# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chiang, Ming-Hsi' _publ_contact_author_email mhchiang@chem.sinica.edu.tw _publ_section_title ; Influences on the Rotated Structure of the Diiron Dithiolate Complexes: Electronic Asymmetry vs. Secondary Coordination Sphere Interaction ; _publ_author_name 'Ming-Hsi Chiang' # Attachment '- complex_1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 793181' #TrackingRef '- complex_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H82 Cl4 Fe4 N2 O8 P4 S4' _chemical_formula_weight 1768.76 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 15.7127(2) _cell_length_b 13.9213(2) _cell_length_c 18.6454(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.2687(7) _cell_angle_gamma 90.00 _cell_volume 4067.20(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23077 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23077 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9311 _reflns_number_gt 6423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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. ; _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^)+(0.0719P)^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 9311 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.40088(2) 0.15198(3) 0.18104(2) 0.02353(11) Uani 1 1 d . . . Fe2 Fe 0.52650(3) 0.03710(3) 0.18084(2) 0.02824(12) Uani 1 1 d . . . S1 S 0.52333(4) 0.18452(5) 0.12707(4) 0.02665(16) Uani 1 1 d . . . S2 S 0.59581(4) -0.02487(5) -0.10716(4) 0.02589(16) Uani 1 1 d . . . P1 P 0.42716(5) 0.26481(5) 0.26343(4) 0.02691(17) Uani 1 1 d . . . P2 P 0.28997(5) 0.23653(5) 0.14047(4) 0.02820(18) Uani 1 1 d . . . N1 N 0.58579(16) 0.20465(16) -0.08027(13) 0.0352(6) Uani 1 1 d . . . C1 C 0.33639(18) 0.09193(19) 0.23769(15) 0.0305(7) Uani 1 1 d . . . C2 C 0.4908(2) -0.0484(2) 0.24201(17) 0.0379(7) Uani 1 1 d . . . C3 C 0.6044(2) 0.0799(2) 0.24691(18) 0.0393(8) Uani 1 1 d . . . C4 C 0.59633(19) -0.0314(2) 0.12770(16) 0.0348(7) Uani 1 1 d . . . C5 C 0.51963(19) 0.1634(2) 0.02922(15) 0.0320(7) Uani 1 1 d . . . H5A H 0.5461 0.1005 0.0200 0.038 Uiso 1 1 calc R . . H5B H 0.4594 0.1609 0.0096 0.038 Uiso 1 1 calc R . . C6 C 0.5663(2) 0.24214(19) -0.00940(16) 0.0372(8) Uani 1 1 d . . . H6A H 0.5299 0.3001 -0.0154 0.045 Uiso 1 1 calc R . . H6B H 0.6197 0.2599 0.0190 0.045 Uiso 1 1 calc R . . C7 C 0.66704(19) 0.1531(2) -0.07601(17) 0.0383(8) Uani 1 1 d . . . H7A H 0.6783 0.1272 -0.0267 0.046 Uiso 1 1 calc R . . H7B H 0.7133 0.1989 -0.0848 0.046 Uiso 1 1 calc R . . C8 C 0.66910(18) 0.07043(19) -0.12979(16) 0.0321(7) Uani 1 1 d . . . H8A H 0.7278 0.0444 -0.1293 0.039 Uiso 1 1 calc R . . H8B H 0.6527 0.0945 -0.1788 0.039 Uiso 1 1 calc R . . C9 C 0.5773(3) 0.2750(2) -0.13930(18) 0.0562(11) Uani 1 1 d . . . H9 H 0.6019 0.2440 -0.1815 0.067 Uiso 1 1 calc R . . C10 C 0.6265(4) 0.3681(3) -0.1254(2) 0.0920(18) Uani 1 1 d . . . H10A H 0.5982 0.4070 -0.0904 0.138 Uiso 1 1 calc R . . H10B H 0.6282 0.4039 -0.1705 0.138 Uiso 1 1 calc R . . H10C H 0.6849 0.3534 -0.1064 0.138 Uiso 1 1 calc R . . C11 C 0.4838(3) 0.2937(3) -0.1616(2) 0.0780(15) Uani 1 1 d . . . H11A H 0.4550 0.2327 -0.1733 0.117 Uiso 1 1 calc R . . H11B H 0.4793 0.3357 -0.2040 0.117 Uiso 1 1 calc R . . H11C H 0.4568 0.3249 -0.1220 0.117 Uiso 1 1 calc R . . C12 C 0.34279(18) 0.3574(2) 0.24901(16) 0.0333(7) Uani 1 1 d . . . H12A H 0.3322 0.3881 0.2954 0.040 Uiso 1 1 calc R . . H12B H 0.3616 0.4077 0.2161 0.040 Uiso 1 1 calc R . . C13 C 0.26133(18) 0.3108(2) 0.21676(15) 0.0308(6) Uani 1 1 d . . . H13A H 0.2194 0.3606 0.2001 0.037 Uiso 1 1 calc R . . H13B H 0.2356 0.2704 0.2531 0.037 Uiso 1 1 calc R . . C14 C 0.52499(19) 0.3371(2) 0.26807(16) 0.0337(7) Uani 1 1 d . . . C15 C 0.5380(2) 0.4050(2) 0.21561(18) 0.0400(8) Uani 1 1 d . . . H15 H 0.4955 0.4147 0.1774 0.048 Uiso 1 1 calc R . . C16 C 0.6127(3) 0.4590(2) 0.2183(2) 0.0553(10) Uani 1 1 d . . . H16 H 0.6206 0.5062 0.1826 0.066 Uiso 1 1 calc R . . C17 C 0.6751(3) 0.4440(3) 0.2728(3) 0.0676(12) Uani 1 1 d . . . H17 H 0.7263 0.4806 0.2745 0.081 Uiso 1 1 calc R . . C18 C 0.6637(2) 0.3765(3) 0.3248(2) 0.0674(12) Uani 1 1 d . . . H18 H 0.7070 0.3664 0.3624 0.081 Uiso 1 1 calc R . . C19 C 0.5891(2) 0.3227(3) 0.32278(19) 0.0486(9) Uani 1 1 d . . . H19 H 0.5817 0.2759 0.3589 0.058 Uiso 1 1 calc R . . C20 C 0.42507(19) 0.2275(2) 0.35799(16) 0.0356(7) Uani 1 1 d . . . C21 C 0.4487(3) 0.1361(3) 0.37722(19) 0.0630(11) Uani 1 1 d . . . H21 H 0.4616 0.0916 0.3410 0.076 Uiso 1 1 calc R . . C22 C 0.4543(4) 0.1072(4) 0.4480(2) 0.1008(19) Uani 1 1 d . . . H22 H 0.4694 0.0428 0.4599 0.121 Uiso 1 1 calc R . . C23 C 0.4381(3) 0.1713(4) 0.5017(2) 0.0836(15) Uani 1 1 d . . . H23 H 0.4452 0.1527 0.5508 0.100 Uiso 1 1 calc R . . C24 C 0.4117(3) 0.2621(3) 0.4831(2) 0.0678(12) Uani 1 1 d . . . H24 H 0.3978 0.3059 0.5195 0.081 Uiso 1 1 calc R . . C25 C 0.4050(2) 0.2910(3) 0.41162(18) 0.0514(9) Uani 1 1 d . . . H25 H 0.3867 0.3543 0.3994 0.062 Uiso 1 1 calc R . . C26 C 0.2899(2) 0.3246(2) 0.06747(16) 0.0389(7) Uani 1 1 d . . . C27 C 0.3665(2) 0.3596(2) 0.04495(16) 0.0389(8) Uani 1 1 d . . . H27 H 0.4191 0.3353 0.0660 0.047 Uiso 1 1 calc R . . C28 C 0.3668(3) 0.4296(2) -0.00795(19) 0.0531(10) Uani 1 1 d . . . H28 H 0.4194 0.4536 -0.0224 0.064 Uiso 1 1 calc R . . C29 C 0.2916(3) 0.4641(3) -0.0393(2) 0.0802(15) Uani 1 1 d . . . H29 H 0.2923 0.5121 -0.0755 0.096 Uiso 1 1 calc R . . C30 C 0.2149(3) 0.4301(4) -0.0190(3) 0.108(2) Uani 1 1 d . . . H30 H 0.1629 0.4540 -0.0413 0.129 Uiso 1 1 calc R . . C31 C 0.2139(3) 0.3601(3) 0.0347(2) 0.0797(15) Uani 1 1 d . . . H31 H 0.1609 0.3367 0.0490 0.096 Uiso 1 1 calc R . . C32 C 0.19428(18) 0.1665(2) 0.11469(16) 0.0354(7) Uani 1 1 d . . . C33 C 0.1935(2) 0.1110(3) 0.05259(18) 0.0503(9) Uani 1 1 d . . . H33 H 0.2397 0.1154 0.0226 0.060 Uiso 1 1 calc R . . C34 C 0.1269(2) 0.0500(3) 0.0340(2) 0.0647(11) Uani 1 1 d . . . H34 H 0.1270 0.0127 -0.0086 0.078 Uiso 1 1 calc R . . C35 C 0.0597(2) 0.0428(3) 0.0776(2) 0.0618(11) Uani 1 1 d . . . H35 H 0.0140 0.0000 0.0649 0.074 Uiso 1 1 calc R . . C36 C 0.0585(2) 0.0966(3) 0.1383(2) 0.0579(10) Uani 1 1 d . . . H36 H 0.0121 0.0916 0.1679 0.069 Uiso 1 1 calc R . . C37 C 0.1258(2) 0.1590(3) 0.15682(18) 0.0471(9) Uani 1 1 d . . . H37 H 0.1247 0.1970 0.1991 0.057 Uiso 1 1 calc R . . O1 O 0.29148(14) 0.05025(14) 0.27407(12) 0.0451(6) Uani 1 1 d . . . O2 O 0.46681(16) -0.10225(16) 0.28316(13) 0.0540(6) Uani 1 1 d . . . O3 O 0.65546(16) 0.10516(18) 0.29030(13) 0.0538(6) Uani 1 1 d . . . O4 O 0.64177(14) -0.07515(16) 0.09488(12) 0.0492(6) Uani 1 1 d . . . C38 C 0.7533(3) 0.2518(3) 0.1768(3) 0.0923(17) Uani 1 1 d . . . H38A H 0.6976 0.2807 0.1606 0.111 Uiso 1 1 calc R . . H38B H 0.7504 0.2319 0.2276 0.111 Uiso 1 1 calc R . . Cl1 Cl 0.76930(8) 0.14884(8) 0.12454(7) 0.0775(3) Uani 1 1 d . . . Cl2 Cl 0.83037(9) 0.33669(12) 0.17281(9) 0.1196(6) 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 0.0237(2) 0.0230(2) 0.0250(2) -0.00171(16) 0.00871(17) 0.00117(16) Fe2 0.0273(2) 0.0281(2) 0.0303(2) 0.00100(17) 0.00847(19) 0.00430(17) S1 0.0262(4) 0.0270(3) 0.0277(4) -0.0018(3) 0.0091(3) -0.0017(3) S2 0.0257(4) 0.0241(3) 0.0292(4) -0.0025(3) 0.0107(3) -0.0014(3) P1 0.0255(4) 0.0295(4) 0.0264(4) -0.0040(3) 0.0065(3) 0.0001(3) P2 0.0268(4) 0.0321(4) 0.0265(4) -0.0030(3) 0.0067(3) 0.0044(3) N1 0.0505(16) 0.0245(12) 0.0336(14) -0.0003(11) 0.0225(13) -0.0010(11) C1 0.0326(16) 0.0261(14) 0.0342(16) -0.0055(12) 0.0113(14) 0.0036(12) C2 0.0374(18) 0.0366(16) 0.0404(18) 0.0034(15) 0.0087(15) 0.0088(14) C3 0.0374(18) 0.0447(18) 0.0367(18) 0.0034(15) 0.0077(16) 0.0109(15) C4 0.0306(16) 0.0374(16) 0.0361(17) 0.0009(14) 0.0005(14) 0.0042(13) C5 0.0378(17) 0.0312(15) 0.0284(15) -0.0036(12) 0.0116(14) -0.0052(13) C6 0.050(2) 0.0274(15) 0.0372(17) -0.0052(13) 0.0250(16) -0.0054(13) C7 0.0409(18) 0.0313(15) 0.0452(18) -0.0109(14) 0.0197(16) -0.0119(14) C8 0.0316(16) 0.0287(14) 0.0381(16) -0.0026(13) 0.0167(14) -0.0045(12) C9 0.100(3) 0.0324(17) 0.041(2) 0.0066(15) 0.038(2) 0.0077(19) C10 0.172(5) 0.0318(19) 0.082(3) -0.001(2) 0.078(3) -0.022(2) C11 0.128(4) 0.058(2) 0.051(2) 0.018(2) 0.031(3) 0.046(3) C12 0.0323(16) 0.0342(15) 0.0340(16) -0.0074(13) 0.0066(14) 0.0040(13) C13 0.0278(15) 0.0337(15) 0.0315(15) -0.0038(13) 0.0072(13) 0.0051(12) C14 0.0317(16) 0.0342(16) 0.0360(16) -0.0140(13) 0.0083(14) -0.0040(13) C15 0.0432(19) 0.0350(16) 0.0433(18) -0.0058(14) 0.0122(16) -0.0036(14) C16 0.060(2) 0.0378(18) 0.072(3) -0.0114(18) 0.033(2) -0.0131(17) C17 0.053(3) 0.068(3) 0.084(3) -0.031(2) 0.022(2) -0.032(2) C18 0.039(2) 0.098(3) 0.064(3) -0.019(3) -0.004(2) -0.023(2) C19 0.0384(19) 0.064(2) 0.0432(19) -0.0086(17) 0.0041(16) -0.0082(17) C20 0.0313(16) 0.0469(18) 0.0293(16) -0.0019(14) 0.0072(14) -0.0022(14) C21 0.090(3) 0.070(3) 0.0307(18) 0.0072(18) 0.012(2) 0.026(2) C22 0.165(6) 0.099(4) 0.041(2) 0.025(2) 0.019(3) 0.053(4) C23 0.105(4) 0.118(4) 0.029(2) 0.015(2) 0.016(2) 0.014(3) C24 0.067(3) 0.106(3) 0.0318(19) -0.020(2) 0.0121(19) 0.001(3) C25 0.056(2) 0.066(2) 0.0341(18) -0.0116(17) 0.0113(17) 0.0007(19) C26 0.0414(18) 0.0442(18) 0.0317(16) 0.0049(14) 0.0068(15) 0.0139(15) C27 0.051(2) 0.0329(16) 0.0343(17) -0.0010(13) 0.0118(16) 0.0076(14) C28 0.073(3) 0.0416(19) 0.048(2) 0.0058(17) 0.025(2) 0.0088(18) C29 0.095(3) 0.085(3) 0.065(3) 0.045(2) 0.037(3) 0.046(3) C30 0.076(3) 0.157(5) 0.093(4) 0.080(4) 0.027(3) 0.056(3) C31 0.057(3) 0.114(4) 0.071(3) 0.050(3) 0.022(2) 0.036(3) C32 0.0272(16) 0.0423(17) 0.0360(17) -0.0041(14) -0.0019(14) 0.0059(13) C33 0.0334(18) 0.073(2) 0.044(2) -0.0227(18) 0.0003(16) 0.0042(17) C34 0.041(2) 0.089(3) 0.062(3) -0.040(2) -0.009(2) 0.000(2) C35 0.036(2) 0.075(3) 0.072(3) -0.016(2) -0.013(2) -0.0108(19) C36 0.040(2) 0.083(3) 0.051(2) -0.008(2) 0.0039(18) -0.017(2) C37 0.0366(19) 0.068(2) 0.0374(18) -0.0131(17) 0.0065(16) -0.0128(17) O1 0.0529(14) 0.0350(11) 0.0515(14) -0.0018(10) 0.0321(12) -0.0049(10) O2 0.0601(16) 0.0509(14) 0.0533(15) 0.0217(12) 0.0179(13) 0.0062(12) O3 0.0521(16) 0.0641(16) 0.0437(14) -0.0074(13) -0.0065(12) 0.0042(13) O4 0.0399(13) 0.0601(15) 0.0480(14) -0.0148(12) 0.0060(11) 0.0183(12) C38 0.070(3) 0.075(3) 0.135(5) -0.028(3) 0.033(3) -0.023(2) Cl1 0.0790(8) 0.0676(6) 0.0906(8) 0.0090(6) 0.0368(7) 0.0004(6) Cl2 0.0927(10) 0.1423(13) 0.1311(12) -0.0502(10) 0.0563(9) -0.0670(9) _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 C1 1.732(3) . ? Fe1 P2 2.1904(8) . ? Fe1 P1 2.2144(8) . ? Fe1 S2 2.2454(7) 3_655 ? Fe1 S1 2.2820(7) . ? Fe1 Fe2 2.5406(5) . ? Fe2 C2 1.769(3) . ? Fe2 C3 1.773(4) . ? Fe2 C4 1.805(3) . ? Fe2 S1 2.2829(8) . ? Fe2 S2 2.2839(9) 3_655 ? S1 C5 1.845(3) . ? S2 C8 1.827(3) . ? S2 Fe1 2.2454(7) 3_655 ? S2 Fe2 2.2839(9) 3_655 ? P1 C14 1.834(3) . ? P1 C20 1.840(3) . ? P1 C12 1.854(3) . ? P2 C32 1.826(3) . ? P2 C26 1.831(3) . ? P2 C13 1.841(3) . ? N1 C7 1.462(4) . ? N1 C9 1.472(4) . ? N1 C6 1.474(3) . ? C1 O1 1.169(3) . ? C2 O2 1.156(3) . ? C3 O3 1.152(4) . ? C4 O4 1.149(3) . ? C5 C6 1.528(4) . ? C7 C8 1.528(4) . ? C9 C11 1.519(6) . ? C9 C10 1.521(5) . ? C12 C13 1.519(4) . ? C14 C15 1.386(4) . ? C14 C19 1.393(4) . ? C15 C16 1.393(4) . ? C16 C17 1.374(6) . ? C17 C18 1.371(6) . ? C18 C19 1.389(5) . ? C20 C21 1.366(5) . ? C20 C25 1.388(4) . ? C21 C22 1.376(5) . ? C22 C23 1.378(6) . ? C23 C24 1.367(6) . ? C24 C25 1.388(5) . ? C26 C31 1.392(5) . ? C26 C27 1.392(4) . ? C27 C28 1.387(4) . ? C28 C29 1.365(6) . ? C29 C30 1.374(6) . ? C30 C31 1.398(6) . ? C32 C37 1.382(4) . ? C32 C33 1.392(4) . ? C33 C34 1.372(5) . ? C34 C35 1.383(5) . ? C35 C36 1.359(5) . ? C36 C37 1.393(5) . ? C38 Cl2 1.697(4) . ? C38 Cl1 1.762(4) . ? 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 C1 Fe1 P2 89.05(10) . . ? C1 Fe1 P1 90.37(9) . . ? P2 Fe1 P1 87.76(3) . . ? C1 Fe1 S2 92.01(9) . 3_655 ? P2 Fe1 S2 105.42(3) . 3_655 ? P1 Fe1 S2 166.64(3) . 3_655 ? C1 Fe1 S1 156.25(10) . . ? P2 Fe1 S1 114.60(3) . . ? P1 Fe1 S1 92.60(3) . . ? S2 Fe1 S1 80.05(3) 3_655 . ? C1 Fe1 Fe2 100.77(9) . . ? P2 Fe1 Fe2 159.38(3) . . ? P1 Fe1 Fe2 110.04(3) . . ? S2 Fe1 Fe2 56.60(2) 3_655 . ? S1 Fe1 Fe2 56.20(2) . . ? C2 Fe2 C3 90.77(15) . . ? C2 Fe2 C4 103.49(13) . . ? C3 Fe2 C4 98.20(13) . . ? C2 Fe2 S1 152.96(10) . . ? C3 Fe2 S1 89.69(10) . . ? C4 Fe2 S1 103.20(10) . . ? C2 Fe2 S2 92.56(11) . 3_655 ? C3 Fe2 S2 161.62(10) . 3_655 ? C4 Fe2 S2 98.58(10) . 3_655 ? S1 Fe2 S2 79.22(3) . 3_655 ? C2 Fe2 Fe1 97.99(10) . . ? C3 Fe2 Fe1 106.47(10) . . ? C4 Fe2 Fe1 146.89(10) . . ? S1 Fe2 Fe1 56.17(2) . . ? S2 Fe2 Fe1 55.17(2) 3_655 . ? C5 S1 Fe1 116.04(10) . . ? C5 S1 Fe2 106.81(9) . . ? Fe1 S1 Fe2 67.63(2) . . ? C8 S2 Fe1 112.76(9) . 3_655 ? C8 S2 Fe2 115.59(11) . 3_655 ? Fe1 S2 Fe2 68.23(2) 3_655 3_655 ? C14 P1 C20 100.62(14) . . ? C14 P1 C12 102.30(13) . . ? C20 P1 C12 105.75(13) . . ? C14 P1 Fe1 122.30(9) . . ? C20 P1 Fe1 116.67(10) . . ? C12 P1 Fe1 107.34(10) . . ? C32 P2 C26 101.92(15) . . ? C32 P2 C13 105.02(13) . . ? C26 P2 C13 102.23(14) . . ? C32 P2 Fe1 115.00(10) . . ? C26 P2 Fe1 124.93(10) . . ? C13 P2 Fe1 105.60(10) . . ? C7 N1 C9 113.4(2) . . ? C7 N1 C6 111.4(2) . . ? C9 N1 C6 114.9(2) . . ? O1 C1 Fe1 177.9(3) . . ? O2 C2 Fe2 178.1(3) . . ? O3 C3 Fe2 178.2(3) . . ? O4 C4 Fe2 178.8(3) . . ? C6 C5 S1 111.8(2) . . ? N1 C6 C5 107.9(2) . . ? N1 C7 C8 113.3(3) . . ? C7 C8 S2 110.53(18) . . ? N1 C9 C11 110.5(3) . . ? N1 C9 C10 115.0(3) . . ? C11 C9 C10 111.7(3) . . ? C13 C12 P1 109.44(19) . . ? C12 C13 P2 107.37(18) . . ? C15 C14 C19 118.6(3) . . ? C15 C14 P1 120.5(2) . . ? C19 C14 P1 120.9(2) . . ? C14 C15 C16 120.7(3) . . ? C17 C16 C15 119.8(4) . . ? C18 C17 C16 120.2(3) . . ? C17 C18 C19 120.3(4) . . ? C18 C19 C14 120.3(4) . . ? C21 C20 C25 118.4(3) . . ? C21 C20 P1 119.4(2) . . ? C25 C20 P1 122.1(3) . . ? C20 C21 C22 121.4(4) . . ? C21 C22 C23 120.4(4) . . ? C24 C23 C22 118.9(4) . . ? C23 C24 C25 120.7(4) . . ? C20 C25 C24 120.1(4) . . ? C31 C26 C27 118.4(3) . . ? C31 C26 P2 121.1(3) . . ? C27 C26 P2 120.4(2) . . ? C28 C27 C26 120.6(3) . . ? C29 C28 C27 120.2(4) . . ? C28 C29 C30 120.6(4) . . ? C29 C30 C31 119.7(4) . . ? C26 C31 C30 120.4(4) . . ? C37 C32 C33 118.2(3) . . ? C37 C32 P2 123.4(2) . . ? C33 C32 P2 118.1(2) . . ? C34 C33 C32 120.8(3) . . ? C33 C34 C35 119.9(3) . . ? C36 C35 C34 120.5(3) . . ? C35 C36 C37 119.5(3) . . ? C32 C37 C36 121.0(3) . . ? Cl2 C38 Cl1 114.3(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.917 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.105 # Attachment '- complex_2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 793182' #TrackingRef '- complex_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H58 Cl4 Fe4 N2 O10 P2 S4' _chemical_formula_weight 1426.38 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 13.2880(6) _cell_length_b 21.5592(9) _cell_length_c 21.8668(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.760(1) _cell_angle_gamma 90.00 _cell_volume 6109.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8408 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 1.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6494 _exptl_absorpt_correction_T_max 0.7120 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46682 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14029 _reflns_number_gt 11322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. ; _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^)+(0.0621P)^2^+8.7304P] 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 14029 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.003 _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 0.29809(4) 0.64006(2) 0.26656(2) 0.02016(11) Uani 1 1 d . . . Fe2 Fe 0.24520(4) 0.67925(2) 0.15601(2) 0.02546(13) Uani 1 1 d . . . Fe3 Fe 0.58106(4) 0.36980(2) 0.23242(2) 0.01931(11) Uani 1 1 d . . . Fe4 Fe 0.53091(4) 0.35587(2) 0.11591(2) 0.02508(12) Uani 1 1 d . . . S1 S 0.40967(6) 0.68486(4) 0.21414(4) 0.02418(18) Uani 1 1 d . . . S2 S 0.66046(7) 0.41965(4) 0.16378(4) 0.02486(19) Uani 1 1 d . . . S3 S 0.27473(6) 0.57758(4) 0.18237(4) 0.02306(18) Uani 1 1 d . . . S4 S 0.44446(6) 0.41844(4) 0.17063(4) 0.02212(18) Uani 1 1 d . . . P1 P 0.38638(6) 0.57451(4) 0.33636(4) 0.01799(17) Uani 1 1 d . . . P2 P 0.61087(6) 0.41756(4) 0.32534(4) 0.01873(17) Uani 1 1 d . . . N1 N 0.6688(2) 0.60811(14) 0.17578(15) 0.0255(6) Uani 1 1 d . . . N2 N 0.2259(2) 0.46238(15) 0.09460(15) 0.0307(7) Uani 1 1 d . . . C1 C 0.3114(3) 0.70760(17) 0.31410(17) 0.0264(8) Uani 1 1 d . . . C2 C 0.1760(3) 0.62411(17) 0.28264(18) 0.0287(8) Uani 1 1 d . . . C3 C 0.2319(3) 0.75965(19) 0.1728(2) 0.0336(9) Uani 1 1 d . . . C4 C 0.1091(3) 0.66661(19) 0.1383(2) 0.0353(9) Uani 1 1 d . . . C5 C 0.2670(3) 0.6860(2) 0.0778(2) 0.0382(10) Uani 1 1 d . . . C6 C 0.6951(3) 0.32530(16) 0.25176(18) 0.0263(7) Uani 1 1 d . . . C7 C 0.5063(3) 0.30801(17) 0.25197(17) 0.0264(8) Uani 1 1 d . . . C8 C 0.6281(3) 0.3003(2) 0.1101(2) 0.0366(9) Uani 1 1 d . . . C9 C 0.4362(3) 0.29618(19) 0.10860(19) 0.0341(9) Uani 1 1 d . . . C10 C 0.5010(3) 0.3881(2) 0.0372(2) 0.0416(10) Uani 1 1 d . . . C11 C 0.4919(3) 0.63351(17) 0.17902(17) 0.0259(7) Uani 1 1 d . . . H11A H 0.4752 0.5897 0.1861 0.031 Uiso 1 1 calc R . . H11B H 0.4782 0.6407 0.1332 0.031 Uiso 1 1 calc R . . C12 C 0.6058(3) 0.64562(17) 0.20779(18) 0.0268(8) Uani 1 1 d . . . H12A H 0.6217 0.6901 0.2036 0.032 Uiso 1 1 calc R . . H12B H 0.6212 0.6350 0.2530 0.032 Uiso 1 1 calc R . . C13 C 0.6775(3) 0.54348(17) 0.19625(18) 0.0293(8) Uani 1 1 d . . . H13A H 0.6445 0.5383 0.2323 0.035 Uiso 1 1 calc R . . H13B H 0.7513 0.5324 0.2103 0.035 Uiso 1 1 calc R . . C14 C 0.6268(3) 0.50054(17) 0.14403(19) 0.0308(8) Uani 1 1 d . . . H14A H 0.6490 0.5118 0.1051 0.037 Uiso 1 1 calc R . . H14B H 0.5510 0.5056 0.1361 0.037 Uiso 1 1 calc R . . C15 C 0.7693(3) 0.63527(19) 0.1719(2) 0.0359(9) Uani 1 1 d . . . H15 H 0.8074 0.6022 0.1542 0.043 Uiso 1 1 calc R . . C16 C 0.8363(3) 0.6523(2) 0.2351(2) 0.0437(11) Uani 1 1 d . . . H16A H 0.8019 0.6845 0.2547 0.052 Uiso 1 1 calc R . . H16B H 0.9029 0.6680 0.2295 0.052 Uiso 1 1 calc R . . H16C H 0.8475 0.6155 0.2621 0.052 Uiso 1 1 calc R . . C17 C 0.7541(4) 0.6876(2) 0.1257(2) 0.0459(11) Uani 1 1 d . . . H17A H 0.7100 0.6738 0.0861 0.055 Uiso 1 1 calc R . . H17B H 0.8212 0.7007 0.1186 0.055 Uiso 1 1 calc R . . H17C H 0.7213 0.7225 0.1424 0.055 Uiso 1 1 calc R . . C18 C 0.1618(3) 0.52721(17) 0.17236(18) 0.0275(8) Uani 1 1 d . . . H18A H 0.1743 0.4945 0.2049 0.033 Uiso 1 1 calc R . . H18B H 0.1012 0.5518 0.1774 0.033 Uiso 1 1 calc R . . C19 C 0.1398(3) 0.49740(19) 0.10753(19) 0.0318(8) Uani 1 1 d . . . H19A H 0.0797 0.4694 0.1036 0.038 Uiso 1 1 calc R . . H19B H 0.1210 0.5303 0.0755 0.038 Uiso 1 1 calc R . . C20 C 0.2350(3) 0.39913(19) 0.1187(2) 0.0358(9) Uani 1 1 d . . . H20A H 0.2497 0.3712 0.0857 0.043 Uiso 1 1 calc R . . H20B H 0.1678 0.3865 0.1273 0.043 Uiso 1 1 calc R . . C21 C 0.3186(3) 0.39014(19) 0.17819(18) 0.0300(8) Uani 1 