data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Xiangfeng Shao' _publ_contact_author_email 'SHAO XF@HOTMAIL.COM' _publ_section_title ; Antiferromagnetic Ordering of the FeBr4 d Spins via Strong pi-d Interaction in a Semiconducting EDT-CP-TTFVS*FeBr4 Salt ; _publ_author_name 'Xiangfeng Shao' # Attachment 'CCDC-715840.cif' data__EDO-CP-TTFVS-FeCl4 _database_code_depnum_ccdc_archive 'CCDC 715840' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C14 H10 Cl4 Fe O2 S7 ' _chemical_formula_moiety 'C14 H10 Cl4 Fe O2 S7 ' _chemical_formula_weight 632.31 _chemical_melting_point '450 K' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.5213(4) _cell_length_b 9.2047(5) _cell_length_c 17.5450(8) _cell_angle_alpha 100.3845(14) _cell_angle_beta 95.2384(12) _cell_angle_gamma 108.5842(16) _cell_volume 1117.96(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9263 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632.00 _exptl_absorpt_coefficient_mu 1.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.547 _exptl_absorpt_correction_T_max 0.897 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 10941 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5048 _reflns_number_gt 4206 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0381 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4219 _refine_ls_number_parameters 263 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 3.1065 1.9721 1.9304 ; _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.36 _refine_diff_density_min -0.68 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe(1) Fe 0.40125(4) 0.43888(4) 0.84131(2) 0.03815(8) Uani 1.00 1 d . . . Cl(1) Cl 0.48460(12) 0.69291(8) 0.85248(5) 0.0648(2) Uani 1.00 1 d . . . Cl(2) Cl 0.36411(10) 0.32146(8) 0.71601(3) 0.05251(15) Uani 1.00 1 d . . . Cl(3) Cl 0.12806(9) 0.35100(10) 0.88141(4) 0.06067(18) Uani 1.00 1 d . . . Cl(4) Cl 0.62249(10) 0.38219(8) 0.90661(4) 0.05766(18) Uani 1.00 1 d . . . S(1) S 0.45833(7) 0.17096(6) 0.48436(3) 0.03367(11) Uani 1.00 1 d . . . S(2) S 0.56540(7) 0.32397(6) 0.35386(3) 0.03311(11) Uani 1.00 1 d . . . S(3) S 0.73926(7) 0.47658(5) 0.60601(3) 0.03191(11) Uani 1.00 1 d . . . S(4) S 0.84994(7) 0.63273(6) 0.47838(3) 0.03242(11) Uani 1.00 1 d . . . S(5) S 0.89341(8) 0.61288(6) 0.77979(3) 0.03964(12) Uani 1.00 1 d . . . S(6) S 1.14989(7) 0.90551(6) 0.75522(3) 0.03475(11) Uani 1.00 1 d . . . S(7) S 1.12627(8) 0.92145(6) 0.58315(3) 0.03895(12) Uani 1.00 1 d . . . O(1) O 0.2532(2) -0.08952(17) 0.38188(10) 0.0431(3) Uani 1.00 1 d . . . O(2) O 0.3543(2) 0.0613(2) 0.25394(9) 0.0487(4) Uani 1.00 1 d . . . C(1) C 0.5919(2) 0.3340(2) 0.45365(11) 0.0294(4) Uani 1.00 1 d . . . C(2) C 0.7132(2) 0.4671(2) 0.50652(11) 0.0290(4) Uani 1.00 1 d . . . C(3) C 0.3651(2) 0.0602(2) 0.39060(12) 0.0333(4) Uani 1.00 1 d . . . C(4) C 0.4122(3) 0.1320(2) 0.33002(12) 0.0347(4) Uani 1.00 1 d . . . C(5) C 0.9142(2) 0.6637(2) 0.63348(11) 0.0287(4) Uani 1.00 1 d . . . C(6) C 0.9696(2) 0.7425(2) 0.57293(11) 0.0291(4) Uani 1.00 1 d . . . C(7) C 0.9822(2) 0.7244(2) 0.71390(11) 0.0289(4) Uani 1.00 1 d . . . C(8) C 1.0259(3) 0.7486(2) 0.86241(12) 0.0349(4) Uani 1.00 1 d . . . C(9) C 1.1437(2) 0.8824(2) 0.85063(12) 0.0344(4) Uani 1.00 1 d . . . C(10) C 0.1561(3) -0.1567(2) 0.30148(15) 0.0488(6) Uani 1.00 1 d . . . C(11) C 0.2874(4) -0.1086(3) 0.24429(16) 0.0539(6) Uani 1.00 1 d . . . C(12) C 1.0336(4) 0.7398(3) 0.94702(13) 0.0511(6) Uani 1.00 1 d . . . C(13) C 1.1938(4) 0.8934(3) 0.98707(15) 0.0596(7) Uani 1.00 1 d . . . C(14) C 1.2584(3) 0.9908(2) 0.92607(13) 0.0491(6) Uani 1.00 1 d . . . H(1) H 0.2221 -0.1565 0.1923 0.059 Uiso 1.00 1 c R . . H(2) H 0.3933 -0.1419 0.2533 0.059 Uiso 1.00 1 c R . . H(3) H 0.1108 -0.2680 0.2933 0.055 Uiso 1.00 1 c R . . H(4) H 0.0518 -0.1212 0.2932 0.054 Uiso 1.00 1 c R . . H(5) H 1.3908 1.0153 0.9253 0.053 Uiso 1.00 1 c R . . H(6) H 1.2299 1.0852 0.9359 0.053 Uiso 1.00 1 c R . . H(7) H 0.9169 0.7368 0.9645 0.058 Uiso 1.00 1 c R . . H(8) H 1.0634 0.6508 0.9559 0.058 Uiso 1.00 1 c R . . H(9) H 1.2977 0.8701 1.0102 0.065 Uiso 1.00 1 c R . . H(10) H 1.1492 0.9516 1.0266 0.065 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.03784(17) 0.03688(16) 0.03924(17) 0.00896(13) 0.00732(13) 0.01363(13) Cl(1) 0.0760(4) 0.0403(3) 0.0869(5) 0.0234(3) 0.0292(3) 0.0215(3) Cl(2) 0.0589(3) 0.0525(3) 0.0394(2) 0.0079(2) 0.0112(2) 0.0122(2) Cl(3) 0.0442(3) 0.0816(4) 0.0460(3) 0.0040(3) 0.0132(2) 0.0179(3) Cl(4) 0.0567(3) 0.0570(3) 0.0588(3) 0.0221(2) -0.0059(2) 0.0143(2) S(1) 0.0413(2) 0.0289(2) 0.0298(2) 0.00980(19) 0.00300(19) 0.00922(17) S(2) 0.0379(2) 0.0320(2) 0.0271(2) 0.00826(19) 0.00652(18) 0.00664(17) S(3) 0.0372(2) 0.0279(2) 0.0267(2) 0.00494(18) 0.00362(18) 0.00839(17) S(4) 0.0377(2) 0.0328(2) 0.0264(2) 0.00953(19) 0.00794(18) 0.00892(17) S(5) 0.0480(2) 0.0325(2) 0.0268(2) -0.0021(2) 0.0063(2) 0.00671(18) S(6) 0.0353(2) 0.0295(2) 0.0336(2) 0.00298(18) 0.00265(19) 0.00894(18) S(7) 0.0422(2) 0.0313(2) 0.0399(2) 0.0040(2) 0.0101(2) 0.0133(2) O(1) 0.0508(8) 0.0274(6) 0.0434(8) 0.0056(6) -0.0027(6) 0.0080(5) O(2) 0.0606(10) 0.0410(8) 0.0303(7) 0.0029(7) 0.0032(6) 0.0011(6) C(1) 0.0317(8) 0.0289(8) 0.0294(8) 0.0126(7) 0.0050(7) 0.0070(6) C(2) 0.0319(8) 0.0291(8) 0.0279(8) 0.0125(7) 0.0064(7) 0.0068(6) C(3) 0.0356(9) 0.0292(8) 0.0338(9) 0.0109(7) 0.0017(7) 0.0055(7) C(4) 0.0379(10) 0.0310(9) 0.0301(9) 0.0078(7) 0.0024(7) 0.0031(7) C(5) 0.0303(8) 0.0273(8) 0.0281(8) 0.0083(6) 0.0063(6) 0.0070(6) C(6) 0.0295(8) 0.0293(8) 0.0302(8) 0.0104(7) 0.0069(7) 0.0091(6) C(7) 0.0289(8) 0.0281(8) 0.0303(8) 0.0089(6) 0.0067(6) 0.0083(6) C(8) 0.0395(10) 0.0328(9) 0.0275(8) 0.0075(8) 0.0038(7) 0.0045(7) C(9) 0.0345(9) 0.0331(9) 0.0321(9) 0.0085(7) 0.0016(7) 0.0060(7) C(10) 0.0532(13) 0.0340(10) 0.0489(12) 0.0083(9) -0.0082(10) 0.0039(9) C(11) 0.0574(14) 0.0424(12) 0.0482(13) 0.0116(10) -0.0003(11) -0.0100(10) C(12) 0.0694(16) 0.0457(12) 0.0288(10) 0.0074(11) 0.0063(10) 0.0079(8) C(13) 0.0716(17) 0.0558(15) 0.0348(11) 0.0054(13) -0.0089(11) 0.0078(10) C(14) 0.0546(13) 0.0401(11) 0.0362(10) 0.0017(10) -0.0052(9) 0.0007(9) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics Ortep3 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) Cl(1) 2.1856(8) yes . . Fe(1) Cl(2) 2.2176(6) yes . . Fe(1) Cl(3) 2.1866(7) yes . . Fe(1) Cl(4) 2.1851(8) yes . . S(1) C(1) 1.7265(19) yes . . S(1) C(3) 1.7223(18) yes . . S(2) C(1) 1.726(2) yes . . S(2) C(4) 1.7244(18) yes . . S(3) C(2) 1.722(2) yes . . S(3) C(5) 1.7527(16) yes . . S(4) C(2) 1.7291(19) yes . . S(4) C(6) 1.7680(17) yes . . S(5) C(7) 1.723(2) yes . . S(5) C(8) 1.7163(18) yes . . S(6) C(7) 1.7186(16) yes . . S(6) C(9) 1.728(2) yes . . S(7) C(6) 1.6591(17) yes . . O(1) C(3) 1.339(2) yes . . O(1) C(10) 1.454(2) yes . . O(2) C(4) 1.340(2) yes . . O(2) C(11) 1.454(3) yes . . C(1) C(2) 1.385(2) yes . . C(3) C(4) 1.365(3) yes . . C(5) C(6) 1.412(2) yes . . C(5) C(7) 1.402(2) yes . . C(8) C(9) 1.332(2) yes . . C(8) C(12) 1.498(3) yes . . C(9) C(14) 1.503(2) yes . . C(10) C(11) 1.497(4) yes . . C(12) C(13) 1.531(3) yes . . C(13) C(14) 1.532(3) yes . . C(10) H(3) 0.950 no . . C(10) H(4) 0.950 no . . C(11) H(1) 0.950 no . . C(11) H(2) 0.950 no . . C(12) H(7) 0.950 no . . C(12) H(8) 0.950 no . . C(13) H(9) 0.950 no . . C(13) H(10) 0.950 no . . C(14) H(5) 0.950 no . . C(14) H(6) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Fe(1) Cl(2) 109.44(3) yes . . . Cl(1) Fe(1) Cl(3) 109.82(3) yes . . . Cl(1) Fe(1) Cl(4) 110.19(3) yes . . . Cl(2) Fe(1) Cl(3) 107.48(2) yes . . . Cl(2) Fe(1) Cl(4) 108.20(3) yes . . . Cl(3) Fe(1) Cl(4) 111.65(3) yes . . . C(1) S(1) C(3) 94.32(9) yes . . . C(1) S(2) C(4) 94.28(9) yes . . . C(2) S(3) C(5) 96.41(8) yes . . . C(2) S(4) C(6) 97.46(8) yes . . . C(7) S(5) C(8) 96.03(9) yes . . . C(7) S(6) C(9) 94.74(9) yes . . . C(3) O(1) C(10) 111.38(18) yes . . . C(4) O(2) C(11) 110.33(18) yes . . . S(1) C(1) S(2) 116.83(9) yes . . . S(1) C(1) C(2) 121.66(15) yes . . . S(2) C(1) C(2) 121.51(15) yes . . . S(3) C(2) S(4) 115.42(8) yes . . . S(3) C(2) C(1) 121.35(15) yes . . . S(4) C(2) C(1) 123.22(15) yes . . . S(1) C(3) O(1) 118.29(16) yes . . . S(1) C(3) C(4) 117.19(13) yes . . . O(1) C(3) C(4) 124.52(17) yes . . . S(2) C(4) O(2) 118.27(16) yes . . . S(2) C(4) C(3) 117.20(13) yes . . . O(2) C(4) C(3) 124.46(16) yes . . . S(3) C(5) C(6) 117.12(12) yes . . . S(3) C(5) C(7) 117.13(14) yes . . . C(6) C(5) C(7) 125.71(15) yes . . . S(4) C(6) S(7) 119.66(12) yes . . . S(4) C(6) C(5) 113.54(11) yes . . . S(7) C(6) C(5) 126.79(12) yes . . . S(5) C(7) S(6) 114.98(10) yes . . . S(5) C(7) C(5) 119.24(12) yes . . . S(6) C(7) C(5) 125.77(15) yes . . . S(5) C(8) C(9) 116.07(16) yes . . . S(5) C(8) C(12) 130.06(15) yes . . . C(9) C(8) C(12) 113.85(16) yes . . . S(6) C(9) C(8) 118.18(14) yes . . . S(6) C(9) C(14) 129.74(16) yes . . . C(8) C(9) C(14) 112.05(19) yes . . . O(1) C(10) C(11) 110.96(18) yes . . . O(2) C(11) C(10) 110.3(2) yes . . . C(8) C(12) C(13) 101.77(19) yes . . . C(12) C(13) C(14) 109.50(19) yes . . . C(9) C(14) C(13) 102.55(18) yes . . . O(1) C(10) H(3) 109.0 no . . . O(1) C(10) H(4) 109.2 no . . . C(11) C(10) H(3) 109.2 no . . . C(11) C(10) H(4) 109.0 no . . . H(3) C(10) H(4) 109.5 no . . . O(2) C(11) H(1) 109.2 no . . . O(2) C(11) H(2) 109.2 no . . . C(10) C(11) H(1) 109.4 no . . . C(10) C(11) H(2) 109.2 no . . . H(1) C(11) H(2) 109.5 no . . . C(8) C(12) H(7) 111.2 no . . . C(8) C(12) H(8) 111.6 no . . . C(13) C(12) H(7) 111.3 no . . . C(13) C(12) H(8) 111.5 no . . . H(7) C(12) H(8) 109.5 no . . . C(12) C(13) H(9) 109.3 no . . . C(12) C(13) H(10) 109.6 no . . . C(14) C(13) H(9) 109.5 no . . . C(14) C(13) H(10) 109.5 no . . . H(9) C(13) H(10) 109.5 no . . . C(9) C(14) H(5) 111.2 no . . . C(9) C(14) H(6) 111.1 no . . . C(13) C(14) H(5) 111.1 no . . . C(13) C(14) H(6) 111.2 no . . . H(5) C(14) H(6) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) S(1) C(3) O(1) 176.03(19) ? . . . . C(1) S(1) C(3) C(4) -3.6(2) ? . . . . C(3) S(1) C(1) S(2) 4.25(15) ? . . . . C(3) S(1) C(1) C(2) -176.4(2) ? . . . . C(1) S(2) C(4) O(2) -176.1(2) ? . . . . C(1) S(2) C(4) C(3) 1.0(2) ? . . . . C(4) S(2) C(1) S(1) -3.48(15) ? . . . . C(4) S(2) C(1) C(2) 177.2(2) ? . . . . C(2) S(3) C(5) C(6) 1.73(19) ? . . . . C(2) S(3) C(5) C(7) 179.62(18) ? . . . . C(5) S(3) C(2) S(4) -2.22(15) ? . . . . C(5) S(3) C(2) C(1) 176.99(19) ? . . . . C(2) S(4) C(6) S(7) -179.58(14) ? . . . . C(2) S(4) C(6) C(5) -0.75(19) ? . . . . C(6) S(4) C(2) S(3) 1.95(15) ? . . . . C(6) S(4) C(2) C(1) -177.2(2) ? . . . . C(7) S(5) C(8) C(9) -0.4(2) ? . . . . C(7) S(5) C(8) C(12) -179.0(2) ? . . . . C(8) S(5) C(7) S(6) 0.29(15) ? . . . . C(8) S(5) C(7) C(5) -179.25(19) ? . . . . C(7) S(6) C(9) C(8) -0.1(2) ? . . . . C(7) S(6) C(9) C(14) 177.7(2) ? . . . . C(9) S(6) C(7) S(5) -0.14(15) ? . . . . C(9) S(6) C(7) C(5) 179.4(2) ? . . . . C(3) O(1) C(10) C(11) 41.9(3) ? . . . . C(10) O(1) C(3) S(1) 168.41(18) ? . . . . C(10) O(1) C(3) C(4) -12.0(3) ? . . . . C(4) O(2) C(11) C(10) 47.2(2) ? . . . . C(11) O(2) C(4) S(2) 159.12(19) ? . . . . C(11) O(2) C(4) C(3) -17.7(3) ? . . . . S(1) C(1) C(2) S(3) 0.7(2) ? . . . . S(1) C(1) C(2) S(4) 179.85(13) ? . . . . S(2) C(1) C(2) S(3) -179.99(10) ? . . . . S(2) C(1) C(2) S(4) -0.8(2) ? . . . . S(1) C(3) C(4) S(2) 1.8(2) ? . . . . S(1) C(3) C(4) O(2) 178.7(2) ? . . . . O(1) C(3) C(4) S(2) -177.74(19) ? . . . . O(1) C(3) C(4) O(2) -0.8(4) ? . . . . S(3) C(5) C(6) S(4) -0.7(2) ? . . . . S(3) C(5) C(6) S(7) 178.06(13) ? . . . . S(3) C(5) C(7) S(5) 0.6(2) ? . . . . S(3) C(5) C(7) S(6) -178.88(13) ? . . . . C(6) C(5) C(7) S(5) 178.29(18) ? . . . . C(6) C(5) C(7) S(6) -1.2(3) ? . . . . C(7) C(5) C(6) S(4) -178.35(18) ? . . . . C(7) C(5) C(6) S(7) 0.4(3) ? . . . . S(5) C(8) C(9) S(6) 0.4(2) ? . . . . S(5) C(8) C(9) C(14) -177.85(19) ? . . . . S(5) C(8) C(12) C(13) 174.7(2) ? . . . . C(9) C(8) C(12) C(13) -3.9(3) ? . . . . C(12) C(8) C(9) S(6) 179.2(2) ? . . . . C(12) C(8) C(9) C(14) 1.0(3) ? . . . . S(6) C(9) C(14) C(13) -175.5(2) ? . . . . C(8) C(9) C(14) C(13) 2.4(3) ? . . . . O(1) C(10) C(11) O(2) -61.6(3) ? . . . . C(8) C(12) C(13) C(14) 5.3(3) ? . . . . C(12) C(13) C(14) C(9) -4.8(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) S(2) 3.5753(10) ? . 2_666 Cl(1) S(5) 3.6667(11) ? . . Cl(1) O(2) 3.2034(19) ? . 2_666 Cl(1) C(8) 3.661(2) ? . 1_455 Cl(1) C(9) 3.531(2) ? . 1_455 Cl(1) C(14) 3.765(3) ? . 1_455 Cl(2) S(2) 3.5908(9) ? . 2_666 Cl(2) S(3) 3.6256(8) ? . . Cl(2) S(4) 3.7882(8) ? . 2_666 Cl(2) S(7) 3.7599(7) ? . 1_445 Cl(2) C(10) 3.679(2) ? . 2_556 Cl(3) C(10) 3.508(2) ? . 2_556 Cl(3) C(11) 3.483(2) ? . 2_556 Cl(3) C(12) 3.488(2) ? . 2_667 Cl(4) S(5) 3.6586(9) ? . . Cl(4) C(11) 3.581(2) ? . 2_656 Cl(4) C(12) 3.629(2) ? . . S(1) S(1) 3.5237(8) ? . 2_656 S(1) S(4) 3.4044(8) ? . 2_666 S(1) S(7) 3.6175(7) ? . 1_445 S(1) S(7) 3.7275(8) ? . 2_766 S(1) O(1) 3.3939(19) ? . 2_656 S(1) C(3) 3.749(2) ? . 2_656 S(1) C(6) 3.652(2) ? . 2_666 S(2) Cl(1) 3.5753(10) ? . 2_666 S(2) Cl(2) 3.5908(9) ? . 2_666 S(2) S(3) 3.4098(8) ? . 2_666 S(2) C(5) 3.670(2) ? . 2_666 S(3) Cl(2) 3.6256(8) ? . . S(3) S(2) 3.4098(8) ? . 2_666 S(3) O(1) 3.6251(17) ? . 2_656 S(3) C(1) 3.646(2) ? . 2_666 S(4) Cl(2) 3.7882(8) ? . 2_666 S(4) S(1) 3.4044(8) ? . 2_666 S(4) C(1) 3.715(2) ? . 2_666 S(4) C(2) 3.683(2) ? . 2_766 S(5) Cl(1) 3.6667(11) ? . . S(5) Cl(4) 3.6586(9) ? . . S(6) O(2) 3.664(2) ? . 2_766 S(7) Cl(2) 3.7599(7) ? . 1_665 S(7) S(1) 3.6175(7) ? . 1_665 S(7) S(1) 3.7275(8) ? . 2_766 S(7) O(1) 3.7336(18) ? . 1_665 S(7) O(1) 3.702(2) ? . 2_666 S(7) C(1) 3.649(2) ? . 2_766 S(7) C(3) 3.757(2) ? . 2_766 O(1) S(1) 3.3939(19) ? . 2_656 O(1) S(3) 3.6251(17) ? . 2_656 O(1) S(7) 3.7336(18) ? . 1_445 O(1) S(7) 3.702(2) ? . 2_666 O(2) Cl(1) 3.2034(19) ? . 2_666 O(2) S(6) 3.664(2) ? . 2_766 O(2) C(7) 3.696(3) ? . 2_666 C(1) S(3) 3.646(2) ? . 2_666 C(1) S(4) 3.715(2) ? . 2_666 C(1) S(7) 3.649(2) ? . 2_766 C(1) C(2) 3.408(3) ? . 2_666 C(1) C(6) 3.637(3) ? . 2_766 C(2) S(4) 3.683(2) ? . 2_766 C(2) C(1) 3.408(3) ? . 2_666 C(2) C(2) 3.443(3) ? . 2_666 C(2) C(6) 3.732(3) ? . 2_766 C(3) S(1) 3.749(2) ? . 2_656 C(3) S(7) 3.757(2) ? . 2_766 C(3) C(6) 3.583(3) ? . 2_666 C(4) C(5) 3.573(3) ? . 2_666 C(4) C(7) 3.687(3) ? . 2_666 C(5) S(2) 3.670(2) ? . 2_666 C(5) C(4) 3.573(3) ? . 2_666 C(6) S(1) 3.652(2) ? . 2_666 C(6) C(1) 3.637(3) ? . 2_766 C(6) C(2) 3.732(3) ? . 2_766 C(6) C(3) 3.583(3) ? . 2_666 C(7) O(2) 3.696(3) ? . 2_666 C(7) C(4) 3.687(3) ? . 2_666 C(8) Cl(1) 3.661(2) ? . 1_655 C(9) Cl(1) 3.531(2) ? . 1_655 C(10) Cl(2) 3.679(2) ? . 2_556 C(10) Cl(3) 3.508(2) ? . 2_556 C(11) Cl(3) 3.483(2) ? . 2_556 C(11) Cl(4) 3.581(2) ? . 2_656 C(12) Cl(3) 3.488(2) ? . 2_667 C(12) Cl(4) 3.629(2) ? . . C(14) Cl(1) 3.765(3) ? . 1_655 Fe(1) H(2) 3.760 ? . 2_656 Cl(1) H(5) 3.327 ? . 1_455 Cl(1) H(7) 3.508 ? . . Cl(1) H(8) 3.742 ? . 1_455 Cl(1) H(9) 3.584 ? . 1_455 Cl(1) H(10) 3.671 ? . 2_777 Cl(2) H(2) 2.901 ? . 2_656 Cl(2) H(3) 3.431 ? . 2_556 Cl(2) H(4) 3.056 ? . 2_556 Cl(3) H(1) 2.711 ? . 2_556 Cl(3) H(3) 3.237 ? . 2_556 Cl(3) H(4) 3.282 ? . 2_556 Cl(3) H(6) 3.065 ? . 1_445 Cl(3) H(7) 2.976 ? . 2_667 Cl(3) H(8) 3.039 ? . 1_455 Cl(3) H(8) 3.312 ? . 2_667 Cl(3) H(10) 3.640 ? . 2_667 Cl(4) H(1) 3.052 ? . 2_656 Cl(4) H(2) 3.211 ? . 2_656 Cl(4) H(5) 3.362 ? . 