# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Jun-ichi Yamada' 'Hiroki Akutsu' 'James S. Brooks' 'Eun S. Choi' 'David Graf' 'Isao Ikemoto' 'Koichi Kikuchi' ; Shin'ici Nakatsuji ; 'Hiroyuki Nishikawa' 'Takashi Toita' _publ_contact_author_name 'Prof Jun-ichi Yamada' _publ_contact_author_address ; Department of Meterial Science, Graduate School of Science Himeji Institute of Technology 3-2-1 Kouto Kamigori-cho, Ako-gun Hyogo 678-1297 JAPAN ; _publ_requested_coeditor_name ? _publ_contact_author_phone +81-791-58-0162 _publ_contact_author_fax +81-791-58-0164 _publ_contact_author_email yamada@sci.himeji-tech.ac.jp #===================================================================== _publ_requested_journal 'Chemical Communications' _publ_section_title ; A new organic superconductor, beta-(BDA-TTP)2GaCl4 [BDA-TTP = 2,5-(1,3-dithian-2-ylidene)-1,3,4,6-tetrathiapentalene] ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; data_(BDA-TTP)2GaCl4 _database_code_CSD 212143 _audit_creation_date 2003-05-15 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'CRYSTALS (Watkin et al 2001)' _computing_publication_material 'teXsan for Windows version 1.06' #------------------------------------------------------------------------------ _cell_length_a 12.4693(11) _cell_length_b 38.768(5) _cell_length_c 7.7351(2) _cell_angle_alpha 90 _cell_angle_beta 91.1990(4) _cell_angle_gamma 90 _cell_volume 3738.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'elongated plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1036.95 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H24 Cl4 Ga S16 ' _chemical_formula_moiety '2(C12 H12 S8), (Ga Cl4)' _chemical_formula_structural ? _chemical_compound_source 'synthesized by the authors' _exptl_crystal_F_000 2092.00 _exptl_absorpt_coefficient_mu 1.937 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; HIGASHI, T. (1995). Abscor - Empirical Absorption Correction, Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_max 1.130 _exptl_absorpt_correction_T_min 0.501 #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Quantum CCD' _diffrn_measurement_device 'Rigaku AFC7' _diffrn_measurement_method CCD _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 8487 _reflns_number_total 8344 _reflns_number_gt 5603 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.52 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_theta_full 24.473 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 96 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 64 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 4 0.163 1.609 ;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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_attached_hydrogens # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom Ga1 Ga 0.60967(4) -0.251246(13) 0.61941(7) 0.0375 1.0000 Uani . Cl1 Cl 0.70004(12) -0.27853(4) 0.8186(2) 0.0636 1.0000 Uani . Cl2 Cl 0.51848(14) -0.28865(5) 0.4715(3) 0.0864 1.0000 Uani . Cl3 Cl 0.50693(13) -0.21372(4) 0.7409(2) 0.0710 1.0000 Uani . Cl4 Cl 0.71789(13) -0.22425(4) 0.4520(2) 0.0649 1.0000 Uani . S1 S 0.04411(9) 0.13631(3) 1.07511(17) 0.0387 1.0000 Uani . S2 S 0.28645(9) 0.15077(3) 1.09096(16) 0.0376 1.0000 Uani . S3 S 0.09323(8) 0.05921(3) 0.98706(16) 0.0348 1.0000 Uani . S4 S 0.32866(8) 0.07376(3) 0.99561(16) 0.0350 1.0000 Uani . S5 S 0.13708(8) -0.01368(3) 0.85679(16) 0.0355 1.0000 Uani . S6 S 0.37217(8) 0.00050(3) 0.86829(16) 0.0347 1.0000 Uani . S7 S 0.17731(9) -0.09031(3) 0.77989(19) 0.0442 1.0000 Uani . S8 S 0.42122(9) -0.07547(3) 0.7818(2) 0.0469 1.0000 Uani . S9 S 0.53721(8) 0.13573(3) 0.83058(16) 0.0360 1.0000 Uani . S10 S 0.77837(9) 0.15209(3) 0.82724(16) 0.0364 1.0000 Uani . S11 S 0.58849(8) 0.05920(3) 0.73438(16) 0.0328 1.0000 Uani . S12 S 0.82357(8) 0.07460(3) 0.74483(16) 0.0338 1.0000 Uani . S13 S 0.63576(8) -0.01380(3) 0.60866(16) 0.0350 1.0000 Uani . S14 S 0.86991(8) 0.00189(3) 0.61550(16) 0.0344 1.0000 Uani . S15 S 0.67976(9) -0.08969(3) 0.5210(2) 0.0491 1.0000 Uani . S16 S 0.92384(9) -0.07381(3) 0.53184(19) 0.0445 1.0000 Uani . C1 C 0.0421(4) 0.17923(13) 0.9848(8) 0.0478 1.0000 Uani . C2 C 0.1323(5) 0.20243(13) 1.0525(9) 0.0519 1.0000 Uani . C3 C 0.2412(4) 0.19081(13) 0.9928(7) 0.0464 1.0000 Uani . C4 C 0.1769(3) 0.12336(11) 1.0449(6) 0.0303 1.0000 Uani . C5 C 0.1972(3) 0.09000(11) 1.0117(6) 0.0303 1.0000 Uani . C6 C 0.1793(3) 0.0272(1) 0.9178(6) 0.0308 1.0000 Uani . C7 C 0.2861(3) 0.0336(1) 0.9232(6) 0.0303 1.0000 Uani . C8 C 0.2679(3) -0.02906(11) 0.8291(6) 0.0314 1.0000 Uani . C9 C 0.2876(3) -0.06278(11) 0.7863(6) 0.0328 1.0000 Uani . C10 C 0.2219(4) -0.12833(13) 0.6670(7) 0.0407 1.0000 Uani . C11 C 0.3316(4) -0.14090(12) 0.7229(7) 0.0380 1.0000 Uani . C12 C 0.4222(4) -0.11697(13) 0.6757(7) 0.0388 1.0000 Uani . C13 C 0.5302(4) 0.17849(13) 0.7380(8) 0.0451 1.0000 