# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_4 _database_code_depnum_ccdc_archive 'CCDC 897054' #TrackingRef 'twocifs.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_structural ; [Ni2L2][ClO4]2n(EtOH)n(MECN) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H60 Cl2 N6 Ni2 O8 S2' _chemical_formula_weight 957.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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 12.800(3) _cell_length_b 14.108(3) _cell_length_c 16.996(3) _cell_angle_alpha 108.23(3) _cell_angle_beta 97.53(3) _cell_angle_gamma 99.30(3) _cell_volume 2822.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8236 _exptl_absorpt_correction_T_max 0.9574 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20993 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9885 _reflns_number_gt 6491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-Area' _computing_cell_refinement 'STOE X-Area' _computing_data_reduction 'STOE X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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^)+(0.1209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0087(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9885 _refine_ls_number_parameters 500 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1872 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.67466(5) 0.05342(5) 0.28986(4) 0.0546(2) Uani 1 1 d . . . Ni2 Ni 0.93774(5) 0.07543(5) 0.30483(4) 0.0576(2) Uani 1 1 d . . . S1 S 0.81136(10) 0.00707(10) 0.37945(8) 0.0571(3) Uani 1 1 d . . . S2 S 0.82174(10) 0.18828(10) 0.30951(8) 0.0582(3) Uani 1 1 d . . . N1 N 0.5848(3) 0.0981(4) 0.3798(3) 0.0638(11) Uani 1 1 d . . . H1 H 0.5890 0.1676 0.3907 0.077 Uiso 1 1 calc R . . N2 N 0.5848(3) -0.0947(3) 0.2354(3) 0.0622(10) Uani 1 1 d . . . H2 H 0.6159 -0.1318 0.2649 0.075 Uiso 1 1 calc R . . N3 N 0.5911(3) 0.0891(4) 0.1924(3) 0.0637(11) Uani 1 1 d . . . H3 H 0.5180 0.0709 0.1928 0.076 Uiso 1 1 calc R . . N4 N 1.0112(3) 0.1222(3) 0.2167(3) 0.0623(11) Uani 1 1 d . . . H4 H 1.0824 0.1155 0.2263 0.075 Uiso 1 1 calc R . . N5 N 0.9867(4) -0.0612(4) 0.2600(3) 0.0740(13) Uani 1 1 d . . . H5 H 0.9522 -0.1036 0.2854 0.089 Uiso 1 1 calc R . . N6 N 1.0589(3) 0.1472(4) 0.4075(3) 0.0693(12) Uani 1 1 d . . . H6 H 1.0711 0.2162 0.4136 0.083 Uiso 1 1 calc R . . C1 C 0.8295(4) 0.1191(4) 0.4691(3) 0.0625(13) Uani 1 1 d . . . C2 C 0.9338(5) 0.1761(5) 0.5115(3) 0.0712(15) Uani 1 1 d . . . C3 C 0.9428(7) 0.2651(6) 0.5810(4) 0.094(2) Uani 1 1 d . . . H3B H 1.0128 0.3048 0.6090 0.113 Uiso 1 1 calc R . . C4 C 0.8544(7) 0.2979(5) 0.6109(4) 0.093(2) Uani 1 1 d . A . C5 C 0.7544(6) 0.2389(5) 0.5690(4) 0.0790(16) Uani 1 1 d . . . H5B H 0.6925 0.2595 0.5882 0.095 Uiso 1 1 calc R . . C6 C 0.7400(5) 0.1505(4) 0.4997(3) 0.0635(13) Uani 1 1 d . . . C7 C 0.8671(9) 0.3949(6) 0.6875(5) 0.132(4) Uani 1 1 d D . . C8A C 0.8958(19) 0.3706(15) 0.7681(10) 0.152(5) Uani 0.50 1 d PD A 1 H8A1 H 0.8989 0.4310 0.8173 0.229 Uiso 0.50 1 calc PR A 1 H8A2 H 0.9662 0.3516 0.7705 0.229 Uiso 0.50 1 calc PR A 1 H8A3 H 0.8407 0.3137 0.7683 0.229 Uiso 0.50 1 calc PR A 1 C9A C 0.7739(17) 0.4529(15) 0.6877(11) 0.152(5) Uani 0.50 1 d PD A 1 H9A1 H 0.8016 0.5254 0.7211 0.229 Uiso 0.50 1 calc PR A 1 H9A2 H 0.7173 0.4240 0.7124 0.229 Uiso 0.50 1 calc PR A 1 H9A3 H 0.7439 0.4461 0.6296 0.229 Uiso 0.50 1 calc PR A 1 C10A C 0.9704(16) 0.4765(12) 0.6851(11) 0.152(5) Uani 0.50 1 d PD A 1 H10A H 0.9596 0.4885 0.6312 0.229 Uiso 0.50 1 calc PR A 1 H10B H 1.0356 0.4494 0.6913 0.229 Uiso 0.50 1 calc PR A 1 H10C H 0.9784 0.5410 0.7316 0.229 Uiso 0.50 1 calc PR A 1 C8B C 0.811(2) 0.3652(18) 0.7505(12) 0.188(8) Uani 0.50 1 d PD A 2 H8B1 H 0.8296 0.4219 0.8045 0.282 Uiso 0.50 1 calc PR A 2 H8B2 H 0.8330 0.3049 0.7584 0.282 Uiso 0.50 1 calc PR A 2 H8B3 H 0.7325 0.3492 0.7300 0.282 Uiso 0.50 1 calc PR A 2 C9B C 0.810(2) 0.4646(17) 0.6588(12) 0.188(8) Uani 0.50 1 d PD A 2 H9B1 H 0.7919 0.5139 0.7075 0.282 Uiso 0.50 1 calc PR A 2 H9B2 H 0.7430 0.4249 0.6186 0.282 Uiso 0.50 1 calc PR A 2 H9B3 H 0.8558 0.5011 0.6312 0.282 Uiso 0.50 1 calc PR A 2 C10B C 0.9796(18) 0.4457(17) 0.7264(12) 0.188(8) Uani 0.50 1 d PD A 2 H10D H 1.0222 0.4433 0.6822 0.282 Uiso 0.50 1 calc PR A 2 H10E H 1.0086 0.4107 0.7631 0.282 Uiso 0.50 1 calc PR A 2 H10F H 0.9832 0.5170 0.7601 0.282 Uiso 0.50 1 calc PR A 2 C11 C 1.0337(5) 0.1411(6) 0.4891(4) 0.0809(17) Uani 1 1 d . . . H11A H 1.0956 0.1828 0.5348 0.097 Uiso 1 1 calc R . . H11B H 1.0262 0.0694 0.4869 0.097 Uiso 1 1 calc R . . C12 C 1.1628(5) 0.1163(6) 0.3967(5) 0.094(2) Uani 1 1 d . . . H12A H 1.2161 0.1519 0.4499 0.113 Uiso 1 1 calc R . . H12B H 1.1898 0.1387 0.3520 0.113 Uiso 1 1 calc R . . C13 C 1.1547(6) 0.0035(7) 0.3737(5) 0.101(2) Uani 1 1 d . . . H13A H 1.1115 -0.0212 0.4104 0.121 Uiso 1 1 calc R . . H13B H 1.2281 -0.0087 0.3861 0.121 Uiso 1 1 calc R . . C14 C 1.1045(5) -0.0595(6) 0.2822(5) 0.095(2) Uani 1 1 d . . . H14A H 1.1434 -0.0313 0.2450 0.114 Uiso 1 1 calc R . . H14B H 1.1139 -0.1305 0.2711 0.114 Uiso 1 1 calc R . . C15 C 0.9433(5) -0.1104(5) 0.1694(4) 0.0823(18) Uani 1 1 d . . . H15A H 0.8638 -0.1199 0.1604 0.099 Uiso 1 1 calc R . . H15B H 0.9601 -0.1792 0.1512 0.099 Uiso 1 1 calc R . . C16 C 0.9842(5) -0.0544(5) 0.1127(4) 0.0782(16) Uani 1 1 d . . . H16A H 1.0633 -0.0480 0.1192 0.094 Uiso 1 1 calc R . . H16B H 0.9516 -0.0964 0.0533 