# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Zhang, Hui' _publ_contact_author_email huizhang@xmu.edu.cn _publ_section_title ; Structure-chiroptical property relationship of kinetically labile camphor-derivative b-diketone Yb(III) complexes: The adducts coexist as diastereomers or not? ; loop_ _publ_author_name 'Yiji Lin' 'Shigang Wan' 'Fang Zou' 'Yuekui Wang' 'Hui Zhang' #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_II _database_code_depnum_ccdc_archive 'CCDC 764761' #TrackingRef '- CIF-R.cif' # start Validation Reply Form _vrf_PLAT241_II ; PROBLEM: Check High Ueq as Compared to Neighbors for C34 RESPONSE: Many crystals tried, best presented - mobile alkyl chains lead to this anomalous value. ; _vrf_PLAT860_II ; PROBLEM: Note: Number of Least-Squares Restraints ....... 39 RESPONSE: Owing to the static disorder of the mobile alkyl chains, 39 least-squares restraints were used to refine the structure.The restraints are listed under _refine_special_details ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 F21 N0 O7 Yb1' _chemical_formula_weight 1232.81 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 '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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.575(5) _cell_length_b 13.191(3) _cell_length_c 31.096(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.925(4) _cell_angle_gamma 90.00 _cell_volume 10075(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9949 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 24.44 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4888 _exptl_absorpt_coefficient_mu 1.979 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6191 _exptl_absorpt_correction_T_max 0.8015 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27046 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18440 _reflns_number_gt 14522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. delu 0.01 F9 C18 delu 0.01 F42 C62 delu 0.01 F12 C20 delu 0.01 F7 C6 delu 0.01 F5 C6 delu 0.01 F28 C48 delu 0.01 F27 C48 DFIX 1.35 0.02 C20 F12 C20 F13 C20 F14 DFIX 2.10 0.02 F12 F13 F13 F14 F14 F12 DFIX 2.10 0.02 F40 F41 F41 F42 F42 F40 F26 F27 F27 F28 F28 F26 DFIX 1.35 0.02 C62 F40 C62 F41 C62 F42 C48 F26 C48 F27 C48 F28 DFIX 1.52 0.02 C60 C61 C61 C62 isor 0.01 C20 delu 0.01 F39 C61 delu 0.01 C18 C19 delu 0.01 C60 C61 delu 0.01 F20 C34 delu 0.01 F21 C34 ; _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^)+(0.0532P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(9) _refine_ls_number_reflns 18440 _refine_ls_number_parameters 1279 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8729(3) 0.7628(7) 0.8687(3) 0.061(2) Uani 1 1 d . . . C2 C 0.8882(3) 0.8696(6) 0.8659(3) 0.0565(19) Uani 1 1 d . . . C3 C 0.8523(3) 0.9415(7) 0.8525(3) 0.059(2) Uani 1 1 d . . . C4 C 0.8693(4) 1.0531(7) 0.8493(3) 0.074(3) Uani 1 1 d . . . C5 C 0.8607(7) 1.1127(11) 0.8913(4) 0.110(4) Uani 1 1 d . . . C6 C 0.8810(12) 1.2190(16) 0.8897(9) 0.179(7) Uani 1 1 d U . . C7 C 0.9102(4) 0.6007(8) 0.9003(3) 0.085(3) Uani 1 1 d . . . H7A H 0.8857 0.6057 0.9236 0.128 Uiso 1 1 calc R . . H7B H 0.9438 0.5705 0.9105 0.128 Uiso 1 1 calc R . . H7C H 0.8941 0.5593 0.8779 0.128 Uiso 1 1 calc R . . C8 C 0.9213(3) 0.7046(8) 0.8830(3) 0.064(2) Uani 1 1 d . . . C9 C 0.9585(3) 0.7083(9) 0.8450(3) 0.087(3) Uani 1 1 d . . . H9A H 0.9390 0.6889 0.8186 0.105 Uiso 1 1 calc R . . H9B H 0.9894 0.6632 0.8495 0.105 Uiso 1 1 calc R . . C10 C 0.9774(4) 0.8193(9) 0.8428(3) 0.092(3) Uani 1 1 d . . . H10A H 0.9672 0.8492 0.8152 0.110 Uiso 1 1 calc R . . H10B H 1.0165 0.8243 0.8473 0.110 Uiso 1 1 calc R . . C11 C 0.9473(3) 0.8721(8) 0.8798(3) 0.073(3) Uani 1 1 d . . . H11 H 0.9618 0.9380 0.8892 0.088 Uiso 1 1 calc R . . C12 C 0.9497(3) 0.7849(8) 0.9140(3) 0.076(2) Uani 1 1 d . . . C13 C 1.0067(4) 0.7536(10) 0.9315(4) 0.124(5) Uani 1 1 d . . . H13A H 1.0122 0.7792 0.9602 0.186 Uiso 1 1 calc R . . H13B H 1.0339 0.7812 0.9134 0.186 Uiso 1 1 calc R . . H13C H 1.0094 0.6810 0.9318 0.186 Uiso 1 1 calc R . . C14 C 0.9159(5) 0.8114(12) 0.9538(3) 0.119(4) Uani 1 1 d . . . H14A H 0.9147 0.7537 0.9726 0.178 Uiso 1 1 calc R . . H14B H 0.8796 0.8297 0.9445 0.178 Uiso 1 1 calc R . . H14C H 0.9326 0.8674 0.9690 0.178 Uiso 1 1 calc R . . C15 C 0.6693(3) 0.9622(6) 0.7886(3) 0.061(2) Uani 1 1 d . . . C16 C 0.6455(4) 1.0003(8) 0.8258(3) 0.068(2) Uani 1 1 d . . . C17 C 0.6565(4) 0.9609(9) 0.8655(3) 0.080(3) Uani 1 1 d . . . C18 C 0.6288(9) 1.0014(13) 0.9068(5) 0.159(7) Uani 1 1 d U . . C19 C 0.6143(8) 0.9284(18) 0.9396(5) 0.149(5) Uani 1 1 d U . . C20 C 0.5767(8) 0.9608(16) 0.9713(8) 0.197(9) Uani 1 1 d DU . . C21 C 0.6770(5) 1.0152(10) 0.7095(3) 0.111(4) Uani 1 1 d . . . H21A H 0.7137 1.0392 0.7137 0.166 Uiso 1 1 calc R . . H21B H 0.6588 1.0543 0.6873 0.166 Uiso 1 1 calc R . . H21C H 0.6775 0.9452 0.7012 0.166 Uiso 1 1 calc R . . C22 C 0.6468(4) 1.0265(7) 0.7516(3) 0.073(3) Uani 1 1 d . . . C23 C 0.5855(4) 0.9951(8) 0.7474(3) 0.086(3) Uani 1 1 d . . . H23A H 0.5688 1.0217 0.7210 0.103 Uiso 1 1 calc R . . H23B H 0.5817 0.9219 0.7474 0.103 Uiso 1 1 calc R . . C24 C 0.5599(4) 1.0404(11) 0.7859(4) 0.103(4) Uani 1 1 d . . . H24A H 0.5331 1.0914 0.7775 0.124 Uiso 1 1 calc R . . H24B H 0.5425 0.9888 0.8029 0.124 Uiso 1 1 calc R . . C25 C 0.6070(5) 1.0867(8) 0.8102(3) 0.088(3) Uani 1 1 d . . . H25 H 0.5974 1.1359 0.8324 0.106 Uiso 1 1 calc R . . C26 C 0.6407(5) 1.1292(8) 0.7738(4) 0.094(3) Uani 1 1 d . . . C27 C 0.6086(6) 1.2098(10) 0.7465(4) 0.130(5) Uani 1 1 d . . . H27A H 0.5960 1.2623 0.7651 0.194 Uiso 1 1 calc R . . H27B H 0.5780 1.1781 0.7320 0.194 Uiso 1 1 calc R . . H27C H 0.6321 1.2387 0.7257 0.194 Uiso 1 1 calc R . . C28 C 0.6967(6) 1.1717(12) 0.7896(6) 0.160(7) Uani 1 1 d . . . H28A H 0.7230 1.1605 0.7680 0.241 Uiso 1 1 calc R . . H28B H 0.7081 1.1379 0.8157 0.241 Uiso 1 1 calc R . . H28C H 0.6935 1.2431 0.7950 0.241 Uiso 1 1 calc R . . C29 C 0.7089(4) 0.6211(8) 0.9027(3) 0.073(3) Uani 1 1 d . . . C30 C 0.6763(4) 0.5662(7) 0.8712(3) 0.075(3) Uani 1 1 d . . . C31 C 0.6708(3) 0.5944(7) 0.8304(3) 0.065(2) Uani 1 1 d . . . C32 C 0.6332(5) 0.5359(9) 0.7971(4) 0.085(3) Uani 1 1 d . . . C33 C 0.5753(8) 0.5619(18) 0.7943(5) 0.149(5) Uani 1 1 d . . . C34 C 0.5586(11) 0.667(5) 0.7963(10) 0.38(2) Uani 1 1 d U . . C35 C 0.7496(6) 0.5982(13) 0.9777(3) 0.146(6) Uani 1 1 d . . . H35A H 0.7834 0.6093 0.9638 0.220 Uiso 1 1 calc R . . H35B H 0.7541 0.5454 0.9987 0.220 Uiso 1 1 calc R . . H35C H 0.7387 0.6596 0.9916 0.220 Uiso 1 1 calc R . . C36 C 0.7053(5) 0.5669(11) 0.9438(4) 0.102(4) Uani 1 1 d . . . C37 C 0.6475(7) 0.5843(14) 0.9568(5) 0.133(5) Uani 1 1 d . . . H37A H 0.6427 0.5609 0.9860 0.159 Uiso 1 1 calc R . . H37B H 0.6387 0.6559 0.9554 0.159 Uiso 1 1 calc R . . C38 C 0.6120(6) 0.5266(14) 0.9264(5) 0.141(7) Uani 1 1 d . . . H38A H 0.5878 0.5710 0.9099 0.169 Uiso 1 1 calc R . . H38B H 0.5906 0.4765 0.9412 0.169 Uiso 1 1 calc R . . C39 C 0.6552(6) 0.4751(10) 0.8971(5) 0.122(5) Uani 1 1 d . . . H39 H 0.6423 0.4167 0.8801 0.146 Uiso 1 1 calc R . . C40 C 0.7031(7) 0.4551(14) 0.9290(6) 0.149(7) Uani 1 1 d . . . C41 C 0.6907(9) 0.3723(14) 0.9655(5) 0.178(8) Uani 1 1 d . . . C42 C 0.7541(7) 0.4255(12) 0.9060(5) 0.156(7) Uani 1 1 d . . . H42A H 0.7458 0.3716 0.8861 0.235 Uiso 1 1 calc R . . H42B H 0.7815 0.4032 0.9266 0.235 Uiso 1 1 calc R . . H42C H 0.7674 0.4830 0.8906 0.235 Uiso 1 1 calc R . . C43 C 0.6124(3) 0.7349(6) 0.6217(2) 0.056(2) Uani 1 1 d . . . C44 C 0.5998(3) 0.6299(8) 0.6221(3) 0.069(2) Uani 1 1 d . . . C45 C 0.6361(4) 0.5601(7) 0.6373(3) 0.076(3) Uani 1 1 d . . . C46 C 0.6195(5) 0.4430(9) 0.6431(4) 0.089(3) Uani 1 1 d . . . C47 C 0.6315(9) 0.3848(12) 0.6051(6) 0.153(8) Uani 1 1 d . . . C48 C 0.6187(8) 0.2694(13) 0.6034(6) 0.176(8) Uani 1 1 d DU . . C49 C 0.5635(4) 0.8991(10) 0.6098(5) 0.125(5) Uani 1 1 d . . . H49A H 0.5715 0.9118 0.6398 0.187 Uiso 1 1 calc R . . H49B H 0.5283 0.9266 0.6020 0.187 Uiso 1 1 calc R . . H49C H 0.5906 0.9308 0.5928 0.187 Uiso 1 1 calc R . . C50 C 0.5634(4) 0.7878(10) 0.6018(3) 0.084(3) Uani 1 1 d . . . C51 C 0.5631(5) 0.7482(11) 0.5545(4) 0.116(5) Uani 1 1 d . . . H51A H 0.5377 0.7872 0.5365 0.139 Uiso 1 1 calc R . . H51B H 0.5991 0.7540 0.5429 0.139 Uiso 1 1 calc R . . C52 C 0.5460(5) 0.6406(13) 0.5559(3) 0.125(5) Uani 1 1 d . . . H52A H 0.5730 0.5964 0.5436 0.151 Uiso 1 1 calc R . . H52B H 0.5112 0.6302 0.5410 0.151 Uiso 1 1 calc R . . C53 C 0.5422(4) 0.6240(9) 0.6043(4) 0.084(3) Uani 1 1 d . . . H53 H 0.5229 0.5621 0.6121 0.101 Uiso 1 1 calc R . . C54 C 0.5170(3) 0.7177(10) 0.6193(3) 0.085(3) Uani 1 1 d . . . C55 C 0.4602(4) 0.7456(10) 0.6008(5) 0.133(5) Uani 1 1 d . . . H55A H 0.4631 0.7678 0.5716 0.199 Uiso 1 1 calc R . . H55B H 0.4452 0.7991 0.6176 0.199 Uiso 1 1 calc R . . H55C H 0.4369 0.6873 0.6017 0.199 Uiso 1 1 calc R . . C56 C 0.5148(5) 0.7235(16) 0.6679(3) 0.141(5) Uani 1 1 d . . . H56A H 0.4906 0.6722 0.6780 0.211 Uiso 1 1 calc R . . H56B H 0.5019 0.7891 0.6761 0.211 Uiso 1 1 calc R . . H56C H 0.5506 0.7127 0.6804 0.211 Uiso 1 1 calc R . . C57 C 0.8071(3) 0.5349(6) 0.7059(3) 0.0542(18) Uani 1 1 d . . . C58 C 0.8277(4) 0.4959(7) 0.6678(3) 0.077(3) Uani 1 1 d . . . C59 C 0.8212(4) 0.5439(9) 0.6302(4) 0.093(4) Uani 1 1 d . . . C60 C 0.8406(7) 0.4950(18) 0.5866(5) 0.178(7) Uani 1 1 d DU . . C61 C 0.8896(8) 0.5517(17) 0.5752(5) 0.178(7) Uani 1 1 d DU . . C62 C 0.9175(7) 0.5491(19) 0.5328(6) 0.38(2) Uani 1 1 d DU . . C63 C 0.8172(5) 0.5009(11) 0.7862(3) 0.116(5) Uani 1 1 d . . . H63A H 0.8466 0.5467 0.7932 0.175 Uiso 1 1 calc R . . H63B H 0.8190 0.4439 0.8054 0.175 Uiso 1 1 calc R . . H63C H 0.7831 0.5352 0.7890 0.175 Uiso 1 1 calc R . . C64 C 0.8219(4) 0.4651(7) 0.7413(3) 0.071(3) Uani 1 1 d . . . C65 C 0.7842(6) 0.3734(10) 0.7300(5) 0.130(5) Uani 1 1 d . . . H65A H 0.7845 0.3256 0.7538 0.156 Uiso 1 1 calc R . . H65B H 0.7471 0.3964 0.7246 0.156 Uiso 1 1 calc R . . C66 C 0.8053(7) 0.3240(9) 0.6908(6) 0.158(7) Uani 1 1 d . . . H66A H 0.7782 0.3232 0.6674 0.190 Uiso 1 1 calc R . . H66B H 0.8177 0.2554 0.6966 0.190 Uiso 1 1 calc R . . C67 C 0.8536(5) 0.3959(9) 0.6810(4) 0.100(4) Uani 1 1 d . . . H67 H 0.8802 0.3689 0.6612 0.120 Uiso 1 1 calc R . . C68 C 0.8762(4) 0.4239(8) 0.7255(3) 0.082(3) Uani 1 1 d . . . C69 C 0.9011(6) 0.3325(9) 0.7508(4) 0.128(5) Uani 1 1 d . . . H69A H 0.9283 0.3005 0.7340 0.192 Uiso 1 1 calc R . . H69B H 0.8729 0.2845 0.7567 0.192 Uiso 1 1 calc R . . H69C H 0.9175 0.3560 0.7775 0.192 Uiso 1 1 calc R . . C70 C 0.9205(4) 0.5040(12) 0.7251(4) 0.112(4) Uani 1 1 d . . . H70A H 0.9552 0.4719 0.7220 0.167 Uiso 1 1 calc R . . H70B H 0.9208 0.5412 0.7517 0.167 Uiso 1 1 calc R . . H70C H 0.9136 0.5496 0.7015 0.167 Uiso 1 1 calc R . . C71 C 0.7748(4) 0.8965(8) 0.5980(3) 0.071(2) Uani 1 1 d . . . C72 C 0.8047(4) 0.9513(8) 0.6302(3) 0.071(2) Uani 1 1 d . . . C73 C 0.8109(3) 0.9180(6) 0.6717(3) 0.059(2) Uani 1 1 d . . . C74 C 0.8466(4) 0.9720(7) 0.7041(3) 0.074(3) Uani 1 1 d . . . C75 C 0.9086(5) 0.9465(9) 0.7024(4) 0.095(4) Uani 1 1 d . . . C76 C 0.9240(4) 0.8391(11) 0.7050(4) 0.096(4) Uani 1 1 d . . . C77 C 0.7605(6) 0.9011(12) 0.5161(3) 0.136(5) Uani 1 1 d . . . H77A H 0.7217 0.8965 0.5124 0.203 Uiso 1 1 calc R . . H77B H 0.7758 0.8342 0.5179 0.203 Uiso 1 1 calc R . . H77C H 0.7751 0.9362 0.4921 0.203 Uiso 1 1 calc R . . C78 C 0.7745(5) 0.9578(10) 0.5565(3) 0.098(4) Uani 1 1 d . . . C79 C 0.7364(5) 1.0451(10) 0.5658(4) 0.108(4) Uani 1 1 d . . . H79A H 0.7023 1.0203 0.5765 0.129 Uiso 1 1 calc R . . H79B H 0.7289 1.0848 0.5400 0.129 Uiso 1 1 calc R . . C80 C 0.7680(6) 1.1114(10) 0.6014(4) 0.125(5) Uani 1 1 d . . . H80A H 0.7751 1.1793 0.5909 0.150 Uiso 1 1 calc R . . H80B H 0.7477 1.1159 0.6275 0.150 Uiso 1 1 calc R . . C81 C 0.8228(5) 1.0500(10) 0.6092(4) 0.099(4) Uani 1 1 d . . . H81 H 0.8529 1.0864 0.6238 0.119 Uiso 1 1 calc R . . C82 C 0.8337(6) 1.0078(11) 0.5626(4) 0.109(5) Uani 1 1 d . . . C83 C 0.8414(6) 1.0960(12) 0.5284(4) 0.136(6) Uani 1 1 d . . . H83A H 0.8222 1.1554 0.5372 0.205 Uiso 1 1 calc R . . H83B H 0.8273 1.0743 0.5007 0.205 Uiso 1 1 calc R . . H83C H 0.8795 1.1115 0.5265 0.205 Uiso 1 1 calc R . . C84 C 0.8796(7) 0.9326(17) 0.5594(6) 0.167(8) Uani 1 1 d . . . H84A H 0.8757 0.8803 0.5805 0.251 Uiso 1 1 calc R . . H84B H 0.9138 0.9666 0.5644 0.251 Uiso 1 1 calc R . . H84C H 0.8786 0.9029 0.5312 0.251 Uiso 1 1 calc R . . F1 F 0.9214(3) 1.0594(5) 0.8387(2) 0.107(2) Uani 1 1 d . . . F2 F 0.8397(3) 1.0990(4) 0.81800(18) 0.0963(18) Uani 1 1 d . . . F3 F 0.8916(6) 1.0671(8) 0.9225(3) 0.193(5) Uani 1 1 d . . . F4 F 0.8070(5) 1.1129(10) 0.9024(4) 0.210(6) Uani 1 1 d . . . F5 F 0.9349(8) 1.2142(17) 0.8882(10) 0.414(18) Uani 1 1 d U . . F6 F 0.8671(8) 1.2580(11) 0.9305(4) 0.294(10) Uani 1 1 d . . . F7 F 0.8615(10) 1.2711(10) 0.8632(5) 0.299(12) Uani 1 1 d U . . F8 F 0.5651(5) 1.0165(14) 0.8939(3) 0.272(10) Uani 1 1 d . . . F9 F 0.6409(9) 1.0882(11) 0.9147(5) 0.285(11) Uani 1 1 d U . . F10 F 0.6688(6) 0.9306(18) 0.9549(4) 0.353(15) Uani 1 1 d . . . F11 F 0.5934(4) 0.8370(9) 0.9170(4) 0.183(5) Uani 1 1 d . . . F12 F 0.5870(8) 0.8927(13) 0.9991(5) 0.371(14) Uani 1 1 d DU . . F13 F 0.5924(8) 1.0497(12) 0.9821(5) 0.315(11) Uani 1 1 d D . . F14 F 0.5260(6) 0.9569(19) 0.9613(5) 0.343(13) Uani 1 1 d D . . F15 F 0.6352(4) 0.4378(6) 0.8032(3) 0.160(4) Uani 1 1 d . . . F16 F 0.6506(3) 0.5523(7) 0.7562(2) 0.124(3) Uani 1 1 d . . . F17 F 0.5514(3) 0.5286(8) 0.8344(3) 0.181(4) Uani 1 1 d . . . F18 F 0.5506(4) 0.5150(9) 0.7614(4) 0.200(5) Uani 1 1 d . . . F19 F 0.5727(3) 0.7131(9) 0.8323(3) 0.151(3) Uani 1 1 d . . . F20 F 0.5047(3) 0.6837(10) 0.7910(3) 0.199(5) Uani 1 1 d U . . F21 F 0.5819(3) 0.7149(9) 0.7641(3) 0.141(3) Uani 1 1 d U . . F22 F 0.6495(3) 0.4020(5) 0.6747(2) 0.111(2) Uani 1 1 d . . . F23 F 0.5689(3) 0.4308(5) 0.6512(3) 0.128(3) Uani 1 1 d . . . F24 F 0.6854(5) 0.3963(10) 0.5949(4) 0.221(7) Uani 1 1 d . . . F25 F 0.6063(6) 0.4268(9) 0.5700(3) 0.227(7) Uani 1 1 d . . . F26 F 0.5691(6) 0.2581(9) 0.6098(8) 0.345(13) Uani 1 1 d D . . F27 F 0.6476(9) 0.2233(12) 0.6306(4) 0.302(11) Uani 1 1 d DU . . F28 F 0.6313(7) 0.2374(11) 0.5660(4) 0.273(8) Uani 1 1 d DU . . F29 F 0.8307(3) 0.9544(5) 0.74395(18) 0.0912(18) Uani 1 1 d . . . F30 F 0.8443(4) 1.0755(5) 0.6982(2) 0.118(2) Uani 1 1 d . . . F31 F 0.9335(4) 0.9947(8) 0.7365(2) 0.153(4) Uani 1 1 d . . . F32 F 0.9279(3) 0.9842(7) 0.6653(2) 0.141(3) Uani 1 1 d . . . F33 F 0.9042(3) 0.7954(8) 0.7395(2) 0.132(2) Uani 1 1 d . . . F34 F 0.9766(3) 0.8302(9) 0.7080(3) 0.164(4) Uani 1 1 d . . . F35 F 0.9052(3) 0.7858(7) 0.6714(3) 0.133(2) Uani 1 1 d . . . F36 F 0.8099(5) 0.5376(14) 0.5517(3) 0.268(9) Uani 1 1 d . . . F37 F 0.8479(5) 0.4049(8) 0.5872(3) 0.173(5) Uani 1 1 d . . . F38 F 0.8933(5) 0.6682(8) 0.5814(5) 0.223(7) Uani 1 1 d . . . F39 F 0.9296(4) 0.5128(11) 0.6087(3) 0.194(5) Uani 1 1 d U . . F40 F 0.8937(8) 0.592(2) 0.5027(6) 0.44(2) Uani 1 1 d D . . F41 F 0.9127(11) 0.4512(14) 0.5321(7) 0.374(14) Uani 1 1 d D . . F42 F 0.9666(6) 0.578(2) 0.5391(4) 0.390(16) Uani 1 1 d DU . . O1W O 0.7911(2) 0.7613(4) 0.77527(16) 0.0594(14) Uani 1 1 d . . . O1 O 0.82705(19) 0.7245(5) 0.86077(17) 0.0620(13) Uani 1 1 d . . . O2 O 0.8008(2) 0.9284(4) 0.84437(18) 0.0619(14) Uani 1 1 d . . . O3 O 0.7002(2) 0.8896(4) 0.78520(17) 0.0616(14) Uani 1 1 d . . . O4 O 0.6880(3) 0.8885(6) 0.87366(19) 0.082(2) Uani 1 1 d . . . O5 O 0.7324(2) 0.7013(6) 0.89714(17) 0.0775(17) Uani 1 1 d . . . O6 O 0.6942(2) 0.6713(4) 0.81257(17) 0.0593(14) Uani 1 1 d . . . O2W O 0.6889(2) 0.7468(4) 0.72118(18) 0.0634(15) Uani 1 1 d . . . O7 O 0.6559(2) 0.7743(4) 0.6320(2) 0.0681(17) Uani 1 1 d . . . O8 O 0.6854(2) 0.5768(4) 0.6499(2) 0.0681(16) Uani 1 1 d . . . O11 O 0.7523(2) 0.8125(5) 0.60103(17) 0.0744(17) Uani 1 1 d . . . O12 O 0.7894(2) 0.8369(4) 0.68636(15) 0.0501(12) Uani 1 1 d . . . O9 O 0.7800(2) 0.6162(4) 0.71021(17) 0.0584(14) Uani 1 1 d . . . O10 O 0.7961(2) 0.6286(5) 0.62304(19) 0.0742(17) Uani 1 1 d . . . Yb1 Yb 0.746537(12) 0.79644(2) 0.838196(10) 0.05445(9) Uani 1 1 d . . . Yb2 Yb 0.736219(12) 0.71389(2) 0.658243(10) 0.05411(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(5) 