Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _publ_contact_author_name ; Jun-ichi Yamada ; _publ_contact_author_address ; Department of Material Science Faculty of Science Himeji Institute Institute of Technology Kouto 3-2-1, Kamigori-cho, Ako-gun, Hyogo 678-1297 Japan ; _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_section_title ; A new organic metal exhibiting antiferromagnetism, beta-(BDA-TTP)2FeCl4 [BDA-TTP = 2,5-bis(1,3-dithian-2-ylidene)-1,3,4,6-tetrathiapentalene] ; _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Akutsu, Hiroki' 'Ikemoto, Isao' 'Kikuchi, Koichi' 'Nakatsuji, Shinichi' 'Nishikawa, Hiroyuki' 'Toita, Takashi' 'Yamada, Jun-ichi' _publ_section_comment ; The study of the titled structure was undertaken to establish its three dimensional structure. Geometries are tabulated below. All Diagrams and calculations were performed using teXsan for Windows. ; _publ_section_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. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; data_(BDA-TTP)2FeCl4 _database_code_CSD 166357 _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows' _computing_structure_solution ; SIR88 (Burla, et. al. 1989) ; _computing_structure_refinement 'teXsan for Windows' _computing_publication_material 'teXsan for Windows' #--------------------------------------------------------------------------- _cell_length_a 12.452(7) _cell_length_b 38.72(1) _cell_length_c 7.731(4) _cell_angle_alpha 90 _cell_angle_beta 91.17(4) _cell_angle_gamma 90 _cell_volume 3727(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.1 _cell_measurement_theta_max 16.6 #--------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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' #--------------------------------------------------------------------------- _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1023.07 _chemical_formula_sum 'C24 H24 Cl4 Fe S16 ' _exptl_crystal_F_000 2072.00 _exptl_absorpt_coefficient_mu 1.609 _exptl_absorpt_correction_type ; ?y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.748 _exptl_special_details ; The scan width was (1.73+0.30tan?q)?% with an ?w scan speed of 0?% per minute (up to 3 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_ambient_temperature 295 _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 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 -2 2 0 -2 0 0 -2 3 0 _diffrn_reflns_number 9069 _reflns_number_total 8692 _reflns_number_gt 4289 _reflns_threshold_expression I>3.00?s(I) _diffrn_reflns_av_R_equivalents 0.04421 _diffrn_reflns_av_sigmaI/netI 0.095 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.76 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05113 _diffrn_orient_matrix_UB_12 0.00493 _diffrn_orient_matrix_UB_13 0.09500 _diffrn_orient_matrix_UB_21 0.01896 _diffrn_orient_matrix_UB_22 0.02507 _diffrn_orient_matrix_UB_23 -0.00531 _diffrn_orient_matrix_UB_31 -0.05897 _diffrn_orient_matrix_UB_32 0.00376 _diffrn_orient_matrix_UB_33 -0.08767 #--------------------------------------------------------------------------- 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) ; Fe 0 4 0.301 0.845 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 16 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 Fe(1) 0.61028(4) -0.25135(1) 0.61935(8) 0.0369(2) 1.000 . Uani d ? Cl(1) 0.70144(9) -0.27859(3) 0.8205(2) 0.0627(4) 1.000 . Uani d ? Cl(2) 0.5188(1) -0.28916(4) 0.4707(2) 0.0876(5) 1.000 . Uani d ? Cl(3) 0.50633(9) -0.21328(3) 0.7411(2) 0.0727(4) 1.000 . Uani d ? Cl(4) 0.71980(9) -0.22436(3) 0.4500(2) 0.0642(4) 1.000 . Uani d ? S(1) 0.04417(7) 0.13639(3) 1.0767(1) 0.0392(3) 1.000 . Uani d ? S(2) 0.28690(8) 0.15086(2) 1.0920(1) 0.0385(3) 1.000 . Uani d ? S(3) 0.09301(7) 0.05936(2) 0.9884(1) 0.0353(3) 1.000 . Uani d ? S(4) 0.32875(7) 0.07383(2) 0.9966(1) 0.0357(3) 1.000 . Uani d ? S(5) 0.13693(7) -0.01349(2) 0.8573(1) 0.0363(3) 1.000 . Uani d ? S(6) 0.37191(7) 0.00063(2) 0.8682(1) 0.0355(3) 1.000 . Uani d ? S(7) 0.17639(8) -0.09012(2) 0.7800(1) 0.0450(3) 1.000 . Uani d ? S(8) 0.42096(8) -0.07529(3) 0.7811(2) 0.0479(3) 1.000 . Uani d ? S(9) 0.53669(7) 0.13555(2) 0.8303(1) 0.0364(3) 1.000 . Uani d ? S(10) 0.77809(7) 0.15208(2) 0.8263(1) 0.0365(3) 1.000 . Uani d ? S(11) 0.58809(7) 0.05912(2) 0.7344(1) 0.0342(3) 1.000 . Uani d ? S(12) 0.82329(7) 0.07450(2) 0.7441(1) 0.0344(3) 1.000 . Uani d ? S(13) 0.63535(7) -0.01391(2) 0.6084(1) 0.0352(3) 1.000 . Uani d ? S(14) 0.86982(7) 0.00191(2) 0.6145(1) 0.0358(3) 1.000 . Uani d ? S(15) 0.67942(8) -0.08965(3) 0.5197(2) 0.0515(3) 1.000 . Uani d ? S(16) 0.92394(8) -0.07373(3) 0.5300(2) 0.0467(3) 1.000 . Uani d ? C(1) 0.0429(3) 0.1794(1) 0.9855(6) 0.049(1) 1.000 . Uani d ? C(2) 0.1320(3) 0.2023(1) 1.0522(6) 0.050(1) 1.000 . Uani d ? C(3) 0.2414(3) 0.1909(1) 0.9930(6) 0.045(1) 1.000 . Uani d ? C(4) 0.1782(3) 0.12345(9) 1.0464(4) 0.029(1) 1.000 . Uani d ? C(5) 0.1971(3) 0.09021(9) 1.0122(4) 0.028(1) 1.000 . Uani d ? C(6) 0.1796(3) 0.02733(8) 0.9177(4) 0.030(1) 1.000 . Uani d ? C(7) 0.2852(3) 0.03344(8) 0.9245(4) 0.028(1) 1.000 . Uani d ? C(8) 0.2680(3) -0.02940(8) 0.8313(5) 0.029(1) 1.000 . Uani d ? C(9) 0.2866(3) -0.06238(9) 0.7870(4) 0.031(1) 1.000 . Uani d ? C(10) 0.2205(3) -0.12781(9) 0.6666(5) 0.036(1) 1.000 . Uani d ? C(11) 0.3315(3) -0.14049(9) 0.7218(5) 0.036(1) 1.000 . Uani d ? C(12) 0.4217(3) -0.1169(1) 0.6783(5) 0.036(1) 1.000 . Uani d ? C(13) 0.5281(3) 0.1788(1) 0.7348(6) 0.048(1) 1.000 . Uani d ? C(14) 0.6181(3) 0.2027(1) 0.7978(5) 0.045(1) 1.000 . Uani d ? C(15) 0.7263(3) 0.1917(1) 0.7336(5) 0.042(1) 1.000 . Uani d ? C(16) 0.6698(3) 0.12382(9) 0.7888(4) 0.027(1) 1.000 . Uani d ? C(17) 0.6911(3) 0.09047(8) 0.7574(4) 0.028(1) 1.000 . Uani d ? C(18) 0.6765(3) 0.02751(8) 0.6680(4) 0.028(1) 1.000 . Uani d ? C(19) 0.7814(3) 0.03428(8) 0.6710(4) 0.028(1) 1.000 . Uani d ? C(20) 0.7679(3) -0.02868(9) 0.5789(5) 0.032(1) 1.000 . Uani d ? C(21) 0.7887(3) -0.06172(9) 0.5330(4) 0.029(1) 1.000 . Uani d ? C(22) 0.7271(3) -0.1279(1) 0.4147(5) 0.040(1) 1.000 . Uani d ? C(23) 0.8385(3) -0.13929(9) 0.4677(5) 0.036(1) 1.000 . Uani d ? C(24) 