0.094 Uiso 1 1 calc R . . C17 C 0.9605(5) 0.0499(5) 0.1296(4) 0.0695(14) Uani 1 1 d . . . H17A H 0.8814 0.0438 0.1215 0.083 Uiso 1 1 calc R . . H17B H 0.9870 0.0788 0.0879 0.083 Uiso 1 1 calc R . . C18 C 1.0153(4) 0.2314(4) 0.2244(4) 0.0668(14) Uani 1 1 d . . . H18A H 1.0359 0.2747 0.2847 0.080 Uiso 1 1 calc R . . H18B H 1.0714 0.2533 0.1950 0.080 Uiso 1 1 calc R . . C19 C 0.9099(4) 0.2473(4) 0.1878(3) 0.0612(12) Uani 1 1 d . . . C20 C 0.8163(4) 0.2258(4) 0.2190(3) 0.0556(11) Uani 1 1 d . . . C21 C 0.7170(4) 0.2329(4) 0.1774(3) 0.0621(12) Uani 1 1 d . . . C22 C 0.7139(5) 0.2662(4) 0.1085(3) 0.0651(13) Uani 1 1 d . . . H22 H 0.6464 0.2713 0.0813 0.078 Uiso 1 1 calc R . . C23 C 0.8052(5) 0.2919(4) 0.0783(3) 0.0625(13) Uani 1 1 d . . . C24 C 0.9018(5) 0.2802(4) 0.1182(3) 0.0667(13) Uani 1 1 d . . . H24 H 0.9654 0.2952 0.0971 0.080 Uiso 1 1 calc R . . C25 C 0.8021(5) 0.3240(4) -0.0007(3) 0.0695(14) Uani 1 1 d . . . C26 C 0.6913(6) 0.3420(6) -0.0299(5) 0.096(2) Uani 1 1 d . . . H26A H 0.6758 0.3990 0.0142 0.144 Uiso 1 1 calc R . . H26B H 0.6362 0.2802 -0.0408 0.144 Uiso 1 1 calc R . . H26C H 0.6910 0.3586 -0.0818 0.144 Uiso 1 1 calc R . . C27 C 0.8219(8) 0.2367(6) -0.0719(4) 0.116(3) Uani 1 1 d . . . H27A H 0.7674 0.1748 -0.0816 0.174 Uiso 1 1 calc R . . H27B H 0.8939 0.2246 -0.0568 0.174 Uiso 1 1 calc R . . H27C H 0.8173 0.2543 -0.1235 0.174 Uiso 1 1 calc R . . C28 C 0.8810(7) 0.4226(7) 0.0189(5) 0.119(3) Uani 1 1 d . . . H28A H 0.8636 0.4755 0.0652 0.179 Uiso 1 1 calc R . . H28B H 0.8772 0.4430 -0.0313 0.179 Uiso 1 1 calc R . . H28C H 0.9541 0.4138 0.0355 0.179 Uiso 1 1 calc R . . C29 C 0.6140(4) 0.1994(5) 0.2031(4) 0.0718(15) Uani 1 1 d . . . H29A H 0.6178 0.2398 0.2631 0.086 Uiso 1 1 calc R . . H29B H 0.5537 0.2137 0.1689 0.086 Uiso 1 1 calc R . . C30 C 0.6084(5) 0.0238(5) 0.1095(3) 0.0737(15) Uani 1 1 d . . . H30A H 0.6869 0.0322 0.1105 0.088 Uiso 1 1 calc R . . H30B H 0.5767 0.0475 0.0647 0.088 Uiso 1 1 calc R . . C31 C 0.5593(5) -0.0881(5) 0.0880(4) 0.0760(15) Uani 1 1 d . . . H31A H 0.4806 -0.0961 0.0854 0.091 Uiso 1 1 calc R . . H31B H 0.5705 -0.1256 0.0310 0.091 Uiso 1 1 calc R . . C32 C 0.6028(5) -0.1377(5) 0.1480(3) 0.0699(14) Uani 1 1 d . . . H32A H 0.5688 -0.2114 0.1255 0.084 Uiso 1 1 calc R . . H32B H 0.6813 -0.1312 0.1499 0.084 Uiso 1 1 calc R . . C33 C 0.4689(4) -0.1168(5) 0.2378(4) 0.0734(15) Uani 1 1 d . . . H33A H 0.4426 -0.1916 0.2208 0.088 Uiso 1 1 calc R . . H33B H 0.4287 -0.0930 0.1965 0.088 Uiso 1 1 calc R . . C34 C 0.4457(5) -0.0654(5) 0.3253(4) 0.0800(17) Uani 1 1 d . . . H34A H 0.3691 -0.0915 0.3253 0.096 Uiso 1 1 calc R . . H34B H 0.4905 -0.0854 0.3669 0.096 Uiso 1 1 calc R . . C35 C 0.4670(5) 0.0484(5) 0.3534(4) 0.0769(16) Uani 1 1 d . . . H35A H 0.4307 0.0737 0.4014 0.092 Uiso 1 1 calc R . . H35B H 0.4350 0.0689 0.3066 0.092 Uiso 1 1 calc R . . C36 C 0.6292(5) 0.0876(5) 0.4620(3) 0.0699(14) Uani 1 1 d . . . H36A H 0.5809 0.1084 0.5023 0.084 Uiso 1 1 calc R . . H36B H 0.6302 0.0149 0.4528 0.084 Uiso 1 1 calc R . . Cl1 Cl 1.28594(12) 0.09789(15) 0.12139(11) 0.0854(5) Uani 1 1 d D . . O1A O 1.1970(7) 0.0802(9) 0.0597(6) 0.129(2) Uani 0.592(10) 1 d PD B 1 O2A O 1.3561(8) 0.1928(8) 0.1303(7) 0.129(2) Uani 0.592(10) 1 d PD B 1 O3A O 1.2492(7) 0.1019(9) 0.1979(6) 0.129(2) Uani 0.592(10) 1 d PD B 1 O4A O 1.3536(7) 0.0282(8) 0.1082(7) 0.129(2) Uani 0.592(10) 1 d PD B 1 O1B O 1.2195(10) 0.0290(11) 0.0425(8) 0.129(2) Uani 0.41 1 d PD B 2 O2B O 1.3733(10) 0.1575(12) 0.1013(10) 0.129(2) Uani 0.41 1 d PD B 2 O3B O 1.2228(10) 0.1568(11) 0.1682(9) 0.129(2) Uani 0.41 1 d PD B 2 O4B O 1.3314(10) 0.0391(11) 0.1660(9) 0.129(2) Uani 0.41 1 d PD B 2 Cl2 Cl 0.58605(16) -0.27792(15) 0.39123(12) 0.0956(5) Uani 1 1 d D . . O6A O 0.5621(9) -0.2705(8) 0.3093(6) 0.136(2) Uani 0.658(10) 1 d PD C 1 O5A O 0.5197(8) -0.3511(7) 0.4068(6) 0.136(2) Uani 0.658(10) 1 d PD C 1 O7A O 0.5956(9) -0.1740(7) 0.4528(6) 0.136(2) Uani 0.658(10) 1 d PD C 1 O8A O 0.6986(7) -0.2893(7) 0.4012(6) 0.136(2) Uani 0.658(10) 1 d PD C 1 O5B O 0.4972(13) -0.3163(13) 0.3250(10) 0.136(2) Uani 0.34 1 d PD C 2 O6B O 0.6582(13) -0.2164(12) 0.3661(11) 0.136(2) Uani 0.34 1 d PD C 2 O7B O 0.5557(15) -0.2215(13) 0.4618(10) 0.136(2) Uani 0.34 1 d PD C 2 O8B O 0.6249(15) -0.3571(12) 0.4038(10) 0.136(2) Uani 0.34 1 d PD C 2 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 0.0533(4) 0.0643(4) 0.0537(4) 0.0266(3) 0.0177(3) 0.0148(3) Ni2 0.0533(4) 0.0674(4) 0.0614(4) 0.0318(3) 0.0168(3) 0.0147(3) S1 0.0592(7) 0.0630(8) 0.0572(7) 0.0286(6) 0.0171(6) 0.0149(6) S2 0.0602(7) 0.0658(8) 0.0580(7) 0.0305(6) 0.0176(6) 0.0156(6) N1 0.067(3) 0.067(3) 0.069(3) 0.033(2) 0.025(2) 0.019(2) N2 0.058(2) 0.071(3) 0.064(3) 0.031(2) 0.012(2) 0.015(2) N3 0.052(2) 0.082(3) 0.069(3) 0.038(2) 0.019(2) 0.017(2) N4 0.054(2) 0.074(3) 0.071(3) 0.036(2) 0.023(2) 0.017(2) N5 0.072(3) 0.083(3) 0.089(3) 0.045(3) 0.039(3) 0.028(2) N6 0.057(2) 0.090(3) 0.073(3) 0.048(3) 0.011(2) 0.009(2) C1 0.075(3) 0.072(3) 0.046(3) 0.028(2) 0.015(2) 0.014(3) C2 0.079(4) 0.078(4) 0.053(3) 0.028(3) 0.008(3) 0.004(3) C3 0.116(6) 0.091(5) 0.063(4) 0.036(4) -0.002(4) -0.017(4) C4 0.137(7) 0.082(5) 0.062(4) 0.030(3) 0.021(4) 0.017(5) C5 0.110(5) 0.075(4) 0.059(3) 0.027(3) 0.025(3) 0.024(4) C6 0.078(3) 0.069(3) 0.050(3) 0.025(3) 0.022(2) 0.017(3) C7 0.222(11) 0.082(6) 0.063(4) 0.018(4) -0.005(6) -0.004(6) C8A 