# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Takanori Suzuki' _publ_contact_author_address ; Division of Chemistry, Graduate School of Science Hokkaido University Kita-ku Kita 10, Nishi 8 Sapporo 060-0810 JAPAN ; _publ_contact_author_email TAK@SCI.HOKUDAI.AC.JP _publ_section_title ; Butane-1,4-diyl dications stabilized by steric factors: electrochiroptical response systems based on reversible interconversion between dihydro[5]helicene-type electron acceptors and electron-donating 1,1'-binaphthyls ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; loop_ _publ_author_name 'Takanori Suzuki' 'Kenshu Fujiwara' 'Hiroki Higuchi' 'Hidetoshi Kawai' 'Eisuke Ohta' #------------------------------------------------------------------------------ data__030703B _database_code_depnum_ccdc_archive 'CCDC 270835' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C58 H48 O4 ' _chemical_formula_moiety ? _chemical_formula_weight 809.01 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 10.54(2) _cell_length_b 25.92(2) _cell_length_c 16.25(1) _cell_angle_alpha 90 _cell_angle_beta 100.15(2) _cell_angle_gamma 90 _cell_volume 4367.7(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 339 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 29.6 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description Prism _exptl_crystal_colour Colorless _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 1.230 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.985 _exptl_absorpt_correction_T_max 0.985 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 27052 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9323 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9323 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9355 _reflns_number_gt 7473 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1093 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9350 _refine_ls_number_parameters 559 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0091 _refine_diff_density_max 0.23 _refine_diff_density_min -0.23 _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) ; O O 0.011 0.006 ;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 O(1) O 1.30877(9) 0.34324(4) 1.06890(6) 0.0385(3) Uani 1.00 d . . . O(2) O 0.49040(10) 0.50375(4) 0.86735(6) 0.0373(3) Uani 1.00 d . . . O(3) O 0.31889(9) 0.46121(4) 0.49107(6) 0.0364(3) Uani 1.00 d . . . O(4) O 1.18115(9) 0.34986(4) 0.65709(6) 0.0406(3) Uani 1.00 d . . . C(1) C 0.5511(1) 0.21825(5) 0.83530(7) 0.0209(3) Uani 1.00 d . . . C(2) C 0.5929(1) 0.25764(5) 0.89121(8) 0.0220(3) Uani 1.00 d . . . C(3) C 0.5017(1) 0.28229(5) 0.93338(9) 0.0294(4) Uani 1.00 d . . . C(4) C 0.3761(1) 0.26827(5) 0.91976(9) 0.0332(4) Uani 1.00 d . . . C(5) C 0.3309(1) 0.22762(5) 0.86465(8) 0.0290(4) Uani 1.00 d . . . C(6) C 0.2008(1) 0.21113(6) 0.85197(10) 0.0386(4) Uani 1.00 d . . . C(7) C 0.1596(1) 0.17122(7) 0.80010(10) 0.0430(5) Uani 1.00 d . . . C(8) C 0.2461(2) 0.14588(6) 0.75765(10) 0.0427(5) Uani 1.00 d . . . C(9) C 0.3723(1) 0.16085(6) 0.76769(8) 0.0327(4) Uani 1.00 d . . . C(10) C 0.4191(1) 0.20200(5) 0.82183(8) 0.0244(3) Uani 1.00 d . . . C(11) C 0.6441(1) 0.19316(5) 0.78743(7) 0.0206(3) Uani 1.00 d . . . C(12) C 0.6734(1) 0.21684(5) 0.71666(8) 0.0221(3) Uani 1.00 d . . . C(13) C 0.7647(1) 0.19316(5) 0.67371(8) 0.0258(3) Uani 1.00 d . . . C(14) C 0.8276(1) 0.14926(5) 0.70236(8) 0.0253(3) Uani 1.00 d . . . C(15) C 0.8012(1) 0.12432(5) 0.77514(8) 0.0223(3) Uani 1.00 d . . . C(16) C 0.8653(1) 0.07846(5) 0.80651(8) 0.0273(3) Uani 1.00 d . . . C(17) C 0.8320(1) 0.05341(5) 0.87324(8) 0.0313(4) Uani 1.00 d . . . C(18) C 0.7336(1) 0.07307(5) 0.91230(8) 0.0302(4) Uani 1.00 d . . . C(19) C 0.6724(1) 0.11813(5) 0.88557(8) 0.0253(3) Uani 1.00 d . . . C(20) C 0.7051(1) 0.14569(5) 0.81675(7) 0.0211(3) Uani 1.00 d . . . C(21) C 0.7302(1) 0.27185(5) 0.91346(7) 0.0229(3) Uani 1.00 d . . . C(22) C 0.7794(1) 0.31932(5) 0.93237(8) 0.0225(3) Uani 1.00 d . . . C(23) C 0.9184(1) 0.32650(5) 0.96793(8) 0.0232(3) Uani 1.00 d . . . C(24) C 0.9855(1) 0.36989(5) 0.94840(9) 0.0297(4) Uani 1.00 d . . . C(25) C 1.1154(1) 0.37685(5) 0.98087(9) 0.0320(4) Uani 1.00 d . . . C(26) C 1.1807(1) 0.34048(6) 1.03424(8) 0.0295(4) Uani 1.00 d . . . C(27) C 1.1156(1) 0.29697(5) 1.05505(8) 0.0309(4) Uani 1.00 d . . . C(28) C 0.9871(1) 0.29033(5) 1.02219(8) 0.0265(3) Uani 1.00 d . . . C(29) C 1.3796(1) 0.38671(7) 1.0490(1) 0.0499(5) Uani 1.00 d . . . C(30) C 0.7007(1) 0.36720(5) 0.91522(8) 0.0228(3) Uani 1.00 d . . . C(31) C 0.6297(1) 0.37637(5) 0.83615(8) 0.0269(3) Uani 1.00 d . . . C(32) C 0.5585(1) 0.42127(5) 0.81747(8) 0.0280(3) Uani 1.00 d . . . C(33) C 0.5570(1) 0.45785(5) 0.87922(8) 0.0261(3) Uani 1.00 d . . . C(34) C 0.6258(1) 0.44937(5) 0.95917(8) 0.0280(3) Uani 1.00 d . . . C(35) C 0.6974(1) 0.40482(5) 0.97637(8) 0.0256(3) Uani 1.00 d . . . C(36) C 0.4396(2) 0.51799(6) 0.7836(1) 0.0454(5) Uani 1.00 d . . . C(37) C 0.6047(1) 0.26381(5) 0.68188(8) 0.0246(3) Uani 1.00 d . . . C(38) C 0.6534(1) 0.30498(5) 0.64722(8) 0.0236(3) Uani 1.00 d . . . C(39) C 0.5650(1) 0.34556(5) 0.60503(7) 0.0230(3) Uani 1.00 d . . . C(40) C 0.4459(1) 0.33270(5) 0.55819(8) 0.0287(3) Uani 1.00 d . . . C(41) C 0.3611(1) 0.36991(5) 0.51899(8) 0.0302(4) Uani 1.00 d . . . C(42) C 0.3949(1) 0.42140(5) 0.52714(8) 0.0273(3) Uani 1.00 d . . . C(43) C 0.5137(1) 0.43545(5) 0.57322(8) 0.0281(3) Uani 1.00 d . . . C(44) C 0.5970(1) 0.39796(5) 0.61093(8) 0.0269(3) Uani 1.00 d . . . C(45) C 0.1939(2) 0.44874(6) 0.4472(1) 0.0517(5) Uani 1.00 d . . . C(46) C 0.7937(1) 0.31445(5) 0.65165(8) 0.0238(3) Uani 1.00 d . . . C(47) C 0.8830(1) 0.30618(5) 0.72443(8) 0.0273(3) Uani 1.00 d . . . C(48) C 1.0132(1) 0.31683(5) 0.72861(8) 0.0298(4) Uani 1.00 d . . . C(49) C 1.0561(1) 0.33651(5) 0.65911(8) 0.0285(4) Uani 1.00 d . . . C(50) C 0.9688(1) 0.34516(5) 0.58607(8) 0.0297(4) Uani 1.00 d . . . C(51) C 0.8398(1) 0.33430(5) 0.58264(8) 0.0269(3) Uani 1.00 d . . . C(52) C 1.2764(1) 0.33609(7) 0.7269(1) 0.0457(5) Uani 1.00 d . . . C(53) C 0.8634(2) 0.48389(7) 0.7837(1) 0.0496(5) Uani 1.00 d . . . C(54) C 0.9508(2) 0.45697(6) 0.7470(1) 0.0431(5) Uani 1.00 d . . . C(55) C 1.0798(2) 0.45855(6) 0.7808(1) 0.0445(5) Uani 1.00 d . . . C(56) C 1.1216(2) 0.48751(7) 0.8518(1) 0.0507(5) Uani 1.00 d . . . C(57) C 1.0348(2) 0.51395(7) 0.8891(1) 0.0560(6) Uani 1.00 d . . . C(58) C 0.9058(2) 0.51240(7) 0.8554(1) 0.0559(6) Uani 1.00 d . . . H(1) H 0.5303 0.3092 0.9721 0.0340 Uiso 1.00 calc . . . H(2) H 0.3174 0.2860 0.9481 0.0386 Uiso 1.00 calc . . . H(3) H 0.1415 0.2284 0.8805 0.0451 Uiso 1.00 calc . . . H(4) H 0.0720 0.1605 0.7925 0.0506 Uiso 1.00 calc . . . H(5) H 0.2163 0.1180 0.7210 0.0500 Uiso 1.00 calc . . . H(6) H 0.4299 0.1432 0.7381 0.0386 Uiso 1.00 calc . . . H(7) H 0.7819 0.2086 0.6235 0.0298 Uiso 1.00 calc . . . H(8) H 0.8904 0.1350 0.6733 0.0292 Uiso 1.00 calc . . . H(9) H 0.9324 0.0650 0.7803 0.0318 Uiso 1.00 calc . . . H(10) H 0.8754 0.0227 0.8937 0.0368 Uiso 1.00 calc . . . H(11) H 0.7092 0.0548 0.9580 0.0355 Uiso 1.00 calc . . . H(12) H 0.6067 0.1313 0.9133 0.0293 Uiso 1.00 calc . . . H(13) H 0.7908 0.2445 0.9147 0.0263 Uiso 1.00 calc . . . H(14) H 0.9412 0.3953 0.9121 0.0348 Uiso 1.00 calc . . . H(15) H 1.1596 0.4064 0.9661 0.0381 Uiso 1.00 calc . . . H(16) H 1.1604 0.2717 1.0918 0.0359 Uiso 1.00 calc . . . H(17) H 0.9434 0.2603 1.0368 0.0307 Uiso 1.00 calc . . . H(18) H 1.4664 0.3841 1.0768 0.0596 Uiso 1.00 calc . . . H(19) H 1.3775 0.3877 0.9901 0.0596 Uiso 1.00 calc . . . H(20) H 1.3420 0.4173 1.0658 0.0596 Uiso 1.00 calc . . . H(21) H 0.6295 0.3511 0.7937 0.0313 Uiso 1.00 calc . . . H(22) H 0.5113 0.4269 0.7626 0.0324 Uiso 1.00 calc . . . H(23) H 0.6237 0.4742 1.0020 0.0328 Uiso 1.00 calc . . . H(24) H 0.7451 0.3996 1.0313 0.0305 Uiso 1.00 calc . . . H(25) H 0.3960 0.5501 0.7832 0.0541 Uiso 1.00 calc . . . H(26) H 0.5081 0.5212 0.7528 0.0541 Uiso 1.00 calc . . . H(27) H 0.3810 0.4923 0.7586 0.0541 Uiso 1.00 calc . . . H(28) H 0.5155 0.2654 0.6848 0.0284 Uiso 1.00 calc . . . H(29) H 0.4216 0.2973 0.5526 0.0339 Uiso 1.00 calc . . . H(30) H 0.2802 0.3600 0.4869 0.0359 Uiso 1.00 calc . . . H(31) H 0.5376 0.4709 0.5789 0.0333 Uiso 1.00 calc . . . H(32) H 0.6788 0.4080 0.6417 0.0313 Uiso 1.00 calc . . . H(33) H 0.1515 0.4793 0.4249 0.0620 Uiso 1.00 calc . . . H(34) H 0.2014 0.4256 0.4028 0.0620 Uiso 1.00 calc . . . H(35) H 0.1457 0.4329 0.4843 0.0620 Uiso 1.00 calc . . . H(36) H 0.8538 0.2928 0.7724 0.0317 Uiso 1.00 calc . . . H(37) H 1.0725 0.3104 0.7791 0.0356 Uiso 1.00 calc . . . H(38) H 0.9979 0.3584 0.5377 0.0348 Uiso 1.00 calc . . . H(39) H 0.7806 0.3407 0.5321 0.0315 Uiso 1.00 calc . . . H(40) H 1.2768 0.2996 0.7338 0.0538 Uiso 1.00 calc . . . H(41) H 1.3588 0.3471 0.7179 0.0538 Uiso 1.00 calc . . . H(42) H 1.2572 0.3520 0.7759 0.0538 Uiso 1.00 calc . . . H(43) H 0.7724 0.4833 0.7593 0.0593 Uiso 1.00 calc . . . H(44) H 0.9212 0.4367 0.6971 0.0514 Uiso 1.00 calc . . . H(45) H 1.1411 0.4393 0.7549 0.0534 Uiso 1.00 calc . . . H(46) H 1.2132 0.4888 0.8748 0.0606 Uiso 1.00 calc . . . H(47) H 1.0645 0.5336 0.9395 0.0656 Uiso 1.00 calc . . . H(48) H 0.8444 0.5313 0.8815 0.0666 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 O(1) 0.0240(5) 0.0539(7) 0.0374(6) -0.0089(5) 0.0049(4) -0.0071(5) O(2) 0.0414(6) 0.0285(5) 0.0392(6) 0.0120(4) -0.0002(5) -0.0005(4) O(3) 0.0333(6) 0.0276(5) 0.0449(6) 0.0056(4) -0.0024(5) 0.0048(4) O(4) 0.0247(5) 0.0518(7) 0.0459(6) -0.0034(5) 0.0083(5) 0.0092(5) C(1) 0.0216(6) 0.0196(6) 0.0218(6) 0.0009(5) 0.0048(5) 0.0040(5) C(2) 0.0246(6) 0.0183(6) 0.0237(6) -0.0003(5) 0.0062(5) 0.0024(5) C(3) 0.0320(7) 0.0242(7) 0.0348(7) -0.0004(6) 0.0131(6) -0.0039(6) C(4) 0.0304(8) 0.0298(7) 0.0432(8) 0.0050(6) 0.0165(6) 0.0005(6) C(5) 0.0224(7) 0.0316(7) 0.0332(7) 0.0016(5) 0.0058(6) 0.0084(6) C(6) 0.0234(7) 0.0478(9) 0.0456(9) 0.0021(7) 0.0086(6) 0.0116(7) C(7) 0.0216(7) 0.060(1) 0.0449(9) -0.0106(7) -0.0002(7) 0.0120(8) C(8) 0.0351(9) 0.053(1) 0.0376(9) -0.0167(7) -0.0012(7) -0.0015(7) C(9) 0.0284(7) 0.0397(8) 0.0290(7) -0.0069(6) 0.0022(6) -0.0002(6) C(10) 0.0226(6) 0.0260(7) 0.0239(6) -0.0011(5) 0.0024(5) 0.0057(5) C(11) 0.0200(6) 0.0193(6) 0.0219(6) -0.0035(5) 0.0022(5) -0.0032(5) C(12) 0.0212(6) 0.0210(6) 0.0238(6) -0.0029(5) 0.0030(5) -0.0017(5) C(13) 0.0277(7) 0.0270(7) 0.0236(7) -0.0030(5) 0.0074(5) -0.0006(5) C(14) 0.0233(7) 