# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 1145/273 ------------------------------------------------------------------------------- data_General _audit_creation_date 'Fri Dec 1 00:42:09 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Hiroshi M. Yamamoto' _publ_contact_author_address ; Hirosawa, Wako-shi, Saitama 351-0198 (Japan) ; _publ_contact_author_email ' yhiroshi@postman.riken.go.jp ' _publ_contact_author_fax ' +81-(0)48-462-4661 ' _publ_contact_author_phone ' +81-(0)48-467-9410 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' ' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # _publ_section_title ; Structural and physical properties of conducting cation radical satls containing supramolecular assmblies based on pBIB derivatives (pBIB=p-Bis(iodoethynyl)benzene) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_ET3Br-DFBIB #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C40 H26 Br F2 I2 S24 ' _chemical_formula_moiety 'C40 H26 Br F2 I2 S24 ' _chemical_formula_weight 1647.80 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.361(2) _cell_length_b 15.373(3) _cell_length_c 9.397(3) _cell_angle_alpha 98.34(2) _cell_angle_beta 107.54(2) _cell_angle_gamma 76.35(2) _cell_volume 1382.5(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.1 _cell_measurement_theta_max 16.8 _cell_measurement_temperature 298.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_meas 1.98(1) _exptl_crystal_density_method 'floating method' _exptl_absorpt_coefficient_mu 2.809 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 10725 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 35.03 _diffrn_reflns_limit_h_min 12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.69 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; ; _reflns_number_total 10231 _reflns_number_gt 7078 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1672 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7078 _refine_ls_number_parameters 313 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0410 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_shift/esd_max 0.041 _refine_ls_shift/esd_mean 0.002 _refine_diff_density_max 2.60 _refine_diff_density_min -1.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.36515(2) 0.99934(2) 0.63709(2) 0.0(5) Uani 1.00 d . . . Br(1) Br 0.5000 1.0000 1.0000 0.0400(1) Uani 1.00 d S . . S(1) S 0.3665(1) 0.58054(6) 1.3826(1) 0.0433(2) Uani 1.00 d . . . S(2) S 0.1133(1) 0.57307(7) 1.1368(1) 0.044(6) Uani 1.00 d . . . S(3) S 0.5424(1) 0.42927(7) 1.1991(1) 0.0443(2) Uani 1.00 d . . . S(4) S 0.2890(1) 0.42005(6) 0.9535(1) 0.0401(2) Uani 1.00 d . . . S(5) S 0.2500(1) 0.74612(9) 1.5380(1) 0.0606(8) Uani 1.00 d . . . S(6) S -0.0527(1) 0.7375(1) 1.2500(2) 0.0660(4) Uani 1.00 d . . . S(7) S 0.7145(1) 0.27097(9) 1.0775(1) 0.0566(3) Uani 1.00 d . . . S(8) S 0.4107(1) 0.26064(8) 0.7900(1) 0.051(10) Uani 1.00 d . . . S(9) S 0.2138(1) 0.42759(7) 1.5344(1) 0.0442(2) Uani 1.00 d . . . S(10) S -0.0391(1) 0.41321(6) 1.2931(1) 0.0434(2) Uani 1.00 d . . . S(11) S 0.3885(1) 0.26959(9) 1.4171(1) 0.056(9) Uani 1.00 d . . . S(12) S 0.0858(1) 0.25168(8) 1.1348(1) 0.0546(3) Uani 1.00 d . . . F(1) F -0.0869(3) 0.9996(2) 0.2432(3) 0.0536(6) Uani 1.00 d . . . C(1) C 0.2907(4) 0.5324(2) 1.2062(4) 0.032(6) Uani 1.00 d . . . C(2) C 0.3648(4) 0.4688(2) 1.1302(4) 0.0324(6) Uani 1.00 d . . . C(3) C 0.2221(4) 0.6659(2) 1.3866(4) 0.0353(7) Uani 1.00 d . . . C(4) C 0.1068(3) 0.6619(2) 1.2745(4) 0.037(10) Uani 1.00 d . . . C(5) C 0.5524(3) 0.3426(2) 1.0574(4) 0.0336(6) Uani 1.00 d . . . C(6) C 0.4373(3) 0.3380(2) 0.9454(4) 0.0317(6) Uani 1.00 d . . . C(7) C 0.0815(6) 0.8212(4) 1.5129(7) 0.071(8) Uani 1.00 d . . . C(8) C -0.0390(5) 0.7792(4) 1.4398(6) 0.061(1) Uani 1.00 d . . . C(9) C 0.6986(4) 0.2350(3) 0.8837(5) 0.0444(8) Uani 1.00 d . . . C(10) C 0.5796(4) 0.1879(3) 0.8114(5) 0.047(3) Uani 1.00 d . . . C(11) C 0.0366(4) 0.4663(2) 1.4632(4) 0.0341(6) Uani 1.00 d . . . C(12) C 0.2250(3) 0.3393(2) 1.3974(4) 0.0355(7) Uani 1.00 d . . . C(13) C 0.1086(4) 0.3320(2) 1.2860(4) 0.03(1) Uani 1.00 d . . . C(14) C 0.3748(5) 0.2363(4) 1.2247(5) 0.054(1) Uani 1.00 d . . . C(15) C 0.2609(5) 0.1894(4) 1.1474(7) 0.065(2) Uani 1.00 d . . . C(16) C 0.2580(4) 0.9993(3) 0.4198(4) 0.0403(10) Uani 1.00 d . . . C(17) C 0.1870(4) 0.9993(2) 0.2930(4) 0.0388(7) Uani 1.00 d . . . C(18) C 0.0960(3) 0.9990(2) 0.1437(4) 0.0307(6) Uani 1.00 d . . . C(19) C -0.0454(4) 1.0005(2) 0.1203(4) 0.03(1) Uani 1.00 d . . . C(20) C -0.1401(3) 1.0015(2) -0.0174(4) 0.0326(6) Uani 1.00 d . . . H(1) H 0.0737 0.8469 1.6089 0.0848 Uiso 1.00 calc . . . H(2) H 0.0780 0.8672 1.4537 0.0848 Uiso 1.00 calc . . . H(3) H -0.1204 0.8228 1.4426 0.0729 Uiso 1.00 calc . . . H(4) H -0.0326 0.7305 1.4951 0.0729 Uiso 1.00 calc . . . H(5) H 0.6852 0.2862 0.8311 0.0533 Uiso 1.00 calc . . . H(6) H 0.7819 0.1949 0.8761 0.0533 Uiso 1.00 calc . . . H(7) H 0.5869 0.1414 0.8716 0.0562 Uiso 1.00 calc . . . H(8) H 0.5868 0.1625 0.7151 0.0562 Uiso 1.00 calc . . . H(9) H 0.3613 0.2886 1.1748 0.0646 Uiso 1.00 calc . . . H(10) H 0.4592 0.1973 1.2178 0.0646 Uiso 1.00 calc . . . H(11) H 0.2748 0.1376 1.1987 0.0783 Uiso 1.00 calc . . . H(12) H 0.2670 0.1716 1.0481 0.0783 Uiso 1.00 calc . . . H(13) H -0.2343 1.0025 -0.0267 0.0391 Uiso 1.00 calc . . . 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 I(1) 0.0325(1) 0.0501(2) 0.0301(1) -0.00885(9) 0.00441(8) 0.00192(8) Br(1) 0.0302(2) 0.0585(3) 0.0303(2) -0.0076(2) 0.0079(2) 0.0040(2) S(1) 0.0415(5) 0.0363(4) 0.0367(4) 0.0065(3) 0.0042(3) -0.0079(3) S(2) 0.0356(4) 0.0408(5) 0.0465(5) -0.0037(3) 0.0082(4) -0.0163(4) S(3) 0.0355(4) 0.0417(5) 0.0455(5) -0.0042(3) 0.0076(4) -0.0153(4) S(4) 0.0374(4) 0.0351(4) 0.0353(4) 0.0060(3) 0.0063(3) -0.0066(3) S(5) 0.0426(5) 0.0631(7) 0.0546(6) 0.0011(5) 0.0084(5) -0.0330(5) S(6) 0.0340(5) 0.0804(8) 0.0580(7) 0.0116(5) 0.0078(4) -0.0267(6) S(7) 0.0301(4) 0.0710(7) 0.0516(6) 0.0059(4) 0.0091(4) -0.0176(5) S(8) 0.0376(5) 0.0537(6) 0.0444(5) 0.0050(4) 0.0076(4) -0.0216(4) S(9) 0.0360(4) 0.0400(5) 0.0465(5) -0.0015(3) 0.0094(4) -0.0137(4) S(10) 0.0389(4) 0.0373(4) 0.0395(5) 0.0070(3) 0.0060(3) -0.0081(3) S(11) 0.0325(4) 0.0680(7) 0.0494(6) 0.0081(4) 0.0097(4) -0.0167(5) S(12) 0.0389(5) 0.0557(6) 0.0534(6) -0.0006(4) 0.0110(4) -0.0267(5) F(1) 0.045(1) 0.091(2) 0.033(1) -0.020(1) 0.0182(10) 0.001(1) C(1) 0.036(2) 0.026(1) 0.033(1) -0.001(1) 0.012(1) -0.002(1) C(2) 0.037(2) 0.026(1) 0.033(1) -0.003(1) 0.013(1) -0.003(1) C(3) 0.033(1) 0.035(2) 0.035(2) -0.002(1) 0.014(1) -0.010(1) C(4) 0.027(1) 0.036(2) 0.043(2) -0.002(1) 0.012(1) -0.009(1) C(5) 0.027(1) 0.033(2) 0.037(2) -0.001(1) 0.012(1) -0.006(1) C(6) 0.031(1) 0.032(1) 0.030(1) 0.000(1) 0.012(1) -0.003(1) C(7) 0.056(3) 0.054(3) 0.077(4) 0.003(2) 0.009(2) -0.031(2) C(8) 0.047(2) 0.076(3) 0.053(3) 0.008(2) 0.025(2) -0.008(2) C(9) 0.043(2) 0.044(2) 0.051(2) -0.004(1) 0.027(2) -0.001(2) C(10) 0.037(2) 0.039(2) 0.057(2) 0.000(1) 0.014(2) -0.009(2) C(11) 0.039(2) 0.025(1) 0.035(2) 0.001(1) 0.013(1) -0.002(1) C(12) 0.029(1) 0.033(2) 0.041(2) -0.001(1) 0.013(1) -0.006(1) C(13) 0.035(2) 0.032(2) 0.035(2) -0.001(1) 0.013(1) -0.003(1) C(14) 0.042(2) 0.073(3) 0.044(2) -0.004(2) 0.019(2) -0.004(2) C(15) 0.044(2) 0.068(3) 0.074(3) -0.008(2) 0.023(2) -0.036(3) C(16) 0.035(2) 0.049(2) 0.032(2) -0.009(1) 0.004(1) 0.001(1) C(17) 0.033(2) 0.037(2) 0.034(2) -0.004(1) -0.006(1) 0.001(1) C(18) 0.031(1) 0.031(1) 0.028(1) -0.006(1) 0.007(1) -0.001(1) C(19) 0.038(2) 0.039(2) 0.031(2) -0.007(1) 0.018(1) -0.001(1) C(20) 0.024(1) 0.043(2) 0.029(1) -0.007(1) 0.006(1) 0.000(1) #------------------------------------------------------------------------------ _computing_data_collection 'WinAFC' _computing_cell_refinement 'WinAFC' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 I(1) C(16) 2.009(3) . . yes S(1) C(1) 1.745(3) . . yes S(1) C(3) 1.747(3) . . yes S(2) C(1) 1.746(3) . . yes S(2) C(4) 1.744(4) . . yes S(3) C(2) 1.744(3) . . yes S(3) C(5) 1.750(3) . . yes S(4) C(2) 1.751(3) . . yes S(4) C(6) 1.757(3) . . yes S(5) C(3) 1.744(4) . . yes S(5) C(7) 1.820(5) . . yes S(6) C(4) 1.754(3) . . yes S(6) C(8) 1.781(5) . . yes S(7) C(5) 1.751(3) . . yes S(7) C(9) 1.795(5) . . yes S(8) C(6) 1.741(3) . . yes S(8) C(10) 1.812(4) . . yes S(9) C(11) 1.741(3) . . yes S(9) C(12) 1.738(4) . . yes S(10) C(11) 1.733(3) . . yes S(10) C(13) 1.744(3) . . yes S(11) C(12) 1.750(3) . . yes S(11) C(14) 1.779(5) . . yes S(12) C(13) 1.740(4) . . yes S(12) C(15) 1.818(5) . . yes F(1) C(19) 1.352(5) . . yes C(1) C(2) 1.352(5) . . yes C(3) C(4) 1.341(4) . . yes C(5) C(6) 1.341(4) . . yes C(7) C(8) 1.477(8) . . yes C(7) H(1) 0.950 . . no C(7) H(2) 0.950 . . no C(8) H(3) 0.950 . . no C(8) H(4) 0.950 . . no C(9) C(10) 1.511(6) . . yes C(9) H(5) 0.950 . . no C(9) H(6) 0.950 . . no C(10) H(7) 0.950 . . no C(10) H(8) 0.950 . . no C(11) C(11) 1.365(7) . 2_568 yes C(12) C(13) 1.354(4) . . yes C(14) C(15) 1.475(7) . . yes C(14) H(9) 0.950 . . no C(14) H(10) 0.950 . . no C(15) H(11) 0.950 . . no C(15) H(12) 0.950 . . no C(16) C(17) 1.197(5) . . yes C(17) C(18) 1.435(4) . . yes C(18) C(19) 1.409(5) . . yes C(18) C(20) 1.393(6) . 2_575 yes C(19) C(20) 1.367(4) . . yes C(20) H(13) 0.950 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S(1) C(3) 94.9(2) . 1_555 1_555 yes C(1) S(2) C(4) 94.7(2) . 1_555 1_555 yes C(2) S(3) C(5) 95.1(1) . 1_555 1_555 yes C(2) S(4) C(6) 94.9(1) . 1_555 1_555 yes C(3) S(5) C(7) 103.2(2) . 1_555 1_555 yes C(4) S(6) C(8) 99.4(2) . 1_555 1_555 yes C(5) S(7) C(9) 98.6(2) . 1_555 1_555 yes C(6) S(8) C(10) 103.2(2) . 1_555 1_555 yes C(11) S(9) C(12) 95.0(2) . 1_555 1_555 yes C(11) S(10) C(13) 95.4(2) . 1_555 1_555 yes C(12) S(11) C(14) 98.7(2) . 1_555 1_555 yes C(13) S(12) C(15) 103.2(2) . 1_555 1_555 yes S(1) C(1) S(2) 114.7(2) . 1_555 1_555 yes S(1) C(1) C(2) 122.1(2) . 1_555 1_555 yes S(2) C(1) C(2) 123.2(2) . 1_555 1_555 yes S(3) C(2) S(4) 114.8(2) . 1_555 1_555 yes S(3) C(2) C(1) 123.0(2) . 1_555 1_555 yes S(4) C(2) C(1) 122.2(2) . 1_555 1_555 yes S(1) C(3) S(5) 114.3(2) . 1_555 1_555 yes S(1) C(3) C(4) 116.9(3) . 1_555 1_555 yes S(5) C(3) C(4) 128.8(3) . 1_555 1_555 yes S(2) C(4) S(6) 115.5(2) . 1_555 1_555 yes S(2) C(4) C(3) 117.7(3) . 1_555 1_555 yes S(6) C(4) C(3) 126.8(3) . 1_555 1_555 yes S(3) C(5) S(7) 115.7(2) . 1_555 1_555 yes S(3) C(5) C(6) 117.5(2) . 1_555 1_555 yes S(7) C(5) C(6) 126.9(3) . 1_555 1_555 yes S(4) C(6) S(8) 113.7(2) . 1_555 1_555 yes S(4) C(6) C(5) 117.0(2) . 1_555 1_555 yes S(8) C(6) C(5) 129.4(3) . 1_555 1_555 yes S(5) C(7) C(8) 115.7(4) . 1_555 1_555 yes S(5) C(7) H(1) 107.9 . 1_555 1_555 no S(5) C(7) H(2) 107.9 . 1_555 1_555 no C(8) C(7) H(1) 107.9 . 1_555 1_555 no C(8) C(7) H(2) 107.9 . 1_555 1_555 no H(1) C(7) H(2) 109.5 . 1_555 1_555 no S(6) C(8) C(7) 114.6(5) . 1_555 1_555 yes S(6) C(8) H(3) 108.2 . 1_555 1_555 no S(6) C(8) H(4) 108.2 . 1_555 1_555 no C(7) C(8) H(3) 108.2 . 1_555 1_555 no C(7) C(8) H(4) 108.2 . 1_555 1_555 no H(3) C(8) H(4) 109.5 . 1_555 1_555 no S(7) C(9) C(10) 113.3(4) . 1_555 1_555 yes S(7) C(9) H(5) 108.5 . 1_555 1_555 no S(7) C(9) H(6) 108.5 . 1_555 1_555 no C(10) C(9) H(5) 108.5 . 1_555 1_555 no C(10) C(9) H(6) 108.5 . 1_555 1_555 no H(5) C(9) H(6) 109.5 . 1_555 1_555 no S(8) C(10) C(9) 114.0(3) . 1_555 1_555 yes S(8) C(10) H(7) 108.3 . 1_555 1_555 no S(8) C(10) H(8) 108.3 . 1_555 1_555 no C(9) C(10) H(7) 108.3 . 1_555 1_555 no C(9) C(10) H(8) 108.3 . 1_555 1_555 no H(7) C(10) H(8) 109.5 . 1_555 1_555 no S(9) C(11) S(10) 115.2(2) . 1_555 1_555 yes S(9) C(11) C(11) 122.1(3) . 1_555 2_568 yes S(10) C(11) C(11) 122.8(3) . 1_555 2_568 yes S(9) C(12) S(11) 115.9(2) . 1_555 1_555 yes S(9) C(12) C(13) 117.5(3) . 1_555 1_555 yes S(11) C(12) C(13) 126.6(3) . 1_555 1_555 yes S(10) C(13) S(12) 114.9(2) . 1_555 1_555 yes S(10) C(13) C(12) 116.5(3) . 1_555 1_555 yes S(12) C(13) C(12) 128.6(3) . 1_555 1_555 yes S(11) C(14) C(15) 114.7(4) . 1_555 1_555 yes S(11) C(14) H(9) 108.1 . 1_555 1_555 no S(11) C(14) H(10) 108.1 . 1_555 1_555 no C(15) C(14) H(9) 108.1 . 1_555 1_555 no C(15) C(14) H(10) 108.1 . 1_555 1_555 no H(9) C(14) H(10) 109.5 . 1_555 1_555 no S(12) C(15) C(14) 117.3(4) . 1_555 1_555 yes S(12) C(15) H(11) 107.5 . 1_555 1_555 no S(12) C(15) H(12) 107.5 . 1_555 1_555 no C(14) C(15) H(11) 107.5 . 1_555 1_555 no C(14) C(15) H(12) 107.5 . 1_555 1_555 no H(11) C(15) H(12) 109.5 . 1_555 1_555 no I(1) C(16) C(17) 175.9(4) . 1_555 1_555 yes C(16) C(17) C(18) 177.0(5) . 1_555 1_555 yes C(17) C(18) C(19) 120.0(4) . 1_555 1_555 yes C(17) C(18) C(20) 123.0(3) . 1_555 2_575 yes C(19) C(18) C(20) 117.1(3) . 1_555 2_575 yes F(1) C(19) C(18) 116.7(3) . 1_555 1_555 yes F(1) C(19) C(20) 119.2(3) . 1_555 1_555 yes C(18) C(19) C(20) 124.1(4) . 1_555 1_555 yes C(18) C(20) C(19) 118.8(3) . 2_575 1_555 yes C(18) C(20) H(13) 120.6 . 2_575 1_555 no C(19) C(20) H(13) 120.6 . 1_555 1_555 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 I(1) F(1) 3.392(3) . 2_576 ? S(8) S(11) 3.462(2) . 1_554 ? F(1) C(7) 3.318(6) . 2_577 ? C(15) C(20) 3.383(7) . 2_566 ? #------------------------------------------------------------------------------ data_ET3Br.pBIB #------------------------------------------------------------------------------ _audit_creation_date 'Wed Dec 17 17:25:08 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MXC Diffractometer Control' _computing_cell_refinement 'MXC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL93' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1611.81 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H28 Br I2 S24 ' _chemical_formula_moiety 'C40 H28 Br I2 S24 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.187(1) _cell_length_b 15.420(2) _cell_length_c 9.418(1) _cell_angle_alpha 99.83(1) _cell_angle_beta 106.89(1) _cell_angle_gamma 77.21(1) _cell_volume 1371.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.6 _cell_measurement_theta_max 14.7 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 793.00 _exptl_absorpt_coefficient_mu 2.824 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Science rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Mac Sciecne MXC18' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.05 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 0 3 -2 9 1 2 4 5 _diffrn_reflns_number 8318 _reflns_number_total 0 _reflns_number_observed 0 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_av_sigmaI/netI 0.234 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.07861 _diffrn_orient_matrix_UB_12 0.04932 _diffrn_orient_matrix_UB_13 -0.03707 _diffrn_orient_matrix_UB_21 -0.03640 _diffrn_orient_matrix_UB_22 -0.04103 _diffrn_orient_matrix_UB_23 -0.09047 _diffrn_orient_matrix_UB_31 -0.05815 _diffrn_orient_matrix_UB_32 -0.01910 _diffrn_orient_matrix_UB_33 0.05103 #------------------------------------------------------------------------------ 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 40 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S 0 24 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H 0 28 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br 0 1 -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I 0 2 -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags I(1) -0.15819(4) 1.00186(2) 0.64480(4) 0.0451(1) Uani d . 1.00 . Br(1) 0.0000 1.0000 1.0000 0.0409(2) Uani d . 0.50 S S(1) 0.5429(1) 0.58417(9) 0.7143(1) 0.0394(3) Uani d . 1.00 . S(2) 0.2855(1) 0.57244(9) 0.4724(2) 0.0409(3) Uani d . 1.00 . S(3) 0.4214(2) 0.7467(1) 0.8813(2) 0.0501(4) Uani d . 1.00 . S(4) 0.1152(2) 0.7307(1) 0.5974(2) 0.0529(4) Uani d . 1.00 . S(5) 0.8728(1) 0.58340(9) 1.3853(1) 0.0393(3) Uani d . 1.00 . S(6) 0.6192(1) 0.57465(9) 1.1374(2) 0.0402(3) Uani d . 1.00 . S(7) 1.0471(1) 0.42571(9) 1.2013(2) 0.0408(3) Uani d . 1.00 . S(8) 0.7943(1) 0.42097(9) 0.9518(1) 0.0385(3) Uani d . 1.00 . S(9) 0.7541(2) 0.7472(1) 1.5490(2) 0.0517(4) Uani d . 1.00 . S(10) 0.4510(2) 0.7363(1) 1.2611(2) 0.0533(4) Uani d . 1.00 . S(11) 1.2147(2) 0.2654(1) 1.0736(2) 0.0515(4) Uani d . 1.00 . S(12) 0.9118(2) 0.2613(1) 0.7801(2) 0.0486(4) Uani d . 1.00 . C(1) 0.4638(5) 0.5325(3) 0.5395(5) 0.0299(9) Uani d . 1.00 . C(2) 0.3952(5) 0.6665(3) 0.7243(5) 0.0315(9) Uani d . 1.00 . C(3) 0.2778(5) 0.6604(3) 0.6153(6) 0.0331(9) Uani d . 1.00 . C(4) 0.2459(8) 0.7973(8) 0.880(1) 0.096(4) Uani d . 1.00 . C(5) 0.1371(10) 0.790(1) 0.774(1) 0.149(7) Uani d . 1.00 . C(6) 0.7965(5) 0.5336(3) 1.2077(5) 0.0303(9) Uani d . 1.00 . C(7) 0.8699(5) 0.4685(3) 1.1305(5) 0.0298(9) Uani d . 1.00 . C(8) 0.7261(5) 0.6676(3) 1.3928(5) 0.0310(9) Uani d . 1.00 . C(9) 0.6108(5) 0.6633(3) 1.2803(5) 0.0324(9) Uani d . 1.00 . C(10) 1.0550(5) 0.3393(3) 1.0556(5) 0.0325(9) Uani d . 1.00 . C(11) 0.9393(5) 0.3368(3) 0.9414(5) 0.0309(9) Uani d . 1.00 . C(12) 0.5832(7) 0.8154(5) 1.5361(8) 0.055(2) Uani d . 1.00 . C(13) 0.4620(7) 0.7710(5) 1.4535(7) 0.049(1) Uani d . 1.00 . C(14) 1.2025(6) 0.2301(4) 0.8787(7) 0.042(1) Uani d . 1.00 . C(15) 1.0781(6) 0.1869(4) 0.8016(7) 0.045(1) Uani d . 1.00 . C(16) -0.5632(6) 1.0037(4) 0.1146(6) 0.043(1) Uani d . 1.00 . C(17) -0.4196(5) 0.9996(3) 0.1486(6) 0.038(1) Uani d . 1.00 . C(18) -0.3580(6) 0.9963(4) 0.0336(6) 0.042(1) Uani d . 1.00 . C(19) -0.3343(5) 1.0005(3) 0.3085(6) 0.0302(9) Uani d . 1.00 . C(20) -0.2672(7) 0.9996(4) 0.4311(7) 0.050(1) Uani d . 1.00 . H(1) 0.2276 0.7681 0.9565 0.1188 Uiso calc . 1.00 . H(2) 0.2458 0.8565 0.9134 0.1188 Uiso calc . 1.00 . H(3) 0.1077 0.8533 0.7518 0.1688 Uiso calc . 1.00 . H(4) 0.0720 0.7770 0.8139 0.1688 Uiso calc . 1.00 . H(5) 0.5741 0.8365 1.6338 0.0687 Uiso calc . 1.00 . H(6) 0.5767 0.8658 1.4853 0.0687 Uiso calc . 1.00 . H(7) 0.3778 0.8113 1.4606 0.0598 Uiso calc . 