# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Darensbourg, Marcetta' _publ_contact_author_email MARCETTA@MAIL.CHEM.TAMU.EDU loop_ _publ_author_name M.Darensbourg C.-H.Hsieh M.Hall S.Brothers data_mm _database_code_depnum_ccdc_archive 'CCDC 817758' #TrackingRef '- Ni2Fe3NO6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common NiFe _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H42 Fe3 N10 Ni2 O7 S4' _chemical_formula_weight 971.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.205(2) _cell_length_b 20.135(4) _cell_length_c 35.578(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7310(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 839 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 56.89 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 13.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5615 _exptl_absorpt_correction_T_max 0.7803 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53902 _diffrn_reflns_av_R_equivalents 0.2010 _diffrn_reflns_av_sigmaI/netI 0.1245 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 59.32 _reflns_number_total 5292 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker APEX' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The included THF solvent molecule was found to be disordered between two positions and modeled with bond restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+64.6296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5292 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.2057 _refine_ls_wR_factor_gt 0.1883 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.46331(18) 0.41153(8) 0.05346(5) 0.0225(5) Uani 1 1 d . . . Ni2 Ni 0.7768(2) 0.53241(9) 0.15043(5) 0.0292(5) Uani 1 1 d . . . Fe1 Fe 0.4708(2) 0.58124(9) 0.12501(5) 0.0329(5) Uani 1 1 d . . . Fe2 Fe 0.5365(2) 0.39968(9) 0.14390(5) 0.0302(5) Uani 1 1 d . . . Fe3 Fe 0.83378(17) 0.42635(9) 0.06764(5) 0.0261(5) Uani 1 1 d . . . S1 S 0.4377(3) 0.47416(14) 0.10287(8) 0.0272(7) Uani 1 1 d . . . S2 S 0.6474(3) 0.45345(13) 0.03419(7) 0.0239(7) Uani 1 1 d . . . S3 S 0.7424(3) 0.43530(13) 0.12645(8) 0.0267(7) Uani 1 1 d . . . S4 S 0.6868(3) 0.58601(14) 0.10452(8) 0.0313(8) Uani 1 1 d . . . O1 O 0.2906(12) 0.6703(5) 0.0924(3) 0.073(3) Uani 1 1 d . . . O2 O 0.4498(12) 0.5960(5) 0.2042(3) 0.070(3) Uani 1 1 d . . . O3 O 0.4882(11) 0.4289(5) 0.2203(3) 0.065(3) Uani 1 1 d . . . O4 O 0.5101(10) 0.2637(5) 0.1257(3) 0.058(3) Uani 1 1 d . . . O5 O 1.0131(9) 0.5331(5) 0.0567(3) 0.056(3) Uani 1 1 d . . . O6 O 0.9314(9) 0.2947(4) 0.0575(2) 0.044(2) Uani 1 1 d . . . N1 N 0.3706(13) 0.6315(5) 0.1023(3) 0.049(3) Uani 1 1 d . . . N2 N 0.4631(12) 0.5844(5) 0.1705(3) 0.051(3) Uani 1 1 d . . . N3 N 0.5036(11) 0.4217(5) 0.1876(3) 0.044(3) Uani 1 1 d . . . N4 N 0.5244(11) 0.3231(5) 0.1309(3) 0.041(3) Uani 1 1 d . . . N5 N 0.9342(10) 0.4887(5) 0.0614(3) 0.037(3) Uani 1 1 d . . . N6 N 0.8816(9) 0.3485(5) 0.0617(3) 0.029(2) Uani 1 1 d . . . N7 N 0.2870(9) 0.3748(5) 0.0619(3) 0.031(2) Uani 1 1 d . . . N8 N 0.4701(10) 0.3450(4) 0.0152(2) 0.028(2) Uani 1 1 d . . . N9 N 0.8214(11) 0.6143(5) 0.1763(3) 0.039(3) Uani 1 1 d . . . N10 N 0.8650(10) 0.4928(5) 0.1932(3) 0.033(3) Uani 1 1 d . . . C18 C 0.7419(15) 0.6681(6) 0.1189(3) 0.044(4) Uani 1 1 d . . . C12 C 0.8125(13) 0.5292(6) 0.2263(3) 0.037(3) Uani 1 1 d . . . C5 C 0.2083(12) 0.4031(6) 0.0302(3) 0.039(3) Uani 1 1 d . . . H18A H 0.8303 0.6769 0.1085 0.052 Uiso 1 1 calc R . . H18B H 0.6812 0.7023 0.1091 0.052 Uiso 1 1 calc R . . H12A H 0.8740 0.5248 0.2477 0.045 Uiso 1 1 calc R . . H12B H 0.7274 0.5097 0.2339 0.045 Uiso 1 1 calc R . . H5A H 0.2267 0.4512 0.0279 0.047 Uiso 1 1 calc R . . H5B H 0.1138 0.3976 0.0357 0.047 Uiso 1 1 calc R . . C10 C 0.8523(12) 0.3889(6) 0.1583(3) 0.032(3) Uani 1 1 d . . . H10A H 0.8264 0.3415 0.1593 0.039 Uiso 1 1 calc R . . H10B H 0.9440 0.3917 0.1493 0.039 Uiso 1 1 calc R . . C3 C 0.2987(12) 0.3011(6) 0.0589(3) 0.035(3) Uani 1 1 d . . . H3A H 0.2156 0.2823 0.0492 0.042 Uiso 1 1 calc R . . H3B H 0.3154 0.2818 0.0840 0.042 Uiso 1 1 calc R . . C8 C 0.6028(12) 0.3344(6) 0.0006(3) 0.035(3) Uani 1 1 d . . . H8A H 0.5991 0.3073 -0.0226 0.042 Uiso 1 1 calc R . . H8B H 0.6562 0.3104 0.0194 0.042 Uiso 1 1 calc R . . C6 C 0.2405(13) 0.3689(6) -0.0068(3) 0.039(3) Uani 1 1 d . . . H6A H 0.2071 0.3228 -0.0057 