0.0258(7) 0.0275(7) -0.0006(5) 0.0062(5) -0.0058(5) C(15) 0.0211(6) 0.0205(6) 0.0243(6) -0.0028(5) 0.0009(5) -0.0058(5) C(16) 0.0256(7) 0.0247(7) 0.0305(7) 0.0020(5) 0.0024(5) -0.0060(5) C(17) 0.0364(8) 0.0221(7) 0.0329(8) 0.0045(6) -0.0004(6) 0.0009(6) C(18) 0.0391(8) 0.0246(7) 0.0265(7) -0.0010(6) 0.0042(6) 0.0029(5) C(19) 0.0295(7) 0.0235(6) 0.0229(7) -0.0018(5) 0.0043(5) -0.0023(5) C(20) 0.0218(6) 0.0190(6) 0.0216(6) -0.0036(5) 0.0014(5) -0.0045(5) C(21) 0.0253(7) 0.0216(6) 0.0227(6) 0.0023(5) 0.0067(5) -0.0004(5) C(22) 0.0252(7) 0.0220(6) 0.0209(6) -0.0001(5) 0.0060(5) 0.0003(5) C(23) 0.0260(7) 0.0207(6) 0.0238(6) -0.0010(5) 0.0070(5) -0.0042(5) C(24) 0.0308(7) 0.0244(7) 0.0341(7) -0.0022(6) 0.0062(6) 0.0026(6) C(25) 0.0319(8) 0.0253(7) 0.0409(8) -0.0084(6) 0.0121(6) -0.0025(6) C(26) 0.0237(7) 0.0382(8) 0.0277(7) -0.0040(6) 0.0077(5) -0.0087(6) C(27) 0.0283(7) 0.0343(8) 0.0302(7) 0.0021(6) 0.0051(6) 0.0046(6) C(28) 0.0269(7) 0.0250(7) 0.0288(7) -0.0020(5) 0.0083(5) 0.0008(5) C(29) 0.0313(9) 0.050(1) 0.070(1) -0.0154(7) 0.0131(8) -0.0193(9) C(30) 0.0243(6) 0.0188(6) 0.0257(7) -0.0020(5) 0.0056(5) 0.0002(5) C(31) 0.0315(7) 0.0232(7) 0.0256(7) -0.0005(5) 0.0038(6) -0.0036(5) C(32) 0.0288(7) 0.0289(7) 0.0247(7) -0.0001(6) 0.0005(5) 0.0005(5) C(33) 0.0228(7) 0.0221(6) 0.0334(7) 0.0016(5) 0.0055(5) -0.0001(5) C(34) 0.0304(7) 0.0242(7) 0.0289(7) 0.0010(5) 0.0042(6) -0.0066(5) C(35) 0.0278(7) 0.0247(7) 0.0236(7) -0.0008(5) 0.0025(5) -0.0001(5) C(36) 0.0461(9) 0.0393(9) 0.0466(9) 0.0159(7) -0.0036(7) 0.0068(7) C(37) 0.0253(7) 0.0254(7) 0.0236(6) 0.0007(5) 0.0058(5) -0.0007(5) C(38) 0.0271(7) 0.0248(7) 0.0195(6) 0.0009(5) 0.0055(5) -0.0020(5) C(39) 0.0268(7) 0.0239(6) 0.0192(6) 0.0011(5) 0.0067(5) 0.0013(5) C(40) 0.0320(7) 0.0225(7) 0.0302(7) -0.0016(5) 0.0016(6) 0.0006(5) C(41) 0.0283(7) 0.0286(7) 0.0310(7) -0.0009(6) -0.0018(6) -0.0005(6) C(42) 0.0299(7) 0.0257(7) 0.0265(7) 0.0045(5) 0.0060(6) 0.0024(5) C(43) 0.0330(7) 0.0212(6) 0.0302(7) -0.0020(6) 0.0063(6) -0.0004(5) C(44) 0.0266(7) 0.0271(7) 0.0267(7) -0.0035(5) 0.0038(5) 0.0003(5) C(45) 0.0419(10) 0.0384(9) 0.066(1) 0.0091(7) -0.0145(8) 0.0042(8) C(46) 0.0278(7) 0.0196(6) 0.0244(6) 0.0011(5) 0.0058(5) 0.0001(5) C(47) 0.0309(7) 0.0264(7) 0.0251(7) 0.0003(5) 0.0064(5) 0.0040(5) C(48) 0.0279(7) 0.0296(7) 0.0303(7) 0.0008(6) 0.0012(6) 0.0040(6) C(49) 0.0255(7) 0.0259(7) 0.0351(8) -0.0001(5) 0.0081(6) 0.0000(6) C(50) 0.0342(8) 0.0287(7) 0.0289(7) 0.0018(6) 0.0128(6) 0.0049(6) C(51) 0.0291(7) 0.0273(7) 0.0242(7) 0.0018(5) 0.0042(5) 0.0025(5) C(52) 0.0266(8) 0.059(1) 0.0497(10) 0.0000(7) 0.0027(7) 0.0007(8) C(53) 0.0415(10) 0.0449(10) 0.063(1) -0.0023(8) 0.0102(8) 0.0050(8) C(54) 0.053(1) 0.0321(8) 0.0437(9) -0.0055(7) 0.0059(8) -0.0004(7) C(55) 0.0488(10) 0.0325(8) 0.054(1) 0.0015(7) 0.0143(8) 0.0080(7) C(56) 0.051(1) 0.049(1) 0.049(1) -0.0142(8) 0.0006(8) 0.0146(8) C(57) 0.083(1) 0.048(1) 0.0371(9) -0.023(1) 0.0124(9) -0.0001(8) C(58) 0.073(1) 0.044(1) 0.058(1) 0.0012(9) 0.032(1) 0.0001(9) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _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 O(1) C(26) 1.369(2) . . yes O(1) C(29) 1.420(2) . . yes O(2) C(33) 1.377(2) . . yes O(2) C(36) 1.420(2) . . yes O(3) C(42) 1.373(2) . . yes O(3) C(45) 1.421(2) . . yes O(4) C(49) 1.368(2) . . yes O(4) C(52) 1.422(2) . . yes C(1) C(2) 1.386(2) . . yes C(1) C(10) 1.433(3) . . yes C(1) C(11) 1.503(2) . . yes C(2) C(3) 1.425(2) . . yes C(2) C(21) 1.475(3) . . yes C(3) C(4) 1.353(3) . . yes C(4) C(5) 1.410(2) . . yes C(5) C(6) 1.416(3) . . yes C(5) C(10) 1.420(2) . . yes C(6) C(7) 1.357(2) . . yes C(7) C(8) 1.400(3) . . yes C(8) C(9) 1.367(3) . . yes C(9) C(10) 1.415(2) . . yes C(11) C(12) 1.385(2) . . yes C(11) C(20) 1.430(2) . . yes C(12) C(13) 1.423(2) . . yes C(12) C(37) 1.477(2) . . yes C(13) C(14) 1.357(2) . . yes C(14) C(15) 1.418(2) . . yes C(15) C(16) 1.417(2) . . yes C(15) C(20) 1.424(2) . . yes C(16) C(17) 1.362(2) . . yes C(17) C(18) 1.403(2) . . yes C(18) C(19) 1.367(2) . . yes C(19) C(20) 1.419(2) . . yes C(21) C(22) 1.349(2) . . yes C(22) C(23) 1.488(3) . . yes C(22) C(30) 1.492(2) . . yes C(23) C(24) 1.395(2) . . yes C(23) C(28) 1.398(2) . . yes C(24) C(25) 1.389(3) . . yes C(25) C(26) 1.380(2) . . yes C(26) C(27) 1.393(2) . . yes C(27) C(28) 1.376(3) . . yes C(30) C(31) 1.388(2) . . yes C(30) C(35) 1.397(2) . . yes C(31) C(32) 1.389(2) . . yes C(32) C(33) 1.383(2) . . yes C(33) C(34) 1.389(2) . . yes C(34) C(35) 1.381(2) . . yes C(37) C(38) 1.349(2) . . yes C(38) C(39) 1.490(2) . . yes C(38) C(46) 1.487(3) . . yes C(39) C(40) 1.389(2) . . yes C(39) C(44) 1.399(2) . . yes C(40) C(41) 1.390(2) . . yes C(41) C(42) 1.382(2) . . yes C(42) C(43) 1.389(2) . . yes C(43) C(44) 1.379(2) . . yes C(46) C(47) 1.392(2) . . yes C(46) C(51) 1.397(2) . . yes C(47) C(48) 1.389(3) . . yes C(48) C(49) 1.386(2) . . yes C(49) C(50) 1.386(2) . . yes C(50) C(51) 1.379(3) . . yes C(53) C(54) 1.373(3) . . yes C(53) C(58) 1.385(3) . . yes C(54) C(55) 1.374(3) . . yes C(55) C(56) 1.382(2) . . yes C(56) C(57) 1.367(3) . . yes C(57) C(58) 1.373(3) . . 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(26) O(1) C(29) 117.8(1) . . . yes C(33) O(2) C(36) 117.1(1) . . . yes C(42) O(3) C(45) 117.6(1) . . . yes C(49) O(4) C(52) 117.7(1) . . . yes C(2) C(1) C(10) 120.3(1) . . . yes C(2) C(1) C(11) 119.8(1) . . . yes C(10) C(1) C(11) 119.9(1) . . . yes C(1) C(2) C(3) 118.8(1) . . . yes C(1) C(2) C(21) 121.9(1) . . . yes C(3) C(2) C(21) 119.0(1) . . . yes C(2) C(3) C(4) 121.6(1) . . . yes C(3) C(4) C(5) 121.1(1) . . . yes C(4) C(5) C(6) 121.9(1) . . . yes C(4) C(5) C(10) 118.9(1) . . . yes C(6) C(5) C(10) 119.2(1) . . . yes C(5) C(6) C(7) 121.1(1) . . . yes C(6) C(7) C(8) 119.9(1) . . . yes C(7) C(8) C(9) 120.8(2) . . . yes C(8) C(9) C(10) 120.9(1) . . . yes C(1) C(10) C(5) 119.3(1) . . . yes C(1) C(10) C(9) 122.6(1) . . . yes C(5) C(10) C(9) 118.1(1) . . . yes C(1) C(11) C(12) 119.9(1) . . . yes C(1) C(11) C(20) 119.7(1) . . . yes C(12) C(11) C(20) 120.3(1) . . . yes C(11) C(12) C(13) 119.0(1) . . . yes C(11) C(12) C(37) 121.1(1) . . . yes C(13) C(12) C(37) 119.7(1) . . . yes C(12) C(13) C(14) 121.7(1) . . . yes C(13) C(14) C(15) 120.8(1) . . . yes C(14) C(15) C(16) 122.1(1) . . . yes C(14) C(15) C(20) 118.6(1) . . . yes C(16) C(15) C(20) 119.3(1) . . . yes C(15) C(16) C(17) 120.9(1) . . . yes C(16) C(17) C(18) 120.1(1) . . . yes C(17) C(18) C(19) 120.7(1) . . . yes C(18) C(19) C(20) 120.9(1) . . . yes C(11) C(20) C(15) 119.4(1) . . . yes C(11) C(20) C(19) 122.6(1) . . . yes C(15) C(20) C(19) 118.0(1) . . . yes C(2) C(21) C(22) 127.2(1) . . . yes C(21) C(22) C(23) 121.0(1) . . . yes C(21) C(22) C(30) 122.5(1) . . . yes C(23) C(22) C(30) 116.5(1) . . . yes C(22) C(23) C(24) 121.1(1) . . . yes C(22) C(23) C(28) 121.7(1) . . . yes C(24) C(23) C(28) 117.2(1) . . . yes C(23) C(24) C(25) 121.6(1) . . . yes C(24) C(25) C(26) 119.9(1) . . . yes O(1) C(26) C(25) 124.7(1) . . . yes O(1) C(26) C(27) 115.8(1) . . . yes C(25) C(26) C(27) 119.6(1) . . . yes C(26) C(27) C(28) 120.0(1) . . . yes C(23) C(28) C(27) 121.7(1) . . . yes C(22) C(30) C(31) 120.4(1) . . . yes C(22) C(30) C(35) 122.0(1) . . . yes C(31) C(30) C(35) 117.5(1) . . . yes C(30) C(31) C(32) 121.9(1) . . . yes C(31) C(32) C(33) 119.4(1) . . . yes O(2) C(33) C(32) 124.2(1) . . . yes O(2) C(33) C(34) 115.9(1) . . . yes C(32) C(33) C(34) 120.0(1) . . . yes C(33) C(34) C(35) 119.9(1) . . . yes C(30) C(35) C(34) 121.4(1) . . . yes C(12) C(37) C(38) 127.9(1) . . . yes C(37) C(38) C(39) 119.8(1) . . . yes C(37) C(38) C(46) 123.9(1) . . . yes C(39) C(38) C(46) 116.2(1) . . . yes C(38) C(39) C(40) 120.9(1) . . . yes C(38) C(39) C(44) 122.0(1) . . . yes C(40) C(39) C(44) 117.0(1) . . . yes C(39) C(40) C(41) 122.0(1) . . . yes C(40) C(41) C(42) 119.5(1) . . . yes O(3) C(42) C(41) 124.3(1) . . . yes O(3) C(42) C(43) 115.8(1) . . . yes C(41) C(42) C(43) 119.8(1) . . . yes C(42) C(43) C(44) 119.8(1) . . . yes C(39) C(44) C(43) 121.8(1) . . . yes C(38) C(46) C(47) 122.2(1) . . . yes C(38) C(46) C(51) 120.4(1) . . . yes C(47) C(46) C(51) 117.4(1) . . . yes C(46) C(47) C(48) 121.6(1) . . . yes C(47) C(48) C(49) 119.7(1) . . . yes O(4) C(49) C(48) 124.5(1) . . . yes O(4) C(49) C(50) 115.8(1) . . . yes C(48) C(49) C(50) 119.6(1) . . . yes C(49) C(50) C(51) 120.2(1) . . . yes C(46) C(51) C(50) 121.5(1) . . . yes C(54) C(53) C(58) 119.7(2) . . . yes C(53) C(54) C(55) 120.2(2) . . . yes C(54) C(55) C(56) 119.8(2) . . . yes C(55) C(56) C(57) 120.2(2) . . . yes C(56) C(57) C(58) 120.1(2) . . . yes C(53) C(58) C(57) 120.0(2) . . . 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 O(1) C(9) 3.183(2) . 4_655 ? O(1) C(8) 3.261(2) . 4_655 ? O(1) C(4) 3.280(2) . 1_655 ? O(2) C(29) 3.336(2) . 3_767 ? O(2) C(34) 3.484(2) . 3_667 ? O(3) C(18) 3.389(2) . 2_656 ? O(3) C(43) 3.468(2) . 3_666 ? O(4) C(41) 3.225(3) . 1_655 ? O(4) C(40) 3.484(4) . 1_655 ? C(4) C(40) 3.445(2) . 4_555 ? C(4) C(26) 3.543(3) . 1_455 ? C(4) C(52) 3.585(2) . 1_455 ? C(5) C(40) 3.530(2) . 4_555 ? C(5) C(41) 3.536(2) . 4_555 ? C(5) C(52) 3.576(2) . 1_455 ? C(8) C(26) 3.591(2) . 4_454 ? C(16) C(55) 3.506(2) . 2_746 ? C(16) C(56) 3.509(2) . 2_746 ? C(17) C(36) 3.599(4) . 2_646 ? C(19) C(51) 3.591(2) . 4_555 ? C(25) C(56) 3.561(2) . . ? C(29) C(34) 3.582(4) . 1_655 ? C(40) C(52) 3.527(3) . 