# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- CC-BMpillar-S2-new2.cif' _journal_year ? _journal_page_first ? _publ_contact_author_name 'Feihe Huang' _publ_contact_author_address ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; _publ_contact_author_email fhuang@zju.edu.cn _publ_contact_author_fax 86-571-87953189 _publ_contact_author_phone 86-571-87953189 _publ_section_title ; Four Structural isomers of BMpillar[5]arene: Synthesis, Crystal Structures and Complexation with N-Octyltrimethyl Ammonium Hexafluorophosphate ; loop_ _publ_author_name _publ_author_address 'Zibin Zhang' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Yan Luo' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Binyuan Xia' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Chengyou Han' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Yihua Yu' ; Shanghai Key Laboratory of Magnetic Resonance Department of Physics East China Normal University Shanghai 200062, P. R. China ; ; Xiaopeng Chen ; ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; 'Feihe Huang' ; Department of Chemistry Zhejiang University Hangzhou 310027, P. R. China ; data_EMpillar[5]arene _database_code_depnum_ccdc_archive 'CCDC 782492' #TrackingRef '- CC-BMpillar-S2-new2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C50 H60 O10), 3(C2 H3 N)' _chemical_formula_sum 'C106 H129 N3 O20' _chemical_formula_weight 1765.12 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' N N 0.0311 0.0180 '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 12.2072(4) _cell_length_b 20.6545(12) _cell_length_c 21.4041(11) _cell_angle_alpha 68.825(5) _cell_angle_beta 88.866(4) _cell_angle_gamma 80.174(4) _cell_volume 4953.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8248 _cell_measurement_theta_min 2.5668 _cell_measurement_theta_max 66.9368 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.53 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31785 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 65.08 _reflns_number_total 16706 _reflns_number_gt 9165 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16706 _refine_ls_number_parameters 1130 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1500 _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.3248 _refine_ls_wR_factor_gt 0.2895 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.4547(4) 0.6343(3) 0.5593(3) 0.1140(17) Uani 1 1 d . . . O2 O 0.7098(4) 0.7776(2) 0.6566(3) 0.1124(17) Uani 1 1 d . . . O3 O 0.8176(4) 0.6201(2) 0.8897(2) 0.0976(13) Uani 1 1 d . . . O4 O 1.0588(4) 0.3832(2) 0.9162(2) 0.0978(13) Uani 1 1 d . . . O5 O 1.0905(3) 0.39517(19) 0.67743(18) 0.0712(9) Uani 1 1 d . . . O6 O 0.6859(3) 0.3954(2) 0.60027(19) 0.0829(11) Uani 1 1 d . . . O7 O 0.3937(3) 0.6402(2) 0.7936(2) 0.0911(12) Uani 1 1 d . . . O8 O 0.8921(3) 0.6302(2) 0.5213(2) 0.0851(11) Uani 1 1 d . . . O9 O 0.6070(4) 0.40450(19) 0.9526(2) 0.0814(11) Uani 1 1 d . . . O10 O 0.7988(3) 0.23997(17) 0.84097(16) 0.0686(9) Uani 1 1 d . . . O11 O 0.3758(3) 0.11900(19) 1.1025(3) 0.0988(15) Uani 1 1 d . . . O12 O 0.5124(3) -0.16316(17) 1.1846(2) 0.0761(10) Uani 1 1 d . . . O13 O 0.7596(3) -0.0017(2) 1.4835(2) 0.0834(11) Uani 1 1 d . . . O14 O 0.9430(3) 0.1650(2) 1.28013(19) 0.0779(10) Uani 1 1 d . . . O15 O 0.4306(3) -0.01468(18) 1.35504(19) 0.0708(9) Uani 1 1 d . . . O16 O 1.1245(2) -0.11877(18) 1.38377(16) 0.0639(8) Uani 1 1 d . . . O17 O 0.7588(3) -0.00940(16) 1.02148(18) 0.0709(9) Uani 1 1 d . . . O18 O 1.0979(3) 0.01663(17) 1.13392(16) 0.0624(8) Uani 1 1 d . . . O19 O 0.7549(3) -0.20947(16) 1.37928(18) 0.0657(9) Uani 1 1 d . . . O20 O 0.7217(2) 0.22348(15) 1.07084(14) 0.0542(7) Uani 1 1 d . . . C1 C 0.9315(4) 0.3422(2) 0.6897(2) 0.0536(10) Uani 1 1 d . . . C2 C 1.0195(4) 0.3564(2) 0.7202(2) 0.0556(11) Uani 1 1 d . . . C3 C 0.8579(4) 0.3033(2) 0.7293(2) 0.0533(10) Uani 1 1 d . . . H3 H 0.7996 0.2930 0.7093 0.064 Uiso 1 1 calc R . . C4 C 0.3316(6) 0.5856(3) 0.8247(4) 0.100(2) Uani 1 1 d . . . H4B H 0.2594 0.5978 0.8025 0.150 Uiso 1 1 calc R . . H4C H 0.3235 0.5800 0.8710 0.150 Uiso 1 1 calc R . . H4A H 0.3699 0.5423 0.8218 0.150 Uiso 1 1 calc R . . C5 C 0.9562(4) 0.2939(2) 0.8302(2) 0.0587(11) Uani 1 1 d . . . C6 C 0.8419(4) 0.5705(3) 0.5403(2) 0.0697(14) Uani 1 1 d . . . C7 C 0.8694(4) 0.2792(2) 0.7987(2) 0.0548(11) Uani 1 1 d . . . C8 C 1.2511(7) 0.4405(7) 0.6446(5) 0.175(5) Uani 1 1 d . . . H8B H 1.2005 0.4782 0.6128 0.263 Uiso 1 1 calc R . . H8A H 1.2837 0.4078 0.6242 0.263 Uiso 1 1 calc R . . H8C H 1.3087 0.4594 0.6586 0.263 Uiso 1 1 calc R . . C9 C 1.0313(4) 0.3321(2) 0.7900(2) 0.0585(11) Uani 1 1 d . . . H9 H 1.0904 0.3418 0.8100 0.070 Uiso 1 1 calc R . . C10 C 0.4436(9) 0.3707(4) 0.9535(5) 0.136(3) Uani 1 1 d D . . H10E H 0.4135 0.4151 0.9195 0.204 Uiso 1 1 calc R . . H10F H 0.4352 0.3743 0.9969 0.204 Uiso 1 1 calc R . . H10D H 0.4046 0.3350 0.9510 0.204 Uiso 1 1 calc R . . C11 C 0.8572(14) 0.8228(9) 0.6514(9) 0.246(7) Uiso 1 1 d D . . H11A H 0.9355 0.8160 0.6440 0.370 Uiso 1 1 calc R . . H11C H 0.8461 0.8072 0.6987 0.370 Uiso 1 1 calc R . . H11B H 0.8260 0.8720 0.6309 0.370 Uiso 1 1 calc R . . C12 C 1.0300(9) 0.6945(7) 0.5373(6) 0.174(5) Uani 1 1 d . . . H12A H 1.0724 0.7090 0.4979 0.261 Uiso 1 1 calc R . . H12C H 1.0735 0.6914 0.5755 0.261 Uiso 1 1 calc R . . H12B H 0.9631 0.7285 0.5318 0.261 Uiso 1 1 calc R . . C13 C 0.7697(6) 0.4516(3) 0.9483(2) 0.0731(15) Uani 1 1 d . . . C14 C 0.8101(7) 0.7878(5) 0.6259(5) 0.122(3) Uiso 1 1 d D . . H14A H 0.8572 0.7427 0.6328 0.146 Uiso 1 1 calc R . . H14B H 0.7967 0.8133 0.5780 0.146 Uiso 1 1 calc R . . C15 C 1.1125(7) 0.4390(5) 0.9177(4) 0.122(3) Uani 1 1 d . . . H15A H 1.0726 0.4833 0.8877 0.183 Uiso 1 1 calc R . . H15B H 1.1874 0.4320 0.9038 0.183 Uiso 1 1 calc R . . H15C H 1.1135 0.4392 0.9624 0.183 Uiso 1 1 calc R . . C16 C 0.8860(6) 0.6682(4) 0.8506(4) 0.100(2) Uani 1 1 d . . . H16B H 0.8514 0.7162 0.8442 0.120 Uiso 1 1 calc R . . H16A H 0.8948 0.6643 0.8069 0.120 Uiso 1 1 calc R . . C17 C 0.3434(7) 0.6260(6) 0.5803(7) 0.177(5) Uani 1 1 d . . . H17A H 0.3151 0.5973 0.5599 0.266 Uiso 1 1 calc R . . H17B H 0.2964 0.6714 0.5668 0.266 Uiso 1 1 calc R . . H17C H 0.3446 0.6036 0.6282 0.266 Uiso 1 1 calc R . . C18 C 0.9935(8) 0.6517(4) 0.8852(5) 0.133(3) Uani 1 1 d . . . H18B H 1.0389 0.6850 0.8601 0.200 Uiso 1 1 calc R . . H18A H 1.0290 0.6050 0.8893 0.200 Uiso 1 1 calc R . . H18C H 0.9840 0.6539 0.9290 0.200 Uiso 1 1 calc R . . C19 C 0.5125(5) 0.7462(3) 0.7208(4) 0.100(2) Uani 1 1 d . . . H19A H 0.4319 0.7554 0.7208 0.120 Uiso 1 1 calc R . . H19B H 0.5393 0.7886 0.7182 0.120 Uiso 1 1 calc R . . C20 C 0.7025(6) 0.5130(3) 0.9635(3) 0.0871(18) Uani 1 1 d . . . H20B H 0.7508 0.5306 0.9866 0.104 Uiso 1 1 calc R . . H20A H 0.6443 0.4960 0.9934 0.104 Uiso 1 1 calc R . . C21 C 1.0000(5) 0.6222(4) 0.5481(3) 0.0833(16) Uani 1 1 d . . . H21A H 1.0532 0.5975 0.5264 0.100 Uiso 1 1 calc R . . H21B H 1.0039 0.5943 0.5956 0.100 Uiso 1 1 calc R . . C22 C 0.6591(5) 0.6553(3) 0.5036(3) 0.0903(19) Uani 1 1 d . . . H22B H 0.7036 0.6869 0.4736 0.108 Uiso 1 1 calc R . . H22A H 0.5951 0.6547 0.4777 0.108 Uiso 1 1 calc R . . C23 C 1.1894(5) 0.4033(4) 0.7044(3) 0.0885(17) Uani 1 1 d . . . H23A H 1.2326 0.3578 0.7309 0.106 Uiso 1 1 calc R . . H23B H 1.1730 0.4312 0.7325 0.106 Uiso 1 1 calc R . . C24 C 0.4826(5) 0.6921(3) 0.6372(4) 0.094(2) Uani 1 1 d . . . H24 H 0.4149 0.6834 0.6562 0.113 Uiso 1 1 calc R . . C25 C 0.5481(5) 0.7275(3) 0.6614(3) 0.0880(19) Uani 1 1 d . . . C26 C 0.5673(5) 0.4050(4) 0.5989(3) 0.0910(18) Uani 1 1 d . . . H26A H 0.5385 0.4268 0.5532 0.137 Uiso 1 1 calc R . . H26C H 0.5391 0.4347 0.6234 0.137 Uiso 1 1 calc R . . H26B H 0.5443 0.3601 0.6191 0.137 Uiso 1 1 calc R . . C27 C 0.5162(5) 0.6699(3) 0.5856(4) 0.095(2) Uani 1 1 d . . . C28 C 0.5539(5) 0.3529(3) 0.9439(3) 0.0801(16) Uani 1 1 d D . . H28A H 0.5641 0.3521 0.8991 0.096 Uiso 1 1 calc R . . H28B H 0.5843 0.3066 0.9762 0.096 Uiso 1 1 calc R . . C29 C 0.8832(6) 0.4462(3) 0.9401(3) 0.0832(18) Uani 1 1 d . . . H29 H 0.9186 0.4812 0.9439 0.100 Uiso 1 1 calc R . . C30 C 0.9622(5) 0.2755(3) 0.9056(2) 0.0720(15) Uani 1 1 d . . . H30A H 0.9319 0.2328 0.9278 0.086 Uiso 1 1 calc R . . H30B H 1.0392 0.2669 0.9213 0.086 Uiso 1 1 calc R . . C31 C 0.6837(5) 0.7189(3) 0.5804(3) 0.0864(19) Uani 1 1 d . . . H31 H 0.7508 0.7284 0.5611 0.104 Uiso 1 1 calc R . . C32 C 0.9462(5) 0.3908(3) 0.9265(3) 0.0772(16) Uani 1 1 d . . . C33 C 0.7114(5) 0.6275(3) 0.8640(3) 0.0771(15) Uani 1 1 d . . . C34 C 0.6488(5) 0.7411(3) 0.6317(3) 0.089(2) Uani 1 1 d . . . C35 C 0.6200(5) 0.6824(3) 0.5572(3) 0.090(2) Uani 1 1 d . . . C36 C 0.5466(5) 0.5793(3) 0.8764(3) 0.0747(15) Uani 1 1 d . . . H36 H 0.5061 0.5443 0.8994 0.090 Uiso 1 1 calc R . . C37 C 0.7276(4) 0.5816(3) 0.5315(2) 0.0750(15) Uani 1 1 d . . . C38 C 0.6763(4) 0.5235(3) 0.5510(2) 0.0746(15) Uani 1 1 d . . . H38 H 0.5993 0.5301 0.5451 0.089 Uiso 1 1 calc R . . C39 C 0.9173(4) 0.3698(3) 0.6138(2) 0.0672(13) Uani 1 1 d . . . H39A H 0.8800 0.3385 0.6005 0.081 Uiso 1 1 calc R . . H39B H 0.9901 0.3694 0.5948 0.081 Uiso 1 1 calc R . . C40 C 0.7041(4) 0.2279(3) 0.8123(3) 0.0722(14) Uani 1 1 d . . . H40A H 0.7277 0.2010 0.7845 0.108 Uiso 1 1 calc R . . H40B H 0.6601 0.2723 0.7856 0.108 Uiso 1 1 calc R . . H40C H 0.6604 0.2023 0.8473 0.108 Uiso 1 1 calc R . . C41 C 0.6625(6) 0.6819(3) 0.8086(3) 0.0762(16) Uani 1 1 d . . . H41 H 0.7027 0.7174 0.7864 0.091 Uiso 1 1 calc R . . C42 C 0.8503(4) 0.4443(3) 0.5855(2) 0.0619(12) Uani 1 1 d . . . C43 C 0.7179(6) 0.3972(3) 0.9447(2) 0.0709(15) Uani 1 1 d . . . C44 C 0.7828(5) 0.3410(3) 0.9314(2) 0.0707(15) Uani 1 1 d . . . H44 H 0.7477 0.3057 0.9281 0.085 Uiso 1 1 calc R . . C45 C 0.5580(5) 0.6869(3) 0.7842(3) 0.0792(16) Uani 1 1 d . . . C46 C 0.6495(5) 0.5734(3) 0.9007(3) 0.0704(14) Uani 1 1 d . . . C47 C 0.9022(4) 0.5021(3) 0.5659(2) 0.0651(13) Uani 1 1 d . . . H47 H 0.9794 0.4954 0.5700 0.078 Uiso 1 1 calc R . . C48 C 0.7353(4) 0.4552(3) 0.5790(2) 0.0655(13) Uani 1 1 d . . . C49 C 0.8965(5) 0.3356(3) 0.9230(2) 0.0690(15) Uani 1 1 d . . . C50 C 0.4951(5) 0.6337(2) 0.8193(3) 0.0690(14) Uani 1 1 d . . . C51 C 0.8585(4) -0.0898(3) 1.44823(19) 0.0543(11) Uani 1 1 d . . . C52 C 0.7597(3) -0.1595(2) 1.4072(2) 0.0507(10) Uani 1 1 d . . . C53 C 1.0043(3) 0.0692(2) 1.1157(2) 0.0515(10) Uani 1 1 d . . . C54 C 0.6511(4) 0.0927(2) 1.0310(2) 0.0522(10) Uani 1 1 d . . . C55 C 0.6623(4) 0.0206(2) 1.0422(2) 0.0531(10) Uani 1 1 d . . . C56 C 1.0814(3) -0.0482(2) 1.3568(2) 0.0524(10) Uani 1 1 d . . . C57 C 0.9244(4) 0.0752(2) 1.0676(2) 0.0524(10) Uani 1 1 d . . . H57 H 0.9337 0.0433 1.0456 0.063 Uiso 1 1 calc R . . C58 C 1.0593(3) 0.0670(2) 1.2680(2) 0.0509(10) Uani 1 1 d . . . C59 C 0.8191(3) 0.1746(2) 1.0856(2) 0.0471(9) Uani 1 1 d . . . C60 C 0.9011(3) 0.1710(2) 1.1306(2) 0.0477(9) Uani 1 1 d . . . H60 H 0.8933 0.2044 1.1508 0.057 Uiso 1 1 calc R . . C61 C 0.8314(4) 0.1276(2) 1.05188(19) 0.0476(9) Uani 1 1 d . . . C62 C 0.5783(4) -0.0154(2) 1.0718(2) 0.0573(12) Uani 1 1 d . . . H62 H 0.5859 -0.0631 1.0785 0.069 Uiso 1 1 calc R . . C63 C 0.2688(17) 0.2285(6) 1.0582(8) 0.264(11) Uani 1 1 d D . . H63B H 0.2867 0.2670 1.0205 0.396 Uiso 1 1 calc R . . H63C H 0.2198 0.2465 1.0860 0.396 Uiso 1 1 calc R . . H63A H 0.2328 0.1989 1.0425 0.396 Uiso 1 1 calc R . . C64 C 0.9963(3) 0.1180(2) 1.1467(2) 0.0482(9) Uani 1 1 d . . . C65 C 1.2579(8) -0.2136(4) 1.3984(5) 0.137(3) Uani 1 1 d . . . H65A H 1.3106 -0.2379 1.3769 0.206 Uiso 1 1 calc R . . H65B H 1.1998 -0.2405 1.4154 0.206 Uiso 1 1 calc R . . H65C H 1.2950 -0.2079 1.4347 0.206 Uiso 1 1 calc R . . C66 C 0.8627(7) 0.1930(4) 1.3174(4) 0.122(3) Uani 1 1 d . . . H66B H 0.8498 0.2436 1.2980 0.184 Uiso 1 1 calc R . . H66C H 0.8902 0.1779 1.3631 0.184 Uiso 1 1 calc R . . H66A H 0.7943 0.1764 1.3162 0.184 Uiso 1 1 calc R . . C67 C 0.6953(6) 0.1137(5) 1.4823(4) 0.116(3) Uani 1 1 d . . . H67A H 0.7567 0.1284 1.4554 0.174 Uiso 1 1 calc R . . H67C H 0.7168 0.0997 1.5289 0.174 Uiso 1 1 calc R . . H67B H 0.6334 0.1520 1.4707 0.174 Uiso 1 1 calc R . . C68 C 0.8493(5) -0.2317(4) 1.3497(4) 0.0919(19) Uani 1 1 d . . . H68B H 0.8680 -0.1922 1.3133 0.138 Uiso 1 1 calc R . . H68A H 0.8346 -0.2668 1.3329 0.138 Uiso 1 1 calc R . . H68C H 0.9102 -0.2514 1.3824 0.138 Uiso 1 1 calc R . . C69 C 0.6116(7) -0.2438(4) 1.1413(4) 0.101(2) Uani 1 1 d . . . H69A H 0.6189 -0.2039 1.1019 0.152 Uiso 1 1 calc R . . H69B H 0.5478 -0.2629 1.1353 0.152 Uiso 1 1 calc R . . H69C H 0.6772 -0.2792 1.1488 0.152 Uiso 1 1 calc R . . C70 C 0.3624(7) 0.1907(5) 1.0938(10) 0.225(9) Uani 1 1 d D . . H70B H 0.3610 0.1950 1.1375 0.270 Uiso 1 1 calc R . . H70A H 0.4257 0.2098 1.0711 0.270 Uiso 1 1 calc R . . C71 C 0.5973(6) -0.2214(3) 1.2005(3) 0.0925(18) Uani 1 1 d . . . H71B H 0.5787 -0.2596 1.2392 0.111 Uiso 1 1 calc R . . H71A H 0.6660 -0.2094 1.2114 0.111 Uiso 1 1 calc R . . C72 C 1.0085(5) -0.0876(3) 1.1684(3) 0.0870(17) Uani 1 1 d . . . H72A H 0.9349 -0.0609 1.1545 0.130 Uiso 1 1 calc R . . H72C H 1.0235 -0.0947 1.2145 0.130 Uiso 1 1 calc R . . H72B H 1.0136 -0.1325 1.1636 0.130 Uiso 1 1 calc R . . C73 C 0.3782(5) 0.0573(3) 1.3292(3) 0.0812(16) Uani 1 1 d . . . H73B H 0.4224 0.0839 1.2951 0.122 Uiso 1 1 calc R . . H73C H 0.3711 0.0755 1.3648 0.122 Uiso 1 1 calc R . . H73A H 0.3057 0.0611 1.3102 0.122 Uiso 1 1 calc R . . C74 C 1.2115(4) -0.1466(3) 1.3514(3) 0.0841(17) Uani 1 1 d . . . H74B H 1.2671 -0.1163 1.3388 0.101 Uiso 1 1 calc R . . H74A H 1.1830 -0.1510 1.3114 0.101 Uiso 1 1 calc R . . C75 C 0.6630(5) 0.0535(4) 1.4700(4) 0.0918(19) Uani 1 1 d . . . H75B H 0.6040 0.0363 1.4991 0.110 Uiso 1 1 calc R . . H75A H 0.6359 0.0681 1.4238 0.110 Uiso 1 1 calc R . . C76 C 0.7738(6) -0.0822(3) 1.0317(3) 0.0840(16) Uani 1 1 d . . . H76B H 0.8356 -0.0939 1.0070 0.126 Uiso 1 1 calc R . . H76A H 0.7076 -0.0924 1.0165 0.126 Uiso 1 1 calc R . . H76C H 0.7884 -0.1095 1.0786 0.126 Uiso 1 1 calc R . . C77 C 1.0921(4) -0.0479(3) 1.1255(3) 0.0695(13) Uani 1 1 d . . . H77B H 1.1650 -0.0777 1.1362 0.083 Uiso 1 1 calc R . . H77A H 1.0731 -0.0380 1.0788 0.083 Uiso 1 1 calc R . . C78 C 0.5496(4) -0.1498(2) 1.4098(2) 0.0625(12) Uani 1 1 d . . . H78A H 0.5613 -0.2008 1.4242 0.075 Uiso 1 1 calc R . . H78B H 0.4928 -0.1357 1.4369 0.075 Uiso 1 1 calc R . . C79 C 0.9596(4) 0.0493(3) 1.3690(2) 0.0626(12) Uani 1 1 d . . . H79 H 0.9101 0.0675 1.3946 0.075 Uiso 1 1 calc R . . C80 C 0.7021(4) 0.2679(3) 1.1089(3) 0.0679(13) Uani 1 1 d . . . H80A H 0.6299 0.2970 1.0963 0.102 Uiso 1 1 calc R . . H80B H 0.7580 0.2972 1.1004 0.102 Uiso 1 1 calc R . . H80C H 0.7050 0.2394 1.1558 0.102 Uiso 1 1 calc R . . C81 C 0.4725(4) 0.0889(2) 1.0804(3) 0.0652(13) Uani 1 1 d . . . C82 C 0.9849(4) 0.0940(3) 1.3069(2) 0.0598(11) Uani 1 1 d . . . C83 C 0.3964(4) -0.0252(2) 1.1284(3) 0.0682(14) Uani 1 1 d . . . H83B H 0.3246 0.0054 1.1228 0.082 Uiso 1 1 calc R . . H83A H 0.3896 -0.0610 1.1101 0.082 Uiso 1 1 calc R . . C84 C 0.5085(3) -0.1185(2) 1.3377(2) 0.0567(11) Uani 1 1 d . . . C85 C 0.9667(4) -0.0694(3) 1.4598(2) 0.0646(13) Uani 1 1 d . . . H85A H 1.0226 -0.1115 1.4790 0.078 Uiso 1 1 calc R . . H85B H 0.9570 -0.0451 1.4912 0.078 Uiso 1 1 calc R . . C86 C 0.5286(4) -0.1564(2) 1.2956(3) 0.0607(12) Uani 1 1 d . . . H86 H 0.5675 -0.2025 1.3128 0.073 Uiso 1 1 calc R . . C87 C 0.7437(4) 0.1327(2) 1.00000(19) 0.0535(10) Uani 1 1 d . . . H87B H 0.7121 0.1819 0.9763 0.064 Uiso 1 1 calc R . . H87A H 0.7789 0.1141 0.9675 0.064 Uiso 1 1 calc R . . C88 C 0.7560(4) -0.0554(3) 1.4601(2) 0.0592(11) Uani 1 1 d . . . C89 C 0.4101(3) -0.0214(2) 1.2449(3) 0.0601(12) Uani 1 1 d . . . H89 H 0.3690 0.0241 1.2283 0.072 Uiso 1 1 calc R . . C90 C 0.4920(4) -0.1276(2) 1.2283(3) 0.0591(12) Uani 1 1 d . . . C91 C 1.0057(3) -0.0220(3) 1.3945(2) 0.0566(11) Uani 1 1 d . . . C92 C 0.5558(4) 0.1258(2) 1.0502(2) 0.0572(11) Uani 1 1 d . . . H92 H 0.5474 0.1736 1.0428 0.069 Uiso 1 1 calc R . . C93 C 0.4828(4) 0.0174(2) 1.0918(2) 0.0567(11) Uani 1 1 d . . . C94 C 0.8574(3) -0.1417(2) 1.4216(2) 0.0524(10) Uani 1 1 d . . . H94 H 0.9247 -0.1653 1.4131 0.063 Uiso 1 1 calc R . . C95 C 0.4487(3) -0.0498(2) 1.3114(3) 0.0591(12) Uani 1 1 d . . . C96 C 0.6584(4) -0.0757(3) 1.4483(2) 0.0570(11) Uani 1 1 d . . . H96 H 0.5911 -0.0536 1.4583 0.068 Uiso 1 1 calc R . . C97 C 1.0830(4) 0.1133(2) 1.1981(2) 