# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Luo, Jia' 'Yan, Qifan' 'Zhou, Yan' 'Zhu, Ningbo' 'Li, Tian' 'Bai, Chuanjiang' 'Cao, Yong' 'Wang, Jian' 'Pei, Jian' 'Zhao, Dahui' _publ_contact_author_name 'Zhao, Dahui' _publ_contact_author_email dhzhao@pku.edu.cn _publ_section_title ; A Photoswitch Based on Self-Assembled Single Microwire of a Phenyleneethynylene Macrocycle ; # Attachment '10088m.cif.txt' data_10088m _database_code_depnum_ccdc_archive 'CCDC 772272' #TrackingRef '10088m.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H96 O6, 0.5(C4 H8 O2)' _chemical_formula_sum 'C86 H100 O7' _chemical_formula_weight 1245.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4266(6) _cell_length_b 14.7760(7) _cell_length_c 20.1053(9) _cell_angle_alpha 84.8020(10) _cell_angle_beta 71.9290(10) _cell_angle_gamma 76.2150(10) _cell_volume 3682.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4621 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.81 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9674 _exptl_absorpt_correction_T_max 0.9897 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28728 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.10 _reflns_number_total 14363 _reflns_number_gt 7776 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT-PLUS (Bruker, 2003)' _computing_data_reduction SAINT-PLUS _computing_structure_solution 'SHELXTL (Bruker, 2005)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of 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 based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors 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 'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14363 _refine_ls_number_parameters 844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.22864(19) 0.55811(16) 0.22728(13) 0.0282(6) Uani 1 1 d . . . C2 C -0.3307(2) 0.60829(16) 0.22760(13) 0.0308(6) Uani 1 1 d . . . H2 H -0.3912 0.5826 0.2509 0.037 Uiso 1 1 calc R . . C3 C -0.34591(19) 0.69430(16) 0.19494(13) 0.0289(6) Uani 1 1 d . . . C4 C -0.2572(2) 0.73209(16) 0.15916(13) 0.0300(6) Uani 1 1 d . . . C5 C -0.1560(2) 0.68390(16) 0.15812(13) 0.0306(6) Uani 1 1 d . . . H5 H -0.0960 0.7098 0.1338 0.037 Uiso 1 1 calc R . . C6 C -0.13952(19) 0.59704(16) 0.19233(13) 0.0284(6) Uani 1 1 d . . . C7 C -0.0331(2) 0.55111(16) 0.19204(13) 0.0312(6) Uani 1 1 d . . . C8 C 0.0571(2) 0.51573(17) 0.19192(13) 0.0338(6) Uani 1 1 d . . . C9 C 0.16434(19) 0.47198(17) 0.19175(13) 0.0308(6) Uani 1 1 d . . . C10 C 0.2514(2) 0.50354(18) 0.14642(14) 0.0390(7) Uani 1 1 d . . . H10 H 0.2391 0.5559 0.1165 0.047 Uiso 1 1 calc R . . C11 C 0.3547(2) 0.46013(19) 0.14427(14) 0.0404(7) Uani 1 1 d . . . H11 H 0.4131 0.4822 0.1125 0.048 Uiso 1 1 calc R . . C12 C 0.37513(19) 0.38423(17) 0.18804(13) 0.0309(6) Uani 1 1 d . . . C13 C 0.2873(2) 0.35431(18) 0.23501(14) 0.0369(6) Uani 1 1 d . . . H13 H 0.2993 0.3034 0.2662 0.044 Uiso 1 1 calc R . . C14 C 0.1842(2) 0.39747(17) 0.23666(14) 0.0362(6) Uani 1 1 d . . . H14 H 0.1257 0.3762 0.2689 0.043 Uiso 1 1 calc R . . C15 C 0.4818(2) 0.33533(18) 0.18575(13) 0.0341(6) Uani 1 1 d . . . C16 C 0.5684(2) 0.29026(17) 0.18545(13) 0.0320(6) Uani 1 1 d . . . C17 C 0.66853(19) 0.23074(17) 0.18682(13) 0.0299(6) Uani 1 1 d . . . C18 C 0.76596(19) 0.26077(17) 0.15906(13) 0.0313(6) Uani 1 1 d . . . H18 H 0.7653 0.3218 0.1394 0.038 Uiso 1 1 calc R . . C19 C 0.86193(19) 0.20189(17) 0.16037(13) 0.0299(6) Uani 1 1 d . . . C20 C 0.86352(19) 0.11188(17) 0.19001(13) 0.0299(6) Uani 1 1 d . . . C21 C 0.76857(19) 0.08235(18) 0.21719(13) 0.0324(6) Uani 1 1 d . . . H21 H 0.7697 0.0216 0.2374 0.039 Uiso 1 1 calc R . . C22 C 0.67098(19) 0.14053(17) 0.21543(13) 0.0300(6) Uani 1 1 d . . . C23 C 0.57560(19) 0.10545(17) 0.24207(13) 0.0304(6) Uani 1 1 d . . . C24 C 0.4990(2) 0.07156(18) 0.26453(13) 0.0335(6) Uani 1 1 d . . . C25 C 0.40957(19) 0.02876(17) 0.29533(12) 0.0297(6) Uani 1 1 d . . . C26 C 0.4259(2) -0.06742(18) 0.30417(14) 0.0370(6) Uani 1 1 d . . . H26 H 0.4961 -0.1050 0.2863 0.044 Uiso 1 1 calc R . . C27 C 0.3420(2) -0.10896(18) 0.33836(14) 0.0366(6) Uani 1 1 d . . . H27 H 0.3550 -0.1748 0.3440 0.044 Uiso 1 1 calc R . . C28 C 0.2382(2) -0.05533(17) 0.36479(12) 0.0307(6) Uani 1 1 d . . . C29 C 0.2208(2) 0.04115(17) 0.35417(13) 0.0336(6) Uani 1 1 d . . . H29 H 0.1503 0.0787 0.3707 0.040 Uiso 1 1 calc R . . C30 C 0.3057(2) 0.08222(17) 0.31973(13) 0.0333(6) Uani 1 1 d . . . H30 H 0.2928 0.1479 0.3126 0.040 Uiso 1 1 calc R . . C31 C 0.1515(2) -0.09778(17) 0.40271(13) 0.0339(6) Uani 1 1 d . . . C32 C 0.0793(2) -0.13280(17) 0.43472(13) 0.0323(6) Uani 1 1 d . . . C33 C -0.00830(19) -0.17552(16) 0.47277(12) 0.0281(6) Uani 1 1 d . . . C34 C 0.01399(19) -0.26377(17) 