# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou Fujian 350002 P.R.China ; _publ_contact_author_email ccn@fjirsm.ac.cn _publ_contact_author_name 'Prof Chang-Neng Chen' _publ_section_title ; Synthesis, Structures and Electrochimestry studies of 2Fe2S-Fe(II)(sip)2 models for H-cluster of [FeFe]-hydrogenases ; loop_ _publ_author_name 'Ming-Qiang Hu' 'Cheng-Bing Ma' 'Hui-Min Wen' 'La Li' 'Qing-Yun Yan' ; Hui Chen ; 'Chang-Neng Chen' data_A _database_code_depnum_ccdc_archive 'CCDC 776575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-[(pentacarbonylpropanedithiolatodiiron)-sulfanylpropyliminomethylpyridine] iron(ii) ; _chemical_name_common ; bis-((pentacarbonylpropanedithiolatodiiron)- sulfanylpropyliminomethylpyridine) iron(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Fe5 N4 O10 S6' _chemical_formula_sum 'C32 H30 Fe5 N4 O10 S6' _chemical_formula_weight 1102.21 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' Fe Fe 0.3463 0.8444 '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)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.330(10) _cell_length_b 10.320(4) _cell_length_c 24.294(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.816(7) _cell_angle_gamma 90.00 _cell_volume 4732(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3901 _cell_measurement_theta_min 2.1580 _cell_measurement_theta_max 27.4642 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2400 _exptl_crystal_size_mid 0.1900 _exptl_crystal_size_min 0.1400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.812 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Mercury2 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 13.6612 _diffrn_measurement_method CCD_Profile_fitting _diffrn_reflns_theta_min 2.1580 _diffrn_reflns_theta_max 27.4642 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35788 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 26 _reflns_number_total 10787 _reflns_number_gt 8111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 333 45 ' ' 2 0.208 0.035 0.908 13 1 ' ' 3 0.792 -0.035 0.092 15 1 ' ' 4 0.500 0.500 1.000 329 45 ' ' 5 0.703 0.481 0.404 12 1 ' ' 6 0.297 0.519 0.596 12 1 ' ' _platon_squeeze_details ; ; _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^)+(0.0740P)^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 10787 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.43966(3) 0.28662(6) 0.45756(3) 0.04675(16) Uani 1 1 d . . . Fe2 Fe 0.42281(3) 0.26188(5) 0.34994(3) 0.04170(15) Uani 1 1 d . . . Fe3 Fe 0.69058(3) -0.29418(6) 0.25201(3) 0.05536(18) Uani 1 1 d . . . Fe4 Fe 0.56513(3) -0.21146(6) 0.20955(3) 0.04851(16) Uani 1 1 d . . . Fe5 Fe 0.42217(3) 0.08155(5) 0.20035(2) 0.04070(15) Uani 1 1 d . . . S1 S 0.45271(6) 0.09442(10) 0.41655(5) 0.0478(2) Uani 1 1 d . . . S2 S 0.51658(6) 0.36683(11) 0.41714(5) 0.0522(3) Uani 1 1 d . . . S3 S 0.60610(7) -0.35033(12) 0.28819(6) 0.0652(3) Uani 1 1 d . . . S4 S 0.65997(6) -0.08639(11) 0.26236(6) 0.0554(3) Uani 1 1 d . . . S5 S 0.47765(5) 0.17708(10) 0.29149(4) 0.0422(2) Uani 1 1 d . . . S6 S 0.48812(5) -0.10086(10) 0.24030(5) 0.0479(2) Uani 1 1 d . . . C11 C 0.3615(3) 0.2199(5) 0.4611(2) 0.0578(11) Uani 1 1 d . . . C12 C 0.4935(3) 0.2832(4) 0.5363(2) 0.0570(11) Uani 1 1 d . . . C13 C 0.3982(3) 0.4421(5) 0.4484(2) 0.0594(11) Uani 1 1 d . . . C14 C 0.3351(2) 0.2050(4) 0.32445(19) 0.0501(10) Uani 1 1 d . . . C15 C 0.3944(2) 0.4094(4) 0.3114(2) 0.0526(10) Uani 1 1 d . . . C17 C 0.5981(2) 0.2719(5) 0.4381(2) 0.0638(12) Uani 1 1 d . . . H17A H 0.6069 0.2521 0.4024 0.077 Uiso 1 1 calc R . . H17B H 0.6370 0.3256 0.4629 0.077 Uiso 1 1 calc R . . C18 C 0.5993(3) 0.1464(5) 0.4706(2) 0.0673(13) Uani 1 1 d . . . H18A H 0.6458 0.1076 0.4814 0.081 Uiso 1 1 calc R . . H18B H 0.5922 0.1661 0.5071 0.081 Uiso 1 1 calc R . . C19 C 0.5447(2) 0.0488(4) 0.4362(2) 0.0602(11) Uani 1 1 d . . . H19A H 0.5529 -0.0304 0.4593 0.072 Uiso 1 1 calc R . . H19B H 0.5523 0.0292 0.4000 0.072 Uiso 1 1 calc R . . C21 C 0.7318(3) -0.2323(5) 0.2041(3) 0.0687(13) Uani 1 1 d . . . C22 C 0.7715(3) -0.3304(5) 0.3136(3) 0.0692(13) Uani 1 1 d . . . C23 C 0.6715(3) -0.4442(5) 0.2129(3) 0.0741(15) Uani 1 1 d . . . C24 C 0.5645(3) -0.1418(5) 0.1441(2) 0.0642(12) Uani 1 1 d . . . C25 C 0.5090(3) -0.3348(6) 0.1692(3) 0.0762(15) Uani 1 1 d . . . C27 C 0.6172(3) -0.2697(6) 0.3576(3) 0.0861(18) Uani 1 1 d . . . H27A H 0.5724 -0.2305 0.3538 0.103 Uiso 1 1 calc R . . H27B H 0.6281 -0.3348 0.3885 0.103 Uiso 1 1 calc R . . C28 C 0.6739(3) -0.1664(7) 0.3775(3) 0.0908(19) Uani 1 1 d . . . H28A H 0.6779 -0.1356 0.4163 0.109 Uiso 1 1 calc R . . H28B H 0.7189 -0.2052 0.3815 0.109 Uiso 1 1 calc R . . C29 C 0.6605(3) -0.0535(6) 0.3366(2) 0.0751(15) Uani 1 1 d . . . H29A H 0.6965 0.0113 0.3551 0.090 Uiso 1 1 calc R . . H29B H 0.6151 -0.0161 0.3324 0.090 Uiso 1 1 calc R . . C101 C 0.3381(3) -0.0574(6) 0.0868(2) 0.0762(15) Uani 1 1 d . . . H10A H 0.3104 -0.0924 0.1061 0.091 Uiso 1 1 calc R . . C102 C 0.3211(4) -0.0856(8) 0.0276(3) 0.108(2) Uani 1 1 d . . . H10B H 0.2825 -0.1384 0.0075 0.129 Uiso 1 1 calc R . . C103 C 0.3617(4) -0.0348(9) -0.0013(3) 0.122(3) Uani 1 1 d . . . H10C H 0.3510 -0.0530 -0.0412 0.146 Uiso 1 1 calc R . . C104 C 0.4187(4) 0.0437(7) 0.0294(3) 0.097(2) Uani 1 1 d . . . H10D H 0.4469 0.0784 0.0105 0.116 Uiso 1 1 calc R . . C105 C 0.4328(3) 0.0695(5) 0.0882(2) 0.0633(12) Uani 1 1 d . . . C106 C 0.4896(3) 0.1505(5) 0.1254(2) 0.0596(12) Uani 1 1 d . . . H10E H 0.5224 0.1882 0.1119 0.072 Uiso 1 1 calc R . . C107 C 0.5480(2) 0.2472(5) 0.2212(2) 0.0595(12) Uani 1 1 d . . . H10F H 0.5625 0.3147 0.2003 0.071 Uiso 1 1 calc R . . H10G H 0.5890 0.1939 0.2423 0.071 Uiso 1 1 calc R . . C108 C 0.5189(3) 0.3072(4) 0.2648(2) 0.0581(11) Uani 1 1 d . . . H10H H 0.4842 0.3735 0.2453 0.070 Uiso 1 1 calc R . . H10I H 0.5569 0.3467 0.2976 0.070 Uiso 1 1 calc R . . C201 C 0.3489(3) 0.3342(5) 0.1482(2) 0.0668(13) Uani 1 1 d . . . H20A H 0.3909 0.3621 0.1452 0.080 Uiso 1 1 calc R . . C202 C 0.2904(4) 0.4136(6) 0.1281(3) 0.0867(18) Uani 1 1 d . . . H20B H 0.2937 0.4949 0.1128 0.104 Uiso 1 1 calc R . . C203 C 0.2277(3) 0.3739(7) 0.1306(3) 0.087(2) Uani 1 1 d . . . H20C H 0.1880 