1_445 Cl(4) H(6) 3.478 ? . 1_445 Cl(4) H(7) 3.221 ? . . Cl(4) H(8) 3.368 ? . . Cl(4) H(8) 3.342 ? . 2_767 Cl(4) H(9) 3.136 ? . 2_767 S(3) H(3) 3.213 ? . 2_656 S(5) H(3) 3.191 ? . 2_656 S(6) H(2) 3.465 ? . 2_766 S(6) H(4) 3.042 ? . 2_666 S(7) H(4) 3.247 ? . 2_666 C(7) H(4) 3.765 ? . 2_666 C(8) H(10) 3.740 ? . 2_777 C(9) H(10) 3.695 ? . 2_777 C(12) H(6) 3.511 ? . 2_777 C(12) H(10) 3.508 ? . 2_777 C(13) H(1) 3.707 ? . 1_666 C(13) H(5) 3.133 ? . 2_877 C(13) H(6) 3.620 ? . 2_777 C(13) H(7) 3.727 ? . 2_777 C(13) H(9) 3.741 ? . 2_877 C(13) H(10) 3.332 ? . 2_777 C(14) H(5) 3.557 ? . 2_877 C(14) H(7) 3.542 ? . 2_777 C(14) H(9) 3.181 ? . 2_877 C(14) H(10) 3.423 ? . 2_777 H(1) Cl(3) 2.711 ? . 2_556 H(1) Cl(4) 3.052 ? . 2_656 H(1) C(13) 3.707 ? . 1_444 H(1) H(5) 3.753 ? . 2_766 H(1) H(9) 3.334 ? . 1_444 H(1) H(10) 3.293 ? . 1_444 H(2) Fe(1) 3.760 ? . 2_656 H(2) Cl(2) 2.901 ? . 2_656 H(2) Cl(4) 3.211 ? . 2_656 H(2) S(6) 3.465 ? . 2_766 H(3) Cl(2) 3.431 ? . 2_556 H(3) Cl(3) 3.237 ? . 2_556 H(3) S(3) 3.213 ? . 2_656 H(3) S(5) 3.191 ? . 2_656 H(4) Cl(2) 3.056 ? . 2_556 H(4) Cl(3) 3.282 ? . 2_556 H(4) S(6) 3.042 ? . 2_666 H(4) S(7) 3.247 ? . 2_666 H(4) C(7) 3.765 ? . 2_666 H(5) Cl(1) 3.327 ? . 1_655 H(5) Cl(4) 3.362 ? . 1_665 H(5) C(13) 3.133 ? . 2_877 H(5) C(14) 3.557 ? . 2_877 H(5) H(1) 3.753 ? . 2_766 H(5) H(5) 3.070 ? . 2_877 H(5) H(9) 2.322 ? . 2_877 H(5) H(10) 3.388 ? . 2_877 H(6) Cl(3) 3.065 ? . 1_665 H(6) Cl(4) 3.478 ? . 1_665 H(6) C(12) 3.511 ? . 2_777 H(6) C(13) 3.620 ? . 2_777 H(6) H(7) 2.726 ? . 2_777 H(6) H(9) 3.465 ? . 2_877 H(6) H(10) 2.913 ? . 2_777 H(7) Cl(1) 3.508 ? . . H(7) Cl(3) 2.976 ? . 2_667 H(7) Cl(4) 3.221 ? . . H(7) C(13) 3.727 ? . 2_777 H(7) C(14) 3.542 ? . 2_777 H(7) H(6) 2.726 ? . 2_777 H(7) H(10) 3.043 ? . 2_777 H(8) Cl(1) 3.742 ? . 1_655 H(8) Cl(3) 3.039 ? . 1_655 H(8) Cl(3) 3.312 ? . 2_667 H(8) Cl(4) 3.368 ? . . H(8) Cl(4) 3.342 ? . 2_767 H(8) H(8) 3.337 ? . 2_767 H(9) Cl(1) 3.584 ? . 1_655 H(9) Cl(4) 3.136 ? . 2_767 H(9) C(13) 3.741 ? . 2_877 H(9) C(14) 3.181 ? . 2_877 H(9) H(1) 3.334 ? . 1_666 H(9) H(5) 2.322 ? . 2_877 H(9) H(6) 3.465 ? . 2_877 H(9) H(9) 3.314 ? . 2_877 H(10) Cl(1) 3.671 ? . 2_777 H(10) Cl(3) 3.640 ? . 2_667 H(10) C(8) 3.740 ? . 2_777 H(10) C(9) 3.695 ? . 2_777 H(10) C(12) 3.508 ? . 2_777 H(10) C(13) 3.332 ? . 2_777 H(10) C(14) 3.423 ? . 2_777 H(10) H(1) 3.293 ? . 1_666 H(10) H(5) 3.388 ? . 2_877 H(10) H(6) 2.913 ? . 2_777 H(10) H(7) 3.043 ? . 2_777 H(10) H(10) 2.810 ? . 2_777 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC-715841.cif' data__EDO-CP-TTFVS-FeBr4 _database_code_depnum_ccdc_archive 'CCDC 715841' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C14 H10 Br4 Fe O2 S7 ' _chemical_formula_moiety 'C14 H10 Br4 Fe O2 S7 ' _chemical_formula_weight 810.11 _chemical_melting_point '435 K' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.6140(15) _cell_length_b 9.4388(18) _cell_length_c 17.891(4) _cell_angle_alpha 101.101(4) _cell_angle_beta 95.706(4) _cell_angle_gamma 107.744(4) _cell_volume 1184.4(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4062 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.271 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776.00 _exptl_absorpt_coefficient_mu 8.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.123 _exptl_absorpt_correction_T_max 0.852 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11465 _diffrn_reflns_av_R_equivalents 0.120 _diffrn_reflns_theta_max 27.42 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.972 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5246 _reflns_number_gt 3484 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.0676 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3484 _refine_ls_number_parameters 263 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 8.9584 -3.2107 6.3827 ; _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.27 _refine_diff_density_min -1.29 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Br 0.1425(2) 0.68758(15) 0.29215(7) 0.0660(4) Uani 1.00 1 d . . . Br(2) Br 0.38070(19) 0.64790(17) 0.11735(8) 0.0695(4) Uani 1.00 1 d . . . Br(3) Br -0.1329(2) 0.62400(16) 0.09208(8) 0.0687(4) Uani 1.00 1 d . . . Br(4) Br 0.0064(2) 0.29929(15) 0.14756(9) 0.0756(5) Uani 1.00 1 d . . . Fe(1) Fe 0.0974(2) 0.56281(19) 0.16063(9) 0.0508(5) Uani 1.00 1 d . . . S(1) S -0.0337(4) 0.1789(3) 0.48661(17) 0.0524(9) Uani 1.00 1 d . . . S(2) S 0.0642(4) 0.3256(3) 0.35870(16) 0.0513(9) Uani 1.00 1 d . . . S(3) S 0.2450(4) 0.4799(3) 0.60671(16) 0.0491(9) Uani 1.00 1 d . . . S(4) S 0.3462(4) 0.6274(3) 0.48081(16) 0.0496(9) Uani 1.00 1 d . . . S(5) S 0.4023(4) 0.6167(3) 0.77775(17) 0.0542(9) Uani 1.00 1 d . . . S(6) S 0.6459(4) 0.9019(3) 0.75293(17) 0.0507(9) Uani 1.00 1 d . . . S(7) S 0.6185(4) 0.9100(3) 0.58296(18) 0.0582(10) Uani 1.00 1 d . . . O(1) O -0.2347(12) -0.0775(9) 0.3856(4) 0.065(2) Uani 1.00 1 d . . . O(2) O -0.1438(12) 0.0711(9) 0.2612(4) 0.066(2) Uani 1.00 1 d . . . C(1) C 0.0974(16) 0.3384(12) 0.4569(6) 0.046(3) Uani 1.00 1 d . . . C(2) C 0.2136(14) 0.4659(11) 0.5090(5) 0.038(3) Uani 1.00 1 d . . . C(3) C -0.1297(17) 0.0704(13) 0.3935(6) 0.050(3) Uani 1.00 1 d . . . C(4) C -0.0852(16) 0.1379(13) 0.3346(7) 0.054(4) Uani 1.00 1 d . . . C(5) C 0.4144(14) 0.6607(12) 0.6310(6) 0.041(3) Uani 1.00 1 d . . . C(6) C 0.4674(14) 0.7366(12) 0.5743(5) 0.042(3) Uani 1.00 1 d . . . C(7) C 0.4855(15) 0.7223(11) 0.7116(6) 0.046(3) Uani 1.00 1 d . . . C(8) C 0.5343(16) 0.7539(12) 0.8579(6) 0.050(3) Uani 1.00 1 d . . . C(9) C 0.6434(17) 0.8853(13) 0.8481(6) 0.049(3) Uani 1.00 1 d . . . C(10) C -0.3305(19) -0.1436(14) 0.3055(7) 0.070(4) Uani 1.00 1 d . . . C(11) C -0.210(2) -0.0940(15) 0.2500(7) 0.081(5) Uani 1.00 1 d . . . C(12) C 0.5403(19) 0.7509(13) 0.9425(6) 0.064(4) Uani 1.00 1 d . . . C(13) C 0.696(2) 0.8989(13) 0.9813(7) 0.073(4) Uani 1.00 1 d . . . C(14) C 0.7540(18) 0.9937(12) 0.9223(7) 0.061(4) Uani 1.00 1 d . . . H(1) H -0.3729 -0.2519 0.2973 0.078 Uiso 1.00 1 c R . . H(2) H -0.4350 -0.1095 0.2985 0.078 Uiso 1.00 1 c R . . H(3) H -0.2773 -0.1381 0.1989 0.096 Uiso 1.00 1 c R . . H(4) H -0.1055 -0.1285 0.2566 0.096 Uiso 1.00 1 c R . . H(5) H 0.4250 0.7500 0.9588 0.076 Uiso 1.00 1 c R . . H(6) H 0.5690 0.6640 0.9519 0.076 Uiso 1.00 1 c R . . H(7) H 0.6544 0.9553 1.0214 0.080 Uiso 1.00 1 c R . . H(8) H 0.8009 0.8759 1.0025 0.080 Uiso 1.00 1 c R . . H(9) H 0.8844 1.0211 0.9213 0.069 Uiso 1.00 1 c R . . H(10) H 0.7200 1.0836 0.9320 0.069 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0731(9) 0.0668(8) 0.0524(8) 0.0150(7) 0.0140(6) 0.0122(6) Br(2) 0.0569(8) 0.0877(10) 0.0638(9) 0.0199(8) 0.0187(7) 0.0199(7) Br(3) 0.0654(9) 0.0713(9) 0.0711(9) 0.0307(7) -0.0002(7) 0.0137(7) Br(4) 0.0820(10) 0.0514(8) 0.0995(11) 0.0265(8) 0.0278(8) 0.0188(7) Fe(1) 0.0508(10) 0.0517(10) 0.0512(11) 0.0180(9) 0.0105(8) 0.0124(8) S(1) 0.058(2) 0.0533(17) 0.0449(18) 0.0181(16) 0.0050(15) 0.0130(15) S(2) 0.057(2) 0.0520(17) 0.0409(18) 0.0161(16) 0.0075(15) 0.0055(15) S(3) 0.0552(19) 0.0492(17) 0.0395(17) 0.0141(16) 0.0065(14) 0.0083(14) S(4) 0.0558(19) 0.0529(18) 0.0411(17) 0.0196(16) 0.0099(14) 0.0096(14) S(5) 0.063(2) 0.0487(17) 0.0420(18) 0.0053(16) 0.0097(15) 0.0109(14) S(6) 0.055(2) 0.0432(16) 0.0491(19) 0.0120(15) 0.0065(15) 0.0089(14) S(7) 0.066(2) 0.0506(18) 0.055(2) 0.0137(17) 0.0134(17) 0.0139(16) O(1) 0.078(6) 0.051(5) 0.061(5) 0.016(4) 0.004(4) 0.016(4) O(2) 0.085(6) 0.054(5) 0.038(5) 0.003(4) 0.004(4) -0.005(4) C(1) 0.050(7) 0.054(7) 0.044(6) 0.036(6) 0.008(5) 0.007(6) C(2) 0.045(6) 0.041(6) 0.026(6) 0.022(5) -0.004(5) -0.003(5) C(3) 0.058(8) 0.058(7) 0.038(7) 0.038(7) -0.013(5) 