data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _audit_creation_date 2005-06-21 _audit_creation_method 'by CrystalStructure v3.5.1' _audit_update_record ? _publ_contact_author_name 'Toyonari Sugimoto' _publ_contact_author_address ; Gakuenntyou1-2, Sakai, Osaka, Japan ; _publ_contact_author_email toyonari@riast.osakafu-u.ac.jp _publ_contact_author_fax ' 072-252-4175 ' _publ_contact_author_phone ' 072-254-9817 ' _publ_section_title ; Metallic/semiconducting behaviors and an antiferromagnetic ordering of FeBr4A | d spins in (Benzo-TTFVS)2A A MX4 (M = Fe, Ga; X = Cl, Br) ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2003). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.5.1. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'Toyonari Sugimoto' 'Hideki Fujiwara' 'Takashi Hiraoka' 'Takekazu Ishida' 'Yohsuke Kamada' 'Hiroko Aruga Katori' ; T.Matsumoto ; 'Hiroyuki Nakazumi' 'Satoru Noguchi' #============================================================================== data_FeCl4salt _database_code_depnum_ccdc_archive 'CCDC 271654' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C13 H6 Cl2 Fe0.50 S7 ' _chemical_formula_moiety 'C13 H6 Cl2 Fe0.50 S7 ' _chemical_formula_weight 485.44 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z x,-y+1/2,z #------------------------------------------------------------------------------ _cell_length_a 7.0447(9) _cell_length_b 34.734(3) _cell_length_c 7.622(1) _cell_angle_alpha 90 _cell_angle_beta 105.980(3) _cell_angle_gamma 90 _cell_volume 1793.0(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10150 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.3 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972.00 _exptl_absorpt_coefficient_mu 1.556 _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 0.716 _exptl_absorpt_correction_T_max 0.954 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 16156 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9964 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9964 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement 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 4180 _reflns_number_gt 1831 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0240 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1845 _refine_ls_number_parameters 214 _refine_ls_goodness_of_fit_ref 1.544 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.59 _refine_diff_density_min -0.63 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 0.6493(2) 0.2500 0.7685(2) 0.0710(5) Uani 1.00 1 d . . . Cl(1) Cl 0.4727(3) 0.19832(5) 0.6863(3) 0.1134(8) Uani 1.00 1 d . . . Cl(2) Cl 0.8978(4) 0.2500 0.6478(4) 0.101(1) Uani 1.00 1 d . . . Cl(3) Cl 0.7650(5) 0.2500 1.0638(3) 0.124(1) Uani 1.00 1 d . . . S(1) S 0.7910(2) 0.03174(4) 1.2876(2) 0.0457(5) Uani 1.00 1 d . . . S(2) S 0.7126(2) 0.07688(4) 0.9487(2) 0.0480(5) Uani 1.00 1 d . . . S(3) S 0.7773(2) -0.04633(4) 1.0531(2) 0.0453(5) Uani 1.00 1 d . . . S(4) S 0.7077(2) -0.00077(4) 0.7188(2) 0.0483(5) Uani 1.00 1 d . . . S(5) S 0.6826(2) -0.06748(4) 0.4772(2) 0.0546(5) Uani 1.00 1 d . . . S(6) S 0.7989(2) -0.13449(4) 1.0659(2) 0.0642(6) Uani 1.00 1 d . . . S(7) S 0.7278(2) -0.14253(4) 0.6755(2) 0.0556(5) Uani 1.00 1 d . . . C(1) C 0.8086(7) 0.1398(2) 1.4795(8) 0.057(2) Uani 1.00 1 d . . . C(2) C 0.7717(8) 0.1610(1) 1.3203(9) 0.056(2) Uani 1.00 1 d . . . C(3) C 0.8172(7) 0.1002(2) 1.4768(7) 0.049(2) Uani 1.00 1 d . . . C(4) C 0.7399(8) 0.1432(1) 1.1527(8) 0.049(2) Uani 1.00 1 d . . . C(5) C 0.7871(7) 0.0820(1) 1.3093(8) 0.040(2) Uani 1.00 1 d . . . C(6) C 0.7496(7) 0.1031(1) 1.1491(7) 0.038(2) Uani 1.00 1 d . . . C(7) C 0.7505(6) 0.0321(1) 1.0527(7) 0.037(2) Uani 1.00 1 d . . . C(8) C 0.7466(6) -0.0008(1) 0.9543(7) 0.039(2) Uani 1.00 1 d . . . C(9) C 0.7465(7) -0.0722(1) 0.8479(7) 0.036(2) Uani 1.00 1 d . . . C(10) C 0.7141(7) -0.0507(1) 0.6872(7) 0.039(2) Uani 1.00 1 d . . . C(11) C 0.7567(7) -0.1116(1) 0.8582(7) 0.040(2) Uani 1.00 1 d . . . C(12) C 0.7938(9) -0.1810(2) 0.9823(9) 0.076(3) Uani 1.00 1 d . . . C(13) C 0.7602(8) -0.1841(2) 0.8046(9) 0.069(2) Uani 1.00 1 d . . . H(1) H 0.8295 0.1527 1.5932 0.066 Uiso 1.00 1 c . . . H(2) H 0.7696 0.1883 1.3284 0.066 Uiso 1.00 1 c . . . H(3) H 0.8411 0.0854 1.5856 0.058 Uiso 1.00 1 c . . . H(4) H 0.7108 0.1579 1.0432 0.057 Uiso 1.00 1 c . . . H(5) H 0.8133 -0.2026 1.0617 0.089 Uiso 1.00 1 c . . . H(6) H 0.7546 -0.2086 0.7479 0.083 Uiso 1.00 1 c . . . 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) 0.099(1) 0.0562(9) 0.0541(9) 0.0000 0.0149(8) 0.0000 Cl(1) 0.138(2) 0.112(2) 0.099(2) -0.055(1) 0.046(1) -0.040(1) Cl(2) 0.096(2) 0.097(2) 0.113(2) 0.0000 0.035(2) 0.0000 Cl(3) 0.227(4) 0.069(2) 0.056(2) 0.0000 0.009(2) 0.0000 S(1) 0.051(1) 0.044(1) 0.042(1) -0.0025(8) 0.0147(8) 0.0009(8) S(2) 0.050(1) 0.051(1) 0.041(1) -0.0011(8) 0.0073(8) 0.0009(8) S(3) 0.046(1) 0.0491(9) 0.042(1) -0.0026(8) 0.0148(8) 0.0002(8) S(4) 0.056(1) 0.0470(9) 0.041(1) 0.0005(8) 0.0107(8) -0.0006(8) S(5) 0.061(1) 0.059(1) 0.039(1) 0.0036(9) 0.0063(8) -0.0028(8) S(6) 0.074(1) 0.059(1) 0.055(1) 0.003(1) 0.0096(9) 0.013(1) S(7) 0.058(1) 0.046(1) 0.060(1) 0.0010(9) 0.0110(9) -0.0066(9) C(1) 0.057(4) 0.058(4) 0.051(5) 0.005(4) 0.007(3) -0.020(4) C(2) 0.056(4) 0.045(4) 0.065(5) 0.012(3) 0.011(4) 0.005(4) C(3) 0.052(4) 0.049(4) 0.044(4) 0.006(3) 0.011(3) 0.003(3) C(4) 0.047(4) 0.046(4) 0.051(4) -0.004(3) 0.010(3) 0.000(4) C(5) 0.030(3) 0.042(4) 0.047(4) -0.002(3) 0.009(3) -0.006(3) C(6) 0.028(3) 0.047(4) 0.038(4) -0.004(3) 0.007(3) -0.001(3) C(7) 0.028(4) 0.046(3) 0.041(4) -0.005(3) 0.014(3) 0.001(3) C(8) 0.031(3) 0.046(3) 0.044(4) -0.003(3) 0.014(3) 0.006(3) C(9) 0.040(4) 0.034(3) 0.038(4) -0.000(3) 0.015(3) 0.000(3) C(10) 0.037(4) 0.038(3) 0.041(4) -0.005(3) 0.008(3) -0.002(3) C(11) 0.028(3) 0.050(4) 0.042(4) -0.002(3) 0.007(3) 0.004(3) C(12) 0.089(5) 0.048(4) 0.087(6) 0.008(4) 0.018(5) 0.014(4) C(13) 0.080(5) 0.045(4) 0.082(5) 0.007(4) 0.023(5) -0.001(4) #============================================================================== _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 Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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) 2.176(2) yes . . Fe(1) Cl(2) 2.190(3) yes . . Fe(1) Cl(3) 2.172(3) yes . . S(1) C(5) 1.754(5) yes . . S(1) C(7) 1.734(5) yes . . S(2) C(6) 1.736(6) yes . . S(2) C(7) 1.734(5) yes . . S(3) C(8) 1.738(5) yes . . S(3) C(9) 1.765(5) yes . . S(4) C(8) 1.740(5) yes . . S(4) C(10) 1.754(5) yes . . S(5) C(10) 1.659(5) yes . . S(6) C(11) 1.722(5) yes . . S(6) C(12) 1.733(6) yes . . S(7) C(11) 1.726(5) yes . . S(7) C(13) 1.727(6) yes . . C(1) C(2) 1.382(9) yes . . C(1) C(3) 1.377(8) yes . . C(2) C(4) 1.380(9) yes . . C(3) C(5) 1.387(8) yes . . C(4) C(6) 1.396(7) yes . . C(5) C(6) 1.387(8) yes . . C(7) C(8) 1.363(7) yes . . C(9) C(10) 1.398(7) yes . . C(9) C(11) 1.372(7) yes . . C(12) C(13) 1.314(9) yes . . 