0.287(17) 0.077(7) 0.071(6) 0.010(5) 0.013(8) 0.026(9) C9A 0.287(17) 0.077(7) 0.071(6) 0.010(5) 0.013(8) 0.026(9) C10A 0.287(17) 0.077(7) 0.071(6) 0.010(5) 0.013(8) 0.026(9) C8B 0.35(3) 0.115(11) 0.081(8) 0.014(7) 0.047(11) 0.036(13) C9B 0.35(3) 0.115(11) 0.081(8) 0.014(7) 0.047(11) 0.036(13) C10B 0.35(3) 0.115(11) 0.081(8) 0.014(7) 0.047(11) 0.036(13) C11 0.068(3) 0.106(5) 0.074(4) 0.050(4) 0.001(3) 0.004(3) C12 0.068(4) 0.136(7) 0.100(5) 0.075(5) 0.014(3) 0.016(4) C13 0.075(4) 0.157(7) 0.119(6) 0.092(6) 0.035(4) 0.058(5) C14 0.083(4) 0.117(6) 0.131(6) 0.075(5) 0.054(4) 0.056(4) C15 0.084(4) 0.073(4) 0.104(5) 0.030(4) 0.048(4) 0.029(3) C16 0.081(4) 0.085(4) 0.082(4) 0.031(3) 0.038(3) 0.031(3) C17 0.067(3) 0.079(4) 0.069(3) 0.030(3) 0.021(3) 0.021(3) C18 0.057(3) 0.080(4) 0.071(3) 0.036(3) 0.019(3) 0.006(3) C19 0.063(3) 0.066(3) 0.063(3) 0.033(3) 0.015(2) 0.012(2) C20 0.063(3) 0.054(3) 0.059(3) 0.028(2) 0.020(2) 0.015(2) C21 0.060(3) 0.062(3) 0.073(3) 0.034(3) 0.017(2) 0.016(2) C22 0.070(3) 0.064(3) 0.073(3) 0.038(3) 0.011(3) 0.019(3) C23 0.078(3) 0.055(3) 0.061(3) 0.029(2) 0.014(3) 0.012(3) C24 0.078(3) 0.064(3) 0.065(3) 0.032(3) 0.021(3) 0.008(3) C25 0.084(4) 0.067(3) 0.065(3) 0.034(3) 0.015(3) 0.012(3) C26 0.106(5) 0.112(6) 0.087(4) 0.060(4) 0.013(4) 0.025(4) C27 0.187(9) 0.112(6) 0.073(4) 0.044(4) 0.047(5) 0.056(6) C28 0.131(6) 0.118(6) 0.123(6) 0.086(5) 0.008(5) -0.009(5) C29 0.060(3) 0.090(4) 0.091(4) 0.052(3) 0.028(3) 0.032(3) C30 0.073(3) 0.092(4) 0.051(3) 0.028(3) 0.008(3) -0.001(3) C31 0.073(4) 0.088(4) 0.064(3) 0.027(3) 0.016(3) 0.006(3) C32 0.071(3) 0.067(4) 0.067(3) 0.017(3) 0.020(3) 0.011(3) C33 0.061(3) 0.090(4) 0.075(3) 0.039(3) 0.017(3) 0.006(3) C34 0.060(3) 0.104(5) 0.084(4) 0.044(4) 0.026(3) 0.008(3) C35 0.063(3) 0.099(5) 0.079(4) 0.036(3) 0.029(3) 0.023(3) C36 0.076(3) 0.090(4) 0.058(3) 0.034(3) 0.030(3) 0.027(3) Cl1 0.0566(8) 0.1235(14) 0.0949(11) 0.0561(10) 0.0231(7) 0.0270(8) O1A 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) O2A 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) O3A 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) O4A 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) O1B 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) O2B 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) O3B 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) O4B 0.096(3) 0.168(5) 0.141(4) 0.070(3) 0.035(2) 0.034(3) Cl2 0.1085(13) 0.0998(13) 0.0989(12) 0.0448(10) 0.0443(10) 0.0377(10) O6A 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) O5A 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) O7A 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) O8A 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) O5B 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) O6B 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) O7B 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) O8B 0.155(5) 0.123(4) 0.137(4) 0.048(3) 0.036(3) 0.032(3) _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 N1 2.038(4) . ? Ni1 N2 2.069(5) . ? Ni1 N3 2.092(4) . ? Ni1 S2 2.3569(17) . ? Ni1 S1 2.4702(15) . ? Ni2 N6 2.038(5) . ? Ni2 N5 2.070(5) . ? Ni2 N4 2.085(4) . ? Ni2 S2 2.3369(15) . ? Ni2 S1 2.4400(14) . ? S1 C1 1.776(6) . ? S2 C20 1.774(5) . ? N1 C36 1.499(7) . ? N1 C35 1.500(7) . ? N1 H1 0.9300 . ? N2 C33 1.474(7) . ? N2 C32 1.482(7) . ? N2 H2 0.9300 . ? N3 C29 1.483(7) . ? N3 C30 1.489(7) . ? N3 H3 0.9300 . ? N4 C18 1.497(7) . ? N4 C17 1.498(7) . ? N4 H4 0.9300 . ? N5 C15 1.464(8) . ? N5 C14 1.500(8) . ? N5 H5 0.9300 . ? N6 C12 1.481(8) . ? N6 C11 1.490(7) . ? N6 H6 0.9300 . ? C1 C6 1.398(7) . ? C1 C2 1.410(8) . ? C2 C3 1.406(9) . ? C2 C11 1.495(9) . ? C3 C4 1.386(11) . ? C3 H3B 0.9500 . ? C4 C5 1.373(10) . ? C4 C7 1.534(11) . ? C5 C6 1.388(8) . ? C5 H5B 0.9500 . ? C6 C36 1.486(8) . ? C7 C10B 1.464(19) . ? C7 C9B 1.480(19) . ? C7 C8B 1.494(18) . ? C7 C8A 1.527(16) . ? C7 C9A 1.553(17) . ? C7 C10A 1.620(17) . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.498(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.521(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.517(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.497(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.490(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.398(7) . ? C19 C20 1.398(7) . ? C20 C21 1.405(7) . ? C21 C22 1.389(7) . ? C21 C29 1.494(7) . ? C22 C23 1.378(7) . ? C22 H22 0.9500 . ? C23 C24 1.390(8) . ? C23 C25 1.543(7) . ? C24 H24 0.9500 . ? C25 C28 1.494(9) . ? C25 C27 1.515(9) . ? C25 C26 1.527(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.510(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.503(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.529(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.491(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? Cl1 O1A 1.374(9) . ? Cl1 O3B 1.396(11) . ? Cl1 O4A 1.398(9) . ? Cl1 O4B 1.427(11) . ? Cl1 O3A 1.428(8) . ? Cl1 O2B 1.432(12) . ? Cl1 O2A 1.439(9) . ? Cl1 O1B 1.444(12) . ? Cl2 O5A 1.343(8) . ? Cl2 O8B 1.357(14) . ? Cl2 O7B 1.359(14) . ? Cl2 O6B 1.365(13) . ? Cl2 O5B 1.392(14) . ? Cl2 O6A 1.427(8) . ? Cl2 O8A 1.469(9) . ? Cl2 O7A 1.486(9) . ? 