1_455 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data__040121r _database_code_depnum_ccdc_archive 'CCDC 270836' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H30 O2 ' _chemical_formula_moiety 'C48 H30 O2 ' _chemical_formula_weight 638.76 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 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 _cell_length_a 11.977(3) _cell_length_b 24.465(6) _cell_length_c 12.250(4) _cell_angle_alpha 90.000(2) _cell_angle_beta 110.328(2) _cell_angle_gamma 90.000(2) _cell_volume 3365.8(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5631 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.030 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.998 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 25563 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 3.2594 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 3.2594 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 25127 _reflns_number_gt 2329 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1640 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7457 _refine_ls_number_parameters 451 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0085 _refine_diff_density_max 0.42 _refine_diff_density_min -0.41 _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) ; O O 0.011 0.006 ;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 O(1) O -1.2384(2) -0.01931(9) -0.5595(2) 0.0670(7) Uani 1.00 d . . . O(2) O -0.5868(2) -0.04276(9) -0.1071(2) 0.0654(7) Uani 1.00 d . . . C(1) C -1.0466(2) -0.2231(1) -0.2225(3) 0.0483(9) Uani 1.00 d . . . C(2) C -1.1052(3) -0.1935(1) -0.3217(3) 0.0536(10) Uani 1.00 d . . . C(3) C -1.1268(3) -0.2181(1) -0.4321(3) 0.062(1) Uani 1.00 d . . . C(4) C -1.0903(3) -0.2698(1) -0.4419(3) 0.065(1) Uani 1.00 d . . . C(5) C -1.0328(3) -0.3018(1) -0.3427(3) 0.056(1) Uani 1.00 d . . . C(6) C -0.9957(3) -0.3559(2) -0.3504(3) 0.069(1) Uani 1.00 d . . . C(7) C -0.9368(3) -0.3858(1) -0.2537(4) 0.072(1) Uani 1.00 d . . . C(8) C -0.9118(3) -0.3619(1) -0.1440(3) 0.066(1) Uani 1.00 d . . . C(9) C -0.9473(3) -0.3097(1) -0.1325(3) 0.062(1) Uani 1.00 d . . . C(10) C -1.0086(3) -0.2785(1) -0.2307(3) 0.0501(9) Uani 1.00 d . . . C(11) C -1.0142(3) -0.1977(1) -0.1054(3) 0.0484(9) Uani 1.00 d . . . C(12) C -0.9072(3) -0.1697(1) -0.0608(3) 0.0520(9) Uani 1.00 d . . . C(13) C -0.8707(3) -0.1483(1) 0.0543(3) 0.064(1) Uani 1.00 d . . . C(14) C -0.9403(4) -0.1536(1) 0.1199(3) 0.081(1) Uani 1.00 d . . . C(15) C -1.0523(4) -0.1786(1) 0.0766(3) 0.072(1) Uani 1.00 d . . . C(16) C -1.1314(5) -0.1812(2) 0.1399(4) 0.103(2) Uani 1.00 d . . . C(17) C -1.2423(5) -0.2037(2) 0.0906(5) 0.122(2) Uani 1.00 d . . . C(18) C -1.2802(4) -0.2255(2) -0.0215(5) 0.111(2) Uani 1.00 d . . . C(19) C -1.2064(3) -0.2252(2) -0.0862(4) 0.081(1) Uani 1.00 d . . . C(20) C -1.0921(3) -0.2012(1) -0.0396(3) 0.060(1) Uani 1.00 d . . . C(21) C -1.1503(3) -0.1382(1) -0.3116(3) 0.0563(10) Uani 1.00 d . . . C(22) C -1.1498(3) -0.0927(1) -0.3736(3) 0.0505(9) Uani 1.00 d . . . C(23) C -1.2127(3) -0.0428(1) -0.3607(3) 0.0534(9) Uani 1.00 d . . . C(24) C -1.2295(3) -0.0265(1) -0.2588(3) 0.064(1) Uani 1.00 d . . . C(25) C -1.2906(4) 0.0204(2) -0.2527(3) 0.080(1) Uani 1.00 d . . . C(26) C -1.3369(4) 0.0523(2) -0.3503(4) 0.087(1) Uani 1.00 d . . . C(27) C -1.3217(3) 0.0381(2) -0.4536(3) 0.075(1) Uani 1.00 d . . . C(28) C -1.2564(3) -0.0086(1) -0.4550(3) 0.059(1) Uani 1.00 d . . . C(29) C -1.1382(3) -0.0501(1) -0.5515(3) 0.0554(10) Uani 1.00 d . . . C(30) C -1.0898(3) -0.0410(1) -0.6359(3) 0.065(1) Uani 1.00 d . . . C(31) C -0.9880(4) -0.0691(2) -0.6291(3) 0.073(1) Uani 1.00 d . . . C(32) C -0.9348(3) -0.1048(2) -0.5384(3) 0.067(1) Uani 1.00 d . . . C(33) C -0.9857(3) -0.1134(1) -0.4550(3) 0.058(1) Uani 1.00 d . . . C(34) C -1.0914(3) -0.0867(1) -0.4604(3) 0.0502(9) Uani 1.00 d . . . C(35) C -0.8279(3) -0.1650(1) -0.1294(3) 0.0508(9) Uani 1.00 d . . . C(36) C -0.7706(3) -0.1212(1) -0.1479(2) 0.0480(9) Uani 1.00 d . . . C(37) C -0.6797(3) -0.1256(1) -0.2038(3) 0.0500(9) Uani 1.00 d . . . C(38) C -0.6743(3) -0.1676(1) -0.2780(3) 0.065(1) Uani 1.00 d . . . C(39) C -0.5825(3) -0.1713(2) -0.3219(3) 0.074(1) Uani 1.00 d . . . C(40) C -0.4953(3) -0.1321(2) -0.2947(3) 0.075(1) Uani 1.00 d . . . C(41) C -0.4969(3) -0.0895(2) -0.2226(3) 0.066(1) Uani 1.00 d . . . C(42) C -0.5901(3) -0.0870(1) -0.1800(3) 0.0533(9) Uani 1.00 d . . . C(43) C -0.6916(3) -0.0277(1) -0.0929(2) 0.0521(9) Uani 1.00 d . . . C(44) C -0.6977(3) 0.0256(1) -0.0579(3) 0.059(1) Uani 1.00 d . . . C(45) C -0.8023(3) 0.0437(1) -0.0488(3) 0.063(1) Uani 1.00 d . . . C(46) C -0.9004(3) 0.0102(1) -0.0756(3) 0.061(1) Uani 1.00 d . . . C(47) C -0.8918(3) -0.0434(1) -0.1073(3) 0.0542(9) Uani 1.00 d . . . C(48) C -0.7854(3) -0.0645(1) -0.1134(2) 0.0472(9) Uani 1.00 d . . . H(1) H -1.1703 -0.1969 -0.5023 0.0726 Uiso 1.00 calc . . . H(2) H -1.1038 -0.2856 -0.5195 0.0781 Uiso 1.00 calc . . . H(3) H -1.0131 -0.3722 -0.4278 0.0815 Uiso 1.00 calc . . . H(4) H -0.9146 -0.4234 -0.2604 0.0859 Uiso 1.00 calc . . . H(5) H -0.8669 -0.3830 -0.0750 0.0769 Uiso 1.00 calc . . . H(6) H -0.9305 -0.2939 -0.0541 0.0724 Uiso 1.00 calc . . . H(7) H -0.7923 -0.1293 0.0845 0.0752 Uiso 1.00 calc . . . H(8) H -0.9080 -0.1402 0.2014 0.0936 Uiso 1.00 calc . . . H(9) H -1.1052 -0.1679 0.2215 0.1217 Uiso 1.00 calc . . . H(10) H -1.2958 -0.2041 0.1335 0.1328 Uiso 1.00 calc . . . H(11) H -1.3618 -0.2408 -0.0556 0.1357 Uiso 1.00 calc . . . H(12) H -1.2328 -0.2416 -0.1652 0.1028 Uiso 1.00 calc . . . H(13) H -1.1854 -0.1339 -0.2498 0.0695 Uiso 1.00 calc . . . H(14) H -1.1971 -0.0500 -0.1894 0.0777 Uiso 1.00 calc . . . H(15) H -1.2981 0.0320 -0.1782 0.0930 Uiso 1.00 calc . . . H(16) H -1.3826 0.0848 -0.3478 0.1006 Uiso 1.00 calc . . . H(17) H -1.3562 0.0606 -0.5244 0.0895 Uiso 1.00 calc . . . H(18) H -1.1263 -0.0157 -0.7004 0.0777 Uiso 1.00 calc . . . H(19) H -0.9518 -0.0632 -0.6887 0.0871 Uiso 1.00 calc . . . H(20) H -0.8618 -0.1243 -0.5341 0.0798 Uiso 1.00 calc . . . H(21) H -0.9476 -0.1383 -0.3905 0.0709 Uiso 1.00 calc . . . H(22) H -0.8151 -0.1988 -0.1661 0.0611 Uiso 1.00 calc . . . H(23) H -0.7374 -0.1955 -0.2998 0.0775 Uiso 1.00 calc . . . H(24) H -0.5801 -0.2015 -0.3736 0.0837 Uiso 1.00 calc . . . H(25) H -0.4300 -0.1354 -0.3246 0.0874 Uiso 1.00 calc . . . H(26) H -0.4354 -0.0615 -0.2034 0.0770 Uiso 1.00 calc . . . H(27) H -0.6275 0.0499 -0.0379 0.0709 Uiso 1.00 calc . . . H(28) H -0.8087 0.0816 -0.0255 0.0715 Uiso 1.00 calc . . . H(29) H -0.9749 0.0239 -0.0710 0.0745 Uiso 1.00 calc . . . H(30) H -0.9626 -0.0671 -0.1273 0.0636 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 O(1) 0.073(2) 0.064(2) 0.059(1) 0.009(1) 0.015(1) 0.010(1) O(2) 0.053(1) 0.067(2) 0.079(2) -0.010(1) 0.026(1) -0.013(1) C(1) 0.040(2) 0.044(2) 0.061(2) -0.006(1) 0.017(1) 0.006(2) C(2) 0.049(2) 0.048(2) 0.062(2) -0.002(2) 0.017(2) 0.006(2) C(3) 0.060(2) 0.056(2) 0.057(2) -0.005(2) 0.002(2) 0.004(2) C(4) 0.062(2) 0.065(2) 0.059(2) -0.008(2) 0.009(2) -0.005(2) C(5) 0.049(2) 0.050(2) 0.066(2) -0.006(2) 0.015(2) -0.003(2) C(6) 0.068(2) 0.057(2) 0.082(2) -0.003(2) 0.025(2) -0.012(2) C(7) 0.071(2) 0.046(2) 0.102(3) 0.005(2) 0.031(2) -0.005(2) C(8) 0.063(2) 0.052(2) 0.080(2) 0.009(2) 0.020(2) 0.011(2) C(9) 0.063(2) 0.049(2) 0.073(2) 0.006(2) 0.022(2) 0.008(2) C(10) 0.044(2) 0.039(2) 0.068(2) -0.007(1) 0.019(2) 0.005(2) C(11) 0.053(2) 0.040(2) 0.057(2) 0.007(1) 0.025(2) 0.009(1) C(12) 0.064(2) 0.041(2) 0.058(2) 0.001(2) 0.029(2) 0.003(1) C(13) 0.091(3) 0.051(2) 0.059(2) -0.005(2) 0.036(2) -0.003(2) C(14) 0.133(3) 0.051(2) 0.079(2) 0.007(2) 0.061(2) 0.000(2) C(15) 0.107(3) 0.049(2) 0.085(2) 0.018(2) 0.064(2) 0.014(2) C(16) 0.163(4) 0.061(3) 0.134(3) 0.028(3) 0.115(3) 0.026(2) C(17) 0.142(3) 0.089(3) 0.194(4) 0.048(3) 0.133(3) 0.060(3) C(18) 0.084(3) 0.113(4) 0.163(4) 0.022(3) 0.079(3) 0.058(3) C(19) 0.061(2) 0.081(3) 0.112(3) 0.006(2) 0.043(2) 0.035(2) C(20) 0.064(2) 0.047(2) 0.081(2) 0.011(2) 0.039(2) 0.023(2) C(21) 0.054(2) 0.054(2) 0.061(2) 0.005(2) 0.020(2) 0.007(2) C(22) 0.050(2) 0.048(2) 0.053(2) 0.002(2) 0.017(1) 0.006(2) C(23) 0.055(2) 0.050(2) 0.058(2) 0.007(2) 0.023(2) 0.012(2) C(24) 0.069(2) 0.060(2) 0.072(2) 0.000(2) 0.036(2) 0.007(2) C(25) 0.096(3) 0.066(3) 0.098(3) 0.007(2) 0.058(2) 0.006(2) C(26) 0.095(3) 0.065(3) 0.123(3) 0.025(2) 0.065(2) 0.012(2) C(27) 0.067(2) 0.067(2) 0.093(3) 0.021(2) 0.031(2) 0.022(2) C(28) 0.056(2) 0.060(2) 0.062(2) 0.001(2) 0.021(2) 0.006(2) C(29) 0.056(2) 0.058(2) 0.047(2) 0.002(2) 0.011(2) 0.001(2) C(30) 0.083(2) 0.062(2) 0.051(2) -0.004(2) 0.024(2) 0.004(2) C(31) 0.098(3) 0.069(3) 0.061(2) -0.012(2) 0.038(2) -0.004(2) C(32) 0.068(2) 0.072(3) 0.070(2) -0.001(2) 0.034(2) -0.003(2) C(33) 0.058(2) 0.053(2) 0.061(2) -0.001(2) 0.019(2) 0.005(2) C(34) 0.051(2) 0.052(2) 0.044(2) -0.004(2) 0.013(1) 0.000(1) C(35) 0.052(2) 0.053(2) 0.053(2) -0.003(2) 0.025(2) -0.003(2) C(36) 0.043(2) 0.051(2) 0.050(2) -0.001(1) 0.016(1) 0.000(1) C(37) 0.043(2) 0.052(2) 0.057(2) 0.000(2) 0.020(1) 0.003(2) C(38) 0.065(2) 0.059(2) 0.079(2) -0.009(2) 0.035(2) -0.013(2) C(39) 0.072(2) 0.070(3) 0.092(3) -0.002(2) 0.044(2) -0.016(2) C(40) 0.066(2) 0.085(3) 0.089(3) 0.001(2) 0.046(2) -0.004(2) C(41) 0.052(2) 0.078(3) 0.077(2) -0.016(2) 0.031(2) -0.007(2) C(42) 0.053(2) 0.054(2) 0.056(2) 0.000(2) 0.023(2) -0.003(2) C(43) 0.052(2) 0.058(2) 0.049(2) -0.005(2) 0.021(2) -0.010(2) C(44) 0.067(2) 0.058(2) 0.054(2) -0.008(2) 0.024(2) -0.002(2) C(45) 0.090(3) 0.050(2) 0.054(2) 0.002(2) 0.032(2) 0.005(2) C(46) 0.073(2) 0.055(2) 0.062(2) 0.012(2) 0.034(2) 0.008(2) C(47) 0.059(2) 0.054(2) 0.053(2) 0.000(2) 0.025(2) 0.005(2) C(48) 0.051(2) 0.045(2) 0.048(2) 0.002(1) 0.021(1) 0.002(1) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _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 O(1) C(28) 1.391(5) . . yes O(1) C(29) 1.394(6) . . yes O(2) C(42) 1.396(5) . . yes O(2) C(43) 1.377(5) . . yes C(1) C(2) 1.384(6) . . yes C(1) C(10) 1.447(6) . . yes C(1) C(11) 1.487(6) . . yes C(2) C(3) 1.415(7) . . yes C(2) C(21) 1.468(6) . . yes C(3) C(4) 1.361(7) . . yes C(4) C(5) 1.411(7) . . yes C(5) C(6) 1.408(7) . . yes C(5) C(10) 1.413(6) . . yes C(6) C(7) 1.360(7) . . yes C(7) C(8) 1.398(7) . . yes C(8) C(9) 1.371(7) . . yes C(9) C(10) 1.398(6) . . yes C(11) C(12) 1.386(6) . . yes C(11) C(20) 1.433(6) . . yes C(12) C(13) 1.424(6) . . yes C(12) C(35) 1.474(6) . . yes C(13) C(14) 1.350(7) . . yes C(14) C(15) 1.401(8) . . yes C(15) C(16) 1.423(8) . . yes C(15) C(20) 1.442(7) . . yes C(16) C(17) 1.36(1) . . yes C(17) C(18) 1.39(1) . . yes C(18) C(19) 1.375(9) . . yes C(19) C(20) 1.411(7) . . yes C(21) C(22) 1.355(6) . . yes C(22) C(23) 1.475(6) . . yes C(22) C(34) 1.472(6) . . yes C(23) C(24) 1.387(6) . . yes C(23) C(28) 1.376(6) . . yes C(24) C(25) 1.377(7) . . yes C(25) C(26) 1.373(8) . . yes C(26) C(27) 1.381(8) . . yes C(27) C(28) 1.388(7) . . yes C(29) C(30) 1.374(7) . . yes C(29) C(34) 1.384(6) . . yes C(30) C(31) 1.373(7) . . yes C(31) C(32) 1.380(7) . . yes C(32) C(33) 1.378(6) . . yes C(33) C(34) 1.401(6) . . yes C(35) C(36) 1.338(6) . . yes C(36) C(37) 1.477(6) . . yes C(36) C(48) 1.481(6) . . yes C(37) C(38) 1.389(6) . . yes C(37) C(42) 1.382(6) . . yes C(38) C(39) 1.386(7) . . yes C(39) C(40) 1.365(7) . . yes C(40) C(41) 1.372(7) . . yes C(41) C(42) 1.393(6) . . yes C(43) C(44) 1.384(6) . . yes C(43) C(48) 1.390(6) . . yes C(44) C(45) 1.372(7) . . yes C(45) C(46) 1.377(7) . . yes C(46) C(47) 1.383(6) . . yes C(47) C(48) 1.402(6) . . 