0.002(6) C(4) 0.061(8) 0.056(7) 0.055(8) 0.037(7) 0.009(6) 0.009(7) C(5) 0.045(7) 0.054(6) 0.038(7) 0.033(6) 0.013(5) 0.011(5) C(6) 0.042(6) 0.056(7) 0.034(6) 0.020(6) 0.017(5) 0.009(5) C(7) 0.045(7) 0.041(6) 0.055(8) 0.017(5) 0.018(6) 0.006(5) C(8) 0.053(7) 0.044(6) 0.055(8) 0.017(6) 0.015(6) 0.008(5) C(9) 0.058(7) 0.052(7) 0.041(7) 0.025(6) 0.005(6) 0.011(6) C(10) 0.073(9) 0.057(8) 0.065(9) 0.008(7) 0.003(7) 0.008(7) C(11) 0.103(12) 0.069(9) 0.068(10) 0.041(9) 0.008(9) -0.006(8) C(12) 0.086(10) 0.063(8) 0.040(7) 0.026(7) -0.000(6) 0.010(6) C(13) 0.090(10) 0.052(7) 0.057(8) 0.006(7) -0.007(7) 0.003(7) C(14) 0.061(8) 0.044(7) 0.068(8) 0.011(6) 0.002(6) 0.004(6) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics Ortep3 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Fe(1) 2.3595(19) yes . . Br(2) Fe(1) 2.326(2) yes . . Br(3) Fe(1) 2.319(2) yes . . Br(4) Fe(1) 2.327(2) yes . . S(1) C(1) 1.745(12) yes . . S(1) C(3) 1.732(10) yes . . S(2) C(1) 1.726(11) yes . . S(2) C(4) 1.732(11) yes . . S(3) C(2) 1.715(10) yes . . S(3) C(5) 1.740(9) yes . . S(4) C(2) 1.748(10) yes . . S(4) C(6) 1.777(9) yes . . S(5) C(7) 1.736(12) yes . . S(5) C(8) 1.717(9) yes . . S(6) C(7) 1.729(9) yes . . S(6) C(9) 1.741(12) yes . . S(7) C(6) 1.657(10) yes . . O(1) C(3) 1.352(13) yes . . O(1) C(10) 1.464(14) yes . . O(2) C(4) 1.309(13) yes . . O(2) C(11) 1.450(15) yes . . C(1) C(2) 1.362(12) yes . . C(3) C(4) 1.353(18) yes . . C(5) C(6) 1.375(16) yes . . C(5) C(7) 1.429(14) yes . . C(8) C(9) 1.320(16) yes . . C(8) C(12) 1.517(16) yes . . C(9) C(14) 1.500(14) yes . . C(10) C(11) 1.47(2) yes . . C(12) C(13) 1.515(15) yes . . C(13) C(14) 1.524(19) yes . . C(10) H(1) 0.950 no . . C(10) H(2) 0.950 no . . C(11) H(3) 0.950 no . . C(11) H(4) 0.950 no . . C(12) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(13) H(8) 0.950 no . . C(14) H(9) 0.950 no . . C(14) H(10) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Fe(1) Br(2) 107.61(7) yes . . . Br(1) Fe(1) Br(3) 108.87(9) yes . . . Br(1) Fe(1) Br(4) 109.78(8) yes . . . Br(2) Fe(1) Br(3) 110.80(9) yes . . . Br(2) Fe(1) Br(4) 109.93(9) yes . . . Br(3) Fe(1) Br(4) 109.80(7) yes . . . C(1) S(1) C(3) 94.5(5) yes . . . C(1) S(2) C(4) 95.0(5) yes . . . C(2) S(3) C(5) 95.7(5) yes . . . C(2) S(4) C(6) 97.4(4) yes . . . C(7) S(5) C(8) 95.3(5) yes . . . C(7) S(6) C(9) 95.7(5) yes . . . C(3) O(1) C(10) 109.8(9) yes . . . C(4) O(2) C(11) 110.6(10) yes . . . S(1) C(1) S(2) 115.8(5) yes . . . S(1) C(1) C(2) 121.3(8) yes . . . S(2) C(1) C(2) 122.8(9) yes . . . S(3) C(2) S(4) 114.7(4) yes . . . S(3) C(2) C(1) 123.0(8) yes . . . S(4) C(2) C(1) 122.3(8) yes . . . S(1) C(3) O(1) 117.3(8) yes . . . S(1) C(3) C(4) 117.4(8) yes . . . O(1) C(3) C(4) 125.2(9) yes . . . S(2) C(4) O(2) 118.0(9) yes . . . S(2) C(4) C(3) 117.1(8) yes . . . O(2) C(4) C(3) 124.9(9) yes . . . S(3) C(5) C(6) 120.0(7) yes . . . S(3) C(5) C(7) 115.6(8) yes . . . C(6) C(5) C(7) 124.3(8) yes . . . S(4) C(6) S(7) 118.9(6) yes . . . S(4) C(6) C(5) 112.1(6) yes . . . S(7) C(6) C(5) 129.0(7) yes . . . S(5) C(7) S(6) 114.2(6) yes . . . S(5) C(7) C(5) 119.8(7) yes . . . S(6) C(7) C(5) 125.9(8) yes . . . S(5) C(8) C(9) 118.6(9) yes . . . S(5) C(8) C(12) 129.1(8) yes . . . C(9) C(8) C(12) 112.3(8) yes . . . S(6) C(9) C(8) 116.2(7) yes . . . S(6) C(9) C(14) 130.5(8) yes . . . C(8) C(9) C(14) 113.3(10) yes . . . O(1) C(10) C(11) 112.1(10) yes . . . O(2) C(11) C(10) 111.9(11) yes . . . C(8) C(12) C(13) 101.8(9) yes . . . C(12) C(13) C(14) 110.0(9) yes . . . C(9) C(14) C(13) 101.9(8) yes . . . O(1) C(10) H(1) 108.4 no . . . O(1) C(10) H(2) 108.1 no . . . C(11) C(10) H(1) 110.9 no . . . C(11) C(10) H(2) 107.9 no . . . H(1) C(10) H(2) 109.5 no . . . O(2) C(11) H(3) 108.4 no . . . O(2) C(11) H(4) 109.5 no . . . C(10) C(11) H(3) 109.4 no . . . C(10) C(11) H(4) 108.2 no . . . H(3) C(11) H(4) 109.5 no . . . C(8) C(12) H(5) 111.5 no . . . C(8) C(12) H(6) 110.6 no . . . C(13) C(12) H(5) 111.5 no . . . C(13) C(12) H(6) 111.9 no . . . H(5) C(12) H(6) 109.5 no . . . C(12) C(13) H(7) 109.4 no . . . C(12) C(13) H(8) 109.2 no . . . C(14) C(13) H(7) 109.7 no . . . C(14) C(13) H(8) 109.1 no . . . H(7) C(13) H(8) 109.5 no . . . C(9) C(14) H(9) 110.9 no . . . C(9) C(14) H(10) 111.1 no . . . C(13) C(14) H(9) 112.0 no . . . C(13) C(14) H(10) 111.4 no . . . H(9) C(14) H(10) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) S(1) C(3) O(1) 173.7(11) ? . . . . C(1) S(1) C(3) C(4) -2.8(12) ? . . . . C(3) S(1) C(1) S(2) 4.4(9) ? . . . . C(3) S(1) C(1) C(2) -177.6(12) ? . . . . C(1) S(2) C(4) O(2) -176.5(11) ? . . . . C(1) S(2) C(4) C(3) 2.4(12) ? . . . . C(4) S(2) C(1) S(1) -4.3(9) ? . . . . C(4) S(2) C(1) C(2) 177.7(12) ? . . . . C(2) S(3) C(5) C(6) 1.8(11) ? . . . . C(2) S(3) C(5) C(7) 179.9(7) ? . . . . C(5) S(3) C(2) S(4) -2.3(8) ? . . . . C(5) S(3) C(2) C(1) 176.6(11) ? . . . . C(2) S(4) C(6) S(7) -179.4(8) ? . . . . C(2) S(4) C(6) C(5) -0.9(10) ? . . . . C(6) S(4) C(2) S(3) 2.1(8) ? . . . . C(6) S(4) C(2) C(1) -176.8(11) ? . . . . C(7) S(5) C(8) C(9) 1.7(13) ? . . . . C(7) S(5) C(8) C(12) 178.8(13) ? . . . . C(8) S(5) C(7) S(6) -0.9(8) ? . . . . C(8) S(5) C(7) C(5) -178.3(10) ? . . . . C(7) S(6) C(9) C(8) 1.1(12) ? . . . . C(7) S(6) C(9) C(14) 177.3(13) ? . . . . C(9) S(6) C(7) S(5) 0.1(7) ? . . . . C(9) S(6) C(7) C(5) 177.3(12) ? . . . . C(3) O(1) C(10) C(11) 40.6(16) ? . . . . C(10) O(1) C(3) S(1) 170.1(10) ? . . . . C(10) O(1) C(3) C(4) -13.7(19) ? . . . . C(4) O(2) C(11) C(10) 45.7(16) ? . . . . C(11) O(2) C(4) S(2) 159.9(10) ? . . . . C(11) O(2) C(4) C(3) -18.8(19) ? . . . . S(1) C(1) C(2) S(3) 1.3(17) ? . . . . S(1) C(1) C(2) S(4) -179.9(6) ? . . . . S(2) C(1) C(2) S(3) 179.2(7) ? . . . . S(2) C(1) C(2) S(4) -2.0(17) ? . . . . S(1) C(3) C(4) S(2) 0.3(12) ? . . . . S(1) C(3) C(4) O(2) 179.0(11) ? . . . . O(1) C(3) C(4) S(2) -175.9(11) ? . . . . O(1) C(3) C(4) O(2) 3(2) ? . . . . S(3) C(5) C(6) S(4) -0.6(12) ? . . . . S(3) C(5) C(6) S(7) 177.7(8) ? . . . . S(3) C(5) C(7) S(5) 0.2(11) ? . . . . S(3) C(5) C(7) S(6) -176.9(7) ? . . . . C(6) C(5) C(7) S(5) 178.2(10) ? . . . . C(6) C(5) C(7) S(6) 1.1(19) ? . . . . C(7) C(5) C(6) S(4) -178.5(10) ? . . . . C(7) C(5) C(6) S(7) -0.2(17) ? . . . . S(5) C(8) C(9) S(6) -2.0(16) ? . . . . S(5) C(8) C(9) C(14) -178.8(10) ? . . . . S(5) C(8) C(12) C(13) 175.1(11) ? . . . . C(9) C(8) C(12) C(13) -7.7(16) ? . . . . C(12) C(8) C(9) S(6) -179.5(9) ? . . . . C(12) C(8) C(9) C(14) 3.6(17) ? . . . . S(6) C(9) C(14) C(13) -174.1(12) ? . . . . C(8) C(9) C(14) C(13) 2.2(16) ? . . . . O(1) C(10) C(11) O(2) -59.0(16) ? . . . . C(8) C(12) C(13) C(14) 8.9(15) ? . . . . C(12) C(13) C(14) C(9) -7.1(15) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(4) O(2) 3.275(8) ? . . S(1) S(4) 3.444(5) ? . 2_566 S(1) O(1) 3.381(10) ? . 2_556 S(2) S(3) 3.433(5) ? . 2_566 S(3) S(2) 3.433(5) ? . 2_566 S(4) S(1) 3.444(5) ? . 2_566 O(1) S(1) 3.381(10) ? . 2_556 O(2) Br(4) 3.275(8) ? . . C(1) C(2) 3.451(18) ? . 2_566 C(2) C(1) 3.451(18) ? . 2_566 C(2) C(2) 3.500(17) ? . 2_566 Br(1) H(1) 3.546 ? . 1_665 Br(1) H(2) 3.181 ? . 1_665 Br(1) H(4) 3.028 ? . 1_565 Br(2) H(1) 3.365 ? . 1_665 Br(2) H(2) 3.463 ? . 1_665 Br(2) H(3) 2.810 ? . 1_665 Br(2) H(5) 3.184 ? . 1_554 Br(2) H(6) 3.424 ? . 1_554 Br(2) H(6) 3.119 ? . 2_666 Br(2) H(10) 3.115 ? . 2_676 Br(3) H(3) 3.190 ? . 1_565 Br(3) H(4) 3.331 ? . 1_565 Br(3) H(5) 3.437 ? . 2_566 Br(3) H(6) 3.367 ? . 1_454 Br(3) H(6) 3.491 ? . 2_566 Br(3) H(8) 3.243 ? . 1_454 Br(3) H(9) 3.376 ? . 2_676 Br(4) H(5) 3.480 ? . 2_566 Br(4) H(8) 3.556 ? . 2_666 Br(4) H(9) 3.414 ? . 2_666 S(3) H(1) 3.301 ? . 2_556 S(5) H(1) 3.377 ? . 