0.0579(11) Uani 1 1 d . . . H97B H 1.0854 0.1603 1.1973 0.069 Uiso 1 1 calc R . . H97A H 1.1555 0.0945 1.1863 0.069 Uiso 1 1 calc R . . C98 C 1.1078(3) -0.0040(2) 1.2939(2) 0.0523(10) Uani 1 1 d . . . H98 H 1.1585 -0.0222 1.2689 0.063 Uiso 1 1 calc R . . C99 C 0.4313(3) -0.0595(2) 1.2018(3) 0.0587(12) Uani 1 1 d . . . C100 C 0.6582(3) -0.1275(2) 1.4223(2) 0.0539(10) Uani 1 1 d . . . C101 C 0.6894(7) 0.0623(5) 1.2517(5) 0.122(3) Uiso 1 1 d D . . C102 C 0.6522(10) 0.1118(6) 1.2687(6) 0.163(4) Uiso 1 1 d D . . H10J H 0.5867 0.1386 1.2414 0.245 Uiso 1 1 calc R . . H10K H 0.7071 0.1414 1.2633 0.245 Uiso 1 1 calc R . . H10L H 0.6335 0.0943 1.3150 0.245 Uiso 1 1 calc R . . C103 C 0.5404(10) 0.4539(6) 0.7549(6) 0.146(3) Uiso 1 1 d D . . C104 C 0.6302(10) 0.4880(7) 0.7483(7) 0.174(4) Uiso 1 1 d D . . H10B H 0.6118 0.5346 0.7150 0.261 Uiso 1 1 calc R . . H10A H 0.6930 0.4621 0.7348 0.261 Uiso 1 1 calc R . . H10C H 0.6481 0.4911 0.7905 0.261 Uiso 1 1 calc R . . C105 C 0.9852(11) 0.5609(7) 0.7392(6) 0.163(4) Uiso 1 1 d D . . C106 C 0.8843(10) 0.5385(7) 0.7405(7) 0.173(4) Uiso 1 1 d D . . H10G H 0.8833 0.5154 0.7088 0.260 Uiso 1 1 calc R . . H10H H 0.8250 0.5784 0.7289 0.260 Uiso 1 1 calc R . . H10I H 0.8747 0.5061 0.7847 0.260 Uiso 1 1 calc R . . N101 N 0.7393(7) 0.0059(5) 1.2360(5) 0.156(3) Uiso 1 1 d D . . N102 N 0.4703(10) 0.4230(6) 0.7643(6) 0.195(4) Uiso 1 1 d D . . N103 N 1.0671(11) 0.5822(7) 0.7343(6) 0.202(4) Uiso 1 1 d 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 O1 0.071(3) 0.110(4) 0.129(4) -0.009(3) 0.035(3) -0.010(3) O2 0.084(3) 0.085(3) 0.133(4) 0.003(3) 0.054(3) -0.022(2) O3 0.135(4) 0.082(3) 0.093(3) -0.035(2) 0.024(3) -0.060(3) O4 0.116(4) 0.106(3) 0.093(3) -0.045(2) -0.005(2) -0.056(3) O5 0.062(2) 0.077(2) 0.074(2) -0.0263(18) 0.0078(16) -0.0148(17) O6 0.075(2) 0.084(3) 0.073(2) -0.0088(19) -0.0163(18) -0.011(2) O7 0.072(3) 0.063(2) 0.126(3) -0.021(2) 0.039(2) -0.0148(19) O8 0.059(2) 0.084(3) 0.083(2) 0.001(2) 0.0199(18) -0.0062(18) O9 0.104(3) 0.061(2) 0.084(2) -0.0194(18) 0.001(2) -0.039(2) O10 0.085(2) 0.0563(19) 0.0608(19) -0.0094(15) -0.0147(16) -0.0282(17) O11 0.0477(19) 0.059(2) 0.201(5) -0.063(3) 0.001(2) -0.0030(16) O12 0.074(2) 0.0508(19) 0.113(3) -0.0424(19) -0.022(2) -0.0026(16) O13 0.069(2) 0.111(3) 0.089(3) -0.066(2) 0.0015(18) 0.000(2) O14 0.092(3) 0.070(2) 0.079(2) -0.0395(19) 0.0159(19) -0.0070(19) O15 0.0589(19) 0.058(2) 0.092(2) -0.0284(18) 0.0112(17) 0.0013(15) O16 0.0507(17) 0.074(2) 0.0590(18) -0.0153(16) 0.0091(14) -0.0087(15) O17 0.095(2) 0.0447(17) 0.076(2) -0.0295(16) 0.0143(18) -0.0055(16) O18 0.0587(18) 0.0587(19) 0.0669(19) -0.0261(16) 0.0093(14) 0.0044(15) O19 0.0578(18) 0.0492(17) 0.093(2) -0.0289(17) 0.0245(16) -0.0136(14) O20 0.0631(18) 0.0432(15) 0.0558(17) -0.0215(13) 0.0012(13) 0.0003(13) C1 0.055(3) 0.050(2) 0.057(2) -0.027(2) -0.005(2) 0.005(2) C2 0.057(3) 0.045(2) 0.062(3) -0.022(2) 0.001(2) 0.004(2) C3 0.057(3) 0.043(2) 0.060(3) -0.023(2) -0.012(2) 0.0028(19) C4 0.109(5) 0.068(4) 0.122(5) -0.025(4) 0.041(4) -0.037(3) C5 0.074(3) 0.038(2) 0.057(3) -0.0091(19) -0.015(2) -0.008(2) C6 0.057(3) 0.082(4) 0.047(2) -0.003(2) 0.017(2) 0.002(3) C7 0.066(3) 0.036(2) 0.058(3) -0.0133(19) -0.009(2) -0.0073(19) C8 0.088(5) 0.300(15) 0.139(8) -0.055(9) 0.020(5) -0.095(8) C9 0.065(3) 0.039(2) 0.068(3) -0.016(2) -0.015(2) -0.002(2) C10 0.180(9) 0.084(5) 0.140(7) -0.043(5) 0.048(6) -0.012(5) C12 0.139(8) 0.212(13) 0.137(9) -0.038(8) 0.017(6) 0.004(8) C13 0.122(5) 0.064(3) 0.045(2) -0.019(2) 0.005(3) -0.046(3) C15 0.137(6) 0.132(7) 0.138(7) -0.077(6) 0.009(5) -0.071(5) C16 0.109(5) 0.082(4) 0.121(5) -0.035(4) 0.020(4) -0.053(4) C17 0.097(6) 0.163(9) 0.235(13) -0.032(9) 0.086(7) -0.024(6) C18 0.152(8) 0.106(6) 0.148(7) -0.031(5) -0.006(6) -0.074(6) C19 0.096(4) 0.041(3) 0.142(6) -0.014(3) 0.057(4) -0.004(3) C20 0.144(5) 0.082(4) 0.062(3) -0.039(3) 0.023(3) -0.063(4) C21 0.078(4) 0.090(4) 0.069(3) -0.011(3) 0.013(3) -0.021(3) C22 0.061(3) 0.095(4) 0.067(3) 0.020(3) 0.014(3) 0.000(3) C23 0.070(4) 0.095(4) 0.099(4) -0.031(4) 0.004(3) -0.020(3) C24 0.072(4) 0.056(3) 0.115(5) 0.006(3) 0.046(4) 0.001(3) C25 0.070(3) 0.048(3) 0.107(4) 0.006(3) 0.041(3) 0.010(3) C26 0.073(4) 0.102(5) 0.083(4) -0.013(3) -0.016(3) -0.022(3) C27 0.059(3) 0.069(4) 0.106(5) 0.020(3) 0.027(3) 0.010(3) C28 0.100(4) 0.050(3) 0.088(4) -0.018(3) -0.009(3) -0.020(3) C29 0.136(6) 0.073(4) 0.059(3) -0.030(3) -0.003(3) -0.052(4) C30 0.097(4) 0.058(3) 0.051(3) -0.001(2) -0.023(2) -0.025(3) C31 0.054(3) 0.072(4) 0.084(4) 0.024(3) 0.026(3) 0.000(3) C32 0.097(4) 0.089(4) 0.051(3) -0.019(3) -0.006(3) -0.044(3) C33 0.093(4) 0.073(4) 0.089(4) -0.047(3) 0.022(3) -0.038(3) C34 0.072(4) 0.052(3) 0.102(4) 0.013(3) 0.040(3) 0.000(3) C35 0.061(3) 0.069(4) 0.083(4) 0.027(3) 0.032(3) 0.012(3) C36 0.098(4) 0.065(3) 0.083(4) -0.044(3) 0.043(3) -0.038(3) C37 0.060(3) 0.088(4) 0.044(2) 0.009(2) 0.016(2) -0.003(3) C38 0.059(3) 0.092(4) 0.045(2) 0.003(2) 0.001(2) -0.001(3) C39 0.069(3) 0.085(4) 0.056(3) -0.040(3) 0.004(2) -0.002(3) C40 0.074(3) 0.064(3) 0.076(3) -0.019(3) -0.014(3) -0.019(3) C41 0.113(5) 0.040(3) 0.084(4) -0.030(3) 0.044(3) -0.025(3) C42 0.065(3) 0.079(3) 0.036(2) -0.021(2) 0.0026(19) 0.002(2) C43 0.120(5) 0.053(3) 0.042(2) -0.009(2) -0.011(3) -0.040(3) C44 0.112(5) 0.053(3) 0.050(3) -0.010(2) -0.007(3) -0.039(3) C45 0.079(4) 0.049(3) 0.111(4) -0.032(3) 0.050(3) -0.016(3) C46 0.110(4) 0.058(3) 0.061(3) -0.036(2) 0.032(3) -0.033(3) C47 0.055(3) 0.087(4) 0.048(2) -0.022(2) 0.014(2) -0.004(3) C48 0.060(3) 0.087(4) 0.040(2) -0.013(2) 0.002(2) -0.010(3) C49 0.110(4) 0.056(3) 0.038(2) -0.005(2) -0.018(2) -0.034(3) C50 0.093(4) 0.039(2) 0.076(3) -0.023(2) 0.033(3) -0.011(2) C51 0.051(2) 0.071(3) 0.034(2) -0.0125(19) 0.0051(17) -0.008(2) C52 0.050(2) 0.041(2) 0.052(2) -0.0064(18) 0.0150(18) -0.0069(18) C53 0.051(2) 0.044(2) 0.054(2) -0.0134(19) 0.0181(19) -0.0033(18) C54 0.074(3) 0.040(2) 0.040(2) -0.0134(17) -0.0146(19) -0.004(2) C55 0.072(3) 0.040(2) 0.048(2) -0.0177(18) -0.010(2) -0.004(2) C56 0.040(2) 0.066(3) 0.052(2) -0.020(2) -0.0017(18) -0.014(2) C57 0.068(3) 0.045(2) 0.044(2) -0.0197(18) 0.0150(19) -0.006(2) C58 0.038(2) 0.066(3) 0.057(2) -0.029(2) 0.0029(17) -0.0164(19) C59 0.058(2) 0.034(2) 0.046(2) -0.0119(16) 0.0138(18) -0.0078(18) C60 0.052(2) 0.040(2) 0.054(2) -0.0192(18) 0.0138(18) -0.0129(18) C61 0.061(3) 0.040(2) 0.041(2) -0.0125(17) 0.0124(17) -0.0098(19) C62 0.074(3) 0.036(2) 0.059(3) -0.0166(19) -0.025(2) 0.001(2) C63 0.48(3) 0.091(7) 0.197(13) -0.060(8) -0.127(16) 0.058(12) C64 0.048(2) 0.044(2) 0.052(2) -0.0159(18) 0.0176(18) -0.0143(18) C65 0.134(7) 0.090(5) 0.170(9) -0.028(5) 0.054(6) -0.019(5) C66 0.152(7) 0.090(5) 0.124(6) -0.053(5) 0.055(5) 0.004(5) C67 0.110(5) 0.149(7) 0.126(6) -0.090(6) 0.039(4) -0.031(5) C68 0.068(3) 0.087(4) 0.147(6) -0.077(4) 0.030(3) -0.011(3) C69 0.129(6) 0.077(4) 0.099(5) -0.043(4) -0.006(4) 0.004(4) C70 0.076(5) 0.086(6) 0.55(3) -0.167(11) 0.049(9) -0.012(4) C71 0.110(5) 0.071(4) 0.083(4) -0.027(3) -0.009(3) 0.019(3) C72 0.092(4) 0.060(3) 0.100(4) -0.023(3) 0.013(3) -0.004(3) C73 0.068(3) 0.059(3) 0.116(5) -0.038(3) -0.011(3) 0.006(2) C74 0.059(3) 0.070(3) 0.100(4) -0.010(3) 0.027(3) -0.001(3) C75 0.074(4) 0.117(5) 0.116(5) -0.079(4) 0.033(3) -0.021(3) C76 0.112(4) 0.046(3) 0.095(4) -0.033(3) 0.007(3) 0.001(3) C77 0.075(3) 0.054(3) 0.076(3) -0.030(2) 0.016(3) 0.008(2) C78 0.050(3) 0.052(3) 0.074(3) -0.008(2) 0.026(2) -0.016(2) C79 0.061(3) 0.090(4) 0.048(2) -0.038(3) 0.004(2) -0.014(3) C80 0.074(3) 0.062(3) 0.075(3) -0.042(3) 0.001(2) 0.007(2) C81 0.057(3) 0.046(2) 0.097(4) -0.034(3) -0.023(3) -0.002(2) C82 0.057(3) 0.069(3) 0.065(3) -0.037(2) 0.001(2) -0.014(2) C83 0.053(3) 0.050(3) 0.102(4) -0.027(3) -0.025(3) -0.009(2) C84 0.041(2) 0.047(2) 0.079(3) -0.015(2) 0.012(2) -0.0171(19) C85 0.060(3) 0.092(4) 0.039(2) -0.022(2) -0.0015(19) -0.011(2) C86 0.044(2) 0.036(2) 0.098(4) -0.018(2) -0.002(2) -0.0095(18) C87 0.080(3) 0.039(2) 0.036(2) -0.0088(16) 0.0030(19) -0.004(2) C88 0.062(3) 0.073(3) 0.042(2) -0.024(2) 0.0106(19) -0.005(2) C89 0.033(2) 0.041(2) 0.100(4) -0.018(2) -0.001(2) -0.0055(17) C90 0.045(2) 0.042(2) 0.095(4) -0.027(2) -0.007(2) -0.0136(19) C91 0.044(2) 0.085(3) 0.046(2) -0.029(2) -0.0040(18) -0.014(2) C92 0.063(3) 0.035(2) 0.072(3) -0.020(2) -0.019(2) 0.000(2) C93 0.054(3) 0.046(2) 0.072(3) -0.024(2) -0.023(2) -0.005(2) C94 0.047(2) 0.052(2) 0.047(2) -0.0078(19) 0.0126(17) -0.0023(19) C95 0.036(2) 0.047(2) 0.095(4) -0.027(2) 0.011(2) -0.0092(18) C96 0.047(2) 0.067(3) 0.051(2) -0.019(2) 0.0160(18) -0.002(2) C97 0.047(2) 0.058(3) 0.070(3) -0.021(2) 0.015(2) -0.019(2) C98 0.035(2) 0.070(3) 0.059(3) -0.028(2) 0.0050(17) -0.0157(19) C99 0.038(2) 0.041(2) 0.098(4) -0.024(2) -0.008(2) -0.0115(18) C100 0.048(2) 0.048(2) 0.051(2) -0.0032(19) 0.0136(18) -0.0028(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C27 1.389(10) . ? O1 C17 1.441(9) . ? O2 C34 1.380(9) . ? O2 C14 1.390(10) . ? O3 C33 1.381(7) . ? O3 C16 1.428(7) . ? O4 C32 1.379(8) . ? O4 C15 1.429(7) . ? O5 C2 1.381(6) . ? O5 C23 1.409(7) . ? O6 C48 1.390(6) . ? O6 C26 1.427(7) . ? O7 C50 1.331(7) . ? O7 C4 1.420(7) . ? O8 C6 1.395(7) . ? O8 C21 1.407(7) . ? O9 C43 1.350(7) . ? O9 C28 1.405(6) . ? O10 C7 1.377(6) . ? O10 C40 1.418(5) . ? O11 C81 1.393(7) . ? O11 C70 1.404(8) . ? O12 C90 1.379(6) . ? O12 C71 1.389(7) . ? O13 C88 1.376(6) . ? O13 C75 1.446(7) . ? O14 C82 1.375(6) . ? O14 C66 1.429(7) . ? O15 C95 1.368(6) . ? O15 C73 1.421(6) . ? O16 C56 1.371(6) . ? O16 C74 1.409(6) . ? O17 C55 1.377(6) . ? O17 C76 1.418(6) . ? O18 C53 1.387(5) . ? O18 C77 1.421(6) . ? O19 C52 1.376(5) . ? O19 C68 1.393(6) . ? O20 C59 1.381(5) . ? O20 C80 1.421(5) . ? C1 C3 1.376(7) . ? C1 C2 1.393(6) . ? C1 C39 1.518(6) . ? C2 C9 1.396(7) . ? C3 C7 1.388(6) . ? C5 C9 1.390(7) . ? C5 C7 1.396(6) . ? C5 C30 1.519(7) . ? C6 C37 1.380(7) . ? C6 C47 1.392(7) . ? C8 C23 1.498(11) . ? C10 C28 1.365(10) . ? C11 C14 1.261(13) . ? C12 C21 1.534(14) . ? C13 C29 1.383(9) . ? C13 C43 1.406(7) . ? C13 C20 1.523(9) . ? C16 C18 1.445(11) . ? C19 C25 1.493(10) . ? C19 C45 1.499(9) . ? C20 C46 1.527(8) . ? C22 C35 1.488(10) . ? C22 C37 1.517(8) . ? C24 C27 1.371(11) . ? C24 C25 1.389(10) . ? C25 C34 1.397(8) . ? C27 C35 1.418(8) . ? C29 C32 1.385(9) . ? C30 C49 1.518(8) . ? C31 C34 1.370(10) . ? C31 C35 1.379(10) . ? C32 C49 1.405(7) . ? C33 C41 1.364(9) . ? C33 C46 1.438(7) . ? C36 C46 1.339(8) . ? C36 C50 1.396(8) . ? C37 C38 1.375(8) . ? C38 C48 1.389(8) . ? C39 C42 1.524(7) . ? C41 C45 1.361(9) . ? C42 C47 1.375(7) . ? C42 C48 1.385(7) . ? C43 C44 1.403(8) . ? C44 C49 1.387(8) . ? C45 C50 1.426(7) . ? C51 C94 1.388(7) . ? C51 C88 1.396(6) . ? C51 C85 1.504(6) . ? C52 C94 1.377(6) . ? C52 C100 1.391(6) . ? C53 C64 1.383(6) . ? C53 C57 1.390(6) . ? C54 C92 1.378(7) . ? C54 C55 1.403(6) . ? C54 C87 1.515(7) . ? C55 C62 1.378(7) . ? C56 C91 1.383(6) . ? C56 C98 1.394(6) . ? C57 C61 1.380(6) . ? C58 C98 1.392(6) . ? C58 C82 1.401(6) . ? C58 C97 1.510(6) . ? C59 C60 1.376(6) . ? C59 C61 1.393(6) . ? C60 C64 1.406(6) . ? C61 C87 1.521(6) . ? C62 C93 1.388(7) . ? C63 C70 1.340(16) . ? C64 C97 1.508(6) . ? C65 C74 1.413(10) . ? C67 C75 1.476(9) . ? C69 C71 1.496(9) . ? C72 C77 1.504(8) . ? C78 C84 1.501(7) . ? C78 C100 1.534(6) . ? C79 C82 1.381(7) . ? C79 C91 1.390(7) . ? C81 C92 1.384(7) . ? C81 C93 1.391(6) . ? C83 C99 1.507(7) . ? C83 C93 1.512(7) . ? C84 C86 1.386(7) . ? C84 C95 1.396(6) . ? C85 C91 1.510(7) . ? C86 C90 1.394(7) . ? C88 C96 1.385(7) . ? C89 C95 1.386(7) . ? C89 C99 1.408(7) . ? C90 C99 1.391(6) . ? C96 C100 1.374(7) . ? C101 C102 1.220(11) . ? C101 N101 1.368(11) . ? C103 N102 1.125(12) . ? C103 C104 1.380(13) . ? C105 N103 1.147(13) . ? C105 C106 1.384(14) . ? 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 C27 O1 C17 120.2(8) . . ? C34 O2 C14 113.7(6) . . ? C33 O3 C16 117.2(5) . . ? C32 O4 C15 116.2(6) . . ? C2 O5 C23 119.0(4) . . ? C48 O6 C26 118.0(4) . . ? C50 O7 C4 118.1(5) . . ? C6 O8 C21 117.6(4) . . ? C43 O9 C28 116.4(5) . . ? C7 O10 C40 118.4(4) . . ? C81 O11 C70 118.2(6) . . ? C90 O12 C71 119.4(4) . . ? C88 O13 C75 117.9(4) . . ? C82 O14 C66 117.3(5) . . ? C95 O15 C73 118.0(4) . . ? C56 O16 C74 118.9(4) . . ? C55 O17 C76 118.2(4) . . ? C53 O18 C77 118.1(4) . . ? C52 O19 C68 118.3(4) . . ? C59 O20 C80 117.3(3) . . ? C3 C1 C2 119.1(4) . . ? C3 C1 C39 120.9(4) . . ? C2 C1 C39 120.0(4) . . ? O5 C2 C1 116.0(4) . . ? O5 C2 C9 124.0(4) . . ? C1 C2 C9 120.0(4) . . ? C1 C3 C7 121.0(4) . . ? C9 C5 C7 118.1(4) . . ? C9 C5 C30 120.2(4) . . ? C7 C5 C30 121.4(4) . . ? C37 C6 C47 120.2(5) . . ? C37 C6 O8 117.0(5) . . ? C47 C6 O8 122.8(4) . . ? O10 C7 C3 123.6(4) . . ? O10 C7 C5 115.6(4) . . ? C3 C7 C5 120.8(4) . . ? C5 C9 C2 121.0(4) . . ? C29 C13 C43 118.2(6) . . ? C29 C13 C20 121.5(5) . . ? C43 C13 C20 120.3(6) . . ? C11 C14 O2 108.2(12) . . ? O3 C16 C18 109.0(6) . . ? C25 C19 C45 110.2(4) . . ? C13 C20 C46 113.1(4) . . ? O8 C21 C12 110.4(6) . . ? C35 C22 C37 112.4(4) . . ? O5 C23 C8 104.9(6) . . ? C27 C24 C25 121.0(6) . . ? C24 C25 C34 118.9(7) . . ? C24 C25 C19 119.3(5) . . ? C34 C25 C19 121.7(7) . . ? C24 C27 O1 123.8(6) . . ? C24 C27 C35 119.5(8) . . ? O1 C27 C35 116.8(7) . . ? C10 C28 O9 106.6(6) . . ? C13 C29 C32 122.5(5) . . ? C49 C30 C5 109.9(4) . . ? C34 C31 C35 120.5(5) . . ? O4 C32 C29 125.4(5) . . ? O4 C32 C49 114.2(6) . . ? C29 C32 C49 120.4(6) . . ? C41 C33 O3 125.1(5) . . ? C41 C33 C46 119.3(6) . . ? O3 C33 C46 115.6(6) . . ? C31 C34 O2 122.5(5) . . ? C31 C34 C25 120.8(7) . . ? O2 C34 C25 116.8(7) . . ? C31 C35 C27 119.4(7) . . ? C31 C35 C22 121.1(5) . . ? C27 C35 C22 119.5(8) . . ? C46 C36 C50 125.3(5) . . ? C38 C37 C6 117.9(5) . . ? C38 C37 C22 120.4(5) . . ? C6 C37 C22 121.7(5) . . ? C37 C38 C48 122.4(5) . . ? C1 C39 C42 112.3(4) . . ? C45 C41 C33 123.4(5) . . ? C47 C42 C48 118.6(5) . . ? C47 C42 C39 121.0(4) . . ? C48 C42 C39 120.5(5) . . ? O9 C43 C44 124.9(4) . . ? O9 C43 C13 116.4(5) . . ? C44 C43 C13 118.7(6) . . ? C49 C44 C43 123.3(5) . . ? C41 C45 C50 118.4(6) . . ? C41 C45 C19 120.2(5) . . ? C50 C45 C19 121.3(6) . . ? C36 C46 C33 116.6(5) . . ? C36 C46 C20 123.5(5) . . ? C33 C46 C20 119.9(6) . . ? C42 C47 C6 121.5(5) . . ? C42 C48 C38 119.4(5) . . ? C42 C48 O6 116.8(5) . . ? C38 C48 O6 123.8(4) . . ? C44 C49 C32 116.8(6) . . ? C44 C49 C30 121.3(4) . . ? C32 C49 C30 121.7(6) . . ? O7 C50 C36 126.5(5) . . ? O7 C50 C45 116.6(5) . . ? C36 C50 C45 116.9(6) . . ? C94 C51 C88 117.5(4) . . ? C94 C51 C85 120.2(4) . . ? C88 C51 C85 122.2(4) . . ? O19 C52 C94 123.8(4) . . ? O19 C52 C100 116.0(4) . . ? C94 C52 C100 120.2(4) . . ? C64 C53 O18 115.9(4) . . ? C64 C53 C57 120.9(4) . . ? O18 C53 C57 123.2(4) . . ? C92 C54 C55 118.9(4) . . ? C92 C54 C87 120.9(4) . . ? C55 C54 C87 120.2(4) . . ? O17 C55 C62 124.2(4) . . ? O17 C55 C54 116.2(4) . . ? C62 C55 C54 119.6(4) . . ? O16 C56 C91 116.5(4) . . ? O16 C56 C98 123.2(4) . . ? C91 C56 C98 120.2(4) . . ? C61 C57 C53 121.3(4) . . ? C98 C58 C82 118.7(4) . . ? C98 C58 C97 120.5(4) . . ? C82 C58 C97 120.7(4) . . ? C60 C59 O20 123.6(4) . . ? C60 C59 C61 120.4(4) . . ? O20 C59 C61 116.0(4) . . ? C59 C60 C64 121.6(4) . . ? C57 C61 C59 118.3(4) . . ? C57 C61 C87 120.7(4) . . ? C59 C61 C87 121.0(4) . . ? C55 C62 C93 121.8(4) . . ? C53 C64 C60 117.3(4) . . ? C53 C64 C97 121.9(4) . . ? C60 C64 C97 120.8(4) . . ? C63 C70 O11 112.5(9) . . ? O12 C71 C69 108.4(5) . . ? O16 C74 C65 105.9(6) . . ? O13 C75 C67 108.4(5) . . ? O18 C77 C72 113.6(4) . . ? C84 C78 C100 113.3(3) . . ? C82 C79 C91 122.2(4) . . ? C92 C81 C93 120.6(5) . . ? C92 C81 O11 123.7(4) . . ? C93 C81 O11 115.7(5) . . ? O14 C82 C79 124.3(4) . . ? O14 C82 C58 116.3(4) . . ? C79 C82 C58 119.3(5) . . ? C99 C83 C93 109.0(3) . . ? C86 C84 C95 118.4(5) . . ? C86 C84 C78 121.3(4) . . ? C95 C84 C78 120.3(5) . . ? C51 C85 C91 110.4(3) . . ? C84 C86 C90 121.9(4) . . ? C54 C87 C61 112.5(3) . . ? O13 C88 C96 123.8(4) . . ? O13 C88 C51 116.1(4) . . ? C96 C88 C51 120.1(4) . . ? C95 C89 C99 121.9(4) . . ? O12 C90 C99 116.3(5) . . ? O12 C90 C86 123.5(4) . . ? C99 C90 C86 120.2(5) . . ? C56 C91 C79 118.4(4) . . ? C56 C91 C85 121.8(5) . . ? C79 C91 C85 119.6(4) . . ? C54 C92 C81 121.1(4) . . ? C62 C93 C81 118.1(5) . . ? C62 C93 C83 120.1(4) . . ? C81 C93 C83 121.8(5) . . ? C52 C94 C51 122.0(4) . . ? O15 C95 C89 123.9(4) . . ? O15 C95 C84 116.1(5) . . ? C89 C95 C84 119.9(5) . . ? C100 C96 C88 121.9(4) . . ? C64 C97 C58 112.1(3) . . ? C58 C98 C56 121.0(4) . . ? C90 C99 C89 117.7(5) . . ? C90 C99 C83 121.5(5) . . ? C89 C99 C83 120.6(4) . . ? C96 C100 C52 118.2(4) . . ? C96 C100 C78 121.4(4) . . ? C52 C100 C78 120.4(4) . . ? C102 C101 N101 174.9(11) . . ? N102 C103 C104 175.4(14) . . ? N103 C105 C106 175.9(15) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 65.08 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.475 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.085 #===END data_1 _database_code_depnum_ccdc_archive 'CCDC 782493' #TrackingRef '- CC-BMpillar-S2-new2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H80 O10' _chemical_formula_sum 'C60 H80 O10' _chemical_formula_weight 961.24 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 12.0537(5) _cell_length_b 14.0506(9) _cell_length_c 18.5235(12) _cell_angle_alpha 88.658(5) _cell_angle_beta 80.286(4) _cell_angle_gamma 64.905(5) _cell_volume 2796.