0.047 Uiso 1 1 calc R . . H6B H 0.1930 0.3920 -0.0272 0.047 Uiso 1 1 calc R . . C11 C 0.8397(13) 0.4201(6) 0.1963(3) 0.037(3) Uani 1 1 d . . . H11A H 0.7505 0.4124 0.2064 0.044 Uiso 1 1 calc R . . H11B H 0.9035 0.3998 0.2139 0.044 Uiso 1 1 calc R . . C7 C 0.3824(12) 0.3667(6) -0.0167(3) 0.029(3) Uani 1 1 d . . . H7A H 0.4147 0.3780 -0.0409 0.035 Uiso 1 1 calc R . . C4 C 0.4117(13) 0.2833(5) 0.0321(4) 0.038(3) Uani 1 1 d . . . H4A H 0.4802 0.2588 0.0462 0.046 Uiso 1 1 calc R . . H4B H 0.3788 0.2540 0.0119 0.046 Uiso 1 1 calc R . . C13 C 0.7939(15) 0.6023(6) 0.2169(4) 0.048(4) Uani 1 1 d . . . H13A H 0.7029 0.6158 0.2227 0.057 Uiso 1 1 calc R . . H13B H 0.8538 0.6296 0.2324 0.057 Uiso 1 1 calc R . . C9 C 0.6649(12) 0.4019(6) -0.0079(3) 0.032(3) Uani 1 1 d . . . H9A H 0.6203 0.4231 -0.0295 0.038 Uiso 1 1 calc R . . H9B H 0.7588 0.3963 -0.0143 0.038 Uiso 1 1 calc R . . C1 C 0.2608(11) 0.4625(6) 0.1088(3) 0.036(3) Uani 1 1 d . . . H1A H 0.2356 0.4712 0.1353 0.043 Uiso 1 1 calc R . . H1B H 0.2122 0.4937 0.0925 0.043 Uiso 1 1 calc R . . C15 C 1.0471(15) 0.5755(6) 0.1931(5) 0.058(4) Uani 1 1 d . . . H15A H 1.1403 0.5810 0.1860 0.070 Uiso 1 1 calc R . . H15B H 1.0392 0.5868 0.2201 0.070 Uiso 1 1 calc R . . C14 C 1.0109(13) 0.5036(6) 0.1882(4) 0.047(4) Uani 1 1 d . . . H14A H 1.0590 0.4765 0.2069 0.056 Uiso 1 1 calc R . . H14B H 1.0374 0.4887 0.1629 0.056 Uiso 1 1 calc R . . C16 C 0.9647(14) 0.6256(7) 0.1703(4) 0.056(4) Uani 1 1 d . . . H16A H 1.0004 0.6591 0.1546 0.067 Uiso 1 1 calc R . . C17 C 0.7461(16) 0.6710(6) 0.1620(4) 0.050(4) Uani 1 1 d . . . H17A H 0.7875 0.7130 0.1703 0.060 Uiso 1 1 calc R . . H17B H 0.6558 0.6696 0.1722 0.060 Uiso 1 1 calc R . . C2 C 0.2282(14) 0.3924(7) 0.0985(3) 0.045(4) Uani 1 1 d . . . H2A H 0.2616 0.3620 0.1182 0.054 Uiso 1 1 calc R . . H2B H 0.1319 0.3872 0.0971 0.054 Uiso 1 1 calc R . . O7 O 0.6271(13) 0.3352(7) 0.3151(4) 0.098(4) Uani 1 1 d . . . C19 C 0.6083(18) 0.2678(8) 0.3236(5) 0.076(5) Uani 1 1 d . . . H19A H 0.5354 0.2491 0.3085 0.092 Uiso 1 1 calc R . . H19B H 0.5884 0.2617 0.3506 0.092 Uiso 1 1 calc R . . C21 C 0.793(2) 0.2738(10) 0.2804(8) 0.118(8) Uani 1 1 d . . . H21A H 0.8830 0.2898 0.2854 0.141 Uiso 1 1 calc R . . H21B H 0.7923 0.2477 0.2568 0.141 Uiso 1 1 calc R . . C20 C 0.7403(19) 0.2335(9) 0.3132(6) 0.091(6) Uani 1 1 d . . . H20A H 0.8020 0.2346 0.3346 0.109 Uiso 1 1 calc R . . H20B H 0.7258 0.1867 0.3057 0.109 Uiso 1 1 calc R . . C22 C 0.700(2) 0.3290(15) 0.2787(8) 0.22(2) Uani 1 1 d . . . H22A H 0.6369 0.3214 0.2580 0.263 Uiso 1 1 calc R . . H22B H 0.7475 0.3708 0.2735 0.263 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0230(11) 0.0223(10) 0.0221(10) -0.0017(9) -0.0021(8) 0.0001(8) Ni2 0.0366(13) 0.0295(11) 0.0214(10) -0.0014(9) -0.0054(9) -0.0002(9) Fe1 0.0481(13) 0.0273(10) 0.0234(10) -0.0024(9) 0.0030(9) 0.0102(10) Fe2 0.0356(12) 0.0297(11) 0.0252(10) 0.0025(9) 0.0038(9) 0.0027(9) Fe3 0.0220(11) 0.0297(11) 0.0266(10) -0.0025(9) 0.0003(8) 0.0008(8) S1 0.0259(18) 0.0287(16) 0.0272(16) -0.0045(14) 0.0008(13) 0.0062(13) S2 0.0255(17) 0.0259(15) 0.0204(15) -0.0020(13) 0.0003(12) -0.0005(13) S3 0.0308(18) 0.0257(15) 0.0236(15) -0.0024(13) -0.0023(13) 0.0012(13) S4 0.041(2) 0.0271(16) 0.0260(16) 0.0009(14) -0.0054(14) -0.0012(14) O1 0.098(9) 0.072(8) 0.048(6) 0.008(6) -0.004(6) 0.053(7) O2 0.121(10) 0.056(6) 0.033(6) 0.002(5) 0.018(6) 0.006(6) O3 0.096(9) 0.067(7) 0.033(6) 0.002(5) 0.018(6) 0.015(6) O4 0.060(7) 0.039(6) 0.076(7) 0.002(5) -0.012(5) 0.003(5) O5 0.022(5) 0.050(6) 0.097(8) 0.014(6) -0.013(5) -0.008(5) O6 0.044(6) 0.039(5) 0.048(6) 0.000(5) 0.004(4) 0.004(5) N1 0.081(10) 0.028(6) 0.037(7) 0.000(6) 0.004(6) 0.020(6) N2 0.084(9) 0.050(7) 0.019(6) -0.007(6) 0.010(6) 0.015(7) N3 0.049(8) 0.048(7) 0.035(7) 0.011(6) 0.016(5) 0.016(5) N4 0.053(8) 0.028(6) 0.042(7) 0.009(5) -0.012(6) 0.004(5) N5 0.025(7) 0.043(6) 0.044(7) -0.011(6) -0.008(5) 0.007(5) N6 0.016(6) 0.045(7) 0.026(6) 0.005(5) 0.000(4) 0.002(5) N7 0.026(6) 0.036(6) 0.030(6) 0.000(5) -0.008(5) -0.006(5) N8 0.035(6) 0.022(5) 0.025(5) -0.004(4) -0.014(5) 0.006(5) N9 0.050(8) 0.044(7) 0.022(6) 0.003(5) -0.006(5) -0.005(6) N10 0.043(7) 0.038(6) 0.019(5) -0.002(5) -0.002(5) 0.003(5) C18 0.068(10) 0.040(8) 0.023(7) 0.012(6) -0.014(7) 0.005(7) C12 0.063(10) 0.043(8) 0.006(6) -0.003(6) -0.014(6) 