Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email KONCH@CHE.NSK.SU _publ_contact_author_name 'Dr Sergei Konchenko' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name S.Konchenko N.A.Pushkarevsky M.Scheer 'Alexander V.Virovets' data_new1 _database_code_CSD 196896 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H15 Fe3 O9 Sb Te' _chemical_formula_weight 804.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.872(2) _cell_length_b 36.208(7) _cell_length_c 14.072(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.73(3) _cell_angle_gamma 90.00 _cell_volume 4906.2(17) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1244 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 26.03 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 4.039 _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 200(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 IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27303 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.03 _reflns_number_total 9214 _reflns_number_gt 7416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SIEMENS-XP _computing_publication_material SHELXL-97 _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^)+(0.0618P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9214 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 Sb1 Sb 0.62378(3) 0.045999(7) 0.242399(18) 0.02702(8) Uani 1 1 d . . . Te1 Te 0.30452(3) 0.060309(8) 0.16339(2) 0.03522(8) Uani 1 1 d . . . Fe1 Fe 0.43727(7) 0.064884(18) 0.33709(4) 0.03288(15) Uani 1 1 d . . . Fe2 Fe 0.51051(7) 0.105555(17) 0.19062(4) 0.03242(14) Uani 1 1 d . . . Fe3 Fe 0.43264(7) 0.000985(17) 0.22807(4) 0.03185(14) Uani 1 1 d . . . C1 C 0.5808(6) 0.06684(14) 0.4386(3) 0.0419(11) Uani 1 1 d . . . O1 O 0.6683(5) 0.06832(13) 0.5062(3) 0.0645(11) Uani 1 1 d . . . C2 C 0.3314(6) 0.03636(17) 0.3935(4) 0.0519(14) Uani 1 1 d . . . O2 O 0.2614(6) 0.02000(15) 0.4339(3) 0.0821(16) Uani 1 1 d . . . C3 C 0.3583(6) 0.10746(16) 0.3562(3) 0.0495(13) Uani 1 1 d . . . O3 O 0.3031(5) 0.13445(12) 0.3693(3) 0.0713(13) Uani 1 1 d . . . C4 C 0.2679(6) -0.01936(14) 0.2356(4) 0.0455(12) Uani 1 1 d . . . O4 O 0.1650(4) -0.03244(12) 0.2402(4) 0.0682(12) Uani 1 1 d . . . C5 C 0.5303(5) -0.03085(13) 0.3139(4) 0.0387(10) Uani 1 1 d . . . O5 O 0.5877(4) -0.05182(11) 0.3680(3) 0.0564(10) Uani 1 1 d . . . C6 C 0.4522(6) -0.02038(14) 0.1189(4) 0.0438(11) Uani 1 1 d . . . O6 O 0.4627(5) -0.03443(12) 0.0482(3) 0.0627(11) Uani 1 1 d . . . C7 C 0.5743(5) 0.10817(13) 0.0830(3) 0.0376(10) Uani 1 1 d . . . O7 O 0.6195(4) 0.11151(10) 0.0148(2) 0.0514(9) Uani 1 1 d . . . C8 C 0.6367(6) 0.13484(14) 0.2646(4) 0.0481(13) Uani 1 1 d . . . O8 O 0.7123(6) 0.15478(13) 0.3104(3) 0.0768(14) Uani 1 1 d . . . C9 C 0.3857(6) 0.14230(14) 0.1655(4) 0.0505(13) Uani 1 1 d . . . O9 O 0.3093(5) 0.16637(13) 0.1478(4) 0.0788(15) Uani 1 1 d . . . C10 C 0.8527(5) 0.03462(12) 0.2849(3) 0.0310(9) Uani 1 1 d . . . C11 C 0.8530(5) 0.02251(12) 0.1828(3) 0.0352(10) Uani 1 1 d . . . C12 C 0.8926(5) 0.05206(13) 0.1355(3) 0.0363(10) Uani 1 1 d . . . C13 C 0.9291(5) 0.08239(13) 0.2025(3) 0.0356(10) Uani 1 1 d . . . C14 C 0.9103(5) 0.07264(12) 0.2917(3) 0.0336(9) Uani 1 1 d . . . C15 C 0.8912(6) 0.00813(14) 0.3689(4) 0.0452(12) Uani 1 1 d . . . H15A H 0.9886 0.0008 0.3768 0.068 Uiso 1 1 calc R . . H15B H 0.8318 -0.0138 0.3559 0.068 Uiso 1 1 calc R . . H15C H 0.8782 0.0201 0.4286 0.068 Uiso 1 1 calc R . . C16 C 0.8221(6) -0.01592(15) 0.1472(4) 0.0503(13) Uani 1 1 d . . . H16A H 0.7513 -0.0266 0.1780 0.075 Uiso 1 1 calc R . . H16B H 0.9069 -0.0308 0.1636 0.075 Uiso 1 1 calc R . . H16C H 0.7876 -0.0156 0.0763 0.075 Uiso 1 1 calc R . . C17 C 0.9010(6) 0.05367(17) 0.0299(3) 0.0499(13) Uani 1 1 d . . . H17A H 0.9931 0.0625 0.0252 0.075 Uiso 1 1 calc R . . H17B H 0.8299 0.0706 -0.0053 0.075 Uiso 1 1 calc R . . H17C H 0.8856 0.0289 0.0012 0.075 Uiso 1 1 calc R . . C18 C 0.9755(6) 0.12010(15) 0.1742(4) 0.0508(13) Uani 1 1 d . . . H18A H 0.8950 0.1336 0.1370 0.076 Uiso 1 1 calc R . . H18B H 1.0442 0.1170 0.1341 0.076 Uiso 1 1 calc R . . H18C H 1.0170 0.1340 0.2331 0.076 Uiso 1 1 calc R . . C19 C 0.9475(6) 0.09319(16) 0.3853(4) 0.0505(13) Uani 1 1 d . . . H19A H 1.0258 0.0809 0.4288 0.076 Uiso 1 1 calc R . . H19B H 0.8676 0.0936 0.4160 0.076 Uiso 1 1 calc R . . H19C H 0.9738 0.1185 0.3728 0.076 Uiso 1 1 calc R . . Sb2 Sb 0.08902(3) 0.182128(7) 0.735017(18) 0.02737(8) Uani 1 1 d . . . Te2 Te 0.37999(3) 0.212893(8) 0.71242(2) 0.03556(8) Uani 1 1 d . . . Fe4 Fe 0.33507(7) 0.164512(17) 0.83051(4) 0.03148(14) Uani 1 1 d . . . Fe5 Fe 0.24084(7) 0.157096(17) 0.63271(4) 0.03005(14) Uani 1 1 d . . . Fe6 Fe 0.21907(7) 0.234426(17) 0.82200(4) 0.03201(14) Uani 1 1 d . . . C20 C 0.2433(6) 0.13211(14) 0.8882(3) 0.0436(11) Uani 1 1 d . . . O10 O 0.1932(5) 0.11036(12) 0.9280(3) 0.0674(12) Uani 1 1 d . . . C21 C 0.4594(6) 0.13174(15) 0.8082(3) 0.0465(12) Uani 1 1 d . . . O11 O 0.5414(5) 0.11053(12) 0.7989(3) 0.0639(12) Uani 1 1 d . . . C22 C 0.4355(6) 0.18451(14) 0.9377(3) 0.0457(12) Uani 1 1 d . . . O12 O 0.5061(5) 0.19500(12) 1.0076(3) 0.0693(13) Uani 1 1 d . . . C23 C 0.1663(5) 0.11226(13) 0.6298(3) 0.0364(10) Uani 1 1 d . . . O13 O 0.1175(5) 0.08374(10) 0.6287(3) 0.0557(10) Uani 1 1 d . . . C24 C 0.3960(5) 0.14160(14) 0.5957(3) 0.0398(11) Uani 1 1 d . . . O14 O 0.4927(4) 0.13202(12) 0.5721(3) 0.0567(10) Uani 1 1 d . . . C25 C 0.1486(5) 0.17410(12) 0.5188(3) 0.0349(10) Uani 1 1 d . . . O15 O 0.0889(4) 0.18433(10) 0.4451(2) 0.0472(9) Uani 1 1 d . . . C26 C 0.1454(6) 0.23205(14) 0.9269(3) 0.0434(12) Uani 1 1 d . . . O16 O 0.1057(5) 0.23117(12) 0.9971(3) 0.0601(11) Uani 1 1 d . . . C27 C 0.1119(6) 0.26928(13) 0.7529(4) 0.0412(11) Uani 1 1 d . . . O17 O 0.0452(5) 0.29126(10) 0.7099(3) 0.0570(10) Uani 1 1 d . . . C28 C 0.3544(6) 0.26437(14) 0.8826(4) 0.0455(12) Uani 1 1 d . . . O18 O 0.4394(5) 0.28427(12) 0.9222(3) 0.0688(12) Uani 1 1 d . . . C29 C -0.1236(5) 0.16204(13) 0.7439(3) 0.0359(10) Uani 1 1 d . . . C30 C -0.1867(5) 0.18692(15) 0.6615(3) 0.0392(11) Uani 1 1 d . . . C31 C -0.2260(5) 0.21831(14) 0.6989(3) 0.0379(10) Uani 1 1 d . . . C32 C -0.1989(5) 0.21521(12) 0.8054(3) 0.0364(10) Uani 1 1 d . . . C33 C -0.1435(5) 0.18157(13) 0.8323(3) 0.0360(10) Uani 1 1 d . . . C34 C -0.1397(6) 0.12089(15) 0.7352(4) 0.0507(13) Uani 1 1 d . . . H34A H -0.1151 0.1126 0.6748 0.076 Uiso 1 1 calc R . . H34B H -0.2362 0.1142 0.7339 0.076 Uiso 1 1 calc R . . H34C H -0.0782 0.1090 0.7910 0.076 Uiso 1 1 calc R . . C35 C -0.2079(6) 0.17594(17) 0.5570(3) 0.0514(13) Uani 1 1 d . . . H35A H -0.2895 0.1598 0.5396 0.077 Uiso 1 1 calc R . . H35B H -0.1258 0.1627 0.5468 0.077 Uiso 1 1 calc R . . H35C H -0.2225 0.1981 0.5159 0.077 Uiso 1 1 calc R . . C36 C -0.2857(6) 0.25211(16) 0.6450(4) 0.0550(14) Uani 1 1 d . . . H36A H -0.2139 0.2712 0.6520 0.082 Uiso 1 1 calc R . . H36B H -0.3631 0.2612 0.6717 0.082 Uiso 1 1 calc R . . H36C H -0.3191 0.2461 0.5759 0.082 Uiso 1 1 calc R . . C37 C -0.2319(7) 0.24522(17) 0.8695(4) 0.0574(15) Uani 1 1 d . . . H37A H -0.3321 0.2501 0.8533 0.086 Uiso 1 1 calc R . . H37B H -0.1818 0.2677 0.8594 0.086 Uiso 1 1 calc R . . H37C H -0.2036 0.2376 0.9378 0.086 Uiso 1 1 calc R . . C38 C -0.1120(6) 0.16465(16) 0.9313(4) 0.0532(14) Uani 1 1 d . . . H38A H -0.0182 0.1542 0.9447 0.080 Uiso 1 1 calc R . . H38B H -0.1795 0.1451 0.9342 0.080 Uiso 1 1 calc R . . H38C H -0.1177 0.1836 0.9800 0.080 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 Sb1 0.02658(17) 0.02679(14) 0.02723(13) -0.00045(10) 0.00493(11) 0.00022(10) Te1 0.03008(19) 0.03831(17) 0.03478(15) 0.00006(11) 0.00178(12) 0.00392(12) Fe1 0.0339(4) 0.0371(3) 0.0290(3) -0.0019(2) 0.0100(3) 0.0017(3) Fe2 0.0375(4) 0.0287(3) 0.0314(3) 0.0008(2) 0.0083(3) 0.0039(3) Fe3 0.0293(4) 0.0310(3) 0.0344(3) -0.0017(2) 0.0052(3) -0.0019(2) C1 0.049(3) 0.049(3) 0.030(2) -0.0055(19) 0.013(2) 0.008(2) O1 0.055(3) 0.096(3) 0.038(2) -0.0094(19) -0.0004(19) 0.011(2) C2 0.053(4) 0.063(4) 0.042(3) -0.007(2) 0.015(3) -0.014(3) O2 0.092(4) 0.103(4) 0.061(3) -0.003(2) 0.038(3) -0.046(3) C3 0.054(4) 0.064(4) 0.031(2) -0.005(2) 0.010(2) 0.011(3) O3 0.092(4) 0.071(3) 0.052(2) -0.017(2) 0.018(2) 0.039(3) C4 0.038(3) 0.041(3) 0.056(3) 0.004(2) 0.007(2) -0.001(2) O4 0.040(3) 0.056(3) 0.110(4) 0.003(2) 0.020(3) -0.0131(19) C5 0.039(3) 0.033(2) 0.046(2) 0.002(2) 0.012(2) -0.003(2) O5 0.055(3) 0.049(2) 0.061(2) 0.0178(18) 0.004(2) 0.0027(18) C6 0.040(3) 0.045(3) 0.044(3) -0.007(2) 0.004(2) -0.008(2) O6 0.077(3) 0.065(3) 0.048(2) -0.0215(19) 0.017(2) -0.012(2) C7 0.042(3) 0.035(2) 0.034(2) 0.0045(18) 0.003(2) 0.004(2) O7 0.061(3) 0.056(2) 0.0390(18) 0.0121(16) 0.0150(18) 0.0088(18) C8 0.062(4) 0.035(3) 0.047(3) -0.001(2) 0.011(3) 0.000(2) O8 0.086(4) 0.053(3) 0.081(3) -0.023(2) -0.005(3) -0.016(2) C9 0.058(4) 0.036(3) 0.061(3) 0.008(2) 0.022(3) 0.001(2) O9 0.075(4) 0.060(3) 0.111(4) 0.027(3) 0.042(3) 0.036(2) C10 0.025(3) 0.035(2) 0.032(2) 0.0021(17) 0.0032(18) -0.0046(17) C11 0.029(3) 0.032(2) 0.042(2) -0.0051(18) 0.005(2) 0.0006(18) C12 0.026(3) 0.049(3) 0.032(2) 0.0005(19) 0.0036(19) 0.0045(19) C13 0.027(3) 0.037(2) 0.042(2) 0.0072(18) 0.006(2) 0.0004(18) C14 0.028(3) 0.035(2) 0.035(2) -0.0030(17) 0.0010(19) -0.0034(18) C15 0.034(3) 0.045(3) 0.054(3) 0.015(2) 0.003(2) 0.002(2) C16 0.035(3) 0.049(3) 0.064(3) -0.016(2) 0.007(3) 0.002(2) C17 0.041(3) 0.073(4) 0.035(2) -0.001(2) 0.009(2) 0.003(3) C18 0.044(3) 0.047(3) 0.062(3) 0.016(2) 0.012(3) -0.003(2) C19 0.050(4) 0.056(3) 0.042(3) -0.012(2) 0.002(2) -0.012(3) Sb2 0.02818(17) 0.02810(15) 0.02644(13) -0.00193(10) 0.00733(11) -0.00049(10) Te2 0.03361(19) 0.03636(17) 0.03849(15) -0.00363(11) 0.01183(13) -0.00574(12) Fe4 0.0323(4) 0.0319(3) 0.0282(3) -0.0030(2) 0.0020(3) 0.0022(3) Fe5 0.0327(4) 0.0319(3) 0.0263(3) -0.0024(2) 0.0079(3) 0.0013(2) Fe6 0.0364(4) 0.0278(3) 0.0318(3) -0.0038(2) 0.0075(3) -0.0011(3) C20 0.042(3) 0.041(3) 0.042(2) 0.007(2) -0.005(2) 0.007(2) O10 0.061(3) 0.064(3) 0.074(3) 0.034(2) 0.008(2) -0.004(2) C21 0.046(3) 0.056(3) 0.033(2) -0.001(2) 0.000(2) 0.010(3) O11 0.068(3) 0.075(3) 0.047(2) -0.0029(18) 0.008(2) 0.041(2) C22 0.053(4) 0.040(3) 0.039(2) 0.000(2) -0.001(2) -0.002(2) O12 0.088(4) 0.055(2) 0.047(2) -0.0092(18) -0.025(2) -0.011(2) C23 0.044(3) 0.031(2) 0.034(2) -0.0029(17) 0.007(2) 0.011(2) O13 0.066(3) 0.033(2) 0.069(2) -0.0025(16) 0.018(2) -0.0012(18) C24 0.044(3) 0.045(3) 0.030(2) -0.0067(18) 0.008(2) 0.002(2) O14 0.046(3) 0.070(3) 0.059(2) -0.0141(19) 0.022(2) 0.0077(19) C25 0.040(3) 0.033(2) 0.034(2) -0.0033(18) 0.013(2) -0.0021(19) O15 0.060(3) 0.046(2) 0.0337(17) 0.0084(14) 0.0068(16) 0.0015(17) C26 0.056(3) 0.037(3) 0.035(2) -0.0087(19) 0.005(2) 0.000(2) O16 0.085(3) 0.065(3) 0.0359(18) -0.0052(16) 0.025(2) -0.006(2) C27 0.047(3) 0.033(2) 0.046(3) -0.004(2) 0.015(2) -0.002(2) O17 0.066(3) 0.038(2) 0.064(2) 0.0109(17) 0.009(2) 0.0120(19) C28 0.046(3) 0.038(3) 0.051(3) -0.011(2) 0.009(2) 0.006(2) O18 0.055(3) 0.053(2) 0.090(3) -0.027(2) -0.002(2) -0.010(2) C29 0.032(3) 0.038(3) 0.041(2) 0.0007(19) 0.015(2) -0.0029(19) C30 0.029(3) 0.054(3) 0.034(2) 0.003(2) 0.006(2) -0.007(2) C31 0.027(3) 0.046(3) 0.041(2) 0.010(2) 0.008(2) 0.0019(19) C32 0.041(3) 0.031(2) 0.041(2) 0.0000(18) 0.018(2) -0.0001(19) C33 0.031(3) 0.046(3) 0.034(2) 0.0081(19) 0.014(2) 0.0015(19) C34 0.042(3) 0.043(3) 0.067(3) -0.007(2) 0.013(3) -0.011(2) C35 0.042(3) 0.074(4) 0.036(2) -0.005(2) 0.005(2) -0.007(3) C36 0.048(4) 0.060(4) 0.058(3) 0.023(3) 0.014(3) 0.009(3) C37 0.058(4) 0.060(4) 0.061(3) -0.008(3) 0.027(3) 0.015(3) C38 0.059(4) 0.065(4) 0.040(3) 0.016(2) 0.019(3) 0.005(3) _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 Sb1 Te1 3.1454(9) . ? Sb1 Fe1 2.5912(9) . ? Sb1 Fe2 2.4641(8) . ? Sb1 Fe3 2.4677(8) . ? Sb1 C10 2.245(5) . ? Te1 Fe1 2.5115(10) . ? Te1 Fe2 2.5735(8) . ? Te1 Fe3 2.5563(8) . ? Fe1 Fe2 2.7561(10) . ? Fe1 Fe3 2.7709(10) . ? Fe1 C1 1.778(5) . ? Fe1 C2 1.776(5) . ? Fe1 C3 1.774(6) . ? Fe2 C7 1.766(4) . ? Fe2 C8 1.785(6) . ? Fe2 C9 1.795(6) . ? Fe3 C4 1.810(5) . ? Fe3 C5 1.790(5) . ? Fe3 C6 1.769(5) . ? C1 O1 1.136(6) . ? C2 O2 1.151(6) . ? C3 O3 1.153(6) . ? C4 O4 1.135(6) . ? C5 O5 1.134(6) . ? C6 O6 1.142(6) . ? C7 O7 1.151(5) . ? C8 O8 1.133(7) . ? C9 O9 1.144(7) . ? C10 C11 1.502(6) . ? C10 C14 1.485(6) . ? C10 C15 1.504(6) . ? C11 C12 1.363(7) . ? C11 C16 1.488(7) . ? C12 C13 1.441(7) . ? C12 C17 1.507(6) . ? C13 C14 1.355(6) . ? C13 C18 1.521(7) . ? C14 C19 1.487(6) . ? Sb2 Te2 3.1616(7) . ? Sb2 Fe4 2.5834(11) . ? Sb2 Fe5 2.4681(8) . ? Sb2 Fe6 2.4575(8) . ? Sb2 C29 2.251(4) . ? Te2 Fe4 2.5202(8) . ? Te2 Fe5 2.5588(8) . ? Te2 Fe6 2.5668(9) . ? Fe4 Fe5 2.7465(11) . ? Fe4 Fe6 2.7700(10) . ? Fe4 C20 1.784(5) . ? Fe4 C21 1.784(5) . ? Fe4 C22 1.767(5) . ? Fe5 C23 1.779(5) . ? Fe5 C24 1.811(5) . ? Fe5 C25 1.770(5) . ? Fe6 C26 1.785(5) . ? Fe6 C27 1.790(5) . ? Fe6 C28 1.785(6) . ? C20 O10 1.140(6) . ? C21 O11 1.145(6) . ? C22 O12 1.139(6) . ? C23 O13 1.138(6) . ? C24 O14 1.133(6) . ? C25 O15 1.136(6) . ? C26 O16 1.141(6) . ? C27 O17 1.121(6) . ? C28 O18 1.152(7) . ? C29 C30 1.493(7) . ? C29 C33 1.481(6) . ? C29 C34 1.500(7) . ? C30 C31 1.346(7) . ? C30 C35 1.493(6) . ? C31 C32 1.466(6) . ? C31 C36 1.491(7) . ? C32 C33 1.354(7) . ? C32 C37 1.494(7) . ? C33 C38 1.490(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 Sb1 Te1 50.81(2) . . ? Fe2 Sb1 Te1 