0.50378(12) 0.0299(6) Uani 1 1 d . . . H34 H 0.0863 -0.2942 0.5000 0.036 Uiso 1 1 calc R . . C35 C -0.06825(19) -0.30681(16) 0.53973(12) 0.0279(6) Uani 1 1 d . . . C36 C -0.17496(19) -0.26148(16) 0.54475(12) 0.0273(5) Uani 1 1 d . . . C37 C -0.1977(2) -0.17498(16) 0.51413(12) 0.0285(6) Uani 1 1 d . . . H37 H -0.2700 -0.1450 0.5176 0.034 Uiso 1 1 calc R . . C38 C -0.1133(2) -0.13071(16) 0.47753(12) 0.0277(6) Uani 1 1 d . . . C39 C -0.1369(2) -0.03986(17) 0.44675(13) 0.0329(6) Uani 1 1 d . . . C40 C -0.1501(2) 0.03662(17) 0.42149(14) 0.0357(6) Uani 1 1 d . . . C41 C -0.1624(2) 0.12876(17) 0.39012(14) 0.0358(6) Uani 1 1 d . . . C42 C -0.2609(2) 0.1913(2) 0.40733(18) 0.0594(9) Uani 1 1 d . . . H42 H -0.3213 0.1741 0.4407 0.071 Uiso 1 1 calc R . . C43 C -0.2712(2) 0.27866(19) 0.37588(18) 0.0592(9) Uani 1 1 d . . . H43 H -0.3388 0.3216 0.3889 0.071 Uiso 1 1 calc R . . C44 C -0.1859(2) 0.30530(17) 0.32597(14) 0.0350(6) Uani 1 1 d . . . C45 C -0.0872(2) 0.24342(17) 0.30975(15) 0.0380(7) Uani 1 1 d . . . H45 H -0.0267 0.2610 0.2767 0.046 Uiso 1 1 calc R . . C46 C -0.0758(2) 0.15634(17) 0.34128(14) 0.0386(7) Uani 1 1 d . . . H46 H -0.0075 0.1144 0.3294 0.046 Uiso 1 1 calc R . . C47 C -0.1998(2) 0.39532(17) 0.29140(14) 0.0366(6) Uani 1 1 d . . . C48 C -0.2133(2) 0.46906(17) 0.26213(14) 0.0339(6) Uani 1 1 d . . . C49 C -0.4850(2) 0.74760(19) 0.14055(15) 0.0432(7) Uani 1 1 d . . . H49A H -0.5172 0.6933 0.1425 0.052 Uiso 1 1 calc R . . H49B H -0.4233 0.7434 0.0975 0.052 Uiso 1 1 calc R . . C50 C -0.5673(2) 0.83656(19) 0.13865(16) 0.0461(7) Uani 1 1 d . . . H50A H -0.6059 0.8294 0.1054 0.055 Uiso 1 1 calc R . . H50B H -0.6206 0.8464 0.1856 0.055 Uiso 1 1 calc R . . C51 C -0.5205(2) 0.92174(18) 0.11751(15) 0.0429(7) Uani 1 1 d . . . H51A H -0.4649 0.9109 0.0715 0.051 Uiso 1 1 calc R . . H51B H -0.4849 0.9307 0.1520 0.051 Uiso 1 1 calc R . . C52 C -0.6040(2) 1.0107(2) 0.11259(16) 0.0521(8) Uani 1 1 d . . . H52A H -0.6405 1.0014 0.0787 0.063 Uiso 1 1 calc R . . H52B H -0.6588 1.0223 0.1588 0.063 Uiso 1 1 calc R . . C53 C -0.5564(3) 1.0957(2) 0.09012(18) 0.0632(10) Uani 1 1 d . . . H53A H -0.4996 1.0831 0.0448 0.076 Uiso 1 1 calc R . . H53B H -0.5222 1.1063 0.1249 0.076 Uiso 1 1 calc R . . C54 C -0.6379(4) 1.1837(2) 0.0825(2) 0.0909(14) Uani 1 1 d . . . H54A H -0.6670 1.1762 0.0448 0.109 Uiso 1 1 calc R . . H54B H -0.6028 1.2366 0.0713 0.109 Uiso 1 1 calc R . . H54C H -0.6964 1.1952 0.1265 0.109 Uiso 1 1 calc R . . C55 C -0.1933(2) 0.86165(17) 0.09341(14) 0.0363(6) Uani 1 1 d . . . H55A H -0.1408 0.8224 0.0549 0.044 Uiso 1 1 calc R . . H55B H -0.1559 0.8711 0.1268 0.044 Uiso 1 1 calc R . . C56 C -0.2402(2) 0.95399(17) 0.06482(14) 0.0376(6) Uani 1 1 d . . . H56A H -0.2940 0.9916 0.1037 0.045 Uiso 1 1 calc R . . H56B H -0.2776 0.9434 0.0318 0.045 Uiso 1 1 calc R . . C57 C -0.1544(2) 1.00809(17) 0.02716(15) 0.0393(7) Uani 1 1 d . . . H57A H -0.1131 1.0140 0.0591 0.047 Uiso 1 1 calc R . . H57B H -0.1039 0.9725 -0.0139 0.047 Uiso 1 1 calc R . . C58 C -0.2011(2) 1.10438(17) 0.00300(14) 0.0394(7) Uani 1 1 d . . . H58A H -0.2551 1.1383 0.0437 0.047 Uiso 1 1 calc R . . H58B H -0.2388 1.0980 -0.0310 0.047 Uiso 1 1 calc R . . C59 C -0.1181(2) 1.16196(18) -0.03078(15) 0.0417(7) Uani 1 1 d . . . H59A H -0.0803 1.1686 0.0031 0.050 Uiso 1 1 calc R . . H59B H -0.0641 1.1284 -0.0717 0.050 Uiso 1 1 calc R . . C60 C -0.1669(3) 1.25824(19) -0.05440(17) 0.0556(8) Uani 1 1 d . . . H60A H -0.2010 1.2522 -0.0899 0.083 Uiso 1 1 calc R . . H60B H -0.1103 1.2930 -0.0744 0.083 Uiso 1 1 calc R . . H60C H -0.2208 1.2917 -0.0142 0.083 Uiso 1 1 calc R . . C61 C 0.96553(19) 0.31138(17) 0.09902(14) 0.0330(6) Uani 1 1 d . . . H61A H 0.9244 0.3630 0.1315 0.040 Uiso 1 1 calc R . . H61B H 0.9353 0.3172 0.0593 0.040 Uiso 1 1 calc R . . C62 C 1.08228(19) 0.31476(17) 0.07298(13) 0.0320(6) Uani 1 1 d . . . H62A H 1.1235 0.2581 0.0458 0.038 Uiso 1 1 calc R . . H62B H 1.1093 0.3147 0.1135 0.038 Uiso 1 1 calc R . . C63 C 1.10120(19) 0.40026(17) 0.02737(13) 0.0317(6) Uani 1 1 d . . . H63A H 1.0732 0.4006 -0.0128 0.038 Uiso 1 1 calc R . . H63B H 1.0605 0.4568 0.0548 0.038 Uiso 1 1 calc R . . C64 C 1.2185(2) 0.40401(17) 0.00010(14) 0.0339(6) Uani 1 1 d . . . H64A H 1.2578 0.3510 -0.0315 0.041 Uiso 1 1 calc R . . H64B H 1.2485 0.3965 0.0400 0.041 Uiso 1 1 calc R . . C65 C 1.2374(2) 0.49404(18) -0.03906(15) 0.0420(7) Uani 1 1 d . . . H65A H 1.1925 0.5472 -0.0090 0.050 Uiso 1 1 calc R . . H65B H 1.2139 0.4985 -0.0815 0.050 Uiso 1 1 calc R . . C66 C 1.3541(2) 0.5021(2) -0.06058(17) 0.0535(8) Uani 1 1 d . . . H66A H 1.3792 0.4950 -0.0191 0.080 Uiso 1 1 calc R . . H66B H 1.3600 0.5633 -0.0826 0.080 Uiso 1 1 calc R . . H66C H 1.3984 0.4532 -0.0939 0.080 Uiso 1 1 calc R . . C67 C 0.9632(2) -0.03066(17) 0.22260(14) 0.0340(6) Uani 1 1 d . . . H67A H 0.9330 -0.0685 0.1989 0.041 Uiso 1 1 calc R . . H67B H 0.9179 -0.0233 0.2719 0.041 Uiso 1 1 calc R . . C68 C 1.07642(19) -0.07962(17) 0.21987(14) 0.0337(6) Uani 1 1 d . . . H68A H 1.1059 -0.0435 0.2453 0.040 Uiso 1 1 calc R . . H68B H 1.1227 -0.0855 0.1707 0.040 Uiso 1 1 calc R . . C69 C 1.0741(2) -0.17598(17) 0.25377(14) 0.0368(6) Uani 1 1 d . . . H69A H 1.0264 -0.1682 0.3025 0.044 Uiso 1 1 calc R . . H69B H 1.0418 -0.2098 0.2285 0.044 Uiso 1 1 calc R . . C70 C 1.1820(2) -0.23563(17) 0.25496(14) 0.0382(6) Uani 1 1 d . . . H70A H 1.2177 -0.2003 0.2766 0.046 Uiso 1 1 calc R . . H70B H 1.2278 -0.2494 0.2063 0.046 Uiso 1 1 calc R . . C71 C 1.1724(3) -0.32670(18) 0.29530(17) 0.0511(8) Uani 1 1 d . . . H71A H 1.1248 -0.3128 0.3435 0.061 Uiso 1 1 calc R . . H71B H 1.1384 -0.3626 0.2728 0.061 Uiso 1 1 calc R . . C72 C 1.2795(3) -0.3861(2) 0.2987(2) 0.0829(13) Uani 1 1 d . . . H72A H 1.3288 -0.3966 0.2512 0.124 Uiso 1 1 calc R . . H72B H 1.2692 -0.4461 0.3214 0.124 Uiso 1 1 calc R . . H72C H 1.3098 -0.3540 0.3257 0.124 Uiso 1 1 calc R . . C73 C 0.05152(19) -0.44368(16) 0.56581(14) 0.0324(6) Uani 1 1 d . . . H73A H 0.0882 -0.4087 0.5869 0.039 Uiso 1 1 calc R . . H73B H 0.0933 -0.4544 0.5160 0.039 Uiso 1 1 calc R . . C74 C 0.0428(2) -0.53563(16) 0.60427(13) 0.0319(6) Uani 1 1 d . . . H74A H 0.0058 -0.5696 0.5826 0.038 Uiso 1 1 calc R . . H74B H -0.0013 -0.5236 0.6535 0.038 Uiso 1 1 calc R . . C75 C 0.1524(2) -0.59622(16) 0.60274(14) 0.0331(6) Uani 1 1 d . . . H75A H 0.1896 -0.5620 0.6241 0.040 Uiso 1 1 calc R . . H75B H 0.1963 -0.6085 0.5535 0.040 Uiso 1 1 calc R . . C76 C 0.14422(19) -0.68877(16) 0.64190(13) 0.0296(6) Uani 1 1 d . . . H76A H 0.0958 -0.6762 0.6901 0.036 Uiso 1 1 calc R . . H76B H 0.1115 -0.7246 0.6185 0.036 Uiso 1 1 calc R . . C77 C 0.2518(2) -0.74763(17) 0.64552(14) 0.0341(6) Uani 1 1 d . . . H77A H 0.2847 -0.7119 0.6689 0.041 Uiso 1 1 calc R . . H77B H 0.3002 -0.7606 0.5974 0.041 Uiso 1 1 calc R . . C78 C 0.2422(2) -0.83966(17) 0.68493(14) 0.0389(7) Uani 1 1 d . . . H78A H 0.1923 -0.8274 0.7321 0.058 Uiso 1 1 calc R . . H78B H 0.3129 -0.8732 0.6881 0.058 Uiso 1 1 calc R . . H78C H 0.2150 -0.8775 0.6599 0.058 Uiso 1 1 calc R . . C79 C -0.35978(19) -0.27168(18) 0.58344(15) 0.0374(6) Uani 1 1 d . . . H79A H -0.3646 -0.2554 0.5355 0.045 Uiso 1 1 calc R . . H79B H -0.3891 -0.2146 0.6118 0.045 Uiso 1 1 calc R . . C80 C -0.4221(2) -0.34567(18) 0.61586(15) 0.0409(7) Uani 1 1 d . . . H80A H -0.4123 -0.3638 0.6624 0.049 Uiso 1 1 calc R . . H80B H -0.4996 -0.3190 0.6228 0.049 Uiso 1 1 calc R . . C81 C -0.3879(2) -0.43177(19) 0.57175(14) 0.0409(7) Uani 1 1 d . . . H81A H -0.3120 -0.4610 0.5679 0.049 Uiso 1 1 calc R . . H81B H -0.3921 -0.4127 0.5240 0.049 Uiso 1 1 calc R . . C82 C -0.4558(2) -0.50419(18) 0.60073(15) 0.0405(7) Uani 1 1 d . . . H82A H -0.4542 -0.5216 0.6492 0.049 Uiso 1 1 calc R . . H82B H -0.5313 -0.4761 0.6025 0.049 Uiso 1 1 calc R . . C83 C -0.4171(3) -0.5911(2) 0.55739(16) 0.0525(8) Uani 1 1 d . . . H83A H -0.3423 -0.6202 0.5568 0.063 Uiso 1 1 calc R . . H83B H -0.4165 -0.5734 0.5086 0.063 Uiso 1 1 calc R . . C84 C -0.4868(3) -0.6628(2) 0.58488(19) 0.0641(10) Uani 1 1 d . . . H84A H -0.4841 -0.6836 0.6321 0.096 Uiso 1 1 calc R . . H84B H -0.4597 -0.7163 0.5538 0.096 Uiso 1 1 calc R . . H84C H -0.5612 -0.6342 0.5863 0.096 Uiso 1 1 calc R . . O1 O -0.44852(13) 0.74611(11) 0.20125(9) 0.0364(4) Uani 1 1 d . . . O2 O -0.28064(13) 0.81736(11) 0.12827(9) 0.0378(5) Uani 1 1 d . . . O3 O 0.95957(13) 0.22336(12) 0.13443(9) 0.0376(5) Uani 1 1 d . . . O4 O 0.96226(13) 0.05909(11) 0.18891(9) 0.0363(4) Uani 1 1 d . . . O5 O -0.05573(13) -0.39243(11) 0.57170(9) 0.0341(4) Uani 1 1 d . . . O6 O -0.25057(13) -0.30968(11) 0.58162(9) 0.0334(4) Uani 1 1 d . . . C85 C 0.4921(3) 0.9413(2) 0.45327(16) 0.0540(8) Uani 1 1 d . . . H85A H 0.4166 0.9654 0.4534 0.065 Uiso 1 1 calc R . . H85B H 0.5251 0.8903 0.4192 0.065 Uiso 1 1 calc R . . C86 C 0.5527(3) 1.0187(2) 0.43159(15) 0.0540(8) Uani 1 1 d . . . H86A H 0.6287 0.9943 0.4301 0.065 Uiso 1 1 calc R . . H86B H 0.5510 1.0421 0.3841 0.065 Uiso 1 1 calc R . . O7 O 0.49462(17) 0.90681(14) 0.52013(11) 0.0549(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0320(14) 0.0202(13) 0.0330(14) 0.0003(11) -0.0139(11) -0.0016(11) C2 0.0316(14) 0.0240(13) 0.0371(15) 0.0025(11) -0.0117(12) -0.0058(11) C3 0.0252(14) 0.0220(13) 0.0369(15) -0.0001(11) -0.0105(11) 0.0013(10) C4 0.0360(15) 0.0223(13) 0.0331(14) 0.0034(11) -0.0150(12) -0.0043(11) C5 0.0282(14) 0.0261(13) 0.0380(15) 0.0009(11) -0.0122(12) -0.0045(11) C6 0.0311(14) 0.0222(13) 0.0318(14) -0.0009(11) -0.0149(11) 0.0018(11) C7 0.0360(16) 