# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 1145/182 data_General _audit_creation_date 'Tue Jun 29 18:14:40 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 ' Tomoyuki Akutagawa ' _publ_contact_author_address ; Research Institute for Electronic Science, Hokkaido University N12W6 kita-ku, Sapporo 060-0812, Japan ; _publ_contact_author_email ' takuta@imd.es.hokudai.ac.jp ' _publ_contact_author_fax ' +81-11-706-4972 ' _publ_contact_author_phone ' +81-11-706-2884 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' J. Mater. Chem. ' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Crystal Structures and Optical Properties of Cation Radical Salts of Tetrathiafulvalene Trisannulated Macrocycle ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Akutagawa, Tomoyuki ' ; FIRST AUTHORS FOOTNOTES ; ; Research Institute for Electronic Science, Hokkaido University N12W6 kita-ku, Sapporo 060-0812, Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; Cation radical salts of the bis(methythio)tetrathiafulvalene (DMT-TTF) trisannulated macrocycles, [tris(DMT-TTF)]I3- (1) and [tris(DMT-TTF)]IBr2- (2), were prepared and the crystal structures and polarized reflectance spectra of the salts 1 and 2 were investigated. An isostructural character is observed for two salts, 1: P1-, a = 13.653(2), b = 20.303(3), c = 12.677(1) A, a = 104.622(10), b = 116.501(7), g = 81.65(1) , V = 3040.8(6) A, Z = 2, R = 0.073 and 2: P1-, a = 13.656(5), b = 20.254(4), c = 12.638(4) A, a = 104.75(2), b = 116.18(3), g = 81.57(2) , V = 3031(1) deg, Z = 2, R = 0.079. The C3 symmetry of tris(DMT-TTF) bearing equivalent three DMT-TTF units (A, B, and C) within a molecule is broken through the formation of cation radical salts. Two DMT-TTF (B and C) of three equivalent units form an intramolecular dimer structure through the face-to-face p-p overlap, whereas the plane of A unit is orthogonal to the dimer plane and isolated from the other units. The intramolecular dimers are further dimerized through the intermolecular B - B' interaction, resulting in a DMT-TTF tetramer unit (C - B - B' - C') within the crystal. The intramolecular bond lengths and polarized reflectance spectra indicate the localization of a unit charge on the B unit rather than A or C. The charge separated A0 - B0 -C0 electronic structure is confirmed. ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; This work was partly supported by a Grant-in-Aid for Science Research from the Ministry of Education, Science, Sports, and Culture of Japan and by the Proposal-Based New Industry Creative Type Technology R&D Promotion Program from the New Energy and Industrial Technology Development Organization (NEDO) in Japan. ; _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. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. F. Wudl, Acc. Chem. Res., 1984, 17, 227. D. O. Cowan,"New Aspects of Organic Chemistry", edited by Z. Yoshida, T. Shiba and Y. Oshiro, Proc. 4th Int. Kyoto Conf., Kodansha Ltd, Tokyo, 1989. J.M. Williams, J. R. Ferraro, R. J. Thorn, K. D. Carlson, U. Geiser, H. H. Wang, A. M. Kini and M. Whangbo, "Organic Superconductors", Prentice-Hall, Englewood Cliffs, New Jersey, 1992. G. Saito, "Metal-Insulator Transition Revisited", edited by P. P. Edwards and C. N. R. Rao, Taylor and Framcis, 1995. Proc. International Conference on Synthetic Metals (ICSM' 96), Synth. Met., 1997, 86, no 1-3. K. B. Simonsen and J. Becher, Synlett., 1997, 1211. M. B. Nielsen and J. Becher, Libigs Ann. Recueil, 1997, 2177. T. Jorgensen, T. K. Hansen and J. Becher, Chem. Soc. Rev., 1994, 41. M. R. Bryce, Adv. Mater., 1999, 11, 11. J. Becher, J. Lau, P. Leriche, P. Mork and N. Svenstrup, J. Chem. Soc. Chem,. Commun., 1994, 2715. K. B. Simonsen, N. Svenstrup,J. Lau, O. Simonsen, P. Monk, G. J. Kristensen and J. Becher, Synthesis, 1996, 407. T. Otsubo, Y. Aso and K. Takimiya, Adv. Mater., 1996, 8, 203. K. Takimiya, Y. Aso, F. Ogura and T. Ostubo, Chem. Lett., 1995, 735. Z. T. Li and J. Becher, J. Chem. Soc., Chem. Commun, 1996, 639. Z. T. Li, P. C. Stein, J. Becher, D. Jensen, P. Mork and N. Svenstrup, Chem. Eur. J., 1996, 2, 624. K. B. Simonsen, N. Thorup and J. Becher, Synthesis, 1997, 1399. S. Yumoki, K. Takimiya, Y. Aso and T. Otsubo,Tetrahedron Lett., 1997, 38, 3071. A. S. Batsanov, D. E. John, M. R. Bryceand J. A. Howard, Adv. Mater., 1998, 10, 1360. M. B. Nielsen, Z. T. Li and J. Becher, J. Mater. Chem., 1997, 7, 1175. J. Lau and J. Becher, Synthesis, 1997, 1015. G. J. Marshallsay,T. K. Hansen, A. J. Moore, M. R. Bryce and J. Becher, Synthesis, 1994, 926. T. Akutagawa, Y. Abe, Y. Nezu, T. Nakamura, M. Kataoka, A. Yamanaka, K. Inoue, T. Inabe, C. A. Christensen and J. Becher, Inorg. Chem., 1998, 37, 2330. Y. Abe, T. Akutagawa, T. Hasegawa, T. Nakamura, K. Sugiura, Y. Sakata, T. Inabe, C. A. Christensen and J. Becher, Synth. Metals, in press. K. Takimiya, N. Thorup, and J. Becher., unpublished result. teXsan: Single crystal structure analysis software. Version 1.9, 1993. igaku Denki Corporation. T. Mori, A. Kobayashi, Y. Sasaki, H. Kobayashi, G. Saito and H. Inokuchi, Bull. Chem. Soc. Jpn. 1984, 57, 627. R. H. Summerville and R. J. Hoffmann,J. Am. Chem. Soc. 1976, 98, 7240. A. J. Berlinsky, J. F. Carolan and L. Weiler, Solid State Commun. 