1.00 . H(8) 0.4688 0.7193 1.5002 0.0598 Uiso calc . 1.00 . H(9) 1.1968 0.2815 0.8320 0.0510 Uiso calc . 1.00 . H(10) 1.2855 0.1889 0.8708 0.0510 Uiso calc . 1.00 . H(11) 1.0780 0.1412 0.8583 0.0536 Uiso calc . 1.00 . H(12) 1.0861 0.1608 0.7052 0.0536 Uiso calc . 1.00 . H(13) -0.6065 1.0069 0.1925 0.0511 Uiso calc . 1.00 . H(14) -0.2588 0.9940 0.0567 0.0513 Uiso calc . 1.00 . 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 I(1) 0.0449(2) 0.0448(2) 0.0394(2) -0.0076(2) 0.0035(2) 0.0023(1) Br(1) 0.0358(4) 0.0515(4) 0.0339(4) -0.0036(3) 0.0127(3) 0.0004(3) S(1) 0.0353(6) 0.0327(6) 0.0357(6) 0.0099(5) 0.0056(5) -0.0070(5) S(2) 0.0324(6) 0.0345(6) 0.0437(7) 0.0014(5) 0.0076(5) -0.0140(5) S(3) 0.0358(7) 0.0533(8) 0.0453(7) 0.0017(6) 0.0099(6) -0.0236(6) S(4) 0.0304(6) 0.0611(9) 0.0469(8) 0.0115(6) 0.0075(6) -0.0176(7) S(5) 0.0377(6) 0.0324(6) 0.0328(6) 0.0091(5) 0.0042(5) -0.0074(5) S(6) 0.0342(6) 0.0355(6) 0.0392(6) 0.0003(5) 0.0067(5) -0.0137(5) S(7) 0.0355(6) 0.0362(6) 0.0384(6) 0.0014(5) 0.0070(5) -0.0136(5) S(8) 0.0372(6) 0.0319(6) 0.0321(6) 0.0092(5) 0.0045(5) -0.0066(4) S(9) 0.0364(7) 0.0543(9) 0.0454(7) 0.0026(6) 0.0078(6) -0.0266(7) S(10) 0.0312(6) 0.067(1) 0.0425(7) 0.0125(6) 0.0076(5) -0.0144(7) S(11) 0.0310(6) 0.0628(10) 0.0426(7) 0.0121(6) 0.0083(5) -0.0135(6) S(12) 0.0357(6) 0.0512(8) 0.0399(7) 0.0064(6) 0.0065(5) -0.0210(6) C(1) 0.033(2) 0.021(2) 0.033(2) 0.002(2) 0.012(2) -0.001(2) C(2) 0.032(2) 0.026(2) 0.031(2) 0.001(2) 0.010(2) -0.005(2) C(3) 0.030(2) 0.029(2) 0.037(2) 0.001(2) 0.014(2) -0.005(2) C(4) 0.039(3) 0.130(8) 0.083(6) 0.004(4) 0.021(4) -0.067(6) C(5) 0.056(5) 0.24(2) 0.064(5) 0.056(7) 0.001(4) -0.076(8) C(6) 0.033(2) 0.024(2) 0.029(2) 0.000(2) 0.009(2) -0.005(2) C(7) 0.033(2) 0.023(2) 0.030(2) 0.001(2) 0.011(2) -0.003(2) C(8) 0.031(2) 0.028(2) 0.031(2) -0.002(2) 0.013(2) -0.007(2) C(9) 0.028(2) 0.033(2) 0.030(2) 0.001(2) 0.010(2) -0.009(2) C(10) 0.028(2) 0.033(2) 0.031(2) 0.000(2) 0.009(2) -0.007(2) C(11) 0.032(2) 0.028(2) 0.030(2) -0.002(2) 0.012(2) -0.004(2) C(12) 0.046(3) 0.051(4) 0.052(3) 0.008(3) 0.013(3) -0.013(3) C(13) 0.042(3) 0.056(3) 0.047(3) 0.004(3) 0.022(3) 0.000(3) C(14) 0.041(3) 0.038(3) 0.048(3) -0.002(2) 0.024(2) -0.006(2) C(15) 0.038(3) 0.038(3) 0.049(3) 0.009(2) 0.014(2) -0.008(2) C(16) 0.039(3) 0.061(3) 0.032(2) -0.005(2) 0.018(2) 0.005(2) C(17) 0.034(2) 0.034(2) 0.039(2) -0.001(2) 0.005(2) 0.003(2) C(18) 0.034(2) 0.045(3) 0.044(3) -0.002(2) 0.012(2) 0.005(2) C(19) 0.025(2) 0.026(2) 0.035(2) -0.001(2) 0.006(2) -0.001(2) C(20) 0.046(3) 0.047(3) 0.049(3) -0.004(2) 0.006(3) 0.004(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^) + (0.1656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 0 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_obs 0.0830 _refine_ls_wR_factor_all 0.2202 _refine_ls_wR_factor_obs ? _refine_ls_goodness_of_fit_all 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_goodness_of_fit_obs ? _refine_ls_shift/esd_max -10.4270 _refine_ls_shift/esd_mean 0.0430 _refine_diff_density_min -2.04 _refine_diff_density_max 11.48 _refine_diff_density_rms 0.35 _atoms_sites_solution_primary 'direct methods' _atoms_sites_solution_secondary 'Fourier difference' #------------------------------------------------------------------------------ _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 I(1) C(20) 1.995(6) 1_555 1_555 yes S(1) C(1) 1.749(4) 1_555 1_555 yes S(1) C(2) 1.755(5) 1_555 1_555 yes S(2) C(1) 1.746(5) 1_555 1_555 yes S(2) C(3) 1.746(5) 1_555 1_555 yes S(3) C(2) 1.755(5) 1_555 1_555 yes S(3) C(4) 1.783(8) 1_555 1_555 yes S(4) C(3) 1.747(5) 1_555 1_555 yes S(4) C(5) 1.73(1) 1_555 1_555 yes S(5) C(6) 1.749(4) 1_555 1_555 yes S(5) C(8) 1.759(5) 1_555 1_555 yes S(6) C(6) 1.744(4) 1_555 1_555 yes S(6) C(9) 1.754(5) 1_555 1_555 yes S(7) C(7) 1.750(4) 1_555 1_555 yes S(7) C(10) 1.748(5) 1_555 1_555 yes S(8) C(7) 1.743(4) 1_555 1_555 yes S(8) C(11) 1.751(5) 1_555 1_555 yes S(9) C(8) 1.746(5) 1_555 1_555 yes S(9) C(12) 1.806(7) 1_555 1_555 yes S(10) C(9) 1.742(5) 1_555 1_555 yes S(10) C(13) 1.778(7) 1_555 1_555 yes S(11) C(10) 1.750(5) 1_555 1_555 yes S(11) C(14) 1.799(6) 1_555 1_555 yes S(12) C(11) 1.743(5) 1_555 1_555 yes S(12) C(15) 1.802(6) 1_555 1_555 yes C(1) C(1) 1.356(9) 1_555 2_666 yes C(2) C(3) 1.340(6) 1_555 1_555 yes C(4) C(5) 1.27(1) 1_555 1_555 yes C(6) C(7) 1.353(6) 1_555 1_555 yes C(8) C(9) 1.339(6) 1_555 1_555 yes C(10) C(11) 1.347(6) 1_555 1_555 yes C(12) C(13) 1.494(10) 1_555 1_555 yes C(14) C(15) 1.501(8) 1_555 1_555 yes C(16) C(17) 1.393(8) 1_555 1_555 yes C(16) C(18) 1.394(7) 1_555 2_475 yes C(17) C(18) 1.390(9) 1_555 1_555 yes C(17) C(19) 1.503(7) 1_555 1_555 yes C(19) C(20) 1.160(8) 1_555 1_555 yes #------------------------------------------------------------------------------ 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(2) 94.6(2) 1_555 1_555 1_555 yes C(1) S(2) C(3) 95.1(2) 1_555 1_555 1_555 yes C(2) S(3) C(4) 101.0(4) 1_555 1_555 1_555 yes C(3) S(4) C(5) 101.2(4) 1_555 1_555 1_555 yes C(6) S(5) C(8) 94.7(2) 1_555 1_555 1_555 yes C(6) S(6) C(9) 95.0(2) 1_555 1_555 1_555 yes C(7) S(7) C(10) 95.0(2) 1_555 1_555 1_555 yes C(7) S(8) C(11) 95.2(2) 1_555 1_555 1_555 yes C(8) S(9) C(12) 103.3(3) 1_555 1_555 1_555 yes C(9) S(10) C(13) 98.5(3) 1_555 1_555 1_555 yes C(10) S(11) C(14) 98.6(2) 1_555 1_555 1_555 yes C(11) S(12) C(15) 102.8(2) 1_555 1_555 1_555 yes S(1) C(1) S(2) 115.1(3) 1_555 1_555 1_555 yes S(1) C(1) C(1) 122.5(5) 1_555 1_555 2_666 yes S(2) C(1) C(1) 122.4(4) 1_555 1_555 2_666 yes S(1) C(2) S(3) 114.3(2) 1_555 1_555 1_555 yes S(1) C(2) C(3) 117.5(4) 1_555 1_555 1_555 yes S(3) C(2) C(3) 128.2(4) 1_555 1_555 1_555 yes S(2) C(3) S(4) 115.1(3) 1_555 1_555 1_555 yes S(2) C(3) C(2) 117.2(4) 1_555 1_555 1_555 yes S(4) C(3) C(2) 127.8(4) 1_555 1_555 1_555 yes S(3) C(4) C(5) 127.4(8) 1_555 1_555 1_555 yes S(3) C(4) H(1) 102.8(6) 1_555 1_555 1_555 no S(3) C(4) H(2) 106.8(7) 1_555 1_555 1_555 no C(5) C(4) H(1) 100(1) 1_555 1_555 1_555 no C(5) C(4) H(2) 109(1) 1_555 1_555 1_555 no H(1) C(4) H(2) 108.6(10) 1_555 1_555 1_555 no S(4) C(5) C(4) 131.2(9) 1_555 1_555 1_555 yes S(4) C(5) H(3) 102.8(8) 1_555 1_555 1_555 no S(4) C(5) H(4) 106.1(10) 1_555 1_555 1_555 no C(4) C(5) H(3) 99(1) 1_555 1_555 1_555 no C(4) C(5) H(4) 107(1) 1_555 1_555 1_555 no H(3) C(5) H(4) 108(1) 1_555 1_555 1_555 no S(5) C(6) S(6) 115.0(3) 1_555 1_555 1_555 yes S(5) C(6) C(7) 122.5(3) 1_555 1_555 1_555 yes S(6) C(6) C(7) 122.6(3) 1_555 1_555 1_555 yes S(7) C(7) S(8) 114.9(3) 1_555 1_555 1_555 yes S(7) C(7) C(6) 122.9(3) 1_555 1_555 1_555 yes S(8) C(7) C(6) 122.2(3) 1_555 1_555 1_555 yes S(5) C(8) S(9) 113.8(2) 1_555 1_555 1_555 yes S(5) C(8) C(9) 117.3(4) 1_555 1_555 1_555 yes S(9) C(8) C(9) 129.0(4) 1_555 1_555 1_555 yes S(6) C(9) S(10) 115.9(2) 1_555 1_555 1_555 yes S(6) C(9) C(8) 117.2(4) 1_555 1_555 1_555 yes S(10) C(9) C(8) 126.9(4) 1_555 1_555 1_555 yes S(7) C(10) S(11) 115.8(2) 1_555 1_555 1_555 yes S(7) C(10) C(11) 117.3(4) 1_555 1_555 1_555 yes S(11) C(10) C(11) 126.9(4) 1_555 1_555 1_555 yes S(8) C(11) S(12) 113.8(2) 1_555 1_555 1_555 yes S(8) C(11) C(10) 117.0(4) 1_555 1_555 1_555 yes S(12) C(11) C(10) 129.2(4) 1_555 1_555 1_555 yes S(9) C(12) C(13) 116.1(5) 1_555 1_555 1_555 yes S(9) C(12) H(5) 108.8(5) 1_555 1_555 1_555 no S(9) C(12) H(6) 107.9(6) 1_555 1_555 1_555 no C(13) C(12) H(5) 108.0(7) 1_555 1_555 1_555 no C(13) C(12) H(6) 107.0(6) 1_555 1_555 1_555 no H(5) C(12) H(6) 108.8(6) 1_555 1_555 1_555 no S(10) C(13) C(12) 114.9(6) 1_555 1_555 1_555 yes S(10) C(13) H(7) 107.9(5) 1_555 1_555 1_555 no S(10) C(13) H(8) 107.9(5) 1_555 1_555 1_555 no C(12) C(13) H(7) 109.0(6) 1_555 1_555 1_555 no C(12) C(13) H(8) 108.1(5) 1_555 1_555 1_555 no H(7) C(13) H(8) 108.8(8) 1_555 1_555 1_555 no S(11) C(14) C(15) 112.8(5) 1_555 1_555 1_555 yes S(11) C(14) H(9) 108.0(4) 1_555 1_555 1_555 no S(11) C(14) H(10) 108.2(4) 1_555 1_555 1_555 no C(15) C(14) H(9) 109.4(5) 1_555 1_555 1_555 no C(15) C(14) H(10) 109.4(5) 1_555 1_555 1_555 no H(9) C(14) H(10) 109.0(7) 1_555 1_555 1_555 no S(12) C(15) C(14) 115.0(4) 1_555 1_555 1_555 yes S(12) C(15) H(11) 107.5(5) 1_555 1_555 1_555 no S(12) C(15) H(12) 107.8(4) 1_555 1_555 1_555 no C(14) C(15) H(11) 108.4(5) 1_555 1_555 1_555 no C(14) C(15) H(12) 108.7(6) 1_555 1_555 1_555 no H(11) C(15) H(12) 109.3(6) 1_555 1_555 1_555 no C(17) C(16) C(18) 119.6(6) 1_555 1_555 2_475 yes C(17) C(16) H(13) 119.8(5) 1_555 1_555 1_555 no C(18) C(16) H(13) 120.7(6) 2_475 1_555 1_555 no C(16) C(17) C(18) 119.1(5) 1_555 1_555 1_555 yes C(16) C(17) C(19) 119.8(5) 1_555 1_555 1_555 yes C(18) C(17) C(19) 121.1(5) 1_555 1_555 1_555 yes C(16) C(18) C(17) 121.3(5) 2_475 1_555 1_555 yes C(16) C(18) H(14) 119.3(6) 2_475 1_555 1_555 no C(17) C(18) H(14) 119.4(5) 1_555 1_555 1_555 no C(17) C(19) C(20) 178.7(5) 1_555 1_555 1_555 yes I(1) C(20) C(19) 177.6(6) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 S(3) S(11) 3.572(2) 1_555 2_767 ? S(4) S(9) 3.529(2) 1_555 1_454 ? S(9) S(11) 3.510(2) 1_555 2_768 ? S(10) S(12) 3.595(2) 1_555 2_667 ? C(2) C(13) 3.530(10) 1_555 1_554 ? C(3) C(13) 3.57(1) 1_555 1_554 ? C(4) C(18) 3.50(1) 1_555 2_576 ? C(8) C(14) 3.538(9) 1_555 2_767 ? C(9) C(14) 3.526(10) 1_555 2_767 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_General _audit_creation_date 'Thu Oct 7 00:42:09 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Hiroshi M. Yamamoto' _publ_contact_author_address ; Hirosawa, Wako-shi, Saitama 351-0198 (Japan) ; _publ_contact_author_email ' yhiroshi@postman.riken.go.jp ' _publ_contact_author_fax ' +81-(0)48-462-4611 ' _publ_contact_author_phone ' +81-(0)48-467-9410 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' ' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # _publ_section_title ; Structural and physical properties of conducting cation radical satls containing supramolecular assmblies based on pBIB derivatives (pBIB=p-Bis(iodoethynyl)benzene) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_ET3Cl.DFBIB #------------------------------------------------------------------------------ _audit_creation_date 'Sat May 23 21:59:14 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MacScience Diffractometer Control' _computing_cell_refinement 'MacScience Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1603.34 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H26 Cl F2 I2 S24 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.3480(6) _cell_length_b 15.550(1) _cell_length_c 9.2610(5) _cell_angle_alpha 98.125(5) _cell_angle_beta 107.703(4) _cell_angle_gamma 75.622(3) _cell_volume 1371.7(1) _cell_formula_units_Z 1 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 791.00 _exptl_absorpt_coefficient_mu 2.150 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Science rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Mac Sciecne DIP320' _diffrn_measurement_method _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l _diffrn_reflns_number 13318 _reflns_number_total 5895 _reflns_number_observed 5137 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 40 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 24 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 26 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 1 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; I 0 2 -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 2 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags I(1) -0.13115(2) 0.99951(1) 0.64710(2) 0.04380(7) Uani d . 1.00 . Cl(1) 0.0000 1.0000 1.0000 0.0513(3) Uani d . 0.50 S S(1) 0.53908(8) 0.58746(5) 0.7070(1) 0.0493(2) Uani d . 1.00 . S(2) 0.28433(8) 0.57190(5) 0.4658(1) 0.0502(2) Uani d . 1.00 . S(3) 0.41243(8) 0.75026(6) 0.8618(1) 0.0589(3) Uani d . 1.00 . S(4) 0.10775(8) 0.73115(7) 0.5809(1) 0.0619(3) Uani d . 1.00 . S(5) 0.86905(8) 0.58277(5) 1.3810(1) 0.0498(2) Uani d . 1.00 . S(6) 0.61247(8) 0.57390(5) 1.1362(1) 0.0506(2) Uani d . 1.00 . S(7) 1.04428(8) 0.42989(5) 1.1973(1) 0.0500(2) Uani d . 1.00 . S(8) 0.78774(8) 0.41887(5) 0.9532(1) 0.0456(2) Uani d . 1.00 . S(9) 0.75068(9) 0.74820(7) 1.5353(1) 0.0656(3) Uani d . 1.00 . S(10) 0.44509(9) 0.73809(8) 1.2494(1) 0.0749(3) Uani d . 1.00 . S(11) 1.21792(8) 0.27145(7) 1.0774(1) 0.0624(3) Uani d . 1.00 . S(12) 0.91003(8) 0.25790(6) 0.7929(1) 0.0566(3) Uani d . 1.00 . F(1) -0.5835(2) 0.9983(1) 0.2483(2) 0.0578(6) Uani d . 1.00 . C(1) 0.4626(3) 0.5339(2) 0.5368(4) 0.0381(8) Uani d . 1.00 . C(2) 0.3891(3) 0.6691(2) 0.7125(4) 0.0375(8) Uani d . 1.00 . C(3) 0.2724(3) 0.6614(2) 0.6011(4) 0.0415(9) Uani d . 1.00 . C(4) 0.2363(4) 0.8121(2) 0.8490(5) 0.059(1) Uani d . 1.00 . C(5) 0.1244(4) 0.7647(2) 0.7764(5) 0.057(1) Uani d . 1.00 . C(6) 0.7916(3) 0.5336(2) 1.2050(4) 0.0366(8) Uani d . 1.00 . C(7) 0.8647(3) 0.4691(2) 1.1284(4) 0.0365(8) Uani d . 1.00 . C(8) 0.7225(3) 0.6677(2) 1.3857(4) 0.0385(8) Uani d . 1.00 . C(9) 0.6058(3) 0.6636(2) 1.2730(4) 0.0434(9) Uani d . 1.00 . C(10) 1.0546(3) 0.3424(2) 1.0571(4) 0.0389(8) Uani d . 1.00 . C(11) 0.9372(3) 0.3369(2) 0.9450(4) 0.0360(8) Uani d . 1.00 . C(12) 0.5829(4) 0.8206(3) 1.5127(5) 0.074(1) Uani d . 1.00 . C(13) 0.4618(4) 0.7810(3) 1.4398(5) 0.069(1) Uani d . 1.00 . C(14) 1.1985(3) 0.2302(2) 0.8833(5) 0.051(1) Uani d . 1.00 . C(15) 1.0791(3) 0.1848(2) 0.8184(4) 0.053(1) Uani d . 1.00 . C(16) -0.5432(3) 0.9994(2) 0.1225(4) 0.0384(8) Uani d . 1.00 . C(17) -0.4029(3) 1.0000(2) 0.1456(4) 0.0366(8) Uani d . 1.00 . C(18) -0.3611(3) 1.0001(2) 0.0158(4) 0.0385(8) Uani d . 1.00 . C(19) -0.3107(3) 1.0002(2) 0.2967(4) 0.0416(8) Uani d . 1.00 . C(20) -0.2394(3) 1.0000(2) 0.4251(4) 0.0440(9) Uani d . 1.00 . H(1) 0.2310 0.8317 0.9495 0.0723 Uiso calc . 1.00 . H(2) 0.2195 0.8624 0.7930 0.0723 Uiso calc . 1.00 . H(3) 0.0387 0.8021 0.7846 0.0682 Uiso calc . 1.00 . H(4) 0.1420 0.7125 0.8289 0.0682 Uiso calc . 1.00 . H(5) 0.5761 0.8451 1.6094 0.0955 Uiso calc . 1.00 . H(6) 0.5772 0.8662 1.4511 0.0955 Uiso calc . 1.00 . H(7) 0.3808 0.8252 1.4425 0.0821 Uiso calc . 1.00 . H(8) 0.4681 0.7333 1.4980 0.0821 Uiso calc . 1.00 . H(9) 1.1838 0.2789 0.8242 0.0618 Uiso calc . 1.00 . H(10) 1.2813 0.1888 0.8765 0.0618 Uiso calc . 1.00 . H(11) 1.0878 0.1423 0.8874 0.0649 Uiso calc . 1.00 . H(12) 1.0857 0.1562 0.7240 0.0649 Uiso calc . 1.00 . H(13) -0.2675 1.0003 0.0250 0.0464 Uiso calc . 1.00 . 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 I(1) 0.0346(1) 0.0558(1) 0.0355(2) -0.00841(8) 0.00288(8) 0.0021(1) Cl(1) 0.0420(5) 0.0735(8) 0.0343(8) -0.0096(5) 0.0059(5) 0.0054(6) S(1) 0.0420(4) 0.0432(4) 0.0454(6) 0.0068(3) 0.0045(4) -0.0085(4) S(2) 0.0399(4) 0.0464(4) 0.0523(7) -0.0022(3) 0.0088(4) -0.0150(4) S(3) 0.0427(4) 0.0595(5) 0.0588(7) -0.0018(4) 0.0114(4) -0.0261(5) S(4) 0.0353(4) 0.0737(6) 0.0578(8) 0.0059(4) 0.0099(4) -0.0201(5) S(5) 0.0453(4) 0.0426(4) 0.0422(6) 0.0080(3) 0.0028(4) -0.0088(4) S(6) 0.0396(4) 0.0478(4) 0.0520(7) -0.0031(3) 0.0083(4) -0.0172(4) S(7) 0.0388(4) 0.0470(4) 0.0519(7) -0.0032(3) 0.0076(4) -0.0159(4) S(8) 0.0404(4) 0.0411(4) 0.0400(6) 0.0069(3) 0.0055(3) -0.0067(4) S(9) 0.0458(4) 0.0678(6) 0.0611(8) 0.0000(4) 0.0091(4) -0.0342(5) S(10) 0.0362(4) 0.0918(7) 0.0675(9) 0.0104(4) 0.0079(4) -0.0333(6) S(11) 0.0327(4) 0.0766(6) 0.0593(8) 0.0046(4) 0.0094(4) -0.0209(5) S(12) 0.0411(4) 0.0585(5) 0.0501(7) 0.0045(3) 0.0069(4) -0.0227(4) F(1) 0.049(1) 0.089(1) 0.042(1) -0.0173(10) 0.0209(9) 0.001(1) C(1) 0.041(1) 0.032(1) 0.038(2) -0.002(1) 0.013(1) -0.002(1) C(2) 0.041(1) 0.035(1) 0.036(2) -0.004(1) 0.016(1) -0.006(1) C(3) 0.036(1) 0.039(1) 0.047(2) -0.001(1) 0.017(1) -0.006(1) C(4) 0.053(2) 0.059(2) 0.057(3) -0.003(2) 0.019(2) -0.018(2) C(5) 0.048(2) 0.061(2) 0.059(3) 0.002(1) 0.022(2) -0.001(2) C(6) 0.040(1) 0.031(1) 0.035(2) -0.003(1) 0.011(1) -0.002(1) C(7) 0.040(1) 0.031(1) 0.035(2) -0.004(1) 0.011(1) -0.002(1) C(8) 0.040(1) 0.039(1) 0.036(2) -0.006(1) 0.018(1) -0.011(1) C(9) 0.035(1) 0.045(2) 0.047(2) -0.004(1) 0.018(1) -0.011(2) C(10) 0.035(1) 0.041(2) 0.039(2) -0.003(1) 0.016(1) -0.007(1) C(11) 0.037(1) 0.036(1) 0.034(2) -0.003(1) 0.015(1) -0.004(1) C(12) 0.061(2) 0.060(2) 0.073(3) 0.008(2) 0.004(2) -0.021(2) C(13) 0.052(2) 0.076(3) 0.066(3) 0.012(2) 0.025(2) -0.008(2) C(14) 0.046(2) 0.046(2) 0.062(3) 0.000(1) 0.027(2) -0.002(2) C(15) 0.044(2) 0.046(2) 0.057(3) 0.005(1) 0.012(2) -0.008(2) C(16) 0.038(1) 0.041(2) 0.036(2) -0.007(1) 0.012(1) -0.002(1) C(17) 0.034(1) 0.035(1) 0.035(2) -0.005(1) 0.004(1) -0.002(1) C(18) 0.030(1) 0.039(1) 0.045(2) -0.007(1) 0.010(1) -0.002(1) C(19) 0.037(1) 0.042(2) 0.043(2) -0.006(1) 0.009(1) -0.002(1) C(20) 0.036(1) 0.051(2) 0.039(2) -0.008(1) 0.004(1) 0.002(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0009(5) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5137 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0327 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0408 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.762 _refine_ls_shift/esd_max 0.2520 _refine_ls_shift/esd_mean 0.0210 _refine_diff_density_min -0.86 _refine_diff_density_max 0.99 _atoms_sites_solution_primary 'direct methods' _atoms_sites_solution_secondary 'Fourier difference' #------------------------------------------------------------------------------ _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 I(1) C(20) 2.021(3) 1_555 1_555 yes S(1) C(1) 1.733(3) 1_555 1_555 yes S(1) C(2) 1.753(3) 1_555 1_555 yes S(2) C(1) 1.736(3) 1_555 1_555 yes S(2) C(3) 1.742(3) 1_555 1_555 yes S(3) C(2) 1.737(3) 1_555 1_555 yes S(3) C(4) 1.814(3) 1_555 1_555 yes S(4) C(3) 1.749(3) 1_555 1_555 yes S(4) C(5) 1.780(4) 1_555 1_555 yes S(5) C(6) 1.744(3) 1_555 1_555 yes S(5) C(8) 1.754(3) 1_555 1_555 yes