Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _audit_creation_method 'manual editing of form.cif' # SUBMISSION DETAILS _publ_contact_author_name 'Dr Berthold Kersting' _publ_contact_author_address ; Institut fuer Anorganische und Analytische Chemie Universitat Freiburg, Albertstr. 21 79104 Freiburg Germany ; _publ_contact_author_email 'kerstber@sun2.ruf.uni-freiburg.de' _publ_contact_author_phone '+49/(0)761/203 6129' _publ_contact_author_fax '+49/(0)761/203 5987' _publ_contact_letter ; Please consider this CIF submission for publication in Chem. Commun. Manuscript No. B103050G ; _publ_requested_journal 'Chem. Commun.' # TITLE AND AUTHORLIST _publ_section_title ; The effect of N-methylation on the chemical reactivity Of binuclear Ni amine-thiophenolate complexes ; loop_ _publ_author_name 'B. Kersting' 'Steinfeld, Gunther' ###################################################################### data_4 _database_code_CSD 162721 #CHEMICAL DATA _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_formula_sum 'C33 H56 Cl2 N6 Ni2 O5 S2' _chemical_formula_weight 869.28 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from methanol ; #CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Iba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, z+1/2' _cell_length_a 23.941(5) _cell_length_b 26.974(5) _cell_length_c 12.477(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8057.5(26) _cell_formula_units_Z 8 _cell_measurement_temperature 293(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 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 #EXPERIMENTAL DATA _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'Bruker SMART CCD' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method 'hemisphere' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25074 _diffrn_reflns_av_R_equivalents 0.1201 _diffrn_reflns_av_sigmaI/netI 0.1582 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 28.29 #REFINEMENT DATA _reflns_number_total 8935 _reflns_number_observed 4578 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 8935 _refine_ls_number_parameters 435 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1481 _refine_ls_R_factor_obs 0.0587 _refine_ls_wR_factor_all 0.1764 _refine_ls_wR_factor_obs 0.1289 _refine_ls_goodness_of_fit_all 0.954 _refine_ls_goodness_of_fit_obs 0.990 _refine_ls_restrained_S_all 0.954 _refine_ls_restrained_S_obs 0.990 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.858 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.164 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.13773(4) 0.17185(4) -0.03788(8) 0.0276(2) Uani 1 d . . Ni2 Ni 0.24121(4) 0.23872(4) -0.00172(8) 0.0272(2) Uani 1 d . . S1 S 0.23516(9) 0.15574(8) -0.0753(2) 0.0306(5) Uani 1 d . . S2 S 0.17336(8) 0.20887(8) 0.1249(2) 0.0269(4) Uani 1 d . . Cl1 Cl 0.16303(9) 0.25375(8) -0.1429(2) 0.0339(5) Uani 1 d . . N1 N 0.1220(3) 0.1023(2) 0.0272(5) 0.031(2) Uani 1 d . . H1 H 0.1171(3) 0.1053(2) 0.0993(5) 0.038 Uiso 1 calc R . N2 N 0.0931(3) 0.1427(3) -0.1686(6) 0.038(2) Uani 1 d . . H2 H 0.1159(3) 0.1415(3) -0.2269(6) 0.045 Uiso 1 calc R . N3 N 0.0623(2) 0.2082(2) -0.0095(5) 0.0288(15) Uani 1 d . . H3 H 0.0693(2) 0.2404(2) -0.0270(5) 0.035 Uiso 1 calc R . N4 N 0.2232(3) 0.3107(3) 0.0521(5) 0.030(2) Uani 1 d . . H4 H 0.1903(3) 0.3185(3) 0.0196(5) 0.036 Uiso 1 calc R . N5 N 0.2988(3) 0.2785(3) -0.1010(5) 0.034(2) Uani 1 d . . H5 H 0.2967(3) 0.2660(3) -0.1687(5) 0.041 Uiso 1 calc R . N6 N 0.3151(3) 0.2219(3) 0.0867(5) 0.032(2) Uani 1 d . . H6 H 0.3070(3) 0.2240(3) 0.1578(5) 0.039 Uiso 1 calc R . C1 C 0.2534(3) 0.1199(3) 0.0384(7) 0.031(2) Uani 1 d . . C2 C 0.2193(3) 0.0798(3) 0.0703(7) 0.033(2) Uani 1 d . . C3 C 0.2349(4) 0.0508(3) 0.1558(7) 0.038(2) Uani 1 d . . H3A H 0.2119(4) 0.0245(3) 0.1753(7) 0.046 Uiso 1 calc R . C4 C 0.2833(4) 0.0590(4) 0.2143(7) 0.040(2) Uani 1 d . . C5 C 0.3162(4) 0.0996(3) 0.1841(7) 0.041(2) Uani 1 d . . H5A H 0.3487(4) 0.1065(3) 0.2221(7) 0.049 Uiso 1 calc R . C6 C 0.3012(3) 0.1300(3) 0.0976(7) 0.033(2) Uani 1 d . . C7 C 0.1673(3) 0.0664(3) 0.0063(8) 0.037(2) Uani 1 d . . H7A H 0.1761(3) 0.0663(3) -0.0696(8) 0.045 Uiso 1 calc R . H7B H 0.1549(3) 0.0334(3) 0.0260(8) 0.045 Uiso 1 calc R . C8 C 0.0698(3) 0.0840(3) -0.0219(7) 0.038(2) Uani 1 d . . H8A H 0.0380(3) 0.1020(3) 0.0067(7) 0.046 Uiso 1 calc R . H8B H 0.0648(3) 0.0491(3) -0.0061(7) 0.046 Uiso 1 calc R . C9 C 0.0737(4) 0.0919(3) -0.1428(8) 0.042(2) Uani 1 d . . H9A H 0.0995(4) 0.0679(3) -0.1731(8) 0.050 Uiso 1 calc R . H9B H 0.0373(4) 0.0864(3) -0.1749(8) 0.050 Uiso 1 calc R . C10 C 0.0471(4) 0.1771(4) -0.1899(7) 0.039(2) Uani 1 d . . H10A H 0.0201(4) 0.1613(4) -0.2368(7) 0.046 Uiso 1 calc R . H10B H 0.0614(4) 0.2063(4) -0.2261(7) 0.046 Uiso 1 calc R . C11 C 0.0187(3) 0.1924(3) -0.0866(7) 0.038(2) Uani 1 d . . H11A H -0.0070(3) 0.2195(3) -0.1000(7) 0.046 Uiso 1 calc R . H11B H -0.0023(3) 0.1647(3) -0.0574(7) 0.046 Uiso 1 calc R . C12 C 0.0433(3) 0.2104(3) 0.1050(6) 0.031(2) Uani 1 d . . H12A H 0.0031(3) 0.2141(3) 0.1078(6) 0.037 Uiso 1 calc R . H12B H 0.0532(3) 0.1799(3) 0.1415(6) 0.037 Uiso 1 calc R . C13 C 0.0708(4) 0.2535(3) 0.1595(7) 0.035(2) Uani 1 d . . C14 C 0.1295(3) 0.2594(3) 0.1592(6) 0.029(2) Uani 1 d . . C15 C 0.1510(4) 0.3044(3) 0.1916(7) 0.035(2) Uani 1 d . . C16 C 0.1163(4) 0.3399(3) 0.2405(7) 0.037(2) Uani 1 d . . H16 H 0.1323(4) 0.3692(3) 0.2653(7) 0.045 Uiso 1 calc R . C17 C 0.0595(4) 0.3330(4) 0.2530(8) 0.041(2) Uani 1 d . . C18 C 0.0374(4) 0.2899(3) 0.2066(7) 0.035(2) Uani 1 d . . H18 H -0.0011(4) 0.2853(3) 0.2073(7) 0.042 Uiso 1 calc R . C19 C 0.2118(3) 0.3174(3) 0.1687(6) 0.032(2) Uani 1 d . . H19A H 0.2191(3) 0.3514(3) 0.1893(6) 0.038 Uiso 1 calc R . H19B H 0.2362(3) 0.2960(3) 0.2103(6) 0.038 Uiso 1 calc R . C20 C 0.2633(4) 0.3469(3) 0.0092(8) 0.039(2) Uani 1 d . . H20A H 0.2962(4) 0.3484(3) 0.0546(8) 0.047 Uiso 1 calc R . H20B H 0.2466(4) 0.3796(3) 0.0065(8) 0.047 Uiso 1 calc R . C21 C 0.2794(4) 0.3299(3) -0.1033(7) 0.036(2) Uani 1 d . . H21A H 0.2473(4) 0.3327(3) -0.1505(7) 0.043 Uiso 1 calc R . H21B H 0.3088(4) 0.3511(3) -0.1311(7) 0.043 Uiso 1 calc R . C22 C 0.3556(3) 0.2705(4) -0.0605(7) 0.037(2) Uani 1 d . . H22A H 0.3781(3) 0.2996(4) -0.0754(7) 0.044 Uiso 1 calc R . H22B H 0.3722(3) 0.2425(4) -0.0977(7) 0.044 Uiso 1 calc R . C23 C 0.3559(4) 0.2603(3) 0.0609(8) 0.038(2) Uani 1 d . . H23A H 0.3929(4) 0.2496(3) 0.0830(8) 0.046 Uiso 1 calc R . H23B H 0.3469(4) 0.2905(3) 0.0994(8) 0.046 Uiso 1 calc R . C24 C 0.3385(3) 0.1723(3) 0.0656(7) 0.034(2) Uani 1 d . . H24A H 0.3736(3) 0.1692(3) 0.1038(7) 0.040 Uiso 1 calc R . H24B H 0.3465(3) 0.1695(3) -0.0104(7) 0.040 Uiso 1 calc R . C25 C 0.2988(4) 0.0242(4) 0.3053(8) 0.048(3) Uani 1 d . . C26 C 0.2505(4) 0.0197(4) 0.3843(9) 0.066(3) Uiso 1 d . . H26A H 0.2174(4) 0.0096(4) 0.3467(9) 0.100 Uiso 1 calc R . H26B H 0.2441(4) 0.0512(4) 0.4179(9) 0.100 Uiso 1 calc R . H26C H 0.2596(4) -0.0045(4) 0.4379(9) 0.100 Uiso 1 calc R . C27 C 0.3095(6) -0.0287(6) 0.2577(13) 0.107(5) Uiso 1 d . . H27A H 0.3365(6) -0.0265(6) 0.2012(13) 0.161 Uiso 1 calc R . H27B H 0.2752(6) -0.0418(6) 0.2298(13) 0.161 Uiso 1 calc R . H27C H 0.3233(6) -0.0501(6) 0.3131(13) 0.161 Uiso 1 calc R . C28 C 0.3496(5) 0.0392(5) 0.3675(12) 0.092(5) Uiso 1 d . . H28A H 0.3592(5) 0.0133(5) 0.4171(12) 0.137 Uiso 1 calc R . H28B H 0.3420(5) 0.0692(5) 0.4062(12) 0.137 Uiso 1 calc R . H28C H 0.3801(5) 0.0446(5) 0.3191(12) 0.137 Uiso 1 calc R . C29 C 0.0224(4) 0.3714(4) 0.3073(8) 0.054(3) Uani 1 d . . C30A C 0.0537(7) 0.4108(8) 0.3676(18) 0.053(5) Uiso 0.63(3) d P 1 H30A H 0.0893(7) 0.3981(8) 0.3897(18) 0.079 Uiso 0.63(3) calc PR 1 H30B H 0.0326(7) 0.4204(8) 0.4296(18) 0.079 Uiso 0.63(3) calc PR 1 H30C H 0.0591(7) 0.4391(8) 0.3221(18) 0.079 Uiso 0.63(3) calc PR 1 C31A C -0.0137(10) 0.3954(9) 0.2226(17) 0.076(8) Uiso 0.63(3) d P 1 H31A H -0.0301(10) 0.3702(9) 0.1782(17) 0.114 Uiso 0.63(3) calc PR 1 H31B H 0.0088(10) 0.4170(9) 0.1793(17) 0.114 Uiso 0.63(3) calc PR 1 H31C H -0.0428(10) 0.4142(9) 0.2565(17) 0.114 Uiso 0.63(3) calc PR 1 C32A C -0.0151(11) 0.3447(8) 0.3929(24) 0.090(8) Uiso 0.63(3) d P 1 H32A H 0.0082(11) 0.3261(8) 0.4411(24) 0.135 Uiso 0.63(3) calc PR 1 H32B H -0.0405(11) 0.3225(8) 0.3573(24) 0.135 Uiso 0.63(3) calc PR 1 H32C H -0.0359(11) 0.3689(8) 0.4325(24) 0.135 Uiso 0.63(3) calc PR 1 C30B C 0.0526(12) 0.3923(14) 0.4050(29) 0.053(9) Uiso 0.37(3) d P 2 H30D H 0.0610(12) 0.3659(14) 0.4540(29) 0.080 Uiso 0.37(3) calc PR 2 H30E H 0.0292(12) 0.4163(14) 0.4399(29) 0.080 Uiso 0.37(3) calc PR 2 H30F H 0.0867(12) 0.4079(14) 0.3827(29) 0.080 Uiso 0.37(3) calc PR 2 C31B C 0.0177(19) 0.4141(15) 0.2240(30) 0.086(14) Uiso 0.37(3) d P 2 H31D H -0.0093(19) 0.4054(15) 0.1703(30) 0.128 Uiso 0.37(3) calc PR 2 H31E H 0.0533(19) 0.4193(15) 0.1907(30) 0.128 Uiso 0.37(3) calc PR 2 H31F H 0.0061(19) 0.4439(15) 0.2595(30) 0.128 Uiso 0.37(3) calc PR 2 C32B C -0.0345(13) 0.3488(11) 0.3368(29) 0.052(10) Uiso 0.37(3) d P 2 H32D H -0.0289(13) 0.3193(11) 0.3785(29) 0.078 Uiso 0.37(3) calc PR 2 H32E H -0.0546(13) 0.3406(11) 0.2725(29) 0.078 Uiso 0.37(3) calc PR 2 H32F H -0.0557(13) 0.3723(11) 0.3779(29) 0.078 Uiso 0.37(3) calc PR 2 Cl2 Cl 0.10275(9) 0.08291(9) 0.5570(2) 0.0410(5) Uani 1 d . . O1 O 0.1435(3) 0.0713(3) 0.6359(6) 0.067(2) Uani 1 d . . O2 O 0.0598(3) 0.0470(3) 0.5561(7) 0.069(2) Uani 1 d . . O3 O 0.1298(3) 0.0850(3) 0.4537(6) 0.083(3) Uani 1 d . . O4 O 0.0805(3) 0.1303(3) 0.5792(7) 0.077(2) Uani 1 d . . C33 C 0.0642(5) 0.0419(4) 0.2476(8) 0.053(3) Uani 1 d . . H33A H 0.0976(5) 0.0252(4) 0.2254(8) 0.080 Uiso 1 calc R . H33B H 0.0352(5) 0.0363(4) 0.1958(8) 0.080 Uiso 1 calc R . H33C H 0.0526(5) 0.0294(4) 0.3161(8) 0.080 Uiso 1 calc R . O5 O 0.0749(3) 0.0938(3) 0.2559(6) 0.054(2) Uani 1 d . . H5B H 0.1033(28) 0.1006(8) 0.2223(80) 0.081 Uiso 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 0.0276(5) 0.0324(6) 0.0230(5) -0.0020(5) -0.0012(5) -0.0027(5) Ni2 0.0274(5) 0.0319(6) 0.0224(5) 0.0004(5) 0.0010(5) -0.0032(5) S1 0.0335(11) 0.0330(12) 0.0253(10) -0.0010(9) 0.0049(9) -0.0013(10) S2 0.0287(10) 0.0316(12) 0.0204(10) -0.0002(9) 0.0002(9) -0.0012(9) Cl1 0.0337(11) 0.0410(13) 0.0270(10) 0.0048(9) -0.0037(9) -0.0044(10) N1 0.031(4) 0.034(4) 0.028(4) 0.004(3) 0.000(3) -0.004(3) N2 0.039(4) 0.049(5) 0.025(4) -0.004(3) -0.004(3) 0.003(4) N3 0.033(3) 0.029(4) 0.024(4) 0.002(3) -0.004(3) 0.000(3) N4 0.034(4) 0.034(4) 0.024(3) 0.004(3) 0.012(3) -0.009(3) N5 0.031(4) 0.049(5) 