# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yingming Yao' _publ_contact_author_email YAOYM@SUDA.EDU.CN _publ_section_title ; Synthesis, characterization and reactivity of heteroleptic rare earth metal bis(phenolate) complexes ; loop_ _publ_author_name 'Yingming Yao.' 'Bao Liu.' 'Ruipeng Qi.' 'Qi Shen.' 'Xiaoping Xu.' ; Zijian Yang ; 'Yong Zhang.' #============================================================end data_complex6 _database_code_depnum_ccdc_archive 'CCDC 294476' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H77 O6 Y, 1.5(C7 H8)' _chemical_formula_sum 'C64.50 H89 O6 Y' _chemical_formula_weight 1049.27 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' Y Y -2.7962 3.5667 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4589(16) _cell_length_b 15.066(2) _cell_length_c 16.943(2) _cell_angle_alpha 106.726(3) _cell_angle_beta 105.974(3) _cell_angle_gamma 90.752(2) _cell_volume 2913.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 11468 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6495 _exptl_absorpt_correction_T_max 0.7793 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29239 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10602 _reflns_number_gt 9295 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0473P)^2^+2.4953P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10602 _refine_ls_number_parameters 663 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.068 _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 Y1 Y 0.92166(2) 0.201754(18) 0.252765(15) 0.02243(9) Uani 1 1 d . . . O1 O 0.89382(15) 0.22929(13) 0.13442(11) 0.0253(4) Uani 1 1 d . . . O2 O 0.79348(16) 0.08164(13) 0.21407(11) 0.0298(4) Uani 1 1 d . . . O3 O 1.07031(15) 0.26265(13) 0.35219(11) 0.0262(4) Uani 1 1 d . . . O4 O 0.83952(16) 0.18645(14) 0.36158(12) 0.0290(4) Uani 1 1 d D . . H4 H 0.799(3) 0.1399(16) 0.330(2) 0.057(12) Uiso 1 1 d D . . O5 O 1.04352(16) 0.09149(13) 0.20726(12) 0.0336(5) Uani 1 1 d . . . O6 O 0.86009(16) 0.35268(13) 0.29898(11) 0.0291(4) Uani 1 1 d . . . C1 C 0.8309(2) 0.23495(18) 0.05769(15) 0.0223(5) Uani 1 1 d . . . C2 C 0.8757(2) 0.27408(18) 0.00555(16) 0.0249(6) Uani 1 1 d . . . C3 C 0.8040(2) 0.2746(2) -0.07368(17) 0.0312(6) Uani 1 1 d . . . H3 H 0.8338 0.2991 -0.1099 0.037 Uiso 1 1 calc R . . C4 C 0.6914(3) 0.2412(2) -0.10238(18) 0.0352(7) Uani 1 1 d . . . C5 C 0.6487(2) 0.2061(2) -0.04910(18) 0.0326(7) Uani 1 1 d . . . H5 H 0.5711 0.1852 -0.0665 0.039 Uiso 1 1 calc R . . C6 C 0.7167(2) 0.20075(18) 0.02939(16) 0.0253(6) Uani 1 1 d . . . C7 C 0.7399(2) 0.01970(19) 0.13622(16) 0.0258(6) Uani 1 1 d . . . C8 C 0.7391(2) -0.07766(19) 0.12278(17) 0.0277(6) Uani 1 1 d . . . C9 C 0.6950(2) -0.1359(2) 0.03802(18) 0.0311(6) Uani 1 1 d . . . H9 H 0.6959 -0.2013 0.0274 0.037 Uiso 1 1 calc R . . C10 C 0.6501(2) -0.1027(2) -0.03104(18) 0.0310(6) Uani 1 1 d . . . C11 C 0.6420(2) -0.0085(2) -0.01436(17) 0.0305(6) Uani 1 1 d . . . H11 H 0.6060 0.0147 -0.0604 0.037 Uiso 1 1 calc R . . C12 C 0.6851(2) 0.05381(19) 0.06811(17) 0.0262(6) Uani 1 1 d . . . C13 C 0.6672(2) 0.15622(19) 0.08213(17) 0.0287(6) Uani 1 1 d . . . H13A H 0.5857 0.1623 0.0679 0.034 Uiso 1 1 calc R . . H13B H 0.7010 0.1906 0.1439 0.034 Uiso 1 1 calc R . . C14 C 0.9989(2) 0.3164(2) 0.03499(17) 0.0283(6) Uani 1 1 d . . . C15 C 1.0271(3) 0.3541(2) -0.0327(2) 0.0438(8) Uani 1 1 d . . . H15A H 1.1057 0.3805 -0.0117 0.066 Uiso 1 1 calc R . . H15B H 0.9784 0.4026 -0.0431 0.066 Uiso 1 1 calc R . . H15C H 1.0153 0.3032 -0.0865 0.066 Uiso 1 1 calc R . . C16 C 1.0796(2) 0.2440(2) 0.0516(2) 0.0376(7) Uani 1 1 d . . . H16A H 1.0669 0.2215 0.0974 0.056 Uiso 1 1 calc R . . H16B H 1.1571 0.2723 0.0692 0.056 Uiso 1 1 calc R . . H16C H 1.0667 0.1916 -0.0012 0.056 Uiso 1 1 calc R . . C17 C 1.0194(3) 0.3985(2) 0.11777(18) 0.0356(7) Uani 1 1 d . . . H17A H 1.0049 0.3763 0.1632 0.053 Uiso 1 1 calc R . . H17B H 0.9689 0.4458 0.1068 0.053 Uiso 1 1 calc R . . H17C H 1.0974 0.4258 0.1361 0.053 Uiso 1 1 calc R . . C18 C 0.6165(3) 0.2457(3) -0.1881(2) 0.0569(10) Uani 1 1 d . . . H18A H 0.5589 0.1925 -0.2129 0.085 Uiso 1 1 calc R . . H18B H 0.6618 0.2438 -0.2275 0.085 Uiso 1 1 calc R . . H18C H 0.5805 0.3038 -0.1793 0.085 Uiso 1 1 calc R . . C19 C 0.7828(3) -0.1187(2) 0.19784(19) 0.0347(7) Uani 1 1 d . . . C20 C 0.7612(3) -0.2250(2) 0.1687(2) 0.0478(8) Uani 1 1 d . . . H20A H 0.6804 -0.2434 0.1435 0.072 Uiso 1 1 calc R . . H20B H 0.7893 -0.2480 0.2184 0.072 Uiso 1 1 calc R . . H20C H 0.8000 -0.2516 0.1255 0.072 Uiso 1 1 calc R . . C21 C 0.7216(4) -0.0821(3) 0.2661(2) 0.0547(10) Uani 1 1 d . . . H21A H 0.7419 -0.0149 0.2928 0.082 Uiso 1 1 calc R . . H21B H 0.7435 -0.1137 0.3104 0.082 Uiso 1 1 calc R . . H21C H 0.6404 -0.0943 0.2389 0.082 Uiso 1 1 calc R . . C22 C 0.9096(3) -0.0947(3) 0.2386(2) 0.0562(10) Uani 1 1 d . . . H22A H 0.9485 -0.1230 0.1960 0.084 Uiso 1 1 calc R . . H22B H 0.9342 -0.1189 0.2879 0.084 Uiso 1 1 calc R . . H22C H 0.9273 -0.0269 0.2582 0.084 Uiso 1 1 calc R . . C23 C 0.6114(3) -0.1673(2) -0.12268(19) 0.0422(8) Uani 1 1 d . . . H23A H 0.5454 -0.1451 -0.1555 0.063 Uiso 1 1 calc R . . H23B H 0.5919 -0.2303 -0.1222 0.063 Uiso 1 1 calc R . . H23C H 0.6718 -0.1683 -0.1496 0.063 Uiso 1 1 calc R . . C24 C 1.1540(2) 0.28521(18) 0.42624(15) 0.0230(6) Uani 1 1 d . . . C25 C 1.2474(2) 0.34941(19) 0.44182(16) 0.0249(6) Uani 1 1 d . . . C26 C 1.3301(2) 0.3685(2) 0.52085(17) 0.0299(6) Uani 1 1 d . . . H26 H 1.3921 0.4126 0.5326 0.036 Uiso 1 1 calc R . . C27 C 1.3269(2) 0.3266(2) 0.58312(17) 0.0334(7) Uani 1 1 d . . . C28 C 1.2354(2) 0.2639(2) 0.56603(17) 0.0325(7) Uani 1 1 d . . . H28 H 1.2318 0.2343 0.6078 0.039 Uiso 1 1 calc R . . C29 C 1.1484(2) 0.24279(19) 0.48947(16) 0.0265(6) Uani 1 1 d . . . C30 C 0.8469(2) 0.21315(19) 0.44918(17) 0.0276(6) Uani 1 1 d . . . C31 C 0.7521(2) 0.2392(2) 0.47677(18) 0.0306(6) Uani 1 1 d . . . C32 C 0.7723(3) 0.2719(2) 0.56626(19) 0.0382(7) Uani 1 1 d . . . H32 H 0.7108 0.2903 0.5881 0.046 Uiso 1 1 calc R . . C33 C 0.8772(3) 0.2789(2) 0.62473(19) 0.0397(7) Uani 1 1 d . . . C34 C 0.9659(3) 0.2487(2) 0.59346(18) 0.0354(7) Uani 1 1 d . . . H34 H 1.0376 0.2513 0.6329 0.042 Uiso 1 1 calc R . . C35 C 0.9526(2) 0.21438(19) 0.50511(17) 0.0279(6) Uani 1 1 d . . . C36 C 1.0504(2) 0.17324(19) 0.47449(18) 0.0289(6) Uani 1 1 d . . . H36A H 1.0782 0.1265 0.5041 0.035 Uiso 1 1 calc R . . H36B H 1.0222 0.1400 0.4120 0.035 Uiso 1 1 calc R . . C37 C 1.2580(2) 0.3961(2) 0.37459(17) 0.0283(6) Uani 1 1 d . . . C38 C 1.3670(3) 0.4617(2) 0.4056(2) 0.0396(7) Uani 1 1 d . . . H38A H 1.3679 0.5110 0.4582 0.059 Uiso 1 1 calc R . . H38B H 1.3708 0.4896 0.3607 0.059 Uiso 1 1 calc R . . H38C H 1.4317 0.4262 0.4175 0.059 Uiso 1 1 calc R . . C39 C 1.2594(3) 0.3228(2) 0.29033(17) 0.0347(7) Uani 1 1 d . . . H39A H 1.3230 0.2861 0.3019 0.052 Uiso 1 1 calc R . . H39B H 1.2668 0.3540 0.2485 0.052 Uiso 1 1 calc R . . H39C H 1.1893 0.2814 0.2670 0.052 Uiso 1 1 calc R . . C40 C 1.1606(3) 0.4561(2) 0.35652(19) 0.0367(7) Uani 1 1 d . . . H40A H 1.0895 0.4160 0.3310 0.055 Uiso 1 1 calc R . . H40B H 1.1712 0.4887 0.3164 0.055 Uiso 1 1 calc R . . H40C H 1.1590 0.5017 0.4106 0.055 Uiso 1 1 calc R . . C41 C 1.4218(3) 0.3469(3) 0.6658(2) 0.0541(10) Uani 1 1 d . . . H41A H 1.4907 0.3257 0.6525 0.081 Uiso 1 1 calc R . . H41B H 1.4029 0.3140 0.7031 0.081 Uiso 1 1 calc R . . H41C H 1.4334 0.4140 0.6954 0.081 Uiso 1 1 calc R . . C42 C 0.6334(2) 0.2309(2) 0.41487(19) 0.0347(7) Uani 1 1 d . . . C43 C 0.5456(3) 0.2545(3) 0.4645(2) 0.0477(8) Uani 1 1 d . . . H43A H 0.5465 0.2117 0.4986 0.072 Uiso 1 1 calc R . . H43B H 0.4710 0.2482 0.4236 0.072 Uiso 1 1 calc R . . H43C H 0.5637 0.3187 0.5030 0.072 Uiso 1 1 calc R . . C44 C 0.5978(3) 0.1310(2) 0.3535(2) 0.0472(8) Uani 1 1 d . . . H44A H 0.6367 0.1196 0.3091 0.071 Uiso 1 1 calc R . . H44B H 0.5165 0.1233 0.3262 0.071 Uiso 1 1 calc R . . H44C H 0.6174 0.0865 0.3862 0.071 Uiso 1 1 calc R . . C45 C 0.6266(3) 0.2979(2) 0.3613(2) 0.0406(7) Uani 1 1 d . . . H45A H 0.6440 0.3621 0.3997 0.061 Uiso 1 1 calc R . . H45B H 0.5507 0.2905 0.3218 0.061 Uiso 1 1 calc R . . H45C H 0.6808 0.2842 0.3281 0.061 Uiso 1 1 calc R . . C46 C 0.8928(3) 0.3151(3) 0.7207(2) 0.0596(10) Uani 1 1 d . . . H46A H 0.8851 0.2627 0.7428 0.089 Uiso 1 1 calc R . . H46B H 0.8358 0.3573 0.7317 0.089 Uiso 1 1 calc R . . H46C H 0.9677 0.3487 0.7499 0.089 Uiso 1 1 calc R . . C47 C 1.1488(3) 0.0714(2) 0.2593(2) 0.0462(8) Uani 1 1 d . . . H47A H 1.1365 0.0509 0.3069 0.055 Uiso 1 1 calc R . . H47B H 1.2036 0.1275 0.2841 0.055 Uiso 1 1 calc R . . C48 C 1.1908(4) -0.0043(3) 0.2004(3) 0.0719(12) Uani 1 1 d . . . H48A H 1.1753 -0.0651 0.2087 0.086 Uiso 1 1 calc R . . H48B H 1.2726 0.0080 0.2114 0.086 Uiso 1 1 calc R . . C49 C 1.1292(3) -0.0044(3) 0.1112(3) 0.0636(11) Uani 1 1 d . . . H49A H 1.1706 0.0374 0.0917 0.076 Uiso 1 1 calc R . . H49B H 1.1178 -0.0680 0.0702 0.076 Uiso 1 1 calc R . . C50 C 1.0199(3) 0.0301(2) 0.11881(19) 0.0393(7) Uani 1 1 d . . . H50A H 0.9908 0.0647 0.0771 0.047 Uiso 1 1 calc R . . H50B H 0.9637 -0.0225 0.1079 0.047 Uiso 1 1 calc R . . C51 C 0.7966(3) 0.4064(2) 0.24654(19) 0.0386(7) Uani 1 1 d . . . H51A H 0.7154 0.3963 0.2394 0.046 Uiso 1 1 calc R . . H51B H 0.8086 0.3885 0.1889 0.046 Uiso 1 1 calc R . . C52 C 0.8391(6) 0.5033(3) 0.2934(3) 0.123(3) Uani 1 1 d . . . H52A H 0.7775 0.5438 0.2859 0.148 Uiso 1 1 calc R . . H52B H 0.8977 0.5233 0.2710 0.148 Uiso 1 1 calc R . . C53 C 0.8862(3) 0.5112(2) 0.3848(2) 0.0441(8) Uani 1 1 d . . . H53A H 0.8366 0.5431 0.4184 0.053 Uiso 1 1 calc R . . H53B H 0.9612 0.5469 0.4084 0.053 Uiso 1 1 calc R . . C54 C 0.8946(3) 0.4127(2) 0.38866(17) 0.0322(7) Uani 1 1 d . . . H54A H 0.9725 0.4043 0.4180 0.039 Uiso 1 1 calc R . . H54B H 0.8445 0.3977 0.4204 0.039 Uiso 1 1 calc R . . C55 C 0.3452(3) 0.4627(2) 0.0098(2) 0.0470(9) Uani 1 1 d . . . C56 C 0.3110(3) 0.4982(2) 0.0825(2) 0.0525(9) Uani 1 1 d . . . H56 H 0.2514 0.5370 0.0804 0.063 Uiso 1 1 calc R . . C57 C 0.3612(3) 0.4788(3) 0.1581(2) 0.0569(10) Uani 1 1 d . . . H57 H 0.3364 0.5043 0.2074 0.068 Uiso 1 1 calc R . . C58 C 0.4468(3) 0.4225(3) 0.1621(3) 0.0590(10) Uani 1 1 d . . . H58 H 0.4813 0.4086 0.2140 0.071 Uiso 1 1 calc R . . C59 C 0.4823(3) 0.3865(3) 0.0908(3) 0.0574(10) Uani 1 1 d . . . H59 H 0.5417 0.3475 0.0933 0.069 Uiso 1 1 calc R . . C60 C 0.4323(3) 0.4064(2) 0.0153(2) 0.0512(9) Uani 1 1 d . . . H60 H 0.4580 0.3812 -0.0337 0.061 Uiso 1 1 calc R . . C61 C 0.2875(3) 0.4835(3) -0.0724(3) 0.0686(12) Uani 1 1 d . . . H61A H 0.2142 0.4469 -0.0991 0.103 Uiso 1 1 calc R . . H61B H 0.3336 0.4674 -0.1120 0.103 Uiso 1 1 calc R . . H61C H 0.2772 0.5500 -0.0596 0.103 Uiso 1 1 calc R . . C62 C 0.4202(8) 1.0047(7) 0.4895(6) 0.077(3) Uiso 0.50 1 d PD . . C63 C 0.4445(11) 0.9323(8) 0.4224(7) 0.080(3) Uiso 0.50 1 d PD . . C64 C 0.5614(10) 0.9250(7) 0.4421(7) 0.084(3) Uiso 0.50 1 d PD . . C65 C 0.6517(12) 0.9673(9) 0.5135(8) 0.100(4) Uiso 0.50 1 d PD . . C66 C 0.6198(12) 1.0378(11) 0.5758(10) 0.129(5) Uiso 0.50 1 d PD . . C67 C 0.5050(10) 1.0546(6) 0.5619(6) 0.060(2) Uiso 0.50 1 d PD . . C68 C 0.2917(12) 1.0045(12) 0.4633(11) 0.133(5) Uiso 0.50 1 d PD . . 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 Y1 0.02230(14) 0.02555(15) 0.01838(14) 0.00733(10) 0.00355(10) 0.00203(10) O1 0.0251(10) 0.0310(10) 0.0176(9) 0.0082(8) 0.0016(8) 0.0025(8) O2 0.0350(11) 0.0286(10) 0.0218(10) 0.0055(8) 0.0043(8) -0.0057(8) O3 0.0225(9) 0.0320(11) 0.0190(9) 0.0051(8) 0.0006(8) 0.0025(8) O4 0.0296(11) 0.0336(11) 0.0214(10) 0.0046(9) 0.0078(9) -0.0013(9) O5 0.0337(11) 0.0325(11) 0.0296(10) 0.0038(9) 0.0069(9) 0.0114(9) O6 0.0320(10) 0.0295(11) 0.0230(9) 0.0074(8) 0.0040(8) 0.0088(8) C1 0.0258(14) 0.0223(13) 0.0170(12) 0.0053(10) 0.0042(11) 0.0041(11) C2 0.0261(14) 0.0252(14) 0.0210(13) 0.0056(11) 0.0045(11) 0.0038(11) C3 0.0366(16) 0.0335(16) 0.0235(14) 0.0129(12) 0.0042(12) 0.0003(13) C4 0.0382(17) 0.0358(17) 0.0247(15) 0.0120(13) -0.0044(13) 0.0001(13) C5 0.0240(14) 0.0354(16) 0.0329(16) 0.0119(13) -0.0019(12) 0.0008(12) C6 0.0244(14) 0.0258(14) 0.0238(14) 0.0070(11) 0.0042(11) 0.0035(11) C7 0.0232(14) 0.0314(15) 0.0236(14) 0.0072(12) 0.0094(11) -0.0016(11) C8 0.0251(14) 0.0308(15) 0.0290(15) 0.0093(12) 0.0106(12) -0.0008(12) C9 0.0321(15) 0.0266(15) 0.0352(16) 0.0065(12) 0.0140(13) -0.0005(12) C10 0.0286(15) 0.0341(16) 0.0273(15) 0.0015(12) 0.0117(12) -0.0027(12) C11 0.0258(14) 0.0400(17) 0.0244(14) 0.0101(13) 0.0053(12) -0.0020(12) C12 0.0224(13) 0.0287(15) 0.0289(14) 0.0076(12) 0.0112(12) 0.0000(11) C13 0.0247(14) 0.0326(16) 0.0285(14) 0.0088(12) 0.0078(12) 0.0038(12) C14 0.0283(15) 0.0328(16) 0.0220(14) 0.0073(12) 0.0058(12) -0.0016(12) C15 0.0419(19) 0.057(2) 0.0331(17) 0.0168(15) 0.0082(14) -0.0101(16) C16 0.0276(15) 0.0452(19) 0.0387(17) 0.0112(14) 0.0092(13) 0.0053(14) C17 0.0339(16) 0.0345(17) 0.0311(16) 0.0052(13) 0.0034(13) -0.0046(13) C18 0.051(2) 0.072(3) 0.0392(19) 0.0316(18) -0.0146(16) -0.0105(19) C19 0.0425(17) 0.0277(16) 0.0346(16) 0.0123(13) 0.0094(14) -0.0008(13) C20 0.066(2) 0.0318(18) 0.047(2) 0.0172(15) 0.0135(17) 0.0045(16) C21 0.087(3) 0.045(2) 0.049(2) 0.0248(17) 0.034(2) 0.0138(19) C22 0.048(2) 0.056(2) 0.064(2) 0.037(2) -0.0030(18) -0.0008(18) C23 0.0477(19) 0.0429(19) 0.0284(16) -0.0002(14) 0.0106(14) -0.0059(15) C24 0.0212(13) 0.0255(14) 0.0170(12) 0.0016(10) 0.0017(10) 0.0083(11) C25 0.0215(13) 0.0289(15) 0.0208(13) 0.0039(11) 0.0045(11) 0.0061(11) C26 0.0212(14) 0.0368(16) 0.0258(14) 0.0044(12) 0.0028(11) 0.0054(12) C27 0.0281(15) 0.0414(17) 0.0234(14) 0.0071(13) -0.0016(12) 0.0080(13) C28 0.0351(16) 0.0390(17) 0.0244(14) 0.0134(13) 0.0056(12) 0.0135(14) C29 0.0275(14) 0.0285(15) 0.0227(13) 0.0073(11) 0.0062(11) 0.0107(12) C30 0.0343(15) 0.0265(15) 0.0233(14) 0.0094(11) 0.0087(12) 0.0011(12) C31 0.0342(16) 0.0313(16) 0.0323(15) 0.0135(12) 0.0153(13) 0.0058(12) C32 0.0479(19) 0.0428(18) 0.0342(16) 0.0154(14) 0.0239(15) 0.0123(15) C33 0.054(2) 0.0449(19) 0.0253(15) 0.0146(14) 0.0155(15) 0.0085(16) C34 0.0394(17) 0.0414(18) 0.0262(15) 0.0147(13) 0.0062(13) 0.0070(14) C35 0.0346(15) 0.0270(15) 0.0252(14) 0.0115(12) 0.0096(12) 0.0046(12) C36 0.0330(15) 0.0267(15) 0.0273(14) 0.0107(12) 0.0060(12) 0.0073(12) C37 0.0238(14) 0.0368(16) 0.0223(14) 0.0080(12) 0.0045(11) 0.0006(12) C38 0.0330(17) 0.0463(19) 0.0359(17) 0.0119(14) 0.0055(14) -0.0053(14) C39 0.0337(16) 0.0448(18) 0.0243(14) 0.0058(13) 0.0112(13) 0.0018(14) C40 0.0350(16) 0.0403(18) 0.0349(16) 0.0154(14) 0.0062(13) 0.0052(14) C41 0.041(2) 0.077(3) 0.0333(18) 0.0200(18) -0.0094(15) 0.0008(18) C42 0.0302(16) 0.0395(17) 0.0385(17) 0.0142(14) 0.0138(13) 0.0071(13) C43 0.0385(18) 0.059(2) 0.058(2) 0.0259(18) 0.0256(17) 0.0121(16) C44 0.0321(17) 0.048(2) 0.057(2) 0.0125(17) 0.0098(16) 0.0002(15) C45 0.0334(17) 0.050(2) 0.0439(18) 0.0228(16) 0.0114(14) 0.0089(15) C46 0.070(3) 0.084(3) 0.0278(17) 0.0160(18) 0.0198(18) 0.018(2) C47 0.0372(18) 0.047(2) 0.0473(19) 0.0092(16) 0.0051(15) 0.0167(15) C48 0.060(3) 0.080(3) 0.079(3) 0.021(2) 0.027(2) 0.041(2) C49 0.054(2) 0.062(3) 0.065(3) -0.009(2) 0.030(2) 0.0065(19) C50 0.0510(19) 0.0329(17) 0.0317(16) 0.0031(13) 0.0150(15) 0.0046(14) C51 0.0411(18) 0.0421(18) 0.0334(16) 0.0171(14) 0.0055(14) 0.0174(14) C52 0.245(8) 0.044(3) 0.045(2) 0.008(2) -0.011(3) 0.051(4) C53 0.056(2) 0.0336(18) 0.0399(18) 0.0061(14) 0.0140(16) 0.0155(15) C54 0.0381(16) 0.0359(17) 0.0202(14) 0.0043(12) 0.0089(12) 0.0053(13) C55 0.0382(19) 0.045(2) 0.053(2) 0.0211(17) -0.0005(16) -0.0127(16) C56 0.045(2) 0.043(2) 0.063(2) 0.0184(18) 0.0041(18) -0.0013(16) C57 0.060(2) 0.053(2) 0.052(2) 0.0139(18) 0.0093(19) -0.0077(19) C58 0.062(2) 0.050(2) 0.055(2) 0.0229(19) -0.0062(19) -0.012(2) C59 0.046(2) 0.043(2) 0.074(3) 0.022(2) 0.000(2) -0.0029(17) C60 0.045(2) 0.046(2) 0.056(2) 0.0130(17) 0.0077(17) -0.0106(17) C61 0.061(3) 0.080(3) 0.067(3) 0.042(2) 0.000(2) -0.009(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 Y1 O1 2.1007(17) . ? Y1 O3 2.1115(17) . ? Y1 O2 2.2181(18) . ? Y1 O5 2.3734(19) . ? Y1 O6 2.3925(18) . ? Y1 O4 2.4035(18) . ? Y1 H4 2.59(3) . ? O1 C1 1.348(3) . ? O2 C7 1.359(3) . ? O3 C24 1.343(3) . ? O4 C30 1.398(3) . ? O4 H4 0.814(10) . ? O5 C47 1.455(4) . ? O5 C50 1.463(3) . ? O6 C51 1.454(3) . ? O6 C54 1.467(3) . ? C1 C6 1.408(4) . ? C1 C2 1.415(4) . ? C2 C3 1.395(4) . ? C2 C14 1.544(4) . ? C3 C4 1.386(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 C18 1.515(4) . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 C13 1.505(4) . ? C7 C12 1.407(4) . ? C7 C8 1.418(4) . ? C8 C9 1.400(4) . ? C8 C19 1.542(4) . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 C11 1.376(4) . ? C10 C23 1.515(4) . ? C11 C12 1.393(4) . ? C11 H11 0.9500 . ? C12 C13 1.521(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C16 1.527(4) . ? C14 C15 1.533(4) . ? C14 C17 1.535(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.530(4) . ? C19 C22 1.531(5) . ? C19 C21 1.535(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.412(4) . ? C24 C25 1.419(4) . ? C25 C26 1.396(4) . ? C25 C37 1.534(4) . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? C27 C28 1.381(4) . ? C27 C41 1.513(4) . ? C28 C29 1.392(4) . ? C28 H28 0.9500 . ? C29 C36 1.515(4) . ? C30 C35 1.391(4) . ? C30 C31 1.406(4) . ? C31 C32 1.401(4) . ? C31 C42 1.539(4) . ? C32 C33 1.388(4) . ? C32 H32 0.9500 . ? C33 C34 1.380(4) . ? C33 C46 1.514(4) . ? C34 C35 1.397(4) . ? C34 H34 0.9500 . ? C35 C36 1.523(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C40 1.538(4) . ? C37 C39 1.538(4) . ? C37 C38 1.540(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C45 1.530(4) . ? C42 C44 1.540(4) . ? C42 C43 1.541(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.489(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.494(6) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.489(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.457(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.466(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.508(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.378(5) . ? C55 C60 1.385(5) . ? C55 C61 1.504(5) . ? C56 C57 1.377(5) . ? C56 H56 0.9500 . ? C57 C58 1.371(6) . ? C57 H57 0.9500 . ? C58 C59 1.368(6) . ? C58 H58 0.9500 . ? C59 C60 1.380(5) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C65 0.990(14) 2_676 ? C62 C66 1.079(15) 2_676 ? C62 C64 1.287(14) 2_676 ? C62 C67 1.386(11) . ? C62 C63 1.435(12) . ? C62 C68 1.538(14) . ? C62 C67 1.564(14) 2_676 ? C62 C63 1.931(15) 2_676 ? C62 C62 1.936(19) 2_676 ? C63 C67 0.617(12) 2_676 ? C63 C66 0.928(14) 2_676 ? C63 C64 1.416(13) . ? C63 C62 1.931(15) 2_676 ? C64 C67 0.879(11) 2_676 ? C64 C62 1.287(14) 2_676 ? C64 C65 1.387(13) . ? C65 C68 0.758(17) 2_676 ? C65 C62 0.990(14) 2_676 ? C65 C66 1.413(14) . ? C65 C67 1.981(17) 2_676 ? C66 C63 0.928(14) 2_676 ? C66 C62 1.079(15) 2_676 ? C66 C67 1.422(14) . ? C66 C68 1.50(2) 2_676 ? C67 C63 0.617(12) 2_676 ? C67 C64 0.879(11) 2_676 ? C67 C62 1.564(14) 2_676 ? C67 C65 1.981(17) 2_676 ? C68 C65 0.758(17) 2_676 ? C68 C66 1.50(2) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y1 O3 118.76(7) . . ? O1 Y1 O2 99.78(7) . . ? O3 Y1 O2 138.99(7) . . ? O1 Y1 O5 87.56(7) . . ? O3 Y1 O5 81.86(7) . . ? O2 Y1 O5 86.64(7) . . ? O1 Y1 O6 84.02(7) . . ? O3 Y1 O6 83.34(7) . . ? O2 Y1 O6 116.06(7) . . ? O5 Y1 O6 156.80(7) . . ? O1 Y1 O4 145.79(7) . . ? O3 Y1 O4 88.00(7) . . ? O2 Y1 O4 63.77(7) . . ? O5 Y1 O4 119.02(7) . . ? O6 Y1 O4 78.08(7) . . ? O1 Y1 H4 135.7(7) . . ? O3 Y1 H4 103.7(5) . . ? O2 Y1 H4 45.5(4) . . ? O5 Y1 H4 111.6(8) . . ? O6 Y1 H4 89.3(7) . . ? O4 Y1 H4 18.2(4) . . ? C1 O1 Y1 155.01(16) . . ? C7 O2 Y1 132.09(16) . . ? C24 O3 Y1 163.44(17) . . ? C30 O4 Y1 146.82(16) . . ? C30 O4 H4 118(3) . . ? Y1 O4 H4 94(3) . . ? C47 O5 C50 109.1(2) . . ? C47 O5 Y1 127.74(17) . . ? C50 O5 Y1 123.16(17) . . ? C51 O6 C54 107.5(2) . . ? C51 O6 Y1 128.51(16) . . ? C54 O6 Y1 123.62(15) . . ? O1 C1 C6 118.2(2) . . ? O1 C1 C2 122.3(2) . . ? C6 C1 C2 119.5(2) . . ? C3 C2 C1 117.7(2) . . ? C3 C2 C14 120.5(2) . . ? C1 C2 C14 121.8(2) . . ? C4 C3 C2 123.4(3) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C5 C4 C3 117.8(3) . . ? C5 C4 C18 120.9(3) . . ? C3 C4 C18 121.3(3) . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.9(2) . . ? C5 C6 C13 119.3(2) . . ? C1 C6 C13 120.8(2) . . ? O2 C7 C12 118.8(2) . . ? O2 C7 C8 121.3(2) . . ? C12 C7 C8 120.0(2) . . ? C9 C8 C7 117.2(3) . . ? C9 C8 C19 120.9(3) . . ? C7 C8 C19 121.9(2) . . ? C10 C9 C8 123.2(3) . . ? C10 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? C11 C10 C9 118.0(3) . . ? C11 C10 C23 120.4(3) . . ? C9 C10 C23 121.6(3) . . ? C10 C11 C12 121.9(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 119.1(3) . . ? C11 C12 C13 118.7(2) . . ? C7 C12 C13 122.1(2) . . ? C6 C13 C12 114.0(2) . . ? C6 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C6 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C16 C14 C15 107.6(2) . . ? C16 C14 C17 109.4(2) . . ? C15 C14 C17 107.3(2) . . ? C16 C14 C2 111.1(2) . . ? C15 C14 C2 111.8(2) . . ? C17 C14 C2 109.5(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 106.8(3) . . ? C20 C19 C21 106.5(3) . . ? C22 C19 C21 109.9(3) . . ? C20 C19 C8 112.2(2) . . ? C22 C19 C8 111.4(2) . . ? C21 C19 C8 109.8(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 C29 118.5(2) . . ? O3 C24 C25 121.8(2) . . ? C29 C24 C25 119.7(2) . . ? C26 C25 C24 117.5(2) . . ? C26 C25 C37 120.9(2) . . ? C24 C25 C37 121.6(2) . . ? C27 C26 C25 123.6(3) . . ? C27 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C28 C27 C26 117.7(3) . . ? C28 C27 C41 121.2(3) . . ? C26 C27 C41 121.1(3) . . ? C27 C28 C29 122.1(3) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C24 119.4(3) . . ? C28 C29 C36 119.5(2) . . ? C24 C29 C36 121.0(2) . . ? C35 C30 O4 115.9(2) . . ? C35 C30 C31 123.6(2) . . ? O4 C30 C31 120.5(2) . . ? C32 C31 C30 115.1(3) . . ? C32 C31 C42 121.3(3) . . ? C30 C31 C42 123.6(2) . . ? C33 C32 C31 123.5(3) . . ? C33 C32 H32 118.3 . . ? C31 C32 H32 118.3 . . ? C34 C33 C32 118.5(3) . . ? C34 C33 C46 120.9(3) . . ? C32 C33 C46 120.6(3) . . ? C33 C34 C35 121.6(3) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C30 C35 C34 117.6(3) . . ? C30 C35 C36 123.0(2) . . ? C34 C35 C36 119.2(2) . . ? C29 C36 C35 115.4(2) . . ? C29 C36 H36A 108.4 . . ? C35 C36 H36A 108.4 . . ? C29 C36 H36B 108.4 . . ? C35 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C25 C37 C40 110.5(2) . . ? C25 C37 C39 110.7(2) . . ? C40 C37 C39 109.8(2) . . ? C25 C37 C38 112.0(2) . . ? C40 C37 C38 106.6(2) . . ? C39 C37 C38 107.0(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 C41 H41A 109.5 . . ? C27 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C27 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C45 C42 C31 111.2(2) . . ? C45 C42 C44 108.8(3) . . ? C31 C42 C44 111.3(2) . . ? C45 C42 C43 107.3(3) . . ? C31 C42 C43 111.3(2) . . ? C44 C42 C43 106.8(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C33 C46 H46A 109.5 . . ? C33 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C33 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 106.3(3) . . ? O5 C47 H47A 110.5 . . ? C48 C47 H47A 110.5 . . ? O5 C47 H47B 110.5 . . ? C48 C47 H47B 110.5 . . ? H47A C47 H47B 108.7 . . ? C47 C48 C49 105.8(3) . . ? C47 C48 H48A 110.6 . . ? C49 C48 H48A 110.6 . . ? C47 C48 H48B 110.6 . . ? C49 C48 H48B 110.6 . . ? H48A C48 H48B 108.7 . . ? C50 C49 C48 104.1(3) . . ? C50 C49 H49A 110.9 . . ? C48 C49 H49A 110.9 . . ? C50 C49 H49B 110.9 . . ? C48 C49 H49B 110.9 . . ? H49A C49 H49B 109.0 . . ? O5 C50 C49 105.4(3) . . ? O5 C50 H50A 110.7 . . ? C49 C50 H50A 110.7 . . ? O5 C50 H50B 110.7 . . ? C49 C50 H50B 110.7 . . ? H50A C50 H50B 108.8 . . ? O6 C51 C52 105.3(3) . . ? O6 C51 H51A 110.7 . . ? C52 C51 H51A 110.7 . . ? O6 C51 H51B 110.7 . . ? C52 C51 H51B 110.7 . . ? H51A C51 H51B 108.8 . . ? C51 C52 C53 108.3(4) . . ? C51 C52 H52A 110.0 . . ? C53 C52 H52A 110.0 . . ? C51 C52 H52B 110.0 . . ? C53 C52 H52B 110.0 . . ? H52A C52 H52B 108.4 . . ? C52 C53 C54 105.8(3) . . ? C52 C53 H53A 110.6 . . ? C54 C53 H53A 110.6 . . ? C52 C53 H53B 110.6 . . ? C54 C53 H53B 110.6 . . ? H53A C53 H53B 108.7 . . ? O6 C54 C53 106.0(2) . . ? O6 C54 H54A 110.5 . . ? C53 C54 H54A 110.5 . . ? O6 C54 H54B 110.5 . . ? C53 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? C56 C55 C60 117.6(3) . . ? C56 C55 C61 120.5(4) . . ? C60 C55 C61 121.9(4) . . ? C57 C56 C55 121.6(4) . . ? C57 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? C58 C57 C56 120.0(4) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C59 C58 C57 119.6(4) . . ? C59 C58 H58 120.2 . . ? C57 C58 H58 120.2 . . ? C58 C59 C60 120.4(4) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? C59 C60 C55 120.9(4) . . ? C59 C60 H60 119.5 . . ? C55 C60 H60 119.5 . . ? C55 C61 H61A 109.5 . . ? C55 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C55 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C65 C62 C66 86.1(12) 2_676 2_676 ? C65 C62 C64 73.8(10) 2_676 2_676 ? C66 C62 C64 157.9(13) 2_676 2_676 ? C65 C62 C67 111.9(11) 2_676 . ? C66 C62 C67 159.0(12) 2_676 . ? C64 C62 C67 38.2(5) 2_676 . ? C65 C62 C63 126.3(12) 2_676 . ? C66 C62 C63 40.3(8) 2_676 . ? C64 C62 C63 158.5(10) 2_676 . ? C67 C62 C63 120.9(9) . . ? C65 C62 C68 24.5(10) 2_676 . ? C66 C62 C68 67.1(11) 2_676 . ? C64 C62 C68 95.4(11) 2_676 . ? C67 C62 C68 133.1(11) . . ? C63 C62 C68 105.9(11) . . ? C65 C62 C67 146.5(12) 2_676 2_676 ? C66 C62 C67 61.9(9) 2_676 2_676 ? C64 C62 C67 135.3(9) 2_676 2_676 ? C67 C62 C67 98.2(8) . 2_676 ? C63 C62 C67 23.2(5) . 2_676 ? C68 C62 C67 128.7(11) . 2_676 ? C65 C62 C63 120.2(12) 2_676 2_676 ? C66 C62 C63 148.9(12) 2_676 2_676 ? C64 C62 C63 47.1(6) 2_676 2_676 ? C67 C62 C63 10.1(6) . 2_676 ? C63 C62 C63 111.6(8) . 2_676 ? C68 C62 C63 142.5(11) . 2_676 ? C67 C62 C63 88.6(6) 2_676 2_676 ? C65 C62 C62 160.1(14) 2_676 2_676 ? C66 C62 C62 106.7(12) 2_676 2_676 ? C64 C62 C62 90.7(8) 2_676 2_676 ? C67 C62 C62 53.1(6) . 2_676 ? C63 C62 C62 68.0(8) . 2_676 ? C68 C62 C62 173.8(12) . 2_676 ? C67 C62 C62 45.1(5) 2_676 2_676 ? C63 C62 C62 43.6(4) 2_676 2_676 ? C67 C63 C66 133(2) 2_676 2_676 ? C67 C63 C64 22.6(13) 2_676 . ? C66 C63 C64 155.7(17) 2_676 . ? C67 C63 C62 90.2(17) 2_676 . ? C66 C63 C62 48.7(11) 2_676 . ? C64 C63 C62 110.2(10) . . ? C67 C63 C62 23.3(13) 2_676 2_676 ? C66 C63 C62 115.3(14) 2_676 2_676 ? C64 C63 C62 41.8(6) . 2_676 ? C62 C63 C62 68.4(8) . 2_676 ? C67 C64 C62 77.0(11) 2_676 2_676 ? C67 C64 C65 120.2(14) 2_676 . ? C62 C64 C65 43.3(7) 2_676 . ? C67 C64 C63 15.6(9) 2_676 . ? C62 C64 C63 91.0(9) 2_676 . ? C65 C64 C63 133.5(11) . . ? C68 C65 C62 123(2) 2_676 2_676 ? C68 C65 C64 155(2) 2_676 . ? C62 C65 C64 63.0(11) 2_676 . ? C68 C65 C66 81.1(18) 2_676 . ? C62 C65 C66 49.6(9) 2_676 . ? C64 C65 C66 112.1(13) . . ? C68 C65 C67 154(2) 2_676 2_676 ? C62 C65 C67 40.5(8) 2_676 2_676 ? C64 C65 C67 22.6(6) . 2_676 ? C66 C65 C67 89.5(10) . 2_676 ? C63 C66 C62 91.0(15) 2_676 2_676 ? C63 C66 C65 135.3(18) 2_676 . ? C62 C66 C65 44.3(8) 2_676 . ? C63 C66 C67 18.4(10) 2_676 . ? C62 C66 C67 76.0(11) 2_676 . ? C65 C66 C67 119.7(13) . . ? C63 C66 C68 155.8(19) 2_676 2_676 ? C62 C66 C68 71.3(11) 2_676 2_676 ? C65 C66 C68 30.0(8) . 