Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2006 data_General _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name 'Mikiji Miyata' _publ_contact_author_address ; Material and Life Science Graduate School of Engineering, Osaka University 2-1 Yamadaoka Suita Osaka 565-0871 JAPAN ; _publ_contact_author_email MIYATA@MOLREC.MLS.ENG.OSAKA-U.AC.JP _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Guest-induced Inversion of an Asymmetric Host Layer in Inclusion Crystals of Cholic Acid ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; loop_ _publ_author_name 'Mikiji Miyata' 'Kazuaki Aburaya' 'Kenji Nakagawa' 'Kazunori Nakano' 'Kazuki Sada' 'Norimitsu Tohnai' ; N.Yoswathananont ; #------------------------------------------------------------------------------ data_aburaya74_ _database_code_depnum_ccdc_archive 'CCDC 297671' _audit_creation_date 'Wed Apr 26 22:38:25 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C57 H92 O10 ' _chemical_formula_moiety ? _chemical_formula_weight 937.35 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 7.478(1) _cell_length_b 25.381(5) _cell_length_c 13.776(3) _cell_angle_alpha 90 _cell_angle_beta 90.70(2) _cell_angle_gamma 90 _cell_volume 2614.5(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 28876 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 68.2 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.644 _exptl_absorpt_correction_T_max 0.882 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5419 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17474 _diffrn_reflns_av_R_equivalents 0.091 _diffrn_reflns_theta_max 68.19 _diffrn_measured_fraction_theta_max 0.9407 _diffrn_reflns_theta_full 68.19 _diffrn_measured_fraction_theta_full 0.9407 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # 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 4589 _reflns_number_gt 4090 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1680 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4589 _refine_ls_number_parameters 604 _refine_ls_goodness_of_fit_ref 1.630 _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 0.0004 _refine_diff_density_max 0.42 _refine_diff_density_min -0.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ;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 0.049 0.032 ;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 -0.6045(4) -0.3443(3) -0.9998(2) 0.0294(7) Uani 1.00 d . . . O(2) O -0.2129(4) -0.4398(3) -0.7683(2) 0.0250(7) Uani 1.00 d . . . O(3) O -0.6562(4) -0.3890(3) -0.5710(2) 0.0229(7) Uani 1.00 d . . . O(4) O -0.3086(4) -0.3368(3) -0.1134(2) 0.0311(8) Uani 1.00 d . . . O(5) O -0.0617(4) -0.3484(3) -0.1989(2) 0.0278(7) Uani 1.00 d . . . O(6) O 0.0663(4) -0.3357(3) -1.4981(2) 0.0287(7) Uani 1.00 d . . . O(7) O -0.3447(3) -0.2469(3) -1.2697(2) 0.0207(7) Uani 1.00 d . . . O(8) O 0.1110(4) -0.2917(3) -1.0667(2) 0.0211(7) Uani 1.00 d . . . O(9) O -0.2276(4) -0.3500(3) -0.6132(2) 0.0324(8) Uani 1.00 d . . . O(10) O -0.4735(4) -0.3339(3) -0.7010(2) 0.0287(7) Uani 1.00 d . . . C(1) C -0.8243(5) -0.4599(3) -0.8807(3) 0.0249(10) Uani 1.00 d . . . C(2) C -0.7881(5) -0.4021(3) -0.9067(3) 0.0257(10) Uani 1.00 d . . . C(3) C -0.6365(5) -0.3988(3) -0.9783(3) 0.0231(9) Uani 1.00 d . . . C(4) C -0.4702(5) -0.4256(3) -0.9372(3) 0.0219(9) Uani 1.00 d . . . C(5) C -0.5030(5) -0.4839(3) -0.9069(3) 0.0229(9) Uani 1.00 d . . . C(6) C -0.3326(5) -0.5097(3) -0.8671(3) 0.0242(10) Uani 1.00 d . . . C(7) C -0.2818(5) -0.4931(3) -0.7638(3) 0.0230(9) Uani 1.00 d . . . C(8) C -0.4404(5) -0.4965(3) -0.6936(3) 0.0197(9) Uani 1.00 d . . . C(9) C -0.6050(5) -0.4674(3) -0.7368(3) 0.0205(9) Uani 1.00 d . . . C(10) C -0.6629(5) -0.4890(3) -0.8375(3) 0.0199(8) Uani 1.00 d . . . C(11) C -0.7571(5) -0.4659(3) -0.6623(3) 0.0210(9) Uani 1.00 d . . . C(12) C -0.7021(5) -0.4439(3) -0.5622(3) 0.0203(9) Uani 1.00 d . . . C(13) C -0.5419(5) -0.4755(3) -0.5194(3) 0.0203(9) Uani 1.00 d . . . C(14) C -0.3919(5) -0.4735(3) -0.5950(3) 0.0174(8) Uani 1.00 d . . . C(15) C -0.2279(5) -0.4956(3) -0.5407(3) 0.0222(9) Uani 1.00 d . . . C(16) C -0.2522(5) -0.4757(3) -0.4352(3) 0.0250(10) Uani 1.00 d . . . C(17) C -0.4414(5) -0.4504(3) -0.4307(3) 0.0194(8) Uani 1.00 d . . . C(18) C -0.6032(6) -0.5317(3) -0.4954(3) 0.0236(10) Uani 1.00 d . . . C(19) C -0.7163(6) -0.5479(3) -0.8318(3) 0.028(1) Uani 1.00 d . . . C(20) C -0.5234(5) -0.4553(3) -0.3297(3) 0.0225(9) Uani 1.00 d . . . C(21) C -0.7103(5) -0.4296(3) -0.3212(3) 0.028(1) Uani 1.00 d . . . C(22) C -0.3950(5) -0.4319(3) -0.2518(3) 0.0240(10) Uani 1.00 d . . . C(23) C -0.3394(6) -0.3746(3) -0.2725(3) 0.029(1) Uani 1.00 d . . . C(24) C -0.2397(5) -0.3511(3) -0.1862(3) 0.0238(8) Uani 1.00 d . . . C(25) C 0.2650(5) -0.2170(3) -1.3764(3) 0.0209(9) Uani 1.00 d . . . C(26) C 0.2399(5) -0.2752(3) -1.4033(3) 0.0238(9) Uani 1.00 d . . . C(27) C 0.0867(5) -0.2809(3) -1.4764(3) 0.0240(9) Uani 1.00 d . . . C(28) C -0.0849(5) -0.2569(3) -1.4360(3) 0.0217(9) Uani 1.00 d . . . C(29) C -0.0625(5) -0.1992(3) -1.4064(3) 0.0199(9) Uani 1.00 d . . . C(30) C -0.2384(5) -0.1760(3) -1.3675(3) 0.0203(9) Uani 1.00 d . . . C(31) C -0.2827(5) -0.1931(3) -1.2634(3) 0.0193(8) Uani 1.00 d . . . C(32) C -0.1234(5) -0.1873(3) -1.1937(3) 0.0178(8) Uani 1.00 d . . . C(33) C 0.0461(5) -0.2142(3) -1.2335(3) 0.0175(8) Uani 1.00 d . . . C(34) C 0.0980(5) -0.1902(3) -1.3349(3) 0.0182(8) Uani 1.00 d . . . C(35) C 0.2012(5) -0.2135(3) -1.1595(3) 0.0229(9) Uani 1.00 d . . . C(36) C 0.1479(5) -0.2354(3) -1.0592(3) 0.0189(8) Uani 1.00 d . . . C(37) C -0.0147(5) -0.2065(3) -1.0182(3) 0.0195(8) Uani 1.00 d . . . C(38) C -0.1678(5) -0.2109(3) -1.0931(3) 0.0177(8) Uani 1.00 d . . . C(39) C -0.3321(5) -0.1907(3) -1.0419(3) 0.0224(9) Uani 1.00 d . . . C(40) C -0.3020(5) -0.2087(3) -0.9360(3) 0.0261(10) Uani 1.00 d . . . C(41) C -0.1092(5) -0.2326(3) -0.9293(3) 0.0195(9) Uani 1.00 d . . . C(42) C 0.0374(5) -0.1494(3) -0.9938(3) 0.0227(10) Uani 1.00 d . . . C(43) C 0.1415(6) -0.1310(3) -1.3276(3) 0.0270(10) Uani 1.00 d . . . C(44) C -0.0266(5) -0.2263(3) -0.8262(3) 0.0215(9) Uani 1.00 d . . . C(45) C 0.1640(5) -0.2480(3) -0.8172(3) 0.0252(10) Uani 1.00 d . . . C(46) C -0.1514(6) -0.2511(3) -0.7491(3) 0.0236(9) Uani 1.00 d . . . C(47) C -0.1946(6) -0.3093(3) -0.7698(3) 0.032(1) Uani 1.00 d . . . C(48) C -0.2992(6) -0.3327(3) -0.6874(3) 0.0249(9) Uani 1.00 d . . . C(49) C -0.9226(6) -0.0561(3) -0.7925(3) 0.0274(10) Uani 1.00 d . . . C(50) C -0.7541(6) -0.0787(3) -0.7868(3) 0.0257(10) Uani 1.00 d . . . C(51) C -0.7132(6) -0.1139(3) -0.7075(3) 0.0250(9) Uani 1.00 d . . . C(52) C -0.8436(6) -0.1241(3) -0.6398(3) 0.0275(10) Uani 1.00 d . . . C(53) C -1.0111(6) -0.1013(3) -0.6459(3) 0.029(1) Uani 1.00 d . . . C(54) C -1.0494(6) -0.0674(3) -0.7233(3) 0.030(1) Uani 1.00 d . . . C(55) C -0.9749(8) -0.0195(3) -0.8767(4) 0.041(1) Uani 1.00 d . . . C(56) C -0.6144(6) -0.0678(3) -0.8612(3) 0.034(1) Uani 1.00 d . . . C(57) C -0.5310(6) -0.1392(3) -0.6989(4) 0.035(1) Uani 1.00 d . . . H(1) H -0.9177 -0.4602 -0.8353 0.0299 Uiso 1.00 calc . . . H(2) H -0.8608 -0.4769 -0.9388 0.0299 Uiso 1.00 calc . . . H(3) H -0.8923 -0.3866 -0.9343 0.0304 Uiso 1.00 calc . . . H(4) H -0.7554 -0.3831 -0.8491 0.0304 Uiso 1.00 calc . . . H(5) H -0.6710 -0.4161 -1.0368 0.0271 Uiso 1.00 calc . . . H(6) H -0.3802 -0.4250 -0.9865 0.0249 Uiso 1.00 calc . . . H(7) H -0.4292 -0.4064 -0.8829 0.0249 Uiso 1.00 calc . . . H(8) H -0.5342 -0.5020 -0.9651 0.0270 Uiso 1.00 calc . . . H(9) H -0.3496 -0.5469 -0.8677 0.0281 Uiso 1.00 calc . . . H(10) H -0.2354 -0.5012 -0.9086 0.0281 Uiso 1.00 calc . . . H(11) H -0.1891 -0.5155 -0.7395 0.0267 Uiso 1.00 calc . . . H(12) H -0.4715 -0.5321 -0.6846 0.0230 Uiso 1.00 calc . . . H(13) H -0.5702 -0.4316 -0.7467 0.0225 Uiso 1.00 calc . . . H(14) H -0.8000 -0.5006 -0.6532 0.0245 Uiso 1.00 calc . . . H(15) H -0.8513 -0.4443 -0.6873 0.0245 Uiso 1.00 calc . . . H(16) H -0.8016 -0.4471 -0.5186 0.0225 Uiso 1.00 calc . . . H(17) H -0.3690 -0.4365 -0.6057 0.0192 Uiso 1.00 calc . . . H(18) H -0.2251 -0.5325 -0.5435 0.0251 Uiso 1.00 calc . . . H(19) H -0.1195 -0.4816 -0.5674 0.0251 Uiso 1.00 calc . . . H(20) H -0.1612 -0.4505 -0.4189 0.0276 Uiso 1.00 calc . . . H(21) H -0.2426 -0.5046 -0.3912 0.0276 Uiso 1.00 calc . . . H(22) H -0.4286 -0.4133 -0.4437 0.0215 Uiso 1.00 calc . . . H(23) H -0.5044 -0.5512 -0.4704 0.0302 Uiso 1.00 calc . . . H(24) H -0.6948 -0.5304 -0.4488 0.0302 Uiso 1.00 calc . . . H(25) H -0.6469 -0.5482 -0.5530 0.0302 Uiso 1.00 calc . . . H(26) H -0.6186 -0.5675 -0.8057 0.0357 Uiso 1.00 calc . . . H(27) H -0.8169 -0.5516 -0.7914 0.0357 Uiso 1.00 calc . . . H(28) H -0.7445 -0.5606 -0.8952 0.0357 Uiso 1.00 calc . . . H(29) H -0.5368 -0.4916 -0.3168 0.0251 Uiso 1.00 calc . . . H(30) H -0.7578 -0.4360 -0.2583 0.0326 Uiso 1.00 calc . . . H(31) H -0.7901 -0.4433 -0.3689 0.0326 Uiso 1.00 calc . . . H(32) H -0.7012 -0.3921 -0.3300 0.0326 Uiso 1.00 calc . . . H(33) H -0.4540 -0.4328 -0.1908 0.0277 Uiso 1.00 calc . . . H(34) H -0.2908 -0.4530 -0.2486 0.0277 Uiso 1.00 calc . . . H(35) H -0.4445 -0.3542 -0.2857 0.0362 Uiso 1.00 calc . . . H(36) H -0.2650 -0.3740 -0.3276 0.0362 Uiso 1.00 calc . . . H(37) H -0.5112 -0.3440 -1.0442 0.0430 Uiso 1.00 calc . . . H(38) H -0.1606 -0.4306 -0.7045 0.0430 Uiso 1.00 calc . . . H(39) H -0.7444 -0.3775 -0.5373 0.0430 Uiso 1.00 calc . . . H(40) H 0.0019 -0.3262 -0.1445 0.0430 Uiso 1.00 calc . . . H(41) H 0.3583 -0.2144 -1.3299 0.0238 Uiso 1.00 calc . . . H(42) H 0.2967 -0.1986 -1.4338 0.0238 Uiso 1.00 calc . . . H(43) H 0.3466 -0.2884 -1.4308 0.0292 Uiso 1.00 calc . . . H(44) H 0.2136 -0.2949 -1.3460 0.0292 Uiso 1.00 calc . . . H(45) H 0.1156 -0.2620 -1.5336 0.0289 Uiso 1.00 calc . . . H(46) H -0.1756 -0.2594 -1.4835 0.0249 Uiso 1.00 calc . . . H(47) H -0.1167 -0.2764 -1.3798 0.0249 Uiso 1.00 calc . . . H(48) H -0.0362 -0.1805 -1.4644 0.0228 Uiso 1.00 calc . . . H(49) H -0.2295 -0.1383 -1.3681 0.0233 Uiso 1.00 calc . . . H(50) H -0.3348 -0.1864 -1.4085 0.0233 Uiso 1.00 calc . . . H(51) H -0.3770 -0.1715 -1.2394 0.0208 Uiso 1.00 calc . . . H(52) H -0.0980 -0.1504 -1.1862 0.0183 Uiso 1.00 calc . . . H(53) H 0.0152 -0.2503 -1.2441 0.0195 Uiso 1.00 calc . . . H(54) H 0.2431 -0.1781 -1.1525 0.0274 Uiso 1.00 calc . . . H(55) H 0.2975 -0.2344 -1.1847 0.0274 Uiso 1.00 calc . . . H(56) H 0.2446 -0.2307 -1.0146 0.0223 Uiso 1.00 calc . . . H(57) H -0.1852 -0.2473 -1.1040 0.0202 Uiso 1.00 calc . . . H(58) H -0.3424 -0.1535 -1.0469 0.0258 Uiso 1.00 calc . . . H(59) H -0.4383 -0.2064 -1.0690 0.0258 Uiso 1.00 calc . . . H(60) H -0.3114 -0.1789 -0.8932 0.0295 Uiso 1.00 calc . . . H(61) H -0.3888 -0.2340 -0.9180 0.0295 Uiso 1.00 calc . . . H(62) H -0.1183 -0.2692 -0.9430 0.0216 Uiso 1.00 calc . . . H(63) H -0.0613 -0.1306 -0.9696 0.0280 Uiso 1.00 calc . . . H(64) H 0.1328 -0.1489 -0.9472 0.0280 Uiso 1.00 calc . . . H(65) H 0.0785 -0.1321 -1.0518 0.0280 Uiso 1.00 calc . . . H(66) H 0.0417 -0.1128 -1.3002 0.0323 Uiso 1.00 calc . . . H(67) H 0.2428 -0.1259 -1.2852 0.0323 Uiso 1.00 calc . . . H(68) H 0.1663 -0.1170 -1.3891 0.0323 Uiso 1.00 calc . . . H(69) H -0.0202 -0.1896 -0.8136 0.0257 Uiso 1.00 calc . . . H(70) H 0.1619 -0.2849 -0.8275 0.0310 Uiso 1.00 calc . . . H(71) H 0.2106 -0.2403 -0.7550 0.0310 Uiso 1.00 calc . . . H(72) H 0.2366 -0.2319 -0.8655 0.0310 Uiso 1.00 calc . . . H(73) H -0.0958 -0.2482 -0.6875 0.0279 Uiso 1.00 calc . . . H(74) H -0.2612 -0.2317 -0.7494 0.0279 Uiso 1.00 calc . . . H(75) H -0.2618 -0.3116 -0.8281 0.0396 Uiso 1.00 calc . . . H(76) H -0.0850 -0.3278 -0.7761 0.0396 Uiso 1.00 calc . . . H(77) H -0.0166 -0.3392 -1.5416 0.0430 Uiso 1.00 calc . . . H(78) H -0.4170 -0.2535 -1.2189 0.0430 Uiso 1.00 calc . . . H(79) H 0.2120 -0.3135 -1.0364 0.0430 Uiso 1.00 calc . . . H(80) H -0.5152 -0.3549 -0.6453 0.0430 Uiso 1.00 calc . . . H(81) H -0.8147 -0.1468 -0.5877 0.0302 Uiso 1.00 calc . . . H(82) H -1.0991 -0.1090 -0.5980 0.0313 Uiso 1.00 calc . . . H(83) H -1.1659 -0.0509 -0.7280 0.0333 Uiso 1.00 calc . . . H(84) H -0.8779 -0.0149 -0.9186 0.0496 Uiso 1.00 calc . . . H(85) H -1.0081 0.0145 -0.8505 0.0496 Uiso 1.00 calc . . . H(86) H -1.0749 -0.0334 -0.9108 0.0496 Uiso 1.00 calc . . . H(87) H -0.5078 -0.0859 -0.8463 0.0394 Uiso 1.00 calc . . . H(88) H -0.5906 -0.0306 -0.8635 0.0394 Uiso 1.00 calc . . . H(89) H -0.6580 -0.0785 -0.9237 0.0394 Uiso 1.00 calc . . . H(90) H -0.4577 -0.1282 -0.7512 0.0446 Uiso 1.00 calc . . . H(91) H -0.4751 -0.1294 -0.6391 0.0446 Uiso 1.00 calc . . . H(92) H -0.5422 -0.1767 -0.7007 0.0446 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) 0.025(1) 0.031(1) 0.032(2) 0.007(1) 0.003(1) 0.010(1) O(2) 0.021(1) 0.027(1) 0.027(2) 0.001(1) 0.003(1) 0.003(1) O(3) 0.023(1) 0.021(1) 0.024(1) 0.003(1) 0.005(1) 0.005(1) O(4) 0.036(2) 0.028(2) 0.030(2) -0.011(1) 0.008(1) -0.004(1) O(5) 0.026(1) 0.027(1) 0.030(1) -0.003(1) -0.004(1) -0.007(1) O(6) 0.026(1) 0.028(1) 0.032(2) 0.006(1) -0.004(1) -0.013(1) O(7) 0.021(1) 0.018(1) 0.023(1) -0.001(1) -0.0023(10) 0.000(1) O(8) 0.023(1) 0.016(1) 0.024(1) 0.001(1) -0.003(1) -0.001(1) O(9) 0.035(2) 0.032(2) 0.031(2) -0.012(1) -0.005(1) 0.007(1) O(10) 0.030(1) 0.028(2) 0.028(2) -0.002(1) -0.001(1) 0.006(1) C(1) 0.022(2) 0.028(2) 0.024(2) -0.003(1) 0.000(1) -0.001(2) C(2) 0.021(2) 0.028(2) 0.029(2) 0.003(2) -0.001(1) -0.002(2) C(3) 0.020(2) 0.028(2) 0.021(2) 0.004(1) -0.005(1) 0.001(1) C(4) 0.019(2) 0.024(2) 0.023(2) 0.002(1) 0.004(1) 0.002(1) C(5) 0.020(2) 0.024(2) 0.025(2) 0.004(1) 0.001(1) -0.001(1) C(6) 0.024(2) 0.026(2) 0.023(2) 0.006(2) 0.003(1) -0.003(2) C(7) 0.022(2) 0.022(2) 0.025(2) 0.005(1) 0.001(1) 0.000(1) C(8) 0.025(2) 0.021(2) 0.013(2) -0.002(1) 0.000(1) -0.001(1) C(9) 0.028(2) 0.014(2) 0.019(2) -0.001(1) 0.003(1) 0.001(1) C(10) 0.021(2) 0.018(2) 0.020(2) -0.002(1) 0.003(1) 0.001(1) C(11) 0.017(2) 0.023(2) 0.023(2) -0.003(1) -0.004(1) -0.003(1) C(12) 0.022(2) 0.023(2) 0.015(2) -0.001(1) 0.007(1) -0.001(1) C(13) 0.024(2) 0.016(2) 0.020(2) -0.003(1) 0.002(1) -0.002(1) C(14) 0.021(2) 0.013(2) 0.018(2) 0.002(1) 0.002(1) -0.001(1) C(15) 0.020(2) 0.022(2) 0.025(2) 0.004(1) 0.001(1) 0.002(1) C(16) 0.024(2) 0.023(2) 0.028(2) 0.004(1) -0.001(2) -0.002(2) C(17) 0.020(2) 0.019(2) 0.019(2) -0.003(1) 0.001(1) 0.002(1) C(18) 0.034(2) 0.019(2) 0.018(2) -0.006(2) 0.003(2) 0.002(1) C(19) 0.032(2) 0.019(2) 0.033(2) -0.007(2) -0.003(2) -0.004(2) C(20) 0.029(2) 0.018(2) 0.020(2) -0.002(1) -0.001(1) -0.001(1) C(21) 0.023(2) 0.037(2) 0.022(2) -0.005(2) 0.005(2) -0.004(2) C(22) 0.029(2) 0.021(2) 0.022(2) -0.003(2) -0.001(1) 0.000(1) C(23) 0.035(2) 0.022(2) 0.029(2) -0.004(2) -0.006(2) -0.002(2) C(24) 0.031(1) 0.011(2) 0.030(2) -0.002(1) 0.002(1) 0.006(1) C(25) 0.021(2) 0.024(2) 0.018(2) -0.002(1) 0.005(1) 0.006(1) C(26) 0.017(2) 0.026(2) 0.029(2) 0.003(1) 0.001(1) 0.000(2) C(27) 0.022(2) 0.025(2) 0.024(2) 0.003(1) -0.001(1) -0.005(2) C(28) 0.020(2) 0.022(2) 0.023(2) 0.004(1) -0.003(1) -0.002(1) C(29) 0.024(2) 0.018(2) 0.017(2) 0.001(1) -0.003(1) 0.003(1) C(30) 0.026(2) 0.017(2) 0.018(2) 0.003(1) 0.000(1) 0.001(1) C(31) 0.020(2) 0.015(1) 0.022(2) 0.000(1) -0.002(1) 0.004(1) C(32) 0.016(2) 0.017(2) 0.021(2) 0.000(1) 0.002(1) 0.002(1) C(33) 0.016(2) 0.025(2) 0.012(2) 0.001(1) 0.003(1) 0.004(1) C(34) 0.019(2) 0.021(2) 0.015(2) -0.002(1) 0.001(1) 0.004(1) C(35) 0.019(2) 0.026(2) 0.023(2) -0.003(1) -0.004(1) 0.004(2) C(36) 0.020(2) 0.017(1) 0.020(2) -0.002(1) -0.001(1) -0.004(1) C(37) 0.016(2) 0.022(2) 0.021(2) -0.002(1) -0.004(1) 0.000(1) C(38) 0.020(2) 0.019(2) 0.015(2) 0.000(1) -0.004(1) -0.001(1) C(39) 0.018(2) 0.027(2) 0.022(2) 0.006(1) 0.005(1) -0.002(1) C(40) 0.021(2) 0.031(2) 0.027(2) 0.004(2) 0.001(2) 0.001(2) C(41) 0.020(2) 0.020(2) 0.018(2) -0.001(1) 0.002(1) -0.003(1) C(42) 0.023(2) 0.020(2) 0.025(2) -0.004(1) 0.003(2) -0.003(1) C(43) 0.027(2) 0.023(2) 0.030(2) -0.006(2) 0.001(2) 0.000(2) C(44) 0.022(2) 0.021(2) 0.021(2) -0.002(1) -0.002(1) -0.002(1) C(45) 0.024(2) 0.027(2) 0.024(2) -0.001(2) -0.002(1) 0.001(2) C(46) 0.032(2) 0.024(2) 0.015(2) -0.003(2) 0.002(1) -0.004(1) C(47) 0.043(2) 0.026(2) 0.026(2) -0.008(2) 0.011(2) -0.001(2) C(48) 0.028(2) 0.018(2) 0.028(2) -0.007(2) 0.001(1) -0.003(1) C(49) 0.038(2) 0.022(2) 0.022(2) 0.000(2) -0.011(1) -0.004(1) C(50) 0.033(2) 0.025(2) 0.019(2) -0.007(1) 0.002(1) -0.006(1) C(51) 0.027(2) 0.023(2) 0.025(2) -0.005(1) -0.003(1) -0.003(1) C(52) 0.034(2) 0.027(2) 0.021(2) 0.000(2) -0.001(1) 0.007(2) C(53) 0.026(2) 0.031(2) 0.029(2) -0.005(2) 0.006(2) -0.005(1) C(54) 0.030(2) 0.023(2) 0.036(2) -0.001(2) -0.004(1) -0.007(2) C(55) 0.067(3) 0.027(2) 0.029(2) -0.001(2) -0.010(2) 0.004(2) C(56) 0.033(2) 0.036(2) 0.033(2) -0.010(2) 0.006(2) 0.000(2) C(57) 0.027(2) 0.040(3) 0.038(3) 0.004(2) -0.003(2) 0.000(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.436(7) . . yes O(2) C(7) 1.448(7) . . yes O(3) C(12) 1.440(6) . . yes O(4) C(24) 1.190(7) . . yes O(5) C(24) 1.346(6) . . yes O(6) C(27) 1.431(6) . . yes O(7) C(31) 1.444(6) . . yes O(8) C(36) 1.457(6) . . yes O(9) C(48) 1.229(7) . . yes O(10) C(48) 1.315(7) . . yes C(1) C(2) 1.536(8) . . yes C(1) C(10) 1.530(7) . . yes C(2) C(3) 1.513(8) . . yes C(3) C(4) 1.520(7) . . yes C(4) C(5) 1.556(7) . . yes C(5) C(6) 1.530(7) . . yes C(5) C(10) 1.546(7) . . yes C(6) C(7) 1.528(7) . . yes C(7) C(8) 1.542(7) . . yes C(8) C(9) 1.548(7) . . yes C(8) C(14) 1.519(6) . . yes C(9) C(10) 1.548(7) . . yes C(9) C(11) 1.543(7) . . yes C(10) C(19) 1.549(7) . . yes C(11) C(12) 1.539(7) . . yes C(12) C(13) 1.551(7) . . yes C(13) C(14) 1.540(7) . . yes C(13) C(17) 1.563(7) . . yes C(13) C(18) 1.536(7) . . yes C(14) C(15) 1.535(6) . . yes C(15) C(16) 1.551(7) . . yes C(16) C(17) 1.557(7) . . yes C(17) C(20) 1.532(7) . . yes C(20) C(21) 1.548(7) . . yes C(20) C(22) 1.550(7) . . yes C(22) C(23) 1.541(7) . . yes C(23) C(24) 1.518(7) . . yes C(25) C(26) 1.533(7) . . yes C(25) C(34) 1.539(7) . . yes C(26) C(27) 1.523(7) . . yes C(27) C(28) 1.531(7) . . yes C(28) C(29) 1.528(7) . . yes C(29) C(30) 1.544(7) . . yes C(29) C(34) 1.560(6) . . yes C(30) C(31) 1.539(7) . . yes C(31) C(32) 1.528(6) . . yes C(32) C(33) 1.546(6) . . yes C(32) C(38) 1.549(6) . . yes C(33) C(34) 1.577(6) . . yes C(33) C(35) 1.535(6) . . yes C(34) C(43) 1.541(7) . . yes C(35) C(36) 1.547(7) . . yes C(36) C(37) 1.533(7) . . yes C(37) C(38) 1.536(6) . . yes C(37) C(41) 1.569(7) . . yes C(37) C(42) 1.536(7) . . yes C(38) C(39) 1.514(7) . . yes C(39) C(40) 1.542(7) . . yes C(40) C(41) 1.566(7) . . yes C(41) C(44) 1.549(6) . . yes C(44) C(45) 1.532(7) . . yes C(44) C(46) 1.556(7) . . yes C(46) C(47) 1.537(8) . . yes C(47) C(48) 1.508(8) . . yes C(49) C(50) 1.386(8) . . yes C(49) C(54) 1.383(9) . . yes C(49) C(55) 1.533(7) . . yes C(50) C(51) 1.441(7) . . yes C(50) C(56) 1.499(8) . . yes C(51) C(52) 1.382(8) . . yes C(51) C(57) 1.509(8) . . yes C(52) C(53) 1.382(8) . . yes C(53) C(54) 1.397(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 C(2) C(1) C(10) 114.3(4) . 1_555 1_555 yes C(1) C(2) C(3) 109.8(4) . 1_555 1_555 yes O(1) C(3) C(2) 108.4(4) . 1_555 1_555 yes O(1) C(3) C(4) 111.7(4) . 1_555 1_555 yes C(2) C(3) C(4) 110.5(4) . 1_555 1_555 yes C(3) C(4) C(5) 113.2(4) . 1_555 1_555 yes C(4) C(5) C(6) 111.8(4) . 1_555 1_555 yes C(4) C(5) C(10) 111.9(4) . 1_555 1_555 yes C(6) C(5) C(10) 112.9(4) . 1_555 1_555 yes C(5) C(6) C(7) 114.3(4) . 1_555 1_555 yes O(2) C(7) C(6) 107.7(4) . 1_555 1_555 yes O(2) C(7) C(8) 110.9(4) . 1_555 1_555 yes C(6) C(7) C(8) 112.6(4) . 1_555 1_555 yes C(7) C(8) C(9) 110.2(4) . 1_555 1_555 yes C(7) C(8) C(14) 111.2(4) . 1_555 1_555 yes C(9) C(8) C(14) 109.9(4) . 1_555 1_555 yes C(8) C(9) C(10) 112.8(4) . 1_555 1_555 yes C(8) C(9) C(11) 110.2(4) . 1_555 1_555 yes C(10) C(9) C(11) 113.9(4) . 1_555 1_555 yes C(1) C(10) C(5) 109.3(4) . 1_555 1_555 yes C(1) C(10) C(9) 112.9(4) . 1_555 1_555 yes C(1) C(10) C(19) 106.4(4) . 1_555 1_555 yes C(5) C(10) C(9) 108.3(4) . 1_555 1_555 yes C(5) C(10) C(19) 108.4(4) . 1_555 1_555 yes C(9) C(10) C(19) 111.5(4) . 1_555 1_555 yes C(9) C(11) C(12) 114.4(4) . 1_555 1_555 yes O(3) C(12) C(11) 109.7(4) . 1_555 1_555 yes O(3) C(12) C(13) 110.3(4) . 1_555 1_555 yes C(11) C(12) C(13) 110.5(4) . 1_555 1_555 yes C(12) C(13) C(14) 107.0(4) . 1_555 1_555 yes C(12) C(13) C(17) 116.7(4) . 1_555 1_555 yes C(12) C(13) C(18) 109.3(4) . 1_555 1_555 yes C(14) C(13) C(17) 99.7(4) . 1_555 1_555 yes C(14) C(13) C(18) 113.4(4) . 1_555 1_555 yes C(17) C(13) C(18) 110.6(4) . 1_555 1_555 yes C(8) C(14) C(13) 115.1(4) . 1_555 1_555 yes C(8) C(14) C(15) 118.4(4) . 1_555 1_555 yes C(13) C(14) C(15) 104.0(4) . 1_555 1_555 yes C(14) C(15) C(16) 103.7(4) . 1_555 1_555 yes C(15) C(16) C(17) 106.8(4) . 1_555 1_555 yes C(13) C(17) C(16) 103.2(4) . 1_555 1_555 yes C(13) C(17) C(20) 118.9(4) . 1_555 1_555 yes C(16) C(17) C(20) 112.1(4) . 1_555 1_555 yes C(17) C(20) C(21) 113.9(4) . 1_555 1_555 yes C(17) C(20) C(22) 110.2(4) . 1_555 1_555 yes C(21) C(20) C(22) 109.8(4) . 1_555 1_555 yes C(20) C(22) C(23) 113.5(4) . 1_555 1_555 yes C(22) C(23) C(24) 110.9(4) . 1_555 1_555 yes O(4) C(24) O(5) 122.2(5) . 1_555 1_555 yes O(4) C(24) C(23) 124.5(5) . 1_555 1_555 yes O(5) C(24) C(23) 113.3(5) . 1_555 1_555 yes C(26) C(25) C(34) 114.7(4) . 1_555 1_555 yes C(25) C(26) C(27) 109.9(4) . 1_555 1_555 yes O(6) C(27) C(26) 107.9(4) . 1_555 1_555 yes O(6) C(27) C(28) 112.0(4) . 1_555 1_555 yes C(26) C(27) C(28) 110.4(4) . 1_555 1_555 yes C(27) C(28) C(29) 112.9(4) . 1_555 1_555 yes C(28) C(29) C(30) 111.6(4) . 1_555 1_555 yes C(28) C(29) C(34) 112.9(4) . 1_555 1_555 yes C(30) C(29) C(34) 112.1(4) . 1_555 1_555 yes C(29) C(30) C(31) 114.2(4) . 1_555 1_555 yes O(7) C(31) C(30) 106.5(4) . 1_555 1_555 yes O(7) C(31) C(32) 112.1(4) . 1_555 1_555 yes C(30) C(31) C(32) 112.5(4) . 1_555 1_555 yes C(31) C(32) C(33) 111.8(4) . 1_555 1_555 yes C(31) C(32) C(38) 110.5(4) . 1_555 1_555 yes C(33) C(32) C(38) 109.4(4) . 1_555 1_555 yes C(32) C(33) C(34) 110.8(4) . 1_555 1_555 yes C(32) C(33) C(35) 112.0(4) . 1_555 1_555 yes C(34) C(33) C(35) 113.0(4) . 1_555 1_555 yes C(25) C(34) C(29) 108.8(4) . 1_555 1_555 yes C(25) C(34) C(33) 111.6(4) . 1_555 1_555 yes C(25) C(34) C(43) 106.5(4) . 1_555 1_555 yes C(29) C(34) C(33) 107.9(4) . 1_555 1_555 yes C(29) C(34) C(43) 110.1(4) . 1_555 1_555 yes C(33) C(34) C(43) 111.9(4) . 1_555 1_555 yes C(33) C(35) C(36) 112.8(4) . 1_555 1_555 yes O(8) C(36) C(35) 109.9(4) . 1_555 1_555 yes O(8) C(36) C(37) 110.2(4) . 1_555 1_555 yes C(35) C(36) C(37) 111.7(4) . 1_555 1_555 yes C(36) C(37) C(38) 107.8(4) . 1_555 1_555 yes C(36) C(37) C(41) 116.8(4) . 1_555 1_555 yes C(36) C(37) C(42) 109.4(4) . 1_555 1_555 yes C(38) C(37) C(41) 98.9(4) . 1_555 1_555 yes C(38) C(37) C(42) 113.5(4) . 1_555 1_555 yes C(41) C(37) C(42) 110.1(4) . 1_555 1_555 yes C(32) C(38) C(37) 114.0(4) . 1_555 1_555 yes C(32) C(38) C(39) 118.1(4) . 1_555 1_555 yes C(37) C(38) C(39) 105.3(4) . 1_555 1_555 yes C(38) C(39) C(40) 103.3(4) . 1_555 1_555 yes C(39) C(40) C(41) 107.1(4) . 1_555 1_555 yes C(37) C(41) C(40) 102.3(4) . 1_555 1_555 yes C(37) C(41) C(44) 119.6(4) . 1_555 1_555 yes C(40) C(41) C(44) 111.7(4) . 1_555 1_555 yes C(41) C(44) C(45) 113.4(4) . 1_555 1_555 yes C(41) C(44) C(46) 110.4(4) . 1_555 1_555 yes C(45) C(44) C(46) 111.4(4) . 1_555 1_555 yes C(44) C(46) C(47) 112.8(4) . 1_555 1_555 yes C(46) C(47) C(48) 110.3(4) . 1_555 1_555 yes O(9) C(48) O(10) 122.1(5) . 1_555 1_555 yes O(9) C(48) C(47) 122.8(5) . 1_555 1_555 yes O(10) C(48) C(47) 115.1(5) . 1_555 1_555 yes C(50) C(49) C(54) 120.3(5) . 1_555 1_555 yes C(50) C(49) C(55) 121.2(5) . 1_555 1_555 yes C(54) C(49) C(55) 118.5(5) . 1_555 1_555 yes C(49) C(50) C(51) 119.0(5) . 1_555 1_555 yes C(49) C(50) C(56) 121.7(5) . 1_555 1_555 yes C(51) C(50) C(56) 119.3(5) . 1_555 1_555 yes C(50) C(51) C(52) 118.8(5) . 1_555 1_555 yes C(50) C(51) C(57) 120.4(5) . 1_555 1_555 yes C(52) C(51) C(57) 120.8(5) . 1_555 1_555 yes C(51) C(52) C(53) 121.8(5) . 1_555 1_555 yes C(52) C(53) C(54) 118.8(5) . 1_555 1_555 yes C(49) C(54) C(53) 121.2(5) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) C(2) C(1) -179.1(4) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 176.3(4) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -73.6(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 69.8(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -52.4(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 65.9(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -65.9(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 44.6(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 170.9(4) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -75.6(7) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 103.5(5) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(26) C(25) -179.1(4) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(28) C(29) 176.4(4) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(30) C(29) -75.1(5) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(33) 68.5(5) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(38) -53.6(5) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(35) C(33) 67.5(5) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(38) -66.1(5) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(41) 44.1(5) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(42) 170.0(4) 1_555 1_555 1_555 1_555 yes O(9) C(48) C(47) C(46) -83.6(7) 1_555 1_555 1_555 1_555 yes O(10) C(48) C(47) C(46) 97.3(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -56.5(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 50.3(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 177.4(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -179.4(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 54.1(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -54.3(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 66.3(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -171.2(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 55.7(6) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 58.1(6) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 179.3(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.0(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 76.1(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -73.1(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 165.8(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 48.9(6) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -58.2(5) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 175.2(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 54.0(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -67.0(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -50.9(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -173.1(4) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -51.1(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 57.3(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -174.2(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -179.6(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -55.7(6) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 60.9(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 52.8(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -59.5(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 178.6(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 61.1(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -164.0(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 58.0(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -178.1(4) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -56.0(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -179.7(4) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) -179.3(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -51.3(5) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -65.7(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 55.6(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 166.1(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -67.6(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 169.3(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -155.9(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 79.3(6) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -34.8(5) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 20.8(5) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -60.8(6) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 175.3(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -41.2(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -166.0(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 8.1(5) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 47.5(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -70.1(5) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 150.0(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.5(5) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 178.8(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 54.9(5) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) 54.8(6) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -46.3(6) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 170.6(4) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) -71.5(6) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -56.3(6) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(28) 49.8(5) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(30) 177.0(4) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(32) -179.2(4) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(35) 54.1(5) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(29) -52.8(5) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(33) 66.1(5) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(43) -171.5(4) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 56.0(6) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(34) 57.2(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 179.1(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(34) -53.4(5) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 76.6(5) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(33) -71.4(5) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(43) 166.2(4) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 48.1(5) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) -59.7(5) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(35) 173.5(4) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) 55.8(5) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) -66.6(5) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -51.5(5) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(38) -173.6(4) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) -51.3(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 58.6(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(35) -174.1(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(37) -179.8(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(39) -55.3(5) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) 61.5(5) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(35) C(36) 52.1(5) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(36) -59.0(5) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(41) 179.0(4) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(42) 62.4(5) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(39) C(40) -163.1(4) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(37) 56.7(5) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(39) -178.8(4) 1_555 1_555 1_555 1_555 yes C(33) C(35) C(36) C(37) -55.2(5) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(38) -178.7(4) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(35) C(36) 178.2(4) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(32) C(38) -51.4(5) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(34) C(43) -65.2(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 56.4(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(41) 166.6(4) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(42) -67.5(5) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) 170.0(4) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(40) -156.7(4) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(44) 79.3(5) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) -34.4(5) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(40) C(39) 22.2(5) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(45) -59.2(6) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(46) 175.0(4) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(40) -41.5(4) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(44) -165.5(4) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) 6.8(5) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(41) 47.9(5) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(42) -68.6(5) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(44) 151.3(4) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(37) C(42) 77.7(4) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(45) -178.6(4) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(46) 55.7(5) 1_555 1_555 1_555 1_555 yes C(41) C(44) C(46) C(47) 55.8(6) 1_555 1_555 1_555 1_555 yes C(42) C(37) C(41) C(44) -46.3(5) 1_555 1_555 1_555 1_555 yes C(44) C(46) C(47) C(48) 174.0(4) 1_555 1_555 1_555 1_555 yes C(45) C(44) C(46) C(47) -71.1(6) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) 0.1(7) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(57) -179.9(5) 1_555 1_555 1_555 1_555 yes C(49) C(54) C(53) C(52) -0.6(8) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(54) C(53) 0.4(8) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) -0.3(8) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(54) -0.2(7) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(55) -178.4(5) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) 0.5(8) 1_555 1_555 1_555 1_555 yes C(52) C(51) C(50) C(56) -179.3(5) 1_555 1_555 1_555 1_555 yes C(53) C(52) C(51) C(57) 179.8(5) 1_555 1_555 1_555 1_555 yes C(53) C(54) C(49) C(55) 178.7(5) 1_555 1_555 1_555 1_555 yes C(54) C(49) C(50) C(56) 179.3(5) 1_555 1_555 1_555 1_555 yes C(55) C(49) C(50) C(56) 1.0(8) 1_555 1_555 1_555 1_555 yes C(56) C(50) C(51) C(57) 0.6(7) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(8) 2.667(5) . 1_455 ? O(1) O(4) 2.733(5) . 1_554 ? O(1) C(36) 3.420(6) . 1_455 ? O(2) C(48) 3.013(7) . . ? O(2) O(9) 3.128(6) . . ? O(2) C(47) 3.316(7) . . ? O(2) C(1) 3.349(6) . 1_655 ? O(2) O(10) 3.454(5) . . ? O(3) O(10) 2.663(5) . . ? O(3) O(6) 2.683(5) . 1_456 ? O(3) O(9) 3.412(5) . . ? O(3) C(48) 3.442(6) . . ? O(4) O(7) 3.146(5) . 1_556 ? O(4) C(38) 3.376(6) . 1_556 ? O(4) O(8) 3.395(5) . 1_556 ? O(4) C(3) 3.474(7) . 1_556 ? O(4) C(4) 3.536(7) . 1_556 ? O(5) O(8) 2.646(5) . 1_556 ? O(5) O(7) 3.466(5) . 1_556 ? O(5) C(33) 3.533(6) . 1_556 ? O(6) O(9) 2.718(5) . 1_554 ? O(6) C(12) 3.370(6) . 1_654 ? O(7) C(24) 2.985(6) . 1_554 ? O(7) C(23) 3.241(6) . 1_554 ? O(7) C(25) 3.339(6) . 1_455 ? O(8) C(24) 3.430(6) . 1_554 ? O(8) C(3) 3.520(6) . 1_655 ? O(9) C(14) 3.378(6) . . ? O(9) C(27) 3.470(6) . 1_556 ? O(9) C(28) 3.552(6) . 1_556 ? O(10) C(9) 3.561(6) . . ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_aburaya89 _database_code_depnum_ccdc_archive 'CCDC 297672' _audit_creation_date 'Wed Apr 26 04:34:11 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C56 H89 Cl O10 ' _chemical_formula_moiety ? _chemical_formula_weight 957.77 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 7.4650(1) _cell_length_b 25.3714(5) _cell_length_c 13.7625(3) _cell_angle_alpha 90 _cell_angle_beta 90.605(1) _cell_angle_gamma 90 _cell_volume 2606.44(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10358 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 68.2 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5419 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15750 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_theta_max 68.21 _diffrn_measured_fraction_theta_max 0.9591 _diffrn_reflns_theta_full 68.21 _diffrn_measured_fraction_theta_full 0.9591 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # 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 4667 _reflns_number_gt 3749 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.2495 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4667 _refine_ls_number_parameters 604 _refine_ls_goodness_of_fit_ref 2.539 _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 0.0003 _refine_diff_density_max 0.89 _refine_diff_density_min -0.74 _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 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.364 0.702 ;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 1.5036(4) 0.0818(3) 2.2007(2) 0.091(1) Uani 1.00 d . . . O(1) O 0.9330(6) -0.1149(3) 1.9991(3) 0.029(1) Uani 1.00 d . . . O(2) O 1.3456(5) -0.0260(3) 1.7687(3) 0.018(1) Uani 1.00 d . . . O(3) O 0.8906(6) -0.0706(3) 1.5665(3) 0.024(1) Uani 1.00 d . . . O(4) O 1.2273(6) -0.1290(3) 1.1133(3) 0.029(1) Uani 1.00 d . . . O(5) O 1.4744(6) -0.1122(3) 1.2001(3) 0.029(1) Uani 1.00 d . . . O(6) O 1.3959(6) 0.3764(3) 1.5001(3) 0.030(1) Uani 1.00 d . . . O(7) O 1.7870(6) 0.2817(3) 1.7325(3) 0.022(1) Uani 1.00 d . . . O(8) O 1.3448(5) 0.3325(3) 1.9312(3) 0.017(1) Uani 1.00 d . . . O(9) O 1.6905(6) 0.3846(3) 2.3863(3) 0.034(1) Uani 1.00 d . . . O(10) O 1.9390(6) 0.3724(3) 2.2997(3) 0.029(1) Uani 1.00 d . . . C(1) C 0.7355(8) 0.0039(4) 1.8773(4) 0.022(2) Uani 1.00 d . . . C(2) C 0.7574(8) -0.0549(4) 1.9034(4) 0.019(2) Uani 1.00 d . . . C(3) C 0.9090(8) -0.0594(4) 1.9754(4) 0.020(1) Uani 1.00 d . . . C(4) C 1.0846(8) -0.0358(4) 1.9359(4) 0.019(1) Uani 1.00 d . . . C(5) C 1.0613(8) 0.0216(3) 1.9062(4) 0.017(1) Uani 1.00 d . . . C(6) C 1.2349(8) 0.0462(4) 1.8642(4) 0.022(2) Uani 1.00 d . . . C(7) C 1.2804(8) 0.0283(4) 1.7632(4) 0.018(1) Uani 1.00 d . . . C(8) C 1.1224(8) 0.0333(3) 1.6931(4) 0.017(1) Uani 1.00 d . . . C(9) C 0.9536(8) 0.0068(3) 1.7335(4) 0.014(1) Uani 1.00 d . . . C(10) C 0.9026(8) 0.0304(4) 1.8335(4) 0.018(1) Uani 1.00 d . . . C(11) C 0.7996(8) 0.0072(3) 1.6574(4) 0.018(1) Uani 1.00 d . . . C(12) C 0.8528(8) -0.0144(4) 1.5577(4) 0.016(1) Uani 1.00 d . . . C(13) C 1.0151(8) 0.0147(4) 1.5174(4) 0.017(1) Uani 1.00 d . . . C(14) C 1.1670(8) 0.0107(3) 1.5932(4) 0.017(1) Uani 1.00 d . . . C(15) C 1.3341(9) 0.0306(4) 1.5396(4) 0.024(2) Uani 1.00 d . . . C(16) C 1.3015(9) 0.0130(4) 1.4336(5) 0.030(2) Uani 1.00 d . . . C(17) C 1.1099(8) -0.0103(4) 1.4277(4) 0.018(1) Uani 1.00 d . . . C(18) C 0.9584(8) 0.0714(4) 1.4935(5) 0.023(2) Uani 1.00 d . . . C(19) C 0.8557(9) 0.0892(4) 1.8274(4) 0.026(2) Uani 1.00 d . . . C(20) C 1.0287(8) -0.0052(4) 1.3270(4) 0.022(1) Uani 1.00 d . . . C(21) C 0.8359(9) -0.0261(4) 1.3151(4) 0.028(2) Uani 1.00 d . . . C(22) C 1.1513(9) -0.0296(4) 1.2495(4) 0.021(2) Uani 1.00 d . . . C(23) C 1.1974(9) -0.0878(4) 1.2687(5) 0.027(2) Uani 1.00 d . . . C(24) C 1.2973(9) -0.1113(4) 1.1861(5) 0.024(1) Uani 1.00 d . . . C(25) C 1.1754(8) 0.2608(4) 1.6201(4) 0.020(2) Uani 1.00 d . . . C(26) C 1.2124(8) 0.3191(4) 1.5928(5) 0.025(2) Uani 1.00 d . . . C(27) C 1.3622(9) 0.3218(4) 1.5231(5) 0.026(2) Uani 1.00 d . . . C(28) C 1.5325(8) 0.2955(4) 1.5630(4) 0.022(2) Uani 1.00 d . . . C(29) C 1.4951(8) 0.2377(4) 1.5940(4) 0.017(1) Uani 1.00 d . . . C(30) C 1.6699(8) 0.2120(3) 1.6343(4) 0.018(1) Uani 1.00 d . . . C(31) C 1.7168(8) 0.2283(4) 1.7379(4) 0.019(1) Uani 1.00 d . . . C(32) C 1.5621(9) 0.2255(4) 1.8066(4) 0.020(1) Uani 1.00 d . . . C(33) C 1.3933(8) 0.2529(4) 1.7646(4) 0.019(1) Uani 1.00 d . . . C(34) C 1.3385(8) 0.2318(4) 1.6638(4) 0.018(1) Uani 1.00 d . . . C(35) C 1.2385(8) 0.2550(4) 1.8398(5) 0.023(2) Uani 1.00 d . . . C(36) C 1.2953(8) 0.2766(4) 1.9365(4) 0.020(1) Uani 1.00 d . . . C(37) C 1.4598(8) 0.2466(4) 1.9794(4) 0.019(1) Uani 1.00 d . . . C(38) C 1.6064(8) 0.2476(3) 1.9047(4) 0.017(1) Uani 1.00 d . . . C(39) C 1.7695(8) 0.2242(4) 1.9597(4) 0.024(2) Uani 1.00 d . . . C(40) C 1.7495(9) 0.2457(4) 2.0654(5) 0.024(2) Uani 1.00 d . . . C(41) C 1.5587(8) 0.2699(3) 2.0691(4) 0.018(1) Uani 1.00 d . . . C(42) C 1.3966(9) 0.1894(4) 2.0058(4) 0.024(2) Uani 1.00 d . . . C(43) C 1.2814(9) 0.1736(4) 1.6692(5) 0.028(2) Uani 1.00 d . . . C(44) C 1.4750(8) 0.2653(3) 2.1708(4) 0.019(1) Uani 1.00 d . . . C(45) C 1.2876(9) 0.2905(4) 2.1797(5) 0.029(2) Uani 1.00 d . . . C(46) C 1.6035(9) 0.2898(4) 2.2514(5) 0.028(2) Uani 1.00 d . . . C(47) C 1.6637(9) 0.3467(4) 2.2282(4) 0.026(2) Uani 1.00 d . . . C(48) C 1.7623(10) 0.3693(4) 2.3136(5) 0.027(1) Uani 1.00 d . . . C(49) C 1.9242(9) 0.1645(4) 2.2916(4) 0.028(2) Uani 1.00 d . . . C(50) C 1.7539(9) 0.1422(4) 2.2876(5) 0.027(2) Uani 1.00 d . . . C(51) C 1.715(1) 0.1072(4) 2.2097(4) 0.038(2) Uani 1.00 d . . . C(52) C 1.8411(10) 0.0963(4) 2.1400(5) 0.034(2) Uani 1.00 d . . . C(53) C 2.0112(9) 0.1173(4) 2.1440(4) 0.027(2) Uani 1.00 d . . . C(54) C 2.0500(9) 0.1522(4) 2.2226(4) 0.027(2) Uani 1.00 d . . . C(55) C 1.9827(5) 0.2047(3) 2.3813(2) -0.0166 Uani 1.00 d . . . C(56) C 1.611(1) 0.1549(4) 2.3628(5) 0.037(2) Uani 1.00 d . . . H(1) H 0.6408 0.0056 1.8314 0.0282 Uiso 1.00 calc . . . H(2) H 0.7061 0.0211 1.9349 0.0282 Uiso 1.00 calc . . . H(3) H 0.7842 -0.0758 1.8466 0.0231 Uiso 1.00 calc . . . H(4) H 0.6504 -0.0690 1.9311 0.0231 Uiso 1.00 calc . . . H(5) H 0.8786 -0.0423 2.0330 0.0237 Uiso 1.00 calc . . . H(6) H 1.1750 -0.0395 1.9851 0.0238 Uiso 1.00 calc . . . H(7) H 1.1206 -0.0572 1.8810 0.0238 Uiso 1.00 calc . . . H(8) H 1.0338 0.0393 1.9633 0.0216 Uiso 1.00 calc . . . H(9) H 1.2210 0.0820 1.8630 0.0275 Uiso 1.00 calc . . . H(10) H 1.3323 0.0358 1.9063 0.0275 Uiso 1.00 calc . . . H(11) H 1.3751 0.0484 1.7399 0.0220 Uiso 1.00 calc . . . H(12) H 1.0973 0.0681 1.6845 0.0209 Uiso 1.00 calc . . . H(13) H 0.9828 -0.0305 1.7446 0.0169 Uiso 1.00 calc . . . H(14) H 0.7593 0.0411 1.6489 0.0216 Uiso 1.00 calc . . . H(15) H 0.7038 -0.0151 1.6813 0.0216 Uiso 1.00 calc . . . H(16) H 0.7539 -0.0112 1.5141 0.0194 Uiso 1.00 calc . . . H(17) H 1.1862 -0.0272 1.6032 0.0209 Uiso 1.00 calc . . . H(18) H 1.3437 0.0665 1.5444 0.0285 Uiso 1.00 calc . . . H(19) H 1.4398 0.0135 1.5662 0.0285 Uiso 1.00 calc . . . H(20) H 1.3122 0.0410 1.3916 0.0359 Uiso 1.00 calc . . . H(21) H 1.3877 -0.0144 1.4165 0.0359 Uiso 1.00 calc . . . H(22) H 1.1203 -0.0483 1.4410 0.0228 Uiso 1.00 calc . . . H(23) H 0.8655 0.0694 1.4456 0.0285 Uiso 1.00 calc . . . H(24) H 1.0579 0.0890 1.4696 0.0285 Uiso 1.00 calc . . . H(25) H 0.9153 0.0865 1.5507 0.0285 Uiso 1.00 calc . . . H(26) H 0.7542 0.0923 1.7862 0.0322 Uiso 1.00 calc . . . H(27) H 0.9546 0.1067 1.8011 0.0322 Uiso 1.00 calc . . . H(28) H 0.8308 0.1008 1.8903 0.0322 Uiso 1.00 calc . . . H(29) H 1.0234 0.0301 1.3126 0.0267 Uiso 1.00 calc . . . H(30) H 0.8331 -0.0639 1.3299 0.0343 Uiso 1.00 calc . . . H(31) H 0.7952 -0.0219 1.2503 0.0343 Uiso 1.00 calc . . . H(32) H 0.7596 -0.0089 1.3585 0.0343 Uiso 1.00 calc . . . H(33) H 1.0925 -0.0288 1.1879 0.0261 Uiso 1.00 calc . . . H(34) H 1.2595 -0.0115 1.2479 0.0261 Uiso 1.00 calc . . . H(35) H 1.0907 -0.1085 1.2775 0.0335 Uiso 1.00 calc . . . H(36) H 1.2703 -0.0915 1.3257 0.0335 Uiso 1.00 calc . . . H(37) H 1.0275 -0.1196 2.0472 0.0349 Uiso 1.00 calc . . . H(38) H 1.3813 -0.0385 1.7051 0.0225 Uiso 1.00 calc . . . H(39) H 0.7867 -0.0896 1.5913 0.0297 Uiso 1.00 calc . . . H(40) H 1.5502 -0.1279 1.1503 0.0352 Uiso 1.00 calc . . . H(41) H 1.1384 0.2412 1.5626 0.0252 Uiso 1.00 calc . . . H(42) H 1.0806 0.2585 1.6657 0.0252 Uiso 1.00 calc . . . H(43) H 1.1079 0.3330 1.5645 0.0315 Uiso 1.00 calc . . . H(44) H 1.2444 0.3369 1.6500 0.0315 Uiso 1.00 calc . . . H(45) H 1.3268 0.3027 1.4646 0.0320 Uiso 1.00 calc . . . H(46) H 1.6207 0.2943 1.5140 0.0266 Uiso 1.00 calc . . . H(47) H 1.5731 0.3135 1.6176 0.0266 Uiso 1.00 calc . . . H(48) H 1.4630 0.2178 1.5365 0.0208 Uiso 1.00 calc . . . H(49) H 1.6551 0.1733 1.6327 0.0216 Uiso 1.00 calc . . . H(50) H 1.7663 0.2202 1.5932 0.0216 Uiso 1.00 calc . . . H(51) H 1.8089 0.2044 1.7616 0.0229 Uiso 1.00 calc . . . H(52) H 1.5330 0.1880 1.8152 0.0243 Uiso 1.00 calc . . . H(53) H 1.4273 0.2872 1.7543 0.0239 Uiso 1.00 calc . . . H(54) H 1.1945 0.2190 1.8492 0.0279 Uiso 1.00 calc . . . H(55) H 1.1457 0.2754 1.8144 0.0279 Uiso 1.00 calc . . . H(56) H 1.1985 0.2716 1.9800 0.0254 Uiso 1.00 calc . . . H(57) H 1.6330 0.2824 1.8946 0.0204 Uiso 1.00 calc . . . H(58) H 1.7656 0.1855 1.9588 0.0288 Uiso 1.00 calc . . . H(59) H 1.8781 0.2346 1.9317 0.0288 Uiso 1.00 calc . . . H(60) H 1.8374 0.2705 2.0783 0.0290 Uiso 1.00 calc . . . H(61) H 1.7609 0.2166 2.1110 0.0290 Uiso 1.00 calc . . . H(62) H 1.5725 0.3053 2.0569 0.0222 Uiso 1.00 calc . . . H(63) H 1.4954 0.1689 2.0325 0.0297 Uiso 1.00 calc . . . H(64) H 1.3041 0.1899 2.0522 0.0297 Uiso 1.00 calc . . . H(65) H 1.3541 0.1707 1.9490 0.0297 Uiso 1.00 calc . . . H(66) H 1.3774 0.1519 1.6965 0.0345 Uiso 1.00 calc . . . H(67) H 1.1794 0.1689 1.7091 0.0345 Uiso 1.00 calc . . . H(68) H 1.2549 0.1596 1.6059 0.0345 Uiso 1.00 calc . . . H(69) H 1.4634 0.2274 2.1849 0.0228 Uiso 1.00 calc . . . H(70) H 1.2413 0.2823 2.2427 0.0360 Uiso 1.00 calc . . . H(71) H 1.2970 0.3263 2.1708 0.0360 Uiso 1.00 calc . . . H(72) H 1.2097 0.2749 2.1319 0.0360 Uiso 1.00 calc . . . H(73) H 1.7060 0.2666 2.2579 0.0343 Uiso 1.00 calc . . . H(74) H 1.5404 0.2887 2.3115 0.0343 Uiso 1.00 calc . . . H(75) H 1.7415 0.3447 2.1738 0.0315 Uiso 1.00 calc . . . H(76) H 1.5623 0.3664 2.2136 0.0315 Uiso 1.00 calc . . . H(77) H 1.4913 0.3769 1.4531 0.0386 Uiso 1.00 calc . . . H(78) H 1.8241 0.2912 1.7967 0.0275 Uiso 1.00 calc . . . H(79) H 1.2429 0.3509 1.9075 0.0210 Uiso 1.00 calc . . . H(80) H 1.9696 0.3936 2.3537 0.0428 Uiso 1.00 calc . . . H(81) H 1.8097 0.0726 2.0873 0.0404 Uiso 1.00 calc . . . H(82) H 2.0973 0.1077 2.0960 0.0315 Uiso 1.00 calc . . . H(83) H 2.1667 0.1656 2.2275 0.0325 Uiso 1.00 calc . . . H(84) H 2.0179 0.2363 2.3549 -0.0199 Uiso 1.00 calc . . . H(85) H 1.8846 0.2082 2.4234 -0.0199 Uiso 1.00 calc . . . H(86) H 2.0808 0.1885 2.4166 -0.0199 Uiso 1.00 calc . . . H(87) H 1.6529 0.1434 2.4252 0.0448 Uiso 1.00 calc . . . H(88) H 1.5877 0.1903 2.3618 0.0448 Uiso 1.00 calc . . . H(89) H 1.5045 0.1348 2.3471 0.0448 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) 0.086(2) 0.090(2) 0.097(2) -0.023(2) -0.002(2) 0.024(2) O(1) 0.029(3) 0.025(2) 0.031(3) -0.006(2) -0.007(2) 0.008(2) O(2) 0.018(2) 0.021(2) 0.015(2) 0.001(2) -0.003(2) -0.004(2) O(3) 0.029(3) 0.012(2) 0.030(2) 0.001(2) -0.002(2) 0.003(2) O(4) 0.036(3) 0.031(3) 0.019(2) 0.006(2) -0.001(2) -0.002(2) O(5) 0.028(2) 0.021(2) 0.037(3) 0.002(2) -0.002(2) -0.005(2) O(6) 0.030(3) 0.030(2) 0.031(2) 0.006(2) 0.005(2) 0.016(2) O(7) 0.025(3) 0.018(2) 0.024(2) -0.003(2) 0.006(2) 0.002(2) O(8) 0.017(2) 0.015(2) 0.019(2) 0.000(2) -0.004(2) 0.002(2) O(9) 0.039(3) 0.031(3) 0.031(2) -0.017(2) 0.008(2) -0.009(2) O(10) 0.033(2) 0.026(2) 0.028(2) 0.001(2) 0.000(2) -0.008(2) C(1) 0.019(3) 0.029(3) 0.020(3) 0.003(3) 0.005(3) 0.001(3) C(2) 0.012(3) 0.027(3) 0.016(3) 0.004(3) 0.005(2) 0.003(2) C(3) 0.014(3) 0.025(2) 0.020(3) -0.001(2) 0.000(2) 0.008(2) C(4) 0.016(3) 0.022(3) 0.020(3) -0.001(2) 0.003(2) 0.005(2) C(5) 0.010(3) 0.022(3) 0.019(3) 0.007(2) -0.004(2) -0.002(2) C(6) 0.019(3) 0.026(3) 0.023(3) -0.004(3) 0.003(3) -0.009(3) C(7) 0.020(3) 0.018(2) 0.018(3) -0.006(2) -0.002(2) 0.004(2) C(8) 0.017(3) 0.020(3) 0.014(3) -0.003(2) 0.004(2) 0.002(2) C(9) 0.012(3) 0.015(3) 0.014(3) 0.000(2) 0.003(2) 0.004(2) C(10) 0.011(3) 0.024(3) 0.018(3) 0.008(2) -0.007(2) 0.000(2) C(11) 0.010(3) 0.025(3) 0.018(3) 0.003(3) 0.002(2) -0.009(2) C(12) 0.020(3) 0.012(2) 0.016(3) 0.002(2) 0.000(2) -0.003(2) C(13) 0.015(3) 0.014(3) 0.023(3) 0.002(2) -0.001(2) 0.000(2) C(14) 0.023(3) 0.018(3) 0.009(3) 0.004(2) 0.001(2) -0.002(2) C(15) 0.025(4) 0.025(3) 0.022(3) -0.004(3) 0.006(3) -0.004(3) C(16) 0.030(3) 0.031(4) 0.029(3) 0.000(3) -0.002(3) -0.007(3) C(17) 0.024(3) 0.016(3) 0.015(2) 0.000(2) -0.003(2) 0.000(2) C(18) 0.019(4) 0.022(3) 0.027(4) 0.004(3) 0.003(3) 0.009(3) C(19) 0.036(4) 0.023(3) 0.020(3) 0.004(3) -0.009(3) -0.002(3) C(20) 0.028(3) 0.022(3) 0.015(3) 0.006(3) 0.001(2) -0.001(2) C(21) 0.031(3) 0.035(4) 0.020(3) -0.004(3) 0.000(3) 0.000(3) C(22) 0.033(4) 0.024(3) 0.007(3) 0.005(3) -0.002(2) 0.005(2) C(23) 0.029(4) 0.023(3) 0.029(3) 0.008(3) 0.006(3) 0.003(3) C(24) 0.031(3) 0.016(3) 0.026(3) -0.003(3) -0.002(2) 0.003(2) C(25) 0.024(3) 0.021(3) 0.015(3) 0.001(2) -0.004(2) -0.001(2) C(26) 0.014(3) 0.024(3) 0.039(4) -0.006(3) -0.002(2) 0.008(3) C(27) 0.016(3) 0.026(3) 0.035(4) 0.004(3) -0.003(2) 0.002(3) C(28) 0.018(3) 0.026(3) 0.024(3) 0.005(3) 0.007(2) 0.006(3) C(29) 0.018(3) 0.024(3) 0.010(3) 0.000(2) 0.001(2) -0.004(2) C(30) 0.018(3) 0.023(3) 0.013(2) 0.006(2) 0.006(2) 0.006(2) C(31) 0.023(3) 0.012(2) 0.023(3) 0.002(2) -0.003(2) -0.002(2) C(32) 0.025(3) 0.018(3) 0.018(3) 0.006(3) -0.001(2) 0.001(2) C(33) 0.017(3) 0.018(3) 0.023(3) 0.000(2) 0.000(2) -0.002(2) C(34) 0.015(3) 0.019(3) 0.020(3) -0.006(2) 0.001(2) 0.005(2) C(35) 0.011(3) 0.026(3) 0.033(3) -0.009(3) -0.003(2) -0.002(3) C(36) 0.015(3) 0.018(2) 0.029(3) -0.002(2) 0.002(2) -0.001(2) C(37) 0.020(3) 0.013(3) 0.023(3) 0.002(2) 0.001(2) 0.000(2) C(38) 0.022(3) 0.011(3) 0.018(3) -0.006(2) -0.003(2) 0.000(2) C(39) 0.021(4) 0.023(3) 0.028(3) 0.006(3) -0.004(3) -0.003(3) C(40) 0.025(3) 0.019(3) 0.028(3) 0.010(3) -0.007(3) -0.002(2) C(41) 0.022(3) 0.017(3) 0.017(3) 0.003(2) 0.008(2) -0.004(2) C(42) 0.034(4) 0.016(3) 0.021(3) -0.012(3) 0.003(3) 0.000(2) C(43) 0.031(4) 0.020(3) 0.033(4) -0.007(3) 0.018(3) -0.001(3) C(44) 0.020(3) 0.020(3) 0.018(3) -0.005(2) 0.007(2) 0.004(2) C(45) 0.020(3) 0.025(3) 0.041(4) -0.002(3) 0.002(3) -0.011(3) C(46) 0.034(4) 0.022(3) 0.027(3) -0.001(3) -0.011(3) -0.001(3) C(47) 0.033(4) 0.025(3) 0.021(3) -0.004(3) -0.003(3) 0.004(3) C(48) 0.035(3) 0.020(3) 0.025(3) -0.002(3) -0.001(2) 0.000(2) C(49) 0.034(3) 0.025(3) 0.027(3) 0.011(3) 0.001(3) 0.007(3) C(50) 0.036(3) 0.016(3) 0.029(3) 0.008(2) 0.002(3) 0.006(2) C(51) 0.066(3) 0.037(4) 0.010(3) 0.011(3) 0.000(3) 0.006(2) C(52) 0.033(4) 0.028(4) 0.040(4) -0.001(3) 0.000(3) -0.001(3) C(53) 0.035(4) 0.025(3) 0.020(3) -0.003(3) 0.005(3) 0.000(2) C(54) 0.036(4) 0.021(3) 0.024(3) -0.007(3) 0.004(3) -0.001(2) C(55) -0.002(2) -0.019(1) -0.030(1) -0.001(1) -0.007(1) -0.003(1) C(56) 0.056(5) 0.036(4) 0.020(3) 0.008(4) 0.009(3) 0.008(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(1) C(51) 1.71(1) . . yes O(1) C(3) 1.46(1) . . yes O(2) C(7) 1.46(1) . . yes O(3) C(12) 1.46(1) . . yes O(4) C(24) 1.21(1) . . yes O(5) C(24) 1.33(1) . . yes O(6) C(27) 1.44(1) . . yes O(7) C(31) 1.46(1) . . yes O(8) C(36) 1.47(1) . . yes O(9) C(48) 1.20(1) . . yes O(10) C(48) 1.34(1) . . yes C(1) C(2) 1.54(1) . . yes C(1) C(10) 1.54(1) . . yes C(2) C(3) 1.50(1) . . yes C(3) C(4) 1.55(1) . . yes C(4) C(5) 1.52(1) . . yes C(5) C(6) 1.55(1) . . yes C(5) C(10) 1.56(1) . . yes C(6) C(7) 1.51(1) . . yes C(7) C(8) 1.52(1) . . yes C(8) C(9) 1.54(1) . . yes C(8) C(14) 1.53(1) . . yes C(9) C(10) 1.55(1) . . yes C(9) C(11) 1.55(1) . . yes C(10) C(19) 1.54(1) . . yes C(11) C(12) 1.53(1) . . yes C(12) C(13) 1.53(1) . . yes C(13) C(14) 1.54(1) . . yes C(13) C(17) 1.56(1) . . yes C(13) C(18) 1.54(1) . . yes C(14) C(15) 1.54(1) . . yes C(15) C(16) 1.54(1) . . yes C(16) C(17) 1.55(1) . . yes C(17) C(20) 1.51(1) . . yes C(20) C(21) 1.54(1) . . yes C(20) C(22) 1.54(1) . . yes C(22) C(23) 1.54(1) . . yes C(23) C(24) 1.49(1) . . yes C(25) C(26) 1.55(1) . . yes C(25) C(34) 1.54(1) . . yes C(26) C(27) 1.48(1) . . yes C(27) C(28) 1.53(1) . . yes C(28) C(29) 1.55(1) . . yes C(29) C(30) 1.56(1) . . yes C(29) C(34) 1.53(1) . . yes C(30) C(31) 1.52(1) . . yes C(31) C(32) 1.50(1) . . yes C(32) C(33) 1.55(1) . . yes C(32) C(38) 1.50(1) . . yes C(33) C(34) 1.54(1) . . yes C(33) C(35) 1.56(1) . . yes C(34) C(43) 1.54(1) . . yes C(35) C(36) 1.50(1) . . yes C(36) C(37) 1.56(1) . . yes C(37) C(38) 1.51(1) . . yes C(37) C(41) 1.55(1) . . yes C(37) C(42) 1.57(1) . . yes C(38) C(39) 1.55(1) . . yes C(39) C(40) 1.56(1) . . yes C(40) C(41) 1.55(1) . . yes C(41) C(44) 1.54(1) . . yes C(44) C(45) 1.55(1) . . yes C(44) C(46) 1.59(1) . . yes C(46) C(47) 1.55(1) . . yes C(47) C(48) 1.49(1) . . yes C(49) C(50) 1.39(1) . . yes C(49) C(54) 1.38(1) . . yes C(49) C(55) 1.66(1) . . yes C(50) C(51) 1.42(1) . . yes C(50) C(56) 1.53(1) . . yes C(51) C(52) 1.38(1) . . yes C(52) C(53) 1.38(1) . . yes C(53) C(54) 1.43(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) C(1) C(10) 115.2(8) . 1_555 1_555 yes C(1) C(2) C(3) 107.8(8) . 1_555 1_555 yes O(1) C(3) C(2) 108.2(8) . 1_555 1_555 yes O(1) C(3) C(4) 110.5(7) . 1_555 1_555 yes C(2) C(3) C(4) 112.0(7) . 1_555 1_555 yes C(3) C(4) C(5) 111.7(8) . 1_555 1_555 yes C(4) C(5) C(6) 112.9(8) . 1_555 1_555 yes C(4) C(5) C(10) 113.1(8) . 1_555 1_555 yes C(6) C(5) C(10) 109.6(8) . 1_555 1_555 yes C(5) C(6) C(7) 114.8(8) . 1_555 1_555 yes O(2) C(7) C(6) 108.3(7) . 1_555 1_555 yes O(2) C(7) C(8) 111.5(7) . 1_555 1_555 yes C(6) C(7) C(8) 112.3(8) . 1_555 1_555 yes C(7) C(8) C(9) 111.6(7) . 1_555 1_555 yes C(7) C(8) C(14) 111.4(7) . 1_555 1_555 yes C(9) C(8) C(14) 110.4(7) . 1_555 1_555 yes C(8) C(9) C(10) 111.3(7) . 1_555 1_555 yes C(8) C(9) C(11) 111.0(7) . 1_555 1_555 yes C(10) C(9) C(11) 114.3(7) . 1_555 1_555 yes C(1) C(10) C(5) 107.5(7) . 1_555 1_555 yes C(1) C(10) C(9) 112.7(7) . 1_555 1_555 yes C(1) C(10) C(19) 105.0(8) . 1_555 1_555 yes C(5) C(10) C(9) 108.8(7) . 1_555 1_555 yes C(5) C(10) C(19) 110.1(7) . 1_555 1_555 yes C(9) C(10) C(19) 112.6(7) . 1_555 1_555 yes C(9) C(11) C(12) 114.0(7) . 1_555 1_555 yes O(3) C(12) C(11) 109.1(7) . 1_555 1_555 yes O(3) C(12) C(13) 110.4(7) . 1_555 1_555 yes C(11) C(12) C(13) 111.5(7) . 1_555 1_555 yes C(12) C(13) C(14) 107.8(7) . 1_555 1_555 yes C(12) C(13) C(17) 117.3(7) . 1_555 1_555 yes C(12) C(13) C(18) 108.2(8) . 1_555 1_555 yes C(14) C(13) C(17) 99.9(7) . 1_555 1_555 yes C(14) C(13) C(18) 114.0(7) . 1_555 1_555 yes C(17) C(13) C(18) 109.6(8) . 1_555 1_555 yes C(8) C(14) C(13) 114.8(8) . 1_555 1_555 yes C(8) C(14) C(15) 119.6(8) . 1_555 1_555 yes C(13) C(14) C(15) 104.5(7) . 1_555 1_555 yes C(14) C(15) C(16) 103.7(8) . 1_555 1_555 yes C(15) C(16) C(17) 107.2(8) . 1_555 1_555 yes C(13) C(17) C(16) 103.3(8) . 1_555 1_555 yes C(13) C(17) C(20) 120.6(8) . 1_555 1_555 yes C(16) C(17) C(20) 112.1(8) . 1_555 1_555 yes C(17) C(20) C(21) 115.6(8) . 1_555 1_555 yes C(17) C(20) C(22) 111.3(8) . 1_555 1_555 yes C(21) C(20) C(22) 110.4(8) . 1_555 1_555 yes C(20) C(22) C(23) 113.6(7) . 1_555 1_555 yes C(22) C(23) C(24) 111.4(8) . 1_555 1_555 yes O(4) C(24) O(5) 122.1(10) . 1_555 1_555 yes O(4) C(24) C(23) 124(1) . 1_555 1_555 yes O(5) C(24) C(23) 113.5(9) . 1_555 1_555 yes C(26) C(25) C(34) 114.2(8) . 1_555 1_555 yes C(25) C(26) C(27) 109.7(8) . 1_555 1_555 yes O(6) C(27) C(26) 108.6(8) . 1_555 1_555 yes O(6) C(27) C(28) 110.5(8) . 1_555 1_555 yes C(26) C(27) C(28) 112.2(8) . 1_555 1_555 yes C(27) C(28) C(29) 111.0(8) . 1_555 1_555 yes C(28) C(29) C(30) 109.9(8) . 1_555 1_555 yes C(28) C(29) C(34) 114.0(7) . 1_555 1_555 yes C(30) C(29) C(34) 112.3(7) . 1_555 1_555 yes C(29) C(30) C(31) 113.9(7) . 1_555 1_555 yes O(7) C(31) C(30) 106.5(7) . 1_555 1_555 yes O(7) C(31) C(32) 110.8(7) . 1_555 1_555 yes C(30) C(31) C(32) 114.0(8) . 1_555 1_555 yes C(31) C(32) C(33) 111.9(7) . 1_555 1_555 yes C(31) C(32) C(38) 112.7(8) . 1_555 1_555 yes C(33) C(32) C(38) 109.9(8) . 1_555 1_555 yes C(32) C(33) C(34) 112.9(8) . 1_555 1_555 yes C(32) C(33) C(35) 112.0(8) . 1_555 1_555 yes C(34) C(33) C(35) 114.7(8) . 1_555 1_555 yes C(25) C(34) C(29) 108.3(7) . 1_555 1_555 yes C(25) C(34) C(33) 112.8(8) . 1_555 1_555 yes C(25) C(34) C(43) 105.1(8) . 1_555 1_555 yes C(29) C(34) C(33) 109.6(7) . 1_555 1_555 yes C(29) C(34) C(43) 109.8(7) . 1_555 1_555 yes C(33) C(34) C(43) 111.2(8) . 1_555 1_555 yes C(33) C(35) C(36) 113.4(8) . 1_555 1_555 yes O(8) C(36) C(35) 112.3(8) . 1_555 1_555 yes O(8) C(36) C(37) 107.1(7) . 1_555 1_555 yes C(35) C(36) C(37) 111.8(8) . 1_555 1_555 yes C(36) C(37) C(38) 107.9(7) . 1_555 1_555 yes C(36) C(37) C(41) 118.8(8) . 1_555 1_555 yes C(36) C(37) C(42) 107.6(8) . 1_555 1_555 yes C(38) C(37) C(41) 101.1(7) . 1_555 1_555 yes C(38) C(37) C(42) 113.4(7) . 1_555 1_555 yes C(41) C(37) C(42) 108.1(7) . 1_555 1_555 yes C(32) C(38) C(37) 116.9(8) . 1_555 1_555 yes C(32) C(38) C(39) 117.6(8) . 1_555 1_555 yes C(37) C(38) C(39) 103.5(7) . 1_555 1_555 yes C(38) C(39) C(40) 103.9(7) . 1_555 1_555 yes C(39) C(40) C(41) 105.4(8) . 1_555 1_555 yes C(37) C(41) C(40) 104.6(7) . 1_555 1_555 yes C(37) C(41) C(44) 120.0(8) . 1_555 1_555 yes C(40) C(41) C(44) 112.3(8) . 1_555 1_555 yes C(41) C(44) C(45) 114.5(8) . 1_555 1_555 yes C(41) C(44) C(46) 110.9(8) . 1_555 1_555 yes C(45) C(44) C(46) 108.9(8) . 1_555 1_555 yes C(44) C(46) C(47) 113.4(8) . 1_555 1_555 yes C(46) C(47) C(48) 109.7(8) . 1_555 1_555 yes O(9) C(48) O(10) 123.3(10) . 1_555 1_555 yes O(9) C(48) C(47) 123(1) . 1_555 1_555 yes O(10) C(48) C(47) 112.9(9) . 1_555 1_555 yes C(50) C(49) C(54) 120.6(10) . 1_555 1_555 yes C(50) C(49) C(55) 120.9(8) . 1_555 1_555 yes C(54) C(49) C(55) 118.5(9) . 1_555 1_555 yes C(49) C(50) C(51) 117.6(10) . 1_555 1_555 yes C(49) C(50) C(56) 122.0(10) . 1_555 1_555 yes C(51) C(50) C(56) 120(1) . 1_555 1_555 yes Cl(1) C(51) C(50) 118.2(9) . 1_555 1_555 yes Cl(1) C(51) C(52) 120.7(9) . 1_555 1_555 yes C(50) C(51) C(52) 121(1) . 1_555 1_555 yes C(51) C(52) C(53) 122(1) . 1_555 1_555 yes C(52) C(53) C(54) 116.7(9) . 1_555 1_555 yes C(49) C(54) C(53) 121.9(10) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl(1) C(51) C(50) C(49) -177.2(8) 1_555 1_555 1_555 1_555 yes Cl(1) C(51) C(50) C(56) 2(1) 1_555 1_555 1_555 1_555 yes Cl(1) C(51) C(52) C(53) 178.3(9) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) -178.9(7) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 177.5(7) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -73(1) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 70.3(9) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -53.6(9) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 67.1(9) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -65.7(9) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 45(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 170.5(7) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -83(1) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 97.8(10) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(26) C(25) -179.1(8) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(28) C(29) 176.5(7) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(30) C(29) -75.3(10) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(33) 71.3(10) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(38) -53.1(10) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(35) C(33) 66(1) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(38) -68.9(9) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(41) 45(1) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(42) 168.4(7) 1_555 1_555 1_555 1_555 yes O(9) C(48) C(47) C(46) -75(1) 1_555 1_555 1_555 1_555 yes O(10) C(48) C(47) C(46) 106.1(10) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -56.9(10) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 51.4(9) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 178.4(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -178.9(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 54.4(10) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -55.2(10) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 64.7(10) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -172.5(8) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 56(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 58.9(10) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -178.9(8) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.7(10) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 73(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -70.9(10) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 165.3(8) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 50(1) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -59.8(9) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 173.5(7) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 56.1(9) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -67.7(10) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -51.5(10) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -175.4(8) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -53(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 57.3(9) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -174.2(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -179.4(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -54(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 62.6(10) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 51.2(10) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -58.2(9) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 178.8(7) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 61(1) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -163.0(8) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 56.0(10) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -178.6(8) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -55.1(10) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -178.3(7) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 178.0(7) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -49.8(9) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -64.1(10) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 55.7(10) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 167.4(8) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -68.0(9) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 168.9(7) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -156.8(8) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 77(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -32.8(9) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 21.6(10) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -56(1) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 176.3(8) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -40.8(9) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -166.9(8) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 6(1) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 45.9(8) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -71.0(9) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 153.0(8) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 79.3(9) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) -178.5(8) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 54(1) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) 56(1) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -46(1) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 173.1(9) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) -73(1) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -56(1) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(28) 51.3(10) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(30) 177.1(8) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(32) -177.4(8) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(35) 52(1) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(29) -53.6(10) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(33) 67.8(10) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(43) -170.9(7) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 55(1) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(34) 57(1) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) -179.9(8) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(34) -52(1) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 78.2(9) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(33) -72.2(10) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(43) 165.4(8) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 47(1) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) -56.7(10) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(35) 173.4(7) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) 53.6(10) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) -68.8(10) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -48(1) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(38) -173.2(8) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) -49(1) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 54(1) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(35) -174.3(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(37) -179.9(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(39) -55(1) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) 64(1) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(35) C(36) 50(1) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(36) -56.9(10) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(41) 177.6(8) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(42) 62(1) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(39) C(40) -166.8(8) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(37) 54(1) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(39) 178.7(8) 1_555 1_555 1_555 1_555 yes C(33) C(35) C(36) C(37) -54(1) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(38) -179.6(7) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(35) C(36) -178.8(8) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(32) C(38) -48(1) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(34) C(43) -65(1) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 54.6(10) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(41) 168.7(8) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(42) -68.2(10) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) 172.1(7) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(40) -157.0(8) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(44) 75(1) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) -36.3(9) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(40) C(39) 16.9(10) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(45) -58(1) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(46) 177.7(8) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(40) -39.2(9) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(44) -166.3(8) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) 11.3(10) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(41) 46.7(8) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(42) -68.7(9) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(44) 148.5(8) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(37) C(42) 80.1(9) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(45) 177.9(8) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(46) 54(1) 1_555 1_555 1_555 1_555 yes C(41) C(44) C(46) C(47) 52(1) 1_555 1_555 1_555 1_555 yes C(42) C(37) C(41) C(44) -46(1) 1_555 1_555 1_555 1_555 yes C(44) C(46) C(47) C(48) 172.1(9) 1_555 1_555 1_555 1_555 yes C(45) C(44) C(46) C(47) -74(1) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) 0(1) 1_555 1_555 1_555 1_555 yes C(49) C(54) C(53) C(52) 0(1) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(54) C(53) 1(1) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) 1(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(54) 0(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(55) -178.7(8) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) -1(1) 1_555 1_555 1_555 1_555 yes C(52) C(51) C(50) C(56) 178.5(10) 1_555 1_555 1_555 1_555 yes C(53) C(54) C(49) C(55) 179.0(8) 1_555 1_555 1_555 1_555 yes C(54) C(49) C(50) C(56) 180.0(9) 1_555 1_555 1_555 1_555 yes C(55) C(49) C(50) C(56) 2(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(8) 2.654(9) . 2_749 ? O(1) O(4) 2.711(10) . 1_556 ? O(1) C(36) 3.36(1) . 2_749 ? O(2) C(48) 2.99(1) . 2_849 ? O(2) O(9) 3.125(9) . 2_849 ? O(2) C(47) 3.23(1) . 2_849 ? O(2) C(1) 3.35(1) . 1_655 ? O(2) O(10) 3.466(9) . 2_849 ? O(3) O(10) 2.656(9) . 2_849 ? O(3) O(6) 2.679(10) . 2_748 ? O(3) O(9) 3.384(10) . 2_849 ? O(3) C(48) 3.42(1) . 2_849 ? O(3) C(27) 3.53(1) . 2_748 ? O(4) O(7) 3.106(9) . 2_848 ? O(4) C(38) 3.38(1) . 2_848 ? O(4) O(8) 3.402(9) . 2_848 ? O(4) C(3) 3.50(1) . 1_554 ? O(4) C(4) 3.55(1) . 1_554 ? O(5) O(8) 2.666(9) . 2_848 ? O(5) O(7) 3.456(9) . 2_848 ? O(5) C(33) 3.59(1) . 2_848 ? O(6) O(9) 2.721(10) . 1_554 ? O(6) C(12) 3.42(1) . 2_758 ? O(7) C(24) 3.01(1) . 2_858 ? O(7) C(23) 3.31(1) . 2_858 ? O(7) C(25) 3.34(1) . 1_655 ? O(8) C(24) 3.45(1) . 2_858 ? O(8) C(3) 3.58(1) . 2_759 ? O(9) C(14) 3.38(1) . 2_859 ? O(9) C(27) 3.49(1) . 1_556 ? O(9) C(28) 3.53(1) . 1_556 ? O(10) C(9) 3.53(1) . 2_859 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_aburaya77_ _database_code_depnum_ccdc_archive 'CCDC 297673' _audit_creation_date 'Thu Apr 27 00:09:24 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C55 H86 Cl2 O10 ' _chemical_formula_moiety ? _chemical_formula_weight 978.18 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 7.463(1) _cell_length_b 25.378(3) _cell_length_c 13.764(2) _cell_angle_alpha 90 _cell_angle_beta 90.63(1) _cell_angle_gamma 90 _cell_volume 2606.9(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 29344 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 68.3 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.900 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.854 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5419 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27351 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_theta_max 68.25 _diffrn_measured_fraction_theta_max 0.9616 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_full 0.9616 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # 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 4682 _reflns_number_gt 4258 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2170 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4682 _refine_ls_number_parameters 604 _refine_ls_goodness_of_fit_ref 2.007 _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 0.0004 _refine_diff_density_max 1.27 _refine_diff_density_min -0.59 _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 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.364 0.702 ;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 0.4076(2) 0.0534(3) 1.13119(10) 0.0419(4) Uani 1.00 d . . . Cl(2) Cl 0.4943(3) -0.0209(3) 1.3025(2) 0.0668(6) Uani 1.00 d . . . O(1) O 0.0641(4) -0.2168(3) 0.5031(3) 0.0266(9) Uani 1.00 d . . . O(2) O -0.3472(4) -0.1271(3) 0.7315(2) 0.0196(8) Uani 1.00 d . . . O(3) O 0.1096(4) -0.1719(3) 0.9331(2) 0.0205(8) Uani 1.00 d . . . O(4) O -0.2289(5) -0.2307(3) 1.3873(3) 0.0275(9) Uani 1.00 d . . . O(5) O -0.4759(5) -0.2140(3) 1.2999(3) 0.0270(9) Uani 1.00 d . . . O(6) O -0.3944(4) 0.2758(3) 0.9982(3) 0.0288(9) Uani 1.00 d . . . O(7) O -0.7872(4) 0.1805(3) 0.7674(2) 0.0198(8) Uani 1.00 d . . . O(8) O -0.3431(4) 0.2305(3) 0.5693(2) 0.0199(8) Uani 1.00 d . . . O(9) O -0.6888(5) 0.2836(3) 0.1129(3) 0.0289(9) Uani 1.00 d . . . O(10) O -0.9357(4) 0.2709(3) 0.1993(2) 0.0243(8) Uani 1.00 d . . . C(1) C 0.2650(6) -0.0980(4) 0.6235(3) 0.018(1) Uani 1.00 d . . . C(2) C 0.2382(6) -0.1558(4) 0.5979(3) 0.020(1) Uani 1.00 d . . . C(3) C 0.0866(6) -0.1616(4) 0.5254(3) 0.019(1) Uani 1.00 d . . . C(4) C -0.0843(6) -0.1383(4) 0.5648(3) 0.019(1) Uani 1.00 d . . . C(5) C -0.0622(6) -0.0796(4) 0.5943(3) 0.0174(10) Uani 1.00 d . . . C(6) C -0.2362(6) -0.0563(4) 0.6330(3) 0.019(1) Uani 1.00 d . . . C(7) C -0.2837(6) -0.0731(4) 0.7365(3) 0.0189(10) Uani 1.00 d . . . C(8) C -0.1241(6) -0.0681(4) 0.8081(3) 0.019(1) Uani 1.00 d . . . C(9) C 0.0474(5) -0.0943(3) 0.7676(3) 0.015(1) Uani 1.00 d . . . C(10) C 0.0959(6) -0.0708(4) 0.6657(3) 0.0184(10) Uani 1.00 d . . . C(11) C 0.2011(6) -0.0934(4) 0.8419(3) 0.019(1) Uani 1.00 d . . . C(12) C 0.1502(6) -0.1163(4) 0.9414(3) 0.0172(10) Uani 1.00 d . . . C(13) C -0.0161(6) -0.0859(4) 0.9832(3) 0.020(1) Uani 1.00 d . . . C(14) C -0.1667(6) -0.0906(3) 0.9055(3) 0.017(1) Uani 1.00 d . . . C(15) C -0.3359(6) -0.0708(4) 0.9585(4) 0.024(1) Uani 1.00 d . . . C(16) C -0.3038(6) -0.0882(4) 1.0663(3) 0.021(1) Uani 1.00 d . . . C(17) C -0.1104(6) -0.1118(3) 1.0723(3) 0.019(1) Uani 1.00 d . . . C(18) C 0.0372(6) -0.0292(4) 1.0072(4) 0.022(1) Uani 1.00 d . . . C(19) C 0.1417(6) -0.0120(4) 0.6722(4) 0.024(1) Uani 1.00 d . . . C(20) C -0.0289(6) -0.1058(4) 1.1740(3) 0.022(1) Uani 1.00 d . . . C(21) C 0.1628(6) -0.1281(4) 1.1830(4) 0.026(1) Uani 1.00 d . . . C(22) C -0.1535(7) -0.1313(4) 1.2513(3) 0.022(1) Uani 1.00 d . . . C(23) C -0.1975(7) -0.1892(4) 1.2307(4) 0.026(1) Uani 1.00 d . . . C(24) C -0.2998(7) -0.2133(4) 1.3136(4) 0.0235(10) Uani 1.00 d . . . C(25) C -0.1757(6) 0.1599(4) 0.8805(4) 0.021(1) Uani 1.00 d . . . C(26) C -0.2097(5) 0.2178(4) 0.9032(3) 0.020(1) Uani 1.00 d . . . C(27) C -0.3610(6) 0.2207(4) 0.9772(4) 0.023(1) Uani 1.00 d . . . C(28) C -0.5308(6) 0.1943(4) 0.9348(4) 0.022(1) Uani 1.00 d . . . C(29) C -0.4937(6) 0.1367(4) 0.9066(3) 0.0173(10) Uani 1.00 d . . . C(30) C -0.6687(6) 0.1099(4) 0.8672(3) 0.019(1) Uani 1.00 d . . . C(31) C -0.7185(6) 0.1270(4) 0.7635(3) 0.0167(10) Uani 1.00 d . . . C(32) C -0.5615(6) 0.1235(3) 0.6923(3) 0.0159(10) Uani 1.00 d . . . C(33) C -0.3936(6) 0.1526(4) 0.7352(3) 0.0155(10) Uani 1.00 d . . . C(34) C -0.3388(6) 0.1299(4) 0.8371(3) 0.0181(10) Uani 1.00 d . . . C(35) C -0.2380(6) 0.1534(4) 0.6609(3) 0.019(1) Uani 1.00 d . . . C(36) C -0.2946(6) 0.1758(4) 0.5611(3) 0.0179(10) Uani 1.00 d . . . C(37) C -0.4541(6) 0.1444(4) 0.5189(3) 0.017(1) Uani 1.00 d . . . C(38) C -0.6079(6) 0.1462(3) 0.5940(3) 0.020(1) Uani 1.00 d . . . C(39) C -0.7725(6) 0.1234(4) 0.5397(3) 0.022(1) Uani 1.00 d . . . C(40) C -0.7475(6) 0.1437(4) 0.4346(3) 0.022(1) Uani 1.00 d . . . C(41) C -0.5586(6) 0.1690(4) 0.4301(3) 0.018(1) Uani 1.00 d . . . C(42) C -0.3945(7) 0.0881(4) 0.4936(4) 0.024(1) Uani 1.00 d . . . C(43) C -0.2811(7) 0.0722(4) 0.8312(4) 0.026(1) Uani 1.00 d . . . C(44) C -0.4763(6) 0.1642(4) 0.3286(3) 0.021(1) Uani 1.00 d . . . C(45) C -0.2868(6) 0.1881(4) 0.3195(3) 0.024(1) Uani 1.00 d . . . C(46) C -0.6038(7) 0.1879(4) 0.2496(4) 0.024(1) Uani 1.00 d . . . C(47) C -0.6615(7) 0.2450(4) 0.2720(4) 0.025(1) Uani 1.00 d . . . C(48) C -0.7615(6) 0.2685(4) 0.1866(4) 0.0212(10) Uani 1.00 d . . . C(49) C 0.0757(7) 0.0625(4) 1.2061(4) 0.030(1) Uani 1.00 d . . . C(50) C 0.2441(7) 0.0402(4) 1.2158(4) 0.029(1) Uani 1.00 d . . . C(51) C 0.2859(7) 0.0059(4) 1.2926(4) 0.030(1) Uani 1.00 d . . . C(52) C 0.1542(7) -0.0055(4) 1.3621(4) 0.027(1) Uani 1.00 d . . . C(53) C -0.0133(7) 0.0152(4) 1.3539(4) 0.025(1) Uani 1.00 d . . . C(54) C -0.0540(7) 0.0502(4) 1.2748(4) 0.028(1) Uani 1.00 d . . . C(55) C 0.0285(4) 0.1029(3) 1.1157(2) -0.0063 Uani 1.00 d . . . H(1) H 0.3593 -0.0951 0.6704 0.0222 Uiso 1.00 calc . . . H(2) H 0.2983 -0.0794 0.5663 0.0222 Uiso 1.00 calc . . . H(3) H 0.2114 -0.1746 0.6555 0.0236 Uiso 1.00 calc . . . H(4) H 0.3456 -0.1689 0.5708 0.0236 Uiso 1.00 calc . . . H(5) H 0.1167 -0.1430 0.4678 0.0222 Uiso 1.00 calc . . . H(6) H -0.1754 -0.1404 0.5162 0.0229 Uiso 1.00 calc . . . H(7) H -0.1194 -0.1575 0.6203 0.0229 Uiso 1.00 calc . . . H(8) H -0.0345 -0.0604 0.5368 0.0207 Uiso 1.00 calc . . . H(9) H -0.3315 -0.0664 0.5910 0.0227 Uiso 1.00 calc . . . H(10) H -0.2260 -0.0186 0.6322 0.0227 Uiso 1.00 calc . . . H(11) H -0.3787 -0.0509 0.7587 0.0225 Uiso 1.00 calc . . . H(12) H -0.0993 -0.0313 0.8162 0.0221 Uiso 1.00 calc . . . H(13) H 0.0188 -0.1300 0.7570 0.0182 Uiso 1.00 calc . . . H(14) H 0.2381 -0.0573 0.8509 0.0229 Uiso 1.00 calc . . . H(15) H 0.2985 -0.1127 0.8167 0.0229 Uiso 1.00 calc . . . H(16) H 0.2494 -0.1116 0.9851 0.0213 Uiso 1.00 calc . . . H(17) H -0.1840 -0.1267 0.8955 0.0208 Uiso 1.00 calc . . . H(18) H -0.3472 -0.0332 0.9537 0.0289 Uiso 1.00 calc . . . H(19) H -0.4409 -0.0866 0.9322 0.0289 Uiso 1.00 calc . . . H(20) H -0.3129 -0.0583 1.1082 0.0259 Uiso 1.00 calc . . . H(21) H -0.3892 -0.1137 1.0842 0.0259 Uiso 1.00 calc . . . H(22) H -0.1200 -0.1481 1.0592 0.0231 Uiso 1.00 calc . . . H(23) H 0.1174 -0.0287 1.0614 0.0270 Uiso 1.00 calc . . . H(24) H -0.0668 -0.0091 1.0227 0.0270 Uiso 1.00 calc . . . H(25) H 0.0943 -0.0135 0.9529 0.0270 Uiso 1.00 calc . . . H(26) H 0.2441 -0.0069 0.7135 0.0282 Uiso 1.00 calc . . . H(27) H 0.0433 0.0070 0.6986 0.0282 Uiso 1.00 calc . . . H(28) H 0.1673 0.0015 0.6094 0.0282 Uiso 1.00 calc . . . H(29) H -0.0220 -0.0688 1.1878 0.0270 Uiso 1.00 calc . . . H(30) H 0.2098 -0.1203 1.2463 0.0299 Uiso 1.00 calc . . . H(31) H 0.2371 -0.1121 1.1357 0.0299 Uiso 1.00 calc . . . H(32) H 0.1600 -0.1649 1.1737 0.0299 Uiso 1.00 calc . . . H(33) H -0.2625 -0.1117 1.2524 0.0259 Uiso 1.00 calc . . . H(34) H -0.0959 -0.1287 1.3130 0.0259 Uiso 1.00 calc . . . H(35) H -0.0890 -0.2079 1.2226 0.0319 Uiso 