data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '5(C10 H8 S8), (C15 Fe O15), 5(H2 O)' _chemical_formula_sum 'C65 H50 Fe O20 S40' _chemical_formula_weight 2489.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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' '-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 42.4125(5) _cell_length_b 11.2100(3) _cell_length_c 20.4336(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.8929(10) _cell_angle_gamma 90.00 _cell_volume 8812.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11460 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 28.283 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5064 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21290 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10937 _reflns_number_gt 6414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0564P)^2^+15.2680P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10937 _refine_ls_number_parameters 574 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 S1 S 0.75710(2) 0.13177(8) 0.43291(5) 0.0281(2) Uani 1 1 d . . . S2 S 0.76243(2) 0.37284(8) 0.38005(4) 0.02541(19) Uani 1 1 d . . . S3 S 0.67568(2) 0.12442(7) 0.32833(5) 0.02454(19) Uani 1 1 d . . . S4 S 0.67955(2) 0.36687(7) 0.27558(4) 0.02361(19) Uani 1 1 d . . . S5 S 0.83006(2) 0.11920(8) 0.53952(5) 0.0278(2) Uani 1 1 d . . . S6 S 0.83623(2) 0.40668(8) 0.47604(5) 0.0263(2) Uani 1 1 d . . . S7 S 0.59848(2) 0.11089(8) 0.25691(5) 0.0270(2) Uani 1 1 d . . . S8 S 0.60367(2) 0.39908(8) 0.19624(5) 0.0277(2) Uani 1 1 d . . . C1 C 0.73583(8) 0.2517(3) 0.37676(17) 0.0221(7) Uani 1 1 d . . . C2 C 0.70129(8) 0.2487(3) 0.33227(17) 0.0216(7) Uani 1 1 d . . . C3 C 0.79758(8) 0.2033(3) 0.47341(17) 0.0229(7) Uani 1 1 d . . . C4 C 0.79991(8) 0.3137(3) 0.44953(17) 0.0210(7) Uani 1 1 d . . . C5 C 0.63576(8) 0.1931(3) 0.27246(17) 0.0227(7) Uani 1 1 d . . . C6 C 0.63766(8) 0.3042(3) 0.24941(17) 0.0224(7) Uani 1 1 d . . . C7 C 0.86820(9) 0.1935(3) 0.54115(19) 0.0266(8) Uani 1 1 d . . . H7A H 0.8891 0.1594 0.5806 0.032 Uiso 1 1 calc R . . H7B H 0.8699 0.1777 0.4951 0.032 Uiso 1 1 calc R . . C8 C 0.86787(9) 0.3269(3) 0.55190(17) 0.0255(8) Uani 1 1 d . . . H8A H 0.8912 0.3589 0.5622 0.031 Uiso 1 1 calc R . . H8B H 0.8632 0.3424 0.5947 0.031 Uiso 1 1 calc R . . C9 C 0.56835(9) 0.2317(3) 0.2420(2) 0.0331(9) Uani 1 1 d . . . H9A H 0.5451 0.1987 0.2322 0.040 Uiso 1 1 calc R . . H9B H 0.5760 0.2808 0.2863 0.040 Uiso 1 1 calc R . . C10 C 0.56553(9) 0.3095(4) 0.1800(2) 0.0382(9) Uani 1 1 d . . . H10A H 0.5454 0.3635 0.1680 0.046 Uiso 1 1 calc R . . H10B H 0.5608 0.2583 0.1374 0.046 Uiso 1 1 calc R . . S9 S 0.77106(2) 0.13379(8) 0.24898(5) 0.0272(2) Uani 1 1 d . . . S10 S 0.77754(2) 0.37540(8) 0.20279(4) 0.02439(19) Uani 1 1 d . . . S11 S 0.68881(2) 0.13766(7) 0.15134(5) 0.02526(19) Uani 1 1 d . . . S12 S 0.69428(2) 0.37311(7) 0.09588(4) 0.02418(19) Uani 1 1 d . . . S13 S 0.84413(2) 0.10897(7) 0.35242(4) 0.02494(19) Uani 1 1 d . . . S14 S 0.85202(2) 0.40293(7) 0.29925(4) 0.02359(19) Uani 1 1 d . . . S15 S 0.61248(2) 0.11986(8) 0.07466(5) 0.0274(2) Uani 1 1 d . . . S16 S 0.61921(2) 0.40181(8) 0.00513(5) 0.0268(2) Uani 1 1 d . . . C11 C 0.75066(9) 0.2557(3) 0.19683(18) 0.0229(7) Uani 1 1 d . . . C12 C 0.71511(8) 0.2558(3) 0.15277(17) 0.0215(7) Uani 1 1 d . . . C13 C 0.81210(8) 0.1991(3) 0.28965(17) 0.0213(7) Uani 1 1 d . . . C14 C 0.81519(8) 0.3118(3) 0.26880(17) 0.0207(7) Uani 1 1 d . . . C15 C 0.64986(8) 0.2030(3) 0.09143(17) 0.0216(7) Uani 1 1 d . . . C16 C 0.65231(8) 0.3132(3) 0.06585(17) 0.0214(7) Uani 1 1 d . . . C17 C 0.88278(9) 0.1846(3) 0.35782(19) 0.0252(7) Uani 1 1 d . . . H17A H 0.9033 0.1469 0.3964 0.030 Uiso 1 1 calc R . . H17B H 0.8848 0.1730 0.3117 0.030 Uiso 1 1 calc R . . C18 C 0.88351(9) 0.3167(3) 0.37287(17) 0.0234(7) Uani 1 1 d . . . H18A H 0.9071 0.3476 0.3837 0.028 Uiso 1 1 calc R . . H18B H 0.8792 0.3287 0.4163 0.028 Uiso 1 1 calc R . . C19 C 0.58099(8) 0.1937(3) -0.00488(18) 0.0250(7) Uani 1 1 d . . . H19A H 0.5860 0.1731 -0.0466 0.030 Uiso 1 1 calc R . . H19B H 0.5575 0.1627 -0.0148 0.030 Uiso 1 1 calc R . . C20 C 0.58063(8) 0.3274(3) 0.00154(18) 0.0250(7) Uani 1 1 d . . . H20A H 0.5776 0.3477 0.0457 0.030 Uiso 1 1 calc R . . H20B H 0.5602 0.3590 -0.0402 0.030 Uiso 1 1 calc R . . S17 S 0.78771(2) 0.12761(8) 0.07481(5) 0.0272(2) Uani 1 1 d . . . S18 S 0.79414(2) 0.36877(8) 0.02667(5) 0.02673(19) Uani 1 1 d . . . S19 S 0.86116(2) 0.09626(8) 0.16997(4) 0.02519(19) Uani 1 1 d . . . S20 S 0.86968(2) 0.38738(8) 0.11268(5) 0.0258(2) Uani 1 1 d . . . C21 C 0.76769(8) 0.2497(3) 0.02199(17) 0.0234(7) Uani 1 1 d . . . C22 C 0.82939(8) 0.1888(3) 0.10894(17) 0.0217(7) Uani 1 1 d . . . C23 C 0.83264(8) 0.3009(3) 0.08677(17) 0.0223(7) Uani 1 1 d . . . C24 C 0.90041(8) 0.1760(3) 0.18365(18) 0.0240(7) Uani 1 1 d . . . H24A H 0.9198 0.1432 0.2268 0.029 Uiso 1 1 calc R . . H24B H 0.9058 0.1618 0.1417 0.029 Uiso 1 1 calc R . . C25 C 0.89824(9) 0.3099(3) 0.19347(17) 0.0237(7) Uani 1 1 d . . . H25A H 0.9219 0.3443 0.2103 0.028 Uiso 1 1 calc R . . H25B H 0.8901 0.3239 0.2316 0.028 Uiso 1 1 calc R . . Fe1 Fe 0.5000 0.86935(7) 0.2500 0.0327(2) Uani 1 2 d S . . C26 C 0.51255(9) 0.9744(3) 0.14185(19) 0.0307(8) Uani 1 1 d . . . C27 C 0.48142(10) 1.0268(3) 0.1372(2) 0.0343(9) Uani 1 1 d . . . C28 C 0.46987(10) 1.1192(4) 0.0819(2) 0.0394(10) Uani 1 1 d . . . C29 C 0.49833(9) 1.1264(4) 0.05511(19) 0.0334(9) Uani 1 1 d . . . C30 C 0.52403(10) 1.0286(3) 0.09086(19) 0.0312(8) Uani 1 1 d . . . C31 C 0.51592(9) 0.6323(3) 0.28171(19) 0.0309(8) Uani 1 1 d . . . C32 C 0.52733(10) 0.5111(4) 0.3037(2) 0.0367(9) Uani 1 1 d . . . C33 C 0.5000 0.4324(6) 0.2500 0.0408(14) Uani 1 2 d S . . O1 O 0.52678(6) 0.8903(2) 0.18798(13) 0.0349(6) Uani 1 1 d . . . O2 O 0.46755(6) 0.9909(2) 0.17871(14) 0.0379(6) Uani 1 1 d . . . O3 O 0.44357(7) 1.1797(3) 0.05956(16) 0.0530(8) Uani 1 1 d . . . O4 O 0.49998(7) 1.1997(3) 0.01255(15) 0.0432(7) Uani 1 1 d . . . O5 O 0.54925(6) 1.0038(2) 0.07835(13) 0.0351(6) Uani 1 1 d . . . O6 O 0.52991(6) 0.7323(2) 0.30969(13) 0.0337(6) Uani 1 1 d . . . O7 O 0.55399(7) 0.4774(3) 0.35490(16) 0.0514(8) Uani 1 1 d . . . O8 O 0.5000 0.3230(4) 0.2500 0.0564(12) Uani 1 2 d S . . O1W O 0.45103(12) 0.4054(4) 0.0127(2) 0.1079(16) Uani 1 1 d D . . O2W O 0.54064(11) 0.6511(4) 0.1452(2) 0.1097(16) Uani 1 1 d D . . O3W O 0.51466(15) 0.4798(7) 0.0512(5) 0.155(5) Uani 0.50 1 d PD . . 