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) 109.80(8) yes . . . Cl(1) Fe(1) Cl(3) 108.67(8) yes . . . Cl(2) Fe(1) Cl(3) 108.7(1) yes . . . C(5) S(1) C(7) 95.1(3) yes . . . C(6) S(2) C(7) 95.9(2) yes . . . C(8) S(3) C(9) 96.3(2) yes . . . C(8) S(4) C(10) 97.9(3) yes . . . C(11) S(6) C(12) 96.4(3) yes . . . C(11) S(7) C(13) 95.3(3) yes . . . C(2) C(1) C(3) 121.2(5) yes . . . C(4) C(2) C(1) 121.2(5) yes . . . C(5) C(3) C(1) 118.2(5) yes . . . C(6) C(4) C(2) 117.9(5) yes . . . C(6) C(5) S(1) 116.6(4) yes . . . C(6) C(5) C(3) 120.9(5) yes . . . S(1) C(5) C(3) 122.5(4) yes . . . S(2) C(6) C(4) 123.0(4) yes . . . S(2) C(6) C(5) 116.3(4) yes . . . C(4) C(6) C(5) 120.6(5) yes . . . C(8) C(7) S(1) 122.4(4) yes . . . C(8) C(7) S(2) 121.6(4) yes . . . S(1) C(7) S(2) 116.0(3) yes . . . S(3) C(8) S(4) 114.4(3) yes . . . S(3) C(8) C(7) 122.9(4) yes . . . S(4) C(8) C(7) 122.7(4) yes . . . C(10) C(9) C(11) 125.2(5) yes . . . C(10) C(9) S(3) 117.1(4) yes . . . C(11) C(9) S(3) 117.7(4) yes . . . S(4) C(10) S(5) 118.5(3) yes . . . S(4) C(10) C(9) 114.3(4) yes . . . S(5) C(10) C(9) 127.1(4) yes . . . S(6) C(11) S(7) 114.0(3) yes . . . S(6) C(11) C(9) 120.4(4) yes . . . S(7) C(11) C(9) 125.6(4) yes . . . C(13) C(12) S(6) 115.8(5) yes . . . S(7) C(13) C(12) 118.5(5) yes . . . 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(7) S(1) C(5) C(3) -178.6(4) yes . . . . C(7) S(1) C(5) C(6) 2.2(4) yes . . . . C(5) S(1) C(7) S(2) -3.4(3) yes . . . . C(5) S(1) C(7) C(8) 177.2(4) yes . . . . C(7) S(2) C(6) C(4) 179.2(4) yes . . . . C(7) S(2) C(6) C(5) -1.8(4) yes . . . . C(6) S(2) C(7) S(1) 3.3(3) yes . . . . C(6) S(2) C(7) C(8) -177.3(4) yes . . . . C(9) S(3) C(8) S(4) -1.2(3) yes . . . . C(9) S(3) C(8) C(7) 178.2(4) yes . . . . C(8) S(3) C(9) C(10) 1.0(4) yes . . . . C(8) S(3) C(9) C(11) -179.1(4) yes . . . . C(10) S(4) C(8) S(3) 1.0(3) yes . . . . C(10) S(4) C(8) C(7) -178.4(4) yes . . . . C(8) S(4) C(10) S(5) 179.8(3) yes . . . . C(8) S(4) C(10) C(9) -0.3(4) yes . . . . C(12) S(6) C(11) S(7) 0.7(3) yes . . . . C(12) S(6) C(11) C(9) -180.0(5) yes . . . . C(11) S(6) C(12) C(13) -0.7(5) yes . . . . C(13) S(7) C(11) S(6) -0.4(3) yes . . . . C(13) S(7) C(11) C(9) -179.7(5) yes . . . . C(11) S(7) C(13) C(12) -0.1(5) yes . . . . C(3) C(1) C(2) C(4) 0.7(8) yes . . . . C(2) C(1) C(3) C(5) -0.2(8) yes . . . . C(1) C(2) C(4) C(6) -1.1(8) yes . . . . C(1) C(3) C(5) S(1) -179.1(4) yes . . . . C(1) C(3) C(5) C(6) 0.1(8) yes . . . . C(2) C(4) C(6) S(2) 179.9(4) yes . . . . C(2) C(4) C(6) C(5) 1.0(8) yes . . . . S(1) C(5) C(6) S(2) -0.2(6) yes . . . . S(1) C(5) C(6) C(4) 178.8(4) yes . . . . C(3) C(5) C(6) S(2) -179.5(4) yes . . . . C(3) C(5) C(6) C(4) -0.5(8) yes . . . . S(1) C(7) C(8) S(3) 1.1(6) yes . . . . S(1) C(7) C(8) S(4) -179.6(3) yes . . . . S(2) C(7) C(8) S(3) -178.2(3) yes . . . . S(2) C(7) C(8) S(4) 1.1(6) yes . . . . S(3) C(9) C(10) S(4) -0.5(6) yes . . . . S(3) C(9) C(10) S(5) 179.4(4) yes . . . . C(11) C(9) C(10) S(4) 179.7(4) yes . . . . C(11) C(9) C(10) S(5) -0.4(8) yes . . . . S(3) C(9) C(11) S(6) -0.2(6) yes . . . . S(3) C(9) C(11) S(7) 179.1(3) yes . . . . C(10) C(9) C(11) S(6) 179.6(4) yes . . . . C(10) C(9) C(11) S(7) -1.1(8) yes . . . . S(6) C(12) C(13) S(7) 0.6(7) yes . . . . 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 Fe(1) Cl(1) 2.176(2) yes . 55501 Fe(1) Cl(1) 2.176(2) yes . 55504 Fe(1) Cl(2) 2.190(3) yes . 55501 Fe(1) Cl(3) 2.172(3) yes . 55501 Cl(1) Fe(1) 2.176(2) yes . 55501 Cl(1) Cl(1) 3.590(2) yes . 55504 Cl(1) Cl(2) 3.572(3) yes . 55501 Cl(1) Cl(3) 3.532(3) yes . 55501 Cl(1) S(7) 3.348(2) yes . 65603 Cl(1) C(13) 3.682(6) yes . 65603 Cl(2) Fe(1) 2.190(3) yes . 55501 Cl(2) Cl(1) 3.572(3) yes . 55501 Cl(2) Cl(1) 3.572(3) yes . 55504 Cl(2) Cl(3) 3.544(4) yes . 55501 Cl(3) Fe(1) 2.172(3) yes . 55501 Cl(3) Cl(1) 3.532(3) yes . 55501 Cl(3) Cl(1) 3.532(3) yes . 55504 Cl(3) Cl(2) 3.544(4) yes . 55501 Cl(3) C(2) 3.651(6) yes . 55501 Cl(3) C(2) 3.651(6) yes . 55504 Cl(3) C(4) 3.783(5) yes . 55501 Cl(3) C(4) 3.783(5) yes . 55504 S(1) S(2) 2.941(2) yes . 55501 S(1) S(3) 3.235(2) yes . 55501 S(1) S(4) 3.672(2) yes . 55601 S(1) S(5) 3.893(2) yes . 55601 S(1) C(3) 2.760(6) yes . 55501 S(1) C(4) 3.997(5) yes . 55501 S(1) C(6) 2.679(5) yes . 55501 S(1) C(8) 2.719(5) yes . 55501 S(2) S(1) 2.941(2) yes . 55501 S(2) S(4) 3.211(2) yes . 55501 S(2) S(5) 3.663(2) yes . 65603 S(2) C(3) 3.971(6) yes . 55501 S(2) C(4) 2.757(6) yes . 55501 S(2) C(5) 2.659(6) yes . 55501 S(2) C(8) 2.709(5) yes . 55501 S(3) S(1) 3.235(2) yes . 55501 S(3) S(4) 2.924(2) yes . 55501 S(3) S(5) 3.553(2) yes . 55601 S(3) S(6) 3.066(2) yes . 55501 S(3) C(7) 2.729(5) yes . 55501 S(3) C(10) 2.705(5) yes . 55501 S(3) C(11) 2.692(5) yes . 55501 S(4) S(2) 3.211(2) yes . 55501 S(4) S(3) 2.924(2) yes . 55501 S(4) S(4) 3.783(2) yes . 65603 S(4) S(5) 2.935(2) yes . 55501 S(4) S(5) 3.626(2) yes . 65603 S(4) C(7) 2.729(5) yes . 55501 S(4) C(9) 2.655(5) yes . 55501 S(4) C(11) 3.984(5) yes . 55501 S(5) S(2) 3.663(2) yes . 65603 S(5) S(4) 2.935(2) yes . 55501 S(5) S(4) 3.626(2) yes . 65603 S(5) S(7) 2.986(2) yes . 55501 S(5) C(9) 2.741(6) yes . 55501 S(5) C(11) 3.197(5) yes . 55501 S(6) S(3) 3.066(2) yes . 55501 S(6) S(7) 2.892(2) yes . 55501 S(6) C(9) 2.691(5) yes . 55501 S(6) C(13) 2.591(6) yes . 55501 S(7) Cl(1) 3.348(2) yes . 65603 S(7) S(5) 2.986(2) yes . 55501 S(7) S(6) 2.892(2) yes . 55501 S(7) C(9) 2.760(5) yes . 55501 S(7) C(10) 3.192(5) yes . 55501 S(7) C(12) 2.621(7) yes . 55501 C(1) Cl(1) 3.778(7) yes . 55601 C(1) C(4) 2.406(8) yes . 55501 C(1) C(5) 2.372(8) yes . 55501 C(1) C(6) 2.749(8) yes . 55501 C(2) Cl(2) 3.919(6) yes . 55601 C(2) Cl(3) 3.651(6) yes . 55501 C(2) C(3) 2.404(8) yes . 55501 C(2) C(5) 2.749(7) yes . 55501 C(2) C(6) 2.378(8) yes . 55501 C(3) S(1) 2.760(6) yes . 55501 C(3) S(2) 3.971(6) yes . 55501 C(3) S(2) 3.949(6) yes . 55601 C(3) C(2) 2.404(8) yes . 55501 C(3) C(4) 2.810(8) yes . 55501 C(3) C(6) 2.413(8) yes . 55501 C(3) C(7) 3.928(7) yes . 55501 C(4) Cl(3) 3.783(5) yes . 55501 C(4) S(1) 3.997(5) yes . 55501 C(4) S(2) 2.757(6) yes . 55501 C(4) C(1) 2.406(8) yes . 55501 C(4) C(3) 2.810(8) yes . 55501 C(4) C(5) 2.417(7) yes . 55501 C(4) C(7) 3.941(7) yes . 55501 C(5) S(2) 2.659(6) yes . 55501 C(5) C(1) 2.372(8) yes . 55501 C(5) C(2) 2.749(7) yes . 55501 C(5) C(4) 2.417(7) yes . 55501 C(5) C(7) 2.573(7) yes . 55501 C(5) C(8) 3.906(7) yes . 55501 C(6) S(1) 2.679(5) yes . 55501 C(6) C(1) 2.749(8) yes . 55501 C(6) C(2) 2.378(8) yes . 55501 C(6) C(3) 2.413(8) yes . 55501 C(6) C(7) 2.576(7) yes . 55501 C(6) C(8) 3.902(7) yes . 55501 C(7) S(3) 2.729(5) yes . 55501 C(7) S(4) 2.729(5) yes . 55501 C(7) C(3) 3.928(7) yes . 55501 C(7) C(4) 3.941(7) yes . 55501 C(7) C(5) 2.573(7) yes . 55501 C(7) C(6) 2.576(7) yes . 55501 C(7) C(9) 3.940(7) yes . 55501 C(7) C(10) 3.962(7) yes . 55501 C(8) S(1) 2.719(5) yes . 55501 C(8) S(2) 2.709(5) yes . 55501 C(8) C(5) 3.906(7) yes . 55501 C(8) C(6) 3.902(7) yes . 55501 C(8) C(9) 2.608(7) yes . 55501 C(8) C(10) 2.635(7) yes . 55501 C(8) C(11) 3.921(7) yes . 55501 C(9) S(4) 2.655(5) yes . 55501 C(9) S(5) 2.741(6) yes . 55501 C(9) S(6) 2.691(5) yes . 55501 C(9) S(7) 2.760(5) yes . 55501 C(9) C(7) 3.940(7) yes . 55501 C(9) C(8) 2.608(7) yes . 55501 C(9) C(12) 3.905(8) yes . 55501 C(9) C(13) 3.904(7) yes . 55501 C(10) S(3) 2.705(5) yes . 55501 C(10) S(7) 3.192(5) yes . 55501 C(10) C(7) 3.962(7) yes . 55501 C(10) C(8) 2.635(7) yes . 55501 C(10) C(11) 2.459(7) yes . 55501 C(11) S(3) 2.692(5) yes . 55501 C(11) S(4) 3.984(5) yes . 55501 C(11) S(5) 3.197(5) yes . 