# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1137 data_Norch #------------------------------------------------------------------------------ _audit_creation_date 'Sat Dec 26 18:35:06 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 865.20 _chemical_formula_analytical ? _chemical_formula_sum 'C49 H84 O12 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.657(1) _cell_length_b 15.309(6) _cell_length_c 7.556(2) _cell_angle_alpha 93.75(1) _cell_angle_beta 106.19(2) _cell_angle_gamma 79.15(2) _cell_volume 1162.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 209.3 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 474.00 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 209.3 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_detector_area_resol_mean 0.010000 _diffrn_mesured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_reflns_number 3609 _reflns_number_total 3609 _reflns_number_gt 3483 _reflns_observed_expression >1.5sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.1287(4) 0.5042(2) 0.2716(7) 0.085(1) Uani 1.00 d . . . O(2) O 0.2104(4) 0.2223(3) -0.1026(6) 0.0812(10) Uani 1.00 d . . . O(3) O 0.2008(3) 0.0882(2) 0.4194(4) 0.0518(7) Uani 1.00 d . . . O(4) O 0.3540(5) -0.3662(3) 0.4083(9) 0.108(1) Uani 1.00 d . . . O(5) O 0.1679(4) -0.3424(2) 0.1828(7) 0.083(1) Uani 1.00 d . . . O(6) O 0.5807(4) -0.4932(2) 0.5433(7) 0.080(1) Uani 1.00 d . . . O(7) O 0.5850(4) -0.2457(2) 0.1242(5) 0.0684(8) Uani 1.00 d . . . O(8) O 0.4675(3) -0.0586(2) 0.5863(4) 0.0511(6) Uani 1.00 d . . . O(9) O 0.3585(4) 0.3872(2) 0.4149(8) 0.095(1) Uani 1.00 d . . . O(10) O 0.5727(4) 0.3429(2) 0.4367(7) 0.085(1) Uani 1.00 d . . . O(11) O 0.4964(8) 0.5863(7) 0.985(1) 0.236(3) Uani 1.00 d . . . O(12) O 0.435(2) -0.211(1) 0.754(3) 0.341(9) Uani 1.00 d . . . C(1) C -0.1219(4) 0.3559(3) 0.2138(6) 0.0557(10) Uani 1.00 d . . . C(2) C -0.0086(4) 0.4014(3) 0.3121(6) 0.0550(10) Uani 1.00 d . . . C(3) C 0.0238(5) 0.4572(3) 0.1773(8) 0.065(1) Uani 1.00 d . . . C(4) C 0.0557(5) 0.3998(3) 0.0196(8) 0.066(1) Uani 1.00 d . . . C(5) C -0.0557(5) 0.3505(3) -0.0822(7) 0.063(1) Uani 1.00 d . . . C(6) C -0.0265(7) 0.2936(4) -0.2463(7) 0.084(1) Uani 1.00 d . . . C(7) C 0.0749(6) 0.2081(3) -0.1873(6) 0.067(1) Uani 1.00 d . . . C(8) C 0.0331(4) 0.1543(3) -0.0556(5) 0.0491(9) Uani 1.00 d . . . C(9) C 0.0089(3) 0.2123(3) 0.1117(5) 0.0419(8) Uani 1.00 d . . . C(10) C -0.1021(4) 0.2954(3) 0.0487(6) 0.0517(9) Uani 1.00 d . . . C(11) C -0.0202(4) 0.1572(3) 0.2558(5) 0.0463(8) Uani 1.00 d . . . C(12) C 0.0764(4) 0.0692(2) 0.3082(5) 0.0450(8) Uani 1.00 d . . . C(13) C 0.0913(3) 0.0130(2) 0.1349(5) 0.0424(8) Uani 1.00 d . . . C(14) C 0.1346(4) 0.0703(2) 0.0126(5) 0.0441(8) Uani 1.00 d . . . C(15) C 0.1736(5) 0.0058(3) -0.1343(6) 0.058(1) Uani 1.00 d . . . C(16) C 0.2303(4) -0.0832(3) -0.0315(6) 0.0537(9) Uani 1.00 d . . . C(17) C 0.2038(3) -0.0702(2) 0.1606(5) 0.0435(8) Uani 1.00 d . . . C(18) C -0.0415(4) -0.0170(3) 0.0410(7) 0.059(1) Uani 1.00 d . . . C(19) C -0.2362(5) 0.2690(3) -0.0489(8) 0.069(1) Uani 1.00 d . . . C(20) C 0.1805(4) -0.1560(3) 0.2347(7) 0.0540(9) Uani 1.00 d . . . C(21) C 0.1593(5) -0.1438(3) 0.4284(8) 0.065(1) Uani 1.00 d . . . C(22) C 0.3004(4) -0.2301(3) 0.2407(7) 0.059(1) Uani 1.00 d . . . C(23) C 0.2775(5) -0.3190(3) 0.2866(8) 0.068(1) Uani 1.00 d . . . C(24) C 0.8103(4) -0.3329(3) 0.7675(5) 0.0515(9) Uani 1.00 d . . . C(25) C 0.6897(5) -0.3791(3) 0.7307(6) 0.059(1) Uani 1.00 d . . . C(26) C 0.6920(5) -0.4478(3) 0.5771(7) 0.064(1) Uani 1.00 d . . . C(27) C 0.6977(5) -0.4042(3) 0.4039(7) 0.063(1) Uani 1.00 d . . . C(28) C 0.8152(4) -0.3547(3) 0.4374(6) 0.0554(9) Uani 1.00 d . . . C(29) C 0.8186(5) -0.3144(3) 0.2588(6) 0.068(1) Uani 1.00 d . . . C(30) C 0.7192(5) -0.2301(3) 0.2000(5) 0.0594(9) Uani 1.00 d . . . C(31) C 0.7232(4) -0.1622(3) 0.3586(5) 0.0468(8) Uani 1.00 d . . . C(32) C 0.7080(3) -0.2039(2) 0.5337(5) 0.0411(7) Uani 1.00 d . . . C(33) C 0.8192(4) -0.2861(2) 0.5976(5) 0.0453(8) Uani 1.00 d . . . C(34) C 0.6980(4) -0.1359(3) 0.6880(5) 0.0448(8) Uani 1.00 d . . . C(35) C 0.6038(4) -0.0468(3) 0.6296(5) 0.0441(7) Uani 1.00 d . . . C(36) C 0.6300(3) -0.0072(2) 0.4633(5) 0.0410(7) Uani 1.00 d . . . C(37) C 0.6179(3) -0.0780(2) 0.3078(5) 0.0422(8) Uani 1.00 d . . . C(38) C 0.6139(4) -0.0284(3) 0.1356(5) 0.0485(8) Uani 1.00 d . . . C(39) C 0.5483(4) 0.0676(3) 0.1665(6) 0.0537(9) Uani 1.00 d . . . C(40) C 0.5258(4) 0.0729(2) 0.3633(6) 0.0449(8) Uani 1.00 d . . . C(41) C 0.7698(4) 0.0195(3) 0.5252(7) 0.0551(10) Uani 1.00 d . . . C(42) C 0.9583(4) -0.2579(3) 0.6598(7) 0.060(1) Uani 1.00 d . . . C(43) C 0.5276(4) 0.1653(2) 0.4569(7) 0.0555(9) Uani 1.00 d . . . C(44) C 0.4979(5) 0.1710(3) 0.6438(7) 0.065(1) Uani 1.00 d . . . C(45) C 0.4299(5) 0.2373(3) 0.3304(8) 0.070(1) Uani 1.00 d . . . C(46) C 0.4493(5) 0.3296(3) 0.3977(8) 0.066(1) Uani 1.00 d . . . C(47) C 0.427(2) 0.446(1) 0.947(2) 0.237(4) Uani 1.00 d . . . C(48) C 0.4086(10) 0.5428(9) 0.912(1) 0.138(3) Uani 1.00 d . . . C(49) C 0.274(1) 0.554(2) 0.773(2) 0.274(6) Uani 1.00 d . . . H(1) H -0.1385 0.3200 0.3007 0.0647 Uiso 1.00 calc . . . H(2) H -0.1984 0.4002 0.1699 0.0647 Uiso 1.00 calc . . . H(3) H -0.0330 0.4389 0.4071 0.0638 Uiso 1.00 calc . . . H(4) H 0.0666 0.3580 0.3647 0.0638 Uiso 1.00 calc . . . H(5) H -0.0535 0.4997 0.1273 0.0760 Uiso 1.00 calc . . . H(6) H 0.0707 0.4365 -0.0648 0.0763 Uiso 1.00 calc . . . H(7) H 0.1325 0.3570 0.0676 0.0763 Uiso 1.00 calc . . . H(8) H -0.1297 0.3954 -0.1329 0.0740 Uiso 1.00 calc . . . H(9) H 0.0087 0.3286 -0.3154 0.0977 Uiso 1.00 calc . . . H(10) H -0.1071 0.2792 -0.3222 0.0977 Uiso 1.00 calc . . . H(11) H 0.0741 0.1726 -0.2965 0.0791 Uiso 1.00 calc . . . H(12) H -0.0491 0.1358 -0.1198 0.0569 Uiso 1.00 calc . . . H(13) H 0.0884 0.2339 0.1697 0.0486 Uiso 1.00 calc . . . H(14) H -0.0165 0.1926 0.3648 0.0540 Uiso 1.00 calc . . . H(15) H -0.1071 0.1444 0.2074 0.0540 Uiso 1.00 calc . . . H(16) H 0.0414 0.0363 0.3795 0.0520 Uiso 1.00 calc . . . H(17) H 0.2136 0.0892 0.0851 0.0521 Uiso 1.00 calc . . . H(18) H 0.2383 0.0241 -0.1808 0.0663 Uiso 1.00 calc . . . H(19) H 0.0976 -0.0004 -0.2354 0.0663 Uiso 1.00 calc . . . H(20) H 0.3227 -0.0989 -0.0186 0.0619 Uiso 1.00 calc . . . H(21) H 0.1870 -0.1297 -0.0978 0.0619 Uiso 1.00 calc . . . H(22) H 0.2806 -0.0540 0.2449 0.0489 Uiso 1.00 calc . . . H(23) H -0.0255 -0.0764 -0.0030 0.0679 Uiso 1.00 calc . . . H(24) H -0.0917 -0.0147 0.1291 0.0679 Uiso 1.00 calc . . . H(25) H -0.0902 0.0211 -0.0575 0.0679 Uiso 1.00 calc . . . H(26) H -0.2267 0.2297 -0.1500 0.0790 Uiso 1.00 calc . . . H(27) H -0.2657 0.2396 0.0343 0.0790 Uiso 1.00 calc . . . H(28) H -0.2994 0.3206 -0.0946 0.0790 Uiso 1.00 calc . . . H(29) H 0.1034 -0.1737 0.1517 0.0629 Uiso 1.00 calc . . . H(30) H 0.1441 -0.1991 0.4648 0.0754 Uiso 1.00 calc . . . H(31) H 0.0822 -0.0999 0.4252 0.0754 Uiso 1.00 calc . . . H(32) H 0.2338 -0.1272 0.5120 0.0754 Uiso 1.00 calc . . . H(33) H 0.3741 -0.2149 0.3341 0.0691 Uiso 1.00 calc . . . H(34) H 0.3186 -0.2341 0.1255 0.0691 Uiso 1.00 calc . . . H(35) H 0.2091 0.4622 0.2885 0.1018 Uiso 1.00 calc . . . H(36) H 0.2693 0.2410 -0.1719 0.0973 Uiso 1.00 calc . . . H(37) H 0.2801 0.0280 0.4257 0.0619 Uiso 1.00 calc . . . H(38) H 0.1411 -0.4003 0.1315 0.1003 Uiso 1.00 calc . . . H(39) H 0.8064 -0.2899 0.8633 0.0575 Uiso 1.00 calc . . . H(40) H 0.8879 -0.3767 0.8062 0.0575 Uiso 1.00 calc . . . H(41) H 0.6903 -0.4070 0.8396 0.0680 Uiso 1.00 calc . . . H(42) H 0.6100 -0.3352 0.6956 0.0680 Uiso 1.00 calc . . . H(43) H 0.7699 -0.4900 0.6167 0.0753 Uiso 1.00 calc . . . H(44) H 0.7059 -0.4496 0.3129 0.0725 Uiso 1.00 calc . . . H(45) H 0.6172 -0.3633 0.3583 0.0725 Uiso 1.00 calc . . . H(46) H 0.8938 -0.3974 0.4744 0.0631 Uiso 1.00 calc . . . H(47) H 0.8006 -0.3581 0.1639 0.0752 Uiso 1.00 calc . . . H(48) H 0.9055 -0.3030 0.2752 0.0752 Uiso 1.00 calc . . . H(49) H 0.7439 -0.2034 0.1068 0.0695 Uiso 1.00 calc . . . H(50) H 0.8068 -0.1443 0.3904 0.0530 Uiso 1.00 calc . . . H(51) H 0.6256 -0.2254 0.4978 0.0467 Uiso 1.00 calc . . . H(52) H 0.6678 -0.1617 0.7757 0.0528 Uiso 1.00 calc . . . H(53) H 0.7840 -0.1232 0.7431 0.0528 Uiso 1.00 calc . . . H(54) H 0.6190 -0.0059 0.7308 0.0507 Uiso 1.00 calc . . . H(55) H 0.5327 -0.0943 0.2876 0.0495 Uiso 1.00 calc . . . H(56) H 0.7015 -0.0302 0.1269 0.0568 Uiso 1.00 calc . . . H(57) H 0.5635 -0.0539 0.0282 0.0568 Uiso 1.00 calc . . . H(58) H 0.4654 0.0816 0.0754 0.0609 Uiso 1.00 calc . . . H(59) H 0.6042 0.1075 0.1579 0.0609 Uiso 1.00 calc . . . H(60) H 0.4402 0.0591 0.3507 0.0511 Uiso 1.00 calc . . . H(61) H 0.7857 0.0451 0.4231 0.0650 Uiso 1.00 calc . . . H(62) H 0.7729 0.0622 0.6226 0.0650 Uiso 1.00 calc . . . H(63) H 0.8359 -0.0312 0.5648 0.0650 Uiso 1.00 calc . . . H(64) H 0.9723 -0.2289 0.5622 0.0708 Uiso 1.00 calc . . . H(65) H 0.9626 -0.2190 0.7638 0.0708 Uiso 1.00 calc . . . H(66) H 1.0247 -0.3097 0.6927 0.0708 Uiso 1.00 calc . . . H(67) H 0.6139 0.1781 0.4770 0.0624 Uiso 1.00 calc . . . H(68) H 0.5039 0.2288 0.6967 0.0745 Uiso 1.00 calc . . . H(69) H 0.5582 0.1278 0.7242 0.0745 Uiso 1.00 calc . . . H(70) H 0.4092 0.1608 0.6284 0.0745 Uiso 1.00 calc . . . H(71) H 0.3418 0.2312 0.3269 0.0786 Uiso 1.00 calc . . . H(72) H 0.4421 0.2287 0.2113 0.0786 Uiso 1.00 calc . . . H(73) H 0.5051 -0.4469 0.4765 0.0957 Uiso 1.00 calc . . . H(74) H 0.5636 -0.3137 0.0831 0.0815 Uiso 1.00 calc . . . H(75) H 0.4668 -0.1206 0.6210 0.0608 Uiso 1.00 calc . . . H(76) H 0.5964 0.3927 0.5230 0.1018 Uiso 1.00 calc . . . H(77) H 0.4487 0.4393 1.0847 0.2827 Uiso 1.00 calc . . . H(78) H 0.5121 0.4164 0.9221 0.2827 Uiso 1.00 calc . . . H(79) H 0.3614 0.4183 0.8908 0.2827 Uiso 1.00 calc . . . H(80) H 0.2787 0.5088 0.6622 0.3222 Uiso 1.00 calc . . . H(81) H 0.2073 0.5318 0.8167 0.3222 Uiso 1.00 calc . . . H(82) H 0.2408 0.6072 0.7199 0.3222 Uiso 1.00 calc . . . H(83) H 0.3386 -0.2108 0.8053 0.4088 Uiso 1.00 calc . . . H(84) H 0.5366 -0.2113 0.8452 0.4088 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) 0.089(2) 0.041(1) 0.132(3) -0.017(1) 0.035(2) -0.002(2) O(2) 0.098(2) 0.063(2) 0.101(2) 0.001(1) 0.061(1) 0.023(2) O(3) 0.058(1) 0.058(1) 0.039(1) -0.016(1) 0.0090(10) -0.002(1) O(4) 0.096(3) 0.075(2) 0.145(4) -0.002(2) 0.016(2) 0.058(2) O(5) 0.096(2) 0.052(2) 0.102(3) -0.033(1) 0.010(2) 0.009(2) O(6) 0.090(2) 0.044(2) 0.100(3) -0.026(1) 0.003(2) 0.005(2) O(7) 0.086(2) 0.060(2) 0.042(1) 0.003(1) 0.000(1) -0.006(1) O(8) 0.054(1) 0.054(1) 0.053(1) -0.0101(10) 0.0236(10) 0.005(1) O(9) 0.078(2) 0.047(2) 0.148(4) 0.002(1) 0.021(2) -0.008(2) O(10) 0.084(2) 0.045(2) 0.124(3) -0.023(1) 0.018(2) -0.009(2) O(11) 0.264(5) 0.351(7) 0.162(7) -0.240(4) 0.066(5) -0.078(6) O(12) 0.40(2) 0.36(2) 0.31(2) -0.11(1) 0.12(1) 0.11(1) C(1) 0.062(2) 0.049(2) 0.054(2) -0.003(1) 0.016(2) 0.000(2) C(2) 0.064(2) 0.035(2) 0.063(2) 0.000(1) 0.019(2) -0.001(1) C(3) 0.072(2) 0.043(2) 0.084(2) -0.001(1) 0.026(2) 0.019(2) C(4) 0.080(2) 0.044(2) 0.083(2) -0.001(2) 0.037(2) 0.025(2) C(5) 0.081(2) 0.056(2) 0.055(2) -0.001(2) 0.026(2) 0.017(2) C(6) 0.127(4) 0.070(3) 0.043(2) 0.026(2) 0.030(2) 0.028(2) C(7) 0.108(2) 0.056(2) 0.042(2) 0.001(2) 0.035(2) 0.012(2) C(8) 0.058(2) 0.047(2) 0.038(2) -0.002(1) 0.011(1) 0.002(1) C(9) 0.042(1) 0.045(2) 0.039(1) -0.004(1) 0.013(1) 0.003(1) C(10) 0.054(2) 0.045(2) 0.051(2) -0.001(1) 0.010(1) 0.005(1) C(11) 0.058(2) 0.040(2) 0.043(2) -0.006(1) 0.018(1) 0.004(1) C(12) 0.056(1) 0.040(2) 0.042(2) -0.009(1) 0.017(1) 0.001(1) C(13) 0.046(1) 0.039(2) 0.044(2) -0.010(1) 0.014(1) -0.004(1) C(14) 0.054(2) 0.041(2) 0.039(2) -0.007(1) 0.015(1) -0.001(1) C(15) 0.083(2) 0.049(2) 0.042(2) -0.007(2) 0.020(2) -0.004(1) C(16) 0.061(2) 0.049(2) 0.049(2) -0.004(2) 0.017(1) -0.003(1) C(17) 0.044(2) 0.038(1) 0.048(2) -0.008(1) 0.012(1) 0.000(1) C(18) 0.052(2) 0.053(2) 0.064(2) -0.015(2) 0.000(2) 0.000(2) C(19) 0.053(2) 0.064(3) 0.070(3) 0.006(2) -0.008(2) 0.004(2) C(20) 0.056(2) 0.037(2) 0.072(2) -0.014(1) 0.016(2) 0.006(2) C(21) 0.077(2) 0.052(2) 0.079(2) -0.014(2) 0.037(2) 0.011(2) C(22) 0.053(2) 0.052(2) 0.076(3) -0.008(1) 0.019(2) 0.011(2) C(23) 0.078(2) 0.043(2) 0.091(3) -0.009(2) 0.036(2) -0.004(2) C(24) 0.069(2) 0.042(2) 0.040(2) -0.003(1) 0.011(2) 0.007(1) C(25) 0.081(2) 0.048(2) 0.047(2) -0.020(2) 0.011(2) 0.005(1) C(26) 0.087(2) 0.036(2) 0.065(2) -0.015(2) 0.010(2) -0.001(1) C(27) 0.080(2) 0.045(2) 0.051(2) 0.000(2) 0.004(2) -0.012(2) C(28) 0.070(2) 0.048(2) 0.041(2) 0.013(1) 0.018(2) 0.000(1) C(29) 0.082(2) 0.069(2) 0.044(2) 0.028(2) 0.029(2) 0.013(2) C(30) 0.079(2) 0.061(2) 0.034(2) 0.012(2) 0.024(1) 0.005(1) C(31) 0.056(2) 0.050(2) 0.038(2) -0.003(1) 0.022(1) 0.007(1) C(32) 0.048(2) 0.042(2) 0.034(1) -0.005(1) 0.015(1) 0.001(1) C(33) 0.052(2) 0.042(2) 0.040(2) -0.005(1) 0.012(1) 0.002(1) C(34) 0.061(2) 0.043(2) 0.032(1) -0.008(1) 0.015(1) 0.002(1) C(35) 0.054(1) 0.043(2) 0.039(2) -0.012(1) 0.018(1) -0.004(1) C(36) 0.049(1) 0.038(1) 0.038(1) -0.015(1) 0.010(1) 0.000(1) C(37) 0.052(2) 0.046(2) 0.030(1) -0.005(1) 0.015(1) 0.002(1) C(38) 0.054(2) 0.054(2) 0.038(2) 0.004(1) 0.018(1) 0.014(1) C(39) 0.060(2) 0.049(2) 0.054(2) -0.003(1) 0.019(1) 0.015(2) C(40) 0.047(2) 0.036(1) 0.050(2) -0.005(1) 0.012(1) 0.003(1) C(41) 0.046(2) 0.054(2) 0.062(2) -0.018(1) 0.001(1) 0.009(2) C(42) 0.047(2) 0.063(2) 0.064(3) -0.009(2) 0.004(2) 0.015(2) C(43) 0.060(2) 0.033(2) 0.068(2) -0.015(1) 0.003(2) 0.000(1) C(44) 0.078(2) 0.043(2) 0.071(2) -0.015(2) 0.016(2) -0.010(2) C(45) 0.072(3) 0.038(2) 0.081(3) -0.009(2) -0.006(2) 0.000(2) C(46) 0.080(2) 0.036(2) 0.072(3) -0.009(1) 0.007(2) 0.002(2) C(47) 0.322(10) 0.177(7) 0.241(10) 0.120(8) 0.208(7) 0.092(8) C(48) 0.135(4) 0.175(6) 0.096(5) 0.030(4) 0.056(3) 0.016(5) C(49) 0.119(5) 0.51(2) 0.154(8) 0.106(9) 0.040(4) 0.177(10) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F^2^ against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^, conventional R-factors (R) are calculated on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 1.5sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.04000(Fo^2^)^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3534 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0902 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.2560 _refine_ls_wR_factor_gt 0.2534 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.255 _refine_ls_shift/su_max 1.6710 _refine_ls_shift/su_mean 0.0740 _refine_diff_density_min -0.40 _refine_diff_density_max 0.64 #------------------------------------------------------------------------------ _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) 1.439(7) 1_555 1_555 yes O(2) C(7) 1.456(8) 1_555 1_555 yes O(3) C(12) 1.429(5) 1_555 1_555 yes O(4) C(23) 1.211(8) 1_555 1_555 yes O(5) C(23) 1.313(7) 1_555 1_555 yes O(6) C(26) 1.439(7) 1_555 1_555 yes O(7) C(30) 1.446(7) 1_555 1_555 yes O(8) C(35) 1.438(5) 1_555 1_555 yes O(9) C(46) 1.214(7) 1_555 1_555 yes O(10) C(46) 1.315(7) 1_555 1_555 yes O(11) C(48) 1.23(2) 1_555 1_555 yes C(1) C(2) 1.498(7) 1_555 1_555 yes C(1) C(10) 1.543(7) 1_555 1_555 yes C(2) C(3) 1.521(8) 1_555 1_555 yes C(3) C(4) 1.511(9) 1_555 1_555 yes C(4) C(5) 1.525(8) 1_555 1_555 yes C(5) C(6) 1.539(8) 1_555 1_555 yes C(5) C(10) 1.571(7) 1_555 1_555 yes C(6) C(7) 1.532(7) 1_555 1_555 yes C(7) C(8) 1.537(7) 1_555 1_555 yes C(8) C(9) 1.550(6) 1_555 1_555 yes C(8) C(14) 1.530(5) 1_555 1_555 yes C(9) C(10) 1.565(5) 1_555 1_555 yes C(9) C(11) 1.548(6) 1_555 1_555 yes C(10) C(19) 1.528(7) 1_555 1_555 yes C(11) C(12) 1.533(6) 1_555 1_555 yes C(12) C(13) 1.548(6) 1_555 1_555 yes C(13) C(14) 1.528(6) 1_555 1_555 yes C(13) C(17) 1.557(5) 1_555 1_555 yes C(13) C(18) 1.535(6) 1_555 1_555 yes C(14) C(15) 1.529(6) 1_555 1_555 yes C(15) C(16) 1.546(7) 1_555 1_555 yes C(16) C(17) 1.546(6) 1_555 1_555 yes C(17) C(20) 1.547(6) 1_555 1_555 yes C(20) C(21) 1.539(8) 1_555 1_555 yes C(20) C(22) 1.533(6) 1_555 1_555 yes C(22) C(23) 1.508(8) 1_555 1_555 yes C(24) C(25) 1.531(7) 1_555 1_555 yes C(24) C(33) 1.543(6) 1_555 1_555 yes C(25) C(26) 1.517(7) 1_555 1_555 yes C(26) C(27) 1.531(8) 1_555 1_555 yes C(27) C(28) 1.534(8) 1_555 1_555 yes C(28) C(29) 1.532(7) 1_555 1_555 yes C(28) C(33) 1.547(6) 1_555 1_555 yes C(29) C(30) 1.509(6) 1_555 1_555 yes C(30) C(31) 1.532(6) 1_555 1_555 yes C(31) C(32) 1.566(5) 1_555 1_555 yes C(31) C(37) 1.533(5) 1_555 1_555 yes C(32) C(33) 1.556(5) 1_555 1_555 yes C(32) C(34) 1.524(5) 1_555 1_555 yes C(33) C(42) 1.560(6) 1_555 1_555 yes C(34) C(35) 1.545(6) 1_555 1_555 yes C(35) C(36) 1.543(6) 1_555 1_555 yes C(36) C(37) 1.541(5) 1_555 1_555 yes C(36) C(40) 1.565(5) 1_555 1_555 yes C(36) C(41) 1.557(6) 1_555 1_555 yes C(37) C(38) 1.535(6) 1_555 1_555 yes C(38) C(39) 1.538(6) 1_555 1_555 yes C(39) C(40) 1.565(7) 1_555 1_555 yes C(40) C(43) 1.539(6) 1_555 1_555 yes C(43) C(44) 1.524(9) 1_555 1_555 yes C(43) C(45) 1.537(7) 1_555 1_555 yes C(45) C(46) 1.501(7) 1_555 1_555 yes C(47) C(48) 1.49(2) 1_555 1_555 yes C(48) C(49) 1.52(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(3) O(1) H(35) 106.2(4) 1_555 1_555 1_555 no C(7) O(2) H(36) 124.2(4) 1_555 1_555 1_555 no C(12) O(3) H(37) 109.7(3) 1_555 1_555 1_555 no C(23) O(5) H(38) 134.8(4) 1_555 1_555 1_555 no C(26) O(6) H(73) 102.1(4) 1_555 1_555 1_555 no C(30) O(7) H(74) 121.4(3) 1_555 1_555 1_555 no C(35) O(8) H(75) 108.0(3) 1_555 1_555 1_555 no C(46) O(10) H(76) 117.0(5) 1_555 1_555 1_555 no H(83) O(12) H(84) 123(2) 1_555 1_555 1_555 no C(2) C(1) C(10) 116.2(4) 1_555 1_555 1_555 yes C(2) C(1) H(1) 108.1(4) 1_555 1_555 1_555 no C(2) C(1) H(2) 108.4(4) 1_555 1_555 1_555 no C(10) C(1) H(1) 107.4(4) 1_555 1_555 1_555 no C(10) C(1) H(2) 107.6(4) 1_555 1_555 1_555 no H(1) C(1) H(2) 108.8(5) 1_555 1_555 1_555 no C(1) C(2) C(3) 109.7(4) 1_555 1_555 1_555 yes C(1) C(2) H(3) 109.1(4) 1_555 1_555 1_555 no C(1) C(2) H(4) 109.4(4) 1_555 1_555 1_555 no C(3) C(2) H(3) 109.3(4) 1_555 1_555 1_555 no C(3) C(2) H(4) 109.8(5) 1_555 1_555 1_555 no H(3) C(2) H(4) 109.5(5) 1_555 1_555 1_555 no O(1) C(3) C(2) 110.3(5) 1_555 1_555 1_555 yes O(1) C(3) C(4) 112.6(5) 1_555 1_555 1_555 yes O(1) C(3) H(5) 108.3(5) 1_555 1_555 1_555 no C(2) C(3) C(4) 110.3(4) 1_555 1_555 1_555 yes C(2) C(3) H(5) 107.4(5) 1_555 1_555 1_555 no C(4) C(3) H(5) 107.7(5) 1_555 1_555 1_555 no C(3) C(4) C(5) 112.9(5) 1_555 1_555 1_555 yes C(3) C(4) H(6) 108.4(5) 1_555 1_555 1_555 no C(3) C(4) H(7) 108.4(5) 1_555 1_555 1_555 no C(5) C(4) H(6) 108.4(5) 1_555 1_555 1_555 no C(5) C(4) H(7) 108.1(5) 1_555 1_555 1_555 no H(6) C(4) H(7) 110.7(6) 1_555 1_555 1_555 no C(4) C(5) C(6) 113.4(5) 1_555 1_555 1_555 yes C(4) C(5) C(10) 113.4(4) 1_555 1_555 1_555 yes C(4) C(5) H(8) 105.6(5) 1_555 1_555 1_555 no C(6) C(5) C(10) 111.6(4) 1_555 1_555 1_555 yes C(6) C(5) H(8) 106.2(5) 1_555 1_555 1_555 no C(10) C(5) H(8) 105.9(5) 1_555 1_555 1_555 no C(5) C(6) C(7) 113.2(4) 1_555 1_555 1_555 yes C(5) C(6) H(9) 108.1(6) 1_555 1_555 1_555 no C(5) C(6) H(10) 108.3(6) 1_555 1_555 1_555 no C(7) C(6) H(9) 108.5(6) 1_555 1_555 1_555 no C(7) C(6) H(10) 109.9(6) 1_555 1_555 1_555 no H(9) C(6) H(10) 108.8(5) 1_555 1_555 1_555 no O(2) C(7) C(6) 114.4(5) 1_555 1_555 1_555 yes O(2) C(7) C(8) 108.9(4) 1_555 1_555 1_555 yes O(2) C(7) H(11) 108.6(5) 1_555 1_555 1_555 no C(6) C(7) C(8) 111.0(5) 1_555 1_555 1_555 yes C(6) C(7) H(11) 106.6(4) 1_555 1_555 1_555 no C(8) C(7) H(11) 107.0(5) 1_555 1_555 1_555 no C(7) C(8) C(9) 111.0(4) 1_555 1_555 1_555 yes C(7) C(8) C(14) 112.7(4) 1_555 1_555 1_555 yes C(7) C(8) H(12) 108.9(4) 1_555 1_555 1_555 no C(9) C(8) C(14) 109.5(3) 1_555 1_555 1_555 yes C(9) C(8) H(12) 107.4(4) 1_555 1_555 1_555 no C(14) C(8) H(12) 107.2(4) 1_555 1_555 1_555 no C(8) C(9) C(10) 111.2(3) 1_555 1_555 1_555 yes C(8) C(9) C(11) 111.9(3) 1_555 1_555 1_555 yes C(8) C(9) H(13) 107.1(4) 1_555 1_555 1_555 no C(10) C(9) C(11) 112.1(3) 1_555 1_555 1_555 yes C(10) C(9) H(13) 106.8(4) 1_555 1_555 1_555 no C(11) C(9) H(13) 107.3(4) 1_555 1_555 1_555 no C(1) C(10) C(5) 107.9(4) 1_555 1_555 1_555 yes C(1) C(10) C(9) 111.6(3) 1_555 1_555 1_555 yes C(1) C(10) C(19) 107.2(4) 1_555 1_555 1_555 yes C(5) C(10) C(9) 107.4(4) 1_555 1_555 1_555 yes C(5) C(10) C(19) 110.8(4) 1_555 1_555 1_555 yes C(9) C(10) C(19) 111.9(4) 1_555 1_555 1_555 yes C(9) C(11) C(12) 115.0(3) 1_555 1_555 1_555 yes C(9) C(11) H(14) 108.0(4) 1_555 1_555 