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 S1 0.0185(4) 0.0226(4) 0.0357(5) 0.0043(4) 0.0041(4) -0.0009(3) S2 0.0183(4) 0.0232(4) 0.0287(4) 0.0049(4) 0.0041(4) -0.0002(3) S3 0.0181(4) 0.0209(4) 0.0307(4) 0.0006(4) 0.0065(4) -0.0002(3) S4 0.0188(4) 0.0219(4) 0.0271(4) 0.0014(4) 0.0067(3) -0.0006(3) S5 0.0221(4) 0.0279(5) 0.0284(4) 0.0077(4) 0.0057(4) 0.0028(4) S6 0.0188(4) 0.0264(5) 0.0295(5) 0.0012(4) 0.0060(4) -0.0034(3) S7 0.0187(4) 0.0249(4) 0.0321(5) -0.0003(4) 0.0054(4) -0.0033(3) S8 0.0199(4) 0.0243(4) 0.0292(5) 0.0028(4) 0.0008(4) -0.0012(3) C1 0.0185(17) 0.0207(17) 0.0244(17) -0.0023(14) 0.0063(14) -0.0008(13) C2 0.0158(17) 0.0237(17) 0.0230(17) -0.0014(14) 0.0059(14) -0.0006(13) C3 0.0172(17) 0.0258(18) 0.0244(17) 0.0000(14) 0.0073(14) 0.0007(14) C4 0.0176(17) 0.0240(17) 0.0203(16) 0.0018(14) 0.0069(14) 0.0038(13) C5 0.0196(17) 0.0228(17) 0.0215(16) -0.0033(14) 0.0045(14) -0.0026(13) C6 0.0186(17) 0.0224(17) 0.0218(17) -0.0022(14) 0.0043(14) 0.0006(13) C7 0.0209(18) 0.0270(19) 0.0289(18) -0.0025(15) 0.0076(15) 0.0016(14) C8 0.0212(18) 0.0274(18) 0.0231(17) -0.0016(14) 0.0047(15) 0.0028(14) C9 0.0218(19) 0.033(2) 0.042(2) -0.0003(17) 0.0112(17) 0.0019(16) C10 0.021(2) 0.038(2) 0.045(2) 0.0095(18) 0.0039(18) -0.0027(17) S9 0.0191(4) 0.0213(4) 0.0361(5) 0.0003(4) 0.0065(4) -0.0020(3) S10 0.0183(4) 0.0228(4) 0.0274(4) 0.0021(4) 0.0052(4) -0.0010(3) S11 0.0175(4) 0.0210(4) 0.0320(5) -0.0001(4) 0.0052(4) -0.0008(3) S12 0.0191(4) 0.0244(4) 0.0270(4) 0.0003(4) 0.0077(3) -0.0025(4) S13 0.0212(4) 0.0228(4) 0.0270(4) 0.0044(4) 0.0065(4) 0.0004(3) S14 0.0180(4) 0.0219(4) 0.0276(4) 0.0014(3) 0.0064(3) -0.0022(3) S15 0.0172(4) 0.0238(4) 0.0355(5) 0.0044(4) 0.0057(4) -0.0023(4) S16 0.0203(4) 0.0250(4) 0.0293(4) 0.0048(4) 0.0047(4) -0.0013(3) C11 0.0205(18) 0.0239(18) 0.0262(17) -0.0016(14) 0.0117(15) -0.0006(13) C12 0.0182(17) 0.0253(18) 0.0205(16) -0.0038(14) 0.0076(14) 0.0000(13) C13 0.0159(16) 0.0231(17) 0.0234(17) -0.0028(14) 0.0068(14) -0.0018(13) C14 0.0163(16) 0.0239(17) 0.0204(16) 0.0003(13) 0.0061(14) 0.0011(13) C15 0.0196(17) 0.0194(16) 0.0222(16) -0.0017(13) 0.0052(14) 0.0007(13) C16 0.0181(17) 0.0230(17) 0.0221(17) -0.0040(14) 0.0073(14) -0.0023(13) C17 0.0213(18) 0.0255(18) 0.0285(18) -0.0004(15) 0.0102(15) 0.0014(14) C18 0.0206(18) 0.0218(17) 0.0231(17) -0.0013(14) 0.0045(14) 0.0008(14) C19 0.0161(17) 0.0268(18) 0.0241(17) 0.0013(14) 0.0008(14) -0.0003(14) C20 0.0183(17) 0.0291(19) 0.0241(17) -0.0002(15) 0.0055(14) 0.0001(14) S17 0.0158(4) 0.0249(4) 0.0354(5) -0.0004(4) 0.0054(4) -0.0013(3) S18 0.0155(4) 0.0237(4) 0.0328(5) -0.0006(4) 0.0023(4) 0.0013(3) S19 0.0194(4) 0.0250(4) 0.0249(4) 0.0034(3) 0.0032(3) -0.0011(3) S20 0.0172(4) 0.0249(4) 0.0289(4) 0.0033(4) 0.0035(4) -0.0027(3) C21 0.0159(16) 0.0257(18) 0.0255(17) -0.0033(14) 0.0055(14) 0.0011(13) C22 0.0173(17) 0.0235(17) 0.0204(16) -0.0031(14) 0.0042(14) -0.0010(13) C23 0.0163(17) 0.0249(18) 0.0226(17) -0.0035(14) 0.0051(14) 0.0011(13) C24 0.0184(17) 0.0250(18) 0.0241(17) 0.0007(14) 0.0046(14) 0.0004(14) C25 0.0180(17) 0.0244(17) 0.0240(17) -0.0021(14) 0.0043(14) 0.0012(13) Fe1 0.0199(4) 0.0458(5) 0.0324(4) 0.000 0.0109(3) 0.000 C26 0.0198(18) 0.039(2) 0.0296(19) -0.0040(17) 0.0067(15) -0.0058(16) C27 0.024(2) 0.040(2) 0.035(2) -0.0034(18) 0.0083(17) -0.0032(17) C28 0.023(2) 0.049(3) 0.038(2) -0.0036(19) 0.0043(17) 0.0002(18) C29 0.028(2) 0.040(2) 0.0279(19) -0.0067(17) 0.0066(16) -0.0044(17) C30 0.027(2) 0.035(2) 0.0251(18) -0.0084(16) 0.0043(16) -0.0070(16) C31 0.0234(18) 0.042(2) 0.0300(19) 0.0003(17) 0.0139(15) -0.0020(17) C32 0.023(2) 0.050(2) 0.038(2) 0.0086(19) 0.0132(18) -0.0008(18) C33 0.026(3) 0.050(4) 0.055(4) 0.000 0.025(3) 0.000 O1 0.0195(13) 0.0524(17) 0.0320(13) 0.0041(13) 0.0102(11) 0.0037(12) O2 0.0220(14) 0.0498(17) 0.0428(16) 0.0022(13) 0.0146(13) 0.0016(12) O3 0.0297(16) 0.068(2) 0.0584(19) 0.0142(17) 0.0154(15) 0.0125(15) O4 0.0375(16) 0.0428(17) 0.0428(16) 0.0057(14) 0.0104(13) -0.0025(13) O5 0.0247(14) 0.0420(16) 0.0387(15) -0.0041(12) 0.0136(12) -0.0043(12) O6 0.0214(13) 0.0444(16) 0.0325(14) 0.0014(12) 0.0085(11) 0.0008(12) O7 0.0325(17) 0.0521(19) 0.0553(18) 0.0201(15) 0.0046(15) -0.0036(14) O8 0.033(2) 0.040(3) 0.096(4) 0.000 0.027(2) 0.000 O1W 0.129(4) 0.071(3) 0.101(3) 0.005(2) 0.026(3) 0.039(3) O2W 0.076(3) 0.153(5) 0.116(4) 0.018(3) 0.055(3) 0.035(3) O3W 0.187(13) 0.128(9) 0.115(8) 0.027(7) 0.031(8) 0.056(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 S1 C1 1.751(3) . ? S1 C3 1.755(3) . ? S2 C1 1.749(3) . ? S2 C4 1.755(3) . ? S3 C2 1.748(3) . ? S3 C5 1.771(3) . ? S4 C2 1.746(3) . ? S4 C6 1.771(3) . ? S5 C3 1.745(3) . ? S5 C7 1.807(3) . ? S6 C4 1.746(3) . ? S6 C8 1.803(3) . ? S7 C5 1.740(3) . ? S7 C9 1.798(4) . ? S8 C6 1.752(3) . ? S8 C10 1.812(4) . ? C1 C2 1.361(4) . ? C3 C4 1.350(5) . ? C5 C6 1.346(5) . ? C7 C8 1.512(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.500(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? S9 C11 1.725(3) . ? S9 C13 1.743(3) . ? S10 C11 1.732(3) . ? S10 C14 1.751(3) . ? S11 C12 1.724(3) . ? S11 C15 1.750(3) . ? S12 C12 1.731(3) . ? S12 C16 1.754(3) . ? S13 C13 1.745(3) . ? S13 C17 1.807(3) . ? S14 C14 1.747(3) . ? S14 C18 1.814(3) . ? S15 C15 1.744(3) . ? S15 C19 1.812(3) . ? S16 C16 1.741(3) . ? S16 C20 1.810(3) . ? C11 C12 1.393(5) . ? C13 C14 1.356(5) . ? C15 C16 1.362(5) . ? C17 C18 1.510(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.505(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? S17 C21 1.729(3) . ? S17 C22 1.745(3) . ? S18 C21 1.720(3) . ? S18 C23 1.751(3) . ? S19 C22 1.741(3) . ? S19 C24 1.804(3) . ? S20 C23 1.729(3) . ? S20 C25 1.806(3) . ? C21 C21 1.387(6) 7_655 ? C22 C23 1.362(5) . ? C24 C25 1.523(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? Fe1 O6 2.038(3) 2_655 ? Fe1 O6 2.038(3) . ? Fe1 O1 2.040(2) 2_655 ? Fe1 O1 2.040(2) . ? Fe1 O2 2.046(3) 2_655 ? Fe1 O2 2.046(3) . ? C26 O1 1.290(4) . ? C26 C27 1.412(5) . ? C26 C30 1.456(5) . ? C27 O2 1.284(4) . ? C27 C28 1.457(6) . ? C28 O3 1.218(5) . ? C28 C29 1.523(5) . ? C29 O4 1.219(4) . ? C29 C30 1.501(5) . ? C30 O5 1.232(4) . ? C31 O6 1.284(4) . ? C31 C31 1.425(7) 2_655 ? C31 C32 1.449(5) . ? C32 O7 1.233(4) . ? C32 C33 1.501(5) . ? C33 O8 1.227(7) . ? C33 C32 1.501(5) 2_655 ? 