S(6) C(6) 1.747(3) 1_555 1_555 yes S(6) C(9) 1.749(3) 1_555 1_555 yes S(7) C(7) 1.749(3) 1_555 1_555 yes S(7) C(10) 1.749(3) 1_555 1_555 yes S(8) C(7) 1.744(3) 1_555 1_555 yes S(8) C(11) 1.757(3) 1_555 1_555 yes S(9) C(8) 1.737(3) 1_555 1_555 yes S(9) C(12) 1.789(4) 1_555 1_555 yes S(10) C(9) 1.746(3) 1_555 1_555 yes S(10) C(13) 1.767(5) 1_555 1_555 yes S(11) C(10) 1.746(3) 1_555 1_555 yes S(11) C(14) 1.789(4) 1_555 1_555 yes S(12) C(11) 1.737(3) 1_555 1_555 yes S(12) C(15) 1.801(3) 1_555 1_555 yes F(1) C(16) 1.355(4) 1_555 1_555 yes C(1) C(1) 1.375(6) 1_555 2_666 yes C(2) C(3) 1.348(4) 1_555 1_555 yes C(4) C(5) 1.465(5) 1_555 1_555 yes C(6) C(7) 1.352(4) 1_555 1_555 yes C(8) C(9) 1.344(4) 1_555 1_555 yes C(10) C(11) 1.349(4) 1_555 1_555 yes C(12) C(13) 1.469(6) 1_555 1_555 yes C(14) C(15) 1.500(5) 1_555 1_555 yes C(16) C(17) 1.403(4) 1_555 1_555 yes C(16) C(18) 1.360(4) 1_555 2_475 yes C(17) C(18) 1.397(5) 1_555 1_555 yes C(17) C(19) 1.434(4) 1_555 1_555 yes C(19) C(20) 1.193(5) 1_555 1_555 yes #------------------------------------------------------------------------------ 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(2) 95.3(1) 1_555 1_555 1_555 yes C(1) S(2) C(3) 95.2(1) 1_555 1_555 1_555 yes C(2) S(3) C(4) 102.9(2) 1_555 1_555 1_555 yes C(3) S(4) C(5) 98.2(2) 1_555 1_555 1_555 yes C(6) S(5) C(8) 95.1(1) 1_555 1_555 1_555 yes C(6) S(6) C(9) 94.8(1) 1_555 1_555 1_555 yes C(7) S(7) C(10) 95.2(1) 1_555 1_555 1_555 yes C(7) S(8) C(11) 95.3(1) 1_555 1_555 1_555 yes C(8) S(9) C(12) 103.4(2) 1_555 1_555 1_555 yes C(9) S(10) C(13) 99.5(2) 1_555 1_555 1_555 yes C(10) S(11) C(14) 99.0(2) 1_555 1_555 1_555 yes C(11) S(12) C(15) 103.0(1) 1_555 1_555 1_555 yes S(1) C(1) S(2) 115.2(2) 1_555 1_555 1_555 yes S(1) C(1) C(1) 122.4(3) 1_555 1_555 2_666 yes S(2) C(1) C(1) 122.3(3) 1_555 1_555 2_666 yes S(1) C(2) S(3) 114.8(2) 1_555 1_555 1_555 yes S(1) C(2) C(3) 116.4(2) 1_555 1_555 1_555 yes S(3) C(2) C(3) 128.7(2) 1_555 1_555 1_555 yes S(2) C(3) S(4) 116.3(2) 1_555 1_555 1_555 yes S(2) C(3) C(2) 117.3(2) 1_555 1_555 1_555 yes S(4) C(3) C(2) 126.3(2) 1_555 1_555 1_555 yes S(3) C(4) C(5) 116.9(2) 1_555 1_555 1_555 yes S(3) C(4) H(1) 107.7(3) 1_555 1_555 1_555 no S(3) C(4) H(2) 107.7(3) 1_555 1_555 1_555 no C(5) C(4) H(1) 107.6(3) 1_555 1_555 1_555 no C(5) C(4) H(2) 107.5(3) 1_555 1_555 1_555 no H(1) C(4) H(2) 109.3(3) 1_555 1_555 1_555 no S(4) C(5) C(4) 114.2(3) 1_555 1_555 1_555 yes S(4) C(5) H(3) 108.2(3) 1_555 1_555 1_555 no S(4) C(5) H(4) 107.9(3) 1_555 1_555 1_555 no C(4) C(5) H(3) 108.9(3) 1_555 1_555 1_555 no C(4) C(5) H(4) 108.5(3) 1_555 1_555 1_555 no H(3) C(5) H(4) 109.1(4) 1_555 1_555 1_555 no S(5) C(6) S(6) 114.7(2) 1_555 1_555 1_555 yes S(5) C(6) C(7) 122.5(2) 1_555 1_555 1_555 yes S(6) C(6) C(7) 122.8(2) 1_555 1_555 1_555 yes S(7) C(7) S(8) 114.8(2) 1_555 1_555 1_555 yes S(7) C(7) C(6) 122.5(2) 1_555 1_555 1_555 yes S(8) C(7) C(6) 122.8(2) 1_555 1_555 1_555 yes S(5) C(8) S(9) 114.5(2) 1_555 1_555 1_555 yes S(5) C(8) C(9) 116.7(2) 1_555 1_555 1_555 yes S(9) C(8) C(9) 128.7(2) 1_555 1_555 1_555 yes S(6) C(9) S(10) 115.8(2) 1_555 1_555 1_555 yes S(6) C(9) C(8) 117.5(2) 1_555 1_555 1_555 yes S(10) C(9) C(8) 126.7(3) 1_555 1_555 1_555 yes S(7) C(10) S(11) 115.9(2) 1_555 1_555 1_555 yes S(7) C(10) C(11) 117.3(2) 1_555 1_555 1_555 yes S(11) C(10) C(11) 126.9(2) 1_555 1_555 1_555 yes S(8) C(11) S(12) 114.1(2) 1_555 1_555 1_555 yes S(8) C(11) C(10) 116.8(2) 1_555 1_555 1_555 yes S(12) C(11) C(10) 129.1(2) 1_555 1_555 1_555 yes S(9) C(12) C(13) 116.9(3) 1_555 1_555 1_555 yes S(9) C(12) H(5) 107.9(3) 1_555 1_555 1_555 no S(9) C(12) H(6) 107.2(4) 1_555 1_555 1_555 no C(13) C(12) H(5) 107.7(4) 1_555 1_555 1_555 no C(13) C(12) H(6) 106.7(4) 1_555 1_555 1_555 no H(5) C(12) H(6) 110.4(4) 1_555 1_555 1_555 no S(10) C(13) C(12) 115.8(3) 1_555 1_555 1_555 yes S(10) C(13) H(7) 108.2(3) 1_555 1_555 1_555 no S(10) C(13) H(8) 107.8(3) 1_555 1_555 1_555 no C(12) C(13) H(7) 108.0(4) 1_555 1_555 1_555 no C(12) C(13) H(8) 107.7(4) 1_555 1_555 1_555 no H(7) C(13) H(8) 109.2(4) 1_555 1_555 1_555 no S(11) C(14) C(15) 113.4(3) 1_555 1_555 1_555 yes S(11) C(14) H(9) 108.6(3) 1_555 1_555 1_555 no S(11) C(14) H(10) 108.7(3) 1_555 1_555 1_555 no C(15) C(14) H(9) 108.2(3) 1_555 1_555 1_555 no C(15) C(14) H(10) 108.3(3) 1_555 1_555 1_555 no H(9) C(14) H(10) 109.5(3) 1_555 1_555 1_555 no S(12) C(15) C(14) 114.6(2) 1_555 1_555 1_555 yes S(12) C(15) H(11) 107.8(3) 1_555 1_555 1_555 no S(12) C(15) H(12) 108.7(3) 1_555 1_555 1_555 no C(14) C(15) H(11) 107.2(3) 1_555 1_555 1_555 no C(14) C(15) H(12) 108.2(3) 1_555 1_555 1_555 no H(11) C(15) H(12) 110.3(3) 1_555 1_555 1_555 no F(1) C(16) C(17) 116.6(3) 1_555 1_555 1_555 yes F(1) C(16) C(18) 118.9(3) 1_555 1_555 2_475 yes C(17) C(16) C(18) 124.5(3) 1_555 1_555 2_475 yes C(16) C(17) C(18) 116.5(3) 1_555 1_555 1_555 yes C(16) C(17) C(19) 120.0(3) 1_555 1_555 1_555 yes C(18) C(17) C(19) 123.4(3) 1_555 1_555 1_555 yes C(16) C(18) C(17) 118.9(3) 2_475 1_555 1_555 yes C(16) C(18) H(13) 121.1(3) 2_475 1_555 1_555 no C(17) C(18) H(13) 120.0(3) 1_555 1_555 1_555 no C(17) C(19) C(20) 176.6(4) 1_555 1_555 1_555 yes I(1) C(20) C(19) 175.8(3) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 I(1) Cl(1) 3.1343(2) 1_555 1_555 ? I(1) F(1) 3.368(2) 1_555 2_476 ? S(3) S(10) 3.530(2) 1_555 1_555 ? S(4) S(12) 3.437(2) 1_555 2_666 ? S(4) S(9) 3.535(1) 1_555 1_454 ? S(9) S(11) 3.551(2) 1_555 2_768 ? S(10) S(12) 3.561(1) 1_555 2_667 ? F(1) C(12) 3.327(4) 1_555 2_577 ? C(4) C(18) 3.408(5) 1_555 2_576 ? C(5) C(11) 3.494(5) 1_555 2_667 ? C(5) C(10) 3.546(5) 1_555 2_667 ? C(8) C(14) 3.520(5) 1_555 2_767 ? C(15) C(19) 3.524(4) 1_555 2_666 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_General _audit_creation_date 'Thu Oct 7 00:42:09 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Hiroshi M. Yamamoto' _publ_contact_author_address ; Hirosawa, Wako-shi, Saitama 351-0198 (Japan) ; _publ_contact_author_email ' yhiroshi@postman.riken.go.jp ' _publ_contact_author_fax ' +81-(0)48-462-4611 ' _publ_contact_author_phone ' +81-(0)48-467-9410 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' ' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # _publ_section_title ; Structural and physical properties of conducting cation radical satls containing supramolecular assmblies based on pBIB derivatives (pBIB=p-Bis(iodoethynyl)benzene) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_A_TEXRAY.INF_fET3Br.DFBIB #------------------------------------------------------------------------------ _audit_creation_date 'Sat Nov 7 04:36:46 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MXC Diffractometer Control' _computing_cell_refinement 'MXC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL93' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1647.80 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H26 Br F2 I2 S24 ' _chemical_formula_moiety 'C40 H26 Br F2 I2 S24 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.353(1) _cell_length_b 15.387(2) _cell_length_c 9.394(1) _cell_angle_alpha 98.466(7) _cell_angle_beta 107.504(8) _cell_angle_gamma 76.364(8) _cell_volume 1382.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 809.00 _exptl_absorpt_coefficient_mu 2.810 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Science rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'ImagingPlate' _diffrn_measurement_device 'MacScience DIP320' _diffrn_measurement_method _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l _diffrn_reflns_number 14601 _reflns_number_total 5988 _reflns_number_observed 3847 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.039 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 30.29 _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 40 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S 0 24 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H 0 26 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br 0 1 -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F 0 2 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I 0 2 -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags I(1) -0.86376(5) 0.00049(3) 0.36237(5) 0.0540(1) Uani d . 1.00 . Br(1) -1.0000 0.0000 0.0000 0.0519(3) Uani d . 0.50 S S(1) -0.6146(2) -0.5728(1) 0.8633(2) 0.0486(5) Uani d . 1.00 . S(2) -0.8683(2) -0.5815(1) 0.6181(2) 0.0484(5) Uani d . 1.00 . S(3) -0.7900(2) -0.4197(1) 1.0466(2) 0.0461(5) Uani d . 1.00 . S(4) -1.0434(2) -0.4290(1) 0.8011(2) 0.0485(5) Uani d . 1.00 . S(5) -0.4478(3) -0.7362(2) 0.7487(3) 0.0670(7) Uani d . 1.00 . S(6) -0.7505(2) -0.7463(1) 0.4623(2) 0.0633(7) Uani d . 1.00 . S(7) -0.9108(2) -0.2596(1) 1.2093(2) 0.0574(6) Uani d . 1.00 . S(8) -1.2145(2) -0.2704(1) 0.9223(3) 0.0611(7) Uani d . 1.00 . S(9) -0.2858(2) -0.5721(1) 0.5334(2) 0.0489(5) Uani d . 1.00 . S(10) -0.5391(2) -0.5860(1) 0.2918(2) 0.0491(5) Uani d . 1.00 . S(11) -0.1125(2) -0.7304(1) 0.4159(3) 0.0606(7) Uani d . 1.00 . S(12) -0.4149(2) -0.7481(1) 0.1339(2) 0.0596(6) Uani d . 1.00 . F(1) -0.4138(6) 0.0002(3) 0.7596(7) 0.074(2) Uani d . 1.00 . C(1) -0.7943(7) -0.5313(4) 0.7941(7) 0.039(2) Uani d . 1.00 . C(2) -0.8641(7) -0.4699(4) 0.8686(7) 0.036(2) Uani d . 1.00 . C(3) -0.6041(7) -0.6628(4) 0.7241(8) 0.042(2) Uani d . 1.00 . C(4) -0.7222(7) -0.6660(4) 0.6119(7) 0.039(2) Uani d . 1.00 . C(5) -0.9369(7) -0.3377(4) 1.0541(7) 0.039(2) Uani d . 1.00 . C(6) -1.0556(7) -0.3419(4) 0.9445(8) 0.041(2) Uani d . 1.00 . C(7) -0.462(1) -0.7778(7) 0.558(1) 0.070(3) Uani d . 1.00 . C(8) -0.581(1) -0.8199(6) 0.485(1) 0.070(3) Uani d . 1.00 . C(9) -1.0797(9) -0.1880(5) 1.1873(9) 0.051(2) Uani d . 1.00 . C(10) -1.1990(9) -0.2345(5) 1.1166(10) 0.052(2) Uani d . 1.00 . C(11) -0.4639(7) -0.5324(4) 0.4641(7) 0.037(2) Uani d . 1.00 . C(12) -0.2734(7) -0.6607(4) 0.3945(8) 0.040(2) Uani d . 1.00 . C(13) -0.3918(7) -0.6667(4) 0.2846(7) 0.038(2) Uani d . 1.00 . C(14) -0.126(1) -0.7654(6) 0.224(1) 0.064(3) Uani d . 1.00 . C(15) -0.240(1) -0.8108(6) 0.149(1) 0.069(3) Uani d . 1.00 . C(16) -0.7562(9) 0.0010(5) 0.5827(9) 0.054(2) Uani d . 1.00 . C(17) -0.6815(7) 0.0012(3) 0.6954(8) 0.038(2) Uani d . 1.00 . C(18) -0.5961(8) 0.0011(4) 0.8570(8) 0.046(2) Uani d . 1.00 . C(19) -0.6378(8) 0.0010(5) 0.9849(9) 0.050(2) Uani d . 1.00 . C(20) -0.4537(7) -0.0009(4) 0.8820(9) 0.047(2) Uani d . 1.00 . H(1) -0.4694 -0.7295 0.5017 0.0879 Uiso calc . 1.00 . H(2) -0.3806 -0.8214 0.5542 0.0879 Uiso calc . 1.00 . H(3) -0.5784 -0.8663 0.5463 0.0857 Uiso calc . 1.00 . H(4) -0.5756 -0.8468 0.3901 0.0857 Uiso calc . 1.00 . H(5) -1.0869 -0.1607 1.2841 0.0662 Uiso calc . 1.00 . H(6) -1.0879 -0.1402 1.1269 0.0662 Uiso calc . 1.00 . H(7) -1.2835 -0.1949 1.1237 0.0657 Uiso calc . 1.00 . H(8) -1.1859 -0.2858 1.1686 0.0657 Uiso calc . 1.00 . H(9) -0.1353 -0.7146 0.1720 0.0788 Uiso calc . 1.00 . H(10) -0.0399 -0.8060 0.2181 0.0788 Uiso calc . 1.00 . H(11) -0.2280 -0.8617 0.2045 0.0902 Uiso calc . 1.00 . H(12) -0.2342 -0.8323 0.0512 0.0902 Uiso calc . 1.00 . H(13) -0.7307 0.0004 0.9788 0.0524 Uiso calc . 1.00 . 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 I(1) 0.0531(3) 0.0581(2) 0.0395(2) -0.0116(2) -0.0034(2) 0.0027(2) Br(1) 0.0518(6) 0.0594(5) 0.0391(5) -0.0091(4) 0.0068(5) 0.0030(4) S(1) 0.0465(9) 0.0450(7) 0.0443(8) -0.0068(7) 0.0064(8) -0.0106(6) S(2) 0.0493(10) 0.0407(7) 0.0396(8) 0.0020(7) 0.0014(8) -0.0049(6) S(3) 0.0462(9) 0.0413(7) 0.0377(7) 0.0021(6) 0.0035(8) -0.0030(6) S(4) 0.0465(9) 0.0450(7) 0.0449(8) -0.0077(7) 0.0073(8) -0.0105(6) S(5) 0.052(1) 0.070(1) 0.057(1) 0.0038(9) 0.005(1) -0.0145(9) S(6) 0.059(1) 0.0572(9) 0.0537(10) -0.0054(8) 0.004(1) -0.0235(8) S(7) 0.051(1) 0.0547(9) 0.0484(9) -0.0011(8) 0.0048(9) -0.0168(7) S(8) 0.050(1) 0.067(1) 0.051(1) -0.0013(9) 0.0070(10) -0.0112(8) S(9) 0.0470(9) 0.0444(7) 0.0465(9) -0.0070(7) 0.0082(8) -0.0098(6) S(10) 0.0463(10) 0.0440(7) 0.0427(8) 0.0011(7) 0.0034(8) -0.0056(6) S(11) 0.051(1) 0.0620(10) 0.051(1) 0.0011(9) 0.0059(10) -0.0115(8) S(12) 0.054(1) 0.0546(9) 0.0533(10) -0.0039(8) 0.0069(10) -0.0191(8) F(1) 0.083(3) 0.083(3) 0.062(3) -0.029(2) 0.021(3) 0.000(2) C(1) 0.042(3) 0.036(2) 0.036(3) -0.005(2) 0.010(3) 0.002(2) C(2) 0.036(3) 0.036(2) 0.032(3) -0.003(2) 0.009(3) 0.003(2) C(3) 0.042(3) 0.041(3) 0.044(3) -0.015(2) 0.012(3) -0.003(2) C(4) 0.043(3) 0.035(2) 0.036(3) -0.008(2) 0.012(3) -0.006(2) C(5) 0.048(4) 0.039(3) 0.028(2) -0.008(2) 0.009(3) -0.002(2) C(6) 0.040(3) 0.042(3) 0.039(3) -0.013(2) 0.010(3) -0.005(2) C(7) 0.059(6) 0.088(6) 0.060(5) 0.001(5) 0.030(5) 0.001(4) C(8) 0.068(5) 0.060(4) 0.058(5) -0.004(4) -0.001(4) -0.015(4) C(9) 0.051(4) 0.046(3) 0.047(4) 0.002(3) 0.010(4) -0.001(3) C(10) 0.045(4) 0.055(4) 0.057(4) -0.004(3) 0.022(4) -0.003(3) C(11) 0.042(3) 0.031(2) 0.037(3) -0.004(2) 0.010(3) 0.001(2) C(12) 0.038(3) 0.037(2) 0.046(3) -0.007(2) 0.014(3) 0.001(2) C(13) 0.039(3) 0.040(3) 0.035(3) -0.003(2) 0.015(3) 0.000(2) C(14) 0.055(5) 0.079(5) 0.057(4) -0.005(4) 0.027(4) -0.004(4) C(15) 0.063(6) 0.075(5) 0.056(5) -0.008(4) 0.014(5) -0.022(4) C(16) 0.048(4) 0.053(3) 0.052(4) -0.010(3) 0.005(4) 0.000(3) C(17) 0.034(3) 0.024(2) 0.048(3) -0.006(2) -0.001(3) -0.003(2) C(18) 0.042(3) 0.049(3) 0.037(3) -0.010(2) -0.002(3) -0.001(2) C(19) 0.048(4) 0.045(3) 0.054(4) -0.003(3) 0.019(4) 0.000(3) C(20) 0.029(3) 0.041(3) 0.062(4) -0.007(2) 0.003(3) -0.005(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^) + (0.3116P)^2^+1.1329P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 0 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1649 _refine_ls_R_factor_obs 0.1413 _refine_ls_wR_factor_all 0.3765 _refine_ls_wR_factor_obs ? _refine_ls_goodness_of_fit_all 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_goodness_of_fit_obs ? _refine_ls_shift/esd_max 9.9440 _refine_ls_shift/esd_mean 0.4590 _refine_diff_density_min -1.88 _refine_diff_density_max 8.61 _refine_diff_density_rms 0.49 _atoms_sites_solution_primary 'direct methods' _atoms_sites_solution_secondary 'Fourier difference' #------------------------------------------------------------------------------ _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 I(1) C(16) 2.034(8) 1_555 1_555 yes S(1) C(1) 1.768(7) 1_555 1_555 yes S(1) C(3) 1.766(7) 1_555 1_555 yes S(2) C(1) 1.748(6) 1_555 1_555 yes S(2) C(4) 1.757(6) 1_555 1_555 yes S(3) C(2) 1.763(6) 1_555 1_555 yes S(3) C(5) 1.745(7) 1_555 1_555 yes S(4) C(2) 1.762(6) 1_555 1_555 yes S(4) C(6) 1.766(6) 1_555 1_555 yes S(5) C(3) 1.714(7) 1_555 1_555 yes S(5) C(7) 1.79(1) 1_555 1_555 yes S(6) C(4) 1.732(6) 1_555 1_555 yes S(6) C(8) 1.820(9) 1_555 1_555 yes S(7) C(5) 1.744(6) 1_555 1_555 yes S(7) C(9) 1.804(8) 1_555 1_555 yes S(8) C(6) 1.722(7) 1_555 1_555 yes S(8) C(10) 1.798(9) 1_555 1_555 yes S(9) C(11) 1.749(7) 1_555 1_555 yes S(9) C(12) 1.754(7) 1_555 1_555 yes S(10) C(11) 1.748(6) 1_555 1_555 yes S(10) C(13) 1.737(7) 1_555 1_555 yes S(11) C(12) 1.728(7) 1_555 1_555 yes S(11) C(14) 1.78(1) 1_555 1_555 yes S(12) C(13) 1.745(6) 1_555 1_555 yes S(12) C(15) 1.81(1) 1_555 1_555 yes F(1) C(20) 1.34(1) 1_555 1_555 yes C(1) C(2) 1.301(9) 1_555 1_555 yes C(3) C(4) 1.359(9) 1_555 1_555 yes C(5) C(6) 1.353(9) 1_555 1_555 yes C(7) C(8) 1.46(1) 1_555 1_555 yes C(9) C(10) 1.50(1) 1_555 1_555 yes C(11) C(11) 1.33(1) 1_555 2_446 yes C(12) C(13) 1.357(9) 1_555 1_555 yes C(14) C(15) 1.46(1) 1_555 1_555 yes C(16) C(17) 1.108(10) 1_555 1_555 yes C(17) C(18) 1.509(9) 1_555 1_555 yes C(18) C(19) 1.39(1) 1_555 1_555 yes C(18) C(20) 1.41(1) 1_555 1_555 yes C(19) C(20) 1.32(1) 1_555 2_457 yes #------------------------------------------------------------------------------ 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(3) 96.1(3) 1_555 1_555 1_555 yes C(1) S(2) C(4) 95.9(3) 1_555 1_555 1_555 yes C(2) S(3) C(5) 95.7(3) 1_555 1_555 1_555 yes C(2) S(4) C(6) 96.4(3) 1_555 1_555 1_555 yes C(3) S(5) C(7) 98.8(4) 1_555 1_555 1_555 yes C(4) S(6) C(8) 103.1(4) 1_555 1_555 1_555 yes C(5) S(7) C(9) 103.0(3) 1_555 1_555 1_555 yes C(6) S(8) C(10) 97.9(3) 1_555 1_555 1_555 yes C(11) S(9) C(12) 96.0(3) 1_555 1_555 1_555 yes C(11) S(10) C(13) 95.7(3) 1_555 1_555 1_555 yes C(12) S(11) C(14) 98.5(4) 1_555 1_555 1_555 yes C(13) S(12) C(15) 102.7(4) 1_555 1_555 1_555 yes S(1) C(1) S(2) 113.6(4) 1_555 1_555 1_555 yes S(1) C(1) C(2) 122.7(5) 1_555 1_555 1_555 yes S(2) C(1) C(2) 123.7(5) 1_555 1_555 1_555 yes S(3) C(2) S(4) 113.2(3) 1_555 1_555 1_555 yes S(3) C(2) C(1) 123.8(5) 1_555 1_555 1_555 yes S(4) C(2) C(1) 123.0(5) 1_555 1_555 1_555 yes S(1) C(3) S(5) 116.3(4) 1_555 1_555 1_555 yes S(1) C(3) C(4) 115.7(5) 1_555 1_555 1_555 yes S(5) C(3) C(4) 128.0(5) 1_555 1_555 1_555 yes S(2) C(4) S(6) 114.3(4) 1_555 1_555 1_555 yes S(2) C(4) C(3) 117.7(5) 1_555 1_555 1_555 yes S(6) C(4) C(3) 128.0(5) 1_555 1_555 1_555 yes S(3) C(5) S(7) 114.0(4) 1_555 1_555 1_555 yes S(3) C(5) C(6) 118.3(5) 1_555 1_555 1_555 yes S(7) C(5) C(6) 127.7(5) 1_555 1_555 1_555 yes S(4) C(6) S(8) 115.9(3) 1_555 1_555 1_555 yes S(4) C(6) C(5) 115.5(5) 1_555 1_555 1_555 yes S(8) C(6) C(5) 128.5(5) 1_555 1_555 1_555 yes S(5) C(7) C(8) 115.0(9) 1_555 1_555 1_555 yes S(5) C(7) H(1) 108.9(7) 1_555 1_555 1_555 no S(5) C(7) H(2) 108.3(7) 1_555 1_555 1_555 no C(8) C(7) H(1) 107.6(8) 1_555 1_555 1_555 no C(8) C(7) H(2) 107.8(9) 1_555 1_555 1_555 no H(1) C(7) H(2) 109(1) 1_555 1_555 1_555 no S(6) C(8) C(7) 115.9(6) 1_555 1_555 1_555 yes S(6) C(8) H(3) 106.1(9) 1_555 1_555 1_555 no S(6) C(8) H(4) 107.8(6) 1_555 1_555 1_555 no C(7) C(8) H(3) 107.9(8) 1_555 1_555 1_555 no C(7) C(8) H(4) 110(1) 1_555 1_555 1_555 no H(3) C(8) H(4) 108.5(8) 1_555 1_555 1_555 no S(7) C(9) C(10) 114.9(5) 1_555 1_555 1_555 yes S(7) C(9) H(5) 108.6(5) 1_555 1_555 1_555 no