1 d . . . H21A H 0.3241 0.3454 0.1888 0.036 Uiso 1 1 calc R . . H21B H 0.2980 0.4122 0.2132 0.036 Uiso 1 1 calc R . . C22 C 0.2356(4) 0.4676(2) 0.0289(2) 0.0514(12) Uani 1 1 d . . . H22 H 0.2933 0.4392 0.0249 0.062 Uiso 1 1 calc R . . C23 C 0.2697(6) 0.5318(3) 0.0150(3) 0.081(2) Uani 1 1 d . . . H23A H 0.2151 0.5617 0.0174 0.097 Uiso 1 1 calc R . . H23B H 0.2835 0.5327 -0.0272 0.097 Uiso 1 1 calc R . . H23C H 0.3326 0.5429 0.0458 0.097 Uiso 1 1 calc R . . C24 C 0.1418(5) 0.4452(3) -0.0186(2) 0.0747(19) Uani 1 1 d . . . H24A H 0.1206 0.4045 -0.0058 0.090 Uiso 1 1 calc R . . H24B H 0.1588 0.4416 -0.0598 0.090 Uiso 1 1 calc R . . H24C H 0.0852 0.4749 -0.0210 0.090 Uiso 1 1 calc R . . C25 C 0.4652(2) 0.51742(15) 0.30438(15) 0.0192(6) Uani 1 1 d . . . H25A H 0.4230 0.5009 0.2647 0.023 Uiso 1 1 calc R . . H25B H 0.5247 0.5395 0.2941 0.023 Uiso 1 1 calc R . . C26 C 0.5064(2) 0.46261(15) 0.34709(16) 0.0200(7) Uani 1 1 d . . . H26A H 0.4482 0.4341 0.3479 0.024 Uiso 1 1 calc R . . H26B H 0.5315 0.4785 0.3902 0.024 Uiso 1 1 calc R . . C27 C 0.3010(2) 0.52860(15) 0.37313(16) 0.0199(7) Uani 1 1 d . . . C28 C 0.2572(3) 0.47366(16) 0.34606(17) 0.0238(7) Uani 1 1 d . . . H28 H 0.2776 0.4574 0.3103 0.029 Uiso 1 1 calc R . . C29 C 0.1841(3) 0.44238(18) 0.37064(18) 0.0292(8) Uani 1 1 d . . . H29 H 0.1555 0.4047 0.3520 0.035 Uiso 1 1 calc R . . C30 C 0.1528(3) 0.46576(19) 0.42181(19) 0.0331(9) Uani 1 1 d . . . H30 H 0.1031 0.4441 0.4388 0.040 Uiso 1 1 calc R . . C31 C 0.1937(3) 0.52084(19) 0.44856(18) 0.0325(9) Uani 1 1 d . . . H31 H 0.1714 0.5372 0.4837 0.039 Uiso 1 1 calc R . . C32 C 0.2668(3) 0.55221(17) 0.42440(17) 0.0269(8) Uani 1 1 d . . . H32 H 0.2942 0.5902 0.4429 0.032 Uiso 1 1 calc R . . C33 C 0.4839(2) 0.60564(15) 0.40137(16) 0.0210(7) Uani 1 1 d . . . C34 C 0.5114(3) 0.57664(16) 0.45987(16) 0.0237(7) Uani 1 1 d . . . H34 H 0.4724 0.5423 0.4690 0.028 Uiso 1 1 calc R . . C35 C 0.5949(3) 0.59759(17) 0.50464(17) 0.0275(8) Uani 1 1 d . . . H35 H 0.6135 0.5772 0.5441 0.033 Uiso 1 1 calc R . . C36 C 0.6514(3) 0.64804(19) 0.49216(19) 0.0328(9) Uani 1 1 d . . . H36 H 0.7090 0.6622 0.5229 0.039 Uiso 1 1 calc R . . C37 C 0.6243(3) 0.67756(18) 0.43545(19) 0.0321(8) Uani 1 1 d . . . H37 H 0.6627 0.7125 0.4271 0.038 Uiso 1 1 calc R . . C38 C 0.5414(3) 0.65677(17) 0.39022(17) 0.0266(8) Uani 1 1 d . . . H38 H 0.5234 0.6776 0.3510 0.032 Uiso 1 1 calc R . . C39 C 0.6341(3) 0.36293(15) 0.39144(16) 0.0228(7) Uani 1 1 d . . . C40 C 0.5519(3) 0.32802(18) 0.40345(19) 0.0320(8) Uani 1 1 d . . . H40 H 0.4857 0.3318 0.3764 0.038 Uiso 1 1 calc R . . C41 C 0.5655(4) 0.28785(19) 0.45438(19) 0.0376(10) Uani 1 1 d . . . H41 H 0.5087 0.2649 0.4623 0.045 Uiso 1 1 calc R . . C42 C 0.6612(4) 0.28153(19) 0.49307(19) 0.0427(11) Uani 1 1 d . . . H42 H 0.6710 0.2539 0.5277 0.051 Uiso 1 1 calc R . . C43 C 0.7429(4) 0.3150(2) 0.48184(19) 0.0411(10) Uani 1 1 d . . . H43 H 0.8089 0.3107 0.5091 0.049 Uiso 1 1 calc R . . C44 C 0.7307(3) 0.35548(18) 0.43090(18) 0.0322(9) Uani 1 1 d . . . H44 H 0.7882 0.3779 0.4232 0.039 Uiso 1 1 calc R . . C45 C 0.7231(2) 0.46880(16) 0.34466(16) 0.0223(7) Uani 1 1 d . . . C46 C 0.7255(3) 0.52101(18) 0.38187(18) 0.0306(8) Uani 1 1 d . . . H46 H 0.6668 0.5315 0.3978 0.037 Uiso 1 1 calc R . . C47 C 0.8127(3) 0.5580(2) 0.3960(2) 0.0423(10) Uani 1 1 d . . . H47 H 0.8127 0.5942 0.4209 0.051 Uiso 1 1 calc R . . C48 C 0.8995(3) 0.5430(2) 0.3744(2) 0.0388(10) Uani 1 1 d . . . H48 H 0.9595 0.5681 0.3849 0.047 Uiso 1 1 calc R . . C49 C 0.8985(3) 0.4915(2) 0.3376(2) 0.0365(9) Uani 1 1 d . . . H49 H 0.9580 0.4811 0.3224 0.044 Uiso 1 1 calc R . . C50 C 0.8114(3) 0.45454(19) 0.32247(18) 0.0306(8) Uani 1 1 d . . . H50 H 0.8115 0.4191 0.2967 0.037 Uiso 1 1 calc R . . O1 O 0.3204(2) 0.75176(13) 0.34361(15) 0.0427(7) Uani 1 1 d . . . O2 O 0.0969(2) 0.61391(15) 0.29246(15) 0.0448(8) Uani 1 1 d . . . O3 O 0.2240(2) 0.81063(14) 0.18357(16) 0.0472(8) Uani 1 1 d . . . O4 O 0.0228(2) 0.65726(16) 0.12733(17) 0.0532(9) Uani 1 1 d . . . O5 O 0.2836(3) 0.69279(18) 0.02972(15) 0.0589(10) Uani 1 1 d . . . O6 O 0.7702(2) 0.29725(13) 0.26165(15) 0.0418(7) Uani 1 1 d . . . O7 O 0.4591(2) 0.26634(13) 0.26142(14) 0.0382(7) Uani 1 1 d . . . O8 O 0.6902(3) 0.26478(17) 0.10870(18) 0.0579(9) Uani 1 1 d . . . O9 O 0.3775(2) 0.25706(16) 0.10514(17) 0.0525(9) Uani 1 1 d . . . O10 O 0.4838(3) 0.4067(2) -0.01194(16) 0.0690(11) Uani 1 1 d . . . C51 C 0.5055(5) 0.7786(3) 0.0474(3) 0.0744(17) Uani 1 1 d . . . H51A H 0.4539 0.7452 0.0349 0.089 Uiso 1 1 calc R . . H51B H 0.5746 0.7606 0.0493 0.089 Uiso 1 1 calc R . . Cl1 Cl 0.49920(14) 0.80538(9) 0.12092(8) 0.0846(5) Uani 1 1 d . . . Cl2 Cl 0.48252(15) 0.83682(10) -0.00905(8) 0.0958(6) Uani 1 1 d . . . C52 C 0.5585(6) 0.8359(4) 0.3279(3) 0.092(2) Uani 1 1 d . . . H52A H 0.6302 0.8348 0.3219 0.110 Uiso 1 1 calc R . . H52B H 0.5275 0.7947 0.3163 0.110 Uiso 1 1 calc R . . Cl3 Cl 0.56236(17) 0.84899(10) 0.40724(11) 0.1121(8) Uani 1 1 d . . . Cl4 Cl 0.4915(2) 0.88950(13) 0.27885(11) 0.1238(9) 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 0.0190(2) 0.0191(2) 0.0226(2) 0.00196(19) 0.00499(19) 0.00373(18) Fe2 0.0225(2) 0.0269(3) 0.0262(3) 0.0071(2) 0.0036(2) 0.0040(2) Fe3 0.0193(2) 0.0179(2) 0.0209(2) -0.00111(18) 0.00480(18) 0.00234(18) Fe4 0.0260(3) 0.0270(3) 0.0230(3) -0.0068(2) 0.0072(2) -0.0012(2) S1 0.0220(4) 0.0226(4) 0.0283(4) 0.0031(3) 0.0065(3) 0.0012(3) S2 0.0244(4) 0.0244(4) 0.0266(4) -0.0006(3) 0.0076(3) -0.0012(3) S3 0.0211(4) 0.0240(4) 0.0236(4) 0.0006(3) 0.0040(3) 0.0005(3) S4 0.0205(4) 0.0235(4) 0.0212(4) -0.0029(3) 0.0022(3) 0.0019(3) P1 0.0179(4) 0.0168(4) 0.0199(4) 0.0005(3) 0.0054(3) 0.0016(3) P2 0.0165(4) 0.0201(4) 0.0193(4) 0.0002(3) 0.0035(3) 0.0039(3) N1 0.0240(15) 0.0222(15) 0.0319(16) 0.0015(13) 0.0096(12) -0.0011(12) N2 0.0242(15) 0.0333(18) 0.0336(18) -0.0032(14) 0.0039(13) 0.0043(13) C1 0.0271(18) 0.0253(19) 0.0273(18) 0.0033(15) 0.0072(15) 0.0062(14) C2 0.0276(19) 0.0284(19) 0.0293(19) 0.0042(15) 0.0044(15) 0.0061(15) C3 0.0257(19) 0.034(2) 0.041(2) 0.0079(18) 0.0084(17) 0.0061(16) C4 0.027(2) 0.035(2) 0.040(2) 0.0069(18) 0.0001(17) 0.0052(16) C5 0.036(2) 0.045(3) 0.030(2) 0.0076(18) 0.0000(17) 0.0009(18) C6 0.0271(18) 0.0225(17) 0.0310(19) 0.0011(15) 0.0100(15) 0.0033(14) C7 0.0250(17) 0.0257(19) 0.0279(19) -0.0018(15) 0.0042(14) 0.0056(15) C8 0.037(2) 0.038(2) 0.037(2) -0.0120(18) 0.0126(18) -0.0008(18) C9 0.033(2) 0.038(2) 0.032(2) -0.0148(17) 0.0084(16) -0.0008(17) C10 0.037(2) 0.055(3) 0.032(2) -0.003(2) 0.0061(18) -0.003(2) C11 0.0208(16) 0.0302(19) 0.0279(18) -0.0017(15) 0.0079(14) 0.0003(14) C12 0.0241(17) 0.0232(18) 0.033(2) -0.0007(15) 0.0068(15) -0.0030(14) C13 0.034(2) 0.0241(18) 0.030(2) 0.0007(15) 0.0077(16) 0.0041(15) C14 0.037(2) 0.0218(18) 0.033(2) 0.0040(15) 0.0061(16) -0.0041(15) C15 0.0285(19) 0.032(2) 0.052(3) 0.0076(19) 0.0191(18) 0.0032(16) C16 0.028(2) 0.033(2) 0.065(3) 0.005(2) -0.001(2) -0.0026(17) C17 0.040(2) 0.048(3) 0.055(3) 0.011(2) 0.020(2) -0.001(2) C18 0.0237(17) 0.0281(19) 0.0309(19) -0.0003(15) 0.0059(15) -0.0033(14) C19 0.0223(18) 0.035(2) 0.035(2) -0.0026(17) 0.0009(15) 0.0016(15) C20 0.0235(18) 0.033(2) 0.046(2) -0.0081(18) -0.0017(16) 0.0004(16) C21 0.0234(17) 0.034(2) 0.033(2) -0.0015(16) 0.0077(15) 0.0004(15) C22 0.054(3) 0.058(3) 0.045(3) -0.007(2) 0.016(2) 0.014(2) C23 0.111(6) 0.083(5) 0.064(4) 0.006(3) 0.052(4) 0.004(4) C24 0.079(4) 0.098(5) 0.039(3) -0.025(3) -0.005(3) 0.023(4) C25 0.0204(15) 0.0193(16) 0.0192(16) 0.0000(13) 0.0070(13) 0.0043(12) C26 0.0175(15) 0.0198(16) 0.0238(17) 0.0012(13) 0.0067(13) 0.0046(12) C27 0.0181(15) 0.0189(16) 0.0235(17) 0.0058(13) 0.0061(13) 0.0033(12) C28 0.0221(16) 0.0240(17) 0.0244(17) 0.0021(14) 0.0033(13) 0.0022(13) C29 0.0209(17) 0.0269(19) 0.038(2) 0.0001(16) 0.0014(15) -0.0020(14) C30 0.0240(18) 0.036(2) 0.040(2) 0.0073(18) 0.0095(16) -0.0042(16) C31 0.0300(19) 0.042(2) 0.030(2) -0.0001(17) 0.0168(16) 0.0035(17) C32 0.0274(18) 0.0241(18) 0.0309(19) -0.0030(15) 0.0101(15) 0.0014(14) C33 0.0204(15) 0.0194(16) 0.0232(17) -0.0028(13) 0.0049(13) 0.0031(13) C34 0.0259(17) 0.0221(17) 0.0246(17) -0.0006(14) 0.0085(14) 0.0027(14) C35 0.0298(18) 0.0300(19) 0.0219(17) -0.0030(15) 0.0040(14) 0.0043(15) C36 0.0247(18) 0.035(2) 0.036(2) -0.0073(17) 0.0014(16) -0.0014(16) C37 0.0297(19) 0.029(2) 0.038(2) 0.0028(17) 0.0079(16) -0.0063(15) C38 0.0288(18) 0.0247(18) 0.0271(18) 0.0035(15) 0.0083(15) -0.0013(14) C39 0.0311(18) 0.0194(17) 0.0183(16) 0.0005(13) 0.0065(14) 0.0085(14) C40 0.038(2) 0.029(2) 0.031(2) 0.0027(16) 0.0128(17) 0.0060(16) C41 0.057(3) 0.027(2) 0.035(2) 0.0060(17) 0.023(2) 0.0093(18) C42 0.076(3) 0.028(2) 0.025(2) 0.0051(17) 0.013(2) 0.017(2) C43 0.052(3) 0.035(2) 0.029(2) 0.0008(17) -0.0071(18) 0.015(2) C44 0.036(2) 0.0275(19) 0.030(2) -0.0004(16) 0.0011(16) 0.0087(16) C45 0.0169(15) 0.0265(18) 0.0218(17) 0.0018(14) 0.0006(13) 0.0013(13) C46 0.0218(17) 0.036(2) 0.035(2) -0.0060(17) 0.0091(15) -0.0006(15) C47 0.032(2) 0.043(2) 0.051(3) -0.019(2) 0.0072(19) -0.0085(18) C48 0.0259(19) 0.045(2) 0.044(2) -0.005(2) 0.0046(17) -0.0089(17) C49 0.0193(17) 0.051(3) 0.039(2) -0.0028(19) 0.0069(16) 0.0005(17) C50 0.0227(17) 0.036(2) 0.032(2) -0.0071(17) 0.0047(15) 0.0036(15) O1 0.0522(19) 0.0301(16) 0.0461(18) -0.0105(14) 0.0112(15) 0.0053(13) O2 0.0238(14) 0.060(2) 0.0533(19) 0.0094(16) 0.0154(13) 0.0043(13) O3 0.0468(18) 0.0278(16) 0.068(2) 0.0055(15) 0.0160(16) 0.0047(13) O4 0.0284(16) 0.053(2) 0.073(2) 0.0064(18) 0.0006(15) 0.0035(14) O5 0.073(2) 0.072(3) 0.0331(18) 0.0123(17) 0.0155(17) -0.0005(19) O6 0.0320(15) 0.0324(15) 0.061(2) 0.0046(14) 0.0109(14) 0.0126(12) O7 0.0356(15) 0.0299(15) 0.0517(18) 0.0050(13) 0.0151(13) -0.0051(12) O8 0.052(2) 0.054(2) 0.074(2) -0.0170(18) 0.0258(18) 0.0163(17) O9 0.0466(19) 0.0476(19) 0.065(2) -0.0288(17) 0.0169(16) -0.0201(16) O10 0.069(2) 0.105(3) 0.0309(18) 0.016(2) 0.0067(17) 0.003(2) C51 0.073(4) 0.057(4) 0.095(5) -0.005(3) 0.022(4) 0.000(3) Cl1 0.0925(12) 0.0932(12) 0.0761(11) 0.0331(9) 0.0357(9) 0.0271(10) Cl2 0.1005(13) 0.1187(15) 0.0614(10) 0.0082(9) 0.0036(9) 0.0653(12) C52 0.103(6) 0.089(5) 0.095(5) 0.011(4) 0.047(5) 0.031(4) Cl3 0.1067(15) 0.1038(15) 0.1050(15) 0.0033(12) -0.0211(12) 0.0477(12) Cl4 0.1325(19) 0.158(2) 0.0933(15) 0.0447(15) 0.0503(14) 0.0600(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 Fe1 C2 1.767(4) . ? Fe1 C1 1.775(4) . ? Fe1 P1 2.2163(9) . ? Fe1 S3 2.2468(10) . ? Fe1 S1 2.2795(10) . ? Fe1 Fe2 2.5102(7) . ? Fe2 C4 1.785(4) . ? Fe2 C3 1.789(4) . ? Fe2 C5 1.803(4) . ? Fe2 S1 2.2759(10) . ? Fe2 S3 2.2782(10) . ? Fe3 C6 1.764(4) . ? Fe3 C7 1.770(4) . ? Fe3 P2 2.2340(10) . ? Fe3 S4 2.2663(9) . ? Fe3 S2 2.2849(10) . ? Fe3 Fe4 2.5049(7) . ? Fe4 C9 1.783(4) . ? Fe4 C8 1.786(4) . ? Fe4 C10 1.816(5) . ? Fe4 S2 2.2703(10) . ? Fe4 S4 2.2757(10) . ? S1 C11 1.839(4) . ? S2 C14 1.828(4) . ? S3 C18 1.826(4) . ? S4 C21 1.822(4) . ? P1 C27 1.821(3) . ? P1 C33 1.826(3) . ? P1 C25 1.850(3) . ? P2 C45 1.829(3) . ? P2 C39 1.837(3) . ? P2 C26 1.841(3) . ? N1 C12 1.450(5) . ? N1 C13 1.460(5) . ? N1 C15 1.478(5) . ? N2 C19 1.450(5) . ? N2 C20 1.457(5) . ? N2 C22 1.474(6) . ? C1 O1 1.142(5) . ? C2 O2 1.141(5) . ? C3 O3 1.134(5) . ? C4 O4 1.137(5) . ? C5 O5 1.130(5) . ? C6 O6 1.146(4) . ? C7 O7 1.141(4) . ? C8 O8 1.131(5) . ? C9 O9 1.139(5) . ? C10 O10 1.123(5) . ? C11 C12 1.528(5) . ? C13 C14 1.508(5) . ? C15 C17 1.498(6) . ? C15 C16 1.515(6) . ? C18 C19 1.525(5) . ? C20 C21 1.525(5) . ? C22 C23 1.509(8) . ? C22 C24 1.516(7) . ? C25 C26 1.530(4) . ? C27 C28 1.393(5) . ? C27 C32 1.395(5) . ? C28 C29 1.385(5) . ? C29 C30 1.373(6) . ? C30 C31 1.381(6) . ? C31 C32 1.381(5) . ? C33 C38 1.393(5) . ? C33 C34 1.398(5) . ? C34 C35 1.384(5) . ? C35 C36 1.383(6) . ? C36 C37 1.369(6) . ? C37 C38 1.383(5) . ? C39 C44 1.388(5) . ? C39 C40 1.398(5) . ? C40 C41 1.391(5) . ? C41 C42 1.370(6) . ? C42 C43 1.371(7) . ? C43 C44 1.396(6) . ? C45 C46 1.385(5) . ? C45 C50 1.399(5) . ? C46 C47 1.384(5) . ? C47 C48 1.379(6) . ? C48 C49 1.369(6) . ? C49 C50 1.383(5) . ? C51 Cl1 1.727(7) . ? C51 Cl2 1.740(7) . ? C52 Cl4 1.690(7) . ? C52 Cl3 1.746(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 C2 Fe1 C1 91.17(17) . . ? C2 Fe1 P1 96.23(12) . . ? C1 Fe1 P1 98.66(12) . . ? C2 Fe1 S3 94.56(13) . . ? C1 Fe1 S3 161.71(12) . . ? P1 Fe1 S3 97.95(4) . . ? C2 Fe1 S1 155.47(12) . . ? C1 Fe1 S1 87.42(12) . . ? P1 Fe1 S1 108.20(4) . . ? S3 Fe1 S1 80.18(4) . . ? C2 Fe1 Fe2 100.54(12) . . ? C1 Fe1 Fe2 104.97(12) . . ? P1 Fe1 Fe2 150.56(3) . . ? S3 Fe1 Fe2 56.91(3) . . ? S1 Fe1 Fe2 56.49(3) . . ? C4 Fe2 C3 92.93(18) . . ? C4 Fe2 C5 100.00(19) . . ? C3 Fe2 C5 99.2(2) . . ? C4 Fe2 S1 158.67(14) . . ? C3 Fe2 S1 87.72(13) . . ? C5 Fe2 S1 100.93(14) . . ? C4 Fe2 S3 91.02(13) . . ? C3 Fe2 S3 154.11(14) . . ? C5 Fe2 S3 105.24(15) . . ? S1 Fe2 S3 79.59(3) . . ? C4 Fe2 Fe1 102.29(14) . . ? C3 Fe2 Fe1 98.49(13) . . ? C5 Fe2 Fe1 150.62(14) . . ? S1 Fe2 Fe1 56.63(3) . . ? S3 Fe2 Fe1 55.71(3) . . ? C6 Fe3 C7 91.76(16) . . ? C6 Fe3 P2 93.56(12) . . ? C7 Fe3 P2 97.09(12) . . ? C6 Fe3 S4 157.97(13) . . ? C7 Fe3 S4 94.25(12) . . ? P2 Fe3 S4 106.66(4) . . ? C6 Fe3 S2 85.22(12) . . ? C7 Fe3 S2 151.41(12) . . ? P2 Fe3 S2 111.46(4) . . ? S4 Fe3 S2 79.40(3) . . ? C6 Fe3 Fe4 101.54(12) . . ? C7 Fe3 Fe4 96.78(12) . . ? P2 Fe3 Fe4 159.11(3) . . ? S4 Fe3 Fe4 56.71(3) . . ? S2 Fe3 Fe4 56.36(3) . . ? C9 Fe4 C8 91.01(19) . . ? C9 Fe4 C10 100.9(2) . . ? C8 Fe4 C10 101.5(2) . . ? C9 Fe4 S2 158.00(14) . . ? C8 Fe4 S2 87.24(14) . . ? C10 Fe4 S2 100.98(14) . . ? C9 Fe4 S4 92.66(13) . . ? C8 Fe4 S4 153.08(14) . . ? C10 Fe4 S4 103.96(15) . . ? S2 Fe4 S4 79.51(3) . . ? C9 Fe4 Fe3 101.64(13) . . ? C8 Fe4 Fe3 96.80(14) . . ? C10 Fe4 Fe3 150.60(15) . . ? S2 Fe4 Fe3 56.92(3) . . ? S4 Fe4 Fe3 56.35(3) . . ? C11 S1 Fe2 108.71(12) . . ? C11 S1 Fe1 117.87(12) . . ? Fe2 S1 Fe1 66.88(3) . . ? C14 S2 Fe4 110.36(13) . . ? C14 S2 Fe3 118.65(14) . . ? Fe4 S2 Fe3 66.72(3) . . ? C18 S3 Fe1 114.58(13) . . ? C18 S3 Fe2 116.80(13) . . ? Fe1 S3 Fe2 67.38(3) . . ? C21 S4 Fe3 114.92(13) . . ? C21 S4 Fe4 115.42(13) . . ? Fe3 S4 Fe4 66.94(3) . . ? C27 P1 C33 105.06(16) . . ? C27 P1 C25 105.36(15) . . ? C33 P1 C25 100.10(15) . . ? C27 P1 Fe1 111.35(11) . . ? C33 P1 Fe1 118.57(11) . . ? C25 P1 Fe1 114.93(11) . . ? C45 P2 C39 102.63(16) . . ? C45 P2 C26 104.19(16) . . ? C39 P2 C26 98.07(15) . . ? C45 P2 Fe3 117.39(12) . . ? C39 P2 Fe3 112.66(11) . . ? C26 P2 Fe3 119.06(11) . . ? C12 N1 C13 113.5(3) . . ? C12 N1 C15 115.6(3) . . ? C13 N1 C15 112.6(3) . . ? C19 N2 C20 115.0(3) . . ? C19 N2 C22 113.1(3) . . ? C20 N2 C22 113.9(3) . . ? O1 C1 Fe1 178.5(4) . . ? O2 C2 Fe1 179.4(4) . . ? O3 C3 Fe2 179.6(4) . . ? O4 C4 Fe2 178.5(4) . . ? O5 C5 Fe2 176.6(4) . . ? O6 C6 Fe3 176.7(4) . . ? O7 C7 Fe3 175.8(3) . . ? O8 C8 Fe4 177.5(4) . . ? O9 C9 Fe4 178.1(4) . . ? O10 C10 Fe4 178.2(5) . . ? C12 C11 S1 110.6(2) . . ? N1 C12 C11 109.3(3) . . ? N1 C13 C14 111.2(3) . . ? C13 C14 S2 111.2(3) . . ? N1 C15 C17 110.4(3) . . ? N1 C15 C16 113.6(3) . . ? C17 C15 C16 113.4(4) . . ? C19 C18 S3 110.2(3) . . ? N2 C19 C18 113.8(3) . . ? N2 C20 C21 114.4(3) . . ? C20 C21 S4 113.0(3) . . ? N2 C22 C23 111.1(4) . . ? N2 C22 C24 114.1(4) . . ? C23 C22 C24 113.1(5) . . ? C26 C25 P1 116.0(2) . . ? C25 C26 P2 116.0(2) . . ? C28 C27 C32 118.1(3) . . ? C28 C27 P1 121.2(3) . . ? C32 C27 P1 120.1(3) . . ? C29 C28 C27 120.8(3) . . ? C30 C29 C28 120.1(3) . . ? C29 C30 C31 120.0(4) . . ? C30 C31 C32 120.2(4) . . ? C31 C32 C27 120.7(3) . . ? C38 C33 C34 118.1(3) . . ? C38 C33 P1 118.5(3) . . ? C34 C33 P1 123.0(3) . . ? C35 C34 C33 120.5(3) . . ? C36 C35 C34 120.2(3) . . ? C37 C36 C35 119.9(4) . . ? C36 C37 C38 120.4(4) . . ? C37 C38 C33 120.8(3) . . ? C44 C39 C40 118.3(3) . . ? C44 C39 P2 122.3(3) . . ? C40 C39 P2 119.4(3) . . ? C41 C40 C39 121.2(4) . . ? C42 C41 C40 119.6(4) . . ? C41 C42 C43 120.1(4) . . ? C42 C43 C44 121.0(4) . . ? C39 C44 C43 119.8(4) . . ? C46 C45 C50 118.1(3) . . ? C46 C45 P2 122.5(3) . . ? C50 C45 P2 119.4(3) . . ? C47 C46 C45 120.6(4) . . ? C48 C47 C46 120.6(4) . . ? C49 C48 C47 119.5(4) . . ? C48 C49 C50 120.4(4) . . ? C49 C50 C45 120.8(4) . . ? Cl1 C51 Cl2 112.5(3) . . ? Cl4 C52 Cl3 114.6(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.307 _refine_diff_density_min -1.474 _refine_diff_density_rms 0.104 # Attachment '- complex_3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 793183' #TrackingRef '- complex_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H68 Fe4 O8 P4 S4' _chemical_formula_weight 1512.76 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.63200(10) _cell_length_b 17.8511(2) _cell_length_c 20.8444(2) _cell_angle_alpha 110.0752(6) _cell_angle_beta 96.6827(6) _cell_angle_gamma 106.1587(6) _cell_volume 3469.11(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42631 _cell_measurement_theta_min 1.07 _cell_measurement_theta_max 27.59 _exptl_crystal_description irregular-block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42631 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15859 _reflns_number_gt 12399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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. ; _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^)+(0.0330P)^2^+1.5216P] 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 15859 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 0.12310(3) 0.278070(18) 0.754736(15) 0.02392(7) Uani 1 1 d . . . Fe2 Fe 0.06294(3) 0.220609(19) 0.847865(15) 0.02938(8) Uani 1 1 d . . . Fe3 Fe -0.09078(3) -0.255850(18) 0.749149(15) 0.02287(7) Uani 1 1 d . . . Fe4 Fe -0.09601(3) -0.212169(19) 0.645097(15) 0.02691(7) Uani 1 1 d . . . S1 S 0.26056(6) 0.23466(3) 0.81411(3) 0.02829(12) Uani 1 1 d . . . S2 S 0.09603(5) -0.19487(3) 0.71746(3) 0.02517(11) Uani 1 1 d . . . S3 S -0.01465(5) 0.14635(3) 0.72952(3) 0.02493(11) Uani 1 1 d . . . S4 S -0.12982(5) -0.13775(3) 0.75065(3) 0.02574(11) Uani 1 1 d . . . P1 P 0.16768(6) 0.26464(3) 0.65234(3) 0.02701(12) Uani 1 1 d . . . P2 P 0.26157(6) 0.41009(3) 0.79391(3) 0.02776(12) Uani 1 1 d . . . P3 P -0.05113(5) -0.24152(3) 0.85865(3) 0.02432(11) Uani 1 1 d . . . P4 P -0.05115(5) -0.37759(3) 0.72089(3) 0.02441(11) Uani 1 1 d . . . C1 C -0.0105(2) 0.31386(13) 0.74209(11) 0.0297(5) Uani 1 1 d . . . C2 C -0.0865(3) 0.24493(16) 0.85677(12) 0.0419(6) Uani 1 1 d . . . C3 C 0.1516(3) 0.30682(15) 0.92909(13) 0.0425(6) Uani 1 1 d . . . C4 C 0.0390(2) 0.12984(14) 0.87157(11) 0.0315(5) Uani 1 1 d . . . C5 C -0.2578(2) -0.31138(13) 0.74208(11) 0.0282(5) Uani 1 1 d . . . C6 C -0.0627(3) -0.29250(15) 0.57732(12) 0.0374(5) Uani 1 1 d . . . C7 C -0.2701(3) -0.26430(15) 0.60734(12) 0.0375(5) Uani 1 1 d . . . C8 C -0.0519(2) -0.12331(14) 0.61902(11) 0.0302(5) Uani 1 1 d . . . C9 C 0.2685(2) 0.12869(13) 0.76713(11) 0.0300(5) Uani 1 1 d . . . H9A H 0.1769 0.0859 0.7513 0.036 Uiso 1 1 calc R . . H9B