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 S1 C3 95.18(15) . . ? C1 S2 C4 95.04(15) . . ? C2 S3 C5 95.17(15) . . ? C2 S4 C6 94.71(15) . . ? C3 S5 C7 100.03(16) . . ? C4 S6 C8 102.17(16) . . ? C5 S7 C9 99.12(16) . . ? C6 S8 C10 102.43(17) . . ? C2 C1 S2 122.7(3) . . ? C2 C1 S1 122.1(3) . . ? S2 C1 S1 115.14(18) . . ? C1 C2 S4 123.0(3) . . ? C1 C2 S3 121.6(3) . . ? S4 C2 S3 115.47(18) . . ? C4 C3 S5 128.4(3) . . ? C4 C3 S1 117.0(2) . . ? S5 C3 S1 114.54(19) . . ? C3 C4 S6 128.7(3) . . ? C3 C4 S2 117.4(3) . . ? S6 C4 S2 113.94(18) . . ? C6 C5 S7 127.6(3) . . ? C6 C5 S3 116.5(3) . . ? S7 C5 S3 115.88(19) . . ? C5 C6 S8 128.6(3) . . ? C5 C6 S4 117.5(2) . . ? S8 C6 S4 113.93(18) . . ? C8 C7 S5 113.3(2) . . ? C8 C7 H7A 108.9 . . ? S5 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? S5 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 S6 114.5(2) . . ? C7 C8 H8A 108.6 . . ? S6 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? S6 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 S7 112.4(3) . . ? C10 C9 H9A 109.1 . . ? S7 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? S7 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C9 C10 S8 114.8(3) . . ? C9 C10 H10A 108.6 . . ? S8 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? S8 C10 H10B 108.6 . . ? H10A C10 H10B 107.5 . . ? C11 S9 C13 95.86(16) . . ? C11 S10 C14 95.65(16) . . ? C12 S11 C15 95.98(15) . . ? C12 S12 C16 95.73(15) . . ? C13 S13 C17 100.29(16) . . ? C14 S14 C18 102.68(15) . . ? C15 S15 C19 101.42(16) . . ? C16 S16 C20 102.11(15) . . ? C12 C11 S9 121.7(3) . . ? C12 C11 S10 123.1(3) . . ? S9 C11 S10 115.23(19) . . ? C11 C12 S11 121.8(3) . . ? C11 C12 S12 122.8(3) . . ? S11 C12 S12 115.37(18) . . ? C14 C13 S9 116.8(2) . . ? C14 C13 S13 128.4(3) . . ? S9 C13 S13 114.78(18) . . ? C13 C14 S14 128.5(3) . . ? C13 C14 S10 116.3(2) . . ? S14 C14 S10 115.14(18) . . ? C16 C15 S15 128.2(3) . . ? C16 C15 S11 116.5(2) . . ? S15 C15 S11 115.24(18) . . ? C15 C16 S16 128.5(3) . . ? C15 C16 S12 116.3(2) . . ? S16 C16 S12 115.21(18) . . ? C18 C17 S13 114.4(2) . . ? C18 C17 H17A 108.7 . . ? S13 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? S13 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 S14 114.1(2) . . ? C17 C18 H18A 108.7 . . ? S14 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? S14 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 S15 114.0(2) . . ? C20 C19 H19A 108.7 . . ? S15 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? S15 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 S16 114.9(2) . . ? C19 C20 H20A 108.6 . . ? S16 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? S16 C20 H20B 108.6 . . ? H20A C20 H20B 107.5 . . ? C21 S17 C22 94.98(16) . . ? C21 S18 C23 95.48(16) . . ? C22 S19 C24 101.61(16) . . ? C23 S20 C25 100.58(16) . . ? C21 C21 S18 122.3(4) 7_655 . ? C21 C21 S17 121.4(4) 7_655 . ? S18 C21 S17 116.25(18) . . ? C23 C22 S19 129.2(3) . . ? C23 C22 S17 117.2(2) . . ? S19 C22 S17 113.60(18) . . ? C22 C23 S20 128.4(3) . . ? C22 C23 S18 116.1(2) . . ? S20 C23 S18 115.45(19) . . ? C25 C24 S19 113.9(2) . . ? C25 C24 H24A 108.8 . . ? S19 C24 H24A 108.8 . . ? C25 C24 H24B 108.8 . . ? S19 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C24 C25 S20 114.1(2) . . ? C24 C25 H25A 108.7 . . ? S20 C25 H25A 108.7 . . ? C24 C25 H25B 108.7 . . ? S20 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? O6 Fe1 O6 82.17(15) 2_655 . ? O6 Fe1 O1 95.13(10) 2_655 2_655 ? O6 Fe1 O1 94.81(10) . 2_655 ? O6 Fe1 O1 94.81(10) 2_655 . ? O6 Fe1 O1 95.13(10) . . ? O1 Fe1 O1 166.80(16) 2_655 . ? O6 Fe1 O2 172.23(11) 2_655 2_655 ? O6 Fe1 O2 90.75(10) . 2_655 ? O1 Fe1 O2 82.23(10) 2_655 2_655 ? O1 Fe1 O2 88.98(10) . 2_655 ? O6 Fe1 O2 90.75(10) 2_655 . ? O6 Fe1 O2 172.23(11) . . ? O1 Fe1 O2 88.98(10) 2_655 . ? O1 Fe1 O2 82.23(10) . . ? O2 Fe1 O2 96.49(15) 2_655 . ? O1 C26 C27 119.4(3) . . ? O1 C26 C30 129.3(3) . . ? C27 C26 C30 111.3(3) . . ? O2 C27 C26 120.0(3) . . ? O2 C27 C28 129.6(4) . . ? C26 C27 C28 110.4(3) . . ? O3 C28 C27 129.9(4) . . ? O3 C28 C29 125.1(4) . . ? C27 C28 C29 104.9(3) . . ? O4 C29 C30 126.2(4) . . ? O4 C29 C28 125.7(4) . . ? C30 C29 C28 108.0(3) . . ? O5 C30 C26 129.5(4) . . ? O5 C30 C29 125.4(3) . . ? C26 C30 C29 105.1(3) . . ? O6 C31 C31 119.23(19) . 2_655 ? O6 C31 C32 130.5(3) . . ? C31 C31 C32 110.3(2) 2_655 . ? O7 C32 C31 128.1(4) . . ? O7 C32 C33 126.2(4) . . ? C31 C32 C33 105.7(3) . . ? O8 C33 C32 126.0(2) . 2_655 ? O8 C33 C32 126.0(2) . . ? C32 C33 C32 108.1(5) 2_655 . ? C26 O1 Fe1 109.1(2) . . ? C27 O2 Fe1 108.8(2) . . ? C31 O6 Fe1 109.7(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.066 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.102 #===END data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 Fe O15, 5(C10 H8 S8), C7 H5 N' _chemical_formula_sum 'C72 H45 Fe N O15 S40' _chemical_formula_weight 2502.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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 19.591(2) _cell_length_b 19.395(2) _cell_length_c 12.9581(12) _cell_angle_alpha 103.194(11) _cell_angle_beta 102.859(11) _cell_angle_gamma 73.680(10) _cell_volume 4534.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 6681 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 25.9 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.375 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2540 _exptl_absorpt_coefficient_mu 1.153 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4478 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details ; Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998) I/sigma threshold for reflections = 5.000 Delta(U)/lambda**2 = 0.000 Highest even order spherical harmonic = 6 Highest odd order spherical harmonic = 3 ; _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 70 mm. 167 exposures (4.5 min per exposure) were obtained with 0 < \f < 250\% and with the crystals rotated through 1.5\% in \f. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE Imaging Plate Diffraction System' _diffrn_measurement_method '\f scan ' _diffrn_standards_decay_% 'negligible' _diffrn_reflns_number 33942 _diffrn_reflns_av_R_equivalents 0.1991 _diffrn_reflns_av_sigmaI/netI 0.3273 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 23.25 _reflns_number_total 12379 _reflns_number_gt 3876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software (Stoe, 1996)' _computing_cell_refinement 'IPDS software (Stoe, 1996)' _computing_data_reduction 'IPDS software (Stoe, 1996)' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Cameron (Watkin, 1996)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)]' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12379 _refine_ls_number_parameters 1174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2029 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 0.682 _refine_ls_restrained_S_all 0.682 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.5673(10) 0.8311(7) 0.5512(11) 0.040(4) Uani 1 1 d . . . H11A H 0.5395 0.8049 0.4888 0.03(4) Uiso 1 1 calc R . . H11B H 0.6189 0.8065 0.5514 0.13(8) Uiso 1 1 calc R . . C12 C 0.5478(9) 0.8216(8) 0.6489(11) 0.039(4) Uani 1 1 d . . . H12A H 0.5526 0.7689 0.6445 0.15(9) Uiso 1 1 calc R . . H12B H 0.4963 0.8465 0.6492 0.25(15) Uiso 1 1 calc R . . C13 C 0.5860(7) 0.9645(6) 0.6585(10) 0.023(3) Uani 1 1 d . . . C14 C 0.6025(7) 0.9372(6) 0.7528(10) 0.024(3) Uani 1 1 d . . . C15 C 0.6253(7) 1.0664(6) 0.8014(10) 0.024(3) Uani 1 1 d . . . C16 C 0.6341(7) 1.1362(6) 0.8505(9) 0.023(3) Uani 1 1 d . . . C17 C 0.6335(7) 1.2706(7) 0.8924(10) 0.027(3) Uani 1 1 d . . . C18 C 0.6511(8) 1.2487(6) 0.9883(10) 0.028(3) Uani 1 1 d . . . C19 C 0.5796(8) 1.4035(6) 0.9863(10) 0.034(4) Uani 1 1 d . . . H19A H 0.5605 1.4561 0.9837 0.02(3) Uiso 1 1 calc R . . H19B H 0.5383 1.3830 0.9849 0.13(8) Uiso 1 1 calc R . . C20 C 0.6334(8) 1.3942(6) 1.0934(10) 0.032(4) Uani 1 1 d . . . H20A H 0.6088 1.4232 1.1540 0.20(12) Uiso 1 1 calc R . . H20B H 0.6744 1.4147 1.0942 0.02(3) Uiso 1 1 calc R . . S11 S 0.5540(2) 0.92003(17) 0.5297(3) 0.0327(9) Uani 1 1 d . . . S12 S 0.5984(2) 0.85430(18) 0.7752(3) 0.0353(10) Uani 1 1 d . . . S13 S 0.5991(2) 1.04834(18) 0.6623(3) 0.0298(9) Uani 1 1 d . . . S14 S 0.6331(2) 0.99619(18) 0.8659(3) 0.0299(9) Uani 1 1 d . . . S15 S 0.6168(2) 1.20491(19) 0.7812(3) 0.0328(9) Uani 1 1 d . . . S16 S 0.6606(2) 1.15774(18) 0.9883(3) 0.0307(9) Uani 1 1 d . . . S17 S 0.6199(2) 1.35981(18) 0.8718(3) 0.0358(10) Uani 1 1 d . . . S18 S 0.6676(2) 1.30305(18) 1.1151(3) 0.0423(10) Uani 1 1 d . . . C21 C 0.8050(9) 0.7619(6) 0.6114(10) 0.033(3) Uani 1 1 d . . . H21A H 0.7965 0.7192 0.5562 0.01(3) Uiso 1 1 calc R . . H21B H 0.8574 0.7593 0.6247 0.06(4) Uiso 1 1 calc R . . C22 C 0.7840(9) 0.7564(6) 0.7154(10) 0.033(3) Uani 1 1 d . . . H22A H 0.8079 0.7071 0.7324 0.05(4) Uiso 1 1 calc R . . H22B H 0.7312 0.7616 0.7032 0.11(7) Uiso 1 1 calc R . . C23 C 0.7788(7) 0.9103(6) 0.6713(9) 0.020(2) Uani 1 1 d . . . C24 C 0.7997(7) 0.8986(6) 0.7750(9) 0.020(2) Uani 1 1 d . . . C25 C 0.8038(7) 1.0311(6) 0.7768(9) 0.018(2) Uani 1 1 d . . . C26 C 0.8103(6) 1.1012(6) 0.8074(10) 0.018(2) Uani 1 1 d . . . C27 C 0.8090(7) 1.2370(7) 0.8195(10) 0.027(3) Uani 1 1 d . . . C28 C 0.8288(7) 1.2235(6) 0.9214(10) 0.021(3) Uani 1 1 d . . . C29 C 0.8468(8) 1.3666(7) 0.8842(10) 0.033(4) Uani 1 1 d . . . H29A H 0.8993 1.3443 0.8917 0.04(4) Uiso 1 1 calc R . . H29B H 0.8386 1.4167 0.8707 0.00(2) Uiso 1 1 calc R . . C30 C 0.8228(10) 1.3708(7) 0.9875(11) 0.043(4) Uani 1 1 d . . . H30A H 0.7695 1.3873 0.9770 1.0(11) Uiso 1 1 calc R . . H30B H 0.8423 1.4082 1.0425 0.05(4) Uiso 1 1 calc R . . S21 S 0.7579(2) 0.84272(18) 0.5587(3) 0.0306(9) Uani 1 1 d . . . S22 S 0.8073(2) 0.82299(18) 0.8293(3) 0.0326(9) Uani 1 1 d . . . S23 S 0.7786(2) 0.99222(18) 0.6433(3) 0.0274(9) Uani 1 1 d . . . S24 S 0.8206(2) 0.97293(17) 0.8666(3) 0.0267(9) Uani 1 1 d . . . S25 S 0.7923(2) 1.16229(18) 0.7229(3) 0.0285(9) Uani 1 1 d . . . S26 S 0.8370(2) 1.13671(18) 0.9424(3) 0.0275(9) Uani 1 1 d . . . S27 S 0.8020(2) 1.31527(18) 0.7708(3) 0.0376(10) Uani 1 1 d . . . S28 S 0.8498(3) 1.28618(19) 1.0385(3) 0.0455(11) Uani 1 1 d . . . C31 C 0.0277(14) 1.2082(9) 0.9264(12) 0.074(7) Uani 1 1 d . . . H31A H -0.0224 1.2313 0.9387 0.07(6) Uiso 1 1 calc R . . H31B H 0.0584 1.2374 0.9791 0.06(5) Uiso 1 1 calc R . . C32 C 0.0303(13) 1.2200(8) 0.8311(11) 0.059(6) Uani 1 1 d . . . H32A H 0.0816 1.2158 0.8295 0.3(2) Uiso 1 1 calc R . . H32B H 0.0047 1.2715 0.8283 0.02(3) Uiso 1 1 calc R . . C33 C 0.0192(7) 1.0690(6) 0.8478(10) 0.021(3) Uani 1 1 d . . . C34 C -0.0031(7) 1.0870(7) 0.7489(10) 0.025(3) Uani 1 1 d . . . C35 C -0.0161(7) 0.9557(6) 0.7291(9) 0.015(3) Uani 1 1 d . . . C36 C -0.0247(7) 0.8892(6) 0.6907(9) 0.019(3) Uani 1 1 d . . . C37 C 0.0001(7) 0.7465(7) 0.6583(11) 0.027(3) Uani 1 1 d . . . C38 C -0.0218(7) 0.7653(6) 0.5586(10) 0.026(3) Uani 1 1 d . . . C39 C -0.0149(9) 0.6104(7) 0.5690(10) 0.035(4) Uani 1 1 d . . . H39A H -0.0014 0.5581 0.5744 0.02(3) Uiso 1 1 calc R . . H39B H -0.0680 0.6275 0.5632 0.06(5) Uiso 1 1 calc R . . C40 C 0.0063(9) 0.6183(6) 0.4662(11) 0.037(4) Uani 1 1 d . . . H40A H -0.0134 0.5842 0.4052 0.06(5) Uiso 1 1 calc R . . H40B H 0.0595 0.6035 0.4735 0.10(7) Uiso 1 1 calc R . . S31 S 0.0497(2) 1.12450(18) 0.9660(3) 0.0333(9) Uani 1 1 d . . . S32 S -0.0041(2) 1.16627(19) 0.7067(3) 0.0354(10) Uani 1 1 d . . . S33 S 0.0096(2) 0.98602(17) 0.8654(3) 0.0282(9) Uani 1 1 d . . . S34 S -0.0350(2) 1.02118(18) 0.6466(3) 0.0281(9) Uani 1 1 d . . . S35 S -0.0077(2) 0.81996(18) 0.7679(3) 0.0279(9) Uani 1 1 d . . . S36 S -0.0541(2) 0.85858(17) 0.5531(3) 0.0273(8) Uani 1 1 d . . . S37 S 0.0266(3) 0.66045(19) 0.6909(3) 0.0476(11) Uani 1 1 d . . . S38 S -0.0245(3) 0.70880(19) 0.4343(3) 0.0448(11) Uani 1 1 d . . . C41 C 0.1899(8) 1.3532(7) 0.9651(10) 0.031(3) Uani 1 1 d . . . H41A H 0.1400 1.3468 0.9435 0.03(3) Uiso 1 1 calc R . . H41B H 0.1894 1.3959 1.0242 0.01(3) Uiso 1 1 calc R . . C42 C 0.2118(9) 1.3705(7) 0.8692(10) 0.038(4) Uani 1 1 d . . . H42A H 0.2628 1.3734 0.8882 0.046 Uiso 1 1 calc R . . H42B H 0.1820 1.4189 0.8547 0.046 Uiso 1 1 calc R . . C43 C 0.2317(7) 1.2112(6) 0.8992(9) 0.026(3) Uani 1 1 d . . . C44 C 0.2132(7) 1.2238(6) 0.7968(10) 0.021(3) Uani 1 1 d . . . C45 C 0.2095(8) 1.0911(7) 0.7814(10) 0.028(3) Uani 1 1 d . . . C46 C 0.1982(7) 1.0238(8) 0.7492(11) 0.033(3) Uani 1 1 d . . . C47 C 0.1814(7) 0.8938(7) 0.7422(10) 0.028(3) Uani 1 1 d . . . C48 C 0.1634(8) 0.9067(7) 0.6357(11) 0.032(4) Uani 1 1 d . . . C49 C 0.1823(12) 0.7488(9) 0.6715(13) 0.064(6) Uani 1 1 d . . . H49A H 0.2242 0.7075 0.6862 0.26(17) Uiso 1 1 calc R . . H49B H 0.1383 0.7311 0.6635 0.13(8) Uiso 1 1 calc R . . C50 C 0.1839(15) 0.7646(9) 0.5719(14) 0.084(8) Uani 1 1 d . . . H50A H 0.1695 0.7242 0.5170 0.07(5) Uiso 1 1 calc R . . H50B H 0.2352 0.7601 0.5703 0.20(14) Uiso 1 1 calc R . . S41 S 0.2456(2) 1.27504(19) 1.0155(3) 0.0388(10) Uani 1 1 d . . . S42 S 0.2014(2) 1.3035(2) 0.7484(3) 0.0388(10) Uani 1 1 d . . . S43 S 0.2372(2) 1.12295(18) 0.9166(3) 0.0299(9) Uani 1 1 d . . . S44 S 0.1957(2) 1.15136(18) 0.6967(3) 0.0309(9) Uani 1 1 d . . . S45 S 0.2105(2) 0.96306(19) 0.8350(3) 0.0326(9) Uani 1 1 d . . . S46 S 0.1700(2) 0.98905(19) 0.6136(3) 0.0320(9) Uani 1 1 d . . . S47 S 0.1835(2) 0.8176(2) 0.7864(3) 0.0435(11) Uani 1 1 d . . . S48 S 0.1359(3) 0.8448(2) 0.5244(3) 0.0491(12) Uani 1 