Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_General _journal_coden_Cambridge 1145 #=========================================================================== _audit_creation_date '19101-02-23' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #=========================================================================== # SUBMISSION DETAILS _publ_requested_journal 'Journal of Materials Chemistry ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name 'Prof Takehiko Mori ' _publ_contact_author_address ; Prof Takehiko Mori Department of Organic and Polymeric Materials Tokyo Institute of Technology Meguro-ku Tokyo 152-8552 JAPAN ; _publ_contact_letter ; ENTER TEXT OF LETTER ; #=========================================================================== #=========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Tetrathiapentalene-Based Organic Conductors With 1:1 Composition ; _publ_section_title_footnote ; ENTER ANY FOOTNOTES TO TITLE ; loop_ _publ_author_name 'Aragaki, Masanobu' 'Katsuhara, Mao' 'Kimura, Shinya' 'Misaki, Yohji' 'Mori, Takehiko' 'Tanaka, Kazuyoshi' #=========================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1998). teXsan for Windows version 1.03. Single Crystal Structure Analysis Software. Version 1.04. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=========================================================================== data_(TTM-TTP)GaCl4(PhCl)0.5 _database_code_CSD 159320 #=========================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; DIRDIF92 ORIENT (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #--------------------------------------------------------------------------- #-- _cell_length_a 13.849(6) _cell_length_b 14.215(8) _cell_length_c 8.600(7) _cell_angle_alpha 106.78(5) _cell_angle_beta 94.77(5) _cell_angle_gamma 78.22(4) _cell_volume 1586(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.7 _cell_measurement_theta_max 14.8 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #--------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 832.78 _chemical_formula_analytical ? _chemical_formula_sum 'C17 H14.50 Cl4.50 Ga S12 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 832.00 _exptl_absorpt_coefficient_mu 2.046 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.851 _exptl_special_details ; ? ; #=========================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.38 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 0 2 2 0 0 1 1 _diffrn_reflns_number 9813 _reflns_number_total 9239 _reflns_number_gt 4116 _reflns_threshold_expression I>5.00\s(I) _diffrn_reflns_av_R_equivalents 0.01262 _diffrn_reflns_av_sigmaI/netI 0.056 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01988 _diffrn_orient_matrix_UB_12 0.07111 _diffrn_orient_matrix_UB_13 0.06584 _diffrn_orient_matrix_UB_21 0.06934 _diffrn_orient_matrix_UB_22 0.00015 _diffrn_orient_matrix_UB_23 0.04295 _diffrn_orient_matrix_UB_31 0.01552 _diffrn_orient_matrix_UB_32 0.02327 _diffrn_orient_matrix_UB_33 -0.09263 #--------------------------------------------------------------------------- #-- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 34 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 24 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 29 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ga 0 2 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 9 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #=========================================================================== #== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ga(1) 0.76367(4) 0.70725(5) 0.24908(9) 0.0718(2) 1.000 . Uani d ? Cl(1) 0.8330(2) 0.6345(2) 0.4355(4) 0.154(1) 1.000 . Uani d ? Cl(2) 0.8297(1) 0.8289(1) 0.2616(4) 0.1472(9) 1.000 . Uani d ? Cl(3) 0.6077(1) 0.7494(1) 0.2968(2) 0.0790(5) 1.000 . Uani d ? Cl(4) 0.7901(2) 0.5940(2) 0.0264(3) 0.1479(8) 1.000 . Uani d ? Cl(5) 0.326(2) 0.181(2) 0.163(5) 0.78(3) 0.500 S Uani d ? S(1) 0.1294(1) 0.9448(1) 0.8967(2) 0.0750(4) 1.000 . Uani d ? S(2) 0.0213(1) 0.7546(1) 0.8788(2) 0.0766(5) 1.000 . Uani d ? S(3) 0.28441(8) 0.79378(8) 0.6879(1) 0.0466(3) 1.000 . Uani d ? S(4) 0.18751(8) 0.62548(9) 0.6638(1) 0.0461(3) 1.000 . Uani d ? S(5) 0.44395(8) 0.64704(8) 0.4232(1) 0.0391(3) 1.000 . Uani d ? S(6) 0.33904(8) 0.48002(8) 0.4015(1) 0.0418(3) 1.000 . Uani d ? S(7) 0.58960(7) 0.50510(8) 0.1705(1) 0.0379(3) 1.000 . Uani d ? S(8) 0.48302(8) 0.33990(8) 0.1504(1) 0.0433(3) 1.000 . Uani d ? S(9) 0.74304(8) 0.35359(8) -0.0885(1) 0.0407(3) 1.000 . Uani d ? S(10) 0.63874(8) 0.19067(8) -0.1119(2) 0.0494(3) 1.000 . Uani d ? S(11) 0.89168(8) 0.2259(1) -0.3375(2) 0.0551(4) 1.000 . Uani d ? S(12) 0.7709(1) 0.0447(1) -0.3713(2) 0.0861(5) 1.000 . Uani d ? C(1) 0.0468(5) 0.9851(4) 0.7452(8) 0.081(2) 1.000 . Uani d ? C(2) -0.0133(5) 0.6345(7) 0.791(1) 0.122(3) 1.000 . Uani d ? C(3) 0.1731(3) 0.8195(4) 0.7879(6) 0.051(1) 1.000 . Uani d ? C(4) 0.1293(3) 0.7436(4) 0.7789(5) 0.048(1) 1.000 . Uani d ? C(5) 0.2817(3) 0.6686(3) 0.6012(5) 0.040(1) 1.000 . Uani d ? C(6) 0.3472(3) 0.6065(3) 0.4890(5) 0.038(1) 1.000 . Uani d ? C(7) 0.4849(3) 0.5327(3) 0.2844(5) 0.035(1) 1.000 . Uani d ? C(8) 0.4362(3) 0.4571(3) 0.2750(5) 0.038(1) 1.000 . Uani d ? C(9) 0.5803(3) 0.3791(3) 0.0857(5) 0.036(1) 1.000 . Uani d ? C(10) 0.6459(3) 0.3148(3) -0.0252(5) 0.038(1) 1.000 . Uani d ? C(11) 0.7881(3) 0.2385(3) -0.2241(5) 0.040(1) 1.000 . Uani d ? C(12) 0.7401(3) 0.1637(3) -0.2361(6) 0.045(1) 1.000 . Uani d ? C(13) 0.9257(4) 0.3462(4) -0.2629(7) 0.065(2) 1.000 . Uani d ? C(14) 0.688(2) 0.001(1) -0.403(3) 0.678(9) 1.000 . Uani d ? C(15) 0.425(2) 0.064(1) 0.022(4) 0.31(1) 1.000 . Uani d ? C(16) 0.4808(9) 0.090(1) 0.220(2) 0.214(6) 1.000 . Uani d ? C(17) 0.543(2) 0.006(2) 0.117(3) 0.30(1) 1.000 . Uani d ? H(1) -0.0168 1.0174 0.7881 0.093 1.000 . Uiso c ? H(2) 0.0723 1.0316 0.7049 0.093 1.000 . Uiso c ? H(3) 0.0383 0.9294 0.6536 0.093 1.000 . Uiso c ? H(4) -0.0229 0.6034 0.8718 0.137 1.000 . Uiso c ? H(5) -0.0732 0.6397 0.7259 0.137 1.000 . Uiso c ? H(6) 0.0373 0.5888 0.7195 0.137 1.000 . Uiso c ? H(7) 0.9319 0.3650 -0.1464 0.077 1.000 . Uiso c ? H(8) 0.9871 0.3462 -0.3054 0.077 1.000 . Uiso c ? H(9) 0.8764 0.3965 -0.2931 0.077 1.000 . Uiso c ? H(10) 0.6653 -0.0064 -0.3103 0.809 1.000 . Uiso c ? H(11) 0.6356 0.0460 -0.4470 0.809 1.000 . Uiso c ? H(12) 0.7007 -0.0602 -0.4858 0.809 1.000 . Uiso 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) 0.0454(3) 0.0642(4) 0.0942(5) -0.0154(3) 0.0152(3) -0.0030(3) Cl(1) 0.100(2) 0.201(2) 0.199(3) -0.043(2) -0.020(2) 0.112(2) Cl(2) 0.097(1) 0.071(1) 0.265(3) -0.036(1) 0.056(2) 0.007(1) Cl(3) 0.0463(7) 0.0695(9) 0.114(1) -0.0114(6) 0.0204(7) 0.0085(8) Cl(4) 0.135(2) 0.100(1) 0.183(2) -0.060(1) 0.097(1) -0.052(1) Cl(5) 0.87(4) 0.57(4) 1.05(8) -0.52(3) 0.66(4) 0.04(4) S(1) 0.086(1) 0.0582(8) 0.0584(9) 0.0239(7) 0.0148(8) 0.0034(7) S(2) 0.0481(7) 0.099(1) 0.080(1) 0.0144(7) 0.0325(7) 0.0317(8) S(3) 0.0453(6) 0.0414(6) 0.0508(7) 0.0036(5) 0.0114(5) 0.0144(5) S(4) 0.0372(5) 0.0520(6) 0.0497(7) -0.0009(5) 0.0117(5) 0.0171(5) S(5) 0.0367(5) 0.0375(5) 0.0417(6) -0.0004(4) 0.0109(4) 0.0109(4) S(6) 0.0347(5) 0.0440(6) 0.0467(6) -0.0044(4) 0.0111(5) 0.0120(5) S(7) 0.0347(5) 0.0365(5) 0.0420(6) -0.0007(4) 0.0113(4) 0.0115(4) S(8) 0.0388(5) 0.0389(6) 0.0498(7) -0.0042(4) 0.0124(5) 0.0076(5) S(9) 0.0370(5) 0.0388(6) 0.0435(6) -0.0001(4) 0.0107(5) 0.0093(5) S(10) 0.0418(6) 0.0389(6) 0.0637(8) -0.0039(5) 0.0123(5) 0.0081(5) S(11) 0.0425(6) 0.0602(7) 0.0552(7) 0.0048(5) 0.0182(5) 0.0101(6) S(12) 0.0685(9) 0.0465(8) 0.116(1) -0.0011(7) 0.0286(9) -0.0206(8) C(1) 0.084(4) 0.063(3) 0.083(4) 0.022(3) 0.010(3) 0.024(3) C(2) 0.092(5) 0.163(7) 0.126(6) -0.053(5) 0.046(4) 0.031(5) C(3) 0.048(3) 0.051(3) 0.047(3) 0.012(2) 0.016(2) 0.011(2) C(4) 0.035(2) 0.061(3) 0.044(3) 0.014(2) 0.014(2) 0.022(2) C(5) 0.040(2) 0.039(2) 0.042(2) 0.001(2) 0.007(2) 0.016(2) C(6) 0.036(2) 0.039(2) 