# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_03289a _database_code_depnum_ccdc_archive 'CCDC 886641' #TrackingRef 'web_deposit_cif_file_0_ZhenguoChi_1339763597.DSA7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H50 O2' _chemical_formula_sum 'C44 H50 O2' _chemical_formula_weight 610.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0098(5) _cell_length_b 15.1250(8) _cell_length_c 20.0151(10) _cell_angle_alpha 74.953(4) _cell_angle_beta 80.961(4) _cell_angle_gamma 79.000(4) _cell_volume 2568.9(2) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11416 _cell_measurement_theta_min 3.0611 _cell_measurement_theta_max 66.9486 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8139 _exptl_absorpt_correction_T_max 0.8556 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_detector_area_resol_mean 10.5058 _diffrn_reflns_number 30374 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.1395 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 67.05 _reflns_number_total 9111 _reflns_number_gt 7275 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) ; _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^)+(0.0973P)^2^+0.1058P] 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 9111 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.63852(16) 0.51771(10) 0.86194(7) 0.0257(3) Uani 1 1 d . . . C2 C 0.68605(16) 0.46186(10) 0.92557(7) 0.0243(3) Uani 1 1 d . . . C3 C 0.82797(17) 0.46656(10) 0.94669(7) 0.0277(3) Uani 1 1 d . . . H3 H 0.8947 0.5043 0.9157 0.033 Uiso 1 1 calc R . . C4 C 0.87008(17) 0.41844(11) 1.01000(7) 0.0295(3) Uani 1 1 d . . . H4 H 0.9651 0.4227 1.0228 0.035 Uiso 1 1 calc R . . C5 C 0.77160(18) 0.36171(10) 1.05688(7) 0.0291(3) Uani 1 1 d . . . H5 H 0.7990 0.3303 1.1019 0.035 Uiso 1 1 calc R . . C6 C 0.63894(17) 0.35202(10) 1.03787(7) 0.0267(3) Uani 1 1 d . . . H6 H 0.5755 0.3131 1.0699 0.032 Uiso 1 1 calc R . . C7 C 0.59134(16) 0.39878(10) 0.97084(7) 0.0239(3) Uani 1 1 d . . . C8 C 0.45302(16) 0.39008(10) 0.95007(7) 0.0248(3) Uani 1 1 d . . . C9 C 0.40580(16) 0.44590(10) 0.88633(7) 0.0256(3) Uani 1 1 d . . . C10 C 0.26470(17) 0.44165(11) 0.86399(7) 0.0303(3) Uani 1 1 d . . . H10 H 0.2040 0.3974 0.8914 0.036 Uiso 1 1 calc R . . C11 C 0.21497(18) 0.49877(12) 0.80487(8) 0.0349(4) Uani 1 1 d . . . H11 H 0.1200 0.4947 0.7918 0.042 Uiso 1 1 calc R . . C12 C 0.30444(19) 0.56468(12) 0.76226(8) 0.0355(4) Uani 1 1 d . . . H12 H 0.2685 0.6052 0.7212 0.043 Uiso 1 1 calc R . . C13 C 0.44119(18) 0.56971(11) 0.78021(7) 0.0310(3) Uani 1 1 d . . . H13 H 0.5007 0.6132 0.7507 0.037 Uiso 1 1 calc R . . C14 C 0.49815(16) 0.51139(10) 0.84229(7) 0.0252(3) Uani 1 1 d . . . C15 C 0.73181(17) 0.58911(11) 0.82127(7) 0.0294(3) Uani 1 1 d . . . H15 H 0.7373 0.6376 0.8425 0.035 Uiso 1 1 calc R . . C16 C 0.80770(18) 0.59247(11) 0.75903(7) 0.0300(3) Uani 1 1 d . . . H16 H 0.8039 0.5435 0.7380 0.036 Uiso 1 1 calc R . . C17 C 0.89785(16) 0.66427(11) 0.71860(7) 0.0277(3) Uani 1 1 d . . . C18 C 0.96774(18) 0.65959(11) 0.65242(7) 0.0316(3) Uani 1 1 d . . . H18 H 0.9612 0.6077 0.6352 0.038 Uiso 1 1 calc R . . C19 C 1.04727(18) 0.72845(11) 0.61038(7) 0.0314(3) Uani 1 1 d . . . H19 H 1.0936 0.7235 0.5652 0.038 Uiso 1 1 calc R . . C20 C 1.05787(17) 0.80389(11) 0.63519(7) 0.0297(3) Uani 1 1 d . . . C21 C 0.9951(2) 0.80783(12) 0.70263(8) 0.0388(4) Uani 1 1 d . . . H21 H 1.0072 0.8578 0.7208 0.047 Uiso 1 1 calc R . . C22 C 0.9155(2) 0.73996(12) 0.74312(8) 0.0358(4) Uani 1 1 d . . . H22 H 0.8716 0.7445 0.7887 0.043 Uiso 1 1 calc R . . C23 C 0.35131(16) 0.32688(10) 0.99515(7) 0.0253(3) Uani 1 1 d . . . H23 H 0.2470 0.3526 1.0026 0.030 Uiso 1 1 calc R . . C24 C 0.39013(16) 0.23784(10) 1.02647(7) 0.0269(3) Uani 1 1 d . . . H24 H 0.4935 0.2107 1.0185 0.032 Uiso 1 1 calc R . . C25 C 0.28544(16) 0.17831(10) 1.07246(7) 0.0255(3) Uani 1 1 d . . . C26 C 0.34224(17) 0.09926(10) 1.12061(7) 0.0287(3) Uani 1 1 d . . . H26 H 0.4492 0.0833 1.1217 0.034 Uiso 1 1 calc R . . C27 C 0.24733(17) 0.04284(10) 1.16716(7) 0.0287(3) Uani 1 1 d . . . H27 H 0.2891 -0.0103 1.1997 0.034 Uiso 1 1 calc R . . C28 C 0.09164(17) 0.06527(10) 1.16531(7) 0.0266(3) Uani 1 1 d . . . C29 C 0.03190(17) 0.14296(10) 1.11659(7) 0.0268(3) Uani 1 1 d . . . H29 H -0.0750 0.1580 1.1149 0.032 Uiso 1 1 calc R . . C30 C 0.12751(16) 0.19799(10) 1.07093(7) 0.0256(3) Uani 1 1 d . . . H30 H 0.0854 0.2503 1.0378 0.031 Uiso 1 1 calc R . . C31 C 1.18440(18) 0.88105(11) 0.52738(7) 0.0318(3) Uani 1 1 d . . . H31A H 1.1037 0.8750 0.5013 0.038 Uiso 1 1 calc R . . H31B H 1.2695 0.8295 0.5246 0.038 Uiso 1 1 calc R . . C32 C 1.23935(19) 0.97310(12) 0.49708(8) 0.0358(4) Uani 1 1 d . . . H32A H 1.3150 0.9796 0.5257 0.043 Uiso 1 1 calc R . . H32B H 1.1523 1.0237 0.4994 0.043 Uiso 1 1 calc R . . C33 C 1.31112(19) 0.98353(12) 0.42193(8) 0.0358(4) Uani 1 1 d . . . H33A H 1.3954 0.9314 0.4194 0.043 Uiso 1 1 calc R . . H33B H 1.2341 0.9796 0.3930 0.043 Uiso 1 1 calc R . . C34 C 1.37239(19) 1.07429(12) 0.39208(8) 0.0356(4) Uani 1 1 d . . . H34A H 1.4415 1.0808 0.4238 0.043 Uiso 1 1 calc R . . H34B H 1.2862 1.1261 0.3908 0.043 Uiso 1 1 calc R . . C35 C 1.45764(19) 1.08311(11) 0.31948(8) 0.0351(4) Uani 1 1 d . . . H35A H 1.5391 1.0289 0.3198 0.042 Uiso 1 1 calc R . . H35B H 1.3864 1.0818 0.2869 0.042 Uiso 1 1 calc R . . C36 C 1.5283(2) 1.17092(12) 0.29277(8) 0.0402(4) Uani 1 1 d . . . H36A H 1.4468 1.2252 0.2920 0.048 Uiso 1 1 calc R . . H36B H 1.5989 1.1725 0.3255 0.048 Uiso 1 1 calc R . . C37 C 1.6143(2) 1.17908(13) 0.22052(9) 0.0482(5) Uani 1 1 d . . . H37A H 1.6893 1.1230 0.2197 0.072 Uiso 1 1 calc R . . H37B H 1.6666 1.2333 0.2085 0.072 Uiso 1 1 calc R . . H37C H 1.5427 1.1862 0.1867 0.072 Uiso 1 1 calc R . . C38 C 0.03165(18) -0.05436(11) 1.26719(7) 0.0321(3) Uani 1 1 d . . . H38A H 0.0911 -0.0310 1.2947 0.038 Uiso 1 1 calc R . . H38B H 0.0947 -0.1086 1.2523 0.038 Uiso 1 1 calc R . . C39 C -0.11502(19) -0.08025(12) 1.30951(8) 0.0368(4) Uani 1 1 d . . . H39A H -0.1703 -0.1047 1.2810 0.044 Uiso 1 1 calc R . . H39B H -0.1795 -0.0234 1.3197 0.044 Uiso 1 1 calc R . . C40 C -0.09383(18) -0.15180(11) 1.37788(7) 0.0328(3) Uani 1 1 d . . . H40A H -0.0482 -0.1257 1.4089 0.039 Uiso 1 1 calc R . . H40B H -0.0232 -0.2072 1.3688 0.039 Uiso 1 1 calc R . . C41 C -0.24570(19) -0.17984(12) 1.41370(8) 0.0365(4) Uani 1 1 d . . . H41A H -0.3176 -0.1230 1.4186 0.044 Uiso 1 1 calc R . . H41B H -0.2870 -0.2087 1.3830 0.044 Uiso 1 1 calc R . . C42 C -0.24119(19) -0.24655(11) 1.48512(7) 0.0338(4) Uani 1 1 d . . . H42A H -0.2092 -0.2163 1.5176 0.041 Uiso 1 1 calc R . . H42B H -0.1647 -0.3021 1.4816 0.041 Uiso 1 1 calc R . . C43 C -0.3955(2) -0.27650(14) 1.51436(9) 0.0457(4) Uani 1 1 d . . . H43A H -0.4706 -0.2209 1.5192 0.055 Uiso 1 1 calc R . . H43B H -0.4290 -0.3039 1.4805 0.055 Uiso 1 1 calc R . . C44 C -0.3958(2) -0.34614(14) 1.58434(9) 0.0493(5) Uani 1 1 d . . . H44A H -0.3284 -0.4036 1.5793 0.074 Uiso 1 1 calc R . . H44B H -0.4994 -0.3592 1.6010 0.074 Uiso 1 1 calc R . . H44C H -0.3597 -0.3205 1.6180 0.074 Uiso 1 1 calc R . . C45 C 0.09851(17) 0.55958(10) 0.45488(7) 0.0276(3) Uani 1 1 d . . . C46 C -0.03575(17) 0.54874(10) 0.43203(7) 0.0274(3) Uani 1 1 d . . . C47 C -0.08370(19) 0.59907(11) 0.36579(7) 0.0316(3) Uani 1 1 d . . . H47 H -0.0202 0.6390 0.3349 0.038 Uiso 1 1 calc R . . C48 C -0.2174(2) 0.59137(12) 0.34584(8) 0.0360(4) Uani 1 1 d . . . H48 H -0.2465 0.6266 0.3019 0.043 Uiso 1 1 calc R . . C49 C -0.31324(19) 0.53119(12) 0.39029(8) 0.0368(4) Uani 1 1 d . . . H49 H -0.4053 0.5249 0.3757 0.044 Uiso 1 1 calc R . . C50 C 0.27347(18) 0.51762(12) 0.54617(8) 0.0335(4) Uani 1 1 d . . . H50 H 0.3398 0.5569 0.5166 0.040 Uiso 1 1 calc R . . C51 C 0.13504(17) 0.51163(10) 0.52250(7) 0.0277(3) Uani 1 1 d . . . C52 C 0.19912(17) 0.62474(11) 0.41225(7) 0.0296(3) Uani 1 1 d . . . H52 H 0.2182 0.6704 0.4332 0.036 Uiso 1 1 calc R . . C53 C 0.26620(18) 0.62670(11) 0.34766(7) 0.0305(3) Uani 1 1 d . . . H53 H 0.2507 0.5799 0.3269 0.037 Uiso 1 1 calc R . . C54 C 0.36170(17) 0.69423(11) 0.30549(7) 0.0286(3) Uani 1 1 d . . . C55 C 0.42413(18) 0.68758(11) 0.23849(8) 0.0325(3) Uani 1 1 d . . . H55 H 0.4067 0.6378 0.2215 0.039 Uiso 1 1 calc R . . C56 C 0.51152(18) 0.75168(11) 0.19554(7) 0.0325(3) Uani 1 1 d . . . H56 H 0.5515 0.7460 0.1498 0.039 Uiso 1 1 calc R . . C57 C 0.53958(17) 0.82374(11) 0.22017(7) 0.0285(3) Uani 1 1 d . . . C58 C 0.47975(19) 0.83086(11) 0.28741(7) 0.0334(4) Uani 1 1 d . . . H58 H 0.4994 0.8798 0.3047 0.040 Uiso 1 1 calc R . . C59 C 0.39266(19) 0.76779(11) 0.32890(7) 0.0336(4) Uani 1 1 d . . . H59 H 0.3524 0.7742 0.3745 0.040 Uiso 1 1 calc R . . C60 C 0.65091(18) 0.90595(11) 0.10988(7) 0.0302(3) Uani 1 1 d . . . H60A H 0.5529 0.9223 0.0898 0.036 Uiso 1 1 calc R . . H60B H 0.7085 0.8496 0.0961 0.036 Uiso 1 1 calc R . . C61 C 0.74162(17) 0.98529(11) 0.08440(7) 0.0290(3) Uani 1 1 d . . . H61A H 0.8474 0.9625 0.0956 0.035 Uiso 1 1 calc R . . H61B H 0.6976 1.0340 0.1099 0.035 Uiso 1 1 calc R . . C62 C 0.74477(17) 1.02805(11) 0.00674(7) 0.0297(3) Uani 1 1 d . . . H62A H 0.6392 1.0491 -0.0053 0.036 Uiso 1 1 calc R . . H62B H 0.7937 0.9806 -0.0192 0.036 Uiso 1 1 calc R . . C63 C 0.83177(17) 1.11006(11) -0.01505(7) 0.0283(3) Uani 1 1 d . . . H63A H 0.7795 1.1576 0.0102 0.034 Uiso 1 1 calc R . . H63B H 0.9347 1.0888 0.0001 0.034 Uiso 1 1 calc R . . C64 C 0.84873(18) 1.15558(11) -0.09235(7) 0.0328(3) Uani 1 1 d . . . H64A H 0.7465 1.1778 -0.1082 0.039 Uiso 1 1 calc R . . H64B H 0.9028 1.1091 -0.1183 0.039 Uiso 1 1 calc R . . C65 C 0.9366(2) 1.23705(12) -0.10873(8) 0.0363(4) Uani 1 1 d . . . H65A H 0.8740 1.2874 -0.0888 0.044 Uiso 1 1 calc R . . H65B H 1.0307 1.2169 -0.0855 0.044 Uiso 1 1 calc R . . C66 C 0.9792(3) 1.27529(16) -0.18562(9) 0.0578(6) Uani 1 1 d . . . H66A H 1.0475 1.2273 -0.2052 0.087 Uiso 1 1 calc R . . H66B H 1.0308 1.3289 -0.1921 0.087 Uiso 1 1 calc R . . H66C H 0.8870 1.2944 -0.2094 0.087 Uiso 1 1 calc R . . O1 O 1.12615(14) 0.87825(8) 0.59835(5) 0.0395(3) Uani 1 1 d . . . O2 O -0.01455(12) 0.01699(8) 1.20797(5) 0.0318(3) Uani 1 1 d . . . O3 O 0.62514(13) 0.89026(8) 0.18411(5) 0.0344(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0239(7) 0.0304(7) 0.0256(7) -0.0117(6) 0.0059(5) -0.0110(6) C2 0.0229(7) 0.0288(7) 0.0243(7) -0.0127(5) 0.0054(5) -0.0094(6) C3 0.0240(8) 0.0323(7) 0.0305(7) -0.0134(6) 0.0061(6) -0.0131(6) C4 0.0238(8) 0.0345(8) 0.0357(8) -0.0141(6) -0.0023(6) -0.0113(6) C5 0.0307(8) 0.0316(7) 0.0278(7) -0.0090(6) -0.0028(6) -0.0097(6) C6 0.0267(8) 0.0309(7) 0.0249(6) -0.0097(5) 0.0036(5) -0.0115(6) C7 0.0233(7) 0.0266(7) 0.0242(6) -0.0117(5) 0.0058(5) -0.0090(6) C8 0.0226(7) 0.0275(7) 0.0259(7) -0.0111(5) 0.0060(5) -0.0089(6) C9 0.0230(7) 0.0309(7) 0.0266(7) -0.0132(6) 0.0038(5) -0.0096(6) C10 0.0269(8) 0.0360(8) 0.0318(7) -0.0119(6) 0.0013(6) -0.0126(6) C11 0.0296(8) 0.0444(9) 0.0361(8) -0.0130(7) -0.0056(6) -0.0123(7) C12 0.0373(9) 0.0408(9) 0.0302(7) -0.0070(6) -0.0063(6) -0.0106(7) C13 0.0341(8) 0.0337(8) 0.0271(7) -0.0087(6) 0.0019(6) -0.0118(7) C14 0.0248(7) 0.0294(7) 0.0242(6) -0.0112(5) 0.0034(5) -0.0090(6) C15 0.0285(8) 0.0341(8) 0.0291(7) -0.0101(6) 0.0038(6) -0.0154(6) C16 0.0310(8) 0.0358(8) 0.0285(7) -0.0117(6) 0.0027(6) -0.0172(7) C17 0.0245(7) 0.0366(8) 0.0247(7) -0.0088(6) 0.0013(6) -0.0125(6) C18 0.0336(8) 0.0366(8) 0.0296(7) -0.0145(6) 0.0055(6) -0.0158(7) C19 0.0317(8) 0.0406(9) 0.0241(7) -0.0108(6) 0.0061(6) -0.0140(7) C20 0.0275(8) 0.0381(8) 0.0252(7) -0.0057(6) 0.0026(6) -0.0160(7) C21 0.0526(10) 0.0434(9) 0.0283(7) -0.0148(6) 0.0065(7) -0.0270(8) C22 0.0441(9) 0.0439(9) 0.0243(7) -0.0125(6) 0.0092(6) -0.0233(8) C23 0.0183(7) 0.0330(8) 0.0281(7) -0.0117(6) 0.0024(5) -0.0104(6) C24 0.0204(7) 0.0332(8) 0.0304(7) -0.0113(6) 0.0023(5) -0.0112(6) C25 0.0240(7) 0.0312(7) 0.0263(7) -0.0127(6) 0.0018(5) -0.0124(6) C26 0.0214(7) 0.0329(8) 0.0342(7) -0.0101(6) -0.0021(6) -0.0079(6) C27 0.0283(8) 0.0316(7) 0.0285(7) -0.0056(6) -0.0042(6) -0.0115(6) C28 0.0289(8) 0.0338(8) 0.0227(6) -0.0101(6) 0.0007(5) -0.0167(6) C29 0.0223(7) 0.0367(8) 0.0253(7) -0.0097(6) -0.0009(5) -0.0125(6) C30 0.0255(7) 0.0302(7) 0.0238(6) -0.0072(5) -0.0019(5) -0.0107(6) C31 0.0291(8) 0.0423(9) 0.0243(7) -0.0073(6) 0.0049(6) -0.0139(7) C32 0.0369(9) 0.0429(9) 0.0288(8) -0.0079(6) 0.0071(6) -0.0184(7) C33 0.0374(9) 0.0414(9) 0.0294(7) -0.0082(6) 0.0075(6) -0.0172(7) C34 0.0386(9) 0.0417(9) 0.0281(7) -0.0090(6) 0.0065(6) -0.0177(7) C35 0.0389(9) 0.0365(8) 0.0305(7) -0.0088(6) 0.0081(6) -0.0162(7) C36 0.0481(10) 0.0409(9) 0.0337(8) -0.0106(7) 0.0105(7) -0.0215(8) C37 0.0601(12) 0.0449(10) 0.0388(9) -0.0097(7) 0.0162(8) -0.0242(9) C38 0.0354(9) 0.0378(8) 0.0253(7) -0.0042(6) -0.0022(6) -0.0164(7) C39 0.0358(9) 0.0466(9) 0.0291(8) -0.0033(7) -0.0002(6) -0.0199(8) C40 0.0348(9) 0.0391(8) 0.0268(7) -0.0073(6) 0.0004(6) -0.0151(7) C41 0.0369(9) 0.0439(9) 0.0296(7) -0.0037(7) -0.0015(6) -0.0177(7) C42 0.0386(9) 0.0366(8) 0.0267(7) -0.0080(6) 0.0030(6) -0.0116(7) C43 0.0468(11) 0.0554(11) 0.0365(9) -0.0041(8) 0.0011(7) -0.0256(9) C44 0.0622(12) 0.0502(11) 0.0344(8) -0.0085(8) 0.0133(8) -0.0240(9) C45 0.0300(8) 0.0314(8) 0.0238(7) -0.0112(6) 0.0026(6) -0.0092(6) C46 0.0299(8) 0.0318(7) 0.0228(6) -0.0106(6) 0.0022(6) -0.0088(6) C47 0.0363(9) 0.0357(8) 0.0245(7) -0.0088(6) 0.0007(6) -0.0109(7) C48 0.0421(9) 0.0424(9) 0.0263(7) -0.0083(6) -0.0075(6) -0.0104(7) C49 0.0337(9) 0.0455(9) 0.0361(8) -0.0110(7) -0.0068(7) -0.0141(7) C50 0.0319(9) 0.0422(9) 0.0297(7) -0.0108(6) 0.0006(6) -0.0138(7) C51 0.0286(8) 0.0322(8) 0.0251(7) -0.0125(6) 0.0025(6) -0.0084(6) C52 0.0302(8) 0.0347(8) 0.0273(7) -0.0099(6) -0.0008(6) -0.0118(7) C53 0.0324(8) 0.0324(8) 0.0296(7) -0.0100(6) 0.0002(6) -0.0118(6) C54 0.0277(8) 0.0332(8) 0.0259(7) -0.0078(6) -0.0010(6) -0.0078(6) C55 0.0348(8) 0.0359(8) 0.0311(7) -0.0152(6) 0.0031(6) -0.0122(7) C56 0.0333(8) 0.0395(8) 0.0262(7) -0.0119(6) 0.0054(6) -0.0109(7) C57 0.0254(8) 0.0349(8) 0.0260(7) -0.0048(6) -0.0021(6) -0.0108(6) C58 0.0408(9) 0.0385(8) 0.0267(7) -0.0108(6) -0.0024(6) -0.0174(7) C59 0.0420(9) 0.0394(9) 0.0229(7) -0.0101(6) 0.0024(6) -0.0164(7) C60 0.0293(8) 0.0380(8) 0.0253(7) -0.0094(6) 0.0011(6) -0.0110(6) C61 0.0223(7) 0.0396(8) 0.0283(7) -0.0119(6) 0.0007(6) -0.0105(6) C62 