H 0.3042 0.1273 0.7251 0.036 Uiso 1 1 calc R . . C10 C 0.3588(2) 0.10716(13) 0.81482(13) 0.0344(5) Uani 1 1 d . . . H10A H 0.3102 0.0924 0.8489 0.041 Uiso 1 1 calc R . . H10B H 0.4400 0.1578 0.8417 0.041 Uiso 1 1 calc R . . C11 C 0.4023(2) 0.03332(14) 0.77412(15) 0.0417(6) Uani 1 1 d . . . H11A H 0.4578 0.0211 0.8082 0.050 Uiso 1 1 calc R . . H11B H 0.4601 0.0512 0.7444 0.050 Uiso 1 1 calc R . . C12 C 0.2869(2) -0.04856(13) 0.72737(12) 0.0322(5) Uani 1 1 d . . . H12A H 0.2365 -0.0383 0.6901 0.039 Uiso 1 1 calc R . . H12B H 0.3251 -0.0927 0.7043 0.039 Uiso 1 1 calc R . . C13 C 0.1899(2) -0.08138(13) 0.76748(11) 0.0284(5) Uani 1 1 d . . . H13A H 0.1262 -0.0497 0.7751 0.034 Uiso 1 1 calc R . . H13B H 0.2406 -0.0725 0.8140 0.034 Uiso 1 1 calc R . . C14 C -0.1924(2) 0.12729(13) 0.69559(12) 0.0299(5) Uani 1 1 d . . . H14A H -0.2269 0.1619 0.7327 0.036 Uiso 1 1 calc R . . H14B H -0.2014 0.1447 0.6555 0.036 Uiso 1 1 calc R . . C15 C -0.2754(2) 0.03385(14) 0.67176(12) 0.0324(5) Uani 1 1 d . . . H15A H -0.2474 0.0007 0.6307 0.039 Uiso 1 1 calc R . . H15B H -0.3713 0.0262 0.6561 0.039 Uiso 1 1 calc R . . C16 C -0.2627(2) -0.00236(14) 0.72778(12) 0.0315(5) Uani 1 1 d . . . H16A H -0.1668 0.0054 0.7439 0.038 Uiso 1 1 calc R . . H16B H -0.2923 0.0297 0.7686 0.038 Uiso 1 1 calc R . . C17 C -0.3458(2) -0.09604(14) 0.70118(13) 0.0361(5) Uani 1 1 d . . . H17A H -0.3375 -0.1249 0.6528 0.043 Uiso 1 1 calc R . . H17B H -0.4417 -0.1018 0.6989 0.043 Uiso 1 1 calc R . . C18 C -0.3049(2) -0.14148(15) 0.74648(13) 0.0351(5) Uani 1 1 d . . . H18A H -0.3654 -0.2014 0.7265 0.042 Uiso 1 1 calc R . . H18B H -0.3158 -0.1143 0.7946 0.042 Uiso 1 1 calc R . . C19 C 0.2329(3) 0.37110(14) 0.64886(12) 0.0374(5) Uani 1 1 d . . . H19A H 0.3214 0.3787 0.6364 0.045 Uiso 1 1 calc R . . H19B H 0.1703 0.3743 0.6116 0.045 Uiso 1 1 calc R . . C20 C 0.2485(3) 0.44243(14) 0.71884(12) 0.0377(5) Uani 1 1 d . . . H20A H 0.1701 0.4617 0.7161 0.045 Uiso 1 1 calc R . . H20B H 0.3303 0.4910 0.7271 0.045 Uiso 1 1 calc R . . C21 C 0.2968(2) 0.22018(13) 0.62193(12) 0.0320(5) Uani 1 1 d . . . C22 C 0.4075(2) 0.23043(14) 0.67056(13) 0.0361(5) Uani 1 1 d . . . H22 H 0.4138 0.2585 0.7193 0.043 Uiso 1 1 calc R . . C23 C 0.5096(3) 0.20038(16) 0.64927(15) 0.0473(6) Uani 1 1 d . . . H23 H 0.5846 0.2079 0.6834 0.057 Uiso 1 1 calc R . . C24 C 0.5020(3) 0.16003(17) 0.57923(17) 0.0528(7) Uani 1 1 d . . . H24 H 0.5705 0.1382 0.5648 0.063 Uiso 1 1 calc R . . C25 C 0.3955(3) 0.15112(16) 0.52990(15) 0.0542(8) Uani 1 1 d . . . H25 H 0.3919 0.1244 0.4814 0.065 Uiso 1 1 calc R . . C26 C 0.2918(3) 0.18116(16) 0.55049(13) 0.0443(6) Uani 1 1 d . . . H26 H 0.2185 0.1750 0.5161 0.053 Uiso 1 1 calc R . . C27 C 0.0183(2) 0.20077(14) 0.58058(11) 0.0309(5) Uani 1 1 d . . . C28 C -0.0241(2) 0.11213(14) 0.55859(12) 0.0354(5) Uani 1 1 d . . . H28 H 0.0301 0.0869 0.5775 0.043 Uiso 1 1 calc R . . C29 C -0.1442(3) 0.06136(17) 0.50961(13) 0.0456(6) Uani 1 1 d . . . H29 H -0.1722 0.0015 0.4953 0.055 Uiso 1 1 calc R . . C30 C -0.2233(3) 0.0969(2) 0.48142(14) 0.0535(7) Uani 1 1 d . . . H30 H -0.3048 0.0614 0.4471 0.064 Uiso 1 1 calc R . . C31 C -0.1847(3) 0.1838(2) 0.50289(14) 0.0509(7) Uani 1 1 d . . . H31 H -0.2398 0.2083 0.4838 0.061 Uiso 1 1 calc R . . C32 C -0.0642(2) 0.23559(17) 0.55283(12) 0.0403(6) Uani 1 1 d . . . H32 H -0.0384 0.2955 0.5680 0.048 Uiso 1 1 calc R . . C33 C 0.2340(2) 0.49804(13) 0.86201(11) 0.0310(5) Uani 1 1 d . . . C34 C 0.3234(2) 0.58080(14) 0.88291(13) 0.0392(6) Uani 1 1 d . . . H34 H 0.3980 0.5912 0.8622 0.047 Uiso 1 1 calc R . . C35 C 0.3033(3) 0.64796(15) 0.93393(13) 0.0441(6) Uani 1 1 d . . . H35 H 0.3639 0.7041 0.9478 0.053 Uiso 1 1 calc R . . C36 C 0.1956(3) 0.63327(16) 0.96442(12) 0.0433(6) Uani 1 1 d . . . H36 H 0.1828 0.6793 0.9996 0.052 Uiso 1 1 calc R . . C37 C 0.1069(3) 0.55238(15) 0.94414(12) 0.0396(6) Uani 1 1 d . . . H37 H 0.0324 0.5425 0.9650 0.048 Uiso 1 1 calc R . . C38 C 0.1262(2) 0.48422(14) 0.89241(11) 0.0348(5) Uani 1 1 d . . . H38 H 0.0646 0.4283 0.8784 0.042 Uiso 1 1 calc R . . C39 C 0.4397(2) 0.43049(13) 0.82617(11) 0.0300(5) Uani 1 1 d . . . C40 C 0.5320(3) 0.43340(16) 0.78453(14) 0.0456(6) Uani 1 1 d . . . H40 H 0.5067 0.4334 0.7393 0.055 Uiso 1 1 calc R . . C41 C 0.6615(3) 0.43634(18) 0.80861(17) 0.0584(8) Uani 1 1 d . . . H41 H 0.7235 0.4369 0.7793 0.070 Uiso 1 1 calc R . . C42 C 0.7005(3) 0.43850(17) 0.87449(17) 0.0565(8) Uani 1 1 d . . . H42 H 0.7890 0.4400 0.8905 0.068 Uiso 1 1 calc R . . C43 C 0.6109(3) 0.43842(16) 0.91779(15) 0.0471(6) Uani 1 1 d . . . H43 H 0.6385 0.4415 0.9639 0.057 Uiso 1 1 calc R . . C44 C 0.4811(2) 0.43381(14) 0.89336(13) 0.0364(5) Uani 1 1 d . . . H44 H 0.4194 0.4329 0.9228 0.044 Uiso 1 1 calc R . . C45 C -0.0953(2) -0.35040(13) 0.85518(11) 0.0291(5) Uani 1 1 d . . . H45A H -0.0650 -0.3495 0.9023 0.035 Uiso 1 1 calc R . . H45B H -0.1941 -0.3797 0.8391 0.035 Uiso 1 1 calc R . . C46 C -0.0236(2) -0.39618(13) 0.80297(11) 0.0283(5) Uani 1 1 d . . . H46A H -0.0588 -0.4578 0.7919 0.034 Uiso 1 1 calc R . . H46B H 0.0742 -0.3750 0.8245 0.034 Uiso 1 1 calc R . . C47 C -0.1519(2) -0.19174(14) 0.91270(11) 0.0284(5) Uani 1 1 d . . . C48 C -0.1269(2) -0.10569(14) 0.92855(12) 0.0347(5) Uani 1 1 d . . . H48 H -0.0612 -0.0762 0.9104 0.042 Uiso 1 1 calc R . . C49 C -0.1971(3) -0.06293(17) 0.97051(13) 0.0427(6) Uani 1 1 d . . . H49 H -0.1798 -0.0044 0.9807 0.051 Uiso 1 1 calc R . . C50 C -0.2909(3) -0.10460(19) 0.99732(14) 0.0483(7) Uani 1 1 d . . . H50 H -0.3376 -0.0747 1.0268 0.058 Uiso 1 1 calc R . . C51 C -0.3184(2) -0.19027(19) 0.98165(14) 0.0492(7) Uani 1 1 d . . . H51 H -0.3843 -0.2191 1.0001 0.059 Uiso 1 1 calc R . . C52 C -0.2497(2) -0.23401(16) 0.93897(12) 0.0378(5) Uani 1 1 d . . . H52 H -0.2696 -0.2930 0.9277 0.045 Uiso 1 1 calc R . . C53 C 0.1154(2) -0.18925(12) 0.92054(11) 0.0252(4) Uani 1 1 d . . . C54 C 0.1261(2) -0.17362(13) 0.99139(11) 0.0308(5) Uani 1 1 d . . . H54 H 0.0473 -0.1906 1.0076 0.037 Uiso 1 1 calc R . . C55 C 0.2507(2) -0.13356(14) 1.03871(12) 0.0351(5) Uani 1 1 d . . . H55 H 0.2568 -0.1231 1.0870 0.042 Uiso 1 1 calc R . . C56 C 0.3651(2) -0.10900(15) 1.01570(12) 0.0377(5) Uani 1 1 d . . . H56 H 0.4502 -0.0808 1.0483 0.045 Uiso 1 1 calc R . . C57 C 0.3568(2) -0.12519(15) 0.94535(12) 0.0354(5) Uani 1 1 d . . . H57 H 0.4363 -0.1089 0.9295 0.042 Uiso 1 1 calc R . . C58 C 0.2323(2) -0.16528(13) 0.89776(11) 0.0290(5) Uani 1 1 d . . . H58 H 0.2270 -0.1764 0.8494 0.035 Uiso 1 1 calc R . . C59 C -0.1849(2) -0.47496(13) 0.65889(11) 0.0266(4) Uani 1 1 d . . . C60 C -0.1826(2) -0.55374(13) 0.65587(12) 0.0328(5) Uani 1 1 d . . . H60 H -0.1114 -0.5565 0.6860 0.039 Uiso 1 1 calc R . . C61 C -0.2822(2) -0.62769(14) 0.60982(13) 0.0404(6) Uani 1 1 d . . . H61 H -0.2803 -0.6809 0.6090 0.049 Uiso 1 1 calc R . . C62 C -0.3845(3) -0.62420(15) 0.56488(14) 0.0453(6) Uani 1 1 d . . . H62 H -0.4533 -0.6751 0.5332 0.054 Uiso 1 1 calc R . . C63 C -0.3869(3) -0.54704(15) 0.56595(14) 0.0463(6) Uani 1 1 d . . . H63 H -0.4569 -0.5448 0.5347 0.056 Uiso 1 1 calc R . . C64 C -0.2874(2) -0.47279(14) 0.61258(12) 0.0356(5) Uani 1 1 d . . . H64 H -0.2894 -0.4198 0.6129 0.043 Uiso 1 1 calc R . . C65 C 0.0967(2) -0.38961(13) 0.68722(12) 0.0295(5) Uani 1 1 d . . . C66 C 0.0863(3) -0.43826(15) 0.61730(13) 0.0391(6) Uani 1 1 d . . . H66 H -0.0002 -0.4697 0.5863 0.047 Uiso 1 1 calc R . . C67 C 0.2009(3) -0.44133(18) 0.59222(15) 0.0509(7) Uani 1 1 d . . . H67 H 0.1926 -0.4754 0.5445 0.061 Uiso 1 1 calc R . . C68 C 0.3269(3) -0.39490(18) 0.63656(17) 0.0526(7) Uani 1 1 d . . . H68 H 0.4054 -0.3961 0.6193 0.063 Uiso 1 1 calc R . . C69 C 0.3381(2) -0.34685(16) 0.70590(16) 0.0468(7) Uani 1 1 d . . . H69 H 0.4247 -0.3155 0.7367 0.056 Uiso 1 1 calc R . . C70 C 0.2246(2) -0.34390(14) 0.73096(13) 0.0363(5) Uani 1 1 d . . . H70 H 0.2339 -0.3101 0.7789 0.044 Uiso 1 1 calc R . . O1 O -0.10225(17) 0.33555(10) 0.73425(9) 0.0423(4) Uani 1 1 d . . . O2 O -0.1822(2) 0.26191(14) 0.86292(10) 0.0638(6) Uani 1 1 d . . . O3 O 0.2069(2) 0.36276(12) 0.98152(10) 0.0663(6) Uani 1 1 d . . . O4 O 0.02172(18) 0.07185(10) 0.88533(8) 0.0413(4) Uani 1 1 d . . . O5 O -0.36804(16) -0.34792(10) 0.74002(9) 0.0427(4) Uani 1 1 d . . . O6 O -0.0460(2) -0.34568(11) 0.53340(9) 0.0556(5) Uani 1 1 d . . . O7 O -0.38365(18) -0.30009(12) 0.58297(10) 0.0532(5) Uani 1 1 d . . . O8 O -0.02935(17) -0.06550(10) 0.60464(8) 0.0403(4) 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 0.03242(16) 0.01910(15) 0.02221(15) 0.00865(12) 0.00603(12) 0.01123(13) Fe2 0.04565(19) 0.02358(16) 0.02314(16) 0.01022(13) 0.01114(14) 0.01553(15) Fe3 0.02478(15) 0.02062(15) 0.02451(15) 0.01096(12) 0.00359(12) 0.00792(12) Fe4 0.03187(16) 0.02363(16) 0.02423(16) 0.01113(13) 0.00263(13) 0.00742(13) S1 0.0364(3) 0.0213(3) 0.0265(3) 0.0092(2) 0.0024(2) 0.0112(2) S2 0.0275(3) 0.0209(3) 0.0278(3) 0.0102(2) 0.0063(2) 0.0087(2) S3 0.0306(3) 0.0209(3) 0.0251(3) 0.0095(2) 0.0070(2) 0.0108(2) S4 0.0261(3) 0.0245(3) 0.0305(3) 0.0140(2) 0.0062(2) 0.0104(2) P1 0.0347(3) 0.0222(3) 0.0237(3) 0.0089(2) 0.0080(2) 0.0090(2) P2 0.0371(3) 0.0196(3) 0.0257(3) 0.0087(2) 0.0034(2) 0.0101(2) P3 0.0268(3) 0.0231(3) 0.0246(3) 0.0108(2) 0.0049(2) 0.0093(2) P4 0.0269(3) 0.0205(3) 0.0254(3) 0.0098(2) 0.0028(2) 0.0080(2) C1 0.0413(13) 0.0221(11) 0.0280(11) 0.0122(9) 0.0094(10) 0.0106(10) C2 0.0647(17) 0.0422(14) 0.0322(13) 0.0188(11) 0.0208(12) 0.0290(13) C3 0.0680(17) 0.0301(13) 0.0341(14) 0.0163(12) 0.0181(13) 0.0167(13) C4 0.0400(13) 0.0310(12) 0.0230(11) 0.0085(10) 0.0086(10) 0.0139(10) C5 0.0326(12) 0.0251(11) 0.0295(12) 0.0122(9) 0.0022(9) 0.0140(10) C6 0.0508(15) 0.0304(13) 0.0308(13) 0.0162(11) 0.0054(11) 0.0097(11) C7 0.0460(15) 0.0326(13) 0.0325(13) 0.0164(11) 0.0007(11) 0.0100(11) C8 0.0333(12) 0.0323(12) 0.0256(11) 0.0111(10) 0.0066(9) 0.0125(10) C9 0.0390(12) 0.0247(11) 0.0304(12) 0.0117(9) 0.0097(10) 0.0153(10) C10 0.0295(11) 0.0219(11) 0.0459(14) 0.0114(10) -0.0012(10) 0.0066(9) C11 0.0277(12) 0.0277(12) 0.0715(18) 0.0201(12) 0.0116(12) 0.0114(10) C12 0.0277(11) 0.0244(11) 0.0478(14) 0.0133(10) 0.0167(10) 0.0117(9) C13 0.0311(11) 0.0223(11) 0.0284(11) 0.0097(9) 0.0027(9) 0.0064(9) C14 0.0328(11) 0.0273(11) 0.0348(12) 0.0159(10) 0.0076(10) 0.0136(10) C15 0.0294(11) 0.0327(12) 0.0395(13) 0.0179(11) 0.0056(10) 0.0134(10) C16 0.0294(11) 0.0314(12) 0.0389(13) 0.0177(10) 0.0074(10) 0.0136(10) C17 0.0247(11) 0.0340(13) 0.0544(15) 0.0234(12) 0.0051(10) 0.0114(10) C18 0.0291(11) 0.0347(13) 0.0503(15) 0.0250(11) 0.0121(11) 0.0125(10) C19 0.0552(15) 0.0272(12) 0.0295(12) 0.0143(10) 0.0106(11) 0.0093(11) C20 0.0547(15) 0.0238(12) 0.0330(13) 0.0134(10) 0.0037(11) 0.0108(11) C21 0.0360(12) 0.0221(11) 0.0340(12) 0.0080(10) 0.0147(10) 0.0053(10) C22 0.0378(13) 0.0314(12) 0.0413(14) 0.0168(11) 0.0127(11) 0.0105(10) C23 0.0401(14) 0.0462(16) 0.0643(19) 0.0271(14) 0.0213(13) 0.0173(12) C24 0.0451(16) 0.0373(15) 0.077(2) 0.0174(15) 0.0317(16) 0.0146(13) C25 0.0523(17) 0.0368(15) 0.0510(17) -0.0035(13) 0.0284(15) 0.0016(13) C26 0.0395(14) 0.0424(15) 0.0361(14) 0.0055(12) 0.0132(11) 0.0027(12) C27 0.0344(12) 0.0356(13) 0.0234(11) 0.0113(10) 0.0117(9) 0.0117(10) C28 0.0384(13) 0.0343(13) 0.0305(12) 0.0081(10) 0.0147(10) 0.0110(11) C29 0.0405(14) 0.0408(15) 0.0373(14) 0.0014(12) 0.0156(12) 0.0021(12) C30 0.0326(13) 0.072(2) 0.0321(14) 0.0044(14) 0.0062(11) 0.0039(14) C31 0.0410(15) 0.077(2) 0.0402(15) 0.0243(15) 0.0089(12) 0.0263(15) C32 0.0436(14) 0.0477(15) 0.0338(13) 0.0184(12) 0.0111(11) 0.0180(12) C33 0.0413(13) 0.0205(11) 0.0271(11) 0.0057(9) -0.0028(10) 0.0135(10) C34 0.0396(13) 0.0286(12) 0.0444(14) 0.0099(11) 0.0017(11) 0.0132(11) C35 0.0534(16) 0.0220(12) 0.0439(15) 0.0044(11) -0.0084(12) 0.0123(11) C36 0.0628(17) 0.0358(14) 0.0292(13) 0.0035(11) -0.0021(12) 0.0306(13) C37 0.0540(15) 0.0399(14) 0.0320(13) 0.0139(11) 0.0100(11) 0.0268(12) C38 0.0463(14) 0.0289(12) 0.0298(12) 0.0105(10) 0.0044(10) 0.0171(11) C39 0.0347(12) 0.0188(10) 0.0320(12) 0.0071(9) 0.0058(10) 0.0069(9) C40 0.0417(14) 0.0414(15) 0.0395(15) 0.0095(12) 0.0097(12) 0.0015(12) C41 0.0356(14) 0.0541(18) 0.062(2) 0.0032(15) 0.0176(14) 0.0022(13) C42 0.0323(14) 0.0440(16) 0.076(2) 0.0084(15) 0.0010(14) 0.0113(12) C43 0.0455(15) 0.0401(15) 0.0494(16) 0.0147(13) -0.0043(13) 0.0150(12) C44 0.0399(13) 0.0315(12) 0.0394(13) 0.0153(11) 0.0072(11) 0.0138(11) C45 0.0333(12) 0.0266(11) 0.0289(11) 0.0146(9) 0.0039(9) 0.0090(9) C46 0.0330(11) 0.0229(11) 0.0284(11) 0.0109(9) 0.0015(9) 0.0100(9) C47 0.0283(11) 0.0324(12) 0.0252(11) 0.0112(9) 0.0037(9) 0.0123(10) C48 0.0412(13) 0.0350(13) 0.0348(13) 0.0161(11) 0.0102(10) 0.0197(11) C49 0.0505(15) 0.0441(15) 0.0377(14) 0.0125(12) 0.0058(12) 0.0291(13) C50 0.0395(14) 0.0652(19) 0.0410(15) 0.0102(13) 0.0101(12) 0.0324(14) C51 0.0293(13) 0.071(2) 0.0433(15) 0.0195(14) 0.0147(11) 0.0127(13) C52 0.0332(12) 0.0421(14) 0.0359(13) 0.0151(11) 0.0072(10) 0.0100(11) C53 0.0293(11) 0.0210(10) 0.0261(11) 0.0090(9) 0.0038(9) 0.0110(9) C54 0.0338(12) 0.0302(12) 0.0282(12) 0.0103(10) 0.0064(10) 0.0125(10) C55 0.0410(13) 0.0346(13) 0.0249(12) 0.0073(10) 0.0005(10) 0.0145(11) C56 0.0332(12) 0.0363(13) 0.0353(13) 0.0092(11) -0.0015(10) 0.0097(10) C57 0.0285(11) 0.0376(13) 0.0391(13) 0.0164(11) 0.0067(10) 0.0088(10) C58 0.0309(11) 0.0284(11) 0.0299(12) 0.0135(10) 0.0063(9) 0.0111(9) C59 0.0294(11) 0.0222(10) 0.0258(11) 0.0086(9) 0.0036(9) 0.0076(9) C60 0.0355(12) 0.0283(12) 0.0346(13) 0.0135(10) 0.0015(10) 0.0121(10) C61 0.0488(14) 0.0226(12) 0.0425(14) 0.0115(11) 0.0006(12) 0.0071(11) C62 0.0449(14) 0.0281(13) 0.0443(15) 0.0090(11) -0.0104(12) 0.0000(11) C63 0.0460(14) 0.0335(14) 0.0460(15) 0.0125(12) -0.0134(12) 0.0072(12) C64 0.0388(13) 0.0262(12) 0.0367(13) 0.0123(10) -0.0033(10) 0.0086(10) C65 0.0323(11) 0.0223(11) 0.0391(13) 0.0152(10) 0.0102(10) 0.0124(9) C66 0.0408(13) 0.0392(14) 0.0403(14) 0.0176(11) 0.0122(11) 0.0146(11) C67 0.0594(18) 0.0554(17) 0.0497(17) 0.0242(14) 0.0297(14) 0.0258(15) C68 0.0437(15) 0.0514(17) 0.080(2) 0.0348(16) 0.0334(15) 0.0240(14) C69 0.0311(13) 0.0368(14) 0.076(2) 0.0233(14) 0.0161(13) 0.0137(11) C70 0.0321(12) 0.0274(12) 0.0487(15) 0.0135(11) 0.0076(11) 0.0118(10) O1 0.0458(10) 0.0417(10) 0.0528(11) 0.0251(9) 0.0124(8) 0.0261(8) O2 0.0831(15) 0.0854(15) 0.0589(13) 0.0359(12) 0.0404(12) 0.0631(13) O3 0.1155(18) 0.0325(10) 0.0305(10) 0.0037(9) 0.0092(11) 0.0095(11) O4 0.0596(11) 0.0305(9) 0.0374(9) 0.0186(8) 0.0099(8) 0.0146(8) O5 0.0271(9) 0.0393(10) 0.0617(12) 0.0242(9) 0.0079(8) 0.0070(8) O6 0.0971(16) 0.0369(10) 0.0357(10) 0.0114(8) 0.0213(10) 0.0288(11) O7 0.0389(10) 0.0485(11) 0.0559(12) 0.0207(9) -0.0116(9) -0.0001(9) O8 0.0581(11) 0.0332(9) 0.0403(10) 0.0228(8) 0.0180(8) 0.0185(8) _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 C1 1.741(2) . ? Fe1 P1 2.1875(6) . ? Fe1 P2 2.2036(6) . ? Fe1 S3 2.2374(6) . ? Fe1 S1 2.2663(6) . ? Fe1 Fe2 2.5535(4) . ? Fe2 C2 1.773(3) . ? Fe2 C3 1.777(3) . ? Fe2 C4 1.812(2) . ? Fe2 S1 2.2681(6) . ? Fe2 S3 2.2794(6) . ? Fe3 C5 1.737(2) . ? Fe3 P3 2.1836(6) . ? Fe3 P4 2.2216(6) . ? Fe3 S4 2.2501(6) . ? Fe3 S2 2.2718(6) . ? Fe3 Fe4 2.5441(4) . ? Fe4 C7 1.763(3) . ? Fe4 C6 1.785(3) . ? Fe4 C8 1.808(2) . ? Fe4 S2 2.2698(6) . ? Fe4 S4 2.2755(6) . ? S1 C9 1.839(2) . ? S2 C13 1.836(2) . ? S3 C14 1.831(2) . ? S4 C18 1.835(2) . ? P1 C27 1.824(2) . ? P1 C21 1.839(2) . ? P1 C19 1.863(2) . ? P2 C39 1.822(2) . ? P2 C33 1.841(2) . ? P2 C20 1.848(2) . ? P3 C47 1.825(2) . ? P3 C53 1.842(2) . ? P3 C45 1.841(2) . ? P4 C65 1.830(2) . ? P4 C59 1.835(2) . ? P4 C46 1.858(2) . ? C1 O1 1.159(3) . ? C2 O2 1.149(3) . ? C3 O3 1.145(3) . ? C4 O4 1.139(3) . ? C5 O5 1.160(3) . ? C6 O6 1.143(3) . ? C7 O7 1.153(3) . ? C8 O8 1.142(2) . ? C9 C10 1.517(3) . ? C10 C11 1.528(3) . ? C11 C12 1.529(3) . ? C12 C13 1.519(3) . ? C14 C15 1.522(3) . ? C15 C16 1.526(3) . ? C16 C17 1.520(3) . ? C17 C18 1.538(3) . ? C19 C20 1.526(3) . ? C21 C22 1.386(3) . ? C21 C26 1.398(3) . ? C22 C23 1.391(3) . ? C23 C24 1.369(4) . ? C24 C25 1.372(4) . ? C25 C26 1.403(4) . ? C27 C32 1.387(3) . ? C27 C28 1.405(3) . ? C28 C29 1.382(3) . ? C29 C30 1.376(4) . ? C30 C31 1.379(4) . ? C31 C32 1.396(4) . ? C33 C38 1.376(3) . ? C33 C34 1.399(3) . ? C34 C35 1.391(3) . ? C35 C36 1.378(4) . ? C36 C37 1.373(4) . ? C37 C38 1.406(3) . ? C39 C40 1.386(3) . ? C39 C44 1.394(3) . ? C40 C41 1.390(4) . ? C41 C42 1.372(4) . ? C42 C43 1.386(4) . ? C43 C44 1.384(3) . ? C45 C46 1.538(3) . ? C47 C52 1.389(3) . ? C47 C48 1.394(3) . ? C48 C49 1.383(3) . ? C49 C50 1.365(4) . ? C50 C51 1.385(4) . ? C51 C52 1.388(3) . ? C53 C54 1.390(3) . ? C53 C58 1.391(3) . ? C54 C55 1.387(3) . ? C55 C56 1.373(3) . ? C56 C57 1.381(3) . ? C57 C58 1.388(3) . ? C59 C64 1.388(3) . ? C59 C60 1.393(3) . ? C60 C61 1.378(3) . ? C61 C62 1.380(3) . ? C62 C63 1.377(3) . ? C63 C64 1.384(3) . ? C65 C66 1.389(3) . ? C65 C70 1.389(3) . ? C66 C67 1.388(3) . ? C67 C68 1.380(4) . ? C68 C69 1.375(4) . ? C69 C70 1.376(3) . ? 