0.9263(3) -0.11466(9) 0.4201(5) 0.036(1) 1.000 . Uani d ? H(1) 0.060(2) 0.1768(8) 0.823(4) 0.051 1.000 . Uiso d ? H(2) -0.007(3) 0.1876(9) 1.008(4) 0.051 1.000 . Uiso d ? H(3) 0.128(2) 0.2246(8) 1.019(4) 0.051 1.000 . Uiso d ? H(4) 0.126(3) 0.2016(8) 1.182(4) 0.051 1.000 . Uiso d ? H(5) 0.293(3) 0.2050(8) 1.032(4) 0.051 1.000 . Uiso d ? H(6) 0.233(2) 0.1889(8) 0.836(4) 0.051 1.000 . Uiso d ? H(7) 0.167(2) -0.1474(8) 0.722(4) 0.051 1.000 . Uiso d ? H(8) 0.209(2) -0.1175(8) 0.529(4) 0.051 1.000 . Uiso d ? H(9) 0.328(3) -0.1455(8) 0.840(4) 0.051 1.000 . Uiso d ? H(10) 0.349(2) -0.1649(8) 0.672(4) 0.051 1.000 . Uiso d ? H(11) 0.424(3) -0.1141(8) 0.546(4) 0.051 1.000 . Uiso d ? H(12) 0.490(3) -0.1253(9) 0.705(4) 0.051 1.000 . Uiso d ? H(13) 0.541(3) 0.1768(9) 0.621(4) 0.051 1.000 . Uiso d ? H(14) 0.472(3) 0.1868(9) 0.772(4) 0.051 1.000 . Uiso d ? H(15) 0.611(2) 0.2259(8) 0.740(4) 0.051 1.000 . Uiso d ? H(16) 0.607(2) 0.2035(8) 0.937(4) 0.051 1.000 . Uiso d ? H(17) 0.775(3) 0.2057(8) 0.775(4) 0.051 1.000 . Uiso d ? H(18) 0.730(3) 0.1915(8) 0.607(4) 0.051 1.000 . Uiso d ? H(19) 0.674(3) -0.1445(8) 0.459(4) 0.051 1.000 . Uiso d ? H(20) 0.709(3) -0.1256(9) 0.297(4) 0.051 1.000 . Uiso d ? H(21) 0.828(3) -0.1452(8) 0.577(4) 0.051 1.000 . Uiso d ? H(22) 0.855(2) -0.1635(8) 0.402(4) 0.051 1.000 . Uiso d ? H(23) 0.919(3) -0.1111(8) 0.308(4) 0.051 1.000 . Uiso d ? H(24) 1.017(3) -0.1201(8) 0.459(4) 0.051 1.000 . 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 Fe(1) 0.0330(3) 0.0316(3) 0.0462(3) 0.0001(3) 0.0037(3) -0.0010(3) Cl(1) 0.0616(7) 0.0496(7) 0.0766(8) 0.0091(6) -0.0069(6) 0.0183(6) Cl(2) 0.0623(8) 0.103(1) 0.098(1) -0.0378(7) 0.0082(7) -0.0433(8) Cl(3) 0.0640(8) 0.0728(8) 0.0819(9) 0.0326(6) 0.0164(7) -0.0052(7) Cl(4) 0.0651(8) 0.0507(7) 0.0778(9) -0.0092(6) 0.0258(6) 0.0123(6) S(1) 0.0277(5) 0.0374(6) 0.0528(7) 0.0015(4) 0.0075(5) 0.0007(5) S(2) 0.0320(5) 0.0322(5) 0.0513(7) -0.0040(4) 0.0016(5) -0.0021(5) S(3) 0.0239(5) 0.0282(5) 0.0540(7) -0.0018(4) 0.0027(5) 0.0023(5) S(4) 0.0239(5) 0.0287(5) 0.0544(7) -0.0019(4) 0.0005(5) 0.0003(5) S(5) 0.0236(5) 0.0279(5) 0.0574(7) -0.0025(4) -0.0006(5) 0.0005(5) S(6) 0.0235(5) 0.0300(5) 0.0529(7) -0.0010(4) 0.0014(5) -0.0006(5) S(7) 0.0264(5) 0.0322(5) 0.0768(8) -0.0033(5) 0.0055(5) -0.0097(6) S(8) 0.0243(5) 0.0386(6) 0.0807(9) 0.0005(5) 0.0029(5) -0.0096(6) S(9) 0.0273(5) 0.0321(5) 0.0501(7) 0.0021(4) 0.0054(5) -0.0002(5) S(10) 0.0303(5) 0.0299(5) 0.0493(7) -0.0054(4) -0.0004(5) -0.0034(5) S(11) 0.0251(5) 0.0252(5) 0.0525(7) -0.0003(4) 0.0053(5) -0.0014(5) S(12) 0.0238(5) 0.0286(5) 0.0506(7) -0.0021(4) 0.0012(5) -0.0019(5) S(13) 0.0247(5) 0.0253(5) 0.0556(7) -0.0011(4) 0.0026(5) -0.0016(5) S(14) 0.0251(5) 0.0288(5) 0.0536(7) 0.0006(4) 0.0057(5) -0.0024(5) S(15) 0.0286(6) 0.0330(6) 0.0932(9) -0.0029(5) 0.0073(6) -0.0162(6) S(16) 0.0262(5) 0.0350(6) 0.0789(9) 0.0011(5) 0.0015(6) -0.0118(6) C(1) 0.039(3) 0.043(2) 0.064(3) 0.009(2) 0.003(2) 0.010(2) C(2) 0.060(3) 0.030(2) 0.062(3) 0.007(2) 0.003(2) -0.000(2) C(3) 0.045(3) 0.036(2) 0.053(3) -0.009(2) 0.001(2) 0.005(2) C(4) 0.028(2) 0.031(2) 0.030(2) -0.000(2) 0.000(2) 0.001(2) C(5) 0.019(2) 0.032(2) 0.034(2) -0.005(2) 0.002(2) 0.003(2) C(6) 0.031(2) 0.024(2) 0.035(2) -0.006(2) 0.001(2) 0.000(2) C(7) 0.025(2) 0.027(2) 0.033(2) -0.000(2) 0.005(2) 0.007(2) C(8) 0.021(2) 0.027(2) 0.038(2) -0.003(2) -0.001(2) 0.002(2) C(9) 0.019(2) 0.037(2) 0.035(2) -0.002(2) -0.001(2) 0.003(2) C(10) 0.035(2) 0.033(2) 0.039(2) 0.002(2) -0.004(2) -0.003(2) C(11) 0.040(2) 0.031(2) 0.037(2) 0.000(2) 0.003(2) -0.001(2) C(12) 0.030(2) 0.040(2) 0.039(3) 0.006(2) 0.005(2) -0.005(2) C(13) 0.049(3) 0.037(2) 0.058(3) 0.012(2) 0.010(2) 0.006(2) C(14) 0.047(3) 0.025(2) 0.063(3) 0.000(2) 0.005(2) -0.001(2) C(15) 0.053(3) 0.032(2) 0.041(3) -0.013(2) 0.002(2) 0.006(2) C(16) 0.021(2) 0.029(2) 0.032(2) 0.002(2) -0.004(2) 0.002(2) C(17) 0.020(2) 0.028(2) 0.036(2) 0.001(2) -0.000(2) 0.002(2) C(18) 0.027(2) 0.021(2) 0.036(2) -0.002(2) 0.004(2) -0.001(2) C(19) 0.029(2) 0.023(2) 0.032(2) 0.002(2) 0.002(2) -0.000(2) C(20) 0.026(2) 0.030(2) 0.040(2) 0.002(2) 0.001(2) 0.001(2) C(21) 0.020(2) 0.032(2) 0.035(2) -0.002(2) 0.001(2) -0.000(2) C(22) 0.040(2) 0.032(2) 0.049(3) 0.003(2) -0.005(2) -0.005(2) C(23) 0.043(2) 0.029(2) 0.035(2) 0.003(2) 0.005(2) -0.002(2) C(24) 0.034(2) 0.034(2) 0.041(3) 0.007(2) 0.004(2) -0.003(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 'w = 1/[?s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef no _refine_ls_number_reflns 4289 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.0360 _refine_ls_goodness_of_fit_all 2.289 _refine_ls_goodness_of_fit_ref 2.290 _refine_ls_shift/su_max 0.1500 _refine_diff_density_min -0.54 _refine_diff_density_max 0.44 #=========================================================================== # MOLECULAR GEOMETRY 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 S1 C1 1.809(6) . . ? S1 C4 1.763(5) . . ? S2 C3 1.815(6) . . ? S2 C4 1.750(5) . . ? S3 C5 1.769(5) . . ? S3 C6 1.739(5) . . ? S4 C5 1.765(5) . . ? S4 C7 1.743(5) . . ? S5 C6 1.729(5) . . ? S5 C8 1.760(5) . . ? S6 C7 1.729(5) . . ? S6 C8 1.758(5) . . ? S7 C9 1.743(5) . . ? S7 C10 1.794(6) . . ? S8 C9 1.748(5) . . ? S8 C12 1.798(6) . . ? S9 C13 1.831(6) . . ? S9 C16 1.755(5) . . ? S10 C15 1.808(6) . . ? S10 C16 1.756(5) . . ? S11 C17 1.772(5) . . ? S11 C18 1.731(5) . . ? S12 C17 1.763(5) . . ? S12 C19 1.734(5) . . ? S13 C18 1.743(5) . . ? S13 C20 1.766(5) . . ? S14 C19 1.731(5) . . ? S14 C20 1.754(5) . . ? S15 C21 1.740(5) . . ? S15 C22 1.796(6) . . ? S16 C21 1.748(5) . . ? S16 C24 1.799(6) . . ? C1 C2 1.503(9) . . ? C1 H1 1.28(5) . . no C1 H2 0.72(5) . . no C2 C3 1.513(8) . . ? C2 H2 1.84(5) . . no C2 H3 0.90(5) . . no C2 H4 1.01(5) . . no C3 H3 1.93(5) . . no C3 H5 0.89(5) . . no C3 H6 1.22(5) . . no C4 C5 1.336(7) . . ? C6 C7 1.335(7) . . ? C8 C9 1.343(7) . . ? C10 C11 1.520(7) . . ? C10 H7 1.10(5) . . no C10 H8 1.14(5) . . no C10 H9 2.00(5) . . no C11 C12 1.491(7) . . ? C11 H9 0.94(5) . . no C11 H10 1.04(5) . . no C12 H11 1.03(5) . . no C12 H12 0.93(5) . . no C13 C14 1.528(8) . . ? C13 H13 0.90(5) . . no C13 H14 0.82(5) . . no C14 C15 1.507(8) . . ? C14 H13 1.93(5) . . no C14 H14 1.92(5) . . no C14 H15 1.01(5) . . no C14 H16 1.08(5) . . no C14 H17 1.97(5) . . no C15 H15 1.96(5) . . no C15 H17 0.87(5) . . no C15 H18 0.98(5) . . no C16 C17 1.342(7) . . ? C18 C19 1.331(7) . . ? C20 C21 1.354(7) . . ? C22 C23 1.504(8) . . ? C22 H19 0.99(5) . . no C22 H20 0.94(5) . . no C22 H21 1.88(5) . . no C23 C24 1.502(7) . . ? C23 H21 0.89(5) . . no C23 H22 1.09(5) . . no C23 H23 1.95(5) . . no C24 H23 0.88(5) . . no C24 H24 1.19(5) . . 