# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Prokhorova, Tatiana' _publ_contact_author_email prokh@icp.ac.ru _publ_section_title ; Effect of electrocrystallization medium on quality, structural features, and conducting properties of single crystals of the (BEDT-TTF)4AI[FeIII(C2O4)3]\^a\/cG family ; _publ_author_name T.Prokhorova # Attachment '- I.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3]BN-(I) _database_code_depnum_ccdc_archive 'CCDC 771729' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, C7 H5 N, H3 O' _chemical_formula_sum 'C53 H40 Fe N O13 S32' _chemical_formula_weight 1980.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 10.2650(6) _cell_length_b 20.1499(10) _cell_length_c 35.2161(19) _cell_angle_alpha 90.00 _cell_angle_beta 92.726(5) _cell_angle_gamma 90.00 _cell_volume 7275.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_radiation CuK\a _cell_measurement_reflns_used 27833 _cell_measurement_theta_min 3.7754 _cell_measurement_theta_max 75.7191 _exptl_crystal_description wedge _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4028 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71209 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 42736 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 29.55 _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.592 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.076 _reflns_number_total 9083 _reflns_number_gt 6008 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0587P)^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 9083 _refine_ls_number_parameters 495 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S11 S 0.42229(6) 0.21423(3) 0.508259(18) 0.04085(16) Uani 1 1 d . . . S12 S 0.66380(6) 0.14372(3) 0.531099(18) 0.03873(16) Uani 1 1 d . . . S13 S 0.54212(6) 0.24565(3) 0.426303(19) 0.04069(16) Uani 1 1 d . . . S14 S 0.78050(6) 0.17389(3) 0.450278(18) 0.03965(16) Uani 1 1 d . . . S15 S 0.29380(6) 0.19316(4) 0.57975(2) 0.04703(18) Uani 1 1 d . . . S16 S 0.58500(6) 0.11108(4) 0.608422(19) 0.04446(17) Uani 1 1 d . . . S17 S 0.62134(8) 0.27435(4) 0.34922(2) 0.0554(2) Uani 1 1 d . . . S18 S 0.91024(7) 0.19311(4) 0.37828(2) 0.04956(19) Uani 1 1 d . . . C11 C 0.5760(2) 0.18807(12) 0.49612(7) 0.0342(5) Uani 1 1 d . . . C12 C 0.6268(2) 0.20107(11) 0.46188(7) 0.0329(5) Uani 1 1 d . . . C13 C 0.4327(2) 0.18024(12) 0.55416(7) 0.0342(5) Uani 1 1 d . . . C14 C 0.5438(2) 0.14794(12) 0.56471(6) 0.0323(5) Uani 1 1 d . . . C15 C 0.6643(2) 0.23996(12) 0.39358(7) 0.0363(6) Uani 1 1 d . . . C16 C 0.7737(2) 0.20783(12) 0.40476(7) 0.0353(5) Uani 1 1 d . . . C17 C 0.3504(3) 0.16962(14) 0.62732(8) 0.0463(7) Uani 1 1 d . . . H17A H 0.4038 0.2052 0.6382 0.056 Uiso 1 1 calc R . . H17B H 0.2755 0.1646 0.6429 0.056 Uiso 1 1 calc R . . C18 C 0.4289(2) 0.10585(13) 0.62912(8) 0.0423(6) Uani 1 1 d . . . H18A H 0.3784 0.0712 0.6162 0.051 Uiso 1 1 calc R . . H18B H 0.4421 0.0928 0.6555 0.051 Uiso 1 1 calc R . . C19 C 0.7664(3) 0.26131(19) 0.32346(9) 0.0663(9) Uani 1 1 d . . . H19A H 0.7434 0.2636 0.2965 0.080 Uiso 1 1 calc R . . H19B H 0.8269 0.2972 0.3294 0.080 Uiso 1 1 calc R . . C20 C 0.8350(3) 0.19587(17) 0.33175(9) 0.0631(9) Uani 1 1 d . . . H20A H 0.9008 0.1890 0.3133 0.076 Uiso 1 1 calc R . . H20B H 0.7722 0.1600 0.3290 0.076 Uiso 1 1 calc R . . S21 S 0.02567(6) 0.08860(3) 0.518850(18) 0.04066(16) Uani 1 1 d . . . S22 S 0.25810(6) 0.01234(3) 0.543503(18) 0.03887(16) Uani 1 1 d . . . S23 S 0.15015(6) 0.11825(4) 0.438927(17) 0.04043(16) Uani 1 1 d . . . S24 S 0.38535(6) 0.04362(3) 0.462822(18) 0.03840(16) Uani 1 1 d . . . S25 S -0.11025(7) 0.07079(5) 0.58926(2) 0.0588(2) Uani 1 1 d . . . S26 S 0.16885(6) -0.01702(4) 0.62027(2) 0.04785(19) Uani 1 1 d . . . S27 S 0.24571(7) 0.15756(4) 0.364361(19) 0.0518(2) Uani 1 1 d . . . S28 S 0.52258(6) 0.07238(3) 0.39240(2) 0.04250(17) Uani 1 1 d . . . C21 C 0.1789(2) 0.05988(12) 0.50833(7) 0.0338(5) Uani 1 1 d . . . C22 C 0.2331(2) 0.07317(12) 0.47427(7) 0.0336(5) Uani 1 1 d . . . C23 C 0.0293(2) 0.05462(12) 0.56440(7) 0.0351(5) Uani 1 1 d . A . C24 C 0.1358(2) 0.01955(12) 0.57597(7) 0.0322(5) Uani 1 1 d . A . C25 C 0.2774(2) 0.11753(12) 0.40760(7) 0.0348(5) Uani 1 1 d . B . C26 C 0.3859(2) 0.08383(11) 0.41895(7) 0.0323(5) Uani 1 1 d . B . C27A C -0.0488(7) 0.0538(4) 0.6374(2) 0.0497(16) Uani 0.73 1 d P A 1 H27A H 0.0131 0.0882 0.6452 0.060 Uiso 0.73 1 calc PR A 1 H27B H -0.1208 0.0561 0.6543 0.060 Uiso 0.73 1 calc PR A 1 C28A C 0.0167(4) -0.0128(2) 0.64232(11) 0.0422(9) Uani 0.73 1 d P A 1 H28A H -0.0408 -0.0469 0.6316 0.051 Uiso 0.73 1 calc PR A 1 H28B H 0.0306 -0.0220 0.6692 0.051 Uiso 0.73 1 calc PR A 1 C27B C -0.0870(18) 0.0298(10) 0.6314(6) 0.043(4) Uani 0.27 1 d P A 2 H27C H -0.1432 0.0490 0.6499 0.051 Uiso 0.27 1 calc PR A 2 H27D H -0.1118 -0.0163 0.6279 0.051 Uiso 0.27 1 calc PR A 2 C28B C 0.0531(11) 0.0332(7) 0.6467(3) 0.052(3) Uani 0.27 1 d P A 2 H28C H 0.0568 0.0186 0.6730 0.063 Uiso 0.27 1 calc PR A 2 H28D H 0.0813 0.0792 0.6464 0.063 Uiso 0.27 1 calc PR A 2 C29A C 0.3656(4) 0.1275(2) 0.33354(12) 0.0482(10) Uani 0.81 1 d P B 1 H29A H 0.3236 0.1197 0.3087 0.058 Uiso 0.81 1 calc PR B 1 H29B H 0.4300 0.1622 0.3306 0.058 Uiso 0.81 1 calc PR B 1 C30A C 0.4358(4) 0.0649(2) 0.34609(10) 0.0459(9) Uani 0.81 1 d P B 1 H30A H 0.4978 0.0532 0.3272 0.055 Uiso 0.81 1 calc PR B 1 H30B H 0.3729 0.0292 0.3472 0.055 Uiso 0.81 1 calc PR B 1 C29B C 0.3427(18) 0.0974(9) 0.3377(5) 0.038(4) Uani 0.19 1 d PU B 2 H29C H 0.3091 0.0533 0.3423 0.046 Uiso 0.19 1 calc PR B 2 H29D H 0.3287 0.1065 0.3108 0.046 Uiso 0.19 1 calc PR B 2 C30B C 0.4865(15) 0.0969(9) 0.3470(4) 0.041(4) Uani 0.19 1 d PU B 2 H30C H 0.5211 0.1411 0.3433 0.050 Uiso 0.19 1 calc PR B 2 H30D H 0.5283 0.0671 0.3297 0.050 Uiso 0.19 1 calc PR B 2 Fe1 Fe 0.5000 0.08324(2) 0.7500 0.03434(13) Uani 1 2 d S . . O1 O 0.42460(18) 0.16063(9) 0.71968(5) 0.0454(4) Uani 1 1 d . . . O2 O 0.39347(16) 0.02190(8) 0.71600(5) 0.0402(4) Uani 1 1 d . . . O3 O 0.64921(17) 0.06541(9) 0.71652(5) 0.0431(4) Uani 1 1 d . . . O4 O 0.4074(2) 0.27107(10) 0.71998(7) 0.0626(6) Uani 1 1 d . . . O5 O 0.21787(19) -0.04299(10) 0.71473(6) 0.0565(5) Uani 1 1 d . . . O6 O 0.81623(19) -0.00429(11) 0.71085(6) 0.0593(5) Uani 1 1 d . . . C1 C 0.4511(2) 0.21863(13) 0.73258(8) 0.0437(6) Uani 1 1 d . . . C2 C 0.2937(2) -0.00370(13) 0.73045(7) 0.0385(6) Uani 1 1 d . . . C3 C 0.7283(2) 0.02037(13) 0.72849(7) 0.0400(6) Uani 1 1 d . . . C31 C 0.0138(8) 0.1147(3) 0.7428(2) 0.0593(17) Uiso 0.50 1 d P . . H31 H 0.0160 0.0687 0.7407 0.071 Uiso 0.50 1 calc PR . . C32 C 0.1057(7) 0.1526(4) 0.7252(2) 0.059(2) Uiso 0.50 1 d P . . H32 H 0.1685 0.1315 0.7113 0.071 Uiso 0.50 1 calc PR . . C33 C 0.1063(9) 0.2195(5) 0.7278(3) 0.055(3) Uiso 0.50 1 d P . . H33 H 0.1700 0.2442 0.7162 0.066 Uiso 0.50 1 calc PR . . C34 C 0.0133(9) 0.2503(2) 0.7473(3) 0.0461(14) Uiso 0.50 1 d P . . C35 C -0.0824(9) 0.2134(5) 0.7665(3) 0.051(3) Uiso 0.50 1 d P . . H35 H -0.1440 0.2348 0.7807 0.061 Uiso 0.50 1 calc PR . . C36 C -0.0810(8) 0.1446(4) 0.7633(2) 0.057(2) Uiso 0.50 1 d P . . H36 H -0.1433 0.1190 0.7749 0.069 Uiso 0.50 1 calc PR . . C37 C 0.0180(9) 0.3215(2) 0.7513(3) 0.0555(17) Uiso 0.50 1 d P . . N31 N 0.0232(7) 0.3765(2) 0.7532(2) 0.0666(16) Uiso 0.50 1 d P . . O41 O 0.0096(7) -0.09826(16) 0.75533(18) 0.0588(11) Uiso 0.50 1 d PD . . H41A H 0.039(4) -0.1522(19) 0.7657(17) 0.088 Uiso 0.50 1 d PD . . H41B H 0.090(4) -0.058(2) 0.7650(19) 0.088 Uiso 0.50 1 d PD . . H41C H -0.095(4) -0.082(2) 0.765(2) 0.088 Uiso 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 S11 0.0350(3) 0.0540(4) 0.0338(3) 0.0047(3) 0.0044(3) 0.0108(3) S12 0.0321(3) 0.0523(4) 0.0323(3) 0.0087(3) 0.0067(3) 0.0088(3) S13 0.0358(3) 0.0519(4) 0.0345(3) 0.0065(3) 0.0033(3) 0.0096(3) S14 0.0337(3) 0.0490(4) 0.0366(4) 0.0074(3) 0.0048(3) 0.0080(3) S15 0.0355(3) 0.0623(4) 0.0442(4) 0.0034(3) 0.0121(3) 0.0115(3) S16 0.0397(4) 0.0576(4) 0.0368(4) 0.0134(3) 0.0093(3) 0.0076(3) S17 0.0664(5) 0.0676(5) 0.0320(4) 0.0107(3) -0.0013(3) 0.0067(4) S18 0.0467(4) 0.0505(4) 0.0535(4) 0.0046(3) 0.0237(3) 0.0039(3) C11 0.0296(12) 0.0416(14) 0.0314(13) 0.0003(11) 0.0009(10) 0.0014(10) C12 0.0318(12) 0.0362(13) 0.0307(13) -0.0015(10) 0.0026(10) 0.0016(10) C13 0.0314(13) 0.0412(14) 0.0303(13) 0.0000(11) 0.0062(10) 0.0014(10) C14 0.0340(12) 0.0347(13) 0.0289(12) 0.0000(10) 0.0074(10) -0.0021(10) C15 0.0423(14) 0.0373(13) 0.0294(13) 0.0005(11) 0.0043(11) -0.0008(11) C16 0.0360(13) 0.0361(13) 0.0345(13) 0.0021(11) 0.0080(11) 0.0003(10) C17 0.0465(16) 0.0527(17) 0.0409(15) -0.0003(13) 0.0159(12) 0.0046(12) C18 0.0448(15) 0.0448(15) 0.0384(15) 0.0028(12) 0.0139(12) -0.0028(11) C19 0.066(2) 0.102(3) 0.0318(15) 0.0111(17) 0.0063(14) -0.0221(19) C20 0.068(2) 0.073(2) 0.0494(18) -0.0166(17) 0.0191(16) -0.0091(17) S21 0.0340(3) 0.0595(4) 0.0288(3) 0.0080(3) 0.0052(3) 0.0140(3) S22 0.0342(3) 0.0512(4) 0.0317(3) 0.0078(3) 0.0071(3) 0.0120(3) S23 0.0350(3) 0.0587(4) 0.0283(3) 0.0069(3) 0.0080(3) 0.0149(3) S24 0.0330(3) 0.0484(4) 0.0342(3) 0.0056(3) 0.0056(3) 0.0110(3) S25 0.0427(4) 0.0921(6) 0.0431(4) 0.0216(4) 0.0177(3) 0.0283(4) S26 0.0359(4) 0.0648(5) 0.0435(4) 0.0259(3) 0.0091(3) 0.0079(3) S27 0.0623(4) 0.0617(5) 0.0326(4) 0.0131(3) 0.0159(3) 0.0234(4) S28 0.0344(3) 0.0483(4) 0.0461(4) 0.0010(3) 0.0155(3) 0.0068(3) C21 0.0291(12) 0.0427(14) 0.0297(12) 0.0014(11) 0.0032(10) 0.0046(10) C22 0.0320(12) 0.0402(13) 0.0288(12) -0.0001(10) 0.0046(10) 0.0056(10) C23 0.0349(13) 0.0442(14) 0.0266(12) 0.0063(11) 0.0059(10) 0.0051(10) C24 0.0296(12) 0.0380(13) 0.0295(12) 0.0069(10) 0.0056(10) 0.0014(9) C25 0.0395(14) 0.0384(13) 0.0271(12) 0.0009(10) 0.0087(10) 0.0062(10) C26 0.0329(13) 0.0351(13) 0.0296(12) 0.0005(10) 0.0082(10) 0.0037(9) C27A 0.053(5) 0.062(5) 0.035(3) 0.009(3) 0.009(3) 0.016(3) C28A 0.037(2) 0.054(3) 0.037(2) 0.0136(19) 0.0086(16) 0.0017(18) C27B 0.030(8) 0.067(12) 0.032(8) 0.015(8) 0.010(6) -0.001(6) C28B 0.049(7) 0.069(8) 0.038(6) 0.001(6) -0.003(5) 0.005(6) C29A 0.054(3) 0.058(3) 0.033(2) 0.005(2) 0.0144(17) 0.006(2) C30A 0.054(2) 0.050(2) 0.0348(19) -0.0080(18) 0.0114(18) 0.0080(19) C29B 0.051(8) 0.036(8) 0.029(7) 0.004(6) 0.012(6) -0.005(6) C30B 0.038(7) 0.047(7) 0.041(7) -0.002(6) 0.017(6) -0.007(6) Fe1 0.0403(3) 0.0354(3) 0.0277(3) 0.000 0.0052(2) 0.000 O1 0.0612(12) 0.0393(10) 0.0352(10) 0.0024(8) -0.0036(9) 0.0040(8) O2 0.0442(10) 0.0451(10) 0.0319(9) -0.0021(8) 0.0081(8) -0.0074(8) O3 0.0441(10) 0.0521(11) 0.0339(10) 0.0047(8) 0.0107(8) -0.0013(8) O4 0.0711(14) 0.0415(11) 0.0752(15) 0.0125(11) 0.0047(12) 0.0080(10) O5 0.0506(11) 0.0693(14) 0.0495(12) -0.0051(11) 0.0029(9) -0.0192(10) O6 0.0542(12) 0.0756(14) 0.0499(12) -0.0019(11) 0.0208(10) 0.0117(10) C1 0.0460(15) 0.0406(16) 0.0458(16) 0.0032(13) 0.0167(12) -0.0001(12) C2 0.0412(14) 0.0394(14) 0.0350(14) 0.0039(12) 0.0011(11) 0.0022(11) C3 0.0375(14) 0.0460(15) 0.0371(14) -0.0091(12) 0.0075(12) -0.0052(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.736(2) . ? S11 C13 1.754(2) . ? S12 C11 1.739(2) . ? S12 C14 1.750(2) . ? S13 C12 1.740(2) . ? S13 C15 1.747(2) . ? S14 C12 1.737(2) . ? S14 C16 1.741(3) . ? S15 C13 1.742(2) . ? S15 C17 1.810(3) . ? S16 C14 1.743(2) . ? S16 C18 1.795(2) . ? S17 C15 1.746(3) . ? S17 C19 1.799(3) . ? S18 C16 1.745(2) . ? S18 C20 1.779(3) . ? C11 C12 1.362(3) . ? C13 C14 1.350(3) . ? C15 C16 1.339(3) . ? C17 C18 1.516(4) . ? C19 C20 1.517(5) . ? S21 C21 1.733(2) . ? S21 C23 1.743(2) . ? S22 C21 1.737(2) . ? S22 C24 1.744(2) . ? S23 C22 1.731(2) . ? S23 C25 1.750(2) . ? S24 C22 1.738(2) . ? S24 C26 1.745(2) . ? S25 C27B 1.71(2) . ? S25 C23 1.744(2) . ? S25 C27A 1.814(8) . ? S26 C24 1.744(2) . ? S26 C28A 1.779(3) . ? S26 C28B 1.846(12) . ? S27 C25 1.740(2) . ? S27 C29A 1.785(4) . ? S27 C29B 1.852(18) . ? S28 C30B 1.698(16) . ? S28 C26 1.738(2) . ? S28 C30A 1.827(4) . ? C21 C22 1.372(3) . ? C23 C24 1.349(3) . ? C25 C26 1.348(3) . ? C27A C28A 1.507(9) . ? C27B C28B 1.51(2) . ? C29A C30A 1.509(6) . ? C29B C30B 1.50(2) . ? Fe1 O2 2.0080(17) . ? Fe1 O2 2.0080(17) 2_656 ? Fe1 O3 2.0093(16) . ? Fe1 O3 2.0093(16) 2_656 ? Fe1 O1 2.0229(18) 2_656 ? Fe1 O1 2.0229(18) . ? O1 C1 1.279(3) . ? O2 C2 1.274(3) . ? O3 C3 1.276(3) . ? O4 C1 1.223(3) . ? O5 C2 1.224(3) . ? O6 C3 1.225(3) . ? C1 C1 1.548(6) 2_656 ? C2 C3 1.552(4) 2_656 ? C3 C2 1.552(4) 2_656 ? C31 C36 1.379(11) . ? C31 C32 1.383(10) . ? C32 C33 1.352(12) . ? C33 C34 1.353(12) . ? C34 C35 1.429(12) . ? C34 C37 1.442(6) . ? C35 C36 1.392(12) . ? C37 N31 1.112(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 C11 S11 C13 95.28(11) . . ? C11 S12 C14 95.53(11) . . ? C12 S13 C15 95.22(11) . . ? C12 S14 C16 95.50(11) . . ? C13 S15 C17 101.82(12) . . ? C14 S16 C18 101.53(12) . . ? C15 S17 C19 102.31(14) . . ? C16 S18 C20 99.35(13) . . ? C12 C11 S11 123.40(19) . . ? C12 C11 S12 121.25(18) . . ? S11 C11 S12 115.34(13) . . ? C11 C12 S14 122.55(19) . . ? C11 C12 S13 122.50(18) . . ? S14 C12 S13 114.95(13) . . ? C14 C13 S15 129.15(19) . . ? C14 C13 S11 117.11(17) . . ? S15 C13 S11 113.74(13) . . ? C13 C14 S16 127.93(17) . . ? C13 C14 S12 116.74(18) . . ? S16 C14 S12 115.31(13) . . ? C16 C15 S17 128.86(19) . . ? C16 C15 S13 117.14(19) . . ? S17 C15 S13 113.91(14) . . ? C15 C16 S14 117.17(18) . . ? C15 C16 S18 127.48(19) . . ? S14 C16 S18 115.30(14) . . ? C18 C17 S15 114.02(19) . . ? C17 C18 S16 114.59(18) . . ? C20 C19 S17 114.7(2) . . ? C19 C20 S18 112.5(2) . . ? C21 S21 C23 94.93(11) . . ? C21 S22 C24 95.43(11) . . ? C22 S23 C25 95.31(11) . . ? C22 S24 C26 94.99(11) . . ? C27B S25 C23 105.2(7) . . ? C23 S25 C27A 100.2(3) . . ? C24 S26 C28A 103.47(15) . . ? C24 S26 C28B 96.7(4) . . ? C25 S27 C29A 105.62(16) . . ? C25 S27 C29B 93.3(6) . . ? C30B S28 C26 108.8(5) . . ? C26 S28 C30A 96.86(15) . . ? C22 C21 S21 122.10(19) . . ? C22 C21 S22 122.40(18) . . ? S21 C21 S22 115.50(13) . . ? C21 C22 S23 121.67(18) . . ? C21 C22 S24 122.83(19) . . ? S23 C22 S24 115.46(13) . . ? C24 C23 S21 117.71(17) . . ? C24 C23 S25 128.29(18) . . ? S21 C23 S25 114.00(13) . . ? C23 C24 S22 116.38(17) . . ? C23 C24 S26 127.73(18) . . ? S22 C24 S26 115.84(13) . . ? C26 C25 S27 127.63(18) . . ? C26 C25 S23 116.60(18) . . ? S27 C25 S23 115.70(13) . . ? C25 C26 S28 125.70(18) . . ? C25 C26 S24 117.34(17) . . ? S28 C26 S24 116.83(13) . . ? C28A C27A S25 114.1(5) . . ? C27A C28A S26 112.9(4) . . ? C28B C27B S25 112.3(11) . . ? C27B C28B S26 114.7(10) . . ? C30A C29A S27 116.0(3) . . ? C29A C30A S28 113.5(3) . . ? C30B C29B S27 116.3(12) . . ? C29B C30B S28 112.1(11) . . ? O2 Fe1 O2 104.02(10) . 2_656 ? O2 Fe1 O3 87.06(7) . . ? O2 Fe1 O3 80.27(7) 2_656 . ? O2 Fe1 O3 80.27(7) . 2_656 ? O2 Fe1 O3 87.06(7) 2_656 2_656 ? O3 Fe1 O3 159.39(11) . 2_656 ? O2 Fe1 O1 166.66(7) . 2_656 ? O2 Fe1 O1 88.62(7) 2_656 2_656 ? O3 Fe1 O1 99.46(7) . 2_656 ? O3 Fe1 O1 96.39(7) 2_656 2_656 ? O2 Fe1 O1 88.62(7) . . ? O2 Fe1 O1 166.66(7) 2_656 . ? O3 Fe1 O1 96.39(7) . . ? O3 Fe1 O1 99.46(7) 2_656 . ? O1 Fe1 O1 79.14(11) 2_656 . ? C1 O1 Fe1 116.58(17) . . ? C2 O2 Fe1 115.89(15) . . ? C3 O3 Fe1 115.10(15) . . ? O4 C1 O1 126.3(3) . . ? O4 C1 C1 120.04(17) . 2_656 ? O1 C1 C1 113.62(15) . 2_656 ? O5 C2 O2 126.0(2) . . ? O5 C2 C3 120.4(2) . 2_656 ? O2 C2 C3 113.6(2) . 2_656 ? O6 C3 O3 126.4(2) . . ? O6 C3 C2 119.3(2) . 2_656 ? O3 C3 C2 114.3(2) . 2_656 ? C36 C31 C32 120.5(6) . . ? C33 C32 C31 121.4(8) . . ? C34 C33 C32 119.4(8) . . ? C33 C34 C35 121.3(6) . . ? C33 C34 C37 119.0(8) . . ? C35 C34 C37 119.5(8) . . ? C36 C35 C34 118.1(8) . . ? C31 C36 C35 119.2(8) . . ? N31 C37 C34 177.7(13) . . ? # Attachment '- II.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3]BN-(II) _database_code_depnum_ccdc_archive 'CCDC 771730' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, C7 H5 N, H3 O' _chemical_formula_sum 'C53 H40 Fe N O13 S32' _chemical_formula_weight 1980.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 10.2615(5) _cell_length_b 20.1539(8) _cell_length_c 35.1975(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.633(4) _cell_angle_gamma 90.00 _cell_volume 7271.