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 C1 Fe1 P1 95.04(7) . . ? C1 Fe1 P2 88.75(7) . . ? P1 Fe1 P2 86.53(2) . . ? C1 Fe1 S3 92.68(7) . . ? P1 Fe1 S3 100.56(2) . . ? P2 Fe1 S3 172.61(2) . . ? C1 Fe1 S1 154.35(7) . . ? P1 Fe1 S1 110.48(2) . . ? P2 Fe1 S1 95.06(2) . . ? S3 Fe1 S1 80.56(2) . . ? C1 Fe1 Fe2 99.94(7) . . ? P1 Fe1 Fe2 152.75(2) . . ? P2 Fe1 Fe2 116.25(2) . . ? S3 Fe1 Fe2 56.355(16) . . ? S1 Fe1 Fe2 55.760(17) . . ? C2 Fe2 C3 90.13(12) . . ? C2 Fe2 C4 103.82(11) . . ? C3 Fe2 C4 102.31(10) . . ? C2 Fe2 S1 153.19(8) . . ? C3 Fe2 S1 88.58(9) . . ? C4 Fe2 S1 102.62(7) . . ? C2 Fe2 S3 92.77(8) . . ? C3 Fe2 S3 159.24(8) . . ? C4 Fe2 S3 96.95(7) . . ? S1 Fe2 S3 79.64(2) . . ? C2 Fe2 Fe1 98.94(7) . . ? C3 Fe2 Fe1 104.44(8) . . ? C4 Fe2 Fe1 144.57(7) . . ? S1 Fe2 Fe1 55.695(16) . . ? S3 Fe2 Fe1 54.801(16) . . ? C5 Fe3 P3 87.39(7) . . ? C5 Fe3 P4 88.36(7) . . ? P3 Fe3 P4 87.95(2) . . ? C5 Fe3 S4 94.60(7) . . ? P3 Fe3 S4 105.68(2) . . ? P4 Fe3 S4 166.15(2) . . ? C5 Fe3 S2 159.45(7) . . ? P3 Fe3 S2 113.16(2) . . ? P4 Fe3 S2 91.93(2) . . ? S4 Fe3 S2 80.57(2) . . ? C5 Fe3 Fe4 104.85(7) . . ? P3 Fe3 Fe4 158.29(2) . . ? P4 Fe3 Fe4 109.892(19) . . ? S4 Fe3 Fe4 56.271(16) . . ? S2 Fe3 Fe4 55.896(16) . . ? C7 Fe4 C6 89.38(11) . . ? C7 Fe4 C8 104.48(10) . . ? C6 Fe4 C8 102.68(10) . . ? C7 Fe4 S2 150.62(7) . . ? C6 Fe4 S2 88.60(8) . . ? C8 Fe4 S2 104.55(7) . . ? C7 Fe4 S4 92.99(8) . . ? C6 Fe4 S4 160.88(7) . . ? C8 Fe4 S4 95.09(7) . . ? S2 Fe4 S4 80.07(2) . . ? C7 Fe4 Fe3 96.62(7) . . ? C6 Fe4 Fe3 105.56(7) . . ? C8 Fe4 Fe3 144.70(7) . . ? S2 Fe4 Fe3 55.969(16) . . ? S4 Fe4 Fe3 55.322(15) . . ? C9 S1 Fe1 116.55(7) . . ? C9 S1 Fe2 109.13(8) . . ? Fe1 S1 Fe2 68.545(18) . . ? C13 S2 Fe4 109.86(7) . . ? C13 S2 Fe3 118.37(7) . . ? Fe4 S2 Fe3 68.135(18) . . ? C14 S3 Fe1 114.45(7) . . ? C14 S3 Fe2 114.93(8) . . ? Fe1 S3 Fe2 68.844(18) . . ? C18 S4 Fe3 115.55(7) . . ? C18 S4 Fe4 113.04(8) . . ? Fe3 S4 Fe4 68.407(18) . . ? C27 P1 C21 103.39(10) . . ? C27 P1 C19 107.92(11) . . ? C21 P1 C19 100.53(11) . . ? C27 P1 Fe1 111.88(7) . . ? C21 P1 Fe1 122.02(8) . . ? C19 P1 Fe1 109.89(7) . . ? C39 P2 C33 101.29(10) . . ? C39 P2 C20 106.85(11) . . ? C33 P2 C20 100.75(10) . . ? C39 P2 Fe1 117.63(7) . . ? C33 P2 Fe1 122.38(8) . . ? C20 P2 Fe1 105.94(8) . . ? C47 P3 C53 100.28(10) . . ? C47 P3 C45 106.28(10) . . ? C53 P3 C45 101.74(9) . . ? C47 P3 Fe3 116.10(7) . . ? C53 P3 Fe3 125.16(7) . . ? C45 P3 Fe3 105.26(7) . . ? C65 P4 C59 101.56(10) . . ? C65 P4 C46 102.72(10) . . ? C59 P4 C46 104.27(10) . . ? C65 P4 Fe3 120.98(7) . . ? C59 P4 Fe3 118.31(7) . . ? C46 P4 Fe3 106.88(7) . . ? O1 C1 Fe1 177.65(19) . . ? O2 C2 Fe2 179.0(2) . . ? O3 C3 Fe2 178.9(3) . . ? O4 C4 Fe2 178.6(2) . . ? O5 C5 Fe3 177.41(19) . . ? O6 C6 Fe4 177.6(2) . . ? O7 C7 Fe4 178.3(2) . . ? O8 C8 Fe4 175.9(2) . . ? C10 C9 S1 110.23(15) . . ? C9 C10 C11 112.51(19) . . ? C10 C11 C12 115.06(18) . . ? C13 C12 C11 113.17(19) . . ? C12 C13 S2 109.79(15) . . ? C15 C14 S3 110.57(14) . . ? C14 C15 C16 114.66(19) . . ? C17 C16 C15 112.67(19) . . ? C16 C17 C18 114.37(19) . . ? C17 C18 S4 111.70(15) . . ? C20 C19 P1 111.88(15) . . ? C19 C20 P2 112.95(15) . . ? C22 C21 C26 118.4(2) . . ? C22 C21 P1 119.61(17) . . ? C26 C21 P1 121.80(19) . . ? C21 C22 C23 121.1(2) . . ? C24 C23 C22 120.1(3) . . ? C23 C24 C25 120.1(3) . . ? C24 C25 C26 120.6(3) . . ? C21 C26 C25 119.7(3) . . ? C32 C27 C28 118.3(2) . . ? C32 C27 P1 123.04(18) . . ? C28 C27 P1 118.12(17) . . ? C29 C28 C27 120.4(2) . . ? C30 C29 C28 120.5(3) . . ? C29 C30 C31 120.1(2) . . ? C30 C31 C32 119.8(3) . . ? C27 C32 C31 120.8(2) . . ? C38 C33 C34 119.2(2) . . ? C38 C33 P2 121.35(17) . . ? C34 C33 P2 119.47(18) . . ? C35 C34 C33 120.1(2) . . ? C36 C35 C34 120.2(2) . . ? C37 C36 C35 120.2(2) . . ? C36 C37 C38 119.9(2) . . ? C33 C38 C37 120.4(2) . . ? C40 C39 C44 118.6(2) . . ? C40 C39 P2 123.08(18) . . ? C44 C39 P2 117.94(17) . . ? C39 C40 C41 120.4(3) . . ? C42 C41 C40 120.4(3) . . ? C41 C42 C43 120.1(3) . . ? C44 C43 C42 119.6(3) . . ? C43 C44 C39 121.0(2) . . ? C46 C45 P3 106.72(14) . . ? C45 C46 P4 110.25(13) . . ? C52 C47 C48 118.8(2) . . ? C52 C47 P3 124.12(17) . . ? C48 C47 P3 117.05(17) . . ? C49 C48 C47 120.5(2) . . ? C50 C49 C48 120.2(2) . . ? C49 C50 C51 120.3(2) . . ? C50 C51 C52 120.0(2) . . ? C51 C52 C47 120.1(2) . . ? C54 C53 C58 118.74(19) . . ? C54 C53 P3 120.04(16) . . ? C58 C53 P3 121.22(16) . . ? C55 C54 C53 120.7(2) . . ? C56 C55 C54 120.0(2) . . ? C55 C56 C57 120.2(2) . . ? C56 C57 C58 120.0(2) . . ? C57 C58 C53 120.3(2) . . ? C64 C59 C60 118.32(19) . . ? C64 C59 P4 121.64(16) . . ? C60 C59 P4 120.00(16) . . ? C61 C60 C59 121.0(2) . . ? C60 C61 C62 119.8(2) . . ? C63 C62 C61 120.1(2) . . ? C62 C63 C64 120.0(2) . . ? C63 C64 C59 120.7(2) . . ? C66 C65 C70 118.2(2) . . ? C66 C65 P4 122.04(17) . . ? C70 C65 P4 119.58(17) . . ? C65 C66 C67 120.7(2) . . ? C68 C67 C66 120.1(3) . . ? C69 C68 C67 119.6(2) . . ? C70 C69 C68 120.4(3) . . ? C69 C70 C65 121.0(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.461 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.058 # Attachment '- complex_4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 793184' #TrackingRef '- complex_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H108 Cl8 F6 Fe4 N2 O14 P4 S4' _chemical_formula_weight 2314.90 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 17.133(3) _cell_length_b 13.281(2) _cell_length_c 23.904(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.252(8) _cell_angle_gamma 90.00 _cell_volume 5194.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20998 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20998 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.1521 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9021 _reflns_number_gt 4580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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. ; _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^)+(0.1661P)^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 9021 _refine_ls_number_parameters 599 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1806 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2928 _refine_ls_wR_factor_gt 0.2289 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Fe1 Fe 0.20871(7) 0.51475(9) 0.01112(5) 0.0330(4) Uani 1 1 d . . . Fe2 Fe 0.24160(7) 0.33867(9) 0.05938(5) 0.0291(4) Uani 1 1 d . . . S1 S 0.21023(13) 0.36803(16) -0.03874(9) 0.0320(5) Uani 1 1 d . . . S2 S -0.12348(13) 0.57846(15) -0.04759(9) 0.0304(5) Uani 1 1 d . . . P1 P 0.36836(14) 0.28843(17) 0.06783(10) 0.0339(6) Uani 1 1 d . . . P2 P 0.20773(14) 0.17851(17) 0.06036(10) 0.0323(6) Uani 1 1 d . . . C1 C 0.1311(6) 0.6044(7) -0.0262(4) 0.042(2) Uani 1 1 d . . . C2 C 0.2841(6) 0.5621(8) -0.0201(5) 0.047(3) Uani 1 1 d . . . C3 C 0.2574(6) 0.5751(6) 0.0779(4) 0.040(2) Uani 1 1 d . . . C4 C 0.2713(5) 0.3510(6) 0.1355(4) 0.031(2) Uani 1 1 d . . . C5 C 0.1055(5) 0.3308(6) -0.0785(3) 0.031(2) Uani 1 1 d . . . H5A H 0.1060 0.2621 -0.0944 0.038 Uiso 1 1 calc R . . H5B H 0.0723 0.3290 -0.0509 0.038 Uiso 1 1 calc R . . C6 C 0.0665(5) 0.4021(6) -0.1279(4) 0.034(2) Uani 1 1 d . . . H6A H 0.0864 0.3867 -0.1619 0.041 Uiso 1 1 calc R . . H6B H 0.0827 0.4720 -0.1154 0.041 Uiso 1 1 calc R . . C7 C -0.0581(5) 0.4303(6) -0.0984(3) 0.031(2) Uani 1 1 d . . . H7A H -0.0113 0.4451 -0.0635 0.038 Uiso 1 1 calc R . . H7B H -0.0908 0.3763 -0.0877 0.038 Uiso 1 1 calc R . . C8 C -0.1111(6) 0.5252(7) -0.1150(4) 0.038(2) Uani 1 1 d . . . H8A H -0.1652 0.5077 -0.1424 0.045 Uiso 1 1 calc R . . H8B H -0.0844 0.5746 -0.1343 0.045 Uiso 1 1 calc R . . C9 C -0.0584(6) 0.2899(6) -0.1704(4) 0.038(2) Uani 1 1 d . . . H9 H -0.0446 0.2413 -0.1369 0.046 Uiso 1 1 calc R . . C10 C -0.0192(6) 0.2532(7) -0.2142(4) 0.051(3) Uani 1 1 d . . . H10A H -0.0426 0.1879 -0.2296 0.076 Uiso 1 1 calc R . . H10B H 0.0397 0.2458 -0.1956 0.076 Uiso 1 1 calc R . . H10C H -0.0288 0.3017 -0.2465 0.076 Uiso 1 1 calc R . . C11 C -0.1504(6) 0.2932(7) -0.1951(4) 0.049(3) Uani 1 1 d . . . H11A H -0.1660 0.3448 -0.2257 0.073 Uiso 1 1 calc R . . H11B H -0.1744 0.3095 -0.1637 0.073 Uiso 1 1 calc R . . H11C H -0.1706 0.2275 -0.2118 0.073 Uiso 1 1 calc R . . C12 C 0.3727(5) 0.1548(6) 0.0884(4) 0.038(2) Uani 1 1 d . . . H12A H 0.4205 0.1222 0.0807 0.045 Uiso 1 1 calc R . . H12B H 0.3782 0.1481 0.1306 0.045 Uiso 1 1 calc R . . C13 C 0.2939(5) 0.1050(7) 0.0519(4) 0.038(2) Uani 1 1 d . . . H13A H 0.2910 0.0350 0.0654 0.045 Uiso 1 1 calc R . . H13B H 0.2923 0.1030 0.0102 0.045 Uiso 1 1 calc R . . C14 C 0.4086(5) 0.2916(7) 0.0058(4) 0.039(2) Uani 1 1 d . . . C15 C 0.4249(6) 0.2049(8) -0.0240(5) 0.056(3) Uani 1 1 d . . . H15 H 0.4123 0.1401 -0.0122 0.068 Uiso 1 1 calc R . . C16 C 0.4582(6) 0.2126(8) -0.0692(5) 0.055(3) Uani 1 1 d . . . H16 H 0.4686 0.1539 -0.0886 0.066 Uiso 1 1 calc R . . C17 C 0.4770(6) 0.3085(9) -0.0866(5) 0.060(3) Uani 1 1 d . . . H17 H 0.5019 0.3147 -0.1170 0.072 Uiso 1 1 calc R . . C18 C 0.4592(6) 0.3932(8) -0.0596(4) 0.049(3) Uani 1 1 d . . . H18 H 0.4701 0.4580 -0.0724 0.058 Uiso 1 1 calc R . . C19 C 0.4263(5) 0.3845(7) -0.0148(4) 0.043(2) Uani 1 1 d . . . H19 H 0.4148 0.4441 0.0033 0.052 Uiso 1 1 calc R . . C20 C 0.4541(5) 0.3432(7) 0.1243(4) 0.034(2) Uani 1 1 d . . . C21 C 0.4471(6) 0.4375(7) 0.1477(4) 0.041(2) Uani 1 1 d . . . H21 H 0.3966 0.4726 0.1347 0.050 Uiso 1 1 calc R . . C22 C 0.5121(6) 0.4814(8) 0.1897(5) 0.052(3) Uani 1 1 d . . . H22 H 0.5063 0.5446 0.2066 0.063 Uiso 1 1 calc R . . C23 C 0.5855(7) 0.4304(9) 0.2061(5) 0.063(3) Uani 1 1 d . . . H23 H 0.6314 0.4603 0.2337 0.075 Uiso 1 1 calc R . . C24 C 0.5938(7) 0.3393(10) 0.1840(5) 0.066(3) Uani 1 1 d . . . H24 H 0.6444 0.3046 0.1967 0.079 Uiso 1 1 calc R . . C25 C 0.5272(6) 0.2962(8) 0.1421(4) 0.053(3) Uani 1 1 d . . . H25 H 0.5336 0.2326 0.1258 0.064 Uiso 1 1 calc R . . C26 C 0.1918(5) 0.1310(6) 0.1282(4) 0.035(2) Uani 1 1 d . . . C27 C 0.2304(5) 0.0446(7) 0.1573(4) 0.040(2) Uani 1 1 d . . . H27 H 0.2688 0.0096 0.1429 0.048 Uiso 1 1 calc R . . C28 C 0.2129(6) 0.0100(7) 0.2063(4) 0.045(3) Uani 1 1 d . . . H28 H 0.2399 -0.0485 0.2255 0.053 Uiso 1 1 calc R . . C29 C 0.1581(6) 0.0572(7) 0.2279(4) 0.045(2) Uani 1 1 d . . . H29 H 0.1452 0.0305 0.2610 0.054 Uiso 1 1 calc R . . C30 C 0.1203(6) 0.1469(8) 0.2008(5) 0.050(3) Uani 1 1 d . . . H30 H 0.0828 0.1815 0.2163 0.060 Uiso 1 1 calc R . . C31 C 0.1374(5) 0.1834(7) 0.1530(4) 0.041(2) Uani 1 1 d . . . H31 H 0.1129 0.2445 0.1357 0.049 Uiso 1 1 calc R . . C32 C 0.1175(6) 0.1293(6) 0.0050(4) 0.038(2) Uani 1 1 d . . . C33 C 0.1237(7) 0.0633(6) -0.0403(4) 0.048(3) Uani 1 1 d . . . H33 H 0.1758 0.0410 -0.0416 0.057 Uiso 1 1 calc R . . C34 C 0.0543(8) 0.0319(7) -0.0822(5) 0.060(3) Uani 1 1 d . . . H34 H 0.0589 -0.0098 -0.1133 0.073 Uiso 1 1 calc R . . C35 C -0.0216(8) 0.0603(8) -0.0795(5) 0.060(3) Uani 1 1 d . . . H35 H -0.0691 0.0365 -0.1083 0.072 Uiso 1 1 calc R . . C36 C -0.0297(6) 0.1221(8) -0.0361(5) 0.055(3) Uani 1 1 d . . . H36 H -0.0825 0.1409 -0.0347 0.066 Uiso 1 1 calc R . . C37 C 0.0402(6) 0.1579(7) 0.0064(4) 0.044(2) Uani 1 1 d . . . H37 H 0.0346 0.2020 0.0363 0.052 Uiso 1 1 calc R . . N1 N -0.0263(4) 0.3933(5) -0.1462(3) 0.0307(17) Uani 1 1 d . . . H1 H -0.0456 0.4383 -0.1771 0.037 Uiso 1 1 calc R . . O1 O 0.0840(4) 0.6637(5) -0.0466(3) 0.0565(19) Uani 1 1 d . . . O2 O 0.3305(4) 0.5950(5) -0.0411(3) 0.060(2) Uani 1 1 d . . . O3 O 0.2897(4) 0.6170(5) 0.1217(3) 0.0503(18) Uani 1 1 d . . . O4 O 0.2888(4) 0.3581(4) 0.1859(3) 0.0398(15) Uani 1 1 d . . . C38 C 0.0494(6) 0.4152(9) 0.2449(5) 0.057(3) Uani 1 1 d . . . C39 C 0.0674(10) 0.3634(9) 0.3039(5) 0.078(4) Uani 1 1 d . . . O5 O 0.0157(5) 0.3658(6) 0.2014(3) 0.066(2) Uani 1 1 d . . . O6 O 0.0728(4) 0.5040(5) 0.2476(3) 0.058(2) Uani 1 1 d . . . F1 F 0.0627(7) 0.4192(6) 0.3468(4) 0.126(4) Uani 1 1 d . . . F2 F 0.0303(6) 0.2792(6) 0.3021(3) 0.115(3) Uani 1 1 d . . . F3 F 0.1501(6) 0.3338(6) 0.3208(4) 0.125(4) Uani 1 1 d . . . C40 C 0.6462(10) 0.1796(11) 0.0420(7) 0.101(5) Uani 1 1 d . . . H40A H 0.5990 0.2220 0.0211 0.121 Uiso 1 1 calc R . . H40B H 0.6745 0.2133 0.0794 0.121 Uiso 1 1 calc R . . Cl1 Cl 0.7133(4) 0.1708(3) -0.0006(3) 0.1405(19) Uani 1 1 d . . . Cl2 Cl 0.6103(3) 0.0619(3) 0.0569(2) 0.1251(16) Uani 1 1 d . . . C41 C 0.8709(10) 0.2242(10) 0.1645(9) 0.133(7) Uani 1 1 d . . . H41A H 0.8885 0.2283 0.1286 0.159 Uiso 1 1 calc R . . H41B H 0.9203 0.2332 0.1983 0.159 Uiso 1 1 calc R . . Cl3 Cl 0.8070(3) 0.3227(4) 0.1636(3) 0.1463(19) Uani 1 1 d . . . Cl4 Cl 0.8352(4) 0.1092(4) 0.1681(3) 0.186(3) Uani 1 1 d . . . O7 O 0.6988(7) 0.1798(12) 0.2935(5) 0.127(4) Uani 1 1 d . . . C42 C 0.6465(17) 0.0478(17) 0.2344(10) 0.176(10) Uani 1 1 d . . . H42A H 0.5953 0.0783 0.2366 0.264 Uiso 1 1 calc R . . H42B H 0.6447 -0.0251 0.2403 0.264 Uiso 1 1 calc R . . H42C H 0.6533 0.0614 0.1958 0.264 Uiso 1 1 calc R . . C43 C 0.7165(11) 0.0919(16) 0.2808(9) 0.114(6) Uani 1 1 d . . . H43A H 0.7295 0.0488 0.3161 0.137 Uiso 1 1 calc R . . H43B H 0.7653 0.0944 0.2667 0.137 Uiso 1 1 calc R . . C44 C 0.7683(10) 0.238(2) 0.3289(8) 0.157(10) Uani 1 1 d . . . H44A H 0.8071 0.2509 0.3062 0.188 Uiso 1 1 calc R . . H44B H 0.7972 0.1996 0.3645 0.188 Uiso 1 1 calc R . . C45 C 0.7382(9) 0.3334(12) 0.3452(7) 0.095(5) Uani 1 1 d . . . H45A H 0.6927 0.3578 0.3126 0.143 Uiso 1 1 calc R . . H45B H 0.7824 0.3832 0.3543 0.143 Uiso 1 1 calc R . . H45C H 0.7193 0.3231 0.3797 0.143 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 Fe1 0.0438(8) 0.0210(7) 0.0295(7) 0.0019(6) 0.0038(6) -0.0013(5) Fe2 0.0374(7) 0.0196(7) 0.0258(7) 0.0001(5) 0.0026(5) -0.0002(5) S1 0.0383(12) 0.0266(12) 0.0276(12) 0.0019(10) 0.0043(10) 0.0020(9) S2 0.0392(12) 0.0212(11) 0.0270(12) 0.0013(10) 0.0041(10) 0.0005(9) P1 0.0367(13) 0.0281(13) 0.0330(13) 0.0000(11) 0.0043(11) 0.0014(10) P2 0.0384(13) 0.0229(12) 0.0299(13) 0.0010(10) 0.0014(10) 0.0006(10) C1 0.061(6) 0.022(5) 0.041(6) 0.001(5) 0.014(5) 0.000(5) C2 0.052(6) 0.036(6) 0.053(7) -0.011(5) 0.015(5) 0.005(5) C3 0.058(6) 0.017(5) 0.044(6) 0.008(5) 0.014(5) 0.004(4) C4 0.033(5) 0.011(4) 0.045(6) 0.009(4) 0.005(4) 0.006(3) C5 0.043(5) 0.023(5) 0.021(4) 0.002(4) -0.001(4) 0.004(4) C6 0.045(5) 0.024(5) 0.027(5) 0.006(4) 0.001(4) -0.001(4) C7 0.047(5) 0.020(5) 0.024(4) 0.001(4) 0.005(4) 0.007(4) C8 0.048(5) 0.031(5) 0.032(5) -0.003(4) 0.008(4) 0.011(4) C9 0.058(6) 0.020(5) 0.030(5) -0.006(4) 0.002(5) -0.002(4) C10 0.059(6) 0.038(6) 0.044(6) -0.011(5) -0.003(5) 0.002(5) C11 0.047(6) 0.038(6) 0.051(6) -0.017(5) -0.002(5) -0.006(5) C12 0.045(5) 0.031(5) 0.034(5) 0.009(4) 0.007(4) 0.012(4) C13 0.045(5) 0.031(5) 0.038(5) 0.014(4) 0.012(4) 0.005(4) C14 0.044(5) 0.031(5) 0.038(5) -0.006(5) 0.003(4) 0.000(4) C15 0.066(7) 0.038(6) 0.072(8) -0.020(6) 0.030(6) 0.003(5) C16 0.064(7) 0.046(7) 0.062(7) -0.011(6) 0.027(6) -0.005(5) C17 0.062(7) 0.079(9) 0.040(6) -0.009(6) 0.017(5) -0.006(6) C18 0.063(7) 0.047(7) 0.040(6) -0.003(5) 0.023(5) -0.008(5) C19 0.049(6) 0.036(6) 0.043(6) -0.006(5) 0.011(5) 0.007(4) C20 0.033(5) 0.033(5) 0.034(5) -0.001(4) 0.006(4) -0.004(4) C21 0.049(6) 0.031(5) 0.041(6) 0.006(5) 0.009(5) -0.002(4) C22 0.057(7) 0.039(6) 0.054(7) -0.002(5) 0.007(6) -0.018(5) C23 0.059(7) 0.065(8) 0.053(7) 0.003(7) -0.001(6) -0.030(6) C24 0.045(7) 0.084(9) 0.053(7) 0.013(7) -0.010(5) 0.001(6) C25 0.057(7) 0.041(6) 0.053(7) -0.006(5) 0.002(6) -0.004(5) C26 0.047(5) 0.025(5) 0.026(5) 0.004(4) -0.001(4) -0.013(4) C27 0.043(5) 0.027(5) 0.047(6) 0.005(5) 0.009(5) -0.002(4) C28 0.059(6) 0.030(5) 0.036(6) 0.013(5) 0.001(5) -0.005(5) C29 0.060(6) 0.037(6) 0.036(5) 0.008(5) 0.010(5) -0.013(5) C30 0.052(6) 0.051(7) 0.050(6) -0.005(6) 0.020(5) -0.010(5) C31 0.051(6) 0.029(5) 0.041(6) -0.001(5) 0.012(5) -0.007(4) C32 0.059(6) 0.020(5) 0.027(5) 0.011(4) 0.002(4) -0.008(4) C33 0.071(7) 0.024(5) 0.039(6) 0.001(5) 0.002(5) -0.005(5) C34 0.090(9) 0.031(6) 0.044(6) -0.012(5) -0.006(6) -0.008(6) C35 0.077(9) 0.034(6) 0.049(7) 0.014(6) -0.014(6) -0.024(6) C36 0.039(6) 0.047(6) 0.065(7) 0.014(6) -0.008(5) -0.009(5) C37 0.044(6) 0.033(5) 0.045(6) 0.009(5) -0.001(5) -0.010(4) N1 0.044(4) 0.019(4) 0.025(4) -0.001(3) 0.004(3) 0.007(3) O1 0.074(5) 0.031(4) 0.055(5) 0.014(4) 0.006(4) 0.012(4) O2 0.066(5) 0.044(5) 0.079(6) 0.010(4) 0.036(4) -0.004(4) O3 0.055(4) 0.043(4) 0.041(4) -0.007(4) -0.003(3) -0.004(3) O4 0.052(4) 0.034(4) 0.028(4) -0.006(3) 0.003(3) 0.006(3) C38 0.046(6) 0.044(7) 0.069(8) 0.006(6) -0.002(6) -0.003(5) C39 0.140(13) 0.044(7) 0.039(7) 0.006(6) 0.007(8) -0.033(8) O5 0.091(6) 0.057(5) 0.046(4) -0.003(4) 0.012(4) -0.018(4) O6 0.076(5) 0.051(5) 0.036(4) 0.014(4) -0.001(4) -0.002(4) F1 0.245(12) 0.080(6) 0.063(5) 0.002(5) 0.062(6) -0.037(7) F2 0.189(9) 0.077(5) 0.070(5) 0.023(4) 0.022(5) -0.064(6) F3 0.137(8) 0.093(6) 0.104(7) 0.043(5) -0.027(6) 0.004(6) C40 0.117(12) 0.078(10) 0.106(12) -0.009(9) 0.032(10) -0.028(9) Cl1 0.192(5) 0.067(3) 0.177(5) -0.023(3) 0.076(4) -0.009(3) Cl2 0.150(4) 0.049(2) 0.169(4) 0.000(3) 0.035(3) -0.006(2) C41 0.111(12) 0.061(10) 0.19(2) 0.010(11) -0.006(12) 0.005(9) Cl3 0.131(4) 0.125(4) 0.167(5) -0.011(4) 0.020(4) 0.023(3) Cl4 0.239(7) 0.109(4) 0.234(7) 0.050(4) 0.108(6) -0.007(4) O7 0.108(9) 0.175(13) 0.101(9) 0.028(9) 0.033(7) 0.033(9) C42 0.27(3) 0.15(2) 0.15(2) 0.023(17) 0.12(2) 0.07(2) C43 0.102(13) 0.132(17) 0.129(16) -0.006(14) 0.068(12) 0.046(12) C44 0.066(11) 0.29(3) 0.092(13) 0.042(17) -0.006(10) -0.051(16) C45 0.084(11) 0.111(13) 0.080(10) 0.036(10) 0.006(8) 0.023(9) _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 C3 1.759(10) . ? Fe1 C2 1.787(12) . ? Fe1 C1 1.811(10) . ? Fe1 S2 2.276(3) 3_565 ? Fe1 S1 2.288(3) . ? Fe1 Fe2 2.5946(17) . ? Fe2 C4 1.745(10) . ? Fe2 P2 2.207(3) . ? Fe2 P1 2.223(3) . ? Fe2 S2 2.247(2) 3_565 ? Fe2 S1 2.279(2) . ? S1 C5 1.832(8) . ? S2 C8 1.829(9) . ? S2 Fe2 2.247(2) 3_565 ? S2 Fe1 2.276(3) 3_565 ? P1 C14 1.812(10) . ? P1 C20 1.825(9) . ? P1 C12 1.837(9) . ? P2 C32 1.831(9) . ? P2 C13 1.831(9) . ? P2 C26 1.835(9) . ? C1 O1 1.129(10) . ? C2 O2 1.145(11) . ? C3 O3 1.170(10) . ? C4 O4 1.155(10) . ? C5 C6 1.508(11) . ? C6 N1 1.524(10) . ? C7 N1 1.488(10) . ? C7 C8 1.535(11) . ? C9 C10 1.485(13) . ? C9 C11 1.511(13) . ? C9 N1 1.528(10) . ? C12 C13 1.524(12) . ? C14 C19 1.395(13) . ? C14 C15 1.424(13) . ? C15 C16 1.367(14) . ? C16 C17 1.407(15) . ? C17 C18 1.375(14) . ? C18 C19 1.356(13) . ? C20 C25 1.351(13) . ? C20 C21 1.391(12) . ? C21 C22 1.388(13) . ? C22 C23 1.379(15) . ? C23 C24 1.344(15) . ? C24 C25 1.398(14) . ? C26 C27 1.402(12) . ? C26 C31 1.425(13) . ? C27 C28 1.372(13) . ? C28 C29 1.351(14) . ? C29 C30 1.419(14) . ? C30 C31 1.351(13) . ? C32 C37 1.388(13) . ? C32 C33 1.421(13) . ? C33 C34 1.372(13) . ? C34 C35 1.374(16) . ? C35 C36 1.360(15) . ? C36 C37 1.405(13) . ? C38 O5 1.220(12) . ? C38 O6 1.241(12) . ? C38 C39 1.516(15) . ? C39 F2 1.280(13) . ? C39 F1 1.287(14) . ? C39 F3 1.410(17) . ? C40 Cl1 1.751(16) . ? C40 Cl2 1.755(14) . ? C41 Cl4 1.657(15) . ? C41 Cl3 1.702(16) . ? O7 C43 1.266(19) . ? O7 C44 1.46(2) . ? C42 C43 1.49(3) . ? C44 C45 1.47(2) . ? 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 C3 Fe1 C2 90.6(4) . . ? C3 Fe1 C1 103.2(4) . . ? C2 Fe1 C1 94.5(4) . . ? C3 Fe1 S2 94.9(3) . 3_565 ? C2 Fe1 S2 167.6(3) . 3_565 ? C1 Fe1 S2 94.9(3) . 3_565 ? C3 Fe1 S1 141.7(3) . . ? C2 Fe1 S1 87.8(3) . . ? C1 Fe1 S1 115.1(3) . . ? S2 Fe1 S1 81.03(9) 3_565 . ? C3 Fe1 Fe2 91.5(3) . . ? C2 Fe1 Fe2 114.5(3) . . ? C1 Fe1 Fe2 147.5(3) . . ? S2 Fe1 Fe2 54.47(6) 3_565 . ? S1 Fe1 Fe2 55.22(7) . . ? C4 Fe2 P2 94.4(3) . . ? C4 Fe2 P1 87.6(3) . . ? P2 Fe2 P1 87.86(9) . . ? C4 Fe2 S2 93.3(3) . 3_565 ? P2 Fe2 S2 104.10(9) . 3_565 ? P1 Fe2 S2 167.88(10) . 3_565 ? C4 Fe2 S1 164.5(3) . . ? P2 Fe2 S1 101.15(9) . . ? P1 Fe2 S1 94.05(9) . . ? S2 Fe2 S1 81.86(9) 3_565 . ? C4 Fe2 Fe1 109.7(3) . . ? P2 Fe2 Fe1 148.25(8) . . ? P1 Fe2 Fe1 112.86(8) . . ? S2 Fe2 Fe1 55.52(7) 3_565 . ? S1 Fe2 Fe1 55.55(7) . . ? C5 S1 Fe2 112.5(3) . . ? C5 S1 Fe1 109.8(3) . . ? Fe2 S1 Fe1 69.23(7) . . ? C8 S2 Fe2 114.5(3) . 3_565 ? C8 S2 Fe1 112.5(3) . 