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6050 _cell_measurement_theta_min 2.4215 _cell_measurement_theta_max 66.9117 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type multi-scan' _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.53 (release 17-11-2009 CrysAlis171 .NET) (compiled Nov 17 2009,16:58:22) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _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_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35262 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 67.02 _reflns_number_total 9911 _reflns_number_gt 5343 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9911 _refine_ls_number_parameters 616 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1571 _refine_ls_R_factor_gt 0.1123 _refine_ls_wR_factor_ref 0.3700 _refine_ls_wR_factor_gt 0.3361 _refine_ls_goodness_of_fit_ref 1.244 _refine_ls_restrained_S_all 1.263 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.5298(5) 0.4890(4) 0.7414(2) 0.1271(17) Uani 1 1 d . . . O2 O 0.6830(4) 0.0727(4) 0.6625(3) 0.1061(13) Uani 1 1 d . . . O3 O 0.8974(3) 0.3101(3) 0.5267(2) 0.0962(11) Uani 1 1 d . . . O4 O 1.1532(3) -0.0887(3) 0.61801(17) 0.0785(9) Uani 1 1 d . . . O5 O 1.2728(4) 0.2236(4) 0.6324(2) 0.0980(12) Uani 1 1 d . . . O6 O 1.3533(3) -0.0805(3) 0.83700(16) 0.0711(9) Uani 1 1 d . E . O7 O 1.1690(3) 0.3371(3) 0.88393(19) 0.0769(9) Uani 1 1 d . E . O8 O 0.9552(2) 0.1182(3) 1.06436(16) 0.0732(9) Uani 1 1 d . . . O9 O 0.7075(3) 0.5069(3) 0.96561(17) 0.0795(10) Uani 1 1 d . . . O10 O 0.5482(3) 0.1990(3) 0.9295(2) 0.0882(11) Uani 1 1 d . E . C1 C 0.5498(14) 0.5552(12) 0.6892(9) 0.209(5) Uiso 1 1 d . . . H1A H 0.5540 0.5281 0.6412 0.313 Uiso 1 1 calc R . . H1C H 0.6266 0.5589 0.6920 0.313 Uiso 1 1 calc R . . H1B H 0.4825 0.6242 0.6983 0.313 Uiso 1 1 calc R . . C2 C 0.5703(5) 0.3865(5) 0.7204(3) 0.0878(16) Uani 1 1 d . . . C3 C 0.5340(4) 0.3273(5) 0.7702(3) 0.0765(14) Uani 1 1 d . E . C4 C 0.5701(4) 0.2230(5) 0.7511(3) 0.0831(16) Uani 1 1 d . . . H4 H 0.5458 0.1820 0.7844 0.100 Uiso 1 1 calc R . . C5 C 0.6418(4) 0.1772(5) 0.6833(3) 0.0823(15) Uani 1 1 d . . . C6 C 0.6806(4) 0.2371(5) 0.6331(2) 0.0748(14) Uani 1 1 d . . . C7 C 0.6417(5) 0.3412(5) 0.6514(3) 0.0847(15) Uani 1 1 d . . . H7 H 0.6630 0.3832 0.6175 0.102 Uiso 1 1 calc R . . C8 C 0.6424(6) 0.0104(6) 0.7087(6) 0.126(3) Uani 1 1 d . B . H8A H 0.5522 0.0404 0.7171 0.151 Uiso 1 1 calc R . . H8B H 0.6684 0.0092 0.7556 0.151 Uiso 1 1 calc R . . C9 C 0.6915(13) -0.0945(10) 0.6778(8) 0.183(4) Uiso 1 1 d D . . H9BD H 0.7815 -0.1234 0.6659 0.220 Uiso 0.50 1 calc PR A 2 H9BC H 0.6692 -0.1386 0.7129 0.220 Uiso 0.50 1 calc PR A 2 H9AB H 0.7800 -0.1202 0.6779 0.220 Uiso 0.50 1 calc PR A 1 H9AA H 0.6830 -0.0839 0.6268 0.220 Uiso 0.50 1 calc PR A 1 C10 C 0.645(2) -0.0925(16) 0.6172(11) 0.149(4) Uiso 0.50 1 d PD B 2 H10B H 0.6890 -0.0693 0.5774 0.179 Uiso 0.50 1 calc PR B 2 H10A H 0.5580 -0.0418 0.6254 0.179 Uiso 0.50 1 calc PR B 2 C11 C 0.653(3) -0.2009(19) 0.5944(16) 0.189(6) Uiso 0.50 1 d PD B 2 H11A H 0.6427 -0.2013 0.5442 0.284 Uiso 0.50 1 calc PR B 2 H11B H 0.5892 -0.2139 0.6253 0.284 Uiso 0.50 1 calc PR B 2 H11C H 0.7332 -0.2548 0.5997 0.284 Uiso 0.50 1 calc PR B 2 C12 C 0.6691(18) -0.1896(12) 0.6926(11) 0.149(4) Uiso 0.50 1 d PD B 1 H12A H 0.5875 -0.1746 0.6819 0.179 Uiso 0.50 1 calc PR B 1 H12B H 0.6656 -0.2000 0.7448 0.179 Uiso 0.50 1 calc PR B 1 C13 C 0.761(2) -0.2935(17) 0.6520(15) 0.189(6) Uiso 0.50 1 d PD B 1 H13A H 0.7511 -0.2913 0.6015 0.284 Uiso 0.50 1 calc PR B 1 H13B H 0.7450 -0.3500 0.6741 0.284 Uiso 0.50 1 calc PR B 1 H13C H 0.8442 -0.3046 0.6549 0.284 Uiso 0.50 1 calc PR B 1 C14 C 0.7608(4) 0.1888(5) 0.5605(2) 0.0818(15) Uani 1 1 d . . . H14B H 0.7401 0.2409 0.5237 0.098 Uiso 1 1 calc R . . H14A H 0.7445 0.1309 0.5456 0.098 Uiso 1 1 calc R . . C15 C 0.9523(10) 0.3783(8) 0.5195(6) 0.149(3) Uiso 1 1 d . . . H15B H 1.0224 0.3526 0.4802 0.224 Uiso 1 1 calc R . . H15C H 0.9797 0.3835 0.5644 0.224 Uiso 1 1 calc R . . H15A H 0.8932 0.4464 0.5090 0.224 Uiso 1 1 calc R . . C16 C 0.9634(4) 0.2111(5) 0.5488(2) 0.0776(14) Uani 1 1 d . . . C17 C 0.9004(4) 0.1481(4) 0.5652(2) 0.0733(14) Uani 1 1 d . . . C18 C 0.9620(4) 0.0481(4) 0.5874(2) 0.0727(13) Uani 1 1 d . . . H18 H 0.9197 0.0060 0.5980 0.087 Uiso 1 1 calc R . . C19 C 1.0875(4) 0.0085(4) 0.5944(2) 0.0702(13) Uani 1 1 d . . . C20 C 1.1523(4) 0.0705(4) 0.5766(2) 0.0711(13) Uani 1 1 d . . . C21 C 1.0886(4) 0.1711(4) 0.5534(2) 0.0747(13) Uani 1 1 d . . . H21 H 1.1311 0.2126 0.5406 0.090 Uiso 1 1 calc R . . C22 C 1.0918(6) -0.1517(5) 0.6390(3) 0.0987(17) Uani 1 1 d DU . . H22A H 1.0633 -0.1685 0.5972 0.118 Uiso 1 1 calc R . . H22B H 1.0198 -0.1143 0.6766 0.118 Uiso 1 1 calc R . . C23 C 1.1776(9) -0.2501(6) 0.6677(5) 0.129(2) Uani 1 1 d DU D . H23B H 1.2083 -0.2304 0.7074 0.155 Uiso 1 1 calc R . . H23A H 1.2486 -0.2853 0.6290 0.155 Uiso 1 1 calc R . . C24 C 1.1271(9) -0.3328(8) 0.6969(6) 0.166(3) Uiso 1 1 d DU . . H24B H 1.1963 -0.3962 0.7071 0.199 Uiso 0.25 1 calc PR C 1 H24A H 1.0698 -0.3046 0.7427 0.199 Uiso 0.25 1 calc PR C 1 H24F H 1.1976 -0.3983 0.7024 0.199 Uiso 0.25 1 calc PR C 3 H24E H 1.0864 -0.3461 0.6600 0.199 Uiso 0.25 1 calc PR C 3 H24C H 1.0921 -0.3517 0.6592 0.199 Uiso 0.50 1 calc PR C 2 H24D H 1.0619 -0.3023 0.7393 0.199 Uiso 0.50 1 calc PR C 2 C25 C 1.060(2) -0.362(2) 0.6428(12) 0.098(6) Uiso 0.25 1 d PDU D 1 H25A H 0.9956 -0.2994 0.6289 0.146 Uiso 0.25 1 calc PR D 1 H25C H 1.0232 -0.4065 0.6662 0.146 Uiso 0.25 1 calc PR D 1 H25B H 1.1186 -0.3993 0.5999 0.146 Uiso 0.25 1 calc PR D 1 C26 C 1.033(2) -0.301(2) 0.7722(11) 0.115(8) Uiso 0.25 1 d PDU D 3 H26B H 0.9890 -0.2252 0.7779 0.173 Uiso 0.25 1 calc PR D 3 H26C H 1.0777 -0.3265 0.8119 0.173 Uiso 0.25 1 calc PR D 3 H26A H 0.9742 -0.3303 0.7725 0.173 Uiso 0.25 1 calc PR D 3 C27 C 1.2381(10) -0.4353(9) 0.7189(7) 0.097(3) Uiso 0.50 1 d PDU D 2 H27A H 1.2272 -0.4967 0.7071 0.146 Uiso 0.50 1 calc PR D 2 H27C H 1.2376 -0.4306 0.7706 0.146 Uiso 0.50 1 calc PR D 2 H27B H 1.3160 -0.4404 0.6922 0.146 Uiso 0.50 1 calc PR D 2 C28 C 1.2883(4) 0.0294(5) 0.5847(2) 0.0753(13) Uani 1 1 d . E . H28A H 1.3294 -0.0460 0.5733 0.090 Uiso 1 1 calc R . . H28B H 1.3291 0.0622 0.5499 0.090 Uiso 1 1 calc R . . C29 C 1.3782(5) -0.1823(4) 0.8131(3) 0.0791(13) Uani 1 1 d . . . H29B H 1.4447 -0.2054 0.7716 0.119 Uiso 1 1 calc R . . H29A H 1.3050 -0.1824 0.7992 0.119 Uiso 1 1 calc R . . H29C H 1.4020 -0.2291 0.8520 0.119 Uiso 1 1 calc R . . C30 C 1.3012(3) 0.0520(4) 0.6615(2) 0.0695(13) Uani 1 1 d . . . C31 C 1.3213(3) -0.0244(4) 0.7123(2) 0.0627(11) Uani 1 1 d . E . H31 H 1.3299 -0.0906 0.6981 0.075 Uiso 1 1 calc R . . C32 C 1.3290(3) -0.0049(4) 0.7849(2) 0.0640(12) Uani 1 1 d . . . C33 C 1.3126(3) 0.0949(4) 0.8072(2) 0.0633(12) Uani 1 1 d . E . C34 C 1.2948(3) 0.1701(4) 0.7560(2) 0.0670(12) Uani 1 1 d . . . H34 H 1.2859 0.2365 0.7698 0.080 Uiso 1 1 calc R E . C35 C 1.2899(4) 0.1487(4) 0.6834(3) 0.0734(13) Uani 1 1 d . E . C36 C 1.3412(14) 0.2700(12) 0.6201(8) 0.104(3) Uiso 0.50 1 d PD E 1 H36A H 1.4261 0.2160 0.6120 0.125 Uiso 0.50 1 calc PR E 1 H36B H 1.3300 0.3090 0.6654 0.125 Uiso 0.50 1 calc PR E 1 C38 C 1.4499(19) 0.2578(16) 0.5128(12) 0.156(5) Uiso 0.50 1 d PD E 1 H38B H 1.5142 0.2247 0.5423 0.188 Uiso 0.50 1 calc PR E 1 H38A H 1.4283 0.2039 0.4962 0.188 Uiso 0.50 1 calc PR E 1 C39 C 1.499(3) 0.299(2) 0.4494(15) 0.197(7) Uiso 0.50 1 d PD E 1 H39A H 1.4470 0.3131 0.4130 0.295 Uiso 0.50 1 calc PR E 1 H39B H 1.5820 0.2488 0.4293 0.295 Uiso 0.50 1 calc PR E 1 H39C H 1.5018 0.3635 0.4638 0.295 Uiso 0.50 1 calc PR E 1 C40 C 1.2991(15) 0.3110(12) 0.6437(9) 0.104(3) Uiso 0.50 1 d P E 2 H40B H 1.3840 0.2856 0.6521 0.125 Uiso 0.50 1 calc PR E 2 H40A H 1.2443 0.3522 0.6873 0.125 Uiso 0.50 1 calc PR E 2 C41 C 1.3335(14) 0.3425(11) 0.5616(8) 0.106(3) Uiso 0.50 1 d PD E 1 H41B H 1.3453 0.4032 0.5754 0.127 Uiso 0.50 1 calc PR E 1 H41A H 1.2582 0.3641 0.5409 0.127 Uiso 0.50 1 calc PR E 1 C42 C 1.4007(15) 0.3799(14) 0.5298(11) 0.156(5) Uiso 0.50 1 d PD E 2 H42B H 1.4707 0.3514 0.5555 0.188 Uiso 0.50 1 calc PR E 2 H42A H 1.4211 0.3363 0.4853 0.188 Uiso 0.50 1 calc PR E 2 C43 C 1.373(2) 0.4931(16) 0.5109(15) 0.197(7) Uiso 0.50 1 d PD E 2 H43B H 1.4236 0.4931 0.4648 0.295 Uiso 0.50 1 calc PR E 2 H43C H 1.3924 0.5266 0.5486 0.295 Uiso 0.50 1 calc PR E 2 H43A H 1.2870 0.5307 0.5075 0.295 Uiso 0.50 1 calc PR E 2 C44 C 1.2825(13) 0.3808(12) 0.5792(8) 0.106(3) Uiso 0.50 1 d PD E 2 H44B H 1.2301 0.4526 0.5980 0.127 Uiso 0.50 1 calc PR E 2 H44A H 1.2372 0.3614 0.5482 0.127 Uiso 0.50 1 calc PR E 2 C45 C 1.3125(3) 0.1212(4) 0.8866(2) 0.0641(12) Uani 1 1 d . . . H45B H 1.3543 0.1668 0.8875 0.077 Uiso 1 1 calc R E . H45A H 1.3588 0.0569 0.9094 0.077 Uiso 1 1 calc R . . C46 C 1.1030(5) 0.4461(5) 0.8803(4) 0.0931(17) Uani 1 1 d . . . H46B H 1.1543 0.4730 0.8494 0.140 Uiso 1 1 calc R . . H46C H 1.0803 0.4792 0.9287 0.140 Uiso 1 1 calc R . . H46A H 1.0292 0.4609 0.8604 0.140 Uiso 1 1 calc R . . C47 C 1.1104(3) 0.2833(4) 0.9265(2) 0.0630(11) Uani 1 1 d . . . C48 C 1.1805(3) 0.1757(4) 0.9308(2) 0.0620(11) Uani 1 1 d . E . C49 C 1.1282(3) 0.1207(4) 0.9753(2) 0.0607(11) Uani 1 1 d . . . H49 H 1.1737 0.0487 0.9781 0.073 Uiso 1 1 calc R E . C50 C 1.0078(3) 0.1703(4) 1.0168(2) 0.0638(12) Uani 1 1 d . E . C51 C 0.9362(3) 0.2763(4) 1.0093(2) 0.0636(12) Uani 1 1 d . . . C52 C 0.9887(4) 0.3315(4) 0.9647(2) 0.0661(12) Uani 1 1 d . E . H52 H 0.9417 0.4029 0.9599 0.079 Uiso 1 1 calc R . . C53 C 1.0373(4) 0.0240(5) 1.0923(3) 0.0789(14) Uani 1 1 d . . . H53B H 1.1043 0.0347 1.1077 0.095 Uiso 1 1 calc R . . H53A H 1.0733 -0.0323 1.0543 0.095 Uiso 1 1 calc R . . C54 C 0.9666(6) -0.0055(5) 1.1558(3) 0.0888(16) Uani 1 1 d . G . H54B H 0.9456 0.0450 1.1964 0.107 Uiso 1 1 calc R . . H54A H 0.8890 0.0017 1.1425 0.107 Uiso 1 1 calc R . . C55 C 1.0273(8) -0.1095(7) 1.1814(4) 0.123(2) Uani 1 1 d D . . H55C H 1.0199 -0.1497 1.1422 0.148 Uiso 0.25 1 calc PR F 2 H55D H 1.1127 -0.1182 1.1698 0.148 Uiso 0.25 1 calc PR F 2 H55A H 1.0483 -0.1607 1.1413 0.148 Uiso 0.75 1 calc PR F 1 H55B H 0.9695 -0.1209 1.2199 0.148 Uiso 0.75 1 calc PR F 1 C56 C 1.1398(6) -0.1278(7) 1.2096(4) 0.088(2) Uani 0.75 1 d PD G 1 H56A H 1.2036 -0.1305 1.1698 0.132 Uiso 0.75 1 calc PR G 1 H56B H 1.1673 -0.1933 1.2332 0.132 Uiso 0.75 1 calc PR G 1 H56C H 1.1227 -0.0716 1.2443 0.132 Uiso 0.75 1 calc PR G 1 C57 C 1.0408(17) -0.1823(16) 1.2366(9) 0.076(5) Uani 0.25 1 d PD G 2 H57C H 1.0113 -0.1454 1.2839 0.114 Uiso 0.25 1 calc PR G 2 H57B H 1.1270 -0.2302 1.2328 0.114 Uiso 0.25 1 calc PR G 2 H57A H 0.9933 -0.2209 1.2307 0.114 Uiso 0.25 1 calc PR G 2 C58 C 0.8016(3) 0.3300(4) 1.0488(2) 0.0670(12) Uani 1 1 d . E . H58B H 0.7853 0.3985 1.0692 0.080 Uiso 1 1 calc R . . H58A H 0.7885 0.2883 1.0889 0.080 Uiso 1 1 calc R . . C59 C 0.7112(3) 0.3431(4) 0.9963(2) 0.0692(13) Uani 1 1 d . . . C60 C 0.6735(3) 0.2638(4) 0.9883(2) 0.0719(13) Uani 1 1 d . E . H60 H 0.7030 0.2038 1.0149 0.086 Uiso 1 1 calc R . . C61 C 0.5906(3) 0.2739(5) 0.9399(2) 0.0761(14) Uani 1 1 d . . . C62 C 0.5459(3) 0.3619(5) 0.9001(2) 0.0747(14) Uani 1 1 d . E . C63 C 0.5846(4) 0.4390(5) 0.9084(2) 0.0770(15) Uani 1 1 d . . . H63 H 0.5556 0.4987 0.8814 0.092 Uiso 1 1 calc R E . C64 C 0.6656(3) 0.4311(4) 0.9557(2) 0.0720(13) Uani 1 1 d . E . C65 C 0.5916(5) 0.1087(6) 0.9686(4) 0.104(2) Uani 1 1 d . . . H65B H 0.6800 0.0709 0.9537 0.155 Uiso 1 1 calc R E . H65A H 0.5520 0.0648 0.9590 0.155 Uiso 1 1 calc R . . H65C H 0.5727 0.1279 1.0201 0.155 Uiso 1 1 calc R . . C66 C 0.6723(5) 0.5934(5) 0.9203(3) 0.0941(18) Uani 1 1 d . . . H66B H 0.5823 0.6305 0.9277 0.113 Uiso 1 1 calc R . . H66A H 0.7024 0.5687 0.8692 0.113 Uiso 1 1 calc R . . C67 C 0.7258(6) 0.6653(6) 0.9388(5) 0.117(2) Uani 1 1 d . . . H67A H 0.8147 0.6279 0.9379 0.140 Uiso 1 1 calc R . . H67B H 0.6858 0.7011 0.9866 0.140 Uiso 1 1 calc R . . C68 C 0.6964(12) 0.7436(9) 0.8762(7) 0.169(4) Uiso 1 1 d D . . H68A H 0.7440 0.7090 0.8291 0.203 Uiso 1 1 calc R . . H68B H 0.6084 0.7741 0.8735 0.203 Uiso 1 1 calc R . . C69 C 0.7339(16) 0.8238(12) 0.8978(10) 0.241(7) Uiso 1 1 d D . . H69A H 0.6809 0.8909 0.8821 0.361 Uiso 1 1 calc R . . H69B H 0.8186 0.8055 0.8753 0.361 Uiso 1 1 calc R . . H69C H 0.7267 0.8274 0.9502 0.361 Uiso 1 1 calc R . . C70 C 0.4599(4) 0.3730(5) 0.8462(3) 0.0853(16) Uani 1 1 d . . . H70B H 0.4053 0.4467 0.8434 0.102 Uiso 1 1 calc R E . H70A H 0.4085 0.3365 0.8634 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.159(4) 0.102(3) 0.080(3) -0.017(2) -0.009(3) -0.021(3) O2 0.076(2) 0.113(3) 0.119(3) -0.035(3) 0.018(2) -0.041(2) O3 0.077(2) 0.111(3) 0.097(3) 0.013(2) -0.0355(19) -0.030(2) O4 0.0765(19) 0.096(2) 0.0616(18) -0.0040(16) -0.0183(15) -0.0325(19) O5 0.115(3) 0.133(3) 0.085(2) 0.033(2) -0.052(2) -0.079(3) O6 0.0574(15) 0.087(2) 0.0545(16) -0.0101(15) -0.0131(12) -0.0154(14) O7 0.0475(14) 0.087(2) 0.091(2) -0.0240(17) 0.0055(14) -0.0290(15) O8 0.0461(14) 0.104(2) 0.0565(16) -0.0042(15) -0.0060(12) -0.0203(15) O9 0.0476(15) 0.101(2) 0.0677(18) -0.0093(17) -0.0090(13) -0.0104(16) O10 0.0519(16) 0.128(3) 0.082(2) -0.004(2) -0.0293(15) -0.0294(18) C2 0.076(3) 0.097(4) 0.066(3) -0.015(3) -0.022(2) -0.010(3) C3 0.044(2) 0.107(4) 0.058(3) -0.009(3) -0.0205(18) -0.008(2) C4 0.043(2) 0.127(5) 0.066(3) -0.008(3) -0.0068(18) -0.023(2) C5 0.045(2) 0.105(4) 0.081(3) -0.021(3) -0.006(2) -0.017(2) C6 0.048(2) 0.110(4) 0.056(2) -0.008(3) -0.0154(18) -0.020(2) C7 0.075(3) 0.113(4) 0.056(2) -0.002(3) -0.018(2) -0.028(3) C8 0.071(3) 0.103(5) 0.178(8) -0.028(5) 0.004(4) -0.023(3) C14 0.057(2) 0.123(4) 0.055(2) -0.013(2) -0.0167(18) -0.024(3) C16 0.064(3) 0.105(4) 0.053(2) -0.005(2) -0.0188(19) -0.022(3) C17 0.054(2) 0.107(4) 0.046(2) -0.020(2) -0.0103(17) -0.020(3) C18 0.059(2) 0.110(4) 0.045(2) -0.021(2) -0.0075(17) -0.031(3) C19 0.064(2) 0.098(3) 0.0407(19) -0.016(2) -0.0104(17) -0.026(2) C20 0.053(2) 0.103(4) 0.045(2) -0.016(2) -0.0069(17) -0.022(2) C21 0.064(2) 0.108(4) 0.049(2) -0.003(2) -0.0142(18) -0.031(3) C22 0.121(4) 0.122(4) 0.066(3) -0.002(3) -0.028(3) -0.060(4) C23 0.157(5) 0.143(5) 0.105(4) 0.008(4) -0.043(4) -0.073(4) C28 0.056(2) 0.110(4) 0.050(2) -0.008(2) -0.0096(17) -0.025(2) C29 0.078(3) 0.087(3) 0.062(3) -0.010(2) -0.016(2) -0.024(2) C30 0.0425(19) 0.102(4) 0.051(2) -0.011(2) -0.0112(16) -0.017(2) C31 0.0376(17) 0.082(3) 0.052(2) -0.012(2) -0.0056(15) -0.0108(17) C32 0.0333(17) 0.090(3) 0.057(2) -0.015(2) -0.0063(15) -0.0150(18) C33 0.0288(16) 0.093(3) 0.057(2) -0.014(2) -0.0075(14) -0.0141(17) C34 0.0437(19) 0.089(3) 0.064(2) -0.009(2) -0.0153(17) -0.0215(19) C35 0.054(2) 0.095(4) 0.071(3) 0.004(3) -0.0209(19) -0.028(2) C45 0.0318(16) 0.096(3) 0.058(2) -0.019(2) -0.0075(15) -0.0203(18) C46 0.079(3) 0.087(4) 0.107(4) -0.022(3) 0.013(3) -0.038(3) C47 0.0430(19) 0.085(3) 0.060(2) -0.019(2) -0.0061(16) -0.025(2) C48 0.0358(17) 0.093(3) 0.052(2) -0.020(2) -0.0063(15) -0.022(2) C49 0.0377(17) 0.082(3) 0.054(2) -0.0092(19) -0.0120(15) -0.0154(18) C50 0.0396(18) 0.097(3) 0.049(2) -0.012(2) -0.0096(15) -0.022(2) C51 0.0378(18) 0.092(3) 0.054(2) -0.020(2) -0.0095(16) -0.019(2) C52 0.047(2) 0.084(3) 0.062(2) -0.017(2) -0.0085(18) -0.022(2) C53 0.063(2) 0.111(4) 