0.0256(7) 0.0388(8) 0.0287(7) -0.0111(6) -0.0013(6) -0.0115(6) C63 0.0246(7) 0.0357(8) 0.0283(7) -0.0117(6) -0.0015(6) -0.0092(6) C64 0.0312(8) 0.0412(9) 0.0287(7) -0.0066(6) -0.0038(6) -0.0141(7) C65 0.0373(9) 0.0380(9) 0.0359(8) -0.0106(7) 0.0010(7) -0.0129(7) C66 0.0657(13) 0.0702(14) 0.0403(9) 0.0022(9) -0.0052(9) -0.0389(11) O1 0.0526(7) 0.0459(7) 0.0252(5) -0.0097(5) 0.0105(5) -0.0312(6) O2 0.0293(6) 0.0413(6) 0.0253(5) -0.0004(4) -0.0010(4) -0.0189(5) O3 0.0388(6) 0.0446(6) 0.0245(5) -0.0080(4) 0.0012(4) -0.0221(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C14 1.409(2) . ? C1 C2 1.412(2) . ? C1 C15 1.4867(18) . ? C2 C3 1.428(2) . ? C2 C7 1.4418(18) . ? C3 C4 1.359(2) . ? C3 H3 0.9500 . ? C4 C5 1.4195(19) . ? C4 H4 0.9500 . ? C5 C6 1.354(2) . ? C5 H5 0.9500 . ? C6 C7 1.434(2) . ? C6 H6 0.9500 . ? C7 C8 1.413(2) . ? C8 C9 1.413(2) . ? C8 C23 1.4813(17) . ? C9 C10 1.430(2) . ? C9 C14 1.4427(18) . ? C10 C11 1.355(2) . ? C10 H10 0.9500 . ? C11 C12 1.421(2) . ? C11 H11 0.9500 . ? C12 C13 1.357(2) . ? C12 H12 0.9500 . ? C13 C14 1.430(2) . ? C13 H13 0.9500 . ? C15 C16 1.317(2) . ? C15 H15 0.9500 . ? C16 C17 1.4723(18) . ? C16 H16 0.9500 . ? C17 C18 1.388(2) . ? C17 C22 1.401(2) . ? C18 C19 1.395(2) . ? C18 H18 0.9500 . ? C19 C20 1.381(2) . ? C19 H19 0.9500 . ? C20 O1 1.3705(17) . ? C20 C21 1.391(2) . ? C21 C22 1.375(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.334(2) . ? C23 H23 0.9500 . ? C24 C25 1.4726(18) . ? C24 H24 0.9500 . ? C25 C26 1.394(2) . ? C25 C30 1.401(2) . ? C26 C27 1.3939(19) . ? C26 H26 0.9500 . ? C27 C28 1.383(2) . ? C27 H27 0.9500 . ? C28 O2 1.3652(16) . ? C28 C29 1.396(2) . ? C29 C30 1.3789(19) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O1 1.4275(18) . ? C31 C32 1.511(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.522(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.518(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.519(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.517(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.516(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 O2 1.4360(18) . ? C38 C39 1.513(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.521(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.524(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.522(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.526(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.518(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.410(2) . ? C45 C51 1.416(2) . ? C45 C52 1.4773(19) . ? C46 C47 1.433(2) . ? C46 C51 1.4445(19) 2_566 ? C47 C48 1.361(2) . ? C47 H47 0.9500 . ? C48 C49 1.416(2) . ? C48 H48 0.9500 . ? C49 C50 1.359(2) 2_566 ? C49 H49 0.9500 . ? C50 C49 1.359(2) 2_566 ? C50 C51 1.428(2) . ? C50 H50 0.9500 . ? C51 C46 1.4445(19) 2_566 ? C52 C53 1.334(2) . ? C52 H52 0.9500 . ? C53 C54 1.4682(19) . ? C53 H53 0.9500 . ? C54 C55 1.392(2) . ? C54 C59 1.402(2) . ? C55 C56 1.395(2) . ? C55 H55 0.9500 . ? C56 C57 1.385(2) . ? C56 H56 0.9500 . ? C57 O3 1.3680(17) . ? C57 C58 1.392(2) . ? C58 C59 1.373(2) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 O3 1.4307(17) . ? C60 C61 1.5144(19) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.519(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.5252(19) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.518(2) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.528(2) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.512(2) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 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 C14 C1 C2 119.86(12) . . ? C14 C1 C15 121.75(13) . . ? C2 C1 C15 118.05(12) . . ? C1 C2 C3 121.08(12) . . ? C1 C2 C7 120.40(13) . . ? C3 C2 C7 118.51(13) . . ? C4 C3 C2 121.72(12) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.78(13) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.49(13) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 122.00(12) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 122.94(12) . . ? C8 C7 C2 119.74(12) . . ? C6 C7 C2 117.17(12) . . ? C9 C8 C7 119.71(12) . . ? C9 C8 C23 118.56(12) . . ? C7 C8 C23 121.65(12) . . ? C8 C9 C10 121.83(12) . . ? C8 C9 C14 120.40(12) . . ? C10 C9 C14 117.75(13) . . ? C11 C10 C9 121.99(13) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C10 C11 C12 120.23(14) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.03(14) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 121.83(13) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C1 C14 C13 122.06(12) . . ? C1 C14 C9 119.80(13) . . ? C13 C14 C9 118.13(13) . . ? C16 C15 C1 127.08(13) . . ? C16 C15 H15 116.5 . . ? C1 C15 H15 116.5 . . ? C15 C16 C17 126.75(14) . . ? C15 C16 H16 116.6 . . ? C17 C16 H16 116.6 . . ? C18 C17 C22 117.01(12) . . ? C18 C17 C16 119.89(13) . . ? C22 C17 C16 123.09(13) . . ? C17 C18 C19 122.23(14) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C20 C19 C18 119.27(13) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? O1 C20 C19 125.30(13) . . ? O1 C20 C21 115.22(13) . . ? C19 C20 C21 119.49(13) . . ? C22 C21 C20 120.47(14) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C17 121.42(13) . . ? C21 C22 H22 119.3 . . ? C17 C22 H22 119.3 . . ? C24 C23 C8 127.11(13) . . ? C24 C23 H23 116.4 . . ? C8 C23 H23 116.4 . . ? C23 C24 C25 125.16(14) . . ? C23 C24 H24 117.4 . . ? C25 C24 H24 117.4 . . ? C26 C25 C30 117.25(12) . . ? C26 C25 C24 120.06(13) . . ? C30 C25 C24 122.69(13) . . ? C27 C26 C25 122.19(13) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C28 C27 C26 119.14(13) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? O2 C28 C27 125.48(13) . . ? O2 C28 C29 114.67(13) . . ? C27 C28 C29 119.85(12) . . ? C30 C29 C28 120.22(13) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C25 121.33(13) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? O1 C31 C32 107.35(12) . . ? O1 C31 H31A 110.2 . . ? C32 C31 H31A 110.2 . . ? O1 C31 H31B 110.2 . . ? C32 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? C31 C32 C33 112.82(13) . . ? C31 C32 H32A 109.0 . . ? C33 C32 H32A 109.0 . . ? C31 C32 H32B 109.0 . . ? C33 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 113.10(14) . . ? C34 C33 H33A 109.0 . . ? C32 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? C32 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 C35 114.43(14) . . ? C33 C34 H34A 108.7 . . ? C35 C34 H34A 108.7 . . ? C33 C34 H34B 108.7 . . ? C35 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C36 C35 C34 113.65(14) . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35B 108.8 . . ? C34 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C35 113.47(14) . . ? C37 C36 H36A 108.9 . . ? C35 C36 H36A 108.9 . . ? C37 C36 H36B 108.9 . . ? C35 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O2 C38 C39 105.17(13) . . ? O2 C38 H38A 110.7 . . ? C39 C38 H38A 110.7 . . ? O2 C38 H38B 110.7 . . ? C39 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? C38 C39 C40 114.46(14) . . ? C38 C39 H39A 108.6 . . ? C40 C39 H39A 108.6 . . ? C38 C39 H39B 108.6 . . ? C40 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? C39 C40 C41 110.75(13) . . ? C39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C42 C41 C40 115.80(14) . . ? C42 C41 H41A 108.3 . . ? C40 C41 H41A 108.3 . . ? C42 C41 H41B 108.3 . . ? C40 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 112.04(14) . . ? C41 C42 H42A 109.2 . . ? C43 C42 H42A 109.2 . . ? C41 C42 H42B 109.2 . . ? C43 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C44 C43 C42 114.18(16) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? 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 C51 119.84(13) . . ? C46 C45 C52 122.12(13) . . ? C51 C45 C52 117.91(13) . . ? C45 C46 C47 122.68(13) . . ? C45 C46 C51 119.91(13) . 2_566 ? C47 C46 C51 117.34(13) . 2_566 ? C48 C47 C46 122.05(13) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C47 C48 C49 120.31(14) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 119.94(14) 2_566 . ? C50 C49 H49 120.0 2_566 . ? C48 C49 H49 120.0 . . ? C49 C50 C51 122.00(14) 2_566 . ? C49 C50 H50 119.0 2_566 . ? C51 C50 H50 119.0 . . ? C45 C51 C50 121.33(13) . . ? C45 C51 C46 120.24(14) . 2_566 ? C50 C51 C46 118.35(13) . 2_566 ? C53 C52 C45 127.38(13) . . ? C53 C52 H52 116.3 . . ? C45 C52 H52 116.3 . . ? C52 C53 C54 126.31(14) . . ? C52 C53 H53 116.8 . . ? C54 C53 H53 116.8 . . ? C55 C54 C59 117.02(13) . . ? C55 C54 C53 119.84(13) . . ? C59 C54 C53 123.13(13) . . ? C54 C55 C56 122.06(14) . . ? C54 C55 H55 119.0 . . ? C56 C55 H55 119.0 . . ? C57 C56 C55 119.47(13) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? O3 C57 C56 125.49(13) . . ? O3 C57 C58 115.20(13) . . ? C56 C57 C58 119.30(13) . . ? C59 C58 C57 120.62(14) . . ? C59 C58 H58 119.7 . . ? C57 C58 H58 119.7 . . ? C58 C59 C54 121.51(13) . . ? C58 C59 H59 119.2 . . ? C54 C59 H59 119.2 . . ? O3 C60 C61 106.60(11) . . ? O3 C60 H60A 110.4 . . ? C61 C60 H60A 110.4 . . ? O3 C60 H60B 110.4 . . ? C61 C60 H60B 110.4 . . ? H60A C60 H60B 108.6 . . ? C60 C61 C62 113.79(12) . . ? C60 C61 H61A 108.8 . . ? C62 C61 H61A 108.8 . . ? C60 C61 H61B 108.8 . . ? C62 C61 H61B 108.8 . . ? H61A C61 H61B 107.7 . . ? C61 C62 C63 111.24(11) . . ? C61 C62 H62A 109.4 . . ? C63 C62 H62A 109.4 . . ? C61 C62 H62B 109.4 . . ? C63 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C64 C63 C62 115.88(12) . . ? C64 C63 H63A 108.3 . . ? C62 C63 H63A 108.3 . . ? C64 C63 H63B 108.3 . . ? C62 C63 H63B 108.3 . . ? H63A C63 H63B 107.4 . . ? C63 C64 C65 111.84(12) . . ? C63 C64 H64A 109.2 . . ? C65 C64 H64A 109.2 . . ? C63 C64 H64B 109.2 . . ? C65 C64 H64B 109.2 . . ? H64A C64 H64B 107.9 . . ? C66 C65 C64 114.18(14) . . ? C66 C65 H65A 108.7 . . ? C64 C65 H65A 108.7 . . ? C66 C65 H65B 108.7 . . ? C64 C65 H65B 108.7 . . ? H65A C65 H65B 107.6 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C20 O1 C31 117.87(12) . . ? C28 O2 C38 119.13(11) . . ? C57 O3 C60 118.40(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 C1 C2 C3 179.77(13) . . . . ? C15 C1 C2 C3 -6.8(2) . . . . ? C14 C1 C2 C7 -0.4(2) . . . . ? C15 C1 C2 C7 173.06(13) . . . . ? C1 C2 C3 C4 175.02(14) . . . . ? C7 C2 C3 C4 -4.8(2) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C3 C4 C5 C6 2.9(2) . . . . ? C4 C5 C6 C7 -0.8(2) . . . . ? C5 C6 C7 C8 -179.63(14) . . . . ? C5 C6 C7 C2 -3.9(2) . . . . ? C1 C2 C7 C8 2.6(2) . . . . ? C3 C2 C7 C8 -177.59(13) . . . . ? C1 C2 C7 C6 -173.26(13) . . . . ? C3 C2 C7 C6 6.57(19) . . . . ? C6 C7 C8 C9 173.13(13) . . . . ? C2 C7 C8 C9 -2.5(2) . . . . ? C6 C7 C8 C23 -3.8(2) . . . . ? C2 C7 C8 C23 -179.38(12) . . . . ? C7 C8 C9 C10 -178.12(13) . . . . ? C23 C8 C9 C10 -1.1(2) . . . . ? C7 C8 C9 C14 0.2(2) . . . . ? C23 C8 C9 C14 177.24(12) . . . . ? C8 C9 C10 C11 176.17(14) . . . . ? C14 C9 C10 C11 -2.2(2) . . . . ? C9 C10 C11 C12 0.9(2) . . . . ? C10 C11 C12 C13 0.9(3) . . . . ? C11 C12 C13 C14 -1.3(2) . . . . ? C2 C1 C14 C13 176.72(13) . . . . ? C15 C1 C14 C13 3.5(2) . . . . ? C2 C1 C14 C9 -1.8(2) . . . . ? C15 C1 C14 C9 -175.06(13) . . . . ? C12 C13 C14 C1 -178.60(15) . . . . ? C12 C13 C14 C9 0.0(2) . . . . ? C8 C9 C14 C1 2.0(2) . . . . ? C10 C9 C14 C1 -179.64(13) . . . . ? C8 C9 C14 C13 -176.66(13) . . . . ? C10 C9 C14 C13 1.8(2) . . . . ? C14 C1 C15 C16 -70.7(2) . . . . ? C2 C1 C15 C16 115.92(18) . . . . ? C1 C15 C16 C17 178.93(15) . . . . ? C15 C16 C17 C18 -177.97(16) . . . . ? C15 C16 C17 C22 0.8(3) . . . . ? C22 C17 C18 C19 -2.5(2) . . . . ? C16 C17 C18 C19 176.33(15) . . . . ? C17 C18 C19 C20 0.3(3) . . . . ? C18 C19 C20 O1 -176.80(15) . . . . ? C18 C19 C20 C21 2.8(2) . . . . ? O1 C20 C21 C22 176.03(16) . . . . ? C19 C20 C21 C22 -3.6(3) . . . . ? C20 C21 C22 C17 1.3(3) . . . . ? C18 C17 C22 C21 1.7(3) . . . . ? C16 C17 C22 C21 -177.10(16) . . . . ? C9 C8 C23 C24 133.27(15) . . . . ? C7 C8 C23 C24 -49.8(2) . . . . ? C8 C23 C24 C25 178.25(13) . . . . ? C23 C24 C25 C26 -157.68(14) . . . . ? C23 C24 C25 C30 21.5(2) . . . . ? C30 C25 C26 C27 -1.9(2) . . . . ? C24 C25 C26 C27 177.34(13) . . . . ? C25 C26 C27 C28 0.6(2) . . . . ? C26 C27 C28 O2 -179.42(13) . . . . ? C26 C27 C28 C29 0.8(2) . . . . ? O2 C28 C29 C30 179.40(12) . . . . ? C27 C28 C29 C30 -0.8(2) . . . . ? C28 C29 C30 C25 -0.6(2) . . . . ? C26 C25 C30 C29 1.9(2) . . . . ? C24 C25 C30 C29 -177.33(13) . . . . ? O1 C31 C32 C33 177.49(14) . . . . ? C31 C32 C33 C34 -177.67(14) . . . . ? C32 C33 C34 C35 174.65(15) . . . . ? C33 C34 C35 C36 -175.59(15) . . . . ? C34 C35 C36 C37 179.54(16) . . . . ? O2 C38 C39 C40 -176.59(13) . . . . ? C38 C39 C40 C41 -174.98(14) . . . . ? C39 C40 C41 C42 -176.13(14) . . . . ? C40 C41 C42 C43 -175.53(15) . . . . ? C41 C42 C43 C44 177.69(16) . . . . ? C51 C45 C46 C47 176.48(14) . . . . ? C52 C45 C46 C47 0.7(2) . . . . ? C51 C45 C46 C51 -0.4(2) . . . 2_566 ? C52 C45 C46 C51 -176.16(13) . . . 2_566 ? C45 C46 C47 C48 -176.66(15) . . . . ? C51 C46 C47 C48 0.3(2) 2_566 . . . ? C46 C47 C48 C49 -1.1(3) . . . . ? C47 C48 C49 C50 1.5(3) . . . 2_566 ? C46 C45 C51 C50 177.07(14) . . . . ? C52 C45 C51 C50 -7.0(2) . . . . ? C46 C45 C51 C46 0.4(2) . . . 2_566 ? C52 C45 C51 C46 176.34(13) . . . 2_566 ? C49 C50 C51 C45 -177.01(15) 2_566 . . . ? C49 C50 C51 C46 -0.3(2) 2_566 . . 2_566 ? C46 C45 C52 C53 -56.9(2) . . . . ? C51 C45 C52 C53 127.20(18) . . . . ? C45 C52 C53 C54 177.80(15) . . . . ? C52 C53 C54 C55 -179.87(16) . . . . ? C52 C53 C54 C59 -0.9(3) . . . . ? C59 C54 C55 C56 -1.1(2) . . . . ? C53 C54 C55 C56 177.90(15) . . . . ? C54 C55 C56 C57 0.9(3) . . . . ? C55 C56 C57 O3 178.88(15) . . . . ? C55 C56 C57 C58 -0.1(2) . . . . ? O3 C57 C58 C59 -179.62(14) . . . . ? C56 C57 C58 C59 -0.6(2) . . . . ? C57 C58 C59 C54 0.4(3) . . . . ? C55 C54 C59 C58 0.5(2) . . . . ? C53 C54 C59 C58 -178.53(15) . . . . ? O3 C60 C61 C62 -165.00(13) . . . . ? C60 C61 C62 C63 177.50(13) . . . . ? C61 C62 C63 C64 177.23(14) . . . . ? C62 C63 C64 C65 179.70(14) . . . . ? C63 C64 C65 C66 170.59(17) . . . . ? C19 C20 O1 C31 3.5(2) . . . . ? C21 C20 O1 C31 -176.18(15) . . . . ? C32 C31 O1 C20 174.70(13) . . . . ? C27 C28 O2 C38 10.6(2) . . . . ? C29 C28 O2 C38 -169.58(12) . . . . ? C39 C38 O2 C28 169.70(12) . . . . ? C56 C57 O3 C60 20.0(2) . . . . ? C58 C57 O3 C60 -160.98(14) . . . . ? C61 C60 O3 C57 177.46(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 67.