52.936(19) . . ? Fe2 Sb1 Fe1 66.02(2) . . ? Fe2 Sb1 Fe3 105.36(3) . . ? Fe3 Sb1 Te1 52.51(2) . . ? Fe3 Sb1 Fe1 66.37(2) . . ? C10 Sb1 Te1 174.83(10) . . ? C10 Sb1 Fe1 134.36(11) . . ? C10 Sb1 Fe2 127.16(11) . . ? C10 Sb1 Fe3 127.39(11) . . ? Fe1 Te1 Sb1 53.10(3) . . ? Fe1 Te1 Fe2 65.63(3) . . ? Fe1 Te1 Fe3 66.28(3) . . ? Fe2 Te1 Sb1 49.82(2) . . ? Fe3 Te1 Sb1 49.992(18) . . ? Fe3 Te1 Fe2 99.74(3) . . ? Sb1 Fe1 Fe2 54.77(2) . . ? Sb1 Fe1 Fe3 54.68(2) . . ? Te1 Fe1 Sb1 76.09(3) . . ? Te1 Fe1 Fe2 58.27(2) . . ? Te1 Fe1 Fe3 57.63(2) . . ? Fe2 Fe1 Fe3 90.41(3) . . ? C1 Fe1 Sb1 83.84(14) . . ? C1 Fe1 Te1 159.56(15) . . ? C1 Fe1 Fe2 106.59(16) . . ? C1 Fe1 Fe3 113.02(16) . . ? C2 Fe1 Sb1 129.1(2) . . ? C2 Fe1 Te1 99.48(18) . . ? C2 Fe1 Fe2 157.24(19) . . ? C2 Fe1 Fe3 79.79(18) . . ? C2 Fe1 C1 96.2(2) . . ? C3 Fe1 Sb1 133.85(18) . . ? C3 Fe1 Te1 92.98(17) . . ? C3 Fe1 Fe2 81.11(17) . . ? C3 Fe1 Fe3 148.75(18) . . ? C3 Fe1 C1 98.2(2) . . ? C3 Fe1 C2 96.7(3) . . ? Sb1 Fe2 Te1 77.24(3) . . ? Sb1 Fe2 Fe1 59.21(2) . . ? Te1 Fe2 Fe1 56.10(3) . . ? C7 Fe2 Sb1 94.37(15) . . ? C7 Fe2 Te1 109.02(17) . . ? C7 Fe2 Fe1 150.66(15) . . ? C7 Fe2 C8 97.7(2) . . ? C7 Fe2 C9 98.7(2) . . ? C8 Fe2 Sb1 97.74(18) . . ? C8 Fe2 Te1 153.10(17) . . ? C8 Fe2 Fe1 98.38(17) . . ? C8 Fe2 C9 92.0(3) . . ? C9 Fe2 Sb1 162.55(17) . . ? C9 Fe2 Te1 87.52(19) . . ? C9 Fe2 Fe1 105.15(16) . . ? Sb1 Fe3 Te1 77.50(3) . . ? Sb1 Fe3 Fe1 58.95(3) . . ? Te1 Fe3 Fe1 56.08(3) . . ? C4 Fe3 Sb1 160.89(17) . . ? C4 Fe3 Te1 89.00(17) . . ? C4 Fe3 Fe1 102.28(17) . . ? C5 Fe3 Sb1 94.68(16) . . ? C5 Fe3 Te1 158.77(15) . . ? C5 Fe3 Fe1 102.92(15) . . ? C5 Fe3 C4 93.2(2) . . ? C6 Fe3 Sb1 97.59(17) . . ? C6 Fe3 Te1 101.43(18) . . ? C6 Fe3 Fe1 148.72(17) . . ? C6 Fe3 C4 98.3(2) . . ? C6 Fe3 C5 99.1(2) . . ? O1 C1 Fe1 176.8(4) . . ? O2 C2 Fe1 175.2(5) . . ? O3 C3 Fe1 177.6(6) . . ? O4 C4 Fe3 179.4(5) . . ? O5 C5 Fe3 177.3(5) . . ? O6 C6 Fe3 178.9(5) . . ? O7 C7 Fe2 176.5(5) . . ? O8 C8 Fe2 176.7(6) . . ? O9 C9 Fe2 177.5(5) . . ? C11 C10 Sb1 90.7(3) . . ? C11 C10 C15 120.8(4) . . ? C14 C10 Sb1 101.3(3) . . ? C14 C10 C11 104.5(3) . . ? C14 C10 C15 120.9(4) . . ? C15 C10 Sb1 113.0(3) . . ? C12 C11 C10 107.4(4) . . ? C12 C11 C16 129.0(4) . . ? C16 C11 C10 123.5(4) . . ? C11 C12 C13 109.6(4) . . ? C11 C12 C17 126.6(5) . . ? C13 C12 C17 123.8(4) . . ? C12 C13 C18 124.0(4) . . ? C14 C13 C12 110.0(4) . . ? C14 C13 C18 126.0(4) . . ? C10 C14 C19 122.5(4) . . ? C13 C14 C10 108.1(4) . . ? C13 C14 C19 129.3(4) . . ? Fe4 Sb2 Te2 50.83(2) . . ? Fe5 Sb2 Te2 52.32(2) . . ? Fe5 Sb2 Fe4 65.83(3) . . ? Fe6 Sb2 Te2 52.56(2) . . ? Fe6 Sb2 Fe4 66.61(3) . . ? Fe6 Sb2 Fe5 104.82(3) . . ? C29 Sb2 Te2 176.88(12) . . ? C29 Sb2 Fe4 132.28(12) . . ? C29 Sb2 Fe5 127.40(12) . . ? C29 Sb2 Fe6 127.77(12) . . ? Fe4 Te2 Sb2 52.63(2) . . ? Fe4 Te2 Fe5 65.47(3) . . ? Fe4 Te2 Fe6 65.98(3) . . ? Fe5 Te2 Sb2 49.762(18) . . ? Fe5 Te2 Fe6 99.18(2) . . ? Fe6 Te2 Sb2 49.48(2) . . ? Sb2 Fe4 Fe5 55.07(3) . . ? Sb2 Fe4 Fe6 54.517(19) . . ? Te2 Fe4 Sb2 76.55(3) . . ? Te2 Fe4 Fe5 57.95(2) . . ? Te2 Fe4 Fe6 57.82(2) . . ? Fe5 Fe4 Fe6 90.06(3) . . ? C20 Fe4 Sb2 83.42(16) . . ? C20 Fe4 Te2 159.76(17) . . ? C20 Fe4 Fe5 107.72(17) . . ? C20 Fe4 Fe6 111.97(17) . . ? C20 Fe4 C21 94.6(2) . . ? C21 Fe4 Sb2 132.63(17) . . ? C21 Fe4 Te2 96.81(17) . . ? C21 Fe4 Fe5 81.33(15) . . ? C21 Fe4 Fe6 153.40(18) . . ? C22 Fe4 Sb2 128.98(19) . . ? C22 Fe4 Te2 97.51(17) . . ? C22 Fe4 Fe5 154.95(17) . . ? C22 Fe4 Fe6 79.11(17) . . ? C22 Fe4 C20 97.3(2) . . ? C22 Fe4 C21 98.3(3) . . ? Sb2 Fe5 Te2 77.92(2) . . ? Sb2 Fe5 Fe4 59.11(3) . . ? Te2 Fe5 Fe4 56.59(2) . . ? C23 Fe5 Sb2 92.72(14) . . ? C23 Fe5 Te2 155.50(15) . . ? C23 Fe5 Fe4 99.14(14) . . ? C23 Fe5 C24 94.7(2) . . ? C24 Fe5 Sb2 160.34(15) . . ? C24 Fe5 Te2 87.96(16) . . ? C24 Fe5 Fe4 101.68(15) . . ? C25 Fe5 Sb2 98.23(14) . . ? C25 Fe5 Te2 103.98(15) . . ? C25 Fe5 Fe4 151.08(14) . . ? C25 Fe5 C23 99.7(2) . . ? C25 Fe5 C24 98.4(2) . . ? Sb2 Fe6 Te2 77.96(2) . . ? Sb2 Fe6 Fe4 58.87(3) . . ? Te2 Fe6 Fe4 56.202(19) . . ? C26 Fe6 Sb2 96.39(16) . . ? C26 Fe6 Te2 154.25(17) . . ? C26 Fe6 Fe4 99.21(16) . . ? C26 Fe6 C27 100.5(2) . . ? C27 Fe6 Sb2 95.24(16) . . ? C27 Fe6 Te2 104.96(14) . . ? C27 Fe6 Fe4 148.99(15) . . ? C28 Fe6 Sb2 163.73(16) . . ? C28 Fe6 Te2 88.54(16) . . ? C28 Fe6 Fe4 106.00(17) . . ? C28 Fe6 C26 91.9(2) . . ? C28 Fe6 C27 97.0(2) . . ? O10 C20 Fe4 175.3(5) . . ? O11 C21 Fe4 176.6(4) . . ? O12 C22 Fe4 174.8(5) . . ? O13 C23 Fe5 179.1(4) . . ? O14 C24 Fe5 179.6(5) . . ? O15 C25 Fe5 178.7(4) . . ? O16 C26 Fe6 176.0(5) . . ? O17 C27 Fe6 179.6(6) . . ? O18 C28 Fe6 178.4(5) . . ? C30 C29 Sb2 89.8(3) . . ? C30 C29 C34 121.1(4) . . ? C33 C29 Sb2 101.0(3) . . ? C33 C29 C30 104.8(4) . . ? C33 C29 C34 120.8(4) . . ? C34 C29 Sb2 113.5(3) . . ? C29 C30 C35 123.3(5) . . ? C31 C30 C29 108.2(4) . . ? C31 C30 C35 128.4(5) . . ? C30 C31 C32 109.4(4) . . ? C30 C31 C36 127.5(4) . . ? C32 C31 C36 123.1(4) . . ? C31 C32 C37 123.1(4) . . ? C33 C32 C31 109.1(4) . . ? C33 C32 C37 127.9(5) . . ? C29 C33 C38 123.3(4) . . ? C32 C33 C29 108.3(4) . . ? C32 C33 C38 128.3(4) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.754 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.140 #___END data_v21 _database_code_CSD 196897 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H13 Fe4 O11 Sb Se' _chemical_formula_weight 853.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.819(2) _cell_length_b 18.667(5) _cell_length_c 14.502(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.85(2) _cell_angle_gamma 90.00 _cell_volume 2652.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 15.1 _cell_measurement_theta_max 17.3 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 4.568 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4177 _exptl_absorpt_correction_T_max 0.9998 _exptl_absorpt_process_details 'X-RED (STOE)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 STADI4' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7321 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 29.02 _reflns_number_total 7067 _reflns_number_gt 5680 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0319P)^2^+0.5371P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00120(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7067 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 Sb Sb 0.43596(2) 0.160455(13) 0.748849(15) 0.01999(7) Uani 1 1 d . . . Se Se 0.38588(4) 0.325487(19) 0.75299(2) 0.02221(9) Uani 1 1 d . . . Fe1 Fe 0.22122(5) 0.23749(3) 0.71427(3) 0.02113(11) Uani 1 1 d . . . Fe2 Fe 0.37976(6) 0.24277(3) 0.87639(3) 0.02164(11) Uani 1 1 d . . . Fe3 Fe 0.45880(6) 0.25491(3) 0.62917(3) 