55501 C(11) C(8) 3.921(7) yes . 55501 C(11) C(10) 2.459(7) yes . 55501 C(11) C(12) 2.576(8) yes . 55501 C(11) C(13) 2.552(7) yes . 55501 C(12) S(7) 2.621(7) yes . 55501 C(12) C(9) 3.905(8) yes . 55501 C(12) C(11) 2.576(8) yes . 55501 C(13) Cl(1) 3.682(6) yes . 65603 C(13) S(6) 2.591(6) yes . 55501 C(13) C(9) 3.904(7) yes . 55501 C(13) C(11) 2.552(7) yes . 55501 #============================================================================== # 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 #============================================================================== #===END data_GaCl4salt _database_code_depnum_ccdc_archive 'CCDC 271655' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C13 H6 Cl2 Ga0.50 S7 ' _chemical_formula_moiety 'C13 H6 Cl2 Ga0.50 S7 ' _chemical_formula_weight 492.38 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z x,-y+1/2,z #------------------------------------------------------------------------------ _cell_length_a 7.063(1) _cell_length_b 34.578(7) _cell_length_c 7.607(2) _cell_angle_alpha 90 _cell_angle_beta 106.17(1) _cell_angle_gamma 90 _cell_volume 1784.4(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7078 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982.00 _exptl_absorpt_coefficient_mu 1.912 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 8326 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9950 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9950 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement 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 4163 _reflns_number_gt 2077 _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 0.0270 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2103 _refine_ls_number_parameters 214 _refine_ls_goodness_of_fit_ref 1.940 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo)' _refine_ls_shift/su_max 0.0030 _refine_diff_density_max 0.61 _refine_diff_density_min -0.77 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; Ga Ga 0.231 1.608 ; 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 Ga(1) Ga 0.6477(2) 0.2500 0.7700(1) 0.0691(4) Uani 1.00 1 d . . . Cl(1) Cl 0.8915(4) 0.2500 0.6493(4) 0.097(1) Uani 1.00 1 d . . . Cl(2) Cl 0.4722(3) 0.19887(5) 0.6862(3) 0.1109(9) Uani 1.00 1 d . . . Cl(3) Cl 0.7626(5) 0.2500 1.0631(4) 0.118(1) Uani 1.00 1 d . . . S(1) S 0.7906(2) 0.03165(4) 1.2869(2) 0.0439(5) Uani 1.00 1 d . . . S(2) S 0.7126(2) 0.07679(4) 0.9483(2) 0.0468(5) Uani 1.00 1 d . . . S(3) S 0.7771(2) -0.04638(4) 1.0526(2) 0.0444(5) Uani 1.00 1 d . . . S(4) S 0.7077(2) -0.00071(4) 0.7182(2) 0.0468(5) Uani 1.00 1 d . . . S(5) S 0.6834(2) -0.06737(4) 0.4765(2) 0.0528(5) Uani 1.00 1 d . . . S(6) S 0.8004(3) -0.13422(4) 1.0660(2) 0.0636(6) Uani 1.00 1 d . . . S(7) S 0.7289(2) -0.14245(4) 0.6752(2) 0.0549(5) Uani 1.00 1 d . . . C(1) C 0.8085(8) 0.1390(2) 1.4807(8) 0.057(2) Uani 1.00 1 d . . . C(2) C 0.7689(9) 0.1608(1) 1.3211(9) 0.054(2) Uani 1.00 1 d . . . C(3) C 0.8165(8) 0.0997(2) 1.4787(7) 0.047(2) Uani 1.00 1 d . . . C(4) C 0.7390(8) 0.1424(1) 1.1545(8) 0.046(2) Uani 1.00 1 d . . . C(5) C 0.7867(8) 0.0817(1) 1.3103(8) 0.038(2) Uani 1.00 1 d . . . C(6) C 0.7477(8) 0.1029(1) 1.1492(8) 0.038(2) Uani 1.00 1 d . . . C(7) C 0.7508(7) 0.0317(1) 1.0498(7) 0.040(2) Uani 1.00 1 d . . . C(8) C 0.7464(7) -0.0011(1) 0.9539(7) 0.040(2) Uani 1.00 1 d . . . C(9) C 0.7476(8) -0.0720(1) 0.8469(7) 0.039(2) Uani 1.00 1 d . . . C(10) C 0.7158(8) -0.0504(1) 0.6864(7) 0.041(2) Uani 1.00 1 d . . . C(11) C 0.7581(8) -0.1118(1) 0.8575(7) 0.041(2) Uani 1.00 1 d . . . C(12) C 0.798(1) -0.1807(2) 0.9844(9) 0.070(3) Uani 1.00 1 d . . . C(13) C 0.765(1) -0.1842(2) 0.8053(9) 0.071(3) Uani 1.00 1 d . . . H(1) H 0.8316 0.1521 1.5945 0.068 Uiso 1.00 1 c . . . H(2) H 0.7637 0.1883 1.3278 0.063 Uiso 1.00 1 c . . . H(3) H 0.8405 0.0848 1.5877 0.056 Uiso 1.00 1 c . . . H(4) H 0.7114 0.1569 1.0442 0.054 Uiso 1.00 1 c . . . H(5) H 0.819 -0.2024 1.0647 0.082 Uiso 1.00 1 c . . . H(6) H 0.761 -0.2088 0.7493 0.085 Uiso 1.00 1 c . . . 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 Ga(1) 0.100(1) 0.0549(7) 0.0508(7) 0.0000 0.0173(7) 0.0000 Cl(1) 0.098(2) 0.097(2) 0.103(2) 0.0000 0.038(2) 0.0000 Cl(2) 0.143(2) 0.108(2) 0.091(2) -0.055(1) 0.047(2) -0.039(1) Cl(3) 0.214(4) 0.075(2) 0.050(2) 0.0000 0.011(2) 0.0000 S(1) 0.049(1) 0.0445(9) 0.0394(9) -0.0018(7) 0.0147(9) 0.0001(8) S(2) 0.051(1) 0.0500(9) 0.0371(9) -0.0008(8) 0.0089(8) -0.0002(8) S(3) 0.048(1) 0.0488(9) 0.0376(9) -0.0049(8) 0.0141(8) -0.0002(8) S(4) 0.057(1) 0.0442(8) 0.0383(9) 0.0003(8) 0.0120(8) -0.0007(8) S(5) 0.062(1) 0.056(1) 0.0368(9) 0.0028(8) 0.0088(9) -0.0042(8) S(6) 0.075(1) 0.059(1) 0.052(1) 0.002(1) 0.010(1) 0.0132(9) S(7) 0.059(1) 0.0468(9) 0.057(1) 0.0010(8) 0.0132(9) -0.0063(9) C(1) 0.060(5) 0.067(4) 0.044(4) -0.004(4) 0.015(4) -0.018(4) C(2) 0.054(4) 0.040(4) 0.064(5) 0.004(3) 0.012(4) 0.001(4) C(3) 0.050(4) 0.050(4) 0.040(4) 0.000(3) 0.013(3) -0.005(3) C(4) 0.040(4) 0.051(4) 0.044(4) 0.001(3) 0.005(3) 0.006(3) C(5) 0.034(4) 0.041(3) 0.041(4) -0.004(3) 0.013(3) -0.003(3) C(6) 0.036(4) 0.037(3) 0.044(4) 0.003(3) 0.013(3) -0.003(3) C(7) 0.028(4) 0.052(3) 0.041(4) -0.004(3) 0.012(3) -0.002(3) C(8) 0.034(4) 0.044(3) 0.045(4) -0.004(3) 0.015(3) 0.001(3) C(9) 0.040(4) 0.041(3) 0.036(4) -0.002(3) 0.010(3) -0.004(3) C(10) 0.034(4) 0.045(3) 0.041(4) -0.004(3) 0.007(3) -0.000(3) C(11) 0.037(4) 0.043(3) 0.040(4) 0.002(3) 0.003(3) 0.003(3) C(12) 0.084(6) 0.044(4) 0.077(5) 0.006(4) 0.017(5) 0.017(4) C(13) 0.087(6) 0.046(4) 0.079(5) -0.000(4) 0.023(5) 0.006(4) #============================================================================== _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 Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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 Ga(1) Cl(1) 2.166(4) yes . . Ga(1) Cl(2) 2.152(2) yes . . Ga(1) Cl(3) 2.150(3) yes . . S(1) C(5) 1.741(5) yes . . S(1) C(7) 1.746(5) yes . . S(2) C(6) 1.732(6) yes . . S(2) C(7) 1.727(5) yes . . S(3) C(8) 1.723(5) yes . . S(3) C(9) 1.760(6) yes . . S(4) C(8) 1.737(6) yes . . S(4) C(10) 1.738(5) yes . . S(5) C(10) 1.656(6) yes . . S(6) C(11) 1.715(6) yes . . S(6) C(12) 1.722(6) yes . . S(7) C(11) 1.711(5) yes . . S(7) C(13) 1.727(6) yes . . C(1) C(2) 1.391(9) yes . . C(1) C(3) 1.362(8) yes . . C(2) C(4) 1.382(9) yes . . C(3) C(5) 1.386(8) yes . . C(4) C(6) 1.371(7) yes . . C(5) C(6) 1.387(8) yes . . C(7) C(8) 1.346(7) yes . . C(9) C(10) 1.396(7) yes . . C(9) C(11) 1.379(7) yes . . C(12) C(13) 1.32(1) yes . . 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) Ga(1) Cl(2) 109.57(8) yes . . . Cl(1) Ga(1) Cl(3) 109.0(1) yes . . . Cl(2) Ga(1) Cl(3) 109.10(8) yes . . . C(5) S(1) C(7) 95.8(3) yes . . . C(6) S(2) C(7) 96.2(3) yes . . . C(8) S(3) C(9) 95.8(3) yes . . . C(8) S(4) C(10) 97.7(3) yes . . . C(11) S(6) C(12) 96.2(3) yes . . . C(11) S(7) C(13) 95.0(3) yes . . . C(2) C(1) C(3) 122.1(6) yes . . . C(4) C(2) C(1) 119.5(5) yes . . . C(5) C(3) C(1) 117.5(5) yes . . . C(6) C(4) C(2) 119.4(5) yes . . . C(6) C(5) S(1) 116.0(4) yes . . . C(6) C(5) C(3) 121.5(5) yes . . . S(1) C(5) C(3) 122.5(4) yes . . . S(2) C(6) C(4) 123.3(4) yes . . . S(2) C(6) C(5) 116.7(4) yes . . . C(4) C(6) C(5) 120.0(5) yes . . . C(8) C(7) S(1) 122.1(4) yes . . . C(8) C(7) S(2) 122.8(4) yes . . . S(1) C(7) S(2) 115.1(3) yes . . . S(3) C(8) S(4) 115.0(3) yes . . . S(3) C(8) C(7) 123.3(4) yes . . . S(4) C(8) C(7) 121.7(4) yes . . . C(10) C(9) C(11) 125.4(5) yes . . . C(10) C(9) S(3) 117.3(4) yes . . . C(11) C(9) S(3) 117.3(4) yes . . . S(4) C(10) S(5) 118.9(3) yes . . . S(4) C(10) C(9) 114.3(4) yes . . . S(5) C(10) C(9) 126.8(4) yes . . . S(6) C(11) S(7) 114.8(3) yes . . . S(6) C(11) C(9) 119.8(4) yes . . . S(7) C(11) C(9) 125.3(4) yes . . . C(13) C(12) H(5) 122.9(7) no . . . C(13) C(12) S(6) 115.8(5) yes . . . S(7) C(13) C(12) 118.1(5) yes . . . 