2_556 S(6) H(2) 3.096 ? . 2_566 S(6) H(4) 3.541 ? . 2_666 S(7) H(2) 3.264 ? . 2_566 C(12) H(7) 3.509 ? . 2_677 C(12) H(10) 3.582 ? . 2_677 C(13) H(7) 3.356 ? . 2_677 C(13) H(9) 3.274 ? . 2_777 C(14) H(5) 3.583 ? . 2_677 C(14) H(7) 3.502 ? . 2_677 C(14) H(8) 3.275 ? . 2_777 H(1) Br(1) 3.546 ? . 1_445 H(1) Br(2) 3.365 ? . 1_445 H(1) S(3) 3.301 ? . 2_556 H(1) S(5) 3.377 ? . 2_556 H(2) Br(1) 3.181 ? . 1_445 H(2) Br(2) 3.463 ? . 1_445 H(2) S(6) 3.096 ? . 2_566 H(2) S(7) 3.264 ? . 2_566 H(3) Br(2) 2.810 ? . 1_445 H(3) Br(3) 3.190 ? . 1_545 H(3) H(7) 3.487 ? . 1_444 H(4) Br(1) 3.028 ? . 1_545 H(4) Br(3) 3.331 ? . 1_545 H(4) S(6) 3.541 ? . 2_666 H(5) Br(2) 3.184 ? . 1_556 H(5) Br(3) 3.437 ? . 2_566 H(5) Br(4) 3.480 ? . 2_566 H(5) C(14) 3.583 ? . 2_677 H(5) H(7) 2.986 ? . 2_677 H(5) H(10) 2.794 ? . 2_677 H(6) Br(2) 3.424 ? . 1_556 H(6) Br(2) 3.119 ? . 2_666 H(6) Br(3) 3.367 ? . 1_656 H(6) Br(3) 3.491 ? . 2_566 H(7) C(12) 3.509 ? . 2_677 H(7) C(13) 3.356 ? . 2_677 H(7) C(14) 3.502 ? . 2_677 H(7) H(3) 3.487 ? . 1_666 H(7) H(5) 2.986 ? . 2_677 H(7) H(7) 2.816 ? . 2_677 H(7) H(9) 3.485 ? . 2_777 H(7) H(10) 2.985 ? . 2_677 H(8) Br(3) 3.243 ? . 1_656 H(8) Br(4) 3.556 ? . 2_666 H(8) C(14) 3.275 ? . 2_777 H(8) H(8) 3.239 ? . 2_777 H(8) H(9) 2.442 ? . 2_777 H(8) H(10) 3.599 ? . 2_777 H(9) Br(3) 3.376 ? . 2_676 H(9) Br(4) 3.414 ? . 2_666 H(9) C(13) 3.274 ? . 2_777 H(9) H(7) 3.485 ? . 2_777 H(9) H(8) 2.442 ? . 2_777 H(9) H(9) 3.325 ? . 2_777 H(10) Br(2) 3.115 ? . 2_676 H(10) C(12) 3.582 ? . 2_677 H(10) H(5) 2.794 ? . 2_677 H(10) H(7) 2.985 ? . 2_677 H(10) H(8) 3.599 ? . 2_777 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC-715842.cif' data__EDT-CP-TTFVS-FeCl4 _database_code_depnum_ccdc_archive 'CCDC 715842' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C14 H10 Cl4 Fe S9 ' _chemical_formula_moiety 'C14 H10 Cl4 Fe S9 ' _chemical_formula_weight 664.43 _chemical_melting_point 422 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.8147(9) _cell_length_b 8.7364(8) _cell_length_c 19.3695(15) _cell_angle_alpha 97.651(2) _cell_angle_beta 99.320(3) _cell_angle_gamma 111.723(3) _cell_volume 1185.08(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5331 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664.00 _exptl_absorpt_coefficient_mu 1.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_T_max 0.928 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11193 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_max 27.41 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5275 _reflns_number_gt 3066 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0524 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3091 _refine_ls_number_parameters 263 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 10.9347 -3.1195 9.4451 ; _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.53 _refine_diff_density_min -0.55 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe(1) Fe 0.05375(11) 0.09198(9) 0.15114(4) 0.04114(19) Uani 1.00 1 d . . . Cl(1) Cl 0.1344(2) 0.1691(2) 0.26849(7) 0.0774(4) Uani 1.00 1 d . . . Cl(2) Cl -0.2519(2) -0.0601(2) 0.12085(8) 0.0633(4) Uani 1.00 1 d . . . Cl(3) Cl 0.2099(2) -0.0588(2) 0.12034(10) 0.0647(4) Uani 1.00 1 d . . . Cl(4) Cl 0.1334(2) 0.3154(2) 0.10420(9) 0.0683(5) Uani 1.00 1 d . . . S(1) S 0.46936(17) 0.20079(14) 0.49654(6) 0.0358(2) Uani 1.00 1 d . . . S(2) S 0.73477(17) 0.50630(15) 0.59951(6) 0.0358(2) Uani 1.00 1 d . . . S(3) S 0.64203(17) 0.36620(14) 0.36927(6) 0.0360(2) Uani 1.00 1 d . . . S(4) S 0.90548(16) 0.66564(14) 0.47440(6) 0.0345(2) Uani 1.00 1 d . . . S(5) S 0.3020(2) 0.02202(17) 0.60233(8) 0.0512(3) Uani 1.00 1 d . . . S(6) S 0.6239(2) 0.38988(19) 0.72758(6) 0.0480(3) Uani 1.00 1 d . . . S(7) S 0.6141(2) 0.30712(16) 0.20778(6) 0.0446(3) Uani 1.00 1 d . . . S(8) S 0.90854(18) 0.63360(15) 0.21514(6) 0.0378(2) Uani 1.00 1 d . . . S(9) S 1.09125(17) 0.83960(15) 0.36980(7) 0.0412(3) Uani 1.00 1 d . . . C(1) C 0.6499(6) 0.3981(5) 0.5110(2) 0.0328(11) Uani 1.00 1 d . . . C(2) C 0.7242(6) 0.4679(5) 0.4579(2) 0.0305(10) Uani 1.00 1 d . . . C(3) C 0.4654(6) 0.2042(5) 0.5867(2) 0.0325(11) Uani 1.00 1 d . . . C(4) C 0.5896(6) 0.3482(5) 0.6345(2) 0.0332(11) Uani 1.00 1 d . . . C(5) C 0.7978(5) 0.5238(5) 0.3354(2) 0.0300(10) Uani 1.00 1 d . . . C(6) C 0.9286(6) 0.6714(5) 0.3859(2) 0.0310(10) Uani 1.00 1 d . . . C(7) C 0.7811(6) 0.4929(5) 0.2603(2) 0.0313(11) Uani 1.00 1 d . . . C(8) C 0.6579(6) 0.3547(6) 0.1273(2) 0.0371(12) Uani 1.00 1 d . . . C(9) C 0.7935(6) 0.5053(5) 0.1318(2) 0.0353(11) Uani 1.00 1 d . . . C(10) C 0.3290(10) 0.0700(9) 0.6983(3) 0.065(2) Uani 1.00 1 d . . . C(11) C 0.5267(9) 0.1742(8) 0.7397(3) 0.0630(19) Uani 1.00 1 d . . . C(12) C 0.5710(8) 0.2545(6) 0.0531(2) 0.0512(15) Uani 1.00 1 d . . . C(13) C 0.6789(9) 0.3736(8) 0.0093(3) 0.0647(18) Uani 1.00 1 d . . . C(14) C 0.8253(7) 0.5355(6) 0.0589(2) 0.0466(14) Uani 1.00 1 d . . . H(1) H 0.2566 0.1335 0.7080 0.082 Uiso 1.00 1 c R . . H(2) H 0.2812 -0.0328 0.7141 0.082 Uiso 1.00 1 c R . . H(3) H 0.6030 0.1200 0.7239 0.080 Uiso 1.00 1 c R . . H(4) H 0.5318 0.1757 0.7891 0.080 Uiso 1.00 1 c R . . H(5) H 0.5898 0.1525 0.0471 0.056 Uiso 1.00 1 c R . . H(6) H 0.4394 0.2294 0.0408 0.056 Uiso 1.00 1 c R . . H(7) H 0.7411 0.3204 -0.0173 0.070 Uiso 1.00 1 c R . . H(8) H 0.5925 0.3992 -0.0227 0.070 Uiso 1.00 1 c R . . H(9) H 0.8025 0.6309 0.0491 0.055 Uiso 1.00 1 c R . . H(10) H 0.9503 0.5511 0.0554 0.055 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0460(4) 0.0392(4) 0.0312(3) 0.0112(3) 0.0060(2) 0.0052(2) Cl(1) 0.0948(12) 0.0617(9) 0.0336(7) -0.0095(8) 0.0073(7) 0.0022(6) Cl(2) 0.0449(8) 0.0720(10) 0.0586(8) 0.0138(7) 0.0059(6) 0.0025(7) Cl(3) 0.0540(8) 0.0517(8) 0.0827(10) 0.0202(7) 0.0107(7) 0.0040(7) Cl(4) 0.0902(12) 0.0618(9) 0.0612(9) 0.0313(8) 0.0225(8) 0.0316(7) S(1) 0.0384(6) 0.0301(5) 0.0316(5) 0.0071(4) 0.0096(4) -0.0001(4) S(2) 0.0351(6) 0.0373(6) 0.0268(5) 0.0094(4) 0.0021(4) 0.0009(4) S(3) 0.0409(6) 0.0285(5) 0.0277(5) 0.0041(4) 0.0042(4) 0.0031(4) S(4) 0.0326(5) 0.0323(5) 0.0291(5) 0.0063(4) 0.0016(4) 0.0019(4) S(5) 0.0572(8) 0.0414(7) 0.0542(7) 0.0120(6) 0.0286(6) 0.0113(5) S(6) 0.0535(8) 0.0663(8) 0.0268(5) 0.0273(7) 0.0094(5) 0.0086(5) S(7) 0.0521(7) 0.0358(6) 0.0293(5) 0.0008(5) 0.0080(5) 0.0037(4) S(8) 0.0398(6) 0.0345(6) 0.0311(5) 0.0060(4) 0.0090(4) 0.0057(4) S(9) 0.0354(6) 0.0340(6) 0.0460(6) 0.0047(5) 0.0097(5) 0.0077(5) C(1) 0.030(2) 0.032(2) 0.028(2) 0.0071(18) 0.0007(17) 0.0005(17) C(2) 0.029(2) 0.032(2) 0.027(2) 0.0108(18) 0.0033(16) 0.0017(16) C(3) 0.036(2) 0.034(2) 0.031(2) 0.0165(19) 0.0127(18) 0.0038(17) C(4) 0.033(2) 0.041(2) 0.031(2) 0.020(2) 0.0103(18) 0.0076(18) C(5) 0.025(2) 0.027(2) 0.035(2) 0.0081(17) 0.0057(17) 0.0054(17) C(6) 0.025(2) 0.028(2) 0.036(2) 0.0097(17) 0.0043(17) 0.0034(17) C(7) 0.031(2) 0.035(2) 0.029(2) 0.0134(19) 0.0084(17) 0.0098(17) C(8) 0.037(2) 0.037(2) 0.032(2) 0.010(2) 0.0089(19) 0.0037(18) C(9) 0.034(2) 0.038(2) 0.030(2) 0.011(2) 0.0057(18) 0.0054(18) C(10) 0.078(4) 0.073(4) 0.052(3) 0.030(3) 0.030(3) 0.028(3) C(11) 0.069(4) 0.086(4) 0.045(3) 0.035(3) 0.022(2) 0.031(3) C(12) 0.062(3) 0.043(2) 0.034(2) 0.009(2) 0.008(2) 0.003(2) C(13) 0.069(4) 0.068(3) 0.038(2) 0.006(3) 0.022(2) -0.000(2) C(14) 0.052(3) 0.051(3) 0.036(2) 0.013(2) 0.020(2) 0.016(2) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics Ortep3 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) Cl(1) 2.1981(14) yes . . Fe(1) Cl(2) 2.1919(15) yes . . Fe(1) Cl(3) 2.190(2) yes . . Fe(1) Cl(4) 2.187(2) yes . . S(1) C(1) 1.727(4) yes . . S(1) C(3) 1.749(4) yes . . S(2) C(1) 1.734(4) yes . . S(2) C(4) 