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(28) O(1) C(29) 116.3(4) . . . yes C(42) O(2) C(43) 117.5(4) . . . yes C(2) C(1) C(10) 120.2(4) . . . yes C(2) C(1) C(11) 120.8(4) . . . yes C(10) C(1) C(11) 119.0(4) . . . yes C(1) C(2) C(3) 118.8(4) . . . yes C(1) C(2) C(21) 119.8(4) . . . yes C(3) C(2) C(21) 121.3(4) . . . yes C(2) C(3) C(4) 122.1(5) . . . yes C(3) C(4) C(5) 120.7(5) . . . yes C(4) C(5) C(6) 122.2(5) . . . yes C(4) C(5) C(10) 119.0(5) . . . yes C(6) C(5) C(10) 118.7(5) . . . yes C(5) C(6) C(7) 121.5(5) . . . yes C(6) C(7) C(8) 119.5(5) . . . yes C(7) C(8) C(9) 120.6(5) . . . yes C(8) C(9) C(10) 120.8(5) . . . yes C(1) C(10) C(5) 119.2(4) . . . yes C(1) C(10) C(9) 121.8(5) . . . yes C(5) C(10) C(9) 118.9(5) . . . yes C(1) C(11) C(12) 118.9(4) . . . yes C(1) C(11) C(20) 120.9(4) . . . yes C(12) C(11) C(20) 120.2(4) . . . yes C(11) C(12) C(13) 119.7(4) . . . yes C(11) C(12) C(35) 120.2(4) . . . yes C(13) C(12) C(35) 119.9(4) . . . yes C(12) C(13) C(14) 120.9(5) . . . yes C(13) C(14) C(15) 121.6(5) . . . yes C(14) C(15) C(16) 123.3(6) . . . yes C(14) C(15) C(20) 119.2(5) . . . yes C(16) C(15) C(20) 117.5(6) . . . yes C(15) C(16) C(17) 120.5(7) . . . yes C(16) C(17) C(18) 122.0(7) . . . yes C(17) C(18) C(19) 120.1(7) . . . yes C(18) C(19) C(20) 120.1(7) . . . yes C(11) C(20) C(15) 118.2(5) . . . yes C(11) C(20) C(19) 121.8(5) . . . yes C(15) C(20) C(19) 119.9(5) . . . yes C(2) C(21) C(22) 129.4(4) . . . yes C(21) C(22) C(23) 121.5(4) . . . yes C(21) C(22) C(34) 125.7(4) . . . yes C(23) C(22) C(34) 112.9(4) . . . yes C(22) C(23) C(24) 124.8(4) . . . yes C(22) C(23) C(28) 117.9(4) . . . yes C(24) C(23) C(28) 117.2(5) . . . yes C(23) C(24) C(25) 121.9(5) . . . yes C(24) C(25) C(26) 119.2(5) . . . yes C(25) C(26) C(27) 121.1(5) . . . yes C(26) C(27) C(28) 118.1(5) . . . yes O(1) C(28) C(23) 121.7(5) . . . yes O(1) C(28) C(27) 115.9(5) . . . yes C(23) C(28) C(27) 122.4(5) . . . yes O(1) C(29) C(30) 115.9(5) . . . yes O(1) C(29) C(34) 120.5(4) . . . yes C(30) C(29) C(34) 123.6(5) . . . yes C(29) C(30) C(31) 117.9(5) . . . yes C(30) C(31) C(32) 121.3(5) . . . yes C(31) C(32) C(33) 119.5(5) . . . yes C(32) C(33) C(34) 121.2(4) . . . yes C(22) C(34) C(29) 118.7(4) . . . yes C(22) C(34) C(33) 124.7(4) . . . yes C(29) C(34) C(33) 116.5(4) . . . yes C(12) C(35) C(36) 128.7(4) . . . yes C(35) C(36) C(37) 121.3(4) . . . yes C(35) C(36) C(48) 126.0(4) . . . yes C(37) C(36) C(48) 112.7(4) . . . yes C(36) C(37) C(38) 124.7(4) . . . yes C(36) C(37) C(42) 119.6(4) . . . yes C(38) C(37) C(42) 115.7(4) . . . yes C(37) C(38) C(39) 121.7(5) . . . yes C(38) C(39) C(40) 120.4(5) . . . yes C(39) C(40) C(41) 120.5(5) . . . yes C(40) C(41) C(42) 117.9(5) . . . yes O(2) C(42) C(37) 121.1(4) . . . yes O(2) C(42) C(41) 115.1(4) . . . yes C(37) C(42) C(41) 123.8(5) . . . yes O(2) C(43) C(44) 116.0(4) . . . yes O(2) C(43) C(48) 121.3(4) . . . yes C(44) C(43) C(48) 122.7(4) . . . yes C(43) C(44) C(45) 118.2(5) . . . yes C(44) C(45) C(46) 121.5(5) . . . yes C(45) C(46) C(47) 119.5(5) . . . yes C(46) C(47) C(48) 121.0(4) . . . yes C(36) C(48) C(43) 119.3(4) . . . yes C(36) C(48) C(47) 123.7(4) . . . yes C(43) C(48) C(47) 116.8(4) . . . 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 O(1) C(8) 3.511(6) . 4_444 ? O(1) C(7) 3.579(7) . 4_444 ? O(2) C(44) 3.322(6) . 3_455 ? O(2) O(2) 3.430(7) . 3_455 ? C(4) C(35) 3.366(7) . 4_444 ? C(16) C(45) 3.547(7) . 3_355 ? C(17) C(38) 3.501(9) . 4_445 ? C(17) C(39) 3.572(9) . 4_445 ? C(27) C(32) 3.512(8) . 3_354 ? C(27) C(31) 3.573(8) . 3_354 ? C(28) C(31) 3.343(8) . 3_354 ? C(30) C(46) 3.571(7) . 3_354 ? C(46) C(46) 3.528(10) . 3_355 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data__040319r _database_code_depnum_ccdc_archive 'CCDC 270837' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C52 H42 Cl12 O4 Sb2 ' _chemical_formula_moiety ? _chemical_formula_weight 1399.84 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,z -x,-y,-z -x,y,-z 1/2+x,1/2+y,z 1/2+x,1/2-y,z 1/2-x,1/2-y,-z 1/2-x,1/2+y,-z _cell_length_a 18.425(7) _cell_length_b 34.50(1) _cell_length_c 10.674(4) _cell_angle_alpha 90.000(2) _cell_angle_beta 115.457(3) _cell_angle_gamma 90.000(2) _cell_volume 6125.4(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6769 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour Red _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.005 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.443 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.993 _exptl_absorpt_correction_T_max 0.993 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 25805 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9841 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9841 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7050 _reflns_number_gt 1874 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1598 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7041 _refine_ls_number_parameters 322 _refine_ls_goodness_of_fit_ref 0.740 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0213 _refine_diff_density_max 2.35 _refine_diff_density_min -2.30 _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) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb Sb -0.587 1.546 ;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 Sb(1) Sb 1.0000 0.29407(2) 0.0000 0.0551(2) Uani 1.00 d S . . Sb(2) Sb 0.81166(7) 0.0000 0.21359(9) 0.1095(3) Uani 1.00 d S . . Cl(1) Cl 1.0000 0.36163(8) 0.0000 0.099(1) Uani 1.00 d S . . Cl(2) Cl 1.0000 0.22533(8) 0.0000 0.0916(9) Uani 1.00 d S . . Cl(3) Cl 1.1184(1) 0.29190(8) 0.2079(2) 0.0992(7) Uani 1.00 d . . . Cl(4) Cl 0.9224(1) 0.29314(6) 0.1280(2) 0.0699(5) Uani 1.00 d . . . Cl(5) Cl 0.8838(8) 0.0000 0.4496(6) 0.401(5) Uani 1.00 d S . . Cl(6) Cl 0.7437(3) 0.0000 -0.0255(4) 0.163(2) Uani 1.00 d S . . Cl(7) Cl 0.7286(2) 0.04765(8) 0.2351(4) 0.225(1) Uani 1.00 d . . . Cl(8) Cl 0.8932(2) 0.0493(1) 0.1973(4) 0.187(2) Uani 1.00 d . . . O(1) O 0.4154(4) 0.4070(2) 0.8392(6) 0.134(3) Uani 1.00 d . . . O(2) O 0.2259(3) 0.3596(2) -0.1373(5) 0.093(2) Uani 1.00 d . . . C(1) C 0.4567(3) 0.2089(2) 0.4860(5) 0.042(1) Uani 1.00 d . . . C(2) C 0.4133(4) 0.2421(2) 0.4410(6) 0.047(2) Uani 1.00 d . . . C(3) C 0.3297(4) 0.2427(2) 0.3967(6) 0.053(2) Uani 1.00 d . . . C(4) C 0.2903(4) 0.2098(2) 0.4039(6) 0.058(2) Uani 1.00 d . . . C(5) C 0.3328(4) 0.1767(2) 0.4629(6) 0.051(2) Uani 1.00 d . . . C(6) C 0.2929(4) 0.1440(2) 0.4836(7) 0.072(2) Uani 1.00 d . . . C(7) C 0.3349(5) 0.1122(2) 0.5550(8) 0.078(2) Uani 1.00 d . . . C(8) C 0.4200(5) 0.1121(2) 0.6149(7) 0.072(2) Uani 1.00 d . . . C(9) C 0.4592(4) 0.1431(2) 0.5917(6) 0.057(2) Uani 1.00 d . . . C(10) C 0.4180(3) 0.1758(2) 0.5122(6) 0.046(2) Uani 1.00 d . . . C(11) C 0.4586(4) 0.2788(2) 0.4378(6) 0.054(2) Uani 1.00 d . . . C(12) C 0.4104(3) 0.3150(2) 0.4078(6) 0.047(2) Uani 1.00 d . . . C(13) C 0.4136(4) 0.3391(2) 0.5188(6) 0.055(2) Uani 1.00 d . . . C(14) C 0.4216(4) 0.3236(2) 0.6474(7) 0.069(2) Uani 1.00 d . . . C(15) C 0.4222(4) 0.3478(3) 0.7503(7) 0.084(3) Uani 1.00 d . . . C(16) C 0.4168(5) 0.3872(3) 0.7320(8) 0.090(3) Uani 1.00 d . . . C(17) C 0.4116(4) 0.4034(2) 0.6118(8) 0.076(2) Uani 1.00 d . . . C(18) C 0.4107(4) 0.3798(2) 0.5074(7) 0.061(2) Uani 1.00 d . . . C(19) C 0.4004(9) 0.4452(4) 0.827(1) 0.197(6) Uani 1.00 d . . . C(20) C 0.3618(3) 0.3258(2) 0.2690(6) 0.048(2) Uani 1.00 d . . . C(21) C 0.3700(4) 0.3094(2) 0.1522(7) 0.068(2) Uani 1.00 d . . . C(22) C 0.3229(4) 0.3204(3) 0.0213(7) 0.080(3) Uani 1.00 d . . . C(23) C 0.2630(4) 0.3486(2) -0.0052(7) 0.066(2) Uani 1.00 d . . . C(24) C 0.2487(4) 0.3627(2) 0.1018(7) 0.061(2) Uani 1.00 d . . . C(25) C 0.2951(4) 0.3514(2) 0.2355(6) 0.055(2) Uani 1.00 d . . . C(26) C 0.1670(5) 0.3932(3) -0.1772(8) 0.117(3) Uani 1.00 d . . . H(1) H 0.2997 0.2667 0.3587 0.0607 Uiso 1.00 calc . . . H(2) H 0.2316 0.2102 0.3635 0.0605 Uiso 1.00 calc . . . H(3) H 0.2344 0.1431 0.4478 0.0758 Uiso 1.00 calc . . . H(4) H 0.3087 0.0909 0.5707 0.0864 Uiso 1.00 calc . . . H(5) H 0.4497 0.0906 0.6692 0.0789 Uiso 1.00 calc . . . H(6) H 0.5189 0.1431 0.6332 0.0579 Uiso 1.00 calc . . . H(7) H 0.4722 0.2754 0.3602 0.0592 Uiso 1.00 calc . . . H(8) H 0.4260 0.2956 0.6614 0.0705 Uiso 1.00 calc . . . H(9) H 0.4276 0.3372 0.8400 0.0879 Uiso 1.00 calc . . . H(10) H 0.4129 0.4315 0.6041 0.0748 Uiso 1.00 calc . . . H(11) H 0.4076 0.3915 0.4215 0.0662 Uiso 1.00 calc . . . H(12) H 0.3973 0.4601 0.8979 0.1827 Uiso 1.00 calc . . . H(13) H 0.4374 0.4604 0.7964 0.1827 Uiso 1.00 calc . . . H(14) H 0.3461 0.4518 0.7413 0.1827 Uiso 1.00 calc . . . H(15) H 0.4103 0.2895 0.1688 0.0724 Uiso 1.00 calc . . . H(16) H 0.3347 0.3095 -0.0529 0.0955 Uiso 1.00 calc . . . H(17) H 0.2026 0.3803 0.0801 0.0677 Uiso 1.00 calc . . . H(18) H 0.2831 0.3617 0.3092 0.0654 Uiso 1.00 calc . . . H(19) H 0.1900 0.4148 -0.1259 0.1079 Uiso 1.00 calc . . . H(20) H 0.1437 0.3964 -0.2715 0.1079 Uiso 1.00 calc . . . H(21) H 0.1228 0.3846 -0.1506 0.1079 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 Sb(1) 0.0633(4) 0.0565(4) 0.0484(3) 0.0000 0.0267(3) 0.0000 Sb(2) 0.1895(9) 0.0620(5) 0.1043(6) 0.0000 0.0891(5) 0.0000 Cl(1) 0.147(2) 0.059(2) 0.121(2) 0.0000 0.087(2) 0.0000 Cl(2) 0.129(2) 0.057(2) 0.127(2) 0.0000 0.090(2) 0.0000 Cl(3) 0.071(1) 0.160(2) 0.055(1) 0.003(2) 0.0167(9) -0.007(1) Cl(4) 0.084(1) 0.076(1) 0.0643(9) 0.005(1) 0.0462(7) 0.0007(9) Cl(5) 0.80(2) 0.172(6) 0.100(4) 0.0000 0.064(7) 0.0000 Cl(6) 0.203(5) 0.126(3) 0.121(3) 0.0000 0.034(3) 0.0000 Cl(7) 0.395(3) 0.061(2) 0.393(3) 0.005(2) 0.336(2) -0.004(2) Cl(8) 0.196(3) 0.137(3) 0.247(4) -0.063(3) 0.115(3) -0.041(3) O(1) 0.157(5) 0.152(6) 0.099(4) 0.039(5) 0.060(4) -0.031(4) O(2) 0.085(4) 0.126(5) 0.049(3) -0.001(4) 0.012(3) 0.012(3) C(1) 0.047(3) 0.039(3) 0.037(3) -0.003(3) 0.016(2) -0.005(3) C(2) 0.046(3) 0.045(4) 0.052(3) 0.001(3) 0.023(3) -0.001(3) C(3) 0.041(3) 0.050(4) 0.061(4) 0.005(3) 0.015(3) 0.000(3) C(4) 0.043(3) 0.064(4) 0.069(4) -0.007(4) 0.026(3) -0.005(3) C(5) 0.057(4) 0.049(4) 0.053(3) -0.012(3) 0.030(3) -0.005(3) C(6) 0.062(4) 0.069(5) 0.082(5) -0.006(4) 0.027(4) 0.004(4) C(7) 0.088(5) 0.061(5) 0.097(5) -0.018(4) 0.051(4) -0.005(4) C(8) 0.085(5) 0.058(4) 0.068(4) 0.000(4) 0.030(4) 0.011(4) C(9) 0.069(4) 0.041(4) 0.060(4) -0.007(3) 0.027(3) 0.004(3) C(10) 0.048(3) 0.043(4) 0.048(3) 0.000(3) 0.023(3) -0.004(3) C(11) 0.058(4) 0.048(4) 0.058(4) 0.009(3) 0.026(3) 0.001(3) C(12) 0.046(3) 0.039(3) 0.058(3) 0.002(3) 0.023(3) 0.010(3) C(13) 0.054(4) 0.056(4) 0.056(4) 0.012(3) 0.023(3) 0.004(3) C(14) 0.067(4) 0.086(5) 0.062(4) 0.031(4) 0.035(3) 0.017(4) C(15) 0.086(5) 0.118(7) 0.058(4) 0.040(5) 0.040(3) 0.012(4) C(16) 0.103(6) 0.104(7) 0.069(5) 0.025(5) 0.042(4) -0.013(5) C(17) 0.080(5) 0.064(5) 0.077(5) 0.009(4) 0.028(4) -0.012(4) C(18) 0.057(4) 0.061(4) 0.060(4) 0.004(4) 0.022(3) -0.002(3) C(19) 0.26(1) 0.19(1) 0.155(9) 0.02(1) 0.104(9) -0.079(9) C(20) 0.042(3) 0.045(4) 0.059(4) 0.004(3) 0.022(3) 0.001(3) C(21) 0.075(4) 0.071(5) 0.062(4) 0.017(4) 0.032(3) -0.004(4) C(22) 0.078(5) 0.117(7) 0.047(4) 0.012(5) 0.030(3) -0.007(4) C(23) 0.066(5) 0.069(5) 0.054(4) -0.013(4) 0.019(3) 0.001(4) C(24) 0.061(4) 0.056(4) 0.056(4) 0.015(4) 0.014(3) 0.004(3) C(25) 0.058(4) 0.053(4) 0.053(4) 0.012(3) 0.022(3) -0.009(3) C(26) 0.093(6) 0.126(8) 0.072(5) 0.024(6) -0.021(5) -0.028(5) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _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 Sb(1) Cl(1) 2.331(3) . . yes Sb(1) Cl(2) 2.371(3) . . yes Sb(1) Cl(3) 2.351(2) . . yes Sb(1) Cl(3) 2.351(2) . 