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 C1 S1 C4 102.2(3) . . . ? C3 S2 C4 101.5(3) . . . ? C5 S3 C6 93.2(2) . . . ? C5 S4 C7 93.5(2) . . . ? C6 S5 C8 94.0(2) . . . ? C7 S6 C8 93.8(2) . . . ? C9 S7 C10 105.5(3) . . . ? C9 S8 C12 106.4(3) . . . ? C13 S9 C16 102.1(3) . . . ? C15 S10 C16 101.4(3) . . . ? C17 S11 C18 92.9(2) . . . ? C17 S12 C19 93.4(2) . . . ? C18 S13 C20 93.5(2) . . . ? C19 S14 C20 93.8(2) . . . ? C21 S15 C22 105.9(3) . . . ? C21 S16 C24 105.4(3) . . . ? S1 C1 C2 114.2(4) . . . ? S1 C1 H1 108(2) . . . no S1 C1 H2 108(4) . . . no C2 C1 H1 104(2) . . . no C2 C1 H2 107(4) . . . no H1 C1 H2 116(5) . . . no C1 C2 C3 112.8(5) . . . ? C1 C2 H2 22(2) . . . no C1 C2 H3 116(3) . . . no C1 C2 H4 105(3) . . . no C3 C2 H2 134(2) . . . no C3 C2 H3 104(3) . . . no C3 C2 H4 112(3) . . . no H2 C2 H3 102(4) . . . no H2 C2 H4 95(3) . . . no H3 C2 H4 108(4) . . . no S2 C3 C2 113.4(4) . . . ? S2 C3 H3 139(2) . . . no S2 C3 H5 99(3) . . . no S2 C3 H6 113(2) . . . no C2 C3 H3 27(1) . . . no C2 C3 H5 112(3) . . . no C2 C3 H6 105(2) . . . no H3 C3 H5 94(4) . . . no H3 C3 H6 96(3) . . . no H5 C3 H6 115(4) . . . no S1 C4 S2 122.1(3) . . . ? S1 C4 C5 118.1(4) . . . ? S2 C4 C5 119.1(4) . . . ? S3 C5 S4 115.4(3) . . . ? S3 C5 C4 122.7(4) . . . ? S4 C5 C4 121.8(4) . . . ? S3 C6 S5 123.2(3) . . . ? S3 C6 C7 118.5(4) . . . ? S5 C6 C7 118.0(4) . . . ? S4 C7 S6 123.2(3) . . . ? S4 C7 C6 118.1(4) . . . ? S6 C7 C6 118.6(4) . . . ? S5 C8 S6 115.5(3) . . . ? S5 C8 C9 121.8(4) . . . ? S6 C8 C9 122.7(4) . . . ? S7 C9 S8 125.2(3) . . . ? S7 C9 C8 117.0(4) . . . ? S8 C9 C8 116.6(4) . . . ? S7 C10 C11 114.3(4) . . . ? S7 C10 H7 100(3) . . . no S7 C10 H8 98(2) . . . no S7 C10 H9 99(1) . . . no C11 C10 H7 103(3) . . . no C11 C10 H8 118(2) . . . no C11 C10 H9 27(1) . . . no H7 C10 H8 122(4) . . . no H7 C10 H9 85(3) . . . no H8 C10 H9 145(3) . . . no C10 C11 C12 115.1(5) . . . ? C10 C11 H9 106(3) . . . no C10 C11 H10 112(3) . . . no C12 C11 H9 114(3) . . . no C12 C11 H10 108(3) . . . no H9 C11 H10 101(4) . . . no S8 C12 C11 116.0(4) . . . ? S8 C12 H11 110(3) . . . no S8 C12 H12 103(3) . . . no C11 C12 H11 109(3) . . . no C11 C12 H12 115(3) . . . no H11 C12 H12 103(4) . . . no S9 C13 C14 113.0(4) . . . ? S9 C13 H13 108(3) . . . no S9 C13 H14 105(4) . . . no C14 C13 H13 103(3) . . . no C14 C13 H14 106(4) . . . no H13 C13 H14 123(5) . . . no C13 C14 C15 112.2(5) . . . ? C13 C14 H13 27(1) . . . no C13 C14 H14 24(2) . . . no C13 C14 H15 110(3) . . . no C13 C14 H16 103(3) . . . no C13 C14 H17 137(2) . . . no C15 C14 H13 93(2) . . . no C15 C14 H14 136(2) . . . no C15 C14 H15 101(3) . . . no C15 C14 H16 118(3) . . . no C15 C14 H17 25(1) . . . no H13 C14 H14 46(2) . . . no H13 C14 H15 96(3) . . . no H13 C14 H16 130(3) . . . no H13 C14 H17 117(2) . . . no H14 C14 H15 99(3) . . . no H14 C14 H16 89(3) . . . no H14 C14 H17 161(2) . . . no H15 C14 H16 114(4) . . . no H15 C14 H17 90(3) . . . no H16 C14 H17 103(3) . . . no S10 C15 C14 115.1(4) . . . ? S10 C15 H15 145(1) . . . no S10 C15 H17 98(3) . . . no S10 C15 H18 111(3) . . . no C14 C15 H15 30(1) . . . no C14 C15 H17 109(3) . . . no C14 C15 H18 113(3) . . . no H15 C15 H17 95(4) . . . no H15 C15 H18 95(3) . . . no H17 C15 H18 109(4) . . . no S9 C16 S10 122.3(3) . . . ? S9 C16 C17 118.2(4) . . . ? S10 C16 C17 118.4(4) . . . ? S11 C17 S12 115.4(3) . . . ? S11 C17 C16 122.2(4) . . . ? S12 C17 C16 122.4(4) . . . ? S11 C18 S13 122.9(3) . . . ? S11 C18 C19 119.0(4) . . . ? S13 C18 C19 118.0(4) . . . ? S12 C19 S14 122.9(3) . . . ? S12 C19 C18 118.1(4) . . . ? S14 C19 C18 118.8(4) . . . ? S13 C20 S14 115.9(3) . . . ? S13 C20 C21 121.6(4) . . . ? S14 C20 C21 122.5(4) . . . ? S15 C21 S16 125.9(3) . . . ? S15 C21 C20 116.7(4) . . . ? S16 C21 C20 116.4(4) . . . ? S15 C22 C23 115.5(4) . . . ? S15 C22 H19 99(3) . . . no S15 C22 H20 107(3) . . . no S15 C22 H21 102(2) . . . no C23 C22 H19 110(3) . . . no C23 C22 H20 120(3) . . . no C23 C22 H21 28(1) . . . no H19 C22 H20 104(4) . . . no H19 C22 H21 89(3) . . . no H20 C22 H21 146(3) . . . no C22 C23 C24 114.7(5) . . . ? C22 C23 H21 100(3) . . . no C22 C23 H22 108(3) . . . no C22 C23 H23 99(2) . . . no C24 C23 H21 121(3) . . . no C24 C23 H22 107(3) . . . no C24 C23 H23 26(1) . . . no H21 C23 H22 105(4) . . . no H21 C23 H23 147(4) . . . no H22 C23 H23 95(3) . . . no S16 C24 C23 115.1(4) . . . ? S16 C24 H23 109(3) . . . no S16 C24 H24 93(2) . . . no C23 C24 H23 106(3) . . . no C23 C24 H24 121(2) . . . no H23 C24 H24 111(4) . . . 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 S7 3.479(2) . 3_557 no S3 S5 3.594(2) . 3_557 no S4 S8 3.529(3) . 3_657 no S5 S14 3.674(3) . 3_656 no S6 S11 3.682(2) . . no S10 C1 3.653(7) . 1_655 no S15 C12 3.616(6) . . no C5 C21 3.686(7) . 3_657 no C9 C17 3.692(7) . 