0.02178(11) Uani 1 1 d . . . Fe4 Fe 0.47200(5) 0.02779(3) 0.75944(4) 0.02133(11) Uani 1 1 d . . . C1 C 0.6510(4) -0.0095(2) 0.6991(3) 0.0250(8) Uani 1 1 d . . . C2 C 0.5696(4) -0.0683(2) 0.7273(3) 0.0297(8) Uani 1 1 d . . . H2 H 0.5972 -0.1037 0.7707 0.030 Uiso 1 1 calc R . . C3 C 0.4413(5) -0.0637(2) 0.6786(3) 0.0363(10) Uani 1 1 d . . . H3 H 0.3689 -0.0961 0.6835 0.036 Uiso 1 1 calc R . . C4 C 0.4386(4) -0.0025(2) 0.6209(3) 0.0330(9) Uani 1 1 d . . . H4 H 0.3646 0.0132 0.5815 0.033 Uiso 1 1 calc R . . C5 C 0.5683(4) 0.0306(2) 0.6337(3) 0.0281(8) Uani 1 1 d . . . H5 H 0.5953 0.0723 0.6037 0.028 Uiso 1 1 calc R . . C6 C 0.8021(4) 0.0027(2) 0.7243(3) 0.0313(9) Uani 1 1 d . . . C7 C 0.8508(5) -0.0402(3) 0.8105(4) 0.0483(13) Uani 1 1 d . . . H7A H 0.8142 -0.0189 0.8647 0.048 Uiso 1 1 calc R . . H7B H 0.9497 -0.0395 0.8175 0.048 Uiso 1 1 calc R . . H7C H 0.8192 -0.0893 0.8040 0.048 Uiso 1 1 calc R . . C8 C 0.8336(4) 0.0827(2) 0.7399(3) 0.0403(10) Uani 1 1 d . . . H8A H 0.7922 0.1103 0.6887 0.040 Uiso 1 1 calc R . . H8B H 0.9316 0.0900 0.7438 0.040 Uiso 1 1 calc R . . H8C H 0.7967 0.0983 0.7970 0.040 Uiso 1 1 calc R . . C9 C 0.8772(5) -0.0246(3) 0.6411(4) 0.0493(13) Uani 1 1 d . . . H9A H 0.8619 -0.0757 0.6337 0.049 Uiso 1 1 calc R . . H9B H 0.9742 -0.0155 0.6517 0.049 Uiso 1 1 calc R . . H9C H 0.8426 0.0002 0.5856 0.049 Uiso 1 1 calc R . . C11 C 0.1301(4) 0.3027(2) 0.6439(3) 0.0314(9) Uani 1 1 d . . . O11 O 0.0719(4) 0.3442(2) 0.5999(2) 0.0508(9) Uani 1 1 d . . . C12 C 0.1032(5) 0.2319(3) 0.8022(3) 0.0352(9) Uani 1 1 d . . . O12 O 0.0177(4) 0.2285(2) 0.8518(2) 0.0546(10) Uani 1 1 d . . . C13 C 0.1652(4) 0.1614(2) 0.6483(3) 0.0312(9) Uani 1 1 d . . . O13 O 0.1272(4) 0.1144(2) 0.6024(2) 0.0501(9) Uani 1 1 d . . . C21 C 0.3096(4) 0.3114(2) 0.9478(3) 0.0308(9) Uani 1 1 d . . . O21 O 0.2701(4) 0.35565(19) 0.9926(2) 0.0513(9) Uani 1 1 d . . . C22 C 0.5553(5) 0.2479(2) 0.9126(3) 0.0349(10) Uani 1 1 d . . . O22 O 0.6686(4) 0.2526(2) 0.9338(3) 0.0579(11) Uani 1 1 d . . . C23 C 0.3265(4) 0.1700(2) 0.9467(3) 0.0295(8) Uani 1 1 d . . . O23 O 0.2923(4) 0.12336(19) 0.9903(2) 0.0481(9) Uani 1 1 d . . . C31 C 0.4217(5) 0.3301(2) 0.5512(3) 0.0327(9) Uani 1 1 d . . . O31 O 0.4020(4) 0.3775(2) 0.5039(2) 0.0561(10) Uani 1 1 d . . . C32 C 0.6398(4) 0.2611(2) 0.6445(3) 0.0307(9) Uani 1 1 d . . . O32 O 0.7560(3) 0.26549(19) 0.6554(2) 0.0465(8) Uani 1 1 d . . . C33 C 0.4365(4) 0.1898(2) 0.5383(3) 0.0290(8) Uani 1 1 d . . . O33 O 0.4202(4) 0.14733(18) 0.4820(2) 0.0443(8) Uani 1 1 d . . . C41 C 0.5516(4) 0.0381(2) 0.8733(3) 0.0300(8) Uani 1 1 d . . . O41 O 0.6008(4) 0.0438(2) 0.9457(2) 0.0503(9) Uani 1 1 d . . . C42 C 0.3074(4) 0.0190(2) 0.8000(3) 0.0359(10) Uani 1 1 d . . . O42 O 0.2008(4) 0.0128(2) 0.8262(3) 0.0622(11) 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 Sb 0.02484(12) 0.01581(11) 0.01955(11) -0.00064(9) 0.00326(8) 0.00084(9) Se 0.02760(18) 0.01642(18) 0.02272(17) -0.00108(13) 0.00249(14) -0.00057(14) Fe1 0.0215(3) 0.0216(3) 0.0203(2) -0.0019(2) 0.00149(19) 0.0004(2) Fe2 0.0271(3) 0.0205(3) 0.0173(2) -0.00213(19) 0.00131(19) 0.0003(2) Fe3 0.0263(3) 0.0198(3) 0.0197(2) 0.00123(19) 0.0047(2) 0.0004(2) Fe4 0.0221(2) 0.0162(3) 0.0262(3) -0.0009(2) 0.0050(2) -0.0004(2) C1 0.0277(19) 0.0189(18) 0.0291(18) 0.0007(14) 0.0085(15) 0.0040(15) C2 0.034(2) 0.0135(17) 0.042(2) 0.0001(16) 0.0083(17) -0.0002(16) C3 0.040(2) 0.024(2) 0.046(2) -0.0171(19) 0.0082(19) -0.0087(18) C4 0.033(2) 0.037(2) 0.030(2) -0.0081(18) 0.0042(16) 0.0034(19) C5 0.035(2) 0.0227(19) 0.0278(18) -0.0006(15) 0.0076(16) 0.0044(17) C6 0.0252(19) 0.027(2) 0.042(2) 0.0050(18) 0.0069(17) 0.0048(16) C7 0.032(2) 0.051(3) 0.062(3) 0.017(3) 0.003(2) 0.008(2) C8 0.030(2) 0.033(3) 0.058(3) 0.003(2) 0.004(2) -0.0057(19) C9 0.040(3) 0.048(3) 0.063(3) 0.000(2) 0.024(2) 0.005(2) C11 0.030(2) 0.036(2) 0.0275(19) -0.0043(17) -0.0025(16) 0.0031(18) O11 0.057(2) 0.047(2) 0.0459(19) 0.0051(16) -0.0101(16) 0.0181(18) C12 0.035(2) 0.037(2) 0.034(2) -0.0049(18) 0.0052(18) -0.0036(19) O12 0.043(2) 0.079(3) 0.0448(19) -0.0100(19) 0.0225(16) -0.0092(19) C13 0.029(2) 0.034(2) 0.032(2) -0.0009(17) 0.0042(16) -0.0029(18) O13 0.050(2) 0.045(2) 0.055(2) -0.0220(17) 0.0014(16) -0.0127(17) C21 0.040(2) 0.030(2) 0.0221(18) 0.0017(16) 0.0016(16) 0.0022(19) O21 0.073(3) 0.042(2) 0.0407(18) -0.0145(15) 0.0110(17) 0.0116(19) C22 0.035(2) 0.040(3) 0.029(2) 0.0000(17) -0.0020(17) -0.0039(19) O22 0.0367(19) 0.082(3) 0.053(2) 0.0084(19) -0.0120(16) -0.0085(19) C23 0.038(2) 0.030(2) 0.0207(17) -0.0019(15) 0.0038(15) 0.0002(18) O23 0.065(2) 0.041(2) 0.0387(18) 0.0086(15) 0.0101(16) -0.0088(18) C31 0.039(2) 0.032(2) 0.0268(19) 0.0018(16) 0.0026(16) 0.0023(18) O31 0.081(3) 0.041(2) 0.046(2) 0.0206(16) 0.0052(18) 0.011(2) C32 0.038(2) 0.025(2) 0.030(2) 0.0019(16) 0.0073(17) -0.0011(17) O32 0.0272(16) 0.049(2) 0.063(2) 0.0032(17) 0.0060(15) -0.0036(15) C33 0.032(2) 0.033(2) 0.0233(18) 0.0033(16) 0.0042(15) 0.0050(18) O33 0.062(2) 0.042(2) 0.0289(15) -0.0078(14) -0.0001(14) 0.0047(17) C41 0.034(2) 0.025(2) 0.031(2) 0.0002(16) 0.0056(17) 0.0024(17) O41 0.062(2) 0.057(2) 0.0304(16) 0.0004(15) -0.0061(15) 0.0095(19) C42 0.032(2) 0.029(2) 0.048(2) -0.0092(19) 0.0095(19) -0.0048(18) O42 0.041(2) 0.064(3) 0.085(3) -0.022(2) 0.0306(19) -0.0192(19) _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 Sb Fe1 2.5737(8) . ? Sb Fe2 2.4948(7) . ? Sb Fe3 2.4947(7) . ? Sb Fe4 2.5050(8) . ? Se Fe1 2.3465(8) . ? Se Fe2 2.3673(7) . ? Se Fe3 2.3760(7) . ? Fe1 Fe2 2.7328(10) . ? Fe1 Fe3 2.7309(10) . ? Fe1 C11 1.789(4) . ? Fe1 C12 1.783(4) . ? Fe1 C13 1.779(4) . ? Fe2 C21 1.812(4) . ? Fe2 C22 1.771(4) . ? Fe2 C23 1.798(4) . ? Fe3 C31 1.824(4) . ? Fe3 C32 1.781(4) . ? Fe3 C33 1.795(4) . ? Fe4 C1 2.132(4) . ? Fe4 C2 2.100(4) . ? Fe4 C3 2.082(4) . ? Fe4 C4 2.092(4) . ? Fe4 C5 2.110(4) . ? Fe4 C41 1.790(4) . ? Fe4 C42 1.764(4) . ? C1 C2 1.434(5) . ? C1 C5 1.420(5) . ? C1 C6 1.522(6) . ? C2 C3 1.405(6) . ? C3 C4 1.415(6) . ? C4 C5 1.417(6) . ? C6 C7 1.534(6) . ? C6 C8 1.538(6) . ? C6 C9 1.542(6) . ? C11 O11 1.134(5) . ? C12 O12 1.143(5) . ? C13 O13 1.148(5) . ? C21 O21 1.135(5) . ? C22 O22 1.137(5) . ? C23 O23 1.139(5) . ? C31 O31 1.128(5) . ? C32 O32 1.144(5) . ? C33 O33 1.142(5) . ? C41 O41 1.131(5) . ? C42 O42 1.143(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe2 Sb Fe1 65.23(2) . . ? Fe2 Sb Fe3 96.61(3) . . ? Fe2 Sb Fe4 126.93(2) . . ? Fe3 Sb Fe1 65.18(2) . . ? Fe3 Sb Fe4 136.26(2) . . ? Fe4 Sb Fe1 132.44(2) . . ? Fe1 Se Fe2 70.86(3) . . ? Fe1 Se Fe3 70.66(3) . . ? Fe2 Se Fe3 103.52(3) . . ? Sb Fe1 Fe2 55.99(2) . . ? Sb Fe1 Fe3 56.01(2) . . ? Se Fe1 Sb 78.59(3) . . ? Se Fe1 Fe2 54.92(2) . . ? Se