# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Dr Carlos Gimenez-Saiz' _publ_contact_author_address ; Instituto de Ciencia Molecular Universidad de Valencia C/ Dr. Moliner, 50. Edificio F, 3er Burjassot Valencia 46100 SPAIN ; _publ_contact_author_email CARLOS.GIMENEZ@UV.ES _publ_section_title ; A novel paramagnetic molecular superconductor formed by bis(ethylenedithio)tetrathiafulvalene, tris(oxalato)ferrate(III) anions and bromobenzene as guest molecule: ET4[(H3O)Fe(C2O4)3]*C6H5Br ; loop_ _publ_author_name 'Carlos Gimenez-Saiz' 'Eugenio Coronado' 'Simona Curreli' 'Carlos J. Gomez-Garcia' data_ETFeBr _database_code_depnum_ccdc_archive 'CCDC 240303' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C10 H8 S8), (C6 Fe O12), (C6 H5 Br), (H3 O)' _chemical_formula_sum 'C52 H40 Br Fe O13 S32' _chemical_formula_weight 2034.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Br Br -0.2901 2.4595 '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 10.2875(3) _cell_length_b 20.0546(15) _cell_length_c 35.513(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.238(5) _cell_angle_gamma 90.00 _cell_volume 7315.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 113186 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4116 _exptl_absorpt_coefficient_mu 1.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.774 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38333 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8228 _reflns_number_gt 4980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.6031P] 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 8228 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 S1 S -0.07720(10) 0.21363(5) 0.00861(3) 0.0401(3) Uani 1 1 d . . . S2 S 0.16517(10) 0.14353(5) 0.03135(3) 0.0372(3) Uani 1 1 d . . . S3 S 0.03920(10) 0.24532(5) -0.07269(3) 0.0402(3) Uani 1 1 d . . . S4 S 0.27889(10) 0.17410(5) -0.04902(3) 0.0388(3) Uani 1 1 d . . . S5 S -0.20272(10) 0.19278(5) 0.07961(3) 0.0463(3) Uani 1 1 d . . . S6 S 0.08970(10) 0.11113(5) 0.10813(3) 0.0432(3) Uani 1 1 d . . . S7 S 0.11348(13) 0.27277(6) -0.14957(3) 0.0564(3) Uani 1 1 d . . . S8 S 0.40513(11) 0.19294(5) -0.12067(3) 0.0493(3) Uani 1 1 d . . . C1 C 0.0764(4) 0.18765(17) -0.00350(10) 0.0317(9) Uani 1 1 d . . . C2 C 0.1253(4) 0.20099(17) -0.03758(10) 0.0325(9) Uani 1 1 d . . . C3 C -0.0649(4) 0.17985(17) 0.05411(11) 0.0352(9) Uani 1 1 d . . . C4 C 0.0470(4) 0.14786(17) 