0.9300 . ? C3E C4E 1.3900 . ? C3E H3E 0.9300 . ? C4E C5E 1.3900 . ? C4E H4E 0.9300 . ? C5E C6E 1.3900 . ? C5E H5E 0.9300 . ? C6E H6E 0.9300 . ? C1F C2F 1.3900 . ? C1F C6F 1.3900 . ? C2F C3F 1.3900 . ? C2F H2F 0.9300 . ? C3F C4F 1.3900 . ? C3F H3F 0.9300 . ? C4F C5F 1.3900 . ? C4F H4F 0.9300 . ? C5F C6F 1.3900 . ? C5F H5F 0.9300 . ? C6F H6F 0.9300 . ? C1G C2G 1.3900 . ? C1G C6G 1.3900 . ? C2G C3G 1.3900 . ? C3G C4G 1.3900 . ? C3G H3G 0.9300 . ? C4G C5G 1.3900 . ? C4G H4G 0.9300 . ? C5G C6G 1.3900 . ? C5G H5G 0.9300 . ? C6G H6G 0.9300 . ? C1H C2H 1.3900 . ? C1H C6H 1.3900 . ? C2H C3H 1.3900 . ? C2H H2H 0.9300 . ? C3H C4H 1.3900 . ? C3H H3H 0.9300 . ? C4H C5H 1.3900 . ? C4H H4H 0.9300 . ? C5H C6H 1.3900 . ? C5H H5H 0.9300 . ? C6H H6H 0.9300 . ? C1I C2I 1.3900 . ? C1I C6I 1.3900 . ? C2I C3I 1.3900 . ? C2I H2I 0.9300 . ? C3I C4I 1.3900 . ? C3I H3I 0.9300 . ? C4I C5I 1.3900 . ? C4I H4I 0.9300 . ? C5I C6I 1.3900 . ? C5I H5I 0.9300 . ? C6I H6I 0.9300 . ? C41 C51 1.519(14) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C51 C61 1.441(15) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C61 C71 1.570(15) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C71 H71A 0.9663 . ? C71 H71B 0.9664 . ? C71 H71C 0.9664 . ? C81 C91 1.507(14) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C91 C101 1.56(2) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C101 C111 1.57(2) . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C111 H11A 1.1293 . ? C111 H11B 1.1527 . ? C111 H11C 1.1520 . ? C42 C52 1.556(14) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C52 C62 1.542(16) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C62 C72 1.558(18) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C72 H72A 0.9608 . ? C72 H72B 0.9608 . ? C72 H72C 0.9608 . ? C82 C92 1.534(14) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C92 C102 1.426(15) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C102 C112 1.646(15) . ? C102 H10C 0.9700 . ? C102 H10D 0.9700 . ? C112 H11D 0.9600 . ? C112 H11E 0.9600 . ? C112 H11F 0.9600 . ? 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 P2 Ni P3 85.70(9) . . ? P2 Ni P1 85.68(9) . . ? P3 Ni P1 123.21(10) . . ? P2 Ni S21 168.03(10) . . ? P3 Ni S21 90.24(10) . . ? P1 Ni S21 87.15(10) . . ? P2 Ni S22 91.43(8) . . ? P3 Ni S22 117.24(10) . . ? P1 Ni S22 119.00(10) . . ? S21 Ni S22 100.43(9) . . ? C1C P1 C1B 103.7(3) . . ? C1C P1 C1A 103.7(3) . . ? C1B P1 C1A 104.1(4) . . ? C1C P1 Ni 105.3(2) . . ? C1B P1 Ni 120.1(3) . . ? C1A P1 Ni 117.9(2) . . ? C1D P2 C2C 102.4(3) . . ? C1D P2 C1G 108.8(3) . . ? C2C P2 C1G 105.3(3) . . ? C1D P2 Ni 111.31(19) . . ? C2C P2 Ni 107.49(19) . . ? C1G P2 Ni 119.9(2) . . ? C1F P3 C1E 107.3(3) . . ? C1F P3 C2D 104.1(3) . . ? C1E P3 C2D 99.9(3) . . ? C1F P3 Ni 117.9(2) . . ? C1E P3 Ni 115.1(3) . . ? C2D P3 Ni 110.43(19) . . ? C1H P4 C1I 100.4(3) . . ? C1H P4 C2G 106.1(3) . . ? C1I P4 C2G 100.0(3) . . ? C21 S21 Ni 112.4(3) . . ? C22 S22 Ni 109.5(3) . . ? C11 N11 C31 109.4(8) . . ? C11 N11 C41 124.0(9) . . ? C31 N11 C41 126.6(8) . . ? C11 N21 C21 107.8(7) . . ? C11 N21 C81 124.0(9) . . ? C21 N21 C81 127.7(10) . . ? C12 N12 C32 109.6(7) . . ? C12 N12 C42 124.2(8) . . ? C32 N12 C42 125.5(8) . . ? C12 N22 C22 110.3(7) . . ? C12 N22 C82 123.8(8) . . ? C22 N22 C82 125.9(8) . . ? N11 C11 N21 107.0(8) . . ? N11 C11 S11 126.2(9) . . ? N21 C11 S11 126.7(8) . . ? C31 C21 N21 108.0(9) . . ? C31 C21 S21 130.2(8) . . ? N21 C21 S21 121.8(7) . . ? C21 C31 C32 128.5(9) . . ? C21 C31 N11 107.8(8) . . ? C32 C31 N11 123.2(8) . . ? N22 C12 N12 106.2(8) . . ? N22 C12 S12 127.7(8) . . ? N12 C12 S12 126.0(8) . . ? C32 C22 N22 105.9(7) . . ? C32 C22 S22 130.1(7) . . ? N22 C22 S22 123.9(6) . . ? C22 C32 N12 107.7(7) . . ? C22 C32 C31 126.1(7) . . ? N12 C32 C31 126.2(7) . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 117.0(4) . . ? C6A C1A P1 123.0(4) . . ? C3A C2A C1A 120.0 . . ? C3A C2A H2A 120.0 . . ? C1A C2A H2A 120.0 . . ? C2A C3A C4A 120.0 . . ? C2A C3A H3A 120.0 . . ? C4A C3A H3A 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6A 120.0 . . ? C1A C6A H6A 120.0 . . ? C2B C1B C6B 120.0 . . ? C2B C1B P1 118.1(5) . . ? C6B C1B P1 121.9(5) . . ? C1B C2B C3B 120.0 . . ? C1B C2B H2B 120.0 . . ? C3B C2B H2B 120.0 . . ? C4B C3B C2B 120.0 . . ? C4B C3B H3B 120.0 . . ? C2B C3B H3B 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C4B C5B C6B 120.0 . . ? C4B C5B H5B 120.0 . . ? C6B C5B H5B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B H6B 120.0 . . ? C1B C6B H6B 120.0 . . ? C2C C1C C6C 120.0 . . ? C2C C1C P1 116.5(3) . . ? C6C C1C P1 123.5(3) . . ? C1C C2C C3C 120.0 . . ? C1C C2C P2 115.9(3) . . ? C3C C2C P2 123.5(3) . . ? C2C C3C C4C 120.0 . . ? C2C C3C H3C 120.0 . . ? C4C C3C H3C 120.0 . . ? C5C C4C C3C 120.0 . . ? C5C C4C H4C 120.0 . . ? C3C C4C H4C 120.0 . . ? C6C C5C C4C 120.0 . . ? C6C C5C H5C 120.0 . . ? C4C C5C H5C 120.0 . . ? C5C C6C C1C 120.0 . . ? C5C C6C H6C 120.0 . . ? C1C C6C H6C 120.0 . . ? C2D C1D C6D 120.0 . . ? C2D C1D P2 116.1(3) . . ? C6D C1D P2 123.7(3) . . ? C3D C2D C1D 120.0 . . ? C3D C2D P3 124.6(3) . . ? C1D C2D P3 115.3(3) . . ? C2D C3D C4D 120.0 . . ? C2D C3D H3D 120.0 . . ? C4D C3D H3D 120.0 . . ? C3D C4D C5D 120.0 . . ? C3D C4D H4D 120.0 . . ? C5D C4D H4D 120.0 . . ? C6D C5D C4D 120.0 . . ? C6D C5D H5D 120.0 . . ? C4D C5D H5D 120.0 . . ? C5D C6D C1D 120.0 . . ? C5D C6D H6D 120.0 . . ? C1D C6D H6D 120.0 . . ? C2E C1E C6E 120.0 . . ? C2E C1E P3 119.4(4) . . ? C6E C1E P3 120.5(4) . . ? C1E C2E C3E 120.0 . . ? C1E C2E H2E 120.0 . . ? C3E C2E H2E 120.0 . . ? C4E C3E C2E 120.0 . . ? C4E C3E H3E 120.0 . . ? C2E C3E H3E 120.0 . . ? C5E C4E C3E 120.0 . . ? C5E C4E H4E 120.0 . . ? C3E C4E H4E 120.0 . . ? C4E C5E C6E 120.0 . . ? C4E C5E H5E 120.0 . . ? C6E C5E H5E 120.0 . . ? C5E C6E C1E 120.0 . . ? C5E C6E H6E 120.0 . . ? C1E C6E H6E 120.0 . . ? C2F C1F C6F 120.0 . . ? C2F C1F P3 118.4(4) . . ? C6F C1F P3 121.5(4) . . ? C3F C2F C1F 120.0 . . ? C3F C2F H2F 120.0 . . ? C1F C2F H2F 120.0 . . ? C2F C3F C4F 120.0 . . ? C2F C3F H3F 120.0 . . ? C4F C3F H3F 120.0 . . ? C5F C4F C3F 120.0 . . ? C5F C4F H4F 120.0 . . ? C3F C4F H4F 120.0 . . ? C4F C5F C6F 120.0 . . ? C4F C5F H5F 120.0 . . ? C6F C5F H5F 120.0 . . ? C5F C6F C1F 120.0 . . ? C5F C6F H6F 120.0 . . ? C1F C6F H6F 120.0 . . ? C2G C1G C6G 120.0 . . ? C2G C1G P2 124.8(3) . . ? C6G C1G P2 114.9(3) . . ? C3G C2G C1G 120.0 . . ? C3G C2G P4 119.4(3) . . ? C1G C2G P4 120.6(3) . . ? C4G C3G C2G 120.0 . . ? C4G C3G H3G 120.0 . . ? C2G C3G H3G 120.0 . . ? C3G C4G C5G 120.0 . . ? C3G C4G H4G 120.0 . . ? C5G C4G H4G 120.0 . . ? C6G C5G C4G 120.0 . . ? C6G C5G H5G 120.0 . . ? C4G C5G H5G 120.0 . . ? C5G C6G C1G 120.0 . . ? C5G C6G H6G 120.0 . . ? C1G C6G H6G 120.0 . . ? C2H C1H C6H 120.0 . . ? C2H C1H P4 116.6(4) . . ? C6H C1H P4 123.1(4) . . ? C3H C2H C1H 120.0 . . ? C3H C2H H2H 120.0 . . ? C1H C2H H2H 120.0 . . ? C2H C3H C4H 120.0 . . ? C2H C3H H3H 120.0 . . ? C4H C3H H3H 120.0 . . ? C3H C4H C5H 120.0 . . ? C3H