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(7) S(1) C(5) C(3) -178.5(5) yes . . . . C(7) S(1) C(5) C(6) 2.8(4) yes . . . . C(5) S(1) C(7) S(2) -3.6(3) yes . . . . C(5) S(1) C(7) C(8) 177.7(4) yes . . . . C(7) S(2) C(6) C(4) 178.6(5) yes . . . . C(7) S(2) C(6) C(5) -1.3(5) yes . . . . C(6) S(2) C(7) S(1) 3.1(3) yes . . . . C(6) S(2) C(7) C(8) -178.1(4) yes . . . . C(9) S(3) C(8) S(4) -0.9(3) yes . . . . C(9) S(3) C(8) C(7) 178.8(4) yes . . . . C(8) S(3) C(9) C(10) 1.0(5) yes . . . . C(8) S(3) C(9) C(11) -179.1(4) yes . . . . C(10) S(4) C(8) S(3) 0.6(3) yes . . . . C(10) S(4) C(8) C(7) -179.1(4) yes . . . . C(8) S(4) C(10) S(5) 179.3(3) yes . . . . C(8) S(4) C(10) C(9) 0.0(4) yes . . . . C(12) S(6) C(11) S(7) 1.3(3) yes . . . . C(12) S(6) C(11) C(9) -179.6(4) yes . . . . C(11) S(6) C(12) C(13) -0.7(6) yes . . . . C(13) S(7) C(11) S(6) -1.3(3) yes . . . . C(13) S(7) C(11) C(9) 179.6(5) yes . . . . C(11) S(7) C(13) C(12) 0.8(6) yes . . . . C(3) C(1) C(2) C(4) -0.8(9) yes . . . . C(2) C(1) C(3) C(5) 1.0(9) yes . . . . C(1) C(2) C(4) C(6) 0.4(9) yes . . . . C(1) C(3) C(5) S(1) -179.4(4) yes . . . . C(1) C(3) C(5) C(6) -0.8(8) yes . . . . C(2) C(4) C(6) S(2) 180.0(5) yes . . . . C(2) C(4) C(6) C(5) -0.1(8) yes . . . . S(1) C(5) C(6) S(2) -1.1(6) yes . . . . S(1) C(5) C(6) C(4) 179.1(5) yes . . . . C(3) C(5) C(6) S(2) -179.8(5) yes . . . . C(3) C(5) C(6) C(4) 0.3(8) yes . . . . S(1) C(7) C(8) S(3) 0.6(7) yes . . . . S(1) C(7) C(8) S(4) -179.7(3) yes . . . . S(2) C(7) C(8) S(3) -178.0(4) yes . . . . S(2) C(7) C(8) S(4) 1.7(7) yes . . . . S(3) C(9) C(10) S(4) -0.7(6) yes . . . . S(3) C(9) C(10) S(5) -179.9(4) yes . . . . C(11) C(9) C(10) S(4) 179.4(5) yes . . . . C(11) C(9) C(10) S(5) 0.2(9) yes . . . . S(3) C(9) C(11) S(6) -0.5(7) yes . . . . S(3) C(9) C(11) S(7) 178.6(4) yes . . . . C(10) C(9) C(11) S(6) 179.4(5) yes . . . . C(10) C(9) C(11) S(7) -1.5(9) yes . . . . S(6) C(12) C(13) S(7) -0.0(8) yes . . . . 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) Cl(2) 3.527(4) yes . 55501 Cl(1) Cl(2) 3.527(4) yes . 55504 Cl(1) Cl(3) 3.512(5) yes . 55501 Cl(2) Cl(1) 3.527(4) yes . 55501 Cl(2) Cl(2) 3.536(2) yes . 55504 Cl(2) Cl(3) 3.504(3) yes . 55501 Cl(2) S(7) 3.348(2) yes . 65603 Cl(2) C(4) 4.039(6) yes . 55501 Cl(2) C(13) 3.682(7) yes . 65603 Cl(3) Cl(1) 3.512(5) yes . 55501 Cl(3) Cl(2) 3.504(3) yes . 55501 Cl(3) Cl(2) 3.504(3) yes . 55504 Cl(3) C(2) 3.648(6) yes . 55501 Cl(3) C(2) 3.648(6) yes . 55504 Cl(3) C(4) 3.796(5) yes . 55501 Cl(3) C(4) 3.796(5) yes . 55504 S(1) S(2) 2.930(2) yes . 55501 S(1) S(3) 3.220(2) yes . 55501 S(1) S(4) 3.664(2) yes . 55601 S(1) S(5) 3.871(2) yes . 55601 S(1) C(1) 3.983(6) yes . 55501 S(1) C(3) 2.746(6) yes . 55501 S(1) C(4) 3.951(5) yes . 55501 S(1) C(6) 2.660(5) yes . 55501 S(1) C(8) 2.713(6) yes . 55501 S(2) S(1) 2.930(2) yes . 55501 S(2) S(4) 3.196(2) yes . 55501 S(2) S(5) 3.652(2) yes . 65603 S(2) C(2) 4.003(6) yes . 55501 S(2) C(3) 3.974(6) yes . 55501 S(2) C(4) 2.735(6) yes . 55501 S(2) C(5) 2.661(6) yes . 55501 S(2) C(8) 2.704(5) yes . 55501 S(3) S(1) 3.220(2) yes . 55501 S(3) S(4) 2.917(2) yes . 55501 S(3) S(5) 3.542(2) yes . 55601 S(3) S(6) 3.042(2) yes . 55501 S(3) C(7) 2.707(5) yes . 55501 S(3) C(10) 2.701(6) yes . 55501 S(3) C(11) 2.689(5) yes . 55501 S(4) S(2) 3.196(2) yes . 55501 S(4) S(3) 2.917(2) yes . 55501 S(4) S(4) 3.769(2) yes . 65603 S(4) S(5) 2.924(2) yes . 55501 S(4) S(5) 3.618(2) yes . 65603 S(4) C(7) 2.699(6) yes . 55501 S(4) C(9) 2.639(5) yes . 55501 S(4) C(10) 4.051(5) yes . 65603 S(4) C(11) 3.975(5) yes . 55501 S(5) S(2) 3.652(2) yes . 65603 S(5) S(4) 2.924(2) yes . 55501 S(5) S(4) 3.618(2) yes . 65603 S(5) S(7) 2.976(2) yes . 55501 S(5) C(9) 2.731(6) yes . 55501 S(5) C(11) 3.192(5) yes . 55501 S(6) S(3) 3.042(2) yes . 55501 S(6) S(5) 4.149(2) yes . 55601 S(6) S(7) 2.887(2) yes . 55501 S(6) C(9) 2.682(5) yes . 55501 S(6) C(10) 4.017(5) yes . 55501 S(6) C(13) 2.588(7) yes . 55501 S(7) Cl(2) 3.348(2) yes . 65603 S(7) S(5) 2.976(2) yes . 55501 S(7) S(6) 2.887(2) yes . 55501 S(7) C(9) 2.749(5) yes . 55501 S(7) C(10) 3.187(5) yes . 55501 S(7) C(12) 2.624(7) yes . 55501 C(1) Cl(1) 4.037(6) yes . 55601 C(1) Cl(2) 3.800(7) yes . 55601 C(1) S(1) 3.983(6) yes . 55501 C(1) C(4) 2.395(9) yes . 55501 C(1) C(5) 2.350(8) yes . 55501 C(1) C(6) 2.739(8) yes . 55501 C(2) Cl(1) 3.909(6) yes . 55601 C(2) Cl(2) 4.132(7) yes . 55601 C(2) Cl(3) 3.648(6) yes . 55501 C(2) S(2) 4.003(6) yes . 55501 C(2) C(3) 2.409(8) yes . 55501 C(2) C(5) 2.742(7) yes . 55501 C(2) C(6) 2.376(8) yes . 55501 C(3) S(1) 2.746(6) yes . 55501 C(3) S(2) 3.974(6) yes . 55501 C(3) S(2) 3.922(6) yes . 55601 C(3) S(4) 4.091(6) yes . 55601 C(3) C(2) 2.409(8) yes . 55501 C(3) C(4) 2.796(8) yes . 55501 C(3) C(6) 2.419(8) yes . 55501 C(3) C(7) 3.941(8) yes . 55501 C(4) Cl(2) 4.039(6) yes . 55501 C(4) Cl(3) 3.796(5) yes . 55501 C(4) S(1) 3.951(5) yes . 55501 C(4) S(2) 2.735(6) yes . 55501 C(4) C(1) 2.395(9) yes . 55501 C(4) C(3) 2.796(8) yes . 55501 C(4) C(5) 2.388(7) yes . 55501 C(4) C(7) 3.915(7) yes . 55501 C(5) S(2) 2.661(6) yes . 55501 C(5) C(1) 2.350(8) yes . 55501 C(5) C(2) 2.742(7) yes . 55501 C(5) C(4) 2.388(7) yes . 55501 C(5) C(7) 2.588(8) yes . 55501 C(5) C(8) 3.899(8) yes . 55501 C(6) S(1) 2.660(5) yes . 55501 C(6) C(1) 2.739(8) yes . 55501 C(6) C(2) 2.376(8) yes . 55501 C(6) C(3) 2.419(8) yes . 55501 C(6) C(7) 2.575(7) yes . 55501 C(6) C(8) 3.890(7) yes . 55501 C(7) S(3) 2.707(5) yes . 55501 C(7) S(4) 2.699(6) yes . 55501 C(7) C(3) 3.941(8) yes . 55501 C(7) C(4) 3.915(7) yes . 55501 C(7) C(5) 2.588(8) yes . 55501 C(7) C(6) 2.575(7) yes . 55501 C(7) C(9) 3.903(7) yes . 55501 C(7) C(10) 3.922(7) yes . 55501 C(8) S(1) 2.713(6) yes . 55501 C(8) S(2) 2.704(5) yes . 55501 C(8) C(5) 3.899(8) yes . 55501 C(8) C(6) 3.890(7) yes . 55501 C(8) C(9) 2.583(7) yes . 55501 C(8) C(10) 2.616(7) yes . 55501 C(8) C(11) 3.902(7) yes . 55501 C(9) S(4) 2.639(5) yes . 55501 C(9) S(5) 2.731(6) yes . 55501 C(9) S(6) 2.682(5) yes . 55501 C(9) S(7) 2.749(5) yes . 55501 C(9) C(7) 3.903(7) yes . 55501 C(9) C(8) 2.583(7) yes . 55501 C(9) C(12) 3.892(7) yes . 55501 C(9) C(13) 3.895(7) yes . 55501 C(10) S(3) 2.701(6) yes . 55501 C(10) S(4) 4.051(5) yes . 65603 C(10) S(6) 4.017(5) yes . 55501 C(10) S(7) 3.187(5) yes . 55501 C(10) C(7) 3.922(7) yes . 55501 C(10) C(8) 2.616(7) yes . 55501 C(10) C(11) 2.466(7) yes . 55501 C(11) S(3) 2.689(5) yes . 55501 C(11) S(4) 3.975(5) yes . 55501 C(11) S(5) 3.192(5) yes . 55501 C(11) C(8) 3.902(7) yes . 55501 C(11) C(10) 2.466(7) yes . 55501 C(11) C(12) 2.557(8) yes . 55501 C(11) C(13) 2.535(7) yes . 55501 C(12) S(7) 2.624(7) yes . 