1.00 calc . . . H(36) H -0.2678 -0.1912 1.1731 0.0319 Uiso 1.00 calc . . . H(37) H -0.0416 -0.2246 0.4653 0.0489 Uiso 1.00 calc . . . H(38) H -0.4286 -0.1463 0.8006 0.0489 Uiso 1.00 calc . . . H(39) H 0.2128 -0.1895 0.9601 0.0489 Uiso 1.00 calc . . . H(40) H -0.5569 -0.2358 1.3553 0.0489 Uiso 1.00 calc . . . H(41) H -0.0808 0.1586 0.8351 0.0252 Uiso 1.00 calc . . . H(42) H -0.1399 0.1433 0.9391 0.0252 Uiso 1.00 calc . . . H(43) H -0.2439 0.2363 0.8457 0.0240 Uiso 1.00 calc . . . H(44) H -0.1043 0.2337 0.9299 0.0240 Uiso 1.00 calc . . . H(45) H -0.3259 0.2033 1.0355 0.0272 Uiso 1.00 calc . . . H(46) H -0.6224 0.1954 0.9822 0.0264 Uiso 1.00 calc . . . H(47) H -0.5687 0.2135 0.8789 0.0264 Uiso 1.00 calc . . . H(48) H -0.4612 0.1190 0.9648 0.0211 Uiso 1.00 calc . . . H(49) H -0.6519 0.0731 0.8676 0.0227 Uiso 1.00 calc . . . H(50) H -0.7646 0.1192 0.9088 0.0227 Uiso 1.00 calc . . . H(51) H -0.8119 0.1050 0.7402 0.0191 Uiso 1.00 calc . . . H(52) H -0.5317 0.0877 0.6844 0.0178 Uiso 1.00 calc . . . H(53) H -0.4283 0.1886 0.7453 0.0188 Uiso 1.00 calc . . . H(54) H -0.1959 0.1189 0.6525 0.0235 Uiso 1.00 calc . . . H(55) H -0.1442 0.1752 0.6868 0.0235 Uiso 1.00 calc . . . H(56) H -0.1962 0.1731 0.5178 0.0212 Uiso 1.00 calc . . . H(57) H -0.6327 0.1827 0.6039 0.0235 Uiso 1.00 calc . . . H(58) H -0.7724 0.0863 0.5414 0.0263 Uiso 1.00 calc . . . H(59) H -0.8807 0.1366 0.5664 0.0263 Uiso 1.00 calc . . . H(60) H -0.7562 0.1157 0.3901 0.0265 Uiso 1.00 calc . . . H(61) H -0.8367 0.1697 0.4197 0.0265 Uiso 1.00 calc . . . H(62) H -0.5724 0.2060 0.4430 0.0219 Uiso 1.00 calc . . . H(63) H -0.3028 0.0898 0.4464 0.0282 Uiso 1.00 calc . . . H(64) H -0.4941 0.0693 0.4681 0.0282 Uiso 1.00 calc . . . H(65) H -0.3506 0.0714 0.5504 0.0282 Uiso 1.00 calc . . . H(66) H -0.1793 0.0699 0.7901 0.0305 Uiso 1.00 calc . . . H(67) H -0.3760 0.0520 0.8046 0.0305 Uiso 1.00 calc . . . H(68) H -0.2506 0.0600 0.8940 0.0305 Uiso 1.00 calc . . . H(69) H -0.4662 0.1280 0.3146 0.0256 Uiso 1.00 calc . . . H(70) H -0.2406 0.1810 0.2569 0.0275 Uiso 1.00 calc . . . H(71) H -0.2925 0.2254 0.3288 0.0275 Uiso 1.00 calc . . . H(72) H -0.2101 0.1733 0.3677 0.0275 Uiso 1.00 calc . . . H(73) H -0.7091 0.1671 0.2457 0.0294 Uiso 1.00 calc . . . H(74) H -0.5451 0.1878 0.1888 0.0294 Uiso 1.00 calc . . . H(75) H -0.7357 0.2457 0.3272 0.0296 Uiso 1.00 calc . . . H(76) H -0.5566 0.2660 0.2850 0.0296 Uiso 1.00 calc . . . H(77) H -0.4980 0.2787 1.0336 0.0489 Uiso 1.00 calc . . . H(78) H -0.8237 0.1919 0.7039 0.0236 Uiso 1.00 calc . . . H(79) H -0.2488 0.2489 0.5417 0.0489 Uiso 1.00 calc . . . H(80) H -0.9938 0.2919 0.1500 0.0489 Uiso 1.00 calc . . . H(81) H 0.1815 -0.0275 1.4159 0.0320 Uiso 1.00 calc . . . H(82) H -0.1023 0.0071 1.3999 0.0290 Uiso 1.00 calc . . . H(83) H -0.1710 0.0651 1.2692 0.0334 Uiso 1.00 calc . . . H(84) H -0.0699 0.0897 1.0791 -0.0076 Uiso 1.00 calc . . . H(85) H 0.1295 0.1067 1.0751 -0.0076 Uiso 1.00 calc . . . H(86) H -0.0027 0.1368 1.1413 -0.0076 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) 0.0478(8) 0.0495(9) 0.0288(6) -0.0208(7) 0.0162(5) -0.0086(6) Cl(2) 0.061(1) 0.071(1) 0.068(1) 0.0116(10) -0.0018(9) -0.011(1) O(1) 0.027(2) 0.026(2) 0.026(2) 0.004(1) -0.001(1) -0.012(1) O(2) 0.012(1) 0.023(2) 0.024(2) -0.003(1) 0.000(1) -0.002(1) O(3) 0.018(2) 0.022(2) 0.021(2) 0.004(1) -0.005(1) -0.001(1) O(4) 0.025(2) 0.031(2) 0.027(2) -0.004(2) -0.003(1) 0.001(2) O(5) 0.024(1) 0.024(2) 0.032(2) 0.002(1) 0.004(1) 0.007(2) O(6) 0.022(2) 0.025(2) 0.039(2) -0.006(1) 0.004(1) -0.014(2) O(7) 0.019(2) 0.018(2) 0.023(2) 0.004(1) 0.003(1) -0.002(1) O(8) 0.018(2) 0.020(2) 0.022(2) 0.001(1) 0.002(1) -0.001(1) O(9) 0.031(2) 0.029(2) 0.027(2) 0.011(1) 0.008(1) 0.007(2) O(10) 0.025(1) 0.025(2) 0.023(2) 0.003(1) 0.004(1) 0.007(1) C(1) 0.017(2) 0.027(2) 0.012(2) -0.003(2) 0.005(2) 0.007(2) C(2) 0.018(2) 0.025(2) 0.017(2) 0.006(2) 0.002(2) 0.002(2) C(3) 0.011(2) 0.023(2) 0.022(2) -0.001(2) 0.003(1) -0.005(2) C(4) 0.015(2) 0.022(2) 0.019(2) 0.005(2) 0.000(2) -0.005(2) C(5) 0.015(2) 0.023(2) 0.014(2) 0.000(2) 0.000(1) 0.000(2) C(6) 0.015(2) 0.023(2) 0.020(2) 0.004(2) -0.001(2) 0.002(2) C(7) 0.024(2) 0.016(2) 0.016(2) 0.005(2) 0.000(2) 0.000(2) C(8) 0.024(2) 0.015(2) 0.017(2) 0.004(2) 0.000(1) 0.000(2) C(9) 0.011(2) 0.022(2) 0.013(2) 0.000(2) 0.002(1) 0.001(2) C(10) 0.020(2) 0.022(2) 0.013(2) -0.002(2) -0.003(1) 0.004(2) C(11) 0.018(2) 0.026(3) 0.014(2) 0.000(2) 0.000(1) 0.002(2) C(12) 0.014(2) 0.023(2) 0.015(2) -0.005(2) 0.002(1) 0.000(2) C(13) 0.019(2) 0.025(2) 0.016(2) -0.003(2) -0.004(1) -0.003(2) C(14) 0.018(2) 0.020(2) 0.013(2) 0.000(2) -0.004(1) -0.001(2) C(15) 0.019(2) 0.032(3) 0.022(2) 0.005(2) 0.000(2) 0.001(2) C(16) 0.012(2) 0.030(3) 0.022(2) -0.004(2) 0.008(2) 0.003(2) C(17) 0.019(2) 0.017(2) 0.021(2) 0.000(2) -0.001(2) -0.001(2) C(18) 0.020(2) 0.025(2) 0.022(2) -0.003(2) -0.003(2) -0.001(2) C(19) 0.024(2) 0.024(2) 0.022(2) -0.002(2) -0.003(2) 0.004(2) C(20) 0.022(2) 0.026(3) 0.019(2) -0.002(2) -0.002(2) 0.004(2) C(21) 0.016(2) 0.039(3) 0.022(2) -0.005(2) -0.001(2) 0.000(2) C(22) 0.031(3) 0.017(2) 0.018(2) -0.001(2) 0.001(2) 0.001(2) C(23) 0.035(3) 0.022(2) 0.023(2) -0.011(2) 0.006(2) -0.003(2) C(24) 0.027(2) 0.017(2) 0.026(2) -0.002(2) 0.001(2) 0.001(2) C(25) 0.015(2) 0.029(2) 0.019(2) 0.000(2) -0.001(2) 0.002(2) C(26) 0.004(2) 0.033(2) 0.025(2) -0.003(2) 0.003(1) -0.002(2) C(27) 0.019(2) 0.029(2) 0.021(2) -0.001(2) 0.005(2) -0.008(2) C(28) 0.023(2) 0.018(2) 0.025(2) -0.006(2) 0.007(2) -0.007(2) C(29) 0.013(2) 0.018(2) 0.021(2) 0.001(2) -0.001(1) 0.004(2) C(30) 0.016(2) 0.026(3) 0.016(2) -0.006(2) 0.003(2) 0.002(2) C(31) 0.015(2) 0.015(2) 0.020(2) -0.002(2) 0.004(1) 0.005(2) C(32) 0.019(2) 0.011(2) 0.017(2) -0.005(2) 0.003(1) 0.005(2) C(33) 0.013(2) 0.020(2) 0.013(2) -0.001(2) -0.002(1) -0.002(2) C(34) 0.014(2) 0.023(2) 0.017(2) 0.002(2) 0.000(1) 0.006(2) C(35) 0.015(2) 0.027(3) 0.016(2) 0.006(2) -0.001(1) 0.004(2) C(36) 0.019(2) 0.021(2) 0.014(2) 0.004(2) 0.003(2) 0.003(2) C(37) 0.018(2) 0.019(2) 0.015(2) -0.002(2) 0.000(1) 0.001(2) C(38) 0.021(2) 0.023(2) 0.015(2) -0.002(2) -0.001(1) 0.001(2) C(39) 0.020(2) 0.030(3) 0.016(2) -0.008(2) 0.000(2) 0.000(2) C(40) 0.017(2) 0.035(3) 0.014(2) -0.006(2) 0.003(2) 0.005(2) C(41) 0.022(2) 0.019(2) 0.013(2) 0.003(2) -0.001(2) -0.001(2) C(42) 0.029(3) 0.018(2) 0.025(2) 0.009(2) 0.005(2) 0.001(2) C(43) 0.026(3) 0.025(2) 0.026(2) 0.012(2) 0.006(2) 0.009(2) C(44) 0.022(2) 0.024(3) 0.017(2) 0.002(2) 0.001(2) -0.004(2) C(45) 0.022(2) 0.030(3) 0.019(2) -0.003(2) -0.001(2) 0.007(2) C(46) 0.032(3) 0.020(2) 0.021(2) 0.002(2) -0.002(2) -0.003(2) C(47) 0.031(3) 0.018(2) 0.027(2) 0.006(2) -0.002(2) 0.003(2) C(48) 0.023(2) 0.016(2) 0.024(2) 0.004(2) 0.002(2) -0.004(2) C(49) 0.040(2) 0.030(3) 0.019(2) -0.005(2) -0.004(2) -0.007(2) C(50) 0.039(2) 0.027(3) 0.020(2) -0.013(2) -0.001(2) -0.006(2) C(51) 0.036(2) 0.034(3) 0.021(2) -0.017(2) 0.003(2) -0.006(2) C(52) 0.031(2) 0.027(3) 0.022(2) 0.003(2) 0.002(2) 0.000(2) C(53) 0.024(2) 0.025(3) 0.025(2) -0.004(2) 0.009(2) -0.003(2) C(54) 0.027(2) 0.022(3) 0.034(2) 0.003(2) -0.004(2) 0.000(2) C(55) 0.004(1) -0.007(1) -0.016(1) 0.002(1) -0.0113(9) 0.001(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(1) C(50) 1.729(8) . . yes Cl(2) C(51) 1.701(9) . . yes O(1) C(3) 1.446(9) . . yes O(2) C(7) 1.452(8) . . yes O(3) C(12) 1.447(8) . . yes O(4) C(24) 1.222(9) . . yes O(5) C(24) 1.326(9) . . yes O(6) C(27) 1.450(9) . . yes O(7) C(31) 1.452(8) . . yes O(8) C(36) 1.441(8) . . yes O(9) C(48) 1.218(9) . . yes O(10) C(48) 1.316(9) . . yes C(1) C(2) 1.52(1) . . yes C(1) C(10) 1.557(9) . . yes C(2) C(3) 1.507(9) . . yes C(3) C(4) 1.512(9) . . yes C(4) C(5) 1.551(10) . . yes C(5) C(6) 1.529(9) . . yes C(5) C(10) 1.543(8) . . yes C(6) C(7) 1.532(9) . . yes C(7) C(8) 1.543(9) . . yes C(8) C(9) 1.551(8) . . yes C(8) C(14) 1.495(9) . . yes C(9) C(10) 1.571(8) . . yes C(9) C(11) 1.529(8) . . yes C(10) C(19) 1.533(10) . . yes C(11) C(12) 1.539(8) . . yes C(12) C(13) 1.576(9) . . yes C(13) C(14) 1.547(8) . . yes C(13) C(17) 1.566(9) . . yes C(13) C(18) 1.528(10) . . yes C(14) C(15) 1.549(9) . . yes C(15) C(16) 1.563(10) . . yes C(16) C(17) 1.564(9) . . yes C(17) C(20) 1.527(9) . . yes C(20) C(21) 1.542(10) . . yes C(20) C(22) 1.561(9) . . yes C(22) C(23) 1.533(10) . . yes C(23) C(24) 1.510(10) . . yes C(25) C(26) 1.52(1) . . yes C(25) C(34) 1.550(9) . . yes C(26) C(27) 1.531(9) . . yes C(27) C(28) 1.543(9) . . yes C(28) C(29) 1.538(9) . . yes C(29) C(30) 1.564(9) . . yes C(29) C(34) 1.519(9) . . yes C(30) C(31) 1.534(9) . . yes C(31) C(32) 1.538(9) . . yes C(32) C(33) 1.565(8) . . yes C(32) C(38) 1.509(9) . . yes C(33) C(34) 1.566(9) . . yes C(33) C(35) 1.555(9) . . yes C(34) C(43) 1.527(10) . . yes C(35) C(36) 1.541(8) . . yes C(36) C(37) 1.541(9) . . yes C(37) C(38) 1.554(9) . . yes C(37) C(41) 1.573(9) . . yes C(37) C(42) 1.537(9) . . yes C(38) C(39) 1.543(9) . . yes C(39) C(40) 1.549(9) . . yes C(40) C(41) 1.551(9) . . yes C(41) C(44) 1.538(9) . . yes C(44) C(45) 1.545(9) . . yes C(44) C(46) 1.558(10) . . yes C(46) C(47) 1.546(10) . . yes C(47) C(48) 1.509(10) . . yes C(49) C(50) 1.38(1) . . yes C(49) C(54) 1.40(1) . . yes C(49) C(55) 1.646(9) . . yes C(50) C(51) 1.40(1) . . yes C(51) C(52) 1.41(1) . . yes C(52) C(53) 1.36(1) . . yes C(53) C(54) 1.43(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) C(1) C(10) 114.1(5) . 1_555 1_555 yes C(1) C(2) C(3) 110.0(5) . 1_555 1_555 yes O(1) C(3) C(2) 108.6(6) . 1_555 1_555 yes O(1) C(3) C(4) 111.0(5) . 1_555 1_555 yes C(2) C(3) C(4) 110.8(5) . 1_555 1_555 yes C(3) C(4) C(5) 112.4(5) . 1_555 1_555 yes C(4) C(5) C(6) 112.0(5) . 1_555 1_555 yes C(4) C(5) C(10) 112.6(5) . 1_555 1_555 yes C(6) C(5) C(10) 111.6(5) . 1_555 1_555 yes C(5) C(6) C(7) 115.0(5) . 1_555 1_555 yes O(2) C(7) C(6) 107.3(5) . 1_555 1_555 yes O(2) C(7) C(8) 110.9(5) . 1_555 1_555 yes C(6) C(7) C(8) 112.7(5) . 1_555 1_555 yes C(7) C(8) C(9) 111.7(5) . 1_555 1_555 yes C(7) C(8) C(14) 111.8(5) . 1_555 1_555 yes C(9) C(8) C(14) 110.0(5) . 1_555 1_555 yes C(8) C(9) C(10) 110.9(5) . 1_555 1_555 yes C(8) C(9) C(11) 111.6(5) . 1_555 1_555 yes C(10) C(9) C(11) 114.4(5) . 1_555 1_555 yes C(1) C(10) C(5) 108.4(5) . 1_555 1_555 yes C(1) C(10) C(9) 111.1(5) . 1_555 1_555 yes C(1) C(10) C(19) 105.8(5) . 1_555 1_555 yes C(5) C(10) C(9) 109.3(5) . 1_555 1_555 yes C(5) C(10) C(19) 110.3(5) . 1_555 1_555 yes C(9) C(10) C(19) 111.8(5) . 1_555 1_555 yes C(9) C(11) C(12) 113.5(5) . 1_555 1_555 yes O(3) C(12) C(11) 110.6(5) . 1_555 1_555 yes O(3) C(12) C(13) 110.0(5) . 1_555 1_555 yes C(11) C(12) C(13) 110.0(5) . 1_555 1_555 yes C(12) C(13) C(14) 106.2(5) . 1_555 1_555 yes C(12) C(13) C(17) 116.3(6) . 1_555 1_555 yes C(12) C(13) C(18) 109.7(5) . 1_555 1_555 yes C(14) C(13) C(17) 100.3(5) . 1_555 1_555 yes C(14) C(13) C(18) 114.1(6) . 1_555 1_555 yes C(17) C(13) C(18) 110.1(5) . 1_555 1_555 yes C(8) C(14) C(13) 115.4(5) . 1_555 1_555 yes C(8) C(14) C(15) 118.7(6) . 1_555 1_555 yes C(13) C(14) C(15) 103.8(5) . 1_555 1_555 yes C(14) C(15) C(16) 103.8(5) . 1_555 1_555 yes C(15) C(16) C(17) 106.8(5) . 1_555 1_555 yes C(13) C(17) C(16) 102.7(5) . 1_555 1_555 yes C(13) C(17) C(20) 119.9(5) . 1_555 1_555 yes C(16) C(17) C(20) 111.6(5) . 1_555 1_555 yes C(17) C(20) C(21) 113.4(6) . 1_555 1_555 yes C(17) C(20) C(22) 110.4(5) . 1_555 1_555 yes C(21) C(20) C(22) 110.6(6) . 1_555 1_555 yes C(20) C(22) C(23) 113.5(6) . 1_555 1_555 yes C(22) C(23) C(24) 111.0(6) . 1_555 1_555 yes O(4) C(24) O(5) 122.2(7) . 1_555 1_555 yes O(4) C(24) C(23) 123.8(7) . 1_555 1_555 yes O(5) C(24) C(23) 114.0(6) . 1_555 1_555 yes C(26) C(25) C(34) 114.9(6) . 1_555 1_555 yes C(25) C(26) C(27) 108.0(6) . 1_555 1_555 yes O(6) C(27) C(26) 107.9(6) . 1_555 1_555 yes O(6) C(27) C(28) 110.6(6) . 1_555 1_555 yes C(26) C(27) C(28) 109.6(5) . 1_555 1_555 yes C(27) C(28) C(29) 111.0(6) . 1_555 1_555 yes C(28) C(29) C(30) 110.3(5) . 1_555 1_555 yes C(28) C(29) C(34) 114.1(5) . 1_555 1_555 yes C(30) C(29) C(34) 111.8(5) . 1_555 1_555 yes C(29) C(30) C(31) 113.1(5) . 1_555 1_555 yes O(7) C(31) C(30) 108.2(5) . 1_555 1_555 yes O(7) C(31) C(32) 110.5(5) . 1_555 1_555 yes C(30) C(31) C(32) 113.4(5) . 1_555 1_555 yes C(31) C(32) C(33) 110.2(5) . 1_555 1_555 yes C(31) C(32) C(38) 112.3(5) . 1_555 1_555 yes C(33) C(32) C(38) 109.4(5) . 1_555 1_555 yes C(32) C(33) C(34) 111.4(5) . 1_555 1_555 yes C(32) C(33) C(35) 111.1(5) . 1_555 1_555 yes C(34) C(33) C(35) 113.8(5) . 1_555 1_555 yes C(25) C(34) C(29) 107.6(5) . 1_555 1_555 yes C(25) C(34) C(33) 111.1(5) . 1_555 1_555 yes C(25) C(34) C(43) 105.7(5) . 1_555 1_555 yes C(29) C(34) C(33) 109.2(5) . 1_555 1_555 yes C(29) C(34) C(43) 111.1(5) . 1_555 1_555 yes C(33) C(34) C(43) 112.1(6) . 1_555 1_555 yes C(33) C(35) C(36) 113.1(5) . 1_555 1_555 yes O(8) C(36) C(35) 110.6(5) . 1_555 1_555 yes O(8) C(36) C(37) 109.5(5) . 1_555 1_555 yes C(35) C(36) C(37) 110.4(5) . 1_555 1_555 yes C(36) C(37) C(38) 107.9(5) . 1_555 1_555 yes C(36) C(37) C(41) 117.5(5) . 1_555 1_555 yes C(36) C(37) C(42) 110.0(5) . 1_555 1_555 yes C(38) C(37) C(41) 98.1(5) . 1_555 1_555 yes C(38) C(37) C(42) 113.3(6) . 1_555 1_555 yes C(41) C(37) C(42) 109.6(5) . 1_555 1_555 yes C(32) C(38) C(37) 114.9(5) . 1_555 1_555 yes C(32) C(38) C(39) 117.7(6) . 1_555 1_555 yes C(37) C(38) C(39) 104.9(5) . 1_555 1_555 yes C(38) C(39) C(40) 103.0(5) . 1_555 1_555 yes C(39) C(40) C(41) 107.1(5) . 1_555 1_555 yes C(37) C(41) C(40) 104.3(5) . 1_555 1_555 yes C(37) C(41) C(44) 118.3(5) . 1_555 1_555 yes C(40) C(41) C(44) 112.0(5) . 1_555 1_555 yes C(41) C(44) C(45) 114.7(6) . 1_555 1_555 yes C(41) C(44) C(46) 110.9(5) . 1_555 1_555 yes C(45) C(44) C(46) 110.2(6) . 1_555 1_555 yes C(44) C(46) C(47) 113.1(6) . 1_555 1_555 yes C(46) C(47) C(48) 110.6(6) . 1_555 1_555 yes O(9) C(48) O(10) 123.1(6) . 1_555 1_555 yes O(9) C(48) C(47) 123.6(6) . 1_555 1_555 yes O(10) C(48) C(47) 113.3(6) . 1_555 1_555 yes C(50) C(49) C(54) 118.5(7) . 1_555 1_555 yes C(50) C(49) C(55) 121.0(6) . 1_555 1_555 yes C(54) C(49) C(55) 120.5(6) . 1_555 1_555 yes Cl(1) C(50) C(49) 120.1(6) . 1_555 1_555 yes Cl(1) C(50) C(51) 118.4(6) . 1_555 1_555 yes C(49) C(50) C(51) 121.5(7) . 1_555 1_555 yes Cl(2) C(51) C(50) 120.3(6) . 1_555 1_555 yes Cl(2) C(51) C(52) 120.6(7) . 1_555 1_555 yes C(50) C(51) C(52) 119.2(8) . 1_555 1_555 yes C(51) C(52) C(53) 120.8(7) . 1_555 1_555 yes C(52) C(53) C(54) 119.3(6) . 1_555 1_555 yes C(49) C(54) C(53) 120.7(6) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl(1) C(50) C(49) C(54) 178.8(6) 1_555 1_555 1_555 1_555 yes Cl(1) C(50) C(49) C(55) -1.3(9) 1_555 1_555 1_555 1_555 yes Cl(1) C(50) C(51) Cl(2) 1.2(9) 1_555 1_555 1_555 1_555 yes Cl(1) C(50) C(51) C(52) -179.8(6) 1_555 1_555 1_555 1_555 yes Cl(2) C(51) C(50) C(49) -179.9(6) 1_555 1_555 1_555 1_555 yes Cl(2) C(51) C(52) C(53) -179.2(6) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) -179.7(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 177.2(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -74.6(7) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 70.8(7) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -52.9(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 64.9(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -65.4(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 45.2(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 170.9(5) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -82.9(9) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 97.0(7) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(26) C(25) -179.5(5) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(28) C(29) 176.6(5) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(30) C(29) -73.6(6) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(33) 70.4(6) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(38) -51.8(7) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(35) C(33) 64.8(7) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(38) -65.5(6) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(41) 44.0(7) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(42) 170.4(5) 1_555 1_555 1_555 1_555 yes O(9) C(48) C(47) C(46) -75.7(9) 1_555 1_555 1_555 1_555 yes O(10) C(48) C(47) C(46) 104.1(7) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -57.5(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 50.2(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 177.2(6) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -178.5(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 54.2(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -53.6(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 66.5(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -171.9(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 56.4(7) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 57.9(7) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 179.4(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.8(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 75.7(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -71.0(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 165.7(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 47.8(8) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -58.9(7) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 173.8(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 56.0(7) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -67.3(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -49.5(8) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -173.2(6) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -51.6(8) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 55.9(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -175.3(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -178.2(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -54.0(8) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 63.5(7) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 52.7(7) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -59.9(8) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 178.7(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 61.1(8) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -162.5(6) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 57.1(8) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -178.7(6) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -56.8(7) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -179.4(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 179.7(6) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -50.6(7) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -63.8(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 56.7(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 167.2(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -67.0(6) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 168.4(6) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -156.3(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 79.3(8) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -32.7(7) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 22.9(7) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -59.4(8) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 175.8(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -42.4(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -166.8(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 5.6(7) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 47.0(7) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -70.7(7) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 152.6(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.2(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) -179.4(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 55.8(8) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) 55.5(8) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -46.2(8) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 173.4(6) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) -70.9(8) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -59.0(7) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(28) 51.3(7) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(30) 177.4(5) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(32) -178.4(5) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(35) 55.1(7) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(29) -55.0(7) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(33) 64.5(7) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(43) -173.7(5) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 57.7(8) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(34) 60.0(7) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 177.9(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(34) -55.3(7) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 75.7(7) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(33) -69.4(7) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(43) 166.5(6) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 49.4(8) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) -59.9(7) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(35) 173.6(6) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) 56.7(7) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) -67.4(7) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -51.2(7) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(38) -173.5(6) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) -52.4(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 56.6(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(35) -175.4(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(37) 179.3(6) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(39) -56.3(8) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) 63.6(7) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(35) C(36) 53.2(8) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(36) -59.4(7) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(41) 178.1(6) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(42) 62.6(7) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(39) C(40) -164.7(6) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(37) 56.7(7) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(39) -179.0(5) 1_555 1_555 1_555 1_555 yes C(33) C(35) C(36) C(37) -56.5(7) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(38) -179.4(5) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(35) C(36) 179.9(6) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(32) C(38) -51.4(7) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(34) C(43) -62.9(7) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 56.5(7) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(41) 166.1(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(42) -67.5(6) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) 169.7(6) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(40) -155.8(6) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(44) 78.9(8) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) -35.6(7) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(40) C(39) 20.5(7) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(45) -57.8(8) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(46) 176.6(6) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(40) -40.7(6) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(44) -166.0(6) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) 8.7(8) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(41) 47.3(6) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(42) -68.3(7) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(44) 149.7(6) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(37) C(42) 77.7(6) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(45) -179.3(6) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(46) 55.2(8) 1_555 1_555 1_555 1_555 yes C(41) C(44) C(46) C(47) 53.5(8) 1_555 1_555 1_555 1_555 yes C(42) C(37) C(41) C(44) -47.6(8) 1_555 1_555 1_555 1_555 yes C(44) C(46) C(47) C(48) 171.6(6) 1_555 1_555 1_555 1_555 yes C(45) C(44) C(46) C(47) -74.5(8) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) 0(1) 1_555 1_555 1_555 1_555 yes C(49) C(54) C(53) C(52) 0(1) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(54) C(53) 0(1) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) 1(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(54) 0(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(55) 179.9(6) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) -1(1) 1_555 1_555 1_555 1_555 yes C(53) C(54) C(49) C(55) -179.7(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(8) 2.676(7) . 2_546 ? O(1) O(4) 2.714(7) . 1_554 ? O(1) C(36) 3.347(8) . 2_546 ? O(2) C(48) 2.987(9) . 2_446 ? O(2) O(9) 3.128(8) . 2_446 ? O(2) C(47) 3.246(9) . 2_446 ? O(2) C(1) 3.322(8) . 1_455 ? O(2) O(10) 3.467(7) . 2_446 ? O(3) O(10) 2.657(7) . 2_446 ? O(3) O(6) 2.671(7) . 2_547 ? O(3) O(9) 3.390(7) . 2_446 ? O(3) C(48) 3.414(8) . 2_446 ? O(3) C(27) 3.526(9) . 2_547 ? O(4) O(7) 3.104(7) . 2_447 ? O(4) C(38) 3.364(9) . 2_447 ? O(4) O(8) 3.402(6) . 2_447 ? O(4) C(3) 3.484(8) . 1_556 ? O(4) C(4) 3.546(9) . 1_556 ? O(5) O(8) 2.666(7) . 2_447 ? O(5) O(7) 3.453(7) . 2_447 ? O(5) C(33) 3.556(9) . 2_447 ? O(6) O(9) 2.727(7) . 1_556 ? O(6) C(12) 3.388(9) . 2_557 ? O(7) C(24) 2.990(9) . 2_457 ? O(7) C(23) 3.308(9) . 2_457 ? O(7) C(25) 3.347(8) . 1_455 ? O(8) C(24) 3.439(9) . 2_457 ? O(8) C(3) 3.594(8) . 2_556 ? O(9) C(14) 3.377(9) . 2_456 ? O(9) C(27) 3.482(9) . 1_554 ? O(9) C(28) 3.550(9) . 1_554 ? O(10) C(9) 3.550(9) . 2_456 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_aburaya78_ _database_code_depnum_ccdc_archive 'CCDC 297674' _audit_creation_date 'Thu Apr 27 02:03:16 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C55 H86 Cl2 O10 ' _chemical_formula_moiety ? _chemical_formula_weight 978.18 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 7.453(1) _cell_length_b 25.368(4) _cell_length_c 13.763(2) _cell_angle_alpha 90 _cell_angle_beta 90.51(2) _cell_angle_gamma 90 _cell_volume 2602.0(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 27928 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 68.1 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.579 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.361 _exptl_absorpt_correction_T_max 0.729 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5419 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23961 _diffrn_reflns_av_R_equivalents 0.101 _diffrn_reflns_theta_max 68.16 _diffrn_measured_fraction_theta_max 0.9903 _diffrn_reflns_theta_full 68.16 _diffrn_measured_fraction_theta_full 0.9903 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # 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 4809 _reflns_number_gt 3878 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1660 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4809 _refine_ls_number_parameters 604 _refine_ls_goodness_of_fit_ref 1.197 _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 0.0004 _refine_diff_density_max 0.30 _refine_diff_density_min -0.31 _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 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.364 0.702 ;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 -0.9918(3) 0.0505(3) -1.3822(1) 0.0453(4) Uani 1.00 d . . . Cl(2) Cl -0.4992(2) -0.0737(3) -1.1994(1) 0.0412(4) Uani 1.00 d . . . O(1) O 0.0677(5) -0.2695(4) -0.9974(3) 0.032(1) Uani 1.00 d . . . O(2) O -0.3429(5) -0.1802(4) -0.7679(3) 0.0251(9) Uani 1.00 d . . . O(3) O 0.1129(5) -0.2254(4) -0.5659(3) 0.0238(9) Uani 1.00 d . . . O(4) O -0.2280(6) -0.2838(4) -0.1123(3) 0.035(1) Uani 1.00 d . . . O(5) O -0.4741(6) -0.2673(4) -0.2003(3) 0.0296(10) Uani 1.00 d . . . O(6) O -0.3971(6) 0.2217(4) -0.5011(3) 0.034(1) Uani 1.00 d . . . O(7) O -0.7875(5) 0.1264(4) -0.7329(3) 0.0256(10) Uani 1.00 d . . . O(8) O -0.3453(5) 0.1774(4) -0.9313(3) 0.0251(9) Uani 1.00 d . . . O(9) O -0.6912(6) 0.2300(4) -1.3868(3) 0.035(1) Uani 1.00 d . . . O(10) O -0.9403(6) 0.2182(4) -1.3003(3) 0.0307(10) Uani 1.00 d . . . C(1) C 0.2673(7) -0.1513(4) -0.8755(4) 0.027(1) Uani 1.00 d . . . C(2) C 0.2426(7) -0.2096(4) -0.9017(4) 0.027(1) Uani 1.00 d . . . C(3) C 0.0887(8) -0.2145(4) -0.9767(4) 0.028(1) Uani 1.00 d . . . C(4) C -0.0817(8) -0.1908(4) -0.9351(4) 0.027(1) Uani 1.00 d . . . C(5) C -0.0587(7) -0.1327(4) -0.9063(4) 0.023(1) Uani 1.00 d . . . C(6) C -0.2334(7) -0.1091(4) -0.8663(4) 0.026(1) Uani 1.00 d . . . C(7) C -0.2820(8) -0.1264(4) -0.7627(4) 0.026(1) Uani 1.00 d . . . C(8) C -0.1197(7) -0.1209(4) -0.6922(4) 0.021(1) Uani 1.00 d . . . C(9) C 0.0473(7) -0.1469(4) -0.7328(4) 0.023(1) Uani 1.00 d . . . C(10) C 0.1013(7) -0.1246(4) -0.8335(4) 0.024(1) Uani 1.00 d . . . C(11) C 0.2030(7) -0.1477(4) -0.6574(4) 0.026(1) Uani 1.00 d . . . C(12) C 0.1504(7) -0.1690(4) -0.5582(4) 0.022(1) Uani 1.00 d . . . C(13) C -0.0130(7) -0.1403(4) -0.5164(4) 0.021(1) Uani 1.00 d . . . C(14) C -0.1663(7) -0.1433(4) -0.5937(4) 0.021(1) Uani 1.00 d . . . C(15) C -0.3291(8) -0.1236(4) -0.5408(4) 0.025(1) Uani 1.00 d . . . C(16) C -0.3030(8) -0.1421(4) -0.4353(4) 0.029(1) Uani 1.00 d . . . C(17) C -0.1074(7) -0.1648(4) -0.4286(4) 0.025(1) Uani 1.00 d . . . C(18) C 0.0404(8) -0.0822(4) -0.4937(4) 0.027(1) Uani 1.00 d . . . C(19) C 0.1466(8) -0.0654(4) -0.8268(4) 0.029(1) Uani 1.00 d . . . C(20) C -0.0271(8) -0.1591(4) -0.3257(4) 0.024(1) Uani 1.00 d . . . C(21) C 0.1637(8) -0.1814(4) -0.3168(4) 0.031(1) Uani 1.00 d . . . C(22) C -0.1518(7) -0.1842(4) -0.2495(4) 0.024(1) Uani 1.00 d . . . C(23) C -0.1963(9) -0.2429(4) -0.2676(4) 0.032(2) Uani 1.00 d . . . C(24) C -0.3000(8) -0.2660(4) -0.1867(4) 0.026(1) Uani 1.00 d . . . C(25) C -0.1761(7) 0.1064(4) -0.6202(4) 0.026(1) Uani 1.00 d . . . C(26) C -0.2098(8) 0.1644(4) -0.5953(4) 0.027(1) Uani 1.00 d . . . C(27) C -0.3668(8) 0.1672(4) -0.5225(4) 0.026(1) Uani 1.00 d . . . C(28) C -0.5311(8) 0.1409(4) -0.5634(4) 0.028(1) Uani 1.00 d . . . C(29) C -0.4994(8) 0.0833(4) -0.5942(4) 0.026(1) Uani 1.00 d . . . C(30) C -0.6710(8) 0.0573(4) -0.6335(4) 0.025(1) Uani 1.00 d . . . C(31) C -0.7205(8) 0.0736(4) -0.7378(4) 0.025(1) Uani 1.00 d . . . C(32) C -0.5598(7) 0.0699(4) -0.8064(4) 0.023(1) Uani 1.00 d . . . C(33) C -0.3948(7) 0.0990(4) -0.7656(4) 0.023(1) Uani 1.00 d . . . C(34) C -0.3390(7) 0.0771(4) -0.6636(4) 0.023(1) Uani 1.00 d . . . C(35) C -0.2425(7) 0.1001(4) -0.8389(4) 0.027(1) Uani 1.00 d . . . C(36) C -0.2981(7) 0.1223(4) -0.9392(4) 0.023(1) Uani 1.00 d . . . C(37) C -0.4582(7) 0.0911(4) -0.9815(4) 0.023(1) Uani 1.00 d . . . C(38) C -0.6079(7) 0.0925(4) -0.9064(4) 0.020(1) Uani 1.00 d . . . C(39) C -0.7734(7) 0.0704(4) -0.9599(4) 0.027(1) Uani 1.00 d . . . C(40) C -0.7500(8) 0.0902(4) -1.0660(4) 0.028(1) Uani 1.00 d . . . C(41) C -0.5582(7) 0.1156(4) -1.0697(4) 0.024(1) Uani 1.00 d . . . C(42) C -0.3970(8) 0.0343(4) -1.0058(5) 0.030(1) Uani 1.00 d . . . C(43) C -0.2836(9) 0.0191(4) -0.6696(5) 0.033(2) Uani 1.00 d . . . C(44) C -0.4781(8) 0.1102(4) -1.1726(4) 0.026(1) Uani 1.00 d . . . C(45) C -0.2900(8) 0.1352(4) -1.1807(4) 0.030(1) Uani 1.00 d . . . C(46) C -0.6082(8) 0.1349(4) -1.2491(4) 0.028(1) Uani 1.00 d . . . C(47) C -0.6626(9) 0.1922(4) -1.2277(5) 0.033(2) Uani 1.00 d . . . C(48) C -0.7659(8) 0.2154(4) -1.3132(4) 0.027(1) Uani 1.00 d . . . C(49) C -0.7516(8) -0.0129(4) -1.2881(4) 0.027(1) Uani 1.00 d . . . C(50) C -0.9277(8) 0.0089(4) -1.2907(4) 0.026(1) Uani 1.00 d . . . C(51) C -1.0528(8) -0.0041(4) -1.2204(4) 0.032(1) Uani 1.00 d . . . C(52) C -1.0084(8) -0.0376(4) -1.1438(4) 0.030(1) Uani 1.00 d . . . C(53) C -0.8374(8) -0.0589(4) -1.1391(4) 0.028(1) Uani 1.00 d . . . C(54) C -0.7105(8) -0.0460(4) -1.2094(4) 0.026(1) Uani 1.00 d . . . C(55) C -0.6142(9) 0.0014(4) -1.3631(5) 0.038(2) Uani 1.00 d . . . H(1) H 0.3617 -0.1484 -0.8298 0.0318 Uiso 1.00 calc . . . H(2) H 0.2978 -0.1335 -0.9338 0.0318 Uiso 1.00 calc . . . H(3) H 0.3510 -0.2234 -0.9265 0.0324 Uiso 1.00 calc . . . H(4) H 0.2133 -0.2289 -0.8432 0.0324 Uiso 1.00 calc . . . H(5) H 0.1198 -0.1959 -1.0336 0.0327 Uiso 1.00 calc . . . H(6) H -0.1773 -0.1945 -0.9807 0.0315 Uiso 1.00 calc . . . H(7) H -0.1147 -0.2111 -0.8774 0.0315 Uiso 1.00 calc . . . H(8) H -0.0310 -0.1144 -0.9638 0.0251 Uiso 1.00 calc . . . H(9) H -0.2203 -0.0717 -0.8665 0.0286 Uiso 1.00 calc . . . H(10) H -0.3284 -0.1187 -0.9093 0.0286 Uiso 1.00 calc . . . H(11) H -0.3782 -0.1053 -0.7393 0.0288 Uiso 1.00 calc . . . H(12) H -0.0946 -0.0849 -0.6848 0.0231 Uiso 1.00 calc . . . H(13) H 0.0167 -0.1835 -0.7441 0.0268 Uiso 1.00 calc . . . H(14) H 0.2466 -0.1127 -0.6490 0.0298 Uiso 1.00 calc . . . H(15) H 0.2994 -0.1691 -0.6819 0.0298 Uiso 1.00 calc . . . H(16) H 0.2487 -0.1651 -0.5133 0.0251 Uiso 1.00 calc . . . H(17) H -0.1863 -0.1800 -0.6037 0.0232 Uiso 1.00 calc . . . H(18) H -0.4356 -0.1382 -0.5683 0.0296 Uiso 1.00 calc . . . H(19) H -0.3357 -0.0861 -0.5442 0.0296 Uiso 1.00 calc . . . H(20) H -0.3142 -0.1132 -0.3909 0.0353 Uiso 1.00 calc . . . H(21) H -0.3886 -0.1684 -0.4185 0.0353 Uiso 1.00 calc . . . H(22) H -0.1152 -0.2023 -0.4420 0.0287 Uiso 1.00 calc . . . H(23) H 0.1343 -0.0817 -0.4464 0.0344 Uiso 1.00 calc . . . H(24) H -0.0611 -0.0640 -0.4685 0.0344 Uiso 1.00 calc . . . H(25) H 0.0789 -0.0655 -0.5512 0.0344 Uiso 1.00 calc . . . H(26) H 0.2506 -0.0615 -0.7858 0.0346 Uiso 1.00 calc . . . H(27) H 0.0497 -0.0473 -0.8005 0.0346 Uiso 1.00 calc . . . H(28) H 0.1740 -0.0528 -0.8898 0.0346 Uiso 1.00 calc . . . H(29) H -0.0216 -0.1225 -0.3118 0.0283 Uiso 1.00 calc . . . H(30) H 0.1636 -0.2181 -0.3329 0.0377 Uiso 1.00 calc . . . H(31) H 0.2093 -0.1769 -0.2532 0.0377 Uiso 1.00 calc . . . H(32) H 0.2409 -0.1636 -0.3617 0.0377 Uiso 1.00 calc . . . H(33) H -0.0983 -0.1818 -0.1872 0.0285 Uiso 1.00 calc . . . H(34) H -0.2639 -0.1660 -0.2498 0.0285 Uiso 1.00 calc . . . H(35) H -0.2610 -0.2463 -0.3267 0.0397 Uiso 1.00 calc . . . H(36) H -0.0848 -0.2618 -0.2731 0.0397 Uiso 1.00 calc . . . H(37) H -0.0298 -0.2737 -1.0271 0.0529 Uiso 1.00 calc . . . H(38) H -0.4178 -0.1965 -0.7015 0.0529 Uiso 1.00 calc . . . H(39) H 0.2351 -0.2476 -0.5565 0.0529 Uiso 1.00 calc . . . H(40) H -0.5143 -0.2881 -0.1453 0.0529 Uiso 1.00 calc . . . H(41) H -0.0831 0.1047 -0.6661 0.0328 Uiso 1.00 calc . . . H(42) H -0.1423 0.0891 -0.5623 0.0328 Uiso 1.00 calc . . . H(43) H -0.2406 0.1832 -0.6539 0.0318 Uiso 1.00 calc . . . H(44) H -0.1041 0.1792 -0.5684 0.0318 Uiso 1.00 calc . . . H(45) H -0.3318 0.1497 -0.4642 0.0336 Uiso 1.00 calc . . . H(46) H -0.6222 0.1413 -0.5154 0.0333 Uiso 1.00 calc . . . H(47) H -0.5707 0.1599 -0.6188 0.0333 Uiso 1.00 calc . . . H(48) H -0.4677 0.0640 -0.5365 0.0326 Uiso 1.00 calc . . . H(49) H -0.6572 0.0200 -0.6320 0.0291 Uiso 1.00 calc . . . H(50) H -0.7681 0.0668 -0.5920 0.0291 Uiso 1.00 calc . . . H(51) H -0.8154 0.0512 -0.7619 0.0278 Uiso 1.00 calc . . . H(52) H -0.5290 0.0335 -0.8144 0.0254 Uiso 1.00 calc . . . H(53) H -0.4305 0.1344 -0.7558 0.0288 Uiso 1.00 calc . . . H(54) H -0.1997 0.0645 -0.8479 0.0320 Uiso 1.00 calc . . . H(55) H -0.1471 0.1208 -0.8142 0.0320 Uiso 1.00 calc . . . H(56) H -0.1994 0.1183 -0.9837 0.0261 Uiso 1.00 calc . . . H(57) H -0.6320 0.1289 -0.8967 0.0220 Uiso 1.00 calc . . . H(58) H -0.8824 0.0846 -0.9322 0.0322 Uiso 1.00 calc . . . H(59) H -0.7790 0.0331 -0.9555 0.0322 Uiso 1.00 calc . . . H(60) H -0.7556 0.0607 -1.1103 0.0324 Uiso 1.00 calc . . . H(61) H -0.8383 0.1149 -1.0838 0.0324 Uiso 1.00 calc . . . H(62) H -0.5722 0.1520 -1.0571 0.0280 Uiso 1.00 calc . . . H(63) H -0.4953 0.0144 -1.0317 0.0363 Uiso 1.00 calc . . . H(64) H -0.3045 0.0354 -1.0536 0.0363 Uiso 1.00 calc . . . H(65) H -0.3523 0.0174 -0.9493 0.0363 Uiso 1.00 calc . . . H(66) H -0.3766 -0.0016 -0.6961 0.0395 Uiso 1.00 calc . . . H(67) H -0.2509 0.0063 -0.6068 0.0395 Uiso 1.00 calc . . . H(68) H -0.1795 0.0161 -0.7108 0.0395 Uiso 1.00 calc . . . H(69) H -0.4680 0.0733 -1.1858 0.0306 Uiso 1.00 calc . . . H(70) H -0.2454 0.1299 -1.2456 0.0364 Uiso 1.00 calc . . . H(71) H -0.2947 0.1717 -1.1679 0.0364 Uiso 1.00 calc . . . H(72) H -0.2078 0.1187 -1.1365 0.0364 Uiso 1.00 calc . . . H(73) H -0.7151 0.1139 -1.2511 0.0331 Uiso 1.00 calc . . . H(74) H -0.5520 0.1334 -1.3105 0.0331 Uiso 1.00 calc . . . H(75) H -0.7324 0.1930 -1.1705 0.0373 Uiso 1.00 calc . . . H(76) H -0.5546 0.2121 -1.2164 0.0373 Uiso 1.00 calc . . . H(77) H -0.4937 0.2354 -0.4561 0.0529 Uiso 1.00 calc . . . H(78) H -0.8419 0.1414 -0.7902 0.0529 Uiso 1.00 calc . . . H(79) H -0.2491 0.1962 -0.9774 0.0529 Uiso 1.00 calc . . . H(80) H -1.0019 0.2496 -1.3517 0.0529 Uiso 1.00 calc . . . H(81) H -1.1711 0.0108 -1.2244 0.0366 Uiso 1.00 calc . . . H(82) H -1.0953 -0.0461 -1.0941 0.0348 Uiso 1.00 calc . . . H(83) H -0.8054 -0.0826 -1.0878 0.0347 Uiso 1.00 calc . . . H(84) H -0.5732 -0.0305 -1.3954 0.0467 Uiso 1.00 calc . . . H(85) H -0.6670 0.0235 -1.4112 0.0467 Uiso 1.00 calc . . . H(86) H -0.5149 0.0180 -1.3342 0.0467 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) 0.068(1) 0.0379(8) 0.0303(7) -0.0002(8) -0.0089(7) 0.0060(7) Cl(2) 0.0312(7) 0.0457(9) 0.0469(9) 0.0080(6) 0.0014(6) -0.0113(7) O(1) 0.023(2) 0.033(2) 0.041(2) 0.000(2) -0.001(2) -0.009(2) O(2) 0.018(2) 0.027(2) 0.030(2) -0.004(1) -0.002(2) 0.000(2) O(3) 0.019(2) 0.022(2) 0.030(2) -0.001(1) -0.004(2) 0.001(2) O(4) 0.035(2) 0.035(2) 0.036(2) -0.009(2) -0.008(2) 0.004(2) O(5) 0.034(2) 0.028(2) 0.027(2) -0.004(2) 0.000(2) 0.007(2) O(6) 0.030(2) 0.030(2) 0.041(2) -0.005(2) 0.004(2) -0.012(2) O(7) 0.023(2) 0.028(2) 0.026(2) 0.004(1) 0.002(2) 0.002(2) O(8) 0.026(2) 0.023(2) 0.026(2) -0.003(1) -0.001(2) -0.002(2) O(9) 0.036(2) 0.037(2) 0.031(2) 0.011(2) 0.007(2) 0.006(2) O(10) 0.033(2) 0.033(2) 0.026(2) 0.001(2) -0.001(2) 0.004(2) C(1) 0.022(3) 0.034(3) 0.026(3) 0.000(2) 0.001(2) 0.003(2) C(2) 0.021(3) 0.028(2) 0.030(3) 0.003(2) 0.002(2) -0.001(2) C(3) 0.026(3) 0.031(2) 0.028(3) 0.001(2) 0.003(2) 0.000(2) C(4) 0.026(3) 0.023(2) 0.033(3) 0.002(2) -0.002(2) -0.007(2) C(5) 0.022(2) 0.021(2) 0.027(3) 0.007(2) 0.000(2) 0.002(2) C(6) 0.023(3) 0.027(3) 0.028(3) 0.006(2) 0.001(2) -0.001(2) C(7) 0.025(3) 0.020(2) 0.031(3) 0.003(2) -0.001(2) 0.002(2) C(8) 0.024(2) 0.015(2) 0.024(2) 0.000(2) 0.001(2) -0.002(2) C(9) 0.021(2) 0.024(3) 0.024(2) -0.001(2) 0.004(2) 0.000(2) C(10) 0.023(2) 0.027(2) 0.023(2) 0.001(2) 0.001(2) 0.002(2) C(11) 0.023(3) 0.029(3) 0.025(3) -0.004(2) 0.001(2) 0.006(2) C(12) 0.020(2) 0.021(2) 0.025(2) -0.002(2) 0.005(2) -0.001(2) C(13) 0.024(2) 0.019(2) 0.021(2) 0.000(2) -0.002(2) -0.004(2) C(14) 0.020(2) 0.020(2) 0.022(2) -0.006(2) 0.000(2) -0.002(2) C(15) 0.026(3) 0.029(3) 0.020(2) 0.000(2) 0.001(2) -0.004(2) C(16) 0.026(2) 0.036(3) 0.025(3) -0.001(2) 0.001(2) 0.005(2) C(17) 0.027(3) 0.028(3) 0.021(2) 0.004(2) 0.002(2) -0.003(2) C(18) 0.037(3) 0.016(2) 0.027(3) -0.006(2) 0.001(2) 0.003(2) C(19) 0.033(3) 0.027(2) 0.025(3) -0.003(2) 0.005(2) 0.005(2) C(20) 0.031(3) 0.021(3) 0.021(2) -0.002(2) 0.002(2) 0.002(2) C(21) 0.031(3) 0.039(3) 0.024(3) -0.008(2) -0.009(2) 0.005(3) C(22) 0.025(3) 0.027(2) 0.021(3) -0.001(2) 0.001(2) 0.001(2) C(23) 0.047(4) 0.025(3) 0.026(3) -0.006(2) 0.008(2) -0.003(2) C(24) 0.035(2) 0.019(3) 0.024(2) -0.004(2) 0.003(2) -0.005(2) C(25) 0.017(2) 0.037(3) 0.026(3) 0.011(2) 0.003(2) 0.002(2) C(26) 0.022(3) 0.032(2) 0.027(3) -0.006(2) -0.001(2) 0.006(2) C(27) 0.022(2) 0.028(2) 0.028(3) 0.002(2) 0.000(2) 0.000(2) C(28) 0.031(3) 0.027(3) 0.024(3) -0.006(2) 0.000(2) -0.004(2) C(29) 0.028(2) 0.027(2) 0.025(3) 0.002(2) 0.005(2) 0.006(2) C(30) 0.032(3) 0.030(3) 0.012(2) -0.008(2) 0.007(2) -0.001(2) C(31) 0.028(3) 0.028(2) 0.019(2) 0.001(2) 0.000(2) 0.001(2) C(32) 0.025(2) 0.021(2) 0.022(2) 0.000(2) 0.002(2) 0.002(2) C(33) 0.027(3) 0.024(3) 0.018(2) 0.003(2) 0.002(2) 0.000(2) C(34) 0.022(2) 0.024(2) 0.024(2) 0.005(2) 0.001(2) 0.005(2) C(35) 0.020(3) 0.036(3) 0.023(2) 0.008(2) -0.001(2) 0.002(2) C(36) 0.021(3) 0.027(2) 0.022(2) 0.005(2) 0.002(2) 0.001(2) C(37) 0.026(3) 0.025(2) 0.017(2) 0.001(2) 0.002(2) 0.004(2) C(38) 0.017(2) 0.023(2) 0.020(2) -0.002(2) 0.004(2) -0.001(2) C(39) 0.019(3) 0.035(3) 0.027(2) -0.005(2) -0.005(2) -0.002(2) C(40) 0.032(3) 0.026(3) 0.026(3) -0.005(2) -0.003(2) 0.001(2) C(41) 0.025(2) 0.026(3) 0.022(2) 0.006(2) -0.004(2) 0.003(2) C(42) 0.034(3) 0.024(3) 0.031(3) 0.009(2) -0.002(2) -0.002(2) C(43) 0.041(3) 0.024(2) 0.032(3) 0.008(2) 0.000(3) 0.014(3) C(44) 0.039(3) 0.021(3) 0.018(2) 0.004(2) -0.002(2) -0.006(2) C(45) 0.034(3) 0.032(3) 0.026(3) 0.007(2) 0.002(2) 0.000(3) C(46) 0.042(3) 0.023(2) 0.018(3) 0.006(2) -0.007(2) -0.004(2) C(47) 0.048(4) 0.019(2) 0.030(3) 0.008(2) -0.009(3) 0.001(2) C(48) 0.032(2) 0.022(3) 0.026(2) 0.006(2) -0.002(2) -0.005(2) C(49) 0.031(2) 0.028(3) 0.023(2) 0.001(2) -0.002(2) -0.005(2) C(50) 0.033(2) 0.023(3) 0.023(2) 0.006(2) -0.005(2) -0.008(2) C(51) 0.035(3) 0.030(3) 0.029(3) 0.006(2) 0.003(2) 0.003(2) C(52) 0.033(3) 0.029(3) 0.028(3) 0.005(2) -0.001(2) 0.002(2) C(53) 0.029(2) 0.032(3) 0.023(3) 0.002(2) 0.001(2) 0.001(2) C(54) 0.032(2) 0.024(3) 0.022(2) -0.001(2) 0.000(2) -0.005(2) C(55) 0.042(4) 0.046(4) 0.027(3) -0.008(3) 0.007(2) 0.001(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(1) C(50) 1.708(6) . . yes Cl(2) C(54) 1.729(7) . . yes O(1) C(3) 1.433(8) . . yes O(2) C(7) 1.441(7) . . yes O(3) C(12) 1.459(7) . . yes O(4) C(24) 1.238(8) . . yes O(5) C(24) 1.310(8) . . yes O(6) C(27) 1.432(8) . . yes O(7) C(31) 1.431(8) . . yes O(8) C(36) 1.444(7) . . yes O(9) C(48) 1.219(8) . . yes O(10) C(48) 1.315(8) . . yes C(1) C(2) 1.533(9) . . yes C(1) C(10) 1.528(9) . . yes C(2) C(3) 1.542(9) . . yes C(3) C(4) 1.521(9) . . yes C(4) C(5) 1.535(8) . . yes C(5) C(6) 1.539(9) . . yes C(5) C(10) 1.564(8) . . yes C(6) C(7) 1.538(9) . . yes C(7) C(8) 1.551(8) . . yes C(8) C(9) 1.519(8) . . yes C(8) C(14) 1.513(8) . . yes C(9) C(10) 1.553(9) . . yes C(9) C(11) 1.550(8) . . yes C(10) C(19) 1.542(9) . . yes C(11) C(12) 1.523(8) . . yes C(12) C(13) 1.535(8) . . yes C(13) C(14) 1.557(7) . . yes C(13) C(17) 1.535(9) . . yes C(13) C(18) 1.557(8) . . yes C(14) C(15) 1.506(9) . . yes C(15) C(16) 1.537(9) . . yes C(16) C(17) 1.569(9) . . yes C(17) C(20) 1.540(8) . . yes C(20) C(21) 1.535(9) . . yes C(20) C(22) 1.544(8) . . yes C(22) C(23) 1.545(9) . . yes C(23) C(24) 1.482(9) . . yes C(25) C(26) 1.531(9) . . yes C(25) C(34) 1.539(9) . . yes C(26) C(27) 1.549(9) . . yes C(27) C(28) 1.501(8) . . yes C(28) C(29) 1.540(9) . . yes C(29) C(30) 1.532(9) . . yes C(29) C(34) 1.545(9) . . yes C(30) C(31) 1.535(8) . . yes C(31) C(32) 1.535(9) . . yes C(32) C(33) 1.537(8) . . yes C(32) C(38) 1.530(8) . . yes C(33) C(34) 1.562(8) . . yes C(33) C(35) 1.526(9) . . yes C(34) C(43) 1.531(8) . . yes C(35) C(36) 1.544(8) . . yes C(36) C(37) 1.543(8) . . yes C(37) C(38) 1.528(8) . . yes C(37) C(41) 1.549(8) . . yes C(37) C(42) 1.549(9) . . yes C(38) C(39) 1.536(8) . . yes C(39) C(40) 1.555(9) . . yes C(40) C(41) 1.570(9) . . yes C(41) C(44) 1.547(9) . . yes C(44) C(45) 1.543(10) . . yes C(44) C(46) 1.557(8) . . yes C(46) C(47) 1.539(9) . . yes C(47) C(48) 1.518(9) . . yes C(49) C(50) 1.424(9) . . yes C(49) C(54) 1.403(9) . . yes C(49) C(55) 1.505(10) . . yes C(50) C(51) 1.389(10) . . yes C(51) C(52) 1.392(9) . . yes C(52) C(53) 1.385(9) . . yes C(53) C(54) 1.398(9) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) C(1) C(10) 114.9(5) . 