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.224 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.056 data_10141m _database_code_depnum_ccdc_archive 'CCDC 886642' #TrackingRef 'web_deposit_cif_file_1_ZhenguoChi_1339763597.DSA8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H54 O2' _chemical_formula_weight 638.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9037(16) _cell_length_b 16.377(3) _cell_length_c 19.649(4) _cell_angle_alpha 79.561(3) _cell_angle_beta 79.148(3) _cell_angle_gamma 78.442(3) _cell_volume 2726.1(9) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4800 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 26.84 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1038 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9702 _exptl_absorpt_correction_T_max 0.9945 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21320 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10506 _reflns_number_gt 5488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0518P)^2^+6.6133P] 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 10506 _refine_ls_number_parameters 652 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1603 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.1934 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.111 _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 C1 C 1.3887(5) 0.4112(3) -0.1528(2) 0.0326(9) Uani 1 1 d . . . C2 C 1.2299(5) 0.4293(3) -0.1508(2) 0.0354(10) Uani 1 1 d . . . H2 H 1.1838 0.4771 -0.1797 0.042 Uiso 1 1 calc R . . C3 C 1.1385(5) 0.3763(2) -0.1056(2) 0.0338(10) Uani 1 1 d . . . H3 H 1.0292 0.3888 -0.1043 0.041 Uiso 1 1 calc R . . C4 C 1.2009(5) 0.3059(2) -0.0623(2) 0.0308(9) Uani 1 1 d . . . C5 C 1.3609(5) 0.2910(3) -0.0641(2) 0.0329(9) Uani 1 1 d . . . H5 H 1.4072 0.2443 -0.0342 0.039 Uiso 1 1 calc R . . C6 C 1.4534(5) 0.3426(3) -0.1084(2) 0.0346(10) Uani 1 1 d . . . H6 H 1.5624 0.3312 -0.1086 0.042 Uiso 1 1 calc R . . C7 C 1.0992(5) 0.2494(3) -0.0189(2) 0.0321(9) Uani 1 1 d . . . H7 H 0.9931 0.2732 -0.0069 0.038 Uiso 1 1 calc R . . C8 C 1.1407(4) 0.1685(2) 0.0052(2) 0.0312(9) Uani 1 1 d . . . H8 H 1.2476 0.1451 -0.0052 0.037 Uiso 1 1 calc R . . C9 C 1.0379(4) 0.1112(2) 0.0465(2) 0.0281(9) Uani 1 1 d . . . C10 C 0.9008(4) 0.1030(2) 0.0247(2) 0.0272(9) Uani 1 1 d . . . C11 C 0.8569(5) 0.1447(2) -0.0412(2) 0.0301(9) Uani 1 1 d . . . H11 H 0.9229 0.1792 -0.0718 0.036 Uiso 1 1 calc R . . C12 C 0.7238(5) 0.1361(3) -0.0608(2) 0.0358(10) Uani 1 1 d . . . H12 H 0.6983 0.1641 -0.1050 0.043 Uiso 1 1 calc R . . C13 C 0.6224(5) 0.0858(3) -0.0163(2) 0.0361(10) Uani 1 1 d . . . H13 H 0.5273 0.0819 -0.0297 0.043 Uiso 1 1 calc R . . C14 C 0.6614(5) 0.0432(3) 0.0454(2) 0.0350(10) Uani 1 1 d . . . H14 H 0.5924 0.0096 0.0749 0.042 Uiso 1 1 calc R . . C15 C 0.8024(4) 0.0473(2) 0.0672(2) 0.0290(9) Uani 1 1 d . . . C16 C 0.8465(4) -0.0021(2) 0.1293(2) 0.0312(9) Uani 1 1 d . . . C17 C 0.9853(4) 0.0036(2) 0.1504(2) 0.0293(9) Uani 1 1 d . . . C18 C 1.0384(5) -0.0470(3) 0.2111(2) 0.0392(10) Uani 1 1 d . . . H18 H 0.9775 -0.0862 0.2387 0.047 Uiso 1 1 calc R . . C19 C 1.1726(5) -0.0409(3) 0.2306(2) 0.0431(11) Uani 1 1 d . . . H19 H 1.2049 -0.0757 0.2713 0.052 Uiso 1 1 calc R . . C20 C 1.2653(5) 0.0169(3) 0.1910(2) 0.0419(11) Uani 1 1 d . . . H20 H 1.3591 0.0213 0.2053 0.050 Uiso 1 1 calc R . . C21 C 1.2208(5) 0.0662(3) 0.1324(2) 0.0380(10) Uani 1 1 d . . . H21 H 1.2842 0.1050 0.1063 0.046 Uiso 1 1 calc R . . C22 C 1.0814(4) 0.0611(2) 0.1090(2) 0.0292(9) Uani 1 1 d . . . C23 C 0.7520(5) -0.0669(3) 0.1673(2) 0.0460(12) Uani 1 1 d . . . H23 H 0.7482 -0.1104 0.1418 0.055 Uiso 1 1 calc R . . C24 C 0.6755(5) -0.0720(3) 0.2294(2) 0.0433(11) Uani 1 1 d . . . H24 H 0.6720 -0.0270 0.2543 0.052 Uiso 1 1 calc R . . C25 C 0.5913(6) -0.1410(3) 0.2666(2) 0.0434(11) Uani 1 1 d U . . C26 C 0.5927(8) -0.2127(4) 0.2411(4) 0.0892(17) Uani 1 1 d U . . H26 H 0.6485 -0.2200 0.1958 0.107 Uiso 1 1 calc R . . C27 C 0.5151(9) -0.2754(4) 0.2792(4) 0.0936(16) Uani 1 1 d U . . H27 H 0.5145 -0.3239 0.2590 0.112 Uiso 1 1 calc R . . C28 C 0.4392(8) -0.2683(4) 0.3456(3) 0.0739(13) Uani 1 1 d U . . C29 C 0.4290(5) -0.1964(3) 0.3701(2) 0.0445(11) Uani 1 1 d U . . H29 H 0.3698 -0.1885 0.4147 0.053 Uiso 1 1 calc R . . C30 C 0.5040(5) -0.1336(3) 0.3311(2) 0.0425(11) Uani 1 1 d U . . H30 H 0.4947 -0.0828 0.3496 0.051 Uiso 1 1 calc R . . C31 C 1.4374(5) 0.5209(3) -0.2500(2) 0.0397(10) Uani 1 1 d U . . H31A H 1.3654 0.5679 -0.2297 0.048 Uiso 1 1 calc R . . H31B H 1.3821 0.4971 -0.2790 0.048 Uiso 1 1 calc R . . C32 C 1.5795(5) 0.5516(3) -0.2939(2) 0.0392(10) Uani 1 1 d U . . H32A H 1.6514 0.5032 -0.3121 0.047 Uiso 1 1 calc R . . H32B H 1.6334 0.5742 -0.2637 0.047 Uiso 1 1 calc R . . C33 C 1.5433(5) 0.6195(3) -0.3555(2) 0.0409(11) Uani 1 1 d U . . H33A H 1.4650 0.6663 -0.3381 0.049 Uiso 1 1 calc R . . H33B H 1.4985 0.5957 -0.3884 0.049 Uiso 1 1 calc R . . C34 C 1.6884(5) 0.6536(3) -0.3941(2) 0.0408(11) Uani 1 1 d U . . H34A H 1.7259 0.6822 -0.3619 0.049 Uiso 1 1 calc R . . H34B H 1.7703 0.6053 -0.4058 0.049 Uiso 1 1 calc R . . C35 C 1.6671(5) 0.7148(3) -0.4610(2) 0.0375(10) Uani 1 1 d U . . H35A H 1.6367 0.6853 -0.4947 0.045 Uiso 1 1 calc R . . H35B H 1.5813 0.7615 -0.4501 0.045 Uiso 1 1 calc R . . C36 C 1.8116(5) 0.7512(3) -0.4953(2) 0.0390(10) Uani 1 1 d U . . H36A H 1.8432 0.7795 -0.4612 0.047 Uiso 1 1 calc R . . H36B H 1.8967 0.7043 -0.5069 0.047 Uiso 1 1 calc R . . C37 C 1.7916(5) 0.8136(3) -0.5612(2) 0.0433(11) Uani 1 1 d U . . H37A H 1.7012 0.8581 -0.5507 0.052 Uiso 1 1 calc R . . H37B H 1.7691 0.7842 -0.5970 0.052 Uiso 1 1 calc R . . C38 C 1.9333(6) 0.8545(3) -0.5913(3) 0.0603(14) Uani 1 1 d U . . H38A H 1.9586 0.8821 -0.5557 0.090 Uiso 1 1 calc R . . H38B H 1.9114 0.8965 -0.6321 0.090 Uiso 1 1 calc R . . H38C H 2.0214 0.8113 -0.6055 0.090 Uiso 1 1 calc R . . C39 C 0.3130(7) -0.3446(4) 0.4475(3) 0.0655(12) Uani 1 1 d U . . H39A H 0.2213 -0.2997 0.4543 0.079 Uiso 1 1 calc R . . H39B H 0.3910 -0.3358 0.4741 0.079 Uiso 1 1 calc R . . C40 C 0.2667(8) -0.4274(4) 0.4752(3) 0.0810(15) Uani 1 1 d U . . H40A H 0.1942 -0.4362 0.4457 0.097 Uiso 1 1 calc R . . H40B H 0.3606 -0.4710 0.4683 0.097 Uiso 1 1 calc R . . C41 C 0.1942(7) -0.4433(3) 0.5480(3) 0.0604(12) Uani 1 1 d U . . H41A H 0.0992 -0.4004 0.5544 0.073 Uiso 1 1 calc R . . H41B H 0.2657 -0.4330 0.5772 0.073 Uiso 1 1 calc R . . C42 C 0.1505(8) -0.5257(4) 0.5769(3) 0.0817(15) Uani 1 1 d U . . H42A H 0.0868 -0.5380 0.5451 0.098 Uiso 1 1 calc R . . H42B H 0.2473 -0.5678 0.5738 0.098 Uiso 1 1 calc R . . C43 C 0.0670(7) -0.5421(3) 0.6480(3) 0.0605(12) Uani 1 1 d U . . H43A H -0.0287 -0.4992 0.6514 0.073 Uiso 1 1 calc R . . H43B H 0.1318 -0.5309 0.6800 0.073 Uiso 1 1 calc R . . C44 C 0.0207(8) -0.6238(4) 0.6766(3) 0.0799(15) Uani 1 1 d U . . H44A H -0.0400 -0.6363 0.6436 0.096 Uiso 1 1 calc R . . H44B H 0.1169 -0.6664 0.6753 0.096 Uiso 1 1 calc R . . C45 C -0.0668(7) -0.6385(3) 0.7455(3) 0.0632(14) Uani 1 1 d U . . H45A H -0.1642 -0.5968 0.7462 0.076 Uiso 1 1 calc R . . H45B H -0.0074 -0.6241 0.7782 0.076 Uiso 1 1 calc R . . C46 C -0.1101(10) -0.7194(4) 0.7756(4) 0.112(3) Uani 1 1 d . . . H46A H -0.1775 -0.7337 0.7470 0.169 Uiso 1 1 calc R . . H46B H -0.1658 -0.7167 0.8234 0.169 Uiso 1 1 calc R . . H46C H -0.0165 -0.7626 0.7767 0.169 Uiso 1 1 calc R . . C47 C 0.0269(5) 0.3070(3) 0.2361(2) 0.0329(9) Uani 1 1 d . . . C48 C -0.0053(5) 0.2461(3) 0.2040(2) 0.0360(10) Uani 1 1 d . . . H48 H 0.0298 0.2450 0.1554 0.043 Uiso 1 1 calc R . . C49 C -0.0899(5) 0.1860(3) 0.2434(2) 0.0354(10) Uani 1 1 d . . . H49 H -0.1106 0.1436 0.2210 0.042 Uiso 1 1 calc R . . C50 C -0.1447(4) 0.1860(2) 0.3143(2) 0.0308(9) Uani 1 1 d . . . C51 C -0.1083(5) 0.2483(3) 0.3456(2) 0.0394(11) Uani 1 1 d . . . H51 H -0.1428 0.2497 0.3942 0.047 Uiso 1 1 calc R . . C52 C -0.0240(5) 0.3071(3) 0.3076(2) 0.0384(10) Uani 1 1 d . . . H52 H 0.0000 0.3484 0.3301 0.046 Uiso 1 1 calc R . . C53 C -0.2383(5) 0.1231(2) 0.3528(2) 0.0324(9) Uani 1 1 d . . . H53 H -0.2551 0.0828 0.3270 0.039 Uiso 1 1 calc R . . C54 C -0.3022(4) 0.1168(2) 0.4201(2) 0.0308(9) Uani 1 1 d . . . H54 H -0.2807 0.1554 0.4462 0.037 Uiso 1 1 calc R . . C55 C -0.4027(4) 0.0563(2) 0.4586(2) 0.0291(9) Uani 1 1 d . . . C56 C -0.5418(4) 0.0494(2) 0.4367(2) 0.0284(9) Uani 1 1 d . . . C57 C -0.5943(5) 0.1002(3) 0.3757(2) 0.0333(9) Uani 1 1 d . . . H57 H -0.5327 0.1391 0.3481 0.040 Uiso 1 1 calc R . . C58 C -0.7287(5) 0.0947(3) 0.3560(2) 0.0370(10) Uani 1 1 d . . . H58 H -0.7595 0.1288 0.3147 0.044 Uiso 1 1 calc R . . C59 C -0.8243(5) 0.0382(3) 0.3967(2) 0.0383(10) Uani 1 1 d . . . H59 H -0.9188 0.0343 0.3827 0.046 Uiso 1 1 calc R . . C60 C -0.2200(5) 0.0103(3) 0.5443(2) 0.0344(10) Uani 1 1 d . . . H60 H -0.1542 0.0473 0.5171 0.041 Uiso 1 1 calc R . . C61 C -0.3620(4) 0.0076(2) 0.5216(2) 0.0287(9) Uani 1 1 d . . . C62 C 0.1368(5) 0.3857(3) 0.1288(2) 0.0355(10) Uani 1 1 d . . . H62A H 0.0376 0.3973 0.1101 0.043 Uiso 1 1 calc R . . H62B H 0.2037 0.3365 0.1097 0.043 Uiso 1 1 calc R . . C63 C 0.2164(5) 0.4617(2) 0.1090(2) 0.0318(9) Uani 1 1 d . . . H63A H 0.3217 0.4461 0.1219 0.038 Uiso 1 1 calc R . . H63B H 0.1576 0.5065 0.1361 0.038 Uiso 1 1 calc R . . C64 C 0.2297(5) 0.4963(2) 0.0310(2) 0.0311(9) Uani 1 1 d . . . H64A H 0.2915 0.4522 0.0038 0.037 Uiso 1 1 calc R . . H64B H 0.1247 0.5105 0.0176 0.037 Uiso 1 1 calc R . . C65 C 0.3058(5) 0.5742(2) 0.0127(2) 0.0298(9) Uani 1 1 d . . . H65A H 0.4091 0.5599 0.0278 0.036 Uiso 1 1 calc R . . H65B H 0.2423 0.6182 0.0396 0.036 Uiso 1 1 calc R . . C66 C 0.3260(5) 0.6105(3) -0.0649(2) 0.0336(10) Uani 1 1 d . . . H66A H 0.3912 0.5671 -0.0918 0.040 Uiso 1 1 calc R . . H66B H 0.2231 0.6242 -0.0803 0.040 Uiso 1 1 calc R . . C67 C 0.3998(5) 0.6892(2) -0.0818(2) 0.0351(10) Uani 1 1 d . . . H67A H 0.4966 0.6777 -0.0612 0.042 Uiso 1 1 calc R . . H67B H 0.3283 0.7350 -0.0597 0.042 Uiso 1 1 calc R . . C68 C 0.4378(6) 0.7191(3) -0.1603(2) 0.0444(11) Uani 1 1 d . . . H68A H 0.5135 0.6745 -0.1822 0.053 Uiso 1 1 calc R . . H68B H 0.3421 0.7281 -0.1814 0.053 Uiso 1 1 calc R . . C69 C 0.5047(6) 0.8002(3) -0.1767(3) 0.0540(13) Uani 1 1 d . . . H69A H 0.4308 0.8446 -0.1549 0.081 Uiso 1 1 calc R . . H69B H 0.5237 0.8174 -0.2276 0.081 Uiso 1 1 calc R . . H69C H 0.6026 0.7909 -0.1583 0.081 Uiso 1 1 calc R . . O1 O 1.4917(3) 0.45706(18) -0.19544(15) 0.0387(7) Uani 1 1 d . . . O2 O 0.3742(6) -0.3384(3) 0.3776(2) 0.0943(12) Uani 1 1 d U . . O3 O 0.1089(4) 0.36967(18) 0.20391(14) 0.0405(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(2) 0.036(2) 0.031(2) -0.0069(18) -0.0007(18) -0.0150(19) C2 0.036(2) 0.033(2) 0.035(2) 0.0014(18) -0.0038(19) -0.0073(19) C3 0.027(2) 0.033(2) 0.040(2) -0.0014(19) -0.0046(18) -0.0070(18) C4 0.030(2) 0.032(2) 0.031(2) -0.0040(18) -0.0015(17) -0.0101(18) C5 0.031(2) 0.033(2) 0.036(2) -0.0018(18) -0.0047(18) -0.0090(18) C6 0.029(2) 0.039(2) 0.039(2) -0.0045(19) -0.0043(18) -0.0130(19) C7 0.026(2) 0.036(2) 0.034(2) -0.0038(18) -0.0022(17) -0.0087(18) C8 0.021(2) 0.035(2) 0.037(2) -0.0024(19) -0.0017(17) -0.0084(17) C9 0.026(2) 0.026(2) 0.031(2) -0.0046(17) 0.0006(17) -0.0050(16) C10 0.025(2) 0.027(2) 0.029(2) -0.0054(17) -0.0014(16) -0.0051(16) C11 0.031(2) 0.025(2) 0.032(2) 0.0001(17) -0.0028(17) -0.0052(17) C12 0.039(2) 0.034(2) 0.035(2) 0.0006(19) -0.0118(19) -0.0065(19) C13 0.025(2) 0.036(2) 0.050(3) -0.005(2) -0.0131(19) -0.0054(18) C14 0.028(2) 0.032(2) 0.045(3) -0.0047(19) -0.0010(19) -0.0102(18) C15 0.025(2) 0.028(2) 0.033(2) -0.0055(17) 0.0025(17) -0.0069(16) C16 0.028(2) 0.031(2) 0.034(2) -0.0033(18) 0.0018(17) -0.0090(17) C17 0.027(2) 0.029(2) 0.029(2) -0.0036(17) -0.0003(17) -0.0059(17) C18 0.043(3) 0.040(2) 0.033(2) -0.001(2) -0.004(2) -0.010(2) C19 0.046(3) 0.045(3) 0.037(3) 0.004(2) -0.014(2) -0.006(2) C20 0.038(3) 0.049(3) 0.043(3) -0.004(2) -0.016(2) -0.010(2) C21 0.033(2) 0.039(2) 0.043(3) -0.003(2) -0.0057(19) -0.0113(19) C22 0.026(2) 0.027(2) 0.034(2) -0.0058(17) -0.0037(17) -0.0038(16) C23 0.045(3) 0.049(3) 0.044(3) 0.001(2) -0.005(2) -0.015(2) C24 0.044(3) 0.043(3) 0.044(3) -0.007(2) -0.007(2) -0.007(2) C25 0.054(3) 0.040(2) 0.038(2) 0.0063(19) -0.010(2) -0.021(2) C26 0.115(3) 0.083(3) 0.072(3) -0.026(2) 0.021(2) -0.043(2) C27 0.124(3) 0.078(2) 0.081(2) -0.026(2) 0.018(2) -0.043(2) C28 0.101(3) 0.064(2) 0.063(2) -0.010(2) 0.007(2) -0.046(2) C29 0.041(2) 0.057(3) 0.036(2) -0.007(2) 0.0015(19) -0.016(2) C30 0.042(2) 0.034(2) 0.053(3) -0.012(2) -0.004(2) -0.0083(19) C31 0.043(2) 0.040(2) 0.035(2) -0.0006(19) -0.0014(19) -0.0146(19) C32 0.037(2) 0.042(2) 0.037(2) 0.0000(19) -0.0026(18) -0.0117(19) C33 0.038(2) 0.042(2) 0.039(2) 0.0025(19) -0.0029(19) -0.0101(19) C34 0.037(2) 0.042(2) 0.041(2) 0.0041(19) -0.0055(19) -0.0112(19) C35 0.038(2) 0.036(2) 0.035(2) 0.0006(18) -0.0023(18) -0.0088(18) C36 0.036(2) 0.042(2) 0.037(2) -0.0008(19) -0.0031(18) -0.0092(19) C37 0.046(2) 0.040(2) 0.038(2) -0.0007(19) 0.0008(19) -0.006(2) C38 0.066(3) 0.064(3) 0.047(3) 0.002(2) 0.001(2) -0.022(3) C39 0.084(2) 0.067(2) 0.052(2) -0.0076(19) -0.003(2) -0.035(2) C40 0.096(3) 0.071(2) 0.071(2) -0.001(2) 0.007(2) -0.030(2) C41 0.071(2) 0.057(2) 0.055(2) -0.0043(18) -0.0047(19) -0.0241(19) C42 0.098(3) 0.067(2) 0.072(2) -0.002(2) 0.011(2) -0.026(2) C43 0.077(3) 0.053(2) 0.053(2) -0.0036(19) -0.005(2) -0.024(2) C44 0.101(3) 0.062(2) 0.069(3) -0.002(2) 0.011(2) -0.025(2) C45 0.073(3) 0.058(3) 0.056(3) 0.003(2) -0.007(2) -0.016(2) C46 0.156(8) 0.074(5) 0.087(5) 0.016(4) 0.032(5) -0.044(5) C47 0.028(2) 0.033(2) 0.034(2) 0.0018(18) 0.0013(17) -0.0102(18) C48 0.041(2) 0.038(2) 0.028(2) -0.0043(19) 0.0033(18) -0.013(2) C49 0.037(2) 0.032(2) 0.035(2) -0.0067(19) 0.0048(19) -0.0112(19) C50 0.027(2) 0.029(2) 0.033(2) -0.0001(18) 0.0006(17) -0.0060(17) C51 0.049(3) 0.042(3) 0.027(2) -0.0020(19) 0.0054(19) -0.021(2) C52 0.049(3) 0.037(2) 0.031(2) -0.0049(19) 0.001(2) -0.020(2) C53 0.035(2) 0.026(2) 0.034(2) -0.0025(18) 0.0007(18) -0.0087(17) C54 0.031(2) 0.027(2) 0.033(2) -0.0007(17) -0.0021(18) -0.0073(17) C55 0.029(2) 0.026(2) 0.029(2) -0.0009(17) 0.0040(17) -0.0075(17) C56 0.027(2) 0.027(2) 0.028(2) -0.0027(17) 