Fe1 Fe3 55.18(2) . . ? Fe3 Fe1 Fe2 85.98(3) . . ? C11 Fe1 Sb 149.65(13) . . ? C11 Fe1 Se 88.31(14) . . ? C11 Fe1 Fe2 134.47(14) . . ? C11 Fe1 Fe3 94.05(14) . . ? C11 Fe1 C12 97.1(2) . . ? C12 Fe1 Sb 113.03(15) . . ? C12 Fe1 Se 109.89(14) . . ? C12 Fe1 Fe2 75.33(14) . . ? C12 Fe1 Fe3 161.11(14) . . ? C13 Fe1 Sb 83.02(14) . . ? C13 Fe1 Se 150.56(13) . . ? C13 Fe1 Fe2 129.00(14) . . ? C13 Fe1 Fe3 95.44(13) . . ? C13 Fe1 C11 96.39(19) . . ? C13 Fe1 C12 98.38(19) . . ? Sb Fe2 Fe1 58.775(19) . . ? Se Fe2 Sb 79.82(2) . . ? Se Fe2 Fe1 54.21(2) . . ? C21 Fe2 Sb 166.06(13) . . ? C21 Fe2 Se 90.02(13) . . ? C21 Fe2 Fe1 107.49(13) . . ? C22 Fe2 Sb 89.61(15) . . ? C22 Fe2 Se 96.62(15) . . ? C22 Fe2 Fe1 138.06(14) . . ? C22 Fe2 C21 101.1(2) . . ? C22 Fe2 C23 100.8(2) . . ? C23 Fe2 Sb 92.42(13) . . ? C23 Fe2 Se 160.90(13) . . ? C23 Fe2 Fe1 106.87(13) . . ? C23 Fe2 C21 94.27(18) . . ? Sb Fe3 Fe1 58.80(2) . . ? Se Fe3 Sb 79.66(2) . . ? Se Fe3 Fe1 54.17(2) . . ? C31 Fe3 Sb 162.12(14) . . ? C31 Fe3 Se 89.07(13) . . ? C31 Fe3 Fe1 103.33(14) . . ? C32 Fe3 Sb 95.44(13) . . ? C32 Fe3 Se 102.62(14) . . ? C32 Fe3 Fe1 145.83(13) . . ? C32 Fe3 C31 100.6(2) . . ? C32 Fe3 C33 101.96(19) . . ? C33 Fe3 Sb 91.13(13) . . ? C33 Fe3 Se 154.43(13) . . ? C33 Fe3 Fe1 100.68(13) . . ? C33 Fe3 C31 93.27(18) . . ? C1 Fe4 Sb 114.48(11) . . ? C2 Fe4 Sb 153.54(11) . . ? C2 Fe4 C1 39.59(14) . . ? C2 Fe4 C5 65.90(15) . . ? C3 Fe4 Sb 139.63(14) . . ? C3 Fe4 C1 66.01(16) . . ? C3 Fe4 C2 39.25(17) . . ? C3 Fe4 C4 39.62(17) . . ? C3 Fe4 C5 65.77(17) . . ? C4 Fe4 Sb 101.32(13) . . ? C4 Fe4 C1 66.32(16) . . ? C4 Fe4 C2 66.44(17) . . ? C4 Fe4 C5 39.40(16) . . ? C5 Fe4 Sb 89.56(11) . . ? C5 Fe4 C1 39.10(14) . . ? C41 Fe4 Sb 90.07(14) . . ? C41 Fe4 C1 95.31(17) . . ? C41 Fe4 C2 96.85(18) . . ? C41 Fe4 C3 130.23(19) . . ? C41 Fe4 C4 161.11(18) . . ? C41 Fe4 C5 126.98(17) . . ? C42 Fe4 Sb 89.05(15) . . ? C42 Fe4 C1 154.89(18) . . ? C42 Fe4 C2 115.88(18) . . ? C42 Fe4 C3 90.59(19) . . ? C42 Fe4 C4 101.92(19) . . ? C42 Fe4 C5 139.80(19) . . ? C42 Fe4 C41 93.2(2) . . ? C2 C1 Fe4 69.0(2) . . ? C2 C1 C6 126.9(4) . . ? C5 C1 Fe4 69.6(2) . . ? C5 C1 C2 106.8(4) . . ? C5 C1 C6 125.9(4) . . ? C6 C1 Fe4 132.1(3) . . ? C1 C2 Fe4 71.4(2) . . ? C3 C2 Fe4 69.7(2) . . ? C3 C2 C1 108.0(4) . . ? C2 C3 Fe4 71.1(2) . . ? C2 C3 C4 109.1(4) . . ? C4 C3 Fe4 70.6(2) . . ? C3 C4 Fe4 69.8(2) . . ? C3 C4 C5 107.1(4) . . ? C5 C4 Fe4 71.0(2) . . ? C1 C5 Fe4 71.3(2) . . ? C4 C5 Fe4 69.6(2) . . ? C4 C5 C1 109.1(4) . . ? C1 C6 C7 111.3(3) . . ? C1 C6 C8 111.3(3) . . ? C1 C6 C9 105.8(4) . . ? C7 C6 C8 109.8(4) . . ? C7 C6 C9 109.0(4) . . ? C8 C6 C9 109.5(4) . . ? O11 C11 Fe1 179.4(4) . . ? O12 C12 Fe1 173.3(4) . . ? O13 C13 Fe1 176.8(4) . . ? O21 C21 Fe2 177.5(4) . . ? O22 C22 Fe2 178.0(4) . . ? O23 C23 Fe2 179.2(4) . . ? O31 C31 Fe3 178.1(4) . . ? O32 C32 Fe3 179.1(4) . . ? O33 C33 Fe3 178.2(4) . . ? O41 C41 Fe4 179.0(4) . . ? O42 C42 Fe4 179.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.123 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.129 #___END data_new2 _database_code_CSD 196898 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H13 Fe4 O11 Sb Te' _chemical_formula_weight 902.05 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0904(18) _cell_length_b 16.776(3) _cell_length_c 17.831(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.56(3) _cell_angle_gamma 90.00 _cell_volume 2643.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used 1278 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 24.04 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 4.288 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6458 _exptl_absorpt_correction_T_max 0.8978 _exptl_absorpt_process_details 'program faceit' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(1) _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 IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10723 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 24.04 _reflns_number_total 4030 _reflns_number_gt 3422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SIEMENS-XP _computing_publication_material SHEXL-97 _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^)+(0.0437P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4030 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Sb Sb 0.92088(3) 0.753167(11) 0.103482(14) 0.02454(9) Uani 1 1 d . . . Te Te 0.71386(3) 0.747796(11) -0.073624(14) 0.03015(9) Uani 1 1 d . . . Fe1 Fe 0.63785(5) 0.72766(3) 0.05264(3) 0.02634(13) Uani 1 1 d . . . Fe2 Fe 0.78488(6) 0.86392(3) 0.02122(3) 0.02844(13) Uani 1 1 d . . . Fe3 Fe 0.86641(6) 0.63958(3) 0.01021(3) 0.02881(13) Uani 1 1 d . . . Fe4 Fe 1.09357(6) 0.74242(2) 0.23631(3) 0.02869(13) Uani 1 1 d . . . C1 C 0.9899(4) 0.8186(2) 0.2708(2) 0.0328(8) Uani 1 1 d . . . O1 O 0.9204(3) 0.86539(16) 0.29402(17) 0.0468(7) Uani 1 1 d . . . C2 C 0.9814(4) 0.6659(2) 0.2628(2) 0.0371(9) Uani 1 1 d . . . O2 O 0.9142(4) 0.61570(17) 0.28329(19) 0.0573(8) Uani 1 1 d . . . C3 C 0.9441(5) 0.8971(2) -0.0128(2) 0.0374(9) Uani 1 1 d . . . O3 O 1.0464(3) 0.91777(16) -0.03512(18) 0.0508(7) Uani 1 1 d . . . C4 C 0.7961(4) 0.9301(2) 0.1022(2) 0.0350(8) Uani 1 1 d . . . O4 O 0.8020(3) 0.97389(15) 0.15164(17) 0.0486(7) Uani 1 1 d . . . C5 C 0.6359(5) 0.9230(2) -0.0385(2) 0.0389(9) Uani 1 1 d . . . O5 O 0.5427(4) 0.96030(17) -0.07620(19) 0.0591(8) Uani 1 1 d . . . C6 C 0.9261(4) 0.5700(2) 0.0875(2) 0.0383(9) Uani 1 1 d . . . O6 O 0.9680(4) 0.52594(16) 0.13681(19) 0.0559(8) Uani 1 1 d . . . C7 C 1.0398(5) 0.6519(2) -0.0169(2) 0.0383(9) Uani 1 1 d . . . O7 O 1.1532(3) 0.65990(18) -0.03383(19) 0.0580(8) Uani 1 1 d . . . C8 C 0.7777(4) 0.5636(2) -0.0582(2) 0.0373(9) Uani 1 1 d . . . O8 O 0.7272(3) 0.51497(15) -0.10134(18) 0.0515(7) Uani 1 1 d . . . C9 C 0.4775(4) 0.7925(2) 0.0261(2) 0.0343(8) Uani 1 1 d . . . O9 O 0.3696(3) 0.82955(16) 0.00957(17) 0.0496(7) Uani 1 1 d . . . C10 C 0.6448(4) 0.7219(2) 0.1527(2) 0.0382(9) Uani 1 1 d . . . O10 O 0.6393(3) 0.7162(2) 0.21616(19) 0.0588(8) Uani 1 1 d . . . C11 C 0.5413(5) 0.6346(2) 0.0304(2) 0.0396(9) Uani 1 1 d . . . O11 O 0.4723(4) 0.57762(16) 0.0189(2) 0.0659(10) Uani 1 1 d . . . C12 C 1.3005(4) 0.8073(2) 0.2448(2) 0.0326(8) Uani 1 1 d . . . C13 C 1.2775(4) 0.75219(19) 0.1826(3) 0.0380(9) Uani 1 1 d . . . H13 H 1.2692 0.7654 0.1299 0.046 Uiso 1 1 calc R . . C14 C 1.2689(4) 0.6740(2) 0.2121(3) 0.0496(11) Uani 1 1 d . . . H14 H 1.2536 0.6261 0.1828 0.059 Uiso 1 1 calc R . . C15 C 1.2873(5) 0.6804(2) 0.2930(3) 0.0511(11) Uani 1 1 d . . . H15 H 1.2882 0.6375 0.3279 0.061 Uiso 1 1 calc R . . C16 C 1.3039(4) 0.7617(2) 0.3127(3) 0.0422(10) Uani 1 1 d . . . H16 H 1.3156 0.7829 0.3631 