Uani . C14 C 0.6188(5) 0.20269(13) 0.7966(8) 0.0491 1.0000 Uani . C15 C 0.7279(4) 0.19210(12) 0.7343(7) 0.0430 1.0000 Uani . C16 C 0.6704(3) 0.1237(1) 0.7899(5) 0.0275 1.0000 Uani . C17 C 0.6912(3) 0.0903(1) 0.7583(5) 0.0274 1.0000 Uani . C18 C 0.6762(3) 0.0274(1) 0.6664(6) 0.0298 1.0000 Uani . C19 C 0.7822(3) 0.0345(1) 0.6707(5) 0.0289 1.0000 Uani . C20 C 0.7676(3) -0.02859(11) 0.5774(6) 0.0324 1.0000 Uani . C21 C 0.7883(3) -0.06186(11) 0.5337(6) 0.0324 1.0000 Uani . C22 C 0.7270(4) -0.12819(13) 0.4138(7) 0.0398 1.0000 Uani . C23 C 0.8379(4) -0.13943(13) 0.4694(7) 0.0401 1.0000 Uani . C24 C 0.9254(4) -0.11506(12) 0.4207(7) 0.0381 1.0000 Uani . H1 H 0.048(4) 0.1750(14) 0.850(6) 0.0507 1.0000 Uiso . H2 H -0.021(4) 0.1861(14) 1.011(6) 0.0507 1.0000 Uiso . H3 H 0.133(4) 0.2243(15) 0.992(6) 0.0507 1.0000 Uiso . H4 H 0.126(4) 0.2064(14) 1.180(6) 0.0507 1.0000 Uiso . H5 H 0.291(4) 0.2072(15) 1.018(6) 0.0507 1.0000 Uiso . H6 H 0.235(4) 0.1866(14) 0.871(6) 0.0507 1.0000 Uiso . H7 H 0.173(4) -0.1448(15) 0.696(6) 0.0507 1.0000 Uiso . H8 H 0.216(4) -0.1254(14) 0.557(6) 0.0507 1.0000 Uiso . H9 H 0.335(4) -0.1462(14) 0.840(6) 0.0507 1.0000 Uiso . H10 H 0.342(4) -0.1636(15) 0.667(6) 0.0507 1.0000 Uiso . H11 H 0.423(4) -0.1105(14) 0.550(6) 0.0507 1.0000 Uiso . H12 H 0.491(4) -0.1265(14) 0.708(5) 0.0507 1.0000 Uiso . H13 H 0.519(4) 0.1750(14) 0.623(6) 0.0507 1.0000 Uiso . H14 H 0.462(4) 0.1866(14) 0.774(6) 0.0507 1.0000 Uiso . H15 H 0.604(4) 0.2257(15) 0.746(5) 0.0507 1.0000 Uiso . H16 H 0.629(4) 0.2048(14) 0.919(6) 0.0507 1.0000 Uiso . H17 H 0.783(4) 0.2088(15) 0.772(5) 0.0507 1.0000 Uiso . H18 H 0.735(4) 0.1913(14) 0.610(6) 0.0507 1.0000 Uiso . H19 H 0.674(4) -0.1436(14) 0.459(6) 0.0507 1.0000 Uiso . H20 H 0.720(4) -0.1250(14) 0.293(6) 0.0507 1.0000 Uiso . H21 H 0.839(4) -0.1432(14) 0.601(6) 0.0507 1.0000 Uiso . H22 H 0.849(4) -0.1643(15) 0.414(6) 0.0507 1.0000 Uiso . H23 H 0.921(4) -0.1105(14) 0.301(6) 0.0507 1.0000 Uiso . H24 H 0.995(4) -0.1231(14) 0.446(5) 0.0507 1.0000 Uiso . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0331(2) 0.0323(2) 0.0471(3) -0.0008(2) 0.0034(2) -0.0000(2) Cl1 0.0636(9) 0.0499(8) 0.077(1) 0.0182(7) -0.0091(7) 0.0092(6) Cl2 0.063(1) 0.0974(13) 0.0992(13) -0.0416(11) 0.0047(9) -0.0369(9) Cl3 0.0649(9) 0.068(1) 0.0805(11) -0.0069(8) 0.0123(8) 0.0306(8) Cl4 0.0676(9) 0.0490(8) 0.079(1) 0.0125(7) 0.0252(8) -0.0086(7) S1 0.0289(5) 0.0353(6) 0.0520(7) 0.0008(5) 0.0065(5) 0.0006(4) S2 0.0305(5) 0.0323(6) 0.0502(7) -0.0028(5) 0.0016(5) -0.0038(4) S3 0.0221(5) 0.0282(5) 0.0543(7) 0.0026(5) 0.0029(5) -0.0018(4) S4 0.0223(5) 0.0284(5) 0.0541(7) -0.0007(5) -0.0013(5) -0.0027(4) S5 0.0221(5) 0.0281(5) 0.0561(7) -0.0011(5) -0.0010(5) -0.0024(4) S6 0.0221(5) 0.0283(5) 0.0537(7) -0.0003(5) 0.0019(5) -0.0022(4) S7 0.0262(5) 0.0322(6) 0.0742(9) -0.0089(6) 0.0037(5) -0.0032(4) S8 0.0244(5) 0.0364(6) 0.0799(9) -0.0104(6) 0.0006(6) -0.0002(4) S9 0.0269(5) 0.0316(5) 0.0497(7) -0.0012(5) 0.0049(5) 0.0021(4) S10 0.0291(5) 0.0303(5) 0.0496(7) -0.0040(5) 0.0007(5) -0.0051(4) S11 0.0224(5) 0.0243(5) 0.0519(7) -0.0013(4) 0.0040(4) 0.0004(4) S12 0.0226(5) 0.0271(5) 0.0516(7) -0.0020(5) -0.0002(4) -0.0012(4) S13 0.0243(5) 0.0265(5) 0.0541(7) -0.0031(5) 0.0012(5) -0.0007(4) S14 0.0219(5) 0.0276(5) 0.0538(7) -0.0030(5) 0.0036(5) 0.0006(4) S15 0.0270(6) 0.0338(6) 0.087(1) -0.0160(6) 0.0064(6) -0.0022(4) S16 0.0260(5) 0.0336(6) 0.0739(9) -0.0115(6) 0.0010(5) 0.0020(4) C1 0.045(3) 0.037(2) 0.061(3) 0.006(2) 0.001(2) 0.013(2) C2 0.056(3) 0.028(2) 0.072(4) -0.003(2) 0.004(3) 0.003(2) C3 0.053(3) 0.033(2) 0.053(3) 0.000(2) 0.003(2) -0.013(2) C4 0.0255(19) 0.0262(19) 0.039(2) -0.0003(17) 0.0032(17) 0.0005(16) C5 0.0238(18) 0.031(2) 0.036(2) 0.0038(17) 0.0021(17) 0.0006(16) C6 0.028(2) 0.0249(19) 0.039(2) 0.0063(17) 0.0005(17) -0.0036(16) C7 0.028(2) 0.0254(19) 0.037(2) -0.0000(17) 0.0022(17) -0.0008(16) C8 0.0229(19) 0.030(2) 0.042(2) 0.0037(18) -0.0011(17) -0.0008(16) C9 0.028(2) 0.030(2) 0.040(2) 0.0028(18) -0.0007(18) -0.0020(16) C10 0.042(2) 0.040(3) 0.040(3) 0.001(2) -0.001(2) -0.003(2) C11 0.041(2) 0.033(2) 0.040(3) 0.001(2) 0.003(2) 0.0020(19) C12 0.031(2) 0.042(2) 0.043(3) 0.001(2) 0.003(2) 0.0052(19) C13 0.045(3) 0.034(2) 0.056(3) 0.005(2) -0.003(2) 0.013(2) C14 0.056(3) 0.027(2) 0.064(3) -0.005(2) -0.003(3) 0.004(2) C15 0.056(3) 0.030(2) 0.044(3) 0.002(2) 0.010(2) -0.004(2) C16 0.0265(19) 0.0261(19) 0.030(2) 0.0001(16) 0.0042(16) 0.0024(15) C17 0.0235(18) 0.0263(19) 0.033(2) 0.0016(16) 0.0044(16) -0.0008(15) C18 0.0255(19) 0.0249(19) 0.039(2) -0.0013(17) 0.0023(17) -0.0033(15) C19 0.0285(19) 0.0231(18) 0.035(2) 0.0031(17) 0.0025(17) 0.0010(15) C20 0.027(2) 0.028(2) 0.042(2) 0.0027(18) -0.0001(18) 0.0032(16) C21 0.030(2) 0.030(2) 0.037(2) -0.0024(18) 0.0014(17) 0.0033(16) C22 0.035(2) 0.038(2) 0.046(3) -0.004(2) -0.001(2) 0.0020(19) C23 0.038(2) 0.036(2) 0.046(3) 0.002(2) -0.001(2) 0.0023(19) C24 0.035(2) 0.036(2) 0.043(3) 0.004(2) 0.004(2) 0.0049(19) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 4.69 -0.513 2.80 ; _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5603 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_all 0.0638 _refine_ls_wR_factor_ref 0.0534 _refine_ls_goodness_of_fit_ref 1.1052 _refine_ls_shift/su_max 0.001226 _refine_diff_density_min -0.525 _refine_diff_density_max 0.569 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ga1 . Cl1 . 