S(7) C(9) H(6) 108.8(8) 1_555 1_555 1_555 no C(10) C(9) H(5) 108.7(9) 1_555 1_555 1_555 no C(10) C(9) H(6) 108.5(7) 1_555 1_555 1_555 no H(5) C(9) H(6) 107.2(7) 1_555 1_555 1_555 no S(8) C(10) C(9) 112.6(7) 1_555 1_555 1_555 yes S(8) C(10) H(7) 108.1(6) 1_555 1_555 1_555 no S(8) C(10) H(8) 108.4(6) 1_555 1_555 1_555 no C(9) C(10) H(7) 109.8(7) 1_555 1_555 1_555 no C(9) C(10) H(8) 108.9(7) 1_555 1_555 1_555 no H(7) C(10) H(8) 108(1) 1_555 1_555 1_555 no S(9) C(11) S(10) 114.1(3) 1_555 1_555 1_555 yes S(9) C(11) C(11) 123.2(6) 1_555 1_555 2_446 yes S(10) C(11) C(11) 122.8(7) 1_555 1_555 2_446 yes S(9) C(12) S(11) 116.0(4) 1_555 1_555 1_555 yes S(9) C(12) C(13) 115.9(5) 1_555 1_555 1_555 yes S(11) C(12) C(13) 128.1(5) 1_555 1_555 1_555 yes S(10) C(13) S(12) 115.0(4) 1_555 1_555 1_555 yes S(10) C(13) C(12) 117.9(5) 1_555 1_555 1_555 yes S(12) C(13) C(12) 127.2(5) 1_555 1_555 1_555 yes S(11) C(14) C(15) 114.0(9) 1_555 1_555 1_555 yes S(11) C(14) H(9) 109.0(7) 1_555 1_555 1_555 no S(11) C(14) H(10) 107.8(7) 1_555 1_555 1_555 no C(15) C(14) H(9) 109.1(8) 1_555 1_555 1_555 no C(15) C(14) H(10) 108.8(8) 1_555 1_555 1_555 no H(9) C(14) H(10) 107(1) 1_555 1_555 1_555 no S(12) C(15) C(14) 118.3(6) 1_555 1_555 1_555 yes S(12) C(15) H(11) 106.6(9) 1_555 1_555 1_555 no S(12) C(15) H(12) 107.5(7) 1_555 1_555 1_555 no C(14) C(15) H(11) 107.3(8) 1_555 1_555 1_555 no C(14) C(15) H(12) 108(1) 1_555 1_555 1_555 no H(11) C(15) H(12) 108.2(8) 1_555 1_555 1_555 no I(1) C(16) C(17) 169.8(9) 1_555 1_555 1_555 yes C(16) C(17) C(18) 172.2(9) 1_555 1_555 1_555 yes C(17) C(18) C(19) 128.9(7) 1_555 1_555 1_555 yes C(17) C(18) C(20) 115.7(7) 1_555 1_555 1_555 yes C(19) C(18) C(20) 115.5(6) 1_555 1_555 1_555 yes C(18) C(19) C(20) 119.7(8) 1_555 1_555 2_457 yes C(18) C(19) H(13) 121.5(7) 1_555 1_555 1_555 no C(20) C(19) H(13) 118.8(9) 2_457 1_555 1_555 no F(1) C(20) C(18) 115.6(6) 1_555 1_555 1_555 yes F(1) C(20) C(19) 119.6(8) 1_555 1_555 2_457 yes C(18) C(20) C(19) 124.8(9) 1_555 1_555 2_457 yes #------------------------------------------------------------------------------ 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 I(1) F(1) 3.395(7) 1_555 2_456 ? S(5) S(12) 3.559(4) 1_555 1_556 ? S(6) S(8) 3.562(3) 1_555 2_346 ? S(6) S(11) 3.593(4) 1_555 1_455 ? S(7) S(11) 3.480(3) 1_555 2_447 ? C(3) C(10) 3.60(1) 1_555 2_347 ? C(4) C(10) 3.54(1) 1_555 2_347 ? C(9) C(17) 3.598(10) 1_555 2_357 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_General _audit_creation_date 'Tue Mar 14 02:27:23 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_ET3Cl.pBIBd4 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C40 H28 Cl I2 S24 ' _chemical_formula_moiety '?' _chemical_formula_weight 1571.36 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.198(1) _cell_length_b 15.559(2) _cell_length_c 9.296(1) _cell_angle_alpha 99.634(6) _cell_angle_beta 106.931(7) _cell_angle_gamma 76.581(7) _cell_volume 1364.6(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.060 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.153 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 5907 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 30.25 _diffrn_measured_fraction_theta_max 0.7263 _diffrn_reflns_theta_full 30.25 _diffrn_measured_fraction_theta_full 0.7263 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5907 _reflns_number_gt 3432 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.0753 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3432 _refine_ls_number_parameters 312 _refine_ls_goodness_of_fit_ref 3.830 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_shift/su_max 12.0060 _refine_diff_density_max 6.71 _refine_diff_density_min -0.90 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _atoms_sites_solution_primary 'direct methods' _atoms_sites_solution_secondary 'Fourier difference' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I -0.15400(6) 1.00131(4) 0.65306(7) 0.0596(2) Uani 1.00 d . . . Cl(1) Cl 0.0000 1.0000 1.0000 0.0372(6) Uani 1.00 d S . . S(1) S 0.5428(2) 0.5853(1) 0.7137(2) 0.0485(5) Uani 1.00 d . . . S(2) S 0.2843(2) 0.5722(1) 0.4727(2) 0.0502(6) Uani 1.00 d . . . S(3) S 0.4208(2) 0.7478(1) 0.8798(2) 0.0586(6) Uani 1.00 d . . . S(4) S 0.1129(2) 0.7310(2) 0.5978(3) 0.0649(6) Uani 1.00 d . . . S(5) S 0.8737(2) 0.5845(1) 0.3845(2) 0.0486(5) Uani 1.00 d . . . S(6) S 0.6177(2) 0.5748(1) 0.1383(2) 0.0496(5) Uani 1.00 d . . . S(7) S 1.0475(2) 0.4266(1) 0.1988(2) 0.0490(5) Uani 1.00 d . . . S(8) S 0.7925(2) 0.4193(1) -0.0486(2) 0.0473(5) Uani 1.00 d . . . S(9) S 0.7545(2) 0.7483(2) 0.5478(3) 0.0611(6) Uani 1.00 d . . . S(10) S 0.4490(2) 0.7365(2) 0.2617(3) 0.0660(7) Uani 1.00 d . . . S(11) S 1.2165(2) 0.2666(2) 0.0724(2) 0.0624(6) Uani 1.00 d . . . S(12) S 0.9110(2) 0.2590(1) -0.2193(2) 0.0580(6) Uani 1.00 d . . . C(1) C 0.4635(7) 0.5327(4) 0.5393(8) 0.041(2) Uani 1.00 d . . . C(2) C 0.3944(7) 0.6670(4) 0.7248(8) 0.040(2) Uani 1.00 d . . . C(3) C 0.2771(7) 0.6607(5) 0.6157(8) 0.043(2) Uani 1.00 d . . . C(4A) C 0.243(1) 0.8096(8) 0.871(2) 0.077(4) Uani 0.80 d P . . C(4B) C 0.254(5) 0.777(4) 0.905(6) 0.0769 Uani 0.20 d P . . C(5A) C 0.128(1) 0.7762(8) 0.785(1) 0.070(4) Uani 0.80 d P . . C(5B) C 0.158(4) 0.825(3) 0.751(5) 0.0700 Uani 0.20 d P . . C(6) C 0.7970(7) 0.5335(4) 0.2072(8) 0.040(2) Uani 1.00 d . . . C(7) C 0.8707(7) 0.4691(4) 0.1294(8) 0.040(2) Uani 1.00 d . . . C(8) C 0.7272(7) 0.6679(4) 0.3935(7) 0.036(2) Uani 1.00 d . . . C(9) C 0.6099(7) 0.6624(5) 0.2808(8) 0.044(2) Uani 1.00 d . . . C(10) C 1.0558(7) 0.3401(5) 0.0535(8) 0.042(2) Uani 1.00 d . . . C(11) C 0.9384(7) 0.3359(4) -0.0594(7) 0.037(2) Uani 1.00 d . . . C(12) C 0.5822(8) 0.8167(6) 0.535(1) 0.067(3) Uani 1.00 d . . . C(13) C 0.4626(9) 0.7744(6) 0.456(1) 0.072(3) Uani 1.00 d . . . C(14) C 1.2026(8) 0.2276(5) -0.1230(9) 0.053(2) Uani 1.00 d . . . C(15) C 1.0782(8) 0.1843(5) -0.1972(9) 0.058(2) Uani 1.00 d . . . C(16) C -0.5564(8) 1.0025(5) 0.107(1) 0.072(3) Uani 1.00 d . . . C(17) C -0.4212(8) 1.0009(5) 0.1451(10) 0.060(2) Uani 1.00 d . . . C(18) C -0.3614(9) 0.9963(5) 0.0304(10) 0.062(3) Uani 1.00 d . . . C(19) C -0.3357(8) 0.9998(5) 0.3052(9) 0.050(2) Uani 1.00 d . . . C(20) C -0.2654(9) 1.0001(6) 0.426(1) 0.064(3) Uani 1.00 d . . . H(1A) H 0.2347 0.8202 0.9718 0.0849 Uiso 0.80 calc P . . H(1B) H 0.2213 0.7264 0.9134 0.0306 Uiso 0.20 calc P . . H(2A) H 0.2360 0.8645 0.8348 0.0849 Uiso 0.80 calc P . . H(2B) H 0.2522 0.8181 0.9935 0.0306 Uiso 0.20 calc P . . H(3A) H 0.0499 0.8236 0.7840 0.0849 Uiso 0.80 calc P . . H(3B) H 0.2100 0.8590 0.7216 0.0306 Uiso 0.20 calc P . . H(4A) H 0.1210 0.7307 0.8375 0.0849 Uiso 0.80 calc P . . H(4B) H 0.0754 0.8620 0.7696 0.0306 Uiso 0.20 calc P . . H(5) H 0.5760 0.8390 0.6355 0.0984 Uiso 1.00 calc . . . H(6) H 0.5761 0.8668 0.4829 0.0984 Uiso 1.00 calc . . . H(7) H 0.3766 0.8142 0.4618 0.0840 Uiso 1.00 calc . . . H(8) H 0.4681 0.7230 0.5054 0.0840 Uiso 1.00 calc . . . H(9) H 1.1969 0.2767 -0.1753 0.0828 Uiso 1.00 calc . . . H(10) H 1.2873 0.1856 -0.1299 0.0828 Uiso 1.00 calc . . . H(11) H 1.0797 0.1388 -0.1379 0.0708 Uiso 1.00 calc . . . H(12) H 1.0849 0.1560 -0.2956 0.0708 Uiso 1.00 calc . . . H(13) H -0.6202 1.0207 0.1976 0.0832 Uiso 1.00 calc . . . H(14) H -0.2570 1.0110 0.0391 0.0832 Uiso 1.00 calc . . . 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 I(1) 0.0569(3) 0.0584(3) 0.0561(3) -0.0113(3) 0.0041(2) 0.0036(3) Cl(1) 0.030(1) 0.052(1) 0.032(1) -0.009(1) 0.0105(9) 0.004(1) S(1) 0.043(1) 0.042(1) 0.045(1) 0.0072(9) 0.0037(9) -0.0053(9) S(2) 0.041(1) 0.044(1) 0.053(1) -0.0020(9) 0.0076(9) -0.0110(10) S(3) 0.043(1) 0.062(1) 0.056(1) -0.002(1) 0.0119(9) -0.023(1) S(4) 0.038(1) 0.075(2) 0.060(1) 0.006(1) 0.0078(9) -0.020(1) S(5) 0.046(1) 0.041(1) 0.042(1) 0.0079(9) 0.0029(8) -0.0061(9) S(6) 0.042(1) 0.045(1) 0.049(1) -0.0027(9) 0.0072(9) -0.0134(9) S(7) 0.042(1) 0.045(1) 0.047(1) -0.0016(9) 0.0060(9) -0.0122(9) S(8) 0.046(1) 0.041(1) 0.039(1) 0.0076(9) 0.0042(8) -0.0049(9) S(9) 0.044(1) 0.063(1) 0.057(1) 0.000(1) 0.0073(9) -0.025(1) S(10) 0.038(1) 0.083(2) 0.054(1) 0.010(1) 0.0070(9) -0.019(1) S(11) 0.038(1) 0.075(2) 0.054(1) 0.007(1) 0.0062(9) -0.016(1) S(12) 0.043(1) 0.060(1) 0.050(1) 0.004(1) 0.0056(9) -0.020(1) C(1) 0.043(4) 0.030(4) 0.043(4) -0.002(3) 0.009(3) -0.002(3) C(2) 0.044(4) 0.035(4) 0.039(4) -0.005(3) 0.016(3) 0.000(3) C(3) 0.041(4) 0.038(4) 0.047(4) -0.001(3) 0.013(3) -0.004(3) C(4A) 0.053(5) 0.072(9) 0.083(8) 0.002(6) 0.019(5) -0.039(6) C(4B) 0.0529 0.0715 0.0834 0.0023 0.0191 -0.0386 C(5A) 0.044(6) 0.096(10) 0.055(7) 0.005(6) 0.018(5) -0.018(6) C(5B) 0.0437 0.0960 0.0552 0.0049 0.0178 -0.0178 C(6) 0.045(4) 0.030(4) 0.039(4) -0.001(3) 0.010(3) -0.001(3) C(7) 0.046(4) 0.031(4) 0.041(4) -0.003(3) 0.012(3) 0.002(3) C(8) 0.038(4) 0.037(4) 0.039(4) -0.007(3) 0.019(3) -0.001(3) C(9) 0.043(4) 0.041(4) 0.043(4) -0.002(3) 0.015(3) -0.006(3) C(10) 0.041(4) 0.039(4) 0.043(4) -0.007(3) 0.014(3) -0.007(3) C(11) 0.037(4) 0.035(4) 0.037(4) -0.001(3) 0.014(3) -0.001(3) C(12) 0.050(5) 0.060(5) 0.071(6) 0.002(4) 0.014(4) -0.027(5) C(13) 0.055(5) 0.086(7) 0.064(5) 0.007(5) 0.022(4) -0.004(5) C(14) 0.050(4) 0.051(5) 0.058(5) -0.001(4) 0.023(4) -0.005(4) C(15) 0.052(5) 0.053(5) 0.057(5) 0.002(4) 0.015(4) -0.012(4) C(16) 0.048(5) 0.026(4) 0.100(6) 0.004(4) -0.035(4) -0.001(4) C(17) 0.051(4) 0.029(4) 0.101(6) 0.004(4) 0.041(4) -0.008(4) C(18) 0.085(6) 0.040(5) 0.061(5) -0.006(4) 0.023(4) 0.002(4) C(19) 0.045(4) 0.037(4) 0.052(5) 0.001(4) 0.001(4) -0.004(4) C(20) 0.060(5) 0.062(6) 0.076(6) -0.008(4) 0.029(4) 0.004(5) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 I(1) C(20) 2.087(9) . . yes S(1) C(1) 1.746(7) . . yes S(1) C(2) 1.752(7) . . yes S(2) C(1) 1.746(7) . . yes S(2) C(3) 1.751(7) . . yes S(3) C(2) 1.748(7) . . yes S(3) C(4A) 1.83(1) . . yes S(3) C(4B) 1.73(5) . . yes S(4) C(3) 1.754(7) . . yes S(4) C(5A) 1.74(1) . . yes S(4) C(5B) 1.90(5) . . yes S(5) C(6) 1.748(7) . . yes S(5) C(8) 1.749(7) . . yes S(6) C(6) 1.754(7) . . yes S(6) C(9) 1.739(7) . . yes S(7) C(7) 1.736(7) . . yes S(7) C(10) 1.745(7) . . yes S(8) C(7) 1.750(7) . . yes S(8) C(11) 1.748(7) . . yes S(9) C(8) 1.740(7) . . yes S(9) C(12) 1.812(8) . . yes S(10) C(9) 1.753(7) . . yes S(10) C(13) 1.779(9) . . yes S(11) C(10) 1.748(7) . . yes S(11) C(14) 1.792(8) . . yes S(12) C(11) 1.743(7) . . yes S(12) C(15) 1.804(8) . . yes C(1) C(1) 1.36(1) . 2_666 yes C(2) C(3) 1.336(9) . . yes C(4A) C(4B) 0.61(6) . . yes C(4A) C(5A) 1.37(2) . . yes C(4A) C(5B) 1.21(4) . . yes C(4B) C(5A) 1.44(5) . . yes C(4B) C(5B) 1.66(7) . . yes C(5A) C(5B) 1.01(5) . . yes C(6) C(7) 1.348(9) . . yes C(8) C(9) 1.350(9) . . yes C(10) C(11) 1.350(9) . . yes C(12) C(13) 1.47(1) . . yes C(14) C(15) 1.51(1) . . yes C(16) C(17) 1.32(1) . . yes C(16) C(18) 1.31(1) . 2_475 yes C(17) C(18) 1.36(1) . . yes C(17) C(19) 1.49(1) . . yes C(19) C(20) 1.14(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S(1) C(2) 95.0(3) 1_555 1_555 1_555 yes C(1) S(2) C(3) 94.9(3) 1_555 1_555 1_555 yes C(2) S(3) C(4A) 102.3(5) 1_555 1_555 1_555 yes C(2) S(3) C(4B) 100(1) 1_555 1_555 1_555 yes C(4A) S(3) C(4B) 19(2) 1_555 1_555 1_555 yes C(3) S(4) C(5A) 100.3(4) 1_555 1_555 1_555 yes C(3) S(4) C(5B) 100(1) 1_555 1_555 1_555 yes C(5A) S(4) C(5B) 31(1) 1_555 1_555 1_555 yes C(6) S(5) C(8) 95.4(3) 1_555 1_555 1_555 yes C(6) S(6) C(9) 95.2(3) 1_555 1_555 1_555 yes C(7) S(7) C(10) 95.4(3) 1_555 1_555 1_555 yes C(7) S(8) C(11) 95.2(3) 1_555 1_555 1_555 yes C(8) S(9) C(12) 103.6(4) 1_555 1_555 1_555 yes C(9) S(10) C(13) 98.9(4) 1_555 1_555 1_555 yes C(10) S(11) C(14) 99.1(3) 1_555 1_555 1_555 yes C(11) S(12) C(15) 103.2(3) 1_555 1_555 1_555 yes S(1) C(1) S(2) 114.9(4) 1_555 1_555 1_555 yes S(1) C(1) C(1) 122.4(7) 1_555 1_555 2_666 yes S(2) C(1) C(1) 122.7(7) 1_555 1_555 2_666 yes S(1) C(2) S(3) 114.7(4) 1_555 1_555 1_555 yes S(1) C(2) C(3) 117.2(5) 1_555 1_555 1_555 yes S(3) C(2) C(3) 128.2(5) 1_555 1_555 1_555 yes S(2) C(3) S(4) 114.9(4) 1_555 1_555 1_555 yes S(2) C(3) C(2) 117.5(5) 1_555 1_555 1_555 yes S(4) C(3) C(2) 127.6(6) 1_555 1_555 1_555 yes S(3) C(4A) C(4B) 71(5) 1_555 1_555 1_555 yes S(3) C(4A) C(5A) 121.8(9) 1_555 1_555 1_555 yes S(3) C(4A) C(5B) 121(2) 1_555 1_555 1_555 yes S(3) C(4A) H(1A) 106.7(10) 1_555 1_555 1_555 no S(3) C(4A) H(2A) 102.2(10) 1_555 1_555 1_555 no S(3) C(4A) H(2B) 100.4(8) 1_555 1_555 1_555 no C(4B) C(4A) C(5A) 83(5) 1_555 1_555 1_555 yes C(4B) C(4A) C(5B) 127(6) 1_555 1_555 1_555 yes C(4B) C(4A) H(1A) 70(5) 1_555 1_555 1_555 no C(4B) C(4A) H(2A) 172(5) 1_555 1_555 1_555 no C(4B) C(4A) H(2B) 64(5) 1_555 1_555 1_555 no C(5A) C(4A) C(5B) 45(2) 1_555 1_555 1_555 yes C(5A) C(4A) H(1A) 112(1) 1_555 1_555 1_555 no C(5A) C(4A) H(2A) 103(1) 1_555 1_555 1_555 no C(5A) C(4A) H(2B) 114(1) 1_555 1_555 1_555 no C(5B) C(4A) H(1A) 131(2) 1_555 1_555 1_555 no C(5B) C(4A) H(2A) 58(2) 1_555 1_555 1_555 no C(5B) C(4A) H(2B) 137(2) 1_555 1_555 1_555 no H(1A) C(4A) H(2A) 108(1) 1_555 1_555 1_555 no H(1A) C(4A) H(2B) 7.1(2) 1_555 1_555 1_555 no H(2A) C(4A) H(2B) 113(1) 1_555 1_555 1_555 no S(3) C(4B) C(4A) 89(6) 1_555 1_555 1_555 yes S(3) C(4B) C(5A) 124(3) 1_555 1_555 1_555 yes S(3) C(4B) C(5B) 104(3) 1_555 1_555 1_555 yes S(3) C(4B) H(1A) 114(4) 1_555 1_555 1_555 no S(3) C(4B) H(1B) 118(3) 1_555 1_555 1_555 no S(3) C(4B) H(2B) 111(3) 1_555 1_555 1_555 no C(4A) C(4B) C(5A) 71(5) 1_555 1_555 1_555 yes C(4A) C(4B) C(5B) 35(4) 1_555 1_555 1_555 yes C(4A) C(4B) H(1A) 70(5) 1_555 1_555 1_555 no C(4A) C(4B) H(1B) 148(7) 1_555 1_555 1_555 no C(4A) C(4B) H(2B) 84(5) 1_555 1_555 1_555 no C(5A) C(4B) C(5B) 36(2) 1_555 1_555 1_555 yes C(5A) C(4B) H(1A) 107(4) 1_555 1_555 1_555 no C(5A) C(4B) H(1B) 80(3) 1_555 1_555 1_555 no C(5A) C(4B) H(2B) 117(3) 1_555 1_555 1_555 no C(5B) C(4B) H(1A) 93(4) 1_555 1_555 1_555 no C(5B) C(4B) H(1B) 117(4) 1_555 1_555 1_555 no C(5B) C(4B) H(2B) 108(4) 1_555 1_555 1_555 no H(1A) C(4B) H(1B) 106(5) 1_555 1_555 1_555 no H(1A) C(4B) H(2B) 15(1) 1_555 1_555 1_555 no H(1B) C(4B) H(2B) 96(5) 1_555 1_555 1_555 no S(4) C(5A) C(4A) 122.0(10) 1_555 1_555 1_555 yes S(4) C(5A) C(4B) 127(2) 1_555 1_555 1_555 yes S(4) C(5A) C(5B) 82(2) 1_555 1_555 1_555 yes S(4) C(5A) H(3A) 108.1(8) 1_555 1_555 1_555 no S(4) C(5A) H(4A) 104.8(9) 1_555 1_555 1_555 no S(4) C(5A) H(4B) 104.2(8) 1_555 1_555 1_555 no C(4A) C(5A) C(4B) 25(2) 1_555 1_555 1_555 yes C(4A) C(5A) C(5B) 59(2) 1_555 1_555 1_555 yes C(4A) C(5A) H(3A) 110(1) 1_555 1_555 1_555 no C(4A) C(5A) H(4A) 105(1) 1_555 1_555 1_555 no C(4A) C(5A) H(4B) 86.5(10) 1_555 1_555 1_555 no C(4B) C(5A) C(5B) 83(3) 1_555 1_555 1_555 yes C(4B) C(5A) H(3A) 121(2) 1_555 1_555 1_555 no C(4B) C(5A) H(4A) 80(2) 1_555 1_555 1_555 no C(4B) C(5A) H(4B) 106(2) 1_555 1_555 1_555 no C(5B) C(5A) H(3A) 86(2) 1_555 1_555 1_555 no C(5B) C(5A) H(4A) 164(2) 1_555 1_555 1_555 no C(5B) C(5A) H(4B) 52(2) 1_555 1_555 1_555 no H(3A) C(5A) H(4A) 103(1) 1_555 1_555 1_555 no H(3A) C(5A) H(4B) 34.3(4) 1_555 1_555 1_555 no H(4A) C(5A) H(4B) 135(1) 1_555 1_555 1_555 no S(4) C(5B) C(4A) 120(3) 1_555 1_555 1_555 yes S(4) C(5B) C(4B) 106(3) 1_555 1_555 1_555 yes S(4) C(5B) C(5A) 65(2) 1_555 1_555 1_555 yes S(4) C(5B) H(2A) 147(3) 1_555 1_555 1_555 no S(4) C(5B) H(3B) 116(3) 1_555 1_555 1_555 no S(4) C(5B) H(4B) 104(3) 1_555 1_555 1_555 no C(4A) C(5B) C(4B) 16(2) 1_555 1_555 1_555 yes C(4A) C(5B) C(5A) 75(3) 1_555 1_555 1_555 yes C(4A) C(5B) H(2A) 50(2) 1_555 1_555 1_555 no C(4A) C(5B) H(3B) 93(3) 1_555 1_555 1_555 no C(4A) C(5B) H(4B) 106(3) 1_555 1_555 1_555 no C(4B) C(5B) C(5A) 59(3) 1_555 1_555 1_555 yes C(4B) C(5B) H(2A) 67(2) 1_555 1_555 1_555 no C(4B) C(5B) H(3B) 108(4) 1_555 1_555 1_555 no C(4B) C(5B) H(4B) 104(4) 1_555 1_555 1_555 no C(5A) C(5B) H(2A) 125(4) 1_555 1_555 1_555 no C(5A) C(5B) H(3B) 166(5) 1_555 1_555 1_555 no C(5A) C(5B) H(4B) 75(3) 1_555 1_555 1_555 no H(2A) C(5B) H(3B) 45(2) 1_555 1_555 1_555 no H(2A) C(5B) H(4B) 107(4) 1_555 1_555 1_555 no H(3B) C(5B) H(4B) 114(5) 1_555 1_555 1_555 no S(5) C(6) S(6) 114.3(4) 1_555 1_555 1_555 yes S(5) C(6) C(7) 122.5(5) 1_555 1_555 1_555 yes S(6) C(6) C(7) 123.1(5) 1_555 1_555 1_555 yes S(7) C(7) S(8) 114.8(4) 1_555 1_555 1_555 yes S(7) C(7) C(6) 123.2(6) 1_555 1_555 1_555 yes S(8) C(7) C(6) 121.9(5) 1_555 1_555 1_555 yes S(5) C(8) S(9) 114.6(4) 1_555 1_555 1_555 yes S(5) C(8) C(9) 116.7(5) 1_555 1_555 1_555 yes S(9) C(8) C(9) 128.8(5) 1_555 1_555 1_555 yes S(6) C(9) S(10) 116.1(4) 1_555 1_555 1_555 yes S(6) C(9) C(8) 117.7(5) 1_555 1_555 1_555 yes S(10) C(9) C(8) 126.3(6) 1_555 1_555 1_555 yes S(7) C(10) S(11) 115.8(4) 1_555 1_555 1_555 yes S(7) C(10) C(11) 117.4(5) 1_555 1_555 1_555 yes S(11) C(10) C(11) 126.8(5) 1_555 1_555 1_555 yes S(8) C(11) S(12) 114.2(4) 1_555 1_555 1_555 yes S(8) C(11) C(10) 116.7(5) 1_555 1_555 1_555 yes S(12) C(11) C(10) 129.0(5) 1_555 1_555 1_555 yes S(9) C(12) C(13) 116.8(6) 1_555 1_555 1_555 yes S(9) C(12) H(5) 107.8(6) 1_555 1_555 1_555 no S(9) C(12) H(6) 107.1(7) 1_555 1_555 1_555 no C(13) C(12) H(5) 109.2(8) 1_555 1_555 1_555 no C(13) C(12) H(6) 107.9(8) 1_555 1_555 1_555 no H(5) C(12) H(6) 107.7(8) 1_555 1_555 1_555 no S(10) C(13) C(12) 115.7(7) 1_555 1_555 1_555 yes S(10) C(13) H(7) 107.4(7) 1_555 1_555 1_555 no S(10) C(13) H(8) 106.7(7) 1_555 1_555 1_555 no C(12) C(13) H(7) 110.6(9) 1_555 1_555 1_555 no C(12) C(13) H(8) 109.1(8) 1_555 1_555 1_555 no H(7) C(13) H(8) 107.0(9) 1_555 1_555 1_555 no S(11) C(14) C(15) 113.3(6) 1_555 1_555 1_555 yes S(11) C(14) H(9) 108.5(6) 1_555 1_555 1_555 no S(11) C(14) H(10) 108.1(6) 1_555 1_555 1_555 no C(15) C(14) H(9) 109.5(7) 1_555 1_555 1_555 no C(15) C(14) H(10) 109.6(7) 1_555 1_555 1_555 no H(9) C(14) H(10) 107.7(8) 1_555 1_555 1_555 