0.080(7) 0.052(4) 0.007(4) 0.006(4) 0.000(4) C2 0.054(5) 0.058(5) 0.058(5) 0.003(4) -0.001(4) -0.003(4) C3 0.062(6) 0.066(6) 0.051(5) -0.002(4) 0.011(4) -0.011(4) C4 0.079(7) 0.055(6) 0.088(7) 0.003(5) -0.006(5) -0.004(4) C5 0.146(13) 0.098(10) 0.085(8) -0.007(7) -0.008(8) 0.011(9) C6 0.275(19) 0.054(9) 0.21(2) -0.033(10) 0.030(17) -0.022(14) C7 0.087(7) 0.078(7) 0.090(7) 0.024(5) -0.015(5) 0.019(5) C8 0.041(4) 0.061(5) 0.088(6) 0.003(5) -0.004(4) 0.010(4) C9 0.065(5) 0.106(7) 0.090(6) -0.023(6) 0.001(4) 0.009(6) C10 0.057(5) 0.120(10) 0.098(7) 0.015(6) 0.016(5) -0.010(5) C11 0.035(4) 0.091(7) 0.093(6) -0.024(5) -0.008(4) -0.001(4) C12 0.068(5) 0.088(7) 0.071(5) 0.002(5) -0.016(4) 0.016(5) C13 0.072(7) 0.140(12) 0.156(11) -0.039(8) -0.048(7) 0.018(6) C14 0.129(9) 0.158(12) 0.069(6) 0.006(7) -0.011(6) 0.035(9) C15 0.045(4) 0.055(5) 0.084(6) -0.002(4) -0.001(4) 0.009(4) C16 0.064(5) 0.079(6) 0.061(5) -0.006(5) 0.003(4) 0.006(5) C17 0.065(6) 0.110(8) 0.067(6) -0.001(5) 0.022(5) 0.030(5) C18 0.26(2) 0.103(9) 0.117(11) -0.001(7) 0.014(11) 0.081(11) C19 0.144(11) 0.212(14) 0.092(7) -0.009(7) 0.029(7) 0.021(10) C20 0.212(13) 0.199(12) 0.180(12) 0.009(8) 0.015(9) 0.022(9) C21 0.151(11) 0.098(9) 0.086(8) 0.016(6) 0.035(7) 0.052(8) C22 0.080(7) 0.060(6) 0.081(6) 0.012(5) 0.017(5) 0.025(5) C23 0.085(7) 0.085(7) 0.088(7) -0.004(5) -0.021(6) 0.018(5) C24 0.047(6) 0.145(11) 0.117(9) 0.005(8) -0.006(6) 0.022(6) C25 0.104(8) 0.069(6) 0.092(7) -0.017(5) 0.012(6) 0.038(6) C26 0.117(9) 0.053(6) 0.111(9) 0.013(6) -0.006(7) 0.020(6) C27 0.192(13) 0.062(7) 0.133(10) 0.035(7) -0.018(9) 0.028(9) C28 0.140(13) 0.119(14) 0.219(18) 0.022(11) -0.054(12) -0.043(9) C29 0.064(5) 0.083(7) 0.074(6) 0.033(5) 0.012(4) 0.005(5) C30 0.099(7) 0.055(6) 0.072(6) 0.023(5) 0.020(5) -0.001(5) C31 0.052(5) 0.061(6) 0.082(6) 0.006(5) 0.014(4) -0.011(4) C32 0.087(8) 0.068(7) 0.100(9) 0.000(6) 0.009(6) -0.007(5) C33 0.144(11) 0.212(14) 0.092(7) -0.009(7) 0.029(7) 0.021(10) C34 0.162(10) 0.76(6) 0.24(2) 0.29(3) 0.123(13) 0.20(2) C35 0.151(12) 0.215(18) 0.072(7) 0.078(9) -0.002(8) 0.004(11) C36 0.105(9) 0.111(10) 0.091(8) 0.045(7) 0.025(7) 0.013(7) C37 0.133(13) 0.167(15) 0.099(9) 0.055(10) 0.015(9) -0.016(11) C38 0.101(10) 0.207(17) 0.116(11) 0.091(12) 0.032(9) -0.032(11) C39 0.156(13) 0.091(9) 0.121(10) 0.047(8) 0.050(10) -0.023(8) C40 0.151(14) 0.145(15) 0.154(14) 0.090(12) 0.030(11) 0.038(11) C41 0.27(2) 0.145(15) 0.119(11) 0.075(11) 0.028(13) -0.012(15) C42 0.196(17) 0.122(12) 0.154(13) 0.067(10) 0.052(12) 0.064(11) C43 0.035(4) 0.067(6) 0.067(5) 0.007(4) -0.003(3) 0.008(3) C44 0.046(5) 0.085(7) 0.074(6) -0.013(5) -0.014(4) 0.002(5) C45 0.063(6) 0.055(6) 0.109(8) 0.002(5) -0.012(5) -0.008(4) C46 0.081(8) 0.087(8) 0.098(8) -0.002(7) -0.014(6) -0.007(6) C47 0.22(2) 0.085(11) 0.150(15) -0.018(10) -0.102(15) -0.001(12) C48 0.22(2) 0.088(15) 0.215(16) -0.048(12) -0.071(14) -0.001(13) C49 0.059(7) 0.114(11) 0.198(14) 0.001(10) -0.039(8) 0.031(6) C50 0.065(6) 0.087(8) 0.098(7) 0.036(7) -0.011(5) 0.014(6) C51 0.098(9) 0.139(12) 0.109(9) 0.059(8) -0.028(7) 0.002(7) C52 0.099(9) 0.207(17) 0.068(7) -0.036(9) -0.019(6) 0.031(10) C53 0.053(5) 0.085(7) 0.112(8) -0.004(6) -0.014(5) 0.007(5) C54 0.050(5) 0.107(7) 0.099(7) -0.019(7) -0.005(4) -0.006(6) C55 0.056(6) 0.122(11) 0.219(15) -0.012(9) -0.019(8) 0.003(6) C56 0.090(8) 0.240(16) 0.094(8) -0.012(11) 0.020(6) 0.007(11) C57 0.054(5) 0.046(5) 0.063(5) -0.003(4) 0.001(4) 0.002(3) C58 0.095(7) 0.058(6) 0.075(6) -0.013(5) -0.021(5) 0.032(5) C59 0.091(7) 0.090(8) 0.095(8) -0.045(6) -0.013(6) 0.040(6) C60 0.192(13) 0.265(18) 0.081(7) 0.023(9) 0.057(7) 0.123(14) C61 0.192(13) 0.265(18) 0.081(7) 0.023(9) 0.057(7) 0.123(14) C62 0.162(10) 0.76(6) 0.24(2) 0.29(3) 0.123(13) 0.20(2) C63 0.123(10) 0.139(12) 0.087(8) 0.045(8) 0.008(7) 0.056(8) C64 0.077(6) 0.054(5) 0.081(6) 0.012(5) 0.001(5) 0.017(4) C65 0.127(11) 0.082(9) 0.178(14) 0.037(9) -0.044(10) -0.023(8) C66 0.209(17) 0.035(7) 0.223(18) -0.028(8) -0.087(14) -0.002(7) C67 0.130(10) 0.073(8) 0.097(8) -0.008(6) 0.004(7) 0.051(7) C68 0.078(7) 0.073(7) 0.095(8) 0.013(5) 0.010(5) 0.037(5) C69 0.159(12) 0.095(10) 0.129(10) 0.012(7) -0.007(9) 0.073(8) C70 0.065(7) 0.149(12) 0.120(10) 0.027(9) -0.006(6) 0.004(7) C71 0.067(6) 0.081(7) 0.066(6) 0.022(5) 0.011(4) 0.001(5) C72 0.066(6) 0.073(6) 0.072(6) 0.002(5) 0.000(5) 0.002(4) C73 0.063(5) 0.056(5) 0.060(5) 0.004(4) 0.002(4) 0.002(4) C74 0.089(7) 0.059(6) 0.075(6) -0.005(5) 0.011(5) -0.020(5) C75 0.081(7) 0.079(8) 0.123(10) 0.012(6) -0.025(7) -0.038(6) C76 0.058(6) 0.140(12) 0.091(8) 0.019(7) -0.005(5) -0.006(6) C77 0.174(14) 0.152(13) 0.079(8) 0.022(8) -0.022(8) -0.033(11) C78 0.102(8) 0.114(10) 0.077(7) 0.042(6) -0.005(6) -0.012(7) C79 0.110(9) 0.107(9) 0.106(9) 0.038(7) 0.000(7) 0.026(7) C80 0.172(13) 0.090(9) 0.113(10) 0.048(7) 0.003(9) 0.004(9) C81 0.112(9) 0.091(8) 0.095(8) 0.025(6) -0.005(7) -0.019(7) C82 0.141(12) 0.113(10) 0.071(7) 0.040(7) -0.002(7) -0.050(9) C83 0.167(14) 0.141(14) 0.101(9) 0.035(9) 0.002(9) -0.052(11) C84 0.106(12) 0.25(2) 0.147(15) -0.032(15) 0.056(11) -0.022(14) F1 0.087(4) 0.078(4) 0.156(6) -0.005(4) 0.025(4) -0.019(3) F2 0.130(5) 0.061(4) 0.097(4) 0.014(3) -0.012(4) -0.014(3) F3 0.320(15) 0.123(7) 0.128(7) -0.048(6) -0.094(8) 0.052(8) F4 0.195(11) 0.210(12) 0.233(12) -0.108(10) 0.106(10) -0.035(9) F5 0.290(18) 0.217(19) 0.74(5) -0.22(3) 0.13(3) -0.128(19) F6 0.46(2) 0.222(17) 0.190(11) -0.119(11) -0.075(13) 0.110(15) F7 0.62(4) 0.091(10) 0.183(12) -0.006(7) 0.021(16) -0.018(14) F8 0.254(13) 0.43(2) 0.135(8) 0.074(11) 0.062(8) 0.240(16) F9 0.46(3) 0.180(12) 0.227(14) -0.106(11) 0.187(17) -0.059(14) F10 0.212(12) 0.69(4) 0.155(9) -0.231(17) -0.097(9) 0.243(19) F11 0.181(9) 0.179(11) 0.195(10) -0.013(8) 0.096(8) -0.035(7) F12 0.51(3) 0.37(2) 0.242(15) 0.147(15) 0.193(18) 0.21(2) F13 0.49(3) 0.31(2) 0.153(11) -0.011(12) 0.106(15) 0.15(2) F14 0.219(16) 0.54(4) 0.267(17) 0.03(2) -0.022(12) 0.14(2) F15 0.225(10) 0.056(5) 0.196(9) 0.001(5) -0.030(7) -0.040(5) F16 0.141(7) 0.144(7) 0.088(5) -0.039(4) 0.025(4) -0.051(5) F17 0.109(6) 0.213(10) 0.222(10) 0.109(8) 0.006(6) -0.067(6) F18 0.142(8) 0.229(12) 0.225(10) -0.048(9) -0.073(7) -0.091(8) F19 0.136(6) 0.179(8) 0.137(6) 0.001(7) 0.019(5) 0.071(7) F20 0.063(4) 0.283(15) 0.250(10) 0.099(10) 0.001(5) 0.003(6) F21 0.103(5) 0.160(7) 0.159(7) 0.042(7) -0.010(4) -0.017(6) F22 0.156(6) 0.073(4) 0.103(4) 0.024(3) -0.025(4) -0.017(4) F23 0.085(4) 0.088(5) 0.212(8) 0.027(5) 0.022(5) -0.031(3) F24 0.214(11) 0.235(14) 0.220(12) -0.143(11) 0.121(10) -0.076(11) F25 0.398(19) 0.165(10) 0.111(6) -0.046(6) -0.084(9) 0.086(11) F26 0.275(17) 0.114(10) 0.65(4) -0.126(15) 0.06(2) -0.074(11) F27 0.55(3) 0.126(10) 0.225(13) -0.030(10) -0.099(15) 0.103(15) F28 0.45(2) 0.152(11) 0.216(12) -0.079(10) -0.057(13) 0.016(13) F29 0.128(5) 0.082(4) 0.064(3) -0.004(3) 0.013(3) -0.025(3) F30 0.186(7) 0.063(4) 0.103(5) -0.001(3) -0.017(5) -0.037(4) F31 0.153(7) 0.187(9) 0.116(6) 0.008(5) -0.032(5) -0.095(7) F32 0.106(5) 0.213(9) 0.104(5) 0.045(5) 0.012(4) -0.071(5) F33 0.114(5) 0.160(7) 0.124(5) 0.052(6) 0.011(4) -0.005(6) F34 0.070(4) 0.245(12) 0.175(7) 0.008(7) -0.011(4) 0.010(5) F35 0.115(5) 0.143(7) 0.140(6) -0.011(6) -0.005(4) 0.031(5) F36 0.246(13) 0.46(2) 0.097(6) -0.136(10) -0.075(7) 0.185(14) F37 0.252(12) 0.139(8) 0.127(7) -0.058(6) -0.008(7) 0.085(8) F38 0.192(10) 0.132(9) 0.357(18) 0.043(9) 0.157(11) 0.023(7) F39 0.156(8) 0.310(14) 0.118(6) 0.011(7) 0.024(5) 0.093(9) F40 0.37(3) 0.71(5) 0.239(17) 0.16(2) 0.041(17) 0.27(3) F41 0.58(4) 0.29(2) 0.26(2) -0.020(17) 0.09(2) 0.10(3) F42 0.256(16) 0.72(5) 0.206(14) 0.17(2) 0.154(13) 0.12(2) O1W 0.054(3) 0.074(4) 0.051(3) 0.004(2) 0.016(2) 0.005(2) O1 0.044(3) 0.054(3) 0.087(4) 0.019(3) -0.008(2) 0.010(3) O2 0.054(3) 0.048(3) 0.084(4) -0.001(3) -0.006(3) -0.012(2) O3 0.061(3) 0.067(4) 0.057(3) 0.012(3) 0.008(3) 0.019(3) O4 0.078(4) 0.105(5) 0.063(4) -0.001(4) 0.015(3) 0.048(4) O5 0.083(4) 0.087(5) 0.063(3) 0.025(4) -0.006(3) -0.006(4) O6 0.044(3) 0.065(4) 0.069(4) 0.000(3) 0.005(2) -0.016(2) O2W 0.046(3) 0.072(4) 0.073(3) 0.000(3) 0.017(2) 0.006(2) O7 0.033(3) 0.061(4) 0.109(4) 0.022(3) -0.014(3) 0.005(2) O8 0.047(3) 0.042(3) 0.115(5) 0.000(3) -0.012(3) -0.005(2) O11 0.074(4) 0.087(5) 0.062(3) 0.023(3) -0.010(3) -0.021(3) O12 0.048(3) 0.045(3) 0.057(3) 0.008(2) -0.005(2) -0.013(2) O9 0.055(3) 0.054(4) 0.066(3) 0.008(3) 0.002(3) 0.013(2) O10 0.062(4) 0.091(5) 0.070(4) -0.009(3) 0.013(3) 0.021(3) Yb1 0.04421(17) 0.0579(2) 0.06119(19) 0.00861(16) 0.00138(12) 0.00169(15) Yb2 0.04217(16) 0.05415(19) 0.0657(2) 0.00529(17) -0.00250(13) -0.00085(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.251(9) . ? C1 C2 1.463(12) . ? C1 C8 1.472(11) . ? C2 C3 1.351(12) . ? C2 C11 1.502(11) . ? C3 O2 1.294(9) . ? C3 C4 1.535(13) . ? C4 F1 1.336(11) . ? C4 F2 1.340(11) . ? C4 C5 1.545(17) . ? C5 F3 1.354(16) . ? C5 F4 1.374(18) . ? C5 C6 1.49(2) . ? C6 F7 1.16(3) . ? C6 F5 1.33(3) . ? C6 F6 1.42(2) . ? C7 C8 1.500(14) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.519(12) . ? C8 C12 1.580(13) . ? C9 C10 1.538(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.550(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.566(15) . ? C11 H11 0.9800 . ? C12 C13 1.542(12) . ? C12 C14 1.555(14) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O3 1.229(9) . ? C15 C16 1.406(12) . ? C15 C22 1.520(13) . ? C16 C17 1.358(13) . ? C16 C25 1.549(13) . ? C17 O4 1.249(11) . ? C17 C18 1.567(18) . ? C18 F9 1.21(2) . ? C18 C19 1.46(2) . ? C18 F8 1.62(2) . ? C19 F10 1.41(2) . ? C19 C20 1.44(3) . ? C19 F11 1.48(2) . ? C20 F12 1.266(17) . ? C20 F13 1.276(17) . ? C20 F14 1.277(17) . ? C21 C22 1.533(14) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C26 1.530(15) . ? C22 C23 1.563(15) . ? C23 C24 1.496(15) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.493(16) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.533(16) . ? C25 H25 0.9800 . ? C26 C28 1.549(17) . ? C26 C27 1.558(14) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O5 1.221(11) . ? C29 C30 1.441(14) . ? C29 C36 1.469(14) . ? C30 C31 1.323(13) . ? C30 C39 1.545(14) . ? C31 O6 1.299(10) . ? C31 C32 1.570(14) . ? C32 F15 1.309(13) . ? C32 F16 1.374(13) . ? C32 C33 1.46(2) . ? C33 F18 1.32(2) . ? C33 C34 1.44(6) . ? C33 F17 1.464(18) . ? C34 F19 1.31(5) . ? C34 F21 1.33(3) . ? C34 F20 1.35(2) . ? C35 C36 1.544(18) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.507(19) . ? C36 C40 1.55(2) . ? C37 C38 1.48(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.58(2) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.54(2) . ? C39 H39 0.9800 . ? C40 C42 1.52(2) . ? C40 C41 1.610(19) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O7 1.222(9) . ? C43 C44 1.419(14) . ? C43 C50 1.507(11) . ? C44 C45 1.357(14) . ? C44 C53 1.504(12) . ? C45 O8 1.279(10) . ? C45 C46 1.609(15) . ? C46 F23 1.287(13) . ? C46 F22 1.324(12) . ? C46 C47 1.45(2) . ? C47 F25 1.355(17) . ? C47 F24 1.38(2) . ? C47 C48 1.56(2) . ? C48 F27 1.243(15) . ? C48 F26 1.250(16) . ? C48 F28 1.285(15) . ? C49 C50 1.490(18) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.560(18) . ? C50 C54 1.579(15) . ? C51 C52 1.481(19) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.526(15) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.466(15) . ? C53 H53 0.9800 . ? C54 C56 1.515(13) . ? C54 C55 1.537(13) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O9 1.272(9) . ? C57 C58 1.401(12) . ? C57 C64 1.472(12) . ? C58 C59 1.334(15) . ? C58 C67 1.515(13) . ? C59 O10 1.292(12) . ? C59 C60 1.590(18) . ? C60 F37 1.20(2) . ? C60 F36 1.417(18) . ? C60 C61 1.470(18) . ? C61 F39 1.498(18) . ? C61 C62 1.507(16) . ? C61 F38 1.55(2) . ? C62 F40 1.228(16) . ? C62 F42 1.276(17) . ? C62 F41 1.297(18) . ? C63 C64 1.481(15) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C68 1.538(13) . ? C64 C65 1.556(16) . ? C65 C66 1.49(2) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.56(2) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.520(15) . ? C67 H67 0.9800 . ? C68 C70 1.517(17) . ? C68 C69 1.555(13) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 O11 1.243(11) . ? C71 C72 1.420(13) . ? C71 C78 1.522(13) . ? C72 C73 1.367(12) . ? C72 C81 1.529(15) . ? C73 O12 1.284(9) . ? C73 C74 1.495(12) . ? C74 F29 1.331(11) . ? C74 F30 1.378(11) . ? C74 C75 1.563(16) . ? C75 F32 1.357(14) . ? C75 F31 1.363(13) . ? C75 C76 1.468(18) . ? C76 F34 1.299(12) . ? C76 F33 1.325(13) . ? C76 F35 1.328(14) . ? C77 C78 1.491(17) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 C79 1.518(17) . ? C78 C82 1.603(17) . ? C79 C80 1.593(19) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 C81 1.582(18) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C82 1.583(18) . ? C81 H81 0.9800 . ? C82 C84 1.51(2) . ? C82 C83 1.594(16) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? O1W Yb1 2.321(5) . ? O1 Yb1 2.283(5) . ? O2 Yb1 2.198(5) . ? O3 Yb1 2.323(5) . ? O4 Yb1 2.206(5) . ? O5 Yb1 2.258(6) . ? O6 Yb1 2.224(5) . ? O2W Yb2 2.351(5) . ? O7 Yb2 2.255(5) . ? O8 Yb2 2.209(5) . ? O11 Yb2 2.250(6) . ? O12 Yb2 2.243(5) . ? O9 Yb2 2.306(5) . ? O10 Yb2 2.176(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 127.5(8) . . ? O1 C1 C8 124.2(8) . . ? C2 C1 C8 108.3(8) . . ? C3 C2 C1 121.8(8) . . ? C3 C2 C11 133.5(8) . . ? C1 C2 C11 104.6(8) . . ? O2 C3 C2 126.2(8) . . ? O2 C3 C4 112.4(8) . . ? C2 C3 C4 121.1(8) . . ? F1 C4 F2 107.1(9) . . ? F1 C4 C3 109.9(8) . . ? F2 C4 C3 109.8(8) . . ? F1 C4 C5 109.8(10) . . ? F2 C4 C5 107.2(9) . . ? C3 C4 C5 112.8(9) . . ? F3 C5 F4 109.9(15) . . ? F3 C5 C6 105.1(17) . . ? F4 C5 C6 109.5(15) . . ? F3 C5 C4 106.9(11) . . ? F4 C5 C4 112.0(12) . . ? C6 C5 C4 113.2(14) . . ? F7 C6 F5 113(3) . . ? F7 C6 F6 108(2) . . ? F5 C6 F6 109(3) . . ? F7 C6 C5 117(3) . . ? F5 C6 C5 107(2) . . ? F6 C6 C5 102.7(18) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 C7 115.5(7) . . ? C1 C8 C9 104.4(7) . . ? C7 C8 C9 115.4(9) . . ? C1 C8 C12 99.8(7) . . ? C7 C8 C12 118.4(8) . . ? C9 C8 C12 100.8(7) . . ? C8 C9 C10 104.7(8) . . ? C8 C9 H9A 110.8 . . ? C10 C9 H9A 110.8 . . ? C8 C9 H9B 110.8 . . ? C10 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? C9 C10 C11 104.1(8) . . ? C9 C10 H10A 110.9 . . ? C11 C10 H10A 110.9 . . ? C9 C10 H10B 110.9 . . ? C11 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C2 C11 C10 105.0(7) . . ? C2 C11 C12 101.1(7) . . ? C10 C11 C12 99.5(8) . . ? C2 C11 H11 116.3 . . ? C10 C11 H11 116.3 . . ? C12 C11 H11 116.3 . . ? C13 C12 C14 106.4(8) . . ? C13 C12 C11 116.7(9) . . ? C14 C12 C11 111.6(9) . . ? C13 C12 C8 114.4(9) . . ? C14 C12 C8 113.6(9) . . ? C11 C12 C8 94.2(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 128.7(9) . . ? O3 C15 C22 125.4(8) . . ? C16 C15 C22 105.8(7) . . ? C17 C16 C15 122.3(9) . . ? C17 C16 C25 131.9(9) . . ? C15 C16 C25 105.8(8) . . ? O4 C17 C16 125.5(8) . . ? O4 C17 C18 112.1(9) . . ? C16 C17 C18 122.3(10) . . ? F9 C18 C19 123.2(19) . . ? F9 C18 C17 112.4(18) . . ? C19 C18 C17 118.2(14) . . ? F9 C18 F8 99.4(15) . . ? C19 C18 F8 89.8(17) . . ? C17 C18 F8 106.4(13) . . ? F10 C19 C20 112.8(15) . . ? F10 C19 C18 88.3(18) . . ? C20 C19 C18 117.6(19) . . ? F10 C19 F11 119.3(18) . . ? C20 C19 F11 110.3(17) . . ? C18 C19 F11 107.2(14) . . ? F12 C20 F13 115(2) . . ? F12 C20 F14 108.0(18) . . ? F13 C20 F14 112.6(19) . . ? F12 C20 C19 98.0(18) . . ? F13 C20 C19 105(2) . . ? F14 C20 C19 118(2) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 C26 101.0(8) . . ? C15 C22 C21 114.7(8) . . ? C26 C22 C21 121.8(9) . . ? C15 C22 C23 104.0(8) . . ? C26 C22 C23 99.4(8) . . ? C21 C22 C23 113.4(10) . . ? C24 C23 C22 104.9(8) . . ? C24 C23 H23A 110.8 . . ? C22 C23 H23A 110.8 . . ? C24 C23 H23B 110.8 . . ? C22 C23 H23B 110.8 . . ? H23A C23 H23B 108.8 . . ? C25 C24 C23 103.2(8) . . ? C25 C24 H24A 111.1 . . ? C23 C24 H24A 111.1 . . ? C25 C24 H24B 111.1 . . ? C23 C24 H24B 111.1 . . ? H24A C24 H24B 109.1 . . ? C24 C25 C26 101.8(9) . . ? C24 C25 C16 108.2(9) . . ? C26 C25 C16 99.3(8) . . ? C24 C25 H25 115.2 . . ? C26 C25 H25 115.2 . . ? C16 C25 H25 115.2 . . ? C22 C26 C25 94.2(8) . . ? C22 C26 C28 111.4(11) . . ? C25 C26 C28 113.1(11) . . ? C22 C26 C27 114.5(10) . . ? C25 C26 C27 112.1(10) . . ? C28 C26 C27 110.7(11) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 C30 126.4(8) . . ? O5 C29 C36 126.0(11) . . ? C30 C29 C36 107.5(10) . . ? C31 C30 C29 123.1(9) . . ? C31 C30 C39 133.9(11) . . ? C29 C30 C39 103.0(10) . . ? O6 C31 C30 126.7(9) . . ? O6 C31 C32 111.1(8) . . ? C30 C31 C32 122.2(9) . . ? F15 C32 F16 106.2(10) . . ? F15 C32 C33 105.9(14) . . ? F16 C32 C33 103.9(11) . . ? F15 C32 C31 111.7(10) . . ? F16 C32 C31 109.8(8) . . ? C33 C32 C31 118.4(12) . . ? F18 C33 C34 111(3) . . ? F18 C33 C32 111.0(15) . . ? C34 C33 C32 120(2) . . ? F18 C33 F17 109.2(17) . . ? C34 C33 F17 97.3(15) . . ? C32 C33 F17 107.2(14) . . ? F19 C34 F21 108(5) . . ? F19 C34 F20 105(3) . . ? F21 C34 F20 105.9(19) . . ? F19 C34 C33 115(2) . . ? F21 C34 C33 107(3) . . ? F20 C34 C33 116(5) . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C29 C36 C37 104.1(10) . . ? C29 C36 C35 113.7(11) . . ? C37 C36 C35 115.1(13) . . ? C29 C36 C40 102.0(11) . . ? C37 C36 C40 101.6(13) . . ? C35 C36 C40 118.4(12) . . ? C38 C37 C36 107.0(15) . . ? C38 C37 H37A 110.3 . . ? C36 C37 H37A 110.3 . . ? C38 C37 H37B 110.3 . . ? C36 C37 H37B 110.3 . . ? H37A C37 H37B 108.6 . . ? C37 C38 C39 101.3(13) . . ? 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 C30 102.0(11) . . ? C40 C39 C38 102.5(13) . . ? C30 C39 C38 102.2(11) . . ? C40 C39 H39 116.0 . . ? C30 C39 H39 116.0 . . ? C38 C39 H39 116.0 . . ? C42 C40 C39 111.4(15) . . ? C42 C40 C36 111.4(14) . . ? C39 C40 C36 92.6(11) . . ? C42 C40 C41 109.7(13) . . ? C39 C40 C41 114.4(15) . . ? C36 C40 C41 116.3(14) . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O7 C43 C44 126.9(7) . . ? O7 C43 C50 126.3(9) . . ? C44 C43 C50 106.5(8) . . ? C45 C44 C43 121.6(8) . . ? C45 C44 C53 133.9(10) . . ? C43 C44 C53 104.5(8) . . ? O8 C45 C44 126.5(9) . . ? O8 C45 C46 111.9(8) . . ? C44 C45 C46 121.6(9) . . ? F23 C46 F22 108.6(11) . . ? F23 C46 C47 108.6(12) . . ? F22 C46 C47 105.4(11) . . ? F23 C46 C45 113.1(9) . . ? F22 C46 C45 109.7(8) . . ? C47 C46 C45 111.1(12) . . ? F25 C47 F24 100.7(19) . . ? F25 C47 C46 109.9(15) . . ? F24 C47 C46 110.6(12) . . ? F25 C47 C48 106.7(12) . . ? F24 C47 C48 107.1(17) . . ? C46 C47 C48 120.0(18) . . ? F27 C48 F26 111.8(18) . . ? F27 C48 F28 107.8(15) . . ? F26 C48 F28 111.7(15) . . ? F27 C48 C47 110.2(15) . . ? F26 C48 C47 107.9(16) . . ? F28 C48 C47 107.3(17) . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C49 C50 C43 113.0(9) . . ? C49 C50 C51 119.2(10) . . ? C43 C50 C51 102.2(9) . . ? C49 C50 C54 121.1(10) . . ? C43 C50 C54 99.4(8) . . ? C51 C50 C54 98.6(10) . . ? C52 C51 C50 106.5(10) . . ? C52 C51 H51A 110.4 . . ? C50 C51 H51A 110.4 . . ? C52 C51 H51B 110.4 . . ? C50 C51 H51B 110.4 . . ? H51A C51 H51B 108.6 . . ? C51 C52 C53 101.2(10) . . ? C51 C52 H52A 111.5 . . ? C53 C52 H52A 111.5 . . ? C51 C52 H52B 111.5 . . ? C53 C52 H52B 111.5 . . ? H52A C52 H52B 109.3 . . ? C54 C53 C44 103.9(8) . . ? C54 C53 C52 103.6(10) . . ? C44 C53 C52 105.5(9) . . ? C54 C53 H53 114.2 . . ? C44 C53 H53 114.2 . . ? C52 C53 H53 114.2 . . ? C53 C54 C56 113.0(12) . . ? C53 C54 C55 118.1(9) . . ? C56 C54 C55 107.4(9) . . ? C53 C54 C50 93.8(8) . . ? C56 C54 C50 111.5(9) . . ? C55 C54 C50 112.8(10) . . ? 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 . . ? O9 C57 C58 127.2(8) . . ? O9 C57 C64 124.3(8) . . ? C58 C57 C64 108.4(7) . . ? C59 C58 C57 122.0(8) . . ? C59 C58 C67 133.4(9) . . ? C57 C58 C67 104.5(9) . . ? O10 C59 C58 127.2(9) . . ? O10 C59 C60 111.1(11) . . ? C58 C59 C60 121.6(11) . . ? F37 C60 F36 118.8(18) . . ? F37 C60 C61 112.6(16) . . ? F36 C60 C61 91.9(15) . . ? F37 C60 C59 115.8(14) . . ? F36 C60 C59 108.9(12) . . ? C61 C60 C59 105.6(15) . . ? C60 C61 F39 100.5(14) . . ? C60 C61 C62 126.8(17) . . ? F39 C61 C62 106.9(13) . . ? C60 C61 F38 121.4(13) . . ? F39 C61 F38 102.6(16) . . ? C62 C61 F38 96.0(16) . . ? F40 C62 F42 113.6(17) . . ? F40 C62 F41 114.1(19) . . ? F42 C62 F41 112.9(18) . . ? F40 C62 C61 116.0(18) . . ? F42 C62 C61 108.4(17) . . ? F41 C62 C61 89.7(17) . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C57 C64 C63 118.8(8) . . ? C57 C64 C68 100.2(8) . . ? C63 C64 C68 120.6(9) . . ? C57 C64 C65 100.8(8) . . ? C63 C64 C65 113.3(11) . . ? C68 C64 C65 99.8(10) . . ? C66 C65 C64 107.6(12) . . ? C66 C65 H65A 110.2 . . ? C64 C65 H65A 110.2 . . ? C66 C65 H65B 110.2 . . ? C64 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? C65 C66 C67 100.5(9) . . ? C65 C66 H66A 111.7 . . ? C67 C66 H66A 111.7 . . ? C65 C66 H66B 111.7 . . ? C67 C66 H66B 111.7 . . ? H66A C66 H66B 109.4 . . ? C58 C67 C68 99.9(8) . . ? C58 C67 C66 105.4(10) . . ? C68 C67 C66 103.2(11) . . ? C58 C67 H67 115.5 . . ? C68 C67 H67 115.5 . . ? C66 C67 H67 115.5 . . ? C70 C68 C67 113.8(10) . . ? C70 C68 C64 112.8(9) . . ? C67 C68 C64 94.7(8) . . ? C70 C68 C69 105.9(10) . . ? C67 C68 C69 113.5(9) . . ? C64 C68 C69 116.3(10) . . ? 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 . . ? O11 C71 C72 128.4(8) . . ? O11 C71 C78 123.2(9) . . ? C72 C71 C78 108.4(9) . . ? C73 C72 C71 122.8(9) . . ? C73 C72 C81 130.6(9) . . ? C71 C72 C81 106.5(9) . . ? O12 C73 C72 124.7(8) . . ? O12 C73 C74 113.4(7) . . ? C72 C73 C74 121.9(8) . . ? F29 C74 F30 106.5(8) . . ? F29 C74 C73 111.1(8) . . ? F30 C74 C73 111.2(8) . . ? F29 C74 C75 108.2(9) . . ? F30 C74 C75 104.2(8) . . ? C73 C74 C75 115.1(9) . . ? F32 C75 F31 109.3(8) . . ? F32 C75 C76 107.6(12) . . ? F31 C75 C76 107.5(11) . . ? F32 C75 C74 108.6(9) . . ? F31 C75 C74 106.6(11) . . ? C76 C75 C74 117.1(8) . . ? F34 C76 F33 107.2(10) . . ? F34 C76 F35 109.2(11) . . ? F33 C76 F35 106.2(11) . . ? F34 C76 C75 110.2(11) . . ? F33 C76 C75 111.2(12) . . ? F35 C76 C75 112.7(10) . . ? C78 C77 H77A 109.5 . . ? C78 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C78 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C77 C78 C79 114.5(11) . . ? C77 C78 C71 116.2(11) . . ? C79 C78 C71 103.2(9) . . ? C77 C78 C82 119.3(11) . . ? C79 C78 C82 103.1(11) . . ? C71 C78 C82 98.0(8) . . ? C78 C79 C80 105.1(10) . . ? 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 . . ? C81 C80 C79 102.6(11) . . ? C81 C80 H80A 111.2 . . ? C79 C80 H80A 111.2 . . ? C81 C80 H80B 111.2 . . ? C79 C80 H80B 111.2 . . ? H80A C80 H80B 109.2 . . ? C72 C81 C80 104.1(9) . . ? C72 C81 C82 98.7(9) . . ? C80 C81 C82 102.0(10) . . ? C72 C81 H81 116.5 . . ? C80 C81 H81 116.5 . . ? C82 C81 H81 116.5 . . ? C84 C82 C81 116.3(11) . . ? C84 C82 C83 109.2(13) . . ? C81 C82 C83 112.5(12) . . ? C84 C82 C78 113.5(13) . . ? C81 C82 C78 94.2(10) . . ? C83 C82 C78 110.5(10) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C1 O1 Yb1 131.1(6) . . ? C3 O2 Yb1 135.2(5) . . ? C15 O3 Yb1 129.8(6) . . ? C17 O4 Yb1 136.7(6) . . ? C29 O5 Yb1 133.2(6) . . ? C31 O6 Yb1 133.2(6) . . ? C43 O7 Yb2 133.9(6) . . ? C45 O8 Yb2 134.6(5) . . ? C71 O11 Yb2 131.8(6) . . ? C73 O12 Yb2 134.9(5) . . ? C57 O9 Yb2 129.1(5) . . ? C59 O10 Yb2 133.4(7) . . ? O2 Yb1 O4 85.7(3) . . ? O2 Yb1 O6 164.0(2) . . ? O4 Yb1 O6 102.0(2) . . ? O2 Yb1 O5 118.6(2) . . ? O4 Yb1 O5 77.2(3) . . ? O6 Yb1 O5 77.0(2) . . ? O2 Yb1 O1 77.6(2) . . ? O4 Yb1 O1 130.4(2) . . ? O6 Yb1 O1 106.6(2) . . ? O5 Yb1 O1 71.0(2) . . ? O2 Yb1 O1W 86.0(2) . . ? O4 Yb1 O1W 150.0(2) . . ? O6 Yb1 O1W 80.40(19) . . ? O5 Yb1 O1W 131.5(2) . . ? O1 Yb1 O1W 75.37(19) . . ? O2 Yb1 O3 85.7(2) . . ? O4 Yb1 O3 75.6(2) . . ? O6 Yb1 O3 82.8(2) . . ? O5 Yb1 O3 141.7(2) . . ? O1 Yb1 O3 146.80(19) . . ? O1W Yb1 O3 75.03(18) . . ? O10 Yb2 O8 84.7(2) . . ? O10 Yb2 O12 100.1(2) . . ? O8 Yb2 O12 163.4(2) . . ? O10 Yb2 O11 76.2(3) . . ? O8 Yb2 O11 119.6(2) . . ? O12 Yb2 O11 76.95(19) . . ? O10 Yb2 O7 126.8(2) . . ? O8 Yb2 O7 76.2(2) . . ? O12 Yb2 O7 112.16(19) . . ? O11 Yb2 O7 71.6(2) . . ? O10 Yb2 O9 75.9(2) . . ? O8 Yb2 O9 82.7(2) . . ? O12 Yb2 O9 83.05(19) . . ? O11 Yb2 O9 141.9(2) . . ? O7 Yb2 O9 146.4(2) . . ? O10 Yb2 O2W 151.2(2) . . ? O8 Yb2 O2W 87.4(2) . . ? O12 Yb2 O2W 80.82(19) . . ? O11 Yb2 O2W 131.1(2) . . ? O7 Yb2 O2W 77.5(2) . . ? O9 Yb2 O2W 75.65(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -2.1(14) . . . . ? C8 C1 C2 C3 178.3(8) . . . . ? O1 C1 C2 C11 178.9(8) . . . . ? C8 C1 C2 C11 -0.7(9) . . . . ? C1 C2 C3 O2 6.5(14) . . . . ? C11 C2 C3 O2 -174.8(8) . . . . ? C1 C2 C3 C4 -179.3(8) . . . . ? C11 C2 C3 C4 -0.6(15) . . . . ? O2 C3 C4 F1 -152.3(8) . . . . ? C2 C3 C4 F1 32.7(12) . . . . ? O2 C3 C4 F2 -34.7(11) . . . . ? C2 C3 C4 F2 150.3(8) . . . . ? O2 C3 C4 C5 84.8(11) . . . . ? C2 C3 C4 C5 -90.2(11) . . . . ? F1 C4 C5 F3 -62.8(15) . . . . ? F2 C4 C5 F3 -178.8(12) . . . . ? C3 C4 C5 F3 60.2(15) . . . . ? F1 C4 C5 F4 176.9(11) . . . . ? F2 C4 C5 F4 60.9(14) . . . . ? C3 C4 C5 F4 -60.2(14) . . . . ? F1 C4 C5 C6 52.5(19) . . . . ? F2 C4 C5 C6 -63.5(19) . . . . ? C3 C4 C5 C6 175.5(17) . . . . ? F3 C5 C6 F7 176(2) . . . . ? F4 C5 C6 F7 -66(3) . . . . ? C4 C5 C6 F7 60(3) . . . . ? F3 C5 C6 F5 49(3) . . . . ? F4 C5 C6 F5 167(2) . . . . ? C4 C5 C6 F5 -68(3) . . . . ? F3 C5 C6 F6 -66(2) . . . . ? F4 C5 C6 F6 52(2) . . . . ? C4 C5 C6 F6 178.2(15) . . . . ? O1 C1 C8 C7 -17.3(12) . . . . ? C2 C1 C8 C7 162.3(8) . . . . ? O1 C1 C8 C9 110.6(9) . . . . ? C2 C1 C8 C9 -69.8(9) . . . . ? O1 C1 C8 C12 -145.5(8) . . . . ? C2 C1 C8 C12 34.2(9) . . . . ? C1 C8 C9 C10 69.2(9) . . . . ? C7 C8 C9 C10 -162.8(8) . . . . ? C12 C8 C9 C10 -34.0(9) . . . . ? C8 C9 C10 C11 -1.7(10) . . . . ? C3 C2 C11 C10 -109.2(11) . . . . ? C1 C2 C11 C10 69.7(9) . . . . ? C3 C2 C11 C12 147.7(10) . . . . ? C1 C2 C11 C12 -33.5(8) . . . . ? C9 C10 C11 C2 -67.4(10) . . . . ? C9 C10 C11 C12 36.9(9) . . . . ? C2 C11 C12 C13 171.7(8) . . . . ? C10 C11 C12 C13 64.3(10) . . . . ? C2 C11 C12 C14 -65.7(9) . . . . ? C10 C11 C12 C14 -173.1(8) . . . . ? C2 C11 C12 C8 51.7(8) . . . . ? C10 C11 C12 C8 -55.8(7) . . . . ? C1 C8 C12 C13 -173.3(9) . . . . ? C7 C8 C12 C13 60.5(12) . . . . ? C9 C8 C12 C13 -66.4(11) . . . . ? C1 C8 C12 C14 64.2(10) . . . . ? C7 C8 C12 C14 -62.0(11) . . . . ? C9 C8 C12 C14 171.1(8) . . . . ? C1 C8 C12 C11 -51.5(8) . . . . ? C7 C8 C12 C11 -177.7(7) . . . . ? C9 C8 C12 C11 55.4(8) . . . . ? O3 C15 C16 C17 3.1(16) . . . . ? C22 C15 C16 C17 -179.8(10) . . . . ? O3 C15 C16 C25 -175.6(9) . . . . ? C22 C15 C16 C25 1.5(10) . . . . ? C15 C16 C17 O4 -0.2(18) . . . . ? C25 C16 C17 O4 178.2(11) . . . . ? C15 C16 C17 C18 -178.4(13) . . . . ? C25 C16 C17 C18 0(2) . . . . ? O4 C17 C18 F9 117.4(19) . . . . ? C16 C17 C18 F9 -64(3) . . . . ? O4 C17 C18 C19 -36(2) . . . . ? C16 C17 C18 C19 142.5(16) . . . . ? O4 C17 C18 F8 -134.8(12) . . . . ? C16 C17 C18 F8 44(2) . . . . ? F9 C18 C19 F10 -69(3) . . . . ? C17 C18 C19 F10 81(2) . . . . ? F8 C18 C19 F10 -170.3(13) . . . . ? F9 C18 C19 C20 46(3) . . . . ? C17 C18 C19 C20 -164.0(17) . . . . ? F8 C18 C19 C20 -55(2) . . . . ? F9 C18 C19 F11 171(2) . . . . ? C17 C18 C19 F11 -39(2) . . . . ? F8 C18 C19 F11 69.5(15) . . . . ? F10 C19 C20 F12 -61(3) . . . . ? C18 C19 C20 F12 -162(2) . . . . ? F11 C19 C20 F12 75(2) . . . . ? F10 C19 C20 F13 57(3) . . . . ? C18 C19 C20 F13 -43(3) . . . . ? F11 C19 C20 F13 -166.7(16) . . . . ? F10 C19 C20 F14 -177(2) . . . . ? C18 C19 C20 F14 83(3) . . . . ? F11 C19 C20 F14 -41(3) . . . . ? O3 C15 C22 C26 -149.4(9) . . . . ? C16 C15 C22 C26 33.4(10) . . . . ? O3 C15 C22 C21 -16.5(15) . . . . ? C16 C15 C22 C21 166.3(9) . . . . ? O3 C15 C22 C23 107.9(10) . . . . ? C16 C15 C22 C23 -69.3(9) . . . . ? C15 C22 C23 C24 71.7(10) . . . . ? C26 C22 C23 C24 -32.2(11) . . . . ? C21 C22 C23 C24 -163.0(9) . . . . ? C22 C23 C24 C25 -3.6(12) . . . . ? C23 C24 C25 C26 38.5(11) . . . . ? C23 C24 C25 C16 -65.4(12) . . . . ? C17 C16 C25 C24 -108.4(13) . . . . ? C15 C16 C25 C24 70.1(11) . . . . ? C17 C16 C25 C26 145.8(12) . . . . ? C15 C16 C25 C26 -35.6(10) . . . . ? C15 C22 C26 C25 -53.2(9) . . . . ? C21 C22 C26 C25 178.4(10) . . . . ? C23 C22 C26 C25 53.2(9) . . . . ? C15 C22 C26 C28 63.6(12) . . . . ? C21 C22 C26 C28 -64.8(14) . . . . ? C23 C22 C26 C28 170.0(10) . . . . ? C15 C22 C26 C27 -169.8(10) . . . . ? C21 C22 C26 C27 61.8(15) . . . . ? C23 C22 C26 C27 -63.4(12) . . . . ? C24 C25 C26 C22 -57.8(9) . . . . ? C16 C25 C26 C22 53.1(9) . . . . ? C24 C25 C26 C28 -173.2(11) . . . . ? C16 C25 C26 C28 -62.3(12) . . . . ? C24 C25 C26 C27 60.7(12) . . . . ? C16 C25 C26 C27 171.7(9) . . . . ? O5 C29 C30 C31 4.7(17) . . . . ? C36 C29 C30 C31 -179.6(10) . . . . ? O5 C29 C30 C39 -177.2(10) . . . . ? C36 C29 C30 C39 -1.5(12) . . . . ? C29 C30 C31 O6 2.0(17) . . . . ? C39 C30 C31 O6 -175.4(11) . . . . ? C29 C30 C31 C32 -177.4(9) . . . . ? C39 C30 C31 C32 5.1(19) . . . . ? O6 C31 C32 F15 142.2(10) . . . . ? C30 C31 C32 F15 -38.2(15) . . . . ? O6 C31 C32 F16 24.7(12) . . . . ? C30 C31 C32 F16 -155.8(10) . . . . ? O6 C31 C32 C33 -94.4(14) . . . . ? C30 C31 C32 C33 85.1(16) . . . . ? F15 C32 C33 F18 -61.2(19) . . . . ? F16 C32 C33 F18 50.5(19) . . . . ? C31 C32 C33 F18 172.6(13) . . . . ? F15 C32 C33 C34 167(2) . . . . ? F16 C32 C33 C34 -81(2) . . . . ? C31 C32 C33 C34 41(3) . . . . ? F15 C32 C33 F17 58.0(17) . . . . ? F16 C32 C33 F17 169.7(12) . . . . ? C31 C32 C33 F17 -68.2(19) . . . . ? F18 C33 C34 F19 167(2) . . . . ? C32 C33 C34 F19 -61(3) . . . . ? F17 C33 C34 F19 53(3) . . . . ? F18 C33 C34 F21 -73(3) . . . . ? C32 C33 C34 F21 59(4) . . . . ? F17 C33 C34 F21 173(2) . . . . ? F18 C33 C34 F20 45(3) . . . . ? C32 C33 C34 F20 176.4(14) . . . . ? F17 C33 C34 F20 -69(3) . . . . ? O5 C29 C36 C37 106.1(14) . . . . ? C30 C29 C36 C37 -69.6(14) . . . . ? O5 C29 C36 C35 -20.0(17) . . . . ? C30 C29 C36 C35 164.3(11) . . . . ? O5 C29 C36 C40 -148.5(12) . . . . ? C30 C29 C36 C40 35.7(13) . . . . ? C29 C36 C37 C38 69.4(15) . . . . ? C35 C36 C37 C38 -165.5(11) . . . . ? C40 C36 C37 C38 -36.3(13) . . . . ? C36 C37 C38 C39 1.4(14) . . . . ? C31 C30 C39 C40 144.4(14) . . . . ? C29 C30 C39 C40 -33.3(14) . . . . ? C31 C30 C39 C38 -109.8(15) . . . . ? C29 C30 C39 C38 72.5(13) . . . . ? C37 C38 C39 C40 34.3(13) . . . . ? C37 C38 C39 C30 -71.1(13) . . . . ? C30 C39 C40 C42 -62.5(17) . . . . ? C38 C39 C40 C42 -168.1(13) . . . . ? C30 C39 C40 C36 51.7(12) . . . . ? C38 C39 C40 C36 -53.9(12) . . . . ? C30 C39 C40 C41 172.2(13) . . . . ? C38 C39 C40 C41 66.7(17) . . . . ? C29 C36 C40 C42 61.3(15) . . . . ? C37 C36 C40 C42 168.6(12) . . . . ? C35 C36 C40 C42 -64.3(16) . . . . ? C29 C36 C40 C39 -53.0(11) . . . . ? C37 C36 C40 C39 54.4(12) . . . . ? C35 C36 C40 C39 -178.5(11) . . . . ? C29 C36 C40 C41 -171.9(14) . . . . ? C37 C36 C40 C41 -64.6(17) . . . . ? C35 C36 C40 C41 62.5(19) . . . . ? O7 C43 C44 C45 4.2(15) . . . . ? C50 C43 C44 C45 178.6(9) . . . . ? O7 C43 C44 C53 -177.1(8) . . . . ? C50 C43 C44 C53 -2.7(10) . . . . ? C43 C44 C45 O8 -5.1(17) . . . . ? C53 C44 C45 O8 176.7(10) . . . . ? C43 C44 C45 C46 172.6(9) . . . . ? C53 C44 C45 C46 -5.7(18) . . . . ? O8 C45 C46 F23 148.2(10) . . . . ? C44 C45 C46 F23 -29.8(16) . . . . ? O8 C45 C46 F22 26.8(13) . . . . ? C44 C45 C46 F22 -151.2(10) . . . . ? O8 C45 C46 C47 -89.3(13) . . . . ? C44 C45 C46 C47 92.7(14) . . . . ? F23 C46 C47 F25 69.2(19) . . . . ? F22 C46 C47 F25 -174.5(15) . . . . ? C45 C46 C47 F25 -55.8(19) . . . . ? F23 C46 C47 F24 179.6(13) . . . . ? F22 C46 C47 F24 -64.2(17) . . . . ? C45 C46 C47 F24 54.6(17) . . . . ? F23 C46 C47 C48 -54.9(18) . . . . ? F22 C46 C47 C48 61.3(18) . . . . ? C45 C46 C47 C48 -179.9(13) . . . . ? F25 C47 C48 F27 169.0(19) . . . . ? F24 C47 C48 F27 62(2) . . . . ? C46 C47 C48 F27 -65(2) . . . . ? F25 C47 C48 F26 -69(2) . . . . ? F24 C47 C48 F26 -175.8(18) . . . . ? C46 C47 C48 F26 57(2) . . . . ? F25 C47 C48 F28 52(2) . . . . ? F24 C47 C48 F28 -55.2(18) . . . . ? C46 C47 C48 F28 177.6(15) . . . . ? O7 C43 C50 C49 -21.5(14) . . . . ? C44 C43 C50 C49 164.0(10) . . . . ? O7 C43 C50 C51 107.8(11) . . . . ? C44 C43 C50 C51 -66.6(10) . . . . ? O7 C43 C50 C54 -151.2(9) . . . . ? C44 C43 C50 C54 34.4(10) . . . . ? C49 C50 C51 C52 -162.9(10) . . . . ? C43 C50 C51 C52 71.8(12) . . . . ? C54 C50 C51 C52 -29.8(11) . . . . ? C50 