0.051 Uiso 1 1 calc R . . C17 C 1.3337(4) 0.8959(2) 0.2406(2) 0.0357(8) Uani 1 1 d . . . C18 C 1.2225(5) 0.9348(2) 0.1726(3) 0.0506(11) Uani 1 1 d . . . H18A H 1.2484 0.9912 0.1695 0.076 Uiso 1 1 calc R . . H18B H 1.1194 0.9303 0.1802 0.076 Uiso 1 1 calc R . . H18C H 1.2283 0.9079 0.1246 0.076 Uiso 1 1 calc R . . C19 C 1.4943(4) 0.9030(2) 0.2275(3) 0.0436(9) Uani 1 1 d . . . H19A H 1.5237 0.9593 0.2290 0.065 Uiso 1 1 calc R . . H19B H 1.4965 0.8804 0.1771 0.065 Uiso 1 1 calc R . . H19C H 1.5652 0.8739 0.2681 0.065 Uiso 1 1 calc R . . C20 C 1.3287(5) 0.9377(2) 0.3155(3) 0.0574(12) Uani 1 1 d . . . H20A H 1.3465 0.9949 0.3106 0.086 Uiso 1 1 calc R . . H20B H 1.4073 0.9156 0.3576 0.086 Uiso 1 1 calc R . . H20C H 1.2292 0.9295 0.3266 0.086 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 Sb 0.02502(14) 0.02445(13) 0.02351(16) 0.00145(8) 0.00439(10) 0.00148(8) Te 0.03178(16) 0.03496(14) 0.02319(16) -0.00021(8) 0.00542(11) 0.00003(9) Fe1 0.0248(3) 0.0286(2) 0.0261(3) 0.0002(2) 0.0070(2) 0.00098(19) Fe2 0.0306(3) 0.0251(2) 0.0286(3) 0.00374(19) 0.0049(2) 0.00185(19) Fe3 0.0300(3) 0.0270(2) 0.0307(3) -0.00252(19) 0.0096(2) 0.00139(19) Fe4 0.0254(3) 0.0311(3) 0.0278(3) 0.00311(19) 0.0028(2) 0.00110(18) C1 0.0286(19) 0.0401(18) 0.027(2) 0.0007(15) 0.0019(16) -0.0050(16) O1 0.0464(17) 0.0517(16) 0.0451(19) -0.0086(13) 0.0165(14) 0.0045(13) C2 0.035(2) 0.042(2) 0.032(2) 0.0071(16) 0.0025(17) 0.0066(17) O2 0.0554(19) 0.0527(16) 0.066(2) 0.0237(15) 0.0178(17) -0.0072(14) C3 0.046(2) 0.0316(18) 0.031(2) 0.0021(15) 0.0005(18) 0.0048(16) O3 0.0485(18) 0.0543(16) 0.055(2) 0.0070(13) 0.0219(16) -0.0078(13) C4 0.033(2) 0.0327(18) 0.039(2) 0.0066(17) 0.0069(17) 0.0018(15) O4 0.0590(19) 0.0417(14) 0.046(2) -0.0101(13) 0.0145(15) 0.0029(13) C5 0.042(2) 0.0352(18) 0.040(3) 0.0077(16) 0.0097(19) -0.0002(17) O5 0.0512(18) 0.0600(17) 0.061(2) 0.0255(15) 0.0036(16) 0.0184(15) C6 0.038(2) 0.0297(18) 0.050(3) -0.0045(18) 0.0175(19) -0.0011(15) O6 0.064(2) 0.0400(15) 0.065(2) 0.0196(15) 0.0176(17) 0.0119(14) C7 0.042(2) 0.0403(19) 0.033(2) -0.0055(16) 0.0106(19) 0.0018(16) O7 0.0402(17) 0.081(2) 0.059(2) -0.0010(16) 0.0247(15) -0.0024(15) C8 0.035(2) 0.0352(19) 0.044(3) -0.0024(17) 0.0150(18) 0.0047(16) O8 0.0546(18) 0.0433(15) 0.056(2) -0.0202(14) 0.0117(15) -0.0066(13) C9 0.036(2) 0.041(2) 0.028(2) 0.0020(15) 0.0111(17) -0.0018(17) O9 0.0326(15) 0.0600(17) 0.058(2) 0.0124(14) 0.0145(14) 0.0179(14) C10 0.0263(19) 0.050(2) 0.040(3) 0.0042(18) 0.0115(17) 0.0042(16) O10 0.0443(18) 0.104(2) 0.032(2) 0.0082(16) 0.0176(14) 0.0145(17) C11 0.040(2) 0.039(2) 0.044(3) 0.0003(17) 0.0172(19) 0.0015(17) O11 0.064(2) 0.0403(16) 0.102(3) -0.0141(16) 0.036(2) -0.0188(15) C12 0.0177(17) 0.0434(19) 0.036(2) -0.0012(16) 0.0049(15) 0.0014(14) C13 0.0221(19) 0.046(2) 0.046(3) -0.0070(16) 0.0091(18) 0.0014(14) C14 0.031(2) 0.0328(19) 0.083(4) -0.0102(19) 0.011(2) 0.0038(16) C15 0.033(2) 0.042(2) 0.070(3) 0.019(2) -0.004(2) 0.0056(17) C16 0.027(2) 0.057(2) 0.035(2) 0.0068(17) -0.0089(17) -0.0016(16) C17 0.0253(18) 0.0383(18) 0.043(2) -0.0025(16) 0.0075(17) -0.0016(14) C18 0.040(2) 0.039(2) 0.070(3) 0.0086(19) 0.008(2) 0.0005(17) C19 0.036(2) 0.048(2) 0.047(3) -0.0021(18) 0.0096(19) -0.0047(17) C20 0.058(3) 0.055(2) 0.064(3) -0.024(2) 0.024(3) -0.014(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 Sb Te 3.2764(11) . ? Sb Fe1 2.5555(8) . ? Sb Fe2 2.5063(7) . ? Sb Fe3 2.5012(6) . ? Sb Fe4 2.5224(10) . ? Te Fe1 2.5278(8) . ? Te Fe2 2.5612(7) . ? Te Fe3 2.5458(7) . ? Fe1 Fe2 2.7706(8) . ? Fe1 Fe3 2.7946(8) . ? Fe1 C9 1.791(4) . ? Fe1 C10 1.773(4) . ? Fe1 C11 1.789(4) . ? Fe2 C3 1.784(4) . ? Fe2 C4 1.805(4) . ? Fe2 C5 1.809(4) . ? Fe3 C6 1.790(4) . ? Fe3 C7 1.765(4) . ? Fe3 C8 1.817(4) . ? Fe4 C1 1.781(4) . ? Fe4 C2 1.771(4) . ? Fe4 C12 2.148(3) . ? Fe4 C13 2.119(4) . ? Fe4 C14 2.090(4) . ? Fe4 C15 2.090(4) . ? Fe4 C16 2.096(4) . ? C1 O1 1.145(4) . ? C2 O2 1.149(4) . ? C3 O3 1.148(5) . ? C4 O4 1.139(4) . ? C5 O5 1.138(5) . ? C6 O6 1.144(5) . ? C7 O7 1.149(5) . ? C8 O8 1.141(4) . ? C9 O9 1.140(4) . ? C10 O10 1.148(4) . ? C11 O11 1.135(4) . ? C12 C13 1.422(5) . ? C12 C16 1.425(6) . ? C12 C17 1.522(5) . ? C13 C14 1.423(5) . ? C14 C15 1.418(7) . ? C15 C16 1.408(5) . ? C17 C18 1.531(5) . ? C17 C19 1.536(5) . ? C17 C20 1.518(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 Sb Te 49.50(3) . . ? Fe2 Sb Te 50.455(18) . . ? Fe2 Sb Fe1 66.36(2) . . ? Fe2 Sb Fe4 135.68(2) . . ? Fe3 Sb Te 50.116(15) . . ? Fe3 Sb Fe1 67.09(2) . . ? Fe3 Sb Fe2 100.49(3) . . ? Fe3 Sb Fe4 123.54(2) . . ? Fe4 Sb Te 173.396(14) . . ? Fe4 Sb Fe1 132.39(3) . . ? Fe1 Te Sb 50.240(18) . . ? Fe1 Te Fe2 65.969(19) . . ? Fe1 Te Fe3 66.85(2) . . ? Fe2 Te Sb 48.989(15) . . ? Fe3 Te Sb 48.930(18) . . ? Fe3 Te Fe2 97.84(3) . . ? Sb Fe1 Fe2 55.965(16) . . ? Sb Fe1 Fe3 55.527(18) . . ? Te Fe1 Sb 80.26(3) . . ? Te Fe1 Fe2 57.596(18) . . ? Te Fe1 Fe3 56.88(2) . . ? Fe2 Fe1 Fe3 87.53(2) . . ? C9 Fe1 Sb 132.95(11) . . ? C9 Fe1 Te 93.39(12) . . ? C9 Fe1 Fe2 81.20(11) . . ? C9 Fe1 Fe3 149.35(12) . . ? C10 Fe1 Sb 81.78(12) . . ? C10 Fe1 Te 161.97(12) . . ? C10 Fe1 Fe2 110.08(13) . . ? C10 Fe1 Fe3 112.99(12) . . ? C10 Fe1 C9 97.66(17) . . ? C10 Fe1 C11 94.30(18) . . ? C11 Fe1 Sb 128.71(13) . . ? C11 Fe1 Te 98.16(13) . . ? C11 Fe1 Fe2 155.51(13) . . ? C11 Fe1 Fe3 80.56(12) . . ? C11 Fe1 C9 98.32(17) . . ? Sb Fe2 Te 80.56(3) . . ? Sb Fe2 Fe1 57.67(2) . . ? Te Fe2 Fe1 56.44(2) . . ? C3 Fe2 Sb 95.85(11) . . ? C3 Fe2 Te 96.40(12) . . ? C3 Fe2 Fe1 142.57(11) . . ? C3 Fe2 C4 100.50(17) . . ? C3 Fe2 C5 100.59(16) . . ? C4 Fe2 Sb 93.47(11) . . ? C4 Fe2 Te 162.58(11) . . ? C4 Fe2 Fe1 106.57(11) . . ? C4 Fe2 C5 91.57(17) . . ? C5 Fe2 Sb 161.62(12) . . ? C5 Fe2 Te 89.45(13) . . ? C5 Fe2 Fe1 103.96(12) . . ? Sb Fe3 Te 80.95(3) . . ? Sb Fe3 Fe1 57.38(2) . . ? Te Fe3 Fe1 56.27(2) . . ? C6 Fe3 Sb 90.45(12) . . ? C6 Fe3 Te 160.39(12) . . ? C6 Fe3 Fe1 104.29(12) . . ? C6 Fe3 C8 93.78(17) . . ? C7 Fe3 Sb 92.41(12) . . ? C7 Fe3 Te 98.86(12) . . ? C7 Fe3 Fe1 141.26(11) . . ? C7 Fe3 C6 99.08(17) . . ? C7 Fe3 C8 100.54(17) . . ? C8 Fe3 Sb 165.54(11) . . ? C8 Fe3 Te 90.65(12) . . ? C8 Fe3 Fe1 108.16(11) . . ? C1 Fe4 Sb 90.55(12) . . ? C1 Fe4 C12 97.90(14) . . ? C1 Fe4 C13 129.64(14) . . ? C1 Fe4 C14 163.07(16) . . ? C1 Fe4 C15 130.10(19) . . ? C1 Fe4 C16 98.11(17) . . ? C2 Fe4 Sb 91.80(12) . . ? C2 Fe4 C1 92.52(17) . . ? C2 Fe4 C12 153.92(16) . . ? C2 Fe4 C13 137.82(15) . . ? C2 Fe4 C14 99.86(16) . . ? C2 Fe4 C15 89.01(16) . . ? C2 Fe4 C16 115.70(16) . . ? C12 Fe4 Sb 111.84(11) . . ? C13 Fe4 Sb 87.31(12) . . ? C13 Fe4 C12 38.93(14) . . ? C14 Fe4 Sb 100.48(14) . . ? C14 Fe4 C12 66.15(14) . . ? C14 Fe4 C13 