3_657 no #--------------------------------------------------------------------------- #End of CIF #=========================================================================== data_(BDA-TTP)3FeCl4(PhCl) _database_code_CSD 166358 _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #--------------------------------------------------------------------------- _cell_length_a 9.780(3) _cell_length_b 35.61(3) _cell_length_c 8.843(3) _cell_angle_alpha 90 _cell_angle_beta 92.05(3) _cell_angle_gamma 90 _cell_volume 3078(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _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 ' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #--------------------------------------------------------------------------- _exptl_crystal_description 'black' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1548.34 _chemical_formula_sum 'C42 H41 Cl5 Fe S24 ' _exptl_crystal_F_000 1576.00 _exptl_absorpt_coefficient_mu 1.309 _exptl_absorpt_correction_type none #=========================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K?a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 2717 _reflns_number_total 2717 _reflns_number_gt 2592 _reflns_threshold_expression I>3.00?s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.047 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 19.94 _diffrn_reflns_reduction_process 'Lp corrections applied' #--------------------------------------------------------------------------- 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) ; Fe 0 2 0.301 0.845 ;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 Fe(1) 0.5797(1) 0.0491 0.6826(1) 0.0534(4) 1.000 . Uani d ? Cl(1) 0.6722(4) -0.00535(7) 0.7096(3) 0.134(1) 1.000 . Uani d ? Cl(2) 0.7339(3) 0.08814(8) 0.5946(3) 0.094(1) 1.000 . Uani d ? Cl(3) 0.5191(4) 0.06825(9) 0.9008(4) 0.145(2) 1.000 . Uani d ? Cl(4) 0.4032(3) 0.04658(8) 0.5235(2) 0.0718(8) 1.000 . Uani d ? Cl(5) 0.1198(7) 0.0356(1) -0.1510(7) 0.380(4) 1.000 . Uani d ? S(1) -0.0325(2) 0.20487(6) 1.0580(2) 0.0424(7) 1.000 . Uani d ? S(2) -0.2387(2) 0.23317(6) 0.8152(2) 0.0407(7) 1.000 . Uani d ? S(3) 0.1689(2) 0.26941(6) 0.9723(2) 0.0337(6) 1.000 . Uani d ? S(4) -0.0313(2) 0.29614(6) 0.7329(2) 0.0366(6) 1.000 . Uani d ? S(5) 0.3643(2) 0.33380(6) 0.8973(2) 0.0358(6) 1.000 . Uani d ? S(6) 0.1654(2) 0.36043(6) 0.6549(2) 0.0360(6) 1.000 . Uani d ? S(7) 0.5513(2) 0.40464(6) 0.8457(2) 0.0502(7) 1.000 . Uani d ? S(8) 0.3460(2) 0.43274(6) 0.6020(2) 0.0483(7) 1.000 . Uani d ? S(9) 0.2481(2) 0.18179(6) 0.7399(2) 0.0434(7) 1.000 . Uani d ? S(10) 0.0388(2) 0.20977(6) 0.5042(2) 0.0425(7) 1.000 . Uani d ? S(11) 0.4456(2) 0.24839(6) 0.6611(2) 0.0381(6) 1.000 . Uani d ? S(12) 0.2448(2) 0.27509(6) 0.4190(2) 0.0354(6) 1.000 . Uani d ? S(13) 0.6344(2) 0.31499(5) 0.5951(2) 0.0365(7) 1.000 . Uani d ? S(14) 0.4351(2) 0.34183(6) 0.3544(2) 0.0344(6) 1.000 . Uani d ? S(15) 0.8438(2) 0.37895(6) 0.5099(2) 0.0450(7) 1.000 . Uani d ? S(16) 0.6384(2) 0.40805(6) 0.2708(2) 0.0454(7) 1.000 . Uani d ? S(17) 0.5455(2) 0.15921(6) 0.3950(2) 0.0439(7) 1.000 . Uani d ? S(18) 0.3290(2) 0.19065(6) 0.1710(2) 0.0456(7) 1.000 . Uani d ? S(19) 0.7211(2) 0.23180(6) 0.3499(2) 0.0389(6) 1.000 . Uani d ? S(20) 0.5189(2) 0.25954(6) 0.1124(2) 0.0364(6) 1.000 . Uani d ? S(21) 0.9134(2) 0.29571(6) 0.2724(2) 0.0392(7) 1.000 . Uani d ? S(22) 0.7132(2) 0.32317(6) 0.0369(2) 0.0369(6) 1.000 . Uani d ? S(23) 1.1186(2) 0.36013(7) 0.1951(2) 0.0499(8) 1.000 . Uani d ? S(24) 0.9111(2) 0.38695(6) -0.0488(2) 0.0512(7) 1.000 . Uani d ? C(1) -0.093(1) 0.1603(2) 0.9838(9) 0.064(3) 1.000 . Uani d ? C(2) -0.2349(9) 0.1606(2) 0.9252(9) 0.059(3) 1.000 . Uani d ? C(3) -0.2676(9) 0.1836(2) 0.7823(8) 0.055(3) 1.000 . Uani d ? C(4) -0.0729(8) 0.2341(2) 0.9087(8) 0.040(3) 1.000 . Uani d ? C(5) 0.0091(7) 0.2632(2) 0.8691(7) 0.034(2) 1.000 . Uani d ? C(6) 0.2108(7) 0.3078(2) 0.8704(8) 0.035(2) 1.000 . Uani d ? C(7) 0.1251(8) 0.3206(2) 0.7591(8) 0.037(3) 1.000 . Uani d ? C(8) 0.3164(8) 0.3688(2) 0.7646(8) 0.038(3) 1.000 . Uani d ? C(9) 0.3933(8) 0.4016(2) 0.7444(7) 0.033(2) 1.000 . Uani d ? C(10) 0.535(1) 0.4520(3) 0.918(1) 0.071(3) 1.000 . Uani d ? C(11) 0.493(1) 0.4806(2) 0.809(1) 0.083(4) 1.000 . Uani d ? C(12) 0.357(1) 0.4758(3) 0.728(2) 0.150(5) 1.000 . Uani d ? C(13) 0.2238(9) 0.1390(2) 0.6358(7) 0.043(3) 1.000 . Uani d ? C(14) 0.0786(9) 0.1329(2) 0.5756(8) 0.044(3) 1.000 . Uani d ? C(15) 0.0412(9) 0.1616(2) 0.437(1) 0.078(3) 1.000 . Uani d ? C(16) 0.2039(7) 0.2131(2) 0.5967(7) 0.028(2) 1.000 . Uani d ? C(17) 0.2849(7) 0.2416(2) 0.5640(7) 0.031(2) 1.000 . Uani d ? C(18) 0.4884(7) 0.2898(2) 0.5613(7) 0.027(2) 1.000 . Uani d ? C(19) 0.3937(7) 0.3020(2) 0.4553(8) 0.033(2) 1.000 . Uani d ? C(20) 0.5969(8) 0.3470(2) 0.4498(9) 0.043(3) 1.000 . Uani d ? C(21) 0.6805(8) 0.3763(2) 0.4154(7) 0.042(3) 1.000 . Uani d ? C(22) 0.8469(8) 0.4280(2) 0.5739(8) 0.050(3) 1.000 . Uani d ? C(23) 0.820(1) 0.4542(2) 0.4257(9) 0.066(3) 1.000 . Uani d ? C(24) 0.6786(8) 0.4527(2) 0.3632(7) 0.042(3) 1.000 . Uani d ? C(25) 0.5172(9) 0.1185(2) 0.2783(9) 0.053(3) 1.000 . Uani d ? C(26) 0.3733(9) 0.1139(2) 0.214(1) 0.061(3) 1.000 . Uani d ? C(27) 0.3342(8) 0.1438(2) 0.0872(7) 0.039(3) 1.000 . Uani d ? C(28) 0.4895(7) 0.1931(2) 0.2663(9) 0.044(3) 1.000 . Uani d ? C(29) 0.5671(7) 0.2233(2) 0.2400(7) 0.029(2) 1.000 . Uani d ? C(30) 0.7600(7) 0.2727(2) 0.2440(7) 0.024(2) 1.000 . Uani d ? C(31) 0.6729(8) 0.2843(2) 0.1467(8) 0.033(2) 1.000 . Uani d ? C(32) 0.8743(7) 0.3294(2) 0.1401(9) 0.038(3) 1.000 . Uani d ? C(33) 0.9605(7) 0.3582(2) 0.1008(8) 0.037(3) 1.000 . Uani d ? C(34) 1.160(1) 0.4088(3) 0.1925(8) 0.070(3) 1.000 . Uani d ? C(35) 1.129(1) 0.4319(3) 0.067(1) 0.088(4) 1.000 . Uani d ? C(36) 0.989(1) 0.4317(2) 0.0070(9) 0.069(3) 1.000 . Uani d ? C(37) 0.022(3) 0.0334(9) -0.031(1) 0.76(1) 1.000 . Uani d ? C(38) -0.069(1) 0.0495(3) 0.012(1) 0.114(4) 1.000 . Uani d ? C(39) -0.124(1) 0.0555(4) 0.178(1) 0.132(5) 1.000 . Uani d ? C(40) -0.035(1) 0.0513(4) 0.2824(9) 0.174(6) 1.000 . Uani d ? C(41) 0.088(2) 0.037(1) 0.246(1) 0.91(2) 1.000 . Uani d ? C(42) 0.110(1) 0.0361(3) 0.150(2) 0.194(6) 1.000 . Uani d ? H(1) -0.0410 0.1531 0.9017 0.051 1.000 . Uiso c ? H(2) -0.0895 0.1421 1.0609 0.051 1.000 . Uiso c ? H(3) -0.2613 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 0.6202 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) -0.1103 0.0681 -0.0596 0.051 1.000 . Uiso c ? H(38) -0.2242 0.0630 0.1913 0.051 1.000 . Uiso c ? H(39) -0.0568 0.0541 0.3805 0.051 1.000 . Uiso c ? H(40) 0.1823 0.0386 0.3125 0.051 1.000 . Uiso c ? H(41) 0.2080 0.0322 0.0932 0.051 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) 0.068(1) 0.0407(7) 0.0507(7) -0.0009(7) -0.0091(7) 0.0027(7) Cl(1) 0.177(3) 0.045(2) 0.170(2) 0.031(2) -0.126(2) -0.013(2) Cl(2) 0.080(2) 0.107(2) 0.093(2) -0.023(2) -0.016(2) 0.036(2) Cl(3) 0.134(3) 0.157(3) 0.146(3) 0.000(3) 0.014(2) -0.059(2) Cl(4) 0.069(2) 0.059(1) 0.086(1) -0.014(1) -0.019(1) 