C51 C52 C53 -4.3(12) . . . . ? C45 C44 C53 C54 145.1(12) . . . . ? C43 C44 C53 C54 -33.3(11) . . . . ? C45 C44 C53 C52 -106.2(14) . . . . ? C43 C44 C53 C52 75.3(11) . . . . ? C51 C52 C53 C54 40.9(11) . . . . ? C51 C52 C53 C44 -68.0(12) . . . . ? C44 C53 C54 C56 -63.4(12) . . . . ? C52 C53 C54 C56 -173.5(10) . . . . ? C44 C53 C54 C55 170.1(10) . . . . ? C52 C53 C54 C55 60.0(13) . . . . ? C44 C53 C54 C50 51.8(9) . . . . ? C52 C53 C54 C50 -58.3(9) . . . . ? C49 C50 C54 C53 -175.9(10) . . . . ? C43 C50 C54 C53 -51.7(9) . . . . ? C51 C50 C54 C53 52.2(9) . . . . ? C49 C50 C54 C56 -59.4(14) . . . . ? C43 C50 C54 C56 64.7(12) . . . . ? C51 C50 C54 C56 168.7(10) . . . . ? C49 C50 C54 C55 61.5(13) . . . . ? C43 C50 C54 C55 -174.3(9) . . . . ? C51 C50 C54 C55 -70.4(11) . . . . ? O9 C57 C58 C59 1.1(16) . . . . ? C64 C57 C58 C59 -179.1(11) . . . . ? O9 C57 C58 C67 -177.2(9) . . . . ? C64 C57 C58 C67 2.6(11) . . . . ? C57 C58 C59 O10 -0.5(19) . . . . ? C67 C58 C59 O10 177.2(12) . . . . ? C57 C58 C59 C60 -175.1(12) . . . . ? C67 C58 C59 C60 3(2) . . . . ? O10 C59 C60 F37 -156.7(15) . . . . ? C58 C59 C60 F37 19(2) . . . . ? O10 C59 C60 F36 -20(2) . . . . ? C58 C59 C60 F36 155.7(15) . . . . ? O10 C59 C60 C61 77.9(15) . . . . ? C58 C59 C60 C61 -106.7(16) . . . . ? F37 C60 C61 F39 -55.4(17) . . . . ? F36 C60 C61 F39 -177.8(13) . . . . ? C59 C60 C61 F39 72.0(14) . . . . ? F37 C60 C61 C62 65(3) . . . . ? F36 C60 C61 C62 -57(2) . . . . ? C59 C60 C61 C62 -167.5(16) . . . . ? F37 C60 C61 F38 -167.3(15) . . . . ? F36 C60 C61 F38 70.3(17) . . . . ? C59 C60 C61 F38 -40(2) . . . . ? C60 C61 C62 F40 73(3) . . . . ? F39 C61 C62 F40 -170(2) . . . . ? F38 C61 C62 F40 -64(2) . . . . ? C60 C61 C62 F42 -158(2) . . . . ? F39 C61 C62 F42 -41(2) . . . . ? F38 C61 C62 F42 65(2) . . . . ? C60 C61 C62 F41 -44(2) . . . . ? F39 C61 C62 F41 74(2) . . . . ? F38 C61 C62 F41 178.7(17) . . . . ? O9 C57 C64 C63 -15.4(14) . . . . ? C58 C57 C64 C63 164.8(10) . . . . ? O9 C57 C64 C68 -148.9(8) . . . . ? C58 C57 C64 C68 31.3(10) . . . . ? O9 C57 C64 C65 109.0(10) . . . . ? C58 C57 C64 C65 -70.8(11) . . . . ? C57 C64 C65 C66 70.5(11) . . . . ? C63 C64 C65 C66 -161.5(10) . . . . ? C68 C64 C65 C66 -32.0(12) . . . . ? C64 C65 C66 C67 -2.3(13) . . . . ? C59 C58 C67 C68 146.0(13) . . . . ? C57 C58 C67 C68 -36.0(11) . . . . ? C59 C58 C67 C66 -107.2(16) . . . . ? C57 C58 C67 C66 70.8(11) . . . . ? C65 C66 C67 C58 -67.6(12) . . . . ? C65 C66 C67 C68 36.8(11) . . . . ? C58 C67 C68 C70 -64.9(12) . . . . ? C66 C67 C68 C70 -173.5(9) . . . . ? C58 C67 C68 C64 52.5(10) . . . . ? C66 C67 C68 C64 -56.1(9) . . . . ? C58 C67 C68 C69 173.9(10) . . . . ? C66 C67 C68 C69 65.3(12) . . . . ? C57 C64 C68 C70 67.3(11) . . . . ? C63 C64 C68 C70 -65.1(13) . . . . ? C65 C64 C68 C70 170.3(10) . . . . ? C57 C64 C68 C67 -51.0(9) . . . . ? C63 C64 C68 C67 176.7(11) . . . . ? C65 C64 C68 C67 52.0(10) . . . . ? C57 C64 C68 C69 -170.1(10) . . . . ? C63 C64 C68 C69 57.5(15) . . . . ? C65 C64 C68 C69 -67.1(12) . . . . ? O11 C71 C72 C73 -3.0(16) . . . . ? C78 C71 C72 C73 177.7(9) . . . . ? O11 C71 C72 C81 -179.5(10) . . . . ? C78 C71 C72 C81 1.1(12) . . . . ? C71 C72 C73 O12 -2.4(15) . . . . ? C81 C72 C73 O12 173.2(10) . . . . ? C71 C72 C73 C74 174.5(9) . . . . ? C81 C72 C73 C74 -9.9(16) . . . . ? O12 C73 C74 F29 -28.0(11) . . . . ? C72 C73 C74 F29 154.8(9) . . . . ? O12 C73 C74 F30 -146.4(8) . . . . ? C72 C73 C74 F30 36.4(13) . . . . ? O12 C73 C74 C75 95.4(10) . . . . ? C72 C73 C74 C75 -81.8(12) . . . . ? F29 C74 C75 F32 -167.1(8) . . . . ? F30 C74 C75 F32 -54.0(11) . . . . ? C73 C74 C75 F32 68.0(11) . . . . ? F29 C74 C75 F31 -49.5(11) . . . . ? F30 C74 C75 F31 63.6(11) . . . . ? C73 C74 C75 F31 -174.4(8) . . . . ? F29 C74 C75 C76 70.8(13) . . . . ? F30 C74 C75 C76 -176.1(11) . . . . ? C73 C74 C75 C76 -54.1(15) . . . . ? F32 C75 C76 F34 64.5(13) . . . . ? F31 C75 C76 F34 -53.1(14) . . . . ? C74 C75 C76 F34 -172.9(10) . . . . ? F32 C75 C76 F33 -176.8(8) . . . . ? F31 C75 C76 F33 65.6(12) . . . . ? C74 C75 C76 F33 -54.3(15) . . . . ? F32 C75 C76 F35 -57.7(12) . . . . ? F31 C75 C76 F35 -175.3(10) . . . . ? C74 C75 C76 F35 64.8(15) . . . . ? O11 C71 C78 C77 -17.6(16) . . . . ? C72 C71 C78 C77 161.8(11) . . . . ? O11 C71 C78 C79 108.6(11) . . . . ? C72 C71 C78 C79 -72.1(11) . . . . ? O11 C71 C78 C82 -145.9(11) . . . . ? C72 C71 C78 C82 33.5(12) . . . . ? C77 C78 C79 C80 -164.3(10) . . . . ? C71 C78 C79 C80 68.4(11) . . . . ? C82 C78 C79 C80 -33.2(11) . . . . ? C78 C79 C80 C81 -1.0(12) . . . . ? C73 C72 C81 C80 -107.2(12) . . . . ? C71 C72 C81 C80 68.9(11) . . . . ? C73 C72 C81 C82 148.0(11) . . . . ? C71 C72 C81 C82 -35.9(11) . . . . ? C79 C80 C81 C72 -67.2(11) . . . . ? C79 C80 C81 C82 35.1(11) . . . . ? C72 C81 C82 C84 -65.4(14) . . . . ? C80 C81 C82 C84 -171.9(12) . . . . ? C72 C81 C82 C83 167.7(11) . . . . ? C80 C81 C82 C83 61.2(14) . . . . ? C72 C81 C82 C78 53.5(10) . . . . ? C80 C81 C82 C78 -53.1(10) . . . . ? C77 C78 C82 C84 -57.5(15) . . . . ? C79 C78 C82 C84 174.3(11) . . . . ? C71 C78 C82 C84 68.7(13) . . . . ? C77 C78 C82 C81 -178.5(11) . . . . ? C79 C78 C82 C81 53.2(10) . . . . ? C71 C78 C82 C81 -52.4(11) . . . . ? C77 C78 C82 C83 65.5(17) . . . . ? C79 C78 C82 C83 -62.7(13) . . . . ? C71 C78 C82 C83 -168.3(12) . . . . ? C2 C1 O1 Yb1 0.7(13) . . . . ? C8 C1 O1 Yb1 -179.7(6) . . . . ? C2 C3 O2 Yb1 -9.9(13) . . . . ? C4 C3 O2 Yb1 175.4(6) . . . . ? C16 C15 O3 Yb1 -11.8(14) . . . . ? C22 C15 O3 Yb1 171.6(7) . . . . ? C16 C17 O4 Yb1 7.6(19) . . . . ? C18 C17 O4 Yb1 -174.1(11) . . . . ? C30 C29 O5 Yb1 -7.6(15) . . . . ? C36 C29 O5 Yb1 177.4(8) . . . . ? C30 C31 O6 Yb1 -5.5(14) . . . . ? C32 C31 O6 Yb1 174.0(6) . . . . ? C44 C43 O7 Yb2 -2.4(13) . . . . ? C50 C43 O7 Yb2 -175.8(7) . . . . ? C44 C45 O8 Yb2 4.3(17) . . . . ? C46 C45 O8 Yb2 -173.6(7) . . . . ? C72 C71 O11 Yb2 9.8(15) . . . . ? C78 C71 O11 Yb2 -170.9(7) . . . . ? C72 C73 O12 Yb2 0.6(13) . . . . ? C74 C73 O12 Yb2 -176.5(6) . . . . ? C58 C57 O9 Yb2 15.7(12) . . . . ? C64 C57 O9 Yb2 -164.1(6) . . . . ? C58 C59 O10 Yb2 -19.0(18) . . . . ? C60 C59 O10 Yb2 156.1(10) . . . . ? C3 O2 Yb1 O4 139.3(7) . . . . ? C3 O2 Yb1 O6 -100.9(10) . . . . ? C3 O2 Yb1 O5 66.4(8) . . . . ? C3 O2 Yb1 O1 6.3(7) . . . . ? C3 O2 Yb1 O1W -69.6(7) . . . . ? C3 O2 Yb1 O3 -144.9(7) . . . . ? C17 O4 Yb1 O2 76.2(11) . . . . ? C17 O4 Yb1 O6 -89.7(11) . . . . ? C17 O4 Yb1 O5 -163.2(11) . . . . ? C17 O4 Yb1 O1 145.8(10) . . . . ? C17 O4 Yb1 O1W 1.9(14) . . . . ? C17 O4 Yb1 O3 -10.5(11) . . . . ? C31 O6 Yb1 O2 171.3(8) . . . . ? C31 O6 Yb1 O4 -71.0(7) . . . . ? C31 O6 Yb1 O5 2.7(7) . . . . ? C31 O6 Yb1 O1 68.1(7) . . . . ? C31 O6 Yb1 O1W 139.5(7) . . . . ? C31 O6 Yb1 O3 -144.5(7) . . . . ? C29 O5 Yb1 O2 -172.7(8) . . . . ? C29 O5 Yb1 O4 109.5(9) . . . . ? C29 O5 Yb1 O6 3.7(8) . . . . ? C29 O5 Yb1 O1 -109.2(9) . . . . ? C29 O5 Yb1 O1W -60.6(9) . . . . ? C29 O5 Yb1 O3 63.8(10) . . . . ? C1 O1 Yb1 O2 -1.8(7) . . . . ? C1 O1 Yb1 O4 -75.0(7) . . . . ? C1 O1 Yb1 O6 162.3(7) . . . . ? C1 O1 Yb1 O5 -128.2(7) . . . . ? C1 O1 Yb1 O1W 87.3(7) . . . . ? C1 O1 Yb1 O3 59.7(8) . . . . ? C15 O3 Yb1 O2 -74.8(7) . . . . ? C15 O3 Yb1 O4 11.9(7) . . . . ? C15 O3 Yb1 O6 116.3(7) . . . . ? C15 O3 Yb1 O5 58.0(9) . . . . ? C15 O3 Yb1 O1 -134.1(7) . . . . ? C15 O3 Yb1 O1W -161.7(7) . . . . ? C59 O10 Yb2 O8 -60.3(9) . . . . ? C59 O10 Yb2 O12 103.7(9) . . . . ? C59 O10 Yb2 O11 177.4(9) . . . . ? C59 O10 Yb2 O7 -128.7(8) . . . . ? C59 O10 Yb2 O9 23.5(9) . . . . ? C59 O10 Yb2 O2W 14.4(12) . . . . ? C45 O8 Yb2 O10 -131.7(9) . . . . ? C45 O8 Yb2 O12 120.7(10) . . . . ? C45 O8 Yb2 O11 -61.0(10) . . . . ? C45 O8 Yb2 O7 -1.8(9) . . . . ? C45 O8 Yb2 O9 151.8(9) . . . . ? C45 O8 Yb2 O2W 76.0(9) . . . . ? C73 O12 Yb2 O10 76.3(7) . . . . ? C73 O12 Yb2 O8 -178.3(8) . . . . ? C73 O12 Yb2 O11 3.2(7) . . . . ? C73 O12 Yb2 O7 -60.5(7) . . . . ? C73 O12 Yb2 O9 150.6(7) . . . . ? C73 O12 Yb2 O2W -132.9(7) . . . . ? C71 O11 Yb2 O10 -112.1(8) . . . . ? C71 O11 Yb2 O8 172.4(7) . . . . ? C71 O11 Yb2 O12 -8.1(8) . . . . ? C71 O11 Yb2 O7 110.9(8) . . . . ? C71 O11 Yb2 O9 -68.3(9) . . . . ? C71 O11 Yb2 O2W 57.1(9) . . . . ? C43 O7 Yb2 O10 73.3(8) . . . . ? C43 O7 Yb2 O8 0.9(7) . . . . ? C43 O7 Yb2 O12 -164.0(7) . . . . ? C43 O7 Yb2 O11 129.1(8) . . . . ? C43 O7 Yb2 O9 -51.8(9) . . . . ? C43 O7 Yb2 O2W -89.4(8) . . . . ? C57 O9 Yb2 O10 -21.4(6) . . . . ? C57 O9 Yb2 O8 64.9(6) . . . . ? C57 O9 Yb2 O12 -123.7(6) . . . . ? C57 O9 Yb2 O11 -65.3(7) . . . . ? C57 O9 Yb2 O7 116.1(7) . . . . ? C57 O9 Yb2 O2W 154.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.173 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.094 # Attachment '- CIF-R.cif' #====================================================================== # SUBMISSION DETAILS data_I _database_code_depnum_ccdc_archive 'CCDC 772227' #TrackingRef '- CIF-R.cif' # start Validation Reply Form _vrf_PLAT241_I ; PROBLEM: Check High Ueq as Compared to Neighbors for C60 RESPONSE: Many crystals tried, best presented - mobile alkyl chains lead to this anomalous value. ; _vrf_PLAT242_I ; PROBLEM: Check Low Ueq as Compared to Neighbors for C20 RESPONSE: Many crystals tried, best presented - mobile alkyl chains lead to this anomalous value. ; _vrf_PLAT860_I ; PROBLEM: Note: Number of Least-Squares Restraints ....... 37 RESPONSE: Owing to the static disorder of the mobile alkyl chains, 37 least-squares restraints were used to refine the structure.The restraints are listed under _refine_special_details ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 F21 N0 O7 Yb1' _chemical_formula_weight 1232.81 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 '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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.573(6) _cell_length_b 13.207(3) _cell_length_c 31.227(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.072(5) _cell_angle_gamma 90.00 _cell_volume 10127(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5132 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 20.15 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.303 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.036 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4888 _exptl_absorpt_coefficient_mu 1.969 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27414 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.1553 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 0.65 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17888 _reflns_number_gt 10198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. delu 0.01 F30 C60 delu 0.01 F12 C20 delu 0.01 F6 C6 delu 0.01 C75 C76 delu 0.01 F26 C48 delu 0.01 C17 C18 delu 0.01 F14 C20 delu 0.01 F13 C20 dfix 1.50 0.02 C19 C20 dfix 1.35 0.02 F8 C18 F9 C18 F3 C5 dfix 1.50 0.02 C17 C18 dfix 1.50 0.02 C5 C6 dfix 1.35 0.02 F33 C62 F35 C62 F34 C62 dfix 1.50 0.02 C61 C62 dfix 1.50 0.02 C60 C61 dfix 1.50 0.02 C47 C48 dfix 1.50 0.02 C18 C19 dfix 1.35 0.02 F31 C61 F32 C61 dfix 1.35 0.02 F13 C20 F12 C20 dfix 2.10 0.02 F33 F34 F34 F35 F35 F33 delu 0.01 F5 C6 delu 0.01 C33 C34 delu 0.01 C37 C38 delu 0.01 C38 C39 delu 0.01 F28 C48 delu 0.01 F32 C61 delu 0.01 F34 C62 delu 0.01 C80 C81 ; _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^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.044(12) _refine_ls_number_reflns 17888 _refine_ls_number_parameters 1224 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1472 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.178 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6272(7) 0.9005(13) 0.6299(4) 0.068(5) Uani 1 1 d . . . C2 C 0.6117(5) 0.7951(11) 0.6333(4) 0.051(3) Uani 1 1 d . . . C3 C 0.6486(9) 0.7226(15) 0.6465(5) 0.089(4) Uani 1 1 d . . . C4 C 0.6314(8) 0.6119(16) 0.6474(6) 0.090(3) Uani 1 1 d . . . C5 C 0.6383(8) 0.5579(15) 0.6077(6) 0.089(4) Uani 1 1 d D . . C6 C 0.6211(13) 0.451(2) 0.6028(11) 0.190(13) Uani 1 1 d DU . . C7 C 0.5890(8) 1.0607(16) 0.5979(7) 0.117(7) Uani 1 1 d . . . H7A H 0.5908 1.1083 0.6211 0.176 Uiso 1 1 calc R . . H7B H 0.5606 1.0802 0.5776 0.176 Uiso 1 1 calc R . . H7C H 0.6232 1.0597 0.5840 0.176 Uiso 1 1 calc R . . C8 C 0.5771(5) 0.9575(17) 0.6149(5) 0.074(4) Uani 1 1 d . . . C9 C 0.5430(6) 0.9605(15) 0.6545(4) 0.088(5) Uani 1 1 d . . . H9A H 0.5132 1.0082 0.6510 0.105 Uiso 1 1 calc R . . H9B H 0.5650 0.9786 0.6798 0.105 Uiso 1 1 calc R . . C10 C 0.5213(6) 0.8484(17) 0.6575(5) 0.107(7) Uani 1 1 d . . . H10A H 0.4822 0.8452 0.6519 0.128 Uiso 1 1 calc R . . H10B H 0.5300 0.8191 0.6854 0.128 Uiso 1 1 calc R . . C11 C 0.5532(6) 0.7937(13) 0.6212(5) 0.078(5) Uani 1 1 d . . . H11 H 0.5388 0.7272 0.6127 0.093 Uiso 1 1 calc R . . C12 C 0.5486(6) 0.8776(16) 0.5853(5) 0.083(4) Uani 1 1 d . . . C13 C 0.5843(6) 0.8559(15) 0.5461(4) 0.090(3) Uani 1 1 d . . . H13A H 0.5852 0.9149 0.5281 0.135 Uiso 1 1 calc R . . H13B H 0.5691 0.8001 0.5299 0.135 Uiso 1 1 calc R . . H13C H 0.6207 0.8392 0.5559 0.135 Uiso 1 1 calc R . . C14 C 0.4900(7) 0.9111(17) 0.5677(7) 0.140(9) Uani 1 1 d . . . H14A H 0.4935 0.9640 0.5469 0.210 Uiso 1 1 calc R . . H14B H 0.4691 0.9354 0.5910 0.210 Uiso 1 1 calc R . . H14C H 0.4718 0.8541 0.5545 0.210 Uiso 1 1 calc R . . C15 C 0.8306(6) 0.6999(14) 0.7106(5) 0.072(4) Uani 1 1 d . . . C16 C 0.8549(8) 0.6674(15) 0.6723(6) 0.094(4) Uani 1 1 d . . . C17 C 0.8433(8) 0.706(2) 0.6312(6) 0.123(6) Uani 1 1 d DU . . C18 C 0.8754(7) 0.6683(12) 0.5938(5) 0.094(4) Uani 1 1 d DU . . C19 C 0.8934(9) 0.7469(18) 0.5610(7) 0.123(6) Uani 1 1 d D . . C20 C 0.9347(10) 0.712(2) 0.5273(8) 0.168(8) Uani 1 1 d DU . . C21 C 0.8233(7) 0.6464(17) 0.7880(5) 0.117(8) Uani 1 1 d . . . H21A H 0.8196 0.7160 0.7963 0.176 Uiso 1 1 calc R . . H21B H 0.8418 0.6095 0.8106 0.176 Uiso 1 1 calc R . . H21C H 0.7879 0.6177 0.7825 0.176 Uiso 1 1 calc R . . C22 C 0.8560(6) 0.6404(13) 0.7475(5) 0.072(4) Uani 1 1 d . . . C23 C 0.9174(6) 0.6741(13) 0.7518(5) 0.088(5) Uani 1 1 d . . . H23A H 0.9207 0.7472 0.7509 0.106 Uiso 1 1 calc R . . H23B H 0.9345 0.6492 0.7782 0.106 Uiso 1 1 calc R . . C24 C 0.9425(7) 0.6252(18) 0.7127(5) 0.106(7) Uani 1 1 d . . . H24A H 0.9692 0.5745 0.7214 0.128 Uiso 1 1 calc R . . H24B H 0.9600 0.6758 0.6953 0.128 Uiso 1 1 calc R . . C25 C 0.8913(8) 0.5736(14) 0.6863(6) 0.093(6) Uani 1 1 d . . . H25 H 0.8994 0.5233 0.6643 0.112 Uiso 1 1 calc R . . C26 C 0.8591(7) 0.5389(17) 0.7240(7) 0.109(7) Uani 1 1 d . . . C27 C 0.8024(7) 0.4933(16) 0.7093(7) 0.133(9) Uani 1 1 d . . . H27A H 0.7769 0.5026 0.7315 0.200 Uiso 1 1 calc R . . H27B H 0.8064 0.4223 0.7035 0.200 Uiso 1 1 calc R . . H27C H 0.7892 0.5272 0.6837 0.200 Uiso 1 1 calc R . . C28 C 0.8925(8) 0.4568(16) 0.7526(6) 0.131(7) Uani 1 1 d . . . H28A H 0.8707 0.4353 0.7759 0.196 Uiso 1 1 calc R . . H28B H 0.9256 0.4867 0.7638 0.196 Uiso 1 1 calc R . . H28C H 0.9009 0.3994 0.7352 0.196 Uiso 1 1 calc R . . C29 C 0.7904(8) 1.0411(16) 0.5954(5) 0.095(7) Uani 1 1 d . . . C30 C 0.8243(6) 1.1010(11) 0.6285(5) 0.067(4) Uani 1 1 d . . . C31 C 0.8295(6) 1.0698(10) 0.6693(5) 0.060(4) Uani 1 1 d . . . C32 C 0.8655(9) 1.1274(15) 0.7012(6) 0.089(6) Uani 1 1 d . . . C33 C 0.9246(8) 1.102(2) 0.7025(8) 0.116(8) Uani 1 1 d U . . C34 C 0.9444(11) 0.996(2) 0.7028(10) 0.136(9) Uani 1 1 d U . . C35 C 0.7475(9) 1.070(2) 0.5214(5) 0.155(11) Uani 1 1 d . . . H35A H 0.7130 1.0752 0.5347 0.232 Uiso 1 1 calc R . . H35B H 0.7533 1.0017 0.5124 0.232 Uiso 1 1 calc R . . H35C H 0.7477 1.1143 0.4970 0.232 Uiso 1 1 calc R . . C36 C 0.7939(8) 1.1021(17) 0.5542(7) 0.102(7) Uani 1 1 d . . . C37 C 0.8512(10) 1.089(3) 0.5416(8) 0.163(12) Uani 1 1 d U . . H37A H 0.8610 1.0180 0.5424 0.195 Uiso 1 1 calc R . . H37B H 0.8552 1.1135 0.5125 0.195 Uiso 1 1 calc R . . C38 C 0.8864(9) 1.145(2) 0.5703(8) 0.137(9) Uani 1 1 d U . . H38A H 0.9061 1.1973 0.5557 0.164 Uiso 1 1 calc R . . H38B H 0.9120 1.1010 0.5857 0.164 Uiso 1 1 calc R . . C39 C 0.8431(9) 1.191(2) 0.6008(7) 0.132(9) Uani 1 1 d U . . H39 H 0.8549 1.2513 0.6168 0.159 Uiso 1 1 calc R . . C40 C 0.7975(11) 1.206(2) 0.5690(7) 0.125(8) Uani 1 1 d . . . C41 C 0.7433(12) 1.2424(18) 0.5920(7) 0.166(11) Uani 1 1 d . . . H41A H 0.7236 