0.06457(10) 0.0324(9) Uani 1 1 d . . . C5 C 0.1595(4) 0.23945(17) -0.10534(10) 0.0356(9) Uani 1 1 d . . . C6 C 0.2703(4) 0.20750(17) -0.09443(10) 0.0331(9) Uani 1 1 d . . . C7 C -0.1448(4) 0.17028(19) 0.12682(11) 0.0445(11) Uani 1 1 d . . . H7A H -0.0917 0.2064 0.1374 0.053 Uiso 1 1 calc R . . H7B H -0.2190 0.1652 0.1423 0.053 Uiso 1 1 calc R . . C8 C -0.0656(4) 0.10637(18) 0.12885(12) 0.0437(11) Uani 1 1 d . . . H8A H -0.1163 0.0712 0.1163 0.052 Uiso 1 1 calc R . . H8B H -0.0513 0.0938 0.1551 0.052 Uiso 1 1 calc R . . C9 C 0.2589(5) 0.2601(3) -0.17532(12) 0.0692(15) Uani 1 1 d . . . H9A H 0.2348 0.2613 -0.2021 0.083 Uiso 1 1 calc R . . H9B H 0.3181 0.2970 -0.1698 0.083 Uiso 1 1 calc R . . C10 C 0.3291(5) 0.1963(2) -0.16650(13) 0.0629(14) Uani 1 1 d . . . H10A H 0.3948 0.1899 -0.1847 0.076 Uiso 1 1 calc R . . H10B H 0.2677 0.1597 -0.1694 0.076 Uiso 1 1 calc R . . S9 S 0.52566(10) 0.08826(5) 0.01982(3) 0.0395(3) Uani 1 1 d . . . S10 S 0.75880(10) 0.01171(5) 0.04408(3) 0.0378(3) Uani 1 1 d . . . S11 S 0.64626(10) 0.11726(5) -0.05979(3) 0.0393(3) Uani 1 1 d . . . S12 S 0.88212(10) 0.04236(5) -0.03613(3) 0.0373(3) Uani 1 1 d . . . S13 S 0.39421(11) 0.07220(6) 0.09000(3) 0.0585(4) Uani 1 1 d . . . S14 S 0.67385(10) -0.01617(5) 0.12085(3) 0.0466(3) Uani 1 1 d . . . S15 S 0.74096(12) 0.15764(6) -0.13353(3) 0.0514(3) Uani 1 1 d . . . S16 S 1.01737(10) 0.07202(5) -0.10570(3) 0.0416(3) Uani 1 1 d . . . C11 C 0.6791(4) 0.05927(17) 0.00916(10) 0.0311(9) Uani 1 1 d . . . C12 C 0.7302(4) 0.07211(17) -0.02460(10) 0.0317(9) Uani 1 1 d . . . C13 C 0.5314(4) 0.05536(17) 0.06528(10) 0.0326(9) Uani 1 1 d . A . C14 C 0.6377(4) 0.02017(17) 0.07663(10) 0.0321(9) Uani 1 1 d . A . C15 C 0.7732(4) 0.11729(17) -0.09063(10) 0.0320(9) Uani 1 1 d . B . C16 C 0.8815(4) 0.08323(17) -0.07936(10) 0.0317(9) Uani 1 1 d . B . C17A C 0.4534(16) 0.0532(6) 0.1389(3) 0.043(3) Uani 0.684(17) 1 d P A 1 H17A H 0.5128 0.0880 0.1479 0.051 Uiso 0.684(17) 1 calc PR A 1 H17B H 0.3802 0.0529 0.1550 0.051 Uiso 0.684(17) 1 calc PR A 1 C18A C 0.5224(6) -0.0135(5) 0.14211(18) 0.037(2) Uani 0.684(17) 1 d P A 1 H18A H 0.4659 -0.0474 0.1306 0.044 Uiso 0.684(17) 1 calc PR A 1 H18B H 0.5365 -0.0247 0.1686 0.044 Uiso 0.684(17) 1 calc PR A 1 C17B C 0.421(4) 0.0331(19) 0.1298(9) 0.082(12) Uani 0.316(17) 1 d P A 2 H17C H 0.3639 0.0521 0.1478 0.099 Uiso 0.316(17) 1 calc PR A 2 H17D H 0.3951 -0.0130 0.1259 0.099 Uiso 0.316(17) 1 calc