0.0033(17) -0.0062(17) C57 0.034(2) 0.033(2) 0.030(2) -0.0003(18) 0.0015(18) -0.0093(18) C58 0.038(2) 0.041(2) 0.029(2) 0.0024(19) -0.0061(19) -0.008(2) C59 0.032(2) 0.042(3) 0.040(3) -0.003(2) -0.0044(19) -0.010(2) C60 0.031(2) 0.034(2) 0.036(2) -0.0009(19) 0.0021(18) -0.0115(18) C61 0.025(2) 0.028(2) 0.031(2) -0.0042(17) 0.0029(17) -0.0052(16) C62 0.039(2) 0.036(2) 0.030(2) 0.0035(18) 0.0012(18) -0.0154(19) C63 0.029(2) 0.030(2) 0.034(2) 0.0023(18) -0.0049(17) -0.0086(17) C64 0.030(2) 0.032(2) 0.031(2) 0.0006(17) -0.0029(17) -0.0109(18) C65 0.030(2) 0.030(2) 0.029(2) 0.0011(17) -0.0034(17) -0.0092(17) C66 0.029(2) 0.038(2) 0.034(2) 0.0048(19) -0.0063(18) -0.0130(18) C67 0.037(2) 0.031(2) 0.035(2) 0.0026(18) -0.0005(19) -0.0108(19) C68 0.047(3) 0.045(3) 0.041(3) 0.009(2) -0.009(2) -0.019(2) C69 0.071(4) 0.043(3) 0.044(3) 0.011(2) 0.000(3) -0.026(3) O1 0.0341(16) 0.0416(17) 0.0387(17) 0.0046(14) -0.0019(13) -0.0159(14) O2 0.137(3) 0.081(2) 0.069(2) -0.0106(18) 0.014(2) -0.060(2) O3 0.0510(19) 0.0413(17) 0.0303(16) 0.0043(13) 0.0016(14) -0.0270(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.366(5) . ? C1 C2 1.380(6) . ? C1 C6 1.390(6) . ? C2 C3 1.391(6) . ? C2 H2 0.9500 . ? C3 C4 1.389(5) . ? C3 H3 0.9500 . ? C4 C5 1.391(5) . ? C4 C7 1.470(5) . ? C5 C6 1.375(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.327(5) . ? C7 H7 0.9500 . ? C8 C9 1.471(5) . ? C8 H8 0.9500 . ? C9 C10 1.406(5) . ? C9 C22 1.420(5) . ? C10 C11 1.434(5) . ? C10 C15 1.437(5) . ? C11 C12 1.353(6) . ? C11 H11 0.9500 . ? C12 C13 1.413(6) . ? C12 H12 0.9500 . ? C13 C14 1.354(6) . ? C13 H13 0.9500 . ? C14 C15 1.419(6) . ? C14 H14 0.9500 . ? C15 C16 1.412(6) . ? C16 C17 1.400(5) . ? C16 C23 1.492(6) . ? C17 C18 1.426(6) . ? C17 C22 1.436(5) . ? C18 C19 1.348(6) . ? C18 H18 0.9500 . ? C19 C20 1.409(6) . ? C19 H19 0.9500 . ? C20 C21 1.357(6) . ? C20 H20 0.9500 . ? C21 C22 1.425(6) . ? C21 H21 0.9500 . ? C23 C24 1.277(6) . ? C23 H23 0.9500 . ? C24 C25 1.486(6) . ? C24 H24 0.9500 . ? C25 C26 1.355(7) . ? C25 C30 1.368(6) . ? C26 C27 1.379(8) . ? C26 H26 0.9500 . ? C27 C28 1.365(8) . ? C27 H27 0.9500 . ? C28 C29 1.332(7) . ? C28 O2 1.385(6) . ? C29 C30 1.374(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O1 1.436(5) . ? C31 C32 1.512(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.522(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.524(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.520(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.516(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.513(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.518(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O2 1.371(6) . ? C39 C40 1.476(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.455(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.464(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.459(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.462(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.434(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.445(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 O3 1.371(5) . ? C47 C48 1.373(6) . ? C47 C52 1.392(6) . ? C48 C49 1.392(5) . ? C48 H48 0.9500 . ? C49 C50 1.387(6) . ? C49 H49 0.9500 . ? C50 C51 1.400(6) . ? C50 C53 1.467(5) . ? C51 C52 1.366(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.332(5) . ? C53 H53 0.9500 . ? C54 C55 1.478(5) . ? C54 H54 0.9500 . ? C55 C61 1.413(5) . ? C55 C56 1.416(5) . ? C56 C57 1.430(5) . ? C56 C61 1.434(5) 2_456 ? C57 C58 1.349(6) . ? C57 H57 0.9500 . ? C58 C59 1.418(6) . ? C58 H58 0.9500 . ? C59 C60 1.359(6) 2_456 ? C59 H59 0.9500 . ? C60 C59 1.359(6) 2_456 ? C60 C61 1.429(6) . ? C60 H60 0.9500 . ? C61 C56 1.434(5) 2_456 ? C62 O3 1.434(5) . ? C62 C63 1.509(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.524(5) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.518(5) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.524(5) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.519(5) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.526(6) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.520(6) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 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 O1 C1 C2 124.8(4) . . ? O1 C1 C6 115.5(4) . . ? C2 C1 C6 119.7(4) . . ? C1 C2 C3 118.8(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 122.6(4) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 117.1(4) . . ? C3 C4 C7 120.0(4) . . ? C5 C4 C7 122.9(4) . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C4 126.6(4) . . ? C8 C7 H7 116.7 . . ? C4 C7 H7 116.7 . . ? C7 C8 C9 126.5(4) . . ? C7 C8 H8 116.7 . . ? C9 C8 H8 116.7 . . ? C10 C9 C22 119.4(3) . . ? C10 C9 C8 121.8(4) . . ? C22 C9 C8 118.8(4) . . ? C9 C10 C11 122.8(4) . . ? C9 C10 C15 119.9(4) . . ? C11 C10 C15 117.2(4) . . ? C12 C11 C10 121.6(4) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 121.8(4) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 121.1(4) . . ? C16 C15 C10 120.2(4) . . ? C14 C15 C10 118.6(4) . . ? C17 C16 C15 120.2(4) . . ? C17 C16 C23 120.8(4) . . ? C15 C16 C23 118.7(4) . . ? C16 C17 C18 122.6(4) . . ? C16 C17 C22 119.6(4) . . ? C18 C17 C22 117.8(4) . . ? C19 C18 C17 121.9(4) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 120.1(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 121.6(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C9 C22 C21 121.3(4) . . ? C9 C22 C17 120.6(4) . . ? C21 C22 C17 118.2(4) . . ? C24 C23 C16 128.9(5) . . ? C24 C23 H23 115.6 . . ? C16 C23 H23 115.6 . . ? C23 C24 C25 126.8(5) . . ? C23 C24 H24 116.6 . . ? C25 C24 H24 116.6 . . ? C26 C25 C30 115.9(5) . . ? C26 C25 C24 124.6(5) . . ? C30 C25 C24 119.5(4) . . ? C25 C26 C27 121.8(6) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 120.4(6) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 118.6(5) . . ? C29 C28 O2 128.2(5) . . ? C27 C28 O2 113.1(5) . . ? C28 C29 C30 120.1(5) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 122.8(4) . . ? C25 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? O1 C31 C32 106.5(3) . . ? O1 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? O1 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 113.7(4) . . ? C31 C32 H32A 108.8 . . ? C33 C32 H32A 108.8 . . ? C31 C32 H32B 108.8 . . ? C33 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C32 C33 C34 111.5(4) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 115.2(4) . . ? C35 C34 H34A 108.5 . . ? C33 C34 H34A 108.5 . . ? C35 C34 H34B 108.5 . . ? C33 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C36 C35 C34 113.4(4) . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C34 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C35 114.2(4) . . ? C37 C36 H36A 108.7 . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36B 108.7 . . ? C35 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C36 C37 C38 113.2(4) . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 C40 111.9(5) . . ? O2 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? O2 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C41 C40 C39 119.0(5) . . ? C41 C40 H40A 107.6 . . ? C39 C40 H40A 107.6 . . ? C41 C40 H40B 107.6 . . ? C39 C40 H40B 107.6 . . ? H40A C40 H40B 107.0 . . ? C40 C41 C42 119.9(5) . . ? C40 C41 H41A 107.3 . . ? C42 C41 H41A 107.3 . . ? C40 C41 H41B 107.3 . . ? C42 C41 H41B 107.3 . . ? H41A C41 H41B 106.9 . . ? C43 C42 C41 121.5(5) . . ? C43 C42 H42A 106.9 . . ? C41 C42 H42A 106.9 . . ? C43 C42 H42B 106.9 . . ? C41 C42 H42B 106.9 . . ? H42A C42 H42B 106.7 . . ? C42 C43 C44 121.6(5) . . ? C42 C43 H43A 106.9 . . ? C44 C43 H43A 106.9 . . ? C42 C43 H43B 106.9 . . ? C44 C43 H43B 106.9 . . ? H43A C43 H43B 106.7 . . ? C45 C44 C43 121.4(5) . . ? C45 C44 H44A 107.0 . . ? C43 C44 H44A 107.0 . . ? C45 C44 H44B 107.0 . . ? C43 C44 H44B 107.0 . . ? H44A C44 H44B 106.7 . . ? C44 C45 C46 122.4(6) . . ? C44 C45 H45A 106.7 . . ? C46 C45 H45A 106.7 . . ? C44 C45 H45B 106.7 . . ? C46 C45 H45B 106.7 . . ? H45A C45 H45B 106.6 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O3 C47 C48 125.5(4) . . ? O3 C47 C52 114.9(4) . . ? C48 C47 C52 119.6(4) . . ? C47 C48 C49 119.4(4) . . ? C47 C48 H48 120.3 . . ? C49 C48 H48 120.3 . . ? C50 C49 C48 122.1(4) . . ? C50 C49 H49 119.0 . . ? C48 C49 H49 119.0 . . ? C49 C50 C51 117.1(4) . . ? C49 C50 C53 119.8(4) . . ? C51 C50 C53 123.1(4) . . ? C52 C51 C50 121.3(4) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C47 120.6(4) . . ? C51 C52 H52 119.7 . . ? C47 C52 H52 119.7 . . ? C54 C53 C50 126.5(4) . . ? C54 C53 H53 116.7 . . ? C50 C53 H53 116.7 . . ? C53 C54 C55 127.1(4) . . ? C53 C54 H54 116.5 . . ? C55 C54 H54 116.5 . . ? C61 C55 C56 119.4(3) . . ? C61 C55 C54 118.1(4) . . ? C56 C55 C54 122.4(4) . . ? C55 C56 C57 122.3(3) . . ? C55 C56 C61 119.5(4) . 2_456 ? C57 C56 C61 118.1(4) . 2_456 ? C58 C57 C56 122.0(4) . . ? C58 C57 H57 119.0 . . ? C56 C57 H57 119.0 . . ? C57 C58 C59 120.3(4) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C60 C59 C58 119.7(4) 2_456 . ? C60 C59 H59 120.2 2_456 . ? C58 C59 H59 120.2 . . ? C59 C60 C61 122.3(4) 2_456 . ? C59 C60 H60 118.8 2_456 . ? C61 C60 H60 118.8 . . ? C55 C61 C60 121.3(4) . . ? C55 C61 C56 121.1(4) . 2_456 ? C60 C61 C56 117.6(4) . 2_456 ? O3 C62 C63 106.4(3) . . ? O3 C62 H62A 110.4 . . ? C63 C62 H62A 110.4 . . ? O3 C62 H62B 110.4 . . ? C63 C62 H62B 110.4 . . ? H62A C62 H62B 108.6 . . ? C62 C63 C64 113.0(3) . . ? C62 C63 H63A 109.0 . . ? C64 C63 H63A 109.0 . . ? C62 C63 H63B 109.0 . . ? C64 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? C65 C64 C63 112.0(3) . . ? C65 C64 H64A 109.2 . . ? C63 C64 H64A 109.2 . . ? C65 C64 H64B 109.2 . . ? C63 C64 H64B 109.2 . . ? H64A C64 H64B 107.9 . . ? C64 C65 C66 114.5(3) . . ? C64 C65 H65A 108.6 . . ? C66 C65 H65A 108.6 . . ? C64 C65 H65B 108.6 . . ? C66 C65 H65B 108.6 . . ? H65A C65 H65B 107.6 . . ? C67 C66 C65 113.6(3) . . ? C67 C66 H66A 108.8 . . ? C65 C66 H66A 108.8 . . ? C67 C66 H66B 108.8 . . ? C65 C66 H66B 108.8 . . ? H66A C66 H66B 107.7 . . ? C66 C67 C68 113.3(4) . . ? C66 C67 H67A 108.9 . . ? C68 C67 H67A 108.9 . . ? C66 C67 H67B 108.9 . . ? C68 C67 H67B 108.9 . . ? H67A C67 H67B 107.7 . . ? C69 C68 C67 112.9(4) . . ? C69 C68 H68A 109.0 . . ? C67 C68 H68A 109.0 . . ? C69 C68 H68B 109.0 . . ? C67 C68 H68B 109.0 . . ? H68A C68 H68B 107.8 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C1 O1 C31 118.8(3) . . ? C39 O2 C28 119.0(5) . . ? C47 O3 C62 118.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 178.9(4) . . . . ? C6 C1 C2 C3 -2.1(6) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 1.8(6) . . . . ? C2 C3 C4 C7 -176.2(4) . . . . ? C3 C4 C5 C6 -1.8(6) . . . . ? C7 C4 C5 C6 176.1(4) . . . . ? C4 C5 C6 C1 -0.1(6) . . . . ? O1 C1 C6 C5 -178.8(4) . . . . ? C2 C1 C6 C5 2.2(6) . . . . ? C3 C4 C7 C8 154.9(4) . . . . ? C5 C4 C7 C8 -22.9(7) . . . . ? C4 C7 C8 C9 -177.6(4) . . . . ? C7 C8 C9 C10 51.4(6) . . . . ? C7 C8 C9 C22 -130.6(4) . . . . ? C22 C9 C10 C11 -173.4(4) . . . . ? C8 C9 C10 C11 4.6(6) . . . . ? C22 C9 C10 C15 3.0(5) . . . . ? C8 C9 C10 C15 -179.0(4) . . . . ? C9 C10 C11 C12 -179.7(4) . . . . ? C15 C10 C11 C12 3.8(6) . . . . ? C10 C11 C12 C13 0.5(6) . . . . ? C11 C12 C13 C14 -2.5(6) . . . . ? C12 C13 C14 C15 0.0(6) . . . . ? C13 C14 C15 C16 -175.4(4) . . . . ? C13 C14 C15 C10 4.4(6) . . . . ? C9 C10 C15 C16 -2.9(6) . . . . ? C11 C10 C15 C16 173.7(3) . . . . ? C9 C10 C15 C14 177.2(4) . . . . ? C11 C10 C15 C14 -6.1(5) . . . . ? C14 C15 C16 C17 -179.3(4) . . . . ? C10 C15 C16 C17 0.9(6) . . . . ? C14 C15 C16 C23 7.5(6) . . . . ? C10 C15 C16 C23 -172.4(4) . . . . ? C15 C16 C17 C18 -177.6(4) . . . . ? C23 C16 C17 C18 -4.5(6) . . . . ? C15 C16 C17 C22 1.0(6) . . . . ? C23 C16 C17 C22 174.1(4) . . . . ? C16 C17 C18 C19 179.8(4) . . . . ? C22 C17 C18 C19 1.2(6) . . . . ? C17 C18 C19 C20 0.3(7) . . . . ? C18 C19 C20 C21 -0.7(7) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C10 C9 C22 C21 178.8(4) . . . . ? C8 C9 C22 C21 0.7(6) . . . . ? C10 C9 C22 C17 -1.1(5) . . . . ? C8 C9 C22 C17 -179.2(4) . . . . ? C20 C21 C22 C9 -178.2(4) . . . . ? C20 C21 C22 C17 1.8(6) . . . . ? C16 C17 C22 C9 -0.9(6) . . . . ? C18 C17 C22 C9 177.8(4) . . . . ? C16 C17 C22 C21 179.2(4) . . . . ? C18 C17 C22 C21 -2.1(5) . . . . ? C17 C16 C23 C24 68.4(7) . . . . ? C15 C16 C23 C24 -118.4(6) . . . . ? C16 C23 C24 C25 -175.7(4) . . . . ? C23 C24 C25 C26 4.8(9) . . . . ? C23 C24 C25 C30 -174.6(5) . . . . ? C30 C25 C26 C27 -2.3(10) . . . . ? C24 C25 C26 C27 178.3(6) . . . . ? C25 C26 C27 C28 -2.7(12) . . . . ? C26 C27 C28 C29 6.4(12) . . . . ? C26 C27 C28 O2 -176.9(7) . . . . ? C27 C28 C29 C30 -4.9(10) . . . . ? O2 C28 C29 C30 178.9(6) . . . . ? C26 C25 C30 C29 3.8(8) . . . . ? C24 C25 C30 C29 -176.8(4) . . . . ? C28 C29 C30 C25 -0.2(8) . . . . ? O1 C31 C32 C33 179.3(4) . . . . ? C31 C32 C33 C34 175.1(4) . . . . ? C32 C33 C34 C35 173.6(4) . . . . ? C33 C34 C35 C36 176.4(4) . . . . ? C34 C35 C36 C37 -178.8(4) . . . . ? C35 C36 C37 C38 175.3(4) . . . . ? O2 C39 C40 C41 -177.7(6) . . . . ? C39 C40 C41 C42 -178.6(6) . . . . ? C40 C41 C42 C43 -175.3(6) . . . . ? C41 C42 C43 C44 178.8(6) . . . . ? C42 C43 C44 C45 -177.4(6) . . . . ? C43 C44 C45 C46 -178.3(7) . . . . ? O3 C47 C48 C49 179.9(4) . . . . ? C52 C47 C48 C49 0.6(6) . . . . ? C47 C48 C49 C50 0.8(7) . . . . ? C48 C49 C50 C51 -1.5(6) . . . . ? C48 C49 C50 C53 177.7(4) . . . . ? C49 C50 C51 C52 0.8(6) . . . . ? C53 C50 C51 C52 -178.3(4) . . . . ? C50 C51 C52 C47 0.5(7) . . . . ? O3 C47 C52 C51 179.4(4) . . . . ? C48 C47 C52 C51 -1.3(7) . . . . ? C49 C50 C53 C54 -178.0(4) . . . . ? C51 C50 C53 C54 1.1(7) . . . . ? C50 C53 C54 C55 176.9(4) . . . . ? C53 C54 C55 C61 127.5(5) . . . . ? C53 C54 C55 C56 -56.4(6) . . . . ? C61 C55 C56 C57 176.4(4) . . . . ? C54 C55 C56 C57 0.3(6) . . . . ? C61 C55 C56 C61 -0.8(6) . . . 2_456 ? C54 C55 C56 C61 -176.9(4) . . . 2_456 ? C55 C56 C57 C58 -178.5(4) . . . . ? C61 C56 C57 C58 -1.2(6) 2_456 . . . ? C56 C57 C58 C59 1.0(6) . . . . ? C57 C58 C59 C60 0.1(6) . . . 2_456 ? C56 C55 C61 C60 177.7(4) . . . . ? C54 C55 C61 C60 -6.1(5) . . . . ? C56 C55 C61 C56 0.8(6) . . . 2_456 ? C54 C55 C61 C56 177.1(3) . . . 