1_555 1_555 yes C(1) C(2) C(3) 108.7(5) . 1_555 1_555 yes O(1) C(3) C(2) 106.9(5) . 1_555 1_555 yes O(1) C(3) C(4) 111.7(5) . 1_555 1_555 yes C(2) C(3) C(4) 109.5(5) . 1_555 1_555 yes C(3) C(4) C(5) 112.7(5) . 1_555 1_555 yes C(4) C(5) C(6) 111.9(5) . 1_555 1_555 yes C(4) C(5) C(10) 112.0(5) . 1_555 1_555 yes C(6) C(5) C(10) 111.3(5) . 1_555 1_555 yes C(5) C(6) C(7) 115.3(5) . 1_555 1_555 yes O(2) C(7) C(6) 107.5(5) . 1_555 1_555 yes O(2) C(7) C(8) 111.1(5) . 1_555 1_555 yes C(6) C(7) C(8) 111.5(5) . 1_555 1_555 yes C(7) C(8) C(9) 111.6(5) . 1_555 1_555 yes C(7) C(8) C(14) 110.1(5) . 1_555 1_555 yes C(9) C(8) C(14) 111.3(5) . 1_555 1_555 yes C(8) C(9) C(10) 113.0(5) . 1_555 1_555 yes C(8) C(9) C(11) 111.8(5) . 1_555 1_555 yes C(10) C(9) C(11) 113.9(5) . 1_555 1_555 yes C(1) C(10) C(5) 108.3(5) . 1_555 1_555 yes C(1) C(10) C(9) 113.2(5) . 1_555 1_555 yes C(1) C(10) C(19) 106.1(5) . 1_555 1_555 yes C(5) C(10) C(9) 108.8(5) . 1_555 1_555 yes C(5) C(10) C(19) 109.3(5) . 1_555 1_555 yes C(9) C(10) C(19) 111.0(5) . 1_555 1_555 yes C(9) C(11) C(12) 114.1(5) . 1_555 1_555 yes O(3) C(12) C(11) 109.5(5) . 1_555 1_555 yes O(3) C(12) C(13) 109.9(5) . 1_555 1_555 yes C(11) C(12) C(13) 112.3(5) . 1_555 1_555 yes C(12) C(13) C(14) 107.5(5) . 1_555 1_555 yes C(12) C(13) C(17) 118.3(5) . 1_555 1_555 yes C(12) C(13) C(18) 108.8(5) . 1_555 1_555 yes C(14) C(13) C(17) 100.3(5) . 1_555 1_555 yes C(14) C(13) C(18) 111.6(5) . 1_555 1_555 yes C(17) C(13) C(18) 110.1(5) . 1_555 1_555 yes C(8) C(14) C(13) 114.9(5) . 1_555 1_555 yes C(8) C(14) C(15) 120.1(5) . 1_555 1_555 yes C(13) C(14) C(15) 104.1(5) . 1_555 1_555 yes C(14) C(15) C(16) 105.0(5) . 1_555 1_555 yes C(15) C(16) C(17) 106.1(5) . 1_555 1_555 yes C(13) C(17) C(16) 103.8(5) . 1_555 1_555 yes C(13) C(17) C(20) 120.6(5) . 1_555 1_555 yes C(16) C(17) C(20) 111.9(5) . 1_555 1_555 yes C(17) C(20) C(21) 113.0(5) . 1_555 1_555 yes C(17) C(20) C(22) 110.8(5) . 1_555 1_555 yes C(21) C(20) C(22) 110.9(5) . 1_555 1_555 yes C(20) C(22) C(23) 114.7(5) . 1_555 1_555 yes C(22) C(23) C(24) 111.9(5) . 1_555 1_555 yes O(4) C(24) O(5) 122.1(6) . 1_555 1_555 yes O(4) C(24) C(23) 122.7(6) . 1_555 1_555 yes O(5) C(24) C(23) 115.2(6) . 1_555 1_555 yes C(26) C(25) C(34) 114.8(5) . 1_555 1_555 yes C(25) C(26) C(27) 108.4(5) . 1_555 1_555 yes O(6) C(27) C(26) 107.4(5) . 1_555 1_555 yes O(6) C(27) C(28) 112.2(5) . 1_555 1_555 yes C(26) C(27) C(28) 110.8(5) . 1_555 1_555 yes C(27) C(28) C(29) 113.5(5) . 1_555 1_555 yes C(28) C(29) C(30) 112.0(5) . 1_555 1_555 yes C(28) C(29) C(34) 112.8(5) . 1_555 1_555 yes C(30) C(29) C(34) 112.7(5) . 1_555 1_555 yes C(29) C(30) C(31) 114.0(5) . 1_555 1_555 yes O(7) C(31) C(30) 106.9(5) . 1_555 1_555 yes O(7) C(31) C(32) 111.2(5) . 1_555 1_555 yes C(30) C(31) C(32) 112.1(5) . 1_555 1_555 yes C(31) C(32) C(33) 111.7(5) . 1_555 1_555 yes C(31) C(32) C(38) 110.6(5) . 1_555 1_555 yes C(33) C(32) C(38) 109.2(5) . 1_555 1_555 yes C(32) C(33) C(34) 111.3(5) . 1_555 1_555 yes C(32) C(33) C(35) 111.3(5) . 1_555 1_555 yes C(34) C(33) C(35) 114.0(5) . 1_555 1_555 yes C(25) C(34) C(29) 108.9(5) . 1_555 1_555 yes C(25) C(34) C(33) 112.4(5) . 1_555 1_555 yes C(25) C(34) C(43) 105.8(5) . 1_555 1_555 yes C(29) C(34) C(33) 108.6(5) . 1_555 1_555 yes C(29) C(34) C(43) 109.9(5) . 1_555 1_555 yes C(33) C(34) C(43) 111.3(5) . 1_555 1_555 yes C(33) C(35) C(36) 113.7(5) . 1_555 1_555 yes O(8) C(36) C(35) 110.5(5) . 1_555 1_555 yes O(8) C(36) C(37) 109.7(5) . 1_555 1_555 yes C(35) C(36) C(37) 110.5(5) . 1_555 1_555 yes C(36) C(37) C(38) 107.5(5) . 1_555 1_555 yes C(36) C(37) C(41) 117.0(5) . 1_555 1_555 yes C(36) C(37) C(42) 109.3(5) . 1_555 1_555 yes C(38) C(37) C(41) 99.9(5) . 1_555 1_555 yes C(38) C(37) C(42) 112.6(5) . 1_555 1_555 yes C(41) C(37) C(42) 110.2(5) . 1_555 1_555 yes C(32) C(38) C(37) 115.7(5) . 1_555 1_555 yes C(32) C(38) C(39) 118.4(5) . 1_555 1_555 yes C(37) C(38) C(39) 104.8(5) . 1_555 1_555 yes C(38) C(39) C(40) 103.7(5) . 1_555 1_555 yes C(39) C(40) C(41) 105.8(5) . 1_555 1_555 yes C(37) C(41) C(40) 104.0(5) . 1_555 1_555 yes C(37) C(41) C(44) 119.6(5) . 1_555 1_555 yes C(40) C(41) C(44) 110.6(5) . 1_555 1_555 yes C(41) C(44) C(45) 112.8(5) . 1_555 1_555 yes C(41) C(44) C(46) 109.9(5) . 1_555 1_555 yes C(45) C(44) C(46) 110.3(5) . 1_555 1_555 yes C(44) C(46) C(47) 114.5(5) . 1_555 1_555 yes C(46) C(47) C(48) 110.5(5) . 1_555 1_555 yes O(9) C(48) O(10) 123.7(6) . 1_555 1_555 yes O(9) C(48) C(47) 122.0(6) . 1_555 1_555 yes O(10) C(48) C(47) 114.4(6) . 1_555 1_555 yes C(50) C(49) C(54) 116.5(6) . 1_555 1_555 yes C(50) C(49) C(55) 121.5(6) . 1_555 1_555 yes C(54) C(49) C(55) 121.9(6) . 1_555 1_555 yes Cl(1) C(50) C(49) 120.6(5) . 1_555 1_555 yes Cl(1) C(50) C(51) 118.4(5) . 1_555 1_555 yes C(49) C(50) C(51) 121.0(6) . 1_555 1_555 yes C(50) C(51) C(52) 121.0(6) . 1_555 1_555 yes C(51) C(52) C(53) 119.1(6) . 1_555 1_555 yes C(52) C(53) C(54) 120.3(6) . 1_555 1_555 yes Cl(2) C(54) C(49) 119.8(5) . 1_555 1_555 yes Cl(2) C(54) C(53) 118.1(5) . 1_555 1_555 yes C(49) C(54) C(53) 122.0(6) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl(1) C(50) C(49) C(54) 179.1(5) 1_555 1_555 1_555 1_555 yes Cl(1) C(50) C(49) C(55) 2.3(8) 1_555 1_555 1_555 1_555 yes Cl(1) C(50) C(51) C(52) -179.8(5) 1_555 1_555 1_555 1_555 yes Cl(2) C(54) C(49) C(50) -179.3(4) 1_555 1_555 1_555 1_555 yes Cl(2) C(54) C(49) C(55) -2.6(8) 1_555 1_555 1_555 1_555 yes Cl(2) C(54) C(53) C(52) 179.8(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) -178.8(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 176.3(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -73.2(6) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 69.6(6) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -54.5(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 68.7(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -67.9(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 44.7(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 171.2(5) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -84.4(8) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 96.8(6) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(26) C(25) -179.4(5) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(28) C(29) 175.8(5) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(30) C(29) -73.6(6) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(33) 68.1(6) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(38) -53.8(6) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(35) C(33) 65.4(7) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(38) -66.8(6) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(41) 44.5(7) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(42) 170.6(5) 1_555 1_555 1_555 1_555 yes O(9) C(48) C(47) C(46) -77.0(8) 1_555 1_555 1_555 1_555 yes O(10) C(48) C(47) C(46) 103.3(7) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -57.5(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 51.2(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 177.3(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -178.9(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 52.1(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -54.7(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 66.1(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -171.9(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 58.1(7) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 58.7(7) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 178.8(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -55.4(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 74.8(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -72.3(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 166.3(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 48.7(7) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -58.4(6) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 172.6(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 53.8(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -67.6(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -50.3(6) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -174.3(5) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -51.4(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 57.2(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -172.8(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) 179.7(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -54.9(7) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 61.9(6) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 49.9(7) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -56.8(6) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 179.0(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 62.4(7) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -164.0(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 55.4(6) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -179.2(5) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -53.6(7) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -179.4(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 179.5(5) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -49.4(6) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -67.0(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 54.2(6) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 166.7(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -66.8(6) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 169.9(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -155.5(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 78.2(7) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -33.6(6) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 19.7(6) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -58.1(7) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 176.7(5) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -39.1(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -165.4(5) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 8.7(6) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 45.6(5) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -71.0(6) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 151.3(5) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.6(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 179.5(5) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 54.3(7) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) 56.6(7) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -47.7(7) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 173.9(5) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) -69.8(7) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -56.5(7) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(28) 49.5(7) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(30) 177.6(5) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(32) -178.9(5) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(35) 54.1(7) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(29) -54.4(7) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(33) 65.9(7) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(43) -172.5(5) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 55.7(7) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(34) 58.0(7) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 178.7(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(34) -52.8(7) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 77.2(7) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(33) -73.2(6) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(43) 164.9(5) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 48.4(7) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) -58.4(6) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(35) 174.6(5) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) 55.0(6) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) -67.0(7) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -51.5(7) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(38) -173.4(5) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) -51.3(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 57.7(6) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(35) -173.9(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(37) 179.8(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(39) -54.6(7) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) 62.6(7) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(35) C(36) 53.7(7) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(36) -58.3(6) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(41) 179.1(5) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(42) 62.2(7) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(39) C(40) -164.9(5) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(37) 56.4(7) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(39) -178.0(5) 1_555 1_555 1_555 1_555 yes C(33) C(35) C(36) C(37) -56.1(7) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(38) -179.6(5) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(35) C(36) -179.3(5) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(32) C(38) -51.2(6) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(34) C(43) -64.3(7) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 55.2(6) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(41) 166.5(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(42) -67.3(6) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) 169.4(5) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(40) -156.2(5) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(44) 79.8(7) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) -34.2(6) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(40) C(39) 20.6(6) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(45) -60.0(7) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(46) 176.5(5) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(40) -40.7(6) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(44) -164.7(5) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) 7.8(6) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(41) 46.8(6) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(42) -70.1(6) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(44) 150.3(5) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(37) C(42) 78.1(6) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(45) 179.3(5) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(46) 55.8(6) 1_555 1_555 1_555 1_555 yes C(41) C(44) C(46) C(47) 53.9(8) 1_555 1_555 1_555 1_555 yes C(42) C(37) C(41) C(44) -45.9(7) 1_555 1_555 1_555 1_555 yes C(44) C(46) C(47) C(48) 171.5(6) 1_555 1_555 1_555 1_555 yes C(45) C(44) C(46) C(47) -71.1(7) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) 1.7(10) 1_555 1_555 1_555 1_555 yes C(49) C(54) C(53) C(52) -2.1(10) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(54) C(53) 2.6(9) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) -1(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(54) -2.4(9) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(55) -179.2(6) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) 1.2(10) 1_555 1_555 1_555 1_555 yes C(53) C(54) C(49) C(55) 179.4(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(8) 2.664(6) . 2_543 ? O(1) O(4) 2.724(6) . 1_554 ? O(1) C(36) 3.355(8) . 2_543 ? O(2) C(48) 2.984(7) . 2_443 ? O(2) O(9) 3.126(7) . 2_443 ? O(2) C(47) 3.236(8) . 2_443 ? O(2) C(1) 3.331(7) . 1_455 ? O(2) O(10) 3.455(6) . 2_443 ? O(3) O(10) 2.655(6) . 2_443 ? O(3) O(6) 2.665(6) . 2_544 ? O(3) O(9) 3.398(6) . 2_443 ? O(3) C(48) 3.412(7) . 2_443 ? O(3) C(27) 3.528(8) . 2_544 ? O(4) O(7) 3.122(7) . 2_444 ? O(4) C(38) 3.380(8) . 2_444 ? O(4) O(8) 3.388(6) . 2_444 ? O(4) C(3) 3.473(8) . 1_556 ? O(4) C(4) 3.557(8) . 1_556 ? O(5) O(8) 2.665(6) . 2_444 ? O(5) O(7) 3.455(6) . 2_444 ? O(5) C(33) 3.558(7) . 2_444 ? O(6) O(9) 2.717(7) . 1_556 ? O(6) C(12) 3.420(7) . 2_554 ? O(7) C(24) 3.017(7) . 2_454 ? O(7) C(23) 3.316(8) . 2_454 ? O(7) C(25) 3.337(8) . 1_455 ? O(8) C(24) 3.430(8) . 2_454 ? O(8) C(3) 3.582(8) . 2_553 ? O(9) C(14) 3.394(7) . 2_453 ? O(9) C(27) 3.457(8) . 1_554 ? O(9) C(28) 3.535(8) . 1_554 ? O(10) C(9) 3.544(8) . 2_453 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_aburaya84_ _database_code_depnum_ccdc_archive 'CCDC 297675' _audit_creation_date 'Thu Apr 27 10:58:34 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C56 H89 Br O10 ' _chemical_formula_moiety ? _chemical_formula_weight 1002.22 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 7.475(2) _cell_length_b 25.385(7) _cell_length_c 13.809(4) _cell_angle_alpha 90 _cell_angle_beta 90.67(2) _cell_angle_gamma 90 _cell_volume 2620(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 17435 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 68.2 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.400 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.523 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.212 _exptl_absorpt_correction_T_max 0.544 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5419 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15356 _diffrn_reflns_av_R_equivalents 0.115 _diffrn_reflns_theta_max 68.21 _diffrn_measured_fraction_theta_max 0.9071 _diffrn_reflns_theta_full 68.21 _diffrn_measured_fraction_theta_full 0.9071 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 1.5 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 4436 _reflns_number_gt 3994 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0924 _refine_ls_wR_factor_ref 0.2567 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4147 _refine_ls_number_parameters 604 _refine_ls_goodness_of_fit_ref 2.594 _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 0.73 _refine_diff_density_min -0.49 _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 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br Br -0.676 1.280 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.049 0.032 ;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 Br(1) Br -1.4944(2) 0.5237(4) -0.1951(1) 0.0509(4) Uani 0.50 d P . . Br(2) Br -1.9932(2) 0.6533(4) -0.38466(10) 0.0471(4) Uani 0.50 d P . . O(1) O -1.3981(6) 0.8212(4) 0.4996(4) 0.042(1) Uani 1.00 d . . . O(2) O -1.7923(5) 0.7266(4) 0.2662(3) 0.033(1) Uani 1.00 d . . . O(3) O -1.3478(5) 0.7785(4) 0.0696(3) 0.0309(9) Uani 1.00 d . . . O(4) O -1.6917(7) 0.8299(4) -0.3848(3) 0.044(1) Uani 1.00 d . . . O(5) O -1.9398(6) 0.8188(4) -0.3005(3) 0.040(1) Uani 1.00 d . . . O(6) O -0.9305(6) 0.3309(4) 0.0020(3) 0.043(1) Uani 1.00 d . . . O(7) O -1.3396(5) 0.4202(4) 0.2311(3) 0.0330(10) Uani 1.00 d . . . O(8) O -0.8839(6) 0.3750(4) 0.4335(3) 0.0331(10) Uani 1.00 d . . . O(9) O -1.2249(6) 0.3164(4) 0.8867(4) 0.045(1) Uani 1.00 d . . . O(10) O -1.4702(6) 0.3333(4) 0.7992(3) 0.040(1) Uani 1.00 d . . . C(1) C -1.1776(9) 0.7078(5) 0.3815(5) 0.039(1) Uani 1.00 d . . . C(2) C -1.2147(8) 0.7648(5) 0.4052(4) 0.036(1) Uani 1.00 d . . . C(3) C -1.3657(8) 0.7662(5) 0.4776(5) 0.039(1) Uani 1.00 d . . . C(4) C -1.5306(8) 0.7407(4) 0.4360(4) 0.031(1) Uani 1.00 d . . . C(5) C -1.5005(8) 0.6828(4) 0.4064(4) 0.035(1) Uani 1.00 d . . . C(6) C -1.6714(8) 0.6575(4) 0.3641(4) 0.036(1) Uani 1.00 d . . . C(7) C -1.7241(8) 0.6738(4) 0.2631(4) 0.031(1) Uani 1.00 d . . . C(8) C -1.5614(8) 0.6701(4) 0.1925(4) 0.033(1) Uani 1.00 d . . . C(9) C -1.3967(8) 0.6996(4) 0.2359(5) 0.035(1) Uani 1.00 d . . . C(10) C -1.3424(9) 0.6773(4) 0.3366(4) 0.034(1) Uani 1.00 d . . . C(11) C -1.2435(8) 0.7021(4) 0.1607(5) 0.035(1) Uani 1.00 d . . . C(12) C -1.3020(8) 0.7225(4) 0.0618(4) 0.033(1) Uani 1.00 d . . . C(13) C -1.4585(8) 0.6918(4) 0.0198(4) 0.030(1) Uani 1.00 d . . . C(14) C -1.6121(8) 0.6940(4) 0.0955(4) 0.029(1) Uani 1.00 d . . . C(15) C -1.7718(8) 0.6708(4) 0.0399(4) 0.037(1) Uani 1.00 d . . . C(16) C -1.7475(9) 0.6912(4) -0.0644(4) 0.036(1) Uani 1.00 d . . . C(17) C -1.5591(9) 0.7164(5) -0.0699(4) 0.037(1) Uani 1.00 d . . . C(18) C -1.3992(9) 0.6360(4) -0.0055(5) 0.037(1) Uani 1.00 d . . . C(19) C -1.283(1) 0.6198(5) 0.3291(5) 0.046(2) Uani 1.00 d . . . C(20) C -1.4767(8) 0.7124(4) -0.1701(4) 0.035(1) Uani 1.00 d . . . C(21) C -1.2920(9) 0.7376(5) -0.1792(4) 0.038(1) Uani 1.00 d . . . C(22) C -1.6088(8) 0.7345(4) -0.2488(4) 0.029(1) Uani 1.00 d . . . C(23) C -1.6613(10) 0.7928(4) -0.2285(5) 0.040(2) Uani 1.00 d . . . C(24) C -1.7643(9) 0.8149(4) -0.3126(4) 0.034(1) Uani 1.00 d . . . C(25) C -0.7317(8) 0.4498(4) 0.1257(4) 0.033(1) Uani 1.00 d . . . C(26) C -0.7586(8) 0.3916(4) 0.0973(5) 0.038(1) Uani 1.00 d . . . C(27) C -0.9089(8) 0.3855(4) 0.0254(4) 0.033(1) Uani 1.00 d . . . C(28) C -1.0798(8) 0.4103(4) 0.0652(5) 0.036(1) Uani 1.00 d . . . C(29) C -1.0572(8) 0.4677(4) 0.0950(4) 0.031(1) Uani 1.00 d . . . C(30) C -1.2320(8) 0.4915(4) 0.1337(4) 0.033(1) Uani 1.00 d . . . C(31) C -1.2761(7) 0.4735(4) 0.2373(4) 0.031(1) Uani 1.00 d . . . C(32) C -1.1181(7) 0.4800(4) 0.3092(4) 0.028(1) Uani 1.00 d . . . C(33) C -0.9505(7) 0.4541(4) 0.2660(5) 0.032(1) Uani 1.00 d . . . C(34) C -0.9033(8) 0.4767(4) 0.1671(4) 0.030(1) Uani 1.00 d . . . C(35) C -0.7967(8) 0.4534(4) 0.3414(4) 0.036(1) Uani 1.00 d . . . C(36) C -0.8461(7) 0.4302(4) 0.4415(4) 0.029(1) Uani 1.00 d . . . C(37) C -1.0093(8) 0.4596(4) 0.4836(5) 0.033(1) Uani 1.00 d . . . C(38) C -1.1616(7) 0.4558(4) 0.4060(4) 0.029(1) Uani 1.00 d . . . C(39) C -1.3266(8) 0.4763(4) 0.4603(4) 0.036(1) Uani 1.00 d . . . C(40) C -1.2981(10) 0.4574(5) 0.5657(5) 0.045(2) Uani 1.00 d . . . C(41) C -1.1054(9) 0.4341(4) 0.5704(4) 0.037(1) Uani 1.00 d . . . C(42) C -0.9601(8) 0.5173(4) 0.5061(5) 0.036(1) Uani 1.00 d . . . C(43) C -0.8510(8) 0.5351(4) 0.1726(5) 0.035(1) Uani 1.00 d . . . C(44) C -1.0237(9) 0.4407(4) 0.6733(4) 0.033(1) Uani 1.00 d . . . C(45) C -0.8326(9) 0.4183(5) 0.6811(5) 0.041(2) Uani 1.00 d . . . C(46) C -1.1459(9) 0.4154(4) 0.7486(4) 0.032(1) Uani 1.00 d . . . C(47) C -1.194(1) 0.3575(4) 0.7293(5) 0.044(2) Uani 1.00 d . . . C(48) C -1.2960(9) 0.3347(4) 0.8102(5) 0.039(1) Uani 1.00 d . . . C(49) C -1.7167(10) 0.5546(5) -0.2042(4) 0.042(1) Uani 1.00 d . . . C(50) C -1.756(1) 0.5880(5) -0.2838(5) 0.045(2) Uani 1.00 d . . . C(51) C -1.924(1) 0.6100(5) -0.2896(5) 0.048(2) Uani 1.00 d . . . C(52) C -2.0511(9) 0.5971(5) -0.2188(6) 0.045(2) Uani 1.00 d . . . C(53) C -2.010(1) 0.5643(5) -0.1427(6) 0.050(2) Uani 1.00 d . . . C(54) C -1.846(1) 0.5427(5) -0.1377(5) 0.042(1) Uani 1.00 d . . . C(55) C -1.616(1) 0.6007(5) -0.3603(5) 0.062(2) Uani 1.00 d . . . H(1) H -1.0825 0.7057 0.3364 0.0466 Uiso 1.00 calc . . . H(2) H -1.1415 0.6895 0.4395 0.0466 Uiso 1.00 calc . . . H(3) H -1.1102 0.7795 0.4325 0.0437 Uiso 1.00 calc . . . H(4) H -1.2484 0.7821 0.3479 0.0437 Uiso 1.00 calc . . . H(5) H -1.3303 0.7470 0.5350 0.0469 Uiso 1.00 calc . . . H(6) H -1.6218 0.7409 0.4831 0.0367 Uiso 1.00 calc . . . H(7) H -1.5671 0.7590 0.3803 0.0367 Uiso 1.00 calc . . . H(8) H -1.4701 0.6628 0.4636 0.0424 Uiso 1.00 calc . . . H(9) H -1.6538 0.6193 0.3639 0.0436 Uiso 1.00 calc . . . H(10) H -1.7672 0.6649 0.4058 0.0436 Uiso 1.00 calc . . . H(11) H -1.8160 0.6501 0.2402 0.0379 Uiso 1.00 calc . . . H(12) H -1.5315 0.6331 0.1835 0.0396 Uiso 1.00 calc . . . H(13) H -1.4334 0.7339 0.2462 0.0420 Uiso 1.00 calc . . . H(14) H -1.1968 0.6667 0.1526 0.0420 Uiso 1.00 calc . . . H(15) H -1.1531 0.7238 0.1850 0.0420 Uiso 1.00 calc . . . H(16) H -1.2039 0.7180 0.0193 0.0386 Uiso 1.00 calc . . . H(17) H -1.6374 0.7291 0.1065 0.0345 Uiso 1.00 calc . . . H(18) H -1.7697 0.6324 0.0419 0.0439 Uiso 1.00 calc . . . H(19) H -1.8815 0.6820 0.0660 0.0439 Uiso 1.00 calc . . . H(20) H -1.7559 0.6617 -0.1091 0.0441 Uiso 1.00 calc . . . H(21) H -1.8361 0.7156 -0.0797 0.0441 Uiso 1.00 calc . . . H(22) H -1.5737 0.7519 -0.0569 0.0449 Uiso 1.00 calc . . . H(23) H -1.3061 0.6364 -0.0515 0.0451 Uiso 1.00 calc . . . H(24) H -1.3571 0.6178 0.0515 0.0451 Uiso 1.00 calc . . . H(25) H -1.4979 0.6160 -0.0319 0.0451 Uiso 1.00 calc . . . H(26) H -1.1824 0.6165 0.2881 0.0555 Uiso 1.00 calc . . . H(27) H -1.2527 0.6059 0.3916 0.0555 Uiso 1.00 calc . . . H(28) H -1.3784 0.5983 0.3025 0.0555 Uiso 1.00 calc . . . H(29) H -1.4617 0.6749 -0.1831 0.0423 Uiso 1.00 calc . . . H(30) H -1.2501 0.7317 -0.2431 0.0464 Uiso 1.00 calc . . . H(31) H -1.3009 0.7732 -0.1658 0.0464 Uiso 1.00 calc . . . H(32) H -1.2117 0.7207 -0.1344 0.0464 Uiso 1.00 calc . . . H(33) H -1.7141 0.7125 -0.2492 0.0343 Uiso 1.00 calc . . . H(34) H -1.5533 0.7314 -0.3101 0.0343 Uiso 1.00 calc . . . H(35) H -1.7319 0.7933 -0.1721 0.0481 Uiso 1.00 calc . . . H(36) H -1.5552 0.8120 -0.2188 0.0481 Uiso 1.00 calc . . . H(37) H -1.4898 0.8228 0.5464 0.0512 Uiso 1.00 calc . . . H(38) H -1.8302 0.7360 0.2029 0.0408 Uiso 1.00 calc . . . H(39) H -1.2471 0.7964 0.0943 0.0374 Uiso 1.00 calc . . . H(40) H -2.0129 0.8316 -0.3514 0.0490 Uiso 1.00 calc . . . H(41) H -0.6396 0.4505 0.1737 0.0407 Uiso 1.00 calc . . . H(42) H -0.6959 0.4676 0.0699 0.0407 Uiso 1.00 calc . . . H(43) H -0.6514 0.3776 0.0697 0.0457 Uiso 1.00 calc . . . H(44) H -0.7850 0.3708 0.1539 0.0457 Uiso 1.00 calc . . . H(45) H -0.8779 0.4028 -0.0317 0.0399 Uiso 1.00 calc . . . H(46) H -1.1704 0.4073 0.0168 0.0432 Uiso 1.00 calc . . . H(47) H -1.1155 0.3896 0.1205 0.0432 Uiso 1.00 calc . . . H(48) H -1.0285 0.4855 0.0382 0.0379 Uiso 1.00 calc . . . H(49) H -1.2211 0.5278 0.1336 0.0395 Uiso 1.00 calc . . . H(50) H -1.3277 0.4804 0.0917 0.0395 Uiso 1.00 calc . . . H(51) H -1.3718 0.4935 0.2597 0.0369 Uiso 1.00 calc . . . H(52) H -1.0958 0.5154 0.3182 0.0336 Uiso 1.00 calc . . . H(53) H -0.9809 0.4172 0.2548 0.0381 Uiso 1.00 calc . . . H(54) H -0.7570 0.4876 0.3510 0.0428 Uiso 1.00 calc . . . H(55) H -0.7012 0.4320 0.3159 0.0428 Uiso 1.00 calc . . . H(56) H -0.7469 0.4336 0.4844 0.0349 Uiso 1.00 calc . . . H(57) H -1.1812 0.4183 0.3948 0.0352 Uiso 1.00 calc . . . H(58) H -1.3320 0.5126 0.4574 0.0433 Uiso 1.00 calc . . . H(59) H -1.4330 0.4607 0.4333 0.0433 Uiso 1.00 calc . . . H(60) H -1.3839 0.4302 0.5817 0.0541 Uiso 1.00 calc . . . H(61) H -1.3086 0.4852 0.6095 0.0541 Uiso 1.00 calc . . . H(62) H -1.1140 0.3963 0.5576 0.0440 Uiso 1.00 calc . . . H(63) H -0.8661 0.5170 0.5530 0.0442 Uiso 1.00 calc . . . H(64) H -1.0617 0.5339 0.5308 0.0442 Uiso 1.00 calc . . . H(65) H -0.9221 0.5330 0.4485 0.0442 Uiso 1.00 calc . . . H(66) H -0.7500 0.5380 0.2146 0.0419 Uiso 1.00 calc . . . H(67) H -0.9484 0.5538 0.1977 0.0419 Uiso 1.00 calc . . . H(68) H -0.8228 0.5465 0.1101 0.0419 Uiso 1.00 calc . . . H(69) H -1.0175 0.4762 0.6868 0.0401 Uiso 1.00 calc . . . H(70) H -0.8353 0.3803 0.6675 0.0488 Uiso 1.00 calc . . . H(71) H -0.7864 0.4227 0.7443 0.0488 Uiso 1.00 calc . . . H(72) H -0.7584 0.4342 0.6352 0.0488 Uiso 1.00 calc . . . H(73) H -1.0884 0.4165 0.8098 0.0395 Uiso 1.00 calc . . . H(74) H -1.2547 0.4339 0.7496 0.0395 Uiso 1.00 calc . . . H(75) H -1.0865 0.3369 0.7218 0.0508 Uiso 1.00 calc . . . H(76) H -1.2641 0.3542 0.6719 0.0508 Uiso 1.00 calc . . . H(77) H -1.0229 0.3260 -0.0455 0.0526 Uiso 1.00 calc . . . H(78) H -1.3736 0.4074 0.2935 0.0406 Uiso 1.00 calc . . . H(79) H -0.7820 0.3561 0.4091 0.0405 Uiso 1.00 calc . . . H(80) H -1.5424 0.3179 0.8493 0.0482 Uiso 1.00 calc . . . H(81) H -2.1685 0.6103 -0.2234 0.0553 Uiso 1.00 calc . . . H(82) H -2.0957 0.5562 -0.0943 0.0600 Uiso 1.00 calc . . . H(83) H -1.8182 0.5177 -0.0870 0.0508 Uiso 1.00 calc . . . H(84) H -1.5919 0.6361 -0.3601 0.0738 Uiso 1.00 calc . . . H(85) H -1.5087 0.5806 -0.3456 0.0738 Uiso 1.00 calc . . . H(86) H -1.6594 0.5890 -0.4222 0.0738 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 Br(1) 0.0394(7) 0.0564(7) 0.0570(9) 0.0076(6) 0.0039(6) -0.0150(6) Br(2) 0.0583(9) 0.0464(6) 0.0365(6) 0.0013(6) -0.0024(6) 0.0027(6) O(1) 0.028(2) 0.041(2) 0.056(3) -0.003(2) 0.007(2) -0.015(2) O(2) 0.031(2) 0.032(2) 0.037(2) 0.003(2) 0.010(2) -0.003(2) O(3) 0.027(2) 0.030(2) 0.036(2) -0.005(1) 0.002(2) 0.003(2) O(4) 0.047(3) 0.050(2) 0.034(2) 0.014(2) 0.005(2) 0.000(2) O(5) 0.043(2) 0.036(2) 0.041(2) -0.002(2) 0.000(2) -0.003(2) O(6) 0.043(2) 0.043(2) 0.044(2) 0.008(2) -0.007(2) -0.015(2) O(7) 0.024(2) 0.035(2) 0.040(2) -0.008(2) 0.002(2) 0.003(2) O(8) 0.035(2) 0.027(2) 0.038(2) 0.005(2) 0.000(2) -0.002(2) O(9) 0.038(2) 0.051(2) 0.046(2) -0.015(2) 0.002(2) 0.008(2) O(10) 0.049(2) 0.039(2) 0.031(2) -0.001(2) 0.003(2) 0.002(2) C(1) 0.041(3) 0.041(3) 0.033(3) 0.002(2) 0.001(3) 0.003(2) C(2) 0.031(3) 0.043(3) 0.034(3) 0.006(2) 0.002(2) 0.005(2) C(3) 0.027(3) 0.039(2) 0.051(4) -0.005(2) 0.010(2) -0.009(3) C(4) 0.035(3) 0.034(2) 0.023(2) 0.002(2) 0.002(2) -0.007(2) C(5) 0.036(3) 0.032(2) 0.036(3) 0.000(2) 0.011(2) 0.005(2) C(6) 0.039(3) 0.037(3) 0.032(2) -0.001(2) 0.017(2) -0.007(2) C(7) 0.025(3) 0.032(2) 0.036(2) 0.004(2) 0.008(2) 0.004(2) C(8) 0.030(3) 0.037(3) 0.032(3) 0.000(2) 0.003(2) 0.005(2) C(9) 0.027(3) 0.041(3) 0.036(3) 0.010(2) -0.005(2) -0.001(2) C(10) 0.039(3) 0.028(2) 0.036(3) 0.003(2) 0.008(2) 0.005(2) C(11) 0.025(3) 0.046(3) 0.034(3) -0.002(2) -0.005(2) -0.003(2) C(12) 0.035(3) 0.032(2) 0.032(2) 0.005(2) 0.009(2) -0.007(2) C(13) 0.031(3) 0.030(2) 0.027(3) -0.002(2) 0.009(2) 0.007(2) C(14) 0.027(2) 0.027(2) 0.033(2) 0.005(2) 0.003(2) 0.000(2) C(15) 0.042(3) 0.035(3) 0.033(3) -0.009(2) -0.003(2) 0.007(2) C(16) 0.046(3) 0.033(3) 0.029(2) -0.002(2) 0.000(3) 0.005(2) C(17) 0.044(3) 0.046(3) 0.020(2) 0.001(2) 0.001(2) 0.001(2) C(18) 0.037(3) 0.034(2) 0.041(3) 0.010(2) 0.004(3) 0.006(2) C(19) 0.054(4) 0.034(3) 0.051(4) 0.013(3) 0.004(3) 0.007(3) C(20) 0.032(3) 0.048(3) 0.025(2) 0.006(2) 0.001(2) 0.003(2) C(21) 0.038(3) 0.053(3) 0.025(3) -0.001(3) 0.007(2) 0.005(2) C(22) 0.038(3) 0.032(2) 0.017(2) 0.004(2) 0.009(2) 0.001(2) C(23) 0.056(4) 0.025(2) 0.038(3) 0.007(2) -0.004(3) 0.004(2) C(24) 0.044(2) 0.023(2) 0.035(2) 0.004(2) -0.007(2) -0.005(2) C(25) 0.027(3) 0.040(3) 0.032(3) -0.005(2) 0.012(2) -0.002(2) C(26) 0.030(3) 0.042(3) 0.042(3) -0.007(2) 0.005(2) 0.001(2) C(27) 0.030(3) 0.039(2) 0.032(3) 0.003(2) 0.008(2) 0.003(2) C(28) 0.020(2) 0.041(3) 0.046(3) -0.001(2) -0.001(2) -0.018(3) C(29) 0.027(2) 0.032(2) 0.035(3) -0.008(2) 0.009(2) 0.006(2) C(30) 0.029(3) 0.033(3) 0.037(3) 0.003(2) -0.001(2) 0.003(2) C(31) 0.021(2) 0.029(2) 0.041(3) 0.006(2) 0.005(2) 0.002(2) C(32) 0.026(2) 0.031(3) 0.027(2) 0.002(2) 0.008(2) 0.004(2) C(33) 0.022(2) 0.029(2) 0.045(3) -0.004(2) 0.004(2) 0.004(2) C(34) 0.024(2) 0.031(2) 0.036(3) -0.003(2) 0.006(2) -0.007(2) C(35) 0.032(3) 0.044(3) 0.031(3) -0.003(2) 0.008(2) 0.001(2) C(36) 0.024(2) 0.025(2) 0.038(3) -0.003(2) 0.001(2) 0.006(2) C(37) 0.030(3) 0.024(2) 0.045(3) -0.001(2) -0.001(2) -0.006(2) C(38) 0.022(2) 0.030(2) 0.034(3) 0.000(2) 0.008(2) 0.005(2) C(39) 0.026(3) 0.048(3) 0.034(3) 0.008(2) 0.010(2) -0.012(2) C(40) 0.046(3) 0.050(4) 0.041(3) 0.005(3) 0.004(3) 0.006(3) C(41) 0.039(3) 0.035(3) 0.036(2) -0.006(2) -0.001(2) -0.016(2) C(42) 0.041(3) 0.027(2) 0.041(3) -0.006(2) 0.002(3) -0.001(2) C(43) 0.028(3) 0.033(2) 0.044(3) -0.006(2) 0.004(2) 0.006(2) C(44) 0.044(3) 0.028(2) 0.027(2) -0.003(2) -0.002(2) 0.003(2) C(45) 0.042(3) 0.050(3) 0.032(3) -0.001(3) 0.002(3) 0.008(3) C(46) 0.047(3) 0.022(2) 0.028(3) 0.003(2) 0.005(2) 0.000(2) C(47) 0.066(4) 0.027(3) 0.038(3) -0.021(3) 0.021(3) -0.010(2) C(48) 0.050(2) 0.027(2) 0.040(3) -0.012(2) 0.010(2) 0.005(2) C(49) 0.049(3) 0.055(4) 0.023(3) 0.006(2) 0.003(2) -0.007(2) C(50) 0.054(3) 0.048(3) 0.033(3) -0.004(3) 0.006(3) -0.001(2) C(51) 0.055(3) 0.055(4) 0.034(3) -0.003(3) -0.012(2) 0.001(2) C(52) 0.036(3) 0.044(3) 0.057(4) 0.001(3) -0.006(2) -0.003(3) C(53) 0.050(3) 0.053(4) 0.047(3) -0.008(3) 0.005(3) -0.002(3) C(54) 0.054(3) 0.047(3) 0.026(3) -0.005(3) 0.003(2) -0.002(3) C(55) 0.087(6) 0.067(5) 0.032(3) -0.033(4) 0.023(4) -0.020(3) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) C(49) 1.84(1) . . yes Br(2) C(51) 1.79(1) . . yes O(1) C(3) 1.45(1) . . yes O(2) C(7) 1.44(1) . . yes O(3) C(12) 1.47(1) . . yes O(4) C(24) 1.20(1) . . yes O(5) C(24) 1.33(1) . . yes O(6) C(27) 1.43(1) . . yes O(7) C(31) 1.43(1) . . yes O(8) C(36) 1.43(1) . . yes O(9) C(48) 1.26(1) . . yes O(10) C(48) 1.31(1) . . yes C(1) C(2) 1.51(1) . . yes C(1) C(10) 1.58(2) . . yes C(2) C(3) 1.52(1) . . yes C(3) C(4) 1.50(1) . . yes C(4) C(5) 1.54(1) . . yes C(5) C(6) 1.54(2) . . yes C(5) C(10) 1.54(1) . . yes C(6) C(7) 1.50(1) . . yes C(7) C(8) 1.57(1) . . yes C(8) C(9) 1.55(1) . . yes C(8) C(14) 1.52(1) . . yes C(9) C(10) 1.55(1) . . yes C(9) C(11) 1.56(1) . . yes C(10) C(19) 1.53(1) . . yes C(11) C(12) 1.52(1) . . yes C(12) C(13) 1.52(1) . . yes C(13) C(14) 1.56(1) . . yes C(13) C(17) 1.57(1) . . yes C(13) C(18) 1.53(1) . . yes C(14) C(15) 1.53(1) . . yes C(15) C(16) 1.54(1) . . yes C(16) C(17) 1.55(2) . . yes C(17) C(20) 1.52(1) . . yes C(20) C(21) 1.53(1) . . yes C(20) C(22) 1.56(1) . . yes C(22) C(23) 1.56(1) . . yes C(23) C(24) 1.50(1) . . yes C(25) C(26) 1.54(1) . . yes C(25) C(34) 1.57(1) . . yes C(26) C(27) 1.50(1) . . yes C(27) C(28) 1.53(1) . . yes C(28) C(29) 1.52(1) . . yes C(29) C(30) 1.54(1) . . yes C(29) C(34) 1.53(1) . . yes C(30) C(31) 1.54(1) . . yes C(31) C(32) 1.54(1) . . yes C(32) C(33) 1.54(1) . . yes C(32) C(38) 1.51(1) . . yes C(33) C(34) 1.53(1) . . yes C(33) C(35) 1.54(1) . . yes C(34) C(43) 1.53(1) . . yes C(35) C(36) 1.55(1) . . yes C(36) C(37) 1.55(1) . . yes C(37) C(38) 1.56(1) . . yes C(37) C(41) 1.55(1) . . yes C(37) C(42) 1.54(1) . . yes C(38) C(39) 1.54(1) . . yes C(39) C(40) 1.54(2) . . yes C(40) C(41) 1.56(2) . . yes C(41) C(44) 1.55(1) . . yes C(44) C(45) 1.54(2) . . yes C(44) C(46) 1.53(1) . . yes C(46) C(47) 1.54(1) . . yes C(47) C(48) 1.48(1) . . yes C(49) C(50) 1.42(2) . . yes C(49) C(54) 1.37(2) . . yes C(50) C(51) 1.37(2) . . yes C(50) C(55) 1.53(2) . . yes C(51) C(52) 1.41(2) . . yes C(52) C(53) 1.37(2) . . yes C(53) C(54) 1.34(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 C(2) C(1) C(10) 114.3(9) . 