0.022(4) -0.004(3) -0.005(3) -0.001(4) N6 0.028(4) 0.044(5) 0.025(4) -0.002(3) 0.003(3) -0.004(3) C1 0.026(4) 0.030(5) 0.036(5) -0.004(4) 0.012(4) 0.003(4) C2 0.031(5) 0.031(5) 0.036(5) -0.003(4) 0.004(4) 0.001(4) C3 0.040(5) 0.026(5) 0.047(6) 0.008(4) 0.007(4) -0.001(4) C4 0.035(5) 0.040(6) 0.044(6) 0.009(5) 0.002(4) -0.001(4) C5 0.041(5) 0.041(6) 0.041(6) 0.008(4) 0.006(4) 0.008(5) C6 0.033(5) 0.041(5) 0.026(5) 0.000(4) 0.004(4) 0.003(4) C7 0.042(5) 0.023(4) 0.046(5) -0.007(4) 0.002(5) -0.002(4) C8 0.037(5) 0.032(5) 0.045(6) 0.002(4) 0.001(4) -0.001(4) C9 0.042(5) 0.039(6) 0.045(6) -0.007(5) -0.009(5) -0.014(4) C10 0.037(5) 0.055(6) 0.024(5) 0.002(4) -0.014(4) -0.005(5) C11 0.030(5) 0.049(6) 0.036(5) -0.003(4) -0.014(4) 0.005(4) C12 0.025(4) 0.039(5) 0.029(5) -0.011(4) -0.001(4) -0.004(4) C13 0.035(5) 0.039(5) 0.032(5) 0.000(4) -0.001(4) -0.003(4) C14 0.034(5) 0.031(5) 0.021(4) 0.004(3) 0.000(4) -0.002(4) C15 0.039(5) 0.040(5) 0.024(5) -0.001(4) 0.005(4) -0.003(4) C16 0.045(6) 0.032(5) 0.034(5) -0.003(4) 0.014(4) -0.006(4) C17 0.032(5) 0.038(6) 0.052(6) 0.003(4) 0.010(4) 0.002(4) C18 0.028(5) 0.044(6) 0.034(5) -0.008(4) 0.005(4) 0.003(4) C19 0.029(4) 0.044(5) 0.024(4) -0.002(4) -0.003(4) -0.009(4) C20 0.040(5) 0.026(4) 0.051(6) 0.005(5) 0.014(5) -0.005(4) C21 0.042(5) 0.030(5) 0.037(5) 0.006(4) 0.009(4) 0.003(4) C22 0.032(5) 0.048(6) 0.030(6) 0.003(4) 0.007(4) -0.001(4) C23 0.029(5) 0.046(6) 0.040(6) -0.002(4) -0.003(4) -0.009(4) C24 0.028(4) 0.037(5) 0.036(5) 0.008(4) 0.001(4) 0.004(4) C25 0.055(6) 0.041(6) 0.047(6) 0.014(5) 0.003(5) 0.008(5) C29 0.053(6) 0.059(7) 0.049(6) -0.007(5) 0.012(5) -0.002(6) Cl2 0.0451(13) 0.0415(14) 0.0364(12) -0.0004(11) 0.0016(11) -0.0096(11) O1 0.052(4) 0.101(6) 0.049(4) 0.011(4) -0.014(4) 0.013(4) O2 0.058(4) 0.057(5) 0.093(6) -0.002(4) 0.002(4) -0.029(4) O3 0.063(5) 0.149(8) 0.037(4) -0.013(5) 0.014(4) -0.033(5) O4 0.116(7) 0.041(4) 0.075(6) -0.008(4) -0.016(5) 0.021(5) C33 0.056(7) 0.051(7) 0.052(7) -0.004(5) 0.002(5) -0.008(5) O5 0.066(5) 0.052(5) 0.045(4) 0.002(3) 0.003(4) -0.008(4) _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. ; #BOND LENGTHS AND ANGLES 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 2.078(6) . ? Ni1 N3 2.085(6) . ? Ni1 N2 2.103(7) . ? Ni1 S1 2.418(2) . ? Ni1 S2 2.419(2) . ? Ni1 Cl1 2.639(2) . ? Ni2 N4 2.099(7) . ? Ni2 N6 2.134(7) . ? Ni2 N5 2.141(7) . ? Ni2 S2 2.405(2) . ? Ni2 S1 2.423(2) . ? Ni2 Cl1 2.602(2) . ? S1 C1 1.771(9) . ? S2 C14 1.773(8) . ? N1 C7 1.477(10) . ? N1 C8 1.478(10) . ? N2 C10 1.466(11) . ? N2 C9 1.483(11) . ? N3 C11 1.483(10) . ? N3 C12 1.500(10) . ? N4 C20 1.471(10) . ? N4 C19 1.491(10) . ? N5 C21 1.463(11) . ? N5 C22 1.467(10) . ? N6 C23 1.462(10) . ? N6 C24 1.474(10) . ? C1 C6 1.388(11) . ? C1 C2 1.415(11) . ? C2 C3 1.373(12) . ? C2 C7 1.522(11) . ? C3 C4 1.387(12) . ? C4 C5 1.401(12) . ? C4 C25 1.520(13) . ? C5 C6 1.403(12) . ? C6 C24 1.502(11) . ? C8 C9 1.526(12) . ? C10 C11 1.514(12) . ? C12 C13 1.498(11) . ? C13 C18 1.395(12) . ? C13 C14 1.414(12) . ? C14 C15 1.381(11) . ? C15 C16 1.406(12) . ? C15 C19 1.523(11) . ? C16 C17 1.383(12) . ? C17 C18 1.403(12) . ? C17 C29 1.522(13) . ? C20 C21 1.526(12) . ? C22 C23 1.539(11) . ? C25 C28 1.50(2) . ? C25 C26 1.524(14) . ? C25 C27 1.57(2) . ? C29 C30A 1.50(2) . ? C29 C31A 1.51(2) . ? C29 C30B 1.53(3) . ? C29 C32B 1.54(3) . ? C29 C31B 1.56(4) . ? C29 C32A 1.57(2) . ? Cl2 O2 1.413(7) . ? Cl2 O4 1.414(7) . ? Cl2 O1 1.422(7) . ? Cl2 O3 1.444(7) . ? C33 O5 1.425(12) . ? 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 N3 101.6(3) . . ? N1 Ni1 N2 82.7(3) . . ? N3 Ni1 N2 82.4(3) . . ? N1 Ni1 S1 95.0(2) . . ? N3 Ni1 S1 162.3(2) . . ? N2 Ni1 S1 105.8(2) . . ? N1 Ni1 S2 96.2(2) . . ? N3 Ni1 S2 88.2(2) . . ? N2 Ni1 S2 170.1(2) . . ? S1 Ni1 S2 84.03(8) . . ? N1 Ni1 Cl1 172.4(2) . . ? N3 Ni1 Cl1 83.6(2) . . ? N2 Ni1 Cl1 92.6(2) . . ? S1 Ni1 Cl1 80.39(7) . . ? S2 Ni1 Cl1 89.45(7) . . ? N4 Ni2 N6 101.7(3) . . ? N4 Ni2 N5 81.6(3) . . ? N6 Ni2 N5 82.7(3) . . ? N4 Ni2 S2 87.7(2) . . ? N6 Ni2 S2 98.6(2) . . ? N5 Ni2 S2 169.3(2) . . ? N4 Ni2 S1 164.4(2) . . ? N6 Ni2 S1 92.8(2) . . ? N5 Ni2 S1 106.4(2) . . ? S2 Ni2 S1 84.22(8) . . ? N4 Ni2 Cl1 85.7(2) . . ? N6 Ni2 Cl1 168.4(2) . . ? N5 Ni2 Cl1 89.6(2) . . ? S2 Ni2 Cl1 90.64(7) . . ? S1 Ni2 Cl1 81.05(8) . . ? C1 S1 Ni1 100.5(3) . . ? C1 S1 Ni2 100.7(3) . . ? Ni1 S1 Ni2 79.55(7) . . ? C14 S2 Ni2 107.6(3) . . ? C14 S2 Ni1 108.1(3) . . ? Ni2 S2 Ni1 79.90(7) . . ? Ni2 Cl1 Ni1 72.46(6) . . ? C7 N1 C8 109.1(6) . . ? C7 N1 Ni1 113.0(5) . . ? C8 N1 Ni1 107.0(5) . . ? C10 N2 C9 112.9(7) . . ? C10 N2 Ni1 106.6(5) . . ? C9 N2 Ni1 109.7(5) . . ? C11 N3 C12 114.6(6) . . ? C11 N3 Ni1 111.3(5) . . ? C12 N3 Ni1 116.3(5) . . ? C20 N4 C19 113.2(7) . . ? C20 N4 Ni2 111.2(5) . . ? C19 N4 Ni2 117.5(5) . . ? C21 N5 C22 116.1(7) . . ? C21 N5 Ni2 106.4(5) . . ? C22 N5 Ni2 108.9(5) . . ? C23 N6 C24 110.5(6) . . ? C23 N6 Ni2 106.8(5) . . ? C24 N6 Ni2 114.6(5) . . ? C6 C1 C2 118.5(8) . . ? C6 C1 S1 121.5(6) . . ? C2 C1 S1 120.0(6) . . ? C3 C2 C1 119.7(8) . . ? C3 C2 C7 119.7(8) . . ? C1 C2 C7 120.4(8) . . ? C2 C3 C4 123.1(8) . . ? C3 C4 C5 116.9(8) . . ? C3 C4 C25 120.0(8) . . ? C5 C4 C25 123.1(9) . . ? C4 C5 C6 121.3(9) . . ? C1 C6 C5 120.4(8) . . ? C1 C6 C24 119.8(8) . . ? C5 C6 C24 119.7(8) . . ? N1 C7 C2 110.6(7) . . ? N1 C8 C9 108.2(7) . . ? N2 C9 C8 111.2(7) . . ? N2 C10 C11 110.8(7) . . ? N3 C11 C10 108.4(7) . . ? C13 C12 N3 109.2(7) . . ? C18 C13 C14 119.3(8) . . ? C18 C13 C12 119.1(8) . . ? C14 C13 C12 121.5(8) . . ? C15 C14 C13 118.0(8) . . ? C15 C14 S2 121.7(7) . . ? C13 C14 S2 120.2(6) . . ? C14 C15 C16 120.3(8) . . ? C14 C15 C19 120.3(8) . . ? C16 C15 C19 119.3(8) . . ? C17 C16 C15 122.6(9) . . ? C16 C17 C18 115.8(8) . . ? C16 C17 C29 122.2(9) . . ? C18 C17 C29 121.9(8) . . ? C13 C18 C17 122.9(8) . . ? N4 C19 C15 109.2(7) . . ? N4 C20 C21 107.5(7) . . ? N5 C21 C20 110.2(7) . . ? N5 C22 C23 111.7(7) . . ? N6 C23 C22 109.8(7) . . ? N6 C24 C6 114.5(7) . . ? C28 C25 C4 114.8(9) . . ? C28 C25 C26 107.6(9) . . ? C4 C25 C26 110.2(8) . . ? C28 C25 C27 108.0(10) . . ? C4 C25 C27 108.7(10) . . ? C26 C25 C27 107.3(10) . . ? C30A C29 C31A 109.4(13) . . ? C30A C29 C17 114.4(10) . . ? C31A C29 C17 108.3(11) . . ? C17 C29 C30B 109.3(14) . . ? C17 C29 C32B 110.7(14) . . ? C30B C29 C32B 112.0(18) . . ? C17 C29 C31B 104.4(16) . . ? C30B C29 C31B 107.1(20) . . ? C32B C29 C31B 112.9(20) . . ? C30A C29 C32A 105.6(13) . . ? C31A C29 C32A 110.2(13) . . ? C17 C29 C32A 108.9(11) . . ? O2 Cl2 O4 110.4(5) . . ? O2 Cl2 O1 110.7(5) . . ? O4 Cl2 O1 108.9(5) . . ? O2 Cl2 O3 110.2(5) . . ? O4 Cl2 O3 108.0(5) . . ? O1 Cl2 O3 108.6(4) . . ? #===END data_5 _database_code_CSD 162722 #CHEMICAL DATA _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_formula_sum 'C63 H88 B Cl N6 Ni2 O S2' _chemical_formula_weight 1173.19 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from methanol ; #CRYSTAL DATA _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 14.668(3) _cell_length_b 20.140(4) _cell_length_c 22.960(5) _cell_angle_alpha 87.65(3) _cell_angle_beta 80.96(3) _cell_angle_gamma 69.39(3) _cell_volume 6269.0(22) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 1.00 #EXPERIMENTAL DATA _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'BRUKER SMART CCD' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method 'multirun' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55881 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.1309 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 28.37 #REFINEMENT DATA _reflns_number_total 28884 _reflns_number_observed 12285 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1765P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28884 _refine_ls_number_parameters 1349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1617 _refine_ls_R_factor_obs 0.0674 _refine_ls_wR_factor_all 0.2718 _refine_ls_wR_factor_obs 0.1933 _refine_ls_goodness_of_fit_all 0.825 _refine_ls_goodness_of_fit_obs 0.909 _refine_ls_restrained_S_all 0.825 _refine_ls_restrained_S_obs 0.909 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.629 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.165 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.32272(5) 0.04169(4) 0.13555(3) 0.0391(2) Uani 1 d . . Ni2 Ni 0.14530(6) 0.15452(4) 0.08095(3) 0.0475(2) Uani 1 d . . S1 S 0.31982(11) 0.09144(8) 0.03541(7) 0.0450(4) Uani 1 d . . S2 S 0.23090(10) 0.16447(8) 0.16041(6) 0.0416(3) Uani 1 d . . Cl1 Cl 0.17286(12) 0.03157(9) 0.11070(8) 0.0589(4) Uani 1 d . . N1 N 0.4839(3) 0.0406(2) 0.1344(2) 0.0418(11) Uani 1 d . . N2 N 0.4074(3) -0.0708(3) 0.1225(2) 0.0448(12) Uani 1 d . . N3 N 0.2905(3) 0.0104(2) 0.2263(2) 0.0436(11) Uani 1 d . . N4 N 0.0041(4) 0.1960(3) 0.1378(2) 0.0544(14) Uani 1 d . . N5 N 0.0529(4) 0.1510(4) 0.0166(2) 0.066(2) Uani 1 d . . N6 N 0.1474(4) 0.2553(3) 0.0237(3) 0.062(2) Uani 1 d . . C1 C 0.3730(4) 0.1579(3) 0.0399(2) 0.0409(13) Uani 1 d . . C2 C 0.4603(4) 0.1425(3) 0.0638(3) 0.0451(14) Uani 1 d . . C3 C 0.4996(5) 0.1953(4) 0.0688(3) 0.056(2) Uani 1 d . . H3 H 0.5572(5) 0.1842(4) 0.0853(3) 0.067 Uiso 1 calc R . C4 C 0.4554(6) 0.2643(4) 0.0499(3) 0.062(2) Uani 1 d . . C5 C 0.3710(6) 0.2771(4) 0.0235(3) 0.063(2) Uani 1 d . . H5 H 0.3412(6) 0.3219(4) 0.0087(3) 0.075 Uiso 1 calc R . C6 C 0.3301(5) 0.2252(3) 0.0188(3) 0.052(2) Uani 1 d . . C7 C 0.5182(4) 0.0682(3) 0.0774(3) 0.0445(14) Uani 1 d . . H7A H 0.5860(4) 0.0647(3) 0.0772(3) 0.053 Uiso 1 calc R . H7B H 0.5180(4) 0.0376(3) 0.0460(3) 0.053 Uiso 1 calc R . C8 C 0.5019(5) 0.0795(4) 0.1820(3) 0.053(2) Uani 1 d . . H8A H 0.4965(5) 0.0552(4) 0.2186(3) 0.080 Uiso 1 calc R . H8B H 0.4539(5) 0.1267(4) 0.1857(3) 0.080 Uiso 1 calc R . H8C H 0.5668(5) 0.0819(4) 0.1728(3) 0.080 Uiso 1 calc R . C9 C 0.5491(4) -0.0357(3) 0.1348(3) 0.051(2) Uani 1 d . . H9A H 0.5499(4) -0.0522(3) 0.1750(3) 0.061 Uiso 1 calc R . H9B H 0.6159(4) -0.0407(3) 0.1174(3) 0.061 Uiso 1 calc R . C10 C 0.5113(4) -0.0792(3) 0.1003(3) 0.049(2) Uani 1 d . . H10A H 0.5168(4) -0.0653(3) 0.0593(3) 0.059 Uiso 1 calc R . H10B H 0.5521(4) -0.1288(3) 0.1020(3) 0.059 Uiso 1 calc R . C11 C 0.3731(5) -0.1063(4) 0.0791(3) 0.066(2) Uani 1 d . . H11A H 0.3064(5) -0.1032(4) 0.0931(3) 0.098 Uiso 1 calc R . H11B H 0.4148(5) -0.1553(4) 0.0746(3) 0.098 Uiso 1 calc R . H11C H 0.3759(5) -0.0833(4) 0.0418(3) 0.098 Uiso 1 calc R . C12 C 0.3998(5) -0.1039(3) 0.1815(3) 0.053(2) Uani 1 d . . H12A H 0.3485(5) -0.1243(3) 