0.0224(13) 0.0368(15) -0.0023(11) -0.0147(12) -0.0037(12) C8 0.0356(16) 0.0306(14) 0.0345(15) -0.0024(12) -0.0128(12) -0.0023(12) C9 0.0253(14) 0.0268(13) 0.0397(15) -0.0035(11) -0.0112(12) -0.0016(11) C10 0.0342(16) 0.0344(15) 0.0457(17) 0.0107(13) -0.0142(13) -0.0038(12) C11 0.0336(16) 0.0437(17) 0.0424(16) 0.0121(13) -0.0101(13) -0.0124(13) C12 0.0266(14) 0.0288(14) 0.0362(15) 0.0007(11) -0.0106(11) -0.0027(11) C13 0.0301(15) 0.0300(14) 0.0456(17) 0.0113(12) -0.0102(12) -0.0030(12) C14 0.0267(14) 0.0328(15) 0.0451(16) 0.0070(12) -0.0082(12) -0.0050(12) C15 0.0297(15) 0.0321(15) 0.0391(16) 0.0058(12) -0.0082(12) -0.0092(12) C16 0.0258(14) 0.0333(15) 0.0354(15) 0.0048(12) -0.0059(11) -0.0099(12) C17 0.0256(14) 0.0340(14) 0.0291(14) 0.0035(11) -0.0082(11) -0.0063(11) C18 0.0253(14) 0.0300(14) 0.0374(15) 0.0065(11) -0.0084(11) -0.0078(11) C19 0.0227(13) 0.0304(14) 0.0388(15) 0.0069(11) -0.0099(11) -0.0120(11) C20 0.0232(13) 0.0323(14) 0.0339(14) 0.0049(11) -0.0088(11) -0.0071(11) C21 0.0280(14) 0.0325(14) 0.0355(15) 0.0049(12) -0.0081(11) -0.0080(11) C22 0.0255(14) 0.0356(15) 0.0299(14) 0.0032(11) -0.0078(11) -0.0102(11) C23 0.0275(14) 0.0323(14) 0.0321(14) 0.0053(11) -0.0095(11) -0.0092(12) C24 0.0290(15) 0.0401(16) 0.0337(15) 0.0051(12) -0.0103(12) -0.0128(12) C25 0.0267(14) 0.0373(15) 0.0278(14) 0.0019(11) -0.0074(11) -0.0141(12) C26 0.0273(14) 0.0354(15) 0.0484(17) -0.0020(13) -0.0102(12) -0.0079(12) C27 0.0383(16) 0.0266(14) 0.0487(17) 0.0052(12) -0.0171(13) -0.0109(12) C28 0.0359(15) 0.0331(14) 0.0286(14) 0.0051(11) -0.0105(12) -0.0193(12) C29 0.0274(14) 0.0332(15) 0.0403(16) 0.0007(12) -0.0056(12) -0.0138(12) C30 0.0314(15) 0.0278(14) 0.0402(15) 0.0019(12) -0.0062(12) -0.0124(12) C31 0.0392(16) 0.0328(15) 0.0334(15) 0.0060(12) -0.0106(12) -0.0178(13) C32 0.0365(15) 0.0295(14) 0.0339(15) 0.0023(11) -0.0114(12) -0.0128(12) C33 0.0319(14) 0.0257(13) 0.0284(14) 0.0040(11) -0.0065(11) -0.0145(11) C34 0.0252(13) 0.0308(14) 0.0336(14) 0.0031(11) -0.0081(11) -0.0080(11) C35 0.0327(14) 0.0211(13) 0.0292(14) 0.0059(10) -0.0087(11) -0.0078(11) C36 0.0300(14) 0.0225(13) 0.0291(14) 0.0040(10) -0.0068(11) -0.0092(11) C37 0.0302(14) 0.0232(13) 0.0299(14) 0.0028(11) -0.0074(11) -0.0050(11) C38 0.0373(15) 0.0202(13) 0.0266(13) 0.0003(10) -0.0082(11) -0.0100(11) C39 0.0425(16) 0.0239(14) 0.0336(15) 0.0023(11) -0.0112(12) -0.0114(12) C40 0.0426(16) 0.0252(14) 0.0402(16) 0.0023(12) -0.0123(13) -0.0104(12) C41 0.0446(17) 0.0213(13) 0.0420(16) 0.0054(12) -0.0166(13) -0.0056(12) C42 0.0430(18) 0.0346(17) 0.085(2) 0.0168(16) -0.0010(17) -0.0103(14) C43 0.0385(18) 0.0273(16) 0.098(3) 0.0128(16) -0.0099(17) -0.0002(13) C44 0.0395(16) 0.0232(14) 0.0455(16) 0.0050(12) -0.0175(13) -0.0087(12) C45 0.0374(16) 0.0261(14) 0.0494(17) 0.0096(12) -0.0142(13) -0.0070(12) C46 0.0356(16) 0.0266(14) 0.0511(17) 0.0090(13) -0.0139(13) -0.0045(12) C47 0.0364(16) 0.0258(15) 0.0511(17) 0.0050(13) -0.0207(13) -0.0055(12) C48 0.0382(16) 0.0248(14) 0.0395(16) 0.0015(12) -0.0161(13) -0.0033(12) C49 0.0385(16) 0.0385(16) 0.0582(19) -0.0007(14) -0.0282(15) -0.0012(13) C50 0.0340(16) 0.0466(18) 0.0553(19) 0.0012(15) -0.0199(14) 0.0036(13) C51 0.0416(17) 0.0376(16) 0.0425(17) 0.0043(13) -0.0128(13) 0.0027(13) C52 0.055(2) 0.0463(19) 0.0494(19) -0.0033(15) -0.0248(16) 0.0119(15) C53 0.091(3) 0.0423(19) 0.062(2) 0.0001(16) -0.046(2) 0.0030(18) C54 0.134(4) 0.046(2) 0.098(3) -0.007(2) -0.068(3) 0.016(2) C55 0.0342(15) 0.0297(14) 0.0467(17) 0.0085(12) -0.0147(13) -0.0103(12) C56 0.0388(16) 0.0279(14) 0.0484(17) 0.0094(12) -0.0181(13) -0.0089(12) C57 0.0411(17) 0.0310(15) 0.0456(17) 0.0065(13) -0.0149(13) -0.0076(12) C58 0.0415(16) 0.0309(15) 0.0438(17) 0.0088(13) -0.0117(13) -0.0095(12) C59 0.0524(18) 0.0302(15) 0.0427(17) 0.0082(13) -0.0136(14) -0.0137(13) C60 0.071(2) 0.0352(17) 0.063(2) 0.0118(15) -0.0232(18) -0.0168(16) C61 0.0311(14) 0.0294(14) 0.0385(15) 0.0084(12) -0.0087(12) -0.0121(11) C62 0.0258(14) 0.0319(14) 0.0373(15) 0.0019(12) -0.0065(11) -0.0092(11) C63 0.0290(14) 0.0293(14) 0.0345(15) 0.0003(11) -0.0061(11) -0.0069(11) C64 0.0318(15) 0.0278(14) 0.0392(15) 0.0012(12) -0.0046(12) -0.0095(11) C65 0.0411(17) 0.0359(16) 0.0487(17) 0.0085(13) -0.0099(14) -0.0160(13) C66 0.0457(19) 0.0447(18) 0.065(2) 0.0123(16) -0.0027(16) -0.0244(15) C67 0.0328(15) 0.0263(14) 0.0433(16) 0.0065(12) -0.0133(12) -0.0074(11) C68 0.0282(14) 0.0320(14) 0.0412(16) 0.0033(12) -0.0111(12) -0.0073(11) C69 0.0349(15) 0.0325(15) 0.0434(16) 0.0033(12) -0.0127(13) -0.0085(12) C70 0.0374(16) 0.0339(15) 0.0441(16) -0.0020(13) -0.0163(13) -0.0033(12) C71 0.066(2) 0.0295(16) 0.060(2) 0.0015(14) -0.0312(17) -0.0002(14) C72 0.101(3) 0.046(2) 0.123(3) 0.001(2) -0.079(3) 