# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jun-Li Hou' _publ_contact_author_email houjl@fudan.edu.cn loop_ _publ_author_name 'Jun-Li Hou' 'Xiao-Bo Hu' 'Zhenxia Chen' 'Lei Chen' 'Ling Zhang' 'Zhan-Ting Li' data_m11231d _database_code_depnum_ccdc_archive 'CCDC 896136' #TrackingRef '- PA[8].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H112 O16' _chemical_formula_weight 1425.78 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5582(15) _cell_length_b 23.309(3) _cell_length_c 34.534(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.489(2) _cell_angle_gamma 90.00 _cell_volume 9261(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7398 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.90 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9829 _exptl_absorpt_correction_T_max 0.9863 _exptl_absorpt_process_details sadabs _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 APEX-II CCD' _diffrn_measurement_method '\f and \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 55205 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.01 _reflns_number_total 16296 _reflns_number_gt 8627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1031P)^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 16296 _refine_ls_number_parameters 953 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _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 O1 O 1.27536(17) 1.03679(8) 0.47100(6) 0.0413(5) Uani 1 1 d . . . O2 O 0.96711(18) 0.85457(9) 0.46633(6) 0.0450(5) Uani 1 1 d . . . O3 O 1.39298(19) 0.81661(8) 0.46393(5) 0.0432(5) Uani 1 1 d . . . O4 O 1.52129(19) 0.98815(9) 0.36551(5) 0.0461(6) Uani 1 1 d . . . O5 O 1.3755(2) 0.78654(9) 0.31915(6) 0.0510(6) Uani 1 1 d . . . O6 O 1.25582(19) 0.99148(9) 0.24615(6) 0.0460(5) Uani 1 1 d . . . O7 O 1.0652(2) 0.79591(9) 0.19981(6) 0.0524(6) Uani 1 1 d . . . O8 O 1.11310(19) 0.97455(9) 0.09742(6) 0.0509(6) Uani 1 1 d . . . O9 O 0.89066(18) 0.78246(9) 0.05636(6) 0.0448(5) Uani 1 1 d . . . O10 O 0.73790(16) 1.00324(8) 0.02202(6) 0.0402(5) Uani 1 1 d . . . O11 O 0.47476(17) 0.82860(8) 0.05929(5) 0.0376(5) Uani 1 1 d . . . O12 O 0.47885(19) 1.04277(8) 0.12858(6) 0.0442(5) Uani 1 1 d . . . O13 O 0.47590(18) 0.84385(9) 0.20471(5) 0.0435(5) Uani 1 1 d . . . O14 O 0.7722(2) 1.02489(10) 0.24605(7) 0.0622(7) Uani 1 1 d . . . O15 O 0.79616(18) 0.83292(8) 0.32738(6) 0.0439(5) Uani 1 1 d . . . O16 O 0.9067(2) 1.04768(9) 0.38784(6) 0.0545(6) Uani 1 1 d . . . C1 C 1.1960(2) 0.99216(12) 0.46939(7) 0.0311(7) Uani 1 1 d . . . C2 C 1.0787(3) 0.99873(12) 0.45793(7) 0.0340(7) Uani 1 1 d . . . H2 H 1.0497 1.0358 0.4509 0.041 Uiso 1 1 calc R . . C3 C 1.0025(2) 0.95267(12) 0.45644(7) 0.0322(7) Uani 1 1 d . . . C4 C 1.0461(3) 0.89897(13) 0.46812(8) 0.0351(7) Uani 1 1 d . . . C5 C 1.1646(3) 0.89273(13) 0.47993(7) 0.0357(7) Uani 1 1 d . . . H5 H 1.1934 0.8560 0.4880 0.043 Uiso 1 1 calc R . . C6 C 1.2414(2) 0.93865(12) 0.48025(7) 0.0312(7) Uani 1 1 d . . . C7 C 1.2331(3) 1.09381(12) 0.46471(9) 0.0421(8) Uani 1 1 d . . . H7A H 1.1723 1.1024 0.4822 0.050 Uiso 1 1 calc R . . H7B H 1.1994 1.0986 0.4375 0.050 Uiso 1 1 calc R . . C8 C 1.3359(3) 1.13311(15) 0.47329(13) 0.0746(12) Uani 1 1 d . . . H8A H 1.3638 1.1305 0.5009 0.112 Uiso 1 1 calc R . . H8B H 1.3126 1.1727 0.4670 0.112 Uiso 1 1 calc R . . H8C H 1.3983 1.1217 0.4576 0.112 Uiso 1 1 calc R . . C9 C 1.0083(3) 0.79900(13) 0.47846(10) 0.0525(9) Uani 1 1 d . . . H9A H 1.0375 0.7995 0.5064 0.063 Uiso 1 1 calc R . . H9B H 1.0723 0.7868 0.4632 0.063 Uiso 1 1 calc R . . C10 C 0.9060(3) 0.75831(15) 0.47155(12) 0.0693(11) Uani 1 1 d . . . H10A H 0.8410 0.7726 0.4851 0.104 Uiso 1 1 calc R . . H10B H 0.9287 0.7202 0.4815 0.104 Uiso 1 1 calc R . . H10C H 0.8821 0.7558 0.4436 0.104 Uiso 1 1 calc R . . C11 C 1.3711(2) 0.92945(13) 0.48897(7) 0.0350(7) Uani 1 1 d . . . H11A H 1.4076 0.9648 0.5003 0.042 Uiso 1 1 calc R . . H11B H 1.3855 0.8981 0.5081 0.042 Uiso 1 1 calc R . . C12 C 1.4242(2) 0.91428(12) 0.45190(7) 0.0314(7) Uani 1 1 d . . . C13 C 1.4595(3) 0.95798(12) 0.42799(8) 0.0353(7) Uani 1 1 d . . . H13 H 1.4600 0.9965 0.4369 0.042 Uiso 1 1 calc R . . C14 C 1.4937(2) 0.94603(12) 0.39151(8) 0.0337(7) Uani 1 1 d . . . C15 C 1.4950(2) 0.88949(12) 0.37799(7) 0.0314(7) Uani 1 1 d . . . C16 C 1.4645(2) 0.84632(12) 0.40251(8) 0.0340(7) Uani 1 1 d . . . H16 H 1.4683 0.8075 0.3942 0.041 Uiso 1 1 calc R . . C17 C 1.4286(2) 0.85816(12) 0.43887(8) 0.0328(7) Uani 1 1 d . . . C18 C 1.3946(3) 0.75820(13) 0.45291(9) 0.0529(9) Uani 1 1 d . . . H18A H 1.3673 0.7551 0.4249 0.064 Uiso 1 1 calc R . . H18B H 1.3393 0.7367 0.4677 0.064 Uiso 1 1 calc R . . C19 C 1.5119(4) 0.73090(17) 0.45981(11) 0.0817(13) Uani 1 1 d . . . H19A H 1.5636 0.7471 0.4417 0.123 Uiso 1 1 calc R . . H19B H 1.5047 0.6894 0.4556 0.123 Uiso 1 1 calc R . . H19C H 1.5443 0.7383 0.4866 0.123 Uiso 1 1 calc R . . C20 C 1.5681(3) 1.04047(13) 0.37978(9) 0.0479(8) Uani 1 1 d . . . H20A H 1.6400 1.0337 0.3971 0.057 Uiso 1 1 calc R . . H20B H 1.5116 1.0608 0.3947 0.057 Uiso 1 1 calc R . . C21 C 1.5940(3) 1.07539(14) 0.34523(10) 0.0582(10) Uani 1 1 d . . . H21A H 1.6426 1.0530 0.3291 0.087 Uiso 1 1 calc R . . H21B H 1.6354 1.1104 0.3541 0.087 Uiso 1 1 calc R . . H21C H 1.5211 1.0856 0.3300 0.087 Uiso 1 1 calc R . . C22 C 1.5234(2) 0.87716(13) 0.33663(8) 0.0361(7) Uani 1 1 d . . . H22A H 1.5834 0.9045 0.3295 0.043 Uiso 1 1 calc R . . H22B H 1.5554 0.8379 0.3354 0.043 Uiso 1 1 calc R . . C23 C 1.4172(2) 0.88239(12) 0.30797(7) 0.0305(7) Uani 1 1 d . . . C24 C 1.3897(2) 0.93419(12) 0.28946(7) 0.0317(7) Uani 1 1 d . . . H24 H 1.4410 0.9659 0.2939 0.038 Uiso 1 1 calc R . . C25 C 1.2881(3) 0.94071(12) 0.26444(7) 0.0317(7) Uani 1 1 d . . . C26 C 1.2131(2) 0.89515(13) 0.25730(7) 0.0324(7) Uani 1 1 d . . . C27 C 1.2405(3) 0.84319(13) 0.27500(8) 0.0370(7) Uani 1 1 d . . . H27 H 1.1899 0.8114 0.2700 0.044 Uiso 1 1 calc R . . C28 C 1.3419(3) 0.83667(12) 0.30022(7) 0.0361(7) Uani 1 1 d . . . C29 C 1.3030(3) 0.73716(13) 0.31362(9) 0.0554(10) Uani 1 1 d . . . H29A H 1.2935 0.7262 0.2858 0.067 Uiso 1 1 calc R . . H29B H 1.2253 0.7451 0.3222 0.067 Uiso 1 1 calc R . . C30 C 1.3618(4) 0.68991(15) 0.33756(11) 0.0833(14) Uani 1 1 d . . . H30A H 1.4369 0.6812 0.3279 0.125 Uiso 1 1 calc R . . H30B H 1.3127 0.6556 0.3356 0.125 Uiso 1 1 calc R . . H30C H 1.3743 0.7021 0.3648 0.125 Uiso 1 1 calc R . . C31 C 1.3245(3) 1.04125(13) 0.25524(10) 0.0569(10) Uani 1 1 d . . . H31A H 1.4050 1.0352 0.2486 0.068 Uiso 1 1 calc R . . H31B H 1.3269 1.0501 0.2833 0.068 Uiso 1 1 calc R . . C32 C 1.2686(5) 1.08891(17) 0.23173(15) 0.119(2) Uani 1 1 d . . . H32A H 1.2615 1.0783 0.2041 0.178 Uiso 1 1 calc R . . H32B H 1.3162 1.1236 0.2356 0.178 Uiso 1 1 calc R . . H32C H 1.1911 1.0963 0.2400 0.178 Uiso 1 1 calc R . . C33 C 1.0989(3) 0.90287(14) 0.23291(8) 0.0419(8) Uani 1 1 d . . . H33A H 1.0709 0.9423 0.2371 0.050 Uiso 1 1 calc R . . H33B H 1.0419 0.8762 0.2428 0.050 Uiso 1 1 calc R . . C34 C 1.0981(2) 0.89346(13) 0.18914(8) 0.0334(7) Uani 1 1 d . . . C35 C 1.0773(2) 0.83924(13) 0.17345(8) 0.0368(7) Uani 1 1 d . . . C36 C 1.0674(2) 0.83129(13) 0.13312(8) 0.0377(7) Uani 1 1 d . . . H36 H 1.0532 0.7939 0.1228 0.045 Uiso 1 1 calc R . . C37 C 1.0778(2) 0.87678(13) 0.10805(8) 0.0341(7) Uani 1 1 d . . . C38 C 1.1025(2) 0.93069(13) 0.12375(8) 0.0357(7) Uani 1 1 d . . . C39 C 1.1107(2) 0.93851(13) 0.16411(8) 0.0373(7) Uani 1 1 d . . . H39 H 1.1253 0.9758 0.1745 0.045 Uiso 1 1 calc R . . C40 C 1.0342(4) 0.74063(15) 0.18674(10) 0.0712(12) Uani 1 1 d . . . H40A H 1.0986 0.7228 0.1741 0.085 Uiso 1 1 calc R . . H40B H 0.9646 0.7421 0.1677 0.085 Uiso 1 1 calc R . . C41 C 1.0092(6) 0.70686(19) 0.22164(13) 0.132(3) Uani 1 1 d . . . H41A H 1.0772 0.7077 0.2409 0.198 Uiso 1 1 calc R . . H41B H 0.9915 0.6671 0.2140 0.198 Uiso 1 1 calc R . . H41C H 0.9423 0.7236 0.2330 0.198 Uiso 1 1 calc R . . C42 C 1.1578(3) 1.02839(13) 0.11096(9) 0.0489(8) Uani 1 1 d . . . H42A H 1.2324 1.0231 0.1272 0.059 Uiso 1 1 calc R . . H42B H 1.1023 1.0475 0.1269 0.059 Uiso 1 1 calc R . . C43 C 1.1756(4) 1.06438(16) 0.07563(11) 0.0707(11) Uani 1 1 d . . . H43A H 1.2287 1.0445 0.0596 0.106 Uiso 1 1 calc R . . H43B H 1.2091 1.1015 0.0840 0.106 Uiso 1 1 calc R . . H43C H 1.1008 1.0705 0.0604 0.106 Uiso 1 1 calc R . . C44 C 1.0580(2) 0.86815(14) 0.06426(8) 0.0386(7) Uani 1 1 d . . . H44A H 1.0777 0.8282 0.0578 0.046 Uiso 1 1 calc R . . H44B H 1.1100 0.8941 0.0512 0.046 Uiso 1 1 calc R . . C45 C 0.9322(2) 0.88035(13) 0.04925(7) 0.0316(7) Uani 1 1 d . . . C46 C 0.8956(2) 0.93601(12) 0.03997(7) 0.0325(7) Uani 1 1 d . . . H46 H 0.9512 0.9661 0.0408 0.039 Uiso 1 1 calc R . . C47 C 0.7796(2) 0.94843(12) 0.02959(7) 0.0315(7) Uani 1 1 d . . . C48 C 0.6973(2) 0.90509(12) 0.02723(7) 0.0275(6) Uani 1 1 d . . . C49 C 0.7345(2) 0.84898(12) 0.03506(7) 0.0321(7) Uani 1 1 d . . . H49 H 0.6796 0.8186 0.0325 0.039 Uiso 1 1 calc R . . C50 C 0.8502(2) 0.83684(12) 0.04645(7) 0.0324(7) Uani 1 1 d . . . C51 C 0.8085(3) 0.73706(12) 0.05723(8) 0.0407(8) Uani 1 1 d . . . H51A H 0.7708 0.7296 0.0308 0.049 Uiso 1 1 calc R . . H51B H 0.7476 0.7473 0.0743 0.049 Uiso 1 1 calc R . . C52 C 0.8732(3) 0.68537(14) 0.07246(10) 0.0605(10) Uani 1 1 d . . . H52A H 0.9437 0.6808 0.0591 0.091 Uiso 1 1 calc R . . H52B H 0.8239 0.6514 0.0679 0.091 Uiso 1 1 calc R . . H52C H 0.8946 0.6898 0.1004 0.091 Uiso 1 1 calc R . . C53 C 0.8188(3) 1.04923(13) 0.02357(9) 0.0434(8) Uani 1 1 d . . . H53A H 0.8742 1.0439 0.0037 0.052 Uiso 1 1 calc R . . H53B H 0.8633 1.0509 0.0495 0.052 Uiso 1 1 calc R . . C54 C 0.7509(3) 1.10346(13) 0.01586(10) 0.0529(9) Uani 1 1 d . . . H54A H 0.7054 1.1008 -0.0095 