0.039(2) 0.001(2) 0.008(2) 0.013(2) C(7) 0.030(2) 0.037(2) 0.036(2) 0.002(2) 0.010(2) 0.013(2) C(8) 0.034(2) 0.041(2) 0.037(2) 0.001(2) 0.009(2) 0.012(2) C(9) 0.033(2) 0.037(2) 0.038(2) -0.002(2) 0.006(2) 0.012(2) C(10) 0.033(2) 0.037(2) 0.041(2) 0.001(2) 0.008(2) 0.009(2) C(11) 0.034(2) 0.045(2) 0.035(2) 0.003(2) 0.004(2) 0.008(2) C(12) 0.039(2) 0.038(2) 0.051(3) 0.004(2) 0.007(2) 0.008(2) C(13) 0.052(3) 0.070(3) 0.078(4) -0.013(2) 0.019(3) 0.020(3) C(14) 0.73(2) 0.33(1) 0.83(2) -0.42(1) 0.69(2) -0.47(1) C(15) 0.35(2) 0.17(1) 0.49(3) -0.07(1) 0.16(2) 0.16(1) C(16) 0.132(8) 0.22(1) 0.39(2) -0.104(7) -0.06(1) 0.21(1) C(17) 0.33(2) 0.24(2) 0.41(3) -0.20(1) -0.04(2) 0.16(2) #=========================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4116 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_all 0.0710 _refine_ls_wR_factor_ref 0.0710 _refine_ls_goodness_of_fit_all 3.407 _refine_ls_goodness_of_fit_ref 3.410 _refine_ls_shift/su_max 7.9600 _refine_ls_shift/su_mean 0.3007 _refine_diff_density_min -4.97 _refine_diff_density_max 5.18 #=========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga(1) Cl(1) 2.204(5) . . ? Ga(1) Cl(2) 2.088(4) . . ? Ga(1) Cl(3) 2.161(3) . . ? Ga(1) Cl(4) 2.118(4) . . ? Cl(5) C(15) 2.08(6) . . ? S(1) C(1) 1.80(1) . . ? S(1) C(3) 1.763(9) . . ? S(2) C(2) 1.80(2) . . ? S(2) C(4) 1.744(8) . . ? S(3) C(3) 1.749(9) . . ? S(3) C(5) 1.727(8) . . ? S(4) C(4) 1.752(9) . . ? S(4) C(5) 1.733(8) . . ? S(5) C(6) 1.755(8) . . ? S(5) C(7) 1.733(8) . . ? S(6) C(6) 1.760(8) . . ? S(6) C(8) 1.720(8) . . ? S(7) C(7) 1.731(7) . . ? S(7) C(9) 1.755(8) . . ? S(8) C(8) 1.728(8) . . ? S(8) C(9) 1.746(8) . . ? S(9) C(10) 1.734(8) . . ? S(9) C(11) 1.740(8) . . ? S(10) C(10) 1.726(8) . . ? S(10) C(12) 1.747(9) . . ? S(11) C(11) 1.751(8) . . ? S(11) C(13) 1.79(1) . . ? S(12) C(12) 1.745(9) . . ? S(12) C(14) 1.38(3) . . ? C(1) H(1) 0.96 . . no C(1) H(2) 0.96 . . no C(1) H(3) 0.96 . . no C(2) H(4) 0.96 . . no C(2) H(5) 0.96 . . no C(2) H(6) 0.97 . . no C(3) C(4) 1.32(1) . . ? C(5) C(6) 1.36(1) . . ? C(7) C(8) 1.36(1) . . ? C(9) C(10) 1.37(1) . . ? C(11) C(12) 1.34(1) . . ? C(13) H(7) 0.96 . . no C(13) H(8) 0.95 . . no C(13) H(9) 0.96 . . no C(14) H(10) 0.93 . . no C(14) H(11) 0.99 . . no C(14) H(12) 0.95 . . no C(15) C(16) 1.78(6) . . ? C(15) C(17) 1.36(5) . . ? C(16) C(17) 1.42(6) . . ? #--------------------------------------------------------------------------- #-- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ga(1) Cl(2) 108.9(2) . . . ? Cl(1) Ga(1) Cl(3) 106.6(2) . . . ? Cl(1) Ga(1) Cl(4) 104.5(2) . . . ? Cl(2) Ga(1) Cl(3) 113.2(2) . . . ? Cl(2) Ga(1) Cl(4) 112.3(2) . . . ? Cl(3) Ga(1) Cl(4) 110.7(2) . . . ? C(1) S(1) C(3) 99.9(5) . . . ? C(2) S(2) C(4) 102.9(5) . . . ? C(3) S(3) C(5) 94.8(4) . . . ? C(4) S(4) C(5) 95.0(4) . . . ? C(6) S(5) C(7) 94.0(4) . . . ? C(6) S(6) C(8) 93.9(4) . . . ? C(7) S(7) C(9) 93.8(4) . . . ? C(8) S(8) C(9) 94.0(4) . . . ? C(10) S(9) C(11) 95.4(4) . . . ? C(10) S(10) C(12) 95.5(4) . . . ? C(11) S(11) C(13) 103.0(4) . . . ? C(12) S(12) C(14) 109(1) . . . ? S(1) C(1) H(1) 111.5 . . . no S(1) C(1) H(2) 111.0 . . . no S(1) C(1) H(3) 111.1 . . . no H(1) C(1) H(2) 107.8 . . . no H(1) C(1) H(3) 108.0 . . . no H(2) C(1) H(3) 107.3 . . . no S(2) C(2) H(4) 112.1 . . . no S(2) C(2) H(5) 111.7 . . . no S(2) C(2) H(6) 111.2 . . . no H(4) C(2) H(5) 107.8 . . . no H(4) C(2) H(6) 107.1 . . . no H(5) C(2) H(6) 106.6 . . . no S(1) C(3) S(3) 117.1(6) . . . ? S(1) C(3) C(4) 125.1(7) . . . ? S(3) C(3) C(4) 117.8(6) . . . ? S(2) C(4) S(4) 119.4(6) . . . ? S(2) C(4) C(3) 123.9(7) . . . ? S(4) C(4) C(3) 116.6(6) . . . ? S(3) C(5) S(4) 115.4(4) . . . ? S(3) C(5) C(6) 123.6(6) . . . ? S(4) C(5) C(6) 121.0(6) . . . ? S(5) C(6) S(6) 116.1(4) . . . ? S(5) C(6) C(5) 122.4(6) . . . ? S(6) C(6) C(5) 121.5(6) . . . ? S(5) C(7) S(7) 124.5(5) . . . ? S(5) C(7) C(8) 117.5(5) . . . ? S(7) C(7) C(8) 117.8(6) . . . ? S(6) C(8) S(8) 123.4(5) . . . ? S(6) C(8) C(7) 118.4(6) . . . ? S(8) C(8) C(7) 117.9(6) . . . ? S(7) C(9) S(8) 116.5(4) . . . ? S(7) C(9) C(10) 121.9(6) . . . ? S(8) C(9) C(10) 121.6(6) . . . ? S(9) C(10) S(10) 115.2(4) . . . ? S(9) C(10) C(9) 121.6(6) . . . ? S(10) C(10) C(9) 123.2(6) . . . ? S(9) C(11) S(11) 119.4(5) . . . ? S(9) C(11) C(12) 117.1(6) . . . ? S(11) C(11) C(12) 123.5(6) . . . ? S(10) C(12) S(12) 119.3(5) . . . ? S(10) C(12) C(11) 116.8(6) . . . ? S(12) C(12) C(11) 123.9(6) . . . ? S(11) C(13) H(7) 110.7 . . . no S(11) C(13) H(8) 111.1 . . . no S(11) C(13) H(9) 110.7 . . . no H(7) C(13) H(8) 108.3 . . . no H(7) C(13) H(9) 107.7 . . . no H(8) C(13) H(9) 108.3 . . . no S(12) C(14) H(10) 112.2 . . . no S(12) C(14) H(11) 108.0 . . . no S(12) C(14) H(12) 110.7 . . . no H(10) C(14) H(11) 107.9 . . . no H(10) C(14) H(12) 111.6 . . . no H(11) C(14) H(12) 106.2 . . . no Cl(5) C(15) C(16) 75(3) . . . ? Cl(5) C(15) C(17) 155(6) . . . ? C(16) C(15) C(17) 130(5) . . . ? C(15) C(16) C(17) 72(3) . . . ? C(15) C(17) C(16) 158(6) 2_655 2_655 2_655 ? #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ga(1) H(8) 3.4041 . 2_765 no Ga(1) H(12) 3.4188 . 1_566 no Ga(1) S(7) 3.995(3) . . no Cl(1) H(5) 2.7064 . 1_655 no Cl(1) H(8) 2.9075 . 2_765 no Cl(1) H(6) 3.2725 . 2_666 no Cl(1) C(2) 3.58(2) . 1_655 no Cl(1) S(4) 3.611(6) . 2_666 no Cl(1) S(6) 3.708(5) . 2_666 no Cl(1) C(13) 3.86(1) . 2_765 no Cl(2) H(2) 2.5613 . 2_676 no Cl(2) H(12) 2.8131 . 1_566 no Cl(2) H(8) 3.2520 . 2_765 no Cl(2) C(1) 3.45(1) . 2_676 no Cl(2) C(14) 3.61(2) . 1_566 no Cl(2) S(12) 3.723(6) . 1_566 no Cl(2) C(13) 3.77(1) . 2_765 no Cl(2) S(11) 3.817(5) . 2_765 no Cl(2) S(1) 3.990(6) . 2_676 no Cl(2) Cl(5) 4.06(9) . 2_665 no Cl(3) H(12) 3.2531 . 1_566 no Cl(3) S(5) 3.334(4) . . no Cl(3) S(7) 3.382(4) . . no Cl(3) S(10) 3.687(4) . 2_665 no Cl(3) C(7) 3.783(9) . . no Cl(3) S(8) 3.874(5) . 2_665 no Cl(3) C(14) 4.07(2) . 1_566 no Cl(4) H(4) 3.0513 . 1_654 no Cl(4) H(9) 3.4032 . . no Cl(4) H(7) 3.4268 . . no Cl(4) S(9) 3.454(5) . . no Cl(4) S(7) 3.708(4) . . no Cl(4) C(2) 3.75(1) . 1_654 no Cl(4) C(13) 3.89(1) . . no Cl(4) S(6) 3.910(7) . 2_665 no Cl(4) C(8) 3.94(1) . 2_665 no Cl(4) Cl(5) 3.99(8) . 2_665 no Cl(4) S(8) 3.990(6) . 2_665 no Cl(5) H(10) 3.0813 . 2_655 no Cl(5) S(8) 3.46(4) . . no Cl(5) C(14) 3.80(8) . 2_655 no S(1) H(1) 3.0968 . 2_577 no S(1) C(12) 3.84(1) . 2_666 no S(1) C(1) 3.86(1) . 2_577 no S(1) S(1) 3.952(6) . 2_577 no S(1) S(10) 3.999(4) . 2_666 no S(2) H(7) 3.1879 . 2_666 no S(2) C(11) 3.799(9) . 2_666 no S(2) S(9) 3.853(4) . 2_666 no S(2) C(13) 3.92(1) . 2_666 no S(2) S(11) 3.976(5) . 2_666 no S(3) C(10) 3.639(9) . 2_666 no S(3) S(10) 3.669(5) . 2_666 no S(3) C(9) 3.690(9) . 2_666 no S(3) S(11) 3.698(4) . 2_665 no S(3) S(8) 3.768(4) . 2_666 no S(3) C(16) 3.87(2) . 2_666 no S(3) C(11) 3.949(9) . 2_665 no S(3) S(12) 3.977(5) . 2_665 no S(3) C(17) 4.00(3) . 2_666 no S(3) C(12) 4.08(1) . 2_665 no S(4) H(9) 3.1807 . 2_665 no S(4) S(9) 3.641(4) . 2_666 no S(4) S(7) 3.669(4) . 2_666 no S(4) C(10) 3.713(9) . 2_666 no S(4) C(9) 3.718(8) . 2_666 no S(4) C(13) 3.76(1) . 2_665 no S(4) S(11) 3.938(4) . 2_665 no S(5) C(8) 3.490(9) . 2_666 no S(5) S(6) 3.629(4) . 2_666 no S(5) S(8) 3.684(4) . 2_666 no S(5) C(10) 3.694(9) . 2_665 no S(5) S(9) 3.708(4) . 2_665 no S(5) C(11) 3.803(9) . 2_665 no S(5) C(12) 3.917(9) . 2_665 no S(5) S(10) 3.972(4) . 2_665 no S(5) C(7) 4.012(9) . 2_666 no S(6) H(9) 3.3466 . 2_665 no S(6) C(7) 3.504(9) . 2_666 no S(6) S(7) 3.688(4) . 2_666 no S(6) S(9) 4.025(4) . 2_665 no S(6) C(8) 4.061(9) . 2_666 no S(7) C(9) 3.571(8) . 2_665 no S(7) S(7) 3.671(5) . 2_665 no S(7) C(6) 3.680(9) . 2_666 no S(7) C(5) 3.681(9) . 2_666 no S(7) C(7) 3.873(9) . 2_665 no S(7) S(8) 3.954(4) . 2_665 no S(7) C(8) 3.998(9) . 2_665 no S(7) C(10) 4.063(8) . 2_665 no S(8) C(6) 3.725(9) . 2_666 no S(8) C(5) 3.745(9) . 2_666 no S(8) C(16) 3.78(2) . . no S(8) C(15) 3.99(3) . . no S(9) C(4) 3.531(9) . 2_666 no S(9) C(6) 3.725(9) . 2_665 no S(9) C(7) 3.745(8) . 