2.1655(15) yes Ga1 . Cl2 . 2.1566(16) yes Ga1 . Cl3 . 2.1657(15) yes Ga1 . Cl4 . 2.1603(15) yes S1 . C1 . 1.804(5) yes S1 . C4 . 1.751(4) yes S2 . C3 . 1.813(5) yes S2 . C4 . 1.761(4) yes S3 . C5 . 1.770(4) yes S3 . C6 . 1.734(4) yes S4 . C5 . 1.763(4) yes S4 . C7 . 1.733(4) yes S5 . C6 . 1.732(4) yes S5 . C8 . 1.754(4) yes S6 . C7 . 1.732(4) yes S6 . C8 . 1.755(4) yes S7 . C9 . 1.740(4) yes S7 . C10 . 1.807(5) yes S8 . C9 . 1.739(4) yes S8 . C12 . 1.806(5) yes S9 . C13 . 1.807(5) yes S9 . C16 . 1.759(4) yes S10 . C15 . 1.817(5) yes S10 . C16 . 1.758(4) yes S11 . C17 . 1.767(4) yes S11 . C18 . 1.737(4) yes S12 . C17 . 1.764(4) yes S12 . C19 . 1.732(4) yes S13 . C18 . 1.731(4) yes S13 . C20 . 1.762(4) yes S14 . C19 . 1.731(4) yes S14 . C20 . 1.759(4) yes S15 . C21 . 1.732(4) yes S15 . C22 . 1.812(5) yes S16 . C21 . 1.753(4) yes S16 . C24 . 1.816(5) yes C1 . C2 . 1.524(8) yes C1 . H1 . 1.06(4) no C1 . H2 . 0.86(5) no C2 . C3 . 1.512(8) yes C2 . H3 . 0.97(5) no C2 . H4 . 1.00(4) no C3 . H5 . 0.91(5) no C3 . H6 . 0.96(4) no C4 . C5 . 1.344(6) yes C6 . C7 . 1.355(6) yes C8 . C9 . 1.372(6) yes C10 . C11 . 1.507(7) yes C10 . H7 . 0.91(5) no C10 . H8 . 0.86(4) no C11 . C12 . 1.513(7) yes C11 . H9 . 0.93(4) no C11 . H10 . 0.99(5) no C12 . H11 . 1.01(4) no C12 . H12 . 0.96(5) no C13 . C14 . 1.512(7) yes C13 . H13 . 0.91(4) no C13 . H14 . 0.95(5) no C14 . C15 . 1.510(8) yes C14 . H15 . 0.99(5) no C14 . H16 . 0.96(4) no C15 . H17 . 0.98(5) no C15 . H18 . 0.97(4) no C16 . C17 . 1.344(6) yes C18 . C19 . 1.350(6) yes C20 . C21 . 1.360(6) yes C22 . C23 . 1.503(6) yes C22 . H19 . 0.96(5) no C22 . H20 . 0.94(4) no C23 . C24 . 1.498(7) yes C23 . H21 . 1.03(4) no C23 . H22 . 1.06(5) no C24 . H23 . 0.94(4) no C24 . H24 . 0.94(5) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ga1 . Cl2 . 108.04(8) yes Cl1 . Ga1 . Cl3 . 108.86(7) yes Cl2 . Ga1 . Cl3 . 111.82(8) yes Cl1 . Ga1 . Cl4 . 109.93(7) yes Cl2 . Ga1 . Cl4 . 109.67(8) yes Cl3 . Ga1 . Cl4 . 108.50(7) yes C1 . S1 . C4 . 102.6(2) yes C3 . S2 . C4 . 101.5(2) yes C5 . S3 . C6 . 93.40(19) yes C5 . S4 . C7 . 93.7(2) yes C6 . S5 . C8 . 93.8(2) yes C7 . S6 . C8 . 93.8(2) yes C9 . S7 . C10 . 105.3(2) yes C9 . S8 . C12 . 106.1(2) yes C13 . S9 . C16 . 102.1(2) yes C15 . S10 . C16 . 102.2(2) yes C17 . S11 . C18 . 93.24(19) yes C17 . S12 . C19 . 93.28(19) yes C18 . S13 . C20 . 93.9(2) yes C19 . S14 . C20 . 94.14(19) yes C21 . S15 . C22 . 106.1(2) yes C21 . S16 . C24 . 104.9(2) yes S1 . C1 . C2 . 114.1(4) yes S1 . C1 . H1 . 103.9(29) no C2 . C1 . H1 . 111.3(28) no S1 . C1 . H2 . 101.5(36) no C2 . C1 . H2 . 114.4(35) no H1 . C1 . H2 . 110.9(40) no C1 . C2 . C3 . 112.3(5) yes C1 . C2 . H3 . 111.5(29) no C3 . C2 . H3 . 95.2(29) no C1 . C2 . H4 . 110.7(30) no C3 . C2 . H4 . 116.0(29) no H3 . C2 . H4 . 110.2(43) no S2 . C3 . C2 . 113.7(4) yes S2 . C3 . H5 . 107.4(33) no C2 . C3 . H5 . 110.1(32) no S2 . C3 . H6 . 106.7(32) no C2 . C3 . H6 . 107.0(30) no H5 . C3 . H6 . 112.0(42) no S1 . C4 . S2 . 122.1(2) yes S1 . C4 . C5 . 118.9(3) yes S2 . C4 . C5 . 118.1(3) yes S3 . C5 . S4 . 115.6(2) yes S3 . C5 . C4 . 122.0(3) yes S4 . C5 . C4 . 122.4(3) yes S3 . C6 . S5 . 123.5(2) yes S3 . C6 . C7 . 118.2(3) yes S5 . C6 . C7 . 118.1(3) yes S4 . C7 . S6 . 123.9(2) yes S4 . C7 . C6 . 118.0(3) yes S6 . C7 . C6 . 118.0(3) yes S5 . C8 . S6 . 116.4(2) yes S5 . C8 . C9 . 121.7(3) yes S6 . C8 . C9 . 121.9(3) yes S7 . C9 . S8 . 125.6(3) yes S7 . C9 . C8 . 116.5(3) yes S8 . C9 . C8 . 116.8(3) yes S7 . C10 . C11 . 114.3(3) yes S7 . C10 . H7 . 103.7(32) no C11 . C10 . H7 . 107.8(32) no S7 . C10 . H8 . 110.5(37) no C11 . C10 . H8 . 112.7(34) no H7 . C10 . H8 . 107.1(45) no C10 . C11 . C12 . 114.3(4) yes C10 . C11 . H9 . 111.9(31) no C12 . C11 . H9 . 110.7(32) no C10 . C11 . H10 . 106.9(28) no C12 . C11 . H10 . 109.6(28) no H9 . C11 . H10 . 102.7(43) no S8 . C12 . C11 . 115.1(3) yes S8 . C12 . H11 . 102.7(30) no C11 . C12 . H11 . 114.1(28) no S8 . C12 . H12 . 103.9(31) no C11 . C12 . H12 . 111.5(31) no H11 . C12 . H12 . 108.6(38) no S9 . C13 . C14 . 114.9(4) yes S9 . C13 . H13 . 104.8(36) no C14 . C13 . H13 . 119.2(34) no S9 . C13 . H14 . 103.0(31) no C14 . C13 . H14 . 111.2(31) no H13 . C13 . H14 . 101.9(41) no C13 . C14 . C15 . 113.2(4) yes C13 . C14 . H15 . 108.1(28) no C15 . C14 . H15 . 