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_radiation CuK\a _cell_measurement_reflns_used 10863 _cell_measurement_theta_min 3.7845 _cell_measurement_theta_max 75.6454 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4028 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.692 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 53398 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 29.62 _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.790 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.081 _reflns_number_total 8855 _reflns_number_gt 6423 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+3.8406P] 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 8855 _refine_ls_number_parameters 495 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1186 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.005 _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 S11 S 0.42237(6) 0.21422(3) 0.508256(18) 0.03947(16) Uani 1 1 d . . . S12 S 0.66384(6) 0.14368(3) 0.531088(17) 0.03745(15) Uani 1 1 d . . . S13 S 0.54204(6) 0.24567(3) 0.426252(18) 0.03921(16) Uani 1 1 d . . . S14 S 0.78058(6) 0.17384(3) 0.450228(17) 0.03805(15) Uani 1 1 d . . . S15 S 0.29394(6) 0.19313(4) 0.57974(2) 0.04550(17) Uani 1 1 d . . . S16 S 0.58527(6) 0.11104(4) 0.608498(18) 0.04305(17) Uani 1 1 d . . . S17 S 0.62163(8) 0.27453(4) 0.349160(19) 0.0539(2) Uani 1 1 d . . . S18 S 0.91042(7) 0.19316(4) 0.37822(2) 0.04820(18) Uani 1 1 d . . . C11 C 0.5767(2) 0.18816(12) 0.49615(6) 0.0326(5) Uani 1 1 d . . . C12 C 0.6265(2) 0.20136(12) 0.46170(6) 0.0319(5) Uani 1 1 d . . . C13 C 0.4324(2) 0.18018(12) 0.55420(6) 0.0331(5) Uani 1 1 d . . . C14 C 0.5442(2) 0.14798(11) 0.56462(6) 0.0316(5) Uani 1 1 d . . . C15 C 0.6641(2) 0.23977(12) 0.39349(7) 0.0343(5) Uani 1 1 d . . . C16 C 0.7739(2) 0.20781(12) 0.40468(7) 0.0340(5) Uani 1 1 d . . . C17 C 0.3507(3) 0.16957(14) 0.62738(7) 0.0442(6) Uani 1 1 d . . . H17A H 0.4044 0.2051 0.6382 0.053 Uiso 1 1 calc R . . H17B H 0.2758 0.1646 0.6430 0.053 Uiso 1 1 calc R . . C18 C 0.4285(3) 0.10584(13) 0.62893(7) 0.0413(6) Uani 1 1 d . . . H18A H 0.3780 0.0715 0.6157 0.050 Uiso 1 1 calc R . . H18B H 0.4409 0.0923 0.6553 0.050 Uiso 1 1 calc R . . C19 C 0.7664(3) 0.26088(19) 0.32314(9) 0.0662(9) Uani 1 1 d . . . H19A H 0.7430 0.2628 0.2961 0.079 Uiso 1 1 calc R . . H19B H 0.8273 0.2967 0.3289 0.079 Uiso 1 1 calc R . . C20 C 0.8345(3) 0.19581(17) 0.33156(9) 0.0616(8) Uani 1 1 d . . . H20A H 0.9002 0.1887 0.3130 0.074 Uiso 1 1 calc R . . H20B H 0.7715 0.1600 0.3289 0.074 Uiso 1 1 calc R . . S21 S 0.02575(6) 0.08865(3) 0.518785(17) 0.03922(16) Uani 1 1 d . . . S22 S 0.25829(6) 0.01228(3) 0.543457(17) 0.03704(15) Uani 1 1 d . . . S23 S 0.14996(6) 0.11825(3) 0.438849(17) 0.03891(16) Uani 1 1 d . . . S24 S 0.38549(6) 0.04374(3) 0.462783(17) 0.03698(15) Uani 1 1 d . . . S25 S -0.11007(7) 0.07069(5) 0.58923(2) 0.0572(2) Uani 1 1 d . . . S26 S 0.16904(6) -0.01710(4) 0.620347(19) 0.04637(18) Uani 1 1 d . . . S27 S 0.24518(7) 0.15773(4) 0.364215(18) 0.05042(19) Uani 1 1 d . . . S28 S 0.52236(6) 0.07244(3) 0.392301(19) 0.04133(16) Uani 1 1 d . . . C21 C 0.1793(2) 0.05993(12) 0.50835(6) 0.0318(5) Uani 1 1 d . . . C22 C 0.2330(2) 0.07318(12) 0.47421(6) 0.0320(5) Uani 1 1 d . . . C23 C 0.0286(2) 0.05456(13) 0.56438(7) 0.0356(5) Uani 1 1 d . A . C24 C 0.1359(2) 0.01973(12) 0.57594(6) 0.0323(5) Uani 1 1 d . A . C25 C 0.2769(2) 0.11742(12) 0.40752(7) 0.0341(5) Uani 1 1 d . B . C26 C 0.3859(2) 0.08360(11) 0.41879(6) 0.0316(5) Uani 1 1 d . B . C27A C -0.0485(6) 0.0543(3) 0.63785(16) 0.0446(13) Uani 0.71 1 d P A 1 H27A H 0.0136 0.0887 0.6455 0.054 Uiso 0.71 1 calc PR A 1 H27B H -0.1205 0.0566 0.6547 0.054 Uiso 0.71 1 calc PR A 1 C28A C 0.0173(4) -0.0129(2) 0.64249(10) 0.0393(8) Uani 0.71 1 d P A 1 H28A H -0.0404 -0.0468 0.6316 0.047 Uiso 0.71 1 calc PR A 1 H28B H 0.0313 -0.0224 0.6694 0.047 Uiso 0.71 1 calc PR A 1 C27B C -0.0879(13) 0.0304(7) 0.6313(4) 0.039(3) Uani 0.29 1 d P A 2 H27C H -0.1440 0.0499 0.6497 0.047 Uiso 0.29 1 calc PR A 2 H27D H -0.1132 -0.0157 0.6279 0.047 Uiso 0.29 1 calc PR A 2 C28B C 0.0532(11) 0.0334(7) 0.6468(3) 0.052(2) Uani 0.29 1 d P A 2 H28C H 0.0564 0.0188 0.6731 0.063 Uiso 0.29 1 calc PR A 2 H28D H 0.0819 0.0793 0.6466 0.063 Uiso 0.29 1 calc PR A 2 C29A C 0.3671(5) 0.1279(3) 0.33355(16) 0.0464(12) Uani 0.78 1 d P B 1 H29A H 0.3266 0.1209 0.3084 0.056 Uiso 0.78 1 calc PR B 1 H29B H 0.4327 0.1622 0.3313 0.056 Uiso 0.78 1 calc PR B 1 C30A C 0.4351(4) 0.0641(2) 0.34617(11) 0.0430(9) Uani 0.78 1 d P B 1 H30A H 0.4964 0.0513 0.3273 0.052 Uiso 0.78 1 calc PR B 1 H30B H 0.3708 0.0290 0.3476 0.052 Uiso 0.78 1 calc PR B 1 C29B C 0.338(2) 0.1013(11) 0.3362(6) 0.051(5) Uani 0.22 1 d PU B 2 H29C H 0.2992 0.0576 0.3382 0.061 Uiso 0.22 1 calc PR B 2 H29D H 0.3269 0.1149 0.3098 0.061 Uiso 0.22 1 calc PR B 2 C30B C 0.4832(16) 0.0951(9) 0.3460(4) 0.053(4) Uani 0.22 1 d PU B 2 H30C H 0.5244 0.1374 0.3410 0.064 Uiso 0.22 1 calc PR B 2 H30D H 0.5196 0.0626 0.3291 0.064 Uiso 0.22 1 calc PR B 2 Fe1 Fe 0.5000 0.08339(2) 0.7500 0.03211(13) Uani 1 2 d S . . O1 O 0.42436(18) 0.16071(9) 0.71968(5) 0.0438(4) Uani 1 1 d . . . O2 O 0.39388(16) 0.02185(8) 0.71594(4) 0.0381(4) Uani 1 1 d . . . O3 O 0.64893(17) 0.06554(9) 0.71653(5) 0.0404(4) Uani 1 1 d . . . O4 O 0.4069(2) 0.27111(10) 0.71981(6) 0.0601(6) Uani 1 1 d . . . O5 O 0.21851(19) -0.04330(11) 0.71470(6) 0.0557(5) Uani 1 1 d . . . O6 O 0.81619(19) -0.00407(11) 0.71089(6) 0.0581(5) Uani 1 1 d . . . C1 C 0.4507(2) 0.21868(13) 0.73252(7) 0.0418(6) Uani 1 1 d . . . C2 C 0.2939(2) -0.00374(12) 0.73027(7) 0.0363(5) Uani 1 1 d . . . C3 C 0.7285(2) 0.02033(13) 0.72861(7) 0.0380(6) Uani 1 1 d . . . C31 C 0.0120(8) 0.1150(3) 0.7425(2) 0.0610(18) Uiso 0.50 1 d P . . H31 H 0.0119 0.0690 0.7400 0.073 Uiso 0.50 1 calc PR . . C32 C 0.1053(7) 0.1515(4) 0.7252(2) 0.058(2) Uiso 0.50 1 d P . . H32 H 0.1692 0.1303 0.7118 0.069 Uiso 0.50 1 calc PR . . C33 C 0.1044(9) 0.2198(5) 0.7279(3) 0.050(2) Uiso 0.50 1 d P . . H33 H 0.1671 0.2446 0.7160 0.060 Uiso 0.50 1 calc PR . . C34 C 0.0132(9) 0.2506(2) 0.7477(3) 0.0454(14) Uiso 0.50 1 d P . . C35 C -0.0829(9) 0.2123(5) 0.7664(3) 0.058(3) Uiso 0.50 1 d P . . H35 H -0.1457 0.2330 0.7804 0.069 Uiso 0.50 1 calc PR . . C36 C -0.0801(8) 0.1446(4) 0.7630(2) 0.061(2) Uiso 0.50 1 d P . . H36 H -0.1416 0.1189 0.7749 0.073 Uiso 0.50 1 calc PR . . C37 C 0.0183(8) 0.3208(2) 0.7514(3) 0.0532(15) Uiso 0.50 1 d P . . N31 N 0.0225(8) 0.3777(3) 0.7530(3) 0.0740(17) Uiso 0.50 1 d P . . O41 O 0.0094(7) -0.09763(16) 0.75539(17) 0.0559(11) Uiso 0.50 1 d PD . . H41A H 0.036(5) -0.1510(19) 0.7647(17) 0.084 Uiso 0.50 1 d PD . . H41B H 0.093(4) -0.060(2) 0.7639(19) 0.084 Uiso 0.50 1 d PD . . H41C H -0.088(5) -0.079(2) 0.768(2) 0.084 Uiso 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 S11 0.0340(3) 0.0520(4) 0.0326(3) 0.0053(3) 0.0033(3) 0.0103(3) S12 0.0316(3) 0.0504(4) 0.0307(3) 0.0081(3) 0.0062(2) 0.0081(3) S13 0.0341(3) 0.0505(4) 0.0331(3) 0.0066(3) 0.0022(3) 0.0094(3) S14 0.0330(3) 0.0467(4) 0.0348(3) 0.0077(3) 0.0039(3) 0.0076(3) S15 0.0345(3) 0.0601(4) 0.0428(4) 0.0037(3) 0.0114(3) 0.0112(3) S16 0.0390(3) 0.0555(4) 0.0352(3) 0.0133(3) 0.0085(3) 0.0078(3) S17 0.0656(5) 0.0658(5) 0.0298(3) 0.0111(3) -0.0015(3) 0.0062(4) S18 0.0458(4) 0.0489(4) 0.0518(4) 0.0049(3) 0.0220(3) 0.0042(3) C11 0.0292(11) 0.0393(13) 0.0293(11) 0.0015(9) 0.0006(10) 0.0007(9) C12 0.0302(11) 0.0374(13) 0.0278(11) 0.0014(9) 0.0000(9) 0.0012(9) C13 0.0342(12) 0.0378(13) 0.0278(11) -0.0014(9) 0.0059(10) 0.0002(10) C14 0.0319(11) 0.0350(13) 0.0281(11) 0.0016(9) 0.0050(9) 0.0001(9) C15 0.0402(13) 0.0337(13) 0.0289(12) 0.0015(9) 0.0021(10) 0.0005(10) C16 0.0361(12) 0.0342(13) 0.0323(12) 0.0020(10) 0.0068(10) -0.0014(10) C17 0.0472(14) 0.0488(16) 0.0378(14) -0.0007(11) 0.0147(12) 0.0044(12) C18 0.0454(14) 0.0422(15) 0.0372(13) 0.0043(11) 0.0106(11) -0.0024(11) C19 0.067(2) 0.100(3) 0.0315(14) 0.0107(16) 0.0029(15) -0.0170(19) C20 0.071(2) 0.071(2) 0.0442(16) -0.0136(15) 0.0174(15) -0.0087(17) S21 0.0337(3) 0.0564(4) 0.0278(3) 0.0080(3) 0.0044(2) 0.0135(3) S22 0.0328(3) 0.0485(4) 0.0302(3) 0.0076(3) 0.0055(2) 0.0113(3) S23 0.0338(3) 0.0569(4) 0.0264(3) 0.0063(3) 0.0066(2) 0.0141(3) S24 0.0323(3) 0.0463(4) 0.0326(3) 0.0054(3) 0.0044(2) 0.0107(3) S25 0.0414(4) 0.0896(6) 0.0420(4) 0.0215(4) 0.0165(3) 0.0278(4) S26 0.0355(3) 0.0622(5) 0.0421(4) 0.0252(3) 0.0076(3) 0.0076(3) S27 0.0619(4) 0.0591(5) 0.0315(3) 0.0127(3) 0.0153(3) 0.0230(3) S28 0.0339(3) 0.0461(4) 0.0453(4) 0.0010(3) 0.0155(3) 0.0066(3) C21 0.0295(11) 0.0397(13) 0.0261(11) 0.0014(9) 0.0018(9) 0.0038(9) C22 0.0311(11) 0.0379(13) 0.0271(11) -0.0002(9) 0.0031(10) 0.0060(9) C23 0.0345(12) 0.0428(14) 0.0297(12) 0.0070(10) 0.0050(10) 0.0057(10) C24 0.0280(11) 0.0375(13) 0.0318(12) 0.0059(10) 0.0048(10) 0.0018(9) C25 0.0374(12) 0.0361(13) 0.0293(11) 0.0012(10) 0.0070(10) 0.0076(10) C26 0.0319(11) 0.0346(13) 0.0288(11) 0.0008(9) 0.0064(10) 0.0019(9) C27A 0.049(4) 0.054(4) 0.031(2) 0.005(2) 0.006(2) 0.010(2) C28A 0.0362(19) 0.046(2) 0.0365(19) 0.0144(17) 0.0095(15) 0.0025(17) C27B 0.033(6) 0.050(9) 0.033(6) 0.014(6) 0.005(5) 0.001(5) C28B 0.057(7) 0.065(8) 0.035(5) 0.008(5) 0.003(5) 0.009(6) C29A 0.047(3) 0.060(3) 0.033(2) 0.006(2) 0.013(2) 0.001(2) C30A 0.049(2) 0.046(2) 0.0355(18) -0.0080(17) 0.0140(18) 0.0040(18) C29B 0.059(10) 0.070(12) 0.027(7) -0.011(8) 0.021(7) -0.015(8) C30B 0.054(9) 0.057(9) 0.050(8) 0.002(7) 0.014(7) 0.001(7) Fe1 0.0381(3) 0.0324(3) 0.0261(2) 0.000 0.0044(2) 0.000 O1 0.0592(11) 0.0355(10) 0.0363(9) 0.0030(7) -0.0031(8) 0.0037(8) O2 0.0439(9) 0.0415(10) 0.0297(8) -0.0041(7) 0.0088(8) -0.0069(8) O3 0.0424(9) 0.0491(11) 0.0303(9) 0.0036(7) 0.0084(8) -0.0024(8) O4 0.0689(13) 0.0370(11) 0.0744(15) 0.0123(10) 0.0037(12) 0.0066(10) O5 0.0497(11) 0.0671(14) 0.0504(11) -0.0070(10) 0.0029(9) -0.0203(10) O6 0.0536(12) 0.0737(14) 0.0488(12) 0.0002(10) 0.0211(10) 0.0128(10) C1 0.0456(14) 0.0374(15) 0.0435(15) 0.0054(11) 0.0146(12) 0.0009(11) C2 0.0382(13) 0.0357(13) 0.0350(13) 0.0025(10) 0.0018(11) 0.0000(10) C3 0.0339(12) 0.0444(15) 0.0363(13) -0.0077(11) 0.0086(11) -0.0039(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.740(2) . ? S11 C13 1.755(2) . ? S12 C11 1.736(2) . ? S12 C14 1.744(2) . ? S13 C12 1.734(2) . ? S13 C15 1.745(2) . ? S14 C12 1.741(2) . ? S14 C16 1.742(2) . ? S15 C13 1.736(2) . ? S15 C17 1.813(3) . ? S16 C14 1.748(2) . ? S16 C18 1.795(2) . ? S17 C15 1.747(2) . ? S17 C19 1.802(3) . ? S18 C16 1.742(2) . ? S18 C20 1.786(3) . ? C11 C12 1.363(3) . ? C13 C14 1.354(3) . ? C15 C16 1.341(3) . ? C17 C18 1.512(4) . ? C19 C20 1.509(5) . ? S21 C21 1.734(2) . ? S21 C23 1.745(2) . ? S22 C21 1.736(2) . ? S22 C24 1.743(2) . ? S23 C22 1.733(2) . ? S23 C25 1.745(2) . ? S24 C22 1.738(2) . ? S24 C26 1.744(2) . ? S25 C27B 1.695(14) . ? S25 C23 1.735(2) . ? S25 C27A 1.827(6) . ? S26 C24 1.750(2) . ? S26 C28A 1.775(3) . ? S26 C28B 1.849(11) . ? S27 C25 1.745(2) . ? S27 C29A 1.793(6) . ? S27 C29B 1.80(2) . ? S28 C30B 1.723(16) . ? S28 C26 1.732(2) . ? S28 C30A 1.826(4) . ? C21 C22 1.371(3) . ? C23 C24 1.353(3) . ? C25 C26 1.353(3) . ? C27A C28A 1.520(7) . ? C27B C28B 1.525(16) . ? C29A C30A 1.520(7) . ? C29B C30B 1.52(3) . ? Fe1 O3 2.0045(16) 2_656 ? Fe1 O3 2.0045(16) . ? Fe1 O2 2.0103(16) 2_656 ? Fe1 O2 2.0103(17) . ? Fe1 O1 2.0233(17) 2_656 ? Fe1 O1 2.0233(17) . ? O1 C1 1.277(3) . ? O2 C2 1.273(3) . ? O3 C3 1.283(3) . ? O4 C1 1.225(3) . ? O5 C2 1.223(3) . ? O6 C3 1.222(3) . ? C1 C1 1.556(6) 2_656 ? C2 C3 1.554(3) 2_656 ? C3 C2 1.554(3) 2_656 ? C31 C36 1.356(12) . ? C31 C32 1.371(10) . ? C32 C33 1.379(12) . ? C33 C34 1.343(13) . ? C34 C37 1.421(6) . ? C34 C35 1.435(13) . ? C35 C36 1.370(12) . ? C37 N31 1.149(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 C11 S11 C13 95.29(11) . . ? C11 S12 C14 95.61(11) . . ? C12 S13 C15 95.18(11) . . ? C12 S14 C16 95.20(11) . . ? C13 S15 C17 101.78(12) . . ? C14 S16 C18 101.22(12) . . ? C15 S17 C19 102.40(14) . . ? C16 S18 C20 99.15(13) . . ? C12 C11 S12 121.90(18) . . ? C12 C11 S11 122.80(19) . . ? S12 C11 S11 115.31(13) . . ? C11 C12 S13 123.02(18) . . ? C11 C12 S14 121.73(18) . . ? S13 C12 S14 115.24(13) . . ? C14 C13 S15 129.44(18) . . ? C14 C13 S11 116.74(17) . . ? S15 C13 S11 113.82(13) . . ? C13 C14 S12 117.04(17) . . ? C13 C14 S16 127.61(17) . . ? S12 C14 S16 115.34(13) . . ? C16 C15 S13 117.22(18) . . ? C16 C15 S17 128.81(19) . . ? S13 C15 S17 113.92(14) . . ? C15 C16 S14 117.13(17) . . ? C15 C16 S18 127.55(19) . . ? S14 C16 S18 115.27(14) . . ? C18 C17 S15 113.73(18) . . ? C17 C18 S16 114.68(18) . . ? C20 C19 S17 114.7(2) . . ? C19 C20 S18 112.6(2) . . ? C21 S21 C23 94.96(11) . . ? C21 S22 C24 95.29(11) . . ? C22 S23 C25 95.30(11) . . ? C22 S24 C26 94.99(11) . . ? C27B S25 C23 105.7(5) . . ? C23 S25 C27A 100.5(2) . . ? C24 S26 C28A 103.52(14) . . ? C24 S26 C28B 96.5(3) . . ? C25 S27 C29A 105.22(19) . . ? C25 S27 C29B 95.9(7) . . ? C30B S28 C26 108.4(5) . . ? C26 S28 C30A 96.62(15) . . ? C22 C21 S21 121.77(19) . . ? C22 C21 S22 122.55(18) . . ? S21 C21 S22 115.66(13) . . ? C21 C22 S23 121.83(18) . . ? C21 C22 S24 122.61(19) . . ? S23 C22 S24 115.52(13) . . ? C24 C23 S25 128.38(18) . . ? C24 C23 S21 117.38(17) . . ? S25 C23 S21 114.24(13) . . ? C23 C24 S22 116.65(18) . . ? C23 C24 S26 127.66(18) . . ? S22 C24 S26 115.67(13) . . ? C26 C25 S27 127.52(18) . . ? C26 C25 S23 116.76(18) . . ? S27 C25 S23 115.66(13) . . ? C25 C26 S28 125.81(18) . . ? C25 C26 S24 117.17(17) . . ? S28 C26 S24 116.92(13) . . ? C28A C27A S25 113.2(4) . . ? C27A C28A S26 112.9(3) . . ? C28B C27B S25 112.4(9) . . ? C27B C28B S26 114.8(9) . . ? C30A C29A S27 115.6(3) . . ? C29A C30A S28 112.4(3) . . ? C30B C29B S27 117.6(14) . . ? C29B C30B S28 114.8(12) . . ? O3 Fe1 O3 159.32(11) 2_656 . ? O3 Fe1 O2 86.88(7) 2_656 2_656 ? O3 Fe1 O2 80.39(7) . 2_656 ? O3 Fe1 O2 80.39(7) 2_656 . ? O3 Fe1 O2 86.88(7) . . ? O2 Fe1 O2 103.82(10) 2_656 . ? O3 Fe1 O1 96.46(7) 2_656 2_656 ? O3 Fe1 O1 99.43(7) . 2_656 ? O2 Fe1 O1 88.64(7) 2_656 2_656 ? O2 Fe1 O1 166.88(7) . 2_656 ? O3 Fe1 O1 99.43(7) 2_656 . ? O3 Fe1 O1 96.46(7) . . ? O2 Fe1 O1 166.88(7) 2_656 . ? O2 Fe1 O1 88.64(7) . . ? O1 Fe1 O1 79.26(10) 2_656 . ? C1 O1 Fe1 116.61(17) . . ? C2 O2 Fe1 115.98(15) . . ? C3 O3 Fe1 115.06(15) . . ? O4 C1 O1 126.3(3) . . ? O4 C1 C1 120.19(17) . 2_656 ? O1 C1 C1 113.53(15) . 2_656 ? O5 C2 O2 126.3(2) . . ? O5 C2 C3 120.2(2) . 2_656 ? O2 C2 C3 113.5(2) . 2_656 ? O6 C3 O3 126.1(2) . . ? O6 C3 C2 119.6(2) . 2_656 ? O3 C3 C2 114.30(19) . 2_656 ? C36 C31 C32 121.2(6) . . ? C31 C32 C33 119.9(8) . . ? C34 C33 C32 120.2(8) . . ? C33 C34 C37 118.9(8) . . ? C33 C34 C35 120.0(6) . . ? C37 C34 C35 121.1(8) . . ? C36 C35 C34 118.6(8) . . ? C31 C36 C35 120.1(8) . . ? N31 C37 C34 177.7(12) . . ? # Attachment '- III.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3]CB-(III) _database_code_depnum_ccdc_archive 'CCDC 771731' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, C6 H5 Cl, H3 O' _chemical_formula_sum 'C52 H40 Cl Fe O13 S32' _chemical_formula_weight 1990.06 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 10.2854(4) _cell_length_b 20.0124(10) _cell_length_c 35.3666(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.093(4) _cell_angle_gamma 90.00 _cell_volume 7269.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_radiation CuK\a _cell_measurement_reflns_used 16274 _cell_measurement_theta_min 3.7518 _cell_measurement_theta_max 77.7637 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4044 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76615 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29344 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 29.58 _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.974 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.071 _reflns_number_total 9013 _reflns_number_gt 7261 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0422P)^2^+13.3483P] 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 9013 _refine_ls_number_parameters 497 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S11 S 0.42294(6) 0.21401(3) 0.508618(16) 0.03727(13) Uani 1 1 d . . . S12 S 0.66452(5) 0.14341(3) 0.531275(16) 0.03449(13) Uani 1 1 d . . . S13 S 0.54014(6) 0.24576(3) 0.427054(16) 0.03737(14) Uani 1 1 d . . . S14 S 0.77923(6) 0.17412(3) 0.450719(16) 0.03591(13) Uani 1 1 d . . . S15 S 0.29654(6) 0.19322(4) 0.579846(19) 0.04361(15) Uani 1 1 d . . . S16 S 0.58822(6) 0.11086(3) 0.608307(17) 0.04053(15) Uani 1 1 d . . . S17 S 0.61614(8) 0.27392(4) 0.350124(18) 0.05430(19) Uani 1 1 d . . . S18 S 0.90682(7) 0.19336(3) 0.37906(2) 0.04744(16) Uani 1 1 d . . . C11 C 0.5764(2) 0.18794(11) 0.49651(6) 0.0298(4) Uani 1 1 d . . . C12 C 0.6258(2) 0.20131(11) 0.46232(6) 0.0298(4) Uani 1 1 d . . . C13 C 0.4346(2) 0.17994(11) 0.55426(6) 0.0314(4) Uani 1 1 d . . . C14 C 0.5458(2) 0.14762(11) 0.56480(6) 0.0302(4) Uani 1 1 d . . . C15 C 0.6607(2) 0.23977(11) 0.39416(6) 0.0342(5) Uani 1 1 d . . . C16 C 0.7708(2) 0.20798(11) 0.40532(6) 0.0333(5) Uani 1 1 d . . . C17 C 0.3551(3) 0.17002(13) 0.62719(7) 0.0417(6) Uani 1 1 d . . . H17A H 0.4091 0.2059 0.6377 0.050 Uiso 1 1 calc R . . H17B H 0.2811 0.1653 0.6429 0.050 Uiso 1 1 calc R . . C18 C 0.4327(2) 0.10590(13) 0.62908(7) 0.0398(5) Uani 1 1 d . . . H18A H 0.3817 0.0710 0.6163 0.048 Uiso 1 1 calc R . . H18B H 0.4465 0.0929 0.6554 0.048 Uiso 1 1 calc R . . C19 C 0.7610(3) 0.26134(19) 0.32428(8) 0.0676(10) Uani 1 1 d . . . H19A H 0.7373 0.2634 0.2974 0.081 Uiso 1 1 calc R . . H19B H 0.8211 0.2977 0.3302 0.081 Uiso 1 1 calc R . . C20 C 0.8299(3) 0.19617(18) 0.33265(8) 0.0636(9) Uani 1 1 d . . . H20A H 0.8950 0.1893 0.3142 0.076 Uiso 1 1 calc R . . H20B H 0.7674 0.1599 0.3300 0.076 Uiso 1 1 calc R . . S21 S 0.02578(5) 0.08841(3) 0.519487(15) 0.03655(14) Uani 1 1 d . . . S22 S 0.25889(5) 0.01206(3) 0.543879(15) 0.03479(13) Uani 1 1 d . . . S23 S 0.14757(5) 0.11765(3) 0.439626(15) 0.03627(14) Uani 1 1 d . . . S24 S 0.38320(5) 0.04276(3) 0.463484(16) 0.03438(13) Uani 1 1 d . . . S25 S -0.10733(7) 0.07133(4) 0.589708(19) 0.0537(2) Uani 1 1 d . . . S26 S 0.17246(6) -0.01661(4) 0.620641(18) 0.04344(16) Uani 1 1 d . . . S27 S 0.24339(7) 0.15737(4) 0.365468(18) 0.04866(17) Uani 1 1 d . . . S28 S 0.51977(6) 0.07217(3) 0.393818(18) 0.03920(14) Uani 1 1 d . . . C21 C 0.1791(2) 0.05967(11) 0.50888(6) 0.0292(4) Uani 1 1 d . . . C22 C 0.2314(2) 0.07240(11) 0.47498(6) 0.0289(4) Uani 1 1 d . . . C23 C 0.0305(2) 0.05470(12) 0.56491(6) 0.0323(5) Uani 1 1 d . A . C24 C 0.1377(2) 0.01988(11) 0.57651(6) 0.0295(4) Uani 1 1 d . A . C25 C 0.2743(2) 0.11732(11) 0.40860(6) 0.0315(5) Uani 1 1 d . B . C26 C 0.3829(2) 0.08338(11) 0.41994(6) 0.0300(4) Uani 1 1 d . B . C27A C -0.0449(6) 0.0534(3) 0.63802(17) 0.0432(13) Uani 0.68 1 d P A 1 H27A H 0.0164 0.0881 0.6460 0.052 Uiso 0.68 1 calc PR A 1 H27B H -0.1167 0.0549 0.6547 0.052 Uiso 0.68 1 calc PR A 1 C28A C 0.0211(3) -0.0132(2) 0.64223(10) 0.0391(8) Uani 0.68 1 d P A 1 H28A H -0.0359 -0.0473 0.6311 0.047 Uiso 0.68 1 calc PR A 1 H28B H 0.0352 -0.0232 0.6690 0.047 Uiso 0.68 1 calc PR A 1 C27B C -0.0845(12) 0.0307(7) 0.6317(4) 0.045(3) Uani 0.32 1 d P A 2 H27C H -0.1408 0.0500 0.6499 0.055 Uiso 0.32 1 calc PR A 2 H27D H -0.1087 -0.0159 0.6284 0.055 Uiso 0.32 1 calc PR A 2 C28B C 0.0570(9) 0.0348(5) 0.6474(2) 0.0463(19) Uani 0.32 1 d P A 2 H28C H 0.0612 0.0203 0.6736 0.056 Uiso 0.32 1 calc PR A 2 H28D H 0.0848 0.0811 0.6469 0.056 Uiso 0.32 1 calc PR A 2 C29A C 0.3596(6) 0.1258(3) 0.33477(16) 0.0454(12) Uani 0.68 1 d P B 1 H29A H 0.3156 0.1171 0.3103 0.054 Uiso 0.68 1 calc PR B 1 H29B H 0.4237 0.1605 0.3311 0.054 Uiso 0.68 1 calc PR B 1 C30A C 0.4303(5) 0.0634(2) 0.34753(10) 0.0419(9) Uani 0.68 1 d P B 1 H30A H 0.4912 0.0512 0.3287 0.050 Uiso 0.68 1 calc PR B 1 H30B H 0.3677 0.0273 0.3490 0.050 Uiso 0.68 1 calc PR B 1 C29B C 0.3366(12) 0.0965(6) 0.3378(3) 0.041(2) Uani 0.32 1 d P B 2 H29C H 0.3030 0.0520 0.3422 0.050 Uiso 0.32 1 calc PR B 2 H29D H 0.3218 0.1064 0.3111 0.050 Uiso 0.32 1 calc PR B 2 C30B C 0.4813(9) 0.0966(5) 0.3475(2) 0.0429(19) Uani 0.32 1 d P B 2 H30C H 0.5152 0.1412 0.3436 0.052 Uiso 0.32 1 calc PR B 2 H30D H 0.5234 0.0666 0.3304 0.052 Uiso 0.32 1 calc PR B 2 Fe1 Fe 0.5000 0.08154(2) 0.7500 0.03493(11) Uani 1 2 d S . . O1 O 0.42779(19) 0.15861(9) 0.71901(5) 0.0470(4) Uani 1 1 d . . . O2 O 0.39749(17) 0.01676(9) 0.71695(5) 0.0420(4) Uani 1 1 d . . . O3 O 0.65117(17) 0.06578(9) 0.71735(5) 0.0422(4) Uani 1 1 d . . . O4 O 0.4145(2) 0.26985(10) 0.71821(7) 0.0629(6) Uani 1 1 d . . . O5 O 0.21910(19) -0.04594(11) 0.71499(5) 0.0543(5) Uani 1 1 d . . . O6 O 0.8222(2) -0.00133(11) 0.71237(6) 0.0592(5) Uani 1 1 d . . . C1 C 0.4540(3) 0.21691(13) 0.73186(7) 0.0441(6) Uani 1 1 d . . . C2 C 0.2941(2) -0.00624(12) 0.73049(7) 0.0376(5) Uani 