0.1847(3) 0.063 Uiso 1 calc R . H12B H 0.4615(5) -0.1423(3) 0.1842(3) 0.063 Uiso 1 calc R . C13 C 0.3778(5) -0.0538(3) 0.2324(3) 0.050(2) Uani 1 d . . H13A H 0.3652(5) -0.0773(3) 0.2689(3) 0.061 Uiso 1 calc R . H13B H 0.4344(5) -0.0400(3) 0.2341(3) 0.061 Uiso 1 calc R . C14 C 0.2028(4) -0.0115(3) 0.2418(3) 0.055(2) Uani 1 d . . H14A H 0.2085(4) -0.0494(3) 0.2158(3) 0.083 Uiso 1 calc R . H14B H 0.1442(4) 0.0281(3) 0.2376(3) 0.083 Uiso 1 calc R . H14C H 0.1992(4) -0.0274(3) 0.2818(3) 0.083 Uiso 1 calc R . C15 C 0.2826(4) 0.0663(3) 0.2686(3) 0.0477(15) Uani 1 d . . H15A H 0.3334(4) 0.0863(3) 0.2552(3) 0.057 Uiso 1 calc R . H15B H 0.2942(4) 0.0452(3) 0.3067(3) 0.057 Uiso 1 calc R . C16 C 0.1840(4) 0.1246(3) 0.2755(3) 0.0460(14) Uani 1 d . . C17 C 0.1509(4) 0.1664(3) 0.2271(3) 0.0437(14) Uani 1 d . . C18 C 0.0506(4) 0.2114(3) 0.2340(3) 0.0475(15) Uani 1 d . . C19 C -0.0083(5) 0.2181(4) 0.2889(3) 0.054(2) Uani 1 d . . H19 H -0.0735(5) 0.2485(4) 0.2927(3) 0.065 Uiso 1 calc R . C20 C 0.0258(4) 0.1817(3) 0.3381(3) 0.0492(15) Uani 1 d . . C21 C 0.1217(5) 0.1334(3) 0.3298(3) 0.053(2) Uani 1 d . . H21 H 0.1455(5) 0.1060(3) 0.3614(3) 0.064 Uiso 1 calc R . C22 C 0.0051(5) 0.2478(3) 0.1820(3) 0.053(2) Uani 1 d . . H22A H 0.0418(5) 0.2768(3) 0.1635(3) 0.063 Uiso 1 calc R . H22B H -0.0620(5) 0.2790(3) 0.1954(3) 0.063 Uiso 1 calc R . C23 C -0.0345(5) 0.1435(4) 0.1690(3) 0.064(2) Uani 1 d . . H23A H 0.0102(5) 0.1165(4) 0.1948(3) 0.096 Uiso 1 calc R . H23B H -0.0411(5) 0.1123(4) 0.1408(3) 0.096 Uiso 1 calc R . H23C H -0.0977(5) 0.1678(4) 0.1917(3) 0.096 Uiso 1 calc R . C24 C -0.0640(5) 0.2351(4) 0.0959(3) 0.069(2) Uani 1 d . . H24A H -0.0496(5) 0.2771(4) 0.0824(3) 0.083 Uiso 1 calc R . H24B H -0.1316(5) 0.2501(4) 0.1158(3) 0.083 Uiso 1 calc R . C25 C -0.0517(5) 0.1868(5) 0.0427(3) 0.075(2) Uani 1 d . . H25A H -0.0807(5) 0.1511(5) 0.0552(3) 0.090 Uiso 1 calc R . H25B H -0.0873(5) 0.2150(5) 0.0128(3) 0.090 Uiso 1 calc R . C26 C 0.0686(7) 0.0781(5) -0.0041(4) 0.093(3) Uani 1 d . . H26A H 0.0404(7) 0.0541(5) 0.0266(4) 0.140 Uiso 1 calc R . H26B H 0.1380(7) 0.0522(5) -0.0139(4) 0.140 Uiso 1 calc R . H26C H 0.0376(7) 0.0809(5) -0.0384(4) 0.140 Uiso 1 calc R . C27 C 0.0785(6) 0.1894(5) -0.0362(3) 0.084(3) Uani 1 d . . H27A H 0.0319(6) 0.1950(5) -0.0633(3) 0.100 Uiso 1 calc R . H27B H 0.1438(6) 0.1622(5) -0.0562(3) 0.100 Uiso 1 calc R . C28 C 0.0763(6) 0.2604(5) -0.0189(4) 0.085(3) Uani 1 d . . H28A H 0.0100(6) 0.2882(5) -0.0008(4) 0.102 Uiso 1 calc R . H28B H 0.0930(6) 0.2848(5) -0.0540(4) 0.102 Uiso 1 calc R . C29 C 0.1218(6) 0.3225(4) 0.0562(4) 0.082(2) Uani 1 d . . H29A H 0.0577(6) 0.3336(4) 0.0794(4) 0.124 Uiso 1 calc R . H29B H 0.1215(6) 0.3598(4) 0.0287(4) 0.124 Uiso 1 calc R . H29C H 0.1697(6) 0.3178(4) 0.0817(4) 0.124 Uiso 1 calc R . C30 C 0.2458(5) 0.2405(4) -0.0146(3) 0.058(2) Uani 1 d . . H30A H 0.2580(5) 0.2002(4) -0.0403(3) 0.069 Uiso 1 calc R . H30B H 0.2428(5) 0.2812(4) -0.0394(3) 0.069 Uiso 1 calc R . C31 C 0.5009(7) 0.3212(4) 0.0571(4) 0.084(3) Uani 1 d . . C32 C 0.4972(10) 0.3330(6) 0.1221(5) 0.132(4) Uani 1 d . . H32A H 0.5423(10) 0.3563(6) 0.1273(5) 0.198 Uiso 1 calc R . H32B H 0.5153(10) 0.2881(6) 0.1415(5) 0.198 Uiso 1 calc R . H32C H 0.4315(10) 0.3620(6) 0.1388(5) 0.198 Uiso 1 calc R . C33 C 0.6128(10) 0.2901(7) 0.0275(6) 0.161(6) Uani 1 d . . H33A H 0.6447(10) 0.2453(7) 0.0447(6) 0.242 Uiso 1 calc R . H33B H 0.6451(10) 0.3225(7) 0.0339(6) 0.242 Uiso 1 calc R . H33C H 0.6163(10) 0.2836(7) -0.0141(6) 0.242 Uiso 1 calc R . C34 C 0.4551(10) 0.3877(5) 0.0264(6) 0.149(5) Uani 1 d . . H34A H 0.4606(10) 0.3777(5) -0.0148(6) 0.223 Uiso 1 calc R . H34B H 0.4881(10) 0.4202(5) 0.0310(6) 0.223 Uiso 1 calc R . H34C H 0.3868(10) 0.4085(5) 0.0429(6) 0.223 Uiso 1 calc R . C35 C -0.0420(5) 0.1949(4) 0.3968(3) 0.058(2) Uani 1 d . . C36 C -0.0693(6) 0.2723(4) 0.4156(3) 0.070(2) Uani 1 d . . H36A H -0.0970(6) 0.3029(4) 0.3848(3) 0.105 Uiso 1 calc R . H36B H -0.0112(6) 0.2804(4) 0.4228(3) 0.105 Uiso 1 calc R . H36C H -0.1166(6) 0.2823(4) 0.4510(3) 0.105 Uiso 1 calc R . C37 C -0.1361(5) 0.1803(4) 0.3910(3) 0.073(2) Uani 1 d . . H37A H -0.1677(5) 0.2094(4) 0.3606(3) 0.110 Uiso 1 calc R . H37B H -0.1800(5) 0.1913(4) 0.4278(3) 0.110 Uiso 1 calc R . H37C H -0.1194(5) 0.1312(4) 0.3810(3) 0.110 Uiso 1 calc R . C38 C 0.0072(6) 0.1484(4) 0.4454(3) 0.080(2) Uani 1 d . . H38A H -0.0353(6) 0.1618(4) 0.4826(3) 0.120 Uiso 1 calc R . H38B H 0.0685(6) 0.1547(4) 0.4476(3) 0.120 Uiso 1 calc R . H38C H 0.0194(6) 0.0996(4) 0.4367(3) 0.120 Uiso 1 calc R . Ni3 Ni 0.79602(5) 0.65541(4) 0.47152(3) 0.0424(2) Uani 1 d . . Ni4 Ni 0.70972(6) 0.67043(4) 0.61001(3) 0.0459(2) Uani 1 d . . S3 S 0.84530(12) 0.57282(8) 0.55317(8) 0.0512(4) Uani 1 d . . S4 S 0.63749(11) 0.66480(8) 0.52576(6) 0.0418(3) Uani 1 d . . Cl2 Cl 0.80632(13) 0.73399(9) 0.55076(8) 0.0608(4) Uani 1 d . . N7 N 0.8260(4) 0.5592(3) 0.4078(2) 0.0500(13) Uani 1 d . . N8 N 0.9305(4) 0.6542(3) 0.4154(2) 0.0504(13) Uani 1 d . . N9 N 0.7292(4) 0.7435(3) 0.4163(2) 0.0497(13) Uani 1 d . . N10 N 0.5888(4) 0.7707(3) 0.6414(2) 0.0561(14) Uani 1 d . . N11 N 0.7575(4) 0.6809(3) 0.6929(2) 0.0598(15) Uani 1 d . . N12 N 0.6591(4) 0.5872(3) 0.6687(2) 0.0527(13) Uani 1 d . . C39 C 0.7868(4) 0.5102(3) 0.5448(3) 0.0474(15) Uani 1 d . . C40 C 0.7946(4) 0.4803(3) 0.4891(3) 0.0484(15) Uani 1 d . . C41 C 0.7427(5) 0.4350(3) 0.4827(3) 0.050(2) Uani 1 d . . H41 H 0.7471(5) 0.4168(3) 0.4454(3) 0.060 Uiso 1 calc R . C42 C 0.6855(5) 0.4162(3) 0.5295(3) 0.052(2) Uani 1 d . . C43 C 0.6843(5) 0.4435(3) 0.5853(3) 0.057(2) Uani 1 d . . H43 H 0.6493(5) 0.4303(3) 0.6183(3) 0.069 Uiso 1 calc R . C44 C 0.7338(5) 0.4896(3) 0.5927(3) 0.053(2) Uani 1 d . . C45 C 0.8640(5) 0.4914(3) 0.4392(3) 0.053(2) Uani 1 d . . H45A H 0.8821(5) 0.4525(3) 0.4111(3) 0.063 Uiso 1 calc R . H45B H 0.9235(5) 0.4896(3) 0.4537(3) 0.063 Uiso 1 calc R . C46 C 0.7416(5) 0.5583(4) 0.3795(3) 0.066(2) Uani 1 d . . H46A H 0.7257(5) 0.5964(4) 0.3521(3) 0.099 Uiso 1 calc R . H46B H 0.6855(5) 0.5639(4) 0.4093(3) 0.099 Uiso 1 calc R . H46C H 0.7594(5) 0.5139(4) 0.3590(3) 0.099 Uiso 1 calc R . C47 C 0.9076(5) 0.5595(4) 0.3610(3) 0.063(2) Uani 1 d . . H47A H 0.8814(5) 0.5908(4) 0.3297(3) 0.075 Uiso 1 calc R . H47B H 0.9414(5) 0.5121(4) 0.3444(3) 0.075 Uiso 1 calc R . C48 C 0.9780(5) 0.5839(4) 0.3856(3) 0.065(2) Uani 1 d . . H48A H 1.0094(5) 0.5494(4) 0.4137(3) 0.079 Uiso 1 calc R . H48B H 1.0290(5) 0.5863(4) 0.3540(3) 0.079 Uiso 1 calc R . C49 C 1.0036(5) 0.6670(5) 0.4482(4) 0.076(2) Uani 1 d . . H49A H 0.9744(5) 0.7125(5) 0.4677(4) 0.114 Uiso 1 calc R . H49B H 1.0608(5) 0.6660(5) 0.4209(4) 0.114 Uiso 1 calc R . H49C H 1.0224(5) 0.6307(5) 0.4769(4) 0.114 Uiso 1 calc R . C50 C 0.9019(5) 0.7101(3) 0.3698(3) 0.052(2) Uani 1 d . . H50A H 0.9459(5) 0.6938(3) 0.3330(3) 0.063 Uiso 1 calc R . H50B H 0.9102(5) 0.7528(3) 0.3823(3) 0.063 Uiso 1 calc R . C51 C 0.7975(4) 0.7280(3) 0.3593(3) 0.051(2) Uani 1 d . . H51A H 0.7798(4) 0.7690(3) 0.3341(3) 0.061 Uiso 1 calc R . H51B H 0.7916(4) 0.6885(3) 0.3393(3) 0.061 Uiso 1 calc R . C52 C 0.7178(5) 0.8155(3) 0.4381(3) 0.057(2) Uani 1 d . . H52A H 0.6760(5) 0.8252(3) 0.4756(3) 0.086 Uiso 1 calc R . H52B H 0.6889(5) 0.8506(3) 0.4104(3) 0.086 Uiso 1 calc R . H52C H 0.7813(5) 0.8167(3) 0.4422(3) 0.086 Uiso 1 calc R . C53 C 0.6293(4) 0.7439(3) 0.4065(3) 0.051(2) Uani 1 d . . H53A H 0.6326(4) 0.6955(3) 0.4016(3) 0.061 Uiso 1 calc R . H53B H 0.6125(4) 0.7690(3) 0.3705(3) 0.061 Uiso 1 calc R . C54 C 0.5494(4) 0.7789(3) 0.4574(3) 0.0472(14) Uani 1 d . . C55 C 0.5527(4) 0.7518(3) 0.5144(3) 0.0454(14) Uani 1 d . . C56 C 0.4850(5) 0.7921(3) 0.5611(3) 0.053(2) Uani 1 d . . C57 C 0.4131(5) 0.8559(4) 0.5497(3) 0.062(2) Uani 1 d . . H57 H 0.3688(5) 0.8821(4) 0.5812(3) 0.074 Uiso 1 calc R . C58 C 0.4048(5) 0.8818(3) 0.4930(3) 0.056(2) Uani 1 d . . C59 C 0.4755(5) 0.8425(3) 0.4478(3) 0.054(2) Uani 1 d . . H59 H 0.4733(5) 0.8594(3) 0.4095(3) 0.065 Uiso 1 calc R . C60 C 0.4947(5) 0.7711(4) 0.6256(3) 0.063(2) Uani 1 d . . H60A H 0.4403(5) 0.8042(4) 0.6514(3) 0.075 Uiso 1 calc R . H60B H 0.4905(5) 0.7242(4) 0.6317(3) 0.075 Uiso 1 calc R . C61 C 0.6038(6) 0.8380(3) 0.6218(3) 0.071(2) Uani 1 d . . H61A H 0.6020(6) 0.8432(3) 0.5802(3) 0.106 Uiso 1 calc R . H61B H 0.6667(6) 0.8368(3) 0.6299(3) 0.106 Uiso 1 calc R . H61C H 0.5525(6) 0.8773(3) 0.6427(3) 0.106 Uiso 1 calc R . C62 C 0.5836(6) 0.7679(4) 0.7059(3) 0.070(2) Uani 1 d . . H62A H 0.5546(6) 0.7331(4) 0.7215(3) 0.084 Uiso 1 calc R . H62B H 0.5420(6) 0.8138(4) 0.7232(3) 0.084 Uiso 1 calc R . C63 C 0.6850(6) 0.7484(4) 0.7219(3) 0.076(2) Uani 1 d . . H63A H 0.7094(6) 0.7867(4) 0.7108(3) 0.091 Uiso 1 calc R . H63B H 0.6808(6) 0.7435(4) 0.7643(3) 0.091 Uiso 1 calc R . C64 C 0.8572(6) 0.6838(5) 0.6847(4) 0.084(2) Uani 1 d . . H64A H 0.9029(6) 0.6412(5) 0.6650(4) 0.125 Uiso 1 calc R . H64B H 0.8752(6) 0.6879(5) 0.7225(4) 0.125 Uiso 1 calc R . H64C H 0.8588(6) 0.7241(5) 0.6614(4) 0.125 Uiso 1 calc R . C65 C 0.7563(7) 0.6201(4) 0.7309(3) 0.076(2) Uani 1 d . . H65A H 0.8150(7) 0.5796(4) 0.7179(3) 0.091 Uiso 1 calc R . H65B H 0.7587(7) 0.6318(4) 0.7711(3) 0.091 Uiso 1 calc R . C66 C 0.6692(7) 0.6002(4) 0.7304(3) 0.078(2) Uani 1 d . . H66A H 0.6106(7) 0.6379(4) 0.7484(3) 0.094 Uiso 1 calc R . H66B H 0.6755(7) 0.5576(4) 0.7532(3) 0.094 Uiso 1 calc R . C67 C 0.5598(6) 0.5852(4) 0.6673(4) 0.079(2) Uani 1 d . . H67A H 0.5511(6) 0.5816(4) 0.6271(4) 0.118 Uiso 1 calc R . H67B H 0.5110(6) 0.6279(4) 0.6851(4) 0.118 Uiso 1 calc R . H67C H 0.5528(6) 0.5449(4) 0.6887(4) 0.118 Uiso 1 calc R . C68 C 0.7321(5) 0.5138(3) 0.6534(3) 0.057(2) Uani 1 d . . H68A H 0.7974(5) 0.5129(3) 0.6573(3) 0.068 Uiso 1 calc R . H68B H 0.7163(5) 0.4807(3) 0.6815(3) 0.068 Uiso 1 calc R . C69 C 0.6290(5) 0.3658(4) 0.5239(3) 0.063(2) Uani 1 d . . C70 C 0.5249(6) 0.3984(6) 0.5558(5) 0.113(4) Uani 1 d . . H70A H 0.5258(6) 0.3997(6) 0.5974(5) 0.169 Uiso 1 calc R . H70B H 0.4868(6) 0.3705(6) 0.5480(5) 0.169 Uiso 1 calc R . H70C H 0.4958(6) 0.4458(6) 0.5422(5) 0.169 Uiso 1 calc R . C71 C 0.6257(7) 0.3523(5) 0.4595(4) 0.092(3) Uani 1 d . . H71A H 0.5963(7) 0.3169(5) 0.4573(4) 0.138 Uiso 1 calc R . H71B H 0.6915(7) 0.3359(5) 0.4381(4) 0.138 Uiso 1 calc R . H71C H 0.5873(7) 0.3955(5) 0.4426(4) 0.138 Uiso 1 calc R . C72 C 0.6808(8) 0.2953(4) 0.5514(4) 0.105(3) Uani 1 d . . H72A H 0.7437(8) 0.2720(4) 0.5279(4) 0.157 Uiso 1 calc R . H72B H 0.6413(8) 0.2659(4) 0.5532(4) 0.157 Uiso 1 calc R . H72C H 0.6903(8) 0.3035(4) 