2_665 no S(9) C(8) 3.884(9) . 2_665 no S(9) C(3) 4.01(1) . 2_666 no S(10) C(3) 3.67(1) . 2_666 no S(11) H(3) 3.0497 . 2_665 no S(11) H(2) 3.4099 . 1_644 no S(11) H(1) 3.4130 . 1_644 no S(11) C(5) 3.570(9) . 2_665 no S(11) C(3) 3.80(1) . 2_665 no S(11) C(1) 3.87(1) . 1_644 no S(11) C(1) 3.92(1) . 2_665 no S(11) C(4) 3.924(9) . 2_665 no S(11) C(6) 4.022(9) . 2_665 no S(12) H(1) 3.1381 . 1_644 no S(12) C(1) 3.85(1) . 1_644 no C(2) H(7) 3.1684 . 2_666 no C(2) C(13) 4.09(2) . 2_666 no C(3) C(10) 3.68(1) . 2_666 no C(3) C(12) 3.90(1) . 2_666 no C(3) C(11) 4.04(1) . 2_666 no C(4) C(10) 3.71(1) . 2_666 no C(4) C(11) 3.86(1) . 2_666 no C(5) C(9) 3.32(1) . 2_666 no C(5) H(9) 3.3351 . 2_665 no C(5) C(10) 3.65(1) . 2_666 no C(5) C(11) 3.82(1) . 2_665 no C(5) C(13) 3.91(1) . 2_665 no C(6) H(9) 3.4031 . 2_665 no C(6) C(7) 3.56(1) . 2_666 no C(6) C(8) 3.59(1) . 2_666 no C(6) C(9) 3.67(1) . 2_666 no C(6) C(11) 3.75(1) . 2_665 no C(7) C(10) 3.67(1) . 2_665 no C(7) C(9) 3.73(1) . 2_665 no C(7) C(8) 3.82(1) . 2_666 no C(7) C(7) 4.04(2) . 2_666 no C(8) C(8) 4.08(2) . 2_666 no C(13) H(4) 3.4480 . 2_666 no C(14) C(16) 3.56(4) . 2_655 no C(15) H(10) 3.2363 . 2_655 no C(16) H(10) 2.8084 . 2_655 no C(17) H(10) 3.4415 . 2_655 no H(4) H(7) 2.5480 . 2_666 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl(5) C(15) C(16) C(17) . . . . 177(2) no Cl(5) C(15) C(17) C(16) . . . . -173(6) no S(1) C(3) S(3) C(5) . . . . -176.8(6) no S(1) C(3) C(4) S(2) . . . . -2(1) no S(1) C(3) C(4) S(4) . . . . -179.7(5) no S(2) C(4) S(4) C(5) . . . . 179.0(6) no S(2) C(4) C(3) S(3) . . . . 176.8(5) no S(3) C(3) S(1) C(1) . . . . 95.2(7) no S(3) C(3) C(4) S(4) . . . . -1(1) no S(3) C(5) S(4) C(4) . . . . 6.1(6) no S(3) C(5) C(6) S(5) . . . . 1(1) no S(3) C(5) C(6) S(6) . . . . -178.6(5) no S(4) C(4) S(2) C(2) . . . . -12.5(8) no S(4) C(5) S(3) C(3) . . . . -6.5(6) no S(4) C(5) C(6) S(5) . . . . -179.7(5) no S(4) C(5) C(6) S(6) . . . . 0(1) no S(5) C(6) S(6) C(8) . . . . -2.7(5) no S(5) C(7) S(7) C(9) . . . . 175.0(5) no S(5) C(7) C(8) S(6) . . . . -0.5(9) no S(5) C(7) C(8) S(8) . . . . -174.4(4) no S(6) C(6) S(5) C(7) . . . . 2.5(5) no S(6) C(8) S(8) C(9) . . . . -174.7(6) no S(6) C(8) C(7) S(7) . . . . 173.9(4) no S(7) C(7) S(5) C(6) . . . . -175.3(6) no S(7) C(7) C(8) S(8) . . . . 0.1(9) no S(7) C(9) S(8) C(8) . . . . 1.8(5) no S(7) C(9) C(10) S(9) . . . . 0(1) no S(7) C(9) C(10) S(10) . . . . -179.7(5) no S(8) C(8) S(6) C(6) . . . . 175.4(6) no S(8) C(9) S(7) C(7) . . . . -1.8(5) no S(8) C(9) C(10) S(9) . . . . -179.5(5) no S(8) C(9) C(10) S(10) . . . . 0(1) no S(9) C(10) S(10) C(12) . . . . -1.7(6) no S(9) C(11) S(11) C(13) . . . . 3.1(7) no S(9) C(11) C(12) S(10) . . . . -1(1) no S(9) C(11) C(12) S(12) . . . . 177.2(5) no S(10) C(10) S(9) C(11) . . . . 1.4(6) no S(10) C(12) S(12) C(14) . . . . 23(3) no S(10) C(12) C(11) S(11) . . . . 179.6(5) no S(11) C(11) S(9) C(10) . . . . 179.3(5) no S(11) C(11) C(12) S(12) . . . . -2(1) no S(12) C(12) S(10) C(10) . . . . -176.5(6) no C(1) S(1) C(3) C(4) . . . . -86(1) no C(2) S(2) C(4) C(3) . . . . 170(1) no C(3) S(3) C(5) C(6) . . . . 172.5(8) no C(3) C(4) S(4) C(5) . . . . -3.0(8) no C(4) S(4) C(5) C(6) . . . . -172.9(7) no C(4) C(3) S(3) C(5) . . . . 4.6(8) no C(5) C(6) S(5) C(7) . . . . -177.4(7) no C(5) C(6) S(6) C(8) . . . . 177.2(7) no C(6) S(5) C(7) C(8) . . . . -1.2(7) no C(6) S(6) C(8) C(7) . . . . 1.9(7) no C(7) S(7) C(9) C(10) . . . . 178.3(7) no C(7) C(8) S(8) C(9) . . . . -1.1(7) no C(8) S(8) C(9) C(10) . . . . -178.3(7) no C(8) C(7) S(7) C(9) . . . . 1.0(7) no C(9) C(10) S(9) C(11) . . . . -178.6(7) no C(9) C(10) S(10) C(12) . . . . 178.3(8) no C(10) S(9) C(11) C(12) . . . . -0.4(8) no C(10) S(10) C(12) C(11) . . . . 1.5(8) no C(11) C(12) S(12) C(14) . . . . -155(3) no C(12) C(11) S(11) C(13) . . . . -177.2(8) no #--------------------------------------------------------------------------- #=========================================================================== # 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 #=========================================================================== #=========================================================================== #(TTM-TTP)GaBr4(PhCl)0.5 #=========================================================================== data_(TTM-TTP)GaBr4(PhCl)0.5 _database_code_CSD 159321 #=========================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #--------------------------------------------------------------------------- _cell_length_a 14.318(4) _cell_length_b 14.507(4) _cell_length_c 8.540(7) _cell_angle_alpha 105.11(4) _cell_angle_beta 93.16(4) _cell_angle_gamma 75.44(2) _cell_volume 1657(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.9 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #--------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 4.050 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1010.58 _chemical_formula_analytical ? _chemical_formula_sum 'C17 H14.50 Br4 Cl0.50 Ga S12 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1952.00 _exptl_absorpt_coefficient_mu 12.947 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.860 _exptl_special_details ; ? ; #=========================================================================== #== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.19 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 0 -2 -2 0 1 -2 0 _diffrn_reflns_number 10241 _reflns_number_total 9637 _reflns_number_gt 2057 _reflns_threshold_expression I>5.00\s(I) _diffrn_reflns_av_R_equivalents 0.03890 _diffrn_reflns_av_sigmaI/netI 0.133 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02669 _diffrn_orient_matrix_UB_12 -0.05745 _diffrn_orient_matrix_UB_13 -0.00020 _diffrn_orient_matrix_UB_21 -0.06588 _diffrn_orient_matrix_UB_22 0.04500 _diffrn_orient_matrix_UB_23 0.02403 _diffrn_orient_matrix_UB_31 -0.01245 _diffrn_orient_matrix_UB_32 -0.01000 _diffrn_orient_matrix_UB_33 -0.11890 #--------------------------------------------------------------------------- #-- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 68 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 58 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 48 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ga 0 4 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br 0 16 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 2 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #=========================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Br(1) 0.6018(2) 0.7514(2) 0.2976(4) 0.087(1) 1.000 . Uani d ? Br(2) 0.8304(2) 0.8271(2) 0.2420(4) 0.101(1) 1.000 . Uani d ? Br(3) 0.7898(2) 0.5877(2) -0.0077(5) 0.124(1) 1.000 . Uani d ? Br(4) 0.8408(3) 0.6190(3) 0.4376(5) 0.135(2) 1.000 . Uani d ? Ga(1) 0.7668(2) 0.6977(2) 0.2442(4) 0.0654(9) 1.000 . Uani d ? Cl(1) 0.368(5) 0.239(5) 0.260(9) 0.55(2) 0.500 S Uiso d ? S(1) 0.1306(4) 0.9503(4) 0.8956(7) 0.064(2) 1.000 . Uani d ? S(2) 0.0303(4) 0.7692(4) 0.8975(8) 0.069(2) 1.000 . Uani d ? S(3) 0.2859(3) 0.7943(3) 0.6875(7) 0.043(2) 1.000 . Uani d ? S(4) 0.1926(3) 0.6360(3) 0.6779(6) 0.040(1) 1.000 . Uani d ? S(5) 0.4444(3) 0.6445(3) 0.4206(6) 0.039(2) 1.000 . Uani d ? S(6) 0.3449(3) 0.4860(3) 0.4111(6) 0.038(1) 1.000 . Uani d ? S(7) 0.5887(3) 0.5022(3) 0.1637(6) 0.038(1) 1.000 . Uani d ? S(8) 0.4884(4) 0.3445(4) 0.1554(6) 0.045(2) 1.000 . Uani d ? S(9) 0.7404(3) 0.3478(3) -0.1001(6) 0.040(2) 1.000 . Uani d ? S(10) 0.6411(3) 0.1942(3) -0.1090(7) 0.047(2) 1.000 . Uani d ? S(11) 0.8894(4) 0.2176(4) -0.3516(7) 0.056(2) 1.000 . Uani d ? S(12) 0.7754(4) 0.0451(4) -0.367(1) 0.087(2) 1.000 . Uani d ? C(1) 0.041(1) 0.991(1) 0.749(2) 0.055(6) 1.000 . Uiso d ? C(2) -0.010(3) 0.665(3) 0.812(5) 0.21(2) 1.000 . Uani d ? C(3) 0.178(1) 0.825(1) 0.798(2) 0.046(6) 1.000 . Uani d ? C(4) 0.134(1) 0.754(1) 0.794(2) 0.045(6) 1.000 . Uani d ? C(5) 0.281(1) 0.668(1) 0.601(2) 0.036(5) 1.000 . Uani d ? C(6) 