1974, 15, 795. A. Bondi, J. Phys. Chem., 1964, 68, 441. W. F. Coopens, N. C. Kenny, J. W. Edmonds, A. Nagel, F. Wudl and P. Coppens, J. Chem. Soc., Chem. Commun, 1971, 889. T. J. Kistenmacher, T. E. Phillips and D. O. Cowan, Acta Crystallogr., Sect. B, 1974, 30, 763. H. Kobayashi, R. Kato, T. Mori, A. Kobayashi, Y. Sasaki, G. Sito, T. Enoki and H. Inokuchi, Mol. Crst. Liq. Cryst., 1984, 107, 33. J. B. Torrance, B. A. Scott, B. Welber, F. B. Kaufman and P. E. Seiden, P hys. Rev. B., 1979, 19, 730. T. Sugano, H. Hayashi, M. Kinoshita and K. Nishikida, Phys. Rev. B., 1989, 39, 11387. ; _publ_section_figure_captions ; Fig. 1 Molecular structure of tris(DMT-TTF) and counter anions (I3, and IBr2) in the salts 1 and 2. The tris(DMT-TTF) molecule is bearing three DMT-TTF units A, B, and C. Fig. 2 Stereoview of the unit cell of [tris(DMT-TTF)](I3-)(DCE)1.5 viewed along the c-axis. Fig. 3 Intramolecular and intermolecular p-p interactions. a) Tetramer units C ~ B ~ B' ~ C viewed along the short axis of the DMT-TTF B. The molecules enclosed by dashed lines correspond to those depicted in Fig. 3b. b) Packing arrangement of DMT-TTF viewed normal to the molecular plane of the DMT-TTF B. c) Side-by-side intermolecular interaction normal to the DMT-TTF A unit. Fig. 4 Polarized reflectance spectra of the [tris(DMT-TTF)](I3)(DCE)1.5 in the energy range from 500 to 25000 cm-1. Polarization spectra are measured with the electric vector parallel (E//) and normal (E) to the a+b axis. ; _publ_section_exptl_prep ; The TTF trisannulated macrocycle, tris(DMT-TTF), was prepared using the cyanoethyleneprotection / deprotection protocol according to the literature. The single crystals of cation radical salts were grown using the standard electrocrystallization method.The electrocrystallization solvent of 1,2 -dichloroethane (DCE) was distilled under argon and was passed through neutral alumina column prior to use. A constant current (2 mA) was applied to the platinum electrodes (1 mmf) equipped with the H-shaped cell (18 ml) during two weeks time at room temperature. The electrocrystallization using the supporting electrolytes of n-(C4H9)4NEI3 or n-(C4H9)4NEIBr2 provided high-quality single crystals, while the formations of crystalline solid were not observed using the electrolytes of n-(C4H9)4NEF, n-(C4H9)4NECl, n-(C4H9)4NEBr, n-(C4H9)4NEI, n-(C4H9)4N EBF4, n-(C4H9)4NEClO4, or n-(C4H9)4NEPF6 under the same condition. The stoichiometries of radical salts were determined by X-ray structural analysis as [tris(DMT-TTF)](I3-)(DCE)1.5 (1) and [tris(DMT-TTF)](IBr2-)(DCE)1.5 (2), respectively. The single crystals 1 and 2 were black plates with typical dimensions of 1.5 x 0.5 x 0.1 and 0.5 x 0.2 x 0.05 mm3 respectively. ; _publ_section_exptl_refinement ; Crystal data of the salts 1 and 2 were collected on a Rigaku AFC-7R diffractometers with MoKa (l = 0.71073 A)radiation at 190 K using graphite monochrometor. The unit cell parameters were determined and refined from 25 reflections. Data were collected with 2q-w scan mode. The structures were solved and refined by the aid of the program of teXsan (Rigaku). The structure refinements were performed by full matrix least-squares method. Table 1 summarizes the crystal data. Parameters were refined using the anisotropic temperature factors in all crystals, and the hydrogen atoms were removed form the refinements. Table 2 summarizes the selected bond lengths. ; #------------------------------------------------------------------------------ data_TTFtrimerIBr2 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C36 H42 Br2 Cl3 I S24 ' _chemical_formula_moiety '?' _chemical_formula_weight 1637.24 _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 13.656(5) _cell_length_b 20.254(4) _cell_length_c 12.638(4) _cell_angle_alpha 104.75(2) _cell_angle_beta 116.18(3) _cell_angle_gamma 81.57(2) _cell_volume 3031(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 173.5 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'Black' _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.380 _exptl_crystal_size_min 0.080 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.839 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.385 _exptl_absorpt_correction_T_max 0.797 #------------------------------------------------------------------------------ # 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 14538 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 450 _diffrn_standards_decay_% 1.56 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 14538 _reflns_number_observed 13955 _reflns_observed_criterion >3sigma(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0790 _refine_ls_wR_factor_obs 0.0878 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 10238 _refine_ls_number_parameters 595 _refine_ls_goodness_of_fit_all 3.506 _refine_ls_weighting_scheme unit _refine_ls_shift/esd_max 0.1890 _refine_diff_density_max 4.55 _refine_diff_density_min -2.37 _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) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; '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) ; #------------------------------------------------------------------------------ # 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.23209(6) 0.38570(4) 