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 N1 Ni1 N2 95.56(18) . . ? N1 Ni1 N3 99.88(16) . . ? N2 Ni1 N3 88.29(18) . . ? N1 Ni1 S2 109.40(14) . . ? N2 Ni1 S2 154.83(12) . . ? N3 Ni1 S2 90.52(13) . . ? N1 Ni1 S1 95.77(13) . . ? N2 Ni1 S1 93.83(12) . . ? N3 Ni1 S1 163.93(11) . . ? S2 Ni1 S1 80.82(5) . . ? N6 Ni2 N5 98.5(2) . . ? N6 Ni2 N4 98.12(17) . . ? N5 Ni2 N4 87.94(17) . . ? N6 Ni2 S2 105.57(15) . . ? N5 Ni2 S2 155.77(16) . . ? N4 Ni2 S2 91.42(12) . . ? N6 Ni2 S1 96.12(12) . . ? N5 Ni2 S1 92.92(13) . . ? N4 Ni2 S1 165.45(13) . . ? S2 Ni2 S1 81.85(5) . . ? C1 S1 Ni2 97.94(17) . . ? C1 S1 Ni1 95.65(18) . . ? Ni2 S1 Ni1 84.44(4) . . ? C20 S2 Ni2 110.08(16) . . ? C20 S2 Ni1 110.54(18) . . ? Ni2 S2 Ni1 89.33(5) . . ? C36 N1 C35 109.7(4) . . ? C36 N1 Ni1 113.0(3) . . ? C35 N1 Ni1 114.9(4) . . ? C36 N1 H1 106.2 . . ? C35 N1 H1 106.2 . . ? Ni1 N1 H1 106.2 . . ? C33 N2 C32 110.8(4) . . ? C33 N2 Ni1 120.0(4) . . ? C32 N2 Ni1 109.0(3) . . ? C33 N2 H2 105.3 . . ? C32 N2 H2 105.3 . . ? Ni1 N2 H2 105.3 . . ? C29 N3 C30 112.7(4) . . ? C29 N3 Ni1 114.3(4) . . ? C30 N3 Ni1 109.7(3) . . ? C29 N3 H3 106.5 . . ? C30 N3 H3 106.5 . . ? Ni1 N3 H3 106.5 . . ? C18 N4 C17 112.3(4) . . ? C18 N4 Ni2 115.0(3) . . ? C17 N4 Ni2 109.5(3) . . ? C18 N4 H4 106.5 . . ? C17 N4 H4 106.5 . . ? Ni2 N4 H4 106.5 . . ? C15 N5 C14 112.4(5) . . ? C15 N5 Ni2 110.0(4) . . ? C14 N5 Ni2 117.5(4) . . ? C15 N5 H5 105.3 . . ? C14 N5 H5 105.3 . . ? Ni2 N5 H5 105.3 . . ? C12 N6 C11 108.9(4) . . ? C12 N6 Ni2 113.9(4) . . ? C11 N6 Ni2 115.5(3) . . ? C12 N6 H6 105.9 . . ? C11 N6 H6 105.9 . . ? Ni2 N6 H6 105.9 . . ? C6 C1 C2 119.1(5) . . ? C6 C1 S1 120.2(4) . . ? C2 C1 S1 120.7(4) . . ? C3 C2 C1 118.0(6) . . ? C3 C2 C11 119.4(6) . . ? C1 C2 C11 122.4(5) . . ? C4 C3 C2 123.2(7) . . ? C4 C3 H3B 118.4 . . ? C2 C3 H3B 118.4 . . ? C5 C4 C3 116.9(6) . . ? C5 C4 C7 121.2(8) . . ? C3 C4 C7 121.9(8) . . ? C4 C5 C6 122.7(6) . . ? C4 C5 H5B 118.6 . . ? C6 C5 H5B 118.6 . . ? C5 C6 C1 120.0(6) . . ? C5 C6 C36 119.0(5) . . ? C1 C6 C36 121.0(5) . . ? C10B C7 C9B 110.6(11) . . ? C10B C7 C8B 109.9(10) . . ? C9B C7 C8B 107.8(11) . . ? C10B C7 C8A 71.8(10) . . ? C9B C7 C8A 138.5(12) . . ? C8B C7 C8A 41.7(11) . . ? C10B C7 C4 113.7(12) . . ? C9B C7 C4 107.2(10) . . ? C8B C7 C4 107.5(11) . . ? C8A C7 C4 109.1(10) . . ? C10B C7 C9A 123.3(14) . . ? C9B C7 C9A 28.5(10) . . ? C8B C7 C9A 79.3(11) . . ? C8A C7 C9A 114.0(10) . . ? C4 C7 C9A 115.9(10) . . ? C10B C7 C10A 35.0(9) . . ? C9B C7 C10A 81.0(11) . . ? C8B C7 C10A 139.4(12) . . ? C8A C7 C10A 106.3(9) . . ? C4 C7 C10A 107.3(9) . . ? C9A C7 C10A 103.5(9) . . ? C7 C8A H8A1 109.5 . . ? C7 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C7 C9A H9A1 109.5 . . ? C7 C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C7 C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C7 C10A H10A 109.5 . . ? C7 C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C7 C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C7 C8B H8B1 109.5 . . ? C7 C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7 C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7 C9B H9B1 109.5 . . ? C7 C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7 C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7 C10B H10D 109.5 . . ? C7 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? N6 C11 C2 115.2(5) . . ? N6 C11 H11A 108.5 . . ? C2 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? C2 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N6 C12 C13 113.5(5) . . ? N6 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N6 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 115.2(6) . . ? C12 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? C12 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N5 C14 C13 113.2(5) . . ? N5 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? N5 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? N5 C15 C16 116.2(6) . . ? N5 C15 H15A 108.2 . . ? C16 C15 H15A 108.2 . . ? N5 C15 H15B 108.2 . . ? C16 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C15 114.9(5) . . ? C17 C16 H16A 108.5 . . ? C15 C16 H16A 108.5 . . ? C17 C16 H16B 108.5 . . ? C15 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C16 C17 N4 113.2(5) . . ? C16 C17 H17A 108.9 . . ? N4 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? N4 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C19 C18 N4 112.3(4) . . ? C19 C18 H18A 109.1 . . ? N4 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? N4 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C24 C19 C20 118.3(5) . . ? C24 C19 C18 119.9(5) . . ? C20 C19 C18 121.8(4) . . ? C19 C20 C21 119.5(4) . . ? C19 C20 S2 120.6(4) . . ? C21 C20 S2 119.9(4) . . ? C22 C21 C20 119.6(5) . . ? C22 C21 C29 119.5(5) . . ? C20 C21 C29 120.9(4) . . ? C23 C22 C21 122.3(5) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C22 C23 C24 117.1(5) . . ? C22 C23 C25 122.8(5) . . ? C24 C23 C25 119.9(5) . . ? C23 C24 C19 123.1(5) . . ? C23 C24 H24 118.5 . . ? C19 C24 H24 118.5 . . ? C28 C25 C27 113.7(6) . . ? C28 C25 C26 106.5(5) . . ? C27 C25 C26 106.8(6) . . ? C28 C25 C23 110.2(5) . . ? C27 C25 C23 108.0(5) . . ? C26 C25 C23 111.6(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 C21 112.8(4) . . ? N3 C29 H29A 109.0 . . ? C21 C29 H29A 109.0 . . ? N3 C29 H29B 109.0 . . ? C21 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? N3 C30 C31 113.3(4) . . ? N3 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? N3 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 115.8(5) . . ? C32 C31 H31A 108.3 . . ? C30 C31 H31A 108.3 . . ? C32 C31 H31B 108.3 . . ? C30 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? N2 C32 C31 114.8(5) . . ? N2 C32 H32A 108.6 . . ? C31 C32 H32A 108.6 . . ? N2 C32 H32B 108.6 . . ? C31 C32 H32B 108.6 . . ? H32A C32 H32B 107.5 . . ? N2 C33 C34 112.4(5) . . ? N2 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? N2 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 114.6(5) . . ? C35 C34 H34A 108.6 . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C33 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C34 C35 N1 113.4(5) . . ? C34 C35 H35A 108.9 . . ? N1 C35 H35A 108.9 . . ? C34 C35 H35B 108.9 . . ? N1 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C6 C36 N1 112.6(4) . . ? C6 C36 H36A 109.1 . . ? N1 C36 H36A 109.1 . . ? C6 C36 H36B 109.1 . . ? N1 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? O1A Cl1 O3B 79.8(7) . . ? O1A Cl1 O4A 118.1(6) . . ? O3B Cl1 O4A 153.8(7) . . ? O1A Cl1 O4B 135.5(8) . . ? O3B Cl1 O4B 111.0(7) . . ? O4A Cl1 O4B 42.8(6) . . ? O1A Cl1 O3A 107.9(5) . . ? O3B Cl1 O3A 46.7(6) . . ? O4A Cl1 O3A 107.4(5) . . ? O4B Cl1 O3A 64.8(6) . . ? O1A Cl1 O2B 106.9(8) . . ? O3B Cl1 O2B 113.3(8) . . ? O4A Cl1 O2B 81.2(7) . . ? O4B Cl1 O2B 107.3(7) . . ? O3A Cl1 O2B 133.8(8) . . ? O1A Cl1 O2A 108.7(6) . . ? O3B Cl1 O2A 86.8(7) . . ? O4A Cl1 O2A 103.4(5) . . ? O4B Cl1 O2A 114.7(8) . . ? O3A Cl1 O2A 111.3(6) . . ? O2B Cl1 O2A 27.0(7) . . ? O1A Cl1 O1B 33.1(6) . . ? O3B Cl1 O1B 109.2(7) . . ? O4A Cl1 O1B 85.2(7) . . ? O4B Cl1 O1B 108.6(8) . . ? O3A Cl1 O1B 118.5(7) . . ? O2B Cl1 O1B 107.2(7) . . ? O2A Cl1 O1B 124.0(8) . . ? O5A Cl2 O8B 60.9(8) . . ? O5A Cl2 O7B 79.3(8) . . ? O8B Cl2 O7B 111.0(8) . . ? O5A Cl2 O6B 170.7(8) . . ? O8B Cl2 O6B 112.5(9) . . ? O7B Cl2 O6B 109.8(9) . . ? O5A Cl2 O5B 72.6(8) . . ? O8B Cl2 O5B 109.0(9) . . ? O7B Cl2 O5B 109.2(9) . . ? O6B Cl2 O5B 105.1(8) . . ? O5A Cl2 O6A 116.6(6) . . ? O8B Cl2 O6A 122.0(8) . . ? O7B Cl2 O6A 125.9(8) . . ? O6B Cl2 O6A 60.0(7) . . ? O5B Cl2 O6A 45.2(7) . . ? O5A Cl2 O8A 112.6(5) . . ? O8B Cl2 O8A 52.2(8) . . ? O7B Cl2 O8A 116.1(9) . . ? O6B Cl2 O8A 62.3(8) . . ? O5B Cl2 O8A 134.6(8) . . ? O6A Cl2 O8A 104.7(5) . . ? O5A Cl2 O7A 113.3(5) . . ? O8B Cl2 O7A 128.4(8) . . ? O7B Cl2 O7A 34.0(7) . . ? O6B Cl2 O7A 75.9(8) . . ? O5B Cl2 O7A 117.8(8) . . ? O6A Cl2 O7A 106.5(5) . . ? O8A Cl2 O7A 101.8(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.611 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.087 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.009 0.500 0.472 879.5 37.9 _platon_squeeze_details ; ; data_5 _database_code_depnum_ccdc_archive 'CCDC 897055' #TrackingRef 'twocifs.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_structural ; [Ni2L2][BPh4]2(MeOH) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H104 B2 N6 Ni2 O S2' _chemical_formula_weight 1428.90 _chemical_compound_source ; Crystals were obtained by recrystallization from MeCN/MeOH. ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 16.917(3) _cell_length_b 23.635(5) _cell_length_c 19.856(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7939(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3048 _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9036 _exptl_absorpt_correction_T_max 0.9718 _exptl_absorpt_process_details STOE-X-AREA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25062 _diffrn_reflns_av_R_equivalents 0.1091 _diffrn_reflns_av_sigmaI/netI 0.1178 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7156 _reflns_number_gt 3725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-Area' _computing_cell_refinement 'STOE X-Area' _computing_data_reduction 'STOE X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00041(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7156 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.0298(16) 0.7000(10) 0.1356(14) 0.286(11) Uiso 0.50 1 d P . . H1B H 0.0168 0.6906 0.1375 0.429 Uiso 0.50 1 d PR . . C59 C -0.0740(16) 0.6586(11) 0.0904(13) 0.187(10) Uiso 0.50 1 d P . . H59A H -0.1270 0.6541 0.1069 0.280 Uiso 0.50 1 d PR . . H59B H -0.0478 0.6225 0.0904 0.280 Uiso 0.50 1 d PR . . H59C H -0.0755 0.6733 0.0453 0.280 Uiso 0.50 1 d PR . . Ni1 Ni 0.28904(3) 0.67821(2) 0.07127(3) 0.03411(17) Uani 1 1 d . . . S1 S 0.18533(9) 0.7500 0.09581(9) 0.0402(4) Uani 1 2 d S . . S2 S 0.33415(9) 0.7500 0.00227(9) 0.0341(4) Uani 1 2 d S . . N1 N 0.2190(2) 0.62736(15) 0.0144(2) 0.0407(10) Uani 1 1 d . . . H1A H 0.2351 0.6319 -0.0301 0.049 Uiso 1 1 calc R . . N2 N 0.2686(2) 0.63462(17) 0.1585(2) 0.0440(10) Uani 1 1 d . . . H2 H 0.2198 0.6470 0.1741 0.053 Uiso 1 1 calc R . . N3 N 0.3976(2) 0.63769(15) 0.0676(2) 0.0349(9) Uani 1 1 d . . . H3A H 0.3874 0.5994 0.0742 0.042 Uiso 1 1 calc R . . C1 C 0.1375(4) 0.7500 0.0156(3) 0.0365(16) Uani 1 2 d S . . C2 C 0.1163(2) 0.69914(19) -0.0152(3) 0.0370(12) Uani 1 1 d . . . C3 C 0.0771(3) 0.6998(2) -0.0771(3) 0.0419(12) Uani 1 1 d . . . H3B H 0.0634 0.6647 -0.0974 0.050 Uiso 1 1 calc R . . C4 C 0.0571(3) 0.7500 -0.1106(4) 0.0374(16) Uani 1 2 d S . . C7 C 0.0131(4) 0.7500 -0.1768(4) 0.0429(18) Uani 1 2 d S . . C8 C 0.0339(4) 0.6977(2) -0.2188(3) 0.0626(16) Uani 1 1 d . . . H8A H 0.0046 0.6988 -0.2614 0.094 Uiso 1 1 calc R . . H8B H 0.0197 0.6634 -0.1938 