106.4(28) no C13 . C14 . H16 . 115.7(32) no C15 . C14 . H16 . 103.4(31) no H15 . C14 . H16 . 109.7(43) no S10 . C15 . C14 . 114.4(4) yes S10 . C15 . H17 . 102.4(30) no C14 . C15 . H17 . 110.6(29) no S10 . C15 . H18 . 109.2(32) no C14 . C15 . H18 . 115.1(29) no H17 . C15 . H18 . 103.9(40) no S9 . C16 . S10 . 121.9(2) yes S9 . C16 . C17 . 118.3(3) yes S10 . C16 . C17 . 118.8(3) yes S11 . C17 . S12 . 115.8(2) yes S11 . C17 . C16 . 122.3(3) yes S12 . C17 . C16 . 121.9(3) yes S11 . C18 . S13 . 123.4(2) yes S11 . C18 . C19 . 118.1(3) yes S13 . C18 . C19 . 118.3(3) yes S12 . C19 . S14 . 123.5(2) yes S12 . C19 . C18 . 118.4(3) yes S14 . C19 . C18 . 117.9(3) yes S13 . C20 . S14 . 115.7(2) yes S13 . C20 . C21 . 121.7(3) yes S14 . C20 . C21 . 122.6(3) yes S15 . C21 . S16 . 126.0(3) yes S15 . C21 . C20 . 116.9(3) yes S16 . C21 . C20 . 116.2(3) yes S15 . C22 . C23 . 114.5(3) yes S15 . C22 . H19 . 96.6(31) no C23 . C22 . H19 . 110.5(30) no S15 . C22 . H20 . 108.7(33) no C23 . C22 . H20 . 112.8(30) no H19 . C22 . H20 . 112.7(41) no C22 . C23 . C24 . 114.6(4) yes C22 . C23 . H21 . 108.5(27) no C24 . C23 . H21 . 110.2(28) no C22 . C23 . H22 . 106.1(25) no C24 . C23 . H22 . 111.4(26) no H21 . C23 . H22 . 105.7(38) no S16 . C24 . C23 . 114.9(3) yes S16 . C24 . H23 . 107.4(33) no C23 . C24 . H23 . 109.8(31) no S16 . C24 . H24 . 102.3(32) no C23 . C24 . H24 . 114.2(33) no H23 . C24 . H24 . 107.6(40) no #============================================================================== data_BDATTP3GaCl4PhCl_ _database_code_CSD 212144 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06' _computing_structure_solution ; isomorphous replacement method from (BDT-TTP)~3~FeCl~4~PhCl ; _computing_structure_refinement 'teXsan for Windows version 1.06' _computing_publication_material 'teXsan for Windows version 1.06' #------------------------------------------------------------------------------ _cell_length_a 9.7552(9) _cell_length_b 35.599(4) _cell_length_c 8.840(2) _cell_angle_alpha 90 _cell_angle_beta 92.12(1) _cell_angle_gamma 90 _cell_volume 3067.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'elongated plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1562.21 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H41 Cl5 Ga S24 ' _chemical_formula_moiety '3(C12 H12 S8), (Ga Cl4), (C6 H5 Cl)' _chemical_formula_structural ? _chemical_compound_source 'synthesized by the authors' _exptl_crystal_F_000 1586.00 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North,Phillips & Matthews, 1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.691 _exptl_special_details ; The scan width was (0.68+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.83 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 7639 _reflns_number_total 7508 _reflns_number_gt 5465 _reflns_threshold_expression I>1.00\s(I) _diffrn_reflns_av_R_equivalents 0.02220 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.08843 _diffrn_orient_matrix_UB_12 -0.00865 _diffrn_orient_matrix_UB_13 0.04914 _diffrn_orient_matrix_UB_21 -0.00957 _diffrn_orient_matrix_UB_22 -0.02464 _diffrn_orient_matrix_UB_23 -0.05366 _diffrn_orient_matrix_UB_31 0.05109 _diffrn_orient_matrix_UB_32 0.01035 _diffrn_orient_matrix_UB_33 -0.08671 #------------------------------------------------------------------------------ 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 84 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 82 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 2 0.163 1.609 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 10 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) 0.5813(1) 0.0491 0.6832(1) 0.0496(3) 1.000 . Uani d ? Cl(1) 0.6708(4) -0.00602(8) 0.7097(4) 0.115(1) 1.000 . Uani d ? Cl(2) 0.7332(3) 0.0876(1) 0.6017(3) 0.093(1) 1.000 . Uani d ? Cl(3) 0.5193(4) 0.0679(1) 0.9007(4) 0.135(2) 1.000 . Uani d ? Cl(4) 0.4062(2) 0.04580(8) 0.5260(3) 0.0684(7) 1.000 . Uani d ? Cl(5) 0.119(1) 0.0342(2) -0.168(1) 0.389(6) 1.000 . Uani d ? S(1) -0.0308(2) 0.20468(7) 1.0592(2) 0.0432(6) 1.000 . Uani d ? S(2) -0.2368(2) 0.23287(7) 0.8146(3) 0.0431(6) 1.000 . Uani d ? S(3) 0.1690(2) 0.26899(6) 0.9709(2) 0.0368(5) 1.000 . Uani d ? S(4) -0.0306(2) 0.29591(6) 0.7318(2) 0.0374(5) 1.000 . Uani d ? S(5) 0.3643(2) 0.33313(6) 0.8963(2) 0.0370(6) 1.000 . Uani d ? S(6) 0.1650(2) 0.35975(6) 0.6545(2) 0.0359(5) 1.000 . Uani d ? S(7) 0.5505(2) 0.40382(7) 0.8454(3) 0.0492(7) 1.000 . Uani d ? S(8) 0.3448(2) 0.43220(7) 0.6044(3) 0.0497(6) 1.000 . Uani d ? S(9) 0.2481(2) 0.18139(7) 0.7389(2) 0.0445(6) 1.000 . Uani d ? S(10) 0.0395(2) 0.20932(7) 0.5030(3) 0.0441(6) 1.000 . Uani d ? S(11) 0.4456(2) 0.24783(6) 0.6589(2) 0.0375(5) 1.000 . Uani d ? S(12) 0.2457(2) 0.27488(6) 0.4191(2) 0.0368(5) 1.000 . Uani d ? S(13) 0.6363(2) 0.31431(6) 0.5936(2) 0.0377(6) 1.000 . Uani d ? S(14) 