1 d . . . C51 C 0.4593(9) 1.1701(8) 0.9396(12) 0.049(4) Uani 1 1 d . . . H51A H 0.4576 1.2066 1.0069 0.058 Uiso 1 1 calc R . . H51B H 0.5094 1.1575 0.9258 0.058 Uiso 1 1 calc R . . C52 C 0.4156(11) 1.2062(9) 0.8566(12) 0.059(5) Uani 1 1 d . . . H52A H 0.4348 1.2482 0.8561 0.071 Uiso 1 1 calc R . . H52B H 0.3667 1.2264 0.8755 0.071 Uiso 1 1 calc R . . C53 C 0.4154(8) 1.0481(7) 0.8395(10) 0.031(3) Uani 1 1 d . . . C54 C 0.3981(8) 1.0737(6) 0.7456(10) 0.027(3) Uani 1 1 d . . . C55 C 0.3685(7) 0.9474(8) 0.7013(11) 0.034(3) Uani 1 1 d . . . C56 C 0.3620(7) 0.8789(7) 0.6584(11) 0.032(3) Uani 1 1 d . . . C57 C 0.3988(7) 0.7399(7) 0.6216(11) 0.029(3) Uani 1 1 d . . . C58 C 0.3770(7) 0.7606(7) 0.5254(10) 0.024(3) Uani 1 1 d . . . C59 C 0.4052(9) 0.5931(7) 0.5271(11) 0.038(4) Uani 1 1 d . . . H59A H 0.4467 0.5603 0.4948 0.046 Uiso 1 1 calc R . . H59B H 0.3811 0.5621 0.5503 0.046 Uiso 1 1 calc R . . C60 C 0.3539(9) 0.6297(7) 0.4425(10) 0.039(4) Uani 1 1 d . . . H60A H 0.3073 0.6521 0.4684 0.047 Uiso 1 1 calc R . . H60B H 0.3453 0.5921 0.3784 0.047 Uiso 1 1 calc R . . S51 S 0.4459(3) 1.0936(2) 0.9669(3) 0.0549(12) Uani 1 1 d . . . S52 S 0.4059(3) 1.1549(2) 0.7206(3) 0.0491(12) Uani 1 1 d . . . S53 S 0.3934(2) 0.9690(2) 0.8432(3) 0.0388(10) Uani 1 1 d . . . S54 S 0.3581(2) 1.01673(19) 0.6336(3) 0.0357(10) Uani 1 1 d . . . S55 S 0.3811(2) 0.8085(2) 0.7312(3) 0.0375(10) Uani 1 1 d . . . S56 S 0.3378(2) 0.85256(19) 0.5192(3) 0.0390(10) Uani 1 1 d . . . S57 S 0.4402(2) 0.65213(19) 0.6465(3) 0.0442(10) Uani 1 1 d . . . S58 S 0.3809(2) 0.69813(19) 0.4023(3) 0.0446(11) Uani 1 1 d . . . Fe1 Fe 0.21867(11) 0.45740(9) 0.31372(14) 0.0279(5) Uani 1 1 d . . . C101 C 0.0938(8) 0.4386(7) 0.1790(9) 0.027(3) Uani 1 1 d . . . C102 C 0.0326(8) 0.4205(7) 0.1043(10) 0.032(3) Uani 1 1 d . . . C103 C -0.0265(8) 0.4904(6) 0.1057(10) 0.025(3) Uani 1 1 d . . . C104 C 0.0055(8) 0.5487(6) 0.1848(11) 0.032(4) Uani 1 1 d . . . C105 C 0.0776(8) 0.5125(7) 0.2269(10) 0.026(3) Uani 1 1 d . . . O101 O 0.1574(5) 0.3972(4) 0.2042(6) 0.025(2) Uani 1 1 d . . . O102 O 0.0249(6) 0.3619(5) 0.0464(8) 0.045(3) Uani 1 1 d . . . O103 O -0.0857(6) 0.4989(4) 0.0489(7) 0.037(2) Uani 1 1 d . . . O104 O -0.0268(5) 0.6135(5) 0.2026(7) 0.038(2) Uani 1 1 d . . . O105 O 0.1279(5) 0.5384(4) 0.2955(6) 0.030(2) Uani 1 1 d . . . C106 C 0.3369(7) 0.3816(6) 0.2171(9) 0.020(3) Uani 1 1 d . . . C107 C 0.3956(7) 0.3319(7) 0.1651(10) 0.028(3) Uani 1 1 d . . . C108 C 0.4019(9) 0.3711(7) 0.0820(11) 0.036(4) Uani 1 1 d . . . C109 C 0.3465(7) 0.4433(6) 0.0880(10) 0.027(3) Uani 1 1 d . . . C110 C 0.3099(8) 0.4461(6) 0.1746(9) 0.025(3) Uani 1 1 d . . . O106 O 0.3070(5) 0.3716(4) 0.2915(6) 0.030(2) Uani 1 1 d . . . O107 O 0.4321(5) 0.2730(5) 0.1828(7) 0.037(2) Uani 1 1 d . . . O108 O 0.4427(6) 0.3474(5) 0.0172(8) 0.041(3) Uani 1 1 d . . . O109 O 0.3373(6) 0.4876(5) 0.0289(7) 0.041(3) Uani 1 1 d . . . O110 O 0.2569(5) 0.4953(4) 0.2115(6) 0.030(2) Uani 1 1 d . . . C111 C 0.2409(7) 0.5124(6) 0.5283(9) 0.024(3) Uani 1 1 d . . . C112 C 0.2540(8) 0.5521(7) 0.6382(11) 0.032(3) Uani 1 1 d . . . C113 C 0.2131(8) 0.5243(8) 0.6964(12) 0.043(4) Uani 1 1 d . . . C114 C 0.1760(7) 0.4700(7) 0.6202(10) 0.030(3) Uani 1 1 d . . . C115 C 0.1972(8) 0.4631(7) 0.5173(11) 0.029(3) Uani 1 1 d . . . O111 O 0.2635(5) 0.5182(4) 0.4433(6) 0.031(2) Uani 1 1 d . . . O112 O 0.2915(6) 0.5956(5) 0.6734(7) 0.044(3) Uani 1 1 d . . . O113 O 0.2113(7) 0.5427(6) 0.7945(8) 0.063(3) Uani 1 1 d . . . O114 O 0.1371(6) 0.4372(6) 0.6410(8) 0.054(3) Uani 1 1 d . . . O115 O 0.1854(5) 0.4208(4) 0.4266(7) 0.032(2) Uani 1 1 d . . . C1 C 0.4375(8) 0.4246(7) 0.6751(12) 0.037(4) Uani 1 1 d . . . C2 C 0.4156(8) 0.3957(7) 0.5687(11) 0.037(4) Uani 1 1 d . . . H2 H 0.4339 0.4057 0.5131 0.044 Uiso 1 1 calc R . . C3 C 0.3665(9) 0.3518(7) 0.5432(12) 0.045(4) Uani 1 1 d . . . H3 H 0.3508 0.3334 0.4698 0.054 Uiso 1 1 calc R . . C4 C 0.3404(8) 0.3345(8) 0.6219(13) 0.054(5) Uani 1 1 d . . . H4 H 0.3077 0.3038 0.6034 0.064 Uiso 1 1 calc R . . C5 C 0.3632(10) 0.3635(9) 0.7312(13) 0.056(5) Uani 1 1 d . . . H5 H 0.3448 0.3533 0.7866 0.067 Uiso 1 1 calc R . . C6 C 0.4107(9) 0.4052(8) 0.7560(12) 0.046(4) Uani 1 1 d . . . H6 H 0.4271 0.4226 0.8295 0.055 Uiso 1 1 calc R . . C7 C 0.4891(9) 0.4676(8) 0.7037(13) 0.050(4) Uani 1 1 d . . . N8 N 0.5290(9) 0.5024(8) 0.7266(13) 0.075(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 C11 0.049(12) 0.042(9) 0.037(9) 0.007(7) 0.003(8) -0.027(9) C12 0.050(12) 0.037(9) 0.041(9) -0.001(7) 0.011(8) -0.030(8) C13 0.027(9) 0.021(7) 0.023(7) 0.004(6) 0.006(7) -0.006(6) C14 0.024(9) 0.014(7) 0.030(8) -0.004(6) 0.014(7) 0.002(6) C15 0.019(8) 0.024(7) 0.019(7) -0.002(6) -0.003(6) 0.000(6) C16 0.029(9) 0.020(7) 0.019(7) 0.005(5) 0.000(6) -0.005(6) C17 0.028(9) 0.029(7) 0.023(7) -0.007(6) 0.010(7) -0.010(6) C18 0.044(10) 0.016(7) 0.029(8) -0.004(6) 0.013(7) -0.013(6) C19 0.044(10) 0.010(6) 0.040(8) -0.008(6) 0.023(8) 0.008(6) C20 0.048(10) 0.021(7) 0.033(8) 0.001(6) 0.011(8) -0.015(7) S11 0.038(2) 0.0273(19) 0.0281(19) 0.0015(15) 0.0023(18) -0.0048(17) S12 0.053(3) 0.0249(19) 0.031(2) 0.0027(16) 0.011(2) -0.0130(18) S13 0.035(2) 0.0288(19) 0.0256(18) 0.0029(15) 0.0041(18) -0.0098(17) S14 0.037(2) 0.0307(19) 0.0251(18) 0.0039(15) 0.0090(18) -0.0111(17) S15 0.042(3) 0.030(2) 0.0262(19) 0.0066(16) 0.0032(19) -0.0093(18) S16 0.039(2) 0.031(2) 0.0200(18) 0.0033(15) 0.0015(18) -0.0088(17) S17 0.053(3) 0.0264(19) 0.029(2) 0.0036(15) 0.015(2) -0.0058(18) S18 0.059(3) 0.032(2) 0.0261(19) -0.0007(16) 0.001(2) -0.0038(19) C21 0.048(8) 0.011(5) 0.037(6) -0.003(4) 0.008(5) -0.007(5) C22 0.048(8) 0.011(5) 0.037(6) -0.003(4) 0.008(5) -0.007(5) C23 0.033(6) 0.009(4) 0.019(4) -0.007(4) 0.019(5) -0.005(4) C24 0.033(6) 0.009(4) 0.019(4) -0.007(4) 0.019(5) -0.005(4) C25 0.006(5) 0.027(5) 0.024(5) 0.011(4) 0.005(4) -0.001(4) C26 0.006(5) 0.027(5) 0.024(5) 0.011(4) 0.005(4) -0.001(4) C27 0.026(9) 0.021(7) 0.031(8) 0.008(6) -0.002(7) -0.005(6) C28 0.017(8) 0.023(7) 0.023(7) 0.003(6) 0.002(6) -0.008(6) C29 0.040(10) 0.022(7) 0.046(9) 0.023(6) 0.013(8) -0.002(7) C30 0.083(14) 0.023(8) 0.029(8) -0.006(6) 0.018(9) -0.024(8) S21 0.040(3) 0.032(2) 0.0219(18) 0.0027(15) 0.0053(18) -0.0130(18) S22 0.046(3) 0.0307(19) 0.0285(19) 0.0078(15) 0.0095(19) -0.0162(18) S23 0.035(2) 0.0268(19) 0.0223(18) 0.0042(15) 0.0069(18) -0.0087(17) S24 0.034(2) 0.0250(19) 0.0236(18) 0.0074(15) 0.0041(18) -0.0086(17) S25 0.043(3) 0.0219(18) 0.0225(18) 0.0050(15) 0.0056(18) -0.0108(17) S26 0.037(2) 0.0269(19) 0.0207(18) 