0.094 Uiso 1 1 calc R . . H8C H 0.0908 0.6975 -0.2282 0.094 Uiso 1 1 calc R . . C9 C -0.0761(4) 0.7500 -0.1620(5) 0.083(3) Uani 1 2 d S . . H9A H -0.1055 0.7500 -0.2046 0.125 Uiso 1 2 calc SR . . H9B H -0.0899 0.7839 -0.1360 0.125 Uiso 0.50 1 calc PR . . H9C H -0.0899 0.7161 -0.1360 0.125 Uiso 0.50 1 calc PR . . C11 C 0.1330(3) 0.6432(2) 0.0170(3) 0.0447(13) Uani 1 1 d . . . H11A H 0.1017 0.6136 -0.0061 0.054 Uiso 1 1 calc R . . H11B H 0.1158 0.6445 0.0646 0.054 Uiso 1 1 calc R . . C12 C 0.2280(3) 0.5658(2) 0.0306(3) 0.0488(14) Uani 1 1 d . . . H12A H 0.2835 0.5544 0.0221 0.059 Uiso 1 1 calc R . . H12B H 0.1939 0.5436 0.0000 0.059 Uiso 1 1 calc R . . C13 C 0.2070(3) 0.5514(2) 0.1024(3) 0.0534(14) Uani 1 1 d . . . H13A H 0.1541 0.5673 0.1121 0.064 Uiso 1 1 calc R . . H13B H 0.2028 0.5097 0.1062 0.064 Uiso 1 1 calc R . . C14 C 0.2633(3) 0.5719(2) 0.1555(3) 0.0521(14) Uani 1 1 d . . . H14A H 0.2459 0.5575 0.1999 0.062 Uiso 1 1 calc R . . H14B H 0.3165 0.5563 0.1462 0.062 Uiso 1 1 calc R . . C15 C 0.3279(3) 0.6538(3) 0.2095(3) 0.0543(14) Uani 1 1 d . . . H15A H 0.3133 0.6381 0.2540 0.065 Uiso 1 1 calc R . . H15B H 0.3258 0.6956 0.2128 0.065 Uiso 1 1 calc R . . C16 C 0.4128(3) 0.6359(2) 0.1929(3) 0.0516(14) Uani 1 1 d . . . H16A H 0.4477 0.6496 0.2295 0.062 Uiso 1 1 calc R . . H16B H 0.4152 0.5941 0.1931 0.062 Uiso 1 1 calc R . . C17 C 0.4460(3) 0.6566(2) 0.1266(2) 0.0437(13) Uani 1 1 d . . . H17A H 0.4483 0.6985 0.1272 0.052 Uiso 1 1 calc R . . H17B H 0.5007 0.6423 0.1214 0.052 Uiso 1 1 calc R . . C18 C 0.4408(3) 0.64214(19) 0.0017(3) 0.0385(11) Uani 1 1 d . . . H18A H 0.4030 0.6352 -0.0354 0.046 Uiso 1 1 calc R . . H18B H 0.4816 0.6121 -0.0002 0.046 Uiso 1 1 calc R . . C19 C 0.4804(3) 0.69882(19) -0.0097(2) 0.0347(11) Uani 1 1 d . . . C20 C 0.4388(4) 0.7500 -0.0055(3) 0.0311(15) Uani 1 2 d S . . C23 C 0.6012(4) 0.7500 -0.0367(4) 0.0386(16) Uani 1 2 d S . . C24 C 0.5606(3) 0.7001(2) -0.0258(2) 0.0367(11) Uani 1 1 d . . . H24 H 0.5884 0.6653 -0.0295 0.044 Uiso 1 1 calc R . . C25 C 0.6870(3) 0.7500 -0.0628(4) 0.0410(17) Uani 1 2 d S . . C26 C 0.7326(4) 0.6984(3) -0.0405(5) 0.106(3) Uani 1 1 d . . . H26A H 0.7350 0.6975 0.0088 0.160 Uiso 1 1 calc R . . H26B H 0.7863 0.7001 -0.0588 0.160 Uiso 1 1 calc R . . H26C H 0.7060 0.6643 -0.0569 0.160 Uiso 1 1 calc R . . C27 C 0.6845(6) 0.7500 -0.1383(5) 0.130(6) Uani 1 2 d S . . H27A H 0.6551 0.7832 -0.1541 0.195 Uiso 0.50 1 calc PR . . H27B H 0.6583 0.7155 -0.1541 0.195 Uiso 0.50 1 calc PR . . H27C H 0.7386 0.7513 -0.1560 0.195 Uiso 1 2 calc SR . . B B 0.0738(4) 0.4853(2) 0.2897(3) 0.0418(14) Uani 1 1 d . . . C35 C 0.1096(3) 0.5489(2) 0.3024(3) 0.0454(13) Uani 1 1 d . . . C36 C 0.1523(3) 0.5618(2) 0.3611(3) 0.0590(16) Uani 1 1 d . . . H36 H 0.1628 0.5320 0.3920 0.071 Uiso 1 1 calc R . . C37 C 0.1801(4) 0.6154(3) 0.3763(4) 0.082(2) Uani 1 1 d . . . H37 H 0.2092 0.6215 0.4165 0.098 Uiso 1 1 calc R . . C38 C 0.1657(4) 0.6592(3) 0.3338(5) 0.088(2) Uani 1 1 d . . . H38 H 0.1842 0.6960 0.3446 0.105 Uiso 1 1 calc R . . C39 C 0.1239(4) 0.6502(3) 0.2748(4) 0.070(2) Uani 1 1 d . . . H39 H 0.1135 0.6807 0.2450 0.084 Uiso 1 1 calc R . . C40 C 0.0970(3) 0.5953(2) 0.2596(3) 0.0547(15) Uani 1 1 d . . . H41 H 0.0692 0.5894 0.2186 0.066 Uiso 1 1 calc R . . C41 C 0.1373(3) 0.4366(2) 0.3149(2) 0.0407(12) Uani 1 1 d . . . C42 C 0.2191(3) 0.4428(2) 0.3137(3) 0.0569(14) Uani 1 1 d . . . H42 H 0.2402 0.4790 0.3032 0.068 Uiso 1 1 calc R . . C43 C 0.2721(3) 0.3987(3) 0.3272(3) 0.0647(17) Uani 1 1 d . . . H43 H 0.3275 0.4051 0.3264 0.078 Uiso 1 1 calc R . . C44 C 0.2423(4) 0.3454(3) 0.3417(3) 0.0656(17) Uani 1 1 d . . . H44 H 0.2772 0.3147 0.3502 0.079 Uiso 1 1 calc R . . C45 C 0.1620(4) 0.3374(2) 0.3437(3) 0.0573(15) Uani 1 1 d . . . H45 H 0.1413 0.3010 0.3536 0.069 Uiso 1 1 calc R . . C46 C 0.1103(3) 0.3823(2) 0.3312(3) 0.0458(13) Uani 1 1 d . . . H46 H 0.0550 0.3757 0.3338 0.055 Uiso 1 1 calc R . . C47 C -0.0084(3) 0.47778(18) 0.3333(3) 0.0400(12) Uani 1 1 d . . . C48 C -0.0712(3) 0.4431(2) 0.3122(3) 0.0480(13) Uani 1 1 d . . . H48 H -0.0692 0.4272 0.2683 0.058 Uiso 1 1 calc R . . C49 C -0.1365(3) 0.4310(2) 0.3527(3) 0.0509(14) Uani 1 1 d . . . H49 H -0.1777 0.4077 0.3358 0.061 Uiso 1 1 calc R . . C50 C -0.1417(3) 0.4525(2) 0.4169(3) 0.0505(14) Uani 1 1 d . . . H50 H -0.1856 0.4437 0.4448 0.061 Uiso 1 1 calc R . . C51 C -0.0816(3) 0.4875(2) 0.4402(3) 0.0469(13) Uani 1 1 d . . . H51 H -0.0844 0.5030 0.4844 0.056 Uiso 1 1 calc R . . C52 C -0.0170(3) 0.5000(2) 0.3987(3) 0.0449(13) Uani 1 1 d . . . H52 H 0.0229 0.5246 0.4154 0.054 Uiso 1 1 calc R . . C53 C 0.0569(3) 0.4733(2) 0.2096(3) 0.0452(13) Uani 1 1 d . . . C54 C 0.1015(3) 0.4362(2) 0.1702(3) 0.0503(14) Uani 1 1 d . . . H54 H 0.1446 0.4170 0.1906 0.060 Uiso 1 1 calc R . . C55 C 0.0858(4) 0.4263(3) 0.1029(3) 0.0674(18) Uani 1 1 d . . . H55 H 0.1178 0.4007 0.0781 0.081 Uiso 1 1 calc R . . C56 C 0.0238(5) 0.4535(3) 0.0722(4) 0.079(2) Uani 1 1 d . . . H56 H 0.0135 0.4470 0.0258 0.094 Uiso 1 1 calc R . . C57 C -0.0230(4) 0.4896(4) 0.1078(4) 0.082(2) Uani 1 1 d . . . H57 H -0.0658 0.5085 0.0865 0.098 Uiso 1 1 calc R . . C58 C -0.0072(4) 0.4986(3) 0.1757(3) 0.0670(17) Uani 1 1 d . . . H58 H -0.0412 0.5229 0.2005 0.080 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 0.0285(3) 0.0344(3) 0.0394(3) 0.0036(3) 0.0006(3) -0.0010(3) S1 0.0299(9) 