0.058(2) -0.003(2) -0.014(2) -0.031(3) C54 0.098(4) 0.125(5) 0.055(3) 0.000(3) -0.016(2) -0.058(3) C55 0.136(6) 0.162(7) 0.085(4) 0.002(5) -0.030(4) -0.071(5) C56 0.059(3) 0.121(6) 0.070(4) -0.001(4) -0.001(3) -0.028(4) C57 0.067(10) 0.093(13) 0.049(9) 0.009(9) -0.007(7) -0.018(9) C58 0.0393(18) 0.100(3) 0.051(2) -0.020(2) -0.0048(15) -0.0201(19) C59 0.0324(17) 0.101(3) 0.055(2) -0.020(2) -0.0023(15) -0.011(2) C60 0.0381(18) 0.107(4) 0.054(2) -0.015(2) -0.0073(16) -0.014(2) C61 0.0360(18) 0.121(4) 0.057(2) -0.014(3) -0.0069(17) -0.020(2) C62 0.0351(18) 0.112(4) 0.057(2) -0.018(2) -0.0079(16) -0.011(2) C63 0.0378(19) 0.112(4) 0.049(2) -0.015(2) -0.0021(15) -0.002(2) C64 0.0362(18) 0.099(3) 0.060(2) -0.024(2) 0.0021(16) -0.012(2) C65 0.065(3) 0.145(6) 0.113(4) 0.005(4) -0.040(3) -0.047(3) C66 0.057(3) 0.112(4) 0.078(3) -0.005(3) -0.002(2) -0.006(3) C67 0.076(3) 0.115(5) 0.137(6) 0.036(4) -0.019(4) -0.021(3) C70 0.044(2) 0.120(4) 0.062(3) -0.018(3) -0.0122(18) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.353(7) . ? O1 C1 1.389(15) . ? O2 C5 1.376(7) . ? O2 C8 1.387(10) . ? O3 C15 1.368(10) . ? O3 C16 1.371(7) . ? O4 C19 1.363(6) . ? O4 C22 1.387(8) . ? O5 C36 1.242(15) . ? O5 C35 1.371(7) . ? O5 C40 1.420(16) . ? O6 C32 1.389(6) . ? O6 C29 1.398(6) . ? O7 C47 1.390(6) . ? O7 C46 1.401(7) . ? O8 C50 1.374(6) . ? O8 C53 1.424(6) . ? O9 C64 1.385(6) . ? O9 C66 1.413(7) . ? O10 C61 1.380(7) . ? O10 C65 1.390(8) . ? C1 H1A 0.9600 . ? C1 H1C 0.9600 . ? C1 H1B 0.9600 . ? C2 C3 1.368(9) . ? C2 C7 1.407(7) . ? C3 C4 1.376(8) . ? C3 C70 1.524(6) . ? C4 C5 1.392(7) . ? C4 H4 0.9300 . ? C5 C6 1.393(8) . ? C6 C7 1.366(8) . ? C6 C14 1.501(6) . ? C7 H7 0.9300 . ? C8 C9 1.426(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.33(2) . ? C9 C12 1.482(9) . ? C9 H9BD 0.9700 . ? C9 H9BC 0.9700 . ? C9 H9AB 0.9700 . ? C9 H9AA 0.9700 . ? C10 C11 1.55(2) . ? C10 H10B 0.9700 . ? C10 H10A 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.524(17) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C17 1.548(6) . ? C14 H14B 0.9700 . ? C14 H14A 0.9700 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15 H15A 0.9600 . ? C16 C21 1.387(7) . ? C16 C17 1.390(8) . ? C17 C18 1.373(8) . ? C18 C19 1.401(6) . ? C18 H18 0.9300 . ? C19 C20 1.398(7) . ? C20 C21 1.392(8) . ? C20 C28 1.522(6) . ? C21 H21 0.9300 . ? C22 C23 1.484(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.572(11) . ? C23 H23B 0.9700 . ? C23 H23A 0.9700 . ? C24 C25 1.555(10) . ? C24 C26 1.583(10) . ? C24 C27 1.598(9) . ? C24 H24B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24F 0.9700 . ? C24 H24E 0.9700 . ? C24 H24C 0.9700 . ? C24 H24D 0.9700 . ? C25 H25A 0.9600 . ? C25 H25C 0.9600 . ? C25 H25B 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C26 H26A 0.9600 . ? C27 H27A 0.9600 . ? C27 H27C 0.9600 . ? C27 H27B 0.9600 . ? C28 C30 1.513(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29B 0.9600 . ? C29 H29A 0.9600 . ? C29 H29C 0.9600 . ? C30 C35 1.371(7) . ? C30 C31 1.381(7) . ? C31 C32 1.405(6) . ? C31 H31 0.9300 . ? C32 C33 1.392(7) . ? C33 C34 1.375(7) . ? C33 C45 1.525(5) . ? C34 C35 1.400(7) . ? C34 H34 0.9300 . ? C36 C41 1.457(15) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C38 C39 1.45(3) . ? C38 C41 1.55(2) . ? C38 H38B 0.9700 . ? C38 H38A 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C44 1.51(2) . ? C40 H40B 0.9700 . ? C40 H40A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41A 0.9700 . ? C42 C43 1.526(10) . ? C42 C44 1.552(9) . ? C42 H42B 0.9700 . ? C42 H42A 0.9700 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C43 H43A 0.9600 . ? C44 H44B 0.9700 . ? C44 H44A 0.9700 . ? C45 C48 1.532(5) . ? C45 H45B 0.9700 . ? C45 H45A 0.9700 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C46 H46A 0.9600 . ? C47 C52 1.393(6) . ? C47 C48 1.393(7) . ? C48 C49 1.371(7) . ? C49 C50 1.404(5) . ? C49 H49 0.9300 . ? C50 C51 1.387(7) . ? C51 C52 1.376(7) . ? C51 C58 1.524(5) . ? C52 H52 0.9300 . ? C53 C54 1.490(8) . ? C53 H53B 0.9700 . ? C53 H53A 0.9700 . ? C54 C55 1.440(10) . ? C54 H54B 0.9700 . ? C54 H54A 0.9700 . ? C55 C57 1.408(19) . ? C55 C56 1.453(10) . ? C55 H55C 0.9700 . ? C55 H55D 0.9700 . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57C 0.9600 . ? C57 H57B 0.9600 . ? C57 H57A 0.9600 . ? C58 C59 1.532(5) . ? C58 H58B 0.9700 . ? C58 H58A 0.9700 . ? C59 C64 1.384(8) . ? C59 C60 1.389(7) . ? C60 C61 1.414(6) . ? C60 H60 0.9300 . ? C61 C62 1.375(8) . ? C62 C63 1.369(8) . ? C62 C70 1.518(6) . ? C63 C64 1.389(6) . ? C63 H63 0.9300 . ? C65 H65B 0.9600 . ? C65 H65A 0.9600 . ? C65 H65C 0.9600 . ? C66 C67 1.483(10) . ? C66 H66B 0.9700 . ? C66 H66A 0.9700 . ? C67 C68 1.559(14) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.466(9) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70B 0.9700 . ? C70 H70A 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C1 117.6(8) . . ? C5 O2 C8 118.7(5) . . ? C15 O3 C16 118.2(5) . . ? C19 O4 C22 118.4(4) . . ? C36 O5 C35 121.8(7) . . ? C36 O5 C40 28.8(8) . . ? C35 O5 C40 120.3(7) . . ? C32 O6 C29 116.7(3) . . ? C47 O7 C46 118.2(3) . . ? C50 O8 C53 117.5(3) . . ? C64 O9 C66 117.2(4) . . ? C61 O10 C65 117.2(4) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? O1 C2 C3 115.6(5) . . ? O1 C2 C7 124.0(6) . . ? C3 C2 C7 120.4(6) . . ? C2 C3 C4 118.1(5) . . ? C2 C3 C70 121.8(5) . . ? C4 C3 C70 120.0(5) . . ? C3 C4 C5 122.0(6) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? O2 C5 C4 124.0(6) . . ? O2 C5 C6 116.1(5) . . ? C4 C5 C6 119.8(6) . . ? C7 C6 C5 118.1(5) . . ? C7 C6 C14 121.0(5) . . ? C5 C6 C14 120.9(5) . . ? C6 C7 C2 121.5(6) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? O2 C8 C9 111.1(8) . . ? O2 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? O2 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 108.6(13) . . ? C10 C9 C12 84.6(14) . . ? C8 C9 C12 137.1(13) . . ? C10 C9 H9BD 110.0 . . ? C8 C9 H9BD 110.0 . . ? C12 C9 H9BD 102.6 . . ? C10 C9 H9BC 110.0 . . ? C8 C9 H9BC 110.0 . . ? C12 C9 H9BC 30.8 . . ? H9BD C9 H9BC 108.3 . . ? C10 C9 H9AB 123.2 . . ? C8 C9 H9AB 102.9 . . ? C12 C9 H9AB 102.9 . . ? H9BD C9 H9AB 13.2 . . ? H9BC C9 H9AB 101.6 . . ? C10 C9 H9AA 22.9 . . ? C8 C9 H9AA 102.9 . . ? C12 C9 H9AA 102.9 . . ? H9BD C9 H9AA 92.4 . . ? H9BC C9 H9AA 131.3 . . ? H9AB C9 H9AA 105.0 . . ? C9 C10 C11 112.8(18) . . ? C9 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? H10B C10 H10A 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 C13 118.8(16) . . ? C9 C12 H12A 107.6 . . ? C13 C12 H12A 107.6 . . ? C9 C12 H12B 107.6 . . ? C13 C12 H12B 107.6 . . ? H12A C12 H12B 107.1 . . ? C6 C14 C17 110.8(3) . . ? C6 C14 H14B 109.5 . . ? C17 C14 H14B 109.5 . . ? C6 C14 H14A 109.5 . . ? C17 C14 H14A 109.5 . . ? H14B C14 H14A 108.1 . . ? O3 C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? O3 C16 C21 123.3(6) . . ? O3 C16 C17 117.2(4) . . ? C21 C16 C17 119.5(5) . . ? C18 C17 C16 119.7(4) . . ? C18 C17 C14 118.8(5) . . ? C16 C17 C14 121.5(5) . . ? C17 C18 C19 121.1(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? O4 C19 C20 116.2(4) . . ? O4 C19 C18 124.1(5) . . ? C20 C19 C18 119.7(5) . . ? C21 C20 C19 118.3(4) . . ? C21 C20 C28 121.2(5) . . ? C19 C20 C28 120.5(5) . . ? C16 C21 C20 121.7(5) . . ? C16 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? O4 C22 C23 109.5(6) . . ? O4 C22 H22A 109.8 . . ? C23 C22 H22A 109.8 . . ? O4 C22 H22B 109.8 . . ? C23 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C22 C23 C24 118.7(7) . . ? C22 C23 H23B 107.6 . . ? C24 C23 H23B 107.6 . . ? C22 C23 H23A 107.6 . . ? C24 C23 H23A 107.6 . . ? H23B C23 H23A 107.1 . . ? C25 C24 C23 114.0(12) . . ? C25 C24 C26 105.1(17) . . ? C23 C24 C26 115.8(14) . . ? C25 C24 C27 110.9(13) . . ? C23 C24 C27 109.6(9) . . ? C26 C24 C27 100.5(13) . . ? C25 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? C26 C24 H24B 103.8 . . ? C27 C24 H24B 3.5 . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C26 C24 H24A 7.1 . . ? C27 C24 H24A 104.3 . . ? H24B C24 H24A 107.6 . . ? C25 C24 H24F 104.6 . . ? C23 C24 H24F 108.3 . . ? C26 C24 H24F 108.3 . . ? C27 C24 H24F 8.7 . . ? H24B C24 H24F 5.3 . . ? H24A C24 H24F 112.5 . . ? C25 C24 H24E 5.7 . . ? C23 C24 H24E 108.3 . . ? C26 C24 H24E 108.3 . . ? C27 C24 H24E 114.3 . . ? H24B C24 H24E 111.9 . . ? H24A C24 H24E 111.4 . . ? H24F C24 H24E 107.4 . . ? C25 C24 H24C 6.0 . . ? C23 C24 H24C 109.7 . . ? C26 C24 H24C 111.0 . . ? C27 C24 H24C 109.7 . . ? H24B C24 H24C 107.3 . . ? H24A C24 H24C 114.5 . . ? H24F C24 H24C 102.8 . . ? H24E C24 H24C 4.7 . . ? C25 C24 H24D 102.5 . . ? C23 C24 H24D 109.7 . . ? C26 C24 H24D 9.4 . . ? C27 C24 H24D 109.7 . . ? H24B C24 H24D 113.1 . . ? H24A C24 H24D 6.9 . . ? H24F C24 H24D 117.7 . . ? H24E C24 H24D 105.0 . . ? H24C C24 H24D 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25C 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? C30 C28 C20 111.6(3) . . ? C30 C28 H28A 109.3 . . ? C20 C28 H28A 109.3 . . ? C30 C28 H28B 109.3 . . ? C20 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? O6 C29 H29B 109.5 . . ? O6 C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? O6 C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? C35 C30 C31 118.2(4) . . ? C35 C30 C28 121.6(5) . . ? C31 C30 C28 120.2(5) . . ? C30 C31 C32 121.7(5) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? O6 C32 C33 116.9(4) . . ? O6 C32 C31 123.6(4) . . ? C33 C32 C31 119.5(4) . . ? C34 C33 C32 118.4(4) . . ? C34 C33 C45 120.5(4) . . ? C32 C33 C45 121.1(4) . . ? C33 C34 C35 121.4(5) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? O5 C35 C30 118.0(4) . . ? O5 C35 C34 121.3(5) . . ? C30 C35 C34 120.7(5) . . ? O5 C36 C41 123.3(13) . . ? O5 C36 H36A 106.5 . . ? C41 C36 H36A 106.5 . . ? O5 C36 H36B 106.5 . . ? C41 C36 H36B 106.5 . . ? H36A C36 H36B 106.5 . . ? C39 C38 C41 113.7(19) . . ? C39 C38 H38B 108.8 . . ? C41 C38 H38B 108.8 . . ? C39 C38 H38A 108.8 . . ? C41 C38 H38A 108.8 . . ? H38B C38 H38A 107.7 . . ? O5 C40 C44 112.4(12) . . ? O5 C40 H40B 109.1 . . ? C44 C40 H40B 109.1 . . ? O5 C40 H40A 109.1 . . ? C44 C40 H40A 109.1 . . ? H40B C40 H40A 107.9 . . ? C36 C41 C38 91.5(12) . . ? C36 C41 H41B 113.4 . . ? C38 C41 H41B 113.4 . . ? C36 C41 H41A 113.4 . . ? C38 C41 H41A 113.4 . . ? H41B C41 H41A 110.7 . . ? C43 C42 C44 107.8(11) . . ? C43 C42 H42B 110.1 . . ? C44 C42 H42B 110.1 . . ? C43 C42 H42A 110.1 . . ? C44 C42 H42A 110.1 . . ? H42B C42 H42A 108.5 . . ? C42 C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C43 H43A 109.5 . . ? H43B C43 H43A 109.5 . . ? H43C C43 H43A 109.5 . . ? C40 C44 C42 118.3(13) . . ? C40 C44 H44B 107.7 . . ? C42 C44 H44B 107.7 . . ? C40 C44 H44A 107.7 . . ? C42 C44 H44A 107.7 . . ? H44B C44 H44A 107.1 . . ? C33 C45 C48 112.0(3) . . ? C33 C45 H45B 109.2 . . ? C48 C45 H45B 109.2 . . ? C33 C45 H45A 109.2 . . ? C48 C45 H45A 109.2 . . ? H45B C45 H45A 107.9 . . ? O7 C46 H46B 109.5 . . ? O7 C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O7 C46 H46A 109.5 . . ? H46B C46 H46A 109.5 . . ? H46C C46 H46A 109.5 . . ? O7 C47 C52 123.5(4) . . ? O7 C47 C48 116.5(3) . . ? C52 C47 C48 119.9(5) . . ? C49 C48 C47 118.3(4) . . ? C49 C48 C45 121.5(4) . . ? C47 C48 C45 120.2(4) . . ? C48 C49 C50 121.8(4) . . ? C48 C49 H49 119.1 . . ? C50 C49 H49 119.1 . . ? O8 C50 C51 117.5(3) . . ? O8 C50 C49 123.1(4) . . ? C51 C50 C49 119.4(4) . . ? C52 C51 C50 118.6(4) . . ? C52 C51 C58 120.8(4) . . ? C50 C51 C58 120.6(4) . . ? C51 C52 C47 121.7(5) . . ? C51 C52 H52 119.2 . . ? C47 C52 H52 119.2 . . ? O8 C53 C54 109.2(4) . . ? O8 C53 H53B 109.8 . . ? C54 C53 H53B 109.8 . . ? O8 C53 H53A 109.8 . . ? C54 C53 H53A 109.8 . . ? H53B C53 H53A 108.3 . . ? C55 C54 C53 116.9(6) . . ? C55 C54 H54B 108.1 . . ? C53 C54 H54B 108.1 . . ? C55 C54 H54A 108.1 . . ? C53 C54 H54A 108.1 . . ? H54B C54 H54A 107.3 . . ? C57 C55 C54 151.0(10) . . ? C57 C55 C56 71.8(10) . . ? C54 C55 C56 113.9(7) . . ? C57 C55 H55C 98.9 . . ? C54 C55 H55C 98.9 . . ? C56 C55 H55C 127.0 . . ? C57 C55 H55D 98.9 . . ? C54 C55 H55D 98.9 . . ? C56 C55 H55D 33.7 . . ? H55C C55 H55D 103.9 . . ? C57 C55 H55A 94.9 . . ? C54 C55 H55A 108.8 . . ? C56 C55 H55A 108.8 . . ? H55C C55 H55A 18.2 . . ? H55D C55 H55A 87.0 . . ? C57 C55 H55B 46.0 . . ? C54 C55 H55B 108.8 . . ? C56 C55 H55B 108.8 . . ? H55C C55 H55B 97.6 . . ? H55D C55 H55B 141.7 . . ? H55A C55 H55B 107.7 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? C55 C57 H57C 109.5 . . ? C55 C57 H57B 109.5 . . ? H57C C57 H57B 109.5 . . ? C55 C57 H57A 109.5 . . ? H57C C57 H57A 109.5 . . ? H57B C57 H57A 109.5 . . ? C51 C58 C59 111.0(3) . . ? C51 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? C51 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? H58B C58 H58A 108.0 . . ? C64 C59 C60 118.3(4) . . ? C64 C59 C58 122.5(5) . . ? C60 C59 C58 119.2(5) . . ? C59 C60 C61 120.2(5) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C62 C61 O10 115.5(4) . . ? C62 C61 C60 120.8(5) . . ? O10 C61 C60 123.7(5) . . ? C63 C62 C61 118.1(4) . . ? C63 C62 C70 120.2(5) . . ? C61 C62 C70 121.6(5) . . ? C62 C63 C64 122.1(5) . . ? C62 C63 H63 118.9 . . ? C64 C63 H63 118.9 . . ? C59 C64 O9 115.5(4) . . ? C59 C64 C63 120.4(5) . . ? O9 C64 C63 124.1(5) . . ? O10 C65 H65B 109.5 . . ? O10 C65 H65A 109.5 . . ? H65B C65 H65A 109.5 . . ? O10 C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? O9 C66 C67 109.3(5) . . ? O9 C66 H66B 109.8 . . ? C67 C66 H66B 109.8 . . ? O9 C66 H66A 109.8 . . ? C67 C66 H66A 109.8 . . ? H66B C66 H66A 108.3 . . ? C66 C67 C68 101.7(7) . . ? C66 C67 H67A 111.4 . . ? C68 C67 H67A 111.4 . . ? C66 C67 H67B 111.4 . . ? C68 C67 H67B 111.4 . . ? H67A C67 H67B 109.3 . . ? C69 C68 C67 103.2(11) . . ? C69 C68 H68A 111.1 . . ? C67 C68 H68A 111.1 . . ? C69 C68 H68B 111.1 . . ? C67 C68 H68B 111.1 . . ? H68A C68 H68B 109.1 . . ? 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 . . ? C62 C70 C3 110.9(3) . . ? C62 C70 H70B 109.5 . . ? C3 C70 H70B 109.5 . . ? C62 C70 H70A 109.5 . . ? C3 C70 H70A 109.5 . . ? H70B C70 H70A 108.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 67.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.153 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.071 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 782494' #TrackingRef '- CC-BMpillar-S2-new2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H80 O10' _chemical_formula_sum 'C60 H80 O10' _chemical_formula_weight 961.24 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 monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.9638(4) _cell_length_b 17.0421(3) _cell_length_c 18.6889(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.1314(16) _cell_angle_gamma 90.00 _cell_volume 5698.50(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16549 _cell_measurement_theta_min 3.58 _cell_measurement_theta_max 67.