PR A 2 C18B C 0.553(2) 0.0338(15) 0.1466(4) 0.068(8) Uani 0.316(17) 1 d P A 2 H18C H 0.5508 0.0169 0.1722 0.082 Uiso 0.316(17) 1 calc PR A 2 H18D H 0.5824 0.0796 0.1482 0.082 Uiso 0.316(17) 1 calc PR A 2 C19A C 0.8585(12) 0.1268(7) -0.1641(3) 0.044(3) Uani 0.67(3) 1 d P B 1 H19A H 0.8157 0.1195 -0.1888 0.052 Uiso 0.67(3) 1 calc PR B 1 H19B H 0.9239 0.1611 -0.1668 0.052 Uiso 0.67(3) 1 calc PR B 1 C20A C 0.9267(11) 0.0633(7) -0.1517(2) 0.040(3) Uani 0.67(3) 1 d P B 1 H20A H 0.9866 0.0504 -0.1706 0.048 Uiso 0.67(3) 1 calc PR B 1 H20B H 0.8627 0.0280 -0.1501 0.048 Uiso 0.67(3) 1 calc PR B 1 C19B C 0.828(3) 0.0990(16) -0.1613(8) 0.059(7) Uani 0.33(3) 1 d P B 2 H19C H 0.7902 0.0552 -0.1582 0.071 Uiso 0.33(3) 1 calc PR B 2 H19D H 0.8142 0.1111 -0.1876 0.071 Uiso 0.33(3) 1 calc PR B 2 C20B C 0.974(3) 0.0937(14) -0.1522(6) 0.061(7) Uani 0.33(3) 1 d P B 2 H20C H 1.0139 0.1362 -0.1576 0.074 Uiso 0.33(3) 1 calc PR B 2 H20D H 1.0095 0.0607 -0.1688 0.074 Uiso 0.33(3) 1 calc PR B 2 Fe1 Fe 1.0000 0.08179(4) 0.2500 0.0375(2) Uani 1 2 d S . . C21 C 1.0454(4) 0.2171(2) 0.26816(11) 0.0446(11) Uani 1 1 d . . . C22 C 0.7698(4) 0.0214(2) 0.27091(12) 0.0428(11) Uani 1 1 d . . . C23 C 0.7922(4) -0.0054(2) 0.23062(11) 0.0408(10) Uani 1 1 d . . . O1 O 1.0725(3) 0.15896(13) 0.28108(7) 0.0480(8) Uani 1 1 d . . . O2 O 1.0853(3) 0.27013(15) 0.28202(10) 0.0673(10) Uani 1 1 d . . . O3 O 0.8500(3) 0.06600(13) 0.28285(7) 0.0443(7) Uani 1 1 d . . . O4 O 0.8964(3) 0.01728(13) 0.21710(7) 0.0448(7) Uani 1 1 d . . . O5 O 0.6801(3) -0.00177(15) 0.28832(8) 0.0600(9) Uani 1 1 d . . . O6 O 0.7157(3) -0.04420(14) 0.21518(8) 0.0560(8) Uani 1 1 d . . . Br1 Br 0.5000 0.35323(4) 0.2500 0.0968(4) Uani 1 2 d S . . C24 C 0.5000 0.2584(3) 0.2500 0.0559(17) Uani 1 2 d S . . C25 C 0.5957(5) 0.2260(2) 0.23107(14) 0.0630(13) Uani 1 1 d . . . H25 H 0.6584 0.2498 0.2188 0.076 Uiso 1 1 calc R . . C26 C 0.5951(6) 0.1582(3) 0.23094(17) 0.0843(18) Uani 1 1 d . . . H26 H 0.6575 0.1349 0.2183 0.101 Uiso 1 1 calc R . . C27 C 0.5000 0.1235(4) 0.2500 0.105(3) Uani 1 2 d S . . H27 H 0.5000 0.0771 0.2500 0.126 Uiso 1 2 calc SR . . O1W O 0.5000 -0.0995(2) 0.2500 0.0789(16) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0339(6) 0.0494(6) 0.0372(6) 0.0040(5) 0.0042(5) 0.0094(5) S2 0.0313(6) 0.0473(6) 0.0337(5) 0.0081(5) 0.0074(5) 0.0078(4) S3 0.0379(6) 0.0477(6) 0.0350(6) 0.0063(5) 0.0029(5) 0.0091(5) S4 0.0338(6) 0.0437(6) 0.0392(6) 