1.730(4) yes . . S(3) C(2) 1.721(4) yes . . S(3) C(5) 1.751(4) yes . . S(4) C(2) 1.729(3) yes . . S(4) C(6) 1.757(4) yes . . S(5) C(3) 1.733(4) yes . . S(5) C(10) 1.809(6) yes . . S(6) C(4) 1.747(4) yes . . S(6) C(11) 1.816(7) yes . . S(7) C(7) 1.713(3) yes . . S(7) C(8) 1.721(5) yes . . S(8) C(7) 1.712(4) yes . . S(8) C(9) 1.724(3) yes . . S(9) C(6) 1.656(4) yes . . C(1) C(2) 1.367(6) yes . . C(3) C(4) 1.370(5) yes . . C(5) C(6) 1.424(4) yes . . C(5) C(7) 1.418(6) yes . . C(8) C(9) 1.330(6) yes . . C(8) C(12) 1.484(6) yes . . C(9) C(14) 1.513(7) yes . . C(10) C(11) 1.491(8) yes . . C(12) C(13) 1.527(8) yes . . C(13) C(14) 1.522(6) yes . . C(10) H(1) 0.950 no . . C(10) H(2) 0.950 no . . C(11) H(3) 0.950 no . . C(11) H(4) 0.950 no . . C(12) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(13) H(8) 0.950 no . . C(14) H(9) 0.950 no . . C(14) H(10) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Fe(1) Cl(2) 107.33(7) yes . . . Cl(1) Fe(1) Cl(3) 106.99(8) yes . . . Cl(1) Fe(1) Cl(4) 109.64(6) yes . . . Cl(2) Fe(1) Cl(3) 110.76(6) yes . . . Cl(2) Fe(1) Cl(4) 112.27(8) yes . . . Cl(3) Fe(1) Cl(4) 109.68(8) yes . . . C(1) S(1) C(3) 95.7(2) yes . . . C(1) S(2) C(4) 96.0(2) yes . . . C(2) S(3) C(5) 96.78(19) yes . . . C(2) S(4) C(6) 98.09(19) yes . . . C(3) S(5) C(10) 102.9(2) yes . . . C(4) S(6) C(11) 98.6(2) yes . . . C(7) S(7) C(8) 96.2(2) yes . . . C(7) S(8) C(9) 94.5(2) yes . . . S(1) C(1) S(2) 115.3(2) yes . . . S(1) C(1) C(2) 123.8(3) yes . . . S(2) C(1) C(2) 120.9(2) yes . . . S(3) C(2) S(4) 115.0(2) yes . . . S(3) C(2) C(1) 122.4(2) yes . . . S(4) C(2) C(1) 122.6(2) yes . . . S(1) C(3) S(5) 114.3(2) yes . . . S(1) C(3) C(4) 116.3(3) yes . . . S(5) C(3) C(4) 129.4(3) yes . . . S(2) C(4) S(6) 115.6(2) yes . . . S(2) C(4) C(3) 116.8(3) yes . . . S(6) C(4) C(3) 127.6(3) yes . . . S(3) C(5) C(6) 116.8(3) yes . . . S(3) C(5) C(7) 117.0(2) yes . . . C(6) C(5) C(7) 126.2(3) yes . . . S(4) C(6) S(9) 119.1(2) yes . . . S(4) C(6) C(5) 113.3(3) yes . . . S(9) C(6) C(5) 127.6(3) yes . . . S(7) C(7) S(8) 115.3(2) yes . . . S(7) C(7) C(5) 119.6(3) yes . . . S(8) C(7) C(5) 125.0(2) yes . . . S(7) C(8) C(9) 115.2(3) yes . . . S(7) C(8) C(12) 130.7(3) yes . . . C(9) C(8) C(12) 114.1(4) yes . . . S(8) C(9) C(8) 118.8(3) yes . . . S(8) C(9) C(14) 129.4(3) yes . . . C(8) C(9) C(14) 111.8(3) yes . . . S(5) C(10) C(11) 114.7(5) yes . . . S(6) C(11) C(10) 115.2(5) yes . . . C(8) C(12) C(13) 102.0(3) yes . . . C(12) C(13) C(14) 109.9(4) yes . . . C(9) C(14) C(13) 102.2(4) yes . . . S(5) C(10) H(1) 107.7 no . . . S(5) C(10) H(2) 108.6 no . . . C(11) C(10) H(1) 106.5 no . . . C(11) C(10) H(2) 109.8 no . . . H(1) C(10) H(2) 109.5 no . . . S(6) C(11) H(3) 107.8 no . . . S(6) C(11) H(4) 108.8 no . . . C(10) C(11) H(3) 106.4 no . . . C(10) C(11) H(4) 108.9 no . . . H(3) C(11) H(4) 109.5 no . . . C(8) C(12) H(5) 111.1 no . . . C(8) C(12) H(6) 111.2 no . . . C(13) C(12) H(5) 111.5 no . . . C(13) C(12) H(6) 111.4 no . . . H(5) C(12) H(6) 109.5 no . . . C(12) C(13) H(7) 109.2 no . . . C(12) C(13) H(8) 109.4 no . . . C(14) C(13) H(7) 109.3 no . . . C(14) C(13) H(8) 109.6 no . . . H(7) C(13) H(8) 109.5 no . . . C(9) C(14) H(9) 111.0 no . . . C(9) C(14) H(10) 111.2 no . . . C(13) C(14) H(9) 111.3 no . . . C(13) C(14) H(10) 111.6 no . . . H(9) C(14) H(10) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) S(1) C(3) S(5) -178.6(3) ? . . . . C(1) S(1) C(3) C(4) 1.5(5) ? . . . . C(3) S(1) C(1) S(2) -2.0(3) ? . . . . C(3) S(1) C(1) C(2) 177.9(5) ? . . . . C(1) S(2) C(4) S(6) 177.6(3) ? . . . . C(1) S(2) C(4) C(3) -0.7(5) ? . . . . C(4) S(2) C(1) S(1) 1.7(3) ? . . . . C(4) S(2) C(1) C(2) -178.1(5) ? . . . . C(2) S(3) C(5) C(6) -0.5(4) ? . . . . C(2) S(3) C(5) C(7) 179.9(3) ? . . . . C(5) S(3) C(2) S(4) 1.1(3) ? . . . . C(5) S(3) C(2) C(1) -179.7(5) ? . . . . C(2) S(4) C(6) S(9) -179.3(3) ? . . . . C(2) S(4) C(6) C(5) 0.9(4) ? . . . . C(6) S(4) C(2) S(3) -1.3(3) ? . . . . C(6) S(4) C(2) C(1) 179.5(5) ? . . . . C(3) S(5) C(10) C(11) -35.9(7) ? . . . . C(10) S(5) C(3) S(1) -178.1(3) ? . . . . C(10) S(5) C(3) C(4) 1.7(6) ? . . . . C(4) S(6) C(11) C(10) -55.6(5) ? . . . . C(11) S(6) C(4) S(2) -157.1(3) ? . . . . C(11) S(6) C(4) C(3) 21.1(6) ? . . . . C(7) S(7) C(8) C(9) -0.1(4) ? . . . . C(7) S(7) C(8) C(12) 179.0(6) ? . . . . C(8) S(7) C(7) S(8) 0.0(3) ? . . . . C(8) S(7) C(7) C(5) 176.6(4) ? . . . . C(7) S(8) C(9) C(8) -0.1(4) ? . . . . C(7) S(8) C(9) C(14) -178.7(5) ? . . . . C(9) S(8) C(7) S(7) 0.1(2) ? . . . . C(9) S(8) C(7) C(5) -176.4(5) ? . . . . S(1) C(1) C(2) S(3) 1.1(7) ? . . . . S(1) C(1) C(2) S(4) -179.8(3) ? . . . . S(2) C(1) C(2) S(3) -179.1(3) ? . . . . S(2) C(1) C(2) S(4) 0.1(6) ? . . . . S(1) C(3) C(4) S(2) -0.6(6) ? . . . . S(1) C(3) C(4) S(6) -178.7(3) ? . . . . S(5) C(3) C(4) S(2) 179.6(3) ? . . . . S(5) C(3) C(4) S(6) 1.5(9) ? . . . . S(3) C(5) C(6) S(4) -0.3(5) ? . . . . S(3) C(5) C(6) S(9) 180.0(3) ? . . . . S(3) C(5) C(7) S(7) -0.3(5) ? . . . . S(3) C(5) C(7) S(8) 176.0(3) ? . . . . C(6) C(5) C(7) S(7) -179.8(4) ? . . . . C(6) C(5) C(7) S(8) -3.5(8) ? . . . . C(7) C(5) C(6) S(4) 179.2(4) ? . . . . C(7) C(5) C(6) S(9) -0.5(8) ? . . . . S(7) C(8) C(9) S(8) 0.1(5) ? . . . . S(7) C(8) C(9) C(14) 179.0(4) ? . . . . S(7) C(8) C(12) C(13) -179.6(5) ? . . . . C(9) C(8) C(12) C(13) -0.4(7) ? . . . . C(12) C(8) C(9) S(8) -179.1(4) ? . . . . C(12) C(8) C(9) C(14) -0.3(7) ? . . . . S(8) C(9) C(14) C(13) 179.6(5) ? . . . . C(8) C(9) C(14) C(13) 0.9(7) ? . . . . S(5) C(10) C(11) S(6) 68.1(7) ? . . . . C(8) C(12) C(13) C(14) 1.0(7) ? . . . . C(12) C(13) C(14) C(9) -1.1(7) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) S(2) 3.2714(18) ? . 2_666 Cl(1) S(6) 3.593(2) ? . 2_666 Cl(3) S(7) 3.5239(16) ? . . Cl(3) C(14) 3.583(4) ? . 1_445 Cl(4) C(14) 3.590(5) ? . 2_665 S(2) Cl(1) 3.2714(18) ? . 2_666 S(2) C(6) 3.508(5) ? . 2_766 S(3) C(4) 3.585(6) ? . 2_666 S(4) C(3) 3.576(5) ? . 2_666 S(6) Cl(1) 3.593(2) ? . 2_666 S(7) Cl(3) 3.5239(16) ? . . S(9) C(4) 3.461(6) ? . 2_766 C(1) C(1) 3.435(8) ? . 2_666 C(3) S(4) 3.576(5) ? . 2_666 C(4) S(3) 3.585(6) ? . 2_666 C(4) S(9) 3.461(6) ? . 2_766 C(6) S(2) 3.508(5) ? . 2_766 C(14) Cl(3) 3.583(4) ? . 1_665 C(14) Cl(4) 3.590(5) ? . 2_665 Cl(1) H(1) 3.365 ? . 2_556 Cl(1) H(2) 3.111 ? . 2_556 Cl(2) H(1) 3.463 ? . 2_556 Cl(2) H(2) 3.259 ? . 2_556 Cl(2) H(4) 2.985 ? . 2_556 Cl(2) H(5) 2.976 ? . 1_455 Cl(2) H(6) 3.132 ? . 2_555 Cl(2) H(8) 3.240 ? . 2_555 Cl(2) H(9) 3.073 ? . 1_445 Cl(3) H(3) 3.332 ? . 2_656 Cl(3) H(4) 3.008 ? . 2_656 Cl(3) H(5) 3.499 ? . . Cl(3) H(6) 3.243 ? . . Cl(3) H(7) 3.005 ? . 2_655 Cl(3) H(9) 3.253 ? . 1_445 Cl(3) H(10) 3.197 ? . 1_445 Cl(4) H(6) 3.135 ? . . Cl(4) H(7) 3.568 ? . 1_455 Cl(4) H(8) 3.390 ? . 2_665 Cl(4) H(9) 3.157 ? . 2_665 Cl(4) H(10) 3.073 ? . 1_455 Cl(4) H(10) 3.494 ? . 2_665 S(3) H(2) 3.436 ? . 2_656 S(7) H(2) 3.274 ? . 2_656 S(8) H(1) 3.128 ? . 2_666 S(8) H(3) 3.519 ? . 2_766 S(9) H(1) 2.992 ? . 2_666 S(9) H(3) 3.175 ? . 2_766 C(5) H(1) 3.369 ? . 2_666 C(6) H(1) 3.179 ? . 2_666 C(7) H(1) 3.369 ? . 2_666 C(12) H(5) 3.472 ? . 2_655 C(13) H(8) 3.415 ? . 2_665 C(13) H(10) 3.222 ? . 2_765 C(14) H(7) 3.422 ? . 2_765 C(14) H(8) 3.495 ? . 2_665 C(14) H(10) 3.216 ? . 2_765 H(1) Cl(1) 3.365 ? . 2_556 H(1) Cl(2) 3.463 ? . 2_556 H(1) S(8) 3.128 ? . 2_666 H(1) S(9) 2.992 ? . 2_666 H(1) C(5) 3.369 ? . 2_666 H(1) C(6) 3.179 ? . 2_666 H(1) C(7) 3.369 ? . 2_666 H(2) Cl(1) 3.111 ? . 2_556 H(2) Cl(2) 3.259 ? . 2_556 H(2) S(3) 3.436 ? . 2_656 H(2) S(7) 3.274 ? . 2_656 H(3) Cl(3) 3.332 ? . 2_656 H(3) S(8) 3.519 ? . 2_766 H(3) S(9) 3.175 ? . 2_766 H(4) Cl(2) 2.985 ? . 2_556 H(4) Cl(3) 3.008 ? . 