39.51(15) . . ? C14 Fe4 C15 39.64(19) . . ? C14 Fe4 C16 66.14(18) . . ? C15 Fe4 Sb 139.28(15) . . ? C15 Fe4 C12 66.03(15) . . ? C15 Fe4 C13 65.98(18) . . ? C15 Fe4 C16 39.30(15) . . ? C16 Fe4 Sb 150.56(13) . . ? C16 Fe4 C12 39.23(15) . . ? C16 Fe4 C13 65.52(18) . . ? O1 C1 Fe4 177.4(3) . . ? O2 C2 Fe4 176.5(4) . . ? O3 C3 Fe2 179.3(4) . . ? O4 C4 Fe2 177.8(3) . . ? O5 C5 Fe2 179.7(4) . . ? O6 C6 Fe3 178.3(3) . . ? O7 C7 Fe3 179.4(4) . . ? O8 C8 Fe3 177.5(3) . . ? O9 C9 Fe1 175.5(3) . . ? O10 C10 Fe1 175.3(4) . . ? O11 C11 Fe1 175.0(3) . . ? C13 C12 Fe4 69.5(2) . . ? C13 C12 C16 106.5(3) . . ? C13 C12 C17 126.2(3) . . ? C16 C12 Fe4 68.4(2) . . ? C16 C12 C17 126.9(4) . . ? C17 C12 Fe4 132.3(2) . . ? C12 C13 Fe4 71.6(2) . . ? C12 C13 C14 108.8(4) . . ? C14 C13 Fe4 69.1(2) . . ? C13 C14 Fe4 71.3(2) . . ? C15 C14 Fe4 70.2(2) . . ? C15 C14 C13 107.6(4) . . ? C14 C15 Fe4 70.2(2) . . ? C16 C15 Fe4 70.6(2) . . ? C16 C15 C14 107.9(4) . . ? C12 C16 Fe4 72.3(2) . . ? C15 C16 Fe4 70.1(2) . . ? C15 C16 C12 109.2(4) . . ? C12 C17 C18 110.7(3) . . ? C12 C17 C19 106.9(3) . . ? C18 C17 C19 108.8(3) . . ? C20 C17 C12 111.1(3) . . ? C20 C17 C18 110.4(3) . . ? C20 C17 C19 108.8(3) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 24.04 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.741 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.112 data_fin _database_code_CSD 196899 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.50 H17 Bi Fe4 O11 Se' _chemical_formula_weight 986.71 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 28.682(6) _cell_length_b 11.118(2) _cell_length_c 18.514(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5904(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.07 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3736 _exptl_absorpt_coefficient_mu 9.148 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7623 _exptl_absorpt_correction_T_max 0.9643 _exptl_absorpt_process_details 'program faceit' _exptl_special_details ; None ; _diffrn_ambient_temperature 200(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 IPDS' _diffrn_measurement_method phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_reflns_number 14580 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 24.07 _reflns_number_total 4625 _reflns_number_gt 3314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SIEMENS-XP _computing_publication_material SHELXL-97 _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^)+(0.0466P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4625 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _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 Bi Bi 0.384676(10) 0.08408(2) 0.236303(15) 0.03171(10) Uani 1 1 d . . . Se Se 0.40536(3) -0.10681(7) 0.10787(4) 0.0381(2) Uani 1 1 d . . . Fe1 Fe 0.33393(4) -0.00895(10) 0.12600(6) 0.0338(3) Uani 1 1 d . . . Fe2 Fe 0.41714(4) 0.10605(10) 0.10724(6) 0.0360(3) Uani 1 1 d . . . Fe3 Fe 0.37692(4) -0.14805(10) 0.22626(6) 0.0364(3) Uani 1 1 d . . . Fe4 Fe 0.36059(4) 0.26445(9) 0.31920(5) 0.0312(3) Uani 1 1 d . . . C1 C 0.3220(3) 0.3160(7) 0.2509(4) 0.041(2) Uani 1 1 d . . . O1 O 0.2966(2) 0.3517(6) 0.2083(3) 0.0568(16) Uani 1 1 d . . . C2 C 0.4084(3) 0.3461(8) 0.2866(4) 0.044(2) Uani 1 1 d . . . O2 O 0.4394(3) 0.4034(7) 0.2673(4) 0.069(2) Uani 1 1 d . . . C3 C 0.4284(4) 0.1018(8) 0.0130(5) 0.058(3) Uani 1 1 d . . . O3 O 0.4366(4) 0.0999(7) -0.0482(4) 0.098(3) Uani 1 1 d . . . C4 C 0.4012(3) 0.2628(9) 0.1085(4) 0.043(2) Uani 1 1 d . . . O4 O 0.3899(2) 0.3617(6) 0.1102(3) 0.0584(17) Uani 1 1 d . . . C5 C 0.4747(4) 0.1153(8) 0.1388(5) 0.053(2) Uani 1 1 d . . . O5 O 0.5129(3) 0.1231(7) 0.1575(4) 0.075(2) Uani 1 1 d . . . C6 C 0.4287(4) -0.1784(9) 0.2771(5) 0.057(3) Uani 1 1 d . . . O6 O 0.4618(3) -0.2010(8) 0.3077(4) 0.083(2) Uani 1 1 d . . . C7 C 0.3324(3) -0.1478(7) 0.2930(5) 0.043(2) Uani 1 1 d . . . O7 O 0.3030(2) -0.1473(6) 0.3356(4) 0.0605(18) Uani 1 1 d . . . C8 C 0.3642(3) -0.3015(9) 0.1992(5) 0.052(2) Uani 1 1 d . . . O8 O 0.3568(3) -0.3996(6) 0.1849(4) 0.072(2) Uani 1 1 d . . . C9 C 0.2881(3) 0.0539(8) 0.1793(5) 0.045(2) Uani 1 1 d . . . O9 O 0.2566(2) 0.0914(6) 0.2111(4) 0.0585(17) Uani 1 1 d . . . C10 C 0.3006(3) -0.1393(9) 0.0967(5) 0.049(2) Uani 1 1 d . . . O10 O 0.2792(2) -0.2180(6) 0.0769(4) 0.0636(19) Uani 1 1 d . . . C11 C 0.3246(3) 0.0826(9) 0.0482(5) 0.050(2) Uani 1 1 d . . . O11 O 0.3149(3) 0.1394(7) -0.0009(4) 0.076(2) Uani 1 1 d . . . C12 C 0.3411(3) 0.3553(7) 0.4153(4) 0.0328(17) Uani 1 1 d . . . C13 C 0.3823(3) 0.2890(8) 0.4258(4) 0.040(2) Uani 1 1 d . . . H13 H 0.4114 0.3229 0.4393 0.048 Uiso 1 1 calc R . . C14 C 0.3746(3) 0.1660(7) 0.4136(4) 0.042(2) Uani 1 1 d . . . H14 H 0.3970 0.1034 0.4177 0.050 Uiso 1 1 calc R . . C15 C 0.3281(3) 0.1531(7) 0.3945(4) 0.042(2) Uani 1 1 d . . . H15 H 0.3130 0.0795 0.3827 0.051 Uiso 1 1 calc R . . C16 C 0.3070(3) 0.2667(7) 0.3953(4) 0.0362(18) Uani 1 1 d . . . H16 H 0.2753 0.2827 0.3845 0.043 Uiso 1 1 calc R . . C17 C 0.3328(3) 0.4885(7) 0.4298(4) 0.0319(17) Uani 1 1 d . . . C18 C 0.3764(3) 0.5620(8) 0.4257(6) 0.053(2) Uani 1 1 d . . . H18A H 0.3687 0.6472 0.4319 0.079 Uiso 1 1 calc R . . H18B H 0.3912 0.5501 0.3785 0.079 Uiso 1 1 calc R . . H18C H 0.3979 0.5367 0.4639 0.079 Uiso 1 1 calc R . . C19 C 0.2976(4) 0.5411(8) 0.3760(6) 0.065(3) Uani 1 1 d . . . H19A H 0.2933 0.6270 0.3858 0.097 Uiso 1 1 calc R . . H19B H 0.2676 0.4994 0.3812 0.097 Uiso 1 1 calc R . . H19C H 0.3092 0.5304 0.3267 0.097 Uiso 1 1 calc R . . C20 C 0.3126(4) 0.4974(9) 0.5061(6) 0.068(3) Uani 1 1 d . . . H20A H 0.3047 0.5813 0.5167 0.102 Uiso 1 1 calc R . . H20B H 0.3356 0.4686 0.5411 0.102 Uiso 1 1 calc R . . H20C H 0.2844 0.4478 0.5093 0.102 Uiso 1 1 calc R . . C21 C 0.4842(5) 0.5742(13) 0.1053(8) 0.092(4) Uiso 1 1 d . A -1 C22 C 0.5073(6) 0.4671(17) -0.0446(10) 0.048(5) Uiso 0.50 1 d P A -1 C23 C 0.5018(6) 0.3916(17) 0.0128(14) 0.032(6) Uiso 0.50 1 d P A -1 C24 C 0.4916(8) 0.446(2) 0.0857(16) 0.074(7) Uiso 0.50 1 d P A -1 C25 C 0.4920(8) 0.646(2) 0.0326(14) 0.065(6) Uiso 0.50 1 d P A -1 C26 C 0.5014(6) 0.5897(18) -0.0381(15) 0.036(6) Uiso 0.50 1 d P A -1 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 Bi 0.03889(17) 0.03095(16) 0.02529(16) -0.00216(13) 0.00111(13) 0.00102(13) Se 0.0474(5) 0.0360(4) 0.0307(4) -0.0039(3) 0.0083(4) 0.0004(4) Fe1 0.0403(7) 0.0342(6) 0.0270(6) -0.0008(5) -0.0014(5) -0.0039(5) Fe2 0.0426(7) 0.0377(6) 0.0278(6) -0.0005(5) 0.0060(5) -0.0061(5) Fe3 0.0481(7) 0.0307(6) 0.0304(6) 0.0013(5) 0.0054(5) 0.0054(5) Fe4 0.0366(6) 0.0303(6) 0.0267(6) -0.0018(4) -0.0030(5) 0.0016(5) C1 0.055(5) 0.036(4) 0.032(5) -0.002(4) 0.000(4) 0.008(4) O1 0.070(4) 0.054(4) 0.046(4) 