0.0456(10) 0.0450(11) 0.000 0.0011(7) 0.000 S2 0.0302(8) 0.0297(9) 0.0424(10) 0.000 0.0042(8) 0.000 N1 0.042(2) 0.032(2) 0.048(2) 0.0064(19) 0.000(2) -0.0018(18) N2 0.032(2) 0.049(3) 0.051(3) 0.012(2) 0.0074(19) 0.0067(18) N3 0.038(2) 0.032(2) 0.035(2) 0.0016(19) 0.0000(19) -0.0031(16) C1 0.030(3) 0.043(4) 0.036(4) 0.000 -0.010(3) 0.000 C2 0.022(2) 0.038(3) 0.051(3) 0.004(2) -0.001(2) -0.0025(19) C3 0.036(2) 0.038(3) 0.052(3) 0.001(3) -0.001(3) -0.004(2) C4 0.019(3) 0.040(4) 0.053(5) 0.000 0.003(3) 0.000 C7 0.031(4) 0.050(4) 0.048(5) 0.000 -0.001(3) 0.000 C8 0.082(4) 0.052(3) 0.054(4) -0.011(3) -0.012(3) 0.000(3) C9 0.031(4) 0.136(9) 0.083(7) 0.000 -0.010(4) 0.000 C11 0.031(3) 0.041(3) 0.062(4) 0.009(3) -0.011(2) -0.004(2) C12 0.042(3) 0.035(3) 0.069(4) 0.008(3) -0.009(3) -0.005(2) C13 0.045(3) 0.038(3) 0.078(4) 0.021(3) 0.003(3) -0.004(3) C14 0.049(3) 0.051(3) 0.057(4) 0.023(3) 0.006(3) 0.001(2) C15 0.055(3) 0.067(4) 0.040(3) 0.007(3) 0.003(3) 0.009(3) C16 0.046(3) 0.063(4) 0.045(3) 0.008(3) -0.003(3) 0.007(3) C17 0.044(3) 0.045(3) 0.042(3) 0.003(2) -0.004(2) 0.004(2) C18 0.038(3) 0.033(3) 0.044(3) 0.002(2) 0.008(2) 0.000(2) C19 0.037(3) 0.031(2) 0.036(3) 0.000(2) 0.006(2) -0.001(2) C20 0.030(3) 0.033(4) 0.030(4) 0.000 0.007(3) 0.000 C23 0.038(4) 0.031(4) 0.047(4) 0.000 0.007(3) 0.000 C24 0.029(2) 0.036(3) 0.045(3) 0.000(2) 0.010(2) 0.005(2) C25 0.030(3) 0.037(4) 0.057(5) 0.000 0.011(3) 0.000 C26 0.046(4) 0.076(5) 0.198(9) 0.051(5) 0.033(4) 0.020(3) C27 0.048(6) 0.288(18) 0.055(6) 0.000 0.023(5) 0.000 B 0.047(3) 0.038(3) 0.040(3) -0.002(3) 0.001(3) -0.003(3) C35 0.047(3) 0.042(3) 0.048(3) -0.002(3) 0.010(3) -0.004(2) C36 0.059(4) 0.058(4) 0.060(4) -0.010(3) 0.002(3) -0.016(3) C37 0.086(5) 0.069(5) 0.090(6) -0.027(4) 0.009(4) -0.024(4) C38 0.086(5) 0.055(4) 0.123(7) -0.029(5) 0.043(5) -0.020(4) C39 0.072(4) 0.044(4) 0.094(6) 0.012(4) 0.050(4) 0.008(3) C40 0.053(3) 0.041(3) 0.070(4) -0.003(3) 0.027(3) 0.005(3) C41 0.044(3) 0.044(3) 0.034(3) -0.004(2) 0.001(2) 0.002(2) C42 0.053(3) 0.054(3) 0.064(4) 0.008(3) 0.000(3) 0.000(3) C43 0.045(3) 0.084(5) 0.065(4) 0.007(4) -0.003(3) 0.008(3) C44 0.066(4) 0.066(4) 0.064(4) 0.005(3) -0.001(3) 0.025(3) C45 0.072(4) 0.051(4) 0.050(4) 0.003(3) -0.001(3) 0.010(3) C46 0.050(3) 0.043(3) 0.044(3) -0.002(3) -0.002(3) 0.006(2) C47 0.050(3) 0.028(3) 0.042(3) 0.003(2) -0.002(2) 0.003(2) C48 0.050(3) 0.041(3) 0.053(3) -0.011(3) -0.001(3) -0.002(2) C49 0.042(3) 0.045(3) 0.066(4) 0.000(3) -0.001(3) -0.001(2) C50 0.048(3) 0.045(3) 0.058(4) 0.004(3) 0.013(3) 0.003(2) C51 0.052(3) 0.043(3) 0.046(3) 0.003(3) 0.001(3) 0.010(2) C52 0.048(3) 0.044(3) 0.043(3) 0.001(3) -0.006(3) 0.003(2) C53 0.056(3) 0.041(3) 0.039(3) 0.005(2) -0.005(3) -0.010(3) C54 0.069(4) 0.041(3) 0.040(3) -0.004(3) 0.004(3) -0.018(3) C55 0.100(5) 0.059(4) 0.043(4) -0.004(3) 0.011(4) -0.037(4) C56 0.107(6) 0.088(5) 0.042(4) 0.006(4) -0.013(4) -0.057(5) C57 0.074(5) 0.117(6) 0.054(4) 0.024(4) -0.025(4) -0.023(4) C58 0.068(4) 0.078(4) 0.055(4) 0.011(4) -0.007(3) -0.012(3) _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 O1 C59 1.53(3) . ? O1 H1B 0.8200 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? Ni1 N1 2.031(4) . ? Ni1 N2 2.045(4) . ? Ni1 N3 2.072(4) . ? Ni1 S2 2.3105(13) . ? Ni1 S1 2.4888(13) . ? S1 C1 1.786(7) . ? S1 Ni1 2.4888(13) 7_575 ? S2 C20 1.776(6) . ? S2 Ni1 2.3105(13) 7_575 ? N1 C12 1.499(6) . ? N1 C11 1.503(6) . ? N1 H1A 0.9300 . ? N2 C14 1.485(6) . ? N2 C15 1.495(6) . ? N2 H2 0.9300 . ? N3 C17 1.498(6) . ? N3 C18 1.504(6) . ? N3 H3A 0.9300 . ? C1 C2 1.396(6) 7_575 ? C1 C2 1.396(6) . ? C2 C3 1.397(7) . ? C2 C11 1.495(6) . ? C3 C4 1.401(6) . ? C3 H3B 0.9500 . ? C4 C3 1.401(6) 7_575 ? C4 C7 1.510(10) . ? C7 C8 1.533(7) . ? C7 C8 1.533(7) 7_575 ? C7 C9 1.538(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.507(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.502(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.533(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.512(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.515(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.394(6) . ? C19 C20 1.402(5) . ? C20 C19 1.402(5) 7_575 ? C23 C24 1.381(6) 7_575 ? C23 C24 1.381(6) . ? C23 C25 1.541(9) . ? C24 H24 0.9500 . ? C25 C27 1.499(12) . ? C25 C26 1.509(7) 7_575 ? C25 C26 1.509(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? B C53 1.641(8) . ? B C35 1.641(7) . ? B C47 1.648(8) . ? B C41 1.652(8) . ? C35 C36 1.403(8) . ? C35 C40 1.403(7) . ? C36 C37 1.385(8) . ? C36 H36 0.9500 . ? C37 C38 1.357(10) . ? C37 H37 0.9500 . ? C38 C39 1.385(10) . ? C38 H38 0.9500 . ? C39 C40 1.408(8) . ? C39 H39 0.9500 . ? C40 H41 0.9500 . ? C41 C42 1.392(7) . ? C41 C46 1.400(7) . ? C42 C43 1.401(8) . ? C42 H42 0.9500 . ? C43 C44 1.386(8) . ? C43 H43 0.9500 . ? C44 C45 1.372(8) . ? C44 H44 0.9500 . ? C45 C46 1.397(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.406(7) . ? C47 C52 1.408(7) . ? C48 C49 1.396(7) . ? C48 H48 0.9500 . ? C49 C50 1.375(7) . ? C49 H49 0.9500 . ? C50 C51 1.390(7) . ? C50 H50 0.9500 . ? C51 C52 1.402(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.395(7) . ? C53 C58 1.408(8) . ? C54 C55 1.383(8) . ? C54 H54 0.9500 . ? C55 C56 1.373(9) . ? C55 H55 0.9500 . ? C56 C57 1.363(10) . ? C56 H56 0.9500 . ? C57 C58 1.391(9) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C59 O1 H1B 108.9 . . ? O1 C59 H59A 109.1 . . ? O1 C59 H59B 110.1 . . ? H59A C59 H59B 109.5 . . ? O1 C59 H59C 109.2 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N1 Ni1 N2 94.28(16) . . ? N1 Ni1 N3 102.94(15) . . ? N2 Ni1 N3 86.93(15) . . ? N1 Ni1 S2 107.30(12) . . ? N2 Ni1 S2 158.14(13) . . ? N3 Ni1 S2 91.49(11) . . ? N1 Ni1 S1 95.81(12) . . ? N2 Ni1 S1 93.36(12) . . ? N3 Ni1 S1 161.18(11) . . ? S2 Ni1 S1 81.28(5) . . ? C1 S1 Ni1 98.34(17) . 