0.022(2) Cl(5) 0.48(1) 0.153(6) 0.515(8) -0.112(6) 0.194(7) -0.066(5) S(1) 0.037(1) 0.042(1) 0.047(1) -0.003(1) -0.008(1) 0.011(1) S(2) 0.026(1) 0.044(1) 0.052(1) -0.008(1) -0.011(1) 0.009(1) S(3) 0.024(1) 0.039(1) 0.037(1) -0.003(1) -0.014(1) 0.014(1) S(4) 0.026(1) 0.036(1) 0.046(1) -0.003(1) -0.018(1) 0.010(1) S(5) 0.019(1) 0.039(1) 0.049(1) -0.003(1) -0.013(1) 0.010(1) S(6) 0.032(1) 0.035(1) 0.040(1) -0.004(1) -0.008(1) 0.008(1) S(7) 0.034(2) 0.051(1) 0.065(1) -0.016(1) -0.015(1) 0.009(1) S(8) 0.053(2) 0.043(1) 0.048(1) -0.005(1) -0.012(1) 0.015(1) S(9) 0.045(2) 0.040(1) 0.044(1) -0.001(1) -0.009(1) 0.013(1) S(10) 0.032(1) 0.047(1) 0.047(1) -0.007(1) -0.012(1) 0.000(1) S(11) 0.026(1) 0.039(1) 0.048(1) -0.000(1) -0.017(1) 0.010(1) S(12) 0.021(1) 0.046(1) 0.039(1) -0.006(1) -0.011(1) 0.009(1) S(13) 0.025(1) 0.039(1) 0.044(1) -0.005(1) -0.012(1) 0.014(1) S(14) 0.025(1) 0.036(1) 0.042(1) -0.000(1) -0.014(1) 0.011(1) S(15) 0.021(1) 0.039(1) 0.073(2) -0.002(1) -0.015(1) 0.005(1) S(16) 0.047(2) 0.039(1) 0.049(1) 0.004(1) -0.005(1) 0.012(1) S(17) 0.046(2) 0.046(1) 0.039(1) -0.006(1) -0.011(1) 0.015(1) S(18) 0.036(1) 0.042(1) 0.058(1) -0.006(1) -0.017(1) 0.007(1) S(19) 0.023(1) 0.039(1) 0.053(1) -0.004(1) -0.013(1) 0.011(1) S(20) 0.021(1) 0.045(1) 0.043(1) -0.007(1) -0.008(1) 0.013(1) S(21) 0.024(1) 0.042(1) 0.050(1) -0.000(1) -0.014(1) 0.012(1) S(22) 0.026(1) 0.042(1) 0.042(1) -0.004(1) -0.008(1) 0.010(1) S(23) 0.030(1) 0.058(2) 0.060(1) -0.009(1) -0.019(1) 0.014(1) S(24) 0.043(2) 0.050(1) 0.059(1) -0.013(1) -0.018(1) 0.018(1) C(1) 0.077(8) 0.029(5) 0.084(7) -0.007(5) -0.037(6) 0.002(5) C(2) 0.063(7) 0.066(7) 0.049(5) -0.020(6) 0.022(5) -0.004(5) C(3) 0.063(7) 0.058(6) 0.044(5) -0.012(5) -0.014(5) -0.013(4) C(4) 0.024(5) 0.055(5) 0.040(5) -0.014(5) -0.010(4) 0.003(4) C(5) 0.021(5) 0.058(5) 0.022(4) -0.014(5) -0.017(4) -0.006(4) C(6) 0.003(4) 0.049(5) 0.051(5) -0.010(4) 0.001(4) 0.009(4) C(7) 0.019(5) 0.050(5) 0.042(5) -0.004(4) 0.002(4) 0.001(4) C(8) 0.033(5) 0.027(5) 0.052(5) 0.007(4) -0.018(4) -0.006(4) C(9) 0.025(5) 0.054(5) 0.020(4) -0.007(4) -0.005(4) 0.032(4) C(10) 0.059(7) 0.083(7) 0.072(6) -0.006(6) 0.017(5) 0.014(6) C(11) 0.13(1) 0.018(5) 0.104(8) 0.005(6) -0.008(7) -0.015(5) C(12) 0.035(7) 0.064(7) 0.34(1) -0.035(5) -0.107(8) 0.124(7) C(13) 0.069(7) 0.052(5) 0.010(4) 0.001(5) 0.029(4) 0.005(4) C(14) 0.049(6) 0.057(6) 0.026(4) -0.004(5) -0.010(4) -0.005(4) C(15) 0.039(6) 0.064(6) 0.127(7) -0.001(5) -0.034(6) -0.070(5) C(16) 0.019(5) 0.040(5) 0.025(4) -0.008(4) 0.010(4) 0.012(4) C(17) 0.019(5) 0.068(6) 0.003(3) 0.002(4) -0.020(3) -0.005(4) C(18) 0.016(5) 0.052(5) 0.013(4) 0.013(4) -0.017(3) 0.002(3) C(19) 0.021(5) 0.033(5) 0.045(5) -0.021(4) 0.004(4) -0.004(4) C(20) 0.015(5) 0.021(5) 0.094(7) -0.003(4) 0.009(5) -0.023(4) C(21) 0.045(6) 0.067(6) 0.011(4) 0.022(5) -0.015(4) -0.004(4) C(22) 0.027(5) 0.067(6) 0.056(5) -0.021(5) -0.014(5) -0.020(5) C(23) 0.14(1) 0.009(4) 0.052(6) -0.009(5) 0.005(6) -0.003(4) C(24) 0.031(5) 0.068(6) 0.026(4) 0.019(5) -0.020(4) -0.009(4) C(25) 0.063(7) 0.016(5) 0.080(6) 0.013(5) -0.005(5) -0.004(4) C(26) 0.037(6) 0.049(6) 0.096(7) -0.023(5) -0.032(5) 0.011(5) C(27) 0.058(6) 0.056(5) 0.004(4) -0.007(5) 0.009(4) 0.006(3) C(28) 0.008(5) 0.022(5) 0.101(6) -0.002(4) -0.027(5) -0.020(4) C(29) 0.001(4) 0.071(6) 0.014(4) 0.005(4) -0.003(3) 0.012(4) C(30) 0.030(5) 0.018(4) 0.024(4) 0.003(4) 0.002(4) -0.002(3) C(31) 0.034(5) 0.029(5) 0.034(4) -0.017(4) -0.031(4) 0.016(4) C(32) 0.002(5) 0.034(5) 0.078(6) -0.000(4) -0.014(4) -0.015(4) C(33) 0.003(5) 0.063(6) 0.045(5) -0.004(4) -0.003(4) -0.009(4) C(34) 0.086(8) 0.085(7) 0.037(5) 0.016(6) -0.022(5) -0.030(5) C(35) 0.071(8) 0.113(9) 0.079(7) -0.048(7) -0.026(6) 0.023(6) C(36) 0.109(9) 0.039(5) 0.057(5) -0.002(6) -0.052(6) 0.017(4) C(37) 1.32(4) 0.99(4) -0.002(7) 0.71(3) 0.33(1) 0.16(1) C(38) 0.095(9) 0.028(5) 0.22(1) -0.032(6) 0.040(9) -0.016(8) C(39) 0.074(9) 0.14(1) 0.18(1) -0.036(9) 0.047(8) 0.04(1) C(40) 0.23(2) 0.24(1) 0.053(6) -0.09(1) 0.072(8) -0.112(7) C(41) 1.20(3) 1.58(6) -0.013(6) -0.50(4) 0.425(9) -0.25(1) C(42) 0.15(1) 0.035(7) 0.39(2) -0.073(7) -0.15(1) 0.075(8) #=========================================================================== # REFINEMENT DATA _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) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000177(1) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_number_reflns 2592 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.0460 _refine_ls_goodness_of_fit_all 5.196 _refine_ls_goodness_of_fit_ref 5.200 _refine_ls_shift/su_max 1.2300 _refine_ls_shift/su_mean 0.0673 _refine_diff_density_min -0.61 _refine_diff_density_max 0.51 #=========================================================================== # 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 Cl(5) C(37) 1.46(4) . . ? S(1) C(1) 1.81(2) . . ? S(1) C(4) 1.72(2) . . ? S(2) C(3) 1.81(2) . . ? S(2) C(4) 1.79(2) . . ? S(3) C(5) 1.80(2) . . ? S(3) C(6) 1.70(2) . . ? S(4) C(5) 1.72(2) . . ? S(4) C(7) 1.77(2) . . ? S(5) C(6) 1.77(2) . . ? S(5) C(8) 1.76(2) . . ? S(6) C(7) 1.74(2) . . ? S(6) C(8) 1.76(2) . . ? S(7) C(9) 1.76(2) . . ? S(7) C(10) 1.81(2) . . ? S(8) C(9) 1.73(1) . . ? S(8) C(12) 1.90(3) . . ? S(9) C(13) 1.79(2) . . ? S(9) C(16) 1.73(2) . . ? S(10) C(15) 1.82(2) . . ? S(10) C(16) 1.79(2) . . ? S(11) C(17) 1.78(2) . . ? S(11) C(18) 1.77(2) . . ? S(12) C(17) 1.78(2) . . ? S(12) C(19) 1.76(2) . . ? S(13) C(18) 1.70(2) . . ? S(13) C(20) 1.75(2) . . ? S(14) C(19) 1.73(2) . . ? S(14) C(20) 1.78(2) . . ? S(15) C(21) 1.78(2) . . ? S(15) C(22) 1.84(2) . . ? S(16) C(21) 1.75(2) . . ? S(16) C(24) 1.82(2) . . ? S(17) C(25) 1.79(2) . . ? S(17) C(28) 1.73(2) . . ? S(18) C(27) 1.83(2) . . ? S(18) C(28) 1.76(2) . . ? S(19) C(29) 1.79(2) . . ? S(19) C(30) 1.78(2) . . ? S(20) C(29) 1.77(2) . . ? S(20) C(31) 1.76(2) . . ? S(21) C(30) 1.72(2) . . ? S(21) C(32) 1.71(2) . . ? S(22) C(31) 1.74(2) . . ? S(22) C(32) 1.81(2) . . ? S(23) C(33) 1.73(2) . . ? S(23) C(34) 1.78(2) . . ? S(24) C(33) 1.73(2) . . ? S(24) C(36) 1.82(2) . . ? C(1) C(2) 1.46(3) . . ? C(1) H(1) 