3_565 ? Fe2 S2 Fe1 70.01(8) 3_565 3_565 ? C14 P1 C20 100.3(4) . . ? C14 P1 C12 104.2(4) . . ? C20 P1 C12 103.1(4) . . ? C14 P1 Fe2 121.1(3) . . ? C20 P1 Fe2 119.8(3) . . ? C12 P1 Fe2 106.0(3) . . ? C32 P2 C13 105.4(4) . . ? C32 P2 C26 101.6(4) . . ? C13 P2 C26 104.5(4) . . ? C32 P2 Fe2 120.3(3) . . ? C13 P2 Fe2 106.8(3) . . ? C26 P2 Fe2 116.7(3) . . ? O1 C1 Fe1 176.0(9) . . ? O2 C2 Fe1 177.5(9) . . ? O3 C3 Fe1 178.7(8) . . ? O4 C4 Fe2 177.9(8) . . ? C6 C5 S1 112.0(6) . . ? C5 C6 N1 111.0(7) . . ? N1 C7 C8 113.3(7) . . ? C7 C8 S2 107.7(6) . . ? C10 C9 C11 111.8(8) . . ? C10 C9 N1 112.0(8) . . ? C11 C9 N1 109.7(7) . . ? C13 C12 P1 107.9(6) . . ? C12 C13 P2 108.2(6) . . ? C19 C14 C15 116.3(9) . . ? C19 C14 P1 119.0(7) . . ? C15 C14 P1 124.7(8) . . ? C16 C15 C14 121.6(11) . . ? C15 C16 C17 119.2(10) . . ? C18 C17 C16 120.0(10) . . ? C19 C18 C17 120.2(10) . . ? C18 C19 C14 122.6(9) . . ? C25 C20 C21 118.2(8) . . ? C25 C20 P1 121.1(7) . . ? C21 C20 P1 120.7(7) . . ? C22 C21 C20 121.5(9) . . ? C23 C22 C21 117.9(10) . . ? C24 C23 C22 121.6(10) . . ? C23 C24 C25 119.5(11) . . ? C20 C25 C24 121.3(10) . . ? C27 C26 C31 117.6(8) . . ? C27 C26 P2 123.3(8) . . ? C31 C26 P2 119.1(7) . . ? C28 C27 C26 120.5(9) . . ? C29 C28 C27 121.6(9) . . ? C28 C29 C30 119.3(9) . . ? C31 C30 C29 120.2(10) . . ? C30 C31 C26 120.6(9) . . ? C37 C32 C33 118.3(9) . . ? C37 C32 P2 119.4(7) . . ? C33 C32 P2 122.2(8) . . ? C34 C33 C32 120.0(10) . . ? C33 C34 C35 120.6(11) . . ? C36 C35 C34 120.8(10) . . ? C35 C36 C37 119.9(10) . . ? C32 C37 C36 120.3(10) . . ? C7 N1 C6 110.1(6) . . ? C7 N1 C9 114.5(7) . . ? C6 N1 C9 113.9(6) . . ? O5 C38 O6 128.2(11) . . ? O5 C38 C39 117.6(10) . . ? O6 C38 C39 114.2(10) . . ? F2 C39 F1 112.5(12) . . ? F2 C39 F3 102.3(12) . . ? F1 C39 F3 103.1(11) . . ? F2 C39 C38 113.8(10) . . ? F1 C39 C38 115.8(11) . . ? F3 C39 C38 107.6(11) . . ? Cl1 C40 Cl2 112.8(9) . . ? Cl4 C41 Cl3 117.5(11) . . ? C43 O7 C44 114.5(17) . . ? O7 C43 C42 110.1(17) . . ? O7 C44 C45 108.7(16) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.305 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.172 # Attachment '- complex_5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 793185' #TrackingRef '- complex_5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87.50 H103 Cl3 F6 Fe4 N4 O15 P4 S6' _chemical_formula_weight 2210.73 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.4839(5) _cell_length_b 17.0452(5) _cell_length_c 21.2654(4) _cell_angle_alpha 94.2320(2) _cell_angle_beta 108.7318(14) _cell_angle_gamma 113.5410(11) _cell_volume 5045.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 63604 _cell_measurement_theta_min 1.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2282 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63604 _diffrn_reflns_av_R_equivalents 0.0917 _diffrn_reflns_av_sigmaI/netI 0.1205 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17651 _reflns_number_gt 9145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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. ; _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^)+(0.1921P)^2^+20.4325P] 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 17651 _refine_ls_number_parameters 1089 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.1789 _refine_ls_R_factor_gt 0.1006 _refine_ls_wR_factor_ref 0.3409 _refine_ls_wR_factor_gt 0.2871 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 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 0.32923(10) 0.70653(9) 0.35766(7) 0.0371(4) Uani 1 1 d . . . Fe2 Fe 0.29915(10) 0.76901(9) 0.25189(7) 0.0345(4) Uani 1 1 d . . . Fe3 Fe 0.13383(11) 0.30219(9) 0.15716(7) 0.0400(4) Uani 1 1 d . . . Fe4 Fe 0.14976(11) 0.22584(9) 0.25541(7) 0.0375(4) Uani 1 1 d . . . S1 S 0.19423(18) 0.72093(15) 0.30416(12) 0.0369(6) Uani 1 1 d . . . S2 S 0.04779(19) 0.28811(16) 0.22419(13) 0.0401(6) Uani 1 1 d . . . S3 S 0.28405(19) 0.63043(16) 0.24930(12) 0.0395(6) Uani 1 1 d . . . S4 S 0.25513(19) 0.36290(16) 0.26219(12) 0.0397(6) Uani 1 1 d . . . P1 P 0.3176(2) 0.90465(16) 0.28438(13) 0.0374(6) Uani 1 1 d . . . P2 P 0.2059(2) 0.76342(17) 0.14890(13) 0.0399(6) Uani 1 1 d . . . P3 P 0.2036(2) 0.21588(18) 0.36168(14) 0.0469(7) Uani 1 1 d . . . P4 P 0.0259(2) 0.09609(17) 0.23773(14) 0.0461(7) Uani 1 1 d . . . N1 N -0.0226(6) 0.4780(5) 0.2822(4) 0.043(2) Uani 1 1 d . . . N2 N 0.4854(6) 0.5347(5) 0.2823(4) 0.043(2) Uani 1 1 d . . . C1 C 0.3091(7) 0.6103(7) 0.3907(5) 0.041(2) Uani 1 1 d . . . C2 C 0.4551(10) 0.7639(7) 0.3719(5) 0.048(3) Uani 1 1 d . . . C3 C 0.3491(8) 0.7758(7) 0.4331(6) 0.044(3) Uani 1 1 d . . . C4 C 0.4050(9) 0.8076(7) 0.2340(5) 0.048(3) Uani 1 1 d . . . C5 C 0.1316(9) 0.3959(8) 0.1236(5) 0.050(3) Uani 1 1 d . . . C6 C 0.0291(9) 0.2162(8) 0.0935(6) 0.048(3) Uani 1 1 d . . . C7 C 0.2084(9) 0.2824(7) 0.1203(6) 0.056(3) Uani 1 1 d . . . C8 C 0.2112(8) 0.1745(7) 0.2331(5) 0.042(2) Uani 1 1 d . . . C9 C 0.0909(7) 0.6139(6) 0.2581(5) 0.039(2) Uani 1 1 d . . . H9A H 0.0363 0.6222 0.2284 0.047 Uiso 1 1 calc R . . H9B H 0.1076 0.5795 0.2293 0.047 Uiso 1 1 calc R . . C10 C 0.0643(7) 0.5655(6) 0.3114(5) 0.040(2) Uani 1 1 d . . . H10A H 0.1193 0.5566 0.3397 0.048 Uiso 1 1 calc R . . H10B H 0.0528 0.6032 0.3419 0.048 Uiso 1 1 calc R . . C11 C -0.0068(7) 0.4162(6) 0.2382(5) 0.040(2) Uani 1 1 d . . . H11A H 0.0023 0.4413 0.1991 0.048 Uiso 1 1 calc R . . H11B H -0.0660 0.3597 0.2196 0.048 Uiso 1 1 calc R . . C12 C 0.0783(7) 0.3964(6) 0.2731(5) 0.038(2) Uani 1 1 d . . . H12A H 0.0871 0.3950 0.3212 0.045 Uiso 1 1 calc R . . H12B H 0.1381 0.4419 0.2721 0.045 Uiso 1 1 calc R . . C13 C -0.1081(8) 0.4888(8) 0.2384(7) 0.059(3) Uani 1 1 d . . . H13A H -0.1111 0.5382 0.2625 0.089 Uiso 1 1 calc R . . H13B H -0.1668 0.4348 0.2291 0.089 Uiso 1 1 calc R . . H13C H -0.1021 0.5003 0.1953 0.089 Uiso 1 1 calc R . . C14 C -0.0414(10) 0.4432(7) 0.3439(6) 0.059(3) Uani 1 1 d . . . H14 H 0.0210 0.4529 0.3792 0.071 Uiso 1 1 calc R . . C15 C -0.0830(12) 0.4937(9) 0.3748(8) 0.083(4) Uani 1 1 d . . . H15A H -0.1415 0.4888 0.3396 0.125 Uiso 1 1 calc R . . H15B H -0.0361 0.5557 0.3926 0.125 Uiso 1 1 calc R . . H15C H -0.0982 0.4689 0.4120 0.125 Uiso 1 1 calc R . . C16 C -0.1108(10) 0.3424(8) 0.3223(8) 0.075(4) Uani 1 1 d . . . H16A H -0.1185 0.3213 0.3627 0.113 Uiso 1 1 calc R . . H16B H -0.0841 0.3106 0.3016 0.113 Uiso 1 1 calc R . . H16C H -0.1734 0.3320 0.2892 0.113 Uiso 1 1 calc R . . C17 C 0.3808(8) 0.6119(7) 0.2369(5) 0.044(3) Uani 1 1 d . . . H17A H 0.3554 0.5707 0.1923 0.053 Uiso 1 1 calc R . . H17B H 0.4315 0.6682 0.2369 0.053 Uiso 1 1 calc R . . C18 C 0.4221(8) 0.5740(7) 0.2935(5) 0.047(3) Uani 1 1 d . . . H18A H 0.3684 0.5278 0.3009 0.057 Uiso 1 1 calc R . . H18B H 0.4598 0.6211 0.3359 0.057 Uiso 1 1 calc R . . C19 C 0.4273(8) 0.4434(7) 0.2370(5) 0.048(3) Uani 1 1 d . . . H19A H 0.4717 0.4262 0.2243 0.058 Uiso 1 1 calc R . . H19B H 0.3822 0.4465 0.1944 0.058 Uiso 1 1 calc R . . C20 C 0.3695(7) 0.3694(7) 0.2638(5) 0.044(3) Uani 1 1 d . . . H20A H 0.4098 0.3755 0.3115 0.053 Uiso 1 1 calc R . . H20B H 0.3565 0.3128 0.2368 0.053 Uiso 1 1 calc R . . C21 C 0.5473(10) 0.5910(9) 0.2459(7) 0.073(4) Uani 1 1 d . . . H21A H 0.5886 0.5655 0.2392 0.109 Uiso 1 1 calc R . . H21B H 0.5871 0.6512 0.2740 0.109 Uiso 1 1 calc R . . H21C H 0.5055 0.5919 0.2015 0.109 Uiso 1 1 calc R . . C22 C 0.5518(9) 0.5355(7) 0.3528(5) 0.053(3) Uani 1 1 d . . . H22 H 0.5119 0.5088 0.3795 0.064 Uiso 1 1 calc R . . C23 C 0.6237(11) 0.6286(10) 0.3915(8) 0.091(5) Uani 1 1 d . . . H23A H 0.6627 0.6282 0.4372 0.137 Uiso 1 1 calc R . . H23B H 0.5899 0.6635 0.3955 0.137 Uiso 1 1 calc R . . H23C H 0.6653 0.6546 0.3669 0.137 Uiso 1 1 calc R . . C24 C 0.6066(10) 0.4840(10) 0.3473(7) 0.077(4) Uani 1 1 d . . . H24A H 0.5614 0.4220 0.3263 0.116 Uiso 1 1 calc R . . H24B H 0.6505 0.4892 0.3930 0.116 Uiso 1 1 calc R . . H24C H 0.6432 0.5075 0.3191 0.116 Uiso 1 1 calc R . . C25 C 0.2159(8) 0.9117(7) 0.2195(5) 0.046(3) Uani 1 1 d . . . H25A H 0.1565 0.8798 0.2274 0.055 Uiso 1 1 calc R . . H25B H 0.2284 0.9740 0.2226 0.055 Uiso 1 1 calc R . . C26 C 0.2042(8) 0.8709(7) 0.1488(5) 0.047(3) Uani 1 1 d . . . H26A H 0.2569 0.9105 0.1365 0.057 Uiso 1 1 calc R . . H26B H 0.1428 0.8631 0.1143 0.057 Uiso 1 1 calc R . . C27 C 0.3134(8) 0.9441(6) 0.3656(5) 0.039(2) Uani 1 1 d . . . C28 C 0.3949(8) 0.9998(7) 0.4215(5) 0.050(3) Uani 1 1 d . . . H28 H 0.4556 1.0188 0.4179 0.060 Uiso 1 1 calc R . . C29 C 0.3911(9) 1.0289(7) 0.4823(6) 0.057(3) Uani 1 1 d . . . H29 H 0.4484 1.0673 0.5198 0.069 Uiso 1 1 calc R . . C30 C 0.3046(10) 1.0023(8) 0.4885(6) 0.056(3) Uani 1 1 d . . . H30 H 0.3017 1.0230 0.5301 0.067 Uiso 1 1 calc R . . C31 C 0.2203(9) 0.9446(7) 0.4337(6) 0.052(3) Uani 1 1 d . . . H31 H 0.1604 0.9237 0.4385 0.062 Uiso 1 1 calc R . . C32 C 0.2248(8) 0.9181(6) 0.3723(5) 0.043(2) Uani 1 1 d . . . H32 H 0.1673 0.8819 0.3342 0.051 Uiso 1 1 calc R . . C33 C 0.4260(8) 0.9964(6) 0.2861(5) 0.040(2) Uani 1 1 d . . . C34 C 0.4263(9) 1.0672(7) 0.2588(6) 0.053(3) Uani 1 1 d . . . H34 H 0.3667 1.0673 0.2352 0.064 Uiso 1 1 calc R . . C35 C 0.5072(11) 1.1361(8) 0.2641(7) 0.068(4) Uani 1 1 d . . . H35 H 0.5043 1.1826 0.2429 0.081 Uiso 1 1 calc R . . C36 C 0.5953(10) 1.1388(9) 0.3007(7) 0.072(4) Uani 1 1 d . . . H36 H 0.6532 1.1880 0.3062 0.087 Uiso 1 1 calc R . . C37 C 0.5977(10) 1.0686(8) 0.3292(7) 0.065(3) Uani 1 1 d . . . H37 H 0.6574 1.0696 0.3542 0.078 Uiso 1 1 calc R . . C38 C 0.5154(8) 0.9992(7) 0.3216(6) 0.051(3) Uani 1 1 d . . . H38 H 0.5180 0.9512 0.3406 0.061 Uiso 1 1 calc R . . C39 C 0.2337(8) 0.7419(7) 0.0741(5) 0.044(3) Uani 1 1 d . . . C40 C 0.1946(11) 0.7668(9) 0.0158(6) 0.067(4) Uani 1 1 d . . . H40 H 0.1564 0.7964 0.0151 0.080 Uiso 1 1 calc R . . C41 C 0.2120(12) 0.7479(10) -0.0413(6) 0.080(4) Uani 1 1 d . . . H41 H 0.1858 0.7656 -0.0812 0.096 Uiso 1 1 calc R . . C42 C 0.2648(11) 0.7056(9) -0.0422(7) 0.075(4) Uani 1 1 d . . . H42 H 0.2756 0.6935 -0.0823 0.090 Uiso 1 1 calc R . . C43 C 0.3031(10) 0.6799(8) 0.0146(6) 0.065(3) Uani 1 1 d . . . H43 H 0.3419 0.6510 0.0147 0.078 Uiso 1 1 calc R . . C44 C 0.2848(8) 0.6963(8) 0.0730(6) 0.054(3) Uani 1 1 d . . . H44 H 0.3082 0.6755 0.1118 0.065 Uiso 1 1 calc R . . C45 C 0.0812(7) 0.6845(7) 0.1174(5) 0.040(2) Uani 1 1 d . . . C46 C 0.0545(9) 0.5983(7) 0.0879(5) 0.048(3) Uani 1 1 d . . . H46 H 0.1016 0.5830 0.0822 0.057 Uiso 1 1 calc R . . C47 C -0.0386(9) 0.5341(8) 0.0667(5) 0.057(3) Uani 1 1 d . . . H47 H -0.0550 0.4751 0.0475 0.069 Uiso 1 1 calc R . . C48 C -0.1095(9) 0.5564(8) 0.0737(6) 0.060(3) Uani 1 1 d . . . H48 H -0.1742 0.5132 0.0591 0.072 Uiso 1 1 calc R . . C49 C -0.0823(9) 0.6415(9) 0.1020(7) 0.068(4) Uani 1 1 d . . . H49 H -0.1297 0.6576 0.1058 0.082 Uiso 1 1 calc R . . C50 C 0.0113(8) 0.7052(8) 0.1253(5) 0.051(3) Uani 1 1 d . . . H50 H 0.0280 0.7634 0.1468 0.061 Uiso 1 1 calc R . . C51 C 0.1564(11) 0.0981(8) 0.3593(6) 0.067(4) Uani 1 1 d . . . H51A H 0.1898 0.0724 0.3397 0.081 Uiso 1 1 calc R . . H51B H 0.1670 0.0888 0.4061 0.081 Uiso 1 1 calc R . . C52 C 0.0482(10) 0.0533(8) 0.3148(6) 0.067(4) Uani 1 1 d . . . H52A H 0.0127 0.0648 0.3412 0.080 Uiso 1 1 calc R . . H52B H 0.0250 -0.0111 0.3019 0.080 Uiso 1 1 calc R . . C53 C 0.3325(9) 0.2572(7) 0.4016(5) 0.052(3) Uani 1 1 d . . . C54 C 0.3763(10) 0.2057(9) 0.3875(6) 0.072(4) Uani 1 1 d . . . H54 H 0.3379 0.1464 0.3621 0.086 Uiso 1 1 calc R . . C55 C 0.4747(11) 0.2411(11) 0.4102(7) 0.079(4) Uani 1 1 d . . . H55 H 0.5030 0.2056 0.4001 0.095 Uiso 1 1 calc R . . C56 C 0.5328(11) 0.3266(11) 0.4474(6) 0.079(4) Uani 1 1 d . . . H56 H 0.6005 0.3505 0.4621 0.095 Uiso 1 1 calc R . . C57 C 0.4905(9) 0.3775(9) 0.4629(6) 0.065(3) Uani 1 1 d . . . H57 H 0.5297 0.4360 0.4898 0.077 Uiso 1 1 calc R . . C58 C 0.3927(9) 0.3439(8) 0.4397(6) 0.058(3) Uani 1 1 d . . . H58 H 0.3651 0.3803 0.4498 0.070 Uiso 1 1 calc R . . C59 C 0.1720(9) 0.2630(7) 0.4246(5) 0.049(3) Uani 1 1 d . . . C60 C 0.1336(10) 0.2158(8) 0.4678(6) 0.064(3) Uani 1 1 d . . . H60 H 0.1230 0.1564 0.4651 0.076 Uiso 1 1 calc R . . C61 C 0.1111(10) 0.2553(10) 0.5142(6) 0.075(4) Uani 1 1 d . . . H61 H 0.0859 0.2235 0.5439 0.090 Uiso 1 1 calc R . . C62 C 0.1258(10) 0.3420(9) 0.5173(7) 0.070(4) Uani 1 1 d . . . H62 H 0.1105 0.3697 0.5492 0.084 Uiso 1 1 calc R . . C63 C 0.1615(10) 0.3867(9) 0.4750(6) 0.062(3) Uani 1 1 d . . . H63 H 0.1713 0.4458 0.4770 0.074 Uiso 1 1 calc R . . C64 C 0.1835(8) 0.3475(7) 0.4299(5) 0.050(3) Uani 1 1 d . . . H64 H 0.2081 0.3802 0.4004 0.060 Uiso 1 1 calc R . . C65 C -0.0901(9) 0.0954(7) 0.2225(7) 0.058(3) Uani 1 1 d . . . C66 C -0.1107(10) 0.1247(8) 0.2761(7) 0.073(4) Uani 1 1 d . . . H66 H -0.0654 0.1432 0.3219 0.088 Uiso 1 1 calc R . . C67 C -0.1981(14) 0.1261(11) 0.2613(12) 0.100(6) Uani 1 1 d . . . H67 H -0.2120 0.1442 0.2983 0.120 Uiso 1 1 calc R . . C68 C -0.2628(15) 0.1042(12) 0.1997(13) 0.115(7) Uani 1 1 d . . . H68 H -0.3212 0.1079 0.1916 0.138 Uiso 1 1 calc R . . C69 C -0.2426(11) 0.0754(11) 0.1467(10) 0.096(5) Uani 1 1 d . . . H69 H -0.2886 0.0593 0.1014 0.115 Uiso 1 1 calc R . . C70 C -0.1600(10) 0.0690(8) 0.1562(8) 0.072(4) Uani 1 1 d . . . H70 H -0.1498 0.0471 0.1185 0.086 Uiso 1 1 calc R . . C71 C -0.0083(9) 0.0030(7) 0.1705(5) 0.050(3) Uani 1 1 d . . . C72 C 0.0300(8) 0.0130(7) 0.1191(5) 0.051(3) Uani 1 1 d . . . H72 H 0.0751 0.0696 0.1196 0.061 Uiso 1 1 calc R . . C73 C 0.0026(9) -0.0586(8) 0.0680(6) 0.060(3) Uani 1 1 d . . . H73 H 0.0299 -0.0518 0.0344 0.072 Uiso 1 1 calc R . . C74 C -0.0652(10) -0.1404(8) 0.0668(6) 0.066(4) Uani 1 1 d . . . H74 H -0.0855 -0.1901 0.0319 0.079 Uiso 1 1 calc R . . C75 C -0.1022(10) -0.1491(8) 0.1150(7) 0.069(4) Uani 1 1 d . . . H75 H -0.1493 -0.2054 0.1130 0.083 Uiso 1 1 calc R . . C76 C -0.0747(10) -0.0799(8) 0.1670(6) 0.063(3) Uani 1 1 d . . . H76 H -0.1015 -0.0892 0.2008 0.076 Uiso 1 1 calc R . . O1 O 0.2975(6) 0.5470(5) 0.4094(4) 0.065(2) Uani 1 1 d . . . O2 O 0.5332(6) 0.7985(6) 0.3824(4) 0.064(2) Uani 1 1 d . . . O3 O 0.3627(6) 0.8185(5) 0.4836(4) 0.060(2) Uani 1 1 d . . . O4 O 0.4716(6) 0.8306(6) 0.2214(4) 0.063(2) Uani 1 1 d . . . O5 O 0.1266(9) 0.4508(6) 0.0990(5) 0.091(3) Uani 1 1 d . . . O6 O -0.0391(6) 0.1579(6) 0.0534(4) 0.066(2) Uani 1 1 d . . . O7 O 0.2556(7) 0.2687(6) 0.0956(4) 0.072(3) Uani 1 1 d . . . O8 O 0.2553(6) 0.1421(5) 0.2176(4) 0.058(2) Uani 1 1 d . . . S5 S 0.9559(2) 0.7661(2) 0.31288(16) 0.0590(8) Uani 1 1 d D . . O9 O 0.9740(8) 0.7004(6) 0.3435(5) 0.092(3) Uani 1 1 d D . . O10 O 0.9704(7) 0.8381(6) 0.3594(5) 0.088(3) Uani 1 1 d D . . O11 O 0.9928(7) 0.7856(8) 0.2620(5) 0.105(4) Uani 1 1 d D . . C77 C 0.8315(9) 0.7130(8) 0.2667(7) 0.074(4) Uani 1 1 d D . . F1 F 0.8047(7) 0.6462(7) 0.2169(5) 0.122(4) Uani 1 1 d D . . F2 F 0.7833(7) 0.6859(7) 0.3066(5) 0.123(4) Uani 1 1 d D . . F3 F 0.7996(7) 0.7668(7) 0.2355(6) 0.128(4) Uani 1 1 d D . . S6 S 0.6142(5) 0.3578(4) 0.1922(3) 0.140(2) Uiso 1 1 d D . . O12 O 0.5193(7) 0.3144(8) 0.1913(7) 0.135(5) Uiso 1 1 d D . . O13 O 0.6475(11) 0.2968(9) 0.1791(8) 0.169(6) Uiso 1 1 d D . . O14 O 0.6771(10) 0.4237(9) 0.2528(6) 0.200 Uiso 1 1 d D . . C78 C 0.6176(10) 0.4320(8) 0.1416(6) 0.091(5) Uiso 1 1 d D . . F4 F 0.6795(8) 0.4400(8) 0.1117(6) 0.143(4) Uiso 1 1 d D . . F5 F 0.5387(10) 0.4400(13) 0.1092(8) 0.244(8) Uiso 1 1 d D . . F6 F 0.6577(10) 0.5005(7) 0.1974(7) 0.200 Uiso 1 1 d D . . O15 O 0.6399(14) 0.9882(12) -0.0716(9) 0.167(6) Uiso 1 1 d . . . C79 C 0.529(3) 1.040(2) -0.0983(18) 0.235(15) Uiso 1 1 d . . . H79A H 0.5060 1.0302 -0.1481 0.353 Uiso 1 1 calc R . . H79B H 0.5883 1.0944 -0.0774 0.353 Uiso 1 1 calc R . . H79C H 0.4800 1.0441 -0.0831 0.353 Uiso 1 1 calc R . . C80 C 0.5444(19) 0.9718(18) -0.0793(13) 0.157(9) Uiso 1 1 d . . . H80A H 0.4975 0.9167 -0.1143 0.189 Uiso 1 1 calc R . . H80B H 0.5363 0.9648 -0.0356 0.189 Uiso 1 1 calc R . . C81 C 0.6581(19) 0.910(2) -0.0585(19) 0.234(15) Uiso 1 1 d D . . H81A H 0.6471 0.8930 -0.0175 0.281 Uiso 1 1 calc R . . H81B H 0.6177 0.8594 -0.0982 0.281 Uiso 1 1 calc R . . C82 C 0.7589(14) 0.9454(13) -0.0480(9) 0.112(6) Uiso 1 1 d D . . H82A H 0.7933 1.0062 -0.0209 0.168 Uiso 1 1 calc R . . H82B H 0.7652 0.9440 -0.0923 0.168 Uiso 1 1 calc R . . H82C H 0.7862 0.9095 -0.0236 0.168 Uiso 1 1 calc R . . C83 C 0.1633(14) 0.0662(16) 0.6314(12) 0.183(11) Uiso 1 1 d D . . H83A H 0.1422 0.1122 0.6206 0.219 Uiso 1 1 calc R . . H83B H 0.1441 0.0448 0.6688 0.219 Uiso 1 1 calc R . . Cl1 Cl 0.2828(9) 0.1118(8) 0.6590(6) 0.264(5) Uiso 1 1 d D . . Cl2 Cl 0.1051(7) -0.0186(7) 0.5615(5) 0.220(4) Uiso 1 1 d D . . C84 C 0.588(3) 0.8007(17) 0.133(2) 0.146(16) Uiso 0.50 1 d PD . . H84A H 0.5339 0.8157 0.1157 0.176 Uiso 0.50 1 calc PR . . H84B H 0.6171 0.8219 0.1833 0.176 Uiso 0.50 1 calc PR . . Cl3 Cl 0.5452(13) 0.6910(12) 0.1134(9) 0.202(6) Uiso 0.50 1 d PD . . Cl4 Cl 0.669(2) 0.8532(18) 0.101(2) 0.396(19) Uiso 0.50 1 d PD . . N3 N 0.8292(17) 0.3824(13) 0.4998(11) 0.147(8) Uani 1 1 d . . . C86 C 0.8321(15) 0.3289(12) 0.4991(8) 0.089(6) Uani 1 1 d . . . C87 C 0.8482(14) 0.2425(11) 0.4994(10) 0.119(7) Uani 1 1 d . . . H87A H 0.9007 0.2515 0.5420 0.179 Uiso 1 1 calc R . . H87B H 0.8644 0.2306 0.4605 0.179 Uiso 1 1 calc R . . H87C H 0.7894 0.1924 0.4962 0.179 Uiso 1 1 calc R . . N4 N 0.3404(14) 0.4899(13) 0.0732(9) 0.125(6) Uani 1 1 d . . . C88 C 0.3496(15) 0.4530(15) 0.0345(10) 0.110(6) Uani 1 1 d . . . C89 C 0.3518(14) 0.4020(16) -0.0199(12) 0.152(9) Uani 1 1 d . . . H89A H 0.2923 0.3470 -0.0392 0.229 Uiso 1 1 calc R . . H89B H 0.4064 0.3885 -0.0028 0.229 Uiso 1 1 calc R . . H89C H 0.3584 0.4350 -0.0552 0.229 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 Fe1 0.0419(9) 0.0320(8) 0.0353(8) 0.0050(6) 0.0099(6) 0.0188(7) Fe2 0.0382(9) 0.0313(8) 0.0351(8) 0.0066(6) 0.0115(6) 0.0188(7) Fe3 0.0491(10) 0.0356(8) 0.0358(8) 0.0051(6) 0.0114(7) 0.0238(7) Fe4 0.0466(9) 0.0301(8) 0.0372(8) 0.0058(6) 0.0124(7) 0.0217(7) S1 0.0418(15) 0.0298(13) 0.0382(13) 0.0056(10) 0.0131(11) 0.0173(12) S2 0.0435(16) 0.0308(13) 0.0437(14) 0.0045(11) 0.0111(12) 0.0195(12) S3 0.0458(16) 0.0363(14) 0.0367(13) 0.0048(11) 0.0095(11) 0.0243(13) S4 0.0436(16) 0.0332(13) 0.0394(14) 0.0031(10) 0.0102(12) 0.0199(12) P1 0.0416(16) 0.0311(14) 0.0390(14) 0.0057(11) 0.0137(12) 0.0177(12) P2 0.0492(17) 0.0379(15) 0.0359(14) 0.0082(11) 0.0131(12) 0.0253(13) P3 0.065(2) 0.0385(16) 0.0398(15) 0.0087(12) 0.0136(14) 0.0302(15) P4 0.0600(19) 0.0305(14) 0.0489(16) 0.0055(12) 0.0213(14) 0.0216(14) N1 0.046(5) 0.036(5) 0.054(5) 0.013(4) 0.022(4) 0.021(4) N2 0.033(5) 0.044(5) 0.055(5) 0.006(4) 0.019(4) 0.019(4) C1 0.042(6) 0.044(6) 0.030(5) 0.004(5) 0.001(5) 0.021(5) C2 0.059(8) 0.039(6) 0.046(6) 0.003(5) 0.014(6) 0.028(6) C3 0.049(7) 0.043(6) 0.048(7) 0.016(5) 0.021(5) 0.025(5) C4 0.059(8) 0.042(6) 0.039(6) 0.002(5) 0.007(6) 0.030(6) C5 0.063(8) 0.048(7) 0.043(6) 0.009(5) 0.017(6) 0.032(6) C6 0.052(7) 0.053(7) 0.042(6) 0.002(5) 0.016(6) 0.029(6) C7 0.061(8) 0.043(7) 0.048(7) 0.003(5) 0.010(6) 0.019(6) C8 0.044(7) 0.034(6) 0.041(6) 0.005(4) 0.010(5) 0.016(5) C9 0.034(6) 0.035(6) 0.041(6) 0.002(4) 0.012(5) 0.013(5) C10 0.044(6) 0.032(5) 0.044(6) 0.001(4) 0.015(5) 0.019(5) C11 0.046(6) 0.025(5) 0.042(6) 0.001(4) 0.011(5) 0.015(5) C12 0.042(6) 0.036(6) 0.037(5) 0.004(4) 0.016(5) 0.019(5) C13 0.045(7) 0.046(7) 0.090(9) 0.009(6) 0.022(6) 0.028(6) C14 0.081(9) 0.039(6) 0.072(8) 0.022(6) 0.046(7) 0.028(6) C15 0.116(13) 0.061(9) 0.093(10) 0.018(7) 0.070(10) 0.034(9) C16 0.085(10) 0.045(7) 0.110(11) 0.032(7) 0.059(9) 0.022(7) C17 0.063(7) 0.034(6) 0.047(6) 0.011(5) 0.026(5) 0.028(5) C18 0.047(7) 0.040(6) 0.050(6) -0.002(5) 0.014(5) 0.021(5) C19 0.037(6) 0.049(7) 0.053(6) -0.002(5) 0.013(5) 0.020(5) C20 0.039(6) 0.040(6) 0.053(6) 0.006(5) 0.014(5) 