0.079 Uiso 1 1 calc R . . H54B H 0.8046 1.1360 0.0158 0.079 Uiso 1 1 calc R . . H54C H 0.6984 1.1090 0.0362 0.079 Uiso 1 1 calc R . . C55 C 0.5678(2) 0.91786(12) 0.01890(7) 0.0306(7) Uani 1 1 d . . . H55A H 0.5567 0.9526 0.0025 0.037 Uiso 1 1 calc R . . H55B H 0.5285 0.8853 0.0047 0.037 Uiso 1 1 calc R . . C56 C 0.5160(2) 0.92720(12) 0.05695(7) 0.0274(6) Uani 1 1 d . . . C57 C 0.4748(2) 0.88153(11) 0.07773(7) 0.0280(6) Uani 1 1 d . . . C58 C 0.4380(2) 0.88973(12) 0.11461(7) 0.0312(7) Uani 1 1 d . . . H58 H 0.4097 0.8581 0.1282 0.037 Uiso 1 1 calc R . . C59 C 0.4424(2) 0.94390(12) 0.13168(7) 0.0294(6) Uani 1 1 d . . . C60 C 0.4797(2) 0.99015(11) 0.11057(8) 0.0302(6) Uani 1 1 d . . . C61 C 0.5163(2) 0.98161(12) 0.07390(7) 0.0294(6) Uani 1 1 d . . . H61 H 0.5423 1.0135 0.0600 0.035 Uiso 1 1 calc R . . C62 C 0.4453(3) 0.77910(12) 0.08062(8) 0.0387(7) Uani 1 1 d . . . H62A H 0.4794 0.7829 0.1079 0.046 Uiso 1 1 calc R . . H62B H 0.4798 0.7448 0.0694 0.046 Uiso 1 1 calc R . . C63 C 0.3161(3) 0.77054(14) 0.08018(10) 0.0528(9) Uani 1 1 d . . . H63A H 0.2833 0.8009 0.0955 0.079 Uiso 1 1 calc R . . H63B H 0.3005 0.7331 0.0915 0.079 Uiso 1 1 calc R . . H63C H 0.2802 0.7721 0.0533 0.079 Uiso 1 1 calc R . . C64 C 0.5064(3) 1.09207(13) 0.10738(10) 0.0539(9) Uani 1 1 d . . . H64A H 0.4552 1.0947 0.0828 0.065 Uiso 1 1 calc R . . H64B H 0.5881 1.0903 0.1010 0.065 Uiso 1 1 calc R . . C65 C 0.4887(4) 1.14337(15) 0.13279(13) 0.0835(13) Uani 1 1 d . . . H65A H 0.4068 1.1456 0.1379 0.125 Uiso 1 1 calc R . . H65B H 0.5102 1.1784 0.1195 0.125 Uiso 1 1 calc R . . H65C H 0.5375 1.1395 0.1575 0.125 Uiso 1 1 calc R . . C66 C 0.4118(2) 0.95022(13) 0.17292(7) 0.0350(7) Uani 1 1 d . . . H66A H 0.3524 0.9214 0.1782 0.042 Uiso 1 1 calc R . . H66B H 0.3788 0.9888 0.1765 0.042 Uiso 1 1 calc R . . C67 C 0.5202(2) 0.94190(12) 0.20137(7) 0.0330(7) Uani 1 1 d . . . C68 C 0.5504(2) 0.88814(12) 0.21641(7) 0.0323(7) Uani 1 1 d . . . C69 C 0.6520(3) 0.88095(13) 0.24066(7) 0.0354(7) Uani 1 1 d . . . H69 H 0.6716 0.8439 0.2508 0.042 Uiso 1 1 calc R . . C70 C 0.7261(2) 0.92707(13) 0.25046(8) 0.0355(7) Uani 1 1 d . . . C71 C 0.6941(3) 0.98100(13) 0.23587(8) 0.0384(7) Uani 1 1 d . . . C72 C 0.5926(3) 0.98799(13) 0.21148(8) 0.0389(7) Uani 1 1 d . . . H72 H 0.5723 1.0250 0.2015 0.047 Uiso 1 1 calc R . . C73 C 0.4973(3) 0.78900(13) 0.22168(9) 0.0452(8) Uani 1 1 d . . . H73A H 0.4976 0.7912 0.2503 0.054 Uiso 1 1 calc R . . H73B H 0.5735 0.7741 0.2154 0.054 Uiso 1 1 calc R . . C74 C 0.4004(3) 0.75036(15) 0.20480(10) 0.0627(10) Uani 1 1 d . . . H74A H 0.3255 0.7663 0.2105 0.094 Uiso 1 1 calc R . . H74B H 0.4102 0.7121 0.2164 0.094 Uiso 1 1 calc R . . H74C H 0.4027 0.7476 0.1766 0.094 Uiso 1 1 calc R . . C75 C 0.7441(4) 1.08085(17) 0.23330(12) 0.0841(14) Uani 1 1 d . . . H75A H 0.6730 1.0942 0.2444 0.101 Uiso 1 1 calc R . . H75B H 0.7299 1.0818 0.2046 0.101 Uiso 1 1 calc R . . C76 C 0.8468(6) 1.1193(2) 0.24692(16) 0.154(3) Uani 1 1 d . . . H76A H 0.9138 1.1091 0.2329 0.231 Uiso 1 1 calc R . . H76B H 0.8669 1.1140 0.2749 0.231 Uiso 1 1 calc R . . H76C H 0.8259 1.1595 0.2417 0.231 Uiso 1 1 calc R . . C77 C 0.8426(3) 0.91757(14) 0.27441(8) 0.0421(8) Uani 1 1 d . . . H77A H 0.8668 0.8773 0.2709 0.051 Uiso 1 1 calc R . . H77B H 0.9014 0.9425 0.2638 0.051 Uiso 1 1 calc R . . C78 C 0.8441(2) 0.92921(12) 0.31752(8) 0.0319(7) Uani 1 1 d . . . C79 C 0.8239(2) 0.88550(12) 0.34374(8) 0.0314(7) Uani 1 1 d . . . C80 C 0.8319(2) 0.89661(12) 0.38319(8) 0.0325(7) Uani 1 1 d . . . H80 H 0.8180 0.8665 0.4007 0.039 Uiso 1 1 calc R . . C81 C 0.8596(2) 0.95062(12) 0.39774(8) 0.0310(7) Uani 1 1 d . . . C82 C 0.8781(3) 0.99432(12) 0.37176(8) 0.0355(7) Uani 1 1 d . . . C83 C 0.8717(2) 0.98333(13) 0.33241(8) 0.0372(7) Uani 1 1 d . . . H83 H 0.8866 1.0135 0.3151 0.045 Uiso 1 1 calc R . . C84 C 0.7833(3) 0.78588(13) 0.35265(10) 0.0527(9) Uani 1 1 d . . . H84A H 0.7231 0.7943 0.3704 0.063 Uiso 1 1 calc R . . H84B H 0.8576 0.7779 0.3685 0.063 Uiso 1 1 calc R . . C85 C 0.7475(4) 0.73484(15) 0.32710(13) 0.0879(14) Uani 1 1 d . . . H85A H 0.6734 0.7431 0.3119 0.132 Uiso 1 1 calc R . . H85B H 0.7387 0.7010 0.3434 0.132 Uiso 1 1 calc R . . H85C H 0.8072 0.7273 0.3094 0.132 Uiso 1 1 calc R . . C86 C 0.9209(3) 1.09457(13) 0.36230(10) 0.0560(9) Uani 1 1 d . . . H86A H 0.8487 1.1008 0.3450 0.067 Uiso 1 1 calc R . . H86B H 0.9850 1.0866 0.3460 0.067 Uiso 1 1 calc R . . C87 C 0.9482(4) 1.14641(14) 0.38684(13) 0.0776(13) Uani 1 1 d . . . H87A H 0.8915 1.1499 0.4061 0.116 Uiso 1 1 calc R . . H87B H 0.9447 1.1806 0.3703 0.116 Uiso 1 1 calc R . . H87C H 1.0265 1.1427 0.4003 0.116 Uiso 1 1 calc R . . C88 C 0.8753(2) 0.96088(13) 0.44137(8) 0.0370(7) Uani 1 1 d . . . H88A H 0.8504 1.0003 0.4472 0.044 Uiso 1 1 calc R . . H88B H 0.8263 0.9337 0.4546 0.044 Uiso 1 1 calc R . . 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 O1 0.0376(12) 0.0335(13) 0.0521(12) -0.0047(10) 0.0008(10) 0.0060(10) O2 0.0430(13) 0.0385(13) 0.0532(13) 0.0089(10) 0.0034(10) -0.0015(11) O3 0.0644(15) 0.0329(13) 0.0331(11) 0.0056(9) 0.0085(10) 0.0089(11) O4 0.0646(15) 0.0382(13) 0.0354(11) -0.0032(10) 0.0053(10) -0.0145(11) O5 0.0681(16) 0.0364(13) 0.0455(12) 0.0044(10) -0.0106(11) -0.0047(11) O6 0.0525(14) 0.0392(13) 0.0444(12) 0.0024(10) -0.0060(10) 0.0055(11) O7 0.0762(17) 0.0401(14) 0.0386(12) 0.0024(10) -0.0062(11) -0.0066(12) O8 0.0573(15) 0.0476(14) 0.0447(12) 0.0060(11) -0.0105(11) -0.0100(11) O9 0.0401(13) 0.0406(14) 0.0521(13) -0.0031(10) -0.0037(10) 0.0087(11) O10 0.0269(11) 0.0379(13) 0.0551(13) 0.0129(10) 0.0008(9) -0.0006(9) O11 0.0494(13) 0.0310(12) 0.0331(10) -0.0006(9) 0.0080(9) -0.0041(10) O12 0.0587(15) 0.0303(13) 0.0437(12) -0.0030(10) 0.0051(10) 0.0029(10) O13 0.0526(14) 0.0393(13) 0.0371(11) 0.0005(10) -0.0033(10) -0.0052(10) O14 0.0659(17) 0.0549(16) 0.0605(14) 0.0179(12) -0.0213(12) -0.0217(13) O15 0.0500(14) 0.0341(13) 0.0460(12) -0.0052(10) -0.0043(10) 0.0018(10) O16 0.0767(17) 0.0333(13) 0.0502(13) -0.0005(10) -0.0119(12) -0.0024(11) C1 0.0338(17) 0.0361(18) 0.0234(14) -0.0035(12) 0.0020(12) 0.0040(14) C2 0.0417(18) 0.0318(18) 0.0284(15) -0.0026(12) 0.0027(13) 0.0078(14) C3 0.0367(17) 0.0398(19) 0.0208(13) -0.0047(12) 0.0062(12) 0.0065(14) C4 0.0398(18) 0.0366(19) 0.0289(15) -0.0002(13) 0.0036(13) 0.0022(15) C5 0.0460(19) 0.0368(18) 0.0243(14) 0.0025(13) 0.0025(13) 0.0117(15) C6 0.0381(17) 0.0366(18) 0.0192(13) -0.0050(12) 0.0039(12) 0.0048(14) C7 0.0433(19) 0.039(2) 0.0424(17) 0.0059(14) -0.0036(15) 0.0073(15) C8 0.051(2) 0.041(2) 0.128(4) 0.016(2) -0.013(2) -0.0011(18) C9 0.065(2) 0.041(2) 0.0504(19) 0.0149(16) 0.0031(18) -0.0024(18) C10 0.074(3) 0.050(2) 0.084(3) 0.022(2) 0.008(2) -0.010(2) C11 0.0390(18) 0.0410(18) 0.0233(14) -0.0007(12) -0.0052(13) 0.0081(14) C12 0.0291(16) 0.0366(18) 0.0276(14) -0.0005(13) -0.0026(12) 0.0080(13) C13 0.0398(18) 0.0308(17) 0.0339(16) -0.0038(13) -0.0035(13) 0.0024(14) C14 0.0302(17) 0.0351(18) 0.0344(15) -0.0005(13) -0.0038(13) -0.0025(13) C15 0.0262(16) 0.0369(18) 0.0308(15) -0.0006(13) 0.0002(12) 0.0054(13) C16 0.0349(17) 0.0316(17) 0.0346(15) -0.0029(13) -0.0008(13) 0.0083(13) C17 0.0331(17) 0.0344(18) 0.0300(15) 0.0031(13) -0.0023(13) 0.0052(13) C18 0.080(3) 0.036(2) 0.0441(18) 0.0056(15) 0.0137(18) 0.0029(18) C19 0.114(4) 0.066(3) 0.065(2) 0.008(2) 0.007(2) 0.042(3) C20 0.055(2) 0.039(2) 0.0493(19) -0.0029(15) 0.0021(16) -0.0056(16) C21 0.058(2) 0.042(2) 0.074(2) -0.0004(18) 0.0039(19) -0.0134(18) C22 0.0355(17) 0.0396(18) 0.0343(15) 0.0000(13) 0.0088(13) 0.0078(14) C23 0.0314(16) 0.0376(18) 0.0236(13) -0.0053(12) 0.0086(12) 0.0016(14) C24 0.0372(17) 0.0335(18) 0.0255(14) -0.0046(12) 0.0090(13) 0.0006(14) C25 0.0393(18) 0.0342(18) 0.0225(13) -0.0036(12) 0.0076(13) 0.0069(14) C26 0.0323(17) 0.0422(19) 0.0243(14) -0.0038(13) 0.0114(12) 0.0020(14) C27 0.0421(19) 0.043(2) 0.0279(14) -0.0060(13) 0.0108(14) -0.0083(15) C28 0.048(2) 0.0366(19) 0.0246(14) 0.0003(13) 0.0082(14) 0.0046(15) C29 0.092(3) 0.038(2) 0.0361(17) -0.0008(15) 0.0043(18) -0.0025(19) C30 0.143(4) 0.042(2) 0.060(2) 0.0072(19) -0.014(3) -0.014(2) C31 0.078(3) 0.036(2) 0.055(2) 0.0062(16) -0.0075(19) -0.0008(18) C32 0.157(5) 0.041(3) 0.143(5) 0.016(3) -0.061(4) 0.004(3) C33 0.0348(18) 0.049(2) 0.0425(17) -0.0101(15) 0.0081(14) 0.0028(15) C34 0.0189(15) 0.0431(19) 0.0374(16) -0.0018(14) -0.0004(12) 0.0061(13) C35 0.0283(17) 0.043(2) 0.0381(16) 0.0048(14) -0.0007(13) 0.0054(14) C36 0.0322(17) 0.0383(19) 0.0409(17) -0.0051(14) -0.0050(14) 0.0074(14) C37 0.0199(15) 0.045(2) 0.0370(16) 0.0006(14) -0.0013(12) 0.0097(13) C38 0.0240(16) 0.044(2) 0.0382(16) 0.0027(14) -0.0009(13) 0.0023(14) C39 0.0268(16) 0.0394(19) 0.0443(17) -0.0032(14) -0.0041(13) 0.0040(14) C40 0.111(4) 0.046(2) 0.053(2) -0.0006(18) -0.013(2) -0.006(2) C41 0.248(8) 0.062(3) 0.077(3) 0.016(2) -0.031(4) -0.060(4) C42 0.050(2) 0.043(2) 0.0513(19) 0.0046(16) -0.0079(16) -0.0071(16) C43 0.086(3) 0.057(3) 0.067(2) 0.0124(19) -0.005(2) -0.021(2) C44 0.0290(16) 0.053(2) 0.0335(15) 0.0010(14) 0.0026(13) 0.0075(14) C45 0.0302(16) 0.0460(19) 0.0187(13) -0.0025(12) 0.0031(12) 0.0058(14) C46 0.0249(16) 0.0397(19) 0.0329(15) 0.0047(13) 0.0034(12) -0.0015(13) C47 0.0290(16) 0.0370(18) 0.0286(14) 0.0072(12) 0.0026(12) 0.0044(14) C48 0.0251(15) 0.0364(17) 0.0205(13) 0.0026(12) 0.0001(11) 0.0005(13) C49 0.0337(17) 0.0364(18) 0.0260(14) -0.0008(12) 0.0022(12) 0.0011(13) C50 0.0332(17) 0.0384(19) 0.0245(14) -0.0027(12) -0.0023(12) 0.0080(14) C51 0.047(2) 0.0380(19) 0.0364(16) 0.0011(14) 0.0014(14) 0.0077(16) C52 0.074(3) 0.039(2) 0.068(2) -0.0067(17) -0.002(2) 0.0138(18) C53 0.0343(18) 0.041(2) 0.0544(19) 0.0104(15) 