C4H H4H 120.0 . . ? C5H C4H H4H 120.0 . . ? C6H C5H C4H 120.0 . . ? C6H C5H H5H 120.0 . . ? C4H C5H H5H 120.0 . . ? C5H C6H C1H 120.0 . . ? C5H C6H H6H 120.0 . . ? C1H C6H H6H 120.0 . . ? C2I C1I C6I 120.0 . . ? C2I C1I P4 115.0(4) . . ? C6I C1I P4 124.9(4) . . ? C3I C2I C1I 120.0 . . ? C3I C2I H2I 120.0 . . ? C1I C2I H2I 120.0 . . ? C2I C3I C4I 120.0 . . ? C2I C3I H3I 120.0 . . ? C4I C3I H3I 120.0 . . ? C5I C4I C3I 120.0 . . ? C5I C4I H4I 120.0 . . ? C3I C4I H4I 120.0 . . ? C4I C5I C6I 120.0 . . ? C4I C5I H5I 120.0 . . ? C6I C5I H5I 120.0 . . ? C5I C6I C1I 120.0 . . ? C5I C6I H6I 120.0 . . ? C1I C6I H6I 120.0 . . ? N11 C41 C51 115.4(11) . . ? N11 C41 H41A 108.4 . . ? C51 C41 H41A 108.5 . . ? N11 C41 H41B 108.5 . . ? C51 C41 H41B 108.3 . . ? H41A C41 H41B 107.5 . . ? C61 C51 C41 111.1(13) . . ? C61 C51 H51A 109.3 . . ? C41 C51 H51A 109.5 . . ? C61 C51 H51B 109.5 . . ? C41 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? C51 C61 C71 110.1(13) . . ? C51 C61 H61A 109.6 . . ? C71 C61 H61A 109.7 . . ? C51 C61 H61B 109.7 . . ? C71 C61 H61B 109.5 . . ? H61A C61 H61B 108.2 . . ? C61 C71 H71A 109.9 . . ? C61 C71 H71B 110.2 . . ? H71A C71 H71B 108.9 . . ? C61 C71 H71C 110.1 . . ? H71A C71 H71C 108.9 . . ? H71B C71 H71C 108.8 . . ? N21 C81 C91 111.0(11) . . ? N21 C81 H81A 109.5 . . ? C91 C81 H81A 109.6 . . ? N21 C81 H81B 109.3 . . ? C91 C81 H81B 109.3 . . ? H81A C81 H81B 108.0 . . ? C81 C91 C101 111.3(18) . . ? C81 C91 H91A 109.3 . . ? C101 C91 H91A 109.1 . . ? C81 C91 H91B 109.1 . . ? C101 C91 H91B 110.1 . . ? H91A C91 H91B 107.9 . . ? C91 C101 C111 104.2(18) . . ? C91 C101 H10A 110.1 . . ? C111 C101 H10A 110.2 . . ? C91 C101 H10B 111.5 . . ? C111 C101 H10B 111.8 . . ? H10A C101 H10B 109.0 . . ? C101 C111 H11A 125.7 . . ? C101 C111 H11B 127.8 . . ? H11A C111 H11B 88.0 . . ? C101 C111 H11C 127.8 . . ? H11A C111 H11C 87.4 . . ? H11B C111 H11C 86.6 . . ? N12 C42 C52 107.8(10) . . ? N12 C42 H42A 110.1 . . ? C52 C42 H42A 110.2 . . ? N12 C42 H42B 110.2 . . ? C52 C42 H42B 110.1 . . ? H42A C42 H42B 108.5 . . ? C62 C52 C42 108.1(13) . . ? C62 C52 H52A 110.1 . . ? C42 C52 H52A 110.0 . . ? C62 C52 H52B 110.1 . . ? C42 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C52 C62 C72 105.4(15) . . ? C52 C62 H62A 110.7 . . ? C72 C62 H62A 110.4 . . ? C52 C62 H62B 110.7 . . ? C72 C62 H62B 110.8 . . ? H62A C62 H62B 108.8 . . ? C62 C72 H72A 109.8 . . ? C62 C72 H72B 109.4 . . ? H72A C72 H72B 109.4 . . ? C62 C72 H72C 109.5 . . ? H72A C72 H72C 109.4 . . ? H72B C72 H72C 109.4 . . ? N22 C82 C92 110.7(11) . . ? N22 C82 H82A 109.4 . . ? C92 C82 H82A 109.6 . . ? N22 C82 H82B 109.5 . . ? C92 C82 H82B 109.6 . . ? H82A C82 H82B 108.0 . . ? C102 C92 C82 113.6(12) . . ? C102 C92 H92A 108.9 . . ? C82 C92 H92A 108.6 . . ? C102 C92 H92B 108.8 . . ? C82 C92 H92B 109.0 . . ? H92A C92 H92B 107.7 . . ? C92 C102 C112 108.5(12) . . ? C92 C102 H10C 110.0 . . ? C112 C102 H10C 109.9 . . ? C92 C102 H10D 110.0 . . ? C112 C102 H10D 110.2 . . ? H10C C102 H10D 108.3 . . ? C102 C112 H11D 109.7 . . ? C102 C112 H11E 109.3 . . ? H11D C112 H11E 109.5 . . ? C102 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 70.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.654 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.074 #=END #=BEGIN data_Compound3 #[Ni(TP)(dmit)] (3) _database_code_CSD 171253 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ni(TP)(dmit)]' _chemical_formula_sum 'C45 H33 Ni P3 S5' _chemical_formula_weight 885.