1.2892 0.5737 0.249 Uiso 1 1 calc R . . H41B H 0.7531 1.2749 0.6186 0.249 Uiso 1 1 calc R . . H41C H 0.7208 1.1846 0.5973 0.249 Uiso 1 1 calc R . . C42 C 0.8110(11) 1.289(2) 0.5336(7) 0.177(12) Uani 1 1 d . . . H42A H 0.8442 1.2710 0.5202 0.266 Uiso 1 1 calc R . . H42B H 0.8151 1.3541 0.5470 0.266 Uiso 1 1 calc R . . H42C H 0.7818 1.2914 0.5124 0.266 Uiso 1 1 calc R . . C43 C 0.8875(5) 0.9305(13) 0.8794(4) 0.058(4) Uani 1 1 d . . . C44 C 0.8992(10) 1.036(2) 0.8784(7) 0.124(5) Uani 1 1 d . . . C45 C 0.8641(11) 1.1063(14) 0.8615(7) 0.115(6) Uani 1 1 d . . . C46 C 0.8807(11) 1.224(3) 0.8575(8) 0.168(8) Uani 1 1 d . . . C47 C 0.8640(11) 1.2863(12) 0.8958(8) 0.115(6) Uani 1 1 d D . . C49 C 0.9355(8) 0.7636(15) 0.8911(9) 0.152(11) Uani 1 1 d . . . H49A H 0.9693 0.7338 0.9010 0.228 Uiso 1 1 calc R . . H49B H 0.9295 0.7493 0.8612 0.228 Uiso 1 1 calc R . . H49C H 0.9062 0.7357 0.9069 0.228 Uiso 1 1 calc R . . C50 C 0.9378(6) 0.8779(16) 0.8979(5) 0.079(5) Uani 1 1 d . . . C51 C 0.9365(7) 0.9107(15) 0.9450(6) 0.107(7) Uani 1 1 d . . . H51A H 0.9621 0.8718 0.9627 0.129 Uiso 1 1 calc R . . H51B H 0.9003 0.9034 0.9560 0.129 Uiso 1 1 calc R . . C52 C 0.9543(8) 1.0286(18) 0.9430(6) 0.125(8) Uani 1 1 d . . . H52A H 0.9273 1.0722 0.9554 0.150 Uiso 1 1 calc R . . H52B H 0.9893 1.0399 0.9576 0.150 Uiso 1 1 calc R . . C53 C 0.9572(6) 1.0447(15) 0.8978(6) 0.086(5) Uani 1 1 d . . . H53 H 0.9760 1.1071 0.8901 0.103 Uiso 1 1 calc R . . C54 C 0.9816(5) 0.9503(16) 0.8798(5) 0.083(4) Uani 1 1 d . . . C55 C 1.0407(7) 0.9243(16) 0.8992(7) 0.149(9) Uani 1 1 d . . . H55A H 1.0518 0.9756 0.9195 0.223 Uiso 1 1 calc R . . H55B H 1.0661 0.9219 0.8765 0.223 Uiso 1 1 calc R . . H55C H 1.0400 0.8598 0.9133 0.223 Uiso 1 1 calc R . . C56 C 0.9861(6) 0.939(2) 0.8310(6) 0.138(8) Uani 1 1 d . . . H56A H 0.9793 0.8698 0.8230 0.207 Uiso 1 1 calc R . . H56B H 1.0220 0.9580 0.8229 0.207 Uiso 1 1 calc R . . H56C H 0.9598 0.9820 0.8167 0.207 Uiso 1 1 calc R . . C57 C 0.6936(6) 1.1284(12) 0.7926(4) 0.063(4) Uani 1 1 d . . . C58 C 0.6715(6) 1.1693(12) 0.8320(5) 0.065(4) Uani 1 1 d . . . C59 C 0.6766(7) 1.1242(15) 0.8713(5) 0.086(5) Uani 1 1 d . . . C60 C 0.6568(11) 1.162(3) 0.9143(10) 0.30(2) Uani 1 1 d DU . . C61 C 0.6047(9) 1.1042(16) 0.9210(5) 0.126(6) Uani 1 1 d DU . . C62 C 0.5837(9) 1.109(2) 0.9649(7) 0.30(2) Uani 1 1 d DU . . C63 C 0.6819(7) 1.1600(16) 0.7119(6) 0.102(6) Uani 1 1 d . . . H63A H 0.6565 1.1052 0.7083 0.153 Uiso 1 1 calc R . . H63B H 0.7181 1.1356 0.7077 0.153 Uiso 1 1 calc R . . H63C H 0.6732 1.2120 0.6913 0.153 Uiso 1 1 calc R . . C64 C 0.6785(6) 1.2025(11) 0.7563(5) 0.067(4) Uani 1 1 d . . . C65 C 0.7129(10) 1.2914(14) 0.7673(7) 0.140(7) Uani 1 1 d . . . H65A H 0.7506 1.2700 0.7705 0.168 Uiso 1 1 calc R . . H65B H 0.7103 1.3399 0.7440 0.168 Uiso 1 1 calc R . . C66 C 0.6971(9) 1.3398(14) 0.8061(8) 0.140(7) Uani 1 1 d . . . H66A H 0.6866 1.4098 0.8013 0.168 Uiso 1 1 calc R . . H66B H 0.7258 1.3366 0.8283 0.168 Uiso 1 1 calc R . . C67 C 0.6469(8) 1.2717(15) 0.8173(6) 0.101(7) Uani 1 1 d . . . H67 H 0.6212 1.3023 0.8368 0.121 Uiso 1 1 calc R . . C68 C 0.6224(8) 1.2400(18) 0.7731(5) 0.105(7) Uani 1 1 d . . . C69 C 0.5782(8) 1.162(2) 0.7724(8) 0.129(8) Uani 1 1 d . . . C70 C 0.5991(9) 1.3338(19) 0.7479(6) 0.152(11) Uani 1 1 d . . . H70A H 0.6282 1.3795 0.7419 0.228 Uiso 1 1 calc R . . H70B H 0.5729 1.3677 0.7649 0.228 Uiso 1 1 calc R . . H70C H 0.5818 1.3116 0.7215 0.228 Uiso 1 1 calc R . . C71 C 0.7271(7) 0.7701(13) 0.9018(5) 0.074(4) Uani 1 1 d . . . C72 C 0.6952(9) 0.716(2) 0.8709(7) 0.126(6) Uani 1 1 d . . . C73 C 0.6917(5) 0.7423(11) 0.8274(5) 0.070(5) Uani 1 1 d . . . C74 C 0.6554(7) 0.6918(13) 0.7952(6) 0.075(5) Uani 1 1 d . . . C75 C 0.5926(8) 0.7183(18) 0.7973(7) 0.097(6) Uani 1 1 d U . . C76 C 0.5773(9) 0.826(2) 0.7926(8) 0.120(8) Uani 1 1 d U . . C77 C 0.7387(9) 0.7698(19) 0.9847(5) 0.140(8) Uani 1 1 d . . . H77A H 0.7741 0.8001 0.9836 0.210 Uiso 1 1 calc R . . H77B H 0.7377 0.7249 1.0088 0.210 Uiso 1 1 calc R . . H77C H 0.7118 0.8218 0.9875 0.210 Uiso 1 1 calc R . . C78 C 0.7263(9) 0.7085(17) 0.9424(6) 0.105(6) Uani 1 1 d . . . C79 C 0.7632(9) 0.6156(17) 0.9321(6) 0.116(7) Uani 1 1 d . . . H79A H 0.7977 0.6380 0.9214 0.139 Uiso 1 1 calc R . . H79B H 0.7702 0.5749 0.9576 0.139 Uiso 1 1 calc R . . C80 C 0.7308(9) 0.5540(18) 0.8976(7) 0.132(8) Uani 1 1 d U . . H80A H 0.7504 0.5501 0.8712 0.158 Uiso 1 1 calc R . . H80B H 0.7232 0.4860 0.9075 0.158 Uiso 1 1 calc R . . C81 C 0.6796(8) 0.6147(15) 0.8916(6) 0.098(6) Uani 1 1 d U . . H81 H 0.6489 0.5790 0.8775 0.118 Uiso 1 1 calc R . . C82 C 0.6690(9) 0.6549(15) 0.9363(6) 0.098(6) Uani 1 1 d . . . C83 C 0.6190(11) 0.736(2) 0.9395(9) 0.169(13) Uani 1 1 d . . . H83A H 0.6184 0.7628 0.9681 0.253 Uiso 1 1 calc R . . H83B H 0.5851 0.7029 0.9326 0.253 Uiso 1 1 calc R . . H83C H 0.6242 0.7906 0.9196 0.253 Uiso 1 1 calc R . . C84 C 0.6590(10) 0.561(2) 0.9687(7) 0.169(12) Uani 1 1 d . . . H84A H 0.6368 0.5828 0.9916 0.254 Uiso 1 1 calc R . . H84B H 0.6934 0.5371 0.9803 0.254 Uiso 1 1 calc R . . H84C H 0.6409 0.5068 0.9533 0.254 Uiso 1 1 calc R . . F1 F 0.6601(4) 0.5661(7) 0.6798(3) 0.094(3) Uani 1 1 d . . . F2 F 0.5794(7) 0.6076(9) 0.6606(4) 0.166(4) Uani 1 1 d . . . F3 F 0.6908(8) 0.5522(15) 0.5967(6) 0.233(7) Uani 1 1 d D . . F4 F 0.6073(7) 0.5976(12) 0.5771(4) 0.175(7) Uani 1 1 d . . . F5 F 0.5666(10) 0.443(2) 0.6119(12) 0.40(2) Uani 1 1 d U . . F6 F 0.6369(16) 0.416(2) 0.5658(8) 0.42(2) Uani 1 1 d U . . F7 F 0.6310(8) 0.3981(10) 0.6329(5) 0.166(4) Uani 1 1 d . . . F8 F 0.8581(9) 0.5797(15) 0.5824(6) 0.233(7) Uani 1 1 d D . . F9 F 0.9298(9) 0.642(2) 0.6036(5) 0.333(19) Uani 1 1 d D . . F10 F 0.8369(9) 0.747(3) 0.5459(6) 0.39(3) Uani 1 1 d . . . F11 F 0.9071(6) 0.8406(13) 0.5854(5) 0.173(6) Uani 1 1 d . . . F12 F 0.9117(14) 0.779(2) 0.5009(7) 0.40(2) Uani 1 1 d DU . . F13 F 0.9165(14) 0.618(2) 0.5232(7) 0.330(17) Uani 1 1 d DU . . F14 F 0.9701(11) 0.754(4) 0.5576(14) 0.51(3) Uani 1 1 d U . . F15 F 0.8607(6) 1.2295(9) 0.6938(4) 0.144(5) Uani 1 1 d . . . F16 F 0.8468(5) 1.1127(11) 0.7420(4) 0.129(5) Uani 1 1 d . . . F17 F 0.9468(5) 1.1394(13) 0.6658(5) 0.176(6) Uani 1 1 d . . . F18 F 0.9495(6) 1.1481(12) 0.7358(5) 0.168(6) Uani 1 1 d . . . F19 F 0.9968(5) 0.9851(16) 0.7084(5) 0.209(9) Uani 1 1 d . . . F20 F 0.9184(5) 0.9542(15) 0.7356(4) 0.152(5) Uani 1 1 d . . . F21 F 0.9275(5) 0.9535(14) 0.6680(4) 0.157(5) Uani 1 1 d . . . F22 F 0.9301(5) 1.2354(9) 0.8485(4) 0.138(4) Uani 1 1 d . . . F23 F 0.8519(6) 1.2637(9) 0.8231(4) 0.142(5) Uani 1 1 d . . . F24 F 0.8945(10) 1.2411(15) 0.9299(5) 0.241(11) Uani 1 1 d . . . F25 F 0.8170(8) 1.2571(17) 0.9070(6) 0.226(11) Uani 1 1 d . . . F26 F 0.8675(12) 1.4251(14) 0.9313(6) 0.273(12) Uani 1 1 d U . . F27 F 0.9283(9) 1.4097(15) 0.8870(12) 0.38(2) Uani 1 1 d . . . F28 F 0.8471(12) 1.4339(19) 0.8680(8) 0.340(17) Uani 1 1 d U . . F29 F 0.6494(7) 1.2545(14) 0.9121(5) 0.192(8) Uani 1 1 d . . . F30 F 0.6908(7) 1.135(2) 0.9473(5) 0.277(14) Uani 1 1 d U . . F31 F 0.5700(6) 1.1503(16) 0.8912(4) 0.205(8) Uani 1 1 d D . . F32 F 0.6047(8) 0.9982(13) 0.9177(7) 0.233(11) Uani 1 1 d DU . . F33 F 0.5988(14) 1.191(3) 0.9840(11) 0.50(3) Uani 1 1 d D . . F34 F 0.5323(8) 1.104(3) 0.9615(5) 0.35(2) Uani 1 1 d DU . . F35 F 0.6054(14) 1.030(3) 0.9814(13) 0.55(3) Uani 1 1 d D . . F36 F 0.6689(5) 0.7102(8) 0.7549(3) 0.100(3) Uani 1 1 d . . . F37 F 0.6540(6) 0.5931(9) 0.8003(4) 0.125(4) Uani 1 1 d . . . F38 F 0.5665(5) 0.6669(14) 0.7636(4) 0.169(7) Uani 1 1 d . . . F39 F 0.5724(4) 0.6788(11) 0.8338(4) 0.140(5) Uani 1 1 d . . . F40 F 0.5955(4) 0.8714(13) 0.7589(4) 0.137(4) Uani 1 1 d . . . F41 F 0.5948(5) 0.8763(13) 0.8280(4) 0.143(4) Uani 1 1 d . . . F42 F 0.5240(5) 0.8378(17) 0.7903(5) 0.200(8) Uani 1 1 d . . . O1 O 0.6729(4) 0.9391(8) 0.6385(3) 0.069(3) Uani 1 1 d . . . O2 O 0.6986(3) 0.7387(6) 0.6539(3) 0.063(3) Uani 1 1 d . . . O3 O 0.8007(4) 0.7748(8) 0.7128(3) 0.063(3) Uani 1 1 d . . . O4 O 0.8110(3) 0.7740(9) 0.6251(3) 0.073(3) Uani 1 1 d . . . O5 O 0.7688(4) 0.9617(10) 0.6011(3) 0.081(3) Uani 1 1 d . . . O6 O 0.8059(3) 0.9948(7) 0.6857(3) 0.055(2) Uani 1 1 d . . . O7 O 0.8446(3) 0.8921(7) 0.8675(3) 0.068(3) Uani 1 1 d . . . O8 O 0.8159(4) 1.0859(7) 0.8496(3) 0.070(3) Uani 1 1 d . . . O9 O 0.7205(4) 1.0502(7) 0.7889(3) 0.056(2) Uani 1 1 d . . . O10 O 0.7036(4) 1.0371(9) 0.8749(3) 0.074(3) Uani 1 1 d . . . O11 O 0.7499(4) 0.8513(8) 0.8975(3) 0.072(3) Uani 1 1 d . . . O12 O 0.7107(3) 0.8283(7) 0.8127(3) 0.055(2) Uani 1 1 d . . . O1W O 0.7101(3) 0.9035(7) 0.7236(3) 0.062(3) Uani 1 1 d . . . O2W O 0.8113(3) 0.9188(7) 0.7778(3) 0.071(3) Uani 1 1 d . . . Yb1 Yb 0.75348(2) 0.86820(4) 0.660177(17) 0.05747(18) Uani 1 1 d . . . Yb2 Yb 0.76418(2) 0.95100(4) 0.840867(17) 0.05746(18) Uani 1 1 d . . . C48 C 0.8838(11) 1.3928(15) 0.8912(8) 0.124(5) Uani 1 1 d DU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.070(11) 0.097(15) 0.037(7) -0.001(7) -0.011(6) 0.014(9) C2 0.030(7) 0.062(10) 0.060(8) 0.009(7) 0.003(6) -0.024(7) C3 0.138(12) 0.071(9) 0.058(8) 0.001(7) -0.009(8) -0.023(9) C4 0.102(9) 0.100(10) 0.067(7) 0.004(7) -0.005(6) -0.003(8) C5 0.138(12) 0.071(9) 0.058(8) 0.001(7) -0.009(8) -0.023(9) C6 0.22(2) 0.17(3) 0.18(2) 0.08(2) 0.05(2) 0.03(3) C7 0.089(14) 0.110(17) 0.149(18) 0.056(14) -0.043(12) 0.014(12) C8 0.052(9) 0.083(12) 0.086(10) -0.009(11) -0.008(7) 0.022(10) C9 0.082(10) 0.108(14) 0.074(10) -0.017(10) 0.011(8) 0.005(12) C10 0.054(10) 0.15(2) 0.116(13) -0.034(14) -0.001(8) 0.022(11) C11 0.071(12) 0.071(11) 0.092(12) -0.018(10) 0.010(9) -0.030(9) C12 0.070(10) 0.101(13) 0.077(10) 0.001(11) -0.014(7) 0.009(11) C13 0.102(9) 0.100(10) 0.067(7) 0.004(7) -0.005(6) -0.003(8) C14 0.114(15) 0.15(2) 0.151(17) -0.033(14) -0.060(13) 0.019(13) C15 0.047(9) 0.086(13) 0.083(11) 0.019(10) -0.007(8) 0.015(8) C16 0.126(12) 0.085(9) 0.071(8) 0.007(7) 0.016(7) 0.037(8) C17 0.106(12) 0.166(17) 0.101(11) -0.008(11) 0.057(9) 0.038(11) C18 0.126(12) 0.085(9) 0.071(8) 0.007(7) 0.016(7) 0.037(8) C19 0.106(12) 0.166(17) 0.101(11) -0.008(11) 0.057(9) 0.038(11) C20 0.116(14) 0.28(2) 0.115(14) 0.037(14) 0.053(10) 0.069(14) C21 0.131(16) 0.137(19) 0.086(13) 0.063(13) 0.033(11) 0.063(14) C22 0.060(11) 0.068(11) 0.088(12) -0.012(9) 0.015(8) 0.018(8) C23 0.085(13) 0.071(11) 0.106(13) -0.002(10) -0.036(10) 0.020(9) C24 0.082(14) 0.16(2) 0.075(12) 0.001(12) -0.004(10) 0.032(13) C25 0.106(15) 0.076(12) 0.099(14) -0.023(10) 0.016(11) 0.003(11) C26 0.068(12) 0.102(16) 0.151(19) 0.012(14) -0.053(12) 0.010(11) C27 0.095(15) 0.103(19) 0.20(2) 0.015(15) -0.018(14) -0.025(12) C28 0.184(19) 0.059(11) 0.150(17) 0.016(13) 0.002(14) 0.068(14) C29 0.119(15) 0.095(15) 0.074(12) 0.062(12) 0.048(10) 0.052(12) C30 0.083(11) 0.037(8) 0.082(11) -0.004(8) 0.000(8) -0.002(7) C31 0.089(11) 0.026(8) 0.066(10) 0.015(7) 0.012(8) 0.001(7) C32 0.131(18) 0.068(14) 0.069(12) 0.004(10) 0.004(11) -0.019(11) C33 0.062(14) 0.133(17) 0.15(2) 0.022(17) -0.033(13) -0.061(12) C34 0.10(2) 0.16(2) 0.15(2) 0.03(2) -0.027(17) -0.006(17) C35 0.15(2) 0.23(3) 0.078(14) 0.086(17) -0.009(13) 0.011(19) C36 0.120(17) 0.083(16) 0.105(16) 0.048(12) 0.038(12) 0.034(12) C37 0.11(2) 0.28(4) 0.101(17) 0.050(18) 0.053(13) 0.000(19) C38 0.079(16) 0.18(3) 0.15(2) 0.099(16) 0.032(11) 0.016(13) C39 0.15(2) 0.15(2) 0.100(16) 0.031(15) 0.054(14) -0.047(16) C40 0.17(2) 0.13(2) 0.079(14) 0.066(14) 0.006(14) 0.010(17) C41 0.27(3) 0.092(18) 0.13(2) 0.057(15) 0.05(2) 0.057(19) C42 0.22(3) 0.16(2) 0.15(2) 0.11(2) 0.040(19) -0.02(2) C43 0.025(7) 0.104(14) 0.043(7) 0.003(7) -0.011(5) 0.015(7) C44 0.132(13) 0.097(13) 0.140(12) -0.005(10) -0.030(9) -0.033(10) C45 0.179(17) 0.027(7) 0.138(14) -0.013(8) -0.022(12) -0.034(8) C46 0.116(14) 0.28(2) 0.115(14) 0.037(14) 0.053(10) 0.069(14) C47 0.179(17) 0.027(7) 0.138(14) -0.013(8) -0.022(12) -0.034(8) C49 0.091(15) 0.068(15) 0.29(3) -0.036(17) -0.040(17) 0.030(12) C50 0.052(9) 0.087(14) 0.097(12) 0.040(12) 0.000(8) 0.028(10) C51 0.087(12) 0.14(2) 0.094(13) 0.039(11) -0.021(9) 0.023(11) C52 0.120(17) 0.15(2) 0.102(15) -0.035(14) -0.056(12) 0.029(15) C53 0.044(10) 0.099(14) 0.113(15) -0.009(11) -0.011(9) -0.009(9) C54 0.043(8) 0.117(13) 0.090(11) -0.031(12) 0.003(7) 0.000(11) C55 0.077(13) 0.112(18) 0.25(3) -0.007(17) -0.032(15) 0.020(12) C56 0.083(12) 0.21(2) 0.125(15) 0.026(18) 0.022(10) -0.035(16) C57 0.057(10) 0.063(11) 0.068(10) 0.005(8) 0.003(7) 0.001(8) C58 0.065(10) 0.074(11) 0.056(9) -0.012(8) 0.003(7) 0.030(8) C59 0.073(11) 0.107(15) 0.078(12) -0.035(10) -0.011(9) 0.038(10) C60 0.25(2) 0.52(6) 0.122(16) -0.08(3) -0.006(16) 0.28(3) C61 0.140(14) 0.165(13) 0.075(10) 0.052(10) 0.047(9) 0.057(12) C62 0.25(2) 0.52(6) 0.122(16) -0.08(3) -0.006(16) 0.28(3) C63 0.106(15) 0.092(15) 0.108(16) 0.021(12) 0.012(11) 0.015(11) C64 0.072(11) 0.050(9) 0.077(10) 0.013(8) -0.005(8) 0.005(8) C65 0.184(15) 0.042(9) 0.191(18) -0.017(8) -0.046(13) -0.010(9) C66 0.184(15) 0.042(9) 0.191(18) -0.017(8) -0.046(13) -0.010(9) C67 0.105(14) 0.106(16) 0.093(13) -0.014(12) 0.014(10) 0.066(13) C68 0.106(16) 0.15(2) 0.062(11) 0.004(11) 0.004(10) 0.065(15) C69 0.074(15) 0.14(2) 0.17(2) 0.011(17) -0.012(13) -0.020(14) C70 0.155(18) 0.19(3) 0.108(15) 0.017(15) 0.000(13) 0.116(19) C71 0.097(12) 0.062(12) 0.059(10) 0.007(9) -0.020(8) 0.003(9) C72 0.140(14) 0.165(13) 0.075(10) 0.052(10) 0.047(9) 0.057(12) C73 0.048(9) 0.044(9) 0.117(13) -0.027(9) 0.016(8) -0.027(7) C74 0.095(13) 0.049(11) 0.082(13) 0.008(9) 0.023(9) -0.022(9) C75 0.077(14) 0.114(15) 0.098(15) 0.004(13) -0.014(11) -0.039(11) C76 0.090(17) 0.157(19) 0.113(18) 0.026(17) -0.019(13) 0.034(15) C77 0.20(2) 0.16(2) 0.057(12) -0.008(13) -0.023(12) 0.004(18) C78 0.136(18) 0.099(17) 0.081(13) 0.031(12) 0.006(11) 0.007(14) C79 0.135(18) 0.106(17) 0.107(15) 0.046(13) -0.011(13) -0.016(14) C80 0.17(2) 0.111(18) 0.112(16) 0.053(14) 0.013(15) 0.001(14) C81 0.128(15) 0.083(13) 0.081(12) 0.023(10) -0.024(11) -0.040(10) C82 0.124(18) 0.085(14) 0.086(14) 0.029(11) 0.032(12) -0.019(13) C83 0.19(3) 0.13(2) 0.19(3) 0.01(2) 0.10(2) -0.04(2) C84 0.15(2) 0.22(3) 0.14(2) 0.09(2) 0.019(16) -0.07(2) F1 0.112(7) 0.064(6) 0.104(7) 0.002(5) -0.003(6) -0.011(5) F2 0.268(13) 0.080(6) 0.149(8) -0.020(6) 0.023(8) -0.040(7) F3 0.275(15) 0.208(14) 0.225(13) -0.138(11) 0.149(11) -0.075(11) F4 0.261(18) 0.137(12) 0.122(10) -0.066(9) -0.073(11) 0.061(11) F5 0.25(2) 0.23(2) 0.73(6) -0.25(3) 0.16(3) -0.13(2) F6 0.75(6) 0.30(4) 0.20(2) -0.13(2) -0.06(3) 0.20(4) F7 0.268(13) 0.080(6) 0.149(8) -0.020(6) 0.023(8) -0.040(7) F8 0.275(15) 0.208(14) 0.225(13) -0.138(11) 0.149(11) -0.075(11) F9 0.33(2) 0.53(4) 0.147(13) 0.123(19) 0.093(14) 0.36(3) F10 0.26(2) 0.79(7) 0.134(14) -0.22(3) -0.080(14) 0.30(3) F11 0.161(12) 0.163(15) 0.203(14) -0.014(13) 0.091(10) -0.017(11) F12 0.57(5) 0.42(4) 0.21(2) 0.14(2) 0.15(3) 0.30(4) F13 0.59(5) 0.23(2) 0.171(18) -0.049(18) 0.06(2) 0.08(2) F14 0.24(3) 0.64(8) 0.65(7) -0.11(6) -0.16(4) -0.09(4) F15 0.221(14) 0.054(8) 0.156(12) -0.003(7) -0.027(10) -0.013(8) F16 0.157(11) 0.146(12) 0.083(8) -0.039(8) 0.008(7) -0.041(9) F17 0.123(10) 0.222(16) 0.183(13) 0.107(12) 0.012(8) -0.048(10) F18 0.142(11) 0.173(14) 0.185(13) -0.010(11) -0.068(10) -0.056(10) F19 0.058(8) 0.32(3) 0.246(16) 0.111(16) -0.007(8) -0.007(10) F20 0.133(10) 0.172(13) 0.153(11) 0.041(13) 0.021(8) -0.025(11) F21 0.134(10) 0.179(13) 0.157(11) -0.021(12) -0.008(8) 0.074(11) F22 0.103(9) 0.101(9) 0.211(13) 0.020(8) 0.032(8) -0.023(7) F23 0.231(14) 0.082(8) 0.110(9) 0.033(7) -0.022(8) -0.032(8) F24 0.40(3) 0.200(18) 0.114(11) -0.053(11) -0.086(14) 0.115(19) F25 0.230(18) 0.25(2) 0.206(17) -0.111(17) 0.112(15) -0.111(18) F26 0.54(4) 0.113(13) 0.167(14) -0.059(11) -0.013(16) 0.021(17) F27 0.24(2) 0.17(2) 0.73(6) -0.22(3) 0.07(3) -0.103(17) F28 0.45(4) 0.27(3) 0.29(2) -0.03(2) -0.11(2) 0.24(3) F29 0.219(17) 0.207(18) 0.150(12) -0.103(13) -0.013(11) 0.098(13) F30 0.217(17) 0.47(3) 0.134(12) -0.193(17) -0.089(11) 0.21(2) F31 0.172(13) 0.34(2) 0.099(9) 0.017(12) 0.015(8) 0.095(15) F32 0.223(16) 0.151(12) 0.34(3) 0.098(15) 0.188(17) 0.036(12) F33 0.55(6) 0.60(7) 0.37(4) -0.26(5) 0.31(4) -0.02(5) F34 0.25(2) 