1 1 d . . . C3 C 0.7316(2) 0.02105(13) 0.72929(7) 0.0391(5) Uani 1 1 d . . . Cl31 Cl 0.0168(18) 0.34935(9) 0.7531(5) 0.085(3) Uani 0.50 1 d P . . C31 C 0.0132(8) 0.1266(3) 0.7426(2) 0.0620(17) Uiso 0.50 1 d P . . H31 H 0.0136 0.0804 0.7396 0.074 Uiso 0.50 1 calc PR . . C32 C 0.1082(8) 0.1657(4) 0.7262(2) 0.063(2) Uiso 0.50 1 d P . . H32 H 0.1733 0.1453 0.7130 0.076 Uiso 0.50 1 calc PR . . C33 C 0.1051(9) 0.2350(4) 0.7295(3) 0.051(2) Uiso 0.50 1 d P . . H33 H 0.1669 0.2611 0.7181 0.061 Uiso 0.50 1 calc PR . . C34 C 0.0158(8) 0.2628(2) 0.7484(3) 0.0461(13) Uiso 0.50 1 d P . . C35 C -0.0851(9) 0.2238(5) 0.7662(3) 0.057(3) Uiso 0.50 1 d P . . H35 H -0.1500 0.2448 0.7791 0.068 Uiso 0.50 1 calc PR . . C36 C -0.0813(8) 0.1566(4) 0.7633(2) 0.0573(18) Uiso 0.50 1 d P . . H36 H -0.1418 0.1305 0.7752 0.069 Uiso 0.50 1 calc PR . . O41 O 0.0095(7) -0.09922(16) 0.75499(18) 0.0562(11) Uiso 0.50 1 d PD . . H41A H 0.042(5) -0.150(2) 0.7692(17) 0.084 Uiso 0.50 1 d PD . . H41B H 0.085(5) -0.058(2) 0.7648(19) 0.084 Uiso 0.50 1 d PD . . H41C H -0.092(5) -0.084(2) 0.766(2) 0.084 Uiso 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 S11 0.0314(3) 0.0487(3) 0.0318(3) 0.0040(2) 0.0028(2) 0.0094(3) S12 0.0294(3) 0.0452(3) 0.0294(3) 0.0074(2) 0.0054(2) 0.0076(2) S13 0.0334(3) 0.0469(3) 0.0317(3) 0.0055(2) 0.0003(2) 0.0091(3) S14 0.0306(3) 0.0431(3) 0.0342(3) 0.0063(2) 0.0034(2) 0.0066(2) S15 0.0328(3) 0.0570(4) 0.0420(3) 0.0029(3) 0.0108(2) 0.0108(3) S16 0.0361(3) 0.0523(4) 0.0337(3) 0.0130(3) 0.0074(2) 0.0065(3) S17 0.0712(5) 0.0625(4) 0.0286(3) 0.0095(3) -0.0032(3) 0.0062(4) S18 0.0474(4) 0.0458(4) 0.0512(4) 0.0028(3) 0.0228(3) 0.0022(3) C11 0.0272(10) 0.0341(11) 0.0281(10) 0.0008(8) 0.0021(8) 0.0017(9) C12 0.0298(10) 0.0329(11) 0.0266(10) 0.0014(8) 0.0004(8) 0.0017(9) C13 0.0303(10) 0.0347(11) 0.0294(10) -0.0012(9) 0.0047(8) 0.0009(9) C14 0.0318(11) 0.0327(11) 0.0265(10) 0.0012(8) 0.0050(8) -0.0008(9) C15 0.0438(13) 0.0338(11) 0.0249(10) 0.0004(9) 0.0019(9) -0.0019(10) C16 0.0371(12) 0.0302(11) 0.0330(11) 0.0016(9) 0.0065(9) -0.0017(9) C17 0.0436(13) 0.0464(14) 0.0365(12) -0.0017(11) 0.0145(10) 0.0037(11) C18 0.0404(13) 0.0410(13) 0.0390(13) 0.0049(10) 0.0122(10) -0.0031(11) C19 0.076(2) 0.098(3) 0.0285(13) 0.0101(15) 0.0028(13) -0.029(2) C20 0.075(2) 0.073(2) 0.0449(16) -0.0178(15) 0.0219(15) -0.0161(18) S21 0.0312(3) 0.0526(4) 0.0261(3) 0.0078(2) 0.0040(2) 0.0131(3) S22 0.0305(3) 0.0459(3) 0.0284(3) 0.0074(2) 0.0053(2) 0.0111(2) S23 0.0311(3) 0.0534(4) 0.0248(3) 0.0066(2) 0.0059(2) 0.0143(3) S24 0.0308(3) 0.0426(3) 0.0300(3) 0.0052(2) 0.0050(2) 0.0104(2) S25 0.0391(3) 0.0837(5) 0.0396(3) 0.0208(3) 0.0160(3) 0.0270(3) S26 0.0328(3) 0.0589(4) 0.0392(3) 0.0245(3) 0.0069(2) 0.0066(3) S27 0.0606(4) 0.0567(4) 0.0300(3) 0.0133(3) 0.0143(3) 0.0229(3) S28 0.0323(3) 0.0435(3) 0.0433(3) 0.0021(3) 0.0151(2) 0.0065(2) C21 0.0281(10) 0.0359(11) 0.0237(9) 0.0018(8) 0.0028(8) 0.0028(9) C22 0.0266(10) 0.0355(11) 0.0247(10) 0.0006(8) 0.0020(8) 0.0039(9) C23 0.0296(10) 0.0403(12) 0.0272(10) 0.0055(9) 0.0050(8) 0.0035(9) C24 0.0284(10) 0.0344(11) 0.0262(10) 0.0063(8) 0.0060(8) 0.0017(9) C25 0.0363(11) 0.0337(11) 0.0253(10) 0.0025(8) 0.0089(8) 0.0069(9) C26 0.0296(10) 0.0317(11) 0.0295(10) -0.0005(8) 0.0077(8) 0.0020(9) C27A 0.045(4) 0.054(4) 0.031(2) 0.008(2) 0.011(2) 0.013(2) C28A 0.0331(18) 0.048(2) 0.0366(18) 0.0149(16) 0.0093(14) 0.0033(17) C27B 0.035(6) 0.067(9) 0.035(6) 0.023(6) 0.012(4) 0.000(5) C28B 0.054(5) 0.060(6) 0.026(4) -0.001(4) 0.004(3) -0.003(5) C29A 0.054(3) 0.053(3) 0.030(2) 0.004(3) 0.0135(19) 0.006(3) C30A 0.050(2) 0.045(2) 0.0321(18) -0.0099(17) 0.0149(17) 0.007(2) C29B 0.055(6) 0.045(6) 0.025(4) -0.006(5) 0.009(4) -0.005(6) C30B 0.049(5) 0.046(5) 0.035(4) -0.003(4) 0.016(4) -0.009(4) Fe1 0.0421(3) 0.0375(2) 0.0257(2) 0.000 0.00563(18) 0.000 O1 0.0625(12) 0.0437(10) 0.0345(9) 0.0032(7) -0.0012(8) 0.0041(9) O2 0.0457(10) 0.0503(10) 0.0311(8) -0.0071(7) 0.0111(7) -0.0060(8) O3 0.0464(10) 0.0513(10) 0.0300(8) 0.0046(7) 0.0117(7) -0.0015(8) O4 0.0710(14) 0.0456(11) 0.0726(15) 0.0154(10) 0.0075(11) 0.0062(10) O5 0.0509(11) 0.0661(13) 0.0458(11) -0.0063(9) 0.0017(9) -0.0144(10) O6 0.0574(12) 0.0731(14) 0.0495(11) -0.0002(10) 0.0247(10) 0.0084(11) C1 0.0484(15) 0.0421(14) 0.0434(14) 0.0055(11) 0.0168(11) 0.0016(12) C2 0.0380(12) 0.0411(13) 0.0338(12) 0.0026(10) 0.0016(10) 0.0048(11) C3 0.0387(13) 0.0457(14) 0.0335(12) -0.0074(10) 0.0072(10) -0.0078(11) Cl31 0.125(8) 0.0683(8) 0.065(5) -0.010(3) 0.041(5) -0.022(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.738(2) . ? S11 C13 1.750(2) . ? S12 C11 1.734(2) . ? S12 C14 1.749(2) . ? S13 C12 1.733(2) . ? S13 C15 1.749(2) . ? S14 C12 1.739(2) . ? S14 C16 1.741(2) . ? S15 C13 1.745(2) . ? S15 C17 1.809(3) . ? S16 C14 1.740(2) . ? S16 C18 1.799(2) . ? S17 C15 1.739(2) . ? S17 C19 1.807(3) . ? S18 C16 1.745(2) . ? S18 C20 1.784(3) . ? C11 C12 1.363(3) . ? C13 C14 1.349(3) . ? C15 C16 1.340(3) . ? C17 C18 1.511(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.506(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? S21 C21 1.738(2) . ? S21 C23 1.741(2) . ? S22 C21 1.733(2) . ? S22 C24 1.751(2) . ? S23 C22 1.735(2) . ? S23 C25 1.749(2) . ? S24 C22 1.739(2) . ? S24 C26 1.741(2) . ? S25 C27B 1.700(13) . ? S25 C23 1.739(2) . ? S25 C27A 1.828(6) . ? S26 C24 1.743(2) . ? S26 C28A 1.772(3) . ? S26 C28B 1.866(9) . ? S27 C25 1.737(2) . ? S27 C29A 1.774(6) . ? S27 C29B 1.860(12) . ? S28 C30B 1.736(9) . ? S28 C26 1.740(2) . ? S28 C30A 1.843(4) . ? C21 C22 1.364(3) . ? C23 C24 1.349(3) . ? C25 C26 1.349(3) . ? C27A C28A 1.500(7) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C27B C28B 1.530(14) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29A C30A 1.503(7) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C29B C30B 1.509(16) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? Fe1 O2 2.0064(17) . ? Fe1 O2 2.0064(17) 2_656 ? Fe1 O1 2.0110(18) . ? Fe1 O1 2.0110(18) 2_656 ? Fe1 O3 2.0109(17) . ? Fe1 O3 2.0109(17) 2_656 ? O1 C1 1.275(3) . ? O2 C2 1.276(3) . ? O3 C3 1.275(3) . ? O4 C1 1.225(3) . ? O5 C2 1.217(3) . ? O6 C3 1.220(3) . ? C1 C1 1.553(6) 2_656 ? C2 C3 1.560(3) 2_656 ? C3 C2 1.560(3) 2_656 ? Cl31 C34 1.741(5) . ? C31 C36 1.385(11) . ? C31 C32 1.402(10) . ? C31 H31 0.9300 . ? C32 C33 1.392(12) . ? C32 H32 0.9300 . ? C33 C34 1.292(11) . ? C33 H33 0.9300 . ? C34 C35 1.466(12) . ? C35 C36 1.350(12) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O41 H41A 1.17(4) . ? O41 H41B 1.18(4) . ? O41 H41C 1.17(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 S11 C13 95.29(10) . . ? C11 S12 C14 95.65(10) . . ? C12 S13 C15 95.31(11) . . ? C12 S14 C16 95.46(11) . . ? C13 S15 C17 101.61(11) . . ? C14 S16 C18 101.45(11) . . ? C15 S17 C19 102.34(14) . . ? C16 S18 C20 98.95(14) . . ? C12 C11 S12 121.62(17) . . ? C12 C11 S11 123.12(17) . . ? S12 C11 S11 115.25(12) . . ? C11 C12 S13 122.68(17) . . ? C11 C12 S14 122.28(17) . . ? S13 C12 S14 115.03(12) . . ? C14 C13 S15 129.14(17) . . ? C14 C13 S11 117.18(16) . . ? S15 C13 S11 113.69(12) . . ? C13 C14 S16 128.01(17) . . ? C13 C14 S12 116.62(16) . . ? S16 C14 S12 115.35(12) . . ? C16 C15 S17 128.88(19) . . ? C16 C15 S13 117.06(17) . . ? S17 C15 S13 114.00(14) . . ? C15 C16 S14 117.10(17) . . ? C15 C16 S18 127.75(18) . . ? S14 C16 S18 115.10(13) . . ? C18 C17 S15 114.06(17) . . ? C18 C17 H17A 108.7 . . ? S15 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? S15 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C17 C18 S16 114.49(17) . . ? C17 C18 H18A 108.6 . . ? S16 C18 H18A 108.6 . . ? C17 C18 H18B 108.6 . . ? S16 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C20 C19 S17 114.4(2) . . ? C20 C19 H19A 108.7 . . ? S17 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? S17 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 S18 112.9(2) . . ? C19 C20 H20A 109.0 . . ? S18 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? S18 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C21 S21 C23 95.18(10) . . ? C21 S22 C24 95.45(10) . . ? C22 S23 C25 95.27(10) . . ? C22 S24 C26 95.09(10) . . ? C27B S25 C23 105.7(5) . . ? C23 S25 C27A 100.3(2) . . ? C24 S26 C28A 103.13(14) . . ? C24 S26 C28B 96.7(3) . . ? C25 S27 C29A 106.0(2) . . ? C25 S27 C29B 94.8(4) . . ? C30B S28 C26 108.4(3) . . ? C26 S28 C30A 95.98(15) . . ? C22 C21 S22 122.40(17) . . ? C22 C21 S21 122.25(17) . . ? S22 C21 S21 115.34(12) . . ? C21 C22 S23 121.75(17) . . ? C21 C22 S24 122.94(17) . . ? S23 C22 S24 115.28(12) . . ? C24 C23 S25 128.36(17) . . ? C24 C23 S21 117.55(16) . . ? S25 C23 S21 114.08(12) . . ? C23 C24 S26 127.84(17) . . ? C23 C24 S22 116.41(16) . . ? S26 C24 S22 115.73(12) . . ? C26 C25 S27 127.05(17) . . ? C26 C25 S23 116.65(16) . . ? S27 C25 S23 116.22(13) . . ? C25 C26 S28 125.99(17) . . ? C25 C26 S24 117.38(16) . . ? S28 C26 S24 116.52(12) . . ? C28A C27A S25 113.7(4) . . ? C28A C27A H27A 108.8 . . ? S25 C27A H27A 108.8 . . ? C28A C27A H27B 108.8 . . ? S25 C27A H27B 108.8 . . ? H27A C27A H27B 107.7 . . ? C27A C28A S26 113.3(3) . . ? C27A C28A H28A 108.9 . . ? S26 C28A H28A 108.9 . . ? C27A C28A H28B 108.9 . . ? S26 C28A H28B 108.9 . . ? H28A C28A H28B 107.7 . . ? C28B C27B S25 111.9(8) . . ? C28B C27B H27C 109.2 . . ? S25 C27B H27C 109.2 . . ? C28B C27B H27D 109.2 . . ? S25 C27B H27D 109.2 . . ? H27C C27B H27D 107.9 . . ? C27B C28B S26 114.0(8) . . ? C27B C28B H28C 108.8 . . ? S26 C28B H28C 108.8 . . ? C27B C28B H28D 108.8 . . ? S26 C28B H28D 108.8 . . ? H28C C28B H28D 107.7 . . ? C30A C29A S27 116.3(3) . . ? C30A C29A H29A 108.2 . . ? S27 C29A H29A 108.2 . . ? C30A C29A H29B 108.2 . . ? S27 C29A H29B 108.2 . . ? H29A C29A H29B 107.4 . . ? C29A C30A S28 113.4(3) . . ? C29A C30A H30A 108.9 . . ? S28 C30A H30A 108.9 . . ? C29A C30A H30B 108.9 . . ? S28 C30A H30B 108.9 . . ? H30A C30A H30B 107.7 . . ? C30B C29B S27 114.3(7) . . ? C30B C29B H29C 108.7 . . ? S27 C29B H29C 108.7 . . ? C30B C29B H29D 108.7 . . ? S27 C29B H29D 108.7 . . ? H29C C29B H29D 107.6 . . ? C29B C30B S28 112.6(7) . . ? C29B C30B H30C 109.1 . . ? S28 C30B H30C 109.1 . . ? C29B C30B H30D 109.1 . . ? S28 C30B H30D 109.1 . . ? H30C C30B H30D 107.8 . . ? O2 Fe1 O2 99.50(11) . 2_656 ? O2 Fe1 O1 90.63(8) . . ? O2 Fe1 O1 168.55(8) 2_656 . ? O2 Fe1 O1 168.55(8) . 2_656 ? O2 Fe1 O1 90.63(8) 2_656 2_656 ? O1 Fe1 O1 79.83(11) . 2_656 ? O2 Fe1 O3 87.85(7) . . ? O2 Fe1 O3 80.50(7) 2_656 . ? O1 Fe1 O3 94.68(7) . . ? O1 Fe1 O3 99.15(8) 2_656 . ? O2 Fe1 O3 80.50(7) . 2_656 ? O2 Fe1 O3 87.85(7) 2_656 2_656 ? O1 Fe1 O3 99.15(8) . 2_656 ? O1 Fe1 O3 94.68(7) 2_656 2_656 ? O3 Fe1 O3 161.95(11) . 2_656 ? C1 O1 Fe1 116.28(17) . . ? C2 O2 Fe1 115.91(15) . . ? C3 O3 Fe1 115.32(15) . . ? O4 C1 O1 126.3(3) . . ? O4 C1 C1 120.01(17) . 2_656 ? O1 C1 C1 113.69(15) . 2_656 ? O5 C2 O2 126.0(2) . . ? O5 C2 C3 120.3(2) . 2_656 ? O2 C2 C3 113.7(2) . 2_656 ? O6 C3 O3 126.5(2) . . ? O6 C3 C2 119.4(2) . 2_656 ? O3 C3 C2 114.2(2) . 2_656 ? C36 C31 C32 120.2(6) . . ? C36 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 120.1(8) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 119.4(8) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 122.2(6) . . ? C33 C34 Cl31 118.5(9) . . ? C35 C34 Cl31 119.3(9) . . ? C36 C35 C34 118.3(8) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C35 C36 C31 119.7(8) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? H41A O41 H41B 108(2) . . ? H41A O41 H41C 109(2) . . ? H41B O41 H41C 107(2) . . ? # Attachment '- IV.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3]FB-(IV) _database_code_depnum_ccdc_archive 'CCDC 771732' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, C6 H5 F, H3 O' _chemical_formula_sum 'C52 H40 F Fe O13 S32' _chemical_formula_weight 1973.61 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 10.3011(5) _cell_length_b 20.0280(10) _cell_length_c 35.249(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.567(5) _cell_angle_gamma 90.00 _cell_volume 7264.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_radiation CuK\a _cell_measurement_reflns_used 10766 _cell_measurement_theta_min 3.7626 _cell_measurement_theta_max 62.0769 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4012 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52073 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _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 54624 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 31.41 _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.908 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.082 _reflns_number_total 11027 _reflns_number_gt 6591 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0414P)^2^+8.1849P] 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 11027 _refine_ls_number_parameters 480 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.010 _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 S11 S 0.42270(6) 0.21456(3) 0.508843(17) 0.04208(15) Uani 1 1 d . . . S12 S 0.66281(6) 0.14325(3) 0.531365(17) 0.03976(14) Uani 1 1 d . . . S13 S 0.54155(6) 0.24636(3) 0.427063(18) 0.04270(15) Uani 1 1 d . . . S14 S 0.77909(6) 0.17417(3) 0.450488(18) 0.04127(15) Uani 1 1 d . . . S15 S 0.29519(6) 0.19383(4) 0.58041(2) 0.04906(17) Uani 1 1 d . . . S16 S 0.58494(6) 0.11059(4) 0.608635(18) 0.04610(16) Uani 1 1 d . . . S17 S 0.61920(9) 0.27577(4) 0.35006(2) 0.0619(2) Uani 1 1 d . . . S18 S 0.90769(7) 0.19400(4) 0.37837(2) 0.05489(19) Uani 1 1 d . . . C11 C 0.5760(2) 0.18819(11) 0.49666(6) 0.0345(5) Uani 1 1 d . . . C12 C 0.6262(2) 0.20145(11) 0.46234(6) 0.0349(5) Uani 1 1 d . . . C13 C 0.4332(2) 0.18063(12) 0.55464(6) 0.0357(5) Uani 1 1 d . . . C14 C 0.5440(2) 0.14768(11) 0.56507(6) 0.0340(5) Uani 1 1 d . . . C15 C 0.6620(2) 0.24084(12) 0.39414(7) 0.0388(5) Uani 1 1 d . . . C16 C 0.7718(2) 0.20862(12) 0.40493(7) 0.0381(5) Uani 1 1 d . . . C17 C 0.3530(3) 0.17039(13) 0.62782(7) 0.0466(6) Uani 1 1 d . . . H17A H 0.4075 0.2060 0.6383 0.056 Uiso 1 1 calc R . . H17B H 0.2790 0.1659 0.6437 0.056 Uiso 1 1 calc R . . C18 C 0.4297(3) 0.10568(13) 0.62934(7) 0.0440(6) Uani 1 1 d . . . H18A H 0.3788 0.0713 0.6163 0.053 Uiso 1 1 calc R . . H18B H 0.4425 0.0922 0.6557 0.053 Uiso 1 1 calc R . . C19 C 0.7628(4) 0.2621(2) 0.32385(9) 0.0766(10) Uani 1 1 d . . . H19A H 0.7391 0.2642 0.2969 0.092 Uiso 1 1 calc R . . H19B H 0.8236 0.2981 0.3295 0.092 Uiso 1 1 calc R . . C20 C 0.8306(4) 0.19669(18) 0.33195(9) 0.0721(10) Uani 1 1 d . . . H20A H 0.8954 0.1895 0.3132 0.086 Uiso 1 1 calc R . . H20B H 0.7677 0.1607 0.3295 0.086 Uiso 1 1 calc R . . S21 S 0.02591(6) 0.08871(3) 0.518973(17) 0.04164(15) Uani 1 1 d . . . S22 S 0.25893(6) 0.01269(3) 0.543415(17) 0.03999(14) Uani 1 1 d . . . S23 S 0.14948(6) 0.11803(3) 0.438615(17) 0.04168(15) Uani 1 1 d . . . S24 S 0.38462(6) 0.04366(3) 0.462818(17) 0.03985(14) Uani 1 1 d . . . S25 S -0.10901(7) 0.07009(4) 0.58941(2) 0.0569(2) Uani 1 1 d . . . S26 S 0.17004(6) -0.01745(4) 0.620112(19) 0.04969(18) Uani 1 1 d . . . S27 S 0.24676(8) 0.15653(4) 0.363806(19) 0.05428(19) Uani 1 1 d . . . S28 S 0.52283(6) 0.07238(3) 0.39302(2) 0.04640(16) Uani 1 1 d . . . C21 C 0.1791(2) 0.06023(12) 0.50812(6) 0.0347(5) Uani 1 1 d . . . C22 C 0.2326(2) 0.07329(11) 0.47419(6) 0.0342(5) Uani 1 1 d . . . C23 C 0.0296(2) 0.05422(12) 0.56440(6) 0.0367(5) Uani 1 1 d . A . C24 C 0.1367(2) 0.01942(11) 0.57580(6) 0.0337(5) Uani 1 1 d . A . C25 C 0.2766(2) 0.11740(11) 0.40744(6) 0.0360(5) Uani 1 1 d . B . C26 C 0.3848(2) 0.08370(11) 0.41878(7) 0.0351(5) Uani 1 1 d . B . C27A C -0.0452(8) 0.0543(3) 0.6381(2) 0.0528(16) Uani 0.65 1 d P A 1 H27A H 0.0164 0.0892 0.6453 0.063 Uiso 0.65 1 calc PR A 1 H27B H -0.1162 0.0566 0.6552 0.063 Uiso 0.65 1 calc PR A 1 C28A C 0.0211(4) -0.0127(2) 0.64287(12) 0.0450(9) Uani 0.65 1 d P A 1 H28A H -0.0367 -0.0471 0.6327 0.054 Uiso 0.65 1 calc PR A 1 H28B H 0.0367 -0.0215 0.6698 0.054 Uiso 0.65 1 calc PR A 1 C27B C -0.0830(12) 0.0286(6) 0.6320(4) 0.044(3) Uani 0.35 1 d P A 2 H27C H -0.1402 0.0468 0.6505 0.053 Uiso 0.35 1 calc PR A 2 H27D H -0.1046 -0.0182 0.6284 0.053 Uiso 0.35 1 calc PR A 2 C28B C 0.0560(8) 0.0343(5) 0.6471(2) 0.0467(18) Uani 0.35 1 d P A 2 H28C H 0.0609 0.0207 0.6735 0.056 Uiso 0.35 1 calc PR A 2 H28D H 0.0827 0.0807 0.6460 0.056 Uiso 0.35 1 calc PR A 2 C29A C 0.3658(8) 0.1242(3) 0.3339(2) 0.0509(16) Uani 0.61 1 d P B 1 H29A H 0.3241 0.1155 0.3092 0.061 Uiso 0.61 1 calc PR B 1 H29B H 0.4304 0.1587 0.3306 0.061 Uiso 0.61 1 calc PR B 1 C30A C 0.4356(6) 0.0617(3) 0.34680(14) 0.0524(12) Uani 0.61 1 d P B 1 H30A H 0.4970 0.0491 0.3280 0.063 Uiso 0.61 1 calc PR B 1 H30B H 0.3731 0.0257 0.3486 0.063 Uiso 0.61 1 calc PR B 1 C29B C 0.3396(14) 0.0968(6) 0.3352(4) 0.055(3) Uani 0.39 1 d P B 2 H29C H 0.3072 0.0520 0.3391 0.067 Uiso 0.39 1 calc PR B 2 H29D H 0.3265 0.1076 0.3085 0.067 Uiso 0.39 1 calc PR B 2 C30B C 0.4823(8) 0.0991(5) 0.3460(2) 0.0513(19) Uani 0.39 1 d P B 2 H30C H 0.5129 0.1445 0.3430 0.062 Uiso 0.39 1 calc PR B 2 H30D H 0.5281 0.0711 0.3285 0.062 Uiso 0.39 1 calc PR B 2 Fe1 Fe 0.5000 0.08261(2) 0.7500 0.03953(13) Uani 1 2 d S . . O1 O 0.42895(19) 0.15973(9) 0.71877(5) 0.0522(5) Uani 1 1 d . . . O2 O 0.40020(17) 0.01713(9) 0.71692(5) 0.0470(4) Uani 1 1 d . . . O3 O 0.65315(18) 0.06759(9) 0.71781(5) 0.0469(4) Uani 1 1 d . . . O4 O 0.4145(2) 0.27113(10) 0.71845(7) 0.0696(6) Uani 1 1 d . . . O5 O 0.2259(2) -0.04883(11) 0.71538(6) 0.0641(6) Uani 1 1 d . . . O6 O 0.8260(2) 0.00107(11) 0.71351(6) 0.0667(6) Uani 1 1 d . . . C1 C 0.4546(3) 0.21819(14) 0.73200(8) 0.0494(6) Uani 1 1 d . . . C2 C 0.2977(3) -0.00648(13) 0.73045(7) 0.0424(6) Uani 1 1 d . . . C3 C 0.7333(3) 0.02236(13) 0.72981(7) 0.0452(6) Uani 1 1 d . . . F31 F 0.0239(11) 0.3365(3) 0.7513(4) 0.179(3) Uiso 0.50 1 d PD . . C31 C 0.0108(9) 0.13271(14) 0.7444(3) 0.097(2) Uiso 0.50 1 d PG . . H31 H 0.0081 0.0863 0.7433 0.116 Uiso 0.50 1 calc PR . . C32 C 0.1077(7) 0.1672(3) 0.7264(2) 0.100(3) Uiso 0.50 1 d PG . . H32 H 0.1697 0.1439 0.7133 0.120 Uiso 0.50 1 calc PR . . C33 C 0.1118(6) 0.2365(3) 0.7279(2) 0.080(2) Uiso 0.50 1 d PGD . . H33 H 0.1766 0.2596 0.7159 0.096 Uiso 0.50 1 calc PR . . C34 C 0.0190(8) 0.27135(14) 0.7474(3) 0.0795(19) Uiso 0.50 1 d PG . . C35 C -0.0779(6) 0.2369(2) 0.7654(2) 0.078(2) Uiso 0.50 1 d PGD . . H35 H -0.1399 0.2601 0.7785 0.093 Uiso 0.50 1 calc PR . . C36 C -0.0820(7) 0.1675(2) 0.7639(2) 0.084(2) Uiso 0.50 1 d PG . . H36 H -0.1468 0.1444 0.7759 0.101 Uiso 0.50 1 