0.021(5) C21 0.064(9) 0.072(9) 0.095(10) 0.024(8) 0.040(8) 0.034(8) C22 0.058(8) 0.052(7) 0.042(6) 0.003(5) 0.005(5) 0.030(6) C23 0.075(11) 0.078(10) 0.088(10) -0.003(8) 0.008(8) 0.026(9) C24 0.064(9) 0.097(11) 0.086(10) 0.026(8) 0.026(8) 0.054(9) C25 0.051(7) 0.037(6) 0.054(6) 0.011(5) 0.016(5) 0.028(5) C26 0.053(7) 0.040(6) 0.052(6) 0.016(5) 0.017(5) 0.025(6) C27 0.048(7) 0.026(5) 0.047(6) 0.011(4) 0.020(5) 0.020(5) C28 0.043(7) 0.040(6) 0.055(7) 0.003(5) 0.021(6) 0.008(5) C29 0.063(9) 0.044(7) 0.047(7) -0.007(5) 0.011(6) 0.017(6) C30 0.075(9) 0.048(7) 0.052(7) 0.011(6) 0.027(7) 0.034(7) C31 0.060(8) 0.047(7) 0.068(8) 0.021(6) 0.034(7) 0.033(6) C32 0.049(7) 0.032(5) 0.048(6) 0.005(5) 0.018(5) 0.020(5) C33 0.051(7) 0.033(5) 0.048(6) 0.014(5) 0.026(5) 0.022(5) C34 0.065(8) 0.042(7) 0.058(7) 0.013(5) 0.030(6) 0.026(6) C35 0.079(10) 0.040(7) 0.094(10) 0.028(7) 0.047(8) 0.023(7) C36 0.063(9) 0.055(8) 0.103(11) 0.019(8) 0.051(9) 0.016(7) C37 0.057(8) 0.057(8) 0.083(9) 0.013(7) 0.032(7) 0.023(7) C38 0.043(7) 0.038(6) 0.068(7) 0.011(5) 0.023(6) 0.015(6) C39 0.053(7) 0.046(6) 0.038(6) 0.010(5) 0.020(5) 0.026(6) C40 0.105(11) 0.080(9) 0.039(7) 0.020(6) 0.028(7) 0.061(9) C41 0.120(13) 0.087(10) 0.047(8) 0.022(7) 0.032(8) 0.059(10) C42 0.115(12) 0.073(9) 0.052(8) 0.012(7) 0.045(8) 0.048(9) C43 0.075(9) 0.065(8) 0.065(8) 0.004(7) 0.033(7) 0.037(8) C44 0.057(8) 0.058(7) 0.046(6) 0.006(5) 0.018(6) 0.027(6) C45 0.039(6) 0.044(6) 0.033(5) 0.003(4) 0.006(4) 0.021(5) C46 0.057(8) 0.051(7) 0.036(6) 0.004(5) 0.015(5) 0.029(6) C47 0.074(9) 0.047(7) 0.040(6) 0.002(5) 0.018(6) 0.023(7) C48 0.046(7) 0.064(8) 0.047(7) -0.007(6) 0.002(5) 0.019(7) C49 0.047(8) 0.070(9) 0.083(9) 0.012(7) 0.018(7) 0.029(7) C50 0.044(7) 0.050(7) 0.056(7) 0.008(5) 0.010(5) 0.026(6) C51 0.108(12) 0.044(7) 0.067(8) 0.025(6) 0.035(8) 0.047(8) C52 0.094(11) 0.043(7) 0.067(8) 0.022(6) 0.037(8) 0.029(7) C53 0.070(8) 0.051(7) 0.039(6) 0.006(5) 0.006(6) 0.043(7) C54 0.086(11) 0.071(9) 0.050(7) -0.008(6) -0.009(7) 0.058(8) C55 0.073(10) 0.104(12) 0.065(9) -0.002(8) 0.002(8) 0.067(10) C56 0.071(10) 0.122(14) 0.041(7) 0.011(8) 0.001(7) 0.057(10) C57 0.057(9) 0.070(9) 0.060(8) 0.002(6) 0.012(6) 0.033(7) C58 0.063(9) 0.056(8) 0.053(7) 0.002(6) 0.010(6) 0.036(7) C59 0.067(8) 0.046(7) 0.038(6) 0.012(5) 0.024(6) 0.027(6) C60 0.082(10) 0.052(7) 0.060(8) 0.015(6) 0.026(7) 0.034(7) C61 0.085(10) 0.082(10) 0.057(8) 0.019(7) 0.041(8) 0.025(8) C62 0.080(10) 0.071(9) 0.060(8) -0.004(7) 0.025(7) 0.039(8) C63 0.085(10) 0.065(8) 0.043(7) 0.009(6) 0.022(7) 0.042(8) C64 0.055(7) 0.045(7) 0.045(6) 0.009(5) 0.005(5) 0.029(6) C65 0.062(8) 0.032(6) 0.088(9) 0.012(6) 0.043(8) 0.018(6) C66 0.072(10) 0.057(8) 0.089(10) -0.003(7) 0.049(8) 0.016(7) C67 0.092(13) 0.068(11) 0.159(18) 0.002(11) 0.077(13) 0.035(10) C68 0.086(14) 0.088(13) 0.160(19) -0.010(13) 0.059(14) 0.027(11) C69 0.054(10) 0.084(11) 0.133(15) 0.010(10) 0.019(9) 0.030(9) C70 0.068(10) 0.050(8) 0.097(11) 0.016(7) 0.029(8) 0.027(7) C71 0.062(8) 0.043(7) 0.044(6) 0.001(5) 0.010(6) 0.032(6) C72 0.055(7) 0.037(6) 0.053(7) 0.003(5) 0.011(6) 0.022(6) C73 0.071(9) 0.061(8) 0.055(7) 0.004(6) 0.018(6) 0.044(7) C74 0.094(11) 0.043(7) 0.054(7) -0.003(6) 0.008(7) 0.043(8) C75 0.084(10) 0.035(7) 0.075(9) 0.005(6) 0.029(8) 0.016(7) C76 0.077(9) 0.042(7) 0.064(8) 0.008(6) 0.025(7) 0.023(7) O1 0.085(7) 0.043(5) 0.059(5) 0.016(4) 0.017(5) 0.030(5) O2 0.031(5) 0.061(5) 0.081(6) -0.002(4) 0.013(4) 0.012(4) O3 0.083(6) 0.055(5) 0.039(4) 0.003(4) 0.018(4) 0.032(5) O4 0.053(5) 0.069(6) 0.075(6) 0.012(4) 0.038(5) 0.025(5) O5 0.152(10) 0.067(6) 0.067(6) 0.029(5) 0.032(6) 0.066(7) O6 0.062(6) 0.064(6) 0.052(5) -0.014(4) -0.001(4) 0.032(5) O7 0.067(6) 0.095(7) 0.065(5) 0.002(5) 0.033(5) 0.043(6) O8 0.058(5) 0.049(5) 0.068(5) 0.003(4) 0.017(4) 0.034(4) S5 0.058(2) 0.064(2) 0.0629(19) 0.0193(16) 0.0260(16) 0.0309(17) O9 0.104(8) 0.071(6) 0.113(8) 0.028(6) 0.030(6) 0.058(6) O10 0.092(7) 0.063(6) 0.108(8) 0.007(5) 0.043(6) 0.032(6) O11 0.064(7) 0.165(11) 0.068(6) 0.019(6) 0.033(5) 0.031(7) C77 0.075(10) 0.078(10) 0.082(10) 0.036(9) 0.036(8) 0.038(9) F1 0.101(7) 0.124(8) 0.093(7) -0.019(6) 0.005(5) 0.037(7) F2 0.075(6) 0.141(9) 0.122(8) 0.036(7) 0.052(6) 0.007(6) F3 0.075(6) 0.151(10) 0.158(9) 0.069(8) 0.028(6) 0.058(7) N3 0.182(19) 0.104(15) 0.140(16) 0.067(14) 0.051(13) 0.053(15) C86 0.125(15) 0.070(11) 0.059(9) 0.024(9) 0.050(9) 0.020(11) C87 0.120(15) 0.093(13) 0.127(15) 0.066(12) 0.030(12) 0.038(12) N4 0.165(17) 0.135(15) 0.095(12) 0.038(11) 0.039(12) 0.092(14) C88 0.107(15) 0.128(18) 0.076(13) 0.013(12) 0.010(11) 0.056(13) C89 0.082(14) 0.17(2) 0.15(2) -0.026(17) 0.024(13) 0.036(15) _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 C3 1.776(11) . ? Fe1 C1 1.783(11) . ? Fe1 C2 1.812(14) . ? Fe1 S1 2.271(3) . ? Fe1 S3 2.287(3) . ? Fe1 Fe2 2.5490(18) . ? Fe2 C4 1.779(14) . ? Fe2 P2 2.204(3) . ? Fe2 P1 2.232(3) . ? Fe2 S1 2.266(3) . ? Fe2 S3 2.269(3) . ? Fe3 C7 1.774(14) . ? Fe3 C6 1.774(12) . ? Fe3 C5 1.806(12) . ? Fe3 S2 2.276(3) . ? Fe3 S4 2.279(3) . ? Fe3 Fe4 2.5397(19) . ? Fe4 C8 1.724(11) . ? Fe4 P3 2.194(3) . ? Fe4 P4 2.231(3) . ? Fe4 S4 2.246(3) . ? Fe4 S2 2.282(3) . ? S1 C9 1.836(10) . ? S2 C12 1.840(9) . ? S3 C17 1.836(11) . ? S4 C20 1.832(10) . ? P1 C33 1.832(11) . ? P1 C27 1.838(10) . ? P1 C25 1.852(10) . ? P2 C45 1.805(11) . ? P2 C39 1.840(10) . ? P2 C26 1.845(10) . ? P3 C59 1.824(11) . ? P3 C53 1.815(12) . ? P3 C51 1.831(11) . ? P4 C71 1.820(10) . ? P4 C65 1.830(13) . ? P4 C52 1.833(12) . ? N1 C10 1.499(13) . ? N1 C11 1.511(12) . ? N1 C13 1.509(14) . ? N1 C14 1.548(14) . ? N2 C19 1.505(13) . ? N2 C18 1.513(13) . ? N2 C21 1.548(15) . ? N2 C22 1.543(14) . ? C1 O1 1.143(12) . ? C2 O2 1.116(13) . ? C3 O3 1.154(12) . ? C4 O4 1.138(13) . ? C5 O5 1.124(13) . ? C6 O6 1.160(13) . ? C7 O7 1.153(14) . ? C8 O8 1.179(12) . ? C9 C10 1.525(14) . ? C11 C12 1.542(14) . ? C14 C15 1.524(17) . ? C14 C16 1.565(16) . ? C17 C18 1.507(14) . ? C19 C20 1.522(15) . ? C22 C24 1.511(16) . ? C22 C23 1.509(18) . ? C25 C26 1.527(14) . ? C27 C28 1.381(15) . ? C27 C32 1.406(14) . ? C28 C29 1.381(15) . ? C29 C30 1.367(17) . ? C30 C31 1.399(17) . ? C31 C32 1.384(15) . ? C33 C34 1.376(14) . ? C33 C38 1.403(15) . ? C34 C35 1.344(17) . ? C35 C36 1.391(19) . ? C36 C37 1.388(18) . ? C37 C38 1.346(16) . ? C39 C44 1.360(15) . ? C39 C40 1.384(15) . ? C40 C41 1.378(17) . ? C41 C42 1.336(19) . ? C42 C43 1.365(18) . ? C43 C44 1.401(16) . ? C45 C50 1.385(14) . ? C45 C46 1.385(14) . ? C46 C47 1.377(16) . ? C47 C48 1.410(17) . ? C48 C49 1.358(17) . ? C49 C50 1.378(17) . ? C51 C52 1.544(19) . ? C53 C58 1.401(16) . ? C53 C54 1.410(15) . ? C54 C55 1.378(19) . ? C55 C56 1.38(2) . ? C56 C57 1.392(18) . ? C57 C58 1.372(17) . ? C59 C64 1.367(14) . ? C59 C60 1.403(16) . ? C60 C61 1.377(17) . ? C61 C62 1.393(18) . ? C62 C63 1.349(18) . ? C63 C64 1.350(15) . ? C65 C70 1.402(18) . ? C65 C66 1.402(16) . ? C66 C67 1.38(2) . ? C67 C68 1.31(3) . ? C68 C69 1.38(2) . ? C69 C70 1.361(19) . ? C71 C76 1.377(16) . ? C71 C72 1.418(16) . ? C72 C73 1.387(15) . ? C73 C74 1.388(18) . ? C74 C75 1.340(18) . ? C75 C76 1.371(16) . ? S5 O11 1.401(9) . ? S5 O10 1.406(9) . ? S5 O9 1.421(8) . ? S5 C77 1.755(12) . ? C77 F3 1.346(13) . ? C77 F1 1.317(13) . ? C77 F2 1.328(13) . ? S6 O14 1.412(10) . ? S6 O13 1.405(10) . ? S6 O12 1.431(9) . ? S6 C78 1.715(11) . ? C78 F6 1.373(12) . ? C78 F4 1.337(11) . ? C78 F5 1.328(12) . ? O15 C80 1.44(3) . ? O15 C81 1.50(3) . ? C79 C80 1.35(3) . ? C81 C82 1.455(18) . ? C83 Cl1 1.672(17) . ? C83 Cl2 1.697(17) . ? C84 Cl4 1.652(19) . ? C84 Cl3 1.676(19) . ? N3 C86 0.93(2) . ? C86 C87 1.60(3) . ? N4 C88 1.09(2) . ? C88 C89 1.41(3) . ? 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 C3 Fe1 C1 95.7(4) . . ? C3 Fe1 C2 90.5(5) . . ? C1 Fe1 C2 108.8(5) . . ? C3 Fe1 S1 88.7(3) . . ? C1 Fe1 S1 114.2(3) . . ? C2 Fe1 S1 136.9(3) . . ? C3 Fe1 S3 168.0(3) . . ? C1 Fe1 S3 92.7(3) . . ? C2 Fe1 S3 94.8(3) . . ? S1 Fe1 S3 80.08(10) . . ? C3 Fe1 Fe2 114.2(3) . . ? C1 Fe1 Fe2 146.8(3) . . ? C2 Fe1 Fe2 85.9(3) . . ? S1 Fe1 Fe2 55.72(8) . . ? S3 Fe1 Fe2 55.63(7) . . ? C4 Fe2 P2 94.4(3) . . ? C4 Fe2 P1 93.2(3) . . ? P2 Fe2 P1 88.10(10) . . ? C4 Fe2 S1 163.4(3) . . ? P2 Fe2 S1 102.26(11) . . ? P1 Fe2 S1 88.07(10) . . ? C4 Fe2 S3 94.5(3) . . ? P2 Fe2 S3 105.25(10) . . ? P1 Fe2 S3 163.99(11) . . ? S1 Fe2 S3 80.59(10) . . ? C4 Fe2 Fe1 108.2(3) . . ? P2 Fe2 Fe1 151.11(10) . . ? P1 Fe2 Fe1 107.86(9) . . ? S1 Fe2 Fe1 55.92(7) . . ? S3 Fe2 Fe1 56.32(7) . . ? C7 Fe3 C6 91.8(5) . . ? C7 Fe3 C5 98.3(5) . . ? C6 Fe3 C5 100.1(5) . . ? C7 Fe3 S2 158.3(4) . . ? C6 Fe3 S2 87.4(4) . . ? C5 Fe3 S2 103.2(4) . . ? C7 Fe3 S4 92.1(4) . . ? C6 Fe3 S4 154.7(4) . . ? C5 Fe3 S4 104.1(4) . . ? S2 Fe3 S4 79.89(10) . . ? C7 Fe3 Fe4 102.6(4) . . ? C6 Fe3 Fe4 99.6(4) . . ? C5 Fe3 Fe4 150.6(3) . . ? S2 Fe3 Fe4 56.24(8) . . ? S4 Fe3 Fe4 55.24(8) . . ? C8 Fe4 P3 91.7(3) . . ? C8 Fe4 P4 91.0(4) . . ? P3 Fe4 P4 86.33(12) . . ? C8 Fe4 S4 95.6(4) . . ? P3 Fe4 S4 100.88(11) . . ? P4 Fe4 S4 170.03(12) . . ? C8 Fe4 S2 149.2(3) . . ? P3 Fe4 S2 119.14(11) . . ? P4 Fe4 S2 90.02(11) . . ? S4 Fe4 S2 80.47(10) . . ? C8 Fe4 Fe3 96.3(3) . . ? P3 Fe4 Fe3 156.57(11) . . ? P4 Fe4 Fe3 115.44(10) . . ? S4 Fe4 Fe3 56.49(8) . . ? S2 Fe4 Fe3 56.02(8) . . ? C9 S1 Fe2 114.0(3) . . ? C9 S1 Fe1 111.7(3) . . ? Fe2 S1 Fe1 68.36(9) . . ? C12 S2 Fe3 110.8(3) . . ? C12 S2 Fe4 120.5(3) . . ? Fe3 S2 Fe4 67.74(9) . . ? C17 S3 Fe2 115.5(3) . . ? C17 S3 Fe1 112.4(3) . . ? Fe2 S3 Fe1 68.04(8) . . ? C20 S4 Fe4 112.7(3) . . ? C20 S4 Fe3 114.0(4) . . ? Fe4 S4 Fe3 68.28(9) . . ? C33 P1 C27 100.9(5) . . ? C33 P1 C25 105.8(5) . . ? C27 P1 C25 103.3(5) . . ? C33 P1 Fe2 117.0(3) . . ? C27 P1 Fe2 122.8(3) . . ? C25 P1 Fe2 105.2(3) . . ? C45 P2 C39 99.8(5) . . ? C45 P2 C26 104.5(5) . . ? C39 P2 C26 103.9(5) . . ? C45 P2 Fe2 117.7(3) . . ? C39 P2 Fe2 120.8(4) . . ? C26 P2 Fe2 108.3(4) . . ? C59 P3 C53 104.5(5) . . ? C59 P3 C51 106.0(6) . . ? C53 P3 C51 104.1(6) . . ? C59 P3 Fe4 119.8(4) . . ? C53 P3 Fe4 115.1(4) . . ? C51 P3 Fe4 106.0(4) . . ? C71 P4 C65 100.9(5) . . ? C71 P4 C52 102.9(5) . . ? C65 P4 C52 103.0(6) . . ? C71 P4 Fe4 121.5(4) . . ? C65 P4 Fe4 117.1(4) . . ? C52 P4 Fe4 109.2(4) . . ? C10 N1 C11 110.8(8) . . ? C10 N1 C13 110.3(8) . . ? C11 N1 C13 108.0(8) . . ? C10 N1 C14 106.3(8) . . ? C11 N1 C14 112.4(8) . . ? C13 N1 C14 109.0(9) . . ? C19 N2 C18 111.7(8) . . ? C19 N2 C21 106.7(9) . . ? C18 N2 C21 109.9(8) . . ? C19 N2 C22 111.6(8) . . ? C18 N2 C22 107.9(8) . . ? C21 N2 C22 109.0(9) . . ? O1 C1 Fe1 176.5(10) . . ? O2 C2 Fe1 178.0(10) . . ? O3 C3 Fe1 177.2(9) . . ? O4 C4 Fe2 178.4(10) . . ? O5 C5 Fe3 175.9(11) . . ? O6 C6 Fe3 177.5(10) . . ? O7 C7 Fe3 179.0(12) . . ? O8 C8 Fe4 177.8(9) . . ? C10 C9 S1 107.4(6) . . ? N1 C10 C9 114.3(8) . . ? N1 C11 C12 116.6(8) . . ? C11 C12 S2 105.9(6) . . ? C15 C14 N1 110.0(9) . . ? C15 C14 C16 110.1(11) . . ? N1 C14 C16 111.1(9) . . ? C18 C17 S3 109.5(7) . . ? C17 C18 N2 116.1(8) . . ? N2 C19 C20 118.9(9) . . ? C19 C20 S4 116.9(7) . . ? C24 C22 C23 107.9(11) . . ? C24 C22 N2 112.3(9) . . ? C23 C22 N2 110.5(10) . . ? C26 C25 P1 108.7(7) . . ? C25 C26 P2 109.5(7) . . ? C28 C27 C32 117.5(9) . . ? C28 C27 P1 122.5(8) . . ? C32 C27 P1 120.0(8) . . ? C29 C28 C27 122.1(11) . . ? C30 C29 C28 119.9(11) . . ? C29 C30 C31 120.1(11) . . ? C30 C31 C32 119.5(11) . . ? C31 C32 C27 120.9(10) . . ? C34 C33 C38 116.9(10) . . ? C34 C33 P1 123.9(9) . . ? C38 C33 P1 119.0(8) . . ? C35 C34 C33 122.8(12) . . ? C34 C35 C36 119.5(12) . . ? C35 C36 C37 119.2(12) . . ? C38 C37 C36 120.2(13) . . ? C37 C38 C33 121.4(11) . . ? C44 C39 C40 119.4(10) . . ? C44 C39 P2 121.8(8) . . ? C40 C39 P2 118.6(8) . . ? C41 C40 C39 119.0(12) . . ? C42 C41 C40 122.0(12) . . ? C41 C42 C43 119.8(12) . . ? C42 C43 C44 119.6(12) . . ? C39 C44 C43 120.1(11) . . ? C50 C45 C46 118.1(10) . . ? C50 C45 P2 122.7(8) . . ? C46 C45 P2 119.1(8) . . ? C47 C46 C45 121.6(11) . . ? C46 C47 C48 119.7(11) . . ? C49 C48 C47 117.9(12) . . ? C48 C49 C50 122.5(12) . . ? C49 C50 C45 120.0(11) . . ? C52 C51 P3 108.4(8) . . ? C51 C52 P4 109.9(8) . . ? C58 C53 C54 117.5(12) . . ? C58 C53 P3 121.9(8) . . ? C54 C53 P3 120.1(9) . . ? C55 C54 C53 120.3(12) . . ? C56 C55 C54 121.6(12) . . ? C55 C56 C57 118.7(13) . . ? C58 C57 C56 120.5(13) . . ? C57 C58 C53 121.4(11) . . ? C64 C59 C60 117.1(10) . . ? C64 C59 P3 119.7(8) . . ? C60 C59 P3 123.2(9) . . ? C61 C60 C59 120.3(11) . . ? C62 C61 C60 119.5(12) . . ? C63 C62 C61 120.0(12) . . ? C64 C63 C62 120.0(12) . . ? C63 C64 C59 123.1(11) . . ? C70 C65 C66 117.8(13) . . ? C70 C65 P4 121.0(10) . . ? C66 C65 P4 121.2(11) . . ? C67 C66 C65 118.8(15) . . ? C68 C67 C66 124.1(17) . . ? C67 C68 C69 117.1(19) . . ? C70 C69 C68 123.2(18) . . ? C69 C70 C65 118.9(15) . . ? C76 C71 C72 117.5(10) . . ? C76 C71 P4 120.7(9) . . ? C72 C71 P4 121.7(9) . . ? C73 C72 C71 120.9(11) . . ? C74 C73 C72 118.8(12) . . ? C75 C74 C73 119.9(11) . . ? C74 C75 C76 122.5(12) . . ? C71 C76 C75 120.3(12) . . ? O11 S5 O10 116.6(7) . . ? O11 S5 O9 113.4(7) . . ? O10 S5 O9 114.3(6) . . ? O11 S5 C77 103.2(6) . . ? O10 S5 C77 104.1(6) . . ? O9 S5 C77 103.0(6) . . ? F3 C77 F1 104.5(11) . . ? F3 C77 F2 105.6(11) . . ? F1 C77 F2 109.3(11) . . ? F3 C77 S5 111.9(9) . . ? F1 C77 S5 112.8(9) . . ? F2 C77 S5 112.2(9) . . ? O14 S6 O13 113.3(9) . . ? O14 S6 O12 111.6(8) . . ? O13 S6 O12 111.2(8) . . ? O14 S6 C78 93.6(7) . . ? O13 S6 C78 117.2(9) . . ? O12 S6 C78 108.8(8) . . ? F6 C78 F4 110.6(12) . . ? F6 C78 F5 98.1(11) . . ? F4 C78 F5 119.7(11) . . ? F6 C78 S6 91.6(7) . . ? F4 C78 S6 111.2(10) . . ? F5 C78 S6 119.8(13) . . ? C80 O15 C81 112(2) . . ? C79 C80 O15 109(3) . . ? C82 C81 O15 101(2) . . ? Cl1 C83 Cl2 114.6(14) . . ? Cl4 C84 Cl3 114.0(18) . . ? N3 C86 C87 174(3) . . ? N4 C88 C89 174(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.567 _refine_diff_density_min -2.565 _refine_diff_density_rms 0.178 # Attachment '- complex_6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 793186' #TrackingRef '- complex_6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H86 Fe4 N2 O9 P4 S4' _chemical_formula_weight 1671.01 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' P P 0.1023 0.0942 '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 Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.5258(4) _cell_length_b 15.5258(4) _cell_length_c 33.5050(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8076.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27175 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27175 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9224 _reflns_number_gt 7117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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. ; _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^)+(0.0927P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(18) _refine_ls_number_reflns 9224 _refine_ls_number_parameters 444 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.088 _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 Fe1 Fe 0.33743(4) 0.46832(4) 0.327123(18) 0.03364(16) Uani 1 1 d . . . Fe2 Fe 0.38479(4) 0.31463(4) 0.311885(18) 0.03402(16) Uani 1 1 d . . . S1 S 0.30890(7) 0.39899(7) 0.26922(3) 0.0338(2) Uani 1 1 d . . . S2 S 0.56928(7) 0.52772(7) 0.19048(3) 0.0361(2) Uani 1 1 d . . . P1 P 0.19628(7) 0.47024(7) 0.33503(3) 0.0346(2) Uani 1 1 d . . . P2 P 0.26878(7) 0.23803(7) 0.32668(3) 0.0333(2) Uani 1 1 d . . . C1 C 0.3471(3) 0.5821(3) 0.32048(16) 0.0491(12) Uani 1 1 d . . . C2 C 0.3579(3) 0.4602(3) 0.37867(15) 0.0451(11) Uani 1 1 d . . . C3 C 0.4341(3) 0.2794(3) 0.35633(16) 0.0462(11) Uani 1 1 d . . . C4 C 0.4324(3) 0.2372(3) 0.27938(15) 0.0450(11) Uani 1 1 d . . . C5 C 0.3738(3) 0.4382(3) 0.22765(13) 0.0391(10) Uani 1 1 d . . . H5A H 0.3619 0.5001 0.2234 0.047 Uiso 1 1 calc R . . H5B H 0.4356 0.4320 0.2343 0.047 Uiso 1 1 calc R . . C6 C 0.3550(3) 0.3894(3) 0.18962(14) 0.0434(11) Uani 1 1 d . . . H6A H 0.3645 0.3271 0.1942 0.052 Uiso 1 1 calc R . . H6B H 0.2938 0.3977 0.1822 0.052 Uiso 1 1 calc R . . C7 C 0.4969(3) 0.3813(3) 0.15835(15) 0.0436(11) Uani 1 1 d . . . H7A H 0.5010 0.3350 0.1381 0.052 Uiso 1 1 calc R . . H7B H 0.5070 0.3551 0.1849 0.052 Uiso 1 1 calc R . . C8 C 0.5654(3) 0.4470(3) 0.15042(14) 0.0440(11) Uani 1 1 d . . . H8A H 0.5536 0.4760 0.1247 0.053 Uiso 1 1 calc R . . H8B H 0.6220 0.4180 0.1483 0.053 Uiso 1 1 calc R . . C9 C 0.3698(4) 0.4141(4) 0.11680(16) 0.0641(16) Uani 1 1 d . . . H9 H 0.4160 0.4300 0.0974 0.077 Uiso 1 1 calc R . . C10 C 0.2998(5) 0.4813(5) 0.11286(19) 0.0788(19) Uani 1 1 d . . . H10A H 0.2551 0.4708 0.1329 0.118 Uiso 1 1 calc R . . H10B H 0.2744 0.4780 0.0861 0.118 Uiso 1 1 calc R . . H10C H 0.3246 0.5387 0.1170 0.118 Uiso 1 1 calc R . . C11 C 0.3390(5) 0.3257(5) 0.10548(19) 0.081(2) Uani 1 1 d . . . H11A H 0.3839 0.2834 0.1117 0.121 Uiso 1 1 calc R . . H11B H 0.3265 0.3241 0.0768 0.121 Uiso 1 1 calc R . . H11C H 0.2867 0.3119 0.1205 0.121 Uiso 1 1 calc R . . C12 C 0.1415(3) 0.3673(3) 0.32698(14) 0.0378(10) Uani 1 1 d . . . H12A H 0.0796 0.3739 0.3335 0.045 Uiso 1 1 calc R . . H12B H 0.1459 0.3514 0.2984 0.045 Uiso 1 1 calc R . . C13 C 0.1796(3) 0.2943(3) 0.35249(12) 0.0363(9) Uani 1 1 d . . . H13A H 0.1336 0.2523 0.3589 0.044 Uiso 1 1 calc R . . H13B H 0.2011 0.3185 0.3779 0.044 Uiso 1 1 calc R . . C14 C 0.1389(3) 0.5426(3) 0.30107(14) 0.0406(10) Uani 1 1 d . . . C15 C 0.1787(3) 0.5790(3) 0.26861(15) 0.0494(12) Uani 1 1 d . . . H15 H 0.2365 0.5645 0.2622 0.059 Uiso 1 1 calc R . . C16 C 0.1319(4) 0.6393(4) 0.24455(18) 0.0640(16) Uani 1 1 d . . . H16 H 0.1594 0.6639 0.2219 0.077 Uiso 1 1 calc R . . C17 C 0.0523(4) 0.6616(4) 0.25267(18) 0.0626(15) Uani 1 1 d . . . H17 H 0.0234 0.7032 0.2368 0.075 Uiso 1 1 calc R . . C18 C 0.0112(4) 0.6236(4) 0.2846(2) 0.0658(16) Uani 1 1 d . . . H18 H -0.0471 0.6379 0.2899 0.079 Uiso 1 1 calc R . . C19 C 0.0524(3) 0.5654(4) 0.30900(18) 0.0565(14) Uani 1 1 d . . . H19 H 0.0229 0.5406 0.3310 0.068 Uiso 1 1 calc R . . C20 C 0.1552(3) 0.5035(3) 0.38398(14) 0.0380(10) Uani 1 1 d . . . C21 C 0.0914(3) 0.4607(4) 0.40406(16) 0.0520(13) Uani 1 1 d . . . H21 H 0.0676 0.4095 0.3930 0.062 Uiso 1 1 calc R . . C22 C 0.0606(4) 0.4919(4) 0.44102(17) 0.0631(16) Uani 1 1 d . . . H22 H 0.0165 0.4614 0.4546 0.076 Uiso 1 1 calc R . . C23 C 0.0928(4) 0.5636(4) 0.45706(17) 0.0577(14) Uani 1 1 d . . . H23 H 0.0714 0.5847 0.4818 0.069 Uiso 1 1 calc R . . C24 C 0.1564(4) 0.6060(4) 0.43752(17) 0.0581(14) Uani 1 1 d . . . H24 H 0.1799 0.6569 0.4489 0.070 Uiso 1 1 calc R . . C25 C 0.1881(3) 0.5763(3) 0.40101(16) 0.0494(12) Uani 1 1 d . . . H25 H 0.2328 0.6071 0.3879 0.059 Uiso 1 1 calc R . . C26 C 0.2955(3) 0.1477(3) 0.35918(14) 0.0413(10) Uani 1 1 d . . . C27 C 0.3316(3) 0.0753(3) 0.34313(18) 0.0540(14) Uani 1 1 d . . . H27 H 0.3374 0.0711 0.3150 0.065 Uiso 1 1 calc R . . C28 C 0.3600(4) 0.0074(4) 