0.63(6) 0.178(16) 0.14(3) 0.111(16) 0.25(3) F35 0.74(9) 0.49(6) 0.40(5) 0.22(5) -0.17(5) 0.07(6) F36 0.156(10) 0.074(7) 0.071(7) -0.006(5) 0.007(6) -0.022(6) F37 0.187(12) 0.080(9) 0.106(8) -0.008(7) 0.001(8) -0.039(8) F38 0.128(10) 0.224(17) 0.151(12) -0.005(11) -0.030(8) -0.105(11) F39 0.102(8) 0.192(13) 0.126(9) 0.034(9) 0.022(7) -0.062(8) F40 0.119(8) 0.163(12) 0.128(9) 0.059(10) 0.000(7) 0.006(10) F41 0.138(9) 0.162(12) 0.128(9) -0.007(10) -0.001(7) 0.051(10) F42 0.065(8) 0.32(3) 0.216(14) 0.024(15) -0.023(8) 0.002(11) O1 0.060(6) 0.046(6) 0.102(7) -0.001(6) -0.014(5) 0.033(5) O2 0.042(5) 0.027(5) 0.117(8) 0.001(5) -0.013(5) -0.018(4) O3 0.072(7) 0.055(7) 0.063(6) 0.008(5) 0.007(5) 0.015(5) O4 0.040(6) 0.089(8) 0.092(7) -0.029(6) 0.029(5) 0.029(5) O5 0.069(6) 0.106(9) 0.067(6) 0.059(7) 0.006(4) -0.008(7) O6 0.033(5) 0.058(7) 0.073(6) -0.008(5) 0.003(4) -0.012(4) O7 0.030(5) 0.059(7) 0.114(7) 0.018(5) -0.025(5) 0.018(4) O8 0.041(6) 0.041(6) 0.128(9) -0.024(6) -0.013(5) -0.013(4) O9 0.063(6) 0.034(6) 0.071(6) 0.021(5) -0.004(4) 0.022(4) O10 0.058(6) 0.105(9) 0.059(6) 0.005(6) 0.017(4) 0.042(6) O11 0.096(7) 0.060(7) 0.061(6) 0.016(6) 0.001(4) -0.030(6) O12 0.054(5) 0.048(6) 0.062(6) -0.003(4) -0.002(4) -0.032(4) O1W 0.057(5) 0.070(7) 0.061(5) 0.015(4) 0.019(4) 0.000(4) O2W 0.065(6) 0.081(8) 0.068(6) -0.007(5) 0.015(4) 0.002(5) Yb1 0.0497(3) 0.0594(4) 0.0632(4) 0.0086(3) 0.0006(2) 0.0020(3) Yb2 0.0495(3) 0.0567(4) 0.0658(4) 0.0059(3) -0.0024(2) 0.0002(3) C48 0.132(13) 0.097(13) 0.140(12) -0.005(10) -0.030(9) -0.033(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.254(17) . ? C1 C2 1.45(2) . ? C1 C8 1.50(2) . ? C2 C3 1.37(2) . ? C2 C11 1.473(19) . ? C3 O2 1.26(2) . ? C3 C4 1.52(3) . ? C4 F1 1.354(19) . ? C4 F2 1.36(2) . ? C4 C5 1.45(2) . ? C5 F4 1.31(2) . ? C5 F3 1.349(16) . ? C5 C6 1.483(19) . ? C6 F7 1.19(3) . ? C6 F6 1.32(3) . ? C6 F5 1.38(3) . ? C7 C8 1.49(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.519(19) . ? C8 C12 1.55(2) . ? C9 C10 1.58(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.58(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.58(2) . ? C11 H11 0.9800 . ? C12 C13 1.56(2) . ? C12 C14 1.59(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O3 1.237(17) . ? C15 C16 1.42(2) . ? C15 C22 1.51(2) . ? C16 C17 1.40(2) . ? C16 C25 1.58(2) . ? C17 O4 1.21(2) . ? C17 C18 1.517(15) . ? C18 F8 1.290(15) . ? C18 F9 1.405(16) . ? C18 C19 1.533(17) . ? C19 F10 1.45(3) . ? C19 F11 1.48(3) . ? C19 C20 1.560(17) . ? C20 F12 1.321(18) . ? C20 F13 1.321(19) . ? C20 F14 1.38(4) . ? C21 C22 1.52(2) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C26 1.53(3) . ? C22 C23 1.57(2) . ? C23 C24 1.53(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.63(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.51(3) . ? C25 H25 0.9800 . ? C26 C27 1.57(2) . ? C26 C28 1.61(2) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O5 1.19(2) . ? C29 C36 1.52(2) . ? C29 C30 1.52(3) . ? C30 C31 1.340(19) . ? C30 C39 1.55(3) . ? C31 O6 1.266(14) . ? C31 C32 1.51(2) . ? C32 F15 1.37(2) . ? C32 F16 1.38(2) . ? C32 C33 1.49(3) . ? C33 F18 1.33(2) . ? C33 F17 1.38(2) . ? C33 C34 1.48(4) . ? C34 F21 1.28(3) . ? C34 F19 1.30(2) . ? C34 F20 1.35(3) . ? C35 C36 1.56(3) . ? C35 H35A 0.9601 . ? C35 H35B 0.9601 . ? C35 H35C 0.9601 . ? C36 C40 1.46(3) . ? C36 C37 1.49(3) . ? C37 C38 1.43(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.57(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.49(3) . ? C39 H39 0.9800 . ? C40 C42 1.59(3) . ? C40 C41 1.61(3) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 O7 1.216(14) . ? C43 C44 1.42(3) . ? C43 C50 1.515(18) . ? C44 C45 1.36(3) . ? C44 C53 1.53(3) . ? C45 O8 1.26(2) . ? C45 C46 1.61(4) . ? C46 F22 1.27(2) . ? C46 F23 1.37(3) . ? C46 C47 1.52(3) . ? C47 F25 1.28(3) . ? C47 F24 1.41(3) . ? C47 C48 1.498(17) . ? C49 C50 1.53(3) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.53(2) . ? C50 C54 1.56(2) . ? C51 C52 1.62(3) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.43(2) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.50(2) . ? C53 H53 0.9800 . ? C54 C56 1.54(2) . ? C54 C55 1.59(2) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 O9 1.233(16) . ? C57 C58 1.467(19) . ? C57 C64 1.53(2) . ? C58 C59 1.36(2) . ? C58 C67 1.55(2) . ? C59 O10 1.331(19) . ? C59 C60 1.53(3) . ? C60 F29 1.24(4) . ? C60 F30 1.35(3) . ? C60 C61 1.51(2) . ? C61 F31 1.382(16) . ? C61 F32 1.404(17) . ? C61 C62 1.483(17) . ? C62 F34 1.267(17) . ? C62 F35 1.273(18) . ? C62 F33 1.281(18) . ? C63 C64 1.50(2) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.48(2) . ? C64 C68 1.57(2) . ? C65 C66 1.44(3) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.58(3) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.54(2) . ? C67 H67 0.9800 . ? C68 C69 1.50(3) . ? C68 C70 1.57(3) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 O11 1.218(18) . ? C71 C72 1.41(3) . ? C71 C78 1.51(2) . ? C72 C73 1.40(2) . ? C72 C81 1.55(3) . ? C73 O12 1.318(16) . ? C73 C74 1.48(2) . ? C74 F37 1.314(18) . ? C74 F36 1.333(18) . ? C74 C75 1.59(3) . ? C75 F39 1.36(2) . ? C75 F38 1.39(2) . ? C75 C76 1.47(3) . ? C76 F40 1.31(3) . ? C76 F42 1.32(2) . ? C76 F41 1.35(3) . ? C77 C78 1.57(3) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 C79 1.57(3) . ? C78 C82 1.58(3) . ? C79 C80 1.55(3) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 C81 1.50(3) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 C82 1.52(3) . ? C81 H81 0.9800 . ? C82 C84 1.63(3) . ? C82 C83 1.64(3) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? F26 C48 1.39(3) . ? F27 C48 1.13(3) . ? F28 C48 1.26(3) . ? O1 Yb1 2.271(8) . ? O2 Yb1 2.182(8) . ? O3 Yb1 2.330(9) . ? O4 Yb1 2.204(8) . ? O5 Yb1 2.264(9) . ? O6 Yb1 2.239(8) . ? O7 Yb2 2.254(7) . ? O8 Yb2 2.200(9) . ? O9 Yb2 2.320(8) . ? O10 Yb2 2.180(9) . ? O11 Yb2 2.243(9) . ? O12 Yb2 2.246(8) . ? O1W Yb1 2.329(8) . ? O2W Yb2 2.359(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 127.8(13) . . ? O1 C1 C8 125.4(16) . . ? C2 C1 C8 106.8(15) . . ? C3 C2 C1 121.3(13) . . ? C3 C2 C11 134.2(15) . . ? C1 C2 C11 104.5(14) . . ? O2 C3 C2 124.5(16) . . ? O2 C3 C4 115.4(18) . . ? C2 C3 C4 119.7(17) . . ? F1 C4 F2 102.9(16) . . ? F1 C4 C5 110.3(17) . . ? F2 C4 C5 112.4(16) . . ? F1 C4 C3 107.9(15) . . ? F2 C4 C3 108.1(17) . . ? C5 C4 C3 114.6(17) . . ? F4 C5 F3 111.9(19) . . ? F4 C5 C4 110.2(17) . . ? F3 C5 C4 112.9(16) . . ? F4 C5 C6 98.7(19) . . ? F3 C5 C6 101(2) . . ? C4 C5 C6 121(2) . . ? F7 C6 F6 116(3) . . ? F7 C6 F5 88(3) . . ? F6 C6 F5 118(3) . . ? F7 C6 C5 115(3) . . ? F6 C6 C5 109(3) . . ? F5 C6 C5 109(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 C1 113.6(14) . . ? C7 C8 C9 112.7(17) . . ? C1 C8 C9 103.2(13) . . ? C7 C8 C12 119.8(15) . . ? C1 C8 C12 101.1(15) . . ? C9 C8 C12 104.6(14) . . ? C8 C9 C10 102.9(14) . . ? C8 C9 H9A 111.2 . . ? C10 C9 H9A 111.2 . . ? C8 C9 H9B 111.2 . . ? C10 C9 H9B 111.2 . . ? H9A C9 H9B 109.1 . . ? C9 C10 C11 102.0(14) . . ? C9 C10 H10A 111.4 . . ? C11 C10 H10A 111.4 . . ? C9 C10 H10B 111.4 . . ? C11 C10 H10B 111.4 . . ? H10A C10 H10B 109.2 . . ? C2 C11 C10 108.3(12) . . ? C2 C11 C12 102.5(11) . . ? C10 C11 C12 99.5(14) . . ? C2 C11 H11 114.9 . . ? C10 C11 H11 114.9 . . ? C12 C11 H11 114.9 . . ? C8 C12 C13 109.8(14) . . ? C8 C12 C11 92.0(11) . . ? C13 C12 C11 113.7(14) . . ? C8 C12 C14 113.7(15) . . ? C13 C12 C14 108.0(13) . . ? C11 C12 C14 118.8(15) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 123.9(15) . . ? O3 C15 C22 127.1(15) . . ? C16 C15 C22 108.1(14) . . ? C17 C16 C15 125.6(16) . . ? C17 C16 C25 129.3(17) . . ? C15 C16 C25 104.8(14) . . ? O4 C17 C16 121.6(15) . . ? O4 C17 C18 118.8(18) . . ? C16 C17 C18 119.4(18) . . ? F8 C18 F9 97.7(18) . . ? F8 C18 C17 109.6(16) . . ? F9 C18 C17 115.5(15) . . ? F8 C18 C19 122.1(18) . . ? F9 C18 C19 91.2(15) . . ? C17 C18 C19 117.4(15) . . ? F10 C19 F11 111.0(19) . . ? F10 C19 C18 86(2) . . ? F11 C19 C18 106.8(15) . . ? F10 C19 C20 115(2) . . ? F11 C19 C20 117(2) . . ? C18 C19 C20 117.4(18) . . ? F12 C20 F13 115(3) . . ? F12 C20 F14 114(4) . . ? F13 C20 F14 130(3) . . ? F12 C20 C19 87.1(17) . . ? F13 C20 C19 97(2) . . ? F14 C20 C19 80(2) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 C21 113.0(13) . . ? C15 C22 C26 96.6(14) . . ? C21 C22 C26 118.7(17) . . ? C15 C22 C23 106.6(14) . . ? C21 C22 C23 116.7(15) . . ? C26 C22 C23 102.9(13) . . ? C24 C23 C22 103.1(13) . . ? C24 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? C24 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.1 . . ? C23 C24 C25 104.8(13) . . ? C23 C24 H24A 110.8 . . ? C25 C24 H24A 110.8 . . ? C23 C24 H24B 110.8 . . ? C25 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? C26 C25 C16 98.4(14) . . ? C26 C25 C24 98.5(14) . . ? C16 C25 C24 103.3(15) . . ? C26 C25 H25 117.7 . . ? C16 C25 H25 117.7 . . ? C24 C25 H25 117.7 . . ? C25 C26 C22 98.4(16) . . ? C25 C26 C27 111.7(17) . . ? C22 C26 C27 114.6(16) . . ? C25 C26 C28 111.5(16) . . ? C22 C26 C28 110.9(15) . . ? C27 C26 C28 109.4(18) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 C36 129(2) . . ? O5 C29 C30 126.2(14) . . ? C36 C29 C30 104.6(18) . . ? C31 C30 C29 121.1(14) . . ? C31 C30 C39 138.2(16) . . ? C29 C30 C39 100.7(15) . . ? O6 C31 C30 126.5(14) . . ? O6 C31 C32 113.2(13) . . ? C30 C31 C32 120.3(14) . . ? F15 C32 F16 105.3(17) . . ? F15 C32 C33 107.7(18) . . ? F16 C32 C33 107.3(16) . . ? F15 C32 C31 109.8(15) . . ? F16 C32 C31 109.2(15) . . ? C33 C32 C31 116.9(17) . . ? F18 C33 F17 107.5(16) . . ? F18 C33 C34 107(2) . . ? F17 C33 C34 102(3) . . ? F18 C33 C32 110(2) . . ? F17 C33 C32 108.1(18) . . ? C34 C33 C32 122.2(19) . . ? F21 C34 F19 111(3) . . ? F21 C34 F20 108(3) . . ? F19 C34 F20 110(2) . . ? F21 C34 C33 108(2) . . ? F19 C34 C33 115(2) . . ? F20 C34 C33 103(3) . . ? C36 C35 H35A 109.4 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C40 C36 C37 98(2) . . ? C40 C36 C29 103.8(18) . . ? C37 C36 C29 104.3(16) . . ? C40 C36 C35 119.8(19) . . ? C37 C36 C35 118(2) . . ? C29 C36 C35 110.4(19) . . ? C38 C37 C36 109(3) . . ? C38 C37 H37A 109.8 . . ? C36 C37 H37A 109.8 . . ? C38 C37 H37B 109.8 . . ? C36 C37 H37B 109.8 . . ? H37A C37 H37B 108.3 . . ? C37 C38 C39 100(2) . . ? C37 C38 H38A 111.8 . . ? C39 C38 H38A 111.7 . . ? C37 C38 H38B 111.8 . . ? C39 C38 H38B 111.8 . . ? H38A C38 H38B 109.5 . . ? C40 C39 C30 104.3(17) . . ? C40 C39 C38 99(2) . . ? C30 C39 C38 105.3(19) . . ? C40 C39 H39 115.4 . . ? C30 C39 H39 115.4 . . ? C38 C39 H39 115.4 . . ? C36 C40 C39 97(2) . . ? C36 C40 C42 116(2) . . ? C39 C40 C42 113(2) . . ? C36 C40 C41 112(2) . . ? C39 C40 C41 111(2) . . ? C42 C40 C41 107.7(19) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O7 C43 C44 125.2(15) . . ? O7 C43 C50 127.7(17) . . ? C44 C43 C50 107.1(16) . . ? C45 C44 C43 123.5(18) . . ? C45 C44 C53 132(2) . . ? C43 C44 C53 105(2) . . ? O8 C45 C44 123.0(17) . . ? O8 C45 C46 115(2) . . ? C44 C45 C46 122(2) . . ? F22 C46 F23 104(2) . . ? F22 C46 C47 113(3) . . ? F23 C46 C47 105(2) . . ? F22 C46 C45 113(2) . . ? F23 C46 C45 108(3) . . ? C47 C46 C45 113(2) . . ? F25 C47 F24 97(2) . . ? F25 C47 C48 128(3) . . ? F24 C47 C48 107.7(19) . . ? F25 C47 C46 108.8(19) . . ? F24 C47 C46 102(2) . . ? C48 C47 C46 110(2) . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C43 C50 C49 112.1(16) . . ? C43 C50 C51 101.0(13) . . ? C49 C50 C51 114.2(17) . . ? C43 C50 C54 98.3(13) . . ? C49 C50 C54 125.4(17) . . ? C51 C50 C54 102.2(16) . . ? C50 C51 C52 102.7(16) . . ? C50 C51 H51A 111.2 . . ? C52 C51 H51A 111.2 . . ? C50 C51 H51B 111.2 . . ? C52 C51 H51B 111.2 . . ? H51A C51 H51B 109.1 . . ? C53 C52 C51 101.8(16) . . ? C53 C52 H52A 111.4 . . ? C51 C52 H52A 111.4 . . ? C53 C52 H52B 111.4 . . ? C51 C52 H52B 111.4 . . ? H52A C52 H52B 109.3 . . ? C52 C53 C54 106.3(17) . . ? C52 C53 C44 107.4(17) . . ? C54 C53 C44 99.7(16) . . ? C52 C53 H53 114.1 . . ? C54 C53 H53 114.1 . . ? C44 C53 H53 114.1 . . ? C53 C54 C56 119.7(19) . . ? C53 C54 C50 94.7(12) . . ? C56 C54 C50 112.0(15) . . ? C53 C54 C55 114.1(14) . . ? C56 C54 C55 105.0(13) . . ? C50 C54 C55 111.2(16) . . ? 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 . . ? O9 C57 C58 127.2(13) . . ? O9 C57 C64 125.4(13) . . ? C58 C57 C64 107.3(13) . . ? C59 C58 C57 124.6(14) . . ? C59 C58 C67 132.3(14) . . ? C57 C58 C67 103.0(13) . . ? O10 C59 C58 118.9(13) . . ? O10 C59 C60 112.3(19) . . ? C58 C59 C60 129(2) . . ? F29 C60 F30 113(3) . . ? F29 C60 C61 112(2) . . ? F30 C60 C61 105(3) . . ? F29 C60 C59 109(3) . . ? F30 C60 C59 112(2) . . ? C61 C60 C59 105(2) . . ? F31 C61 F32 113(2) . . ? F31 C61 C62 112.1(17) . . ? F32 C61 C62 96.5(17) . . ? F31 C61 C60 101.0(19) . . ? F32 C61 C60 119(2) . . ? C62 C61 C60 115(2) . . ? F34 C62 F35 113(2) . . ? F34 C62 F33 110.9(17) . . ? F35 C62 F33 113.0(19) . . ? F34 C62 C61 107.5(19) . . ? F35 C62 C61 101(3) . . ? F33 C62 C61 112(2) . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C63 117.4(16) . . ? C65 C64 C57 102.4(14) . . ? C63 C64 C57 115.1(14) . . ? C65 C64 C68 99.9(17) . . ? C63 C64 C68 120.3(14) . . ? C57 C64 C68 98.4(13) . . ? C66 C65 C64 112(2) . . ? C66 C65 H65A 109.2 . . ? C64 C65 H65A 109.2 . . ? C66 C65 H65B 109.1 . . ? C64 C65 H65B 109.1 . . ? H65A C65 H65B 107.9 . . ? C65 C66 C67 99.8(16) . . ? C65 C66 H66A 111.8 . . ? C67 C66 H66A 111.8 . . ? C65 C66 H66B 111.8 . . ? C67 C66 H66B 111.8 . . ? H66A C66 H66B 109.5 . . ? C68 C67 C58 99.5(14) . . ? C68 C67 C66 103.9(17) . . ? C58 C67 C66 105.3(14) . . ? C68 C67 H67 115.4 . . ? C58 C67 H67 115.4 . . ? C66 C67 H67 115.4 . . ? C69 C68 C67 117.3(19) . . ? C69 C68 C70 106.5(18) . . ? C67 C68 C70 111.0(18) . . ? C69 C68 C64 115.0(19) . . ? C67 C68 C64 93.8(14) . . ? C70 C68 C64 113.1(16) . . ? 