1_555 no C(9) C(11) H(15) 108.0(4) 1_555 1_555 1_555 no C(12) C(11) H(14) 108.1(4) 1_555 1_555 1_555 no C(12) C(11) H(15) 108.2(4) 1_555 1_555 1_555 no H(14) C(11) H(15) 109.3(4) 1_555 1_555 1_555 no O(3) C(12) C(11) 108.6(3) 1_555 1_555 1_555 yes O(3) C(12) C(13) 111.9(3) 1_555 1_555 1_555 yes O(3) C(12) H(16) 108.5(4) 1_555 1_555 1_555 no C(11) C(12) C(13) 111.3(3) 1_555 1_555 1_555 yes C(11) C(12) H(16) 108.1(4) 1_555 1_555 1_555 no C(13) C(12) H(16) 108.3(4) 1_555 1_555 1_555 no C(12) C(13) C(14) 107.6(3) 1_555 1_555 1_555 yes C(12) C(13) C(17) 118.0(3) 1_555 1_555 1_555 yes C(12) C(13) C(18) 108.4(3) 1_555 1_555 1_555 yes C(14) C(13) C(17) 101.2(3) 1_555 1_555 1_555 yes C(14) C(13) C(18) 113.3(4) 1_555 1_555 1_555 yes C(17) C(13) C(18) 108.4(3) 1_555 1_555 1_555 yes C(8) C(14) C(13) 113.7(3) 1_555 1_555 1_555 yes C(8) C(14) C(15) 117.0(3) 1_555 1_555 1_555 yes C(8) C(14) H(17) 106.9(4) 1_555 1_555 1_555 no C(13) C(14) C(15) 104.5(3) 1_555 1_555 1_555 yes C(13) C(14) H(17) 107.2(4) 1_555 1_555 1_555 no C(15) C(14) H(17) 106.9(4) 1_555 1_555 1_555 no C(14) C(15) C(16) 103.8(4) 1_555 1_555 1_555 yes C(14) C(15) H(18) 112.1(4) 1_555 1_555 1_555 no C(14) C(15) H(19) 111.2(4) 1_555 1_555 1_555 no C(16) C(15) H(18) 110.7(5) 1_555 1_555 1_555 no C(16) C(15) H(19) 110.4(4) 1_555 1_555 1_555 no H(18) C(15) H(19) 108.7(5) 1_555 1_555 1_555 no C(15) C(16) C(17) 107.5(4) 1_555 1_555 1_555 yes C(15) C(16) H(20) 110.3(5) 1_555 1_555 1_555 no C(15) C(16) H(21) 110.2(4) 1_555 1_555 1_555 no C(17) C(16) H(20) 110.2(4) 1_555 1_555 1_555 no C(17) C(16) H(21) 109.7(4) 1_555 1_555 1_555 no H(20) C(16) H(21) 108.9(4) 1_555 1_555 1_555 no C(13) C(17) C(16) 103.1(3) 1_555 1_555 1_555 yes C(13) C(17) C(20) 118.1(3) 1_555 1_555 1_555 yes C(13) C(17) H(22) 107.3(3) 1_555 1_555 1_555 no C(16) C(17) C(20) 113.2(4) 1_555 1_555 1_555 yes C(16) C(17) H(22) 107.8(4) 1_555 1_555 1_555 no C(20) C(17) H(22) 106.9(4) 1_555 1_555 1_555 no C(13) C(18) H(23) 109.7(4) 1_555 1_555 1_555 no C(13) C(18) H(24) 109.1(4) 1_555 1_555 1_555 no C(13) C(18) H(25) 110.1(4) 1_555 1_555 1_555 no H(23) C(18) H(24) 108.5(5) 1_555 1_555 1_555 no H(23) C(18) H(25) 110.2(5) 1_555 1_555 1_555 no H(24) C(18) H(25) 109.1(5) 1_555 1_555 1_555 no C(10) C(19) H(26) 109.5(5) 1_555 1_555 1_555 no C(10) C(19) H(27) 109.9(5) 1_555 1_555 1_555 no C(10) C(19) H(28) 109.9(5) 1_555 1_555 1_555 no H(26) C(19) H(27) 109.0(6) 1_555 1_555 1_555 no H(26) C(19) H(28) 109.0(6) 1_555 1_555 1_555 no H(27) C(19) H(28) 109.6(6) 1_555 1_555 1_555 no C(17) C(20) C(21) 113.1(4) 1_555 1_555 1_555 yes C(17) C(20) C(22) 109.2(4) 1_555 1_555 1_555 yes C(17) C(20) H(29) 108.4(4) 1_555 1_555 1_555 no C(21) C(20) C(22) 108.5(4) 1_555 1_555 1_555 yes C(21) C(20) H(29) 108.7(4) 1_555 1_555 1_555 no C(22) C(20) H(29) 108.8(4) 1_555 1_555 1_555 no C(20) C(21) H(30) 108.6(5) 1_555 1_555 1_555 no C(20) C(21) H(31) 109.3(5) 1_555 1_555 1_555 no C(20) C(21) H(32) 110.1(5) 1_555 1_555 1_555 no H(30) C(21) H(31) 108.1(5) 1_555 1_555 1_555 no H(30) C(21) H(32) 110.1(6) 1_555 1_555 1_555 no H(31) C(21) H(32) 110.7(6) 1_555 1_555 1_555 no C(20) C(22) C(23) 112.5(4) 1_555 1_555 1_555 yes C(20) C(22) H(33) 108.1(5) 1_555 1_555 1_555 no C(20) C(22) H(34) 108.9(4) 1_555 1_555 1_555 no C(23) C(22) H(33) 108.0(5) 1_555 1_555 1_555 no C(23) C(22) H(34) 109.1(5) 1_555 1_555 1_555 no H(33) C(22) H(34) 110.2(5) 1_555 1_555 1_555 no O(4) C(23) O(5) 122.0(5) 1_555 1_555 1_555 yes O(4) C(23) C(22) 123.8(5) 1_555 1_555 1_555 yes O(5) C(23) C(22) 114.2(5) 1_555 1_555 1_555 yes C(25) C(24) C(33) 113.9(3) 1_555 1_555 1_555 yes C(25) C(24) H(39) 108.6(5) 1_555 1_555 1_555 no C(25) C(24) H(40) 107.8(4) 1_555 1_555 1_555 no C(33) C(24) H(39) 108.8(4) 1_555 1_555 1_555 no C(33) C(24) H(40) 108.3(4) 1_555 1_555 1_555 no H(39) C(24) H(40) 109.4(4) 1_555 1_555 1_555 no C(24) C(25) C(26) 110.2(4) 1_555 1_555 1_555 yes C(24) C(25) H(41) 110.0(4) 1_555 1_555 1_555 no C(24) C(25) H(42) 109.0(4) 1_555 1_555 1_555 no C(26) C(25) H(41) 109.7(4) 1_555 1_555 1_555 no C(26) C(25) H(42) 109.5(4) 1_555 1_555 1_555 no H(41) C(25) H(42) 108.4(6) 1_555 1_555 1_555 no O(6) C(26) C(25) 110.9(5) 1_555 1_555 1_555 yes O(6) C(26) C(27) 112.4(4) 1_555 1_555 1_555 yes O(6) C(26) H(43) 108.0(4) 1_555 1_555 1_555 no C(25) C(26) C(27) 110.0(4) 1_555 1_555 1_555 yes C(25) C(26) H(43) 107.4(5) 1_555 1_555 1_555 no C(27) C(26) H(43) 108.1(6) 1_555 1_555 1_555 no C(26) C(27) C(28) 113.2(4) 1_555 1_555 1_555 yes C(26) C(27) H(44) 108.2(5) 1_555 1_555 1_555 no C(26) C(27) H(45) 109.1(5) 1_555 1_555 1_555 no C(28) C(27) H(44) 108.5(5) 1_555 1_555 1_555 no C(28) C(27) H(45) 109.0(5) 1_555 1_555 1_555 no H(44) C(27) H(45) 108.8(5) 1_555 1_555 1_555 no C(27) C(28) C(29) 111.2(4) 1_555 1_555 1_555 yes C(27) C(28) C(33) 112.4(4) 1_555 1_555 1_555 yes C(27) C(28) H(46) 107.2(5) 1_555 1_555 1_555 no C(29) C(28) C(33) 112.8(4) 1_555 1_555 1_555 yes C(29) C(28) H(46) 106.7(4) 1_555 1_555 1_555 no C(33) C(28) H(46) 106.1(4) 1_555 1_555 1_555 no C(28) C(29) C(30) 115.1(4) 1_555 1_555 1_555 yes C(28) C(29) H(47) 106.7(5) 1_555 1_555 1_555 no C(28) C(29) H(48) 107.7(4) 1_555 1_555 1_555 no C(30) C(29) H(47) 108.1(4) 1_555 1_555 1_555 no C(30) C(29) H(48) 109.6(5) 1_555 1_555 1_555 no H(47) C(29) H(48) 109.5(5) 1_555 1_555 1_555 no O(7) C(30) C(29) 113.2(4) 1_555 1_555 1_555 yes O(7) C(30) C(31) 109.4(4) 1_555 1_555 1_555 yes O(7) C(30) H(49) 108.0(4) 1_555 1_555 1_555 no C(29) C(30) C(31) 111.6(4) 1_555 1_555 1_555 yes C(29) C(30) H(49) 107.8(4) 1_555 1_555 1_555 no C(31) C(30) H(49) 106.5(5) 1_555 1_555 1_555 no C(30) C(31) C(32) 111.4(4) 1_555 1_555 1_555 yes C(30) C(31) C(37) 113.3(3) 1_555 1_555 1_555 yes C(30) C(31) H(50) 108.1(4) 1_555 1_555 1_555 no C(32) C(31) C(37) 109.1(3) 1_555 1_555 1_555 yes C(32) C(31) H(50) 107.7(3) 1_555 1_555 1_555 no C(37) C(31) H(50) 107.0(4) 1_555 1_555 1_555 no C(31) C(32) C(33) 110.7(3) 1_555 1_555 1_555 yes C(31) C(32) C(34) 112.9(3) 1_555 1_555 1_555 yes C(31) C(32) H(51) 107.0(3) 1_555 1_555 1_555 no C(33) C(32) C(34) 112.9(3) 1_555 1_555 1_555 yes C(33) C(32) H(51) 106.6(4) 1_555 1_555 1_555 no C(34) C(32) H(51) 106.3(3) 1_555 1_555 1_555 no C(24) C(33) C(28) 108.5(3) 1_555 1_555 1_555 yes C(24) C(33) C(32) 114.3(3) 1_555 1_555 1_555 yes C(24) C(33) C(42) 104.1(3) 1_555 1_555 1_555 yes C(28) C(33) C(32) 109.5(3) 1_555 1_555 1_555 yes C(28) C(33) C(42) 109.6(4) 1_555 1_555 1_555 yes C(32) C(33) C(42) 110.7(3) 1_555 1_555 1_555 yes C(32) C(34) C(35) 115.8(3) 1_555 1_555 1_555 yes C(32) C(34) H(52) 108.2(4) 1_555 1_555 1_555 no C(32) C(34) H(53) 107.7(4) 1_555 1_555 1_555 no C(35) C(34) H(52) 107.5(4) 1_555 1_555 1_555 no C(35) C(34) H(53) 107.6(4) 1_555 1_555 1_555 no H(52) C(34) H(53) 109.9(4) 1_555 1_555 1_555 no O(8) C(35) C(34) 110.3(3) 1_555 1_555 1_555 yes O(8) C(35) C(36) 110.2(3) 1_555 1_555 1_555 yes O(8) C(35) H(54) 108.2(4) 1_555 1_555 1_555 no C(34) C(35) C(36) 111.5(3) 1_555 1_555 1_555 yes C(34) C(35) H(54) 108.1(4) 1_555 1_555 1_555 no C(36) C(35) H(54) 108.5(4) 1_555 1_555 1_555 no C(35) C(36) C(37) 107.5(3) 1_555 1_555 1_555 yes C(35) C(36) C(40) 117.7(3) 1_555 1_555 1_555 yes C(35) C(36) C(41) 108.7(3) 1_555 1_555 1_555 yes C(37) C(36) C(40) 100.9(3) 1_555 1_555 1_555 yes C(37) C(36) C(41) 112.7(3) 1_555 1_555 1_555 yes C(40) C(36) C(41) 109.3(3) 1_555 1_555 1_555 yes C(31) C(37) C(36) 112.8(3) 1_555 1_555 1_555 yes C(31) C(37) C(38) 117.1(3) 1_555 1_555 1_555 yes C(31) C(37) H(55) 107.9(4) 1_555 1_555 1_555 no C(36) C(37) C(38) 104.9(3) 1_555 1_555 1_555 yes C(36) C(37) H(55) 106.7(3) 1_555 1_555 1_555 no C(38) C(37) H(55) 106.9(3) 1_555 1_555 1_555 no C(37) C(38) C(39) 104.5(3) 1_555 1_555 1_555 yes C(37) C(38) H(56) 110.0(4) 1_555 1_555 1_555 no C(37) C(38) H(57) 110.5(4) 1_555 1_555 1_555 no C(39) C(38) H(56) 110.6(4) 1_555 1_555 1_555 no C(39) C(38) H(57) 111.2(4) 1_555 1_555 1_555 no H(56) C(38) H(57) 110.0(4) 1_555 1_555 1_555 no C(38) C(39) C(40) 107.5(3) 1_555 1_555 1_555 yes C(38) C(39) H(58) 109.3(4) 1_555 1_555 1_555 no C(38) C(39) H(59) 109.9(4) 1_555 1_555 1_555 no C(40) C(39) H(58) 110.1(4) 1_555 1_555 1_555 no C(40) C(39) H(59) 110.5(4) 1_555 1_555 1_555 no H(58) C(39) H(59) 109.5(4) 1_555 1_555 1_555 no C(36) C(40) C(39) 102.6(3) 1_555 1_555 1_555 yes C(36) C(40) C(43) 117.8(3) 1_555 1_555 1_555 yes C(36) C(40) H(60) 106.8(4) 1_555 1_555 1_555 no C(39) C(40) C(43) 114.5(4) 1_555 1_555 1_555 yes C(39) C(40) H(60) 107.5(4) 1_555 1_555 1_555 no C(43) C(40) H(60) 107.1(4) 1_555 1_555 1_555 no C(36) C(41) H(61) 108.9(4) 1_555 1_555 1_555 no C(36) C(41) H(62) 109.6(4) 1_555 1_555 1_555 no C(36) C(41) H(63) 110.2(4) 1_555 1_555 1_555 no H(61) C(41) H(62) 109.0(5) 1_555 1_555 1_555 no H(61) C(41) H(63) 109.2(5) 1_555 1_555 1_555 no H(62) C(41) H(63) 109.8(5) 1_555 1_555 1_555 no C(33) C(42) H(64) 109.6(4) 1_555 1_555 1_555 no C(33) C(42) H(65) 109.4(5) 1_555 1_555 1_555 no C(33) C(42) H(66) 108.9(5) 1_555 1_555 1_555 no H(64) C(42) H(65) 109.9(5) 1_555 1_555 1_555 no H(64) C(42) H(66) 109.8(5) 1_555 1_555 1_555 no H(65) C(42) H(66) 109.2(5) 1_555 1_555 1_555 no C(40) C(43) C(44) 113.9(4) 1_555 1_555 1_555 yes C(40) C(43) C(45) 110.7(4) 1_555 1_555 1_555 yes C(40) C(43) H(67) 107.7(4) 1_555 1_555 1_555 no C(44) C(43) C(45) 109.4(4) 1_555 1_555 1_555 yes C(44) C(43) H(67) 107.1(5) 1_555 1_555 1_555 no C(45) C(43) H(67) 107.8(5) 1_555 1_555 1_555 no C(43) C(44) H(68) 109.8(5) 1_555 1_555 1_555 no C(43) C(44) H(69) 110.5(5) 1_555 1_555 1_555 no C(43) C(44) H(70) 109.6(5) 1_555 1_555 1_555 no H(68) C(44) H(69) 109.6(5) 1_555 1_555 1_555 no H(68) C(44) H(70) 108.2(6) 1_555 1_555 1_555 no H(69) C(44) H(70) 109.0(6) 1_555 1_555 1_555 no C(43) C(45) C(46) 112.3(4) 1_555 1_555 1_555 yes C(43) C(45) H(71) 108.4(5) 1_555 1_555 1_555 no C(43) C(45) H(72) 108.6(5) 1_555 1_555 1_555 no C(46) C(45) H(71) 108.6(5) 1_555 1_555 1_555 no C(46) C(45) H(72) 109.1(6) 1_555 1_555 1_555 no H(71) C(45) H(72) 109.8(5) 1_555 1_555 1_555 no O(9) C(46) O(10) 122.6(5) 1_555 1_555 1_555 yes O(9) C(46) C(45) 122.4(5) 1_555 1_555 1_555 yes O(10) C(46) C(45) 115.0(5) 1_555 1_555 1_555 yes C(48) C(47) H(77) 106(1) 1_555 1_555 1_555 no C(48) C(47) H(78) 107(1) 1_555 1_555 1_555 no C(48) C(47) H(79) 118(1) 1_555 1_555 1_555 no H(77) C(47) H(78) 99(1) 1_555 1_555 1_555 no H(77) C(47) H(79) 110(1) 1_555 1_555 1_555 no H(78) C(47) H(79) 111(1) 1_555 1_555 1_555 no O(11) C(48) C(47) 121(1) 1_555 1_555 1_555 yes O(11) C(48) C(49) 140(1) 1_555 1_555 1_555 yes C(47) C(48) C(49) 97(1) 1_555 1_555 1_555 yes C(48) C(49) H(80) 108(1) 1_555 1_555 1_555 no C(48) C(49) H(81) 112(1) 1_555 1_555 1_555 no C(48) C(49) H(82) 116(2) 1_555 1_555 1_555 no H(80) C(49) H(81) 100(2) 1_555 1_555 1_555 no H(80) C(49) H(82) 105(1) 1_555 1_555 1_555 no H(81) C(49) H(82) 111(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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) 177.6(4) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) -179.5(4) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -70.8(7) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 72.3(5) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(14) -50.9(5) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(11) C(9) 72.4(4) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(14) -66.0(4) 1_555 1_555 1_555 1_555 yes O(3) C(12) C(13) C(17) 47.5(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(23) C(22) C(20) -128.7(7) 1_555 1_555 1_555 1_555 yes O(5) C(23) C(22) C(20) 52.1(7) 1_555 1_555 1_555 1_555 yes O(6) C(26) C(25) C(24) 178.9(4) 1_555 1_555 1_555 1_555 yes O(6) C(26) C(27) C(28) 179.6(4) 1_555 1_555 1_555 1_555 yes O(7) C(30) C(29) C(28) -74.3(6) 1_555 1_555 1_555 1_555 yes O(7) C(30) C(31) C(32) 73.0(4) 1_555 1_555 1_555 1_555 yes O(7) C(30) C(31) C(37) -50.4(5) 1_555 1_555 1_555 1_555 yes O(8) C(35) C(34) C(32) 73.5(4) 1_555 1_555 1_555 1_555 yes O(8) C(35) C(36) C(37) -67.2(4) 1_555 1_555 1_555 1_555 yes O(8) C(35) C(36) C(40) 45.7(4) 1_555 1_555 1_555 1_555 yes O(8) C(35) C(36) C(41) 170.5(3) 1_555 1_555 1_555 1_555 yes O(9) C(46) C(45) C(43) -129.6(7) 1_555 1_555 1_555 1_555 yes O(10) C(46) C(45) C(43) 50.1(8) 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) 47.3(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 176.8(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -177.1(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 56.8(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -51.3(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 66.5(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -170.7(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 56.8(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 57.5(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 178.5(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -52.9(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 74.5(7) 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) 164.4(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 53.0(7) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -59.0(4) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 174.9(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 56.4(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -66.1(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -54.5(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -177.7(4) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -55.0(7) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 59.3(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -174.4(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) -54.6(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 62.9(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 47.7(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -62.1(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 173.6(3) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 57.7(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -159.5(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 59.3(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -178.6(4) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -51.2(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -175.7(4) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 173.5(3) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -49.4(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -63.3(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 55.7(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 169.3(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -67.1(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 169.2(3) 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) 78.6(5) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -32.8(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 19.2(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -61.5(5) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 177.5(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -38.7(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -164.4(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 7.8(5) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 44.8(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -71.0(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 148.0(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 80.7(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 177.9(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 56.9(5) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -172.2(4) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -45.0(5) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 64.0(6) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) -56.2(5) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(27) 51.4(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(29) 178.1(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(31) -178.8(3) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(34) 53.6(4) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(28) -54.7(5) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(32) 67.8(5) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(42) -171.4(4) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 55.5(5) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(24) C(33) 58.3(5) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 178.5(4) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(33) -53.9(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 77.0(6) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(32) -74.0(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(42) 164.4(4) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 49.7(6) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(31) -56.8(4) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(34) 175.6(4) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(32) 52.7(5) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(42) -68.9(5) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -53.1(5) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(37) -176.5(4) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(28) C(33) -50.3(6) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) 57.9(4) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(34) -174.4(3) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(36) -175.6(4) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(38) -53.7(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(42) 64.1(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(34) C(35) 45.3(5) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(35) -63.6(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(40) 172.6(3) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(41) 56.1(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(38) C(39) -156.0(4) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(36) 59.8(4) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(38) -178.4(3) 1_555 1_555 1_555 1_555 yes C(32) C(34) C(35) C(36) -49.3(5) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(37) -176.3(3) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(34) C(35) 171.8(4) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(31) C(37) -48.7(4) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(33) C(42) -63.5(5) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) 55.6(4) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(40) 168.5(3) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(41) -66.6(4) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 167.8(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(39) -156.5(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(43) 76.8(5) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) -30.2(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(39) C(38) 22.5(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(44) -62.4(5) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(45) 173.7(4) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(39) -40.0(4) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(43) -166.7(4) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) 4.3(5) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(40) 44.0(4) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(41) -72.4(4) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(43) 151.3(4) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(36) C(41) 79.0(4) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(44) 176.9(4) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(45) 53.0(5) 1_555 1_555 1_555 1_555 yes C(40) C(43) C(45) C(46) -167.5(5) 1_555 1_555 1_555 1_555 yes C(41) C(36) C(40) C(43) -47.7(5) 1_555 1_555 1_555 1_555 yes C(44) C(43) C(45) C(46) 66.2(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(5) 2.620(6) 1_555 1_565 ? O(1) O(9) 2.738(6) 1_555 1_555 ? O(1) O(4) 3.298(7) 1_555 1_565 ? O(1) C(23) 3.365(7) 1_555 1_565 ? O(2) C(45) 3.473(7) 1_555 1_555 ? O(3) O(8) 3.270(4) 1_555 1_555 ? O(3) C(40) 3.568(5) 1_555 1_555 ? O(3) C(44) 3.569(6) 1_555 1_555 ? O(4) O(6) 2.789(6) 1_555 1_555 ? O(4) O(12) 3.42(3) 1_555 1_555 ? O(4) C(49) 3.47(2) 1_555 1_545 ? O(4) C(26) 3.483(8) 1_555 1_555 ? O(6) O(10) 2.595(5) 1_555 1_545 ? O(6) O(9) 3.164(6) 1_555 1_545 ? O(6) C(46) 3.273(6) 1_555 1_545 ? O(7) O(12) 2.83(3) 1_555 1_554 ? O(7) O(11) 2.93(1) 1_555 1_544 ? O(7) C(22) 3.348(7) 1_555 1_555 ? O(8) O(12) 2.88(3) 1_555 1_555 ? O(9) C(3) 3.514(7) 1_555 1_555 ? O(11) C(27) 3.30(1) 1_555 1_566 ? O(11) C(25) 3.32(1) 1_555 1_565 ? O(11) O(12) 3.49(3) 1_555 1_565 ? O(12) C(21) 3.32(3) 1_555 1_555 ? O(12) C(25) 3.36(3) 1_555 1_555 ? O(12) C(16) 3.39(3) 1_555 1_556 ? O(12) C(34) 3.39(3) 1_555 1_555 ? #------------------------------------------------------------------------------ _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 565-8710 Japan ; _publ_contact_author_email ' miyata@ap.chem.eng.osaka-u.ac.jp ' _publ_contact_author_fax ' +81-6-879-7404 ' _publ_contact_author_phone ' +81-6-879-7406 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chem.Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; A Robust Structural Motif in Inclusion Crystals of Norbile Acids ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Michihiro Sugahara ' ? ; Material and Life Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-8710 Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_Nord #------------------------------------------------------------------------------ _audit_creation_date 'Sat Dec 26 17:27:16 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 815.18 _chemical_formula_analytical ? _chemical_formula_sum 'C49 H82 O9 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.5710(9) _cell_length_b 15.269(2) _cell_length_c 7.583(3) _cell_angle_alpha 92.47(2) _cell_angle_beta 104.61(2) _cell_angle_gamma 80.221(9) _cell_volume 1167.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 209.4 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448.00 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 209.4 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_detector_area_resol_mean 0.010000 _diffrn_mesured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_reflns_number 3696 _reflns_number_total 3696 _reflns_number_gt 3561 _reflns_observed_expression >1.5sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.035 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O -0.8681(4) -0.8399(2) -0.4841(7) 0.089(1) Uani 1.00 d . . . O(2) O -0.9762(3) -0.4089(2) -0.4336(4) 0.0496(6) Uani 1.00 d . . . O(3) O -1.0913(4) 0.0373(2) -0.6185(8) 0.099(1) Uani 1.00 d . . . O(4) O -0.8768(3) -0.0029(2) -0.5892(7) 0.082(1) Uani 1.00 d . . . O(5) O -0.3164(3) 0.1577(2) -0.7579(6) 0.0722(9) Uani 1.00 d . . . O(6) O -0.2491(3) -0.2586(2) -0.6168(3) 0.0458(6) Uani 1.00 d . . . O(7) O -0.0889(4) -0.7128(2) -0.6307(6) 0.085(1) Uani 1.00 d . . . O(8) O -0.2724(3) -0.6898(2) -0.8575(6) 0.0732(9) Uani 1.00 d . . . O(9) O 0.0157(9) -0.7385(8) -0.041(2) 0.222(4) Uani 1.00 d . . . C(1) C -0.6395(4) -0.6804(2) -0.2536(5) 0.0468(8) Uani 1.00 d . . . C(2) C -0.7604(4) -0.7268(3) -0.2918(6) 0.0550(9) Uani 1.00 d . . . C(3) C -0.7560(5) -0.7949(2) -0.4433(6) 0.0610(10) Uani 1.00 d . . . C(4) C -0.7418(5) -0.7508(3) -0.6124(6) 0.0602(10) Uani 1.00 d . . . C(5) C -0.6227(4) -0.7013(3) -0.5745(5) 0.0560(9) Uani 1.00 d . . . C(6) C -0.6112(6) -0.6578(3) -0.7511(6) 0.074(1) Uani 1.00 d . . . C(7) C -0.7222(5) -0.5772(3) -0.8098(5) 0.065(1) Uani 1.00 d . . . C(8) C -0.7162(3) -0.5090(3) -0.6545(5) 0.0445(8) Uani 1.00 d . . . C(9) C -0.7323(3) -0.5518(2) -0.4840(4) 0.0379(7) Uani 1.00 d . . . C(10) C -0.6217(4) -0.6329(2) -0.4161(5) 0.0433(8) Uani 1.00 d . . . C(11) C -0.7471(4) -0.4833(2) -0.3309(5) 0.0417(8) Uani 1.00 d . . . C(12) C -0.8411(4) -0.3942(2) -0.3898(4) 0.0391(7) Uani 1.00 d . . . C(13) C -0.8120(3) -0.3541(2) -0.5556(4) 0.0364(7) Uani 1.00 d . . . C(14) C -0.8203(3) -0.4260(2) -0.7088(4) 0.0407(7) Uani 1.00 d . . . C(15) C -0.8214(4) -0.3746(3) -0.8792(5) 0.0490(8) Uani 1.00 d . . . C(16) C -0.8885(4) -0.2791(3) -0.8493(5) 0.0482(8) Uani 1.00 d . . . C(17) C -0.9150(3) -0.2751(2) -0.6572(5) 0.0412(7) Uani 1.00 d . . . C(18) C -0.6745(4) -0.3259(3) -0.4967(6) 0.0522(9) Uani 1.00 d . . . C(19) C -0.4839(4) -0.6046(3) -0.3527(7) 0.059(1) Uani 1.00 d . . . C(20) C -0.9151(4) -0.1830(2) -0.5663(6) 0.0499(8) Uani 1.00 d . . . C(21) C -0.9519(5) -0.1766(3) -0.3852(6) 0.062(1) Uani 1.00 d . . . C(22) C -1.0115(4) -0.1120(3) -0.6966(7) 0.061(1) Uani 1.00 d . . . C(23) C -1.0004(5) -0.0183(3) -0.6309(7) 0.0614(10) Uani 1.00 d . . . C(24) C -0.5717(4) 0.0061(3) -0.8165(6) 0.0485(9) Uani 1.00 d . . . C(25) C -0.4560(4) 0.0524(2) -0.7177(5) 0.0455(8) Uani 1.00 d . . . C(26) C -0.4208(4) 0.1112(2) -0.8487(6) 0.0514(9) Uani 1.00 d . . . C(27) C -0.3890(5) 0.0546(3) -1.0064(6) 0.0566(9) Uani 1.00 d . . . C(28) C -0.5009(5) 0.0051(3) -1.1073(6) 0.0577(10) Uani 1.00 d . . . C(29) C -0.4634(7) -0.0496(3) -1.2689(6) 0.079(1) Uani 1.00 d . . . C(30) C -0.3608(6) -0.1317(3) -1.2066(5) 0.066(1) Uani 1.00 d . . . C(31) C -0.4070(4) -0.1894(2) -1.0853(5) 0.0472(8) Uani 1.00 d . . . C(32) C -0.4375(3) -0.1365(2) -0.9178(5) 0.0389(7) Uani 1.00 d . . . C(33) C -0.5445(4) -0.0516(3) -0.9784(6) 0.0498(8) Uani 1.00 d . . . C(34) C -0.4694(3) -0.1940(2) -0.7789(5) 0.0435(8) Uani 1.00 d . . . C(35) C -0.3712(3) -0.2810(2) -0.7297(5) 0.0384(7) Uani 1.00 d . . . C(36) C -0.3502(3) -0.3343(2) -0.9002(4) 0.0367(7) Uani 1.00 d . . . C(37) C -0.3042(3) -0.2725(2) -1.0174(4) 0.0381(7) Uani 1.00 d . . . C(38) C -0.2591(4) -0.3350(3) -1.1632(5) 0.0530(9) Uani 1.00 d . . . C(39) C -0.2035(4) -0.4255(3) -1.0648(5) 0.0466(8) Uani 1.00 d . . . C(40) C -0.2347(3) -0.4162(2) -0.8717(5) 0.0399(7) Uani 1.00 d . . . C(41) C -0.4803(4) -0.3661(3) -0.9981(6) 0.0532(9) Uani 1.00 d . . . C(42) C -0.6818(4) -0.0795(3) -1.0743(9) 0.075(1) Uani 1.00 d . . . C(43) C -0.2582(3) -0.5025(2) -0.8043(6) 0.0462(8) Uani 1.00 d . . . C(44) C -0.2829(4) -0.4954(3) -0.6111(6) 0.060(1) Uani 1.00 d . . . C(45) C -0.1370(4) -0.5774(2) -0.7984(6) 0.0514(9) Uani 1.00 d . . . C(46) C -0.1625(4) -0.6669(2) -0.7521(7) 0.0548(9) Uani 1.00 d . . . C(47) C -0.012(2) -0.903(1) -0.065(2) 0.333(6) Uani 1.00 d . . . C(48) C -0.0494(8) -0.801(1) -0.114(1) 0.180(3) Uani 1.00 d . . . C(49) C -0.1733(9) -0.803(1) -0.269(2) 0.223(5) Uani 1.00 d . . . H(1) H -0.5634 -0.7236 -0.2124 0.0554 Uiso 1.00 calc . . . H(2) H -0.6481 -0.6374 -0.1622 0.0554 Uiso 1.00 calc . . . H(3) H -0.8389 -0.6848 -0.3247 0.0623 Uiso 1.00 calc . . . H(4) H -0.7600 -0.7575 -0.1838 0.0623 Uiso 1.00 calc . . . H(5) H -0.6798 -0.8382 -0.4052 0.0742 Uiso 1.00 calc . . . H(6) H -0.7335 -0.7961 -0.7018 0.0703 Uiso 1.00 calc . . . H(7) H -0.8222 -0.7102 -0.6589 0.0703 Uiso 1.00 calc . . . H(8) H -0.5469 -0.7457 -0.5357 0.0641 Uiso 1.00 calc . . . H(9) H -0.6111 -0.6983 -0.8472 0.0818 Uiso 1.00 calc . . . H(10) H -0.5261 -0.6350 -0.7243 0.0818 Uiso 1.00 calc . . . H(11) H -0.7129 -0.5510 -0.9161 0.0753 Uiso 1.00 calc . . . H(12) H -0.8043 -0.5987 -0.8361 0.0753 Uiso 1.00 calc . . . H(13) H -0.6323 -0.4904 -0.6257 0.0491 Uiso 1.00 calc . . . H(14) H -0.8136 -0.5753 -0.5200 0.0404 Uiso 1.00 calc . . . H(15) H -0.7788 -0.5102 -0.2426 0.0479 Uiso 1.00 calc . . . H(16) H -0.6616 -0.4694 -0.2742 0.0479 Uiso 1.00 calc . . . H(17) H -0.8294 -0.3536 -0.2910 0.0445 Uiso 1.00 calc . . . H(18) H -0.9059 -0.4432 -0.7280 0.0460 Uiso 1.00 calc . . . H(19) H -0.8695 -0.4009 -0.9883 0.0558 Uiso 1.00 calc . . . H(20) H -0.7326 -0.3760 -0.8913 0.0558 Uiso 1.00 calc . . . H(21) H -0.8327 -0.2380 -0.8613 0.0537 Uiso 1.00 calc . . . H(22) H -0.9706 -0.2654 -0.9409 0.0537 Uiso 1.00 calc . . . H(23) H -0.9989 -0.2903 -0.6687 0.0461 Uiso 1.00 calc . . . H(24) H -0.6756 -0.2757 -0.4190 0.0670 Uiso 1.00 calc . . . H(25) H -0.6482 -0.3104 -0.6033 0.0670 Uiso 1.00 calc . . . H(26) H -0.6105 -0.3736 -0.4366 0.0670 Uiso 1.00 calc . . . H(27) H -0.4836 -0.5657 -0.2491 0.0705 Uiso 1.00 calc . . . H(28) H -0.4671 -0.5740 -0.4470 0.0705 Uiso 1.00 calc . . . H(29) H -0.4180 -0.6552 -0.3168 0.0705 Uiso 1.00 calc . . . H(30) H -0.8270 -0.1689 -0.5464 0.0567 Uiso 1.00 calc . . . H(31) H -0.8926 -0.2208 -0.3051 0.0747 Uiso 1.00 calc . . . H(32) H -1.0393 -0.1874 -0.4041 0.0747 Uiso 1.00 calc . . . H(33) H -0.9435 -0.1198 -0.3348 0.0747 Uiso 1.00 calc . . . H(34) H -1.0984 -0.1209 -0.7067 0.0748 Uiso 1.00 calc . . . H(35) H -0.9917 -0.1187 -0.8136 0.0748 Uiso 1.00 calc . . . H(36) H -0.9470 -0.7895 -0.4926 0.1064 Uiso 1.00 calc . . . H(37) H -0.9839 -0.4627 -0.5136 0.0596 Uiso 1.00 calc . . . H(38) H -0.8856 0.0596 -0.5450 0.0977 Uiso 1.00 calc . . . H(39) H -0.5894 -0.0290 -0.7307 0.0535 Uiso 1.00 calc . . . H(40) H -0.6455 0.0518 -0.8607 0.0535 Uiso 1.00 calc . . . H(41) H -0.4804 0.0888 -0.6222 0.0525 Uiso 1.00 calc . . . H(42) H -0.3811 0.0097 -0.6690 0.0525 Uiso 1.00 calc . . . H(43) H -0.4960 0.1552 -0.8965 0.0587 Uiso 1.00 calc . . . H(44) H -0.3680 0.0918 -1.0892 0.0650 Uiso 1.00 calc . . . H(45) H -0.3102 0.0120 -0.9571 0.0650 Uiso 1.00 calc . . . H(46) H -0.5753 0.0485 -1.1587 0.0663 Uiso 1.00 calc . . . H(47) H -0.5388 -0.0715 -1.3436 0.0922 Uiso 1.00 calc . . . H(48) H -0.4289 -0.0153 -1.3398 0.0922 Uiso 1.00 calc . . . H(49) H -0.2805 -0.1112 -1.1390 0.0805 Uiso 1.00 calc . . . H(50) H -0.3429 -0.1638 -1.3093 0.0805 Uiso 1.00 calc . . . H(51) H -0.4867 -0.2067 -1.1552 0.0549 Uiso 1.00 calc . . . H(52) H -0.3573 -0.1152 -0.8587 0.0437 Uiso 1.00 calc . . . H(53) H -0.4680 -0.1605 -0.6681 0.0520 Uiso 1.00 calc . . . H(54) H -0.5562 -0.2079 -0.8251 0.0520 Uiso 1.00 calc . . . H(55) H -0.4052 -0.3172 -0.6610 0.0459 Uiso 1.00 calc . . . H(56) H -0.2269 -0.2530 -0.9433 0.0450 Uiso 1.00 calc . . . H(57) H -0.1913 -0.3132 -1.2024 0.0594 Uiso 1.00 calc . . . H(58) H -0.3315 -0.3392 -1.2641 0.0594 Uiso 1.00 calc . . . H(59) H -0.1119 -0.4410 -1.0556 0.0544 Uiso 1.00 calc . . . H(60) H -0.2484 -0.4707 -1.1340 0.0544 Uiso 1.00 calc . . . H(61) H -0.1585 -0.3978 -0.7892 0.0431 Uiso 1.00 calc . . . H(62) H -0.4667 -0.4002 -1.1041 0.0652 Uiso 1.00 calc . . . H(63) H -0.5049 -0.4035 -0.9202 0.0652 Uiso 1.00 calc . . . H(64) H -0.5474 -0.3171 -1.0354 0.0652 Uiso 1.00 calc . . . H(65) H -0.6746 -0.1157 -1.1774 0.1046 Uiso 1.00 calc . . . H(66) H -0.7110 -0.1111 -0.9910 0.1046 Uiso 1.00 calc . . . H(67) H -0.7459 -0.0272 -1.1135 0.1046 Uiso 1.00 calc . . . H(68) H -0.3337 -0.5208 -0.8866 0.0516 Uiso 1.00 calc . . . H(69) H -0.2996 -0.5498 -0.5763 0.0711 Uiso 1.00 calc . . . H(70) H -0.3569 -0.4498 -0.6106 0.0711 Uiso 1.00 calc . . . H(71) H -0.2065 -0.4793 -0.5269 0.0711 Uiso 1.00 calc . . . H(72) H -0.0620 -0.5622 -0.7058 0.0617 Uiso 1.00 calc . . . H(73) H -0.1138 -0.5800 -0.9123 0.0617 Uiso 1.00 calc . . . H(74) H -0.2241 0.1169 -0.7221 0.0866 Uiso 1.00 calc . . . H(75) H -0.1893 -0.3110 -0.5923 0.0550 Uiso 1.00 calc . . . H(76) H -0.2861 -0.7468 -0.7908 0.0880 Uiso 1.00 calc . . . H(77) H 0.0664 -0.9031 0.0405 0.3997 Uiso 1.00 calc . . . H(78) H 0.0087 -0.9309 -0.1589 0.3997 Uiso 1.00 calc . . . H(79) H -0.0805 -0.9163 -0.0227 0.3997 Uiso 1.00 calc . . . H(80) H -0.1495 -0.8385 -0.3665 0.2660 Uiso 1.00 calc . . . H(81) H -0.2388 -0.8247 -0.2304 0.2660 Uiso 1.00 calc . . . H(82) H -0.2039 -0.7431 -0.3119 0.2660 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) 0.092(2) 0.034(1) 0.121(3) -0.023(1) -0.023(2) 0.012(2) O(2) 0.052(1) 0.053(1) 0.050(1) -0.007(1) 0.0225(10) 0.001(1) O(3) 0.077(2) 0.041(2) 0.156(4) 0.010(1) 0.000(2) -0.005(2) O(4) 0.068(2) 0.040(1) 0.128(3) -0.014(1) 0.004(2) -0.005(2) O(5) 0.075(2) 0.034(1) 0.100(3) -0.013(1) 0.005(2) 0.001(1) O(6) 0.048(1) 0.051(1) 0.034(1) -0.011(1) -0.0002(9) -0.0026(10) O(7) 0.077(2) 0.065(2) 0.100(3) 0.006(2) 0.004(2) 0.034(2) O(8) 0.077(2) 0.046(1) 0.091(2) -0.029(1) -0.004(2) 0.010(2) O(9) 0.206(7) 0.284(10) 0.214(10) -0.134(6) 0.072(6) -0.066(8) C(1) 0.061(2) 0.037(2) 0.038(2) -0.007(1) 0.005(1) 0.004(1) C(2) 0.071(2) 0.037(2) 0.057(2) -0.021(1) 0.004(2) 0.010(1) C(3) 0.081(2) 0.027(1) 0.063(2) -0.010(2) -0.006(2) 0.009(1) C(4) 0.081(2) 0.036(2) 0.044(2) 0.008(2) -0.007(2) -0.006(1) C(5) 0.068(2) 0.046(2) 0.041(2) 0.023(1) 0.011(2) 0.002(1) C(6) 0.110(3) 0.063(2) 0.039(2) 0.036(2) 0.032(2) 0.007(2) C(7) 0.097(3) 0.056(2) 0.033(2) 0.022(2) 0.021(2) 0.003(1) C(8) 0.046(2) 0.051(2) 0.033(1) 0.008(1) 0.014(1) 0.007(1) C(9) 0.045(1) 0.037(1) 0.029(1) -0.004(1) 0.006(1) 0.001(1) C(10) 0.047(1) 0.045(2) 0.034(1) 0.004(1) 0.009(1) 0.007(1) C(11) 0.057(2) 0.035(1) 0.029(1) -0.005(1) 0.004(1) 0.001(1) C(12) 0.053(1) 0.036(1) 0.027(1) -0.003(1) 0.011(1) -0.006(1) C(13) 0.037(1) 0.037(1) 0.033(1) -0.002(1) 0.006(1) 0.001(1) C(14) 0.045(2) 0.044(2) 0.029(1) 0.002(1) 0.008(1) 0.000(1) C(15) 0.055(2) 0.048(2) 0.044(2) 0.001(1) 0.016(1) 0.015(1) C(16) 0.052(2) 0.044(2) 0.047(2) -0.005(1) 0.009(1) 0.013(1) C(17) 0.037(1) 0.039(1) 0.042(2) -0.004(1) -0.001(1) 0.004(1) C(18) 0.037(1) 0.048(2) 0.065(2) -0.011(1) -0.004(2) 0.010(2) C(19) 0.050(2) 0.053(2) 0.069(2) -0.001(2) 0.007(2) 0.010(2) C(20) 0.046(2) 0.034(1) 0.062(2) -0.009(1) -0.004(1) 0.004(1) C(21) 0.073(2) 0.045(2) 0.059(2) -0.011(2) 0.002(2) -0.011(2) C(22) 0.055(2) 0.040(2) 0.074(3) -0.006(2) -0.010(2) 0.007(2) C(23) 0.063(2) 0.043(2) 0.068(3) -0.007(1) -0.003(2) 0.002(2) C(24) 0.046(2) 0.041(2) 0.055(2) -0.001(1) 0.009(1) 0.002(1) C(25) 0.057(2) 0.031(1) 0.047(2) -0.005(1) 0.010(1) -0.005(1) C(26) 0.060(2) 0.032(2) 0.061(2) -0.004(1) 0.014(1) 0.008(1) C(27) 0.079(2) 0.034(2) 0.060(2) -0.002(2) 0.026(2) 0.014(1) C(28) 0.074(2) 0.042(2) 0.045(2) 0.009(2) 0.003(2) 0.011(1) C(29) 0.132(4) 0.056(2) 0.039(2) 0.014(2) 0.020(2) 0.008(2) C(30) 0.118(3) 0.044(2) 0.036(2) -0.006(2) 0.023(2) 0.007(1) C(31) 0.064(2) 0.036(1) 0.033(2) -0.004(1) 0.001(1) -0.005(1) C(32) 0.042(1) 0.037(1) 0.033(1) -0.003(1) 0.003(1) 0.001(1) C(33) 0.048(2) 0.041(2) 0.049(2) 0.003(1) -0.003(1) 0.000(1) C(34) 0.049(2) 0.040(2) 0.044(2) -0.002(1) 0.019(1) 0.001(1) C(35) 0.042(1) 0.037(1) 0.039(1) -0.011(1) 0.013(1) 0.000(1) C(36) 0.035(1) 0.036(1) 0.038(1) -0.005(1) 0.006(1) 0.001(1) C(37) 0.050(1) 0.034(1) 0.031(1) -0.013(1) 0.006(1) 0.001(1) C(38) 0.073(2) 0.043(2) 0.039(2) 0.001(2) 0.014(2) -0.003(1) C(39) 0.054(2) 0.041(2) 0.047(2) -0.009(1) 0.017(1) -0.005(1) C(40) 0.035(1) 0.038(1) 0.043(2) -0.005(1) 0.003(1) 0.000(1) C(41) 0.039(2) 0.043(2) 0.070(2) -0.013(1) -0.002(2) -0.010(2) C(42) 0.048(2) 0.053(2) 0.103(4) -0.005(2) -0.018(2) 0.001(3) C(43) 0.039(1) 0.036(1) 0.062(2) -0.010(1) 0.006(1) 0.003(1) C(44) 0.069(2) 0.051(2) 0.070(2) -0.008(2) 0.033(2) 0.007(2) C(45) 0.050(2) 0.033(1) 0.072(2) -0.004(1) 0.017(2) 0.002(2) C(46) 0.060(2) 0.034(2) 0.075(2) -0.009(1) 0.024(1) 0.002(1) C(47) 0.29(1) 0.38(1) 0.29(1) 0.251(9) 0.173(9) 0.238(9) C(48) 0.113(4) 0.296(8) 0.160(5) -0.056(5) 0.087(3) -0.113(6) C(49) 0.101(5) 0.40(2) 0.140(7) 0.072(7) 0.035(4) 0.129(8) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F^2^ against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^, conventional R-factors (R) are calculated on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 1.5sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.04000(Fo^2^)^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3619 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.2195 _refine_ls_wR_factor_gt 0.2183 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_shift/su_max 0.2760 _refine_ls_shift/su_mean 0.0220 _refine_diff_density_min -0.34 _refine_diff_density_max 0.70 #------------------------------------------------------------------------------ _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) 1.430(6) 1_555 1_555 yes O(2) C(12) 1.437(4) 1_555 1_555 yes O(3) C(23) 1.189(6) 1_555 1_555 yes O(4) C(23) 1.324(6) 1_555 1_555 yes O(5) C(26) 1.428(5) 1_555 1_555 yes O(6) C(35) 1.443(4) 1_555 1_555 yes O(7) C(46) 1.205(6) 1_555 1_555 yes O(8) C(46) 1.325(5) 1_555 1_555 yes O(9) C(48) 1.30(2) 1_555 1_555 yes C(1) C(2) 1.524(6) 1_555 1_555 yes C(1) C(10) 1.523(5) 1_555 1_555 yes C(2) C(3) 1.520(6) 1_555 1_555 yes C(3) C(4) 1.525(7) 1_555 1_555 yes C(4) C(5) 1.537(7) 1_555 1_555 yes C(5) C(6) 1.560(6) 1_555 1_555 yes C(5) C(10) 1.556(5) 1_555 1_555 yes C(6) C(7) 1.543(6) 1_555 1_555 yes C(7) C(8) 1.535(6) 1_555 1_555 yes C(8) C(9) 1.533(5) 1_555 1_555 yes C(8) C(14) 1.525(5) 1_555 1_555 yes C(9) C(10) 1.557(4) 1_555 1_555 yes C(9) C(11) 1.549(5) 1_555 1_555 yes C(10) C(19) 1.544(6) 1_555 1_555 yes C(11) C(12) 1.552(5) 1_555 1_555 yes C(12) C(13) 1.541(4) 1_555 1_555 yes C(13) C(14) 1.561(5) 1_555 1_555 yes C(13) C(17) 1.564(4) 1_555 1_555 yes C(13) C(18) 1.538(5) 1_555 1_555 yes C(14) C(15) 1.537(5) 1_555 1_555 yes C(15) C(16) 1.543(6) 1_555 1_555 yes C(16) C(17) 1.548(6) 1_555 1_555 yes C(17) C(20) 1.539(5) 1_555 1_555 yes C(20) C(21) 1.514(7) 1_555 1_555 yes C(20) C(22) 1.549(5) 1_555 1_555 yes C(22) C(23) 1.508(6) 1_555 1_555 yes C(24) C(25) 1.530(5) 1_555 1_555 yes C(24) C(33) 1.538(6) 1_555 1_555 yes C(25) C(26) 1.519(6) 1_555 1_555 yes C(26) C(27) 1.518(6) 1_555 1_555 yes C(27) C(28) 1.534(7) 1_555 1_555 yes C(28) C(29) 1.549(7) 1_555 1_555 yes C(28) C(33) 1.535(6) 1_555 1_555 yes C(29) C(30) 1.517(7) 1_555 1_555 yes C(30) C(31) 1.518(6) 1_555 1_555 yes C(31) C(32) 1.549(5) 1_555 1_555 yes C(31) C(37) 1.536(5) 1_555 1_555 yes C(32) C(33) 1.569(5) 1_555 1_555 yes C(32) C(34) 1.535(5) 1_555 1_555 yes C(33) C(42) 1.571(6) 1_555 1_555 yes C(34) C(35) 1.536(5) 1_555 1_555 yes C(35) C(36) 1.541(5) 1_555 1_555 yes C(36) C(37) 1.538(5) 1_555 1_555 yes C(36) C(40) 1.573(4) 1_555 1_555 yes C(36) C(41) 1.535(4) 1_555 1_555 yes C(37) C(38) 1.543(5) 1_555 1_555 yes C(38) C(39) 1.550(5) 1_555 1_555 yes C(39) C(40) 1.575(5) 1_555 1_555 yes C(40) C(43) 1.514(5) 1_555 1_555 yes C(43) C(44) 1.548(6) 1_555 1_555 yes C(43) C(45) 1.558(5) 1_555 1_555 yes C(45) C(46) 1.510(6) 1_555 1_555 yes C(47) C(48) 1.57(2) 1_555 1_555 yes C(48) C(49) 1.53(1) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(3) O(1) H(36) 103.7(3) 1_555 1_555 1_555 no C(12) O(2) H(37) 108.7(2) 1_555 1_555 1_555 no C(23) O(4) H(38) 103.1(3) 1_555 1_555 1_555 no C(26) O(5) H(74) 113.2(3) 1_555 1_555 1_555 no C(35) O(6) H(75) 107.1(3) 1_555 1_555 1_555 no C(46) O(8) H(76) 104.0(3) 1_555 1_555 1_555 no C(2) C(1) C(10) 115.2(3) 1_555 1_555 1_555 yes C(2) C(1) H(1) 108.1(3) 1_555 1_555 1_555 no C(2) C(1) H(2) 107.6(4) 1_555 1_555 1_555 no C(10) C(1) H(1) 108.0(4) 1_555 1_555 1_555 no C(10) C(1) H(2) 107.5(3) 1_555 1_555 1_555 no H(1) C(1) H(2) 110.5(4) 1_555 1_555 1_555 no C(1) C(2) C(3) 110.6(4) 1_555 1_555 1_555 yes C(1) C(2) H(3) 110.3(3) 1_555 1_555 1_555 no C(1) C(2) H(4) 108.8(4) 1_555 1_555 1_555 no C(3) C(2) H(3) 109.8(4) 1_555 1_555 1_555 no C(3) C(2) H(4) 108.1(3) 1_555 1_555 1_555 no H(3) C(2) H(4) 109.2(5) 1_555 1_555 1_555 no O(1) C(3) C(2) 112.4(4) 1_555 1_555 1_555 yes O(1) C(3) C(4) 111.5(4) 1_555 1_555 1_555 yes O(1) C(3) H(5) 107.4(3) 1_555 1_555 1_555 no C(2) C(3) C(4) 110.0(3) 1_555 1_555 1_555 yes C(2) C(3) H(5) 108.6(4) 1_555 1_555 1_555 no C(4) C(3) H(5) 106.8(5) 1_555 1_555 1_555 no C(3) C(4) C(5) 113.2(3) 1_555 1_555 1_555 yes C(3) C(4) H(6) 107.7(4) 1_555 1_555 1_555 no C(3) C(4) H(7) 107.7(5) 1_555 1_555 1_555 no C(5) C(4) H(6) 110.1(5) 1_555 1_555 1_555 no C(5) C(4) H(7) 109.9(4) 1_555 1_555 1_555 no H(6) C(4) H(7) 108.1(4) 1_555 1_555 1_555 no C(4) C(5) C(6) 111.5(4) 1_555 1_555 1_555 yes C(4) C(5) C(10) 113.1(3) 1_555 1_555 1_555 yes C(4) C(5) H(8) 105.3(4) 1_555 1_555 1_555 no C(6) C(5) C(10) 111.7(3) 1_555 1_555 1_555 yes C(6) C(5) H(8) 107.9(4) 1_555 1_555 1_555 no C(10) C(5) H(8) 106.8(3) 1_555 1_555 1_555 no C(5) C(6) C(7) 111.0(4) 1_555 1_555 1_555 yes C(5) C(6) H(9) 112.6(5) 1_555 1_555 1_555 no C(5) C(6) H(10) 108.5(4) 1_555 1_555 1_555 no C(7) C(6) H(9) 110.4(4) 1_555 1_555 1_555 no C(7) C(6) H(10) 106.8(5) 1_555 1_555 1_555 no H(9) C(6) H(10) 107.2(5) 1_555 1_555 1_555 no C(6) C(7) C(8) 109.8(3) 1_555 1_555 1_555 yes C(6) C(7) H(11) 110.0(4) 1_555 1_555 1_555 no C(6) C(7) H(12) 107.2(5) 1_555 1_555 1_555 no C(8) C(7) H(11) 110.3(4) 1_555 1_555 1_555 no C(8) C(7) H(12) 110.1(4) 1_555 1_555 1_555 no H(11) C(7) H(12) 109.4(4) 1_555 1_555 1_555 no C(7) C(8) C(9) 109.8(3) 1_555 1_555 1_555 yes C(7) C(8) C(14) 111.8(3) 1_555 1_555 1_555 yes C(7) C(8) H(13) 109.2(4) 1_555 1_555 1_555 no C(9) C(8) C(14) 110.8(3) 1_555 1_555 1_555 yes C(9) C(8) H(13) 108.1(3) 1_555 1_555 1_555 no C(14) C(8) H(13) 