55501 C(12) C(9) 3.892(7) yes . 55501 C(12) C(11) 2.557(8) yes . 55501 C(13) Cl(2) 3.682(7) yes . 65603 C(13) S(6) 2.588(7) yes . 55501 C(13) C(9) 3.895(7) yes . 55501 C(13) C(11) 2.535(7) yes . 55501 #============================================================================== # 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 #============================================================================== #===END #============================================================================== data_FeBr4salt _database_code_depnum_ccdc_archive 'CCDC 271656' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C13 H6 Br2 Fe0.50 S7 ' _chemical_formula_moiety 'C13 H6 Br2 Fe0.50 S7 ' _chemical_formula_weight 574.34 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z x,-y+1/2,z #------------------------------------------------------------------------------ _cell_length_a 7.063(3) _cell_length_b 35.514(12) _cell_length_c 7.661(3) _cell_angle_alpha 90.0000(11) _cell_angle_beta 105.673(1) _cell_angle_gamma 90.0000(11) _cell_volume 1850.3(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4118 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116.00 _exptl_absorpt_coefficient_mu 5.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.946 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 33074 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9776 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9776 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement 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 4242 _reflns_number_gt 2247 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.0420 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2247 _refine_ls_number_parameters 214 _refine_ls_goodness_of_fit_ref 2.293 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.48 _refine_diff_density_min -1.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; Br Br -0.290 2.459 ; 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) ; S S 0.125 0.123 ; 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 0.9285(2) 0.2500 0.6421(2) 0.0786(5) Uani 1.00 1 d . . . Br(2) Br 0.7904(3) 0.2500 1.0874(2) 0.0985(6) Uani 1.00 1 d . . . Br(3) Br 0.4781(2) 0.19605(3) 0.6870(1) 0.0858(4) Uani 1.00 1 d . . . Fe(1) Fe 0.6673(3) 0.2500 0.7737(2) 0.0545(6) Uani 1.00 1 d . . . S(1) S 0.7923(3) 0.03072(5) 1.2877(3) 0.0383(6) Uani 1.00 1 d . . . S(2) S 0.7122(3) 0.07526(6) 0.9517(2) 0.0397(6) Uani 1.00 1 d . . . S(3) S 0.7770(3) -0.04527(5) 1.0532(2) 0.0373(6) Uani 1.00 1 d . . . S(4) S 0.7069(3) -0.00050(5) 0.7211(2) 0.0406(6) Uani 1.00 1 d . . . S(5) S 0.6818(3) -0.06564(6) 0.4802(2) 0.0460(6) Uani 1.00 1 d . . . S(6) S 0.8012(3) -0.13133(6) 1.0652(3) 0.0551(7) Uani 1.00 1 d . . . S(7) S 0.7294(3) -0.13909(6) 0.6763(3) 0.0462(6) Uani 1.00 1 d . . . C(1) C 0.8101(11) 0.1358(2) 1.4829(11) 0.050(3) Uani 1.00 1 d . . . C(2) C 0.7724(10) 0.1572(2) 1.3255(11) 0.049(3) Uani 1.00 1 d . . . C(3) C 0.8196(10) 0.0972(2) 1.4787(10) 0.042(3) Uani 1.00 1 d . . . C(4) C 0.7413(10) 0.1394(2) 1.1596(10) 0.042(2) Uani 1.00 1 d . . . C(5) C 0.7882(9) 0.0793(2) 1.3108(9) 0.030(2) Uani 1.00 1 d . . . C(6) C 0.7486(9) 0.1008(2) 1.1523(9) 0.031(2) Uani 1.00 1 d . . . C(7) C 0.7520(9) 0.0309(2) 1.0539(9) 0.033(2) Uani 1.00 1 d . . . C(8) C 0.7472(9) -0.0011(2) 0.9552(9) 0.033(2) Uani 1.00 1 d . . . C(9) C 0.7486(9) -0.0703(2) 0.8492(9) 0.029(2) Uani 1.00 1 d . . . C(10) C 0.7143(9) -0.0493(2) 0.6893(9) 0.033(2) Uani 1.00 1 d . . . C(11) C 0.7585(9) -0.1095(2) 0.8580(9) 0.033(2) Uani 1.00 1 d . . . C(12) C 0.7949(12) -0.1766(2) 0.9816(12) 0.065(3) Uani 1.00 1 d . . . C(13) C 0.7663(12) -0.1793(2) 0.8076(12) 0.064(3) Uani 1.00 1 d . . . H(1) H 0.8296 0.1482 1.5963 0.063 Uiso 1.00 1 c . . . H(2) H 0.7686 0.1839 1.3327 0.058 Uiso 1.00 1 c . . . H(3) H 0.8468 0.0827 1.5871 0.051 Uiso 1.00 1 c . . . H(4) H 0.7145 0.1536 1.0505 0.051 Uiso 1.00 1 c . . . H(5) H 0.8112 -0.1980 1.0590 0.078 Uiso 1.00 1 c . . . H(6) H 0.7654 -0.2032 0.7517 0.077 Uiso 1.00 1 c . . . 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) 0.0733(10) 0.0854(12) 0.0811(10) 0.0000 0.0275(8) 0.0000 Br(2) 0.177(2) 0.0599(10) 0.0472(8) 0.0000 0.0103(10) 0.0000 Br(3) 0.1051(8) 0.0794(8) 0.0798(7) -0.0333(7) 0.0369(6) -0.0280(6) Fe(1) 0.0723(12) 0.0454(11) 0.0440(10) 0.0000 0.0124(9) 0.0000 S(1) 0.0434(12) 0.0368(12) 0.0389(11) -0.0018(10) 0.0183(10) 0.0023(9) S(2) 0.0420(11) 0.0428(12) 0.0355(11) -0.0015(10) 0.0123(9) -0.0002(10) S(3) 0.0392(11) 0.0411(12) 0.0338(11) -0.0029(10) 0.0137(9) -0.0001(10) S(4) 0.0467(12) 0.0384(12) 0.0369(11) 0.0010(11) 0.0118(10) 0.0012(10) S(5) 0.0541(13) 0.048(1) 0.0334(11) 0.0022(11) 0.0082(10) -0.0015(10) S(6) 0.066(2) 0.049(1) 0.0490(13) 0.0033(12) 0.0129(12) 0.0130(11) S(7) 0.0477(12) 0.0382(13) 0.0516(13) 0.0014(11) 0.0116(11) -0.0038(10) C(1) 0.048(5) 0.055(6) 0.055(6) -0.003(5) 0.025(5) -0.021(5) C(2) 0.045(5) 0.040(5) 0.062(6) 0.009(4) 0.014(5) -0.001(5) C(3) 0.043(5) 0.045(5) 0.040(5) 0.005(4) 0.016(4) 0.002(4) C(4) 0.047(5) 0.038(5) 0.042(5) 0.002(4) 0.014(4) 0.001(4) C(5) 0.024(4) 0.031(4) 0.037(4) -0.002(3) 0.011(4) -0.003(4) C(6) 0.019(4) 0.042(5) 0.033(4) -0.002(4) 0.010(3) -0.005(4) C(7) 0.021(4) 0.046(5) 0.038(4) -0.006(4) 0.018(4) 0.002(4) C(8) 0.021(4) 0.043(5) 0.038(4) -0.005(4) 0.015(3) -0.005(4) C(9) 0.017(4) 0.036(5) 0.037(4) -0.000(3) 0.011(3) -0.001(4) C(10) 0.022(4) 0.040(5) 0.035(4) 0.003(4) 0.006(3) 0.004(4) C(11) 0.019(4) 0.044(5) 0.038(4) -0.002(4) 0.010(3) 0.002(4) C(12) 0.080(7) 0.044(6) 0.070(6) 0.001(5) 0.020(6) 0.021(5) C(13) 0.074(6) 0.036(6) 0.082(7) 0.006(5) 0.022(6) 0.001(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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) 2.329(2) yes . . Br(2) Fe(1) 2.325(2) yes . . Br(3) Fe(1) 2.328(1) yes . . S(1) C(5) 1.737(7) yes . . S(1) C(7) 1.736(7) yes . . S(2) C(6) 1.742(7) yes . . S(2) C(7) 1.748(7) yes . . S(3) C(8) 1.726(7) yes . . S(3) C(9) 1.762(7) yes . . S(4) C(8) 1.739(7) yes . . S(4) C(10) 1.751(7) yes . . S(5) C(10) 1.661(7) yes . . S(6) C(11) 1.719(7) yes . . S(6) C(12) 1.728(9) yes . . S(7) C(11) 1.713(7) yes . . S(7) C(13) 1.725(9) yes . . C(1) C(2) 1.39(1) yes . . C(1) C(3) 1.37(1) yes . . C(2) C(4) 1.38(1) yes . . C(3) C(5) 1.40(1) yes . . C(4) C(6) 1.37(1) yes . . C(5) C(6) 1.40(1) yes . . C(7) C(8) 1.36(1) yes . . C(9) C(10) 1.40(1) yes . . C(9) C(11) 1.39(1) yes . . C(12) C(13) 1.30(1) yes . . 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) 109.19(9) yes . . . Br(1) Fe(1) Br(3) 109.72(6) yes . . . Br(2) Fe(1) Br(3) 108.70(6) yes . . . C(5) S(1) C(7) 95.7(3) yes . . . C(6) S(2) C(7) 96.1(3) yes . . . C(8) S(3) C(9) 95.8(3) yes . . . C(8) S(4) C(10) 97.4(3) yes . . . C(11) S(6) C(12) 95.6(4) yes . . . C(11) S(7) C(13) 93.9(4) yes . . . C(2) C(1) C(3) 121.7(7) yes . . . C(4) C(2) C(1) 119.6(7) yes . . . C(5) C(3) C(1) 118.5(7) yes . . . C(6) C(4) C(2) 119.7(7) yes . . . C(6) C(5) S(1) 117.3(5) yes . . . C(6) C(5) C(3) 119.9(6) yes . . . S(1) C(5) C(3) 122.8(5) yes . . . S(2) C(6) C(4) 123.8(6) yes . . . S(2) C(6) C(5) 115.5(5) yes . . . C(4) C(6) C(5) 120.6(6) yes . . . C(8) C(7) S(1) 122.8(5) yes . . . C(8) C(7) S(2) 121.8(5) yes . . . S(1) C(7) S(2) 115.3(4) yes . . . S(3) C(8) S(4) 115.3(4) yes . . . S(3) C(8) C(7) 122.4(5) yes . . . S(4) C(8) C(7) 122.3(6) yes . . . C(10) C(9) C(11) 124.7(6) yes . . . C(10) C(9) S(3) 117.4(5) yes . . . C(11) C(9) S(3) 117.9(5) yes . . . S(4) C(10) S(5) 118.6(4) yes . . . S(4) C(10) C(9) 114.2(5) yes . . . S(5) C(10) C(9) 127.2(6) yes . . . S(6) C(11) S(7) 115.2(4) yes . . . S(6) C(11) C(9) 119.3(5) yes . . . S(7) C(11) C(9) 125.5(5) yes . . . C(13) C(12) S(6) 115.4(7) yes . . . S(7) C(13) C(12) 119.8(7) yes . . . 