1_555 1_555 yes C(1) C(2) C(3) 107.8(8) . 1_555 1_555 yes O(1) C(3) C(2) 106.8(8) . 1_555 1_555 yes O(1) C(3) C(4) 111.0(8) . 1_555 1_555 yes C(2) C(3) C(4) 110.6(8) . 1_555 1_555 yes C(3) C(4) C(5) 113.0(8) . 1_555 1_555 yes C(4) C(5) C(6) 112.1(8) . 1_555 1_555 yes C(4) C(5) C(10) 111.6(7) . 1_555 1_555 yes C(6) C(5) C(10) 111.3(8) . 1_555 1_555 yes C(5) C(6) C(7) 116.4(8) . 1_555 1_555 yes O(2) C(7) C(6) 108.6(8) . 1_555 1_555 yes O(2) C(7) C(8) 110.6(7) . 1_555 1_555 yes C(6) C(7) C(8) 111.3(8) . 1_555 1_555 yes C(7) C(8) C(9) 110.3(8) . 1_555 1_555 yes C(7) C(8) C(14) 109.7(8) . 1_555 1_555 yes C(9) C(8) C(14) 109.7(8) . 1_555 1_555 yes C(8) C(9) C(10) 111.6(8) . 1_555 1_555 yes C(8) C(9) C(11) 110.3(8) . 1_555 1_555 yes C(10) C(9) C(11) 115.2(8) . 1_555 1_555 yes C(1) C(10) C(5) 108.1(8) . 1_555 1_555 yes C(1) C(10) C(9) 111.6(8) . 1_555 1_555 yes C(1) C(10) C(19) 105.6(9) . 1_555 1_555 yes C(5) C(10) C(9) 109.4(8) . 1_555 1_555 yes C(5) C(10) C(19) 110.8(8) . 1_555 1_555 yes C(9) C(10) C(19) 111.1(9) . 1_555 1_555 yes C(9) C(11) C(12) 114.0(8) . 1_555 1_555 yes O(3) C(12) C(11) 109.2(7) . 1_555 1_555 yes O(3) C(12) C(13) 110.3(8) . 1_555 1_555 yes C(11) C(12) C(13) 112.5(8) . 1_555 1_555 yes C(12) C(13) C(14) 107.1(7) . 1_555 1_555 yes C(12) C(13) C(17) 117.2(8) . 1_555 1_555 yes C(12) C(13) C(18) 109.9(8) . 1_555 1_555 yes C(14) C(13) C(17) 99.4(7) . 1_555 1_555 yes C(14) C(13) C(18) 113.9(7) . 1_555 1_555 yes C(17) C(13) C(18) 109.1(8) . 1_555 1_555 yes C(8) C(14) C(13) 113.5(8) . 1_555 1_555 yes C(8) C(14) C(15) 118.4(8) . 1_555 1_555 yes C(13) C(14) C(15) 103.1(7) . 1_555 1_555 yes C(14) C(15) C(16) 103.8(8) . 1_555 1_555 yes C(15) C(16) C(17) 107.5(8) . 1_555 1_555 yes C(13) C(17) C(16) 103.0(7) . 1_555 1_555 yes C(13) C(17) C(20) 119.6(8) . 1_555 1_555 yes C(16) C(17) C(20) 113.2(8) . 1_555 1_555 yes C(17) C(20) C(21) 114.9(9) . 1_555 1_555 yes C(17) C(20) C(22) 110.4(8) . 1_555 1_555 yes C(21) C(20) C(22) 110.8(8) . 1_555 1_555 yes C(20) C(22) C(23) 112.0(8) . 1_555 1_555 yes C(22) C(23) C(24) 110.3(8) . 1_555 1_555 yes O(4) C(24) O(5) 122.5(9) . 1_555 1_555 yes O(4) C(24) C(23) 121.9(9) . 1_555 1_555 yes O(5) C(24) C(23) 115.5(9) . 1_555 1_555 yes C(26) C(25) C(34) 114.0(8) . 1_555 1_555 yes C(25) C(26) C(27) 111.2(8) . 1_555 1_555 yes O(6) C(27) C(26) 109.2(8) . 1_555 1_555 yes O(6) C(27) C(28) 112.7(8) . 1_555 1_555 yes C(26) C(27) C(28) 110.1(8) . 1_555 1_555 yes C(27) C(28) C(29) 113.5(8) . 1_555 1_555 yes C(28) C(29) C(30) 112.2(8) . 1_555 1_555 yes C(28) C(29) C(34) 113.6(8) . 1_555 1_555 yes C(30) C(29) C(34) 110.4(8) . 1_555 1_555 yes C(29) C(30) C(31) 113.3(8) . 1_555 1_555 yes O(7) C(31) C(30) 107.4(8) . 1_555 1_555 yes O(7) C(31) C(32) 112.9(7) . 1_555 1_555 yes C(30) C(31) C(32) 113.3(7) . 1_555 1_555 yes C(31) C(32) C(33) 108.9(7) . 1_555 1_555 yes C(31) C(32) C(38) 110.8(7) . 1_555 1_555 yes C(33) C(32) C(38) 110.7(7) . 1_555 1_555 yes C(32) C(33) C(34) 112.5(7) . 1_555 1_555 yes C(32) C(33) C(35) 110.2(8) . 1_555 1_555 yes C(34) C(33) C(35) 115.4(7) . 1_555 1_555 yes C(25) C(34) C(29) 108.0(7) . 1_555 1_555 yes C(25) C(34) C(33) 111.1(8) . 1_555 1_555 yes C(25) C(34) C(43) 103.3(7) . 1_555 1_555 yes C(29) C(34) C(33) 110.2(7) . 1_555 1_555 yes C(29) C(34) C(43) 111.5(8) . 1_555 1_555 yes C(33) C(34) C(43) 112.4(8) . 1_555 1_555 yes C(33) C(35) C(36) 115.0(8) . 1_555 1_555 yes O(8) C(36) C(35) 110.6(7) . 1_555 1_555 yes O(8) C(36) C(37) 110.2(7) . 1_555 1_555 yes C(35) C(36) C(37) 110.3(7) . 1_555 1_555 yes C(36) C(37) C(38) 106.5(7) . 1_555 1_555 yes C(36) C(37) C(41) 117.6(8) . 1_555 1_555 yes C(36) C(37) C(42) 110.3(8) . 1_555 1_555 yes C(38) C(37) C(41) 99.5(7) . 1_555 1_555 yes C(38) C(37) C(42) 111.7(7) . 1_555 1_555 yes C(41) C(37) C(42) 110.8(8) . 1_555 1_555 yes C(32) C(38) C(37) 114.9(7) . 1_555 1_555 yes C(32) C(38) C(39) 118.4(7) . 1_555 1_555 yes C(37) C(38) C(39) 103.1(8) . 1_555 1_555 yes C(38) C(39) C(40) 104.6(8) . 1_555 1_555 yes C(39) C(40) C(41) 105.9(8) . 1_555 1_555 yes C(37) C(41) C(40) 104.2(8) . 1_555 1_555 yes C(37) C(41) C(44) 118.9(8) . 1_555 1_555 yes C(40) C(41) C(44) 110.6(8) . 1_555 1_555 yes C(41) C(44) C(45) 112.3(8) . 1_555 1_555 yes C(41) C(44) C(46) 110.1(8) . 1_555 1_555 yes C(45) C(44) C(46) 110.9(8) . 1_555 1_555 yes C(44) C(46) C(47) 115.1(7) . 1_555 1_555 yes C(46) C(47) C(48) 111.4(8) . 1_555 1_555 yes O(9) C(48) O(10) 119.7(8) . 1_555 1_555 yes O(9) C(48) C(47) 124(1) . 1_555 1_555 yes O(10) C(48) C(47) 116.3(10) . 1_555 1_555 yes Br(1) C(49) C(50) 119.1(8) . 1_555 1_555 yes Br(1) C(49) C(54) 120.1(9) . 1_555 1_555 yes C(50) C(49) C(54) 120(1) . 1_555 1_555 yes C(49) C(50) C(51) 117(1) . 1_555 1_555 yes C(49) C(50) C(55) 121(1) . 1_555 1_555 yes C(51) C(50) C(55) 120(1) . 1_555 1_555 yes Br(2) C(51) C(50) 123.4(9) . 1_555 1_555 yes Br(2) C(51) C(52) 117.3(9) . 1_555 1_555 yes C(50) C(51) C(52) 119(1) . 1_555 1_555 yes C(51) C(52) C(53) 121(1) . 1_555 1_555 yes C(52) C(53) C(54) 118(1) . 1_555 1_555 yes C(49) C(54) C(53) 121(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) C(49) C(50) C(51) 179.2(9) 1_555 1_555 1_555 1_555 yes Br(1) C(49) C(50) C(55) -2(1) 1_555 1_555 1_555 1_555 yes Br(1) C(49) C(54) C(53) -179.6(9) 1_555 1_555 1_555 1_555 yes Br(2) C(51) C(50) C(49) 179.4(9) 1_555 1_555 1_555 1_555 yes Br(2) C(51) C(50) C(55) 0(1) 1_555 1_555 1_555 1_555 yes Br(2) C(51) C(52) C(53) -179.7(9) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) 179.7(8) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 177.0(8) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -72.9(10) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 69.7(10) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -51(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 68(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -66.3(9) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 44(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 169.5(7) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -79(1) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 103.4(9) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(26) C(25) -179.3(7) 1_555 1_555 1_555 1_555 yes O(6) C(27) C(28) C(29) 177.3(8) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(30) C(29) -74.9(9) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(33) 71.2(9) 1_555 1_555 1_555 1_555 yes O(7) C(31) C(32) C(38) -50.8(9) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(35) C(33) 66.7(10) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(38) -66.9(9) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(41) 43(1) 1_555 1_555 1_555 1_555 yes O(8) C(36) C(37) C(42) 171.8(8) 1_555 1_555 1_555 1_555 yes O(9) C(48) C(47) C(46) -82(1) 1_555 1_555 1_555 1_555 yes O(10) C(48) C(47) C(46) 97(1) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -59(1) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 49(1) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 175.8(8) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -179.0(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 54(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -55(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 65(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -173.8(8) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 58(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 59(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 179.9(8) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -54(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 74.6(10) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -72(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 165.1(9) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 49(1) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -59.4(10) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 173.8(8) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 53(1) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -68(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -51.0(10) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -172.0(8) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -51(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 57.7(9) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -172.8(8) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -179.5(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -58(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 63(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 50(1) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -60.3(9) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 177.2(8) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 61(1) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -162.5(8) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 59.1(10) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -179.9(8) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -54(1) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) 178.7(7) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 178.1(8) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -51.8(10) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -63(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 55.9(9) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 166.5(8) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -68.3(9) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 170.5(7) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -155.6(8) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 77(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -36.3(9) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 19.5(10) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -59(1) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 174.3(8) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -40.6(8) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -167.2(9) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 10(1) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 48.0(8) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -67.8(10) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 150.1(9) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.8(9) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 179.0(8) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 52(1) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) 57(1) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -47(1) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 171.4(8) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) -70(1) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -55(1) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(28) 50.8(10) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(30) 177.8(7) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(32) 179.6(7) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(35) 51.9(10) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(29) -52(1) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(33) 68(1) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(43) -170.6(8) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 55(1) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(34) 56(1) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 179.4(8) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(34) -54(1) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 75(1) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(33) -70.8(9) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(43) 163.6(8) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 50(1) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) -60.7(9) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(35) 171.6(7) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) 56.3(9) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) -69.3(9) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -51.3(9) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(38) -173.2(7) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) -52.0(10) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 57.0(9) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(35) -172.6(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(37) 179.2(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(39) -58(1) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) 64(1) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(35) C(36) 51.4(10) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(36) -60.1(9) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(41) 177.3(7) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(42) 60(1) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(39) C(40) -162.5(8) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(37) 58.3(10) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(39) -179.4(8) 1_555 1_555 1_555 1_555 yes C(33) C(35) C(36) C(37) -55(1) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(38) 179.0(7) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(35) C(36) -179.9(7) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(32) C(38) -50.6(9) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(34) C(43) -63(1) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 55.6(9) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(41) 166.0(8) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(42) -65.8(10) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) 169.7(7) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(40) -156.1(8) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(44) 80(1) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) -34.4(10) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(40) C(39) 21.5(10) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(45) -59(1) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(46) 176.4(8) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(40) -41.8(8) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(44) -165.4(8) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) 8(1) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(41) 47.1(8) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(42) -69.8(9) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(44) 150.3(8) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(37) C(42) 75.9(10) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(45) -179.9(8) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(46) 56(1) 1_555 1_555 1_555 1_555 yes C(41) C(44) C(46) C(47) 54(1) 1_555 1_555 1_555 1_555 yes C(42) C(37) C(41) C(44) -47(1) 1_555 1_555 1_555 1_555 yes C(44) C(46) C(47) C(48) 174.0(10) 1_555 1_555 1_555 1_555 yes C(45) C(44) C(46) C(47) -70(1) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) -2(1) 1_555 1_555 1_555 1_555 yes C(49) C(54) C(53) C(52) 3(1) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(54) C(53) -3(1) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) 1(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(54) 3(1) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) -2(1) 1_555 1_555 1_555 1_555 yes C(52) C(51) C(50) C(55) 179(1) 1_555 1_555 1_555 1_555 yes C(54) C(49) C(50) C(55) -178(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(8) 2.667(10) . 2_356 ? O(1) O(4) 2.737(10) . 1_556 ? O(1) C(36) 3.41(1) . 2_356 ? O(2) C(48) 3.01(1) . 2_256 ? O(2) O(9) 3.11(1) . 2_256 ? O(2) C(47) 3.32(1) . 2_256 ? O(2) C(1) 3.34(1) . 1_455 ? O(2) O(10) 3.470(9) . 2_256 ? O(3) O(6) 2.668(9) . 2_355 ? O(3) O(10) 2.670(9) . 2_256 ? O(3) O(9) 3.397(9) . 2_256 ? O(3) C(48) 3.46(1) . 2_256 ? O(3) C(27) 3.58(1) . 2_355 ? O(4) O(7) 3.13(1) . 2_255 ? O(4) C(38) 3.39(1) . 2_255 ? O(4) O(8) 3.43(1) . 2_255 ? O(4) C(3) 3.50(1) . 1_554 ? O(4) C(4) 3.57(1) . 1_554 ? O(5) O(8) 2.66(1) . 2_255 ? O(5) O(7) 3.444(10) . 2_255 ? O(5) C(33) 3.56(1) . 2_255 ? O(6) O(9) 2.73(1) . 1_554 ? O(6) C(12) 3.38(1) . 2_345 ? O(7) C(24) 3.00(1) . 2_245 ? O(7) C(23) 3.24(1) . 2_245 ? O(7) C(25) 3.34(1) . 1_455 ? O(8) C(24) 3.45(1) . 2_245 ? O(8) C(3) 3.54(1) . 2_346 ? O(9) C(14) 3.35(1) . 2_246 ? O(9) C(27) 3.50(1) . 1_556 ? O(9) C(28) 3.59(1) . 1_556 ? O(10) C(9) 3.57(1) . 2_246 ? #------------------------------------------------------------------------------ #===END data_nung _database_code_depnum_ccdc_archive 'CCDC 297676' _audit_creation_date 'Thu Oct 28 11:44:02 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C32 H51 N O5 ' _chemical_formula_moiety ? _chemical_formula_weight 529.76 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 13.625(3) _cell_length_b 7.745(1) _cell_length_c 15.218(3) _cell_angle_alpha 90 _cell_angle_beta 112.357(8) _cell_angle_gamma 90 _cell_volume 1485.1(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6431 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 50.4 _cell_measurement_temperature 203.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.973 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7298 _diffrn_reflns_av_R_equivalents 0.130 _diffrn_reflns_theta_max 68.24 _diffrn_measured_fraction_theta_max 0.9874 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.9874 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # 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 2907 _reflns_number_gt 1208 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1040 _refine_ls_wR_factor_ref 0.2842 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2907 _refine_ls_number_parameters 344 _refine_ls_goodness_of_fit_ref 1.101 _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 0.0003 _refine_diff_density_max 0.36 _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 -2.0(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.031 0.018 ;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 0.6085(8) 0.334(3) 1.0918(7) 0.040(3) Uani 1.00 d . . . O(2) O 0.2642(7) 0.572(3) 0.8977(7) 0.035(3) Uani 1.00 d . . . O(3) O 0.2009(6) 0.014(3) 0.8017(6) 0.035(2) Uani 1.00 d . . . O(4) O -0.1945(9) 0.243(3) 0.3270(7) 0.047(3) Uani 1.00 d . . . O(5) O -0.2610(7) -0.019(3) 0.2699(6) 0.031(2) Uani 1.00 d . . . N(1) N 0.322(1) 0.098(4) 0.661(1) 0.059(5) Uani 1.00 d . . . C(1) C 0.3798(10) 0.119(4) 1.1299(9) 0.031(3) Uani 1.00 d . . . C(2) C 0.4743(10) 0.140(4) 1.1004(9) 0.031(3) Uani 1.00 d . . . C(3) C 0.525(1) 0.313(4) 1.1260(10) 0.034(3) Uani 1.00 d . . . C(4) C 0.439(1) 0.456(4) 1.080(1) 0.035(4) Uani 1.00 d . . . C(5) C 0.342(1) 0.433(4) 1.106(1) 0.039(4) Uani 1.00 d . . . C(6) C 0.260(1) 0.576(4) 1.0583(9) 0.030(3) Uani 1.00 d . . . C(7) C 0.197(1) 0.549(4) 0.9512(9) 0.033(3) Uani 1.00 d . . . C(8) C 0.1473(9) 0.368(4) 0.9296(9) 0.024(3) Uani 1.00 d . . . C(9) C 0.2327(10) 0.226(4) 0.9766(9) 0.025(3) Uani 1.00 d . . . C(10) C 0.292(1) 0.255(4) 1.0857(9) 0.034(3) Uani 1.00 d . . . C(11) C 0.178(1) 0.052(4) 0.9481(10) 0.037(4) Uani 1.00 d . . . C(12) C 0.1207(9) 0.020(3) 0.8393(9) 0.025(3) Uani 1.00 d . . . C(13) C 0.038(1) 0.164(4) 0.7946(9) 0.033(3) Uani 1.00 d . . . C(14) C 0.099(1) 0.342(4) 0.8258(9) 0.029(3) Uani 1.00 d . . . C(15) C 0.021(1) 0.472(4) 0.7633(9) 0.031(3) Uani 1.00 d . . . C(16) C -0.037(1) 0.380(4) 0.670(1) 0.038(4) Uani 1.00 d . . . C(17) C 0.0004(10) 0.188(4) 0.6834(9) 0.026(3) Uani 1.00 d . . . C(18) C -0.056(1) 0.148(4) 0.824(1) 0.040(4) Uani 1.00 d . . . C(19) C 0.213(1) 0.228(4) 1.1382(10) 0.046(5) Uani 1.00 d . . . C(20) C -0.085(1) 0.066(4) 0.617(1) 0.038(3) Uani 1.00 d . . . C(21) C -0.061(1) -0.123(4) 0.6353(10) 0.046(4) Uani 1.00 d . . . C(22) C -0.105(1) 0.111(4) 0.5115(10) 0.045(4) Uani 1.00 d . . . C(23) C -0.187(1) 0.013(4) 0.4364(8) 0.033(3) Uani 1.00 d . . . C(24) C -0.214(1) 0.097(4) 0.3392(9) 0.037(3) Uani 1.00 d . . . C(25) C 0.425(1) 0.115(4) 0.661(1) 0.046(4) Uani 1.00 d . . . C(26) C 0.463(1) -0.020(4) 0.619(1) 0.050(4) Uani 1.00 d . . . C(27) C 0.567(1) -0.005(4) 0.618(1) 0.049(4) Uani 1.00 d . . . C(28) C 0.627(1) 0.137(4) 0.659(1) 0.053(5) Uani 1.00 d . . . C(29) C 0.587(1) 0.266(4) 0.695(1) 0.051(5) Uani 1.00 d . . . C(30) C 0.486(1) 0.256(4) 0.696(1) 0.052(4) Uani 1.00 d . . . C(31) C 0.393(2) -0.178(4) 0.580(1) 0.067(6) Uani 1.00 d . . . C(32) C 0.607(2) -0.147(4) 0.576(1) 0.061(6) Uani 1.00 d . . . H(1) H 0.3481 0.0111 1.1049 0.0399 Uiso 1.00 calc . . . H(2) H 0.4031 0.1201 1.1960 0.0399 Uiso 1.00 calc . . . H(3) H 0.5264 0.0630 1.1297 0.0288 Uiso 1.00 calc . . . H(4) H 0.4511 0.1376 1.0329 0.0288 Uiso 1.00 calc . . . H(5) H 0.5520 0.3276 1.1932 0.0319 Uiso 1.00 calc . . . H(6) H 0.4681 0.5679 1.1015 0.0548 Uiso 1.00 calc . . . H(7) H 0.4156 0.4516 1.0130 0.0548 Uiso 1.00 calc . . . H(8) H 0.3629 0.4507 1.1738 0.0598 Uiso 1.00 calc . . . H(9) H 0.2095 0.5850 1.0874 0.0288 Uiso 1.00 calc . . . H(10) H 0.2978 0.6846 1.0676 0.0288 Uiso 1.00 calc . . . H(11) H 0.1413 0.6391 0.9271 0.0416 Uiso 1.00 calc . . . H(12) H 0.0935 0.3611 0.9566 0.0304 Uiso 1.00 calc . . . H(13) H 0.2825 0.2334 0.9466 0.0340 Uiso 1.00 calc . . . H(14) H 0.2282 -0.0319 0.9746 0.0514 Uiso 1.00 calc . . . H(15) H 0.1243 0.0507 0.9742 0.0514 Uiso 1.00 calc . . . H(16) H 0.0896 -0.0869 0.8306 0.0277 Uiso 1.00 calc . . . H(17) H 0.1573 0.3404 0.8046 0.0269 Uiso 1.00 calc . . . H(18) H -0.0288 0.5069 0.7893 0.0303 Uiso 1.00 calc . . . H(19) H 0.0556 0.5733 0.7520 0.0303 Uiso 1.00 calc . . . H(20) H -0.1123 0.3908 0.6509 0.0384 Uiso 1.00 calc . . . H(21) H -0.0197 0.4346 0.6191 0.0384 Uiso 1.00 calc . . . H(22) H 0.0595 0.1831 0.6668 0.0380 Uiso 1.00 calc . . . H(23) H -0.0991 0.2533 0.8087 0.0452 Uiso 1.00 calc . . . H(24) H -0.1013 0.0553 0.7926 0.0452 Uiso 1.00 calc . . . H(25) H -0.0346 0.1318 0.8917 0.0452 Uiso 1.00 calc . . . H(26) H 0.1574 0.3161 1.1141 0.0592 Uiso 1.00 calc . . . H(27) H 0.1801 0.1195 1.1169 0.0592 Uiso 1.00 calc . . . H(28) H 0.2455 0.2355 1.2022 0.0592 Uiso 1.00 calc . . . H(29) H -0.1519 0.0924 0.6237 0.0463 Uiso 1.00 calc . . . H(30) H -0.1161 -0.1851 0.5936 0.0515 Uiso 1.00 calc . . . H(31) H 0.0034 -0.1407 0.6255 0.0515 Uiso 1.00 calc . . . H(32) H -0.0500 -0.1413 0.6992 0.0515 Uiso 1.00 calc . . . H(33) H -0.1237 0.2318 0.5041 0.0460 Uiso 1.00 calc . . . H(34) H -0.0381 0.0971 0.5075 0.0460 Uiso 1.00 calc . . . H(35) H -0.1582 -0.0985 0.4335 0.0338 Uiso 1.00 calc . . . H(36) H -0.2477 0.0034 0.4501 0.0338 Uiso 1.00 calc . . . H(37) H 0.6380 0.4519 1.1072 0.0522 Uiso 1.00 calc . . . H(38) H 0.2995 0.6880 0.9112 0.0318 Uiso 1.00 calc . . . H(39) H 0.1937 -0.0892 0.7466 0.0506 Uiso 1.00 calc . . . H(40) H -0.2162 -0.0283 0.2347 0.0363 Uiso 1.00 calc . . . H(41) H 0.2961 0.1864 0.6907 0.0766 Uiso 1.00 calc . . . H(42) H 0.2840 0.0007 0.6350 0.0766 Uiso 1.00 calc . . . H(43) H 0.6960 0.1465 0.6599 0.0657 Uiso 1.00 calc . . . H(44) H 0.6322 0.3659 0.7208 0.0582 Uiso 1.00 calc . . . H(45) H 0.4642 0.3511 0.7235 0.0593 Uiso 1.00 calc . . . H(46) H 0.3306 -0.1350 0.5283 0.0828 Uiso 1.00 calc . . . H(47) H 0.4309 -0.2504 0.5554 0.0828 Uiso 1.00 calc . . . H(48) H 0.3748 -0.2265 0.6263 0.0828 Uiso 1.00 calc . . . H(49) H 0.6068 -0.2492 0.6097 0.0807 Uiso 1.00 calc . . . H(50) H 0.5599 -0.1583 0.5116 0.0807 Uiso 1.00 calc . . . H(51) H 0.6750 -0.1180 0.5806 0.0807 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) 0.035(5) 0.041(6) 0.040(5) 0.001(5) 0.010(4) 0.007(5) O(2) 0.023(4) 0.037(6) 0.042(5) -0.001(4) 0.010(4) 0.005(5) O(3) 0.018(4) 0.053(7) 0.024(4) 0.013(4) -0.002(3) -0.002(5) O(4) 0.069(7) 0.031(5) 0.039(6) -0.004(5) 0.018(5) 0.009(5) O(5) 0.035(5) 0.024(5) 0.029(4) 0.004(4) 0.007(4) 0.001(4) N(1) 0.061(8) 0.07(1) 0.067(9) -0.015(8) 0.045(8) -0.030(9) C(1) 0.023(6) 0.039(8) 0.024(6) -0.011(5) 0.001(5) -0.003(6) C(2) 0.019(6) 0.040(7) 0.025(7) 0.003(5) -0.001(5) -0.014(6) C(3) 0.043(7) 0.028(6) 0.032(7) 0.015(5) 0.015(6) 0.012(6) C(4) 0.040(7) 0.026(8) 0.037(7) 0.012(5) 0.012(6) 0.000(6) C(5) 0.045(8) 0.039(7) 0.034(8) -0.004(5) 0.017(6) -0.010(6) C(6) 0.039(7) 0.024(6) 0.031(6) -0.024(5) 0.017(5) -0.025(5) C(7) 0.030(6) 0.031(6) 0.030(5) -0.009(5) 0.004(4) 0.004(6) C(8) 0.013(5) 0.032(5) 0.027(5) -0.002(4) 0.007(4) 0.000(5) C(9) 0.024(6) 0.030(6) 0.019(4) 0.002(4) 0.005(4) 0.006(5) C(10) 0.047(8) 0.033(6) 0.018(5) 0.007(5) 0.009(5) 0.001(6) C(11) 0.053(9) 0.032(7) 0.027(5) -0.011(6) 0.016(6) -0.012(6) C(12) 0.021(5) 0.023(6) 0.027(5) -0.009(4) 0.005(4) 0.001(5) C(13) 0.026(6) 0.033(6) 0.026(5) 0.006(4) -0.004(5) 0.004(6) C(14) 0.033(7) 0.030(6) 0.027(5) 0.006(5) 0.014(5) 0.005(5) C(15) 0.035(7) 0.022(7) 0.039(6) -0.005(5) 0.016(5) 0.015(5) C(16) 0.041(8) 0.028(6) 0.039(7) 0.001(6) 0.008(6) 0.010(6) C(17) 0.026(6) 0.025(5) 0.030(5) -0.012(4) 0.012(5) 0.019(5) C(18) 0.036(8) 0.042(9) 0.045(8) -0.011(7) 0.021(6) -0.009(8) C(19) 0.07(1) 0.06(1) 0.025(7) -0.001(9) 0.035(7) -0.007(8) C(20) 0.032(7) 0.042(6) 0.031(6) -0.012(5) 0.002(5) -0.007(6) C(21) 0.053(10) 0.042(6) 0.021(7) 0.004(7) -0.010(6) -0.025(7) C(22) 0.031(7) 0.07(1) 0.027(5) -0.003(7) -0.001(5) -0.016(7) C(23) 0.037(7) 0.040(8) 0.018(5) 0.004(5) 0.006(5) -0.002(5) C(24) 0.052(8) 0.029(5) 0.023(5) 0.001(6) 0.007(5) 0.002(4) C(25) 0.057(7) 0.050(8) 0.031(7) -0.007(6) 0.018(6) 0.010(6) C(26) 0.046(7) 0.066(10) 0.028(7) 0.007(7) 0.003(6) 0.002(7) C(27) 0.052(7) 0.07(1) 0.025(6) 0.005(7) 0.020(6) -0.006(8) C(28) 0.029(7) 0.09(1) 0.042(8) 0.001(6) 0.013(6) -0.029(9) C(29) 0.051(8) 0.042(9) 0.06(1) -0.006(7) 0.026(8) -0.005(8) C(30) 0.048(8) 0.052(10) 0.055(9) 0.004(6) 0.018(8) -0.016(9) C(31) 0.07(1) 0.07(1) 0.07(1) -0.013(9) 0.025(10) -0.01(1) C(32) 0.07(1) 0.07(1) 0.06(1) -0.004(10) 0.040(9) -0.03(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.43(2) . . yes O(2) C(7) 1.45(2) . . yes O(3) C(12) 1.41(2) . . yes O(4) C(24) 1.19(2) . . yes O(5) C(24) 1.34(2) . . yes N(1) C(25) 1.40(2) . . yes C(1) C(2) 1.52(2) . . yes C(1) C(10) 1.54(2) . . yes C(2) C(3) 1.49(2) . . yes C(3) C(4) 1.57(2) . . yes C(4) C(5) 1.53(2) . . yes C(5) C(6) 1.54(2) . . yes C(5) C(10) 1.52(2) . . yes C(6) C(7) 1.54(2) . . yes C(7) C(8) 1.54(2) . . yes C(8) C(9) 1.56(2) . . yes C(8) C(14) 1.48(2) . . yes C(9) C(10) 1.56(2) . . yes C(9) C(11) 1.52(2) . . yes C(10) C(19) 1.57(2) . . yes C(11) C(12) 1.56(2) . . yes C(12) C(13) 1.55(2) . . yes C(13) C(14) 1.59(2) . . yes C(13) C(17) 1.58(2) . . yes C(13) C(18) 1.51(2) . . yes C(14) C(15) 1.51(2) . . yes C(15) C(16) 1.52(2) . . yes C(16) C(17) 1.56(2) . . yes C(17) C(20) 1.55(2) . . yes C(20) C(21) 1.50(2) . . yes C(20) C(22) 1.56(2) . . yes C(22) C(23) 1.47(2) . . yes C(23) C(24) 1.53(2) . . yes C(25) C(26) 1.42(2) . . yes C(25) C(30) 1.36(3) . . yes C(26) C(27) 1.44(2) . . yes C(26) C(31) 1.52(3) . . yes C(27) C(28) 1.37(3) . . yes C(27) C(32) 1.48(2) . . yes C(28) C(29) 1.35(2) . . yes C(29) C(30) 1.38(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 C(2) C(1) C(10) 113(1) . 1_555 1_555 yes C(1) C(2) C(3) 112(1) . 1_555 1_555 yes O(1) C(3) C(2) 111(1) . 1_555 1_555 yes O(1) C(3) C(4) 108(1) . 1_555 1_555 yes C(2) C(3) C(4) 108(1) . 1_555 1_555 yes C(3) C(4) C(5) 112(1) . 1_555 1_555 yes C(4) C(5) C(6) 109(1) . 1_555 1_555 yes C(4) C(5) C(10) 114(1) . 1_555 1_555 yes C(6) C(5) C(10) 111(1) . 1_555 1_555 yes C(5) C(6) C(7) 114(1) . 1_555 1_555 yes O(2) C(7) C(6) 111(1) . 1_555 1_555 yes O(2) C(7) C(8) 107(1) . 1_555 1_555 yes C(6) C(7) C(8) 111(1) . 1_555 1_555 yes C(7) C(8) C(9) 110.8(10) . 1_555 1_555 yes C(7) C(8) C(14) 109(1) . 1_555 1_555 yes C(9) C(8) C(14) 110(1) . 1_555 1_555 yes C(8) C(9) C(10) 112(1) . 1_555 1_555 yes C(8) C(9) C(11) 107(1) . 1_555 1_555 yes C(10) C(9) C(11) 115(1) . 1_555 1_555 yes C(1) C(10) C(5) 108(1) . 1_555 1_555 yes C(1) C(10) C(9) 111(1) . 1_555 1_555 yes C(1) C(10) C(19) 104(1) . 1_555 1_555 yes C(5) C(10) C(9) 111(1) . 1_555 1_555 yes C(5) C(10) C(19) 110(1) . 1_555 1_555 yes C(9) C(10) C(19) 110(1) . 1_555 1_555 yes C(9) C(11) C(12) 116(1) . 1_555 1_555 yes O(3) C(12) C(11) 106(1) . 1_555 1_555 yes O(3) C(12) C(13) 113(1) . 1_555 1_555 yes C(11) C(12) C(13) 109(1) . 1_555 1_555 yes C(12) C(13) C(14) 106.4(10) . 1_555 1_555 yes C(12) C(13) C(17) 116(1) . 1_555 1_555 yes C(12) C(13) C(18) 111(1) . 1_555 1_555 yes C(14) C(13) C(17) 97(1) . 1_555 1_555 yes C(14) C(13) C(18) 112(1) . 1_555 1_555 yes C(17) C(13) C(18) 111(1) . 1_555 1_555 yes C(8) C(14) C(13) 114(1) . 1_555 1_555 yes C(8) C(14) C(15) 120(1) . 1_555 1_555 yes C(13) C(14) C(15) 103(1) . 1_555 1_555 yes C(14) C(15) C(16) 105(1) . 1_555 1_555 yes C(15) C(16) C(17) 107(1) . 1_555 1_555 yes C(13) C(17) C(16) 102(1) . 1_555 1_555 yes C(13) C(17) C(20) 118(1) . 1_555 1_555 yes C(16) C(17) C(20) 111(1) . 1_555 1_555 yes C(17) C(20) C(21) 114(1) . 1_555 1_555 yes C(17) C(20) C(22) 109(1) . 1_555 1_555 yes C(21) C(20) C(22) 110(1) . 1_555 1_555 yes C(20) C(22) C(23) 117(1) . 1_555 1_555 yes C(22) C(23) C(24) 111(1) . 1_555 1_555 yes O(4) C(24) O(5) 125(1) . 1_555 1_555 yes O(4) C(24) C(23) 124(1) . 1_555 1_555 yes O(5) C(24) C(23) 110(1) . 1_555 1_555 yes N(1) C(25) C(26) 117(1) . 1_555 1_555 yes N(1) C(25) C(30) 122(1) . 1_555 1_555 yes C(26) C(25) C(30) 120(1) . 1_555 1_555 yes C(25) C(26) C(27) 118(1) . 1_555 1_555 yes C(25) C(26) C(31) 119(1) . 1_555 1_555 yes C(27) C(26) C(31) 122(1) . 1_555 1_555 yes C(26) C(27) C(28) 118(1) . 1_555 1_555 yes C(26) C(27) C(32) 118(1) . 1_555 1_555 yes C(28) C(27) C(32) 122(1) . 1_555 1_555 yes C(27) C(28) C(29) 120(1) . 1_555 1_555 yes C(28) C(29) C(30) 121(1) . 1_555 1_555 yes C(25) C(30) C(29) 120(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) C(2) C(1) -175(1) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 174(1) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -69(1) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 71(1) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -50(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 65(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -65(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 41(1) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 170(1) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -17(2) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 160(1) 1_555 1_555 1_555 1_555 yes N(1) C(25) C(26) C(27) -179(1) 1_555 1_555 1_555 1_555 yes N(1) C(25) C(26) C(31) -1(2) 1_555 1_555 1_555 1_555 yes N(1) C(25) C(30) C(29) 179(1) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -56(1) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 50(1) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 175(1) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -176(1) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 59(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -52(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 69(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -170(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 53(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 58(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -179(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 75(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -71(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 165(1) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 51(1) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -55(1) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) -178(1) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 53(1) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -69(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -51(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -173(1) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -52(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 54(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -177(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -175(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -51(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 67(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 55(1) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -59(1) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) -179(1) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 63(1) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -162(1) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 61(1) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -174(1) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -56(1) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) 176(1) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) -178(1) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -56(1) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -55(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 52(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 160(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -70(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 167(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -155(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 81(1) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -33(1) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 24(1) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -53(2) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) -178(1) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -42(1) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -166(1) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 5(1) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 47(1) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -69(1) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 152(1) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 75(1) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) -171(1) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 63(1) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -178(1) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -48(1) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 167(1) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 54(1) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 1(2) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(32) 178(1) 1_555 1_555 1_555 1_555 yes C(25) C(30) C(29) C(28) 0(2) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(30) C(29) -2(2) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) -3(2) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(30) 1(2) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 3(2) 1_555 1_555 1_555 1_555 yes C(28) C(27) C(26) C(31) -176(1) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(27) C(32) 178(1) 1_555 1_555 1_555 1_555 yes C(30) C(25) C(26) C(31) 179(1) 1_555 1_555 1_555 1_555 yes C(31) C(26) C(27) C(32) 0(2) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(2) 2.63(1) . 2_647 ? O(1) O(3) 2.85(1) . 2_657 ? O(2) O(5) 2.63(1) . 2_556 ? O(2) C(24) 3.41(2) . 2_556 ? O(2) O(4) 3.45(1) . 2_556 ? O(2) C(3) 3.56(2) . 2_657 ? O(2) C(2) 3.59(2) . 2_657 ? O(3) O(4) 2.85(1) . 2_546 ? O(3) N(1) 3.22(2) . . ? O(4) N(1) 3.29(2) . 2_556 ? O(4) C(21) 3.47(2) . 2_556 ? O(4) C(31) 3.55(2) . 2_556 ? O(5) C(14) 3.26(2) . 2_546 ? O(5) N(1) 3.36(2) . 2_546 ? O(5) C(15) 3.49(2) . 2_546 ? C(24) C(31) 3.57(3) . 2_556 ? #------------------------------------------------------------------------------ #===END data_1_2_4-Trimethylbenzene _database_code_depnum_ccdc_archive 'CCDC 297677' _audit_creation_date 'Thu Oct 28 11:10:29 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C33 H52 O5 ' _chemical_formula_moiety ? _chemical_formula_weight 528.77 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 11.9707(9) _cell_length_b 8.0690(5) _cell_length_c 16.220(1) _cell_angle_alpha 90 _cell_angle_beta 111.245(2) _cell_angle_gamma 90 _cell_volume 1460.3(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6626 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 68.2 _cell_measurement_temperature 198.