Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author 'Jianhui Liu' _publ_contact_author_address ; Dalian University of technology, Zhongshan Road 158-46, 116012 Dalian, P. R. China, Fax: +86-411-83702185 ; _publ_contact_author_email liujh@dlut.edu.cn _publ_section_title ; Fe-S complexes containing five-membered heterocycles: novel models for the active site of hydrogenases with unusual low reduction potential ; _publ_contact_author_name 'Jianhui Liu' loop_ _publ_author_name 'Jian-Hui Liu.' B.Akermark 'Shi Jiang.' 'Yu Shi.' 'Licheng Sun.' 'Zhen Wang.' data_furan _database_code_depnum_ccdc_archive 'CCDC 245082' #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _audit_creation_date 'Mar 10 21:12:03 2005' _audit_creation_method SHELXL-97 _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #------------------------------------------------------------------------------ _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H9 Fe2 N O7 S2' _chemical_formula_sum 'C13 H9 Fe2 N O7 S2' _chemical_formula_weight 467.03 #------------------------------------------------------------------------------ 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 triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5684(15) _cell_length_b 10.878(2) _cell_length_c 12.426(3) _cell_angle_alpha 111.59(3) _cell_angle_beta 96.93(3) _cell_angle_gamma 108.30(3) _cell_volume 870.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3567 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 17.84 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 1.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5498 _exptl_absorpt_correction_T_max 0.8005 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAPID IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7286 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3804 _reflns_number_gt 3361 _reflns_threshold_expression >2sigma(I) #------------------------------------------------------------------------------ _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^)+(0.0819P)^2^+0.0589P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3804 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.46703(4) 0.69757(4) 0.30370(3) 0.02799(12) Uani 1 1 d . . . Fe2 Fe -0.16947(4) 0.67002(3) 0.38659(3) 0.02465(11) Uani 1 1 d . . . S1 S -0.47262(8) 0.52800(6) 0.36601(5) 0.03059(15) Uani 1 1 d . . . S2 S -0.28024(8) 0.61750(6) 0.19184(5) 0.02607(14) Uani 1 1 d . . . N N -0.3956(3) 0.3435(2) 0.17516(19) 0.0320(4) Uani 1 1 d . . . O1 O -0.2965(3) 0.9657(2) 0.2795(2) 0.0531(5) Uani 1 1 d . . . O2 O -0.5577(3) 0.8390(3) 0.52855(19) 0.0558(6) Uani 1 1 d . . . O3 O -0.8508(3) 0.5585(2) 0.13225(19) 0.0515(5) Uani 1 1 d . . . O4 O -0.1270(3) 0.7981(2) 0.64567(16) 0.0441(4) Uani 1 1 d . . . O5 O 0.0426(3) 0.4812(2) 0.37066(19) 0.0467(5) Uani 1 1 d . . . O6 O 0.1347(3) 0.9292(2) 0.40859(18) 0.0447(4) Uani 1 1 d . . . O7 O -0.3324(3) 0.1383(2) -0.08064(19) 0.0508(5) Uani 1 1 d . . . C1 C -0.3662(4) 0.8623(3) 0.2878(2) 0.0367(5) Uani 1 1 d . . . C2 C -0.5252(4) 0.7847(3) 0.4399(2) 0.0380(5) Uani 1 1 d . . . C3 C -0.7022(4) 0.6144(3) 0.1981(2) 0.0358(5) Uani 