0.0022(15) -0.0040(15) C54 0.042(2) 0.040(2) 0.076(2) 0.0138(17) 0.0019(18) -0.0035(16) C55 0.0300(16) 0.0379(18) 0.0234(13) 0.0077(12) 0.0006(12) 0.0015(13) C56 0.0219(15) 0.0336(17) 0.0257(13) 0.0040(12) -0.0022(11) 0.0032(12) C57 0.0244(15) 0.0295(17) 0.0286(14) -0.0010(12) -0.0046(12) 0.0011(12) C58 0.0298(16) 0.0351(18) 0.0283(14) 0.0044(12) 0.0005(12) -0.0010(13) C59 0.0257(15) 0.0366(18) 0.0251(13) -0.0023(12) -0.0017(12) 0.0064(13) C60 0.0296(16) 0.0253(16) 0.0347(15) -0.0020(13) -0.0018(12) 0.0040(13) C61 0.0232(15) 0.0340(17) 0.0307(15) 0.0083(12) 0.0004(12) 0.0018(13) C62 0.048(2) 0.0265(17) 0.0424(17) 0.0014(13) 0.0107(15) 0.0045(14) C63 0.051(2) 0.054(2) 0.053(2) -0.0125(17) 0.0078(17) -0.0111(17) C64 0.062(2) 0.032(2) 0.068(2) 0.0003(17) 0.0094(19) -0.0014(17) C65 0.114(4) 0.032(2) 0.106(3) -0.008(2) 0.020(3) -0.003(2) C66 0.0326(17) 0.0437(19) 0.0283(14) 0.0002(13) 0.0008(12) 0.0055(14) C67 0.0335(17) 0.0404(19) 0.0260(14) -0.0021(13) 0.0069(12) 0.0019(14) C68 0.0352(17) 0.0409(19) 0.0215(13) -0.0045(13) 0.0071(12) -0.0009(14) C69 0.0415(18) 0.0411(19) 0.0238(14) -0.0007(13) 0.0049(13) 0.0068(15) C70 0.0308(17) 0.050(2) 0.0270(14) -0.0025(14) 0.0085(13) 0.0023(15) C71 0.0425(19) 0.044(2) 0.0280(15) 0.0009(14) 0.0014(13) -0.0094(16) C72 0.0417(19) 0.0417(19) 0.0332(15) 0.0026(14) 0.0021(14) 0.0019(15) C73 0.056(2) 0.041(2) 0.0399(17) -0.0047(15) 0.0104(16) 0.0002(16) C74 0.082(3) 0.050(2) 0.056(2) -0.0044(17) 0.008(2) -0.014(2) C75 0.104(4) 0.069(3) 0.071(3) 0.028(2) -0.031(2) -0.037(3) C76 0.204(7) 0.097(4) 0.138(5) 0.073(4) -0.101(5) -0.101(4) C77 0.0325(17) 0.061(2) 0.0333(16) -0.0010(14) 0.0064(13) 0.0031(15) C78 0.0190(15) 0.0421(19) 0.0342(15) -0.0016(14) 0.0008(12) 0.0048(13) C79 0.0225(15) 0.0310(17) 0.0391(16) -0.0019(13) -0.0060(12) 0.0027(12) C80 0.0285(16) 0.0322(17) 0.0368(16) 0.0057(13) 0.0025(13) 0.0009(13) C81 0.0266(16) 0.0297(17) 0.0358(15) -0.0024(13) -0.0020(12) 0.0040(13) C82 0.0372(18) 0.0254(17) 0.0417(17) -0.0003(13) -0.0078(14) -0.0027(13) C83 0.0325(17) 0.0345(18) 0.0443(17) 0.0101(14) 0.0016(14) 0.0006(14) C84 0.054(2) 0.0310(19) 0.069(2) 0.0001(17) -0.0155(18) 0.0009(16) C85 0.112(4) 0.038(2) 0.105(3) -0.008(2) -0.033(3) 0.000(2) C86 0.053(2) 0.034(2) 0.077(2) 0.0110(18) -0.0106(19) -0.0057(16) C87 0.076(3) 0.032(2) 0.119(3) -0.002(2) -0.019(3) -0.0076(19) C88 0.0345(17) 0.0431(19) 0.0339(15) -0.0030(13) 0.0056(13) 0.0035(14) _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 O1 C1 1.385(3) . ? O1 C7 1.426(3) . ? O2 C4 1.378(3) . ? O2 C9 1.429(4) . ? O3 C17 1.387(3) . ? O3 C18 1.414(3) . ? O4 C14 1.388(3) . ? O4 C20 1.404(3) . ? O5 C28 1.376(3) . ? O5 C29 1.425(4) . ? O6 C25 1.376(3) . ? O6 C31 1.424(4) . ? O7 C35 1.376(3) . ? O7 C40 1.401(4) . ? O8 C38 1.381(3) . ? O8 C42 1.419(3) . ? O9 C50 1.383(3) . ? O9 C51 1.424(4) . ? O10 C47 1.382(3) . ? O10 C53 1.420(3) . ? O11 C57 1.388(3) . ? O11 C62 1.428(3) . ? O12 C60 1.376(3) . ? O12 C64 1.415(4) . ? O13 C68 1.380(3) . ? O13 C73 1.418(3) . ? O14 C71 1.388(4) . ? O14 C75 1.405(4) . ? O15 C79 1.374(3) . ? O15 C84 1.418(4) . ? O16 C82 1.389(3) . ? O16 C86 1.424(4) . ? C1 C2 1.384(4) . ? C1 C6 1.391(4) . ? C2 C3 1.387(4) . ? C2 H2 0.9500 . ? C3 C4 1.395(4) . ? C3 C88 1.524(4) . ? C4 C5 1.398(4) . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C11 1.516(4) . ? C7 C8 1.508(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.517(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.514(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.386(4) . ? C12 C13 1.396(4) . ? C13 C14 1.384(4) . ? C13 H13 0.9500 . ? C14 C15 1.399(4) . ? C15 C16 1.382(4) . ? C15 C22 1.523(4) . ? C16 C17 1.388(4) . ? C16 H16 0.9500 . ? C18 C19 1.496(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.499(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.506(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.385(4) . ? C23 C24 1.389(4) . ? C24 C25 1.399(4) . ? C24 H24 0.9500 . ? C25 C26 1.378(4) . ? C26 C27 1.380(4) . ? C26 C33 1.508(4) . ? C27 C28 1.400(4) . ? C27 H27 0.9500 . ? C29 C30 1.500(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.487(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.526(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.377(4) . ? C34 C35 1.387(4) . ? C35 C36 1.399(4) . ? C36 C37 1.381(4) . ? C36 H36 0.9500 . ? C37 C38 1.387(4) . ? C37 C44 1.521(4) . ? C38 C39 1.400(4) . ? C39 H39 0.9500 . ? C40 C41 1.491(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.511(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.522(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C50 1.386(4) . ? C45 C46 1.393(4) . ? C46 C47 1.384(4) . ? C46 H46 0.9500 . ? C47 C48 1.385(4) . ? C48 C49 1.395(4) . ? C48 C55 1.526(4) . ? C49 C50 1.386(4) . ? C49 H49 0.9500 . ? C51 C52 1.487(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.498(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.511(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.393(4) . ? C56 C61 1.397(4) . ? C57 C58 1.394(4) . ? C58 C59 1.392(4) . ? C58 H58 0.9500 . ? C59 C60 1.392(4) . ? C59 C66 1.507(4) . ? C60 C61 1.388(4) . ? C61 H61 0.9500 . ? C62 C63 1.505(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.509(5) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.529(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C72 1.385(4) . ? C67 C68 1.388(4) . ? C68 C69 1.386(4) . ? C69 C70 1.396(4) . ? C69 H69 0.9500 . ? C70 C71 1.391(4) . ? C70 C77 1.527(4) . ? C71 C72 1.387(4) . ? C72 H72 0.9500 . ? C73 C74 1.510(4) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.525(6) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.512(4) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C83 1.388(4) . ? C78 C79 1.397(4) . ? C79 C80 1.381(4) . ? C80 C81 1.382(4) . ? C80 H80 0.9500 . ? C81 C82 1.387(4) . ? C81 C88 1.519(4) . ? C82 C83 1.378(4) . ? C83 H83 0.9500 . ? C84 C85 1.515(5) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 C87 1.492(5) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? 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 C1 O1 C7 118.6(2) . . ? C4 O2 C9 117.8(2) . . ? C17 O3 C18 119.5(2) . . ? C14 O4 C20 119.5(2) . . ? C28 O5 C29 119.1(3) . . ? C25 O6 C31 118.6(2) . . ? C35 O7 C40 120.1(2) . . ? C38 O8 C42 119.3(2) . . ? C50 O9 C51 118.4(2) . . ? C47 O10 C53 118.3(2) . . ? C57 O11 C62 118.1(2) . . ? C60 O12 C64 118.6(2) . . ? C68 O13 C73 118.3(2) . . ? C71 O14 C75 118.7(3) . . ? C79 O15 C84 118.1(2) . . ? C82 O16 C86 118.5(2) . . ? C2 C1 O1 123.7(3) . . ? C2 C1 C6 120.7(3) . . ? O1 C1 C6 115.6(2) . . ? C1 C2 C3 121.8(3) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C2 C3 C4 118.2(3) . . ? C2 C3 C88 120.3(3) . . ? C4 C3 C88 121.5(3) . . ? O2 C4 C3 116.2(3) . . ? O2 C4 C5 124.2(3) . . ? C3 C4 C5 119.7(3) . . ? C6 C5 C4 121.9(3) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C1 C6 C5 117.7(3) . . ? C1 C6 C11 121.4(3) . . ? C5 C6 C11 120.8(3) . . ? O1 C7 C8 106.5(3) . . ? O1 C7 H7A 110.4 . . ? C8 C7 H7A 110.4 . . ? O1 C7 H7B 110.4 . . ? C8 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C10 106.7(3) . . ? O2 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? O2 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C6 109.8(2) . . ? C12 C11 H11A 109.7 . . ? C6 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? C6 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C17 C12 C13 118.3(2) . . ? C17 C12 C11 121.7(3) . . ? C13 C12 C11 119.6(3) . . ? C14 C13 C12 121.1(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 O4 123.4(3) . . ? C13 C14 C15 120.4(3) . . ? O4 C14 C15 116.1(2) . . ? C16 C15 C14 118.0(2) . . ? C16 C15 C22 121.8(3) . . ? C14 C15 C22 120.1(2) . . ? C15 C16 C17 121.7(3) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? O3 C17 C12 115.7(2) . . ? O3 C17 C16 123.9(3) . . ? C12 C17 C16 120.3(3) . . ? O3 C18 C19 113.7(3) . . ? O3 C18 H18A 108.8 . . ? C19 C18 H18A 108.8 . . ? O3 C18 H18B 108.8 . . ? C19 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C20 C21 107.0(3) . . ? O4 C20 H20A 110.3 . . ? C21 C20 H20A 110.3 . . ? O4 C20 H20B 110.3 . . ? C21 C20 H20B 110.3 . . ? H20A C20 H20B 108.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C15 111.5(2) . . ? C23 C22 H22A 109.3 . . ? C15 C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? C15 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C28 C23 C24 117.9(3) . . ? C28 C23 C22 121.4(3) . . ? C24 C23 C22 120.6(3) . . ? C23 C24 C25 121.4(3) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? O6 C25 C26 116.3(3) . . ? O6 C25 C24 123.5(3) . . ? C26 C25 C24 120.2(3) . . ? C25 C26 C27 118.9(3) . . ? C25 C26 C33 120.7(3) . . ? C27 C26 C33 120.3(3) . . ? C26 C27 C28 120.9(3) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? O5 C28 C23 114.7(3) . . ? O5 C28 C27 124.7(3) . . ? C23 C28 C27 120.6(3) . . ? O5 C29 C30 106.8(3) . . ? O5 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O5 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O6 C31 C32 106.5(3) . . ? O6 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? O6 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 C34 117.3(2) . . ? C26 C33 H33A 108.0 . . ? C34 C33 H33A 108.0 . . ? C26 C33 H33B 108.0 . . ? C34 C33 H33B 108.0 . . ? H33A C33 H33B 107.2 . . ? C39 C34 C35 118.3(3) . . ? C39 C34 C33 121.4(3) . . ? C35 C34 C33 120.1(3) . . ? O7 C35 C34 115.8(3) . . ? O7 C35 C36 123.9(3) . . ? C34 C35 C36 120.3(3) . . ? C37 C36 C35 121.2(3) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 118.5(3) . . ? C36 C37 C44 120.5(3) . . ? C38 C37 C44 120.9(3) . . ? O8 C38 C37 116.2(2) . . ? O8 C38 C39 123.9(3) . . ? C37 C38 C39 119.9(3) . . ? C34 C39 C38 121.6(3) . . ? C34 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? O7 C40 C41 106.8(3) . . ? O7 C40 H40A 110.4 . . ? C41 C40 H40A 110.4 . . ? O7 C40 H40B 110.4 . . ? C41 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O8 C42 C43 107.4(3) . . ? O8 C42 H42A 110.2 . . ? C43 C42 H42A 110.2 . . ? O8 C42 H42B 110.2 . . ? C43 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C37 C44 C45 111.2(2) . . ? C37 C44 H44A 109.4 . . ? C45 C44 H44A 109.4 . . ? C37 C44 H44B 109.4 . . ? C45 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C50 C45 C46 118.3(3) . . ? C50 C45 C44 120.8(3) . . ? C46 C45 C44 120.8(3) . . ? C47 C46 C45 121.3(3) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? O10 C47 C46 123.6(3) . . ? O10 C47 C48 116.0(2) . . ? C46 C47 C48 120.4(3) . . ? C47 C48 C49 118.4(3) . . ? C47 C48 C55 121.6(2) . . ? C49 C48 C55 119.9(2) . . ? C50 C49 C48 121.1(3) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? O9 C50 C45 116.1(3) . . ? O9 C50 C49 123.5(3) . . ? C45 C50 C49 120.4(3) . . ? O9 C51 C52 107.2(3) . . ? O9 C51 H51A 110.3 . . ? C52 C51 H51A 110.3 . . ? O9 C51 H51B 110.3 . . ? C52 C51 H51B 110.3 . . ? H51A C51 H51B 108.