no S(12) C(15) C(14) 114.8(6) 1_555 1_555 1_555 yes S(12) C(15) H(11) 107.9(6) 1_555 1_555 1_555 no S(12) C(15) H(12) 108.0(6) 1_555 1_555 1_555 no C(14) C(15) H(11) 108.9(7) 1_555 1_555 1_555 no C(14) C(15) H(12) 109.4(8) 1_555 1_555 1_555 no H(11) C(15) H(12) 107.5(8) 1_555 1_555 1_555 no C(17) C(16) C(18) 125.6(10) 1_555 1_555 2_475 yes C(17) C(16) H(13) 121.3(8) 1_555 1_555 1_555 no C(18) C(16) H(13) 111.5(7) 2_475 1_555 1_555 no C(16) C(17) C(18) 116.8(9) 1_555 1_555 1_555 yes C(16) C(17) C(19) 121.9(8) 1_555 1_555 1_555 yes C(18) C(17) C(19) 121.2(7) 1_555 1_555 1_555 yes C(16) C(18) C(17) 117.5(9) 2_475 1_555 1_555 yes C(16) C(18) H(14) 112.8(9) 2_475 1_555 1_555 no C(17) C(18) H(14) 127.3(8) 1_555 1_555 1_555 no C(17) C(19) C(20) 176.8(10) 1_555 1_555 1_555 yes I(1) C(20) C(19) 174.5(8) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I(1) C(20) C(19) C(17) 162(9) 1_555 1_555 1_555 1_555 yes S(1) C(1) S(2) C(3) 7.0(5) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(1) S(1) 180.0 1_555 1_555 2_666 2_666 yes S(1) C(1) C(1) S(2) 1(1) 1_555 1_555 2_666 2_666 yes S(1) C(2) S(3) C(4A) -171.6(6) 1_555 1_555 1_555 1_555 yes S(1) C(2) S(3) C(4B) -151(2) 1_555 1_555 1_555 1_555 yes S(1) C(2) C(3) S(2) -0.5(9) 1_555 1_555 1_555 1_555 yes S(1) C(2) C(3) S(4) 179.0(5) 1_555 1_555 1_555 1_555 yes S(2) C(1) S(1) C(2) -7.2(5) 1_555 1_555 1_555 1_555 yes S(2) C(1) C(1) S(2) 180.0 1_555 1_555 2_666 2_666 yes S(2) C(3) S(4) C(5A) 156.7(6) 1_555 1_555 1_555 1_555 yes S(2) C(3) S(4) C(5B) -171(1) 1_555 1_555 1_555 1_555 yes S(2) C(3) C(2) S(3) 179.1(4) 1_555 1_555 1_555 1_555 yes S(3) C(2) S(1) C(1) -175.0(4) 1_555 1_555 1_555 1_555 yes S(3) C(2) C(3) S(4) -1(1) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(4B) C(5A) -126(1) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(4B) C(5B) -115(5) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(5A) S(4) -48(1) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(5A) C(4B) 63(5) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(5A) C(5B) -104(3) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(5B) S(4) 55(4) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(5B) C(4B) 89(7) 1_555 1_555 1_555 1_555 yes S(3) C(4A) C(5B) C(5A) 105(2) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(4A) C(5A) 126(1) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(4A) C(5B) 115(5) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(5A) S(4) 10(6) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(5A) C(4A) -75(6) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(5A) C(5B) -65(4) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(5B) S(4) 81(3) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(5B) C(4A) -68(7) 1_555 1_555 1_555 1_555 yes S(3) C(4B) C(5B) C(5A) 129(3) 1_555 1_555 1_555 1_555 yes S(4) C(3) S(2) C(1) 176.5(5) 1_555 1_555 1_555 1_555 yes S(4) C(5A) C(4A) C(4B) -111(5) 1_555 1_555 1_555 1_555 yes S(4) C(5A) C(4A) C(5B) 56(3) 1_555 1_555 1_555 1_555 yes S(4) C(5A) C(4B) C(4A) 86(5) 1_555 1_555 1_555 1_555 yes S(4) C(5A) C(4B) C(5B) 75(3) 1_555 1_555 1_555 1_555 yes S(4) C(5A) C(5B) C(4A) -134(1) 1_555 1_555 1_555 1_555 yes S(4) C(5A) C(5B) C(4B) -129(2) 1_555 1_555 1_555 1_555 yes S(4) C(5B) C(4A) C(4B) -34(9) 1_555 1_555 1_555 1_555 yes S(4) C(5B) C(4A) C(5A) -49(2) 1_555 1_555 1_555 1_555 yes S(4) C(5B) C(4B) C(4A) 149(7) 1_555 1_555 1_555 1_555 yes S(4) C(5B) C(4B) C(5A) -47(2) 1_555 1_555 1_555 1_555 yes S(4) C(5B) C(5A) C(4A) 134(1) 1_555 1_555 1_555 1_555 yes S(4) C(5B) C(5A) C(4B) 129(2) 1_555 1_555 1_555 1_555 yes S(5) C(6) S(6) C(9) 7.9(5) 1_555 1_555 1_555 1_555 yes S(5) C(6) C(7) S(7) 2(1) 1_555 1_555 1_555 1_555 yes S(5) C(6) C(7) S(8) -179.5(4) 1_555 1_555 1_555 1_555 yes S(5) C(8) S(9) C(12) -174.4(5) 1_555 1_555 1_555 1_555 yes S(5) C(8) C(9) S(6) -1.0(9) 1_555 1_555 1_555 1_555 yes S(5) C(8) C(9) S(10) 180.0(4) 1_555 1_555 1_555 1_555 yes S(6) C(6) S(5) C(8) -8.3(5) 1_555 1_555 1_555 1_555 yes S(6) C(6) C(7) S(7) -178.7(4) 1_555 1_555 1_555 1_555 yes S(6) C(6) C(7) S(8) -0.9(10) 1_555 1_555 1_555 1_555 yes S(6) C(9) S(10) C(13) 153.3(5) 1_555 1_555 1_555 1_555 yes S(6) C(9) C(8) S(9) 178.1(4) 1_555 1_555 1_555 1_555 yes S(7) C(7) S(8) C(11) 7.1(5) 1_555 1_555 1_555 1_555 yes S(7) C(10) S(11) C(14) -154.9(5) 1_555 1_555 1_555 1_555 yes S(7) C(10) C(11) S(8) 1.4(9) 1_555 1_555 1_555 1_555 yes S(7) C(10) C(11) S(12) -179.9(4) 1_555 1_555 1_555 1_555 yes S(8) C(7) S(7) C(10) -6.5(5) 1_555 1_555 1_555 1_555 yes S(8) C(11) S(12) C(15) 179.5(4) 1_555 1_555 1_555 1_555 yes S(8) C(11) C(10) S(11) -179.9(4) 1_555 1_555 1_555 1_555 yes S(9) C(8) S(5) C(6) -173.6(4) 1_555 1_555 1_555 1_555 yes S(9) C(8) C(9) S(10) 0(1) 1_555 1_555 1_555 1_555 yes S(9) C(12) C(13) S(10) -62.1(9) 1_555 1_555 1_555 1_555 yes S(10) C(9) S(6) C(6) 175.0(5) 1_555 1_555 1_555 1_555 yes S(11) C(10) S(7) C(7) -175.8(5) 1_555 1_555 1_555 1_555 yes S(11) C(10) C(11) S(12) -1(1) 1_555 1_555 1_555 1_555 yes S(11) C(14) C(15) S(12) 68.1(8) 1_555 1_555 1_555 1_555 yes S(12) C(11) S(8) C(7) 176.0(4) 1_555 1_555 1_555 1_555 yes C(1) S(1) C(2) C(3) 4.7(7) 1_555 1_555 1_555 1_555 yes C(1) S(2) C(3) C(2) -4.0(7) 1_555 1_555 1_555 1_555 yes C(1) C(1) S(1) C(2) -171.8(9) 1_555 2_666 2_666 2_666 yes C(1) C(1) S(2) C(3) 172.0(9) 1_555 2_666 2_666 2_666 yes C(2) S(3) C(4A) C(4B) 85(5) 1_555 1_555 1_555 1_555 yes C(2) S(3) C(4A) C(5A) 15(1) 1_555 1_555 1_555 1_555 yes C(2) S(3) C(4A) C(5B) -38(3) 1_555 1_555 1_555 1_555 yes C(2) S(3) C(4B) C(4A) -98(5) 1_555 1_555 1_555 1_555 yes C(2) S(3) C(4B) C(5A) -31(4) 1_555 1_555 1_555 1_555 yes C(2) S(3) C(4B) C(5B) -66(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) S(4) C(5A) -22.9(9) 1_555 1_555 1_555 1_555 yes C(2) C(3) S(4) C(5B) 9(1) 1_555 1_555 1_555 1_555 yes C(3) S(4) C(5A) C(4A) 47(1) 1_555 1_555 1_555 1_555 yes C(3) S(4) C(5A) C(4B) 18(3) 1_555 1_555 1_555 1_555 yes C(3) S(4) C(5A) C(5B) 94(2) 1_555 1_555 1_555 1_555 yes C(3) S(4) C(5B) C(4A) -38(3) 1_555 1_555 1_555 1_555 yes C(3) S(4) C(5B) C(4B) -47(3) 1_555 1_555 1_555 1_555 yes C(3) S(4) C(5B) C(5A) -91(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) S(3) C(4A) 8.8(9) 1_555 1_555 1_555 1_555 yes C(3) C(2) S(3) C(4B) 28(2) 1_555 1_555 1_555 1_555 yes C(4A) S(3) C(4B) C(5A) 66(5) 1_555 1_555 1_555 1_555 yes C(4A) S(3) C(4B) C(5B) 32(4) 1_555 1_555 1_555 1_555 yes C(4A) C(4B) C(5A) C(5B) 10(5) 1_555 1_555 1_555 1_555 yes C(4A) C(4B) C(5B) C(5A) -162(9) 1_555 1_555 1_555 1_555 yes C(4A) C(5A) S(4) C(5B) -46(2) 1_555 1_555 1_555 1_555 yes C(4A) C(5A) C(4B) C(5B) -10(5) 1_555 1_555 1_555 1_555 yes C(4A) C(5A) C(5B) C(4B) 5(2) 1_555 1_555 1_555 1_555 yes C(4A) C(5B) S(4) C(5A) 53(3) 1_555 1_555 1_555 1_555 yes C(4A) C(5B) C(4B) C(5A) 162(9) 1_555 1_555 1_555 1_555 yes C(4A) C(5B) C(5A) C(4B) -5(2) 1_555 1_555 1_555 1_555 yes C(4B) S(3) C(4A) C(5A) -69(5) 1_555 1_555 1_555 1_555 yes C(4B) S(3) C(4A) C(5B) -123(6) 1_555 1_555 1_555 1_555 yes C(4B) C(4A) C(5A) C(5B) -167(6) 1_555 1_555 1_555 1_555 yes C(4B) C(4A) C(5B) C(5A) 15(8) 1_555 1_555 1_555 1_555 yes C(4B) C(5A) S(4) C(5B) -76(4) 1_555 1_555 1_555 1_555 yes C(4B) C(5A) C(4A) C(5B) 167(6) 1_555 1_555 1_555 1_555 yes C(4B) C(5B) S(4) C(5A) 44(2) 1_555 1_555 1_555 1_555 yes C(4B) C(5B) C(4A) C(5A) -15(8) 1_555 1_555 1_555 1_555 yes C(5A) C(4A) C(4B) C(5B) 10(5) 1_555 1_555 1_555 1_555 yes C(5A) C(4B) C(4A) C(5B) -10(5) 1_555 1_555 1_555 1_555 yes C(6) S(5) C(8) C(9) 5.6(7) 1_555 1_555 1_555 1_555 yes C(6) S(6) C(9) C(8) -4.2(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) S(7) C(10) 171.5(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) S(8) C(11) -171.0(7) 1_555 1_555 1_555 1_555 yes C(7) S(7) C(10) C(11) 3.1(7) 1_555 1_555 1_555 1_555 yes C(7) S(8) C(11) C(10) -5.1(7) 1_555 1_555 1_555 1_555 yes C(7) C(6) S(5) C(8) 170.5(7) 1_555 1_555 1_555 1_555 yes C(7) C(6) S(6) C(9) -170.9(7) 1_555 1_555 1_555 1_555 yes C(8) S(9) C(12) C(13) 25.2(9) 1_555 1_555 1_555 1_555 yes C(8) C(9) S(10) C(13) -27.6(8) 1_555 1_555 1_555 1_555 yes C(9) S(10) C(13) C(12) 58.9(8) 1_555 1_555 1_555 1_555 yes C(9) C(8) S(9) C(12) 6.5(9) 1_555 1_555 1_555 1_555 yes C(10) S(11) C(14) C(15) -58.9(6) 1_555 1_555 1_555 1_555 yes C(10) C(11) S(12) C(15) 0.7(8) 1_555 1_555 1_555 1_555 yes C(11) S(12) C(15) C(14) -34.1(7) 1_555 1_555 1_555 1_555 yes C(11) C(10) S(11) C(14) 26.3(8) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(19) C(20) -164(14) 1_555 1_555 1_555 1_555 yes C(16) C(18) C(17) C(19) -180.0(7) 1_555 2_475 2_475 2_475 yes C(18) C(16) C(17) C(19) -179.8(8) 1_555 2_475 2_475 2_475 yes C(18) C(17) C(19) C(20) 18(15) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 S(3) S(10) 3.508(3) . 1_556 ? S(3) S(11) 3.553(3) . 2_766 ? S(4) S(12) 3.483(3) . 2_665 ? S(4) S(9) 3.499(3) . 1_455 ? S(9) S(11) 3.498(3) . 2_766 ? S(10) C(4B) 3.41(5) . 1_554 ? S(10) S(12) 3.561(3) . 2_665 ? C(4A) C(18) 3.40(2) . 2_576 ? C(8) C(14) 3.53(1) . 2_765 ? C(9) C(14) 3.57(1) . 2_765 ? #------------------------------------------------------------------------------ #===END data_General _audit_creation_date 'Mon Aug 2 05:39:05 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Hiroshi M. Yamamoto' _publ_contact_author_address ; Hirosawa, Wako-shi, Saitama 351-0198 (Japan) ; _publ_contact_author_email ' yhiroshi@postman.riken.go.jp ' _publ_contact_author_fax ' +81-(0)48-462-4611 ' _publ_contact_author_phone ' +81-(0)48-467-9410 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' ' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # _publ_section_title ; Structural and physical properties of conducting cation radical satls containing supramolecular assmblies based on pBIB derivatives (pBIB=p-Bis(iodoethynyl)benzene) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_ET3Br.pBIBd4 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C40 H28 Br I2 S24 ' _chemical_formula_moiety '?' _chemical_formula_weight 1615.81 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.193(2) _cell_length_b 15.034(3) _cell_length_c 9.423(2) _cell_angle_alpha 95.75(2) _cell_angle_beta 106.92(2) _cell_angle_gamma 86.66(2) _cell_volume 1373.9(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 13.2 _cell_measurement_theta_max 14.8 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.819 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'MacScience MXC18' _diffrn_reflns_number 10570 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_theta_max 32.50 _diffrn_measured_fraction_theta_max 1.0010 _diffrn_reflns_theta_full 32.50 _diffrn_measured_fraction_theta_full 1.0010 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 0 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9947 _reflns_number_gt 4819 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.1008 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4819 _refine_ls_number_parameters 311 _refine_ls_goodness_of_fit_ref 2.335 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 11.2840 _refine_diff_density_max 9.64 _refine_diff_density_min -1.52 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.15793(7) 0.00236(4) 0.35554(7) 0.0444(2) Uani 1.00 d . . . Br(1) Br 0.0000 0.0000 0.0000 0.0419(3) Uani 1.00 d S . . S(1) S 0.8120(2) 0.4241(1) -0.0592(2) 0.0411(5) Uani 1.00 d . . . S(2) S 1.0647(2) 0.4199(1) 0.1905(2) 0.0382(5) Uani 1.00 d . . . S(3) S 0.6975(2) 0.2635(2) 0.0125(3) 0.0520(6) Uani 1.00 d . . . S(4) S 0.9998(2) 0.2601(2) 0.3072(3) 0.0485(6) Uani 1.00 d . . . S(5) S 0.4759(2) 0.4267(1) 0.2800(2) 0.0401(5) Uani 1.00 d . . . S(6) S 0.7356(2) 0.4159(1) 0.5194(2) 0.0380(5) Uani 1.00 d . . . S(7) S 0.5973(2) 0.5824(1) 0.1457(2) 0.0394(5) Uani 1.00 d . . . S(8) S 0.8568(2) 0.5721(1) 0.3856(2) 0.0397(5) Uani 1.00 d . . . S(9) S 0.3612(2) 0.2657(2) 0.3510(3) 0.0544(7) Uani 1.00 d . . . S(10) S 0.6711(2) 0.2524(2) 0.6296(3) 0.0516(6) Uani 1.00 d . . . S(11) S 0.6640(2) 0.7452(2) 0.0329(3) 0.0506(6) Uani 1.00 d . . . S(12) S 0.9739(2) 0.7306(2) 0.3139(3) 0.0535(6) Uani 1.00 d . . . C(1) C 0.9742(8) 0.4673(5) 0.0280(8) 0.030(2) Uani 1.00 d . . . C(2) C 0.8308(8) 0.3374(5) 0.0562(9) 0.034(2) Uani 1.00 d . . . C(3) C 0.9476(8) 0.3349(5) 0.1708(8) 0.030(2) Uani 1.00 d . . . C(4) C 0.7184(9) 0.2285(6) 0.1950(10) 0.040(2) Uani 1.00 d . . . C(5) C 0.8569(10) 0.1860(6) 0.262(1) 0.044(2) Uani 1.00 d . . . C(6) C 0.6408(8) 0.4670(5) 0.3618(8) 0.030(2) Uani 1.00 d . . . C(7) C 0.6928(8) 0.5317(5) 0.3046(8) 0.031(2) Uani 1.00 d . . . C(8) C 0.4982(8) 0.3382(5) 0.3925(9) 0.035(2) Uani 1.00 d . . . C(9) C 0.6175(8) 0.3326(5) 0.5025(8) 0.031(2) Uani 1.00 d . . . C(10) C 0.7157(8) 0.6653(5) 0.1615(9) 0.032(2) Uani 1.00 d . . . C(11) C 0.8353(8) 0.6603(5) 0.2714(9) 0.033(2) Uani 1.00 d . . . C(12) C 0.389(1) 0.2283(7) 0.532(1) 0.055(3) Uani 1.00 d . . . C(13) C 0.521(1) 0.1852(7) 0.596(1) 0.057(3) Uani 1.00 d . . . C(14A) C 0.825(2) 0.780(1) 0.027(2) 0.041(4) Uani 0.50 d P . . C(14B) C 0.816(2) 0.813(1) 0.077(2) 0.0415 Uani 0.50 d P . . C(15A) C 0.916(2) 0.814(1) 0.178(2) 0.041(4) Uani 0.50 d P . . C(15B) C 0.952(2) 0.767(1) 0.136(2) 0.0409 Uani 0.50 d P . . C(16) C 0.3609(9) -0.0029(7) 0.967(1) 0.048(3) Uani 1.00 d . . . C(17) C 0.4214(9) -0.0003(5) 0.8504(9) 0.037(2) Uani 1.00 d . . . C(18) C 0.5583(9) 0.0053(6) 0.894(1) 0.052(2) Uani 1.00 d . . . C(19) C 0.3362(7) 0.0019(5) 0.6931(8) 0.027(2) Uani 1.00 d . . . C(20) C 0.274(1) 0.0013(7) 0.575(1) 0.058(3) Uani 1.00 d . . . H(1) H 0.7057 0.2800 0.2594 0.0653 Uiso 1.00 calc . . . H(2) H 0.6489 0.1872 0.1890 0.0653 Uiso 1.00 calc . . . H(3) H 0.8732 0.1389 0.1916 0.0540 Uiso 1.00 calc . . . H(4) H 0.8572 0.1606 0.3503 0.0540 Uiso 1.00 calc . . . H(5) H 0.3788 0.2792 0.5987 0.0653 Uiso 1.00 calc . . . H(6) H 0.3186 0.1874 0.5271 0.0653 Uiso 1.00 calc . . . H(7) H 0.5300 0.1346 0.5295 0.0692 Uiso 1.00 calc . . . H(8) H 0.5207 0.1648 0.6887 0.0692 Uiso 1.00 calc . . . H(9) H 0.8724 0.7300 -0.0087 0.0512 Uiso 0.50 calc P . . H(10) H 0.8182 0.8377 -0.0124 0.0512 Uiso 1.00 calc . . . H(11) H 0.8095 0.8600 0.1490 0.0512 Uiso 0.50 calc P . . H(12) H 0.9079 0.8693 0.2342 0.0501 Uiso 0.50 calc P . . H(13) H 1.0238 0.8060 0.1404 0.0501 Uiso 1.00 calc . . . H(14) H 0.9593 0.7155 0.0681 0.0501 Uiso 0.50 calc P . . H(15) H 0.2585 -0.0043 0.9436 0.0507 Uiso 1.00 calc . . . H(16) H 0.6034 0.0081 0.8121 0.0507 Uiso 1.00 calc . . . 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 I(1) 0.0449(3) 0.0442(3) 0.0387(3) -0.0028(2) 0.0025(2) 0.0058(2) Br(1) 0.0401(6) 0.0551(8) 0.0338(5) -0.0091(6) 0.0124(5) 0.0087(5) S(1) 0.039(1) 0.039(1) 0.044(1) -0.0094(9) 0.0012(9) 0.0201(9) S(2) 0.045(1) 0.0324(10) 0.0342(9) -0.0160(9) 0.0006(8) 0.0102(8) S(3) 0.041(1) 0.063(1) 0.049(1) -0.025(1) -0.0018(10) 0.025(1) S(4) 0.042(1) 0.052(1) 0.049(1) -0.0170(10) -0.0024(10) 0.0291(10) S(5) 0.035(1) 0.038(1) 0.045(1) -0.0077(9) 0.0004(9) 0.0205(9) S(6) 0.041(1) 0.0331(10) 0.0361(10) -0.0144(8) -0.0012(8) 0.0125(8) S(7) 0.041(1) 0.036(1) 0.0371(10) -0.0169(9) -0.0019(9) 0.0132(8) S(8) 0.035(1) 0.036(1) 0.045(1) -0.0076(8) 0.0002(9) 0.0182(8) S(9) 0.038(1) 0.070(2) 0.052(1) -0.027(1) -0.0037(10) 0.029(1) S(10) 0.040(1) 0.055(1) 0.059(1) -0.014(1) -0.001(1) 0.036(1) S(11) 0.039(1) 0.058(1) 0.055(1) -0.013(1) 0.0002(10) 0.035(1) S(12) 0.040(1) 0.064(1) 0.054(1) -0.024(1) -0.0032(10) 0.029(1) C(1) 0.040(4) 0.021(3) 0.029(3) -0.006(3) 0.011(3) 0.004(3) C(2) 0.034(4) 0.034(4) 0.034(4) -0.008(3) 0.007(3) 0.011(3) C(3) 0.034(4) 0.027(4) 0.032(3) -0.005(3) 0.008(3) 0.010(3) C(4) 0.037(4) 0.043(5) 0.048(4) -0.006(4) 0.019(4) 0.010(4) C(5) 0.049(5) 0.035(4) 0.049(5) -0.011(4) 0.011(4) 0.013(4) C(6) 0.035(4) 0.023(3) 0.031(3) -0.005(3) 0.009(3) 0.004(3) C(7) 0.035(4) 0.025(4) 0.031(3) -0.005(3) 0.007(3) 0.006(3) C(8) 0.036(4) 0.034(4) 0.037(4) -0.008(3) 0.008(3) 0.013(3) C(9) 0.031(4) 0.031(4) 0.033(3) -0.004(3) 0.011(3) 0.008(3) C(10) 0.030(4) 0.031(4) 0.035(4) -0.004(3) 0.008(3) 0.009(3) C(11) 0.031(4) 0.029(4) 0.040(4) -0.003(3) 0.009(3) 0.015(3) C(12) 0.052(5) 0.068(6) 0.049(5) -0.022(5) 0.014(4) 0.016(5) C(13) 0.052(6) 0.054(6) 0.067(6) -0.016(5) 0.008(5) 0.027(5) C(14A) 0.054(6) 0.033(8) 0.038(8) -0.017(6) 0.011(6) 0.007(5) C(14B) 0.0543 0.0329 0.0385 -0.0169 0.0107 0.0073 C(15A) 0.042(7) 0.041(8) 0.043(7) -0.013(6) 0.012(5) 0.011(5) C(15B) 0.0415 0.0410 0.0434 -0.0134 0.0123 0.0108 C(16) 0.045(5) 0.060(6) 0.044(5) -0.009(4) 0.020(4) 0.008(4) C(17) 0.048(5) 0.035(4) 0.034(4) -0.004(4) 0.017(4) 0.005(3) C(18) 0.037(4) 0.048(5) 0.058(5) -0.015(4) -0.012(4) 0.015(4) C(19) 0.018(3) 0.027(4) 0.031(3) 0.002(3) 0.000(3) 0.003(3) C(20) 0.062(6) 0.037(5) 0.089(8) -0.002(4) 0.045(5) 0.005(5) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? _atoms_sites_solution_primary 'direct methods' _atoms_sites_solution_secondary 'Fourier difference' #------------------------------------------------------------------------------ _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 I(1) C(20) 2.07(1) . . yes S(1) C(1) 1.748(8) . . yes S(1) C(2) 1.747(8) . . yes S(2) C(1) 1.739(8) . . yes S(2) C(3) 1.758(8) . . yes S(3) C(2) 1.735(8) . . yes S(3) C(4) 1.798(9) . . yes S(4) C(3) 1.738(7) . . yes S(4) C(5) 1.809(9) . . yes S(5) C(6) 1.749(8) . . yes S(5) C(8) 1.747(8) . . yes S(6) C(6) 1.742(8) . . yes S(6) C(9) 1.751(8) . . yes S(7) C(7) 1.751(8) . . yes S(7) C(10) 1.750(8) . . yes S(8) C(7) 1.740(8) . . yes S(8) C(11) 1.755(8) . . yes S(9) C(8) 1.752(8) . . yes S(9) C(12) 1.79(1) . . yes S(10) C(9) 1.738(8) . . yes S(10) C(13) 1.82(1) . . yes S(11) C(10) 1.742(8) . . yes S(11) C(14A) 1.77(2) . . yes S(11) C(14B) 1.82(2) . . yes S(12) C(11) 1.742(8) . . yes S(12) C(15A) 1.84(2) . . yes S(12) C(15B) 1.77(2) . . yes C(1) C(1) 1.36(1) . 