1 1 d . . . C4 C -0.1422(3) 0.7470(3) 0.5453(2) 0.0321(5) Uani 1 1 d . . . C5 C -0.0405(3) 0.5523(3) 0.3759(2) 0.0327(5) Uani 1 1 d . . . C6 C 0.0184(3) 0.8274(3) 0.4001(2) 0.0309(5) Uani 1 1 d . . . C7 C -0.5390(4) 0.3533(3) 0.2415(2) 0.0380(5) Uani 1 1 d . . . H7C H -0.5618 0.2815 0.2725 0.046 Uiso 1 1 calc R . . H7A H -0.6593 0.3309 0.1867 0.046 Uiso 1 1 calc R . . C8 C -0.3842(4) 0.4231(3) 0.1041(2) 0.0334(5) Uani 1 1 d . . . H8A H -0.5132 0.3951 0.0560 0.040 Uiso 1 1 calc R . . H8B H -0.3071 0.3971 0.0494 0.040 Uiso 1 1 calc R . . C9 C -0.4340(4) 0.1916(3) 0.1026(3) 0.0434(6) Uani 1 1 d . . . H9A H -0.5586 0.1474 0.0441 0.052 Uiso 1 1 calc R . . H9B H -0.4417 0.1431 0.1547 0.052 Uiso 1 1 calc R . . C10 C -0.2852(4) 0.1697(2) 0.0385(2) 0.0345(5) Uani 1 1 d . . . C11 C -0.1128(4) 0.1675(4) 0.0700(3) 0.0514(7) Uani 1 1 d . . . H11A H -0.0489 0.1844 0.1460 0.062 Uiso 1 1 calc R . . C12 C -0.0443(5) 0.1344(4) -0.0346(3) 0.0605(9) Uani 1 1 d . . . H12A H 0.0729 0.1255 -0.0404 0.073 Uiso 1 1 calc R . . C13 C -0.1795(6) 0.1188(4) -0.1215(3) 0.0590(8) Uani 1 1 d . . . H13A H -0.1718 0.0974 -0.2000 0.071 Uiso 1 1 calc R . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02633(19) 0.0346(2) 0.02550(19) 0.01283(15) 0.00671(13) 0.01511(14) Fe2 0.02422(18) 0.03020(19) 0.02236(18) 0.01299(14) 0.00678(12) 0.01189(13) S1 0.0282(3) 0.0399(3) 0.0289(3) 0.0189(2) 0.0123(2) 0.0130(2) S2 0.0294(3) 0.0287(3) 0.0229(3) 0.0131(2) 0.0088(2) 0.0117(2) N 0.0341(10) 0.0284(10) 0.0333(10) 0.0141(8) 0.0132(8) 0.0097(8) O1 0.0538(12) 0.0404(11) 0.0642(14) 0.0252(10) 0.0110(10) 0.0157(9) O2 0.0544(12) 0.0719(15) 0.0403(11) 0.0123(11) 0.0211(9) 0.0346(11) O3 0.0319(10) 0.0677(14) 0.0465(12) 0.0241(10) -0.0004(8) 0.0135(9) O4 0.0511(11) 0.0514(12) 0.0255(9) 0.0142(8) 0.0098(8) 0.0174(9) O5 0.0491(11) 0.0542(12) 0.0557(12) 0.0303(10) 0.0183(9) 0.0343(10) O6 0.0412(10) 0.0379(10) 0.0451(11) 0.0177(8) 0.0095(8) 0.0039(8) O7 0.0653(13) 0.0577(13) 0.0368(10) 0.0226(9) 0.0100(9) 0.0318(10) C1 0.0347(12) 0.0408(14) 0.0345(13) 0.0127(11) 0.0066(10) 0.0196(10) C2 0.0321(12) 0.0466(14) 0.0384(13) 0.0168(11) 0.0097(10) 0.0211(11) C3 0.0369(13) 0.0437(14) 0.0333(12) 0.0198(11) 0.0118(10) 0.0189(11) C4 0.0297(11) 0.0371(13) 0.0323(12) 0.0175(10) 0.0073(9) 0.0140(9) C5 0.0351(12) 0.0383(13) 0.0310(12) 0.0197(10) 0.0106(9) 0.0156(10) C6 0.0318(11) 0.0347(12) 0.0247(11) 0.0112(9) 0.0052(8) 0.0138(9) C7 0.0349(12) 0.0337(13) 0.0418(14) 0.0170(11) 0.0148(10) 0.0064(10) C8 0.0405(13) 0.0296(12) 0.0244(11) 0.0075(9) 0.0071(9) 0.0120(9) C9 0.0430(14) 0.0264(12) 0.0519(16) 0.0109(12) 0.0153(12) 0.0085(10) C10 0.0415(13) 0.0248(11) 0.0310(12) 0.0089(9) 0.0062(10) 0.0103(9) C11 0.0504(17) 0.0586(18) 0.0399(15) 0.0154(14) 0.0045(12) 0.0242(14) C12 0.0511(18) 0.063(2) 0.066(2) 0.0198(17) 0.0232(16) 0.0279(16) C13 0.092(3) 0.0581(19) 0.0474(18) 0.0287(15) 0.0379(17) 0.0401(18) #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.794(3) . ? Fe1 C3 1.806(3) . ? Fe1 C1 1.808(3) . ? Fe1 S1 2.2391(8) . ? Fe1 S2 2.2464(9) . ? Fe1 Fe2 2.5127(8) . ? Fe2 C6 1.784(3) . ? Fe2 C4 1.792(3) . ? Fe2 C5 1.817(3) . ? Fe2 