0.004(2) C73 0.0277(14) 0.0294(14) 0.0392(15) 0.0050(12) -0.0116(12) -0.0050(11) C74 0.0339(15) 0.0270(14) 0.0331(15) 0.0050(11) -0.0086(12) -0.0078(11) C75 0.0352(15) 0.0270(14) 0.0374(15) 0.0028(12) -0.0122(12) -0.0065(11) C76 0.0302(14) 0.0256(13) 0.0327(14) 0.0031(11) -0.0098(11) -0.0064(11) C77 0.0368(15) 0.0271(14) 0.0386(15) 0.0052(12) -0.0129(12) -0.0074(12) C78 0.0373(16) 0.0317(15) 0.0461(17) 0.0057(13) -0.0124(13) -0.0069(12) C79 0.0253(14) 0.0344(15) 0.0521(17) 0.0042(13) -0.0135(13) -0.0053(12) C80 0.0239(14) 0.0452(17) 0.0532(18) 0.0043(14) -0.0088(13) -0.0126(12) C81 0.0408(16) 0.0473(17) 0.0391(16) 0.0119(13) -0.0135(13) -0.0209(13) C82 0.0336(15) 0.0413(16) 0.0513(18) 0.0119(14) -0.0179(13) -0.0148(13) C83 0.060(2) 0.0508(19) 0.0513(19) 0.0088(15) -0.0173(16) -0.0240(16) C84 0.076(2) 0.0448(19) 0.083(3) 0.0113(17) -0.032(2) -0.0306(18) O1 0.0285(10) 0.0305(10) 0.0473(11) 0.0038(8) -0.0142(9) 0.0010(8) O2 0.0317(10) 0.0261(9) 0.0555(12) 0.0150(9) -0.0171(9) -0.0068(8) O3 0.0225(9) 0.0336(10) 0.0558(12) 0.0158(9) -0.0114(8) -0.0114(8) O4 0.0245(10) 0.0304(10) 0.0529(12) 0.0131(9) -0.0124(8) -0.0079(8) O5 0.0265(10) 0.0257(9) 0.0472(11) 0.0143(8) -0.0100(8) -0.0071(7) O6 0.0246(9) 0.0307(10) 0.0429(11) 0.0124(8) -0.0087(8) -0.0091(8) C85 0.061(2) 0.052(2) 0.048(2) -0.0068(16) -0.0181(16) -0.0057(16) C86 0.059(2) 0.060(2) 0.0379(17) 0.0022(16) -0.0088(15) -0.0116(17) O7 0.0656(14) 0.0414(12) 0.0554(14) 0.0077(10) -0.0201(11) -0.0079(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.392(3) . ? C1 C6 1.411(3) . ? C1 C48 1.435(3) . ? C2 C3 1.377(3) . ? C2 H2 0.9500 . ? C3 O1 1.381(3) . ? C3 C4 1.400(3) . ? C4 O2 1.365(3) . ? C4 C5 1.371(3) . ? C5 C6 1.403(3) . ? C5 H5 0.9500 . ? C6 C7 1.427(3) . ? C7 C8 1.198(3) . ? C8 C9 1.430(3) . ? C9 C14 1.388(3) . ? C9 C10 1.391(3) . ? C10 C11 1.372(4) . ? C10 H10 0.9500 . ? C11 C12 1.390(3) . ? C11 H11 0.9500 . ? C12 C13 1.400(3) . ? C12 C15 1.430(3) . ? C13 C14 1.371(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.194(3) . ? C16 C17 1.427(3) . ? C17 C22 1.400(3) . ? C17 C18 1.414(3) . ? C18 C19 1.379(3) . ? C18 H18 0.9500 . ? C19 O3 1.355(3) . ? C19 C20 1.405(3) . ? C20 O4 1.363(3) . ? C20 C21 1.380(3) . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 C23 1.427(3) . ? C23 C24 1.196(3) . ? C24 C25 1.433(3) . ? C25 C26 1.389(3) . ? C25 C30 1.389(3) . ? C26 C27 1.375(3) . ? C26 H26 0.9500 . ? C27 C28 1.394(3) . ? C27 H27 0.9500 . ? C28 C29 1.396(3) . ? C28 C31 1.429(3) . ? C29 C30 1.382(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.189(3) . ? C32 C33 1.440(3) . ? C33 C38 1.385(3) . ? C33 C34 1.400(3) . ? C34 C35 1.379(3) . ? C34 H34 0.9500 . ? C35 O5 1.364(3) . ? C35 C36 1.406(3) . ? C36 O6 1.367(3) . ? C36 C37 1.376(3) . ? C37 C38 1.414(3) . ? C37 H37 0.9500 . ? C38 C39 1.433(3) . ? C39 C40 1.193(3) . ? C40 C41 1.442(3) . ? C41 C42 1.383(4) . ? C41 C46 1.388(4) . ? C42 C43 1.381(4) . ? C42 H42 0.9500 . ? C43 C44 1.380(4) . ? C43 H43 0.9500 . ? C44 C45 1.381(4) . ? C44 C47 1.443(3) . ? C45 C46 1.378(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.192(3) . ? C49 O1 1.446(3) . ? C49 C50 1.508(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.508(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.529(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.512(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.516(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 O2 1.438(3) . ? C55 C56 1.504(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.526(3) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.514(3) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.519(3) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.518(4) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 O3 1.432(3) . ? C61 C62 1.502(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.517(3) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.512(3) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.517(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.522(4) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 O4 1.433(3) . ? C67 C68 1.506(3) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.525(3) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.512(3) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.518(4) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.513(4) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 O5 1.432(3) . ? C73 C74 1.512(3) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.523(3) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.525(3) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.517(3) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.523(3) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 O6 1.430(3) . ? C79 C80 1.513(3) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.513(4) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.529(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.511(4) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.532(4) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 O7 1.401(3) . ? C85 C86 1.514(4) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 O7 1.426(3) 2_676 ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? O7 C86 1.426(3) 2_676 ? 