calc PR . . O41 O 0.0102(7) -0.09761(16) 0.75525(18) 0.0612(11) Uiso 0.50 1 d PD . . H41A H 0.022(5) -0.1548(18) 0.7639(17) 0.092 Uiso 0.50 1 d PD . . H41B H 0.100(4) -0.063(2) 0.766(2) 0.092 Uiso 0.50 1 d PD . . H41C H -0.092(4) -0.074(2) 0.764(2) 0.092 Uiso 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 S11 0.0369(3) 0.0540(4) 0.0356(3) 0.0039(3) 0.0041(2) 0.0104(3) S12 0.0343(3) 0.0513(4) 0.0342(3) 0.0082(3) 0.0070(2) 0.0077(3) S13 0.0399(3) 0.0532(4) 0.0352(3) 0.0064(3) 0.0025(3) 0.0098(3) S14 0.0362(3) 0.0484(4) 0.0396(3) 0.0065(3) 0.0054(3) 0.0065(3) S15 0.0377(3) 0.0635(4) 0.0469(4) 0.0039(3) 0.0128(3) 0.0114(3) S16 0.0425(4) 0.0579(4) 0.0385(3) 0.0140(3) 0.0090(3) 0.0074(3) S17 0.0836(6) 0.0693(5) 0.0326(3) 0.0104(3) -0.0003(4) 0.0074(4) S18 0.0552(4) 0.0510(4) 0.0609(4) 0.0024(3) 0.0285(4) 0.0018(3) C11 0.0319(12) 0.0408(13) 0.0309(11) 0.0014(10) 0.0026(9) 0.0023(10) C12 0.0338(12) 0.0400(13) 0.0309(11) 0.0004(10) 0.0016(9) 0.0023(10) C13 0.0364(13) 0.0402(12) 0.0310(11) -0.0009(10) 0.0063(9) -0.0002(10) C14 0.0351(12) 0.0365(12) 0.0308(11) 0.0007(10) 0.0059(9) -0.0013(10) C15 0.0490(15) 0.0381(13) 0.0295(11) 0.0011(10) 0.0052(10) -0.0013(11) C16 0.0431(14) 0.0355(12) 0.0365(12) 0.0012(10) 0.0108(10) -0.0012(10) C17 0.0486(15) 0.0498(15) 0.0427(14) -0.0010(12) 0.0158(12) 0.0032(12) C18 0.0487(15) 0.0444(14) 0.0400(13) 0.0037(11) 0.0149(11) -0.0038(11) C19 0.084(2) 0.110(3) 0.0356(15) 0.0096(18) 0.0089(16) -0.026(2) C20 0.085(2) 0.081(2) 0.0524(18) -0.0224(17) 0.0261(17) -0.0153(19) S21 0.0367(3) 0.0574(4) 0.0311(3) 0.0072(3) 0.0050(2) 0.0138(3) S22 0.0353(3) 0.0508(4) 0.0343(3) 0.0078(3) 0.0063(2) 0.0114(3) S23 0.0369(3) 0.0579(4) 0.0308(3) 0.0063(3) 0.0072(2) 0.0144(3) S24 0.0351(3) 0.0473(4) 0.0376(3) 0.0050(3) 0.0060(2) 0.0105(3) S25 0.0422(4) 0.0850(5) 0.0449(4) 0.0176(4) 0.0163(3) 0.0242(4) S26 0.0389(3) 0.0653(4) 0.0455(4) 0.0255(3) 0.0087(3) 0.0073(3) S27 0.0655(5) 0.0627(4) 0.0359(3) 0.0133(3) 0.0158(3) 0.0217(4) S28 0.0388(3) 0.0495(4) 0.0524(4) 0.0029(3) 0.0186(3) 0.0070(3) C21 0.0323(12) 0.0425(13) 0.0294(11) 0.0008(10) 0.0019(9) 0.0055(10) C22 0.0341(12) 0.0397(12) 0.0288(11) 0.0000(9) 0.0024(9) 0.0061(10) C23 0.0328(12) 0.0453(13) 0.0327(11) 0.0059(10) 0.0076(9) 0.0038(10) C24 0.0317(12) 0.0378(12) 0.0321(11) 0.0068(10) 0.0058(9) 0.0017(9) C25 0.0391(13) 0.0372(12) 0.0325(11) 0.0019(10) 0.0093(10) 0.0057(10) C26 0.0366(12) 0.0351(12) 0.0342(11) 0.0002(10) 0.0098(10) 0.0010(10) C27A 0.064(5) 0.061(5) 0.034(3) 0.005(3) 0.011(3) 0.018(3) C28A 0.041(2) 0.056(3) 0.039(2) 0.014(2) 0.0130(17) 0.006(2) C27B 0.043(6) 0.055(8) 0.035(5) 0.013(5) 0.011(4) 0.006(5) C28B 0.052(5) 0.055(5) 0.033(4) 0.004(4) 0.002(3) 0.002(4) C29A 0.053(4) 0.061(5) 0.039(3) -0.003(4) 0.011(3) 0.003(3) C30A 0.066(4) 0.051(3) 0.041(2) -0.010(2) 0.015(2) 0.011(3) C29B 0.072(7) 0.055(8) 0.040(5) -0.020(6) 0.017(4) -0.017(6) C30B 0.058(5) 0.051(5) 0.047(4) -0.005(4) 0.023(4) 0.000(4) Fe1 0.0476(3) 0.0415(3) 0.0300(2) 0.000 0.0078(2) 0.000 O1 0.0703(13) 0.0471(11) 0.0387(10) 0.0037(8) -0.0014(9) 0.0056(9) O2 0.0516(11) 0.0549(11) 0.0356(9) -0.0088(8) 0.0127(8) -0.0084(9) O3 0.0529(11) 0.0532(11) 0.0355(9) 0.0054(8) 0.0130(8) -0.0017(9) O4 0.0829(16) 0.0480(12) 0.0785(15) 0.0158(11) 0.0092(13) 0.0082(11) O5 0.0604(13) 0.0771(14) 0.0554(12) -0.0106(11) 0.0090(10) -0.0201(11) O6 0.0626(13) 0.0833(15) 0.0567(12) 0.0029(11) 0.0295(11) 0.0115(11) C1 0.0549(17) 0.0478(15) 0.0471(15) 0.0068(13) 0.0198(12) 0.0024(13) C2 0.0444(14) 0.0465(14) 0.0365(13) 0.0022(11) 0.0063(11) 0.0009(12) C3 0.0452(15) 0.0519(15) 0.0394(13) -0.0076(12) 0.0118(11) -0.0084(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.738(2) . ? S11 C13 1.750(2) . ? S12 C11 1.734(2) . ? S12 C14 1.745(2) . ? S13 C12 1.738(2) . ? S13 C15 1.740(3) . ? S14 C12 1.736(2) . ? S14 C16 1.746(2) . ? S15 C13 1.741(2) . ? S15 C17 1.811(3) . ? S16 C14 1.741(2) . ? S16 C18 1.790(2) . ? S17 C15 1.743(2) . ? S17 C19 1.800(4) . ? S18 C16 1.743(2) . ? S18 C20 1.787(4) . ? C11 C12 1.363(3) . ? C13 C14 1.355(3) . ? C15 C16 1.343(3) . ? C17 C18 1.518(3) . ? C19 C20 1.506(5) . ? S21 C21 1.737(2) . ? S21 C23 1.743(2) . ? S22 C24 1.742(2) . ? S22 C21 1.743(2) . ? S23 C22 1.735(2) . ? S23 C25 1.747(2) . ? S24 C22 1.739(2) . ? S24 C26 1.747(2) . ? S25 C27B 1.726(13) . ? S25 C23 1.741(2) . ? S25 C27A 1.838(7) . ? S26 C24 1.748(2) . ? S26 C28A 1.766(4) . ? S26 C28B 1.861(8) . ? S27 C25 1.741(2) . ? S27 C29A 1.774(8) . ? S27 C29B 1.856(14) . ? S28 C26 1.736(2) . ? S28 C30B 1.773(8) . ? S28 C30A 1.837(5) . ? C21 C22 1.364(3) . ? C23 C24 1.351(3) . ? C25 C26 1.348(3) . ? C27A C28A 1.510(9) . ? C27B C28B 1.510(14) . ? C29A C30A 1.504(10) . ? C29B C30B 1.503(17) . ? Fe1 O3 2.0066(17) 2_656 ? Fe1 O3 2.0066(17) . ? Fe1 O2 2.0072(17) . ? Fe1 O2 2.0072(17) 2_656 ? Fe1 O1 2.0153(18) 2_656 ? Fe1 O1 2.0153(18) . ? O1 C1 1.283(3) . ? O2 C2 1.269(3) . ? O3 C3 1.285(3) . ? O4 C1 1.227(3) . ? O5 C2 1.230(3) . ? O6 C3 1.213(3) . ? C1 C1 1.542(6) 2_656 ? C2 C3 1.562(3) 2_656 ? C3 C2 1.562(3) 2_656 ? F31 C34 1.313(6) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 S11 C13 95.19(11) . . ? C11 S12 C14 95.68(11) . . ? C12 S13 C15 95.43(11) . . ? C12 S14 C16 95.46(11) . . ? C13 S15 C17 101.53(12) . . ? C14 S16 C18 101.42(12) . . ? C15 S17 C19 102.46(15) . . ? C16 S18 C20 98.75(14) . . ? C12 C11 S12 121.56(18) . . ? C12 C11 S11 123.04(18) . . ? S12 C11 S11 115.41(13) . . ? C11 C12 S14 122.46(18) . . ? C11 C12 S13 122.56(18) . . ? S14 C12 S13 114.98(13) . . ? C14 C13 S15 129.05(18) . . ? C14 C13 S11 117.11(17) . . ? S15 C13 S11 113.84(13) . . ? C13 C14 S16 127.94(18) . . ? C13 C14 S12 116.60(17) . . ? S16 C14 S12 115.44(13) . . ? C16 C15 S13 117.29(18) . . ? C16 C15 S17 128.4(2) . . ? S13 C15 S17 114.20(14) . . ? C15 C16 S18 127.96(19) . . ? C15 C16 S14 116.82(18) . . ? S18 C16 S14 115.17(14) . . ? C18 C17 S15 113.77(18) . . ? C17 C18 S16 114.33(18) . . ? C20 C19 S17 114.8(2) . . ? C19 C20 S18 112.5(2) . . ? C21 S21 C23 95.13(11) . . ? C24 S22 C21 95.39(11) . . ? C22 S23 C25 95.26(11) . . ? C22 S24 C26 94.87(11) . . ? C27B S25 C23 104.7(5) . . ? C23 S25 C27A 100.0(3) . . ? C24 S26 C28A 104.08(15) . . ? C24 S26 C28B 96.8(3) . . ? C25 S27 C29A 105.1(3) . . ? C25 S27 C29B 96.6(5) . . ? C26 S28 C30B 106.6(3) . . ? C26 S28 C30A 95.7(2) . . ? C22 C21 S21 122.44(18) . . ? C22 C21 S22 122.32(18) . . ? S21 C21 S22 115.24(13) . . ? C21 C22 S23 121.82(18) . . ? C21 C22 S24 122.67(18) . . ? S23 C22 S24 115.46(13) . . ? C24 C23 S25 128.40(18) . . ? C24 C23 S21 117.50(17) . . ? S25 C23 S21 114.10(13) . . ? C23 C24 S22 116.72(17) . . ? C23 C24 S26 127.51(18) . . ? S22 C24 S26 115.73(13) . . ? C26 C25 S27 126.74(18) . . ? C26 C25 S23 116.73(18) . . ? S27 C25 S23 116.43(13) . . ? C25 C26 S28 126.57(18) . . ? C25 C26 S24 117.38(17) . . ? S28 C26 S24 115.98(13) . . ? C28A C27A S25 113.4(4) . . ? C27A C28A S26 113.3(4) . . ? C28B C27B S25 112.2(8) . . ? C27B C28B S26 112.7(7) . . ? C30A C29A S27 117.3(5) . . ? C29A C30A S28 112.3(4) . . ? C30B C29B S27 111.4(7) . . ? C29B C30B S28 114.5(7) . . ? O3 Fe1 O3 162.76(11) 2_656 . ? O3 Fe1 O2 80.52(7) 2_656 . ? O3 Fe1 O2 88.22(7) . . ? O3 Fe1 O2 88.22(7) 2_656 2_656 ? O3 Fe1 O2 80.52(7) . 2_656 ? O2 Fe1 O2 98.41(11) . 2_656 ? O3 Fe1 O1 94.67(8) 2_656 2_656 ? O3 Fe1 O1 98.53(8) . 2_656 ? O2 Fe1 O1 169.15(8) . 2_656 ? O2 Fe1 O1 91.11(8) 2_656 2_656 ? O3 Fe1 O1 98.53(8) 2_656 . ? O3 Fe1 O1 94.67(8) . . ? O2 Fe1 O1 91.11(8) . . ? O2 Fe1 O1 169.15(8) 2_656 . ? O1 Fe1 O1 79.92(11) 2_656 . ? C1 O1 Fe1 115.90(17) . . ? C2 O2 Fe1 116.00(15) . . ? C3 O3 Fe1 115.45(15) . . ? O4 C1 O1 125.9(3) . . ? O4 C1 C1 120.11(18) . 2_656 ? O1 C1 C1 113.98(15) . 2_656 ? O5 C2 O2 126.1(2) . . ? O5 C2 C3 120.0(2) . 2_656 ? O2 C2 C3 114.0(2) . 2_656 ? O6 C3 O3 126.9(3) . . ? O6 C3 C2 119.4(3) . 2_656 ? O3 C3 C2 113.7(2) . 2_656 ? C32 C31 C36 120.0 . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? F31 C34 C33 121.7(6) . . ? F31 C34 C35 118.2(6) . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? # Attachment '- IX.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.40(FB)0.60-(IX) _database_code_depnum_ccdc_archive 'CCDC 771733' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, 0.40(C7 H5 N), 0.60(C6 H5 F), H3 O' _chemical_formula_sum 'C52.40 H40 F0.60 Fe N0.40 O13 S32' _chemical_formula_weight 1976.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 10.2794(6) _cell_length_b 20.0190(10) _cell_length_c 35.255(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.496(5) _cell_angle_gamma 90.00 _cell_volume 7248.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11972 _cell_measurement_theta_min 3.7618 _cell_measurement_theta_max 70.9236 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4018 _exptl_absorpt_coefficient_mu 1.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80539 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40145 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 29.68 _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.789 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.071 _reflns_number_total 9209 _reflns_number_gt 7130 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0514P)^2^+14.7849P] 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 9209 _refine_ls_number_parameters 483 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S11 S 0.42261(6) 0.21453(4) 0.508719(19) 0.04152(16) Uani 1 1 d . . . S12 S 0.66304(6) 0.14339(3) 0.531303(18) 0.03892(15) Uani 1 1 d . . . S13 S 0.54173(6) 0.24610(4) 0.426906(19) 0.04181(16) Uani 1 1 d . . . S14 S 0.77974(6) 0.17404(3) 0.450442(19) 0.04028(15) Uani 1 1 d . . . S15 S 0.29462(7) 0.19374(4) 0.58021(2) 0.04827(18) Uani 1 1 d . . . S16 S 0.58485(7) 0.11081(4) 0.60852(2) 0.04500(17) Uani 1 1 d . . . S17 S 0.62006(9) 0.27516(5) 0.34990(2) 0.0595(2) Uani 1 1 d . . . S18 S 0.90864(8) 0.19353(4) 0.37846(2) 0.0529(2) Uani 1 1 d . . . C11 C 0.5762(2) 0.18814(12) 0.49648(7) 0.0338(5) Uani 1 1 d . . . C12 C 0.6261(2) 0.20136(12) 0.46221(7) 0.0338(5) Uani 1 1 d . . . C13 C 0.4328(2) 0.18049(13) 0.55438(7) 0.0353(5) Uani 1 1 d . . . C14 C 0.5440(2) 0.14806(12) 0.56491(7) 0.0340(5) Uani 1 1 d . . . C15 C 0.6628(3) 0.24038(13) 0.39402(7) 0.0375(5) Uani 1 1 d . . . C16 C 0.7728(3) 0.20830(12) 0.40500(7) 0.0369(5) Uani 1 1 d . . . C17 C 0.3518(3) 0.17009(15) 0.62754(8) 0.0462(7) Uani 1 1 d . . . H17A H 0.4057 0.2058 0.6382 0.055 Uiso 1 1 calc R . . H17B H 0.2774 0.1653 0.6433 0.055 Uiso 1 1 calc R . . C18 C 0.4292(3) 0.10602(14) 0.62925(8) 0.0437(6) Uani 1 1 d . . . H18A H 0.3785 0.0713 0.6164 0.052 Uiso 1 1 calc R . . H18B H 0.4420 0.0928 0.6556 0.052 Uiso 1 1 calc R . . C19 C 0.7645(4) 0.2616(2) 0.32371(9) 0.0716(11) Uani 1 1 d . . . H19A H 0.7411 0.2637 0.2968 0.086 Uiso 1 1 calc R . . H19B H 0.8254 0.2976 0.3294 0.086 Uiso 1 1 calc R . . C20 C 0.8321(4) 0.19623(19) 0.33195(10) 0.0693(10) Uani 1 1 d . . . H20A H 0.8973 0.1890 0.3133 0.083 Uiso 1 1 calc R . . H20B H 0.7690 0.1603 0.3294 0.083 Uiso 1 1 calc R . . S21 S 0.02568(6) 0.08871(4) 0.518964(18) 0.04101(16) Uani 1 1 d . . . S22 S 0.25866(6) 0.01271(3) 0.543447(18) 0.03921(15) Uani 1 1 d . . . S23 S 0.14981(6) 0.11803(4) 0.438795(18) 0.04072(16) Uani 1 1 d . . . S24 S 0.38500(6) 0.04363(3) 0.462894(18) 0.03898(15) Uani 1 1 d . . . S25 S -0.10973(7) 0.07033(5) 0.58929(2) 0.0571(2) Uani 1 1 d . . . S26 S 0.16941(7) -0.01719(4) 0.62013(2) 0.04907(19) Uani 1 1 d . . . S27 S 0.24690(8) 0.15674(4) 0.36410(2) 0.0536(2) Uani 1 1 d . . . S28 S 0.52311(7) 0.07220(4) 0.39295(2) 0.04483(17) Uani 1 1 d . . . C21 C 0.1792(2) 0.06017(12) 0.50830(7) 0.0337(5) Uani 1 1 d . . . C22 C 0.2326(2) 0.07309(12) 0.47423(7) 0.0332(5) Uani 1 1 d . . . C23 C 0.0292(2) 0.05433(13) 0.56434(7) 0.0363(5) Uani 1 1 d . A . C24 C 0.1361(2) 0.01965(13) 0.57593(7) 0.0348(5) Uani 1 1 d . A . C25 C 0.2767(3) 0.11730(12) 0.40754(7) 0.0359(5) Uani 1 1 d . B . C26 C 0.3854(2) 0.08371(12) 0.41898(7) 0.0344(5) Uani 1 1 d . B . C27A C -0.0462(8) 0.0541(4) 0.6379(2) 0.0495(16) Uani 0.65 1 d P A 1 H27A H 0.0160 0.0887 0.6452 0.059 Uiso 0.65 1 calc PR A 1 H27B H -0.1174 0.0566 0.6550 0.059 Uiso 0.65 1 calc PR A 1 C28A C 0.0191(4) -0.0130(2) 0.64243(12) 0.0420(9) Uani 0.65 1 d P A 1 H28A H -0.0386 -0.0471 0.6318 0.050 Uiso 0.65 1 calc PR A 1 H28B H 0.0335 -0.0225 0.6693 0.050 Uiso 0.65 1 calc PR A 1 C27B C -0.0861(13) 0.0309(8) 0.6314(4) 0.049(3) Uani 0.35 1 d P A 2 H27C H -0.1425 0.0508 0.6497 0.059 Uiso 0.35 1 calc PR A 2 H27D H -0.1110 -0.0156 0.6284 0.059 Uiso 0.35 1 calc PR A 2 C28B C 0.0536(9) 0.0342(6) 0.6471(2) 0.053(2) Uani 0.35 1 d P A 2 H28C H 0.0564 0.0193 0.6733 0.063 Uiso 0.35 1 calc PR A 2 H28D H 0.0822 0.0804 0.6469 0.063 Uiso 0.35 1 calc PR A 2 C29A C 0.3677(7) 0.1254(3) 0.33387(19) 0.0474(14) Uani 0.65 1 d P B 1 H29A H 0.3269 0.1176 0.3089 0.057 Uiso 0.65 1 calc PR B 1 H29B H 0.4330 0.1599 0.3311 0.057 Uiso 0.65 1 calc PR B 1 C30A C 0.4357(6) 0.0622(3) 0.34671(14) 0.0483(11) Uani 0.65 1 d P B 1 H30A H 0.4970 0.0491 0.3279 0.058 Uiso 0.65 1 calc PR B 1 H30B H 0.3719 0.0267 0.3485 0.058 Uiso 0.65 1 calc PR B 1 C29B C 0.3404(14) 0.0977(7) 0.3355(4) 0.053(3) Uani 0.35 1 d P B 2 H29C H 0.3061 0.0530 0.3387 0.064 Uiso 0.35 1 calc PR B 2 H29D H 0.3287 0.1095 0.3089 0.064 Uiso 0.35 1 calc PR B 2 C30B C 0.4834(11) 0.0975(6) 0.3464(3) 0.055(2) Uani 0.35 1 d P B 2 H30C H 0.5171 0.1423 0.3429 0.066 Uiso 0.35 1 calc PR B 2 H30D H 0.5272 0.0682 0.3292 0.066 Uiso 0.35 1 calc PR B 2 Fe1 Fe 0.5000 0.08266(3) 0.7500 0.04077(14) Uani 1 2 d S . . O1 O 0.4276(2) 0.15987(11) 0.71906(6) 0.0540(5) Uani 1 1 d . . . O2 O 0.3978(2) 0.01875(11) 0.71659(5) 0.0493(5) Uani 1 1 d . . . O3 O 0.6519(2) 0.06668(10) 0.71736(5) 0.0489(5) Uani 1 1 d . . . O4 O 0.4121(3) 0.27080(12) 0.71901(8) 0.0718(7) Uani 1 1 d . . . O5 O 0.2227(2) -0.04657(13) 0.71499(7) 0.0650(6) Uani 1 1 d . . . O6 O 0.8230(2) -0.00102(13) 0.71247(7) 0.0689(7) Uani 1 1 d . . . C1 C 0.4535(3) 0.21812(16) 0.73216(9) 0.0512(7) Uani 1 1 d . . . C2 C 0.2958(3) -0.00564(15) 0.73036(8) 0.0446(6) Uani 1 1 d . . . C3 C 0.7315(3) 0.02149(15) 0.72934(8) 0.0467(7) Uani 1 1 d . . . C41 C 0.0000 0.2492(7) 0.7500 0.0800(12) Uiso 0.400(10) 2 d SPD . 1 C42 C 0.0915(10) 0.2151(6) 0.7312(3) 0.0800(12) Uiso 0.400(10) 1 d PD . 1 H42 H 0.1555 0.2381 0.7187 0.096 Uiso 0.400(10) 1 calc PR . 1 C43 C 0.0896(9) 0.1486(6) 0.7307(3) 0.0800(12) Uiso 0.400(10) 1 d PD . 1 H43 H 0.1503 0.1252 0.7171 0.096 Uiso 0.400(10) 1 calc PR . 1 C44 C 0.0000 0.1149(7) 0.7500 0.0800(12) Uiso 0.400(10) 2 d SPD . 1 H44 H 0.0000 0.0684 0.7500 0.096 Uiso 0.400(10) 2 calc SPR . 1 C45 C 0.0000 0.3195(7) 0.7500 0.0800(12) Uiso 0.400(10) 2 d SPD . 1 N41 N 0.0000 0.3828(7) 0.7500 0.0800(12) Uiso 0.400(10) 2 d SP . 1 F31 F 0.0337(7) 0.3374(4) 0.7529(3) 0.0800(12) Uiso 0.300(5) 1 d PD . 2 C31 C 0.0198(10) 0.2724(4) 0.7487(3) 0.0800(12) Uiso 0.300(5) 1 d PGD . 2 C32 C -0.0783(9) 0.2364(5) 0.7654(3) 0.0800(12) Uiso 0.300(5) 1 d PGD . 2 H32 H -0.1410 0.2586 0.7788 0.096 Uiso 0.300(5) 1 calc PR . 2 C33 C -0.0826(10) 0.1673(5) 0.7619(3) 0.0800(12) Uiso 0.300(5) 1 d PGD . 2 H33 H -0.1483 0.1432 0.7730 0.096 Uiso 0.300(5) 1 calc PR . 2 C34 C 0.0112(11) 0.1342(4) 0.7418(3) 0.0800(12) Uiso 0.300(5) 1 d PGD . 2 H34 H 0.0083 0.0879 0.7394 0.096 Uiso 0.300(5) 1 calc PR . 2 C35 C 0.1093(10) 0.1702(5) 0.7251(3) 0.0800(12) Uiso 0.300(5) 1 d PGD . 2 H35 H 0.1720 0.1480 0.7117 0.096 Uiso 0.300(5) 1 calc PR . 2 C36 C 0.1136(9) 0.2393(5) 0.7286(3) 0.0800(12) Uiso 0.300(5) 1 d PGD . 2 H36 H 0.1792 0.2634 0.7175 0.096 Uiso 0.300(5) 1 calc PR . 2 O51 O 0.0100(8) -0.09769(18) 0.75530(19) 0.0606(12) Uiso 0.50 1 d PD C 2 H51A H 0.044(5) -0.153(2) 0.764(2) 0.091 Uiso 0.50 1 d PD D 2 H51B H 0.091(5) -0.055(2) 0.762(2) 0.091 Uiso 0.50 1 d PD E 2 H51C H -0.097(5) -0.082(2) 0.765(2) 0.091 Uiso 0.50 1 d PD F 2 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 S11 0.0357(3) 0.0528(4) 0.0362(3) 0.0045(3) 0.0040(3) 0.0105(3) S12 0.0333(3) 0.0495(4) 0.0344(3) 0.0082(3) 0.0065(2) 0.0080(3) S13 0.0374(3) 0.0518(4) 0.0363(3) 0.0065(3) 0.0022(3) 0.0095(3) S14 0.0348(3) 0.0475(4) 0.0389(3) 0.0067(3) 0.0047(3) 0.0075(3) S15 0.0364(3) 0.0618(4) 0.0476(4) 0.0039(3) 0.0129(3) 0.0113(3) S16 0.0418(4) 0.0556(4) 0.0383(4) 0.0138(3) 0.0089(3) 0.0076(3) S17 0.0768(6) 0.0677(5) 0.0337(4) 0.0107(3) -0.0012(4) 0.0063(4) S18 0.0523(4) 0.0496(4) 0.0589(5) 0.0033(3) 0.0262(4) 0.0027(3) C11 0.0317(12) 0.0375(13) 0.0323(12) 0.0003(10) 0.0029(10) 0.0012(10) C12 0.0332(12) 0.0371(13) 0.0312(12) 0.0002(10) 0.0026(10) 0.0023(10) C13 0.0355(13) 0.0385(13) 0.0325(12) -0.0006(10) 0.0070(10) 0.0010(10) C14 0.0333(12) 0.0377(13) 0.0315(12) 0.0014(10) 0.0060(10) 0.0000(10) C15 0.0475(15) 0.0369(13) 0.0284(12) 0.0014(10) 0.0046(11) -0.0016(11) C16 0.0406(14) 0.0354(13) 0.0353(13) 0.0002(10) 0.0095(11) -0.0008(10) C17 0.0485(16) 0.0507(16) 0.0406(15) -0.0005(12) 0.0172(12) 0.0025(13) C18 0.0454(15) 0.0450(15) 0.0418(15) 0.0045(12) 0.0145(12) -0.0015(12) C19 0.077(2) 0.102(3) 0.0359(16) 0.0102(18) 0.0063(16) -0.027(2) C20 0.083(3) 0.075(2) 0.0522(19) -0.0186(17) 0.0278(18) -0.018(2) S21 0.0354(3) 0.0565(4) 0.0314(3) 0.0073(3) 0.0052(2) 0.0137(3) S22 0.0346(3) 0.0498(4) 0.0337(3) 0.0077(3) 0.0058(2) 0.0116(3) S23 0.0352(3) 0.0568(4) 0.0307(3) 0.0062(3) 0.0068(2) 0.0144(3) S24 0.0344(3) 0.0461(4) 0.0369(3) 0.0047(3) 0.0056(3) 0.0108(3) S25 0.0416(4) 0.0858(6) 0.0453(4) 0.0192(4) 0.0163(3) 0.0252(4) S26 0.0378(4) 0.0642(5) 0.0457(4) 0.0259(3) 0.0086(3) 0.0077(3) S27 0.0647(5) 0.0611(5) 0.0362(4) 0.0136(3) 0.0158(3) 0.0221(4) S28 0.0373(3) 0.0476(4) 0.0509(4) 0.0023(3) 0.0174(3) 0.0068(3) C21 0.0327(12) 0.0380(13) 0.0305(12) 0.0024(10) 0.0032(9) 0.0029(10) C22 0.0307(12) 0.0382(13) 0.0308(12) 0.0012(10) 0.0037(9) 0.0043(10) C23 0.0331(12) 0.0429(13) 0.0333(12) 0.0057(10) 0.0062(10) 0.0052(10) C24 0.0315(12) 0.0399(13) 0.0335(13) 0.0078(10) 0.0062(10) 0.0017(10) C25 0.0406(13) 0.0372(13) 0.0305(12) 0.0036(10) 0.0101(10) 0.0072(10) C26 0.0361(13) 0.0330(12) 0.0349(12) 0.0006(10) 0.0093(10) 0.0025(10) C27A 0.052(5) 0.063(5) 0.034(3) 0.006(3) 0.009(3) 0.016(3) C28A 0.040(2) 0.048(3) 0.039(2) 0.013(2) 0.0105(17) 0.0048(19) C27B 0.041(7) 0.072(10) 0.035(6) 0.015(6) 0.013(5) 0.005(5) C28B 0.056(6) 0.072(7) 0.030(4) -0.002(4) 0.002(4) 0.005(5) C29A 0.051(4) 0.056(4) 0.036(2) -0.001(3) 0.010(2) -0.001(3) C30A 0.057(3) 0.046(3) 0.043(2) -0.010(2) 0.014(2) 0.008(2) C29B 0.061(7) 