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O10 C53 C54 107.4(3) . . ? O10 C53 H53A 110.2 . . ? C54 C53 H53A 110.2 . . ? O10 C53 H53B 110.2 . . ? C54 C53 H53B 110.2 . . ? H53A C53 H53B 108.5 . . ? 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 . . ? C56 C55 C48 109.1(2) . . ? C56 C55 H55A 109.9 . . ? C48 C55 H55A 109.9 . . ? C56 C55 H55B 109.9 . . ? C48 C55 H55B 109.9 . . ? H55A C55 H55B 108.3 . . ? C57 C56 C61 117.7(2) . . ? C57 C56 C55 121.4(2) . . ? C61 C56 C55 120.6(2) . . ? O11 C57 C56 115.4(2) . . ? O11 C57 C58 123.6(2) . . ? C56 C57 C58 121.0(2) . . ? C57 C58 C59 120.6(3) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? C60 C59 C58 118.7(2) . . ? C60 C59 C66 122.1(2) . . ? C58 C59 C66 119.1(2) . . ? O12 C60 C61 123.8(2) . . ? O12 C60 C59 116.0(2) . . ? C61 C60 C59 120.2(2) . . ? C60 C61 C56 121.6(2) . . ? C60 C61 H61 119.2 . . ? C56 C61 H61 119.2 . . ? O11 C62 C63 112.8(2) . . ? O11 C62 H62A 109.0 . . ? C63 C62 H62A 109.0 . . ? O11 C62 H62B 109.0 . . ? C63 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O12 C64 C65 107.0(3) . . ? O12 C64 H64A 110.3 . . ? C65 C64 H64A 110.3 . . ? O12 C64 H64B 110.3 . . ? C65 C64 H64B 110.3 . . ? H64A C64 H64B 108.6 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C59 C66 C67 110.0(2) . . ? C59 C66 H66A 109.7 . . ? C67 C66 H66A 109.7 . . ? C59 C66 H66B 109.7 . . ? C67 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? C72 C67 C68 118.8(3) . . ? C72 C67 C66 120.1(3) . . ? C68 C67 C66 121.1(3) . . ? O13 C68 C69 123.7(3) . . ? O13 C68 C67 116.0(3) . . ? C69 C68 C67 120.2(3) . . ? C68 C69 C70 121.2(3) . . ? C68 C69 H69 119.4 . . ? C70 C69 H69 119.4 . . ? C71 C70 C69 118.2(3) . . ? C71 C70 C77 121.2(3) . . ? C69 C70 C77 120.6(3) . . ? O14 C71 C72 124.0(3) . . ? O14 C71 C70 115.5(3) . . ? C72 C71 C70 120.4(3) . . ? C67 C72 C71 121.2(3) . . ? C67 C72 H72 119.4 . . ? C71 C72 H72 119.4 . . ? O13 C73 C74 106.5(3) . . ? O13 C73 H73A 110.4 . . ? C74 C73 H73A 110.4 . . ? O13 C73 H73B 110.4 . . ? C74 C73 H73B 110.4 . . ? H73A C73 H73B 108.6 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O14 C75 C76 107.4(4) . . ? O14 C75 H75A 110.2 . . ? C76 C75 H75A 110.2 . . ? O14 C75 H75B 110.2 . . ? C76 C75 H75B 110.2 . . ? H75A C75 H75B 108.5 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C70 115.7(2) . . ? C78 C77 H77A 108.4 . . ? C70 C77 H77A 108.4 . . ? C78 C77 H77B 108.4 . . ? C70 C77 H77B 108.4 . . ? H77A C77 H77B 107.4 . . ? C83 C78 C79 118.0(3) . . ? C83 C78 C77 120.6(3) . . ? C79 C78 C77 121.4(3) . . ? O15 C79 C80 124.3(3) . . ? O15 C79 C78 115.5(2) . . ? C80 C79 C78 120.2(3) . . ? C79 C80 C81 121.4(3) . . ? C79 C80 H80 119.3 . . ? C81 C80 H80 119.3 . . ? C80 C81 C82 118.6(3) . . ? C80 C81 C88 120.4(2) . . ? C82 C81 C88 121.0(3) . . ? C83 C82 C81 120.3(3) . . ? C83 C82 O16 123.3(3) . . ? C81 C82 O16 116.4(2) . . ? C82 C83 C78 121.5(3) . . ? C82 C83 H83 119.2 . . ? C78 C83 H83 119.2 . . ? O15 C84 C85 106.7(3) . . ? O15 C84 H84A 110.4 . . ? C85 C84 H84A 110.4 . . ? O15 C84 H84B 110.4 . . ? C85 C84 H84B 110.4 . . ? H84A C84 H84B 108.6 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? O16 C86 C87 107.5(3) . . ? O16 C86 H86A 110.2 . . ? C87 C86 H86A 110.2 . . ? O16 C86 H86B 110.2 . . ? C87 C86 H86B 110.2 . . ? H86A C86 H86B 108.5 . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C3 C88 C81 109.8(2) . . ? C3 C88 H88A 109.7 . . ? C81 C88 H88A 109.7 . . ? C3 C88 H88B 109.7 . . ? C81 C88 H88B 109.7 . . ? H88A C88 H88B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.225 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.056 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.168 0.943 0.360 216.8 42.1 2 -0.168 0.056 0.640 217.0 42.1 3 0.198 1.054 0.856 195.8 40.1 4 0.332 0.443 0.140 216.9 42.1 5 0.302 0.554 0.644 195.8 40.1 6 0.668 0.557 0.860 216.8 42.1 7 0.698 0.446 0.356 195.8 40.0 8 0.802 0.946 0.144 195.8 40.0 _platon_squeeze_details ; The disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 1660.1 Ang^3^, and a void electron population of 329 per cell. Because the solvent we used in the synthesis is acetonitrile, the amount of the disordered solvent was 16 per cell suggested by electron count. The overall formula should be (C88H112O16).4(CH3CN), considering the contribution of solvent. Refinement after the SQUEEZE routine gave significantly improved R values. [R values before SQUEEZE] R1 = 0.1803, wR2 = 0.4899, GooF = S = 1.857 for all data ; # Attachment '- PA[9].cif' data_m11231cs _database_code_depnum_ccdc_archive 'CCDC 896137' #TrackingRef '- PA[9].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H126 O18' _chemical_formula_weight 1604.00 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.872(3) _cell_length_b 43.653(11) _cell_length_c 21.478(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.396(4) _cell_angle_gamma 90.00 _cell_volume 11038(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9962 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.40 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9775 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_process_details sadabs _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 APEX-II CCD' _diffrn_measurement_method '\f and \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 25441 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9716 _reflns_number_gt 6522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.2000P)^2^+35.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00045(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9716 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1374 _refine_ls_R_factor_gt 0.1098 _refine_ls_wR_factor_ref 0.3564 _refine_ls_wR_factor_gt 0.3368 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _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 O1 O 0.8153(2) 0.15948(6) 0.40077(15) 0.0438(8) Uani 1 1 d . . . O2 O 1.2049(2) 0.11667(6) 0.31507(14) 0.0394(7) Uani 1 1 d . . . O3 O 0.7794(2) 0.27230(7) 0.38720(16) 0.0473(8) Uani 1 1 d . . . O4 O 1.1984(3) 0.21553(7) 0.42779(18) 0.0549(9) Uani 1 1 d . . . O5 O 0.7566(3) 0.38256(7) 0.44931(17) 0.0555(9) Uani 1 1 d . . . O6 O 1.1526(3) 0.33106(7) 0.38958(19) 0.0594(10) Uani 1 1 d . . . O7 O 0.7567(3) 0.49365(9) 0.38107(19) 0.0671(10) Uani 1 1 d . . . O8 O 1.1544(3) 0.44043(7) 0.49102(15) 0.0470(8) Uani 1 1 d . . . O9 O 1.1737(4) 0.52846(10) 0.34763(17) 0.0743(12) Uani 1 1 d . . . C1 C 1.0000 0.09700(12) 0.2500 0.0366(13) Uani 1 2 d S . . H1A H 0.9320 0.0837 0.2478 0.044 Uiso 0.50 1 calc PR . . H1B H 1.0680 0.0837 0.2522 0.044 Uiso 0.50 1 calc PR . . C2 C 1.0073(3) 0.11694(8) 0.30784(19) 0.0339(9) Uani 1 1 d . . . C3 C 1.1095(3) 0.12733(8) 0.33894(19) 0.0334(9) Uani 1 1 d . . . C4 C 1.1124(3) 0.14745(8) 0.38776(19) 0.0330(9) Uani 1 1 d . . . H4 H 1.1841 0.1541 0.4080 0.040 Uiso 1 1 calc R . . C5 C 1.0145(3) 0.15847(8) 0.40885(18) 0.0319(8) Uani 1 1 d . . . C6 C 0.9112(3) 0.14782(8) 0.3789(2) 0.0342(9) Uani 1 1 d . . . C7 C 0.9079(3) 0.12729(8) 0.33016(19) 0.0335(9) Uani 1 1 d . . . H7 H 0.8364 0.1199 0.3111 0.040 Uiso 1 1 calc R . . C8 C 0.7091(4) 0.14629(11) 0.3812(3) 0.0564(13) Uani 1 1 d . . . H8A H 0.7084 0.1247 0.3954 0.068 Uiso 1 1 calc R . . H8B H 0.6936 0.1466 0.3348 0.068 Uiso 1 1 calc R . . C9 C 0.6209(4) 0.16408(11) 0.4084(3) 0.0521(12) Uani 1 1 d . . . H9A H 0.6393 0.1647 0.4542 0.078 Uiso 1 1 calc R . . H9B H 0.5467 0.1543 0.3973 0.078 Uiso 1 1 calc R . . H9C H 0.6183 0.1850 0.3917 0.078 Uiso 1 1 calc R . . C10 C 1.3118(4) 0.12082(13) 0.3512(2) 0.0559(13) Uani 1 1 d . . . H10A H 1.3152 0.1093 0.3911 0.067 Uiso 1 1 calc R . . H10B H 1.3245 0.1428 0.3612 0.067 Uiso 1 1 calc R . . C11 C 1.4013(4) 0.10929(11) 0.3134(2) 0.0499(11) Uani 1 1 d . . . H11A H 1.3802 0.0888 0.2970 0.075 Uiso 1 1 calc R . . H11B H 1.4745 0.1082 0.3402 0.075 Uiso 1 1 calc R . . H11C H 1.4074 0.1233 0.2784 0.075 Uiso 1 1 calc R . . C12 C 1.0182(4) 0.18222(9) 0.4596(2) 0.0380(9) Uani 1 1 d . . . H12A H 1.0917 0.1808 0.4871 0.046 Uiso 1 1 calc R . . H12B H 0.9569 0.1781 0.4857 0.046 Uiso 1 1 calc R . . C13 C 1.0038(3) 0.21482(9) 0.43229(18) 0.0319(9) Uani 1 1 d . . . C14 C 1.0955(3) 0.23058(9) 0.41513(19) 0.0344(9) Uani 1 1 d . . . C15 C 1.0794(4) 0.25868(9) 0.3855(2) 0.0399(10) Uani 1 1 d . . . H15 H 1.1426 0.2688 0.3719 0.048 Uiso 1 1 calc R . . C16 C 0.9734(3) 0.27234(9) 0.37534(19) 0.0350(9) Uani 1 1 d . . . C17 C 0.8815(3) 0.25755(8) 0.39629(19) 