0.3671(2) 0.0721(19) Uani 1 1 d . . . H28 H 0.3841 -0.0428 0.3554 0.087 Uiso 1 1 calc R . . C29 C 0.3529(4) 0.0140(5) 0.4073(2) 0.080(2) Uani 1 1 d . . . H29 H 0.3709 -0.0326 0.4236 0.095 Uiso 1 1 calc R . . C30 C 0.3209(4) 0.0850(5) 0.42432(19) 0.0713(19) Uani 1 1 d . . . H30 H 0.3188 0.0891 0.4526 0.086 Uiso 1 1 calc R . . C31 C 0.2908(4) 0.1530(4) 0.40103(16) 0.0583(14) Uani 1 1 d . . . H31 H 0.2671 0.2027 0.4134 0.070 Uiso 1 1 calc R . . C32 C 0.2096(3) 0.1816(3) 0.28689(13) 0.0374(10) Uani 1 1 d . . . C33 C 0.2342(3) 0.1848(3) 0.24752(14) 0.0460(11) Uani 1 1 d . . . H33 H 0.2829 0.2180 0.2399 0.055 Uiso 1 1 calc R . . C34 C 0.1880(4) 0.1396(3) 0.21890(17) 0.0598(15) Uani 1 1 d . . . H34 H 0.2049 0.1428 0.1917 0.072 Uiso 1 1 calc R . . C35 C 0.1196(4) 0.0915(4) 0.2293(2) 0.0646(16) Uani 1 1 d . . . H35 H 0.0881 0.0616 0.2093 0.077 Uiso 1 1 calc R . . C36 C 0.0958(4) 0.0857(5) 0.2677(2) 0.079(2) Uani 1 1 d . . . H36 H 0.0481 0.0504 0.2746 0.095 Uiso 1 1 calc R . . C37 C 0.1389(4) 0.1296(4) 0.29710(18) 0.0617(16) Uani 1 1 d . . . H37 H 0.1210 0.1249 0.3241 0.074 Uiso 1 1 calc R . . N1 N 0.4091(3) 0.4182(3) 0.15735(11) 0.0422(9) Uani 1 1 d . . . O1 O 0.3548(2) 0.6546(2) 0.31664(15) 0.0668(11) Uani 1 1 d . . . O2 O 0.3739(3) 0.4563(3) 0.41202(10) 0.0667(11) Uani 1 1 d . . . O3 O 0.4687(2) 0.2581(3) 0.38506(11) 0.0608(10) Uani 1 1 d . . . O4 O 0.4623(3) 0.1872(3) 0.25858(12) 0.0667(11) Uani 1 1 d . . . O5 O 0.7912(5) 0.2088(5) 0.2500 0.150 Uiso 1 2 d SD . . C38 C 0.7064(6) 0.2047(7) 0.2693(3) 0.141(4) Uiso 1 1 d D . . H38A H 0.7141 0.1967 0.2984 0.169 Uiso 1 1 calc R . . H38B H 0.6742 0.1545 0.2589 0.169 Uiso 1 1 calc R . . C39 C 0.6544(5) 0.2876(5) 0.2616(3) 0.118(3) Uiso 1 1 d D . . H39A H 0.6016 0.2746 0.2461 0.141 Uiso 1 1 calc R . . H39B H 0.6376 0.3149 0.2871 0.141 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 Fe1 0.0328(3) 0.0373(3) 0.0308(3) 0.0013(3) 0.0006(2) -0.0019(3) Fe2 0.0328(3) 0.0374(3) 0.0319(3) 0.0046(3) 0.0033(2) -0.0012(3) S1 0.0364(6) 0.0373(6) 0.0277(5) 0.0035(4) 0.0019(4) -0.0021(4) S2 0.0410(6) 0.0330(5) 0.0342(5) 0.0012(4) 0.0066(5) -0.0033(4) P1 0.0336(6) 0.0368(6) 0.0335(6) -0.0005(5) 0.0004(4) -0.0006(5) P2 0.0349(6) 0.0362(6) 0.0287(5) 0.0034(4) 0.0025(4) -0.0025(5) C1 0.037(2) 0.050(3) 0.060(3) -0.005(2) 0.005(2) -0.001(2) C2 0.039(2) 0.057(3) 0.040(3) -0.003(2) 0.000(2) 0.002(2) C3 0.039(3) 0.046(3) 0.053(3) 0.012(2) 0.002(2) -0.008(2) C4 0.042(3) 0.043(3) 0.050(3) 0.009(2) 0.009(2) 0.001(2) C5 0.048(3) 0.038(2) 0.032(2) 0.0048(19) 0.002(2) -0.0108(19) C6 0.047(3) 0.053(3) 0.031(2) 0.001(2) -0.001(2) -0.008(2) C7 0.049(3) 0.040(2) 0.042(2) -0.003(2) 0.005(2) -0.003(2) C8 0.053(3) 0.040(3) 0.039(3) -0.011(2) 0.011(2) -0.003(2) C9 0.076(4) 0.084(4) 0.032(3) -0.001(3) -0.004(3) -0.012(3) C10 0.080(4) 0.106(5) 0.051(3) 0.017(4) -0.012(3) 0.012(4) C11 0.092(5) 0.100(5) 0.050(3) -0.016(3) -0.007(3) -0.025(4) C12 0.035(2) 0.042(2) 0.036(2) -0.0034(19) 0.0001(19) -0.0013(18) C13 0.034(2) 0.041(2) 0.033(2) 0.0014(18) 0.0069(18) -0.0011(18) C14 0.043(3) 0.040(2) 0.039(3) -0.001(2) -0.0079(19) 0.000(2) C15 0.051(3) 0.050(3) 0.048(3) 0.006(2) -0.005(2) 0.005(2) C16 0.076(4) 0.064(4) 0.052(3) 0.018(3) -0.007(3) 0.002(3) C17 0.067(4) 0.062(3) 0.059(4) 0.009(3) -0.026(3) 0.006(3) C18 0.046(3) 0.068(4) 0.083(4) 0.012(3) -0.005(3) 0.006(3) C19 0.046(3) 0.062(3) 0.061(3) 0.017(3) 0.000(3) 0.003(2) C20 0.037(2) 0.042(2) 0.035(2) -0.0021(19) 0.0017(18) 0.0058(19) C21 0.052(3) 0.060(3) 0.044(3) -0.009(3) 0.006(2) 0.002(2) C22 0.062(3) 0.083(4) 0.045(3) -0.006(3) 0.016(3) 0.001(3) C23 0.058(3) 0.069(4) 0.046(3) -0.020(3) 0.011(3) 0.008(3) C24 0.057(3) 0.059(3) 0.058(3) -0.022(3) -0.011(3) 0.011(3) C25 0.044(3) 0.054(3) 0.051(3) -0.008(2) 0.003(2) 0.005(2) C26 0.040(2) 0.045(3) 0.039(2) 0.007(2) 0.001(2) -0.004(2) C27 0.045(3) 0.052(3) 0.065(3) 0.018(3) 0.011(3) 0.006(2) C28 0.055(4) 0.062(4) 0.099(5) 0.035(4) 0.015(3) 0.016(3) C29 0.049(3) 0.094(5) 0.096(5) 0.060(4) 0.009(3) 0.020(3) C30 0.055(3) 0.105(5) 0.053(3) 0.043(4) -0.003(3) -0.011(4) C31 0.054(3) 0.076(4) 0.045(3) 0.014(3) 0.001(2) -0.006(3) C32 0.040(2) 0.035(2) 0.036(2) -0.0035(19) -0.0003(18) 0.0003(19) C33 0.060(3) 0.039(3) 0.039(2) -0.002(2) -0.003(2) -0.002(2) C34 0.085(4) 0.050(3) 0.044(3) -0.005(2) -0.009(3) 0.000(3) C35 0.059(4) 0.062(4) 0.072(4) -0.008(3) -0.014(3) -0.008(3) C36 0.059(4) 0.107(5) 0.070(4) -0.024(4) 0.008(3) -0.033(4) C37 0.058(3) 0.077(4) 0.050(3) -0.011(3) 0.010(3) -0.032(3) N1 0.048(2) 0.052(2) 0.0259(18) 0.0039(17) 0.0002(16) -0.0045(18) O1 0.059(2) 0.0332(19) 0.108(3) 0.005(2) 0.005(2) -0.0034(16) O2 0.065(2) 0.104(3) 0.0318(18) -0.004(2) -0.0083(17) 0.013(2) O3 0.046(2) 0.074(3) 0.063(2) 0.026(2) -0.0183(18) -0.0085(18) O4 0.070(3) 0.060(2) 0.069(3) -0.008(2) 0.028(2) 0.009(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 Fe1 C2 1.761(5) . ? Fe1 C1 1.787(5) . ? Fe1 P1 2.2076(13) . ? Fe1 S2 2.2521(12) 8_665 ? Fe1 S1 2.2624(12) . ? Fe1 Fe2 2.5485(9) . ? Fe2 C3 1.761(5) . ? Fe2 C4 1.782(5) . ? Fe2 P2 2.2145(12) . ? Fe2 S2 2.2584(12) 8_665 ? Fe2 S1 2.2686(12) . ? S1 C5 1.824(4) . ? S2 C8 1.837(5) . ? S2 Fe1 2.2521(12) 8_665 ? S2 Fe2 2.2583(12) 8_665 ? P1 C14 1.831(5) . ? P1 C12 1.831(4) . ? P1 C20 1.834(5) . ? P2 C26 1.824(5) . ? P2 C32 1.841(5) . ? P2 C13 1.852(4) . ? C1 O1 1.139(6) . ? C2 O2 1.146(6) . ? C3 O3 1.151(6) . ? C4 O4 1.142(6) . ? C5 C6 1.511(6) . ? C6 N1 1.441(6) . ? C7 N1 1.479(6) . ? C7 C8 1.498(7) . ? C9 N1 1.491(6) . ? C9 C11 1.503(9) . ? C9 C10 1.512(9) . ? C12 C13 1.537(6) . ? C14 C15 1.372(7) . ? C14 C19 1.413(7) . ? C15 C16 1.433(8) . ? C16 C17 1.311(9) . ? C17 C18 1.378(9) . ? C18 C19 1.376(8) . ? C20 C25 1.366(7) . ? C20 C21 1.370(7) . ? C21 C22 1.413(7) . ? C22 C23 1.333(8) . ? C23 C24 1.355(8) . ? C24 C25 1.397(7) . ? C26 C27 1.365(7) . ? C26 C31 1.407(7) . ? C27 C28 1.397(8) . ? C28 C29 1.355(10) . ? C29 C30 1.336(10) . ? C30 C31 1.394(9) . ? C32 C33 1.374(6) . ? C32 C37 1.406(7) . ? C33 C34 1.388(7) . ? C34 C35 1.344(9) . ? C35 C36 1.342(9) . ? C36 C37 1.373(8) . ? O5 C38 1.467(8) 8_665 ? O5 C38 1.467(8) . ? C38 C39 1.542(8) . ? C39 C39 1.492(9) 8_665 ? 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 C2 Fe1 C1 100.2(2) . . ? C2 Fe1 P1 93.59(16) . . ? C1 Fe1 P1 94.89(16) . . ? C2 Fe1 S2 94.04(16) . 8_665 ? C1 Fe1 S2 98.35(16) . 8_665 ? P1 Fe1 S2 163.29(5) . 8_665 ? C2 Fe1 S1 147.42(18) . . ? C1 Fe1 S1 112.34(18) . . ? P1 Fe1 S1 85.12(4) . . ? S2 Fe1 S1 80.45(4) 8_665 . ? C2 Fe1 Fe2 94.45(17) . . ? C1 Fe1 Fe2 151.21(17) . . ? P1 Fe1 Fe2 108.85(4) . . ? S2 Fe1 Fe2 55.71(3) 8_665 . ? S1 Fe1 Fe2 55.89(3) . . ? C3 Fe2 C4 97.3(2) . . ? C3 Fe2 P2 89.88(16) . . ? C4 Fe2 P2 96.40(16) . . ? C3 Fe2 S2 90.90(17) . 8_665 ? C4 Fe2 S2 105.52(16) . 8_665 ? P2 Fe2 S2 157.77(5) . 8_665 ? C3 Fe2 S1 159.65(18) . . ? C4 Fe2 S1 102.69(16) . . ? P2 Fe2 S1 91.64(5) . . ? S2 Fe2 S1 80.18(4) 8_665 . ? C3 Fe2 Fe1 104.27(17) . . ? C4 Fe2 Fe1 150.87(15) . . ? P2 Fe2 Fe1 102.90(4) . . ? S2 Fe2 Fe1 55.48(3) 8_665 . ? S1 Fe2 Fe1 55.66(3) . . ? C5 S1 Fe1 112.82(15) . . ? C5 S1 Fe2 112.75(17) . . ? Fe1 S1 Fe2 68.45(4) . . ? C8 S2 Fe1 115.73(18) . 8_665 ? C8 S2 Fe2 114.26(16) . 8_665 ? Fe1 S2 Fe2 68.81(4) 8_665 8_665 ? C14 P1 C12 102.6(2) . . ? C14 P1 C20 102.4(2) . . ? C12 P1 C20 102.5(2) . . ? C14 P1 Fe1 114.63(16) . . ? C12 P1 Fe1 115.58(15) . . ? C20 P1 Fe1 117.14(15) . . ? C26 P2 C32 100.4(2) . . ? C26 P2 C13 104.7(2) . . ? C32 P2 C13 100.9(2) . . ? C26 P2 Fe2 111.20(16) . . ? C32 P2 Fe2 119.95(15) . . ? C13 P2 Fe2 117.36(15) . . ? O1 C1 Fe1 178.7(5) . . ? O2 C2 Fe1 177.6(5) . . ? O3 C3 Fe2 177.7(5) . . ? O4 C4 Fe2 179.5(5) . . ? C6 C5 S1 111.7(3) . . ? N1 C6 C5 111.3(4) . . ? N1 C7 C8 112.7(4) . . ? C7 C8 S2 111.0(3) . . ? N1 C9 C11 113.5(5) . . ? N1 C9 C10 110.1(5) . . ? C11 C9 C10 112.3(6) . . ? C13 C12 P1 112.5(3) . . ? C12 C13 P2 112.1(3) . . ? C15 C14 C19 118.3(4) . . ? C15 C14 P1 121.8(4) . . ? C19 C14 P1 119.9(4) . . ? C14 C15 C16 119.1(5) . . ? C17 C16 C15 122.2(6) . . ? C16 C17 C18 118.9(5) . . ? C19 C18 C17 121.8(6) . . ? C18 C19 C14 119.6(5) . . ? C25 C20 C21 117.8(5) . . ? C25 C20 P1 118.5(4) . . ? C21 C20 P1 123.6(4) . . ? C20 C21 C22 120.5(5) . . ? C23 C22 C21 120.9(6) . . ? C22 C23 C24 118.9(5) . . ? C23 C24 C25 121.3(5) . . ? C20 C25 C24 120.5(5) . . ? C27 C26 C31 117.5(5) . . ? C27 C26 P2 119.4(4) . . ? C31 C26 P2 122.5(4) . . ? C26 C27 C28 121.6(6) . . ? C29 C28 C27 119.2(6) . . ? C30 C29 C28 121.1(6) . . ? C29 C30 C31 120.7(6) . . ? C30 C31 C26 119.7(6) . . ? C33 C32 C37 118.1(4) . . ? C33 C32 P2 122.6(4) . . ? C37 C32 P2 119.1(4) . . ? C32 C33 C34 120.1(5) . . ? C35 C34 C33 120.7(6) . . ? C36 C35 C34 120.2(6) . . ? C35 C36 C37 121.4(6) . . ? C36 C37 C32 119.4(5) . . ? C6 N1 C7 113.6(4) . . ? C6 N1 C9 115.6(4) . . ? C7 N1 C9 112.4(4) . . ? C38 O5 C38 105.9(11) 8_665 . ? O5 C38 C39 111.1(9) . . ? C39 C39 C38 106.0(4) 8_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.138 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.105 # Attachment '- complex_7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 793187' #TrackingRef '- complex_7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H106 Fe4 N2 O12 P4 S4' _chemical_formula_weight 1859.27 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' P P 0.1023 0.0942 '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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 37.7214(7) _cell_length_b 13.5805(3) _cell_length_c 21.1039(4) _cell_angle_alpha 90.00 _cell_angle_beta 123.2606(12) _cell_angle_gamma 90.00 _cell_volume 9040.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30121 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 27.50 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30121 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18044 _reflns_number_gt 12807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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. ; _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^)+(0.0601P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(12) _refine_ls_number_reflns 18044 _refine_ls_number_parameters 931 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.009 _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 0.49000(2) -0.04326(5) 0.98146(4) 0.02631(17) Uani 1 1 d . . . Fe2 Fe 0.47870(2) -0.05790(5) 0.85235(4) 0.02764(17) Uani 1 1 d . . . Fe3 Fe 0.25790(2) -0.01705(6) 0.80477(4) 0.02845(17) Uani 1 1 d . . . Fe4 Fe 0.30170(2) 0.13444(5) 0.86942(4) 0.02982(17) Uani 1 1 d . . . S1 S 0.47565(4) 0.08628(9) 0.90310(7) 0.0286(3) Uani 1 1 d . . . S2 S 0.31207(4) 0.03369(10) 0.79614(7) 0.0315(3) Uani 1 1 d . . . S3 S 0.42919(4) -0.09631(10) 0.87642(7) 0.0290(3) Uani 1 1 d . . . S4 S 0.31077(4) -0.01014(10) 0.93005(7) 0.0307(3) Uani 1 1 d . . . P1 P 0.55809(4) -0.00503(10) 1.04522(7) 0.0271(3) Uani 1 1 d . . . P2 P 0.54366(4) -0.01379(10) 0.88840(7) 0.0278(3) Uani 1 1 d . . . P3 P 0.21342(4) 0.00028(10) 0.84250(7) 0.0282(3) Uani 1 1 d . . . P4 P 0.26639(4) 0.18650(10) 0.91845(8) 0.0295(3) Uani 1 1 d . . . C1 C 0.50427(16) -0.1632(4) 1.0169(3) 0.0344(13) Uani 1 1 d . . . C2 C 0.47485(17) 0.0052(4) 1.0422(3) 0.0354(13) Uani 1 1 d . . . C3 C 0.49249(17) -0.1817(4) 0.8549(3) 0.0345(13) Uani 1 1 d . . . C4 C 0.45078(17) -0.0346(5) 0.7537(3) 0.0389(14) Uani 1 1 d . . . C5 C 0.25300(18) -0.1420(4) 0.7796(3) 0.0368(13) Uani 1 1 d . . . C6 C 0.21983(18) 0.0349(4) 0.7173(3) 0.0360(13) Uani 1 1 d . . . C7 C 0.35020(19) 0.1980(5) 0.9265(4) 0.0422(14) Uani 1 1 d . . . C8 C 0.27661(18) 0.2229(4) 0.7976(3) 0.0379(13) Uani 1 1 d . . . C9 C 0.42131(16) 0.1309(4) 0.8626(3) 0.0325(12) Uani 1 1 d . . . H9A H 0.4028 0.0748 0.8562 0.039 Uiso 1 1 calc R . . H9B H 0.4211 0.1784 0.8980 0.039 Uiso 1 1 calc R . . C10 C 0.40387(16) 0.1804(4) 0.7865(3) 0.0370(13) Uani 1 1 d . . . H10A H 0.4176 0.2452 0.7940 0.044 Uiso 1 1 calc R . . H10B H 0.4100 0.1393 0.7548 0.044 Uiso 1 1 calc R . . C11 C 0.33477(19) 0.1073(4) 0.7016(3) 0.0391(14) Uani 1 1 d . . . H11A H 0.3541 0.0498 0.7198 0.047 Uiso 1 1 calc R . . H11B H 0.3256 0.1203 0.6486 0.047 Uiso 1 1 calc R . . C12 C 0.29599(18) 0.0822(4) 0.7035(3) 0.0366(13) Uani 1 1 d . . . H12A H 0.2785 0.0327 0.6639 0.044 Uiso 1 1 calc R . . H12B H 0.2785 0.1420 0.6925 0.044 Uiso 1 1 calc R . . C13 C 0.3417(2) 0.2871(5) 0.7088(3) 0.0469(15) Uani 1 1 d . . . H13 H 0.3101 0.2825 0.6798 0.056 Uiso 1 1 calc R . . C14 C 0.3546(2) 0.3699(5) 0.7658(4) 0.0575(18) Uani 1 1 d . . . H14A H 0.3436 0.3565 0.7976 0.086 Uiso 1 1 calc R . . H14B H 0.3428 0.4322 0.7388 0.086 Uiso 1 1 calc R . . H14C H 0.3855 0.3744 0.7977 0.086 Uiso 1 1 calc R . . C15 C 0.3530(2) 0.3101(5) 0.6509(4) 0.0546(17) Uani 1 1 d . . . H15A H 0.3837 0.3191 0.6773 0.082 Uiso 1 1 calc R . . H15B H 0.3385 0.3706 0.6235 0.082 Uiso 1 1 calc R . . H15C H 0.3440 0.2554 0.6149 0.082 Uiso 1 1 calc R . . C16 C 0.41746(17) -0.2277(4) 0.8716(3) 0.0339(13) Uani 1 1 d . . . H16A H 0.4092 -0.2541 0.8215 0.041 Uiso 1 1 calc R . . H16B H 0.4430 -0.2635 0.9111 0.041 Uiso 1 1 calc R . . C17 C 0.38157(17) -0.2436(4) 0.8833(3) 0.0369(13) Uani 1 1 d . . . H17A H 0.3578 -0.1990 0.8490 0.044 Uiso 1 1 calc R . . H17B H 0.3712 -0.3121 0.8693 0.044 Uiso 1 1 calc R . . C18 C 0.35973(18) -0.1806(4) 0.9641(3) 0.0360(13) Uani 1 1 d . . . H18A H 0.3633 -0.1957 1.0132 0.043 Uiso 1 1 calc R . . H18B H 0.3321 -0.2076 0.9230 0.043 Uiso 1 1 calc R . . C19 C 0.36051(16) -0.0703(4) 0.9548(3) 0.0333(13) Uani 1 1 d . . . H19A H 0.3658 -0.0565 0.9147 0.040 Uiso 1 1 calc R . . H19B H 0.3842 -0.0418 1.0027 0.040 Uiso 1 1 calc R . . C20 C 0.41416(19) -0.3116(4) 1.0101(3) 0.0441(15) Uani 1 1 d . . . H20 H 0.4333 -0.3414 0.9963 0.053 Uiso 1 1 calc R . . C21 C 0.4423(2) -0.2791(6) 1.0937(4) 0.064(2) Uani 1 1 d . . . H21A H 0.4633 -0.2312 1.0995 0.096 Uiso 1 1 calc R . . H21B H 0.4569 -0.3367 1.1257 0.096 Uiso 1 1 calc R . . H21C H 0.4246 -0.2490 1.1092 0.096 Uiso 1 1 calc R . . C22 C 0.3828(2) -0.3922(5) 1.0000(4) 0.0595(19) Uani 1 1 d . . . H22A H 0.3656 -0.3680 1.0186 0.089 Uiso 1 1 calc R . . H22B H 0.3985 -0.4509 1.0287 0.089 Uiso 1 1 calc R . . H22C H 0.3642 -0.4090 0.9461 0.089 Uiso 1 1 calc R . . C23 C 0.58076(17) -0.0399(4) 0.9905(3) 0.0316(12) Uani 1 1 d . . . H23A H 0.5876 -0.1110 0.9975 0.038 Uiso 1 1 calc R . . H23B H 0.6074 -0.0030 1.0097 0.038 Uiso 1 1 calc R . . C24 C 0.59196(16) -0.0710(4) 1.1348(3) 0.0289(11) Uani 1 1 d . . . C25 C 0.57992(19) -0.0722(4) 1.1869(3) 0.0405(14) Uani 1 1 d . . . H25 H 0.5543 -0.0407 1.1743 0.049 Uiso 1 1 calc R . . C26 C 0.60435(19) -0.1180(4) 1.2557(3) 0.0410(14) Uani 1 1 d . . . H26 H 0.5957 -0.1175 1.2903 0.049 Uiso 1 1 calc R . . C27 C 0.6415(2) -0.1649(4) 1.2750(3) 0.0431(14) Uani 1 1 d . . . H27 H 0.6584 -0.1967 1.3227 0.052 Uiso 1 1 calc R . . C28 C 0.65377(18) -0.1653(4) 1.2247(3) 0.0394(14) Uani 1 1 d . . . H28 H 0.6792 -0.1978 1.2378 0.047 Uiso 1 1 calc R . . C29 C 0.62925(16) -0.1183(4) 1.1542(3) 0.0328(12) Uani 1 1 d . . . H29 H 0.6381 -0.1189 1.1199 0.039 Uiso 1 1 calc R . . C30 C 0.57753(17) 0.1207(4) 1.0754(3) 0.0315(12) Uani 1 1 d . . . C31 C 0.62098(17) 0.1413(4) 1.1105(3) 0.0361(13) Uani 1 1 d . . . H31 H 0.6400 0.0896 1.1185 0.043 Uiso 1 1 calc R . . C32 C 0.63638(18) 0.2361(4) 1.1335(3) 0.0368(13) Uani 1 1 d . . . H32 H 0.6657 0.2497 1.1563 0.044 Uiso 1 1 calc R . . C33 C 0.6089(2) 0.3098(4) 1.1229(3) 0.0421(14) Uani 1 1 d . . . H33 H 0.6193 0.3751 1.1375 0.051 Uiso 1 1 calc R . . C34 C 0.56643(19) 0.2919(4) 1.0918(3) 0.0402(14) Uani 1 1 d . . . H34 H 0.5482 0.3434 1.0874 0.048 Uiso 1 1 calc R . . C35 C 0.55064(17) 0.1969(4) 1.0667(3) 0.0326(12) Uani 1 1 d . . . H35 H 0.5212 0.1843 1.0435 0.039 Uiso 1 1 calc R . . C36 C 0.55451(17) 0.1128(4) 0.8761(3) 0.0320(12) Uani 1 1 d . . . C37 C 0.5930(2) 0.1593(5) 0.9254(3) 0.0465(15) Uani 1 1 d . . . H37 H 0.6141 0.1256 0.9698 0.056 Uiso 1 1 calc R . . C38 C 0.6014(3) 0.2525(5) 0.9119(4) 0.0609(19) Uani 1 1 d . . . H38 H 0.6278 0.2832 0.9471 0.073 Uiso 1 1 calc R . . C39 C 0.5711(2) 0.3018(5) 0.8462(4) 0.0601(19) Uani 1 1 d . . . H39 H 0.5769 0.3658 0.8359 0.072 Uiso 1 1 calc R . . C40 C 0.5327(2) 0.2580(5) 0.7963(4) 0.0590(18) Uani 1 1 d . . . H40 H 0.5118 0.2919 0.7518 0.071 Uiso 1 1 calc R . . C41 C 0.52460(19) 0.1638(5) 0.8111(3) 0.0450(15) Uani 1 1 d . . . H41 H 0.4981 0.1337 0.7762 0.054 Uiso 1 1 calc R . . C42 C 0.56857(17) -0.0807(4) 0.8472(3) 0.0356(13) Uani 1 1 d . . . C43 C 0.6118(2) -0.0908(6) 0.8842(4) 0.059(2) Uani 1 1 d . . . H43 H 0.6296 -0.0636 0.9334 0.070 Uiso 1 1 calc R . . C44 C 0.6298(2) -0.1403(6) 0.8508(4) 0.071(2) Uani 1 1 d . . . H44 H 0.6597 -0.1462 0.8770 0.086 Uiso 1 1 calc R . . C45 C 0.6039(2) -0.1809(5) 0.7793(4) 0.0582(19) Uani 1 1 d . . . H45 H 0.6160 -0.2153 0.7564 0.070 Uiso 1 1 calc R . . C46 C 0.5614(2) -0.1713(5) 0.7422(4) 0.0566(18) Uani 1 1 d . . . H46 H 0.5437 -0.1988 0.6930 0.068 Uiso 1 1 calc R . . C47 C 0.5434(2) -0.1216(5) 0.7753(3) 0.0456(15) Uani 1 1 d . . . H47 H 0.5134 -0.1154 0.7485 0.055 Uiso 1 1 calc R . . C48 C 0.21437(16) 0.1281(4) 0.8719(3) 0.0316(12) Uani 1 1 d . . . H48A H 0.1940 0.1673 0.8267 0.038 Uiso 1 1 calc R . . H48B H 0.2046 0.1293 0.9069 0.038 Uiso 1 1 calc R . . C49 C 0.22078(16) -0.0783(4) 0.9200(3) 0.0332(12) Uani 1 1 d . . . C50 C 0.20556(18) -0.0509(4) 0.9636(3) 0.0390(13) Uani 1 1 d . . . H50 H 0.1933 0.0123 0.9573 0.047 Uiso 1 1 calc R . . C51 C 0.20822(19) -0.1171(5) 1.0175(3) 0.0493(16) Uani 1 1 d . . . H51 H 0.1975 -0.0989 1.0473 0.059 Uiso 1 1 calc R . . C52 C 0.22663(19) -0.2089(5) 1.0269(3) 0.0448(15) Uani 1 1 d . . . H52 H 0.2286 -0.2537 1.0633 0.054 Uiso 1 1 calc R . . C53 C 0.2419(2) -0.2346(5) 0.9834(3) 0.0470(16) Uani 1 1 d . . . H53 H 0.2539 -0.2982 0.9893 0.056 Uiso 1 1 calc R . . C54 C 0.24027(17) -0.1704(4) 0.9312(3) 0.0368(13) Uani 1 1 d . . . H54 H 0.2522 -0.1883 0.9032 0.044 Uiso 1 1 calc R . . C55 C 0.15653(16) -0.0174(4) 0.7743(3) 0.0305(12) Uani 1 1 d . . . C56 C 0.12656(18) 0.0332(5) 0.7810(3) 0.0415(14) Uani 1 1 d . . . H56 H 0.1356 0.0811 0.8197 0.050 Uiso 1 1 calc R . . C57 C 0.08325(18) 0.0137(5) 0.7310(3) 0.0478(16) Uani 1 1 d . . . H57 H 0.0631 0.0495 0.7355 0.057 Uiso 1 1 calc R . . C58 C 0.06971(19) -0.0557(5) 0.6762(4) 0.0474(16) Uani 1 1 d . . . H58 H 0.0403 -0.0694 0.6430 0.057 Uiso 1 1 calc R . . C59 C 0.0992(2) -0.1062(5) 0.6693(4) 0.0528(17) Uani 1 1 d . . . H59 H 0.0900 -0.1548 0.6310 0.063 Uiso 1 1 calc R . . C60 C 0.14237(19) -0.0866(4) 0.7180(3) 0.0434(14) Uani 1 1 d . . . H60 H 0.1622 -0.1216 0.7122 0.052 Uiso 1 1 calc R . . C61 C 0.28682(17) 0.1738(4) 1.0188(3) 0.0355(13) Uani 1 1 d . . . C62 C 0.32932(19) 0.1508(5) 1.0721(3) 0.0434(14) Uani 1 1 d . . . H62 H 0.3478 0.1376 1.0558 0.052 Uiso 1 1 calc R . . C63 C 0.3447(2) 0.1472(5) 1.1496(3) 0.0546(17) Uani 1 1 d . . . H63 H 0.3737 0.1321 1.1855 0.065 Uiso 1 1 calc R . . C64 C 0.3185(2) 