107.0(3) 1_555 1_555 1_555 no C(8) C(9) C(10) 112.3(3) 1_555 1_555 1_555 yes C(8) C(9) C(11) 112.4(3) 1_555 1_555 1_555 yes C(8) C(9) H(14) 106.4(3) 1_555 1_555 1_555 no C(10) C(9) C(11) 112.5(3) 1_555 1_555 1_555 yes C(10) C(9) H(14) 105.8(3) 1_555 1_555 1_555 no C(11) C(9) H(14) 106.8(3) 1_555 1_555 1_555 no C(1) C(10) C(5) 107.7(3) 1_555 1_555 1_555 yes C(1) C(10) C(9) 113.6(3) 1_555 1_555 1_555 yes C(1) C(10) C(19) 105.5(3) 1_555 1_555 1_555 yes C(5) C(10) C(9) 108.6(3) 1_555 1_555 1_555 yes C(5) C(10) C(19) 109.8(3) 1_555 1_555 1_555 yes C(9) C(10) C(19) 111.5(3) 1_555 1_555 1_555 yes C(9) C(11) C(12) 116.5(3) 1_555 1_555 1_555 yes C(9) C(11) H(15) 108.4(3) 1_555 1_555 1_555 no C(9) C(11) H(16) 108.0(3) 1_555 1_555 1_555 no C(12) C(11) H(15) 107.6(3) 1_555 1_555 1_555 no C(12) C(11) H(16) 107.3(3) 1_555 1_555 1_555 no H(15) C(11) H(16) 108.7(3) 1_555 1_555 1_555 no O(2) C(12) C(11) 109.4(3) 1_555 1_555 1_555 yes O(2) C(12) C(13) 109.8(3) 1_555 1_555 1_555 yes O(2) C(12) H(17) 108.1(3) 1_555 1_555 1_555 no C(11) C(12) C(13) 111.1(3) 1_555 1_555 1_555 yes C(11) C(12) H(17) 109.0(3) 1_555 1_555 1_555 no C(13) C(12) H(17) 109.3(3) 1_555 1_555 1_555 no C(12) C(13) C(14) 107.6(3) 1_555 1_555 1_555 yes C(12) C(13) C(17) 117.7(3) 1_555 1_555 1_555 yes C(12) C(13) C(18) 108.7(3) 1_555 1_555 1_555 yes C(14) C(13) C(17) 100.9(2) 1_555 1_555 1_555 yes C(14) C(13) C(18) 112.5(3) 1_555 1_555 1_555 yes C(17) C(13) C(18) 109.3(3) 1_555 1_555 1_555 yes C(8) C(14) C(13) 112.7(3) 1_555 1_555 1_555 yes C(8) C(14) C(15) 118.4(3) 1_555 1_555 1_555 yes C(8) C(14) H(18) 107.8(3) 1_555 1_555 1_555 no C(13) C(14) C(15) 103.9(3) 1_555 1_555 1_555 yes C(13) C(14) H(18) 106.3(3) 1_555 1_555 1_555 no C(15) C(14) H(18) 107.1(3) 1_555 1_555 1_555 no C(14) C(15) C(16) 104.8(3) 1_555 1_555 1_555 yes C(14) C(15) H(19) 110.9(3) 1_555 1_555 1_555 no C(14) C(15) H(20) 110.7(3) 1_555 1_555 1_555 no C(16) C(15) H(19) 111.8(3) 1_555 1_555 1_555 no C(16) C(15) H(20) 111.6(4) 1_555 1_555 1_555 no H(19) C(15) H(20) 107.1(4) 1_555 1_555 1_555 no C(15) C(16) C(17) 107.7(3) 1_555 1_555 1_555 yes C(15) C(16) H(21) 109.7(4) 1_555 1_555 1_555 no C(15) C(16) H(22) 109.3(4) 1_555 1_555 1_555 no C(17) C(16) H(21) 111.7(4) 1_555 1_555 1_555 no C(17) C(16) H(22) 110.3(3) 1_555 1_555 1_555 no H(21) C(16) H(22) 108.1(4) 1_555 1_555 1_555 no C(13) C(17) C(16) 102.9(3) 1_555 1_555 1_555 yes C(13) C(17) C(20) 117.3(3) 1_555 1_555 1_555 yes C(13) C(17) H(23) 106.4(3) 1_555 1_555 1_555 no C(16) C(17) C(20) 114.4(3) 1_555 1_555 1_555 yes C(16) C(17) H(23) 107.8(3) 1_555 1_555 1_555 no C(20) C(17) H(23) 107.4(3) 1_555 1_555 1_555 no C(13) C(18) H(24) 111.2(4) 1_555 1_555 1_555 no C(13) C(18) H(25) 109.5(3) 1_555 1_555 1_555 no C(13) C(18) H(26) 110.3(3) 1_555 1_555 1_555 no H(24) C(18) H(25) 108.2(4) 1_555 1_555 1_555 no H(24) C(18) H(26) 109.8(4) 1_555 1_555 1_555 no H(25) C(18) H(26) 107.9(4) 1_555 1_555 1_555 no C(10) C(19) H(27) 108.4(4) 1_555 1_555 1_555 no C(10) C(19) H(28) 109.8(4) 1_555 1_555 1_555 no C(10) C(19) H(29) 110.0(4) 1_555 1_555 1_555 no H(27) C(19) H(28) 109.2(5) 1_555 1_555 1_555 no H(27) C(19) H(29) 108.6(5) 1_555 1_555 1_555 no H(28) C(19) H(29) 110.8(5) 1_555 1_555 1_555 no C(17) C(20) C(21) 114.7(3) 1_555 1_555 1_555 yes C(17) C(20) C(22) 109.7(3) 1_555 1_555 1_555 yes C(17) C(20) H(30) 107.7(3) 1_555 1_555 1_555 no C(21) C(20) C(22) 108.6(4) 1_555 1_555 1_555 yes C(21) C(20) H(30) 108.1(4) 1_555 1_555 1_555 no C(22) C(20) H(30) 107.8(4) 1_555 1_555 1_555 no C(20) C(21) H(31) 108.5(4) 1_555 1_555 1_555 no C(20) C(21) H(32) 108.8(4) 1_555 1_555 1_555 no C(20) C(21) H(33) 109.3(5) 1_555 1_555 1_555 no H(31) C(21) H(32) 109.7(5) 1_555 1_555 1_555 no H(31) C(21) H(33) 109.6(4) 1_555 1_555 1_555 no H(32) C(21) H(33) 111.0(5) 1_555 1_555 1_555 no C(20) C(22) C(23) 112.9(3) 1_555 1_555 1_555 yes C(20) C(22) H(34) 108.9(4) 1_555 1_555 1_555 no C(20) C(22) H(35) 108.4(4) 1_555 1_555 1_555 no C(23) C(22) H(34) 108.2(4) 1_555 1_555 1_555 no C(23) C(22) H(35) 108.5(4) 1_555 1_555 1_555 no H(34) C(22) H(35) 109.9(4) 1_555 1_555 1_555 no O(3) C(23) O(4) 122.4(4) 1_555 1_555 1_555 yes O(3) C(23) C(22) 124.9(4) 1_555 1_555 1_555 yes O(4) C(23) C(22) 112.7(4) 1_555 1_555 1_555 yes C(25) C(24) C(33) 113.8(3) 1_555 1_555 1_555 yes C(25) C(24) H(39) 107.2(4) 1_555 1_555 1_555 no C(25) C(24) H(40) 106.8(3) 1_555 1_555 1_555 no C(33) C(24) H(39) 109.8(4) 1_555 1_555 1_555 no C(33) C(24) H(40) 108.7(4) 1_555 1_555 1_555 no H(39) C(24) H(40) 110.5(4) 1_555 1_555 1_555 no C(24) C(25) C(26) 110.5(3) 1_555 1_555 1_555 yes C(24) C(25) H(41) 109.6(4) 1_555 1_555 1_555 no C(24) C(25) H(42) 109.9(3) 1_555 1_555 1_555 no C(26) C(25) H(41) 108.4(3) 1_555 1_555 1_555 no C(26) C(25) H(42) 108.6(4) 1_555 1_555 1_555 no H(41) C(25) H(42) 109.8(4) 1_555 1_555 1_555 no O(5) C(26) C(25) 111.5(3) 1_555 1_555 1_555 yes O(5) C(26) C(27) 113.0(4) 1_555 1_555 1_555 yes O(5) C(26) H(43) 106.6(3) 1_555 1_555 1_555 no C(25) C(26) C(27) 108.7(3) 1_555 1_555 1_555 yes C(25) C(26) H(43) 108.8(4) 1_555 1_555 1_555 no C(27) C(26) H(43) 108.0(4) 1_555 1_555 1_555 no C(26) C(27) C(28) 113.8(4) 1_555 1_555 1_555 yes C(26) C(27) H(44) 108.6(4) 1_555 1_555 1_555 no C(26) C(27) H(45) 107.3(4) 1_555 1_555 1_555 no C(28) C(27) H(44) 110.0(4) 1_555 1_555 1_555 no C(28) C(27) H(45) 109.3(4) 1_555 1_555 1_555 no H(44) C(27) H(45) 107.7(5) 1_555 1_555 1_555 no C(27) C(28) C(29) 111.2(4) 1_555 1_555 1_555 yes C(27) C(28) C(33) 112.3(3) 1_555 1_555 1_555 yes C(27) C(28) H(46) 107.5(4) 1_555 1_555 1_555 no C(29) C(28) C(33) 112.3(4) 1_555 1_555 1_555 yes C(29) C(28) H(46) 106.4(4) 1_555 1_555 1_555 no C(33) C(28) H(46) 106.8(4) 1_555 1_555 1_555 no C(28) C(29) C(30) 112.5(3) 1_555 1_555 1_555 yes C(28) C(29) H(47) 110.6(6) 1_555 1_555 1_555 no C(28) C(29) H(48) 111.1(5) 1_555 1_555 1_555 no C(30) C(29) H(47) 105.1(4) 1_555 1_555 1_555 no C(30) C(29) H(48) 107.6(6) 1_555 1_555 1_555 no H(47) C(29) H(48) 109.8(4) 1_555 1_555 1_555 no C(29) C(30) C(31) 111.0(4) 1_555 1_555 1_555 yes C(29) C(30) H(49) 107.0(4) 1_555 1_555 1_555 no C(29) C(30) H(50) 109.6(4) 1_555 1_555 1_555 no C(31) C(30) H(49) 109.8(3) 1_555 1_555 1_555 no C(31) C(30) H(50) 110.9(4) 1_555 1_555 1_555 no H(49) C(30) H(50) 108.4(5) 1_555 1_555 1_555 no C(30) C(31) C(32) 111.0(3) 1_555 1_555 1_555 yes C(30) C(31) C(37) 112.3(4) 1_555 1_555 1_555 yes C(30) C(31) H(51) 107.2(3) 1_555 1_555 1_555 no C(32) C(31) C(37) 108.6(3) 1_555 1_555 1_555 yes C(32) C(31) H(51) 108.0(4) 1_555 1_555 1_555 no C(37) C(31) H(51) 109.7(3) 1_555 1_555 1_555 no C(31) C(32) C(33) 111.1(3) 1_555 1_555 1_555 yes C(31) C(32) C(34) 113.4(3) 1_555 1_555 1_555 yes C(31) C(32) H(52) 105.2(3) 1_555 1_555 1_555 no C(33) C(32) C(34) 113.5(3) 1_555 1_555 1_555 yes C(33) C(32) H(52) 105.9(3) 1_555 1_555 1_555 no C(34) C(32) H(52) 107.0(3) 1_555 1_555 1_555 no C(24) C(33) C(28) 108.9(3) 1_555 1_555 1_555 yes C(24) C(33) C(32) 112.9(3) 1_555 1_555 1_555 yes C(24) C(33) C(42) 104.4(4) 1_555 1_555 1_555 yes C(28) C(33) C(32) 110.2(3) 1_555 1_555 1_555 yes C(28) C(33) C(42) 110.4(4) 1_555 1_555 1_555 yes C(32) C(33) C(42) 110.0(3) 1_555 1_555 1_555 yes C(32) C(34) C(35) 114.0(3) 1_555 1_555 1_555 yes C(32) C(34) H(53) 108.7(3) 1_555 1_555 1_555 no C(32) C(34) H(54) 109.4(3) 1_555 1_555 1_555 no C(35) C(34) H(53) 107.6(3) 1_555 1_555 1_555 no C(35) C(34) H(54) 108.8(3) 1_555 1_555 1_555 no H(53) C(34) H(54) 108.2(4) 1_555 1_555 1_555 no O(6) C(35) C(34) 107.7(3) 1_555 1_555 1_555 yes O(6) C(35) C(36) 112.3(3) 1_555 1_555 1_555 yes O(6) C(35) H(55) 108.3(3) 1_555 1_555 1_555 no C(34) C(35) C(36) 112.1(3) 1_555 1_555 1_555 yes C(34) C(35) H(55) 109.1(3) 1_555 1_555 1_555 no C(36) C(35) H(55) 107.3(3) 1_555 1_555 1_555 no C(35) C(36) C(37) 106.9(3) 1_555 1_555 1_555 yes C(35) C(36) C(40) 117.5(3) 1_555 1_555 1_555 yes C(35) C(36) C(41) 108.8(3) 1_555 1_555 1_555 yes C(37) C(36) C(40) 101.8(3) 1_555 1_555 1_555 yes C(37) C(36) C(41) 113.3(3) 1_555 1_555 1_555 yes C(40) C(36) C(41) 108.7(3) 1_555 1_555 1_555 yes C(31) C(37) C(36) 113.6(3) 1_555 1_555 1_555 yes C(31) C(37) C(38) 117.2(3) 1_555 1_555 1_555 yes C(31) C(37) H(56) 107.7(3) 1_555 1_555 1_555 no C(36) C(37) C(38) 103.7(3) 1_555 1_555 1_555 yes C(36) C(37) H(56) 107.3(3) 1_555 1_555 1_555 no C(38) C(37) H(56) 106.8(3) 1_555 1_555 1_555 no C(37) C(38) C(39) 104.7(3) 1_555 1_555 1_555 yes C(37) C(38) H(57) 110.0(4) 1_555 1_555 1_555 no C(37) C(38) H(58) 110.2(4) 1_555 1_555 1_555 no C(39) C(38) H(57) 110.4(4) 1_555 1_555 1_555 no C(39) C(38) H(58) 111.8(4) 1_555 1_555 1_555 no H(57) C(38) H(58) 109.6(4) 1_555 1_555 1_555 no C(38) C(39) C(40) 107.2(3) 1_555 1_555 1_555 yes C(38) C(39) H(59) 110.7(4) 1_555 1_555 1_555 no C(38) C(39) H(60) 108.9(3) 1_555 1_555 1_555 no C(40) C(39) H(59) 111.8(3) 1_555 1_555 1_555 no C(40) C(39) H(60) 109.3(4) 1_555 1_555 1_555 no H(59) C(39) H(60) 108.8(4) 1_555 1_555 1_555 no C(36) C(40) C(39) 102.1(3) 1_555 1_555 1_555 yes C(36) C(40) C(43) 118.3(3) 1_555 1_555 1_555 yes C(36) C(40) H(61) 107.3(3) 1_555 1_555 1_555 no C(39) C(40) C(43) 112.8(3) 1_555 1_555 1_555 yes C(39) C(40) H(61) 106.3(3) 1_555 1_555 1_555 no C(43) C(40) H(61) 109.1(3) 1_555 1_555 1_555 no C(36) C(41) H(62) 108.7(3) 1_555 1_555 1_555 no C(36) C(41) H(63) 110.1(4) 1_555 1_555 1_555 no C(36) C(41) H(64) 110.0(3) 1_555 1_555 1_555 no H(62) C(41) H(63) 108.2(4) 1_555 1_555 1_555 no H(62) C(41) H(64) 109.1(4) 1_555 1_555 1_555 no H(63) C(41) H(64) 110.6(4) 1_555 1_555 1_555 no C(33) C(42) H(65) 110.4(5) 1_555 1_555 1_555 no C(33) C(42) H(66) 109.8(5) 1_555 1_555 1_555 no C(33) C(42) H(67) 109.3(4) 1_555 1_555 1_555 no H(65) C(42) H(66) 109.7(5) 1_555 1_555 1_555 no H(65) C(42) H(67) 108.9(6) 1_555 1_555 1_555 no H(66) C(42) H(67) 108.8(6) 1_555 1_555 1_555 no C(40) C(43) C(44) 113.4(3) 1_555 1_555 1_555 yes C(40) C(43) C(45) 110.8(3) 1_555 1_555 1_555 yes C(40) C(43) H(68) 109.1(3) 1_555 1_555 1_555 no C(44) C(43) C(45) 107.3(3) 1_555 1_555 1_555 yes C(44) C(43) H(68) 108.3(4) 1_555 1_555 1_555 no C(45) C(43) H(68) 107.8(3) 1_555 1_555 1_555 no C(43) C(44) H(69) 110.6(4) 1_555 1_555 1_555 no C(43) C(44) H(70) 109.1(4) 1_555 1_555 1_555 no C(43) C(44) H(71) 108.9(4) 1_555 1_555 1_555 no H(69) C(44) H(70) 109.9(5) 1_555 1_555 1_555 no H(69) C(44) H(71) 109.8(5) 1_555 1_555 1_555 no H(70) C(44) H(71) 108.4(5) 1_555 1_555 1_555 no C(43) C(45) C(46) 112.4(3) 1_555 1_555 1_555 yes C(43) C(45) H(72) 108.4(3) 1_555 1_555 1_555 no C(43) C(45) H(73) 109.7(4) 1_555 1_555 1_555 no C(46) C(45) H(72) 108.4(4) 1_555 1_555 1_555 no C(46) C(45) H(73) 110.3(4) 1_555 1_555 1_555 no H(72) C(45) H(73) 107.5(4) 1_555 1_555 1_555 no O(7) C(46) O(8) 123.8(4) 1_555 1_555 1_555 yes O(7) C(46) C(45) 122.6(4) 1_555 1_555 1_555 yes O(8) C(46) C(45) 113.6(4) 1_555 1_555 1_555 yes C(48) C(47) H(77) 101(1) 1_555 1_555 1_555 no C(48) C(47) H(78) 107(1) 1_555 1_555 1_555 no C(48) C(47) H(79) 105(1) 1_555 1_555 1_555 no H(77) C(47) H(78) 111(1) 1_555 1_555 1_555 no H(77) C(47) H(79) 108(1) 1_555 1_555 1_555 no H(78) C(47) H(79) 120(2) 1_555 1_555 1_555 no O(9) C(48) C(47) 126(1) 1_555 1_555 1_555 yes O(9) C(48) C(49) 133(1) 1_555 1_555 1_555 yes C(47) C(48) C(49) 99(1) 1_555 1_555 1_555 yes C(48) C(49) H(80) 109.1(8) 1_555 1_555 1_555 no C(48) C(49) H(81) 111(1) 1_555 1_555 1_555 no C(48) C(49) H(82) 106(1) 1_555 1_555 1_555 no H(80) C(49) H(81) 111(2) 1_555 1_555 1_555 no H(80) C(49) H(82) 107(1) 1_555 1_555 1_555 no H(81) C(49) H(82) 110(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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) -179.8(3) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 179.7(3) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(11) C(9) 73.2(4) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(13) C(14) -66.4(3) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(13) C(17) 46.6(4) 1_555 1_555 1_555 1_555 yes O(2) C(12) C(13) C(18) 171.5(3) 1_555 1_555 1_555 1_555 yes O(3) C(23) C(22) C(20) -129.7(6) 1_555 1_555 1_555 1_555 yes O(4) C(23) C(22) C(20) 51.0(6) 1_555 1_555 1_555 1_555 yes O(5) C(26) C(25) C(24) 177.8(3) 1_555 1_555 1_555 1_555 yes O(5) C(26) C(27) C(28) -179.2(3) 1_555 1_555 1_555 1_555 yes O(6) C(35) C(34) C(32) 72.7(4) 1_555 1_555 1_555 1_555 yes O(6) C(35) C(36) C(37) -65.0(3) 1_555 1_555 1_555 1_555 yes O(6) C(35) C(36) C(40) 48.4(4) 1_555 1_555 1_555 1_555 yes O(6) C(35) C(36) C(41) 172.4(3) 1_555 1_555 1_555 1_555 yes O(7) C(46) C(45) C(43) -127.5(5) 1_555 1_555 1_555 1_555 yes O(8) C(46) C(45) C(43) 52.8(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -54.9(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 50.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 177.5(3) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -176.5(3) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 55.4(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -54.1(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 66.2(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -171.3(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 54.3(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 58.0(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 179.6(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.5(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 71.6(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -72.8(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 165.1(3) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 57.6(6) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -56.7(4) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 175.3(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 54.0(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -68.1(4) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -59.1(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) 177.5(4) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -56.0(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 60.0(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -171.9(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -177.6(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -56.2(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 64.4(4) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 43.9(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -62.9(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 173.2(3) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 56.9(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -155.7(3) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 59.5(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -179.0(3) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -48.3(4) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -175.9(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 172.0(3) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -47.9(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -63.6(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 54.8(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 167.8(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -67.3(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 167.8(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -157.0(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 76.5(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -29.9(3) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 22.8(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -64.1(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 173.4(3) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -40.3(3) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -166.8(3) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 4.3(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 43.8(3) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -72.5(3) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 151.1(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.4(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 175.3(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 52.8(4) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -170.5(4) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -48.1(4) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 63.5(5) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) -57.0(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(27) 50.4(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(29) 176.6(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(31) -176.4(3) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(34) 54.4(4) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(28) -53.7(4) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(32) 68.9(4) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(42) -171.6(3) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 56.4(4) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(24) C(33) 58.4(4) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 178.8(3) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(33) -54.5(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 73.1(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(32) -73.8(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(42) 164.5(4) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 55.4(6) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(31) -54.5(4) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(34) 176.3(3) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(32) 52.4(5) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(42) -69.3(5) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -57.4(4) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(37) -179.1(3) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(28) C(33) -53.6(6) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) 57.3(4) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(34) -173.4(3) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(36) -177.8(3) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(38) -56.8(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(42) 67.4(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(34) C(35) 47.5(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(35) -62.6(3) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(40) 173.7(3) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(41) 57.2(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(38) C(39) -158.6(3) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(36) 59.2(4) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(38) -179.8(3) 1_555 1_555 1_555 1_555 yes C(32) C(34) C(35) C(36) -51.2(4) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(37) -178.8(3) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(34) C(35) 175.5(3) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(31) C(37) -49.6(4) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(33) C(42) -61.8(5) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) 56.4(3) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(40) 169.8(3) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(41) -66.3(4) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 169.1(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(39) -156.0(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(43) 79.4(4) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) -32.6(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(39) C(38) 20.2(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(44) -63.5(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(45) 175.8(3) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(39) -39.8(3) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(43) -164.3(3) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) 7.1(4) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(40) 45.4(3) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(41) -71.1(3) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(43) 148.2(3) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(36) C(41) 80.0(3) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(44) 177.5(3) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(45) 56.7(4) 1_555 1_555 1_555 1_555 yes C(40) C(43) C(45) C(46) -173.6(3) 1_555 1_555 1_555 1_555 yes C(41) C(36) C(40) C(43) -44.5(4) 1_555 1_555 1_555 1_555 yes C(44) C(43) C(45) C(46) 62.1(4) 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(4) 2.591(5) 1_555 1_545 ? O(1) O(7) 2.790(5) 1_555 1_455 ? O(1) O(3) 3.201(6) 1_555 1_545 ? O(1) C(23) 3.296(5) 1_555 1_545 ? O(2) O(6) 3.394(4) 1_555 1_455 ? O(3) O(5) 2.752(5) 1_555 1_455 ? O(3) C(26) 3.496(6) 1_555 1_455 ? O(5) O(8) 2.628(5) 1_555 1_565 ? O(5) O(7) 3.302(5) 1_555 1_565 ? O(5) C(46) 3.354(5) 1_555 1_565 ? O(6) C(17) 3.587(4) 1_555 1_655 ? O(6) C(21) 3.590(5) 1_555 1_655 ? O(7) C(3) 3.479(6) 1_555 1_655 ? O(7) C(49) 3.50(1) 1_555 1_555 ? O(7) O(9) 3.54(1) 1_555 1_554 ? O(7) C(4) 3.584(7) 1_555 1_655 ? O(8) C(48) 3.593(9) 1_555 1_554 ? O(9) C(46) 3.28(1) 1_555 1_556 ? O(9) C(2) 3.42(1) 1_555 1_655 ? O(9) C(45) 3.44(1) 1_555 1_556 ? O(9) C(4) 3.59(1) 1_555 1_656 ? #------------------------------------------------------------------------------ _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 565-8710 Japan ; _publ_contact_author_email ' miyata@ap.chem.eng.osaka-u.ac.jp ' _publ_contact_author_fax ' +81-6-879-7404 ' _publ_contact_author_phone ' +81-6-879-7406 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chem.Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; A Robust Structural Motif in Inclusion Crystals of Norbile Acids ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Michihiro Sugahara ' ? ; Material and Life Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-8710 Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_Nor #------------------------------------------------------------------------------ _audit_creation_date 'Sat Dec 26 17:34:42 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 815.18 _chemical_formula_analytical ? _chemical_formula_sum 'C49 H82 O9 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.490(1) _cell_length_b 15.257(1) _cell_length_c 7.567(3) _cell_angle_alpha 92.785(3) _cell_angle_beta 104.24(2) _cell_angle_gamma 79.999(8) _cell_volume 1155.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 210.4 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448.00 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 210.4 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_detector_area_resol_mean 0.010000 _diffrn_mesured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_reflns_number 3603 _reflns_number_total 3603 _reflns_number_gt 3467 _reflns_observed_expression >1.5sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.1882(3) 1.1017(2) 0.9494(5) 0.0581(8) Uani 1.00 d . . . O(2) O 0.2885(3) 0.8225(2) 0.5854(4) 0.0587(8) Uani 1.00 d . . . O(3) O 0.4213(4) 0.2251(2) 1.0662(6) 0.084(1) Uani 1.00 d . . . O(4) O 0.2353(3) 0.2523(2) 0.8472(5) 0.0705(9) Uani 1.00 d . . . O(5) O -0.3521(3) 0.1048(2) 1.2170(5) 0.0703(9) Uani 1.00 d . . . O(6) O -0.3228(3) 0.3537(2) 0.8144(4) 0.0550(7) Uani 1.00 d . . . O(7) O -0.5793(4) 0.9872(2) 1.0715(7) 0.086(1) Uani 1.00 d . . . O(8) O -0.3628(3) 0.9390(2) 1.1248(6) 0.076(1) Uani 1.00 d . . . O(9) O 0.3890(9) 0.9693(4) 0.497(2) 0.258(3) Uani 1.00 d . . . C(1) C -0.0628(4) 0.9453(3) 0.8848(6) 0.0464(9) Uani 1.00 d . . . C(2) C 0.0498(4) 0.9952(3) 0.9864(6) 0.0459(9) Uani 1.00 d . . . C(3) C 0.0847(4) 1.0530(3) 0.8551(6) 0.0485(9) Uani 1.00 d . . . C(4) C 0.1233(4) 0.9976(3) 0.6999(6) 0.0512(10) Uani 1.00 d . . . C(5) C 0.0150(4) 0.9454(3) 0.5953(6) 0.054(1) Uani 1.00 d . . . C(6) C 0.0559(5) 0.8891(3) 0.4378(6) 0.063(1) Uani 1.00 d . . . C(7) C 0.1585(5) 0.8062(3) 0.4940(5) 0.0535(9) Uani 1.00 d . . . C(8) C 0.1123(4) 0.7486(2) 0.6210(5) 0.0419(8) Uani 1.00 d . . . C(9) C 0.0789(4) 0.8034(3) 0.7849(5) 0.0420(8) Uani 1.00 d . . . C(10) C -0.0314(4) 0.8879(3) 0.7207(6) 0.0479(9) Uani 1.00 d . . . C(11) C 0.0502(4) 0.7469(3) 0.9281(5) 0.0471(9) Uani 1.00 d . . . C(12) C 0.1489(4) 0.6610(3) 0.9763(5) 0.0454(9) Uani 1.00 d . . . C(13) C 0.1664(3) 0.6058(2) 0.8076(5) 0.0380(8) Uani 1.00 d . . . C(14) C 0.2130(3) 0.6663(2) 0.6858(5) 0.0389(8) Uani 1.00 d . . . C(15) C 0.2581(4) 0.6039(3) 0.5416(6) 0.0510(9) Uani 1.00 d . . . C(16) C 0.3128(4) 0.5151(3) 0.6407(6) 0.0508(9) Uani 1.00 d . . . C(17) C 0.2832(3) 0.5242(2) 0.8331(5) 0.0414(8) Uani 1.00 d . . . C(18) C 0.0346(4) 0.5758(3) 0.7087(6) 0.0509(10) Uani 1.00 d . . . C(19) C -0.1655(4) 0.8582(3) 0.6221(8) 0.063(1) Uani 1.00 d . . . C(20) C 0.2610(4) 0.4380(2) 0.9086(6) 0.0468(9) Uani 1.00 d . . . C(21) C 0.2464(5) 0.4469(3) 1.1044(7) 0.068(1) Uani 1.00 d . . . C(22) C 0.3758(4) 0.3605(3) 0.8980(7) 0.058(1) Uani 1.00 d . . . C(23) C 0.3493(4) 0.2737(3) 0.9477(7) 0.0560(10) Uani 1.00 d . . . C(24) C -0.1269(4) 0.2652(3) 1.4524(5) 0.0472(9) Uani 1.00 d . . . C(25) C -0.2479(4) 0.2170(3) 1.4119(6) 0.0512(10) Uani 1.00 d . . . C(26) C -0.2386(4) 0.1512(3) 1.2578(6) 0.0536(10) Uani 1.00 d . . . C(27) C -0.2242(4) 0.1945(3) 1.0888(6) 0.0527(10) Uani 1.00 d . . . C(28) C -0.1049(4) 0.2437(2) 1.1288(5) 0.0445(8) Uani 1.00 d . . . C(29) C -0.0918(4) 0.2881(3) 0.9565(5) 0.055(1) Uani 1.00 d . . . C(30) C -0.1908(4) 0.3716(3) 0.8965(5) 0.0484(9) Uani 1.00 d . . . C(31) C -0.1970(3) 0.4381(2) 1.0537(5) 0.0377(8) Uani 1.00 d . . . C(32) C -0.2186(3) 0.3931(2) 1.2211(4) 0.0364(7) Uani 1.00 d . . . C(33) C -0.1064(4) 0.3122(2) 1.2891(5) 0.0409(8) Uani 1.00 d . . . C(34) C -0.2391(4) 0.4618(2) 1.3765(5) 0.0444(9) Uani 1.00 d . . . C(35) C -0.3355(4) 0.5480(3) 1.3117(5) 0.0438(9) Uani 1.00 d . . . C(36) C -0.2995(3) 0.5909(2) 1.1557(5) 0.0376(8) Uani 1.00 d . . . C(37) C -0.3024(3) 0.5221(2) 1.0012(5) 0.0396(8) Uani 1.00 d . . . C(38) C -0.3028(4) 0.5730(3) 0.8331(5) 0.0518(9) Uani 1.00 d . . . C(39) C -0.3773(4) 0.6678(3) 0.8616(5) 0.0479(9) Uani 1.00 d . . . C(40) C -0.4051(3) 0.6688(2) 1.0539(5) 0.0377(7) Uani 1.00 d . . . C(41) C -0.1635(4) 0.6229(3) 1.2200(6) 0.0506(10) Uani 1.00 d . . . C(42) C 0.0316(4) 0.3400(3) 1.3559(7) 0.057(1) Uani 1.00 d . . . C(43) C -0.4099(4) 0.7616(3) 1.1444(6) 0.0458(8) Uani 1.00 d . . . C(44) C -0.4482(5) 0.7667(3) 1.3285(6) 0.058(1) Uani 1.00 d . . . C(45) C -0.5053(4) 0.8324(3) 1.0180(7) 0.059(1) Uani 1.00 d . . . C(46) C -0.4891(4) 0.9250(3) 1.0750(7) 0.0579(10) Uani 1.00 d . . . C(47) C 0.3307(9) 1.1277(7) 0.430(1) 0.116(3) Uani 1.00 d . . . C(48) C 0.4147(8) 1.0457(5) 0.529(1) 0.113(2) Uani 1.00 d . . . C(49) C 0.531(1) 1.068(1) 0.670(2) 0.191(5) Uani 1.00 d . . . H(1) H -0.0789 0.9065 0.9701 0.0528 Uiso 1.00 calc . . . H(2) H -0.1422 0.9875 0.8431 0.0528 Uiso 1.00 calc . . . H(3) H 0.0193 1.0324 1.0785 0.0506 Uiso 1.00 calc . . . H(4) H 0.1251 0.9542 1.0400 0.0506 Uiso 1.00 calc . . . H(5) H 0.0075 1.0959 0.8055 0.0563 Uiso 1.00 calc . . . H(6) H 0.2011 0.9572 0.7474 0.0605 Uiso 1.00 calc . . . H(7) H 0.1394 1.0369 0.6164 0.0605 Uiso 1.00 calc . . . H(8) H -0.0605 0.9889 0.5421 0.0608 Uiso 1.00 calc . . . H(9) H -0.0209 0.8734 0.3602 0.0706 Uiso 1.00 calc . . . H(10) H 0.0944 0.9266 0.3736 0.0706 Uiso 1.00 calc . . . H(11) H 0.1641 0.7728 0.3872 0.0629 Uiso 1.00 calc . . . H(12) H 0.0327 0.7309 0.5533 0.0484 Uiso 1.00 calc . . . H(13) H 0.1565 0.8266 0.8459 0.0473 Uiso 1.00 calc . . . H(14) H 0.0499 0.7821 1.0359 0.0537 Uiso 1.00 calc . . . H(15) H -0.0372 0.7323 0.8814 0.0537 Uiso 1.00 calc . . . H(16) H 0.1176 0.6272 1.0538 0.0525 Uiso 1.00 calc . . . H(17) H 0.2325 0.6761 1.0396 0.0525 Uiso 1.00 calc . . . H(18) H 0.2889 0.6874 0.7606 0.0444 Uiso 1.00 calc . . . H(19) H 0.1848 0.5985 0.4423 0.0596 Uiso 1.00 calc . . . H(20) H 0.3253 0.6254 0.5013 0.0596 Uiso 1.00 calc . . . H(21) H 0.4058 0.5014 0.6530 0.0590 Uiso 1.00 calc . . . H(22) H 0.2699 0.4700 0.5751 0.0590 Uiso 1.00 calc . . . H(23) H 0.3579 0.5444 0.9161 0.0485 Uiso 1.00 calc . . . H(24) H 0.0460 0.5429 0.6030 0.0584 Uiso 1.00 calc . . . H(25) H 0.0082 0.5401 0.7881 0.0584 Uiso 1.00 calc . . . H(26) H -0.0332 0.6268 0.6743 0.0584 Uiso 1.00 calc . . . H(27) H -0.1531 0.8227 0.5189 0.0787 Uiso 1.00 calc . . . H(28) H -0.1924 0.8236 0.7037 0.0787 Uiso 1.00 calc . . . H(29) H -0.2322 0.9084 0.5843 0.0787 Uiso 1.00 calc . . . H(30) H 0.1796 0.4233 0.8346 0.0535 Uiso 1.00 calc . . . H(31) H 0.3247 0.4640 1.1822 0.0772 Uiso 1.00 calc . . . H(32) H 0.1719 0.4933 1.1118 0.0772 Uiso 1.00 calc . . . H(33) H 0.2312 0.3933 1.1447 0.0772 Uiso 1.00 calc . . . H(34) H 0.4535 0.3748 0.9791 0.0685 Uiso 1.00 calc . . . H(35) H 0.3852 0.3587 0.7766 0.0685 Uiso 1.00 calc . . . H(36) H 0.2725 1.0611 1.0043 0.0696 Uiso 1.00 calc . . . H(37) H 0.3242 0.8627 0.5145 0.0702 Uiso 1.00 calc . . . H(38) H 0.2210 0.1910 0.8680 0.0843 Uiso 1.00 calc . . . H(39) H -0.1384 0.3098 1.5432 0.0550 Uiso 1.00 calc . . . H(40) H -0.0492 0.2237 1.4977 0.0550 Uiso 1.00 calc . . . H(41) H -0.3281 0.2588 1.3802 0.0597 Uiso 1.00 calc . . . H(42) H -0.2476 0.1857 1.5188 0.0597 Uiso 1.00 calc . . . H(43) H -0.1624 0.1080 1.2983 0.0613 Uiso 1.00 calc . . . H(44) H -0.2115 0.1490 1.0017 0.0624 Uiso 1.00 calc . . . H(45) H -0.3037 0.2348 1.0414 0.0624 Uiso 1.00 calc . . . H(46) H -0.0281 0.2013 1.1665 0.0521 Uiso 1.00 calc . . . H(47) H -0.1044 0.2463 0.8588 0.0629 Uiso 1.00 calc . . . H(48) H -0.0049 0.3022 0.9787 0.0629 Uiso 1.00 calc . . . H(49) H -0.1617 0.4000 0.8095 0.0565 Uiso 1.00 calc . . . H(50) H -0.1141 0.4581 1.0914 0.0439 Uiso 1.00 calc . . . H(51) H -0.3005 0.3708 1.1825 0.0424 Uiso 1.00 calc . . . H(52) H -0.2719 0.4347 1.4622 0.0523 Uiso 1.00 calc . . . H(53) H -0.1546 0.4776 1.4348 0.0523 Uiso 1.00 calc . . . H(54) H -0.4235 0.5349 1.2713 0.0524 Uiso 1.00 calc . . . H(55) H -0.3327 0.5890 1.4117 0.0524 Uiso 1.00 calc . . . H(56) H -0.3882 0.5035 0.9777 0.0458 Uiso 1.00 calc . . . H(57) H -0.3487 0.5469 0.7261 0.0600 Uiso 1.00 calc . . . H(58) H -0.2150 0.5758 0.8280 0.0600 Uiso 1.00 calc . . . H(59) H -0.3256 0.7116 0.8542 0.0542 Uiso 1.00 calc . . . H(60) H -0.4607 0.6799 0.7715 0.0542 Uiso 1.00 calc . . . H(61) H -0.4915 0.6534 1.0396 0.0443 Uiso 1.00 calc . . . H(62) H -0.1670 0.6650 1.3152 0.0580 Uiso 1.00 calc . . . H(63) H -0.1458 0.6500 1.1195 0.0580 Uiso 1.00 calc . . . H(64) H -0.0969 0.5734 1.2602 0.0580 Uiso 1.00 calc . . . H(65) H 0.0302 0.3808 1.4583 0.0662 Uiso 1.00 calc . . . H(66) H 0.0502 0.3712 1.2614 0.0662 Uiso 1.00 calc . . . H(67) H 0.0980 0.2907 1.3927 0.0662 Uiso 1.00 calc . . . H(68) H -0.3236 0.7776 1.1657 0.0505 Uiso 1.00 calc . . . H(69) H -0.3882 0.7256 1.4092 0.0712 Uiso 1.00 calc . . . H(70) H -0.5368 0.7541 1.3095 0.0712 Uiso 1.00 calc . . . H(71) H -0.4473 0.8257 1.3777 0.0712 Uiso 1.00 calc . . . H(72) H -0.5945 0.8262 1.0138 0.0699 Uiso 1.00 calc . . . H(73) H -0.4901 0.8244 0.8993 0.0699 Uiso 1.00 calc . . . H(74) H -0.4331 0.1454 1.1478 0.0842 Uiso 1.00 calc . . . H(75) H -0.3272 0.2988 0.7287 0.0658 Uiso 1.00 calc . . . H(76) H -0.3594 1.0010 1.1764 0.0913 Uiso 1.00 calc . . . H(77) H 0.3305 1.1233 0.3032 0.1413 Uiso 1.00 calc . . . H(78) H 0.3736 1.1795 0.4774 0.1413 Uiso 1.00 calc . . . H(79) H 0.2448 1.1380 0.4457 0.1413 Uiso 1.00 calc . . . H(80) H 0.6057 1.0281 0.6310 0.2295 Uiso 1.00 calc . . . H(81) H 0.5325 1.1222 0.6673 0.2295 Uiso 1.00 calc . . . H(82) H 0.5235 1.0414 0.7778 0.2295 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) 0.057(1) 0.035(1) 0.083(2) -0.011(1) 0.014(1) -0.007(1) O(2) 0.066(1) 0.057(2) 0.063(2) -0.009(1) 0.032(1) 0.005(1) O(3) 0.076(2) 0.046(2) 0.121(3) -0.006(2) -0.001(2) 0.034(2) O(4) 0.067(2) 0.062(2) 0.082(2) -0.020(1) 0.009(2) 0.006(2) O(5) 0.070(2) 0.037(1) 0.098(2) -0.020(1) -0.001(2) 0.012(1) O(6) 0.069(1) 0.040(1) 0.048(1) -0.004(1) 0.004(1) -0.005(1) O(7) 0.072(2) 0.041(2) 0.136(3) 0.011(1) 0.017(2) 0.004(2) O(8) 0.060(1) 0.042(2) 0.119(3) -0.013(1) 0.007(2) -0.006(2) O(9) 0.389(6) 0.078(3) 0.452(8) -0.099(3) 0.341(4) -0.069(4) C(1) 0.045(2) 0.041(2) 0.056(2) -0.010(1) 0.014(1) 0.001(1) C(2) 0.047(2) 0.040(2) 0.050(2) -0.005(1) 0.013(1) -0.007(1) C(3) 0.049(2) 0.035(2) 0.063(2) -0.006(1) 0.017(1) -0.003(1) C(4) 0.060(2) 0.040(2) 0.057(2) -0.003(1) 0.024(1) 0.005(1) C(5) 0.055(2) 0.058(2) 0.044(2) 0.000(2) 0.009(1) 0.002(1) C(6) 0.091(3) 0.054(2) 0.040(2) -0.001(2) 0.014(2) 0.006(2) C(7) 0.074(2) 0.054(2) 0.034(2) -0.008(2) 0.019(1) 0.001(1) C(8) 0.046(2) 0.038(2) 0.039(2) -0.008(1) 0.005(1) -0.002(1) C(9) 0.036(1) 0.053(2) 0.036(2) -0.007(1) 0.007(1) -0.003(1) C(10) 0.039(2) 0.050(2) 0.048(2) -0.005(1) 0.001(1) -0.005(1) C(11) 0.052(2) 0.049(2) 0.043(2) -0.005(1) 0.020(1) -0.004(1) C(12) 0.054(2) 0.048(2) 0.038(2) -0.007(1) 0.015(1) 0.004(1) C(13) 0.037(1) 0.038(2) 0.040(2) -0.011(1) 0.009(1) -0.002(1) C(14) 0.042(2) 0.037(2) 0.038(2) -0.008(1) 0.010(1) 0.002(1) C(15) 0.062(2) 0.048(2) 0.046(2) -0.004(2) 0.023(1) -0.004(1) C(16) 0.057(2) 0.044(2) 0.055(2) -0.003(2) 0.024(2) -0.004(1) C(17) 0.035(1) 0.040(2) 0.048(2) -0.008(1) 0.005(1) 0.003(1) C(18) 0.035(2) 0.049(2) 0.065(2) -0.012(1) 0.003(2) 0.000(2) C(19) 0.042(2) 0.057(2) 0.077(3) -0.007(2) -0.007(2) -0.008(2) C(20) 0.041(2) 0.033(2) 0.066(2) -0.009(1) 0.010(2) 0.004(1) C(21) 0.093(3) 0.053(2) 0.072(2) -0.017(2) 0.040(2) 0.006(2) C(22) 0.050(2) 0.032(2) 0.094(3) -0.002(1) 0.022(2) 0.016(2) C(23) 0.057(2) 0.030(2) 0.087(3) -0.006(1) 0.027(1) 0.007(1) C(24) 0.060(2) 0.039(2) 0.041(2) -0.009(1) 0.008(2) 0.003(1) C(25) 0.065(2) 0.040(2) 0.051(2) -0.017(1) 0.011(2) 0.007(1) C(26) 0.054(2) 0.042(2) 0.056(2) -0.003(1) 0.002(2) 0.000(1) C(27) 0.056(2) 0.041(2) 0.052(2) 0.004(1) 0.006(2) -0.010(1) C(28) 0.050(2) 0.035(2) 0.044(2) 0.008(1) 0.012(1) 0.002(1) C(29) 0.067(2) 0.053(2) 0.041(2) 0.009(2) 0.023(2) 0.000(1) C(30) 0.061(2) 0.050(2) 0.036(2) 0.001(1) 0.022(1) 0.002(1) C(31) 0.039(1) 0.040(2) 0.035(1) -0.001(1) 0.014(1) 0.004(1) C(32) 0.039(1) 0.041(2) 0.031(1) -0.010(1) 0.009(1) -0.002(1) C(33) 0.043(2) 0.037(2) 0.041(2) -0.002(1) 0.010(1) 0.002(1) C(34) 0.064(2) 0.037(2) 0.033(2) -0.011(1) 0.013(1) 0.000(1) C(35) 0.054(2) 0.045(2) 0.035(2) -0.012(1) 0.015(1) -0.005(1) C(36) 0.039(1) 0.038(2) 0.033(1) -0.007(1) 0.003(1) 0.002(1) C(37) 0.036(1) 0.043(2) 0.039(2) -0.004(1) 0.011(1) -0.003(1) C(38) 0.053(2) 0.061(2) 0.041(2) 0.006(2) 0.021(1) 0.007(1) C(39) 0.053(2) 0.049(2) 0.041(2) -0.007(1) 0.011(1) 0.008(1) C(40) 0.039(2) 0.033(1) 0.040(2) -0.007(1) 0.007(1) 0.002(1) C(41) 0.043(2) 0.041(2) 0.064(2) -0.012(1) 0.001(2) 0.004(2) C(42) 0.044(2) 0.056(2) 0.065(2) -0.004(2) 0.001(2) 0.010(2) C(43) 0.038(2) 0.040(2) 0.057(2) -0.011(1) 0.004(1) -0.007(1) C(44) 0.076(2) 0.041(2) 0.065(2) -0.011(2) 0.030(2) -0.012(2) C(45) 0.051(2) 0.042(2) 0.072(3) -0.003(2) -0.006(2) -0.004(2) C(46) 0.056(2) 0.043(2) 0.067(3) -0.001(1) 0.006(2) -0.006(2) C(47) 0.127(6) 0.115(5) 0.096(5) -0.001(4) 0.017(4) 0.014(4) C(48) 0.145(4) 0.073(3) 0.151(5) 0.002(3) 0.104(3) 0.009(3) C(49) 0.107(6) 0.28(1) 0.166(9) 0.041(7) 0.019(5) 0.096(8) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F^2^ against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^, conventional R-factors (R) are calculated on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 1.5sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.04000(Fo^2^)^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3531 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.2206 _refine_ls_wR_factor_gt 0.2197 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_shift/su_max 0.1860 _refine_ls_shift/su_mean 0.0460 _refine_diff_density_min -0.34 _refine_diff_density_max 0.59 #------------------------------------------------------------------------------ _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) 1.444(5) 1_555 1_555 yes O(2) C(7) 1.427(6) 1_555 1_555 yes O(3) C(23) 1.209(6) 1_555 1_555 yes O(4) C(23) 1.334(6) 1_555 1_555 yes O(5) C(26) 1.451(6) 1_555 1_555 yes O(6) C(30) 1.438(5) 1_555 1_555 yes O(7) C(46) 1.214(6) 1_555 1_555 yes O(8) C(46) 1.337(6) 1_555 1_555 yes O(9) C(48) 1.24(1) 1_555 1_555 yes C(1) C(2) 1.540(5) 1_555 1_555 yes C(1) C(10) 1.553(6) 1_555 1_555 yes C(2) C(3) 1.509(6) 1_555 1_555 yes C(3) C(4) 1.509(6) 1_555 1_555 yes C(4) C(5) 1.537(6) 1_555 1_555 yes C(5) C(6) 1.538(7) 1_555 1_555 yes C(5) C(10) 1.537(7) 1_555 1_555 yes C(6) C(7) 1.515(6) 1_555 1_555 yes C(7) C(8) 1.546(6) 1_555 1_555 yes C(8) C(9) 1.539(5) 1_555 1_555 yes C(8) C(14) 1.509(5) 1_555 1_555 yes C(9) C(10) 1.582(5) 1_555 1_555 yes C(9) C(11) 1.532(6) 1_555 1_555 yes C(10) C(19) 1.553(6) 1_555 1_555 yes C(11) C(12) 1.521(6) 1_555 1_555 yes C(12) C(13) 1.526(5) 1_555 1_555 yes C(13) C(14) 1.550(5) 1_555 1_555 yes C(13) C(17) 1.571(5) 1_555 1_555 yes C(13) C(18) 1.536(5) 1_555 1_555 yes C(14) C(15) 1.523(5) 1_555 1_555 yes C(15) C(16) 1.532(6) 1_555 1_555 yes C(16) C(17) 1.557(6) 1_555 1_555 yes C(17) C(20) 1.535(5) 1_555 1_555 yes C(20) C(21) 1.524(7) 1_555 1_555 yes C(20) C(22) 1.548(5) 1_555 1_555 yes C(22) C(23) 1.485(6) 1_555 1_555 yes C(24) C(25) 1.534(6) 1_555 1_555 yes C(24) C(33) 1.536(5) 1_555 1_555 yes C(25) C(26) 1.512(6) 1_555 1_555 yes C(26) C(27) 1.519(7) 1_555 1_555 yes C(27) C(28) 1.529(6) 1_555 1_555 yes C(28) C(29) 1.545(6) 1_555 1_555 yes C(28) C(33) 1.563(5) 1_555 1_555 yes C(29) C(30) 1.507(6) 1_555 1_555 yes C(30) C(31) 1.533(5) 1_555 1_555 yes C(31) C(32) 1.551(4) 1_555 1_555 yes C(31) C(37) 1.537(5) 1_555 1_555 yes C(32) C(33) 1.560(5) 1_555 1_555 yes C(32) C(34) 1.566(5) 1_555 1_555 yes C(33) C(42) 1.538(6) 1_555 1_555 yes C(34) C(35) 1.533(5) 1_555 1_555 yes C(35) C(36) 1.531(5) 1_555 1_555 yes C(36) C(37) 1.531(5) 1_555 1_555 yes C(36) C(40) 1.563(5) 1_555 1_555 yes C(36) C(41) 1.545(5) 1_555 1_555 yes C(37) C(38) 1.521(6) 1_555 1_555 yes C(38) C(39) 1.552(6) 1_555 1_555 yes C(39) C(40) 1.553(5) 1_555 1_555 yes C(40) C(43) 1.541(5) 1_555 1_555 yes C(43) C(44) 1.537(7) 1_555 1_555 yes C(43) C(45) 1.528(6) 1_555 1_555 yes C(45) C(46) 1.483(6) 1_555 1_555 yes C(47) C(48) 1.51(1) 1_555 1_555 yes C(48) C(49) 1.49(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(3) O(1) H(36) 111.8(3) 1_555 1_555 1_555 no C(7) O(2) H(37) 112.8(3) 1_555 1_555 1_555 no C(23) O(4) H(38) 114.6(3) 1_555 1_555 1_555 no C(26) O(5) H(74) 109.5(3) 1_555 1_555 1_555 no C(30) O(6) H(75) 115.3(3) 1_555 1_555 1_555 no C(46) O(8) H(76) 110.1(3) 1_555 1_555 1_555 no C(2) C(1) C(10) 114.5(3) 1_555 1_555 1_555 yes C(2) C(1) H(1) 107.9(4) 1_555 1_555 1_555 no C(2) C(1) H(2) 108.9(3) 1_555 1_555 1_555 no C(10) C(1) H(1) 107.9(4) 1_555 1_555 1_555 no C(10) C(1) H(2) 109.2(4) 1_555 1_555 1_555 no H(1) C(1) H(2) 108.3(4) 1_555 1_555 1_555 no C(1) C(2) C(3) 109.9(3) 1_555 1_555 1_555 yes C(1) C(2) H(3) 108.8(4) 1_555 1_555 1_555 no C(1) C(2) H(4) 109.7(4) 1_555 1_555 1_555 no C(3) C(2) H(3) 108.7(4) 1_555 1_555 1_555 no C(3) C(2) H(4) 109.6(4) 1_555 1_555 1_555 no H(3) C(2) H(4) 110.0(4) 1_555 1_555 1_555 no O(1) C(3) C(2) 110.6(3) 1_555 1_555 1_555 yes O(1) C(3) C(4) 112.1(3) 1_555 1_555 1_555 yes O(1) C(3) H(5) 107.2(4) 1_555 1_555 1_555 no C(2) C(3) C(4) 110.4(3) 1_555 1_555 1_555 yes C(2) C(3) H(5) 108.4(4) 1_555 1_555 1_555 no C(4) C(3) H(5) 108.1(4) 1_555 1_555 1_555 no C(3) C(4) C(5) 113.6(4) 1_555 1_555 1_555 yes C(3) C(4) H(6) 108.4(4) 1_555 1_555 1_555 no C(3) C(4) H(7) 107.8(4) 1_555 1_555 1_555 no C(5) C(4) H(6) 108.8(4) 1_555 1_555 1_555 no C(5) C(4) H(7) 108.1(4) 1_555 1_555 1_555 no H(6) C(4) H(7) 110.2(4) 1_555 1_555 1_555 no C(4) C(5) C(6) 112.9(4) 1_555 1_555 1_555 yes C(4) C(5) C(10) 112.7(3) 1_555 1_555 1_555 yes C(4) C(5) H(8) 106.3(4) 1_555 1_555 1_555 no C(6) C(5) C(10) 110.7(4) 1_555 1_555 1_555 yes C(6) C(5) H(8) 107.0(4) 1_555 1_555 1_555 no C(10) C(5) H(8) 106.8(4) 1_555 1_555 1_555 no C(5) C(6) C(7) 115.4(3) 1_555 1_555 1_555 yes C(5) C(6) H(9) 108.3(5) 1_555 1_555 1_555 no C(5) C(6) H(10) 106.7(4) 1_555 1_555 1_555 no C(7) C(6) H(9) 109.5(4) 1_555 1_555 1_555 no C(7) C(6) H(10) 107.2(5) 1_555 1_555 1_555 no H(9) C(6) H(10) 109.6(4) 1_555 1_555 1_555 no O(2) C(7) C(6) 114.7(4) 1_555 1_555 1_555 yes O(2) C(7) C(8) 107.6(3) 1_555 1_555 1_555 yes O(2) C(7) H(11) 108.9(4) 1_555 1_555 1_555 no C(6) C(7) C(8) 110.3(4) 1_555 1_555 1_555 yes C(6) C(7) H(11) 107.3(4) 1_555 1_555 1_555 no C(8) C(7) H(11) 107.8(4) 1_555 1_555 1_555 no C(7) C(8) C(9) 111.1(3) 1_555 1_555 1_555 yes C(7) C(8) C(14) 112.5(3) 1_555 1_555 1_555 yes C(7) C(8) H(12) 107.1(3) 1_555 1_555 1_555 no C(9) C(8) C(14) 110.3(3) 1_555 1_555 1_555 yes C(9) C(8) H(12) 107.1(3) 1_555 1_555 1_555 no