2_765 yes C(2) C(3) 1.36(1) . . yes C(4) C(5) 1.50(1) . . yes C(6) C(7) 1.36(1) . . yes C(8) C(9) 1.35(1) . . yes C(10) C(11) 1.35(1) . . yes C(12) C(13) 1.45(1) . . yes C(14A) C(14B) 0.66(2) . . yes C(14A) C(15A) 1.51(3) . . yes C(14A) C(15B) 1.41(3) . . yes C(14B) C(15A) 1.18(3) . . yes C(14B) C(15B) 1.49(3) . . yes C(15A) C(15B) 0.89(2) . . yes C(16) C(17) 1.42(1) . . yes C(16) C(18) 1.33(1) . 2_657 yes C(17) C(18) 1.34(1) . . yes C(17) C(19) 1.49(1) . . yes C(19) C(20) 1.11(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S(1) C(2) 95.4(4) 1_555 1_555 1_555 yes C(1) S(2) C(3) 95.1(4) 1_555 1_555 1_555 yes C(2) S(3) C(4) 99.0(4) 1_555 1_555 1_555 yes C(3) S(4) C(5) 102.8(4) 1_555 1_555 1_555 yes C(6) S(5) C(8) 94.9(4) 1_555 1_555 1_555 yes C(6) S(6) C(9) 95.4(4) 1_555 1_555 1_555 yes C(7) S(7) C(10) 95.2(4) 1_555 1_555 1_555 yes C(7) S(8) C(11) 95.2(4) 1_555 1_555 1_555 yes C(8) S(9) C(12) 98.6(4) 1_555 1_555 1_555 yes C(9) S(10) C(13) 103.7(4) 1_555 1_555 1_555 yes C(10) S(11) C(14A) 100.7(7) 1_555 1_555 1_555 yes C(10) S(11) C(14B) 102.0(7) 1_555 1_555 1_555 yes C(14A) S(11) C(14B) 21.2(8) 1_555 1_555 1_555 yes C(11) S(12) C(15A) 103.3(6) 1_555 1_555 1_555 yes C(11) S(12) C(15B) 99.1(6) 1_555 1_555 1_555 yes C(15A) S(12) C(15B) 28.5(8) 1_555 1_555 1_555 yes S(1) C(1) S(2) 115.1(4) 1_555 1_555 1_555 yes S(1) C(1) C(1) 122.3(8) 1_555 1_555 2_765 yes S(2) C(1) C(1) 122.6(8) 1_555 1_555 2_765 yes S(1) C(2) S(3) 116.5(4) 1_555 1_555 1_555 yes S(1) C(2) C(3) 116.8(6) 1_555 1_555 1_555 yes S(3) C(2) C(3) 126.7(6) 1_555 1_555 1_555 yes S(2) C(3) S(4) 113.6(4) 1_555 1_555 1_555 yes S(2) C(3) C(2) 117.0(6) 1_555 1_555 1_555 yes S(4) C(3) C(2) 129.4(6) 1_555 1_555 1_555 yes S(3) C(4) C(5) 113.2(6) 1_555 1_555 1_555 yes S(3) C(4) H(1) 108.6(7) 1_555 1_555 1_555 no S(3) C(4) H(2) 108.9(7) 1_555 1_555 1_555 no C(5) C(4) H(1) 108.7(8) 1_555 1_555 1_555 no C(5) C(4) H(2) 109.3(8) 1_555 1_555 1_555 no H(1) C(4) H(2) 108.1(8) 1_555 1_555 1_555 no S(4) C(5) C(4) 115.4(6) 1_555 1_555 1_555 yes S(4) C(5) H(3) 107.3(7) 1_555 1_555 1_555 no S(4) C(5) H(4) 107.8(7) 1_555 1_555 1_555 no C(4) C(5) H(3) 108.2(8) 1_555 1_555 1_555 no C(4) C(5) H(4) 109.4(9) 1_555 1_555 1_555 no H(3) C(5) H(4) 108.5(9) 1_555 1_555 1_555 no S(5) C(6) S(6) 115.0(4) 1_555 1_555 1_555 yes S(5) C(6) C(7) 122.6(6) 1_555 1_555 1_555 yes S(6) C(6) C(7) 122.4(6) 1_555 1_555 1_555 yes S(7) C(7) S(8) 115.0(4) 1_555 1_555 1_555 yes S(7) C(7) C(6) 122.1(6) 1_555 1_555 1_555 yes S(8) C(7) C(6) 122.8(6) 1_555 1_555 1_555 yes S(5) C(8) S(9) 115.8(5) 1_555 1_555 1_555 yes S(5) C(8) C(9) 117.6(6) 1_555 1_555 1_555 yes S(9) C(8) C(9) 126.6(6) 1_555 1_555 1_555 yes S(6) C(9) S(10) 114.9(4) 1_555 1_555 1_555 yes S(6) C(9) C(8) 116.5(6) 1_555 1_555 1_555 yes S(10) C(9) C(8) 128.6(6) 1_555 1_555 1_555 yes S(7) C(10) S(11) 115.4(4) 1_555 1_555 1_555 yes S(7) C(10) C(11) 116.8(6) 1_555 1_555 1_555 yes S(11) C(10) C(11) 127.7(6) 1_555 1_555 1_555 yes S(8) C(11) S(12) 114.9(4) 1_555 1_555 1_555 yes S(8) C(11) C(10) 117.1(6) 1_555 1_555 1_555 yes S(12) C(11) C(10) 128.0(6) 1_555 1_555 1_555 yes S(9) C(12) C(13) 116.2(8) 1_555 1_555 1_555 yes S(9) C(12) H(5) 108.0(8) 1_555 1_555 1_555 no S(9) C(12) H(6) 108.2(8) 1_555 1_555 1_555 no C(13) C(12) H(5) 107.8(10) 1_555 1_555 1_555 no C(13) C(12) H(6) 108.3(10) 1_555 1_555 1_555 no H(5) C(12) H(6) 108(1) 1_555 1_555 1_555 no S(10) C(13) C(12) 116.8(7) 1_555 1_555 1_555 yes S(10) C(13) H(7) 107.4(9) 1_555 1_555 1_555 no S(10) C(13) H(8) 107.8(8) 1_555 1_555 1_555 no C(12) C(13) H(7) 107.4(10) 1_555 1_555 1_555 no C(12) C(13) H(8) 108(1) 1_555 1_555 1_555 no H(7) C(13) H(8) 108.8(10) 1_555 1_555 1_555 no S(11) C(14A) C(14B) 84(3) 1_555 1_555 1_555 yes S(11) C(14A) C(15A) 113(1) 1_555 1_555 1_555 yes S(11) C(14A) C(15B) 125(1) 1_555 1_555 1_555 yes S(11) C(14A) H(9) 108(1) 1_555 1_555 1_555 no S(11) C(14A) H(10) 112(1) 1_555 1_555 1_555 no C(14B) C(14A) C(15A) 48(2) 1_555 1_555 1_555 yes C(14B) C(14A) C(15B) 83(2) 1_555 1_555 1_555 yes C(14B) C(14A) H(9) 155(3) 1_555 1_555 1_555 no C(14B) C(14A) H(10) 69(2) 1_555 1_555 1_555 no C(15A) C(14A) C(15B) 35(1) 1_555 1_555 1_555 yes C(15A) C(14A) H(9) 106(1) 1_555 1_555 1_555 no C(15A) C(14A) H(10) 93(1) 1_555 1_555 1_555 no C(15B) C(14A) H(9) 71(1) 1_555 1_555 1_555 no C(15B) C(14A) H(10) 112(1) 1_555 1_555 1_555 no H(9) C(14A) H(10) 121(2) 1_555 1_555 1_555 no S(11) C(14B) C(14A) 74(2) 1_555 1_555 1_555 yes S(11) C(14B) C(15A) 131(1) 1_555 1_555 1_555 yes S(11) C(14B) C(15B) 117(1) 1_555 1_555 1_555 yes S(11) C(14B) H(10) 108(1) 1_555 1_555 1_555 no S(11) C(14B) H(11) 109(1) 1_555 1_555 1_555 no C(14A) C(14B) C(15A) 106(3) 1_555 1_555 1_555 yes C(14A) C(14B) C(15B) 70(2) 1_555 1_555 1_555 yes C(14A) C(14B) H(10) 69(2) 1_555 1_555 1_555 no C(14A) C(14B) H(11) 175(4) 1_555 1_555 1_555 no C(15A) C(14B) C(15B) 36(1) 1_555 1_555 1_555 yes C(15A) C(14B) H(10) 117(2) 1_555 1_555 1_555 no C(15A) C(14B) H(11) 70(1) 1_555 1_555 1_555 no C(15B) C(14B) H(10) 106(1) 1_555 1_555 1_555 no C(15B) C(14B) H(11) 106(1) 1_555 1_555 1_555 no H(10) C(14B) H(11) 108(1) 1_555 1_555 1_555 no S(12) C(15A) C(14A) 115(1) 1_555 1_555 1_555 yes S(12) C(15A) C(14B) 126(1) 1_555 1_555 1_555 yes S(12) C(15A) C(15B) 71(1) 1_555 1_555 1_555 yes S(12) C(15A) H(11) 128(1) 1_555 1_555 1_555 no S(12) C(15A) H(12) 105(1) 1_555 1_555 1_555 no S(12) C(15A) H(13) 92(1) 1_555 1_555 1_555 no C(14A) C(15A) C(14B) 24(1) 1_555 1_555 1_555 yes C(14A) C(15A) C(15B) 66(1) 1_555 1_555 1_555 yes C(14A) C(15A) H(11) 70(1) 1_555 1_555 1_555 no C(14A) C(15A) H(12) 127(1) 1_555 1_555 1_555 no C(14A) C(15A) H(13) 95(1) 1_555 1_555 1_555 no C(14B) C(15A) C(15B) 91(2) 1_555 1_555 1_555 yes C(14B) C(15A) H(11) 46(1) 1_555 1_555 1_555 no C(14B) C(15A) H(12) 103(1) 1_555 1_555 1_555 no C(14B) C(15A) H(13) 114(1) 1_555 1_555 1_555 no C(15B) C(15A) H(11) 137(2) 1_555 1_555 1_555 no C(15B) C(15A) H(12) 162(2) 1_555 1_555 1_555 no C(15B) C(15A) H(13) 50(1) 1_555 1_555 1_555 no H(11) C(15A) H(12) 58(1) 1_555 1_555 1_555 no H(11) C(15A) H(13) 138(1) 1_555 1_555 1_555 no H(12) C(15A) H(13) 113(1) 1_555 1_555 1_555 no S(12) C(15B) C(14A) 125(1) 1_555 1_555 1_555 yes S(12) C(15B) C(14B) 112(1) 1_555 1_555 1_555 yes S(12) C(15B) C(15A) 80(1) 1_555 1_555 1_555 yes S(12) C(15B) H(13) 109(1) 1_555 1_555 1_555 no S(12) C(15B) H(14) 108(1) 1_555 1_555 1_555 no C(14A) C(15B) C(14B) 26.3(10) 1_555 1_555 1_555 yes C(14A) C(15B) C(15A) 78(2) 1_555 1_555 1_555 yes C(14A) C(15B) H(13) 117(1) 1_555 1_555 1_555 no C(14A) C(15B) H(14) 82(1) 1_555 1_555 1_555 no C(14B) C(15B) C(15A) 52(1) 1_555 1_555 1_555 yes C(14B) C(15B) H(13) 109(1) 1_555 1_555 1_555 no C(14B) C(15B) H(14) 109(1) 1_555 1_555 1_555 no C(15A) C(15B) H(13) 84(2) 1_555 1_555 1_555 no C(15A) C(15B) H(14) 160(2) 1_555 1_555 1_555 no H(13) C(15B) H(14) 107(1) 1_555 1_555 1_555 no C(17) C(16) C(18) 119.1(9) 1_555 1_555 2_657 yes C(17) C(16) H(15) 119.4(9) 1_555 1_555 1_555 no C(18) C(16) H(15) 121.5(9) 2_657 1_555 1_555 no C(16) C(17) C(18) 115.1(8) 1_555 1_555 1_555 yes C(16) C(17) C(19) 121.4(8) 1_555 1_555 1_555 yes C(18) C(17) C(19) 123.4(8) 1_555 1_555 1_555 yes C(16) C(18) C(17) 125.7(10) 2_657 1_555 1_555 yes C(16) C(18) H(16) 117.9(9) 2_657 1_555 1_555 no C(17) C(18) H(16) 116.4(9) 1_555 1_555 1_555 no C(17) C(19) C(20) 178.2(9) 1_555 1_555 1_555 yes I(1) C(20) C(19) 179.0(9) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I(1) C(20) C(19) C(17) -150(39) 1_555 1_555 1_555 1_555 yes S(1) C(1) S(2) C(3) 8.0(5) 1_555 1_555 1_555 1_555 yes S(1) C(1) C(1) S(1) -180.0 1_555 1_555 2_765 2_765 yes S(1) C(1) C(1) S(2) 0(1) 1_555 1_555 2_765 2_765 yes S(1) C(2) S(3) C(4) -152.9(5) 1_555 1_555 1_555 1_555 yes S(1) C(2) C(3) S(2) 0.7(10) 1_555 1_555 1_555 1_555 yes S(1) C(2) C(3) S(4) 179.4(5) 1_555 1_555 1_555 1_555 yes S(2) C(1) S(1) C(2) -7.7(5) 1_555 1_555 1_555 1_555 yes S(2) C(1) C(1) S(2) -180.0 1_555 1_555 2_765 2_765 yes S(2) C(3) S(4) C(5) 177.5(5) 1_555 1_555 1_555 1_555 yes S(2) C(3) C(2) S(3) -179.1(5) 1_555 1_555 1_555 1_555 yes S(3) C(2) S(1) C(1) -176.0(5) 1_555 1_555 1_555 1_555 yes S(3) C(2) C(3) S(4) 0(1) 1_555 1_555 1_555 1_555 yes S(3) C(4) C(5) S(4) 67.3(8) 1_555 1_555 1_555 1_555 yes S(4) C(3) S(2) C(1) 175.9(5) 1_555 1_555 1_555 1_555 yes S(5) C(6) S(6) C(9) 7.9(5) 1_555 1_555 1_555 1_555 yes S(5) C(6) C(7) S(7) 1(1) 1_555 1_555 1_555 1_555 yes S(5) C(6) C(7) S(8) 180.0(4) 1_555 1_555 1_555 1_555 yes S(5) C(8) S(9) C(12) -152.8(6) 1_555 1_555 1_555 1_555 yes S(5) C(8) C(9) S(6) 0.3(10) 1_555 1_555 1_555 1_555 yes S(5) C(8) C(9) S(10) -178.8(5) 1_555 1_555 1_555 1_555 yes S(6) C(6) S(5) C(8) -7.7(5) 1_555 1_555 1_555 1_555 yes S(6) C(6) C(7) S(7) 179.7(4) 1_555 1_555 1_555 1_555 yes S(6) C(6) C(7) S(8) -1(1) 1_555 1_555 1_555 1_555 yes S(6) C(9) S(10) C(13) 173.8(5) 1_555 1_555 1_555 1_555 yes S(6) C(9) C(8) S(9) -179.2(5) 1_555 1_555 1_555 1_555 yes S(7) C(7) S(8) C(11) 7.4(5) 1_555 1_555 1_555 1_555 yes S(7) C(10) S(11) C(14A) -154.7(7) 1_555 1_555 1_555 1_555 yes S(7) C(10) S(11) C(14B) -176.4(8) 1_555 1_555 1_555 1_555 yes S(7) C(10) C(11) S(8) -0.6(10) 1_555 1_555 1_555 1_555 yes S(7) C(10) C(11) S(12) 178.8(5) 1_555 1_555 1_555 1_555 yes S(8) C(7) S(7) C(10) -7.6(5) 1_555 1_555 1_555 1_555 yes S(8) C(11) S(12) C(15A) -179.2(8) 1_555 1_555 1_555 1_555 yes S(8) C(11) S(12) C(15B) 152.1(8) 1_555 1_555 1_555 1_555 yes S(8) C(11) C(10) S(11) 179.1(5) 1_555 1_555 1_555 1_555 yes S(9) C(8) S(5) C(6) -176.0(5) 1_555 1_555 1_555 1_555 yes S(9) C(8) C(9) S(10) 1(1) 1_555 1_555 1_555 1_555 yes S(9) C(12) C(13) S(10) 61(1) 1_555 1_555 1_555 1_555 yes S(10) C(9) S(6) C(6) 174.3(5) 1_555 1_555 1_555 1_555 yes S(11) C(10) S(7) C(7) -174.8(5) 1_555 1_555 1_555 1_555 yes S(11) C(10) C(11) S(12) -1(1) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(14B) C(15A) 129(2) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(14B) C(15B) 126(1) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(15A) S(12) 65(1) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(15A) C(14B) -57(3) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(15A) C(15B) 118(2) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(15B) S(12) -12(2) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(15B) C(14B) -77(3) 1_555 1_555 1_555 1_555 yes S(11) C(14A) C(15B) C(15A) -80(2) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(14A) C(15A) -129(2) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(14A) C(15B) -126(1) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(15A) S(12) 12(3) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(15A) C(14A) 84(3) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(15A) C(15B) 80(2) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(15B) S(12) -67(1) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(15B) C(14A) 60(2) 1_555 1_555 1_555 1_555 yes S(11) C(14B) C(15B) C(15A) -123(2) 1_555 1_555 1_555 1_555 yes S(12) C(11) S(8) C(7) 176.4(5) 1_555 1_555 1_555 1_555 yes S(12) C(15A) C(14A) C(14B) 122(3) 1_555 1_555 1_555 1_555 yes S(12) C(15A) C(14A) C(15B) -53(1) 1_555 1_555 1_555 1_555 yes S(12) C(15A) C(14B) C(14A) -71(4) 1_555 1_555 1_555 1_555 yes S(12) C(15A) C(14B) C(15B) -67(2) 1_555 1_555 1_555 1_555 yes S(12) C(15A) C(15B) C(14A) 130(1) 1_555 1_555 1_555 1_555 yes S(12) C(15A) C(15B) C(14B) 128(1) 1_555 1_555 1_555 1_555 yes S(12) C(15B) C(14A) C(14B) 65(3) 1_555 1_555 1_555 1_555 yes S(12) C(15B) C(14A) C(15A) 68(2) 1_555 1_555 1_555 1_555 yes S(12) C(15B) C(14B) C(14A) -127(2) 1_555 1_555 1_555 1_555 yes S(12) C(15B) C(14B) C(15A) 56(1) 1_555 1_555 1_555 1_555 yes S(12) C(15B) C(15A) C(14A) -130(1) 1_555 1_555 1_555 1_555 yes S(12) C(15B) C(15A) C(14B) -128(1) 1_555 1_555 1_555 1_555 yes C(1) S(1) C(2) C(3) 4.2(8) 1_555 1_555 1_555 1_555 yes C(1) S(2) C(3) C(2) -5.3(7) 1_555 1_555 1_555 1_555 yes C(1) C(1) S(1) C(2) -171.8(10) 1_555 2_765 2_765 2_765 yes C(1) C(1) S(2) C(3) 171.6(10) 1_555 2_765 2_765 2_765 yes C(2) S(3) C(4) C(5) -59.4(7) 1_555 1_555 1_555 1_555 yes C(2) C(3) S(4) C(5) -1.2(10) 1_555 1_555 1_555 1_555 yes C(3) S(4) C(5) C(4) -32.5(8) 1_555 1_555 1_555 1_555 yes C(3) C(2) S(3) C(4) 26.9(9) 1_555 1_555 1_555 1_555 yes C(6) S(5) C(8) C(9) 4.4(8) 1_555 1_555 1_555 1_555 yes C(6) S(6) C(9) C(8) -4.9(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) S(7) C(10) 170.9(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) S(8) C(11) -171.2(7) 1_555 1_555 1_555 1_555 yes C(7) S(7) C(10) C(11) 4.9(7) 1_555 1_555 1_555 1_555 yes C(7) S(8) C(11) C(10) -4.1(8) 1_555 1_555 1_555 1_555 yes C(7) C(6) S(5) C(8) 170.6(7) 1_555 1_555 1_555 1_555 yes C(7) C(6) S(6) C(9) -170.4(7) 1_555 1_555 1_555 1_555 yes C(8) S(9) C(12) C(13) -58.7(9) 1_555 1_555 1_555 1_555 yes C(8) C(9) S(10) C(13) -7.1(10) 1_555 1_555 1_555 1_555 yes C(9) S(10) C(13) C(12) -24(1) 1_555 1_555 1_555 1_555 yes C(9) C(8) S(9) C(12) 26.7(9) 1_555 1_555 1_555 1_555 yes C(10) S(11) C(14A) C(14B) -95(2) 1_555 1_555 1_555 1_555 yes C(10) S(11) C(14A) C(15A) -56(1) 1_555 1_555 1_555 1_555 yes C(10) S(11) C(14A) C(15B) -18(1) 1_555 1_555 1_555 1_555 yes C(10) S(11) C(14B) C(14A) 88(2) 1_555 1_555 1_555 1_555 yes C(10) S(11) C(14B) C(15A) -10(2) 1_555 1_555 1_555 1_555 yes C(10) S(11) C(14B) C(15B) 30(1) 1_555 1_555 1_555 1_555 yes C(10) C(11) S(12) C(15A) 1(1) 1_555 1_555 1_555 1_555 yes C(10) C(11) S(12) C(15B) -27(1) 1_555 1_555 1_555 1_555 yes C(11) S(12) C(15A) C(14A) -33(1) 1_555 1_555 1_555 1_555 yes C(11) S(12) C(15A) C(14B) -7(2) 1_555 1_555 1_555 1_555 yes C(11) S(12) C(15A) C(15B) -84(1) 1_555 1_555 1_555 1_555 yes C(11) S(12) C(15B) C(14A) 33(1) 1_555 1_555 1_555 1_555 yes C(11) S(12) C(15B) C(14B) 59(1) 1_555 1_555 1_555 1_555 yes C(11) S(12) C(15B) C(15A) 101(1) 1_555 1_555 1_555 1_555 yes C(11) C(10) S(11) C(14A) 25(1) 1_555 1_555 1_555 1_555 yes C(11) C(10) S(11) C(14B) 3(1) 1_555 1_555 1_555 1_555 yes C(14A) S(11) C(14B) C(15A) -99(3) 1_555 1_555 1_555 1_555 yes C(14A) S(11) C(14B) C(15B) -57(2) 1_555 1_555 1_555 1_555 yes C(14A) C(14B) C(15A) C(15B) -3(3) 1_555 1_555 1_555 1_555 yes C(14A) C(14B) C(15B) C(15A) 176(3) 1_555 1_555 1_555 1_555 yes C(14A) C(15A) S(12) C(15B) 51(1) 1_555 1_555 1_555 1_555 yes C(14A) C(15A) C(14B) C(15B) 3(3) 1_555 1_555 1_555 1_555 yes C(14A) C(15A) C(15B) C(14B) -1(1) 1_555 1_555 1_555 1_555 yes C(14A) C(15B) S(12) C(15A) -67(2) 1_555 1_555 1_555 1_555 yes C(14A) C(15B) C(14B) C(15A) -176(3) 1_555 1_555 1_555 1_555 yes C(14A) C(15B) C(15A) C(14B) 1(1) 1_555 1_555 1_555 1_555 yes C(14B) S(11) C(14A) C(15A) 39(2) 1_555 1_555 1_555 1_555 yes C(14B) S(11) C(14A) C(15B) 77(2) 1_555 1_555 1_555 1_555 yes C(14B) C(14A) C(15A) C(15B) 175(4) 1_555 1_555 1_555 1_555 yes C(14B) C(14A) C(15B) C(15A) -3(3) 1_555 1_555 1_555 1_555 yes C(14B) C(15A) S(12) C(15B) 77(2) 1_555 1_555 1_555 1_555 yes C(14B) C(15A) C(14A) C(15B) -175(4) 1_555 1_555 1_555 1_555 yes C(14B) C(15B) S(12) C(15A) -41(1) 1_555 1_555 1_555 1_555 yes C(14B) C(15B) C(14A) C(15A) 3(3) 1_555 1_555 1_555 1_555 yes C(15A) C(14A) C(14B) C(15B) -2(2) 1_555 1_555 1_555 1_555 yes C(15A) C(14B) C(14A) C(15B) 2(2) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(19) C(20) -106(31) 1_555 1_555 1_555 1_555 yes C(16) C(18) C(17) C(19) 179.4(9) 1_555 2_657 2_657 2_657 yes C(18) C(16) C(17) C(19) -179.6(9) 1_555 2_657 2_657 2_657 yes C(18) C(17) C(19) C(20) 77(31) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 I(1) Br(1) 3.2650(6) . . ? S(3) S(10) 3.526(4) . 1_554 ? S(3) S(11) 3.592(4) . 2_665 ? S(4) S(12) 3.491(4) . 2_766 ? S(4) S(9) 3.591(4) . 1_655 ? S(9) C(14A) 3.54(2) . 2_665 ? S(9) S(11) 3.539(4) . 2_665 ? S(10) S(12) 3.522(4) . 2_766 ? C(2) C(15B) 3.46(2) . 2_765 ? C(3) C(15B) 3.52(2) . 2_765 ? C(4) C(9) 3.54(1) . . ? C(4) C(8) 3.55(1) . . ? C(10) C(12) 3.56(1) . 2_666 ? C(11) C(12) 3.58(1) . 2_666 ? C(14B) C(16) 3.28(2) . 2_666 ? #------------------------------------------------------------------------------ #===END data_General _audit_creation_date 'Thu Oct 7 00:42:09 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Hiroshi M. Yamamoto' _publ_contact_author_address ; Hirosawa, Wako-shi, Saitama 351-0198 (Japan) ; _publ_contact_author_email ' yhiroshi@postman.riken.go.jp ' _publ_contact_author_fax ' +81-(0)48-462-4611 ' _publ_contact_author_phone ' +81-(0)48-467-9410 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' ' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # _publ_section_title ; Structural and physical properties of conducting cation radical satls containing supramolecular assmblies based on pBIB derivatives (pBIB=p-Bis(iodoethynyl)benzene) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_ET3Br.TFBIB #------------------------------------------------------------------------------ _audit_creation_date 'Fri Dec 25 06:57:19 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MXC Diffractometer Control' _computing_cell_refinement 'MXC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1683.78 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H24 Br F4 I2 S24 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 13.180(1) _cell_length_b 19.128(2) _cell_length_c 12.4640(6) _cell_angle_alpha 105.250(4) _cell_angle_beta 112.817(5) _cell_angle_gamma 82.455(4) _cell_volume 2792.