0.4272 0.1167 0.104 Uiso 1 1 calc R . . C204 C 0.2238(3) 0.2542(6) 0.1537(2) 0.0758(17) Uani 1 1 d . . . H20D H 0.1813 0.2244 0.1553 0.091 Uiso 1 1 calc R . . C205 C 0.2847(2) 0.1781(5) 0.1750(2) 0.0580(12) Uani 1 1 d . . . C206 C 0.2891(2) 0.0538(5) 0.2023(2) 0.0601(12) Uani 1 1 d . . . H20E H 0.2505 0.0164 0.2080 0.072 Uiso 1 1 calc R . . C207 C 0.3638(2) -0.1249(5) 0.2526(2) 0.0630(12) Uani 1 1 d . . . H20F H 0.3199 -0.1719 0.2446 0.076 Uiso 1 1 calc R . . H20G H 0.3845 -0.1066 0.2947 0.076 Uiso 1 1 calc R . . C208 C 0.4141(3) -0.2050(4) 0.2343(3) 0.0669(13) Uani 1 1 d . . . H20H H 0.3909 -0.2352 0.1938 0.080 Uiso 1 1 calc R . . H20I H 0.4302 -0.2797 0.2601 0.080 Uiso 1 1 calc R . . O11 O 0.3095(2) 0.1778(4) 0.4624(2) 0.0897(12) Uani 1 1 d . . . O12 O 0.5260(2) 0.2816(4) 0.58603(16) 0.0789(11) Uani 1 1 d . . . O13 O 0.3671(2) 0.5376(4) 0.44031(19) 0.0857(12) Uani 1 1 d . . . O14 O 0.27677(17) 0.1729(4) 0.31289(16) 0.0751(10) Uani 1 1 d . . . O15 O 0.3757(2) 0.5063(3) 0.28729(19) 0.0819(11) Uani 1 1 d . . . O21 O 0.7592(3) -0.1951(5) 0.1740(2) 0.1094(16) Uani 1 1 d . . . O22 O 0.8237(2) -0.3534(5) 0.3509(2) 0.1039(15) Uani 1 1 d . . . O23 O 0.6569(2) -0.5390(4) 0.1870(2) 0.1009(15) Uani 1 1 d . . . O24 O 0.5682(3) -0.1056(5) 0.09998(19) 0.0985(14) Uani 1 1 d . . . O25 O 0.4749(3) -0.4213(5) 0.1442(3) 0.1218(18) Uani 1 1 d . . . N1 N 0.39350(18) 0.0193(4) 0.11797(16) 0.0552(9) Uani 1 1 d . . . N2 N 0.49200(18) 0.1675(3) 0.17893(16) 0.0493(8) Uani 1 1 d . . . N3 N 0.34701(19) 0.2167(4) 0.17212(16) 0.0523(9) Uani 1 1 d . . . N4 N 0.34976(17) -0.0030(4) 0.21862(16) 0.0509(8) Uani 1 1 d . . . 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 Fe1 0.0548(3) 0.0449(3) 0.0418(3) -0.0044(3) 0.0193(3) -0.0003(2) Fe2 0.0469(3) 0.0381(3) 0.0405(3) 0.0006(2) 0.0168(2) 0.0011(2) Fe3 0.0550(4) 0.0502(4) 0.0660(4) 0.0060(3) 0.0284(3) 0.0068(3) Fe4 0.0529(3) 0.0426(3) 0.0537(4) 0.0006(3) 0.0241(3) 0.0023(2) Fe5 0.0403(3) 0.0453(3) 0.0398(3) 0.0007(2) 0.0188(2) -0.0007(2) S1 0.0601(6) 0.0388(5) 0.0457(6) 0.0016(4) 0.0209(4) 0.0020(4) S2 0.0559(6) 0.0457(6) 0.0559(7) -0.0074(5) 0.0220(5) -0.0074(4) S3 0.0685(7) 0.0556(7) 0.0813(9) 0.0208(6) 0.0392(6) 0.0071(5) S4 0.0582(6) 0.0494(6) 0.0643(7) -0.0023(5) 0.0292(5) -0.0027(5) S5 0.0445(5) 0.0417(5) 0.0420(5) -0.0004(4) 0.0178(4) -0.0018(4) S6 0.0525(6) 0.0412(5) 0.0565(6) 0.0041(5) 0.0276(5) 0.0017(4) C11 0.066(3) 0.057(3) 0.050(3) -0.002(2) 0.022(2) 0.000(2) C12 0.068(3) 0.055(3) 0.049(3) -0.005(2) 0.023(2) -0.006(2) C13 0.067(3) 0.057(3) 0.054(3) -0.007(2) 0.023(2) -0.005(2) C14 0.063(3) 0.048(2) 0.039(2) 0.0015(18) 0.0182(18) 0.0023(19) C15 0.055(2) 0.050(2) 0.057(3) 0.007(2) 0.026(2) 0.0084(18) C17 0.051(3) 0.071(3) 0.066(3) -0.009(3) 0.019(2) -0.006(2) C18 0.063(3) 0.078(3) 0.054(3) 0.006(3) 0.014(2) 0.020(2) C19 0.071(3) 0.050(3) 0.063(3) 0.009(2) 0.028(2) 0.018(2) C21 0.071(3) 0.062(3) 0.081(4) -0.005(3) 0.038(3) 0.000(2) C22 0.060(3) 0.073(3) 0.075(4) 0.007(3) 0.026(3) 0.007(2) C23 0.064(3) 0.054(3) 0.112(5) -0.001(3) 0.043(3) 0.008(2) C24 0.074(3) 0.065(3) 0.057(3) 0.000(2) 0.028(2) 0.009(2) C25 0.070(3) 0.070(3) 0.084(4) -0.011(3) 0.023(3) -0.001(3) C27 0.099(4) 0.104(5) 0.068(4) 0.030(3) 0.046(3) 0.019(4) C28 0.090(4) 0.125(6) 0.059(4) 0.001(4) 0.029(3) 0.023(4) C29 0.074(3) 0.088(4) 0.063(3) -0.020(3) 0.026(3) 0.000(3) C101 0.078(3) 0.098(4) 0.054(3) -0.025(3) 0.027(2) -0.014(3) C102 0.116(5) 0.140(6) 0.071(4) -0.047(4) 0.039(4) -0.039(5) C103 0.132(6) 0.184(9) 0.052(4) -0.035(5) 0.037(4) -0.025(6) C104 0.112(5) 0.137(6) 0.057(4) -0.007(4) 0.049(3) -0.007(4) C105 0.072(3) 0.078(3) 0.047(3) 0.002(2) 0.031(2) 0.008(2) C106 0.068(3) 0.068(3) 0.058(3) 0.013(2) 0.041(2) 0.007(2) C107 0.055(3) 0.061(3) 0.069(3) 0.002(2) 0.032(2) -0.014(2) C108 0.067(3) 0.050(2) 0.062(3) -0.006(2) 0.029(2) -0.020(2) C201 0.078(3) 0.061(3) 0.060(3) 0.009(3) 0.024(2) 0.017(2) C202 0.101(4) 0.078(4) 0.076(4) 0.016(3) 0.027(3) 0.043(3) C203 0.070(4) 0.108(5) 0.065(4) -0.021(3) 0.004(3) 0.037(3) C204 0.054(3) 0.100(4) 0.063(3) -0.031(3) 0.011(2) 0.019(3) C205 0.046(2) 0.076(3) 0.049(3) -0.019(2) 0.0144(18) 0.007(2) C206 0.043(2) 0.077(3) 0.059(3) -0.022(3) 0.0185(19) -0.011(2) C207 0.058(3) 0.060(3) 0.080(3) 0.001(3) 0.036(2) -0.020(2) C208 0.077(3) 0.046(3) 0.090(4) 0.002(2) 0.046(3) -0.010(2) O11 0.073(2) 0.106(3) 0.100(3) -0.005(3) 0.044(2) -0.019(2) O12 0.090(3) 0.091(3) 0.045(2) -0.0039(19) 0.0134(17) -0.005(2) O13 0.091(3) 0.063(2) 0.098(3) -0.005(2) 0.029(2) 0.021(2) O14 0.0530(19) 0.097(3) 0.070(2) 0.001(2) 0.0165(16) -0.0114(18) O15 0.093(3) 0.060(2) 0.100(3) 0.032(2) 0.045(2) 0.0188(19) O21 0.135(4) 0.115(4) 0.116(4) 0.001(3) 0.090(4) -0.011(3) O22 0.083(3) 0.133(4) 0.083(3) 0.016(3) 0.016(2) 0.034(3) O23 0.092(3) 0.070(3) 0.152(5) -0.028(3) 0.057(3) -0.008(2) O24 0.128(4) 0.116(4) 0.065(3) 0.019(2) 0.051(3) 0.026(3) O25 0.130(4) 0.097(4) 0.124(4) -0.045(3) 0.031(3) -0.044(3) N1 0.060(2) 0.062(2) 0.046(2) -0.0015(18) 0.0227(16) 0.0057(17) N2 0.056(2) 0.0453(19) 0.054(2) 0.0057(16) 0.0292(16) 0.0064(15) N3 0.053(2) 0.062(2) 0.041(2) -0.0012(17) 0.0158(15) 0.0107(16) N4 0.0465(18) 0.060(2) 0.052(2) -0.0129(17) 0.0247(15) -0.0094(16) _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 Fe1 C11 1.762(5) . ? Fe1 C13 1.788(5) . ? Fe1 C12 1.817(5) . ? Fe1 S1 2.2790(14) . ? Fe1 S2 2.2883(15) . ? Fe1 Fe2 2.5205(16) . ? Fe2 C14 1.757(5) . ? Fe2 C15 1.768(4) . ? Fe2 S2 2.2714(14) . ? Fe2 S5 2.2808(13) . ? Fe2 S1 2.2900(14) . ? Fe3 C23 1.783(6) . ? Fe3 C21 1.786(6) . ? Fe3 C22 1.804(5) . ? Fe3 S4 2.2727(16) . ? Fe3 S3 2.2759(16) . ? Fe3 Fe4 2.5183(14) . ? Fe4 C24 1.742(5) . ? Fe4 C25 1.747(6) . ? Fe4 S6 2.2763(14) . ? Fe4 S4 2.2783(15) . ? Fe4 S3 2.2837(16) . ? Fe5 N4 1.900(3) . ? Fe5 N2 1.903(3) . ? Fe5 N1 1.972(4) . ? Fe5 N3 1.993(4) . ? Fe5 S5 2.3001(15) . ? Fe5 S6 2.3058(14) . ? S1 C19 1.812(5) . ? S2 C17 1.827(5) . ? S3 C27 1.818(6) . ? S4 C29 1.831(5) . ? S5 C108 1.825(4) . ? S6 C208 1.810(5) . ? C11 O11 1.155(6) . ? C12 O12 1.142(6) . ? C13 O13 1.148(6) . ? C14 O14 1.161(5) . ? C15 O15 1.150(5) . ? C17 C18 1.513(7) . ? C18 C19 1.501(7) . ? C21 O21 1.138(6) . ? C22 O22 1.135(6) . ? C23 O23 1.141(6) . ? C24 O24 1.162(6) . ? C25 O25 1.155(6) . ? C27 C28 1.510(9) . ? C28 C29 1.489(8) . ? C101 N1 1.354(6) . ? C101 C102 1.379(8) . ? C102 C103 1.371(9) . ? C103 C104 1.382(9) . ? C104 C105 1.375(7) . ? C105 N1 1.365(6) . ? C105 C106 1.440(7) . ? C106 N2 1.295(6) . ? C107 N2 1.469(6) . ? C107 C108 1.523(7) . ? C201 N3 1.351(6) . ? C201 C202 1.375(7) . ? C202 C203 1.362(9) . ? C203 C204 1.372(9) . ? C204 C205 1.392(7) . ? C205 N3 1.355(6) . ? C205 C206 1.432(7) . ? C206 N4 1.287(5) . ? C207 N4 1.474(6) . ? C207 C208 1.505(7) . ? 