0.060(8) 0.039(5) -0.021(6) 0.017(5) -0.023(6) C30B 0.064(6) 0.052(6) 0.051(5) -0.005(5) 0.022(5) 0.002(5) Fe1 0.0476(3) 0.0452(3) 0.0300(3) 0.000 0.0067(2) 0.000 O1 0.0707(14) 0.0511(12) 0.0400(11) 0.0048(9) -0.0018(10) 0.0035(10) O2 0.0522(12) 0.0618(13) 0.0348(10) -0.0081(9) 0.0122(9) -0.0082(10) O3 0.0529(12) 0.0579(12) 0.0368(10) 0.0049(9) 0.0124(9) -0.0018(10) O4 0.0811(17) 0.0522(13) 0.0824(18) 0.0137(12) 0.0082(14) 0.0079(12) O5 0.0597(14) 0.0812(16) 0.0546(13) -0.0088(12) 0.0073(11) -0.0202(12) O6 0.0638(15) 0.0889(18) 0.0563(14) 0.0010(13) 0.0280(12) 0.0111(13) C1 0.0551(18) 0.0511(17) 0.0488(16) 0.0068(14) 0.0194(14) 0.0025(14) C2 0.0464(16) 0.0504(16) 0.0372(14) 0.0030(12) 0.0043(12) 0.0036(13) C3 0.0445(16) 0.0543(17) 0.0421(15) -0.0068(13) 0.0110(12) -0.0082(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.737(3) . ? S11 C13 1.747(3) . ? S12 C11 1.736(2) . ? S12 C14 1.742(2) . ? S13 C12 1.735(2) . ? S13 C15 1.742(3) . ? S14 C12 1.739(2) . ? S14 C16 1.741(3) . ? S15 C13 1.741(3) . ? S15 C17 1.808(3) . ? S16 C14 1.743(3) . ? S16 C18 1.790(3) . ? S17 C15 1.743(3) . ? S17 C19 1.803(4) . ? S18 C16 1.740(3) . ? S18 C20 1.789(4) . ? C11 C12 1.359(3) . ? C13 C14 1.352(3) . ? C15 C16 1.342(4) . ? C17 C18 1.509(4) . ? C19 C20 1.504(6) . ? S21 C21 1.735(3) . ? S21 C23 1.740(3) . ? S22 C21 1.737(2) . ? S22 C24 1.744(2) . ? S23 C22 1.732(2) . ? S23 C25 1.744(2) . ? S24 C22 1.737(2) . ? S24 C26 1.744(3) . ? S25 C27B 1.691(14) . ? S25 C23 1.739(3) . ? S25 C27A 1.837(8) . ? S26 C24 1.744(2) . ? S26 C28A 1.766(4) . ? S26 C28B 1.865(9) . ? S27 C25 1.738(3) . ? S27 C29A 1.785(7) . ? S27 C29B 1.850(14) . ? S28 C26 1.736(2) . ? S28 C30B 1.749(10) . ? S28 C30A 1.838(5) . ? C21 C22 1.367(3) . ? C23 C24 1.349(3) . ? C25 C26 1.350(3) . ? C27A C28A 1.506(9) . ? C27B C28B 1.517(15) . ? C29A C30A 1.507(9) . ? C29B C30B 1.503(18) . ? Fe1 O3 2.005(2) . ? Fe1 O3 2.005(2) 2_656 ? Fe1 O2 2.005(2) . ? Fe1 O2 2.005(2) 2_656 ? Fe1 O1 2.016(2) 2_656 ? Fe1 O1 2.016(2) . ? O1 C1 1.278(4) . ? O2 C2 1.272(3) . ? O3 C3 1.279(4) . ? O4 C1 1.221(4) . ? O5 C2 1.222(4) . ? O6 C3 1.221(3) . ? C1 C1 1.546(7) 2_656 ? C2 C3 1.558(4) 2_656 ? C3 C2 1.558(4) 2_656 ? C41 C42 1.358(9) 2_556 ? C41 C42 1.358(9) . ? C41 C45 1.408(5) . ? C42 C43 1.332(14) . ? C43 C44 1.348(9) . ? C44 C43 1.348(9) 2_556 ? C45 N41 1.27(2) . ? F31 C31 1.316(11) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 S11 C13 95.25(12) . . ? C11 S12 C14 95.65(12) . . ? C12 S13 C15 95.42(12) . . ? C12 S14 C16 95.42(12) . . ? C13 S15 C17 101.70(13) . . ? C14 S16 C18 101.41(13) . . ? C15 S17 C19 102.43(16) . . ? C16 S18 C20 99.01(15) . . ? C12 C11 S12 121.8(2) . . ? C12 C11 S11 123.0(2) . . ? S12 C11 S11 115.24(14) . . ? C11 C12 S13 122.8(2) . . ? C11 C12 S14 122.20(19) . . ? S13 C12 S14 114.96(14) . . ? C14 C13 S15 129.0(2) . . ? C14 C13 S11 117.15(19) . . ? S15 C13 S11 113.88(14) . . ? C13 C14 S12 116.69(19) . . ? C13 C14 S16 127.98(19) . . ? S12 C14 S16 115.32(14) . . ? C16 C15 S13 117.17(19) . . ? C16 C15 S17 128.7(2) . . ? S13 C15 S17 114.08(15) . . ? C15 C16 S18 127.7(2) . . ? C15 C16 S14 117.01(19) . . ? S18 C16 S14 115.23(15) . . ? C18 C17 S15 114.1(2) . . ? C17 C18 S16 114.64(19) . . ? C20 C19 S17 114.6(2) . . ? C19 C20 S18 112.6(2) . . ? C21 S21 C23 94.96(12) . . ? C21 S22 C24 95.40(12) . . ? C22 S23 C25 95.39(12) . . ? C22 S24 C26 94.87(12) . . ? C27B S25 C23 105.6(5) . . ? C23 S25 C27A 100.0(3) . . ? C24 S26 C28A 103.66(16) . . ? C24 S26 C28B 96.7(3) . . ? C25 S27 C29A 105.4(2) . . ? C25 S27 C29B 96.5(5) . . ? C26 S28 C30B 107.2(3) . . ? C26 S28 C30A 96.02(19) . . ? C22 C21 S21 122.15(19) . . ? C22 C21 S22 122.4(2) . . ? S21 C21 S22 115.44(14) . . ? C21 C22 S23 121.90(19) . . ? C21 C22 S24 122.60(19) . . ? S23 C22 S24 115.46(14) . . ? C24 C23 S25 128.2(2) . . ? C24 C23 S21 117.78(19) . . ? S25 C23 S21 114.05(14) . . ? C23 C24 S26 127.9(2) . . ? C23 C24 S22 116.39(19) . . ? S26 C24 S22 115.70(14) . . ? C26 C25 S27 126.95(19) . . ? C26 C25 S23 116.57(19) . . ? S27 C25 S23 116.41(14) . . ? C25 C26 S28 126.3(2) . . ? C25 C26 S24 117.43(19) . . ? S28 C26 S24 116.20(14) . . ? C28A C27A S25 113.3(5) . . ? C27A C28A S26 112.9(4) . . ? C28B C27B S25 113.4(9) . . ? C27B C28B S26 113.9(8) . . ? C30A C29A S27 116.2(4) . . ? C29A C30A S28 112.2(4) . . ? C30B C29B S27 112.8(8) . . ? C29B C30B S28 115.2(8) . . ? O3 Fe1 O3 161.65(12) . 2_656 ? O3 Fe1 O2 87.84(8) . . ? O3 Fe1 O2 80.46(8) 2_656 . ? O3 Fe1 O2 80.46(8) . 2_656 ? O3 Fe1 O2 87.84(8) 2_656 2_656 ? O2 Fe1 O2 100.69(13) . 2_656 ? O3 Fe1 O1 98.89(9) . 2_656 ? O3 Fe1 O1 95.17(9) 2_656 2_656 ? O2 Fe1 O1 168.23(9) . 2_656 ? O2 Fe1 O1 90.00(9) 2_656 2_656 ? O3 Fe1 O1 95.17(9) . . ? O3 Fe1 O1 98.90(9) 2_656 . ? O2 Fe1 O1 90.00(9) . . ? O2 Fe1 O1 168.23(9) 2_656 . ? O1 Fe1 O1 79.83(13) 2_656 . ? C1 O1 Fe1 116.0(2) . . ? C2 O2 Fe1 116.13(18) . . ? C3 O3 Fe1 115.24(17) . . ? O4 C1 O1 126.0(3) . . ? O4 C1 C1 120.1(2) . 2_656 ? O1 C1 C1 113.94(17) . 2_656 ? O5 C2 O2 126.1(3) . . ? O5 C2 C3 120.4(3) . 2_656 ? O2 C2 C3 113.5(3) . 2_656 ? O6 C3 O3 126.6(3) . . ? O6 C3 C2 119.3(3) . 2_656 ? O3 C3 C2 114.2(2) . 2_656 ? C42 C41 C42 119.7(10) 2_556 . ? C42 C41 C45 120.2(5) 2_556 . ? C42 C41 C45 120.2(5) . . ? C43 C42 C41 119.9(5) . . ? C42 C43 C44 120.3(5) . . ? C43 C44 C43 120.0(10) . 2_556 ? N41 C45 C41 180.000(9) . . ? F31 C31 C32 122.9(6) . . ? F31 C31 C36 117.0(6) . . ? C32 C31 C36 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? # Attachment '- VII.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.86(DCB)0.14-(VII) _database_code_depnum_ccdc_archive 'CCDC 771734' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, 0.86(C7 H5 N), 0.14(C6 H4 Cl2), H3 O' _chemical_formula_sum 'C52.86 H39.86 Cl0.28 Fe N0.86 O13 S32' _chemical_formula_weight 1986.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 10.2877(7) _cell_length_b 20.1034(15) _cell_length_c 35.198(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.821(8) _cell_angle_gamma 90.00 _cell_volume 7270.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_radiation CuK\a _cell_measurement_reflns_used 3217 _cell_measurement_theta_min 12.0714 _cell_measurement_theta_max 52.3202 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4039 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79652 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43893 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 29.69 _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.913 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.083 _reflns_number_total 9296 _reflns_number_gt 6480 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0726P)^2^+4.8705P] 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 9296 _refine_ls_number_parameters 480 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S11 S 0.42274(6) 0.21439(4) 0.50827(2) 0.04089(17) Uani 1 1 d . . . S12 S 0.66365(6) 0.14362(4) 0.531095(19) 0.03877(16) Uani 1 1 d . . . S13 S 0.54238(6) 0.24589(4) 0.42639(2) 0.04050(17) Uani 1 1 d . . . S14 S 0.78021(6) 0.17398(3) 0.45040(2) 0.03948(16) Uani 1 1 d . . . S15 S 0.29452(7) 0.19307(4) 0.57969(2) 0.04726(19) Uani 1 1 d . . . S16 S 0.58521(7) 0.11079(4) 0.60835(2) 0.04468(18) Uani 1 1 d . . . S17 S 0.62184(9) 0.27493(4) 0.34935(2) 0.0553(2) Uani 1 1 d . . . S18 S 0.90993(7) 0.19337(4) 0.37840(2) 0.0501(2) Uani 1 1 d . . . C11 C 0.5764(2) 0.18817(13) 0.49615(7) 0.0341(5) Uani 1 1 d . . . C12 C 0.6264(2) 0.20155(12) 0.46188(7) 0.0330(5) Uani 1 1 d . . . C13 C 0.4330(2) 0.17996(12) 0.55411(7) 0.0343(5) Uani 1 1 d . . . C14 C 0.5442(2) 0.14786(12) 0.56460(7) 0.0326(5) Uani 1 1 d . . . C15 C 0.6642(3) 0.24004(13) 0.39373(7) 0.0368(6) Uani 1 1 d . . . C16 C 0.7738(2) 0.20815(12) 0.40480(8) 0.0359(6) Uani 1 1 d . . . C17 C 0.3515(3) 0.16931(15) 0.62728(8) 0.0468(7) Uani 1 1 d . . . H17A H 0.4050 0.2049 0.6382 0.056 Uiso 1 1 calc R . . H17B H 0.2769 0.1643 0.6429 0.056 Uiso 1 1 calc R . . C18 C 0.4289(3) 0.10580(14) 0.62890(8) 0.0436(6) Uani 1 1 d . . . H18A H 0.3784 0.0713 0.6158 0.052 Uiso 1 1 calc R . . H18B H 0.4418 0.0924 0.6553 0.052 Uiso 1 1 calc R . . C19 C 0.7668(4) 0.2614(2) 0.32342(10) 0.0665(10) Uani 1 1 d . . . H19A H 0.7436 0.2637 0.2964 0.080 Uiso 1 1 calc R . . H19B H 0.8276 0.2973 0.3294 0.080 Uiso 1 1 calc R . . C20 C 0.8345(4) 0.19585(19) 0.33174(10) 0.0649(9) Uani 1 1 d . . . H20A H 0.8999 0.1887 0.3133 0.078 Uiso 1 1 calc R . . H20B H 0.7714 0.1601 0.3290 0.078 Uiso 1 1 calc R . . S21 S 0.02577(6) 0.08851(4) 0.518849(19) 0.04043(17) Uani 1 1 d . . . S22 S 0.25800(6) 0.01227(3) 0.543543(19) 0.03873(16) Uani 1 1 d . . . S23 S 0.15019(6) 0.11831(4) 0.439002(18) 0.03999(17) Uani 1 1 d . . . S24 S 0.38507(6) 0.04367(3) 0.462996(19) 0.03828(16) Uani 1 1 d . . . S25 S -0.10975(7) 0.07038(5) 0.58924(2) 0.0576(2) Uani 1 1 d . . . S26 S 0.16930(7) -0.01707(4) 0.62036(2) 0.0482(2) Uani 1 1 d . . . S27 S 0.24596(8) 0.15770(4) 0.36445(2) 0.0517(2) Uani 1 1 d . . . S28 S 0.52224(7) 0.07244(4) 0.39269(2) 0.04335(18) Uani 1 1 d . . . C21 C 0.1793(2) 0.05980(13) 0.50837(7) 0.0329(5) Uani 1 1 d . . . C22 C 0.2328(2) 0.07317(12) 0.47441(7) 0.0326(5) Uani 1 1 d . . . C23 C 0.0287(2) 0.05425(13) 0.56432(7) 0.0360(6) Uani 1 1 d . A . C24 C 0.1360(2) 0.01951(12) 0.57599(7) 0.0333(5) Uani 1 1 d . A . C25 C 0.2771(2) 0.11768(12) 0.40781(7) 0.0350(5) Uani 1 1 d . B . C26 C 0.3855(2) 0.08383(12) 0.41911(7) 0.0339(5) Uani 1 1 d . B . C27A C -0.0498(6) 0.0534(3) 0.63772(15) 0.0464(13) Uani 0.72 1 d P A 1 H27A H 0.0112 0.0880 0.6458 0.056 Uiso 0.72 1 calc PR A 1 H27B H -0.1222 0.0551 0.6543 0.056 Uiso 0.72 1 calc PR A 1 C28A C 0.0166(4) -0.0134(2) 0.64233(11) 0.0411(9) Uani 0.72 1 d P A 1 H28A H -0.0403 -0.0475 0.6314 0.049 Uiso 0.72 1 calc PR A 1 H28B H 0.0305 -0.0230 0.6692 0.049 Uiso 0.72 1 calc PR A 1 C27B C -0.0871(14) 0.0293(8) 0.6308(4) 0.044(3) Uani 0.28 1 d PU A 2 H27C H -0.1443 0.0478 0.6492 0.052 Uiso 0.28 1 calc PR A 2 H27D H -0.1101 -0.0171 0.6270 0.052 Uiso 0.28 1 calc PR A 2 C28B C 0.0533(12) 0.0339(7) 0.6465(3) 0.056(3) Uani 0.28 1 d PU A 2 H28C H 0.0569 0.0199 0.6729 0.067 Uiso 0.28 1 calc PR A 2 H28D H 0.0808 0.0800 0.6458 0.067 Uiso 0.28 1 calc PR A 2 C29A C 0.3662(5) 0.1281(3) 0.33395(14) 0.0482(11) Uani 0.77 1 d P B 1 H29A H 0.3251 0.1210 0.3089 0.058 Uiso 0.77 1 calc PR B 1 H29B H 0.4311 0.1627 0.3316 0.058 Uiso 0.77 1 calc PR B 1 C30A C 0.4353(5) 0.0646(2) 0.34619(12) 0.0480(10) Uani 0.77 1 d P B 1 H30A H 0.4968 0.0527 0.3273 0.058 Uiso 0.77 1 calc PR B 1 H30B H 0.3720 0.0290 0.3473 0.058 Uiso 0.77 1 calc PR B 1 C29B C 0.3401(17) 0.0978(8) 0.3372(5) 0.045(4) Uani 0.23 1 d PU B 2 H29C H 0.3050 0.0536 0.3410 0.054 Uiso 0.23 1 calc PR B 2 H29D H 0.3277 0.1083 0.3103 0.054 Uiso 0.23 1 calc PR B 2 C30B C 0.4848(15) 0.0964(8) 0.3475(4) 0.051(4) Uani 0.23 1 d PU B 2 H30C H 0.5203 0.1405 0.3436 0.062 Uiso 0.23 1 calc PR B 2 H30D H 0.5265 0.0663 0.3303 0.062 Uiso 0.23 1 calc PR B 2 Fe1 Fe 0.5000 0.08239(3) 0.7500 0.03477(14) Uani 1 2 d S . . O1 O 0.4265(2) 0.15984(10) 0.71936(6) 0.0495(5) Uani 1 1 d . . . O2 O 0.39425(17) 0.02084(9) 0.71613(5) 0.0416(4) Uani 1 1 d . . . O3 O 0.64927(18) 0.06485(10) 0.71667(5) 0.0432(4) Uani 1 1 d . . . O4 O 0.4089(3) 0.27033(11) 0.71927(8) 0.0696(7) Uani 1 1 d . . . O5 O 0.2182(2) -0.04399(11) 0.71459(6) 0.0565(6) Uani 1 1 d . . . O6 O 0.8168(2) -0.00425(12) 0.71102(6) 0.0607(6) Uani 1 1 d . . . C1 C 0.4516(3) 0.21789(14) 0.73242(9) 0.0491(7) Uani 1 1 d . . . C2 C 0.2940(3) -0.00472(13) 0.73026(8) 0.0391(6) Uani 1 1 d . . . C3 C 0.7288(3) 0.01974(14) 0.72864(8) 0.0403(6) Uani 1 1 d . . . Cl31 Cl 0.0404(13) 0.3365(6) 0.7538(5) 0.0688(6) Uiso 0.0698(16) 1 d P . 1 Cl32 Cl -0.1730(13) 0.2488(7) 0.7874(4) 0.0688(6) Uiso 0.0698(16) 1 d P . 1 C32 C -0.0640(17) 0.2136(3) 0.7595(7) 0.0688(6) Uiso 0.0698(16) 1 d PG . 1 C33 C -0.0673(19) 0.1456(3) 0.7525(9) 0.0688(6) Uiso 0.0698(16) 1 d PG . 1 H33 H -0.1330 0.1196 0.7620 0.083 Uiso 0.0698(16) 1 calc PR . 1 C34 C 0.0275(12) 0.11642(19) 0.7311(6) 0.0688(6) Uiso 0.0698(16) 1 d PG . 1 H34 H 0.0253 0.0709 0.7264 0.083 Uiso 0.0698(16) 1 calc PR . 1 C35 C 0.1256(6) 0.1553(2) 0.7168(2) 0.0688(6) Uiso 0.0698(16) 1 d PG . 1 H35 H 0.1891 0.1357 0.7026 0.083 Uiso 0.0698(16) 1 calc PR . 1 C36 C 0.1290(5) 0.2233(2) 0.72388(19) 0.0688(6) Uiso 0.0698(16) 1 d PG . 1 H36 H 0.1946 0.2493 0.7143 0.083 Uiso 0.0698(16) 1 calc PR . 1 C31 C 0.0342(7) 0.25248(15) 0.7452(2) 0.0688(6) Uiso 0.0698(16) 1 d PG . 1 N41 N 0.0200(8) 0.37687(17) 0.7535(3) 0.0688(6) Uiso 0.4302(16) 1 d PG . 2 C47 C 0.0126(6) 0.32008(16) 0.7519(2) 0.0688(6) Uiso 0.4302(16) 1 d PG . 2 C41 C 0.0000(9) 0.25003(17) 0.7500(4) 0.0688(6) Uiso 0.860(3) 2 d SPG . 2 C42 C 0.0938(4) 0.21580(17) 0.73072(13) 0.0688(6) Uiso 0.860(3) 1 d PG . 2 H42 H 0.1569 0.2386 0.7179 0.083 Uiso 0.860(3) 1 calc PR . 2 C43 C 0.0913(4) 0.1470(2) 0.73112(13) 0.0688(6) Uiso 0.860(3) 1 d P . 2 H43 H 0.1530 0.1232 0.7183 0.083 Uiso 0.860(3) 1 calc PR . 2 C44 C 0.0000 0.1141(3) 0.7500 0.0688(6) Uiso 0.860(3) 2 d SP . 2 H44 H 0.0000 0.0678 0.7500 0.083 Uiso 0.860(3) 2 calc SPR . 2 O51 O 0.0097(7) -0.09881(17) 0.75553(18) 0.0579(12) Uiso 0.50 1 d PD . . H51A H 0.030(5) -0.153(2) 0.7645(19) 0.087 Uiso 0.50 1 d PD . . H51B H 0.092(5) -0.062(2) 0.767(2) 0.087 Uiso 0.50 1 d PD . . H51C H -0.092(5) -0.080(2) 0.765(2) 0.087 Uiso 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 S11 0.0334(3) 0.0514(4) 0.0381(4) 0.0048(3) 0.0038(3) 0.0103(3) S12 0.0314(3) 0.0494(4) 0.0359(3) 0.0082(3) 0.0061(3) 0.0084(3) S13 0.0341(3) 0.0498(4) 0.0377(4) 0.0061(3) 0.0022(3) 0.0096(3) S14 0.0323(3) 0.0465(4) 0.0399(4) 0.0077(3) 0.0043(3) 0.0077(3) S15 0.0350(4) 0.0593(5) 0.0484(4) 0.0036(3) 0.0116(3) 0.0115(3) S16 0.0386(4) 0.0558(4) 0.0402(4) 0.0135(3) 0.0086(3) 0.0075(3) S17 0.0659(5) 0.0642(5) 0.0355(4) 0.0106(3) -0.0012(4) 0.0071(4) S18 0.0467(4) 0.0486(4) 0.0568(5) 0.0038(3) 0.0226(4) 0.0043(3) C11 0.0282(12) 0.0396(14) 0.0344(13) -0.0002(11) 0.0016(10) 0.0018(10) C12 0.0291(12) 0.0343(13) 0.0356(13) 0.0012(10) 0.0002(10) 0.0017(10) C13 0.0337(13) 0.0360(13) 0.0337(13) -0.0018(10) 0.0081(11) 0.0011(10) C14 0.0302(12) 0.0350(13) 0.0330(13) 0.0008(10) 0.0046(10) -0.0003(10) C15 0.0423(14) 0.0343(13) 0.0338(13) 0.0008(11) 0.0027(11) -0.0002(11) C16 0.0369(13) 0.0340(13) 0.0374(14) 0.0011(11) 0.0073(11) 0.0017(11) C17 0.0468(16) 0.0490(17) 0.0460(16) 0.0001(13) 0.0161(13) 0.0056(13) C18 0.0450(15) 0.0442(15) 0.0426(15) 0.0062(12) 0.0121(13) -0.0038(12) C19 0.066(2) 0.095(3) 0.0387(17) 0.0113(18) 0.0069(16) -0.012(2) C20 0.071(2) 0.073(2) 0.052(2) -0.0177(17) 0.0210(17) -0.0097(19) S21 0.0331(3) 0.0553(4) 0.0332(3) 0.0077(3) 0.0046(3) 0.0135(3) S22 0.0328(3) 0.0484(4) 0.0354(3) 0.0081(3) 0.0057(3) 0.0120(3) S23 0.0332(3) 0.0559(4) 0.0313(3) 0.0068(3) 0.0066(3) 0.0142(3) S24 0.0323(3) 0.0453(4) 0.0376(3) 0.0055(3) 0.0049(3) 0.0110(3) S25 0.0403(4) 0.0877(6) 0.0463(4) 0.0204(4) 0.0164(3) 0.0267(4) S26 0.0354(4) 0.0631(5) 0.0466(4) 0.0260(4) 0.0083(3) 0.0077(3) S27 0.0611(5) 0.0596(5) 0.0356(4) 0.0127(3) 0.0157(3) 0.0226(4) S28 0.0339(3) 0.0456(4) 0.0519(4) 0.0012(3) 0.0160(3) 0.0064(3) C21 0.0280(12) 0.0392(13) 0.0315(12) 0.0016(10) 0.0012(10) 0.0053(10) C22 0.0288(12) 0.0365(13) 0.0327(13) 0.0006(10) 0.0025(10) 0.0067(10) C23 0.0323(13) 0.0427(14) 0.0335(13) 0.0061(11) 0.0062(11) 0.0058(11) C24 0.0296(12) 0.0375(13) 0.0333(13) 0.0072(10) 0.0058(10) 0.0040(10) C25 0.0381(13) 0.0345(13) 0.0330(13) 0.0019(10) 0.0085(11) 0.0085(11) C26 0.0338(13) 0.0347(13) 0.0339(13) -0.0005(10) 0.0088(11) 0.0023(10) C27A 0.052(4) 0.056(3) 0.032(2) 0.004(2) 0.006(2) 0.015(3) C28A 0.037(2) 0.049(2) 0.038(2) 0.0137(18) 0.0089(16) 0.0044(18) C27B 0.038(6) 0.051(7) 0.042(6) -0.001(5) 0.006(5) -0.001(5) C28B 0.066(7) 0.068(6) 0.034(5) 0.003(5) 0.002(5) 0.000(6) C29A 0.050(3) 0.060(3) 0.036(2) 0.000(2) 0.0131(19) 0.002(2) C30A 0.053(3) 0.050(2) 0.042(2) -0.0085(19) 0.013(2) 0.004(2) C29B 0.054(7) 0.043(7) 0.039(6) -0.010(6) 0.013(6) -0.012(6) C30B 0.050(7) 0.051(7) 0.054(7) -0.004(6) 0.016(6) -0.007(6) Fe1 0.0399(3) 0.0336(3) 0.0312(3) 0.000 0.0053(2) 0.000 O1 0.0685(14) 0.0382(11) 0.0415(11) 0.0047(8) 0.0001(10) 0.0051(9) O2 0.0416(10) 0.0464(11) 0.0375(10) -0.0057(8) 0.0096(8) -0.0063(8) O3 0.0433(10) 0.0480(11) 0.0393(10) 0.0051(9) 0.0106(9) -0.0026(9) O4 0.0840(17) 0.0417(12) 0.0832(17) 0.0135(12) 0.0057(14) 0.0100(11) O5 0.0462(12) 0.0691(14) 0.0542(13) -0.0070(11) 0.0033(10) -0.0176(11) O6 0.0542(13) 0.0736(15) 0.0562(14) -0.0018(11) 0.0219(11) 0.0116(11) C1 0.0609(19) 0.0363(15) 0.0517(18) 0.0074(13) 0.0185(14) 0.0007(13) C2 0.0380(14) 0.0406(14) 0.0387(14) 0.0049(11) 0.0029(12) 0.0011(12) C3 0.0377(14) 0.0456(15) 0.0383(14) -0.0092(12) 0.0082(12) -0.0071(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.740(3) . ? S11 C13 1.754(3) . ? S12 C11 1.735(3) . ? S12 C14 1.747(3) . ? S13 C12 1.731(2) . ? S13 C15 1.746(3) . ? S14 C12 1.743(3) . ? S14 C16 1.744(3) . ? S15 C13 1.742(3) . ? S15 C17 1.811(3) . ? S16 C14 1.744(3) . ? S16 C18 1.798(3) . ? S17 C15 1.748(3) . ? S17 C19 1.806(4) . ? S18 C16 1.744(3) . ? S18 C20 1.783(4) . ? C11 C12 1.361(4) . ? C13 C14 1.349(3) . ? C15 C16 1.338(4) . ? C17 C18 1.505(4) . ? C19 C20 1.513(5) . ? S21 C21 1.738(3) . ? S21 C23 1.741(3) . ? S22 C21 1.733(2) . ? S22 C24 1.744(3) . ? S23 C22 1.731(2) . ? S23 C25 1.747(3) . ? S24 C22 1.741(2) . ? S24 C26 1.743(3) . ? S25 C27B 1.684(16) . ? S25 C23 1.740(3) . ? S25 C27A 1.818(5) . ? S26 C24 1.745(3) . ? S26 C28A 1.786(4) . ? S26 C28B 1.852(13) . ? S27 C25 1.741(3) . ? S27 C29A 1.780(5) . ? S27 C29B 1.844(17) . ? S28 C30B 1.689(16) . ? S28 C26 1.739(3) . ? S28 C30A 1.833(4) . ? C21 C22 1.367(4) . ? C23 C24 1.353(3) . ? C25 C26 1.349(4) . ? C27A C28A 1.512(7) . ? C27B C28B 1.524(18) . ? C29A C30A 1.513(6) . ? C29B C30B 1.52(2) . ? Fe1 O2 2.0019(18) . ? Fe1 O2 2.0019(18) 2_656 ? Fe1 O3 2.0091(19) 2_656 ? Fe1 O3 2.0091(19) . ? Fe1 O1 2.0196(19) 2_656 ? Fe1 O1 2.0196(19) . ? O1 C1 1.276(4) . ? O2 C2 1.275(3) . ? O3 C3 1.279(3) . ? O4 C1 1.224(4) . ? O5 C2 1.222(3) . ? O6 C3 1.221(3) . ? C1 C1 1.550(6) 2_656 ? C2 C3 1.557(4) 2_656 ? C3 C2 1.557(4) 2_656 ? Cl31 C31 1.717(13) . ? Cl32 C32 1.681(16) . ? C32 C33 1.3900 . ? C32 C31 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C31 1.3900 . ? N41 C47 1.1454 . ? C47 C41 1.4154 . ? C41 C42 1.389(8) 2_556 ? C41 C42 1.3893 . ? C41 C47 1.4154(17) 2_556 ? C42 C43 1.383(5) . ? C43 C44 1.350(6) . ? C44 C43 1.350(5) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 S11 C13 95.26(12) . . ? C11 S12 C14 95.57(12) . . ? C12 S13 C15 95.25(12) . . ? C12 S14 C16 95.42(12) . . ? C13 S15 C17 101.68(13) . . ? C14 S16 C18 101.36(13) . . ? C15 S17 C19 102.45(15) . . ? C16 S18 C20 99.29(15) . . ? C12 C11 S12 121.7(2) . . ? C12 C11 S11 123.0(2) . . ? S12 C11 S11 115.27(15) . . ? C11 C12 S13 123.0(2) . . ? C11 C12 S14 121.95(19) . . ? S13 C12 S14 115.04(15) . . ? C14 C13 S15 129.4(2) . . ? C14 C13 S11 116.89(19) . . ? S15 C13 S11 113.69(14) . . ? C13 C14 S16 127.7(2) . . ? C13 C14 S12 117.00(19) . . ? S16 C14 S12 115.32(14) . . ? C16 C15 S13 117.5(2) . . ? C16 C15 S17 128.5(2) . . ? S13 C15 S17 113.94(15) . . ? C15 C16 S18 127.9(2) . . ? C15 C16 S14 116.7(2) . . ? S18 C16 S14 115.36(14) . . ? C18 C17 S15 113.9(2) . . ? C17 C18 S16 114.8(2) . . ? C20 C19 S17 114.6(2) . . ? C19 C20 S18 112.2(2) . . ? C21 S21 C23 95.09(12) . . ? C21 S22 C24 95.51(12) . . ? C22 S23 C25 95.34(12) . . ? C22 S24 C26 95.06(12) . . ? C27B S25 C23 105.3(5) . . ? C23 S25 C27A 100.9(2) . . ? C24 S26 C28A 103.42(15) . . ? C24 S26 C28B 96.2(4) . . ? C25 S27 C29A 105.70(18) . . ? C25 S27 C29B 94.3(6) . . ? C30B S28 C26 108.3(5) . . ? C26 S28 C30A 96.72(17) . . ? C22 C21 S22 122.63(19) . . ? C22 C21 S21 121.96(19) . . ? S22 C21 S21 115.41(15) . . ? C21 C22 S23 121.90(19) . . ? C21 C22 S24 122.72(19) . . ? S23 C22 S24 115.34(15) . . ? C24 C23 S25 128.3(2) . . ? C24 C23 S21 117.4(2) . . ? S25 C23 S21 114.33(14) . . ? C23 C24 S22 116.53(19) . . ? C23 C24 S26 127.6(2) . . ? S22 C24 S26 115.81(14) . . ? C26 C25 S27 127.3(2) . . ? C26 C25 S23 116.8(2) . . ? S27 C25 S23 115.87(14) . . ? C25 C26 S28 125.9(2) . . ? C25 C26 S24 117.2(2) . . ? S28 C26 S24 116.76(14) . . ? C28A C27A S25 113.4(4) . . ? C27A C28A S26 113.1(3) . . ? C28B C27B S25 112.0(10) . . ? C27B C28B S26 114.1(9) . . ? C30A C29A S27 116.2(3) . . ? C29A C30A S28 112.6(3) . . ? C30B C29B S27 115.0(11) . . ? C29B C30B S28 114.0(11) . . ? O2 Fe1 O2 103.65(11) . 