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.460 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.190 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.620 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 0.915 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8356 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 68.23 _diffrn_measured_fraction_theta_max 0.9658 _diffrn_reflns_theta_full 68.23 _diffrn_measured_fraction_theta_full 0.9658 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -7.0 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 2794 _reflns_number_gt 1906 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1951 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2794 _refine_ls_number_parameters 344 _refine_ls_goodness_of_fit_ref 1.377 _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 0.0004 _refine_diff_density_max 0.30 _refine_diff_density_min -0.39 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -1.4(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ;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 0.049 0.032 ;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 1.1142(3) 0.526(2) 0.5974(2) 0.048(1) Uani 1.00 d . . . O(2) O 0.7529(3) 0.753(2) 0.3800(2) 0.0417(9) Uani 1.00 d . . . O(3) O 0.6952(3) 0.218(2) 0.2878(2) 0.049(1) Uani 1.00 d . . . O(4) O 0.2928(6) 0.443(2) -0.1781(3) 0.081(2) Uani 1.00 d . . . O(5) O 0.2245(4) 0.189(2) -0.2249(2) 0.056(1) Uani 1.00 d . . . C(1) C 0.8300(5) 0.319(2) 0.5958(3) 0.039(1) Uani 1.00 d . . . C(2) C 0.9524(5) 0.341(2) 0.5856(3) 0.040(1) Uani 1.00 d . . . C(3) C 1.0029(5) 0.509(2) 0.6142(3) 0.041(1) Uani 1.00 d . . . C(4) C 0.9153(4) 0.638(2) 0.5637(3) 0.039(1) Uani 1.00 d . . . C(5) C 0.7893(4) 0.626(2) 0.5698(3) 0.036(1) Uani 1.00 d . . . C(6) C 0.7070(5) 0.764(2) 0.5163(3) 0.040(1) Uani 1.00 d . . . C(7) C 0.6594(5) 0.735(2) 0.4160(3) 0.041(1) Uani 1.00 d . . . C(8) C 0.6053(4) 0.562(2) 0.3926(3) 0.036(1) Uani 1.00 d . . . C(9) C 0.6902(4) 0.425(2) 0.4434(3) 0.034(1) Uani 1.00 d . . . C(10) C 0.7345(5) 0.448(2) 0.5452(3) 0.039(1) Uani 1.00 d . . . C(11) C 0.6327(4) 0.257(2) 0.4113(3) 0.038(1) Uani 1.00 d . . . C(12) C 0.5904(5) 0.227(2) 0.3110(3) 0.039(1) Uani 1.00 d . . . C(13) C 0.5026(5) 0.363(2) 0.2614(3) 0.037(1) Uani 1.00 d . . . C(14) C 0.5656(4) 0.534(2) 0.2941(3) 0.037(1) Uani 1.00 d . . . C(15) C 0.4849(5) 0.658(2) 0.2315(3) 0.045(1) Uani 1.00 d . . . C(16) C 0.4373(5) 0.573(2) 0.1426(3) 0.051(1) Uani 1.00 d . . . C(17) C 0.4737(5) 0.385(2) 0.1595(3) 0.045(1) Uani 1.00 d . . . C(18) C 0.3850(5) 0.348(2) 0.2783(3) 0.043(1) Uani 1.00 d . . . C(19) C 0.6297(5) 0.431(2) 0.5780(3) 0.042(1) Uani 1.00 d . . . C(20) C 0.3838(5) 0.269(2) 0.0936(3) 0.048(1) Uani 1.00 d . . . C(21) C 0.4173(8) 0.090(2) 0.1100(4) 0.072(2) Uani 1.00 d . . . C(22) C 0.3723(6) 0.321(2) -0.0002(3) 0.057(2) Uani 1.00 d . . . C(23) C 0.2732(7) 0.244(2) -0.0738(3) 0.072(2) Uani 1.00 d . . . C(24) C 0.2636(5) 0.305(2) -0.1649(4) 0.055(1) Uani 1.00 d . . . C(25) C 0.993(1) 0.433(3) 0.1373(8) 0.110(4) Uani 1.00 d . . . C(26) C 0.889(2) 0.365(3) 0.0830(8) 0.157(5) Uani 1.00 d . . . C(27) C 0.857(1) 0.369(2) -0.0084(8) 0.117(4) Uani 1.00 d . . . C(28) C 0.933(1) 0.426(3) -0.0488(7) 0.145(5) Uani 1.00 d . . . C(29) C 1.032(1) 0.513(3) 0.0035(10) 0.152(6) Uani 1.00 d . . . C(30) C 1.064(1) 0.508(3) 0.0986(8) 0.120(4) Uani 1.00 d . . . C(31) C 1.028(1) 0.430(3) 0.2341(8) 0.154(6) Uani 1.00 d . . . C(32) C 0.799(2) 0.292(3) 0.121(2) 0.22(1) Uani 1.00 d . . . C(33) C 0.899(2) 0.446(4) -0.1478(9) 0.24(1) Uani 1.00 d . . . H(1) H 0.7999 0.2088 0.5742 0.0465 Uiso 1.00 calc . . . H(2) H 0.8413 0.3233 0.6566 0.0465 Uiso 1.00 calc . . . H(3) H 1.0064 0.2579 0.6213 0.0494 Uiso 1.00 calc . . . H(4) H 0.9425 0.3224 0.5256 0.0494 Uiso 1.00 calc . . . H(5) H 1.0178 0.5221 0.6758 0.0503 Uiso 1.00 calc . . . H(6) H 0.9482 0.7422 0.5848 0.0473 Uiso 1.00 calc . . . H(7) H 0.9064 0.6262 0.5030 0.0473 Uiso 1.00 calc . . . H(8) H 0.7999 0.6419 0.6303 0.0437 Uiso 1.00 calc . . . H(9) H 0.6414 0.7747 0.5355 0.0491 Uiso 1.00 calc . . . H(10) H 0.7522 0.8651 0.5288 0.0491 Uiso 1.00 calc . . . H(11) H 0.5990 0.8148 0.3895 0.0489 Uiso 1.00 calc . . . H(12) H 0.5357 0.5528 0.4077 0.0445 Uiso 1.00 calc . . . H(13) H 0.7597 0.4298 0.4271 0.0417 Uiso 1.00 calc . . . H(14) H 0.6896 0.1707 0.4392 0.0467 Uiso 1.00 calc . . . H(15) H 0.5654 0.2438 0.4286 0.0467 Uiso 1.00 calc . . . H(16) H 0.5488 0.1240 0.2979 0.0443 Uiso 1.00 calc . . . H(17) H 0.6379 0.5286 0.2806 0.0456 Uiso 1.00 calc . . . H(18) H 0.4219 0.6846 0.2506 0.0556 Uiso 1.00 calc . . . H(19) H 0.5293 0.7519 0.2286 0.0556 Uiso 1.00 calc . . . H(20) H 0.3520 0.5812 0.1171 0.0611 Uiso 1.00 calc . . . H(21) H 0.4709 0.6184 0.1029 0.0611 Uiso 1.00 calc . . . H(22) H 0.5471 0.3720 0.1502 0.0566 Uiso 1.00 calc . . . H(23) H 0.3985 0.3561 0.3394 0.0529 Uiso 1.00 calc . . . H(24) H 0.3292 0.4309 0.2468 0.0529 Uiso 1.00 calc . . . H(25) H 0.3483 0.2409 0.2577 0.0529 Uiso 1.00 calc . . . H(26) H 0.6565 0.4523 0.6397 0.0525 Uiso 1.00 calc . . . H(27) H 0.5692 0.5106 0.5478 0.0525 Uiso 1.00 calc . . . H(28) H 0.5954 0.3232 0.5663 0.0525 Uiso 1.00 calc . . . H(29) H 0.3081 0.2813 0.0998 0.0580 Uiso 1.00 calc . . . H(30) H 0.4239 0.0546 0.1670 0.0879 Uiso 1.00 calc . . . H(31) H 0.3608 0.0201 0.0666 0.0879 Uiso 1.00 calc . . . H(32) H 0.4950 0.0704 0.1042 0.0879 Uiso 1.00 calc . . . H(33) H 0.3609 0.4371 -0.0043 0.0657 Uiso 1.00 calc . . . H(34) H 0.4447 0.2928 -0.0078 0.0657 Uiso 1.00 calc . . . H(35) H 0.2824 0.1259 -0.0709 0.0903 Uiso 1.00 calc . . . H(36) H 0.1981 0.2687 -0.0664 0.0903 Uiso 1.00 calc . . . H(37) H 1.1656 0.5919 0.6392 0.0777 Uiso 1.00 calc . . . H(38) H 0.7963 0.8507 0.3838 0.0777 Uiso 1.00 calc . . . H(39) H 0.7001 0.1119 0.2520 0.2204 Uiso 1.00 calc . . . H(40) H 0.2513 0.2211 -0.2771 0.0777 Uiso 1.00 calc . . . H(41) H 0.7817 0.3232 -0.0437 0.1567 Uiso 1.00 calc . . . H(42) H 1.0747 0.5856 -0.0237 0.1666 Uiso 1.00 calc . . . H(43) H 1.1469 0.5359 0.1374 0.1422 Uiso 1.00 calc . . . H(44) H 1.0302 0.3028 0.2494 0.2085 Uiso 1.00 calc . . . H(45) H 1.0996 0.4694 0.2660 0.2085 Uiso 1.00 calc . . . H(46) H 0.9638 0.4676 0.2499 0.2085 Uiso 1.00 calc . . . H(47) H 0.7237 0.3552 0.1005 0.2194 Uiso 1.00 calc . . . H(48) H 0.7777 0.1794 0.1038 0.2194 Uiso 1.00 calc . . . H(49) H 0.8290 0.2976 0.1842 0.2194 Uiso 1.00 calc . . . H(50) H 0.8728 0.5493 -0.1700 0.2282 Uiso 1.00 calc . . . H(51) H 0.9528 0.3976 -0.1692 0.2282 Uiso 1.00 calc . . . H(52) H 0.8207 0.3714 -0.1775 0.2282 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) 0.031(2) 0.058(2) 0.050(2) -0.001(2) 0.008(1) -0.005(2) O(2) 0.038(2) 0.050(2) 0.036(2) -0.004(2) 0.012(1) 0.002(2) O(3) 0.037(2) 0.067(3) 0.040(2) 0.010(2) 0.012(1) 0.002(2) O(4) 0.107(4) 0.079(3) 0.043(2) -0.033(3) 0.011(2) 0.002(3) O(5) 0.053(2) 0.076(3) 0.036(2) -0.004(2) 0.012(2) -0.002(2) C(1) 0.035(2) 0.050(3) 0.026(2) 0.003(2) 0.005(2) 0.004(2) C(2) 0.034(2) 0.046(3) 0.037(2) 0.003(2) 0.008(2) 0.004(2) C(3) 0.034(2) 0.051(3) 0.034(2) -0.006(2) 0.007(2) -0.003(2) C(4) 0.025(2) 0.055(3) 0.031(2) -0.010(2) 0.002(2) -0.002(2) C(5) 0.033(2) 0.050(3) 0.026(2) 0.000(2) 0.011(2) -0.002(2) C(6) 0.035(3) 0.051(3) 0.033(2) 0.004(2) 0.009(2) -0.005(2) C(7) 0.037(2) 0.050(3) 0.033(2) 0.002(2) 0.011(2) -0.004(2) C(8) 0.027(2) 0.049(2) 0.032(2) 0.001(2) 0.011(2) 0.001(2) C(9) 0.023(2) 0.049(2) 0.029(2) 0.005(2) 0.009(2) -0.002(2) C(10) 0.033(2) 0.050(3) 0.029(2) -0.002(2) 0.006(2) 0.003(2) C(11) 0.032(2) 0.048(3) 0.029(2) 0.004(2) 0.004(2) 0.004(2) C(12) 0.035(2) 0.045(3) 0.028(2) 0.002(2) 0.002(2) 0.001(2) C(13) 0.031(2) 0.047(3) 0.026(2) 0.000(2) 0.004(2) 0.005(2) C(14) 0.025(2) 0.052(3) 0.031(2) -0.004(2) 0.007(2) 0.002(2) C(15) 0.035(3) 0.055(3) 0.035(2) -0.002(3) 0.000(2) 0.007(2) C(16) 0.043(3) 0.068(3) 0.031(2) -0.005(3) 0.002(2) 0.010(2) C(17) 0.034(3) 0.070(3) 0.027(2) -0.002(3) 0.005(2) -0.004(2) C(18) 0.030(2) 0.062(4) 0.031(2) -0.004(3) 0.003(2) 0.004(3) C(19) 0.035(2) 0.060(4) 0.032(2) -0.003(3) 0.012(2) -0.001(3) C(20) 0.043(3) 0.067(3) 0.025(2) 0.004(3) 0.002(2) -0.008(2) C(21) 0.092(6) 0.066(4) 0.036(3) 0.012(4) -0.002(3) -0.006(3) C(22) 0.046(3) 0.090(5) 0.027(2) 0.006(3) 0.004(2) -0.001(3) C(23) 0.076(5) 0.102(6) 0.025(2) -0.027(5) 0.001(3) -0.002(3) C(24) 0.039(3) 0.084(3) 0.029(2) -0.016(3) -0.001(2) -0.002(2) C(25) 0.107(7) 0.137(10) 0.098(4) 0.043(7) 0.054(4) 0.037(7) C(26) 0.154(9) 0.16(1) 0.101(5) 0.048(9) -0.024(5) -0.035(8) C(27) 0.112(9) 0.14(1) 0.110(5) -0.013(8) 0.046(6) -0.031(9) C(28) 0.100(8) 0.25(2) 0.074(5) 0.014(10) 0.018(5) 0.013(9) C(29) 0.11(1) 0.24(2) 0.106(5) -0.03(1) 0.047(7) 0.02(1) C(30) 0.078(6) 0.17(1) 0.103(5) 0.001(8) 0.023(5) 0.008(9) C(31) 0.17(1) 0.19(2) 0.097(5) 0.09(1) 0.040(8) 0.04(1) C(32) 0.25(2) 0.15(1) 0.37(3) -0.01(2) 0.25(2) 0.01(2) C(33) 0.29(2) 0.33(3) 0.078(6) 0.11(3) 0.05(1) 0.05(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.460(8) . . yes O(2) C(7) 1.446(7) . . yes O(3) C(12) 1.436(8) . . yes O(4) C(24) 1.20(1) . . yes O(5) C(24) 1.308(10) . . yes C(1) C(2) 1.543(9) . . yes C(1) C(10) 1.546(9) . . yes C(2) C(3) 1.487(10) . . yes C(3) C(4) 1.499(10) . . yes C(4) C(5) 1.550(8) . . yes C(5) C(6) 1.530(9) . . yes C(5) C(10) 1.57(1) . . yes C(6) C(7) 1.534(8) . . yes C(7) C(8) 1.53(1) . . yes C(8) C(9) 1.528(8) . . yes C(8) C(14) 1.509(8) . . yes C(9) C(10) 1.551(8) . . yes C(9) C(11) 1.524(10) . . yes C(10) C(19) 1.536(9) . . yes C(11) C(12) 1.538(7) . . yes C(12) C(13) 1.534(8) . . yes C(13) C(14) 1.568(9) . . yes C(13) C(17) 1.571(8) . . yes C(13) C(18) 1.534(9) . . yes C(14) C(15) 1.502(9) . . yes C(15) C(16) 1.511(10) . . yes C(16) C(17) 1.57(1) . . yes C(17) C(20) 1.531(9) . . yes C(20) C(21) 1.50(1) . . yes C(20) C(22) 1.536(9) . . yes C(22) C(23) 1.484(10) . . yes C(23) C(24) 1.52(1) . . yes C(25) C(26) 1.35(2) . . yes C(25) C(30) 1.37(2) . . yes C(25) C(31) 1.47(2) . . yes C(26) C(27) 1.39(2) . . yes C(26) C(32) 1.54(3) . . yes C(27) C(28) 1.38(2) . . yes C(28) C(29) 1.38(2) . . yes C(28) C(33) 1.52(2) . . yes C(29) C(30) 1.45(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 C(2) C(1) C(10) 114.4(5) . 1_555 1_555 yes C(1) C(2) C(3) 111.5(6) . 1_555 1_555 yes O(1) C(3) C(2) 108.8(6) . 1_555 1_555 yes O(1) C(3) C(4) 109.7(6) . 1_555 1_555 yes C(2) C(3) C(4) 109.9(5) . 1_555 1_555 yes C(3) C(4) C(5) 115.2(6) . 1_555 1_555 yes C(4) C(5) C(6) 111.0(5) . 1_555 1_555 yes C(4) C(5) C(10) 111.6(5) . 1_555 1_555 yes C(6) C(5) C(10) 113.4(5) . 1_555 1_555 yes C(5) C(6) C(7) 114.0(5) . 1_555 1_555 yes O(2) C(7) C(6) 111.6(5) . 1_555 1_555 yes O(2) C(7) C(8) 108.2(5) . 1_555 1_555 yes C(6) C(7) C(8) 111.4(6) . 1_555 1_555 yes C(7) C(8) C(9) 112.9(5) . 1_555 1_555 yes C(7) C(8) C(14) 110.1(5) . 1_555 1_555 yes C(9) C(8) C(14) 110.8(5) . 1_555 1_555 yes C(8) C(9) C(10) 113.0(5) . 1_555 1_555 yes C(8) C(9) C(11) 109.3(4) . 1_555 1_555 yes C(10) C(9) C(11) 114.1(5) . 1_555 1_555 yes C(1) C(10) C(5) 108.8(5) . 1_555 1_555 yes C(1) C(10) C(9) 112.7(5) . 1_555 1_555 yes C(1) C(10) C(19) 107.1(5) . 1_555 1_555 yes C(5) C(10) C(9) 109.3(5) . 1_555 1_555 yes C(5) C(10) C(19) 108.2(6) . 1_555 1_555 yes C(9) C(10) C(19) 110.6(5) . 1_555 1_555 yes C(9) C(11) C(12) 115.9(5) . 1_555 1_555 yes O(3) C(12) C(11) 107.5(5) . 1_555 1_555 yes O(3) C(12) C(13) 113.3(5) . 1_555 1_555 yes C(11) C(12) C(13) 109.9(5) . 1_555 1_555 yes C(12) C(13) C(14) 107.5(5) . 1_555 1_555 yes C(12) C(13) C(17) 118.7(6) . 1_555 1_555 yes C(12) C(13) C(18) 110.3(5) . 1_555 1_555 yes C(14) C(13) C(17) 98.8(5) . 1_555 1_555 yes C(14) C(13) C(18) 111.7(6) . 1_555 1_555 yes C(17) C(13) C(18) 109.4(5) . 1_555 1_555 yes C(8) C(14) C(13) 114.7(5) . 1_555 1_555 yes C(8) C(14) C(15) 119.6(6) . 1_555 1_555 yes C(13) C(14) C(15) 104.2(5) . 1_555 1_555 yes C(14) C(15) C(16) 105.6(6) . 1_555 1_555 yes C(15) C(16) C(17) 106.7(5) . 1_555 1_555 yes C(13) C(17) C(16) 103.5(5) . 1_555 1_555 yes C(13) C(17) C(20) 119.7(6) . 1_555 1_555 yes C(16) C(17) C(20) 112.8(5) . 1_555 1_555 yes C(17) C(20) C(21) 113.1(6) . 1_555 1_555 yes C(17) C(20) C(22) 108.2(7) . 1_555 1_555 yes C(21) C(20) C(22) 111.2(7) . 1_555 1_555 yes C(20) C(22) C(23) 116.1(7) . 1_555 1_555 yes C(22) C(23) C(24) 113.6(7) . 1_555 1_555 yes O(4) C(24) O(5) 125.2(7) . 1_555 1_555 yes O(4) C(24) C(23) 123.2(7) . 1_555 1_555 yes O(5) C(24) C(23) 111.6(7) . 1_555 1_555 yes C(26) C(25) C(30) 117(1) . 1_555 1_555 yes C(26) C(25) C(31) 122(1) . 1_555 1_555 yes C(30) C(25) C(31) 120(1) . 1_555 1_555 yes C(25) C(26) C(27) 121(2) . 1_555 1_555 yes C(25) C(26) C(32) 120(1) . 1_555 1_555 yes C(27) C(26) C(32) 118(1) . 1_555 1_555 yes C(26) C(27) C(28) 122(1) . 1_555 1_555 yes C(27) C(28) C(29) 116(1) . 1_555 1_555 yes C(27) C(28) C(33) 124(1) . 1_555 1_555 yes C(29) C(28) C(33) 115(2) . 1_555 1_555 yes C(28) C(29) C(30) 118(1) . 1_555 1_555 yes C(25) C(30) C(29) 122(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) C(2) C(1) -176.2(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 175.5(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -70.8(8) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 70.6(6) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -53.9(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 67.6(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -66.8(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 44.0(8) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 171.2(5) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -29(1) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 147.7(8) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -56.0(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 47.8(6) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 174.1(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -174.2(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 60.0(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -51.6(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 69.9(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -168.3(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 55.9(7) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 57.1(7) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 179.9(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -52.5(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 75.9(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -75.7(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 163.9(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 50.3(7) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -53.1(7) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) -178.8(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 50.6(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -69.9(6) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -52.4(7) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -176.9(5) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -50.7(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 55.7(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -176.0(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -177.1(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -52.2(7) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 66.0(7) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 53.8(6) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -57.5(7) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 178.6(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 63.6(7) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -165.5(6) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 57.3(7) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -177.9(5) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -56.2(7) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) 179.7(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) -178.5(5) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -52.0(6) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -59.8(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 53.5(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 164.3(6) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -68.5(7) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 169.9(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -153.8(6) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 79.6(8) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -35.7(7) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 18.6(7) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -57.3(9) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 179.1(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -38.3(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -164.9(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 10.4(7) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 46.0(6) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -69.0(6) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 149.4(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.5(7) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) -179.3(7) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 57.1(8) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -169.3(8) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -48.0(9) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 177.7(8) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 66(1) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 6(3) 1_555 1_555 1_555 1_555 yes C(25) C(30) C(29) C(28) -6(3) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(30) C(29) -1(3) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) -13(3) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(33) -174(2) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(30) 0(2) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(31) 179(1) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 12(3) 1_555 1_555 1_555 1_555 yes C(28) C(27) C(26) C(32) -177(1) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(25) C(31) 179(1) 1_555 1_555 1_555 1_555 yes C(30) C(25) C(26) C(32) -174(1) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(28) C(33) 175(2) 1_555 1_555 1_555 1_555 yes C(31) C(25) C(26) C(32) 4(2) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(2) 2.658(7) . 2_746 ? O(1) O(3) 2.829(7) . 2_756 ? O(1) O(4) 3.555(7) . 1_656 ? O(2) O(5) 2.677(6) . 2_655 ? O(2) C(2) 3.439(8) . 2_756 ? O(2) C(24) 3.447(8) . 2_655 ? O(2) O(4) 3.473(7) . 2_655 ? O(2) C(3) 3.548(9) . 2_756 ? O(3) O(4) 2.881(8) . 2_645 ? O(3) C(32) 3.41(2) . . ? O(4) C(32) 3.27(2) . 2_655 ? O(4) C(21) 3.45(1) . 2_655 ? O(5) C(14) 3.345(8) . 2_645 ? O(5) C(15) 3.527(9) . 2_645 ? C(21) C(27) 3.57(2) . 2_645 ? C(23) C(26) 3.60(2) . 2_645 ? C(26) C(29) 3.44(3) . 2_745 ? C(27) C(29) 3.15(3) . 2_745 ? C(27) C(30) 3.53(2) . 2_745 ? C(28) C(29) 3.40(4) . 2_745 ? C(28) C(30) 3.47(3) . 2_745 ? #------------------------------------------------------------------------------ #===END data_2cl-p-xylene _database_code_depnum_ccdc_archive 'CCDC 297678' _audit_creation_date 'Thu Oct 28 11:18:34 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C32 H49 Cl O5 ' _chemical_formula_moiety 'C32 H49 Cl O5 ' _chemical_formula_weight 549.19 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 12.078(1) _cell_length_b 8.0989(9) _cell_length_c 16.226(2) _cell_angle_alpha 90 _cell_angle_beta 111.031(6) _cell_angle_gamma 90 _cell_volume 1481.4(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3227 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 67.2 _cell_measurement_temperature 203.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.441 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.392 _exptl_absorpt_correction_T_max 0.539 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5334 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 68.20 _diffrn_measured_fraction_theta_max 0.9396 _diffrn_reflns_theta_full 68.20 _diffrn_measured_fraction_theta_full 0.9396 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # 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 2752 _reflns_number_gt 2386 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1995 _refine_ls_wR_factor_ref 0.4387 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2752 _refine_ls_number_parameters 263 _refine_ls_goodness_of_fit_ref 3.447 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.10000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0041 _refine_diff_density_max 2.15 _refine_diff_density_min -0.48 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 1.1(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.364 0.702 ;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 0.6121(3) 0.4347(7) 0.5986(3) 0.0609(10) Uani 1.00 d . . . O(2) O 0.2551(3) 0.6628(7) 0.3807(2) 0.0550(9) Uani 1.00 d . . . O(3) O 0.1989(3) 0.1319(7) 0.2891(2) 0.0605(10) Uani 1.00 d . . . O(4) O -0.2175(8) 0.3633(9) -0.1759(4) 0.122(2) Uani 1.00 d . . . O(5) O -0.2738(4) 0.1105(9) -0.2214(3) 0.083(1) Uani 1.00 d . . . C(1) C 0.3305(5) 0.2319(8) 0.5960(3) 0.052(1) Uani 1.00 d . . . C(2) C 0.4496(5) 0.2468(8) 0.5849(3) 0.053(1) Uani 1.00 d . . . C(3) C 0.5019(4) 0.4192(8) 0.6148(3) 0.052(1) Uani 1.00 d . . . C(4) C 0.4150(4) 0.5479(8) 0.5624(3) 0.050(1) Uani 1.00 d . . . C(5) C 0.2928(4) 0.5310(8) 0.5694(3) 0.048(1) Uani 1.00 d . . . C(6) C 0.2104(4) 0.6702(8) 0.5167(3) 0.052(1) Uani 1.00 d . . . C(7) C 0.1639(4) 0.6447(8) 0.4178(3) 0.048(1) Uani 1.00 d . . . C(8) C 0.1100(4) 0.4732(8) 0.3947(3) 0.0445(10) Uani 1.00 d . . . C(9) C 0.1945(4) 0.3324(7) 0.4451(3) 0.0415(9) Uani 1.00 d . . . C(10) C 0.2376(4) 0.3584(8) 0.5470(3) 0.048(1) Uani 1.00 d . . . C(11) C 0.1383(4) 0.1666(8) 0.4134(3) 0.048(1) Uani 1.00 d . . . C(12) C 0.0948(5) 0.1384(8) 0.3126(3) 0.052(1) Uani 1.00 d . . . C(13) C 0.0095(4) 0.2735(8) 0.2627(3) 0.047(1) Uani 1.00 d . . . C(14) C 0.0711(4) 0.4432(8) 0.2950(3) 0.047(1) Uani 1.00 d . . . C(15) C -0.0109(5) 0.5661(9) 0.2334(4) 0.062(1) Uani 1.00 d . . . C(16) C -0.0595(5) 0.4737(10) 0.1438(4) 0.068(1) Uani 1.00 d . . . C(17) C -0.0198(4) 0.2965(9) 0.1615(3) 0.055(1) Uani 1.00 d . . . C(18) C -0.1070(4) 0.2545(8) 0.2801(3) 0.054(1) Uani 1.00 d . . . C(19) C 0.1333(5) 0.3397(9) 0.5800(3) 0.057(1) Uani 1.00 d . . . C(20) C -0.1078(5) 0.1790(10) 0.0959(3) 0.066(1) Uani 1.00 d . . . C(21) C -0.0718(9) -0.004(1) 0.1129(6) 0.101(2) Uani 1.00 d . . . C(22) C -0.1211(6) 0.229(1) 0.0005(4) 0.075(2) Uani 1.00 d . . . C(23) C -0.2261(6) 0.161(1) -0.0715(4) 0.084(2) Uani 1.00 d . . . C(24) C -0.2357(6) 0.224(1) -0.1596(4) 0.073(1) Uani 1.00 d . . . H(1) H 0.2999 0.1252 0.5757 0.0594 Uiso 1.00 calc . . . H(2) H 0.3438 0.2416 0.6570 0.0594 Uiso 1.00 calc . . . H(3) H 0.5031 0.1660 0.6196 0.0619 Uiso 1.00 calc . . . H(4) H 0.4403 0.2323 0.5245 0.0619 Uiso 1.00 calc . . . H(5) H 0.5162 0.4334 0.6761 0.0596 Uiso 1.00 calc . . . H(6) H 0.4462 0.6533 0.5836 0.0587 Uiso 1.00 calc . . . H(7) H 0.4067 0.5366 0.5024 0.0587 Uiso 1.00 calc . . . H(8) H 0.3045 0.5503 0.6296 0.0540 Uiso 1.00 calc . . . H(9) H 0.1447 0.6788 0.5357 0.0596 Uiso 1.00 calc . . . H(10) H 0.2532 0.7726 0.5293 0.0596 Uiso 1.00 calc . . . H(11) H 0.1028 0.7248 0.3909 0.0542 Uiso 1.00 calc . . . H(12) H 0.0413 0.4675 0.4100 0.0513 Uiso 1.00 calc . . . H(13) H 0.2628 0.3410 0.4290 0.0488 Uiso 1.00 calc . . . H(14) H 0.1952 0.0841 0.4399 0.0564 Uiso 1.00 calc . . . H(15) H 0.0720 0.1549 0.4309 0.0564 Uiso 1.00 calc . . . H(16) H 0.0548 0.0367 0.2994 0.0623 Uiso 1.00 calc . . . H(17) H 0.1414 0.4429 0.2817 0.0543 Uiso 1.00 calc . . . H(18) H -0.0735 0.5950 0.2535 0.0739 Uiso 1.00 calc . . . H(19) H 0.0311 0.6628 0.2294 0.0739 Uiso 1.00 calc . . . H(20) H -0.1441 0.4804 0.1199 0.0802 Uiso 1.00 calc . . . H(21) H -0.0288 0.5227 0.1029 0.0802 Uiso 1.00 calc . . . H(22) H 0.0530 0.2869 0.1518 0.0641 Uiso 1.00 calc . . . H(23) H -0.0912 0.2652 0.3415 0.0618 Uiso 1.00 calc . . . H(24) H -0.1608 0.3387 0.2490 0.0618 Uiso 1.00 calc . . . H(25) H -0.1405 0.1496 0.2602 0.0618 Uiso 1.00 calc . . . H(26) H 0.1600 0.3637 0.6416 0.0687 Uiso 1.00 calc . . . H(27) H 0.0725 0.4192 0.5498 0.0687 Uiso 1.00 calc . . . H(28) H 0.1013 0.2333 0.5690 0.0687 Uiso 1.00 calc . . . H(29) H -0.1819 0.1931 0.1022 0.0777 Uiso 1.00 calc . . . H(30) H -0.1326 -0.0691 0.0718 0.1190 Uiso 1.00 calc . . . H(31) H 0.0005 -0.0208 0.1040 0.1190 Uiso 1.00 calc . . . H(32) H -0.0642 -0.0319 0.1709 0.1190 Uiso 1.00 calc . . . H(33) H -0.1268 0.3478 -0.0035 0.0882 Uiso 1.00 calc . . . H(34) H -0.0521 0.1960 -0.0101 0.0882 Uiso 1.00 calc . . . H(35) H -0.2177 0.0455 -0.0704 0.1007 Uiso 1.00 calc . . . H(36) H -0.2944 0.1918 -0.0598 0.1007 Uiso 1.00 calc . . . H(37) H 0.6661 0.3525 0.6308 0.0707 Uiso 1.00 calc . . . H(38) H 0.2788 0.7660 0.3789 0.1077 Uiso 1.00 calc . . . H(39) H 0.1755 0.1090 0.2279 0.0710 Uiso 1.00 calc . . . H(40) H -0.2171 0.0966 -0.2492 0.0943 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) 0.042(1) 0.070(2) 0.067(2) 0.002(2) 0.016(1) 0.000(2) O(2) 0.056(2) 0.059(2) 0.056(2) -0.003(2) 0.027(1) 0.008(2) O(3) 0.059(2) 0.075(2) 0.045(2) 0.020(2) 0.015(1) 0.003(2) O(4) 0.191(7) 0.094(3) 0.057(3) -0.051(4) 0.016(3) -0.002(3) O(5) 0.085(3) 0.106(4) 0.065(2) -0.002(3) 0.037(2) -0.008(2) C(1) 0.057(2) 0.057(3) 0.036(2) -0.003(2) 0.011(2) 0.007(2) C(2) 0.052(2) 0.058(2) 0.046(2) 0.010(2) 0.013(2) -0.002(2) C(3) 0.043(2) 0.064(2) 0.043(2) -0.002(2) 0.008(2) 0.002(2) C(4) 0.042(2) 0.055(3) 0.050(2) -0.007(2) 0.012(2) -0.002(2) C(5) 0.048(2) 0.061(2) 0.038(2) 0.007(2) 0.018(2) -0.002(2) C(6) 0.055(2) 0.051(3) 0.053(2) 0.006(2) 0.023(2) -0.009(2) C(7) 0.050(2) 0.047(2) 0.050(2) 0.002(2) 0.021(2) -0.001(2) C(8) 0.041(2) 0.050(2) 0.042(2) 0.003(2) 0.013(2) -0.001(2) C(9) 0.042(2) 0.053(2) 0.033(2) 0.006(2) 0.016(1) 0.004(2) C(10) 0.041(2) 0.066(2) 0.036(2) 0.000(2) 0.013(2) -0.005(2) C(11) 0.049(2) 0.052(2) 0.036(2) 0.000(2) 0.008(2) 0.007(2) C(12) 0.064(2) 0.054(3) 0.040(2) 0.001(2) 0.020(2) -0.001(2) C(13) 0.047(2) 0.059(2) 0.037(2) -0.003(2) 0.017(2) -0.001(2) C(14) 0.048(2) 0.055(2) 0.039(2) -0.003(2) 0.017(2) 0.007(2) C(15) 0.063(3) 0.063(3) 0.051(3) 0.014(2) 0.010(2) 0.009(2) C(16) 0.065(3) 0.081(3) 0.044(2) 0.003(3) 0.004(2) 0.014(2) C(17) 0.047(2) 0.080(3) 0.037(2) 0.006(2) 0.014(2) 0.012(2) C(18) 0.046(2) 0.065(3) 0.049(2) -0.008(2) 0.014(2) 0.006(2) C(19) 0.060(2) 0.075(4) 0.052(2) -0.011(3) 0.037(2) -0.005(2) C(20) 0.070(3) 0.086(3) 0.035(2) 0.003(3) 0.010(2) 0.002(2) C(21) 0.126(6) 0.080(3) 0.064(4) -0.008(4) -0.005(4) -0.008(3) C(22) 0.065(3) 0.124(6) 0.038(2) 0.001(3) 0.020(2) 0.004(3) C(23) 0.078(4) 0.121(6) 0.046(2) -0.015(4) 0.014(2) 0.011(3) C(24) 0.067(3) 0.097(3) 0.047(2) 0.000(3) 0.009(2) 0.016(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 109.4(3) . . . . 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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. O1 N1 1.541(1) . . yes #------------------------------------------------------------------------------ #===END data_2_4-Dichlorotoluene _database_code_depnum_ccdc_archive 'CCDC 297679' _audit_creation_date 'Thu Oct 28 11:14:55 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C31 H46 Cl2 O5 ' _chemical_formula_moiety ? _chemical_formula_weight 569.61 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 12.083(2) _cell_length_b 8.1351(5) _cell_length_c 16.265(1) _cell_angle_alpha 90 _cell_angle_beta 111.618(6) _cell_angle_gamma 90 _cell_volume 1486.3(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2426 _cell_measurement_theta_min 6.2 _cell_measurement_theta_max 68.2 _cell_measurement_temperature 203.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.264 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.394 _exptl_absorpt_correction_T_max 0.719 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5496 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 68.23 _diffrn_measured_fraction_theta_max 0.9526 _diffrn_reflns_theta_full 68.23 _diffrn_measured_fraction_theta_full 0.9526 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # 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 2797 _reflns_number_gt 2298 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2202 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2797 _refine_ls_number_parameters 344 _refine_ls_goodness_of_fit_ref 1.986 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.07000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0029 _refine_diff_density_max 0.83 _refine_diff_density_min -0.62 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.4(1) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.364 0.702 ;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 -0.7262(4) -0.700(2) -0.8982(3) 0.185(2) Uani 1.00 d . . . Cl(2) Cl -0.6016(5) -0.503(2) -1.1638(2) 0.193(2) Uani 1.00 d . . . O(1) O -0.3874(3) -0.449(1) -0.4021(2) 0.0482(9) Uani 1.00 d . . . O(2) O -0.7467(3) -0.218(1) -0.6171(2) 0.0401(8) Uani 1.00 d . . . O(3) O -0.8036(3) -0.748(1) -0.7120(2) 0.0487(9) Uani 1.00 d . . . O(4) O -1.2020(5) -0.529(2) -1.1796(2) 0.081(1) Uani 1.00 d . . . O(5) O -1.2739(4) -0.775(2) -1.2249(2) 0.057(1) Uani 1.00 d . . . C(1) C -0.6682(4) -0.655(2) -0.4046(3) 0.0397(10) Uani 1.00 d . . . C(2) C -0.5477(4) -0.636(2) -0.4156(3) 0.040(1) Uani 1.00 d . . . C(3) C -0.4962(4) -0.467(2) -0.3846(3) 0.0400(9) Uani 1.00 d . . . C(4) C -0.5838(4) -0.338(2) -0.4351(3) 0.039(1) Uani 1.00 d . . . C(5) C -0.7065(4) -0.352(2) -0.4288(2) 0.0354(9) Uani 1.00 d . . . C(6) C -0.7896(4) -0.214(2) -0.4809(3) 0.041(1) Uani 1.00 d . . . C(7) C -0.8390(4) -0.241(2) -0.5806(3) 0.0359(9) Uani 1.00 d . . . C(8) C -0.8927(4) -0.410(2) -0.6058(2) 0.0325(9) Uani 1.00 d . . . C(9) C -0.8078(4) -0.548(2) -0.5568(2) 0.0314(9) Uani 1.00 d . . . C(10) C -0.7619(4) -0.526(2) -0.4541(2) 0.0346(9) Uani 1.00 d . . . C(11) C -0.8643(4) -0.718(2) -0.5888(2) 0.0362(10) Uani 1.00 d . . . C(12) C -0.9082(4) -0.744(1) -0.6893(2) 0.039(1) Uani 1.00 d . . . C(13) C -0.9941(4) -0.604(2) -0.7386(2) 0.0333(9) Uani 1.00 d . . . C(14) C -0.9329(4) -0.438(2) -0.7055(2) 0.0327(9) Uani 1.00 d . . . C(15) C -1.0141(4) -0.310(2) -0.7658(3) 0.043(1) Uani 1.00 d . . . C(16) C -1.0624(5) -0.397(2) -0.8552(3) 0.047(1) Uani 1.00 d . . . C(17) C -1.0216(4) -0.579(2) -0.8388(2) 0.0371(9) Uani 1.00 d . . . C(18) C -1.1115(4) -0.626(1) -0.7213(3) 0.043(1) Uani 1.00 d . . . C(19) C -0.8665(4) -0.546(2) -0.4207(3) 0.045(1) Uani 1.00 d . . . C(20) C -1.1111(4) -0.698(2) -0.9074(3) 0.041(1) Uani 1.00 d . . . C(21) C -1.0741(7) -0.875(2) -0.8903(3) 0.072(2) Uani 1.00 d . . . C(22) C -1.1229(5) -0.643(2) -0.9995(3) 0.052(1) Uani 1.00 d . . . C(23) C -1.2230(5) -0.724(2) -1.0745(3) 0.061(2) Uani 1.00 d . . . C(24) C -1.2330(4) -0.664(2) -1.1640(3) 0.047(1) Uani 1.00 d . . . C(25) C -0.5206(10) -0.548(2) -0.8743(5) 0.099(2) Uani 1.00 d . . . C(26) C -0.623(1) -0.610(2) -0.9289(6) 0.115(3) Uani 1.00 d . . . C(27) C -0.6525(9) -0.596(2) -1.0243(6) 0.101(3) Uani 1.00 d . . . C(28) C -0.571(1) -0.531(2) -1.0510(5) 0.100(2) Uani 1.00 d . . . C(29) C -0.469(1) -0.476(2) -0.9951(8) 0.135(4) Uani 1.00 d . . . C(30) C -0.444(1) -0.481(2) -0.9034(7) 0.130(4) Uani 1.00 d . . . C(31) C -0.494(2) -0.559(3) -0.7737(6) 0.208(7) Uani 1.00 d . . . H(1) H -0.6991 -0.7628 -0.4248 0.0458 Uiso 1.00 calc . . . H(2) H -0.6546 -0.6482 -0.3429 0.0458 Uiso 1.00 calc . . . H(3) H -0.4933 -0.7191 -0.3815 0.0478 Uiso 1.00 calc . . . H(4) H -0.5585 -0.6510 -0.4763 0.0478 Uiso 1.00 calc . . . H(5) H -0.4805 -0.4567 -0.3230 0.0458 Uiso 1.00 calc . . . H(6) H -0.5523 -0.2330 -0.4119 0.0474 Uiso 1.00 calc . . . H(7) H -0.5937 -0.3441 -0.4953 0.0474 Uiso 1.00 calc . . . H(8) H -0.6944 -0.3374 -0.3681 0.0411 Uiso 1.00 calc . . . H(9) H -0.8554 -0.2069 -0.4615 0.0489 Uiso 1.00 calc . . . H(10) H -0.7479 -0.1131 -0.4691 0.0489 Uiso 1.00 calc . . . H(11) H -0.9007 -0.1621 -0.6065 0.0421 Uiso 1.00 calc . . . H(12) H -0.9624 -0.4172 -0.5905 0.0362 Uiso 1.00 calc . . . H(13) H -0.7406 -0.5416 -0.5734 0.0368 Uiso 1.00 calc . . . H(14) H -0.8070 -0.8005 -0.5609 0.0450 Uiso 1.00 calc . . . H(15) H -0.9308 -0.7307 -0.5710 0.0450 Uiso 1.00 calc . . . H(16) H -0.9484 -0.8450 -0.7044 0.0459 Uiso 1.00 calc . . . H(17) H -0.8616 -0.4389 -0.7183 0.0383 Uiso 1.00 calc . . . H(18) H -1.0760 -0.2806 -0.7465 0.0520 Uiso 1.00 calc . . . H(19) H -0.9705 -0.2151 -0.7698 0.0520 Uiso 1.00 calc . . . H(20) H -1.1476 -0.3936 -0.8779 0.0566 Uiso 1.00 calc . . . H(21) H -1.0336 -0.3485 -0.8955 0.0566 Uiso 1.00 calc . . . H(22) H -0.9476 -0.5868 -0.8470 0.0443 Uiso 1.00 calc . . . H(23) H -1.0962 -0.6187 -0.6599 0.0503 Uiso 1.00 calc . . . H(24) H -1.1669 -0.5413 -0.7515 0.0503 Uiso 1.00 calc . . . H(25) H -1.1464 -0.7298 -0.7430 0.0503 Uiso 1.00 calc . . . H(26) H -0.8389 -0.5277 -0.3591 0.0529 Uiso 1.00 calc . . . H(27) H -0.9276 -0.4686 -0.4503 0.0529 Uiso 1.00 calc . . . H(28) H -0.8989 -0.6543 -0.4336 0.0529 Uiso 1.00 calc . . . H(29) H -1.1868 -0.6849 -0.9020 0.0491 Uiso 1.00 calc . . . H(30) H -1.0696 -0.9074 -0.8325 0.0881 Uiso 1.00 calc . . . H(31) H -1.1316 -0.9442 -0.9327 0.0881 Uiso 1.00 calc . . . H(32) H -0.9988 -0.8919 -0.8947 0.0881 Uiso 1.00 calc . . . H(33) H -1.1368 -0.5264 -1.0040 0.0621 Uiso 1.00 calc . . . H(34) H -1.0496 -0.6642 -1.0068 0.0621 Uiso 1.00 calc . . . H(35) H -1.2087 -0.8415 -1.0717 0.0778 Uiso 1.00 calc . . . H(36) H -1.2967 -0.7062 -1.0672 0.0778 Uiso 1.00 calc . . . H(37) H -0.3467 -0.3772 -0.3657 0.0948 Uiso 1.00 calc . . . H(38) H -0.7143 -0.0824 -0.6241 0.0948 Uiso 1.00 calc . . . H(39) H -0.8229 -0.8313 -0.7566 0.0948 Uiso 1.00 calc . . . H(40) H -1.2761 -0.7631 -1.2791 0.0948 Uiso 1.00 calc . . . H(41) H -0.7232 -0.6398 -1.0636 0.1177 Uiso 1.00 calc . . . H(42) H -0.4160 -0.4271 -1.0197 0.1592 Uiso 1.00 calc . . . H(43) H -0.3647 -0.4489 -0.8627 0.1441 Uiso 1.00 calc . . . H(44) H -0.4912 -0.6756 -0.7565 0.2446 Uiso 1.00 calc . . . H(45) H -0.4201 -0.5121 -0.7390 0.2446 Uiso 1.00 calc . . . H(46) H -0.5559 -0.5099 -0.7588 0.2446 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) 0.204(4) 0.152(3) 0.270(5) -0.037(3) 0.171(4) -0.006(3) Cl(2) 0.297(5) 0.198(4) 0.078(1) -0.040(4) 0.063(2) 0.005(2) O(1) 0.030(1) 0.046(2) 0.060(2) -0.003(2) 0.006(1) -0.008(2) O(2) 0.041(2) 0.044(2) 0.037(1) -0.004(1) 0.016(1) 0.004(1) O(3) 0.049(2) 0.054(2) 0.039(1) 0.014(2) 0.011(1) -0.002(1) O(4) 0.125(4) 0.063(2) 0.043(2) -0.029(3) 0.016(2) 0.006(2) O(5) 0.071(2) 0.065(2) 0.034(1) -0.004(2) 0.019(1) -0.003(1) C(1) 0.044(2) 0.040(2) 0.026(2) -0.003(2) 0.002(2) 0.004(2) C(2) 0.037(2) 0.034(2) 0.040(2) 0.006(2) 0.002(2) 0.002(2) C(3) 0.034(2) 0.042(2) 0.034(2) -0.001(2) 0.002(1) -0.001(2) C(4) 0.036(2) 0.041(2) 0.033(2) 0.004(2) 0.006(2) -0.002(2) C(5) 0.042(2) 0.042(2) 0.023(2) 0.000(2) 0.012(1) -0.003(1) C(6) 0.038(2) 0.046(2) 0.037(2) 0.004(2) 0.013(2) -0.004(2) C(7) 0.032(2) 0.033(2) 0.037(2) 0.008(2) 0.007(1) 0.002(2) C(8) 0.029(2) 0.038(2) 0.030(2) 0.000(1) 0.010(1) -0.002(1) C(9) 0.032(2) 0.036(2) 0.023(1) -0.003(1) 0.006(1) 0.000(1) C(10) 0.040(2) 0.041(2) 0.022(1) -0.002(2) 0.010(1) 0.003(2) C(11) 0.043(2) 0.034(2) 0.026(2) -0.005(2) 0.007(2) 0.002(2) C(12) 0.049(2) 0.034(2) 0.028(2) 0.002(2) 0.008(2) 0.001(2) C(13) 0.035(2) 0.038(2) 0.024(1) 0.000(2) 0.007(1) 0.003(1) C(14) 0.031(2) 0.038(2) 0.027(2) -0.001(2) 0.008(1) 0.002(1) C(15) 0.039(2) 0.041(3) 0.038(2) 0.006(2) 0.003(2) 0.006(2) C(16) 0.049(3) 0.051(2) 0.034(2) 0.000(2) 0.005(2) 0.007(2) C(17) 0.031(2) 0.052(2) 0.025(1) 0.000(2) 0.005(1) 0.002(2) C(18) 0.035(2) 0.059(3) 0.032(2) -0.004(2) 0.009(2) 0.002(2) C(19) 0.045(2) 0.063(3) 0.030(2) -0.003(2) 0.017(2) -0.002(2) C(20) 0.039(2) 0.051(2) 0.026(2) 0.001(2) 0.002(1) -0.005(2) C(21) 0.092(5) 0.052(3) 0.044(3) 0.011(3) -0.008(3) -0.009(2) C(22) 0.048(3) 0.071(4) 0.029(2) -0.008(3) 0.005(2) 0.000(2) C(23) 0.070(3) 0.083(4) 0.024(2) -0.021(3) 0.009(2) -0.004(2) C(24) 0.046(2) 0.062(2) 0.026(2) 0.003(2) 0.003(2) 0.004(2) C(25) 0.134(6) 0.083(5) 0.071(3) 0.039(4) 0.027(3) -0.005(4) C(26) 0.141(6) 0.082(6) 0.100(4) 0.041(4) 0.019(4) -0.021(4) C(27) 0.104(6) 0.088(6) 0.103(4) -0.003(5) 0.027(4) -0.021(5) C(28) 0.141(7) 0.084(5) 0.080(2) -0.014(5) 0.044(4) 0.007(4) C(29) 0.15(1) 0.14(1) 0.111(5) -0.048(9) 0.041(6) -0.015(7) C(30) 0.152(10) 0.124(9) 0.109(5) -0.039(8) 0.041(6) -0.006(7) C(31) 0.32(2) 0.20(2) 0.065(4) 0.16(2) 0.031(8) 0.010(7) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(1) C(26) 1.67(2) . . yes Cl(2) C(28) 1.75(1) . . yes O(1) C(3) 1.452(8) . . yes O(2) C(7) 1.456(7) . . yes O(3) C(12) 1.442(8) . . yes O(4) C(24) 1.22(1) . . yes O(5) C(24) 1.299(9) . . yes C(1) C(2) 1.539(9) . . yes C(1) C(10) 1.536(9) . . yes C(2) C(3) 1.521(10) . . yes C(3) C(4) 1.502(9) . . yes C(4) C(5) 1.528(9) . . yes C(5) C(6) 1.539(9) . . yes C(5) C(10) 1.553(9) . . yes C(6) C(7) 1.523(8) . . yes C(7) C(8) 1.511(9) . . yes C(8) C(9) 1.536(8) . . yes C(8) C(14) 1.530(7) . . yes C(9) C(10) 1.564(6) . . yes C(9) C(11) 1.540(9) . . yes C(10) C(19) 1.558(8) . . yes C(11) C(12) 1.536(7) . . yes C(12) C(13) 1.546(9) . . yes C(13) C(14) 1.544(9) . . yes C(13) C(17) 1.553(7) . . yes C(13) C(18) 1.555(9) . . yes C(14) C(15) 1.512(9) . . yes C(15) C(16) 1.526(9) . . yes C(16) C(17) 1.55(1) . . yes C(17) C(20) 1.565(9) . . yes C(20) C(21) 1.51(1) . . yes C(20) C(22) 1.519(9) . . yes C(22) C(23) 1.518(9) . . yes C(23) C(24) 1.499(9) . . yes C(25) C(26) 1.33(2) . . yes C(25) C(30) 1.30(2) . . yes C(25) C(31) 1.55(2) . . yes C(26) C(27) 1.46(2) . . yes C(27) C(28) 1.32(2) . . yes C(28) C(29) 1.31(2) . . yes C(29) C(30) 1.41(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 C(2) C(1) C(10) 114.6(5) . 1_555 1_555 yes C(1) C(2) C(3) 110.0(5) . 1_555 1_555 yes O(1) C(3) C(2) 108.2(5) . 1_555 1_555 yes O(1) C(3) C(4) 109.3(5) . 1_555 1_555 yes C(2) C(3) C(4) 109.4(5) . 1_555 1_555 yes C(3) C(4) C(5) 114.4(5) . 1_555 1_555 yes C(4) C(5) C(6) 110.9(5) . 1_555 1_555 yes C(4) C(5) C(10) 112.8(5) . 1_555 1_555 yes C(6) C(5) C(10) 113.0(5) . 1_555 1_555 yes C(5) C(6) C(7) 113.7(5) . 1_555 1_555 yes O(2) C(7) C(6) 110.9(5) . 1_555 1_555 yes O(2) C(7) C(8) 108.7(5) . 1_555 1_555 yes C(6) C(7) C(8) 112.3(5) . 1_555 1_555 yes C(7) C(8) C(9) 113.0(4) . 1_555 1_555 yes C(7) C(8) C(14) 111.0(5) . 1_555 1_555 yes C(9) C(8) C(14) 109.4(5) . 1_555 1_555 yes C(8) C(9) C(10) 112.0(5) . 1_555 1_555 yes C(8) C(9) C(11) 110.7(4) . 1_555 1_555 yes C(10) C(9) C(11) 113.8(5) . 1_555 1_555 yes C(1) C(10) C(5) 108.7(5) . 1_555 1_555 yes C(1) C(10) C(9) 112.5(5) . 1_555 1_555 yes C(1) C(10) C(19) 106.3(5) . 1_555 1_555 yes C(5) C(10) C(9) 109.7(4) . 1_555 1_555 yes C(5) C(10) C(19) 109.3(5) . 1_555 1_555 yes C(9) C(10) C(19) 110.2(5) . 1_555 1_555 yes C(9) C(11) C(12) 114.8(5) . 1_555 1_555 yes O(3) C(12) C(11) 106.5(5) . 1_555 1_555 yes O(3) C(12) C(13) 111.7(5) . 1_555 1_555 yes C(11) C(12) C(13) 110.7(5) . 1_555 1_555 yes C(12) C(13) C(14) 108.7(4) . 1_555 1_555 yes C(12) C(13) C(17) 118.9(5) . 1_555 1_555 yes C(12) C(13) C(18) 107.8(5) . 1_555 1_555 yes C(14) C(13) C(17) 98.0(4) . 1_555 1_555 yes C(14) C(13) C(18) 112.9(5) . 1_555 1_555 yes C(17) C(13) C(18) 110.4(5) . 1_555 1_555 yes C(8) C(14) C(13) 115.0(5) . 1_555 1_555 yes C(8) C(14) C(15) 117.6(5) . 1_555 1_555 yes C(13) C(14) C(15) 105.2(5) . 1_555 1_555 yes C(14) C(15) C(16) 103.2(5) . 1_555 1_555 yes C(15) C(16) C(17) 107.1(5) . 1_555 1_555 yes C(13) C(17) C(16) 103.7(5) . 1_555 1_555 yes C(13) C(17) C(20) 119.5(5) . 1_555 1_555 yes C(16) C(17) C(20) 111.8(5) . 1_555 1_555 yes C(17) C(20) C(21) 112.2(5) . 1_555 1_555 yes C(17) C(20) C(22) 108.2(6) . 1_555 1_555 yes C(21) C(20) C(22) 112.1(6) . 1_555 1_555 yes C(20) C(22) C(23) 115.0(6) . 1_555 1_555 yes C(22) C(23) C(24) 113.0(7) . 1_555 1_555 yes O(4) C(24) O(5) 122.1(6) . 1_555 1_555 yes O(4) C(24) C(23) 125.3(7) . 1_555 1_555 yes O(5) C(24) C(23) 112.5(7) . 1_555 1_555 yes C(26) C(25) C(30) 121(1) . 1_555 1_555 yes C(26) C(25) C(31) 117(1) . 1_555 1_555 yes C(30) C(25) C(31) 120(1) . 1_555 1_555 yes Cl(1) C(26) C(25) 125(1) . 1_555 1_555 yes Cl(1) C(26) C(27) 115(1) . 1_555 1_555 yes C(25) C(26) C(27) 118(1) . 1_555 1_555 yes C(26) C(27) C(28) 117(1) . 1_555 1_555 yes Cl(2) C(28) C(27) 120(1) . 1_555 1_555 yes Cl(2) C(28) C(29) 117(1) . 1_555 1_555 yes C(27) C(28) C(29) 122(1) . 1_555 1_555 yes C(28) C(29) C(30) 120(1) . 