0.16679(6) 0.0578(2) Uani 1.00 d . . . Br(1) Br 0.36090(9) 0.50508(5) 0.27448(8) 0.0487(3) Uani 1.00 d . . . Br(2) Br 0.09768(8) 0.27085(6) 0.06619(8) 0.0492(2) Uani 1.00 d . . . Cl(1) Cl 0.6776(3) 0.0113(2) 0.2624(3) 0.0710(9) Uani 1.00 d . . . Cl(2) Cl 0.8507(3) 0.1980(2) 0.4458(3) 0.0695(9) Uani 1.00 d . . . Cl(3) Cl 1.0068(3) 0.1080(2) 1.0563(4) 0.099(1) Uani 1.00 d . . . S(1) S 0.7252(2) 0.0168(1) 0.6230(2) 0.0424(6) Uani 1.00 d . . . S(2) S 0.5005(2) 0.1066(1) 0.5105(2) 0.0398(5) Uani 1.00 d . . . S(3) S 0.2981(2) 0.1745(2) 0.3492(2) 0.0500(6) Uani 1.00 d . . . S(4) S 0.4335(2) 0.3188(1) 0.4762(3) 0.0569(7) Uani 1.00 d . . . S(5) S 0.6241(2) 0.2331(1) 0.6198(2) 0.0401(5) Uani 1.00 d . . . S(6) S 0.8522(2) 0.1410(1) 0.7234(2) 0.0395(5) Uani 1.00 d . . . S(7) S 1.0631(2) 0.0608(2) 0.7376(3) 0.0634(8) Uani 1.00 d . . . S(8) S 0.9212(2) -0.0760(1) 0.6275(4) 0.0719(9) Uani 1.00 d . . . S(9) S 0.2244(2) 0.2979(1) -0.3848(2) 0.0353(5) Uani 1.00 d . . . S(10) S 0.4353(2) 0.2090(1) -0.2412(2) 0.0350(5) Uani 1.00 d . . . S(11) S 0.5745(2) 0.0831(1) -0.1888(2) 0.0355(5) Uani 1.00 d . . . S(12) S 0.5070(2) 0.1013(1) 0.0412(2) 0.0390(5) Uani 1.00 d . . . S(13) S 0.3688(2) 0.2266(1) -0.0435(2) 0.0322(5) Uani 1.00 d . . . S(14) S 0.1545(2) 0.3224(1) -0.1887(2) 0.0363(5) Uani 1.00 d . . . S(15) S -0.0700(2) 0.3768(1) -0.3376(2) 0.0482(6) Uani 1.00 d . . . S(16) S 0.0061(2) 0.3413(1) -0.5642(2) 0.0478(6) Uani 1.00 d . . . S(17) S 0.2979(2) 0.4764(1) -0.0587(2) 0.0330(5) Uani 1.00 d . . . S(18) S 0.5121(2) 0.3897(1) 0.0955(2) 0.0327(5) Uani 1.00 d . . . S(19) S 0.7085(2) 0.3078(1) 0.2435(2) 0.0437(6) Uani 1.00 d . . . S(20) S 0.7935(2) 0.2958(1) 0.0297(2) 0.0365(5) Uani 1.00 d . . . S(21) S 0.5873(2) 0.3723(1) -0.0936(2) 0.0330(5) Uani 1.00 d . . . S(22) S 0.3725(2) 0.4528(1) -0.2492(2) 0.0339(5) Uani 1.00 d . . . S(23) S 0.1634(2) 0.5124(1) -0.4204(2) 0.0445(6) Uani 1.00 d . . . S(24) S 0.0843(2) 0.5445(1) -0.2033(2) 0.0446(6) Uani 1.00 d . . . C(1) C 0.826(1) -0.1133(6) 0.475(1) 0.078(4) Uani 1.00 d . . . C(2) C 0.8630(7) 0.0060(5) 0.6461(10) 0.048(3) Uani 1.00 d . . . C(3) C 0.9224(7) 0.0631(5) 0.6949(9) 0.043(2) Uani 1.00 d . . . C(4) C 1.0879(9) 0.1502(6) 0.759(1) 0.069(4) Uani 1.00 d . . . C(5) C 0.7225(7) 0.1060(5) 0.6407(8) 0.036(2) Uani 1.00 d . . . C(6) C 0.6301(7) 0.1429(4) 0.5953(7) 0.035(2) Uani 1.00 d . . . C(7) C 0.4350(7) 0.1803(5) 0.4546(7) 0.038(2) Uani 1.00 d . . . C(8) C 0.4908(7) 0.2380(5) 0.5051(8) 0.039(2) Uani 1.00 d . . . C(9) C 0.3103(7) 0.1165(6) 0.2212(8) 0.045(2) Uani 1.00 d . . . C(10) C 0.3884(7) 0.1415(5) 0.1824(8) 0.040(2) Uani 1.00 d . . . C(11) C 0.3938(7) 0.0885(5) 0.0726(8) 0.040(2) Uani 1.00 d . . . C(12) C 0.4530(6) 0.1538(4) -0.0641(7) 0.031(2) Uani 1.00 d . . . C(13) C 0.3380(6) 0.2443(4) -0.1845(7) 0.032(2) Uani 1.00 d . . . C(14) C 0.2507(6) 0.2820(4) -0.2451(7) 0.031(2) Uani 1.00 d . . . C(15) C 0.0547(7) 0.3369(4) -0.3300(8) 0.034(2) Uani 1.00 d . . . C(16) C -0.1096(9) 0.3313(7) -0.257(1) 0.063(3) Uani 1.00 d . . . C(17) C 0.0269(10) 0.2636(7) -0.6629(9) 0.065(3) Uani 1.00 d . . . C(18) C 0.0860(7) 0.3240(4) -0.4210(8) 0.034(2) Uani 1.00 d . . . C(19) C 0.4841(6) 0.1459(4) -0.1537(7) 0.031(2) Uani 1.00 d . . . C(20) C 0.7028(7) 0.0933(5) -0.0489(8) 0.039(2) Uani 1.00 d . . . C(21) C 0.7302(7) 0.1677(5) 0.0192(7) 0.035(2) Uani 1.00 d . . . C(22) C 0.7512(7) 0.2083(5) -0.0549(8) 0.040(2) Uani 1.00 d . . . C(23) C 0.6694(6) 0.3344(4) 0.0274(7) 0.031(2) Uani 1.00 d . . . C(24) C 0.4881(7) 0.4052(4) -0.0433(7) 0.033(2) Uani 1.00 d . . . C(25) C 0.3958(6) 0.4413(4) -0.1092(7) 0.029(2) Uani 1.00 d . . . C(26) C 0.2415(6) 0.4884(4) -0.2826(7) 0.030(2) Uani 1.00 d . . . C(27) C 0.2235(9) 0.4600(6) -0.5176(9) 0.052(3) Uani 1.00 d . . . C(28) C 0.2079(6) 0.5011(4) -0.1928(7) 0.032(2) Uani 1.00 d . . . C(29) C 0.0721(8) 0.5286(6) -0.0753(9) 0.058(3) Uani 1.00 d . . . C(30) C 0.6352(6) 0.3434(4) 0.1156(7) 0.031(2) Uani 1.00 d . . . C(31) C 0.6539(8) 0.3533(5) 0.3519(8) 0.041(2) Uani 1.00 d . . . C(32) C 0.5629(8) 0.3155(5) 0.3506(9) 0.045(2) Uani 1.00 d . . . C(33) C 0.5410(8) 0.3553(5) 0.4602(8) 0.047(2) Uani 1.00 d . . . C(34) C 0.773(2) 0.0769(10) 0.364(2) 0.151(8) Uani 1.00 d . . . C(35) C 0.755(2) 0.132(1) 0.346(2) 0.247(9) Uani 1.00 d . . . C(36) C 1.018(2) 0.023(1) 1.048(2) 0.154(8) Uani 1.00 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0558(3) 0.0792(5) 0.0417(3) 0.0283(3) 0.0263(2) 0.0243(3) Br(1) 0.0661(6) 0.0433(5) 0.0340(4) 0.0049(4) 0.0237(4) 0.0022(4) Br(2) 0.0383(4) 0.0783(7) 0.0457(4) 0.0088(4) 0.0235(3) 0.0321(4) Cl(1) 0.054(2) 0.064(2) 0.081(2) -0.008(1) 0.006(1) 0.028(1) Cl(2) 0.083(2) 0.054(2) 0.056(2) -0.012(1) 0.012(1) 0.013(1) Cl(3) 0.050(2) 0.099(3) 0.132(3) 0.002(2) 0.014(2) 0.044(2) S(1) 0.0326(10) 0.036(1) 0.060(1) 0.0000(9) 0.0176(9) 0.0161(10) S(2) 0.0321(10) 0.044(1) 0.043(1) 0.0012(9) 0.0129(8) 0.0142(9) S(3) 0.032(1) 0.077(2) 0.044(1) 0.015(1) 0.0190(8) 0.019(1) S(4) 0.063(1) 0.053(1) 0.080(1) 0.029(1) 0.048(1) 0.037(1) S(5) 0.040(1) 0.037(1) 0.047(1) 0.0042(9) 0.0190(8) 0.0148(9) S(6) 0.0341(10) 0.032(1) 0.052(1) 0.0002(8) 0.0190(8) 0.0066(9) S(7) 0.034(1) 0.049(2) 0.109(2) 0.002(1) 0.030(1) 0.019(1) S(8) 0.049(1) 0.033(1) 0.120(3) 0.007(1) 0.028(2) 0.008(2) S(9) 0.0321(10) 0.036(1) 0.0373(10) 0.0025(8) 