0.4353(2) 0.34157(6) 0.3546(2) 0.0367(5) 1.000 . Uani d ? S(15) 0.8445(2) 0.37831(6) 0.5103(3) 0.0446(6) 1.000 . Uani d ? S(16) 0.6384(2) 0.40729(7) 0.2709(2) 0.0424(6) 1.000 . Uani d ? S(17) 0.5474(2) 0.15866(7) 0.3935(2) 0.0490(7) 1.000 . Uani d ? S(18) 0.3290(2) 0.19033(6) 0.1713(3) 0.0444(6) 1.000 . Uani d ? S(19) 0.7219(2) 0.23141(6) 0.3494(2) 0.0369(5) 1.000 . Uani d ? S(20) 0.5192(2) 0.25910(6) 0.1133(2) 0.0359(5) 1.000 . Uani d ? S(21) 0.9150(2) 0.29521(6) 0.2732(2) 0.0384(6) 1.000 . Uani d ? S(22) 0.7147(2) 0.32289(6) 0.0386(2) 0.0364(5) 1.000 . Uani d ? S(23) 1.1186(2) 0.35943(7) 0.1968(3) 0.0505(7) 1.000 . Uani d ? S(24) 0.9123(2) 0.38686(7) -0.0494(3) 0.0490(7) 1.000 . Uani d ? C(1) -0.093(1) 0.1599(2) 0.989(1) 0.056(3) 1.000 . Uani d ? C(2) -0.240(1) 0.1596(3) 0.932(1) 0.063(3) 1.000 . Uani d ? C(3) -0.2649(8) 0.1831(3) 0.787(1) 0.059(3) 1.000 . Uani d ? C(4) -0.0747(7) 0.2340(2) 0.9057(8) 0.034(2) 1.000 . Uani d ? C(5) 0.0111(7) 0.2622(2) 0.8708(8) 0.029(2) 1.000 . Uani d ? C(6) 0.2121(7) 0.3077(2) 0.8680(8) 0.034(2) 1.000 . Uani d ? C(7) 0.1229(7) 0.3201(2) 0.7566(8) 0.032(2) 1.000 . Uani d ? C(8) 0.3172(7) 0.3683(2) 0.7612(8) 0.031(2) 1.000 . Uani d ? C(9) 0.3930(7) 0.3989(2) 0.7434(8) 0.037(2) 1.000 . Uani d ? C(10) 0.5312(9) 0.4503(3) 0.918(1) 0.061(3) 1.000 . Uani d ? C(11) 0.498(1) 0.4792(3) 0.800(1) 0.062(3) 1.000 . Uani d ? C(12) 0.358(1) 0.4741(3) 0.719(1) 0.066(3) 1.000 . Uani d ? C(13) 0.2233(9) 0.1372(2) 0.637(1) 0.049(3) 1.000 . Uani d ? C(14) 0.0809(9) 0.1328(2) 0.565(1) 0.050(3) 1.000 . Uani d ? C(15) 0.0441(9) 0.1604(3) 0.440(1) 0.053(3) 1.000 . Uani d ? C(16) 0.2020(7) 0.2132(2) 0.5931(9) 0.036(2) 1.000 . Uani d ? C(17) 0.2879(7) 0.2409(2) 0.5599(8) 0.027(2) 1.000 . Uani d ? C(18) 0.4859(7) 0.2886(2) 0.5589(8) 0.033(2) 1.000 . Uani d ? C(19) 0.3959(7) 0.3003(2) 0.4535(8) 0.031(2) 1.000 . Uani d ? C(20) 0.5958(7) 0.3480(2) 0.4515(8) 0.035(2) 1.000 . Uani d ? C(21) 0.6788(7) 0.3754(2) 0.4196(8) 0.032(2) 1.000 . Uani d ? C(22) 0.8473(8) 0.4270(3) 0.567(1) 0.049(3) 1.000 . Uani d ? C(23) 0.8133(9) 0.4545(2) 0.440(1) 0.056(3) 1.000 . Uani d ? C(24) 0.6719(9) 0.4511(2) 0.368(1) 0.051(3) 1.000 . Uani d ? C(25) 0.5241(9) 0.1178(2) 0.273(1) 0.052(3) 1.000 . Uani d ? C(26) 0.3772(9) 0.1128(2) 0.209(1) 0.056(3) 1.000 . Uani d ? C(27) 0.3366(9) 0.1428(2) 0.0964(9) 0.050(3) 1.000 . Uani d ? C(28) 0.4885(7) 0.1928(2) 0.2638(9) 0.038(2) 1.000 . Uani d ? C(29) 0.5657(6) 0.2236(2) 0.2449(8) 0.031(2) 1.000 . Uani d ? C(30) 0.7636(7) 0.2714(2) 0.2458(8) 0.031(2) 1.000 . Uani d ? C(31) 0.6709(7) 0.2835(2) 0.1419(8) 0.029(2) 1.000 . Uani d ? C(32) 0.8729(7) 0.3290(2) 0.1350(8) 0.033(2) 1.000 . Uani d ? C(33) 0.9581(7) 0.3585(2) 0.1042(8) 0.035(2) 1.000 . Uani d ? C(34) 1.159(1) 0.4073(3) 0.204(1) 0.083(4) 1.000 . Uani d ? C(35) 1.129(1) 0.4304(3) 0.067(1) 0.078(4) 1.000 . Uani d ? C(36) 0.984(1) 0.4309(3) 0.007(1) 0.075(3) 1.000 . Uani d ? C(37) 0.047(2) 0.0399(5) -0.012(1) 0.160 1.000 G Uiso d ? C(38) 0.135(1) 0.0333(4) 0.113(2) 0.160 1.000 G Uiso d ? C(39) 0.087(1) 0.0367(4) 0.259(1) 0.160 1.000 G Uiso d ? C(40) -0.049(2) 0.0467(4) 0.280(1) 0.160 1.000 G Uiso d ? C(41) -0.137(1) 0.0533(4) 0.155(2) 0.160 1.000 G Uiso d ? C(42) -0.089(1) 0.0499(4) 0.009(1) 0.160 1.000 G Uiso d ? H(1) -0.0410 0.1531 0.9018 0.051 1.000 . Uiso c ? H(2) -0.0895 0.1421 1.0609 0.051 1.000 . Uiso c ? H(3) -0.2612 0.1356 0.9056 0.051 1.000 . Uiso c ? H(4) -0.2894 0.1704 1.0050 0.051 1.000 . Uiso c ? H(5) -0.3610 0.1794 0.7603 0.051 1.000 . Uiso c ? H(6) -0.2116 0.1745 0.7103 0.051 1.000 . Uiso c ? H(7) 0.4637 0.4520 0.9883 0.051 1.000 . Uiso c ? H(8) 0.6169 0.4597 0.9607 0.051 1.000 . Uiso c ? H(9) 0.4897 0.5037 0.8525 0.051 1.000 . Uiso c ? H(10) 0.5633 0.4807 0.7304 0.051 1.000 . Uiso c ? H(11) 0.3482 0.4960 0.6534 0.051 1.000 . Uiso c ? H(12) 0.2917 0.4742 0.7896 0.051 1.000 . Uiso c ? H(13) 0.2871 0.1389 0.5565 0.051 1.000 . Uiso c ? H(14) 0.2495 0.1188 0.7049 0.051 1.000 . Uiso c ? H(15) 0.0671 0.1085 0.5386 0.051 1.000 . Uiso c ? H(16) 0.0159 0.1377 0.6539 0.051 1.000 . Uiso c ? H(17) -0.0468 0.1566 0.3933 0.051 1.000 . Uiso c ? H(18) 0.1076 0.1604 0.3619 0.051 1.000 . Uiso c ? H(19) 0.7733 0.4326 0.6367 0.051 1.000 . Uiso c ? H(20) 0.9306 0.4340 0.6203 0.051 1.000 . Uiso c ? H(21) 0.8460 0.4794 0.4527 0.051 1.000 . Uiso c ? H(22) 0.8862 0.4461 0.3503 0.051 1.000 . Uiso c ? H(23) 0.6629 0.4714 0.2869 0.051 1.000 . Uiso c ? H(24) 0.6152 0.4557 0.4399 0.051 1.000 . Uiso c ? H(25) 0.5800 0.1199 0.2003 0.051 1.000 . Uiso c ? H(26) 0.5395 0.0974 0.3419 0.051 1.000 . Uiso c ? H(27) 0.3642 0.0895 0.1690 0.051 1.000 . Uiso c ? H(28) 0.3087 0.1163 0.2909 0.051 1.000 . Uiso c ? H(29) 0.2481 0.1376 0.0411 0.051 1.000 . Uiso c ? H(30) 0.4024 0.1431 0.0123 0.051 1.000 . Uiso c ? H(31) 1.1151 0.4201 0.2747 0.051 1.000 . Uiso c ? H(32) 1.2566 