4_755 yes Sb(1) Cl(4) 2.365(2) . . yes Sb(1) Cl(4) 2.365(2) . 4_755 yes Sb(2) Cl(5) 2.287(6) . . yes Sb(2) Cl(6) 2.309(4) . . yes Sb(2) Cl(7) 2.324(3) . . yes Sb(2) Cl(7) 2.324(3) . 2_555 yes Sb(2) Cl(8) 2.325(4) . . yes Sb(2) Cl(8) 2.325(4) . 2_555 yes O(1) C(16) 1.342(9) . . yes O(1) C(19) 1.34(1) . . yes O(2) C(23) 1.330(7) . . yes O(2) C(26) 1.520(10) . . yes C(1) C(1) 1.49(1) . 4_656 yes C(1) C(2) 1.361(7) . . yes C(1) C(10) 1.433(8) . . yes C(2) C(3) 1.403(8) . . yes C(2) C(11) 1.526(8) . . yes C(3) C(4) 1.366(8) . . yes C(4) C(5) 1.376(8) . . yes C(5) C(6) 1.415(9) . . yes C(5) C(10) 1.427(8) . . yes C(6) C(7) 1.368(10) . . yes C(7) C(8) 1.417(10) . . yes C(8) C(9) 1.373(9) . . yes C(9) C(10) 1.420(8) . . yes C(11) C(11) 1.53(1) . 4_656 yes C(11) C(12) 1.486(8) . . yes C(12) C(13) 1.426(8) . . yes C(12) C(20) 1.412(8) . . yes C(13) C(14) 1.421(9) . . yes C(13) C(18) 1.410(9) . . yes C(14) C(15) 1.376(10) . . yes C(15) C(16) 1.37(1) . . yes C(16) C(17) 1.36(1) . . yes C(17) C(18) 1.374(9) . . yes C(20) C(21) 1.435(8) . . yes C(20) C(25) 1.430(8) . . yes C(21) C(22) 1.344(9) . . yes C(22) C(23) 1.407(10) . . yes C(23) C(24) 1.367(9) . . yes C(24) C(25) 1.368(8) . . 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 Cl(1) Sb(1) Cl(2) 180.0 . . . yes Cl(1) Sb(1) Cl(3) 91.82(7) . . . yes Cl(1) Sb(1) Cl(3) 91.82(7) . . 4_755 yes Cl(1) Sb(1) Cl(4) 90.77(5) . . . yes Cl(1) Sb(1) Cl(4) 90.77(5) . . 4_755 yes Cl(2) Sb(1) Cl(3) 88.18(7) . . . yes Cl(2) Sb(1) Cl(3) 88.18(7) . . 4_755 yes Cl(2) Sb(1) Cl(4) 89.23(5) . . . yes Cl(2) Sb(1) Cl(4) 89.23(5) . . 4_755 yes Cl(3) Sb(1) Cl(3) 176.4(1) . . 4_755 yes Cl(3) Sb(1) Cl(4) 90.03(7) . . . yes Cl(3) Sb(1) Cl(4) 89.92(7) . . 4_755 yes Cl(3) Sb(1) Cl(4) 89.92(7) 4_755 . . yes Cl(3) Sb(1) Cl(4) 90.03(7) 4_755 . 4_755 yes Cl(4) Sb(1) Cl(4) 178.45(10) . . 4_755 yes Cl(5) Sb(2) Cl(6) 177.7(4) . . . yes Cl(5) Sb(2) Cl(7) 89.2(3) . . . yes Cl(5) Sb(2) Cl(7) 89.2(3) . . 2_555 yes Cl(5) Sb(2) Cl(8) 89.7(3) . . . yes Cl(5) Sb(2) Cl(8) 89.7(3) . . 2_555 yes Cl(6) Sb(2) Cl(7) 92.4(1) . . . yes Cl(6) Sb(2) Cl(7) 92.4(1) . . 2_555 yes Cl(6) Sb(2) Cl(8) 88.7(1) . . . yes Cl(6) Sb(2) Cl(8) 88.7(1) . . 2_555 yes Cl(7) Sb(2) Cl(7) 90.1(2) . . 2_555 yes Cl(7) Sb(2) Cl(8) 88.0(1) . . . yes Cl(7) Sb(2) Cl(8) 177.7(1) . . 2_555 yes Cl(7) Sb(2) Cl(8) 177.7(1) 2_555 . . yes Cl(7) Sb(2) Cl(8) 88.0(1) 2_555 . 2_555 yes Cl(8) Sb(2) Cl(8) 94.0(2) . . 2_555 yes C(16) O(1) C(19) 119.6(9) . . . yes C(23) O(2) C(26) 119.6(6) . . . yes C(1) C(1) C(2) 119.1(4) 4_656 . . yes C(1) C(1) C(10) 122.6(4) 4_656 . . yes C(2) C(1) C(10) 118.1(5) . . . yes C(1) C(2) C(3) 121.7(6) . . . yes C(1) C(2) C(11) 117.5(5) . . . yes C(3) C(2) C(11) 120.7(6) . . . yes C(2) C(3) C(4) 120.0(6) . . . yes C(3) C(4) C(5) 120.3(6) . . . yes C(4) C(5) C(6) 120.2(6) . . . yes C(4) C(5) C(10) 120.4(6) . . . yes C(6) C(5) C(10) 119.3(6) . . . yes C(5) C(6) C(7) 121.2(7) . . . yes C(6) C(7) C(8) 120.4(7) . . . yes C(7) C(8) C(9) 118.8(7) . . . yes C(8) C(9) C(10) 122.7(6) . . . yes C(1) C(10) C(5) 118.2(5) . . . yes C(1) C(10) C(9) 124.5(5) . . . yes C(5) C(10) C(9) 117.3(6) . . . yes C(2) C(11) C(11) 109.4(4) . . 4_656 yes C(2) C(11) C(12) 114.9(5) . . . yes C(11) C(11) C(12) 117.8(4) 4_656 . . yes C(11) C(12) C(13) 120.2(5) . . . yes C(11) C(12) C(20) 119.9(5) . . . yes C(13) C(12) C(20) 120.0(5) . . . yes C(12) C(13) C(14) 122.3(6) . . . yes C(12) C(13) C(18) 121.5(6) . . . yes C(14) C(13) C(18) 116.2(6) . . . yes C(13) C(14) C(15) 120.4(7) . . . yes C(14) C(15) C(16) 120.9(7) . . . yes O(1) C(16) C(15) 114.2(8) . . . yes O(1) C(16) C(17) 125.1(9) . . . yes C(15) C(16) C(17) 120.7(7) . . . yes C(16) C(17) C(18) 119.5(7) . . . yes C(13) C(18) C(17) 122.3(6) . . . yes C(12) C(20) C(21) 123.5(6) . . . yes C(12) C(20) C(25) 121.0(5) . . . yes C(21) C(20) C(25) 115.2(5) . . . yes C(20) C(21) C(22) 122.0(7) . . . yes C(21) C(22) C(23) 120.3(6) . . . yes O(2) C(23) C(22) 114.3(7) . . . yes O(2) C(23) C(24) 126.1(7) . . . yes C(22) C(23) C(24) 119.7(6) . . . yes C(23) C(24) C(25) 120.7(6) . . . yes C(20) C(25) C(24) 121.5(6) . . . yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data__040224r _database_code_depnum_ccdc_archive 'CCDC 270838' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C50 H32 Cl6 O3 ' _chemical_formula_moiety ? _chemical_formula_weight 893.52 _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 11.219(4) _cell_length_b 12.480(5) _cell_length_c 16.557(7) _cell_angle_alpha 86.02(1) _cell_angle_beta 89.83(1) _cell_angle_gamma 64.63(1) _cell_volume 2088.6(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6640 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.872 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 11080 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 27.00 _diffrn_measured_fraction_theta_max 0.8972 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.8972 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8173 _reflns_number_gt 5013 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1756 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8156 _refine_ls_number_parameters 532 _refine_ls_goodness_of_fit_ref 1.357 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.80 _refine_diff_density_min -0.70 _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) ; O O 0.011 0.006 ;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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1) Cl -0.9685(1) -0.9088(1) -0.75050(8) 0.1057(5) Uani 1.00 d . . . Cl(2) Cl -0.9317(1) -1.0655(1) -0.60929(8) 0.1100(5) Uani 1.00 d . . . Cl(3) Cl -0.7102(1) -1.0412(1) -0.6782(1) 0.1191(6) Uani 1.00 d . . . Cl(4) Cl -1.0712(1) -0.5653(1) -0.65768(10) 0.1218(6) Uani 1.00 d . . . Cl(5) Cl -0.9701(2) -0.7425(2) -0.5274(1) 0.1788(9) Uani 1.00 d . . . Cl(6) Cl -0.8185(2) -0.6177(2) -0.58816(10) 0.1372(7) Uani 1.00 d . . . O(1) O -0.9716(2) -0.1267(2) -0.9090(1) 0.0477(6) Uani 1.00 d . . . O(2) O -0.3484(2) -0.3722(2) -0.7137(1) 0.0493(7) Uani 1.00 d . . . O(3) O -0.7246(2) -0.2882(2) -0.8023(1) 0.0334(5) Uani 1.00 d . . . C(1) C -0.6507(3) -0.6882(2) -0.7992(2) 0.0315(7) Uani 1.00 d . . . C(2) C -0.7524(3) -0.5762(2) -0.8171(2) 0.0320(7) Uani 1.00 d . . . C(3) C -0.8698(3) -0.5625(3) -0.8572(2) 0.0404(8) Uani 1.00 d . . . C(4) C -0.8806(3) -0.6592(3) -0.8841(2) 0.0454(9) Uani 1.00 d . . . C(5) C -0.7725(3) -0.7722(3) -0.8779(2) 0.0418(9) Uani 1.00 d . . . C(6) C -0.7762(4) -0.8699(3) -0.9157(2) 0.060(1) Uani 1.00 d . . . C(7) C -0.6681(4) -0.9741(3) -0.9163(2) 0.070(1) Uani 1.00 d . . . C(8) C -0.5501(4) -0.9876(3) -0.8803(2) 0.061(1) Uani 1.00 d . . . C(9) C -0.5424(3) -0.8979(3) -0.8413(2) 0.0453(9) Uani 1.00 d . . . C(10) C -0.6545(3) -0.7879(2) -0.8368(2) 0.0344(8) Uani 1.00 d . . . C(11) C -0.5372(3) -0.6993(2) -0.7468(2) 0.0324(7) Uani 1.00 d . . . C(12) C -0.4962(3) -0.6084(2) -0.7535(2) 0.0314(7) Uani 1.00 d . . . C(13) C -0.3743(3) -0.6264(3) -0.7173(2) 0.0382(8) Uani 1.00 d . . . C(14) C -0.3023(3) -0.7264(3) -0.6689(2) 0.0398(8) Uani 1.00 d . . . C(15) C -0.3525(3) -0.8110(3) -0.6492(2) 0.0391(8) Uani 1.00 d . . . C(16) C -0.2898(3) -0.9051(3) -0.5891(2) 0.0498(9) Uani 1.00 d . . . C(17) C -0.3428(4) -0.9816(3) -0.5665(2) 0.056(1) Uani 1.00 d . . . C(18) C -0.4622(4) -0.9673(3) -0.6025(2) 0.053(1) Uani 1.00 d . . . C(19) C -0.5253(3) -0.8783(3) -0.6615(2) 0.0424(9) Uani 1.00 d . . . C(20) C -0.4719(3) -0.7977(2) -0.6881(2) 0.0344(7) Uani 1.00 d . . . C(21) C -0.7296(3) -0.4736(2) -0.7905(2) 0.0303(7) Uani 1.00 d . . . C(22) C -0.8058(3) -0.3473(2) -0.8299(2) 0.0312(7) Uani 1.00 d . . . C(23) C -0.9418(3) -0.2746(2) -0.7993(2) 0.0341(8) Uani 1.00 d . . . C(24) C -0.9956(3) -0.3067(3) -0.7300(2) 0.0411(9) Uani 1.00 d . . . C(25) C -1.1178(3) -0.2295(3) -0.7036(2) 0.0493(10) Uani 1.00 d . . . C(26) C -1.1881(3) -0.1202(3) -0.7459(2) 0.054(1) Uani 1.00 d . . . C(27) C -1.1389(3) -0.0874(3) -0.8140(2) 0.0491(9) Uani 1.00 d . . . C(28) C -1.0166(3) -0.1646(3) -0.8400(2) 0.0389(8) Uani 1.00 d . . . C(29) C -0.8865(3) -0.2151(3) -0.9553(2) 0.0389(8) Uani 1.00 d . . . C(30) C -0.8792(3) -0.1807(3) -1.0357(2) 0.0486(9) Uani 1.00 d . . . C(31) C -0.8036(3) -0.2659(3) -1.0869(2) 0.0505(10) Uani 1.00 d . . . C(32) C -0.7391(3) -0.3839(3) -1.0569(2) 0.0461(9) Uani 1.00 d . . . C(33) C -0.7434(3) -0.4153(3) -0.9756(2) 0.0373(8) Uani 1.00 d . . . C(34) C -0.8136(3) -0.3303(2) -0.9216(2) 0.0323(7) Uani 1.00 d . . . C(35) C -0.5859(2) -0.4942(2) -0.8003(2) 0.0299(7) Uani 1.00 d . . . C(36) C -0.5895(3) -0.3723(2) -0.7791(2) 0.0305(7) Uani 1.00 d . . . C(37) C -0.4941(3) -0.3402(2) -0.8291(2) 0.0328(7) Uani 1.00 d . . . C(38) C -0.5168(3) -0.3077(3) -0.9122(2) 0.0402(9) Uani 1.00 d . . . C(39) C -0.4225(4) -0.2894(3) -0.9583(2) 0.0491(10) Uani 1.00 d . . . C(40) C -0.3053(4) -0.3032(3) -0.9235(2) 0.055(1) Uani 1.00 d . . . C(41) C -0.2827(3) -0.3317(3) -0.8417(2) 0.053(1) Uani 1.00 d . . . C(42) C -0.3783(3) -0.3475(3) -0.7952(2) 0.0391(9) Uani 1.00 d . . . C(43) C -0.4495(3) -0.3626(3) -0.6626(2) 0.0419(9) Uani 1.00 d . . . C(44) C -0.4243(3) -0.3563(3) -0.5817(2) 0.058(1) Uani 1.00 d . . . C(45) C -0.5179(4) -0.3485(4) -0.5260(2) 0.066(1) Uani 1.00 d . . . C(46) C -0.6366(3) -0.3447(3) -0.5507(2) 0.057(1) Uani 1.00 d . . . C(47) C -0.6623(3) -0.3502(3) -0.6317(2) 0.0416(9) Uani 1.00 d . . . C(48) C -0.5667(3) -0.3621(2) -0.6898(2) 0.0352(8) Uani 1.00 d . . . C(49) C -0.8612(4) -1.0419(3) -0.6978(2) 0.061(1) Uani 1.00 d . . . C(50) C -0.9303(5) -0.6744(5) -0.6122(3) 0.109(2) Uani 1.00 d . . . H(1) H -0.9417 -0.4847 -0.8657 0.0481 Uiso 1.00 calc . . . H(2) H -0.9643 -0.6497 -0.9071 0.0528 Uiso 1.00 calc . . . H(3) H -0.8584 -0.8606 -0.9421 0.0697 Uiso 1.00 calc . . . H(4) H -0.6717 -1.0382 -0.9435 0.0811 Uiso 1.00 calc . . . H(5) H -0.4725 -1.0624 -0.8822 0.0733 Uiso 1.00 calc . . . H(6) H -0.4597 -0.9090 -0.8166 0.0542 Uiso 1.00 calc . . . H(7) H -0.3421 -0.5659 -0.7267 0.0455 Uiso 1.00 calc . . . H(8) H -0.2169 -0.7401 -0.6483 0.0478 Uiso 1.00 calc . . . H(9) H -0.2075 -0.9153 -0.5643 0.0595 Uiso 1.00 calc . . . H(10) H -0.2991 -1.0452 -0.5253 0.0670 Uiso 1.00 calc . . . H(11) H -0.5009 -1.0211 -0.5849 0.0618 Uiso 1.00 calc . . . H(12) H -0.6078 -0.8694 -0.6859 0.0514 Uiso 1.00 calc . . . H(13) H -0.7452 -0.4701 -0.7332 0.0376 Uiso 1.00 calc . . . H(14) H -0.9469 -0.3827 -0.7010 0.0497 Uiso 1.00 calc . . . H(15) H -1.1537 -0.2517 -0.6558 0.0593 Uiso 1.00 calc . . . H(16) H -1.2732 -0.0674 -0.7267 0.0642 Uiso 1.00 calc . . . H(17) H -1.1882 -0.0122 -0.8438 0.0585 Uiso 1.00 calc . . . H(18) H -0.9268 -0.0987 -1.0557 0.0564 Uiso 1.00 calc . . . H(19) H -0.7951 -0.2434 -1.1427 0.0606 Uiso 1.00 calc . . . H(20) H -0.6904 -0.4440 -1.0933 0.0545 Uiso 1.00 calc . . . H(21) H -0.6984 -0.4974 -0.9558 0.0449 Uiso 1.00 calc . . . H(22) H -0.5667 -0.5029 -0.8571 0.0366 Uiso 1.00 calc . . . H(23) H -0.5984 -0.2988 -0.9374 0.0482 Uiso 1.00 calc . . . H(24) H -0.4412 -0.2670 -1.0164 0.0604 Uiso 1.00 calc . . . H(25) H -0.2395 -0.2928 -0.9565 0.0657 Uiso 1.00 calc . . . H(26) H -0.2002 -0.3417 -0.8164 0.0624 Uiso 1.00 calc . . . H(27) H -0.3403 -0.3586 -0.5648 0.0693 Uiso 1.00 calc . . . H(28) H -0.5009 -0.3456 -0.4688 0.0788 Uiso 1.00 calc . . . H(29) H -0.7031 -0.3391 -0.5117 0.0680 Uiso 1.00 calc . . . H(30) H -0.7471 -0.3442 -0.6491 0.0506 Uiso 1.00 calc . . . H(31) H -0.8463 -1.1058 -0.7324 0.0728 Uiso 1.00 calc . . . H(32) H -0.8891 -0.7343 -0.6536 0.1281 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 Cl(1) 0.1041(10) 0.0888(9) 0.0980(9) -0.0203(8) -0.0254(7) 0.0214(7) Cl(2) 0.0880(9) 0.106(1) 0.1102(10) -0.0203(8) 0.0220(7) 0.0148(8) Cl(3) 0.0710(8) 0.0887(10) 0.208(2) -0.0472(8) -0.0214(9) 0.0112(10) Cl(4) 0.0931(10) 0.121(1) 0.151(1) -0.0546(9) -0.0486(9) 0.0565(10) Cl(5) 0.173(2) 0.170(2) 0.187(2) -0.083(2) -0.057(1) 0.100(2) Cl(6) 0.0862(10) 0.199(2) 0.128(1) -0.066(1) -0.0268(8) 0.013(1) O(1) 0.048(1) 0.028(1) 0.050(1) 0.0001(10) 0.0073(10) -0.0012(9) O(2) 0.041(1) 0.067(2) 0.045(1) -0.028(1) -0.0021(10) -0.011(1) O(3) 0.031(1) 0.0258(10) 0.039(1) -0.0081(8) -0.0016(8) -0.0044(8) C(1) 0.031(1) 0.030(1) 0.032(1) -0.011(1) 0.002(1) -0.003(1) C(2) 0.031(1) 0.029(1) 0.034(1) -0.012(1) 0.001(1) -0.002(1) C(3) 0.030(2) 0.033(2) 0.052(2) -0.009(1) -0.003(1) -0.002(1) C(4) 0.038(2) 0.044(2) 0.055(2) -0.018(2) -0.008(1) -0.003(1) C(5) 0.047(2) 0.038(2) 0.043(2) -0.021(1) 0.000(1) -0.005(1) C(6) 0.068(2) 0.051(2) 0.070(2) -0.033(2) -0.009(2) -0.011(2) C(7) 0.087(3) 0.041(2) 0.083(3) -0.027(2) -0.009(2) -0.019(2) C(8) 0.069(3) 0.034(2) 0.069(2) -0.009(2) -0.001(2) -0.014(2) C(9) 0.050(2) 0.033(2) 0.047(2) -0.012(1) -0.001(1) -0.004(1) C(10) 0.039(2) 0.029(1) 0.033(1) -0.012(1) 0.002(1) 0.000(1) C(11) 0.028(1) 0.030(1) 0.032(1) -0.006(1) 0.003(1) -0.003(1) C(12) 0.029(1) 0.030(1) 0.031(1) -0.008(1) 0.001(1) -0.003(1) C(13) 0.032(2) 0.038(2) 0.042(2) -0.012(1) 0.002(1) -0.008(1) C(14) 0.028(1) 0.040(2) 0.044(2) -0.008(1) -0.003(1) -0.004(1) C(15) 0.033(2) 0.039(2) 0.031(2) -0.002(1) 0.002(1) -0.004(1) C(16) 0.043(2) 0.049(2) 0.039(2) -0.003(2) -0.006(1) 0.001(1) C(17) 0.057(2) 0.047(2) 0.042(2) -0.002(2) -0.002(2) 0.011(1) C(18) 0.061(2) 0.047(2) 0.044(2) -0.018(2) 0.008(2) 0.009(1) C(19) 0.044(2) 0.041(2) 0.037(2) -0.013(1) 0.003(1) 0.002(1) C(20) 0.032(1) 0.033(2) 0.032(1) -0.007(1) 0.004(1) -0.004(1) C(21) 0.026(1) 0.025(1) 0.034(1) -0.006(1) -0.002(1) -0.003(1) C(22) 0.029(1) 0.026(1) 0.035(2) -0.008(1) -0.001(1) -0.004(1) C(23) 0.029(1) 0.032(2) 0.038(2) -0.009(1) -0.001(1) -0.010(1) C(24) 0.035(2) 0.041(2) 0.044(2) -0.013(1) 0.002(1) -0.006(1) C(25) 0.039(2) 0.058(2) 0.050(2) -0.019(2) 0.009(1) -0.014(2) C(26) 0.034(2) 0.055(2) 0.062(2) -0.006(2) 0.007(1) -0.019(2) C(27) 0.039(2) 0.039(2) 0.053(2) 0.000(1) 0.001(1) -0.009(1) C(28) 0.034(2) 0.032(2) 0.042(2) -0.006(1) 0.001(1) -0.009(1) C(29) 0.036(2) 0.031(2) 0.043(2) -0.007(1) -0.001(1) -0.007(1) C(30) 0.048(2) 0.039(2) 0.047(2) -0.008(2) -0.005(1) 0.008(1) C(31) 0.055(2) 0.051(2) 0.035(2) -0.013(2) -0.001(1) 0.002(1) C(32) 0.048(2) 0.043(2) 0.040(2) -0.012(2) 0.000(1) -0.009(1) C(33) 0.039(2) 0.030(2) 0.037(2) -0.008(1) -0.004(1) -0.005(1) C(34) 0.029(1) 0.029(1) 0.034(2) -0.009(1) -0.004(1) -0.002(1) C(35) 0.027(1) 0.027(1) 0.032(1) -0.009(1) 0.000(1) -0.003(1) C(36) 0.028(1) 0.028(1) 0.032(1) -0.008(1) -0.001(1) -0.005(1) C(37) 0.035(2) 0.025(1) 0.037(2) -0.012(1) 0.004(1) -0.006(1) C(38) 0.047(2) 0.033(2) 0.039(2) -0.016(1) 0.004(1) -0.003(1) C(39) 0.068(2) 0.041(2) 0.042(2) -0.027(2) 0.014(2) -0.006(1) C(40) 0.059(2) 0.050(2) 0.065(2) -0.031(2) 0.023(2) -0.011(2) C(41) 0.044(2) 0.056(2) 0.069(2) -0.029(2) 0.012(2) -0.019(2) C(42) 0.041(2) 0.039(2) 0.041(2) -0.019(1) 0.006(1) -0.011(1) C(43) 0.039(2) 0.043(2) 0.040(2) -0.014(1) 0.001(1) -0.009(1) C(44) 0.049(2) 0.073(3) 0.047(2) -0.019(2) -0.007(2) -0.019(2) C(45) 0.065(3) 0.082(3) 0.036(2) -0.014(2) -0.005(2) -0.018(2) C(46) 0.053(2) 0.069(3) 0.036(2) -0.012(2) 0.010(2) -0.012(2) C(47) 0.040(2) 0.042(2) 0.036(2) -0.011(1) 0.003(1) -0.007(1) C(48) 0.037(2) 0.030(1) 0.035(2) -0.010(1) 0.000(1) -0.005(1) C(49) 0.060(2) 0.054(2) 0.067(2) -0.022(2) -0.006(2) -0.014(2) C(50) 0.079(3) 0.102(4) 0.125(4) -0.018(3) -0.024(3) -0.007(3) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _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 Cl(1) C(49) 1.750(4) . . yes Cl(2) C(49) 1.730(4) . . yes Cl(3) C(49) 1.730(4) . . yes Cl(4) C(50) 1.715(5) . . yes Cl(5) C(50) 1.746(6) . . yes Cl(6) C(50) 1.742(6) . . yes O(1) C(28) 1.382(4) . . yes O(1) C(29) 1.388(3) . . yes O(2) C(42) 1.374(4) . . yes O(2) C(43) 1.382(4) . . yes O(3) C(22) 1.485(3) . . yes O(3) C(36) 1.460(3) . . yes C(1) C(2) 1.387(4) . . yes C(1) C(10) 1.446(4) . . yes C(1) C(11) 1.494(4) . . yes C(2) C(3) 1.414(4) . . yes C(2) C(21) 1.503(4) . . yes C(3) C(4) 1.368(4) . . yes C(4) C(5) 1.409(4) . . yes C(5) C(6) 1.425(4) . . yes C(5) C(10) 1.421(4) . . yes C(6) C(7) 1.346(5) . . yes C(7) C(8) 1.391(5) . . yes C(8) C(9) 1.364(5) . . yes C(9) C(10) 1.416(4) . . yes C(11) C(12) 1.393(4) . . yes C(11) C(20) 1.434(4) . . yes C(12) C(13) 1.416(4) . . yes C(12) C(35) 1.506(4) . . yes C(13) C(14) 1.361(4) . . yes C(14) C(15) 1.414(4) . . yes C(15) C(16) 1.414(4) . . yes C(15) C(20) 1.427(4) . . yes C(16) C(17) 1.356(5) . . yes C(17) C(18) 1.403(5) . . yes C(18) C(19) 1.366(4) . . yes C(19) C(20) 1.420(4) . . yes C(21) C(22) 1.532(4) . . yes C(21) C(35) 1.530(4) . . yes C(22) C(23) 1.510(4) . . yes C(22) C(34) 1.516(4) . . yes C(23) C(24) 1.406(4) . . yes C(23) C(28) 1.390(4) . . yes C(24) C(25) 1.386(4) . . yes C(25) C(26) 1.386(5) . . yes C(26) C(27) 1.368(5) . . yes C(27) C(28) 1.384(4) . . yes C(29) C(30) 1.382(4) . . yes C(29) C(34) 1.390(4) . . yes C(30) C(31) 1.385(4) . . yes C(31) C(32) 1.388(4) . . yes C(32) C(33) 1.382(4) . . yes C(33) C(34) 1.399(4) . . yes C(35) C(36) 1.569(4) . . yes C(36) C(37) 1.520(4) . . yes C(36) C(48) 1.525(4) . . yes C(37) C(38) 1.399(4) . . yes C(37) C(42) 1.380(4) . . yes C(38) C(39) 1.389(4) . . yes C(39) C(40) 1.374(5) . . yes C(40) C(41) 1.372(5) . . yes C(41) C(42) 1.393(4) . . yes C(43) C(44) 1.385(4) . . yes C(43) C(48) 1.388(4) . . yes C(44) C(45) 1.371(5) . . yes C(45) C(46) 1.375(5) . . yes C(46) C(47) 1.384(4) . . yes C(47) C(48) 1.404(4) . . 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(28) O(1) C(29) 116.3(2) . . . yes C(42) O(2) C(43) 117.6(2) . . . yes C(22) O(3) C(36) 112.8(2) . . . yes C(2) C(1) C(10) 118.4(2) . . . yes C(2) C(1) C(11) 118.6(2) . . . yes C(10) C(1) C(11) 122.8(2) . . . yes C(1) C(2) C(3) 120.8(3) . . . yes C(1) C(2) C(21) 115.8(2) . . . yes C(3) C(2) C(21) 123.4(2) . . . yes C(2) C(3) C(4) 120.2(3) . . . yes C(3) C(4) C(5) 120.8(3) . . . yes C(4) C(5) C(6) 121.4(3) . . . yes C(4) C(5) C(10) 119.5(3) . . . yes C(6) C(5) C(10) 119.0(3) . . . yes C(5) C(6) C(7) 120.9(3) . . . yes C(6) C(7) C(8) 120.2(3) . . . yes C(7) C(8) C(9) 121.1(3) . . . yes C(8) C(9) C(10) 120.8(3) . . . yes C(1) C(10) C(5) 118.8(3) . . . yes C(1) C(10) C(9) 123.1(3) . . . yes C(5) C(10) C(9) 117.8(3) . . . yes C(1) C(11) C(12) 118.5(2) . . . yes C(1) C(11) C(20) 122.6(3) . . . yes C(12) C(11) C(20) 118.8(2) . . . yes C(11) C(12) C(13) 119.7(2) . . . yes C(11) C(12) C(35) 117.3(2) . . . yes C(13) C(12) C(35) 123.0(2) . . . yes C(12) C(13) C(14) 121.2(3) . . . yes C(13) C(14) C(15) 120.3(3) . . . yes C(14) C(15) C(16) 121.1(3) . . . yes C(14) C(15) C(20) 119.3(3) . . . yes C(16) C(15) C(20) 119.6(3) . . . yes C(15) C(16) C(17) 121.1(3) . . . yes C(16) C(17) C(18) 119.9(3) . . . yes C(17) C(18) C(19) 120.9(3) . . . yes C(18) C(19) C(20) 121.0(3) . . . yes C(11) C(20) C(15) 119.0(3) . . . yes C(11) C(20) C(19) 123.3(3) . . . yes C(15) C(20) C(19) 117.5(3) . . . yes C(2) C(21) C(22) 121.5(2) . . . yes C(2) C(21) C(35) 111.6(2) . . . yes C(22) C(21) C(35) 102.4(2) . . . yes O(3) C(22) C(21) 101.3(2) . . . yes O(3) C(22) C(23) 104.5(2) . . . yes O(3) C(22) C(34) 106.4(2) . . . yes C(21) C(22) C(23) 117.2(2) . . . yes C(21) C(22) C(34) 118.0(2) . . . yes C(23) C(22) C(34) 107.7(2) . . . yes C(22) C(23) C(24) 125.0(2) . . . yes C(22) C(23) C(28) 117.4(3) . . . yes C(24) C(23) C(28) 117.5(3) . . . yes C(23) C(24) C(25) 120.4(3) . . . yes C(24) C(25) C(26) 120.0(3) . . . yes C(25) C(26) C(27) 120.8(3) . . . yes C(26) C(27) C(28) 119.1(3) . . . yes O(1) C(28) C(23) 121.2(2) . . . yes O(1) C(28) C(27) 116.6(3) . . . yes