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 C11 Fe1 C13 88.0(2) . . ? C11 Fe1 C12 98.3(2) . . ? C13 Fe1 C12 102.7(2) . . ? C11 Fe1 S1 86.25(16) . . ? C13 Fe1 S1 148.52(16) . . ? C12 Fe1 S1 108.71(15) . . ? C11 Fe1 S2 159.09(16) . . ? C13 Fe1 S2 89.28(16) . . ? C12 Fe1 S2 102.57(16) . . ? S1 Fe1 S2 85.30(5) . . ? C11 Fe1 Fe2 103.48(16) . . ? C13 Fe1 Fe2 94.90(16) . . ? C12 Fe1 Fe2 152.39(15) . . ? S1 Fe1 Fe2 56.73(3) . . ? S2 Fe1 Fe2 56.12(4) . . ? C14 Fe2 C15 90.7(2) . . ? C14 Fe2 S2 152.06(15) . . ? C15 Fe2 S2 89.53(16) . . ? C14 Fe2 S5 108.62(15) . . ? C15 Fe2 S5 98.07(15) . . ? S2 Fe2 S5 99.01(6) . . ? C14 Fe2 S1 88.00(14) . . ? C15 Fe2 S1 166.57(15) . . ? S2 Fe2 S1 85.44(5) . . ? S5 Fe2 S1 95.02(5) . . ? C14 Fe2 Fe1 97.38(14) . . ? C15 Fe2 Fe1 110.70(15) . . ? S2 Fe2 Fe1 56.76(4) . . ? S5 Fe2 Fe1 140.82(4) . . ? S1 Fe2 Fe1 56.31(4) . . ? C23 Fe3 C21 91.4(3) . . ? C23 Fe3 C22 102.3(3) . . ? C21 Fe3 C22 96.3(3) . . ? C23 Fe3 S4 149.79(18) . . ? C21 Fe3 S4 87.07(17) . . ? C22 Fe3 S4 107.85(19) . . ? C23 Fe3 S3 86.48(18) . . ? C21 Fe3 S3 161.26(19) . . ? C22 Fe3 S3 102.32(19) . . ? S4 Fe3 S3 85.45(5) . . ? C23 Fe3 Fe4 95.11(17) . . ? C21 Fe3 Fe4 105.14(18) . . ? C22 Fe3 Fe4 151.94(18) . . ? S4 Fe3 Fe4 56.51(4) . . ? S3 Fe3 Fe4 56.62(5) . . ? C24 Fe4 C25 90.4(3) . . ? C24 Fe4 S6 108.70(17) . . ? C25 Fe4 S6 99.45(19) . . ? C24 Fe4 S4 89.88(18) . . ? C25 Fe4 S4 165.54(18) . . ? S6 Fe4 S4 94.15(6) . . ? C24 Fe4 S3 154.13(17) . . ? C25 Fe4 S3 88.3(2) . . ? S6 Fe4 S3 96.98(6) . . ? S4 Fe4 S3 85.14(6) . . ? C24 Fe4 Fe3 100.16(17) . . ? C25 Fe4 Fe3 109.48(18) . . ? S6 Fe4 Fe3 138.67(5) . . ? S4 Fe4 Fe3 56.30(4) . . ? S3 Fe4 Fe3 56.33(4) . . ? N4 Fe5 N2 177.70(16) . . ? N4 Fe5 N1 97.18(15) . . ? N2 Fe5 N1 81.00(16) . . ? N4 Fe5 N3 80.81(16) . . ? N2 Fe5 N3 97.70(15) . . ? N1 Fe5 N3 88.80(15) . . ? N4 Fe5 S5 96.74(11) . . ? N2 Fe5 S5 85.10(12) . . ? N1 Fe5 S5 166.07(11) . . ? N3 Fe5 S5 94.03(11) . . ? N4 Fe5 S6 84.64(12) . . ? N2 Fe5 S6 96.86(11) . . ? N1 Fe5 S6 93.88(12) . . ? N3 Fe5 S6 165.43(12) . . ? S5 Fe5 S6 86.81(5) . . ? C19 S1 Fe1 112.78(16) . . ? C19 S1 Fe2 111.07(16) . . ? Fe1 S1 Fe2 66.96(5) . . ? C17 S2 Fe2 112.15(16) . . ? C17 S2 Fe1 112.34(18) . . ? Fe2 S2 Fe1 67.11(5) . . ? C27 S3 Fe3 113.0(2) . . ? C27 S3 Fe4 111.7(2) . . ? Fe3 S3 Fe4 67.05(5) . . ? C29 S4 Fe3 112.5(2) . . ? C29 S4 Fe4 110.72(19) . . ? Fe3 S4 Fe4 67.19(5) . . ? C108 S5 Fe2 109.53(16) . . ? C108 S5 Fe5 95.68(16) . . ? Fe2 S5 Fe5 125.84(5) . . ? C208 S6 Fe4 109.16(17) . . ? C208 S6 Fe5 96.59(17) . . ? Fe4 S6 Fe5 129.39(6) . . ? O11 C11 Fe1 178.6(5) . . ? O12 C12 Fe1 178.4(4) . . ? O13 C13 Fe1 175.2(5) . . ? O14 C14 Fe2 172.9(4) . . ? O15 C15 Fe2 178.7(4) . . ? C18 C17 S2 116.2(3) . . ? C19 C18 C17 114.8(4) . . ? C18 C19 S1 116.7(3) . . ? O21 C21 Fe3 178.5(6) . . ? O22 C22 Fe3 177.4(5) . . ? O23 C23 Fe3 177.7(5) . . ? O24 C24 Fe4 173.3(5) . . ? O25 C25 Fe4 176.2(6) . . ? C28 C27 S3 115.9(4) . . ? C29 C28 C27 114.3(5) . . ? C28 C29 S4 116.4(4) . . ? N1 C101 C102 122.7(6) . . ? C103 C102 C101 119.2(6) . . ? C102 C103 C104 119.5(6) . . ? C105 C104 C103 118.9(6) . . ? N1 C105 C104 122.7(5) . . ? N1 C105 C106 112.3(4) . . ? C104 C105 C106 125.1(5) . . ? N2 C106 C105 115.5(4) . . ? N2 C107 C108 108.3(4) . . ? C107 C108 S5 107.2(3) . . ? N3 C201 C202 121.9(5) . . ? C203 C202 C201 120.3(6) . . ? C202 C203 C204 119.1(5) . . ? C203 C204 C205 118.7(6) . . ? N3 C205 C204 122.3(5) . . ? N3 C205 C206 112.8(4) . . ? C204 C205 C206 124.8(5) . . ? N4 C206 C205 116.0(4) . . ? N4 C207 C208 108.3(4) . . ? C207 C208 S6 106.6(3) . . ? C101 N1 C105 117.1(4) . . ? C101 N1 Fe5 128.9(3) . . ? C105 N1 Fe5 113.8(3) . . ? C106 N2 C107 120.5(4) . . ? C106 N2 Fe5 117.3(3) . . ? C107 N2 Fe5 122.2(3) . . ? C205 N3 C201 117.5(4) . . ? C205 N3 Fe5 112.9(3) . . ? C201 N3 Fe5 129.5(3) . . ? C206 N4 C207 121.7(4) . . ? C206 N4 Fe5 117.1(4) . . ? C207 N4 Fe5 121.2(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.523 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.089 # Attachment '- 776576.cif' data_B1 _database_code_depnum_ccdc_archive 'CCDC 776576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-[(pentacarbonylpropanedithiolatodiiron)-sulfanylpropyliminomethylpyridine] nickel(ii) ; _chemical_name_common ; bis-((pentacarbonylpropanedithiolatodiiron)- sulfanylpropyliminomethylpyridine) nickel(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Fe4.58 N4 Ni0.42 O10 S6' _chemical_formula_sum 'C32 H30 Fe4.58 N4 Ni0.42 O10 S6' _chemical_formula_weight 1103.41 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.136(4) _cell_length_b 10.365(2) _cell_length_c 24.184(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.313(3) _cell_angle_gamma 90.00 _cell_volume 4669.