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'rod' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1650.00 _exptl_absorpt_coefficient_mu 2.789 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Science rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Mac Sciecne DIP320' _diffrn_measurement_method _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l _diffrn_reflns_number 23512 _reflns_number_total 10750 _reflns_number_observed 6618 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _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 80 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 48 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; F 0 8 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; I 0 4 -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br 0 2 -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags I(1) 0.66614(3) 0.52821(2) 0.51763(3) 0.0400(1) Uani d . 1.00 . I(2) 0.33722(3) 0.47548(2) -0.01667(3) 0.0405(1) Uani d . 1.00 . Br(1) 0.49766(5) 0.50154(3) 0.25239(4) 0.0529(2) Uani d . 1.00 . S(1) 0.6818(1) 0.13512(7) 0.4792(1) 0.0455(4) Uani d . 1.00 . S(2) 0.8562(1) 0.12770(7) 0.7118(1) 0.0476(4) Uani d . 1.00 . S(3) 0.7534(1) -0.02781(7) 0.3659(1) 0.0477(4) Uani d . 1.00 . S(4) 0.9338(1) -0.03042(7) 0.5961(1) 0.0489(4) Uani d . 1.00 . S(5) 0.6293(1) 0.29156(7) 0.5503(1) 0.0469(4) Uani d . 1.00 . S(6) 0.8338(1) 0.28003(7) 0.8300(1) 0.0464(4) Uani d . 1.00 . S(7) 0.7997(1) -0.17382(7) 0.2422(1) 0.0537(4) Uani d . 1.00 . S(8) 1.0158(1) -0.17786(8) 0.5165(1) 0.0672(5) Uani d . 1.00 . S(9) 0.8425(1) -0.00934(7) 0.8709(1) 0.0546(5) Uani d . 1.00 . S(10) 0.8356(1) -0.05559(7) 1.0755(1) 0.0496(4) Uani d . 1.00 . S(11) 0.7718(1) 0.15357(7) 0.9782(1) 0.0460(4) Uani d . 1.00 . S(12) 0.7677(1) 0.10834(7) 1.1847(1) 0.0489(4) Uani d . 1.00 . S(13) 0.9162(1) -0.15136(8) 0.7592(1) 0.0635(5) Uani d . 1.00 . S(14) 0.9096(1) -0.20608(7) 1.0039(1) 0.0508(4) Uani d . 1.00 . S(15) 0.7369(1) 0.31040(7) 1.0727(1) 0.0491(4) Uani d . 1.00 . S(16) 0.7330(1) 0.25376(8) 1.3178(1) 0.0602(5) Uani d . 1.00 . S(17) 0.4441(1) -0.07759(7) 0.3270(1) 0.0447(4) Uani d . 1.00 . S(18) 0.6226(1) -0.08520(7) 0.5564(1) 0.0443(4) Uani d . 1.00 . S(19) 0.4750(1) -0.22627(7) 0.2015(1) 0.0480(4) Uani d . 1.00 . S(20) 0.6883(1) -0.23807(7) 0.4753(1) 0.0476(4) Uani d . 1.00 . S(21) 0.5288(1) -0.06001(7) 0.8387(1) 0.0482(4) Uani d . 1.00 . S(22) 0.5334(1) -0.10468(7) 1.0493(1) 0.0462(4) Uani d . 1.00 . S(23) 0.5836(1) -0.20375(7) 0.7154(1) 0.0484(4) Uani d . 1.00 . S(24) 0.5932(1) -0.25848(7) 0.9679(1) 0.0519(4) Uani d . 1.00 . F(1) 0.8768(2) 0.6251(1) 1.0086(2) 0.0495(9) Uani d . 1.00 . F(2) 0.9814(2) 0.4073(2) 0.7891(2) 0.0497(9) Uani d . 1.00 . F(3) 0.0246(2) 0.5982(2) -0.2919(2) 0.0562(10) Uani d . 1.00 . F(4) 0.1184(2) 0.3731(2) -0.5030(2) 0.0570(10) Uani d . 1.00 . C(1) 0.8215(4) 0.0170(2) 0.5134(4) 0.037(1) Uani d . 1.00 . C(2) 0.7901(4) 0.0850(2) 0.5613(4) 0.035(1) Uani d . 1.00 . C(3) 0.8380(4) -0.1062(2) 0.3763(4) 0.039(1) Uani d . 1.00 . C(4) 0.9183(4) -0.1084(3) 0.4794(4) 0.041(2) Uani d . 1.00 . C(5) 0.7097(4) 0.2156(2) 0.5913(4) 0.036(1) Uani d . 1.00 . C(6) 0.7872(4) 0.2118(2) 0.6973(4) 0.035(1) Uani d . 1.00 . C(7) 0.8980(6) -0.2439(4) 0.2847(6) 0.112(3) Uani d . 1.00 . C(8) 0.9660(7) -0.2475(4) 0.3948(6) 0.132(3) Uani d . 1.00 . C(9) 0.7038(4) 0.3628(3) 0.6695(4) 0.044(2) Uani d . 1.00 . C(10) 0.7301(4) 0.3502(2) 0.7929(4) 0.043(2) Uani d . 1.00 . C(11) 0.8205(4) 0.0155(2) 1.0055(4) 0.039(1) Uani d . 1.00 . C(12) 0.7912(4) 0.0839(2) 1.0520(4) 0.036(1) Uani d . 1.00 . C(13) 0.8795(4) -0.0992(2) 0.8778(4) 0.041(2) Uani d . 1.00 . C(14) 0.8792(4) -0.1205(2) 0.9716(4) 0.036(1) Uani d . 1.00 . C(15) 0.7521(4) 0.2223(2) 1.0955(4) 0.039(1) Uani d . 1.00 . C(16) 0.7538(4) 0.2017(3) 1.1910(4) 0.040(1) Uani d . 1.00 . C(17) 0.8979(5) -0.2403(3) 0.7685(4) 0.059(2) Uani d . 1.00 . C(18) 0.9559(5) -0.2565(3) 0.8872(5) 0.059(2) Uani d . 1.00 . C(19) 0.6777(5) 0.3558(3) 1.1814(5) 0.065(2) Uani d . 1.00 . C(20) 0.7360(6) 0.3440(3) 1.3024(5) 0.072(2) Uani d . 1.00 . C(21) 0.5135(4) -0.0346(2) 0.4746(4) 0.034(1) Uani d . 1.00 . C(22) 0.5200(4) -0.1596(2) 0.3367(4) 0.037(1) Uani d . 1.00 . C(23) 0.6000(4) -0.1637(2) 0.4409(4) 0.033(1) Uani d . 1.00 . C(24) 0.5803(4) -0.2962(3) 0.2335(4) 0.050(2) Uani d . 1.00 . C(25) 0.6168(5) -0.3104(3) 0.3552(4) 0.050(2) Uani d . 1.00 . C(26) 0.5129(4) -0.0348(2) 0.9751(4) 0.038(1) Uani d . 1.00 . C(27) 0.5586(4) -0.1515(2) 0.8404(4) 0.037(1) Uani d . 1.00 . C(28) 0.5638(4) -0.1721(2) 0.9373(4) 0.036(1) Uani d . 1.00 . C(29) 0.5743(4) -0.2937(3) 0.7301(4) 0.047(2) Uani d . 1.00 . C(30) 0.6392(4) -0.3075(3) 0.8495(5) 0.049(2) Uani d . 1.00 . C(31) 0.7787(4) 0.5349(3) 0.6845(4) 0.041(2) Uani d . 1.00 . C(32) 0.8455(4) 0.5308(3) 0.7815(5) 0.041(2) Uani d . 1.00 . C(33) 0.9244(4) 0.5170(3) 0.8926(4) 0.034(1) Uani d . 1.00 . C(34) 0.9371(4) 0.5630(2) 1.0018(4) 0.034(1) Uani d . 1.00 . C(35) 0.9908(4) 0.4532(3) 0.8935(4) 0.035(1) Uani d . 1.00 . C(36) 0.2246(4) 0.4692(3) -0.1846(4) 0.042(2) Uani d . 1.00 . C(37) 0.1569(4) 0.4735(3) -0.2813(5) 0.044(2) Uani d . 1.00 . C(38) 0.0772(4) 0.4853(3) -0.3904(4) 0.035(1) Uani d . 1.00 . C(39) 0.0131(4) 0.5487(3) -0.3937(4) 0.038(2) Uani d . 1.00 . C(40) 0.0607(4) 0.4365(3) -0.4997(5) 0.039(2) Uani d . 1.00 . H(1) 0.8584 -0.2878 0.2530 0.1283 Uiso calc . 1.00 . H(2) 0.9465 -0.2469 0.2417 0.1283 Uiso calc . 1.00 . H(3) 1.0309 -0.2743 0.3856 0.1555 Uiso calc . 1.00 . H(4) 0.9300 -0.2777 0.4188 0.1555 Uiso calc . 1.00 . H(5) 0.7742 0.3669 0.6620 0.0525 Uiso calc . 1.00 . H(6) 0.6647 0.4081 0.6621 0.0525 Uiso calc . 1.00 . H(7) 0.6621 0.3368 0.7942 0.0504 Uiso calc . 1.00 . H(8) 0.7521 0.3945 0.8520 0.0504 Uiso calc . 1.00 . H(9) 0.8201 -0.2461 0.7474 0.0716 Uiso calc . 1.00 . H(10) 0.9204 -0.2753 0.7107 0.0716 Uiso calc . 1.00 . H(11) 1.0331 -0.2465 0.9116 0.0719 Uiso calc . 1.00 . H(12) 0.9519 -0.3071 0.8808 0.0719 Uiso calc . 1.00 . H(13) 0.6694 0.4067 1.1847 0.0756 Uiso calc . 1.00 . H(14) 0.6026 0.3385 1.1542 0.0756 Uiso calc . 1.00 . H(15) 0.7083 0.3775 1.3565 0.0862 Uiso calc . 1.00 . H(16) 0.8122 0.3553 1.3240 0.0862 Uiso calc . 1.00 . H(17) 0.5573 -0.3399 0.1750 0.0580 Uiso calc . 1.00 . H(18) 0.6461 -0.2816 0.2280 0.0580 Uiso calc . 1.00 . H(19) 0.6602 -0.3541 0.3583 0.0616 Uiso calc . 1.00 . H(20) 0.5495 -0.3187 0.3656 0.0616 Uiso calc . 1.00 . H(21) 0.4976 -0.3008 0.7152 0.0585 Uiso calc . 1.00 . H(22) 0.5938 -0.3284 0.6709 0.0585 Uiso calc . 1.00 . H(23) 0.7143 -0.2937 0.8688 0.0598 Uiso calc . 1.00 . H(24) 0.6421 -0.3582 0.8441 0.0598 Uiso calc . 1.00 . 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 I(1) 0.0426(2) 0.0387(2) 0.0299(2) 0.0033(1) 0.0040(2) 0.0100(1) I(2) 0.0399(2) 0.0430(2) 0.0302(2) 0.0019(1) 0.0045(2) 0.0089(1) Br(1) 0.0496(3) 0.0576(3) 0.0317(4) 0.0128(2) 0.0030(3) 0.0025(2) S(1) 0.0513(9) 0.0320(7) 0.0412(9) 0.0043(6) 0.0093(7) 0.0028(5) S(2) 0.0622(10) 0.0303(7) 0.0418(9) 0.0088(6) 0.0141(7) 0.0069(5) S(3) 0.0539(9) 0.0350(7) 0.0411(9) 0.0095(6) 0.0100(7) 0.0036(6) S(4) 0.0582(9) 0.0357(7) 0.0396(9) 0.0076(6) 0.0098(7) 0.0034(6) S(5) 0.0537(9) 0.0365(7) 0.0398(8) 0.0131(6) 0.0121(7) 0.0057(6) S(6) 0.0533(9) 0.0362(7) 0.0383(8) 0.0083(6) 0.0122(7) 0.0014(5) S(7) 0.066(1) 0.0375(7) 0.0459(9) 0.0037(7) 0.0164(7) -0.0013(6) S(8) 0.066(1) 0.0496(9) 0.061(1) 0.0253(8) 0.0096(8) 0.0049(7) S(9) 0.091(1) 0.0309(7) 0.0491(9) 0.0106(7) 0.0366(8) 0.0106(6) S(10) 0.075(1) 0.0329(7) 0.0484(9) 0.0103(6) 0.0337(7) 0.0099(6) S(11) 0.0669(10) 0.0281(6) 0.0438(8) 0.0061(6) 0.0259(7) 0.0042(5) S(12) 0.0668(10) 0.0365(7) 0.0506(9) 0.0068(6) 0.0314(7) 0.0105(6) S(13) 0.108(1) 0.0408(8) 0.0565(9) 0.0104(8) 0.0515(8) 0.0090(6) S(14) 0.072(1) 0.0321(7) 0.0533(9) 0.0116(6) 0.0305(7) 0.0122(6) S(15) 0.0659(10) 0.0293(6) 0.0559(9) 0.0061(6) 0.0307(7) 0.0065(6) S(16) 0.084(1) 0.0510(9) 0.0474(9) 0.0264(8) 0.0354(8) 0.0107(7) S(17) 0.0537(9) 0.0294(6) 0.0406(8) 0.0081(6) 0.0106(7) 0.0052(5) S(18) 0.0525(9) 0.0313(6) 0.0379(8) 0.0027(6) 0.0092(7) 0.0025(5) S(19) 0.0564(9) 0.0337(7) 0.0409(9) 0.0058(6) 0.0098(7) 0.0030(6) S(20) 0.0514(9) 0.0396(7) 0.0388(9) 0.0138(6) 0.0090(7) 0.0065(6) S(21) 0.075(1) 0.0312(7) 0.0439(8) 0.0089(6) 0.0284(7) 0.0112(5) S(22) 0.0689(10) 0.0311(6) 0.0409(8) 0.0082(6) 0.0258(7) 0.0078(5) S(23) 0.0700(10) 0.0377(7) 0.0427(8) 0.0107(6) 0.0296(7) 0.0097(6) S(24) 0.085(1) 0.0290(7) 0.0429(8) 0.0060(7) 0.0267(7) 0.0088(5) F(1) 0.049(2) 0.038(2) 0.046(2) 0.010(1) 0.006(1) 0.009(1) F(2) 0.052(2) 0.048(2) 0.041(2) 0.002(1) 0.013(1) 0.002(1) F(3) 0.056(2) 0.056(2) 0.036(2) 0.002(2) 0.010(1) -0.009(1) F(4) 0.054(2) 0.042(2) 0.054(2) 0.013(1) 0.006(2) 0.004(1) C(1) 0.043(3) 0.031(3) 0.036(3) 0.002(2) 0.014(2) 0.010(2) C(2) 0.043(3) 0.031(3) 0.024(3) -0.002(2) 0.009(2) 0.003(2) C(3) 0.051(3) 0.027(2) 0.039(3) 0.008(2) 0.020(3) 0.005(2) C(4) 0.048(3) 0.033(3) 0.034(3) 0.010(2) 0.012(3) 0.004(2) C(5) 0.049(3) 0.028(2) 0.031(3) 0.008(2) 0.017(2) 0.008(2) C(6) 0.048(3) 0.028(2) 0.030(3) 0.005(2) 0.020(2) 0.002(2) C(7) 0.117(6) 0.056(4) 0.089(6) 0.043(4) -0.001(5) -0.022(4) C(8) 0.192(9) 0.069(5) 0.046(5) 0.060(5) -0.020(5) -0.004(4) C(9) 0.051(3) 0.035(3) 0.043(3) 0.002(2) 0.016(3) 0.010(2) C(10) 0.042(3) 0.029(3) 0.053(3) 0.005(2) 0.020(3) -0.001(2) C(11) 0.046(3) 0.027(2) 0.048(3) 0.002(2) 0.025(2) 0.005(2) C(12) 0.040(3) 0.028(2) 0.037(3) 0.001(2) 0.014(2) 0.003(2) C(13) 0.053(3) 0.031(3) 0.040(3) 0.006(2) 0.020(3) 0.007(2) C(14) 0.037(3) 0.026(2) 0.039(3) 0.005(2) 0.012(2) 0.003(2) C(15) 0.042(3) 0.024(2) 0.043(3) 0.007(2) 0.014(3) 0.002(2) C(16) 0.046(3) 0.033(3) 0.035(3) 0.008(2) 0.015(2) 0.005(2) C(17) 0.088(5) 0.039(3) 0.035(4) 0.011(3) 0.011(3) 0.006(2) C(18) 0.067(4) 0.036(3) 0.085(4) 0.013(3) 0.045(3) 0.011(3) C(19) 0.091(5) 0.032(3) 0.095(4) 0.016(3) 0.065(3) 0.013(3) C(20) 0.111(5) 0.057(4) 0.053(4) -0.026(4) 0.048(3) -0.017(3) C(21) 0.042(3) 0.029(2) 0.032(3) 0.000(2) 0.015(2) 0.007(2) C(22) 0.049(3) 0.026(2) 0.041(3) 0.003(2) 0.025(2) 0.005(2) C(23) 0.037(3) 0.033(2) 0.023(3) 0.003(2) 0.006(2) 0.007(2) C(24) 0.064(4) 0.033(3) 0.051(3) 0.010(3) 0.026(3) 0.005(2) C(25) 0.062(4) 0.031(3) 0.053(4) 0.005(2) 0.018(3) 0.012(2) C(26) 0.040(3) 0.027(2) 0.045(3) 0.000(2) 0.018(2) 0.005(2) C(27) 0.047(3) 0.026(2) 0.039(3) 0.006(2) 0.018(2) 0.008(2) C(28) 0.040(3) 0.027(2) 0.033(3) 0.005(2) 0.007(2) 0.006(2) C(29) 0.061(4) 0.033(3) 0.039(3) 0.005(2) 0.014(3) 0.002(2) C(30) 0.055(4) 0.035(3) 0.058(4) 0.011(2) 0.023(3) 0.013(2) C(31) 0.047(3) 0.042(3) 0.022(3) 0.003(2) -0.003(3) 0.012(2) C(32) 0.040(3) 0.031(3) 0.053(4) -0.001(2) 0.017(3) 0.010(2) C(33) 0.032(3) 0.037(3) 0.032(3) -0.001(2) 0.004(2) 0.015(2) C(34) 0.030(3) 0.035(3) 0.027(3) 0.002(2) 0.000(2) 0.008(2) C(35) 0.038(3) 0.035(3) 0.028(3) -0.005(2) 0.010(2) 0.000(2) C(36) 0.041(3) 0.048(3) 0.030(3) -0.001(2) 0.006(3) 0.009(2) C(37) 0.043(3) 0.044(3) 0.041(4) -0.004(2) 0.011(3) 0.011(2) C(38) 0.024(3) 0.049(3) 0.025(3) -0.003(2) -0.002(2) 0.013(2) C(39) 0.029(3) 0.044(3) 0.034(3) -0.004(2) 0.006(2) 0.003(2) C(40) 0.029(3) 0.038(3) 0.040(3) 0.000(2) 0.006(2) 0.004(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6618 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0383 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0421 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.157 _refine_ls_shift/esd_max 2.4362 _refine_ls_shift/esd_mean 0.0180 _refine_diff_density_min -0.64 _refine_diff_density_max 1.07 _atoms_sites_solution_primary 'direct methods' _atoms_sites_solution_secondary 'Fourier difference' #------------------------------------------------------------------------------ _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 I(1) C(31) 2.015(5) 1_555 1_555 yes I(2) C(36) 2.026(5) 1_555 1_555 yes S(1) C(2) 1.741(5) 1_555 1_555 yes S(1) C(5) 1.754(4) 1_555 1_555 yes S(2) C(2) 1.748(4) 1_555 1_555 yes S(2) C(6) 1.757(4) 1_555 1_555 yes S(3) C(1) 1.736(5) 1_555 1_555 yes S(3) C(3) 1.750(5) 1_555 1_555 yes S(4) C(1) 1.740(5) 1_555 1_555 yes S(4) C(4) 1.758(4) 1_555 1_555 yes S(5) C(5) 1.749(4) 1_555 1_555 yes S(5) C(9) 1.784(5) 1_555 1_555 yes S(6) C(6) 1.762(4) 1_555 1_555 yes S(6) C(10) 1.799(5) 1_555 1_555 yes S(7) C(3) 1.760(4) 1_555 1_555 yes S(7) C(7) 1.772(6) 1_555 1_555 yes S(8) C(4) 1.745(5) 1_555 1_555 yes S(8) C(8) 1.702(7) 1_555 1_555 yes S(9) C(11) 1.745(5) 1_555 1_555 yes S(9) C(13) 1.740(5) 1_555 1_555 yes S(10) C(11) 1.751(5) 1_555 1_555 yes S(10) C(14) 1.759(4) 1_555 1_555 yes S(11) C(12) 1.750(5) 1_555 1_555 yes S(11) C(15) 1.768(4) 1_555 1_555 yes S(12) C(12) 1.732(5) 1_555 1_555 yes S(12) C(16) 1.754(5) 1_555 1_555 yes S(13) C(13) 1.752(5) 1_555 1_555 yes S(13) C(17) 1.789(6) 1_555 1_555 yes S(14) C(14) 1.748(5) 1_555 1_555 yes S(14) C(18) 1.792(5) 1_555 1_555 yes S(15) C(15) 1.755(5) 1_555 1_555 yes S(15) C(19) 1.794(6) 1_555 1_555 yes S(16) C(16) 1.732(5) 1_555 1_555 yes S(16) C(20) 1.793(6) 1_555 1_555 yes S(17) C(21) 1.730(4) 1_555 1_555 yes S(17) C(22) 1.753(4) 1_555 1_555 yes S(18) C(21) 1.749(5) 1_555 1_555 yes S(18) C(23) 1.750(4) 1_555 1_555 yes S(19) C(22) 1.764(4) 1_555 1_555 yes S(19) C(24) 1.799(5) 1_555 1_555 yes S(20) C(23) 1.750(4) 1_555 1_555 yes S(20) C(25) 1.788(5) 1_555 1_555 yes S(21) C(26) 1.728(5) 1_555 1_555 yes S(21) C(27) 1.747(4) 1_555 1_555 yes S(22) C(26) 1.755(5) 1_555 1_555 yes S(22) C(28) 1.768(4) 1_555 1_555 yes S(23) C(27) 1.740(4) 1_555 1_555 yes S(23) C(29) 1.801(5) 1_555 1_555 yes S(24) C(28) 1.753(5) 1_555 1_555 yes S(24) C(30) 1.801(5) 1_555 1_555 yes F(1) C(34) 1.341(5) 1_555 1_555 yes F(2) C(35) 1.335(5) 1_555 1_555 yes F(3) C(39) 1.337(5) 1_555 1_555 yes F(4) C(40) 1.344(5) 1_555 1_555 yes C(1) C(2) 1.365(6) 1_555 1_555 yes C(3) C(4) 1.317(6) 1_555 1_555 yes C(5) C(6) 1.333(6) 1_555 1_555 yes C(7) C(8) 1.331(8) 1_555 1_555 yes C(9) C(10) 1.517(7) 1_555 1_555 yes C(11) C(12) 1.357(6) 1_555 1_555 yes C(13) C(14) 1.336(6) 1_555 1_555 yes C(15) C(16) 1.341(6) 1_555 1_555 yes C(17) C(18) 1.473(7) 1_555 1_555 yes C(19) C(20) 1.467(8) 1_555 1_555 yes C(21) C(21) 1.375(8) 1_555 2_656 yes C(22) C(23) 1.332(6) 1_555 1_555 yes C(24) C(25) 1.491(7) 1_555 1_555 yes C(26) C(26) 1.372(8) 1_555 2_657 yes C(27) C(28) 1.340(6) 1_555 1_555 yes C(29) C(30) 1.475(7) 1_555 1_555 yes C(31) C(32) 1.204(6) 1_555 1_555 yes C(32) C(33) 1.439(7) 1_555 1_555 yes C(33) C(34) 1.374(6) 1_555 1_555 yes C(33) C(35) 1.405(6) 1_555 1_555 yes C(34) C(35) 1.370(6) 1_555 2_767 yes C(36) C(37) 1.206(6) 1_555 1_555 yes C(37) C(38) 1.412(6) 1_555 1_555 yes C(38) C(39) 1.384(6) 1_555 1_555 yes C(38) C(40) 1.390(6) 1_555 1_555 yes C(39) C(40) 1.384(6) 1_555 2_564 yes #------------------------------------------------------------------------------ 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(2) S(1) C(5) 94.9(2) 1_555 1_555 1_555 yes C(2) S(2) C(6) 94.4(2) 1_555 1_555 1_555 yes C(1) S(3) C(3) 94.5(2) 1_555 1_555 1_555 yes C(1) S(4) C(4) 94.9(2) 1_555 1_555 1_555 yes C(5) S(5) C(9) 101.0(2) 1_555 1_555 1_555 yes C(6) S(6) C(10) 100.6(2) 1_555 1_555 1_555 yes C(3) S(7) C(7) 101.0(3) 1_555 1_555 1_555 yes C(4) S(8) C(8) 102.1(3) 1_555 1_555 1_555 yes C(11) S(9) C(13) 95.2(2) 1_555 1_555 1_555 yes C(11) S(10) C(14) 94.9(2) 1_555 1_555 1_555 yes C(12) S(11) C(15) 94.5(2) 1_555 1_555 1_555 yes C(12) S(12) C(16) 95.3(2) 1_555 1_555 1_555 yes C(13) S(13) C(17) 99.9(3) 1_555 1_555 1_555 yes C(14) S(14) C(18) 102.2(2) 1_555 1_555 1_555 yes C(15) S(15) C(19) 99.6(2) 1_555 1_555 1_555 yes C(16) S(16) C(20) 101.8(3) 1_555 1_555 1_555 yes C(21) S(17) C(22) 94.8(2) 1_555 1_555 1_555 yes C(21) S(18) C(23) 95.0(2) 1_555 1_555 1_555 yes C(22) S(19) C(24) 101.2(2) 1_555 1_555 1_555 yes C(23) S(20) C(25) 101.5(2) 1_555 1_555 1_555 yes C(26) S(21) C(27) 95.6(2) 1_555 1_555 1_555 yes C(26) S(22) C(28) 94.6(2) 1_555 1_555 1_555 yes C(27) S(23) C(29) 100.6(2) 1_555 1_555 1_555 yes C(28) S(24) C(30) 101.4(2) 1_555 1_555 1_555 yes S(3) C(1) S(4) 115.5(3) 1_555 1_555 1_555 yes S(3) C(1) C(2) 122.5(4) 1_555 1_555 1_555 yes S(4) C(1) C(2) 122.1(4) 1_555 1_555 1_555 yes S(1) C(2) S(2) 115.1(2) 1_555 1_555 1_555 yes S(1) C(2) C(1) 123.1(3) 1_555 1_555 1_555 yes S(2) C(2) C(1) 121.8(4) 1_555 1_555 1_555 yes S(3) C(3) S(7) 113.0(3) 1_555 1_555 1_555 yes S(3) C(3) C(4) 118.3(3) 1_555 1_555 1_555 yes S(7) C(3) C(4) 128.7(4) 1_555 1_555 1_555 yes S(4) C(4) S(8) 114.4(3) 1_555 1_555 1_555 yes S(4) C(4) C(3) 116.8(4) 1_555 1_555 1_555 yes S(8) C(4) C(3) 128.8(4) 1_555 1_555 1_555 yes S(1) C(5) S(5) 115.2(3) 1_555 1_555 1_555 yes S(1) C(5) C(6) 117.0(3) 1_555 1_555 1_555 yes S(5) C(5) C(6) 127.8(3) 1_555 1_555 1_555 yes S(2) C(6) S(6) 112.9(3) 1_555 1_555 1_555 yes S(2) C(6) C(5) 117.6(3) 1_555 1_555 1_555 yes S(6) C(6) C(5) 129.5(4) 1_555 1_555 1_555 yes S(7) C(7) C(8) 127.3(5) 1_555 1_555 1_555 yes S(7) C(7) H(1) 106.1(5) 1_555 1_555 1_555 no S(7) C(7) H(2) 105.4(6) 1_555 1_555 1_555 no C(8) C(7) H(1) 105.3(8) 1_555 1_555 1_555 no C(8) C(7) H(2) 104.1(7) 1_555 1_555 1_555 no H(1) C(7) H(2) 107.3(6) 1_555 1_555 1_555 no S(8) C(8) C(7) 128.1(6) 1_555 1_555 1_555 yes S(8) C(8) H(3) 104.8(6) 1_555 1_555 1_555 no S(8) C(8) H(4) 105.3(6) 1_555 1_555 1_555 no C(7) C(8) H(3) 105.5(7) 1_555 1_555 1_555 no C(7) C(8) H(4) 104.7(8) 1_555 1_555 1_555 no H(3) C(8) H(4) 107.1(7) 1_555 1_555 1_555 no S(5) C(9) C(10) 113.7(4) 1_555 1_555 1_555 yes S(5) C(9) H(5) 108.6(4) 1_555 1_555 1_555 no S(5) C(9) H(6) 110.0(4) 1_555 1_555 1_555 no C(10) C(9) H(5) 107.4(4) 1_555 1_555 1_555 no C(10) C(9) H(6) 110.6(4) 1_555 1_555 1_555 no H(5) C(9) H(6) 106.2(5) 1_555 1_555 1_555 no S(6) C(10) C(9) 113.8(3) 1_555 1_555 1_555 yes S(6) C(10) H(7) 109.2(4) 1_555 1_555 1_555 no S(6) C(10) H(8) 109.9(4) 1_555 1_555 1_555 no C(9) C(10) H(7) 106.9(4) 1_555 1_555 1_555 no C(9) C(10) H(8) 109.7(5) 1_555 1_555 1_555 no H(7) C(10) H(8) 107.1(5) 1_555 1_555 1_555 no S(9) C(11) S(10) 114.9(3) 1_555 1_555 1_555 yes S(9) C(11) C(12) 123.3(4) 1_555 1_555 1_555 yes S(10) C(11) C(12) 121.9(4) 1_555 1_555 1_555 yes S(11) C(12) S(12) 