0.0111(8) 0.0143(8) S(10) 0.0312(9) 0.042(1) 0.0367(9) 0.0047(8) 0.0146(7) 0.0180(8) S(11) 0.0366(10) 0.035(1) 0.0345(9) 0.0058(8) 0.0160(7) 0.0077(8) S(12) 0.042(1) 0.043(1) 0.0398(10) 0.0098(9) 0.0201(8) 0.0203(8) S(13) 0.0300(9) 0.034(1) 0.0314(9) 0.0026(8) 0.0115(7) 0.0081(8) S(14) 0.0322(10) 0.035(1) 0.0383(10) 0.0018(8) 0.0124(8) 0.0071(8) S(15) 0.034(1) 0.044(1) 0.065(1) 0.0122(9) 0.0188(10) 0.020(1) S(16) 0.047(1) 0.041(1) 0.044(1) 0.011(1) 0.0062(10) 0.0200(9) S(17) 0.0295(9) 0.033(1) 0.0375(9) 0.0025(8) 0.0143(7) 0.0102(8) S(18) 0.0312(9) 0.033(1) 0.0352(9) 0.0036(8) 0.0143(7) 0.0107(8) S(19) 0.044(1) 0.050(1) 0.0365(10) 0.0121(10) 0.0144(8) 0.0196(9) S(20) 0.0266(9) 0.039(1) 0.045(1) 0.0039(8) 0.0137(7) 0.0148(9) S(21) 0.0321(9) 0.034(1) 0.0359(9) 0.0055(8) 0.0152(7) 0.0131(8) S(22) 0.0308(9) 0.034(1) 0.0362(9) 0.0061(8) 0.0139(7) 0.0102(8) S(23) 0.043(1) 0.046(1) 0.039(1) 0.0153(10) 0.0136(9) 0.0156(9) S(24) 0.035(1) 0.050(1) 0.057(1) 0.0132(9) 0.0228(8) 0.0230(10) C(1) 0.13(1) 0.037(6) 0.062(7) -0.002(7) 0.041(7) 0.005(5) C(2) 0.036(4) 0.037(5) 0.071(6) 0.004(4) 0.024(4) 0.012(4) C(3) 0.029(4) 0.037(5) 0.065(5) 0.002(3) 0.023(3) 0.012(4) C(4) 0.053(6) 0.052(7) 0.105(9) -0.020(5) 0.039(5) -0.001(6) C(5) 0.030(4) 0.040(5) 0.040(4) 0.003(3) 0.017(3) 0.011(3) C(6) 0.036(4) 0.035(4) 0.039(4) 0.003(3) 0.016(3) 0.016(3) C(7) 0.031(4) 0.053(5) 0.034(4) 0.010(4) 0.017(3) 0.017(3) C(8) 0.035(4) 0.048(5) 0.045(4) 0.012(4) 0.024(3) 0.022(4) C(9) 0.038(4) 0.063(6) 0.041(4) -0.002(4) 0.021(3) 0.014(4) C(10) 0.046(4) 0.042(5) 0.039(4) -0.003(4) 0.022(3) 0.011(4) C(11) 0.042(4) 0.043(5) 0.041(4) -0.008(4) 0.021(3) 0.007(4) C(12) 0.028(4) 0.034(4) 0.029(3) -0.002(3) 0.007(3) 0.010(3) C(13) 0.030(4) 0.033(4) 0.032(4) -0.005(3) 0.010(3) 0.009(3) C(14) 0.029(4) 0.021(4) 0.037(4) -0.004(3) 0.010(3) 0.003(3) C(15) 0.030(4) 0.027(4) 0.042(4) 0.002(3) 0.010(3) 0.012(3) C(16) 0.055(5) 0.073(8) 0.077(6) 0.014(5) 0.041(4) 0.029(5) C(17) 0.062(6) 0.081(8) 0.035(5) 0.027(6) 0.015(4) 0.010(5) C(18) 0.031(4) 0.024(4) 0.042(4) -0.001(3) 0.008(3) 0.009(3) C(19) 0.032(4) 0.031(4) 0.033(4) 0.001(3) 0.015(3) 0.010(3) C(20) 0.035(4) 0.037(5) 0.039(4) 0.008(4) 0.012(3) 0.009(4) C(21) 0.034(4) 0.038(5) 0.035(4) 0.002(3) 0.014(3) 0.010(3) C(22) 0.043(4) 0.038(5) 0.042(4) 0.007(4) 0.021(3) 0.013(4) C(23) 0.026(3) 0.029(4) 0.036(4) 0.002(3) 0.009(3) 0.012(3) C(24) 0.032(4) 0.027(4) 0.034(4) 0.000(3) 0.009(3) 0.006(3) C(25) 0.026(3) 0.025(4) 0.033(4) 0.000(3) 0.008(3) 0.007(3) C(26) 0.030(4) 0.026(4) 0.034(4) 0.003(3) 0.013(3) 0.010(3) C(27) 0.063(6) 0.053(6) 0.043(4) 0.013(5) 0.030(4) 0.012(4) C(28) 0.029(4) 0.027(4) 0.040(4) 0.000(3) 0.012(3) 0.010(3) C(29) 0.045(5) 0.083(8) 0.059(5) 0.022(5) 0.032(4) 0.033(5) C(30) 0.026(3) 0.031(4) 0.033(4) 0.003(3) 0.010(3) 0.008(3) C(31) 0.051(5) 0.041(5) 0.032(4) -0.005(4) 0.018(3) 0.007(3) C(32) 0.045(5) 0.043(5) 0.046(5) -0.003(4) 0.020(4) 0.007(4) C(33) 0.065(5) 0.042(5) 0.054(4) 0.009(4) 0.044(3) 0.015(4) C(34) 0.16(2) 0.06(1) 0.14(2) -0.01(1) -0.01(1) -0.01(1) C(35) 0.20(2) 0.14(1) 0.25(2) -0.12(1) -0.13(2) 0.14(1) C(36) 0.09(1) 0.12(2) 0.13(2) 0.02(1) -0.03(1) -0.01(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF92 (PATTY)' _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) Br(1) 2.872(2) . . ? I(1) Br(2) 2.843(2) . . ? Cl(1) C(34) 1.81(2) . . ? Cl(2) C(35) 1.81(2) . . ? Cl(3) C(36) 1.69(2) . . ? S(1) C(2) 1.761(10) . . ? S(1) C(5) 1.760(9) . . ? S(2) C(6) 1.768(9) . . ? S(2) C(7) 1.765(9) . . ? S(3) C(7) 1.752(8) . . ? S(3) C(9) 1.80(1) . . ? S(4) C(8) 1.761(9) . . ? S(4) C(33) 1.84(1) . . ? S(5) C(6) 1.770(9) . . ? S(5) C(8) 1.765(9) . . ? S(6) C(3) 1.765(9) . . ? S(6) C(5) 1.757(9) . . ? S(7) C(3) 1.748(9) . . ? S(7) C(4) 1.82(1) . . ? S(8) C(1) 1.82(1) . . ? S(8) C(2) 1.739(10) . . ? S(9) C(14) 1.746(9) . . ? S(9) C(18) 1.769(9) . . ? S(10) C(13) 1.758(9) . . ? S(10) C(19) 1.766(8) . . ? S(11) C(19) 1.753(8) . . ? S(11) C(20) 1.850(9) . . ? S(12) C(11) 1.825(10) . . ? S(12) C(12) 1.751(8) . . ? S(13) C(12) 1.772(9) . . ? S(13) C(13) 1.761(8) . . ? S(14) C(14) 1.766(9) . . ? S(14) C(15) 1.770(8) . . ? S(15) C(15) 1.747(9) . . ? S(15) C(16) 1.82(1) . . ? S(16) C(17) 1.82(1) . . ? S(16) C(18) 1.749(9) . . ? S(17) C(25) 1.716(9) . . ? S(17) C(28) 1.745(8) . . ? S(18) C(24) 1.740(9) . . ? S(18) C(30) 1.747(8) . . ? S(19) C(30) 1.758(8) . . ? S(19) C(31) 1.827(10) . . ? S(20) C(22) 1.847(10) . . ? S(20) C(23) 1.750(8) . . ? S(21) C(23) 1.737(8) . . ? S(21) C(24) 1.721(9) . . ? S(22) C(25) 1.726(9) . . ? S(22) C(26) 1.736(8) . . ? S(23) C(26) 1.744(8) . . ? S(23) C(27) 1.81(1) . . ? S(24) C(28) 1.751(8) . . ? S(24) C(29) 1.81(1) . . ? C(2) C(3) 1.36(1) . . ? C(5) C(6) 1.34(1) . . ? C(7) C(8) 1.34(1) . . ? C(9) C(10) 1.54(1) . . ? C(10) C(11) 1.55(1) . . ? C(12) C(19) 1.34(1) . . ? C(13) C(14) 1.35(1) . . ? C(15) C(18) 1.35(1) . . ? C(20) C(21) 1.54(1) . . ? C(21) C(22) 1.53(1) . . ? C(23) C(30) 1.35(1) . . ? C(24) C(25) 1.39(1) . . ? C(26) C(28) 1.36(1) . . ? C(31) C(32) 1.54(1) . . ? C(32) C(33) 1.54(1) . . ? C(34) C(35) 1.17(3) . . ? C(36) C(36) 1.26(4) . 