2_676 ? C67 C66 C68 146.8(14) . 2_676 ? C63 C67 C64 142(2) 2_676 2_676 ? C63 C67 C62 146.6(18) 2_676 . ? C64 C67 C62 64.8(11) 2_676 . ? C63 C67 C66 28.4(15) 2_676 . ? C64 C67 C66 170.2(15) 2_676 . ? C62 C67 C66 123.5(9) . . ? C63 C67 C62 66.6(15) 2_676 2_676 ? C64 C67 C62 144.7(13) 2_676 2_676 ? C62 C67 C62 81.8(8) . 2_676 ? C66 C67 C62 42.0(7) . 2_676 ? C63 C67 C65 162.3(19) 2_676 2_676 ? C64 C67 C65 37.3(9) 2_676 2_676 ? C62 C67 C65 27.6(5) . 2_676 ? C66 C67 C65 150.5(9) . 2_676 ? C62 C67 C65 108.5(8) 2_676 2_676 ? C65 C68 C66 68.9(15) 2_676 2_676 ? C65 C68 C62 32.8(14) 2_676 . ? C66 C68 C62 41.6(7) 2_676 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.875 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.058 #============================================================end data_complex4 _database_code_depnum_ccdc_archive 'CCDC 294477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C81 H114 La2 O9, 2(C7 H8)' _chemical_formula_sum 'C95 H130 La2 O9' _chemical_formula_weight 1693.81 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' La La -0.2871 2.4523 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4810(8) _cell_length_b 15.3116(11) _cell_length_c 21.5012(15) _cell_angle_alpha 85.694(4) _cell_angle_beta 80.533(4) _cell_angle_gamma 83.864(4) _cell_volume 4345.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 13716 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7100 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43041 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.1089 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.35 _reflns_number_total 15826 _reflns_number_gt 12172 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0385P)^2^+7.5755P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15826 _refine_ls_number_parameters 974 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.145 _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 La1 La 0.11257(2) 0.30998(2) 0.171833(16) 0.02559(10) Uani 1 1 d . . . La2 La 0.22061(2) 0.11005(2) 0.283679(16) 0.02765(11) Uani 1 1 d . . . O1 O 0.1685(3) 0.4408(2) 0.16295(19) 0.0288(9) Uani 1 1 d . . . O2 O -0.0487(3) 0.3567(2) 0.17333(18) 0.0289(9) Uani 1 1 d . . . O3 O 0.2249(3) 0.1714(2) 0.17551(17) 0.0258(9) Uani 1 1 d . . . O4 O 0.0981(3) 0.0212(3) 0.27466(19) 0.0329(10) Uani 1 1 d . . . O5 O 0.1085(3) 0.2508(2) 0.28023(17) 0.0244(8) Uani 1 1 d . . . O6 O 0.3690(3) 0.1595(3) 0.29737(19) 0.0318(9) Uani 1 1 d . . . O7 O 0.1142(3) 0.3174(3) 0.0521(2) 0.0426(11) Uani 1 1 d . . . O8 O 0.2242(4) 0.0537(3) 0.3991(2) 0.0561(13) Uani 1 1 d . . . O9 O 0.3228(3) -0.0362(3) 0.2452(2) 0.0477(12) Uani 1 1 d . . . C1 C 0.1508(4) 0.5286(3) 0.1559(3) 0.0239(12) Uani 1 1 d . . . C2 C 0.2235(4) 0.5812(4) 0.1219(3) 0.0253(12) Uani 1 1 d . . . C3 C 0.1969(5) 0.6717(4) 0.1153(3) 0.0316(14) Uani 1 1 d . . . H3 H 0.2450 0.7072 0.0914 0.038 Uiso 1 1 calc R . . C4 C 0.1050(4) 0.7126(4) 0.1414(3) 0.0338(14) Uani 1 1 d . . . C5 C 0.0375(4) 0.6600(4) 0.1773(3) 0.0310(14) Uani 1 1 d . . . H5 H -0.0249 0.6871 0.1976 0.037 Uiso 1 1 calc R . . C6 C 0.0567(4) 0.5695(4) 0.1851(3) 0.0245(12) Uani 1 1 d . . . C7 C -0.1265(4) 0.4201(4) 0.1753(3) 0.0260(13) Uani 1 1 d . . . C8 C -0.2180(4) 0.4066(4) 0.1544(3) 0.0286(13) Uani 1 1 d . . . C9 C -0.2920(4) 0.4771(4) 0.1556(3) 0.0362(15) Uani 1 1 d . . . H9 H -0.3527 0.4693 0.1406 0.043 Uiso 1 1 calc R . . C10 C -0.2826(4) 0.5586(4) 0.1776(3) 0.0398(16) Uani 1 1 d . . . C11 C -0.1944(4) 0.5681(4) 0.2005(3) 0.0359(15) Uani 1 1 d . . . H11 H -0.1871 0.6221 0.2175 0.043 Uiso 1 1 calc R . . C12 C -0.1163(4) 0.5010(4) 0.1992(3) 0.0266(13) Uani 1 1 d . . . C13 C -0.0217(4) 0.5170(4) 0.2263(3) 0.0272(13) Uani 1 1 d . . . H13A H -0.0442 0.5474 0.2659 0.033 Uiso 1 1 calc R . . H13B H 0.0123 0.4589 0.2377 0.033 Uiso 1 1 calc R . . C14 C 0.3281(4) 0.5416(4) 0.0908(3) 0.0354(15) Uani 1 1 d . . . C15 C 0.3981(5) 0.6127(5) 0.0629(4) 0.0512(19) Uani 1 1 d . . . H15A H 0.3696 0.6472 0.0286 0.077 Uiso 1 1 calc R . . H15B H 0.4650 0.5846 0.0463 0.077 Uiso 1 1 calc R . . H15C H 0.4042 0.6516 0.0960 0.077 Uiso 1 1 calc R . . C16 C 0.3162(5) 0.4860(4) 0.0372(3) 0.0411(16) Uani 1 1 d . . . H16A H 0.2777 0.4365 0.0542 0.062 Uiso 1 1 calc R . . H16B H 0.3831 0.4636 0.0159 0.062 Uiso 1 1 calc R . . H16C H 0.2803 0.5222 0.0068 0.062 Uiso 1 1 calc R . . C17 C 0.3829(5) 0.4849(4) 0.1399(3) 0.0448(17) Uani 1 1 d . . . H17A H 0.3875 0.5206 0.1752 0.067 Uiso 1 1 calc R . . H17B H 0.4511 0.4638 0.1200 0.067 Uiso 1 1 calc R . . H17C H 0.3450 0.4346 0.1558 0.067 Uiso 1 1 calc R . . C18 C 0.0815(6) 0.8109(4) 0.1315(4) 0.0517(19) Uani 1 1 d . . . H18A H 0.0328 0.8231 0.1020 0.078 Uiso 1 1 calc R . . H18B H 0.1437 0.8376 0.1140 0.078 Uiso 1 1 calc R . . H18C H 0.0526 0.8356 0.1720 0.078 Uiso 1 1 calc R . . C19 C -0.2360(4) 0.3177(4) 0.1329(3) 0.0357(15) Uani 1 1 d . . . C20 C -0.3431(5) 0.3169(5) 0.1176(4) 0.0494(18) Uani 1 1 d . . . H20A H -0.3924 0.3266 0.1559 0.074 Uiso 1 1 calc R . . H20B H -0.3501 0.2599 0.1018 0.074 Uiso 1 1 calc R . . H20C H -0.3552 0.3638 0.0853 0.074 Uiso 1 1 calc R . . C21 C -0.2244(5) 0.2454(4) 0.1861(3) 0.0391(16) Uani 1 1 d . . . H21A H -0.1573 0.2443 0.1982 0.059 Uiso 1 1 calc R . . H21B H -0.2321 0.1881 0.1709 0.059 Uiso 1 1 calc R . . H21C H -0.2763 0.2579 0.2227 0.059 Uiso 1 1 calc R . . C22 C -0.1615(5) 0.2940(5) 0.0735(3) 0.0457(17) Uani 1 1 d . . . H22A H -0.1709 0.3388 0.0394 0.069 Uiso 1 1 calc R . . H22B H -0.1737 0.2365 0.0607 0.069 Uiso 1 1 calc R . . H22C H -0.0922 0.2915 0.0824 0.069 Uiso 1 1 calc R . . C23 C -0.3673(5) 0.6315(5) 0.1796(4) 0.066(2) Uani 1 1 d . . . H23A H -0.3979 0.6329 0.1412 0.098 Uiso 1 1 calc R . . H23B H -0.3406 0.6879 0.1822 0.098 Uiso 1 1 calc R . . H23C H -0.4185 0.6210 0.2167 0.098 Uiso 1 1 calc R . . C24 C 0.2212(4) 0.1225(3) 0.1254(3) 0.0241(12) Uani 1 1 d . . . C25 C 0.3052(4) 0.1105(4) 0.0768(3) 0.0287(13) Uani 1 1 d . . . C26 C 0.2979(5) 0.0535(4) 0.0309(3) 0.0355(15) Uani 1 1 d . . . H26 H 0.3547 0.0426 -0.0010 0.043 Uiso 1 1 calc R . . C27 C 0.2118(5) 0.0115(4) 0.0289(3) 0.0368(15) Uani 1 1 d . . . C28 C 0.1273(5) 0.0307(4) 0.0748(3) 0.0364(15) Uani 1 1 d . . . H28 H 0.0666 0.0050 0.0735 0.044 Uiso 1 1 calc R . . C29 C 0.1307(4) 0.0866(4) 0.1220(3) 0.0288(13) Uani 1 1 d . . . C30 C 0.0198(4) -0.0109(4) 0.2555(3) 0.0295(13) Uani 1 1 d . . . C31 C -0.0269(4) -0.0847(4) 0.2863(3) 0.0341(14) Uani 1 1 d . . . C32 C -0.1077(5) -0.1121(4) 0.2620(3) 0.0405(16) Uani 1 1 d . . . H32 H -0.1399 -0.1608 0.2829 0.049 Uiso 1 1 calc R . . C33 C -0.1434(4) -0.0715(4) 0.2088(3) 0.0380(16) Uani 1 1 d . . . C34 C -0.0971(4) 0.0001(4) 0.1802(3) 0.0345(14) Uani 1 1 d . . . H34 H -0.1212 0.0298 0.1444 0.041 Uiso 1 1 calc R . . C35 C -0.0163(4) 0.0306(4) 0.2019(3) 0.0307(14) Uani 1 1 d . . . C36 C 0.0339(4) 0.1083(4) 0.1684(3) 0.0300(13) Uani 1 1 d . . . H36A H 0.0498 0.1452 0.2006 0.036 Uiso 1 1 calc R . . H36B H -0.0152 0.1442 0.1451 0.036 Uiso 1 1 calc R . . C37 C 0.4032(4) 0.1544(4) 0.0752(3) 0.0311(14) Uani 1 1 d . . . C38 C 0.4726(5) 0.1463(5) 0.0111(3) 0.054(2) Uani 1 1 d . . . H38A H 0.4960 0.0842 0.0050 0.081 Uiso 1 1 calc R . . H38B H 0.5310 0.1797 0.0103 0.081 Uiso 1 1 calc R . . H38C H 0.4352 0.1697 -0.0229 0.081 Uiso 1 1 calc R . . C39 C 0.4610(5) 0.1127(5) 0.1264(4) 0.058(2) Uani 1 1 d . . . H39A H 0.4197 0.1213 0.1679 0.087 Uiso 1 1 calc R . . H39B H 0.5240 0.1403 0.1240 0.087 Uiso 1 1 calc R . . H39C H 0.4766 0.0496 0.1206 0.087 Uiso 1 1 calc R . . C40 C 0.3804(5) 0.2536(4) 0.0833(4) 0.055(2) Uani 1 1 d . . . H40A H 0.3342 0.2788 0.0545 0.082 Uiso 1 1 calc R . . H40B H 0.4435 0.2819 0.0737 0.082 Uiso 1 1 calc R . . H40C H 0.3490 0.2636 0.1270 0.082 Uiso 1 1 calc R . . C41 C 0.2103(6) -0.0543(5) -0.0200(4) 0.062(2) Uani 1 1 d . . . H41A H 0.2320 -0.1134 -0.0035 0.093 Uiso 1 1 calc R . . H41B H 0.2562 -0.0389 -0.0586 0.093 Uiso 1 1 calc R . . H41C H 0.1416 -0.0532 -0.0296 0.093 Uiso 1 1 calc R . . C42 C 0.0083(5) -0.1343(4) 0.3446(3) 0.0441(17) Uani 1 1 d . . . C43 C -0.0528(6) -0.2120(5) 0.3702(4) 0.064(2) Uani 1 1 d . . . H43A H -0.0268 -0.2408 0.4073 0.096 Uiso 1 1 calc R . . H43B H -0.0466 -0.2544 0.3374 0.096 Uiso 1 1 calc R . . H43C H -0.1241 -0.1905 0.3820 0.096 Uiso 1 1 calc R . . C44 C -0.0006(6) -0.0728(5) 0.3978(4) 0.057(2) Uani 1 1 d . . . H44A H 0.0411 -0.0242 0.3840 0.086 Uiso 1 1 calc R . . H44B H 0.0226 -0.1052 0.4346 0.086 Uiso 1 1 calc R . . H44C H -0.0713 -0.0493 0.4091 0.086 Uiso 1 1 calc R . . C45 C 0.1191(5) -0.1732(5) 0.3273(4) 0.054(2) Uani 1 1 d . . . H45A H 0.1621 -0.1253 0.3140 0.081 Uiso 1 1 calc R . . H45B H 0.1244 -0.2124 0.2926 0.081 Uiso 1 1 calc R . . H45C H 0.1410 -0.2064 0.3641 0.081 Uiso 1 1 calc R . . C46 C -0.2274(5) -0.1071(5) 0.1826(4) 0.053(2) Uani 1 1 d . . . H46A H -0.2756 -0.0582 0.1715 0.080 Uiso 1 1 calc R . . H46B H -0.2621 -0.1473 0.2145 0.080 Uiso 1 1 calc R . . H46C H -0.1989 -0.1389 0.1448 0.080 Uiso 1 1 calc R . . C47 C 0.1146(4) 0.2874(4) 0.3356(3) 0.0246(12) Uani 1 1 d . . . C48 C 0.0344(4) 0.2901(4) 0.3876(3) 0.0281(13) Uani 1 1 d . . . C49 C 0.0515(5) 0.3235(4) 0.4422(3) 0.0389(16) Uani 1 1 d . . . H49 H -0.0013 0.3246 0.4774 0.047 Uiso 1 1 calc R . . C50 C 0.1416(5) 0.3558(5) 0.4486(3) 0.0397(16) Uani 1 1 d . . . C51 C 0.2177(5) 0.3541(4) 0.3969(3) 0.0373(15) Uani 1 1 d . . . H51 H 0.2801 0.3755 0.4003 0.045 Uiso 1 1 calc R . . C52 C 0.2053(4) 0.3222(4) 0.3403(3) 0.0282(13) Uani 1 1 d . . . C53 C 0.4295(4) 0.2213(4) 0.3048(3) 0.0284(13) Uani 1 1 d . . . C54 C 0.5282(4) 0.2000(4) 0.3197(3) 0.0302(13) Uani 1 1 d . . . C55 C 0.5841(4) 0.2707(4) 0.3271(3) 0.0340(14) Uani 1 1 d . . . H55 H 0.6501 0.2572 0.3374 0.041 Uiso 1 1 calc R . . C56 C 0.5482(4) 0.3581(4) 0.3203(3) 0.0351(15) Uani 1 1 d . . . C57 C 0.4522(4) 0.3769(4) 0.3040(3) 0.0338(14) Uani 1 1 d . . . H57 H 0.4263 0.4365 0.2974 0.041 Uiso 1 1 calc R . . C58 C 0.3936(4) 0.3103(4) 0.2970(3) 0.0287(13) Uani 1 1 d . . . C59 C 0.2875(4) 0.3326(4) 0.2832(3) 0.0277(13) Uani 1 1 d . . . H59A H 0.2764 0.2944 0.2503 0.033 Uiso 1 1 calc R . . H59B H 0.2809 0.3942 0.2657 0.033 Uiso 1 1 calc R . . C60 C -0.0693(4) 0.2581(4) 0.3835(3) 0.0335(14) Uani 1 1 d . . . C61 C -0.1434(5) 0.2700(6) 0.4446(3) 0.056(2) Uani 1 1 d . . . H61A H -0.2073 0.2475 0.4406 0.085 Uiso 1 1 calc R . . H61B H -0.1556 0.3327 0.4528 0.085 Uiso 1 1 calc R . . H61C H -0.1150 0.2376 0.4797 0.085 Uiso 1 1 calc R . . C62 C -0.0567(5) 0.1600(5) 0.3722(4) 0.056(2) Uani 1 1 d . . . H62A H -0.1233 0.1387 0.3746 0.084 Uiso 1 1 calc R . . H62B H -0.0213 0.1278 0.4045 0.084 Uiso 1 1 calc R . . H62C H -0.0174 0.1505 0.3303 0.084 Uiso 1 1 calc R . . C63 C -0.1151(5) 0.3110(6) 0.3306(3) 0.056(2) Uani 1 1 d . . . H63A H -0.0697 0.3031 0.2905 0.084 Uiso 1 1 calc R . . H63B H -0.1245 0.3735 0.3395 0.084 Uiso 1 1 calc R . . H63C H -0.1807 0.2906 0.3279 0.084 Uiso 1 1 calc R . . C64 C 0.1546(6) 0.3927(6) 0.5096(3) 0.066(2) Uani 1 1 d . . . H64A H 0.1676 0.3443 0.5405 0.099 Uiso 1 1 calc R . . H64B H 0.0928 0.4290 0.5261 0.099 Uiso 1 1 calc R . . H64C H 0.2116 0.4288 0.5018 0.099 Uiso 1 1 calc R . . C65 C 0.5748(4) 0.1046(4) 0.3271(3) 0.0329(14) Uani 1 1 d . . . C66 C 0.6826(5) 0.0971(5) 0.3427(3) 0.0448(17) Uani 1 1 d . . . H66A H 0.7102 0.0352 0.3434 0.067 Uiso 1 1 calc R . . H66B H 0.6812 0.1200 0.3842 0.067 Uiso 1 1 calc R . . H66C H 0.7252 0.1313 0.3106 0.067 Uiso 1 1 calc R . . C67 C 0.5797(5) 0.0594(4) 0.2657(3) 0.0423(16) Uani 1 1 d . . . H67A H 0.5124 0.0651 0.2533 0.063 Uiso 1 1 calc R . . H67B H 0.6029 -0.0030 0.2719 0.063 Uiso 1 1 calc R . . H67C H 0.6269 0.0871 0.2324 0.063 Uiso 1 1 calc R . . C68 C 0.5104(5) 0.0559(4) 0.3816(3) 0.0438(17) Uani 1 1 d . . . H68A H 0.4411 0.0576 0.3728 0.066 Uiso 1 1 calc R . . H68B H 0.5099 0.0844 0.4210 0.066 Uiso 1 1 calc R . . H68C H 0.5390 -0.0055 0.3859 0.066 Uiso 1 1 calc R . . C69 C 0.6122(5) 0.4305(4) 0.3283(4) 0.0462(18) Uani 1 1 d . . . H69A H 0.6403 0.4184 0.3677 0.069 Uiso 1 1 calc R . . H69B H 0.5704 0.4869 0.3300 0.069 Uiso 1 1 calc R . . H69C H 0.6674 0.4330 0.2926 0.069 Uiso 1 1 calc R . . C70 C 0.1317(8) 0.2571(5) 0.0031(4) 0.079(3) Uani 1 1 d D . . H70A H 0.0790 0.2155 0.0101 0.094 Uiso 1 1 calc R . . H70B H 0.1984 0.2229 0.0029 0.094 Uiso 1 1 calc R . . C71 C 0.1289(12) 0.3082(6) -0.0573(4) 0.136(6) Uani 1 1 d D . . H71A H 0.0921 0.2787 -0.0847 0.164 Uiso 1 1 calc R . . H71B H 0.1982 0.3147 -0.0797 0.164 Uiso 1 1 calc R . . C72 C 0.0753(9) 0.3956(6) -0.0411(4) 0.088(3) Uani 1 1 d . . . H72A H 0.1128 0.4432 -0.0645 0.106 Uiso 1 1 calc R . . H72B H 0.0066 0.4011 -0.0524 0.106 Uiso 1 1 calc R . . C73 C 0.0696(5) 0.4020(4) 0.0276(3) 0.0346(14) Uani 1 1 d . . . H73A H 0.1075 0.4505 0.0361 0.041 Uiso 1 1 calc R . . H73B H -0.0016 0.4134 0.0479 0.041 Uiso 1 1 calc R . . C74 C 0.2297(8) 0.1131(6) 0.4481(4) 0.079(3) Uani 1 1 d . . . H74A H 0.1616 0.1414 0.4639 0.094 Uiso 1 1 calc R . . H74B H 0.2741 0.1596 0.4311 0.094 Uiso 1 1 calc R . . C75 C 0.2714(7) 0.0592(7) 0.5000(4) 0.079(3) Uani 1 1 d . . . H75A H 0.3446 0.0644 0.4972 0.095 Uiso 1 1 calc R . . H75B H 0.2364 0.0776 0.5418 0.095 Uiso 1 1 calc R . . C76 C 0.2531(10) -0.0310(7) 0.4903(4) 0.101(4) Uani 1 1 d D . . H76A H 0.1879 -0.0455 0.5153 0.121 Uiso 1 1 calc R . . H76B H 0.3076 -0.0732 0.5036 0.121 Uiso 1 1 calc R . . C77 C 0.2509(9) -0.0356(6) 0.4222(4) 0.090(3) Uani 1 1 d D . . H77A H 0.3179 -0.0584 0.4001 0.109 Uiso 1 1 calc R . . H77B H 0.2001 -0.0746 0.4154 0.109 Uiso 1 1 calc R . . C78 C 0.3949(6) -0.0983(5) 0.2724(4) 0.060(2) Uani 1 1 d . . . H78A H 0.3596 -0.1418 0.3020 0.072 Uiso 1 1 calc R . . H78B H 0.4370 -0.0674 0.2955 0.072 Uiso 1 1 calc R . . C79 C 0.4581(6) -0.1424(6) 0.2183(5) 0.073(3) Uani 1 1 d . . . H79A H 0.4892 -0.2008 0.2318 0.088 Uiso 1 1 calc R . . H79B H 0.5119 -0.1060 0.1973 0.088 Uiso 1 1 calc R . . C80 C 0.3806(8) -0.1507(7) 0.1754(5) 0.103(4) Uani 1 1 d . . . H80A H 0.4112 -0.1426 0.1304 0.124 Uiso 1 1 calc R . . H80B H 0.3548 -0.2094 0.1825 0.124 Uiso 1 1 calc R . . C81 C 0.2986(6) -0.0813(5) 0.1918(4) 0.056(2) Uani 1 1 d . . . H81A H 0.2335 -0.1072 0.2042 0.067 Uiso 1 1 calc R . . H81B H 0.2930 -0.0390 0.1552 0.067 Uiso 1 1 calc R . . C82 C 0.2040(5) 0.5900(5) 0.3507(4) 0.0460(17) Uani 1 1 d . . . C83 C 0.2614(6) 0.6090(5) 0.2932(4) 0.055(2) Uani 1 1 d . . . H83 H 0.2354 0.6014 0.2557 0.066 Uiso 1 1 calc R . . C84 C 0.3536(6) 0.6383(6) 0.2884(5) 0.072(3) Uani 1 1 d . . . H84 H 0.3915 0.6494 0.2478 0.087 Uiso 1 1 calc R . . C85 C 0.3924(8) 0.6518(6) 0.3404(7) 0.093(4) Uani 1 1 d . . . H85 H 0.4566 0.6736 0.3369 0.112 Uiso 1 1 calc R . . C86 C 0.3376(10) 0.6336(7) 0.3982(6) 0.104(4) Uani 1 1 d . . . H86 H 0.3644 0.6428 0.4351 0.125 Uiso 1 1 calc R . . C87 C 0.2437(7) 0.6020(6) 0.4044(4) 0.071(2) Uani 1 1 d . . . H87 H 0.2070 0.5887 0.4450 0.086 Uiso 1 1 calc R . . C88 C 0.1016(6) 0.5585(6) 0.3559(4) 0.073(3) Uani 1 1 d . . . H88A H 0.0723 0.5506 0.4006 0.109 Uiso 1 1 calc R . . H88B H 0.1073 0.5023 0.3361 0.109 Uiso 1 1 calc R . . H88C H 0.0578 0.6020 0.3346 0.109 Uiso 1 1 calc R . . C89A C 0.5736(16) 0.7072(12) 0.4521(9) 0.100(7) Uiso 0.55 1 d PD . . C89B C 0.5845(15) 0.6490(13) 0.4593(9) 0.069(5) Uiso 0.45 1 d PD . . C90A C 0.5780(17) 0.7930(13) 0.4255(10) 0.082(5) Uiso 0.55 1 d PD . . C90B C 0.535(2) 0.7245(16) 0.4876(15) 0.108(9) Uiso 0.45 1 d PD . . C91A C 0.6339(13) 0.7992(10) 0.3638(8) 0.063(4) Uiso 0.55 1 d PD . . C91B C 0.545(2) 0.8021(19) 0.4503(14) 0.119(11) Uiso 0.45 1 d PD . . C92A C 0.6840(16) 0.7257(11) 0.3314(10) 0.090(7) Uiso 0.55 1 d PD . . C92B C 0.607(3) 0.791(2) 0.3919(16) 0.124(11) Uiso 0.45 1 d PD . . C93A C 0.6756(14) 0.6419(11) 0.3627(8) 0.080(5) Uiso 0.55 1 d PD . . C93B C 0.663(2) 0.7217(16) 0.3597(14) 0.109(10) Uiso 0.45 1 d PD . . C94A C 0.6185(13) 0.6314(11) 0.4229(9) 0.064(5) Uiso 0.55 1 d PD . . C94B C 0.6408(17) 0.6473(14) 0.3986(11) 0.068(6) Uiso 0.45 1 d PD . . C95A C 0.5202(17) 0.6915(16) 0.5198(10) 0.110(8) Uiso 0.55 1 d PD . . C95B C 0.566(2) 0.5669(16) 0.5006(12) 0.118(9) Uiso 0.45 1 d PD . . 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 La1 0.02461(18) 0.02106(19) 0.0310(2) 0.00200(14) -0.00799(15) 0.00133(14) La2 0.02492(18) 0.02306(19) 0.0361(2) 0.00384(15) -0.01124(15) -0.00156(15) O1 0.025(2) 0.019(2) 0.042(2) -0.0011(17) -0.0054(18) 0.0023(17) O2 0.026(2) 0.025(2) 0.036(2) -0.0002(17) -0.0090(18) 0.0028(17) O3 0.025(2) 0.021(2) 0.031(2) -0.0040(17) -0.0072(17) 0.0019(17) O4 0.031(2) 0.027(2) 0.042(3) 0.0027(18) -0.0088(19) -0.0060(18) O5 0.0214(19) 0.028(2) 0.025(2) -0.0038(17) -0.0048(16) -0.0036(17) O6 0.027(2) 0.031(2) 0.041(2) -0.0013(18) -0.0134(18) -0.0048(18) O7 0.053(3) 0.035(3) 0.037(3) -0.005(2) -0.010(2) 0.013(2) O8 0.066(3) 0.061(3) 0.045(3) 0.015(3) -0.023(3) -0.018(3) O9 0.044(3) 0.039(3) 0.062(3) -0.001(2) -0.016(2) 0.002(2) C1 0.026(3) 0.020(3) 0.027(3) 0.000(2) -0.009(2) 0.001(2) C2 0.023(3) 0.023(3) 0.029(3) -0.002(2) -0.006(2) 0.001(2) C3 0.037(3) 0.025(3) 0.031(3) 0.000(3) -0.002(3) -0.003(3) C4 0.034(3) 0.021(3) 0.045(4) -0.003(3) -0.005(3) 0.002(3) C5 0.023(3) 0.029(3) 0.039(4) -0.007(3) -0.002(3) 0.004(3) C6 0.024(3) 0.026(3) 0.024(3) -0.004(2) -0.007(2) 0.000(2) C7 0.027(3) 0.028(3) 0.023(3) 0.002(2) -0.005(2) 0.000(3) C8 0.025(3) 0.031(3) 0.032(3) 0.003(3) -0.007(3) -0.006(3) C9 0.023(3) 0.038(4) 0.048(4) -0.003(3) -0.012(3) 0.003(3) C10 0.024(3) 0.043(4) 0.051(4) -0.003(3) -0.009(3) 0.008(3) C11 0.035(3) 0.023(3) 0.047(4) -0.004(3) -0.001(3) 0.002(3) C12 0.021(3) 0.029(3) 0.028(3) 0.004(2) -0.002(2) -0.002(2) C13 0.027(3) 0.028(3) 0.026(3) 0.000(2) -0.004(2) -0.003(3) C14 0.029(3) 0.030(3) 0.044(4) -0.003(3) 0.002(3) -0.002(3) C15 0.035(4) 0.045(4) 0.066(5) 0.000(4) 0.012(4) -0.005(3) C16 0.038(4) 0.039(4) 0.040(4) 0.000(3) 0.007(3) -0.001(3) C17 0.026(3) 0.045(4) 0.063(5) -0.002(3) -0.011(3) 0.002(3) C18 0.057(5) 0.028(4) 0.063(5) 0.000(3) 0.005(4) 0.003(3) C19 0.028(3) 0.039(4) 0.041(4) -0.001(3) -0.006(3) -0.007(3) C20 0.038(4) 0.047(4) 0.069(5) -0.007(4) -0.020(4) -0.009(3) C21 0.033(3) 0.030(4) 0.055(4) 0.000(3) -0.008(3) -0.008(3) C22 0.047(4) 0.048(4) 0.046(4) -0.013(3) -0.013(3) -0.009(3) C23 0.042(4) 0.046(5) 0.111(7) -0.023(5) -0.024(4) 0.019(4) C24 0.029(3) 0.013(3) 0.031(3) -0.006(2) -0.009(3) 0.006(2) C25 0.034(3) 0.019(3) 0.031(3) -0.003(2) -0.005(3) 0.005(3) C26 0.040(4) 0.027(3) 0.036(4) -0.006(3) -0.001(3) 0.005(3) C27 0.050(4) 0.028(3) 0.033(4) -0.007(3) -0.009(3) -0.003(3) C28 0.047(4) 0.027(3) 0.039(4) -0.001(3) -0.015(3) -0.007(3) C29 0.033(3) 0.019(3) 0.033(3) 0.003(2) -0.006(3) 0.001(3) C30 0.022(3) 0.022(3) 0.046(4) -0.004(3) -0.007(3) -0.005(2) C31 0.032(3) 0.023(3) 0.047(4) -0.001(3) -0.003(3) -0.003(3) C32 0.033(3) 0.025(3) 0.060(5) 0.001(3) 0.007(3) -0.008(3) C33 0.025(3) 0.031(4) 0.059(5) -0.010(3) -0.005(3) -0.007(3) C34 0.026(3) 0.029(3) 0.049(4) -0.005(3) -0.010(3) 0.002(3) C35 0.027(3) 0.020(3) 0.045(4) -0.005(3) -0.004(3) -0.002(3) C36 0.020(3) 0.029(3) 0.042(4) -0.004(3) -0.009(3) -0.002(3) C37 0.029(3) 0.021(3) 0.041(4) -0.002(3) 0.002(3) -0.003(3) C38 0.048(4) 0.058(5) 0.053(5) -0.010(4) 0.007(4) -0.011(4) C39 0.041(4) 0.064(5) 0.068(5) 0.015(4) -0.014(4) -0.006(4) C40 0.042(4) 0.032(4) 0.086(6) -0.010(4) 0.001(4) 0.000(3) C41 0.081(6) 0.058(5) 0.050(5) -0.024(4) -0.008(4) -0.008(4) C42 0.043(4) 0.033(4) 0.054(4) 0.009(3) -0.002(3) -0.009(3) C43 0.066(5) 0.044(5) 0.084(6) 0.034(4) -0.020(5) -0.024(4) C44 0.062(5) 0.045(4) 0.062(5) 0.013(4) -0.007(4) -0.009(4) C45 0.045(4) 0.039(4) 0.078(6) 0.012(4) -0.015(4) 0.001(3) C46 0.035(4) 0.046(4) 0.083(6) -0.015(4) -0.009(4) -0.015(3) C47 0.026(3) 0.020(3) 0.029(3) -0.001(2) -0.011(2) 0.003(2) C48 0.024(3) 0.032(3) 0.029(3) 0.000(3) -0.006(3) -0.001(3) C49 0.031(3) 0.053(4) 0.032(4) -0.004(3) -0.001(3) -0.004(3) C50 0.039(4) 0.053(4) 0.031(4) -0.010(3) -0.007(3) -0.014(3) C51 0.031(3) 0.041(4) 0.044(4) -0.004(3) -0.014(3) -0.008(3) C52 0.028(3) 0.028(3) 0.027(3) -0.002(3) -0.004(3) 0.002(3) C53 0.025(3) 0.028(3) 0.033(3) 0.003(3) -0.009(3) -0.003(3) C54 0.025(3) 0.031(3) 0.033(3) 0.001(3) -0.002(3) 0.000(3) C55 0.019(3) 0.043(4) 0.039(4) -0.004(3) -0.007(3) 0.004(3) C56 0.029(3) 0.033(4) 0.043(4) -0.005(3) -0.005(3) -0.003(3) C57 0.029(3) 0.027(3) 0.044(4) -0.008(3) -0.005(3) 0.004(3) C58 0.021(3) 0.036(4) 0.031(3) -0.001(3) -0.008(2) -0.003(3) C59 0.026(3) 0.027(3) 0.030(3) 0.001(3) -0.005(3) -0.003(3) C60 0.021(3) 0.049(4) 0.031(3) -0.002(3) -0.004(3) -0.005(3) C61 0.035(4) 0.089(6) 0.047(5) -0.011(4) 0.002(3) -0.021(4) C62 0.038(4) 0.045(4) 0.085(6) -0.016(4) 0.002(4) -0.012(3) C63 0.023(3) 0.088(6) 0.057(5) 0.017(4) -0.016(3) -0.008(4) C64 0.059(5) 0.105(7) 0.041(4) -0.024(4) -0.005(4) -0.035(5) C65 0.025(3) 0.027(3) 0.046(4) 0.006(3) -0.013(3) 0.004(3) C66 0.031(3) 0.043(4) 0.061(5) 0.005(3) -0.016(3) 0.002(3) C67 0.036(4) 0.031(4) 0.059(5) -0.002(3) -0.011(3) 0.005(3) C68 0.033(3) 0.043(4) 0.054(4) 0.010(3) -0.013(3) 0.003(3) C69 0.028(3) 0.041(4) 0.072(5) -0.005(4) -0.013(3) -0.006(3) C70 0.127(8) 0.055(5) 0.048(5) -0.013(4) -0.023(5) 0.039(5) C71 0.269(17) 0.069(7) 0.054(6) -0.013(5) -0.029(8) 0.077(9) C72 0.154(10) 0.055(5) 0.040(5) -0.003(4) -0.015(5) 0.051(6) C73 0.039(3) 0.025(3) 0.037(4) 0.007(3) -0.007(3) 0.006(3) C74 0.089(7) 0.084(7) 0.059(6) 0.003(5) -0.007(5) -0.004(6) C75 0.067(6) 0.124(9) 0.048(5) 0.002(5) -0.010(4) -0.021(6) C76 0.152(11) 0.083(8) 0.063(6) 0.026(5) -0.034(7) 0.013(7) C77 0.130(9) 0.068(6) 0.088(7) 0.040(5) -0.059(7) -0.040(6) C78 0.051(5) 0.049(5) 0.086(6) 0.001(4) -0.030(4) -0.001(4) C79 0.050(5) 0.052(5) 0.115(8) -0.010(5) -0.017(5) 0.019(4) C80 0.091(7) 0.093(8) 0.122(9) -0.042(7) -0.026(7) 0.044(6) C81 0.061(5) 0.044(4) 0.064(5) 0.002(4) -0.020(4) 0.002(4) C82 0.044(4) 0.039(4) 0.058(5) -0.014(3) -0.021(4) 0.007(3) C83 0.060(5) 0.056(5) 0.051(5) -0.019(4) -0.017(4) 0.016(4) C84 0.051(5) 0.067(6) 0.095(7) -0.009(5) -0.008(5) 0.011(5) C85 0.068(6) 0.061(6) 0.164(12) 0.020(7) -0.062(8) -0.017(5) C86 0.136(10) 0.086(8) 0.116(10) 0.013(7) -0.092(9) -0.034(8) C87 0.091(7) 0.064(6) 0.065(6) -0.006(4) -0.027(5) -0.007(5) C88 0.056(5) 0.076(6) 0.087(7) -0.010(5) -0.025(5) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.199(4) . ? La1 O2 2.211(4) . ? La1 O5 2.431(4) . ? La1 O3 2.475(4) . ? La1 O7 2.564(4) . ? La1 La2 4.0458(5) . ? La2 O6 2.283(4) . ? La2 O4 2.289(4) . ? La2 O3 2.436(4) . ? La2 O5 2.500(4) . ? La2 O8 2.571(5) . ? La2 O9 2.616(5) . ? La2 C47 3.125(5) . ? O1 C1 1.342(6) . ? O2 C7 1.349(6) . ? O3 C24 1.367(6) . ? O4 C30 1.346(7) . ? O5 C47 1.371(6) . ? O6 C53 1.348(7) . ? O7 C70 1.427(8) . ? O7 C73 1.468(7) . ? O8 C77 1.448(9) . ? O8 C74 1.459(10) . ? O9 C78 1.449(8) . ? O9 C81 1.479(8) . ? C1 C2 1.410(7) . ? C1 C6 1.422(7) . ? C2 C3 1.396(8) . ? C2 C14 1.540(8) . ? C3 C4 1.379(8) . ? C3 H3 0.9500 . ? C4 C5 1.379(8) . ? C4 C18 1.511(8) . ? C5 C6 1.385(8) . ? C5 H5 0.9500 . ? C6 C13 1.522(7) . ? C7 C12 1.405(8) . ? C7 C8 1.421(8) . ? C8 C9 1.388(8) . ? C8 C19 1.525(8) . ? C9 C10 1.393(9) . ? C9 H9 0.9500 . ? C10 C11 1.383(8) . ? C10 C23 1.506(9) . ? C11 C12 1.389(8) . ? C11 H11 0.9500 . ? C12 C13 1.534(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C16 1.522(9) . ? C14 C15 1.541(8) . ? C14 C17 1.548(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C22 1.530(9) . ? C19 C20 1.534(8) . ? C19 C21 1.546(9) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.406(8) . ? C24 C25 1.416(8) . ? C25 C26 1.388(8) . ? C25 C37 1.539(8) . ? C26 C27 1.394(9) . ? C26 H26 0.9500 . ? C27 C28 1.401(9) . ? C27 C41 1.514(9) . ? C28 C29 1.385(8) . ? C28 H28 0.9500 . ? C29 C36 1.529(8) . ? C30 C35 1.407(8) . ? C30 C31 1.418(8) . ? C31 C32 1.398(9) . ? C31 C42 1.532(9) . ? C32 C33 1.392(9) . ? C32 H32 0.9500 . ? C33 C34 1.375(8) . ? C33 C46 1.511(9) . ? C34 C35 1.389(8) . ? C34 H34 0.9500 . ? C35 C36 1.509(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C39 1.517(9) . ? C37 C40 1.535(8) . ? C37 C38 1.539(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.517(10) . ? C42 C43 1.536(8) . ? C42 C45 1.543(9) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C52 1.407(8) . ? C47 C48 1.421(8) . ? C48 C49 1.378(8) . ? C48 C60 1.548(8) . ? C49 C50 1.390(8) . ? C49 H49 0.9500 . ? C50 C51 1.382(9) . ? C50 C64 1.510(9) . ? C51 C52 1.386(8) . ? C51 H51 0.9500 . ? C52 C59 1.525(8) . ? C53 C58 1.403(8) . ? C53 C54 1.419(8) . ? C54 C55 1.416(8) . ? C54 C65 1.534(8) . ? C55 C56 1.379(8) . ? C55 H55 0.9500 . ? C56 C57 1.392(8) . ? C56 C69 1.512(8) . ? C57 C58 1.385(8) . ? C57 H57 0.9500 . ? C58 C59 1.507(7) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C63 1.522(9) . ? C60 C61 1.523(8) . ? C60 C62 1.527(9) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C67 1.524(9) . ? C65 C66 1.536(8) . ? C65 C68 1.536(8) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.469(10) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.489(11) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.475(9) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.488(12) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.464(13) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.477(11) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.484(11) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.525(13) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.467(11) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.374(10) . ? C82 C87 1.382(10) . ? C82 C88 1.495(10) . ? C83 C84 1.350(11) . ? C83 H83 0.9500 . ? C84 C85 1.349(13) . ? C84 H84 0.9500 . ? C85 C86 1.363(15) . ? C85 H85 0.9500 . ? C86 C87 1.387(14) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89A C94A 1.393(17) . ? C89A C90A 1.397(17) . ? C89A C95A 1.528(17) . ? C89B C94B 1.398(18) . ? C89B C90B 1.399(18) . ? C89B C95B 1.504(18) . ? C90A C91A 1.416(18) . ? C90B C91B 1.389(18) . ? C91A C92A 1.418(16) . ? C91B C92B 1.400(19) . ? C92A C93A 1.409(17) . ? C92B C93B 1.392(19) . ? C93A C94A 1.401(17) . ? C93B C94B 1.392(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O2 96.53(13) . . ? O1 La1 O5 108.92(13) . . ? O2 La1 O5 100.26(13) . . ? O1 La1 O3 123.01(13) . . ? O2 La1 O3 140.45(13) . . ? O5 La1 O3 69.65(12) . . ? O1 La1 O7 89.59(14) . . ? O2 La1 O7 82.83(14) . . ? O5 La1 O7 160.59(13) . . ? O3 La1 O7 95.67(13) . . ? O1 La1 La2 122.42(10) . . ? O2 La1 La2 125.45(10) . . ? O5 La1 La2 35.43(8) . . ? O3 La1 La2 34.23(9) . . ? O7 La1 La2 128.72(9) . . ? O6 La2 O4 163.06(14) . . ? O6 La2 O3 95.43(13) . . ? O4 La2 O3 92.49(13) . . ? O6 La2 O5 101.43(13) . . ? O4 La2 O5 95.38(13) . . ? O3 La2 O5 69.15(12) . . ? O6 La2 O8 80.85(15) . . ? O4 La2 O8 91.53(15) . . ? O3 La2 O8 175.92(14) . . ? O5 La2 O8 109.80(15) . . ? O6 La2 O9 88.60(14) . . ? O4 La2 O9 76.22(14) . . ? O3 La2 O9 91.58(13) . . ? O5 La2 O9 158.86(13) . . ? O8 La2 O9 90.02(16) . . ? O6 La2 C47 86.70(14) . . ? O4 La2 C47 108.19(14) . . ? O3 La2 C47 90.69(13) . . ? O5 La2 C47 25.23(12) . . ? O8 La2 C47 87.42(16) . . ? O9 La2 C47 174.95(14) . . ? O6 La2 La1 100.60(10) . . ? O4 