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/n' 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 9.541(6) _cell_length_b 21.873(5) _cell_length_c 19.730(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.97(2) _cell_angle_gamma 90.00 _cell_volume 4055(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 18 _cell_measurement_theta_max 40 _exptl_crystal_description 'prism' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 4.470 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6968 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED diffractometer' _diffrn_measurement_method '\q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 7886 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 70.00 _reflns_number_total 7665 _reflns_number_gt 5770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens AED local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP' _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^)+(0.1118P)^2^+1.7368P] 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 7665 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1715 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.38473(6) 0.18296(2) 0.31283(3) 0.04862(18) Uani 1 1 d . A . S1 S 0.45369(14) 0.08516(5) 0.32617(6) 0.0777(3) Uani 1 1 d . . . S2 S 0.51015(11) 0.19623(4) 0.22153(5) 0.0618(2) Uani 1 1 d . . . S3 S 0.58809(13) 0.09624(6) 0.12929(6) 0.0781(3) Uani 1 1 d . . . S4 S 0.53172(16) -0.00068(5) 0.21802(7) 0.0873(4) Uani 1 1 d . . . S5 S 0.62785(18) -0.03290(8) 0.08678(8) 0.1065(5) Uani 1 1 d . . . P1 P 0.16351(9) 0.15291(4) 0.26810(5) 0.0488(2) Uani 1 1 d . . . P2 P 0.30372(9) 0.27470(4) 0.30491(5) 0.0483(2) Uani 1 1 d . . . P3 P 0.47713(9) 0.20587(4) 0.42074(4) 0.0498(2) Uani 1 1 d . . . C1 C 0.5323(4) 0.11906(19) 0.2052(2) 0.0609(9) Uani 1 1 d . . . C2 C 0.5062(5) 0.07346(19) 0.2466(2) 0.0671(10) Uani 1 1 d . . . C3 C 0.5857(5) 0.0180(2) 0.1418(2) 0.0759(11) Uani 1 1 d . . . C1A C 0.0670(7) 0.1113(2) 0.3261(3) 0.053(3) Uiso 0.604(8) 1 d PG A 1 C2A C 0.1303(5) 0.0601(3) 0.3603(3) 0.078(2) Uiso 0.604(8) 1 d PG A 1 H2A H 0.2171 0.0460 0.3512 0.093 Uiso 0.604(8) 1 calc PR A 1 C3A C 0.0639(6) 0.0301(2) 0.4082(3) 0.075(2) Uiso 0.604(8) 1 d PG A 1 H3A H 0.1062 -0.0042 0.4310 0.091 Uiso 0.604(8) 1 calc PR A 1 C4A C -0.0659(7) 0.0512(3) 0.4218(3) 0.101(3) Uiso 0.604(8) 1 d PG A 1 H4A H -0.1103 0.0311 0.4538 0.122 Uiso 0.604(8) 1 calc PR A 1 C5A C -0.1291(7) 0.1024(3) 0.3876(4) 0.132(4) Uiso 0.604(8) 1 d PG A 1 H5A H -0.2159 0.1165 0.3967 0.158 Uiso 0.604(8) 1 calc PR A 1 C6A C -0.0627(8) 0.1324(3) 0.3397(4) 0.109(3) Uiso 0.604(8) 1 d PG A 1 H6A H -0.1050 0.1667 0.3169 0.131 Uiso 0.604(8) 1 calc PR A 1 C1A1 C 0.0514(9) 0.1146(4) 0.3242(4) 0.065(6) Uiso 0.396(8) 1 d PG A 2 C2A1 C 0.1169(7) 0.0962(5) 0.3895(4) 0.085(4) Uiso 0.396(8) 1 d PG A 2 H2A1 H 0.2139 0.1027 0.4037 0.102 Uiso 0.396(8) 1 calc PR A 2 C3A1 C 0.0375(9) 0.0682(5) 0.4335(3) 0.103(5) Uiso 0.396(8) 1 d PG A 2 H3A1 H 0.0813 0.0559 0.4772 0.123 Uiso 0.396(8) 1 calc PR A 2 C4A1 C -0.1074(9) 0.0586(4) 0.4122(4) 0.065(3) Uiso 0.396(8) 1 d PG A 2 H4A1 H -0.1606 0.0398 0.4417 0.079 Uiso 0.396(8) 1 calc PR A 2 C5A1 C -0.1730(7) 0.0769(4) 0.3470(4) 0.087(4) Uiso 0.396(8) 1 d PG A 2 H5A1 H -0.2699 0.0705 0.3328 0.104 Uiso 0.396(8) 1 calc PR A 2 C6A1 C -0.0935(9) 0.1050(4) 0.3030(3) 0.086(4) Uiso 0.396(8) 1 d PG A 2 H6A1 H -0.1374 0.1173 0.2593 0.103 Uiso 0.396(8) 1 calc PR A 2 C1B C 0.1439(4) 0.10753(17) 0.18979(19) 0.0569(8) Uani 1 1 d . A . C2B C 