1_555 1_555 yes C(25) C(30) C(29) 119(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl(1) C(26) C(25) C(30) 179(1) 1_555 1_555 1_555 1_555 yes Cl(1) C(26) C(25) C(31) 0(1) 1_555 1_555 1_555 1_555 yes Cl(1) C(26) C(27) C(28) -177(1) 1_555 1_555 1_555 1_555 yes Cl(2) C(28) C(27) C(26) -177(1) 1_555 1_555 1_555 1_555 yes Cl(2) C(28) C(29) C(30) 174(1) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) -175.8(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 174.8(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -71.7(7) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 70.8(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -52.5(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 67.7(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -65.9(6) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 44.9(7) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 171.4(5) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -27(1) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 149.8(7) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -56.8(6) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 48.3(6) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 175.1(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -174.8(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 58.7(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -52.2(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 69.5(7) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -169.7(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 56.4(6) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 57.8(6) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 178.9(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.2(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 76.9(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -75.1(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 163.9(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 50.3(7) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -53.6(6) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 179.9(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 51.7(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -69.3(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -52.4(6) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -175.7(5) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -51.0(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 55.0(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -176.8(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -177.5(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -52.6(7) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 66.8(7) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 53.8(6) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -57.0(6) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 178.7(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 62.5(6) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -165.0(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 57.2(6) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -178.0(5) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -54.0(7) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) 179.2(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) -179.0(5) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -52.6(6) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -59.7(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 52.6(6) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 163.4(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -70.0(6) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 171.9(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -157.2(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 77.6(7) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -35.4(6) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 20.9(6) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -57.1(8) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 178.8(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -40.6(5) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -165.8(5) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 8.4(7) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 47.6(5) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -68.6(6) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 150.9(5) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 77.6(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) -178.3(6) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 57.6(7) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -169.3(7) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -47.6(8) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 178.7(7) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 66.5(9) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 4(1) 1_555 1_555 1_555 1_555 yes C(25) C(30) C(29) C(28) 3(3) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(30) C(29) 0(2) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) -1(2) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(30) -3(2) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(31) 177(1) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) -1(3) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(25) C(31) 178(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) O(4) 3.21(1) . 2_343 ? Cl(1) O(3) 3.505(7) . . ? O(1) O(2) 2.671(7) . 2_444 ? O(1) O(3) 2.878(7) . 2_454 ? O(1) O(4) 3.545(8) . 1_656 ? O(2) O(5) 2.712(6) . 2_353 ? O(2) C(2) 3.462(8) . 2_454 ? O(2) O(4) 3.490(7) . 2_353 ? O(2) C(24) 3.505(7) . 2_353 ? O(2) C(3) 3.570(8) . 2_454 ? O(3) O(4) 2.900(8) . 2_343 ? O(4) C(21) 3.34(1) . 2_353 ? O(5) C(14) 3.369(8) . 2_343 ? O(5) C(15) 3.550(9) . 2_343 ? C(21) C(27) 3.56(2) . 2_343 ? C(26) C(29) 3.55(2) . 2_443 ? C(27) C(29) 3.39(2) . 2_443 ? #------------------------------------------------------------------------------ #===END data_3_4-dichlorotoluene _database_code_depnum_ccdc_archive 'CCDC 297680' _audit_creation_date 'Thu Oct 28 11:16:04 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C31 H46 Cl2 O5 ' _chemical_formula_moiety ? _chemical_formula_weight 569.61 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 13.3968(5) _cell_length_b 8.0808(4) _cell_length_c 14.0372(6) _cell_angle_alpha 90 _cell_angle_beta 104.763(2) _cell_angle_gamma 90 _cell_volume 1469.5(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6556 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 67.8 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.290 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.169 _exptl_absorpt_correction_T_max 0.538 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7548 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_max 68.24 _diffrn_measured_fraction_theta_max 0.9841 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.9841 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # 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 2856 _reflns_number_gt 2652 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0798 _refine_ls_wR_factor_ref 0.1913 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2856 _refine_ls_number_parameters 344 _refine_ls_goodness_of_fit_ref 1.575 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.10000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0006 _refine_diff_density_max 0.35 _refine_diff_density_min -0.50 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.02(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.364 0.702 ;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 0.07106(10) -0.122(1) -1.0727(1) 0.0935(5) Uani 1.00 d . . . Cl(2) Cl -0.16032(10) -0.218(1) -1.17823(10) 0.0732(4) Uani 1.00 d . . . O(1) O -0.5948(2) -0.266(1) -1.1056(2) 0.0469(7) Uani 1.00 d . . . O(2) O -0.4055(2) -0.495(1) -0.7825(2) 0.0389(6) Uani 1.00 d . . . O(3) O -0.3101(2) 0.039(1) -0.7162(2) 0.0437(7) Uani 1.00 d . . . O(4) O 0.1607(2) -0.184(1) -0.3106(3) 0.0626(9) Uani 1.00 d . . . O(5) O 0.2021(2) 0.065(1) -0.2472(2) 0.0492(7) Uani 1.00 d . . . C(1) C -0.6621(3) -0.070(1) -0.8869(3) 0.0378(8) Uani 1.00 d . . . C(2) C -0.6198(3) -0.083(1) -0.9786(3) 0.0399(8) Uani 1.00 d . . . C(3) C -0.6399(3) -0.255(1) -1.0229(2) 0.0373(8) Uani 1.00 d . . . C(4) C -0.5912(3) -0.381(1) -0.9461(2) 0.0337(7) Uani 1.00 d . . . C(5) C -0.6334(2) -0.373(1) -0.8542(2) 0.0339(7) Uani 1.00 d . . . C(6) C -0.5876(3) -0.510(1) -0.7806(3) 0.0394(8) Uani 1.00 d . . . C(7) C -0.4769(3) -0.481(1) -0.7224(3) 0.0354(8) Uani 1.00 d . . . C(8) C -0.4642(3) -0.308(1) -0.6751(2) 0.0318(7) Uani 1.00 d . . . C(9) C -0.5054(2) -0.171(1) -0.7508(2) 0.0286(7) Uani 1.00 d . . . C(10) C -0.6208(2) -0.198(1) -0.8055(2) 0.0350(8) Uani 1.00 d . . . C(11) C -0.4830(3) 0.001(1) -0.7007(3) 0.0363(8) Uani 1.00 d . . . C(12) C -0.3705(3) 0.029(1) -0.6444(2) 0.0330(7) Uani 1.00 d . . . C(13) C -0.3305(2) -0.110(1) -0.5679(2) 0.0305(7) Uani 1.00 d . . . C(14) C -0.3527(2) -0.276(1) -0.6227(2) 0.0291(7) Uani 1.00 d . . . C(15) C -0.2979(3) -0.404(1) -0.5473(3) 0.0411(9) Uani 1.00 d . . . C(16) C -0.2011(3) -0.313(1) -0.4889(3) 0.0438(9) Uani 1.00 d . . . C(17) C -0.2124(2) -0.128(1) -0.5216(2) 0.0329(7) Uani 1.00 d . . . C(18) C -0.3869(3) -0.093(1) -0.4846(3) 0.0433(9) Uani 1.00 d . . . C(19) C -0.6909(3) -0.186(1) -0.7339(3) 0.0466(9) Uani 1.00 d . . . C(20) C -0.1547(3) -0.014(1) -0.4394(3) 0.0394(8) Uani 1.00 d . . . C(21) C -0.1674(4) 0.169(1) -0.4651(4) 0.054(1) Uani 1.00 d . . . C(22) C -0.0396(3) -0.067(1) -0.4124(3) 0.0496(10) Uani 1.00 d . . . C(23) C 0.0273(3) 0.021(1) -0.3246(3) 0.055(1) Uani 1.00 d . . . C(24) C 0.1363(3) -0.047(1) -0.2949(3) 0.0417(8) Uani 1.00 d . . . C(25) C -0.0681(4) -0.085(1) -0.8542(4) 0.060(1) Uani 1.00 d . . . C(26) C 0.0048(4) -0.084(1) -0.9090(4) 0.062(1) Uani 1.00 d . . . C(27) C -0.0225(3) -0.126(1) -1.0089(4) 0.056(1) Uani 1.00 d . . . C(28) C -0.1234(3) -0.172(1) -1.0534(4) 0.0543(10) Uani 1.00 d . . . C(29) C -0.1960(3) -0.177(1) -0.9998(4) 0.059(1) Uani 1.00 d . . . C(30) C -0.1691(4) -0.133(1) -0.9006(4) 0.063(1) Uani 1.00 d . . . C(31) C -0.0395(6) -0.028(1) -0.7485(4) 0.080(2) Uani 1.00 d . . . H(1) H -0.6453 0.0349 -0.8590 0.0460 Uiso 1.00 calc . . . H(2) H -0.7348 -0.0841 -0.9070 0.0460 Uiso 1.00 calc . . . H(3) H -0.6531 -0.0056 -1.0260 0.0460 Uiso 1.00 calc . . . H(4) H -0.5476 -0.0651 -0.9610 0.0460 Uiso 1.00 calc . . . H(5) H -0.7126 -0.2752 -1.0440 0.0429 Uiso 1.00 calc . . . H(6) H -0.6046 -0.4901 -0.9743 0.0385 Uiso 1.00 calc . . . H(7) H -0.5189 -0.3641 -0.9270 0.0385 Uiso 1.00 calc . . . H(8) H -0.7055 -0.3946 -0.8750 0.0390 Uiso 1.00 calc . . . H(9) H -0.6290 -0.5230 -0.7351 0.0441 Uiso 1.00 calc . . . H(10) H -0.5893 -0.6123 -0.8161 0.0441 Uiso 1.00 calc . . . H(11) H -0.4596 -0.5620 -0.6715 0.0417 Uiso 1.00 calc . . . H(12) H -0.5030 -0.3065 -0.6272 0.0368 Uiso 1.00 calc . . . H(13) H -0.4669 -0.1780 -0.7989 0.0346 Uiso 1.00 calc . . . H(14) H -0.5012 0.0820 -0.7502 0.0419 Uiso 1.00 calc . . . H(15) H -0.5250 0.0111 -0.6557 0.0419 Uiso 1.00 calc . . . H(16) H -0.3661 0.1294 -0.6104 0.0391 Uiso 1.00 calc . . . H(17) H -0.3166 -0.2749 -0.6724 0.0351 Uiso 1.00 calc . . . H(18) H -0.3400 -0.4380 -0.5051 0.0472 Uiso 1.00 calc . . . H(19) H -0.2799 -0.5008 -0.5790 0.0472 Uiso 1.00 calc . . . H(20) H -0.1960 -0.3239 -0.4203 0.0522 Uiso 1.00 calc . . . H(21) H -0.1416 -0.3625 -0.5030 0.0522 Uiso 1.00 calc . . . H(22) H -0.1794 -0.1185 -0.5739 0.0386 Uiso 1.00 calc . . . H(23) H -0.3721 0.0098 -0.4536 0.0507 Uiso 1.00 calc . . . H(24) H -0.4592 -0.1055 -0.5115 0.0507 Uiso 1.00 calc . . . H(25) H -0.3638 -0.1801 -0.4371 0.0507 Uiso 1.00 calc . . . H(26) H -0.6873 -0.0782 -0.7071 0.0576 Uiso 1.00 calc . . . H(27) H -0.7603 -0.2109 -0.7678 0.0576 Uiso 1.00 calc . . . H(28) H -0.6688 -0.2642 -0.6812 0.0576 Uiso 1.00 calc . . . H(29) H -0.1812 -0.0355 -0.3833 0.0449 Uiso 1.00 calc . . . H(30) H -0.1316 0.2308 -0.4091 0.0651 Uiso 1.00 calc . . . H(31) H -0.1394 0.1903 -0.5188 0.0651 Uiso 1.00 calc . . . H(32) H -0.2385 0.1959 -0.4808 0.0651 Uiso 1.00 calc . . . H(33) H -0.0359 -0.1834 -0.3988 0.0585 Uiso 1.00 calc . . . H(34) H -0.0129 -0.0463 -0.4676 0.0585 Uiso 1.00 calc . . . H(35) H 0.0302 0.1336 -0.3408 0.0653 Uiso 1.00 calc . . . H(36) H -0.0035 0.0087 -0.2711 0.0653 Uiso 1.00 calc . . . H(37) H -0.6064 -0.3756 -1.1338 0.0536 Uiso 1.00 calc . . . H(38) H -0.4100 -0.6030 -0.8114 0.0442 Uiso 1.00 calc . . . H(39) H -0.2740 0.1620 -0.7327 0.0853 Uiso 1.00 calc . . . H(40) H 0.2818 0.0421 -0.2309 0.0853 Uiso 1.00 calc . . . H(41) H 0.0745 -0.0546 -0.8781 0.0745 Uiso 1.00 calc . . . H(42) H -0.2644 -0.2154 -1.0295 0.0705 Uiso 1.00 calc . . . H(43) H -0.2202 -0.1346 -0.8648 0.0748 Uiso 1.00 calc . . . H(44) H 0.0148 -0.0958 -0.7109 0.0947 Uiso 1.00 calc . . . H(45) H -0.0182 0.0829 -0.7456 0.0947 Uiso 1.00 calc . . . H(46) H -0.0982 -0.0389 -0.7222 0.0947 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) 0.0449(6) 0.167(2) 0.0685(7) -0.0088(8) 0.0146(5) -0.013(1) Cl(2) 0.0552(6) 0.0930(9) 0.0619(7) 0.0034(6) -0.0023(5) -0.0027(7) O(1) 0.068(2) 0.044(1) 0.027(1) 0.000(1) 0.009(1) 0.005(1) O(2) 0.033(1) 0.039(1) 0.042(1) 0.0022(9) 0.0040(9) -0.008(1) O(3) 0.044(1) 0.050(1) 0.036(1) -0.008(1) 0.0075(10) 0.005(1) O(4) 0.043(2) 0.053(1) 0.082(2) 0.004(1) -0.002(1) -0.010(2) O(5) 0.036(1) 0.052(1) 0.059(2) -0.005(1) 0.011(1) -0.008(1) C(1) 0.033(2) 0.042(2) 0.034(2) 0.010(1) 0.002(1) -0.003(1) C(2) 0.044(2) 0.041(2) 0.031(2) 0.005(1) 0.003(1) 0.006(1) C(3) 0.039(2) 0.044(2) 0.026(1) 0.001(1) 0.003(1) 0.003(1) C(4) 0.036(2) 0.035(1) 0.027(1) -0.002(1) 0.001(1) 0.001(1) C(5) 0.025(1) 0.045(2) 0.030(2) -0.002(1) 0.003(1) 0.002(1) C(6) 0.038(2) 0.043(2) 0.033(2) -0.008(1) 0.000(1) 0.005(1) C(7) 0.037(2) 0.035(1) 0.032(2) -0.002(1) 0.005(1) 0.004(1) C(8) 0.032(1) 0.034(1) 0.027(1) 0.003(1) 0.004(1) 0.003(1) C(9) 0.024(1) 0.034(1) 0.028(1) 0.004(1) 0.006(1) 0.000(1) C(10) 0.026(1) 0.047(2) 0.030(1) 0.005(1) 0.002(1) 0.001(1) C(11) 0.032(2) 0.036(1) 0.036(2) 0.006(1) -0.003(1) -0.003(1) C(12) 0.029(1) 0.034(2) 0.031(2) 0.005(1) -0.001(1) -0.004(1) C(13) 0.028(1) 0.036(1) 0.025(1) 0.004(1) 0.002(1) -0.002(1) C(14) 0.028(1) 0.031(1) 0.025(1) 0.004(1) 0.002(1) -0.001(1) C(15) 0.045(2) 0.038(2) 0.033(2) 0.000(1) -0.004(1) 0.008(1) C(16) 0.038(2) 0.045(2) 0.040(2) 0.005(1) -0.005(1) 0.005(1) C(17) 0.028(1) 0.042(2) 0.026(1) 0.000(1) 0.002(1) -0.003(1) C(18) 0.039(2) 0.064(2) 0.030(2) 0.001(2) 0.015(1) -0.010(2) C(19) 0.031(2) 0.072(2) 0.042(2) 0.005(2) 0.017(1) 0.001(2) C(20) 0.034(2) 0.047(2) 0.032(2) 0.001(1) 0.000(1) -0.005(1) C(21) 0.052(2) 0.047(2) 0.054(2) -0.010(2) -0.004(2) -0.002(2) C(22) 0.035(2) 0.061(2) 0.045(2) 0.003(2) -0.006(1) -0.007(2) C(23) 0.030(2) 0.069(3) 0.055(2) 0.004(2) -0.007(2) -0.023(2) C(24) 0.035(2) 0.050(2) 0.037(2) 0.001(1) 0.003(1) -0.001(1) C(25) 0.070(2) 0.055(2) 0.058(2) 0.016(2) 0.022(2) 0.006(2) C(26) 0.055(2) 0.075(3) 0.053(2) 0.007(2) 0.008(2) -0.003(2) C(27) 0.039(2) 0.074(3) 0.052(2) 0.005(2) 0.007(1) 0.003(2) C(28) 0.041(2) 0.057(2) 0.059(2) 0.003(2) 0.002(1) 0.006(2) C(29) 0.045(2) 0.059(2) 0.075(2) -0.001(2) 0.019(2) 0.010(2) C(30) 0.064(2) 0.057(2) 0.077(2) 0.017(2) 0.035(2) 0.013(2) C(31) 0.111(5) 0.067(3) 0.061(2) 0.019(3) 0.022(3) 0.001(2) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(1) C(27) 1.717(6) . . yes Cl(2) C(28) 1.736(6) . . yes O(1) C(3) 1.442(5) . . yes O(2) C(7) 1.432(5) . . yes O(3) C(12) 1.446(5) . . yes O(4) C(24) 1.194(7) . . yes O(5) C(24) 1.322(6) . . yes C(1) C(2) 1.538(6) . . yes C(1) C(10) 1.533(6) . . yes C(2) C(3) 1.513(7) . . yes C(3) C(4) 1.508(6) . . yes C(4) C(5) 1.536(6) . . yes C(5) C(6) 1.534(6) . . yes C(5) C(10) 1.561(6) . . yes C(6) C(7) 1.519(6) . . yes C(7) C(8) 1.534(6) . . yes C(8) C(9) 1.536(5) . . yes C(8) C(14) 1.511(5) . . yes C(9) C(10) 1.556(5) . . yes C(9) C(11) 1.552(6) . . yes C(10) C(19) 1.543(5) . . yes C(11) C(12) 1.530(6) . . yes C(12) C(13) 1.551(6) . . yes C(13) C(14) 1.535(5) . . yes C(13) C(17) 1.557(5) . . yes C(13) C(18) 1.551(5) . . yes C(14) C(15) 1.531(5) . . yes C(15) C(16) 1.534(7) . . yes C(16) C(17) 1.562(7) . . yes C(17) C(20) 1.522(6) . . yes C(20) C(21) 1.527(8) . . yes C(20) C(22) 1.550(7) . . yes C(22) C(23) 1.505(7) . . yes C(23) C(24) 1.515(6) . . yes C(25) C(26) 1.390(9) . . yes C(25) C(30) 1.40(1) . . yes C(25) C(31) 1.507(10) . . yes C(26) C(27) 1.398(9) . . yes C(27) C(28) 1.387(7) . . yes C(28) C(29) 1.373(8) . . yes C(29) C(30) 1.39(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) C(1) C(10) 116.0(3) . 1_555 1_555 yes C(1) C(2) C(3) 109.9(4) . 1_555 1_555 yes O(1) C(3) C(2) 108.8(4) . 1_555 1_555 yes O(1) C(3) C(4) 109.7(4) . 1_555 1_555 yes C(2) C(3) C(4) 109.1(3) . 1_555 1_555 yes C(3) C(4) C(5) 112.7(4) . 1_555 1_555 yes C(4) C(5) C(6) 111.4(4) . 1_555 1_555 yes C(4) C(5) C(10) 112.7(3) . 1_555 1_555 yes C(6) C(5) C(10) 112.4(3) . 1_555 1_555 yes C(5) C(6) C(7) 114.6(4) . 1_555 1_555 yes O(2) C(7) C(6) 112.2(4) . 1_555 1_555 yes O(2) C(7) C(8) 108.0(3) . 1_555 1_555 yes C(6) C(7) C(8) 111.1(4) . 1_555 1_555 yes C(7) C(8) C(9) 112.0(3) . 1_555 1_555 yes C(7) C(8) C(14) 110.8(3) . 1_555 1_555 yes C(9) C(8) C(14) 110.3(3) . 1_555 1_555 yes C(8) C(9) C(10) 112.2(3) . 1_555 1_555 yes C(8) C(9) C(11) 109.8(3) . 1_555 1_555 yes C(10) C(9) C(11) 113.6(3) . 1_555 1_555 yes C(1) C(10) C(5) 107.7(3) . 1_555 1_555 yes C(1) C(10) C(9) 113.5(4) . 1_555 1_555 yes C(1) C(10) C(19) 106.2(4) . 1_555 1_555 yes C(5) C(10) C(9) 108.9(3) . 1_555 1_555 yes C(5) C(10) C(19) 109.1(4) . 1_555 1_555 yes C(9) C(10) C(19) 111.2(3) . 1_555 1_555 yes C(9) C(11) C(12) 114.7(3) . 1_555 1_555 yes O(3) C(12) C(11) 107.5(3) . 1_555 1_555 yes O(3) C(12) C(13) 111.5(3) . 1_555 1_555 yes C(11) C(12) C(13) 111.9(4) . 1_555 1_555 yes C(12) C(13) C(14) 107.2(3) . 1_555 1_555 yes C(12) C(13) C(17) 119.5(3) . 1_555 1_555 yes C(12) C(13) C(18) 108.1(3) . 1_555 1_555 yes C(14) C(13) C(17) 100.0(3) . 1_555 1_555 yes C(14) C(13) C(18) 112.5(4) . 1_555 1_555 yes C(17) C(13) C(18) 109.3(3) . 1_555 1_555 yes C(8) C(14) C(13) 115.9(3) . 1_555 1_555 yes C(8) C(14) C(15) 117.3(4) . 1_555 1_555 yes C(13) C(14) C(15) 104.4(3) . 1_555 1_555 yes C(14) C(15) C(16) 103.6(4) . 1_555 1_555 yes C(15) C(16) C(17) 107.3(3) . 1_555 1_555 yes C(13) C(17) C(16) 103.0(3) . 1_555 1_555 yes C(13) C(17) C(20) 121.7(4) . 1_555 1_555 yes C(16) C(17) C(20) 111.3(3) . 1_555 1_555 yes C(17) C(20) C(21) 113.8(4) . 1_555 1_555 yes C(17) C(20) C(22) 107.5(4) . 1_555 1_555 yes C(21) C(20) C(22) 111.6(4) . 1_555 1_555 yes C(20) C(22) C(23) 114.8(4) . 1_555 1_555 yes C(22) C(23) C(24) 112.7(4) . 1_555 1_555 yes O(4) C(24) O(5) 123.5(5) . 1_555 1_555 yes O(4) C(24) C(23) 125.2(5) . 1_555 1_555 yes O(5) C(24) C(23) 111.3(4) . 1_555 1_555 yes C(26) C(25) C(30) 118.5(6) . 1_555 1_555 yes C(26) C(25) C(31) 120.3(7) . 1_555 1_555 yes C(30) C(25) C(31) 121.1(6) . 1_555 1_555 yes C(25) C(26) C(27) 120.8(6) . 1_555 1_555 yes Cl(1) C(27) C(26) 118.6(4) . 1_555 1_555 yes Cl(1) C(27) C(28) 121.8(5) . 1_555 1_555 yes C(26) C(27) C(28) 119.5(6) . 1_555 1_555 yes Cl(2) C(28) C(27) 120.4(5) . 1_555 1_555 yes Cl(2) C(28) C(29) 119.1(4) . 1_555 1_555 yes C(27) C(28) C(29) 120.5(6) . 1_555 1_555 yes C(28) C(29) C(30) 120.0(6) . 1_555 1_555 yes C(25) C(30) C(29) 120.7(5) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl(1) C(27) C(26) C(25) -179.9(5) 1_555 1_555 1_555 1_555 yes Cl(1) C(27) C(28) Cl(2) -2.9(8) 1_555 1_555 1_555 1_555 yes Cl(1) C(27) C(28) C(29) 178.4(5) 1_555 1_555 1_555 1_555 yes Cl(2) C(28) C(27) C(26) 177.7(5) 1_555 1_555 1_555 1_555 yes Cl(2) C(28) C(29) C(30) -176.8(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) -177.1(3) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 178.4(3) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -70.2(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 70.7(4) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -53.0(4) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 68.8(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -67.7(4) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 44.9(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 170.8(3) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -26.0(9) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 155.1(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -57.4(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 49.3(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 176.1(3) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -175.7(3) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 59.0(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -50.9(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 69.8(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -167.7(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 59.3(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 56.6(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 176.3(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -56.4(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 75.6(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -74.3(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 164.1(3) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 50.9(5) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -55.7(4) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 179.0(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 52.6(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -69.0(4) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -52.8(4) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -176.5(3) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -52.0(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 57.0(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -175.6(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -177.2(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -53.0(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 64.6(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 52.1(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -57.2(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 177.4(3) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 61.5(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -164.6(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 58.2(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -177.7(3) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -53.9(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -179.1(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 178.7(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -51.7(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -60.7(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 52.7(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 165.3(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -68.8(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 172.1(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -156.3(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 78.2(5) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -34.8(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 19.6(5) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -55.4(6) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) -179.5(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -39.9(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -165.4(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 8.8(5) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 46.8(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -69.1(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 151.6(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.5(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) -177.0(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 58.8(5) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -173.8(5) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -47.1(5) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 174.2(5) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 60.8(6) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 0(1) 1_555 1_555 1_555 1_555 yes C(25) C(30) C(29) C(28) -1.4(10) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(30) C(29) 0.0(9) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) -0.9(10) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(30) 1.0(10) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(31) -175.8(7) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 1.9(9) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(25) C(31) 176.7(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(24) 3.500(5) . 1_554 ? O(1) O(2) 2.701(4) . 2_453 ? O(1) O(3) 2.958(5) . 2_443 ? O(2) O(5) 2.693(5) . 2_544 ? O(2) C(24) 3.517(6) . 2_544 ? O(2) C(2) 3.528(5) . 2_443 ? O(2) O(4) 3.554(5) . 2_544 ? O(3) O(4) 2.964(5) . 2_554 ? O(4) C(21) 3.386(8) . 2_544 ? O(4) C(31) 3.426(9) . 2_544 ? O(5) C(30) 3.303(7) . 2_554 ? O(5) C(14) 3.305(5) . 2_554 ? O(5) C(15) 3.452(7) . 2_554 ? #------------------------------------------------------------------------------ #===END data_4-Bromo-o-xylene _database_code_depnum_ccdc_archive 'CCDC 297681' _audit_creation_date 'Thu Oct 28 11:17:11 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C32 H49 Br O5 ' _chemical_formula_moiety ? _chemical_formula_weight 593.64 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 11.9681(6) _cell_length_b 8.1491(3) _cell_length_c 16.3101(7) _cell_angle_alpha 90 _cell_angle_beta 111.379(2) _cell_angle_gamma 90 _cell_volume 1481.2(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5772 _cell_measurement_theta_min 5.7 _cell_measurement_theta_max 68.2 _cell_measurement_temperature 203.2 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.193 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_T_max 0.733 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8901 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 68.23 _diffrn_measured_fraction_theta_max 0.9791 _diffrn_reflns_theta_full 68.23 _diffrn_measured_fraction_theta_full 0.9791 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # 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 2865 _reflns_number_gt 2444 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1436 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2865 _refine_ls_number_parameters 344 _refine_ls_goodness_of_fit_ref 1.569 _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 0.25 _refine_diff_density_min -0.76 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.12(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ;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 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br Br -0.676 1.280 ;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 Br(1) Br 0.6207(1) 0.280(1) 1.16838(4) 0.1131(3) Uani 1.00 d . . . O(1) O 0.3857(2) 0.351(1) 0.4015(2) 0.0319(7) Uani 1.00 d . . . O(2) O 0.7465(2) 0.578(1) 0.6186(2) 0.0271(6) Uani 1.00 d . . . O(3) O 0.8058(2) 0.050(1) 0.7141(2) 0.0304(6) Uani 1.00 d . . . O(4) O 1.2054(3) 0.268(1) 1.1803(2) 0.0470(8) Uani 1.00 d . . . O(5) O 1.2757(3) 0.018(1) 1.2257(2) 0.0349(7) Uani 1.00 d . . . C(1) C 0.6693(4) 0.144(1) 0.4073(2) 0.0283(8) Uani 1.00 d . . . C(2) C 0.5481(3) 0.164(1) 0.4173(3) 0.0283(8) Uani 1.00 d . . . C(3) C 0.4967(3) 0.331(1) 0.3864(2) 0.0274(8) Uani 1.00 d . . . C(4) C 0.5841(3) 0.462(1) 0.4367(2) 0.0251(8) Uani 1.00 d . . . C(5) C 0.7079(3) 0.445(1) 0.4300(2) 0.0253(8) Uani 1.00 d . . . C(6) C 0.7920(3) 0.583(1) 0.4833(2) 0.0266(8) Uani 1.00 d . . . C(7) C 0.8393(3) 0.559(1) 0.5827(2) 0.0244(8) Uani 1.00 d . . . C(8) C 0.8947(3) 0.389(1) 0.6077(2) 0.0241(8) Uani 1.00 d . . . C(9) C 0.8095(3) 0.252(1) 0.5579(2) 0.0210(7) Uani 1.00 d . . . C(10) C 0.7644(3) 0.273(1) 0.4561(2) 0.0246(7) Uani 1.00 d . . . C(11) C 0.8684(3) 0.084(1) 0.5908(2) 0.0251(8) Uani 1.00 d . . . C(12) C 0.9115(3) 0.058(1) 0.6912(2) 0.0236(8) Uani 1.00 d . . . C(13) C 0.9979(3) 0.195(1) 0.7405(2) 0.0221(7) Uani 1.00 d . . . C(14) C 0.9339(3) 0.360(1) 0.7067(2) 0.0241(8) Uani 1.00 d . . . C(15) C 1.0140(4) 0.488(1) 0.7673(2) 0.0308(9) Uani 1.00 d . . . C(16) C 1.0632(4) 0.403(1) 0.8580(3) 0.0316(9) Uani 1.00 d . . . C(17) C 1.0243(3) 0.220(1) 0.8413(2) 0.0246(8) Uani 1.00 d . . . C(18) C 1.1162(3) 0.179(1) 0.7242(2) 0.0288(9) Uani 1.00 d . . . C(19) C 0.8693(3) 0.252(1) 0.4236(2) 0.0322(9) Uani 1.00 d . . . C(20) C 1.1137(3) 0.103(1) 0.9085(2) 0.0293(8) Uani 1.00 d . . . C(21) C 1.0736(5) -0.073(1) 0.8938(3) 0.046(1) Uani 1.00 d . . . C(22) C 1.1280(4) 0.161(1) 1.0015(2) 0.0349(10) Uani 1.00 d . . . C(23) C 1.2251(4) 0.075(1) 1.0754(2) 0.038(1) Uani 1.00 d . . . C(24) C 1.2342(3) 0.132(1) 1.1645(2) 0.0285(8) Uani 1.00 d . . . C(25) C 0.5074(5) 0.260(1) 0.8634(3) 0.048(1) Uani 1.00 d . . . C(26) C 0.6182(5) 0.196(1) 0.9176(4) 0.052(1) Uani 1.00 d . . . C(27) C 0.6501(5) 0.200(1) 1.0074(4) 0.052(1) Uani 1.00 d . . . C(28) C 0.5734(6) 0.269(1) 1.0441(3) 0.053(1) Uani 1.00 d . . . C(29) C 0.4655(6) 0.328(1) 0.9935(4) 0.060(1) Uani 1.00 d . . . C(30) C 0.4326(5) 0.326(1) 0.9030(4) 0.057(1) Uani 1.00 d . . . C(31) C 0.4678(8) 0.258(2) 0.7641(4) 0.083(2) Uani 1.00 d . . . C(32) C 0.6995(8) 0.116(1) 0.8774(6) 0.085(3) Uani 1.00 d . . . H(1) H 0.6998 0.0395 0.4294 0.0340 Uiso 1.00 calc . . . H(2) H 0.6566 0.1505 0.3464 0.0340 Uiso 1.00 calc . . . H(3) H 0.4944 0.0841 0.3832 0.0338 Uiso 1.00 calc . . . H(4) H 0.5585 0.1530 0.4774 0.0338 Uiso 1.00 calc . . . H(5) H 0.4815 0.3433 0.3252 0.0329 Uiso 1.00 calc . . . H(6) H 0.5520 0.5671 0.4143 0.0302 Uiso 1.00 calc . . . H(7) H 0.5936 0.4554 0.4970 0.0302 Uiso 1.00 calc . . . H(8) H 0.6972 0.4628 0.3698 0.0300 Uiso 1.00 calc . . . H(9) H 0.8589 0.5903 0.4651 0.0317 Uiso 1.00 calc . . . H(10) H 0.7491 0.6847 0.4702 0.0317 Uiso 1.00 calc . . . H(11) H 0.8997 0.6397 0.6090 0.0292 Uiso 1.00 calc . . . H(12) H 0.9643 0.3844 0.5926 0.0289 Uiso 1.00 calc . . . H(13) H 0.7409 0.2604 0.5738 0.0250 Uiso 1.00 calc . . . H(14) H 0.8113 0.0019 0.5634 0.0301 Uiso 1.00 calc . . . H(15) H 0.9357 0.0738 0.5737 0.0301 Uiso 1.00 calc . . . H(16) H 0.9527 -0.0431 0.7054 0.0282 Uiso 1.00 calc . . . H(17) H 0.8625 0.3597 0.7194 0.0290 Uiso 1.00 calc . . . H(18) H 1.0777 0.5184 0.7484 0.0368 Uiso 1.00 calc . . . H(19) H 0.9695 0.5841 0.7695 0.0368 Uiso 1.00 calc . . . H(20) H 1.1482 0.4116 0.8825 0.0376 Uiso 1.00 calc . . . H(21) H 1.0301 0.4522 0.8970 0.0376 Uiso 1.00 calc . . . H(22) H 0.9497 0.2112 0.8491 0.0293 Uiso 1.00 calc . . . H(23) H 1.1520 0.0770 0.7454 0.0346 Uiso 1.00 calc . . . H(24) H 1.1004 0.1882 0.6629 0.0346 Uiso 1.00 calc . . . H(25) H 1.1694 0.2657 0.7543 0.0346 Uiso 1.00 calc . . . H(26) H 0.9014 0.1455 0.4370 0.0382 Uiso 1.00 calc . . . H(27) H 0.8417 0.2703 0.3619 0.0382 Uiso 1.00 calc . . . H(28) H 0.9303 0.3311 0.4524 0.0382 Uiso 1.00 calc . . . H(29) H 1.1892 0.1129 0.9022 0.0349 Uiso 1.00 calc . . . H(30) H 0.9980 -0.0839 0.9000 0.0547 Uiso 1.00 calc . . . H(31) H 1.0661 -0.1051 0.8359 0.0547 Uiso 1.00 calc . . . H(32) H 1.1310 -0.1403 0.9356 0.0547 Uiso 1.00 calc . . . H(33) H 1.1458 0.2758 1.0055 0.0419 Uiso 1.00 calc . . . H(34) H 1.0538 0.1444 1.0091 0.0419 Uiso 1.00 calc . . . H(35) H 1.2087 -0.0384 1.0711 0.0450 Uiso 1.00 calc . . . H(36) H 1.2998 0.0956 1.0692 0.0450 Uiso 1.00 calc . . . H(37) H 0.3277 0.4297 0.3790 0.0865 Uiso 1.00 calc . . . H(38) H 0.7015 0.6616 0.6043 0.0865 Uiso 1.00 calc . . . H(39) H 0.8292 -0.0184 0.7601 0.0865 Uiso 1.00 calc . . . H(40) H 1.2168 -0.0040 1.2511 0.0425 Uiso 1.00 calc . . . H(41) H 0.7249 0.1561 1.0443 0.0617 Uiso 1.00 calc . . . H(42) H 0.4121 0.3700 1.0197 0.0715 Uiso 1.00 calc . . . H(43) H 0.3576 0.3727 0.8672 0.0683 Uiso 1.00 calc . . . H(44) H 0.4526 0.3681 0.7422 0.0985 Uiso 1.00 calc . . . H(45) H 0.5296 0.2123 0.7477 0.0985 Uiso 1.00 calc . . . H(46) H 0.3970 0.1954 0.7399 0.0985 Uiso 1.00 calc . . . H(47) H 0.7091 0.0041 0.8933 0.1006 Uiso 1.00 calc . . . H(48) H 0.6641 0.1254 0.8147 0.1006 Uiso 1.00 calc . . . H(49) H 0.7749 0.1697 0.8975 0.1006 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 Br(1) 0.193(1) 0.1018(6) 0.0351(3) -0.0113(7) 0.0309(4) -0.0006(4) O(1) 0.024(1) 0.031(1) 0.039(1) -0.001(1) 0.009(1) 0.001(1) O(2) 0.031(1) 0.030(1) 0.021(1) 0.007(1) 0.0101(10) 0.0014(10) O(3) 0.032(1) 0.034(1) 0.025(1) -0.005(1) 0.010(1) 0.003(1) O(4) 0.076(2) 0.034(1) 0.028(1) 0.013(2) 0.016(1) 0.000(1) O(5) 0.048(2) 0.036(1) 0.022(1) 0.004(1) 0.014(1) 0.004(1) C(1) 0.030(2) 0.032(2) 0.019(2) 0.000(2) 0.005(1) -0.002(1) C(2) 0.028(2) 0.028(2) 0.026(2) -0.003(1) 0.007(1) -0.002(1) C(3) 0.025(2) 0.029(2) 0.024(2) -0.002(1) 0.005(1) 0.004(1) C(4) 0.026(1) 0.027(2) 0.021(1) 0.001(1) 0.007(1) 0.002(1) C(5) 0.028(2) 0.034(2) 0.015(1) -0.001(1) 0.008(1) 0.006(1) C(6) 0.024(2) 0.031(2) 0.024(1) 0.000(1) 0.008(1) 0.005(1) C(7) 0.025(2) 0.027(2) 0.023(1) -0.003(1) 0.010(1) 0.000(1) C(8) 0.027(2) 0.026(2) 0.020(1) -0.003(1) 0.009(1) 0.003(1) C(9) 0.024(2) 0.025(2) 0.014(1) 0.002(1) 0.008(1) 0.003(1) C(10) 0.024(2) 0.036(2) 0.013(1) 0.004(1) 0.005(1) 0.003(1) C(11) 0.029(2) 0.026(2) 0.019(1) 0.000(1) 0.008(1) -0.003(1) C(12) 0.026(2) 0.021(2) 0.021(1) 0.003(1) 0.006(1) 0.002(1) C(13) 0.023(1) 0.029(2) 0.014(1) -0.001(1) 0.006(1) 0.001(1) C(14) 0.021(2) 0.031(2) 0.019(1) 0.002(1) 0.006(1) 0.000(1) C(15) 0.033(2) 0.028(2) 0.024(2) -0.002(2) 0.001(1) -0.001(1) C(16) 0.038(2) 0.029(2) 0.022(2) -0.004(2) 0.005(2) -0.003(1) C(17) 0.028(2) 0.029(2) 0.015(1) 0.001(1) 0.005(1) 0.000(1) C(18) 0.021(1) 0.043(2) 0.023(2) 0.003(2) 0.008(1) 0.001(2) C(19) 0.029(2) 0.046(2) 0.026(2) 0.003(2) 0.015(1) 0.001(2) C(20) 0.030(2) 0.037(2) 0.016(1) 0.003(2) 0.003(1) 0.004(1) C(21) 0.059(3) 0.039(2) 0.026(2) -0.001(2) -0.001(2) 0.009(2) C(22) 0.038(2) 0.046(2) 0.018(2) 0.008(2) 0.008(1) 0.002(2) C(23) 0.053(3) 0.044(2) 0.016(1) 0.017(2) 0.010(2) 0.003(2) C(24) 0.033(2) 0.034(2) 0.017(1) 0.001(2) 0.008(1) 0.000(1) C(25) 0.059(2) 0.045(3) 0.041(2) -0.018(2) 0.020(2) -0.006(2) C(26) 0.063(2) 0.034(2) 0.063(2) -0.012(2) 0.027(2) 0.008(2) C(27) 0.050(3) 0.038(2) 0.062(2) 0.005(2) 0.015(2) 0.015(2) C(28) 0.079(3) 0.044(2) 0.035(1) 0.002(3) 0.019(2) -0.001(2) C(29) 0.073(3) 0.058(3) 0.059(2) 0.016(3) 0.037(3) -0.003(3) C(30) 0.043(2) 0.067(4) 0.056(2) 0.006(2) 0.012(2) 0.004(3) C(31) 0.107(5) 0.099(5) 0.040(2) -0.050(5) 0.023(3) -0.008(3) C(32) 0.123(6) 0.052(3) 0.135(7) 0.015(4) 0.113(6) 0.004(4) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) C(28) 1.897(6) . . yes O(1) C(3) 1.445(6) . . yes O(2) C(7) 1.441(5) . . yes O(3) C(12) 1.444(6) . . yes O(4) C(24) 1.217(7) . . yes O(5) C(24) 1.319(6) . . yes C(1) C(2) 1.528(7) . . yes C(1) C(10) 1.541(7) . . yes C(2) C(3) 1.503(7) . . yes C(3) C(4) 1.506(7) . . yes C(4) C(5) 1.531(6) . . yes C(5) C(6) 1.547(7) . . yes C(5) C(10) 1.549(7) . . yes C(6) C(7) 1.523(6) . . yes C(7) C(8) 1.527(7) . . yes C(8) C(9) 1.528(6) . . yes C(8) C(14) 1.527(6) . . yes C(9) C(10) 1.557(5) . . yes C(9) C(11) 1.546(6) . . yes C(10) C(19) 1.539(6) . . yes C(11) C(12) 1.542(6) . . yes C(12) C(13) 1.539(6) . . yes C(13) C(14) 1.545(7) . . yes C(13) C(17) 1.570(6) . . yes C(13) C(18) 1.538(6) . . yes C(14) C(15) 1.513(7) . . yes C(15) C(16) 1.544(7) . . yes C(16) C(17) 1.556(7) . . yes C(17) C(20) 1.548(6) . . yes C(20) C(21) 1.508(9) . . yes C(20) C(22) 1.536(6) . . yes C(22) C(23) 1.508(7) . . yes C(23) C(24) 1.489(6) . . yes C(25) C(26) 1.40(1) . . yes C(25) C(30) 1.39(1) . . yes C(25) C(31) 1.512(8) . . yes C(26) C(27) 1.37(1) . . yes C(26) C(32) 1.51(1) . . yes C(27) C(28) 1.39(1) . . yes C(28) C(29) 1.34(1) . . yes C(29) C(30) 1.38(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) C(1) C(10) 115.0(4) . 1_555 1_555 yes C(1) C(2) C(3) 110.5(4) . 1_555 1_555 yes O(1) C(3) C(2) 109.3(4) . 1_555 1_555 yes O(1) C(3) C(4) 109.2(4) . 1_555 1_555 yes C(2) C(3) C(4) 109.7(4) . 1_555 1_555 yes C(3) C(4) C(5) 113.4(4) . 1_555 1_555 yes C(4) C(5) C(6) 110.2(4) . 1_555 1_555 yes C(4) C(5) C(10) 113.3(4) . 1_555 1_555 yes C(6) C(5) C(10) 112.0(4) . 1_555 1_555 yes C(5) C(6) C(7) 114.8(4) . 1_555 1_555 yes O(2) C(7) C(6) 112.1(4) . 1_555 1_555 yes O(2) C(7) C(8) 108.3(3) . 1_555 1_555 yes C(6) C(7) C(8) 110.9(4) . 1_555 1_555 yes C(7) C(8) C(9) 112.3(4) . 1_555 1_555 yes C(7) C(8) C(14) 110.9(4) . 1_555 1_555 yes C(9) C(8) C(14) 109.9(4) . 1_555 1_555 yes C(8) C(9) C(10) 113.1(4) . 1_555 1_555 yes C(8) C(9) C(11) 109.3(3) . 1_555 1_555 yes C(10) C(9) C(11) 113.8(4) . 1_555 1_555 yes C(1) C(10) C(5) 108.1(4) . 1_555 1_555 yes C(1) C(10) C(9) 112.4(4) . 1_555 1_555 yes C(1) C(10) C(19) 106.8(4) . 1_555 1_555 yes C(5) C(10) C(9) 109.8(4) . 1_555 1_555 yes C(5) C(10) C(19) 109.5(4) . 1_555 1_555 yes C(9) C(10) C(19) 110.2(4) . 1_555 1_555 yes C(9) C(11) C(12) 115.2(4) . 1_555 1_555 yes O(3) C(12) C(11) 107.2(4) . 1_555 1_555 yes O(3) C(12) C(13) 112.5(4) . 1_555 1_555 yes C(11) C(12) C(13) 110.7(4) . 1_555 1_555 yes C(12) C(13) C(14) 107.2(3) . 1_555 1_555 yes C(12) C(13) C(17) 118.6(4) . 1_555 1_555 yes C(12) C(13) C(18) 109.5(4) . 1_555 1_555 yes C(14) C(13) C(17) 98.5(3) . 1_555 1_555 yes C(14) C(13) C(18) 112.4(4) . 1_555 1_555 yes C(17) C(13) C(18) 110.2(3) . 1_555 1_555 yes C(8) C(14) C(13) 115.5(4) . 1_555 1_555 yes C(8) C(14) C(15) 117.6(4) . 1_555 1_555 yes C(13) C(14) C(15) 104.6(3) . 1_555 1_555 yes C(14) C(15) C(16) 104.1(4) . 1_555 1_555 yes C(15) C(16) C(17) 106.2(4) . 1_555 1_555 yes C(13) C(17) C(16) 103.7(4) . 1_555 1_555 yes C(13) C(17) C(20) 119.2(4) . 1_555 1_555 yes C(16) C(17) C(20) 112.3(4) . 1_555 1_555 yes C(17) C(20) C(21) 112.1(4) . 1_555 1_555 yes C(17) C(20) C(22) 108.0(4) . 1_555 1_555 yes C(21) C(20) C(22) 111.4(4) . 1_555 1_555 yes C(20) C(22) C(23) 115.0(4) . 1_555 1_555 yes C(22) C(23) C(24) 113.5(4) . 1_555 1_555 yes O(4) C(24) O(5) 122.5(4) . 1_555 1_555 yes O(4) C(24) C(23) 124.2(4) . 1_555 1_555 yes O(5) C(24) C(23) 113.3(4) . 1_555 1_555 yes C(26) C(25) C(30) 118.3(6) . 1_555 1_555 yes C(26) C(25) C(31) 121.8(7) . 1_555 1_555 yes C(30) C(25) C(31) 119.9(7) . 1_555 1_555 yes C(25) C(26) C(27) 119.8(7) . 1_555 1_555 yes C(25) C(26) C(32) 120.1(7) . 1_555 1_555 yes C(27) C(26) C(32) 120.0(8) . 1_555 1_555 yes C(26) C(27) C(28) 119.9(6) . 1_555 1_555 yes Br(1) C(28) C(27) 119.6(5) . 1_555 1_555 yes Br(1) C(28) C(29) 119.1(5) . 1_555 1_555 yes C(27) C(28) C(29) 121.3(6) . 1_555 1_555 yes C(28) C(29) C(30) 119.3(6) . 