La2 La1 94.46(10) . . ? O3 La2 La1 34.85(8) . . ? O5 La2 La1 34.30(8) . . ? O8 La2 La1 144.00(12) . . ? O9 La2 La1 125.88(11) . . ? C47 La2 La1 57.00(10) . . ? C1 O1 La1 149.6(3) . . ? C7 O2 La1 153.0(3) . . ? C24 O3 La2 123.8(3) . . ? C24 O3 La1 111.1(3) . . ? La2 O3 La1 110.92(14) . . ? C30 O4 La2 161.9(4) . . ? C47 O5 La1 133.4(3) . . ? C47 O5 La2 103.8(3) . . ? La1 O5 La2 110.27(13) . . ? C53 O6 La2 154.8(4) . . ? C70 O7 C73 108.7(5) . . ? C70 O7 La1 137.1(4) . . ? C73 O7 La1 113.3(3) . . ? C77 O8 C74 108.6(6) . . ? C77 O8 La2 127.3(5) . . ? C74 O8 La2 121.7(5) . . ? C78 O9 C81 104.4(5) . . ? C78 O9 La2 132.7(4) . . ? C81 O9 La2 121.9(4) . . ? O1 C1 C2 121.9(5) . . ? O1 C1 C6 118.7(5) . . ? C2 C1 C6 119.4(5) . . ? C3 C2 C1 117.8(5) . . ? C3 C2 C14 120.0(5) . . ? C1 C2 C14 122.2(5) . . ? C4 C3 C2 123.8(6) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C5 C4 C3 117.0(5) . . ? C5 C4 C18 122.4(6) . . ? C3 C4 C18 120.6(6) . . ? C4 C5 C6 123.0(5) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C5 C6 C1 118.9(5) . . ? C5 C6 C13 119.3(5) . . ? C1 C6 C13 121.8(5) . . ? O2 C7 C12 118.6(5) . . ? O2 C7 C8 121.6(5) . . ? C12 C7 C8 119.7(5) . . ? C9 C8 C7 117.3(5) . . ? C9 C8 C19 121.0(5) . . ? C7 C8 C19 121.7(5) . . ? C8 C9 C10 124.0(6) . . ? C8 C9 H9 118.0 . . ? C10 C9 H9 118.0 . . ? C11 C10 C9 117.1(6) . . ? C11 C10 C23 121.7(6) . . ? C9 C10 C23 121.2(6) . . ? C10 C11 C12 122.0(6) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 119.8(5) . . ? C11 C12 C13 118.4(5) . . ? C7 C12 C13 121.8(5) . . ? C6 C13 C12 118.2(5) . . ? C6 C13 H13A 107.8 . . ? C12 C13 H13A 107.8 . . ? C6 C13 H13B 107.8 . . ? C12 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? C16 C14 C2 109.7(5) . . ? C16 C14 C15 107.6(5) . . ? C2 C14 C15 112.4(5) . . ? C16 C14 C17 110.1(5) . . ? C2 C14 C17 110.7(5) . . ? C15 C14 C17 106.2(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C19 C22 110.6(5) . . ? C8 C19 C20 112.2(5) . . ? C22 C19 C20 107.6(5) . . ? C8 C19 C21 110.2(5) . . ? C22 C19 C21 109.6(5) . . ? C20 C19 C21 106.4(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 C29 118.6(5) . . ? O3 C24 C25 121.1(5) . . ? C29 C24 C25 120.4(5) . . ? C26 C25 C24 117.0(5) . . ? C26 C25 C37 120.2(5) . . ? C24 C25 C37 122.8(5) . . ? C25 C26 C27 123.7(6) . . ? C25 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C26 C27 C28 117.6(6) . . ? C26 C27 C41 121.4(6) . . ? C28 C27 C41 121.0(6) . . ? C29 C28 C27 121.1(6) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C24 119.8(5) . . ? C28 C29 C36 118.2(5) . . ? C24 C29 C36 122.0(5) . . ? O4 C30 C35 117.9(5) . . ? O4 C30 C31 123.2(5) . . ? C35 C30 C31 118.9(5) . . ? C32 C31 C30 118.0(6) . . ? C32 C31 C42 119.7(5) . . ? C30 C31 C42 122.3(5) . . ? C33 C32 C31 123.4(6) . . ? C33 C32 H32 118.3 . . ? C31 C32 H32 118.3 . . ? C34 C33 C32 117.3(6) . . ? C34 C33 C46 121.7(6) . . ? C32 C33 C46 121.0(6) . . ? C33 C34 C35 122.3(6) . . ? C33 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C34 C35 C30 120.2(5) . . ? C34 C35 C36 120.7(6) . . ? C30 C35 C36 119.2(5) . . ? C35 C36 C29 116.0(5) . . ? C35 C36 H36A 108.3 . . ? C29 C36 H36A 108.3 . . ? C35 C36 H36B 108.3 . . ? C29 C36 H36B 108.3 . . ? H36A C36 H36B 107.4 . . ? C39 C37 C40 109.7(6) . . ? C39 C37 C38 108.4(6) . . ? C40 C37 C38 105.4(5) . . ? C39 C37 C25 110.5(5) . . ? C40 C37 C25 111.0(5) . . ? C38 C37 C25 111.7(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 C41 H41A 109.5 . . ? C27 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C27 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C31 110.3(6) . . ? C44 C42 C43 107.2(6) . . ? C31 C42 C43 113.5(6) . . ? C44 C42 C45 109.9(6) . . ? C31 C42 C45 109.4(6) . . ? C43 C42 C45 106.4(6) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C33 C46 H46A 109.5 . . ? C33 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C33 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C52 117.5(5) . . ? O5 C47 C48 122.7(5) . . ? C52 C47 C48 119.7(5) . . ? O5 C47 La2 51.0(2) . . ? C52 C47 La2 94.6(3) . . ? C48 C47 La2 122.0(4) . . ? C49 C48 C47 117.6(5) . . ? C49 C48 C60 120.5(5) . . ? C47 C48 C60 121.9(5) . . ? C48 C49 C50 123.7(6) . . ? C48 C49 H49 118.2 . . ? C50 C49 H49 118.2 . . ? C51 C50 C49 117.6(6) . . ? C51 C50 C64 121.5(6) . . ? C49 C50 C64 120.8(6) . . ? C50 C51 C52 121.7(6) . . ? C50 C51 H51 119.1 . . ? C52 C51 H51 119.1 . . ? C51 C52 C47 119.6(5) . . ? C51 C52 C59 118.7(5) . . ? C47 C52 C59 121.6(5) . . ? O6 C53 C58 118.7(5) . . ? O6 C53 C54 122.6(5) . . ? C58 C53 C54 118.7(5) . . ? C55 C54 C53 117.4(5) . . ? C55 C54 C65 120.3(5) . . ? C53 C54 C65 122.3(5) . . ? C56 C55 C54 123.8(5) . . ? C56 C55 H55 118.1 . . ? C54 C55 H55 118.1 . . ? C55 C56 C57 117.4(5) . . ? C55 C56 C69 121.1(6) . . ? C57 C56 C69 121.5(6) . . ? C58 C57 C56 121.2(6) . . ? C58 C57 H57 119.4 . . ? C56 C57 H57 119.4 . . ? C57 C58 C53 121.4(5) . . ? C57 C58 C59 120.0(5) . . ? C53 C58 C59 118.5(5) . . ? C58 C59 C52 114.4(5) . . ? C58 C59 H59A 108.7 . . ? C52 C59 H59A 108.7 . . ? C58 C59 H59B 108.7 . . ? C52 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? C63 C60 C61 107.8(6) . . ? C63 C60 C62 110.8(6) . . ? C61 C60 C62 106.9(6) . . ? C63 C60 C48 109.4(5) . . ? C61 C60 C48 111.9(5) . . ? C62 C60 C48 109.9(5) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C50 C64 H64A 109.5 . . ? C50 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C50 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C67 C65 C54 109.7(5) . . ? C67 C65 C66 107.3(5) . . ? C54 C65 C66 113.3(5) . . ? C67 C65 C68 110.4(5) . . ? C54 C65 C68 109.2(5) . . ? C66 C65 C68 106.8(5) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C56 C69 H69A 109.5 . . ? C56 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C56 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O7 C70 C71 107.9(7) . . ? O7 C70 H70A 110.1 . . ? C71 C70 H70A 110.1 . . ? O7 C70 H70B 110.1 . . ? C71 C70 H70B 110.1 . . ? H70A C70 H70B 108.4 . . ? C70 C71 C72 105.9(7) . . ? C70 C71 H71A 110.6 . . ? C72 C71 H71A 110.6 . . ? C70 C71 H71B 110.6 . . ? C72 C71 H71B 110.6 . . ? H71A C71 H71B 108.7 . . ? C73 C72 C71 107.3(6) . . ? C73 C72 H72A 110.2 . . ? C71 C72 H72A 110.2 . . ? C73 C72 H72B 110.2 . . ? C71 C72 H72B 110.2 . . ? H72A C72 H72B 108.5 . . ? O7 C73 C72 106.7(5) . . ? O7 C73 H73A 110.4 . . ? C72 C73 H73A 110.4 . . ? O7 C73 H73B 110.4 . . ? C72 C73 H73B 110.4 . . ? H73A C73 H73B 108.6 . . ? O8 C74 C75 107.1(8) . . ? O8 C74 H74A 110.3 . . ? C75 C74 H74A 110.3 . . ? O8 C74 H74B 110.3 . . ? C75 C74 H74B 110.3 . . ? H74A C74 H74B 108.6 . . ? C76 C75 C74 104.3(8) . . ? C76 C75 H75A 110.9 . . ? C74 C75 H75A 110.9 . . ? C76 C75 H75B 110.9 . . ? C74 C75 H75B 110.9 . . ? H75A C75 H75B 108.9 . . ? C75 C76 C77 106.9(8) . . ? C75 C76 H76A 110.3 . . ? C77 C76 H76A 110.3 . . ? C75 C76 H76B 110.3 . . ? C77 C76 H76B 110.3 . . ? H76A C76 H76B 108.6 . . ? O8 C77 C76 105.8(8) . . ? O8 C77 H77A 110.6 . . ? C76 C77 H77A 110.6 . . ? O8 C77 H77B 110.6 . . ? C76 C77 H77B 110.6 . . ? H77A C77 H77B 108.7 . . ? O9 C78 C79 105.7(7) . . ? O9 C78 H78A 110.6 . . ? C79 C78 H78A 110.6 . . ? O9 C78 H78B 110.6 . . ? C79 C78 H78B 110.6 . . ? H78A C78 H78B 108.7 . . ? C78 C79 C80 101.7(7) . . ? C78 C79 H79A 111.4 . . ? C80 C79 H79A 111.4 . . ? C78 C79 H79B 111.4 . . ? C80 C79 H79B 111.4 . . ? H79A C79 H79B 109.3 . . ? C81 C80 C79 106.1(8) . . ? C81 C80 H80A 110.5 . . ? C79 C80 H80A 110.5 . . ? C81 C80 H80B 110.5 . . ? C79 C80 H80B 110.5 . . ? H80A C80 H80B 108.7 . . ? C80 C81 O9 107.6(7) . . ? C80 C81 H81A 110.2 . . ? O9 C81 H81A 110.2 . . ? C80 C81 H81B 110.2 . . ? O9 C81 H81B 110.2 . . ? H81A C81 H81B 108.5 . . ? C83 C82 C87 117.6(7) . . ? C83 C82 C88 122.1(7) . . ? C87 C82 C88 120.3(8) . . ? C84 C83 C82 122.1(8) . . ? C84 C83 H83 118.9 . . ? C82 C83 H83 118.9 . . ? C85 C84 C83 120.9(10) . . ? C85 C84 H84 119.6 . . ? C83 C84 H84 119.6 . . ? C84 C85 C86 118.6(9) . . ? C84 C85 H85 120.7 . . ? C86 C85 H85 120.7 . . ? C85 C86 C87 121.6(9) . . ? C85 C86 H86 119.2 . . ? C87 C86 H86 119.2 . . ? C82 C87 C86 119.2(9) . . ? C82 C87 H87 120.4 . . ? C86 C87 H87 120.4 . . ? C82 C88 H88A 109.5 . . ? C82 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C82 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C94A C89A C90A 125.3(18) . . ? C94A C89A C95A 114.9(18) . . ? C90A C89A C95A 119.7(19) . . ? C94B C89B C90B 125(2) . . ? C94B C89B C95B 123(2) . . ? C90B C89B C95B 112(2) . . ? C89A C90A C91A 114.4(17) . . ? C91B C90B C89B 115(3) . . ? C90A C91A C92A 123.8(16) . . ? C90B C91B C92B 114(3) . . ? C93A C92A C91A 117.3(18) . . ? C93B C92B C91B 137(3) . . ? C94A C93A C92A 121.4(17) . . ? C94B C93B C92B 104(3) . . ? C89A C94A C93A 117.7(17) . . ? C93B C94B C89B 125(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.413 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.106 # Attachment 'Qi-dalton.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 682654' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H59 La O5' _chemical_formula_sum 'C40 H59 La O5' _chemical_formula_weight 758.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 20.652(4) _cell_length_b 9.8049(17) _cell_length_c 18.579(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.742(5) _cell_angle_gamma 90.00 _cell_volume 3743.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 13415 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.521 _exptl_absorpt_correction_T_max 0.703 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34877 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6841 _reflns_number_gt 6161 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0184P)^2^+7.4936P] 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 6841 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _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 La1 La 0.812308(10) 0.68103(2) 0.459895(11) 0.02295(8) Uani 1 1 d . . . O1 O 0.71453(12) 0.6836(3) 0.50134(13) 0.0270(6) Uani 1 1 d . . . O2 O 0.80097(13) 0.4676(3) 0.41146(14) 0.0307(6) Uani 1 1 d . . . O3 O 0.73513(13) 0.7629(3) 0.34563(15) 0.0393(7) Uani 1 1 d . . . O4 O 0.84047(14) 0.9454(3) 0.44552(15) 0.0372(7) Uani 1 1 d . . . O5 O 0.90218(13) 0.7195(3) 0.36579(14) 0.0338(7) Uani 1 1 d . . . C1 C 0.66191(18) 0.6322(4) 0.5301(2) 0.0247(8) Uani 1 1 d . . . C2 C 0.61342(18) 0.7185(4) 0.5542(2) 0.0260(9) Uani 1 1 d . . . C3 C 0.56026(17) 0.6564(4) 0.5825(2) 0.0311(10) Uani 1 1 d . . . H3 H 0.5278 0.7132 0.5996 0.037 Uiso 1 1 calc R . . C4 C 0.55287(18) 0.5160(4) 0.5869(2) 0.0299(9) Uani 1 1 d . . . C5 C 0.60173(19) 0.4343(4) 0.5641(2) 0.0285(9) Uani 1 1 d . . . H5 H 0.5984 0.3380 0.5683 0.034 Uiso 1 1 calc R . . C6 C 0.65548(18) 0.4898(4) 0.5351(2) 0.0261(9) Uani 1 1 d . . . C7 C 0.75071(19) 0.3880(4) 0.3860(2) 0.0264(9) Uani 1 1 d . . . C8 C 0.74731(19) 0.3299(4) 0.3153(2) 0.0265(9) Uani 1 1 d . . . C9 C 0.6900(2) 0.2636(4) 0.2892(2) 0.0341(10) Uani 1 1 d . . . H9 H 0.6869 0.2277 0.2414 0.041 Uiso 1 1 calc R . . C10 C 0.6372(2) 0.2473(5) 0.3294(2) 0.0390(11) Uani 1 1 d . . . C11 C 0.6445(2) 0.2932(4) 0.4001(2) 0.0329(10) Uani 1 1 d . . . H11 H 0.6102 0.2783 0.4296 0.039 Uiso 1 1 calc R . . C12 C 0.69998(19) 0.3600(4) 0.4296(2) 0.0272(9) Uani 1 1 d . . . C13 C 0.70666(19) 0.3951(4) 0.5102(2) 0.0290(9) Uani 1 1 d . . . H13A H 0.7058 0.3091 0.5380 0.035 Uiso 1 1 calc R . . H13B H 0.7499 0.4374 0.5226 0.035 Uiso 1 1 calc R . . C14 C 0.61791(19) 0.8740(4) 0.5492(2) 0.0308(9) Uani 1 1 d . . . C15 C 0.5606(2) 0.9479(5) 0.5800(2) 0.0407(11) Uani 1 1 d . . . H15A H 0.5195 0.9180 0.5538 0.061 Uiso 1 1 calc R . . H15B H 0.5654 1.0466 0.5742 0.061 Uiso 1 1 calc R . . H15C H 0.5605 0.9260 0.6314 0.061 Uiso 1 1 calc R . . C16 C 0.6176(2) 0.9159(5) 0.4698(2) 0.0394(11) Uani 1 1 d . . . H16A H 0.6539 0.8715 0.4489 0.059 Uiso 1 1 calc R . . H16B H 0.6223 1.0151 0.4667 0.059 Uiso 1 1 calc R . . H16C H 0.5765 0.8880 0.4431 0.059 Uiso 1 1 calc R . . C17 C 0.6801(2) 0.9258(4) 0.5934(2) 0.0390(11) Uani 1 1 d . . . H17A H 0.6773 0.9078 0.6449 0.058 Uiso 1 1 calc R . . H17B H 0.6846 1.0241 0.5858 0.058 Uiso 1 1 calc R . . H17C H 0.7180 0.8784 0.5776 0.058 Uiso 1 1 calc R . . C18 C 0.49307(19) 0.4529(5) 0.6148(2) 0.0383(10) Uani 1 1 d . . . H18A H 0.4563 0.4585 0.5773 0.057 Uiso 1 1 calc R . . H18B H 0.4825 0.5024 0.6579 0.057 Uiso 1 1 calc R . . H18C H 0.5018 0.3571 0.6272 0.057 Uiso 1 1 calc R . . C19 C 0.8053(2) 0.3366(4) 0.2697(2) 0.0305(9) Uani 1 1 d . . . C20 C 0.7944(2) 0.2508(5) 0.2007(2) 0.0471(12) Uani 1 1 d . . . H20A H 0.7855 0.1561 0.2135 0.071 Uiso 1 1 calc R . . H20B H 0.8335 0.2540 0.1749 0.071 Uiso 1 1 calc R . . H20C H 0.7573 0.2872 0.1696 0.071 Uiso 1 1 calc R . . C21 C 0.8668(2) 0.2806(5) 0.3139(2) 0.0434(12) Uani 1 1 d . . . H21A H 0.8619 0.1823 0.3212 0.065 Uiso 1 1 calc R . . H21B H 0.8727 0.3265 0.3609 0.065 Uiso 1 1 calc R . . H21C H 0.9048 0.2974 0.2876 0.065 Uiso 1 1 calc R . . C22 C 0.8172(2) 0.4841(4) 0.2464(2) 0.0397(11) Uani 1 1 d . . . H22A H 0.8559 0.4873 0.2199 0.060 Uiso 1 1 calc R . . H22B H 0.8240 0.5424 0.2894 0.060 Uiso 1 1 calc R . . H22C H 0.7794 0.5168 0.2151 0.060 Uiso 1 1 calc R . . C23 C 0.5750(2) 0.1807(6) 0.2970(3) 0.0569(14) Uani 1 1 d . . . H23A H 0.5598 0.1158 0.3317 0.085 Uiso 1 1 calc R . . H23B H 0.5832 0.1324 0.2526 0.085 Uiso 1 1 calc R . . H23C H 0.5417 0.2508 0.2856 0.085 Uiso 1 1 calc R . . C24 C 0.8420(3) 0.6249(8) 0.6103(3) 0.0647(18) Uani 1 1 d . . . H24A H 0.8089 0.6064 0.6448 0.078 Uiso 1 1 calc R . . C25 C 0.8705(5) 0.7472(7) 0.6018(4) 0.096(3) Uani 1 1 d . . . H25A H 0.8621 0.8321 0.6292 0.115 Uiso 1 1 calc R . . C26 C 0.9231(4) 0.7245(11) 0.5658(5) 0.111(4) Uani 1 1 d . . . H26A H 0.9588 0.7917 0.5609 0.133 Uiso 1 1 calc R . . C27 C 0.9263(3) 0.5916(11) 0.5516(3) 0.089(3) Uani 1 1 d . . . H27A H 0.9647 0.5440 0.5345 0.107 Uiso 1 1 calc R . . C28 C 0.8753(3) 0.5291(6) 0.5789(3) 0.0637(17) Uani 1 1 d . . . H28A H 0.8709 0.4286 0.5863 0.076 Uiso 1 1 calc R . . C29 C 0.6769(2) 0.6814(5) 0.3265(2) 0.0400(11) Uani 1 1 d . . . H29A H 0.6555 0.6580 0.3702 0.048 Uiso 1 1 calc R . . H29B H 0.6880 0.5959 0.3021 0.048 Uiso 1 1 calc R . . C30 C 0.6329(2) 0.7694(5) 0.2759(3) 0.0486(12) Uani 1 1 d . . . H30A H 0.6095 0.7140 0.2371 0.058 Uiso 1 1 calc R . . H30B H 0.6007 0.8184 0.3025 0.058 Uiso 1 1 calc R . . C31 C 0.6791(3) 0.8675(6) 0.2456(3) 0.0720(18) Uani 1 1 d . . . H31 H 0.6748 0.9089 0.1991 0.086 Uiso 1 1 calc R . . C32 C 0.7303(3) 0.8845(7) 0.3013(3) 0.0741(19) Uani 1 1 d . . . H32A H 0.7216 0.9647 0.3313 0.089 Uiso 1 1 calc R . . H32B H 0.7718 0.9001 0.2801 0.089 Uiso 1 1 calc R . . C33 C 0.7958(2) 1.0517(4) 0.4601(3) 0.0438(12) Uani 1 1 d . . . H33A H 0.7561 1.0126 0.4777 0.053 Uiso 1 1 calc R . . H33B H 0.7831 1.1053 0.4158 0.053 Uiso 1 1 calc R . . C34 C 0.8309(3) 1.1392(6) 0.5167(3) 0.0679(17) Uani 1 1 d . . . H34A H 0.8176 1.1164 0.5650 0.081 Uiso 1 1 calc R . . H34B H 0.8214 1.2367 0.5067 0.081 Uiso 1 1 calc R . . C35 C 0.9016(3) 1.1113(5) 0.5142(3) 0.0561(14) Uani 1 1 d . . . H35A H 0.9212 1.0752 0.5612 0.067 Uiso 1 1 calc R . . H35B H 0.9250 1.1956 0.5029 0.067 Uiso 1 1 calc R . . C36 C 0.9051(2) 1.0076(4) 0.4557(3) 0.0406(11) Uani 1 1 d . . . H36A H 0.9159 1.0516 0.4104 0.049 Uiso 1 1 calc R . . H36B H 0.9387 0.9381 0.4703 0.049 Uiso 1 1 calc R . . C37 C 0.9005(2) 0.8061(5) 0.3021(2) 0.0359(10) Uani 1 1 d . . . H37A H 0.8879 0.9003 0.3137 0.043 Uiso 1 1 calc R . . H37B H 0.8689 0.7705 0.2630 0.043 Uiso 1 1 calc R . . C38 C 0.9681(2) 0.8030(5) 0.2794(3) 0.0471(12) Uani 1 1 d . . . H38A H 0.9970 0.8686 0.3076 0.057 Uiso 1 1 calc R . . H38B H 0.9683 0.8227 0.2272 0.057 Uiso 1 1 calc R . . C39 C 0.9878(2) 0.6573(5) 0.2968(3) 0.0522(13) Uani 1 1 d . . . H39A H 0.9697 0.5943 0.2583 0.063 Uiso 1 1 calc R . . H39B H 1.0357 0.6475 0.3033 0.063 Uiso 1 1 calc R . . C40 C 0.9584(2) 0.6310(5) 0.3668(3) 0.0411(11) Uani 1 1 d . . . H40A H 0.9453 0.5342 0.3699 0.049 Uiso 1 1 calc R . . H40B H 0.9902 0.6523 0.4087 0.049 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 La1 0.02168(13) 0.02579(13) 0.02139(13) 0.00264(10) 0.00223(9) 0.00265(10) O1 0.0232(14) 0.0308(15) 0.0280(14) 0.0027(12) 0.0071(11) 0.0024(12) O2 0.0333(15) 0.0296(15) 0.0299(15) -0.0044(12) 0.0071(12) -0.0022(13) O3 0.0340(16) 0.0450(18) 0.0372(17) 0.0093(14) -0.0046(13) 0.0027(14) O4 0.0457(18) 0.0251(15) 0.0386(17) 0.0018(13) -0.0069(14) 0.0003(14) O5 0.0304(15) 0.0415(17) 0.0311(16) 0.0102(13) 0.0109(12) 0.0064(13) C1 0.0214(19) 0.031(2) 0.0215(19) 0.0005(16) 0.0015(15) 0.0031(17) C2 0.023(2) 0.033(2) 0.021(2) 0.0002(17) -0.0008(16) 0.0054(17) C3 0.0112(18) 0.038(3) 0.045(3) 0.007(2) 0.0080(17) 0.0036(17) C4 0.024(2) 0.044(3) 0.022(2) 0.0001(18) 0.0046(16) -0.0019(19) C5 0.034(2) 0.030(2) 0.022(2) 0.0017(17) 0.0026(17) -0.0007(18) C6 0.028(2) 0.031(2) 0.0198(19) -0.0013(16) 0.0037(16) 0.0012(17) C7 0.030(2) 0.021(2) 0.028(2) -0.0007(16) 0.0019(17) 0.0061(17) C8 0.035(2) 0.021(2) 0.025(2) 0.0032(16) 0.0071(17) 0.0033(17) C9 0.040(2) 0.035(2) 0.027(2) -0.0081(18) 0.0064(19) 0.001(2) C10 0.037(2) 0.039(3) 0.042(3) -0.012(2) 0.007(2) -0.004(2) C11 0.031(2) 0.033(2) 0.037(2) -0.0034(19) 0.0125(19) 0.0000(19) C12 0.030(2) 0.024(2) 0.027(2) -0.0009(16) 0.0045(17) 0.0049(17) C13 0.029(2) 0.029(2) 0.030(2) 0.0022(18) 0.0069(17) 0.0057(18) C14 0.029(2) 0.031(2) 0.032(2) 0.0015(18) 0.0050(18) 0.0041(18) C15 0.038(2) 0.038(3) 0.048(3) -0.001(2) 0.014(2) 0.010(2) C16 0.038(2) 0.037(3) 0.045(3) 0.011(2) 0.010(2) 0.011(2) C17 0.039(3) 0.034(3) 0.044(3) -0.004(2) 0.008(2) -0.005(2) C18 0.028(2) 0.046(3) 0.041(3) 0.002(2) 0.0080(19) -0.002(2) C19 0.035(2) 0.035(2) 0.023(2) -0.0008(18) 0.0087(17) 0.0035(19) C20 0.062(3) 0.045(3) 0.038(3) -0.005(2) 0.022(2) 0.000(2) C21 0.042(3) 0.051(3) 0.039(3) 0.010(2) 0.016(2) 0.014(2) C22 0.046(3) 0.040(3) 0.034(2) 0.008(2) 0.009(2) -0.005(2) C23 0.039(3) 0.075(4) 0.057(3) -0.029(3) 0.009(2) -0.011(3) C24 0.044(3) 0.128(6) 0.021(2) 0.014(3) 0.001(2) 0.012(4) C25 0.165(8) 0.047(4) 0.058(4) -0.022(3) -0.070(5) 0.028(5) C26 0.076(5) 0.142(8) 0.101(6) 0.094(6) -0.064(5) -0.065(6) C27 0.053(4) 0.171(8) 0.044(3) 0.036(5) 0.005(3) 0.066(5) C28 0.093(5) 0.040(3) 0.049(3) 0.016(3) -0.034(3) -0.001(3) C29 0.043(3) 0.040(3) 0.036(2) 0.000(2) -0.003(2) -0.003(2) C30 0.041(3) 0.055(3) 0.045(3) 0.003(2) -0.015(2) 0.004(2) C31 0.070(4) 0.072(4) 0.067(4) 0.034(3) -0.029(3) -0.023(3) C32 0.053(3) 0.094(5) 0.071(4) 0.054(4) -0.016(3) -0.017(3) C33 0.039(3) 0.029(2) 0.065(3) 0.005(2) 0.015(2) 0.007(2) C34 0.067(4) 0.072(4) 0.063(4) -0.032(3) -0.003(3) 0.023(3) C35 0.057(3) 0.045(3) 0.063(3) -0.011(3) -0.005(3) 0.000(3) C36 0.034(2) 0.033(2) 0.056(3) 0.001(2) 0.005(2) -0.001(2) C37 0.042(3) 0.038(3) 0.028(2) 0.0079(19) 0.0058(19) 0.003(2) C38 0.046(3) 0.058(3) 0.039(3) 0.009(2) 0.013(2) -0.009(2) C39 0.044(3) 0.063(4) 0.054(3) 0.005(3) 0.021(2) 0.007(3) C40 0.032(2) 0.043(3) 0.050(3) 0.010(2) 0.011(2) 0.010(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 La1 O1 2.232(2) . ? La1 O2 2.281(3) . ? La1 O3 2.649(3) . ? La1 O4 2.675(3) . ? La1 O5 2.701(3) . ? La1 C24 2.854(5) . ? La1 C25 2.861(5) . ? La1 C28 2.868(5) . ? La1 C26 2.897(6) . ? La1 C27 2.901(5) . ? O1 C1 1.355(4) . ? O2 C7 1.346(5) . ? O3 C32 1.446(6) . ? O3 C29 1.459(5) . ? O4 C33 1.436(5) . ? O4 C36 1.463(5) . ? O5 C40 1.449(5) . ? O5 C37 1.454(5) . ? C1 C6 1.407(5) . ? C1 C2 1.417(5) . ? C2 C3 1.403(5) . ? C2 C14 1.531(6) . ? C3 C4 1.389(6) . ? C3 H3 0.9500 . ? C4 C5 1.387(5) . ? C4 C18 1.518(5) . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 C13 1.514(5) . ? C7 C12 1.414(5) . ? C7 C8 1.427(5) . ? C8 C9 1.394(6) . ? C8 C19 1.536(5) . ? C9 C10 1.393(6) . ? C9 H9 0.9500 . ? C10 C11 1.381(6) . ? C10 C23 1.510(6) . ? C11 C12 1.384(6) . ? C11 H11 0.9500 . ? C12 C13 1.529(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C16 1.531(6) . ? C14 C17 1.539(6) . ? C14 C15 1.545(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.531(6) . ? C19 C22 1.537(6) . ? C19 C21 1.544(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C28 1.332(8) . ? C24 C25 1.352(9) . ? C24 H24A 1.0000 . ? C25 C26 1.350(11) . ? C25 H25A 1.0000 . ? C26 C27 1.332(11) . ? C26 H26A 1.0000 . ? C27 C28 1.361(9) . ? C27 H27A 1.0000 . ? C28 H28A 1.0000 . ? C29 C30 1.511(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.503(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.415(7) . ? C31 H31 0.9500 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.489(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.490(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.496(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.499(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.512(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.510(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O2 94.92(9) . . ? O1 La1 O3 77.32(9) . . ? O2 La1 O3 86.11(10) . . ? O1 La1 O4 103.69(9) . . ? O2 La1 O4 149.79(9) . . ? O3 La1 O4 75.27(9) . . ? O1 La1 O5 157.79(9) . . ? O2 La1 O5 85.58(9) . . ? O3 La1 O5 80.57(9) . . ? O4 La1 O5 68.26(9) . . ? O1 La1 C24 77.15(12) . . ? O2 La1 C24 102.28(18) . . ? O3 La1 C24 153.69(13) . . ? O4 La1 C24 104.90(17) . . ? O5 La1 C24 124.51(12) . . ? O1 La1 C25 89.5(2) . . ? O2 La1 C25 126.06(15) . . ? O3 La1 C25 146.49(14) . . ? O4 La1 C25 78.29(17) . . ? O5 La1 C25 108.2(2) . . ? C24 La1 C25 27.37(19) . . ? O1 La1 C28 95.50(16) . . ? O2 La1 C28 81.27(13) . . ? O3 La1 C28 164.91(13) . . ? O4 La1 C28 119.60(13) . . ? O5 La1 C28 106.49(16) . . ? C24 La1 C28 26.92(16) . . ? C25 La1 C28 44.83(17) . . ? O1 La1 C26 116.4(2) . . ? O2 La1 C26 116.5(3) . . ? O3 La1 C26 150.58(16) . . ? O4 La1 C26 76.13(19) . . ? O5 La1 C26 82.6(2) . . ? C24 La1 C26 44.40(18) . . ? C25 La1 C26 27.1(2) . . ? C28 La1 C26 44.47(18) . . ? O1 La1 C27 120.66(15) . . ? O2 La1 C27 90.0(2) . . ? O3 La1 C27 161.91(14) . . ? O4 La1 C27 100.3(2) . . ? O5 La1 C27 81.52(15) . . ? C24 La1 C27 44.28(16) . . ? C25 La1 C27 44.4(2) . . ? C28 La1 C27 27.29(18) . . ? C26 La1 C27 26.6(2) . . ? C1 O1 La1 157.0(2) . . ? C7 O2 La1 135.7(2) . . ? C32 O3 C29 107.8(3) . . ? C32 O3 La1 135.0(3) . . ? C29 O3 La1 116.4(2) . . ? C33 O4 C36 105.6(3) . . ? C33 O4 La1 122.3(2) . . ? C36 O4 La1 126.6(2) . . ? C40 O5 C37 108.3(3) . . ? C40 O5 La1 120.7(2) . . ? C37 O5 La1 130.3(2) . . ? O1 C1 C6 118.7(3) . . ? O1 C1 C2 121.5(3) . . ? C6 C1 C2 119.8(4) . . ? C3 C2 C1 117.6(4) . . ? C3 C2 C14 120.6(3) . . ? C1 C2 C14 121.8(3) . . ? C4 C3 C2 123.1(4) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C5 C4 C3 117.9(4) . . ? C5 C4 C18 120.7(4) . . ? C3 C4 C18 121.4(4) . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 C13 119.1(4) . . ? C1 C6 C13 121.0(3) . . ? O2 C7 C12 120.0(3) . . ? O2 C7 C8 121.3(3) . . ? C12 C7 C8 118.6(4) . . ? C9 C8 C7 117.9(3) . . ? C9 C8 C19 120.6(3) . . ? C7 C8 C19 121.4(3) . . ? C10 C9 C8 123.4(4) . . ? C10 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C11 C10 C9 117.1(4) . . ? C11 C10 C23 121.9(4) . . ? C9 C10 C23 121.0(4) . . ? C10 C11 C12 122.6(4) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C7 119.7(4) . . ? C11 C12 C13 119.0(3) . . ? C7 C12 C13 121.2(3) . . ? C6 C13 C12 116.1(3) . . ? C6 C13 H13A 108.3 . . ? C12 C13 H13A 108.3 . . ? C6 C13 H13B 108.3 . . ? C12 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C2 C14 C16 109.3(3) . . ? C2 C14 C17 110.4(3) . . ? C16 C14 C17 110.3(3) . . ? C2 C14 C15 113.1(3) . . ? C16 C14 C15 107.5(3) . . ? C17 C14 C15 106.1(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C8 112.4(3) . . ? C20 C19 C22 107.3(3) . . ? C8 C19 C22 110.6(3) . . ? C20 C19 C21 107.1(4) . . ? C8 C19 C21 109.7(3) . . ? C22 C19 C21 109.7(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C28 C24 C25 109.0(6) . . ? C28 C24 La1 77.1(3) . . ? C25 C24 La1 76.6(3) . . ? C28 C24 H24A 124.7 . . ? C25 C24 H24A 124.7 . . ? La1 C24 H24A 124.7 . . ? C26 C25 C24 107.0(6) . . ? C26 C25 La1 77.9(4) . . ? C24 C25 La1 76.0(3) . . ? C26 C25 H25A 125.4 . . ? C24 C25 H25A 125.4 . . ? La1 C25 H25A 125.4 . . ? C27 C26 C25 108.5(6) . . ? C27 C26 La1 76.9(4) . . ? C25 C26 La1 75.0(4) . . ? C27 C26 H26A 125.1 . . ? C25 C26 H26A 125.1 . . ? La1 C26 H26A 125.1 . . ? C26 C27 C28 108.2(6) . . ? C26 C27 La1 76.5(3) . . ? C28 C27 La1 75.0(3) . . ? C26 C27 H27A 125.2 . . ? C28 C27 H27A 125.2 . . ? La1 C27 H27A 125.2 . . ? C24 C28 C27 107.3(6) . . ? C24 C28 La1 75.9(3) . . ? C27 C28 La1 77.7(3) . . ? C24 C28 H28A 125.3 . . ? C27 C28 H28A 125.3 . . ? La1 C28 H28A 125.3 . . ? O3 C29 C30 105.6(4) . . ? O3 C29 H29A 110.6 . . ? C30 C29 H29A 110.6 . . ? O3 C29 H29B 110.6 . . ? C30 C29 H29B 110.6 . . ? H29A C29 H29B 108.8 . . ? C31 C30 C29 103.5(4) . . ? C31 C30 H30A 111.1 . . ? C29 C30 H30A 111.1 . . ? C31 C30 H30B 111.1 . . ? C29 C30 H30B 111.1 . . ? H30A C30 H30B 109.0 . . ? C32 C31 C30 104.9(4) . . ? C32 C31 H31 127.6 . . ? C30 C31 H31 127.6 . . ? C31 C32 O3 108.9(5) . . ? C31 C32 H32A 109.9 . . ? O3 C32 H32A 109.9 . . ? C31 C32 H32B 109.9 . . ? O3 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? O4 C33 C34 106.0(4) . . ? O4 C33 H33A 110.5 . . ? C34 C33 H33A 110.5 . . ? O4 C33 H33B 110.5 . . ? C34 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? C33 C34 C35 106.3(4) . . ? C33 C34 H34A 110.5 . . ? C35 C34 H34A 110.5 . . ? C33 C34 H34B 110.5 . . ? C35 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C34 C35 C36 105.5(4) . . ? C34 C35 H35A 110.6 . . ? C36 C35 H35A 110.6 . . ? C34 C35 H35B 110.6 . . ? C36 C35 H35B 110.6 . . ? H35A C35 H35B 108.8 . . ? O4 C36 C35 105.5(4) . . ? O4 C36 H36A 110.6 . . ? C35 C36 H36A 110.6 . . ? O4 C36 H36B 110.6 . . ? C35 C36 H36B 110.6 . . ? H36A C36 H36B 108.8 . . ? O5 C37 C38 105.7(3) . . ? O5 C37 H37A 110.6 . . ? C38 C37 H37A 110.6 . . ? O5 C37 H37B 110.6 . . ? C38 C37 H37B 110.6 . . ? H37A C37 H37B 108.7 . . ? C37 C38 C39 101.3(4) . . ? C37 C38 H38A 111.5 . . ? C39 C38 H38A 111.5 . . ? C37 C38 H38B 111.5 . . ? C39 C38 H38B 111.5 . . ? H38A C38 H38B 109.3 . . ? C40 C39 C38 102.9(4) . . ? C40 C39 H39A 111.2 . . ? C38 C39 H39A 111.2 . . ? C40 C39 H39B 111.2 . . ? C38 C39 H39B 111.2 . . ? H39A C39 H39B 109.1 . . ? O5 C40 C39 106.1(3) . . ? O5 C40 H40A 110.5 . . ? C39 C40 H40A 110.5 . . ? O5 C40 H40B 110.5 . . ? C39 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.673 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.087 #===================================================end data_complex2 _database_code_depnum_ccdc_archive 'CCDC 682655' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H51 O4 Yb, C4 H8 O' _chemical_formula_sum 'C40 H59 O5 Yb' _chemical_formula_weight 792.91 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' Yb Yb -0.3850 5.5486 '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' _symmetry_Int_Tables_number 14 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 8.6570(5) _cell_length_b 25.0986(15) _cell_length_c 34.913(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.892(2) _cell_angle_gamma 90.00 _cell_volume 7584.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24547 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 2.