0.0918(7) 0.0488(2) 0.1849(3) 0.0972(18) Uani 1 1 d . . . H2B H 0.0597 0.0309 0.2221 0.117 Uiso 1 1 calc R A . C3B C 0.0872(10) 0.0165(3) 0.1238(3) 0.126(3) Uani 1 1 d . A . H3B H 0.0492 -0.0228 0.1203 0.152 Uiso 1 1 calc R . . C4B C 0.1366(7) 0.0406(3) 0.0695(3) 0.0948(16) Uani 1 1 d . . . H4B H 0.1351 0.0179 0.0296 0.114 Uiso 1 1 calc R A . C5B C 0.1888(5) 0.0987(2) 0.0739(3) 0.0808(12) Uani 1 1 d . A . H5B H 0.2227 0.1159 0.0368 0.097 Uiso 1 1 calc R . . C6B C 0.1912(5) 0.1320(2) 0.1333(2) 0.0731(11) Uani 1 1 d . . . H6B H 0.2256 0.1719 0.1355 0.088 Uiso 1 1 calc R A . C1C C 0.0566(3) 0.22084(16) 0.24130(18) 0.0515(7) Uani 1 1 d . A . C2C C -0.0834(4) 0.2200(2) 0.2055(2) 0.0684(10) Uani 1 1 d . . . H2C H -0.1268 0.1830 0.1916 0.082 Uiso 1 1 calc R A . C3C C -0.1575(4) 0.2740(2) 0.1908(3) 0.0806(13) Uani 1 1 d . A . H3C H -0.2520 0.2729 0.1689 0.097 Uiso 1 1 calc R . . C4C C -0.0935(5) 0.3290(2) 0.2080(3) 0.0803(13) Uani 1 1 d . . . H4C H -0.1444 0.3650 0.1974 0.096 Uiso 1 1 calc R A . C5C C 0.0474(4) 0.33163(19) 0.2414(2) 0.0675(10) Uani 1 1 d . A . H5C H 0.0919 0.3691 0.2522 0.081 Uiso 1 1 calc R . . C6C C 0.1208(4) 0.27680(16) 0.25851(19) 0.0531(8) Uani 1 1 d . A . C1D C 0.3985(4) 0.33151(15) 0.26257(19) 0.0529(8) Uani 1 1 d . A . C2D C 0.3668(5) 0.3390(2) 0.1920(2) 0.0751(11) Uani 1 1 d . . . H2D H 0.2926 0.3169 0.1664 0.090 Uiso 1 1 calc R A . C3D C 0.4458(6) 0.3793(3) 0.1592(3) 0.0939(16) Uani 1 1 d . A . H3D H 0.4252 0.3840 0.1116 0.113 Uiso 1 1 calc R . . C4D C 0.5551(6) 0.4123(2) 0.1976(3) 0.0854(14) Uani 1 1 d . . . H4D H 0.6065 0.4402 0.1760 0.103 Uiso 1 1 calc R A . C5D C 0.5873(5) 0.4043(2) 0.2665(3) 0.0800(13) Uani 1 1 d . A . H5D H 0.6627 0.4259 0.2917 0.096 Uiso 1 1 calc R . . C6D C 0.5103(4) 0.36428(18) 0.3004(2) 0.0657(9) Uani 1 1 d . . . H6D H 0.5331 0.3595 0.3479 0.079 Uiso 1 1 calc R A . C1E C 0.3052(4) 0.30615(16) 0.39087(19) 0.0525(7) Uani 1 1 d . A . C2E C 0.2362(4) 0.36096(18) 0.4041(2) 0.0653(9) Uani 1 1 d . . . H2E H 0.1807 0.3823 0.3684 0.078 Uiso 1 1 calc R A . C3E C 0.2524(5) 0.3821(2) 0.4705(2) 0.0721(11) Uani 1 1 d . A . H3E H 0.2079 0.4183 0.4796 0.087 Uiso 1 1 calc R . . C4E C 0.3334(5) 0.3507(2) 0.5239(2) 0.0742(11) Uani 1 1 d . . . H4E H 0.3435 0.3657 0.5685 0.089 Uiso 1 1 calc R A . C5E C 0.3991(4) 0.2973(2) 0.5113(2) 0.0680(10) Uani 1 1 d . A . H5E H 0.4530 0.2761 0.5476 0.082 Uiso 1 1 calc R . . C6E C 0.3858(3) 0.27420(16) 0.44428(18) 0.0522(7) Uani 1 1 d . A . C1F C 0.6648(4) 0.22840(17) 0.4425(2) 0.0559(8) Uani 1 1 d . A . C2F C 0.7345(4) 0.2329(2) 0.5104(2) 0.0689(10) Uani 1 1 d . . . H2F H 0.6886 0.2207 0.5460 0.083 Uiso 1 1 calc R A . C3F C 0.8717(5) 0.2554(3) 0.5248(3) 0.0837(13) Uani 1 1 d . A . H3F H 0.9178 0.2583 0.5702 0.100 Uiso 1 1 calc R . . C4F C 0.9403(5) 0.2736(3) 0.4727(3) 0.1026(19) Uani 1 1 d . . . H4F H 1.0332 0.2881 0.4826 0.123 Uiso 1 1 calc R A . C5F C 0.8707(6) 0.2705(3) 0.4055(3) 0.1036(19) Uani 1 1 d . A . H5F H 0.9158 0.2839 0.3701 0.124 Uiso 1 1 calc R . . C6F C 0.7334(4) 0.2474(3) 0.3906(2) 0.0773(12) Uani 1 1 d . . . H6F H 0.6876 0.2448 0.3451 0.093 Uiso 1 1 calc R A . C1G C 0.4514(4) 0.14925(18) 0.48533(19) 0.0593(8) Uani 1 1 d . A . C2G C 0.3223(6) 0.1465(2) 0.5077(3) 0.0861(14) Uani 1 1 d . . . H2G H 0.2522 0.1754 0.4928 0.103 Uiso 1 1 calc R A . C3G C 0.2975(8) 0.1003(3) 0.5528(4) 0.111(2) Uani 1 1 d . A . H3G H 0.2095 0.0979 0.5668 0.133 Uiso 1 1 calc R . . C4G C 0.4002(8) 0.0583(3) 0.5766(3) 0.0968(17) Uani 1 1 d . . . H4G H 0.3831 0.0282 0.6075 0.116 Uiso 1 1 calc R A . C5G C 0.5277(7) 0.0609(2) 0.5548(3) 0.0956(16) Uani 1 1 d . A . H5G H 0.5980 0.0323 0.5706 0.115 Uiso 1 1 calc R . . C6G C 0.5538(5) 0.1063(2) 0.5086(2) 0.0758(11) Uani 1 1 d . . . H6G H 0.6409 0.1075 0.4935 0.091 Uiso 1 1 calc R A . 