0.0076(5) 0.0049(5) 0.0070(5) S5 0.0338(6) 0.0595(7) 0.0464(7) 0.0026(6) 0.0115(5) 0.0102(5) S6 0.0383(6) 0.0539(6) 0.0382(6) 0.0125(5) 0.0099(5) 0.0060(5) S7 0.0723(9) 0.0625(7) 0.0338(6) 0.0093(6) -0.0015(6) 0.0071(6) S8 0.0491(7) 0.0471(6) 0.0540(7) 0.0027(5) 0.0231(6) 0.0016(5) C1 0.031(2) 0.034(2) 0.031(2) -0.0015(17) 0.0025(18) 0.0003(16) C2 0.033(2) 0.035(2) 0.030(2) -0.0010(17) 0.0012(18) 0.0015(17) C3 0.036(2) 0.033(2) 0.037(2) -0.0036(18) 0.0080(19) -0.0008(17) C4 0.033(2) 0.035(2) 0.030(2) 0.0041(17) 0.0068(18) 0.0002(17) C5 0.046(3) 0.032(2) 0.029(2) -0.0008(17) 0.0059(19) -0.0018(18) C6 0.039(2) 0.0300(19) 0.030(2) -0.0004(17) 0.0065(19) -0.0011(17) C7 0.049(3) 0.045(2) 0.041(2) -0.002(2) 0.016(2) 0.003(2) C8 0.046(3) 0.044(2) 0.042(2) 0.002(2) 0.015(2) -0.003(2) C9 0.069(4) 0.107(4) 0.032(3) 0.011(3) 0.001(2) -0.032(3) C10 0.072(4) 0.062(3) 0.057(3) -0.013(3) 0.020(3) -0.007(3) S9 0.0344(6) 0.0550(6) 0.0295(5) 0.0085(5) 0.0056(5) 0.0132(5) S10 0.0341(6) 0.0477(6) 0.0322(6) 0.0071(5) 0.0071(5) 0.0109(5) S11 0.0341(6) 0.0550(6) 0.0293(5) 0.0067(5) 0.0074(5) 0.0147(5) S12 0.0339(6) 0.0445(6) 0.0339(5) 0.0053(5) 0.0061(5) 0.0099(5) S13 0.0437(7) 0.0897(9) 0.0440(7) 0.0235(6) 0.0190(6) 0.0293(6) S14 0.0350(6) 0.0618(7) 0.0435(6) 0.0260(5) 0.0087(5) 0.0069(5) S15 0.0635(8) 0.0580(7) 0.0341(6) 0.0134(5) 0.0154(6) 0.0233(6) S16 0.0356(6) 0.0450(6) 0.0458(6) 0.0022(5) 0.0164(5) 0.0069(5) C11 0.030(2) 0.037(2) 0.0261(19) 0.0019(17) 0.0042(17) 0.0045(17) C12 0.031(2) 0.039(2) 0.0255(19) -0.0022(17) 0.0023(17) 0.0057(17) C13 0.033(2) 0.0349(19) 0.030(2) 0.0078(17) 0.0080(18) 0.0066(17) C14 0.031(2) 0.036(2) 0.029(2) 0.0065(17) 0.0037(18) 0.0009(17) C15 0.031(2) 0.035(2) 0.031(2) 0.0025(17) 0.0077(18) 0.0053(17) C16 0.034(2) 0.0312(19) 0.030(2) -0.0001(16) 0.0100(18) -0.0026(16) C17A 0.053(8) 0.052(5) 0.024(6) 0.010(5) 0.009(5) 0.026(5) C18A 0.036(4) 0.044(5) 0.031(3) 0.012(3) 0.012(3) 0.002(3) C17B 0.07(2) 0.14(3) 0.039(16) -0.019(15) 0.016(14) 0.019(19) C18B 0.104(18) 0.078(18) 0.023(8) 0.007(10) 0.022(10) 0.008(14) C19A 0.034(6) 0.062(7) 0.036(4) 0.003(5) 0.016(4) 0.001(4) C20A 0.052(6) 0.040(6) 0.030(4) -0.006(4) 0.015(4) 0.003(4) C19B 0.058(15) 0.09(2) 0.034(10) -0.023(13) 0.016(9) -0.030(13) C20B 0.085(17) 0.048(12) 0.057(11) 0.004(9) 0.049(11) -0.002(11) Fe1 0.0451(5) 0.0395(4) 0.0283(4) 0.000 0.0064(4) 0.000 C21 0.047(3) 0.045(2) 0.043(3) -0.004(2) 0.016(2) -0.004(2) C22 