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(7) S(1) C(5) C(3) -178.2(6) yes . . . . C(7) S(1) C(5) C(6) 2.8(5) yes . . . . C(5) S(1) C(7) S(2) -3.8(4) yes . . . . C(5) S(1) C(7) C(8) 177.6(5) yes . . . . C(7) S(2) C(6) C(4) 178.1(6) yes . . . . C(7) S(2) C(6) C(5) -1.4(5) yes . . . . C(6) S(2) C(7) S(1) 3.4(4) yes . . . . C(6) S(2) C(7) C(8) -178.0(5) yes . . . . C(9) S(3) C(8) S(4) -0.2(4) yes . . . . C(9) S(3) C(8) C(7) 178.9(5) yes . . . . C(8) S(3) C(9) C(10) -0.1(5) yes . . . . C(8) S(3) C(9) C(11) -179.1(5) yes . . . . C(10) S(4) C(8) S(3) 0.3(4) yes . . . . C(10) S(4) C(8) C(7) -178.7(5) yes . . . . C(8) S(4) C(10) S(5) 179.7(4) yes . . . . C(8) S(4) C(10) C(9) -0.4(5) yes . . . . C(12) S(6) C(11) S(7) 0.4(4) yes . . . . C(12) S(6) C(11) C(9) 179.9(6) yes . . . . C(11) S(6) C(12) C(13) 1.0(7) yes . . . . C(13) S(7) C(11) S(6) -1.2(4) yes . . . . C(13) S(7) C(11) C(9) 179.3(6) yes . . . . C(11) S(7) C(13) C(12) 2.1(8) yes . . . . C(3) C(1) C(2) C(4) 0(1) yes . . . . C(2) C(1) C(3) C(5) 0(1) yes . . . . C(1) C(2) C(4) C(6) 0(1) yes . . . . C(1) C(3) C(5) S(1) -178.9(5) yes . . . . C(1) C(3) C(5) C(6) 0(1) yes . . . . C(2) C(4) C(6) S(2) -179.9(6) yes . . . . C(2) C(4) C(6) C(5) 0(1) yes . . . . S(1) C(5) C(6) S(2) -1.0(7) yes . . . . S(1) C(5) C(6) C(4) 179.5(6) yes . . . . C(3) C(5) C(6) S(2) 180.0(5) yes . . . . C(3) C(5) C(6) C(4) 0(1) yes . . . . S(1) C(7) C(8) S(3) 1.1(9) yes . . . . S(1) C(7) C(8) S(4) -179.9(4) yes . . . . S(2) C(7) C(8) S(3) -177.5(4) yes . . . . S(2) C(7) C(8) S(4) 1.5(9) yes . . . . S(3) C(9) C(10) S(4) 0.4(7) yes . . . . S(3) C(9) C(10) S(5) -179.8(4) yes . . . . C(11) C(9) C(10) S(4) 179.2(5) yes . . . . C(11) C(9) C(10) S(5) 0(1) yes . . . . S(3) C(9) C(11) S(6) -1.0(8) yes . . . . S(3) C(9) C(11) S(7) 178.4(4) yes . . . . C(10) C(9) C(11) S(6) -179.8(5) yes . . . . C(10) C(9) C(11) S(7) 0(1) yes . . . . S(6) C(12) C(13) S(7) -2(1) yes . . . . S(6) C(12) C(13) H(6) 177(1) no . . . . 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(1) Br(2) 3.793(2) yes . 55501 Br(1) Br(3) 3.808(2) yes . 55501 Br(1) Br(3) 3.808(2) yes . 55504 Br(1) Fe(1) 2.329(2) yes . 55501 Br(2) Br(1) 3.793(2) yes . 55501 Br(2) Br(3) 3.781(1) yes . 55501 Br(2) Br(3) 3.781(1) yes . 55504 Br(2) Fe(1) 2.325(2) yes . 55501 Br(2) C(2) 3.786(8) yes . 55501 Br(2) C(2) 3.786(8) yes . 55504 Br(2) C(4) 3.996(7) yes . 55501 Br(2) C(4) 3.996(7) yes . 55504 Br(3) Br(1) 3.808(2) yes . 55501 Br(3) Br(2) 3.781(1) yes . 55501 Br(3) Br(3) 3.832(2) yes . 55504 Br(3) Fe(1) 2.328(1) yes . 55501 Br(3) S(7) 3.432(2) yes . 65603 Br(3) C(13) 3.763(9) yes . 65603 Fe(1) Br(1) 2.329(2) yes . 55501 Fe(1) Br(2) 2.325(2) yes . 55501 Fe(1) Br(3) 2.328(1) yes . 55501 Fe(1) Br(3) 2.328(1) yes . 55504 S(1) S(2) 2.943(3) yes . 55501 S(1) S(3) 3.227(3) yes . 55501 S(1) S(4) 3.701(3) yes . 55601 S(1) S(5) 3.888(3) yes . 55601 S(1) C(3) 2.755(8) yes . 55501 S(1) C(4) 3.974(8) yes . 55501 S(1) C(6) 2.681(8) yes . 55501 S(1) C(8) 2.726(7) yes . 55501 S(2) S(1) 2.943(3) yes . 55501 S(2) S(4) 3.213(3) yes . 55501 S(2) S(5) 3.719(2) yes . 65603 S(2) C(3) 3.978(7) yes . 55501 S(2) C(4) 2.754(8) yes . 55501 S(2) C(5) 2.661(7) yes . 55501 S(2) C(8) 2.724(8) yes . 55501 S(3) S(1) 3.227(3) yes . 55501 S(3) S(4) 2.927(3) yes . 55501 S(3) S(5) 3.586(3) yes . 55601 S(3) S(6) 3.061(3) yes . 55501 S(3) C(7) 2.711(7) yes . 55501 S(3) C(10) 2.706(7) yes . 55501 S(3) C(11) 2.710(7) yes . 55501 S(4) S(2) 3.213(3) yes . 55501 S(4) S(3) 2.927(3) yes . 55501 S(4) S(4) 3.830(2) yes . 65603 S(4) S(5) 2.935(3) yes . 55501 S(4) S(5) 3.626(3) yes . 65603 S(4) C(7) 2.722(7) yes . 55501 S(4) C(9) 2.652(7) yes . 55501 S(5) S(2) 3.719(2) yes . 65603 S(5) S(4) 2.935(3) yes . 55501 S(5) S(4) 3.626(3) yes . 65603 S(5) S(7) 2.984(3) yes . 55501 S(5) C(9) 2.742(7) yes . 55501 S(5) C(11) 3.201(7) yes . 55501 S(6) S(3) 3.061(3) yes . 55501 S(6) S(7) 2.897(3) yes . 55501 S(6) C(9) 2.692(7) yes . 55501 S(6) C(13) 2.567(9) yes . 55501 S(7) Br(3) 3.432(2) yes . 65603 S(7) S(5) 2.984(3) yes . 55501 S(7) S(6) 2.897(3) yes . 55501 S(7) C(9) 2.766(7) yes . 55501 S(7) C(10) 3.195(7) yes . 55501 S(7) C(12) 2.623(9) yes . 55501 C(1) Br(3) 3.809(9) yes . 55601 C(1) C(4) 2.40(1) yes . 55501 C(1) C(5) 2.38(1) yes . 55501 C(1) C(6) 2.75(1) yes . 55501 C(2) Br(2) 3.786(8) yes . 55501 C(2) C(3) 2.41(1) yes . 55501 C(2) C(5) 2.77(1) yes . 55501 C(2) C(6) 2.38(1) yes . 55501 C(3) S(1) 2.755(8) yes . 55501 C(3) S(2) 3.978(7) yes . 55501 C(3) S(2) 3.974(8) yes . 55601 C(3) C(2) 2.41(1) yes . 55501 C(3) C(4) 2.79(1) yes . 55501 C(3) C(6) 2.42(1) yes . 55501 C(3) C(7) 3.94(1) yes . 55501 C(4) Br(2) 3.996(7) yes . 55501 C(4) S(1) 3.974(8) yes . 55501 C(4) S(2) 2.754(8) yes . 55501 C(4) C(1) 2.40(1) yes . 55501 C(4) C(3) 2.79(1) yes . 55501 C(4) C(5) 2.41(1) yes . 55501 C(4) C(7) 3.94(1) yes . 55501 C(5) S(2) 2.661(7) yes . 55501 C(5) C(1) 2.38(1) yes . 55501 C(5) C(2) 2.77(1) yes . 55501 C(5) C(4) 2.41(1) yes . 55501 C(5) C(7) 2.57(1) yes . 55501 C(5) C(8) 3.90(1) yes . 55501 C(6) S(1) 2.681(8) yes . 55501 C(6) C(1) 2.75(1) yes . 55501 C(6) C(2) 2.38(1) yes . 55501 C(6) C(3) 2.42(1) yes . 55501 C(6) C(7) 2.59(1) yes . 55501 C(6) C(8) 3.92(1) yes . 55501 C(7) S(3) 2.711(7) yes . 55501 C(7) S(4) 2.722(7) yes . 55501 C(7) C(3) 3.94(1) yes . 55501 C(7) C(4) 3.94(1) yes . 55501 C(7) C(5) 2.57(1) yes . 55501 C(7) C(6) 2.59(1) yes . 55501 C(7) C(9) 3.92(1) yes . 55501 C(7) C(10) 3.95(1) yes . 55501 C(8) S(1) 2.726(7) yes . 55501 C(8) S(2) 2.724(8) yes . 55501 C(8) C(5) 3.90(1) yes . 55501 C(8) C(6) 3.92(1) yes . 55501 C(8) C(9) 2.59(1) yes . 55501 C(8) C(10) 2.62(1) yes . 55501 C(8) C(11) 3.92(1) yes . 55501 C(9) S(4) 2.652(7) yes . 55501 C(9) S(5) 2.742(7) yes . 55501 C(9) S(6) 2.692(7) yes . 55501 C(9) S(7) 2.766(7) yes . 55501 C(9) C(7) 3.92(1) yes . 55501 C(9) C(8) 2.59(1) yes . 55501 C(9) C(12) 3.90(1) yes . 55501 C(9) C(13) 3.89(1) yes . 55501 C(10) S(3) 2.706(7) yes . 55501 C(10) S(7) 3.195(7) yes . 55501 C(10) C(7) 3.95(1) yes . 55501 C(10) C(8) 2.62(1) yes . 55501 C(10) C(11) 2.47(1) yes . 55501 C(11) S(3) 2.710(7) yes . 55501 C(11) S(5) 3.201(7) yes . 55501 C(11) C(8) 3.92(1) yes . 55501 C(11) C(10) 2.47(1) yes . 55501 C(11) C(12) 2.55(1) yes . 55501 C(11) C(13) 2.51(1) yes . 55501 C(12) S(7) 2.623(9) yes . 55501 C(12) C(9) 3.90(1) yes . 55501 C(12) C(11) 2.55(1) yes . 55501 C(13) Br(3) 3.763(9) yes . 65603 C(13) S(6) 2.567(9) yes . 55501 C(13) C(9) 3.89(1) yes . 55501 C(13) C(11) 2.51(1) yes . 