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10164 _cell_measurement_theta_min 2.2491 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.6000 _exptl_crystal_size_mid 0.2300 _exptl_crystal_size_min 0.1600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2227 _exptl_absorpt_coefficient_mu 1.875 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7823 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294.1500 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn70 (4x4 bin mode) ; _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34774 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10458 _reflns_number_gt 8961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 310 45 ' ' 2 0.797 0.049 0.590 10 0 ' ' 3 0.499 0.501 0.500 310 45 ' ' 4 0.299 0.456 0.092 10 0 ' ' 5 0.701 0.544 0.908 9 0 ' ' 6 0.201 0.956 0.408 9 0 ' ' _platon_squeeze_details ; ; _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^)+(0.0690P)^2^+2.4916P] 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 10458 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.923437(19) 0.57990(4) 0.199721(16) 0.03923(15) Uani 0.42(2) 1 d P . . Fe5 Fe 0.923437(19) 0.57990(4) 0.199721(16) 0.03923(15) Uani 0.58(2) 1 d P . . Fe1 Fe 1.19173(3) 0.20249(5) 0.25041(2) 0.05216(13) Uani 1 1 d . . . Fe2 Fe 1.06409(2) 0.28014(5) 0.20961(2) 0.04824(13) Uani 1 1 d . . . Fe3 Fe 0.94057(2) 0.78578(4) 0.457993(18) 0.04349(12) Uani 1 1 d . . . Fe4 Fe 0.92488(2) 0.76036(4) 0.350439(17) 0.04014(11) Uani 1 1 d . . . S1 S 1.10939(5) 0.14390(9) 0.28915(5) 0.0639(2) Uani 1 1 d . . . S2 S 1.15931(5) 0.40770(8) 0.26119(4) 0.05275(19) Uani 1 1 d . . . S3 S 0.98691(4) 0.39197(8) 0.24014(4) 0.04954(18) Uani 1 1 d . . . S4 S 1.01878(4) 0.86621(8) 0.41864(4) 0.05040(18) Uani 1 1 d . . . S5 S 0.95501(4) 0.59456(7) 0.41755(3) 0.04555(17) Uani 1 1 d . . . S6 S 0.98101(4) 0.67531(7) 0.29281(3) 0.04127(16) Uani 1 1 d . . . N1 N 0.84629(14) 0.7185(3) 0.16977(11) 0.0513(6) Uani 1 1 d . . . N2 N 0.84641(13) 0.4970(3) 0.21583(12) 0.0503(6) Uani 1 1 d . . . N3 N 0.89303(15) 0.5227(3) 0.11379(13) 0.0593(7) Uani 1 1 d . . . N4 N 0.99541(13) 0.6681(3) 0.17852(11) 0.0465(6) Uani 1 1 d . . . C1 C 1.2315(2) 0.2658(4) 0.2019(2) 0.0691(10) Uani 1 1 d . . . C2 C 1.2744(2) 0.1664(4) 0.31174(19) 0.0655(9) Uani 1 1 d . . . C3 C 1.1708(2) 0.0552(4) 0.2090(2) 0.0684(10) Uani 1 1 d . . . C4 C 1.0603(2) 0.3503(4) 0.14232(16) 0.0613(9) Uani 1 1 d . . . C5 C 1.0078(2) 0.1554(4) 0.1704(2) 0.0741(11) Uani 1 1 d . . . C6 C 1.1225(3) 0.2272(5) 0.3594(2) 0.0854(14) Uani 1 1 d . . . H6A H 1.0771 0.2658 0.3558 0.102 Uiso 1 1 calc R . . H6B H 1.1344 0.1632 0.3909 0.102 Uiso 1 1 calc R . . C7 C 1.1784(3) 0.3291(5) 0.37822(18) 0.0827(13) Uani 1 1 d . . . H7A H 1.2240 0.2910 0.3822 0.099 Uiso 1 1 calc R . . H7B H 1.1830 0.3606 0.4173 0.099 Uiso 1 1 calc R . . C8 C 1.1636(2) 0.4415(4) 0.33611(18) 0.0711(10) Uani 1 1 d . . . H8A H 1.2007 0.5057 0.3539 0.085 Uiso 1 1 calc R . . H8B H 1.1183 0.4799 0.3329 0.085 Uiso 1 1 calc R . . C11 C 0.99430(19) 0.7816(3) 0.53764(15) 0.0538(7) Uani 1 1 d . . . C12 C 0.8605(2) 0.7192(4) 0.46057(16) 0.0566(8) Uani 1 1 d . . . C13 C 0.89887(19) 0.9397(3) 0.44813(15) 0.0544(8) Uani 1 1 d . . . C14 C 0.89617(18) 0.9059(3) 0.31137(15) 0.0523(7) Uani 1 1 d . . . C15 C 0.83684(18) 0.6998(3) 0.32356(14) 0.0515(7) Uani 1 1 d . . . C16 C 1.10166(19) 0.7710(4) 0.44051(18) 0.0646(9) Uani 1 1 d . . . H16A H 1.1105 0.7513 0.4047 0.078 Uiso 1 1 calc R . . H16B H 1.1411 0.8245 0.4657 0.078 Uiso 1 1 calc R . . C17 C 1.1033(2) 0.6474(4) 0.47283(17) 0.0701(10) Uani 1 1 d . . . H17A H 1.1507 0.6095 0.4841 0.084 Uiso 1 1 calc R . . H17B H 1.0959 0.6666 0.5093 0.084 Uiso 1 1 calc R . . C18 C 1.0488(2) 0.5503(4) 0.43785(16) 0.0604(9) Uani 1 1 d . . . H18A H 1.0576 0.4710 0.4609 0.073 Uiso 1 1 calc R . . H18B H 1.0565 0.5318 0.4014 0.073 Uiso 1 1 calc R . . C32 C 0.78291(17) 0.6814(4) 0.17182(15) 0.0567(8) Uani 1 1 d . . . C33 C 0.7217(2) 0.7594(5) 0.15094(18) 0.0771(13) Uani 1 1 d . . . H33A H 0.6785 0.7304 0.1521 0.092 Uiso 1 1 calc R . . C34 C 0.7264(3) 0.8787(5) 0.12894(19) 0.0853(15) Uani 1 1 d . . . H34A H 0.6868 0.9333 0.1160 0.102 Uiso 1 1 calc R . . C35 C 0.7904(3) 0.9170(5) 0.1262(2) 0.0870(14) Uani 1 1 d . . . H35A H 0.7942 0.9973 0.1105 0.104 Uiso 1 1 calc R . . C36 C 0.8495(2) 0.8350(4) 0.14704(16) 0.0674(10) Uani 1 1 d . . . H36A H 0.8926 0.8620 0.1451 0.081 Uiso 1 1 calc R . . C37 C 0.78571(17) 0.5564(4) 0.19855(17) 0.0626(10) Uani 1 1 d . . . H37A H 0.7458 0.5204 0.2031 0.075 Uiso 1 1 calc R . . C38 C 0.8588(2) 0.3758(4) 0.2497(2) 0.0699(10) Uani 1 1 d . . . H38A H 0.8137 0.3310 0.2413 0.084 Uiso 1 1 calc R . . H38B H 0.8804 0.3932 0.2922 0.084 Uiso 1 1 calc R . . C39 C 0.9090(2) 0.2933(4) 0.2307(2) 0.0753(12) Uani 1 1 d . . . H39A H 0.8854 0.2671 0.1893 0.090 Uiso 1 1 calc R . . H39B H 0.9231 0.2165 0.2554 0.090 Uiso 1 1 calc R . . C42 C 0.9329(2) 0.5787(4) 0.08597(15) 0.0660(10) Uani 1 1 d . . . C43 C 0.9180(3) 0.5581(7) 0.0254(2) 0.1081(19) Uani 1 1 d . . . H43A H 0.9465 0.5948 0.0070 0.130 Uiso 1 1 calc R . . C44 C 0.8598(4) 0.4817(9) -0.0064(2) 0.144(3) Uani 1 1 d . . . H44A H 0.8484 0.4680 -0.0470 0.173 Uiso 1 1 calc R . . C45 C 0.8193(4) 0.4267(8) 0.0206(3) 0.128(3) Uani 1 1 d . . . H45A H 0.7801 0.3752 -0.0008 0.153 Uiso 1 1 calc R . . C46 C 0.8374(3) 0.4485(5) 0.0810(2) 0.0897(15) Uani 1 1 d . . . H46A H 0.8097 0.4100 0.0997 0.108 Uiso 1 1 calc R . . C47 C 0.9913(2) 0.6570(4) 0.12475(16) 0.0622(9) Uani 1 1 d . . . H47A H 1.0239 0.6967 0.1114 0.075 Uiso 1 1 calc R . . C48 C 1.05196(19) 0.7441(4) 0.22232(17) 0.0574(8) Uani 1 1 d . . . H48A H 1.0681 0.8109 0.2023 0.069 Uiso 1 1 calc R . . H48B H 1.0926 0.6891 0.2439 0.069 Uiso 1 1 calc R . . C49 C 1.02231(19) 0.8050(3) 0.26582(16) 0.0543(8) Uani 1 1 d . . . H49A H 0.9870 0.8705 0.2457 0.065 Uiso 1 1 calc R . . H49B H 1.0607 0.8450 0.2989 0.065 Uiso 1 1 calc R . . O1 O 1.2575(2) 0.3056(4) 0.17092(18) 0.1104(13) Uani 1 1 d . . . O2 O 1.32731(17) 0.1418(4) 0.34977(15) 0.0927(10) Uani 1 1 d . . . O3 O 1.15619(18) -0.0363(3) 0.18162(18) 0.0935(10) Uani 1 1 d . . . O4 O 1.0612(2) 0.3869(4) 0.09826(14) 0.1031(12) Uani 1 1 d . . . O5 O 0.9719(2) 0.0715(4) 0.1448(2) 0.1203(14) Uani 1 1 d . . . O11 O 1.02639(16) 0.7794(3) 0.58778(11) 0.0746(8) Uani 1 1 d . . . O12 O 0.80823(16) 0.6787(3) 0.46164(15) 0.0837(9) Uani 1 1 d . . . O13 O 0.86689(17) 1.0335(3) 0.43957(14) 0.0794(8) Uani 1 1 d . . . O14 O 0.87607(16) 1.0007(3) 0.28553(15) 0.0813(8) Uani 1 1 d . . . O15 O 0.77828(14) 0.6658(3) 0.31077(13) 0.0772(8) Uani 1 1 d . . . 