0.041(3) 0.050(3) 0.038(2) 0.012(2) 0.007(2) 0.013(2) C23 0.043(3) 0.044(2) 0.036(2) 0.006(2) 0.002(2) 0.008(2) O1 0.065(2) 0.0427(16) 0.0363(16) -0.0029(13) -0.0003(15) 0.0001(14) O2 0.079(2) 0.0482(18) 0.076(2) -0.0193(17) 0.012(2) -0.0086(17) O3 0.0474(18) 0.0519(16) 0.0348(16) -0.0043(14) 0.0113(14) -0.0003(14) O4 0.0466(18) 0.0550(17) 0.0342(16) -0.0063(13) 0.0136(14) -0.0068(14) O5 0.056(2) 0.079(2) 0.0473(19) 0.0042(17) 0.0224(17) -0.0065(17) O6 0.051(2) 0.067(2) 0.0500(19) -0.0066(17) 0.0006(16) -0.0160(17) Br1 0.1609(10) 0.0571(5) 0.0793(6) 0.000 0.0687(7) 0.000 C24 0.073(5) 0.053(4) 0.040(4) 0.000 -0.006(4) 0.000 C25 0.065(4) 0.065(3) 0.056(3) -0.003(3) -0.017(3) 0.009(3) C26 0.071(4) 0.076(4) 0.101(5) -0.014(4) -0.036(4) 0.019(3) C27 0.092(8) 0.057(5) 0.160(10) 0.000 -0.054(7) 0.000 O1W 0.077(4) 0.065(3) 0.097(4) 0.000 0.027(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.740(4) . ? S1 C3 1.750(4) . ? S2 C1 1.738(4) . ? S2 C4 1.744(3) . ? S3 C2 1.734(4) . ? S3 C5 1.747(4) . ? S4 C2 1.739(4) . ? S4 C6 1.744(4) . ? S5 C3 1.744(4) . ? S5 C7 1.805(4) . ? S6 C4 1.747(4) . ? S6 C8 1.799(4) . ? S7 C5 1.748(4) . ? S7 C9 1.815(5) . ? S8 C6 1.739(4) . ? S8 C10 1.767(5) . ? C1 C2 1.363(5) . ? C3 C4 1.351(5) . ? C5 C6 1.345(5) . ? C7 C8 1.518(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.495(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? S9 C13 1.742(4) . ? S9 C11 1.743(4) . ? S10 C11 1.734(4) . ? S10 C14 1.754(3) . ? S11 C12 1.734(4) . ? S11 C15 1.751(3) . ? S12 C16 1.740(4) . ? S12 C12 1.743(3) . ? S13 C17B 1.62(3) . ? S13 C13 1.737(3) . ? S13 C17A 1.848(12) . ? S14 C14 1.752(4) . ? S14 C18A 1.770(6) . ? S14 C18B 1.88(2) . ? S15 C15 1.740(4) . ? S15 C19A 1.780(10) . ? S15 C19B 1.81(3) . ? S16 C16 1.740(3) . ? S16 C20B 1.74(2) . ? S16 C20A 1.844(9) . ? C11 C12 1.361(5) . ? C13 C14 1.344(5) . ? C15 C16 1.349(5) . ? C17A C18A 1.515(16) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C17B C18B 1.45(5) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C19A C20A 1.51(2) . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C20A H20A 0.9700 . ? C20A H20B 0.9700 . ? C19B C20B 1.52(5) . ? C19B H19C 0.9700 . ? C19B H19D 0.9700 . ? C20B H20C 0.9700 . ? C20B H20D 0.9700 . ? Fe1 O4 2.009(3) . ? Fe1 O4 2.009(3) 2_755 ? Fe1 O3 2.011(2) . ? Fe1 O3 2.011(2) 2_755 ? Fe1 O1 2.019(3) . ? Fe1 O1 2.019(3) 2_755 ? C21 O2 1.233(5) . ? C21 O1 1.278(5) . ? C21 