2_757 ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br(1) I(1) Br(2) 177.08(4) 1_555 1_555 1_555 ? C(2) S(1) C(5) 93.7(4) 1_555 1_555 1_555 ? C(6) S(2) C(7) 94.7(4) 1_555 1_555 1_555 ? C(7) S(3) C(9) 101.3(4) 1_555 1_555 1_555 ? C(8) S(4) C(33) 102.9(4) 1_555 1_555 1_555 ? C(6) S(5) C(8) 94.7(4) 1_555 1_555 1_555 ? C(3) S(6) C(5) 94.0(4) 1_555 1_555 1_555 ? C(3) S(7) C(4) 102.1(5) 1_555 1_555 1_555 ? C(1) S(8) C(2) 100.7(6) 1_555 1_555 1_555 ? C(14) S(9) C(18) 95.0(4) 1_555 1_555 1_555 ? C(13) S(10) C(19) 94.0(4) 1_555 1_555 1_555 ? C(19) S(11) C(20) 104.3(4) 1_555 1_555 1_555 ? C(11) S(12) C(12) 105.4(4) 1_555 1_555 1_555 ? C(12) S(13) C(13) 93.4(4) 1_555 1_555 1_555 ? C(14) S(14) C(15) 94.6(4) 1_555 1_555 1_555 ? C(15) S(15) C(16) 103.8(5) 1_555 1_555 1_555 ? C(17) S(16) C(18) 102.2(5) 1_555 1_555 1_555 ? C(25) S(17) C(28) 95.1(4) 1_555 1_555 1_555 ? C(24) S(18) C(30) 95.1(4) 1_555 1_555 1_555 ? C(30) S(19) C(31) 104.7(4) 1_555 1_555 1_555 ? C(22) S(20) C(23) 100.9(4) 1_555 1_555 1_555 ? C(23) S(21) C(24) 96.4(4) 1_555 1_555 1_555 ? C(25) S(22) C(26) 95.5(4) 1_555 1_555 1_555 ? C(26) S(23) C(27) 102.9(4) 1_555 1_555 1_555 ? C(28) S(24) C(29) 102.1(4) 1_555 1_555 1_555 ? S(1) C(2) S(8) 119.5(6) 1_555 1_555 1_555 ? S(1) C(2) C(3) 116.8(7) 1_555 1_555 1_555 ? S(8) C(2) C(3) 123.0(7) 1_555 1_555 1_555 ? S(6) C(3) S(7) 120.4(5) 1_555 1_555 1_555 ? S(6) C(3) C(2) 116.6(7) 1_555 1_555 1_555 ? S(7) C(3) C(2) 122.9(7) 1_555 1_555 1_555 ? S(1) C(5) S(6) 113.6(5) 1_555 1_555 1_555 ? S(1) C(5) C(6) 122.6(7) 1_555 1_555 1_555 ? S(6) C(5) C(6) 123.8(7) 1_555 1_555 1_555 ? S(2) C(6) S(5) 113.2(5) 1_555 1_555 1_555 ? S(2) C(6) C(5) 123.2(7) 1_555 1_555 1_555 ? S(5) C(6) C(5) 123.5(7) 1_555 1_555 1_555 ? S(2) C(7) S(3) 117.4(6) 1_555 1_555 1_555 ? S(2) C(7) C(8) 117.1(6) 1_555 1_555 1_555 ? S(3) C(7) C(8) 125.1(7) 1_555 1_555 1_555 ? S(4) C(8) S(5) 118.5(5) 1_555 1_555 1_555 ? S(4) C(8) C(7) 123.9(7) 1_555 1_555 1_555 ? S(5) C(8) C(7) 117.2(7) 1_555 1_555 1_555 ? S(3) C(9) C(10) 112.5(7) 1_555 1_555 1_555 ? C(9) C(10) C(11) 108.7(8) 1_555 1_555 1_555 ? S(12) C(11) C(10) 112.7(6) 1_555 1_555 1_555 ? S(12) C(12) S(13) 120.4(5) 1_555 1_555 1_555 ? S(12) C(12) C(19) 121.8(6) 1_555 1_555 1_555 ? S(13) C(12) C(19) 117.2(6) 1_555 1_555 1_555 ? S(10) C(13) S(13) 113.4(4) 1_555 1_555 1_555 ? S(10) C(13) C(14) 121.4(7) 1_555 1_555 1_555 ? S(13) C(13) C(14) 125.2(7) 1_555 1_555 1_555 ? S(9) C(14) S(14) 113.5(4) 1_555 1_555 1_555 ? S(9) C(14) C(13) 123.2(7) 1_555 1_555 1_555 ? S(14) C(14) C(13) 123.3(7) 1_555 1_555 1_555 ? S(14) C(15) S(15) 118.4(5) 1_555 1_555 1_555 ? S(14) C(15) C(18) 116.8(6) 1_555 1_555 1_555 ? S(15) C(15) C(18) 124.3(6) 1_555 1_555 1_555 ? S(9) C(18) S(16) 117.9(5) 1_555 1_555 1_555 ? S(9) C(18) C(15) 116.5(6) 1_555 1_555 1_555 ? S(16) C(18) C(15) 125.1(7) 1_555 1_555 1_555 ? S(10) C(19) S(11) 115.7(5) 1_555 1_555 1_555 ? S(10) C(19) C(12) 116.5(6) 1_555 1_555 1_555 ? S(11) C(19) C(12) 127.6(6) 1_555 1_555 1_555 ? S(11) C(20) C(21) 115.0(6) 1_555 1_555 1_555 ? C(20) C(21) C(22) 111.8(7) 1_555 1_555 1_555 ? S(20) C(22) C(21) 112.3(6) 1_555 1_555 1_555 ? S(20) C(23) S(21) 116.9(5) 1_555 1_555 1_555 ? S(20) C(23) C(30) 126.6(6) 1_555 1_555 1_555 ? S(21) C(23) C(30) 116.2(6) 1_555 1_555 1_555 ? S(18) C(24) S(21) 115.0(5) 1_555 1_555 1_555 ? S(18) C(24) C(25) 122.8(7) 1_555 1_555 1_555 ? S(21) C(24) C(25) 122.2(7) 1_555 1_555 1_555 ? S(17) C(25) S(22) 115.8(4) 1_555 1_555 1_555 ? S(17) C(25) C(24) 122.9(7) 1_555 1_555 1_555 ? S(22) C(25) C(24) 121.3(7) 1_555 1_555 1_555 ? S(22) C(26) S(23) 120.8(5) 1_555 1_555 1_555 ? S(22) C(26) C(28) 116.2(6) 1_555 1_555 1_555 ? S(23) C(26) C(28) 122.7(6) 1_555 1_555 1_555 ? S(17) C(28) S(24) 119.8(5) 1_555 1_555 1_555 ? S(17) C(28) C(26) 116.9(6) 1_555 1_555 1_555 ? S(24) C(28) C(26) 123.2(6) 1_555 1_555 1_555 ? S(18) C(30) S(19) 120.9(5) 1_555 1_555 1_555 ? S(18) C(30) C(23) 117.3(6) 1_555 1_555 1_555 ? S(19) C(30) C(23) 121.8(6) 1_555 1_555 1_555 ? S(19) C(31) C(32) 113.6(6) 1_555 1_555 1_555 ? C(31) C(32) C(33) 105.8(8) 1_555 1_555 1_555 ? S(4) C(33) C(32) 113.3(7) 1_555 1_555 1_555 ? Cl(1) C(34) C(35) 118(1) 1_555 1_555 1_555 ? Cl(2) C(35) C(34) 119(1) 1_555 1_555 1_555 ? Cl(3) C(36) C(36) 125(2) 1_555 1_555 2_757 ? #------------------------------------------------------------------------------ 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) 2.872(2) . . ? I(1) Br(2) 2.843(2) . . ? Cl(1) S(12) 3.489(4) . . ? Cl(2) S(19) 3.536(4) . . ? S(6) C(22) 3.539(10) . 1_556 ? S(14) C(4) 3.56(1) . 1_454 ? S(16) S(23) 3.473(3) . 2_564 ? S(17) S(21) 3.361(3) . 2_665 ? S(18) S(22) 3.472(3) . 2_665 ? S(20) S(24) 3.577(4) . 2_665 ? C(1) C(4) 3.52(2) . 2_756 ? C(24) C(25) 3.40(1) . 2_665 ? #------------------------------------------------------------------------------ data_TTFtrimerI3 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C39 H42 Cl3 I3 S24 ' _chemical_formula_moiety '?' _chemical_formula_weight 1767.27 _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 13.653(2) _cell_length_b 20.303(3) _cell_length_c 12.677(1) _cell_angle_alpha 104.622(10) _cell_angle_beta 116.501(7) _cell_angle_gamma 81.65(1) _cell_volume 3040.8(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 12.7 _cell_measurement_theta_max 14.8 _cell_measurement_temperature 196.