55501 #============================================================================== # 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 #============================================================================== #===END #============================================================================== data_GaBr4salt _database_code_depnum_ccdc_archive 'CCDC 271657' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C13 H6 Br2 Ga0.50 S7 ' _chemical_formula_moiety 'C13 H6 Br2 Ga0.50 S7 ' _chemical_formula_weight 581.28 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z x,-y+1/2,z #------------------------------------------------------------------------------ _cell_length_a 7.073(2) _cell_length_b 35.602(7) _cell_length_c 7.661(2) _cell_angle_alpha 90.0000(8) _cell_angle_beta 106.0624(10) _cell_angle_gamma 90.0000(8) _cell_volume 1853.8(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4602 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126.00 _exptl_absorpt_coefficient_mu 5.877 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 8596 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9874 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9874 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement 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 4298 _reflns_number_gt 2297 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0350 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2297 _refine_ls_number_parameters 214 _refine_ls_goodness_of_fit_ref 2.063 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/\s^2^(Fo)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.52 _refine_diff_density_min -1.34 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ga Ga 0.231 1.608 ; 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) ; #============================================================================== # 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 0.4774(1) 0.30358(3) 0.68633(12) 0.0842(3) Uani 1.00 1 d . . . Br(2) Br 0.9257(2) 0.2500 0.6462(2) 0.0778(5) Uani 1.00 1 d . . . Br(3) Br 0.7855(2) 0.2500 1.0886(2) 0.0922(5) Uani 1.00 1 d . . . Ga(1) Ga 0.6656(2) 0.2500 0.7759(1) 0.0531(4) Uani 1.00 1 d . . . S(1) S 0.7910(2) 0.03058(5) 1.2862(2) 0.0382(5) Uani 1.00 1 d . . . S(2) S 0.7117(2) 0.07508(5) 0.9501(2) 0.0402(5) Uani 1.00 1 d . . . S(3) S 0.7772(2) -0.04517(5) 1.0522(2) 0.0375(5) Uani 1.00 1 d . . . S(4) S 0.7076(2) -0.00058(5) 0.7195(2) 0.0403(5) Uani 1.00 1 d . . . S(5) S 0.6838(3) -0.06559(5) 0.4791(2) 0.0459(6) Uani 1.00 1 d . . . S(6) S 0.8029(3) -0.13093(5) 1.0656(2) 0.0552(6) Uani 1.00 1 d . . . S(7) S 0.7315(3) -0.13890(5) 0.6769(2) 0.0464(6) Uani 1.00 1 d . . . C(1) C 0.8060(9) 0.1351(2) 1.4818(9) 0.049(2) Uani 1.00 1 d . . . C(2) C 0.7676(9) 0.1567(2) 1.3234(10) 0.051(2) Uani 1.00 1 d . . . C(3) C 0.8167(9) 0.0971(2) 1.4779(8) 0.042(2) Uani 1.00 1 d . . . C(4) C 0.7390(9) 0.1392(2) 1.1572(9) 0.041(2) Uani 1.00 1 d . . . C(5) C 0.7854(8) 0.0791(2) 1.3089(8) 0.032(2) Uani 1.00 1 d . . . C(6) C 0.7473(8) 0.1005(2) 1.1514(8) 0.032(2) Uani 1.00 1 d . . . C(7) C 0.7503(8) 0.0310(2) 1.0515(8) 0.032(2) Uani 1.00 1 d . . . C(8) C 0.7466(8) -0.0008(2) 0.9536(7) 0.032(2) Uani 1.00 1 d . . . C(9) C 0.7492(8) -0.0701(2) 0.8472(8) 0.031(2) Uani 1.00 1 d . . . C(10) C 0.7172(8) -0.0492(2) 0.6887(8) 0.033(2) Uani 1.00 1 d . . . C(11) C 0.7600(8) -0.1091(2) 0.8579(8) 0.035(2) Uani 1.00 1 d . . . C(12) C 0.7989(11) -0.1759(2) 0.9836(11) 0.064(3) Uani 1.00 1 d . . . C(13) C 0.7685(11) -0.1791(2) 0.8075(11) 0.063(3) Uani 1.00 1 d . . . H(1) H 0.8258 0.1473 1.5958 0.059 Uiso 1.00 1 c . . . H(2) H 0.7609 0.1833 1.3305 0.061 Uiso 1.00 1 c . . . H(3) H 0.8441 0.0827 1.5864 0.051 Uiso 1.00 1 c . . . H(4) H 0.7140 0.1533 1.0480 0.048 Uiso 1.00 1 c . . . H(5) H 0.8165 -0.1971 1.0622 0.077 Uiso 1.00 1 c . . . H(6) H 0.7682 -0.2030 0.7524 0.076 Uiso 1.00 1 c . . . 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) 0.1040(7) 0.0766(7) 0.0766(7) 0.0328(6) 0.0327(5) 0.0275(5) Br(2) 0.0735(8) 0.0851(10) 0.0783(9) 0.0000 0.0269(7) 0.0000 Br(3) 0.164(1) 0.0581(9) 0.0438(8) 0.0000 0.0104(8) 0.0000 Ga(1) 0.0712(8) 0.0429(7) 0.0432(7) 0.0000 0.0125(6) 0.0000 S(1) 0.0447(10) 0.0360(10) 0.0367(10) -0.0028(9) 0.0159(8) 0.0009(8) S(2) 0.0461(10) 0.0409(11) 0.0318(10) -0.0013(9) 0.0080(8) -0.0005(8) S(3) 0.0420(10) 0.0400(10) 0.0313(10) -0.0031(9) 0.0112(8) -0.0009(8) S(4) 0.0500(10) 0.0366(10) 0.0323(10) 0.0010(9) 0.0082(8) 0.0007(8) S(5) 0.0575(11) 0.0466(12) 0.0297(10) 0.0020(10) 0.0058(8) -0.0025(8) S(6) 0.0689(13) 0.0479(13) 0.0452(12) 0.0024(11) 0.0099(10) 0.0128(9) S(7) 0.0507(11) 0.0366(11) 0.0484(12) 0.0022(9) 0.0082(9) -0.0042(9) C(1) 0.049(4) 0.054(5) 0.044(5) 0.002(4) 0.013(4) -0.015(4) C(2) 0.050(4) 0.041(5) 0.061(5) 0.007(4) 0.015(4) -0.008(4) C(3) 0.048(4) 0.046(5) 0.034(4) 0.007(4) 0.012(3) 0.002(3) C(4) 0.047(4) 0.036(4) 0.037(5) 0.001(4) 0.007(3) 0.004(3) C(5) 0.031(3) 0.032(4) 0.034(4) -0.000(3) 0.010(3) 0.001(3) C(6) 0.025(3) 0.036(4) 0.033(4) -0.002(3) 0.006(3) -0.003(3) C(7) 0.025(3) 0.038(4) 0.036(4) -0.006(3) 0.011(3) -0.003(3) C(8) 0.027(3) 0.038(4) 0.032(4) 0.001(3) 0.009(3) -0.000(3) C(9) 0.024(3) 0.034(4) 0.034(4) -0.002(3) 0.006(3) -0.001(3) C(10) 0.025(3) 0.038(4) 0.034(4) 0.000(3) 0.004(3) 0.002(3) C(11) 0.021(3) 0.046(5) 0.035(4) -0.002(3) 0.002(3) 0.004(3) C(12) 0.072(5) 0.043(5) 0.078(6) 0.012(4) 0.022(5) 0.023(4) C(13) 0.072(5) 0.039(5) 0.079(6) 0.008(4) 0.023(5) -0.000(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure Ver. 3.5.1' _computing_molecular_graphics ? #============================================================================== # 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) Ga(1) 2.318(1) yes . . Br(2) Ga(1) 2.320(2) yes . . Br(3) Ga(1) 2.310(1) yes . . S(1) C(5) 1.738(6) yes . . S(1) C(7) 1.741(6) yes . . S(2) C(6) 1.746(6) yes . . S(2) C(7) 1.739(6) yes . . S(3) C(8) 1.737(6) yes . . S(3) C(9) 1.767(6) yes . . S(4) C(8) 1.737(6) yes . . S(4) C(10) 1.749(6) yes . . S(5) C(10) 1.663(6) yes . . S(6) C(11) 1.720(6) yes . . S(6) C(12) 1.718(8) yes . . S(7) C(11) 1.712(6) yes . . S(7) C(13) 1.724(8) yes . . C(1) C(2) 1.40(1) yes . . C(1) C(3) 1.36(1) yes . . C(2) C(4) 1.38(1) yes . . C(3) C(5) 1.406(9) yes . . C(4) C(6) 1.377(9) yes . . C(5) C(6) 1.390(9) yes . . C(7) C(8) 1.356(8) yes . . C(9) C(10) 1.389(8) yes . . C(9) C(11) 1.392(9) yes . . C(12) C(13) 1.31(1) yes . . 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) Ga(1) Br(2) 109.35(5) yes . . . Br(1) Ga(1) Br(3) 108.85(5) yes . . . Br(2) Ga(1) Br(3) 109.69(7) yes . . . C(5) S(1) C(7) 95.3(3) yes . . . C(6) S(2) C(7) 96.2(3) yes . . . C(8) S(3) C(9) 95.8(3) yes . . . C(8) S(4) C(10) 97.6(3) yes . . . C(11) S(6) C(12) 95.9(4) yes . . . C(11) S(7) C(13) 94.5(3) yes . . . C(2) C(1) C(3) 121.8(7) yes . . . C(4) C(2) C(1) 119.7(6) yes . . . C(5) C(3) C(1) 118.7(6) yes . . . C(6) C(4) C(2) 119.0(6) yes . . . C(6) C(5) S(1) 117.6(5) yes . . . C(6) C(5) C(3) 119.5(6) yes . . . S(1) C(5) C(3) 122.9(5) yes . . . S(2) C(6) C(4) 123.4(5) yes . . . S(2) C(6) C(5) 115.3(5) yes . . . C(4) C(6) C(5) 121.3(6) yes . . . C(8) C(7) S(1) 122.4(5) yes . . . C(8) C(7) S(2) 122.1(4) yes . . . S(1) C(7) S(2) 115.5(3) yes . . . S(3) C(8) S(4) 114.8(3) yes . . . S(3) C(8) C(7) 122.6(5) yes . . . S(4) C(8) C(7) 122.7(5) yes . . . C(10) C(9) C(11) 125.5(6) yes . . . C(10) C(9) S(3) 117.2(5) yes . . . C(11) C(9) S(3) 117.3(4) yes . . . S(4) C(10) S(5) 118.5(3) yes . . . S(4) C(10) C(9) 114.6(5) yes . . . S(5) C(10) C(9) 126.9(5) yes . . . S(6) C(11) S(7) 114.9(4) yes . . . S(6) C(11) C(9) 119.8(5) yes . . . S(7) C(11) C(9) 125.3(5) yes . . . C(13) C(12) S(6) 116.0(6) yes . . . S(7) C(13) C(12) 118.8(6) yes . . . 