S1 2.2489(11) . ? Fe2 S2 2.2535(9) . ? S1 C7 1.818(3) . ? S2 C8 1.825(3) . ? N C8 1.439(3) . ? N C7 1.447(3) . ? N C9 1.472(3) . ? O1 C1 1.131(3) . ? O2 C2 1.140(3) . ? O3 C3 1.134(3) . ? O4 C4 1.137(3) . ? O5 C5 1.130(3) . ? O6 C6 1.136(3) . ? O7 C13 1.363(4) . ? O7 C10 1.363(3) . ? C7 H7C 0.9700 . ? C7 H7A 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.485(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.327(4) . ? C11 C12 1.422(5) . ? C11 H11A 0.9300 . ? C12 C13 1.315(5) . ? C12 H12A 0.9300 . ? C13 H13A 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 C2 Fe1 C3 100.24(12) . . ? C2 Fe1 C1 92.90(13) . . ? C3 Fe1 C1 101.02(12) . . ? C2 Fe1 S1 86.19(9) . . ? C3 Fe1 S1 101.24(9) . . ? C1 Fe1 S1 157.52(8) . . ? C2 Fe1 S2 155.85(8) . . ? C3 Fe1 S2 103.50(9) . . ? C1 Fe1 S2 86.90(9) . . ? S1 Fe1 S2 84.94(3) . . ? C2 Fe1 Fe2 100.50(8) . . ? C3 Fe1 Fe2 147.83(8) . . ? C1 Fe1 Fe2 102.19(8) . . ? S1 Fe1 Fe2 56.14(3) . . ? S2 Fe1 Fe2 56.19(2) . . ? C6 Fe2 C4 91.13(12) . . ? C6 Fe2 C5 100.93(11) . . ? C4 Fe2 C5 99.98(11) . . ? C6 Fe2 S1 156.50(8) . . ? C4 Fe2 S1 87.38(9) . . ? C5 Fe2 S1 102.42(8) . . ? C6 Fe2 S2 88.28(9) . . ? C4 Fe2 S2 158.11(8) . . ? C5 Fe2 S2 101.61(8) . . ? S1 Fe2 S2 84.55(5) . . ? C6 Fe2 Fe1 102.00(8) . . ? C4 Fe2 Fe1 102.99(8) . . ? C5 Fe2 Fe1 146.98(8) . . ? S1 Fe2 Fe1 55.77(3) . . ? S2 Fe2 Fe1 55.92(3) . . ? C7 S1 Fe1 112.29(9) . . ? C7 S1 Fe2 109.57(9) . . ? Fe1 S1 Fe2 68.09(3) . . ? C8 S2 Fe1 112.83(9) . . ? C8 S2 Fe2 109.24(9) . . ? Fe1 S2 Fe2 67.89(3) . . ? C8 N C7 112.3(2) . . ? C8 N C9 112.4(2) . . ? C7 N C9 109.45(19) . . ? C13 O7 C10 106.1(2) . . ? O1 C1 Fe1 177.4(2) . . ? O2 C2 Fe1 177.6(2) . . ? O3 C3 Fe1 177.9(2) . . ? O4 C4 Fe2 178.2(2) . . ? O5 C5 Fe2 178.7(3) . . ? O6 C6 Fe2 178.3(2) . . ? N C7 S1 114.20(17) . . ? N C7 H7C 108.7 . . ? S1 C7 H7C 108.7 . . ? N C7 H7A 108.7 . . ? S1 C7 H7A 108.7 . . ? H7C C7 H7A 107.6 . . ? N C8 S2 114.23(16) . . ? N C8 H8A 108.7 . . ? S2 C8 H8A 108.7 . . ? N C8 H8B 108.7 . . ? S2 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N C9 C10 113.7(2) . . ? N C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 O7 109.8(2) . . ? C11 C10 C9 134.0(3) . . ? O7 C10 C9 116.1(2) . . ? C10 C11 C12 106.9(3) . . ? C10 C11 H11A 126.6 . . ? C12 C11 H11A 126.6 . . ? C13 C12 C11 106.4(3) . . ? C13 C12 H12A 126.8 . . ? C11 C12 H12A 126.8 . . ? C12 C13 O7 110.7(3) . . ? C12 C13 H13A 124.6 . . ? O7 C13 H13A 124.6 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.485 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.158 #===END # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 266225 data_thiophene _database_code_depnum_ccdc_archive 'CCDC 266225' #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ? #------------------------------------------------------------------------------ _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #------------------------------------------------------------------------------ _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H9 Fe2 N O6 S3' _chemical_formula_sum 'C13 H9 Fe2 N O6 S3' _chemical_formula_weight 483.09 #------------------------------------------------------------------------------ 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 C2/c #------------------------------------------------------------------------------ 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 25.2878(17) _cell_length_b 7.5720(5) _cell_length_c 22.6997(15) _cell_angle_alpha 90.00 _cell_angle_beta 121.1030(10) _cell_angle_gamma 90.00 _cell_volume 3721.