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.930 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.530 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.442 _exptl_absorpt_correction_T_max 0.603 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 14557 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 500 _diffrn_standards_decay_% 1.07 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 14557 _reflns_number_observed 13972 _reflns_observed_criterion >2.0sigma(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.00730 _refine_ls_wR_factor_obs 0.0793 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6563 _refine_ls_number_parameters 595 _refine_ls_goodness_of_fit_all 1.690 _refine_ls_weighting_scheme unit _refine_ls_shift/esd_max 0.1130 _refine_diff_density_max 2.02 _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) ; 'S' 'S' 0.125 0.123 ;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) ; 'Cl' 'Cl' 0.148 0.159 ;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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.2287(1) 0.38291(6) 0.1637(1) 0.0413(3) Uani 1.00 d . . . I(2) I 0.3594(1) 0.50629(7) 0.2757(1) 0.0547(4) Uani 1.00 d . . . I(3) I 0.0941(1) 0.26568(8) 0.0589(1) 0.0558(4) Uani 1.00 d . . . Cl(1) Cl 0.6771(4) 0.0118(3) 0.2613(5) 0.062(2) Uani 1.00 d . . . Cl(2) Cl 0.8504(5) 0.1972(3) 0.4444(5) 0.066(2) Uani 1.00 d . . . Cl(3) Cl 1.0060(5) 0.1066(3) 0.0658(7) 0.085(2) Uani 1.00 d . . . S(1) S 0.8516(3) 0.1408(2) 1.7253(4) 0.031(1) Uani 1.00 d . . . S(2) S 0.6223(3) 0.2323(2) 1.6185(4) 0.032(1) Uani 1.00 d . . . S(3) S 0.4318(4) 0.3165(2) 1.4721(5) 0.049(1) Uani 1.00 d . . . S(4) S 0.2971(4) 0.1730(3) 1.3449(4) 0.042(1) Uani 1.00 d . . . S(5) S 0.4998(3) 0.1060(2) 1.5077(4) 0.030(1) Uani 1.00 d . . . S(6) S 0.7244(3) 0.0168(2) 1.6209(4) 0.033(1) Uani 1.00 d . . . S(7) S 0.9191(4) -0.0750(2) 1.6203(6) 0.065(2) Uani 1.00 d . . . S(8) S 1.0620(4) 0.0621(2) 1.7382(6) 0.059(2) Uani 1.00 d . . . S(9) S 0.3730(3) 0.4536(2) 0.7523(3) 0.0255(10) Uani 1.00 d . . . S(10) S 0.5869(3) 0.3729(2) 0.9076(3) 0.0251(9) Uani 1.00 d . . . S(11) S 0.7938(3) 0.2968(2) 1.0321(4) 0.0269(10) Uani 1.00 d . . . S(12) S 0.7063(3) 0.3069(2) 1.2420(4) 0.034(1) Uani 1.00 d . . . S(13) S 0.5112(3) 0.3895(2) 1.0942(3) 0.0244(9) Uani 1.00 d . . . S(14) S 0.2975(3) 0.4764(2) 0.9399(3) 0.0242(9) Uani 1.00 d . . . S(15) S 0.0832(3) 0.5435(2) 0.7941(4) 0.036(1) Uani 1.00 d . . . S(16) S 0.1644(4) 0.5131(2) 0.5801(4) 0.037(1) Uani 1.00 d . . . S(17) S 0.1547(3) 0.3220(2) 0.8095(3) 0.0258(9) Uani 1.00 d . . . S(18) S 0.3680(3) 0.2255(2) 0.9543(3) 0.0242(9) Uani 1.00 d . . . S(19) S 0.5061(3) 0.1012(2) 1.0384(3) 0.029(1) Uani 1.00 d . . . S(20) S 0.5748(3) 0.0841(2) 0.8108(3) 0.0259(10) Uani 1.00 d . . . S(21) S 0.4354(3) 0.2098(2) 0.7590(3) 0.0261(10) Uani 1.00 d . . . S(22) S 0.2254(3) 0.2989(2) 0.6154(3) 0.0253(10) Uani 1.00 d . . . S(23) S 0.0065(4) 0.3411(2) 0.4358(4) 0.040(1) Uani 1.00 d . . . S(24) S -0.0705(4) 0.3756(2) 0.6591(4) 0.039(1) Uani 1.00 d . . . C(1) C 1.088(1) 0.1485(9) 1.751(2) 0.048(5) Uani 1.00 d . . . C(2) C 0.920(1) 0.0637(8) 1.692(1) 0.030(4) Uani 1.00 d . . . C(3) C 0.865(1) 0.0083(8) 1.645(2) 0.038(5) Uani 1.00 d . . . C(4) C 0.816(2) -0.1126(9) 1.470(2) 0.057(6) Uani 1.00 d . . . C(5) C 0.723(1) 0.1046(7) 1.641(1) 0.023(4) Uani 1.00 d . . . C(6) C 0.628(1) 0.1431(7) 1.594(1) 0.022(4) Uani 1.00 d . . . C(7) C 0.488(1) 0.2356(8) 1.503(1) 0.032(5) Uani 1.00 d . . . C(8) C 0.434(1) 0.1807(8) 1.450(1) 0.032(4) Uani 1.00 d . . . C(9) C 0.539(2) 0.3523(7) 1.456(2) 0.037(5) Uani 1.00 d . . . C(10) C 0.563(1) 0.3147(7) 1.349(1) 0.027(4) Uani 1.00 d . . . C(11) C 0.651(1) 0.3529(8) 1.349(1) 0.032(4) Uani 1.00 d . . . C(12) C 0.635(1) 0.3433(6) 1.118(1) 0.019(3) Uani 1.00 d . . . C(13) C 0.485(1) 0.4047(6) 0.955(1) 0.022(4) Uani 1.00 d . . . C(14) C 0.396(1) 0.4420(6) 0.892(1) 0.022(4) Uani 1.00 d . . . C(15) C 0.208(1) 0.5014(7) 0.806(1) 0.024(4) Uani 1.00 d . . . C(16) C 0.070(1) 0.526(1) 0.918(2) 0.054(6) Uani 1.00 d . . . C(17) C 0.222(1) 0.4612(8) 0.484(1) 0.033(5) Uani 1.00 d . . . C(18) C 0.243(1) 0.4895(6) 0.718(1) 0.022(4) Uani 1.00 d . . . C(19) C 0.670(1) 0.3355(6) 1.031(1) 0.024(4) Uani 1.00 d . . . C(20) C 0.751(1) 0.2091(7) 0.946(1) 0.029(4) Uani 1.00 d . . . C(21) C 0.730(1) 0.1691(7) 1.020(1) 0.024(4) Uani 1.00 d . . . C(22) C 0.704(1) 0.0942(7) 0.954(1) 0.028(4) Uani 1.00 d . . . C(23) C 0.484(1) 0.1465(7) 0.847(1) 0.025(4) Uani 1.00 d . . . C(24) C 0.340(1) 0.2448(6) 0.817(1) 0.020(3) Uani 1.00 d . . . C(25) C 0.250(1) 0.2823(6) 0.754(1) 0.019(3) Uani 1.00 d . . . C(26) C 0.087(1) 0.3243(7) 0.579(1) 0.027(4) Uani 1.00 d . . . C(27) C 0.030(2) 0.264(1) 0.338(2) 0.059(6) Uani 1.00 d . . . C(28) C 0.054(1) 0.3362(7) 0.668(1) 0.029(4) Uani 1.00 d . . . C(29) C -0.107(2) 0.330(1) 0.742(2) 0.053(6) Uani 1.00 d . . . C(30) C 0.453(1) 0.1545(7) 0.935(1) 0.020(3) Uani 1.00 d . . . C(31) C 0.394(1) 0.0880(7) 1.070(1) 0.031(4) Uani 1.00 d . . . C(32) C 0.390(1) 0.1400(8) 1.180(1) 0.028(4) Uani 1.00 d . . . C(33) C 0.310(1) 0.1129(8) 1.215(1) 0.029(4) Uani 1.00 d . . . C(34) C 0.757(4) 0.130(2) 0.342(4) 0.23(2) Uani 1.00 d . . . C(35) C 0.770(3) 0.074(1) 0.366(3) 0.13(1) Uani 1.00 d . . . C(36) C 1.019(2) 0.022(1) 0.051(3) 0.11(1) Uani 1.00 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0428(7) 0.0515(7) 0.0342(6) 0.0199(5) 0.0228(5) 0.0164(5) I(2) 0.078(1) 0.0455(7) 0.0455(8) 0.0048(7) 0.0359(7) 0.0035(6) I(3) 