2_456 ? C59 C60 C61 C55 -177.6(4) 2_456 . . . ? C59 C60 C61 C56 -0.6(6) 2_456 . . 2_456 ? O3 C62 C63 C64 -170.2(3) . . . . ? C62 C63 C64 C65 178.3(3) . . . . ? C63 C64 C65 C66 178.6(3) . . . . ? C64 C65 C66 C67 179.0(3) . . . . ? C65 C66 C67 C68 173.0(4) . . . . ? C66 C67 C68 C69 177.3(4) . . . . ? C2 C1 O1 C31 -10.3(6) . . . . ? C6 C1 O1 C31 170.7(4) . . . . ? C32 C31 O1 C1 -172.3(3) . . . . ? C40 C39 O2 C28 -172.9(6) . . . . ? C29 C28 O2 C39 -12.5(11) . . . . ? C27 C28 O2 C39 171.2(6) . . . . ? C48 C47 O3 C62 14.0(6) . . . . ? C52 C47 O3 C62 -166.7(4) . . . . ? C63 C62 O3 C47 175.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.776 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.067 data_09161m _database_code_depnum_ccdc_archive 'CCDC 886643' #TrackingRef 'web_deposit_cif_file_2_ZhenguoChi_1339763597.DSA9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H58 O2' _chemical_formula_weight 666.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7236(13) _cell_length_b 12.0059(18) _cell_length_c 19.476(3) _cell_angle_alpha 103.551(2) _cell_angle_beta 100.225(2) _cell_angle_gamma 100.499(2) _cell_volume 1897.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6316 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.97 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9710 _exptl_absorpt_correction_T_max 0.9823 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15934 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.03 _reflns_number_total 8055 _reflns_number_gt 5563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0572P)^2^+0.3862P] 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 8055 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 C1 C 0.98050(17) 0.59061(13) 0.75755(8) 0.0293(3) Uani 1 1 d . . . C2 C 1.00353(18) 0.70224(13) 0.74663(8) 0.0338(3) Uani 1 1 d . . . H2 H 1.0867 0.7647 0.7789 0.041 Uiso 1 1 calc R . . C3 C 0.90625(18) 0.72258(13) 0.68920(8) 0.0339(3) Uani 1 1 d . . . H3 H 0.9224 0.7995 0.6827 0.041 Uiso 1 1 calc R . . C4 C 0.78440(17) 0.63229(13) 0.64031(8) 0.0284(3) Uani 1 1 d . . . C5 C 0.76935(18) 0.52045(13) 0.65036(8) 0.0327(3) Uani 1 1 d . . . H5 H 0.6907 0.4567 0.6165 0.039 Uiso 1 1 calc R . . C6 C 0.86561(18) 0.49862(13) 0.70838(8) 0.0342(4) Uani 1 1 d . . . H6 H 0.8524 0.4212 0.7141 0.041 Uiso 1 1 calc R . . C7 C 0.66975(17) 0.65178(13) 0.58174(8) 0.0305(3) Uani 1 1 d . . . H7 H 0.6006 0.5834 0.5475 0.037 Uiso 1 1 calc R . . C8 C 0.65276(17) 0.75457(13) 0.57177(8) 0.0285(3) Uani 1 1 d . . . H8 H 0.7268 0.8227 0.6040 0.034 Uiso 1 1 calc R . . C9 C 0.53023(16) 0.77442(12) 0.51564(7) 0.0257(3) Uani 1 1 d . . . C10 C 0.58106(16) 0.84472(12) 0.47147(7) 0.0253(3) Uani 1 1 d . . . C11 C 0.74736(17) 0.88820(13) 0.47657(8) 0.0294(3) Uani 1 1 d . . . H11 H 0.8243 0.8626 0.5064 0.035 Uiso 1 1 calc R . . C12 C 0.79790(18) 0.96534(13) 0.43980(8) 0.0315(3) Uani 1 1 d . . . H12 H 0.9093 0.9934 0.4443 0.038 Uiso 1 1 calc R . . C13 C 0.68557(18) 1.00421(13) 0.39479(8) 0.0309(3) Uani 1 1 d . . . H13 H 0.7219 1.0614 0.3712 0.037 Uiso 1 1 calc R . . C14 C 0.52670(17) 0.96033(12) 0.38511(7) 0.0283(3) Uani 1 1 d . . . H14 H 0.4531 0.9857 0.3535 0.034 Uiso 1 1 calc R . . C15 C 0.46638(16) 0.87660(12) 0.42129(7) 0.0247(3) Uani 1 1 d . . . C16 C 0.30146(17) 0.83160(12) 0.41318(7) 0.0261(3) Uani 1 1 d . . . C17 C 0.25061(16) 0.76258(12) 0.45810(7) 0.0253(3) Uani 1 1 d . . . C18 C 0.08452(17) 0.72048(13) 0.45420(8) 0.0319(3) Uani 1 1 d . . . H18 H 0.0071 0.7332 0.4177 0.038 Uiso 1 1 calc R . . C19 C 0.03420(18) 0.66287(14) 0.50122(8) 0.0354(4) Uani 1 1 d . . . H19 H -0.0772 0.6376 0.4981 0.042 Uiso 1 1 calc R . . C20 C 0.14649(18) 0.64026(14) 0.55480(8) 0.0351(4) Uani 1 1 d . . . H20 H 0.1104 0.6013 0.5882 0.042 Uiso 1 1 calc R . . C21 C 0.30557(18) 0.67377(13) 0.55892(8) 0.0308(3) Uani 1 1 d . . . H21 H 0.3794 0.6561 0.5946 0.037 Uiso 1 1 calc R . . C22 C 0.36515(16) 0.73531(12) 0.51071(7) 0.0256(3) Uani 1 1 d . . . C23 C 0.18019(17) 0.86410(13) 0.36317(8) 0.0286(3) Uani 1 1 d . . . H23 H 0.0992 0.8939 0.3832 0.034 Uiso 1 1 calc R . . C24 C 0.17174(17) 0.85625(13) 0.29313(8) 0.0291(3) Uani 1 1 d . . . H24 H 0.2474 0.8213 0.2718 0.035 Uiso 1 1 calc R . . C25 C 0.05605(17) 0.89678(12) 0.24599(7) 0.0277(3) Uani 1 1 d . . . C26 C 0.08221(18) 0.91105(14) 0.18020(8) 0.0336(3) Uani 1 1 d . . . H26 H 0.1716 0.8881 0.1644 0.040 Uiso 1 1 calc R . . C27 C -0.01736(18) 0.95778(14) 0.13632(8) 0.0331(3) Uani 1 1 d . . . H27 H 0.0041 0.9662 0.0914 0.040 Uiso 1 1 calc R . . C28 C -0.14736(17) 0.99170(12) 0.15864(7) 0.0277(3) Uani 1 1 d . . . C29 C -0.17889(18) 0.97474(14) 0.22339(8) 0.0342(3) Uani 1 1 d . . . H29 H -0.2700 0.9958 0.2384 0.041 Uiso 1 1 calc R . . C30 C -0.07992(17) 0.92795(14) 0.26605(8) 0.0333(3) Uani 1 1 d . . . H30 H -0.1043 0.9166 0.3099 0.040 Uiso 1 1 calc R . . C31 C 1.03578(18) 0.47785(14) 0.84165(8) 0.0336(3) Uani 1 1 d . . . H31A H 1.0467 0.4078 0.8059 0.040 Uiso 1 1 calc R . . H31B H 0.9235 0.4653 0.8468 0.040 Uiso 1 1 calc R . . C32 C 1.14868(19) 0.49713(13) 0.91372(8) 0.0333(3) Uani 1 1 d . . . H32A H 1.1365 0.5680 0.9483 0.040 Uiso 1 1 calc R . . H32B H 1.2601 0.5125 0.9076 0.040 Uiso 1 1 calc R . . C33 C 1.12093(19) 0.39350(14) 0.94574(8) 0.0354(4) Uani 1 1 d . . . H33A H 1.1295 0.3219 0.9106 0.042 Uiso 1 1 calc R . . H33B H 1.0109 0.3799 0.9538 0.042 Uiso 1 1 calc R . . C34 C 1.24007(19) 0.41313(14) 1.01718(8) 0.0350(4) Uani 1 1 d . . . H34A H 1.3498 0.4288 1.0090 0.042 Uiso 1 1 calc R . . H34B H 1.2299 0.4843 1.0522 0.042 Uiso 1 1 calc R . . C35 C 1.2195(2) 0.31079(14) 1.05096(8) 0.0383(4) Uani 1 1 d . . . H35A H 1.1126 0.2983 1.0624 0.046 Uiso 1 1 calc R . . H35B H 1.2232 0.2383 1.0151 0.046 Uiso 1 1 calc R . . C36 C 1.3466(2) 0.33046(14) 1.11960(8) 0.0381(4) Uani 1 1 d . . . H36A H 1.4534 0.3504 1.1088 0.046 Uiso 1 1 calc R . . H36B H 1.3363 0.3992 1.1566 0.046 Uiso 1 1 calc R . . C37 C 1.3390(2) 0.22644(14) 1.15149(8) 0.0370(4) Uani 1 1 d . . . H37A H 1.2337 0.2079 1.1638 0.044 Uiso 1 1 calc R . . H37B H 1.3463 0.1570 1.1141 0.044 Uiso 1 1 calc R . . C38 C 1.4698(2) 0.24667(15) 1.21861(9) 0.0446(4) Uani 1 1 d . . . H38A H 1.4598 0.3139 1.2568 0.054 Uiso 1 1 calc R . . H38B H 1.5752 0.2683 1.2069 0.054 Uiso 1 1 calc R . . C39 C 1.4649(2) 0.14036(16) 1.24813(10) 0.0524(5) Uani 1 1 d . . . H39A H 1.3622 0.1198 1.2613 0.079 Uiso 1 1 calc R . . H39B H 1.5525 0.1588 1.2912 0.079 Uiso 1 1 calc R . . H39C H 1.4767 0.0737 1.2110 0.079 Uiso 1 1 calc R . . C40 C -0.21837(18) 1.07193(14) 0.05849(8) 0.0329(3) Uani 1 1 d . . . H40A H -0.2318 0.9990 0.0193 0.039 Uiso 1 1 calc R . . H40B H -0.1068 1.1184 0.0686 0.039 Uiso 1 1 calc R . . C41 C -0.33420(18) 1.14276(14) 0.03556(8) 0.0323(3) Uani 1 1 d . . . H41A H -0.3093 1.2202 0.0721 0.039 Uiso 1 1 calc R . . H41B H -0.4444 1.1012 0.0337 0.039 Uiso 1 1 calc R . . C42 C -0.32598(19) 1.16170(14) -0.03862(8) 0.0333(3) Uani 1 1 d . . . H42A H -0.2159 1.2043 -0.0362 0.040 Uiso 1 1 calc R . . H42B H -0.3480 1.0839 -0.0746 0.040 Uiso 1 1 calc R . . C43 C -0.44370(18) 1.23088(14) -0.06469(8) 0.0330(3) Uani 1 1 d . . . H43A H -0.5538 1.1884 -0.0670 0.040 Uiso 1 1 calc R . . H43B H -0.4215 1.3088 -0.0288 0.040 Uiso 1 1 calc R . . C44 C -0.43530(18) 1.24928(14) -0.13892(8) 0.0330(3) Uani 1 1 d . . . H44A H -0.3256 1.2928 -0.1364 0.040 Uiso 1 1 calc R . . H44B H -0.4558 1.1714 -0.1746 0.040 Uiso 1 1 calc R . . C45 C -0.55418(19) 1.31669(14) -0.16565(8) 0.0339(3) Uani 1 1 d . . . H45A H -0.5321 1.3951 -0.1303 0.041 Uiso 1 1 calc R . . H45B H -0.6635 1.2741 -0.1670 0.041 Uiso 1 1 calc R . . C46 C -0.55011(19) 1.33369(14) -0.24041(8) 0.0349(4) Uani 1 1 d . . . H46A H -0.4434 1.3815 -0.2384 0.042 Uiso 1 1 calc R . . H46B H -0.5649 1.2558 -0.2753 0.042 Uiso 1 1 calc R . . C47 C -0.6777(2) 1.39372(14) -0.26796(8) 0.0370(4) Uani 1 1 d . . . H47A H -0.7845 1.3421 -0.2743 0.044 Uiso 1 1 calc R . . H47B H -0.6695 1.4679 -0.2307 0.044 Uiso 1 1 calc R . . C48 C -0.6662(2) 1.42192(15) -0.33920(9) 0.0437(4) Uani 1 1 d . . . H48A H -0.5629 1.4761 -0.3329 0.066 Uiso 1 1 calc R . . H48B H -0.7533 1.4588 -0.3540 0.066 Uiso 1 1 calc R . . H48C H -0.6750 1.3490 -0.3766 0.066 Uiso 1 1 calc R . . O1 O 1.07798(13) 0.58133(9) 0.81832(6) 0.0372(3) Uani 1 1 d . . . O2 O -0.25114(12) 1.04311(9) 0.12239(5) 0.0336(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0290(8) 0.0351(8) 0.0262(7) 0.0127(6) 0.0020(6) 0.0120(6) C2 0.0319(8) 0.0317(8) 0.0331(8) 0.0099(6) -0.0027(6) 0.0045(6) C3 0.0349(8) 0.0311(8) 0.0361(8) 0.0152(7) 0.0011(7) 0.0079(7) C4 0.0276(7) 0.0308(8) 0.0277(7) 0.0092(6) 0.0035(6) 0.0103(6) C5 0.0324(8) 0.0304(8) 0.0310(8) 0.0055(6) -0.0014(6) 0.0090(6) C6 0.0387(9) 0.0286(8) 0.0353(8) 0.0125(7) 0.0007(7) 0.0107(7) C7 0.0289(8) 0.0327(8) 0.0273(7) 0.0065(6) 0.0003(6) 0.0091(6) C8 0.0257(7) 0.0341(8) 0.0256(7) 0.0095(6) 0.0018(6) 0.0089(6) C9 0.0280(7) 0.0264(7) 0.0219(7) 0.0052(6) 0.0012(6) 0.0109(6) C10 0.0272(7) 0.0253(7) 0.0230(7) 0.0047(6) 0.0032(6) 0.0105(6) C11 0.0279(8) 0.0333(8) 0.0272(7) 0.0078(6) 0.0026(6) 0.0117(6) C12 0.0263(7) 0.0363(8) 0.0301(8) 0.0073(6) 0.0050(6) 0.0066(6) C13 0.0351(8) 0.0322(8) 0.0276(7) 0.0122(6) 0.0073(6) 0.0083(6) C14 0.0333(8) 0.0290(8) 0.0228(7) 0.0069(6) 0.0032(6) 0.0116(6) C15 0.0277(7) 0.0264(7) 0.0202(6) 0.0046(5) 0.0038(6) 0.0108(6) C16 0.0290(7) 0.0283(7) 0.0215(7) 0.0051(6) 0.0042(6) 0.0122(6) C17 0.0258(7) 0.0269(7) 0.0230(7) 0.0055(6) 0.0027(6) 0.0099(6) C18 0.0278(8) 0.0352(8) 0.0319(8) 0.0095(6) 0.0016(6) 0.0103(6) C19 0.0257(8) 0.0393(9) 0.0419(9) 0.0136(7) 0.0076(7) 0.0068(7) C20 0.0357(8) 0.0376(9) 0.0373(8) 0.0178(7) 0.0113(7) 0.0095(7) C21 0.0330(8) 0.0338(8) 0.0287(7) 0.0134(6) 0.0034(6) 0.0124(6) C22 0.0280(7) 0.0247(7) 0.0229(7) 0.0048(6) 0.0028(6) 0.0085(6) C23 0.0258(7) 0.0327(8) 0.0279(7) 0.0088(6) 0.0032(6) 0.0109(6) C24 0.0286(8) 0.0313(8) 0.0279(7) 0.0080(6) 0.0034(6) 0.0113(6) C25 0.0282(7) 0.0271(7) 0.0251(7) 0.0067(6) 0.0003(6) 0.0065(6) C26 0.0348(8) 0.0422(9) 0.0272(7) 0.0100(7) 0.0069(6) 0.0172(7) C27 0.0375(9) 0.0403(9) 0.0234(7) 0.0121(6) 0.0053(6) 0.0115(7) C28 0.0267(7) 0.0261(7) 0.0267(7) 0.0091(6) -0.0027(6) 0.0032(6) C29 0.0262(8) 0.0478(9) 0.0339(8) 0.0178(7) 0.0068(6) 0.0132(7) C30 0.0291(8) 0.0464(9) 0.0282(8) 0.0179(7) 0.0048(6) 0.0105(7) C31 0.0351(8) 0.0372(9) 0.0313(8) 0.0163(7) 0.0036(7) 0.0108(7) C32 0.0371(9) 0.0340(8) 0.0300(8) 0.0128(7) 0.0033(7) 0.0108(7) C33 0.0383(9) 0.0378(9) 0.0316(8) 0.0152(7) 0.0031(7) 0.0100(7) C34 0.0396(9) 0.0363(9) 0.0313(8) 0.0153(7) 0.0034(7) 0.0109(7) C35 0.0418(9) 0.0393(9) 0.0347(8) 0.0180(7) 0.0015(7) 0.0085(7) C36 0.0452(10) 0.0366(9) 0.0335(8) 0.0158(7) 0.0022(7) 0.0104(7) C37 0.0441(9) 0.0385(9) 0.0320(8) 0.0164(7) 0.0052(7) 0.0136(7) C38 0.0552(11) 0.0437(10) 0.0343(9) 0.0165(8) -0.0009(8) 0.0134(8) C39 0.0712(13) 0.0489(11) 0.0383(10) 0.0183(8) -0.0017(9) 0.0224(10) C40 0.0356(8) 0.0378(9) 0.0281(7) 0.0154(7) 0.0035(6) 0.0110(7) C41 0.0340(8) 0.0354(8) 0.0295(8) 0.0132(6) 0.0032(6) 0.0117(7) C42 0.0387(9) 0.0352(8) 0.0289(8) 0.0129(6) 0.0045(6) 0.0133(7) C43 0.0349(8) 0.0355(8) 0.0301(8) 0.0131(7) 0.0029(6) 0.0116(7) C44 0.0362(8) 0.0349(8) 0.0297(8) 0.0126(6) 0.0034(6) 0.0123(7) C45 0.0385(9) 0.0346(8) 0.0310(8) 0.0121(7) 0.0046(7) 0.0140(7) C46 0.0383(9) 0.0372(9) 0.0322(8) 0.0135(7) 0.0041(7) 0.0154(7) C47 0.0404(9) 0.0388(9) 0.0357(8) 0.0157(7) 0.0046(7) 0.0161(7) C48 0.0499(10) 0.0455(10) 0.0365(9) 0.0163(8) 0.0008(8) 0.0155(8) O1 0.0395(6) 0.0367(6) 0.0333(6) 0.0177(5) -0.0055(5) 0.0068(5) O2 0.0326(6) 0.0426(6) 0.0309(5) 0.0200(5) 0.0036(4) 0.0130(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.3694(16) . ? C1 C6 1.379(2) . ? C1 C2 1.390(2) . ? C2 C3 1.377(2) . ? C2 H2 0.9500 . ? C3 C4 1.396(2) . ? C3 H3 0.9500 . ? C4 C5 1.388(2) . ? C4 C7 1.4704(19) . ? C5 C6 1.390(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.323(2) . ? C7 H7 0.9500 . ? C8 C9 1.4814(18) . ? C8 H8 0.9500 . ? C9 C22 1.410(2) . ? C9 C10 1.4101(19) . ? C10 C11 1.427(2) . ? C10 C15 1.4388(18) . ? C11 C12 1.356(2) . ? C11 H11 0.9500 . ? C12 C13 1.414(2) . ? C12 H12 0.9500 . ? C13 C14 1.352(2) . ? C13 H13 0.9500 . ? C14 C15 1.4334(19) . ? C14 H14 0.9500 . ? C15 C16 1.4081(19) . ? C16 C17 1.4116(19) . ? C16 C23 1.4773(19) . ? C17 C18 1.427(2) . ? C17 C22 1.4383(18) . ? C18 C19 1.356(2) . ? C18 H18 0.9500 . ? C19 C20 1.410(2) . ? C19 H19 0.9500 . ? C20 C21 1.355(2) . ? C20 H20 0.9500 . ? C21 C22 1.4339(19) . ? C21 H21 0.9500 . ? C23 C24 1.3330(19) . ? C23 H23 0.9500 . ? C24 C25 1.4688(19) . ? C24 H24 0.9500 . ? C25 C26 1.384(2) . ? C25 C30 1.399(2) . ? C26 C27 1.392(2) . ? C26 H26 0.9500 . ? C27 C28 1.379(2) . ? C27 H27 0.9500 . ? C28 O2 1.3711(16) . ? C28 C29 1.389(2) . ? C29 C30 1.376(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 O1 1.4292(17) . ? C31 C32 1.506(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.518(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.522(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.521(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.518(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.516(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.513(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.515(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 O2 1.4290(17) . ? C40 C41 1.508(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.526(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.525(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.525(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.5210(19) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.522(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.519(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.519(2) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 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 O1 C1 C6 124.72(13) . . ? O1 C1 C2 115.56(13) . . ? C6 C1 C2 119.73(13) . . ? C3 C2 C1 120.24(14) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 121.26(14) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 117.27(13) . . ? C5 C4 C7 119.56(13) . . ? C3 C4 C7 123.12(13) . . ? C4 C5 C6 122.14(14) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C1 C6 C5 119.22(14) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C8 C7 C4 126.80(14) . . ? C8 C7 H7 116.6 . . ? C4 C7 H7 116.6 . . ? C7 C8 C9 126.74(14) . . ? C7 C8 H8 116.6 . . ? C9 C8 H8 116.6 . . ? C22 C9 C10 119.57(12) . . ? C22 C9 C8 121.49(13) . . ? C10 C9 C8 118.60(12) . . ? C9 C10 C11 120.87(12) . . ? C9 C10 C15 120.76(12) . . ? C11 C10 C15 118.35(13) . . ? C12 C11 C10 121.39(13) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 120.33(14) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.32(14) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 121.75(13) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 122.71(12) . . ? C16 C15 C10 119.63(13) . . ? C14 C15 C10 117.52(12) . . ? C15 C16 C17 119.47(12) . . ? C15 C16 C23 121.15(13) . . ? C17 C16 C23 119.15(12) . . ? C16 C17 C18 121.19(12) . . ? C16 C17 C22 120.83(13) . . ? C18 C17 C22 117.95(13) . . ? C19 C18 C17 121.77(14) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 120.30(14) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 120.38(14) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 121.55(13) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C9 C22 C21 122.46(13) . . ? C9 C22 C17 119.54(13) . . ? C21 C22 C17 117.92(13) . . ? C24 C23 C16 127.22(13) . . ? C24 C23 H23 116.4 . . ? C16 C23 H23 116.4 . . ? C23 C24 C25 125.94(13) . . ? C23 C24 H24 117.0 . . ? C25 C24 H24 117.0 . . ? C26 C25 C30 116.85(13) . . ? C26 C25 C24 120.48(13) . . ? C30 C25 C24 122.59(13) . . ? C25 C26 C27 122.54(14) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C28 C27 C26 119.38(14) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? O2 C28 C27 125.51(13) . . ? O2 C28 C29 115.41(13) . . ? C27 C28 C29 119.07(13) . . ? C30 C29 C28 120.89(14) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C25 121.18(14) . . ? C29 C30 H30 119.4 . . ? C25 C30 H30 119.4 . . ? O1 C31 C32 106.80(12) . . ? O1 C31 H31A 110.4 . . ? C32 C31 H31A 110.4 . . ? O1 C31 H31B 110.4 . . ? C32 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C31 C32 C33 113.44(13) . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C32 C33 C34 112.53(13) . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33B 109.1 . . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 114.68(13) . . ? C35 C34 H34A 108.6 . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C33 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C36 C35 C34 113.15(13) . . ? C36 C35 H35A 108.9 . . ? C34 C35 H35A 108.9 . . ? C36 C35 H35B 108.9 . . ? C34 C35 H35B 108.9 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C35 114.88(14) . . ? C37 C36 H36A 108.5 . . ? C35 C36 H36A 108.5 . . ? C37 C36 H36B 108.5 . . ? C35 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C38 C37 C36 113.99(14) . . ? C38 C37 H37A 108.8 . . ? C36 C37 H37A 108.8 . . ? C38 C37 H37B 108.8 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.6 . . ? C37 C38 C39 113.43(15) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O2 C40 C41 107.94(12) . . ? O2 C40 H40A 110.1 . . ? C41 C40 H40A 110.1 . . ? O2 C40 H40B 110.1 . . ? C41 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? C40 C41 C42 111.81(12) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? C43 C42 C41 113.60(13) . . ? C43 C42 H42A 108.8 . . ? C41 C42 H42A 108.8 . . ? C43 C42 H42B 108.8 . . ? C41 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C42 113.39(13) . . ? C44 C43 H43A 108.9 . . ? C42 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? C42 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C45 C44 C43 113.59(13) . . ? C45 C44 H44A 108.8 . . ? C43 C44 H44A 108.8 . . ? C45 C44 H44B 108.8 . . ? C43 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C44 C45 C46 114.38(13) . . ? C44 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? C44 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C47 C46 C45 113.24(13) . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46A 108.9 . . ? C47 C46 H46B 108.9 . . ? C45 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C48 C47 C46 114.15(14) . . ? C48 C47 H47A 108.7 . . ? C46 C47 H47A 108.7 . . ? C48 C47 H47B 108.7 . . ? C46 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C1 O1 C31 117.82(12) . . ? C28 O2 C40 118.38(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -176.65(14) . . . . ? C6 C1 C2 C3 3.6(2) . . . . ? C1 C2 C3 C4 -0.8(2) . . . . ? C2 C3 C4 C5 -2.4(2) . . . . ? C2 C3 C4 C7 175.03(14) . . . . ? C3 C4 C5 C6 3.0(2) . . . . ? C7 C4 C5 C6 -174.54(14) . . . . ? O1 C1 C6 C5 177.25(14) . . . . ? C2 C1 C6 C5 -3.0(2) . . . . ? C4 C5 C6 C1 -0.3(2) . . . . ? C5 C4 C7 C8 169.17(15) . . . . ? C3 C4 C7 C8 -8.2(2) . . . . ? C4 C7 C8 C9 -175.65(14) . . . . ? C7 C8 C9 C22 58.6(2) . . . . ? C7 C8 C9 C10 -128.17(16) . . . . ? C22 C9 C10 C11 178.35(13) . . . . ? C8 C9 C10 C11 4.9(2) . . . . ? C22 C9 C10 C15 -0.2(2) . . . . ? C8 C9 C10 C15 -173.63(12) . . . . ? C9 C10 C11 C12 -173.30(13) . . . . ? C15 C10 C11 C12 5.3(2) . . . . ? C10 C11 C12 C13 -0.4(2) . . . . ? C11 C12 C13 C14 -3.3(2) . . . . ? C12 C13 C14 C15 1.9(2) . . . . ? C13 C14 C15 C16 178.65(13) . . . . ? C13 C14 C15 C10 3.0(2) . . . . ? C9 C10 C15 C16 -3.7(2) . . . . ? C11 C10 C15 C16 177.74(12) . . . . ? C9 C10 C15 C14 172.15(12) . . . . ? C11 C10 C15 C14 -6.46(19) . . . . ? C14 C15 C16 C17 -171.11(13) . . . . ? C10 C15 C16 C17 4.47(19) . . . . ? C14 C15 C16 C23 3.3(2) . . . . ? C10 C15 C16 C23 178.88(12) . . . . ? C15 C16 C17 C18 176.70(13) . . . . ? C23 C16 C17 C18 2.2(2) . . . . ? C15 C16 C17 C22 -1.5(2) . . . . ? C23 C16 C17 C22 -176.07(12) . . . . ? C16 C17 C18 C19 -174.20(14) . . . . ? C22 C17 C18 C19 4.1(2) . . . . ? C17 C18 C19 C20 -1.6(2) . . . . ? C18 C19 C20 C21 -1.3(2) . . . . ? C19 C20 C21 C22 1.5(2) . . . . ? C10 C9 C22 C21 -173.59(13) . . . . ? C8 C9 C22 C21 -0.4(2) . . . . ? C10 C9 C22 C17 3.15(19) . . . . ? C8 C9 C22 C17 176.37(12) . . . . ? C20 C21 C22 C9 177.82(14) . . . . ? C20 C21 C22 C17 1.0(2) . . . . ? C16 C17 C22 C9 -2.3(2) . . . . ? C18 C17 C22 C9 179.38(13) . . . . ? C16 C17 C22 C21 174.57(12) . . . . ? C18 C17 C22 C21 -3.73(19) . . . . ? C15 C16 C23 C24 52.8(2) . . . . ? C17 C16 C23 C24 -132.77(16) . . . . ? C16 C23 C24 C25 -175.55(14) . . . . ? C23 C24 C25 C26 163.91(15) . . . . ? C23 C24 C25 C30 -13.0(2) . . . . ? C30 C25 C26 C27 2.1(2) . . . . ? C24 C25 C26 C27 -174.93(14) . . . . ? C25 C26 C27 C28 0.1(2) . . . . ? C26 C27 C28 O2 177.26(14) . . . . ? C26 C27 C28 C29 -2.1(2) . . . . ? O2 C28 C29 C30 -177.59(13) . . . . ? C27 C28 C29 C30 1.8(2) . . . . ? C28 C29 C30 C25 0.5(2) . . . . ? C26 C25 C30 C29 -2.4(2) . . . . ? C24 C25 C30 C29 174.58(14) . . . . ? O1 C31 C32 C33 -179.22(12) . . . . ? C31 C32 C33 C34 177.95(13) . . . . ? C32 C33 C34 C35 -178.92(13) . . . . ? C33 C34 C35 C36 176.42(14) . . . . ? C34 C35 C36 C37 -175.02(14) . . . . ? C35 C36 C37 C38 178.29(14) . . . . ? C36 C37 C38 C39 -177.65(15) . . . . ? O2 C40 C41 C42 -171.23(12) . . . . ? C40 C41 C42 C43 178.82(13) . . . . ? C41 C42 C43 C44 -179.85(13) . . . . ? C42 C43 C44 C45 179.16(13) . . . . ? C43 C44 C45 C46 -178.76(13) . . . . ? C44 C45 C46 C47 175.99(13) . . . . ? C45 C46 C47 C48 174.58(13) . . . . ? C6 C1 O1 C31 -14.7(2) . . . . ? C2 C1 O1 C31 165.54(13) . . . . ? C32 C31 O1 C1 -172.88(12) . . . . ? C27 C28 O2 C40 -4.4(2) . . . . ? C29 C28 O2 C40 175.00(12) . . . . ? C41 C40 O2 C28 -171.75(12) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.267 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.040 data_04021m _database_code_depnum_ccdc_archive 'CCDC 886644' #TrackingRef 'web_deposit_cif_file_3_ZhenguoChi_1339763597.DSA10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H62 O2' _chemical_formula_sum 'C50 H62 O2' _chemical_formula_weight 695.00 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 triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.2873(11) _cell_length_b 11.926(2) _cell_length_c 16.467(3) _cell_angle_alpha 95.422(3) _cell_angle_beta 98.427(3) _cell_angle_gamma 96.703(3) _cell_volume 1013.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4113 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.97 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 378 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9815 _exptl_absorpt_correction_T_max 0.9867 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8376 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 27.05 _reflns_number_total 4276 _reflns_number_gt 3219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0642P)^2^+0.2398P] 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 4276 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1 C 0.9113(3) 1.40764(11) 0.43689(8) 0.0264(3) Uani 1 1 d . . . C2 C 0.7836(3) 1.50496(11) 0.43973(8) 0.0261(3) Uani 1 1 d . . . C3 C 0.5638(3) 1.51400(13) 0.38023(9) 0.0320(3) Uani 1 1 d . . . H3 H 0.5026 1.4530 0.3379 0.038 Uiso 1 1 calc R . . C4 C 0.4398(3) 1.60750(14) 0.38252(9) 0.0372(4) Uani 1 1 d . . . H4 H 0.2913 1.6105 0.3430 0.045 Uiso 1 1 calc R . . C5 C 0.5315(3) 1.70038(13) 0.44374(10) 0.0374(4) Uani 1 1 d . . . H5 H 0.4456 1.7660 0.4448 0.045 Uiso 1 1 calc R . . C6 C 0.7411(3) 1.69634(12) 0.50083(9) 0.0325(3) Uani 1 1 d . . . H6 H 0.8019 1.7603 0.5407 0.039 Uiso 1 1 calc R . . C7 C 0.8738(3) 1.59829(11) 0.50282(8) 0.0265(3) Uani 1 1 d . . . C8 C 0.8158(3) 1.31216(12) 0.37079(9) 0.0321(3) Uani 1 1 d . . . H8 H 0.6512 1.2709 0.3713 0.039 Uiso 1 1 calc R . . C9 C 0.9435(3) 1.28077(12) 0.31154(9) 0.0302(3) Uani 1 1 d . . . H9 H 1.1046 1.3254 0.3117 0.036 Uiso 1 1 calc R . . C10 C 0.8713(3) 1.18624(11) 0.24526(8) 0.0266(3) Uani 1 1 d . . . C11 C 1.0238(3) 1.17560(12) 0.18293(8) 0.0281(3) Uani 1 1 d . . . H11 H 1.1700 1.2305 0.1841 0.034 Uiso 1 1 calc R . . C12 C 0.9669(3) 1.08719(11) 0.11974(8) 0.0272(3) Uani 1 1 d . . . H12 H 1.0732 1.0820 0.0781 0.033 Uiso 1 1 calc R . . C13 C 0.7543(3) 1.00609(11) 0.11723(8) 0.0253(3) Uani 1 1 d . . . C14 C 0.6000(3) 1.01424(11) 0.17814(8) 0.0273(3) Uani 1 1 d . . . H14 H 0.4540 0.9590 0.1767 0.033 Uiso 1 1 calc R . . C15 C 0.6596(3) 1.10349(12) 0.24139(8) 0.0279(3) Uani 1 1 d . . . H15 H 0.5532 1.1082 0.2830 0.033 Uiso 1 1 calc R . . C16 C 0.5013(3) 0.83375(11) 0.04734(8) 0.0279(3) Uani 1 1 d . . . H16A H 0.3362 0.8659 0.0404 0.033 Uiso 1 1 calc R . . H16B H 0.5151 0.7952 0.0982 0.033 Uiso 1 1 calc R . . C17 C 0.5136(3) 0.75093(11) -0.02691(8) 0.0281(3) Uani 1 1 d . . . H17A H 0.6870 0.7261 -0.0213 0.034 Uiso 1 1 calc R . . H17B H 0.4901 0.7904 -0.0772 0.034 Uiso 1 1 calc R . . C18 C 0.3114(3) 0.64675(11) -0.03754(9) 0.0298(3) Uani 1 1 d . . . H18A H 0.1374 0.6710 -0.0442 0.036 Uiso 1 1 calc R . . H18B H 0.3333 0.6072 0.0127 0.036 Uiso 1 1 calc R . . C19 C 0.3327(3) 0.56495(12) -0.11237(9) 0.0310(3) Uani 1 1 d . . . H19A H 0.3069 0.6049 -0.1624 0.037 Uiso 1 1 calc R . . H19B H 0.5097 0.5440 -0.1062 0.037 Uiso 1 1 calc R . . C20 C 0.1417(3) 0.45651(11) -0.12562(9) 0.0318(3) Uani 1 1 d . . . H20A H 0.1649 0.4163 -0.0757 0.038 Uiso 1 1 calc R . . H20B H -0.0361 0.4765 -0.1335 0.038 Uiso 1 1 calc R . . C21 C 0.1760(3) 0.37745(12) -0.20016(9) 0.0316(3) Uani 1 1 d . . . H21A H 0.3556 0.3597 -0.1922 0.038 Uiso 1 1 calc R . . H21B H 0.1520 0.4185 -0.2497 0.038 Uiso 1 1 calc R . . C22 C -0.0056(3) 0.26607(11) -0.21708(9) 0.0298(3) Uani 1 1 d . . . H22A H -0.1860 0.2827 -0.2224 0.036 Uiso 1 1 calc R . . H22B H 0.0255 0.2217 -0.1696 0.036 Uiso 1 1 calc R . . C23 C 0.0300(3) 0.19492(12) -0.29547(9) 0.0313(3) Uani 1 1 d . . . H23A H 0.0121 0.2419 -0.3419 0.038 Uiso 1 1 calc R . . H23B H 0.2075 0.1745 -0.2883 0.038 Uiso 1 1 calc R . . C24 C -0.1591(3) 0.08679(12) -0.31823(9) 0.0346(3) Uani 1 1 d . . . H24A H -0.3370 0.1063 -0.3220 0.042 Uiso 1 1 calc R . . H24B H -0.1331 0.0370 -0.2738 0.042 Uiso 1 1 calc R . . C25 C -0.1297(4) 0.02192(15) -0.39983(11) 0.0523(5) Uani 1 1 d . . . H25A H -0.1498 0.0715 -0.4439 0.078 Uiso 1 1 calc R . . H25B H -0.2620 -0.0447 -0.4130 0.078 Uiso 1 1 calc R . . H25C H 0.0417 -0.0028 -0.3951 0.078 Uiso 1 1 calc R . . O1 O 0.71374(19) 0.92159(8) 0.05262(6) 0.0312(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0304(7) 0.0246(7) 0.0232(7) -0.0033(5) 0.0087(5) -0.0019(5) C2 0.0282(7) 0.0271(7) 0.0227(6) 0.0008(5) 0.0082(5) -0.0009(5) C3 0.0320(7) 0.0366(8) 0.0257(7) 0.0014(6) 0.0061(6) -0.0025(6) C4 0.0336(8) 0.0473(9) 0.0327(8) 0.0117(7) 0.0055(6) 0.0070(7) C5 0.0430(9) 0.0350(8) 0.0396(9) 0.0112(7) 0.0138(7) 0.0124(7) C6 0.0420(8) 0.0265(7) 0.0308(7) 0.0018(6) 0.0124(6) 0.0054(6) C7 0.0308(7) 0.0252(7) 0.0243(7) 0.0007(5) 0.0103(5) 0.0011(5) C8 0.0327(7) 0.0290(7) 0.0315(8) -0.0065(6) 0.0076(6) -0.0037(6) C9 0.0302(7) 0.0294(7) 0.0281(7) -0.0036(6) 0.0056(6) -0.0035(6) C10 0.0291(7) 0.0271(7) 0.0221(6) -0.0024(5) 0.0032(5) 0.0031(5) C11 0.0260(7) 0.0292(7) 0.0272(7) -0.0016(5) 0.0051(5) -0.0007(5) C12 0.0279(7) 0.0306(7) 0.0233(7) -0.0010(5) 0.0076(5) 0.0032(5) C13 0.0288(7) 0.0249(7) 0.0208(6) -0.0013(5) 0.0015(5) 0.0043(5) C14 0.0271(7) 0.0260(7) 0.0270(7) -0.0014(5) 0.0049(5) -0.0011(5) C15 0.0299(7) 0.0307(7) 0.0229(7) -0.0026(5) 0.0088(5) 0.0023(6) C16 0.0313(7) 0.0257(7) 0.0249(7) -0.0022(5) 0.0054(5) -0.0004(5) C17 0.0311(7) 0.0262(7) 0.0261(7) -0.0015(5) 0.0055(5) 0.0031(5) C18 0.0331(7) 0.0263(7) 0.0289(7) -0.0008(6) 0.0064(6) 0.0008(6) C19 0.0352(8) 0.0258(7) 0.0310(7) -0.0014(6) 0.0074(6) 0.0009(6) C20 0.0351(8) 0.0268(7) 0.0320(8) -0.0019(6) 0.0068(6) -0.0003(6) C21 0.0353(8) 0.0258(7) 0.0326(8) -0.0012(6) 0.0078(6) -0.0001(6) C22 0.0335(7) 0.0252(7) 0.0299(7) 0.0009(6) 0.0060(6) 0.0019(6) C23 0.0352(8) 0.0263(7) 0.0328(8) -0.0002(6) 0.0098(6) 0.0034(6) C24 0.0422(9) 0.0264(7) 0.0342(8) -0.0014(6) 0.0078(6) 0.0022(6) C25 0.0740(13) 0.0370(9) 0.0436(10) -0.0100(7) 0.0106(9) 0.0081(8) O1 0.0354(5) 0.0296(5) 0.0259(5) -0.0079(4) 0.0099(4) -0.0039(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 C1 C7 1.4082(19) 2_786 ? C1 C2 1.4098(19) . ? C1 C8 1.4855(18) . ? C2 C3 1.428(2) . ? C2 C7 1.4346(18) . ? C3 C4 1.358(2) . ? C3 H3 0.9500 . ? C4 C5 1.414(2) . ? C4 H4 0.9500 . ? C5 C6 1.352(2) . ? C5 H5 0.9500 . ? C6 C7 1.4327(19) . ? C6 H6 0.9500 . ? C7 C1 1.4082(19) 2_786 ? C8 C9 1.316(2) . ? C8 H8 0.9500 . ? C9 C10 1.4672(18) . ? C9 H9 0.9500 . ? C10 C15 1.3930(19) . ? C10 C11 1.4005(19) . ? C11 C12 1.3826(18) . ? C11 H11 0.9500 . ? C12 C13 1.3878(19) . ? C12 H12 0.9500 . ? C13 O1 1.3688(15) . ? C13 C14 1.3862(19) . ? C14 C15 1.3903(18) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 O1 1.4303(16) . ? C16 C17 1.5116(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.5202(19) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.5237(19) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.5220(19) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.5214(19) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.5224(19) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.5242(19) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.517(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.523(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 C1 C2 119.60(12) 2_786 . ? C7 C1 C8 120.85(12) 2_786 . ? C2 C1 C8 119.54(12) . . ? C1 C2 C3 121.39(12) . . ? C1 C2 C7 120.36(12) . . ? C3 C2 C7 118.25(13) . . ? C4 C3 C2 121.74(14) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 120.02(14) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.39(14) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.82(14) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C1 C7 C6 122.22(12) 2_786 . ? C1 C7 C2 120.03(12) 2_786 . ? C6 C7 C2 117.74(13) . . ? C9 C8 C1 124.50(13) . . ? C9 C8 H8 117.7 . . ? C1 C8 H8 117.7 . . ? C8 C9 C10 128.90(13) . . ? C8 C9 H9 115.5 . . ? C10 C9 H9 115.5 . . ? C15 C10 C11 117.24(12) . . ? C15 C10 C9 123.46(12) . . ? C11 C10 C9 119.28(12) . . ? C12 C11 C10 121.70(13) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 119.87(12) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? O1 C13 C14 124.47(12) . . ? O1 C13 C12 115.76(11) . . ? C14 C13 C12 119.77(12) . . ? C13 C14 C15 119.75(12) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C10 121.67(12) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? O1 C16 C17 106.58(11) . . ? O1 C16 H16A 110.4 . . ? C17 C16 H16A 110.4 . . ? O1 C16 H16B 110.4 . . ? C17 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? C16 C17 C18 113.28(11) . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 111.56(12) . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C20 C19 C18 114.72(12) . . ? C20 C19 H19A 108.6 . . ? C18 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? C18 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C19 112.21(12) . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 115.54(12) . . ? C20 C21 H21A 108.4 . . ? C22 C21 H21A 108.4 . . ? C20 C21 H21B 108.4 . . ? C22 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C21 C22 C23 112.33(12) . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 114.35(12) . . ? C24 C23 H23A 108.7 . . ? C22 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? C22 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C23 C24 C25 112.91(13) . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 O1 C16 118.67(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C1 C2 C3 -179.47(12) 2_786 . . . ? C8 C1 C2 C3 -0.1(2) . . . . ? C7 C1 C2 C7 0.9(2) 2_786 . . . ? C8 C1 C2 C7 -179.67(12) . . . . ? C1 C2 C3 C4 -179.96(13) . . . . ? C7 C2 C3 C4 -0.4(2) . . . . ? C2 C3 C4 C5 1.6(2) . . . . ? C3 C4 C5 C6 -0.7(2) . . . . ? C4 C5 C6 C7 -1.3(2) . . . . ? C5 C6 C7 C1 -178.60(13) . . . 2_786 ? C5 C6 C7 C2 2.5(2) . . . . ? C1 C2 C7 C1 -0.9(2) . . . 2_786 ? C3 C2 C7 C1 179.46(12) . . . 2_786 ? C1 C2 C7 C6 177.98(12) . . . . ? C3 C2 C7 C6 -1.61(18) . . . . ? C7 C1 C8 C9 -67.1(2) 2_786 . . . ? C2 C1 C8 C9 113.57(17) . . . . ? C1 C8 C9 C10 177.87(14) . . . . ? C8 C9 C10 C15 -8.5(2) . . . . ? C8 C9 C10 C11 172.98(15) . . . . ? C15 C10 C11 C12 0.3(2) . . . . ? C9 C10 C11 C12 178.97(13) . . . . ? C10 C11 C12 C13 -0.1(2) . . . . ? C11 C12 C13 O1 -179.79(12) . . . . ? C11 C12 C13 C14 0.0(2) . . . . ? O1 C13 C14 C15 179.68(12) . . . . ? C12 C13 C14 C15 -0.1(2) . . . . ? C13 C14 C15 C10 0.3(2) . . . . ? C11 C10 C15 C14 -0.4(2) . . . . ? C9 C10 C15 C14 -179.00(13) . . . . ? O1 C16 C17 C18 175.56(11) . . . . ? C16 C17 C18 C19 -179.31(11) . . . . ? C17 C18 C19 C20 178.17(12) . . . . ? C18 C19 C20 C21 -178.89(12) . . . . ? C19 C20 C21 C22 179.20(12) . . . . ? C20 C21 C22 C23 176.60(12) . . . . ? C21 C22 C23 C24 -176.02(12) . . . . ? C22 C23 C24 C25 176.15(13) . . . . ? C14 C13 O1 C16 -1.22(19) . . . . ? C12 C13 O1 C16 178.59(12) . . . . ? C17 C16 O1 C13 -177.31(11) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.242 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.042 data_02226 _database_code_depnum_ccdc_archive 'CCDC 886645' #TrackingRef 'web_deposit_cif_file_4_ZhenguoChi_1339763597.DSA11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H66 O2' _chemical_formula_sum 'C52 H66 O2' _chemical_formula_weight 723.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7012(6) _cell_length_b 7.8232(7) _cell_length_c 23.669(3) _cell_angle_alpha 92.182(8) _cell_angle_beta 96.212(8) _cell_angle_gamma 92.041(8) _cell_volume 1047.87(18) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3985 _cell_measurement_theta_min 3.7573 _cell_measurement_theta_max 66.9917 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_T_min 0.8342 _exptl_absorpt_correction_T_max 0.8708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.5058 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9977 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 67.10 _reflns_number_total 3713 _reflns_number_gt 3145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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^)+(0.0694P)^2^+0.1754P] 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 3713 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 C1 C -0.2254(3) -0.19914(18) -0.01652(6) 0.0362(3) Uani 1 1 d . . . H1 H -0.0800 -0.1735 0.0063 0.043 Uiso 1 1 calc R . . C2 C -0.3636(2) -0.34779(15) -0.00581(5) 0.0248(3) Uani 1 1 d . . . C3 C -0.2864(2) -0.46162(15) 0.03678(5) 0.0236(3) Uani 1 1 d . . . C4 C -0.4200(2) -0.61443(15) 0.04198(5) 0.0236(3) Uani 1 1 d . . . C5 C -0.3504(2) -0.73139(16) 0.08524(5) 0.0295(3) Uani 1 1 d . . . H5 H -0.2064 -0.7094 0.1090 0.035 Uiso 1 1 calc R . . C6 C -0.4859(3) -0.87309(18) 0.09305(6) 0.0375(3) Uani 1 1 d . . . H6 H -0.4349 -0.9498 0.1216 0.045 Uiso 1 1 calc R . . C7 C -0.7023(3) -0.90653(19) 0.05878(6) 0.0440(4) Uani 1 1 d . . . H7 H -0.7986 -1.0039 0.0653 0.053 Uiso 1 1 calc R . . C8 C -0.0718(2) -0.42294(16) 0.07711(5) 0.0252(3) Uani 1 1 d . . . H8 H 0.0481 -0.5044 0.0793 0.030 Uiso 1 1 calc R . . C9 C -0.0362(2) -0.28076(15) 0.11057(5) 0.0242(3) Uani 1 1 d . . . H9 H -0.1533 -0.1976 0.1056 0.029 Uiso 1 1 calc R . . C10 C 0.1627(2) -0.23805(15) 0.15414(5) 0.0231(3) Uani 1 1 d . . . C11 C 0.3668(2) -0.33331(16) 0.16104(5) 0.0260(3) Uani 1 1 d . . . H11 H 0.3828 -0.4280 0.1356 0.031 Uiso 1 1 calc R . . C12 C 0.5450(2) -0.29191(16) 0.20420(5) 0.0275(3) Uani 1 1 d . . . H12 H 0.6814 -0.3586 0.2081 0.033 Uiso 1 1 calc R . . C13 C 0.5268(2) -0.15303(16) 0.24220(5) 0.0245(3) Uani 1 1 d . . . C14 C 0.3300(2) -0.05374(16) 0.23546(5) 0.0262(3) Uani 1 1 d . . . H14 H 0.3171 0.0430 0.2603 0.031 Uiso 1 1 calc R . . C15 C 0.1516(2) -0.09749(15) 0.19186(5) 0.0261(3) Uani 1 1 d . . . H15 H 0.0169 -0.0291 0.1876 0.031 Uiso 1 1 calc R . . C16 C 0.7012(2) 0.01320(16) 0.32498(5) 0.0265(3) Uani 1 1 d . . . H16A H 0.5613 -0.0031 0.3459 0.032 Uiso 1 1 calc R . . H16B H 0.6899 0.1234 0.3058 0.032 Uiso 1 1 calc R . . C17 C 0.9255(2) 0.01311(16) 0.36556(5) 0.0264(3) Uani 1 1 d . . . H17A H 1.0628 0.0273 0.3437 0.032 Uiso 1 1 calc R . . H17B H 0.9355 -0.0994 0.3833 0.032 Uiso 1 1 calc R . . C18 C 0.9409(2) 0.15377(16) 0.41249(5) 0.0260(3) Uani 1 1 d . . . H18A H 0.9313 0.2665 0.3949 0.031 Uiso 1 1 calc R . . H18B H 0.8045 0.1396 0.4347 0.031 Uiso 1 1 calc R . . C19 C 1.1690(2) 0.15084(16) 0.45261(5) 0.0259(3) Uani 1 1 d . . . H19A H 1.3045 0.1666 0.4302 0.031 Uiso 1 1 calc R . . H19B H 1.1795 0.0367 0.4692 0.031 Uiso 1 1 calc R . . C20 C 1.1904(2) 0.28723(16) 0.50101(5) 0.0263(3) Uani 1 1 d . . . H20A H 1.0544 0.2726 0.5233 0.032 Uiso 1 1 calc R . . H20B H 1.1827 0.4017 0.4846 0.032 Uiso 1 1 calc R . . C21 C 1.4189(2) 0.27990(16) 0.54092(5) 0.0261(3) Uani 1 1 d . . . H21A H 1.4275 0.1645 0.5566 0.031 Uiso 1 1 calc R . . H21B H 1.5544 0.2960 0.5185 0.031 Uiso 1 1 calc R . . C22 C 1.4436(2) 0.41317(16) 0.59031(5) 0.0267(3) Uani 1 1 d . . . H22A H 1.4374 0.5289 0.5748 0.032 Uiso 1 1 calc R . . H22B H 1.3081 0.3980 0.6127 0.032 Uiso 1 1 calc R . . C23 C 1.6721(2) 0.40151(16) 0.62963(5) 0.0271(3) Uani 1 1 d . . . H23A H 1.8066 0.4113 0.6066 0.032 Uiso 1 1 calc R . . H23B H 1.6746 0.2869 0.6460 0.032 Uiso 1 1 calc R . . C24 C 1.7092(2) 0.53642(16) 0.67830(5) 0.0271(3) Uani 1 1 d . . . H24A H 1.7143 0.6514 0.6623 0.033 Uiso 1 1 calc R . . H24B H 1.5733 0.5297 0.7009 0.033 Uiso 1 1 calc R . . C25 C 1.9359(2) 0.51433(17) 0.71729(6) 0.0314(3) Uani 1 1 d . . . H25A H 1.9273 0.4009 0.7343 0.038 Uiso 1 1 calc R . . H25B H 2.0704 0.5154 0.6941 0.038 Uiso 1 1 calc R . . C26 C 1.9847(3) 0.65114(18) 0.76503(6) 0.0373(3) Uani 1 1 d . . . H26A H 2.0029 0.7635 0.7487 0.056 Uiso 1 1 calc R . . H26B H 2.1302 0.6264 0.7888 0.056 Uiso 1 1 calc R . . H26C H 1.8526 0.6516 0.7883 0.056 Uiso 1 1 calc R . . O1 O 0.71194(15) -0.12487(12) 0.28406(4) 0.0306(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0383(7) 0.0419(7) 0.0265(7) 0.0055(6) -0.0017(5) -0.0138(6) C2 0.0261(6) 0.0305(6) 0.0181(6) -0.0007(5) 0.0056(5) -0.0015(5) C3 0.0230(6) 0.0303(6) 0.0177(6) -0.0025(5) 0.0057(4) -0.0003(5) C4 0.0244(6) 0.0288(6) 0.0181(6) -0.0011(5) 0.0057(4) 0.0009(5) C5 0.0311(7) 0.0341(7) 0.0227(6) 0.0017(5) 0.0008(5) 0.0004(5) C6 0.0476(8) 0.0361(7) 0.0278(7) 0.0096(6) -0.0011(6) -0.0033(6) C7 0.0543(9) 0.0419(8) 0.0333(8) 0.0124(6) -0.0041(6) -0.0197(7) C8 0.0228(6) 0.0321(6) 0.0211(6) 0.0022(5) 0.0039(5) 0.0007(5) C9 0.0221(6) 0.0303(6) 0.0207(6) 0.0050(5) 0.0034(5) 0.0004(5) C10 0.0235(6) 0.0279(6) 0.0187(6) 0.0047(5) 0.0054(5) -0.0014(5) C11 0.0262(6) 0.0300(6) 0.0222(6) -0.0017(5) 0.0053(5) 0.0018(5) C12 0.0238(6) 0.0343(7) 0.0250(6) -0.0002(5) 0.0038(5) 0.0056(5) C13 0.0217(6) 0.0332(6) 0.0185(6) 0.0019(5) 0.0025(4) 0.0001(5) C14 0.0272(6) 0.0288(6) 0.0224(6) -0.0021(5) 0.0028(5) 0.0030(5) C15 0.0245(6) 0.0291(6) 0.0251(6) 0.0023(5) 0.0028(5) 0.0038(5) C16 0.0257(6) 0.0328(7) 0.0209(6) -0.0013(5) 0.0024(5) 0.0028(5) C17 0.0240(6) 0.0329(7) 0.0224(6) 0.0005(5) 0.0022(5) 0.0024(5) C18 0.0241(6) 0.0314(6) 0.0225(6) 0.0010(5) 0.0016(5) 0.0031(5) C19 0.0252(6) 0.0308(6) 0.0219(6) 0.0011(5) 0.0022(5) 0.0030(5) C20 0.0255(6) 0.0303(7) 0.0232(6) 0.0006(5) 0.0028(5) 0.0033(5) C21 0.0253(6) 0.0309(7) 0.0220(6) 0.0001(5) 0.0017(5) 0.0038(5) C22 0.0262(6) 0.0311(7) 0.0228(6) -0.0003(5) 0.0024(5) 0.0037(5) C23 0.0275(7) 0.0307(6) 0.0230(6) 0.0013(5) 0.0019(5) 0.0037(5) C24 0.0293(7) 0.0298(6) 0.0224(6) 0.0022(5) 0.0026(5) 0.0032(5) C25 0.0349(7) 0.0316(7) 0.0265(7) 0.0014(5) -0.0032(5) 0.0059(5) C26 0.0454(8) 0.0355(7) 0.0288(7) -0.0021(6) -0.0065(6) 0.0054(6) O1 0.0249(5) 0.0408(5) 0.0247(5) -0.0070(4) -0.0028(3) 0.0071(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 C1 C7 1.361(2) 2_445 ? C1 C2 1.4273(18) . ? C1 H1 0.9500 . ? C2 C3 1.4153(17) . ? C2 C4 1.4385(17) 2_445 ? C3 C4 1.4110(17) . ? C3 C8 1.4825(17) . ? C4 C5 1.4325(17) . ? C4 C2 1.4385(17) 2_445 ? C5 C6 1.3583(19) . ? C5 H5 0.9500 . ? C6 C7 1.412(2) . ? C6 H6 0.9500 . ? C7 C1 1.361(2) 2_445 ? C7 H7 0.9500 . ? C8 C9 1.3371(17) . ? C8 H8 0.9500 . ? C9 C10 1.4677(17) . ? C9 H9 0.9500 . ? C10 C15 1.3975(17) . ? C10 C11 1.4021(17) . ? C11 C12 1.3810(17) . ? C11 H11 0.9500 . ? C12 C13 1.3978(17) . ? C12 H12 0.9500 . ? C13 O1 1.3728(15) . ? C13 C14 1.3857(17) . ? C14 C15 1.3922(17) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 O1 1.4305(15) . ? C16 C17 1.5139(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.5269(17) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.5263(17) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.5275(17) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.5283(17) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.5279(17) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.5245(17) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.5246(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.5238(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.5226(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 C1 C2 121.35(13) 2_445 . ? C7 C1 H1 119.3 2_445 . ? C2 C1 H1 119.3 . . ? C3 C2 C1 121.81(11) . . ? C3 C2 C4 120.06(11) . 2_445 ? C1 C2 C4 118.04(11) . 2_445 ? C4 C3 C2 119.23(11) . . ? C4 C3 C8 118.91(11) . . ? C2 C3 C8 121.84(11) . . ? C3 C4 C5 120.96(11) . . ? C3 C4 C2 120.68(11) . 2_445 ? C5 C4 C2 118.28(11) . 2_445 ? C6 C5 C4 121.45(12) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 120.09(12) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C1 C7 C6 120.73(12) 2_445 . ? C1 C7 H7 119.6 2_445 . ? C6 C7 H7 119.6 . . ? C9 C8 C3 124.23(11) . . ? C9 C8 H8 117.9 . . ? C3 C8 H8 117.9 . . ? C8 C9 C10 127.61(11) . . ? C8 C9 H9 116.2 . . ? C10 C9 H9 116.2 . . ? C15 C10 C11 116.93(11) . . ? C15 C10 C9 119.68(10) . . ? C11 C10 C9 123.39(11) . . ? C12 C11 C10 121.15(11) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.74(11) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? O1 C13 C14 124.63(11) . . ? O1 C13 C12 115.99(10) . . ? C14 C13 C12 119.38(11) . . ? C13 C14 C15 119.17(11) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C10 122.60(11) . . ? C14 C15 H15 118.7 . . ? C10 C15 H15 118.7 . . ? O1 C16 C17 107.05(9) . . ? O1 C16 H16A 110.3 . . ? C17 C16 H16A 110.3 . . ? O1 C16 H16B 110.3 . . ? C17 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C16 C17 C18 113.59(10) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C19 C18 C17 112.42(10) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 114.37(10) . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C19 C20 C21 113.24(10) . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 114.42(10) . . ? C22 C21 H21A 108.7 . . ? C20 C21 H21A 108.7 . . ? C22 C21 H21B 108.7 . . ? C20 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C21 113.16(10) . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? C22 C23 C24 115.10(10) . . ? C22 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? C22 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C23 112.66(10) . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C24 114.27(11) . . ? C26 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C13 O1 C16 118.60(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C1 C2 C3 177.86(13) 2_445 . . . ? C7 C1 C2 C4 1.5(2) 2_445 . . 2_445 ? C1 C2 C3 C4 -174.28(11) . . . . ? C4 C2 C3 C4 2.05(18) 2_445 . . . ? C1 C2 C3 C8 7.23(18) . . . . ? C4 C2 C3 C8 -176.45(10) 2_445 . . . ? C2 C3 C4 C5 -178.76(11) . . . . ? C8 C3 C4 C5 -0.23(16) . . . . ? C2 C3 C4 C2 -2.06(18) . . . 2_445 ? C8 C3 C4 C2 176.48(10) . . . 2_445 ? C3 C4 C5 C6 175.57(12) . . . . ? C2 C4 C5 C6 -1.21(18) 2_445 . . . ? C4 C5 C6 C7 -1.0(2) . . . . ? C5 C6 C7 C1 2.0(2) . . . 2_445 ? C4 C3 C8 C9 -122.90(13) . . . . ? C2 C3 C8 C9 55.60(16) . . . . ? C3 C8 C9 C10 175.56(10) . . . . ? C8 C9 C10 C15 -168.96(12) . . . . ? C8 C9 C10 C11 10.00(19) . . . . ? C15 C10 C11 C12 1.67(17) . . . . ? C9 C10 C11 C12 -177.32(11) . . . . ? C10 C11 C12 C13 -0.20(18) . . . . ? C11 C12 C13 O1 178.94(10) . . . . ? C11 C12 C13 C14 -1.56(18) . . . . ? O1 C13 C14 C15 -178.79(11) . . . . ? C12 C13 C14 C15 1.76(18) . . . . ? C13 C14 C15 C10 -0.24(18) . . . . ? C11 C10 C15 C14 -1.46(17) . . . . ? C9 C10 C15 C14 177.56(10) . . . . ? O1 C16 C17 C18 -179.69(9) . . . . ? C16 C17 C18 C19 -179.85(10) . . . . ? C17 C18 C19 C20 -178.89(10) . . . . ? C18 C19 C20 C21 179.29(10) . . . . ? C19 C20 C21 C22 -179.10(10) . . . . ? C20 C21 C22 C23 179.47(10) . . . . ? C21 C22 C23 C24 177.73(10) . . . . ? C22 C23 C24 C25 177.95(10) . . . . ? C23 C24 C25 C26 177.55(11) . . . . ? C14 C13 O1 C16 1.85(17) . . . . ? C12 C13 O1 C16 -178.69(10) . . . . ? C17 C16 O1 C13 179.70(9) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 67.10 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.196 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.042 data_03216a _database_code_depnum_ccdc_archive 'CCDC 886646' #TrackingRef 'web_deposit_cif_file_5_ZhenguoChi_1339763597.DSA12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H70 O2' _chemical_formula_sum 'C54 H70 O2' _chemical_formula_weight 751.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4356(9) _cell_length_b 7.4034(14) _cell_length_c 27.665(3) _cell_angle_alpha 86.595(11) _cell_angle_beta 84.863(10) _cell_angle_gamma 89.167(14) _cell_volume 1106.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2762 _cell_measurement_theta_min 3.2106 _cell_measurement_theta_max 66.9139 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 0.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8220 _exptl_absorpt_correction_T_max 0.8530 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.01(10) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.5058 _diffrn_reflns_number 10165 _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 67.02 _reflns_number_total 3908 _reflns_number_gt 3127 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) ; _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^)+(0.0806P)^2^+0.1124P] 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 3908 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 C1 C 0.4760(2) 1.34693(17) 0.03363(5) 0.0237(3) Uani 1 1 d . . . C2 C 0.6456(2) 1.48422(17) 0.03981(5) 0.0238(3) Uani 1 1 d . . . C3 C 0.7986(3) 1.47393(18) 0.07912(5) 0.0277(3) Uani 1 1 d . . . H3 H 0.7819 1.3741 0.1024 0.033 Uiso 1 1 calc R . . C4 C 0.9677(3) 1.60309(19) 0.08422(5) 0.0305(3) Uani 1 1 d . . . H4 H 1.0683 1.5921 0.1106 0.037 Uiso 1 1 calc R . . C5 C 0.9948(3) 1.75366(19) 0.05048(5) 0.0310(3) Uani 1 1 d . . . H5 H 1.1146 1.8430 0.0540 0.037 Uiso 1 1 calc R . . C6 C 0.8502(3) 1.77101(18) 0.01296(5) 0.0279(3) Uani 1 1 d . . . H6 H 0.8689 1.8740 -0.0092 0.033 Uiso 1 1 calc R . . C7 C 0.6701(2) 1.63835(17) 0.00582(5) 0.0241(3) Uani 1 1 d . . . C8 C 0.4607(3) 1.18323(18) 0.06756(5) 0.0291(3) Uani 1 1 d . . . H8 H 0.5731 1.0872 0.0602 0.035 Uiso 1 1 calc R . . C9 C 0.3081(3) 1.15878(19) 0.10641(5) 0.0295(3) Uani 1 1 d . . . H9 H 0.1982 1.2565 0.1136 0.035 Uiso 1 1 calc R . . C10 C 0.2848(2) 0.99850(18) 0.14051(5) 0.0250(3) Uani 1 1 d . . . C11 C 0.4610(2) 0.85986(18) 0.14070(5) 0.0263(3) Uani 1 1 d . . . H11 H 0.6045 0.8700 0.1185 0.032 Uiso 1 1 calc R . . C12 C 0.4332(3) 0.70799(18) 0.17223(5) 0.0269(3) Uani 1 1 d . . . H12 H 0.5569 0.6160 0.1718 0.032 Uiso 1 1 calc R . . C13 C 0.2225(2) 0.69101(18) 0.20467(5) 0.0239(3) Uani 1 1 d . . . C14 C 0.0445(2) 0.82867(19) 0.20546(5) 0.0274(3) Uani 1 1 d . . . H14 H -0.0988 0.8184 0.2277 0.033 Uiso 1 1 calc R . . C15 C 0.0763(3) 0.97948(19) 0.17398(5) 0.0287(3) Uani 1 1 d . . . H15 H -0.0459 1.0726 0.1750 0.034 Uiso 1 1 calc R . . C16 C 0.3502(3) 0.39865(18) 0.23578(5) 0.0279(3) Uani 1 1 d . . . H16A H 0.5137 0.4420 0.2430 0.033 Uiso 1 1 calc R . . H16B H 0.3676 0.3489 0.2032 0.033 Uiso 1 1 calc R . . C17 C 0.2582(3) 0.25440(18) 0.27362(5) 0.0288(3) Uani 1 1 d . . . H17A H 0.0962 0.2105 0.2657 0.035 Uiso 1 1 calc R . . H17B H 0.2344 0.3071 0.3058 0.035 Uiso 1 1 calc R . . C18 C 0.4398(3) 0.09532(18) 0.27604(5) 0.0281(3) Uani 1 1 d . . . H18A H 0.4598 0.0415 0.2440 0.034 Uiso 1 1 calc R . . H18B H 0.6030 0.1407 0.2828 0.034 Uiso 1 1 calc R . . C19 C 0.3570(3) -0.05098(18) 0.31486(5) 0.0273(3) Uani 1 1 d . . . H19A H 0.1955 -0.0981 0.3077 0.033 Uiso 1 1 calc R . . H19B H 0.3337 0.0034 0.3468 0.033 Uiso 1 1 calc R . . C20 C 0.5407(3) -0.20785(18) 0.31795(5) 0.0282(3) Uani 1 1 d . . . H20A H 0.5609 -0.2631 0.2861 0.034 Uiso 1 1 calc R . . H20B H 0.7031 -0.1594 0.3241 0.034 Uiso 1 1 calc R . . C21 C 0.4672(3) -0.35482(18) 0.35715(5) 0.0283(3) Uani 1 1 d . . . H21A H 0.3081 -0.4072 0.3505 0.034 Uiso 1 1 calc R . . H21B H 0.4425 -0.2999 0.3890 0.034 Uiso 1 1 calc R . . C22 C 0.6601(3) -0.50581(19) 0.35997(5) 0.0289(3) Uani 1 1 d . . . H22A H 0.6869 -0.5581 0.3278 0.035 Uiso 1 1 calc R . . H22B H 0.8182 -0.4529 0.3671 0.035 Uiso 1 1 calc R . . C23 C 0.5915(3) -0.65729(19) 0.39814(5) 0.0289(3) Uani 1 1 d . . . H23A H 0.4334 -0.7106 0.3912 0.035 Uiso 1 1 calc R . . H23B H 0.5661 -0.6058 0.4305 0.035 Uiso 1 1 calc R . . C24 C 0.7874(3) -0.80634(19) 0.39980(5) 0.0303(3) Uani 1 1 d . . . H24A H 0.8125 -0.8571 0.3674 0.036 Uiso 1 1 calc R . . H24B H 0.9453 -0.7523 0.4066 0.036 Uiso 1 1 calc R . . C25 C 0.7241(3) -0.95974(19) 0.43770(5) 0.0299(3) Uani 1 1 d . . . H25A H 0.5632 -1.0113 0.4318 0.036 Uiso 1 1 calc R . . H25B H 0.7061 -0.9104 0.4703 0.036 Uiso 1 1 calc R . . C26 C 0.9181(3) -1.1102(2) 0.43720(6) 0.0354(4) Uani 1 1 d . . . H26A H 0.9377 -1.1580 0.4044 0.043 Uiso 1 1 calc R . . H26B H 1.0784 -1.0586 0.4435 0.043 Uiso 1 1 calc R . . C27 C 0.8558(4) -1.2657(2) 0.47443(6) 0.0466(4) Uani 1 1 d . . . H27A H 0.8444 -1.2209 0.5072 0.070 Uiso 1 1 calc R . . H27B H 0.9856 -1.3587 0.4716 0.070 Uiso 1 1 calc R . . H27C H 0.6974 -1.3179 0.4685 0.070 Uiso 1 1 calc R . . O1 O 0.17405(18) 0.54536(13) 0.23676(4) 0.0307(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0260(6) 0.0227(6) 0.0212(7) 0.0007(5) 0.0036(5) -0.0009(5) C2 0.0248(7) 0.0241(6) 0.0219(7) -0.0008(5) 0.0007(5) 0.0010(5) C3 0.0312(7) 0.0273(7) 0.0241(7) 0.0005(5) -0.0015(5) 0.0025(6) C4 0.0300(7) 0.0353(8) 0.0276(8) -0.0054(6) -0.0080(6) 0.0020(6) C5 0.0301(7) 0.0306(7) 0.0331(8) -0.0063(6) -0.0033(6) -0.0058(6) C6 0.0303(7) 0.0244(6) 0.0283(7) 0.0002(5) 0.0004(5) -0.0045(5) C7 0.0251(7) 0.0242(6) 0.0223(7) -0.0014(5) 0.0010(5) -0.0008(5) C8 0.0339(7) 0.0247(7) 0.0275(8) 0.0039(6) 0.0004(6) 0.0016(6) C9 0.0284(7) 0.0290(7) 0.0295(8) 0.0071(6) 0.0000(6) 0.0033(6) C10 0.0251(6) 0.0276(7) 0.0223(7) 0.0039(5) -0.0044(5) -0.0044(5) C11 0.0237(6) 0.0313(7) 0.0228(7) 0.0045(5) 0.0004(5) -0.0034(5) C12 0.0274(7) 0.0272(7) 0.0260(7) 0.0028(5) -0.0039(5) -0.0002(5) C13 0.0269(7) 0.0252(7) 0.0199(7) 0.0032(5) -0.0057(5) -0.0057(5) C14 0.0254(7) 0.0320(7) 0.0235(7) 0.0043(5) 0.0009(5) -0.0029(6) C15 0.0263(7) 0.0311(7) 0.0277(7) 0.0050(6) -0.0022(5) 0.0028(5) C16 0.0313(7) 0.0255(7) 0.0266(7) 0.0034(6) -0.0033(6) -0.0023(6) C17 0.0334(7) 0.0264(7) 0.0260(7) 0.0046(6) -0.0031(6) -0.0044(6) C18 0.0304(7) 0.0270(7) 0.0265(7) 0.0036(6) -0.0032(6) -0.0051(6) C19 0.0301(7) 0.0258(7) 0.0255(7) 0.0037(6) -0.0027(5) -0.0029(6) C20 0.0290(7) 0.0269(7) 0.0282(8) 0.0025(6) -0.0022(5) -0.0041(6) C21 0.0296(7) 0.0260(7) 0.0285(8) 0.0032(6) -0.0017(6) -0.0033(6) C22 0.0287(7) 0.0275(7) 0.0301(8) 0.0026(6) -0.0028(6) -0.0027(6) C23 0.0293(7) 0.0277(7) 0.0293(8) 0.0037(6) -0.0032(6) -0.0027(6) C24 0.0296(7) 0.0298(7) 0.0312(8) 0.0038(6) -0.0051(6) -0.0023(6) C25 0.0311(7) 0.0293(7) 0.0289(8) 0.0040(6) -0.0046(6) -0.0031(6) C26 0.0403(8) 0.0314(8) 0.0343(9) 0.0041(6) -0.0057(6) 0.0014(6) C27 0.0629(11) 0.0344(9) 0.0422(10) 0.0086(7) -0.0109(8) 0.0019(8) O1 0.0341(5) 0.0267(5) 0.0291(6) 0.0107(4) 0.0015(4) -0.0021(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 C1 C7 1.404(2) 2_685 ? C1 C2 1.4102(19) . ? C1 C8 1.4867(17) . ? C2 C3 1.425(2) . ? C2 C7 1.4349(18) . ? C3 C4 1.358(2) . ? C3 H3 0.9500 . ? C4 C5 1.412(2) . ? C4 H4 0.9500 . ? C5 C6 1.356(2) . ? C5 H5 0.9500 . ? C6 C7 1.4307(19) . ? C6 H6 0.9500 . ? C7 C1 1.404(2) 2_685 ? C8 C9 1.303(2) . ? C8 H8 0.9500 . ? C9 C10 1.4711(17) . ? C9 H9 0.9500 . ? C10 C11 1.3935(19) . ? C10 C15 1.401(2) . ? C11 C12 1.3830(18) . ? C11 H11 0.9500 . ? C12 C13 1.393(2) . ? C12 H12 0.9500 . ? C13 O1 1.3685(15) . ? C13 C14 1.395(2) . ? C14 C15 1.3777(19) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 O1 1.4375(17) . ? C16 C17 1.5086(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.528(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.5228(18) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.5241(19) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.5214(18) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.5246(19) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.5208(18) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.524(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.5209(18) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.523(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.520(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 C1 C2 119.84(12) 2_685 . ? C7 C1 C8 120.21(12) 2_685 . ? C2 C1 C8 119.89(12) . . ? C1 C2 C3 121.63(12) . . ? C1 C2 C7 120.22(12) . . ? C3 C2 C7 118.14(12) . . ? C4 C3 C2 121.70(12) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 120.33(13) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.10(13) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 121.77(12) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C1 C7 C6 122.10(12) 2_685 . ? C1 C7 C2 119.94(12) 2_685 . ? C6 C7 C2 117.94(12) . . ? C9 C8 C1 126.28(13) . . ? C9 C8 H8 116.9 . . ? C1 C8 H8 116.9 . . ? C8 C9 C10 127.99(13) . . ? C8 C9 H9 116.0 . . ? C10 C9 H9 116.0 . . ? C11 C10 C15 117.40(11) . . ? C11 C10 C9 122.80(12) . . ? C15 C10 C9 119.79(12) . . ? C12 C11 C10 122.02(12) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C11 C12 C13 119.48(12) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? O1 C13 C12 124.36(12) . . ? O1 C13 C14 116.07(12) . . ? C12 C13 C14 119.56(12) . . ? C15 C14 C13 120.09(12) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C10 121.43(13) . . ? C14 C15 H15 119.3 . . ? C10 C15 H15 119.3 . . ? O1 C16 C17 108.00(11) . . ? O1 C16 H16A 110.1 . . ? C17 C16 H16A 110.1 . . ? O1 C16 H16B 110.1 . . ? C17 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? C16 C17 C18 111.34(12) . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C19 C18 C17 112.96(11) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 112.94(11) . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 114.51(11) . . ? C21 C20 H20A 108.6 . . ? C19 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? C19 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 112.68(11) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C21 114.34(11) . . ? C23 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? C23 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C22 C23 C24 112.98(11) . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 114.19(12) . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C26 113.05(12) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 113.68(13) . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26B 108.8 . . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C13 O1 C16 117.40(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C1 C2 C3 -179.53(13) 2_685 . . . ? C8 C1 C2 C3 -2.4(2) . . . . ? C7 C1 C2 C7 -0.3(2) 2_685 . . . ? C8 C1 C2 C7 176.89(12) . . . . ? C1 C2 C3 C4 177.82(13) . . . . ? C7 C2 C3 C4 -1.4(2) . . . . ? C2 C3 C4 C5 0.6(2) . . . . ? C3 C4 C5 C6 0.6(2) . . . . ? C4 C5 C6 C7 -1.0(2) . . . . ? C5 C6 C7 C1 -178.36(14) . . . 2_685 ? C5 C6 C7 C2 0.1(2) . . . . ? C1 C2 C7 C1 0.3(2) . . . 2_685 ? C3 C2 C7 C1 179.55(12) . . . 2_685 ? C1 C2 C7 C6 -178.17(12) . . . . ? C3 C2 C7 C6 1.09(19) . . . . ? C7 C1 C8 C9 -88.41(19) 2_685 . . . ? C2 C1 C8 C9 94.42(18) . . . . ? C1 C8 C9 C10 179.16(13) . . . . ? C8 C9 C10 C11 12.9(2) . . . . ? C8 C9 C10 C15 -165.82(15) . . . . ? C15 C10 C11 C12 0.4(2) . . . . ? C9 C10 C11 C12 -178.37(12) . . . . ? C10 C11 C12 C13 0.5(2) . . . . ? C11 C12 C13 O1 178.75(12) . . . . ? C11 C12 C13 C14 -1.0(2) . . . . ? O1 C13 C14 C15 -179.19(12) . . . . ? C12 C13 C14 C15 0.6(2) . . . . ? C13 C14 C15 C10 0.3(2) . . . . ? C11 C10 C15 C14 -0.8(2) . . . . ? C9 C10 C15 C14 177.98(13) . . . . ? O1 C16 C17 C18 -178.21(10) . . . . ? C16 C17 C18 C19 178.36(11) . . . . ? C17 C18 C19 C20 -178.86(11) . . . . ? C18 C19 C20 C21 178.64(11) . . . . ? C19 C20 C21 C22 -178.18(11) . . . . ? C20 C21 C22 C23 -178.96(11) . . . . ? C21 C22 C23 C24 179.68(11) . . . . ? C22 C23 C24 C25 179.93(11) . . . . ? C23 C24 C25 C26 177.73(12) . . . . ? C24 C25 C26 C27 -179.22(12) . . . . ? C12 C13 O1 C16 -1.72(19) . . . . ? C14 C13 O1 C16 178.09(11) . . . . ? C17 C16 O1 C13 -179.61(10) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 67.02 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.202 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.043