0.0035(15) 0.0038(17) -0.0122(17) S27 0.057(3) 0.0243(19) 0.032(2) 0.0104(16) 0.000(2) -0.0127(19) S28 0.082(4) 0.035(2) 0.027(2) 0.0020(16) 0.007(2) -0.030(2) C31 0.14(2) 0.035(10) 0.024(9) 0.011(8) -0.027(12) -0.010(12) C32 0.131(19) 0.023(9) 0.030(9) 0.001(7) -0.002(10) -0.043(10) C33 0.022(8) 0.015(6) 0.022(7) -0.005(5) 0.001(7) -0.005(6) C34 0.023(9) 0.031(8) 0.017(7) -0.008(6) 0.003(7) -0.009(6) C35 0.015(8) 0.015(7) 0.013(6) 0.000(5) -0.004(6) -0.005(6) C36 0.028(9) 0.014(6) 0.016(7) 0.006(5) 0.016(6) 0.006(6) C37 0.017(8) 0.030(8) 0.037(8) 0.007(6) 0.003(7) -0.007(6) C38 0.024(9) 0.017(7) 0.038(8) -0.003(6) 0.014(7) -0.007(6) C39 0.058(12) 0.014(7) 0.029(8) -0.005(6) 0.005(8) -0.011(7) C40 0.052(12) 0.015(7) 0.045(9) -0.006(6) 0.027(8) -0.003(7) S31 0.045(3) 0.030(2) 0.0225(18) -0.0015(15) 0.0004(19) -0.0134(18) S32 0.049(3) 0.032(2) 0.0297(19) 0.0082(16) 0.0016(19) -0.0190(19) S33 0.043(3) 0.0230(19) 0.0177(17) -0.0011(14) 0.0085(18) -0.0083(17) S34 0.037(3) 0.0259(19) 0.0200(18) 0.0024(14) 0.0005(18) -0.0110(17) S35 0.035(2) 0.0256(19) 0.0227(18) 0.0005(15) 0.0082(18) -0.0068(17) S36 0.035(2) 0.0227(18) 0.0199(18) -0.0023(14) 0.0030(17) -0.0070(17) S37 0.079(3) 0.024(2) 0.038(2) 0.0083(16) -0.001(2) -0.015(2) S38 0.073(3) 0.031(2) 0.029(2) -0.0059(16) 0.010(2) -0.018(2) C41 0.026(9) 0.045(9) 0.021(7) 0.006(7) 0.008(7) -0.003(7) C42 0.054(12) 0.036(8) 0.028(8) -0.003(6) 0.018(8) -0.015(8) C43 0.033(9) 0.021(7) 0.017(7) -0.005(5) 0.003(7) -0.003(6) C44 0.023(8) 0.020(7) 0.017(7) 0.003(5) 0.003(7) -0.001(6) C45 0.031(9) 0.032(8) 0.029(8) 0.004(6) 0.004(7) -0.024(7) C46 0.020(9) 0.044(9) 0.038(8) 0.013(7) 0.011(7) -0.004(7) C47 0.020(9) 0.046(9) 0.027(8) 0.007(6) 0.012(7) -0.013(7) C48 0.043(10) 0.025(7) 0.032(8) 0.001(6) 0.003(8) -0.018(7) C49 0.096(17) 0.033(10) 0.042(11) -0.009(8) -0.025(11) -0.026(11) C50 0.16(2) 0.049(11) 0.049(12) -0.038(9) 0.071(14) -0.025(12) S41 0.050(3) 0.030(2) 0.030(2) 0.0039(17) -0.003(2) -0.0101(19) S42 0.053(3) 0.038(2) 0.031(2) 0.0102(17) 0.008(2) -0.017(2) S43 0.039(3) 0.027(2) 0.0215(18) 0.0073(15) 0.0043(18) -0.0032(17) S44 0.041(3) 0.030(2) 0.0222(18) 0.0027(15) 0.0100(18) -0.0082(18) S45 0.040(3) 0.033(2) 0.0259(19) 0.0067(16) 0.0045(19) -0.0106(18) S46 0.039(3) 0.037(2) 0.0209(18) 0.0051(16) 0.0029(18) -0.0123(19) S47 0.054(3) 0.037(2) 0.045(2) 0.0085(18) 0.014(2) -0.014(2) S48 0.064(3) 0.054(3) 0.032(2) -0.0036(19) 0.005(2) -0.030(2) C51 0.034(11) 0.068(11) 0.033(9) -0.016(8) 0.003(9) -0.015(9) C52 0.067(14) 0.061(11) 0.040(10) -0.016(9) 0.014(10) -0.020(10) C53 0.022(9) 0.044(9) 0.022(7) 0.002(6) 0.002(7) -0.005(7) C54 0.025(9) 0.021(7) 0.027(8) -0.013(6) 0.002(7) -0.010(6) C55 0.010(8) 0.053(10) 0.030(8) -0.006(7) 0.012(7) 0.000(7) C56 0.016(8) 0.038(8) 0.035(8) -0.004(7) 0.003(7) -0.005(7) C57 0.026(9) 0.026(7) 0.039(9) 0.009(6) 0.009(7) -0.010(6) C58 0.015(8) 0.029(7) 0.030(8) 0.010(6) 0.007(7) -0.002(6) C59 0.067(12) 0.018(7) 0.036(8) -0.003(6) 0.020(8) -0.018(7) C60 0.079(13) 0.022(7) 0.019(7) 0.008(6) 0.014(8) -0.008(7) S51 0.070(4) 0.056(3) 0.031(2) -0.0038(19) -0.004(2) -0.023(2) S52 0.066(3) 0.038(2) 0.048(2) -0.0094(19) 0.027(2) -0.021(2) S53 0.045(3) 0.036(2) 0.030(2) 0.0046(17) 0.007(2) -0.0015(19) S54 0.043(3) 0.030(2) 0.033(2) 0.0026(16) 0.011(2) -0.0074(19) S55 0.047(3) 0.037(2) 0.029(2) 0.0054(17) 0.010(2) -0.0090(19) S56 0.050(3) 0.034(2) 0.032(2) 0.0059(17) 0.006(2) -0.0097(19) S57 0.054(3) 0.034(2) 0.041(2) 0.0085(17) 0.002(2) -0.010(2) S58 0.064(3) 0.037(2) 0.034(2) 0.0001(17) 0.013(2) -0.016(2) Fe1 0.0363(13) 0.0248(10) 0.0226(10) 0.0043(8) 0.0065(10) -0.0065(9) C101 0.038(10) 0.032(8) 0.017(7) 0.010(6) 0.011(7) -0.009(7) C102 0.034(10) 0.022(7) 0.029(8) -0.019(6) 0.008(8) -0.007(7) C103 0.026(9) 0.024(7) 0.030(8) 0.003(6) 0.014(8) -0.007(6) C104 0.041(10) 0.007(7) 0.047(9) -0.001(6) 0.018(8) -0.003(7) C105 0.026(9) 0.032(8) 0.024(7) -0.005(6) 0.015(7) -0.013(7) O101 0.033(6) 0.022(5) 0.015(4) -0.001(4) 0.003(4) -0.001(4) O102 0.055(8) 0.029(6) 0.042(6) -0.004(5) -0.005(6) -0.016(5) O103 0.035(7) 0.024(5) 0.040(6) -0.002(4) 0.002(6) -0.001(5) O104 0.049(7) 0.030(6) 0.033(5) 0.004(4) 0.008(5) -0.005(5) O105 0.038(6) 0.030(5) 0.026(5) 0.000(4) 0.014(5) -0.013(5) C106 0.028(8) 0.016(6) 0.017(6) 0.004(5) -0.004(6) -0.011(6) C107 0.019(8) 0.026(8) 0.034(8) 0.006(6) 0.002(7) 0.002(6) C108 0.049(11) 0.030(8) 0.031(8) -0.005(6) 0.001(8) -0.027(8) C109 0.024(8) 0.021(7) 0.030(7) 0.010(6) -0.004(7) 0.000(6) C110 0.040(10) 0.027(7) 0.020(7) 0.004(6) 0.002(7) -0.027(7) O106 0.034(6) 0.037(5) 0.031(5) 0.015(4) 0.014(5) -0.011(4) O107 0.034(6) 0.040(6) 0.046(6) 0.019(5) 0.012(5) -0.009(5) O108 0.047(7) 0.040(6) 0.045(6) 0.003(5) 0.023(6) -0.014(5) O109 0.057(8) 0.035(6) 0.036(5) 0.010(5) 0.015(6) -0.009(5) O110 0.028(6) 0.025(5) 0.033(5) 0.005(4) 0.011(5) 0.004(4) C111 0.017(8) 0.041(8) 0.021(7) 0.012(6) 0.012(6) -0.006(6) C112 0.022(9) 0.036(8) 0.035(8) 0.001(7) 0.007(7) -0.003(7) C113 0.029(10) 0.044(9) 0.048(11) -0.001(8) 0.016(8) 0.006(7) C114 0.025(9) 0.033(8) 0.034(8) 0.011(6) -0.007(7) -0.013(7) C115 0.038(9) 0.020(7) 0.034(8) 0.014(6) 0.005(7) -0.005(6) O111 0.030(6) 0.043(5) 0.026(5) 0.009(4) 0.004(5) -0.018(5) O112 0.057(8) 0.031(5) 0.039(6) -0.007(4) 0.005(6) -0.016(5) O113 0.084(10) 0.087(8) 0.024(6) -0.006(5) 0.016(6) -0.039(7) O114 0.055(8) 0.074(7) 0.048(6) 0.014(5) 0.018(6) -0.029(6) O115 0.036(6) 0.030(5) 0.025(5) -0.006(4) 0.005(5) -0.010(4) C1 0.032(9) 0.022(7) 0.049(10) 0.010(7) 0.005(8) 0.008(7) C2 0.041(10) 0.033(8) 0.033(9) 0.009(7) 0.005(8) -0.001(7) C3 0.049(11) 0.037(9) 0.045(9) 0.004(7) -0.001(9) -0.011(8) C4 0.041(11) 0.058(10) 0.071(12) 0.046(9) 0.004(10) -0.004(8) C5 0.063(14) 0.066(11) 0.034(10) 0.000(8) 0.016(10) -0.012(10) C6 0.045(11) 0.056(10) 0.037(9) 0.013(8) 0.015(9) -0.002(9) C7 0.038(11) 0.048(10) 0.049(10) 0.001(8) -0.021(9) -0.014(9) N8 0.062(12) 0.067(10) 0.084(12) 0.017(9) -0.007(10) -0.010(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 C11 C12 1.463(17) . ? C11 S11 1.748(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 S12 1.795(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.379(16) . ? C13 S13 1.704(11) . ? C13 S11 1.762(13) . ? C14 S12 1.724(11) . ? C14 S14 1.745(13) . ? C15 C16 1.399(16) . ? C15 S14 1.710(12) . ? C15 S13 1.742(13) . ? C16 S15 1.690(11) . ? C16 S16 1.732(12) . ? C17 C18 1.346(17) . ? C17 S15 1.730(13) . ? C17 S17 1.748(12) . ? C18 S16 1.721(11) . ? C18 S18 1.755(13) . ? C19 C20 1.557(19) . ? C19 S17 