0.5906(4) 0.157 Uiso 1 calc R . C73 C 0.3238(5) 0.9496(4) 0.4811(4) 0.067(2) Uani 1 d . . C74A C 0.2254(13) 0.9424(9) 0.4981(9) 0.088(6) Uiso 0.52(2) d P 1 H74A H 0.2112(13) 0.9403(9) 0.5403(9) 0.132 Uiso 0.52(2) calc PR 1 H74B H 0.2257(13) 0.8998(9) 0.4807(9) 0.132 Uiso 0.52(2) calc PR 1 H74C H 0.1758(13) 0.9826(9) 0.4843(9) 0.132 Uiso 0.52(2) calc PR 1 C75A C 0.3342(15) 0.9721(11) 0.4192(9) 0.102(7) Uiso 0.52(2) d P 1 H75A H 0.2834(15) 1.0169(11) 0.4150(9) 0.153 Uiso 0.52(2) calc PR 1 H75B H 0.3285(15) 0.9373(11) 0.3941(9) 0.153 Uiso 0.52(2) calc PR 1 H75C H 0.3976(15) 0.9768(11) 0.4082(9) 0.153 Uiso 0.52(2) calc PR 1 C76A C 0.3272(16) 1.0112(11) 0.5182(9) 0.106(7) Uiso 0.52(2) d P 1 H76A H 0.3922(16) 1.0136(11) 0.5107(9) 0.159 Uiso 0.52(2) calc PR 1 H76B H 0.3109(16) 1.0030(11) 0.5593(9) 0.159 Uiso 0.52(2) calc PR 1 H76C H 0.2805(16) 1.0552(11) 0.5074(9) 0.159 Uiso 0.52(2) calc PR 1 C74B C 0.2596(18) 0.9320(13) 0.4449(12) 0.125(9) Uiso 0.48(2) d P 2 H74D H 0.1984(18) 0.9711(13) 0.4463(12) 0.188 Uiso 0.48(2) calc PR 2 H74E H 0.2469(18) 0.8905(13) 0.4602(12) 0.188 Uiso 0.48(2) calc PR 2 H74F H 0.2919(18) 0.9230(13) 0.4048(12) 0.188 Uiso 0.48(2) calc PR 2 C75B C 0.3660(15) 1.0008(11) 0.4456(9) 0.091(7) Uiso 0.48(2) d P 2 H75D H 0.4058(15) 1.0149(11) 0.4684(9) 0.137 Uiso 0.48(2) calc PR 2 H75E H 0.3130(15) 1.0419(11) 0.4362(9) 0.137 Uiso 0.48(2) calc PR 2 H75F H 0.4057(15) 0.9777(11) 0.4097(9) 0.137 Uiso 0.48(2) calc PR 2 C76B C 0.2648(19) 0.9911(13) 0.5346(11) 0.117(9) Uiso 0.48(2) d P 2 H76D H 0.3081(19) 0.9959(13) 0.5601(11) 0.176 Uiso 0.48(2) calc PR 2 H76E H 0.2234(19) 0.9671(13) 0.5550(11) 0.176 Uiso 0.48(2) calc PR 2 H76F H 0.2245(19) 1.0373(13) 0.5234(11) 0.176 Uiso 0.48(2) calc PR 2 B1 B 0.8663(6) -0.0702(4) 0.2346(3) 0.051(2) Uani 1 d . . C101 C 0.7741(5) -0.1014(3) 0.2449(3) 0.055(2) Uani 1 d . . C102 C 0.7673(6) -0.1537(4) 0.2095(3) 0.065(2) Uani 1 d . . H102 H 0.8178(6) -0.1732(4) 0.1784(3) 0.078 Uiso 1 calc R . C103 C 0.6882(7) -0.1782(5) 0.2186(5) 0.083(3) Uani 1 d . . H103 H 0.6861(7) -0.2134(5) 0.1944(5) 0.100 Uiso 1 calc R . C104 C 0.6148(7) -0.1492(6) 0.2637(5) 0.090(3) Uani 1 d . . H104 H 0.5629(7) -0.1662(6) 0.2716(5) 0.108 Uiso 1 calc R . C105 C 0.6153(6) -0.0947(5) 0.2981(4) 0.080(2) Uani 1 d . . H105 H 0.5627(6) -0.0738(5) 0.3277(4) 0.096 Uiso 1 calc R . C106 C 0.6939(5) -0.0718(4) 0.2883(3) 0.067(2) Uani 1 d . . H106 H 0.6934(5) -0.0350(4) 0.3116(3) 0.081 Uiso 1 calc R . C201 C 0.9637(5) -0.1204(3) 0.1913(3) 0.051(2) Uani 1 d . . C202 C 0.9983(5) -0.1947(4) 0.1947(3) 0.066(2) Uani 1 d . . H202 H 0.9616(5) -0.2159(4) 0.2205(3) 0.079 Uiso 1 calc R . C203 C 1.0840(6) -0.2376(4) 0.1613(4) 0.081(2) Uani 1 d . . H203 H 1.1030(6) -0.2867(4) 0.1644(4) 0.097 Uiso 1 calc R . C204 C 1.1409(6) -0.2087(6) 0.1242(4) 0.086(3) Uani 1 d . . H204 H 1.1990(6) -0.2379(6) 0.1021(4) 0.103 Uiso 1 calc R . C205 C 1.1131(6) -0.1375(5) 0.1192(4) 0.076(2) Uani 1 d . . H205 H 1.1518(6) -0.1173(5) 0.0940(4) 0.091 Uiso 1 calc R . C206 C 1.0253(5) -0.0948(4) 0.1527(3) 0.059(2) Uani 1 d . . H206 H 1.0070(5) -0.0459(4) 0.1486(3) 0.071 Uiso 1 calc R . C301 C 0.9061(5) -0.0653(3) 0.2956(3) 0.0495(15) Uani 1 d . . C302 C 0.9615(6) -0.0231(4) 0.3014(3) 0.065(2) Uani 1 d . . H302 H 0.9698(6) 0.0066(4) 0.2705(3) 0.079 Uiso 1 calc R . C303 C 1.0056(6) -0.0228(4) 0.3513(3) 0.069(2) Uani 1 d . . H303 H 1.0409(6) 0.0072(4) 0.3532(3) 0.083 Uiso 1 calc R . C304 C 0.9968(6) -0.0665(5) 0.3969(4) 0.075(2) Uani 1 d . . H304 H 1.0273(6) -0.0676(5) 0.4297(4) 0.090 Uiso 1 calc R . C305 C 0.9421(6) -0.1091(4) 0.3938(4) 0.076(2) Uani 1 d . . H305 H 0.9348(6) -0.1389(4) 0.4248(4) 0.091 Uiso 1 calc R . C306 C 0.8979(5) -0.1077(4) 0.3443(3) 0.062(2) Uani 1 d . . H306 H 0.8606(5) -0.1366(4) 0.3436(3) 0.074 Uiso 1 calc R . C401 C 0.8162(5) 0.0095(4) 0.2070(3) 0.055(2) Uani 1 d . . C402 C 0.7725(6) 0.0707(4) 0.2424(4) 0.070(2) Uani 1 d . . H402 H 0.7748(6) 0.0674(4) 0.2827(4) 0.084 Uiso 1 calc R . C403 C 0.7258(6) 0.1360(4) 0.2192(5) 0.083(3) Uani 1 d . . H403 H 0.6954(6) 0.1755(4) 0.2441(5) 0.100 Uiso 1 calc R . C404 C 0.7240(6) 0.1430(5) 0.1603(5) 0.085(3) Uani 1 d . . H404 H 0.6955(6) 0.1874(5) 0.1445(5) 0.102 Uiso 1 calc R . C405 C 0.7640(6) 0.0846(5) 0.1244(4) 0.080(3) Uani 1 d . . H405 H 0.7609(6) 0.0887(5) 0.0842(4) 0.096 Uiso 1 calc R . C406 C 0.8096(5) 0.0187(4) 0.1480(3) 0.061(2) Uani 1 d . . H406 H 0.8366(5) -0.0207(4) 0.1229(3) 0.073 Uiso 1 calc R . B2 B -0.2363(8) 0.5059(5) 0.1570(4) 0.075(3) Uani 1 d . . C501 C -0.2130(6) 0.4822(4) 0.0869(4) 0.072(2) Uani 1 d . . C502 C -0.1295(8) 0.4796(6) 0.0495(4) 0.106(3) Uani 1 d . . H502 H -0.0811(8) 0.4916(6) 0.0636(4) 0.127 Uiso 1 calc R . C503 C -0.1155(9) 0.4588(7) -0.0111(5) 0.124(4) Uani 1 d . . H503 H -0.0577(9) 0.4588(7) -0.0346(5) 0.148 Uiso 1 calc R . C504 C -0.1736(11) 0.4407(6) -0.0354(5) 0.114(4) Uani 1 d . . H504 H -0.1570(11) 0.4218(6) -0.0735(5) 0.136 Uiso 1 calc R . C505 C -0.2681(11) 0.4511(7) -0.0005(5) 0.134(4) Uani 1 d . . H505 H -0.3175(11) 0.4445(7) -0.0178(5) 0.161 Uiso 1 calc R . C506 C -0.2867(9) 0.4710(6) 0.0591(4) 0.113(4) Uani 1 d . . H506 H -0.3482(9) 0.4770(6) 0.0809(4) 0.136 Uiso 1 calc R . C601 C -0.2504(6) 0.4408(4) 0.1989(3) 0.073(2) Uani 1 d . . C602 C -0.2858(7) 0.3914(5) 0.1831(4) 0.098(3) Uani 1 d . . H602 H -0.2984(7) 0.3915(5) 0.1446(4) 0.118 Uiso 1 calc R . C603 C -0.3043(8) 0.3402(6) 0.2215(5) 0.111(4) Uani 1 d . . H603 H -0.3277(8) 0.3075(6) 0.2077(5) 0.133 Uiso 1 calc R . C604 C -0.2892(7) 0.3375(5) 0.2773(5) 0.091(3) Uani 1 d . . H604 H -0.3096(7) 0.3077(5) 0.3040(5) 0.109 Uiso 1 calc R . C605 C -0.2434(9) 0.3795(5) 0.2939(4) 0.110(4) Uani 1 d . . H605 H -0.2240(9) 0.3744(5) 0.3310(4) 0.132 Uiso 1 calc R . C606 C -0.2252(11) 0.4302(6) 0.2558(4) 0.130(5) Uani 1 d . . H606 H -0.1946(11) 0.4589(6) 0.2689(4) 0.156 Uiso 1 calc R . C701 C -0.1453(9) 0.5285(5) 0.1748(4) 0.093(3) Uani 1 d . . C702 C -0.0528(10) 0.4780(7) 0.1765(5) 0.121(4) Uani 1 d . . H702 H -0.0437(10) 0.4307(7) 0.1698(5) 0.145 Uiso 1 calc R . C703 C 0.0281(12) 0.4950(10) 0.1877(6) 0.145(5) Uani 1 d . . H703 H 0.0892(12) 0.4597(10) 0.1883(6) 0.174 Uiso 1 calc R . C704 C 0.0150(15) 0.5641(12) 0.1976(6) 0.159(7) Uani 1 d . . H704 H 0.0675(15) 0.5772(12) 0.2041(6) 0.191 Uiso 1 calc R . C705 C -0.0778(15) 0.6145(9) 0.1979(6) 0.141(5) Uani 1 d . . H705 H -0.0877(15) 0.6615(9) 0.2064(6) 0.170 Uiso 1 calc R . C706 C -0.1537(10) 0.5982(6) 0.1865(4) 0.110(4) Uani 1 d . . H706 H -0.2143(10) 0.6343(6) 0.1863(4) 0.132 Uiso 1 calc R . C801 C -0.3361(8) 0.5730(4) 0.1708(4) 0.095(3) Uani 1 d . . C802 C -0.3665(7) 0.6277(4) 0.1315(4) 0.088(3) Uani 1 d . . H802 H -0.3274(7) 0.6226(4) 0.0948(4) 0.106 Uiso 1 calc R . C803 C -0.4464(9) 0.6872(5) 0.1408(6) 0.138(5) Uani 1 d . . H803 H -0.4658(9) 0.7192(5) 0.1109(6) 0.165 Uiso 1 calc R . C804 C -0.4991(11) 0.6983(6) 0.1987(9) 0.177(8) Uani 1 d . . H804 H -0.5535(11) 0.7396(6) 0.2075(9) 0.212 Uiso 1 calc R . C805 C -0.4720(10) 0.6494(7) 0.2430(7) 0.170(6) Uani 1 d . . H805 H -0.5058(10) 0.6579(7) 0.2813(7) 0.204 Uiso 1 calc R . C806 C -0.3926(10) 0.5874(6) 0.2278(5) 0.135(5) Uani 1 d . . H806 H -0.3755(10) 0.5533(6) 0.2566(5) 0.162 Uiso 1 calc R . O1 O 1.1794(7) -0.2110(5) 0.2904(4) 0.180(3) Uiso 1 d . . H1 H 1.1815(63) -0.2498(35) 0.3037(55) 0.269 Uiso 1 calc R . C77 C -0.7288(8) 0.8081(6) 0.3077(5) 0.133(3) Uiso 1 d . . H77A H -0.7438(8) 0.8243(6) 0.3480(5) 0.199 Uiso 1 calc R . H77B H -0.7182(8) 0.8448(6) 0.2824(5) 0.199 Uiso 1 calc R . H77C H -0.6702(8) 0.7666(6) 0.3028(5) 0.199 Uiso 1 calc R . O2 O 1.3267(7) -0.4212(6) 0.1806(4) 0.207(3) Uiso 1 d . . H2 H 1.3296(31) -0.4055(82) 0.2124(28) 0.311 Uiso 1 calc R . C78 C 1.4195(10) -0.4397(7) 0.1447(6) 0.185(5) Uiso 1 d . . H78A H 1.4107(10) -0.4288(7) 0.1045(6) 0.278 Uiso 1 calc R . H78B H 1.4548(10) -0.4895(7) 0.1479(6) 0.278 Uiso 1 calc R . H78C H 1.4563(10) -0.4133(7) 0.1574(6) 0.278 Uiso 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 0.0366(4) 0.0397(4) 0.0389(4) -0.0031(3) -0.0011(3) -0.0124(3) Ni2 0.0386(4) 0.0609(5) 0.0404(4) -0.0065(4) -0.0064(3) -0.0134(4) S1 0.0422(8) 0.0518(9) 0.0385(8) -0.0054(7) -0.0005(6) -0.0151(7) S2 0.0387(8) 0.0446(8) 0.0381(8) -0.0030(6) -0.0032(6) -0.0111(6) Cl1 0.0510(9) 0.0629(10) 0.0690(11) -0.0043(8) -0.0093(8) -0.0270(8) N1 0.039(3) 0.043(3) 0.044(3) 0.003(2) -0.004(2) -0.016(2) N2 0.041(3) 0.042(3) 0.049(3) -0.006(2) 0.001(2) -0.016(2) N3 0.043(3) 0.039(3) 0.044(3) 0.000(2) 0.000(2) -0.011(2) N4 0.047(3) 0.071(4) 0.044(3) -0.007(3) -0.013(2) -0.016(3) N5 0.055(4) 0.093(5) 0.048(3) -0.005(3) -0.016(3) -0.019(3) N6 0.056(3) 0.065(4) 0.056(4) 0.007(3) -0.010(3) -0.009(3) C1 0.045(3) 0.042(3) 0.033(3) 0.002(2) 0.001(3) -0.014(3) C2 0.049(3) 0.043(3) 0.041(3) 0.000(3) 0.000(3) -0.017(3) C3 0.056(4) 0.057(4) 0.057(4) 0.006(3) -0.009(3) -0.023(3) C4 0.083(5) 0.051(4) 0.060(4) 0.015(3) -0.016(4) -0.032(4) C5 0.075(5) 0.052(4) 0.057(4) 0.022(3) -0.013(4) -0.017(4) C6 0.055(4) 0.050(4) 0.046(4) 0.005(3) -0.005(3) -0.014(3) C7 0.041(3) 0.046(3) 0.046(3) 0.002(3) -0.002(3) -0.015(3) C8 0.055(4) 0.066(4) 0.046(4) -0.008(3) -0.008(3) -0.027(3) C9 0.036(3) 0.043(3) 0.064(4) 0.006(3) 0.000(3) -0.006(3) C10 0.041(3) 0.038(3) 0.058(4) -0.005(3) 0.008(3) -0.006(3) C11 0.063(4) 0.058(4) 0.077(5) -0.024(4) -0.006(4) -0.021(4) C12 0.051(4) 0.038(3) 0.059(4) 0.002(3) 0.010(3) -0.011(3) C13 0.045(3) 0.044(3) 0.053(4) 0.009(3) 0.000(3) -0.009(3) C14 0.045(4) 0.053(4) 0.062(4) 0.004(3) 0.009(3) -0.018(3) C15 0.047(3) 0.052(4) 0.041(3) -0.002(3) -0.005(3) -0.014(3) C16 0.043(3) 0.047(3) 0.043(3) -0.006(3) -0.006(3) -0.010(3) C17 0.043(3) 0.045(3) 0.040(3) -0.009(3) -0.002(3) -0.012(3) C18 0.043(3) 0.043(3) 0.050(4) -0.003(3) -0.007(3) -0.007(3) C19 0.038(3) 0.062(4) 0.050(4) -0.010(3) -0.001(3) -0.004(3) C20 0.043(3) 0.054(4) 0.044(4) -0.004(3) 0.003(3) -0.013(3) C21 0.049(4) 0.058(4) 0.043(4) -0.003(3) 0.002(3) -0.010(3) C22 0.042(3) 0.056(4) 0.052(4) -0.006(3) -0.006(3) -0.006(3) C23 0.048(4) 0.078(5) 0.068(5) 0.001(4) -0.002(3) -0.027(4) C24 0.044(4) 0.088(6) 0.058(4) -0.008(4) -0.008(3) -0.002(4) C25 0.046(4) 0.125(7) 0.053(4) -0.004(4) -0.020(3) -0.024(4) C26 0.097(7) 0.116(7) 0.075(6) -0.031(5) -0.031(5) -0.036(6) C27 0.067(5) 0.128(8) 0.056(5) -0.002(5) -0.021(4) -0.029(5) C28 0.049(4) 0.124(8) 0.064(5) 0.043(5) -0.018(4) -0.009(5) C29 0.080(6) 0.063(5) 0.088(6) 0.010(4) -0.001(5) -0.012(4) C30 0.051(4) 0.069(5) 0.051(4) 