C21 1.549(9) 2_755 ? C22 O5 1.231(5) . ? C22 O3 1.273(5) . ? C22 C23 1.557(6) . ? C23 O6 1.215(5) . ? C23 O4 1.283(5) . ? Br1 C24 1.902(6) . ? C24 C25 1.385(5) 2_655 ? C24 C25 1.385(5) . ? C25 C26 1.359(6) . ? C25 H25 0.9300 . ? C26 C27 1.406(6) . ? C26 H26 0.9300 . ? C27 C26 1.406(6) 2_655 ? C27 H27 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C3 95.34(17) . . ? C1 S2 C4 95.61(17) . . ? C2 S3 C5 95.19(18) . . ? C2 S4 C6 95.60(18) . . ? C3 S5 C7 102.12(19) . . ? C4 S6 C8 101.53(19) . . ? C5 S7 C9 102.2(2) . . ? C6 S8 C10 99.3(2) . . ? C2 C1 S2 121.8(3) . . ? C2 C1 S1 123.1(3) . . ? S2 C1 S1 115.12(19) . . ? C1 C2 S3 122.7(3) . . ? C1 C2 S4 122.2(3) . . ? S3 C2 S4 115.2(2) . . ? C4 C3 S5 129.2(3) . . ? C4 C3 S1 117.0(3) . . ? S5 C3 S1 113.8(2) . . ? C3 C4 S2 117.0(3) . . ? C3 C4 S6 127.7(3) . . ? S2 C4 S6 115.3(2) . . ? C6 C5 S3 117.5(3) . . ? C6 C5 S7 128.5(3) . . ? S3 C5 S7 113.9(2) . . ? C5 C6 S8 127.9(3) . . ? C5 C6 S4 116.6(3) . . ? S8 C6 S4 115.5(2) . . ? C8 C7 S5 113.8(3) . . ? C8 C7 H7A 108.8 . . ? S5 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? S5 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 S6 115.0(3) . . ? C7 C8 H8A 108.5 . . ? S6 C8 H8A 108.5 . . ? C7 C8 H8B 108.5 . . ? S6 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 S7 114.6(3) . . ? C10 C9 H9A 108.6 . . ? S7 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? S7 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C9 C10 S8 114.2(3) . . ? C9 C10 H10A 108.7 . . ? S8 C10 H10A 108.7 . . ? C9 C10 H10B 108.7 . . ? S8 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C13 S9 C11 95.23(17) . . ? C11 S10 C14 95.35(17) . . ? C12 S11 C15 95.30(17) . . ? C16 S12 C12 95.03(17) . . ? C17B S13 C13 104.1(15) . . ? C13 S13 C17A 101.6(5) . . ? C14 S14 C18A 102.9(2) . . ? C14 S14 C18B 95.9(6) . . ? C15 S15 C19A 105.6(4) . . ? C15 S15 C19B 95.7(11) . . ? C16 S16 C20B 107.9(7) . . ? C16 S16 C20A 96.2(4) . . ? C12 C11 S10 122.9(3) . . ? C12 C11 S9 121.9(3) . . ? S10 C11 S9 115.20(19) . . ? C11 C12 S11 122.2(3) . . ? C11 C12 S12 122.6(3) . . ? S11 C12 S12 115.22(19) . . ? C14 C13 S13 128.4(3) . . ? C14 C13 S9 117.5(3) . . ? S13 C13 S9 114.1(2) . . ? C13 C14 S14 127.9(3) . . ? C13 C14 S10 116.7(3) . . ? S14 C14 S10 115.3(2) . . ? C16 C15 S15 127.5(3) . . ? C16 C15 S11 116.6(3) . . ? S15 C15 S11 115.8(2) . . ? C15 C16 S16 125.5(3) . . ? C15 C16 S12 117.5(3) . . ? S16 C16 S12 116.8(2) . . ? C18A