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 0.0473(3) 0.0427(3) 0.0561(3) 0.0037(2) 0.0094(2) 0.0027(2) S1 0.1098(9) 0.0583(6) 0.0718(6) 0.0174(5) 0.0345(6) 0.0328(6) S2 0.0694(6) 0.0541(5) 0.0661(5) 0.0020(4) 0.0239(4) -0.0056(4) S3 0.0844(7) 0.0823(7) 0.0745(7) -0.0049(5) 0.0331(6) 0.0049(6) S4 0.1149(10) 0.0580(6) 0.0956(8) 0.0025(5) 0.0364(7) 0.0251(6) S5 0.1152(11) 0.1058(11) 0.0992(10) -0.0330(8) 0.0203(8) 0.0307(9) P1 0.0483(4) 0.0421(4) 0.0563(5) 0.0004(3) 0.0100(4) -0.0050(3) P2 0.0459(4) 0.0406(4) 0.0578(5) 0.0025(3) 0.0075(3) -0.0012(3) P3 0.0463(4) 0.0506(5) 0.0525(5) 0.0025(4) 0.0089(3) 0.0007(3) C1 0.059(2) 0.062(2) 0.065(2) -0.0014(17) 0.0214(17) 0.0046(16) C2 0.075(2) 0.055(2) 0.075(3) 0.0039(18) 0.023(2) 0.0153(18) C3 0.072(3) 0.076(3) 0.080(3) -0.011(2) 0.015(2) 0.016(2) C1B 0.0563(19) 0.0508(18) 0.063(2) -0.0046(16) 0.0076(16) -0.0029(15) C2B 0.161(6) 0.057(2) 0.081(3) -0.007(2) 0.039(3) -0.029(3) C3B 0.220(8) 0.064(3) 0.099(4) -0.023(3) 0.038(5) -0.029(4) C4B 0.134(5) 0.079(3) 0.071(3) -0.020(3) 0.018(3) 0.009(3) C5B 0.083(3) 0.092(3) 0.068(3) -0.006(2) 0.017(2) -0.004(3) C6B 0.079(3) 0.076(3) 0.064(2) -0.010(2) 0.013(2) -0.023(2) C1C 0.0445(16) 0.0526(18) 0.0571(19) 0.0017(14) 0.0076(14) 0.0004(14) C2C 0.051(2) 0.068(2) 0.082(3) 0.003(2) 0.0005(18) -0.0078(17) C3C 0.0449(19) 0.092(3) 0.099(3) 0.013(3) -0.004(2) 0.005(2) C4C 0.059(2) 0.080(3) 0.099(3) 0.017(3) 0.005(2) 0.019(2) C5C 0.058(2) 0.055(2) 0.085(3) 0.0091(19) 0.0018(19) 0.0071(17) C6C 0.0460(16) 0.0485(18) 0.064(2) 0.0048(15) 0.0081(14) 0.0003(14) C1D 0.0511(18) 0.0448(16) 0.064(2) 0.0019(15) 0.0129(15) -0.0039(14) C2D 0.084(3) 0.077(3) 0.064(2) 0.005(2) 0.011(2) -0.018(2) C3D 0.112(4) 0.096(4) 0.077(3) 0.021(3) 0.026(3) -0.018(3) C4D 0.096(3) 0.066(3) 0.103(4) 0.011(2) 0.042(3) -0.015(2) C5D 0.069(3) 0.072(3) 0.103(4) -0.004(2) 0.025(2) -0.022(2) C6D 0.063(2) 0.058(2) 0.077(2) 0.0002(18) 0.0124(18) -0.0115(17) C1E 0.0489(17) 0.0481(17) 0.061(2) 0.0000(15) 0.0109(14) -0.0018(14) C2E 0.070(2) 0.053(2) 0.073(2) -0.0028(18) 0.0133(19) 0.0090(17) C3E 0.074(3) 0.058(2) 0.089(3) -0.011(2) 0.027(2) 0.0042(19) C4E 0.070(3) 0.079(3) 0.075(3) -0.020(2) 0.017(2) 0.002(2) C5E 0.064(2) 0.079(3) 0.062(2) -0.0071(19) 0.0125(18) 0.0067(19) C6E 0.0456(16) 0.0529(18) 0.0597(19) -0.0044(15) 0.0135(14) -0.0026(14) C1F 0.0468(17) 0.057(2) 0.064(2) 0.0045(16) 0.0098(15) -0.0001(15) C2F 0.059(2) 0.085(3) 0.061(2) -0.002(2) 0.0046(17) -0.007(2) C3F 0.065(2) 0.105(4) 0.077(3) -0.008(3) -0.002(2) -0.014(2) C4F 0.058(3) 0.142(5) 0.103(4) 0.004(4) 0.003(3) -0.034(3) C5F 0.074(3) 0.152(6) 0.086(3) 0.017(3) 0.018(3) -0.035(3) C6F 0.056(2) 0.111(4) 0.063(2) 0.011(2) 0.0063(18) -0.012(2) C1G 0.067(2) 0.056(2) 0.056(2) 0.0031(16) 0.0152(16) -0.0050(17) C2G 0.083(3) 0.086(3) 0.097(3) 0.019(3) 0.034(3) -0.004(2) C3G 0.132(5) 0.094(4) 0.122(5) 0.013(4) 0.066(4) -0.020(4) C4G 0.140(5) 0.074(3) 0.081(3) 0.014(3) 0.032(3) -0.015(3) C5G 0.132(5) 0.065(3) 0.087(3) 0.019(2) 0.012(3) 0.009(3) C6G 0.085(3) 0.064(2) 0.079(3) 0.011(2) 0.017(2) 0.003(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 P2 2.1464(11) . ? Ni P3 2.2161(12) . ? Ni S1 2.2400(12) . ? Ni P1 2.2407(16) . ? Ni