0.017(3) -0.011(3) -0.019(3) C31 0.115(7) 0.069(5) 0.092(6) 0.024(5) -0.037(6) -0.055(5) C32 0.199(13) 0.111(9) 0.124(9) -0.006(7) -0.062(9) -0.084(9) C33 0.170(13) 0.150(11) 0.210(14) 0.004(10) 0.012(11) -0.130(11) C34 0.211(14) 0.086(7) 0.203(13) 0.056(8) -0.097(11) -0.096(9) C35 0.056(4) 0.063(4) 0.048(4) -0.008(3) 0.011(3) -0.018(3) C36 0.064(5) 0.075(5) 0.064(5) -0.021(4) 0.018(4) -0.023(4) C37 0.066(5) 0.087(6) 0.067(5) -0.009(4) 0.014(4) -0.036(4) C38 0.076(5) 0.095(6) 0.047(4) -0.001(4) 0.014(4) -0.012(5) Ni3 0.0397(4) 0.0372(4) 0.0491(5) 0.0059(3) -0.0051(3) -0.0135(3) Ni4 0.0529(5) 0.0425(4) 0.0460(5) -0.0008(3) -0.0114(4) -0.0194(4) S3 0.0506(9) 0.0428(8) 0.0601(10) 0.0072(7) -0.0128(8) -0.0152(7) S4 0.0418(8) 0.0406(8) 0.0429(8) 0.0013(6) -0.0064(6) -0.0143(6) Cl2 0.0708(11) 0.0527(10) 0.0682(11) 0.0013(8) -0.0111(9) -0.0330(9) N7 0.045(3) 0.043(3) 0.058(3) -0.006(2) 0.001(2) -0.013(2) N8 0.048(3) 0.039(3) 0.061(3) 0.014(2) -0.005(3) -0.015(2) N9 0.044(3) 0.052(3) 0.052(3) 0.008(2) -0.002(2) -0.019(2) N10 0.065(4) 0.051(3) 0.054(3) -0.013(3) -0.012(3) -0.021(3) N11 0.074(4) 0.058(3) 0.057(3) 0.004(3) -0.024(3) -0.029(3) N12 0.064(3) 0.052(3) 0.045(3) -0.001(2) -0.006(3) -0.025(3) C39 0.045(3) 0.037(3) 0.061(4) 0.006(3) -0.010(3) -0.014(3) C40 0.046(3) 0.036(3) 0.059(4) -0.002(3) -0.003(3) -0.011(3) C41 0.053(4) 0.041(3) 0.054(4) -0.001(3) -0.002(3) -0.016(3) C42 0.058(4) 0.037(3) 0.058(4) -0.008(3) 0.001(3) -0.019(3) C43 0.065(4) 0.046(4) 0.066(4) 0.007(3) -0.003(4) -0.029(3) C44 0.058(4) 0.046(4) 0.054(4) 0.004(3) -0.008(3) -0.021(3) C45 0.045(3) 0.038(3) 0.069(4) -0.001(3) 0.003(3) -0.012(3) C46 0.072(5) 0.059(4) 0.069(5) -0.015(4) -0.015(4) -0.022(4) C47 0.066(5) 0.052(4) 0.059(4) -0.008(3) 0.011(4) -0.014(3) C48 0.048(4) 0.049(4) 0.083(5) 0.012(4) 0.011(4) -0.006(3) C49 0.049(4) 0.098(6) 0.088(6) 0.022(5) -0.021(4) -0.032(4) C50 0.048(4) 0.043(3) 0.061(4) 0.012(3) 0.000(3) -0.014(3) C51 0.048(4) 0.046(4) 0.054(4) 0.011(3) -0.004(3) -0.012(3) C52 0.056(4) 0.040(3) 0.073(5) 0.013(3) -0.008(4) -0.016(3) C53 0.041(3) 0.052(4) 0.055(4) 0.009(3) -0.005(3) -0.013(3) C54 0.047(3) 0.040(3) 0.053(4) 0.005(3) -0.007(3) -0.014(3) C55 0.049(3) 0.035(3) 0.052(4) -0.006(3) -0.004(3) -0.015(3) C56 0.049(4) 0.048(4) 0.057(4) 0.001(3) -0.002(3) -0.015(3) C57 0.052(4) 0.050(4) 0.069(5) -0.006(3) 0.002(3) -0.004(3) C58 0.054(4) 0.040(3) 0.066(5) 0.005(3) -0.005(3) -0.008(3) C59 0.052(4) 0.045(4) 0.058(4) 0.010(3) -0.005(3) -0.010(3) C60 0.057(4) 0.062(4) 0.061(4) -0.010(4) -0.007(4) -0.011(3) C61 0.088(6) 0.039(4) 0.084(5) -0.012(4) -0.016(4) -0.019(4) C62 0.080(5) 0.074(5) 0.048(4) -0.008(4) -0.011(4) -0.016(4) C63 0.103(6) 0.070(5) 0.061(5) -0.014(4) -0.021(4) -0.035(5) C64 0.084(6) 0.102(7) 0.082(6) 0.000(5) -0.038(5) -0.043(5) C65 0.108(7) 0.076(5) 0.057(5) 0.001(4) -0.032(5) -0.039(5) C66 0.121(7) 0.076(5) 0.051(4) 0.000(4) -0.009(5) -0.051(5) C67 0.068(5) 0.070(5) 0.101(7) -0.001(5) -0.003(5) -0.032(4) C68 0.075(5) 0.052(4) 0.046(4) 0.009(3) -0.013(3) -0.025(4) C69 0.053(4) 0.066(5) 0.076(5) -0.016(4) 0.007(4) -0.033(4) C70 0.064(5) 0.135(9) 0.149(9) -0.072(7) 0.023(6) -0.055(6) C71 0.090(6) 0.116(8) 0.092(6) -0.027(6) -0.002(5) -0.066(6) C72 0.150(9) 0.066(5) 0.112(8) 0.002(5) 0.001(7) -0.064(6) C73 0.055(4) 0.051(4) 0.077(5) 0.012(4) -0.001(4) -0.004(3) B1 0.057(4) 0.046(4) 0.053(4) 0.011(3) -0.008(4) -0.023(3) C101 0.056(4) 0.052(4) 0.059(4) 0.019(3) -0.015(3) -0.021(3) C102 0.076(5) 0.062(4) 0.070(5) 0.016(4) -0.028(4) -0.035(4) C103 0.084(6) 0.083(6) 0.108(7) 0.042(5) -0.055(6) -0.047(5) C104 0.074(6) 0.116(8) 0.107(8) 0.071(6) -0.052(6) -0.057(6) C105 0.055(5) 0.102(7) 0.088(6) 0.032(5) -0.019(4) -0.034(5) C106 0.059(4) 0.068(5) 0.075(5) 0.019(4) -0.010(4) -0.025(4) C201 0.055(4) 0.051(4) 0.051(4) 0.005(3) -0.015(3) -0.021(3) C202 0.063(5) 0.062(5) 0.073(5) 0.004(4) -0.014(4) -0.020(4) C203 0.075(6) 0.058(5) 0.099(7) -0.009(5) -0.021(5) -0.005(4) C204 0.053(5) 0.102(7) 0.088(6) -0.026(5) -0.002(4) -0.012(5) C205 0.053(4) 0.105(7) 0.075(5) -0.009(5) -0.006(4) -0.033(5) C206 0.052(4) 0.067(5) 0.060(4) 0.002(3) -0.008(3) -0.022(4) C301 0.054(4) 0.045(3) 0.051(4) -0.003(3) 0.001(3) -0.023(3) C302 0.079(5) 0.075(5) 0.055(4) 0.002(4) 0.001(4) -0.046(4) C303 0.071(5) 0.083(5) 0.065(5) -0.018(4) 0.005(4) -0.046(4) C304 0.075(5) 0.096(6) 0.064(5) -0.004(4) -0.012(4) -0.043(5) C305 0.090(6) 0.085(6) 0.067(5) 0.018(4) -0.027(4) -0.043(5) C306 0.076(5) 0.057(4) 0.064(5) 0.015(3) -0.018(4) -0.037(4) C401 0.047(4) 0.053(4) 0.067(5) 0.010(3) -0.002(3) -0.024(3) C402 0.068(5) 0.060(5) 0.080(5) 0.006(4) 0.005(4) -0.027(4) C403 0.065(5) 0.047(4) 0.130(8) 0.005(5) 0.004(5) -0.018(4) C404 0.058(5) 0.059(5) 0.146(9) 0.042(6) -0.039(6) -0.027(4) C405 0.064(5) 0.094(6) 0.100(7) 0.043(5) -0.041(5) -0.043(5) C406 0.059(4) 0.059(4) 0.071(5) 0.018(4) -0.021(4) -0.025(3) B2 0.093(7) 0.054(5) 0.068(6) 0.008(4) -0.008(5) -0.019(5) C501 0.082(6) 0.063(5) 0.067(5) 0.008(4) -0.013(5) -0.020(4) C502 0.107(8) 0.140(9) 0.076(6) 0.001(6) -0.007(6) -0.055(7) C503 0.107(9) 0.173(12) 0.075(7) 0.003(7) 0.021(6) -0.044(9) C504 0.143(11) 0.117(9) 0.071(7) -0.014(6) -0.010(7) -0.035(8) C505 0.164(12) 0.181(12) 0.085(8) 0.008(8) -0.036(8) -0.088(10) C506 0.131(10) 0.133(9) 0.072(7) 0.008(6) -0.006(6) -0.045(8) C601 0.096(6) 0.057(5) 0.058(5) -0.002(4) -0.013(4) -0.016(4) C602 0.127(8) 0.110(8) 0.090(7) 0.041(6) -0.044(6) -0.073(7) C603 0.130(9) 0.123(9) 0.111(8) 0.046(7) -0.047(7) -0.076(7) C604 0.088(6) 0.086(7) 0.098(7) 0.027(6) -0.020(6) -0.028(5) C605 0.175(11) 0.090(7) 0.061(6) 0.015(5) -0.022(6) -0.041(7) C606 0.248(15) 0.091(7) 0.067(6) -0.007(5) -0.028(8) -0.077(9) C701 0.138(9) 0.087(7) 0.064(5) 0.005(5) -0.019(6) -0.050(7) C702 0.126(10) 0.111(9) 0.124(10) -0.002(7) -0.043(8) -0.028(8) C703 0.154(13) 0.196(17) 0.110(10) 0.021(10) -0.055(9) -0.080(13) C704 0.210(18) 0.229(21) 0.100(10) 0.019(12) -0.052(12) -0.144(17) C705 0.221(18) 0.147(13) 0.102(9) 0.007(9) -0.034(12) -0.117(14) C706 0.164(11) 0.093(8) 0.098(8) 0.009(6) -0.026(7) -0.073(8) C801 0.115(8) 0.060(5) 0.088(7) 0.009(5) 0.015(6) -0.018(5) C802 0.104(7) 0.058(5) 0.087(6) 0.010(4) 0.001(5) -0.016(5) C803 0.137(10) 0.053(6) 0.177(13) 0.019(7) 0.032(9) -0.003(6) C804 0.141(12) 0.056(7) 0.273(21) 0.031(10) 0.043(13) 0.004(7) C805 0.152(12) 0.087(8) 0.198(14) 0.022(9) 0.043(10) 0.015(8) C806 0.158(11) 0.088(8) 0.115(9) 0.003(6) 0.000(8) 0.003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #BOND LENGTHS AND ANGLES 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 N2 2.173(5) . ? Ni1 N3 2.181(5) . ? Ni1 N1 2.352(5) . ? Ni1 S2 2.405(2) . ? Ni1 Cl1 2.433(2) . ? Ni1 S1 2.471(2) . ? Ni2 N4 2.171(5) . ? Ni2 N5 2.175(6) . ? Ni2 N6 2.380(6) . ? Ni2 S2 2.423(2) . ? Ni2 Cl1 2.450(2) . ? Ni2 S1 2.498(2) . ? S1 C1 1.785(6) . ? S2 C17 1.770(6) . ? N1 C7 1.484(7) . ? N1 C8 1.478(7) . ? N1 C9 1.498(7) . ? N2 C10 1.482(7) . ? N2 C11 1.494(8) . ? N2 C12 1.491(8) . ? N3 C15 1.477(7) . ? N3 C13 1.485(7) . ? N3 C14 1.490(7) . ? N4 C23 1.476(9) . ? N4 C24 1.493(8) . ? N4 C22 1.493(8) . ? N5 C27 1.481(10) . ? N5 C26 1.490(10) . ? N5 C25 1.484(9) . ? N6 C30 1.505(8) . ? N6 C29 1.471(10) . ? N6 C28 1.514(9) . ? C1 C6 1.383(8) . ? C1 C2 1.401(8) . ? C2 C3 1.393(8) . ? C2 C7 1.485(8) . ? C3 C4 1.395(9) . ? C4 C5 1.402(10) . ? C4 C31 1.541(10) . ? C5 C6 1.391(9) . ? C6 C30 1.490(9) . ? C9 C10 1.496(9) . ? C12 C13 1.495(9) . ? C15 C16 1.497(8) . ? C16 C21 1.401(8) . ? C16 C17 1.409(8) . ? C17 C18 1.418(8) . ? C18 C19 1.394(8) . ? C18 C22 1.497(9) . ? C19 C20 1.383(9) . ? C20 C21 1.389(8) . ? C20 C35 1.516(8) . ? C24 C25 1.540(10) . ? C27 C28 1.487(12) . ? C31 C34 1.478(12) . ? C31 C32 1.510(13) . ? C31 C33 1.584(15) . ? C35 C38 1.529(10) . ? C35 C37 1.535(10) . ? C35 C36 1.530(10) . ? Ni3 N9 2.167(5) . ? Ni3 N8 2.173(5) . ? Ni3 N7 2.349(5) . ? Ni3 S4 2.407(2) . ? Ni3 S3 2.475(2) . ? Ni3 Cl2 2.516(2) . ? Ni4 N11 2.172(5) . ? Ni4 N10 2.222(5) . ? Ni4 N12 2.357(5) . ? Ni4 S4 2.371(2) . ? Ni4 Cl2 2.455(2) . ? Ni4 S3 2.483(2) . ? S3 C39 1.788(6) . ? S4 C55 1.793(6) . ? N7 C45 1.484(8) . ? N7 C47 1.480(8) . ? N7 C46 1.491(8) . ? N8 C48 1.482(8) . ? N8 C50 1.500(8) . ? N8 C49 1.499(9) . ? N9 C51 1.488(8) . ? N9 C53 1.514(8) . ? N9 C52 1.498(8) . ? N10 C62 1.470(8) . ? N10 C60 1.479(9) . ? N10 C61 1.490(9) . ? N11 C64 1.467(9) . ? N11 C63 1.502(9) . ? N11 C65 1.477(9) . ? N12 C66 1.490(9) . ? N12 C67 1.476(9) . ? N12 C68 1.506(8) . ? C39 C44 1.380(9) . ? C39 C40 1.407(9) . ? C40 C41 1.402(8) . ? C40 C45 1.474(8) . ? C41 C42 1.381(9) . ? C42 C43 1.410(9) . ? C42 C69 1.539(9) . ? C43 C44 1.395(9) . ? C44 C68 1.489(9) . ? C47 C48 1.480(10) . ? C50 C51 1.502(9) . ? C53 C54 1.513(8) . ? C54 C55 1.399(9) . ? C54 C59 1.394(8) . ? C55 C56 1.401(8) . ? C56 C57 1.391(9) . ? C56 C60 1.537(9) . ? C57 C58 1.389(10) . ? C58 C59 1.390(9) . ? C58 C73 1.509(9) . ? C62 C63 1.500(11) . ? C65 C66 1.470(11) . ? C69 C71 1.526(11) . ? C69 C72 1.520(12) . ? C69 C70 1.510(10) . ? C73 C75A 1.48(2) . ? C73 C74B 1.49(2) . ? C73 C74A 1.49(2) . ? C73 C75B 1.53(2) . ? C73 C76A 1.55(2) . ? C73 C76B 1.48(2) . ? B1 C301 1.618(10) . ? B1 C201 1.634(10) . ? B1 C401 1.660(10) . ? B1 C101 1.663(10) . ? C101 C102 1.396(9) . ? C101 C106 1.385(10) . ? C102 C103 1.396(10) . ? C103 C104 1.352(13) . ? C104 C105 1.382(13) . ? C105 C106 1.370(10) . ? C201 C206 1.381(9) . ? C201 C202 1.403(9) . ? C202 C203 1.379(10) . ? C203 C204 1.357(12) . ? C204 C205 1.351(12) . ? C205 C206 1.397(10) . ? C301 C302 1.390(9) . ? C301 C306 1.396(9) . ? C302 C303 1.404(10) . ? C303 C304 1.360(11) . ? C304 C305 1.376(10) . ? C305 C306 1.388(10) . ? C401 C406 1.373(10) . ? C401 C402 1.397(10) . ? C402 C403 1.380(11) . ? C403 C404 1.358(13) . ? C404 C405 1.358(13) . ? C405 C406 1.389(10) . ? B2 C801 1.602(13) . ? B2 C701 1.664(15) . ? B2 C501 1.647(12) . ? B2 C601 1.647(12) . ? C501 C502 1.367(12) . ? C501 C506 1.425(13) . ? C502 C503 1.433(14) . ? C503 C504 1.247(15) . ? C504 C505 1.44(2) . ? C505 C506 1.398(14) . ? C601 C606 1.401(12) . ? C601 C602 1.357(11) . ? C602 C603 1.401(12) . ? C603 C604 1.330(13) . ? C604 C605 1.347(13) . ? C605 C606 1.389(13) . ? C701 C706 1.400(13) . ? C701 C702 1.385(14) . ? C702 C703 1.41(2) . ? C703 C704 1.36(2) . ? C704 C705 1.38(2) . ? C705 C706 1.33(2) . ? C801 C806 1.417(13) . ? C801 C802 1.386(12) . ? C802 C803 1.346(12) . ? C803 C804 1.41(2) . ? C804 C805 1.39(2) . ? C805 C806 1.386(15) . ? O1 C77 1.633(12) 1_745 ? C77 O1 1.633(12) 1_365 ? O2 C78 1.410(13) . ? 