0.351(1) 0.609(1) 0.496(2) 0.047(6) 1.000 . Uani d ? C(7) 0.485(1) 0.532(1) 0.287(2) 0.029(4) 1.000 . Uiso d ? C(8) 0.440(1) 0.463(1) 0.281(2) 0.031(5) 1.000 . Uani d ? C(9) 0.582(1) 0.374(1) 0.087(2) 0.034(4) 1.000 . Uiso d ? C(10) 0.646(1) 0.313(1) -0.027(2) 0.041(6) 1.000 . Uani d ? C(11) 0.792(1) 0.230(2) -0.234(2) 0.052(7) 1.000 . Uani d ? C(12) 0.738(1) 0.168(1) -0.237(3) 0.053(6) 1.000 . Uani d ? C(13) 0.924(1) 0.331(1) -0.284(3) 0.067(7) 1.000 . Uani d ? C(14) 0.660(4) 0.027(4) -0.431(7) 0.24(2) 1.000 . Uiso d ? C(15) 0.414(4) 0.085(4) 0.053(7) 0.25(2) 1.000 . Uiso d ? C(16) 0.469(3) 0.108(3) 0.252(5) 0.14(1) 1.000 . Uiso d ? C(17) 0.539(3) 0.006(3) 0.118(5) 0.18(2) 1.000 . Uiso d ? H(1) -0.0237 1.0201 0.8083 0.194 1.000 . Uiso c ? H(2) 0.0540 1.0403 0.7109 0.194 1.000 . Uiso c ? H(3) 0.0311 0.9376 0.6656 0.194 1.000 . Uiso c ? H(4) -0.0291 0.6399 0.8777 0.329 1.000 . Uiso c ? H(5) -0.0704 0.6926 0.7433 0.329 1.000 . Uiso c ? H(6) 0.0333 0.6248 0.7260 0.329 1.000 . Uiso c ? H(7) 0.9299 0.3461 -0.1674 0.076 1.000 . Uiso c ? H(8) 0.9842 0.3252 -0.3301 0.076 1.000 . Uiso c ? H(9) 0.8763 0.3820 -0.3117 0.076 1.000 . Uiso c ? H(10) 0.6395 0.0073 -0.3371 1.115 1.000 . Uiso c ? H(11) 0.6296 0.0656 -0.4684 1.115 1.000 . Uiso c ? H(12) 0.6827 -0.0452 -0.5094 1.115 1.000 . Uiso 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) 0.044(1) 0.070(2) 0.141(3) -0.017(1) 0.020(2) 0.006(2) Br(2) 0.064(2) 0.047(1) 0.189(3) -0.023(1) 0.023(2) 0.011(2) Br(3) 0.114(2) 0.089(2) 0.150(3) -0.048(2) 0.054(2) -0.036(2) Br(4) 0.105(3) 0.148(3) 0.185(4) -0.059(2) -0.030(3) 0.082(3) Ga(1) 0.043(1) 0.053(2) 0.097(2) -0.022(1) 0.011(1) 0.002(1) S(1) 0.068(4) 0.047(3) 0.058(4) 0.007(3) 0.008(3) -0.004(3) S(2) 0.051(3) 0.064(4) 0.084(5) -0.007(3) 0.032(3) 0.003(3) S(3) 0.032(3) 0.031(3) 0.063(4) 0.001(2) 0.010(3) 0.013(3) S(4) 0.034(3) 0.038(3) 0.046(3) -0.001(2) 0.011(2) 0.011(3) S(5) 0.038(3) 0.039(3) 0.036(3) -0.008(2) 0.007(2) 0.005(3) S(6) 0.025(2) 0.038(3) 0.048(4) -0.002(2) 0.005(2) 0.009(3) S(7) 0.033(3) 0.033(3) 0.041(3) -0.003(2) 0.009(2) 0.004(2) S(8) 0.045(3) 0.045(3) 0.042(4) -0.017(2) 0.015(3) -0.003(3) S(9) 0.034(3) 0.032(3) 0.047(4) 0.001(2) 0.007(3) 0.006(2) S(10) 0.036(3) 0.031(3) 0.068(4) -0.004(2) 0.010(3) 0.004(3) S(11) 0.047(3) 0.058(4) 0.054(4) -0.005(3) 0.020(3) 0.003(3) S(12) 0.064(4) 0.043(4) 0.130(7) -0.008(3) 0.027(4) -0.021(4) C(2) 0.20(4) 0.22(4) 0.21(4) -0.15(3) 0.16(3) -0.10(3) C(3) 0.04(1) 0.06(1) 0.02(1) 0.01(1) 0.006(9) -0.01(1) C(4) 0.04(1) 0.03(1) 0.07(2) -0.027(9) 0.01(1) 0.01(1) C(5) 0.04(1) 0.03(1) 0.03(1) 0.007(8) 0.013(9) 0.000(8) C(6) 0.05(1) 0.05(1) 0.04(1) -0.02(1) 0.03(1) -0.00(1) C(8) 0.010(8) 0.03(1) 0.04(1) 0.001(7) 0.007(8) 0.005(9) C(10) 0.04(1) 0.05(1) 0.03(1) -0.02(1) 0.01(1) 0.01(1) C(11) 0.06(1) 0.07(2) 0.02(1) -0.01(1) -0.00(1) -0.00(1) C(12) 0.022(9) 0.05(1) 0.08(2) -0.021(9) 0.00(1) -0.01(1) C(13) 0.04(1) 0.04(1) 0.11(2) 0.013(9) 0.04(1) 0.01(1) #=========================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2057 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.1150 _refine_ls_wR_factor_all 0.1520 _refine_ls_wR_factor_ref 0.1520 _refine_ls_goodness_of_fit_all 5.993 _refine_ls_goodness_of_fit_ref 5.990 _refine_ls_shift/su_max 2.6800 _refine_ls_shift/su_mean 0.0560 _refine_diff_density_min -0.99 _refine_diff_density_max 2.37 #=========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Ga(1) 2.325(8) . . ? Br(2) Ga(1) 2.288(8) . . ? Br(3) Ga(1) 2.30(1) . . ? Br(4) Ga(1) 2.31(1) . . ? Cl(1) C(16) 2.1(2) . . ? S(1) C(1) 1.84(5) . . ? S(1) C(3) 1.76(5) . . ? S(2) C(2) 1.72(8) . . ? S(2) C(4) 1.71(4) . . ? S(3) C(3) 1.76(4) . . ? S(3) C(5) 1.80(4) . . ? S(4) C(4) 1.76(4) . . ? S(4) C(5) 1.68(4) . . ? S(5) C(6) 1.75(4) . . ? S(5) C(7) 1.72(4) . . ? S(6) C(6) 1.77(4) . . ? S(6) C(8) 1.71(4) . . ? S(7) C(7) 1.76(4) . . ? S(7) C(9) 1.83(4) . . ? S(8) C(8) 1.76(4) . . ? S(8) C(9) 1.68(4) . . ? S(9) C(10) 1.75(4) . . ? S(9) C(11) 1.79(5) . . ? S(10) C(10) 1.70(5) . . ? S(10) C(12) 1.71(5) . . ? S(11) C(11) 1.72(5) . . ? S(11) C(13) 1.78(5) . . ? S(12) C(12) 1.80(5) . . ? S(12) C(14) 1.8(1) . . ? C(1) H(1) 1.02 . . no C(1) H(2) 0.92 . . no C(1) H(3) 0.94 . . no C(2) H(4) 0.84 . . no C(2) H(5) 1.07 . . no C(2) H(6) 0.95 . . no C(3) C(4) 1.32(6) . . ? C(5) C(6) 1.34(5) . . ? C(7) C(8) 1.31(5) . . ? C(9) C(10) 1.35(5) . . ? C(11) C(12) 1.32(6) . . ? C(13) H(7) 0.96 . . no C(13) H(8) 0.94 . . no C(13) H(9) 0.94 . . no C(14) H(10) 1.00 . . no C(14) H(11) 0.75 . . no C(14) H(12) 1.07 . . no C(15) C(16) 1.8(2) . . ? C(15) C(17) 1.7(1) . . ? C(16) C(17) 1.7(1) . . ? #--------------------------------------------------------------------------- #-- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br(1) Ga(1) Br(2) 110.7(3) . . . ? Br(1) Ga(1) Br(3) 108.0(4) . . . ? Br(1) Ga(1) Br(4) 109.2(4) . . . ? Br(2) Ga(1) Br(3) 108.9(4) . . . ? Br(2) Ga(1) Br(4) 110.7(4) . . . ? Br(3) Ga(1) Br(4) 109.3(4) . . . ? C(1) S(1) C(3) 102(2) . . . ? C(2) S(2) C(4) 105(3) . . . ? C(3) S(3) C(5) 94(2) . . . ? C(4) S(4) C(5) 98(2) . . . ? C(6) S(5) C(7) 94(2) . . . ? C(6) S(6) C(8) 93(2) . . . ? C(7) S(7) C(9) 92(2) . . . ? C(8) S(8) C(9) 96(2) . . . ? C(10) S(9) C(11) 96(2) . . . ? C(10) S(10) C(12) 94(2) . . . ? C(11) S(11) C(13) 106(2) . . . ? C(12) S(12) C(14) 98(5) . . . ? S(1) C(1) H(1) 107.4 . . . no S(1) C(1) H(2) 112.8 . . . no S(1) C(1) H(3) 111.8 . . . no H(1) C(1) H(2) 106.2 . . . no H(1) C(1) H(3) 104.9 . . . no H(2) C(1) H(3) 113.0 . . . no S(2) C(2) H(4) 115.4 . . . no S(2) C(2) H(5) 102.4 . . . no S(2) C(2) H(6) 108.5 . . . no H(4) C(2) H(5) 108.1 . . . no H(4) C(2) H(6) 119.8 . . . no H(5) C(2) H(6) 100.1 . . . no S(1) C(3) S(3) 117(3) . . . ? S(1) C(3) C(4) 125(4) . . . ? S(3) C(3) C(4) 118(3) . . . ? S(2) C(4) S(4) 119(2) . . . ? S(2) C(4) C(3) 125(4) . . . ? S(4) C(4) C(3) 116(3) . . . ? S(3) C(5) S(4) 114(2) . . . ? S(3) C(5) C(6) 119(3) . . . ? S(4) C(5) C(6) 127(3) . . . ? S(5) C(6) S(6) 115(2) . . . ? S(5) C(6) C(5) 126(4) . . . ? S(6) C(6) C(5) 118(3) . . . ? S(5) C(7) S(7) 123(2) . . . ? S(5) C(7) C(8) 119(3) . . . ? S(7) C(7) C(8) 118(3) . . . ? S(6) C(8) S(8) 122(2) . . . ? S(6) C(8) C(7) 119(3) . . . ? S(8) C(8) C(7) 118(3) . . . ? S(7) C(9) S(8) 116(2) . . . ? S(7) C(9) C(10) 119(3) . . . ? S(8) C(9) C(10) 125(3) . . . ? S(9) C(10) S(10) 115(2) . . . ? S(9) C(10) C(9) 124(3) . . . ? S(10) C(10) C(9) 121(3) . . . ? S(9) C(11) S(11) 119(3) . . . ? S(9) C(11) C(12) 111(4) . . . ? S(11) C(11) C(12) 130(4) . . . ? S(10) C(12) S(12) 119(3) . . . ? S(10) C(12) C(11) 123(4) . . . ? S(12) C(12) C(11) 118(4) . . . ? S(11) C(13) H(7) 108.4 . . . no S(11) C(13) H(8) 109.6 . . . no S(11) C(13) H(9) 109.6 . . . no H(7) C(13) H(8) 109.0 . . . no H(7) C(13) H(9) 109.0 . . . no H(8) C(13) H(9) 111.0 . . . no S(12) C(14) H(10) 101.1 . . . no S(12) C(14) H(11) 115.4 . . . no S(12) C(14) H(12) 98.2 . . . no H(10) C(14) H(11) 124.7 . . . no H(10) C(14) H(12) 96.9 . . . no H(11) C(14) H(12) 116.0 . . . no C(16) C(15) C(17) 127(10) . . . ? Cl(1) C(16) C(15) 77(7) . . . ? Cl(1) C(16) C(17) 142(8) . . . ? C(15) C(16) C(17) 69(6) . . . ? C(15) C(17) C(16) 164(10) 2_655 2_655 2_655 ? #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) S(5) 3.38(1) . . no Br(1) H(12) 3.4253 . 1_566 no Br(1) S(7) 3.55(1) . . no Br(1) S(10) 3.74(1) . 2_665 no Br(1) Cl(1) 3.7(2) . 2_666 no Br(1) C(16) 3.91(9) . 2_666 no Br(1) C(7) 3.93(4) . . no Br(1) S(8) 4.01(2) . 2_665 no Br(2) H(2) 2.7793 . 2_676 no Br(2) H(12) 2.9811 . 1_566 no Br(2) H(8) 3.1929 . 2_765 no Br(2) C(1) 3.56(5) . 2_676 no Br(2) C(13) 3.74(5) . 2_765 no Br(2) S(1) 3.88(2) . 2_676 no Br(2) C(14) 3.9(1) . 1_566 no Br(2) S(12) 3.91(2) . 1_566 no Br(2) S(2) 4.00(1) . 1_654 no Br(2) S(11) 4.00(1) . 2_765 no Br(3) H(4) 3.1471 . 1_654 no Br(3) H(9) 3.4113 . . no Br(3) S(9) 3.60(1) . . no Br(3) C(2) 3.86(7) . 1_654 no Br(3) S(6) 3.89(2) . 