C(23) C(28) C(27) 122.2(3) . . . yes O(1) C(29) C(30) 115.9(3) . . . yes O(1) C(29) C(34) 121.1(3) . . . yes C(30) C(29) C(34) 123.0(3) . . . yes C(29) C(30) C(31) 119.1(3) . . . yes C(30) C(31) C(32) 119.3(3) . . . yes C(31) C(32) C(33) 120.4(3) . . . yes C(32) C(33) C(34) 121.4(3) . . . yes C(22) C(34) C(29) 116.5(2) . . . yes C(22) C(34) C(33) 126.8(2) . . . yes C(29) C(34) C(33) 116.2(2) . . . yes C(12) C(35) C(21) 109.6(2) . . . yes C(12) C(35) C(36) 120.8(2) . . . yes C(21) C(35) C(36) 102.5(2) . . . yes O(3) C(36) C(35) 102.6(2) . . . yes O(3) C(36) C(37) 109.2(2) . . . yes O(3) C(36) C(48) 108.2(2) . . . yes C(35) C(36) C(37) 111.9(2) . . . yes C(35) C(36) C(48) 115.4(2) . . . yes C(37) C(36) C(48) 109.2(2) . . . yes C(36) C(37) C(38) 121.4(2) . . . yes C(36) C(37) C(42) 121.3(2) . . . yes C(38) C(37) C(42) 117.3(3) . . . yes C(37) C(38) C(39) 120.4(3) . . . yes C(38) C(39) C(40) 120.8(3) . . . yes C(39) C(40) C(41) 119.6(3) . . . yes C(40) C(41) C(42) 119.5(3) . . . yes O(2) C(42) C(37) 122.7(3) . . . yes O(2) C(42) C(41) 115.2(3) . . . yes C(37) C(42) C(41) 122.2(3) . . . yes O(2) C(43) C(44) 115.0(3) . . . yes O(2) C(43) C(48) 122.7(3) . . . yes C(44) C(43) C(48) 122.3(3) . . . yes C(43) C(44) C(45) 119.4(3) . . . yes C(44) C(45) C(46) 120.1(3) . . . yes C(45) C(46) C(47) 120.5(3) . . . yes C(46) C(47) C(48) 120.7(3) . . . yes C(36) C(48) C(43) 120.7(3) . . . yes C(36) C(48) C(47) 122.3(3) . . . yes C(43) C(48) C(47) 117.0(3) . . . yes Cl(1) C(49) Cl(2) 110.2(2) . . . yes Cl(1) C(49) Cl(3) 110.8(2) . . . yes Cl(2) C(49) Cl(3) 111.2(2) . . . yes Cl(4) C(50) Cl(5) 109.9(3) . . . yes Cl(4) C(50) Cl(6) 111.0(3) . . . yes Cl(5) C(50) Cl(6) 112.1(3) . . . yes #------------------------------------------------------------------------------ data_050516r _database_code_depnum_ccdc_archive 'CCDC 273466' _audit_creation_date 'Thu Jun 9 10:47:37 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C99 H60 Cl30 O4 Sb4 ' _chemical_formula_moiety ? _chemical_formula_weight 2864.15 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2 ' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z 1/4-x,1/4+y,1/4+z 1/4+x,1/4-y,1/4+z x,1/2+y,1/2+z -x,1/2-y,1/2+z 1/4-x,3/4+y,3/4+z 1/4+x,3/4-y,3/4+z 1/2+x,y,1/2+z 1/2-x,-y,1/2+z 3/4-x,1/4+y,3/4+z 3/4+x,1/4-y,3/4+z 1/2+x,1/2+y,z 1/2-x,1/2-y,z 3/4-x,3/4+y,1/4+z 3/4+x,3/4-y,1/4+z _cell_length_a 57.17(1) _cell_length_b 35.880(9) _cell_length_c 10.483(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 21504(8) _cell_formula_units_Z 8 _cell_measurement_reflns_used 11176 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.010 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.791 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.982 _exptl_absorpt_correction_T_max 0.982 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 41676 _diffrn_reflns_av_R_equivalents 0.144 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9692 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9692 _diffrn_reflns_limit_h_min -63 _diffrn_reflns_limit_h_max 72 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 9 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6324 _reflns_number_gt 1582 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.2134 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6324 _refine_ls_number_parameters 610 _refine_ls_goodness_of_fit_ref 0.451 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0069 _refine_diff_density_max 3.62 #--The largest peak appeared very close to Sb2 (0.04 angstrom apart) _refine_diff_density_min -1.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.17(10) 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) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb Sb -0.587 1.546 ;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 Sb(1) Sb 0.86945(3) 0.11871(4) 0.4201 0.0428(4) Uani 1.00 d . . . Sb(2) Sb 0.77124(3) 0.09002(5) 0.7908(2) 0.0416(4) Uani 1.00 d . . . Cl(1) Cl 0.9054(1) 0.1475(3) 0.3788(9) 0.086(2) Uani 1.00 d . . . Cl(2) Cl 0.8822(1) 0.0643(2) 0.3169(8) 0.067(2) Uani 1.00 d . . . Cl(3) Cl 0.8333(1) 0.0915(2) 0.4639(7) 0.059(2) Uani 1.00 d . . . Cl(4) Cl 0.8562(2) 0.1736(2) 0.5194(9) 0.096(3) Uani 1.00 d . . . Cl(5) Cl 0.8836(1) 0.0972(2) 0.6194(7) 0.069(2) Uani 1.00 d . . . Cl(6) Cl 0.8547(1) 0.1414(2) 0.2239(6) 0.046(2) Uani 1.00 d . . . Cl(7) Cl 0.7755(1) 0.1331(2) 0.9594(7) 0.059(2) Uani 1.00 d . . . Cl(8) Cl 0.8115(1) 0.0748(2) 0.8061(8) 0.059(2) Uani 1.00 d . . . Cl(9) Cl 0.7678(1) 0.0454(2) 0.6253(6) 0.061(2) Uani 1.00 d . . . Cl(10) Cl 0.7310(1) 0.1034(2) 0.7780(7) 0.054(2) Uani 1.00 d . . . Cl(11) Cl 0.7625(1) 0.0435(2) 0.9429(6) 0.047(2) Uani 1.00 d . . . Cl(12) Cl 0.7800(1) 0.1363(2) 0.6423(8) 0.081(2) Uani 1.00 d . . . Cl(13) Cl 0.5218(3) 0.0789(5) 0.056(2) 0.168(6) Uani 1.00 d . . . Cl(14) Cl 0.5566(5) 0.0162(4) 0.124(2) 0.29(1) Uani 1.00 d . . . Cl(15) Cl 0.0234(2) 0.0143(5) 0.283(2) 0.148(5) Uani 1.00 d . . . O(1) O 0.8836(3) -0.0210(4) 0.398(2) 0.040(4) Uani 1.00 d . . . O(2) O 0.8297(3) 0.0674(4) 0.103(2) 0.041(4) Uani 1.00 d . . . C(1) C 0.8120(4) -0.1281(6) 0.085(2) 0.032(5) Uani 1.00 d . . . C(2) C 0.8277(4) -0.1115(5) 0.172(2) 0.034(5) Uani 1.00 d . . . C(3) C 0.8350(4) -0.1323(6) 0.276(2) 0.034(5) Uani 1.00 d . . . C(4) C 0.8273(4) -0.1668(6) 0.303(3) 0.042(6) Uani 1.00 d . . . C(5) C 0.8102(4) -0.1839(6) 0.221(2) 0.037(6) Uani 1.00 d . . . C(6) C 0.8006(5) -0.2173(7) 0.254(3) 0.056(8) Uani 1.00 d . . . C(7) C 0.7818(5) -0.2311(6) 0.195(3) 0.065(8) Uani 1.00 d . . . C(8) C 0.7707(5) -0.2097(8) 0.094(3) 0.061(8) Uani 1.00 d . . . C(9) C 0.7812(4) -0.1762(7) 0.055(3) 0.045(6) Uani 1.00 d . . . C(10) C 0.8010(4) -0.1635(6) 0.115(2) 0.035(5) Uani 1.00 d . . . C(11) C 0.8052(4) -0.1068(7) -0.031(2) 0.034(5) Uani 1.00 d . . . C(12) C 0.8072(4) -0.0674(6) -0.023(2) 0.037(5) Uani 1.00 d . . . C(13) C 0.7960(5) -0.0461(7) -0.121(2) 0.047(7) Uani 1.00 d . . . C(14) C 0.7862(4) -0.0606(7) -0.221(2) 0.044(6) Uani 1.00 d . . . C(15) C 0.7882(4) -0.0997(7) -0.247(2) 0.042(6) Uani 1.00 d . . . C(16) C 0.7813(5) -0.1143(8) -0.360(2) 0.059(7) Uani 1.00 d . . . C(17) C 0.7858(6) -0.1504(8) -0.392(3) 0.067(8) Uani 1.00 d . . . C(18) C 0.7967(5) -0.1738(7) -0.305(3) 0.054(7) Uani 1.00 d . . . C(19) C 0.8041(5) -0.1590(7) -0.190(3) 0.056(7) Uani 1.00 d . . . C(20) C 0.7985(4) -0.1225(6) -0.152(2) 0.037(5) Uani 1.00 d . . . C(21) C 0.8340(4) -0.0726(6) 0.160(3) 0.043(6) Uani 1.00 d . . . C(22) C 0.8506(4) -0.0565(6) 0.246(2) 0.040(5) Uani 1.00 d . . . C(23) C 0.8440(5) -0.0401(6) 0.357(2) 0.043(6) Uani 1.00 d . . . C(24) C 0.8211(5) -0.0393(8) 0.406(3) 0.056(7) Uani 1.00 d . . . C(25) C 0.8163(6) -0.020(1) 0.516(3) 0.08(1) Uani 1.00 d . . . C(26) C 0.8325(7) -0.0009(10) 0.578(3) 0.081(10) Uani 1.00 d . . . C(27) C 0.8546(6) -0.0017(6) 0.545(3) 0.061(7) Uani 1.00 d . . . C(28) C 0.8615(4) -0.0206(6) 0.429(2) 0.040(5) Uani 1.00 d . . . C(29) C 0.8909(4) -0.0392(6) 0.293(2) 0.041(5) Uani 1.00 d . . . C(30) C 0.9152(5) -0.0392(8) 0.270(3) 0.064(8) Uani 1.00 d . . . C(31) C 0.9233(5) -0.0595(9) 0.172(3) 0.074(9) Uani 1.00 d . . . C(32) C 0.9077(5) -0.0797(9) 0.095(3) 0.075(9) Uani 1.00 d . . . C(33) C 0.8850(5) -0.0800(7) 0.114(2) 0.046(6) Uani 1.00 d . . . C(34) C 0.8755(4) -0.0570(5) 0.219(2) 0.033(5) Uani 1.00 d . . . C(35) C 0.8191(4) -0.0504(6) 0.081(2) 0.045(6) Uani 1.00 d . . . C(36) C 0.8230(5) -0.0097(7) 0.080(3) 0.047(6) Uani 1.00 d . . . C(37) C 0.8417(5) 0.0073(6) 0.017(2) 0.041(5) Uani 1.00 d . . . C(38) C 0.8571(5) -0.0107(6) -0.062(2) 0.045(6) Uani 1.00 d . . . C(39) C 0.8745(5) 0.0069(8) -0.118(2) 0.056(7) Uani 1.00 d . . . C(40) C 0.8775(5) 0.0457(8) -0.102(3) 0.059(8) Uani 1.00 d . . . C(41) C 0.8631(4) 0.0655(7) -0.027(2) 0.045(6) Uani 1.00 d . . . C(42) C 0.8442(4) 0.0457(6) 0.028(2) 0.040(5) Uani 1.00 d . . . C(43) C 0.8109(4) 0.0523(6) 0.158(3) 0.040(5) Uani 1.00 d . . . C(44) C 0.7959(5) 0.0755(7) 0.220(3) 0.047(7) Uani 1.00 d . . . C(45) C 0.7769(4) 0.0638(7) 0.281(3) 0.051(6) Uani 1.00 d . . . C(46) C 0.7728(4) 0.0260(7) 0.277(3) 0.049(6) Uani 1.00 d . . . C(47) C 0.7860(5) 0.0031(7) 0.210(3) 0.055(8) Uani 1.00 d . . . C(48) C 0.8065(4) 0.0140(6) 0.153(2) 0.041(5) Uani 1.00 d . . . C(49) C 0.5458(9) 0.065(1) 0.105(5) 0.126(7) Uiso 1.00 d . . . C(50) C 0.0000 0.0000 0.384(7) 0.125(5) Uiso 1.00 d S . . H(1) H 0.8432 -0.1203 0.3481 0.0355 Uiso 1.00 calc . . . H(2) H 0.8382 -0.1818 0.3589 0.0544 Uiso 1.00 calc . . . H(3) H 0.8087 -0.2359 0.3081 0.0553 Uiso 1.00 calc . . . H(4) H 0.7757 -0.2579 0.2104 0.0566 Uiso 1.00 calc . . . H(5) H 0.7581 -0.2266 0.0390 0.0822 Uiso 1.00 calc . . . H(6) H 0.7733 -0.1616 -0.0070 0.0447 Uiso 1.00 calc . . . H(7) H 0.7966 -0.0183 -0.1074 0.0335 Uiso 1.00 calc . . . H(8) H 0.7776 -0.0437 -0.2698 0.0583 Uiso 1.00 calc . . . H(9) H 0.7753 -0.0981 -0.4225 0.0717 Uiso 1.00 calc . . . H(10) H 0.7800 -0.1634 -0.4660 0.0650 Uiso 1.00 calc . . . H(11) H 0.7998 -0.1990 -0.3274 0.0526 Uiso 1.00 calc . . . H(12) H 0.8123 -0.1757 -0.1283 0.0360 Uiso 1.00 calc . . . H(13) H 0.8455 -0.0745 0.1023 0.0648 Uiso 1.00 calc . . . H(14) H 0.8099 -0.0531 0.3544 0.0741 Uiso 1.00 calc . . . H(15) H 0.7988 -0.0222 0.5331 0.1092 Uiso 1.00 calc . . . H(16) H 0.8269 0.0174 0.6484 0.1186 Uiso 1.00 calc . . . H(17) H 0.8673 0.0114 0.5843 0.0709 Uiso 1.00 calc . . . H(18) H 0.9225 -0.0216 0.3313 0.0728 Uiso 1.00 calc . . . H(19) H 0.9394 -0.0543 0.1611 0.0715 Uiso 1.00 calc . . . H(20) H 0.9152 -0.0891 0.0342 0.0834 Uiso 1.00 calc . . . H(21) H 0.8754 -0.0939 0.0510 0.0383 Uiso 1.00 calc . . . H(22) H 0.8065 -0.0485 0.1364 0.0463 Uiso 1.00 calc . . . H(23) H 0.8550 -0.0375 -0.0738 0.0490 Uiso 1.00 calc . . . H(24) H 0.8847 -0.0083 -0.1729 0.0546 Uiso 1.00 calc . . . H(25) H 0.8908 0.0592 -0.1412 0.0716 Uiso 1.00 calc . . . H(26) H 0.8670 0.0903 -0.0051 0.0744 Uiso 1.00 calc . . . H(27) H 0.8011 0.0998 0.2381 0.0462 Uiso 1.00 calc . . . H(28) H 0.7659 0.0794 0.3126 0.0449 Uiso 1.00 calc . . . H(29) H 0.7608 0.0157 0.3377 0.0294 Uiso 1.00 calc . . . H(30) H 0.7809 -0.0229 0.2036 0.0848 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 Sb(1) 0.0531(9) 0.0389(7) 0.0365(7) -0.0097(7) -0.0037(7) 0.0050(7) Sb(2) 0.0361(7) 0.0511(8) 0.0378(7) 0.0052(7) -0.0012(7) 0.0037(7) Cl(1) 0.056(3) 0.102(5) 0.099(6) -0.043(4) -0.024(4) 0.053(4) Cl(2) 0.091(5) 0.044(3) 0.066(5) 0.022(3) 0.028(4) 