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(7) S(1) C(5) C(3) -178.1(5) yes . . . . C(7) S(1) C(5) C(6) 2.1(5) yes . . . . C(5) S(1) C(7) S(2) -3.2(3) yes . . . . C(5) S(1) C(7) C(8) 177.5(5) yes . . . . C(7) S(2) C(6) C(4) 178.5(5) yes . . . . C(7) S(2) C(6) C(5) -1.6(5) yes . . . . C(6) S(2) C(7) S(1) 3.0(3) yes . . . . C(6) S(2) C(7) C(8) -177.7(5) yes . . . . C(9) S(3) C(8) S(4) -0.4(3) yes . . . . C(9) S(3) C(8) C(7) 178.7(5) yes . . . . C(8) S(3) C(9) C(10) 0.6(5) yes . . . . C(8) S(3) C(9) C(11) -179.0(4) yes . . . . C(10) S(4) C(8) S(3) 0.2(3) yes . . . . C(10) S(4) C(8) C(7) -178.9(5) yes . . . . C(8) S(4) C(10) S(5) 179.0(3) yes . . . . C(8) S(4) C(10) C(9) 0.2(5) yes . . . . C(12) S(6) C(11) S(7) 0.7(3) yes . . . . C(12) S(6) C(11) C(9) -179.8(5) yes . . . . C(11) S(6) C(12) C(13) 0.2(6) yes . . . . C(13) S(7) C(11) S(6) -1.2(3) yes . . . . C(13) S(7) C(11) C(9) 179.4(5) yes . . . . C(11) S(7) C(13) C(12) 1.5(7) yes . . . . C(3) C(1) C(2) C(4) 0(1) yes . . . . C(2) C(1) C(3) C(5) 0(1) yes . . . . C(1) C(2) C(4) C(6) 0(1) yes . . . . C(1) C(3) C(5) S(1) -178.8(5) yes . . . . C(1) C(3) C(5) C(6) 0.9(9) yes . . . . C(2) C(4) C(6) S(2) 179.4(5) yes . . . . C(2) C(4) C(6) C(5) -0.5(9) yes . . . . S(1) C(5) C(6) S(2) -0.4(7) yes . . . . S(1) C(5) C(6) C(4) 179.6(5) yes . . . . C(3) C(5) C(6) S(2) 179.8(5) yes . . . . C(3) C(5) C(6) C(4) -0.2(9) yes . . . . S(1) C(7) C(8) S(3) 1.4(8) yes . . . . S(1) C(7) C(8) S(4) -179.6(4) yes . . . . S(2) C(7) C(8) S(3) -177.9(4) yes . . . . S(2) C(7) C(8) S(4) 1.1(8) yes . . . . S(3) C(9) C(10) S(4) -0.6(7) yes . . . . S(3) C(9) C(10) S(5) -179.3(4) yes . . . . C(11) C(9) C(10) S(4) 179.0(5) yes . . . . C(11) C(9) C(10) S(5) 0.3(9) yes . . . . S(3) C(9) C(11) S(6) -1.0(7) yes . . . . S(3) C(9) C(11) S(7) 178.4(4) yes . . . . C(10) C(9) C(11) S(6) 179.4(5) yes . . . . C(10) C(9) C(11) S(7) -1.2(9) yes . . . . S(6) C(12) C(13) S(7) -1.2(9) yes . . . . 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(1) Br(1) 3.815(2) yes . 55504 Br(1) Br(2) 3.785(2) yes . 55501 Br(1) Br(3) 3.764(1) yes . 55501 Br(1) S(7) 3.442(2) yes . 65602 Br(1) C(4) 4.111(6) yes . 55504 Br(1) C(13) 3.752(8) yes . 65602 Br(2) Br(1) 3.785(2) yes . 55501 Br(2) Br(1) 3.785(2) yes . 55504 Br(2) Br(3) 3.786(2) yes . 55501 Br(3) Br(1) 3.764(1) yes . 55501 Br(3) Br(1) 3.764(1) yes . 55504 Br(3) Br(2) 3.786(2) yes . 55501 Br(3) Br(2) 4.109(2) yes . 55601 Br(3) C(2) 3.797(7) yes . 55501 Br(3) C(2) 3.797(7) yes . 55504 Br(3) C(4) 4.007(6) yes . 55501 Br(3) C(4) 4.007(6) yes . 55504 S(1) S(2) 2.942(2) yes . 55501 S(1) S(3) 3.225(2) yes . 55501 S(1) S(4) 3.699(2) yes . 55601 S(1) S(5) 3.886(3) yes . 55601 S(1) C(1) 4.002(8) yes . 55501 S(1) C(3) 2.766(7) yes . 55501 S(1) C(4) 3.982(7) yes . 55501 S(1) C(6) 2.681(7) yes . 55501 S(1) C(8) 2.721(6) yes . 55501 S(2) S(1) 2.942(2) yes . 55501 S(2) S(4) 3.217(2) yes . 55501 S(2) S(5) 3.696(2) yes . 65603 S(2) C(2) 4.019(8) yes . 55501 S(2) C(3) 3.982(7) yes . 55501 S(2) C(4) 2.755(7) yes . 55501 S(2) C(5) 2.656(6) yes . 55501 S(2) C(8) 2.714(6) yes . 55501 S(3) S(1) 3.225(2) yes . 55501 S(3) S(4) 2.926(2) yes . 55501 S(3) S(5) 3.586(2) yes . 55601 S(3) S(6) 3.059(3) yes . 55501 S(3) C(7) 2.719(6) yes . 55501 S(3) C(10) 2.702(6) yes . 55501 S(3) C(11) 2.704(6) yes . 55501 S(4) S(2) 3.217(2) yes . 55501 S(4) S(3) 2.926(2) yes . 55501 S(4) S(4) 3.804(2) yes . 65603 S(4) S(5) 2.934(2) yes . 55501 S(4) S(5) 3.633(2) yes . 65603 S(4) C(7) 2.720(6) yes . 55501 S(4) C(9) 2.649(7) yes . 55501 S(4) C(10) 4.092(5) yes . 65603 S(4) C(11) 3.997(7) yes . 55501 S(5) S(2) 3.696(2) yes . 65603 S(5) S(4) 2.934(2) yes . 55501 S(5) S(4) 3.633(2) yes . 65603 S(5) S(7) 2.990(2) yes . 55501 S(5) C(9) 2.733(6) yes . 55501 S(5) C(11) 3.202(6) yes . 55501 S(6) S(3) 3.059(3) yes . 55501 S(6) S(5) 4.199(3) yes . 55601 S(6) S(7) 2.893(3) yes . 55501 S(6) C(9) 2.698(6) yes . 55501 S(6) C(10) 4.026(6) yes . 55501 S(6) C(13) 2.578(8) yes . 55501 S(7) Br(1) 3.442(2) yes . 64602 S(7) S(5) 2.990(2) yes . 55501 S(7) S(6) 2.893(3) yes . 55501 S(7) C(9) 2.761(7) yes . 55501 S(7) C(10) 3.199(6) yes . 55501 S(7) C(12) 2.621(8) yes . 55501 C(1) Br(1) 3.826(8) yes . 55604 C(1) S(1) 4.002(8) yes . 55501 C(1) C(4) 2.40(1) yes . 55501 C(1) C(5) 2.38(1) yes . 55501 C(1) C(6) 2.741(9) yes . 55501 C(2) Br(1) 4.136(8) yes . 55604 C(2) Br(2) 4.108(7) yes . 55601 C(2) Br(3) 3.797(7) yes . 55501 C(2) S(2) 4.019(8) yes . 55501 C(2) C(3) 2.41(1) yes . 55501 C(2) C(5) 2.768(9) yes . 55501 C(2) C(6) 2.38(1) yes . 55501 C(3) S(1) 2.766(7) yes . 55501 C(3) S(2) 3.982(7) yes . 55501 C(3) S(2) 3.967(7) yes . 55601 C(3) S(4) 4.112(7) yes . 55601 C(3) C(2) 2.41(1) yes . 55501 C(3) C(4) 2.798(9) yes . 55501 C(3) C(6) 2.415(9) yes . 55501 C(3) C(7) 3.947(9) yes . 55501 C(4) Br(1) 4.111(6) yes . 55504 C(4) Br(3) 4.007(6) yes . 55501 C(4) S(1) 3.982(7) yes . 55501 C(4) S(2) 2.755(7) yes . 55501 C(4) C(1) 2.40(1) yes . 55501 C(4) C(3) 2.798(9) yes . 55501 C(4) C(5) 2.412(9) yes . 55501 C(4) C(7) 3.940(9) yes . 55501 C(5) S(2) 2.656(6) yes . 55501 C(5) C(1) 2.38(1) yes . 55501 C(5) C(2) 2.768(9) yes . 55501 C(5) C(4) 2.412(9) yes . 55501 C(5) C(7) 2.571(9) yes . 55501 C(5) C(8) 3.895(9) yes . 55501 C(6) S(1) 2.681(7) yes . 55501 C(6) C(1) 2.741(9) yes . 55501 C(6) C(2) 2.38(1) yes . 55501 C(6) C(3) 2.415(9) yes . 55501 C(6) C(7) 2.593(9) yes . 55501 C(6) C(8) 3.914(9) yes . 55501 C(7) S(3) 2.719(6) yes . 55501 C(7) S(4) 2.720(6) yes . 55501 C(7) C(3) 3.947(9) yes . 55501 C(7) C(4) 3.940(9) yes . 55501 C(7) C(5) 2.571(9) yes . 55501 C(7) C(6) 2.593(9) yes . 55501 C(7) C(9) 3.925(9) yes . 55501 C(7) C(10) 3.945(8) yes . 55501 C(8) S(1) 2.721(6) yes . 55501 C(8) S(2) 2.714(6) yes . 55501 C(8) C(5) 3.895(9) yes . 55501 C(8) C(6) 3.914(9) yes . 55501 C(8) C(9) 2.599(9) yes . 55501 C(8) C(10) 2.624(8) yes . 55501 C(8) C(11) 3.930(9) yes . 55501 C(9) S(4) 2.649(7) yes . 55501 C(9) S(5) 2.733(6) yes . 55501 C(9) S(6) 2.698(6) yes . 55501 C(9) S(7) 2.761(7) yes . 55501 C(9) C(7) 3.925(9) yes . 55501 C(9) C(8) 2.599(9) yes . 55501 C(9) C(12) 3.90(1) yes . 55501 C(9) C(13) 3.90(1) yes . 55501 C(10) S(3) 2.702(6) yes . 55501 C(10) S(4) 4.092(5) yes . 65603 C(10) S(6) 4.026(6) yes . 55501 C(10) S(7) 3.199(6) yes . 55501 C(10) C(7) 3.945(8) yes . 55501 C(10) C(8) 2.624(8) yes . 55501 C(10) C(11) 2.473(9) yes . 55501 C(11) S(3) 2.704(6) yes . 55501 C(11) S(4) 3.997(7) yes . 55501 C(11) S(5) 3.202(6) yes . 55501 C(11) C(8) 3.930(9) yes . 55501 C(11) C(10) 2.473(9) yes . 55501 C(11) C(12) 2.55(1) yes . 55501 C(11) C(13) 2.52(1) yes . 55501 C(12) S(7) 2.621(8) yes . 55501 C(12) C(9) 3.90(1) yes . 55501 C(12) C(11) 2.55(1) yes . 55501 C(13) Br(1) 3.752(8) yes . 64602 C(13) S(6) 2.578(8) yes . 55501 C(13) C(9) 3.90(1) yes . 55501 C(13) C(11) 2.52(1) yes . 55501 #============================================================================== # 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 #==============================================================================