0.94 . . no C(1) H(2) 0.94 . . no C(1) H(3) 1.97 . . no C(1) H(4) 1.97 . . no C(2) C(3) 1.53(2) . . ? C(2) H(1) 1.93 . . no C(2) H(2) 1.94 . . no C(2) H(3) 0.94 . . no C(2) H(4) 0.97 . . no C(2) H(5) 1.99 . . no C(2) H(6) 1.98 . . no C(3) H(5) 0.94 . . no C(3) H(6) 0.91 . . no C(4) C(5) 1.36(2) . . ? C(6) C(7) 1.35(2) . . ? C(8) C(9) 1.40(2) . . ? C(10) C(11) 1.45(3) . . ? C(10) H(7) 0.95 . . no C(10) H(8) 0.92 . . no C(10) H(9) 1.98 . . no C(10) H(10) 1.98 . . no C(11) C(12) 1.50(3) . . ? C(11) H(7) 1.92 . . no C(11) H(8) 1.93 . . no C(11) H(9) 0.91 . . no C(11) H(10) 0.99 . . no C(11) H(12) 1.99 . . no C(12) H(9) 1.94 . . no C(12) H(11) 0.98 . . no C(12) H(12) 0.86 . . no C(13) C(14) 1.51(3) . . ? C(13) H(13) 0.95 . . no C(13) H(14) 0.97 . . no C(14) C(15) 1.63(3) . . ? C(14) H(15) 0.93 . . no C(14) H(16) 0.96 . . no C(15) H(17) 0.95 . . no C(15) H(18) 0.94 . . no C(16) C(17) 1.33(2) . . ? C(18) C(19) 1.36(2) . . ? C(20) C(21) 1.37(2) . . ? C(22) C(23) 1.62(2) . . ? C(22) H(19) 0.94 . . no C(22) H(20) 0.93 . . no C(23) C(24) 1.47(3) . . ? C(23) H(21) 0.96 . . no C(23) H(22) 0.99 . . no C(24) H(23) 0.96 . . no C(24) H(24) 0.94 . . no C(25) C(26) 1.51(3) . . ? C(25) H(25) 0.94 . . no C(25) H(26) 0.96 . . no C(26) C(27) 1.58(2) . . ? C(26) H(27) 0.96 . . no C(26) H(28) 0.95 . . no C(27) H(29) 0.95 . . no C(27) H(30) 0.96 . . no C(28) C(29) 1.34(2) . . ? C(30) C(31) 1.26(2) . . ? C(32) C(33) 1.38(2) . . ? C(34) C(35) 1.40(3) . . ? C(34) H(31) 0.95 . . no C(34) H(32) 0.95 . . no C(34) H(33) 1.91 . . no C(34) H(34) 1.90 . . no C(35) C(36) 1.46(3) . . ? C(35) H(31) 1.89 . . no C(35) H(32) 1.90 . . no C(35) H(33) 0.96 . . no C(35) H(34) 0.95 . . no C(35) H(35) 1.97 . . no C(35) H(36) 1.98 . . no C(36) H(33) 1.99 . . no C(36) H(34) 1.99 . . no C(36) H(35) 0.95 . . no C(36) H(36) 0.95 . . no C(37) C(38) 1.13(5) . . ? C(37) C(42) 1.79(5) . . ? C(37) H(37) 1.80 . . no C(38) C(39) 1.59(3) . . ? C(38) H(37) 0.99 . . no C(39) C(40) 1.25(4) . . ? C(39) H(38) 1.03 . . no C(39) H(39) 1.89 . . no C(40) C(41) 1.36(6) . . ? C(40) C(42) 1.95(4) . . ? C(40) H(39) 0.90 . . no C(41) C(42) 0.88(4) . . ? C(41) H(39) 1.98 . . no C(41) H(40) 1.07 . . no C(41) H(41) 1.83 . . no C(42) H(40) 1.58 . . no C(42) H(41) 1.11 . . no H(1) H(2) 1.55 . . no H(3) H(4) 1.55 . . no H(5) H(6) 1.55 . . no H(7) H(8) 1.55 . . no H(9) H(10) 1.55 . . no H(11) H(12) 1.55 . . no H(13) H(14) 1.55 . . no H(15) H(16) 1.55 . . no H(17) H(18) 1.55 . . no H(19) H(20) 1.55 . . no H(21) H(22) 1.55 . . no H(23) H(24) 1.55 . . no H(25) H(26) 1.55 . . no H(27) H(28) 1.55 . . no H(29) H(30) 1.55 . . no H(31) H(32) 1.55 . . no H(33) H(34) 1.55 . . no H(35) H(36) 1.55 . . no H(40) H(41) 1.98 . . 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 C(1) S(1) C(4) 100.9(8) . . . ? C(3) S(2) C(4) 103.0(9) . . . ? C(5) S(3) C(6) 93.0(8) . . . ? C(5) S(4) C(7) 94.0(8) . . . ? C(6) S(5) C(8) 94.4(8) . . . ? C(7) S(6) C(8) 92.8(8) . . . ? C(9) S(7) C(10) 98.5(9) . . . ? C(9) S(8) C(12) 94.6(9) . . . ? C(13) S(9) C(16) 98.4(8) . . . ? C(15) S(10) C(16) 101.0(9) . . . ? C(17) S(11) C(18) 95.3(8) . . . ? C(17) S(12) C(19) 94.2(8) . . . ? C(18) S(13) C(20) 93.6(8) . . . ? C(19) S(14) C(20) 93.5(8) . . . ? C(21) S(15) C(22) 101.6(8) . . . ? C(21) S(16) C(24) 101.3(8) . . . ? C(25) S(17) C(28) 98.4(8) . . . ? C(27) S(18) C(28) 101.7(8) . . . ? C(29) S(19) C(30) 92.5(8) . . . ? C(29) S(20) C(31) 92.8(8) . . . ? C(30) S(21) C(32) 93.5(8) . . . ? C(31) S(22) C(32) 91.6(8) . . . ? C(33) S(23) C(34) 103.6(9) . . . ? C(33) S(24) C(36) 102.0(8) . . . ? S(1) C(1) C(2) 115(1) . . . ? S(1) C(1) H(1) 109.7 . . . no S(1) C(1) H(2) 109.8 . . . no S(1) C(1) H(3) 141.2 . . . no S(1) C(1) H(4) 96.5 . . . no C(2) C(1) H(1) 105.3 . . . no C(2) C(1) H(2) 106.0 . . . no C(2) C(1) H(3) 27.1 . . . no C(2) C(1) H(4) 28.1 . . . no H(1) C(1) H(2) 111.3 . . . no H(1) C(1) H(3) 94.5 . . . no H(1) C(1) H(4) 133.2 . . . no H(2) C(1) H(3) 87.6 . . . no H(2) C(1) H(4) 94.1 . . . no H(3) C(1) H(4) 46.5 . . . no C(1) C(2) C(3) 118(2) . . . ? C(1) C(2) H(1) 27.9 . . . no C(1) C(2) H(2) 27.7 . . . no C(1) C(2) H(3) 107.9 . . . no C(1) C(2) H(4) 106.5 . . . no C(1) C(2) H(5) 144.7 . . . no C(1) C(2) H(6) 101.6 . . . no C(3) C(2) H(1) 99.3 . . . no C(3) C(2) H(2) 144.9 . . . no C(3) C(2) H(3) 107.9 . . . no C(3) C(2) H(4) 107.7 . . . no C(3) C(2) H(5) 27.1 . . . no C(3) C(2) H(6) 26.3 . . . no H(1) C(2) H(2) 47.2 . . . no H(1) C(2) H(3) 96.4 . . . no H(1) C(2) H(4) 134.2 . . . no H(1) C(2) H(5) 123.5 . . . no H(1) C(2) H(6) 77.6 . . . no H(2) C(2) H(3) 89.0 . . . no H(2) C(2) H(4) 94.8 . . . no H(2) C(2) H(5) 170.6 . . . no H(2) C(2) H(6) 124.7 . . . no H(3) C(2) H(4) 108.9 . . . no H(3) C(2) H(5) 91.5 . . . no H(3) C(2) H(6) 95.7 . . . no H(4) C(2) H(5) 94.0 . . . no H(4) C(2) H(6) 134.0 . . . no H(5) C(2) H(6) 45.9 . . . no S(2) C(3) C(2) 111(1) . . . ? S(2) C(3) H(5) 109.5 . . . no S(2) C(3) H(6) 111.3 . . . no C(2) C(3) H(5) 105.0 . . . no C(2) C(3) H(6) 105.8 . . . no H(5) C(3) H(6) 113.7 . . . no S(1) C(4) S(2) 122(1) . . . ? S(1) C(4) C(5) 122(1) . . . ? S(2) C(4) C(5) 115(1) . . . ? S(3) C(5) S(4) 116.5(9) . . . ? S(3) C(5) C(4) 118(1) . . . ? S(4) C(5) C(4) 125(1) . . . ? S(3) C(6) S(5) 125(1) . . . ? S(3) C(6) C(7) 120(1) . . . ? S(5) C(6) C(7) 115(1) . . . ? S(4) C(7) S(6) 123(1) . . . ? S(4) C(7) C(6) 116(1) . . . ? S(6) C(7) C(6) 121(1) . . . ? S(5) C(8) S(6) 116(1) . . . ? S(5) C(8) C(9) 123(1) . . . ? S(6) C(8) C(9) 121(1) . . . ? S(7) C(9) S(8) 123(1) . . . ? S(7) C(9) C(8) 117(1) . . . ? S(8) C(9) C(8) 120(1) . . . ? S(7) C(10) C(11) 116(2) . . . ? S(7) C(10) H(7) 108.0 . . . no S(7) C(10) H(8) 109.6 . . . no S(7) C(10) H(9) 141.6 . . . no S(7) C(10) H(10) 99.6 . . . no C(11) C(10) H(7) 104.0 . . . no C(11) C(10) H(8) 106.4 . . . no C(11) C(10) H(9) 25.5 . . . no C(11) C(10) H(10) 28.6 . . . no H(7) C(10) H(8) 112.7 . . . no H(7) C(10) H(9) 91.8 . . . no H(7) C(10) H(10) 132.6 . . . no H(8) C(10) H(9) 91.3 . . . no H(8) C(10) H(10) 92.3 . . . no H(9) C(10) H(10) 46.2 . . . no C(10) C(11) C(12) 117(2) . . . ? C(10) C(11) H(7) 28.6 . . . no C(10) C(11) H(8) 