2_656 ? O2 Fe1 O3 80.25(8) . 2_656 ? O2 Fe1 O3 87.27(8) 2_656 2_656 ? O2 Fe1 O3 87.27(8) . . ? O2 Fe1 O3 80.25(8) 2_656 . ? O3 Fe1 O3 159.78(11) 2_656 . ? O2 Fe1 O1 166.56(8) . 2_656 ? O2 Fe1 O1 88.88(8) 2_656 2_656 ? O3 Fe1 O1 95.76(8) 2_656 2_656 ? O3 Fe1 O1 99.81(8) . 2_656 ? O2 Fe1 O1 88.88(8) . . ? O2 Fe1 O1 166.56(8) 2_656 . ? O3 Fe1 O1 99.81(8) 2_656 . ? O3 Fe1 O1 95.76(8) . . ? O1 Fe1 O1 79.11(12) 2_656 . ? C1 O1 Fe1 116.68(19) . . ? C2 O2 Fe1 116.32(17) . . ? C3 O3 Fe1 115.30(17) . . ? O4 C1 O1 126.1(3) . . ? O4 C1 C1 120.4(2) . 2_656 ? O1 C1 C1 113.47(17) . 2_656 ? O5 C2 O2 126.5(3) . . ? O5 C2 C3 120.1(2) . 2_656 ? O2 C2 C3 113.4(2) . 2_656 ? O6 C3 O3 126.2(3) . . ? O6 C3 C2 119.8(3) . 2_656 ? O3 C3 C2 114.0(2) . 2_656 ? Cl31 Cl31 C31 85.4(7) 2_556 . ? Cl31 Cl31 C31 67.2(6) 2_556 2_556 ? C32 Cl32 C35 51.2(6) . 2_556 ? C31 Cl32 C35 78.0(5) 2_556 2_556 ? C33 C32 C31 120.0 . . ? C33 C32 Cl32 120.4(6) . . ? C31 C32 Cl32 119.5(6) . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 Cl32 139.2(4) . 2_556 ? C35 C36 C31 120.0 . . ? C31 C31 C32 114.5(9) 2_556 2_556 ? C31 C31 C36 152.7(12) 2_556 . ? C32 C31 C32 80.3(8) 2_556 . ? C36 C31 C32 120.0 . . ? C31 C31 Cl31 87.3(7) 2_556 . ? C32 C31 Cl31 156.7(18) 2_556 . ? C36 C31 Cl31 119.3(6) . . ? C32 C31 Cl31 120.7(6) . . ? C32 C31 Cl31 170(3) 2_556 2_556 ? C36 C31 Cl31 134.1(5) . 2_556 ? C32 C31 Cl31 101.3(5) . 2_556 ? C31 C31 Cl32 167(2) 2_556 2_556 ? C32 C31 Cl32 141.9(5) . 2_556 ? Cl31 C31 Cl32 97.0(7) . 2_556 ? Cl31 C31 Cl32 112.0(6) 2_556 2_556 ? N41 N41 C47 85.4 2_556 . ? N41 N41 C47 71.7(7) 2_556 2_556 ? C47 C47 N41 94.5 2_556 . ? C47 C47 N41 71.7(7) 2_556 2_556 ? C47 C47 C41 84.2 2_556 . ? N41 C47 C41 178.59(9) . . ? N41 C47 C41 155.9(7) 2_556 . ? C42 C41 C42 120.62(19) 2_556 . ? C42 C41 C47 122.2(4) 2_556 . ? C42 C41 C47 116.9 . . ? C42 C41 C47 116.9(6) 2_556 2_556 ? C42 C41 C47 122.2(6) . 2_556 ? C43 C42 C41 118.4(4) . . ? C44 C43 C42 120.6(5) . . ? C43 C44 C43 121.3(6) 2_556 . ? # Attachment '- VIIa.cif' data_pseudo-kappa-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.88(DCB)0.12-(VIIa) _database_code_depnum_ccdc_archive 'CCDC 771735' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, 0.88(C7 H5 N), 0.12(C6 H4 Cl2), H3 O' _chemical_formula_sum 'C52.88 H39.88 Cl0.24 Fe N0.88 O13 S32' _chemical_formula_weight 1985.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bcn' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 10.4247(7) _cell_length_b 19.6843(17) _cell_length_c 36.096(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7407.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2898 _cell_measurement_theta_min 12.5176 _cell_measurement_theta_max 53.2276 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4038 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62687 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 73766 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.0947 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 29.81 _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.599 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.070 _reflns_number_total 9743 _reflns_number_gt 4926 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0501P)^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 9743 _refine_ls_number_parameters 448 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 S11 S 0.22783(8) 0.51913(4) 0.53337(2) 0.0511(2) Uani 1 1 d . . . S12 S 0.02854(8) 0.42651(4) 0.55894(2) 0.0456(2) Uani 1 1 d . . . S13 S 0.21636(8) 0.45570(4) 0.45311(2) 0.0479(2) Uani 1 1 d . . . S14 S 0.01714(8) 0.36062(4) 0.47552(2) 0.0500(2) Uani 1 1 d . . . S15 S 0.26753(10) 0.58643(5) 0.60433(3) 0.0686(3) Uani 1 1 d . . . S16 S 0.03654(9) 0.47757(5) 0.63711(2) 0.0545(2) Uani 1 1 d . . . S17 S 0.24431(9) 0.40362(5) 0.37766(2) 0.0605(3) Uani 1 1 d . . . S18 S -0.00322(9) 0.29185(5) 0.40375(3) 0.0649(3) Uani 1 1 d . . . C11 C 0.1222(3) 0.45486(15) 0.52272(8) 0.0431(7) Uani 1 1 d . . . C12 C 0.1175(3) 0.42614(15) 0.48805(8) 0.0439(7) Uani 1 1 d . . . C13 C 0.1834(3) 0.52536(15) 0.57961(8) 0.0445(8) Uani 1 1 d . . . C14 C 0.0905(3) 0.48303(15) 0.59134(8) 0.0434(8) Uani 1 1 d . . . C15 C 0.1647(3) 0.39780(16) 0.41993(8) 0.0456(8) Uani 1 1 d . . . C16 C 0.0714(3) 0.35508(16) 0.42996(8) 0.0469(8) Uani 1 1 d . . . C17 C 0.2352(5) 0.5669(3) 0.65143(11) 0.1095(17) Uani 1 1 d . . . H17A H 0.3136 0.5738 0.6654 0.131 Uiso 1 1 calc R . . H17B H 0.1728 0.5994 0.6605 0.131 Uiso 1 1 calc R . . C18 C 0.1872(4) 0.4983(2) 0.65965(10) 0.0858(13) Uani 1 1 d . . . H18A H 0.1762 0.4940 0.6862 0.103 Uiso 1 1 calc R . . H18B H 0.2514 0.4654 0.6521 0.103 Uiso 1 1 calc R . . C19 C 0.1487(4) 0.3501(2) 0.34884(10) 0.0798(12) Uani 1 1 d . . . H19A H 0.0734 0.3756 0.3413 0.096 Uiso 1 1 calc R . . H19B H 0.1974 0.3399 0.3266 0.096 Uiso 1 1 calc R . . C20 C 0.1069(5) 0.2876(2) 0.36466(11) 0.0903(14) Uani 1 1 d . . . H20A H 0.1824 0.2626 0.3725 0.108 Uiso 1 1 calc R . . H20B H 0.0661 0.2612 0.3453 0.108 Uiso 1 1 calc R . . S21 S 0.21138(9) 0.26515(4) 0.54254(2) 0.0554(2) Uani 1 1 d . . . S22 S -0.01633(8) 0.18378(5) 0.56237(2) 0.0539(2) Uani 1 1 d . . . S23 S 0.22423(9) 0.19731(4) 0.46317(2) 0.0540(2) Uani 1 1 d . . . S24 S -0.00603(8) 0.11446(5) 0.47950(2) 0.0559(2) Uani 1 1 d . . . S25 S 0.25286(9) 0.32089(5) 0.61686(2) 0.0567(2) Uani 1 1 d . . . S26 S -0.01043(9) 0.21785(5) 0.64173(2) 0.0586(2) Uani 1 1 d . . . S27 S 0.28041(9) 0.12744(6) 0.39274(3) 0.0682(3) Uani 1 1 d . . . S28 S 0.02046(9) 0.03295(5) 0.40999(3) 0.0645(3) Uani 1 1 d . . . C21 C 0.1022(3) 0.20263(16) 0.52935(9) 0.0500(8) Uani 1 1 d . . . C22 C 0.1068(3) 0.17351(16) 0.49565(8) 0.0479(8) Uani 1 1 d . . . C23 C 0.1617(3) 0.26652(16) 0.58901(8) 0.0448(8) Uani 1 1 d . . . C24 C 0.0595(3) 0.22901(16) 0.59829(8) 0.0453(8) Uani 1 1 d . . . C25 C 0.1845(3) 0.13181(16) 0.43188(8) 0.0450(8) Uani 1 1 d . . . C26 C 0.0822(3) 0.09473(16) 0.43949(8) 0.0462(8) Uani 1 1 d . . . C27 C 0.2026(4) 0.2946(2) 0.66166(9) 0.0795(13) Uani 1 1 d . . . H27A H 0.2433 0.2515 0.6673 0.095 Uiso 1 1 calc R . . H27B H 0.2329 0.3275 0.6796 0.095 Uiso 1 1 calc R . . C28 C 0.0616(4) 0.2867(2) 0.66622(10) 0.0787(12) Uani 1 1 d . . . H28A H 0.0207 0.3285 0.6583 0.094 Uiso 1 1 calc R . . H28B H 0.0434 0.2810 0.6924 0.094 Uiso 1 1 calc R . . C29 C 0.1788(4) 0.0928(2) 0.35708(9) 0.0800(12) Uani 1 1 d . . . H29A H 0.1785 0.1244 0.3364 0.096 Uiso 1 1 calc R . . H29B H 0.2174 0.0509 0.3484 0.096 Uiso 1 1 calc R . . C30 C 0.0469(4) 0.0786(3) 0.36693(10) 0.0929(15) Uani 1 1 d . . . H30A H 0.0086 0.0526 0.3470 0.112 Uiso 1 1 calc R . . H30B H 0.0012 0.1215 0.3683 0.112 Uiso 1 1 calc R . . Fe1 Fe 0.5000 0.29880(3) 0.7500 0.04256(17) Uani 1 2 d S . . O1 O 0.4429(2) 0.37571(11) 0.71805(5) 0.0521(6) Uani 1 1 d . . . O2 O 0.4146(2) 0.22702(11) 0.71918(5) 0.0495(5) Uani 1 1 d . . . O3 O 0.6639(2) 0.28905(11) 0.72107(5) 0.0527(6) Uani 1 1 d . . . O4 O 0.4423(3) 0.48765(13) 0.71526(7) 0.0872(9) Uani 1 1 d . . . O5 O 0.2518(3) 0.15524(14) 0.72153(7) 0.0860(9) Uani 1 1 d . . . O6 O 0.8432(2) 0.22835(14) 0.71970(7) 0.0775(8) Uani 1 1 d . . . C1 C 0.4678(3) 0.4345(2) 0.73063(9) 0.0537(9) Uani 1 1 d . . . C2 C 0.3113(3) 0.20336(17) 0.73296(9) 0.0496(8) Uani 1 1 d . . . C3 C 0.7398(3) 0.24253(18) 0.73286(9) 0.0489(8) Uani 1 1 d . . . Cl31 Cl 0.3607(15) -0.1206(8) 0.7653(5) 0.0730(8) Uiso 0.0612(15) 1 d PD A 1 Cl32 Cl 0.306(2) 0.0315(9) 0.7803(8) 0.0730(8) Uiso 0.0612(15) 1 d PD A 1 C31 C 0.473(2) -0.0610(9) 0.7560(9) 0.0730(8) Uiso 0.0612(15) 1 d PGD A 1 C32 C 0.442(3) 0.0075(8) 0.7585(9) 0.0730(8) Uiso 0.0612(15) 1 d PGD A 1 C33 C 0.528(3) 0.0565(10) 0.7464(13) 0.0730(8) Uiso 0.0612(15) 1 d PGD A 1 H33 H 0.5074 0.1023 0.7480 0.088 Uiso 0.0612(15) 1 calc PR A 1 C34 C 0.646(3) 0.0370(14) 0.7318(11) 0.0730(8) Uiso 0.0612(15) 1 d PG A 1 H34 H 0.7039 0.0697 0.7236 0.088 Uiso 0.0612(15) 1 calc PR A 1 C35 C 0.678(2) -0.0315(15) 0.7293(13) 0.0730(8) Uiso 0.0612(15) 1 d PG A 1 H35 H 0.7563 -0.0446 0.7195 0.088 Uiso 0.0612(15) 1 calc PR A 1 C36 C 0.591(2) -0.0805(12) 0.7414(15) 0.0730(8) Uiso 0.0612(15) 1 d PGD A 1 H36 H 0.6122 -0.1263 0.7398 0.088 Uiso 0.0612(15) 1 calc PR A 1 C47 C 0.2948(13) 0.0185(4) 0.7802(4) 0.0730(8) Uiso 0.4388(15) 1 d PD A 2 N41 N 0.2149(7) 0.0416(3) 0.79493(19) 0.0730(8) Uiso 0.4388(15) 1 d PD A 2 C41 C 0.5000 0.03020(15) 0.7500 0.0730(8) Uiso 0.878(3) 2 d SPGD A 2 H41 H 0.4909 0.0772 0.7505 0.088 Uiso 0.4388(15) 1 calc PR A 2 C42 C 0.6126(2) 0.0004(2) 0.73489(12) 0.0730(8) Uiso 0.4388(15) 1 d PG A 2 H42 H 0.6783 0.0277 0.7258 0.088 Uiso 0.4388(15) 1 calc PR A 2 C43 C 0.6238(5) -0.0700(2) 0.7339(2) 0.0730(8) Uiso 0.4388(15) 1 d PG A 2 H43 H 0.6968 -0.0899 0.7238 0.088 Uiso 0.4388(15) 1 calc PR A 2 C44 C 0.5258(6) -0.11048(16) 0.7478(3) 0.0730(8) Uiso 0.4388(15) 1 d PG A 2 H44 H 0.5332 -0.1575 0.7471 0.088 Uiso 0.4388(15) 1 calc PR A 2 C45 C 0.4166(5) -0.08064(15) 0.7627(2) 0.0730(8) Uiso 0.4388(15) 1 d PGD A 2 H45 H 0.3510 -0.1077 0.7721 0.088 Uiso 0.4388(15) 1 calc PR A 2 C46 C 0.4054(2) -0.01030(16) 0.76378(12) 0.0730(8) Uiso 0.4388(15) 1 d PG A 2 H51A H 0.5000 0.5579(18) 0.7500 0.109 Uiso 1 2 d SD . . O51 O 0.5027(9) 0.61756(19) 0.74384(19) 0.0677(15) Uiso 0.50 1 d PD . . H51B H 0.595(3) 0.6470(11) 0.7554(10) 0.102 Uiso 1 1 d 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 S11 0.0474(5) 0.0535(5) 0.0523(5) -0.0038(4) 0.0062(4) -0.0079(4) S12 0.0532(5) 0.0439(5) 0.0396(4) 0.0026(3) 0.0032(4) -0.0061(4) S13 0.0492(5) 0.0532(5) 0.0412(4) -0.0050(4) 0.0047(4) -0.0053(4) S14 0.0539(5) 0.0480(5) 0.0480(5) 0.0022(4) -0.0007(4) -0.0064(4) S15 0.0641(6) 0.0590(6) 0.0828(7) -0.0234(5) 0.0035(5) -0.0154(5) S16 0.0578(6) 0.0643(6) 0.0413(5) -0.0043(4) 0.0052(4) 0.0034(5) S17 0.0632(6) 0.0733(6) 0.0449(5) -0.0118(4) 0.0088(4) -0.0006(5) S18 0.0616(6) 0.0631(6) 0.0701(6) -0.0191(5) -0.0082(5) -0.0071(5) C11 0.0434(18) 0.0408(18) 0.0452(18) 0.0035(14) 0.0035(15) 0.0025(15) C12 0.0408(18) 0.0499(19) 0.0410(18) 0.0040(14) -0.0014(15) 0.0041(15) C13 0.0409(18) 0.0410(18) 0.0516(19) -0.0076(15) 0.0001(16) 0.0031(16) C14 0.0444(19) 0.0429(18) 0.0431(18) -0.0054(14) -0.0030(15) 0.0091(16) C15 0.0460(19) 0.0492(19) 0.0415(18) -0.0051(15) -0.0059(16) 0.0045(17) C16 0.0441(19) 0.049(2) 0.0479(19) -0.0041(15) -0.0064(16) 0.0029(17) C17 0.124(4) 0.132(4) 0.072(3) -0.048(3) 0.008(3) -0.047(4) C18 0.086(3) 0.108(4) 0.063(3) -0.001(2) -0.025(2) -0.020(3) C19 0.086(3) 0.094(3) 0.060(2) -0.025(2) 0.004(2) -0.015(3) C20 0.124(4) 0.077(3) 0.070(3) -0.027(2) -0.006(3) 0.004(3) S21 0.0586(6) 0.0582(6) 0.0493(5) -0.0041(4) 0.0000(4) -0.0092(5) S22 0.0468(5) 0.0716(6) 0.0433(5) -0.0047(4) -0.0040(4) -0.0068(4) S23 0.0535(5) 0.0571(6) 0.0513(5) -0.0021(4) 0.0030(4) -0.0090(4) S24 0.0475(5) 0.0717(6) 0.0485(5) -0.0113(4) 0.0065(4) -0.0128(5) S25 0.0516(5) 0.0580(6) 0.0605(6) -0.0191(4) -0.0011(5) -0.0033(4) S26 0.0615(6) 0.0688(6) 0.0455(5) -0.0047(4) 0.0031(4) -0.0092(5) S27 0.0508(6) 0.1071(8) 0.0468(5) -0.0003(5) 0.0075(4) 0.0085(5) S28 0.0574(6) 0.0777(7) 0.0583(6) -0.0195(5) -0.0019(5) -0.0091(5) C21 0.0473(19) 0.051(2) 0.052(2) -0.0007(15) -0.0043(17) 0.0040(16) C22 0.0432(18) 0.055(2) 0.0454(19) 0.0004(15) 0.0047(16) 0.0024(16) C23 0.0469(19) 0.0449(19) 0.0427(18) -0.0093(14) -0.0028(16) 0.0048(17) C24 0.0444(19) 0.0482(19) 0.0434(18) -0.0094(15) -0.0056(15) 0.0041(17) C25 0.0417(19) 0.055(2) 0.0383(17) 0.0009(14) -0.0028(15) 0.0037(16) C26 0.0441(19) 0.055(2) 0.0393(18) -0.0060(15) -0.0025(15) -0.0012(17) C27 0.103(4) 0.081(3) 0.054(2) 0.0035(19) -0.027(2) -0.029(3) C28 0.098(3) 0.087(3) 0.051(2) -0.022(2) 0.017(2) -0.021(3) C29 0.103(4) 0.093(3) 0.043(2) -0.003(2) -0.006(2) 0.004(3) C30 0.068(3) 0.167(5) 0.044(2) -0.007(3) -0.012(2) 0.026(3) Fe1 0.0425(4) 0.0502(4) 0.0349(3) 0.000 0.0009(3) 0.000 O1 0.0620(15) 0.0510(14) 0.0433(13) 0.0019(10) -0.0101(11) 0.0035(12) O2 0.0476(13) 0.0632(14) 0.0377(12) -0.0093(10) 0.0046(11) -0.0038(12) O3 0.0491(13) 0.0611(15) 0.0478(13) 0.0105(11) 0.0115(11) 0.0017(12) O4 0.136(3) 0.0587(18) 0.0674(17) 0.0007(13) -0.0350(17) 0.0136(17) O5 0.091(2) 0.086(2) 0.0810(19) -0.0290(16) 0.0225(16) -0.0384(17) O6 0.0517(16) 0.102(2) 0.0788(17) 0.0190(15) 0.0228(14) 0.0210(15) C1 0.060(2) 0.053(2) 0.0482(19) 0.0046(18) -0.0057(17) 0.0100(19) C2 0.054(2) 0.049(2) 0.0452(19) -0.0006(16) -0.0029(18) -0.0053(18) C3 0.043(2) 0.061(2) 0.0425(18) -0.0065(17) -0.0007(17) -0.0011(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.720(3) . ? S11 C13 1.736(3) . ? S12 C11 1.725(3) . ? S12 C14 1.739(3) . ? S13 C12 1.730(3) . ? S13 C15 1.739(3) . ? S14 C12 1.721(3) . ? S14 C16 1.742(3) . ? S15 C13 1.735(3) . ? S15 C17 1.775(4) . ? S16 C14 1.748(3) . ? S16 C18 1.815(4) . ? S17 C15 1.741(3) . ? S17 C19 1.785(4) . ? S18 C16 1.747(3) . ? S18 C20 1.821(4) . ? C11 C12 1.374(4) . ? C13 C14 1.346(4) . ? C15 C16 1.335(4) . ? C17 C18 1.471(6) . ? C19 C20 1.426(5) . ? S21 C21 1.743(3) . ? S21 C23 1.756(3) . ? S22 C21 1.756(3) . ? S22 C24 1.760(3) . ? S23 C22 1.758(3) . ? S23 C25 1.763(3) . ? S24 C26 1.755(3) . ? S24 C22 1.753(3) . ? S25 C23 1.749(3) . ? S25 C27 1.777(4) . ? S26 C24 1.743(3) . ? S26 C28 1.783(4) . ? S27 C25 1.733(3) . ? S27 C29 1.801(4) . ? S28 C26 1.740(3) . ? S28 C30 1.817(4) . ? C21 C22 1.346(4) . ? C23 C24 1.339(4) . ? C25 C26 1.321(4) . ? C27 C28 1.488(6) . ? C29 C30 1.447(5) . ? Fe1 O1 1.994(2) 4_656 ? Fe1 O1 1.994(2) . ? Fe1 O2 2.007(2) . ? Fe1 O2 2.007(2) 4_656 ? Fe1 O3 2.012(2) . ? Fe1 O3 2.012(2) 4_656 ? O1 C1 1.269(4) . ? O2 C2 1.275(4) . ? O3 C3 1.283(4) . ? O4 C1 1.214(4) . ? O5 C2 1.205(4) . ? O6 C3 1.210(4) . ? C1 C1 1.551(6) 4_656 ? C2 C3 1.549(5) 4_656 ? C3 C2 1.549(5) 4_656 ? Cl31 C31 1.69(2) . ? Cl32 C32 1.69(2) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C47 N41 1.086(14) . ? C47 C46 1.416(14) . ? C41 C42 1.4216 . ? C41 C46 1.3618 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 S11 C13 95.52(15) . . ? C11 S12 C14 95.31(15) . . ? C12 S13 C15 95.57(15) . . ? C12 S14 C16 95.60(15) . . ? C13 S15 C17 104.29(19) . . ? C14 S16 C18 97.54(18) . . ? C15 S17 C19 101.88(18) . . ? C16 S18 C20 99.90(18) . . ? C12 C11 S11 122.0(2) . . ? C12 C11 S12 122.5(2) . . ? S11 C11 S12 115.52(17) . . ? C11 C12 S14 124.7(2) . . ? C11 C12 S13 120.3(2) . . ? S14 C12 S13 114.99(17) . . ? C14 C13 S11 116.8(2) . . ? C14 C13 S15 129.1(2) . . ? S11 C13 S15 114.10(18) . . ? C13 C14 S12 116.9(2) . . ? C13 C14 S16 124.5(2) . . ? S12 C14 S16 118.47(19) . . ? C16 C15 S13 116.9(2) . . ? C16 C15 S17 128.8(2) . . ? S13 C15 S17 114.37(19) . . ? C15 C16 S14 116.9(2) . . ? C15 C16 S18 128.8(2) . . ? S14 C16 S18 114.28(19) . . ? C18 C17 S15 117.1(3) . . ? C17 C18 S16 114.2(3) . . ? C20 C19 S17 116.5(3) . . ? C19 C20 S18 117.6(3) . . ? C21 S21 C23 94.53(15) . . ? C21 S22 C24 94.44(15) . . ? C22 S23 C25 93.93(15) . . ? C26 S24 C22 93.94(15) . . ? C23 S25 C27 100.63(17) . . ? C24 S26 C28 100.04(17) . . ? C25 S27 C29 105.19(18) . . ? C26 S28 C30 96.98(19) . . ? C22 C21 S21 121.6(3) . . ? C22 C21 S22 123.3(3) . . ? S21 C21 S22 115.05(18) . . ? C21 C22 S23 120.9(3) . . ? C21 C22 S24 124.0(3) . . ? S23 C22 S24 114.96(17) . . ? C24 C23 S25 128.7(2) . . ? C24 C23 S21 117.7(2) . . ? S25 C23 S21 113.48(19) . . ? C23 C24 S26 128.8(2) . . ? C23 C24 S22 116.9(2) . . ? S26 C24 S22 114.29(19) . . ? C26 C25 S27 127.4(2) . . ? C26 C25 S23 117.4(2) . . ? S27 C25 S23 115.01(19) . . ? C25 C26 S28 123.9(2) . . ? C25 C26 S24 118.1(2) . . ? S28 C26 S24 117.67(19) . . ? C28 C27 S25 115.0(3) . . ? C27 C28 S26 116.1(3) . . ? C30 C29 S27 117.2(3) . . ? C29 C30 S28 116.7(3) . . ? O1 Fe1 O1 81.20(13) 4_656 . ? O1 Fe1 O2 170.99(9) 4_656 . ? O1 Fe1 O2 94.68(9) . . ? O1 Fe1 O2 94.68(9) 4_656 4_656 ? O1 Fe1 O2 170.99(9) . 4_656 ? O2 Fe1 O2 90.47(12) . 4_656 ? O1 Fe1 O3 96.85(9) 4_656 . ? O1 Fe1 O3 91.47(9) . . ? O2 Fe1 O3 91.24(9) . . ? O2 Fe1 O3 81.03(9) 4_656 . ? O1 Fe1 O3 91.47(9) 4_656 4_656 ? O1 Fe1 O3 96.85(9) . 4_656 ? O2 Fe1 O3 81.03(9) . 4_656 ? O2 Fe1 O3 91.24(9) 4_656 4_656 ? O3 Fe1 O3 169.05(13) . 4_656 ? C1 O1 Fe1 115.1(2) . . ? C2 O2 Fe1 114.6(2) . . ? C3 O3 Fe1 114.8(2) . . ? O4 C1 O1 125.3(3) . . ? O4 C1 C1 120.4(2) . 4_656 ? O1 C1 C1 114.25(17) . 4_656 ? O5 C2 O2 126.1(3) . . ? O5 C2 C3 119.1(3) . 4_656 ? O2 C2 C3 114.8(3) . 4_656 ? O6 C3 O3 125.7(3) . . ? O6 C3 C2 120.3(3) . 4_656 ? O3 C3 C2 114.0(3) . 