0.4105 0.2107 0.051 1.000 . Uiso c ? H(33) 1.1533 0.4569 0.0978 0.051 1.000 . Uiso c ? H(34) 1.1891 0.4243 -0.0099 0.051 1.000 . Uiso c ? H(35) 0.9847 0.4472 -0.0811 0.051 1.000 . Uiso c ? H(36) 0.9318 0.4423 0.0810 0.051 1.000 . Uiso c ? H(37) 0.228(1) 0.0264(5) 0.098(3) 0.160 1.000 G Uiso d ? H(38) 0.147(2) 0.0322(6) 0.344(2) 0.160 1.000 G Uiso d ? H(39) -0.082(2) 0.0490(7) 0.379(1) 0.160 1.000 G Uiso d ? H(40) -0.230(1) 0.0601(6) 0.169(3) 0.160 1.000 G Uiso d ? H(41) -0.149(2) 0.0544(6) -0.077(2) 0.160 1.000 G Uiso d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ga(1) 0.0708(6) 0.0322(5) 0.0457(5) -0.0009(5) 0.0003(5) 0.0000(5) Cl(1) 0.153(3) 0.042(1) 0.143(3) 0.027(2) -0.082(2) -0.008(2) Cl(2) 0.078(2) 0.099(2) 0.100(2) -0.026(2) -0.013(2) 0.040(2) Cl(3) 0.162(3) 0.171(4) 0.075(2) -0.003(3) 0.032(2) -0.046(2) Cl(4) 0.074(1) 0.051(1) 0.079(2) -0.011(1) -0.017(1) 0.016(1) Cl(5) 0.53(1) 0.186(8) 0.47(1) -0.124(8) 0.30(1) -0.094(8) S(1) 0.047(1) 0.043(1) 0.039(1) -0.006(1) -0.002(1) 0.008(1) S(2) 0.028(1) 0.041(1) 0.059(1) -0.0048(9) -0.0074(9) 0.001(1) S(3) 0.032(1) 0.037(1) 0.041(1) -0.0050(8) -0.0078(8) 0.0096(9) S(4) 0.029(1) 0.038(1) 0.044(1) -0.0028(8) -0.0111(9) 0.0087(9) S(5) 0.029(1) 0.038(1) 0.044(1) -0.0034(8) -0.0073(9) 0.0094(9) S(6) 0.032(1) 0.035(1) 0.039(1) -0.0027(8) -0.0072(9) 0.0089(9) S(7) 0.040(1) 0.049(1) 0.057(1) -0.012(1) -0.012(1) 0.008(1) S(8) 0.060(1) 0.039(1) 0.050(1) -0.003(1) -0.011(1) 0.014(1) S(9) 0.049(1) 0.042(1) 0.042(1) -0.004(1) -0.003(1) 0.008(1) S(10) 0.035(1) 0.047(1) 0.050(1) -0.0052(9) -0.0093(9) 0.000(1) S(11) 0.033(1) 0.037(1) 0.042(1) -0.0038(8) -0.0102(9) 0.0110(9) S(12) 0.031(1) 0.038(1) 0.040(1) -0.0048(8) -0.0099(9) 0.0049(9) S(13) 0.031(1) 0.039(1) 0.043(1) -0.0045(8) -0.0097(9) 0.008(1) S(14) 0.033(1) 0.035(1) 0.042(1) 0.0016(8) -0.0090(9) 0.0067(9) S(15) 0.041(1) 0.037(1) 0.055(1) -0.006(1) -0.010(1) 0.002(1) S(16) 0.051(1) 0.036(1) 0.040(1) 0.001(1) -0.006(1) 0.007(1) S(17) 0.054(1) 0.044(1) 0.048(1) -0.010(1) -0.013(1) 0.016(1) S(18) 0.038(1) 0.038(1) 0.057(1) -0.0058(9) -0.008(1) 0.008(1) S(19) 0.033(1) 0.040(1) 0.037(1) -0.0031(9) -0.0043(8) 0.0117(9) S(20) 0.028(1) 0.034(1) 0.045(1) -0.0034(8) -0.0073(8) 0.0084(9) S(21) 0.030(1) 0.042(1) 0.041(1) -0.0052(9) -0.0094(9) 0.010(1) S(22) 0.031(1) 0.035(1) 0.043(1) -0.0033(8) -0.0059(9) 0.0104(9) S(23) 0.038(1) 0.049(1) 0.063(2) -0.011(1) -0.013(1) 0.013(1) S(24) 0.045(1) 0.050(1) 0.052(1) -0.011(1) -0.007(1) 0.014(1) C(1) 0.076(6) 0.041(5) 0.051(6) -0.007(5) 0.006(5) 0.013(5) C(2) 0.071(6) 0.039(5) 0.079(7) -0.035(5) 0.004(5) -0.006(5) C(3) 0.053(5) 0.043(5) 0.081(7) -0.009(4) -0.014(5) -0.006(5) C(4) 0.032(4) 0.037(4) 0.031(4) -0.002(3) -0.003(3) -0.001(4) C(5) 0.025(4) 0.032(4) 0.031(4) -0.002(3) -0.007(3) 0.004(3) C(6) 0.028(4) 0.035(4) 0.038(5) -0.001(3) -0.001(3) 0.000(4) C(7) 0.020(3) 0.038(4) 0.038(4) -0.003(3) 0.002(3) -0.004(4) C(8) 0.034(4) 0.027(4) 0.031(4) 0.001(3) 0.000(3) 0.006(3) C(9) 0.036(4) 0.040(5) 0.034(4) -0.005(4) -0.003(3) 0.007(4) C(10) 0.069(6) 0.053(6) 0.060(6) -0.015(5) -0.001(5) -0.003(5) C(11) 0.077(7) 0.046(6) 0.065(7) -0.013(5) 0.007(6) -0.010(5) C(12) 0.094(7) 0.049(6) 0.057(6) 0.025(5) 0.025(6) 0.016(5) C(13) 0.069(6) 0.030(4) 0.048(5) 0.000(4) 0.006(4) 0.003(4) C(14) 0.075(6) 0.024(4) 0.052(6) -0.014(4) 0.011(5) -0.011(4) C(15) 0.056(5) 0.058(6) 0.045(5) -0.007(5) 0.000(4) -0.019(5) C(16) 0.034(4) 0.033(4) 0.042(5) -0.002(3) -0.001(4) -0.005(4) C(17) 0.028(4) 0.023(4) 0.029(4) 0.007(3) 0.004(3) 0.002(3) C(18) 0.030(4) 0.032(4) 0.036(4) -0.001(3) -0.001(3) 0.003(3) C(19) 0.025(4) 0.037(4) 0.031(4) 0.003(3) -0.008(3) 0.002(3) C(20) 0.038(4) 0.035(4) 0.031(4) 0.001(3) -0.009(3) 0.002(4) C(21) 0.038(4) 0.027(4) 0.030(4) -0.001(3) 0.001(3) 0.003(3) C(22) 0.048(5) 0.053(6) 0.048(5) -0.015(4) 0.002(4) -0.018(4) C(23) 0.061(6) 0.039(5) 0.069(7) -0.008(4) 0.004(5) -0.007(5) C(24) 0.065(6) 0.027(4) 0.061(6) 0.003(4) 0.003(5) 0.014(4) C(25) 0.077(6) 0.032(5) 0.047(5) -0.008(4) 0.007(5) 0.016(4) C(26) 0.072(6) 0.043(5) 0.053(6) -0.005(5) 0.003(5) -0.009(5) C(27) 0.062(6) 0.050(5) 0.037(5) -0.014(4) -0.004(4) -0.002(4) C(28) 0.029(4) 0.034(4) 0.050(5) 0.004(3) -0.002(4) 0.003(4) C(29) 0.024(4) 0.038(4) 0.031(4) -0.003(3) 0.003(3) -0.000(3) C(30) 0.039(4) 0.017(3) 0.038(4) -0.004(3) 0.001(3) 0.005(3) C(31) 0.029(4) 0.027(4) 0.033(4) 0.003(3) -0.002(3) -0.003(3) C(32) 0.027(4) 0.026(4) 0.045(5) 0.005(3) 0.004(3) -0.006(4) C(33) 0.031(4) 0.037(4) 0.038(5) 0.002(3) 0.006(3) 0.001(4) C(34) 0.113(9) 0.040(6) 0.094(8) -0.034(6) -0.016(7) -0.010(6) C(35) 0.100(9) 0.065(7) 0.069(8) -0.024(6) 0.003(6) 0.008(6) C(36) 0.114(8) 0.032(5) 0.077(7) -0.005(6) -0.026(7) 0.007(5) #============================================================================== # REFINEMENT DATA _refine_special_details ; We used a rigid model for the phenyl ring of the solvent molecule, PhCl (C37-C42 and H37-H41) because of a heavy disorder of PhCl. In the model, the C-C and C-H bond length were fixed at 1.395 and 0.95 \%A, respectively. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'refine Flack parameter' _refine_ls_abs_structure_Flack 0.158(1) _refine_ls_number_reflns 5465 _refine_ls_number_parameters 601 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_all 0.0540 _refine_ls_wR_factor_ref 0.0540 _refine_ls_goodness_of_fit_all 1.633 _refine_ls_goodness_of_fit_ref 1.630 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.66 _refine_diff_density_max 0.81 #============================================================================== _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 GA1 CL1 2.158(3) . . ? GA1 CL2 2.161(4) . . ? GA1 CL3 2.144(4) . . ? GA1 CL4 2.165(3) . . ? S1 C1 1.81(1) . . ? S1 C4 1.752(9) . . ? S2 C3 1.81(1) . . ? S2 C4 1.748(9) . . ? S3 C5 1.764(8) . . ? S3 C6 1.71(1) . . ? S4 C5 1.755(9) . . ? S4 C7 1.735(9) . . ? S5 C6 1.748(9) . . ? S5 C8 1.778(9) . . ? S6 C7 1.73(1) . . ? S6 C8 1.756(9) . . ? S7 C9 1.761(9) . . ? S7 C10 1.79(1) . . ? S8 C9 1.76(1) . . ? S8 C12 1.81(1) . . ? S9 C13 1.83(1) . . ? S9 C16 1.76(1) . . ? S10 C15 1.83(1) . . ? S10 C16 1.753(9) . . ? S11 C17 1.759(9) . . ? S11 C18 1.752(9) . . ? S12 C17 1.773(9) . . ? S12 C19 1.739(9) . . ? S13 C18 1.746(9) . . ? S13 C20 1.771(9) . . ? S14 C19 1.76(1) . . ? S14 C20 1.772(9) . . ? S15 C21 1.781(9) . . ? S15 C22 1.80(1) . . ? S16 C21 1.770(9) . . ? S16 C24 1.81(1) . . ? S17 C25 1.81(1) . . ? S17 C28 1.75(1) . . ? S18 C27 1.82(1) . . ? S18 C28 1.733(9) . . ? S19 C29 1.775(9) . . ? S19 C30 1.748(9) . . ? S20 C29 1.765(9) . . ? S20 C31 1.727(9) . . ? S21 C30 1.713(9) . . ? S21 C32 1.75(1) . . ? S22 C31 1.734(9) . . ? S22 C32 1.748(9) . . ? S23 C33 1.740(9) . . ? S23 C34 1.75(1) . . ? S24 C33 1.74(1) . . ? S24 C36 1.78(1) . . ? C1 C2 1.50(2) . . ? C1 H1 0.97 . . no C1 H2 0.90 . . no C2 C3 1.54(2) . . ? C2 H3 0.91 . . no C2 H4 0.90 . . no C3 H5 0.97 . . no C3 H6 0.92 . . no C4 C5 1.35(1) . . ? C6 C7 1.36(1) . . ? C8 C9 1.33(1) . . ? C10 C11 1.49(2) . . ? C10 H7 0.93 . . no C10 H8 0.96 . . no C11 C12 1.53(2) . . ? C11 H9 0.99 . . no C11 H10 0.90 . . no C12 H11 0.97 . . no C12 H12 0.91 . . no C13 C14 1.52(1) . . ? C13 H13 0.96 . . no C13 H14 0.92 . . no C14 C15 1.51(2) . . ? C14 H15 0.90 . . no C14 H16 1.05 . . no C15 H17 0.97 . . no C15 H18 0.95 . . no C16 C17 1.33(1) . . ? C18 C19 1.32(1) . . ? C20 C21 1.31(1) . . ? C22 C23 1.52(2) . . ? C22 H19 0.99 . . no C22 H20 0.95 . . no C23 C24 1.50(1) . . ? C23 H21 0.95 . . no C23 H22 1.13 . . no C24 H23 1.02 . . no C24 H24 0.87 . . no C25 C26 1.53(2) . . ? C25 H25 0.86 . . no C25 H26 0.96 . . no C26 C27 1.50(1) . . ? C26 H27 0.91 . . no C26 H28 1.01 . . no C27 H29 0.99 . . no C27 H30 1.00 . . no C28 C29 1.34(1) . . ? C30 C31 1.34(1) . . ? C32 C33 1.37(1) . . ? C34 C35 1.48(2) . . ? C34 H31 0.90 . . no C34 H32 0.96 . . no C35 C36 1.49(2) . . ? C35 H33 1.01 . . no C35 H34 0.94 . . no C36 H35 0.97 . . no C36 H36 0.93 . . no #------------------------------------------------------------------------------ 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 CL1 GA1 CL2 109.5(2) . . . ? CL1 GA1 CL3 108.3(2) . . . ? CL1 GA1 CL4 109.0(1) . . . ? CL2 GA1 CL3 108.7(2) . . . ? CL2 GA1 CL4 110.8(1) . . . ? CL3 GA1 CL4 110.5(2) . . . ? C1 S1 C4 100.9(5) . . . ? C3 S2 C4 102.4(5) . . . ? C5 S3 C6 94.1(4) . . . ? C5 S4 C7 94.3(4) . . . ? C6 S5 C8 94.1(4) . . . ? C7 S6 C8 94.2(4) . . . ? C9 S7 C10 100.0(5) . . . ? C9 S8 C12 98.9(5) . . . ? C13 S9 C16 99.7(5) . . . ? C15 S10 C16 100.4(5) . . . ? C17 S11 C18 94.2(4) . . . ? C17 S12 C19 93.4(4) . . . ? C18 S13 C20 93.8(4) . . . ? C19 S14 C20 94.2(4) . . . ? C21 S15 C22 100.7(5) . . . ? C21 S16 C24 99.7(5) . . . ? C25 S17 C28 98.0(5) . . . ? C27 S18 C28 99.8(5) . . . ? C29 S19 C30 93.8(4) . . . ? C29 S20 C31 93.8(4) . . . ? C30 S21 C32 93.6(4) . . . ? C31 S22 C32 94.3(4) . . . ? C33 S23 C34 103.5(6) . . . ? C33 S24 C36 101.8(5) . . . ? S1 C1 C2 115.0(8) . . . ? S1 C1 H1 108.6 . . . no S1 C1 H2 112.1 . . . no C2 C1 H1 104.7 . . . no C2 C1 H2 103.7 . . . no H1 C1 H2 112.6 . . . no C1 C2 C3 113.1(9) . . . ? C1 C2 H3 107.5 . . . no C1 C2 H4 106.9 . . . no C3 C2 H3 105.3 . . . no C3 C2 H4 106.6 . . . no H3 C2 H4 117.6 . . . no S2 C3 C2 113.6(8) . . . ? S2 C3 H5 107.8 . . . no S2 C3 H6 109.6 . . . no C2 C3 H5 104.7 . . . no C2 C3 H6 110.9 . . . no H5 C3 H6 110.0 . . . no S1 C4 S2 122.3(5) . . . ? S1 C4 C5 118.9(6) . . . ? S2 C4 C5 118.0(7) . . . ? S3 C5 S4 115.6(5) . . . ? S3 C5 C4 121.7(7) . . . ? S4 C5 C4 122.6(6) . . . ? S3 C6 S5 124.3(5) . . . ? S3 C6 C7 118.8(7) . . . ? S5 C6 C7 116.9(7) . . . ? S4 C7 S6 124.0(5) . . . ? S4 C7 C6 117.1(7) . . . ? S6 C7 C6 118.9(7) . . . ? S5 