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.250 _exptl_absorpt_correction_T_max 0.548 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67398 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 13851 _reflns_number_gt 12269 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0178P)^2^+17.6294P] 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 13851 _refine_ls_number_parameters 846 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.202 _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 Yb1 Yb 0.40740(2) 0.614673(8) 0.702086(6) 0.02421(6) Uani 1 1 d . . . Yb2 Yb 0.74589(2) 0.681793(8) 0.973687(6) 0.02469(6) Uani 1 1 d . . . O1 O 0.4628(4) 0.59052(13) 0.64737(9) 0.0307(8) Uani 1 1 d . . . O2 O 0.4390(4) 0.69301(12) 0.68503(9) 0.0276(8) Uani 1 1 d . . . O3 O 0.5523(4) 0.64223(14) 0.75542(10) 0.0351(9) Uani 1 1 d . . . O4 O 0.5642(4) 0.53941(13) 0.71911(11) 0.0353(9) Uani 1 1 d . . . O5 O 0.8689(13) 0.4580(4) 0.5706(3) 0.181(4) Uani 1 1 d D . . O6 O 0.6611(4) 0.72230(13) 0.92668(10) 0.0303(8) Uani 1 1 d . . . O7 O 0.7444(4) 0.61109(13) 0.94245(9) 0.0275(8) Uani 1 1 d . . . O8 O 0.5705(4) 0.73860(13) 1.00503(9) 0.0284(8) Uani 1 1 d . . . O9 O 0.6205(4) 0.62603(13) 1.01894(10) 0.0335(8) Uani 1 1 d . . . O10 O 0.1132(9) 0.3184(3) 0.7436(3) 0.144(3) Uani 1 1 d . . . C1 C 0.5517(6) 0.59586(19) 0.61675(14) 0.0267(11) Uani 1 1 d . . . C2 C 0.5096(6) 0.57182(19) 0.58125(15) 0.0287(11) Uani 1 1 d . . . C3 C 0.6121(6) 0.5766(2) 0.55117(15) 0.0334(12) Uani 1 1 d . . . H3 H 0.5844 0.5606 0.5274 0.040 Uiso 1 1 calc R . . C4 C 0.7538(6) 0.6034(2) 0.55385(15) 0.0310(12) Uani 1 1 d . . . C5 C 0.7880(6) 0.62781(19) 0.58844(15) 0.0306(12) Uani 1 1 d . . . H5 H 0.8826 0.6467 0.5911 0.037 Uiso 1 1 calc R . . C6 C 0.6900(6) 0.62574(18) 0.61931(14) 0.0255(11) Uani 1 1 d . . . C7 C 0.5225(5) 0.72924(18) 0.66623(14) 0.0246(11) Uani 1 1 d . . . C8 C 0.4675(5) 0.78205(18) 0.66099(14) 0.0243(11) Uani 1 1 d . . . C9 C 0.5651(6) 0.81839(19) 0.64377(14) 0.0275(11) Uani 1 1 d . . . H9 H 0.5288 0.8538 0.6402 0.033 Uiso 1 1 calc R . . C10 C 0.7123(6) 0.8062(2) 0.63152(14) 0.0296(12) Uani 1 1 d . . . C11 C 0.7605(6) 0.7539(2) 0.63570(14) 0.0292(11) Uani 1 1 d . . . H11 H 0.8596 0.7440 0.6267 0.035 Uiso 1 1 calc R . . C12 C 0.6691(5) 0.71526(18) 0.65255(13) 0.0235(10) Uani 1 1 d . . . C13 C 0.7301(5) 0.65866(18) 0.65471(14) 0.0259(11) Uani 1 1 d . . . H13A H 0.6869 0.6410 0.6775 0.031 Uiso 1 1 calc R . . H13B H 0.8439 0.6597 0.6580 0.031 Uiso 1 1 calc R . . C14 C 0.3534(6) 0.5436(2) 0.57631(16) 0.0371(13) Uani 1 1 d . . . C15 C 0.3303(8) 0.5216(3) 0.53586(18) 0.0603(19) Uani 1 1 d . . . H15A H 0.4117 0.4956 0.5305 0.091 Uiso 1 1 calc R . . H15B H 0.3352 0.5508 0.5173 0.091 Uiso 1 1 calc R . . H15C H 0.2292 0.5042 0.5338 0.091 Uiso 1 1 calc R . . C16 C 0.2229(6) 0.5831(2) 0.58388(17) 0.0423(14) Uani 1 1 d . . . H16A H 0.2269 0.6122 0.5652 0.063 Uiso 1 1 calc R . . H16B H 0.2348 0.5977 0.6098 0.063 Uiso 1 1 calc R . . H16C H 0.1232 0.5648 0.5815 0.063 Uiso 1 1 calc R . . C17 C 0.3443(7) 0.4964(2) 0.60390(18) 0.0486(16) Uani 1 1 d . . . H17A H 0.2456 0.4779 0.6000 0.073 Uiso 1 1 calc R . . H17B H 0.3521 0.5093 0.6304 0.073 Uiso 1 1 calc R . . H17C H 0.4294 0.4717 0.5990 0.073 Uiso 1 1 calc R . . C18 C 0.8609(7) 0.6055(2) 0.52024(16) 0.0458(15) Uani 1 1 d . . . H18A H 0.9464 0.6300 0.5260 0.069 Uiso 1 1 calc R . . H18B H 0.8039 0.6181 0.4975 0.069 Uiso 1 1 calc R . . H18C H 0.9021 0.5699 0.5154 0.069 Uiso 1 1 calc R . . C19 C 0.3060(6) 0.7981(2) 0.67448(16) 0.0342(13) Uani 1 1 d . . . C20 C 0.2670(7) 0.8564(2) 0.6653(2) 0.0531(17) Uani 1 1 d . . . H20A H 0.3387 0.8799 0.6792 0.080 Uiso 1 1 calc R . . H20B H 0.1610 0.8641 0.6730 0.080 Uiso 1 1 calc R . . H20C H 0.2764 0.8625 0.6377 0.080 Uiso 1 1 calc R . . C21 C 0.2966(7) 0.7913(2) 0.71822(17) 0.0436(15) Uani 1 1 d . . . H21A H 0.3211 0.7544 0.7251 0.065 Uiso 1 1 calc R . . H21B H 0.1920 0.8000 0.7266 0.065 Uiso 1 1 calc R . . H21C H 0.3709 0.8153 0.7308 0.065 Uiso 1 1 calc R . . C22 C 0.1830(6) 0.7631(2) 0.65387(17) 0.0426(14) Uani 1 1 d . . . H22A H 0.1823 0.7710 0.6264 0.064 Uiso 1 1 calc R . . H22B H 0.0810 0.7707 0.6643 0.064 Uiso 1 1 calc R . . H22C H 0.2080 0.7254 0.6578 0.064 Uiso 1 1 calc R . . C23 C 0.8153(6) 0.8484(2) 0.61482(17) 0.0415(14) Uani 1 1 d . . . H23A H 0.7849 0.8549 0.5881 0.062 Uiso 1 1 calc R . . H23B H 0.9229 0.8363 0.6160 0.062 Uiso 1 1 calc R . . H23C H 0.8051 0.8815 0.6295 0.062 Uiso 1 1 calc R . . C24 C 0.1113(6) 0.6032(3) 0.69064(18) 0.0441(15) Uani 1 1 d . . . H24A H 0.0559 0.6092 0.6657 0.053 Uiso 1 1 calc R . . C25 C 0.1231(6) 0.6401(2) 0.72021(19) 0.0465(16) Uani 1 1 d . . . H25A H 0.0789 0.6769 0.7197 0.056 Uiso 1 1 calc R . . C26 C 0.1782(7) 0.6136(3) 0.75286(18) 0.0470(15) Uani 1 1 d . . . H26A H 0.1831 0.6285 0.7794 0.056 Uiso 1 1 calc R . . C27 C 0.2018(6) 0.5606(2) 0.74266(18) 0.0430(15) Uani 1 1 d . . . H27A H 0.2272 0.5311 0.7610 0.052 Uiso 1 1 calc R . . C28 C 0.1599(6) 0.5537(2) 0.70446(18) 0.0421(14) Uani 1 1 d . . . H28A H 0.1462 0.5188 0.6911 0.051 Uiso 1 1 calc R . . C29 C 0.6418(8) 0.6913(2) 0.75899(18) 0.0524(17) Uani 1 1 d . . . H29A H 0.7002 0.6979 0.7353 0.063 Uiso 1 1 calc R . . H29B H 0.5727 0.7220 0.7635 0.063 Uiso 1 1 calc R . . C30 C 0.7474(9) 0.6838(3) 0.7915(2) 0.075(2) Uani 1 1 d D . . H30A H 0.8546 0.6800 0.7824 0.090 Uiso 1 1 calc R . . H30B H 0.7431 0.7150 0.8087 0.090 Uiso 1 1 calc R . . C31 C 0.7017(8) 0.6360(3) 0.8119(2) 0.067(2) Uani 1 1 d D . . H31A H 0.6824 0.6444 0.8391 0.080 Uiso 1 1 calc R . . H31B H 0.7844 0.6088 0.8108 0.080 Uiso 1 1 calc R . . C32 C 0.5582(7) 0.6159(2) 0.79290(16) 0.0484(16) Uani 1 1 d . . . H32A H 0.5623 0.5767 0.7899 0.058 Uiso 1 1 calc R . . H32B H 0.4664 0.6253 0.8081 0.058 Uiso 1 1 calc R . . C33 C 0.7309(6) 0.5407(2) 0.7170(2) 0.0557(18) Uani 1 1 d . . . H33A H 0.7737 0.5704 0.7326 0.067 Uiso 1 1 calc R . . H33B H 0.7641 0.5451 0.6902 0.067 Uiso 1 1 calc R . . C34 C 0.7823(7) 0.4882(3) 0.7327(3) 0.078(3) Uani 1 1 d . . . H34A H 0.8793 0.4766 0.7205 0.093 Uiso 1 1 calc R . . H34B H 0.7997 0.4904 0.7607 0.093 Uiso 1 1 calc R . . C35 C 0.6549(8) 0.4507(3) 0.7234(2) 0.0595(19) Uani 1 1 d . . . H35A H 0.6263 0.4298 0.7463 0.071 Uiso 1 1 calc R . . H35B H 0.6855 0.4257 0.7029 0.071 Uiso 1 1 calc R . . C36 C 0.5225(7) 0.4851(2) 0.7102(2) 0.0552(18) Uani 1 1 d . . . H36A H 0.5047 0.4809 0.6823 0.066 Uiso 1 1 calc R . . H36B H 0.4268 0.4750 0.7236 0.066 Uiso 1 1 calc R . . C37 C 0.8501(13) 0.4768(4) 0.6108(3) 0.115(4) Uani 1 1 d D . . H37A H 0.9471 0.4931 0.6206 0.138 Uiso 1 1 calc R . . H37B H 0.7664 0.5036 0.6122 0.138 Uiso 1 1 calc R . . C38 C 0.8127(17) 0.4315(5) 0.6327(3) 0.142(5) Uani 1 1 d D . . H38A H 0.7148 0.4376 0.6463 0.171 Uiso 1 1 calc R . . H38B H 0.8952 0.4247 0.6521 0.171 Uiso 1 1 calc R . . C39 C 0.7971(15) 0.3867(5) 0.6080(5) 0.186(9) Uani 1 1 d D . . H39A H 0.8677 0.3579 0.6167 0.223 Uiso 1 1 calc R . . H39B H 0.6899 0.3730 0.6088 0.223 Uiso 1 1 calc R . . C40 C 0.8325(16) 0.4019(4) 0.5710(4) 0.154(6) Uani 1 1 d D . . H40A H 0.7434 0.3947 0.5536 0.185 Uiso 1 1 calc R . . H40B H 0.9219 0.3811 0.5618 0.185 Uiso 1 1 calc R . . C41 C 0.5504(6) 0.72852(19) 0.89950(14) 0.0271(11) Uani 1 1 d . . . C42 C 0.5478(6) 0.7743(2) 0.87566(14) 0.0322(12) Uani 1 1 d . . . C43 C 0.4289(7) 0.7784(2) 0.84871(15) 0.0379(14) Uani 1 1 d . . . H43 H 0.4273 0.8084 0.8321 0.046 Uiso 1 1 calc R . . C44 C 0.3122(6) 0.7408(2) 0.84478(15) 0.0345(13) Uani 1 1 d . . . C45 C 0.3158(6) 0.6972(2) 0.86851(15) 0.0319(12) Uani 1 1 d . . . H45 H 0.2360 0.6714 0.8664 0.038 Uiso 1 1 calc R . . C46 C 0.4342(6) 0.68993(19) 0.89563(14) 0.0259(11) Uani 1 1 d . . . C47 C 0.6737(5) 0.58131(18) 0.91528(13) 0.0228(10) Uani 1 1 d . . . C48 C 0.7503(5) 0.53866(18) 0.89735(14) 0.0249(11) Uani 1 1 d . . . C49 C 0.6693(5) 0.50828(18) 0.87042(14) 0.0262(11) Uani 1 1 d . . . H49 H 0.7205 0.4793 0.8586 0.031 Uiso 1 1 calc R . . C50 C 0.5169(6) 0.51862(19) 0.86020(14) 0.0274(11) Uani 1 1 d . . . C51 C 0.4459(5) 0.56176(18) 0.87695(13) 0.0240(11) Uani 1 1 d . . . H51 H 0.3427 0.5702 0.8695 0.029 Uiso 1 1 calc R . . C52 C 0.5195(5) 0.59350(18) 0.90442(14) 0.0238(10) Uani 1 1 d . . . C53 C 0.4335(5) 0.64052(18) 0.92068(14) 0.0238(10) Uani 1 1 d . . . H53A H 0.4799 0.6496 0.9459 0.029 Uiso 1 1 calc R . . H53B H 0.3250 0.6299 0.9249 0.029 Uiso 1 1 calc R . . C54 C 0.6745(7) 0.8174(2) 0.87963(16) 0.0420(14) Uani 1 1 d . . . C55 C 0.6489(9) 0.8630(2) 0.85104(18) 0.0600(19) Uani 1 1 d . . . H55A H 0.7334 0.8888 0.8536 0.090 Uiso 1 1 calc R . . H55B H 0.5505 0.8807 0.8563 0.090 Uiso 1 1 calc R . . H55C H 0.6464 0.8487 0.8249 0.090 Uiso 1 1 calc R . . C56 C 0.8328(7) 0.7930(2) 0.87210(19) 0.0530(17) Uani 1 1 d . . . H56A H 0.8504 0.7629 0.8895 0.080 Uiso 1 1 calc R . . H56B H 0.9130 0.8200 0.8765 0.080 Uiso 1 1 calc R . . H56C H 0.8366 0.7806 0.8455 0.080 Uiso 1 1 calc R . . C57 C 0.6729(8) 0.8425(2) 0.91999(16) 0.0473(16) Uani 1 1 d . . . H57A H 0.6964 0.8152 0.9392 0.071 Uiso 1 1 calc R . . H57B H 0.5705 0.8576 0.9247 0.071 Uiso 1 1 calc R . . H57C H 0.7507 0.8708 0.9216 0.071 Uiso 1 1 calc R . . C58 C 0.1827(7) 0.7482(3) 0.81543(17) 0.0495(16) Uani 1 1 d . . . H58A H 0.2147 0.7337 0.7907 0.074 Uiso 1 1 calc R . . H58B H 0.1595 0.7862 0.8126 0.074 Uiso 1 1 calc R . . H58C H 0.0903 0.7293 0.8240 0.074 Uiso 1 1 calc R . . C59 C 0.4320(6) 0.4840(2) 0.83140(16) 0.0377(13) Uani 1 1 d . . . H59A H 0.4942 0.4804 0.8083 0.057 Uiso 1 1 calc R . . H59B H 0.3326 0.5005 0.8247 0.057 Uiso 1 1 calc R . . H59C H 0.4142 0.4488 0.8425 0.057 Uiso 1 1 calc R . . C60 C 0.9237(6) 0.5288(2) 0.90545(16) 0.0337(13) Uani 1 1 d . . . C61 C 0.9870(6) 0.4813(2) 0.8825(2) 0.0552(18) Uani 1 1 d . . . H61A H 0.9745 0.4884 0.8550 0.083 Uiso 1 1 calc R . . H61B H 0.9298 0.4489 0.8891 0.083 Uiso 1 1 calc R . . H61C H 1.0967 0.4763 0.8887 0.083 Uiso 1 1 calc R . . C62 C 0.9552(6) 0.5172(2) 0.94812(17) 0.0442(15) Uani 1 1 d . . . H62A H 1.0670 0.5154 0.9529 0.066 Uiso 1 1 calc R . . H62B H 0.9081 0.4830 0.9549 0.066 Uiso 1 1 calc R . . H62C H 0.9107 0.5456 0.9637 0.066 Uiso 1 1 calc R . . C63 C 1.0132(6) 0.5782(2) 0.89292(18) 0.0421(14) Uani 1 1 d . . . H63A H 1.0049 0.5821 0.8650 0.063 Uiso 1 1 calc R . . H63B H 1.1222 0.5744 0.9005 0.063 Uiso 1 1 calc R . . H63C H 0.9700 0.6099 0.9052 0.063 Uiso 1 1 calc R . . C64 C 1.0313(6) 0.7089(3) 0.96074(18) 0.0477(16) Uani 1 1 d . . . H64A H 1.0760 0.7153 0.9349 0.057 Uiso 1 1 calc R . . C65 C 1.0460(6) 0.6626(2) 0.98164(19) 0.0441(15) Uani 1 1 d . . . H65A H 1.0995 0.6296 0.9728 0.053 Uiso 1 1 calc R . . C66 C 0.9998(6) 0.6721(3) 1.01860(18) 0.0460(15) Uani 1 1 d . . . H66A H 1.0121 0.6470 1.0407 0.055 Uiso 1 1 calc R . . C67 C 0.9545(6) 0.7255(3) 1.02112(19) 0.0513(17) Uani 1 1 d . . . H67A H 0.9316 0.7452 1.0453 0.062 Uiso 1 1 calc R . . C68 C 0.9743(7) 0.7484(2) 0.9850(2) 0.0542(18) Uani 1 1 d . . . H68A H 0.9716 0.7874 0.9793 0.065 Uiso 1 1 calc R . . C69 C 0.5869(6) 0.7594(2) 1.04402(15) 0.0389(14) Uani 1 1 d . . . H69A H 0.6648 0.7883 1.0451 0.047 Uiso 1 1 calc R . . H69B H 0.6190 0.7308 1.0620 0.047 Uiso 1 1 calc R . . C70 C 0.4293(7) 0.7804(2) 1.05395(17) 0.0463(15) Uani 1 1 d . . . H70A H 0.4363 0.8091 1.0734 0.056 Uiso 1 1 calc R . . H70B H 0.3615 0.7517 1.0634 0.056 Uiso 1 1 calc R . . C71 C 0.3721(7) 0.8017(2) 1.01556(17) 0.0447(15) Uani 1 1 d . . . H71A H 0.2581 0.8048 1.0148 0.054 Uiso 1 1 calc R . . H71B H 0.4181 0.8370 1.0100 0.054 Uiso 1 1 calc R . . C72 C 0.4272(6) 0.7601(2) 0.98806(15) 0.0345(13) Uani 1 1 d . . . H72A H 0.3490 0.7316 0.9849 0.041 Uiso 1 1 calc R . . H72B H 0.4472 0.7760 0.9627 0.041 Uiso 1 1 calc R . . C73 C 0.6737(8) 0.5711(2) 1.02374(19) 0.0497(16) Uani 1 1 d . . . H73A H 0.7803 0.5703 1.0344 0.060 Uiso 1 1 calc R . . H73B H 0.6723 0.5521 0.9989 0.060 Uiso 1 1 calc R . . C74 C 0.5645(9) 0.5459(3) 1.0507(2) 0.070(2) Uani 1 1 d . . . H74A H 0.6006 0.5502 1.0775 0.084 Uiso 1 1 calc R . . H74B H 0.5520 0.5075 1.0451 0.084 Uiso 1 1 calc R . . C75 C 0.4169(8) 0.5752(3) 1.0437(2) 0.073(2) Uani 1 1 d . . . H75A H 0.3506 0.5740 1.0665 0.087 Uiso 1 1 calc R . . H75B H 0.3592 0.5601 1.0215 0.087 Uiso 1 1 calc R . . C76 C 0.4681(6) 0.6309(2) 1.03557(18) 0.0444(15) Uani 1 1 d . . . H76A H 0.3956 0.6485 1.0174 0.053 Uiso 1 1 calc R . . H76B H 0.4734 0.6521 1.0595 0.053 Uiso 1 1 calc R . . C77 C 0.0461(9) 0.3695(3) 0.7343(3) 0.095(3) Uani 1 1 d D . . H77A H -0.0559 0.3733 0.7464 0.114 Uiso 1 1 calc R . . H77B H 0.0319 0.3731 0.7062 0.114 Uiso 1 1 calc R . . C78 C 0.1510(10) 0.4100(3) 0.7486(4) 0.124(5) Uani 1 1 d D . . H78A H 0.1831 0.4336 0.7275 0.149 Uiso 1 1 calc R . . H78B H 0.0998 0.4319 0.7682 0.149 Uiso 1 1 calc R . . C79 C 0.2828(11) 0.3834(4) 0.7650(3) 0.116(4) Uani 1 1 d D . . H79A H 0.3019 0.3955 0.7916 0.140 Uiso 1 1 calc R . . H79B H 0.3761 0.3906 0.7498 0.140 Uiso 1 1 calc R . . C80 C 0.2451(19) 0.3277(4) 0.7641(4) 0.184(8) Uani 1 1 d D . . H80A H 0.3313 0.3077 0.7526 0.220 Uiso 1 1 calc R . . H80B H 0.2322 0.3147 0.7907 0.220 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 Yb1 0.02320(11) 0.02205(12) 0.02735(12) 0.00318(9) -0.00012(9) -0.00084(8) Yb2 0.02232(11) 0.02470(12) 0.02695(12) -0.00264(9) -0.00282(9) -0.00066(9) O1 0.034(2) 0.0303(19) 0.0273(19) -0.0030(15) 0.0015(16) -0.0050(15) O2 0.0283(18) 0.0228(18) 0.0317(19) 0.0055(15) 0.0047(16) 0.0008(14) O3 0.046(2) 0.031(2) 0.028(2) 0.0086(16) -0.0058(17) -0.0122(16) O4 0.033(2) 0.028(2) 0.044(2) 0.0063(17) -0.0034(17) 0.0047(15) O5 0.261(12) 0.126(8) 0.157(9) -0.017(6) 0.007(8) -0.002(7) O6 0.033(2) 0.0287(19) 0.029(2) 0.0008(15) -0.0025(16) -0.0022(15) O7 0.0217(17) 0.0294(19) 0.0311(19) -0.0046(15) -0.0057(15) 0.0041(14) O8 0.0272(18) 0.032(2) 0.0256(19) -0.0041(15) -0.0053(15) 0.0045(15) O9 0.036(2) 0.0252(19) 0.039(2) 0.0030(16) 0.0057(17) 0.0004(15) O10 0.119(6) 0.078(5) 0.235(10) 0.018(6) 0.002(6) 0.008(4) C1 0.028(3) 0.023(3) 0.029(3) 0.001(2) -0.004(2) 0.004(2) C2 0.032(3) 0.022(3) 0.032(3) 0.000(2) -0.005(2) 0.001(2) C3 0.042(3) 0.033(3) 0.025(3) -0.006(2) -0.001(2) 0.001(2) C4 0.035(3) 0.028(3) 0.029(3) 0.003(2) 0.002(2) 0.003(2) C5 0.028(3) 0.027(3) 0.036(3) 0.006(2) -0.002(2) 0.002(2) C6 0.030(3) 0.022(3) 0.025(3) 0.001(2) -0.002(2) 0.005(2) C7 0.027(3) 0.021(3) 0.025(3) 0.004(2) -0.005(2) -0.005(2) C8 0.024(2) 0.023(3) 0.026(3) -0.001(2) -0.004(2) -0.001(2) C9 0.037(3) 0.019(3) 0.026(3) 0.004(2) -0.005(2) 0.001(2) C10 0.032(3) 0.031(3) 0.025(3) 0.000(2) -0.006(2) -0.010(2) C11 0.025(3) 0.032(3) 0.030(3) -0.004(2) -0.002(2) 0.000(2) C12 0.024(3) 0.025(3) 0.022(3) 0.000(2) -0.006(2) -0.004(2) C13 0.021(2) 0.027(3) 0.030(3) 0.003(2) -0.003(2) 0.004(2) C14 0.038(3) 0.038(3) 0.035(3) -0.010(2) -0.004(3) -0.012(2) C15 0.060(4) 0.077(5) 0.044(4) -0.020(3) -0.005(3) -0.028(4) C16 0.037(3) 0.046(4) 0.043(3) 0.007(3) -0.009(3) -0.010(3) C17 0.051(4) 0.034(3) 0.061(4) 0.000(3) -0.001(3) -0.011(3) C18 0.048(4) 0.053(4) 0.036(3) 0.003(3) 0.010(3) -0.005(3) C19 0.028(3) 0.026(3) 0.048(3) 0.003(2) 0.000(3) 0.006(2) C20 0.048(4) 0.031(3) 0.081(5) 0.010(3) 0.014(4) 0.012(3) C21 0.043(3) 0.041(3) 0.047(4) 0.002(3) 0.012(3) 0.009(3) C22 0.030(3) 0.046(4) 0.052(4) 0.009(3) -0.006(3) 0.004(3) C23 0.044(3) 0.031(3) 0.050(4) 0.005(3) 0.007(3) -0.010(2) C24 0.018(3) 0.065(4) 0.049(4) 0.009(3) 0.002(3) 0.004(3) C25 0.028(3) 0.040(3) 0.072(5) 0.012(3) 0.015(3) 0.008(3) C26 0.039(3) 0.060(4) 0.043(4) -0.004(3) 0.016(3) -0.006(3) C27 0.028(3) 0.041(4) 0.059(4) 0.019(3) 0.010(3) -0.005(2) C28 0.029(3) 0.038(3) 0.058(4) -0.003(3) 0.004(3) -0.011(2) C29 0.069(4) 0.038(4) 0.049(4) 0.002(3) -0.016(3) -0.026(3) C30 0.083(5) 0.070(5) 0.072(5) 0.015(4) -0.044(4) -0.034(4) C31 0.068(5) 0.086(5) 0.046(4) 0.023(4) -0.017(4) -0.024(4) C32 0.062(4) 0.051(4) 0.032(3) 0.013(3) -0.008(3) -0.016(3) C33 0.030(3) 0.048(4) 0.089(5) 0.018(4) -0.001(3) 0.006(3) C34 0.040(4) 0.053(4) 0.140(8) 0.040(5) -0.014(4) 0.010(3) C35 0.059(4) 0.041(4) 0.078(5) 0.014(3) 0.005(4) 0.017(3) C36 0.057(4) 0.026(3) 0.082(5) -0.001(3) -0.018(4) 0.010(3) C37 0.138(10) 0.130(9) 0.076(7) -0.025(7) 0.004(7) -0.001(7) C38 0.233(15) 0.149(11) 0.046(6) 0.052(7) 0.038(7) -0.029(11) C39 0.124(10) 0.109(10) 0.33(2) 0.131(13) 0.106(13) 0.034(8) C40 0.178(13) 0.057(7) 0.229(17) -0.005(8) 0.041(12) -0.027(7) C41 0.033(3) 0.025(3) 0.024(3) -0.005(2) 0.001(2) 0.006(2) C42 0.045(3) 0.028(3) 0.024(3) -0.003(2) 0.003(2) 0.006(2) C43 0.059(4) 0.031(3) 0.024(3) 0.005(2) 0.004(3) 0.017(3) C44 0.039(3) 0.038(3) 0.027(3) -0.004(2) -0.005(2) 0.014(2) C45 0.028(3) 0.035(3) 0.033(3) -0.005(2) -0.001(2) 0.009(2) C46 0.029(3) 0.024(3) 0.024(3) -0.006(2) 0.001(2) 0.008(2) C47 0.024(2) 0.020(2) 0.024(3) 0.003(2) 0.000(2) 0.0019(19) C48 0.026(3) 0.020(3) 0.029(3) 0.002(2) 0.003(2) -0.0007(19) C49 0.028(3) 0.020(3) 0.031(3) -0.003(2) 0.007(2) 0.001(2) C50 0.034(3) 0.024(3) 0.025(3) 0.000(2) -0.001(2) -0.006(2) C51 0.017(2) 0.028(3) 0.027(3) 0.003(2) 0.001(2) -0.0026(19) C52 0.023(2) 0.023(3) 0.026(3) 0.002(2) 0.004(2) 0.0010(19) C53 0.020(2) 0.027(3) 0.024(3) -0.002(2) -0.002(2) 0.0007(19) C54 0.067(4) 0.024(3) 0.035(3) 0.004(2) 0.001(3) -0.012(3) C55 0.097(6) 0.038(4) 0.046(4) 0.005(3) 0.004(4) -0.016(3) C56 0.052(4) 0.048(4) 0.059(4) -0.004(3) 0.008(3) -0.018(3) C57 0.082(5) 0.027(3) 0.033(3) -0.003(2) 0.000(3) -0.007(3) C58 0.051(4) 0.057(4) 0.040(4) 0.003(3) -0.015(3) 0.014(3) C59 0.042(3) 0.032(3) 0.039(3) -0.005(2) -0.003(3) -0.004(2) C60 0.025(3) 0.028(3) 0.049(3) -0.009(2) 0.001(3) 0.007(2) C61 0.030(3) 0.051(4) 0.085(5) -0.026(4) -0.003(3) 0.018(3) C62 0.033(3) 0.041(3) 0.058(4) 0.001(3) -0.011(3) 0.009(3) C63 0.025(3) 0.048(4) 0.053(4) -0.010(3) 0.006(3) -0.001(2) C64 0.025(3) 0.076(5) 0.043(4) -0.004(3) 0.006(3) -0.017(3) C65 0.021(3) 0.051(4) 0.060(4) -0.012(3) -0.005(3) -0.001(2) C66 0.028(3) 0.065(4) 0.045(4) 0.003(3) -0.011(3) -0.002(3) C67 0.025(3) 0.074(5) 0.055(4) -0.031(4) -0.007(3) 0.001(3) C68 0.037(3) 0.036(4) 0.089(6) -0.001(4) -0.013(4) -0.014(3) C69 0.048(3) 0.039(3) 0.030(3) -0.014(2) -0.012(3) 0.004(3) C70 0.050(4) 0.051(4) 0.038(3) -0.016(3) 0.002(3) 0.012(3) C71 0.034(3) 0.044(4) 0.056(4) -0.014(3) -0.003(3) 0.009(3) C72 0.030(3) 0.041(3) 0.032(3) -0.002(2) -0.006(2) 0.010(2) C73 0.064(4) 0.027(3) 0.058(4) 0.009(3) 0.009(3) 0.009(3) C74 0.086(6) 0.042(4) 0.084(6) 0.018(4) 0.008(5) -0.010(4) C75 0.061(5) 0.061(5) 0.098(6) 0.018(4) 0.015(4) -0.015(4) C76 0.038(3) 0.044(4) 0.051(4) 0.008(3) 0.010(3) -0.007(3) C77 0.056(5) 0.054(5) 0.174(10) 0.027(6) -0.006(6) 0.007(4) C78 0.076(6) 0.029(4) 0.268(15) -0.004(6) -0.018(8) -0.005(4) C79 0.104(8) 0.083(7) 0.160(10) -0.028(7) -0.080(7) -0.008(6) C80 0.306(19) 0.090(8) 0.149(11) -0.018(7) -0.184(13) 0.054(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.067(3) . ? Yb1 O2 2.074(3) . ? Yb1 O3 2.334(3) . ? Yb1 O4 2.396(3) . ? Yb1 C24 2.604(5) . ? Yb1 C25 2.629(5) . ? Yb1 C28 2.634(5) . ? Yb1 C27 2.664(5) . ? Yb1 C26 2.681(5) . ? Yb2 O6 2.056(3) . ? Yb2 O7 2.083(3) . ? Yb2 O8 2.364(3) . ? Yb2 O9 2.385(3) . ? Yb2 C64 2.609(5) . ? Yb2 C68 2.615(6) . ? Yb2 C65 2.653(5) . ? Yb2 C67 2.667(6) . ? Yb2 C66 2.691(6) . ? O1 C1 1.334(6) . ? O2 C7 1.340(5) . ? O3 C29 1.459(6) . ? O3 C32 1.466(6) . ? O4 C36 1.442(7) . ? O4 C33 1.446(6) . ? O5 C40 1.444(10) . ? O5 C37 1.494(10) . ? O6 C41 1.347(6) . ? O7 C47 1.347(6) . ? O8 C69 1.463(6) . ? O8 C72 1.468(6) . ? O9 C76 1.454(6) . ? O9 C73 1.464(6) . ? O10 C80 1.360(12) . ? O10 C77 1.444(9) . ? C1 C6 1.414(7) . ? C1 C2 1.421(7) . ? C2 C3 1.391(7) . ? C2 C14 1.534(7) . ? C3 C4 1.402(7) . ? C3 H3 0.9500 . ? C4 C5 1.381(7) . ? C4 C18 1.508(7) . ? C5 C6 1.383(7) . ? C5 H5 0.9500 . ? C6 C13 1.522(7) . ? C7 C12 1.408(7) . ? C7 C8 1.419(6) . ? C8 C9 1.387(7) . ? C8 C19 1.536(7) . ? C9 C10 1.385(7) . ? C9 H9 0.9500 . ? C10 C11 1.386(7) . ? C10 C23 1.508(7) . ? C11 C12 1.387(7) . ? C11 H11 0.9500 . ? C12 C13 1.517(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.527(7) . ? C14 C16 1.530(8) . ? C14 C17 1.530(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.537(7) . ? C19 C21 1.540(8) . ? C19 C22 1.549(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.390(9) . ? C24 C28 1.394(8) . ? C24 H24A 1.0000 . ? C25 C26 1.397(8) . ? C25 H25A 1.0000 . ? C26 C27 1.394(8) . ? C26 H26A 1.0000 . ? C27 C28 1.387(8) . ? C27 H27A 1.0000 . ? C28 H28A 1.0000 . ? C29 C30 1.458(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.452(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.488(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.493(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.482(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.503(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.411(11) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.421(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.388(17) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.402(7) . ? C41 C42 1.419(7) . ? C42 C43 1.388(8) . ? C42 C54 1.544(8) . ? C43 C44 1.387(8) . ? C43 H43 0.9500 . ? C44 C45 1.373(7) . ? C44 C58 1.518(7) . ? C45 C46 1.396(7) . ? C45 H45 0.9500 . ? C46 C53 1.518(7) . ? C47 C48 1.411(6) . ? C47 C52 1.416(6) . ? C48 C49 1.392(7) . ? C48 C60 1.543(7) . ? C49 C50 1.385(7) . ? C49 H49 0.9500 . ? C50 C51 1.380(7) . ? C50 C59 1.511(7) . ? C51 C52 1.393(7) . ? C51 H51 0.9500 . ? C52 C53 1.511(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C56 1.527(8) . ? C54 C55 1.534(8) . ? C54 C57 1.545(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C63 1.531(7) . ? C60 C62 1.538(8) . ? C60 C61 1.544(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.379(9) . ? C64 C68 1.399(9) . ? C64 H64A 1.0000 . ? C65 C66 1.378(8) . ? C65 H65A 1.0000 . ? C66 C67 1.399(9) . ? C66 H66A 1.0000 . ? C67 C68 1.398(9) . ? C67 H67A 1.0000 . ? C68 H68A 1.0000 . ? C69 C70 1.509(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.519(8) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.503(7) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.485(9) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.491(10) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.495(8) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.445(10) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.433(10) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.436(11) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O2 88.81(13) . . ? O1 Yb1 O3 134.01(13) . . ? O2 Yb1 O3 82.91(12) . . ? O1 Yb1 O4 81.92(13) . . ? O2 Yb1 O4 137.93(12) . . ? O3 Yb1 O4 74.96(12) . . ? O1 Yb1 C24 93.86(17) . . ? O2 Yb1 C24 101.23(16) . . ? O3 Yb1 C24 132.13(17) . . ? O4 Yb1 C24 120.21(16) . . ? O1 Yb1 C25 121.65(18) . . ? O2 Yb1 C25 88.10(16) . . ? O3 Yb1 C25 103.26(18) . . ? O4 Yb1 C25 131.34(16) . . ? C24 Yb1 C25 30.80(19) . . ? O1 Yb1 C28 93.39(17) . . ? O2 Yb1 C28 132.08(16) . . ? O3 Yb1 C28 125.04(16) . . ? O4 Yb1 C28 89.56(16) . . ? C24 Yb1 C28 30.86(18) . . ? C25 Yb1 C28 50.85(19) . . ? O1 Yb1 C27 120.55(17) . . ? O2 Yb1 C27 136.72(15) . . ? O3 Yb1 C27 94.70(16) . . ? O4 Yb1 C27 81.19(15) . . ? C24 Yb1 C27 50.28(19) . . ? C25 Yb1 C27 50.21(18) . . ? C28 Yb1 C27 30.35(18) . . ? O1 Yb1 C26 142.42(17) . . ? O2 Yb1 C26 107.53(16) . . ? O3 Yb1 C26 82.49(16) . . ? O4 Yb1 C26 104.51(17) . . ? C24 Yb1 C26 50.49(19) . . ? C25 Yb1 C26 30.48(18) . . ? C28 Yb1 C26 50.44(19) . . ? C27 Yb1 C26 30.24(18) . . ? O6 Yb2 O7 90.24(13) . . ? O6 Yb2 O8 81.22(12) . . ? O7 Yb2 O8 139.24(12) . . ? O6 Yb2 O9 131.18(13) . . ? O7 Yb2 O9 81.24(12) . . ? O8 Yb2 O9 75.22(12) . . ? O6 Yb2 C64 93.43(18) . . ? O7 Yb2 C64 97.46(17) . . ? O8 Yb2 C64 122.66(17) . . ? O9 Yb2 C64 135.24(17) . . ? O6 Yb2 C68 93.69(19) . . ? O7 Yb2 C68 128.49(18) . . ? O8 Yb2 C68 91.96(17) . . ? O9 Yb2 C68 128.75(19) . . ? C64 Yb2 C68 31.06(19) . . ? O6 Yb2 C65 120.69(17) . . ? O7 Yb2 C65 84.13(15) . . ? O8 Yb2 C65 134.14(15) . . ? O9 Yb2 C65 106.21(17) . . ? C64 Yb2 C65 30.36(19) . . ? C68 Yb2 C65 50.46(19) . . ? O6 Yb2 C67 121.48(19) . . ? O7 Yb2 C67 132.37(16) . . ? O8 Yb2 C67 84.17(15) . . ? O9 Yb2 C67 98.09(18) . . ? C64 Yb2 C67 50.68(19) . . ? C68 Yb2 C67 30.7(2) . . ? C65 Yb2 C67 50.00(18) . . ? O6 Yb2 C66 141.99(17) . . ? O7 Yb2 C66 103.09(16) . . ? O8 Yb2 C66 108.03(16) . . ? O9 Yb2 C66 86.40(16) . . ? C64 Yb2 C66 50.02(19) . . ? C68 Yb2 C66 50.3(2) . . ? C65 Yb2 C66 29.88(18) . . ? C67 Yb2 C66 30.26(19) . . ? C1 O1 Yb1 148.9(3) . . ? C7 O2 Yb1 149.2(3) . . ? C29 O3 C32 107.0(4) . . ? C29 O3 Yb1 126.6(3) . . ? C32 O3 Yb1 126.1(3) . . ? C36 O4 C33 104.9(4) . . ? C36 O4 Yb1 123.5(3) . . ? C33 O4 Yb1 122.1(3) . . ? C40 O5 C37 105.8(10) . . ? C41 O6 Yb2 149.4(3) . . ? C47 O7 Yb2 147.2(3) . . ? C69 O8 C72 108.3(4) . . ? C69 O8 Yb2 126.3(3) . . ? C72 O8 Yb2 125.4(3) . . ? C76 O9 C73 108.7(4) . . ? C76 O9 Yb2 129.8(3) . . ? C73 O9 Yb2 118.9(3) . . ? C80 O10 C77 107.2(8) . . ? O1 C1 C6 120.1(4) . . ? O1 C1 C2 120.9(4) . . ? C6 C1 C2 119.1(4) . . ? C3 C2 C1 117.6(5) . . ? C3 C2 C14 121.8(5) . . ? C1 C2 C14 120.5(4) . . ? C2 C3 C4 124.0(5) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C5 C4 C3 116.5(5) . . ? C5 C4 C18 122.6(5) . . ? C3 C4 C18 120.9(5) . . ? C4 C5 C6 122.6(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 120.0(5) . . ? C5 C6 C13 118.5(4) . . ? C1 C6 C13 121.4(4) . . ? O2 C7 C12 119.6(4) . . ? O2 C7 C8 120.9(4) . . ? C12 C7 C8 119.4(4) . . ? C9 C8 C7 117.7(4) . . ? C9 C8 C19 121.6(4) . . ? C7 C8 C19 120.7(4) . . ? C10 C9 C8 123.9(4) . . ? C10 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C9 C10 C11 117.0(4) . . ? C9 C10 C23 121.1(5) . . ? C11 C10 C23 121.9(5) . . ? C10 C11 C12 122.3(5) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C7 119.6(4) . . ? C11 C12 C13 118.3(4) . . ? C7 C12 C13 122.1(4) . . ? C12 C13 C6 113.1(4) . . ? C12 C13 H13A 108.9 . . ? C6 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? C6 C13 H13B 108.9 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C16 107.9(5) . . ? C15 C14 C17 107.1(5) . . ? C16 C14 C17 110.4(5) . . ? C15 C14 C2 111.9(5) . . ? C16 C14 C2 109.5(4) . . ? C17 C14 C2 109.9(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C19 C20 112.5(4) . . ? C8 C19 C21 109.7(4) . . ? C20 C19 C21 107.3(5) . . ? C8 C19 C22 109.4(4) . . ? C20 C19 C22 107.2(5) . . ? C21 C19 C22 110.6(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C28 108.5(6) . . ? C25 C24 Yb1 75.6(3) . . ? C28 C24 Yb1 75.8(3) . . ? C25 C24 H24A 125.1 . . ? C28 C24 H24A 125.1 . . ? Yb1 C24 H24A 125.1 . . ? C24 C25 C26 108.0(5) . . ? C24 C25 Yb1 73.6(3) . . ? C26 C25 Yb1 76.8(3) . . ? C24 C25 H25A 125.4 . . ? C26 C25 H25A 125.4 . . ? Yb1 C25 H25A 125.4 . . ? C27 C26 C25 107.2(6) . . ? C27 C26 Yb1 74.2(3) . . ? C25 C26 Yb1 72.7(3) . . ? C27 C26 H26A 126.1 . . ? C25 C26 H26A 126.1 . . ? Yb1 C26 H26A 126.1 . . ? C28 C27 C26 109.1(5) . . ? C28 C27 Yb1 73.7(3) . . ? C26 C27 Yb1 75.6(3) . . ? C28 C27 H27A 125.1 . . ? C26 C27 H27A 125.1 . . ? Yb1 C27 H27A 125.1 . . ? C27 C28 C24 107.2(5) . . ? C27 C28 Yb1 76.0(3) . . ? C24 C28 Yb1 73.4(3) . . ? C27 C28 H28A 125.8 . . ? C24 C28 H28A 125.8 . . ? Yb1 C28 H28A 125.8 . . ? C30 C29 O3 106.5(5) . . ? C30 C29 H29A 110.4 . . ? O3 C29 H29A 110.4 . . ? C30 C29 H29B 110.4 . . ? O3 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C31 C30 C29 108.4(5) . . ? C31 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? C31 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? C30 C31 C32 107.0(5) . . ? C30 C31 H31A 110.3 . . ? C32 C31 H31A 110.3 . . ? C30 C31 H31B 110.3 . . ? C32 C31 H31B 110.3 . . ? H31A C31 H31B 108.6 . . ? O3 C32 C31 105.2(5) . . ? O3 C32 H32A 110.7 . . ? C31 C32 H32A 110.7 . . ? O3 C32 H32B 110.7 . . ? C31 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? O4 C33 C34 104.7(5) . . ? O4 C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? O4 C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? C35 C34 C33 105.4(5) . . ? C35 C34 H34A 110.7 . . ? C33 C34 H34A 110.7 . . ? C35 C34 H34B 110.7 . . ? C33 C34 H34B 110.7 . . ? H34A C34 H34B 108.8 . . ? C34 C35 C36 105.2(5) . . ? C34 C35 H35A 110.7 . . ? C36 C35 H35A 110.7 . . ? C34 C35 H35B 110.7 . . ? C36 C35 H35B 110.7 . . ? H35A C35 H35B 108.8 . . ? O4 C36 C35 106.9(5) . . ? O4 C36 H36A 110.3 . . ? C35 C36 H36A 110.3 . . ? O4 C36 H36B 110.3 . . ? C35 C36 H36B 110.3 . . ? H36A C36 H36B 108.6 . . ? C38 C37 O5 106.5(9) . . ? C38 C37 H37A 110.4 . . ? O5 C37 H37A 110.4 . . ? C38 C37 H37B 110.4 . . ? O5 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? C37 C38 C39 109.2(9) . . ? C37 C38 H38A 109.8 . . ? C39 C38 H38A 109.8 . . ? C37 C38 H38B 109.8 . . ? C39 C38 H38B 109.8 . . ? H38A C38 H38B 108.3 . . ? C40 C39 C38 109.1(9) . . ? C40 C39 H39A 109.9 . . ? C38 C39 H39A 109.9 . . ? C40 C39 H39B 109.9 . . ? C38 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? C39 C40 O5 109.2(11) . . ? C39 C40 H40A 109.8 . . ? O5 C40 H40A 109.8 . . ? C39 C40 H40B 109.8 . . ? O5 C40 H40B 109.8 . . ? H40A C40 H40B 108.3 . . ? O6 C41 C46 119.3(4) . . ? O6 C41 C42 120.8(5) . . ? C46 C41 C42 119.9(5) . . ? C43 C42 C41 117.5(5) . . ? C43 C42 C54 121.9(5) . . ? C41 C42 C54 120.6(5) . . ? C44 C43 C42 123.3(5) . . ? C44 C43 H43 118.4 . . ? C42 C43 H43 118.4 . . ? C45 C44 C43 118.2(5) . . ? C45 C44 C58 120.9(5) . . ? C43 C44 C58 120.9(5) . . ? C44 C45 C46 121.5(5) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C45 C46 C41 119.6(5) . . ? C45 C46 C53 119.2(4) . . ? C41 C46 C53 121.2(4) . . ? O7 C47 C48 121.4(4) . . ? O7 C47 C52 119.0(4) . . ? C48 C47 C52 119.5(4) . . ? C49 C48 C47 118.7(4) . . ? C49 C48 C60 121.0(4) . . ? C47 C48 C60 120.2(4) . . ? C50 C49 C48 122.6(4) . . ? C50 C49 H49 118.7 . . ? C48 C49 H49 118.7 . . ? C51 C50 C49 117.8(4) . . ? C51 C50 C59 121.2(5) . . ? C49 C50 C59 121.0(4) . . ? C50 C51 C52 122.6(4) . . ? C50 C51 H51 118.7 . . ? C52 C51 H51 118.7 . . ? C51 C52 C47 118.7(4) . . ? C51 C52 C53 118.8(4) . . ? C47 C52 C53 122.4(4) . . ? C52 C53 C46 114.5(4) . . ? C52 C53 H53A 108.6 . . ? C46 C53 H53A 108.6 . . ? C52 C53 H53B 108.6 . . ? C46 C53 H53B 108.6 . . ? H53A C53 H53B 107.6 . . ? C56 C54 C55 107.9(5) . . ? C56 C54 C42 110.1(5) . . ? C55 C54 C42 111.7(5) . . ? C56 C54 C57 110.0(5) . . ? C55 C54 C57 106.5(5) . . ? C42 C54 C57 110.6(5) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C44 C58 H58A 109.5 . . ? C44 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C44 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C50 C59 H59A 109.5 . . ? C50 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C50 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C63 C60 C62 110.4(5) . . ? C63 C60 C48 108.2(4) . . ? C62 C60 C48 111.4(4) . . ? C63 C60 C61 107.0(5) . . ? C62 C60 C61 107.3(5) . . ? C48 C60 C61 112.4(4) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C68 107.9(6) . . ? C65 C64 Yb2 76.6(3) . . ? C68 C64 Yb2 74.7(3) . . ? C65 C64 H64A 125.3 . . ? C68 C64 H64A 125.3 . . ? Yb2 C64 H64A 125.3 . . ? C66 C65 C64 108.8(6) . . ? C66 C65 Yb2 76.6(3) . . ? C64 C65 Yb2 73.1(3) . . ? C66 C65 H65A 125.1 . . ? C64 C65 H65A 125.1 . . ? Yb2 C65 H65A 125.1 . . ? C65 C66 C67 108.1(6) . . ? C65 C66 Yb2 73.5(3) . . ? C67 C66 Yb2 73.9(3) . . ? C65 C66 H66A 125.6 . . ? C67 C66 H66A 125.6 . . ? Yb2 C66 H66A 125.6 . . ? C68 C67 C66 107.4(6) . . ? C68 C67 Yb2 72.6(3) . . ? C66 C67 Yb2 75.8(3) . . ? C68 C67 H67A 125.8 . . ? C66 C67 H67A 125.8 . . ? Yb2 C67 H67A 125.8 . . ? C67 C68 C64 107.7(6) . . ? C67 C68 Yb2 76.7(3) . . ? C64 C68 Yb2 74.2(3) . . ? C67 C68 H68A 125.5 . . ? C64 C68 H68A 125.5 . . ? Yb2 C68 H68A 125.5 . . ? O8 C69 C70 105.3(4) . . ? O8 C69 H69A 110.7 . . ? C70 C69 H69A 110.7 . . ? O8 C69 H69B 110.7 . . ? C70 C69 H69B 110.7 . . ? H69A C69 H69B 108.8 . . ? C69 C70 C71 101.7(5) . . ? C69 C70 H70A 111.4 . . ? C71 C70 H70A 111.4 . . ? C69 C70 H70B 111.4 . . ? C71 C70 H70B 111.4 . . ? H70A C70 H70B 109.3 . . ? C72 C71 C70 102.5(4) . . ? C72 C71 H71A 111.3 . . ? C70 C71 H71A 111.3 . . ? C72 C71 H71B 111.3 . . ? C70 C71 H71B 111.3 . . ? H71A C71 H71B 109.2 . . ? O8 C72 C71 105.8(4) . . ? O8 C72 H72A 110.6 . . ? C71 C72 H72A 110.6 . . ? O8 C72 H72B 110.6 . . ? C71 C72 H72B 110.6 . . ? H72A C72 H72B 108.7 . . ? O9 C73 C74 105.7(5) . . ? O9 C73 H73A 110.6 . . ? C74 C73 H73A 110.6 . . ? O9 C73 H73B 110.6 . . ? C74 C73 H73B 110.6 . . ? H73A C73 H73B 108.7 . . ? C73 C74 C75 103.9(6) . . ? C73 C74 H74A 111.0 . . ? C75 C74 H74A 111.0 . . ? C73 C74 H74B 111.0 . . ? C75 C74 H74B 111.0 . . ? H74A C74 H74B 109.0 . . ? C74 C75 C76 103.7(6) . . ? C74 C75 H75A 111.0 . . ? C76 C75 H75A 111.0 . . ? C74 C75 H75B 111.0 . . ? C76 C75 H75B 111.0 . . ? H75A C75 H75B 109.0 . . ? O9 C76 C75 105.7(5) . . ? O9 C76 H76A 110.6 . . ? C75 C76 H76A 110.6 . . ? O9 C76 H76B 110.6 . . ? C75 C76 H76B 110.6 . . ? H76A C76 H76B 108.7 . . ? O10 C77 C78 107.4(7) . . ? O10 C77 H77A 110.2 . . ? C78 C77 H77A 110.2 . . ? O10 C77 H77B 110.2 . . ? C78 C77 H77B 110.2 . . ? H77A C77 H77B 108.5 . . ? C79 C78 C77 107.7(7) . . ? C79 C78 H78A 110.2 . . ? C77 C78 H78A 110.2 . . ? C79 C78 H78B 110.2 . . ? C77 C78 H78B 110.2 . . ? H78A C78 H78B 108.5 . . ? C78 C79 C80 105.4(8) . . ? C78 C79 H79A 110.7 . . ? C80 C79 H79A 110.7 . . ? C78 C79 H79B 110.7 . . ? C80 C79 H79B 110.7 . . ? H79A C79 H79B 108.8 . . ? O10 C80 C79 111.6(8) . . ? O10 C80 H80A 109.3 . . ? C79 C80 H80A 109.3 . . ? O10 C80 H80B 109.3 . . ? C79 C80 H80B 109.3 . . ? H80A C80 H80B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.244 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.100 #============================================================end data_complex5 _database_code_depnum_ccdc_archive 'CCDC 682656' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H77 O6 Yb, 2(0.5(C6H14))' _chemical_formula_sum 'C60 H91 O6 Yb' _chemical_formula_weight 1081.37 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' Yb Yb -0.3850 5.5486 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4994(19) _cell_length_b 14.861(2) _cell_length_c 16.937(3) _cell_angle_alpha 106.815(3) _cell_angle_beta 106.272(2) _cell_angle_gamma 93.210(2) _cell_volume 2858.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11788 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_T_max 0.668 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27901 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.34 _reflns_number_total 10375 _reflns_number_gt 9725 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0455P)^2^+7.9800P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10375 _refine_ls_number_parameters 566 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.915184(14) 0.202716(12) 0.244358(11) 0.02377(7) Uani 1 1 d . . . O1 O 0.8877(2) 0.2205(2) 0.12395(18) 0.0288(6) Uani 1 1 d . . . O2 O 0.8012(3) 0.0695(2) 0.20760(18) 0.0306(7) Uani 1 1 d . . . O3 O 1.0581(2) 0.2743(2) 0.34582(18) 0.0292(6) Uani 1 1 d . . . O4 O 0.8223(3) 0.1895(2) 0.34476(19) 0.0310(7) Uani 1 1 d D . . H4A H 0.800(4) 0.1348(18) 0.315(3) 0.037 Uiso 1 1 d D . . O5 O 1.0439(3) 0.1020(2) 0.20619(19) 0.0338(7) Uani 1 1 d . . . O6 O 0.8506(3) 0.3510(2) 0.2809(2) 0.0377(8) Uani 1 1 d . . . C1 C 0.8245(4) 0.2162(3) 0.0438(3) 0.0256(9) Uani 1 1 d . . . C2 C 0.8675(4) 0.2590(3) -0.0076(3) 0.0296(9) Uani 1 1 d . . . C3 C 0.7951(4) 0.2496(4) -0.0907(3) 0.0413(12) Uani 1 1 d . . . H3 H 0.8224 0.2770 -0.1262 0.050 Uiso 1 1 calc R . . C4 C 0.6858(4) 0.2023(4) -0.1230(3) 0.0461(13) Uani 1 1 d . . . C5 C 0.6456(4) 0.1631(4) -0.0705(3) 0.0413(12) Uani 1 1 d . . . H5 H 0.5708 0.1321 -0.0909 0.050 Uiso 1 1 calc R . . C6 C 0.7130(4) 0.1684(3) 0.0119(3) 0.0295(9) Uani 1 1 d . . . C7 C 0.7452(4) -0.0017(3) 0.1331(3) 0.0285(9) Uani 1 1 d . . . C8 C 0.7454(4) -0.0985(3) 0.1288(3) 0.0296(9) Uani 1 1 d . . . C9 C 0.6945(4) -0.1661(3) 0.0479(3) 0.0345(10) Uani 1 1 d . . . H9 H 0.6950 -0.2307 0.0433 0.041 Uiso 1 1 calc R . . C10 C 0.6426(4) -0.1432(4) -0.0266(3) 0.0371(11) Uani 1 1 d . . . C11 C 0.6376(4) -0.0494(3) -0.0184(3) 0.0324(10) Uani 1 1 d . . . H11 H 0.6004 -0.0328 -0.0675 0.039 Uiso 1 1 calc R . . C12 C 0.6857(3) 0.0223(3) 0.0603(3) 0.0281(9) Uani 1 1 d . . . C13 C 0.6650(4) 0.1236(3) 0.0664(3) 0.0301(9) Uani 1 1 d . . . H13A H 0.5835 0.1242 0.0496 0.036 Uiso 1 1 calc R . . H13B H 0.6968 0.1634 0.1272 0.036 Uiso 1 1 calc R . . C14 C 0.9868(4) 0.3143(3) 0.0246(3) 0.0344(10) Uani 1 1 d . . . C15 C 1.0133(5) 0.3552(4) -0.0426(4) 0.0508(14) Uani 1 1 d . . . H15A H 1.0051 0.3038 -0.0955 0.076 Uiso 1 1 calc R . . H15B H 1.0900 0.3884 -0.0196 0.076 Uiso 1 1 calc R . . H15C H 0.9615 0.3991 -0.0550 0.076 Uiso 1 1 calc R . . C16 C 1.0746(4) 0.2501(4) 0.0453(3) 0.0427(12) Uani 1 1 d . . . H16A H 1.0636 0.2264 0.0906 0.064 Uiso 1 1 calc R . . H16B H 1.1496 0.2862 0.0650 0.064 Uiso 1 1 calc R . . H16C H 1.0665 0.1971 -0.0064 0.064 Uiso 1 1 calc R . . C17 C 1.0007(5) 0.3993(4) 0.1066(3) 0.0435(12) Uani 1 1 d . . . H17A H 0.9455 0.4405 0.0933 0.065 Uiso 1 1 calc R . . H17B H 1.0760 0.4347 0.1260 0.065 Uiso 1 1 calc R . . H17C H 0.9894 0.3761 0.1521 0.065 Uiso 1 1 calc R . . C18 C 0.6122(6) 0.1957(6) -0.2132(4) 0.076(2) Uani 1 1 d . . . H18A H 0.5764 0.1305 -0.2445 0.115 Uiso 1 1 calc R . . H18B H 0.6584 0.2159 -0.2442 0.115 Uiso 1 1 calc R . . H18C H 0.5548 0.2365 -0.2086 0.115 Uiso 1 1 calc R . . C19 C 0.7961(4) -0.1283(3) 0.2095(3) 0.0374(11) Uani 1 1 d . . . C20 C 0.7753(5) -0.2362(4) 0.1902(4) 0.0519(14) Uani 1 1 d . . . H20A H 0.6950 -0.2590 0.1651 0.078 Uiso 1 1 calc R . . H20B H 0.8037 -0.2513 0.2436 0.078 Uiso 1 1 calc R . . H20C H 0.8139 -0.2668 0.1496 0.078 Uiso 1 1 calc R . . C21 C 0.7416(6) -0.0846(4) 0.2801(4) 0.0559(15) Uani 1 1 d . . . H21A H 0.7609 -0.0160 0.2999 0.084 Uiso 1 1 calc R . . H21B H 0.7693 -0.1085 0.3285 0.084 Uiso 1 1 calc R . . H21C H 0.6604 -0.1019 0.2563 0.084 Uiso 1 1 calc R . . C22 C 0.9241(5) -0.0975(4) 0.2456(4) 0.0509(14) Uani 1 1 d . . . H22A H 0.9588 -0.1291 0.2025 0.076 Uiso 1 1 calc R . . H22B H 0.9537 -0.1148 0.2977 0.076 Uiso 1 1 calc R . . H22C H 0.9409 -0.0292 0.2593 0.076 Uiso 1 1 calc R . . C23 C 0.5923(5) -0.2209(4) -0.1131(3) 0.0529(14) Uani 1 1 d . . . H23A H 0.5372 -0.2658 -0.1082 0.079 Uiso 1 1 calc R . . H23B H 0.6517 -0.2537 -0.1295 0.079 Uiso 1 1 calc R . . H23C H 0.5561 -0.1930 -0.1570 0.079 Uiso 1 1 calc R . . C24 C 1.1442(3) 0.2935(3) 0.4196(3) 0.0254(9) Uani 1 1 d . . . C25 C 1.2417(4) 0.3582(3) 0.4372(3) 0.0268(9) Uani 1 1 d . . . C26 C 1.3276(4) 0.3723(3) 0.5152(3) 0.0323(10) Uani 1 1 d . . . H26 H 1.3924 0.4160 0.5282 0.039 Uiso 1 1 calc R . . C27 C 1.3223(4) 0.3254(4) 0.5741(3) 0.0358(11) Uani 1 1 d . . . C28 C 1.2257(4) 0.2624(3) 0.5546(3) 0.0327(10) Uani 1 1 d . . . H28 H 1.2207 0.2293 0.5934 0.039 Uiso 1 1 calc R . . C29 C 1.1357(4) 0.2465(3) 0.4796(3) 0.0271(9) Uani 1 1 d . . . C30 C 0.8310(4) 0.2125(3) 0.4324(3) 0.0281(9) Uani 1 1 d . . . C31 C 0.7363(4) 0.2348(3) 0.4594(3) 0.0305(9) Uani 1 1 d . . . C32 C 0.7540(4) 0.2639(3) 0.5482(3) 0.0354(10) Uani 1 1 d . . . H32 H 0.6927 0.2798 0.5686 0.042 Uiso 1 1 calc R . . C33 C 0.8587(4) 0.2705(3) 0.6086(3) 0.0364(11) Uani 1 1 d . . . C34 C 0.9479(4) 0.2452(3) 0.5785(3) 0.0340(10) Uani 1 1 d . . . H34 H 1.0188 0.2490 0.6185 0.041 Uiso 1 1 calc R . . C35 C 0.9354(4) 0.2141(3) 0.4901(3) 0.0286(9) Uani 1 1 d . . . C36 C 1.0330(4) 0.1754(3) 0.4604(3) 0.0311(10) Uani 1 1 d . . . H36A H 1.0570 0.1268 0.4874 0.037 Uiso 1 1 calc R . . H36B H 1.0047 0.1437 0.3975 0.037 Uiso 1 1 calc R . . C37 C 1.2543(4) 0.4095(3) 0.3730(3) 0.0324(10) Uani 1 1 d . . . C38 C 1.3665(4) 0.4762(4) 0.4064(3) 0.0454(12) Uani 1 1 d . . . H38A H 1.3723 0.5223 0.4619 0.068 Uiso 1 1 calc R . . H38B H 1.3700 0.5090 0.3651 0.068 Uiso 1 1 calc R . . H38C H 1.4282 0.4394 0.4135 0.068 Uiso 1 1 calc R . . C39 C 1.2514(4) 0.3389(4) 0.2860(3) 0.0439(12) Uani 1 1 d . . . H39A H 1.3144 0.3036 0.2948 0.066 Uiso 1 1 calc R . . H39B H 1.2568 0.3732 0.2461 0.066 Uiso 1 1 calc R . . H39C H 1.1813 0.2950 0.2619 0.066 Uiso 1 1 calc R . . C40 C 1.1602(4) 0.4703(4) 0.3571(4) 0.0430(12) Uani 1 1 d . . . H40A H 1.0881 0.4293 0.3285 0.064 Uiso 1 1 calc R . . H40B H 1.1736 0.5065 0.3205 0.064 Uiso 1 1 calc R . . H40C H 1.1595 0.5136 0.4121 0.064 Uiso 1 1 calc R . . C41 C 1.4197(5) 0.3394(5) 0.6551(4) 0.0589(16) Uani 1 1 d . . . H41A H 1.3920 0.3242 0.6985 0.088 Uiso 1 1 calc R . . H41B H 1.4559 0.4050 0.6775 0.088 Uiso 1 1 calc R . . H41C H 1.4738 0.2979 0.6415 0.088 Uiso 1 1 calc R . . C42 C 0.6171(4) 0.2261(3) 0.3950(3) 0.0340(10) Uani 1 1 d . . . C43 C 0.5279(4) 0.2408(4) 0.4420(4) 0.0462(13) Uani 1 1 d . . . H43A H 0.4542 0.2331 0.4000 0.069 Uiso 1 1 calc R . . H43B H 0.5450 0.3044 0.4835 0.069 Uiso 1 1 calc R . . H43C H 0.5280 0.1944 0.4721 0.069 Uiso 1 1 calc R . . C44 C 0.5809(4) 0.1273(4) 0.3259(4) 0.0488(13) Uani 1 1 d . . . H44A H 0.5992 0.0788 0.3533 0.073 Uiso 1 1 calc R . . H44B H 0.6204 0.1230 0.2834 0.073 Uiso 1 1 calc R . . H44C H 0.5003 0.1179 0.2973 0.073 Uiso 1 1 calc R . . C45 C 0.6146(4) 0.3024(4) 0.3501(3) 0.0405(11) Uani 1 1 d . . . H45A H 0.6658 0.2920 0.3157 0.061 Uiso 1 1 calc R . . H45B H 0.6377 0.3648 0.3936 0.061 Uiso 1 1 calc R . . H45C H 0.5388 0.2986 0.3127 0.061 Uiso 1 1 calc R . . C46 C 0.8730(5) 0.3016(5) 0.7048(3) 0.0536(15) Uani 1 1 d . . . H46A H 0.8777 0.2466 0.7249 0.080 Uiso 1 1 calc R . . H46B H 0.8088 0.3312 0.7152 0.080 Uiso 1 1 calc R . . H46C H 0.9414 0.3469 0.7360 0.080 Uiso 1 1 calc R . . C47 C 1.1502(5) 0.0897(5) 0.2614(4) 0.0596(8) Uani 1 1 d D . . H47A H 1.1369 0.0549 0.2997 0.072 Uiso 1 1 calc R . . H47B H 1.1953 0.1516 0.2973 0.072 Uiso 1 1 calc R . . C48 C 1.2087(5) 0.0355(5) 0.2035(4) 0.0596(8) Uani 1 1 d D . . H48A H 1.2255 -0.0230 0.2169 0.072 Uiso 1 1 calc R . . H48B H 1.2799 0.0733 0.2113 0.072 Uiso 1 1 calc R . . C49 C 1.1343(5) 0.0122(5) 0.1127(4) 0.0596(8) Uani 1 1 d D . . H49A H 1.1283 -0.0555 0.0813 0.072 Uiso 1 1 calc R . . H49B H 1.1640 0.0495 0.0823 0.072 Uiso 1 1 calc R . . C50 C 1.0224(5) 0.0365(5) 0.1190(4) 0.0596(8) Uani 1 1 d . . . H50A H 0.9881 0.0667 0.0756 0.072 Uiso 1 1 calc R . . H50B H 0.9714 -0.0207 0.1098 0.072 Uiso 1 1 calc R . . C51 C 0.7822(7) 0.3962(4) 0.2236(5) 0.0709(10) Uani 1 1 d . . . H51A H 0.7017 0.3778 0.2133 0.085 Uiso 1 1 calc R . . H51B H 0.7972 0.3795 0.1677 0.085 Uiso 1 1 calc R . . C52 C 0.8181(7) 0.5004(4) 0.2720(4) 0.0709(10) Uani 1 1 d D . . H52A H 0.8720 0.5269 0.2493 0.085 Uiso 1 1 calc R . . H52B H 0.7525 0.5339 0.2644 0.085 Uiso 1 1 calc R . . C53 C 0.8703(7) 0.5132(4) 0.3643(4) 0.0709(10) Uani 1 1 d D . . H53A H 0.8220 0.5426 0.3980 0.085 Uiso 1 1 calc R . . H53B H 0.9437 0.5538 0.3864 0.085 Uiso 1 1 calc R . . C54 C 0.8842(7) 0.4163(4) 0.3705(5) 0.0709(10) Uani 1 1 d . . . H54A H 0.9627 0.4142 0.4010 0.085 Uiso 1 1 calc R . . H54B H 0.8362 0.3986 0.4022 0.085 Uiso 1 1 calc R . . C55 C 0.5543(6) -0.0099(7) 0.4927(6) 0.102(3) Uiso 1 1 d D . . H55A H 0.5618 0.0163 0.4473 0.122 Uiso 1 1 calc R . . H55B H 0.5496 -0.0790 0.4694 0.122 Uiso 1 1 calc R . . C56 C 0.6600(10) 0.0257(9) 0.5668(8) 0.141(4) Uiso 1 1 d D . . H56A H 0.6574 -0.0054 0.6102 0.170 Uiso 1 1 calc R . . H56B H 0.6631 0.0941 0.5939 0.170 Uiso 1 1 calc R . . C57 C 0.7655(7) 0.0095(6) 0.5433(6) 0.091(2) Uiso 1 1 d . . . H57A H 0.7656 -0.0582 0.5195 0.136 Uiso 1 1 calc R . . H57B H 0.8303 0.0363 0.5947 0.136 Uiso 1 1 calc R . . H57C H 0.7691 0.0399 0.5004 0.136 Uiso 1 1 calc R . . C58 C 0.668(5) 0.488(5) 0.883(4) 0.255(10) Uiso 0.50 1 d PD . . C59 C 0.637(4) 0.493(5) 0.965(3) 0.255(10) Uiso 0.50 1 d PD . . C60 C 0.512(4) 0.497(4) 0.939(3) 0.255(10) Uiso 0.50 1 d PD . . C61 C 0.477(5) 0.476(4) 1.013(4) 0.255(10) Uiso 0.50 1 d PD . . C62 C 0.387(4) 0.540(4) 1.017(3) 0.255(10) Uiso 0.50 1 d PD . . C63 C 0.362(6) 0.523(5) 1.096(4) 0.255(10) Uiso 0.50 1 d PD . . 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 Yb1 0.02362(11) 0.02536(11) 0.02124(11) 0.00701(7) 0.00585(7) 0.00268(7) O1 0.0311(16) 0.0337(16) 0.0209(15) 0.0102(13) 0.0060(13) 0.0034(13) O2 0.0381(17) 0.0265(15) 0.0236(15) 0.0043(12) 0.0091(13) -0.0018(13) O3 0.0297(16) 0.0300(16) 0.0226(15) 0.0053(12) 0.0035(13) 0.0022(13) O4 0.0340(17) 0.0310(16) 0.0254(16) 0.0048(13) 0.0104(14) -0.0005(14) O5 0.0322(17) 0.0346(17) 0.0292(16) 0.0024(13) 0.0072(13) 0.0138(14) O6 0.047(2) 0.0289(17) 0.0393(18) 0.0102(14) 0.0163(16) 0.0133(15) C1 0.027(2) 0.027(2) 0.020(2) 0.0058(17) 0.0044(17) 0.0074(17) C2 0.034(2) 0.031(2) 0.025(2) 0.0104(18) 0.0095(19) 0.0084(19) C3 0.049(3) 0.049(3) 0.032(3) 0.023(2) 0.012(2) 0.009(2) C4 0.041(3) 0.059(3) 0.035(3) 0.023(2) -0.001(2) 0.003(3) C5 0.033(3) 0.048(3) 0.038(3) 0.016(2) 0.001(2) 0.005(2) C6 0.026(2) 0.033(2) 0.029(2) 0.0110(19) 0.0076(18) 0.0095(18) C7 0.027(2) 0.033(2) 0.025(2) 0.0055(18) 0.0112(18) 0.0024(18) C8 0.025(2) 0.030(2) 0.033(2) 0.0080(19) 0.0108(19) 0.0021(18) C9 0.031(2) 0.031(2) 0.037(3) 0.002(2) 0.012(2) 0.0044(19) C10 0.027(2) 0.043(3) 0.030(2) -0.003(2) 0.007(2) 0.003(2) C11 0.027(2) 0.041(3) 0.028(2) 0.009(2) 0.0099(19) 0.005(2) C12 0.022(2) 0.035(2) 0.029(2) 0.0093(19) 0.0119(18) 0.0029(18) C13 0.024(2) 0.035(2) 0.032(2) 0.0098(19) 0.0103(18) 0.0057(18) C14 0.040(3) 0.035(3) 0.030(2) 0.012(2) 0.013(2) 0.002(2) C15 0.055(3) 0.057(3) 0.046(3) 0.024(3) 0.019(3) -0.003(3) C16 0.032(3) 0.051(3) 0.047(3) 0.015(2) 0.015(2) 0.007(2) C17 0.049(3) 0.035(3) 0.040(3) 0.008(2) 0.011(2) -0.004(2) C18 0.062(4) 0.115(6) 0.047(4) 0.047(4) -0.010(3) -0.004(4) C19 0.043(3) 0.032(2) 0.036(3) 0.011(2) 0.012(2) 0.002(2) C20 0.063(4) 0.039(3) 0.055(3) 0.021(3) 0.015(3) 0.006(3) C21 0.085(4) 0.050(3) 0.051(3) 0.027(3) 0.036(3) 0.016(3) C22 0.050(3) 0.049(3) 0.050(3) 0.026(3) -0.001(3) 0.003(3) C23 0.053(3) 0.053(3) 0.034(3) -0.005(2) 0.003(2) 0.009(3) C24 0.024(2) 0.027(2) 0.021(2) 0.0027(17) 0.0047(17) 0.0085(17) C25 0.026(2) 0.029(2) 0.023(2) 0.0027(17) 0.0086(17) 0.0074(17) C26 0.021(2) 0.041(3) 0.029(2) 0.004(2) 0.0057(18) 0.0067(19) C27 0.029(2) 0.049(3) 0.027(2) 0.011(2) 0.0050(19) 0.010(2) C28 0.035(2) 0.038(3) 0.028(2) 0.015(2) 0.0073(19) 0.017(2) C29 0.029(2) 0.026(2) 0.026(2) 0.0076(17) 0.0087(18) 0.0113(18) C30 0.035(2) 0.025(2) 0.026(2) 0.0083(17) 0.0116(19) 0.0025(18) C31 0.032(2) 0.030(2) 0.032(2) 0.0124(19) 0.0114(19) 0.0052(19) C32 0.042(3) 0.037(3) 0.035(3) 0.016(2) 0.020(2) 0.012(2) C33 0.048(3) 0.038(3) 0.028(2) 0.014(2) 0.015(2) 0.008(2) C34 0.035(2) 0.038(3) 0.031(2) 0.017(2) 0.007(2) 0.006(2) C35 0.032(2) 0.027(2) 0.029(2) 0.0118(18) 0.0100(19) 0.0049(18) C36 0.032(2) 0.029(2) 0.034(2) 0.0116(19) 0.010(2) 0.0076(19) C37 0.028(2) 0.036(2) 0.026(2) 0.0056(19) 0.0037(18) -0.0018(19) C38 0.039(3) 0.050(3) 0.045(3) 0.018(2) 0.009(2) -0.005(2) C39 0.038(3) 0.065(3) 0.024(2) 0.005(2) 0.013(2) 0.005(2) C40 0.037(3) 0.041(3) 0.053(3) 0.021(2) 0.011(2) 0.006(2) C41 0.036(3) 0.094(5) 0.040(3) 0.027(3) -0.003(2) 0.006(3) C42 0.030(2) 0.039(3) 0.037(3) 0.016(2) 0.013(2) 0.008(2) C43 0.034(3) 0.059(3) 0.054(3) 0.026(3) 0.017(2) 0.012(2) C44 0.033(3) 0.048(3) 0.055(3) 0.007(3) 0.008(2) -0.003(2) C45 0.034(3) 0.048(3) 0.044(3) 0.021(2) 0.011(2) 0.010(2) C46 0.066(4) 0.071(4) 0.031(3) 0.020(3) 0.021(3) 0.017(3) C47 0.0508(17) 0.071(2) 0.0460(16) 0.0001(14) 0.0136(14) 0.0242(15) C48 0.0508(17) 0.071(2) 0.0460(16) 0.0001(14) 0.0136(14) 0.0242(15) C49 0.0508(17) 0.071(2) 0.0460(16) 0.0001(14) 0.0136(14) 0.0242(15) C50 0.0508(17) 0.071(2) 0.0460(16) 0.0001(14) 0.0136(14) 0.0242(15) C51 0.101(3) 0.0430(17) 0.077(2) 0.0182(17) 0.039(2) 0.0258(18) C52 0.101(3) 0.0430(17) 0.077(2) 0.0182(17) 0.039(2) 0.0258(18) C53 0.101(3) 0.0430(17) 0.077(2) 0.0182(17) 0.039(2) 0.0258(18) C54 0.101(3) 0.0430(17) 0.077(2) 0.0182(17) 0.039(2) 0.0258(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 Yb1 O1 2.068(3) . ? Yb1 O3 2.070(3) . ? Yb1 O2 2.193(3) . ? Yb1 O5 2.353(3) . ? Yb1 O4 2.356(3) . ? Yb1 O6 2.362(3) . ? Yb1 H4A 2.45(5) . ? O1 C1 1.347(5) . ? O2 C7 1.360(5) . ? O3 C24 1.345(5) . ? O4 C30 1.394(5) . ? O4 H4A 0.81(2) . ? O5 C47 1.450(6) . ? O5 C50 1.454(6) . ? O6 C51 1.451(7) . ? O6 C54 1.472(7) . ? C1 C6 1.409(6) . ? C1 C2 1.413(6) . ? C2 C3 1.407(6) . ? C2 C14 1.531(6) . ? C3 C4 1.383(7) . ? C3 H3 0.9400 . ? C4 C5 1.378(7) . ? C4 C18 1.518(7) . ? C5 C6 1.391(6) . ? C5 H5 0.9400 . ? C6 C13 1.509(6) . ? C7 C12 1.404(6) . ? C7 C8 1.419(6) . ? C8 C9 1.391(6) . ? C8 C19 1.537(6) . ? C9 C10 1.395(7) . ? C9 H9 0.9400 . ? C10 C11 1.367(7) . ? C10 C23 1.516(6) . ? C11 C12 1.389(6) . ? C11 H11 0.9400 . ? C12 C13 1.520(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C16 1.527(7) . ? C14 C15 1.536(7) . ? C14 C17 1.543(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.532(7) . ? C19 C22 1.533(7) . ? C19 C21 1.540(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C29 1.413(6) . ? C24 C25 1.413(6) . ? C25 C26 1.400(6) . ? C25 C37 1.534(6) . ? C26 C27 1.386(7) . ? C26 H26 0.9400 . ? C27 C28 1.384(7) . ? C27 C41 1.510(7) . ? C28 C29 1.389(6) . ? C28 H28 0.9400 . ? C29 C36 1.511(6) . ? C30 C35 1.389(6) . ? C30 C31 1.407(6) . ? C31 C32 1.387(6) . ? C31 C42 1.554(6) . ? C32 C33 1.395(7) . ? C32 H32 0.9400 . ? C33 C34 1.378(7) . ? C33 C46 1.514(6) . ? C34 C35 1.393(6) . ? C34 H34 0.9400 . ? C35 C36 1.525(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.531(6) . ? C37 C39 1.532(6) . ? C37 C40 1.534(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 C43 1.532(7) . ? C42 C45 1.535(7) . ? C42 C44 1.538(7) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C46 H46C 0.9700 . ? C47 C48 1.469(7) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 C49 1.484(7) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.490(8) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.500(9) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 C53 1.465(9) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.490(8) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C55 1.477(13) 2_656 ? C55 C56 1.486(11) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 C57 1.493(13) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C57 H57C 0.9700 . ? C58 C63 0.63(9) 2_667 ? C58 C59 1.53(2) . ? C59 C62 0.73(9) 2_667 ? C59 C63 0.99(8) 2_667 ? C59 C60 1.51(2) . ? C59 C61 1.63(9) 2_667 ? C60 C61 0.77(9) 2_667 ? C60 C62 1.50(8) 2_667 ? C60 C61 1.533(19) . ? C60 C63 1.85(8) 2_667 ? C61 C60 0.77(9) 2_667 ? C61 C61 1.13(11) 2_667 ? C61 C62 1.52(2) . ? C61 C59 1.63(9) 2_667 ? C61 C62 1.92(9) 2_667 ? C62 C59 0.73(9) 2_667 ? C62 C60 1.50(8) 2_667 ? C62 C63 1.53(2) . ? C62 C61 1.92(9) 2_667 ? C63 C58 0.63(9) 2_667 ? C63 C59 0.99(8) 2_667 ? C63 C60 1.85(8) 2_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O3 120.33(12) . . ? O1 Yb1 O2 99.84(11) . . ? O3 Yb1 O2 135.97(11) . . ? O1 Yb1 O5 85.97(11) . . ? O3 Yb1 O5 81.54(11) . . ? O2 Yb1 O5 84.29(11) . . ? O1 Yb1 O4 142.26(11) . . ? O3 Yb1 O4 89.87(11) . . ? O2 Yb1 O4 64.13(10) . . ? O5 Yb1 O4 123.12(11) . . ? O1 Yb1 O6 84.10(11) . . ? O3 Yb1 O6 83.11(12) . . ? O2 Yb1 O6 120.80(12) . . ? O5 Yb1 O6 154.25(12) . . ? O4 Yb1 O6 77.26(11) . . ? O1 Yb1 H4A 135.3(11) . . ? O3 Yb1 H4A 103.4(10) . . ? O2 Yb1 H4A 45.1(6) . . ? O5 Yb1 H4A 111.0(10) . . ? O4 Yb1 H4A 19.2(5) . . ? O6 Yb1 H4A 92.6(9) . . ? C1 O1 Yb1 154.7(3) . . ? C7 O2 Yb1 136.8(3) . . ? C24 O3 Yb1 159.8(3) . . ? C30 O4 Yb1 145.3(3) . . ? C30 O4 H4A 118(4) . . ? Yb1 O4 H4A 87(4) . . ? C47 O5 C50 109.0(4) . . ? C47 O5 Yb1 128.5(3) . . ? C50 O5 Yb1 122.5(3) . . ? C51 O6 C54 109.0(4) . . ? C51 O6 Yb1 128.5(3) . . ? C54 O6 Yb1 122.3(3) . . ? O1 C1 C6 118.5(4) . . ? O1 C1 C2 121.4(4) . . ? C6 C1 C2 120.1(4) . . ? C3 C2 C1 117.0(4) . . ? C3 C2 C14 120.6(4) . . ? C1 C2 C14 122.4(4) . . ? C4 C3 C2 123.5(5) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C5 C4 C3 118.1(4) . . ? C5 C4 C18 121.4(5) . . ? C3 C4 C18 120.5(5) . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.8(4) . . ? C5 C6 C13 119.4(4) . . ? C1 C6 C13 120.8(4) . . ? O2 C7 C12 118.7(4) . . ? O2 C7 C8 121.0(4) . . ? C12 C7 C8 120.3(4) . . ? C9 C8 C7 116.8(4) . . ? C9 C8 C19 121.0(4) . . ? C7 C8 C19 122.2(4) . . ? C8 C9 C10 123.4(4) . . ? C8 C9 H9 118.3 . . ? C10 C9 H9 118.3 . . ? C11 C10 C9 117.8(4) . . ? C11 C10 C23 121.9(5) . . ? C9 C10 C23 120.3(5) . . ? C10 C11 C12 122.1(4) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C7 119.1(4) . . ? C11 C12 C13 118.8(4) . . ? C7 C12 C13 121.9(4) . . ? C6 C13 C12 116.1(4) . . ? C6 C13 H13A 108.3 . . ? C12 C13 H13A 108.3 . . ? C6 C13 H13B 108.3 . . ? C12 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C16 C14 C2 110.7(4) . . ? C16 C14 C15 107.2(4) . . ? C2 C14 C15 112.6(4) . . ? C16 C14 C17 109.4(4) . . ? C2 C14 C17 109.9(4) . . ? C15 C14 C17 106.9(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 106.9(4) . . ? C20 C19 C8 112.4(4) . . ? C22 C19 C8 111.0(4) . . ? C20 C19 C21 106.4(4) . . ? C22 C19 C21 109.7(5) . . ? C8 C19 C21 110.3(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 C29 118.2(4) . . ? O3 C24 C25 121.5(4) . . ? C29 C24 C25 120.3(4) . . ? C26 C25 C24 117.2(4) . . ? C26 C25 C37 121.2(4) . . ? C24 C25 C37 121.6(4) . . ? C27 C26 C25 123.6(4) . . ? C27 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C28 C27 C26 117.5(4) . . ? C28 C27 C41 120.9(5) . . ? C26 C27 C41 121.6(5) . . ? C27 C28 C29 122.1(4) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C28 C29 C24 119.2(4) . . ? C28 C29 C36 120.1(4) . . ? C24 C29 C36 120.6(4) . . ? C35 C30 O4 117.5(4) . . ? C35 C30 C31 122.6(4) . . ? O4 C30 C31 119.8(4) . . ? C32 C31 C30 116.3(4) . . ? C32 C31 C42 120.7(4) . . ? C30 C31 C42 123.0(4) . . ? C31 C32 C33 122.9(4) . . ? C31 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C34 C33 C32 118.4(4) . . ? C34 C33 C46 120.9(5) . . ? C32 C33 C46 120.7(4) . . ? C33 C34 C35 121.5(4) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C30 C35 C34 118.1(4) . . ? C30 C35 C36 122.7(4) . . ? C34 C35 C36 119.0(4) . . ? C29 C36 C35 116.9(4) . . ? C29 C36 H36A 108.1 . . ? C35 C36 H36A 108.1 . . ? C29 C36 H36B 108.1 . . ? C35 C36 H36B 108.1 . . ? H36A C36 H36B 107.3 . . ? C38 C37 C39 106.4(4) . . ? C38 C37 C25 112.0(4) . . ? C39 C37 C25 111.4(4) . . ? C38 C37 C40 107.1(4) . . ? C39 C37 C40 108.9(4) . . ? C25 C37 C40 110.8(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 C41 H41A 109.5 . . ? C27 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C27 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C45 107.2(4) . . ? C43 C42 C44 107.0(4) . . ? C45 C42 C44 109.3(4) . . ? C43 C42 C31 111.3(4) . . ? C45 C42 C31 110.2(4) . . ? C44 C42 C31 111.7(4) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C33 C46 H46A 109.5 . . ? C33 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C33 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 106.6(4) . . ? O5 C47 H47A 110.4 . . ? C48 C47 H47A 110.4 . . ? O5 C47 H47B 110.4 . . ? C48 C47 H47B 110.4 . . ? H47A C47 H47B 108.6 . . ? C47 C48 C49 108.2(5) . . ? C47 C48 H48A 110.1 . . ? C49 C48 H48A 110.1 . . ? C47 C48 H48B 110.1 . . ? C49 C48 H48B 110.1 . . ? H48A C48 H48B 108.4 . . ? C48 C49 C50 105.8(5) . . ? C48 C49 H49A 110.6 . . ? C50 C49 H49A 110.6 . . ? C48 C49 H49B 110.6 . . ? C50 C49 H49B 110.6 . . ? H49A C49 H49B 108.7 . . ? O5 C50 C49 105.8(4) . . ? O5 C50 H50A 110.6 . . ? C49 C50 H50A 110.6 . . ? O5 C50 H50B 110.6 . . ? C49 C50 H50B 110.6 . . ? H50A C50 H50B 108.7 . . ? O6 C51 C52 103.6(6) . . ? O6 C51 H51A 111.0 . . ? C52 C51 H51A 111.0 . . ? O6 C51 H51B 111.0 . . ? C52 C51 H51B 111.0 . . ? H51A C51 H51B 109.0 . . ? C53 C52 C51 109.0(6) . . ? C53 C52 H52A 109.9 . . ? C51 C52 H52A 109.9 . . ? C53 C52 H52B 109.9 . . ? C51 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? C52 C53 C54 106.1(6) . . ? C52 C53 H53A 110.5 . . ? C54 C53 H53A 110.5 . . ? C52 C53 H53B 110.5 . . ? C54 C53 H53B 110.5 . . ? H53A C53 H53B 108.7 . . ? O6 C54 C53 106.5(5) . . ? O6 C54 H54A 110.4 . . ? C53 C54 H54A 110.4 . . ? O6 C54 H54B 110.4 . . ? C53 C54 H54B 110.4 . . ? H54A C54 H54B 108.6 . . ? C55 C55 C56 119.1(11) 2_656 . ? C55 C55 H55A 107.5 2_656 . ? C56 C55 H55A 107.5 . . ? C55 C55 H55B 107.5 2_656 . ? C56 C55 H55B 107.5 . . ? H55A C55 H55B 107.0 . . ? C55 C56 C57 114.6(9) . . ? C55 C56 H56A 108.6 . . ? C57 C56 H56A 108.6 . . ? C55 C56 H56B 108.6 . . ? C57 C56 H56B 108.6 . . ? H56A C56 H56B 107.6 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C63 C58 C59 24(10) 2_667 . ? C62 C59 C63 126(10) 2_667 2_667 ? C62 C59 C60 75(7) 2_667 . ? C63 C59 C60 93(6) 2_667 . ? C62 C59 C58 138(10) 2_667 . ? C63 C59 C58 15(7) 2_667 . ? C60 C59 C58 104(4) . . ? C62 C59 C61 68(6) 2_667 2_667 ? C63 C59 C61 119(7) 2_667 2_667 ? C60 C59 C61 28(3) . 