1.765(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 S18 1.769(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.528(17) . ? C21 S21 1.780(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 S22 1.793(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.366(16) . ? C23 S23 1.707(10) . ? C23 S21 1.783(12) . ? C24 S22 1.723(10) . ? C24 S24 1.729(12) . ? C25 C26 1.361(16) . ? C25 S24 1.719(11) . ? C25 S23 1.743(13) . ? C26 S25 1.707(11) . ? C26 S26 1.747(13) . ? C27 C28 1.355(17) . ? C27 S27 1.732(11) . ? C27 S25 1.742(13) . ? C28 S26 1.723(11) . ? C28 S28 1.763(13) . ? C29 C30 1.493(17) . ? C29 S27 1.780(14) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 S28 1.806(13) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.32(2) . ? C31 S31 1.724(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 S32 1.811(15) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.351(16) . ? C33 S33 1.742(11) . ? C33 S31 1.751(12) . ? C34 S32 1.739(12) . ? C34 S34 1.757(13) . ? C35 C36 1.316(15) . ? C35 S33 1.736(12) . ? C35 S34 1.752(11) . ? C36 S36 1.765(12) . ? C36 S35 1.770(10) . ? C37 C38 1.366(18) . ? C37 S37 1.724(12) . ? C37 S35 1.766(14) . ? C38 S38 1.728(13) . ? C38 S36 1.753(12) . ? C39 C40 1.531(17) . ? C39 S37 1.808(13) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 S38 1.800(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.534(16) . ? C41 S41 1.766(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 S42 1.804(14) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.355(16) . ? C43 S41 1.742(12) . ? C43 S43 1.747(12) . ? C44 S42 1.736(11) . ? C44 S44 1.736(13) . ? C45 C46 1.343(17) . ? C45 S44 1.709(12) . ? C45 S43 1.736(14) . ? C46 S45 1.732(12) . ? C46 S46 1.755(15) . ? C47 C48 1.409(17) . ? C47 S47 1.689(12) . ? C47 S45 1.721(14) . ? C48 S46 1.729(12) . ? C48 S48 1.744(14) . ? C49 C50 1.40(2) . ? C49 S47 1.759(15) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 S48 1.74(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.41(2) . ? C51 S51 1.701(15) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 S52 1.814(16) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.356(17) . ? C53 S53 1.720(13) . ? C53 S51 1.748(14) . ? C54 S52 1.731(12) . ? C54 S54 1.786(13) . ? C55 C56 1.349(18) . ? C55 S54 1.710(14) . ? C55 S53 1.777(14) . ? C56 S55 1.742(13) . ? C56 S56 1.754(14) . ? C57 C58 1.338(17) . ? C57 S55 1.734(14) . ? C57 S57 1.737(13) . ? C58 S56 1.746(12) . ? C58 S58 1.772(13) . ? C59 C60 1.476(19) . ? C59 S57 1.827(14) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 S58 1.774(11) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? Fe1 O111 2.001(8) . ? Fe1 O110 2.014(7) . ? Fe1 O101 2.022(8) . ? Fe1 O105 2.025(9) . ? Fe1 O115 2.056(8) . ? Fe1 O106 2.057(9) . ? C101 O101 1.295(15) . ? C101 C105 1.403(17) . ? C101 C102 1.437(19) . ? C102 O102 1.239(14) . ? C102 C103 1.514(18) . ? C103 O103 1.218(15) . ? C103 C104 1.518(18) . ? C104 O104 1.232(14) . ? C104 C105 1.436(19) . ? C105 O105 1.303(15) . ? C106 O106 1.308(12) . ? C106 C110 1.400(15) . ? C106 C107 1.460(17) . ? C107 O107 1.207(13) . ? C107 C108 1.496(18) . ? C108 O108 1.215(16) . ? C108 C109 1.508(19) . ? C109 O109 1.229(12) . ? C109 C110 1.445(17) . ? C110 O110 1.292(15) . ? C111 O111 1.313(12) . ? C111 C115 1.417(16) . ? C111 C112 1.462(18) . ? C112 O112 1.217(15) . ? C112 C113 1.484(18) . ? C113 O113 1.244(16) . ? C113 C114 1.500(19) . ? C114 O114 1.225(13) . ? C114 C115 1.450(18) . ? C115 O115 1.285(15) . ? C1 C2 1.386(19) . ? C1 C7 1.42(2) . ? C1 C6 1.431(18) . ? C2 C3 1.395(19) . ? C2 H2 0.9500 . ? C3 C4 1.379(18) . ? C3 H3 0.9500 . ? C4 C5 1.42(2) . ? C4 H4 0.9500 . ? C5 C6 1.34(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N8 1.121(18) . ? 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 C12 C11 S11 118.0(11) . . ? C12 C11 H11A 107.8 . . ? S11 C11 H11A 107.8 . . ? C12 C11 H11B 107.8 . . ? S11 C11 H11B 107.8 . . ? H11A C11 H11B 107.1 . . ? C11 C12 S12 117.3(10) . . ? C11 C12 H12A 108.0 . . ? S12 C12 H12A 108.0 . . ? C11 C12 H12B 108.0 . . ? S12 C12 H12B 108.0 . . ? H12A C12 H12B 107.2 . . ? C14 C13 S13 118.7(10) . . ? C14 C13 S11 126.4(9) . . ? S13 C13 S11 114.9(6) . . ? C13 C14 S12 130.1(10) . . ? C13 C14 S14 114.1(9) . . ? S12 C14 S14 115.8(7) . . ? C16 C15 S14 126.0(9) . . ? C16 C15 S13 118.8(8) . . ? S14 C15 S13 115.1(7) . . ? C15 C16 S15 122.7(9) . . ? C15 C16 S16 121.2(8) . . ? S15 C16 S16 116.1(7) . . ? C18 C17 S15 116.1(9) . . ? C18 C17 S17 125.9(10) . . ? S15 C17 S17 117.8(7) . . ? C17 C18 S16 117.4(10) . . ? C17 C18 S18 126.8(9) . . ? S16 C18 S18 115.8(7) . . ? C20 C19 S17 112.5(10) . . ? C20 C19 H19A 109.1 . . ? S17 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? S17 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 S18 114.8(9) . . ? C19 C20 H20A 108.6 . . ? S18 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? S18 C20 H20B 108.6 . . ? H20A C20 H20B 107.5 . . ? C11 S11 C13 101.9(6) . . ? C14 S12 C12 100.5(6) . . ? C13 S13 C15 95.2(6) . . ? C15 S14 C14 96.6(6) . . ? C16 S15 C17 95.7(6) . . ? C18 S16 C16 94.5(6) . . ? C17 S17 C19 96.3(6) . . ? C18 S18 C20 105.2(6) . . ? C22 C21 S21 114.9(10) . . ? C22 C21 H21A 108.5 . . ? S21 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? S21 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 S22 114.5(9) . . ? C21 C22 H22A 108.6 . . ? S22 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? S22 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C24 C23 S23 119.2(9) . . ? C24 C23 S21 124.3(8) . . ? S23 C23 S21 116.3(6) . . ? C23 C24 S22 130.8(9) . . ? C23 C24 S24 114.1(8) . . ? S22 C24 S24 115.1(7) . . ? C26 C25 S24 122.8(10) . . ? C26 C25 S23 123.0(8) . . ? S24 C25 S23 114.2(7) . . ? C25 C26 S25 125.0(10) . . ? C25 C26 S26 120.9(8) . . ? S25 C26 S26 114.1(7) . . ? C28 C27 S27 130.0(10) . . ? C28 C27 S25 114.2(8) . . ? S27 C27 S25 115.7(7) . . ? C27 C28 S26 118.7(10) . . ? C27 C28 S28 126.4(9) . . ? S26 C28 S28 114.9(7) . . ? C30 C29 S27 114.1(10) . . ? C30 C29 H29A 108.7 . . ? S27 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? S27 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C29 C30 S28 114.8(10) . . ? C29 C30 H30A 108.6 . . ? S28 C30 H30A 108.6 . . ? C29 C30 H30B 108.6 . . ? S28 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C21 S21 C23 100.2(6) . . ? C24 S22 C22 104.2(6) . . ? C23 S23 C25 95.1(5) . . ? C25 S24 C24 97.3(6) . . ? C26 S25 C27 97.7(6) . . ? C28 S26 C26 95.3(6) . . ? C27 S27 C29 101.2(6) . . ? C28 S28 C30 101.6(6) . . ? C32 C31 S31 126.3(15) . . ? C32 