27.2 . . . no C(10) C(11) H(9) 111.2 . . . no C(10) C(11) H(10) 106.7 . . . no C(10) C(11) H(12) 103.2 . . . no C(12) C(11) H(7) 100.1 . . . no C(12) C(11) H(8) 144.5 . . . no C(12) C(11) H(9) 105.0 . . . no C(12) C(11) H(10) 107.2 . . . no C(12) C(11) H(12) 23.5 . . . no H(7) C(11) H(8) 47.6 . . . no H(7) C(11) H(9) 96.7 . . . no H(7) C(11) H(10) 135.3 . . . no H(7) C(11) H(12) 80.2 . . . no H(8) C(11) H(9) 94.8 . . . no H(8) C(11) H(10) 93.3 . . . no H(8) C(11) H(12) 127.7 . . . no H(9) C(11) H(10) 109.2 . . . no H(9) C(11) H(12) 95.0 . . . no H(10) C(11) H(12) 130.6 . . . no S(8) C(12) C(11) 114(2) . . . ? S(8) C(12) H(9) 140.3 . . . no S(8) C(12) H(11) 101.1 . . . no S(8) C(12) H(12) 106.9 . . . no C(11) C(12) H(9) 27.0 . . . no C(11) C(12) H(11) 107.1 . . . no C(11) C(12) H(12) 112.4 . . . no H(9) C(12) H(11) 92.8 . . . no H(9) C(12) H(12) 100.1 . . . no H(11) C(12) H(12) 115.3 . . . no S(9) C(13) C(14) 114(1) . . . ? S(9) C(13) H(13) 107.6 . . . no S(9) C(13) H(14) 106.3 . . . no C(14) C(13) H(13) 111.5 . . . no C(14) C(13) H(14) 109.4 . . . no H(13) C(13) H(14) 107.4 . . . no C(13) C(14) C(15) 111(1) . . . ? C(13) C(14) H(15) 111.0 . . . no C(13) C(14) H(16) 109.7 . . . no C(15) C(14) H(15) 107.4 . . . no C(15) C(14) H(16) 107.4 . . . no H(15) C(14) H(16) 110.4 . . . no S(10) C(15) C(14) 110(1) . . . ? S(10) C(15) H(17) 106.8 . . . no S(10) C(15) H(18) 107.1 . . . no C(14) C(15) H(17) 111.2 . . . no C(14) C(15) H(18) 110.8 . . . no H(17) C(15) H(18) 110.3 . . . no S(9) C(16) S(10) 119.3(9) . . . ? S(9) C(16) C(17) 121(1) . . . ? S(10) C(16) C(17) 119(1) . . . ? S(11) C(17) S(12) 115(1) . . . ? S(11) C(17) C(16) 121(1) . . . ? S(12) C(17) C(16) 123(1) . . . ? S(11) C(18) S(13) 124.1(9) . . . ? S(11) C(18) C(19) 116(1) . . . ? S(13) C(18) C(19) 120(1) . . . ? S(12) C(19) S(14) 124(1) . . . ? S(12) C(19) C(18) 119(1) . . . ? S(14) C(19) C(18) 117(1) . . . ? S(13) C(20) S(14) 116.2(9) . . . ? S(13) C(20) C(21) 123(1) . . . ? S(14) C(20) C(21) 120(1) . . . ? S(15) C(21) S(16) 120(1) . . . ? S(15) C(21) C(20) 118(1) . . . ? S(16) C(21) C(20) 122(1) . . . ? S(15) C(22) C(23) 107(1) . . . ? S(15) C(22) H(19) 110.0 . . . no S(15) C(22) H(20) 111.0 . . . no C(23) C(22) H(19) 105.9 . . . no C(23) C(22) H(20) 110.0 . . . no H(19) C(22) H(20) 112.5 . . . no C(22) C(23) C(24) 114(2) . . . ? C(22) C(23) H(21) 107.6 . . . no C(22) C(23) H(22) 106.7 . . . no C(24) C(23) H(21) 111.3 . . . no C(24) C(23) H(22) 111.5 . . . no H(21) C(23) H(22) 105.4 . . . no S(16) C(24) C(23) 113(1) . . . ? S(16) C(24) H(23) 105.4 . . . no S(16) C(24) H(24) 106.5 . . . no C(23) C(24) H(23) 111.4 . . . no C(23) C(24) H(24) 111.1 . . . no H(23) C(24) H(24) 109.6 . . . no S(17) C(25) C(26) 115(1) . . . ? S(17) C(25) H(25) 106.7 . . . no S(17) C(25) H(26) 105.7 . . . no C(26) C(25) H(25) 110.6 . . . no C(26) C(25) H(26) 109.0 . . . no H(25) C(25) H(26) 109.3 . . . no C(25) C(26) C(27) 113(2) . . . ? C(25) C(26) H(27) 109.0 . . . no C(25) C(26) H(28) 110.8 . . . no C(27) C(26) H(27) 107.5 . . . no C(27) C(26) H(28) 107.4 . . . no H(27) C(26) H(28) 108.8 . . . no S(18) C(27) C(26) 110(1) . . . ? S(18) C(27) H(29) 110.5 . . . no S(18) C(27) H(30) 109.6 . . . no C(26) C(27) H(29) 109.7 . . . no C(26) C(27) H(30) 108.4 . . . no H(29) C(27) H(30) 109.0 . . . no S(17) C(28) S(18) 122(1) . . . ? S(17) C(28) C(29) 120(1) . . . ? S(18) C(28) C(29) 117(1) . . . ? S(19) C(29) S(20) 115.0(9) . . . ? S(19) C(29) C(28) 121(1) . . . ? S(20) C(29) C(28) 124(1) . . . ? S(19) C(30) S(21) 120.9(9) . . . ? S(19) C(30) C(31) 118(1) . . . ? S(21) C(30) C(31) 121(1) . . . ? S(20) C(31) S(22) 120.7(9) . . . ? S(20) C(31) C(30) 120(1) . . . ? S(22) C(31) C(30) 119(1) . . . ? S(21) C(32) S(22) 115.4(9) . . . ? S(21) C(32) C(33) 125(1) . . . ? S(22) C(32) C(33) 120(1) . . . ? S(23) C(33) S(24) 124(1) . . . ? S(23) C(33) C(32) 117(1) . . . ? S(24) C(33) C(32) 118(1) . . . ? S(23) C(34) C(35) 123(2) . . . ? S(23) C(34) H(31) 106.7 . . . no S(23) C(34) H(32) 106.7 . . . no S(23) C(34) H(33) 151.1 . . . no S(23) C(34) H(34) 109.6 . . . no C(35) C(34) H(31) 105.0 . . . no C(35) C(34) H(32) 106.3 . . . no C(35) C(34) H(33) 28.7 . . . no C(35) C(34) H(34) 28.8 . . . no H(31) C(34) H(32) 109.1 . . . no H(31) C(34) H(33) 86.8 . . . no H(31) C(34) H(34) 133.1 . . . no H(32) C(34) H(33) 92.1 . . . no H(32) C(34) H(34) 87.9 . . . no H(33) C(34) H(34) 48.0 . . . no C(34) C(35) C(36) 117(2) . . . ? C(34) C(35) H(31) 29.1 . . . no C(34) C(35) H(32) 28.6 . . . no C(34) C(35) H(33) 106.3 . . . no C(34) C(35) H(34) 106.0 . . . no C(34) C(35) H(35) 144.6 . . . no C(34) C(35) H(36) 104.2 . . . no C(36) C(35) H(31) 104.6 . . . no C(36) C(35) H(32) 145.7 . . . no C(36) C(35) H(33) 109.1 . . . no C(36) C(35) H(34) 109.3 . . . no C(36) C(35) H(35) 27.4 . . . no C(36) C(35) H(36) 27.3 . . . no H(31) C(35) H(32) 48.2 . . . no H(31) C(35) H(33) 87.8 . . . no H(31) C(35) H(34) 134.3 . . . no H(31) C(35) H(35) 129.1 . . . no H(31) C(35) H(36) 82.9 . . . no H(32) C(35) H(33) 92.2 . . . no H(32) C(35) H(34) 87.7 . . . no H(32) C(35) H(35) 171.9 . . . no H(32) C(35) H(36) 130.6 . . . no H(33) C(35) H(34) 108.6 . . . no H(33) C(35) H(35) 95.4 . . . no H(33) C(35) H(36) 92.2 . . . no H(34) C(35) H(35) 92.6 . . . no H(34) C(35) H(36) 136.3 . . . no H(35) C(35) H(36) 46.3 . . . no S(24) C(36) C(35) 119(2) . . . ? S(24) C(36) H(33) 145.8 . . . no S(24) C(36) H(34) 105.4 . . . no S(24) C(36) H(35) 106.2 . . . no S(24) C(36) H(36) 106.6 . . . no C(35) C(36) H(33) 27.0 . . . no C(35) C(36) H(34) 26.9 . . . no C(35) C(36) H(35) 107.8 . . . no C(35) C(36) H(36) 108.2 . . . no H(33) C(36) H(34) 45.9 . . . no H(33) C(36) H(35) 94.4 . . . no H(33) C(36) H(36) 91.5 . . . no H(34) C(36) H(35) 91.5 . . . no H(34) C(36) H(36) 134.9 . . . no H(35) C(36) H(36) 108.8 . . . no Cl(5) C(37) C(38) 140(5) . . . ? Cl(5) C(37) C(42) 110(4) . . . ? Cl(5) C(37) H(37) 110.4 . . . no C(38) C(37) C(42) 92(3) . . . ? C(38) C(37) H(37) 30.0 . . . no C(42) C(37) H(37) 114.3 . . . no C(37) C(38) C(39) 132(3) . . . ? C(37) C(38) H(37) 115.5 . . . no C(39) C(38) H(37) 110.7 . . . no C(38) C(39) C(40) 