2_665 no Br(3) S(7) 3.90(1) . . no Br(3) C(13) 3.93(5) . . no Br(3) Cl(1) 3.9(2) . 2_665 no Br(3) C(8) 4.03(4) . 2_665 no Br(3) S(8) 4.07(2) . 2_665 no Br(4) H(5) 2.9049 . 1_655 no Br(4) H(8) 3.0723 . 2_765 no Br(4) S(4) 3.72(1) . 2_666 no Br(4) C(2) 3.8(1) . 1_655 no Br(4) S(6) 3.81(1) . 2_666 no Br(4) Cl(1) 3.8(2) . 2_666 no Br(4) C(13) 3.97(5) . 2_765 no Cl(1) S(8) 2.9(2) . . no Cl(1) S(6) 3.4(2) . . no Cl(1) C(8) 3.6(2) . . no Cl(1) S(5) 4.1(2) . 2_666 no S(1) H(1) 2.9072 . 2_577 no S(1) C(1) 3.79(5) . 2_577 no S(1) C(12) 3.92(6) . 2_666 no S(1) S(1) 3.99(3) . 2_577 no S(1) S(10) 4.04(2) . 2_666 no S(2) H(7) 3.1339 . 2_666 no S(2) H(1) 3.3965 . 2_577 no S(2) C(11) 3.73(5) . 2_666 no S(2) S(9) 3.84(2) . 2_666 no S(2) C(13) 3.90(6) . 2_666 no S(2) C(1) 3.92(5) . 2_577 no S(2) S(11) 3.95(2) . 2_666 no S(3) C(9) 3.60(5) . 2_666 no S(3) C(10) 3.62(5) . 2_666 no S(3) S(10) 3.67(2) . 2_666 no S(3) S(11) 3.71(2) . 2_665 no S(3) S(8) 3.74(2) . 2_666 no S(3) C(11) 3.92(5) . 2_665 no S(3) S(12) 3.96(2) . 2_665 no S(3) C(12) 4.01(6) . 2_665 no S(3) C(14) 4.0(1) . 2_665 no S(3) C(16) 4.06(9) . 2_666 no S(4) H(9) 3.1915 . 2_665 no S(4) S(9) 3.64(2) . 2_666 no S(4) S(7) 3.67(2) . 2_666 no S(4) C(9) 3.70(4) . 2_666 no S(4) C(10) 3.70(5) . 2_666 no S(4) C(13) 3.76(6) . 2_665 no S(4) S(11) 3.89(2) . 2_665 no S(5) C(8) 3.46(5) . 2_666 no S(5) S(6) 3.58(2) . 2_666 no S(5) S(8) 3.67(2) . 2_666 no S(5) C(10) 3.68(5) . 2_665 no S(5) S(9) 3.70(2) . 2_665 no S(5) C(12) 3.86(5) . 2_665 no S(5) C(11) 3.89(5) . 2_665 no S(5) S(10) 3.94(2) . 2_665 no S(5) C(7) 3.95(5) . 2_666 no S(6) H(9) 3.4534 . 2_665 no S(6) C(7) 3.47(4) . 2_666 no S(6) S(7) 3.67(2) . 2_666 no S(6) S(9) 3.98(2) . 2_665 no S(6) C(8) 4.03(4) . 2_666 no S(7) C(9) 3.61(5) . 2_665 no S(7) C(6) 3.64(5) . 2_666 no S(7) C(5) 3.67(5) . 2_666 no S(7) S(7) 3.67(3) . 2_665 no S(7) C(7) 3.87(5) . 2_665 no S(7) S(8) 3.90(2) . 2_665 no S(7) C(8) 3.95(5) . 2_665 no S(7) C(10) 4.06(5) . 2_665 no S(8) C(6) 3.69(5) . 2_666 no S(8) C(5) 3.79(5) . 2_666 no S(8) C(16) 3.81(9) . . no S(8) C(15) 4.0(1) . . no S(9) C(4) 3.52(5) . 2_666 no S(9) C(6) 3.70(5) . 2_665 no S(9) C(7) 3.75(4) . 2_665 no S(9) C(8) 3.85(4) . 2_665 no S(9) C(3) 3.98(5) . 2_666 no S(10) C(3) 3.62(5) . 2_666 no S(11) H(3) 3.0750 . 2_665 no S(11) H(2) 3.1591 . 1_644 no S(11) H(1) 3.4177 . 1_644 no S(11) C(5) 3.54(5) . 2_665 no S(11) C(1) 3.73(5) . 1_644 no S(11) C(3) 3.81(5) . 2_665 no S(11) C(4) 3.89(5) . 2_665 no S(11) C(1) 3.89(5) . 2_665 no S(11) C(6) 4.06(5) . 2_665 no S(12) H(1) 3.1515 . 1_644 no S(12) C(1) 3.81(5) . 1_644 no C(2) H(7) 3.2164 . 2_666 no C(3) C(10) 3.63(7) . 2_666 no C(3) C(12) 3.86(7) . 2_666 no C(3) C(11) 3.98(7) . 2_666 no C(4) C(10) 3.69(7) . 2_666 no C(4) C(11) 3.81(7) . 2_666 no C(5) C(9) 3.31(6) . 2_666 no C(5) H(9) 3.3175 . 2_665 no C(5) C(10) 3.69(7) . 2_666 no C(5) C(11) 3.80(7) . 2_665 no C(5) C(13) 3.89(7) . 2_665 no C(6) C(7) 3.50(7) . 2_666 no C(6) C(8) 3.54(7) . 2_666 no C(6) C(9) 3.60(7) . 2_666 no C(6) C(11) 3.80(7) . 2_665 no C(7) C(10) 3.67(6) . 2_665 no C(7) C(9) 3.77(6) . 2_665 no C(7) C(8) 3.78(6) . 2_666 no C(7) C(7) 3.96(9) . 2_666 no C(8) C(8) 4.03(9) . 2_666 no C(14) C(16) 3.6(2) . 2_655 no C(14) C(16) 3.9(2) . 1_554 no C(15) H(10) 3.2634 . 2_655 no C(16) H(10) 2.7944 . 2_655 no C(16) H(11) 3.2884 . 1_556 no C(17) H(10) 3.3257 . 2_655 no H(4) H(7) 2.7709 . 2_666 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl(1) C(16) C(15) C(17) . . . . 161(12) no Cl(1) C(16) C(17) C(15) . . . . -18(41) no S(1) C(3) S(3) C(5) . . . . -172(3) no S(1) C(3) C(4) S(2) . . . . -7(7) no S(1) C(3) C(4) S(4) . . . . 176(3) no S(2) C(4) S(4) C(5) . . . . 177(3) no S(2) C(4) C(3) S(3) . . . . 178(3) no S(3) C(3) S(1) C(1) . . . . 97(3) no S(3) C(3) C(4) S(4) . . . . 1(6) no S(3) C(5) S(4) C(4) . . . . 8(3) no S(3) C(5) C(6) S(5) . . . . -5(7) no S(3) C(5) C(6) S(6) . . . . -180(3) no S(4) C(4) S(2) C(2) . . . . -17(6) no S(4) C(5) S(3) C(3) . . . . -7(3) no S(4) C(5) C(6) S(5) . . . . -179(3) no S(4) C(5) C(6) S(6) . . . . 6(7) no S(5) C(6) S(6) C(8) . . . . -2(3) no S(5) C(7) S(7) C(9) . . . . 174(3) no S(5) C(7) C(8) S(6) . . . . -2(5) no S(5) C(7) C(8) S(8) . . . . -175(3) no S(6) C(6) S(5) C(7) . . . . 1(3) no S(6) C(8) S(8) C(9) . . . . -173(3) no S(6) C(8) C(7) S(7) . . . . 174(2) no S(7) C(7) S(5) C(6) . . . . -176(3) no S(7) C(7) C(8) S(8) . . . . 2(5) no S(7) C(9) S(8) C(8) . . . . -1(3) no S(7) C(9) C(10) S(9) . . . . 3(6) no S(7) C(9) C(10) S(10) . . . . -178(3) no S(8) C(8) S(6) C(6) . . . . 175(3) no S(8) C(9) S(7) C(7) . . . . 2(3) no S(8) C(9) C(10) S(9) . . . . 178(3) no S(8) C(9) C(10) S(10) . . . . -3(6) no S(9) C(10) S(10) C(12) . . . . -2(3) no S(9) C(11) S(11) C(13) . . . . 8(4) no S(9) C(11) C(12) S(10) . . . . -8(6) no S(9) C(11) C(12) S(12) . . . . 179(3) no S(10) C(10) S(9) C(11) . . . . -1(3) no S(10) C(12) S(12) C(14) . . . . 44(6) no S(10) C(12) C(11) S(11) . . . . -179(3) no S(11) C(11) S(9) C(10) . . . . 178(3) no S(11) C(11) C(12) S(12) . . . . 8(8) no S(12) C(12) S(10) C(10) . . . . 179(3) no C(1) S(1) C(3) C(4) . . . . -78(5) no C(2) S(2) C(4) C(3) . . . . 166(7) no C(3) S(3) C(5) C(6) . . . . 178(4) no C(3) C(4) S(4) C(5) . . . . -6(5) no C(4) S(4) C(5) C(6) . . . . -178(5) no C(4) C(3) S(3) C(5) . . . . 4(5) no C(5) C(6) S(5) C(7) . . . . -174(5) no C(5) C(6) S(6) C(8) . . . . 173(4) no C(6) S(5) C(7) C(8) . . . . 0(4) no C(6) S(6) C(8) C(7) . . . . 3(4) no C(7) S(7) C(9) C(10) . . . . 176(4) no C(7) C(8) S(8) C(9) . . . . -1(4) no C(8) S(8) C(9) C(10) . . . . -175(4) no C(8) C(7) S(7) C(9) . . . . -2(4) no C(9) C(10) S(9) C(11) . . . . 178(4) no C(9) C(10) S(10) C(12) . . . . 179(4) no C(10) S(9) C(11) C(12) . . . . 5(4) no C(10) S(10) C(12) C(11) . . . . 6(5) no C(11) C(12) S(12) C(14) . . . . -143(6) no C(12) C(11) S(11) C(13) . . . . 178(5) no #--------------------------------------------------------------------------- #-- #=========================================================================== # 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 #=========================================================================== #=========================================================================== #(TTM-TTP)GaCl2.0Br2.0(PhCl)0.5 #=========================================================================== data_(TTM-TTP)GaCl2Br2(PhCl)0.5 _database_code_CSD 159322 #=========================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1997) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #--------------------------------------------------------------------------- #-- _cell_length_a 14.136(2) _cell_length_b 14.361(3) _cell_length_c 8.571(1) _cell_angle_alpha 105.88(1) _cell_angle_beta 93.89(1) _cell_angle_gamma 76.65(1) _cell_volume 1628.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.6 _cell_measurement_theta_max 14.8 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #--------------------------------------------------------------------------- #-- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 921.68 _chemical_formula_analytical ? _chemical_formula_sum 'C17 H14.50 Br2 Cl2.50 Ga S12 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 904.00 _exptl_absorpt_coefficient_mu 4.291 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.291 _exptl_special_details ; ? ; #=========================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -7.47 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 1 -2 -1 2 -2 1 0 -1 _diffrn_reflns_number 10082 _reflns_number_total 9491 _reflns_number_gt 2421 _reflns_threshold_expression I>5.00\s(I) _diffrn_reflns_av_R_equivalents 0.07808 _diffrn_reflns_av_sigmaI/netI 0.112 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00044 _diffrn_orient_matrix_UB_12 0.00969 _diffrn_orient_matrix_UB_13 -0.11111 _diffrn_orient_matrix_UB_21 0.04246 _diffrn_orient_matrix_UB_22 0.04860 _diffrn_orient_matrix_UB_23 0.04024 _diffrn_orient_matrix_UB_31 0.05902 _diffrn_orient_matrix_UB_32 -0.05528 _diffrn_orient_matrix_UB_33 -0.02738 #--------------------------------------------------------------------------- #-- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 34 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 24 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 29 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ga 0 2 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 5 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br 0 4 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #=========================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Br(1) 0.60298(8) 0.7535(1) 0.2994(2) 0.0849(5) 0.831(3) S Uani d ? Br(2) 0.8302(1) 0.8295(1) 0.2461(3) 0.1187(7) 0.732(3) S Uani d ? Br(3) 0.7891(1) 0.5911(1) 0.0047(3) 0.1278(7) 0.711(3) S Uani d ? Br(4) 0.8371(2) 0.6287(2) 0.4404(3) 0.1281(9) 0.647(3) S Uani d ? Ga(1) 0.76509(7) 0.70241(8) 0.2462(1) 0.0661(3) 1.000 . Uani d ? Cl(1) 0.354(2) 0.159(2) 0.182(4) 0.55(2) 0.500 S Uiso d ? S(1) 0.1306(2) 0.9477(2) 0.8963(3) 0.0688(8) 1.000 . Uani d ? S(2) 0.0267(2) 0.7622(2) 0.8898(3) 0.0687(8) 1.000 . Uani d ? S(3) 0.2847(1) 0.7944(1) 0.6877(3) 0.0426(6) 1.000 . Uani d ? S(4) 0.1911(1) 0.6303(2) 0.6718(2) 0.0410(5) 1.000 . Uani d ? S(5) 0.4435(1) 0.6468(1) 0.4217(2) 0.0358(5) 1.000 . Uani d ? S(6) 0.3423(1) 0.4836(1) 0.4066(2) 0.0381(5) 1.000 . Uani d ? S(7) 0.5891(1) 0.5036(1) 0.1669(2) 0.0354(5) 1.000 . Uani d ? S(8) 0.4863(1) 0.3425(1) 0.1535(2) 0.0387(5) 1.000 . Uani d ? S(9) 0.7421(1) 0.3509(1) -0.0942(2) 0.0382(5) 1.000 . Uani d ? S(10) 0.6415(1) 0.1919(2) -0.1102(3) 0.0465(6) 1.000 . Uani d ? S(11) 0.8900(1) 0.2217(2) -0.3460(3) 0.0519(6) 1.000 . Uani d ? S(12) 0.7735(2) 0.0452(2) -0.3702(4) 0.0818(9) 1.000 . Uani d ? C(1) 0.0456(7) 0.9861(7) 0.749(1) 0.071(3) 1.000 . Uani d ? C(2) -0.0094(8) 0.655(1) 0.804(2) 0.150(5) 1.000 . Uani d ? C(3) 0.1752(6) 0.8247(6) 0.7914(9) 0.047(2) 1.000 . Uani d ? C(4) 0.1317(5) 0.7510(6) 0.7861(9) 0.043(2) 1.000 . Uani d ? C(5) 0.2830(5) 0.6703(5) 0.6037(8) 0.033(2) 1.000 . Uani d ? C(6) 0.3498(5) 0.6075(5) 0.4914(8) 0.033(2) 1.000 . Uani d ? C(7) 0.4855(5) 0.5315(5) 0.2826(8) 0.033(2) 1.000 . Uani d ? C(8) 0.4389(5) 0.4587(5) 0.2784(8) 0.033(2) 1.000 . Uani d ? C(9) 0.5806(5) 0.3783(5) 0.0857(8) 0.031(2) 1.000 . Uani d ? C(10) 0.6465(5) 0.3133(5) -0.0261(8) 0.032(2) 1.000 . Uani d ? C(11) 0.7876(5) 0.2320(6) -0.2290(8) 0.040(2) 1.000 . Uani d ? C(12) 0.7423(5) 0.1625(6) -0.236(1) 0.045(2) 1.000 . Uani d ? C(13) 0.9228(6) 0.3401(7) -0.274(1) 0.059(3) 1.000 . Uani d ? C(14) 0.694(2) 0.003(1) -0.399(3) 0.56(1) 1.000 . Uani d ? C(15) 0.424(2) 0.061(2) 0.014(3) 0.211(9) 1.000 . Uiso d ? C(16) 0.476(1) 0.097(1) 0.231(2) 0.151(6) 1.000 . Uiso d ? C(17) 0.540(1) 0.014(2) 0.126(2) 0.187(8) 1.000 . Uiso d ? H(1) -0.0168 1.0174 0.7881 0.093 1.000 . Uiso c ? H(2) 0.0723 1.0316 0.7049 0.093 1.000 . Uiso c ? H(3) 0.0383 0.9294 0.6536 0.093 1.000 . Uiso c ? H(4) -0.0229 0.6034 0.8718 0.137 1.000 . Uiso c ? H(5) -0.0732 0.6397 0.7259 0.137 1.000 . Uiso c ? H(6) 0.0373 0.5888 0.7195 0.137 1.000 . Uiso c ? H(7) 0.9319 0.3650 -0.1464 0.077 1.000 . Uiso c ? H(8) 0.9871 0.3462 -0.3054 0.077 1.000 . Uiso c ? H(9) 0.8764 0.3965 -0.2931 0.077 1.000 . Uiso c ? H(10) 0.6653 -0.0064 -0.3103 0.809 1.000 . Uiso c ? H(11) 0.6356 0.0460 -0.4470 0.809 1.000 . Uiso c ? H(12) 0.7007 -0.0602 -0.4858 0.809 1.000 . Uiso 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) 0.0431(6) 0.0798(9) 0.125(1) -0.0141(6) 0.0202(7) 0.0110(8) Br(2) 0.086(1) 0.066(1) 0.202(2) -0.0278(8) 0.037(1) 0.013(1) Br(3) 0.122(1) 0.098(1) 0.142(2) -0.049(1) 0.068(1) -0.038(1) Br(4) 0.089(1) 0.163(2) 0.169(2) -0.043(1) -0.024(1) 0.098(1) Ga(1) 0.0406(5) 0.0600(6) 0.0913(8) -0.0138(5) 0.0142(5) 0.0037(6) S(1) 0.080(2) 0.049(1) 0.054(1) 0.019(1) 0.014(1) 0.000(1) S(2) 0.041(1) 0.089(2) 0.069(2) 0.011(1) 0.029(1) 0.023(1) S(3) 0.038(1) 0.039(1) 0.048(1) 0.0023(9) 0.0107(9) 0.0138(9) S(4) 0.033(1) 0.043(1) 0.044(1) 0.0012(9) 0.0127(9) 0.0124(9) S(5) 0.0314(9) 0.037(1) 0.036(1) 0.0021(8) 0.0106(8) 0.0092(8) S(6) 0.0313(9) 0.042(1) 0.040(1) -0.0031(8) 0.0111(8) 0.0097(9) S(7) 0.0318(9) 0.033(1) 0.040(1) 0.0016(8) 0.0116(8) 0.0115(8) S(8) 0.0322(9) 0.034(1) 0.047(1) -0.0031(8) 0.0114(9) 0.0054(9) S(9) 0.033(1) 0.038(1) 0.039(1) -0.0002(9) 0.0093(8) 0.0071(9) S(10) 0.034(1) 0.039(1) 0.060(1) -0.0024(9) 0.011(1) 0.005(1) S(11) 0.039(1) 0.058(1) 0.049(1) 0.006(1) 0.018(1) 0.009(1) S(12) 0.067(2) 0.041(1) 0.112(2) -0.000(1) 0.032(1) -0.019(1) C(1) 0.067(6) 0.056(6) 0.078(7) 0.021(5) 0.013(5) 0.024(5) C(2) 0.090(7) 0.24(2) 0.11(1) -0.089(8) 0.047(7) -0.03(1) C(3) 0.038(4) 0.047(5) 0.043(5) 0.011(4) 0.010(4) 0.008(4) C(4) 0.023(4) 0.059(5) 0.044(5) 0.005(4) 0.007(3) 0.017(4) C(5) 0.028(4) 0.036(4) 0.032(4) 0.001(3) 0.004(3) 0.008(3) C(6) 0.022(3) 0.038(4) 0.034(4) 0.004(3) 0.001(3) 0.009(3) C(7) 0.041(4) 0.017(4) 0.035(4) 0.007(3) 0.012(3) 0.007(3) C(8) 0.028(4) 0.037(4) 0.030(4) 0.008(3) 0.008(3) 0.015(3) C(9) 0.021(3) 0.040(4) 0.033(4) 0.001(3) -0.000(3) 0.017(3) C(10) 0.030(4) 0.029(4) 0.031(4) 0.000(3) 0.003(3) 0.006(3) C(11) 0.031(4) 0.058(5) 0.023(4) 0.013(4) -0.001(3) 0.014(4) C(12) 0.029(4) 0.042(5) 0.061(5) -0.004(3) 0.008(4) 0.009(4) C(13) 0.038(4) 0.074(6) 0.069(6) -0.016(4) 0.015(4) 0.018(5) C(14) 0.61(2) 0.26(1) 0.71(3) -0.35(1) 0.56(2) -0.36(2) #=========================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2421 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_all 0.0930 _refine_ls_wR_factor_ref 0.0930 _refine_ls_goodness_of_fit_all 5.095 _refine_ls_goodness_of_fit_ref 5.100 _refine_ls_shift/su_max 4.2500 _refine_ls_shift/su_mean 0.0866 _refine_diff_density_min -0.99 _refine_diff_density_max 1.43 #=========================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Ga(1) 2.276(3) . . ? Br(2) Ga(1) 2.226(5) . . ? Br(3) Ga(1) 2.234(5) . . ? Br(4) Ga(1) 2.272(6) . . ? Cl(1) C(16) 1.82(7) . . ? S(1) C(1) 1.79(2) . . ? S(1) C(3) 1.74(2) . . ? S(2) C(2) 1.69(3) . . ? S(2) C(4) 1.74(2) . . ? S(3) C(3) 1.74(2) . . ? S(3) C(5) 1.74(2) . . ? S(4) C(4) 1.78(2) . . ? S(4) C(5) 1.73(2) . . ? S(5) C(6) 1.75(2) . . ? S(5) C(7) 1.75(1) . . ? S(6) C(6) 1.75(2) . . ? S(6) C(8) 1.72(2) . . ? S(7) C(7) 1.73(2) . . ? S(7) C(9) 1.77(2) . . ? S(8) C(8) 1.73(2) . . ? S(8) C(9) 1.72(2) . . ? S(9) C(10) 1.75(2) . . ? S(9) C(11) 1.78(2) . . ? S(10) C(10) 1.71(2) . . ? S(10) C(12) 1.75(2) . . ? S(11) C(11) 1.77(2) . . ? S(11) C(13) 1.80(2) . . ? S(12) C(12) 1.74(2) . . ? S(12) C(14) 1.38(5) . . ? C(1) H(1) 0.93 . . no C(1) H(2) 0.99 . . no C(1) H(3) 1.00 . . no C(2) H(4) 1.11 . . no C(2) H(5) 1.11 . . no C(2) H(6) 1.12 . . no C(3) C(4) 1.33(2) . . ? C(5) C(6) 1.37(2) . . ? C(7) C(8) 1.35(2) . . ? C(9) C(10) 1.37(2) . . ? C(11) C(12) 1.29(2) . . ? C(13) H(7) 1.06 . . no C(13) H(8) 1.00 . . no C(13) H(9) 0.96 . . no C(14) H(10) 0.94 . . no C(14) H(11) 1.04 . . no C(14) H(12) 0.99 . . no C(15) C(16) 1.94(6) . . ? C(15) C(17) 1.41(5) . . ? C(16) C(17) 1.44(5) . . ? #--------------------------------------------------------------------------- #-- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br(1) Ga(1) Br(2) 111.3(2) . . . ? Br(1) Ga(1) Br(3) 109.7(2) . . . ? Br(1) Ga(1) Br(4) 107.9(2) . . . ? Br(2) Ga(1) Br(3) 109.2(2) . . . ? Br(2) Ga(1) Br(4) 110.0(2) . . . ? Br(3) Ga(1) Br(4) 108.8(2) . . . ? C(1) S(1) C(3) 99.6(9) . . . ? C(2) S(2) C(4) 104(1) . . . ? C(3) S(3) C(5) 95.6(8) . . . ? C(4) S(4) C(5) 94.8(8) . . . ? C(6) S(5) C(7) 93.4(8) . . . ? C(6) S(6) C(8) 93.6(8) . . . ? C(7) S(7) C(9) 92.5(7) . . . ? C(8) S(8) C(9) 94.4(8) . . . ? C(10) S(9) C(11) 93.6(8) . . . ? C(10) S(10) C(12) 96.0(8) . . . ? C(11) S(11) C(13) 104.8(8) . . . ? C(12) S(12) C(14) 109(2) . . . ? S(1) C(1) H(1) 114.6 . . . no S(1) C(1) H(2) 107.5 . . . no S(1) C(1) H(3) 112.4 . . . no H(1) C(1) H(2) 109.3 . . . no H(1) C(1) H(3) 106.5 . . . no H(2) C(1) H(3) 106.1 . . . no