0.003(3) -0.019(3) 0.015(3) C2 0.057(6) 0.049(5) 0.025(4) -0.005(4) -0.004(4) 0.001(5) O2 0.073(5) 0.079(5) 0.055(4) -0.006(4) 0.010(4) -0.037(4) C3 0.084(7) 0.047(6) 0.044(6) -0.007(4) 0.010(5) -0.032(5) O3 0.169(9) 0.085(6) 0.041(4) -0.012(4) 0.033(5) -0.051(6) C4 0.044(5) 0.063(6) 0.022(4) -0.003(4) 0.003(4) -0.012(4) O4 0.083(5) 0.040(4) 0.052(4) 0.006(3) -0.001(3) 0.007(3) C5 0.067(7) 0.037(5) 0.055(6) 0.003(4) 0.011(5) -0.003(5) O5 0.042(4) 0.095(6) 0.087(6) 0.006(4) -0.003(4) -0.005(4) C6 0.068(7) 0.058(6) 0.045(6) 0.000(5) 0.009(5) 0.017(5) O6 0.071(5) 0.114(7) 0.063(5) 0.000(4) -0.016(4) 0.041(5) C7 0.060(6) 0.031(5) 0.039(5) -0.001(4) 0.003(5) 0.003(4) O7 0.065(4) 0.055(4) 0.061(4) -0.001(3) 0.032(4) -0.003(3) C8 0.063(6) 0.065(7) 0.028(5) 0.004(4) 0.014(4) 0.013(5) O8 0.108(6) 0.027(4) 0.081(5) -0.016(3) 0.020(4) -0.009(4) C9 0.048(6) 0.038(5) 0.048(5) 0.003(4) -0.011(4) -0.017(4) O9 0.037(3) 0.064(4) 0.074(5) -0.015(4) 0.017(3) -0.003(3) C10 0.044(5) 0.057(6) 0.045(5) 0.002(5) 0.005(4) 0.005(5) O10 0.071(5) 0.050(4) 0.071(5) -0.014(3) -0.009(4) -0.024(4) C11 0.055(5) 0.054(6) 0.042(5) 0.000(5) -0.006(4) -0.013(5) O11 0.091(6) 0.086(5) 0.050(4) 0.034(4) -0.023(4) -0.018(4) C12 0.034(4) 0.040(4) 0.024(4) -0.001(3) 0.002(3) -0.003(4) C13 0.032(4) 0.057(6) 0.029(4) 0.001(4) -0.005(3) 0.004(4) C14 0.061(6) 0.033(5) 0.032(4) 0.001(4) 0.000(4) 0.018(4) C15 0.063(6) 0.029(4) 0.034(4) 0.000(4) 0.007(4) -0.005(4) C16 0.038(5) 0.035(4) 0.036(4) 0.000(4) -0.002(4) -0.001(4) C17 0.033(4) 0.034(4) 0.029(4) -0.005(3) 0.004(3) -0.001(3) C18 0.050(6) 0.042(5) 0.067(6) -0.008(4) 0.009(5) -0.010(4) C19 0.070(7) 0.038(5) 0.087(8) -0.004(5) -0.025(6) 0.013(5) C20 0.090(8) 0.044(5) 0.069(7) -0.018(5) 0.027(6) -0.008(5) _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 Bi Se 3.2418(9) . ? Bi Fe1 2.7128(11) . ? Bi Fe2 2.5762(12) . ? Bi Fe3 2.5970(12) . ? Bi Fe4 2.6181(11) . ? Se Fe1 2.3438(14) . ? Se Fe2 2.3905(14) . ? Se Fe3 2.3832(14) . ? Fe1 Fe2 2.7297(16) . ? Fe1 Fe3 2.7125(15) . ? Fe1 C9 1.785(10) . ? Fe1 C10 1.819(11) . ? Fe1 C11 1.784(10) . ? Fe2 C3 1.775(10) . ? Fe2 C4 1.801(10) . ? Fe2 C5 1.753(11) . ? Fe3 C6 1.790(11) . ? Fe3 C7 1.778(9) . ? Fe3 C8 1.815(11) . ? Fe4 C1 1.775(9) . ? Fe4 C2 1.751(10) . ? Fe4 C12 2.121(7) . ? Fe4 C13 2.087(8) . ? Fe4 C14 2.101(8) . ? Fe4 C15 2.085(8) . ? Fe4 C16 2.085(8) . ? C1 O1 1.145(9) . ? C2 O2 1.152(10) . ? C3 O3 1.158(11) . ? C4 O4 1.147(11) . ? C5 O5 1.154(11) . ? C6 O6 1.134(11) . ? C7 O7 1.154(10) . ? C8 O8 1.141(11) . ? C9 O9 1.157(11) . ? C10 O10 1.130(11) . ? C11 O11 1.142(11) . ? C12 C13 1.406(11) . ? C12 C16 1.436(11) . ? C12 C17 1.524(11) . ? C13 C14 1.403(12) . ? C14 C15 1.388(12) . ? C15 C16 1.400(11) . ? C17 C18 1.496(11) . ? C17 C19 1.535(12) . ? C17 C20 1.530(12) . ? C21 C24 1.49(3) . ? C21 C25 1.58(3) . ? C22 C23 1.36(3) . ? C22 C26 1.38(3) . ? C23 C24 1.51(3) . ? C25 C26 1.47(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 Fe1 Bi Se 45.28(3) . . ? Fe2 Bi Se 46.81(3) . . ? Fe2 Bi Fe1 62.08(4) . . ? Fe2 Bi Fe3 93.37(3) . . ? Fe2 Bi Fe4 124.51(4) . . ? Fe3 Bi Se 46.58(3) . . ? Fe3 Bi Fe1 61.39(3) . . ? Fe3 Bi Fe4 141.31(4) . . ? Fe4 Bi Se 168.43(3) . . ? Fe4 Bi Fe1 126.29(4) . . ? Fe1 Se Bi 55.33(3) . . ? Fe1 Se Fe2 70.41(4) . . ? Fe1 Se Fe3 70.03(4) . . ? Fe2 Se Bi 51.79(3) . . ? Fe3 Se Bi 52.32(3) . . ? Fe3 Se Fe2 104.09(5) . . ? Bi Fe1 Fe2 56.50(3) . . ? Se Fe1 Bi 79.38(4) . . ? Se Fe1 Fe2 55.59(4) . . ? Se Fe1 Fe3 55.67(4) . . ? Fe3 Fe1 Bi 57.20(3) . . ? Fe3 Fe1 Fe2 87.52(5) . . ? C9 Fe1 Bi 80.2(3) . . ? C9 Fe1 Se 154.7(3) . . ? C9 Fe1 Fe2 122.0(3) . . ? C9 Fe1 Fe3 100.3(3) . . ? C9 Fe1 C10 95.2(4) . . ? C10 Fe1 Bi 144.1(3) . . ? C10 Fe1 Se 92.7(3) . . ? C10 Fe1 Fe2 142.6(3) . . ? C10 Fe1 Fe3 89.3(3) . . ? C11 Fe1 Bi 118.1(3) . . ? C11 Fe1 Se 106.3(3) . . ? C11 Fe1 Fe2 76.2(3) . . ? C11 Fe1 Fe3 161.1(3) . . ? C11 Fe1 C9 96.4(4) . . ? C11 Fe1 C10 97.8(4) . . ? Bi Fe2 Fe1 61.42(3) . . ? Se Fe2 Bi 81.40(4) . . ? Se Fe2 Fe1 53.99(4) . . ? C3 Fe2 Bi 167.2(3) . . ? C3 Fe2 Se 90.3(3) . . ? C3 Fe2 Fe1 105.8(3) . . ? C3 Fe2 C4 94.8(4) . . ? C4 Fe2 Bi 89.3(2) . . ? C4 Fe2 Se 157.2(3) . . ? C4 Fe2 Fe1 103.3(3) . . ? C5 Fe2 Bi 92.1(3) . . ? C5 Fe2 Se 100.9(3) . . ? C5 Fe2 Fe1 143.9(3) . . ? C5 Fe2 C3 99.1(5) . . ? C5 Fe2 C4 100.2(4) . . ? Bi Fe3 Fe1 61.41(3) . . ? Se Fe3 Bi 81.10(4) . . ? Se Fe3 Fe1 54.30(4) . . ? C6 Fe3 Bi 94.5(3) . . ? C6 Fe3 Se 103.6(3) . . ? C6 Fe3 Fe1 147.6(3) . . ? C6 Fe3 C8 97.8(4) . . ? C7 Fe3 Bi 90.6(3) . . ? C7 Fe3 Se 152.3(3) . . ? C7 Fe3 Fe1 98.6(3) . . ? C7 Fe3 C6 103.3(4) . . ? C7 Fe3 C8 92.8(4) . . ? C8 Fe3 Bi 166.1(3) . . ? C8 Fe3 Se 89.7(3) . . ? C8 Fe3 Fe1 104.8(3) . . ? C1 Fe4 Bi 89.7(3) . . ? C1 Fe4 C12 106.2(3) . . ? C1 Fe4 C13 144.8(3) . . ? C1 Fe4 C14 151.6(4) . . ? C1 Fe4 C15 112.9(4) . . ? C1 Fe4 C16 91.0(3) . . ? C2 Fe4 Bi 89.4(3) . . ? C2 Fe4 C1 94.3(4) . . ? C2 Fe4 C12 104.4(3) . . ? C2 Fe4 C13 91.4(4) . . ? C2 Fe4 C14 114.0(4) . . ? C2 Fe4 C15 152.7(4) . . ? C2 Fe4 C16 143.4(3) . . ? C12 Fe4 Bi 157.8(2) . . ? C13 Fe4 Bi 125.2(2) . . ? C13 Fe4 C12 39.0(3) . . ? C13 Fe4 C14 39.2(3) . . ? C14 Fe4 Bi 92.2(2) . . ? C14 Fe4 C12 66.4(3) . . ? C15 Fe4 Bi 93.1(2) . . ? C15 Fe4 C12 66.7(3) . . ? C15 Fe4 C13 65.1(3) . . ? C15 Fe4 C14 38.7(3) . . ? C15 Fe4 C16 39.3(3) . . ? C16 Fe4 Bi 126.9(2) . . ? C16 Fe4 C12 39.9(3) . . ? C16 Fe4 C13 65.1(3) . . ? C16 Fe4 C14 65.4(3) . . ? O1 C1 Fe4 178.0(7) . . ? O2 C2 Fe4 177.2(8) . . ? O3 C3 Fe2 178.7(10) . . ? O4 C4 Fe2 178.0(8) . . ? O5 C5 Fe2 177.8(9) . . ? O6 C6 Fe3 177.6(9) . . ? O7 C7 Fe3 178.9(8) . . ? O8 C8 Fe3 177.1(9) . . ? O9 C9 Fe1 176.0(7) . . ? O10 C10 Fe1 177.7(9) . . ? O11 C11 Fe1 174.5(8) . . ? C13 C12 Fe4 69.2(4) . . ? C13 C12 C16 104.4(7) . . ? C13 C12 C17 128.1(7) . . ? C16 C12 Fe4 68.7(4) . . ? C16 C12 C17 127.3(7) . . ? C17 C12 Fe4 130.7(5) . . ? C12 C13 Fe4 71.8(4) . . ? C14 C13 Fe4 71.0(5) . . ? C14 C13 C12 110.9(7) . . ? C13 C14 Fe4 69.9(4) . . ? C15 C14 Fe4 70.0(5) . . ? C15 C14 C13 107.1(7) . . ? C14 C15 Fe4 71.3(5) . . ? C14 C15 C16 108.5(7) . . ? C16 C15 Fe4 70.4(5) . . ? C12 C16 Fe4 71.4(4) . . ? C15 C16 Fe4 70.3(5) . . ? C15 C16 C12 109.2(7) . . ? C12 C17 C19 111.0(7) . . ? C12 C17 C20 106.5(7) . . ? C18 C17 C12 113.0(7) . . ? C18 C17 C19 108.0(7) . . ? C18 C17 C20 109.2(7) . . ? C20 C17 C19 109.0(8) . . ? C24 C21 C25 104.8(15) . . ? C23 C22 C26 121.7(18) . . ? C22 C23 C24 118.3(19) . . ? C21 C24 C23 129.1(19) . . ? C26 C25 C21 124.7(18) . . ? C22 C26 C25 121.2(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.07 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.724 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.176