114(3) . . . ? C(38) C(39) H(38) 120.0 . . . no C(38) C(39) H(39) 138.6 . . . no C(40) C(39) H(38) 125.6 . . . no C(40) C(39) H(39) 24.2 . . . no H(38) C(39) H(39) 101.4 . . . no C(39) C(40) C(41) 118(2) . . . ? C(39) C(40) C(42) 95(2) . . . ? C(39) C(40) H(39) 121.1 . . . no C(41) C(40) C(42) 23(2) . . . ? C(41) C(40) H(39) 120.5 . . . no C(42) C(40) H(39) 143.7 . . . no C(40) C(41) C(42) 119(5) . . . ? C(40) C(41) H(39) 23.2 . . . no C(40) C(41) H(40) 127.3 . . . no C(40) C(41) H(41) 144.2 . . . no C(42) C(41) H(39) 142.4 . . . no C(42) C(41) H(40) 107.7 . . . no C(42) C(41) H(41) 26.5 . . . no H(39) C(41) H(40) 106.0 . . . no H(39) C(41) H(41) 165.2 . . . no H(40) C(41) H(41) 81.5 . . . no C(37) C(42) C(40) 102(2) . . . ? C(37) C(42) C(41) 138(5) . . . ? C(37) C(42) H(40) 177.8 . . . no C(37) C(42) H(41) 89.4 . . . no C(40) C(42) C(41) 37(4) . . . ? C(40) C(42) H(40) 75.5 . . . no C(40) C(42) H(41) 165.4 . . . no C(41) C(42) H(40) 40.2 . . . no C(41) C(42) H(41) 132.7 . . . no H(40) C(42) H(41) 92.8 . . . no C(1) H(1) C(2) 46.8 . . . no C(1) H(1) H(2) 34.4 . . . no C(2) H(1) H(2) 66.7 . . . no C(1) H(2) C(2) 46.3 . . . no C(1) H(2) H(1) 34.3 . . . no C(2) H(2) H(1) 66.1 . . . no C(1) H(3) C(2) 45.0 . . . no C(1) H(3) H(4) 66.8 . . . no C(2) H(3) H(4) 36.1 . . . no C(1) H(4) C(2) 45.4 . . . no C(1) H(4) H(3) 66.7 . . . no C(2) H(4) H(3) 35.0 . . . no C(2) H(5) C(3) 47.9 . . . no C(2) H(5) H(6) 66.8 . . . no C(3) H(5) H(6) 32.6 . . . no C(2) H(6) C(3) 47.9 . . . no C(2) H(6) H(5) 67.3 . . . no C(3) H(6) H(5) 33.6 . . . no C(10) H(7) C(11) 47.4 . . . no C(10) H(7) H(8) 33.1 . . . no C(11) H(7) H(8) 66.5 . . . no C(10) H(8) C(11) 46.4 . . . no C(10) H(8) H(7) 34.3 . . . no C(11) H(8) H(7) 65.9 . . . no C(10) H(9) C(11) 43.3 . . . no C(10) H(9) C(12) 80.0 . . . no C(10) H(9) H(10) 67.1 . . . no C(11) H(9) C(12) 48.1 . . . no C(11) H(9) H(10) 37.1 . . . no C(12) H(9) H(10) 69.8 . . . no C(10) H(10) C(11) 44.7 . . . no C(10) H(10) H(9) 66.8 . . . no C(11) H(10) H(9) 33.7 . . . no C(12) H(11) H(12) 29.9 . . . no C(11) H(12) C(12) 44.1 . . . no C(11) H(12) H(11) 68.2 . . . no C(12) H(12) H(11) 34.8 . . . no C(13) H(13) H(14) 36.7 . . . no C(13) H(14) H(13) 35.8 . . . no C(14) H(15) H(16) 35.3 . . . no C(14) H(16) H(15) 34.2 . . . no C(15) H(17) H(18) 34.8 . . . no C(15) H(18) H(17) 34.9 . . . no C(22) H(19) H(20) 33.5 . . . no C(22) H(20) H(19) 34.0 . . . no C(23) H(21) H(22) 37.9 . . . no C(23) H(22) H(21) 36.7 . . . no C(24) H(23) H(24) 34.8 . . . no C(24) H(24) H(23) 35.6 . . . no C(25) H(25) H(26) 35.8 . . . no C(25) H(26) H(25) 34.9 . . . no C(26) H(27) H(28) 35.4 . . . no C(26) H(28) H(27) 35.8 . . . no C(27) H(29) H(30) 35.7 . . . no C(27) H(30) H(29) 35.3 . . . no C(34) H(31) C(35) 45.8 . . . no C(34) H(31) H(32) 35.4 . . . no C(35) H(31) H(32) 66.3 . . . no C(34) H(32) C(35) 45.1 . . . no C(34) H(32) H(31) 35.5 . . . no C(35) H(32) H(31) 65.5 . . . no C(34) H(33) C(35) 44.9 . . . no C(34) H(33) C(36) 77.7 . . . no C(34) H(33) H(34) 65.8 . . . no C(35) H(33) C(36) 43.9 . . . no C(35) H(33) H(34) 35.7 . . . no C(36) H(33) H(34) 67.1 . . . no C(34) H(34) C(35) 45.2 . . . no C(34) H(34) C(36) 77.8 . . . no C(34) H(34) H(33) 66.2 . . . no C(35) H(34) C(36) 43.8 . . . no C(35) H(34) H(33) 35.8 . . . no C(36) H(34) H(33) 67.0 . . . no C(35) H(35) C(36) 44.8 . . . no C(35) H(35) H(36) 67.0 . . . no C(36) H(35) H(36) 35.6 . . . no C(35) H(36) C(36) 44.5 . . . no C(35) H(36) H(35) 66.7 . . . no C(36) H(36) H(35) 35.6 . . . no C(37) H(37) C(38) 34.6 . . . no C(39) H(39) C(40) 34.7 . . . no C(39) H(39) C(41) 70.7 . . . no C(40) H(39) C(41) 36.3 . . . no C(41) H(40) C(42) 32.1 . . . no C(41) H(40) H(41) 66.0 . . . no C(42) H(40) H(41) 34.0 . . . no C(41) H(41) C(42) 20.8 . . . no C(41) H(41) H(40) 32.5 . . . no C(42) H(41) H(40) 53.1 . . . 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 Cl(1) H(33) 2.7225 . 2_746 no Cl(1) C(35) 3.52(2) . 2_746 no Cl(1) S(8) 3.528(8) . 2_646 no Cl(1) C(34) 3.56(2) . 2_746 no Cl(2) H(26) 2.9004 . . no Cl(2) H(39) 3.0855 . 1_655 no Cl(2) S(17) 3.562(8) . . no Cl(2) C(25) 3.61(2) . . no Cl(3) H(27) 2.9579 . 1_556 no Cl(3) H(30) 3.0751 . 1_556 no Cl(3) C(26) 3.55(2) . 1_556 no Cl(3) C(27) 3.67(2) . 1_556 no Cl(4) H(26) 2.7889 . . no Cl(4) H(40) 2.8183 . . no Cl(4) C(25) 3.56(2) . . no Cl(4) C(24) 3.59(2) . 2_646 no Cl(4) C(26) 3.64(2) . . no S(1) C(30) 3.59(2) . 1_456 no S(1) S(18) 3.674(7) . 1_556 no S(2) S(11) 3.373(7) . 1_455 no S(2) C(31) 3.58(2) . 1_456 no S(2) S(13) 3.694(6) . 1_455 no S(3) S(20) 3.615(7) . 1_556 no S(3) S(18) 3.634(7) . 1_556 no S(4) S(13) 3.512(6) . 1_455 no S(5) S(20) 3.562(6) . 1_556 no S(5) S(22) 3.607(7) . 1_556 no S(5) C(18) 3.61(2) . . no S(6) S(15) 3.418(7) . 1_455 no S(6) C(19) 3.57(2) . . no S(7) H(19) 3.0663 . . no S(7) S(24) 3.662(7) . 1_556 no S(7) S(22) 3.687(7) . 1_556 no S(9) H(29) 3.0933 . 1_556 no S(9) H(30) 3.1171 . 1_556 no S(9) C(27) 3.43(2) . 1_556 no S(10) S(19) 3.439(7) . 1_455 no S(11) C(6) 3.67(2) . . no S(12) S(21) 3.525(6) . 1_455 no S(12) C(7) 3.65(2) . . no S(13) C(30) 3.70(1) . . no S(14) S(23) 3.417(7) . 1_455 no S(14) C(31) 3.65(2) . . no S(16) C(10) 3.60(2) . 1_554 no S(17) H(13) 3.0338 . . no S(18) H(18) 2.9936 . . no S(19) C(18) 3.64(2) . . no S(20) C(19) 3.64(2) . . no S(23) C(6) 3.57(2) . 1_654 no S(24) C(7) 3.62(2) . 1_654 no S(24) C(22) 3.68(2) . 1_554 no C(5) C(16) 3.60(2) . . no C(5) C(32) 3.64(2) . 1_456 no C(6) C(17) 3.68(2) . . no C(7) C(17) 3.68(2) . . no C(8) H(34) 3.0985 . 1_456 no C(9) H(34) 3.1089 . 1_456 no C(20) C(31) 3.59(2) . . no C(20) C(30) 3.61(2) . . no C(21) C(32) 3.55(2) . . no C(36) C(37) 3.63(7) . 2_655 no C(42) H(27) 3.1332 . . no H(1) H(16) 2.3449 . . no H(6) H(16) 2.6444 . . no H(12) H(34) 2.7267 . 1_456 no H(13) H(28) 2.4999 . . no H(15) H(39) 2.6571 . . no H(18) H(28) 2.6103 . . no H(20) H(35) 2.7154 . 1_556 no H(22) H(36) 2.4421 . . no H(22) H(31) 2.5354 . . no H(27) H(41) 2.6214 . . no #--------------------------------------------------------------------------- #=========================================================================== #End of CIF