0.0508(8) 0.0739(9) 0.0542(8) 0.0014(7) 0.0281(7) 0.0228(7) Cl(1) 0.049(3) 0.048(3) 0.073(4) -0.010(2) 0.004(3) 0.021(3) Cl(2) 0.086(4) 0.044(3) 0.050(3) -0.011(3) 0.012(3) 0.007(2) Cl(3) 0.046(3) 0.059(4) 0.131(6) 0.000(3) 0.018(4) 0.025(4) S(1) 0.025(2) 0.020(2) 0.046(2) 0.002(2) 0.017(2) 0.003(2) S(2) 0.035(2) 0.024(2) 0.041(2) 0.004(2) 0.019(2) 0.013(2) S(3) 0.056(3) 0.043(3) 0.075(3) 0.033(2) 0.048(3) 0.037(2) S(4) 0.028(2) 0.066(3) 0.036(2) 0.015(2) 0.019(2) 0.016(2) S(5) 0.025(2) 0.029(2) 0.037(2) 0.002(2) 0.013(2) 0.011(2) S(6) 0.029(2) 0.024(2) 0.057(3) 0.000(2) 0.023(2) 0.013(2) S(7) 0.044(3) 0.021(2) 0.117(5) 0.008(2) 0.030(3) 0.005(3) S(8) 0.029(3) 0.040(3) 0.119(5) 0.004(2) 0.040(3) 0.016(3) S(9) 0.029(2) 0.019(2) 0.031(2) 0.005(1) 0.015(2) 0.006(1) S(10) 0.029(2) 0.022(2) 0.029(2) 0.007(1) 0.016(2) 0.010(1) S(11) 0.017(2) 0.025(2) 0.040(2) 0.002(1) 0.011(2) 0.010(2) S(12) 0.039(2) 0.036(2) 0.034(2) 0.014(2) 0.019(2) 0.018(2) S(13) 0.028(2) 0.023(2) 0.028(2) 0.004(1) 0.016(2) 0.008(1) S(14) 0.026(2) 0.021(2) 0.029(2) 0.002(1) 0.015(2) 0.005(1) S(15) 0.027(2) 0.035(2) 0.054(3) 0.013(2) 0.022(2) 0.021(2) S(16) 0.039(2) 0.037(2) 0.032(2) 0.018(2) 0.015(2) 0.016(2) S(17) 0.024(2) 0.020(2) 0.032(2) 0.002(1) 0.011(2) 0.003(1) S(18) 0.027(2) 0.021(2) 0.025(2) 0.004(1) 0.012(2) 0.006(1) S(19) 0.035(2) 0.031(2) 0.032(2) 0.012(2) 0.021(2) 0.017(2) S(20) 0.029(2) 0.024(2) 0.027(2) 0.004(2) 0.016(2) 0.004(1) S(21) 0.022(2) 0.030(2) 0.032(2) 0.007(2) 0.013(2) 0.016(2) S(22) 0.026(2) 0.021(2) 0.031(2) 0.003(1) 0.011(2) 0.010(2) S(23) 0.043(3) 0.030(2) 0.040(2) 0.017(2) 0.011(2) 0.018(2) S(24) 0.033(2) 0.032(2) 0.059(3) 0.014(2) 0.024(2) 0.019(2) C(1) 0.04(1) 0.038(10) 0.06(1) -0.011(8) 0.021(10) -0.007(9) C(2) 0.022(8) 0.032(8) 0.042(9) 0.008(6) 0.018(7) 0.016(7) C(3) 0.026(8) 0.029(9) 0.06(1) 0.011(7) 0.024(8) 0.008(8) C(4) 0.09(2) 0.029(9) 0.06(1) -0.003(10) 0.05(1) 0.001(9) C(5) 0.012(7) 0.025(7) 0.033(8) 0.005(5) 0.006(6) 0.018(6) C(6) 0.014(7) 0.031(8) 0.027(7) 0.004(6) 0.013(6) 0.009(6) C(7) 0.036(9) 0.033(9) 0.040(9) 0.014(7) 0.024(8) 0.020(7) C(8) 0.036(9) 0.038(9) 0.028(8) 0.012(7) 0.021(7) 0.012(7) C(9) 0.07(1) 0.012(7) 0.06(1) 0.006(7) 0.05(1) 0.012(7) C(10) 0.032(8) 0.021(7) 0.023(7) -0.005(6) 0.009(7) 0.001(6) C(11) 0.044(10) 0.030(8) 0.022(7) -0.002(7) 0.016(7) 0.002(6) C(12) 0.020(7) 0.011(6) 0.023(7) -0.003(5) 0.008(6) -0.001(5) C(13) 0.029(8) 0.010(6) 0.024(7) 0.001(5) 0.012(6) -0.003(5) C(14) 0.025(7) 0.013(6) 0.027(7) 0.005(5) 0.013(6) 0.004(6) C(15) 0.010(7) 0.029(8) 0.028(8) -0.001(6) 0.002(6) 0.007(6) C(16) 0.04(1) 0.08(1) 0.06(1) 0.028(10) 0.03(1) 0.04(1) C(17) 0.034(9) 0.040(9) 0.043(9) 0.008(7) 0.028(8) 0.020(8) C(18) 0.021(7) 0.012(6) 0.036(8) 0.001(5) 0.012(6) 0.010(6) C(19) 0.033(8) 0.009(6) 0.030(8) 0.005(6) 0.015(7) 0.003(6) C(20) 0.031(9) 0.023(8) 0.033(8) -0.002(6) 0.013(7) 0.005(6) C(21) 0.028(8) 0.025(7) 0.013(6) -0.007(6) 0.001(6) 0.005(5) C(22) 0.035(9) 0.021(7) 0.028(8) -0.004(6) 0.016(7) -0.003(6) C(23) 0.026(8) 0.024(7) 0.033(8) 0.004(6) 0.019(7) 0.009(6) C(24) 0.024(8) 0.016(6) 0.018(7) -0.007(6) 0.008(6) 0.000(5) C(25) 0.016(7) 0.009(6) 0.026(7) 0.001(5) 0.006(6) -0.001(5) C(26) 0.024(8) 0.013(7) 0.037(9) -0.002(6) 0.005(7) 0.008(6) C(27) 0.06(1) 0.08(1) 0.032(10) 0.02(1) 0.019(10) 0.010(10) C(28) 0.037(9) 0.014(7) 0.036(9) 0.000(6) 0.010(7) 0.013(6) C(29) 0.05(1) 0.06(1) 0.08(1) -0.004(10) 0.05(1) 0.02(1) C(30) 0.022(7) 0.019(7) 0.021(7) 0.000(5) 0.011(6) 0.003(5) C(31) 0.05(1) 0.022(7) 0.038(9) -0.008(7) 0.037(8) 0.001(6) C(32) 0.023(8) 0.041(9) 0.023(7) 0.003(7) 0.015(7) 0.003(7) C(33) 0.024(8) 0.035(8) 0.041(9) -0.006(6) 0.026(7) 0.001(7) C(34) 0.16(4) 0.18(4) 0.21(5) -0.12(4) -0.11(3) 0.09(4) C(35) 0.13(3) 0.05(2) 0.16(3) -0.04(2) 0.02(2) -0.01(2) C(36) 0.07(2) 0.08(2) 0.12(3) -0.01(2) -0.02(2) 0.00(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF92 (PATTY)' _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) I(2) 2.952(2) . . ? I(1) I(3) 2.881(2) . . ? Cl(1) C(35) 1.75(3) . . ? Cl(2) C(34) 1.83(3) . . ? Cl(3) C(36) 1.67(3) . . ? S(1) C(2) 1.76(1) . . ? S(1) C(5) 1.76(1) . . ? S(2) C(6) 1.75(1) . . ? S(2) C(7) 1.77(2) . . ? S(3) C(7) 1.77(1) . . ? S(3) C(9) 1.83(2) . . ? S(4) C(8) 1.75(2) . . ? S(4) C(33) 1.85(1) . . ? S(5) C(6) 1.76(1) . . ? S(5) C(8) 1.79(2) . . ? S(6) C(3) 1.79(2) . . ? S(6) C(5) 1.73(1) . . ? S(7) C(3) 1.76(2) . . ? S(7) C(4) 1.84(2) . . ? S(8) C(1) 1.79(2) . . ? S(8) C(2) 1.76(1) . . ? S(9) C(14) 1.72(1) . . ? S(9) C(18) 1.72(1) . . ? S(10) C(13) 1.74(1) . . ? S(10) C(19) 1.76(1) . . ? S(11) C(19) 1.75(1) . . ? S(11) C(20) 1.86(1) . . ? S(12) C(11) 1.83(1) . . ? S(12) C(12) 1.72(1) . . ? S(13) C(12) 1.75(1) . . ? S(13) C(13) 1.74(1) . . ? S(14) C(14) 1.71(1) . . ? S(14) C(15) 1.74(1) . . ? S(15) C(15) 1.75(1) . . ? S(15) C(16) 1.79(2) . . ? S(16) C(17) 1.78(2) . . ? S(16) C(18) 1.75(1) . . ? S(17) C(25) 1.75(1) . . ? S(17) C(28) 1.77(2) . . ? S(18) C(24) 1.75(1) . . ? S(18) C(30) 1.75(1) . . ? S(19) C(30) 1.74(1) . . ? S(19) C(31) 1.81(1) . . ? S(20) C(22) 1.87(2) . . ? S(20) C(23) 1.77(1) . . ? S(21) C(23) 1.77(1) . . ? S(21) C(24) 1.74(1) . . ? S(22) C(25) 1.75(1) . . ? S(22) C(26) 1.77(1) . . ? S(23) C(26) 1.75(2) . . ? S(23) C(27) 1.82(2) . . ? S(24) C(28) 1.74(2) . . ? S(24) C(29) 1.83(2) . . ? C(2) C(3) 1.30(2) . . ? C(5) C(6) 1.37(2) . . ? C(7) C(8) 1.29(2) . . ? C(9) C(10) 1.54(2) . . ? C(10) C(11) 1.52(2) . . ? C(12) C(19) 1.36(2) . . ? C(13) C(14) 1.36(2) . . ? C(15) C(18) 1.36(2) . . ? C(20) C(21) 1.53(2) . . ? C(21) C(22) 1.55(2) . . ? C(23) C(30) 1.33(2) . . ? C(24) C(25) 1.37(2) . . ? C(26) C(28) 1.34(2) . . ? C(31) C(32) 1.54(2) . . ? C(32) C(33) 1.55(2) . . ? C(34) C(35) 1.22(4) . . ? C(36) C(36) 1.30(5) . 