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_3 _geom_angle_publ_flag C2 C1 C6 118.6(2) . . ? C2 C1 C48 121.3(2) . . ? C6 C1 C48 120.1(2) . . ? C3 C2 C1 121.6(2) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 O1 120.3(2) . . ? C2 C3 C4 119.8(2) . . ? O1 C3 C4 119.8(2) . . ? O2 C4 C5 125.0(2) . . ? O2 C4 C3 115.4(2) . . ? C5 C4 C3 119.6(2) . . ? C4 C5 C6 121.1(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 119.3(2) . . ? C5 C6 C7 119.1(2) . . ? C1 C6 C7 121.6(2) . . ? C8 C7 C6 177.5(3) . . ? C7 C8 C9 179.0(3) . . ? C14 C9 C10 118.5(2) . . ? C14 C9 C8 121.1(2) . . ? C10 C9 C8 120.5(2) . . ? C11 C10 C9 120.9(2) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 120.8(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C13 118.1(2) . . ? C11 C12 C15 122.4(2) . . ? C13 C12 C15 119.4(2) . . ? C14 C13 C12 120.8(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C9 120.8(2) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? C16 C15 C12 176.3(3) . . ? C15 C16 C17 175.8(3) . . ? C22 C17 C18 119.1(2) . . ? C22 C17 C16 119.7(2) . . ? C18 C17 C16 121.2(2) . . ? C19 C18 C17 120.3(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? O3 C19 C18 124.9(2) . . ? O3 C19 C20 114.8(2) . . ? C18 C19 C20 120.2(2) . . ? O4 C20 C21 124.6(2) . . ? O4 C20 C19 115.8(2) . . ? C21 C20 C19 119.6(2) . . ? C20 C21 C22 120.9(2) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C17 119.8(2) . . ? C21 C22 C23 118.6(2) . . ? C17 C22 C23 121.5(2) . . ? C24 C23 C22 176.6(3) . . ? C23 C24 C25 176.2(3) . . ? C26 C25 C30 118.5(2) . . ? C26 C25 C24 120.3(2) . . ? C30 C25 C24 121.1(2) . . ? C27 C26 C25 121.0(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.6(2) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 118.6(2) . . ? C27 C28 C31 120.9(2) . . ? C29 C28 C31 120.5(2) . . ? C30 C29 C28 120.3(2) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 120.9(2) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C32 C31 C28 179.5(3) . . ? C31 C32 C33 179.4(3) . . ? C38 C33 C34 120.3(2) . . ? C38 C33 C32 120.4(2) . . ? C34 C33 C32 119.3(2) . . ? C35 C34 C33 120.5(2) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? O5 C35 C34 125.4(2) . . ? O5 C35 C36 115.2(2) . . ? C34 C35 C36 119.4(2) . . ? O6 C36 C37 124.5(2) . . ? O6 C36 C35 114.9(2) . . ? C37 C36 C35 120.6(2) . . ? C36 C37 C38 120.0(2) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C33 C38 C37 119.3(2) . . ? C33 C38 C39 120.6(2) . . ? C37 C38 C39 120.1(2) . . ? C40 C39 C38 175.5(3) . . ? C39 C40 C41 178.2(3) . . ? C42 C41 C46 118.5(2) . . ? C42 C41 C40 120.9(3) . . ? C46 C41 C40 120.7(2) . . ? C43 C42 C41 119.9(3) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C42 121.7(3) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C43 C44 C45 118.3(2) . . ? C43 C44 C47 120.8(2) . . ? C45 C44 C47 120.9(2) . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 121.2(2) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? C48 C47 C44 178.2(3) . . ? C47 C48 C1 179.3(3) . . ? O1 C49 C50 109.7(2) . . ? O1 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? O1 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? C51 C50 C49 114.0(2) . . ? C51 C50 H50A 108.8 . . ? C49 C50 H50A 108.8 . . ? C51 C50 H50B 108.8 . . ? C49 C50 H50B 108.8 . . ? H50A C50 H50B 107.6 . . ? C50 C51 C52 113.5(2) . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51B 108.9 . . ? C52 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C53 C52 C51 113.4(3) . . ? C53 C52 H52A 108.9 . . ? C51 C52 H52A 108.9 . . ? C53 C52 H52B 108.9 . . ? C51 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? C52 C53 C54 113.8(3) . . ? C52 C53 H53A 108.8 . . ? C54 C53 H53A 108.8 . . ? C52 C53 H53B 108.8 . . ? C54 C53 H53B 108.8 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O2 C55 C56 107.4(2) . . ? O2 C55 H55A 110.2 . . ? C56 C55 H55A 110.2 . . ? O2 C55 H55B 110.2 . . ? C56 C55 H55B 110.2 . . ? H55A C55 H55B 108.5 . . ? C55 C56 C57 112.0(2) . . ? C55 C56 H56A 109.2 . . ? C57 C56 H56A 109.2 . . ? C55 C56 H56B 109.2 . . ? C57 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? C58 C57 C56 112.8(2) . . ? C58 C57 H57A 109.0 . . ? C56 C57 H57A 109.0 . . ? C58 