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5167 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 28.05 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6607 _exptl_absorpt_correction_T_max 0.9066 _exptl_absorpt_process_details SADABS #------------------------------------------------------------------------------ _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11269 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4356 _reflns_number_gt 3514 _reflns_threshold_expression >2sigma(I) #------------------------------------------------------------------------------ _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^)+(0.0875P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4356 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.66347(2) 0.12891(6) 0.33920(2) 0.04488(15) Uani 1 1 d . . . Fe2 Fe 0.695375(19) 0.43084(5) 0.32317(2) 0.04017(15) Uani 1 1 d . . . S1 S 0.68368(3) 0.19711(10) 0.25628(4) 0.0452(2) Uani 1 1 d . . . S2 S 0.59957(3) 0.36307(10) 0.29874(4) 0.04339(19) Uani 1 1 d . . . S3 S 0.52445(6) 0.7593(2) 0.08747(8) 0.1030(4) Uani 1 1 d . . . N N 0.57468(13) 0.3673(4) 0.16488(13) 0.0483(6) Uani 1 1 d . . . O1 O 0.57320(16) -0.1609(4) 0.2815(2) 0.0942(10) Uani 1 1 d . . . O2 O 0.66999(18) 0.1752(5) 0.47097(16) 0.0980(11) Uani 1 1 d . . . O3 O 0.77950(15) -0.0711(5) 0.40075(19) 0.0965(10) Uani 1 1 d . . . O4 O 0.71084(16) 0.6189(4) 0.44343(16) 0.0856(9) Uani 1 1 d . . . O5 O 0.83014(12) 0.4033(4) 0.39168(15) 0.0777(8) Uani 1 1 d . . . O6 O 0.67315(13) 0.7314(4) 0.23036(15) 0.0729(7) Uani 1 1 d . . . C1 C 0.60841(17) -0.0511(5) 0.3035(2) 0.0612(9) Uani 1 1 d . . . C2 C 0.66686(19) 0.1543(5) 0.4195(2) 0.0624(9) Uani 1 1 d . . . C3 C 0.73431(17) 0.0073(5) 0.37832(19) 0.0634(9) Uani 1 1 d . . . C4 C 0.70473(17) 0.5470(5) 0.39633(18) 0.0550(8) Uani 1 1 d . . . C5 C 0.77770(17) 0.4119(5) 0.36380(17) 0.0534(8) Uani 1 1 d . . . C6 C 0.68155(16) 0.6135(5) 0.26541(18) 0.0509(7) Uani 1 1 d . . . C7 C 0.61331(15) 0.2187(5) 0.17254(16) 0.0541(8) Uani 1 1 d . . . H7A H 0.6246 0.2273 0.1378 0.065 Uiso 1 1 calc R . . H7B H 0.5892 0.1116 0.1634 0.065 Uiso 1 1 calc R . . C8 C 0.54657(14) 0.3484(5) 0.20590(16) 0.0523(8) Uani 1 1 d . . . H8A H 0.5258 0.2349 0.1955 0.063 Uiso 1 1 calc R . . H8B H 0.5153 0.4391 0.1923 0.063 Uiso 1 1 calc R . . C9 C 0.52676(19) 0.3906(5) 0.09167(18) 0.0636(9) Uani 1 1 d . . . H9A H 0.4980 0.2925 0.0775 0.076 Uiso 1 1 calc R . . H9B H 0.5463 0.3862 0.0645 0.076 Uiso 1 1 calc R . . C10 C 0.49154(17) 0.5581(5) 0.07628(17) 0.0579(8) Uani 1 1 d . . . C11 C 0.42582(14) 0.5676(5) 0.04495(17) 0.0510(7) Uani 1 1 d . . . H11A H 0.3990 0.4728 0.0343 0.061 Uiso 1 1 calc R . . C12 C 0.4090(2) 0.7531(6) 0.0329(3) 0.0825(12) Uani 1 1 d . . . H12A H 0.3685 0.7927 0.0127 0.099 Uiso 1 1 calc R . . C13 C 0.4570(3) 0.8614(7) 0.0534(3) 0.1013(17) Uani 1 1 d . . . H13A H 0.4529 0.9835 0.0490 0.122 Uiso 1 1 calc R . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0440(3) 0.0429(3) 0.0452(3) 0.00464(17) 0.0212(2) 0.00039(17) Fe2 0.0422(2) 0.0422(2) 0.0397(2) -0.00246(16) 0.02366(19) -0.00292(17) S1 0.0419(4) 0.0496(4) 0.0468(4) -0.0051(3) 0.0249(3) 0.0035(3) S2 0.0429(4) 0.0506(4) 0.0439(4) 0.0040(3) 0.0276(3) 0.0044(3) S3 0.0759(8) 0.0831(8) 0.1086(10) -0.0059(7) 0.0184(7) -0.0153(7) N 0.0496(15) 0.0569(16) 0.0373(12) 0.0016(11) 0.0217(11) 0.0076(12) O1 0.072(2) 0.0725(19) 0.128(3) -0.0124(19) 0.045(2) -0.0191(16) O2 0.134(3) 0.112(3) 0.0614(18) 0.0188(17) 0.060(2) 0.014(2) O3 0.0594(18) 0.096(2) 0.109(3) 0.026(2) 0.0255(18) 0.0242(17) O4 0.106(3) 0.090(2) 0.0724(19) -0.0351(16) 0.0546(19) -0.0227(17) O5 0.0447(15) 0.116(2) 0.0665(17) -0.0113(15) 0.0246(13) -0.0077(14) O6 0.0797(18) 0.0679(17) 0.0787(17) 0.0237(14) 0.0464(16) 0.0028(14) C1 0.0515(19) 0.0503(19) 0.078(2) 0.0031(17) 0.0306(18) -0.0011(16) C2 0.070(2) 0.060(2) 0.057(2) 0.0146(17) 0.0329(19) 0.0051(18) C3 0.055(2) 0.058(2) 0.062(2) 0.0098(17) 0.0203(17) 0.0025(17) C4 0.059(2) 0.0569(19) 0.0526(18) -0.0065(15) 0.0317(16) -0.0088(16) C5 0.054(2) 0.063(2) 0.0451(17) -0.0069(14) 0.0274(15) -0.0088(15) C6 0.0509(18) 0.0551(19) 0.0536(18) -0.0051(15) 0.0318(16) -0.0035(14) C7 0.0552(18) 0.062(2) 0.0409(16) -0.0088(14) 0.0219(15) 0.0061(15) C8 0.0374(15) 0.069(2) 0.0462(17) 0.0059(15) 0.0187(14) 0.0035(14) C9 0.069(2) 0.069(2) 0.0406(17) -0.0006(15) 0.0191(16) 0.0052(18) C10 0.062(2) 0.063(2) 0.0399(16) 0.0025(14) 0.0195(15) -0.0011(16) C11 0.0389(15) 0.0594(19) 0.0486(17) 0.0165(14) 0.0182(13) 0.0056(13) C12 0.062(2) 0.080(3) 0.087(3) 0.005(2) 0.026(2) 0.008(2) C13 0.112(4) 0.061(3) 0.093(4) 0.000(2) 0.027(3) 0.011(3) #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C3 1.789(4) . ? Fe1 C2 1.791(4) . ? Fe1 C1 1.813(4) . ? Fe1 S1 2.2504(9) . ? Fe1 S2 2.2505(9) . ? Fe1 Fe2 2.5126(6) . ? Fe2 C4 1.784(3) . ? Fe2 C5 1.795(4) . ? Fe2 C6 1.811(4) . ? Fe2 S2 2.2476(8) . ? Fe2 S1 2.2498(8) . ? S1 C7 1.820(3) . ? S2 C8 1.825(3) . ? S3 C13 1.656(6) . ? S3 C10 1.692(4) . ? N C7 1.441(4) . ? N C8 1.441(4) . ? N C9 1.477(4) . ? O1 C1 1.129(5) . ? O2 C2 1.140(4) . ? O3 C3 1.147(5) . ? O4 C4 1.137(4) . ? O5 C5 1.138(4) . ? O6 C6 1.140(4) . ? C9 C10 1.484(5) . ? C10 C11 1.432(5) . ? C11 C12 1.452(6) . ? C12 C13 1.334(7) . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C2 92.34(18) . . ? C3 Fe1 C1 100.13(17) . . ? C2 Fe1 C1 99.05(18) . . ? C3 Fe1 S1 86.07(13) . . ? C2 Fe1 S1 156.17(13) . . ? C1 Fe1 S1 104.64(13) . . ? C3 Fe1 S2 158.68(13) . . ? C2 Fe1 S2 88.71(12) . . ? C1 Fe1 S2 100.73(12) . . ? S1 Fe1 S2 84.45(3) . . ? C3 Fe1 Fe2 103.06(13) . . ? C2 Fe1 Fe2 101.51(13) . . ? C1 Fe1 Fe2 148.13(12) . . ? S1 Fe1 Fe2 56.05(2) . . ? S2 Fe1 Fe2 55.99(2) . . ? C4 Fe2 C5 90.02(16) . . ? C4 Fe2 C6 100.41(15) . . ? C5 Fe2 C6 99.90(15) . . ? C4 Fe2 S2 87.13(12) . . ? C5 Fe2 S2 157.63(12) . . ? C6 Fe2 S2 102.44(11) . . ? C4 Fe2 S1 