S2 2.3468(13) . ? S1 C2 1.747(4) . ? S2 C1 1.738(4) . ? S3 C3 1.729(5) . ? S3 C1 1.747(4) . ? S4 C3 1.721(5) . ? S4 C2 1.748(4) . ? S5 C3 1.653(4) . ? P1 C1B 1.819(4) . ? P1 C1C 1.828(4) . ? P1 C1A 1.830(4) . ? P1 C1A1 1.866(6) . ? P2 C1D 1.822(3) . ? P2 C6C 1.825(4) . ? P2 C1E 1.828(4) . ? P3 C1G 1.824(4) . ? P3 C6E 1.830(4) . ? P3 C1F 1.835(4) . ? C1 C2 1.340(6) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A H2A 0.9300 . ? C3A C4A 1.3900 . ? C3A H3A 0.9300 . ? C4A C5A 1.3900 . ? C4A H4A 0.9300 . ? C5A C6A 1.3900 . ? C5A H5A 0.9300 . ? C6A H6A 0.9300 . ? C1A1 C2A1 1.3900 . ? C1A1 C6A1 1.3900 . ? C2A1 C3A1 1.3900 . ? C2A1 H2A1 0.9300 . ? C3A1 C4A1 1.3900 . ? C3A1 H3A1 0.9300 . ? C4A1 C5A1 1.3900 . ? C4A1 H4A1 0.9300 . ? C5A1 C6A1 1.3900 . ? C5A1 H5A1 0.9300 . ? C6A1 H6A1 0.9300 . ? C1B C2B 1.374(6) . ? C1B C6B 1.381(6) . ? C2B C3B 1.392(7) . ? C2B H2B 0.9300 . ? C3B C4B 1.351(8) . ? C3B H3B 0.9300 . ? C4B C5B 1.362(7) . ? C4B H4B 0.9300 . ? C5B C6B 1.376(6) . ? C5B H5B 0.9300 . ? C6B H6B 0.9300 . ? C1C C6C 1.384(5) . ? C1C C2C 1.399(5) . ? C2C C3C 1.382(6) . ? C2C H2C 0.9300 . ? C3C C4C 1.365(7) . ? C3C H3C 0.9300 . ? C4C C5C 1.392(6) . ? C4C H4C 0.9300 . ? C5C C6C 1.400(5) . ? C5C H5C 0.9300 . ? C1D C2D 1.383(6) . ? C1D C6D 1.390(5) . ? C2D C3D 1.391(6) . ? C2D H2D 0.9300 . ? C3D C4D 1.382(8) . ? C3D H3D 0.9300 . ? C4D C5D 1.353(7) . ? C4D H4D 0.9300 . ? C5D C6D 1.387(6) . ? C5D H5D 0.9300 . ? C6D H6D 0.9300 . ? C1E C6E 1.382(5) . ? C1E C2E 1.414(5) . ? C2E C3E 1.372(6) . ? C2E H2E 0.9300 . ? C3E C4E 1.378(7) . ? C3E H3E 0.9300 . ? C4E C5E 1.368(6) . ? C4E H4E 0.9300 . ? C5E C6E 1.400(5) . ? C5E H5E 0.9300 . ? C1F C6F 1.372(5) . ? C1F C2F 1.392(5) . ? C2F C3F 1.382(6) . ? C2F H2F 0.9300 . ? C3F C4F 1.370(7) . ? C3F H3F 0.9300 . ? C4F C5F 1.377(8) . ? C4F H4F 0.9300 . ? C5F C6F 1.387(6) . ? C5F H5F 0.9300 . ? C6F H6F 0.9300 . ? C1G C6G 1.375(6) . ? C1G C2G 1.380(6) . ? C2G C3G 1.394(7) . ? C2G H2G 0.9300 . ? C3G C4G 1.366(9) . ? C3G H3G 0.9300 . ? C4G C5G 1.361(8) . ? C4G H4G 0.9300 . ? C5G C6G 1.400(6) . ? C5G H5G 0.9300 . ? C6G H6G 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 P2 Ni P3 86.38(4) . . ? P2 Ni S1 174.93(5) . . ? P3 Ni S1 92.48(5) . . ? P2 Ni P1 86.72(4) . . ? P3 Ni P1 129.47(4) . . ? S1 Ni P1 90.21(5) . . ? P2 Ni S2 93.07(4) . . ? P3 Ni S2 122.58(5) . . ? S1 Ni S2 91.71(4) . . ? P1 Ni S2 107.74(5) . . ? C2 S1 Ni 99.12(14) . . ? C1 S2 Ni 96.69(13) . . ? C3 S3 C1 98.4(2) . . ? C3 S4 C2 98.1(2) . . ? C1B P1 C1C 103.17(17) . . ? C1B P1 C1A 105.7(2) . . ? C1C P1 C1A 105.6(2) . . ? C1B P1 C1A1 105.9(3) . . ? C1C P1 C1A1 100.8(3) . . ? C1A P1 C1A1 5.0(4) . . ? C1B P1 Ni 116.50(13) . . ? C1C P1 Ni 108.41(12) . . ? C1A P1 Ni 116.2(2) . . ? C1A1 P1 Ni 119.7(3) . . ? C1D P2 C6C 105.07(16) . . ? C1D P2 C1E 104.13(16) . . ? C6C P2 C1E 107.99(17) . . ? C1D P2 Ni 118.03(12) . . ? C6C P2 Ni 111.16(12) . . ? C1E P2 Ni 109.84(12) . . ? C1G P3 C6E 104.47(17) . . ? C1G P3 C1F 105.23(18) . . ? C6E P3 C1F 102.09(16) . . ? C1G P3 Ni 116.00(13) . . ? C6E P3 Ni 107.51(12) . . ? C1F P3 Ni 119.67(13) . . ? C2 C1 S2 124.7(3) . . ? C2 C1 S3 115.2(3) . . ? S2 C1 S3 120.1(2) . . ? C1 C2 S1 123.4(3) . . ? C1 C2 S4 116.3(3) . . ? S1 C2 S4 120.2(2) . . ? S5 C3 S4 123.9(3) . . ? S5 C3 S3 124.2(3) . . ? S4 C3 S3 111.9(2) . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 118.7(4) . . ? C6A C1A P1 121.1(4) . . ? C1A C2A C3A 120.0 . . ? C1A C2A H2A 120.0 . . ? C3A C2A H2A 120.0 . . ? C2A C3A C4A 120.0 . . ? C2A C3A H3A 120.0 . . ? C4A C3A H3A 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6A 120.0 . . ? C1A C6A H6A 120.0 . . ? C2A1 C1A1 C6A1 120.0 . . ? C2A1 C1A1 P1 117.9(5) . . ? C6A1 C1A1 P1 122.1(5) . . ? C1A1 C2A1 C3A1 120.0 . . ? C1A1 C2A1 H2A1 120.0 . . ? C3A1 C2A1 H2A1 120.0 . . ? C4A1 C3A1 C2A1 120.0 . . ? C4A1 C3A1 H3A1 120.0 . . ? C2A1 C3A1 H3A1 120.0 . . ? C3A1 C4A1 C5A1 120.0 . . ? C3A1 C4A1 H4A1 120.0 . . ? C5A1 C4A1 H4A1 120.0 . . ? C4A1 C5A1 C6A1 120.0 . . ? C4A1 C5A1 H5A1 120.0 . . ? C6A1 C5A1 H5A1 120.0 . . ? C5A1 C6A1 C1A1 120.0 . . ? C5A1 C6A1 H6A1 120.0 . . ? C1A1 C6A1 H6A1 120.0 . . ? C2B C1B C6B 118.0(4) . . ? C2B C1B P1 123.6(3) . . ? C6B C1B P1 118.3(3) . . ? C1B C2B C3B 119.6(5) . . ? C1B C2B H2B 120.2 . . ? C3B C2B H2B 120.2 . . ? C4B C3B C2B 121.6(5) . . ? C4B C3B H3B 119.2 . . ? C2B C3B H3B 119.2 . . ? C3B C4B C5B 119.3(5) . . ? C3B C4B H4B 120.4 . . ? C5B C4B H4B 120.4 . . ? C4B C5B C6B 120.0(5) . . ? C4B C5B H5B 120.0 . . ? C6B C5B H5B 120.0 . . ? C5B C6B C1B 121.5(4) . . ? C5B C6B H6B 119.2 . . ? C1B C6B H6B 119.2 . . ? C6C C1C C2C 118.6(3) . . ? C6C C1C P1 116.5(2) . . ? C2C C1C P1 124.9(3) . . ? C3C C2C C1C 120.3(4) . . ? C3C C2C H2C 119.8 . . ? C1C C2C H2C 119.8 . . ? C4C C3C C2C 120.7(4) . . ? C4C C3C H3C 119.7 . . ? C2C C3C H3C 119.7 . . ? C3C C4C C5C 120.5(4) . . ? C3C C4C H4C 119.7 . . ? C5C C4C H4C 119.7 . . ? C4C C5C C6C 118.7(4) . . ? C4C C5C H5C 120.6 . . ? C6C C5C H5C 120.6 . . ? C1C C6C C5C 121.1(3) . . ? C1C C6C P2 116.4(3) . . ? C5C C6C P2 122.5(3) . . ? C2D C1D C6D 119.6(4) . . ? C2D C1D P2 120.2(3) . . ? C6D C1D P2 120.1(3) . . ? C1D C2D C3D 120.1(4) . . ? C1D C2D H2D 119.9 . . ? C3D C2D H2D 119.9 . . ? C4D C3D C2D 119.7(5) . . ? C4D C3D H3D 120.2 . . ? C2D C3D H3D 120.2 . . ? C5D C4D C3D 120.1(4) . . ? C5D C4D H4D 120.0 . . ? C3D C4D H4D 120.0 . . ? C4D C5D C6D 121.3(4) . . ? C4D C5D H5D 119.3 . . ? C6D C5D H5D 119.3 . . ? C5D C6D C1D 119.2(4) . . ? C5D C6D H6D 120.4 . . ? C1D C6D H6D 120.4 . . ? C6E C1E C2E 120.2(3) . . ? C6E C1E P2 115.5(3) . . ? C2E C1E P2 124.2(3) . . ? C3E C2E C1E 118.9(4) . . ? C3E C2E H2E 120.5 . . ? C1E C2E H2E 120.5 . . ? C2E C3E C4E 121.0(4) . . ? C2E C3E H3E 119.5 . . ? C4E C3E H3E 119.5 . . ? C5E C4E C3E 120.2(4) . . ? C5E C4E H4E 119.9 . . ? C3E C4E H4E 119.9 . . ? C4E C5E C6E 120.6(4) . . ? C4E C5E H5E 119.7 . . ? C6E C5E H5E 119.7 . . ? C1E C6E C5E 119.0(3) . . ? C1E C6E P3 116.5(3) . . ? C5E C6E P3 124.4(3) . . ? C6F C1F C2F 119.1(4) . . ? C6F C1F P3 118.7(3) . . ? C2F C1F P3 121.9(3) . . ? C3F C2F C1F 120.1(4) . . ? C3F C2F H2F 120.0 . . ? C1F C2F H2F 120.0 . . ? C4F C3F C2F 120.5(4) . . ? C4F C3F H3F 119.7 . . ? C2F C3F H3F 119.7 . . ? C3F C4F C5F 119.6(4) . . ? C3F C4F H4F 120.2 . . ? C5F C4F H4F 120.2 . . ? C4F C5F C6F 120.2(5) . . ? C4F C5F H5F 119.9 . . ? C6F C5F H5F 119.9 . . ? C1F C6F C5F 120.5(4) . . ? C1F C6F H6F 119.8 . . ? C5F C6F H6F 119.8 . . ? C6G C1G C2G 119.0(4) . . ? C6G C1G P3 121.6(3) . . ? C2G C1G P3 119.2(3) . . ? C1G C2G C3G 119.7(5) . . ? C1G C2G H2G 120.2 . . ? C3G C2G H2G 120.2 . . ? C4G C3G C2G 121.1(6) . . ? C4G C3G H3G 119.4 . . ? C2G C3G H3G 119.4 . . ? C5G C4G C3G 119.4(5) . . ? C5G C4G H4G 120.3 . . ? C3G C4G H4G 120.3 . . ? C4G C5G C6G 120.3(5) . . ? C4G C5G H5G 119.8 . . ? C6G C5G H5G 119.8 . . ? C1G C6G C5G 120.4(5) . . ? C1G C6G H6G 119.8 . . ? C5G C6G H6G 119.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.722 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.073 #=END