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 N2 Ni1 N3 83.2(2) . . ? N2 Ni1 N1 78.9(2) . . ? N3 Ni1 N1 100.2(2) . . ? N2 Ni1 S2 174.14(14) . . ? N3 Ni1 S2 91.43(13) . . ? N1 Ni1 S2 99.87(12) . . ? N2 Ni1 Cl1 94.19(14) . . ? N3 Ni1 Cl1 91.95(14) . . ? N1 Ni1 Cl1 165.15(13) . . ? S2 Ni1 Cl1 88.29(6) . . ? N2 Ni1 S1 105.22(14) . . ? N3 Ni1 S1 167.40(13) . . ? N1 Ni1 S1 90.78(13) . . ? S2 Ni1 S1 80.48(6) . . ? Cl1 Ni1 S1 78.26(7) . . ? N4 Ni2 N5 82.4(2) . . ? N4 Ni2 N6 101.8(2) . . ? N5 Ni2 N6 79.5(2) . . ? N4 Ni2 S2 91.03(14) . . ? N5 Ni2 S2 173.5(2) . . ? N6 Ni2 S2 101.7(2) . . ? N4 Ni2 Cl1 93.6(2) . . ? N5 Ni2 Cl1 93.2(2) . . ? N6 Ni2 Cl1 161.81(15) . . ? S2 Ni2 Cl1 87.46(7) . . ? N4 Ni2 S1 167.21(15) . . ? N5 Ni2 S1 106.9(2) . . ? N6 Ni2 S1 88.68(15) . . ? S2 Ni2 S1 79.58(6) . . ? Cl1 Ni2 S1 77.41(7) . . ? C1 S1 Ni1 102.0(2) . . ? C1 S1 Ni2 101.6(2) . . ? Ni1 S1 Ni2 79.70(6) . . ? C17 S2 Ni1 106.9(2) . . ? C17 S2 Ni2 106.9(2) . . ? Ni1 S2 Ni2 82.51(6) . . ? Ni1 Cl1 Ni2 81.38(6) . . ? C7 N1 C8 107.4(5) . . ? C7 N1 C9 105.2(4) . . ? C8 N1 C9 109.1(5) . . ? C7 N1 Ni1 109.9(3) . . ? C8 N1 Ni1 118.0(4) . . ? C9 N1 Ni1 106.6(3) . . ? C10 N2 C11 107.6(5) . . ? C10 N2 C12 110.2(5) . . ? C11 N2 C12 110.4(5) . . ? C10 N2 Ni1 108.4(3) . . ? C11 N2 Ni1 113.9(4) . . ? C12 N2 Ni1 106.4(3) . . ? C15 N3 C13 110.3(5) . . ? C15 N3 C14 108.6(5) . . ? C13 N3 C14 106.2(5) . . ? C15 N3 Ni1 111.2(4) . . ? C13 N3 Ni1 102.9(3) . . ? C14 N3 Ni1 117.3(4) . . ? C23 N4 C24 108.6(5) . . ? C23 N4 C22 108.5(5) . . ? C24 N4 C22 108.4(5) . . ? C23 N4 Ni2 116.9(4) . . ? C24 N4 Ni2 102.9(4) . . ? C22 N4 Ni2 111.2(4) . . ? C27 N5 C26 106.3(6) . . ? C27 N5 C25 110.2(6) . . ? C26 N5 C25 110.1(6) . . ? C27 N5 Ni2 107.7(5) . . ? C26 N5 Ni2 114.2(5) . . ? C25 N5 Ni2 108.4(4) . . ? C30 N6 C29 108.7(6) . . ? C30 N6 C28 104.9(5) . . ? C29 N6 C28 111.8(6) . . ? C30 N6 Ni2 110.6(4) . . ? C29 N6 Ni2 116.6(5) . . ? C28 N6 Ni2 103.5(5) . . ? C6 C1 C2 118.7(6) . . ? C6 C1 S1 120.6(5) . . ? C2 C1 S1 120.7(4) . . ? C3 C2 C1 120.2(6) . . ? C3 C2 C7 118.9(6) . . ? C1 C2 C7 120.5(5) . . ? C2 C3 C4 122.0(7) . . ? C3 C4 C5 116.4(6) . . ? C3 C4 C31 120.1(7) . . ? C5 C4 C31 123.5(6) . . ? C6 C5 C4 122.4(6) . . ? C1 C6 C5 120.2(6) . . ? C1 C6 C30 120.1(6) . . ? C5 C6 C30 119.4(6) . . ? C2 C7 N1 116.2(5) . . ? N1 C9 C10 109.4(5) . . ? N2 C10 C9 112.5(5) . . ? C13 C12 N2 114.3(5) . . ? N3 C13 C12 110.6(5) . . ? N3 C15 C16 112.7(5) . . ? C21 C16 C17 120.1(5) . . ? C21 C16 C15 118.9(6) . . ? C17 C16 C15 120.7(5) . . ? C18 C17 C16 117.5(5) . . ? C18 C17 S2 120.7(5) . . ? C16 C17 S2 121.8(4) . . ? C19 C18 C17 119.8(6) . . ? C19 C18 C22 119.3(5) . . ? C17 C18 C22 120.7(6) . . ? C18 C19 C20 123.1(6) . . ? C21 C20 C19 116.6(6) . . ? C21 C20 C35 123.8(6) . . ? C19 C20 C35 119.6(6) . . ? C16 C21 C20 122.4(6) . . ? C18 C22 N4 111.8(5) . . ? N4 C24 C25 109.9(6) . . ? N5 C25 C24 112.9(6) . . ? N5 C27 C28 110.3(6) . . ? C27 C28 N6 112.2(6) . . ? C6 C30 N6 114.3(5) . . ? C34 C31 C32 112.6(9) . . ? C34 C31 C4 113.2(8) . . ? C32 C31 C4 108.7(7) . . ? C34 C31 C33 106.6(9) . . ? C32 C31 C33 108.5(9) . . ? C4 C31 C33 107.0(7) . . ? C38 C35 C20 112.1(6) . . ? C38 C35 C37 108.8(6) . . ? C20 C35 C37 110.1(6) . . ? C38 C35 C36 107.5(6) . . ? C20 C35 C36 108.9(6) . . ? C37 C35 C36 109.4(6) . . ? N9 Ni3 N8 82.5(2) . . ? N9 Ni3 N7 100.6(2) . . ? N8 Ni3 N7 78.6(2) . . ? N9 Ni3 S4 91.43(14) . . ? N8 Ni3 S4 173.76(14) . . ? N7 Ni3 S4 101.05(13) . . ? N9 Ni3 S3 166.71(15) . . ? N8 Ni3 S3 107.19(14) . . ? N7 Ni3 S3 90.36(14) . . ? S4 Ni3 S3 79.02(6) . . ? N9 Ni3 Cl2 93.80(15) . . ? N8 Ni3 Cl2 95.7(2) . . ? N7 Ni3 Cl2 163.57(14) . . ? S4 Ni3 Cl2 86.33(7) . . ? S3 Ni3 Cl2 76.53(6) . . ? N11 Ni4 N10 82.4(2) . . ? N11 Ni4 N12 78.4(2) . . ? N10 Ni4 N12 100.7(2) . . ? N11 Ni4 S4 173.0(2) . . ? N10 Ni4 S4 91.86(15) . . ? N12 Ni4 S4 98.72(14) . . ? N11 Ni4 Cl2 95.9(2) . . ? N10 Ni4 Cl2 92.5(2) . . ? N12 Ni4 Cl2 164.68(15) . . ? S4 Ni4 Cl2 88.51(6) . . ? N11 Ni4 S3 106.8(2) . . ? N10 Ni4 S3 166.9(2) . . ? N12 Ni4 S3 90.46(14) . . ? S4 Ni4 S3 79.54(6) . . ? Cl2 Ni4 S3 77.51(6) . . ? C39 S3 Ni3 102.3(2) . . ? C39 S3 Ni4 102.1(2) . . ? Ni3 S3 Ni4 80.90(6) . . ? C55 S4 Ni4 107.8(2) . . ? C55 S4 Ni3 107.8(2) . . ? Ni4 S4 Ni3 84.63(6) . . ? Ni4 Cl2 Ni3 80.66(6) . . ? C45 N7 C47 105.5(5) . . ? C45 N7 C46 108.5(5) . . ? C47 N7 C46 108.7(5) . . ? C45 N7 Ni3 110.0(4) . . ? C47 N7 Ni3 106.8(4) . . ? C46 N7 Ni3 116.7(4) . . ? C48 N8 C50 109.1(5) . . ? C48 N8 C49 108.0(6) . . ? C50 N8 C49 109.9(5) . . ? C48 N8 Ni3 108.5(4) . . ? C50 N8 Ni3 107.6(4) . . ? C49 N8 Ni3 113.7(4) . . ? C51 N9 C53 109.3(5) . . ? C51 N9 C52 108.7(5) . . ? C53 N9 C52 108.7(5) . . ? C51 N9 Ni3 104.0(4) . . ? C53 N9 Ni3 110.1(4) . . ? C52 N9 Ni3 115.8(4) . . ? C62 N10 C60 109.4(6) . . ? C62 N10 C61 107.5(5) . . ? C60 N10 C61 109.2(6) . . ? C62 N10 Ni4 103.7(4) . . ? C60 N10 Ni4 110.1(4) . . ? C61 N10 Ni4 116.6(4) . . ? C64 N11 C63 109.9(6) . . ? C64 N11 C65 108.3(6) . . ? C63 N11 C65 109.7(6) . . ? C64 N11 Ni4 112.6(5) . . ? C63 N11 Ni4 106.6(4) . . ? C65 N11 Ni4 109.9(4) . . ? C66 N12 C67 109.6(6) . . ? C66 N12 C68 104.5(5) . . ? C67 N12 C68 107.5(5) . . ? C66 N12 Ni4 106.4(4) . . ? C67 N12 Ni4 118.7(4) . . ? C68 N12 Ni4 109.3(4) . . ? C44 C39 C40 118.5(6) . . ? C44 C39 S3 121.0(5) . . ? C40 C39 S3 120.5(5) . . ? C41 C40 C39 119.6(6) . . ? C41 C40 C45 120.3(6) . . ? C39 C40 C45 119.9(6) . . ? C42 C41 C40 122.9(6) . . ? C41 C42 C43 116.0(6) . . ? C41 C42 C69 124.0(6) . . ? C43 C42 C69 120.0(6) . . ? C42 C43 C44 122.2(6) . . ? C39 C44 C43 120.6(6) . . ? C39 C44 C68 120.5(6) . . ? C43 C44 C68 118.8(6) . . ? C40 C45 N7 114.9(5) . . ? N7 C47 C48 110.0(6) . . ? N8 C48 C47 112.9(6) . . ? N8 C50 C51 113.0(5) . . ? N9 C51 C50 110.3(5) . . ? N9 C53 C54 112.1(5) . . ? C55 C54 C59 119.6(6) . . ? C55 C54 C53 121.5(5) . . ? C59 C54 C53 118.7(6) . . ? C54 C55 C56 118.6(6) . . ? C54 C55 S4 119.8(4) . . ? C56 C55 S4 121.5(5) . . ? C57 C56 C55 119.9(6) . . ? C57 C56 C60 118.8(6) . . ? C55 C56 C60 121.1(6) . . ? C56 C57 C58 122.5(6) . . ? C59 C58 C57 116.6(6) . . ? C59 C58 C73 121.5(6) . . ? C57 C58 C73 121.9(6) . . ? C54 C59 C58 122.6(6) . . ? N10 C60 C56 112.1(6) . . ? N10 C62 C63 109.9(6) . . ? N11 C63 C62 113.9(6) . . ? C66 C65 N11 113.6(7) . . ? C65 C66 N12 110.2(6) . . ? C44 C68 N12 113.5(5) . . ? C42 C69 C71 111.4(6) . . ? C42 C69 C72 108.9(6) . . ? C71 C69 C72 108.5(7) . . ? C42 C69 C70 109.1(6) . . ? C71 C69 C70 109.0(7) . . ? C72 C69 C70 109.9(8) . . ? C75A C73 C58 113.4(9) . . ? C58 C73 C74B 108.5(11) . . ? C75A C73 C74A 109.4(12) . . ? C58 C73 C74A 110.6(9) . . ? C58 C73 C75B 111.1(9) . . ? C74B C73 C75B 107.2(13) . . ? C75A C73 C76A 105.5(12) . . ? C58 C73 C76A 109.4(10) . . ? C74A C73 C76A 108.3(11) . . ? C58 C73 C76B 114.7(11) . . ? C74B C73 C76B 110.9(15) . . ? C75B C73 C76B 104.1(13) . . ? C301 B1 C201 104.3(5) . . ? C301 B1 C401 111.4(6) . . ? C201 B1 C401 112.6(5) . . ? C301 B1 C101 112.1(5) . . ? C201 B1 C101 113.6(6) . . ? C401 B1 C101 103.1(5) . . ? C102 C101 C106 115.5(7) . . ? C102 C101 B1 124.3(6) . . ? C106 C101 B1 120.0(6) . . ? C101 C102 C103 123.1(8) . . ? C104 C103 C102 118.0(9) . . ? C103 C104 C105 121.3(8) . . ? C106 C105 C104 119.5(9) . . ? C105 C106 C101 122.5(8) . . ? C206 C201 C202 113.4(6) . . ? C206 C201 B1 124.1(6) . . ? C202 C201 B1 122.2(6) . . ? C203 C202 C201 123.0(7) . . ? C202 C203 C204 120.4(8) . . ? C205 C204 C203 120.0(8) . . ? C204 C205 C206 118.9(8) . . ? C201 C206 C205 124.3(7) . . ? C302 C301 C306 113.7(6) . . ? C302 C301 B1 121.9(6) . . ? C306 C301 B1 124.0(6) . . ? C303 C302 C301 123.6(7) . . ? C304 C303 C302 120.0(7) . . ? C303 C304 C305 118.9(7) . . ? C304 C305 C306 120.1(7) . . ? C305 C306 C301 123.7(7) . . ? C406 C401 C402 115.7(7) . . ? C406 C401 B1 121.6(6) . . ? C402 C401 B1 122.5(7) . . ? C401 C402 C403 121.8(8) . . ? C404 C403 C402 120.4(9) . . ? C403 C404 C405 119.6(8) . . ? C406 C405 C404 119.8(9) . . ? C405 C406 C401 122.6(8) . . ? C801 B2 C701 107.7(8) . . ? C801 B2 C501 111.2(7) . . ? C701 B2 C501 110.1(7) . . ? C801 B2 C601 107.3(7) . . ? C701 B2 C601 110.2(7) . . ? C501 B2 C601 110.3(7) . . ? C502 C501 C506 114.5(8) . . ? C502 C501 B2 124.6(9) . . ? C506 C501 B2 120.5(8) . . ? C501 C502 C503 120.9(10) . . ? C504 C503 C502 126.0(11) . . ? C503 C504 C505 115.5(11) . . ? C504 C505 C506 121.0(12) . . ? C505 C506 C501 121.1(11) . . ? C606 C601 C602 112.4(8) . . ? C606 C601 B2 122.4(8) . . ? C602 C601 B2 125.2(8) . . ? C601 C602 C603 123.6(9) . . ? C604 C603 C602 121.5(10) . . ? C603 C604 C605 117.8(9) . . ? C604 C605 C606 120.2(10) . . ? C605 C606 C601 123.8(10) . . ? C706 C701 C702 115.1(11) . . ? C706 C701 B2 123.9(10) . . ? C702 C701 B2 120.9(9) . . ? C703 C702 C701 123.0(13) . . ? C704 C703 C702 118.7(16) . . ? C703 C704 C705 118.5(16) . . ? C706 C705 C704 122.4(16) . . ? C705 C706 C701 122.1(14) . . ? C806 C801 C802 113.6(9) . . ? C806 C801 B2 122.1(9) . . ? C802 C801 B2 123.5(8) . . ? C803 C802 C801 127.1(10) . . ? C804 C803 C802 116.1(11) . . ? C803 C804 C805 121.9(11) . . ? C806 C805 C804 117.4(13) . . ? C801 C806 C805 123.6(11) . . ? #===END data_6 _database_code_CSD 162723 #CHEMICAL DATA _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_formula_sum 'C63 H89 B N6 Ni2 O2 S2' _chemical_formula_weight 1154.75 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from methanol ; #CRYSTAL DATA _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 13.734(3) _cell_length_b 14.093(3) _cell_length_c 18.094(4) _cell_angle_alpha 103.24(3) _cell_angle_beta 97.42(3) _cell_angle_gamma 98.09(3) _cell_volume 3327.