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 0.0379(2) 0.0462(3) 0.0371(2) 0.00056(15) 0.01823(16) -0.00145(15) Fe5 0.0379(2) 0.0462(3) 0.0371(2) 0.00056(15) 0.01823(16) -0.00145(15) Fe1 0.0514(2) 0.0500(3) 0.0610(3) 0.0054(2) 0.0280(2) 0.0058(2) Fe2 0.0494(2) 0.0486(3) 0.0505(3) 0.00082(19) 0.0233(2) 0.00164(18) Fe3 0.0506(2) 0.0437(2) 0.0376(2) -0.00389(16) 0.01840(18) 0.00004(17) Fe4 0.0465(2) 0.0388(2) 0.0359(2) 0.00152(15) 0.01649(17) 0.00251(16) S1 0.0666(5) 0.0589(5) 0.0768(6) 0.0205(4) 0.0390(5) 0.0058(4) S2 0.0559(4) 0.0500(4) 0.0589(5) -0.0013(4) 0.0291(4) -0.0022(3) S3 0.0509(4) 0.0499(4) 0.0547(4) 0.0058(3) 0.0278(3) 0.0029(3) S4 0.0536(4) 0.0464(4) 0.0532(4) -0.0067(3) 0.0226(3) -0.0067(3) S5 0.0577(4) 0.0384(4) 0.0425(4) 0.0026(3) 0.0212(3) 0.0026(3) S6 0.0446(3) 0.0426(4) 0.0388(3) 0.0001(3) 0.0184(3) -0.0013(3) N1 0.0509(14) 0.0635(17) 0.0368(12) -0.0021(11) 0.0136(11) 0.0084(12) N2 0.0457(13) 0.0593(16) 0.0527(14) -0.0089(12) 0.0264(11) -0.0079(12) N3 0.0564(15) 0.0698(19) 0.0528(15) -0.0081(14) 0.0221(13) -0.0006(14) N4 0.0495(13) 0.0508(14) 0.0448(13) 0.0063(11) 0.0242(11) 0.0040(11) C1 0.075(2) 0.066(2) 0.081(3) -0.001(2) 0.046(2) 0.0036(19) C2 0.065(2) 0.065(2) 0.075(2) 0.0098(19) 0.037(2) 0.0103(18) C3 0.061(2) 0.059(2) 0.092(3) 0.000(2) 0.036(2) 0.0034(17) C4 0.069(2) 0.066(2) 0.0521(19) 0.0015(16) 0.0263(16) 0.0114(18) C5 0.073(2) 0.070(3) 0.079(3) -0.011(2) 0.029(2) -0.007(2) C6 0.094(3) 0.111(4) 0.066(2) 0.024(2) 0.047(2) 0.014(3) C7 0.081(3) 0.116(4) 0.049(2) 0.001(2) 0.0216(19) 0.014(3) C8 0.066(2) 0.087(3) 0.061(2) -0.018(2) 0.0257(18) -0.003(2) C11 0.0590(18) 0.0541(19) 0.0506(18) -0.0059(14) 0.0235(15) -0.0030(15) C12 0.062(2) 0.060(2) 0.0513(18) -0.0045(15) 0.0256(15) 0.0017(16) C13 0.0583(18) 0.055(2) 0.0492(17) -0.0040(14) 0.0201(14) -0.0015(15) C14 0.0551(17) 0.0515(18) 0.0556(18) 0.0055(15) 0.0271(14) 0.0064(14) C15 0.0575(18) 0.0558(19) 0.0417(15) 0.0008(13) 0.0194(13) 0.0021(15) C16 0.0487(18) 0.078(3) 0.066(2) -0.0066(19) 0.0200(16) -0.0038(17) C17 0.0561(19) 0.093(3) 0.055(2) 0.005(2) 0.0143(16) 0.015(2) C18 0.068(2) 0.057(2) 0.0593(19) 0.0140(16) 0.0280(17) 0.0204(17) C32 0.0434(15) 0.077(2) 0.0463(16) -0.0169(16) 0.0131(13) 0.0082(15) C33 0.0458(18) 0.111(4) 0.062(2) -0.034(2) 0.0064(16) 0.017(2) C34 0.076(3) 0.095(4) 0.062(2) -0.017(2) 0.002(2) 0.036(3) C35 0.099(3) 0.081(3) 0.065(3) 0.009(2) 0.014(2) 0.034(3) C36 0.071(2) 0.073(2) 0.054(2) 0.0094(18) 0.0195(17) 0.0173(19) C37 0.0386(14) 0.087(3) 0.067(2) -0.0258(19) 0.0256(15) -0.0096(16) C38 0.067(2) 0.071(2) 0.092(3) 0.004(2) 0.053(2) -0.0143(19) C39 0.080(3) 0.052(2) 0.115(3) 0.008(2) 0.060(3) -0.0107(19) C42 0.069(2) 0.091(3) 0.0427(17) -0.0041(17) 0.0266(16) 0.006(2) C43 0.123(4) 0.162(6) 0.052(2) -0.019(3) 0.048(3) -0.011(4) C44 0.136(5) 0.234(9) 0.059(3) -0.060(4) 0.033(3) -0.031(6) C45 0.110(4) 0.190(7) 0.083(4) -0.063(4) 0.036(3) -0.033(5) C46 0.081(3) 0.111(4) 0.074(3) -0.040(3) 0.027(2) -0.026(3) C47 0.066(2) 0.079(2) 0.0547(19) 0.0110(18) 0.0374(17) 0.0056(18) C48 0.0527(17) 0.060(2) 0.068(2) 0.0037(16) 0.0319(16) -0.0138(15) C49 0.0599(18) 0.0476(17) 0.0584(19) -0.0025(14) 0.0259(15) -0.0129(14) O1 0.137(3) 0.120(3) 0.115(3) 0.009(2) 0.093(3) -0.008(3) O2 0.0709(18) 0.119(3) 0.079(2) 0.0143(19) 0.0174(16) 0.0252(19) O3 0.088(2) 0.0673(19) 0.130(3) -0.028(2) 0.047(2) -0.0071(16) O4 0.134(3) 0.127(3) 0.0599(18) 0.0189(18) 0.051(2) 0.022(2) O5 0.124(3) 0.105(3) 0.119(3) -0.044(2) 0.032(2) -0.045(2) O11 0.0823(18) 0.095(2) 0.0394(13) -0.0027(13) 0.0146(12) -0.0036(15) O12 0.0694(17) 0.099(2) 0.094(2) -0.0118(18) 0.0437(16) -0.0172(16) O13 0.0873(19) 0.0577(16) 0.086(2) -0.0024(14) 0.0243(16) 0.0191(15) O14 0.0908(19) 0.0624(17) 0.100(2) 0.0350(16) 0.0470(17) 0.0240(15) O15 0.0534(14) 0.098(2) 0.0716(17) 0.0037(16) 0.0141(12) -0.0126(14) _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 N2 1.937(3) . ? Ni1 N4 1.940(3) . ? Ni1 N3 2.020(3) . ? Ni1 N1 2.037(3) . ? Ni1 S6 2.3256(9) . ? Ni1 S3 2.3312(10) . ? Fe1 C1 1.780(4) . ? Fe1 C3 1.786(4) . ? Fe1 C2 1.799(4) . ? Fe1 S2 2.2688(10) . ? Fe1 S1 2.2749(11) . ? Fe1 Fe2 2.5103(8) . ? Fe2 C5 1.743(4) . ? Fe2 C4 1.758(4) . ? Fe2 S2 2.2725(10) . ? Fe2 S3 2.2749(9) . ? Fe2 S1 2.2790(11) . ? Fe3 C12 1.776(4) . ? Fe3 C13 1.776(4) . ? Fe3 C11 1.817(3) . ? Fe3 S5 2.2772(9) . ? Fe3 S4 2.2844(10) . ? Fe3 Fe4 2.5121(8) . ? Fe4 C15 1.756(4) . ? Fe4 C14 1.757(3) . ? Fe4 S4 2.2653(9) . ? Fe4 S6 2.2789(9) . ? Fe4 S5 2.2821(9) . ? S1 C6 1.833(5) . ? S2 C8 1.815(4) . ? S3 C39 1.813(4) . ? S4 C16 1.835(4) . ? S5 C18 1.821(4) . ? S6 C49 1.827(3) . ? N1 C36 1.338(5) . ? N1 C32 1.352(4) . ? N2 C37 1.288(4) . ? N2 C38 1.469(5) . ? N3 C46 1.342(5) . ? N3 C42 1.358(5) . ? N4 C47 1.277(4) . ? N4 C48 1.457(4) . ? C1 O1 1.141(5) . ? C2 O2 1.141(5) . ? C3 O3 1.129(5) . ? C4 O4 1.137(5) . ? C5 O5 1.150(5) . ? C6 C7 1.483(7) . ? C7 C8 1.502(6) . ? C11 O11 1.137(4) . ? C12 O12 1.143(4) . ? C13 O13 1.141(4) . ? C14 O14 1.153(4) . ? C15 O15 1.155(4) . ? C16 C17 1.495(6) . ? C17 C18 1.493(6) . ? C32 C33 1.398(5) . ? C32 C37 1.440(6) . ? C33 C34 1.363(7) . ? C34 C35 1.375(8) . ? C35 C36 1.392(6) . ? C38 C39 1.521(6) . ? C42 C43 1.395(5) . ? C42 C47 1.444(6) . ? C43 C44 1.382(9) . ? C44 C45 1.350(10) . ? C45 C46 1.382(7) . ? C48 C49 1.529(5) . ? 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 N4 175.92(11) . . ? N2 Ni1 N3 97.10(12) . . ? N4 Ni1 N3 80.30(12) . . ? N2 Ni1 N1 79.84(12) . . ? N4 Ni1 N1 96.83(11) . . ? N3 Ni1 N1 87.08(11) . . ? N2 Ni1 S6 97.86(8) . . ? N4 Ni1 S6 84.69(8) . . ? N3 Ni1 S6 164.99(9) . . ? N1 Ni1 S6 94.40(8) . . ? N2 Ni1 S3 84.18(9) . . ? N4 Ni1 S3 99.15(8) . . ? N3 Ni1 S3 95.15(10) . . ? N1 Ni1 S3 164.01(9) . . ? S6 Ni1 S3 87.54(3) . . ? C1 Fe1 C3 90.86(19) . . ? C1 Fe1 C2 96.5(2) . . ? C3 Fe1 C2 103.43(19) . . ? C1 Fe1 S2 87.21(13) . . ? C3 Fe1 S2 148.06(14) . . ? C2 Fe1 S2 108.47(14) . . ? C1 Fe1 S1 162.09(15) . . ? C3 Fe1 S1 87.07(13) . . ? C2 Fe1 S1 101.30(13) . . ? S2 Fe1 S1 85.21(4) . . ? C1 Fe1 Fe2 105.84(15) . . ? C3 Fe1 Fe2 93.72(13) . . ? C2 Fe1 Fe2 151.60(13) . . ? S2 Fe1 Fe2 56.51(3) . . ? S1 Fe1 Fe2 56.63(3) . . ? C5 Fe2 C4 90.8(2) . . ? C5 Fe2 S2 165.64(15) . . ? C4 Fe2 S2 89.90(14) . . ? C5 Fe2 S3 99.87(15) . . ? C4 Fe2 S3 107.17(12) . . ? S2 Fe2 S3 93.63(4) . . ? C5 Fe2 S1 88.19(16) . . ? C4 Fe2 S1 154.23(12) . . ? S2 Fe2 S1 85.02(4) . . ? S3 Fe2 S1 98.37(4) . . ? C5 Fe2 Fe1 109.44(15) . . ? C4 Fe2 Fe1 100.03(12) . . ? S2 Fe2 Fe1 56.37(3) . . ? S3 Fe2 Fe1 139.41(3) . . ? S1 Fe2 Fe1 56.47(3) . . ? C12 Fe3 C13 87.98(17) . . ? C12 Fe3 C11 97.85(16) . . ? C13 