0.1649(5) 1.1732(4) 0.0555(18) Uani 1 1 d . . . H64 H 0.3290 0.1617 1.2257 0.067 Uiso 1 1 calc R . . C65 C 0.2771(2) 0.1875(5) 1.1219(4) 0.0566(18) Uani 1 1 d . . . H65 H 0.2588 0.1993 1.1391 0.068 Uiso 1 1 calc R . . C66 C 0.26099(19) 0.1935(5) 1.0451(3) 0.0427(15) Uani 1 1 d . . . H66 H 0.2322 0.2112 1.0103 0.051 Uiso 1 1 calc R . . C67 C 0.25439(17) 0.3181(4) 0.9043(3) 0.0339(13) Uani 1 1 d . . . C68 C 0.2849(2) 0.3839(4) 0.9578(4) 0.0476(15) Uani 1 1 d . . . H68 H 0.3097 0.3597 1.0024 0.057 Uiso 1 1 calc R . . C69 C 0.2785(2) 0.4851(5) 0.9449(4) 0.0563(18) Uani 1 1 d . . . H69 H 0.2988 0.5297 0.9816 0.068 Uiso 1 1 calc R . . C70 C 0.2439(3) 0.5209(5) 0.8809(4) 0.0559(18) Uani 1 1 d . . . H70 H 0.2402 0.5899 0.8722 0.067 Uiso 1 1 calc R . . C71 C 0.2138(2) 0.4561(5) 0.8285(4) 0.0533(17) Uani 1 1 d . . . H71 H 0.1890 0.4805 0.7842 0.064 Uiso 1 1 calc R . . C72 C 0.21981(19) 0.3558(4) 0.8403(3) 0.0409(14) Uani 1 1 d . . . H72 H 0.1993 0.3121 0.8029 0.049 Uiso 1 1 calc R . . N1 N 0.35808(13) 0.1933(3) 0.7482(2) 0.0337(10) Uani 1 1 d . . . N2 N 0.39412(13) -0.2256(3) 0.9612(2) 0.0300(10) Uani 1 1 d . . . O1 O 0.51426(13) -0.2427(3) 1.0399(3) 0.0509(11) Uani 1 1 d . . . O2 O 0.46567(14) 0.0371(4) 1.0812(3) 0.0573(12) Uani 1 1 d . . . O3 O 0.50149(16) -0.2630(3) 0.8584(3) 0.0597(13) Uani 1 1 d . . . O4 O 0.43221(15) -0.0195(4) 0.6885(2) 0.0609(13) Uani 1 1 d . . . O5 O 0.24924(14) -0.2231(3) 0.7591(3) 0.0504(11) Uani 1 1 d . . . O6 O 0.19488(13) 0.0701(3) 0.6589(2) 0.0493(11) Uani 1 1 d . . . O7 O 0.38110(15) 0.2405(4) 0.9627(3) 0.0703(15) Uani 1 1 d . . . O8 O 0.26028(15) 0.2808(3) 0.7489(3) 0.0538(12) Uani 1 1 d . . . O9 O 0.4758(3) 0.4425(8) 0.1542(6) 0.153(3) Uiso 1 1 d . . . C73 C 0.4604(5) 0.3418(12) 0.1256(10) 0.177(6) Uiso 1 1 d . . . H73A H 0.4833 0.2924 0.1521 0.213 Uiso 1 1 calc R . . H73B H 0.4475 0.3371 0.0703 0.213 Uiso 1 1 calc R . . C74 C 0.4252(5) 0.3296(10) 0.1466(9) 0.156(5) Uiso 1 1 d D . . H74A H 0.3967 0.3244 0.0994 0.187 Uiso 1 1 calc R . . H74B H 0.4308 0.2684 0.1761 0.187 Uiso 1 1 calc R . . C75 C 0.4263(5) 0.4099(11) 0.1888(9) 0.170(6) Uiso 1 1 d D . . H75A H 0.4270 0.3889 0.2344 0.204 Uiso 1 1 calc R . . H75B H 0.4020 0.4548 0.1581 0.204 Uiso 1 1 calc R . . C76 C 0.4685(4) 0.4567(10) 0.2094(8) 0.140(5) Uiso 1 1 d . . . H76A H 0.4677 0.5283 0.2177 0.167 Uiso 1 1 calc R . . H76B H 0.4920 0.4276 0.2573 0.167 Uiso 1 1 calc R . . O10 O 0.46844(18) 0.6401(4) 0.4384(3) 0.0828(16) Uiso 1 1 d . . . C77 C 0.4911(3) 0.6337(6) 0.4021(5) 0.079(2) Uiso 1 1 d . . . H77A H 0.5117 0.6885 0.4186 0.095 Uiso 1 1 calc R . . H77B H 0.4713 0.6369 0.3464 0.095 Uiso 1 1 calc R . . C78 C 0.5132(4) 0.5389(9) 0.4246(7) 0.127(4) Uiso 1 1 d . . . H78A H 0.5174 0.5128 0.3853 0.152 Uiso 1 1 calc R . . H78B H 0.5411 0.5440 0.4733 0.152 Uiso 1 1 calc R . . C79 C 0.4837(5) 0.4790(10) 0.4318(9) 0.147(5) Uiso 1 1 d . . . H79A H 0.4630 0.4475 0.3826 0.177 Uiso 1 1 calc R . . H79B H 0.4993 0.4264 0.4697 0.177 Uiso 1 1 calc R . . C80 C 0.4621(4) 0.5396(8) 0.4547(7) 0.110(3) Uiso 1 1 d . . . H80A H 0.4741 0.5313 0.5095 0.132 Uiso 1 1 calc R . . H80B H 0.4315 0.5231 0.4260 0.132 Uiso 1 1 calc R . . O11 O 0.1895(2) 0.4781(4) 0.0749(4) 0.0900(18) Uiso 1 1 d . . . C81 C 0.2207(5) 0.4673(13) 0.1559(9) 0.175(6) Uiso 1 1 d . . . H81A H 0.2190 0.5251 0.1827 0.210 Uiso 1 1 calc R . . H81B H 0.2139 0.4080 0.1744 0.210 Uiso 1 1 calc R . . C82 C 0.2628(3) 0.4590(8) 0.1736(6) 0.097(3) Uiso 1 1 d . . . H82A H 0.2728 0.3900 0.1860 0.117 Uiso 1 1 calc R . . H82B H 0.2824 0.5014 0.2173 0.117 Uiso 1 1 calc R . . C83 C 0.2601(4) 0.4913(9) 0.1056(7) 0.115(4) Uiso 1 1 d . . . H83A H 0.2703 0.5600 0.1119 0.139 Uiso 1 1 calc R . . H83B H 0.2782 0.4491 0.0962 0.139 Uiso 1 1 calc R . . C84 C 0.2169(4) 0.4852(9) 0.0428(7) 0.122(4) Uiso 1 1 d . . . H84A H 0.2127 0.4263 0.0117 0.147 Uiso 1 1 calc R . . H84B H 0.2091 0.5443 0.0104 0.147 Uiso 1 1 calc R . . O12 O 0.1479(2) 0.8545(5) 0.4551(4) 0.102(2) Uiso 1 1 d . . . C85 C 0.1051(5) 0.8881(12) 0.4247(9) 0.169(6) Uiso 1 1 d . . . H85A H 0.0840 0.8356 0.3957 0.203 Uiso 1 1 calc R . . H85B H 0.0981 0.9468 0.3920 0.203 Uiso 1 1 calc R . . C86 C 0.1079(8) 0.9133(17) 0.4989(13) 0.248(10) Uiso 1 1 d . . . H86A H 0.1197 0.9800 0.5174 0.298 Uiso 1 1 calc R . . H86B H 0.0798 0.9088 0.4921 0.298 Uiso 1 1 calc R . . C87 C 0.1357(6) 0.8395(16) 0.5485(12) 0.227(9) Uiso 1 1 d D . . H87A H 0.1509 0.8605 0.6021 0.273 Uiso 1 1 calc R . . H87B H 0.1206 0.7769 0.5421 0.273 Uiso 1 1 calc R . . C88 C 0.1630(5) 0.8317(13) 0.5231(10) 0.186(7) Uiso 1 1 d D . . H88A H 0.1880 0.8740 0.5557 0.223 Uiso 1 1 calc R . . H88B H 0.1732 0.7629 0.5308 0.223 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 Fe1 0.0240(4) 0.0305(4) 0.0262(4) 0.0004(3) 0.0149(3) 0.0009(3) Fe2 0.0260(4) 0.0326(4) 0.0274(4) -0.0022(3) 0.0167(3) -0.0011(3) Fe3 0.0257(4) 0.0348(4) 0.0272(4) 0.0001(3) 0.0160(3) 0.0021(3) Fe4 0.0276(4) 0.0351(4) 0.0306(4) 0.0000(3) 0.0184(3) 0.0012(3) S1 0.0259(7) 0.0314(7) 0.0297(7) 0.0002(6) 0.0160(6) 0.0008(5) S2 0.0313(7) 0.0375(8) 0.0312(7) 0.0001(6) 0.0206(6) 0.0036(6) S3 0.0249(7) 0.0332(7) 0.0310(7) 0.0006(6) 0.0167(6) -0.0009(5) S4 0.0259(7) 0.0373(8) 0.0295(7) -0.0005(6) 0.0157(6) 0.0031(6) P1 0.0247(7) 0.0317(7) 0.0264(7) -0.0010(6) 0.0151(6) 0.0003(5) P2 0.0271(7) 0.0319(8) 0.0280(7) -0.0014(6) 0.0174(6) 0.0000(6) P3 0.0240(7) 0.0343(8) 0.0277(7) -0.0003(6) 0.0150(6) -0.0001(6) P4 0.0266(7) 0.0331(8) 0.0300(7) -0.0013(6) 0.0163(6) 0.0011(6) C1 0.018(3) 0.040(3) 0.039(3) -0.004(3) 0.012(2) -0.006(2) C2 0.022(3) 0.050(4) 0.034(3) 0.000(3) 0.015(3) -0.003(2) C3 0.039(3) 0.030(3) 0.047(3) -0.002(3) 0.031(3) 0.003(2) C4 0.024(3) 0.057(4) 0.039(4) -0.001(3) 0.019(3) -0.002(3) C5 0.036(3) 0.042(4) 0.031(3) 0.004(3) 0.017(3) 0.002(3) C6 0.033(3) 0.044(3) 0.041(3) -0.001(3) 0.027(3) 0.004(3) C7 0.035(3) 0.053(4) 0.048(4) -0.007(3) 0.028(3) -0.003(3) C8 0.041(3) 0.039(3) 0.045(3) 0.001(3) 0.030(3) 0.006(3) C9 0.030(3) 0.034(3) 0.039(3) 0.002(2) 0.023(3) 0.007(2) C10 0.029(3) 0.047(3) 0.035(3) 0.012(3) 0.018(3) 0.004(3) C11 0.045(4) 0.041(3) 0.042(3) 0.003(3) 0.031(3) 0.002(3) C12 0.041(3) 0.042(3) 0.029(3) -0.003(2) 0.021(3) 0.002(3) C13 0.039(3) 0.055(4) 0.043(4) 0.015(3) 0.020(3) 0.013(3) C14 0.048(4) 0.051(4) 0.071(5) 0.008(4) 0.031(4) 0.014(3) C15 0.055(4) 0.055(4) 0.057(4) 0.020(3) 0.033(4) 0.006(3) C16 0.034(3) 0.038(3) 0.032(3) -0.009(2) 0.020(3) -0.010(2) C17 0.034(3) 0.038(3) 0.042(3) -0.002(3) 0.023(3) 0.000(2) C18 0.036(3) 0.034(3) 0.043(3) 0.006(3) 0.024(3) 0.005(2) C19 0.025(3) 0.037(3) 0.042(3) 0.005(3) 0.021(3) 0.003(2) C20 0.047(4) 0.043(4) 0.044(3) 0.014(3) 0.027(3) 0.013(3) C21 0.051(4) 0.086(6) 0.049(4) 0.022(4) 0.023(4) 0.016(4) C22 0.074(5) 0.042(4) 0.077(5) 0.021(4) 0.051(4) 0.007(3) C23 0.030(3) 0.038(3) 0.031(3) -0.002(2) 0.019(3) -0.002(2) C24 0.030(3) 0.028(3) 0.023(3) -0.005(2) 0.012(2) -0.001(2) C25 0.041(3) 0.048(4) 0.038(3) 0.007(3) 0.025(3) 0.008(3) C26 0.044(4) 0.053(4) 0.029(3) 0.006(3) 0.022(3) 0.004(3) C27 0.050(4) 0.040(3) 0.032(3) 0.009(3) 0.018(3) 0.005(3) C28 0.031(3) 0.041(3) 0.040(3) 0.007(3) 0.016(3) 0.006(3) C29 0.034(3) 0.030(3) 0.037(3) -0.002(2) 0.022(3) -0.002(2) C30 0.038(3) 0.034(3) 0.025(3) 0.002(2) 0.019(3) 0.000(2) C31 0.030(3) 0.042(3) 0.034(3) 0.001(3) 0.016(3) 0.003(2) C32 0.033(3) 0.041(3) 0.030(3) -0.005(3) 0.013(3) -0.007(3) C33 0.057(4) 0.039(3) 0.029(3) -0.006(3) 0.023(3) -0.013(3) C34 0.044(4) 0.038(3) 0.035(3) 0.001(3) 0.020(3) 0.004(3) C35 0.032(3) 0.034(3) 0.028(3) -0.004(2) 0.014(3) 0.000(2) C36 0.035(3) 0.034(3) 0.042(3) -0.003(2) 0.030(3) -0.005(2) C37 0.054(4) 0.051(4) 0.033(3) 0.000(3) 0.024(3) -0.015(3) C38 0.076(5) 0.056(4) 0.048(4) -0.010(4) 0.032(4) -0.030(4) C39 0.077(5) 0.042(4) 0.065(5) -0.007(3) 0.041(4) -0.024(4) C40 0.061(5) 0.049(4) 0.062(4) 0.027(4) 0.030(4) 0.006(3) C41 0.035(3) 0.049(4) 0.045(4) 0.002(3) 0.018(3) -0.002(3) C42 0.034(3) 0.044(3) 0.038(3) 0.004(3) 0.026(3) 0.002(3) C43 0.033(4) 0.103(6) 0.041(4) -0.020(4) 0.020(3) 0.006(4) C44 0.039(4) 0.133(7) 0.046(4) -0.018(4) 0.026(3) 0.020(4) C45 0.065(5) 0.071(5) 0.061(4) -0.001(4) 0.048(4) 0.015(4) C46 0.060(5) 0.081(5) 0.045(4) -0.016(4) 0.040(4) -0.003(4) C47 0.047(4) 0.059(4) 0.038(3) -0.017(3) 0.027(3) -0.006(3) C48 0.028(3) 0.035(3) 0.036(3) 0.002(2) 0.020(3) -0.001(2) C49 0.025(3) 0.046(3) 0.025(3) -0.001(2) 0.011(2) -0.011(2) C50 0.041(3) 0.047(4) 0.035(3) 0.003(3) 0.025(3) 0.002(3) C51 0.040(4) 0.070(5) 0.038(3) -0.005(3) 0.021(3) -0.013(3) C52 0.046(4) 0.051(4) 0.028(3) 0.013(3) 0.014(3) -0.002(3) C53 0.060(4) 0.041(4) 0.036(3) 0.004(3) 0.024(3) -0.003(3) C54 0.033(3) 0.041(3) 0.037(3) -0.001(3) 0.019(3) -0.001(3) C55 0.030(3) 0.029(3) 0.032(3) 0.007(2) 0.017(3) -0.001(2) C56 0.028(3) 0.054(4) 0.041(3) -0.004(3) 0.019(3) -0.002(3) C57 0.027(3) 0.072(5) 0.041(4) 0.008(3) 0.016(3) 0.004(3) C58 0.030(3) 0.062(4) 0.039(3) 0.010(3) 0.012(3) -0.009(3) C59 0.040(4) 0.048(4) 0.056(4) -0.009(3) 0.016(3) -0.010(3) C60 0.037(3) 0.044(4) 0.040(3) -0.003(3) 0.015(3) 0.000(3) C61 0.035(3) 0.039(3) 0.031(3) -0.007(2) 0.018(3) 0.000(2) C62 0.039(3) 0.055(4) 0.029(3) 0.004(3) 0.014(3) 0.008(3) C63 0.052(4) 0.062(4) 0.031(3) 0.002(3) 0.011(3) 0.009(3) C64 0.072(5) 0.060(4) 0.032(3) 0.000(3) 0.027(4) -0.007(4) C65 0.066(5) 0.078(5) 0.036(4) -0.006(3) 0.034(4) 0.002(4) C66 0.044(4) 0.057(4) 0.030(3) 0.000(3) 0.023(3) 0.007(3) C67 0.037(3) 0.038(3) 0.035(3) -0.006(2) 0.025(3) -0.004(2) C68 0.041(4) 0.033(3) 0.051(4) -0.001(3) 0.014(3) -0.005(3) C69 0.065(5) 0.044(4) 0.053(4) -0.007(3) 0.028(4) -0.008(3) C70 0.090(6) 0.027(3) 0.063(5) 0.001(3) 0.050(5) 0.002(3) C71 0.053(4) 0.054(4) 0.044(4) 0.008(3) 0.021(3) 0.016(3) C72 0.042(3) 0.029(3) 0.042(3) -0.003(3) 0.017(3) 0.001(3) N1 0.025(2) 0.039(3) 0.032(2) 0.008(2) 0.012(2) 0.005(2) N2 0.028(2) 0.033(2) 0.029(2) 0.0046(19) 0.015(2) 0.0001(19) O1 0.039(2) 0.033(2) 0.061(3) 0.009(2) 0.015(2) 0.0035(19) O2 0.047(3) 0.088(4) 0.048(3) -0.020(2) 0.033(2) -0.004(2) O3 0.073(3) 0.037(3) 0.097(4) -0.001(3) 0.065(3) 0.001(2) O4 0.046(3) 0.101(4) 0.037(3) 0.003(3) 0.023(2) 0.004(3) O5 0.053(3) 0.043(3) 0.061(3) -0.009(2) 0.035(2) -0.004(2) O6 0.040(2) 0.069(3) 0.041(3) 0.017(2) 0.023(2) 0.015(2) O7 0.055(3) 0.097(4) 0.069(3) -0.041(3) 0.041(3) -0.029(3) O8 0.075(3) 0.046(3) 0.060(3) 0.015(2) 0.050(3) 0.019(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 Fe1 C1 1.750(6) . ? Fe1 C2 1.791(6) . ? Fe1 P1 2.2105(15) . ? Fe1 S3 2.2622(15) . ? Fe1 S1 2.2674(15) . ? Fe1 Fe2 2.5242(9) . ? Fe2 C3 1.752(6) . ? Fe2 C4 1.772(6) . ? Fe2 P2 2.2128(15) . ? Fe2 S3 2.2490(14) . ? Fe2 S1 2.2647(15) . ? Fe3 C6 1.750(6) . ? Fe3 C5 1.757(6) . ? Fe3 P3 2.2291(14) . ? Fe3 S2 2.2565(14) . ? Fe3 S4 2.2787(15) . ? Fe3 Fe4 2.5202(11) . ? Fe4 C8 1.750(6) . ? Fe4 C7 1.768(6) . ? Fe4 P4 2.2038(15) . ? Fe4 S2 2.2540(15) . ? Fe4 S4 2.2648(15) . ? S1 C9 1.838(5) . ? S2 C12 1.823(5) . ? S3 C16 1.828(5) . ? S4 C19 1.840(5) . ? P1 C30 1.830(5) . ? P1 C24 1.833(5) . ? P1 C23 1.837(5) . ? P2 C36 1.819(5) . ? P2 C42 1.833(5) . ? P2 C23 1.849(5) . ? P3 C55 1.829(5) . ? P3 C48 1.838(5) . ? P3 C49 1.841(5) . ? P4 C61 1.821(5) . ? P4 C48 1.825(5) . ? P4 C67 1.828(6) . ? C1 O1 1.159(7) . ? C2 O2 1.139(7) . ? C3 O3 1.145(6) . ? C4 O4 1.169(7) . ? C5 O5 1.164(7) . ? C6 O6 1.165(7) . ? C7 O7 1.139(7) . ? C8 O8 1.167(7) . ? C9 C10 1.518(7) . ? C10 N1 1.462(7) . ? C11 N1 1.468(7) . ? C11 C12 1.524(7) . ? C13 N1 1.459(7) . ? C13 C14 1.519(9) . ? C13 C15 1.531(9) . ? C16 C17 1.519(7) . ? C17 N2 1.461(7) . ? C18 N2 1.465(7) . ? C18 C19 1.512(7) . ? C20 N2 1.464(7) . ? C20 C22 1.539(9) . ? C20 C21 1.543(9) . ? C24 C29 1.388(7) . ? C24 C25 1.401(7) . ? C25 C26 1.370(8) . ? C26 C27 1.381(8) . ? C27 C28 1.372(8) . ? C28 C29 1.402(8) . ? C30 C35 1.388(7) . ? C30 C31 1.408(7) . ? C31 C32 1.385(8) . ? C32 C33 1.370(8) . ? C33 C34 1.379(8) . ? C34 C35 1.398(8) . ? C36 C37 1.391(8) . ? C36 C41 1.391(8) . ? C37 C38 1.373(8) . ? C38 C39 1.393(10) . ? C39 C40 1.372(10) . ? C40 C41 1.391(9) . ? C42 C43 1.374(8) . ? C42 C47 1.391(8) . ? C43 C44 1.391(8) . ? C44 C45 1.385(10) . ? C45 C46 1.350(9) . ? C46 C47 1.388(8) . ? C49 C50 1.376(7) . ? C49 C54 1.404(8) . ? C50 C51 1.410(8) . ? C51 C52 1.387(9) . ? C52 C53 1.370(8) . ? C53 C54 1.380(8) . ? C55 C60 1.372(8) . ? C55 C56 1.395(8) . ? C56 C57 1.400(8) . ? C57 C58 1.356(9) . ? C58 C59 1.381(9) . ? C59 C60 1.394(8) . ? C61 C66 1.386(7) . ? C61 C62 1.398(8) . ? C62 C63 1.404(8) . ? C63 C64 1.352(9) . ? C64 C65 1.361(9) . ? C65 C66 1.389(8) . ? C67 C72 1.362(8) . ? C67 C68 1.405(8) . ? C68 C69 1.397(9) . ? C69 C70 1.353(10) . ? C70 C71 1.382(10) . ? C71 C72 1.380(8) . ? O9 C76 1.349(14) . ? O9 C73 1.479(15) . ? C73 C74 1.619(18) . ? C74 C75 1.394(9) . ? C75 C76 1.537(18) . ? O10 C77 1.429(9) . ? O10 C80 1.460(11) . ? C77 C78 1.464(13) . ? C78 C79 1.453(16) . ? C79 C80 1.418(16) . ? O11 C81 1.457(16) . ? O11 C84 1.514(13) . ? C81 C82 1.420(17) . ? C82 C83 1.452(14) . ? C83 C84 1.434(14) . ? O12 C88 1.258(17) . ? O12 C85 1.447(15) . ? C85 C86 1.55(2) . ? C86 C87 1.41(2) . ? C87 C88 1.402(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C2 100.4(3) . . ? C1 Fe1 P1 88.63(17) . . ? C2 Fe1 P1 101.44(18) . . ? C1 Fe1 S3 91.78(18) . . ? C2 Fe1 S3 105.58(18) . . ? P1 Fe1 S3 152.43(6) . . ? C1 Fe1 S1 158.20(19) . . ? C2 Fe1 S1 101.25(19) . . ? P1 Fe1 S1 89.69(5) . . ? S3 Fe1 S1 79.88(5) . . ? C1 Fe1 Fe2 102.60(19) . . ? C2 Fe1 Fe2 150.53(18) . . ? P1 Fe1 Fe2 97.32(4) . . ? S3 Fe1 Fe2 55.73(4) . . ? S1 Fe1 Fe2 56.10(4) . . ? C3 Fe2 C4 100.5(3) . . ? C3 Fe2 P2 89.72(18) . . ? C4 Fe2 P2 100.83(18) . . ? C3 Fe2 S3 92.27(17) . . ? C4 Fe2 S3 105.96(17) . . ? P2 Fe2 S3 152.28(6) . . ? C3 Fe2 S1 155.00(19) . . ? C4 Fe2 S1 104.5(2) . . ? P2 Fe2 S1 86.40(5) . . ? S3 Fe2 S1 80.21(5) . . ? C3 Fe2 Fe1 99.83(18) . . ? C4 Fe2 Fe1 153.40(18) . . ? P2 Fe2 Fe1 96.20(5) . . ? S3 Fe2 Fe1 56.22(4) . . ? S1 Fe2 Fe1 56.21(4) . . ? C6 Fe3 C5 100.4(3) . . ? C6 Fe3 P3 89.51(17) . . ? C5 Fe3 P3 103.58(19) . . ? C6 Fe3 S2 92.70(18) . . ? C5 Fe3 S2 102.73(19) . . ? P3 Fe3 S2 152.73(6) . . ? C6 Fe3 S4 153.8(2) . . ? C5 Fe3 S4 105.69(18) . . ? P3 Fe3 S4 86.13(5) . . ? S2 Fe3 S4 79.98(5) . . ? C6 Fe3 Fe4 99.03(19) . . ? C5 Fe3 Fe4 151.76(19) . . ? P3 Fe3 Fe4 96.83(5) . . ? S2 Fe3 Fe4 55.98(4) . . ? S4 Fe3 Fe4 56.05(4) . . ? C8 Fe4 C7 96.9(3) . . ? C8 Fe4 P4 90.43(18) . . ? C7 Fe4 P4 100.94(18) . . ? C8 Fe4 S2 92.14(18) . . ? C7 Fe4 S2 105.04(19) . . ? P4 Fe4 S2 153.37(6) . . ? C8 Fe4 S4 157.9(2) . . ? C7 Fe4 S4 105.0(2) . . ? P4 Fe4 S4 87.46(5) . . ? S2 Fe4 S4 80.33(5) . . ? C8 Fe4 Fe3 102.1(2) . . ? C7 Fe4 Fe3 153.3(2) . . ? P4 Fe4 Fe3 97.50(5) . . ? S2 Fe4 Fe3 56.08(4) . . ? S4 Fe4 Fe3 56.58(4) . . ? C9 S1 Fe2 113.46(19) . . ? C9 S1 Fe1 110.74(18) . . ? Fe2 S1 Fe1 67.69(4) . . ? C12 S2 Fe4 115.82(19) . . ? C12 S2 Fe3 114.42(19) . . ? Fe4 S2 Fe3 67.94(4) . . ? C16 S3 Fe2 114.79(17) . . ? C16 S3 Fe1 116.75(19) . . ? Fe2 S3 Fe1 68.05(4) . . ? C19 S4 Fe4 111.11(18) . . ? C19 S4 Fe3 114.74(19) . . ? Fe4 S4 Fe3 67.38(5) . . ? C30 P1 C24 100.2(2) . . ? C30 P1 C23 102.9(2) . . ? C24 P1 C23 102.8(2) . . ? C30 P1 Fe1 122.76(18) . . ? C24 P1 Fe1 115.67(18) . . ? C23 P1 Fe1 110.06(18) . . ? C36 P2 C42 100.7(2) . . ? C36 P2 C23 105.2(3) . . ? C42 P2 C23 101.5(2) . . ? C36 P2 Fe2 120.02(18) . . ? C42 P2 Fe2 117.51(19) . . ? C23 P2 Fe2 109.68(17) . . ? C55 P3 C48 100.8(2) . . ? C55 P3 C49 99.4(2) . . ? C48 P3 C49 106.4(3) . . ? C55 P3 Fe3 119.53(18) . . ? C48 P3 Fe3 109.96(17) . . ? C49 P3 Fe3 118.66(19) . . ? C61 P4 C48 103.3(3) . . ? C61 P4 C67 101.1(2) . . ? C48 P4 C67 103.9(2) . . ? C61 P4 Fe4 122.43(18) . . ? C48 P4 Fe4 110.87(18) . . ? C67 P4 Fe4 113.32(17) . . ? O1 C1 Fe1 178.7(5) . . ? O2 C2 Fe1 178.9(5) . . ? O3 C3 Fe2 178.1(5) . . ? O4 C4 Fe2 179.7(6) . . ? O5 C5 Fe3 176.3(5) . . ? O6 C6 Fe3 179.1(5) . . ? O7 C7 Fe4 178.8(7) . . ? O8 C8 Fe4 178.5(5) . . ? C10 C9 S1 111.3(4) . . ? N1 C10 C9 109.4(4) . . ? N1 C11 C12 113.1(4) . . ? C11 C12 S2 110.4(4) . . ? N1 C13 C14 110.1(5) . . ? N1 C13 C15 114.6(5) . . ? C14 C13 C15 111.9(6) . . ? C17 C16 S3 109.8(4) . . ? N2 C17 C16 113.1(4) . . ? N2 C18 C19 109.1(4) . . ? C18 C19 S4 112.8(4) . . ? N2 C20 C22 114.1(5) . . ? N2 C20 C21 110.1(5) . . ? C22 C20 C21 110.9(5) . . ? P1 C23 P2 111.6(3) . . ? C29 C24 C25 118.4(5) . . ? C29 C24 P1 123.4(4) . . ? C25 C24 P1 118.2(4) . . ? C26 C25 C24 121.2(5) . . ? C25 C26 C27 120.4(5) . . ? C28 C27 C26 119.5(5) . . ? C27 C28 C29 120.9(5) . . ? C24 C29 C28 119.7(5) . . ? C35 C30 C31 118.5(5) . . ? C35 C30 P1 121.7(4) . . ? C31 C30 P1 119.8(4) . . ? C32 C31 C30 120.8(5) . . ? C33 C32 C31 119.2(5) . . ? C32 C33 C34 121.7(5) . . ? C33 C34 C35 119.1(5) . . ? C30 C35 C34 120.6(5) . . ? C37 C36 C41 117.4(5) . . ? C37 C36 P2 123.2(5) . . ? C41 C36 P2 119.2(4) . . ? C38 C37 C36 122.0(6) . . ? C37 C38 C39 119.5(7) . . ? C40 C39 C38 120.0(6) . . ? C39 C40 C41 119.7(6) . . ? C40 C41 C36 121.3(6) . . ? C43 C42 C47 117.9(5) . . ? C43 C42 P2 122.5(5) . . ? C47 C42 P2 119.6(4) . . ? C42 C43 C44 121.2(6) . . ? C45 C44 C43 119.7(6) . . ? C46 C45 C44 119.8(6) . . ? C45 C46 C47 120.6(6) . . ? C46 C47 C42 120.8(6) . . ? P4 C48 P3 114.1(3) . . ? C50 C49 C54 120.0(5) . . ? C50 C49 P3 121.5(5) . . ? C54 C49 P3 118.4(4) . . ? C49 C50 C51 119.7(6) . . ? C52 C51 C50 119.8(6) . . ? C53 C52 C51 119.7(6) . . ? C52 C53 C54 121.4(6) . . ? C53 C54 C49 119.3(5) . . ? C60 C55 C56 118.2(5) . . ? C60 C55 P3 120.2(4) . . ? C56 C55 P3 121.5(4) . . ? C55 C56 C57 120.4(6) . . ? C58 C57 C56 120.8(6) . . ? C57 C58 C59 119.1(6) . . ? C58 C59 C60 120.7(6) . . ? C55 C60 C59 120.8(6) . . ? C66 C61 C62 117.9(5) . . ? C66 C61 P4 120.3(4) . . ? C62 C61 P4 121.6(4) . . ? C61 C62 C63 120.3(6) . . ? C64 C63 C62 120.3(6) . . ? C63 C64 C65 120.0(6) . . ? C64 C65 C66 121.2(6) . . ? C61 C66 C65 120.2(6) . . ? C72 C67 C68 118.4(5) . . ? C72 C67 P4 123.1(4) . . ? C68 C67 P4 118.0(4) . . ? C69 C68 C67 119.4(6) . . ? C70 C69 C68 121.2(6) . . ? C69 C70 C71 119.3(6) . . ? C72 C71 C70 120.2(6) . . ? C67 C72 C71 121.5(6) . . ? C13 N1 C10 115.0(4) . . ? C13 N1 C11 113.7(4) . . ? C10 N1 C11 111.5(4) . . ? C17 N2 C20 112.6(4) . . ? C17 N2 C18 111.6(4) . . ? C20 N2 C18 115.5(4) . . ? C76 O9 C73 105.4(11) . . ? O9 C73 C74 100.3(11) . . ? C75 C74 C73 110.7(13) . . ? C74 C75 C76 99.6(12) . . ? O9 C76 C75 111.4(12) . . ? C77 O10 C80 107.1(7) . . ? O10 C77 C78 106.4(8) . . ? C79 C78 C77 101.1(11) . . ? C80 C79 C78 109.1(12) . . ? C79 C80 O10 105.2(10) . . ? C81 O11 C84 102.8(9) . . ? C82 C81 O11 112.6(12) . . ? C81 C82 C83 104.7(11) . . ? C84 C83 C82 108.8(10) . . ? C83 C84 O11 107.5(10) . . ? C88 O12 C85 106.4(11) . . ? O12 C85 C86 100.4(14) . . ? C87 C86 C85 101.7(18) . . ? C88 C87 C86 100.0(18) . . ? O12 C88 C87 116.7(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.890 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.150