0.008(7) C5 0.024(8) 0.044(8) 0.050(9) 0.002(7) 0.000(6) -0.006(6) C10 0.035(8) 0.036(7) 0.026(7) 0.000(6) -0.009(6) 0.008(6) C3 0.037(8) 0.039(8) 0.029(7) 0.014(6) -0.007(6) -0.025(6) C8 0.033(8) 0.039(8) 0.032(7) -0.026(6) -0.005(6) 0.013(6) C6 0.035(9) 0.039(8) 0.042(8) 0.008(7) 0.000(7) -0.003(6) C11 0.046(9) 0.045(8) 0.020(7) 0.002(6) -0.005(6) 0.008(7) C7 0.037(8) 0.036(7) 0.013(6) -0.004(5) -0.008(6) 0.003(6) C4 0.055(10) 0.018(6) 0.042(8) -0.008(6) -0.016(7) 0.000(6) C13 0.066(10) 0.044(8) 0.034(8) -0.009(7) -0.012(7) 0.002(7) C9 0.029(8) 0.047(8) 0.020(6) -0.004(6) 0.000(5) 0.004(6) C1 0.020(7) 0.056(9) 0.031(7) -0.013(7) 0.005(6) 0.005(6) C15 0.048(10) 0.050(9) 0.078(11) 0.012(8) -0.014(8) -0.013(8) C14 0.034(9) 0.047(9) 0.059(9) 0.001(8) -0.016(7) -0.006(7) C16 0.043(10) 0.051(9) 0.074(11) 0.030(8) -0.019(8) -0.016(8) C17 0.085(12) 0.021(7) 0.045(8) -0.004(7) 0.000(8) -0.006(7) C2 0.036(9) 0.068(10) 0.031(8) 0.009(7) -0.004(6) 0.012(7) O7 0.089(10) 0.095(10) 0.110(11) 0.028(9) 0.010(8) 0.016(8) C19 0.083(14) 0.060(11) 0.086(13) 0.007(10) -0.012(11) -0.005(10) C21 0.074(16) 0.088(15) 0.19(3) 0.023(17) 0.022(16) -0.006(12) C20 0.074(15) 0.075(13) 0.124(17) -0.029(13) -0.021(13) 0.007(11) C22 0.14(2) 0.30(4) 0.22(3) 0.22(3) 0.14(2) 0.14(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N8 1.912(9) . ? Ni1 N7 1.968(10) . ? Ni1 S2 2.171(3) . ? Ni1 S1 2.179(3) . ? Ni2 N10 1.939(9) . ? Ni2 N9 1.942(10) . ? Ni2 S3 2.162(3) . ? Ni2 S4 2.163(3) . ? Fe1 N2 1.623(10) . ? Fe1 N1 1.650(12) . ? Fe1 S1 2.320(3) . ? Fe1 S4 2.323(4) . ? Fe2 N4 1.614(11) . ? Fe2 N3 1.651(11) . ? Fe2 S3 2.305(4) . ? Fe2 S1 2.323(3) . ? Fe3 N5 1.636(11) . ? Fe3 N6 1.656(11) . ? Fe3 S3 2.298(3) . ? Fe3 S2 2.309(3) . ? S1 C1 1.833(12) . ? S2 C9 1.832(11) . ? S3 C10 1.848(11) . ? S4 C18 1.819(13) . ? O1 N1 1.184(13) . ? O2 N2 1.226(13) . ? O3 N3 1.183(13) . ? O5 N5 1.215(12) . ? O6 N6 1.205(11) . ? N4 O4 1.219(12) . ? N7 C2 1.478(15) . ? N7 C3 1.492(15) . ? N7 C5 1.498(15) . ? N8 C8 1.466(15) . ? N8 C4 1.505(15) . ? N8 C7 1.508(14) . ? N9 C17 1.467(16) . ? N9 C13 1.491(16) . ? N9 C16 1.495(17) . ? N10 C11 1.491(15) . ? N10 C14 1.515(16) . ? C18 C17 1.538(17) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C12 N10 1.489(14) . ? C12 C13 1.523(17) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C5 C6 1.521(17) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C10 C11 1.499(15) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C3 C4 1.537(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C8 C9 1.529(16) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C6 C7 1.491(17) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C7 H7A 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C1 C2 1.495(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C15 C14 1.503(17) . ? C15 C16 1.545(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C16 H16A 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O7 C19 1.404(18) . ? O7 C22 1.50(2) . ? C19 C20 1.56(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 C22 1.46(3) . ? C21 C20 1.52(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? 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 N8 Ni1 N7 83.0(4) . . ? N8 Ni1 S2 90.9(3) . . ? N7 Ni1 S2 170.2(3) . . ? N8 Ni1 S1 169.9(3) . . ? N7 Ni1 S1 89.1(3) . . ? S2 Ni1 S1 97.68(12) . . ? N10 Ni2 N9 82.5(4) . . ? N10 Ni2 S3 90.8(3) . . ? N9 Ni2 S3 173.1(3) . . ? N10 Ni2 S4 174.2(3) . . ? N9 Ni2 S4 91.9(3) . . ? S3 Ni2 S4 94.84(13) . . ? N2 Fe1 N1 115.8(5) . . ? N2 Fe1 S1 111.6(4) . . ? N1 Fe1 S1 108.3(4) . . ? N2 Fe1 S4 110.9(5) . . ? N1 Fe1 S4 114.1(4) . . ? S1 Fe1 S4 94.02(12) . . ? N4 Fe2 N3 120.7(5) . . ? N4 Fe2 S3 106.8(4) . . ? N3 Fe2 S3 110.8(4) . . ? N4 Fe2 S1 113.8(4) . . ? N3 Fe2 S1 109.3(4) . . ? S3 Fe2 S1 91.47(12) . . ? N5 Fe3 N6 121.6(5) . . ? N5 Fe3 S3 108.5(4) . . ? N6 Fe3 S3 108.1(3) . . ? N5 Fe3 S2 105.4(4) . . ? N6 Fe3 S2 113.6(3) . . ? S3 Fe3 S2 96.69(12) . . ? C1 S1 Ni1 97.9(4) . . ? C1 S1 Fe1 102.9(4) . . ? Ni1 S1 Fe1 142.57(15) . . ? C1 S1 Fe2 105.8(4) . . ? Ni1 S1 Fe2 94.66(12) . . ? Fe1 S1 Fe2 108.86(13) . . ? C9 S2 Ni1 97.0(4) . . ? C9 S2 Fe3 102.0(4) . . ? Ni1 S2 Fe3 117.27(13) . . ? C10 S3 Ni2 96.7(4) . . ? C10 S3 Fe3 105.8(4) . . ? Ni2 S3 Fe3 111.36(14) . . ? C10 S3 Fe2 103.4(4) . . ? Ni2 S3 Fe2 