0.0327(9) Uani 1 1 d . . . C18 C 0.8978(3) 0.22859(9) 0.42365(19) 0.0343(9) Uani 1 1 d . . . H18 H 0.8347 0.2181 0.4366 0.041 Uiso 1 1 calc R . . C19 C 0.6811(4) 0.25672(10) 0.4002(3) 0.0492(11) Uani 1 1 d . . . H19A H 0.6888 0.2508 0.4450 0.059 Uiso 1 1 calc R . . H19B H 0.6697 0.2379 0.3743 0.059 Uiso 1 1 calc R . . C20 C 0.5838(4) 0.27762(13) 0.3854(3) 0.0678(16) Uani 1 1 d . . . H20A H 0.5991 0.2969 0.4083 0.102 Uiso 1 1 calc R . . H20B H 0.5153 0.2681 0.3978 0.102 Uiso 1 1 calc R . . H20C H 0.5723 0.2818 0.3402 0.102 Uiso 1 1 calc R . . C21 C 1.3001(4) 0.23276(11) 0.4289(2) 0.0468(11) Uani 1 1 d . . . H21A H 1.2977 0.2509 0.4564 0.056 Uiso 1 1 calc R . . H21B H 1.3090 0.2399 0.3861 0.056 Uiso 1 1 calc R . . C22 C 1.3951(4) 0.21281(12) 0.4528(3) 0.0549(12) Uani 1 1 d . . . H22A H 1.3763 0.2017 0.4898 0.082 Uiso 1 1 calc R . . H22B H 1.4632 0.2253 0.4646 0.082 Uiso 1 1 calc R . . H22C H 1.4094 0.1981 0.4202 0.082 Uiso 1 1 calc R . . C23 C 0.9553(4) 0.30255(9) 0.3396(2) 0.0398(10) Uani 1 1 d . . . H23A H 1.0158 0.3049 0.3122 0.048 Uiso 1 1 calc R . . H23B H 0.8817 0.3017 0.3121 0.048 Uiso 1 1 calc R . . C24 C 0.9558(4) 0.33040(9) 0.38160(19) 0.0388(10) Uani 1 1 d . . . C25 C 1.0558(4) 0.34413(9) 0.4056(2) 0.0419(10) Uani 1 1 d . . . C26 C 1.0557(4) 0.36917(9) 0.4452(2) 0.0432(10) Uani 1 1 d . . . H26 H 1.1260 0.3779 0.4627 0.052 Uiso 1 1 calc R . . C27 C 0.9561(4) 0.38172(8) 0.45988(19) 0.0357(9) Uani 1 1 d . . . C28 C 0.8540(4) 0.36869(9) 0.4334(2) 0.0407(10) Uani 1 1 d . . . C29 C 0.8549(4) 0.34280(9) 0.3957(2) 0.0422(10) Uani 1 1 d . . . H29 H 0.7850 0.3335 0.3793 0.051 Uiso 1 1 calc R . . C30 C 0.6515(4) 0.36922(12) 0.4287(3) 0.0602(14) Uani 1 1 d . . . H30A H 0.6493 0.3480 0.4445 0.072 Uiso 1 1 calc R . . H30B H 0.6387 0.3687 0.3823 0.072 Uiso 1 1 calc R . . C31 C 0.5622(5) 0.38797(13) 0.4531(3) 0.0667(15) Uani 1 1 d . . . H31A H 0.5752 0.3882 0.4990 0.100 Uiso 1 1 calc R . . H31B H 0.4874 0.3791 0.4390 0.100 Uiso 1 1 calc R . . H31C H 0.5651 0.4090 0.4372 0.100 Uiso 1 1 calc R . . C32 C 1.2545(5) 0.34836(15) 0.3971(4) 0.083(2) Uani 1 1 d . . . H32A H 1.2826 0.3512 0.4421 0.100 Uiso 1 1 calc R . . H32B H 1.2422 0.3687 0.3772 0.100 Uiso 1 1 calc R . . C33 C 1.3387(7) 0.3298(2) 0.3649(6) 0.137(4) Uani 1 1 d . . . H33A H 1.3546 0.3104 0.3874 0.206 Uiso 1 1 calc R . . H33B H 1.4093 0.3414 0.3652 0.206 Uiso 1 1 calc R . . H33C H 1.3063 0.3255 0.3215 0.206 Uiso 1 1 calc R . . C34 C 0.9565(4) 0.40907(8) 0.50313(19) 0.0384(10) Uani 1 1 d . . . H34A H 0.8886 0.4081 0.5254 0.046 Uiso 1 1 calc R . . H34B H 1.0245 0.4080 0.5350 0.046 Uiso 1 1 calc R . . C35 C 0.9566(3) 0.43941(8) 0.46912(17) 0.0310(8) Uani 1 1 d . . . C36 C 1.0559(3) 0.45488(8) 0.46377(17) 0.0293(8) Uani 1 1 d . . . C37 C 1.0559(3) 0.48313(8) 0.43524(17) 0.0322(9) Uani 1 1 d . . . H37 H 1.1254 0.4936 0.4333 0.039 Uiso 1 1 calc R . . C38 C 0.9532(4) 0.49625(8) 0.40917(17) 0.0320(9) Uani 1 1 d . . . C39 C 0.8536(4) 0.48021(9) 0.4106(2) 0.0386(9) Uani 1 1 d . . . C40 C 0.8557(4) 0.45227(9) 0.44152(19) 0.0371(9) Uani 1 1 d . . . H40 H 0.7863 0.4417 0.4438 0.045 Uiso 1 1 calc R . . C41 C 0.6546(6) 0.47824(18) 0.3797(5) 0.100(3) Uani 1 1 d . . . H41A H 0.6332 0.4763 0.4225 0.120 Uiso 1 1 calc R . . H41B H 0.6601 0.4575 0.3617 0.120 Uiso 1 1 calc R . . C42 C 0.5654(8) 0.4980(3) 0.3375(7) 0.159(5) Uani 1 1 d . . . H42A H 0.5383 0.5145 0.3626 0.239 Uiso 1 1 calc R . . H42B H 0.5012 0.4851 0.3206 0.239 Uiso 1 1 calc R . . H42C H 0.6008 0.5068 0.3028 0.239 Uiso 1 1 calc R . . C43 C 1.2587(5) 0.45575(13) 0.4900(3) 0.0694(16) Uani 1 1 d . . . H43A H 1.2582 0.4757 0.5118 0.083 Uiso 1 1 calc R . . H43B H 1.2730 0.4594 0.4462 0.083 Uiso 1 1 calc R . . C44 C 1.3473(6) 0.4353(2) 0.5228(6) 0.132(4) Uani 1 1 d . . . H44A H 1.3468 0.4369 0.5683 0.198 Uiso 1 1 calc R . . H44B H 1.4220 0.4413 0.5122 0.198 Uiso 1 1 calc R . . H44C H 1.3315 0.4141 0.5096 0.198 Uiso 1 1 calc R . . C45 C 0.9544(4) 0.52797(9) 0.37974(18) 0.0401(10) Uani 1 1 d . . . H45A H 0.8799 0.5379 0.3814 0.048 Uiso 1 1 calc R . . H45B H 1.0129 0.5406 0.4048 0.048 Uiso 1 1 calc R . . C46 C 0.9785(4) 0.52734(8) 0.31309(18) 0.0382(10) Uani 1 1 d . . . C47 C 0.8912(4) 0.52724(10) 0.2646(2) 0.0455(11) Uani 1 1 d . . . H47 H 0.8151 0.5269 0.2738 0.055 Uiso 1 1 calc R . . C48 C 1.0884(4) 0.52767(10) 0.29812(19) 0.0441(11) Uani 1 1 d . . . C49 C 1.2683(5) 0.54552(16) 0.3433(3) 0.0777(18) Uani 1 1 d . . . H49A H 1.2454 0.5659 0.3255 0.093 Uiso 1 1 calc R . . H49B H 1.3148 0.5353 0.3142 0.093 Uiso 1 1 calc R . . C50 C 1.3372(6) 0.54962(18) 0.4050(3) 0.087(2) Uani 1 1 d . . . H50A H 1.3016 0.5651 0.4292 0.131 Uiso 1 1 calc R . . H50B H 1.4137 0.5564 0.3989 0.131 Uiso 1 1 calc R . . H50C H 1.3419 0.5301 0.4278 0.131 Uiso 1 1 calc R . . 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 O1 0.0364(17) 0.0358(15) 0.0624(19) -0.0044(13) 0.0182(14) -0.0001(13) O2 0.0307(16) 0.0328(14) 0.0561(18) -0.0070(12) 0.0109(13) 0.0033(12) O3 0.0321(16) 0.0400(16) 0.071(2) -0.0047(14) 0.0098(14) -0.0020(13) O4 0.0356(18) 0.0364(16) 0.094(3) -0.0098(16) 0.0119(17) 0.0030(14) O5 0.049(2) 0.0433(18) 0.076(2) -0.0146(16) 0.0147(17) -0.0103(15) O6 0.046(2) 0.0386(17) 0.095(3) -0.0163(17) 0.0163(18) -0.0019(15) O7 0.058(2) 0.059(2) 0.080(3) -0.0081(19) -0.0101(19) 0.0125(18) O8 0.0401(18) 0.0361(15) 0.063(2) -0.0029(14) 0.0006(14) 0.0030(13) O9 0.077(3) 0.095(3) 0.047(2) 0.0128(19) -0.0061(18) -0.042(2) C1 0.035(3) 0.022(2) 0.055(3) 0.000 0.013(3) 0.000 C2 0.037(2) 0.0167(16) 0.050(2) 0.0043(15) 0.0146(18) 0.0009(16) C3 0.037(2) 0.0205(17) 0.045(2) 0.0028(15) 0.0135(18) 0.0019(16) C4 0.029(2) 0.0276(18) 0.042(2) 0.0013(16) 0.0060(16) 0.0014(16) C5 0.031(2) 0.0300(19) 0.036(2) 0.0036(15) 0.0084(16) 0.0048(16) C6 0.031(2) 0.0245(18) 0.049(2) 0.0048(16) 0.0126(18) 0.0034(16) C7 0.034(2) 0.0191(16) 0.051(2) 0.0027(15) 0.0156(18) -0.0038(15) C8 0.044(3) 0.042(2) 0.089(4) -0.003(2) 0.028(3) 0.001(2) C9 0.041(3) 0.048(3) 0.072(3) -0.001(2) 0.022(2) 0.000(2) C10 0.041(3) 0.069(3) 0.058(3) -0.005(2) 0.006(2) 0.015(2) C11 0.037(2) 0.046(2) 0.067(3) -0.005(2) 0.009(2) 0.009(2) C12 0.033(2) 0.038(2) 0.044(2) 0.0002(17) 0.0095(18) 0.0035(18) C13 0.030(2) 0.0306(19) 0.035(2) -0.0092(15) 0.0049(16) -0.0001(16) C14 0.028(2) 0.0305(19) 0.046(2) -0.0090(17) 0.0073(17) 0.0029(16) C15 0.034(2) 0.036(2) 0.053(2) -0.0121(18) 0.0191(19) -0.0033(18) C16 0.035(2) 0.0307(19) 0.040(2) -0.0096(16) 0.0057(17) -0.0014(17) C17 0.029(2) 0.0267(18) 0.043(2) -0.0038(16) 0.0043(16) -0.0011(15) C18 0.029(2) 0.034(2) 0.042(2) -0.0061(16) 0.0093(16) -0.0006(16) C19 0.040(3) 0.041(2) 0.068(3) -0.004(2) 0.012(2) 0.001(2) C20 0.045(3) 0.056(3) 0.104(5) -0.008(3) 0.014(3) -0.002(2) C21 0.042(3) 0.046(2) 0.054(3) -0.006(2) 0.015(2) -0.001(2) C22 0.041(3) 0.056(3) 0.068(3) -0.009(2) 0.012(2) 0.006(2) C23 0.041(2) 0.037(2) 0.042(2) -0.0015(17) 0.0054(18) -0.0027(18) C24 0.046(3) 0.0299(19) 0.041(2) 0.0024(17) 0.0079(18) 0.0006(18) C25 0.042(3) 0.028(2) 0.056(3) 0.0003(18) 0.008(2) 0.0002(18) C26 0.045(3) 0.027(2) 0.058(3) -0.0019(18) 0.005(2) -0.0036(18) C27 0.043(2) 0.0231(18) 0.041(2) 0.0010(16) 0.0070(18) -0.0072(17) C28 0.048(3) 0.028(2) 0.049(2) -0.0006(17) 0.014(2) -0.0037(18) C29 0.044(3) 0.035(2) 0.049(2) -0.0008(18) 0.006(2) -0.0041(19) C30 0.054(3) 0.050(3) 0.080(4) -0.012(3) 0.020(3) -0.011(2) C31 0.058(3) 0.057(3) 0.089(4) -0.018(3) 0.027(3) -0.015(3) C32 0.051(3) 0.071(4) 0.129(6) -0.035(4) 0.013(4) -0.006(3) C33 0.061(5) 0.128(7) 0.229(12) -0.077(8) 0.045(6) 0.001(5) C34 0.050(3) 0.0254(18) 0.040(2) 0.0025(16) 0.0078(19) -0.0028(18) C35 0.039(2) 0.0230(17) 0.0313(19) -0.0023(14) 0.0051(16) 0.0001(16) C36 0.033(2) 0.0215(16) 0.0339(19) -0.0030(14) 0.0042(15) 0.0012(15) C37 0.038(2) 0.0297(19) 0.0299(19) -0.0014(15) 0.0085(16) -0.0052(17) C38 0.045(2) 0.0260(18) 0.0253(18) -0.0051(14) 0.0067(16) -0.0013(17) C39 0.038(2) 0.033(2) 0.043(2) -0.0032(17) -0.0014(18) 0.0049(18) C40 0.039(2) 0.032(2) 0.040(2) -0.0064(16) 0.0036(18) -0.0037(17) C41 0.055(4) 0.094(5) 0.143(7) -0.023(5) -0.017(4) 0.014(4) C42 0.095(7) 0.125(8) 0.237(14) -0.014(8) -0.057(8) 0.022(6) C43 0.051(3) 0.057(3) 0.099(4) -0.016(3) 0.005(3) 0.003(3) C44 0.062(5) 0.099(6) 0.222(11) -0.032(7) -0.036(6) 0.018(4) C45 0.061(3) 0.0281(19) 0.031(2) -0.0008(15) 0.0041(19) 0.0042(19) C46 0.059(3) 0.0228(18) 0.033(2) 0.0003(15) 0.0040(19) -0.0002(18) C47 0.058(3) 0.037(2) 0.041(2) -0.0026(18) 0.009(2) 0.014(2) C48 0.061(3) 0.036(2) 0.033(2) 0.0053(17) -0.002(2) -0.014(2) C49 0.070(4) 0.081(4) 0.077(4) 0.024(3) -0.008(3) -0.021(3) C50 0.069(4) 0.105(5) 0.087(5) -0.011(4) 0.004(3) -0.020(4) _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 O1 C6 1.384(5) . ? O1 C8 1.400(6) . ? O2 C3 1.383(5) . ? O2 C10 1.411(6) . ? O3 C17 1.364(5) . ? O3 C19 1.409(5) . ? O4 C14 1.383(5) . ? O4 C21 1.420(5) . ? O5 C28 1.386(5) . ? O5 C30 1.397(6) . ? O6 C25 1.365(5) . ? O6 C32 1.418(6) . ? O7 C39 1.372(5) . ? O7 C41 1.383(8) . ? O8 C36 1.390(5) . ? O8 C43 1.411(6) . ? O9 C49 1.361(7) . ? O9 C48 1.371(6) . ? C1 C2 1.510(5) . ? C1 C2 1.510(5) 2_755 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.384(6) . ? C2 C7 1.404(5) . ? C3 C4 1.365(6) . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(6) . ? C5 C12 1.501(6) . ? C6 C7 1.374(6) . ? C7 H7 0.9500 . ? C8 C9 1.483(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.503(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.540(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.377(5) . ? C13 C18 1.386(5) . ? C14 C15 1.383(6) . ? C15 C16 1.385(6) . ? C15 H15 0.9500 . ? C16 C17 1.391(5) . ? C16 C23 1.527(6) . ? C17 C18 1.397(6) . ? C18 H18 0.9500 . ? C19 C20 1.474(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.465(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.514(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.370(6) . ? C24 C29 1.383(6) . ? C25 C26 1.386(6) . ? C26 C27 1.375(6) . ? C26 H26 0.9500 . ? C27 C28 1.393(6) . ? C27 C34 1.512(5) . ? C28 C29 1.391(6) . ? C29 H29 0.9500 . ? C30 C31 1.487(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.520(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.512(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.376(5) . ? C35 C40 1.386(6) . ? C36 C37 1.377(5) . ? C37 C38 1.397(6) . ? C37 H37 0.9500 . ? C38 C39 1.377(6) . ? C38 C45 1.523(5) . ? C39 C40 1.387(6) . ? C40 H40 0.9500 . ? C41 C42 1.562(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.487(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.495(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.371(6) . ? C46 C48 1.383(7) . ? C47 C48 1.399(6) 2_755 ? C47 H47 0.9500 . ? C48 C47 1.399(6) 2_755 ? C49 C50 1.476(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? 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 C6 O1 C8 119.7(3) . . ? C3 O2 C10 118.4(3) . . ? C17 O3 C19 119.1(3) . . ? C14 O4 C21 118.6(3) . . ? C28 O5 C30 118.6(3) . . ? C25 O6 C32 118.8(4) . . ? C39 O7 C41 118.8(5) . . ? C36 O8 C43 118.1(4) . . ? C49 O9 C48 119.6(4) . . ? C2 C1 C2 109.6(4) . 2_755 ? C2 C1 H1A 109.8 . . ? C2 C1 H1A 109.7 2_755 . ? C2 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 2_755 . ? H1A C1 H1B 108.2 . . ? C3 C2 C7 116.9(4) . . ? C3 C2 C1 122.7(3) . . ? C7 C2 C1 120.3(3) . . ? C4 C3 O2 124.0(4) . . ? C4 C3 C2 121.1(4) . . ? O2 C3 C2 114.9(3) . . ? C3 C4 C5 122.3(4) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C4 C5 C6 117.4(4) . . ? C4 C5 C12 122.0(4) . . ? C6 C5 C12 120.6(3) . . ? C7 C6 O1 123.6(4) . . ? C7 C6 C5 120.5(3) . . ? O1 C6 C5 115.8(3) . . ? C6 C7 C2 121.8(4) . . ? C6 C7 H7 119.1 . . ? C2 C7 H7 119.1 . . ? O1 C8 C9 108.7(4) . . ? O1 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? O1 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C11 107.9(4) . . ? O2 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? O2 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 C13 111.7(3) . . ? C5 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C5 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C18 118.9(4) . . ? C14 C13 C12 120.7(3) . . ? C18 C13 C12 120.4(3) . . ? C13 C14 O4 114.7(4) . . ? C13 C14 C15 119.9(4) . . ? O4 C14 C15 125.3(4) . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 C23 121.2(4) . . ? C17 C16 C23 119.9(4) . . ? O3 C17 C16 117.0(3) . . ? O3 C17 C18 124.0(3) . . ? C16 C17 C18 119.0(4) . . ? C13 C18 C17 121.5(4) . . ? C13 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? O3 C19 C20 107.7(4) . . ? O3 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O3 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 C22 107.8(4) . . ? O4 C21 H21A 110.1 . . ? C22 C21 H21A 110.1 . . ? O4 C21 H21B 110.1 . . ? C22 C21 H21B 110.1 . . ? H21A C21 H21B 108.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C16 113.8(3) . . ? C24 C23 H23A 108.8 . . ? C16 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C16 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C29 118.7(4) . . ? C25 C24 C23 120.8(4) . . ? C29 C24 C23 120.5(4) . . ? O6 C25 C24 116.0(4) . . ? O6 C25 C26 123.5(4) . . ? C24 C25 C26 120.4(4) . . ? C27 C26 C25 121.6(4) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C26 C27 C28 118.2(4) . . ? C26 C27 C34 121.4(4) . . ? C28 C27 C34 120.4(4) . . ? O5 C28 C29 124.6(4) . . ? O5 C28 C27 115.5(4) . . ? C29 C28 C27 119.8(4) . . ? C24 C29 C28 121.1(4) . . ? C24 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? O5 C30 C31 107.9(4) . . ? O5 C30 H30A 110.1 . . ? C31 C30 H30A 110.1 . . ? O5 C30 H30B 110.1 . . ? C31 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C32 C33 105.4(5) . . ? O6 C32 H32A 110.7 . . ? C33 C32 H32A 110.7 . . ? O6 C32 H32B 110.7 . . ? C33 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C27 113.2(3) . . ? C35 C34 H34A 108.9 . . ? C27 C34 H34A 108.9 . . ? C35 C34 H34B 108.9 . . ? C27 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C40 117.9(3) . . ? C36 C35 C34 121.6(4) . . ? C40 C35 C34 120.4(4) . . ? C35 C36 C37 121.7(4) . . ? C35 C36 O8 115.2(3) . . ? C37 C36 O8 123.1(3) . . ? C36 C37 C38 119.7(4) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 119.3(3) . . ? C39 C38 C45 121.7(4) . . ? C37 C38 C45 119.0(4) . . ? O7 C39 C38 116.3(4) . . ? O7 C39 C40 124.0(4) . . ? C38 C39 C40 119.7(4) . . ? C35 C40 C39 121.5(4) . . ? C35 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? O7 C41 C42 105.7(7) . . ? O7 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? O7 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O8 C43 C44 106.0(6) . . ? O8 C43 H43A 110.5 . . ? C44 C43 H43A 110.5 . . ? O8 C43 H43B 110.5 . . ? C44 C43 H43B 110.5 . . ? H43A C43 H43B 108.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C38 113.2(3) . . ? C46 C45 H45A 108.9 . . ? C38 C45 H45A 108.9 . . ? C46 C45 H45B 108.9 . . ? C38 C45 H45B 108.9 . . ? H45A C45 H45B 107.8 . . ? C47 C46 C48 117.8(4) . . ? C47 C46 C45 120.6(4) . . ? C48 C46 C45 121.6(4) . . ? C46 C47 C48 121.6(5) . 2_755 ? C46 C47 H47 119.2 . . ? C48 C47 H47 119.2 2_755 . ? O9 C48 C46 116.4(4) . . ? O9 C48 C47 123.0(5) . 2_755 ? C46 C48 C47 120.6(4) . 2_755 ? O9 C49 C50 111.8(5) . . ? O9 C49 H49A 109.3 . . ? C50 C49 H49A 109.3 . . ? O9 C49 H49B 109.3 . . ? C50 C49 H49B 109.3 . . ? H49A C49 H49B 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.337 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.080 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 15.6 0.9 2 0.000 0.000 0.500 15.6 0.9 3 -0.021 0.089 0.750 407.2 78.8 4 -0.019 0.220 0.250 252.5 81.8 5 -0.018 0.281 0.750 252.0 81.2 6 -0.019 0.412 0.250 406.7 77.9 7 -0.021 0.589 0.750 407.2 78.8 8 -0.015 0.720 0.250 252.5 81.8 9 -0.020 0.781 0.750 252.0 81.2 10 -0.018 0.912 0.250 406.7 77.9 11 0.500 0.500 0.500 15.6 0.9 12 0.500 0.500 0.000 15.6 0.9 _platon_squeeze_details ; The disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 2703.6 Ang^3^, and a void electron population of 643 per cell. Because the solvent we used in the synthesis is N,N'-dimethylformide, the amount of the disordered solvent was 16 per cell suggested by electron count. The overall formula should be (C99H126O18).4(NC3OH7), considering the contribution of solvent. Refinement after the SQUEEZE routine gave significantly improved R values. [R values before SQUEEZE] R1 = 0.2576, wR2 = 0.6285, GooF = S = 2.866 for all data ; # Attachment '- PA[10].cif' data_m11226d _database_code_depnum_ccdc_archive 'CCDC 896138' #TrackingRef '- PA[10].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H140 O20' _chemical_formula_weight 1782.22 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 46.342(7) _cell_length_b 12.654(2) _cell_length_c 25.206(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.625(2) _cell_angle_gamma 90.00 _cell_volume 12449(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8637 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.66 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9904 _exptl_absorpt_correction_T_max 0.9936 _exptl_absorpt_process_details sadabs _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 APEX-II CCD' _diffrn_measurement_method '\f and \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 35930 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10895 _reflns_number_gt 6669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1980P)^2^+8.8163P] 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 SHELXL _refine_ls_extinction_coef 0.00042(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10895 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.1013 _refine_ls_wR_factor_ref 0.3394 _refine_ls_wR_factor_gt 0.3210 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _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 O1 O 0.01563(7) 0.5511(2) 0.14419(14) 0.0544(7) Uani 1 1 d . . . O2 O 0.04118(7) 0.9232(2) 0.06136(14) 0.0578(7) Uani 1 1 d . . . O3 O 0.08017(6) 0.5457(2) 0.03483(12) 0.0486(7) Uani 1 1 d . . . O4 O 0.16122(6) 0.9044(2) 0.10259(12) 0.0532(7) Uani 1 1 d . . . O5 O 0.20698(7) 0.5238(2) 0.20766(14) 0.0573(7) Uani 1 1 d . . . O6 O 0.22969(7) 0.8978(2) 0.33837(13) 0.0570(7) Uani 1 1 d . . . O7 O 0.22016(7) 0.5239(2) 0.42413(15) 0.0596(8) Uani 1 1 d . . . O8 O 0.16660(6) 0.89439(19) 0.45375(12) 0.0473(6) Uani 1 1 d . . . O9 O 0.10584(6) 0.5323(2) 0.41736(12) 0.0482(7) Uani 1 1 d . . . O10 O 0.03794(7) 0.9155(2) 0.36277(14) 0.0590(8) Uani 1 1 d . . . C1 C 0.00329(9) 0.7369(3) 0.18717(18) 0.0503(9) Uani 1 1 d . . . H1A H 0.0108 0.8022 0.2128 0.060 Uiso 1 1 calc R . . H1B H 0.0127 0.6757 0.2162 0.060 Uiso 1 1 calc R . . C2 C 0.01688(8) 0.7363(3) 0.14427(16) 0.0416(8) Uani 1 1 d . . . C3 C 0.02350(9) 0.8309(3) 0.12440(17) 0.0445(9) Uani 1 1 d . . . H3 H 0.0210 0.8959 0.1404 0.053 Uiso 1 1 calc R . . C4 C 0.03361(9) 0.8320(3) 0.08182(17) 0.0430(9) Uani 1 1 d . . . C5 C 0.03681(8) 0.7383(3) 0.05699(16) 0.0410(8) Uani 1 1 d . . . C6 C 0.03101(8) 0.6437(3) 0.07794(16) 0.0407(8) Uani 1 1 d . . . H6 H 0.0336 0.5787 0.0620 0.049 Uiso 1 1 calc R . . C7 C 0.02165(8) 0.6421(3) 0.12130(17) 0.0402(8) Uani 1 1 d . . . C8 C 0.02260(11) 0.4524(3) 0.1262(2) 0.0594(11) Uani 1 1 d . . . H8A H 0.0468 0.4497 0.1383 0.071 Uiso 1 1 calc R . . H8B H 0.0076 0.4428 0.0801 0.071 Uiso 1 1 calc R . . C9 C 0.01588(14) 0.3671(4) 0.1598(2) 0.0789(14) Uiso 