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not determined' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 1.00 #EXPERIMENTAL DATA _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'BRUKER SMART CCD' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method 'multirun' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30866 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.3313 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.32 #REFINEMENT DATA _reflns_number_total 15786 _reflns_number_observed 4271 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1349P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15786 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2617 _refine_ls_R_factor_obs 0.0893 _refine_ls_wR_factor_all 0.3036 _refine_ls_wR_factor_obs 0.2381 _refine_ls_goodness_of_fit_all 0.853 _refine_ls_goodness_of_fit_obs 1.332 _refine_ls_restrained_S_all 0.853 _refine_ls_restrained_S_obs 1.332 _refine_ls_shift/esd_max -0.056 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 1.699 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.215 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.30720(10) 0.13733(8) 0.06896(7) 0.0510(4) Uani 1 d . . Ni2 Ni 0.39327(9) 0.14605(8) 0.23415(6) 0.0430(3) Uani 1 d . . S1 S 0.4326(2) 0.04667(15) 0.11385(12) 0.0428(6) Uani 1 d . . S2 S 0.2259(2) 0.0844(2) 0.16984(15) 0.0592(7) Uani 1 d . . O1 O 0.3865(5) 0.2454(5) 0.1637(4) 0.064(2) Uiso 1 d . . N1 N 0.2494(5) -0.0028(5) -0.0393(4) 0.043(2) Uani 1 d . . N2 N 0.3681(6) 0.1890(5) -0.0211(4) 0.045(2) Uani 1 d . . N3 N 0.2018(6) 0.2329(6) 0.0518(5) 0.065(2) Uani 1 d . . N4 N 0.3481(6) 0.2482(5) 0.3277(4) 0.052(2) Uani 1 d . . N5 N 0.5407(6) 0.2055(5) 0.2990(4) 0.051(2) Uani 1 d . . N6 N 0.4226(5) 0.0161(5) 0.2928(4) 0.044(2) Uani 1 d . . C1 C 0.3619(6) -0.0706(5) 0.1043(5) 0.037(2) Uani 1 d . . C2 C 0.2997(6) -0.1235(5) 0.0353(5) 0.037(2) Uani 1 d . . C3 C 0.2416(7) -0.2147(6) 0.0290(5) 0.047(2) Uani 1 d . . H3 H 0.2012(7) -0.2481(6) -0.0176(5) 0.056 Uiso 1 calc R . C4 C 0.2428(7) -0.2574(6) 0.0919(6) 0.048(2) Uani 1 d . . C5 C 0.3081(6) -0.2069(6) 0.1591(5) 0.043(2) Uani 1 d . . H5 H 0.3123(6) -0.2356(6) 0.2006(5) 0.052 Uiso 1 calc R . C6 C 0.3672(6) -0.1161(5) 0.1671(5) 0.037(2) Uani 1 d . . C7 C 0.3071(7) -0.0832(6) -0.0354(5) 0.044(2) Uani 1 d . . H7A H 0.3767(7) -0.0585(6) -0.0355(5) 0.053 Uiso 1 calc R . H7B H 0.2836(7) -0.1370(6) -0.0812(5) 0.053 Uiso 1 calc R . C8 C 0.1439(7) -0.0454(7) -0.0522(6) 0.070(3) Uani 1 d . . H8A H 0.1281(7) -0.0670(7) -0.0079(6) 0.105 Uiso 1 calc R . H8B H 0.1292(7) -0.1010(7) -0.0965(6) 0.105 Uiso 1 calc R . H8C H 0.1048(7) 0.0036(7) -0.0609(6) 0.105 Uiso 1 calc R . C9 C 0.2764(8) 0.0312(7) -0.1063(5) 0.058(3) Uani 1 d . . H9A H 0.2834(8) -0.0252(7) -0.1464(5) 0.070 Uiso 1 calc R . H9B H 0.2237(8) 0.0620(7) -0.1267(5) 0.070 Uiso 1 calc R . C10 C 0.3699(7) 0.1022(6) -0.0847(5) 0.054(3) Uani 1 d . . H10A H 0.3846(7) 0.1250(6) -0.1294(5) 0.065 Uiso 1 calc R . H10B H 0.4234(7) 0.0688(6) -0.0694(5) 0.065 Uiso 1 calc R . C11 C 0.4708(7) 0.2435(7) 0.0068(6) 0.065(3) Uani 1 d . . H11A H 0.5002(7) 0.2567(7) -0.0359(6) 0.098 Uiso 1 calc R . H11B H 0.5093(7) 0.2043(7) 0.0317(6) 0.098 Uiso 1 calc R . H11C H 0.4698(7) 0.3049(7) 0.0428(6) 0.098 Uiso 1 calc R . C12 C 0.3073(7) 0.2558(7) -0.0480(5) 0.058(3) Uani 1 d . . H12A H 0.3048(7) 0.2469(7) -0.1030(5) 0.070 Uiso 1 calc R . H12B H 0.3374(7) 0.3240(7) -0.0226(5) 0.070 Uiso 1 calc R . C13 C 0.2000(8) 0.2342(7) -0.0302(6) 0.070(3) Uani 1 d . . H13A H 0.1633(8) 0.2846(7) -0.0416(6) 0.083 Uiso 1 calc R . H13B H 0.1658(8) 0.1706(7) -0.0630(6) 0.083 Uiso 1 calc R . C14 C 0.2296(9) 0.3364(7) 0.0981(7) 0.094(4) Uani 1 d . . H14A H 0.1945(9) 0.3779(7) 0.0732(7) 0.141 Uiso 1 calc R . H14B H 0.3001(9) 0.3579(7) 0.1029(7) 0.141 Uiso 1 calc R . H14C H 0.2122(9) 0.3408(7) 0.1484(7) 0.141 Uiso 1 calc R . C15 C 0.1030(8) 0.1928(8) 0.0647(5) 0.067(3) Uani 1 d . . H15A H 0.0890(8) 0.1216(8) 0.0434(5) 0.081 Uiso 1 calc R . H15B H 0.0528(8) 0.2211(8) 0.0384(5) 0.081 Uiso 1 calc R . C16 C 0.0974(8) 0.2163(8) 0.1515(6) 0.069(3) Uani 1 d . . C17 C 0.1628(8) 0.1816(8) 0.2035(6) 0.066(3) Uani 1 d . . C18 C 0.1667(9) 0.2250(8) 0.2829(6) 0.073(3) Uani 1 d . . C19 C 0.1030(9) 0.2922(9) 0.3067(6) 0.094(4) Uani 1 d . . H19 H 0.1079(9) 0.3204(9) 0.3591(6) 0.113 Uiso 1 calc R . C20 C 0.0340(8) 0.3179(9) 0.2561(6) 0.087(4) Uani 1 d . . C21 C 0.0364(8) 0.2853(9) 0.1785(6) 0.094(4) Uani 1 d . . H21 H -0.0027(8) 0.3090(9) 0.1433(6) 0.112 Uiso 1 calc R . C22 C 0.2516(8) 0.2096(9) 0.3426(6) 0.077(3) Uani 1 d . . H22A H 0.2438(8) 0.2429(9) 0.3941(6) 0.092 Uiso 1 calc R . H22B H 0.2470(8) 0.1395(9) 0.3397(6) 0.092 Uiso 1 calc R . C23 C 0.3447(8) 0.3497(7) 0.3149(6) 0.080(4) Uani 1 d . . H23A H 0.4022(8) 0.3707(7) 0.2937(6) 0.120 Uiso 1 calc R . H23B H 0.3446(8) 0.3956(7) 0.3632(6) 0.120 Uiso 1 calc R . H23C H 0.2853(8) 0.3474(7) 0.2798(6) 0.120 Uiso 1 calc R . C24 C 0.4255(8) 0.2547(7) 0.3937(5) 0.064(3) Uani 1 d . . H24A H 0.4173(8) 0.1930(7) 0.4092(5) 0.077 Uiso 1 calc R . H24B H 0.4187(8) 0.3074(7) 0.4368(5) 0.077 Uiso 1 calc R . C25 C 0.5281(8) 0.2752(7) 0.3721(6) 0.074(3) Uani 1 d . . H25A H 0.5404(8) 0.3424(7) 0.3665(6) 0.089 Uiso 1 calc R . H25B H 0.5778(8) 0.2705(7) 0.4138(6) 0.089 Uiso 1 calc R . C26 C 0.6067(8) 0.2575(8) 0.2611(6) 0.078(3) Uani 1 d . . H26A H 0.5907(8) 0.3222(8) 0.2635(6) 0.117 Uiso 1 calc R . H26B H 0.5996(8) 0.2215(8) 0.2082(6) 0.117 Uiso 1 calc R . H26C H 0.6742(8) 0.2637(8) 0.2860(6) 0.117 Uiso 1 calc R . C27 C 0.5859(7) 0.1236(7) 0.3185(5) 0.056(3) Uani 1 d . . H27A H 0.6458(7) 0.1510(7) 0.3565(5) 0.067 Uiso 1 calc R . H27B H 0.6053(7) 0.0853(7) 0.2727(5) 0.067 Uiso 1 calc R . C28 C 0.5172(6) 0.0568(6) 0.3494(5) 0.050(2) Uani 1 d . . H28A H 0.5020(6) 0.0932(6) 0.3977(5) 0.060 Uiso 1 calc R . H28B H 0.5491(6) 0.0027(6) 0.3593(5) 0.060 Uiso 1 calc R . C29 C 0.3393(8) -0.0232(7) 0.3308(5) 0.066(3) Uani 1 d . . H29A H 0.3254(8) 0.0299(7) 0.3695(5) 0.099 Uiso 1 calc R . H29B H 0.3592(8) -0.0736(7) 0.3543(5) 0.099 Uiso 1 calc R . H29C H 0.2805(8) -0.0508(7) 0.2928(5) 0.099 Uiso 1 calc R . C30 C 0.4447(7) -0.0717(6) 0.2368(5) 0.046(2) Uani 1 d . . H30A H 0.5071(7) -0.0517(6) 0.2202(5) 0.056 Uiso 1 calc R . H30B H 0.4545(7) -0.1226(6) 0.2638(5) 0.056 Uiso 1 calc R . C31 C 0.1746(8) -0.3594(6) 0.0802(6) 0.061(3) Uani 1 d . . C32 C 0.2032(9) -0.4351(7) 0.0168(6) 0.087(4) Uani 1 d . . H32A H 0.2699(9) -0.4448(7) 0.0323(6) 0.130 Uiso 1 calc R . H32B H 0.2001(9) -0.4119(7) -0.0292(6) 0.130 Uiso 1 calc R . H32C H 0.1579(9) -0.4967(7) 0.0071(6) 0.130 Uiso 1 calc R . C33 C 0.1911(10) -0.3972(7) 0.1533(6) 0.104(5) Uani 1 d . . H33A H 0.1357(10) -0.4475(7) 0.1524(6) 0.156 Uiso 1 calc R . H33B H 0.1964(10) -0.3432(7) 0.1979(6) 0.156 Uiso 1 calc R . H33C H 0.2514(10) -0.4243(7) 0.1554(6) 0.156 Uiso 1 calc R . C34 C 0.0678(8) -0.3500(9) 0.0559(8) 0.099(4) Uani 1 d . . H34A H 0.0538(8) -0.2906(9) 0.0876(8) 0.149 Uiso 1 calc R . H34B H 0.0239(8) -0.4062(9) 0.0617(8) 0.149 Uiso 1 calc R . H34C H 0.0578(8) -0.3473(9) 0.0030(8) 0.149 Uiso 1 calc R . C35 C -0.0420(8) 0.3776(10) 0.2827(7) 0.087(4) Uani 1 d . . C36 C -0.1245(9) 0.3800(10) 0.2217(7) 0.120(6) Uani 1 d . . H36A H -0.1002(9) 0.4216(10) 0.1905(7) 0.179 Uiso 1 calc R . H36B H -0.1774(9) 0.4057(10) 0.2452(7) 0.179 Uiso 1 calc R . H36C H -0.1493(9) 0.3141(10) 0.1902(7) 0.179 Uiso 1 calc R . C37 C 0.0128(10) 0.4833(10) 0.3275(9) 0.143(7) Uani 1 d . . H37A H 0.0277(10) 0.4860(10) 0.3813(9) 0.215 Uiso 1 calc R . H37B H -0.0291(10) 0.5306(10) 0.3202(9) 0.215 Uiso 1 calc R . H37C H 0.0737(10) 0.4985(10) 0.3085(9) 0.215 Uiso 1 calc R . C38 C -0.0936(13) 0.3308(14) 0.3425(10) 0.177(8) Uani 1 d . . H38A H -0.1333(13) 0.2675(14) 0.3163(10) 0.265 Uiso 1 calc R . H38B H -0.1355(13) 0.3739(14) 0.3659(10) 0.265 Uiso 1 calc R . H38C H -0.0434(13) 0.3227(14) 0.3815(10) 0.265 Uiso 1 calc R . B B 0.5941(8) 0.6873(7) 0.3529(6) 0.043(3) Uani 1 d . . C101 C 0.6563(7) 0.6297(6) 0.4072(4) 0.045(2) Uani 1 d . . C102 C 0.7579(7) 0.6428(7) 0.4223(5) 0.054(2) Uani 1 d . . H102 H 0.7943(7) 0.6904(7) 0.4038(5) 0.064 Uiso 1 calc R . C103 C 0.8096(8) 0.5891(8) 0.4636(5) 0.061(3) Uani 1 d . . H103 H 0.8790(8) 0.6014(8) 0.4722(5) 0.073 Uiso 1 calc R . C104 C 0.7598(9) 0.5181(7) 0.4919(5) 0.056(3) Uani 1 d . . H104 H 0.7950(9) 0.4813(7) 0.5187(5) 0.068 Uiso 1 calc R . C105 C 0.6586(8) 0.5013(6) 0.4806(5) 0.050(2) Uani 1 d . . H105 H 0.6246(8) 0.4536(6) 0.5005(5) 0.060 Uiso 1 calc R . C106 C 0.6044(8) 0.5560(6) 0.4388(5) 0.051(2) Uani 1 d . . H106 H 0.5351(8) 0.5444(6) 0.4317(5) 0.061 Uiso 1 calc R . C201 C 0.6585(7) 0.8001(7) 0.3641(5) 0.048(2) Uani 1 d . . C202 C 0.6833(7) 0.8400(7) 0.3033(5) 0.055(3) Uani 1 d . . H202 H 0.6641(7) 0.8016(7) 0.2529(5) 0.066 Uiso 1 calc R . C203 C 0.7354(8) 0.9345(8) 0.3167(6) 0.066(3) Uani 1 d . . H203 H 0.7471(8) 0.9596(8) 0.2747(6) 0.079 Uiso 1 calc R . C204 C 0.7711(8) 0.9936(8) 0.3898(7) 0.070(3) Uani 1 d . . H204 H 0.8092(8) 1.0561(8) 0.3973(7) 0.084 Uiso 1 calc R . C205 C 0.7493(8) 0.9584(7) 0.4506(6) 0.068(3) Uani 1 d . . H205 H 0.7696(8) 0.9977(7) 0.5005(6) 0.081 Uiso 1 calc R . C206 C 0.6963(8) 0.8630(8) 0.4375(6) 0.063(3) Uani 1 d . . H206 H 0.6851(8) 0.8392(8) 0.4801(6) 0.076 Uiso 1 calc R . C301 C 0.5818(7) 0.6220(7) 0.2627(5) 0.049(2) Uani 1 d . . C302 C 0.5143(7) 0.6377(7) 0.2023(5) 0.055(2) Uani 1 d . . H302 H 0.4751(7) 0.6860(7) 0.2140(5) 0.066 Uiso 1 calc R . C303 C 0.5046(8) 0.5842(7) 0.1271(5) 0.060(3) Uani 1 d . . H303 H 0.4584(8) 0.5973(7) 0.0901(5) 0.072 Uiso 1 calc R . C304 C 0.5586(9) 0.5142(8) 0.1048(6) 0.072(3) Uani 1 d . . H304 H 0.5515(9) 0.4794(8) 0.0536(6) 0.086 Uiso 1 calc R . C305 C 0.6248(10) 0.4960(9) 0.1608(6) 0.097(4) Uani 1 d . . H305 H 0.6629(10) 0.4471(9) 0.1474(6) 0.116 Uiso 1 calc R . C306 C 0.6367(9) 0.5496(8) 0.2382(5) 0.076(3) Uani 1 d . . H306 H 0.6834(9) 0.5356(8) 0.2744(5) 0.092 Uiso 1 calc R . C401 C 0.4808(7) 0.6945(7) 0.3724(5) 0.047(2) Uani 1 d . . C402 C 0.4550(8) 0.7765(8) 0.4207(5) 0.059(3) Uani 1 d . . H402 H 0.5039(8) 0.8323(8) 0.4423(5) 0.071 Uiso 1 calc R . C403 C 0.3602(9) 0.7779(9) 0.4374(6) 0.074(3) Uani 1 d . . H403 H 0.3466(9) 0.8341(9) 0.4699(6) 0.088 Uiso 1 calc R . C404 C 0.2844(9) 0.6962(11) 0.4061(7) 0.081(4) Uani 1 d . . H404 H 0.2208(9) 0.6977(11) 0.4183(7) 0.097 Uiso 1 calc R . C405 C 0.3042(9) 0.6126(9) 0.3568(6) 0.075(3) Uani 1 d . . C406 C 0.4026(6) 0.6171(6) 0.3444(5) 0.059(3) Uani 1 d . . H406 H 0.4170(6) 0.5603(6) 0.3131(5) 0.071 Uiso 1 calc R . O2 O -0.0259(6) 0.0875(6) -0.1483(5) 0.105(5) Uiso 0.50 d PR . C39 C -0.0073(6) 0.0461(6) -0.2256(5) 0.156(13) Uiso 0.50 d PR . O3 O 0.9742(6) 1.1876(6) 0.5150(5) 0.214(12) Uiso 0.50 d PR . C40 C 1.0424(6) 1.1305(6) 0.4710(5) 0.193(17) Uiso 0.50 d PR . 