2_667 ? C58 C59 C61 128(5) . 2_667 ? C61 C60 C62 77(6) 2_667 2_667 ? C61 C60 C59 85(7) 2_667 . ? C62 C60 C59 28(3) 2_667 . ? C61 C60 C61 45(8) 2_667 . ? C62 C60 C61 78(4) 2_667 . ? C59 C60 C61 103(4) . . ? C61 C60 C63 115(8) 2_667 2_667 ? C62 C60 C63 53(3) 2_667 2_667 ? C59 C60 C63 32(3) . 2_667 ? C61 C60 C63 132(4) . 2_667 ? C60 C61 C61 106(10) 2_667 2_667 ? C60 C61 C62 74(6) 2_667 . ? C61 C61 C62 92(6) 2_667 . ? C60 C61 C60 135(8) 2_667 . ? C61 C61 C60 29(5) 2_667 . ? C62 C61 C60 99(3) . . ? C60 C61 C59 67(6) 2_667 2_667 ? C61 C61 C59 118(7) 2_667 2_667 ? C62 C61 C59 27(4) . 2_667 ? C60 C61 C59 123(4) . 2_667 ? C60 C61 C62 112(8) 2_667 2_667 ? C61 C61 C62 52(4) 2_667 2_667 ? C62 C61 C62 144(4) . 2_667 ? C60 C61 C62 50(3) . 2_667 ? C59 C61 C62 170(5) 2_667 2_667 ? C59 C62 C60 77(6) 2_667 2_667 ? C59 C62 C61 86(8) 2_667 . ? C60 C62 C61 29(4) 2_667 . ? C59 C62 C63 32(7) 2_667 . ? C60 C62 C63 75(4) 2_667 . ? C61 C62 C63 97(4) . . ? C59 C62 C61 122(9) 2_667 2_667 ? C60 C62 C61 52(3) 2_667 2_667 ? C61 C62 C61 36(4) . 2_667 ? C63 C62 C61 127(5) . 2_667 ? C58 C63 C59 140(10) 2_667 2_667 ? C58 C63 C62 157(10) 2_667 . ? C59 C63 C62 23(6) 2_667 . ? C58 C63 C60 146(10) 2_667 2_667 ? C59 C63 C60 55(4) 2_667 2_667 ? C62 C63 C60 52(3) . 2_667 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.697 _refine_diff_density_min -2.301 _refine_diff_density_rms 0.101 #============================================================end data_complex7 _database_code_depnum_ccdc_archive 'CCDC 682657' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H76 O6 Yb, C35 H56 O6 Yb, 2(C4 H8 O), 0.5(C6 H14)' _chemical_formula_sum 'C100 H155 O14 Yb2' _chemical_formula_weight 1927.32 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' Yb Yb -0.3850 5.5486 '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' _symmetry_Int_Tables_number 14 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 22.2232(16) _cell_length_b 22.7689(17) _cell_length_c 19.3062(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.006(2) _cell_angle_gamma 90.00 _cell_volume 9768.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 33257 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4028 _exptl_absorpt_coefficient_mu 1.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 0.716 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95001 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 17827 _reflns_number_gt 14297 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0280P)^2^+44.4941P] 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 17827 _refine_ls_number_parameters 1064 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.164 _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 Yb1 Yb 0.779331(14) 0.701511(14) 0.081513(16) 0.02850(10) Uani 1 1 d . . . Yb2 Yb 0.766155(15) 0.343157(15) 0.073405(19) 0.03737(11) Uani 1 1 d . . . O1 O 0.7339(2) 0.6424(2) 0.0147(3) 0.0342(12) Uani 1 1 d . . . O2 O 0.8631(2) 0.7000(2) 0.0255(2) 0.0343(12) Uani 1 1 d . . . O3 O 0.8115(2) 0.6418(2) 0.1563(3) 0.0389(13) Uani 1 1 d . . . O4 O 0.6964(2) 0.7200(2) 0.1333(3) 0.0359(12) Uani 1 1 d . . . O5 O 0.8134(2) 0.7778(2) 0.1595(3) 0.0385(13) Uani 1 1 d . . . O6 O 0.7591(2) 0.7756(2) -0.0041(3) 0.0390(13) Uani 1 1 d . . . O7 O 0.8078(2) 0.2714(2) 0.1142(3) 0.0404(13) Uani 1 1 d . . . O8 O 0.7275(2) 0.3098(2) -0.0149(3) 0.0408(13) Uani 1 1 d . . . O9 O 0.6806(3) 0.3258(3) 0.1343(3) 0.0558(16) Uani 1 1 d . . . O10 O 0.8500(2) 0.3786(2) 0.0213(3) 0.0417(13) Uani 1 1 d . . . O11 O 0.7318(3) 0.4401(2) 0.0549(3) 0.0517(15) Uani 1 1 d . . . O12 O 0.7953(3) 0.4091(3) 0.1647(3) 0.0617(18) Uani 1 1 d . . . O13 O 0.5720(6) 0.4815(5) 0.2267(8) 0.148(4) Uani 1 1 d . . . O14 O 0.6233(10) 0.1293(10) 0.1160(13) 0.282(9) Uiso 1 1 d D . . C1 C 0.7310(3) 0.6070(3) -0.0408(4) 0.0314(17) Uani 1 1 d . . . C2 C 0.6747(3) 0.5986(3) -0.0756(4) 0.0319(17) Uani 1 1 d . . . C3 C 0.6755(4) 0.5626(3) -0.1341(4) 0.0376(19) Uani 1 1 d . . . H3 H 0.6391 0.5580 -0.1594 0.045 Uiso 1 1 calc R . . C4 C 0.7258(4) 0.5335(3) -0.1572(4) 0.0375(19) Uani 1 1 d . . . C5 C 0.7793(3) 0.5413(3) -0.1208(4) 0.0374(19) Uani 1 1 d . . . H5 H 0.8147 0.5220 -0.1362 0.045 Uiso 1 1 calc R . . C6 C 0.7820(3) 0.5767(3) -0.0627(4) 0.0328(17) Uani 1 1 d . . . C7 C 0.8962(3) 0.6811(3) -0.0272(4) 0.0321(18) Uani 1 1 d . . . C8 C 0.9430(3) 0.7162(3) -0.0570(4) 0.0348(18) Uani 1 1 d . . . C9 C 0.9729(3) 0.6957(4) -0.1155(4) 0.043(2) Uani 1 1 d . . . H9 H 1.0020 0.7204 -0.1369 0.051 Uiso 1 1 calc R . . C10 C 0.9620(3) 0.6404(4) -0.1439(4) 0.046(2) Uani 1 1 d . . . C11 C 0.9189(3) 0.6057(4) -0.1119(4) 0.0389(19) Uani 1 1 d . . . H11 H 0.9115 0.5675 -0.1298 0.047 Uiso 1 1 calc R . . C12 C 0.8867(3) 0.6243(3) -0.0553(4) 0.0337(18) Uani 1 1 d . . . C13 C 0.8413(3) 0.5829(3) -0.0235(4) 0.0333(17) Uani 1 1 d . . . H13A H 0.8324 0.5966 0.0241 0.040 Uiso 1 1 calc R . . H13B H 0.8600 0.5435 -0.0197 0.040 Uiso 1 1 calc R . . C14 C 0.6163(3) 0.6271(4) -0.0509(4) 0.040(2) Uani 1 1 d . . . C15 C 0.5618(4) 0.6083(4) -0.0934(5) 0.057(3) Uani 1 1 d . . . H15A H 0.5673 0.6203 -0.1417 0.086 Uiso 1 1 calc R . . H15B H 0.5255 0.6269 -0.0747 0.086 Uiso 1 1 calc R . . H15C H 0.5575 0.5655 -0.0911 0.086 Uiso 1 1 calc R . . C16 C 0.6206(4) 0.6944(4) -0.0570(5) 0.052(2) Uani 1 1 d . . . H16A H 0.6539 0.7087 -0.0283 0.078 Uiso 1 1 calc R . . H16B H 0.5829 0.7122 -0.0412 0.078 Uiso 1 1 calc R . . H16C H 0.6279 0.7052 -0.1054 0.078 Uiso 1 1 calc R . . C17 C 0.6036(4) 0.6115(4) 0.0252(4) 0.046(2) Uani 1 1 d . . . H17A H 0.5990 0.5689 0.0298 0.069 Uiso 1 1 calc R . . H17B H 0.5665 0.6310 0.0403 0.069 Uiso 1 1 calc R . . H17C H 0.6372 0.6248 0.0541 0.069 Uiso 1 1 calc R . . C18 C 0.7233(4) 0.4948(4) -0.2214(4) 0.057(3) Uani 1 1 d . . . H18A H 0.6824 0.4795 -0.2273 0.085 Uiso 1 1 calc R . . H18B H 0.7515 0.4620 -0.2161 0.085 Uiso 1 1 calc R . . H18C H 0.7345 0.5180 -0.2622 0.085 Uiso 1 1 calc R . . C19 C 0.9615(4) 0.7752(4) -0.0250(4) 0.044(2) Uani 1 1 d . . . C20 C 1.0154(4) 0.8036(4) -0.0616(5) 0.056(2) Uani 1 1 d . . . H20A H 1.0504 0.7775 -0.0582 0.084 Uiso 1 1 calc R . . H20B H 1.0247 0.8412 -0.0395 0.084 Uiso 1 1 calc R . . H20C H 1.0056 0.8101 -0.1105 0.084 Uiso 1 1 calc R . . C21 C 0.9793(4) 0.7659(4) 0.0510(4) 0.055(2) Uani 1 1 d . . . H21A H 0.9475 0.7441 0.0749 0.083 Uiso 1 1 calc R . . H21B H 0.9850 0.8041 0.0734 0.083 Uiso 1 1 calc R . . H21C H 1.0170 0.7435 0.0531 0.083 Uiso 1 1 calc R . . C22 C 0.9093(4) 0.8190(4) -0.0290(5) 0.049(2) Uani 1 1 d . . . H22A H 0.8988 0.8259 -0.0776 0.074 Uiso 1 1 calc R . . H22B H 0.9214 0.8561 -0.0074 0.074 Uiso 1 1 calc R . . H22C H 0.8744 0.8030 -0.0044 0.074 Uiso 1 1 calc R . . C23 C 0.9957(4) 0.6204(5) -0.2084(5) 0.066(3) Uani 1 1 d . . . H23A H 0.9849 0.5796 -0.2189 0.099 Uiso 1 1 calc R . . H23B H 1.0391 0.6230 -0.2001 0.099 Uiso 1 1 calc R . . H23C H 0.9848 0.6456 -0.2475 0.099 Uiso 1 1 calc R . . C24 C 0.8067(3) 0.6105(3) 0.2145(4) 0.0305(17) Uani 1 1 d . . . C25 C 0.8593(3) 0.5939(3) 0.2524(4) 0.0321(17) Uani 1 1 d . . . C26 C 0.8508(4) 0.5629(3) 0.3137(4) 0.0378(19) Uani 1 1 d . . . H26 H 0.8852 0.5532 0.3407 0.045 Uiso 1 1 calc R . . C27 C 0.7951(4) 0.5455(3) 0.3373(4) 0.042(2) Uani 1 1 d . . . C28 C 0.7451(4) 0.5590(3) 0.2968(4) 0.0386(19) Uani 1 1 d . . . H28 H 0.7065 0.5457 0.3111 0.046 Uiso 1 1 calc R . . C29 C 0.7499(3) 0.5915(3) 0.2360(4) 0.0317(17) Uani 1 1 d . . . C30 C 0.6558(3) 0.7101(4) 0.1833(4) 0.0356(19) Uani 1 1 d . . . C31 C 0.6131(3) 0.7540(4) 0.2028(4) 0.0363(18) Uani 1 1 d . . . C32 C 0.5753(3) 0.7417(4) 0.2583(4) 0.042(2) Uani 1 1 d . . . H32 H 0.5474 0.7710 0.2722 0.050 Uiso 1 1 calc R . . C33 C 0.5758(3) 0.6898(4) 0.2943(4) 0.043(2) Uani 1 1 d . . . C34 C 0.6155(3) 0.6466(4) 0.2721(4) 0.041(2) Uani 1 1 d . . . H34 H 0.6154 0.6097 0.2951 0.049 Uiso 1 1 calc R . . C35 C 0.6551(3) 0.6553(3) 0.2175(4) 0.0322(17) Uani 1 1 d . . . C36 C 0.6941(3) 0.6045(3) 0.1947(4) 0.0346(18) Uani 1 1 d . . . H36A H 0.6688 0.5687 0.1947 0.042 Uiso 1 1 calc R . . H36B H 0.7064 0.6118 0.1462 0.042 Uiso 1 1 calc R . . C37 C 0.9229(4) 0.6095(4) 0.2275(4) 0.042(2) Uani 1 1 d . . . C38 C 0.9725(4) 0.5829(4) 0.2726(5) 0.061(3) Uani 1 1 d . . . H38A H 0.9688 0.5978 0.3200 0.092 Uiso 1 1 calc R . . H38B H 1.0119 0.5938 0.2538 0.092 Uiso 1 1 calc R . . H38C H 0.9686 0.5400 0.2728 0.092 Uiso 1 1 calc R . . C39 C 0.9322(4) 0.6761(4) 0.2251(5) 0.061(3) Uani 1 1 d . . . H39A H 0.9026 0.6937 0.1937 0.091 Uiso 1 1 calc R . . H39B H 0.9729 0.6847 0.2084 0.091 Uiso 1 1 calc R . . H39C H 0.9271 0.6925 0.2717 0.091 Uiso 1 1 calc R . . C40 C 0.9326(4) 0.5835(5) 0.1541(5) 0.067(3) Uani 1 1 d . . . H40A H 0.9276 0.5407 0.1558 0.100 Uiso 1 1 calc R . . H40B H 0.9733 0.5929 0.1381 0.100 Uiso 1 1 calc R . . H40C H 0.9031 0.6003 0.1221 0.100 Uiso 1 1 calc R . . C41 C 0.7890(4) 0.5129(4) 0.4057(5) 0.061(3) Uani 1 1 d . . . H41A H 0.7464 0.5106 0.4185 0.091 Uiso 1 1 calc R . . H41B H 0.8112 0.5340 0.4418 0.091 Uiso 1 1 calc R . . H41C H 0.8054 0.4732 0.4007 0.091 Uiso 1 1 calc R . . C42 C 0.6093(4) 0.8125(4) 0.1646(4) 0.045(2) Uani 1 1 d . . . C43 C 0.5550(4) 0.8500(4) 0.1895(5) 0.062(3) Uani 1 1 d . . . H43A H 0.5178 0.8275 0.1837 0.093 Uiso 1 1 calc R . . H43B H 0.5528 0.8861 0.1619 0.093 Uiso 1 1 calc R . . H43C H 0.5604 0.8600 0.2384 0.093 Uiso 1 1 calc R . . C44 C 0.5995(4) 0.8015(4) 0.0865(4) 0.050(2) Uani 1 1 d . . . H44A H 0.6342 0.7802 0.0676 0.075 Uiso 1 1 calc R . . H44B H 0.5953 0.8392 0.0625 0.075 Uiso 1 1 calc R . . H44C H 0.5630 0.7781 0.0798 0.075 Uiso 1 1 calc R . . C45 C 0.6659(4) 0.8489(4) 0.1762(5) 0.052(2) Uani 1 1 d . . . H45A H 0.6703 0.8574 0.2257 0.079 Uiso 1 1 calc R . . H45B H 0.6627 0.8859 0.1504 0.079 Uiso 1 1 calc R . . H45C H 0.7011 0.8269 0.1600 0.079 Uiso 1 1 calc R . . C46 C 0.5339(4) 0.6780(4) 0.3556(5) 0.057(3) Uani 1 1 d . . . H46A H 0.5213 0.7154 0.3760 0.085 Uiso 1 1 calc R . . H46B H 0.5552 0.6546 0.3905 0.085 Uiso 1 1 calc R . . H46C H 0.4984 0.6564 0.3396 0.085 Uiso 1 1 calc R . . C47 C 0.8486(5) 0.8306(4) 0.1536(5) 0.062(3) Uani 1 1 d . . . H47A H 0.8389 0.8514 0.1100 0.075 Uiso 1 1 calc R . . H47B H 0.8921 0.8212 0.1538 0.075 Uiso 1 1 calc R . . C48 C 0.8329(5) 0.8670(5) 0.2139(5) 0.074(3) Uani 1 1 d . . . H48A H 0.7967 0.8911 0.2044 0.089 Uiso 1 1 calc R . . H48B H 0.8666 0.8933 0.2267 0.089 Uiso 1 1 calc R . . C49 C 0.8208(5) 0.8225(4) 0.2702(5) 0.071(3) Uani 1 1 d . . . H49A H 0.8583 0.8126 0.2953 0.085 Uiso 1 1 calc R . . H49B H 0.7910 0.8377 0.3038 0.085 Uiso 1 1 calc R . . C50 C 0.7969(4) 0.7703(4) 0.2330(4) 0.050(2) Uani 1 1 d . . . H50A H 0.8148 0.7338 0.2518 0.060 Uiso 1 1 calc R . . H50B H 0.7526 0.7680 0.2381 0.060 Uiso 1 1 calc R . . C51 C 0.7386(4) 0.8352(3) -0.0031(4) 0.043(2) Uani 1 1 d . . . H51A H 0.7730 0.8629 -0.0043 0.052 Uiso 1 1 calc R . . H51B H 0.7143 0.8431 0.0388 0.052 Uiso 1 1 calc R . . C52 C 0.7013(4) 0.8406(4) -0.0670(4) 0.051(2) Uani 1 1 d . . . H52A H 0.6974 0.8821 -0.0816 0.061 Uiso 1 1 calc R . . H52B H 0.6606 0.8239 -0.0597 0.061 Uiso 1 1 calc R . . C53 C 0.7365(4) 0.8049(4) -0.1201(4) 0.053(2) Uani 1 1 d . . . H53A H 0.7093 0.7877 -0.1552 0.064 Uiso 1 1 calc R . . H53B H 0.7668 0.8297 -0.1438 0.064 Uiso 1 1 calc R . . C54 C 0.7665(4) 0.7573(4) -0.0776(4) 0.0395(19) Uani 1 1 d . . . H54A H 0.7470 0.7189 -0.0859 0.047 Uiso 1 1 calc R . . H54B H 0.8097 0.7542 -0.0897 0.047 Uiso 1 1 calc R . . C55 C 0.8196(4) 0.2125(3) 0.1147(4) 0.041(2) Uani 1 1 d . . . C56 C 0.8305(4) 0.1826(4) 0.1776(4) 0.042(2) Uani 1 1 d . . . C57 C 0.8389(4) 0.1216(4) 0.1729(5) 0.053(2) Uani 1 1 d . . . H57 H 0.8455 0.1004 0.2146 0.063 Uiso 1 1 calc R . . C58 C 0.8380(4) 0.0905(4) 0.1120(5) 0.053(2) Uani 1 1 d . . . C59 C 0.8297(4) 0.1221(4) 0.0522(4) 0.044(2) Uani 1 1 d . . . H59 H 0.8308 0.1018 0.0093 0.053 Uiso 1 1 calc R . . C60 C 0.8200(3) 0.1821(4) 0.0513(4) 0.0379(19) Uani 1 1 d . . . C61 C 0.7096(4) 0.2599(4) -0.0471(4) 0.0396(19) Uani 1 1 d . . . C62 C 0.6528(4) 0.2559(4) -0.0806(5) 0.047(2) Uani 1 1 d . . . C63 C 0.6365(4) 0.2023(4) -0.1081(5) 0.059(3) Uani 1 1 d . . . H63 H 0.5980 0.1987 -0.1289 0.071 Uiso 1 1 calc R . . C64 C 0.6743(5) 0.1528(4) -0.1068(5) 0.063(3) Uani 1 1 d . . . C65 C 0.7297(5) 0.1593(4) -0.0763(5) 0.055(2) Uani 1 1 d . . . H65 H 0.7559 0.1263 -0.0755 0.067 Uiso 1 1 calc R . . C66 C 0.7495(4) 0.2111(4) -0.0467(4) 0.042(2) Uani 1 1 d . . . C67 C 0.8124(3) 0.2141(3) -0.0168(4) 0.0367(19) Uani 1 1 d . . . H67A H 0.8234 0.2559 -0.0101 0.044 Uiso 1 1 calc R . . H67B H 0.8409 0.1973 -0.0509 0.044 Uiso 1 1 calc R . . C68 C 0.8339(4) 0.2157(4) 0.2476(4) 0.049(2) Uani 1 1 d . . . C69 C 0.8488(6) 0.1743(5) 0.3072(5) 0.082(4) Uani 1 1 d . . . H69A H 0.8177 0.1440 0.3107 0.123 Uiso 1 1 calc R . . H69B H 0.8505 0.1966 0.3506 0.123 Uiso 1 1 calc R . . H69C H 0.8879 0.1557 0.2987 0.123 Uiso 1 1 calc R . . C70 C 0.7732(4) 0.2433(4) 0.2634(4) 0.059(3) Uani 1 1 d . . . H70A H 0.7631 0.2719 0.2273 0.089 Uiso 1 1 calc R . . H70B H 0.7749 0.2631 0.3084 0.089 Uiso 1 1 calc R . . H70C H 0.7423 0.2126 0.2648 0.089 Uiso 1 1 calc R . . C71 C 0.8843(4) 0.2610(4) 0.2441(5) 0.059(3) Uani 1 1 d . . . H71A H 0.9231 0.2408 0.2405 0.088 Uiso 1 1 calc R . . H71B H 0.8837 0.2852 0.2861 0.088 Uiso 1 1 calc R . . H71C H 0.8785 0.2862 0.2035 0.088 Uiso 1 1 calc R . . C72 C 0.8458(5) 0.0249(4) 0.1121(6) 0.077(3) Uani 1 1 d . . . H72A H 0.8112 0.0066 0.1350 0.115 Uiso 1 1 calc R . . H72B H 0.8828 0.0147 0.1371 0.115 Uiso 1 1 calc R . . H72C H 0.8486 0.0107 0.0643 0.115 Uiso 1 1 calc R . . C73 C 0.6119(4) 0.3093(4) -0.0897(5) 0.054(2) Uani 1 1 d . . . C74 C 0.5548(4) 0.2952(5) -0.1308(6) 0.076(3) Uani 1 1 d . . . H74A H 0.5659 0.2799 -0.1765 0.115 Uiso 1 1 calc R . . H74B H 0.5309 0.3310 -0.1364 0.115 Uiso 1 1 calc R . . H74C H 0.5312 0.2657 -0.1059 0.115 Uiso 1 1 calc R . . C75 C 0.6458(4) 0.3564(4) -0.1322(5) 0.062(3) Uani 1 1 d . . . H75A H 0.6835 0.3665 -0.1088 0.093 Uiso 1 1 calc R . . H75B H 0.6207 0.3916 -0.1363 0.093 Uiso 1 1 calc R . . H75C H 0.6546 0.3410 -0.1785 0.093 Uiso 1 1 calc R . . C76 C 0.5913(4) 0.3326(4) -0.0197(5) 0.063(3) Uani 1 1 d . . . H76A H 0.5659 0.3032 0.0030 0.094 Uiso 1 1 calc R . . H76B H 0.5683 0.3689 -0.0265 0.094 Uiso 1 1 calc R . . H76C H 0.6265 0.3408 0.0093 0.094 Uiso 1 1 calc R . . C77 C 0.6536(6) 0.0945(4) -0.1361(6) 0.098(5) Uani 1 1 d . . . H77A H 0.6876 0.0747 -0.1585 0.147 Uiso 1 1 calc R . . H77B H 0.6217 0.1012 -0.1703 0.147 Uiso 1 1 calc R . . H77C H 0.6381 0.0698 -0.0986 0.147 Uiso 1 1 calc R . . C78 C 0.6396(5) 0.3639(5) 0.1721(7) 0.088(4) Uani 1 1 d . . . H78A H 0.6260 0.3966 0.1422 0.105 Uiso 1 1 calc R . . H78B H 0.6598 0.3805 0.2134 0.105 Uiso 1 1 calc R . . C79 C 0.5882(5) 0.3272(6) 0.1928(7) 0.090(4) Uani 1 1 d . . . H79A H 0.5549 0.3304 0.1590 0.108 Uiso 1 1 calc R . . H79B H 0.5732 0.3386 0.2392 0.108 Uiso 1 1 calc R . . C80 C 0.6136(6) 0.2665(7) 0.1937(7) 0.108(5) Uani 1 1 d . . . H80A H 0.6342 0.2584 0.2382 0.130 Uiso 1 1 calc R . . H80B H 0.5815 0.2369 0.1868 0.130 Uiso 1 1 calc R . . C81 C 0.6565(4) 0.2657(4) 0.1359(5) 0.061(3) Uani 1 1 d . . . H81A H 0.6889 0.2367 0.1441 0.073 Uiso 1 1 calc R . . H81B H 0.6360 0.2560 0.0918 0.073 Uiso 1 1 calc R . . C82 C 0.8510(4) 0.4130(4) -0.0406(5) 0.050(2) Uani 1 1 d . . . H82A H 0.8323 0.4519 -0.0324 0.060 Uiso 1 1 calc R . . H82B H 0.8287 0.3929 -0.0781 0.060 Uiso 1 1 calc R . . C83 C 0.9157(4) 0.4198(5) -0.0595(6) 0.072(3) Uani 1 1 d . . . H83A H 0.9270 0.3911 -0.0957 0.087 Uiso 1 1 calc R . . H83B H 0.9235 0.4599 -0.0772 0.087 Uiso 1 1 calc R . . C84 C 0.9484(5) 0.4096(7) 0.0013(7) 0.113(6) Uani 1 1 d . . . H84A H 0.9547 0.4468 0.0269 0.135 Uiso 1 1 calc R . . H84B H 0.9882 0.3923 -0.0097 0.135 Uiso 1 1 calc R . . C85 C 0.9117(4) 0.3680(5) 0.0429(5) 0.064(3) Uani 1 1 d . . . H85A H 0.9235 0.3269 0.0332 0.076 Uiso 1 1 calc R . . H85B H 0.9166 0.3757 0.0930 0.076 Uiso 1 1 calc R . . C86 C 0.7468(5) 0.4857(4) 0.1044(6) 0.071(3) Uani 1 1 d . . . H86A H 0.7136 0.4906 0.1380 0.085 Uiso 1 1 calc R . . H86B H 0.7528 0.5235 0.0801 0.085 Uiso 1 1 calc R . . C87 C 0.8019(6) 0.4690(4) 0.1406(6) 0.080(3) Uani 1 1 d . . . H87A H 0.8368 0.4720 0.1089 0.096 Uiso 1 1 calc R . . H87B H 0.8089 0.4956 0.1803 0.096 Uiso 1 1 calc R . . C88 C 0.6873(4) 0.4581(4) 0.0070(6) 0.070(3) Uani 1 1 d . . . H88A H 0.6495 0.4656 0.0316 0.105 Uiso 1 1 calc R . . H88B H 0.6811 0.4270 -0.0274 0.105 Uiso 1 1 calc R . . H88C H 0.7005 0.4941 -0.0164 0.105 Uiso 1 1 calc R . . C89 C 0.8079(6) 0.4021(5) 0.2351(6) 0.100(4) Uani 1 1 d . . . H89A H 0.8497 0.4134 0.2442 0.149 Uiso 1 1 calc R . . H89B H 0.8020 0.3609 0.2482 0.149 Uiso 1 1 calc R . . H89C H 0.7808 0.4269 0.2624 0.149 Uiso 1 1 calc R . . C90 C 0.5528(7) 0.5014(8) 0.1674(8) 0.109(5) Uani 1 1 d . . . H90A H 0.5373 0.4684 0.1392 0.131 Uiso 1 1 calc R . . H90B H 0.5865 0.5198 0.1419 0.131 Uiso 1 1 calc R . . C91 C 0.5062(10) 0.5435(7) 0.1779(11) 0.146(8) Uani 1 1 d . . . H91A H 0.4763 0.5422 0.1399 0.175 Uiso 1 1 calc R . . H91B H 0.5228 0.5837 0.1814 0.175 Uiso 1 1 calc R . . C92 C 0.4796(8) 0.5250(10) 0.2430(12) 0.155(8) Uani 1 1 d . . . H92A H 0.4453 0.4981 0.2353 0.186 Uiso 1 1 calc R . . H92B H 0.4660 0.5591 0.2706 0.186 Uiso 1 1 calc R . . C93 C 0.5306(9) 0.4944(8) 0.2769(9) 0.128(6) Uani 1 1 d . . . H93A H 0.5488 0.5200 0.3127 0.153 Uiso 1 1 calc R . . H93B H 0.5164 0.4579 0.2995 0.153 Uiso 1 1 calc R . . C94 C 0.6807(12) 0.0984(14) 0.1136(19) 0.127(11) Uiso 0.50 1 d PD . . C94' C 0.6652(14) 0.1027(13) 0.1617(15) 0.111(10) Uiso 0.50 1 d PD . . C95 C 0.6747(18) 0.0363(16) 0.084(3) 0.175(18) Uiso 0.50 1 d PD . . C95' C 0.6576(18) 0.0475(15) 0.1188(17) 0.143(15) Uiso 0.50 1 d PD . . C96 C 0.6110(18) 0.0291(16) 0.053(2) 0.168(15) Uiso 0.50 1 d PD . . C96' C 0.662(2) 0.062(2) 0.0438(17) 0.151(14) Uiso 0.50 1 d PD . . C97 C 0.592(2) 0.093(2) 0.060(3) 0.28(3) Uiso 0.50 1 d PD . . C97' C 0.641(4) 0.125(3) 0.043(2) 0.37(5) Uiso 0.50 1 d PD . . C98 C 0.0242(5) 0.9837(5) 0.0176(6) 0.073(3) Uani 1 1 d . . . H98A H 0.0568 1.0119 0.0284 0.087 Uiso 1 1 calc R . . H98B H 0.0407 0.9549 -0.0157 0.087 Uiso 1 1 calc R . . C99 C 0.0092(5) 0.9518(5) 0.0823(6) 0.077(3) Uani 1 1 d . . . H99A H -0.0241 0.9242 0.0722 0.092 Uiso 1 1 calc R . . H99B H -0.0058 0.9806 0.1166 0.092 Uiso 1 1 calc R . . C100 C 0.0602(5) 0.9174(5) 0.1153(6) 0.082(3) Uani 1 1 d . . . H10A H 0.0763 0.8892 0.0817 0.123 Uiso 1 1 calc R . . H10B H 0.0450 0.8963 0.1559 0.123 Uiso 1 1 calc R . . H10C H 0.0921 0.9445 0.1296 0.123 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 Yb1 0.02979(18) 0.02875(18) 0.02694(18) -0.00046(14) 0.00264(13) -0.00225(14) Yb2 0.0361(2) 0.02731(19) 0.0487(2) -0.00358(16) 0.00778(16) -0.00080(15) O1 0.034(3) 0.033(3) 0.036(3) -0.006(2) 0.002(2) -0.001(2) O2 0.035(3) 0.034(3) 0.035(3) -0.001(2) 0.005(2) -0.002(2) O3 0.031(3) 0.045(3) 0.041(3) 0.005(3) 0.000(2) -0.001(2) O4 0.035(3) 0.033(3) 0.040(3) -0.003(2) 0.012(2) -0.001(2) O5 0.049(3) 0.034(3) 0.032(3) -0.006(2) 0.002(2) -0.010(3) O6 0.053(3) 0.032(3) 0.032(3) 0.005(2) -0.001(3) 0.007(3) O7 0.043(3) 0.031(3) 0.047(3) 0.003(2) 0.003(3) 0.002(2) O8 0.035(3) 0.036(3) 0.051(3) -0.003(3) 0.005(3) -0.002(2) O9 0.044(4) 0.053(4) 0.071(4) -0.003(3) 0.025(3) -0.007(3) O10 0.030(3) 0.037(3) 0.058(4) 0.010(3) 0.000(3) -0.001(2) O11 0.052(4) 0.028(3) 0.075(4) 0.001(3) 0.009(3) 0.011(3) O12 0.089(5) 0.039(4) 0.057(4) -0.019(3) 0.007(4) -0.009(3) O13 0.150(11) 0.150(11) 0.145(11) 0.045(9) 0.019(9) 0.053(8) C1 0.037(4) 0.026(4) 0.031(4) 0.003(3) 0.002(3) 0.000(3) C2 0.032(4) 0.031(4) 0.033(4) 0.004(3) 0.002(3) -0.004(3) C3 0.042(5) 0.031(4) 0.040(5) -0.010(4) -0.004(4) -0.009(4) C4 0.043(5) 0.035(5) 0.034(4) -0.010(3) 0.003(4) -0.005(4) C5 0.035(4) 0.032(4) 0.045(5) 0.000(4) 0.008(4) 0.004(3) C6 0.044(5) 0.023(4) 0.031(4) 0.001(3) 0.005(3) 0.006(3) C7 0.024(4) 0.047(5) 0.026(4) 0.013(3) 0.000(3) 0.007(3) C8 0.025(4) 0.039(5) 0.040(5) 0.010(4) 0.001(3) -0.002(3) C9 0.024(4) 0.060(6) 0.044(5) 0.015(4) 0.005(4) -0.002(4) C10 0.029(4) 0.072(7) 0.038(5) -0.005(4) 0.007(4) 0.002(4) C11 0.028(4) 0.045(5) 0.044(5) -0.010(4) -0.004(4) -0.001(4) C12 0.031(4) 0.038(5) 0.033(4) 0.004(3) 0.005(3) 0.004(3) C13 0.033(4) 0.029(4) 0.038(4) -0.001(3) 0.004(3) 0.007(3) C14 0.031(4) 0.050(5) 0.038(5) -0.006(4) -0.006(4) 0.003(4) C15 0.035(5) 0.074(7) 0.062(6) -0.012(5) -0.009(4) 0.003(5) C16 0.049(5) 0.046(6) 0.061(6) -0.001(4) -0.009(4) 0.011(4) C17 0.033(4) 0.062(6) 0.043(5) 0.008(4) -0.001(4) 0.004(4) C18 0.057(6) 0.063(6) 0.049(6) -0.015(5) -0.002(5) -0.017(5) C19 0.036(5) 0.047(5) 0.048(5) 0.004(4) 0.008(4) -0.010(4) C20 0.043(5) 0.053(6) 0.072(7) 0.008(5) 0.009(5) -0.018(4) C21 0.047(5) 0.064(6) 0.055(6) -0.001(5) 0.003(4) -0.018(5) C22 0.053(6) 0.038(5) 0.056(6) 0.002(4) 0.010(4) -0.008(4) C23 0.047(6) 0.101(9) 0.050(6) -0.019(6) 0.020(5) -0.012(6) C24 0.039(4) 0.025(4) 0.027(4) 0.008(3) 0.001(3) 0.006(3) C25 0.037(4) 0.028(4) 0.031(4) 0.000(3) 0.000(3) -0.001(3) C26 0.049(5) 0.030(4) 0.035(4) 0.004(4) -0.005(4) 0.002(4) C27 0.055(6) 0.023(4) 0.048(5) 0.007(4) 0.012(4) 0.012(4) C28 0.046(5) 0.020(4) 0.050(5) 0.002(4) 0.015(4) 0.001(4) C29 0.043(5) 0.021(4) 0.031(4) -0.003(3) 0.001(3) -0.005(3) C30 0.025(4) 0.049(5) 0.032(4) -0.012(4) -0.001(3) -0.001(4) C31 0.030(4) 0.043(5) 0.037(4) -0.007(4) 0.006(3) 0.003(4) C32 0.029(4) 0.052(6) 0.045(5) -0.009(4) 0.009(4) 0.009(4) C33 0.029(4) 0.062(6) 0.039(5) -0.005(4) 0.004(4) -0.006(4) C34 0.033(4) 0.045(5) 0.046(5) 0.000(4) -0.003(4) -0.012(4) C35 0.025(4) 0.034(4) 0.038(4) -0.007(3) -0.001(3) -0.005(3) C36 0.030(4) 0.038(5) 0.036(4) -0.010(3) 0.002(3) -0.007(3) C37 0.040(5) 0.048(5) 0.039(5) 0.007(4) -0.004(4) -0.003(4) C38 0.038(5) 0.077(7) 0.070(7) 0.023(5) -0.014(5) -0.002(5) C39 0.045(5) 0.057(6) 0.080(7) 0.021(5) -0.016(5) -0.021(5) C40 0.033(5) 0.106(9) 0.061(7) 0.006(6) 0.004(4) 0.002(5) C41 0.071(7) 0.060(6) 0.051(6) 0.028(5) 0.012(5) 0.007(5) C42 0.037(5) 0.053(6) 0.045(5) -0.003(4) 0.007(4) 0.008(4) C43 0.061(6) 0.065(7) 0.059(6) 0.008(5) 0.015(5) 0.018(5) C44 0.047(5) 0.053(6) 0.051(5) -0.005(4) 0.001(4) 0.006(4) C45 0.064(6) 0.041(5) 0.053(6) -0.008(4) 0.005(5) -0.004(5) C46 0.043(5) 0.076(7) 0.052(6) 0.004(5) 0.015(4) 0.003(5) C47 0.079(7) 0.050(6) 0.057(6) -0.011(5) 0.018(5) -0.027(5) C48 0.101(9) 0.055(7) 0.067(7) -0.012(5) -0.010(6) -0.024(6) C49 0.108(9) 0.058(7) 0.047(6) -0.014(5) -0.001(6) -0.017(6) C50 0.070(6) 0.047(5) 0.033(5) -0.004(4) -0.002(4) -0.017(5) C51 0.050(5) 0.026(5) 0.053(5) -0.001(4) 0.001(4) 0.008(4) C52 0.049(5) 0.048(6) 0.055(6) 0.013(4) -0.002(4) 0.012(4) C53 0.058(6) 0.054(6) 0.046(5) 0.008(4) 0.001(4) 0.021(5) C54 0.054(5) 0.038(5) 0.026(4) 0.002(3) 0.001(4) 0.008(4) C55 0.038(5) 0.029(5) 0.056(5) 0.013(4) 0.003(4) 0.003(4) C56 0.040(5) 0.043(5) 0.043(5) 0.010(4) 0.003(4) 0.000(4) C57 0.055(6) 0.047(6) 0.056(6) 0.027(5) 0.004(5) 0.009(4) C58 0.066(6) 0.038(5) 0.054(6) 0.007(4) 0.017(5) 0.013(4) C59 0.052(5) 0.037(5) 0.043(5) 0.001(4) 0.013(4) 0.008(4) C60 0.033(4) 0.041(5) 0.040(5) 0.000(4) 0.002(4) -0.001(4) C61 0.037(5) 0.036(5) 0.045(5) 0.002(4) 0.004(4) -0.003(4) C62 0.048(5) 0.036(5) 0.056(6) 0.002(4) -0.004(4) -0.009(4) C63 0.061(6) 0.051(6) 0.065(6) -0.001(5) -0.019(5) -0.006(5) C64 0.085(8) 0.040(6) 0.066(7) -0.005(5) -0.023(6) -0.009(5) C65 0.075(7) 0.033(5) 0.058(6) -0.007(4) -0.009(5) -0.002(5) C66 0.043(5) 0.037(5) 0.046(5) 0.004(4) 0.008(4) -0.003(4) C67 0.037(4) 0.032(4) 0.042(5) 0.000(4) 0.011(4) 0.005(3) C68 0.061(6) 0.046(5) 0.041(5) 0.009(4) 0.003(4) -0.002(5) C69 0.116(10) 0.086(8) 0.044(6) 0.009(6) -0.015(6) -0.002(7) C70 0.067(7) 0.074(7) 0.037(5) -0.008(5) 0.015(5) -0.003(5) C71 0.053(6) 0.070(7) 0.053(6) -0.003(5) -0.003(5) -0.005(5) C72 0.110(9) 0.040(6) 0.079(8) 0.017(5) 0.025(7) 0.023(6) C73 0.041(5) 0.055(6) 0.067(6) 0.007(5) -0.007(5) 0.004(4) C74 0.052(6) 0.081(8) 0.096(9) -0.004(7) -0.017(6) 0.005(6) C75 0.061(6) 0.059(7) 0.067(7) 0.009(5) 0.008(5) 0.012(5) C76 0.042(5) 0.069(7) 0.077(7) -0.001(6) 0.006(5) 0.015(5) C77 0.135(11) 0.045(7) 0.115(10) 0.004(6) -0.066(9) -0.020(7) C78 0.069(7) 0.088(9) 0.105(10) -0.025(7) 0.053(7) -0.009(6) C79 0.056(7) 0.115(11) 0.099(10) 0.020(8) 0.036(6) 0.013(7) C80 0.067(8) 0.130(13) 0.128(12) 0.018(10) 0.037(8) -0.019(8) C81 0.056(6) 0.049(6) 0.077(7) 0.002(5) 0.009(5) -0.013(5) C82 0.043(5) 0.049(6) 0.058(6) 0.018(4) 0.007(4) 0.005(4) C83 0.047(6) 0.093(9) 0.078(8) 0.032(6) 0.016(5) 0.005(6) C84 0.042(6) 0.192(16) 0.103(10) 0.073(10) 0.000(6) -0.035(8) C85 0.040(5) 0.084(8) 0.066(7) 0.016(6) 0.007(5) 0.004(5) C86 0.085(8) 0.037(6) 0.090(8) -0.019(5) 0.024(7) -0.009(5) C87 0.104(10) 0.044(7) 0.091(9) -0.022(6) 0.006(7) -0.018(6) C88 0.064(7) 0.045(6) 0.102(9) 0.017(6) 0.015(6) 0.020(5) C89 0.148(13) 0.079(9) 0.072(9) -0.026(7) -0.015(8) 0.003(8) C90 0.090(11) 0.131(14) 0.107(12) 0.021(10) -0.019(9) -0.029(10) C91 0.18(2) 0.081(11) 0.180(19) -0.001(12) -0.106(16) 0.016(12) C92 0.090(12) 0.19(2) 0.18(2) -0.066(17) 0.008(14) 