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.53 (release 17-11-2009 CrysAlis171 .NET) (compiled Nov 17 2009,16:58:22) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _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_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16549 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 67.00 _reflns_number_total 4912 _reflns_number_gt 4236 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1120P)^2^+94.1242P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00073(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4912 _refine_ls_number_parameters 331 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1553 _refine_ls_R_factor_gt 0.1460 _refine_ls_wR_factor_ref 0.3790 _refine_ls_wR_factor_gt 0.3743 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.0471(3) 0.5061(4) 0.3869(3) 0.0582(15) Uani 1 1 d . . . O2 O 0.2278(2) 0.1352(3) 0.3177(2) 0.0418(11) Uani 1 1 d . . . O3 O 0.0695(3) 0.2623(3) 0.5144(2) 0.0488(13) Uani 1 1 d . . . O4 O -0.0457(2) 0.0183(3) 0.3853(2) 0.0399(11) Uani 1 1 d . . . O5 O 0.2209(3) 0.4246(3) 0.3165(2) 0.0439(12) Uani 1 1 d . A . C1 C -0.1102(7) 0.2029(8) 0.6604(8) 0.118(5) Uani 1 1 d . . . H1A H -0.0986 0.1496 0.6492 0.176 Uiso 1 1 calc R . . H1B H -0.1628 0.2117 0.6501 0.176 Uiso 1 1 calc R . . H1C H -0.0963 0.2126 0.7104 0.176 Uiso 1 1 calc R . . C2 C 0.0723(9) 0.2940(9) 0.5840(6) 0.066(3) Uani 0.60 1 d PD A 1 H2A H 0.0567 0.3485 0.5815 0.079 Uiso 0.60 1 calc PR A 1 H2B H 0.1232 0.2921 0.6062 0.079 Uiso 0.60 1 calc PR A 1 C3 C 0.0207(8) 0.2472(10) 0.6299(7) 0.065(3) Uani 0.60 1 d PD A 1 H3B H 0.0346 0.2604 0.6798 0.079 Uiso 0.60 1 calc PR A 1 H3A H 0.0320 0.1920 0.6242 0.079 Uiso 0.60 1 calc PR A 1 C4 C -0.0679(7) 0.2572(9) 0.6160(8) 0.110(4) Uiso 1 1 d D . . H4BC H -0.1016 0.2773 0.5769 0.132 Uiso 0.40 1 calc PR A 2 H4BD H -0.0502 0.3014 0.6455 0.132 Uiso 0.40 1 calc PR A 2 H4AB H -0.0811 0.3109 0.6266 0.132 Uiso 0.60 1 calc PR A 1 H4AA H -0.0828 0.2476 0.5656 0.132 Uiso 0.60 1 calc PR A 1 C5 C -0.2268(6) 0.1359(7) 0.4848(6) 0.092(4) Uani 1 1 d . . . H5A H -0.2438 0.1430 0.4350 0.138 Uiso 1 1 calc R . . H5B H -0.1847 0.1695 0.4971 0.138 Uiso 1 1 calc R . . H5C H -0.2664 0.1490 0.5140 0.138 Uiso 1 1 calc R . . C7 C -0.1518(8) 0.4203(8) 0.3665(8) 0.049(3) Uani 0.50 1 d PD B 1 H7A H -0.1473 0.4239 0.3152 0.059 Uiso 0.50 1 calc PR B 1 H7B H -0.2041 0.4130 0.3741 0.059 Uiso 0.50 1 calc PR B 1 C11 C -0.1255(9) 0.4827(9) 0.3991(9) 0.040(2) Uiso 0.50 1 d P B 1 H11B H -0.1279 0.4751 0.4503 0.049 Uiso 0.50 1 calc PR B 1 H11A H -0.1583 0.5262 0.3847 0.049 Uiso 0.50 1 calc PR B 1 C9 C -0.2039(4) 0.0509(5) 0.4979(5) 0.061(2) Uani 1 1 d . . . H9B H -0.1742 0.0469 0.5436 0.073 Uiso 1 1 calc R . . H9A H -0.2484 0.0191 0.5005 0.073 Uiso 1 1 calc R . . C10 C 0.2771(5) 0.3853(5) 0.2820(5) 0.064(2) Uani 1 1 d . . . H10B H 0.2968 0.4199 0.2479 0.096 Uiso 1 1 calc R . . H10A H 0.2561 0.3398 0.2577 0.096 Uiso 1 1 calc R . . H10C H 0.3165 0.3696 0.3172 0.096 Uiso 1 1 calc R . . C12 C 0.1071(4) 0.5064(4) 0.3782(4) 0.0413(16) Uani 1 1 d . A . H12A H 0.1514 0.5358 0.3686 0.050 Uiso 1 1 calc R . . H12B H 0.0856 0.5310 0.4184 0.050 Uiso 1 1 calc R . . C13 C 0.2464(4) 0.1280(5) 0.2457(4) 0.0507(18) Uani 1 1 d . . . H13A H 0.2072 0.1504 0.2138 0.076 Uiso 1 1 calc R . . H13B H 0.2521 0.0736 0.2343 0.076 Uiso 1 1 calc R . . H13C H 0.2923 0.1552 0.2404 0.076 Uiso 1 1 calc R . . C14 C -0.1596(4) 0.0192(4) 0.4396(4) 0.0425(16) Uani 1 1 d . . . H14A H -0.1861 0.0305 0.3932 0.051 Uiso 1 1 calc R . . H14B H -0.1556 -0.0373 0.4444 0.051 Uiso 1 1 calc R . . C15 C 0.1806(4) 0.1792(4) 0.4500(3) 0.0365(14) Uani 1 1 d . A . H15A H 0.2335 0.1695 0.4472 0.044 Uiso 1 1 calc R . . H15B H 0.1690 0.1674 0.4986 0.044 Uiso 1 1 calc R . . C16 C 0.0759(4) 0.5102(4) 0.2440(4) 0.0441(17) Uani 1 1 d . . . H16 H 0.1270 0.5118 0.2393 0.053 Uiso 1 1 calc R . . C17 C -0.0813(4) 0.0543(4) 0.4422(4) 0.0394(15) Uani 1 1 d . . . H17A H -0.0840 0.1107 0.4354 0.047 Uiso 1 1 calc R . . H17B H -0.0538 0.0435 0.4881 0.047 Uiso 1 1 calc R . . C18 C 0.2018(3) 0.3058(4) 0.3842(3) 0.0363(14) Uani 1 1 d . A . H18 H 0.2400 0.2807 0.3625 0.044 Uiso 1 1 calc R . . C19 C -0.0254(4) 0.5088(4) 0.3179(3) 0.0394(15) Uani 1 1 d . . . C20 C 0.0506(4) 0.5092(4) 0.3121(4) 0.0387(15) Uani 1 1 d . . . C21 C 0.0916(4) 0.3822(4) 0.4488(3) 0.0387(15) Uani 1 1 d . . . H21 H 0.0547 0.4082 0.4715 0.046 Uiso 1 1 calc R A . C22 C 0.0000 -0.0217(5) 0.2500 0.0321(18) Uani 1 2 d S . . H22A H 0.0326 -0.0551 0.2247 0.039 Uiso 0.50 1 calc PR . . H22B H -0.0326 -0.0551 0.2753 0.039 Uiso 0.50 1 calc PR . . C23 C 0.0655(3) 0.0966(4) 0.4161(3) 0.0332(14) Uani 1 1 d . . . H23 H 0.0480 0.1104 0.4598 0.040 Uiso 1 1 calc R . . C24 C 0.1844(4) 0.3831(4) 0.3657(3) 0.0359(14) Uani 1 1 d . . . C25 C 0.1074(4) 0.3039(4) 0.4667(3) 0.0411(16) Uani 1 1 d . A . C26 C 0.1591(3) 0.1050(4) 0.3328(3) 0.0367(14) Uani 1 1 d . . . C27 C 0.0464(3) 0.0280(3) 0.3033(3) 0.0301(13) Uani 1 1 d . . . C28 C 0.1358(3) 0.1258(3) 0.3980(3) 0.0311(13) Uani 1 1 d . . . C29 C 0.0234(3) 0.0487(4) 0.3697(3) 0.0343(14) Uani 1 1 d . . . C30 C 0.1158(3) 0.0568(3) 0.2857(3) 0.0320(13) Uani 1 1 d . . . H30 H 0.1330 0.0434 0.2418 0.038 Uiso 1 1 calc R . . C31 C 0.1639(3) 0.2651(4) 0.4340(3) 0.0335(14) Uani 1 1 d . . . C32 C 0.1292(3) 0.4225(4) 0.3981(3) 0.0360(14) Uani 1 1 d . A . C6 C -0.1060(9) 0.3546(9) 0.3984(10) 0.065(5) Uani 0.50 1 d PD B 1 H6A H -0.0568 0.3767 0.4107 0.078 Uiso 0.50 1 calc PR B 1 H6B H -0.1262 0.3434 0.4438 0.078 Uiso 0.50 1 calc PR B 1 C8 C -0.0933(6) 0.2824(6) 0.3690(6) 0.027(2) Uiso 0.50 1 d PD B 1 H8A H -0.0513 0.2858 0.3407 0.040 Uiso 0.50 1 calc PR B 1 H8B H -0.1367 0.2664 0.3389 0.040 Uiso 0.50 1 calc PR B 1 H8C H -0.0829 0.2447 0.4067 0.040 Uiso 0.50 1 calc PR B 1 C2A C 0.0149(14) 0.2940(14) 0.5495(10) 0.066(3) Uani 0.40 1 d P A 2 H2AA H -0.0225 0.3171 0.5152 0.079 Uiso 0.40 1 calc PR A 2 H2AB H 0.0355 0.3354 0.5810 0.079 Uiso 0.40 1 calc PR A 2 C3A C -0.0223(15) 0.2311(14) 0.5946(11) 0.065(3) Uani 0.40 1 d P A 2 H3AA H -0.0387 0.1869 0.5645 0.079 Uiso 0.40 1 calc PR A 2 H3AB H 0.0132 0.2122 0.6330 0.079 Uiso 0.40 1 calc PR A 2 C51 C -0.1254(9) 0.5073(9) 0.3912(9) 0.040(2) Uiso 0.50 1 d P B 2 H51B H -0.1468 0.5509 0.3641 0.061 Uiso 0.50 1 calc PR B 2 H51C H -0.1357 0.5124 0.4405 0.061 Uiso 0.50 1 calc PR B 2 H51A H -0.1468 0.4593 0.3719 0.061 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.043(3) 0.086(4) 0.046(3) -0.026(3) 0.003(2) 0.005(3) O2 0.033(2) 0.049(3) 0.044(3) -0.006(2) 0.0080(19) -0.008(2) O3 0.059(3) 0.051(3) 0.038(3) 0.003(2) 0.015(2) -0.008(2) O4 0.041(3) 0.044(3) 0.036(2) -0.0046(19) 0.0074(19) -0.010(2) O5 0.043(3) 0.042(3) 0.047(3) 0.007(2) 0.008(2) -0.005(2) C1 0.080(8) 0.119(11) 0.154(13) 0.033(9) 0.015(8) -0.010(7) C2 0.086(9) 0.078(8) 0.033(6) 0.002(5) 0.007(5) -0.018(7) C3 0.085(10) 0.077(8) 0.037(7) 0.014(6) 0.021(6) -0.013(7) C5 0.070(7) 0.106(9) 0.100(8) -0.029(7) 0.007(6) 0.032(6) C7 0.046(8) 0.059(9) 0.041(7) 0.002(7) 0.001(6) -0.010(7) C9 0.043(4) 0.075(6) 0.066(5) -0.012(4) 0.015(4) -0.002(4) C10 0.058(5) 0.054(5) 0.084(6) 0.018(4) 0.028(4) 0.000(4) C12 0.038(4) 0.040(4) 0.045(4) 0.002(3) -0.003(3) 0.001(3) C13 0.043(4) 0.052(4) 0.060(4) -0.001(3) 0.016(3) -0.007(3) C14 0.038(4) 0.044(4) 0.045(4) 0.006(3) 0.003(3) -0.005(3) C15 0.034(3) 0.041(4) 0.034(3) 0.004(3) -0.002(3) -0.008(3) C16 0.040(4) 0.045(4) 0.047(4) 0.016(3) 0.000(3) -0.008(3) C17 0.038(4) 0.037(3) 0.043(4) 0.003(3) 0.004(3) -0.003(3) C18 0.032(3) 0.036(3) 0.039(3) -0.006(3) -0.003(3) -0.004(3) C19 0.042(4) 0.038(4) 0.037(3) -0.014(3) 0.002(3) 0.007(3) C20 0.039(4) 0.030(3) 0.046(4) 0.003(3) -0.001(3) -0.002(3) C21 0.042(4) 0.036(3) 0.038(3) -0.004(3) 0.000(3) 0.000(3) C22 0.034(5) 0.028(4) 0.034(4) 0.000 0.006(4) 0.000 C23 0.037(3) 0.035(3) 0.027(3) 0.000(2) -0.001(2) -0.004(3) C24 0.041(4) 0.036(3) 0.029(3) 0.002(2) -0.006(3) -0.010(3) C25 0.046(4) 0.038(4) 0.037(3) 0.002(3) -0.008(3) -0.010(3) C26 0.033(3) 0.035(3) 0.042(3) 0.006(3) -0.002(3) 0.004(3) C27 0.030(3) 0.026(3) 0.034(3) 0.005(2) 0.000(2) 0.001(2) C28 0.031(3) 0.030(3) 0.031(3) 0.003(2) -0.001(2) 0.003(2) C29 0.030(3) 0.032(3) 0.041(3) 0.003(3) 0.001(3) -0.003(2) C30 0.032(3) 0.032(3) 0.032(3) 0.000(2) 0.004(2) 0.003(2) C31 0.034(3) 0.036(3) 0.030(3) -0.002(2) -0.004(2) -0.005(3) C32 0.036(3) 0.032(3) 0.039(3) -0.002(3) -0.007(3) -0.004(3) C6 0.052(9) 0.063(11) 0.079(12) 0.013(9) 0.002(8) -0.017(8) C2A 0.086(9) 0.078(8) 0.033(6) 0.002(5) 0.007(5) -0.018(7) C3A 0.085(10) 0.077(8) 0.037(7) 0.014(6) 0.021(6) -0.013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C19 1.381(8) . ? O1 C51 1.416(17) . ? O1 C11 1.500(17) . ? O2 C26 1.390(8) . ? O2 C13 1.421(9) . ? O3 C2A 1.34(2) . ? O3 C25 1.366(8) . ? O3 C2 1.406(14) . ? O4 C29 1.399(7) . ? O4 C17 1.428(8) . ? O5 C24 1.372(8) . ? O5 C10 1.413(9) . ? C1 C4 1.494(17) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.540(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.598(15) . ? C3 H3B 0.9700 . ? C3 H3A 0.9700 . ? C4 C3A 1.04(3) . ? C4 H4BC 0.9700 . ? C4 H4BD 0.9700 . ? C4 H4AB 0.9700 . ? C4 H4AA 0.9700 . ? C5 C9 1.520(14) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C7 C11 1.29(2) . ? C7 C6 1.484(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C9 C14 1.505(10) . ? C9 H9B 0.9700 . ? C9 H9A 0.9700 . ? C10 H10B 0.9600 . ? C10 H10A 0.9600 . ? C10 H10C 0.9600 . ? C12 C32 1.520(9) . ? C12 C20 1.528(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C17 1.525(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C28 1.510(8) . ? C15 C31 1.518(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C20 1.389(10) . ? C16 C19 1.405(9) 2 ? C16 H16 0.9300 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C31 1.388(9) . ? C18 C24 1.391(9) . ? C18 H18 0.9300 . ? C19 C20 1.380(9) . ? C19 C16 1.405(9) 2 ? C21 C32 1.393(9) . ? C21 C25 1.398(9) . ? C21 H21 0.9300 . ? C22 C27 1.502(7) 2 ? C22 C27 1.502(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C29 1.369(8) . ? C23 C28 1.426(9) . ? C23 H23 0.9300 . ? C24 C32 1.382(9) . ? C25 C31 1.398(10) . ? C26 C28 1.371(9) . ? C26 C30 1.390(9) . ? C27 C29 1.388(9) . ? C27 C30 1.407(8) . ? C30 H30 0.9300 . ? C6 C8 1.375(18) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C2A C3A 1.55(3) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C51 H51A 0.9600 . ? 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 C19 O1 C51 114.7(8) . . ? C19 O1 C11 119.8(8) . . ? C51 O1 C11 17.2(9) . . ? C26 O2 C13 116.6(5) . . ? C2A O3 C25 122.6(11) . . ? C2A O3 C2 50.2(11) . . ? C25 O3 C2 115.2(7) . . ? C29 O4 C17 117.4(5) . . ? C24 O5 C10 117.8(5) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 C3 110.1(11) . . ? O3 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? O3 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.2 . . ? C2 C3 C4 119.6(12) . . ? C2 C3 H3B 107.4 . . ? C4 C3 H3B 107.4 . . ? C2 C3 H3A 107.4 . . ? C4 C3 H3A 107.4 . . ? H3B C3 H3A 106.9 . . ? C3A C4 C1 113.9(18) . . ? C3A C4 C3 38.0(15) . . ? C1 C4 C3 113.1(11) . . ? C3A C4 H4BC 108.8 . . ? C1 C4 H4BC 108.8 . . ? C3 C4 H4BC 135.0 . . ? C3A C4 H4BD 108.8 . . ? C1 C4 H4BD 108.8 . . ? C3 C4 H4BD 73.8 . . ? H4BC C4 H4BD 107.7 . . ? C3A C4 H4AB 134.0 . . ? C1 C4 H4AB 109.0 . . ? C3 C4 H4AB 109.0 . . ? H4BC C4 H4AB 70.8 . . ? H4BD C4 H4AB 39.1 . . ? C3A C4 H4AA 73.4 . . ? C1 C4 H4AA 109.0 . . ? C3 C4 H4AA 109.0 . . ? H4BC C4 H4AA 39.4 . . ? H4BD C4 H4AA 136.9 . . ? H4AB C4 H4AA 107.8 . . ? C9 C5 H5A 109.5 . . ? C9 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C9 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C7 C6 105.3(13) . . ? C11 C7 H7A 110.7 . . ? C6 C7 H7A 110.7 . . ? C11 C7 H7B 110.7 . . ? C6 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C7 C11 O1 117.1(14) . . ? C7 C11 H11B 108.0 . . ? O1 C11 H11B 108.0 . . ? C7 C11 H11A 108.0 . . ? O1 C11 H11A 108.0 . . ? H11B C11 H11A 107.3 . . ? C14 C9 C5 112.2(8) . . ? C14 C9 H9B 109.2 . . ? C5 C9 H9B 109.2 . . ? C14 C9 H9A 109.2 . . ? C5 C9 H9A 109.2 . . ? H9B C9 H9A 107.9 . . ? O5 C10 H10B 109.5 . . ? O5 C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? O5 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? C32 C12 C20 111.5(5) . . ? C32 C12 H12A 109.3 . . ? C20 C12 H12A 109.3 . . ? C32 C12 H12B 109.3 . . ? C20 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? O2 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 C17 112.5(6) . . ? C9 C14 H14A 109.1 . . ? C17 C14 H14A 109.1 . . ? C9 C14 H14B 109.1 . . ? C17 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C28 C15 C31 111.7(5) . . ? C28 C15 H15A 109.3 . . ? C31 C15 H15A 109.3 . . ? C28 C15 H15B 109.3 . . ? C31 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C20 C16 C19 121.0(6) . 2 ? C20 C16 H16 119.5 . . ? C19 C16 H16 119.5 2 . ? O4 C17 C14 106.3(5) . . ? O4 C17 H17A 110.5 . . ? C14 C17 H17A 110.5 . . ? O4 C17 H17B 110.5 . . ? C14 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? C31 C18 C24 121.8(6) . . ? C31 C18 H18 119.1 . . ? C24 C18 H18 119.1 . . ? C20 C19 O1 116.0(6) . . ? C20 C19 C16 120.3(6) . 2 ? O1 C19 C16 123.7(6) . 2 ? C19 C20 C16 118.7(6) . . ? C19 C20 C12 121.7(6) . . ? C16 C20 C12 119.6(6) . . ? C32 C21 C25 122.2(6) . . ? C32 C21 H21 118.9 . . ? C25 C21 H21 118.9 . . ? C27 C22 C27 111.4(7) 2 . ? C27 C22 H22A 109.4 2 . ? C27 C22 H22A 109.4 . . ? C27 C22 H22B 109.4 2 . ? C27 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C29 C23 C28 120.6(6) . . ? C29 C23 H23 119.7 . . ? C28 C23 H23 119.7 . . ? O5 C24 C32 116.7(6) . . ? O5 C24 C18 122.9(6) . . ? C32 C24 C18 120.4(6) . . ? O3 C25 C31 117.6(6) . . ? O3 C25 C21 123.3(7) . . ? C31 C25 C21 119.1(6) . . ? C28 C26 O2 115.6(5) . . ? C28 C26 C30 121.2(6) . . ? O2 C26 C30 123.2(6) . . ? C29 C27 C30 117.5(5) . . ? C29 C27 C22 123.0(5) . . ? C30 C27 C22 119.4(5) . . ? C26 C28 C23 117.9(5) . . ? C26 C28 C15 122.8(6) . . ? C23 C28 C15 119.4(5) . . ? C23 C29 C27 121.7(6) . . ? C23 C29 O4 122.6(6) . . ? C27 C29 O4 115.6(5) . . ? C26 C30 C27 121.0(6) . . ? C26 C30 H30 119.5 . . ? C27 C30 H30 119.5 . . ? C18 C31 C25 118.5(6) . . ? C18 C31 C15 120.9(6) . . ? C25 C31 C15 120.5(6) . . ? C24 C32 C21 118.0(6) . . ? C24 C32 C12 122.1(6) . . ? C21 C32 C12 119.9(6) . . ? C8 C6 C7 128.3(15) . . ? C8 C6 H6A 105.2 . . ? C7 C6 H6A 105.2 . . ? C8 C6 H6B 105.2 . . ? C7 C6 H6B 105.2 . . ? H6A C6 H6B 105.9 . . ? O3 C2A C3A 110.9(19) . . ? O3 C2A H2AA 109.5 . . ? C3A C2A H2AA 109.5 . . ? O3 C2A H2AB 109.5 . . ? C3A C2A H2AB 109.5 . . ? H2AA C2A H2AB 108.0 . . ? C4 C3A C2A 108(2) . . ? C4 C3A H3AA 110.2 . . ? C2A C3A H3AA 110.2 . . ? C4 C3A H3AB 110.2 . . ? C2A C3A H3AB 110.2 . . ? H3AA C3A H3AB 108.5 . . ? O1 C51 H51B 109.5 . . ? O1 C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O1 C51 H51A 109.5 . . ? H51B C51 H51A 109.5 . . ? H51C C51 H51A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.522 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.114 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 782495' #TrackingRef '- CC-BMpillar-S2-new2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H80 O10' _chemical_formula_sum 'C60 H80 O10' _chemical_formula_weight 961.24 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.96204(12) _cell_length_b 12.44483(17) _cell_length_c 40.2960(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.4743(12) _cell_angle_gamma 90.00 _cell_volume 5993.09(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30540 _cell_measurement_theta_min 3.70 _cell_measurement_theta_max 67.06 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type multi-scan' _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _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_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30540 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 67.06 _reflns_number_total 10596 _reflns_number_gt 7468 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1510P)^2^+3.4897P] 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 10596 _refine_ls_number_parameters 631 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2632 _refine_ls_wR_factor_gt 0.2458 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.0359(2) -0.1805(2) 0.10800(7) 0.0623(7) Uani 1 1 d . . . O2 O 0.31164(19) 0.2100(2) 0.25013(7) 0.0515(6) Uani 1 1 d . . . O3 O 0.2836(2) 0.3992(2) 0.05316(8) 0.0627(7) Uani 1 1 d . . . O4 O -0.10180(19) 0.23358(18) 0.08823(6) 0.0471(6) Uani 1 1 d . . . O5 O 0.19507(18) -0.2081(2) 0.21779(7) 0.0518(6) Uani 1 1 d . . . O6 O 0.5528(2) 0.04000(19) 0.07145(6) 0.0503(6) Uani 1 1 d . . . O7 O 0.5304(2) 0.35926(19) 0.15637(6) 0.0481(6) Uani 1 1 d . . . O8 O 0.58231(19) -0.06596(19) 0.19365(6) 0.0480(6) Uani 1 1 d . . . O9 O -0.08479(19) 0.1271(2) 0.20536(6) 0.0486(6) Uani 1 1 d . . . O10 O 0.18357(18) -0.00567(19) 0.01270(6) 0.0450(5) Uani 1 1 d . . . C1 C 0.0851(10) -0.5135(6) 0.1825(2) 0.169(5) Uani 1 1 d . . . H1A H 0.0503 -0.5169 0.1606 0.254 Uiso 1 1 calc R . . H1B H 0.0284 -0.5095 0.1986 0.254 Uiso 1 1 calc R . . H1C H 0.1297 -0.5766 0.1864 0.254 Uiso 1 1 calc R . . C2 C 0.6182(6) -0.3481(5) 0.0568(2) 0.109(2) Uani 1 1 d . . . H2A H 0.5887 -0.4096 0.0450 0.163 Uiso 1 1 calc R . . H2B H 0.6168 -0.3609 0.0802 0.163 Uiso 1 1 calc R . . H2C H 0.6940 -0.3358 0.0507 0.163 Uiso 1 1 calc R . . C3 C 0.5447(7) 0.5459(4) 0.16534(14) 0.108(2) Uani 1 1 d . . . H3A H 0.4825 0.5618 0.1499 0.129 Uiso 1 1 calc R . . H3B H 0.5458 0.6007 0.1825 0.129 Uiso 1 1 calc R . . C4 C -0.0600(8) -0.3529(7) 0.06146(18) 0.143(4) Uani 1 1 d D . . H4A H -0.0893 -0.2837 0.0542 0.171 Uiso 1 1 calc R . . H4B H -0.1170 -0.3879 0.0741 0.171 Uiso 1 1 calc R . . C5 C 0.6498(9) 0.5545(5) 0.14727(16) 0.125(3) Uani 1 1 d . . . H5A H 0.6463 0.5060 0.1284 0.150 Uiso 1 1 calc R . . H5B H 