Fe3 C11 102.98(16) . . ? C12 Fe3 S5 86.69(12) . . ? C13 Fe3 S5 148.76(11) . . ? C11 Fe3 S5 108.24(11) . . ? C12 Fe3 S4 159.19(12) . . ? C13 Fe3 S4 88.96(12) . . ? C11 Fe3 S4 102.89(12) . . ? S5 Fe3 S4 85.30(3) . . ? C12 Fe3 Fe4 103.68(11) . . ? C13 Fe3 Fe4 95.04(11) . . ? C11 Fe3 Fe4 152.32(11) . . ? S5 Fe3 Fe4 56.66(2) . . ? S4 Fe3 Fe4 56.12(3) . . ? C15 Fe4 C14 91.60(16) . . ? C15 Fe4 S4 152.73(11) . . ? C14 Fe4 S4 89.37(12) . . ? C15 Fe4 S6 107.50(11) . . ? C14 Fe4 S6 98.13(11) . . ? S4 Fe4 S6 99.32(4) . . ? C15 Fe4 S5 87.28(11) . . ? C14 Fe4 S5 166.72(11) . . ? S4 Fe4 S5 85.63(3) . . ? S6 Fe4 S5 94.82(3) . . ? C15 Fe4 Fe3 97.66(10) . . ? C14 Fe4 Fe3 110.68(11) . . ? S4 Fe4 Fe3 56.85(3) . . ? S6 Fe4 Fe3 141.00(3) . . ? S5 Fe4 Fe3 56.47(3) . . ? C6 S1 Fe1 112.65(17) . . ? C6 S1 Fe2 111.16(16) . . ? Fe1 S1 Fe2 66.90(3) . . ? C8 S2 Fe1 112.90(15) . . ? C8 S2 Fe2 111.77(14) . . ? Fe1 S2 Fe2 67.11(3) . . ? C39 S3 Fe2 109.70(14) . . ? C39 S3 Ni1 96.20(14) . . ? Fe2 S3 Ni1 128.53(4) . . ? C16 S4 Fe4 111.45(13) . . ? C16 S4 Fe3 112.28(14) . . ? Fe4 S4 Fe3 67.03(3) . . ? C18 S5 Fe3 113.09(13) . . ? C18 S5 Fe4 110.49(12) . . ? Fe3 S5 Fe4 66.87(3) . . ? C49 S6 Fe4 109.43(12) . . ? C49 S6 Ni1 95.41(11) . . ? Fe4 S6 Ni1 125.16(4) . . ? C36 N1 C32 117.7(3) . . ? C36 N1 Ni1 129.3(3) . . ? C32 N1 Ni1 112.9(2) . . ? C37 N2 C38 122.0(3) . . ? C37 N2 Ni1 117.2(3) . . ? C38 N2 Ni1 120.8(2) . . ? C46 N3 C42 118.0(4) . . ? C46 N3 Ni1 129.5(3) . . ? C42 N3 Ni1 112.3(2) . . ? C47 N4 C48 121.3(3) . . ? C47 N4 Ni1 117.4(2) . . ? C48 N4 Ni1 121.2(2) . . ? O1 C1 Fe1 179.4(5) . . ? O2 C2 Fe1 178.4(4) . . ? O3 C3 Fe1 178.2(5) . . ? O4 C4 Fe2 174.2(4) . . ? O5 C5 Fe2 178.6(4) . . ? C7 C6 S1 116.5(3) . . ? C6 C7 C8 114.4(4) . . ? C7 C8 S2 116.7(3) . . ? O11 C11 Fe3 178.3(3) . . ? O12 C12 Fe3 178.5(4) . . ? O13 C13 Fe3 174.4(3) . . ? O14 C14 Fe4 178.8(3) . . ? O15 C15 Fe4 173.1(3) . . ? C17 C16 S4 116.7(3) . . ? C18 C17 C16 114.6(3) . . ? C17 C18 S5 116.5(3) . . ? N1 C32 C33 122.5(4) . . ? N1 C32 C37 113.3(3) . . ? C33 C32 C37 124.2(4) . . ? C34 C33 C32 118.9(4) . . ? C33 C34 C35 119.1(4) . . ? C34 C35 C36 119.6(5) . . ? N1 C36 C35 122.1(4) . . ? N2 C37 C32 116.5(3) . . ? N2 C38 C39 107.7(3) . . ? C38 C39 S3 106.7(3) . . ? N3 C42 C43 121.5(4) . . ? N3 C42 C47 114.1(3) . . ? C43 C42 C47 124.4(4) . . ? C44 C43 C42 118.1(5) . . ? C45 C44 C43 120.8(5) . . ? C44 C45 C46 118.5(6) . . ? N3 C46 C45 123.0(5) . . ? N4 C47 C42 115.7(3) . . ? N4 C48 C49 108.8(3) . . ? C48 C49 S6 106.9(2) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.480 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.072 # Attachment '- 776577.cif' data_B2 _database_code_depnum_ccdc_archive 'CCDC 776577' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-[(pentacarbonylpropanedithiolatodiiron)-sulfanylpropyliminomethylpyridine] nickel(ii) ; _chemical_name_common ; bis-((pentacarbonylpropanedithiolatodiiron)- sulfanylpropyliminomethylpyridine) nickel(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Fe4 N4 Ni O10 S6' _chemical_formula_sum 'C32 H30 Fe4 N4 Ni O10 S6' _chemical_formula_weight 1105.07 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.100(6) _cell_length_b 10.429(3) _cell_length_c 24.241(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.275(4) _cell_angle_gamma 90.00 _cell_volume 4702(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8424 _cell_measurement_theta_min 3.0588 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.915 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7603 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury70 (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35264 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10722 _reflns_number_gt 7750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 315 44 ' ' 2 0.795 0.055 0.589 9 1 ' ' 3 0.499 0.501 0.500 315 44 ' ' 4 0.297 0.451 0.091 9 1 ' ' 5 0.703 0.549 0.909 8 0 ' ' 6 0.203 0.951 0.409 8 1 ' ' _platon_squeeze_details ; ; _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^)+(0.0528P)^2^+0.7292P] 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 10722 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1313 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.92368(3) 0.57670(5) 0.19937(2) 0.04605(14) Uani 1 1 d . . . Fe1 Fe 1.19140(3) 0.19733(6) 0.24997(3) 0.05765(17) Uani 1 1 d . . . Fe2 Fe 1.06327(3) 0.27317(6) 0.20917(3) 0.05361(16) Uani 1 1 d . . . Fe3 Fe 0.94105(3) 0.78486(5) 0.45773(2) 0.04774(15) Uani 1 1 d . . . Fe4 Fe 0.92633(3) 0.75761(5) 0.35071(2) 0.04369(14) Uani 1 1 d . . . S1 S 1.10882(7) 0.13710(12) 0.28822(6) 0.0700(3) Uani 1 1 d . . . S2 S 1.15803(6) 0.40095(11) 0.26067(5) 0.0577(3) Uani 1 1 d . . . S3 S 0.98517(6) 0.38444(11) 0.23894(5) 0.0551(3) Uani 1 1 d . . . S4 S 0.95664(6) 0.59419(9) 0.41828(4) 0.0500(2) Uani 1 1 d . . . S5 S 1.01968(6) 0.86493(11) 0.41861(5) 0.0551(3) Uani 1 1 d . . . S6 S 0.98259(5) 0.67156(9) 0.29337(4) 0.0453(2) Uani 1 1 d . . . N1 N 0.84493(18) 0.7186(4) 0.16921(15) 0.0570(9) Uani 1 1 d . . . N2 N 0.84427(17) 0.4941(3) 0.21396(16) 0.0556(9) Uani 1 1 d . . . N3 N 0.89279(19) 0.5245(4) 0.11089(17) 0.0630(10) Uani 1 1 d . . . N4 N 0.99684(17) 0.6660(3) 0.17815(14) 0.0491(8) Uani 1 1 d . . . O1 O 1.3267(2) 0.1370(4) 0.34927(18) 0.1011(13) Uani 1 1 d . . . O2 O 1.1573(2) -0.0399(4) 0.1814(2) 0.1013(13) Uani 1 1 d . . . O3 O 1.2567(3) 0.3025(4) 0.1706(2) 0.1142(15) Uani 1 1 d . . . O4 O 0.9719(3) 0.0641(5) 0.1439(2) 0.1281(17) Uani 1 1 d . . . O5 O 1.0574(3) 0.3833(4) 0.09785(17) 0.1098(14) Uani 1 1 d . . . O11 O 1.02579(19) 0.7790(4) 0.58725(14) 0.0809(10) Uani 1 1 d . . . O12 O 0.86761(19) 1.0326(3) 0.43907(17) 0.0834(10) Uani 1 1 d . . . O13 O 0.80756(19) 0.6799(4) 0.45988(17) 0.0885(11) Uani 1 1 d . . . O14 O 0.8770(2) 0.9959(3) 0.28561(17) 0.0876(11) Uani 1 1 d . . . O15 O 0.78041(18) 0.6589(4) 0.30888(15) 0.0818(10) Uani 1 1 d . . . C1 C 1.2738(3) 0.1612(5) 0.3108(2) 0.0713(13) Uani 1 1 d . . . C2 C 1.1712(3) 0.0529(5) 0.2093(3) 0.0755(14) Uani 1 1 d . . . C3 C 1.2309(3) 0.2608(5) 0.2018(3) 0.0743(14) Uani 1 1 d . . . C4 C 1.0079(3) 0.1471(6) 0.1699(3) 0.0814(15) Uani 1 1 d . . . C5 