C57 H57B 109.0 . . ? C56 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? C57 C58 C59 113.9(2) . . ? C57 C58 H58A 108.8 . . ? C59 C58 H58A 108.8 . . ? C57 C58 H58B 108.8 . . ? C59 C58 H58B 108.8 . . ? H58A C58 H58B 107.7 . . ? C60 C59 C58 112.9(2) . . ? C60 C59 H59A 109.0 . . ? C58 C59 H59A 109.0 . . ? C60 C59 H59B 109.0 . . ? C58 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O3 C61 C62 106.91(19) . . ? O3 C61 H61A 110.3 . . ? C62 C61 H61A 110.3 . . ? O3 C61 H61B 110.3 . . ? C62 C61 H61B 110.3 . . ? H61A C61 H61B 108.6 . . ? C61 C62 C63 112.3(2) . . ? C61 C62 H62A 109.1 . . ? C63 C62 H62A 109.1 . . ? C61 C62 H62B 109.1 . . ? C63 C62 H62B 109.1 . . ? H62A C62 H62B 107.9 . . ? C64 C63 C62 112.9(2) . . ? C64 C63 H63A 109.0 . . ? C62 C63 H63A 109.0 . . ? C64 C63 H63B 109.0 . . ? C62 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? C63 C64 C65 113.4(2) . . ? C63 C64 H64A 108.9 . . ? C65 C64 H64A 108.9 . . ? C63 C64 H64B 108.9 . . ? C65 C64 H64B 108.9 . . ? H64A C64 H64B 107.7 . . ? C64 C65 C66 113.6(2) . . ? C64 C65 H65A 108.8 . . ? C66 C65 H65A 108.8 . . ? C64 C65 H65B 108.8 . . ? C66 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O4 C67 C68 110.1(2) . . ? O4 C67 H67A 109.6 . . ? C68 C67 H67A 109.6 . . ? O4 C67 H67B 109.6 . . ? C68 C67 H67B 109.6 . . ? H67A C67 H67B 108.2 . . ? C67 C68 C69 108.2(2) . . ? C67 C68 H68A 110.1 . . ? C69 C68 H68A 110.1 . . ? C67 C68 H68B 110.1 . . ? C69 C68 H68B 110.1 . . ? H68A C68 H68B 108.4 . . ? C70 C69 C68 115.4(2) . . ? C70 C69 H69A 108.4 . . ? C68 C69 H69A 108.4 . . ? C70 C69 H69B 108.4 . . ? C68 C69 H69B 108.4 . . ? H69A C69 H69B 107.5 . . ? C69 C70 C71 112.5(2) . . ? C69 C70 H70A 109.1 . . ? C71 C70 H70A 109.1 . . ? C69 C70 H70B 109.1 . . ? C71 C70 H70B 109.1 . . ? H70A C70 H70B 107.8 . . ? C72 C71 C70 113.1(3) . . ? C72 C71 H71A 109.0 . . ? C70 C71 H71A 109.0 . . ? C72 C71 H71B 109.0 . . ? C70 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O5 C73 C74 107.02(19) . . ? O5 C73 H73A 110.3 . . ? C74 C73 H73A 110.3 . . ? O5 C73 H73B 110.3 . . ? C74 C73 H73B 110.3 . . ? H73A C73 H73B 108.6 . . ? C73 C74 C75 112.0(2) . . ? C73 C74 H74A 109.2 . . ? C75 C74 H74A 109.2 . . ? C73 C74 H74B 109.2 . . ? C75 C74 H74B 109.2 . . ? H74A C74 H74B 107.9 . . ? C74 C75 C76 112.3(2) . . ? C74 C75 H75A 109.1 . . ? C76 C75 H75A 109.1 . . ? C74 C75 H75B 109.1 . . ? C76 C75 H75B 109.1 . . ? H75A C75 H75B 107.9 . . ? C77 C76 C75 113.4(2) . . ? C77 C76 H76A 108.9 . . ? C75 C76 H76A 108.9 . . ? C77 C76 H76B 108.9 . . ? C75 C76 H76B 108.9 . . ? H76A C76 H76B 107.7 . . ? C76 C77 C78 112.7(2) . . ? C76 C77 H77A 109.0 . . ? C78 C77 H77A 109.0 . . ? C76 C77 H77B 109.0 . . ? C78 C77 H77B 109.0 . . ? H77A C77 H77B 107.8 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O6 C79 C80 107.0(2) . . ? O6 C79 H79A 110.3 . . ? C80 C79 H79A 110.3 . . ? O6 C79 H79B 110.3 . . ? C80 C79 H79B 110.3 . . ? H79A C79 H79B 108.6 . . ? C81 C80 C79 113.1(2) . . ? C81 C80 H80A 109.0 . . ? C79 C80 H80A 109.0 . . ? C81 C80 H80B 109.0 . . ? C79 C80 H80B 109.0 . . ? H80A C80 H80B 107.8 . . ? C80 C81 C82 113.9(2) . . ? C80 C81 H81A 108.8 . . ? C82 C81 H81A 108.8 . . ? C80 C81 H81B 108.8 . . ? C82 C81 H81B 108.8 . . ? H81A C81 H81B 107.7 . . ? C83 C82 C81 112.8(2) . . ? C83 C82 H82A 109.0 . . ? C81 C82 H82A 109.0 . . ? C83 C82 H82B 109.0 . . ? C81 C82 H82B 109.0 . . ? H82A C82 H82B 107.8 . . ? C82 C83 C84 113.1(3) . . ? C82 C83 H83A 109.0 . . ? C84 C83 H83A 109.0 . . ? C82 C83 H83B 109.0 . . ? C84 C83 H83B 109.0 . . ? H83A C83 H83B 107.8 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C3 O1 C49 115.46(19) . . ? C4 O2 C55 117.95(19) . . ? C19 O3 C61 118.19(18) . . ? C20 O4 C67 115.74(18) . . ? C35 O5 C73 117.76(18) . . ? C36 O6 C79 117.92(18) . . ? O7 C85 C86 110.3(3) . . ? O7 C85 H85A 109.6 . . ? C86 C85 H85A 109.6 . . ? O7 C85 H85B 109.6 . . ? C86 C85 H85B 109.6 . . ? H85A C85 H85B 108.1 . . ? O7 C86 C85 110.2(2) 2_676 . ? O7 C86 H86A 109.6 2_676 . ? C85 C86 H86A 109.6 . . ? O7 C86 H86B 109.6 2_676 . ? C85 C86 H86B 109.6 . . ? H86A C86 H86B 108.1 . . ? C85 O7 C86 108.8(2) . 2_676 ? 