C(14) C(8) H(12) 108.5(3) 1_555 1_555 1_555 no C(8) C(9) C(10) 111.4(3) 1_555 1_555 1_555 yes C(8) C(9) C(11) 113.3(3) 1_555 1_555 1_555 yes C(8) C(9) H(13) 107.2(3) 1_555 1_555 1_555 no C(10) C(9) C(11) 114.3(3) 1_555 1_555 1_555 yes C(10) C(9) H(13) 105.0(4) 1_555 1_555 1_555 no C(11) C(9) H(13) 104.9(3) 1_555 1_555 1_555 no C(1) C(10) C(5) 109.2(3) 1_555 1_555 1_555 yes C(1) C(10) C(9) 111.9(3) 1_555 1_555 1_555 yes C(1) C(10) C(19) 104.9(3) 1_555 1_555 1_555 yes C(5) C(10) C(9) 110.0(3) 1_555 1_555 1_555 yes C(5) C(10) C(19) 110.9(4) 1_555 1_555 1_555 yes C(9) C(10) C(19) 109.9(3) 1_555 1_555 1_555 yes C(9) C(11) C(12) 114.4(3) 1_555 1_555 1_555 yes C(9) C(11) H(14) 108.5(4) 1_555 1_555 1_555 no C(9) C(11) H(15) 107.8(3) 1_555 1_555 1_555 no C(12) C(11) H(14) 109.1(3) 1_555 1_555 1_555 no C(12) C(11) H(15) 108.5(4) 1_555 1_555 1_555 no H(14) C(11) H(15) 108.4(4) 1_555 1_555 1_555 no C(11) C(12) C(13) 112.2(3) 1_555 1_555 1_555 yes C(11) C(12) H(16) 108.5(4) 1_555 1_555 1_555 no C(11) C(12) H(17) 108.0(4) 1_555 1_555 1_555 no C(13) C(12) H(16) 109.4(4) 1_555 1_555 1_555 no C(13) C(12) H(17) 109.2(4) 1_555 1_555 1_555 no H(16) C(12) H(17) 109.5(4) 1_555 1_555 1_555 no C(12) C(13) C(14) 106.3(3) 1_555 1_555 1_555 yes C(12) C(13) C(17) 117.7(3) 1_555 1_555 1_555 yes C(12) C(13) C(18) 110.4(3) 1_555 1_555 1_555 yes C(14) C(13) C(17) 100.6(3) 1_555 1_555 1_555 yes C(14) C(13) C(18) 111.7(3) 1_555 1_555 1_555 yes C(17) C(13) C(18) 109.7(3) 1_555 1_555 1_555 yes C(8) C(14) C(13) 113.4(3) 1_555 1_555 1_555 yes C(8) C(14) C(15) 117.6(3) 1_555 1_555 1_555 yes C(8) C(14) H(18) 105.5(3) 1_555 1_555 1_555 no C(13) C(14) C(15) 104.7(3) 1_555 1_555 1_555 yes C(13) C(14) H(18) 106.5(3) 1_555 1_555 1_555 no C(15) C(14) H(18) 108.6(3) 1_555 1_555 1_555 no C(14) C(15) C(16) 104.1(3) 1_555 1_555 1_555 yes C(14) C(15) H(19) 110.2(4) 1_555 1_555 1_555 no C(14) C(15) H(20) 110.0(4) 1_555 1_555 1_555 no C(16) C(15) H(19) 111.0(4) 1_555 1_555 1_555 no C(16) C(15) H(20) 111.0(4) 1_555 1_555 1_555 no H(19) C(15) H(20) 110.3(4) 1_555 1_555 1_555 no C(15) C(16) C(17) 108.4(3) 1_555 1_555 1_555 yes C(15) C(16) H(21) 109.5(4) 1_555 1_555 1_555 no C(15) C(16) H(22) 109.6(4) 1_555 1_555 1_555 no C(17) C(16) H(21) 109.5(4) 1_555 1_555 1_555 no C(17) C(16) H(22) 108.9(4) 1_555 1_555 1_555 no H(21) C(16) H(22) 110.8(4) 1_555 1_555 1_555 no C(13) C(17) C(16) 102.1(3) 1_555 1_555 1_555 yes C(13) C(17) C(20) 117.7(3) 1_555 1_555 1_555 yes C(13) C(17) H(23) 105.4(3) 1_555 1_555 1_555 no C(16) C(17) C(20) 114.8(3) 1_555 1_555 1_555 yes C(16) C(17) H(23) 107.7(4) 1_555 1_555 1_555 no C(20) C(17) H(23) 108.3(3) 1_555 1_555 1_555 no C(13) C(18) H(24) 109.6(4) 1_555 1_555 1_555 no C(13) C(18) H(25) 109.3(4) 1_555 1_555 1_555 no C(13) C(18) H(26) 109.6(4) 1_555 1_555 1_555 no H(24) C(18) H(25) 110.0(4) 1_555 1_555 1_555 no H(24) C(18) H(26) 109.3(4) 1_555 1_555 1_555 no H(25) C(18) H(26) 109.0(4) 1_555 1_555 1_555 no C(10) C(19) H(27) 109.2(4) 1_555 1_555 1_555 no C(10) C(19) H(28) 109.1(4) 1_555 1_555 1_555 no C(10) C(19) H(29) 110.5(4) 1_555 1_555 1_555 no H(27) C(19) H(28) 109.0(5) 1_555 1_555 1_555 no H(27) C(19) H(29) 109.7(5) 1_555 1_555 1_555 no H(28) C(19) H(29) 109.4(5) 1_555 1_555 1_555 no C(17) C(20) C(21) 113.4(4) 1_555 1_555 1_555 yes C(17) C(20) C(22) 111.1(3) 1_555 1_555 1_555 yes C(17) C(20) H(30) 107.3(3) 1_555 1_555 1_555 no C(21) C(20) C(22) 108.8(4) 1_555 1_555 1_555 yes C(21) C(20) H(30) 107.3(4) 1_555 1_555 1_555 no C(22) C(20) H(30) 108.8(4) 1_555 1_555 1_555 no C(20) C(21) H(31) 109.9(5) 1_555 1_555 1_555 no C(20) C(21) H(32) 109.7(4) 1_555 1_555 1_555 no C(20) C(21) H(33) 110.9(5) 1_555 1_555 1_555 no H(31) C(21) H(32) 107.5(5) 1_555 1_555 1_555 no H(31) C(21) H(33) 110.1(5) 1_555 1_555 1_555 no H(32) C(21) H(33) 108.8(5) 1_555 1_555 1_555 no C(20) C(22) C(23) 112.5(4) 1_555 1_555 1_555 yes C(20) C(22) H(34) 106.9(4) 1_555 1_555 1_555 no C(20) C(22) H(35) 106.7(4) 1_555 1_555 1_555 no C(23) C(22) H(34) 110.0(4) 1_555 1_555 1_555 no C(23) C(22) H(35) 110.3(4) 1_555 1_555 1_555 no H(34) C(22) H(35) 110.4(5) 1_555 1_555 1_555 no O(3) C(23) O(4) 121.4(4) 1_555 1_555 1_555 yes O(3) C(23) C(22) 125.2(4) 1_555 1_555 1_555 yes O(4) C(23) C(22) 113.4(4) 1_555 1_555 1_555 yes C(25) C(24) C(33) 115.4(3) 1_555 1_555 1_555 yes C(25) C(24) H(39) 108.0(4) 1_555 1_555 1_555 no C(25) C(24) H(40) 108.9(4) 1_555 1_555 1_555 no C(33) C(24) H(39) 107.1(3) 1_555 1_555 1_555 no C(33) C(24) H(40) 107.9(4) 1_555 1_555 1_555 no H(39) C(24) H(40) 109.6(4) 1_555 1_555 1_555 no C(24) C(25) C(26) 109.3(4) 1_555 1_555 1_555 yes C(24) C(25) H(41) 110.2(4) 1_555 1_555 1_555 no C(24) C(25) H(42) 109.0(4) 1_555 1_555 1_555 no C(26) C(25) H(41) 110.2(4) 1_555 1_555 1_555 no C(26) C(25) H(42) 109.2(4) 1_555 1_555 1_555 no H(41) C(25) H(42) 108.8(5) 1_555 1_555 1_555 no O(5) C(26) C(25) 110.3(4) 1_555 1_555 1_555 yes O(5) C(26) C(27) 111.4(3) 1_555 1_555 1_555 yes O(5) C(26) H(43) 106.7(4) 1_555 1_555 1_555 no C(25) C(26) C(27) 112.4(4) 1_555 1_555 1_555 yes C(25) C(26) H(43) 107.7(4) 1_555 1_555 1_555 no C(27) C(26) H(43) 108.1(4) 1_555 1_555 1_555 no C(26) C(27) C(28) 112.3(3) 1_555 1_555 1_555 yes C(26) C(27) H(44) 108.0(4) 1_555 1_555 1_555 no C(26) C(27) H(45) 108.7(4) 1_555 1_555 1_555 no C(28) C(27) H(44) 108.5(4) 1_555 1_555 1_555 no C(28) C(27) H(45) 109.7(4) 1_555 1_555 1_555 no H(44) C(27) H(45) 109.7(4) 1_555 1_555 1_555 no C(27) C(28) C(29) 111.9(3) 1_555 1_555 1_555 yes C(27) C(28) C(33) 112.8(3) 1_555 1_555 1_555 yes C(27) C(28) H(46) 107.3(4) 1_555 1_555 1_555 no C(29) C(28) C(33) 111.2(3) 1_555 1_555 1_555 yes C(29) C(28) H(46) 107.0(4) 1_555 1_555 1_555 no C(33) C(28) H(46) 106.3(3) 1_555 1_555 1_555 no C(28) C(29) C(30) 115.4(3) 1_555 1_555 1_555 yes C(28) C(29) H(47) 107.8(4) 1_555 1_555 1_555 no C(28) C(29) H(48) 108.3(4) 1_555 1_555 1_555 no C(30) C(29) H(47) 107.2(4) 1_555 1_555 1_555 no C(30) C(29) H(48) 108.3(4) 1_555 1_555 1_555 no H(47) C(29) H(48) 109.7(4) 1_555 1_555 1_555 no O(6) C(30) C(29) 112.7(4) 1_555 1_555 1_555 yes O(6) C(30) C(31) 109.2(3) 1_555 1_555 1_555 yes O(6) C(30) H(49) 108.3(3) 1_555 1_555 1_555 no C(29) C(30) C(31) 112.1(3) 1_555 1_555 1_555 yes C(29) C(30) H(49) 108.0(4) 1_555 1_555 1_555 no C(31) C(30) H(49) 106.3(4) 1_555 1_555 1_555 no C(30) C(31) C(32) 111.1(3) 1_555 1_555 1_555 yes C(30) C(31) C(37) 113.9(3) 1_555 1_555 1_555 yes C(30) C(31) H(50) 108.6(3) 1_555 1_555 1_555 no C(32) C(31) C(37) 110.1(3) 1_555 1_555 1_555 yes C(32) C(31) H(50) 106.9(3) 1_555 1_555 1_555 no C(37) C(31) H(50) 105.9(3) 1_555 1_555 1_555 no C(31) C(32) C(33) 111.7(3) 1_555 1_555 1_555 yes C(31) C(32) C(34) 112.0(3) 1_555 1_555 1_555 yes C(31) C(32) H(51) 107.2(3) 1_555 1_555 1_555 no C(33) C(32) C(34) 112.9(3) 1_555 1_555 1_555 yes C(33) C(32) H(51) 107.3(3) 1_555 1_555 1_555 no C(34) C(32) H(51) 105.2(3) 1_555 1_555 1_555 no C(24) C(33) C(28) 108.5(3) 1_555 1_555 1_555 yes C(24) C(33) C(32) 112.8(3) 1_555 1_555 1_555 yes C(24) C(33) C(42) 104.9(3) 1_555 1_555 1_555 yes C(28) C(33) C(32) 108.4(3) 1_555 1_555 1_555 yes C(28) C(33) C(42) 109.8(3) 1_555 1_555 1_555 yes C(32) C(33) C(42) 112.2(3) 1_555 1_555 1_555 yes C(32) C(34) C(35) 114.7(3) 1_555 1_555 1_555 yes C(32) C(34) H(52) 109.0(3) 1_555 1_555 1_555 no C(32) C(34) H(53) 108.1(4) 1_555 1_555 1_555 no C(35) C(34) H(52) 108.1(4) 1_555 1_555 1_555 no C(35) C(34) H(53) 107.5(3) 1_555 1_555 1_555 no H(52) C(34) H(53) 109.4(4) 1_555 1_555 1_555 no C(34) C(35) C(36) 111.8(3) 1_555 1_555 1_555 yes C(34) C(35) H(54) 108.9(4) 1_555 1_555 1_555 no C(34) C(35) H(55) 109.0(3) 1_555 1_555 1_555 no C(36) C(35) H(54) 109.1(3) 1_555 1_555 1_555 no C(36) C(35) H(55) 109.1(4) 1_555 1_555 1_555 no H(54) C(35) H(55) 108.8(4) 1_555 1_555 1_555 no C(35) C(36) C(37) 107.0(3) 1_555 1_555 1_555 yes C(35) C(36) C(40) 116.4(3) 1_555 1_555 1_555 yes C(35) C(36) C(41) 111.3(3) 1_555 1_555 1_555 yes C(37) C(36) C(40) 100.0(3) 1_555 1_555 1_555 yes C(37) C(36) C(41) 112.9(3) 1_555 1_555 1_555 yes C(40) C(36) C(41) 108.9(3) 1_555 1_555 1_555 yes C(31) C(37) C(36) 113.1(3) 1_555 1_555 1_555 yes C(31) C(37) C(38) 118.1(3) 1_555 1_555 1_555 yes C(31) C(37) H(56) 106.7(3) 1_555 1_555 1_555 no C(36) C(37) C(38) 105.9(3) 1_555 1_555 1_555 yes C(36) C(37) H(56) 106.3(3) 1_555 1_555 1_555 no C(38) C(37) H(56) 106.0(3) 1_555 1_555 1_555 no C(37) C(38) C(39) 104.3(3) 1_555 1_555 1_555 yes C(37) C(38) H(57) 110.9(4) 1_555 1_555 1_555 no C(37) C(38) H(58) 110.3(3) 1_555 1_555 1_555 no C(39) C(38) H(57) 110.4(4) 1_555 1_555 1_555 no C(39) C(38) H(58) 109.9(4) 1_555 1_555 1_555 no H(57) C(38) H(58) 111.0(4) 1_555 1_555 1_555 no C(38) C(39) C(40) 106.4(3) 1_555 1_555 1_555 yes C(38) C(39) H(59) 111.4(4) 1_555 1_555 1_555 no C(38) C(39) H(60) 110.4(4) 1_555 1_555 1_555 no C(40) C(39) H(59) 110.3(4) 1_555 1_555 1_555 no C(40) C(39) H(60) 109.3(4) 1_555 1_555 1_555 no H(59) C(39) H(60) 109.0(4) 1_555 1_555 1_555 no C(36) C(40) C(39) 103.9(3) 1_555 1_555 1_555 yes C(36) C(40) C(43) 117.7(3) 1_555 1_555 1_555 yes C(36) C(40) H(61) 108.1(3) 1_555 1_555 1_555 no C(39) C(40) C(43) 112.8(3) 1_555 1_555 1_555 yes C(39) C(40) H(61) 107.5(3) 1_555 1_555 1_555 no C(43) C(40) H(61) 106.4(3) 1_555 1_555 1_555 no C(36) C(41) H(62) 109.5(4) 1_555 1_555 1_555 no C(36) C(41) H(63) 108.5(4) 1_555 1_555 1_555 no C(36) C(41) H(64) 108.8(4) 1_555 1_555 1_555 no H(62) C(41) H(63) 109.5(4) 1_555 1_555 1_555 no H(62) C(41) H(64) 110.6(4) 1_555 1_555 1_555 no H(63) C(41) H(64) 109.8(5) 1_555 1_555 1_555 no C(33) C(42) H(65) 108.9(4) 1_555 1_555 1_555 no C(33) C(42) H(66) 109.5(4) 1_555 1_555 1_555 no C(33) C(42) H(67) 111.2(4) 1_555 1_555 1_555 no H(65) C(42) H(66) 107.5(5) 1_555 1_555 1_555 no H(65) C(42) H(67) 109.1(5) 1_555 1_555 1_555 no H(66) C(42) H(67) 110.6(5) 1_555 1_555 1_555 no C(40) C(43) C(44) 114.2(3) 1_555 1_555 1_555 yes C(40) C(43) C(45) 111.3(3) 1_555 1_555 1_555 yes C(40) C(43) H(68) 108.3(3) 1_555 1_555 1_555 no C(44) C(43) C(45) 108.8(4) 1_555 1_555 1_555 yes C(44) C(43) H(68) 107.4(4) 1_555 1_555 1_555 no C(45) C(43) H(68) 106.5(4) 1_555 1_555 1_555 no C(43) C(44) H(69) 109.7(4) 1_555 1_555 1_555 no C(43) C(44) H(70) 108.9(4) 1_555 1_555 1_555 no C(43) C(44) H(71) 109.6(4) 1_555 1_555 1_555 no H(69) C(44) H(70) 110.2(5) 1_555 1_555 1_555 no H(69) C(44) H(71) 110.2(5) 1_555 1_555 1_555 no H(70) C(44) H(71) 108.3(4) 1_555 1_555 1_555 no C(43) C(45) C(46) 113.9(4) 1_555 1_555 1_555 yes C(43) C(45) H(72) 109.1(5) 1_555 1_555 1_555 no C(43) C(45) H(73) 109.2(4) 1_555 1_555 1_555 no C(46) C(45) H(72) 107.9(4) 1_555 1_555 1_555 no C(46) C(45) H(73) 107.0(5) 1_555 1_555 1_555 no H(72) C(45) H(73) 109.6(4) 1_555 1_555 1_555 no O(7) C(46) O(8) 119.5(4) 1_555 1_555 1_555 yes O(7) C(46) C(45) 125.5(4) 1_555 1_555 1_555 yes O(8) C(46) C(45) 114.9(4) 1_555 1_555 1_555 yes C(48) C(47) H(77) 109.9(9) 1_555 1_555 1_555 no C(48) C(47) H(78) 108.3(8) 1_555 1_555 1_555 no C(48) C(47) H(79) 112.7(9) 1_555 1_555 1_555 no H(77) C(47) H(78) 106(1) 1_555 1_555 1_555 no H(77) C(47) H(79) 111.1(9) 1_555 1_555 1_555 no H(78) C(47) H(79) 108.6(10) 1_555 1_555 1_555 no O(9) C(48) C(47) 124.1(9) 1_555 1_555 1_555 yes O(9) C(48) C(49) 124.1(10) 1_555 1_555 1_555 yes C(47) C(48) C(49) 111.7(9) 1_555 1_555 1_555 yes C(48) C(49) H(80) 100(1) 1_555 1_555 1_555 no C(48) C(49) H(81) 109.4(10) 1_555 1_555 1_555 no C(48) C(49) H(82) 103(1) 1_555 1_555 1_555 no H(80) C(49) H(81) 115(1) 1_555 1_555 1_555 no H(80) C(49) H(82) 105(1) 1_555 1_555 1_555 no H(81) C(49) H(82) 120(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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) 178.7(3) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) -179.5(3) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(6) C(5) -68.4(6) 1_555 1_555 1_555 1_555 yes O(2) C(7) C(8) C(9) 71.8(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(23) C(22) C(20) -123.9(5) 1_555 1_555 1_555 1_555 yes O(4) C(23) C(22) C(20) 56.2(6) 1_555 1_555 1_555 1_555 yes O(5) C(26) C(25) C(24) -180.0(3) 1_555 1_555 1_555 1_555 yes O(5) C(26) C(27) C(28) -179.9(3) 1_555 1_555 1_555 1_555 yes O(6) C(30) C(29) C(28) -73.6(4) 1_555 1_555 1_555 1_555 yes O(6) C(30) C(31) C(32) 73.8(4) 1_555 1_555 1_555 1_555 yes O(6) C(30) C(31) C(37) -51.2(4) 1_555 1_555 1_555 1_555 yes O(7) C(46) C(45) C(43) -138.5(6) 1_555 1_555 1_555 1_555 yes O(8) C(46) C(45) C(43) 45.1(6) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -56.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 48.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 176.3(3) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -178.2(3) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 51.8(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -51.6(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 70.4(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -170.6(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 56.8(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 56.4(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -179.9(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.5(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 73.7(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -74.4(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 163.8(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 53.3(6) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -56.7(4) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 173.3(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 53.2(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -68.6(4) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -54.1(4) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -178.3(3) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -53.8(6) 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) -172.4(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -177.9(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -55.3(4) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 65.7(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 45.3(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -62.5(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 174.3(3) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 58.0(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -159.1(3) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 57.5(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) 180.0 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -52.0(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -177.5(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 174.4(3) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -47.0(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -64.3(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 57.7(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 169.4(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -63.6(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 168.1(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -153.9(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 79.4(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -32.2(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 20.6(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -65.6(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 171.5(3) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -39.0(3) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -165.7(3) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 6.7(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 44.9(3) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -71.5(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 149.1(3) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 78.8(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 174.1(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 51.2(4) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -172.7(4) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -47.9(4) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 61.8(5) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) -55.0(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(27) 50.5(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(29) 177.1(3) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(31) -178.8(3) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(34) 53.9(4) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(28) -52.9(4) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(32) 67.3(4) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(42) -170.3(3) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 55.7(4) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(24) C(33) 55.7(4) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) -179.6(3) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(33) -53.4(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 75.2(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(32) -72.4(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(42) 164.7(3) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 50.0(5) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(31) -58.6(4) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(34) 174.1(3) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(32) 54.2(4) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(42) -68.7(4) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -51.8(4) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(37) -176.8(3) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(28) C(33) -51.9(5) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) 57.8(4) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(34) -174.4(3) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(36) -175.5(3) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(38) -51.1(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(42) 62.9(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(34) C(35) 45.4(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(35) -63.6(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(40) 174.7(3) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(41) 59.1(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(38) C(39) -158.7(3) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(36) 59.0(4) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(38) -176.7(3) 1_555 1_555 1_555 1_555 yes C(32) C(34) C(35) C(36) -51.5(4) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(37) -175.1(3) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(34) C(35) 172.5(3) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(31) C(37) -47.4(4) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(33) C(42) -64.4(4) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) 58.1(4) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(40) 168.8(3) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(41) -65.7(4) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 165.6(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(39) -154.3(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(43) 80.2(4) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) -30.8(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(39) C(38) 21.9(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(44) -63.6(4) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(45) 172.8(4) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(39) -39.5(3) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(43) -165.1(3) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) 4.9(4) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(40) 43.9(3) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(41) -71.7(4) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(43) 150.4(3) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(36) C(41) 79.0(4) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(44) 175.4(3) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(45) 51.7(4) 1_555 1_555 1_555 1_555 yes C(40) C(43) C(45) C(46) -165.0(4) 1_555 1_555 1_555 1_555 yes C(41) C(36) C(40) C(43) -46.5(4) 1_555 1_555 1_555 1_555 yes C(44) C(43) C(45) C(46) 68.2(5) 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(4) 2.622(5) 1_555 1_565 ? O(1) O(7) 2.725(4) 1_555 1_655 ? O(1) O(3) 3.268(5) 1_555 1_565 ? O(1) C(23) 3.361(5) 1_555 1_565 ? O(2) O(9) 2.807(7) 1_555 1_555 ? O(2) C(45) 3.464(6) 1_555 1_655 ? O(3) O(5) 2.770(5) 1_555 1_655 ? O(3) C(26) 3.510(6) 1_555 1_655 ? O(3) C(47) 3.58(1) 1_555 1_546 ? O(5) O(8) 2.605(4) 1_555 1_545 ? O(5) O(7) 3.180(5) 1_555 1_545 ? O(5) C(46) 3.326(6) 1_555 1_545 ? O(6) C(22) 3.356(6) 1_555 1_455 ? O(7) O(9) 3.35(1) 1_555 1_456 ? O(7) C(3) 3.493(6) 1_555 1_455 ? O(7) C(48) 3.54(1) 1_555 1_456 ? O(7) C(47) 3.58(1) 1_555 1_456 ? O(9) C(4) 3.454(9) 1_555 1_555 ? O(9) C(44) 3.599(8) 1_555 1_654 ? #------------------------------------------------------------------------------ _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 565-8710 Japan ; _publ_contact_author_email ' miyata@ap.chem.eng.osaka-u.ac.jp ' _publ_contact_author_fax ' +81-6-879-7404 ' _publ_contact_author_phone ' +81-6-879-7406 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chem.Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; A Robust Structural Motif in Inclusion Crystals of Norbile Acids ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Michihiro Sugahara ' ? ; Material and Life Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-8710 Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_Norl #------------------------------------------------------------------------------ _audit_creation_date 'Sat Dec 26 17:46:50 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 783.18 _chemical_formula_analytical ? _chemical_formula_sum 'C49 H82 O7 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.466(4) _cell_length_b 15.243(2) _cell_length_c 7.555(3) _cell_angle_alpha 92.36(2) _cell_angle_beta 103.08(3) _cell_angle_gamma 80.78(2) _cell_volume 1158.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 210.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.350 _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432.00 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 210.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku RAXIS-IV' _diffrn_detector_area_resol_mean 0.010000 _diffrn_mesured_fraction_theta_max ? _diffrn_reflns_theta_full ? _diffrn_reflns_number 3462 _reflns_number_total 3462 _reflns_number_gt 3260 _reflns_observed_expression >1.5sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.020 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O -1.2578(4) -0.9977(3) 0.2566(8) 0.094(1) Uani 1.00 d ... O(2) O -1.4868(4) -0.1199(3) 0.1185(8) 0.092(1) Uani 1.00 d ... O(3) O -1.2683(4) -0.1640(2) 0.1709(7) 0.081(1) Uani 1.00 d ... O(4) O -0.7048(4) -0.0004(2) -0.0232(7) 0.076(1) Uani 1.00 d ... O(5) O -0.4737(5) -0.8710(3) 0.1042(8) 0.088(1) Uani 1.00 d ... O(6) O -0.6562(4) -0.8463(2) -0.1105(6) 0.069(1) Uani 1.00 d ... O(7) O -0.398(2) -0.052(1) 0.677(3) 0.2925 Uiso 1.00 d ... C(1) C -1.0303(5) -0.8415(3) 0.5000(6) 0.051(1) Uani 1.00 d ... C(2) C -1.1553(6) -0.8866(3) 0.4515(8) 0.063(1) Uani 1.00 d ... C(3) C -1.1453(6) -0.9523(3) 0.3029(8) 0.065(1) Uani 1.00 d ... C(4) C -1.1207(5) -0.9065(3) 0.1387(7) 0.061(1) Uani 1.00 d ... C(5) C -0.9993(5) -0.8579(3) 0.1828(6) 0.054(1) Uani 1.00 d ... C(6) C -0.9873(7) -0.8132(4) 0.0086(7) 0.079(2) Uani 1.00 d ... C(7) C -1.0924(6) -0.7321(4) -0.0487(7) 0.070(1) Uani 1.00 d ... C(8) C -1.0915(4) -0.6647(3) 0.1103(6) 0.0480(10) Uani 1.00 d ... C(9) C -1.1129(4) -0.7097(3) 0.2774(5) 0.0366(8) Uani 1.00 d ... C(10) C -1.0065(4) -0.7914(3) 0.3429(6) 0.0450(10) Uani 1.00 d ... C(11) C -1.1343(5) -0.6423(3) 0.4306(6) 0.050(1) Uani 1.00 d ... C(12) C -1.2311(5) -0.5555(3) 0.3664(6) 0.048(1) Uani 1.00 d ... C(13) C -1.1947(4) -0.5125(3) 0.2099(6) 0.0384(8) Uani 1.00 d ... C(14) C -1.1987(4) -0.5827(3) 0.0538(5) 0.0402(9) Uani 1.00 d ... C(15) C -1.1982(5) -0.5314(3) -0.1144(6) 0.057(1) Uani 1.00 d ... C(16) C -1.2766(5) -0.4381(3) -0.0865(6) 0.0487(10) Uani 1.00 d ... C(17) C -1.3034(4) -0.4363(3) 0.1043(6) 0.0395(8) Uani 1.00 d ... C(18) C -1.0624(4) -0.4794(3) 0.2702(8) 0.059(1) Uani 1.00 d ... C(19) C -0.8666(5) -0.7626(4) 0.4113(9) 0.069(1) Uani 1.00 d ... C(20) C -1.3081(4) -0.3425(3) 0.1943(7) 0.0484(10) Uani 1.00 d ... C(21) C -1.3491(6) -0.3384(4) 0.3759(8) 0.068(1) Uani 1.00 d ... C(22) C -1.4057(6) -0.2731(3) 0.0631(8) 0.064(1) Uani 1.00 d ... C(23) C -1.3883(5) -0.1777(3) 0.1213(7) 0.057(1) Uani 1.00 d ... C(24) C -0.9628(4) -0.1533(3) -0.0710(7) 0.050(1) Uani 1.00 d ... C(25) C -0.8474(5) -0.1057(3) 0.0242(6) 0.051(1) Uani 1.00 d ... C(26) C -0.8088(4) -0.0482(3) -0.1103(7) 0.053(1) Uani 1.00 d ... C(27) C -0.7789(5) -0.1030(3) -0.2724(7) 0.059(1) Uani 1.00 d ... C(28) C -0.8911(6) -0.1549(3) -0.3636(6) 0.060(1) Uani 1.00 d ... C(29) C -0.8574(8) -0.2100(4) -0.5289(7) 0.080(2) Uani 1.00 d ... C(30) C -0.7469(6) -0.2901(3) -0.4648(6) 0.065(1) Uani 1.00 d ... C(31) C -0.7948(5) -0.3490(3) -0.3414(6) 0.047(1) Uani 1.00 d ... C(32) C -0.8266(4) -0.2949(3) -0.1754(6) 0.0419(9) Uani 1.00 d ... C(33) C -0.9367(4) -0.2131(3) -0.2331(7) 0.0480(10) Uani 1.00 d ... C(34) C -0.8546(5) -0.3526(3) -0.0302(6) 0.050(1) Uani 1.00 d ... C(35) C -0.7539(5) -0.4381(3) 0.0186(6) 0.0455(10) Uani 1.00 d ... C(36) C -0.7360(4) -0.4925(3) -0.1536(5) 0.0383(9) Uani 1.00 d ... C(37) C -0.6896(4) -0.4314(3) -0.2780(6) 0.0424(9) Uani 1.00 d ... C(38) C -0.6441(6) -0.4946(3) -0.4224(6) 0.058(1) Uani 1.00 d ... C(39) C -0.5866(5) -0.5833(3) -0.3240(7) 0.053(1) Uani 1.00 d ... C(40) C -0.6171(4) -0.5726(3) -0.1284(6) 0.0411(9) Uani 1.00 d ... C(41) C -0.8624(5) -0.5289(3) -0.2457(8) 0.057(1) Uani 1.00 d ... C(42) C -1.0677(6) -0.2398(4) -0.3274(9) 0.076(2) Uani 1.00 d ... C(43) C -0.6364(4) -0.6598(3) -0.0510(7) 0.0467(10) Uani 1.00 d ... C(44) C -0.6522(7) -0.6518(3) 0.1449(8) 0.070(1) Uani 1.00 d ... C(45) C -0.5205(4) -0.7343(3) -0.0593(8) 0.058(1) Uani 1.00 d ... C(46) C -0.5459(5) -0.8232(3) -0.0133(8) 0.060(1) Uani 1.00 d ... C(47) C -0.382(3) 0.106(2) 0.722(4) 0.0760 Uiso 1.00 d ... C(48) C -0.436(2) 0.026(1) 0.638(3) 0.2925 Uiso 1.00 d ... C(49) C -0.546(2) 0.052(1) 0.491(3) 0.2925 Uiso 1.00 d ... H(1) H -0.9550 -0.8861 0.5392 0.0617 Uiso 1.00 calc ... H(2) H -1.0388 -0.8010 0.5970 0.0617 Uiso 1.00 calc ... H(3) H -1.2295 -0.8431 0.4168 0.0766 Uiso 1.00 calc ... H(4) H -1.1606 -0.9169 0.5575 0.0766 Uiso 1.00 calc ... H(5) H -1.0691 -0.9961 0.3440 0.0783 Uiso 1.00 calc ... H(6) H -1.1076 -0.9507 0.0487 0.0754 Uiso 1.00 calc ... H(7) H -1.1969 -0.8647 0.0918 0.0754 Uiso 1.00 calc ... H(8) H -0.9226 -0.9013 0.2184 0.0673 Uiso 1.00 calc ... H(9) H -0.9964 -0.8562 -0.0869 0.0941 Uiso 1.00 calc ... H(10) H -0.9032 -0.7958 0.0297 0.0941 Uiso 1.00 calc ... H(11) H -1.0755 -0.7052 -0.1503 0.0835 Uiso 1.00 calc ... H(12) H -1.1787 -0.7501 -0.0832 0.0835 Uiso 1.00 calc ... H(13) H -1.0069 -0.6455 0.1397 0.0580 Uiso 1.00 calc ... H(14) H -1.1944 -0.7322 0.2381 0.0461 Uiso 1.00 calc ... H(15) H -1.0500 -0.6261 0.4877 0.0609 Uiso 1.00 calc ... H(16) H -1.1671 -0.6705 0.5166 0.0609 Uiso 1.00 calc ... H(17) H -1.3188 -0.5697 0.3285 0.0587 Uiso 1.00 calc ... H(18) H -1.2285 -0.5149 0.4656 0.0587 Uiso 1.00 calc ... H(19) H -1.2827 -0.6024 0.0327 0.0504 Uiso 1.00 calc ... H(20) H -1.2391 -0.5592 -0.2217 0.0695 Uiso 1.00 calc ... H(21) H -1.1087 -0.5269 -0.1201 0.0695 Uiso 1.00 calc ... H(22) H -1.2258 -0.3931 -0.0979 0.0613 Uiso 1.00 calc ... H(23) H -1.3579 -0.4291 -0.1754 0.0613 Uiso 1.00 calc ... H(24) H -1.3884 -0.4539 0.0944 0.0504 Uiso 1.00 calc ... H(25) H -1.0647 -0.4386 0.3675 0.0721 Uiso 1.00 calc ... H(26) H -1.0425 -0.4512 0.1713 0.0721 Uiso 1.00 calc ... H(27) H -0.9936 -0.5288 0.3090 0.0721 Uiso 1.00 calc ... H(28) H -0.8641 -0.7305 0.5220 0.0877 Uiso 1.00 calc ... H(29) H -0.8503 -0.7257 0.3226 0.0877 Uiso 1.00 calc ... H(30) H -0.8008 -0.8139 0.4297 0.0877 Uiso 1.00 calc ... H(31) H -1.2215 -0.3269 0.2133 0.0595 Uiso 1.00 calc ... H(32) H -1.2778 -0.3660 0.4667 0.0843 Uiso 1.00 calc ... H(33) H -1.4240 -0.3677 0.3657 0.0843 Uiso 1.00 calc ... H(34) H -1.3721 -0.2777 0.4086 0.0843 Uiso 1.00 calc ... H(35) H -1.389(2) -0.283(2) -0.053(4) 0.0757 Uiso 1.00 calc ... H(36) H -1.492(2) -0.281(2) 0.066(4) 0.0757 Uiso 1.00 calc ... H(37) H -1.3344 -0.9528 0.1932 0.1140 Uiso 1.00 calc ... H(38) H -1.2370 -0.1075 0.1564 0.0974 Uiso 1.00 calc ... H(39) H -0.9814 -0.1896 0.0169 0.0600 Uiso 1.00 calc ... H(40) H -1.0373 -0.1095 -0.1130 0.0600 Uiso 1.00 calc ... H(41) H -0.8731 -0.0693 0.1189 0.0613 Uiso 1.00 calc ... H(42) H -0.7729 -0.1490 0.0742 0.0613 Uiso 1.00 calc ... H(43) H -0.8841 -0.0051 -0.1558 0.0657 Uiso 1.00 calc ... H(44) H -0.7632 -0.0639 -0.3590 0.0742 Uiso 1.00 calc ... H(45) H -0.6981 -0.1439 -0.2318 0.0742 Uiso 1.00 calc ... H(46) H -0.9664 -0.1115 -0.4102 0.0731 Uiso 1.00 calc ... H(47) H -0.9367 -0.2319 -0.5958 0.0947 Uiso 1.00 calc ... H(48) H -0.8307 -0.1732 -0.6073 0.0947 Uiso 1.00 calc ... H(49) H -0.6687 -0.2689 -0.3998 0.0801 Uiso 1.00 calc ... H(50) H -0.7273 -0.3239 -0.5672 0.0801 Uiso 1.00 calc ... H(51) H -0.8730 -0.3688 -0.4076 0.0589 Uiso 1.00 calc ... H(52) H -0.7482 -0.2711 -0.1194 0.0514 Uiso 1.00 calc ... H(53) H -0.8540 -0.3181 0.0773 0.0613 Uiso 1.00 calc ... H(54) H -0.9391 -0.3696 -0.0741 0.0613 Uiso 1.00 calc ... H(55) H -0.7830 -0.4732 0.0976 0.0556 Uiso 1.00 calc ... H(56) H -0.6694 -0.4224 0.0801 0.0556 Uiso 1.00 calc ... H(57) H -0.6124 -0.4107 -0.2072 0.0519 Uiso 1.00 calc ... H(58) H -0.5784 -0.4720 -0.4685 0.0695 Uiso 1.00 calc ... H(59) H -0.7174 -0.5012 -0.5197 0.0695 Uiso 1.00 calc ... H(60) H -0.4929 -0.5962 -0.3146 0.0641 Uiso 1.00 calc ... H(61) H -0.6269 -0.6305 -0.3879 0.0641 Uiso 1.00 calc ... H(62) H -0.5426 -0.5526 -0.0500 0.0502 Uiso 1.00 calc ... H(63) H -0.935(2) -0.482(2) -0.262(4) 0.0679 Uiso 1.00 calc ... H(64) H -0.853(2) -0.554(2) -0.359(4) 0.0679 Uiso 1.00 calc ... H(65) H -0.876(2) -0.573(2) -0.170(4) 0.0679 Uiso 1.00 calc ... H(66) H -1.0553 -0.2830 -0.4199 0.0921 Uiso 1.00 calc ... H(67) H -1.1049 -0.2659 -0.2411 0.0921 Uiso 1.00 calc ... H(68) H -1.1277 -0.1897 -0.3800 0.0921 Uiso 1.00 calc ... H(69) H -0.7146 -0.6778 -0.1236 0.0581 Uiso 1.00 calc ... H(70) H -0.6458 -0.7097 0.1920 0.0834 Uiso 1.00 calc ... H(71) H -0.7368 -0.6189 0.1476 0.0834 Uiso 1.00 calc ... H(72) H -0.5846 -0.6227 0.2153 0.0834 Uiso 1.00 calc ... H(73) H -0.5050 -0.7370 -0.1789 0.0711 Uiso 1.00 calc ... H(74) H -0.4432 -0.7211 0.0244 0.0711 Uiso 1.00 calc ... H(75) H -0.6202 -0.0235 0.0618 0.0910 Uiso 1.00 calc ... H(76) H -0.6499 -0.9065 -0.0595 0.0827 Uiso 1.00 calc ... H(77) H -0.338(3) 0.104(2) 0.824(4) 0.2925 Uiso 1.00 calc ... H(78) H -0.336(3) 0.137(2) 0.633(5) 0.2925 Uiso 1.00 calc ... H(79) H -0.459(3) 0.168(1) 0.715(4) 0.2925 Uiso 1.00 calc ... H(80) H -0.562(3) 0.030(2) 0.376(3) 0.2925 Uiso 1.00 calc ... H(81) H -0.557(3) 0.128(1) 0.436(4) 0.2925 Uiso 1.00 calc ... H(82) H -0.642(2) 0.072(2) 0.516(5) 0.2925 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) 0.088(2) 0.036(2) 0.143(4) -0.023(2) -0.024(3) 0.022(2) O(2) 0.066(2) 0.037(2) 0.155(4) 0.008(1) 0.000(3) -0.001(2) O(3) 0.068(2) 0.033(2) 0.136(4) -0.020(1) 0.003(2) -0.004(2) O(4) 0.068(2) 0.030(2) 0.125(3) -0.014(1) 0.007(2) 0.004(2) O(5) 0.092(3) 0.045(2) 0.116(3) -0.006(2) 0.000(2) 0.022(2) O(6) 0.075(2) 0.036(2) 0.093(3) -0.018(1) 0.006(2) 0.007(2) C(1) 0.071(2) 0.035(2) 0.044(2) -0.005(2) 0.008(2) 0.005(2) C(2) 0.085(3) 0.035(2) 0.071(3) -0.018(2) 0.011(2) 0.009(2) C(3) 0.080(3) 0.022(2) 0.083(3) -0.005(2) -0.002(3) 0.006(2) C(4) 0.075(2) 0.029(2) 0.060(2) 0.010(2) -0.012(2) -0.010(2) C(5) 0.081(2) 0.032(2) 0.049(2) 0.001(2) 0.019(2) -0.005(2) C(6) 0.127(4) 0.053(3) 0.060(2) 0.029(3) 0.053(2) 0.015(2) C(7) 0.118(4) 0.047(2) 0.049(2) 0.018(2) 0.046(2) 0.006(2) C(8) 0.066(2) 0.033(2) 0.052(2) -0.002(2) 0.032(2) 0.008(1) C(9) 0.043(2) 0.029(2) 0.039(2) -0.008(1) 0.009(1) -0.004(1) C(10) 0.057(2) 0.032(2) 0.042(2) 0.000(2) 0.007(2) 0.002(1) C(11) 0.076(3) 0.031(2) 0.040(2) -0.005(2) 0.010(2) -0.004(1) C(12) 0.075(2) 0.026(2) 0.043(2) -0.006(2) 0.018(2) -0.005(1) C(13) 0.043(2) 0.028(2) 0.042(2) -0.011(1) 0.002(1) -0.003(1) C(14) 0.053(2) 0.031(2) 0.042(2) -0.010(1) 0.020(2) -0.005(1) C(15) 0.078(3) 0.047(2) 0.048(2) 0.009(2) 0.027(2) 0.012(2) C(16) 0.060(2) 0.042(2) 0.045(2) -0.004(2) 0.013(2) 0.014(2) C(17) 0.047(2) 0.029(2) 0.043(2) -0.012(1) 0.006(1) 0.000(1) C(18) 0.048(2) 0.037(2) 0.084(3) -0.014(2) -0.010(2) 0.013(2) C(19) 0.065(2) 0.050(3) 0.089(4) -0.015(2) 0.003(3) 0.009(3) C(20) 0.048(2) 0.027(2) 0.069(2) -0.011(2) 0.008(2) -0.004(2) C(21) 0.098(4) 0.041(3) 0.062(2) -0.009(2) 0.017(2) -0.011(2) C(22) 0.078(3) 0.029(2) 0.075(3) -0.009(2) -0.002(2) 0.003(2) C(23) 0.060(2) 0.030(2) 0.072(3) -0.004(1) -0.002(2) 0.004(2) C(24) 0.049(2) 0.035(2) 0.066(2) 0.001(2) 0.020(2) 0.002(2) C(25) 0.068(2) 0.026(2) 0.054(2) 0.000(2) 0.008(2) -0.005(2) C(26) 0.050(2) 0.035(2) 0.072(2) -0.001(1) 0.008(2) 0.011(2) C(27) 0.076(3) 0.031(2) 0.073(3) -0.002(2) 0.025(2) 0.016(2) C(28) 0.093(3) 0.035(2) 0.047(2) -0.009(2) 0.006(2) 0.010(2) C(29) 0.134(5) 0.052(3) 0.051(2) 0.003(3) 0.026(3) 0.006(2) C(30) 0.122(4) 0.041(2) 0.043(2) -0.010(2) 0.042(2) -0.001(2) C(31) 0.067(2) 0.033(2) 0.036(2) -0.005(2) 0.002(2) -0.005(1) C(32) 0.056(2) 0.029(2) 0.044(2) -0.014(1) 0.013(2) -0.005(1) C(33) 0.050(2) 0.036(2) 0.056(2) -0.008(1) 0.006(2) -0.002(2) C(34) 0.074(2) 0.026(2) 0.057(2) -0.003(2) 0.030(2) 0.001(2) C(35) 0.067(2) 0.029(2) 0.045(2) -0.006(2) 0.023(2) 0.000(1) C(36) 0.045(2) 0.027(2) 0.048(2) -0.008(1) 0.019(1) -0.006(1) C(37) 0.061(2) 0.028(2) 0.041(2) -0.011(1) 0.015(2) -0.001(1) C(38) 0.092(3) 0.042(2) 0.045(2) -0.008(2) 0.030(2) -0.004(2) C(39) 0.068(2) 0.038(2) 0.061(2) -0.005(2) 0.029(2) -0.008(2) C(40) 0.043(2) 0.026(2) 0.056(2) -0.008(1) 0.013(2) -0.002(2) C(41) 0.053(2) 0.037(2) 0.083(3) -0.019(2) 0.010(2) -0.007(2) C(42) 0.062(2) 0.055(3) 0.098(4) -0.014(2) -0.013(3) -0.009(3) C(43) 0.049(2) 0.027(2) 0.067(2) -0.013(1) 0.012(2) 0.003(2) C(44) 0.114(4) 0.034(2) 0.069(2) -0.012(2) 0.034(3) 0.007(2) C(45) 0.052(2) 0.029(2) 0.092(3) -0.003(2) 0.016(2) 0.012(2) C(46) 0.066(2) 0.028(2) 0.095(3) -0.011(2) 0.031(2) 0.000(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F^2^ against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^, conventional R-factors (R) are calculated on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 1.5sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factor based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + 0.04000(Fo^2^)^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3351 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.2665 _refine_ls_wR_factor_gt 0.2646 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_shift/su_max 0.4580 _refine_ls_shift/su_mean 0.0310 _refine_diff_density_min -0.47 _refine_diff_density_max 0.36 #------------------------------------------------------------------------------ _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) 1.429(6) 1_555 1_555 yes O(2) C(23) 1.241(6) 1_555 1_555 yes O(3) C(23) 1.275(6) 1_555 1_555 yes O(4) C(26) 1.428(6) 1_555 1_555 yes O(5) C(46) 1.209(7) 1_555 1_555 yes O(6) C(46) 1.312(6) 1_555 1_555 yes C(1) C(2) 1.539(8) 1_555 1_555 yes C(1) C(10) 1.525(7) 1_555 1_555 yes C(2) C(3) 1.484(8) 1_555 1_555 yes C(3) C(4) 1.538(9) 1_555 1_555 yes C(4) C(5) 1.538(8) 1_555 1_555 yes C(5) C(6) 1.546(8) 1_555 1_555 yes C(5) C(10) 1.553(6) 1_555 1_555 yes C(6) C(7) 1.522(8) 1_555 1_555 yes C(7) C(8) 1.547(7) 1_555 1_555 yes C(8) C(9) 1.537(7) 1_555 1_555 yes C(8) C(14) 1.543(5) 1_555 1_555 yes C(9) C(10) 1.547(5) 1_555 1_555 yes C(9) C(11) 1.546(6) 1_555 1_555 yes C(10) C(19) 1.564(7) 1_555 1_555 yes C(11) C(12) 1.554(6) 1_555 1_555 yes C(12) C(13) 1.523(7) 1_555 1_555 yes C(13) C(14) 1.557(6) 1_555 1_555 yes C(13) C(17) 1.587(5) 1_555 1_555 yes C(13) C(18) 1.516(6) 1_555 1_555 yes C(14) C(15) 1.520(7) 1_555 1_555 yes C(15) C(16) 1.556(7) 1_555 1_555 yes C(16) C(17) 1.528(7) 1_555 1_555 yes C(17) C(20) 1.556(6) 1_555 1_555 yes C(20) C(21) 1.523(9) 1_555 1_555 yes C(20) C(22) 1.558(6) 1_555 1_555 yes C(22) C(23) 1.529(7) 1_555 1_555 yes C(24) C(25) 1.531(7) 1_555 1_555 yes C(24) C(33) 1.544(7) 1_555 1_555 yes C(25) C(26) 1.529(8) 1_555 1_555 yes C(26) C(27) 1.517(8) 1_555 1_555 yes C(27) C(28) 1.538(8) 1_555 1_555 yes C(28) C(29) 1.552(8) 1_555 1_555 yes C(28) C(33) 1.551(8) 1_555 1_555 yes C(29) C(30) 1.550(8) 1_555 1_555 yes C(30) C(31) 1.533(8) 1_555 1_555 yes C(31) C(32) 1.543(6) 1_555 1_555 yes C(31) C(37) 1.545(6) 1_555 1_555 yes C(32) C(33) 1.559(6) 1_555 1_555 yes C(32) C(34) 1.540(7) 1_555 1_555 yes C(33) C(42) 1.505(7) 1_555 1_555 yes C(34) C(35) 1.539(6) 1_555 1_555 yes C(35) C(36) 1.545(6) 1_555 1_555 yes C(36) C(37) 1.553(7) 1_555 1_555 yes C(36) C(40) 1.582(5) 1_555 1_555 yes C(36) C(41) 1.526(6) 1_555 1_555 yes C(37) C(38) 1.531(7) 1_555 1_555 yes C(38) C(39) 1.537(7) 1_555 1_555 yes C(39) C(40) 1.578(7) 1_555 1_555 yes C(40) C(43) 1.534(6) 1_555 1_555 yes C(43) C(44) 1.524(8) 1_555 1_555 yes C(43) C(45) 1.534(6) 1_555 1_555 yes C(45) C(46) 1.491(7) 1_555 1_555 yes O(7) C(48) 1.22(2) 1_555 1_555 yes C(50) C(48) 1.43(3) 1_555 1_555 yes C(48) C(49) 1.42(2) 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(3) O(1) H(37) 106.2(4) 1_555 1_555 1_555 no C(23) O(3) H(38) 125.2(4) 1_555 1_555 1_555 no C(26) O(4) H(75) 128.0(4) 1_555 1_555 1_555 no C(46) O(6) H(76) 99.7(4) 1_555 1_555 1_555 no C(2) C(1) C(10) 114.1(4) 1_555 1_555 1_555 yes C(2) C(1) H(1) 108.5(4) 1_555 1_555 1_555 no C(2) C(1) H(2) 108.2(5) 1_555 1_555 1_555 no C(10) C(1) H(1) 108.1(5) 1_555 1_555 1_555 no C(10) C(1) H(2) 108.8(4) 1_555 1_555 1_555 no H(1) C(1) H(2) 109.1(4) 1_555 1_555 1_555 no C(1) C(2) C(3) 110.3(5) 1_555 1_555 1_555 yes C(1) C(2) H(3) 108.9(5) 1_555 1_555 1_555 no C(1) C(2) H(4) 107.7(5) 1_555 1_555 1_555 no C(3) C(2) H(3) 110.6(5) 1_555 1_555 1_555 no C(3) C(2) H(4) 109.0(5) 1_555 1_555 1_555 no H(3) C(2) H(4) 110.4(7) 1_555 1_555 1_555 no O(1) C(3) C(2) 112.2(5) 1_555 1_555 1_555 yes O(1) C(3) C(4) 112.7(5) 1_555 1_555 1_555 yes O(1) C(3) H(5) 107.2(4) 1_555 1_555 1_555 no C(2) C(3) C(4) 109.6(4) 1_555 1_555 1_555 yes C(2) C(3) H(5) 108.2(5) 1_555 1_555 1_555 no C(4) C(3) H(5) 106.7(6) 1_555 1_555 1_555 no C(3) C(4) C(5) 114.2(4) 1_555 1_555 1_555 yes C(3) C(4) H(6) 108.2(4) 1_555 1_555 1_555 no C(3) C(4) H(7) 108.3(5) 1_555 1_555 1_555 no C(5) C(4) H(6) 108.1(5) 1_555 1_555 1_555 no C(5) C(4) H(7) 108.5(4) 1_555 1_555 1_555 no H(6) C(4) H(7) 109.4(5) 1_555 1_555 1_555 no C(4) C(5) C(6) 109.1(4) 1_555 1_555 1_555 yes C(4) C(5) C(10) 111.2(4) 1_555 1_555 1_555 yes C(4) C(5) H(8) 107.7(4) 1_555 1_555 1_555 no C(6) C(5) C(10) 112.9(4) 1_555 1_555 1_555 yes C(6) C(5) H(8) 107.6(5) 1_555 1_555 1_555 no C(10) C(5) H(8) 108.2(4) 1_555 1_555 1_555 no C(5) C(6) C(7) 113.7(5) 1_555 1_555 1_555 yes C(5) C(6) H(9) 107.5(5) 1_555 1_555 1_555 no C(5) C(6) H(10) 108.1(5) 1_555 1_555 1_555 no C(7) C(6) H(9) 108.5(5) 1_555 1_555 1_555 no C(7) C(6) H(10) 108.8(5) 1_555 1_555 1_555 no H(9) C(6) H(10) 110.3(7) 1_555 1_555 1_555 no C(6) C(7) C(8) 110.3(4) 1_555 1_555 1_555 yes C(6) C(7) H(11) 109.4(6) 1_555 1_555 1_555 no C(6) C(7) H(12) 109.5(5) 1_555 1_555 1_555 no C(8) C(7) H(11) 110.1(5) 1_555 1_555 1_555 no C(8) C(7) H(12) 108.9(5) 1_555 1_555 1_555 no H(11) C(7) H(12) 108.5(5) 1_555 1_555 1_555 no C(7) C(8) C(9) 109.9(4) 1_555 1_555 1_555 yes C(7) C(8) C(14) 110.6(3) 1_555 1_555 1_555 yes C(7) C(8) H(13) 108.0(5) 1_555 1_555 1_555 no C(9) C(8) C(14) 110.9(4) 1_555 1_555 1_555 yes C(9) C(8) H(13) 109.0(4) 1_555 1_555 1_555 no C(14) C(8) H(13) 108.3(4) 1_555 1_555 1_555 no C(8) C(9) C(10) 113.2(4) 1_555 1_555 1_555 yes C(8) C(9) C(11) 112.1(3) 1_555 1_555 1_555 yes C(8) C(9) H(14) 105.7(3) 1_555 1_555 1_555 no C(10) C(9) C(11) 113.6(3) 1_555 1_555 1_555 yes C(10) C(9) H(14) 105.7(4) 1_555 1_555 1_555 no C(11) C(9) H(14) 105.6(4) 1_555 1_555 1_555 no C(1) C(10) C(5) 107.9(4) 1_555 1_555 1_555 yes C(1) C(10) C(9) 114.5(4) 1_555 1_555 1_555 yes C(1) C(10) C(19) 105.9(4) 1_555 1_555 1_555 yes C(5) C(10) C(9) 109.6(3) 1_555 1_555 1_555 yes C(5) C(10) C(19) 108.2(4) 1_555 1_555 1_555 yes C(9) C(10) C(19) 110.5(4) 1_555 1_555 1_555 yes C(9) C(11) C(12) 114.9(3) 1_555 1_555 1_555 yes C(9) C(11) H(15) 107.8(4) 1_555 1_555 1_555 no