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 . . ? O11 C71 C72 127.8(16) . . ? O11 C71 C78 125.9(15) . . ? C72 C71 C78 106.2(17) . . ? C73 C72 C71 124(2) . . ? C73 C72 C81 128(2) . . ? C71 C72 C81 106.9(16) . . ? O12 C73 C72 122.7(16) . . ? O12 C73 C74 111.2(15) . . ? C72 C73 C74 124.4(17) . . ? F37 C74 F36 107.7(15) . . ? F37 C74 C73 112.5(15) . . ? F36 C74 C73 113.3(13) . . ? F37 C74 C75 100.5(14) . . ? F36 C74 C75 105.9(15) . . ? C73 C74 C75 115.8(15) . . ? F39 C75 F38 105.9(15) . . ? F39 C75 C76 111(2) . . ? F38 C75 C76 106.6(19) . . ? F39 C75 C74 109.5(16) . . ? F38 C75 C74 106.6(18) . . ? C76 C75 C74 117.0(17) . . ? F40 C76 F42 105.7(17) . . ? F40 C76 F41 109(3) . . ? F42 C76 F41 106(2) . . ? F40 C76 C75 115(2) . . ? F42 C76 C75 112(2) . . ? F41 C76 C75 108.8(19) . . ? C78 C77 H77A 109.5 . . ? C78 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C78 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C71 C78 C79 103.0(15) . . ? C71 C78 C77 115.0(18) . . ? C79 C78 C77 118.8(17) . . ? C71 C78 C82 100.3(14) . . ? C79 C78 C82 98.2(17) . . ? C77 C78 C82 118.5(18) . . ? C80 C79 C78 105.6(18) . . ? C80 C79 H79A 110.6 . . ? C78 C79 H79A 110.6 . . ? C80 C79 H79B 110.6 . . ? C78 C79 H79B 110.6 . . ? H79A C79 H79B 108.8 . . ? C81 C80 C79 102.3(19) . . ? C81 C80 H80A 111.3 . . ? C79 C80 H80A 111.3 . . ? C81 C80 H80B 111.3 . . ? C79 C80 H80B 111.3 . . ? H80A C80 H80B 109.2 . . ? C80 C81 C82 104.1(16) . . ? C80 C81 C72 107.2(17) . . ? C82 C81 C72 97.7(16) . . ? C80 C81 H81 115.3 . . ? C82 C81 H81 115.3 . . ? C72 C81 H81 115.3 . . ? C81 C82 C78 95.0(15) . . ? C81 C82 C84 109.7(18) . . ? C78 C82 C84 114.9(17) . . ? C81 C82 C83 115.9(18) . . ? C78 C82 C83 111.4(18) . . ? C84 C82 C83 109.5(17) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C1 O1 Yb1 131.3(10) . . ? C3 O2 Yb1 138.1(11) . . ? C15 O3 Yb1 131.8(10) . . ? C17 O4 Yb1 140.5(11) . . ? C29 O5 Yb1 133.6(12) . . ? C31 O6 Yb1 135.0(9) . . ? C43 O7 Yb2 135.0(10) . . ? C45 O8 Yb2 138.1(11) . . ? C57 O9 Yb2 129.9(9) . . ? C59 O10 Yb2 139.2(11) . . ? C71 O11 Yb2 133.5(9) . . ? C73 O12 Yb2 134.0(9) . . ? O2 Yb1 O4 85.3(4) . . ? O2 Yb1 O6 164.3(4) . . ? O4 Yb1 O6 103.2(3) . . ? O2 Yb1 O5 118.4(4) . . ? O4 Yb1 O5 77.0(4) . . ? O6 Yb1 O5 76.8(4) . . ? O2 Yb1 O1 76.6(4) . . ? O4 Yb1 O1 130.7(4) . . ? O6 Yb1 O1 106.4(4) . . ? O5 Yb1 O1 72.6(3) . . ? O2 Yb1 O1W 86.1(3) . . ? O4 Yb1 O1W 149.0(3) . . ? O6 Yb1 O1W 79.8(3) . . ? O5 Yb1 O1W 132.7(4) . . ? O1 Yb1 O1W 75.5(3) . . ? O2 Yb1 O3 86.5(3) . . ? O4 Yb1 O3 74.9(4) . . ? O6 Yb1 O3 83.1(4) . . ? O5 Yb1 O3 140.4(3) . . ? O1 Yb1 O3 146.6(3) . . ? O1W Yb1 O3 74.8(3) . . ? O10 Yb2 O8 85.4(4) . . ? O10 Yb2 O11 78.0(4) . . ? O8 Yb2 O11 119.0(4) . . ? O10 Yb2 O12 99.6(4) . . ? O8 Yb2 O12 163.7(4) . . ? O11 Yb2 O12 77.3(3) . . ? O10 Yb2 O7 127.3(4) . . ? O8 Yb2 O7 74.9(4) . . ? O11 Yb2 O7 70.5(4) . . ? O12 Yb2 O7 112.9(3) . . ? O10 Yb2 O9 74.9(3) . . ? O8 Yb2 O9 83.1(4) . . ? O11 Yb2 O9 143.3(4) . . ? O12 Yb2 O9 83.3(3) . . ? O7 Yb2 O9 146.2(3) . . ? O10 Yb2 O2W 149.9(3) . . ? O8 Yb2 O2W 87.1(4) . . ? O11 Yb2 O2W 130.4(4) . . ? O12 Yb2 O2W 80.8(3) . . ? O7 Yb2 O2W 78.3(3) . . ? O9 Yb2 O2W 75.3(3) . . ? F27 C48 F28 122(3) . . ? F27 C48 F26 111(2) . . ? F28 C48 F26 99(3) . . ? F27 C48 C47 121(3) . . ? F28 C48 C47 103(2) . . ? F26 C48 C47 95.4(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -1(2) . . . . ? C8 C1 C2 C3 -179.9(13) . . . . ? O1 C1 C2 C11 177.5(13) . . . . ? C8 C1 C2 C11 -1.2(15) . . . . ? C1 C2 C3 O2 -5(2) . . . . ? C11 C2 C3 O2 177.0(14) . . . . ? C1 C2 C3 C4 -176.9(14) . . . . ? C11 C2 C3 C4 5(3) . . . . ? O2 C3 C4 F1 39(2) . . . . ? C2 C3 C4 F1 -148.4(15) . . . . ? O2 C3 C4 F2 149.4(15) . . . . ? C2 C3 C4 F2 -38(2) . . . . ? O2 C3 C4 C5 -84(2) . . . . ? C2 C3 C4 C5 88(2) . . . . ? F1 C4 C5 F4 175.1(17) . . . . ? F2 C4 C5 F4 61(2) . . . . ? C3 C4 C5 F4 -63(2) . . . . ? F1 C4 C5 F3 -59(2) . . . . ? F2 C4 C5 F3 -173.2(19) . . . . ? C3 C4 C5 F3 63(2) . . . . ? F1 C4 C5 C6 61(3) . . . . ? F2 C4 C5 C6 -53(3) . . . . ? C3 C4 C5 C6 -177(2) . . . . ? F4 C5 C6 F7 -161(3) . . . . ? F3 C5 C6 F7 85(3) . . . . ? C4 C5 C6 F7 -41(4) . . . . ? F4 C5 C6 F6 67(3) . . . . ? F3 C5 C6 F6 -48(3) . . . . ? C4 C5 C6 F6 -173(3) . . . . ? F4 C5 C6 F5 -64(3) . . . . ? F3 C5 C6 F5 -178(3) . . . . ? C4 C5 C6 F5 56(4) . . . . ? O1 C1 C8 C7 18(2) . . . . ? C2 C1 C8 C7 -163.5(15) . . . . ? O1 C1 C8 C9 -104.6(17) . . . . ? C2 C1 C8 C9 74.1(16) . . . . ? O1 C1 C8 C12 147.4(14) . . . . ? C2 C1 C8 C12 -33.9(15) . . . . ? C7 C8 C9 C10 163.3(13) . . . . ? C1 C8 C9 C10 -73.8(16) . . . . ? C12 C8 C9 C10 31.6(16) . . . . ? C8 C9 C10 C11 6.7(16) . . . . ? C3 C2 C11 C10 109(2) . . . . ? C1 C2 C11 C10 -69.1(16) . . . . ? C3 C2 C11 C12 -146.1(18) . . . . ? C1 C2 C11 C12 35.5(14) . . . . ? C9 C10 C11 C2 65.1(16) . . . . ? C9 C10 C11 C12 -41.6(14) . . . . ? C7 C8 C12 C13 61(2) . . . . ? C1 C8 C12 C13 -65.1(17) . . . . ? C9 C8 C12 C13 -172.0(14) . . . . ? C7 C8 C12 C11 176.6(15) . . . . ? C1 C8 C12 C11 51.0(14) . . . . ? C9 C8 C12 C11 -55.9(15) . . . . ? C7 C8 C12 C14 -61(2) . . . . ? C1 C8 C12 C14 173.9(15) . . . . ? C9 C8 C12 C14 66.9(19) . . . . ? C2 C11 C12 C8 -53.2(13) . . . . ? C10 C11 C12 C8 58.1(12) . . . . ? C2 C11 C12 C13 59.4(16) . . . . ? C10 C11 C12 C13 170.8(13) . . . . ? C2 C11 C12 C14 -171.8(15) . . . . ? C10 C11 C12 C14 -60.4(18) . . . . ? O3 C15 C16 C17 -9(3) . . . . ? C22 C15 C16 C17 -178(2) . . . . ? O3 C15 C16 C25 177.1(16) . . . . ? C22 C15 C16 C25 7(2) . . . . ? C15 C16 C17 O4 1(4) . . . . ? C25 C16 C17 O4 174(2) . . . . ? C15 C16 C17 C18 176.0(19) . . . . ? C25 C16 C17 C18 -11(4) . . . . ? O4 C17 C18 F8 -108(3) . . . . ? C16 C17 C18 F8 77(3) . . . . ? O4 C17 C18 F9 143(2) . . . . ? C16 C17 C18 F9 -33(3) . . . . ? O4 C17 C18 C19 37(3) . . . . ? C16 C17 C18 C19 -138(2) . . . . ? F8 C18 C19 F10 66(2) . . . . ? F9 C18 C19 F10 165.6(17) . . . . ? C17 C18 C19 F10 -75(2) . . . . ? F8 C18 C19 F11 176.5(19) . . . . ? F9 C18 C19 F11 -83.7(18) . . . . ? C17 C18 C19 F11 36(2) . . . . ? F8 C18 C19 C20 -50(3) . . . . ? F9 C18 C19 C20 50(3) . . . . ? C17 C18 C19 C20 170(2) . . . . ? F10 C19 C20 F12 51(4) . . . . ? F11 C19 C20 F12 -82(3) . . . . ? C18 C19 C20 F12 150(3) . . . . ? F10 C19 C20 F13 -64(3) . . . . ? F11 C19 C20 F13 163(2) . . . . ? C18 C19 C20 F13 34(3) . . . . ? F10 C19 C20 F14 166(3) . . . . ? F11 C19 C20 F14 33(3) . . . . ? C18 C19 C20 F14 -96(3) . . . . ? O3 C15 C22 C21 27(3) . . . . ? C16 C15 C22 C21 -164.1(17) . . . . ? O3 C15 C22 C26 151.7(17) . . . . ? C16 C15 C22 C26 -39.0(18) . . . . ? O3 C15 C22 C23 -102.7(18) . . . . ? C16 C15 C22 C23 66.5(18) . . . . ? C15 C22 C23 C24 -72.1(17) . . . . ? C21 C22 C23 C24 160.7(16) . . . . ? C26 C22 C23 C24 29.0(18) . . . . ? C22 C23 C24 C25 4.5(19) . . . . ? C17 C16 C25 C26 -146(2) . . . . ? C15 C16 C25 C26 27.7(19) . . . . ? C17 C16 C25 C24 113(2) . . . . ? C15 C16 C25 C24 -73.2(18) . . . . ? C23 C24 C25 C26 -36.6(19) . . . . ? C23 C24 C25 C16 64.2(18) . . . . ? C16 C25 C26 C22 -51.2(15) . . . . ? C24 C25 C26 C22 53.7(15) . . . . ? C16 C25 C26 C27 69.5(19) . . . . ? C24 C25 C26 C27 174.4(16) . . . . ? C16 C25 C26 C28 -167.7(16) . . . . ? C24 C25 C26 C28 -62.8(19) . . . . ? C15 C22 C26 C25 55.6(14) . . . . ? C21 C22 C26 C25 176.3(15) . . . . ? C23 C22 C26 C25 -53.1(15) . . . . ? C15 C22 C26 C27 -63(2) . . . . ? C21 C22 C26 C27 58(2) . . . . ? C23 C22 C26 C27 -171.8(17) . . . . ? C15 C22 C26 C28 172.5(16) . . . . ? C21 C22 C26 C28 -67(2) . . . . ? C23 C22 C26 C28 64(2) . . . . ? O5 C29 C30 C31 -5(3) . . . . ? C36 C29 C30 C31 178.9(14) . . . . ? O5 C29 C30 C39 176.5(17) . . . . ? C36 C29 C30 C39 0.0(18) . . . . ? C29 C30 C31 O6 -4(2) . . . . ? C39 C30 C31 O6 173.8(19) . . . . ? C29 C30 C31 C32 177.0(15) . . . . ? C39 C30 C31 C32 -5(3) . . . . ? O6 C31 C32 F15 -140.4(15) . . . . ? C30 C31 C32 F15 38(2) . . . . ? O6 C31 C32 F16 -25(2) . . . . ? C30 C31 C32 F16 153.3(15) . . . . ? O6 C31 C32 C33 96.6(19) . . . . ? C30 C31 C32 C33 -85(2) . . . . ? F15 C32 C33 F18 64(2) . . . . ? F16 C32 C33 F18 -48(2) . . . . ? C31 C32 C33 F18 -171.4(17) . . . . ? F15 C32 C33 F17 -53(2) . . . . ? F16 C32 C33 F17 -165.4(18) . . . . ? C31 C32 C33 F17 72(2) . . . . ? F15 C32 C33 C34 -170(2) . . . . ? F16 C32 C33 C34 77(3) . . . . ? C31 C32 C33 C34 -46(3) . . . . ? F18 C33 C34 F21 -171(2) . . . . ? F17 C33 C34 F21 -58(2) . . . . ? C32 C33 C34 F21 62(4) . . . . ? F18 C33 C34 F19 -46(3) . . . . ? F17 C33 C34 F19 66(3) . . . . ? C32 C33 C34 F19 -173(2) . . . . ? F18 C33 C34 F20 74(2) . . . . ? F17 C33 C34 F20 -173.3(16) . . . . ? C32 C33 C34 F20 -53(3) . . . . ? O5 C29 C36 C40 151(2) . . . . ? C30 C29 C36 C40 -33(2) . . . . ? O5 C29 C36 C37 -106(2) . . . . ? C30 C29 C36 C37 70(2) . . . . ? O5 C29 C36 C35 21(3) . . . . ? C30 C29 C36 C35 -162.2(16) . . . . ? C40 C36 C37 C38 35(3) . . . . ? C29 C36 C37 C38 -72(3) . . . . ? C35 C36 C37 C38 165(2) . . . . ? C36 C37 C38 C39 0(3) . . . . ? C31 C30 C39 C40 -147(2) . . . . ? C29 C30 C39 C40 32(2) . . . . ? C31 C30 C39 C38 110(2) . . . . ? C29 C30 C39 C38 -72(2) . . . . ? C37 C38 C39 C40 -35(2) . . . . ? C37 C38 C39 C30 73(2) . . . . ? C37 C36 C40 C39 -55.7(19) . . . . ? C29 C36 C40 C39 51(2) . . . . ? C35 C36 C40 C39 175.0(17) . . . . ? C37 C36 C40 C42 64(2) . . . . ? C29 C36 C40 C42 171(2) . . . . ? C35 C36 C40 C42 -65(3) . . . . ? C37 C36 C40 C41 -171.7(17) . . . . ? C29 C36 C40 C41 -65(2) . . . . ? C35 C36 C40 C41 59(2) . . . . ? C30 C39 C40 C36 -52(2) . . . . ? C38 C39 C40 C36 57(2) . . . . ? C30 C39 C40 C42 -174(2) . . . . ? C38 C39 C40 C42 -65(3) . . . . ? C30 C39 C40 C41 65(2) . . . . ? C38 C39 C40 C41 173.5(19) . . . . ? O7 C43 C44 C45 -4(3) . . . . ? C50 C43 C44 C45 176(2) . . . . ? O7 C43 C44 C53 178.5(13) . . . . ? C50 C43 C44 C53 -1(2) . . . . ? C43 C44 C45 O8 8(4) . . . . ? C53 C44 C45 O8 -175(2) . . . . ? C43 C44 C45 C46 -175(2) . . . . ? C53 C44 C45 C46 2(4) . . . . ? O8 C45 C46 F22 -147(2) . . . . ? C44 C45 C46 F22 36(4) . . . . ? O8 C45 C46 F23 -32(3) . . . . ? C44 C45 C46 F23 151(2) . . . . ? O8 C45 C46 C47 84(3) . . . . ? C44 C45 C46 C47 -94(3) . . . . ? F22 C46 C47 F25 -169(2) . . . . ? F23 C46 C47 F25 78(3) . . . . ? C45 C46 C47 F25 -40(3) . . . . ? F22 C46 C47 F24 -67(3) . . . . ? F23 C46 C47 F24 180(2) . . . . ? C45 C46 C47 F24 63(3) . . . . ? F22 C46 C47 C48 47(3) . . . . ? F23 C46 C47 C48 -66(3) . . . . ? C45 C46 C47 C48 177(2) . . . . ? O7 C43 C50 C49 13(2) . . . . ? C44 C43 C50 C49 -166.6(18) . . . . ? O7 C43 C50 C51 -108.6(17) . . . . ? C44 C43 C50 C51 71.4(18) . . . . ? O7 C43 C50 C54 147.2(14) . . . . ? C44 C43 C50 C54 -32.9(18) . . . . ? C43 C50 C51 C52 -73.0(17) . . . . ? C49 C50 C51 C52 166.5(15) . . . . ? C54 C50 C51 C52 28.2(16) . . . . ? C50 C51 C52 C53 5.2(18) . . . . ? C51 C52 C53 C54 -39.1(18) . . . . ? C51 C52 C53 C44 67(2) . . . . ? C45 C44 C53 C52 109(3) . . . . ? C43 C44 C53 C52 -74(2) . . . . ? C45 C44 C53 C54 -141(3) . . . . ? C43 C44 C53 C54 37(2) . . . . ? C52 C53 C54 C56 175.0(15) . . . . ? C44 C53 C54 C56 63(2) . . . . ? C52 C53 C54 C50 56.3(16) . . . . ? C44 C53 C54 C50 -55.2(15) . . . . ? C52 C53 C54 C55 -59(2) . . . . ? C44 C53 C54 C55 -170.9(17) . . . . ? C43 C50 C54 C53 53.8(14) . . . . ? C49 C50 C54 C53 178.5(17) . . . . ? C51 C50 C54 C53 -49.5(14) . . . . ? C43 C50 C54 C56 -70.9(19) . . . . ? C49 C50 C54 C56 54(2) . . . . ? C51 C50 C54 C56 -174.2(16) . . . . ? C43 C50 C54 C55 171.9(14) . . . . ? C49 C50 C54 C55 -63(2) . . . . ? C51 C50 C54 C55 68.7(17) . . . . ? O9 C57 C58 C59 -2(3) . . . . ? C64 C57 C58 C59 179.8(16) . . . . ? O9 C57 C58 C67 175.1(15) . . . . ? C64 C57 C58 C67 -3.6(16) . . . . ? C57 C58 C59 O10 0(3) . . . . ? C67 C58 C59 O10 -175.2(17) . . . . ? C57 C58 C59 C60 178(2) . . . . ? C67 C58 C59 C60 2(3) . . . . ? O10 C59 C60 F29 157(2) . . . . ? C58 C59 C60 F29 -20(3) . . . . ? O10 C59 C60 F30 32(3) . . . . ? C58 C59 C60 F30 -146(3) . . . . ? O10 C59 C60 C61 -82(2) . . . . ? C58 C59 C60 C61 100(3) . . . . ? F29 C60 C61 F31 46(3) . . . . ? F30 C60 C61 F31 169(2) . . . . ? C59 C60 C61 F31 -72(2) . . . . ? F29 C60 C61 F32 170(2) . . . . ? F30 C60 C61 F32 -66(3) . . . . ? C59 C60 C61 F32 52(3) . . . . ? F29 C60 C61 C62 -75(3) . . . . ? F30 C60 C61 C62 48(3) . . . . ? C59 C60 C61 C62 166.8(19) . . . . ? F31 C61 C62 F34 34(3) . . . . ? F32 C61 C62 F34 -84(2) . . . . ? C60 C61 C62 F34 149(2) . . . . ? F31 C61 C62 F35 152(3) . . . . ? F32 C61 C62 F35 34(3) . . . . ? C60 C61 C62 F35 -93(3) . . . . ? F31 C61 C62 F33 -88(3) . . . . ? F32 C61 C62 F33 154(3) . . . . ? C60 C61 C62 F33 27(3) . . . . ? O9 C57 C64 C65 -109.0(18) . . . . ? C58 C57 C64 C65 69.6(17) . . . . ? O9 C57 C64 C63 19(2) . . . . ? C58 C57 C64 C63 -161.8(14) . . . . ? O9 C57 C64 C68 148.8(16) . . . . ? C58 C57 C64 C68 -32.6(16) . . . . ? C63 C64 C65 C66 166.1(17) . . . . ? C57 C64 C65 C66 -67(2) . . . . ? C68 C64 C65 C66 34(2) . . . . ? C64 C65 C66 C67 -2(2) . . . . ? C59 C58 C67 C68 -144(2) . . . . ? C57 C58 C67 C68 39.3(17) . . . . ? C59 C58 C67 C66 108(2) . . . . ? C57 C58 C67 C66 -68.0(16) . . . . ? C65 C66 C67 C68 -32.3(19) . . . . ? C65 C66 C67 C58 71.8(19) . . . . ? C58 C67 C68 C69 63(2) . . . . ? C66 C67 C68 C69 171.5(18) . . . . ? C58 C67 C68 C70 -174.2(17) . . . . ? C66 C67 C68 C70 -66(2) . . . . ? C58 C67 C68 C64 -57.7(17) . . . . ? C66 C67 C68 C64 50.8(17) . . . . ? C65 C64 C68 C69 -172.3(18) . . . . ? C63 C64 C68 C69 58(2) . . . . ? C57 C64 C68 C69 -68.1(18) . . . . ? C65 C64 C68 C67 -49.8(17) . . . . ? C63 C64 C68 C67 -179.8(16) . . . . ? C57 C64 C68 C67 54.4(17) . . . . ? C65 C64 C68 C70 65(2) . . . . ? C63 C64 C68 C70 -65(2) . . . . ? C57 C64 C68 C70 169.2(17) . . . . ? O11 C71 C72 C73 10(3) . . . . ? C78 C71 C72 C73 -171.4(17) . . . . ? O11 C71 C72 C81 175.9(17) . . . . ? C78 C71 C72 C81 -6(2) . . . . ? C71 C72 C73 O12 -11(3) . . . . ? C81 C72 C73 O12 -173.7(17) . . . . ? C71 C72 C73 C74 -175.3(17) . . . . ? C81 C72 C73 C74 22(3) . . . . ? O12 C73 C74 F37 153.5(14) . . . . ? C72 C73 C74 F37 -41(2) . . . . ? O12 C73 C74 F36 31.1(19) . . . . ? C72 C73 C74 F36 -163.4(16) . . . . ? O12 C73 C74 C75 -91.6(17) . . . . ? C72 C73 C74 C75 74(2) . . . . ? F37 C74 C75 F39 53.2(19) . . . . ? F36 C74 C75 F39 165.2(15) . . . . ? C73 C74 C75 F39 -68(2) . . . . ? F37 C74 C75 F38 -60.9(18) . . . . ? F36 C74 C75 F38 51.1(19) . . . . ? C73 C74 C75 F38 177.6(16) . . . . ? F37 C74 C75 C76 -180.0(19) . . . . ? F36 C74 C75 C76 -68(2) . . . . ? C73 C74 C75 C76 59(3) . . . . ? F39 C75 C76 F40 178.8(17) . . . . ? F38 C75 C76 F40 -67(2) . . . . ? C74 C75 C76 F40 53(3) . . . . ? F39 C75 C76 F42 -60(2) . . . . ? F38 C75 C76 F42 54(3) . . . . ? C74 C75 C76 F42 173.4(17) . . . . ? F39 C75 C76 F41 56(2) . . . . ? F38 C75 C76 F41 170.8(18) . . . . ? C74 C75 C76 F41 -70(3) . . . . ? O11 C71 C78 C79 -110(2) . . . . ? C72 C71 C78 C79 72(2) . . . . ? O11 C71 C78 C77 21(3) . . . . ? C72 C71 C78 C77 -157.1(18) . . . . ? O11 C71 C78 C82 149.4(18) . . . . ? C72 C71 C78 C82 -29(2) . . . . ? C71 C78 C79 C80 -68.6(19) . . . . ? C77 C78 C79 C80 163.0(19) . . . . ? C82 C78 C79 C80 34.0(18) . . . . ? C78 C79 C80 C81 -1(2) . . . . ? C79 C80 C81 C82 -35.3(19) . . . . ? C79 C80 C81 C72 68(2) . . . . ? C73 C72 C81 C80 97(2) . . . . ? C71 C72 C81 C80 -68(2) . . . . ? C73 C72 C81 C82 -155.7(19) . . . . ? C71 C72 C81 C82 40(2) . . . . ? C80 C81 C82 C78 56.3(17) . . . . ? C72 C81 C82 C78 -53.7(17) . . . . ? C80 C81 C82 C84 -62(2) . . . . ? C72 C81 C82 C84 -172.5(18) . . . . ? C80 C81 C82 C83 173.0(18) . . . . ? C72 C81 C82 C83 63(2) . . . . ? C71 C78 C82 C81 51.8(17) . . . . ? C79 C78 C82 C81 -53.1(16) . . . . ? C77 C78 C82 C81 177.7(18) . . . . ? C71 C78 C82 C84 166.3(18) . . . . ? C79 C78 C82 C84 61(2) . . . . ? C77 C78 C82 C84 -68(3) . . . . ? C71 C78 C82 C83 -69(2) . . . . ? C79 C78 C82 C83 -173.4(16) . . . . ? C77 C78 C82 C83 57(2) . . . . ? C2 C1 O1 Yb1 3(2) . . . . ? C8 C1 O1 Yb1 -178.7(10) . . . . ? C2 C3 O2 Yb1 10(3) . . . . ? C4 C3 O2 Yb1 -177.8(11) . . . . ? C16 C15 O3 Yb1 17(2) . . . . ? C22 C15 O3 Yb1 -175.1(11) . . . . ? C16 C17 O4 Yb1 -3(4) . . . . ? C18 C17 O4 Yb1 -178.3(11) . . . . ? C36 C29 O5 Yb1 -173.8(12) . . . . ? C30 C29 O5 Yb1 11(3) . . . . ? C30 C31 O6 Yb1 7(2) . . . . ? C32 C31 O6 Yb1 -173.9(11) . . . . ? C44 C43 O7 Yb2 -2(2) . . . . ? C50 C43 O7 Yb2 178.2(11) . . . . ? C44 C45 O8 Yb2 -8(4) . . . . ? C46 C45 O8 Yb2 175.2(13) . . . . ? C58 C57 O9 Yb2 -15(2) . . . . ? C64 C57 O9 Yb2 163.7(10) . . . . ? C58 C59 O10 Yb2 21(3) . . . . ? C60 C59 O10 Yb2 -156.6(15) . . . . ? C72 C71 O11 Yb2 -9(3) . . . . ? C78 C71 O11 Yb2 173.4(13) . . . . ? C72 C73 O12 Yb2 12(2) . . . . ? C74 C73 O12 Yb2 177.4(9) . . . . ? C3 O2 Yb1 O4 -140.3(15) . . . . ? C3 O2 Yb1 O6 96.3(19) . . . . ? C3 O2 Yb1 O5 -67.8(16) . . . . ? C3 O2 Yb1 O1 -6.4(15) . . . . ? C3 O2 Yb1 O1W 69.6(15) . . . . ? C3 O2 Yb1 O3 144.6(15) . . . . ? C17 O4 Yb1 O2 -81(2) . . . . ? C17 O4 Yb1 O6 86(2) . . . . ? C17 O4 Yb1 O5 159(2) . . . . ? C17 O4 Yb1 O1 -148(2) . . . . ? C17 O4 Yb1 O1W -6(3) . . . . ? C17 O4 Yb1 O3 7(2) . . . . ? C31 O6 Yb1 O2 -168.2(12) . . . . ? C31 O6 Yb1 O4 70.4(12) . . . . ? C31 O6 Yb1 O5 -2.6(12) . . . . ? C31 O6 Yb1 O1 -69.7(12) . . . . ? C31 O6 Yb1 O1W -141.2(12) . . . . ? C31 O6 Yb1 O3 143.1(12) . . . . ? C29 O5 Yb1 O2 169.2(14) . . . . ? C29 O5 Yb1 O4 -113.6(15) . . . . ? C29 O5 Yb1 O6 -6.5(14) . . . . ? C29 O5 Yb1 O1 105.7(15) . . . . ? C29 O5 Yb1 O1W 56.0(16) . . . . ? C29 O5 Yb1 O3 -67.9(17) . . . . ? C1 O1 Yb1 O2 -0.1(11) . . . . ? C1 O1 Yb1 O4 71.4(12) . . . . ? C1 O1 Yb1 O6 -164.1(11) . . . . ? C1 O1 Yb1 O5 125.8(12) . . . . ? C1 O1 Yb1 O1W -89.5(11) . . . . ? C1 O1 Yb1 O3 -61.6(14) . . . . ? C15 O3 Yb1 O2 72.5(14) . . . . ? C15 O3 Yb1 O4 -13.6(13) . . . . ? C15 O3 Yb1 O6 -119.2(14) . . . . ? C15 O3 Yb1 O5 -59.7(16) . . . . ? C15 O3 Yb1 O1 131.4(13) . . . . ? C15 O3 Yb1 O1W 159.5(14) . . . . ? C59 O10 Yb2 O8 58.0(16) . . . . ? C59 O10 Yb2 O11 179.0(16) . . . . ? C59 O10 Yb2 O12 -106.4(16) . . . . ? C59 O10 Yb2 O7 125.1(15) . . . . ? C59 O10 Yb2 O9 -26.1(15) . . . . ? C59 O10 Yb2 O2W -18(2) . . . . ? C45 O8 Yb2 O10 133(2) . . . . ? C45 O8 Yb2 O11 60(2) . . . . ? C45 O8 Yb2 O12 -118(2) . . . . ? C45 O8 Yb2 O7 2.6(19) . . . . ? C45 O8 Yb2 O9 -151(2) . . . . ? C45 O8 Yb2 O2W -76.0(19) . . . . ? C71 O11 Yb2 O10 108.4(15) . . . . ? C71 O11 Yb2 O8 -173.8(14) . . . . ? C71 O11 Yb2 O12 5.6(14) . . . . ? C71 O11 Yb2 O7 -114.6(15) . . . . ? C71 O11 Yb2 O9 65.3(17) . . . . ? C71 O11 Yb2 O2W -60.4(16) . . . . ? C73 O12 Yb2 O10 -82.5(12) . . . . ? C73 O12 Yb2 O8 170.8(13) . . . . ? C73 O12 Yb2 O11 -7.2(12) . . . . ? C73 O12 Yb2 O7 55.1(12) . . . . ? C73 O12 Yb2 O9 -155.8(12) . . . . ? C73 O12 Yb2 O2W 128.1(12) . . . . ? C43 O7 Yb2 O10 -69.8(13) . . . . ? C43 O7 Yb2 O8 2.2(11) . . . . ? C43 O7 Yb2 O11 -126.7(13) . . . . ? C43 O7 Yb2 O12 167.0(11) . . . . ? C43 O7 Yb2 O9 53.4(15) . . . . ? C43 O7 Yb2 O2W 92.4(12) . . . . ? C57 O9 Yb2 O10 20.6(12) . . . . ? C57 O9 Yb2 O8 -66.5(12) . . . . ? C57 O9 Yb2 O11 64.4(13) . . . . ? C57 O9 Yb2 O12 122.5(12) . . . . ? C57 O9 Yb2 O7 -115.7(12) . . . . ? C57 O9 Yb2 O2W -155.3(12) . . . . ? F25 C47 C48 F27 169(3) . . . . ? F24 C47 C48 F27 54(4) . . . . ? C46 C47 C48 F27 -56(4) . . . . ? F25 C47 C48 F28 -50(4) . . . . ? F24 C47 C48 F28 -165(2) . . . . ? C46 C47 C48 F28 85(3) . . . . ? F25 C47 C48 F26 50(3) . . . . ? F24 C47 C48 F26 -64(3) . . . . ? C46 C47 C48 F26 -174(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.583 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.112 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_IV _database_code_depnum_ccdc_archive 'CCDC 777708' #TrackingRef '- CIF-R.cif' # start Validation Reply Form _vrf_PLAT241_IV ; PROBLEM: Check High Ueq as Compared to Neighbors for C24 RESPONSE: Many crystals tried, best presented - the static/positional disorder of the ligand lead to this anomalous value. ; _vrf_PLAT242_IV ; PROBLEM: Check Low Ueq as Compared to Neighbors for C20 RESPONSE: Many crystals tried, best presented - the static/positional disorder of the ligand lead to this anomalous value. ; _vrf_PLAT602_IV ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The lattice contains large solvent accessible voids, but the solvent was highly disordered and therefore could not be modeled. Instead, the disordered solvent was accounted for using the program SQUEEZE, which estimated that 188 electrons were located in the voids of 1201.8 A3, which is equivalent to 1 molecules of CHCl3 and 3 molecules of hexane; these were included in the formula in Table 2. ; _vrf_PLAT112_IV ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 RESPONSE: see comments under _refine_special_details ; _vrf_PLAT860_IV ; PROBLEM: Note: Number of Least-Squares Restraints ....... 