1_555 1_555 yes C(25) C(30) C(29) 121.3(6) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) C(28) C(27) C(26) -178.0(5) 1_555 1_555 1_555 1_555 yes Br(1) C(28) C(29) C(30) 177.4(6) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) -176.6(4) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 176.2(4) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -69.8(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 70.8(4) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -52.5(4) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 67.7(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -66.7(4) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 43.6(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(18) 171.1(3) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) -27.6(8) 1_555 1_555 1_555 1_555 yes O(5) C(24) C(23) C(22) 151.7(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -56.9(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 48.5(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 173.9(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -174.4(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 60.1(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -51.5(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 69.8(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -169.2(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 56.5(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 57.4(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 180.0(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.7(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 75.3(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -74.4(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 164.5(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 51.4(5) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -54.2(5) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) -179.6(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 51.0(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -70.1(4) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -52.6(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -175.9(4) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -51.7(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 55.7(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -176.4(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -176.7(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -52.3(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 66.5(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 53.9(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -57.9(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 178.5(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 62.5(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -165.4(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 58.6(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -177.0(4) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -55.3(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) 179.6(4) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) -178.6(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -52.6(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -59.0(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 53.3(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 163.5(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -69.0(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 171.2(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -155.7(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 78.5(5) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -35.7(5) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 20.5(5) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -60.2(6) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 176.6(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -40.7(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -166.5(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 8.8(5) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 47.6(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -68.4(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 150.6(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 77.0(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 178.2(5) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 55.1(5) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -171.9(5) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -48.7(5) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) -178.5(5) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 64.6(6) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -1.0(10) 1_555 1_555 1_555 1_555 yes C(25) C(30) C(29) C(28) 2(1) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(30) C(29) 0(1) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 2(1) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(30) 0.0(10) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(31) -179.7(7) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) -3(1) 1_555 1_555 1_555 1_555 yes C(28) C(27) C(26) C(32) -177.9(7) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(25) C(31) 179.1(8) 1_555 1_555 1_555 1_555 yes C(30) C(25) C(26) C(32) 176.8(7) 1_555 1_555 1_555 1_555 yes C(31) C(25) C(26) C(32) -2(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(2) 2.678(5) . 2_646 ? O(1) O(3) 2.880(5) . 2_656 ? O(1) O(4) 3.530(5) . 1_454 ? O(2) O(5) 2.692(4) . 2_757 ? O(2) C(2) 3.429(6) . 2_656 ? O(2) O(4) 3.479(5) . 2_757 ? O(2) C(24) 3.487(5) . 2_757 ? O(2) C(3) 3.545(6) . 2_656 ? O(3) O(4) 2.906(5) . 2_747 ? O(3) C(32) 3.387(8) . . ? O(4) C(32) 3.316(9) . 2_757 ? O(4) C(21) 3.368(8) . 2_757 ? O(5) C(14) 3.342(6) . 2_747 ? O(5) C(15) 3.519(7) . 2_747 ? C(23) C(26) 3.593(8) . 2_747 ? C(27) C(29) 3.332(10) . 2_647 ? #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_aburaya94 _database_code_depnum_ccdc_archive 'CCDC 297682' _audit_creation_date 'Thu Apr 27 09:31:46 2006' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C57 H92 O8 ' _chemical_formula_moiety ? _chemical_formula_weight 905.35 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 7.3178(2) _cell_length_b 25.8105(6) _cell_length_c 13.6157(3) _cell_angle_alpha 90 _cell_angle_beta 90.889(1) _cell_angle_gamma 90 _cell_volume 2571.4(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10113 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 68.1 _cell_measurement_temperature 93.2 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5419 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18177 _diffrn_reflns_av_R_equivalents 0.149 _diffrn_reflns_theta_max 68.24 _diffrn_measured_fraction_theta_max 0.9763 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.9763 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # 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 4706 _reflns_number_gt 2791 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2027 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4706 _refine_ls_number_parameters 586 _refine_ls_goodness_of_fit_ref 1.374 _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 0.0001 _refine_diff_density_max 0.60 _refine_diff_density_min -0.51 _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 0.018 0.009 ;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 0.049 0.032 ;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 1.4005(6) 0.3632(4) -0.0009(3) 0.041(2) Uani 1.00 d . . . O(2) O 1.3227(6) 0.3271(4) 0.4252(3) 0.032(1) Uani 1.00 d . . . O(3) O 1.7204(7) 0.3677(4) 0.9051(4) 0.048(2) Uani 1.00 d . . . O(4) O 1.9334(6) 0.3771(4) 0.7904(3) 0.038(1) Uani 1.00 d . . . O(5) O 0.9396(6) -0.1152(4) 0.4981(3) 0.041(2) Uani 1.00 d . . . O(6) O 0.8668(6) -0.0785(4) 0.0700(3) 0.034(1) Uani 1.00 d . . . O(7) O 1.2612(7) -0.1217(4) -0.4040(4) 0.047(2) Uani 1.00 d . . . O(8) O 1.4759(6) -0.1285(4) -0.2872(3) 0.038(2) Uani 1.00 d . . . C(1) C 1.1406(10) 0.2571(5) 0.1177(5) 0.032(2) Uani 1.00 d . . . C(2) C 1.1955(9) 0.3128(4) 0.0918(5) 0.031(2) Uani 1.00 d . . . C(3) C 1.3512(10) 0.3107(4) 0.0200(5) 0.031(2) Uani 1.00 d . . . C(4) C 1.5127(9) 0.2806(4) 0.0617(5) 0.032(2) Uani 1.00 d . . . C(5) C 1.4581(9) 0.2251(4) 0.0926(5) 0.027(2) Uani 1.00 d . . . C(6) C 1.6261(10) 0.1961(4) 0.1349(5) 0.035(2) Uani 1.00 d . . . C(7) C 1.6824(9) 0.2157(4) 0.2342(5) 0.032(2) Uani 1.00 d . . . C(8) C 1.5266(10) 0.2160(4) 0.3079(5) 0.030(2) Uani 1.00 d . . . C(9) C 1.3560(10) 0.2452(4) 0.2667(5) 0.029(2) Uani 1.00 d . . . C(10) C 1.2946(9) 0.2244(4) 0.1629(5) 0.029(2) Uani 1.00 d . . . C(11) C 1.2057(9) 0.2498(4) 0.3407(5) 0.033(2) Uani 1.00 d . . . C(12) C 1.2710(9) 0.2732(4) 0.4377(5) 0.031(2) Uani 1.00 d . . . C(13) C 1.4346(9) 0.2434(4) 0.4819(5) 0.026(2) Uani 1.00 d . . . C(14) C 1.5821(9) 0.2414(4) 0.4062(5) 0.027(2) Uani 1.00 d . . . C(15) C 1.7484(9) 0.2197(4) 0.4628(5) 0.032(2) Uani 1.00 d . . . C(16) C 1.7320(10) 0.2434(4) 0.5650(6) 0.037(2) Uani 1.00 d . . . C(17) C 1.5385(9) 0.2688(4) 0.5710(5) 0.030(2) Uani 1.00 d . . . C(18) C 1.3674(9) 0.1887(4) 0.5146(5) 0.033(2) Uani 1.00 d . . . C(19) C 1.224(1) 0.1679(4) 0.1738(5) 0.040(2) Uani 1.00 d . . . C(20) C 1.4632(10) 0.2657(4) 0.6741(5) 0.033(2) Uani 1.00 d . . . C(21) C 1.2722(9) 0.2904(5) 0.6825(5) 0.041(2) Uani 1.00 d . . . C(22) C 1.5930(10) 0.2897(4) 0.7516(5) 0.035(2) Uani 1.00 d . . . C(23) C 1.641(1) 0.3462(5) 0.7367(6) 0.045(2) Uani 1.00 d . . . C(24) C 1.766(1) 0.3639(4) 0.8199(6) 0.035(2) Uani 1.00 d . . . C(25) C 0.6923(10) -0.0058(4) 0.3746(5) 0.035(2) Uani 1.00 d . . . C(26) C 0.7398(10) -0.0611(4) 0.4039(5) 0.035(2) Uani 1.00 d . . . C(27) C 0.8984(9) -0.0617(4) 0.4748(5) 0.032(2) Uani 1.00 d . . . C(28) C 1.0637(9) -0.0340(4) 0.4367(5) 0.030(2) Uani 1.00 d . . . C(29) C 1.0199(9) 0.0219(4) 0.4048(5) 0.031(2) Uani 1.00 d . . . C(30) C 1.193(1) 0.0490(4) 0.3654(5) 0.037(2) Uani 1.00 d . . . C(31) C 1.2436(10) 0.0297(4) 0.2644(5) 0.033(2) Uani 1.00 d . . . C(32) C 1.0853(9) 0.0316(4) 0.1896(5) 0.027(2) Uani 1.00 d . . . C(33) C 0.9140(9) 0.0040(4) 0.2314(5) 0.027(2) Uani 1.00 d . . . C(34) C 0.8550(9) 0.0255(4) 0.3319(5) 0.028(2) Uani 1.00 d . . . C(35) C 0.7596(9) 0.0002(4) 0.1528(5) 0.035(2) Uani 1.00 d . . . C(36) C 0.8187(9) -0.0237(4) 0.0563(5) 0.029(2) Uani 1.00 d . . . C(37) C 0.9846(9) 0.0050(4) 0.0136(5) 0.028(2) Uani 1.00 d . . . C(38) C 1.1359(9) 0.0062(4) 0.0931(5) 0.028(2) Uani 1.00 d . . . C(39) C 1.3042(9) 0.0254(4) 0.0391(5) 0.032(2) Uani 1.00 d . . . C(40) C 1.2813(9) 0.0040(4) -0.0658(5) 0.041(2) Uani 1.00 d . . . C(41) C 1.0884(9) -0.0208(4) -0.0718(5) 0.027(2) Uani 1.00 d . . . C(42) C 0.9204(10) 0.0599(4) -0.0159(5) 0.036(2) Uani 1.00 d . . . C(43) C 0.792(1) 0.0814(4) 0.3244(5) 0.038(2) Uani 1.00 d . . . C(44) C 1.0084(10) -0.0173(4) -0.1783(5) 0.030(2) Uani 1.00 d . . . C(45) C 0.8149(10) -0.0403(4) -0.1901(5) 0.038(2) Uani 1.00 d . . . C(46) C 1.1400(9) -0.0404(4) -0.2541(5) 0.031(2) Uani 1.00 d . . . C(47) C 1.185(1) -0.0981(5) -0.2384(5) 0.041(2) Uani 1.00 d . . . C(48) C 1.308(1) -0.1175(4) -0.3177(6) 0.038(2) Uani 1.00 d . . . C(49) C 1.889(1) 0.1589(5) 0.7965(6) 0.064(3) Uani 1.00 d . . . C(50) C 1.729(1) 0.1373(5) 0.7878(7) 0.067(3) Uani 1.00 d . . . C(51) C 1.675(1) 0.1018(5) 0.7096(6) 0.054(3) Uani 1.00 d . . . C(52) C 1.818(1) 0.0957(5) 0.6409(7) 0.075(3) Uani 1.00 d . . . C(53) C 1.982(1) 0.1152(5) 0.6460(7) 0.056(3) Uani 1.00 d . . . C(54) C 2.024(1) 0.1476(5) 0.7219(7) 0.072(4) Uani 1.00 d . . . C(55) C 1.960(1) 0.1934(5) 0.8703(7) 0.077(4) Uani 1.00 d . . . C(56) C 1.580(2) 0.1485(5) 0.8624(6) 0.089(4) Uani 1.00 d . . . C(57) C 1.505(1) 0.0786(6) 0.698(1) 0.140(6) Uani 1.00 d . . . H(1) H 1.0444 0.2585 0.1627 0.0395 Uiso 1.00 calc . . . H(2) H 1.1009 0.2404 0.0589 0.0395 Uiso 1.00 calc . . . H(3) H 1.0940 0.3303 0.0626 0.0382 Uiso 1.00 calc . . . H(4) H 1.2339 0.3306 0.1494 0.0382 Uiso 1.00 calc . . . H(5) H 1.3098 0.2944 -0.0392 0.0375 Uiso 1.00 calc . . . H(6) H 1.6041 0.2786 0.0134 0.0385 Uiso 1.00 calc . . . H(7) H 1.5583 0.2984 0.1177 0.0385 Uiso 1.00 calc . . . H(8) H 1.4207 0.2070 0.0343 0.0328 Uiso 1.00 calc . . . H(9) H 1.5983 0.1603 0.1391 0.0432 Uiso 1.00 calc . . . H(10) H 1.7254 0.2009 0.0912 0.0432 Uiso 1.00 calc . . . H(11) H 1.7279 0.2500 0.2289 0.0381 Uiso 1.00 calc . . . H(12) H 1.7771 0.1939 0.2605 0.0381 Uiso 1.00 calc . . . H(13) H 1.4917 0.1814 0.3212 0.0369 Uiso 1.00 calc . . . H(14) H 1.3962 0.2801 0.2558 0.0349 Uiso 1.00 calc . . . H(15) H 1.1598 0.2160 0.3537 0.0396 Uiso 1.00 calc . . . H(16) H 1.1109 0.2707 0.3145 0.0396 Uiso 1.00 calc . . . H(17) H 1.1735 0.2715 0.4824 0.0375 Uiso 1.00 calc . . . H(18) H 1.6111 0.2766 0.3910 0.0339 Uiso 1.00 calc . . . H(19) H 1.8598 0.2301 0.4327 0.0389 Uiso 1.00 calc . . . H(20) H 1.7443 0.1829 0.4651 0.0389 Uiso 1.00 calc . . . H(21) H 1.8249 0.2684 0.5751 0.0465 Uiso 1.00 calc . . . H(22) H 1.7439 0.2168 0.6131 0.0465 Uiso 1.00 calc . . . H(23) H 1.5542 0.3047 0.5558 0.0374 Uiso 1.00 calc . . . H(24) H 1.4679 0.1699 0.5417 0.0391 Uiso 1.00 calc . . . H(25) H 1.2763 0.1927 0.5627 0.0391 Uiso 1.00 calc . . . H(26) H 1.3185 0.1707 0.4596 0.0391 Uiso 1.00 calc . . . H(27) H 1.3198 0.1467 0.2005 0.0500 Uiso 1.00 calc . . . H(28) H 1.1234 0.1673 0.2166 0.0500 Uiso 1.00 calc . . . H(29) H 1.1885 0.1549 0.1114 0.0500 Uiso 1.00 calc . . . H(30) H 1.4513 0.2298 0.6898 0.0395 Uiso 1.00 calc . . . H(31) H 1.1901 0.2744 0.6376 0.0518 Uiso 1.00 calc . . . H(32) H 1.2798 0.3263 0.6697 0.0518 Uiso 1.00 calc . . . H(33) H 1.2288 0.2854 0.7480 0.0518 Uiso 1.00 calc . . . H(34) H 1.7039 0.2704 0.7530 0.0413 Uiso 1.00 calc . . . H(35) H 1.5368 0.2866 0.8147 0.0413 Uiso 1.00 calc . . . H(36) H 1.5324 0.3665 0.7366 0.0550 Uiso 1.00 calc . . . H(37) H 1.7014 0.3502 0.6764 0.0550 Uiso 1.00 calc . . . H(38) H 1.4969 0.3629 -0.0494 0.0500 Uiso 1.00 calc . . . H(39) H 1.2188 0.3462 0.3995 0.0401 Uiso 1.00 calc . . . H(40) H 2.0231 0.3889 0.8384 0.0455 Uiso 1.00 calc . . . H(41) H 0.5977 -0.0067 0.3265 0.0426 Uiso 1.00 calc . . . H(42) H 0.6511 0.0121 0.4312 0.0426 Uiso 1.00 calc . . . H(43) H 0.7704 -0.0801 0.3471 0.0426 Uiso 1.00 calc . . . H(44) H 0.6362 -0.0764 0.4339 0.0426 Uiso 1.00 calc . . . H(45) H 0.8613 -0.0449 0.5339 0.0401 Uiso 1.00 calc . . . H(46) H 1.1536 -0.0330 0.4879 0.0377 Uiso 1.00 calc . . . H(47) H 1.1078 -0.0526 0.3827 0.0377 Uiso 1.00 calc . . . H(48) H 0.9853 0.0401 0.4624 0.0376 Uiso 1.00 calc . . . H(49) H 1.1706 0.0854 0.3609 0.0454 Uiso 1.00 calc . . . H(50) H 1.2928 0.0431 0.4092 0.0454 Uiso 1.00 calc . . . H(51) H 1.3418 0.0500 0.2397 0.0411 Uiso 1.00 calc . . . H(52) H 1.2840 -0.0056 0.2697 0.0411 Uiso 1.00 calc . . . H(53) H 1.0555 0.0668 0.1769 0.0331 Uiso 1.00 calc . . . H(54) H 0.9515 -0.0308 0.2436 0.0327 Uiso 1.00 calc . . . H(55) H 0.6630 -0.0202 0.1780 0.0422 Uiso 1.00 calc . . . H(56) H 0.7158 0.0340 0.1386 0.0422 Uiso 1.00 calc . . . H(57) H 0.7188 -0.0219 0.0112 0.0346 Uiso 1.00 calc . . . H(58) H 1.1602 -0.0294 0.1088 0.0347 Uiso 1.00 calc . . . H(59) H 1.3087 0.0622 0.0398 0.0390 Uiso 1.00 calc . . . H(60) H 1.4133 0.0122 0.0697 0.0390 Uiso 1.00 calc . . . H(61) H 1.2890 0.0317 -0.1121 0.0497 Uiso 1.00 calc . . . H(62) H 1.3720 -0.0209 -0.0790 0.0497 Uiso 1.00 calc . . . H(63) H 1.1024 -0.0565 -0.0559 0.0330 Uiso 1.00 calc . . . H(64) H 0.8257 0.0576 -0.0639 0.0437 Uiso 1.00 calc . . . H(65) H 1.0203 0.0787 -0.0413 0.0437 Uiso 1.00 calc . . . H(66) H 0.8756 0.0772 0.0408 0.0437 Uiso 1.00 calc . . . H(67) H 0.6862 0.0830 0.2831 0.0459 Uiso 1.00 calc . . . H(68) H 0.8866 0.1016 0.2967 0.0459 Uiso 1.00 calc . . . H(69) H 0.7645 0.0939 0.3876 0.0459 Uiso 1.00 calc . . . H(70) H 0.9986 0.0184 -0.1940 0.0375 Uiso 1.00 calc . . . H(71) H 0.7366 -0.0240 -0.1452 0.0480 Uiso 1.00 calc . . . H(72) H 0.7717 -0.0345 -0.2555 0.0480 Uiso 1.00 calc . . . H(73) H 0.8199 -0.0765 -0.1777 0.0480 Uiso 1.00 calc . . . H(74) H 1.0866 -0.0367 -0.3178 0.0384 Uiso 1.00 calc . . . H(75) H 1.2516 -0.0218 -0.2507 0.0384 Uiso 1.00 calc . . . H(76) H 1.0739 -0.1175 -0.2406 0.0489 Uiso 1.00 calc . . . H(77) H 1.2435 -0.1026 -0.1770 0.0489 Uiso 1.00 calc . . . H(78) H 1.0385 -0.1158 0.5467 0.0509 Uiso 1.00 calc . . . H(79) H 0.7620 -0.0971 0.0952 0.0412 Uiso 1.00 calc . . . H(80) H 1.5642 -0.1419 -0.3336 0.0449 Uiso 1.00 calc . . . H(81) H 1.7909 0.0746 0.5851 0.0871 Uiso 1.00 calc . . . H(82) H 2.0692 0.1075 0.5973 0.0675 Uiso 1.00 calc . . . H(83) H 2.1421 0.1629 0.7275 0.0866 Uiso 1.00 calc . . . H(84) H 1.8667 0.2001 0.9178 0.0917 Uiso 1.00 calc . . . H(85) H 1.9945 0.2252 0.8414 0.0917 Uiso 1.00 calc . . . H(86) H 2.0613 0.1780 0.9025 0.0917 Uiso 1.00 calc . . . H(87) H 1.6229 0.1382 0.9257 0.1063 Uiso 1.00 calc . . . H(88) H 1.4738 0.1303 0.8448 0.1063 Uiso 1.00 calc . . . H(89) H 1.5565 0.1849 0.8629 0.1063 Uiso 1.00 calc . . . H(90) H 1.4289 0.0873 0.7487 0.1787 Uiso 1.00 calc . . . H(91) H 1.4528 0.0895 0.6357 0.1787 Uiso 1.00 calc . . . H(92) H 1.5217 0.0417 0.6946 0.1787 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) 0.044(3) 0.032(3) 0.047(3) -0.002(2) 0.007(3) 0.016(3) O(2) 0.031(3) 0.029(3) 0.036(3) 0.003(2) -0.008(2) 0.005(2) O(3) 0.049(3) 0.061(4) 0.033(3) -0.018(3) 0.005(2) -0.007(3) O(4) 0.036(3) 0.041(3) 0.037(3) -0.005(2) 0.002(2) -0.005(3) O(5) 0.041(3) 0.042(3) 0.041(3) -0.005(3) -0.003(3) 0.016(3) O(6) 0.031(3) 0.029(3) 0.041(3) 0.000(2) 0.004(2) 0.007(2) O(7) 0.046(3) 0.060(4) 0.035(3) 0.015(3) -0.004(3) 0.002(3) O(8) 0.043(3) 0.040(3) 0.031(3) 0.005(3) 0.000(2) -0.004(2) C(1) 0.034(4) 0.043(4) 0.018(4) -0.005(3) 0.001(3) 0.008(3) C(2) 0.030(4) 0.038(4) 0.025(4) 0.003(3) -0.002(3) 0.006(3) C(3) 0.032(4) 0.033(3) 0.028(4) -0.002(3) 0.003(3) 0.005(3) C(4) 0.033(4) 0.028(4) 0.034(4) -0.001(3) 0.003(3) 0.001(3) C(5) 0.034(4) 0.029(4) 0.020(4) -0.004(3) 0.002(2) -0.004(3) C(6) 0.038(4) 0.045(5) 0.024(4) 0.004(3) 0.003(3) 0.002(3) C(7) 0.035(4) 0.035(5) 0.026(3) 0.011(4) 0.004(3) 0.000(3) C(8) 0.035(4) 0.037(5) 0.017(3) 0.005(3) -0.001(2) 0.004(3) C(9) 0.034(4) 0.029(4) 0.025(3) 0.002(3) -0.001(2) 0.005(3) C(10) 0.037(4) 0.030(4) 0.020(3) 0.002(3) 0.008(2) 0.006(3) C(11) 0.028(4) 0.039(5) 0.032(4) -0.002(3) 0.001(3) -0.001(3) C(12) 0.032(4) 0.028(3) 0.033(4) -0.001(3) -0.002(3) 0.000(3) C(13) 0.028(4) 0.030(4) 0.021(4) 0.000(3) 0.004(2) -0.003(3) C(14) 0.033(4) 0.031(4) 0.018(3) -0.001(3) 0.004(2) 0.001(3) C(15) 0.028(4) 0.033(5) 0.036(4) 0.004(3) 0.003(3) 0.000(3) C(16) 0.034(4) 0.042(5) 0.035(4) 0.005(3) -0.007(4) 0.001(3) C(17) 0.030(3) 0.034(5) 0.026(3) -0.004(3) -0.002(3) -0.007(3) C(18) 0.037(4) 0.028(4) 0.034(4) -0.002(3) 0.014(3) -0.006(3) C(19) 0.044(5) 0.037(4) 0.037(5) -0.016(4) -0.005(4) -0.001(4) C(20) 0.037(4) 0.034(5) 0.028(3) 0.002(3) 0.004(3) 0.000(3) C(21) 0.028(4) 0.063(6) 0.033(5) -0.006(4) 0.001(3) -0.010(4) C(22) 0.039(4) 0.030(4) 0.035(4) -0.010(4) 0.001(3) 0.008(3) C(23) 0.067(6) 0.028(4) 0.039(5) -0.013(4) -0.009(4) -0.004(4) C(24) 0.042(3) 0.027(4) 0.037(3) -0.013(4) 0.009(3) -0.005(4) C(25) 0.039(4) 0.042(4) 0.025(4) 0.006(3) 0.004(3) 0.002(3) C(26) 0.039(4) 0.041(4) 0.025(4) -0.001(3) -0.006(3) 0.006(3) C(27) 0.032(4) 0.038(3) 0.027(4) -0.002(3) 0.000(3) -0.001(3) C(28) 0.035(4) 0.029(4) 0.025(4) 0.002(3) 0.003(3) 0.004(3) C(29) 0.040(4) 0.031(4) 0.022(4) -0.003(3) -0.005(3) -0.001(3) C(30) 0.043(4) 0.040(5) 0.030(4) -0.004(3) 0.006(3) -0.005(4) C(31) 0.040(4) 0.034(5) 0.026(3) -0.004(4) -0.006(3) -0.006(3) C(32) 0.034(4) 0.026(4) 0.023(3) 0.000(3) 0.002(2) -0.002(3) C(33) 0.036(4) 0.019(4) 0.026(3) 0.000(3) 0.001(2) -0.002(3) C(34) 0.034(4) 0.028(3) 0.023(3) 0.008(3) -0.002(2) -0.004(3) C(35) 0.041(4) 0.039(5) 0.026(4) 0.008(4) -0.008(3) -0.008(3) C(36) 0.036(4) 0.027(3) 0.025(4) 0.003(3) 0.002(3) 0.001(3) C(37) 0.034(4) 0.034(4) 0.016(3) 0.002(3) -0.001(2) 0.006(3) C(38) 0.035(4) 0.035(4) 0.014(3) -0.009(3) 0.001(2) 0.004(3) C(39) 0.035(4) 0.037(5) 0.024(3) -0.002(3) 0.007(3) 0.011(3) C(40) 0.033(4) 0.059(6) 0.031(4) -0.005(4) 0.009(3) -0.018(4) C(41) 0.035(4) 0.029(4) 0.017(3) 0.004(3) -0.002(3) 0.005(3) C(42) 0.041(5) 0.032(4) 0.035(5) 0.004(3) -0.004(4) -0.002(3) C(43) 0.047(5) 0.030(4) 0.036(5) 0.013(4) 0.008(4) 0.003(4) C(44) 0.042(4) 0.029(4) 0.019(3) 0.003(3) -0.009(3) -0.007(3) C(45) 0.037(4) 0.045(5) 0.031(4) 0.006(3) -0.007(3) -0.002(4) C(46) 0.038(4) 0.033(4) 0.022(4) 0.007(3) 0.005(3) 0.006(3) C(47) 0.051(5) 0.034(4) 0.039(5) 0.011(4) 0.010(4) 0.006(4) C(48) 0.045(3) 0.033(5) 0.035(3) 0.005(4) 0.002(3) 0.005(4) C(49) 0.090(6) 0.067(7) 0.035(5) 0.020(5) -0.013(4) 0.004(4) C(50) 0.095(6) 0.066(7) 0.040(5) 0.001(5) -0.008(4) 0.019(4) C(51) 0.071(5) 0.053(6) 0.037(5) 0.020(4) 0.008(4) 0.018(4) C(52) 0.064(6) 0.095(8) 0.068(7) -0.009(6) 0.025(5) 0.015(6) C(53) 0.056(5) 0.067(7) 0.045(5) 0.010(4) 0.023(4) -0.007(4) C(54) 0.086(7) 0.074(8) 0.058(6) -0.004(6) 0.007(5) -0.007(5) C(55) 0.095(8) 0.055(7) 0.079(7) -0.020(6) -0.051(6) 0.015(5) C(56) 0.16(1) 0.076(7) 0.037(5) 0.086(7) 0.033(5) 0.019(5) C(57) 0.064(7) 0.12(1) 0.23(2) -0.013(6) -0.037(9) 0.13(1) #------------------------------------------------------------------------------ _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.431(9) . . yes O(2) C(12) 1.452(9) . . yes O(3) C(24) 1.216(9) . . yes O(4) C(24) 1.341(9) . . yes O(5) C(27) 1.448(9) . . yes O(6) C(36) 1.468(9) . . yes O(7) C(48) 1.223(9) . . yes O(8) C(48) 1.321(9) . . yes C(1) C(2) 1.54(1) . . yes C(1) C(10) 1.53(1) . . yes C(2) C(3) 1.51(1) . . yes C(3) C(4) 1.52(1) . . yes C(4) C(5) 1.55(1) . . yes C(5) C(6) 1.54(1) . . yes C(5) C(10) 1.544(10) . . yes C(6) C(7) 1.50(1) . . yes C(7) C(8) 1.53(1) . . yes C(8) C(9) 1.55(1) . . yes C(8) C(14) 1.54(1) . . yes C(9) C(10) 1.57(1) . . yes C(9) C(11) 1.51(1) . . yes C(10) C(19) 1.55(1) . . yes C(11) C(12) 1.52(1) . . yes C(12) C(13) 1.54(1) . . yes C(13) C(14) 1.505(10) . . yes C(13) C(17) 1.565(10) . . yes C(13) C(18) 1.56(1) . . yes C(14) C(15) 1.54(1) . . yes C(15) C(16) 1.53(1) . . yes C(16) C(17) 1.56(1) . . yes C(17) C(20) 1.52(1) . . yes C(20) C(21) 1.54(1) . . yes C(20) C(22) 1.54(1) . . yes C(22) C(23) 1.51(1) . . yes C(23) C(24) 1.51(1) . . yes C(25) C(26) 1.52(1) . . yes C(25) C(34) 1.56(1) . . yes C(26) C(27) 1.50(1) . . yes C(27) C(28) 1.50(1) . . yes C(28) C(29) 1.54(1) . . yes C(29) C(30) 1.55(1) . . yes C(29) C(34) 1.55(1) . . yes C(30) C(31) 1.51(1) . . yes C(31) C(32) 1.53(1) . . yes C(32) C(33) 1.56(1) . . yes C(32) C(38) 1.52(1) . . yes C(33) C(34) 1.54(1) . . yes C(33) C(35) 1.55(1) . . yes C(34) C(43) 1.52(1) . . yes C(35) C(36) 1.52(1) . . yes C(36) C(37) 1.54(1) . . yes C(37) C(38) 1.537(10) . . yes C(37) C(41) 1.55(1) . . yes C(37) C(42) 1.55(1) . . yes C(38) C(39) 1.53(1) . . yes C(39) C(40) 1.54(1) . . yes C(40) C(41) 1.55(1) . . yes C(41) C(44) 1.56(1) . . yes C(44) C(45) 1.54(1) . . yes C(44) C(46) 1.54(1) . . yes C(46) C(47) 1.54(1) . . yes C(47) C(48) 1.50(1) . . yes C(49) C(50) 1.30(1) . . yes C(49) C(54) 1.46(1) . . yes C(49) C(55) 1.43(1) . . yes C(50) C(51) 1.46(1) . . yes C(50) C(56) 1.53(1) . . yes C(51) C(52) 1.42(1) . . yes C(51) C(57) 1.39(2) . . yes C(52) C(53) 1.30(1) . . yes C(53) C(54) 1.36(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) C(1) C(10) 114.6(7) . 1_555 1_555 yes C(1) C(2) C(3) 108.5(7) . 1_555 1_555 yes O(1) C(3) C(2) 106.8(6) . 1_555 1_555 yes O(1) C(3) C(4) 111.2(7) . 1_555 1_555 yes C(2) C(3) C(4) 111.5(6) . 1_555 1_555 yes C(3) C(4) C(5) 111.9(7) . 1_555 1_555 yes C(4) C(5) C(6) 110.1(6) . 1_555 1_555 yes C(4) C(5) C(10) 112.7(6) . 1_555 1_555 yes C(6) C(5) C(10) 112.5(6) . 1_555 1_555 yes C(5) C(6) C(7) 112.3(7) . 1_555 1_555 yes C(6) C(7) C(8) 113.4(7) . 1_555 1_555 yes C(7) C(8) C(9) 111.7(6) . 1_555 1_555 yes C(7) C(8) C(14) 112.5(7) . 1_555 1_555 yes C(9) C(8) C(14) 107.9(6) . 1_555 1_555 yes C(8) C(9) C(10) 112.0(7) . 1_555 1_555 yes C(8) C(9) C(11) 112.8(6) . 1_555 1_555 yes C(10) C(9) C(11) 115.3(7) . 1_555 1_555 yes C(1) C(10) C(5) 108.4(6) . 1_555 1_555 yes C(1) C(10) C(9) 111.8(7) . 1_555 1_555 yes C(1) C(10) C(19) 108.2(7) . 1_555 1_555 yes C(5) C(10) C(9) 109.9(6) . 1_555 1_555 yes C(5) C(10) C(19) 109.4(7) . 1_555 1_555 yes C(9) C(10) C(19) 109.0(7) . 1_555 1_555 yes C(9) C(11) C(12) 112.9(6) . 1_555 1_555 yes O(2) C(12) C(11) 110.9(7) . 1_555 1_555 yes O(2) C(12) C(13) 108.8(6) . 1_555 1_555 yes C(11) C(12) C(13) 111.9(7) . 1_555 1_555 yes C(12) C(13) C(14) 108.1(6) . 1_555 1_555 yes C(12) C(13) C(17) 117.4(7) . 1_555 1_555 yes C(12) C(13) C(18) 108.5(6) . 1_555 1_555 yes C(14) C(13) C(17) 101.5(6) . 1_555 1_555 yes C(14) C(13) C(18) 113.3(6) . 1_555 1_555 yes C(17) C(13) C(18) 108.0(7) . 1_555 1_555 yes C(8) C(14) C(13) 115.3(7) . 1_555 1_555 yes C(8) C(14) C(15) 118.5(7) . 1_555 1_555 yes C(13) C(14) C(15) 103.9(6) . 1_555 1_555 yes C(14) C(15) C(16) 103.8(6) . 1_555 1_555 yes C(15) C(16) C(17) 107.4(6) . 1_555 1_555 yes C(13) C(17) C(16) 102.3(6) . 1_555 1_555 yes C(13) C(17) C(20) 121.0(7) . 1_555 1_555 yes C(16) C(17) C(20) 111.6(7) . 1_555 1_555 yes C(17) C(20) C(21) 113.0(7) . 1_555 1_555 yes C(17) C(20) C(22) 112.6(7) . 1_555 1_555 yes C(21) C(20) C(22) 109.4(7) . 1_555 1_555 yes C(20) C(22) C(23) 116.0(7) . 1_555 1_555 yes C(22) C(23) C(24) 109.2(7) . 1_555 1_555 yes O(3) C(24) O(4) 122.0(8) . 1_555 1_555 yes O(3) C(24) C(23) 124.6(8) . 1_555 1_555 yes O(4) C(24) C(23) 113.3(8) . 1_555 1_555 yes C(26) C(25) C(34) 114.3(7) . 1_555 1_555 yes C(25) C(26) C(27) 110.5(7) . 1_555 1_555 yes O(5) C(27) C(26) 107.9(7) . 1_555 1_555 yes O(5) C(27) C(28) 111.3(7) . 1_555 1_555 yes C(26) C(27) C(28) 113.1(7) . 1_555 1_555 yes C(27) C(28) C(29) 112.2(7) . 1_555 1_555 yes C(28) C(29) C(30) 110.6(7) . 1_555 1_555 yes C(28) C(29) C(34) 113.1(6) . 1_555 1_555 yes C(30) C(29) C(34) 112.5(6) . 1_555 1_555 yes C(29) C(30) C(31) 112.1(7) . 1_555 1_555 yes C(30) C(31) C(32) 113.7(7) . 1_555 1_555 yes C(31) C(32) C(33) 110.3(6) . 1_555 1_555 yes C(31) C(32) C(38) 111.7(6) . 1_555 1_555 yes C(33) C(32) C(38) 109.0(6) . 1_555 1_555 yes C(32) C(33) C(34) 113.3(7) . 1_555 1_555 yes C(32) C(33) C(35) 111.0(6) . 1_555 1_555 yes C(34) C(33) C(35) 115.1(6) . 1_555 1_555 yes C(25) C(34) C(29) 108.7(6) . 1_555 1_555 yes C(25) C(34) C(33) 111.7(7) . 1_555 1_555 yes C(25) C(34) C(43) 106.6(7) . 1_555 1_555 yes C(29) C(34) C(33) 108.7(6) . 1_555 1_555 yes C(29) C(34) C(43) 109.3(7) . 1_555 1_555 yes C(33) C(34) C(43) 111.8(7) . 1_555 1_555 yes C(33) C(35) C(36) 114.1(7) . 1_555 1_555 yes O(6) C(36) C(35) 110.6(7) . 1_555 1_555 yes O(6) C(36) C(37) 108.8(6) . 1_555 1_555 yes C(35) C(36) C(37) 111.5(7) . 1_555 1_555 yes C(36) C(37) C(38) 107.8(6) . 1_555 1_555 yes C(36) C(37) C(41) 118.3(7) . 1_555 1_555 yes C(36) C(37) C(42) 107.5(7) . 1_555 1_555 yes C(38) C(37) C(41) 100.4(6) . 1_555 1_555 yes C(38) C(37) C(42) 112.2(7) . 1_555 1_555 yes C(41) C(37) C(42) 110.5(6) . 1_555 1_555 yes C(32) C(38) C(37) 115.8(7) . 1_555 1_555 yes C(32) C(38) C(39) 119.0(7) . 1_555 1_555 yes C(37) C(38) C(39) 104.2(6) . 1_555 1_555 yes C(38) C(39) C(40) 104.7(7) . 1_555 1_555 yes C(39) C(40) C(41) 106.4(7) . 1_555 1_555 yes C(37) C(41) C(40) 103.9(6) . 1_555 1_555 yes C(37) C(41) C(44) 119.5(6) . 1_555 1_555 yes C(40) C(41) C(44) 110.7(7) . 1_555 1_555 yes C(41) C(44) C(45) 114.0(7) . 1_555 1_555 yes C(41) C(44) C(46) 111.8(6) . 1_555 1_555 yes C(45) C(44) C(46) 111.4(6) . 1_555 1_555 yes C(44) C(46) C(47) 114.6(7) . 1_555 1_555 yes C(46) C(47) C(48) 110.7(7) . 1_555 1_555 yes O(7) C(48) O(8) 121.9(8) . 1_555 1_555 yes O(7) C(48) C(47) 123.9(8) . 1_555 1_555 yes O(8) C(48) C(47) 114.2(8) . 1_555 1_555 yes C(50) C(49) C(54) 118(1) . 1_555 1_555 yes C(50) C(49) C(55) 130(1) . 1_555 1_555 yes C(54) C(49) C(55) 111(1) . 1_555 1_555 yes C(49) C(50) C(51) 124(1) . 1_555 1_555 yes C(49) C(50) C(56) 120(1) . 1_555 1_555 yes C(51) C(50) C(56) 114(1) . 1_555 1_555 yes C(50) C(51) C(52) 110(1) . 1_555 1_555 yes C(50) C(51) C(57) 126(1) . 1_555 1_555 yes C(52) C(51) C(57) 122(1) . 1_555 1_555 yes C(51) C(52) C(53) 127(1) . 1_555 1_555 yes C(52) C(53) C(54) 118(1) . 1_555 1_555 yes C(49) C(54) C(53) 119(1) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) C(2) C(1) -178.9(6) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 175.3(6) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(11) C(9) 67.1(8) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(13) C(14) -67.9(8) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(13) C(17) 46.1(9) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(13) C(18) 168.8(6) 1_555 1_555 1_555 1_555 yes O(3) C(24) C(23) C(22) -66(1) 1_555 1_555 1_555 1_555 yes O(4) C(24) C(23) C(22) 115.4(8) 1_555 1_555 1_555 1_555 yes O(5) C(27) C(26) C(25) -178.7(6) 1_555 1_555 1_555 1_555 yes O(5) C(27) C(28) C(29) 176.1(6) 1_555 1_555 1_555 1_555 yes O(6) C(36) C(35) C(33) 66.3(9) 1_555 1_555 1_555 1_555 yes O(6) C(36) C(37) C(38) -68.0(8) 1_555 1_555 1_555 1_555 yes O(6) C(36) C(37) C(41) 44.9(8) 1_555 1_555 1_555 1_555 yes O(6) C(36) C(37) C(42) 170.9(6) 1_555 1_555 1_555 1_555 yes O(7) C(48) C(47) C(46) -67(1) 1_555 1_555 1_555 1_555 yes O(8) C(48) C(47) C(46) 110.8(8) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -57.3(8) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 51.0(8) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 176.2(7) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -173.5(6) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 55.7(9) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -55.1(9) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 66.2(9) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -173.7(7) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 56.3(9) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 58.7(8) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -179.7(7) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.3(9) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 72.1(9) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -71.5(8) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 168.8(7) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 53.4(9) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -53.1(9) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 176.1(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 53.7(9) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -66.0(8) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -52.8(9) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -174.2(7) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -54.5(9) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 52.5(9) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -175.4(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) 179.5(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -56.4(9) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 66.8(9) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 53.1(9) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -58.1(9) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 177.8(7) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 62.2(9) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -165.5(7) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 55.9(9) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) 180.0(6) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -54.7(9) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) 176.6(6) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) -176.5(7) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -51.3(8) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -64.0(9) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 55.1(9) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 169.1(7) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -68.2(8) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 170.5(6) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -155.8(7) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 79.4(10) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -36.0(8) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 16.5(9) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -59.5(10) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 175.9(7) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -38.2(8) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -163.0(7) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 11.1(9) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 46.4(7) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -69.1(8) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 147.3(7) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 81.3(7) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) -179.9(7) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 55.5(9) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) 58.6(10) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -43.6(9) 1_555 1_555 1_555 1_555 yes C(20) C(22) C(23) C(24) 178.8(7) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) -67.8(9) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -55.1(9) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(28) 50.0(9) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(29) C(30) 176.3(7) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(32) -175.9(6) 1_555 1_555 1_555 1_555 yes C(25) C(34) C(33) C(35) 54.8(9) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(29) -52.3(9) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(33) 67.6(9) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(34) C(43) -170.1(7) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 54.4(9) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(34) 55.2(9) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) -179.6(6) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(34) -52.4(9) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 74.1(8) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(33) -71.7(9) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(34) C(43) 166.1(7) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) 52.1(10) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(32) -55.9(9) 1_555 1_555 1_555 1_555 yes C(29) C(34) C(33) C(35) 174.7(7) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(33) 54.5(9) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(34) C(43) -67.7(8) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) -52.0(9) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(38) -173.4(7) 1_555 1_555 1_555 1_555 yes C(31) C(30) C(29) C(34) -53.5(9) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 54.8(9) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(35) -173.8(6) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(37) 178.7(7) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(38) C(39) -55.9(9) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(43) 64.8(9) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(35) C(36) 52.6(9) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(36) -57.9(9) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(41) 177.6(7) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(37) C(42) 60.2(9) 1_555 1_555 1_555 1_555 yes C(32) C(38) C(39) C(40) -163.3(7) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(37) 56.6(9) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(38) C(39) -178.1(6) 1_555 1_555 1_555 1_555 yes C(33) C(35) C(36) C(37) -54.9(9) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(32) C(38) 177.8(6) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(35) C(36) -176.9(7) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(32) C(38) -50.8(8) 1_555 1_555 1_555 1_555 yes C(35) C(33) C(34) C(43) -64.5(9) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 54.2(9) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(41) 167.2(6) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(42) -66.9(8) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) 169.4(7) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(40) -156.7(7) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(41) C(44) 79.3(9) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) -32.5(8) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(40) C(39) 20.6(8) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(45) -58.3(9) 1_555 1_555 1_555 1_555 yes C(37) C(41) C(44) C(46) 174.3(7) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(40) -39.8(8) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(41) C(44) -163.7(7) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) 7.1(9) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(41) 44.9(8) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(42) -72.4(8) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(44) 150.1(7) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(37) C(42) 78.8(8) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(45) -178.9(7) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(44) C(46) 53.7(9) 1_555 1_555 1_555 1_555 yes C(41) C(44) C(46) C(47) 60.6(9) 1_555 1_555 1_555 1_555 yes C(42) C(37) C(41) C(44) -45.2(9) 1_555 1_555 1_555 1_555 yes C(44) C(46) C(47) C(48) 177.8(7) 1_555 1_555 1_555 1_555 yes C(45) C(44) C(46) C(47) -68.2(9) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) -2(1) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(57) -179(1) 1_555 1_555 1_555 1_555 yes C(49) C(54) C(53) C(52) 1(1) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(54) C(53) 0(1) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) 4(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(54) 1(1) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(55) -178.8(10) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) -3(1) 1_555 1_555 1_555 1_555 yes C(52) C(51) C(50) C(56) 177.1(9) 1_555 1_555 1_555 1_555 yes C(53) C(52) C(51) C(57) -178(1) 1_555 1_555 1_555 1_555 yes C(53) C(54) C(49) C(55) 179(1) 1_555 1_555 1_555 1_555 yes C(54) C(49) C(50) C(56) -178.7(9) 1_555 1_555 1_555 1_555 yes C(55) C(49) C(50) C(56) 1(1) 1_555 1_555 1_555 1_555 yes C(56) C(50) C(51) C(57) 0(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(6) 2.630(7) . 2_755 ? O(1) O(3) 2.688(8) . 1_554 ? O(1) C(36) 3.409(10) . 2_755 ? O(2) O(5) 2.656(7) . 2_756 ? O(2) O(8) 2.664(8) . 2_855 ? O(2) O(7) 3.336(7) . 2_855 ? O(2) C(48) 3.41(1) . 2_855 ? O(2) C(27) 3.57(1) . 2_756 ? O(3) O(6) 3.338(7) . 2_856 ? O(3) C(4) 3.46(1) . 1_556 ? O(3) C(3) 3.47(1) . 1_556 ? O(4) O(6) 2.641(7) . 2_856 ? O(4) C(33) 3.473(10) . 2_856 ? O(5) O(7) 2.692(7) . 1_556 ? O(5) C(12) 3.39(1) . 2_746 ? O(6) C(24) 3.400(10) . 2_846 ? O(6) C(3) 3.487(10) . 2_745 ? O(6) C(2) 3.592(10) . 2_745 ? O(7) C(28) 3.439(10) . 1_554 ? O(7) C(27) 3.469(10) . 1_554 ? O(8) C(9) 3.49(1) . 2_845 ? #------------------------------------------------------------------------------ #===END