108.85(14) . . ? Fe3 S3 Fe2 126.22(14) . . ? C18 S4 Ni2 96.3(4) . . ? C18 S4 Fe1 104.1(5) . . ? Ni2 S4 Fe1 98.35(13) . . ? O1 N1 Fe1 167.9(10) . . ? O2 N2 Fe1 170.5(10) . . ? O3 N3 Fe2 170.4(10) . . ? O4 N4 Fe2 171.8(10) . . ? O5 N5 Fe3 177.3(9) . . ? O6 N6 Fe3 172.2(9) . . ? C5 N7 Ni1 103.5(7) . . ? C3 N7 Ni1 106.9(7) . . ? C2 N7 Ni1 114.5(8) . . ? C3 N7 C5 111.5(9) . . ? C2 N7 C5 110.8(9) . . ? C2 N7 C3 109.6(9) . . ? C7 N8 Ni1 108.1(6) . . ? C4 N8 Ni1 106.2(7) . . ? C8 N8 Ni1 112.8(7) . . ? C4 N8 C7 107.8(9) . . ? C8 N8 C7 108.9(9) . . ? C8 N8 C4 112.8(9) . . ? C17 N9 C13 111.2(10) . . ? C17 N9 C16 110.2(10) . . ? C13 N9 C16 110.2(10) . . ? C17 N9 Ni2 112.0(8) . . ? C13 N9 Ni2 106.1(8) . . ? C16 N9 Ni2 107.0(8) . . ? C12 N10 Ni2 104.6(7) . . ? C11 N10 Ni2 112.5(7) . . ? C14 N10 Ni2 107.9(7) . . ? C11 N10 C14 108.7(9) . . ? C12 N10 C14 112.0(10) . . ? C12 N10 C11 111.1(9) . . ? C17 C18 S4 108.9(8) . . ? C17 C18 H18A 109.9 . . ? S4 C18 H18A 109.9 . . ? C17 C18 H18B 109.9 . . ? S4 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? N10 C12 C13 110.2(10) . . ? N10 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? N10 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N7 C5 C6 111.3(10) . . ? N7 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N7 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C11 C10 S3 106.8(8) . . ? C11 C10 H10A 110.4 . . ? S3 C10 H10A 110.4 . . ? C11 C10 H10B 110.4 . . ? S3 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? N7 C3 C4 109.7(9) . . ? N7 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N7 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N8 C8 C9 108.9(9) . . ? N8 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? N8 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C7 C6 C5 115.4(10) . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? N10 C11 C10 109.2(10) . . ? N10 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? N10 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? C6 C7 N8 114.0(10) . . ? C6 C7 H7A 123.0 . . ? N8 C7 H7A 123.0 . . ? N8 C4 C3 110.6(9) . . ? N8 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N8 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N9 C13 C12 110.3(10) . . ? N9 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? N9 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C8 C9 S2 107.5(8) . . ? C8 C9 H9A 110.2 . . ? S2 C9 H9A 110.2 . . ? C8 C9 H9B 110.2 . . ? S2 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C2 C1 S1 108.2(9) . . ? C2 C1 H1A 110.1 . . ? S1 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 . . ? S1 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? C14 C15 C16 115.7(12) . . ? C14 C15 H15A 108.4 . . ? C16 C15 H15A 108.4 . . ? C14 C15 H15B 108.4 . . ? C16 C15 H15B 108.4 . . ? H15A C15 H15B 107.4 . . ? C15 C14 N10 111.5(11) . . ? C15 C14 H14A 109.3 . . ? N10 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? N10 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? N9 C16 C15 111.0(11) . . ? N9 C16 H16A 124.5 . . ? C15 C16 H16A 124.5 . . ? N9 C17 C18 109.2(10) . . ? N9 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? N9 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? N7 C2 C1 110.7(11) . . ? N7 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N7 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C19 O7 C22 99.9(16) . . ? O7 C19 C20 105.0(15) . . ? O7 C19 H19A 110.7 . . ? C20 C19 H19A 110.7 . . ? O7 C19 H19B 110.7 . . ? C20 C19 H19B 110.7 . . ? H19A C19 H19B 108.8 . . ? C22 C21 C20 102.0(17) . . ? C22 C21 H21A 111.4 . . ? C20 C21 H21A 111.4 . . ? C22 C21 H21B 111.4 . . ? C20 C21 H21B 111.4 . . ? H21A C21 H21B 109.2 . . ? C21 C20 C19 104.5(16) . . ? C21 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? C21 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? H20A C20 H20B 108.9 . . ? C21 C22 O7 110.5(17) . . ? C21 C22 H22A 109.6 . . ? O7 C22 H22A 109.6 . . ? C21 C22 H22B 109.6 . . ? O7 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Ni1 S1 C1 -51.8(18) . . . . ? N7 Ni1 S1 C1 -13.2(5) . . . . ? S2 Ni1 S1 C1 159.7(4) . . . . ? N8 Ni1 S1 Fe1 -175.3(17) . . . . ? N7 Ni1 S1 Fe1 -136.8(4) . . . . ? S2 Ni1 S1 Fe1 36.2(3) . . . . ? N8 Ni1 S1 Fe2 54.9(17) . . . . ? N7 Ni1 S1 Fe2 93.4(3) . . . . ? S2 Ni1 S1 Fe2 -93.63(13) . . . . ? N2 Fe1 S1 