115.5(2) 1_555 1_555 1_555 yes S(11) C(12) C(11) 121.2(4) 1_555 1_555 1_555 yes S(12) C(12) C(11) 123.3(4) 1_555 1_555 1_555 yes S(9) C(13) S(13) 114.6(3) 1_555 1_555 1_555 yes S(9) C(13) C(14) 117.9(4) 1_555 1_555 1_555 yes S(13) C(13) C(14) 127.5(4) 1_555 1_555 1_555 yes S(10) C(14) S(14) 113.7(3) 1_555 1_555 1_555 yes S(10) C(14) C(13) 116.8(3) 1_555 1_555 1_555 yes S(14) C(14) C(13) 129.4(4) 1_555 1_555 1_555 yes S(11) C(15) S(15) 114.7(3) 1_555 1_555 1_555 yes S(11) C(15) C(16) 117.1(3) 1_555 1_555 1_555 yes S(15) C(15) C(16) 128.2(4) 1_555 1_555 1_555 yes S(12) C(16) S(16) 113.7(3) 1_555 1_555 1_555 yes S(12) C(16) C(15) 117.0(3) 1_555 1_555 1_555 yes S(16) C(16) C(15) 129.1(4) 1_555 1_555 1_555 yes S(13) C(17) C(18) 115.3(4) 1_555 1_555 1_555 yes S(13) C(17) H(9) 108.3(4) 1_555 1_555 1_555 no S(13) C(17) H(10) 109.0(5) 1_555 1_555 1_555 no C(18) C(17) H(9) 107.1(5) 1_555 1_555 1_555 no C(18) C(17) H(10) 109.3(5) 1_555 1_555 1_555 no H(9) C(17) H(10) 107.4(5) 1_555 1_555 1_555 no S(14) C(18) C(17) 116.4(4) 1_555 1_555 1_555 yes S(14) C(18) H(11) 107.8(4) 1_555 1_555 1_555 no S(14) C(18) H(12) 108.6(4) 1_555 1_555 1_555 no C(17) C(18) H(11) 107.2(5) 1_555 1_555 1_555 no C(17) C(18) H(12) 109.4(5) 1_555 1_555 1_555 no H(11) C(18) H(12) 107.0(5) 1_555 1_555 1_555 no S(15) C(19) C(20) 115.9(4) 1_555 1_555 1_555 yes S(15) C(19) H(13) 110.0(4) 1_555 1_555 1_555 no S(15) C(19) H(14) 108.5(4) 1_555 1_555 1_555 no C(20) C(19) H(13) 109.7(5) 1_555 1_555 1_555 no C(20) C(19) H(14) 106.5(5) 1_555 1_555 1_555 no H(13) C(19) H(14) 105.8(5) 1_555 1_555 1_555 no S(16) C(20) C(19) 115.6(4) 1_555 1_555 1_555 yes S(16) C(20) H(15) 109.7(5) 1_555 1_555 1_555 no S(16) C(20) H(16) 108.4(5) 1_555 1_555 1_555 no C(19) C(20) H(15) 109.5(6) 1_555 1_555 1_555 no C(19) C(20) H(16) 105.6(5) 1_555 1_555 1_555 no H(15) C(20) H(16) 107.7(5) 1_555 1_555 1_555 no S(17) C(21) S(18) 115.3(2) 1_555 1_555 1_555 yes S(17) C(21) C(21) 123.1(5) 1_555 1_555 2_656 yes S(18) C(21) C(21) 121.5(5) 1_555 1_555 2_656 yes S(17) C(22) S(19) 112.5(3) 1_555 1_555 1_555 yes S(17) C(22) C(23) 117.9(3) 1_555 1_555 1_555 yes S(19) C(22) C(23) 129.6(4) 1_555 1_555 1_555 yes S(18) C(23) S(20) 115.7(2) 1_555 1_555 1_555 yes S(18) C(23) C(22) 116.8(3) 1_555 1_555 1_555 yes S(20) C(23) C(22) 127.5(3) 1_555 1_555 1_555 yes S(19) C(24) C(25) 116.0(4) 1_555 1_555 1_555 yes S(19) C(24) H(17) 109.9(4) 1_555 1_555 1_555 no S(19) C(24) H(18) 108.3(4) 1_555 1_555 1_555 no C(25) C(24) H(17) 109.4(5) 1_555 1_555 1_555 no C(25) C(24) H(18) 105.5(5) 1_555 1_555 1_555 no H(17) C(24) H(18) 107.4(5) 1_555 1_555 1_555 no S(20) C(25) C(24) 114.9(4) 1_555 1_555 1_555 yes S(20) C(25) H(19) 110.4(4) 1_555 1_555 1_555 no S(20) C(25) H(20) 108.5(4) 1_555 1_555 1_555 no C(24) C(25) H(19) 109.9(5) 1_555 1_555 1_555 no C(24) C(25) H(20) 106.0(5) 1_555 1_555 1_555 no H(19) C(25) H(20) 106.7(5) 1_555 1_555 1_555 no S(21) C(26) S(22) 115.4(2) 1_555 1_555 1_555 yes S(21) C(26) C(26) 123.6(5) 1_555 1_555 2_657 yes S(22) C(26) C(26) 121.0(5) 1_555 1_555 2_657 yes S(21) C(27) S(23) 114.1(3) 1_555 1_555 1_555 yes S(21) C(27) C(28) 117.5(3) 1_555 1_555 1_555 yes S(23) C(27) C(28) 128.4(4) 1_555 1_555 1_555 yes S(22) C(28) S(24) 114.3(3) 1_555 1_555 1_555 yes S(22) C(28) C(27) 116.8(3) 1_555 1_555 1_555 yes S(24) C(28) C(27) 128.9(4) 1_555 1_555 1_555 yes S(23) C(29) C(30) 115.1(4) 1_555 1_555 1_555 yes S(23) C(29) H(21) 108.0(4) 1_555 1_555 1_555 no S(23) C(29) H(22) 109.6(4) 1_555 1_555 1_555 no C(30) C(29) H(21) 106.1(5) 1_555 1_555 1_555 no C(30) C(29) H(22) 110.1(5) 1_555 1_555 1_555 no H(21) C(29) H(22) 107.6(5) 1_555 1_555 1_555 no S(24) C(30) C(29) 115.7(4) 1_555 1_555 1_555 yes S(24) C(30) H(23) 108.8(4) 1_555 1_555 1_555 no S(24) C(30) H(24) 110.2(4) 1_555 1_555 1_555 no C(29) C(30) H(23) 105.9(5) 1_555 1_555 1_555 no C(29) C(30) H(24) 108.9(4) 1_555 1_555 1_555 no H(23) C(30) H(24) 106.9(5) 1_555 1_555 1_555 no I(1) C(31) C(32) 172.8(4) 1_555 1_555 1_555 yes C(31) C(32) C(33) 173.4(5) 1_555 1_555 1_555 yes C(32) C(33) C(34) 123.0(4) 1_555 1_555 1_555 yes C(32) C(33) C(35) 120.4(4) 1_555 1_555 1_555 yes C(34) C(33) C(35) 116.6(4) 1_555 1_555 1_555 yes F(1) C(34) C(33) 120.3(4) 1_555 1_555 1_555 yes F(1) C(34) C(35) 118.0(4) 1_555 1_555 2_767 yes C(33) C(34) C(35) 121.6(4) 1_555 1_555 2_767 yes F(2) C(35) C(33) 118.4(4) 1_555 1_555 1_555 yes F(2) C(35) C(34) 119.8(4) 1_555 1_555 2_767 yes C(33) C(35) C(34) 121.7(4) 1_555 1_555 2_767 yes I(2) C(36) C(37) 173.1(4) 1_555 1_555 1_555 yes C(36) C(37) C(38) 174.7(5) 1_555 1_555 1_555 yes C(37) C(38) C(39) 120.8(5) 1_555 1_555 1_555 yes C(37) C(38) C(40) 123.0(5) 1_555 1_555 1_555 yes C(39) C(38) C(40) 116.2(4) 1_555 1_555 1_555 yes F(3) C(39) C(38) 119.5(4) 1_555 1_555 1_555 yes F(3) C(39) C(40) 118.7(4) 1_555 1_555 2_564 yes C(38) C(39) C(40) 121.8(4) 1_555 1_555 2_564 yes F(4) C(40) C(38) 119.4(4) 1_555 1_555 1_555 yes F(4) C(40) C(39) 118.6(4) 1_555 1_555 2_564 yes C(38) C(40) C(39) 122.0(4) 1_555 1_555 2_564 yes #------------------------------------------------------------------------------ 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 I(1) Br(1) 3.1364(6) 1_555 1_555 ? I(2) Br(1) 3.1407(6) 1_555 1_555 ? Br(1) C(19) 3.575(5) 1_555 1_554 ? S(4) S(13) 3.538(2) 1_555 1_555 ? S(5) C(29) 3.491(5) 1_555 2_656 ? S(5) S(16) 3.536(2) 1_555 1_554 ? S(5) S(23) 3.573(2) 1_555 2_656 ? S(6) S(14) 3.546(2) 1_555 2_757 ? S(6) F(2) 3.556(3) 1_555 1_555 ? S(7) S(24) 3.571(2) 1_555 1_554 ? S(8) S(16) 3.514(2) 1_555 2_757 ? S(11) S(19) 3.511(2) 1_555 2_656 ? S(14) F(1) 3.332(3) 1_555 1_545 ? S(15) F(3) 3.560(3) 1_555 2_666 ? S(15) S(19) 3.599(2) 1_555 2_656 ? S(18) S(23) 3.576(2) 1_555 1_555 ? S(20) F(4) 3.368(3) 1_555 2_655 ? F(1) C(30) 3.297(6) 1_555 1_565 ? F(1) C(18) 3.486(7) 1_555 1_565 ? F(2) C(37) 3.263(6) 1_555 1_656 ? F(2) C(7) 3.386(7) 1_555 2_756 ? F(2) C(36) 3.429(6) 1_555 1_656 ? F(2) C(8) 3.475(7) 1_555 2_756 ? F(2) C(9) 3.502(6) 1_555 1_555 ? F(3) C(32) 3.341(6) 1_555 1_454 ? F(3) C(18) 3.342(6) 1_555 1_464 ? F(3) C(17) 3.360(6) 1_555 1_464 ? F(3) C(31) 3.486(6) 1_555 1_454 ? F(3) C(20) 3.537(7) 1_555 2_666 ? F(4) C(25) 3.478(6) 1_555 2_655 ? F(4) C(8) 3.52(1) 1_555 2_655 ? F(4) C(17) 3.553(6) 1_555 2_655 ? C(9) C(31) 3.499(7) 1_555 1_555 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_General _audit_creation_date 'Thu Oct 7 00:42:09 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Hiroshi M. Yamamoto' _publ_contact_author_address ; Hirosawa, Wako-shi, Saitama 351-0198 (Japan) ; _publ_contact_author_email ' yhiroshi@postman.riken.go.jp ' _publ_contact_author_fax ' +81-(0)48-462-4611 ' _publ_contact_author_phone ' +81-(0)48-467-9410 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Journal of Materials Chemistry' _publ_requested_category ' ' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # _publ_section_title ; Structural and physical properties of conducting cation radical satls containing supramolecular assmblies based on pBIB derivatives (pBIB=p-Bis(iodoethynyl)benzene) ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_ET4Cl4pDMBIB2 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 18 11:24:22 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 2492.43 _chemical_formula_analytical ? _chemical_formula_sum 'C64 H48 Cl4 I4 S32 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 23.072(2) _cell_length_b 14.695(1) _cell_length_c 6.2770(3) _cell_angle_alpha 90 _cell_angle_beta 96.928(5) _cell_angle_gamma 90 _cell_volume 2112.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293.2 _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/n ' _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,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1224.00 _exptl_absorpt_coefficient_mu 2.434 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mac Science rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Mac Sciecne DIP320' _diffrn_measurement_method _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l _diffrn_reflns_number 20422 _reflns_number_total 5446 _reflns_number_observed 3986 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.051 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 30.4 _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 64 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 32 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 4 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; I 0 4 -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags I(1) 0.33570(1) 0.23018(2) 0.01416(5) 0.0470(1) Uani d . 1.00 . Cl(1) 0.24953(6) 0.1267(1) -0.2704(3) 0.0649(5) Uani d . 1.00 . S(1) 0.53543(5) 0.14939(9) 0.3155(2) 0.0500(4) Uani d . 1.00 . S(2) 0.47988(6) 0.1817(1) 0.6973(2) 0.0594(5) Uani d . 1.00 . S(3) 0.43014(5) 0.01527(8) 0.1359(2) 0.0474(4) Uani d . 1.00 . S(4) 0.37049(6) 0.0577(1) 0.5043(2) 0.0660(5) Uani d . 1.00 . S(5) 0.63375(6) 0.2764(1) 0.4278(3) 0.0620(5) Uani d . 1.00 . S(6) 0.56559(6) 0.3121(1) 0.8934(2) 0.0610(5) Uani d . 1.00 . S(7) 0.33862(6) -0.10112(10) -0.0791(3) 0.0593(4) Uani d . 1.00 . S(8) 0.26347(8) -0.0473(2) 0.3525(3) 0.0935(7) Uani d . 1.00 . C(1) 0.4776(2) 0.1271(3) 0.4556(8) 0.044(1) Uani d . 1.00 . C(2) 0.4315(2) 0.0710(3) 0.3758(8) 0.046(1) Uani d . 1.00 . C(3) 0.5704(2) 0.2269(3) 0.5013(9) 0.045(1) Uani d . 1.00 . C(4) 0.5440(2) 0.2414(3) 0.6772(9) 0.045(2) Uani d . 1.00 . C(5) 0.3617(2) -0.0324(3) 0.1412(8) 0.043(1) Uani d . 1.00 . C(6) 0.3334(2) -0.0132(4) 0.3096(9) 0.055(2) Uani d . 1.00 . C(7) 0.6599(3) 0.3331(6) 0.666(1) 0.113(3) Uani d . 1.00 . C(8) 0.6304(3) 0.3612(6) 0.819(1) 0.112(3) Uani d . 1.00 . C(9) 0.2614(2) -0.1072(4) -0.069(1) 0.069(2) Uani d . 1.00 . C(10) 0.2419(3) -0.1104(8) 0.134(1) 0.145(4) Uani d . 1.00 . C(11) 0.3933(2) 0.3096(4) 0.2055(9) 0.054(2) Uani d . 1.00 . C(12) 0.4247(2) 0.3633(3) 0.3053(9) 0.049(2) Uani d . 1.00 . C(13) 0.4629(2) 0.4318(3) 0.4101(8) 0.042(1) Uani d . 1.00 . C(14) 0.5094(2) 0.4628(3) 0.3072(8) 0.048(2) Uani d . 1.00 . C(15) 0.5470(2) 0.5313(3) 0.3948(8) 0.046(2) Uani d . 1.00 . C(16) 0.5967(3) 0.5609(4) 0.2766(10) 0.071(2) Uani d . 1.00 . H(1) 0.6887 0.2943 0.7354 0.1374 Uiso calc . 1.00 . H(2) 0.6775 0.3870 0.6194 0.1374 Uiso calc . 1.00 . H(3) 0.6206 0.4227 0.7843 0.1353 Uiso calc . 1.00 . H(4) 0.6576 0.3594 0.9452 0.1353 Uiso calc . 1.00 . H(5) 0.2443 -0.0557 -0.1409 0.0829 Uiso calc . 1.00 . H(6) 0.2477 -0.1611 -0.1435 0.0829 Uiso calc . 1.00 . H(7) 0.2488 -0.1717 0.1813 0.1740 Uiso calc . 1.00 . H(8) 0.2010 -0.1004 0.1071 0.1740 Uiso calc . 1.00 . H(9) 0.5157 0.4365 0.1702 0.0582 Uiso calc . 1.00 . H(10) 0.6213 0.5103 0.2594 0.0857 Uiso calc . 1.00 . H(11) 0.5814 0.5834 0.1387 0.0857 Uiso calc . 1.00 . H(12) 0.6181 0.6073 0.3550 0.0857 Uiso calc . 1.00 . 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 I(1) 0.0451(2) 0.0430(2) 0.0514(3) 0.0007(1) -0.0009(1) 0.0009(1) Cl(1) 0.0538(8) 0.0663(9) 0.072(1) -0.0022(6) -0.0032(7) -0.0175(7) S(1) 0.0407(6) 0.0537(8) 0.0560(10) -0.0109(5) 0.0079(6) -0.0142(6) S(2) 0.0520(8) 0.085(1) 0.0414(10) -0.0199(7) 0.0051(6) 0.0005(7) S(3) 0.0358(6) 0.0458(7) 0.0611(10) -0.0026(5) 0.0081(5) -0.0046(6) S(4) 0.0596(9) 0.099(1) 0.0406(10) -0.0388(8) 0.0097(6) -0.0075(8) S(5) 0.0505(8) 0.0741(10) 0.064(1) -0.0258(7) 0.0162(7) -0.0276(8) S(6) 0.0604(9) 0.0750(10) 0.047(1) -0.0081(7) 0.0035(6) -0.0163(7) S(7) 0.0475(7) 0.0584(8) 0.073(1) -0.0054(6) 0.0124(7) -0.0236(7) S(8) 0.070(1) 0.154(2) 0.060(1) -0.066(1) 0.0232(8) -0.029(1) C(1) 0.040(3) 0.045(3) 0.043(3) -0.003(2) -0.003(2) 0.005(2) C(2) 0.037(2) 0.048(3) 0.053(4) -0.003(2) -0.001(2) 0.007(2) C(3) 0.039(2) 0.047(3) 0.048(4) -0.005(2) 0.004(2) -0.008(2) C(4) 0.039(2) 0.047(3) 0.049(4) -0.002(2) 0.000(2) 0.003(2) C(5) 0.036(2) 0.044(3) 0.048(4) -0.002(2) 0.003(2) 0.004(2) C(6) 0.049(3) 0.072(4) 0.043(4) -0.021(3) 0.006(2) 0.000(3) C(7) 0.099(6) 0.173(8) 0.073(6) -0.081(6) 0.028(4) -0.057(5) C(8) 0.082(5) 0.159(8) 0.099(6) -0.057(5) 0.029(4) -0.075(6) C(9) 0.046(3) 0.088(4) 0.073(5) -0.017(3) 0.005(3) -0.010(3) C(10) 0.060(5) 0.29(1) 0.088(7) -0.068(6) 0.028(4) -0.058(7) C(11) 0.053(3) 0.054(3) 0.053(4) 0.000(3) -0.003(2) -0.001(3) C(12) 0.052(3) 0.048(3) 0.045(4) 0.005(2) 0.000(2) 0.008(2) C(13) 0.047(3) 0.040(3) 0.037(3) 0.006(2) -0.006(2) 0.005(2) C(14) 0.052(3) 0.052(3) 0.039(3) 0.006(2) 0.001(2) -0.008(2) C(15) 0.043(3) 0.054(3) 0.042(4) 0.002(2) 0.001(2) 0.001(2) C(16) 0.068(4) 0.089(4) 0.057(4) -0.017(3) 0.012(3) 0.006(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3986 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0463 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0518 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.537 _refine_ls_shift/esd_max 3.9940 _refine_ls_shift/esd_mean 0.0180 _refine_diff_density_min -1.33 _refine_diff_density_max 1.63 #------------------------------------------------------------------------------ _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 I(1) C(11) 2.046(6) 1_555 1_555 yes S(1) C(1) 1.716(5) 1_555 1_555 yes S(1) C(3) 1.756(5) 1_555 1_555 yes S(2) C(1) 1.712(5) 1_555 1_555 yes S(2) C(4) 1.737(5) 1_555 1_555 yes S(3) C(2) 1.711(5) 1_555 1_555 yes S(3) C(5) 1.731(4) 1_555 1_555 yes S(4) C(2) 1.715(5) 1_555 1_555 yes S(4) C(6) 1.748(5) 1_555 1_555 yes S(5) C(3) 1.743(5) 1_555 1_555 yes S(5) C(7) 1.756(7) 1_555 1_555 yes S(6) C(4) 1.734(5) 1_555 1_555 yes S(6) C(8) 1.773(7) 1_555 1_555 yes S(7) C(5) 1.743(5) 1_555 1_555 yes S(7) C(9) 1.792(6) 1_555 1_555 yes S(8) C(6) 1.742(5) 1_555 1_555 yes S(8) C(10) 1.679(9) 1_555 1_555 yes C(1) C(2) 1.391(6) 1_555 1_555 yes C(3) C(4) 1.341(7) 1_555 1_555 yes C(5) C(6) 1.337(7) 1_555 1_555 yes C(7) C(8) 1.306(10) 1_555 1_555 yes C(9) C(10) 1.403(10) 1_555 1_555 yes C(11) C(12) 1.196(7) 1_555 1_555 yes C(12) C(13) 1.443(7) 1_555 1_555 yes C(13) C(14) 1.395(7) 1_555 1_555 yes C(13) C(15) 1.384(7) 1_555 3_666 yes C(14) C(15) 1.398(7) 1_555 1_555 yes C(15) C(16) 1.503(7) 1_555 1_555 yes #------------------------------------------------------------------------------ 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(3) 96.2(2) 1_555 1_555 1_555 yes C(1) S(2) C(4) 96.2(2) 1_555 1_555 1_555 yes C(2) S(3) C(5) 95.5(2) 1_555 1_555 1_555 yes C(2) S(4) C(6) 95.7(2) 1_555 1_555 1_555 yes C(3) S(5) C(7) 100.7(3) 1_555 1_555 1_555 yes C(4) S(6) C(8) 102.1(3) 1_555 1_555 1_555 yes C(5) S(7) C(9) 102.1(3) 1_555 1_555 1_555 yes C(6) S(8) C(10) 102.8(3) 1_555 1_555 1_555 yes S(1) C(1) S(2) 114.9(3) 1_555 1_555 1_555 yes S(1) C(1) C(2) 122.5(4) 1_555 1_555 1_555 yes S(2) C(1) C(2) 122.5(4) 1_555 1_555 1_555 yes S(3) C(2) S(4) 115.5(3) 1_555 1_555 1_555 yes S(3) C(2) C(1) 122.2(4) 1_555 1_555 1_555 yes S(4) C(2) C(1) 122.2(4) 1_555 1_555 1_555 yes S(1) C(3) S(5) 115.3(3) 1_555 1_555 1_555 yes S(1) C(3) C(4) 115.6(4) 1_555 1_555 1_555 yes S(5) C(3) C(4) 129.1(4) 1_555 1_555 1_555 yes S(2) C(4) S(6) 114.4(3) 1_555 1_555 1_555 yes S(2) C(4) C(3) 117.1(4) 1_555 1_555 1_555 yes S(6) C(4) C(3) 128.6(4) 1_555 1_555 1_555 yes S(3) C(5) S(7) 114.3(3) 1_555 1_555 1_555 yes S(3) C(5) C(6) 117.6(4) 1_555 1_555 1_555 yes S(7) C(5) C(6) 128.2(4) 1_555 1_555 1_555 yes S(4) C(6) S(8) 116.6(3) 1_555 1_555 1_555 yes S(4) C(6) C(5) 115.7(4) 1_555 1_555 1_555 yes S(8) C(6) C(5) 127.7(4) 1_555 1_555 1_555 yes S(5) C(7) C(8) 128.3(6) 1_555 1_555 1_555 yes S(5) C(7) H(1) 104.8(6) 1_555 1_555 1_555 no S(5) C(7) H(2) 104.2(6) 1_555 1_555 1_555 no C(8) C(7) H(1) 104.9(9) 1_555 1_555 1_555 no C(8) C(7) H(2) 104.1(9) 1_555 1_555 1_555 no H(1) C(7) H(2) 109.9(7) 1_555 1_555 1_555 no S(6) C(8) C(7) 126.5(6) 1_555 1_555 1_555 yes S(6) C(8) H(3) 105.2(6) 1_555 1_555 1_555 no S(6) C(8) H(4) 105.1(7) 1_555 1_555 1_555 no C(7) C(8) H(3) 105.3(9) 1_555 1_555 1_555 no C(7) C(8) H(4) 104.6(8) 1_555 1_555 1_555 no H(3) C(8) H(4) 109.5(7) 1_555 1_555 1_555 no S(7) C(9) C(10) 117.7(5) 1_555 1_555 1_555 yes S(7) C(9) H(5) 107.7(5) 1_555 1_555 1_555 no S(7) C(9) H(6) 107.1(5) 1_555 1_555 1_555 no C(10) C(9) H(5) 107.5(7) 1_555 1_555 1_555 no C(10) C(9) H(6) 107.2(7) 1_555 1_555 1_555 no H(5) C(9) H(6) 109.5(6) 1_555 1_555 1_555 no S(8) C(10) C(9) 128.8(6) 1_555 1_555 1_555 yes S(8) C(10) H(7) 104.4(7) 1_555 1_555 1_555 no S(8) C(10) H(8) 104.6(7) 1_555 1_555 1_555 no C(9) C(10) H(7) 104.6(8) 1_555 1_555 1_555 no C(9) C(10) H(8) 104.6(8) 1_555 1_555 1_555 no H(7) C(10) H(8) 109.1(9) 1_555 1_555 1_555 no I(1) C(11) C(12) 173.3(5) 1_555 1_555 1_555 yes C(11) C(12) C(13) 175.5(6) 1_555 1_555 1_555 yes C(12) C(13) C(14) 118.6(5) 1_555 1_555 1_555 yes C(12) C(13) C(15) 121.3(5) 1_555 1_555 3_666 yes C(14) C(13) C(15) 120.0(4) 1_555 1_555 3_666 yes C(13) C(14) C(15) 122.0(5) 1_555 1_555 1_555 yes C(13) C(14) H(9) 119.1(5) 1_555 1_555 1_555 no C(15) C(14) H(9) 118.9(5) 1_555 1_555 1_555 no C(13) C(15) C(14) 118.0(5) 3_666 1_555 1_555 yes C(13) C(15) C(16) 122.7(5) 3_666 1_555 1_555 yes C(14) C(15) C(16) 119.3(5) 1_555 1_555 1_555 yes C(15) C(16) H(10) 109.3(5) 1_555 1_555 1_555 no C(15) C(16) H(11) 109.1(5) 1_555 1_555 1_555 no C(15) C(16) H(12) 109.4(6) 1_555 1_555 1_555 no H(10) C(16) H(11) 109.2(6) 1_555 1_555 1_555 no H(10) C(16) H(12) 110.0(6) 1_555 1_555 1_555 no H(11) C(16) H(12) 109.7(6) 1_555 1_555 1_555 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 I(1) Cl(1) 2.933(1) 1_555 1_555 ? Cl(1) S(5) 3.393(2) 1_555 4_454 ? Cl(1) S(4) 3.431(2) 1_555 1_554 ? Cl(1) S(8) 3.524(2) 1_555 1_554 ? Cl(1) C(8) 3.539(8) 1_555 4_453 ? S(1) S(7) 3.491(2) 1_555 3_655 ? S(5) S(7) 3.488(2) 1_555 3_655 ? S(5) S(6) 3.568(2) 1_555 1_554 ? C(1) C(11) 3.563(7) 1_555 1_555 ? C(10) C(11) 3.589(9) 1_555 2_545 ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;