C 1.0582(3) 0.3446(5) 0.1425(2) 0.0715(13) Uani 1 1 d . . . C6 C 1.1214(3) 0.2184(6) 0.3585(3) 0.0944(18) Uani 1 1 d . . . H6A H 1.0758 0.2556 0.3550 0.113 Uiso 1 1 calc R . . H6B H 1.1338 0.1544 0.3898 0.113 Uiso 1 1 calc R . . C7 C 1.1778(3) 0.3228(7) 0.3779(2) 0.0955(19) Uani 1 1 d . . . H7A H 1.1822 0.3537 0.4168 0.115 Uiso 1 1 calc R . . H7B H 1.2238 0.2862 0.3819 0.115 Uiso 1 1 calc R . . C8 C 1.1619(3) 0.4341(5) 0.3358(2) 0.0792(15) Uani 1 1 d . . . H8A H 1.1984 0.4991 0.3535 0.095 Uiso 1 1 calc R . . H8B H 1.1161 0.4705 0.3325 0.095 Uiso 1 1 calc R . . C11 C 0.9945(2) 0.7815(4) 0.5372(2) 0.0576(11) Uani 1 1 d . . . C12 C 0.8992(2) 0.9387(4) 0.44752(19) 0.0583(11) Uani 1 1 d . . . C13 C 0.8606(3) 0.7199(4) 0.4593(2) 0.0592(11) Uani 1 1 d . . . C14 C 0.8969(2) 0.9013(4) 0.3113(2) 0.0576(11) Uani 1 1 d . . . C15 C 0.8388(2) 0.6952(4) 0.32310(17) 0.0527(10) Uani 1 1 d . . . C16 C 1.0500(2) 0.5499(4) 0.4382(2) 0.0623(12) Uani 1 1 d . . . H16A H 1.0587 0.4712 0.4612 0.075 Uiso 1 1 calc R . . H16B H 1.0577 0.5316 0.4019 0.075 Uiso 1 1 calc R . . C17 C 1.1042(3) 0.6469(5) 0.4731(2) 0.0750(14) Uani 1 1 d . . . H17A H 1.1517 0.6094 0.4845 0.090 Uiso 1 1 calc R . . H17B H 1.0965 0.6658 0.5094 0.090 Uiso 1 1 calc R . . C18 C 1.1029(2) 0.7709(5) 0.4411(2) 0.0719(13) Uani 1 1 d . . . H18A H 1.1125 0.7518 0.4056 0.086 Uiso 1 1 calc R . . H18B H 1.1421 0.8240 0.4666 0.086 Uiso 1 1 calc R . . C32 C 0.7818(2) 0.6804(5) 0.17079(19) 0.0603(12) Uani 1 1 d . . . C33 C 0.7202(3) 0.7559(6) 0.1508(2) 0.0809(17) Uani 1 1 d . . . H33A H 0.6771 0.7265 0.1519 0.097 Uiso 1 1 calc R . . C34 C 0.7257(3) 0.8761(7) 0.1293(2) 0.096(2) Uani 1 1 d . . . H34A H 0.6857 0.9297 0.1158 0.116 Uiso 1 1 calc R . . C35 C 0.7890(4) 0.9169(6) 0.1275(2) 0.0931(18) Uani 1 1 d . . . H35A H 0.7930 0.9982 0.1132 0.112 Uiso 1 1 calc R . . C36 C 0.8474(3) 0.8353(5) 0.1474(2) 0.0752(14) Uani 1 1 d . . . H36A H 0.8905 0.8628 0.1455 0.090 Uiso 1 1 calc R . . C37 C 0.7838(2) 0.5535(5) 0.1965(2) 0.0661(13) Uani 1 1 d . . . H37A H 0.7434 0.5173 0.2001 0.079 Uiso 1 1 calc R . . C38 C 0.8554(3) 0.3720(5) 0.2455(3) 0.0810(15) Uani 1 1 d . . . H38A H 0.8098 0.3286 0.2361 0.097 Uiso 1 1 calc R . . H38B H 0.8764 0.3867 0.2882 0.097 Uiso 1 1 calc R . . C39 C 0.9052(3) 0.2898(4) 0.2269(3) 0.0824(16) Uani 1 1 d . . . H39A H 0.8823 0.2662 0.1852 0.099 Uiso 1 1 calc R . . H39B H 0.9175 0.2120 0.2506 0.099 Uiso 1 1 calc R . . C42 C 0.9333(3) 0.5821(5) 0.0846(2) 0.0686(13) Uani 1 1 d . . . C43 C 0.9194(4) 0.5670(7) 0.0244(3) 0.116(2) Uani 1 1 d . . . H43A H 0.9486 0.6055 0.0072 0.139 Uiso 1 1 calc R . . C44 C 0.8616(5) 0.4940(10) -0.0091(3) 0.153(4) Uani 1 1 d . . . H44A H 0.8510 0.4838 -0.0497 0.184 Uiso 1 1 calc R . . C45 C 0.8189(5) 0.4354(9) 0.0167(4) 0.150(3) Uani 1 1 d . . . H45A H 0.7795 0.3855 -0.0057 0.180 Uiso 1 1 calc R . . C46 C 0.8367(3) 0.4534(6) 0.0769(3) 0.0971(19) Uani 1 1 d . . . H46A H 0.8084 0.4144 0.0948 0.116 Uiso 1 1 calc R . . C47 C 0.9917(2) 0.6581(5) 0.1248(2) 0.0640(12) Uani 1 1 d . . . H47A H 1.0241 0.6996 0.1118 0.077 Uiso 1 1 calc R . . C48 C 1.0537(2) 0.7402(4) 0.2231(2) 0.0600(11) Uani 1 1 d . . . H48A H 1.0708 0.8069 0.2039 0.072 Uiso 1 1 calc R . . H48B H 1.0939 0.6846 0.2447 0.072 Uiso 1 1 calc R . . C49 C 1.0240(2) 0.7992(4) 0.2657(2) 0.0571(11) Uani 1 1 d . . . H49A H 0.9885 0.8640 0.2454 0.069 Uiso 1 1 calc R . . H49B H 1.0623 0.8396 0.2986 0.069 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 0.0446(2) 0.0524(3) 0.0441(3) 0.0009(2) 0.0202(2) -0.0018(2) Fe1 0.0570(3) 0.0540(4) 0.0672(4) 0.0062(3) 0.0295(3) 0.0058(3) Fe2 0.0551(3) 0.0528(4) 0.0559(4) 0.0016(3) 0.0244(3) 0.0021(3) Fe3 0.0557(3) 0.0472(3) 0.0408(3) -0.0038(2) 0.0188(3) 0.0003(3) Fe4 0.0514(3) 0.0414(3) 0.0386(3) 0.0016(2) 0.0174(2) 0.0028(2) S1 0.0720(7) 0.0624(7) 0.0863(9) 0.0222(7) 0.0420(7) 0.0066(6) S2 0.0616(6) 0.0535(6) 0.0634(7) -0.0011(5) 0.0296(6) -0.0016(5) S3 0.0561(6) 0.0544(6) 0.0610(6) 0.0067(5) 0.0291(5) 0.0038(5) S4 0.0641(6) 0.0417(5) 0.0462(5) 0.0035(4) 0.0231(5) 0.0048(5) S5 0.0585(6) 0.0510(6) 0.0571(6) -0.0080(5) 0.0232(5) -0.0076(5) S6 0.0504(5) 0.0449(5) 0.0430(5) 0.0003(4) 0.0204(4) -0.0004(4) N1 0.0518(19) 0.071(3) 0.0460(19) -0.0031(18) 0.0157(16) 0.0090(18) N2 0.0526(19) 0.061(2) 0.061(2) -0.0052(18) 0.0309(17) -0.0059(17) N3 0.062(2) 0.069(2) 0.060(2) -0.0125(19) 0.0245(19) -0.0029(19) N4 0.0530(18) 0.051(2) 0.0482(19) 0.0062(15) 0.0251(16) 0.0033(16) O1 0.077(2) 0.130(4) 0.090(3) 0.023(3) 0.024(2) 0.030(2) O2 0.097(3) 0.074(3) 0.138(4) -0.028(3) 0.051(3) -0.010(2) O3 0.135(4) 0.122(4) 0.120(4) 0.011(3) 0.087(3) -0.007(3) O4 0.124(4) 0.114(4) 0.128(4) -0.040(3) 0.028(3) -0.050(3) O5 0.146(4) 0.130(4) 0.067(2) 0.020(2) 0.055(3) 0.023(3) O11 0.086(2) 0.106(3) 0.0401(17) -0.0019(18) 0.0124(17) -0.001(2) O12 0.092(2) 0.061(2) 0.089(3) 0.0000(19) 0.024(2) 0.020(2) O13 0.075(2) 0.100(3) 0.101(3) -0.012(2) 0.045(2) -0.017(2) O14 0.100(3) 0.068(2) 0.105(3) 0.036(2) 0.050(2) 0.029(2) O15 0.0611(19) 0.102(3) 0.073(2) 0.009(2) 0.0151(18) -0.0086(19) C1 0.066(3) 0.074(3) 0.080(3) 0.007(3) 0.035(3) 0.009(3) C2 0.064(3) 0.061(3) 0.108(4) -0.005(3) 0.041(3) 0.001(3) C3 0.084(3) 0.069(3) 0.086(4) -0.001(3) 0.050(3) 0.003(3) C4 0.076(3) 0.080(4) 0.084(4) -0.010(3) 0.025(3) -0.011(3) C5 0.079(3) 0.077(3) 0.057(3) 0.000(3) 0.025(3) 0.012(3) C6 0.104(4) 0.121(5) 0.075(4) 0.030(3) 0.052(4) 0.017(4) C7 0.090(4) 0.142(6) 0.058(3) 0.006(4) 0.031(3) 0.022(4) C8 0.073(3) 0.096(4) 0.072(3) -0.020(3) 0.031(3) 0.000(3) C11 0.062(2) 0.058(3) 0.056(3) -0.005(2) 0.026(2) -0.002(2) C12 0.064(3) 0.059(3) 0.048(2) -0.003(2) 0.017(2) -0.003(2) C13 0.069(3) 0.056(3) 0.054(3) -0.009(2) 0.025(2) -0.001(2) C14 0.059(2) 0.059(3) 0.061(3) 0.008(2) 0.030(2) 0.011(2) C15 0.061(2) 0.057(3) 0.039(2) 0.0054(19) 0.017(2) 0.007(2) C16 0.073(3) 0.058(3) 0.059(3) 0.015(2) 0.029(2) 0.021(2) C17 0.064(3) 0.095(4) 0.061(3) 0.009(3) 0.018(2) 0.023(3) C18 0.054(2) 0.089(4) 0.072(3) -0.011(3) 0.023(2) -0.001(2) C32 0.047(2) 0.081(3) 0.046(2) -0.019(2) 0.0092(19) 0.006(2) C33 0.051(3) 0.109(5) 0.066(3) -0.033(3) 0.004(2) 0.017(3) C34 0.086(4) 0.116(5) 0.062(3) -0.026(3) -0.002(3) 