S(2) C(2) H(4) 125.0 . . . no S(2) C(2) H(5) 131.1 . . . no S(2) C(2) H(6) 123.4 . . . no H(4) C(2) H(5) 88.4 . . . no H(4) C(2) H(6) 87.6 . . . no H(5) C(2) H(6) 88.4 . . . no S(1) C(3) S(3) 118(1) . . . ? S(1) C(3) C(4) 124(1) . . . ? S(3) C(3) C(4) 117(1) . . . ? S(2) C(4) S(4) 118(1) . . . ? S(2) C(4) C(3) 125(1) . . . ? S(4) C(4) C(3) 117(1) . . . ? S(3) C(5) S(4) 115.3(8) . . . ? S(3) C(5) C(6) 123(1) . . . ? S(4) C(5) C(6) 122(1) . . . ? S(5) C(6) S(6) 116.8(8) . . . ? S(5) C(6) C(5) 122(1) . . . ? S(6) C(6) C(5) 121(1) . . . ? S(5) C(7) S(7) 124(1) . . . ? S(5) C(7) C(8) 117(1) . . . ? S(7) C(7) C(8) 119(1) . . . ? S(6) C(8) S(8) 124(1) . . . ? S(6) C(8) C(7) 119(1) . . . ? S(8) C(8) C(7) 117(1) . . . ? S(7) C(9) S(8) 116.9(8) . . . ? S(7) C(9) C(10) 121(1) . . . ? S(8) C(9) C(10) 122(1) . . . ? S(9) C(10) S(10) 115.2(8) . . . ? S(9) C(10) C(9) 121(1) . . . ? S(10) C(10) C(9) 123(1) . . . ? S(9) C(11) S(11) 116(1) . . . ? S(9) C(11) C(12) 118(1) . . . ? S(11) C(11) C(12) 126(1) . . . ? S(10) C(12) S(12) 120(1) . . . ? S(10) C(12) C(11) 117(1) . . . ? S(12) C(12) C(11) 123(1) . . . ? S(11) C(13) H(7) 115.7 . . . no S(11) C(13) H(8) 118.4 . . . no S(11) C(13) H(9) 116.4 . . . no H(7) C(13) H(8) 97.5 . . . no H(7) C(13) H(9) 100.3 . . . no H(8) C(13) H(9) 105.7 . . . no S(12) C(14) H(10) 118.0 . . . no S(12) C(14) H(11) 111.9 . . . no S(12) C(14) H(12) 116.1 . . . no H(10) C(14) H(11) 102.6 . . . no H(10) C(14) H(12) 106.7 . . . no H(11) C(14) H(12) 99.2 . . . no C(16) C(15) C(17) 132(4) . . . ? Cl(1) C(16) C(15) 59(3) . . . ? Cl(1) C(16) C(17) 127(4) . . . ? C(15) C(16) C(17) 68(3) . . . ? C(15) C(17) C(16) 160(5) 2_655 2_655 2_655 ? #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) S(5) 3.365(5) . . no Br(1) S(7) 3.503(5) . . no Br(2) H(2) 2.6044 . 2_676 no Br(2) H(12) 2.8948 . 1_566 no Br(2) C(1) 3.49(2) . 2_676 no Br(3) H(4) 3.0210 . 1_654 no Br(3) S(9) 3.527(6) . . no Br(4) H(5) 2.6612 . 1_655 no Br(4) H(8) 2.9456 . 2_765 no Cl(1) H(10) 2.7790 . 2_655 no Cl(1) C(14) 3.55(9) . 2_655 no S(5) C(8) 3.47(2) . 2_666 no S(6) C(7) 3.50(2) . 2_666 no S(7) C(9) 3.57(2) . 2_665 no S(9) C(4) 3.54(2) . 2_666 no S(11) H(3) 2.9833 . 2_665 no S(11) C(5) 3.56(2) . 2_665 no C(5) C(9) 3.32(2) . 2_666 no C(6) C(7) 3.54(2) . 2_666 no C(6) C(8) 3.55(2) . 2_666 no C(16) H(10) 2.8344 . 2_655 no H(4) H(7) 2.5839 . 2_666 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl(1) C(16) C(15) C(17) . . . . -175(7) no Cl(1) C(16) C(17) C(15) . . . . 4(17) no S(1) C(3) S(3) C(5) . . . . -176(1) no S(1) C(3) C(4) S(2) . . . . -3(3) no S(1) C(3) C(4) S(4) . . . . -180(1) no S(2) C(4) S(4) C(5) . . . . 180(1) no S(2) C(4) C(3) S(3) . . . . 176(1) no S(3) C(3) S(1) C(1) . . . . 98(1) no S(3) C(3) C(4) S(4) . . . . -0(2) no S(3) C(5) S(4) C(4) . . . . 7(1) no S(3) C(5) C(6) S(5) . . . . -0(2) no S(3) C(5) C(6) S(6) . . . . -178.2(9) no S(4) C(4) S(2) C(2) . . . . -17(2) no S(4) C(5) S(3) C(3) . . . . -7(1) no S(4) C(5) C(6) S(5) . . . . -179.8(9) no S(4) C(5) C(6) S(6) . . . . 2(2) no S(5) C(6) S(6) C(8) . . . . -2(1) no S(5) C(7) S(7) C(9) . . . . 175(1) no S(5) C(7) C(8) S(6) . . . . 1(2) no S(5) C(7) C(8) S(8) . . . . -174.9(9) no S(6) C(6) S(5) C(7) . . . . 2(1) no S(6) C(8) S(8) C(9) . . . . -175(1) no S(6) C(8) C(7) S(7) . . . . 174.4(9) no S(7) C(7) S(5) C(6) . . . . -175(1) no S(7) C(7) C(8) S(8) . . . . -1(2) no S(7) C(9) S(8) C(8) . . . . 1(1) no S(7) C(9) C(10) S(9) . . . . -0(2) no S(7) C(9) C(10) S(10) . . . . -179.4(9) no S(8) C(8) S(6) C(6) . . . . 176(1) no S(8) C(9) S(7) C(7) . . . . -2(1) no S(8) C(9) C(10) S(9) . . . . 180.0(9) no S(8) C(9) C(10) S(10) . . . . 1(2) no S(9) C(10) S(10) C(12) . . . . -1(1) no S(9) C(11) S(11) C(13) . . . . 5(1) no S(9) C(11) C(12) S(10) . . . . -1(2) no S(9) C(11) C(12) S(12) . . . . 176(1) no S(10) C(10) S(9) C(11) . . . . 0(1) no S(10) C(12) S(12) C(14) . . . . 21(4) no S(10) C(12) C(11) S(11) . . . . -179(1) no S(11) C(11) S(9) C(10) . . . . 178(1) no S(11) C(11) C(12) S(12) . . . . -2(3) no S(12) C(12) S(10) C(10) . . . . -176(1) no C(1) S(1) C(3) C(4) . . . . -83(2) no C(2) S(2) C(4) C(3) . . . . 167(2) no C(3) S(3) C(5) C(6) . . . . 173(2) no C(3) C(4) S(4) C(5) . . . . -4(2) no C(4) S(4) C(5) C(6) . . . . -173(1) no C(4) C(3) S(3) C(5) . . . . 4(2) no C(5) C(6) S(5) C(7) . . . . -176(2) no C(5) C(6) S(6) C(8) . . . . 177(1) no C(6) S(5) C(7) C(8) . . . . -1(1) no C(6) S(6) C(8) C(7) . . . . 1(1) no C(7) S(7) C(9) C(10) . . . . 178(1) no C(7) C(8) S(8) C(9) . . . . -0(1) no C(8) S(8) C(9) C(10) . . . . -179(1) no C(8) C(7) S(7) C(9) . . . . 2(1) no C(9) C(10) S(9) C(11) . . . . -179(1) no C(9) C(10) S(10) C(12) . . . . 179(2) no C(10) S(9) C(11) C(12) . . . . 0(2) no C(10) S(10) C(12) C(11) . . . . 1(2) no C(11) C(12) S(12) C(14) . . . . -155(4) no C(12) C(11) S(11) C(13) . . . . -177(2) no #--------------------------------------------------------------------------- #=========================================================================== # 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 #=========================================================================== #=========================================================================== #(TTM-TTP)FeGaCl4 #========================================================================= data_(TTM-TTP)Fe0.9Ga0.1Cl4 _database_code_CSD 159323 #=========================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1997) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #--------------------------------------------------------------------------- #-- _cell_length_a 24.021(7) _cell_length_b 5.850(2) _cell_length_c 22.435(7) _cell_angle_alpha 90 _cell_angle_beta 118.77(2) _cell_angle_gamma 90 _cell_volume 2764(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.5 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, -y, -z' ' +x, -y,1/2+z' '1/2+x,1/2+y, +z' '1/2-x,1/2+y,1/2-z' '1/2-x,1/2-y, -z' '1/2+x,1/2-y,1/2+z' #--------------------------------------------------------------------------- _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 764.02 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H12 Cl4 Fe0.90 Ga0.10 S12 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1530.00 _exptl_absorpt_coefficient_mu 1.890 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.920 _exptl_special_details ; ? ; #=========================================================================== #== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.25 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 1 -4 -4 0 -4 -2 0 -2 _diffrn_reflns_number 4511 _reflns_number_total 4409 _reflns_number_gt 1510 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04397 _diffrn_reflns_av_sigmaI/netI 0.178 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01218 _diffrn_orient_matrix_UB_12 -0.01174 _diffrn_orient_matrix_UB_13 -0.04925 _diffrn_orient_matrix_UB_21 -0.04556 _diffrn_orient_matrix_UB_22 -0.01772 _diffrn_orient_matrix_UB_23 -0.01177 _diffrn_orient_matrix_UB_31 -0.00560 _diffrn_orient_matrix_UB_32 0.16961 _diffrn_orient_matrix_UB_33 -0.00464 #--------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 56 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 48 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ga 0 0 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 3 0.301 0.845 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #=========================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Fe(1) 0.5000 0.5179(3) 0.2500 0.0433(5) 0.502(7) S Uani d ? Cl(1) 0.5094(1) 0.3058(6) 0.3333(1) 0.082(1) 1.000 . Uani d ? Cl(2) 0.5858(2) 0.7275(6) 0.2862(2) 0.093(1) 1.000 . Uani d ? S(1) 0.3299(1) -0.3175(5) -0.1640(1) 0.0561(8) 1.000 . Uani d ? S(2) 0.4474(1) -0.3168(4) -0.0062(1) 0.0495(7) 1.000 . Uani d ? S(3) 0.2803(1) 0.0923(4) -0.1238(1) 0.0398(6) 1.000 . Uani d ? S(4) 0.38580(9) 0.0971(4) 0.0156(1) 0.0371(6) 1.000 . Uani d ? S(5) 