C31 H31A 105.7 . . ? S31 C31 H31A 105.7 . . ? C32 C31 H31B 105.7 . . ? S31 C31 H31B 105.7 . . ? H31A C31 H31B 106.2 . . ? C31 C32 S32 122.5(13) . . ? C31 C32 H32A 106.7 . . ? S32 C32 H32A 106.7 . . ? C31 C32 H32B 106.7 . . ? S32 C32 H32B 106.7 . . ? H32A C32 H32B 106.6 . . ? C34 C33 S33 118.3(9) . . ? C34 C33 S31 126.6(9) . . ? S33 C33 S31 114.9(7) . . ? C33 C34 S32 129.4(10) . . ? C33 C34 S34 116.1(9) . . ? S32 C34 S34 114.5(7) . . ? C36 C35 S33 122.4(8) . . ? C36 C35 S34 121.9(9) . . ? S33 C35 S34 115.6(6) . . ? C35 C36 S36 123.0(8) . . ? C35 C36 S35 125.0(9) . . ? S36 C36 S35 112.0(6) . . ? C38 C37 S37 128.3(10) . . ? C38 C37 S35 115.7(9) . . ? S37 C37 S35 115.8(7) . . ? C37 C38 S38 128.6(9) . . ? C37 C38 S36 117.1(10) . . ? S38 C38 S36 114.3(7) . . ? C40 C39 S37 114.2(10) . . ? C40 C39 H39A 108.7 . . ? S37 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? S37 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 S38 114.8(9) . . ? C39 C40 H40A 108.6 . . ? S38 C40 H40A 108.6 . . ? C39 C40 H40B 108.6 . . ? S38 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C31 S31 C33 101.8(7) . . ? C34 S32 C32 101.8(6) . . ? C35 S33 C33 94.3(5) . . ? C35 S34 C34 94.6(6) . . ? C37 S35 C36 95.7(6) . . ? C38 S36 C36 95.7(6) . . ? C37 S37 C39 99.6(6) . . ? C38 S38 C40 103.9(6) . . ? C42 C41 S41 115.6(10) . . ? C42 C41 H41A 108.4 . . ? S41 C41 H41A 108.4 . . ? C42 C41 H41B 108.4 . . ? S41 C41 H41B 108.4 . . ? H41A C41 H41B 107.4 . . ? C41 C42 S42 113.2(9) . . ? C41 C42 H42A 108.9 . . ? S42 C42 H42A 108.9 . . ? C41 C42 H42B 108.9 . . ? S42 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C44 C43 S41 126.6(9) . . ? C44 C43 S43 116.5(9) . . ? S41 C43 S43 116.7(7) . . ? C43 C44 S42 129.8(10) . . ? C43 C44 S44 116.8(9) . . ? S42 C44 S44 113.4(7) . . ? C46 C45 S44 123.8(11) . . ? C46 C45 S43 120.4(9) . . ? S44 C45 S43 115.8(7) . . ? C45 C46 S45 124.0(11) . . ? C45 C46 S46 122.2(9) . . ? S45 C46 S46 113.8(8) . . ? C48 C47 S47 128.0(10) . . ? C48 C47 S45 114.1(9) . . ? S47 C47 S45 117.7(7) . . ? C47 C48 S46 117.8(10) . . ? C47 C48 S48 124.4(9) . . ? S46 C48 S48 117.8(7) . . ? C50 C49 S47 119.5(12) . . ? C50 C49 H49A 107.5 . . ? S47 C49 H49A 107.5 . . ? C50 C49 H49B 107.5 . . ? S47 C49 H49B 107.5 . . ? H49A C49 H49B 107.0 . . ? C49 C50 S48 125.3(14) . . ? C49 C50 H50A 106.0 . . ? S48 C50 H50A 106.0 . . ? C49 C50 H50B 106.0 . . ? S48 C50 H50B 106.0 . . ? H50A C50 H50B 106.3 . . ? C43 S41 C41 97.5(6) . . ? C44 S42 C42 103.4(6) . . ? C45 S43 C43 94.9(6) . . ? C45 S44 C44 95.8(6) . . ? C47 S45 C46 98.3(7) . . ? C48 S46 C46 95.8(6) . . ? C47 S47 C49 105.7(7) . . ? C50 S48 C48 98.0(8) . . ? C52 C51 S51 123.1(13) . . ? C52 C51 H51A 106.6 . . ? S51 C51 H51A 106.6 . . ? C52 C51 H51B 106.6 . . ? S51 C51 H51B 106.6 . . ? H51A C51 H51B 106.5 . . ? C51 C52 S52 118.6(12) . . ? C51 C52 H52A 107.7 . . ? S52 C52 H52A 107.7 . . ? C51 C52 H52B 107.7 . . ? S52 C52 H52B 107.7 . . ? H52A C52 H52B 107.1 . . ? C54 C53 S53 119.1(11) . . ? C54 C53 S51 127.1(10) . . ? S53 C53 S51 113.0(7) . . ? C53 C54 S52 129.3(10) . . ? C53 C54 S54 114.7(9) . . ? S52 C54 S54 115.9(7) . . ? C56 C55 S54 127.2(11) . . ? C56 C55 S53 117.7(10) . . ? S54 C55 S53 115.1(8) . . ? C55 C56 S55 124.7(11) . . ? C55 C56 S56 120.9(10) . . ? S55 C56 S56 114.3(8) . . ? C58 C57 S55 115.5(10) . . ? C58 C57 S57 126.9(11) . . ? S55 C57 S57 117.6(7) . . ? C57 C58 S56 119.2(10) . . ? C57 C58 S58 123.1(10) . . ? S56 C58 S58 117.6(7) . . ? C60 C59 S57 116.7(9) . . ? C60 C59 H59A 108.1 . . ? S57 C59 H59A 108.1 . . ? C60 C59 H59B 108.1 . . ? S57 C59 H59B 108.1 . . ? H59A C59 H59B 107.3 . . ? C59 C60 S58 115.9(11) . . ? C59 C60 H60A 108.3 . . ? S58 C60 H60A 108.3 . . ? C59 C60 H60B 108.3 . . ? S58 C60 H60B 108.3 . . ? H60A C60 H60B 107.4 . . ? C51 S51 C53 102.8(7) . . ? C54 S52 C52 100.0(7) . . ? C53 S53 C55 94.0(6) . . ? C55 S54 C54 95.3(7) . . ? C57 S55 C56 94.3(6) . . ? C58 S56 C56 92.2(6) . . ? C57 S57 C59 104.0(6) . . ? C58 S58 C60 96.4(6) . . ? O111 Fe1 O110 93.0(3) . . ? O111 Fe1 O101 167.1(3) . . ? O110 Fe1 O101 98.6(3) . . ? O111 Fe1 O105 91.9(4) . . ? O110 Fe1 O105 88.2(3) . . ? O101 Fe1 O105 82.8(4) . . ? O111 Fe1 O115 83.1(3) . . ? O110 Fe1 O115 175.9(4) . . ? O101 Fe1 O115 85.4(3) . . ? O105 Fe1 O115 93.5(3) . . ? O111 Fe1 O106 98.9(4) . . ? O110 Fe1 O106 82.1(3) . . ? O101 Fe1 O106 88.4(3) . . ? O105 Fe1 O106 165.8(3) . . ? O115 Fe1 O106 96.9(3) . . ? O101 C101 C105 120.1(13) . . ? O101 C101 C102 129.3(12) . . ? C105 C101 C102 110.6(12) . . ? O102 C102 C101 130.6(13) . . ? O102 C102 C103 123.1(13) . . ? C101 C102 C103 106.3(11) . . ? O103 C103 C102 126.6(12) . . ? O103 C103 C104 127.1(12) . . ? C102 C103 C104 106.1(12) . . ? O104 C104 C105 130.1(12) . . ? O104 C104 C103 123.8(13) . . ? C105 C104 C103 106.0(11) . . ? O105 C105 C101 118.6(13) . . ? O105 C105 C104 130.3(11) . . ? C101 C105 C104 110.9(12) . . ? C101 O101 Fe1 109.0(7) . . ? C105 O105 Fe1 109.4(8) . . ? O106 C106 C110 119.4(11) . . ? O106 C106 C107 128.6(10) . . ? C110 C106 C107 112.0(10) . . ? O107 C107 C106 129.9(11) . . ? O107 C107 C108 126.4(12) . . ? C106 C107 C108 103.7(11) . . ? O108 C108 C107 125.5(13) . . ? O108 C108 C109 125.4(11) . . ? C107 C108 C109 109.0(12) . . ? O109 C109 C110 130.2(12) . . ? O109 C109 C108 124.7(12) . . ? C110 C109 C108 105.1(10) . . ? O110 C110 C106 119.3(10) . . ? O110 C110 C109 130.4(10) . . ? C106 C110 C109 110.2(12) . . ? C106 O106 Fe1 108.3(7) . . ? C110 O110 Fe1 110.2(6) . . ? O111 C111 C115 119.3(12) . . ? O111 C111 C112 128.0(10) . . ? C115 C111 C112 112.7(10) . . ? O112 C112 C111 128.0(11) . . ? O112 C112 C113 128.8(13) . . ? C111 C112 C113 103.1(11) . . ? O113 C113 C112 124.5(14) . . ? O113 C113 C114 125.5(13) . . ? C112 C113 C114 109.9(12) . . ? O114 C114 C115 127.2(12) . . ? O114 C114 C113 127.2(12) . . ? C115 C114 C113 105.6(11) . . ? O115 C115 C111 119.4(11) . . ? O115 C115 C114 132.0(11) . . ? C111 C115 C114 108.5(12) . . ? C111 O111 Fe1 108.8(7) . . ? C115 O115 Fe1 107.7(7) . . ? C2 C1 C7 121.0(13) . . ? C2 C1 C6 117.9(13) . . ? C7 C1 C6 120.9(14) . . ? C1 C2 C3 119.8(13) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 121.6(15) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 118.8(14) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 119.7(14) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 122.1(15) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? N8 C7 C1 179(2) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.467 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.107