4_656 ? C32 C31 C36 120.0 . . ? C32 C31 Cl31 119.76(16) . . ? C36 C31 Cl31 119.71(17) . . ? C33 C32 C31 120.0 . . ? C33 C32 Cl32 119.83(16) . . ? C31 C32 Cl32 119.86(16) . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? N41 C47 C46 175.1(16) . . ? C42 C41 C46 119.7 . . ? C43 C42 C41 119.4 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.8 . . ? C45 C46 C47 118.61(8) . . ? C41 C46 C47 120.54(8) . . ? # Attachment '- X.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.35(CB)0.65-(X) _database_code_depnum_ccdc_archive 'CCDC 771736' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, 0.35(C7 H5 N), 0.65(C6 H5 Cl), H3 O' _chemical_formula_sum 'C52.35 H40 Cl0.65 Fe N0.35 O13 S32' _chemical_formula_weight 1986.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 10.2763(6) _cell_length_b 20.0670(10) _cell_length_c 35.369(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.915(6) _cell_angle_gamma 90.00 _cell_volume 7284.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_radiation CuK\a _cell_measurement_reflns_used 8138 _cell_measurement_theta_min 3.7509 _cell_measurement_theta_max 70.9421 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4038 _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63728 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 50869 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 31.68 _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.946 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.075 _reflns_number_total 11242 _reflns_number_gt 8874 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0482P)^2^+11.7459P] 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 11242 _refine_ls_number_parameters 484 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _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 S11 S 0.42214(5) 0.21374(3) 0.508284(14) 0.02943(11) Uani 1 1 d . . . S12 S 0.66487(5) 0.14324(3) 0.531331(14) 0.02759(10) Uani 1 1 d . . . S13 S 0.54107(5) 0.24611(3) 0.426537(14) 0.02933(11) Uani 1 1 d . . . S14 S 0.78052(5) 0.17409(3) 0.450844(14) 0.02836(10) Uani 1 1 d . . . S15 S 0.29496(5) 0.19242(3) 0.579630(16) 0.03404(12) Uani 1 1 d . . . S16 S 0.58809(5) 0.11043(3) 0.608650(15) 0.03188(11) Uani 1 1 d . . . S17 S 0.61890(6) 0.27495(3) 0.349549(16) 0.04190(14) Uani 1 1 d . . . S18 S 0.91007(5) 0.19420(3) 0.379202(17) 0.03639(12) Uani 1 1 d . . . C11 C 0.57630(18) 0.18791(9) 0.49630(5) 0.0242(4) Uani 1 1 d . . . C12 C 0.62651(18) 0.20127(9) 0.46207(5) 0.0235(3) Uani 1 1 d . . . C13 C 0.43373(18) 0.17948(10) 0.55408(5) 0.0246(4) Uani 1 1 d . . . C14 C 0.54580(18) 0.14730(9) 0.56473(5) 0.0237(3) Uani 1 1 d . . . C15 C 0.6625(2) 0.24055(10) 0.39392(5) 0.0271(4) Uani 1 1 d . . . C16 C 0.77381(19) 0.20856(10) 0.40535(5) 0.0258(4) Uani 1 1 d . . . C17 C 0.3531(2) 0.16908(11) 0.62725(6) 0.0325(4) Uani 1 1 d . . . H17A H 0.4071 0.2048 0.6378 0.039 Uiso 1 1 calc R . . H17B H 0.2788 0.1644 0.6429 0.039 Uiso 1 1 calc R . . C18 C 0.4312(2) 0.10457(10) 0.62908(6) 0.0305(4) Uani 1 1 d . . . H18A H 0.3809 0.0699 0.6160 0.037 Uiso 1 1 calc R . . H18B H 0.4441 0.0912 0.6554 0.037 Uiso 1 1 calc R . . C19 C 0.7643(3) 0.26208(15) 0.32373(7) 0.0492(6) Uani 1 1 d . . . H19A H 0.7411 0.2642 0.2968 0.059 Uiso 1 1 calc R . . H19B H 0.8247 0.2982 0.3296 0.059 Uiso 1 1 calc R . . C20 C 0.8328(3) 0.19632(14) 0.33225(7) 0.0483(6) Uani 1 1 d . . . H20A H 0.8981 0.1890 0.3138 0.058 Uiso 1 1 calc R . . H20B H 0.7698 0.1604 0.3297 0.058 Uiso 1 1 calc R . . S21 S 0.02556(5) 0.08803(3) 0.519382(14) 0.02890(11) Uani 1 1 d . . . S22 S 0.25958(5) 0.01163(3) 0.544125(13) 0.02733(10) Uani 1 1 d . . . S23 S 0.14774(5) 0.11774(3) 0.439426(13) 0.02869(11) Uani 1 1 d . . . S24 S 0.38456(5) 0.04298(3) 0.463499(14) 0.02723(10) Uani 1 1 d . . . S25 S -0.10898(5) 0.07005(3) 0.589642(17) 0.04186(15) Uani 1 1 d . . . S26 S 0.17233(5) -0.01794(3) 0.621030(15) 0.03428(12) Uani 1 1 d . . . S27 S 0.24294(6) 0.15855(3) 0.365091(15) 0.03776(13) Uani 1 1 d . . . S28 S 0.52105(5) 0.07310(3) 0.393450(15) 0.03091(11) Uani 1 1 d . . . C21 C 0.17946(18) 0.05941(10) 0.50900(5) 0.0242(4) Uani 1 1 d . . . C22 C 0.23229(17) 0.07260(9) 0.47497(5) 0.0235(4) Uani 1 1 d . . . C23 C 0.02968(18) 0.05374(10) 0.56491(5) 0.0257(4) Uani 1 1 d . A . C24 C 0.13763(18) 0.01891(10) 0.57664(5) 0.0242(4) Uani 1 1 d . A . C25 C 0.27492(19) 0.11803(10) 0.40833(5) 0.0254(4) Uani 1 1 d . B . C26 C 0.38423(18) 0.08407(9) 0.41982(5) 0.0235(3) Uani 1 1 d . B . C27A C -0.0456(4) 0.0533(2) 0.63837(12) 0.0352(9) Uani 0.74 1 d P A 1 H27A H 0.0170 0.0876 0.6459 0.042 Uiso 0.74 1 calc PR A 1 H27B H -0.1169 0.0556 0.6553 0.042 Uiso 0.74 1 calc PR A 1 C28A C 0.0194(3) -0.01449(15) 0.64254(8) 0.0304(6) Uani 0.74 1 d P A 1 H28A H -0.0380 -0.0481 0.6311 0.036 Uiso 0.74 1 calc PR A 1 H28B H 0.0324 -0.0249 0.6692 0.036 Uiso 0.74 1 calc PR A 1 C27B C -0.0850(11) 0.0311(7) 0.6321(4) 0.036(3) Uani 0.26 1 d P A 2 H27C H -0.1403 0.0516 0.6502 0.043 Uiso 0.26 1 calc PR A 2 H27D H -0.1108 -0.0152 0.6293 0.043 Uiso 0.26 1 calc PR A 2 C28B C 0.0555(9) 0.0342(5) 0.6474(2) 0.0365(18) Uani 0.26 1 d P A 2 H28C H 0.0591 0.0199 0.6737 0.044 Uiso 0.26 1 calc PR A 2 H28D H 0.0843 0.0802 0.6469 0.044 Uiso 0.26 1 calc PR A 2 C29A C 0.3630(4) 0.1276(2) 0.33444(10) 0.0344(7) Uani 0.75 1 d P B 1 H29A H 0.3210 0.1199 0.3096 0.041 Uiso 0.75 1 calc PR B 1 H29B H 0.4280 0.1620 0.3316 0.041 Uiso 0.75 1 calc PR B 1 C30A C 0.4322(3) 0.06416(17) 0.34708(8) 0.0332(6) Uani 0.75 1 d P B 1 H30A H 0.4932 0.0516 0.3283 0.040 Uiso 0.75 1 calc PR B 1 H30B H 0.3687 0.0286 0.3486 0.040 Uiso 0.75 1 calc PR B 1 C29B C 0.3366(11) 0.0977(6) 0.3379(3) 0.038(2) Uani 0.25 1 d P B 2 H29C H 0.3022 0.0535 0.3422 0.045 Uiso 0.25 1 calc PR B 2 H29D H 0.3226 0.1075 0.3111 0.045 Uiso 0.25 1 calc PR B 2 C30B C 0.4811(10) 0.0970(5) 0.3475(2) 0.0336(18) Uani 0.25 1 d P B 2 H30C H 0.5157 0.1412 0.3434 0.040 Uiso 0.25 1 calc PR B 2 H30D H 0.5224 0.0667 0.3304 0.040 Uiso 0.25 1 calc PR B 2 Fe1 Fe 0.5000 0.08106(2) 0.7500 0.03032(10) Uani 1 2 d S . . O1 O 0.42602(17) 0.15859(8) 0.71907(4) 0.0409(4) Uani 1 1 d . . . O2 O 0.39598(15) 0.01697(8) 0.71657(4) 0.0363(3) Uani 1 1 d . . . O3 O 0.64981(16) 0.06470(8) 0.71693(4) 0.0363(3) Uani 1 1 d . . . O4 O 0.4111(2) 0.27011(9) 0.71862(6) 0.0536(5) Uani 1 1 d . . . O5 O 0.21742(17) -0.04672(9) 0.71476(5) 0.0448(4) Uani 1 1 d . . . O6 O 0.81959(19) -0.00402(10) 0.71150(5) 0.0506(5) Uani 1 1 d . . . C1 C 0.4524(2) 0.21690(12) 0.73197(7) 0.0385(5) Uani 1 1 d . . . C2 C 0.2937(2) -0.00696(11) 0.73044(6) 0.0323(4) Uani 1 1 d . . . C3 C 0.7302(2) 0.01946(11) 0.72875(6) 0.0330(4) Uani 1 1 d . . . Cl31 Cl 0.0238(2) 0.34815(9) 0.75367(6) 0.0409(5) Uiso 0.326(3) 1 d P . 1 C31 C 0.0141(7) 0.2640(2) 0.7485(2) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 C32 C -0.0804(6) 0.2254(3) 0.7648(2) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H32 H -0.1452 0.2456 0.7782 0.049 Uiso 0.326(3) 1 calc PR . 1 C33 C -0.0782(5) 0.1565(3) 0.76101(18) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H33 H -0.1414 0.1306 0.7719 0.049 Uiso 0.326(3) 1 calc PR . 1 C34 C 0.0186(5) 0.1262(2) 0.74098(17) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H34 H 0.0202 0.0801 0.7385 0.049 Uiso 0.326(3) 1 calc PR . 1 C35 C 0.1132(5) 0.1648(3) 0.72473(16) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H35 H 0.1779 0.1446 0.7113 0.049 Uiso 0.326(3) 1 calc PR . 1 C36 C 0.1109(6) 0.2338(3) 0.7285(2) 0.0409(5) Uiso 0.326(3) 1 d PG . 1 H36 H 0.1741 0.2596 0.7176 0.049 Uiso 0.326(3) 1 calc PR . 1 N41 N 0.0000 0.3726(7) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 C45 C 0.0000 0.3230(8) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 C41 C 0.0000 0.2489(5) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 C42 C 0.0953(8) 0.2151(4) 0.7296(2) 0.0409(5) Uiso 0.348(7) 1 d P . 2 H42 H 0.1573 0.2384 0.7166 0.049 Uiso 0.348(7) 1 calc PR . 2 C43 C 0.0922(8) 0.1474(4) 0.7297(2) 0.0409(5) Uiso 0.348(7) 1 d P . 2 H43 H 0.1519 0.1236 0.7162 0.049 Uiso 0.348(7) 1 calc PR . 2 C44 C 0.0000 0.1135(6) 0.7500 0.0409(5) Uiso 0.348(7) 2 d SP . 2 H44 H 0.0000 0.0672 0.7500 0.049 Uiso 0.348(7) 2 calc SPR . 2 O51 O 0.0101(6) -0.09987(14) 0.75499(15) 0.0464(9) Uiso 0.50 1 d PD . . H51A H 0.046(4) -0.151(2) 0.7674(16) 0.070 Uiso 0.50 1 d PD . . H51B H 0.090(4) -0.059(2) 0.7621(18) 0.070 Uiso 0.50 1 d PD . . H51C H -0.086(5) -0.084(2) 0.7689(18) 0.070 Uiso 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 S11 0.0249(2) 0.0382(3) 0.0253(2) 0.0037(2) 0.00228(18) 0.00720(19) S12 0.0233(2) 0.0363(3) 0.0234(2) 0.00607(19) 0.00412(17) 0.00582(18) S13 0.0259(2) 0.0366(3) 0.0253(2) 0.00447(19) 0.00048(18) 0.00661(19) S14 0.0244(2) 0.0341(2) 0.0268(2) 0.00516(19) 0.00274(17) 0.00553(18) S15 0.0259(2) 0.0443(3) 0.0326(3) 0.0024(2) 0.00790(19) 0.0081(2) S16 0.0282(2) 0.0413(3) 0.0265(2) 0.0099(2) 0.00501(19) 0.0054(2) S17 0.0519(3) 0.0502(3) 0.0231(3) 0.0079(2) -0.0027(2) 0.0039(3) S18 0.0353(3) 0.0363(3) 0.0390(3) 0.0019(2) 0.0163(2) 0.0017(2) C11 0.0232(8) 0.0277(9) 0.0216(9) 0.0003(7) 0.0008(7) 0.0014(7) C12 0.0228(8) 0.0266(9) 0.0210(8) 0.0017(7) 0.0009(7) 0.0024(7) C13 0.0253(9) 0.0280(9) 0.0209(8) 0.0001(7) 0.0050(7) 0.0003(7) C14 0.0251(8) 0.0268(9) 0.0192(8) 0.0024(7) 0.0026(7) 0.0001(7) C15 0.0327(10) 0.0286(9) 0.0200(9) 0.0011(7) 0.0014(7) -0.0005(8) C16 0.0274(9) 0.0261(9) 0.0243(9) 0.0010(7) 0.0058(7) -0.0008(7) C17 0.0341(10) 0.0359(11) 0.0284(10) -0.0006(8) 0.0100(8) 0.0030(8) C18 0.0302(10) 0.0321(10) 0.0300(10) 0.0037(8) 0.0097(8) -0.0012(8) C19 0.0509(14) 0.0734(18) 0.0233(11) 0.0065(11) 0.0025(10) -0.0170(13) C20 0.0563(15) 0.0565(16) 0.0337(13) -0.0147(11) 0.0173(11) -0.0124(12) S21 0.0251(2) 0.0409(3) 0.0209(2) 0.00603(19) 0.00289(17) 0.00969(19) S22 0.0244(2) 0.0357(3) 0.0221(2) 0.00544(18) 0.00335(17) 0.00805(18) S23 0.0248(2) 0.0416(3) 0.0200(2) 0.00504(19) 0.00413(17) 0.01064(19) S24 0.0246(2) 0.0332(2) 0.0241(2) 0.00410(18) 0.00318(17) 0.00781(18) S25 0.0305(3) 0.0645(4) 0.0316(3) 0.0151(3) 0.0117(2) 0.0196(3) S26 0.0264(2) 0.0463(3) 0.0305(3) 0.0182(2) 0.00491(19) 0.0049(2) S27 0.0466(3) 0.0435(3) 0.0240(2) 0.0102(2) 0.0108(2) 0.0174(2) S28 0.0256(2) 0.0339(3) 0.0341(3) 0.0013(2) 0.01074(19) 0.00510(19) C21 0.0233(8) 0.0292(9) 0.0201(8) 0.0020(7) 0.0008(6) 0.0043(7) C22 0.0220(8) 0.0290(9) 0.0196(8) 0.0019(7) 0.0006(6) 0.0049(7) C23 0.0247(8) 0.0321(9) 0.0205(9) 0.0049(7) 0.0042(7) 0.0042(7) C24 0.0230(8) 0.0279(9) 0.0220(9) 0.0056(7) 0.0035(7) 0.0014(7) C25 0.0290(9) 0.0271(9) 0.0207(9) 0.0030(7) 0.0063(7) 0.0060(7) C26 0.0234(8) 0.0256(9) 0.0220(9) 0.0008(7) 0.0050(7) 0.0023(7) C27A 0.038(3) 0.045(2) 0.0226(17) 0.0038(16) 0.0059(16) 0.0108(16) C28A 0.0267(13) 0.0380(15) 0.0271(13) 0.0116(11) 0.0082(10) 0.0039(11) C27B 0.024(5) 0.055(8) 0.028(6) 0.015(5) 0.008(4) 0.009(4) C28B 0.039(5) 0.046(5) 0.025(4) 0.001(3) 0.003(3) 0.000(4) C29A 0.0356(17) 0.043(2) 0.0248(15) 0.0012(15) 0.0079(12) 0.0039(15) C30A 0.0390(16) 0.0340(16) 0.0274(14) -0.0060(12) 0.0081(12) 0.0065(13) C29B 0.050(6) 0.046(6) 0.018(4) -0.004(4) 0.011(4) -0.016(5) C30B 0.041(5) 0.035(5) 0.026(4) -0.002(4) 0.011(4) -0.001(4) Fe1 0.0370(2) 0.0329(2) 0.02130(19) 0.000 0.00394(16) 0.000 O1 0.0561(10) 0.0378(8) 0.0286(8) 0.0028(6) -0.0004(7) 0.0036(7) O2 0.0381(8) 0.0464(9) 0.0250(7) -0.0052(6) 0.0069(6) -0.0047(7) O3 0.0408(8) 0.0426(9) 0.0261(7) 0.0037(6) 0.0076(6) -0.0026(7) O4 0.0621(12) 0.0402(10) 0.0590(12) 0.0117(9) 0.0092(10) 0.0056(8) O5 0.0408(9) 0.0550(11) 0.0386(9) -0.0043(8) 0.0019(7) -0.0090(8) O6 0.0523(11) 0.0609(12) 0.0405(10) 0.0013(8) 0.0207(8) 0.0058(9) C1 0.0434(12) 0.0388(12) 0.0345(12) 0.0046(9) 0.0132(10) 0.0003(10) C2 0.0341(10) 0.0374(11) 0.0255(10) 0.0026(8) 0.0022(8) 0.0048(9) C3 0.0359(11) 0.0378(11) 0.0259(10) -0.0044(8) 0.0077(8) -0.0087(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.7396(19) . ? S11 C13 1.7582(19) . ? S12 C14 1.7454(19) . ? S12 C11 1.7471(19) . ? S13 C12 1.7458(19) . ? S13 C15 1.746(2) . ? S14 C12 1.7390(19) . ? S14 C16 1.750(2) . ? S15 C13 1.7460(19) . ? S15 C17 1.819(2) . ? S16 C14 1.7552(19) . ? S16 C18 1.803(2) . ? S17 C15 1.752(2) . ? S17 C19 1.809(3) . ? S18 C16 1.7410(19) . ? S18 C20 1.804(3) . ? C11 C12 1.367(3) . ? C13 C14 1.357(3) . ? C15 C16 1.355(3) . ? C17 C18 1.523(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.518(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? S21 C21 1.7392(19) . ? S21 C23 1.7497(19) . ? S22 C21 1.7427(19) . ? S22 C24 1.7496(19) . ? S23 C22 1.7449(19) . ? S23 C25 1.7504(19) . ? S24 C22 1.7410(18) . ? S24 C26 1.7509(19) . ? S25 C27B 1.700(12) . ? S25 C23 1.7405(19) . ? S25 C27A 1.842(4) . ? S26 C24 1.7554(19) . ? S26 C28A 1.782(3) . ? S26 C28B 1.876(9) . ? S27 C25 1.7485(19) . ? S27 C29A 1.794(3) . ? S27 C29B 1.855(12) . ? S28 C30B 1.724(9) . ? S28 C26 1.7403(18) . ? S28 C30A 1.845(3) . ? C21 C22 1.371(3) . ? C23 C24 1.358(3) . ? C25 C26 1.358(3) . ? C27A C28A 1.519(5) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C27B C28B 1.518(14) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29A C30A 1.514(5) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C29B C30B 1.506(15) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? Fe1 O3 2.0071(15) 2_656 ? Fe1 O3 2.0071(15) . ? Fe1 O2 2.0166(16) . ? Fe1 O2 2.0166(16) 2_656 ? Fe1 O1 2.0275(17) 2_656 ? Fe1 O1 2.0275(17) . ? O1 C1 1.280(3) . ? O2 C2 1.276(3) . ? O3 C3 1.283(3) . ? O4 C1 1.234(3) . ? O5 C2 1.231(3) . ? O6 C3 1.222(3) . ? C1 C1 1.568(5) 2_656 ? C2 C3 1.569(3) 2_656 ? C3 C2 1.569(3) 2_656 ? Cl31 Cl31 0.542(4) 2_556 ? Cl31 C31 1.700(5) . ? Cl31 C31 1.733(5) 2_556 ? C31 C31 0.313(12) 2_556 ? C31 C32 1.149(7) 2_556 ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 C36 1.669(9) 2_556 ? C31 Cl31 1.733(4) 2_556 ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N41 C45 1.00(2) . ? C45 C41 1.486(17) . ? C41 C42 1.419(8) 2_556 ? C41 C42 1.419(8) . ? C42 C43 1.359(10) . ? C42 H42 0.9300 . ? C43 C44 1.395(9) . ? C43 H43 0.9300 . ? C44 C43 1.395(9) 2_556 ? C44 H44 0.9300 . ? O51 H51A 1.17(3) . ? O51 H51B 1.17(4) . ? O51 H51C 1.17(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 C11 S11 C13 95.05(9) . . ? C14 S12 C11 95.63(9) . . ? C12 S13 C15 95.31(9) . . ? C12 S14 C16 95.29(9) . . ? C13 S15 C17 101.67(9) . . ? C14 S16 C18 101.30(10) . . ? C15 S17 C19 102.46(11) . . ? C16 S18 C20 99.02(11) . . ? C12 C11 S11 123.16(15) . . ? C12 C11 S12 121.49(15) . . ? S11 C11 S12 115.35(11) . . ? C11 C12 S14 121.99(14) . . ? C11 C12 S13 122.70(14) . . ? S14 C12 S13 115.31(10) . . ? C14 C13 S15 129.14(15) . . ? C14 C13 S11 117.29(14) . . ? S15 C13 S11 113.57(11) . . ? C13 C14 S12 116.67(14) . . ? C13 C14 S16 127.93(15) . . ? S12 C14 S16 115.39(10) . . ? C16 C15 S13 116.99(15) . . ? C16 C15 S17 128.88(16) . . ? S13 C15 S17 114.07(11) . . ? C15 C16 S18 127.53(16) . . ? C15 C16 S14 117.07(15) . . ? S18 C16 S14 115.34(11) . . ? C18 C17 S15 113.94(15) . . ? C18 C17 H17A 108.8 . . ? S15 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? S15 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 S16 114.05(14) . . ? C17 C18 H18A 108.7 . . ? S16 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? S16 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 S17 114.22(17) . . ? C20 C19 H19A 108.7 . . ? S17 C19 H19A 108.7 . . ? C20 C19 H19B 108.7 . . ? S17 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 S18 112.41(17) . . ? C19 C20 H20A 109.1 . . ? S18 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? S18 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? C21 S21 C23 94.87(9) . . ? C21 S22 C24 95.42(9) . . ? C22 S23 C25 95.40(9) . . ? C22 S24 C26 94.78(9) . . ? C27B S25 C23 105.8(4) . . ? C23 S25 C27A 100.15(16) . . ? C24 S26 C28A 102.82(11) . . ? C24 S26 C28B 96.0(3) . . ? C25 S27 C29A 105.24(13) . . ? C25 S27 C29B 93.9(4) . . ? C30B S28 C26 108.1(3) . . ? C26 S28 C30A 96.43(12) . . ? C22 C21 S21 121.78(14) . . ? C22 C21 S22 122.56(14) . . ? S21 C21 S22 115.65(11) . . ? C21 C22 S24 122.64(14) . . ? C21 C22 S23 121.85(14) . . ? S24 C22 S23 115.46(10) . . ? C24 C23 S25 128.33(15) . . ? C24 C23 S21 117.69(14) . . ? S25 C23 S21 113.98(11) . . ? C23 C24 S22 116.32(14) . . ? C23 C24 S26 128.00(15) . . ? S22 C24 S26 115.66(10) . . ? C26 C25 S27 127.65(15) . . ? C26 C25 S23 116.29(14) . . ? S27 C25 S23 115.98(11) . . ? C25 C26 S28 125.55(15) . . ? C25 C26 S24 117.69(14) . . ? S28 C26 S24 116.61(10) . . ? C28A C27A S25 112.8(3) . . ? C28A C27A H27A 109.0 . . ? S25 C27A H27A 109.0 . . ? C28A C27A H27B 109.0 . . ? S25 C27A H27B 109.0 . . ? H27A C27A H27B 107.8 . . ? C27A C28A S26 112.7(2) . . ? C27A C28A H28A 109.0 . . ? S26 C28A H28A 109.0 . . ? C27A C28A H28B 109.0 . . ? S26 C28A H28B 109.0 . . ? H28A C28A H28B 107.8 . . ? C28B C27B S25 112.9(8) . . ? C28B C27B H27C 109.0 . . ? S25 C27B H27C 109.0 . . ? C28B C27B H27D 109.0 . . ? S25 C27B H27D 109.0 . . ? H27C C27B H27D 107.8 . . ? C27B C28B S26 114.9(7) . . ? C27B C28B H28C 108.5 . . ? S26 C28B H28C 108.5 . . ? C27B C28B H28D 108.5 . . ? S26 C28B H28D 108.5 . . ? H28C C28B H28D 107.5 . . ? C30A C29A S27 116.1(2) . . ? C30A C29A H29A 108.3 . . ? S27 C29A H29A 108.3 . . ? C30A C29A H29B 108.3 . . ? S27 C29A H29B 108.3 . . ? H29A C29A H29B 107.4 . . ? C29A C30A S28 112.6(2) . . ? C29A C30A H30A 109.1 . . ? S28 C30A H30A 109.1 . . ? C29A C30A H30B 109.1 . . ? S28 C30A H30B 109.1 . . ? H30A C30A H30B 107.8 . . ? C30B C29B S27 114.8(7) . . ? C30B C29B H29C 108.6 . . ? S27 C29B H29C 108.6 . . ? C30B C29B H29D 108.6 . . ? S27 C29B H29D 108.6 . . ? H29C C29B H29D 107.5 . . ? C29B C30B S28 113.6(7) . . ? C29B C30B H30C 108.8 . . ? S28 C30B H30C 108.8 . . ? C29B C30B H30D 108.8 . . ? S28 C30B H30D 108.8 . . ? H30C C30B H30D 107.7 . . ? O3 Fe1 O3 161.17(10) 2_656 . ? O3 Fe1 O2 80.67(6) 2_656 . ? O3 Fe1 O2 87.33(6) . . ? O3 Fe1 O2 87.33(6) 2_656 2_656 ? O3 Fe1 O2 80.67(6) . 2_656 ? O2 Fe1 O2 100.75(10) . 2_656 ? O3 Fe1 O1 95.09(7) 2_656 2_656 ? O3 Fe1 O1 99.34(7) . 2_656 ? O2 Fe1 O1 168.19(7) . 2_656 ? O2 Fe1 O1 90.00(7) 2_656 2_656 ? O3 Fe1 O1 99.34(7) 2_656 . ? O3 Fe1 O1 95.09(7) . . ? O2 Fe1 O1 90.00(7) . . ? O2 Fe1 O1 168.19(7) 2_656 . ? O1 Fe1 O1 79.77(10) 2_656 . ? C1 O1 Fe1 116.26(15) . . ? C2 O2 Fe1 115.90(14) . . ? C3 O3 Fe1 115.24(13) . . ? O4 C1 O1 126.3(2) . . ? O4 C1 C1 119.99(15) . 2_656 ? O1 C1 C1 113.71(13) . 2_656 ? O5 C2 O2 126.1(2) . . ? O5 C2 C3 120.5(2) . 2_656 ? O2 C2 C3 113.43(19) . 2_656 ? O6 C3 O3 126.7(2) . . ? O6 C3 C2 119.1(2) . 2_656 ? O3 C3 C2 114.20(18) . 