0.22030(9) 0.5398(4) -0.08740(9) 0.0340(5) 1.000 . Uani d ? S(6) 0.33017(9) 0.5319(4) 0.05246(9) 0.0343(5) 1.000 . Uani d ? C(1) 0.3469(5) -0.145(2) -0.2189(5) 0.067(4) 1.000 . Uani d ? C(2) 0.5013(4) -0.209(2) 0.0765(5) 0.050(3) 1.000 . Uani d ? C(3) 0.3386(4) -0.116(1) -0.1028(4) 0.035(2) 1.000 . Uani d ? C(4) 0.3868(4) -0.115(1) -0.0380(4) 0.032(2) 1.000 . Uani d ? C(5) 0.3163(3) 0.226(1) -0.0442(4) 0.033(2) 1.000 . Uani d ? C(6) 0.2917(3) 0.411(1) -0.0290(4) 0.033(2) 1.000 . Uani d ? C(7) 0.2252(3) 0.750(1) -0.0321(3) 0.026(2) 1.000 . Uani d ? H(1) 0.3625 0.0037 -0.1989 0.076 1.000 . Uiso c ? H(2) 0.3789 -0.2136 -0.2270 0.076 1.000 . Uiso c ? H(3) 0.3099 -0.1212 -0.2618 0.076 1.000 . Uiso c ? H(4) 0.4863 -0.2421 0.1083 0.057 1.000 . Uiso c ? H(5) 0.5424 -0.2772 0.0934 0.057 1.000 . Uiso c ? H(6) 0.5060 -0.0467 0.0755 0.057 1.000 . Uiso 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) 0.043(1) 0.041(1) 0.0317(9) 0.0000 0.0064(7) 0.0000 Cl(1) 0.084(2) 0.082(2) 0.055(2) -0.021(2) 0.013(1) 0.017(2) Cl(2) 0.081(2) 0.092(2) 0.069(2) -0.040(2) 0.007(2) 0.019(2) S(1) 0.072(2) 0.046(1) 0.055(1) -0.001(1) 0.034(1) -0.020(1) S(2) 0.045(1) 0.038(1) 0.059(1) 0.017(1) 0.020(1) -0.005(1) S(3) 0.040(1) 0.037(1) 0.034(1) 0.009(1) 0.0116(9) -0.0037(9) S(4) 0.030(1) 0.032(1) 0.038(1) 0.0111(9) 0.0087(9) -0.0081(9) S(5) 0.033(1) 0.030(1) 0.0294(9) 0.0091(9) 0.0074(8) -0.0052(9) S(6) 0.029(1) 0.031(1) 0.032(1) 0.0104(9) 0.0059(8) -0.0029(9) C(1) 0.065(7) 0.096(9) 0.045(6) -0.008(6) 0.030(5) -0.017(6) C(2) 0.044(5) 0.039(5) 0.057(6) 0.019(4) 0.017(4) 0.004(5) C(3) 0.046(5) 0.029(4) 0.038(4) 0.000(4) 0.026(4) -0.011(4) C(4) 0.040(4) 0.021(4) 0.043(4) 0.004(3) 0.027(4) -0.009(3) C(5) 0.025(4) 0.033(5) 0.042(5) 0.004(3) 0.017(3) -0.000(4) C(6) 0.026(4) 0.030(4) 0.034(4) 0.004(3) 0.007(3) -0.005(3) C(7) 0.022(4) 0.024(4) 0.031(4) 0.008(3) 0.011(3) -0.000(3) #=========================================================================== #== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1510 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_all 0.0520 _refine_ls_wR_factor_ref 0.0520 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min 0.00 _refine_diff_density_max 0.00 #=========================================================================== #== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe(1) Cl(1) 2.163(4) . . ? Fe(1) Cl(1) 2.163(4) . . ? Fe(1) Cl(2) 2.191(4) . . ? Fe(1) Cl(2) 2.191(4) . . ? S(1) C(1) 1.78(1) . . ? S(1) C(3) 1.745(9) . . ? S(2) C(2) 1.789(9) . . ? S(2) C(4) 1.737(8) . . ? S(3) C(3) 1.741(9) . . ? S(3) C(5) 1.749(8) . . ? S(4) C(4) 1.736(9) . . ? S(4) C(5) 1.732(7) . . ? S(5) C(6) 1.749(7) . . ? S(5) C(7) 1.713(8) . . ? S(6) C(6) 1.752(8) . . ? S(6) C(7) 1.736(7) . . ? C(1) H(1) 0.97 . . no C(1) H(2) 0.96 . . no C(1) H(3) 0.96 . . no C(2) H(4) 0.96 . . no C(2) H(5) 0.96 . . no C(2) H(6) 0.96 . . no C(3) C(4) 1.355(9) . . ? C(5) C(6) 1.35(1) . . ? C(7) C(7) 1.36(1) . . ? #--------------------------------------------------------------------------- #-- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Fe(1) Cl(1) 110.0(2) . . . ? Cl(1) Fe(1) Cl(2) 108.2(1) . . . ? Cl(1) Fe(1) Cl(2) 109.3(1) . . . ? Cl(1) Fe(1) Cl(2) 109.3(1) 2_655 2_655 2_655 ? Cl(1) Fe(1) Cl(2) 108.2(1) 2_655 2_655 2_655 ? Cl(2) Fe(1) Cl(2) 111.9(2) . . . ? C(1) S(1) C(3) 100.4(5) . . . ? C(2) S(2) C(4) 103.4(4) . . . ? C(3) S(3) C(5) 95.7(4) . . . ? C(4) S(4) C(5) 96.0(4) . . . ? C(6) S(5) C(7) 93.8(3) . . . ? C(6) S(6) C(7) 93.9(3) . . . ? S(1) C(1) H(1) 110.8 . . . no S(1) C(1) H(2) 111.4 . . . no S(1) C(1) H(3) 111.6 . . . no H(1) C(1) H(2) 107.2 . . . no H(1) C(1) H(3) 107.4 . . . no H(2) C(1) H(3) 108.2 . . . no S(2) C(2) H(4) 110.9 . . . no S(2) C(2) H(5) 111.1 . . . no S(2) C(2) H(6) 111.2 . . . no H(4) C(2) H(5) 107.8 . . . no H(4) C(2) H(6) 107.8 . . . no H(5) C(2) H(6) 108.0 . . . no S(1) C(3) S(3) 119.0(4) . . . ? S(1) C(3) C(4) 124.3(7) . . . ? S(3) C(3) C(4) 116.7(7) . . . ? S(2) C(4) S(4) 119.3(4) . . . ? S(2) C(4) C(3) 123.6(7) . . . ? S(4) C(4) C(3) 117.1(6) . . . ? S(3) C(5) S(4) 114.5(5) . . . ? S(3) C(5) C(6) 123.6(5) . . . ? S(4) C(5) C(6) 121.9(6) . . . ? S(5) C(6) S(6) 116.3(5) . . . ? S(5) C(6) C(5) 123.0(5) . . . ? S(6) C(6) C(5) 120.6(5) . . . ? S(5) C(7) S(6) 124.1(3) . . . ? S(5) C(7) C(7) 119.0(8) . . . ? S(6) C(7) C(7) 116.9(8) 7_565 7_565 7_565 ? #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Fe(1) H(4) 3.3432 . 1_565 no Fe(1) H(4) 3.3432 . 2_665 no Cl(1) H(2) 2.8033 . 4 no Cl(1) H(4) 2.9311 . 2_665 no Cl(1) H(6) 3.0494 . 2_655 no Cl(1) S(4) 3.333(3) . 2_655 no Cl(1) H(4) 3.4449 . 2_655 no Cl(1) C(2) 3.57(1) . 2_665 no Cl(1) C(1) 3.62(1) . 4 no Cl(1) S(6) 3.697(4) . 2_655 no Cl(1) C(2) 3.71(1) . 2_655 no Cl(2) H(1) 3.1932 . 3_665 no Cl(2) S(6) 3.384(4) . 2_655 no Cl(2) S(5) 3.393(4) . 8_565 no Cl(2) H(2) 3.4146 . 3_665 no Cl(2) C(1) 3.64(1) . 3_665 no Cl(2) C(7) 3.835(6) . 8_565 no S(1) H(3) 3.4387 . 6_544 no S(1) S(5) 3.865(5) . 1_545 no S(1) S(3) 3.898(4) . 1_545 no S(1) C(6) 3.90(1) . 1_545 no S(1) C(5) 3.91(1) . 1_545 no S(2) H(6) 3.1422 . 3_655 no S(2) H(5) 3.1610 . 3_645 no S(2) S(2) 3.224(5) . 3_645 no S(2) C(2) 3.68(1) . 3_645 no S(2) S(6) 3.743(4) . 1_545 no S(2) S(4) 3.858(4) . 1_545 no S(2) C(6) 3.865(9) . 1_545 no S(2) C(5) 3.901(9) . 1_545 no S(2) C(2) 3.92(1) . 3_655 no S(3) H(3) 2.9559 . 6_554 no S(3) C(7) 3.550(9) . 1_545 no S(3) C(1) 3.711(9) . 6_554 no S(3) S(6) 3.770(4) . 7 no S(3) S(5) 3.784(4) . 1_545 no S(3) C(7) 4.086(9) . 7 no S(4) C(7) 3.510(9) . 7 no S(4) S(5) 3.699(4) . 7 no S(4) S(6) 3.803(3) . 1_545 no S(4) C(7) 4.022(8) . 1_545 no S(5) H(3) 3.2401 . 6_554 no S(5) C(3) 3.63(1) . 1_565 no S(5) S(6) 3.766(3) . 7 no S(5) C(5) 3.79(1) . 7 no S(5) C(6) 3.820(9) . 7 no S(5) C(1) 3.99(1) . 6_554 no S(6) C(4) 3.59(1) . 1_565 no S(6) C(5) 3.749(9) . 7 no S(6) C(6) 3.753(9) . 7 no C(1) C(2) 4.07(1) . 3_655 no C(2) H(1) 3.3242 . 3_655 no C(2) C(4) 3.72(1) . 3_655 no C(2) C(3) 4.07(1) . 3_655 no C(3) C(6) 3.67(1) . 1_545 no C(3) C(7) 3.84(1) . 1_545 no C(3) C(7) 4.07(1) . 7 no C(4) H(6) 3.2137 . 3_655 no C(4) H(5) 3.4274 . 3_655 no C(4) C(6) 3.66(1) . 1_545 no C(4) C(7) 3.79(1) . 7 no C(4) C(7) 4.03(1) . 1_545 no C(5) C(7) 3.63(1) . 1_545 no C(5) C(7) 3.65(1) . 7 no C(5) C(6) 3.76(1) . 7 no C(6) C(6) 3.43(2) . 7 no H(1) H(5) 2.8591 . 3_655 no H(1) H(6) 3.0473 . 3_655 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag S(1) C(3) S(3) C(5) . . . . 179.5(6) no S(1) C(3) C(4) S(2) . . . . -0(1) no S(1) C(3) C(4) S(4) . . . . -178.7(6) no S(2) C(4) S(4) C(5) . . . . -178.6(6) no S(2) C(4) C(3) S(3) . . . . 176.9(6) no S(3) C(3) S(1) C(1) . . . . 73.2(7) no S(3) C(3) C(4) S(4) . . . . -2(1) no S(3) C(5) S(4) C(4) . . . . 1.5(6) no S(3) C(5) C(6) S(5) . . . . 0(1) no S(3) C(5) C(6) S(6) . . . . 179.0(5) no S(4) C(4) S(2) C(2) . . . . -8.7(8) no S(4) C(5) S(3) C(3) . . . . -2.2(6) no S(4) C(5) C(6) S(5) . . . . -177.9(5) no S(4) C(5) C(6) S(6) . . . . 1(1) no S(5) C(6) S(6) C(7) . . . . -2.8(6) no S(5) C(7) S(6) C(6) . . . . 178.2(6) no S(5) C(7) C(7) S(5) . . . . -180.0000 no S(5) C(7) C(7) S(6) . . . . 0(1) no S(6) C(6) S(5) C(7) . . . . 2.9(6) no S(6) C(7) S(5) C(6) . . . . -178.4(6) no S(6) C(7) C(7) S(6) . . . . 180.0000(1) no C(1) S(1) C(3) C(4) . . . . -109.9(9) no C(2) S(2) C(4) C(3) . . . . 172.7(9) no C(3) S(3) C(5) C(6) . . . . 179.4(9) no C(3) C(4) S(4) C(5) . . . . 0.0(9) no C(4) S(4) C(5) C(6) . . . . 179.9(8) no C(4) C(3) S(3) C(5) . . . . 2.3(9) no C(5) C(6) S(5) C(7) . . . . -178.4(9) no C(5) C(6) S(6) C(7) . . . . 178.5(8) no C(6) S(5) C(7) C(7) . . . . -2(1) no C(6) S(6) C(7) C(7) . . . . 1(1) no #--------------------------------------------------------------------------- #=========================================================================== # 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 #===========================================================================