C(9) C(11) H(16) 108.4(4) 1_555 1_555 1_555 no C(12) C(11) H(15) 107.8(4) 1_555 1_555 1_555 no C(12) C(11) H(16) 108.8(5) 1_555 1_555 1_555 no H(15) C(11) H(16) 109.2(4) 1_555 1_555 1_555 no C(11) C(12) C(13) 111.7(4) 1_555 1_555 1_555 yes C(11) C(12) H(17) 108.3(4) 1_555 1_555 1_555 no C(11) C(12) H(18) 108.9(4) 1_555 1_555 1_555 no C(13) C(12) H(17) 109.6(4) 1_555 1_555 1_555 no C(13) C(12) H(18) 109.2(4) 1_555 1_555 1_555 no H(17) C(12) H(18) 109.0(5) 1_555 1_555 1_555 no C(12) C(13) C(14) 106.6(3) 1_555 1_555 1_555 yes C(12) C(13) C(17) 116.1(4) 1_555 1_555 1_555 yes C(12) C(13) C(18) 111.3(4) 1_555 1_555 1_555 yes C(14) C(13) C(17) 98.3(3) 1_555 1_555 1_555 yes C(14) C(13) C(18) 113.9(4) 1_555 1_555 1_555 yes C(17) C(13) C(18) 110.1(3) 1_555 1_555 1_555 yes C(8) C(14) C(13) 111.1(3) 1_555 1_555 1_555 yes C(8) C(14) C(15) 118.8(4) 1_555 1_555 1_555 yes C(8) C(14) H(19) 107.2(4) 1_555 1_555 1_555 no C(13) C(14) C(15) 105.4(3) 1_555 1_555 1_555 yes C(13) C(14) H(19) 107.3(4) 1_555 1_555 1_555 no C(15) C(14) H(19) 106.5(3) 1_555 1_555 1_555 no C(14) C(15) C(16) 103.9(4) 1_555 1_555 1_555 yes C(14) C(15) H(20) 111.4(5) 1_555 1_555 1_555 no C(14) C(15) H(21) 110.2(4) 1_555 1_555 1_555 no C(16) C(15) H(20) 111.7(4) 1_555 1_555 1_555 no C(16) C(15) H(21) 110.6(5) 1_555 1_555 1_555 no H(20) C(15) H(21) 109.0(5) 1_555 1_555 1_555 no C(15) C(16) C(17) 107.2(4) 1_555 1_555 1_555 yes C(15) C(16) H(22) 110.2(4) 1_555 1_555 1_555 no C(15) C(16) H(23) 109.5(4) 1_555 1_555 1_555 no C(17) C(16) H(22) 110.2(4) 1_555 1_555 1_555 no C(17) C(16) H(23) 110.5(4) 1_555 1_555 1_555 no H(22) C(16) H(23) 109.3(4) 1_555 1_555 1_555 no C(13) C(17) C(16) 104.4(3) 1_555 1_555 1_555 yes C(13) C(17) C(20) 116.0(3) 1_555 1_555 1_555 yes C(13) C(17) H(24) 107.7(4) 1_555 1_555 1_555 no C(16) C(17) C(20) 113.3(4) 1_555 1_555 1_555 yes C(16) C(17) H(24) 107.7(4) 1_555 1_555 1_555 no C(20) C(17) H(24) 107.3(4) 1_555 1_555 1_555 no C(13) C(18) H(25) 110.3(5) 1_555 1_555 1_555 no C(13) C(18) H(26) 110.1(4) 1_555 1_555 1_555 no C(13) C(18) H(27) 109.5(4) 1_555 1_555 1_555 no H(25) C(18) H(26) 109.5(5) 1_555 1_555 1_555 no H(25) C(18) H(27) 109.2(5) 1_555 1_555 1_555 no H(26) C(18) H(27) 108.3(5) 1_555 1_555 1_555 no C(10) C(19) H(28) 109.6(5) 1_555 1_555 1_555 no C(10) C(19) H(29) 109.4(5) 1_555 1_555 1_555 no C(10) C(19) H(30) 109.3(5) 1_555 1_555 1_555 no H(28) C(19) H(29) 109.4(6) 1_555 1_555 1_555 no H(28) C(19) H(30) 109.8(6) 1_555 1_555 1_555 no H(29) C(19) H(30) 109.4(6) 1_555 1_555 1_555 no C(17) C(20) C(21) 113.5(4) 1_555 1_555 1_555 yes C(17) C(20) C(22) 109.8(4) 1_555 1_555 1_555 yes C(17) C(20) H(31) 107.5(4) 1_555 1_555 1_555 no C(21) C(20) C(22) 109.1(4) 1_555 1_555 1_555 yes C(21) C(20) H(31) 108.7(4) 1_555 1_555 1_555 no C(22) C(20) H(31) 108.1(4) 1_555 1_555 1_555 no C(20) C(21) H(32) 109.8(6) 1_555 1_555 1_555 no C(20) C(21) H(33) 109.6(5) 1_555 1_555 1_555 no C(20) C(21) H(34) 109.3(5) 1_555 1_555 1_555 no H(32) C(21) H(33) 109.8(6) 1_555 1_555 1_555 no H(32) C(21) H(34) 109.3(5) 1_555 1_555 1_555 no H(33) C(21) H(34) 109.1(6) 1_555 1_555 1_555 no C(20) C(22) C(23) 112.0(4) 1_555 1_555 1_555 yes O(2) C(23) O(3) 124.5(5) 1_555 1_555 1_555 yes O(2) C(23) C(22) 120.4(5) 1_555 1_555 1_555 yes O(3) C(23) C(22) 115.1(4) 1_555 1_555 1_555 yes C(25) C(24) C(33) 115.1(4) 1_555 1_555 1_555 yes C(25) C(24) H(39) 107.6(4) 1_555 1_555 1_555 no C(25) C(24) H(40) 107.9(4) 1_555 1_555 1_555 no C(33) C(24) H(39) 108.1(4) 1_555 1_555 1_555 no C(33) C(24) H(40) 108.5(4) 1_555 1_555 1_555 no H(39) C(24) H(40) 109.6(5) 1_555 1_555 1_555 no C(24) C(25) C(26) 110.7(4) 1_555 1_555 1_555 yes C(24) C(25) H(41) 109.3(5) 1_555 1_555 1_555 no C(24) C(25) H(42) 109.0(4) 1_555 1_555 1_555 no C(26) C(25) H(41) 109.4(4) 1_555 1_555 1_555 no C(26) C(25) H(42) 109.1(5) 1_555 1_555 1_555 no H(41) C(25) H(42) 109.4(4) 1_555 1_555 1_555 no O(4) C(26) C(25) 111.7(4) 1_555 1_555 1_555 yes O(4) C(26) C(27) 113.7(4) 1_555 1_555 1_555 yes O(4) C(26) H(43) 106.6(4) 1_555 1_555 1_555 no C(25) C(26) C(27) 110.7(4) 1_555 1_555 1_555 yes C(25) C(26) H(43) 107.1(5) 1_555 1_555 1_555 no C(27) C(26) H(43) 106.5(4) 1_555 1_555 1_555 no C(26) C(27) C(28) 113.1(5) 1_555 1_555 1_555 yes C(26) C(27) H(44) 108.5(4) 1_555 1_555 1_555 no C(26) C(27) H(45) 108.2(4) 1_555 1_555 1_555 no C(28) C(27) H(44) 109.8(4) 1_555 1_555 1_555 no C(28) C(27) H(45) 109.5(4) 1_555 1_555 1_555 no H(44) C(27) H(45) 107.6(6) 1_555 1_555 1_555 no C(27) C(28) C(29) 111.7(5) 1_555 1_555 1_555 yes C(27) C(28) C(33) 114.9(4) 1_555 1_555 1_555 yes C(27) C(28) H(46) 106.3(4) 1_555 1_555 1_555 no C(29) C(28) C(33) 111.1(4) 1_555 1_555 1_555 yes C(29) C(28) H(46) 106.6(4) 1_555 1_555 1_555 no C(33) C(28) H(46) 105.7(5) 1_555 1_555 1_555 no C(28) C(29) C(30) 110.6(4) 1_555 1_555 1_555 yes C(28) C(29) H(47) 108.7(7) 1_555 1_555 1_555 no C(28) C(29) H(48) 109.7(5) 1_555 1_555 1_555 no C(30) C(29) H(47) 109.1(5) 1_555 1_555 1_555 no C(30) C(29) H(48) 110.6(7) 1_555 1_555 1_555 no H(47) C(29) H(48) 108.1(5) 1_555 1_555 1_555 no C(29) C(30) C(31) 109.0(5) 1_555 1_555 1_555 yes C(29) C(30) H(49) 109.4(5) 1_555 1_555 1_555 no C(29) C(30) H(50) 110.0(4) 1_555 1_555 1_555 no C(31) C(30) H(49) 109.9(4) 1_555 1_555 1_555 no C(31) C(30) H(50) 109.5(5) 1_555 1_555 1_555 no H(49) C(30) H(50) 108.9(6) 1_555 1_555 1_555 no C(30) C(31) C(32) 109.9(4) 1_555 1_555 1_555 yes C(30) C(31) C(37) 111.1(4) 1_555 1_555 1_555 yes C(30) C(31) H(51) 108.8(4) 1_555 1_555 1_555 no C(32) C(31) C(37) 110.0(3) 1_555 1_555 1_555 yes C(32) C(31) H(51) 108.8(4) 1_555 1_555 1_555 no C(37) C(31) H(51) 108.2(4) 1_555 1_555 1_555 no C(31) C(32) C(33) 111.7(3) 1_555 1_555 1_555 yes C(31) C(32) C(34) 113.0(4) 1_555 1_555 1_555 yes C(31) C(32) H(52) 106.2(4) 1_555 1_555 1_555 no C(33) C(32) C(34) 113.3(4) 1_555 1_555 1_555 yes C(33) C(32) H(52) 105.9(4) 1_555 1_555 1_555 no C(34) C(32) H(52) 106.0(4) 1_555 1_555 1_555 no C(24) C(33) C(28) 107.0(4) 1_555 1_555 1_555 yes C(24) C(33) C(32) 112.9(4) 1_555 1_555 1_555 yes C(24) C(33) C(42) 106.7(4) 1_555 1_555 1_555 yes C(28) C(33) C(32) 108.7(4) 1_555 1_555 1_555 yes C(28) C(33) C(42) 109.0(4) 1_555 1_555 1_555 yes C(32) C(33) C(42) 112.4(4) 1_555 1_555 1_555 yes C(32) C(34) C(35) 114.7(4) 1_555 1_555 1_555 yes C(32) C(34) H(53) 108.3(4) 1_555 1_555 1_555 no C(32) C(34) H(54) 108.3(4) 1_555 1_555 1_555 no C(35) C(34) H(53) 107.9(4) 1_555 1_555 1_555 no C(35) C(34) H(54) 107.5(4) 1_555 1_555 1_555 no H(53) C(34) H(54) 110.1(5) 1_555 1_555 1_555 no C(34) C(35) C(36) 111.1(3) 1_555 1_555 1_555 yes C(34) C(35) H(55) 109.7(4) 1_555 1_555 1_555 no C(34) C(35) H(56) 109.0(4) 1_555 1_555 1_555 no C(36) C(35) H(55) 109.5(4) 1_555 1_555 1_555 no C(36) C(35) H(56) 108.8(4) 1_555 1_555 1_555 no H(55) C(35) H(56) 108.6(4) 1_555 1_555 1_555 no C(35) C(36) C(37) 107.1(3) 1_555 1_555 1_555 yes C(35) C(36) C(40) 116.6(3) 1_555 1_555 1_555 yes C(35) C(36) C(41) 111.5(4) 1_555 1_555 1_555 yes C(37) C(36) C(40) 100.1(3) 1_555 1_555 1_555 yes C(37) C(36) C(41) 113.6(4) 1_555 1_555 1_555 yes C(40) C(36) C(41) 107.6(3) 1_555 1_555 1_555 yes C(31) C(37) C(36) 112.1(4) 1_555 1_555 1_555 yes C(31) C(37) C(38) 118.5(3) 1_555 1_555 1_555 yes C(31) C(37) H(57) 107.5(4) 1_555 1_555 1_555 no C(36) C(37) C(38) 104.1(4) 1_555 1_555 1_555 yes C(36) C(37) H(57) 107.0(3) 1_555 1_555 1_555 no C(38) C(37) H(57) 107.0(4) 1_555 1_555 1_555 no C(37) C(38) C(39) 105.3(4) 1_555 1_555 1_555 yes C(37) C(38) H(58) 110.2(5) 1_555 1_555 1_555 no C(37) C(38) H(59) 110.2(5) 1_555 1_555 1_555 no C(39) C(38) H(58) 111.0(5) 1_555 1_555 1_555 no C(39) C(38) H(59) 111.0(5) 1_555 1_555 1_555 no H(58) C(38) H(59) 109.1(5) 1_555 1_555 1_555 no C(38) C(39) C(40) 106.8(4) 1_555 1_555 1_555 yes C(38) C(39) H(60) 110.4(5) 1_555 1_555 1_555 no C(38) C(39) H(61) 110.6(4) 1_555 1_555 1_555 no C(40) C(39) H(60) 110.0(4) 1_555 1_555 1_555 no C(40) C(39) H(61) 110.2(5) 1_555 1_555 1_555 no H(60) C(39) H(61) 108.9(5) 1_555 1_555 1_555 no C(36) C(40) C(39) 102.7(3) 1_555 1_555 1_555 yes C(36) C(40) C(43) 118.0(4) 1_555 1_555 1_555 yes C(36) C(40) H(62) 107.3(3) 1_555 1_555 1_555 no C(39) C(40) C(43) 113.4(4) 1_555 1_555 1_555 yes C(39) C(40) H(62) 107.1(4) 1_555 1_555 1_555 no C(43) C(40) H(62) 107.7(4) 1_555 1_555 1_555 no C(33) C(42) H(66) 110.2(5) 1_555 1_555 1_555 no C(33) C(42) H(67) 109.5(6) 1_555 1_555 1_555 no C(33) C(42) H(68) 110.5(5) 1_555 1_555 1_555 no H(66) C(42) H(67) 108.2(6) 1_555 1_555 1_555 no H(66) C(42) H(68) 109.4(6) 1_555 1_555 1_555 no H(67) C(42) H(68) 109.0(6) 1_555 1_555 1_555 no C(40) C(43) C(44) 113.6(4) 1_555 1_555 1_555 yes C(40) C(43) C(45) 111.6(4) 1_555 1_555 1_555 yes C(40) C(43) H(69) 108.1(4) 1_555 1_555 1_555 no C(44) C(43) C(45) 107.8(4) 1_555 1_555 1_555 yes C(44) C(43) H(69) 108.0(5) 1_555 1_555 1_555 no C(45) C(43) H(69) 107.5(4) 1_555 1_555 1_555 no C(43) C(44) H(70) 109.1(5) 1_555 1_555 1_555 no C(43) C(44) H(71) 109.1(5) 1_555 1_555 1_555 no C(43) C(44) H(72) 109.5(6) 1_555 1_555 1_555 no H(70) C(44) H(71) 109.4(7) 1_555 1_555 1_555 no H(70) C(44) H(72) 109.7(5) 1_555 1_555 1_555 no H(71) C(44) H(72) 110.0(5) 1_555 1_555 1_555 no C(43) C(45) C(46) 113.0(4) 1_555 1_555 1_555 yes C(43) C(45) H(73) 108.8(4) 1_555 1_555 1_555 no C(43) C(45) H(74) 108.9(4) 1_555 1_555 1_555 no C(46) C(45) H(73) 108.6(5) 1_555 1_555 1_555 no C(46) C(45) H(74) 108.3(4) 1_555 1_555 1_555 no H(73) C(45) H(74) 109.2(5) 1_555 1_555 1_555 no O(5) C(46) O(6) 121.5(5) 1_555 1_555 1_555 yes O(5) C(46) C(45) 124.2(5) 1_555 1_555 1_555 yes O(6) C(46) C(45) 114.3(4) 1_555 1_555 1_555 yes C(48) C(50) H(77) 130(3) 1_555 1_555 1_555 no C(48) C(50) H(78) 111(2) 1_555 1_555 1_555 no C(48) C(50) H(79) 112(2) 1_555 1_555 1_555 no H(77) C(50) H(78) 107(3) 1_555 1_555 1_555 no H(77) C(50) H(79) 100(3) 1_555 1_555 1_555 no H(78) C(50) H(79) 81(2) 1_555 1_555 1_555 no O(7) C(48) C(50) 125(1) 1_555 1_555 1_555 yes O(7) C(48) C(49) 121(1) 1_555 1_555 1_555 yes C(50) C(48) C(49) 112(1) 1_555 1_555 1_555 yes C(48) C(49) H(80) 127(2) 1_555 1_555 1_555 no C(48) C(49) H(81) 115(2) 1_555 1_555 1_555 no C(48) C(49) H(82) 120(2) 1_555 1_555 1_555 no H(80) C(49) H(81) 92(2) 1_555 1_555 1_555 no H(80) C(49) H(82) 103(3) 1_555 1_555 1_555 no H(81) C(49) H(82) 85(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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) 178.4(4) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) -179.3(4) 1_555 1_555 1_555 1_555 yes O(2) C(23) C(22) C(20) -136.5(6) 1_555 1_555 1_555 1_555 yes O(3) C(23) C(22) C(20) 43.5(7) 1_555 1_555 1_555 1_555 yes O(4) C(26) C(25) C(24) 177.7(4) 1_555 1_555 1_555 1_555 yes O(4) C(26) C(27) C(28) 179.4(4) 1_555 1_555 1_555 1_555 yes O(5) C(46) C(45) C(43) -124.9(6) 1_555 1_555 1_555 1_555 yes O(6) C(46) C(45) C(43) 54.3(7) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -55.6(5) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(4) 52.0(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(5) C(6) 175.0(4) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -175.9(3) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(11) 54.7(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(5) -56.6(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 65.8(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(19) -172.2(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 55.0(6) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) 60.1(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -178.8(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(10) -53.6(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 72.5(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(9) -73.3(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(10) C(19) 166.2(4) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 54.2(7) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) -54.5(5) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(11) 176.1(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 49.7(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(19) -70.9(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -56.7(6) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) -179.4(5) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -51.6(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 58.6(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(11) -171.3(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(13) -177.5(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(14) C(15) -55.1(6) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(19) 64.7(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(11) C(12) 44.8(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(12) -64.5(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(17) 175.0(4) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(13) C(18) 58.7(5) 1_555 1_555 1_555 1_555 yes C(8) C(14) C(15) C(16) -158.4(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(13) 60.3(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(14) C(15) -177.3(4) 1_555 1_555 1_555 1_555 yes C(9) C(11) C(12) C(13) -51.0(5) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -178.8(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(11) C(12) 174.7(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(8) C(14) -48.7(4) 1_555 1_555 1_555 1_555 yes C(11) C(9) C(10) C(19) -64.7(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 58.5(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(17) 166.8(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(18) -66.3(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 165.6(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(16) -153.0(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(17) C(20) 81.5(5) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -33.2(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(16) C(15) 21.3(4) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(21) -65.2(5) 1_555 1_555 1_555 1_555 yes C(13) C(17) C(20) C(22) 172.4(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(16) -39.8(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(17) C(20) -165.3(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 6.8(5) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(17) 45.1(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -71.3(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(20) 148.5(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(13) C(18) 79.5(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(21) 173.9(4) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(20) C(22) 51.6(5) 1_555 1_555 1_555 1_555 yes C(17) C(20) C(22) C(23) -165.3(5) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(17) C(20) -46.0(5) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(22) C(23) 69.7(6) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) -54.5(5) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(27) 50.0(5) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(28) C(29) 178.0(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(31) -175.3(4) 1_555 1_555 1_555 1_555 yes C(24) C(33) C(32) C(34) 55.6(5) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(28) -53.4(5) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(32) 66.1(5) 1_555 1_555 1_555 1_555 yes C(25) C(24) C(33) C(42) -169.9(4) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) 52.7(5) 1_555 1_555 1_555 1_555 yes C(26) C(25) C(24) C(33) 57.6(5) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 179.9(4) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(33) -52.4(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 71.4(6) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(32) -72.2(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(33) C(42) 165.0(4) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 59.4(6) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(31) -56.8(5) 1_555 1_555 1_555 1_555 yes C(28) C(33) C(32) C(34) 174.2(4) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(32) 55.7(5) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(33) C(42) -67.0(6) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -59.6(5) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(37) 178.4(4) 1_555 1_555 1_555 1_555 yes C(30) C(29) C(28) C(33) -58.3(7) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(33) 59.7(5) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(32) C(34) -171.1(4) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(36) -179.7(3) 1_555 1_555 1_555 1_555 yes C(30) C(31) C(37) C(38) -58.3(5) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(42) 63.8(6) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(34) C(35) 46.8(5) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(35) -63.1(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(40) 174.9(3) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(36) C(41) 60.5(4) 1_555 1_555 1_555 1_555 yes C(31) C(37) C(38) C(39) -158.5(4) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(36) 58.4(5) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(37) C(38) 179.8(4) 1_555 1_555 1_555 1_555 yes C(32) C(34) C(35) C(36) -52.1(5) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(37) -177.7(4) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(34) C(35) 175.2(4) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(31) C(37) -48.5(5) 1_555 1_555 1_555 1_555 yes C(34) C(32) C(33) C(42) -65.2(6) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) 58.1(5) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(40) 169.2(4) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(41) -66.7(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 167.6(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(39) -155.1(4) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(40) C(43) 79.4(5) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) -33.1(5) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(39) C(38) 20.9(5) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(44) -65.6(5) 1_555 1_555 1_555 1_555 yes C(36) C(40) C(43) C(45) 172.2(4) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(39) -40.0(4) 1_555 1_555 1_555 1_555 yes C(37) C(36) C(40) C(43) -165.5(4) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) 7.0(5) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(40) 45.6(4) 1_555 1_555 1_555 1_555 yes C(38) C(37) C(36) C(41) -68.8(4) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(43) 149.4(4) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(36) C(41) 78.8(4) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(44) 174.3(4) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(43) C(45) 52.1(5) 1_555 1_555 1_555 1_555 yes C(40) C(43) C(45) C(46) -170.8(4) 1_555 1_555 1_555 1_555 yes C(41) C(36) C(40) C(43) -46.7(5) 1_555 1_555 1_555 1_555 yes C(44) C(43) C(45) C(46) 63.8(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(3) 2.604(6) 1_555 1_545 ? O(1) O(5) 2.787(5) 1_555 1_455 ? O(1) O(2) 3.231(5) 1_555 1_545 ? O(1) C(23) 3.283(6) 1_555 1_545 ? O(2) O(4) 2.719(5) 1_555 1_455 ? O(2) C(26) 3.446(6) 1_555 1_455 ? O(4) O(6) 2.621(6) 1_555 1_565 ? O(4) O(5) 3.315(6) 1_555 1_565 ? O(4) C(46) 3.381(7) 1_555 1_565 ? O(5) C(50) 3.21(3) 1_555 1_544 ? O(5) C(3) 3.472(7) 1_555 1_655 ? O(5) C(49) 3.47(3) 1_555 1_545 ? O(5) C(4) 3.597(8) 1_555 1_655 ? O(6) C(50) 3.37(3) 1_555 1_544 ? C(2) C(50) 3.50(3) 1_555 1_445 ? C(45) C(50) 3.28(2) 1_555 1_544 ? C(46) C(50) 3.00(3) 1_555 1_544 ? #------------------------------------------------------------------------------ _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 565-8710 Japan ; _publ_contact_author_email ' miyata@ap.chem.eng.osaka-u.ac.jp ' _publ_contact_author_fax ' +81-6-879-7404 ' _publ_contact_author_phone ' +81-6-879-7406 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chem.Commun.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; A Robust Structural Motif in Inclusion Crystals of Norbile Acids ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' Michihiro Sugahara ' ; Material and Life Science, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-8710 Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _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 ;