157.55(12) . . ? C5 Fe2 S1 89.83(11) . . ? C6 Fe2 S1 101.73(11) . . ? S2 Fe2 S1 84.53(3) . . ? C4 Fe2 Fe1 102.23(11) . . ? C5 Fe2 Fe1 103.11(11) . . ? C6 Fe2 Fe1 147.49(11) . . ? S2 Fe2 Fe1 56.10(2) . . ? S1 Fe2 Fe1 56.07(2) . . ? C7 S1 Fe2 110.56(11) . . ? C7 S1 Fe1 111.85(11) . . ? Fe2 S1 Fe1 67.88(2) . . ? C8 S2 Fe2 110.72(10) . . ? C8 S2 Fe1 111.55(12) . . ? Fe2 S2 Fe1 67.92(3) . . ? C13 S3 C10 92.4(2) . . ? C7 N C8 112.0(3) . . ? C7 N C9 109.9(3) . . ? C8 N C9 110.3(3) . . ? O1 C1 Fe1 178.5(4) . . ? O2 C2 Fe1 177.9(4) . . ? O3 C3 Fe1 177.1(4) . . ? O4 C4 Fe2 179.1(3) . . ? O5 C5 Fe2 177.4(3) . . ? O6 C6 Fe2 178.3(3) . . ? N C7 S1 115.6(2) . . ? N C8 S2 115.3(2) . . ? N C9 C10 114.2(3) . . ? C11 C10 C9 124.1(3) . . ? C11 C10 S3 112.6(3) . . ? C9 C10 S3 123.1(3) . . ? C10 C11 C12 107.1(3) . . ? C13 C12 C11 113.8(4) . . ? C12 C13 S3 114.1(4) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.914 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.098 #===END # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 276211 data_Brthiophene _database_code_depnum_ccdc_archive 'CCDC 276211' #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' #------------------------------------------------------------------------------ _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H8 Br Fe2 N O6 S3' _chemical_formula_sum 'C13 H8 Br Fe2 N O6 S3' _chemical_formula_weight 561.99 #------------------------------------------------------------------------------ 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' 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 P2(1)/c #------------------------------------------------------------------------------ loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.160(4) _cell_length_b 18.101(8) _cell_length_c 12.148(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.265(8) _cell_angle_gamma 90.00 _cell_volume 1901.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1992 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 22.10 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 3.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4826 _exptl_absorpt_correction_T_max 0.8317 _exptl_absorpt_process_details SADABS #------------------------------------------------------------------------------ _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11402 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4300 _reflns_number_gt 2402 _reflns_threshold_expression >2sigma(I) #------------------------------------------------------------------------------ _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^)+(0.0156P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4300 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 0.790 _refine_ls_restrained_S_all 0.790 _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 Br Br 0.80547(8) 0.62395(3) 0.76605(6) 0.0846(2) Uani 1 1 d . . . Fe1 Fe 0.51034(7) 0.17329(3) 0.48526(5) 0.03931(18) Uani 1 1 d . . . Fe2 Fe 0.74089(7) 0.14096(3) 0.42753(5) 0.03658(17) Uani 1 1 d . . . S1 S 0.58103(13) 0.23634(6) 0.35189(10) 0.0409(3) Uani 1 1 d . . . S2 S 0.75728(12) 0.19131(6) 0.60060(9) 