1 1 d . . . H9A H 0.0312 0.3764 0.2054 0.118 Uiso 1 1 calc R . . H9B H 0.0200 0.2978 0.1477 0.118 Uiso 1 1 calc R . . H9C H -0.0080 0.3714 0.1481 0.118 Uiso 1 1 calc R . . C10 C 0.03649(13) 1.0226(3) 0.0836(2) 0.0662(12) Uani 1 1 d . . . H10A H 0.0500 1.0242 0.1302 0.079 Uiso 1 1 calc R . . H10B H 0.0120 1.0331 0.0684 0.079 Uiso 1 1 calc R . . C11 C 0.04844(14) 1.1076(4) 0.0582(3) 0.0794(14) Uiso 1 1 d . . . H11A H 0.0727 1.0965 0.0738 0.119 Uiso 1 1 calc R . . H11B H 0.0455 1.1768 0.0722 0.119 Uiso 1 1 calc R . . H11C H 0.0349 1.1049 0.0121 0.119 Uiso 1 1 calc R . . C12 C 0.04651(9) 0.7381(3) 0.00792(16) 0.0464(9) Uani 1 1 d . . . H12A H 0.0353 0.6773 -0.0208 0.056 Uiso 1 1 calc R . . H12B H 0.0379 0.8036 -0.0174 0.056 Uiso 1 1 calc R . . C13 C 0.08477(9) 0.7310(3) 0.03784(15) 0.0398(8) Uani 1 1 d . . . C14 C 0.10447(9) 0.8226(3) 0.05370(16) 0.0449(9) Uani 1 1 d . . . H14 H 0.0936 0.8898 0.0434 0.054 Uiso 1 1 calc R . . C15 C 0.14035(9) 0.8162(3) 0.08487(17) 0.0435(9) Uani 1 1 d . . . C16 C 0.15687(9) 0.7189(3) 0.10065(16) 0.0415(8) Uani 1 1 d . . . C17 C 0.13678(9) 0.6279(3) 0.08354(16) 0.0439(9) Uani 1 1 d . . . H17 H 0.1475 0.5606 0.0931 0.053 Uiso 1 1 calc R . . C18 C 0.10114(9) 0.6341(3) 0.05252(16) 0.0414(8) Uani 1 1 d . . . C19 C 0.09564(10) 0.4447(3) 0.0491(2) 0.0512(10) Uani 1 1 d . . . H19A H 0.1115 0.4371 0.0953 0.061 Uiso 1 1 calc R . . H19B H 0.1090 0.4361 0.0293 0.061 Uiso 1 1 calc R . . C20 C 0.06824(12) 0.3624(3) 0.0248(2) 0.0632(12) Uani 1 1 d . . . H20A H 0.0557 0.3697 0.0459 0.095 Uiso 1 1 calc R . . H20B H 0.0787 0.2921 0.0333 0.095 Uiso 1 1 calc R . . H20C H 0.0524 0.3716 -0.0207 0.095 Uiso 1 1 calc R . . C21 C 0.14655(12) 1.0059(3) 0.0927(2) 0.0618(11) Uani 1 1 d . . . H21A H 0.1341 1.0121 0.1146 0.074 Uiso 1 1 calc R . . H21B H 0.1301 1.0181 0.0472 0.074 Uiso 1 1 calc R . . C22 C 0.17463(14) 1.0853(4) 0.1181(2) 0.0808(15) Uani 1 1 d . . . H22A H 0.1922 1.0674 0.1618 0.121 Uiso 1 1 calc R . . H22B H 0.1654 1.1556 0.1167 0.121 Uiso 1 1 calc R . . H22C H 0.1848 1.0850 0.0926 0.121 Uiso 1 1 calc R . . C23 C 0.19538(9) 0.7111(3) 0.13912(18) 0.0494(9) Uani 1 1 d . . . H23A H 0.2053 0.7723 0.1298 0.059 Uiso 1 1 calc R . . H23B H 0.2026 0.6459 0.1277 0.059 Uiso 1 1 calc R . . C24 C 0.20882(8) 0.7095(3) 0.20946(17) 0.0439(9) Uani 1 1 d . . . C25 C 0.21360(9) 0.8049(3) 0.24080(17) 0.0457(9) Uani 1 1 d . . . H25 H 0.2093 0.8697 0.2186 0.055 Uiso 1 1 calc R . . C26 C 0.22476(9) 0.8062(3) 0.30469(17) 0.0419(8) Uani 1 1 d . . . C27 C 0.23183(8) 0.7125(3) 0.33794(16) 0.0390(8) Uani 1 1 d . . . C28 C 0.22658(8) 0.6177(3) 0.30628(17) 0.0452(9) Uani 1 1 d . . . H28 H 0.2315 0.5530 0.3287 0.054 Uiso 1 1 calc R . . C29 C 0.21410(9) 0.6160(3) 0.24179(17) 0.0435(9) Uani 1 1 d . . . C30 C 0.20900(11) 0.4265(3) 0.2373(2) 0.0635(12) Uani 1 1 d . . . H30A H 0.1949 0.4298 0.2558 0.076 Uiso 1 1 calc R . . H30B H 0.2330 0.4125 0.2715 0.076 Uiso 1 1 calc R . . C31 C 0.19647(13) 0.3408(4) 0.1900(3) 0.0788(15) Uani 1 1 d . . . H31A H 0.1719 0.3499 0.1593 0.118 Uiso 1 1 calc R . . H31B H 0.2005 0.2724 0.2111 0.118 Uiso 1 1 calc R . . H31C H 0.2087 0.3433 0.1682 0.118 Uiso 1 1 calc R . . C32 C 0.22190(12) 0.9963(3) 0.3057(2) 0.0579(11) Uani 1 1 d . . . H32A H 0.1977 0.9975 0.2701 0.069 Uiso 1 1 calc R . . H32B H 0.2367 1.0070 0.2890 0.069 Uiso 1 1 calc R . . C33 C 0.22826(14) 1.0814(4) 0.3524(2) 0.0766(14) Uiso 1 1 d . . . H33A H 0.2109 1.0770 0.3633 0.115 Uiso 1 1 calc R . . H33B H 0.2269 1.1507 0.3338 0.115 Uiso 1 1 calc R . . H33C H 0.2511 1.0721 0.3905 0.115 Uiso 1 1 calc R . . C34 C 0.24539(9) 0.7126(3) 0.40750(17) 0.0478(9) Uani 1 1 d . . . H34A H 0.2594 0.7769 0.4268 0.057 Uiso 1 1 calc R . . H34B H 0.2606 0.6506 0.4273 0.057 Uiso 1 1 calc R . . C35 C 0.21762(8) 0.7094(3) 0.42194(16) 0.0417(8) Uani 1 1 d . . . C36 C 0.20418(8) 0.8032(3) 0.42816(16) 0.0415(8) Uani 1 1 d . . . H36 H 0.2116 0.8685 0.4208 0.050 Uiso 1 1 calc R . . C37 C 0.17998(8) 0.8035(3) 0.44502(16) 0.0390(8) Uani 1 1 d . . . C38 C 0.16910(8) 0.7084(3) 0.45625(15) 0.0384(8) Uani 1 1 d . . . C39 C 0.18192(9) 0.6150(3) 0.44906(17) 0.0444(9) Uani 1 1 d . . . H39 H 0.1743 0.5498 0.4561 0.053 Uiso 1 1 calc R . . C40 C 0.20591(9) 0.6145(3) 0.43152(17) 0.0435(8) Uani 1 1 d . . . C41 C 0.20960(13) 0.4252(3) 0.4347(3) 0.0696(13) Uani 1 1 d . . . H41A H 0.1845 0.4172 0.4065 0.083 Uiso 1 1 calc R . . H41B H 0.2159 0.4201 0.4789 0.083 Uiso 1 1 calc R . . C42 C 0.22767(15) 0.3407(5) 0.4212(3) 0.0898(16) Uiso 1 1 d . . . H42A H 0.2203 0.3441 0.3767 0.135 Uiso 1 1 calc R . . H42B H 0.2220 0.2711 0.4302 0.135 Uiso 1 1 calc R . . H42C H 0.2525 0.3518 0.4478 0.135 Uiso 1 1 calc R . . C43 C 0.17916(11) 0.9931(3) 0.4461(2) 0.0525(10) Uani 1 1 d . . . H43A H 0.1738 0.9997 0.4026 0.063 Uiso 1 1 calc R . . H43B H 0.2043 0.9971 0.4755 0.063 Uiso 1 1 calc R . . C44 C 0.16211(13) 1.0807(3) 0.4599(3) 0.0699(13) Uani 1 1 d . . . H44A H 0.1373 1.0773 0.4298 0.105 Uiso 1 1 calc R . . H44B H 0.1707 1.1490 0.4560 0.105 Uiso 1 1 calc R . . H44C H 0.1672 1.0726 0.5028 0.105 Uiso 1 1 calc R . . C45 C 0.14587(9) 0.7068(3) 0.48193(17) 0.0470(9) Uani 1 1 d . . . H45A H 0.1526 0.7657 0.5122 0.056 Uiso 1 1 calc R . . H45B H 0.1500 0.6401 0.5056 0.056 Uiso 1 1 calc R . . C46 C 0.10732(9) 0.7157(3) 0.43267(17) 0.0424(8) Uani 1 1 d . . . C47 C 0.09108(10) 0.8125(3) 0.41971(18) 0.0484(9) Uani 1 1 d . . . H47 H 0.1043 0.8743 0.4390 0.058 Uiso 1 1 calc R . . C48 C 0.05546(9) 0.8215(3) 0.37860(18) 0.0460(9) Uani 1 1 d . . . C49 C 0.03614(9) 0.7311(3) 0.35212(16) 0.0427(8) Uani 1 1 d . . . C50 C 0.05250(9) 0.6341(3) 0.36409(17) 0.0458(9) Uani 1 1 d . . . H50 H 0.0393 0.5721 0.3451 0.055 Uiso 1 1 calc R . . C51 C 0.08801(9) 0.6261(3) 0.40348(16) 0.0404(8) Uani 1 1 d . . . C52 C 0.08674(10) 0.4359(3) 0.39576(19) 0.0516(10) Uani 1 1 d . . . H52A H 0.0715 0.4364 0.3492 0.062 Uiso 1 1 calc R . . H52B H 0.0724 0.4278 0.4136 0.062 Uiso 1 1 calc R . . C53 C 0.11166(12) 0.3469(3) 0.4166(2) 0.0631(11) Uani 1 1 d . . . H53A H 0.1251 0.3541 0.3973 0.095 Uiso 1 1 calc R . . H53B H 0.0992 0.2797 0.4038 0.095 Uiso 1 1 calc R . . H53C H 0.1271 0.3485 0.4626 0.095 Uiso 1 1 calc R . . C54 C 0.05610(12) 1.0097(4) 0.3864(3) 0.0763(14) Uani 1 1 d . . . H54A H 0.0739 1.0145 0.3762 0.092 Uiso 1 1 calc R . . H54B H 0.0676 1.0114 0.4327 0.092 Uiso 1 1 calc R . . C55 C 0.03222(14) 1.1009(4) 0.3580(3) 0.0825(15) Uiso 1 1 d . . . H55A H 0.0222 1.1019 0.3124 0.124 Uiso 1 1 calc R . . H55B H 0.0448 1.1668 0.3766 0.124 Uiso 1 1 calc R . . H55C H 0.0139 1.0940 0.3663 0.124 Uiso 1 1 calc R . . 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 O1 0.0577(16) 0.0537(17) 0.0667(18) 0.0111(13) 0.0434(15) 0.0010(13) O2 0.0622(17) 0.0547(17) 0.0720(19) 0.0098(14) 0.0463(15) 0.0015(13) O3 0.0416(13) 0.0485(15) 0.0587(16) -0.0104(12) 0.0289(12) -0.0108(11) O4 0.0451(14) 0.0587(17) 0.0505(15) -0.0020(13) 0.0223(12) -0.0155(12) O5 0.0641(17) 0.0531(17) 0.0581(17) -0.0164(13) 0.0352(14) -0.0019(13) O6 0.0694(18) 0.0515(17) 0.0521(16) -0.0094(13) 0.0340(14) -0.0118(13) O7 0.0578(17) 0.0531(17) 0.078(2) -0.0045(14) 0.0435(16) 0.0006(13) O8 0.0494(14) 0.0451(15) 0.0574(16) -0.0019(12) 0.0354(13) -0.0016(11) O9 0.0397(13) 0.0532(16) 0.0524(15) -0.0108(12) 0.0253(12) -0.0017(11) O10 0.0495(15) 0.0512(17) 0.078(2) 0.0032(14) 0.0357(15) 0.0012(13) C1 0.042(2) 0.067(3) 0.042(2) 0.0022(18) 0.0227(17) -0.0009(17) C2 0.0305(16) 0.056(2) 0.0364(18) 0.0005(16) 0.0166(15) -0.0018(15) C3 0.0351(18) 0.049(2) 0.049(2) -0.0029(17) 0.0228(16) -0.0026(15) C4 0.0368(18) 0.047(2) 0.0434(19) 0.0070(16) 0.0207(16) -0.0030(15) C5 0.0268(16) 0.057(2) 0.0390(18) 0.0019(16) 0.0172(15) -0.0041(15) C6 0.0304(17) 0.049(2) 0.0411(19) 0.0015(16) 0.0185(15) -0.0010(15) C7 0.0282(16) 0.047(2) 0.0436(19) 0.0051(16) 0.0179(15) -0.0011(14) C8 0.060(2) 0.052(2) 0.067(3) 0.005(2) 0.034(2) -0.0056(19) C10 0.070(3) 0.049(3) 0.080(3) -0.001(2) 0.041(3) -0.011(2) C12 0.0388(19) 0.062(2) 0.0362(18) 0.0030(16) 0.0189(16) -0.0057(16) C13 0.0369(17) 0.054(2) 0.0319(17) -0.0037(15) 0.0205(15) -0.0097(16) C14 0.0411(19) 0.056(2) 0.0384(18) 0.0008(16) 0.0219(16) -0.0020(16) C15 0.0423(19) 0.054(2) 0.0396(19) -0.0066(16) 0.0257(16) -0.0144(16) C16 0.0350(17) 0.058(2) 0.0346(17) -0.0084(16) 0.0210(15) -0.0076(16) C17 0.0402(19) 0.058(2) 0.0405(19) -0.0113(16) 0.0264(16) -0.0038(16) C18 0.0391(18) 0.053(2) 0.0388(18) -0.0102(16) 0.0252(15) -0.0104(16) C19 0.050(2) 0.055(2) 0.057(2) -0.0076(19) 0.0341(19) -0.0076(18) C20 0.073(3) 0.054(3) 0.078(3) -0.012(2) 0.051(3) -0.017(2) C21 0.068(3) 0.056(3) 0.056(2) -0.004(2) 0.029(2) -0.013(2) C22 0.092(4) 0.064(3) 0.068(3) -0.006(2) 0.031(3) -0.028(3) C23 0.0407(19) 0.066(3) 0.049(2) -0.0119(18) 0.0292(17) -0.0101(17) C24 0.0306(17) 0.062(2) 0.0409(19) -0.0121(17) 0.0207(15) -0.0058(16) C25 0.0403(19) 0.052(2) 0.045(2) -0.0058(17) 0.0230(17) -0.0062(16) C26 0.0398(19) 0.046(2) 0.0425(19) -0.0139(16) 0.0237(16) -0.0114(15) C27 0.0309(16) 0.046(2) 0.0413(18) -0.0063(15) 0.0199(15) -0.0044(14) C28 0.0349(18) 0.055(2) 0.047(2) -0.0052(17) 0.0225(16) 0.0016(15) C29 0.0376(18) 0.050(2) 0.046(2) -0.0103(17) 0.0247(16) -0.0012(15) C30 0.057(2) 0.054(3) 0.083(3) -0.016(2) 0.040(2) -0.0034(19) C31 0.075(3) 0.061(3) 0.096(4) -0.022(3) 0.043(3) -0.004(2) C32 0.067(3) 0.048(2) 0.070(3) -0.007(2) 0.044(2) -0.0051(19) C34 0.0396(19) 0.062(2) 0.041(2) -0.0041(17) 0.0211(16) -0.0025(17) C35 0.0311(17) 0.055(2) 0.0317(17) -0.0050(15) 0.0121(14) -0.0031(15) C36 0.0355(18) 0.049(2) 0.0352(18) -0.0011(15) 0.0160(15) -0.0034(15) C37 0.0324(17) 0.046(2) 0.0360(17) -0.0034(15) 0.0167(15) 0.0003(15) C38 0.0293(16) 