C8 S6 115.6(5) . . . ? S5 C8 C9 121.7(7) . . . ? S6 C8 C9 122.8(7) . . . ? S7 C9 S8 119.7(6) . . . ? S7 C9 C8 120.0(7) . . . ? S8 C9 C8 120.0(7) . . . ? S7 C10 C11 114.4(8) . . . ? S7 C10 H7 112.8 . . . no S7 C10 H8 111.1 . . . no C11 C10 H7 106.5 . . . no C11 C10 H8 101.5 . . . no H7 C10 H8 109.9 . . . no C10 C11 C12 114(1) . . . ? C10 C11 H9 107.5 . . . no C10 C11 H10 112.2 . . . no C12 C11 H9 103.6 . . . no C12 C11 H10 109.0 . . . no H9 C11 H10 109.6 . . . no S8 C12 C11 113.7(8) . . . ? S8 C12 H11 108.9 . . . no S8 C12 H12 110.4 . . . no C11 C12 H11 104.5 . . . no C11 C12 H12 108.6 . . . no H11 C12 H12 110.7 . . . no S9 C13 C14 113.5(7) . . . ? S9 C13 H13 103.3 . . . no S9 C13 H14 105.2 . . . no C14 C13 H13 107.6 . . . no C14 C13 H14 115.7 . . . no H13 C13 H14 110.9 . . . no C13 C14 C15 115.6(9) . . . ? C13 C14 H15 109.2 . . . no C13 C14 H16 103.7 . . . no C15 C14 H15 114.2 . . . no C15 C14 H16 107.9 . . . no H15 C14 H16 105.2 . . . no S10 C15 C14 114.1(7) . . . ? S10 C15 H17 103.3 . . . no S10 C15 H18 104.4 . . . no C14 C15 H17 114.1 . . . no C14 C15 H18 112.8 . . . no H17 C15 H18 107.2 . . . no S9 C16 S10 118.9(6) . . . ? S9 C16 C17 119.4(7) . . . ? S10 C16 C17 121.6(7) . . . ? S11 C17 S12 115.4(5) . . . ? S11 C17 C16 122.7(7) . . . ? S12 C17 C16 121.8(7) . . . ? S11 C18 S13 123.3(5) . . . ? S11 C18 C19 117.4(7) . . . ? S13 C18 C19 119.3(7) . . . ? S12 C19 S14 123.0(5) . . . ? S12 C19 C18 119.5(7) . . . ? S14 C19 C18 117.5(6) . . . ? S13 C20 S14 115.2(5) . . . ? S13 C20 C21 122.4(7) . . . ? S14 C20 C21 122.4(7) . . . ? S15 C21 S16 118.1(5) . . . ? S15 C21 C20 120.4(7) . . . ? S16 C21 C20 121.1(7) . . . ? S15 C22 C23 114.4(7) . . . ? S15 C22 H19 111.4 . . . no S15 C22 H20 113.1 . . . no C23 C22 H19 100.6 . . . no C23 C22 H20 110.6 . . . no H19 C22 H20 105.7 . . . no C22 C23 C24 115.7(9) . . . ? C22 C23 H21 117.0 . . . no C22 C23 H22 102.9 . . . no C24 C23 H21 115.2 . . . no C24 C23 H22 105.9 . . . no H21 C23 H22 96.5 . . . no S16 C24 C23 114.7(7) . . . ? S16 C24 H23 105.5 . . . no S16 C24 H24 113.4 . . . no C23 C24 H23 107.1 . . . no C23 C24 H24 106.0 . . . no H23 C24 H24 109.9 . . . no S17 C25 C26 114.0(8) . . . ? S17 C25 H25 107.5 . . . no S17 C25 H26 102.8 . . . no C26 C25 H25 110.1 . . . no C26 C25 H26 105.6 . . . no H25 C25 H26 116.9 . . . no C25 C26 C27 112.3(9) . . . ? C25 C26 H27 111.5 . . . no C25 C26 H28 110.7 . . . no C27 C26 H27 111.3 . . . no C27 C26 H28 102.7 . . . no H27 C26 H28 107.8 . . . no S18 C27 C26 115.8(7) . . . ? S18 C27 H29 107.9 . . . no S18 C27 H30 107.4 . . . no C26 C27 H29 113.2 . . . no C26 C27 H30 109.7 . . . no H29 C27 H30 101.8 . . . no S17 C28 S18 122.7(6) . . . ? S17 C28 C29 118.4(7) . . . ? S18 C28 C29 118.7(7) . . . ? S19 C29 S20 115.2(5) . . . ? S19 C29 C28 122.5(7) . . . ? S20 C29 C28 122.3(7) . . . ? S19 C30 S21 123.0(5) . . . ? S19 C30 C31 117.3(7) . . . ? S21 C30 C31 119.7(7) . . . ? S20 C31 S22 123.8(5) . . . ? S20 C31 C30 119.4(7) . . . ? S22 C31 C30 116.7(7) . . . ? S21 C32 S22 115.7(5) . . . ? S21 C32 C33 122.3(7) . . . ? S22 C32 C33 121.9(7) . . . ? S23 C33 S24 123.9(6) . . . ? S23 C33 C32 117.5(7) . . . ? S24 C33 C32 117.4(7) . . . ? S23 C34 C35 118.3(9) . . . ? S23 C34 H31 113.8 . . . no S23 C34 H32 110.0 . . . no C35 C34 H31 101.7 . . . no C35 C34 H32 98.9 . . . no H31 C34 H32 113.3 . . . no C34 C35 C36 117(1) . . . ? C34 C35 H33 105.2 . . . no C34 C35 H34 110.4 . . . no C36 C35 H33 107.2 . . . no C36 C35 H34 110.9 . . . no H33 C35 H34 105.4 . . . no S24 C36 C35 116.4(9) . . . ? S24 C36 H35 108.2 . . . no S24 C36 H36 111.4 . . . no C35 C36 H35 104.6 . . . no C35 C36 H36 106.9 . . . no H35 C36 H36 108.9 . . . no #------------------------------------------------------------------------------ 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 S1 C30 3.554(9) . 1_456 no S1 S18 3.647(4) . 1_556 no S2 S11 3.386(3) . 1_455 no S2 C31 3.553(9) . 1_456 no S2 S13 3.685(4) . 1_455 no S3 S20 3.614(3) . 1_556 no S3 S18 3.635(4) . 1_556 no S4 S13 3.492(3) . 1_455 no S5 S20 3.563(3) . 1_556 no S5 C18 3.62(1) . . no S5 S22 3.617(3) . 1_556 no S6 S15 3.397(3) . 1_455 no S6 C19 3.607(9) . . no S7 S24 3.666(4) . 1_556 no S7 S22 3.685(4) . 1_556 no S9 C27 3.52(1) . 1_556 no S10 S19 3.427(3) . 1_455 no S11 C6 3.67(1) . . no S12 S21 3.505(3) . 1_455 no S12 C7 3.633(9) . . no S13 C30 3.69(1) . . no S14 S23 3.402(3) . 1_455 no S14 C31 3.661(9) . . no S16 C10 3.60(1) . 1_554 no S19 C18 3.63(1) . . no S20 C19 3.59(1) . . no S23 C6 3.59(1) . 1_654 no S24 C7 3.615(9) . 1_654 no C4 C30 3.69(1) . 1_456 no C5 C16 3.59(1) . . no C5 C32 3.63(1) . 1_456 no C20 C31 3.67(1) . . no C20 C30 3.69(1) . . no C21 C32 3.60(1) . . no #============================================================================== # End of CIF #==============================================================================