0.010(3) Cl(3) 0.048(3) 0.070(4) 0.058(4) -0.007(3) 0.010(3) 0.016(3) Cl(4) 0.182(10) 0.044(4) 0.064(5) 0.009(5) -0.005(6) -0.028(3) Cl(5) 0.086(5) 0.079(5) 0.043(3) -0.015(4) -0.022(3) 0.026(3) Cl(6) 0.063(4) 0.034(3) 0.039(3) -0.006(3) -0.006(3) 0.006(2) Cl(7) 0.063(4) 0.050(4) 0.063(4) -0.005(3) 0.007(3) -0.014(3) Cl(8) 0.037(2) 0.077(4) 0.064(4) 0.013(3) -0.005(3) -0.013(4) Cl(9) 0.063(4) 0.089(5) 0.031(3) 0.002(4) 0.001(3) -0.019(3) Cl(10) 0.038(2) 0.069(4) 0.056(4) 0.013(3) 0.000(3) 0.010(3) Cl(11) 0.055(4) 0.047(3) 0.041(3) 0.000(3) -0.005(3) 0.003(2) Cl(12) 0.073(5) 0.085(4) 0.084(5) 0.004(4) 0.024(4) 0.069(3) Cl(13) 0.18(1) 0.21(1) 0.12(1) -0.099(10) 0.016(9) -0.03(1) Cl(14) 0.57(3) 0.110(9) 0.20(2) -0.18(1) -0.02(2) 0.01(1) Cl(15) 0.097(8) 0.21(1) 0.14(1) -0.041(8) 0.017(8) 0.02(1) O(1) 0.057(8) 0.014(6) 0.049(9) 0.004(6) -0.016(7) 0.006(6) O(2) 0.035(8) 0.033(8) 0.053(10) -0.007(6) -0.002(6) -0.003(7) C(1) 0.03(1) 0.025(9) 0.05(1) 0.007(7) -0.001(8) 0.005(8) C(2) 0.03(1) 0.026(8) 0.04(1) 0.009(7) -0.007(9) 0.005(8) C(3) 0.03(1) 0.038(10) 0.03(1) -0.006(8) -0.010(9) 0.001(8) C(4) 0.021(10) 0.036(10) 0.07(2) 0.004(8) -0.015(10) 0.01(1) C(5) 0.04(1) 0.03(1) 0.04(1) 0.002(8) -0.007(9) 0.008(8) C(6) 0.08(2) 0.03(1) 0.06(2) -0.02(1) -0.02(1) 0.02(1) C(7) 0.07(2) 0.02(1) 0.10(2) -0.01(1) -0.03(1) 0.01(1) C(8) 0.05(2) 0.06(2) 0.07(2) -0.02(1) 0.00(1) 0.02(1) C(9) 0.03(1) 0.05(1) 0.06(2) 0.002(8) -0.01(1) 0.00(1) C(10) 0.022(9) 0.033(10) 0.05(1) 0.000(7) 0.003(8) 0.022(9) C(11) 0.04(1) 0.040(8) 0.027(8) -0.001(9) 0.005(8) -0.008(7) C(12) 0.03(1) 0.039(8) 0.04(1) 0.009(9) -0.003(8) -0.002(8) C(13) 0.05(1) 0.06(2) 0.03(1) -0.01(1) -0.006(9) 0.014(9) C(14) 0.04(1) 0.047(10) 0.04(1) 0.00(1) -0.02(1) 0.013(10) C(15) 0.04(1) 0.047(10) 0.04(1) -0.01(1) -0.008(9) 0.007(8) C(16) 0.08(2) 0.06(1) 0.04(1) -0.02(1) -0.02(1) 0.01(1) C(17) 0.08(2) 0.07(1) 0.05(2) 0.00(1) -0.03(1) -0.01(1) C(18) 0.07(2) 0.03(1) 0.06(1) 0.00(1) -0.01(1) -0.021(10) C(19) 0.07(2) 0.05(1) 0.05(1) 0.02(1) 0.00(1) -0.01(1) C(20) 0.04(1) 0.038(9) 0.030(9) -0.027(8) -0.009(9) 0.002(7) C(21) 0.04(1) 0.025(8) 0.06(1) 0.008(8) -0.023(10) 0.001(10) C(22) 0.047(9) 0.03(1) 0.04(1) -0.005(10) -0.002(8) 0.001(8) C(23) 0.06(1) 0.04(1) 0.026(9) 0.012(10) -0.016(8) 0.014(8) C(24) 0.07(1) 0.05(2) 0.05(1) 0.01(1) 0.00(1) 0.01(1) C(25) 0.10(2) 0.11(3) 0.04(1) 0.01(2) 0.03(1) 0.00(1) C(26) 0.11(2) 0.08(2) 0.06(2) 0.04(2) -0.01(2) 0.00(2) C(27) 0.11(2) 0.02(1) 0.05(1) 0.01(1) 0.01(2) -0.01(1) C(28) 0.059(8) 0.022(10) 0.04(1) 0.021(8) -0.013(9) 0.007(8) C(29) 0.049(9) 0.05(1) 0.027(9) -0.013(9) -0.024(8) 0.014(7) C(30) 0.05(1) 0.05(2) 0.09(2) -0.01(1) -0.02(1) 0.02(1) C(31) 0.06(2) 0.09(2) 0.08(2) 0.03(1) 0.02(1) 0.05(1) C(32) 0.06(1) 0.10(2) 0.06(2) 0.05(1) 0.01(1) 0.03(1) C(33) 0.06(1) 0.04(1) 0.03(1) 0.02(1) 0.00(1) 0.008(9) C(34) 0.044(9) 0.004(8) 0.05(1) -0.008(8) -0.011(8) -0.001(7) C(35) 0.06(1) 0.033(9) 0.04(1) 0.023(9) -0.023(10) -0.008(9) C(36) 0.05(1) 0.037(9) 0.05(2) -0.002(9) -0.017(9) -0.002(10) C(37) 0.06(1) 0.029(8) 0.03(1) 0.017(8) -0.005(9) 0.013(8) C(38) 0.07(1) 0.02(1) 0.04(1) 0.024(9) -0.002(10) 0.004(9) C(39) 0.08(2) 0.06(1) 0.03(1) 0.02(1) 0.03(1) 0.00(1) C(40) 0.08(2) 0.06(1) 0.03(1) 0.00(1) 0.01(1) -0.01(1) C(41) 0.05(1) 0.04(1) 0.05(1) -0.004(9) -0.021(9) 0.001(9) C(42) 0.05(1) 0.031(8) 0.04(1) 0.007(8) -0.013(9) 0.000(9) C(43) 0.023(9) 0.035(8) 0.06(1) -0.002(7) -0.016(8) 0.003(10) C(44) 0.05(1) 0.03(1) 0.05(2) 0.003(9) 0.00(1) 0.00(1) C(45) 0.05(1) 0.049(10) 0.05(2) 0.01(1) 0.01(1) -0.01(1) C(46) 0.04(1) 0.052(10) 0.06(2) -0.01(1) 0.00(1) 0.02(1) C(47) 0.05(1) 0.04(1) 0.07(2) 0.01(1) -0.02(1) 0.01(1) C(48) 0.06(1) 0.033(8) 0.03(1) 0.001(8) -0.024(9) 0.008(8) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _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 Sb(1) Cl(1) 2.341(5) . . yes Sb(1) Cl(2) 2.347(5) . . yes Sb(1) Cl(3) 2.334(5) . . yes Sb(1) Cl(4) 2.352(5) . . yes Sb(1) Cl(5) 2.371(4) . . yes Sb(1) Cl(6) 2.367(4) . . yes Sb(2) Cl(7) 2.361(5) . . yes Sb(2) Cl(8) 2.371(4) . . yes Sb(2) Cl(9) 2.369(5) . . yes Sb(2) Cl(10) 2.353(4) . . yes Sb(2) Cl(11) 2.362(4) . . yes Sb(2) Cl(12) 2.332(4) . . yes Cl(13) C(49) 1.55(4) . . yes Cl(14) C(49) 1.86(4) . . yes Cl(15) C(50) 1.78(3) . . yes O(1) C(28) 1.30(2) . . yes O(1) C(29) 1.35(2) . . yes O(2) C(42) 1.38(2) . . yes O(2) C(43) 1.34(2) . . yes C(1) C(2) 1.41(2) . . yes C(1) C(10) 1.45(2) . . yes C(1) C(11) 1.49(2) . . yes C(2) C(3) 1.38(2) . . yes C(2) C(21) 1.45(2) . . yes C(3) C(4) 1.34(2) . . yes C(4) C(5) 1.44(2) . . yes C(5) C(6) 1.36(2) . . yes C(5) C(10) 1.43(2) . . yes C(6) C(7) 1.34(3) . . yes C(7) C(8) 1.45(3) . . yes C(8) C(9) 1.40(2) . . yes C(9) C(10) 1.37(2) . . yes C(11) C(12) 1.42(2) . . yes C(11) C(20) 1.44(2) . . yes C(12) C(13) 1.43(2) . . yes C(12) C(35) 1.42(2) . . yes C(13) C(14) 1.30(2) . . yes C(14) C(15) 1.43(2) . . yes C(15) C(16) 1.35(2) . . yes C(15) C(20) 1.42(2) . . yes C(16) C(17) 1.36(3) . . yes C(17) C(18) 1.39(3) . . yes C(18) C(19) 1.39(3) . . yes C(19) C(20) 1.41(2) . . yes C(21) C(22) 1.43(2) . . yes C(21) C(35) 1.43(2) . . yes C(22) C(23) 1.36(2) . . yes C(22) C(34) 1.45(2) . . yes C(23) C(24) 1.40(3) . . yes C(23) C(28) 1.44(2) . . yes C(24) C(25) 1.37(3) . . yes C(25) C(26) 1.33(3) . . yes C(26) C(27) 1.31(3) . . yes C(27) C(28) 1.45(2) . . yes C(29) C(30) 1.41(2) . . yes C(29) C(34) 1.33(2) . . yes C(30) C(31) 1.34(3) . . yes C(31) C(32) 1.40(3) . . yes C(32) C(33) 1.31(3) . . yes C(33) C(34) 1.48(2) . . yes C(35) C(36) 1.47(2) . . yes C(36) C(37) 1.40(2) . . yes C(36) C(48) 1.48(2) . . yes C(37) C(38) 1.37(2) . . yes C(37) C(42) 1.39(2) . . yes C(38) C(39) 1.32(2) . . yes C(39) C(40) 1.41(3) . . yes C(40) C(41) 1.34(3) . . yes C(41) C(42) 1.42(2) . . yes C(43) C(44) 1.36(2) . . yes C(43) C(48) 1.40(2) . . yes C(44) C(45) 1.33(2) . . yes C(45) C(46) 1.38(2) . . yes C(46) C(47) 1.32(3) . . yes C(47) C(48) 1.37(2) . . 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 Cl(1) Sb(1) Cl(2) 90.5(2) . . . yes Cl(1) Sb(1) Cl(3) 178.4(2) . . . yes Cl(1) Sb(1) Cl(4) 89.7(3) . . . yes Cl(1) Sb(1) Cl(5) 90.4(2) . . . yes Cl(1) Sb(1) Cl(6) 90.0(2) . . . yes Cl(2) Sb(1) Cl(3) 91.0(2) . . . yes Cl(2) Sb(1) Cl(4) 178.7(2) . . . yes Cl(2) Sb(1) Cl(5) 91.7(2) . . . yes Cl(2) Sb(1) Cl(6) 89.7(2) . . . yes Cl(3) Sb(1) Cl(4) 88.7(2) . . . yes Cl(3) Sb(1) Cl(5) 89.6(2) . . . yes Cl(3) Sb(1) Cl(6) 90.0(2) . . . yes Cl(4) Sb(1) Cl(5) 89.5(2) . . . yes Cl(4) Sb(1) Cl(6) 89.0(2) . . . yes Cl(5) Sb(1) Cl(6) 178.5(2) . . . yes Cl(7) Sb(2) Cl(8) 90.1(2) . . . yes Cl(7) Sb(2) Cl(9) 178.1(2) . . . yes Cl(7) Sb(2) Cl(10) 90.5(2) . . . yes Cl(7) Sb(2) Cl(11) 88.8(2) . . . yes Cl(7) Sb(2) Cl(12) 90.7(2) . . . yes Cl(8) Sb(2) Cl(9) 88.6(2) . . . yes Cl(8) Sb(2) Cl(10) 178.3(2) . . . yes Cl(8) Sb(2) Cl(11) 89.8(2) . . . yes Cl(8) Sb(2) Cl(12) 90.0(2) . . . yes Cl(9) Sb(2) Cl(10) 90.8(2) . . . yes Cl(9) Sb(2) Cl(11) 90.0(2) . . . yes Cl(9) Sb(2) Cl(12) 90.6(2) . . . yes Cl(10) Sb(2) Cl(11) 88.6(2) . . . yes Cl(10) Sb(2) Cl(12) 91.6(2) . . . yes Cl(11) Sb(2) Cl(12) 179.4(2) . . . yes C(28) O(1) C(29) 120(1) . . . yes C(42) O(2) C(43) 120(1) . . . yes C(2) C(1) C(10) 120(1) . . . yes C(2) C(1) C(11) 118(1) . . . yes C(10) C(1) C(11) 120(1) . . . yes C(1) C(2) C(3) 118(1) . . . yes C(1) C(2) C(21) 120(1) . . . yes C(3) C(2) C(21) 120(1) . . . yes C(2) C(3) C(4) 124(1) . . . yes C(3) C(4) C(5) 118(1) . . . yes C(4) C(5) C(6) 119(1) . . . yes C(4) C(5) C(10) 119(1) . . . yes C(6) C(5) C(10) 119(1) . . . yes C(5) C(6) C(7) 122(1) . . . yes C(6) C(7) C(8) 119(1) . . . yes C(7) C(8) C(9) 118(1) . . . yes C(8) C(9) C(10) 120(1) . . . yes C(1) C(10) C(5) 116(1) . . . yes C(1) C(10) C(9) 123(1) . . . yes C(5) C(10) C(9) 119(1) . . . yes C(1) C(11) C(12) 116(1) . . . yes C(1) C(11) C(20) 125(1) . . . yes C(12) C(11) C(20) 117(1) . . . yes C(11) C(12) C(13) 116(1) . . . yes C(11) C(12) C(35) 120(1) . . . yes C(13) C(12) C(35) 122(1) . . . yes C(12) C(13) C(14) 124(1) . . . yes C(13) C(14) C(15) 120(1) . . . yes C(14) C(15) C(16) 121(1) . . . yes C(14) C(15) C(20) 117(1) . . . yes C(16) C(15) C(20) 120(1) . . . yes C(15) C(16) C(17) 122(1) . . . yes C(16) C(17) C(18) 119(1) . . . yes C(17) C(18) C(19) 118(1) . . . yes C(18) C(19) C(20) 122(1) . . . yes C(11) C(20) C(15) 120(1) . . . yes C(11) C(20) C(19) 123(1) . . . yes C(15) C(20) C(19) 115(1) . . . yes C(2) C(21) C(22) 119(1) . . . yes C(2) C(21) C(35) 116(1) . . . yes C(22) C(21) C(35) 122(1) . . . yes C(21) C(22) C(23) 122(1) . . . yes C(21) C(22) C(34) 121(1) . . . yes C(23) C(22) C(34) 116(1) . . . yes C(22) C(23) C(24) 125(1) . . . yes C(22) C(23) C(28) 117(1) . . . yes C(24) C(23) C(28) 116(1) . . . yes C(23) C(24) C(25) 120(1) . . . yes C(24) C(25) C(26) 122(2) . . . yes C(25) C(26) C(27) 122(2) . . . yes C(26) C(27) C(28) 119(1) . . . yes O(1) C(28) C(23) 122(1) . . . yes O(1) C(28) C(27) 118(1) . . . yes C(23) C(28) C(27) 118(1) . . . yes O(1) C(29) C(30) 116(1) . . . yes O(1) C(29) C(34) 120(1) . . . yes C(30) C(29) C(34) 123(1) . . . yes C(29) C(30) C(31) 118(1) . . . yes C(30) C(31) C(32) 119(1) . . . yes C(31) C(32) C(33) 123(2) . . . yes C(32) C(33) C(34) 117(1) . . . yes C(22) C(34) C(29) 121(1) . . . yes C(22) C(34) C(33) 120(1) . . . yes C(29) C(34) C(33) 117(1) . . . yes C(12) C(35) C(21) 119(1) . . . yes C(12) C(35) C(36) 119(1) . . . yes C(21) C(35) C(36) 117(1) . . . yes C(35) C(36) C(37) 122(1) . . . yes C(35) C(36) C(48) 118(1) . . . yes C(37) C(36) C(48) 118(1) . . . yes C(36) C(37) C(38) 125(1) . . . yes C(36) C(37) C(42) 117(1) . . . yes C(38) C(37) C(42) 117(1) . . . yes C(37) C(38) C(39) 121(1) . . . yes C(38) C(39) C(40) 120(1) . . . yes C(39) C(40) C(41) 121(1) . . . yes C(40) C(41) C(42) 115(1) . . . yes O(2) C(42) C(37) 123(1) . . . yes O(2) C(42) C(41) 113(1) . . . yes C(37) C(42) C(41) 122(1) . . . yes O(2) C(43) C(44) 117(1) . . . yes O(2) C(43) C(48) 121(1) . . . yes C(44) C(43) C(48) 120(1) . . . yes C(43) C(44) C(45) 123(1) . . . yes C(44) C(45) C(46) 115(1) . . . yes C(45) C(46) C(47) 121(1) . . . yes C(46) C(47) C(48) 122(1) . . . yes C(36) C(48) C(43) 118(1) . . . yes C(36) C(48) C(47) 127(1) . . . yes C(43) C(48) C(47) 114(1) . . . yes Cl(13) C(49) Cl(14) 129(2) . . . yes Cl(15) C(50) Cl(15) 106(2) . . 2_555 yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------