0.029(13) C93 0.135(15) 0.125(14) 0.123(14) 0.043(11) 0.008(12) -0.062(12) C98 0.075(8) 0.069(8) 0.073(8) -0.008(6) 0.008(6) -0.006(6) C99 0.084(8) 0.077(8) 0.070(8) -0.012(6) 0.006(6) -0.012(7) C100 0.096(9) 0.067(8) 0.083(8) 0.003(6) 0.004(7) -0.018(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 Yb1 O3 2.109(5) . ? Yb1 O1 2.121(5) . ? Yb1 O4 2.139(5) . ? Yb1 O2 2.154(5) . ? Yb1 O6 2.403(5) . ? Yb1 O5 2.419(5) . ? Yb2 O7 2.037(5) . ? Yb2 O8 2.055(5) . ? Yb2 O10 2.266(5) . ? Yb2 O9 2.271(5) . ? Yb2 O11 2.364(5) . ? Yb2 O12 2.405(6) . ? O1 C1 1.341(8) . ? O2 C7 1.326(8) . ? O3 C24 1.335(8) . ? O4 C30 1.341(9) . ? O5 C47 1.440(10) . ? O5 C50 1.475(9) . ? O6 C51 1.432(9) . ? O6 C54 1.488(8) . ? O7 C55 1.367(9) . ? O8 C61 1.355(9) . ? O9 C78 1.454(11) . ? O9 C81 1.469(10) . ? O10 C82 1.429(9) . ? O10 C85 1.452(10) . ? O11 C88 1.414(11) . ? O11 C86 1.449(11) . ? O12 C89 1.397(12) . ? O12 C87 1.448(11) . ? O13 C90 1.303(15) . ? O13 C93 1.369(18) . ? O14 C94' 1.420(18) . ? O14 C94 1.458(18) . ? O14 C97' 1.47(2) . ? O14 C97 1.524(19) . ? C1 C6 1.392(10) . ? C1 C2 1.433(10) . ? C2 C3 1.395(10) . ? C2 C14 1.527(10) . ? C3 C4 1.375(11) . ? C3 H3 0.9500 . ? C4 C5 1.391(10) . ? C4 C18 1.522(11) . ? C5 C6 1.383(10) . ? C5 H5 0.9500 . ? C6 C13 1.527(10) . ? C7 C12 1.419(11) . ? C7 C8 1.431(10) . ? C8 C9 1.391(11) . ? C8 C19 1.534(11) . ? C9 C10 1.395(12) . ? C9 H9 0.9500 . ? C10 C11 1.387(11) . ? C10 C23 1.523(11) . ? C11 C12 1.373(10) . ? C11 H11 0.9500 . ? C12 C13 1.510(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.525(11) . ? C14 C17 1.538(11) . ? C14 C16 1.539(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C22 1.531(12) . ? C19 C21 1.533(11) . ? C19 C20 1.535(11) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.396(10) . ? C24 C25 1.431(10) . ? C25 C26 1.391(10) . ? C25 C37 1.533(11) . ? C26 C27 1.378(11) . ? C26 H26 0.9500 . ? C27 C28 1.393(11) . ? C27 C41 1.520(11) . ? C28 C29 1.392(10) . ? C28 H28 0.9500 . ? C29 C36 1.505(10) . ? C30 C35 1.410(11) . ? C30 C31 1.429(10) . ? C31 C32 1.391(10) . ? C31 C42 1.525(11) . ? C32 C33 1.371(12) . ? C32 H32 0.9500 . ? C33 C34 1.388(11) . ? C33 C46 1.530(11) . ? C34 C35 1.389(10) . ? C34 H34 0.9500 . ? C35 C36 1.510(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.530(11) . ? C37 C39 1.531(12) . ? C37 C40 1.552(12) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C45 1.524(12) . ? C42 C44 1.543(11) . ? C42 C43 1.553(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.472(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.511(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.488(12) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.492(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.524(12) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.514(11) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C60 1.406(11) . ? C55 C56 1.412(11) . ? C56 C57 1.406(12) . ? C56 C68 1.548(12) . ? C57 C58 1.372(12) . ? C57 H57 0.9500 . ? C58 C59 1.372(11) . ? C58 C72 1.504(12) . ? C59 C60 1.382(11) . ? C59 H59 0.9500 . ? C60 C67 1.514(10) . ? C61 C62 1.421(11) . ? C61 C66 1.421(11) . ? C62 C63 1.379(12) . ? C62 C73 1.528(12) . ? C63 C64 1.407(13) . ? C63 H63 0.9500 . ? C64 C65 1.372(13) . ? C64 C77 1.515(13) . ? C65 C66 1.383(11) . ? C65 H65 0.9500 . ? C66 C67 1.514(11) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C70 1.519(12) . ? C68 C71 1.524(12) . ? C68 C69 1.525(12) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C76 1.522(13) . ? C73 C74 1.531(12) . ? C73 C75 1.547(13) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.471(14) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.493(17) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.469(14) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.491(12) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.400(14) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.486(13) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.460(15) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 C91 1.43(2) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.45(2) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C93 1.48(2) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.529(19) . ? C94' C95' 1.515(19) . ? C95 C96 1.549(19) . ? C95' C96' 1.488(19) . ? C96 C97 1.528(19) . ? C96' C97' 1.51(2) . ? C98 C98 1.47(2) 3_575 ? C98 C99 1.483(14) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 C100 1.516(15) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Yb1 O1 99.7(2) . . ? O3 Yb1 O4 95.73(19) . . ? O1 Yb1 O4 89.95(19) . . ? O3 Yb1 O2 92.29(19) . . ? O1 Yb1 O2 95.48(18) . . ? O4 Yb1 O2 169.43(19) . . ? O3 Yb1 O6 170.64(19) . . ? O1 Yb1 O6 86.47(18) . . ? O4 Yb1 O6 91.24(19) . . ? O2 Yb1 O6 80.08(18) . . ? O3 Yb1 O5 85.99(19) . . ? O1 Yb1 O5 169.46(18) . . ? O4 Yb1 O5 80.63(18) . . ? O2 Yb1 O5 93.11(18) . . ? O6 Yb1 O5 89.01(17) . . ? O7 Yb2 O8 102.4(2) . . ? O7 Yb2 O10 94.82(19) . . ? O8 Yb2 O10 96.2(2) . . ? O7 Yb2 O9 92.3(2) . . ? O8 Yb2 O9 90.9(2) . . ? O10 Yb2 O9 168.7(2) . . ? O7 Yb2 O11 162.7(2) . . ? O8 Yb2 O11 94.9(2) . . ? O10 Yb2 O11 82.26(19) . . ? O9 Yb2 O11 88.4(2) . . ? O7 Yb2 O12 95.5(2) . . ? O8 Yb2 O12 162.1(2) . . ? O10 Yb2 O12 83.2(2) . . ? O9 Yb2 O12 87.4(2) . . ? O11 Yb2 O12 67.3(2) . . ? C1 O1 Yb1 152.8(5) . . ? C7 O2 Yb1 150.4(5) . . ? C24 O3 Yb1 153.3(5) . . ? C30 O4 Yb1 152.0(5) . . ? C47 O5 C50 107.9(6) . . ? C47 O5 Yb1 136.0(5) . . ? C50 O5 Yb1 116.0(4) . . ? C51 O6 C54 108.2(5) . . ? C51 O6 Yb1 135.7(5) . . ? C54 O6 Yb1 116.1(4) . . ? C55 O7 Yb2 151.3(5) . . ? C61 O8 Yb2 144.4(5) . . ? C78 O9 C81 108.5(7) . . ? C78 O9 Yb2 132.8(6) . . ? C81 O9 Yb2 118.6(5) . . ? C82 O10 C85 108.4(6) . . ? C82 O10 Yb2 125.3(4) . . ? C85 O10 Yb2 126.2(5) . . ? C88 O11 C86 112.7(7) . . ? C88 O11 Yb2 126.5(5) . . ? C86 O11 Yb2 119.7(6) . . ? C89 O12 C87 113.7(8) . . ? C89 O12 Yb2 134.0(6) . . ? C87 O12 Yb2 112.3(6) . . ? C90 O13 C93 109.1(13) . . ? C94' O14 C94 40.4(17) . . ? C94' O14 C97' 113(4) . . ? C94 O14 C97' 73(4) . . ? C94' O14 C97 121(3) . . ? C94 O14 C97 97(3) . . ? C97' O14 C97 54(4) . . ? O1 C1 C6 120.0(7) . . ? O1 C1 C2 119.8(6) . . ? C6 C1 C2 120.2(7) . . ? C3 C2 C1 116.6(7) . . ? C3 C2 C14 120.9(7) . . ? C1 C2 C14 122.6(7) . . ? C4 C3 C2 123.7(7) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C3 C4 C5 118.0(7) . . ? C3 C4 C18 120.9(7) . . ? C5 C4 C18 121.1(7) . . ? C6 C5 C4 121.5(7) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 119.9(7) . . ? C5 C6 C13 119.6(7) . . ? C1 C6 C13 120.5(6) . . ? O2 C7 C12 120.4(6) . . ? O2 C7 C8 122.0(7) . . ? C12 C7 C8 117.6(7) . . ? C9 C8 C7 119.1(7) . . ? C9 C8 C19 119.5(7) . . ? C7 C8 C19 121.4(7) . . ? C8 C9 C10 122.6(7) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C11 C10 C9 117.4(7) . . ? C11 C10 C23 122.2(8) . . ? C9 C10 C23 120.4(8) . . ? C12 C11 C10 122.6(8) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C7 120.5(7) . . ? C11 C12 C13 118.7(7) . . ? C7 C12 C13 120.9(7) . . ? C12 C13 C6 115.6(6) . . ? C12 C13 H13A 108.4 . . ? C6 C13 H13A 108.4 . . ? C12 C13 H13B 108.4 . . ? C6 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C2 112.8(7) . . ? C15 C14 C17 107.6(7) . . ? C2 C14 C17 110.9(6) . . ? C15 C14 C16 106.8(7) . . ? C2 C14 C16 110.2(7) . . ? C17 C14 C16 108.3(7) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 C21 109.5(7) . . ? C22 C19 C8 110.3(7) . . ? C21 C19 C8 109.5(7) . . ? C22 C19 C20 107.1(7) . . ? C21 C19 C20 107.3(7) . . ? C8 C19 C20 113.1(7) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 C29 119.3(6) . . ? O3 C24 C25 120.4(7) . . ? C29 C24 C25 120.3(6) . . ? C26 C25 C24 117.3(7) . . ? C26 C25 C37 120.6(7) . . ? C24 C25 C37 122.1(6) . . ? C27 C26 C25 123.3(7) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C26 C27 C28 118.0(7) . . ? C26 C27 C41 120.5(8) . . ? C28 C27 C41 121.5(8) . . ? C29 C28 C27 121.9(7) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C28 C29 C24 119.1(7) . . ? C28 C29 C36 119.1(7) . . ? C24 C29 C36 121.8(7) . . ? O4 C30 C35 119.6(7) . . ? O4 C30 C31 121.2(7) . . ? C35 C30 C31 119.2(7) . . ? C32 C31 C30 117.6(7) . . ? C32 C31 C42 121.0(7) . . ? C30 C31 C42 121.4(7) . . ? C33 C32 C31 123.9(7) . . ? C33 C32 H32 118.0 . . ? C31 C32 H32 118.0 . . ? C32 C33 C34 117.4(7) . . ? C32 C33 C46 122.5(8) . . ? C34 C33 C46 120.1(8) . . ? C33 C34 C35 122.4(8) . . ? C33 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C34 C35 C30 119.3(7) . . ? C34 C35 C36 118.4(7) . . ? C30 C35 C36 122.3(7) . . ? C29 C36 C35 118.0(6) . . ? C29 C36 H36A 107.8 . . ? C35 C36 H36A 107.8 . . ? C29 C36 H36B 107.8 . . ? C35 C36 H36B 107.8 . . ? H36A C36 H36B 107.1 . . ? C38 C37 C39 108.2(7) . . ? C38 C37 C25 113.2(7) . . ? C39 C37 C25 111.3(7) . . ? C38 C37 C40 105.5(7) . . ? C39 C37 C40 109.4(8) . . ? C25 C37 C40 109.1(7) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 C41 H41A 109.5 . . ? C27 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C27 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C45 C42 C31 111.0(7) . . ? C45 C42 C44 110.3(7) . . ? C31 C42 C44 109.9(7) . . ? C45 C42 C43 107.2(7) . . ? C31 C42 C43 112.0(7) . . ? C44 C42 C43 106.4(7) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C33 C46 H46A 109.5 . . ? C33 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C33 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 106.2(7) . . ? O5 C47 H47A 110.5 . . ? C48 C47 H47A 110.5 . . ? O5 C47 H47B 110.5 . . ? C48 C47 H47B 110.5 . . ? H47A C47 H47B 108.7 . . ? C47 C48 C49 103.5(8) . . ? C47 C48 H48A 111.1 . . ? C49 C48 H48A 111.1 . . ? C47 C48 H48B 111.1 . . ? C49 C48 H48B 111.1 . . ? H48A C48 H48B 109.0 . . ? C50 C49 C48 104.6(7) . . ? C50 C49 H49A 110.8 . . ? C48 C49 H49A 110.8 . . ? C50 C49 H49B 110.8 . . ? C48 C49 H49B 110.8 . . ? H49A C49 H49B 108.9 . . ? O5 C50 C49 106.5(7) . . ? O5 C50 H50A 110.4 . . ? C49 C50 H50A 110.4 . . ? O5 C50 H50B 110.4 . . ? C49 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? O6 C51 C52 104.1(6) . . ? O6 C51 H51A 110.9 . . ? C52 C51 H51A 110.9 . . ? O6 C51 H51B 110.9 . . ? C52 C51 H51B 110.9 . . ? H51A C51 H51B 109.0 . . ? C51 C52 C53 103.1(7) . . ? C51 C52 H52A 111.1 . . ? C53 C52 H52A 111.1 . . ? C51 C52 H52B 111.1 . . ? C53 C52 H52B 111.1 . . ? H52A C52 H52B 109.1 . . ? C54 C53 C52 104.1(7) . . ? C54 C53 H53A 110.9 . . ? C52 C53 H53A 110.9 . . ? C54 C53 H53B 110.9 . . ? C52 C53 H53B 110.9 . . ? H53A C53 H53B 109.0 . . ? O6 C54 C53 105.6(6) . . ? O6 C54 H54A 110.6 . . ? C53 C54 H54A 110.6 . . ? O6 C54 H54B 110.6 . . ? C53 C54 H54B 110.6 . . ? H54A C54 H54B 108.8 . . ? O7 C55 C60 118.6(7) . . ? O7 C55 C56 120.7(8) . . ? C60 C55 C56 120.7(7) . . ? C57 C56 C55 116.2(8) . . ? C57 C56 C68 122.2(7) . . ? C55 C56 C68 121.6(7) . . ? C58 C57 C56 124.3(8) . . ? C58 C57 H57 117.8 . . ? C56 C57 H57 117.8 . . ? C57 C58 C59 116.9(8) . . ? C57 C58 C72 120.6(8) . . ? C59 C58 C72 122.5(9) . . ? C58 C59 C60 123.3(8) . . ? C58 C59 H59 118.4 . . ? C60 C59 H59 118.4 . . ? C59 C60 C55 118.5(7) . . ? C59 C60 C67 120.2(7) . . ? C55 C60 C67 121.2(7) . . ? O8 C61 C62 121.4(7) . . ? O8 C61 C66 118.1(7) . . ? C62 C61 C66 120.5(7) . . ? C63 C62 C61 117.7(8) . . ? C63 C62 C73 120.2(8) . . ? C61 C62 C73 122.1(7) . . ? C62 C63 C64 123.1(9) . . ? C62 C63 H63 118.5 . . ? C64 C63 H63 118.5 . . ? C65 C64 C63 117.2(8) . . ? C65 C64 C77 121.8(9) . . ? C63 C64 C77 121.0(9) . . ? C64 C65 C66 123.7(9) . . ? C64 C65 H65 118.1 . . ? C66 C65 H65 118.2 . . ? C65 C66 C61 117.7(8) . . ? C65 C66 C67 119.4(8) . . ? C61 C66 C67 122.9(7) . . ? C66 C67 C60 114.3(6) . . ? C66 C67 H67A 108.7 . . ? C60 C67 H67A 108.7 . . ? C66 C67 H67B 108.7 . . ? C60 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? C70 C68 C71 112.5(8) . . ? C70 C68 C69 107.3(8) . . ? C71 C68 C69 106.9(8) . . ? C70 C68 C56 109.5(7) . . ? C71 C68 C56 109.1(7) . . ? C69 C68 C56 111.6(8) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C58 C72 H72A 109.5 . . ? C58 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C58 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C76 C73 C62 110.8(8) . . ? C76 C73 C74 106.5(8) . . ? C62 C73 C74 112.7(8) . . ? C76 C73 C75 112.0(8) . . ? C62 C73 C75 108.9(7) . . ? C74 C73 C75 105.8(8) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C64 C77 H77A 109.5 . . ? C64 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C64 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? O9 C78 C79 106.5(9) . . ? O9 C78 H78A 110.4 . . ? C79 C78 H78A 110.4 . . ? O9 C78 H78B 110.4 . . ? C79 C78 H78B 110.4 . . ? H78A C78 H78B 108.6 . . ? C78 C79 C80 103.7(9) . . ? C78 C79 H79A 111.0 . . ? C80 C79 H79A 111.0 . . ? C78 C79 H79B 111.0 . . ? C80 C79 H79B 111.0 . . ? H79A C79 H79B 109.0 . . ? C81 C80 C79 104.3(10) . . ? C81 C80 H80A 110.9 . . ? C79 C80 H80A 110.9 . . ? C81 C80 H80B 110.9 . . ? C79 C80 H80B 110.9 . . ? H80A C80 H80B 108.9 . . ? O9 C81 C80 103.9(9) . . ? O9 C81 H81A 111.0 . . ? C80 C81 H81A 111.0 . . ? O9 C81 H81B 111.0 . . ? C80 C81 H81B 111.0 . . ? H81A C81 H81B 109.0 . . ? O10 C82 C83 106.0(7) . . ? O10 C82 H82A 110.5 . . ? C83 C82 H82A 110.5 . . ? O10 C82 H82B 110.5 . . ? C83 C82 H82B 110.5 . . ? H82A C82 H82B 108.7 . . ? C84 C83 C82 106.2(8) . . ? C84 C83 H83A 110.5 . . ? C82 C83 H83A 110.5 . . ? C84 C83 H83B 110.5 . . ? C82 C83 H83B 110.5 . . ? H83A C83 H83B 108.7 . . ? C83 C84 C85 105.9(9) . . ? C83 C84 H84A 110.6 . . ? C85 C84 H84A 110.6 . . ? C83 C84 H84B 110.6 . . ? C85 C84 H84B 110.6 . . ? H84A C84 H84B 108.7 . . ? O10 C85 C84 104.9(8) . . ? O10 C85 H85A 110.8 . . ? C84 C85 H85A 110.8 . . ? O10 C85 H85B 110.8 . . ? C84 C85 H85B 110.8 . . ? H85A C85 H85B 108.8 . . ? O11 C86 C87 108.8(8) . . ? O11 C86 H86A 109.9 . . ? C87 C86 H86A 109.9 . . ? O11 C86 H86B 109.9 . . ? C87 C86 H86B 109.9 . . ? H86A C86 H86B 108.3 . . ? O12 C87 C86 108.3(9) . . ? O12 C87 H87A 110.0 . . ? C86 C87 H87A 110.0 . . ? O12 C87 H87B 110.0 . . ? C86 C87 H87B 110.0 . . ? H87A C87 H87B 108.4 . . ? O11 C88 H88A 109.5 . . ? O11 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? O11 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? O12 C89 H89A 109.5 . . ? O12 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? O12 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? O13 C90 C91 110.3(15) . . ? O13 C90 H90A 109.6 . . ? C91 C90 H90A 109.6 . . ? O13 C90 H90B 109.6 . . ? C91 C90 H90B 109.6 . . ? H90A C90 H90B 108.1 . . ? C90 C91 C92 102.9(14) . . ? C90 C91 H91A 111.2 . . ? C92 C91 H91A 111.2 . . ? C90 C91 H91B 111.2 . . ? C92 C91 H91B 111.2 . . ? H91A C91 H91B 109.1 . . ? C91 C92 C93 102.0(14) . . ? C91 C92 H92A 111.4 . . ? C93 C92 H92A 111.4 . . ? C91 C92 H92B 111.4 . . ? C93 C92 H92B 111.4 . . ? H92A C92 H92B 109.2 . . ? O13 C93 C92 107.5(14) . . ? O13 C93 H93A 110.2 . . ? C92 C93 H93A 110.2 . . ? O13 C93 H93B 110.2 . . ? C92 C93 H93B 110.2 . . ? H93A C93 H93B 108.5 . . ? O14 C94 C95 112(3) . . ? O14 C94' C95' 87(2) . . ? C94 C95 C96 109(2) . . ? C96' C95' C94' 110(3) . . ? C97 C96 C95 97(2) . . ? C95' C96' C97' 102(3) . . ? C96 C97 O14 117(3) . . ? O14 C97' C96' 98(3) . . ? C98 C98 C99 118.2(12) 3_575 . ? C98 C98 H98A 107.7 3_575 . ? C99 C98 H98A 107.7 . . ? C98 C98 H98B 107.7 3_575 . ? C99 C98 H98B 107.7 . . ? H98A C98 H98B 107.1 . . ? C98 C99 C100 116.1(10) . . ? C98 C99 H99A 108.3 . . ? C100 C99 H99A 108.3 . . ? C98 C99 H99B 108.3 . . ? C100 C99 H99B 108.3 . . ? H99A C99 H99B 107.4 . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.701 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.123 #============================================================end data_complex8 _database_code_depnum_ccdc_archive 'CCDC 682658' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H76 O6 Zn2, C7 H8' _chemical_formula_sum 'C61 H84 O6 Zn2' _chemical_formula_weight 1044.02 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' Zn Zn 0.2839 1.4301 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1620(13) _cell_length_b 11.4951(12) _cell_length_c 14.1651(17) _cell_angle_alpha 67.703(5) _cell_angle_beta 89.201(7) _cell_angle_gamma 86.309(7) _cell_volume 1527.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5780 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.622 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15004 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5547 _reflns_number_gt 5052 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0899P)^2^+1.9362P] 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 5547 _refine_ls_number_parameters 312 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1653 _refine_ls_wR_factor_gt 0.1601 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.144 _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 Zn1 Zn 0.00250(4) 0.41630(4) 0.10923(3) 0.02447(17) Uani 1 1 d . . . O1 O 0.1015(3) 0.3508(2) 0.22939(19) 0.0320(6) Uani 1 1 d . . . O2 O 0.0719(2) 0.4140(2) -0.02197(17) 0.0240(5) Uani 1 1 d . . . O3 O -0.1542(3) 0.3063(2) 0.1586(2) 0.0337(6) Uani 1 1 d . . . C1 C 0.2109(4) 0.3884(3) 0.2589(3) 0.0295(8) Uani 1 1 d . . . C2 C 0.2351(4) 0.3579(4) 0.3645(3) 0.0340(9) Uani 1 1 d . . . C3 C 0.3494(4) 0.3990(4) 0.3912(3) 0.0427(10) Uani 1 1 d . . . H3 H 0.3665 0.3791 0.4609 0.051 Uiso 1 1 calc R . . C4 C 0.4393(4) 0.4675(5) 0.3214(3) 0.0434(10) Uani 1 1 d . . . C5 C 0.4140(4) 0.4962(4) 0.2190(3) 0.0363(9) Uani 1 1 d . . . H5 H 0.4736 0.5429 0.1701 0.044 Uiso 1 1 calc R . . C6 C 0.3015(4) 0.4570(3) 0.1870(3) 0.0284(8) Uani 1 1 d . . . C7 C 0.1962(3) 0.3568(3) -0.0174(3) 0.0227(7) Uani 1 1 d . . . C8 C 0.2196(4) 0.2659(3) -0.0609(3) 0.0273(8) Uani 1 1 d . . . C9 C 0.3460(4) 0.2087(3) -0.0506(3) 0.0326(8) Uani 1 1 d . . . H9 H 0.3641 0.1490 -0.0804 0.039 Uiso 1 1 calc R . . C10 C 0.4473(4) 0.2357(4) 0.0017(3) 0.0358(9) Uani 1 1 d . . . C11 C 0.4205(4) 0.3251(4) 0.0432(3) 0.0307(8) Uani 1 1 d . . . H11 H 0.4877 0.3443 0.0788 0.037 Uiso 1 1 calc R . . C12 C 0.2965(3) 0.3880(3) 0.0338(3) 0.0247(7) Uani 1 1 d . . . C13 C 0.2785(4) 0.4941(3) 0.0737(3) 0.0262(7) Uani 1 1 d . . . H13A H 0.3389 0.5590 0.0369 0.031 Uiso 1 1 calc R . . H13B H 0.1885 0.5322 0.0570 0.031 Uiso 1 1 calc R . . C14 C 0.1370(5) 0.2868(4) 0.4460(3) 0.0419(10) Uani 1 1 d . . . C15 C 0.1827(6) 0.2632(6) 0.5553(4) 0.0630(14) Uani 1 1 d . . . H15A H 0.2669 0.2147 0.5693 0.095 Uiso 1 1 calc R . . H15B H 0.1180 0.2167 0.6035 0.095 Uiso 1 1 calc R . . H15C H 0.1921 0.3432 0.5618 0.095 Uiso 1 1 calc R . . C16 C 0.1185(6) 0.1561(5) 0.4436(4) 0.0588(14) Uani 1 1 d . . . H16A H 0.0857 0.1657 0.3769 0.088 Uiso 1 1 calc R . . H16B H 0.0557 0.1129 0.4953 0.088 Uiso 1 1 calc R . . H16C H 0.2024 0.1072 0.4573 0.088 Uiso 1 1 calc R . . C17 C 0.0040(5) 0.3619(5) 0.4282(4) 0.0573(13) Uani 1 1 d . . . H17A H 0.0150 0.4430 0.4324 0.086 Uiso 1 1 calc R . . H17B H -0.0576 0.3159 0.4797 0.086 Uiso 1 1 calc R . . H17C H -0.0299 0.3747 0.3610 0.086 Uiso 1 1 calc R . . C18 C 0.5605(5) 0.5142(6) 0.3539(4) 0.0637(15) Uani 1 1 d . . . H18A H 0.5341 0.5616 0.3957 0.095 Uiso 1 1 calc R . . H18B H 0.6054 0.5680 0.2939 0.095 Uiso 1 1 calc R . . H18C H 0.6195 0.4427 0.3929 0.095 Uiso 1 1 calc R . . C19 C 0.1102(4) 0.2296(3) -0.1169(3) 0.0308(8) Uani 1 1 d . . . C20 C 0.1591(5) 0.1243(4) -0.1530(3) 0.0413(10) Uani 1 1 d . . . H20A H 0.2318 0.1525 -0.1996 0.062 Uiso 1 1 calc R . . H20B H 0.0878 0.1038 -0.1877 0.062 Uiso 1 1 calc R . . H20C H 0.1887 0.0501 -0.0946 0.062 Uiso 1 1 calc R . . C21 C 0.0627(5) 0.3433(4) -0.2122(3) 0.0397(10) Uani 1 1 d . . . H21A H 0.0259 0.4103 -0.1920 0.059 Uiso 1 1 calc R . . H21B H -0.0043 0.3184 -0.2476 0.059 Uiso 1 1 calc R . . H21C H 0.1366 0.3731 -0.2572 0.059 Uiso 1 1 calc R . . C22 C -0.0062(4) 0.1811(4) -0.0449(3) 0.0409(10) Uani 1 1 d . . . H22A H 0.0258 0.1135 0.0172 0.061 Uiso 1 1 calc R . . H22B H -0.0701 0.1498 -0.0783 0.061 Uiso 1 1 calc R . . H22C H -0.0476 0.2493 -0.0284 0.061 Uiso 1 1 calc R . . C23 C 0.5824(5) 0.1674(5) 0.0130(5) 0.0585(14) Uani 1 1 d . . . H23A H 0.6499 0.2268 0.0031 0.088 Uiso 1 1 calc R . . H23B H 0.5920 0.1296 -0.0376 0.088 Uiso 1 1 calc R . . H23C H 0.5918 0.1020 0.0808 0.088 Uiso 1 1 calc R . . C24 C -0.1282(5) 0.1698(4) 0.2097(4) 0.0480(11) Uani 1 1 d D . . H24A H -0.1366 0.1284 0.1612 0.058 Uiso 1 1 calc R . . H24B H -0.0389 0.1501 0.2390 0.058 Uiso 1 1 calc R . . C25 C -0.2259(8) 0.1274(6) 0.2898(6) 0.095(2) Uani 1 1 d D . . H25A H -0.1817 0.0881 0.3565 0.114 Uiso 1 1 calc R . . H25B H -0.2785 0.0647 0.2793 0.114 Uiso 1 1 calc R . . C26 C -0.3115(8) 0.2358(6) 0.2870(6) 0.105(3) Uani 1 1 d D . . H26A H -0.3142 0.2410 0.3545 0.126 Uiso 1 1 calc R . . H26B H -0.4014 0.2277 0.2673 0.126 Uiso 1 1 calc R . . C27 C -0.2576(4) 0.3490(4) 0.2122(4) 0.0450(10) Uani 1 1 d . . . H27A H -0.3267 0.4006 0.1642 0.054 Uiso 1 1 calc R . . H27B H -0.2213 0.3997 0.2466 0.054 Uiso 1 1 calc R . . C28 C 0.4029(16) 0.9561(15) 0.3799(12) 0.109(2) Uiso 0.50 1 d PD . . C29 C 0.3557(15) 1.0561(16) 0.2938(12) 0.109(2) Uiso 0.50 1 d PD . . C30 C 0.2790(16) 1.0334(16) 0.2239(13) 0.109(2) Uiso 0.50 1 d PD . . C31 C 0.2351(17) 0.9174(15) 0.2413(13) 0.109(2) Uiso 0.50 1 d PD . . C32 C 0.3003(17) 0.8147(16) 0.3186(13) 0.109(2) Uiso 0.50 1 d PD . . C33 C 0.3758(17) 0.8366(16) 0.3889(13) 0.109(2) Uiso 0.50 1 d PD . . C34 C 0.472(2) 0.992(2) 0.4561(17) 0.151(8) Uiso 0.50 1 d PD . . 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 Zn1 0.0256(3) 0.0251(2) 0.0211(2) -0.00739(17) -0.00105(16) 0.00063(16) O1 0.0338(14) 0.0334(14) 0.0241(13) -0.0047(11) -0.0066(11) -0.0065(11) O2 0.0238(12) 0.0256(12) 0.0227(12) -0.0102(10) -0.0004(10) 0.0031(10) O3 0.0312(14) 0.0304(14) 0.0338(14) -0.0057(11) 0.0022(11) -0.0034(11) C1 0.0323(19) 0.0297(19) 0.0272(18) -0.0122(15) -0.0046(15) 0.0034(15) C2 0.041(2) 0.035(2) 0.0259(19) -0.0124(16) -0.0048(16) 0.0032(17) C3 0.047(2) 0.057(3) 0.030(2) -0.023(2) -0.0089(18) -0.001(2) C4 0.038(2) 0.061(3) 0.041(2) -0.031(2) -0.0062(19) -0.006(2) C5 0.033(2) 0.045(2) 0.038(2) -0.0238(19) 0.0002(17) -0.0036(17) C6 0.0303(19) 0.0305(19) 0.0284(18) -0.0163(16) -0.0030(15) 0.0027(15) C7 0.0229(17) 0.0191(16) 0.0224(16) -0.0044(13) 0.0000(13) 0.0034(13) C8 0.0334(19) 0.0249(18) 0.0237(17) -0.0099(15) -0.0009(15) 0.0009(15) C9 0.035(2) 0.0274(18) 0.038(2) -0.0162(17) 0.0002(17) 0.0054(15) C10 0.029(2) 0.034(2) 0.044(2) -0.0145(18) 0.0004(17) 0.0048(16) C11 0.0254(18) 0.0328(19) 0.0329(19) -0.0119(16) -0.0009(15) 0.0019(15) C12 0.0254(17) 0.0233(17) 0.0238(17) -0.0072(14) 0.0006(14) -0.0008(14) C13 0.0265(18) 0.0265(18) 0.0266(18) -0.0109(15) 0.0013(14) -0.0034(14) C14 0.054(3) 0.045(2) 0.0211(18) -0.0053(17) -0.0059(18) -0.002(2) C15 0.073(4) 0.084(4) 0.031(2) -0.019(2) -0.001(2) -0.012(3) C16 0.085(4) 0.046(3) 0.034(2) 0.000(2) -0.007(2) -0.016(3) C17 0.050(3) 0.071(3) 0.040(3) -0.010(2) 0.010(2) -0.002(2) C18 0.049(3) 0.102(4) 0.057(3) -0.048(3) -0.008(2) -0.015(3) C19 0.037(2) 0.0264(18) 0.0330(19) -0.0165(16) -0.0012(16) -0.0005(16) C20 0.050(3) 0.037(2) 0.045(2) -0.026(2) -0.006(2) 0.0044(19) C21 0.053(3) 0.033(2) 0.035(2) -0.0161(18) -0.0128(19) 0.0053(18) C22 0.042(2) 0.037(2) 0.050(2) -0.023(2) 0.0047(19) -0.0091(18) C23 0.038(3) 0.057(3) 0.090(4) -0.040(3) -0.009(3) 0.018(2) C24 0.055(3) 0.026(2) 0.058(3) -0.009(2) 0.003(2) -0.0060(19) C25 0.112(6) 0.049(3) 0.092(5) 0.009(3) 0.045(4) -0.011(3) C26 0.114(6) 0.062(4) 0.107(6) 0.002(4) 0.066(5) -0.007(4) C27 0.037(2) 0.047(3) 0.049(3) -0.016(2) 0.013(2) -0.0050(19) _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 Zn1 O1 1.858(2) . ? Zn1 O2 1.978(2) 2_565 ? Zn1 O2 1.988(2) . ? Zn1 O3 2.045(3) . ? Zn1 Zn1 2.9588(8) 2_565 ? O1 C1 1.346(4) . ? O2 C7 1.377(4) . ? O2 Zn1 1.978(2) 2_565 ? O3 C27 1.455(5) . ? O3 C24 1.464(5) . ? C1 C6 1.402(5) . ? C1 C2 1.422(5) . ? C2 C3 1.391(6) . ? C2 C14 1.533(6) . ? C3 C4 1.381(6) . ? C3 H3 0.9400 . ? C4 C5 1.384(6) . ? C4 C18 1.518(6) . ? C5 C6 1.396(5) . ? C5 H5 0.9400 . ? C6 C13 1.514(5) . ? C7 C12 1.399(5) . ? C7 C8 1.408(5) . ? C8 C9 1.388(5) . ? C8 C19 1.541(5) . ? C9 C10 1.394(6) . ? C9 H9 0.9400 . ? C10 C11 1.376(6) . ? C10 C23 1.517(6) . ? C11 C12 1.394(5) . ? C11 H11 0.9400 . ? C12 C13 1.526(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C17 1.526(7) . ? C14 C16 1.539(7) . ? C14 C15 1.540(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.537(5) . ? C19 C21 1.537(5) . ? C19 C22 1.538(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 C25 1.457(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.462(9) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.465(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C33 1.377(15) . ? C28 C29 1.386(16) . ? C28 C34 1.490(16) . ? C29 C30 1.378(16) . ? C30 C31 1.365(16) . ? C31 C32 1.403(16) . ? C32 C33 1.372(16) . ? C34 C34 1.45(4) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 134.89(11) . 2_565 ? O1 Zn1 O2 122.14(11) . . ? O2 Zn1 O2 83.47(10) 2_565 . ? O1 Zn1 O3 97.67(11) . . ? O2 Zn1 O3 106.30(10) 2_565 . ? O2 Zn1 O3 111.84(10) . . ? O1 Zn1 Zn1 146.00(8) . 2_565 ? O2 Zn1 Zn1 41.86(7) 2_565 2_565 ? O2 Zn1 Zn1 41.61(7) . 2_565 ? O3 Zn1 Zn1 115.94(8) . 2_565 ? C1 O1 Zn1 131.9(2) . . ? C7 O2 Zn1 131.2(2) . 2_565 ? C7 O2 Zn1 115.69(19) . . ? Zn1 O2 Zn1 96.53(10) 2_565 . ? C27 O3 C24 109.4(3) . . ? C27 O3 Zn1 117.1(2) . . ? C24 O3 Zn1 118.5(2) . . ? O1 C1 C6 120.9(3) . . ? O1 C1 C2 119.5(3) . . ? C6 C1 C2 119.6(3) . . ? C3 C2 C1 117.4(4) . . ? C3 C2 C14 121.0(4) . . ? C1 C2 C14 121.6(4) . . ? C4 C3 C2 123.9(4) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C3 C4 C5 117.8(4) . . ? C3 C4 C18 122.0(4) . . ? C5 C4 C18 120.1(4) . . ? C4 C5 C6 121.2(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 C13 118.4(3) . . ? C1 C6 C13 121.4(3) . . ? O2 C7 C12 118.8(3) . . ? O2 C7 C8 120.0(3) . . ? C12 C7 C8 121.2(3) . . ? C9 C8 C7 117.1(3) . . ? C9 C8 C19 120.9(3) . . ? C7 C8 C19 121.9(3) . . ? C8 C9 C10 123.1(3) . . ? C8 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C11 C10 C9 118.0(3) . . ? C11 C10 C23 121.3(4) . . ? C9 C10 C23 120.7(4) . . ? C10 C11 C12 121.8(4) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 118.7(3) . . ? C11 C12 C13 118.5(3) . . ? C7 C12 C13 122.7(3) . . ? C6 C13 C12 116.1(3) . . ? C6 C13 H13A 108.3 . . ? C12 C13 H13A 108.3 . . ? C6 C13 H13B 108.3 . . ? C12 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C17 C14 C2 110.1(3) . . ? C17 C14 C16 109.4(4) . . ? C2 C14 C16 110.7(4) . . ? C17 C14 C15 107.4(4) . . ? C2 C14 C15 113.0(4) . . ? C16 C14 C15 106.1(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 107.0(3) . . ? C20 C19 C22 107.4(3) . . ? C21 C19 C22 110.1(3) . . ? C20 C19 C8 111.8(3) . . ? C21 C19 C8 110.4(3) . . ? C22 C19 C8 110.1(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 O3 106.4(4) . . ? C25 C24 H24A 110.5 . . ? O3 C24 H24A 110.5 . . ? C25 C24 H24B 110.5 . . ? O3 C24 H24B 110.5 . . ? H24A C24 H24B 108.6 . . ? C24 C25 C26 108.9(5) . . ? C24 C25 H25A 109.9 . . ? C26 C25 H25A 109.9 . . ? C24 C25 H25B 109.9 . . ? C26 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C25 C26 C27 107.7(5) . . ? C25 C26 H26A 110.2 . . ? C27 C26 H26A 110.2 . . ? C25 C26 H26B 110.2 . . ? C27 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? O3 C27 C26 106.7(4) . . ? O3 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? O3 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C33 C28 C29 117.6(16) . . ? C33 C28 C34 126.9(17) . . ? C29 C28 C34 115.3(17) . . ? C30 C29 C28 119.5(17) . . ? C31 C30 C29 122.3(17) . . ? C30 C31 C32 116.6(17) . . ? C33 C32 C31 119.0(17) . . ? C32 C33 C28 122.4(17) . . ? C34 C34 C28 170(3) 2_676 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.966 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.094 #============================================================end data_complex9 _database_code_depnum_ccdc_archive 'CCDC 682659' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H84 Li O7 Yb, C7 H8, 0.5(C4 H8 O)' _chemical_formula_sum 'C67 H96 Li O7.50 Yb' _chemical_formula_weight 1201.42 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' Li Li -0.0003 0.0001 '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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 34.070(6) _cell_length_b 14.625(2) _cell_length_c 26.306(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.862(4) _cell_angle_gamma 90.00 _cell_volume 12726(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20255 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5048 _exptl_absorpt_coefficient_mu 1.