0.050(4) C35 0.105(4) 0.087(4) 0.072(4) 0.012(3) 0.016(3) 0.043(4) C36 0.082(3) 0.076(3) 0.061(3) 0.015(3) 0.019(3) 0.016(3) C37 0.043(2) 0.090(4) 0.068(3) -0.027(3) 0.025(2) -0.007(2) C38 0.074(3) 0.077(4) 0.114(4) 0.004(3) 0.060(3) -0.012(3) C39 0.087(3) 0.052(3) 0.131(5) 0.012(3) 0.068(4) -0.008(3) C42 0.075(3) 0.087(4) 0.045(2) -0.004(2) 0.024(2) 0.011(3) C43 0.120(5) 0.179(7) 0.054(3) -0.024(4) 0.041(4) -0.014(5) C44 0.145(7) 0.244(11) 0.063(4) -0.063(6) 0.030(5) -0.014(7) C45 0.133(6) 0.204(9) 0.111(6) -0.088(6) 0.043(5) -0.038(6) C46 0.083(4) 0.118(5) 0.087(4) -0.037(4) 0.029(3) -0.017(4) C47 0.065(3) 0.083(3) 0.057(3) 0.012(2) 0.038(2) 0.006(2) C48 0.055(2) 0.062(3) 0.070(3) 0.004(2) 0.031(2) -0.011(2) C49 0.065(2) 0.049(2) 0.061(3) -0.004(2) 0.028(2) -0.013(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 N2 1.960(3) . ? Ni1 N4 1.966(3) . ? Ni1 N3 2.067(4) . ? Ni1 N1 2.086(3) . ? Ni1 S6 2.3512(12) . ? Ni1 S3 2.3599(13) . ? Fe1 C2 1.761(6) . ? Fe1 C3 1.771(5) . ? Fe1 C1 1.790(5) . ? Fe1 S2 2.2712(14) . ? Fe1 S1 2.2752(14) . ? Fe1 Fe2 2.5111(10) . ? Fe2 C5 1.748(5) . ? Fe2 C4 1.753(6) . ? Fe2 S2 2.2715(13) . ? Fe2 S3 2.2783(13) . ? Fe2 S1 2.2789(14) . ? Fe3 C13 1.767(5) . ? Fe3 C12 1.785(5) . ? Fe3 C11 1.815(5) . ? Fe3 S4 2.2790(12) . ? Fe3 S5 2.2871(13) . ? Fe3 Fe4 2.5133(10) . ? Fe4 C15 1.753(5) . ? Fe4 C14 1.755(5) . ? Fe4 S5 2.2675(12) . ? Fe4 S4 2.2808(12) . ? Fe4 S6 2.2821(12) . ? S1 C6 1.833(6) . ? S2 C8 1.827(5) . ? S3 C39 1.813(5) . ? S4 C16 1.811(4) . ? S5 C18 1.835(5) . ? S6 C49 1.827(4) . ? N1 C36 1.335(6) . ? N1 C32 1.345(5) . ? N2 C37 1.284(5) . ? N2 C38 1.459(6) . ? N3 C46 1.340(6) . ? N3 C42 1.351(6) . ? N4 C47 1.261(5) . ? N4 C48 1.466(5) . ? O1 C1 1.146(6) . ? O2 C2 1.154(6) . ? O3 C3 1.151(6) . ? O4 C4 1.150(6) . ? O5 C5 1.149(6) . ? O11 C11 1.136(5) . ? O12 C12 1.142(5) . ? O13 C13 1.150(5) . ? O14 C14 1.154(5) . ? O15 C15 1.155(5) . ? C6 C7 1.512(8) . ? C7 C8 1.497(7) . ? C16 C17 1.493(7) . ? C17 C18 1.502(7) . ? C32 C33 1.390(6) . ? C32 C37 1.457(7) . ? C33 C34 1.379(8) . ? C34 C35 1.359(9) . ? C35 C36 1.380(7) . ? C38 C39 1.510(7) . ? C42 C43 1.385(7) . ? C42 C47 1.445(7) . ? C43 C44 1.368(10) . ? C44 C45 1.383(11) . ? C45 C46 1.375(9) . ? C48 C49 1.507(6) . ? 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 N4 174.85(14) . . ? N2 Ni1 N3 97.27(15) . . ? N4 Ni1 N3 79.26(14) . . ? N2 Ni1 N1 79.24(15) . . ? N4 Ni1 N1 96.65(14) . . ? N3 Ni1 N1 86.19(14) . . ? N2 Ni1 S6 98.94(11) . . ? N4 Ni1 S6 84.40(10) . . ? N3 Ni1 S6 163.61(11) . . ? N1 Ni1 S6 94.46(10) . . ? N2 Ni1 S3 83.69(11) . . ? N4 Ni1 S3 100.39(10) . . ? N3 Ni1 S3 95.91(11) . . ? N1 Ni1 S3 162.93(11) . . ? S6 Ni1 S3 88.27(4) . . ? C2 Fe1 C3 90.9(2) . . ? C2 Fe1 C1 103.0(2) . . ? C3 Fe1 C1 96.6(2) . . ? C2 Fe1 S2 148.02(18) . . ? C3 Fe1 S2 87.23(16) . . ? C1 Fe1 S2 108.88(17) . . ? C2 Fe1 S1 86.76(17) . . ? C3 Fe1 S1 161.97(19) . . ? C1 Fe1 S1 101.32(16) . . ? S2 Fe1 S1 85.35(5) . . ? C2 Fe1 Fe2 93.72(16) . . ? C3 Fe1 Fe2 105.80(18) . . ? C1 Fe1 Fe2 151.74(16) . . ? S2 Fe1 Fe2 56.45(3) . . ? S1 Fe1 Fe2 56.61(4) . . ? C5 Fe2 C4 90.9(3) . . ? C5 Fe2 S2 90.04(18) . . ? C4 Fe2 S2 165.11(19) . . ? C5 Fe2 S3 105.69(17) . . ? C4 Fe2 S3 100.49(19) . . ? S2 Fe2 S3 93.56(5) . . ? C5 Fe2 S1 155.11(17) . . ? C4 Fe2 S1 87.68(19) . . ? S2 Fe2 S1 85.26(5) . . ? S3 Fe2 S1 98.99(5) . . ? C5 Fe2 Fe1 100.94(17) . . ? C4 Fe2 Fe1 108.85(19) . . ? S2 Fe2 Fe1 56.44(4) . . ? S3 Fe2 Fe1 139.70(4) . . ? S1 Fe2 Fe1 56.47(4) . . ? C13 Fe3 C12 87.7(2) . . ? C13 Fe3 C11 98.6(2) . . ? C12 Fe3 C11 102.89(19) . . ? C13 Fe3 S4 86.95(14) . . ? C12 Fe3 S4 149.17(14) . . ? C11 Fe3 S4 107.93(14) . . ? C13 Fe3 S5 158.54(15) . . ? C12 Fe3 S5 88.74(15) . . ? C11 Fe3 S5 102.85(14) . . ? S4 Fe3 S5 85.30(4) . . ? C13 Fe3 Fe4 103.17(14) . . ? C12 Fe3 Fe4 95.37(14) . . ? C11 Fe3 Fe4 152.05(14) . . ? S4 Fe3 Fe4 56.59(3) . . ? S5 Fe3 Fe4 56.14(3) . . ? C15 Fe4 C14 91.5(2) . . ? C15 Fe4 S5 153.50(14) . . ? C14 Fe4 S5 89.40(15) . . ? C15 Fe4 S4 87.30(13) . . ? C14 Fe4 S4 166.46(15) . . ? S5 Fe4 S4 85.71(5) . . ? C15 Fe4 S6 106.17(14) . . ? C14 Fe4 S6 98.44(14) . . ? S5 Fe4 S6 99.87(5) . . ? S4 Fe4 S6 94.84(4) . . ? C15 Fe4 Fe3 98.32(13) . . ? C14 Fe4 Fe3 110.44(15) . . ? S5 Fe4 Fe3 56.88(4) . . ? S4 Fe4 Fe3 56.52(3) . . ? S6 Fe4 Fe3 141.39(4) . . ? C6 S1 Fe1 112.7(2) . . ? C6 S1 Fe2 111.30(19) . . ? Fe1 S1 Fe2 66.93(4) . . ? C8 S2 Fe1 112.84(19) . . ? C8 S2 Fe2 111.65(18) . . ? Fe1 S2 Fe2 67.12(4) . . ? C39 S3 Fe2 110.30(17) . . ? C39 S3 Ni1 95.82(17) . . ? Fe2 S3 Ni1 128.43(5) . . ? C16 S4 Fe3 113.82(16) . . ? C16 S4 Fe4 110.49(15) . . ? Fe3 S4 Fe4 66.90(4) . . ? C18 S5 Fe4 111.23(17) . . ? C18 S5 Fe3 112.17(17) . . ? Fe4 S5 Fe3 66.98(4) . . ? C49 S6 Fe4 109.68(14) . . ? C49 S6 Ni1 94.75(14) . . ? Fe4 S6 Ni1 124.89(5) . . ? C36 N1 C32 117.3(4) . . ? C36 N1 Ni1 130.4(3) . . ? C32 N1 Ni1 112.3(3) . . ? C37 N2 C38 122.2(4) . . ? C37 N2 Ni1 117.5(3) . . ? C38 N2 Ni1 120.3(3) . . ? C46 N3 C42 118.2(5) . . ? C46 N3 Ni1 129.5(4) . . ? C42 N3 Ni1 112.0(3) . . ? C47 N4 C48 122.3(4) . . ? C47 N4 Ni1 117.3(3) . . ? C48 N4 Ni1 120.4(3) . . ? O1 C1 Fe1 179.2(5) . . ? O2 C2 Fe1 178.3(6) . . ? O3 C3 Fe1 179.7(5) . . ? O4 C4 Fe2 179.4(6) . . ? O5 C5 Fe2 174.7(5) . . ? C7 C6 S1 116.4(4) . . ? C8 C7 C6 113.9(5) . . ? C7 C8 S2 116.7(4) . . ? O11 C11 Fe3 177.5(4) . . ? O12 C12 Fe3 174.9(4) . . ? O13 C13 Fe3 178.6(5) . . ? O14 C14 Fe4 179.3(4) . . ? O15 C15 Fe4 174.3(4) . . ? C17 C16 S4 116.0(3) . . ? C16 C17 C18 115.2(4) . . ? C17 C18 S5 116.6(3) . . ? N1 C32 C33 123.2(5) . . ? N1 C32 C37 114.0(4) . . ? C33 C32 C37 122.7(5) . . ? C34 C33 C32 117.3(5) . . ? C35 C34 C33 120.5(5) . . ? C34 C35 C36 118.6(6) . . ? N1 C36 C35 123.2(6) . . ? N2 C37 C32 116.7(4) . . ? N2 C38 C39 109.1(4) . . ? C38 C39 S3 106.8(3) . . ? N3 C42 C43 121.9(5) . . ? N3 C42 C47 113.9(4) . . ? C43 C42 C47 124.1(5) . . ? C44 C43 C42 118.4(7) . . ? C43 C44 C45 120.7(6) . . ? C46 C45 C44 117.5(7) . . ? N3 C46 C45 123.2(7) . . ? N4 C47 C42 117.3(4) . . ? N4 C48 C49 109.0(3) . . ? C48 C49 S6 107.9(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.413 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.076