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 0.0783(9) 0.0276(6) 0.0642(8) 0.0215(5) 0.0404(7) 0.0239(6) Ni2 0.0656(9) 0.0287(6) 0.0334(6) 0.0027(5) 0.0039(6) 0.0162(6) S1 0.061(2) 0.0257(11) 0.0423(13) 0.0071(9) 0.0187(12) 0.0037(10) S2 0.075(2) 0.0453(14) 0.064(2) 0.0129(12) 0.0229(15) 0.0244(13) N1 0.043(5) 0.030(4) 0.056(5) 0.015(3) 0.001(4) 0.011(3) N2 0.060(5) 0.036(4) 0.049(4) 0.019(3) 0.018(4) 0.018(4) N3 0.072(6) 0.052(5) 0.089(7) 0.033(5) 0.039(5) 0.017(4) N4 0.057(5) 0.051(5) 0.047(5) -0.001(4) 0.004(4) 0.026(4) N5 0.062(5) 0.030(4) 0.058(5) 0.006(4) 0.009(4) 0.011(4) N6 0.064(5) 0.032(4) 0.042(4) 0.010(3) 0.016(4) 0.019(4) C1 0.047(5) 0.023(4) 0.043(5) 0.005(4) 0.015(4) 0.015(4) C2 0.048(6) 0.026(4) 0.042(5) 0.012(4) 0.013(4) 0.016(4) C3 0.058(6) 0.025(4) 0.053(6) 0.007(4) 0.000(5) 0.009(4) C4 0.052(6) 0.025(4) 0.072(7) 0.017(5) 0.012(5) 0.011(4) C5 0.059(6) 0.026(4) 0.046(5) 0.015(4) 0.004(5) 0.009(4) C6 0.048(6) 0.025(4) 0.044(5) 0.014(4) 0.013(4) 0.015(4) C7 0.060(6) 0.032(5) 0.040(5) 0.005(4) 0.001(5) 0.016(4) C8 0.077(8) 0.055(6) 0.086(8) 0.036(6) -0.001(6) 0.021(6) C9 0.097(8) 0.046(6) 0.042(6) 0.017(5) 0.022(6) 0.029(6) C10 0.076(7) 0.045(6) 0.055(6) 0.018(5) 0.033(5) 0.024(5) C11 0.080(8) 0.059(6) 0.076(7) 0.044(6) 0.031(6) 0.015(6) C12 0.081(8) 0.047(6) 0.067(7) 0.035(5) 0.030(6) 0.033(5) C13 0.086(9) 0.052(6) 0.073(8) 0.014(5) -0.002(7) 0.037(6) C14 0.134(11) 0.032(6) 0.135(11) 0.023(6) 0.057(9) 0.043(7) C15 0.080(8) 0.071(7) 0.056(7) 0.013(5) 0.022(6) 0.027(6) C16 0.076(8) 0.065(7) 0.073(8) 0.018(6) 0.022(7) 0.026(6) C17 0.072(8) 0.077(7) 0.053(6) 0.016(6) 0.007(6) 0.033(6) C18 0.094(9) 0.081(8) 0.049(6) 0.008(6) 0.012(6) 0.043(7) C19 0.096(10) 0.136(11) 0.053(7) -0.006(7) 0.012(7) 0.078(9) C20 0.066(8) 0.117(10) 0.055(7) -0.040(7) -0.007(6) 0.056(7) C21 0.082(9) 0.122(11) 0.070(8) -0.011(7) -0.007(7) 0.072(8) C22 0.082(9) 0.086(8) 0.062(7) 0.002(6) 0.015(7) 0.036(7) C23 0.120(10) 0.058(7) 0.056(6) -0.008(5) -0.008(7) 0.056(7) C24 0.086(8) 0.065(7) 0.031(5) -0.014(5) -0.013(5) 0.045(6) C25 0.071(8) 0.046(6) 0.085(8) -0.010(6) -0.028(7) 0.022(6) C26 0.072(8) 0.061(7) 0.098(9) 0.021(7) 0.013(7) -0.002(6) C27 0.061(7) 0.048(6) 0.048(6) -0.002(5) -0.007(5) 0.013(5) C28 0.049(6) 0.046(6) 0.045(5) 0.004(4) -0.011(5) 0.005(5) C29 0.099(8) 0.061(7) 0.046(6) 0.020(5) 0.026(6) 0.019(6) C30 0.054(6) 0.043(5) 0.044(5) 0.009(4) 0.007(5) 0.019(5) C31 0.077(8) 0.026(5) 0.080(7) 0.017(5) 0.009(6) 0.003(5) C32 0.140(11) 0.029(5) 0.077(8) 0.005(5) -0.006(8) 0.001(6) C33 0.178(13) 0.037(6) 0.095(9) 0.034(6) 0.031(9) -0.022(7) C34 0.060(8) 0.073(8) 0.160(13) 0.045(9) 0.000(8) -0.014(6) C35 0.045(7) 0.122(11) 0.078(8) -0.019(8) 0.001(6) 0.043(7) C36 0.092(10) 0.153(13) 0.096(10) -0.021(9) -0.014(8) 0.076(10) C37 0.118(12) 0.110(12) 0.171(15) -0.046(11) 0.017(11) 0.058(10) C38 0.190(18) 0.242(23) 0.163(16) 0.076(16) 0.080(15) 0.163(17) B 0.056(7) 0.039(6) 0.039(6) 0.015(5) 0.008(5) 0.014(5) C101 0.061(7) 0.044(5) 0.031(5) 0.002(4) 0.006(5) 0.022(5) C102 0.051(7) 0.056(6) 0.056(6) 0.014(5) 0.012(5) 0.012(5) C103 0.055(7) 0.078(8) 0.053(6) 0.011(6) 0.006(5) 0.037(6) C104 0.083(8) 0.050(6) 0.035(5) 0.002(4) 0.006(6) 0.028(6) C105 0.076(8) 0.046(5) 0.030(5) 0.011(4) 0.005(5) 0.019(5) C106 0.076(7) 0.039(5) 0.035(5) 0.003(4) 0.001(5) 0.019(5) C201 0.052(6) 0.051(6) 0.046(6) 0.014(5) 0.008(5) 0.017(5) C202 0.071(7) 0.053(6) 0.053(6) 0.026(5) 0.023(5) 0.017(5) C203 0.079(8) 0.066(7) 0.067(7) 0.035(6) 0.021(6) 0.026(6) C204 0.064(8) 0.047(6) 0.099(9) 0.025(7) 0.006(7) 0.004(5) C205 0.076(8) 0.048(6) 0.066(7) 0.004(5) -0.006(6) 0.000(6) C206 0.079(8) 0.063(7) 0.051(6) 0.015(5) 0.017(6) 0.021(6) C301 0.061(6) 0.046(5) 0.040(5) 0.016(4) 0.002(5) 0.011(5) C302 0.057(7) 0.055(6) 0.057(6) 0.024(5) 0.005(5) 0.012(5) C303 0.086(8) 0.049(6) 0.040(6) 0.018(5) -0.001(6) -0.001(6) C304 0.119(10) 0.056(7) 0.035(6) 0.014(5) -0.002(6) 0.010(7) C305 0.148(12) 0.084(9) 0.060(8) -0.005(7) 0.019(8) 0.063(9) C306 0.108(9) 0.088(8) 0.043(6) 0.011(6) 0.011(6) 0.063(7) C401 0.060(6) 0.055(6) 0.043(5) 0.031(5) 0.017(5) 0.026(5) C402 0.070(7) 0.070(7) 0.055(6) 0.035(5) 0.019(6) 0.033(6) C403 0.092(9) 0.090(9) 0.070(8) 0.042(7) 0.040(7) 0.059(8) C404 0.060(8) 0.128(12) 0.084(9) 0.075(9) 0.019(7) 0.034(8) C405 0.085(9) 0.097(9) 0.069(8) 0.049(7) 0.021(7) 0.046(7) C406 0.061(7) 0.059(7) 0.072(7) 0.032(6) 0.016(6) 0.024(6) _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. ; #BOND LENGHTS AND ANGLES 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 O1 2.073(6) . ? Ni1 N2 2.148(7) . ? Ni1 N3 2.152(8) . ? Ni1 N1 2.398(7) . ? Ni1 S1 2.447(3) . ? Ni1 S2 2.460(3) . ? Ni2 O1 2.102(6) . ? Ni2 N5 2.154(8) . ? Ni2 N4 2.175(7) . ? Ni2 N6 2.373(6) . ? Ni2 S2 2.383(3) . ? Ni2 S1 2.472(2) . ? S1 C1 1.754(8) . ? S2 C17 1.757(10) . ? N1 C8 1.455(11) . ? N1 C9 1.474(10) . ? N1 C7 1.481(9) . ? N2 C12 1.465(10) . ? N2 C11 1.472(11) . ? N2 C10 1.481(10) . ? N3 C15 1.464(12) . ? N3 C14 1.475(12) . ? N3 C13 1.486(12) . ? N4 C22 1.442(12) . ? N4 C24 1.468(10) . ? N4 C23 1.506(11) . ? N5 C26 1.425(11) . ? N5 C27 1.474(10) . ? N5 C25 1.502(11) . ? N6 C30 1.503(9) . ? N6 C28 1.498(10) . ? N6 C29 1.513(11) . ? C1 C2 1.401(10) . ? C1 C6 1.426(10) . ? C2 C3 1.386(11) . ? C2 C7 1.524(11) . ? C3 C4 1.402(11) . ? C4 C5 1.390(11) . ? C4 C31 1.556(12) . ? C5 C6 1.382(11) . ? C6 C30 1.490(11) . ? C9 C10 1.460(12) . ? C12 C13 1.553(13) . ? C15 C16 1.543(13) . ? C16 C21 1.415(13) . ? C16 C17 1.430(13) . ? C17 C18 1.418(13) . ? C18 C19 1.411(13) . ? C18 C22 1.557(14) . ? C19 C20 1.376(14) . ? C20 C21 1.380(14) . ? C20 C35 1.491(13) . ? C24 C25 1.517(14) . ? C27 C28 1.491(12) . ? C31 C32 1.511(13) . ? C31 C34 1.509(14) . ? C31 C33 1.537(14) . ? C35 C36 1.486(14) . ? C35 C37 1.55(2) . ? C35 C38 1.58(2) . ? B C101 1.642(12) . ? B C401 1.651(13) . ? B C301 1.654(13) . ? B C201 1.661(13) . ? C101 C102 1.365(12) . ? C101 C106 1.443(12) . ? C102 C103 1.382(12) . ? C103 C104 1.365(13) . ? C104 C105 1.357(12) . ? C105 C106 1.415(11) . ? C201 C206 1.403(12) . ? C201 C202 1.404(12) . ? C202 C203 1.373(13) . ? C203 C204 1.377(13) . ? C204 C205 1.356(14) . ? C205 C206 1.389(13) . ? C301 C306 1.379(12) . ? C301 C302 1.417(11) . ? C302 C303 1.377(12) . ? C303 C304 1.337(13) . ? C304 C305 1.365(14) . ? C305 C306 1.408(13) . ? C401 C406 1.370(12) . ? C401 C402 1.400(12) . ? C402 C403 1.375(13) . ? C403 C404 1.39(2) . ? C404 C405 1.39(2) . ? C405 C406 1.393(13) . ? O2 C39 1.46 . ? O3 C40 1.51 . ? 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 O1 Ni1 N2 99.5(3) . . ? O1 Ni1 N3 90.1(3) . . ? N2 Ni1 N3 83.2(3) . . ? O1 Ni1 N1 167.1(2) . . ? N2 Ni1 N1 78.4(3) . . ? N3 Ni1 N1 102.2(3) . . ? O1 Ni1 S1 80.1(2) . . ? N2 Ni1 S1 103.0(2) . . ? N3 Ni1 S1 169.2(2) . . ? N1 Ni1 S1 87.9(2) . . ? O1 Ni1 S2 81.2(2) . . ? N2 Ni1 S2 175.4(2) . . ? N3 Ni1 S2 92.3(2) . . ? N1 Ni1 S2 101.9(2) . . ? S1 Ni1 S2 81.62(9) . . ? O1 Ni2 N5 98.7(3) . . ? O1 Ni2 N4 91.9(3) . . ? N5 Ni2 N4 83.4(3) . . ? O1 Ni2 N6 166.7(2) . . ? N5 Ni2 N6 79.3(3) . . ? N4 Ni2 N6 100.9(3) . . ? O1 Ni2 S2 82.6(2) . . ? N5 Ni2 S2 176.2(2) . . ? N4 Ni2 S2 93.0(2) . . ? N6 Ni2 S2 100.3(2) . . ? O1 Ni2 S1 79.0(2) . . ? N5 Ni2 S1 101.0(2) . . ? N4 Ni2 S1 170.3(2) . . ? N6 Ni2 S1 88.4(2) . . ? S2 Ni2 S1 82.68(9) . . ? C1 S1 Ni1 102.4(3) . . ? C1 S1 Ni2 102.8(3) . . ? Ni1 S1 Ni2 76.25(8) . . ? C17 S2 Ni2 103.3(4) . . ? C17 S2 Ni1 103.4(4) . . ? Ni2 S2 Ni1 77.67(9) . . ? Ni2 O1 Ni1 93.3(3) . . ? C8 N1 C9 111.0(7) . . ? C8 N1 C7 107.9(6) . . ? C9 N1 C7 104.0(6) . . ? C8 N1 Ni1 116.6(6) . . ? C9 N1 Ni1 105.2(5) . . ? C7 N1 Ni1 111.4(5) . . ? C12 N2 C11 108.3(7) . . ? C12 N2 C10 110.8(7) . . ? C11 N2 C10 108.6(7) . . ? C12 N2 Ni1 109.8(5) . . ? C11 N2 Ni1 110.8(5) . . ? C10 N2 Ni1 108.5(5) . . ? C15 N3 C14 108.2(8) . . ? C15 N3 C13 110.8(8) . . ? C14 N3 C13 107.4(8) . . ? C15 N3 Ni1 111.4(6) . . ? C14 N3 Ni1 116.1(7) . . ? C13 N3 Ni1 102.8(6) . . ? C22 N4 C24 110.1(8) . . ? C22 N4 C23 108.0(8) . . ? C24 N4 C23 110.0(7) . . ? C22 N4 Ni2 111.5(6) . . ? C24 N4 Ni2 103.0(5) . . ? C23 N4 Ni2 114.2(6) . . ? C26 N5 C27 108.5(8) . . ? C26 N5 C25 108.8(8) . . ? C27 N5 C25 108.8(7) . . ? C26 N5 Ni2 115.2(6) . . ? C27 N5 Ni2 108.7(5) . . ? C25 N5 Ni2 106.7(6) . . ? C30 N6 C28 105.4(6) . . ? C30 N6 C29 106.5(7) . . ? C28 N6 C29 111.4(7) . . ? C30 N6 Ni2 112.2(5) . . ? C28 N6 Ni2 105.0(5) . . ? C29 N6 Ni2 115.8(5) . . ? C2 C1 C6 117.6(7) . . ? C2 C1 S1 121.9(6) . . ? C6 C1 S1 120.5(6) . . ? C3 C2 C1 121.5(7) . . ? C3 C2 C7 120.7(8) . . ? C1 C2 C7 117.5(7) . . ? C2 C3 C4 121.1(8) . . ? C5 C4 C3 117.3(8) . . ? C5 C4 C31 124.9(8) . . ? C3 C4 C31 117.8(8) . . ? C6 C5 C4 123.0(8) . . ? C5 C6 C1 119.5(8) . . ? C5 C6 C30 120.4(7) . . ? C1 C6 C30 119.7(7) . . ? N1 C7 C2 113.8(7) . . ? C10 C9 N1 110.7(8) . . ? C9 C10 N2 113.5(7) . . ? N2 C12 C13 110.2(7) . . ? N3 C13 C12 111.1(8) . . ? N3 C15 C16 110.8(9) . . ? C21 C16 C17 121.5(10) . . ? C21 C16 C15 116.9(10) . . ? C17 C16 C15 120.8(9) . . ? C18 C17 C16 115.8(9) . . ? C18 C17 S2 122.8(8) . . ? C16 C17 S2 121.2(8) . . ? C19 C18 C17 120.2(10) . . ? C19 C18 C22 120.0(9) . . ? C17 C18 C22 119.2(9) . . ? C20 C19 C18 123.1(10) . . ? C21 C20 C19 117.5(9) . . ? C21 C20 C35 120.4(10) . . ? C19 C20 C35 122.1(10) . . ? C20 C21 C16 121.1(10) . . ? N4 C22 C18 110.8(9) . . ? N4 C24 C25 110.0(8) . . ? N5 C25 C24 113.6(8) . . ? N5 C27 C28 112.7(8) . . ? C27 C28 N6 110.1(7) . . ? C6 C30 N6 115.9(7) . . ? C32 C31 C34 108.1(9) . . ? C32 C31 C33 106.2(8) . . ? C34 C31 C33 113.6(10) . . ? C32 C31 C4 109.6(8) . . ? C34 C31 C4 109.0(8) . . ? C33 C31 C4 110.2(8) . . ? C20 C35 C36 115.4(10) . . ? C20 C35 C37 108.3(10) . . ? C36 C35 C37 112.0(12) . . ? C20 C35 C38 108.6(12) . . ? C36 C35 C38 105.6(11) . . ? C37 C35 C38 106.5(11) . . ? C101 B C401 112.8(7) . . ? C101 B C301 107.2(7) . . ? C401 B C301 107.3(8) . . ? C101 B C201 108.8(7) . . ? C401 B C201 110.1(7) . . ? C301 B C201 110.5(7) . . ? C102 C101 C106 115.4(8) . . ? C102 C101 B 123.9(8) . . ? C106 C101 B 120.7(8) . . ? C101 C102 C103 123.5(9) . . ? C104 C103 C102 120.6(10) . . ? C105 C104 C103 119.8(9) . . ? C104 C105 C106 120.4(9) . . ? C105 C106 C101 120.3(9) . . ? C206 C201 C202 114.1(9) . . ? C206 C201 B 121.6(8) . . ? C202 C201 B 124.3(8) . . ? C203 C202 C201 121.3(9) . . ? C204 C203 C202 122.6(10) . . ? C205 C204 C203 118.4(10) . . ? C204 C205 C206 119.4(10) . . ? C205 C206 C201 124.2(9) . . ? C306 C301 C302 113.4(8) . . ? C306 C301 B 124.2(8) . . ? C302 C301 B 122.3(8) . . ? C303 C302 C301 122.5(9) . . ? C304 C303 C302 122.9(10) . . ? C303 C304 C305 117.0(9) . . ? C304 C305 C306 121.5(10) . . ? C301 C306 C305 122.7(10) . . ? C406 C401 C402 113.1(9) . . ? C406 C401 B 122.2(8) . . ? C402 C401 B 124.6(9) . . ? C403 C402 C401 122.6(11) . . ? C402 C403 C404 120.8(11) . . ? C403 C404 C405 119.7(11) . . ? C406 C405 C404 115.5(11) . . ? C401 C406 C405 128.2(9) . . ? #===END