C17A S13 112.3(8) . . ? C18A C17A H17A 109.1 . . ? S13 C17A H17A 109.1 . . ? C18A C17A H17B 109.1 . . ? S13 C17A H17B 109.1 . . ? H17A C17A H17B 107.9 . . ? C17A C18A S14 114.5(8) . . ? C17A C18A H18A 108.6 . . ? S14 C18A H18A 108.6 . . ? C17A C18A H18B 108.6 . . ? S14 C18A H18B 108.6 . . ? H18A C18A H18B 107.6 . . ? C18B C17B S13 118(3) . . ? C18B C17B H17C 107.9 . . ? S13 C17B H17C 107.9 . . ? C18B C17B H17D 107.9 . . ? S13 C17B H17D 107.9 . . ? H17C C17B H17D 107.2 . . ? C17B C18B S14 115(2) . . ? C17B C18B H18C 108.5 . . ? S14 C18B H18C 108.5 . . ? C17B C18B H18D 108.5 . . ? S14 C18B H18D 108.5 . . ? H18C C18B H18D 107.5 . . ? C20A C19A S15 115.9(9) . . ? C20A C19A H19A 108.3 . . ? S15 C19A H19A 108.3 . . ? C20A C19A H19B 108.3 . . ? S15 C19A H19B 108.3 . . ? H19A C19A H19B 107.4 . . ? C19A C20A S16 112.4(9) . . ? C19A C20A H20A 109.1 . . ? S16 C20A H20A 109.1 . . ? C19A C20A H20B 109.1 . . ? S16 C20A H20B 109.1 . . ? H20A C20A H20B 107.9 . . ? C20B C19B S15 116(2) . . ? C20B C19B H19C 108.2 . . ? S15 C19B H19C 108.2 . . ? C20B C19B H19D 108.2 . . ? S15 C19B H19D 108.2 . . ? H19C C19B H19D 107.3 . . ? C19B C20B S16 114.5(19) . . ? C19B C20B H20C 108.6 . . ? S16 C20B H20C 108.6 . . ? C19B C20B H20D 108.6 . . ? S16 C20B H20D 108.6 . . ? H20C C20B H20D 107.6 . . ? O4 Fe1 O4 99.82(16) . 2_755 ? O4 Fe1 O3 80.59(11) . . ? O4 Fe1 O3 87.74(11) 2_755 . ? O4 Fe1 O3 87.74(11) . 2_755 ? O4 Fe1 O3 80.59(11) 2_755 2_755 ? O3 Fe1 O3 161.88(16) . 2_755 ? O4 Fe1 O1 168.30(12) . . ? O4 Fe1 O1 90.46(12) 2_755 . ? O3 Fe1 O1 94.34(11) . . ? O3 Fe1 O1 99.54(11) 2_755 . ? O4 Fe1 O1 90.46(12) . 2_755 ? O4 Fe1 O1 168.30(12) 2_755 2_755 ? O3 Fe1 O1 99.54(11) . 2_755 ? O3 Fe1 O1 94.34(11) 2_755 2_755 ? O1 Fe1 O1 79.93(16) . 2_755 ? O2 C21 O1 125.6(4) . . ? O2 C21 C21 120.3(3) . 2_755 ? O1 C21 C21 114.1(2) . 2_755 ? O5 C22 O3 126.0(4) . . ? O5 C22 C23 119.0(4) . . ? O3 C22 C23 115.0(3) . . ? O6 C23 O4 126.3(4) . . ? O6 C23 C22 120.7(4) . . ? O4 C23 C22 113.0(4) . . ? C21 O1 Fe1 115.9(3) . . ? C22 O3 Fe1 114.9(2) . . ? C23 O4 Fe1 116.0(3) . . ? C25 C24 C25 124.0(6) 2_655 . ? C25 C24 Br1 118.0(3) 2_655 . ? C25 C24 Br1 118.0(3) . . ? C26 C25 C24 117.9(5) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C26 120.6(8) . 2_655 ? C26 C27 H27 119.7 . . ? C26 C27 H27 119.7 2_655 . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.746 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.117