2_656 H(5) Cl(2) 2.976 ? . 1_655 H(5) Cl(3) 3.499 ? . . H(5) C(12) 3.472 ? . 2_655 H(5) H(5) 2.741 ? . 2_655 H(5) H(6) 3.447 ? . 2_655 H(6) Cl(2) 3.132 ? . 2_555 H(6) Cl(3) 3.243 ? . . H(6) Cl(4) 3.135 ? . . H(6) H(5) 3.447 ? . 2_655 H(6) H(8) 3.404 ? . 2_665 H(6) H(9) 3.049 ? . 2_665 H(7) Cl(3) 3.005 ? . 2_655 H(7) Cl(4) 3.568 ? . 1_655 H(7) C(14) 3.422 ? . 2_765 H(7) H(9) 3.597 ? . 2_765 H(7) H(10) 2.532 ? . 2_765 H(8) Cl(2) 3.240 ? . 2_555 H(8) Cl(4) 3.390 ? . 2_665 H(8) C(13) 3.415 ? . 2_665 H(8) C(14) 3.495 ? . 2_665 H(8) H(6) 3.404 ? . 2_665 H(8) H(8) 2.801 ? . 2_665 H(8) H(9) 2.951 ? . 2_665 H(9) Cl(2) 3.073 ? . 1_665 H(9) Cl(3) 3.253 ? . 1_665 H(9) Cl(4) 3.157 ? . 2_665 H(9) H(6) 3.049 ? . 2_665 H(9) H(7) 3.597 ? . 2_765 H(9) H(8) 2.951 ? . 2_665 H(10) Cl(3) 3.197 ? . 1_665 H(10) Cl(4) 3.073 ? . 1_655 H(10) Cl(4) 3.494 ? . 2_665 H(10) C(13) 3.222 ? . 2_765 H(10) C(14) 3.216 ? . 2_765 H(10) H(7) 2.532 ? . 2_765 H(10) H(10) 2.560 ? . 2_765 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'CCDC-715843.cif' data__EDT-CP-TTFVS-FeBr4 _database_code_depnum_ccdc_archive 'CCDC 715843' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C14 H10 Br4 Fe S9 ' _chemical_formula_moiety 'C14 H10 Br4 Fe S9 ' _chemical_formula_weight 842.24 _chemical_melting_point 436 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.8986(6) _cell_length_b 8.9341(7) _cell_length_c 19.6260(14) _cell_angle_alpha 97.549(2) _cell_angle_beta 99.3134(18) _cell_angle_gamma 111.839(2) _cell_volume 1240.54(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6469 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 2.255 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808.00 _exptl_absorpt_coefficient_mu 7.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.061 _exptl_absorpt_correction_T_max 0.731 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 12281 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5627 _reflns_number_gt 2481 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.0758 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2504 _refine_ls_number_parameters 263 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 10.4947 5.3748 8.0925 ; _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.13 _refine_diff_density_min -1.50 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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(1) Br 0.84467(19) 0.67594(15) 0.89276(7) 0.0702(4) Uani 1.00 1 d . . . Br(2) Br 0.76708(15) 1.06611(13) 0.87675(7) 0.0663(3) Uani 1.00 1 d . . . Br(3) Br 1.25628(14) 1.06991(15) 0.88168(6) 0.0653(3) Uani 1.00 1 d . . . Br(4) Br 0.8615(2) 0.83665(15) 0.72262(6) 0.0797(3) Uani 1.00 1 d . . . Fe(1) Fe 0.93450(18) 0.91151(16) 0.84568(7) 0.0431(3) Uani 1.00 1 d . . . S(1) S 0.4718(3) 0.2021(2) 0.49356(11) 0.0422(6) Uani 1.00 1 d . . . S(2) S 0.7288(3) 0.5024(2) 0.59401(12) 0.0403(5) Uani 1.00 1 d . . . S(3) S 0.6558(3) 0.3625(2) 0.36872(12) 0.0437(6) Uani 1.00 1 d . . . S(4) S 0.9054(2) 0.6571(2) 0.47238(11) 0.0384(5) Uani 1.00 1 d . . . S(5) S 0.2992(3) 0.0316(3) 0.59820(16) 0.0586(8) Uani 1.00 1 d . . . S(6) S 0.6101(3) 0.3961(3) 0.71966(13) 0.0539(7) Uani 1.00 1 d . . . S(7) S 0.6331(3) 0.3071(3) 0.21026(12) 0.0518(6) Uani 1.00 1 d . . . S(8) S 0.9194(3) 0.6289(2) 0.21782(11) 0.0406(6) Uani 1.00 1 d . . . S(9) S 1.0951(3) 0.8287(2) 0.37098(13) 0.0437(6) Uani 1.00 1 d . . . C(1) C 0.6495(10) 0.3939(10) 0.5075(4) 0.034(2) Uani 1.00 1 d . . . C(2) C 0.7283(11) 0.4630(10) 0.4553(4) 0.035(2) Uani 1.00 1 d . . . C(3) C 0.4631(11) 0.2091(11) 0.5817(5) 0.041(2) Uani 1.00 1 d . . . C(4) C 0.5795(12) 0.3487(11) 0.6286(4) 0.037(2) Uani 1.00 1 d . . . C(5) C 0.8104(10) 0.5178(10) 0.3356(4) 0.034(2) Uani 1.00 1 d . . . C(6) C 0.9340(10) 0.6622(10) 0.3856(4) 0.034(2) Uani 1.00 1 d . . . C(7) C 0.7961(10) 0.4898(10) 0.2622(4) 0.035(2) Uani 1.00 1 d . . . C(8) C 0.6757(11) 0.3565(11) 0.1304(4) 0.040(2) Uani 1.00 1 d . . . C(9) C 0.8052(10) 0.5065(10) 0.1353(4) 0.033(2) Uani 1.00 1 d . . . C(10) C 0.334(2) 0.079(2) 0.6912(8) 0.107(6) Uani 1.00 1 d . . . C(11) C 0.507(2) 0.187(2) 0.7328(9) 0.118(6) Uani 1.00 1 d . . . C(12) C 0.5894(14) 0.2588(12) 0.0562(5) 0.051(2) Uani 1.00 1 d . . . C(13) C 0.6853(16) 0.3846(14) 0.0140(5) 0.065(3) Uani 1.00 1 d . . . C(14) C 0.8355(13) 0.5373(11) 0.0641(4) 0.046(2) Uani 1.00 1 d . . . H(1) H 0.2496 0.1280 0.7007 0.125 Uiso 1.00 1 c R . . H(2) H 0.3004 -0.0225 0.7066 0.125 Uiso 1.00 1 c R . . H(3) H 0.5916 0.1368 0.7245 0.140 Uiso 1.00 1 c R . . H(4) H 0.4992 0.1943 0.7808 0.140 Uiso 1.00 1 c R . . H(5) H 0.6167 0.1639 0.0486 0.056 Uiso 1.00 1 c R . . H(6) H 0.4575 0.2264 0.0457 0.056 Uiso 1.00 1 c R . . H(7) H 0.7395 0.3368 -0.0175 0.071 Uiso 1.00 1 c R . . H(8) H 0.5948 0.4143 -0.0121 0.071 Uiso 1.00 1 c R . . H(9) H 0.8195 0.6345 0.0563 0.055 Uiso 1.00 1 c R . . H(10) H 0.9568 0.5473 0.0593 0.055 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0949(8) 0.0606(7) 0.0630(7) 0.0310(6) 0.0230(6) 0.0335(5) Br(2) 0.0518(6) 0.0444(6) 0.0956(9) 0.0138(4) 0.0176(5) 0.0065(5) Br(3) 0.0452(5) 0.0678(8) 0.0689(7) 0.0128(5) 0.0063(5) 0.0060(5) Br(4) 0.1093(10) 0.0543(7) 0.0362(6) -0.0056(6) 0.0089(6) 0.0050(5) Fe(1) 0.0481(7) 0.0368(7) 0.0349(7) 0.0083(5) 0.0060(6) 0.0074(5) S(1) 0.0423(11) 0.0389(13) 0.0327(12) 0.0028(9) 0.0102(10) 0.0040(9) S(2) 0.0426(11) 0.0380(12) 0.0285(11) 0.0063(9) 0.0033(9) 0.0037(9) S(3) 0.0483(12) 0.0354(12) 0.0292(11) -0.0019(9) 0.0053(10) 0.0068(9) S(4) 0.0381(10) 0.0332(12) 0.0315(12) 0.0038(8) 0.0017(9) 0.0055(9) S(5) 0.0613(15) 0.0469(15) 0.0630(17) 0.0080(12) 0.0328(13) 0.0145(12) S(6) 0.0634(15) 0.0685(17) 0.0308(12) 0.0255(13) 0.0153(11) 0.0113(11) S(7) 0.0619(14) 0.0379(14) 0.0286(12) -0.0082(10) 0.0069(11) 0.0066(9) S(8) 0.0448(12) 0.0341(12) 0.0306(11) 0.0021(9) 0.0082(10) 0.0078(9) S(9) 0.0422(11) 0.0331(12) 0.0445(13) 0.0024(9) 0.0092(10) 0.0101(9) C(1) 0.033(4) 0.033(4) 0.027(4) 0.005(3) 0.002(3) 0.008(3) C(2) 0.039(4) 0.032(4) 0.030(4) 0.010(3) 0.004(3) 0.006(3) C(3) 0.037(4) 0.044(5) 0.043(5) 0.015(4) 0.010(4) 0.013(4) C(4) 0.045(4) 0.040(5) 0.035(4) 0.021(4) 0.017(4) 0.011(3) C(5) 0.035(4) 0.032(4) 0.025(4) 0.004(3) -0.001(3) 0.009(3) C(6) 0.030(4) 0.033(4) 0.033(4) 0.010(3) 0.002(3) 0.007(3) C(7) 0.028(3) 0.031(4) 0.039(4) 0.002(3) 0.006(3) 0.014(3) C(8) 0.040(4) 0.040(5) 0.033(4) 0.010(4) 0.004(4) 0.010(3) C(9) 0.034(4) 0.034(4) 0.028(4) 0.009(3) 0.007(3) 0.007(3) C(10) 0.130(13) 0.106(12) 0.076(9) 0.016(10) 0.055(9) 0.044(8) C(11) 0.094(10) 0.158(16) 0.097(12) 0.019(10) 0.035(9) 0.092(12) C(12) 0.058(5) 0.037(5) 0.043(5) 0.003(4) 0.021(4) 0.004(4) C(13) 0.081(7) 0.065(7) 0.032(5) 0.009(5) 0.022(5) -0.001(4) C(14) 0.057(5) 0.042(5) 0.037(5) 0.016(4) 0.017(4) 0.011(4) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics Ortep3 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Fe(1) 2.3235(19) yes . . Br(2) Fe(1) 2.330(2) yes . . Br(3) Fe(1) 2.3327(15) yes . . Br(4) Fe(1) 2.3347(17) yes . . S(1) C(1) 1.716(7) yes . . S(1) C(3) 1.736(10) yes . . S(2) C(1) 1.728(7) yes . . S(2) C(4) 1.742(9) yes . . S(3) C(2) 1.710(8) yes . . S(3) C(5) 1.752(8) yes . . S(4) C(2) 1.723(7) yes . . S(4) C(6) 1.759(9) yes . . S(5) C(3) 1.743(9) yes . . S(5) C(10) 1.771(15) yes . . S(6) C(4) 1.737(9) yes . . S(6) C(11) 1.81(2) yes . . S(7) C(7) 1.713(7) yes . . S(7) C(8) 1.734(10) yes . . S(8) C(7) 1.707(9) yes . . S(8) C(9) 1.721(7) yes . . S(9) C(6) 1.653(8) yes . . C(1) C(2) 1.380(12) yes . . C(3) C(4) 1.349(10) yes . . C(5) C(6) 1.414(9) yes . . C(5) C(7) 1.408(12) yes . . C(8) C(9) 1.329(11) yes . . C(8) C(12) 1.499(11) yes . . C(9) C(14) 1.499(13) yes . . C(10) C(11) 1.39(2) yes . . C(12) C(13) 1.529(15) yes . . C(13) C(14) 1.516(11) yes . . C(10) H(1) 0.950 no . . C(10) H(2) 0.950 no . . C(11) H(3) 0.950 no . . C(11) H(4) 0.950 no . . C(12) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(13) H(8) 0.950 no . . C(14) H(9) 0.950 no . . C(14) H(10) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Fe(1) Br(2) 109.50(7) yes . . . Br(1) Fe(1) Br(3) 112.12(7) yes . . . Br(1) Fe(1) Br(4) 109.61(6) yes . . . Br(2) Fe(1) Br(3) 110.76(6) yes . . . Br(2) Fe(1) Br(4) 107.49(8) yes . . . Br(3) Fe(1) Br(4) 107.22(7) yes . . . C(1) S(1) C(3) 95.5(3) yes . . . C(1) S(2) C(4) 95.8(3) yes . . . C(2) S(3) C(5) 97.1(3) yes . . . C(2) S(4) C(6) 97.9(3) yes . . . C(3) S(5) C(10) 102.4(6) yes . . . C(4) S(6) C(11) 97.6(6) yes . . . C(7) S(7) C(8) 96.1(4) yes . . . C(7) S(8) C(9) 95.0(3) yes . . . S(1) C(1) S(2) 115.3(5) yes . . . S(1) C(1) C(2) 124.6(5) yes . . . S(2) C(1) C(2) 120.1(5) yes . . . S(3) C(2) S(4) 115.1(5) yes . . . S(3) C(2) C(1) 122.4(5) yes . . . S(4) C(2) C(1) 122.5(5) yes . . . S(1) C(3) S(5) 114.7(4) yes . . . S(1) C(3) C(4) 117.5(7) yes . . . S(5) C(3) C(4) 127.9(8) yes . . . S(2) C(4) S(6) 114.5(4) yes . . . S(2) C(4) C(3) 115.8(7) yes . . . S(6) C(4) C(3) 129.6(7) yes . . . S(3) C(5) C(6) 116.3(6) yes . . . S(3) C(5) C(7) 117.4(5) yes . . . C(6) C(5) C(7) 126.3(7) yes . . . S(4) C(6) S(9) 118.6(4) yes . . . S(4) C(6) C(5) 113.7(6) yes . . . S(9) C(6) C(5) 127.7(7) yes . . . S(7) C(7) S(8) 115.3(5) yes . . . S(7) C(7) C(5) 119.1(6) yes . . . S(8) C(7) C(5) 125.5(5) yes . . . S(7) C(8) C(9) 115.0(6) yes . . . S(7) C(8) C(12) 130.8(6) yes . . . C(9) C(8) C(12) 114.2(8) yes . . . S(8) C(9) C(8) 118.7(7) yes . . . S(8) C(9) C(14) 129.9(5) yes . . . C(8) C(9) C(14) 111.4(6) yes . . . S(5) C(10) C(11) 120.4(14) yes . . . S(6) C(11) C(10) 119.5(15) yes . . . C(8) C(12) C(13) 101.2(6) yes . . . C(12) C(13) C(14) 109.7(7) yes . . . C(9) C(14) C(13) 103.0(7) yes . . . S(5) C(10) H(1) 106.5 no . . . S(5) C(10) H(2) 107.0 no . . . C(11) C(10) H(1) 105.4 no . . . C(11) C(10) H(2) 107.8 no . . . H(1) C(10) H(2) 109.5 no . . . S(6) C(11) H(3) 107.1 no . . . S(6) C(11) H(4) 106.8 no . . . C(10) C(11) H(3) 105.7 no . . . C(10) C(11) H(4) 108.0 no . . . H(3) C(11) H(4) 109.5 no . . . C(8) C(12) H(5) 111.5 no . . . C(8) C(12) H(6) 110.7 no . . . C(13) C(12) H(5) 111.8 no . . . C(13) C(12) H(6) 111.9 no . . . H(5) C(12) H(6) 109.5 no . . . C(12) C(13) H(7) 109.1 no . . . C(12) C(13) H(8) 109.2 no . . . C(14) C(13) H(7) 110.1 no . . . C(14) C(13) H(8) 109.3 no . . . H(7) C(13) H(8) 109.5 no . . . C(9) C(14) H(9) 110.6 no . . . C(9) C(14) H(10) 111.3 no . . . C(13) C(14) H(9) 111.6 no . . . C(13) C(14) H(10) 110.8 no . . . H(9) C(14) H(10) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) S(1) C(3) S(5) -178.6(6) ? . . . . C(1) S(1) C(3) C(4) 2.2(10) ? . . . . C(3) S(1) C(1) S(2) -1.9(7) ? . . . . C(3) S(1) C(1) C(2) 178.2(9) ? . . . . C(1) S(2) C(4) S(6) 177.8(6) ? . . . . C(1) S(2) C(4) C(3) 0.3(7) ? . . . . C(4) S(2) C(1) S(1) 1.2(7) ? . . . . C(4) S(2) C(1) C(2) -179.0(9) ? . . . . C(2) S(3) C(5) C(6) 0.1(6) ? . . . . C(2) S(3) C(5) C(7) -177.9(8) ? . . . . C(5) S(3) C(2) S(4) 0.4(6) ? . . . . C(5) S(3) C(2) C(1) 179.8(6) ? . . . . C(2) S(4) C(6) S(9) -179.7(5) ? . . . . C(2) S(4) C(6) C(5) 0.6(8) ? . . . . C(6) S(4) C(2) S(3) -0.6(7) ? . . . . C(6) S(4) C(2) C(1) 179.9(7) ? . . . . C(3) S(5) C(10) C(11) -28(2) ? . . . . C(10) S(5) C(3) S(1) 178.3(9) ? . . . . C(10) S(5) C(3) C(4) -2.6(13) ? . . . . C(4) S(6) C(11) C(10) -49.4(17) ? . . . . C(11) S(6) C(4) S(2) -158.0(8) ? . . . . C(11) S(6) C(4) C(3) 19.2(13) ? . . . . C(7) S(7) C(8) C(9) -1.3(9) ? . . . . C(7) S(7) C(8) C(12) 179.5(10) ? . . . . C(8) S(7) C(7) S(8) -0.1(5) ? . . . . C(8) S(7) C(7) C(5) 176.1(8) ? . . . . C(7) S(8) C(9) C(8) -2.1(9) ? . . . . C(7) S(8) C(9) C(14) -178.0(10) ? . . . . C(9) S(8) C(7) S(7) 1.1(6) ? . . . . C(9) S(8) C(7) C(5) -174.8(9) ? . . . . S(1) C(1) C(2) S(3) 0.0(13) ? . . . . S(1) C(1) C(2) S(4) 179.5(6) ? . . . . S(2) C(1) C(2) S(3) -179.8(5) ? . . . . S(2) C(1) C(2) S(4) -0.3(9) ? . . . . S(1) C(3) C(4) S(2) -1.7(12) ? . . . . S(1) C(3) C(4) S(6) -178.8(7) ? . . . . S(5) C(3) C(4) S(2) 179.2(6) ? . . . . S(5) C(3) C(4) S(6) 2.1(17) ? . . . . S(3) C(5) C(6) S(4) -0.5(10) ? . . . . S(3) C(5) C(6) S(9) 179.8(4) ? . . . . S(3) C(5) C(7) S(7) -0.9(11) ? . . . . S(3) C(5) C(7) S(8) 174.9(5) ? . . . . C(6) C(5) C(7) S(7) -178.7(8) ? . . . . C(6) C(5) C(7) S(8) -2.9(15) ? . . . . C(7) C(5) C(6) S(4) 177.3(8) ? . . . . C(7) C(5) C(6) S(9) -2.4(16) ? . . . . S(7) C(8) C(9) S(8) 2.3(12) ? . . . . S(7) C(8) C(9) C(14) 178.9(7) ? . . . . S(7) C(8) C(12) C(13) 176.1(9) ? . . . . C(9) C(8) C(12) C(13) -3.2(13) ? . . . . C(12) C(8) C(9) S(8) -178.3(8) ? . . . . C(12) C(8) C(9) C(14) -1.7(13) ? . . . . S(8) C(9) C(14) C(13) -178.1(9) ? . . . . C(8) C(9) C(14) C(13) 5.8(13) ? . . . . S(5) C(10) C(11) S(6) 59(2) ? . . . . C(8) C(12) C(13) C(14) 6.7(13) ? . . . . C(12) C(13) C(14) C(9) -7.7(13) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Br(2) S(7) 3.598(2) ? . 2_666 Br(4) S(2) 3.350(2) ? . . S(2) Br(4) 3.350(2) ? . . S(2) C(6) 3.485(10) ? . 2_766 S(4) C(2) 3.594(10) ? . 2_766 S(4) C(3) 3.598(11) ? . 2_666 S(7) Br(2) 3.598(2) ? . 2_666 S(9) C(4) 3.485(11) ? . 2_766 C(1) C(1) 3.536(14) ? . 2_666 C(2) S(4) 3.594(10) ? . 2_766 C(3) S(4) 3.598(11) ? . 2_666 C(4) S(9) 3.485(11) ? . 2_766 C(6) S(2) 3.485(10) ? . 2_766 Br(1) H(6) 3.181 ? . 2_666 Br(1) H(8) 3.428 ? . 1_556 Br(1) H(9) 3.309 ? . 1_556 Br(1) H(10) 3.109 ? . 2_766 Br(2) H(3) 3.324 ? . 1_565 Br(2) H(4) 3.227 ? . 1_565 Br(2) H(6) 3.280 ? . 2_666 Br(2) H(7) 3.069 ? . 1_566 Br(2) H(9) 3.276 ? . 2_776 Br(2) H(10) 3.260 ? . 2_776 Br(3) H(2) 3.531 ? . 1_665 Br(3) H(4) 3.010 ? . 1_665 Br(3) H(5) 3.018 ? . 2_766 Br(3) H(6) 3.218 ? . 1_666 Br(3) H(8) 3.369 ? . 1_666 Br(3) H(9) 3.063 ? . 2_776 Br(4) H(1) 3.338 ? . 1_665 Br(4) H(2) 3.303 ? . 1_665 S(3) H(2) 3.362 ? . 2_656 S(7) H(2) 3.349 ? . 2_656 S(8) H(1) 3.316 ? . 2_666 S(8) H(3) 3.539 ? . 2_766 S(9) H(1) 3.038 ? . 2_666 S(9) H(3) 3.289 ? . 2_766 C(5) H(1) 3.514 ? . 2_666 C(6) H(1) 3.247 ? . 2_666 C(7) H(1) 3.559 ? . 2_666 C(13) H(8) 3.328 ? . 2_665 C(13) H(10) 3.272 ? . 2_765 C(14) H(7) 3.439 ? . 2_765 C(14) H(8) 3.587 ? . 2_665 C(14) H(10) 3.296 ? . 2_765 H(1) Br(4) 3.338 ? . 1_445 H(1) S(8) 3.316 ? . 2_666 H(1) S(9) 3.038 ? . 2_666 H(1) C(5) 3.514 ? . 2_666 H(1) C(6) 3.247 ? . 2_666 H(1) C(7) 3.559 ? . 2_666 H(2) Br(3) 3.531 ? . 1_445 H(2) Br(4) 3.303 ? . 1_445 H(2) S(3) 3.362 ? . 2_656 H(2) S(7) 3.349 ? . 2_656 H(3) Br(2) 3.324 ? . 1_545 H(3) S(8) 3.539 ? . 2_766 H(3) S(9) 3.289 ? . 2_766 H(4) Br(2) 3.227 ? . 1_545 H(4) Br(3) 3.010 ? . 1_445 H(5) Br(3) 3.018 ? . 2_766 H(5) H(5) 2.998 ? . 2_655 H(5) H(6) 3.516 ? . 2_655 H(6) Br(1) 3.181 ? . 2_666 H(6) Br(2) 3.280 ? . 2_666 H(6) Br(3) 3.218 ? . 1_444 H(6) H(5) 3.516 ? . 2_655 H(6) H(8) 3.517 ? . 2_665 H(6) H(9) 3.406 ? . 2_665 H(7) Br(2) 3.069 ? . 1_544 H(7) C(14) 3.439 ? . 2_765 H(7) H(10) 2.552 ? . 2_765 H(8) Br(1) 3.428 ? . 1_554 H(8) Br(3) 3.369 ? . 1_444 H(8) C(13) 3.328 ? . 2_665 H(8) C(14) 3.587 ? . 2_665 H(8) H(6) 3.517 ? . 2_665 H(8) H(8) 2.562 ? . 2_665 H(8) H(9) 3.094 ? . 2_665 H(9) Br(1) 3.309 ? . 1_554 H(9) Br(2) 3.276 ? . 2_776 H(9) Br(3) 3.063 ? . 2_776 H(9) H(6) 3.406 ? . 2_665 H(9) H(8) 3.094 ? . 2_665 H(10) Br(1) 3.109 ? . 2_766 H(10) Br(2) 3.260 ? . 2_776 H(10) C(13) 3.272 ? . 2_765 H(10) C(14) 3.296 ? . 2_765 H(10) H(7) 2.552 ? . 2_765 H(10) H(10) 2.652 ? . 2_765 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================