7_575 ? C1 S1 Ni1 98.34(17) . . ? Ni1 S1 Ni1 85.96(6) 7_575 . ? C20 S2 Ni1 112.37(14) . 7_575 ? C20 S2 Ni1 112.37(14) . . ? Ni1 S2 Ni1 94.50(7) 7_575 . ? C12 N1 C11 109.5(4) . . ? C12 N1 Ni1 113.3(3) . . ? C11 N1 Ni1 113.5(3) . . ? C12 N1 H1A 106.7 . . ? C11 N1 H1A 106.7 . . ? Ni1 N1 H1A 106.7 . . ? C14 N2 C15 111.7(4) . . ? C14 N2 Ni1 118.6(3) . . ? C15 N2 Ni1 107.9(3) . . ? C14 N2 H2 105.9 . . ? C15 N2 H2 105.9 . . ? Ni1 N2 H2 105.9 . . ? C17 N3 C18 113.2(3) . . ? C17 N3 Ni1 108.6(3) . . ? C18 N3 Ni1 115.5(3) . . ? C17 N3 H3A 106.3 . . ? C18 N3 H3A 106.3 . . ? Ni1 N3 H3A 106.3 . . ? C2 C1 C2 118.9(6) 7_575 . ? C2 C1 S1 120.5(3) 7_575 . ? C2 C1 S1 120.5(3) . . ? C3 C2 C1 119.9(5) . . ? C3 C2 C11 118.4(4) . . ? C1 C2 C11 121.7(4) . . ? C2 C3 C4 122.8(5) . . ? C2 C3 H3B 118.6 . . ? C4 C3 H3B 118.6 . . ? C3 C4 C3 115.7(6) 7_575 . ? C3 C4 C7 122.1(3) 7_575 . ? C3 C4 C7 122.1(3) . . ? C4 C7 C8 111.2(4) . . ? C4 C7 C8 111.2(4) . 7_575 ? C8 C7 C8 107.5(6) . 7_575 ? C4 C7 C9 108.5(6) . . ? C8 C7 C9 109.2(4) . . ? C8 C7 C9 109.2(4) 7_575 . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C11 N1 112.9(4) . . ? C2 C11 H11A 109.0 . . ? N1 C11 H11A 109.0 . . ? C2 C11 H11B 109.0 . . ? N1 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N1 C12 C13 113.5(4) . . ? N1 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N1 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C12 116.1(4) . . ? C14 C13 H13A 108.3 . . ? C12 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? C12 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? N2 C14 C13 112.9(4) . . ? N2 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? N2 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N2 C15 C16 113.6(4) . . ? N2 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N2 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 116.5(4) . . ? C17 C16 H16A 108.2 . . ? C15 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? C15 C16 H16B 108.2 . . ? H16A C16 H16B 107.3 . . ? N3 C17 C16 112.4(4) . . ? N3 C17 H17A 109.1 . . ? C16 C17 H17A 109.1 . . ? N3 C17 H17B 109.1 . . ? C16 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? N3 C18 C19 114.0(4) . . ? N3 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? N3 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C24 C19 C20 118.9(4) . . ? C24 C19 C18 118.9(4) . . ? C20 C19 C18 122.1(4) . . ? C19 C20 C19 119.2(6) 7_575 . ? C19 C20 S2 120.4(3) 7_575 . ? C19 C20 S2 120.4(3) . . ? C24 C23 C24 117.2(6) 7_575 . ? C24 C23 C25 121.4(3) 7_575 . ? C24 C23 C25 121.4(3) . . ? C23 C24 C19 122.6(5) . . ? C23 C24 H24 118.7 . . ? C19 C24 H24 118.7 . . ? C27 C25 C26 107.9(5) . 7_575 ? C27 C25 C26 107.9(5) . . ? C26 C25 C26 107.7(7) 7_575 . ? C27 C25 C23 108.1(6) . . ? C26 C25 C23 112.5(4) 7_575 . ? C26 C25 C23 112.5(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C53 B C35 111.8(4) . . ? C53 B C47 110.1(4) . . ? C35 B C47 109.2(4) . . ? C53 B C41 106.7(4) . . ? C35 B C41 110.6(4) . . ? C47 B C41 108.3(4) . . ? C36 C35 C40 114.3(5) . . ? C36 C35 B 121.1(5) . . ? C40 C35 B 124.5(5) . . ? C37 C36 C35 123.6(6) . . ? C37 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C38 C37 C36 120.1(7) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0(6) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 119.2(6) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? C35 C40 C39 122.7(6) . . ? C35 C40 H41 118.6 . . ? C39 C40 H41 118.6 . . ? C42 C41 C46 115.2(5) . . ? C42 C41 B 124.6(5) . . ? C46 C41 B 119.8(4) . . ? C41 C42 C43 123.6(5) . . ? C41 C42 H42 118.2 . . ? C43 C42 H42 118.2 . . ? C44 C43 C42 119.0(5) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C45 C44 C43 119.4(5) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 120.7(6) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C41 122.2(5) . . ? C45 C46 H46 118.9 . . ? C41 C46 H46 118.9 . . ? C48 C47 C52 114.5(5) . . ? C48 C47 B 123.0(5) . . ? C52 C47 B 122.1(4) . . ? C49 C48 C47 123.1(5) . . ? C49 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C50 C49 C48 120.6(5) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 118.9(5) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C50 C51 C52 120.0(5) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C51 C52 C47 123.0(5) . . ? C51 C52 H52 118.5 . . ? C47 C52 H52 118.5 . . ? C54 C53 C58 114.6(5) . . ? C54 C53 B 123.8(5) . . ? C58 C53 B 121.6(5) . . ? C55 C54 C53 122.9(6) . . ? C55 C54 H54 118.5 . . ? C53 C54 H54 118.5 . . ? C56 C55 C54 119.8(7) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C57 C56 C55 120.4(7) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C56 C57 C58 119.2(7) . . ? C56 C57 H57 120.4 . . ? C58 C57 H57 120.4 . . ? C57 C58 C53 123.0(7) . . ? C57 C58 H58 118.5 . . ? C53 C58 H58 118.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.682 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.066 #===END