0.052(2) 0.0309(16) -0.0016(15) 0.0144(14) -0.0016(14) C39 0.0376(18) 0.044(2) 0.045(2) -0.0014(16) 0.0179(16) -0.0061(15) C40 0.0354(18) 0.045(2) 0.047(2) -0.0039(16) 0.0199(16) -0.0013(15) C41 0.073(3) 0.048(3) 0.096(4) -0.006(2) 0.050(3) -0.002(2) C43 0.058(2) 0.051(2) 0.061(2) 0.0024(18) 0.040(2) 0.0011(18) C44 0.084(3) 0.048(3) 0.100(4) 0.000(2) 0.064(3) 0.002(2) C45 0.045(2) 0.058(2) 0.0400(19) -0.0063(17) 0.0241(17) -0.0067(17) C46 0.0375(18) 0.056(2) 0.0405(19) -0.0002(16) 0.0252(16) -0.0014(16) C47 0.049(2) 0.050(2) 0.055(2) -0.0006(18) 0.0340(19) -0.0045(17) C48 0.042(2) 0.054(2) 0.051(2) 0.0020(17) 0.0306(18) -0.0028(17) C49 0.0388(18) 0.060(2) 0.0377(18) -0.0005(16) 0.0260(16) 0.0009(16) C50 0.0415(19) 0.058(2) 0.044(2) -0.0106(17) 0.0270(17) -0.0067(17) C51 0.0388(18) 0.052(2) 0.0391(18) -0.0024(16) 0.0267(16) -0.0021(16) C52 0.046(2) 0.060(2) 0.053(2) -0.0061(19) 0.0299(18) -0.0039(18) C53 0.071(3) 0.061(3) 0.066(3) -0.008(2) 0.042(2) 0.001(2) C54 0.059(3) 0.065(3) 0.095(4) 0.005(3) 0.036(3) -0.003(2) _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 O1 C7 1.382(4) . ? O1 C8 1.424(5) . ? O2 C4 1.383(4) . ? O2 C10 1.441(5) . ? O3 C18 1.389(4) . ? O3 C19 1.413(5) . ? O4 C15 1.384(4) . ? O4 C21 1.411(5) . ? O5 C29 1.380(4) . ? O5 C30 1.416(5) . ? O6 C26 1.381(4) . ? O6 C32 1.429(5) . ? O7 C40 1.385(4) . ? O7 C41 1.418(5) . ? O8 C37 1.380(4) . ? O8 C43 1.434(4) . ? O9 C51 1.380(4) . ? O9 C52 1.431(4) . ? O10 C48 1.372(5) . ? O10 C54 1.395(5) . ? C1 C2 1.517(5) . ? C1 C49 1.541(5) 2 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.394(5) . ? C2 C3 1.394(5) . ? C3 C4 1.383(5) . ? C3 H3 0.9500 . ? C4 C5 1.386(5) . ? C5 C6 1.392(5) . ? C5 C12 1.527(5) . ? C6 C7 1.376(5) . ? C6 H6 0.9500 . ? C8 C9 1.504(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.501(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.510(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.383(5) . ? C13 C14 1.394(5) . ? C14 C15 1.407(5) . ? C14 H14 0.9500 . ? C15 C16 1.390(5) . ? C16 C17 1.394(5) . ? C16 C23 1.506(5) . ? C17 C18 1.397(5) . ? C17 H17 0.9500 . ? C19 C20 1.495(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.487(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.530(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.381(5) . ? C24 C25 1.394(5) . ? C25 C26 1.401(5) . ? C25 H25 0.9500 . ? C26 C27 1.385(5) . ? C27 C28 1.388(5) . ? C27 C34 1.510(5) . ? C28 C29 1.401(5) . ? C28 H28 0.9500 . ? C30 C31 1.479(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.502(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.515(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.388(5) . ? C35 C40 1.392(5) . ? C36 C37 1.397(5) . ? C36 H36 0.9500 . ? C37 C38 1.391(5) . ? C38 C39 1.378(5) . ? C38 C45 1.526(5) . ? C39 C40 1.401(5) . ? C39 H39 0.9500 . ? C41 C42 1.507(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.506(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.534(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.381(5) . ? C46 C51 1.385(5) . ? C47 C48 1.403(5) . ? C47 H47 0.9500 . ? C48 C49 1.382(5) . ? C49 C50 1.388(5) . ? C49 C1 1.541(5) 2 ? C50 C51 1.394(5) . ? C50 H50 0.9500 . ? C52 C53 1.491(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.488(7) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? 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 C7 O1 C8 117.8(3) . . ? C4 O2 C10 117.5(3) . . ? C18 O3 C19 118.4(3) . . ? C15 O4 C21 119.4(3) . . ? C29 O5 C30 118.7(3) . . ? C26 O6 C32 118.1(3) . . ? C40 O7 C41 117.8(3) . . ? C37 O8 C43 117.1(3) . . ? C51 O9 C52 118.3(3) . . ? C48 O10 C54 119.4(3) . . ? C2 C1 C49 110.2(3) . 2 ? C2 C1 H1A 109.6 . . ? C49 C1 H1A 109.6 2 . ? C2 C1 H1B 109.6 . . ? C49 C1 H1B 109.6 2 . ? H1A C1 H1B 108.1 . . ? C7 C2 C3 118.0(3) . . ? C7 C2 C1 121.3(3) . . ? C3 C2 C1 120.6(3) . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 O2 123.9(3) . . ? C3 C4 C5 120.3(3) . . ? O2 C4 C5 115.8(3) . . ? C4 C5 C6 118.4(3) . . ? C4 C5 C12 121.2(3) . . ? C6 C5 C12 120.5(3) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 O1 124.4(3) . . ? C6 C7 C2 120.4(3) . . ? O1 C7 C2 115.2(3) . . ? O1 C8 C9 107.5(4) . . ? O1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? O1 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C11 107.0(4) . . ? O2 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? O2 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C5 112.0(3) . . ? C13 C12 H12A 109.2 . . ? C5 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C5 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C18 C13 C14 118.7(3) . . ? C18 C13 C12 120.9(3) . . ? C14 C13 C12 120.3(3) . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? O4 C15 C16 116.2(3) . . ? O4 C15 C14 122.9(3) . . ? C16 C15 C14 120.9(3) . . ? C15 C16 C17 118.0(3) . . ? C15 C16 C23 121.3(3) . . ? C17 C16 C23 120.5(3) . . ? C16 C17 C18 121.2(3) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C13 C18 O3 116.1(3) . . ? C13 C18 C17 120.8(3) . . ? O3 C18 C17 123.1(3) . . ? O3 C19 C20 108.9(3) . . ? O3 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O3 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 C22 108.2(4) . . ? O4 C21 H21A 110.1 . . ? C22 C21 H21A 110.1 . . ? O4 C21 H21B 110.1 . . ? C22 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 C24 110.3(3) . . ? C16 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? C16 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C29 C24 C25 119.0(3) . . ? C29 C24 C23 121.8(3) . . ? C25 C24 C23 119.1(4) . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? O6 C26 C27 116.1(3) . . ? O6 C26 C25 123.5(3) . . ? C27 C26 C25 120.4(3) . . ? C26 C27 C28 118.7(3) . . ? C26 C27 C34 121.1(3) . . ? C28 C27 C34 120.2(3) . . ? C27 C28 C29 121.0(4) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? O5 C29 C24 116.7(3) . . ? O5 C29 C28 123.2(3) . . ? C24 C29 C28 120.1(3) . . ? O5 C30 C31 109.1(4) . . ? O5 C30 H30A 109.9 . . ? C31 C30 H30A 109.9 . . ? O5 C30 H30B 109.9 . . ? C31 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C32 C33 107.0(4) . . ? O6 C32 H32A 110.3 . . ? C33 C32 H32A 110.3 . . ? O6 C32 H32B 110.3 . . ? C33 C32 H32B 110.3 . . ? H32A C32 H32B 108.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C27 C34 C35 113.8(3) . . ? C27 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? C27 C34 H34B 108.8 . . ? C35 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C40 118.5(3) . . ? C36 C35 C34 119.7(3) . . ? C40 C35 C34 121.7(3) . . ? C35 C36 C37 121.2(3) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? O8 C37 C38 116.4(3) . . ? O8 C37 C36 123.6(3) . . ? C38 C37 C36 119.9(3) . . ? C39 C38 C37 119.0(3) . . ? C39 C38 C45 119.8(3) . . ? C37 C38 C45 121.0(3) . . ? C38 C39 C40 121.1(3) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? O7 C40 C35 115.6(3) . . ? O7 C40 C39 124.3(3) . . ? C35 C40 C39 120.1(3) . . ? O7 C41 C42 107.0(4) . . ? O7 C41 H41A 110.3 . . ? C42 C41 H41A 110.3 . . ? O7 C41 H41B 110.3 . . ? C42 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O8 C43 C44 108.0(3) . . ? O8 C43 H43A 110.1 . . ? C44 C43 H43A 110.1 . . ? O8 C43 H43B 110.1 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C38 C45 C46 115.8(3) . . ? C38 C45 H45A 108.3 . . ? C46 C45 H45A 108.3 . . ? C38 C45 H45B 108.3 . . ? C46 C45 H45B 108.3 . . ? H45A C45 H45B 107.4 . . ? C47 C46 C51 119.1(3) . . ? C47 C46 C45 120.3(3) . . ? C51 C46 C45 120.4(3) . . ? C46 C47 C48 121.4(4) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? O10 C48 C49 116.7(3) . . ? O10 C48 C47 124.1(3) . . ? C49 C48 C47 119.2(3) . . ? C48 C49 C50 119.4(3) . . ? C48 C49 C1 120.4(3) . 2 ? C50 C49 C1 120.1(3) . 2 ? C49 C50 C51 121.0(3) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? O9 C51 C46 116.3(3) . . ? O9 C51 C50 124.0(3) . . ? C46 C51 C50 119.7(3) . . ? O9 C52 C53 107.9(3) . . ? O9 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? O9 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O10 C54 C55 109.7(4) . . ? O10 C54 H54A 109.7 . . ? C55 C54 H54A 109.7 . . ? O10 C54 H54B 109.7 . . ? C55 C54 H54B 109.7 . . ? H54A C54 H54B 108.2 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.423 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.076 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.099 0.250 742.9 177.9 2 0.000 -0.127 0.750 743.3 178.0 3 0.500 -0.169 0.250 742.9 177.9 4 0.500 0.143 0.750 743.3 178.0 5 0.301 0.040 0.914 8.7 0.3 6 0.500 0.042 0.750 8.9 0.4 7 0.699 0.040 0.586 8.7 0.3 8 0.298 0.217 0.470 6.8 0.2 9 0.702 0.217 0.030 6.8 0.1 10 0.202 0.283 0.530 6.8 0.2 11 0.798 0.283 0.970 6.8 0.2 12 0.000 0.458 0.250 9.3 0.4 13 0.199 0.459 0.086 8.7 0.3 14 0.801 0.459 0.414 8.7 0.3 15 0.000 0.542 0.750 8.9 0.4 16 0.199 0.540 0.586 8.7 0.3 17 0.801 0.540 0.914 8.7 0.3 18 0.202 0.717 0.030 6.8 0.1 19 0.798 0.717 0.470 6.8 0.2 20 0.298 0.783 0.970 6.8 0.2 21 0.702 0.783 0.530 6.8 0.2 22 0.301 0.959 0.414 8.7 0.3 23 0.500 0.958 0.250 9.3 0.4 24 0.699 0.959 0.086 8.7 0.3 _platon_squeeze_details ; The disordered solvents within the void were not crystallographically well defined. The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 3134.3 Ang^3^, and a void electron population of 717 per cell. Because the solvent we used in the synthesis is acetone, the amount of the disordered solvent was about 24 per cell suggested by electron count. The overall formula should be (C110H140O20).6(C3OH6), considering the contribution of solvent. Refinement after the SQUEEZE routine gave significantly improved R values. [R values before SQUEEZE] R1 = 0.1700, wR2 = 0.4740, GooF = S = 1.943 for all data ;