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_T_max 0.545 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59679 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11654 _reflns_number_gt 10075 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+51.2738P] 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 11654 _refine_ls_number_parameters 703 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.137 _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 Yb1 Yb 0.376574(6) 0.614779(15) 0.146743(8) 0.02768(9) Uani 1 1 d . . . O1 O 0.34913(11) 0.5354(2) 0.08301(13) 0.0340(8) Uani 1 1 d . . . O2 O 0.39265(10) 0.7459(2) 0.11740(13) 0.0317(8) Uani 1 1 d . . . O3 O 0.38431(11) 0.5511(2) 0.21901(13) 0.0329(8) Uani 1 1 d . . . O4 O 0.33397(10) 0.7079(2) 0.16658(13) 0.0300(8) Uani 1 1 d . . . O5 O 0.43893(12) 0.5536(3) 0.14270(16) 0.0490(11) Uani 1 1 d . . . O6 O 0.34592(14) 0.9264(3) 0.17818(18) 0.0576(12) Uani 1 1 d . . . O7 O 0.32157(12) 0.8856(3) 0.06591(16) 0.0455(10) Uani 1 1 d . . . O8 O 0.4962(5) 0.1508(10) 0.1685(6) 0.110(4) Uiso 0.50 1 d PD . . C1 C 0.33816(15) 0.5167(4) 0.0313(2) 0.0303(12) Uani 1 1 d . . . C2 C 0.32818(15) 0.4278(4) 0.0126(2) 0.0324(12) Uani 1 1 d . . . C3 C 0.31789(16) 0.4151(4) -0.0417(2) 0.0379(13) Uani 1 1 d . . . H3 H 0.3116 0.3550 -0.0548 0.045 Uiso 1 1 calc R . . C4 C 0.31635(16) 0.4860(4) -0.0777(2) 0.0366(13) Uani 1 1 d . . . C5 C 0.32587(15) 0.5719(4) -0.0579(2) 0.0331(12) Uani 1 1 d . . . H5 H 0.3251 0.6212 -0.0816 0.040 Uiso 1 1 calc R . . C6 C 0.33662(15) 0.5898(4) -0.0042(2) 0.0298(12) Uani 1 1 d . . . C7 C 0.41125(15) 0.7481(3) 0.07699(19) 0.0271(11) Uani 1 1 d . . . C8 C 0.45098(15) 0.7842(3) 0.0843(2) 0.0290(11) Uani 1 1 d . . . C9 C 0.46965(16) 0.7745(4) 0.0429(2) 0.0316(12) Uani 1 1 d . . . H9 H 0.4965 0.7965 0.0474 0.038 Uiso 1 1 calc R . . C10 C 0.45103(17) 0.7343(4) -0.0045(2) 0.0372(13) Uani 1 1 d . . . C11 C 0.41131(16) 0.7066(4) -0.0115(2) 0.0332(12) Uani 1 1 d . . . H11 H 0.3975 0.6823 -0.0445 0.040 Uiso 1 1 calc R . . C12 C 0.39109(15) 0.7133(3) 0.0280(2) 0.0283(11) Uani 1 1 d . . . C13 C 0.34642(15) 0.6857(4) 0.0153(2) 0.0338(12) Uani 1 1 d . . . H13A H 0.3363 0.6941 0.0473 0.041 Uiso 1 1 calc R . . H13B H 0.3312 0.7285 -0.0114 0.041 Uiso 1 1 calc R . . C14 C 0.32992(17) 0.3465(4) 0.0501(2) 0.0400(13) Uani 1 1 d . . . C15 C 0.3172(2) 0.2559(4) 0.0215(3) 0.0494(16) Uani 1 1 d . . . H15A H 0.3355 0.2416 -0.0010 0.074 Uiso 1 1 calc R . . H15B H 0.2895 0.2613 -0.0001 0.074 Uiso 1 1 calc R . . H15C H 0.3183 0.2068 0.0471 0.074 Uiso 1 1 calc R . . C16 C 0.3015(2) 0.3628(4) 0.0868(2) 0.0467(15) Uani 1 1 d . . . H16A H 0.3043 0.3124 0.1120 0.070 Uiso 1 1 calc R . . H16B H 0.2735 0.3657 0.0661 0.070 Uiso 1 1 calc R . . H16C H 0.3086 0.4205 0.1056 0.070 Uiso 1 1 calc R . . C17 C 0.37333(18) 0.3346(4) 0.0824(3) 0.0489(15) Uani 1 1 d . . . H17A H 0.3913 0.3250 0.0588 0.073 Uiso 1 1 calc R . . H17B H 0.3748 0.2816 0.1055 0.073 Uiso 1 1 calc R . . H17C H 0.3817 0.3896 0.1034 0.073 Uiso 1 1 calc R . . C18 C 0.30528(19) 0.4670(5) -0.1357(2) 0.0487(16) Uani 1 1 d . . . H18A H 0.2959 0.5236 -0.1548 0.073 Uiso 1 1 calc R . . H18B H 0.2837 0.4212 -0.1436 0.073 Uiso 1 1 calc R . . H18C H 0.3290 0.4439 -0.1465 0.073 Uiso 1 1 calc R . . C19 C 0.47358(17) 0.8299(4) 0.1348(2) 0.0433(15) Uani 1 1 d . . . C20 C 0.51248(18) 0.8788(4) 0.1293(2) 0.0479(16) Uani 1 1 d . . . H20A H 0.5311 0.8339 0.1203 0.072 Uiso 1 1 calc R . . H20B H 0.5254 0.9083 0.1626 0.072 Uiso 1 1 calc R . . H20C H 0.5057 0.9250 0.1017 0.072 Uiso 1 1 calc R . . C21 C 0.4869(2) 0.7583(7) 0.1775(3) 0.081(3) Uani 1 1 d . . . H21A H 0.4630 0.7297 0.1854 0.122 Uiso 1 1 calc R . . H21B H 0.5031 0.7875 0.2092 0.122 Uiso 1 1 calc R . . H21C H 0.5032 0.7115 0.1655 0.122 Uiso 1 1 calc R . . C22 C 0.4472(2) 0.9037(6) 0.1518(3) 0.084(3) Uani 1 1 d . . . H22A H 0.4379 0.9471 0.1231 0.126 Uiso 1 1 calc R . . H22B H 0.4631 0.9361 0.1825 0.126 Uiso 1 1 calc R . . H22C H 0.4238 0.8748 0.1607 0.126 Uiso 1 1 calc R . . C23 C 0.4737(2) 0.7249(5) -0.0472(3) 0.0602(19) Uani 1 1 d . . . H23A H 0.4791 0.7858 -0.0596 0.090 Uiso 1 1 calc R . . H23B H 0.4573 0.6898 -0.0764 0.090 Uiso 1 1 calc R . . H23C H 0.4993 0.6931 -0.0333 0.090 Uiso 1 1 calc R . . C24 C 0.39462(15) 0.5508(4) 0.2716(2) 0.0298(12) Uani 1 1 d . . . C25 C 0.39679(15) 0.4689(4) 0.30087(19) 0.0285(11) Uani 1 1 d . . . C26 C 0.40966(15) 0.4757(4) 0.3557(2) 0.0328(12) Uani 1 1 d . . . H26 H 0.4118 0.4210 0.3757 0.039 Uiso 1 1 calc R . . C27 C 0.41936(16) 0.5572(4) 0.3822(2) 0.0342(13) Uani 1 1 d . . . C28 C 0.41519(15) 0.6362(4) 0.3528(2) 0.0327(12) Uani 1 1 d . . . H28 H 0.4214 0.6932 0.3703 0.039 Uiso 1 1 calc R . . C29 C 0.40215(15) 0.6353(3) 0.2981(2) 0.0290(12) Uani 1 1 d . . . C30 C 0.31936(15) 0.7210(4) 0.2101(2) 0.0296(12) Uani 1 1 d . . . C31 C 0.27696(16) 0.7162(4) 0.2057(2) 0.0342(13) Uani 1 1 d . . . C32 C 0.26353(18) 0.7430(4) 0.2499(2) 0.0447(15) Uani 1 1 d . . . H32 H 0.2353 0.7438 0.2473 0.054 Uiso 1 1 calc R . . C33 C 0.28922(19) 0.7684(4) 0.2969(2) 0.0442(15) Uani 1 1 d . . . C34 C 0.33033(18) 0.7627(4) 0.3010(2) 0.0386(14) Uani 1 1 d . . . H34 H 0.3485 0.7758 0.3336 0.046 Uiso 1 1 calc R . . C35 C 0.34575(16) 0.7381(3) 0.2583(2) 0.0300(12) Uani 1 1 d . . . C36 C 0.39104(15) 0.7239(4) 0.2686(2) 0.0320(12) Uani 1 1 d . . . H36A H 0.3993 0.7216 0.2350 0.038 Uiso 1 1 calc R . . H36B H 0.4053 0.7755 0.2895 0.038 Uiso 1 1 calc R . . C37 C 0.38298(17) 0.3788(4) 0.2740(2) 0.0350(13) Uani 1 1 d . . . C38 C 0.3880(2) 0.2985(4) 0.3129(2) 0.0473(15) Uani 1 1 d . . . H38A H 0.4167 0.2900 0.3295 0.071 Uiso 1 1 calc R . . H38B H 0.3772 0.2427 0.2941 0.071 Uiso 1 1 calc R . . H38C H 0.3733 0.3119 0.3398 0.071 Uiso 1 1 calc R . . C39 C 0.40735(19) 0.3524(4) 0.2339(2) 0.0428(14) Uani 1 1 d . . . H39A H 0.4036 0.3992 0.2064 0.064 Uiso 1 1 calc R . . H39B H 0.3979 0.2933 0.2181 0.064 Uiso 1 1 calc R . . H39C H 0.4361 0.3481 0.2515 0.064 Uiso 1 1 calc R . . C40 C 0.33821(18) 0.3841(4) 0.2461(2) 0.0445(15) Uani 1 1 d . . . H40A H 0.3221 0.3933 0.2720 0.067 Uiso 1 1 calc R . . H40B H 0.3300 0.3269 0.2270 0.067 Uiso 1 1 calc R . . H40C H 0.3338 0.4353 0.2214 0.067 Uiso 1 1 calc R . . C41 C 0.43221(19) 0.5600(5) 0.4413(2) 0.0477(16) Uani 1 1 d . . . H41A H 0.4536 0.6056 0.4523 0.072 Uiso 1 1 calc R . . H41B H 0.4424 0.4997 0.4546 0.072 Uiso 1 1 calc R . . H41C H 0.4090 0.5763 0.4554 0.072 Uiso 1 1 calc R . . C42 C 0.24763(16) 0.6769(4) 0.1572(2) 0.0420(14) Uani 1 1 d . . . C43 C 0.20359(19) 0.6826(6) 0.1611(3) 0.072(2) Uani 1 1 d . . . H43A H 0.2005 0.6494 0.1922 0.108 Uiso 1 1 calc R . . H43B H 0.1860 0.6551 0.1298 0.108 Uiso 1 1 calc R . . H43C H 0.1961 0.7468 0.1636 0.108 Uiso 1 1 calc R . . C44 C 0.2583(2) 0.5765(5) 0.1518(3) 0.0621(19) Uani 1 1 d . . . H44A H 0.2857 0.5722 0.1462 0.093 Uiso 1 1 calc R . . H44B H 0.2390 0.5495 0.1219 0.093 Uiso 1 1 calc R . . H44C H 0.2571 0.5435 0.1838 0.093 Uiso 1 1 calc R . . C45 C 0.24964(18) 0.7287(5) 0.1071(2) 0.0495(16) Uani 1 1 d . . . H45A H 0.2449 0.7940 0.1117 0.074 Uiso 1 1 calc R . . H45B H 0.2289 0.7050 0.0776 0.074 Uiso 1 1 calc R . . H45C H 0.2764 0.7203 0.1001 0.074 Uiso 1 1 calc R . . C46 C 0.2729(2) 0.7989(6) 0.3427(3) 0.071(2) Uani 1 1 d . . . H46A H 0.2536 0.7535 0.3494 0.107 Uiso 1 1 calc R . . H46B H 0.2593 0.8580 0.3347 0.107 Uiso 1 1 calc R . . H46C H 0.2953 0.8051 0.3739 0.107 Uiso 1 1 calc R . . C47 C 0.4501(2) 0.5348(5) 0.0933(3) 0.0576(19) Uani 1 1 d . . . H47A H 0.4653 0.5868 0.0834 0.069 Uiso 1 1 calc R . . H47B H 0.4257 0.5237 0.0648 0.069 Uiso 1 1 calc R . . C48 C 0.4764(2) 0.4496(5) 0.1039(4) 0.081(3) Uani 1 1 d . . . H48A H 0.4624 0.3970 0.0837 0.098 Uiso 1 1 calc R . . H48B H 0.5022 0.4598 0.0937 0.098 Uiso 1 1 calc R . . C49 C 0.4840(3) 0.4316(8) 0.1605(5) 0.132(5) Uani 1 1 d . . . H49A H 0.5130 0.4190 0.1755 0.159 Uiso 1 1 calc R . . H49B H 0.4681 0.3784 0.1673 0.159 Uiso 1 1 calc R . . C50 C 0.4712(2) 0.5169(6) 0.1841(3) 0.076(3) Uani 1 1 d . . . H50A H 0.4613 0.5024 0.2156 0.091 Uiso 1 1 calc R . . H50B H 0.4939 0.5608 0.1937 0.091 Uiso 1 1 calc R . . C51 C 0.3734(3) 0.9698(6) 0.2214(4) 0.087(3) Uani 1 1 d D . . C52 C 0.3553(6) 1.0664(14) 0.2242(11) 0.098(8) Uiso 0.40 1 d PD . . C52' C 0.3492(5) 1.0319(13) 0.2480(7) 0.102(6) Uiso 0.60 1 d PD . . C53 C 0.3108(5) 1.0577(14) 0.1992(8) 0.065(5) Uiso 0.40 1 d PD . . C53' C 0.3055(4) 1.0145(11) 0.2232(6) 0.084(4) Uiso 0.60 1 d PD . . C54 C 0.3054(3) 0.9608(7) 0.1755(4) 0.109(4) Uani 1 1 d . . . C55 C 0.28020(19) 0.8991(5) 0.0360(3) 0.0532(17) Uani 1 1 d . . . H55A H 0.2619 0.9074 0.0596 0.064 Uiso 1 1 calc R . . H55B H 0.2709 0.8458 0.0131 0.064 Uiso 1 1 calc R . . C56 C 0.2810(2) 0.9839(6) 0.0037(3) 0.072(2) Uani 1 1 d . . . H56A H 0.2601 0.9815 -0.0297 0.086 Uiso 1 1 calc R . . H56B H 0.2769 1.0397 0.0231 0.086 Uiso 1 1 calc R . . C57 C 0.3227(2) 0.9805(5) -0.0054(3) 0.064(2) Uani 1 1 d . . . H57A H 0.3239 0.9385 -0.0345 0.077 Uiso 1 1 calc R . . H57B H 0.3319 1.0420 -0.0133 0.077 Uiso 1 1 calc R . . C58 C 0.3474(2) 0.9454(5) 0.0455(3) 0.0554(18) Uani 1 1 d . . . H58A H 0.3713 0.9116 0.0401 0.066 Uiso 1 1 calc R . . H58B H 0.3569 0.9965 0.0700 0.066 Uiso 1 1 calc R . . C59 C 0.4102(2) 0.9980(5) 0.4290(3) 0.063(2) Uani 1 1 d . . . C60 C 0.3906(2) 0.9184(6) 0.4135(3) 0.071(2) Uani 1 1 d . . . H60 H 0.3722 0.9154 0.3802 0.085 Uiso 1 1 calc R . . C61 C 0.3965(2) 0.8441(6) 0.4440(4) 0.070(2) Uani 1 1 d . . . H61 H 0.3825 0.7892 0.4315 0.084 Uiso 1 1 calc R . . C62 C 0.4219(3) 0.8452(6) 0.4924(4) 0.080(3) Uani 1 1 d . . . H62 H 0.4258 0.7921 0.5138 0.096 Uiso 1 1 calc R . . C63 C 0.4423(3) 0.9275(7) 0.5101(4) 0.089(3) Uani 1 1 d . . . H63 H 0.4600 0.9312 0.5439 0.107 Uiso 1 1 calc R . . C64 C 0.4360(2) 1.0024(6) 0.4774(3) 0.073(2) Uani 1 1 d . . . H64 H 0.4498 1.0579 0.4887 0.088 Uiso 1 1 calc R . . C65 C 0.4034(3) 1.0809(8) 0.3936(5) 0.116(4) Uani 1 1 d . . . H65A H 0.3805 1.0696 0.3637 0.174 Uiso 1 1 calc R . . H65B H 0.4278 1.0927 0.3809 0.174 Uiso 1 1 calc R . . H65C H 0.3976 1.1341 0.4132 0.174 Uiso 1 1 calc R . . C66 C 0.5214(10) 0.139(3) 0.2221(9) 0.192(15) Uiso 0.50 1 d PD . . C67 C 0.5035(8) 0.153(2) 0.2708(10) 0.174(13) Uiso 0.50 1 d PD . . C68 C 0.4624(6) 0.1381(16) 0.2334(9) 0.108(7) Uiso 0.50 1 d PD . . C69 C 0.4566(7) 0.156(2) 0.1729(10) 0.153(10) Uiso 0.50 1 d PD . . Li1 Li 0.3481(3) 0.8192(6) 0.1314(4) 0.038(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02833(14) 0.03523(15) 0.02117(13) 0.00030(10) 0.00924(9) 0.00378(10) O1 0.041(2) 0.034(2) 0.028(2) -0.0070(16) 0.0087(16) 0.0019(17) O2 0.0302(19) 0.043(2) 0.0245(19) -0.0017(16) 0.0111(15) -0.0017(16) O3 0.047(2) 0.033(2) 0.0200(18) -0.0025(15) 0.0111(16) -0.0004(17) O4 0.0275(18) 0.037(2) 0.0279(19) -0.0004(16) 0.0112(15) 0.0034(15) O5 0.037(2) 0.065(3) 0.048(3) 0.019(2) 0.0177(19) 0.019(2) O6 0.063(3) 0.055(3) 0.058(3) -0.020(2) 0.021(2) 0.002(2) O7 0.044(2) 0.045(2) 0.049(3) 0.013(2) 0.0127(19) 0.0037(19) C1 0.023(3) 0.042(3) 0.028(3) -0.003(2) 0.010(2) 0.004(2) C2 0.029(3) 0.037(3) 0.035(3) -0.005(2) 0.015(2) -0.005(2) C3 0.031(3) 0.046(3) 0.038(3) -0.015(3) 0.012(2) -0.008(3) C4 0.028(3) 0.055(4) 0.028(3) -0.009(3) 0.009(2) -0.004(3) C5 0.021(3) 0.046(3) 0.033(3) -0.001(3) 0.007(2) -0.001(2) C6 0.023(3) 0.038(3) 0.028(3) -0.006(2) 0.006(2) 0.000(2) C7 0.031(3) 0.025(3) 0.028(3) 0.006(2) 0.012(2) 0.009(2) C8 0.028(3) 0.028(3) 0.030(3) 0.004(2) 0.006(2) 0.005(2) C9 0.030(3) 0.033(3) 0.035(3) 0.002(2) 0.015(2) 0.000(2) C10 0.036(3) 0.047(4) 0.032(3) -0.006(3) 0.014(2) -0.002(3) C11 0.037(3) 0.033(3) 0.031(3) -0.003(2) 0.012(2) -0.003(2) C12 0.028(3) 0.027(3) 0.030(3) 0.000(2) 0.007(2) 0.004(2) C13 0.031(3) 0.042(3) 0.028(3) 0.003(2) 0.006(2) 0.005(2) C14 0.041(3) 0.038(3) 0.043(3) -0.008(3) 0.016(3) -0.005(3) C15 0.062(4) 0.038(4) 0.052(4) -0.002(3) 0.021(3) -0.011(3) C16 0.059(4) 0.045(4) 0.041(4) 0.002(3) 0.023(3) -0.006(3) C17 0.049(4) 0.040(4) 0.058(4) -0.005(3) 0.012(3) 0.000(3) C18 0.048(4) 0.067(4) 0.029(3) -0.012(3) 0.006(3) -0.011(3) C19 0.033(3) 0.060(4) 0.037(3) -0.011(3) 0.011(3) -0.012(3) C20 0.038(3) 0.064(4) 0.042(4) -0.014(3) 0.010(3) -0.017(3) C21 0.060(5) 0.143(8) 0.034(4) 0.026(4) 0.001(3) -0.027(5) C22 0.047(4) 0.117(7) 0.096(6) -0.081(6) 0.034(4) -0.034(4) C23 0.053(4) 0.087(5) 0.050(4) -0.025(4) 0.031(3) -0.017(4) C24 0.024(3) 0.040(3) 0.027(3) 0.002(2) 0.009(2) -0.001(2) C25 0.026(3) 0.034(3) 0.025(3) -0.001(2) 0.006(2) -0.002(2) C26 0.030(3) 0.038(3) 0.031(3) 0.008(2) 0.008(2) 0.002(2) C27 0.032(3) 0.047(4) 0.022(3) -0.001(2) 0.003(2) 0.003(3) C28 0.026(3) 0.040(3) 0.031(3) -0.006(2) 0.004(2) -0.002(2) C29 0.025(3) 0.033(3) 0.031(3) -0.002(2) 0.010(2) 0.000(2) C30 0.033(3) 0.030(3) 0.031(3) 0.005(2) 0.019(2) 0.006(2) C31 0.031(3) 0.046(3) 0.030(3) 0.009(2) 0.014(2) 0.008(2) C32 0.038(3) 0.058(4) 0.045(4) 0.017(3) 0.024(3) 0.020(3) C33 0.056(4) 0.048(4) 0.035(3) 0.006(3) 0.022(3) 0.017(3) C34 0.048(4) 0.041(3) 0.029(3) 0.001(2) 0.015(3) 0.013(3) C35 0.035(3) 0.030(3) 0.029(3) -0.001(2) 0.014(2) 0.000(2) C36 0.031(3) 0.035(3) 0.032(3) -0.003(2) 0.011(2) -0.004(2) C37 0.038(3) 0.037(3) 0.029(3) 0.002(2) 0.005(2) -0.005(2) C38 0.062(4) 0.034(3) 0.043(4) 0.003(3) 0.006(3) -0.007(3) C39 0.059(4) 0.031(3) 0.040(3) -0.005(3) 0.015(3) 0.005(3) C40 0.044(3) 0.050(4) 0.035(3) 0.001(3) 0.002(3) -0.006(3) C41 0.055(4) 0.057(4) 0.026(3) -0.002(3) 0.001(3) 0.003(3) C42 0.025(3) 0.060(4) 0.042(3) 0.004(3) 0.010(2) 0.001(3) C43 0.032(4) 0.113(7) 0.069(5) 0.012(5) 0.010(3) -0.007(4) C44 0.052(4) 0.065(5) 0.063(5) -0.003(4) 0.001(3) -0.014(4) C45 0.040(3) 0.067(4) 0.039(4) 0.007(3) 0.004(3) 0.009(3) C46 0.079(5) 0.098(6) 0.047(4) 0.004(4) 0.036(4) 0.032(5) C47 0.061(4) 0.056(4) 0.072(5) 0.011(4) 0.047(4) 0.025(3) C48 0.046(4) 0.052(5) 0.158(9) 0.020(5) 0.047(5) 0.018(4) C49 0.102(8) 0.133(9) 0.191(12) 0.101(9) 0.092(8) 0.092(7) C50 0.036(4) 0.100(6) 0.085(6) 0.059(5) 0.002(4) 0.005(4) C51 0.077(6) 0.092(7) 0.084(6) -0.046(5) 0.004(5) 0.011(5) C54 0.064(5) 0.118(8) 0.146(9) -0.079(7) 0.026(6) 0.023(5) C55 0.043(4) 0.064(5) 0.053(4) 0.007(3) 0.013(3) 0.006(3) C56 0.061(5) 0.079(6) 0.077(5) 0.028(4) 0.022(4) 0.018(4) C57 0.060(5) 0.070(5) 0.067(5) 0.019(4) 0.024(4) 0.002(4) C58 0.047(4) 0.049(4) 0.073(5) 0.018(4) 0.019(3) 0.006(3) C59 0.052(4) 0.063(5) 0.077(5) -0.005(4) 0.022(4) 0.009(4) C60 0.062(5) 0.084(6) 0.074(6) -0.021(5) 0.032(4) -0.011(5) C61 0.066(5) 0.072(6) 0.081(6) -0.021(5) 0.035(5) -0.007(4) C62 0.075(6) 0.065(5) 0.112(8) 0.023(5) 0.047(5) 0.010(5) C63 0.075(6) 0.099(7) 0.086(7) 0.015(6) 0.006(5) -0.010(5) C64 0.069(5) 0.061(5) 0.086(6) -0.022(5) 0.013(5) -0.017(4) C65 0.097(8) 0.106(8) 0.141(10) 0.037(8) 0.022(7) 0.010(6) Li1 0.045(5) 0.037(5) 0.035(5) 0.002(4) 0.018(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O1 2.070(3) . ? Yb1 O3 2.076(3) . ? Yb1 O4 2.144(3) . ? Yb1 O2 2.186(4) . ? Yb1 O5 2.331(4) . ? Yb1 C7 3.099(5) . ? Yb1 Li1 3.138(9) . ? O1 C1 1.350(6) . ? O2 C7 1.362(6) . ? O2 Li1 1.962(10) . ? O3 C24 1.344(6) . ? O4 C30 1.368(6) . ? O4 Li1 1.988(10) . ? O5 C50 1.452(7) . ? O5 C47 1.464(7) . ? O6 C51 1.437(9) . ? O6 C54 1.456(9) . ? O6 Li1 2.007(10) . ? O7 C58 1.434(7) . ? O7 C55 1.454(7) . ? O7 Li1 1.995(10) . ? O8 C69 1.383(17) . ? O8 C66 1.475(19) . ? O8 C67 1.59(3) 2_655 ? C1 C2 1.403(8) . ? C1 C6 1.411(7) . ? C2 C3 1.399(7) . ? C2 C14 1.538(8) . ? C3 C4 1.395(8) . ? C3 H3 0.9500 . ? C4 C5 1.368(8) . ? C4 C18 1.509(7) . ? C5 C6 1.397(7) . ? C5 H5 0.9500 . ? C6 C13 1.504(7) . ? C7 C12 1.403(7) . ? C7 C8 1.423(7) . ? C8 C9 1.395(7) . ? C8 C19 1.521(7) . ? C9 C10 1.387(7) . ? C9 H9 0.9500 . ? C10 C11 1.382(7) . ? C10 C23 1.513(8) . ? C11 C12 1.382(7) . ? C11 H11 0.9500 . ? C12 C13 1.532(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C17 1.529(8) . ? C14 C15 1.535(8) . ? C14 C16 1.540(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.524(10) . ? C19 C22 1.537(9) . ? C19 C20 1.542(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.412(7) . ? C24 C25 1.416(7) . ? C25 C26 1.407(7) . ? C25 C37 1.516(7) . ? C26 C27 1.381(8) . ? C26 H26 0.9500 . ? C27 C28 1.378(8) . ? C27 C41 1.512(7) . ? C28 C29 1.401(7) . ? C28 H28 0.9500 . ? C29 C36 1.511(7) . ? C30 C35 1.388(7) . ? C30 C31 1.423(7) . ? C31 C32 1.402(8) . ? C31 C42 1.532(8) . ? C32 C33 1.384(9) . ? C32 H32 0.9500 . ? C33 C34 1.381(8) . ? C33 C46 1.511(8) . ? C34 C35 1.398(7) . ? C34 H34 0.9500 . ? C35 C36 1.515(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C40 1.528(8) . ? C37 C38 1.538(8) . ? C37 C39 1.541(8) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.527(10) . ? C42 C43 1.531(8) . ? C42 C45 1.536(8) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.523(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.474(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.503(14) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52' 1.505(19) . ? C51 C52 1.550(17) . ? C52 C53 1.508(17) . ? C52' C53' 1.499(15) . ? C53 C54 1.54(2) . ? C53' C54 1.480(17) . ? C55 C56 1.508(9) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.498(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.492(9) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.356(11) . ? C59 C64 1.363(11) . ? C59 C65 1.513(12) . ? C60 C61 1.337(12) . ? C60 H60 0.9500 . ? C61 C62 1.358(12) . ? C61 H61 0.9500 . ? C62 C63 1.411(13) . ? C62 H62 0.9500 . ? C63 C64 1.378(12) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 0.94(5) 2_655 ? C66 C68 1.17(3) 2_655 ? C66 C67 1.560(19) . ? C67 C66 0.94(5) 2_655 ? C67 C67 1.06(5) 2_655 ? C67 C68 1.21(4) 2_655 ? C67 C68 1.522(19) . ? C67 O8 1.59(3) 2_655 ? C67 C69 1.75(4) 2_655 ? C68 C66 1.17(3) 2_655 ? C68 C67 1.21(4) 2_655 ? C68 C69 1.580(18) . ? C69 C67 1.75(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O3 115.05(14) . . ? O1 Yb1 O4 110.67(13) . . ? O3 Yb1 O4 90.41(13) . . ? O1 Yb1 O2 108.01(14) . . ? O3 Yb1 O2 136.85(13) . . ? O4 Yb1 O2 76.70(13) . . ? O1 Yb1 O5 89.28(15) . . ? O3 Yb1 O5 87.26(14) . . ? O4 Yb1 O5 158.82(15) . . ? O2 Yb1 O5 90.72(14) . . ? O1 Yb1 C7 92.05(14) . . ? O3 Yb1 C7 147.32(14) . . ? O4 Yb1 C7 96.94(13) . . ? O2 Yb1 C7 22.40(12) . . ? O5 Yb1 C7 74.54(13) . . ? O1 Yb1 Li1 111.4(2) . . ? O3 Yb1 Li1 120.87(19) . . ? O4 Yb1 Li1 38.76(18) . . ? O2 Yb1 Li1 38.22(19) . . ? O5 Yb1 Li1 128.1(2) . . ? C7 Yb1 Li1 58.28(18) . . ? C1 O1 Yb1 153.2(3) . . ? C7 O2 Li1 131.2(4) . . ? C7 O2 Yb1 119.9(3) . . ? Li1 O2 Yb1 98.2(3) . . ? C24 O3 Yb1 152.7(3) . . ? C30 O4 Li1 117.0(4) . . ? C30 O4 Yb1 134.1(3) . . ? Li1 O4 Yb1 98.8(3) . . ? C50 O5 C47 106.6(5) . . ? C50 O5 Yb1 130.0(4) . . ? C47 O5 Yb1 123.0(4) . . ? C51 O6 C54 108.5(6) . . ? C51 O6 Li1 135.9(5) . . ? C54 O6 Li1 114.5(5) . . ? C58 O7 C55 108.5(5) . . ? C58 O7 Li1 115.3(5) . . ? C55 O7 Li1 135.5(4) . . ? C69 O8 C66 107(2) . . ? C69 O8 C67 71.8(17) . 2_655 ? C66 O8 C67 35.3(18) . 2_655 ? O1 C1 C2 121.7(5) . . ? O1 C1 C6 118.1(5) . . ? C2 C1 C6 120.2(5) . . ? C3 C2 C1 117.5(5) . . ? C3 C2 C14 121.0(5) . . ? C1 C2 C14 121.5(5) . . ? C4 C3 C2 123.5(5) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C5 C4 C3 117.2(5) . . ? C5 C4 C18 122.2(6) . . ? C3 C4 C18 120.6(5) . . ? C4 C5 C6 122.5(5) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 119.1(5) . . ? C5 C6 C13 120.2(5) . . ? C1 C6 C13 120.8(5) . . ? O2 C7 C12 119.5(4) . . ? O2 C7 C8 120.5(4) . . ? C12 C7 C8 120.0(4) . . ? O2 C7 Yb1 37.7(2) . . ? C12 C7 Yb1 98.3(3) . . ? C8 C7 Yb1 129.7(3) . . ? C9 C8 C7 116.9(5) . . ? C9 C8 C19 119.8(5) . . ? C7 C8 C19 123.3(5) . . ? C10 C9 C8 123.4(5) . . ? C10 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C11 C10 C9 117.8(5) . . ? C11 C10 C23 122.1(5) . . ? C9 C10 C23 120.1(5) . . ? C12 C11 C10 121.8(5) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 119.7(5) . . ? C11 C12 C13 117.8(5) . . ? C7 C12 C13 122.5(4) . . ? C6 C13 C12 116.6(4) . . ? C6 C13 H13A 108.2 . . ? C12 C13 H13A 108.2 . . ? C6 C13 H13B 108.2 . . ? C12 C13 H13B 108.2 . . ? H13A C13 H13B 107.3 . . ? C17 C14 C15 107.3(5) . . ? C17 C14 C16 109.9(5) . . ? C15 C14 C16 107.1(5) . . ? C17 C14 C2 109.1(5) . . ? C15 C14 C2 112.9(5) . . ? C16 C14 C2 110.5(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C19 C21 109.9(5) . . ? C8 C19 C22 110.7(5) . . ? C21 C19 C22 111.1(6) . . ? C8 C19 C20 112.9(5) . . ? C21 C19 C20 106.0(5) . . ? C22 C19 C20 106.1(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 C29 118.5(5) . . ? O3 C24 C25 121.9(5) . . ? C29 C24 C25 119.5(5) . . ? C26 C25 C24 117.4(5) . . ? C26 C25 C37 121.6(5) . . ? C24 C25 C37 120.8(4) . . ? C27 C26 C25 123.8(5) . . ? C27 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? C28 C27 C26 117.4(5) . . ? C28 C27 C41 121.3(5) . . ? C26 C27 C41 121.2(5) . . ? C27 C28 C29 122.2(5) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C28 C29 C24 119.4(5) . . ? C28 C29 C36 119.9(5) . . ? C24 C29 C36 120.2(5) . . ? O4 C30 C35 120.2(4) . . ? O4 C30 C31 119.4(5) . . ? C35 C30 C31 120.4(5) . . ? C32 C31 C30 116.4(5) . . ? C32 C31 C42 121.2(5) . . ? C30 C31 C42 122.2(5) . . ? C33 C32 C31 123.6(5) . . ? C33 C32 H32 118.2 . . ? C31 C32 H32 118.2 . . ? C34 C33 C32 117.8(5) . . ? C34 C33 C46 121.0(6) . . ? C32 C33 C46 121.2(6) . . ? C33 C34 C35 121.5(5) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C30 C35 C34 119.6(5) . . ? C30 C35 C36 123.3(4) . . ? C34 C35 C36 117.0(5) . . ? C29 C36 C35 109.2(4) . . ? C29 C36 H36A 109.8 . . ? C35 C36 H36A 109.8 . . ? C29 C36 H36B 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? C25 C37 C40 110.0(5) . . ? C25 C37 C38 112.4(4) . . ? C40 C37 C38 107.3(5) . . ? C25 C37 C39 112.3(4) . . ? C40 C37 C39 108.8(5) . . ? C38 C37 C39 105.8(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 C41 H41A 109.5 . . ? C27 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C27 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C43 108.5(6) . . ? C44 C42 C31 108.4(5) . . ? C43 C42 C31 112.2(5) . . ? C44 C42 C45 109.5(5) . . ? C43 C42 C45 106.0(5) . . ? C31 C42 C45 112.1(5) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C33 C46 H46A 109.5 . . ? C33 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C33 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 105.0(6) . . ? O5 C47 H47A 110.8 . . ? C48 C47 H47A 110.8 . . ? O5 C47 H47B 110.8 . . ? C48 C47 H47B 110.8 . . ? H47A C47 H47B 108.8 . . ? C49 C48 C47 106.5(7) . . ? C49 C48 H48A 110.4 . . ? C47 C48 H48A 110.4 . . ? C49 C48 H48B 110.4 . . ? C47 C48 H48B 110.4 . . ? H48A C48 H48B 108.6 . . ? C48 C49 C50 105.7(7) . . ? C48 C49 H49A 110.6 . . ? C50 C49 H49A 110.6 . . ? C48 C49 H49B 110.6 . . ? C50 C49 H49B 110.6 . . ? H49A C49 H49B 108.7 . . ? O5 C50 C49 103.9(7) . . ? O5 C50 H50A 111.0 . . ? C49 C50 H50A 111.0 . . ? O5 C50 H50B 111.0 . . ? C49 C50 H50B 111.0 . . ? H50A C50 H50B 109.0 . . ? O6 C51 C52' 108.0(9) . . ? O6 C51 C52 104.4(10) . . ? C52' C51 C52 32.9(11) . . ? C53 C52 C51 105.9(15) . . ? C53' C52' C51 107.1(13) . . ? C52 C53 C54 105.2(14) . . ? C54 C53' C52' 105.0(12) . . ? O6 C54 C53' 109.4(9) . . ? O6 C54 C53 106.2(9) . . ? C53' C54 C53 36.2(8) . . ? O7 C55 C56 105.7(5) . . ? O7 C55 H55A 110.6 . . ? C56 C55 H55A 110.6 . . ? O7 C55 H55B 110.6 . . ? C56 C55 H55B 110.6 . . ? H55A C55 H55B 108.7 . . ? C57 C56 C55 102.0(6) . . ? C57 C56 H56A 111.4 . . ? C55 C56 H56A 111.4 . . ? C57 C56 H56B 111.4 . . ? C55 C56 H56B 111.4 . . ? H56A C56 H56B 109.2 . . ? C58 C57 C56 102.9(6) . . ? C58 C57 H57A 111.2 . . ? C56 C57 H57A 111.2 . . ? C58 C57 H57B 111.2 . . ? C56 C57 H57B 111.2 . . ? H57A C57 H57B 109.1 . . ? O7 C58 C57 106.3(5) . . ? O7 C58 H58A 110.5 . . ? C57 C58 H58A 110.5 . . ? O7 C58 H58B 110.5 . . ? C57 C58 H58B 110.5 . . ? H58A C58 H58B 108.7 . . ? C60 C59 C64 118.8(8) . . ? C60 C59 C65 120.8(9) . . ? C64 C59 C65 120.5(8) . . ? C61 C60 C59 121.8(9) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C60 C61 C62 121.5(9) . . ? C60 C61 H61 119.3 . . ? C62 C61 H61 119.3 . . ? C61 C62 C63 118.2(8) . . ? C61 C62 H62 120.9 . . ? C63 C62 H62 120.9 . . ? C64 C63 C62 118.7(9) . . ? C64 C63 H63 120.6 . . ? C62 C63 H63 120.6 . . ? C59 C64 C63 121.1(8) . . ? C59 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C59 C65 H65A 109.5 . . ? C59 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C59 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 C68 92(3) 2_655 2_655 ? C67 C66 O8 79(2) 2_655 . ? C68 C66 O8 170(3) 2_655 . ? C67 C66 C67 42(3) 2_655 . ? C68 C66 C67 50.4(19) 2_655 . ? O8 C66 C67 121(2) . . ? C66 C67 C67 102(3) 2_655 2_655 ? C66 C67 C68 156(5) 2_655 2_655 ? C67 C67 C68 84(3) 2_655 2_655 ? C66 C67 C68 50.0(19) 2_655 . ? C67 C67 C68 52(2) 2_655 . ? C68 C67 C68 132(2) 2_655 . ? C66 C67 C66 133(4) 2_655 . ? C67 C67 C66 36(2) 2_655 . ? C68 C67 C66 47.8(15) 2_655 . ? C68 C67 C66 86.1(19) . . ? C66 C67 O8 65(2) 2_655 2_655 ? C67 C67 O8 168(4) 2_655 2_655 ? C68 C67 O8 108(2) 2_655 2_655 ? C68 C67 O8 115(2) . 2_655 ? C66 C67 O8 155(2) . 2_655 ? C66 C67 C69 113(3) 2_655 2_655 ? C67 C67 C69 144(4) 2_655 2_655 ? C68 C67 C69 61.1(16) 2_655 2_655 ? C68 C67 C69 163(2) . 2_655 ? C66 C67 C69 108.7(18) . 2_655 ? O8 C67 C69 48.5(10) 2_655 2_655 ? C66 C68 C67 82(2) 2_655 2_655 ? C66 C68 C67 38(2) 2_655 . ? C67 C68 C67 44(2) 2_655 . ? C66 C68 C69 157(3) 2_655 . ? C67 C68 C69 76.6(19) 2_655 . ? C67 C68 C69 120(2) . . ? O8 C69 C68 100.7(18) . . ? O8 C69 C67 59.7(15) . 2_655 ? C68 C69 C67 42.3(14) . 2_655 ? O2 Li1 O4 85.7(4) . . ? O2 Li1 O7 108.4(4) . . ? O4 Li1 O7 133.6(5) . . ? O2 Li1 O6 133.3(5) . . ? O4 Li1 O6 107.7(4) . . ? O7 Li1 O6 94.2(4) . . ? O2 Li1 Yb1 43.6(2) . . ? O4 Li1 Yb1 42.5(2) . . ? O7 Li1 Yb1 129.6(4) . . ? O6 Li1 Yb1 136.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.855 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.096 #==================================================END OF CIF