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 C6 C1 C2 C3 -0.1(4) . . . . ? C48 C1 C2 C3 179.2(2) . . . . ? C1 C2 C3 O1 -174.3(2) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C2 C3 C4 O2 179.7(2) . . . . ? O1 C3 C4 O2 -4.6(3) . . . . ? C2 C3 C4 C5 -1.3(4) . . . . ? O1 C3 C4 C5 174.4(2) . . . . ? O2 C4 C5 C6 179.0(2) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 C1 1.1(4) . . . . ? C4 C5 C6 C7 -177.7(2) . . . . ? C2 C1 C6 C5 -1.1(3) . . . . ? C48 C1 C6 C5 179.6(2) . . . . ? C2 C1 C6 C7 177.7(2) . . . . ? C48 C1 C6 C7 -1.7(4) . . . . ? C5 C6 C7 C8 35(7) . . . . ? C1 C6 C7 C8 -144(6) . . . . ? C6 C7 C8 C9 178(100) . . . . ? C7 C8 C9 C14 -47(17) . . . . ? C7 C8 C9 C10 133(16) . . . . ? C14 C9 C10 C11 2.3(4) . . . . ? C8 C9 C10 C11 -177.9(2) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C10 C11 C12 C13 -0.9(4) . . . . ? C10 C11 C12 C15 177.9(3) . . . . ? C11 C12 C13 C14 1.4(4) . . . . ? C15 C12 C13 C14 -177.5(2) . . . . ? C12 C13 C14 C9 0.0(4) . . . . ? C10 C9 C14 C13 -1.8(4) . . . . ? C8 C9 C14 C13 178.3(2) . . . . ? C11 C12 C15 C16 -156(4) . . . . ? C13 C12 C15 C16 22(5) . . . . ? C12 C15 C16 C17 5(8) . . . . ? C15 C16 C17 C22 -8(4) . . . . ? C15 C16 C17 C18 172(4) . . . . ? C22 C17 C18 C19 -0.1(4) . . . . ? C16 C17 C18 C19 -179.5(2) . . . . ? C17 C18 C19 O3 179.1(2) . . . . ? C17 C18 C19 C20 -0.7(4) . . . . ? O3 C19 C20 O4 0.3(3) . . . . ? C18 C19 C20 O4 -179.9(2) . . . . ? O3 C19 C20 C21 -179.2(2) . . . . ? C18 C19 C20 C21 0.7(4) . . . . ? O4 C20 C21 C22 -179.2(2) . . . . ? C19 C20 C21 C22 0.2(4) . . . . ? C20 C21 C22 C17 -1.1(4) . . . . ? C20 C21 C22 C23 177.9(2) . . . . ? C18 C17 C22 C21 1.0(4) . . . . ? C16 C17 C22 C21 -179.7(2) . . . . ? C18 C17 C22 C23 -177.9(2) . . . . ? C16 C17 C22 C23 1.4(4) . . . . ? C21 C22 C23 C24 -11(5) . . . . ? C17 C22 C23 C24 168(5) . . . . ? C22 C23 C24 C25 58(8) . . . . ? C23 C24 C25 C26 -65(4) . . . . ? C23 C24 C25 C30 113(4) . . . . ? C30 C25 C26 C27 -2.2(4) . . . . ? C24 C25 C26 C27 175.1(2) . . . . ? C25 C26 C27 C28 0.2(4) . . . . ? C26 C27 C28 C29 1.7(4) . . . . ? C26 C27 C28 C31 -177.6(2) . . . . ? C27 C28 C29 C30 -1.7(4) . . . . ? C31 C28 C29 C30 177.6(2) . . . . ? C28 C29 C30 C25 -0.3(4) . . . . ? C26 C25 C30 C29 2.2(4) . . . . ? C24 C25 C30 C29 -175.0(2) . . . . ? C27 C28 C31 C32 108(43) . . . . ? C29 C28 C31 C32 -72(43) . . . . ? C28 C31 C32 C33 172(100) . . . . ? C31 C32 C33 C38 -77(29) . . . . ? C31 C32 C33 C34 101(29) . . . . ? C38 C33 C34 C35 -0.4(4) . . . . ? C32 C33 C34 C35 -179.1(2) . . . . ? C33 C34 C35 O5 179.9(2) . . . . ? C33 C34 C35 C36 0.3(4) . . . . ? O5 C35 C36 O6 0.6(3) . . . . ? C34 C35 C36 O6 -179.8(2) . . . . ? O5 C35 C36 C37 -179.5(2) . . . . ? C34 C35 C36 C37 0.0(4) . . . . ? O6 C36 C37 C38 179.5(2) . . . . ? C35 C36 C37 C38 -0.3(4) . . . . ? C34 C33 C38 C37 0.1(4) . . . . ? C32 C33 C38 C37 178.9(2) . . . . ? C34 C33 C38 C39 179.2(2) . . . . ? C32 C33 C38 C39 -2.1(4) . . . . ? C36 C37 C38 C33 0.2(3) . . . . ? C36 C37 C38 C39 -178.8(2) . . . . ? C33 C38 C39 C40 -24(4) . . . . ? C37 C38 C39 C40 155(3) . . . . ? C38 C39 C40 C41 29(12) . . . . ? C39 C40 C41 C42 -167(9) . . . . ? C39 C40 C41 C46 14(9) . . . . ? C46 C41 C42 C43 0.2(5) . . . . ? C40 C41 C42 C43 -179.0(3) . . . . ? C41 C42 C43 C44 1.5(5) . . . . ? C42 C43 C44 C45 -2.6(5) . . . . ? C42 C43 C44 C47 177.0(3) . . . . ? C43 C44 C45 C46 2.0(4) . . . . ? C47 C44 C45 C46 -177.6(2) . . . . ? C44 C45 C46 C41 -0.4(4) . . . . ? C42 C41 C46 C45 -0.8(4) . . . . ? C40 C41 C46 C45 178.5(2) . . . . ? C43 C44 C47 C48 -60(10) . . . . ? C45 C44 C47 C48 119(10) . . . . ? C44 C47 C48 C1 177(100) . . . . ? C2 C1 C48 C47 -135(32) . . . . ? C6 C1 C48 C47 44(32) . . . . ? O1 C49 C50 C51 74.0(3) . . . . ? C49 C50 C51 C52 177.4(2) . . . . ? C50 C51 C52 C53 -179.0(3) . . . . ? C51 C52 C53 C54 177.9(3) . . . . ? O2 C55 C56 C57 179.3(2) . . . . ? C55 C56 C57 C58 -175.5(2) . . . . ? C56 C57 C58 C59 176.5(2) . . . . ? C57 C58 C59 C60 -179.9(2) . . . . ? O3 C61 C62 C63 173.7(2) . . . . ? C61 C62 C63 C64 -179.3(2) . . . . ? C62 C63 C64 C65 -173.8(2) . . . . ? C63 C64 C65 C66 174.5(2) . . . . ? O4 C67 C68 C69 -177.9(2) . . . . ? C67 C68 C69 C70 179.4(2) . . . . ? C68 C69 C70 C71 174.7(2) . . . . ? C69 C70 C71 C72 -178.4(3) . . . . ? O5 C73 C74 C75 -179.1(2) . . . . ? C73 C74 C75 C76 179.6(2) . . . . ? C74 C75 C76 C77 -176.0(2) . . . . ? C75 C76 C77 C78 179.9(2) . . . . ? O6 C79 C80 C81 -65.1(3) . . . . ? C79 C80 C81 C82 -175.5(2) . . . . ? C80 C81 C82 C83 -177.6(2) . . . . ? C81 C82 C83 C84 -178.3(2) . . . . ? C2 C3 O1 C49 -104.3(3) . . . . ? C4 C3 O1 C49 80.0(3) . . . . ? C50 C49 O1 C3 -152.7(2) . . . . ? C5 C4 O2 C55 -1.7(4) . . . . ? C3 C4 O2 C55 177.3(2) . . . . ? C56 C55 O2 C4 -179.4(2) . . . . ? C18 C19 O3 C61 -4.1(4) . . . . ? C20 C19 O3 C61 175.7(2) . . . . ? C62 C61 O3 C19 -177.3(2) . . . . ? C21 C20 O4 C67 -3.9(4) . . . . ? C19 C20 O4 C67 176.7(2) . . . . ? C68 C67 O4 C20 -177.8(2) . . . . ? C34 C35 O5 C73 -2.2(3) . . . . ? C36 C35 O5 C73 177.4(2) . . . . ? C74 C73 O5 C35 -179.0(2) . . . . ? C37 C36 O6 C79 5.8(3) . . . . ? C35 C36 O6 C79 -174.4(2) . . . . ? C80 C79 O6 C36 170.1(2) . . . . ? O7 C85 C86 O7 -59.9(3) . . . 2_676 ? C86 C85 O7 C86 59.0(3) . . . 2_676 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.363 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.056