2_755 ? #------------------------------------------------------------------------------ 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 I(2) I(1) I(3) 177.35(6) 1_555 1_555 1_555 ? C(2) S(1) C(5) 92.4(7) 1_555 1_555 1_555 ? C(6) S(2) C(7) 93.6(7) 1_555 1_555 1_555 ? C(7) S(3) C(9) 103.6(7) 1_555 1_555 1_555 ? C(8) S(4) C(33) 101.3(7) 1_555 1_555 1_555 ? C(6) S(5) C(8) 93.9(7) 1_555 1_555 1_555 ? C(3) S(6) C(5) 92.3(7) 1_555 1_555 1_555 ? C(3) S(7) C(4) 101.7(9) 1_555 1_555 1_555 ? C(1) S(8) C(2) 103.3(8) 1_555 1_555 1_555 ? C(14) S(9) C(18) 95.6(7) 1_555 1_555 1_555 ? C(13) S(10) C(19) 96.6(7) 1_555 1_555 1_555 ? C(19) S(11) C(20) 101.3(7) 1_555 1_555 1_555 ? C(11) S(12) C(12) 103.7(7) 1_555 1_555 1_555 ? C(12) S(13) C(13) 97.1(6) 1_555 1_555 1_555 ? C(14) S(14) C(15) 95.4(7) 1_555 1_555 1_555 ? C(15) S(15) C(16) 102.3(7) 1_555 1_555 1_555 ? C(17) S(16) C(18) 103.3(7) 1_555 1_555 1_555 ? C(25) S(17) C(28) 94.8(7) 1_555 1_555 1_555 ? C(24) S(18) C(30) 93.5(6) 1_555 1_555 1_555 ? C(30) S(19) C(31) 105.8(7) 1_555 1_555 1_555 ? C(22) S(20) C(23) 103.7(7) 1_555 1_555 1_555 ? C(23) S(21) C(24) 93.4(6) 1_555 1_555 1_555 ? C(25) S(22) C(26) 93.8(7) 1_555 1_555 1_555 ? C(26) S(23) C(27) 102.3(8) 1_555 1_555 1_555 ? C(28) S(24) C(29) 102.5(8) 1_555 1_555 1_555 ? S(1) C(2) S(8) 119.5(9) 1_555 1_555 1_555 ? S(1) C(2) C(3) 118(1) 1_555 1_555 1_555 ? S(8) C(2) C(3) 122(1) 1_555 1_555 1_555 ? S(6) C(3) S(7) 116.8(10) 1_555 1_555 1_555 ? S(6) C(3) C(2) 116(1) 1_555 1_555 1_555 ? S(7) C(3) C(2) 125(1) 1_555 1_555 1_555 ? S(1) C(5) S(6) 114.7(7) 1_555 1_555 1_555 ? S(1) C(5) C(6) 122(1) 1_555 1_555 1_555 ? S(6) C(5) C(6) 122(1) 1_555 1_555 1_555 ? S(2) C(6) S(5) 114.0(7) 1_555 1_555 1_555 ? S(2) C(6) C(5) 124(1) 1_555 1_555 1_555 ? S(5) C(6) C(5) 121(1) 1_555 1_555 1_555 ? S(2) C(7) S(3) 117.3(10) 1_555 1_555 1_555 ? S(2) C(7) C(8) 119(1) 1_555 1_555 1_555 ? S(3) C(7) C(8) 123(1) 1_555 1_555 1_555 ? S(4) C(8) S(5) 115.7(10) 1_555 1_555 1_555 ? S(4) C(8) C(7) 127(1) 1_555 1_555 1_555 ? S(5) C(8) C(7) 116(1) 1_555 1_555 1_555 ? S(3) C(9) C(10) 115(1) 1_555 1_555 1_555 ? C(9) C(10) C(11) 107(1) 1_555 1_555 1_555 ? S(12) C(11) C(10) 112(1) 1_555 1_555 1_555 ? S(12) C(12) S(13) 122.3(8) 1_555 1_555 1_555 ? S(12) C(12) C(19) 121(1) 1_555 1_555 1_555 ? S(13) C(12) C(19) 116(1) 1_555 1_555 1_555 ? S(10) C(13) S(13) 113.7(8) 1_555 1_555 1_555 ? S(10) C(13) C(14) 122(1) 1_555 1_555 1_555 ? S(13) C(13) C(14) 123(1) 1_555 1_555 1_555 ? S(9) C(14) S(14) 115.5(8) 1_555 1_555 1_555 ? S(9) C(14) C(13) 121(1) 1_555 1_555 1_555 ? S(14) C(14) C(13) 123(1) 1_555 1_555 1_555 ? S(14) C(15) S(15) 119.8(8) 1_555 1_555 1_555 ? S(14) C(15) C(18) 116(1) 1_555 1_555 1_555 ? S(15) C(15) C(18) 123(1) 1_555 1_555 1_555 ? S(9) C(18) S(16) 121.1(8) 1_555 1_555 1_555 ? S(9) C(18) C(15) 116(1) 1_555 1_555 1_555 ? S(16) C(18) C(15) 122(1) 1_555 1_555 1_555 ? S(10) C(19) S(11) 116.1(8) 1_555 1_555 1_555 ? S(10) C(19) C(12) 116(1) 1_555 1_555 1_555 ? S(11) C(19) C(12) 127(1) 1_555 1_555 1_555 ? S(11) C(20) C(21) 111.4(10) 1_555 1_555 1_555 ? C(20) C(21) C(22) 111(1) 1_555 1_555 1_555 ? S(20) C(22) C(21) 113.8(10) 1_555 1_555 1_555 ? S(20) C(23) S(21) 114.8(7) 1_555 1_555 1_555 ? S(20) C(23) C(30) 128(1) 1_555 1_555 1_555 ? S(21) C(23) C(30) 116(1) 1_555 1_555 1_555 ? S(18) C(24) S(21) 114.6(8) 1_555 1_555 1_555 ? S(18) C(24) C(25) 124(1) 1_555 1_555 1_555 ? S(21) C(24) C(25) 121(1) 1_555 1_555 1_555 ? S(17) C(25) S(22) 114.0(7) 1_555 1_555 1_555 ? S(17) C(25) C(24) 123(1) 1_555 1_555 1_555 ? S(22) C(25) C(24) 122(1) 1_555 1_555 1_555 ? S(22) C(26) S(23) 117.2(9) 1_555 1_555 1_555 ? S(22) C(26) C(28) 117(1) 1_555 1_555 1_555 ? S(23) C(26) C(28) 124(1) 1_555 1_555 1_555 ? S(17) C(28) S(24) 118.8(9) 1_555 1_555 1_555 ? S(17) C(28) C(26) 115(1) 1_555 1_555 1_555 ? S(24) C(28) C(26) 124(1) 1_555 1_555 1_555 ? S(18) C(30) S(19) 120.9(7) 1_555 1_555 1_555 ? S(18) C(30) C(23) 117(1) 1_555 1_555 1_555 ? S(19) C(30) C(23) 120(1) 1_555 1_555 1_555 ? S(19) C(31) C(32) 112(1) 1_555 1_555 1_555 ? C(31) C(32) C(33) 106(1) 1_555 1_555 1_555 ? S(4) C(33) C(32) 110.4(10) 1_555 1_555 1_555 ? Cl(2) C(34) C(35) 119(2) 1_555 1_555 1_555 ? Cl(1) C(35) C(34) 116(3) 1_555 1_555 1_555 ? Cl(3) C(36) C(36) 124(3) 1_555 1_555 2_755 ? #------------------------------------------------------------------------------ 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) I(2) 2.952(2) . . ? I(1) I(3) 2.881(2) . . ? Cl(1) S(19) 3.493(6) . 1_554 ? Cl(2) S(12) 3.538(6) . 1_554 ? S(1) C(20) 3.55(2) . 1_556 ? S(9) S(13) 3.467(5) . 2_667 ? S(10) S(14) 3.359(5) . 2_667 ? S(11) S(15) 3.585(6) . 2_667 ? S(16) S(23) 3.481(5) . 2_566 ? S(17) C(1) 3.58(2) . 1_454 ? C(1) C(4) 3.49(3) . 2_758 ? C(13) C(14) 3.42(2) . 2_667 ? C(14) C(14) 3.59(3) . 2_667 ? #------------------------------------------------------------------------------