C1 74.6(6) . . . . ? N1 Fe1 S1 C1 -54.0(6) . . . . ? S4 Fe1 S1 C1 -171.0(4) . . . . ? N2 Fe1 S1 Ni1 -163.3(5) . . . . ? N1 Fe1 S1 Ni1 68.1(5) . . . . ? S4 Fe1 S1 Ni1 -48.9(3) . . . . ? N2 Fe1 S1 Fe2 -37.3(5) . . . . ? N1 Fe1 S1 Fe2 -165.9(4) . . . . ? S4 Fe1 S1 Fe2 77.10(14) . . . . ? N4 Fe2 S1 C1 71.8(6) . . . . ? N3 Fe2 S1 C1 -66.3(6) . . . . ? S3 Fe2 S1 C1 -179.0(4) . . . . ? N4 Fe2 S1 Ni1 -27.7(5) . . . . ? N3 Fe2 S1 Ni1 -165.9(4) . . . . ? S3 Fe2 S1 Ni1 81.41(13) . . . . ? N4 Fe2 S1 Fe1 -178.2(5) . . . . ? N3 Fe2 S1 Fe1 43.7(5) . . . . ? S3 Fe2 S1 Fe1 -69.02(14) . . . . ? N10 Ni2 S3 C10 -11.8(5) . . . . ? N9 Ni2 S3 C10 -1(3) . . . . ? S4 Ni2 S3 C10 166.8(4) . . . . ? N10 Ni2 S3 Fe3 -121.6(3) . . . . ? N9 Ni2 S3 Fe3 -111(3) . . . . ? S4 Ni2 S3 Fe3 56.90(16) . . . . ? N10 Ni2 S3 Fe2 94.8(3) . . . . ? N9 Ni2 S3 Fe2 105(3) . . . . ? S4 Ni2 S3 Fe2 -86.62(15) . . . . ? N5 Fe3 S3 C10 -90.3(6) . . . . ? N6 Fe3 S3 C10 43.5(5) . . . . ? S2 Fe3 S3 C10 161.0(4) . . . . ? N5 Fe3 S3 Ni2 13.7(4) . . . . ? N6 Fe3 S3 Ni2 147.4(4) . . . . ? S2 Fe3 S3 Ni2 -95.03(15) . . . . ? N5 Fe3 S3 Fe2 149.5(4) . . . . ? N6 Fe3 S3 Fe2 -76.8(4) . . . . ? S2 Fe3 S3 Fe2 40.75(18) . . . . ? N4 Fe2 S3 C10 -69.4(5) . . . . ? N3 Fe2 S3 C10 63.9(5) . . . . ? S1 Fe2 S3 C10 175.2(4) . . . . ? N4 Fe2 S3 Ni2 -171.4(4) . . . . ? N3 Fe2 S3 Ni2 -38.1(4) . . . . ? S1 Fe2 S3 Ni2 73.19(14) . . . . ? N4 Fe2 S3 Fe3 52.0(4) . . . . ? N3 Fe2 S3 Fe3 -174.7(4) . . . . ? S1 Fe2 S3 Fe3 -63.46(17) . . . . ? N10 Ni2 S4 C18 -4(3) . . . . ? N9 Ni2 S4 C18 9.2(6) . . . . ? S3 Ni2 S4 C18 -169.4(5) . . . . ? N10 Ni2 S4 Fe1 -109(3) . . . . ? N9 Ni2 S4 Fe1 -96.1(3) . . . . ? S3 Ni2 S4 Fe1 85.35(14) . . . . ? N2 Fe1 S4 C18 -64.7(6) . . . . ? N1 Fe1 S4 C18 68.3(6) . . . . ? S1 Fe1 S4 C18 -179.6(4) . . . . ? N2 Fe1 S4 Ni2 34.0(4) . . . . ? N1 Fe1 S4 Ni2 167.0(4) . . . . ? S1 Fe1 S4 Ni2 -80.92(13) . . . . ? N8 Ni1 S2 C9 6.7(5) . . . . ? N7 Ni1 S2 C9 -44.8(18) . . . . ? S1 Ni1 S2 C9 -178.5(4) . . . . ? N8 Ni1 S2 Fe3 -100.7(3) . . . . ? N7 Ni1 S2 Fe3 -152.2(18) . . . . ? S1 Ni1 S2 Fe3 74.08(16) . . . . ? N5 Fe3 S2 C9 102.7(5) . . . . ? N6 Fe3 S2 C9 -32.8(5) . . . . ? S3 Fe3 S2 C9 -145.9(4) . . . . ? N5 Fe3 S2 Ni1 -152.8(4) . . . . ? N6 Fe3 S2 Ni1 71.7(4) . . . . ? S3 Fe3 S2 Ni1 -41.44(16) . . . . ? N7 Ni1 N8 C8 -166.8(8) . . . . ? S2 Ni1 N8 C8 20.9(7) . . . . ? S1 Ni1 N8 C8 -127.9(16) . . . . ? N7 Ni1 N8 C4 -42.8(7) . . . . ? S2 Ni1 N8 C4 144.9(7) . . . . ? S1 Ni1 N8 C4 -4(2) . . . . ? N7 Ni1 N8 C7 72.7(8) . . . . ? S2 Ni1 N8 C7 -99.6(7) . . . . ? S1 Ni1 N8 C7 111.6(16) . . . . ? N8 Ni1 N7 C2 162.7(8) . . . . ? S2 Ni1 N7 C2 -145.3(15) . . . . ? S1 Ni1 N7 C2 -11.0(8) . . . . ? N8 Ni1 N7 C3 41.1(7) . . . . ? S2 Ni1 N7 C3 93.2(19) . . . . ? S1 Ni1 N7 C3 -132.6(7) . . . . ? N8 Ni1 N7 C5 -76.7(7) . . . . ? S2 Ni1 N7 C5 -25(2) . . . . ? S1 Ni1 N7 C5 109.6(7) . . . . ? N5 Fe3 N6 O6 15(7) . . . . ? S3 Fe3 N6 O6 -111(6) . . . . ? S2 Fe3 N6 O6 143(6) . . . . ? Ni2 S4 C18 C17 -33.7(10) . . . . ? Fe1 S4 C18 C17 66.6(10) . . . . ? N3 Fe2 N4 O4 1(7) . . . . ? S3 Fe2 N4 O4 129(7) . . . . ? S1 Fe2 N4 O4 -131(7) . . . . ? N6 Fe3 N5 O5 -12(21) . . . . ? S3 Fe3 N5 O5 114(21) . . . . ? S2 Fe3 N5 O5 -143(21) . . . . ? C2 N7 C5 C6 -162.4(10) . . . . ? C3 N7 C5 C6 -40.1(13) . . . . ? Ni1 N7 C5 C6 74.4(10) . . . . ? Ni2 S3 C10 C11 37.3(9) . . . . ? Fe3 S3 C10 C11 151.8(8) . . . . ? Fe2 S3 C10 C11 -73.9(9) . . . . ? N4 Fe2 N3 O3 37(7) . . . . ? S3 Fe2 N3 O3 -89(7) . . . . ? S1 Fe2 N3 O3 172(7) . . . . ? C13 C12 N10 C11 -159.6(11) . . . . ? C13 C12 N10 C14 78.6(13) . . . . ? C13 C12 N10 Ni2 -38.0(12) . . . . ? N9 Ni2 N10 C12 45.3(8) . . . . ? S3 Ni2 N10 C12 -136.0(7) . . . . ? S4 Ni2 N10 C12 59(3) . . . . ? N9 Ni2 N10 C11 166.0(9) . . . . ? S3 Ni2 N10 C11 -15.2(8) . . . . ? S4 Ni2 N10 C11 179(100) . . . . ? N9 Ni2 N10 C14 -74.1(8) . . . . ? S3 Ni2 N10 C14 104.6(7) . . . . ? S4 Ni2 N10 C14 -61(3) . . . . ? N10 Ni2 N9 C17 -163.9(9) . . . . ? S3 Ni2 N9 C17 -174(2) . . . . ? S4 Ni2 N9 C17 17.4(9) . . . . ? N10 Ni2 N9 C13 -42.5(8) . . . . ? S3 Ni2 N9 C13 -53(3) . . . . ? S4 Ni2 N9 C13 138.8(8) . . . . ? N10 Ni2 N9 C16 75.2(8) . . . . ? S3 Ni2 N9 C16 65(3) . . . . ? S4 Ni2 N9 C16 -103.5(7) . . . . ? N2 Fe1 N1 O1 -4(6) . . . . ? S1 Fe1 N1 O1 122(6) . . . . ? S4 Fe1 N1 O1 -135(6) . . . . ? C2 N7 C3 C4 -153.4(10) . . . . ? C5 N7 C3 C4 83.6(12) . . . . ? Ni1 N7 C3 C4 -28.8(11) . . . . ? C4 N8 C8 C9 -167.6(9) . . . . ? C7 N8 C8 C9 72.8(11) . . . . ? Ni1 N8 C8 C9 -47.3(11) . . . . ? N1 Fe1 N2 O2 -23(8) . . . . ? S1 Fe1 N2 O2 -148(7) . . . . ? S4 Fe1 N2 O2 109(7) . . . . ? N7 C5 C6 C7 -52.8(14) . . . . ? C12 N10 C11 C10 161.4(10) . . . . ? C14 N10 C11 C10 -74.9(12) . . . . ? Ni2 N10 C11 C10 44.5(12) . . . . ? S3 C10 C11 N10 -53.9(12) . . . . ? C5 C6 C7 N8 46.9(14) . . . . ? C8 N8 C7 C6 170.9(10) . . . . ? C4 N8 C7 C6 48.2(12) . . . . ? Ni1 N8 C7 C6 -66.2(11) . . . . ? C8 N8 C4 C3 159.8(9) . . . . ? C7 N8 C4 C3 -79.9(11) . . . . ? Ni1 N8 C4 C3 35.8(11) . . . . ? N7 C3 C4 N8 -3.9(13) . . . . ? C17 N9 C13 C12 151.6(11) . . . . ? C16 N9 C13 C12 -85.9(13) . . . . ? Ni2 N9 C13 C12 29.6(13) . . . . ? N10 C12 C13 N9 5.5(15) . . . . ? N8 C8 C9 S2 51.7(11) . . . . ? Ni1 S2 C9 C8 -31.9(8) . . . . ? Fe3 S2 C9 C8 88.0(8) . . . . ? Ni1 S1 C1 C2 36.1(9) . . . . ? Fe1 S1 C1 C2 -175.2(8) . . . . ? Fe2 S1 C1 C2 -61.0(9) . . . . ? C16 C15 C14 N10 -50.0(18) . . . . ? C12 N10 C14 C15 -44.6(14) . . . . ? C11 N10 C14 C15 -167.8(11) . . . . ? Ni2 N10 C14 C15 70.0(12) . . . . ? C17 N9 C16 C15 166.5(11) . . . . ? C13 N9 C16 C15 43.4(15) . . . . ? Ni2 N9 C16 C15 -71.5(12) . . . . ? C14 C15 C16 N9 51.3(18) . . . . ? C13 N9 C17 C18 -162.0(11) . . . . ? C16 N9 C17 C18 75.5(14) . . . . ? Ni2 N9 C17 C18 -43.5(13) . . . . ? S4 C18 C17 N9 51.6(14) . . . . ? C3 N7 C2 C1 158.4(10) . . . . ? C5 N7 C2 C1 -78.1(12) . . . . ? Ni1 N7 C2 C1 38.4(12) . . . . ? S1 C1 C2 N7 -49.2(12) . . . . ? C22 O7 C19 C20 41(2) . . . . ? C22 C21 C20 C19 7(3) . . . . ? O7 C19 C20 C21 -32(2) . . . . ? C20 C21 C22 O7 19(3) . . . . ? C19 O7 C22 C21 -39(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 59.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.920 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.141 # Attachment '- NiFeCONO2.cif' data_platon _database_code_depnum_ccdc_archive 'CCDC 817759' #TrackingRef '- NiFeCONO2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common None _chemical_melting_point None _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 Fe N4 Ni O3 S2' _chemical_formula_weight 420.96 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' Fe Fe 0.3463 0.8444 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.107(8) _cell_length_b 16.982(16) _cell_length_c 13.501(10) _cell_angle_alpha 90.00 _cell_angle_beta 122.67(4) _cell_angle_gamma 90.00 _cell_volume 1565(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3362 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.61 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3787 _exptl_absorpt_correction_T_max 0.6443 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKE APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12652 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2711 _reflns_number_gt 2328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2711 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.11199(7) -0.11949(2) 0.13551(4) 0.0199(2) Uani 1 1 d . . . Fe1 Fe 0.15997(9) -0.30670(3) 0.11707(5) 0.0314(2) Uani 1 1 d . . . S1 S 0.00776(15) -0.20014(5) -0.01126(8) 0.0247(3) Uani 1 1 d . . . S2 S 0.38993(15) -0.09810(6) 0.15382(9) 0.0286(3) Uani 1 1 d . . . O1 O 0.2799(4) -0.27784(17) 0.3565(2) 0.0364(7) Uani 1 1 d . . . O2 O -0.1207(6) -0.4301(2) 0.0046(3) 0.0624(11) Uani 1 1 d . . . O3 O 0.5231(5) -0.32738(18) 0.1236(3) 0.0445(8) Uani 1 1 d . . . N1 N 0.2276(5) -0.28437(18) 0.2569(3) 0.0296(8) Uani 1 1 d . . . N2 N -0.0041(6) -0.38000(19) 0.0476(3) 0.0364(9) Uani 1 1 d . . . N3 N 0.1811(5) -0.04907(17) 0.2648(3) 0.0247(7) Uani 1 1 d . . . N4 N -0.1320(5) -0.12861(17) 0.1293(3) 0.0247(7) Uani 1 1 d . . . C1 C 0.3770(6) -0.3158(2) 0.1163(3) 0.0242(8) Uani 1 1 d . . . C2 C 0.4715(6) -0.0170(2) 0.2606(3) 0.0314(9) Uani 1 1 d . . . H2A H 0.6135 -0.0143 0.3074 0.038 Uiso 1 1 calc R . . H2B H 0.4211 0.0328 0.2198 0.038 Uiso 1 1 calc R . . C3 C 0.3953(6) -0.0327(2) 0.3383(3) 0.0316(9) Uani 1 1 d . . . H3A H 0.4633 -0.0775 0.3887 0.038 Uiso 1 1 calc R . . H3B H 0.4195 0.0127 0.3880 0.038 Uiso 1 1 calc R . . C4 C 0.0691(6) 0.0262(2) 0.2104(3) 0.0305(9) Uani 1 1 d . . . H4A H 0.1188 0.0667 0.2705 0.037 Uiso 1 1 calc R . . H4B H 0.0923 0.0434 0.1504 0.037 Uiso 1 1 