0.6572 0.6271 0.1389 0.150 Uiso 1 1 calc R . . C6 C 0.7492(7) 0.5281(7) 0.16888(18) 0.127(3) Uani 1 1 d . . . H6A H 0.8155 0.5352 0.1565 0.190 Uiso 1 1 calc R . . H6B H 0.7432 0.4556 0.1767 0.190 Uiso 1 1 calc R . . H6C H 0.7533 0.5764 0.1875 0.190 Uiso 1 1 calc R . . C7 C 0.1599(7) -0.4133(5) 0.1853(2) 0.120(3) Uani 1 1 d . . . H7A H 0.2141 -0.4169 0.1681 0.144 Uiso 1 1 calc R . . H7B H 0.1137 -0.3505 0.1809 0.144 Uiso 1 1 calc R . . C8 C 0.0364(7) -0.3362(6) 0.0826(2) 0.135(3) Uani 1 1 d DU . . H8A H 0.0904 -0.2954 0.0704 0.162 Uiso 1 1 calc R . . H8B H 0.0697 -0.4055 0.0878 0.162 Uiso 1 1 calc R . . C9 C 0.5494(4) -0.2526(4) 0.04804(14) 0.0767(13) Uani 1 1 d . . . H9A H 0.4728 -0.2667 0.0538 0.092 Uiso 1 1 calc R . . H9B H 0.5495 -0.2420 0.0242 0.092 Uiso 1 1 calc R . . C10 C -0.0385(6) -0.4192(4) 0.03176(13) 0.0856(15) Uani 1 1 d . . . H10A H -0.1006 -0.4130 0.0160 0.128 Uiso 1 1 calc R . . H10B H -0.0293 -0.4930 0.0382 0.128 Uiso 1 1 calc R . . H10C H 0.0284 -0.3944 0.0219 0.128 Uiso 1 1 calc R . . C11 C 0.2206(4) -0.3984(4) 0.21742(14) 0.0777(13) Uani 1 1 d . . . H11A H 0.2759 -0.4549 0.2205 0.093 Uiso 1 1 calc R . . H11B H 0.1684 -0.4046 0.2351 0.093 Uiso 1 1 calc R . . C12 C 0.3128(6) 0.4937(4) 0.0707(2) 0.116(3) Uani 1 1 d . . . H12A H 0.2586 0.5486 0.0654 0.175 Uiso 1 1 calc R . . H12B H 0.3854 0.5173 0.0645 0.175 Uiso 1 1 calc R . . H12C H 0.3144 0.4794 0.0941 0.175 Uiso 1 1 calc R . . C13 C 0.0165(6) -0.2785(4) 0.11452(14) 0.0937(18) Uani 1 1 d . . . H13A H -0.0300 -0.3224 0.1283 0.112 Uiso 1 1 calc R . . H13B H 0.0873 -0.2665 0.1266 0.112 Uiso 1 1 calc R . . C14 C -0.0807(4) 0.3436(3) 0.09339(13) 0.0682(11) Uani 1 1 d . . . H14A H -0.1377 0.3735 0.1067 0.102 Uiso 1 1 calc R . . H14B H -0.0812 0.3798 0.0724 0.102 Uiso 1 1 calc R . . H14C H -0.0089 0.3525 0.1046 0.102 Uiso 1 1 calc R . . C15 C 0.5229(4) 0.4393(3) 0.18135(10) 0.0612(10) Uani 1 1 d . . . H15A H 0.5778 0.4259 0.1993 0.073 Uiso 1 1 calc R . . H15B H 0.4490 0.4386 0.1904 0.073 Uiso 1 1 calc R . . C16 C 0.2254(4) 0.2876(3) 0.25234(13) 0.0670(11) Uani 1 1 d . . . H16A H 0.2577 0.3560 0.2582 0.100 Uiso 1 1 calc R . . H16B H 0.1751 0.2660 0.2690 0.100 Uiso 1 1 calc R . . H16C H 0.1852 0.2933 0.2313 0.100 Uiso 1 1 calc R . . C17 C 0.2469(4) -0.2933(3) -0.00469(13) 0.0684(11) Uani 1 1 d . . . H17A H 0.2554 -0.3141 0.0185 0.082 Uiso 1 1 calc R . . H17B H 0.1719 -0.3131 -0.0125 0.082 Uiso 1 1 calc R . . C18 C 0.5881(4) -0.1494(3) 0.06506(12) 0.0631(10) Uani 1 1 d . . . H18A H 0.5853 -0.1581 0.0889 0.076 Uiso 1 1 calc R . . H18B H 0.6652 -0.1352 0.0599 0.076 Uiso 1 1 calc R . . C19 C 0.2779(3) -0.2913(3) 0.21993(12) 0.0603(10) Uani 1 1 d . . . H19A H 0.3205 -0.2861 0.2409 0.072 Uiso 1 1 calc R . . H19B H 0.3291 -0.2836 0.2021 0.072 Uiso 1 1 calc R . . C20 C 0.3298(4) -0.3555(4) -0.02416(14) 0.0795(14) Uani 1 1 d . . . H20A H 0.3170 -0.4310 -0.0215 0.119 Uiso 1 1 calc R . . H20B H 0.4044 -0.3381 -0.0162 0.119 Uiso 1 1 calc R . . H20C H 0.3209 -0.3369 -0.0472 0.119 Uiso 1 1 calc R . . C21 C 0.5175(3) -0.0565(3) 0.05442(10) 0.0557(9) Uani 1 1 d . . . H21A H 0.5222 -0.0462 0.0307 0.067 Uiso 1 1 calc R . . H21B H 0.4401 -0.0714 0.0590 0.067 Uiso 1 1 calc R . . C22 C 0.6383(4) -0.1378(3) 0.17219(11) 0.0599(10) Uani 1 1 d . . . H22A H 0.6418 -0.2081 0.1820 0.090 Uiso 1 1 calc R . . H22B H 0.7129 -0.1122 0.1691 0.090 Uiso 1 1 calc R . . H22C H 0.5980 -0.1414 0.1511 0.090 Uiso 1 1 calc R . . C23 C 0.2238(3) 0.2154(3) 0.01591(8) 0.0428(7) Uani 1 1 d . . . H23A H 0.2026 0.2875 0.0090 0.051 Uiso 1 1 calc R . . H23B H 0.2404 0.1744 -0.0037 0.051 Uiso 1 1 calc R . . C24 C 0.4868(2) 0.0693(3) 0.23945(8) 0.0416(7) Uani 1 1 d . . . H24A H 0.4956 0.1260 0.2559 0.050 Uiso 1 1 calc R . . H24B H 0.5336 0.0094 0.2468 0.050 Uiso 1 1 calc R . . C25 C -0.1360(4) 0.2262(3) 0.19663(10) 0.0588(10) Uani 1 1 d . . . H25A H -0.1377 0.2714 0.2159 0.088 Uiso 1 1 calc R . . H25B H -0.2110 0.2135 0.1881 0.088 Uiso 1 1 calc R . . H25C H -0.0940 0.2610 0.1799 0.088 Uiso 1 1 calc R . . C26 C 0.0196(2) -0.0647(3) 0.22518(9) 0.0439(8) Uani 1 1 d . . . H26A H 0.0123 -0.1404 0.2304 0.053 Uiso 1 1 calc R . . H26B H -0.0251 -0.0244 0.2404 0.053 Uiso 1 1 calc R . . C27 C 0.6127(2) 0.2215(3) 0.10908(8) 0.0369(7) Uani 1 1 d . . . H27A H 0.6713 0.1762 0.1008 0.044 Uiso 1 1 calc R . . H27B H 0.6417 0.2942 0.1109 0.044 Uiso 1 1 calc R . . C28 C 0.0260(2) 0.0046(3) 0.04906(8) 0.0383(7) Uani 1 1 d . . . H28A H 0.0158 -0.0695 0.0480 0.046 Uiso 1 1 calc R . . C29 C -0.0133(2) -0.1236(3) 0.16574(9) 0.0445(8) Uani 1 1 d . . . H29A H 0.0187 -0.1893 0.1717 0.053 Uiso 1 1 calc R . . C30 C 0.2588(3) -0.1714(3) -0.00708(9) 0.0495(8) Uani 1 1 d . . . H30A H 0.3329 -0.1497 0.0011 0.059 Uiso 1 1 calc R . . H30B H 0.2492 -0.1487 -0.0301 0.059 Uiso 1 1 calc R . . C31 C -0.1114(2) 0.0686(2) 0.14769(8) 0.0367(7) Uani 1 1 d . . . H31A H -0.1453 0.1336 0.1419 0.044 Uiso 1 1 calc R . . C32 C -0.1346(2) 0.0122(3) 0.08740(8) 0.0373(7) Uani 1 1 d . . . H32A H -0.1542 -0.0555 0.0767 0.045 Uiso 1 1 calc R . . H32B H -0.2009 0.0571 0.0867 0.045 Uiso 1 1 calc R . . C33 C 0.3946(3) 0.1301(3) 0.04341(8) 0.0406(7) Uani 1 1 d . . . H33A H 0.3780 0.0690 0.0309 0.049 Uiso 1 1 calc R . . C34 C 0.3543(3) 0.3114(3) 0.05795(9) 0.0423(7) Uani 1 1 d . . . C35 C 0.5122(2) 0.2165(3) 0.19754(8) 0.0392(7) Uani 1 1 d . . . H35A H 0.4837 0.2646 0.2127 0.047 Uiso 1 1 calc R . . C36 C 0.1683(2) 0.0737(3) 0.23813(8) 0.0413(7) Uani 1 1 d . . . H36A H 0.1114 0.1233 0.2411 0.050 Uiso 1 1 calc R . . C37 C 0.3379(2) -0.0719(3) 0.22945(8) 0.0395(7) Uani 1 1 d . . . H37A H 0.3948 -0.1216 0.2268 0.047 Uiso 1 1 calc R . . C38 C 0.1718(3) -0.1199(3) 0.01323(9) 0.0453(8) Uani 1 1 d . . . H38A H 0.0980 -0.1396 0.0044 0.054 Uiso 1 1 calc R . . H38B H 0.1796 -0.1455 0.0360 0.054 Uiso 1 1 calc R . . C39 C 0.1113(2) 0.0522(3) 0.03150(8) 0.0379(7) Uani 1 1 d . . . C40 C 0.2269(2) -0.1053(3) 0.22580(8) 0.0391(7) Uani 1 1 d . . . C41 C -0.0277(2) 0.1763(3) 0.06936(8) 0.0382(7) Uani 1 1 d . . . C42 C 0.4461(3) 0.3112(3) 0.07992(8) 0.0406(7) Uani 1 1 d . . . H42A H 0.4637 0.3730 0.0920 0.049 Uiso 1 1 calc R . . C43 C 0.5128(2) 0.2201(2) 0.08443(7) 0.0341(6) Uani 1 1 d . . . C44 C -0.0485(3) -0.1061(3) 0.13283(9) 0.0423(7) Uani 1 1 d . . . C45 C 0.4858(3) 0.1288(3) 0.06594(8) 0.0384(7) Uani 1 1 d . . . C46 C 0.5966(2) 0.0756(2) 0.15219(8) 0.0369(7) Uani 1 1 d . . . H46A H 0.6245 0.0273 0.1370 0.044 Uiso 1 1 calc R . . C47 C -0.0251(2) -0.0452(3) 0.18999(8) 0.0389(7) Uani 1 1 d . . . C48 C 0.0572(3) 0.2242(3) 0.05191(8) 0.0396(7) Uani 1 1 d . . . H48A H 0.0668 0.2983 0.0529 0.048 Uiso 1 1 calc R . . C49 C 0.1410(2) -0.0318(3) 0.23016(8) 0.0389(7) Uani 1 1 d . . . C50 C -0.0754(2) 0.0517(3) 0.18035(8) 0.0389(7) Uani 1 1 d . . . C51 C 0.3655(2) 0.0336(3) 0.23700(7) 0.0377(7) Uani 1 1 d . . . C52 C 0.5694(2) 0.0390(2) 0.18342(8) 0.0372(7) Uani 1 1 d . . . C53 C 0.3277(2) 0.2207(3) 0.03914(8) 0.0393(7) Uani 1 1 d . . . C54 C 0.2794(3) 0.1067(3) 0.24179(8) 0.0414(7) Uani 1 1 d . . . C55 C -0.0984(2) -0.0088(2) 0.12333(8) 0.0350(6) Uani 1 1 d . . . C56 C 0.5249(2) 0.1097(3) 0.20630(8) 0.0373(7) Uani 1 1 d . . . C57 C 0.5414(2) 0.2535(3) 0.16642(8) 0.0381(7) Uani 1 1 d . . . C58 C 0.1272(2) 0.1630(3) 0.03313(8) 0.0391(7) Uani 1 1 d . . . C59 C -0.0443(2) 0.0667(3) 0.06819(7) 0.0358(6) Uani 1 1 d . . . C60 C 0.5831(2) 0.1824(3) 0.14323(7) 0.0349(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0780(17) 0.0398(14) 0.0680(17) -0.0070(12) -0.0087(13) 0.0161(13) O2 0.0417(12) 0.0496(14) 0.0628(15) -0.0095(11) -0.0012(11) -0.0013(10) O3 0.0621(15) 0.0397(14) 0.0838(19) 0.0011(12) -0.0263(14) 0.0114(12) O4 0.0501(12) 0.0320(12) 0.0596(14) -0.0033(10) 0.0076(11) 0.0033(10) O5 0.0345(11) 0.0448(14) 0.0751(17) 0.0067(12) -0.0110(11) 0.0015(10) O6 0.0532(13) 0.0427(13) 0.0537(14) -0.0122(11) -0.0123(11) 0.0129(11) O7 0.0654(14) 0.0381(12) 0.0405(12) -0.0022(10) -0.0016(10) 0.0080(11) O8 0.0462(12) 0.0385(13) 0.0594(15) 0.0079(10) 0.0033(10) 0.0006(10) O9 0.0476(12) 0.0519(14) 0.0453(13) -0.0046(10) -0.0094(10) 0.0105(11) O10 0.0399(11) 0.0473(13) 0.0474(13) -0.0080(10) -0.0008(9) 0.0017(10) C1 0.267(12) 0.082(4) 0.148(7) 0.013(4) -0.107(8) -0.061(6) C2 0.108(4) 0.067(3) 0.152(6) -0.008(4) 0.011(4) 0.011(3) C3 0.213(8) 0.045(3) 0.068(3) -0.005(2) 0.034(4) 0.009(3) C4 0.207(8) 0.125(6) 0.092(4) -0.047(4) -0.051(5) 0.076(6) C5 0.248(10) 0.058(3) 0.071(4) 0.002(3) 0.036(5) -0.019(4) C6 0.155(7) 0.143(7) 0.082(4) -0.018(4) 0.006(4) 0.013(5) C7 0.150(6) 0.069(4) 0.137(6) -0.007(4) -0.057(5) 0.014(4) C8 0.185(6) 0.095(4) 0.123(5) -0.016(4) -0.032(5) 0.064(5) C9 0.084(3) 0.055(3) 0.091(3) -0.009(2) 0.006(3) 0.000(2) C10 0.140(5) 0.054(3) 0.062(3) -0.004(2) -0.001(3) 0.012(3) C11 0.078(3) 0.056(3) 0.098(4) 0.002(2) -0.012(3) 0.006(2) C12 0.117(4) 0.051(3) 0.175(7) -0.021(3) -0.071(4) 0.034(3) C13 0.133(5) 0.063(3) 0.083(3) -0.010(2) -0.026(3) 0.042(3) C14 0.075(3) 0.040(2) 0.090(3) -0.016(2) 0.020(2) -0.0084(19) C15 0.091(3) 0.042(2) 0.051(2) -0.0059(16) 0.009(2) 0.0113(19) C16 0.058(2) 0.051(2) 0.090(3) -0.009(2) -0.016(2) 0.0087(18) C17 0.072(3) 0.055(2) 0.080(3) 0.000(2) 0.021(2) 0.006(2) C18 0.063(2) 0.056(2) 0.070(3) -0.0048(19) -0.0047(19) 0.0048(19) C19 0.0418(18) 0.053(2) 0.086(3) -0.0007(19) -0.0043(18) 0.0076(16) C20 0.087(3) 0.057(3) 0.097(4) -0.010(2) 0.027(3) 0.005(2) C21 0.062(2) 0.047(2) 0.057(2) -0.0129(16) -0.0071(17) 0.0079(17) C22 0.079(3) 0.0365(19) 0.064(2) 0.0017(17) 0.005(2) 0.0062(18) C23 0.0389(16) 0.0485(19) 0.0401(17) 0.0078(14) -0.0065(13) -0.0023(14) C24 0.0289(14) 0.0523(19) 0.0431(17) 0.0057(14) -0.0041(12) -0.0029(13) C25 0.070(2) 0.048(2) 0.057(2) -0.0137(17) -0.0148(18) 0.0134(18) C26 0.0288(14) 0.054(2) 0.0494(18) 0.0122(15) 0.0015(13) 0.0023(13) C27 0.0302(14) 0.0380(16) 0.0422(16) -0.0021(13) -0.0010(12) -0.0006(12) C28 0.0342(14) 0.0360(16) 0.0437(17) -0.0033(13) -0.0082(12) 0.0002(12) C29 0.0314(14) 0.0387(17) 0.063(2) 0.0113(15) -0.0068(14) 0.0019(13) C30 0.0449(17) 0.054(2) 0.0495(19) -0.0046(16) -0.0017(14) 0.0046(15) C31 0.0259(13) 0.0349(16) 0.0488(18) 0.0024(13) -0.0054(12) 0.0031(11) C32 0.0275(13) 0.0360(16) 0.0479(17) -0.0018(13) -0.0043(12) -0.0002(12) C33 0.0417(16) 0.0436(18) 0.0363(16) -0.0030(13) -0.0027(12) -0.0027(14) C34 0.0386(15) 0.0368(17) 0.0510(19) 0.0067(14) -0.0033(13) 0.0011(13) C35 0.0331(14) 0.0469(19) 0.0372(16) -0.0032(13) -0.0040(12) 0.0023(13) C36 0.0319(14) 0.0525(19) 0.0394(16) 0.0039(14) -0.0008(12) 0.0046(13) C37 0.0306(14) 0.0459(18) 0.0417(17) 0.0079(13) -0.0030(12) 0.0020(13) C38 0.0470(17) 0.0443(18) 0.0438(18) -0.0033(14) -0.0060(14) 0.0022(14) C39 0.0316(14) 0.0435(18) 0.0379(16) -0.0014(13) -0.0055(12) 0.0006(12) C40 0.0312(14) 0.0427(18) 0.0429(17) 0.0083(13) -0.0064(12) 0.0010(12) C41 0.0367(15) 0.0367(16) 0.0406(16) -0.0025(13) -0.0069(12) 0.0040(12) C42 0.0402(15) 0.0343(16) 0.0469(18) 0.0013(13) -0.0033(13) -0.0016(13) C43 0.0303(13) 0.0371(16) 0.0351(15) 0.0012(12) 0.0024(11) -0.0008(11) C44 0.0376(15) 0.0351(17) 0.0535(19) -0.0002(14) -0.0053(14) 0.0028(13) C45 0.0376(15) 0.0400(17) 0.0376(16) -0.0005(13) 0.0012(12) 0.0038(13) C46 0.0317(14) 0.0356(16) 0.0432(17) -0.0023(13) -0.0025(12) 0.0009(12) C47 0.0249(13) 0.0450(18) 0.0466(17) 0.0078(14) -0.0030(12) -0.0045(12) C48 0.0393(15) 0.0346(16) 0.0443(17) 0.0016(13) -0.0069(13) -0.0020(13) C49 0.0302(14) 0.0495(18) 0.0367(16) 0.0107(13) -0.0037(12) 0.0018(13) C50 0.0249(13) 0.0428(17) 0.0486(18) 0.0005(14) -0.0040(12) -0.0020(12) C51 0.0296(14) 0.0487(18) 0.0343(15) 0.0081(13) -0.0056(11) -0.0001(13) C52 0.0289(13) 0.0358(16) 0.0463(17) 0.0032(13) -0.0054(12) -0.0009(12) C53 0.0348(15) 0.0468(18) 0.0362(16) 0.0091(13) -0.0010(12) -0.0049(13) C54 0.0369(15) 0.0484(19) 0.0383(16) 0.0014(13) -0.0043(12) -0.0006(13) C55 0.0229(12) 0.0363(16) 0.0453(17) 0.0023(13) -0.0043(11) -0.0025(11) C56 0.0236(12) 0.0451(17) 0.0425(17) 0.0043(13) -0.0079(11) -0.0035(12) C57 0.0360(14) 0.0350(16) 0.0426(17) -0.0001(13) -0.0079(12) 0.0005(12) C58 0.0332(14) 0.0439(18) 0.0392(16) 0.0021(13) -0.0120(12) -0.0017(13) C59 0.0290(13) 0.0404(17) 0.0373(16) -0.0024(12) -0.0086(11) 0.0016(12) C60 0.0251(12) 0.0404(16) 0.0387(16) -0.0015(12) -0.0050(11) -0.0015(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C44 1.377(4) . ? O1 C13 1.391(5) . ? O2 C54 1.380(4) . ? O2 C16 1.418(5) . ? O3 C34 1.390(4) . ? O3 C12 1.408(6) . ? O4 C41 1.390(4) . ? O4 C14 1.405(4) . ? O5 C40 1.369(4) . ? O5 C19 1.434(4) . ? O6 C45 1.377(4) . ? O6 C21 1.438(4) . ? O7 C57 1.382(4) . ? O7 C15 1.421(4) . ? O8 C52 1.377(4) . ? O8 C22 1.431(5) . ? O9 C50 1.385(4) . ? O9 C25 1.415(4) . ? O10 C39 1.377(4) . ? O10 C38 1.428(4) . ? C1 C7 1.536(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C9 1.480(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C5 1.484(11) . ? C3 C15 1.503(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C8 1.419(8) . ? C4 C10 1.485(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.480(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C11 1.467(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.502(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C18 1.519(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C19 1.499(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C20 1.505(6) . ? C17 C30 1.527(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C21 1.483(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C58 1.520(5) . ? C23 C53 1.525(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C56 1.515(4) . ? C24 C51 1.517(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C47 1.513(5) . ? C26 C49 1.513(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C60 1.516(4) . ? C27 C43 1.521(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C59 1.398(4) . ? C28 C39 1.399(5) . ? C28 H28A 0.9300 . ? C29 C44 1.391(5) . ? C29 C47 1.392(5) . ? C29 H29A 0.9300 . ? C30 C38 1.496(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C50 1.383(5) . ? C31 C55 1.390(4) . ? C31 H31A 0.9300 . ? C32 C59 1.516(4) . ? C32 C55 1.516(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C53 1.389(5) . ? C33 C45 1.389(4) . ? C33 H33A 0.9300 . ? C34 C42 1.380(4) . ? C34 C53 1.390(5) . ? C35 C56 1.382(5) . ? C35 C57 1.395(5) . ? C35 H35A 0.9300 . ? C36 C49 1.387(5) . ? C36 C54 1.394(4) . ? C36 H36A 0.9300 . ? C37 C51 1.384(5) . ? C37 C40 1.393(4) . ? C37 H37A 0.9300 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C58 1.393(5) . ? C40 C49 1.392(5) . ? C41 C59 1.378(4) . ? C41 C48 1.393(5) . ? C42 C43 1.393(4) . ? C42 H42A 0.9300 . ? C43 C45 1.390(4) . ? C44 C55 1.395(4) . ? C46 C60 1.384(4) . ? C46 C52 1.390(5) . ? C46 H46A 0.9300 . ? C47 C50 1.396(5) . ? C48 C58 1.381(5) . ? C48 H48A 0.9300 . ? C51 C54 1.394(5) . ? C52 C56 1.396(5) . ? C57 C60 1.395(4) . ? 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 C44 O1 C13 121.0(3) . . ? C54 O2 C16 117.0(3) . . ? C34 O3 C12 116.7(3) . . ? C41 O4 C14 117.8(3) . . ? C40 O5 C19 118.5(3) . . ? C45 O6 C21 115.9(2) . . ? C57 O7 C15 117.9(3) . . ? C52 O8 C22 117.5(3) . . ? C50 O9 C25 117.2(3) . . ? C39 O10 C38 116.6(3) . . ? C7 C1 H1A 109.5 . . ? C7 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C7 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C9 C2 H2A 109.5 . . ? C9 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C9 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C5 C3 C15 116.2(5) . . ? C5 C3 H3A 108.2 . . ? C15 C3 H3A 108.2 . . ? C5 C3 H3B 108.2 . . ? C15 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C8 C4 C10 113.6(7) . . ? C8 C4 H4A 108.9 . . ? C10 C4 H4A 108.9 . . ? C8 C4 H4B 108.9 . . ? C10 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C3 111.8(6) . . ? C6 C5 H5A 109.3 . . ? C3 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C3 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C11 C7 C1 115.7(6) . . ? C11 C7 H7A 108.4 . . ? C1 C7 H7A 108.4 . . ? C11 C7 H7B 108.4 . . ? C1 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C4 C8 C13 115.4(7) . . ? C4 C8 H8A 108.4 . . ? C13 C8 H8A 108.4 . . ? C4 C8 H8B 108.4 . . ? C13 C8 H8B 108.4 . . ? H8A C8 H8B 107.5 . . ? C2 C9 C18 114.6(5) . . ? C2 C9 H9A 108.6 . . ? C18 C9 H9A 108.6 . . ? C2 C9 H9B 108.6 . . ? C18 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 C19 112.3(5) . . ? C7 C11 H11A 109.1 . . ? C19 C11 H11A 109.1 . . ? C7 C11 H11B 109.1 . . ? C19 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? O3 C12 H12A 109.5 . . ? O3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 C8 110.1(5) . . ? O1 C13 H13A 109.6 . . ? C8 C13 H13A 109.6 . . ? O1 C13 H13B 109.6 . . ? C8 C13 H13B 109.6 . . ? H13A C13 H13B 108.2 . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O7 C15 C3 107.3(3) . . ? O7 C15 H15A 110.3 . . ? C3 C15 H15A 110.3 . . ? O7 C15 H15B 110.3 . . ? C3 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C30 114.4(4) . . ? C20 C17 H17A 108.7 . . ? C30 C17 H17A 108.7 . . ? C20 C17 H17B 108.7 . . ? C30 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C21 C18 C9 111.7(4) . . ? C21 C18 H18A 109.3 . . ? C9 C18 H18A 109.3 . . ? C21 C18 H18B 109.3 . . ? C9 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? O5 C19 C11 109.0(3) . . ? O5 C19 H19A 109.9 . . ? C11 C19 H19A 109.9 . . ? O5 C19 H19B 109.9 . . ? C11 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O6 C21 C18 111.2(3) . . ? O6 C21 H21A 109.4 . . ? C18 C21 H21A 109.4 . . ? O6 C21 H21B 109.4 . . ? C18 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O8 C22 H22A 109.5 . . ? O8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C58 C23 C53 110.7(3) . . ? C58 C23 H23A 109.5 . . ? C53 C23 H23A 109.5 . . ? C58 C23 H23B 109.5 . . ? C53 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C56 C24 C51 111.3(2) . . ? C56 C24 H24A 109.4 . . ? C51 C24 H24A 109.4 . . ? C56 C24 H24B 109.4 . . ? C51 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? O9 C25 H25A 109.5 . . ? O9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C47 C26 C49 112.3(3) . . ? C47 C26 H26A 109.2 . . ? C49 C26 H26A 109.2 . . ? C47 C26 H26B 109.2 . . ? C49 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C60 C27 C43 112.4(2) . . ? C60 C27 H27A 109.1 . . ? C43 C27 H27A 109.1 . . ? C60 C27 H27B 109.1 . . ? C43 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C59 C28 C39 120.9(3) . . ? C59 C28 H28A 119.5 . . ? C39 C28 H28A 119.5 . . ? C44 C29 C47 121.6(3) . . ? C44 C29 H29A 119.2 . . ? C47 C29 H29A 119.2 . . ? C38 C30 C17 108.8(3) . . ? C38 C30 H30A 109.9 . . ? C17 C30 H30A 109.9 . . ? C38 C30 H30B 109.9 . . ? C17 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C50 C31 C55 121.8(3) . . ? C50 C31 H31A 119.1 . . ? C55 C31 H31A 119.1 . . ? C59 C32 C55 112.6(2) . . ? C59 C32 H32A 109.1 . . ? C55 C32 H32A 109.1 . . ? C59 C32 H32B 109.1 . . ? C55 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C53 C33 C45 121.5(3) . . ? C53 C33 H33A 119.2 . . ? C45 C33 H33A 119.2 . . ? C42 C34 C53 120.4(3) . . ? C42 C34 O3 123.6(3) . . ? C53 C34 O3 116.0(3) . . ? C56 C35 C57 121.2(3) . . ? C56 C35 H35A 119.4 . . ? C57 C35 H35A 119.4 . . ? C49 C36 C54 121.1(3) . . ? C49 C36 H36A 119.4 . . ? C54 C36 H36A 119.4 . . ? C51 C37 C40 121.6(3) . . ? C51 C37 H37A 119.2 . . ? C40 C37 H37A 119.2 . . ? O10 C38 C30 110.3(3) . . ? O10 C38 H38A 109.6 . . ? C30 C38 H38A 109.6 . . ? O10 C38 H38B 109.6 . . ? C30 C38 H38B 109.6 . . ? H38A C38 H38B 108.1 . . ? O10 C39 C58 117.2(3) . . ? O10 C39 C28 123.1(3) . . ? C58 C39 C28 119.8(3) . . ? O5 C40 C49 116.4(3) . . ? O5 C40 C37 123.9(3) . . ? C49 C40 C37 119.7(3) . . ? C59 C41 O4 115.6(3) . . ? C59 C41 C48 120.9(3) . . ? O4 C41 C48 123.5(3) . . ? C34 C42 C43 121.4(3) . . ? C34 C42 H42A 119.3 . . ? C43 C42 H42A 119.3 . . ? C45 C43 C42 118.5(3) . . ? C45 C43 C27 121.1(3) . . ? C42 C43 C27 120.4(3) . . ? O1 C44 C29 123.3(3) . . ? O1 C44 C55 116.3(3) . . ? C29 C44 C55 120.4(3) . . ? O6 C45 C33 123.4(3) . . ? O6 C45 C43 116.7(3) . . ? C33 C45 C43 119.9(3) . . ? C60 C46 C52 121.4(3) . . ? C60 C46 H46A 119.3 . . ? C52 C46 H46A 119.3 . . ? C29 C47 C50 117.7(3) . . ? C29 C47 C26 120.2(3) . . ? C50 C47 C26 122.0(3) . . ? C58 C48 C41 120.9(3) . . ? C58 C48 H48A 119.6 . . ? C41 C48 H48A 119.6 . . ? C36 C49 C40 118.9(3) . . ? C36 C49 C26 120.1(3) . . ? C40 C49 C26 121.0(3) . . ? C31 C50 O9 123.9(3) . . ? C31 C50 C47 120.6(3) . . ? O9 C50 C47 115.5(3) . . ? C37 C51 C54 118.6(3) . . ? C37 C51 C24 120.7(3) . . ? C54 C51 C24 120.7(3) . . ? O8 C52 C46 123.7(3) . . ? O8 C52 C56 116.2(3) . . ? C46 C52 C56 120.2(3) . . ? C33 C53 C34 118.3(3) . . ? C33 C53 C23 119.4(3) . . ? C34 C53 C23 122.1(3) . . ? O2 C54 C36 123.7(3) . . ? O2 C54 C51 116.2(3) . . ? C36 C54 C51 120.1(3) . . ? C31 C55 C44 117.9(3) . . ? C31 C55 C32 121.2(3) . . ? C44 C55 C32 120.8(3) . . ? C35 C56 C52 118.5(3) . . ? C35 C56 C24 120.7(3) . . ? C52 C56 C24 120.7(3) . . ? O7 C57 C35 123.6(3) . . ? O7 C57 C60 116.2(3) . . ? C35 C57 C60 120.2(3) . . ? C48 C58 C39 119.1(3) . . ? C48 C58 C23 120.3(3) . . ? C39 C58 C23 120.5(3) . . ? C41 C59 C28 118.4(3) . . ? C41 C59 C32 122.1(3) . . ? C28 C59 C32 119.5(3) . . ? C46 C60 C57 118.4(3) . . ? C46 C60 C27 121.1(3) . . ? C57 C60 C27 120.6(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 67.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.597 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.068 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 782496' #TrackingRef '- CC-BMpillar-S2-new2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H94 O10' _chemical_formula_sum 'C66 H94 O10' _chemical_formula_weight 1047.41 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 12.4158(4) _cell_length_b 14.2139(5) _cell_length_c 18.3290(6) _cell_angle_alpha 79.011(3) _cell_angle_beta 78.437(3) _cell_angle_gamma 75.797(3) _cell_volume 3037.87(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11522 _cell_measurement_theta_min 3.3518 _cell_measurement_theta_max 29.3294 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30321 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10666 _reflns_number_gt 6555 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10666 _refine_ls_number_parameters 667 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2809 _refine_ls_wR_factor_gt 0.2619 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.20421(18) 0.66366(17) 0.56447(13) 0.0288(6) Uani 1 1 d . . . C1 C 0.3651(9) 0.4291(10) 0.0378(7) 0.228(6) Uani 1 1 d U . . H1B H 0.4092 0.4050 -0.0068 0.342 Uiso 1 1 calc R . . H1A H 0.3281 0.3795 0.0679 0.342 Uiso 1 1 calc R . . H1C H 0.4135 0.4452 0.0663 0.342 Uiso 1 1 calc R . . C63 C 0.4646(3) 0.9237(2) 0.39368(17) 0.0205(7) Uani 1 1 d . . . O2 O -0.10503(19) 1.01438(16) 0.24178(13) 0.0296(6) Uani 1 1 d . . . C2 C 0.1852(6) 0.5305(4) 0.0773(3) 0.0882(19) Uani 1 1 d U . . H2B H 0.2039 0.4967 0.1259 0.106 Uiso 1 1 calc R . . H2A H 0.1258 0.5045 0.0665 0.106 Uiso 1 1 calc R . . O3 O 0.26334(18) 0.92451(17) 0.04591(12) 0.0274(6) Uani 1 1 d . . . C3 C 0.2866(6) 0.5109(4) 0.0182(4) 0.096(2) Uani 1 1 d U . . H3A H 0.2625 0.5040 -0.0273 0.115 Uiso 1 1 calc R . . H3B H 0.3214 0.5672 0.0067 0.115 Uiso 1 1 calc R . . O4 O -0.12593(18) 0.70534(16) 0.42914(13) 0.0280(6) Uani 1 1 d . . . C4 C 0.8706(5) 0.7281(3) -0.0254(3) 0.0724(16) Uani 1 1 d . . . H4A H 0.8180 0.7498 -0.0602 0.109 Uiso 1 1 calc R . . H4B H 0.9149 0.6643 -0.0334 0.109 Uiso 1 1 calc R . . H4C H 0.9193 0.7735 -0.0332 0.109 Uiso 1 1 calc R . . O5 O 0.60398(18) 0.90165(16) 0.17020(12) 0.0252(5) Uani 1 1 d . . . C5 C 0.2524(3) 0.7801(3) -0.1358(2) 0.0347(9) Uani 1 1 d . . . H5C H 0.2016 0.8103 -0.1709 0.052 Uiso 1 1 calc R . . H5A H 0.2205 0.7323 -0.0991 0.052 Uiso 1 1 calc R . . H5B H 0.3228 0.7483 -0.1623 0.052 Uiso 1 1 calc R . . O6 O 0.27674(18) 0.44717(16) 0.34993(12) 0.0268(6) Uani 1 1 d . . . C6 C 0.8777(4) 0.4269(3) 0.1719(3) 0.0494(11) Uani 1 1 d . . . H6A H 0.8919 0.3789 0.1388 0.074 Uiso 1 1 calc R . . H6C H 0.9323 0.4085 0.2053 0.074 Uiso 1 1 calc R . . H6B H 0.8829 0.4898 0.1427 0.074 Uiso 1 1 calc R . . O7 O 0.42133(19) 0.92787(15) 0.46917(12) 0.0249(5) Uani 1 1 d . . . C7 C 0.1416(4) 0.6423(3) 0.0815(3) 0.0523(12) Uani 1 1 d . . . H7B H 0.2031 0.6715 0.0847 0.063 Uiso 1 1 calc R . . H7A H 0.1097 0.6753 0.0368 0.063 Uiso 1 1 calc R . . O8 O 0.60097(18) 0.58999(16) 0.36300(12) 0.0242(5) Uani 1 1 d . . . C8 C 0.2721(3) 0.8583(2) -0.09643(19) 0.0288(8) Uani 1 1 d . . . H8B H 0.3009 0.9080 -0.1340 0.035 Uiso 1 1 calc R . . H8A H 0.2009 0.8897 -0.0695 0.035 Uiso 1 1 calc R . . O9 O 0.0596(2) 0.65199(17) 0.14557(14) 0.0317(6) Uani 1 1 d . . . C9 C 0.5514(3) 0.2026(3) 0.3302(2) 0.0312(8) Uani 1 1 d . . . H9A H 0.5645 0.1700 0.2869 0.047 Uiso 1 1 calc R . . H9B H 0.5586 0.1546 0.3745 0.047 Uiso 1 1 calc R . . H9C H 0.6056 0.2426 0.3242 0.047 Uiso 1 1 calc R . . O10 O 0.22645(19) 1.15760(17) 0.26281(13) 0.0305(6) Uani 1 1 d . . . C10 C 0.1763(3) 0.7509(3) 0.5970(2) 0.0445(10) Uani 1 1 d . . . H10A H 0.1739 0.8065 0.5579 0.067 Uiso 1 1 calc R . . H10C H 0.2320 0.7500 0.6268 0.067 Uiso 1 1 calc R . . H10B H 0.1039 0.7555 0.6285 0.067 Uiso 1 1 calc R . . C11 C 0.8077(4) 0.7232(3) 0.0538(2) 0.0420(10) Uani 1 1 d . . . H11B H 0.8616 0.7028 0.0885 0.050 Uiso 1 1 calc R . . H11A H 0.7631 0.6738 0.0623 0.050 Uiso 1 1 calc R . . C12 C 0.7603(3) 0.4326(3) 0.2177(2) 0.0370(9) Uani 1 1 d . . . H12A H 0.7055 0.4487 0.1837 0.044 Uiso 1 1 calc R . . H12B H 0.7554 0.3691 0.2472 0.044 Uiso 1 1 calc R . . C13 C 0.4338(3) 0.2668(2) 0.33802(19) 0.0281(8) Uani 1 1 d . . . H13A H 0.3797 0.2263 0.3422 0.034 Uiso 1 1 calc R . . H13B H 0.4189 0.2952 0.3841 0.034 Uiso 1 1 calc R . . C14 C -0.0837(3) 0.6559(2) 0.28390(19) 0.0253(8) Uani 1 1 d . . . H14B H -0.1603 0.6718 0.3104 0.030 Uiso 1 1 calc R . . H14A H -0.0803 0.6081 0.2517 0.030 Uiso 1 1 calc R . . C15 C 0.0457(3) 1.0099(2) 0.10736(18) 0.0240(7) Uani 1 1 d . . . H15B H -0.0154 1.0666 0.1146 0.029 Uiso 1 1 calc R . . H15A H 0.0617 1.0043 0.0542 0.029 Uiso 1 1 calc R . . C16 C 0.2399(3) 0.5011(2) 0.49189(18) 0.0246(7) Uani 1 1 d . . . H16A H 0.2792 0.4348 0.4847 0.029 Uiso 1 1 calc R . . H16B H 0.2019 0.4992 0.5437 0.029 Uiso 1 1 calc R . . C17 C -0.1890(3) 1.0204(3) 0.3074(2) 0.0387(9) Uani 1 1 d . . . H17A H -0.2538 1.0011 0.2991 0.058 Uiso 1 1 calc R . . H17C H -0.2101 1.0867 0.3180 0.058 Uiso 1 1 calc R . . H17B H -0.1595 0.9776 0.3494 0.058 Uiso 1 1 calc R . . C18 C 0.5671(3) 0.7510(2) 0.43867(18) 0.0220(7) Uani 1 1 d . . . H18B H 0.5658 0.7750 0.4850 0.026 Uiso 1 1 calc R . . H18A H 0.6422 0.7130 0.4242 0.026 Uiso 1 1 calc R . . C19 C -0.1489(3) 0.7343(3) 0.5013(2) 0.0320(8) Uani 1 1 d . . . H19C H -0.0912 0.7656 0.5065 0.048 Uiso 1 1 calc R . . H19A H -0.1505 0.6775 0.5391 0.048 Uiso 1 1 calc R . . H19B H -0.2206 0.7793 0.5071 0.048 Uiso 1 1 calc R . . C20 C 0.3494(3) 1.0173(2) 0.48777(19) 0.0293(8) Uani 1 1 d . . . H20A H 0.2823 1.0292 0.4659 0.044 Uiso 1 1 calc R . . H20C H 0.3875 1.0702 0.4685 0.044 Uiso 1 1 calc R . . H20B H 0.3297 1.0129 0.5415 0.044 Uiso 1 1 calc R . . C21 C 0.4442(3) 1.0733(2) 0.19925(18) 0.0229(7) Uani 1 1 d . . . H21B H 0.4278 1.1361 0.2171 0.027 Uiso 1 1 calc R . . H21A H 0.5047 1.0738 0.1566 0.027 Uiso 1 1 calc R . . C22 C 0.1180(3) 1.1972(3) 0.2999(2) 0.0393(10) Uani 1 1 d . . . H22B H 0.0747 1.2395 0.2638 0.059 Uiso 1 1 calc R . . H22C H 0.1247 1.2342 0.3369 0.059 Uiso 1 1 calc R . . H22A H 0.0811 1.1449 0.3242 0.059 Uiso 1 1 calc R . . C23 C 0.0495(3) 0.8287(2) 0.12581(19) 0.0246(7) Uani 1 1 d . . . H23 H 0.0976 0.8250 0.0800 0.029 Uiso 1 1 calc R . . C24 C 0.3545(3) 0.8157(2) -0.04166(19) 0.0269(8) Uani 1 1 d . . . H24B H 0.3285 0.7620 -0.0073 0.032 Uiso 1 1 calc R . . H24A H 0.4269 0.7887 -0.0697 0.032 Uiso 1 1 calc R . . C25 C 0.3709(3) 0.8877(3) 0.00415(19) 0.0266(8) Uani 1 1 d . . . H25A H 0.4240 0.8551 0.0381 0.032 Uiso 1 1 calc R . . H25B H 0.3999 0.9410 -0.0288 0.032 Uiso 1 1 calc R . . C26 C 0.7292(3) 0.8221(3) 0.0710(2) 0.0375(9) Uani 1 1 d . . . H26B H 0.7712 0.8739 0.0573 0.045 Uiso 1 1 calc R . . H26A H 0.6684 0.8388 0.0417 0.045 Uiso 1 1 calc R . . C27 C 0.4174(3) 0.3486(2) 0.27233(19) 0.0271(8) Uani 1 1 d . . . H27A H 0.4710 0.3895 0.2686 0.032 Uiso 1 1 calc R . . H27B H 0.4333 0.3202 0.2262 0.032 Uiso 1 1 calc R . . C28 C 0.1386(3) 1.0845(2) 0.18591(18) 0.0233(7) Uani 1 1 d . . . H28 H 0.0670 1.1133 0.2082 0.028 Uiso 1 1 calc R . . C29 C -0.0963(3) 0.8382(2) 0.26027(19) 0.0242(7) Uani 1 1 d . . . H29 H -0.1464 0.8421 0.3053 0.029 Uiso 1 1 calc R . . C30 C 0.0961(3) 0.5453(2) 0.31987(19) 0.0242(7) Uani 1 1 d . . . H30 H 0.1105 0.5247 0.2730 0.029 Uiso 1 1 calc R . . C31 C 0.3839(3) 0.7042(2) 0.50326(18) 0.0218(7) Uani 1 1 d . . . H31 H 0.3704 0.7565 0.5300 0.026 Uiso 1 1 calc R . . C32 C 0.7323(3) 0.5094(2) 0.26996(19) 0.0248(7) Uani 1 1 d . . . H32B H 0.7901 0.4956 0.3015 0.030 Uiso 1 1 calc R . . H32A H 0.7330 0.5734 0.2400 0.030 Uiso 1 1 calc R . . C33 C 0.2999(3) 0.4123(3) 0.27914(19) 0.0283(8) Uani 1 1 d . . . H33B H 0.2954 0.4670 0.2383 0.034 Uiso 1 1 calc R . . H33A H 0.2457 0.3745 0.2769 0.034 Uiso 1 1 calc R . . C34 C 0.3517(3) 1.0019(2) 0.11908(17) 0.0229(7) Uani 1 1 d . . . H34 H 0.4232 0.9747 0.0955 0.027 Uiso 1 1 calc R . . C35 C 0.4235(3) 0.5467(2) 0.42758(17) 0.0217(7) Uani 1 1 d . . . H35 H 0.4378 0.4931 0.4022 0.026 Uiso 1 1 calc R . . C36 C 0.0197(3) 0.7437(2) 0.16794(19) 0.0252(8) Uani 1 1 d . . . C37 C 0.4362(3) 0.9990(2) 0.33634(17) 0.0207(7) Uani 1 1 d . . . H37 H 0.3851 1.0560 0.3481 0.025 Uiso 1 1 calc R . . C38 C 0.0526(3) 0.6022(2) 0.46040(19) 0.0228(7) Uani 1 1 d . . . H38 H 0.0368 0.6210 0.5080 0.027 Uiso 1 1 calc R . . C39 C 0.6820(3) 0.8132(2) 0.15358(19) 0.0268(8) Uani 1 1 d . . . H39A H 0.6444 0.7586 0.1677 0.032 Uiso 1 1 calc R . . H39B H 0.7428 0.8002 0.1826 0.032 Uiso 1 1 calc R . . C40 C -0.0534(3) 0.7478(2) 0.23585(18) 0.0213(7) Uani 1 1 d . . . C41 C -0.0245(3) 0.6389(2) 0.41170(19) 0.0227(7) Uani 1 1 d . . . C42 C 0.2327(3) 1.1007(2) 0.20832(17) 0.0215(7) Uani 1 1 d . . . C43 C -0.0664(3) 0.9224(2) 0.21921(18) 0.0230(7) Uani 1 1 d . . . C44 C 0.6189(3) 0.5125(2) 0.31975(18) 0.0232(7) Uani 1 1 d . . . H44A H 0.5601 0.5246 0.2893 0.028 Uiso 1 1 calc R . . H44B H 0.6183 0.4505 0.3527 0.028 Uiso 1 1 calc R . . C45 C 0.5876(3) 0.8308(2) 0.30263(18) 0.0220(7) Uani 1 1 d . . . H45 H 0.6389 0.7739 0.2909 0.026 Uiso 1 1 calc R . . C46 C 0.0086(3) 0.9192(2) 0.15122(18) 0.0229(7) Uani 1 1 d . . . C47 C 0.4819(3) 0.9915(2) 0.26174(17) 0.0206(7) Uani 1 1 d . . . C48 C 0.3044(3) 0.6472(2) 0.51516(18) 0.0225(7) Uani 1 1 d . . . C49 C 0.1533(3) 0.5377(2) 0.43968(18) 0.0208(7) Uani 1 1 d . . . C50 C 0.1497(3) 1.0262(2) 0.13102(17) 0.0209(7) Uani 1 1 d . . . C51 C 0.3249(3) 0.5659(2) 0.47807(17) 0.0190(7) Uani 1 1 d . . . C52 C 0.2573(3) 0.9839(2) 0.09827(17) 0.0209(7) Uani 1 1 d . . . C54 C 0.5601(3) 0.9061(2) 0.24492(17) 0.0194(7) Uani 1 1 d . . . C55 C 0.5020(3) 0.6055(2) 0.41369(17) 0.0196(7) Uani 1 1 d . . . C56 C 0.4835(3) 0.6854(2) 0.45237(17) 0.0206(7) Uani 1 1 d . . . C58 C -0.0048(3) 0.6120(2) 0.34033(18) 0.0212(7) Uani 1 1 d . . . C59 C 0.1741(3) 0.5100(2) 0.36780(18) 0.0223(7) Uani 1 1 d . . . C60 C 0.3406(3) 1.0596(2) 0.17442(17) 0.0200(7) Uani 1 1 d . . . C62 C 0.5410(3) 0.8373(2) 0.37776(17) 0.0188(7) Uani 1 1 d . . . C73 C 0.3156(9) 0.7270(7) 0.2434(6) 0.156(4) Uiso 1 1 d D . . H73A H 0.3049 0.6643 0.2722 0.187 Uiso 1 1 calc R . . H73B H 0.2644 0.7451 0.2070 0.187 Uiso 1 1 calc R . . C76 C 0.1266(9) 0.9013(8) 0.3896(7) 0.185(4) Uiso 1 1 d D . . H76B H 0.0751 0.9531 0.3644 0.278 Uiso 1 1 calc R . . H76C H 0.1849 0.9274 0.4006 0.278 Uiso 1 1 calc R . . H76A H 0.0868 0.8728 0.4357 0.278 Uiso 1 1 calc R . . C74 C 0.2810(10) 0.8001(9) 0.2954(7) 0.204(5) Uiso 1 1 d D . . H74A H 0.3357 0.7810 0.3295 0.245 Uiso 1 1 calc R . . H74B H 0.2948 0.8611 0.2649 0.245 Uiso 1 1 calc R . . C75 C 0.1765(11) 0.8261(10) 0.3411(8) 0.228(6) Uiso 1 1 d D . . H75B H 0.1683 0.7655 0.3742 0.273 Uiso 1 1 calc R . . H75A H 0.1229 0.8362 0.3070 0.273 Uiso 1 1 calc R . . C72 C 0.4278(11) 0.7125(11) 0.2026(9) 0.262(7) Uiso 1 1 d D . . H72A H 0.4802 0.6907 0.2383 0.315 Uiso 1 1 calc R . . H72B H 0.4406 0.7749 0.1744 0.315 Uiso 1 1 calc R . . C71 C 0.4526(9) 0.6395(8) 0.1492(6) 0.176(4) Uiso 1 1 d D . . H71B H 0.4152 0.6676 0.1066 0.264 Uiso 1 1 calc R . . H71A H 0.4261 0.5817 0.1743 0.264 Uiso 1 1 calc R . . H71C H 0.5323 0.6223 0.1326 0.264 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0262(12) 0.0274(13) 0.0338(13) -0.0158(11) 0.0046(10) -0.0064(10) C1 0.118(7) 0.316(14) 0.176(9) 0.092(9) -0.041(7) 0.007(9) C63 0.0216(16) 0.0170(17) 