0.0385(3) Uani 1 1 d . . . S3 S 0.93437(14) 0.48240(7) 0.68507(11) 0.0502(3) Uani 1 1 d . . . N N 0.8265(4) 0.31470(18) 0.4960(3) 0.0401(9) Uani 1 1 d . . . O5 O 0.5812(4) 0.06828(17) 0.2051(3) 0.0591(9) Uani 1 1 d . . . O6 O 1.0347(4) 0.1881(2) 0.4002(3) 0.0766(12) Uani 1 1 d . . . C1 C 0.3970(5) 0.2366(2) 0.5369(4) 0.0451(12) Uani 1 1 d . . . C2 C 0.5098(5) 0.0972(3) 0.5768(4) 0.0512(13) Uani 1 1 d . . . C3 C 0.3560(6) 0.1363(3) 0.3655(5) 0.0523(12) Uani 1 1 d . . . C4 C 0.8023(5) 0.0556(3) 0.4966(4) 0.0477(12) Uani 1 1 d . . . C5 C 0.6472(5) 0.0954(2) 0.2914(4) 0.0421(11) Uani 1 1 d . . . C6 C 0.9212(6) 0.1709(3) 0.4110(4) 0.0483(12) Uani 1 1 d . . . C7 C 0.6771(5) 0.3225(2) 0.4076(4) 0.0439(11) Uani 1 1 d . . . H7A H 0.6894 0.3504 0.3430 0.053 Uiso 1 1 calc R . . H7B H 0.6110 0.3510 0.4396 0.053 Uiso 1 1 calc R . . C8 C 0.8194(5) 0.2874(2) 0.6048(4) 0.0447(11) Uani 1 1 d . . . H8A H 0.7485 0.3181 0.6289 0.054 Uiso 1 1 calc R . . H8B H 0.9209 0.2923 0.6633 0.054 Uiso 1 1 calc R . . C9 C 0.9237(5) 0.3809(2) 0.5074(4) 0.0505(12) Uani 1 1 d . . . H9A H 0.9378 0.3901 0.4328 0.061 Uiso 1 1 calc R . . H9B H 1.0247 0.3704 0.5635 0.061 Uiso 1 1 calc R . . C10 C 0.8635(5) 0.4503(2) 0.5444(4) 0.0434(11) Uani 1 1 d . . . C11 C 0.7494(6) 0.4949(3) 0.4792(4) 0.0572(14) Uani 1 1 d . . . H11A H 0.6969 0.4872 0.4003 0.069 Uiso 1 1 calc R . . C12 C 0.7179(6) 0.5543(2) 0.5432(5) 0.0586(14) Uani 1 1 d . . . H12A H 0.6417 0.5895 0.5111 0.070 Uiso 1 1 calc R . . C13 C 0.8082(5) 0.5548(2) 0.6534(4) 0.0506(12) Uani 1 1 d . . . O2 O 0.5144(5) 0.04732(19) 0.6359(4) 0.0795(12) Uani 1 1 d . . . O1 O 0.3222(4) 0.27534(19) 0.5688(3) 0.0706(11) Uani 1 1 d . . . O3 O 0.2623(4) 0.1144(2) 0.2852(3) 0.0766(12) Uani 1 1 d . . . O4 O 0.8407(5) -0.0009(2) 0.5397(3) 0.0769(12) Uani 1 1 d . . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br 0.0817(4) 0.0808(4) 0.0924(5) -0.0227(3) 0.0304(4) 0.0020(4) Fe1 0.0330(3) 0.0445(4) 0.0414(4) -0.0020(3) 0.0134(3) -0.0043(3) Fe2 0.0336(3) 0.0434(4) 0.0322(3) -0.0024(3) 0.0100(3) -0.0016(3) S1 0.0394(6) 0.0451(6) 0.0326(6) 0.0009(5) 0.0045(5) -0.0022(5) S2 0.0392(6) 0.0450(6) 0.0296(6) 0.0008(5) 0.0090(5) -0.0042(5) S3 0.0418(7) 0.0552(8) 0.0495(8) 0.0034(6) 0.0095(6) -0.0011(6) N 0.040(2) 0.039(2) 0.040(2) 0.0035(17) 0.0114(18) -0.0060(17) O5 0.057(2) 0.070(2) 0.047(2) -0.0213(18) 0.0122(18) -0.0081(19) O6 0.044(2) 0.107(3) 0.087(3) -0.014(2) 0.034(2) -0.018(2) C1 0.043(3) 0.046(3) 0.043(3) 0.005(2) 0.010(2) -0.004(2) C2 0.041(3) 0.052(3) 0.061(4) -0.008(3) 0.018(3) -0.007(2) C3 0.036(3) 0.065(3) 0.065(4) -0.008(3) 0.027(3) -0.008(2) C4 0.044(3) 0.055(3) 0.041(3) -0.009(2) 0.009(2) 0.001(2) C5 0.039(3) 0.039(3) 0.051(3) 0.002(2) 0.018(2) 0.002(2) C6 0.047(3) 0.056(3) 0.035(3) -0.009(2) 0.005(2) -0.006(3) C7 0.047(3) 0.040(3) 0.046(3) 0.008(2) 0.018(2) -0.001(2) C8 0.042(3) 0.052(3) 0.038(3) -0.004(2) 0.011(2) -0.005(2) C9 0.042(3) 0.062(3) 0.049(3) -0.002(2) 0.016(2) -0.010(2) C10 0.041(3) 0.040(3) 0.047(3) 0.003(2) 0.011(2) -0.013(2) C11 0.065(4) 0.051(3) 0.046(3) 0.004(2) 0.004(3) -0.008(3) C12 0.051(3) 0.041(3) 0.071(4) 0.007(3) 0.002(3) 0.000(2) C13 