2_656 ? Cl31 Cl31 C31 84.4(3) 2_556 . ? Cl31 Cl31 C31 77.5(3) 2_556 2_556 ? C31 C31 C32 135.7(11) 2_556 2_556 ? C32 C31 C32 103.6(3) 2_556 . ? C31 C31 C36 150.3(16) 2_556 . ? C32 C31 C36 120.0 . . ? C32 C31 C36 116.17(19) 2_556 2_556 ? C36 C31 C36 132.63(14) . 2_556 ? C31 C31 Cl31 90.9(4) 2_556 . ? C32 C31 Cl31 132.9(6) 2_556 . ? C32 C31 Cl31 123.3(3) . . ? C36 C31 Cl31 116.7(3) . . ? C36 C31 Cl31 110.6(5) 2_556 . ? C31 C31 Cl31 78.8(5) 2_556 2_556 ? C32 C31 Cl31 140.9(7) 2_556 2_556 ? C32 C31 Cl31 113.7(4) . 2_556 ? C36 C31 Cl31 124.6(4) . 2_556 ? C36 C31 Cl31 101.5(5) 2_556 2_556 ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? N41 C45 C41 180.000(8) . . ? C42 C41 C42 122.9(10) 2_556 . ? C42 C41 C45 118.6(5) 2_556 . ? C42 C41 C45 118.6(5) . . ? C43 C42 C41 117.3(7) . . ? C43 C42 H42 121.3 . . ? C41 C42 H42 121.3 . . ? C42 C43 C44 120.4(7) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C43 121.6(10) . 2_556 ? C43 C44 H44 119.2 . . ? C43 C44 H44 119.2 2_556 . ? H51A O51 H51B 109(2) . . ? H51A O51 H51C 110(2) . . ? H51B O51 H51C 108(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C20 H20A O4 0.97 2.46 3.332(3) 149.0 7_656 C27A H27B O6 0.97 2.44 3.208(5) 136.1 1_455 C28A H28B O5 0.97 2.47 3.249(3) 137.5 . C27B H27C O6 0.97 2.49 3.102(12) 120.9 1_455 C28B H28C O5 0.97 2.51 3.267(9) 134.6 . C30A H30A O2 0.97 2.43 3.353(3) 159.5 5_656 C29B H29C O6 0.97 2.43 2.978(11) 115.3 5_656 C30B H30D O2 0.97 2.53 3.500(9) 173.3 5_656 C35 H35 O1 0.93 2.57 3.234(5) 129.1 . C36 H36 O4 0.93 2.44 3.206(6) 139.4 . O51 H51B O6 1.17(4) 1.70(4) 2.821(5) 158(5) 2_656 O51 H51C O5 1.17(3) 1.67(4) 2.829(6) 169(4) 2_556 O51 H51A O4 1.17(3) 1.71(3) 2.874(4) 173(5) 4_546 # Attachment '- XI.cif' data_beta''-(BEDT-TTF)4H3O[Fe(C2O4)3](BN)0.17(BB)0.83-(XI) _database_code_depnum_ccdc_archive 'CCDC 771737' _audit_creation_method ; CrysAlis RED (Oxford Diffraction Ltd.), SHELXL-97 and WinGX routine-INITIALISE ; _chemical_name_systematic ; ? ; _chemical_compound_source 'synthesis as described' _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), C6 Fe O12, 0.17(C7 H5 N), 0.83(C6 H5 Br), H3 O' _chemical_formula_sum 'C52.17 H40 Br0.83 Fe N0.17 O13 S32' _chemical_formula_weight 2025.36 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 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 10.2589(6) _cell_length_b 20.0680(10) _cell_length_c 35.450(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.174(5) _cell_angle_gamma 90.00 _cell_volume 7287.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10407 _cell_measurement_theta_min 3.7433 _cell_measurement_theta_max 71.1622 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4101 _exptl_absorpt_coefficient_mu 1.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65720 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Scale3AbsPack program of CrysAlisPro software' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 40850 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 32.30 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.786 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.083 _reflns_number_total 12230 _reflns_number_gt 8221 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997), DIAMOND 3.1 (Crystal Impact GbR 2005)' _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^ > 2\s(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^)+(0.0735P)^2^+1.8137P] 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 12230 _refine_ls_number_parameters 487 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S11 S 0.42316(6) 0.21376(3) 0.508580(19) 0.04400(15) Uani 1 1 d . . . S12 S 0.66485(6) 0.14359(3) 0.531251(18) 0.04131(14) Uani 1 1 d . . . S13 S 0.53992(6) 0.24540(4) 0.427173(19) 0.04411(15) Uani 1 1 d . . . S14 S 0.77928(6) 0.17410(3) 0.450805(18) 0.04254(15) Uani 1 1 d . . . S15 S 0.29681(6) 0.19278(4) 0.57959(2) 0.05048(17) Uani 1 1 d . . . S16 S 0.58861(6) 0.11089(4) 0.608114(19) 0.04756(16) Uani 1 1 d . . . S17 S 0.61530(9) 0.27317(4) 0.35019(2) 0.0605(2) Uani 1 1 d . . . S18 S 0.90629(7) 0.19303(4) 0.37922(2) 0.05365(18) Uani 1 1 d . . . C11 C 0.5762(2) 0.18787(12) 0.49649(7) 0.0358(5) Uani 1 1 d . . . C12 C 0.6260(2) 0.20104(12) 0.46229(7) 0.0352(5) Uani 1 1 d . . . C13 C 0.4345(2) 0.17979(12) 0.55415(7) 0.0378(5) Uani 1 1 d . . . C14 C 0.5466(2) 0.14766(12) 0.56465(7) 0.0365(5) Uani 1 1 d . . . C15 C 0.6600(2) 0.23944(12) 0.39427(7) 0.0406(5) Uani 1 1 d . . . C16 C 0.7713(2) 0.20769(12) 0.40547(7) 0.0398(5) Uani 1 1 d . . . C17 C 0.3555(3) 0.17002(15) 0.62698(8) 0.0499(6) Uani 1 1 d . . . H17A H 0.4094 0.2059 0.6375 0.060 Uiso 1 1 calc R . . H17B H 0.2813 0.1653 0.6426 0.060 Uiso 1 1 calc R . . C18 C 0.4339(3) 0.10612(13) 0.62902(8) 0.0465(6) Uani 1 1 d . . . H18A H 0.3827 0.0711 0.6165 0.056 Uiso 1 1 calc R . . H18B H 0.4485 0.0936 0.6553 0.056 Uiso 1 1 calc R . . C19 C 0.7606(3) 0.2608(2) 0.32455(9) 0.0711(10) Uani 1 1 d . . . H19A H 0.7369 0.2629 0.2977 0.085 Uiso 1 1 calc R . . H19B H 0.8207 0.2971 0.3305 0.085 Uiso 1 1 calc R . . C20 C 0.8298(4) 0.19592(19) 0.33287(9) 0.0700(9) Uani 1 1 d . . . H20A H 0.8954 0.1892 0.3146 0.084 Uiso 1 1 calc R . . H20B H 0.7674 0.1597 0.3300 0.084 Uiso 1 1 calc R . . S21 S 0.02557(6) 0.08822(3) 0.519660(17) 0.04333(15) Uani 1 1 d . . . S22 S 0.25843(6) 0.01183(3) 0.543985(18) 0.04181(15) Uani 1 1 d . . . S23 S 0.14703(6) 0.11753(4) 0.440076(17) 0.04363(15) Uani 1 1 d . . . S24 S 0.38245(6) 0.04252(3) 0.463775(18) 0.04106(14) Uani 1 1 d . . . S25 S -0.10678(7) 0.07167(5) 0.58983(2) 0.0627(2) Uani 1 1 d . . . S26 S 0.17278(6) -0.01633(4) 0.62074(2) 0.05064(18) Uani 1 1 d . . . S27 S 0.24235(8) 0.15773(4) 0.36621(2) 0.05611(19) Uani 1 1 d . . . S28 S 0.51846(6) 0.07213(3) 0.39411(2) 0.04601(16) Uani 1 1 d . . . C21 C 0.1784(2) 0.05930(12) 0.50909(6) 0.0350(5) Uani 1 1 d . . . C22 C 0.2311(2) 0.07235(12) 0.47533(6) 0.0354(5) Uani 1 1 d . . . C23 C 0.0307(2) 0.05496(13) 0.56516(7) 0.0396(5) Uani 1 1 d . A . C24 C 0.1378(2) 0.01992(12) 0.57657(7) 0.0372(5) Uani 1 1 d . A . C25 C 0.2734(2) 0.11732(12) 0.40893(7) 0.0378(5) Uani 1 1 d . B . C26 C 0.3821(2) 0.08318(12) 0.42031(7) 0.0373(5) Uani 1 1 d . B . C27A C -0.0453(6) 0.0534(3) 0.63783(18) 0.0503(13) Uani 0.72 1 d P A 1 H27A H 0.0162 0.0878 0.6460 0.060 Uiso 0.72 1 calc PR A 1 H27B H -0.1175 0.0548 0.6544 0.060 Uiso 0.72 1 calc PR A 1 C28A C 0.0209(4) -0.0133(2) 0.64204(11) 0.0458(8) Uani 0.72 1 d P A 1 H28A H -0.0361 -0.0473 0.6307 0.055 Uiso 0.72 1 calc PR A 1 H28B H 0.0347 -0.0236 0.6687 0.055 Uiso 0.72 1 calc PR A 1 C27B C -0.0852(13) 0.0308(8) 0.6317(5) 0.049(4) Uani 0.28 1 d P A 2 H27C H -0.1401 0.0508 0.6501 0.059 Uiso 0.28 1 calc PR A 2 H27D H -0.1112 -0.0154 0.6284 0.059 Uiso 0.28 1 calc PR A 2 C28B C 0.0577(10) 0.0341(6) 0.6466(3) 0.050(2) Uani 0.28 1 d P A 2 H28C H 0.0626 0.0198 0.6728 0.060 Uiso 0.28 1 calc PR A 2 H28D H 0.0859 0.0802 0.6461 0.060 Uiso 0.28 1 calc PR A 2 C29A C 0.3587(5) 0.1263(3) 0.33567(14) 0.0517(11) Uani 0.73 1 d P B 1 H29A H 0.3148 0.1185 0.3111 0.062 Uiso 0.73 1 calc PR B 1 H29B H 0.4238 0.1606 0.3325 0.062 Uiso 0.73 1 calc PR B 1 C30A C 0.4281(5) 0.0634(2) 0.34783(12) 0.0502(9) Uani 0.73 1 d P B 1 H30A H 0.4888 0.0511 0.3290 0.060 Uiso 0.73 1 calc PR B 1 H30B H 0.3648 0.0277 0.3493 0.060 Uiso 0.73 1 calc PR B 1 C29B C 0.3336(14) 0.0959(7) 0.3389(4) 0.050(3) Uani 0.27 1 d PU B 2 H29C H 0.2980 0.0520 0.3433 0.060 Uiso 0.27 1 calc PR B 2 H29D H 0.3189 0.1056 0.3122 0.060 Uiso 0.27 1 calc PR B 2 C30B C 0.4803(12) 0.0941(6) 0.3484(3) 0.049(3) Uani 0.27 1 d P B 2 H30C H 0.5167 0.1377 0.3436 0.059 Uiso 0.27 1 calc PR B 2 H30D H 0.5200 0.0625 0.3318 0.059 Uiso 0.27 1 calc PR B 2 Fe1 Fe 0.5000 0.08181(2) 0.7500 0.03694(12) Uani 1 2 d S . . O1 O 0.42733(19) 0.15903(9) 0.71919(5) 0.0498(4) Uani 1 1 d . . . O2 O 0.39602(17) 0.01789(9) 0.71687(5) 0.0456(4) Uani 1 1 d . . . O3 O 0.64986(17) 0.06550(9) 0.71702(5) 0.0453(4) Uani 1 1 d . . . O4 O 0.4140(2) 0.26959(11) 0.71820(7) 0.0670(6) Uani 1 1 d . . . O5 O 0.21650(19) -0.04419(11) 0.71481(6) 0.0590(5) Uani 1 1 d . . . O6 O 0.8188(2) -0.00255(12) 0.71161(6) 0.0633(6) Uani 1 1 d . . . C1 C 0.4540(3) 0.21698(13) 0.73191(8) 0.0466(6) Uani 1 1 d . . . C2 C 0.2930(2) -0.00530(13) 0.73059(7) 0.0412(5) Uani 1 1 d . . . C3 C 0.7299(2) 0.02061(13) 0.72886(7) 0.0417(5) Uani 1 1 d . . . C31 C 0.0131(7) 0.26082(15) 0.7489(2) 0.0507(8) Uiso 0.413(2) 1 d PG . 1 C32 C -0.0815(6) 0.2229(2) 0.7655(2) 0.0507(8) Uiso 0.413(2) 1 d PG . 1 H32 H -0.1454 0.2436 0.7790 0.061 Uiso 0.413(2) 1 calc PR . 1 C33 C -0.0806(4) 0.1539(2) 0.76203(15) 0.0507(8) Uiso 0.413(2) 1 d PG . 1 H33 H -0.1440 0.1285 0.7731 0.061 Uiso 0.413(2) 1 calc PR . 1 C34 C 0.0148(5) 0.12284(15) 0.74193(15) 0.0507(8) Uiso 0.413(2) 1 d PG . 1 H34 H 0.0154 0.0767 0.7396 0.061 Uiso 0.413(2) 1 calc PR . 1 C35 C 0.1094(4) 0.1608(2) 0.72531(14) 0.0507(8) Uiso 0.413(2) 1 d PG . 1 H35 H 0.1733 0.1400 0.7119 0.061 Uiso 0.413(2) 1 calc PR . 1 C36 C 0.1086(5) 0.2298(2) 0.72880(19) 0.0507(8) Uiso 0.413(2) 1 d PG . 1 H36 H 0.1719 0.2552 0.7177 0.061 Uiso 0.413(2) 1 calc PR . 1 Br1 Br 0.0188(7) 0.35202(5) 0.7534(2) 0.0815(15) Uani 0.413(2) 1 d P . 1 C41 C 0.0000 0.2456(10) 0.7500 0.0507(8) Uiso 0.174(4) 2 d SPD . 2 C42 C 0.0939(15) 0.2113(9) 0.7304(5) 0.0507(8) Uiso 0.174(4) 1 d PD . 2 H42 H 0.1603 0.2344 0.7192 0.061 Uiso 0.174(4) 1 calc PR . 2 C43 C 0.0860(14) 0.1406(9) 0.7278(4) 0.0507(8) Uiso 0.174(4) 1 d PD . 2 H43 H 0.1376 0.1174 0.7115 0.061 Uiso 0.174(4) 1 calc PR . 2 C44 C 0.0000 0.1068(10) 0.7500 0.0507(8) Uiso 0.174(4) 2 d SPD . 2 H44 H 0.0000 0.0605 0.7500 0.061 Uiso 0.174(4) 2 calc SPR . 2 C45 C 0.0000 0.3257(18) 0.7500 0.0507(8) Uiso 0.174(4) 2 d SP . 2 N41 N 0.0000 0.3744(16) 0.7500 0.0507(8) Uiso 0.174(4) 2 d SP . 2 O51 O 0.0104(7) -0.09979(18) 0.75542(19) 0.0618(11) Uiso 0.50 1 d PD . . H51A H 0.036(5) -0.1515(19) 0.760(2) 0.093 Uiso 0.50 1 d PD . . H51B H 0.092(4) -0.069(3) 0.765(2) 0.093 Uiso 0.50 1 d PD . . H51C H -0.071(6) -0.087(3) 0.772(2) 0.093 Uiso 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 S11 0.0393(3) 0.0545(4) 0.0385(3) 0.0037(3) 0.0048(2) 0.0107(3) S12 0.0374(3) 0.0506(4) 0.0365(3) 0.0078(3) 0.0074(2) 0.0081(2) S13 0.0416(3) 0.0524(4) 0.0384(3) 0.0060(3) 0.0029(2) 0.0100(3) S14 0.0388(3) 0.0489(4) 0.0403(3) 0.0068(3) 0.0056(2) 0.0072(3) S15 0.0400(3) 0.0633(4) 0.0493(4) 0.0027(3) 0.0134(3) 0.0113(3) S16 0.0445(3) 0.0581(4) 0.0409(4) 0.0136(3) 0.0096(3) 0.0070(3) S17 0.0780(5) 0.0682(5) 0.0348(4) 0.0096(3) -0.0015(3) 0.0069(4) S18 0.0539(4) 0.0516(4) 0.0577(4) 0.0025(3) 0.0237(3) 0.0021(3) C11 0.0346(10) 0.0392(12) 0.0337(12) -0.0009(9) 0.0026(9) 0.0033(9) C12 0.0331(10) 0.0387(12) 0.0339(12) -0.0007(9) 0.0019(9) 0.0031(9) C13 0.0363(11) 0.0403(13) 0.0374(12) -0.0025(10) 0.0089(9) 0.0000(9) C14 0.0391(11) 0.0365(12) 0.0343(12) 0.0009(9) 0.0066(9) 0.0003(9) C15 0.0527(14) 0.0366(12) 0.0328(12) 0.0006(9) 0.0044(10) -0.0010(10) C16 0.0443(12) 0.0356(12) 0.0405(13) -0.0015(10) 0.0101(10) -0.0010(10) C17 0.0534(15) 0.0526(16) 0.0452(15) -0.0012(12) 0.0164(12) 0.0043(12) C18 0.0488(14) 0.0473(15) 0.0447(14) 0.0053(11) 0.0155(11) -0.0013(11) C19 0.078(2) 0.101(3) 0.0347(15) 0.0104(16) 0.0028(14) -0.025(2) C20 0.079(2) 0.078(2) 0.0556(19) -0.0193(17) 0.0258(16) -0.0156(18) S21 0.0399(3) 0.0584(4) 0.0321(3) 0.0077(3) 0.0058(2) 0.0140(3) S22 0.0395(3) 0.0513(4) 0.0353(3) 0.0075(3) 0.0076(2) 0.0117(3) S23 0.0403(3) 0.0595(4) 0.0318(3) 0.0066(3) 0.0081(2) 0.0158(3) S24 0.0395(3) 0.0480(4) 0.0362(3) 0.0050(3) 0.0066(2) 0.0109(2) S25 0.0487(4) 0.0944(6) 0.0468(4) 0.0231(4) 0.0191(3) 0.0303(4) S26 0.0412(3) 0.0653(4) 0.0462(4) 0.0259(3) 0.0091(3) 0.0072(3) S27 0.0703(4) 0.0627(5) 0.0370(3) 0.0139(3) 0.0170(3) 0.0246(4) S28 0.0400(3) 0.0484(4) 0.0512(4) 0.0018(3) 0.0171(3) 0.0067(3) C21 0.0349(10) 0.0407(12) 0.0296(11) 0.0018(9) 0.0042(8) 0.0054(9) C22 0.0354(11) 0.0409(12) 0.0302(11) -0.0011(9) 0.0040(8) 0.0056(9) C23 0.0364(11) 0.0468(13) 0.0364(12) 0.0068(10) 0.0101(9) 0.0042(10) C24 0.0365(11) 0.0396(13) 0.0360(12) 0.0058(9) 0.0061(9) 0.0008(9) C25 0.0424(12) 0.0380(12) 0.0338(12) 0.0037(9) 0.0101(9) 0.0079(9) C26 0.0389(11) 0.0367(12) 0.0372(12) -0.0006(9) 0.0115(9) 0.0017(9) C27A 0.052(4) 0.060(4) 0.040(2) 0.008(2) 0.011(3) 0.012(2) C28A 0.0427(18) 0.053(2) 0.043(2) 0.0161(17) 0.0101(15) 0.0022(17) C27B 0.034(6) 0.070(11) 0.045(8) 0.023(7) 0.012(5) 0.001(5) C28B 0.053(6) 0.071(7) 0.026(4) 0.006(4) 0.002(4) 0.002(5) C29A 0.056(3) 0.061(3) 0.039(2) 0.003(2) 0.0120(18) 0.006(2) C30A 0.060(3) 0.050(2) 0.042(2) -0.0083(18) 0.0163(19) 0.005(2) C29B 0.060(6) 0.057(7) 0.035(5) -0.016(5) 0.013(4) -0.010(6) C30B 0.062(7) 0.055(7) 0.033(5) -0.003(5) 0.023(5) -0.002(5) Fe1 0.0439(3) 0.0359(3) 0.0316(2) 0.000 0.00670(19) 0.000 O1 0.0634(11) 0.0440(10) 0.0417(10) 0.0026(8) -0.0001(8) 0.0021(8) O2 0.0498(10) 0.0513(11) 0.0368(9) -0.0063(8) 0.0121(7) -0.0079(8) O3 0.0487(10) 0.0498(10) 0.0385(9) 0.0042(8) 0.0115(8) -0.0024(8) O4 0.0751(14) 0.0465(12) 0.0799(16) 0.0154(11) 0.0080(12) 0.0077(10) O5 0.0545(11) 0.0682(14) 0.0542(12) -0.0053(10) 0.0022(9) -0.0186(10) O6 0.0585(12) 0.0771(15) 0.0568(13) -0.0045(11) 0.0254(10) 0.0090(10) C1 0.0516(14) 0.0393(14) 0.0507(15) 0.0040(11) 0.0189(11) 0.0010(11) C2 0.0446(13) 0.0397(13) 0.0395(13) 0.0070(10) 0.0032(10) 0.0035(10) C3 0.0433(12) 0.0445(14) 0.0382(13) -0.0093(10) 0.0095(10) -0.0066(10) Br1 0.126(4) 0.0597(6) 0.063(2) -0.0039(9) 0.043(2) -0.0182(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S11 C11 1.730(2) . ? S11 C13 1.751(3) . ? S12 C11 1.735(2) . ? S12 C14 1.744(2) . ? S13 C12 1.732(2) . ? S13 C15 1.747(3) . ? S14 C12 1.733(2) . ? S14 C16 1.740(3) . ? S15 C13 1.738(2) . ? S15 C17 1.811(3) . ? S16 C14 1.741(2) . ? S16 C18 1.791(3) . ? S17 C15 1.741(3) . ? S17 C19 1.805(4) . ? S18 C16 1.736(2) . ? S18 C20 1.782(4) . ? C11 C12 1.367(3) . ? C13 C14 1.352(3) . ? C15 C16 1.348(3) . ? C17 C18 1.513(4) . ? C19 C20 1.505(5) . ? S21 C21 1.732(2) . ? S21 C23 1.744(2) . ? S22 C21 1.732(2) . ? S22 C24 1.747(2) . ? S23 C22 1.735(2) . ? S23 C25 1.749(2) . ? S24 C22 1.734(2) . ? S24 C26 1.743(2) . ? S25 C27B 1.701(16) . ? S25 C23 1.733(2) . ? S25 C27A 1.819(6) . ? S26 C24 1.746(2) . ? S26 C28A 1.769(4) . ? S26 C28B 1.837(11) . ? S27 C25 1.732(2) . ? S27 C29A 1.771(5) . ? S27 C29B 1.858(13) . ? S28 C30B 1.705(11) . ? S28 C26 1.736(2) . ? S28 C30A 1.848(5) . ? C21 C22 1.366(3) . ? C23 C24 1.347(3) . ? C25 C26 1.351(3) . ? C27A C28A 1.505(8) . ? C27B C28B 1.531(16) . ? C29A C30A 1.501(7) . ? C29B C30B 1.524(19) . ? Fe1 O2 2.0060(18) . ? Fe1 O2 2.0060(18) 2_656 ? Fe1 O3 2.0091(17) . ? Fe1 O3 2.0091(17) 2_656 ? Fe1 O1 2.0149(19) 2_656 ? Fe1 O1 2.0149(19) . ? O1 C1 1.271(3) . ? O2 C2 1.276(3) . ? O3 C3 1.274(3) . ? O4 C1 1.223(3) . ? O5 C2 1.220(3) . ? O6 C3 1.217(3) . ? C1 C1 1.550(6) 2_656 ? C2 C3 1.559(4) 2_656 ? C3 C2 1.559(4) 2_656 ? C31 C31 0.285(13) 2_556 ? C31 C32 1.171(7) 2_556 ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 C36 1.638(9) 2_556 ? C31 Br1 1.838(3) . ? C31 Br1 1.860(3) 2_556 ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? Br1 Br1 0.444(14) 2_556 ? Br1 C31 1.860(3) 2_556 ? C41 C42 1.400(14) 2_556 ? C41 C42 1.400(14) . ? C41 C45 1.61(4) . ? C42 C43 1.42(2) . ? C43 C44 1.391(14) . ? C44 C43 1.391(14) 2_556 ? C45 N41 0.98(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 C11 S11 C13 95.54(11) . . ? C11 S12 C14 95.80(11) . . ? C12 S13 C15 95.41(11) . . ? C12 S14 C16 95.69(11) . . ? C13 S15 C17 101.85(12) . . ? C14 S16 C18 101.95(12) . . ? C15 S17 C19 102.40(14) . . ? C16 S18 C20 99.50(14) . . ? C12 C11 S11 123.40(18) . . ? C12 C11 S12 121.46(18) . . ? S11 C11 S12 115.14(13) . . ? C11 C12 S14 122.45(18) . . ? C11 C12 S13 122.41(17) . . ? S14 C12 S13 115.14(13) . . ? C14 C13 S15 129.2(2) . . ? C14 C13 S11 116.87(17) . . ? S15 C13 S11 113.94(13) . . ? C13 C14 S16 127.67(18) . . ? C13 C14 S12 116.64(18) . . ? S16 C14 S12 115.68(13) . . ? C16 C15 S17 128.7(2) . . ? C16 C15 S13 116.92(19) . . ? S17 C15 S13 114.35(14) . . ? C15 C16 S18 127.6(2) . . ? C15 C16 S14 116.81(18) . . ? S18 C16 S14 115.54(14) . . ? C18 C17 S15 114.0(2) . . ? C17 C18 S16 114.56(19) . . ? C20 C19 S17 114.5(2) . . ? C19 C20 S18 112.8(2) . . ? C21 S21 C23 95.20(11) . . ? C21 S22 C24 95.52(11) . . ? C22 S23 C25 95.57(11) . . ? C22 S24 C26 95.10(11) . . ? C27B S25 C23 106.1(6) . . ? C23 S25 C27A 100.6(2) . . ? C24 S26 C28A 103.09(14) . . ? C24 S26 C28B 96.4(3) . . ? C25 S27 C29A 105.67(18) . . ? C25 S27 C29B 94.0(5) . . ? C30B S28 C26 109.0(4) . . ? C26 S28 C30A 96.19(16) . . ? C22 C21 S22 122.45(18) . . ? C22 C21 S21 122.17(18) . . ? S22 C21 S21 115.37(13) . . ? C21 C22 S24 122.95(18) . . ? C21 C22 S23 121.76(18) . . ? S24 C22 S23 115.24(13) . . ? C24 C23 S25 128.48(19) . . ? C24 C23 S21 117.38(18) . . ? S25 C23 S21 114.14(13) . . ? C23 C24 S26 127.63(18) . . ? C23 C24 S22 116.47(18) . . ? S26 C24 S22 115.87(13) . . ? C26 C25 S27 127.41(18) . . ? C26 C25 S23 116.17(18) . . ? S27 C25 S23 116.36(13) . . ? C25 C26 S28 125.54(19) . . ? C25 C26 S24 117.56(17) . . ? S28 C26 S24 116.79(14) . . ? C28A C27A S25 113.8(4) . . ? C27A C28A S26 113.0(3) . . ? C28B C27B S25 110.8(9) . . ? C27B C28B S26 115.8(9) . . ? C30A C29A S27 116.7(3) . . ? C29A C30A S28 112.5(3) . . ? C30B C29B S27 114.9(8) . . ? C29B C30B S28 112.8(8) . . ? O2 Fe1 O2 100.50(11) . 2_656 ? O2 Fe1 O3 87.38(7) . . ? O2 Fe1 O3 80.64(7) 2_656 . ? O2 Fe1 O3 80.64(7) . 2_656 ? O2 Fe1 O3 87.38(7) 2_656 2_656 ? O3 Fe1 O3 161.25(11) . 2_656 ? O2 Fe1 O1 167.95(8) . 2_656 ? O2 Fe1 O1 90.32(8) 2_656 2_656 ? O3 Fe1 O1 99.70(8) . 2_656 ? O3 Fe1 O1 94.71(8) 2_656 2_656 ? O2 Fe1 O1 90.32(8) . . ? O2 Fe1 O1 167.95(8) 2_656 . ? O3 Fe1 O1 94.71(8) . . ? O3 Fe1 O1 99.70(8) 2_656 . ? O1 Fe1 O1 79.46(11) 2_656 . ? C1 O1 Fe1 116.46(18) . . ? C2 O2 Fe1 115.79(16) . . ? C3 O3 Fe1 115.06(16) . . ? O4 C1 O1 126.0(3) . . ? O4 C1 C1 120.26(18) . 2_656 ? O1 C1 C1 113.73(15) . 2_656 ? O5 C2 O2 125.7(2) . . ? O5 C2 C3 120.7(2) . 2_656 ? O2 C2 C3 113.6(2) . 2_656 ? O6 C3 O3 126.2(3) . . ? O6 C3 C2 119.4(2) . 2_656 ? O3 C3 C2 114.3(2) . 2_656 ? C32 C31 C36 120.0 . . ? C32 C31 Br1 121.8(4) . . ? C36 C31 Br1 118.1(4) . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C42 121.1(14) 2_556 . ? C42 C41 C45 119.4(7) 2_556 . ? C42 C41 C45 119.4(7) . . ? C41 C42 C43 118.9(8) . . ? C44 C43 C42 119.0(8) . . ? C43 C44 C43 121.6(15) . 2_556 ? N41 C45 C41 180.000(16) . . ?