0.0250(17) -0.0054(14) -0.0033(13) -0.0067(14) O2 0.0316(13) 0.0195(13) 0.0351(13) -0.0096(10) 0.0044(10) -0.0041(10) C2 0.110(4) 0.072(4) 0.075(4) -0.035(3) 0.040(3) -0.030(3) O3 0.0245(12) 0.0307(14) 0.0294(13) -0.0156(11) 0.0026(10) -0.0075(10) C3 0.120(5) 0.051(3) 0.096(4) -0.039(3) 0.029(4) 0.004(3) O4 0.0235(12) 0.0231(13) 0.0363(14) -0.0128(11) 0.0003(10) -0.0006(10) C4 0.103(4) 0.034(3) 0.056(3) -0.011(2) 0.030(3) -0.001(3) O5 0.0299(13) 0.0192(12) 0.0233(12) -0.0076(10) 0.0020(10) -0.0008(10) C5 0.048(2) 0.030(2) 0.0290(19) -0.0082(16) -0.0041(17) -0.0119(18) O6 0.0264(12) 0.0218(13) 0.0316(13) -0.0130(10) -0.0032(10) 0.0017(10) C6 0.050(3) 0.046(3) 0.055(3) -0.032(2) 0.016(2) -0.016(2) O7 0.0337(13) 0.0161(12) 0.0227(12) -0.0067(9) 0.0011(10) -0.0026(10) C7 0.061(3) 0.026(2) 0.062(3) -0.019(2) 0.024(2) -0.010(2) O8 0.0258(12) 0.0196(12) 0.0286(12) -0.0136(10) 0.0044(10) -0.0068(10) C8 0.0306(19) 0.0253(19) 0.0316(19) -0.0119(15) 0.0012(15) -0.0070(15) O9 0.0336(13) 0.0210(13) 0.0404(14) -0.0142(11) 0.0037(11) -0.0063(11) C9 0.034(2) 0.0238(19) 0.038(2) -0.0095(16) -0.0065(16) -0.0049(16) O10 0.0247(12) 0.0336(14) 0.0359(13) -0.0205(11) 0.0006(10) -0.0040(11) C10 0.032(2) 0.046(2) 0.058(3) -0.036(2) 0.0118(18) -0.0070(18) C11 0.054(3) 0.035(2) 0.035(2) -0.0128(18) -0.0025(19) -0.0030(19) C12 0.039(2) 0.035(2) 0.042(2) -0.0227(18) 0.0098(17) -0.0170(18) C13 0.0312(19) 0.0217(18) 0.0310(19) -0.0108(15) -0.0002(15) -0.0035(15) C14 0.0234(17) 0.0173(17) 0.0358(19) -0.0081(15) -0.0010(14) -0.0056(14) C15 0.0254(17) 0.0211(18) 0.0266(17) -0.0055(14) -0.0048(14) -0.0049(14) C16 0.0278(18) 0.0161(17) 0.0281(18) -0.0042(14) -0.0005(14) -0.0041(14) C17 0.042(2) 0.027(2) 0.041(2) -0.0154(17) 0.0138(17) -0.0052(17) C18 0.0261(17) 0.0152(17) 0.0253(17) -0.0063(14) -0.0026(13) -0.0041(14) C19 0.0282(19) 0.026(2) 0.041(2) -0.0159(17) 0.0007(16) -0.0015(16) C20 0.035(2) 0.0201(18) 0.0270(18) -0.0066(15) 0.0018(15) 0.0012(15) C21 0.0234(17) 0.0164(17) 0.0280(18) -0.0060(14) 0.0001(14) -0.0041(14) C22 0.033(2) 0.041(2) 0.047(2) -0.0302(19) 0.0045(17) -0.0041(18) C23 0.0211(17) 0.0257(19) 0.0283(18) -0.0105(15) -0.0020(14) -0.0041(14) C24 0.0290(18) 0.0203(18) 0.0292(18) -0.0085(15) 0.0046(14) -0.0047(15) C25 0.0222(17) 0.0270(19) 0.0302(18) -0.0122(15) 0.0040(14) -0.0052(15) C26 0.049(2) 0.028(2) 0.032(2) -0.0117(17) 0.0089(17) -0.0096(18) C27 0.0287(18) 0.0222(18) 0.0308(18) -0.0104(15) -0.0012(15) -0.0044(15) C28 0.0227(17) 0.0164(17) 0.0265(17) -0.0022(14) -0.0008(14) 0.0004(14) C29 0.0203(17) 0.0239(19) 0.0291(18) -0.0076(15) -0.0022(14) -0.0047(14) C30 0.0284(18) 0.0174(17) 0.0289(18) -0.0076(14) -0.0010(14) -0.0087(14) C31 0.0274(17) 0.0148(16) 0.0253(17) -0.0095(13) -0.0037(14) -0.0039(14) C32 0.0277(18) 0.0186(18) 0.0287(18) -0.0085(14) 0.0000(14) -0.0060(14) C33 0.0293(19) 0.0246(19) 0.0293(18) -0.0094(15) -0.0036(15) 0.0006(15) C34 0.0232(17) 0.0184(17) 0.0237(17) -0.0023(14) 0.0032(13) -0.0046(14) C35 0.0292(18) 0.0122(16) 0.0239(17) -0.0061(13) -0.0053(14) -0.0013(14) C36 0.0254(18) 0.0186(18) 0.0342(19) -0.0105(15) -0.0052(15) -0.0040(14) C37 0.0210(16) 0.0127(16) 0.0296(18) -0.0081(14) -0.0012(13) -0.0041(13) C38 0.0255(17) 0.0153(17) 0.0291(18) -0.0075(14) 0.0025(14) -0.0095(14) C39 0.0296(18) 0.0202(18) 0.0295(18) -0.0085(15) -0.0032(15) -0.0007(15) C40 0.0175(16) 0.0201(17) 0.0281(17) -0.0050(14) -0.0053(13) -0.0052(13) C41 0.0193(16) 0.0123(16) 0.0351(19) -0.0046(14) 0.0015(14) -0.0044(13) C42 0.0262(17) 0.0145(16) 0.0233(16) -0.0053(13) 0.0014(13) -0.0060(14) C43 0.0223(17) 0.0183(17) 0.0292(18) -0.0072(14) -0.0059(14) -0.0016(14) C44 0.0259(17) 0.0196(17) 0.0267(17) -0.0121(14) -0.0006(14) -0.0059(14) C45 0.0222(17) 0.0161(17) 0.0287(18) -0.0080(14) -0.0038(14) -0.0027(13) C46 0.0210(16) 0.0221(18) 0.0277(17) -0.0065(14) -0.0064(14) -0.0044(14) C47 0.0212(16) 0.0175(17) 0.0265(17) -0.0051(14) -0.0030(13) -0.0101(14) C48 0.0205(16) 0.0219(18) 0.0223(16) -0.0029(14) -0.0015(13) -0.0012(14) C49 0.0210(16) 0.0142(16) 0.0273(17) -0.0034(14) 0.0012(13) -0.0076(13) C50 0.0252(17) 0.0149(16) 0.0200(16) 0.0015(13) -0.0015(13) -0.0042(14) C51 0.0213(16) 0.0121(16) 0.0221(16) 0.0019(13) -0.0053(13) -0.0027(13) C52 0.0285(18) 0.0162(17) 0.0184(16) -0.0022(13) -0.0031(13) -0.0065(14) C54 0.0201(16) 0.0159(17) 0.0238(16) -0.0051(13) -0.0013(13) -0.0072(13) C55 0.0191(16) 0.0161(16) 0.0221(16) -0.0041(13) -0.0004(13) -0.0021(13) C56 0.0230(16) 0.0164(17) 0.0227(16) -0.0035(13) -0.0049(13) -0.0036(13) C58 0.0204(16) 0.0140(16) 0.0311(18) -0.0054(14) -0.0010(14) -0.0083(13) C59 0.0222(17) 0.0121(16) 0.0326(18) -0.0064(14) 0.0005(14) -0.0052(14) C60 0.0242(17) 0.0137(16) 0.0208(16) 0.0007(13) -0.0048(13) -0.0030(13) C62 0.0219(16) 0.0145(16) 0.0236(16) -0.0052(13) -0.0051(13) -0.0078(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C48 1.381(4) . ? O1 C10 1.415(4) . ? C1 C3 1.362(11) . ? C1 H1B 0.9600 . ? C1 H1A 0.9600 . ? C1 H1C 0.9600 . ? C63 C37 1.381(5) . ? C63 O7 1.387(4) . ? C63 C62 1.396(4) . ? O2 C43 1.390(4) . ? O2 C17 1.426(4) . ? C2 C3 1.494(7) . ? C2 C7 1.560(7) . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? O3 C52 1.374(4) . ? O3 C25 1.430(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? O4 C41 1.397(4) . ? O4 C19 1.413(4) . ? C4 C11 1.501(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? O5 C54 1.376(4) . ? O5 C39 1.429(4) . ? C5 C8 1.526(5) . ? C5 H5C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? O6 C59 1.384(4) . ? O6 C33 1.427(4) . ? C6 C12 1.520(5) . ? C6 H6A 0.9600 . ? C6 H6C 0.9600 . ? C6 H6B 0.9600 . ? O7 C20 1.419(4) . ? C7 O9 1.396(4) . ? C7 H7B 0.9700 . ? C7 H7A 0.9700 . ? O8 C55 1.382(4) . ? O8 C44 1.426(3) . ? C8 C24 1.515(5) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? O9 C36 1.385(4) . ? C9 C13 1.516(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? O10 C42 1.379(4) . ? O10 C22 1.414(4) . ? C10 H10A 0.9600 . ? C10 H10C 0.9600 . ? C10 H10B 0.9600 . ? C11 C26 1.549(5) . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C12 C32 1.520(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C27 1.514(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C58 1.510(5) . ? C14 C40 1.515(4) . ? C14 H14B 0.9700 . ? C14 H14A 0.9700 . ? C15 C46 1.506(4) . ? C15 C50 1.523(4) . ? C15 H15B 0.9700 . ? C15 H15A 0.9700 . ? C16 C49 1.513(4) . ? C16 C51 1.518(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17C 0.9600 . ? C17 H17B 0.9600 . ? C18 C62 1.511(4) . ? C18 C56 1.513(4) . ? C18 H18B 0.9700 . ? C18 H18A 0.9700 . ? C19 H19C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C20 H20A 0.9600 . ? C20 H20C 0.9600 . ? C20 H20B 0.9600 . ? C21 C60 1.514(4) . ? C21 C47 1.525(5) . ? C21 H21B 0.9700 . ? C21 H21A 0.9700 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C22 H22A 0.9600 . ? C23 C36 1.393(5) . ? C23 C46 1.394(4) . ? C23 H23 0.9300 . ? C24 C25 1.514(4) . ? C24 H24B 0.9700 . ? C24 H24A 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C39 1.503(5) . ? C26 H26B 0.9700 . ? C26 H26A 0.9700 . ? C27 C33 1.512(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C50 1.387(4) . ? C28 C42 1.395(4) . ? C28 H28 0.9300 . ? C29 C43 1.378(5) . ? C29 C40 1.387(4) . ? C29 H29 0.9300 . ? C30 C59 1.377(5) . ? C30 C58 1.404(5) . ? C30 H30 0.9300 . ? C31 C48 1.385(4) . ? C31 C56 1.393(4) . ? C31 H31 0.9300 . ? C32 C44 1.512(4) . ? C32 H32B 0.9700 . ? C32 H32A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33A 0.9700 . ? C34 C60 1.388(4) . ? C34 C52 1.396(4) . ? C34 H34 0.9300 . ? C35 C51 1.381(4) . ? C35 C55 1.390(4) . ? C35 H35 0.9300 . ? C36 C40 1.388(5) . ? C37 C47 1.385(4) . ? C37 H37 0.9300 . ? C38 C41 1.380(5) . ? C38 C49 1.389(4) . ? C38 H38 0.9300 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C58 1.391(4) . ? C42 C60 1.394(4) . ? C43 C46 1.399(5) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C54 1.384(5) . ? C45 C62 1.394(4) . ? C45 H45 0.9300 . ? C47 C54 1.398(4) . ? C48 C51 1.396(4) . ? C49 C59 1.403(4) . ? C50 C52 1.388(4) . ? C55 C56 1.400(4) . ? C73 C72 1.429(9) . ? C73 C74 1.473(8) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C76 C75 1.461(8) . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C76 H76A 0.9600 . ? C74 C75 1.403(8) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 H75B 0.9700 . ? C75 H75A 0.9700 . ? C72 C71 1.496(9) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C71 H71B 0.9600 . ? C71 H71A 0.9600 . ? C71 H71C 0.9600 . ? 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 C48 O1 C10 117.1(3) . . ? C3 C1 H1B 109.5 . . ? C3 C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? C3 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? C37 C63 O7 123.6(3) . . ? C37 C63 C62 120.5(3) . . ? O7 C63 C62 115.8(3) . . ? C43 O2 C17 116.0(3) . . ? C3 C2 C7 112.1(4) . . ? C3 C2 H2B 109.2 . . ? C7 C2 H2B 109.2 . . ? C3 C2 H2A 109.2 . . ? C7 C2 H2A 109.2 . . ? H2B C2 H2A 107.9 . . ? C52 O3 C25 118.6(2) . . ? C1 C3 C2 114.2(7) . . ? C1 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? C1 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C41 O4 C19 116.8(3) . . ? C11 C4 H4A 109.5 . . ? C11 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C11 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C54 O5 C39 116.4(2) . . ? C8 C5 H5C 109.5 . . ? C8 C5 H5A 109.5 . . ? H5C C5 H5A 109.5 . . ? C8 C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C59 O6 C33 117.7(3) . . ? C12 C6 H6A 109.5 . . ? C12 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? C12 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? C63 O7 C20 117.2(2) . . ? O9 C7 C2 107.6(3) . . ? O9 C7 H7B 110.2 . . ? C2 C7 H7B 110.2 . . ? O9 C7 H7A 110.2 . . ? C2 C7 H7A 110.2 . . ? H7B C7 H7A 108.5 . . ? C55 O8 C44 117.2(2) . . ? C24 C8 C5 112.2(3) . . ? C24 C8 H8B 109.2 . . ? C5 C8 H8B 109.2 . . ? C24 C8 H8A 109.2 . . ? C5 C8 H8A 109.2 . . ? H8B C8 H8A 107.9 . . ? C36 O9 C7 118.6(3) . . ? C13 C9 H9A 109.5 . . ? C13 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C13 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C42 O10 C22 117.3(3) . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? O1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C4 C11 C26 113.3(3) . . ? C4 C11 H11B 108.9 . . ? C26 C11 H11B 108.9 . . ? C4 C11 H11A 108.9 . . ? C26 C11 H11A 108.9 . . ? H11B C11 H11A 107.7 . . ? C32 C12 C6 111.7(3) . . ? C32 C12 H12A 109.3 . . ? C6 C12 H12A 109.3 . . ? C32 C12 H12B 109.3 . . ? C6 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C27 C13 C9 112.9(3) . . ? C27 C13 H13A 109.0 . . ? C9 C13 H13A 109.0 . . ? C27 C13 H13B 109.0 . . ? C9 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C58 C14 C40 111.4(2) . . ? C58 C14 H14B 109.4 . . ? C40 C14 H14B 109.4 . . ? C58 C14 H14A 109.4 . . ? C40 C14 H14A 109.4 . . ? H14B C14 H14A 108.0 . . ? C46 C15 C50 112.6(3) . . ? C46 C15 H15B 109.1 . . ? C50 C15 H15B 109.1 . . ? C46 C15 H15A 109.1 . . ? C50 C15 H15A 109.1 . . ? H15B C15 H15A 107.8 . . ? C49 C16 C51 112.1(3) . . ? C49 C16 H16A 109.2 . . ? C51 C16 H16A 109.2 . . ? C49 C16 H16B 109.2 . . ? C51 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? C62 C18 C56 111.9(3) . . ? C62 C18 H18B 109.2 . . ? C56 C18 H18B 109.2 . . ? C62 C18 H18A 109.2 . . ? C56 C18 H18A 109.2 . . ? H18B C18 H18A 107.9 . . ? O4 C19 H19C 109.5 . . ? O4 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O7 C20 H20A 109.5 . . ? O7 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? O7 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? C60 C21 C47 111.1(2) . . ? C60 C21 H21B 109.4 . . ? C47 C21 H21B 109.4 . . ? C60 C21 H21A 109.4 . . ? C47 C21 H21A 109.4 . . ? H21B C21 H21A 108.0 . . ? O10 C22 H22B 109.5 . . ? O10 C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O10 C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? C36 C23 C46 121.1(3) . . ? C36 C23 H23 119.4 . . ? C46 C23 H23 119.4 . . ? C25 C24 C8 115.1(3) . . ? C25 C24 H24B 108.5 . . ? C8 C24 H24B 108.5 . . ? C25 C24 H24A 108.5 . . ? C8 C24 H24A 108.5 . . ? H24B C24 H24A 107.5 . . ? O3 C25 C24 107.1(3) . . ? O3 C25 H25A 110.3 . . ? C24 C25 H25A 110.3 . . ? O3 C25 H25B 110.3 . . ? C24 C25 H25B 110.3 . . ? H25A C25 H25B 108.6 . . ? C39 C26 C11 109.2(3) . . ? C39 C26 H26B 109.8 . . ? C11 C26 H26B 109.8 . . ? C39 C26 H26A 109.8 . . ? C11 C26 H26A 109.8 . . ? H26B C26 H26A 108.3 . . ? C33 C27 C13 113.3(3) . . ? C33 C27 H27A 108.9 . . ? C13 C27 H27A 108.9 . . ? C33 C27 H27B 108.9 . . ? C13 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C50 C28 C42 121.3(3) . . ? C50 C28 H28 119.3 . . ? C42 C28 H28 119.3 . . ? C43 C29 C40 121.3(3) . . ? C43 C29 H29 119.3 . . ? C40 C29 H29 119.3 . . ? C59 C30 C58 121.3(3) . . ? C59 C30 H30 119.3 . . ? C58 C30 H30 119.3 . . ? C48 C31 C56 121.8(3) . . ? C48 C31 H31 119.1 . . ? C56 C31 H31 119.1 . . ? C44 C32 C12 112.9(3) . . ? C44 C32 H32B 109.0 . . ? C12 C32 H32B 109.0 . . ? C44 C32 H32A 109.0 . . ? C12 C32 H32A 109.0 . . ? H32B C32 H32A 107.8 . . ? O6 C33 C27 107.2(3) . . ? O6 C33 H33B 110.3 . . ? C27 C33 H33B 110.3 . . ? O6 C33 H33A 110.3 . . ? C27 C33 H33A 110.3 . . ? H33B C33 H33A 108.5 . . ? C60 C34 C52 121.0(3) . . ? C60 C34 H34 119.5 . . ? C52 C34 H34 119.5 . . ? C51 C35 C55 121.7(3) . . ? C51 C35 H35 119.1 . . ? C55 C35 H35 119.1 . . ? O9 C36 C40 116.4(3) . . ? O9 C36 C23 123.2(3) . . ? C40 C36 C23 120.4(3) . . ? C63 C37 C47 121.5(3) . . ? C63 C37 H37 119.2 . . ? C47 C37 H37 119.2 . . ? C41 C38 C49 121.2(3) . . ? C41 C38 H38 119.4 . . ? C49 C38 H38 119.4 . . ? O5 C39 C26 110.3(3) . . ? O5 C39 H39A 109.6 . . ? C26 C39 H39A 109.6 . . ? O5 C39 H39B 109.6 . . ? C26 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C29 C40 C36 118.5(3) . . ? C29 C40 C14 120.2(3) . . ? C36 C40 C14 121.3(3) . . ? C38 C41 C58 121.3(3) . . ? C38 C41 O4 123.5(3) . . ? C58 C41 O4 115.1(3) . . ? O10 C42 C60 116.2(3) . . ? O10 C42 C28 123.7(3) . . ? C60 C42 C28 120.1(3) . . ? C29 C43 O2 123.7(3) . . ? C29 C43 C46 120.9(3) . . ? O2 C43 C46 115.4(3) . . ? O8 C44 C32 107.2(2) . . ? O8 C44 H44A 110.3 . . ? C32 C44 H44A 110.3 . . ? O8 C44 H44B 110.3 . . ? C32 C44 H44B 110.3 . . ? H44A C44 H44B 108.5 . . ? C54 C45 C62 122.3(3) . . ? C54 C45 H45 118.9 . . ? C62 C45 H45 118.9 . . ? C23 C46 C43 117.7(3) . . ? C23 C46 C15 120.9(3) . . ? C43 C46 C15 121.4(3) . . ? C37 C47 C54 118.7(3) . . ? C37 C47 C21 120.4(3) . . ? C54 C47 C21 120.9(3) . . ? O1 C48 C31 123.8(3) . . ? O1 C48 C51 116.1(3) . . ? C31 C48 C51 120.1(3) . . ? C38 C49 C59 118.0(3) . . ? C38 C49 C16 121.1(3) . . ? C59 C49 C16 120.9(3) . . ? C28 C50 C52 118.5(3) . . ? C28 C50 C15 120.3(3) . . ? C52 C50 C15 121.2(3) . . ? C35 C51 C48 118.4(3) . . ? C35 C51 C16 120.8(3) . . ? C48 C51 C16 120.8(3) . . ? O3 C52 C50 116.0(3) . . ? O3 C52 C34 123.5(3) . . ? C50 C52 C34 120.4(3) . . ? O5 C54 C45 123.6(3) . . ? O5 C54 C47 116.9(3) . . ? C45 C54 C47 119.4(3) . . ? O8 C55 C35 123.8(3) . . ? O8 C55 C56 116.1(3) . . ? C35 C55 C56 120.2(3) . . ? C31 C56 C55 117.8(3) . . ? C31 C56 C18 120.6(3) . . ? C55 C56 C18 121.6(3) . . ? C41 C58 C30 117.5(3) . . ? C41 C58 C14 122.6(3) . . ? C30 C58 C14 119.8(3) . . ? C30 C59 O6 124.1(3) . . ? C30 C59 C49 120.7(3) . . ? O6 C59 C49 115.2(3) . . ? C34 C60 C42 118.6(3) . . ? C34 C60 C21 120.1(3) . . ? C42 C60 C21 121.2(3) . . ? C45 C62 C63 117.5(3) . . ? C45 C62 C18 120.7(3) . . ? C63 C62 C18 121.6(3) . . ? C72 C73 C74 118.5(9) . . ? C72 C73 H73A 107.7 . . ? C74 C73 H73A 107.7 . . ? C72 C73 H73B 107.7 . . ? C74 C73 H73B 107.7 . . ? H73A C73 H73B 107.1 . . ? C75 C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C76 H76A 109.5 . . ? H76B C76 H76A 109.5 . . ? H76C C76 H76A 109.5 . . ? C75 C74 C73 128.4(11) . . ? C75 C74 H74A 105.2 . . ? C73 C74 H74A 105.2 . . ? C75 C74 H74B 105.2 . . ? C73 C74 H74B 105.2 . . ? H74A C74 H74B 105.9 . . ? C74 C75 C76 134.9(12) . . ? C74 C75 H75B 103.5 . . ? C76 C75 H75B 103.5 . . ? C74 C75 H75A 103.5 . . ? C76 C75 H75A 103.5 . . ? H75B C75 H75A 105.3 . . ? C73 C72 C71 114.0(10) . . ? C73 C72 H72A 108.7 . . ? C71 C72 H72A 108.7 . . ? C73 C72 H72B 108.7 . . ? C71 C72 H72B 108.7 . . ? H72A C72 H72B 107.6 . . ? C72 C71 H71B 109.5 . . ? C72 C71 H71A 109.5 . . ? H71B C71 H71A 109.5 . . ? C72 C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.524 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.088 #===END