calc R . . C5 C -0.1480(6) 0.0176(2) 0.1560(3) 0.0317(10) Uani 1 1 d . . . H5A H -0.2122 0.0651 0.1119 0.038 Uiso 1 1 calc R . . H5B H -0.1725 0.0134 0.2186 0.038 Uiso 1 1 calc R . . C6 C -0.2413(6) -0.0532(2) 0.0743(3) 0.0293(9) Uani 1 1 d . . . H6A H -0.3754 -0.0588 0.0535 0.035 Uiso 1 1 calc R . . H6B H -0.2446 -0.0436 0.0024 0.035 Uiso 1 1 calc R . . C7 C 0.1118(6) -0.0881(2) 0.3356(3) 0.0294(9) Uani 1 1 d . . . H7A H 0.0879 -0.0485 0.3781 0.035 Uiso 1 1 calc R . . H7B H 0.2127 -0.1234 0.3926 0.035 Uiso 1 1 calc R . . C8 C -0.0762(6) -0.1346(2) 0.2555(4) 0.0303(9) Uani 1 1 d . . . H8A H -0.0565 -0.1893 0.2796 0.036 Uiso 1 1 calc R . . H8B H -0.1812 -0.1137 0.2622 0.036 Uiso 1 1 calc R . . C9 C -0.2520(6) -0.1979(2) 0.0590(4) 0.0307(9) Uani 1 1 d . . . H9A H -0.3864 -0.1910 0.0372 0.037 Uiso 1 1 calc R . . H9B H -0.2009 -0.2453 0.1060 0.037 Uiso 1 1 calc R . . C10 C -0.2462(6) -0.2059(2) -0.0507(4) 0.0308(9) Uani 1 1 d . . . H10A H -0.3228 -0.1642 -0.1057 0.037 Uiso 1 1 calc R . . H10B H -0.3028 -0.2560 -0.0885 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0220(4) 0.0209(3) 0.0194(3) 0.00131(17) 0.0128(3) 0.00105(18) Fe1 0.0362(5) 0.0241(3) 0.0286(4) 0.0033(2) 0.0140(3) 0.0041(2) S1 0.0293(6) 0.0236(5) 0.0216(5) 0.0004(4) 0.0141(5) 0.0015(4) S2 0.0271(6) 0.0317(5) 0.0318(6) -0.0007(4) 0.0189(5) -0.0028(4) O1 0.0347(19) 0.0505(18) 0.0236(17) 0.0035(13) 0.0154(14) 0.0084(14) O2 0.068(3) 0.053(2) 0.049(2) 0.0002(17) 0.0196(19) -0.034(2) O3 0.040(2) 0.0456(18) 0.052(2) 0.0111(15) 0.0276(17) 0.0044(15) N1 0.026(2) 0.0303(17) 0.033(2) 0.0027(14) 0.0161(17) 0.0039(14) N2 0.043(3) 0.032(2) 0.030(2) 0.0029(15) 0.0162(19) -0.0038(16) N3 0.0282(19) 0.0259(16) 0.0198(16) 0.0030(13) 0.0128(15) 0.0026(14) N4 0.025(2) 0.0242(16) 0.0271(18) 0.0052(13) 0.0153(16) 0.0064(13) C1 0.024(2) 0.0215(18) 0.025(2) 0.0044(15) 0.0123(18) 0.0032(16) C2 0.023(2) 0.036(2) 0.030(2) -0.0019(17) 0.0103(19) -0.0081(18) C3 0.037(3) 0.029(2) 0.024(2) -0.0002(16) 0.013(2) -0.0002(18) C4 0.043(3) 0.0238(19) 0.026(2) 0.0043(16) 0.019(2) 0.0068(18) C5 0.045(3) 0.0262(19) 0.030(2) 0.0073(16) 0.024(2) 0.0125(19) C6 0.026(2) 0.031(2) 0.031(2) 0.0104(17) 0.0151(19) 0.0098(17) C7 0.041(3) 0.030(2) 0.023(2) 0.0027(16) 0.021(2) 0.0049(18) C8 0.034(3) 0.035(2) 0.033(2) 0.0116(17) 0.025(2) 0.0085(18) C9 0.025(2) 0.032(2) 0.033(2) 0.0039(17) 0.014(2) -0.0018(17) C10 0.028(3) 0.027(2) 0.032(2) 0.0011(16) 0.012(2) -0.0007(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 1.933(3) . ? Ni1 N4 1.940(4) . ? Ni1 S2 2.161(2) . ? Ni1 S1 2.1699(17) . ? Ni1 Fe1 3.229(3) . ? Fe1 N2 1.689(4) . ? Fe1 N1 1.701(4) . ? Fe1 C1 1.771(5) . ? Fe1 S1 2.3433(19) . ? S1 C10 1.830(5) . ? S2 C2 1.840(4) . ? O1 N1 1.176(4) . ? O2 N2 1.167(5) . ? O3 C1 1.151(5) . ? N3 C3 1.489(5) . ? N3 C7 1.499(5) . ? N3 C4 1.509(5) . ? N4 C9 1.494(5) . ? N4 C6 1.506(5) . ? N4 C8 1.512(5) . ? C2 C3 1.501(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.504(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.527(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.528(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.513(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? 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 N3 Ni1 N4 83.11(14) . . ? N3 Ni1 S2 90.97(11) . . ? N4 Ni1 S2 173.82(10) . . ? N3 Ni1 S1 174.53(11) . . ? N4 Ni1 S1 91.42(11) . . ? S2 Ni1 S1 94.51(6) . . ? N3 Ni1 Fe1 133.68(9) . . ? N4 Ni1 Fe1 94.62(9) . . ? S2 Ni1 Fe1 90.73(4) . . ? S1 Ni1 Fe1 46.52(4) . . ? N2 Fe1 N1 117.78(17) . . ? N2 Fe1 C1 114.80(19) . . ? N1 Fe1 C1 107.45(18) . . ? N2 Fe1 S1 102.48(14) . . ? N1 Fe1 S1 111.97(12) . . ? C1 Fe1 S1 101.05(12) . . ? N2 Fe1 Ni1 132.62(14) . . ? N1 Fe1 Ni1 71.03(11) . . ? C1 Fe1 Ni1 104.35(11) . . ? S1 Fe1 Ni1 42.21(5) . . ? C10 S1 Ni1 96.99(14) . . ? C10 S1 Fe1 103.57(14) . . ? Ni1 S1 Fe1 91.27(8) . . ? C2 S2 Ni1 97.31(14) . . ? O1 N1 Fe1 172.4(3) . . ? O2 N2 Fe1 175.8(4) . . ? C3 N3 C7 111.2(3) . . ? C3 N3 C4 110.1(3) . . ? C7 N3 C4 110.6(3) . . ? C3 N3 Ni1 112.5(2) . . ? C7 N3 Ni1 106.0(2) . . ? C4 N3 Ni1 106.2(2) . . ? C9 N4 C6 110.4(3) . . ? C9 N4 C8 111.1(3) . . ? C6 N4 C8 110.6(3) . . ? C9 N4 Ni1 112.9(2) . . ? C6 N4 Ni1 105.5(2) . . ? C8 N4 Ni1 106.2(3) . . ? O3 C1 Fe1 173.5(3) . . ? C3 C2 S2 107.8(3) . . ? C3 C2 H2A 110.2 . . ? S2 C2 H2A 110.2 . . ? C3 C2 H2B 110.2 . . ? S2 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? N3 C3 C2 109.9(3) . . ? N3 C3 H3A 109.7 . . ? C2 C3 H3A 109.7 . . ? N3 C3 H3B 109.7 . . ? C2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 N3 113.2(3) . . ? C5 C4 H4A 108.9 . . ? N3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? N3 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? C4 C5 C6 114.9(3) . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? N4 C6 C5 112.5(3) . . ? N4 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N4 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N3 C7 C8 110.6(3) . . ? N3 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N4 C8 C7 109.9(3) . . ? N4 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? N4 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N4 C9 C10 109.8(3) . . ? N4 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? N4 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 S1 109.6(3) . . ? C9 C10 H10A 109.8 . . ? S1 C10 H10A 109.8 . . ? C9 C10 H10B 109.8 . . ? S1 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni1 Fe1 N2 117.7(2) . . . . ? N4 Ni1 Fe1 N2 32.8(2) . . . . ? S2 Ni1 Fe1 N2 -150.27(18) . . . . ? S1 Ni1 Fe1 N2 -54.75(18) . . . . ? N3 Ni1 Fe1 N1 7.01(19) . . . . ? N4 Ni1 Fe1 N1 -77.87(16) . . . . ? S2 Ni1 Fe1 N1 99.04(14) . . . . ? S1 Ni1 Fe1 N1 -165.44(13) . . . . ? N3 Ni1 Fe1 C1 -96.8(2) . . . . ? N4 Ni1 Fe1 C1 178.28(15) . . . . ? S2 Ni1 Fe1 C1 -4.81(13) . . . . ? S1 Ni1 Fe1 C1 90.71(15) . . . . ? N3 Ni1 Fe1 S1 172.44(15) . . . . ? N4 Ni1 Fe1 S1 87.57(12) . . . . ? S2 Ni1 Fe1 S1 -95.52(7) . . . . ? N3 Ni1 S1 C10 9.2(10) . . . . ? N4 Ni1 S1 C10 8.81(16) . . . . ? S2 Ni1 S1 C10 -169.44(13) . . . . ? Fe1 Ni1 S1 C10 103.83(14) . . . . ? N3 Ni1 S1 Fe1 -94.6(9) . . . . ? N4 Ni1 S1 Fe1 -95.02(10) . . . . ? S2 Ni1 S1 Fe1 86.73(6) . . . . ? N2 Fe1 S1 C10 44.5(2) . . . . ? N1 Fe1 S1 C10 -82.65(19) . . . . ? C1 Fe1 S1 C10 163.25(19) . . . . ? Ni1 Fe1 S1 C10 -97.51(14) . . . . ? N2 Fe1 S1 Ni1 142.01(14) . . . . ? N1 Fe1 S1 Ni1 14.85(13) . . . . ? C1 Fe1 S1 Ni1 -99.24(14) . . . . ? N3 Ni1 S2 C2 -8.98(15) . . . . ? N4 Ni1 S2 C2 7.4(9) . . . . ? S1 Ni1 S2 C2 170.89(13) . . . . ? Fe1 Ni1 S2 C2 -142.69(13) . . . . ? N2 Fe1 N1 O1 55(2) . . . . ? C1 Fe1 N1 O1 -76(2) . . . . ? S1 Fe1 N1 O1 173(2) . . . . ? Ni1 Fe1 N1 O1 -176(2) . . . . ? N1 Fe1 N2 O2 19(5) . . . . ? C1 Fe1 N2 O2 147(5) . . . . ? S1 Fe1 N2 O2 -104(5) . . . . ? Ni1 Fe1 N2 O2 -70(5) . . . . ? N4 Ni1 N3 C3 164.7(2) . . . . ? S2 Ni1 N3 C3 -17.0(2) . . . . ? S1 Ni1 N3 C3 164.3(8) . . . . ? Fe1 Ni1 N3 C3 74.9(3) . . . . ? N4 Ni1 N3 C7 43.0(2) . . . . ? S2 Ni1 N3 C7 -138.8(2) . . . . ? S1 Ni1 N3 C7 42.6(11) . . . . ? Fe1 Ni1 N3 C7 -46.9(3) . . . . ? N4 Ni1 N3 C4 -74.7(3) . . . . ? S2 Ni1 N3 C4 103.5(2) . . . . ? S1 Ni1 N3 C4 -75.1(10) . . . . ? Fe1 Ni1 N3 C4 -164.54(19) . . . . ? N3 Ni1 N4 C9 -164.0(3) . . . . ? S2 Ni1 N4 C9 180(67) . . . . ? S1 Ni1 N4 C9 16.0(2) . . . . ? Fe1 Ni1 N4 C9 -30.5(2) . . . . ? N3 Ni1 N4 C6 75.3(2) . . . . ? S2 Ni1 N4 C6 58.9(10) . . . . ? S1 Ni1 N4 C6 -104.7(2) . . . . ? Fe1 Ni1 N4 C6 -151.2(2) . . . . ? N3 Ni1 N4 C8 -42.1(2) . . . . ? S2 Ni1 N4 C8 -58.5(10) . . . . ? S1 Ni1 N4 C8 137.9(2) . . . . ? Fe1 Ni1 N4 C8 91.4(2) . . . . ? N2 Fe1 C1 O3 -73(3) . . . . ? N1 Fe1 C1 O3 60(3) . . . . ? S1 Fe1 C1 O3 177(3) . . . . ? Ni1 Fe1 C1 O3 134(3) . . . . ? Ni1 S2 C2 C3 33.7(3) . . . . ? C7 N3 C3 C2 162.9(3) . . . . ? C4 N3 C3 C2 -74.1(4) . . . . ? Ni1 N3 C3 C2 44.1(4) . . . . ? S2 C2 C3 N3 -51.1(4) . . . . ? C3 N3 C4 C5 -168.0(3) . . . . ? C7 N3 C4 C5 -44.7(4) . . . . ? Ni1 N3 C4 C5 69.9(3) . . . . ? N3 C4 C5 C6 -49.0(4) . . . . ? C9 N4 C6 C5 166.9(3) . . . . ? C8 N4 C6 C5 43.6(4) . . . . ? Ni1 N4 C6 C5 -70.8(3) . . . . ? C4 C5 C6 N4 49.7(4) . . . . ? C3 N3 C7 C8 -156.4(3) . . . . ? C4 N3 C7 C8 80.9(4) . . . . ? Ni1 N3 C7 C8 -33.9(4) . . . . ? C9 N4 C8 C7 154.5(3) . . . . ? C6 N4 C8 C7 -82.6(4) . . . . ? Ni1 N4 C8 C7 31.4(3) . . . . ? N3 C7 C8 N4 1.5(4) . . . . ? C6 N4 C9 C10 76.7(4) . . . . ? C8 N4 C9 C10 -160.3(3) . . . . ? Ni1 N4 C9 C10 -41.2(4) . . . . ? N4 C9 C10 S1 48.7(4) . . . . ? Ni1 S1 C10 C9 -32.5(3) . . . . ? Fe1 S1 C10 C9 60.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.780 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.161