0.046(3) 0.043(3) 0.062(3) 0.001(2) 0.016(3) -0.008(2) O2 0.091(3) 0.064(2) 0.087(3) 0.023(2) 0.035(2) -0.012(2) O1 0.071(3) 0.075(3) 0.069(3) -0.009(2) 0.027(2) 0.020(2) O3 0.051(2) 0.104(3) 0.068(3) -0.020(2) 0.010(2) -0.031(2) O4 0.085(3) 0.062(2) 0.075(3) 0.012(2) 0.015(2) 0.014(2) #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br C13 1.861(5) . ? Fe1 C2 1.772(5) . ? Fe1 C3 1.790(5) . ? Fe1 C1 1.793(5) . ? Fe1 S1 2.2448(14) . ? Fe1 S2 2.2571(15) . ? Fe1 Fe2 2.5042(12) . ? Fe2 C4 1.760(5) . ? Fe2 C5 1.793(5) . ? Fe2 C6 1.812(5) . ? Fe2 S2 2.2506(15) . ? Fe2 S1 2.2541(14) . ? S1 C7 1.808(4) . ? S2 C8 1.826(4) . ? S3 C13 1.705(5) . ? S3 C10 1.717(5) . ? N C8 1.433(5) . ? N C7 1.441(5) . ? N C9 1.472(5) . ? O5 C5 1.135(5) . ? O6 C6 1.133(5) . ? C1 O1 1.134(5) . ? C2 O2 1.145(5) . ? C3 O3 1.138(5) . ? C4 O4 1.149(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.498(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.351(6) . ? C11 C12 1.411(6) . ? C11 H11A 0.9300 . ? C12 C13 1.321(6) . ? C12 H12A 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 C2 Fe1 C3 93.1(2) . . ? C2 Fe1 C1 98.9(2) . . ? C3 Fe1 C1 97.5(2) . . ? C2 Fe1 S1 155.47(16) . . ? C3 Fe1 S1 86.67(16) . . ? C1 Fe1 S1 105.42(15) . . ? C2 Fe1 S2 86.14(16) . . ? C3 Fe1 S2 156.83(15) . . ? C1 Fe1 S2 105.53(15) . . ? S1 Fe1 S2 84.61(5) . . ? C2 Fe1 Fe2 99.88(15) . . ? C3 Fe1 Fe2 101.41(15) . . ? C1 Fe1 Fe2 152.44(14) . . ? S1 Fe1 Fe2 56.35(4) . . ? S2 Fe1 Fe2 56.13(4) . . ? C4 Fe2 C5 90.9(2) . . ? C4 Fe2 C6 99.0(2) . . ? C5 Fe2 C6 102.2(2) . . ? C4 Fe2 S2 89.89(15) . . ? C5 Fe2 S2 155.79(15) . . ? C6 Fe2 S2 101.55(14) . . ? C4 Fe2 S1 158.35(16) . . ? C5 Fe2 S1 85.82(14) . . ? C6 Fe2 S1 102.64(15) . . ? S2 Fe2 S1 84.54(5) . . ? C4 Fe2 Fe1 103.79(16) . . ? C5 Fe2 Fe1 100.06(14) . . ? C6 Fe2 Fe1 147.69(15) . . ? S2 Fe2 Fe1 56.37(4) . . ? S1 Fe2 Fe1 56.00(4) . . ? C7 S1 Fe1 112.89(15) . . ? C7 S1 Fe2 109.72(15) . . ? Fe1 S1 Fe2 67.65(4) . . ? C8 S2 Fe2 109.65(14) . . ? C8 S2 Fe1 113.22(15) . . ? Fe2 S2 Fe1 67.50(4) . . ? C13 S3 C10 91.7(2) . . ? C8 N C7 113.6(4) . . ? C8 N C9 113.8(3) . . ? C7 N C9 112.7(3) . . ? O1 C1 Fe1 178.2(4) . . ? O2 C2 Fe1 177.6(5) . . ? O3 C3 Fe1 176.0(5) . . ? O4 C4 Fe2 178.7(4) . . ? O5 C5 Fe2 176.6(4) . . ? O6 C6 Fe2 178.5(5) . . ? N C7 S1 114.8(3) . . ? N C7 H7A 108.6 . . ? S1 C7 H7A 108.6 . . ? N C7 H7B 108.6 . . ? S1 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? N C8 S2 114.3(3) . . ? N C8 H8A 108.7 . . ? S2 C8 H8A 108.7 . . ? N C8 H8B 108.7 . . ? S2 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N C9 C10 116.0(4) . . ? N C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? N C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C9 128.0(4) . . ? C11 C10 S3 110.3(4) . . ? C9 C10 S3 121.8(3) . . ? C10 C11 C12 113.1(5) . . ? C10 C11 H11A 123.5 . . ? C12 C11 H11A 123.5 . . ? C13 C12 C11 112.9(4) . . ? C13 C12 H12A 123.5 . . ? C11 C12 H12A 123.5 . . ? C12 C13 S3 112.0(4) . . ? C12 C13 Br 126.4(4) . . ? S3 C13 Br 121.6(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.664 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.097 #===END