23 RESPONSE: Owing to the static/positional disorder of the ligand, 23 least-squares restraints were used to refine the structure.The restraints are listed under _refine_special_details ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84.33 H78.33 Cl F21 O8 P2 Yb' _chemical_formula_weight 1889.23 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 14.862(2) _cell_length_b 14.862(2) _cell_length_c 34.432(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6586(2) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4861 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 22.29 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2863 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50295 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17175 _reflns_number_gt 13657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There is one crystallographically independent molecule on a general position in this structure. Increasing the space group symmetry from P31 to P3121 effectively adds a 2-fold rotation axis through the Yb center and C16 with the Yb located on the rotation axis. While the belta-diketone ligands containing O1O2 and O5O6 and TPPO ligands are compatible with this symmetry element the belta-diketone ligands containing O3O4 are not. The ligands suffer from the static/positional disorder which is incompatible with the 2-fold axis. It is thus proposed that this rotation is a pseudo-symmetry element only, rather than a genuine symmetry element. This is supported by the ADDSYM-EXT routine in PLATON, which does not detect missed symmetry in space group P31. For these reasons, we are convinced that P31 is the correct space group for this complex. dfix 2.50 0.02 C18 C20 dfix 2.10 0.02 F12 F13 F13 F14 F14 F12 dfix 1.54 0.02 C25 C26 C22 C23 dfix 1.54 0.02 C19 C20 dfix 1.35 0.02 F14 C20 F12 C20 F13 C20 C19 F10 dfix 2.40 0.02 C22 C25 dfix 1.54 0.02 C25 C24 C26 C28 dfix 1.54 0.02 C24 C23 delu 0.01 C26 C27 C16 C25 delu 0.01 F10 C19 delu 0.01 C19 C20 ; _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^)+(0.1297P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.042(10) _refine_ls_number_reflns 17175 _refine_ls_number_parameters 964 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1761 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.128 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8046(8) 0.4128(7) 0.2827(2) 0.082(2) Uani 1 1 d . . . C2 C 0.7291(8) 0.4410(7) 0.2719(3) 0.082(2) Uani 1 1 d . . . C3 C 0.7495(8) 0.5415(8) 0.2742(2) 0.082(3) Uani 1 1 d . . . C4 C 0.6585(9) 0.5685(8) 0.2628(3) 0.106(3) Uani 1 1 d . . . C5 C 0.6602(10) 0.6038(12) 0.2234(4) 0.119(4) Uani 1 1 d . . . C6 C 0.5859(14) 0.6463(19) 0.2155(5) 0.152(7) Uani 1 1 d . . . C7 C 0.8225(11) 0.2510(8) 0.2822(4) 0.118(4) Uani 1 1 d . . . H7A H 0.7904 0.1828 0.2710 0.177 Uiso 1 1 calc R . . H7B H 0.8401 0.2476 0.3088 0.177 Uiso 1 1 calc R . . H7C H 0.8845 0.2965 0.2680 0.177 Uiso 1 1 calc R . . C8 C 0.7485(10) 0.2919(7) 0.2805(3) 0.100(3) Uani 1 1 d . . . C9 C 0.6625(11) 0.2555(11) 0.3119(3) 0.131(5) Uani 1 1 d . . . H9A H 0.6323 0.1814 0.3162 0.157 Uiso 1 1 calc R . . H9B H 0.6926 0.2910 0.3362 0.157 Uiso 1 1 calc R . . C10 C 0.5805(10) 0.2783(10) 0.2992(4) 0.124(4) Uani 1 1 d . . . H10A H 0.5737 0.3255 0.3168 0.149 Uiso 1 1 calc R . . H10B H 0.5137 0.2156 0.2961 0.149 Uiso 1 1 calc R . . C11 C 0.6293(13) 0.3318(9) 0.2585(3) 0.131(5) Uani 1 1 d . . . H11 H 0.5816 0.3375 0.2403 0.157 Uiso 1 1 calc R . . C12 C 0.6801(10) 0.2744(8) 0.2440(3) 0.097(3) Uani 1 1 d . . . C13 C 0.7485(11) 0.3271(10) 0.2071(3) 0.119(4) Uani 1 1 d . . . H13A H 0.7725 0.4003 0.2076 0.179 Uiso 1 1 calc R . . H13B H 0.7077 0.2970 0.1842 0.179 Uiso 1 1 calc R . . H13C H 0.8070 0.3164 0.2071 0.179 Uiso 1 1 calc R . . C14 C 0.5998(13) 0.1582(10) 0.2349(5) 0.154(6) Uani 1 1 d . . . H14A H 0.6215 0.1367 0.2121 0.231 Uiso 1 1 calc R . . H14B H 0.5327 0.1509 0.2304 0.231 Uiso 1 1 calc R . . H14C H 0.5960 0.1156 0.2565 0.231 Uiso 1 1 calc R . . C15 C 0.9601(8) 0.8472(8) 0.3325(3) 0.089(3) Uani 1 1 d . . . C16 C 1.0021(10) 0.9119(8) 0.3007(3) 0.093(3) Uani 1 1 d U . . C17 C 1.0404(8) 0.8832(7) 0.2693(2) 0.083(3) Uani 1 1 d . . . C18 C 1.0881(16) 0.9731(13) 0.2383(4) 0.146(4) Uani 1 1 d D . . C21 C 0.8390(11) 0.8019(11) 0.3882(5) 0.139(5) Uani 1 1 d . . . H21A H 0.8514 0.8180 0.4153 0.209 Uiso 1 1 calc R . . H21B H 0.8409 0.7395 0.3828 0.209 Uiso 1 1 calc R . . H21C H 0.7720 0.7920 0.3813 0.209 Uiso 1 1 calc R . . C22 C 0.9167(11) 0.8849(8) 0.3661(3) 0.124(5) Uani 1 1 d D A . C23 C 1.0231(16) 0.9760(14) 0.3860(4) 0.196(10) Uani 1 1 d D . . H23A H 1.0092 1.0027 0.4096 0.235 Uiso 1 1 calc R . . H23B H 1.0722 0.9527 0.3914 0.235 Uiso 1 1 calc R . . C24 C 1.062(2) 1.0589(13) 0.3517(7) 0.38(3) Uani 1 1 d D . . H24A H 1.1330 1.0807 0.3446 0.455 Uiso 1 1 calc R . . H24B H 1.0572 1.1194 0.3591 0.455 Uiso 1 1 calc R . . C25 C 0.9802(14) 0.9946(10) 0.3152(4) 0.158(5) Uani 1 1 d DU A . H25 H 0.9785 1.0396 0.2948 0.189 Uiso 1 1 calc R . . C26 C 0.8761(13) 0.9422(13) 0.3436(5) 0.153(4) Uani 1 1 d DU . . C27 C 0.7932(13) 0.8884(13) 0.3178(5) 0.153(4) Uani 1 1 d U A . H27A H 0.7599 0.8153 0.3231 0.230 Uiso 1 1 calc R . . H27B H 0.8190 0.9012 0.2916 0.230 Uiso 1 1 calc R . . H27C H 0.7440 0.9118 0.3209 0.230 Uiso 1 1 calc R . . C28 C 0.847(2) 1.018(2) 0.3659(8) 0.247(11) Uiso 0.50 1 d PD A 1 C28' C 0.847(2) 1.018(2) 0.3659(8) 0.247(11) Uiso 0.50 1 d P A 2 C29 C 1.1946(8) 0.6106(8) 0.3191(3) 0.084(2) Uani 1 1 d . . . C30 C 1.2760(9) 0.7148(8) 0.3321(2) 0.086(3) Uani 1 1 d . . . C31 C 1.2534(9) 0.7924(8) 0.3304(3) 0.085(3) Uani 1 1 d . . . C32 C 1.3402(10) 0.9088(9) 0.3369(3) 0.096(3) Uani 1 1 d . . . C33 C 1.3403(10) 0.9472(11) 0.3787(3) 0.110(4) Uani 1 1 d . . . C34 C 1.4248(16) 1.0501(13) 0.3915(6) 0.185(10) Uani 1 1 d . . . C35 C 1.1798(13) 0.4267(10) 0.3212(4) 0.135(5) Uani 1 1 d . . . H35A H 1.1411 0.4087 0.2974 0.202 Uiso 1 1 calc R . . H35B H 1.1328 0.4066 0.3428 0.202 Uiso 1 1 calc R . . H35C H 1.2187 0.3911 0.3226 0.202 Uiso 1 1 calc R . . C36 C 1.2569(11) 0.5478(10) 0.3225(3) 0.110(4) Uani 1 1 d . . . C37 C 1.3350(12) 0.5846(13) 0.2888(4) 0.134(5) Uani 1 1 d . . . H37A H 1.3037 0.5884 0.2646 0.160 Uiso 1 1 calc R . . H37B H 1.3650 0.5402 0.2855 0.160 Uiso 1 1 calc R . . C38 C 1.4220(10) 0.7018(12) 0.3050(4) 0.123(4) Uani 1 1 d . . . H38A H 1.4883 0.7063 0.3101 0.147 Uiso 1 1 calc R . . H38B H 1.4321 0.7556 0.2866 0.147 Uiso 1 1 calc R . . C39 C 1.3720(10) 0.7097(10) 0.3419(4) 0.108(3) Uani 1 1 d . . . H39 H 1.4198 0.7651 0.3594 0.130 Uiso 1 1 calc R . . C40 C 1.3249(9) 0.5992(10) 0.3594(3) 0.106(3) Uani 1 1 d . . . C41 C 1.2556(12) 0.5745(13) 0.3972(3) 0.131(5) Uani 1 1 d . . . H41A H 1.2169 0.5008 0.4013 0.197 Uiso 1 1 calc R . . H41B H 1.2083 0.6004 0.3940 0.197 Uiso 1 1 calc R . . H41C H 1.2994 0.6075 0.4192 0.197 Uiso 1 1 calc R . . C42 C 1.3972(13) 0.5606(13) 0.3699(5) 0.152(5) Uani 1 1 d . . . H42A H 1.4491 0.6084 0.3875 0.228 Uiso 1 1 calc R . . H42B H 1.4303 0.5548 0.3468 0.228 Uiso 1 1 calc R . . H42C H 1.3588 0.4937 0.3820 0.228 Uiso 1 1 calc R . . C45 C 0.7835(8) 0.4945(7) 0.4000(2) 0.082(2) Uani 1 1 d . . . C46 C 0.7362(9) 0.5330(8) 0.3773(2) 0.086(3) Uani 1 1 d . . . H46 H 0.7770 0.5882 0.3608 0.104 Uiso 1 1 calc R . . C47 C 0.6286(10) 0.4938(10) 0.3775(4) 0.108(3) Uani 1 1 d . . . H47 H 0.5993 0.5247 0.3625 0.130 Uiso 1 1 calc R . . C48 C 0.5661(9) 0.4072(12) 0.4007(4) 0.126(5) Uani 1 1 d . . . H48 H 0.4944 0.3793 0.4009 0.151 Uiso 1 1 calc R . . C49 C 0.6094(10) 0.3641(10) 0.4227(4) 0.121(4) Uani 1 1 d . . . H49 H 0.5668 0.3062 0.4377 0.145 Uiso 1 1 calc R . . C50 C 0.7124(9) 0.4025(8) 0.4235(3) 0.096(3) Uani 1 1 d . . . H50 H 0.7398 0.3710 0.4391 0.115 Uiso 1 1 calc R . . C51 C 0.9486(7) 0.4461(6) 0.4163(3) 0.079(2) Uani 1 1 d . . . C52 C 0.9406(11) 0.3788(8) 0.3897(3) 0.101(3) Uani 1 1 d . . . H52 H 0.9205 0.3845 0.3646 0.122 Uiso 1 1 calc R . . C53 C 0.9614(13) 0.2988(9) 0.3983(4) 0.130(5) Uani 1 1 d . . . H53 H 0.9579 0.2526 0.3793 0.156 Uiso 1 1 calc R . . C54 C 0.9878(12) 0.2915(12) 0.4368(5) 0.138(5) Uani 1 1 d . . . H54 H 0.9971 0.2363 0.4438 0.166 Uiso 1 1 calc R . . C55 C 1.0003(13) 0.3637(11) 0.4643(4) 0.128(4) Uani 1 1 d . . . H55 H 1.0231 0.3614 0.4892 0.153 Uiso 1 1 calc R . . C56 C 0.9783(10) 0.4376(9) 0.4538(3) 0.104(3) Uani 1 1 d . . . H56 H 0.9831 0.4851 0.4725 0.125 Uiso 1 1 calc R . . C57 C 0.9732(9) 0.6467(7) 0.4407(4) 0.061(3) Uani 1 1 d . . . C58 C 0.9137(9) 0.6361(8) 0.4723(3) 0.090(3) Uani 1 1 d . . . H58 H 0.8462 0.5808 0.4746 0.108 Uiso 1 1 calc R . . C59 C 0.9601(11) 0.7140(10) 0.5017(3) 0.113(4) Uani 1 1 d . . . H59 H 0.9219 0.7092 0.5237 0.136 Uiso 1 1 calc R . . C60 C 1.0562(11) 0.7930(10) 0.4983(4) 0.113(4) Uani 1 1 d . . . H60 H 1.0875 0.8412 0.5181 0.136 Uiso 1 1 calc R . . C61 C 1.1080(10) 0.8007(10) 0.4641(4) 0.127(4) Uani 1 1 d . . . H61 H 1.1718 0.8605 0.4602 0.152 Uiso 1 1 calc R . . C62 C 1.0724(11) 0.7270(12) 0.4356(4) 0.122(4) Uani 1 1 d . . . H62 H 1.1126 0.7311 0.4143 0.147 Uiso 1 1 calc R . . C63 C 1.0353(11) 0.6751(7) 0.1647(4) 0.074(3) Uani 1 1 d . . . C64 C 1.0853(8) 0.7211(8) 0.1299(3) 0.086(3) Uani 1 1 d . . . H64 H 1.1506 0.7287 0.1259 0.103 Uiso 1 1 calc R . . C65 C 1.0463(10) 0.7568(11) 0.1006(3) 0.112(4) Uani 1 1 d . . . H65 H 1.0855 0.7936 0.0792 0.135 Uiso 1 1 calc R . . C66 C 0.9402(12) 0.7318(11) 0.1063(3) 0.120(4) Uani 1 1 d . . . H66 H 0.9069 0.7472 0.0867 0.144 Uiso 1 1 calc R . . C67 C 0.8893(10) 0.6880(15) 0.1384(4) 0.143(6) Uani 1 1 d . . . H67 H 0.8235 0.6797 0.1417 0.171 Uiso 1 1 calc R . . C68 C 0.9267(10) 0.6554(11) 0.1659(3) 0.107(4) Uani 1 1 d . . . H68 H 0.8845 0.6190 0.1868 0.128 Uiso 1 1 calc R . . C69 C 1.0534(7) 0.4995(6) 0.1866(2) 0.073(2) Uani 1 1 d . . . C70 C 1.0636(11) 0.4401(9) 0.2154(3) 0.102(3) Uani 1 1 d . . . H70 H 1.0808 0.4643 0.2407 0.123 Uiso 1 1 calc R . . C71 C 1.0469(15) 0.3409(10) 0.2046(4) 0.140(5) Uani 1 1 d . . . H71 H 1.0569 0.2998 0.2224 0.168 Uiso 1 1 calc R . . C72 C 1.0145(15) 0.3050(9) 0.1659(5) 0.155(7) Uani 1 1 d . . . H72 H 1.0083 0.2421 0.1583 0.186 Uiso 1 1 calc R . . C73 C 0.9932(15) 0.3573(11) 0.1411(5) 0.152(6) Uani 1 1 d . . . H73 H 0.9592 0.3263 0.1181 0.183 Uiso 1 1 calc R . . C74 C 1.0215(10) 0.4597(8) 0.1490(3) 0.104(3) Uani 1 1 d . . . H74 H 1.0193 0.5018 0.1295 0.125 Uiso 1 1 calc R . . C75 C 1.2222(7) 0.7108(6) 0.2017(2) 0.070(2) Uani 1 1 d . . . C76 C 1.2637(8) 0.7979(7) 0.2261(2) 0.083(2) Uani 1 1 d . . . H76 H 1.2212 0.8132 0.2411 0.100 Uiso 1 1 calc R . . C77 C 1.3717(11) 0.8606(9) 0.2267(3) 0.103(3) Uani 1 1 d . . . H77 H 1.4020 0.9154 0.2443 0.124 Uiso 1 1 calc R . . C78 C 1.4304(10) 0.8444(11) 0.2036(4) 0.113(4) Uani 1 1 d . . . H78 H 1.5002 0.8950 0.2017 0.135 Uiso 1 1 calc R . . C79 C 1.3961(10) 0.7592(13) 0.1825(4) 0.121(4) Uani 1 1 d . . . H79 H 1.4410 0.7435 0.1692 0.145 Uiso 1 1 calc R . . C80 C 1.2809(9) 0.6897(9) 0.1812(3) 0.099(3) Uani 1 1 d . . . H80 H 1.2519 0.6310 0.1654 0.118 Uiso 1 1 calc R . . F1 F 0.5645(13) 0.4897(14) 0.2710(4) 0.257(5) Uani 1 1 d . . . F2 F 0.6721(11) 0.6462(10) 0.2901(3) 0.202(3) Uani 1 1 d . . . F3 F 0.6541(7) 0.5311(7) 0.1993(2) 0.132(2) Uani 1 1 d . . . F4 F 0.7593(6) 0.6946(6) 0.2177(3) 0.143(3) Uani 1 1 d . . . F5 F 0.4888(9) 0.5625(13) 0.2212(4) 0.226(6) Uani 1 1 d . . . F6 F 0.5819(9) 0.6535(11) 0.1774(4) 0.204(5) Uani 1 1 d . . . F7 F 0.5923(12) 0.7191(13) 0.2349(5) 0.226(6) Uani 1 1 d . . . F8 F 1.1669(18) 0.9682(14) 0.2177(6) 0.325(12) Uani 1 1 d . . . F9 F 1.1255(10) 1.0669(7) 0.2581(3) 0.188(4) Uani 1 1 d . . . F15 F 1.3234(12) 0.9782(8) 0.3148(4) 0.225(4) Uani 1 1 d . . . F16 F 1.4337(5) 0.9190(5) 0.33001(19) 0.1144(19) Uani 1 1 d . . . F17 F 1.2429(6) 0.9360(7) 0.3849(3) 0.148(3) Uani 1 1 d . . . F18 F 1.3477(7) 0.8793(6) 0.4037(2) 0.134(2) Uani 1 1 d . . . F19 F 1.5135(8) 1.0742(9) 0.3822(4) 0.198(5) Uani 1 1 d . . . F20 F 1.4134(11) 1.0721(8) 0.4274(3) 0.205(5) Uani 1 1 d . . . F21 F 1.4040(12) 1.1227(7) 0.3687(3) 0.228(7) Uani 1 1 d . . . O1 O 0.8950(6) 0.4702(5) 0.29582(19) 0.0871(18) Uani 1 1 d . . . O2 O 0.8368(5) 0.6228(5) 0.28252(17) 0.0822(16) Uani 1 1 d . . . O3 O 0.9582(5) 0.7614(4) 0.33889(18) 0.0807(16) Uani 1 1 d . . . O4 O 1.0435(5) 0.8045(4) 0.26333(15) 0.0788(16) Uani 1 1 d . . . O5 O 1.1084(5) 0.5774(5) 0.30675(17) 0.0813(16) Uani 1 1 d . . . O6 O 1.1626(5) 0.7827(5) 0.32110(19) 0.0856(16) Uani 1 1 d . . . O11 O 0.9695(5) 0.5926(5) 0.36351(14) 0.0788(16) Uani 1 1 d . . . O22 O 1.0307(5) 0.6232(4) 0.23952(14) 0.0771(15) Uani 1 1 d . . . P1 P 0.92076(18) 0.54819(17) 0.40153(5) 0.0674(5) Uani 1 1 d . . . P2 P 1.07939(18) 0.62711(16) 0.20136(5) 0.0665(5) Uani 1 1 d . . . Yb1 Yb 1.00014(4) 0.65694(3) 0.30142(3) 0.06217(12) Uani 1 1 d . . . C19 C 0.9990(19) 0.9617(12) 0.2148(4) 0.191(10) Uani 1 1 d DU . . F11 F 0.9441(17) 0.9911(17) 0.2385(8) 0.309(9) Uani 1 1 d . . . F10 F 0.9408(11) 0.8623(10) 0.1995(3) 0.202(3) Uani 1 1 d DU . . F13 F 1.0995(11) 1.1271(7) 0.1808(3) 0.225(4) Uani 1 1 d D . . F12 F 1.1351(11) 1.0271(12) 0.1579(4) 0.257(5) Uani 1 1 d D . . C20 C 1.0479(12) 1.0220(10) 0.1730(3) 0.146(4) Uani 1 1 d DU . . F14 F 0.995(2) 1.0093(16) 0.1394(7) 0.57(3) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.114(7) 0.076(5) 0.037(4) -0.002(3) 0.006(4) 0.034(5) C2 0.101(6) 0.069(5) 0.079(6) -0.003(4) -0.018(5) 0.044(5) C3 0.088(7) 0.117(7) 0.040(4) -0.007(4) -0.001(4) 0.049(6) C4 0.101(7) 0.086(6) 0.096(8) -0.002(5) 0.020(6) 0.021(5) C5 0.098(8) 0.144(11) 0.119(10) 0.024(8) 0.029(7) 0.064(8) C6 0.142(13) 0.24(2) 0.126(12) 0.062(13) 0.036(10) 0.135(15) C7 0.160(11) 0.065(6) 0.116(9) -0.008(6) -0.004(8) 0.046(7) C8 0.140(9) 0.067(5) 0.071(6) -0.010(4) -0.004(5) 0.034(6) C9 0.132(10) 0.120(9) 0.068(7) 0.007(6) 0.012(6) 0.008(8) C10 0.101(8) 0.096(8) 0.142(11) 0.023(7) 0.024(8) 0.023(6) C11 0.189(14) 0.090(7) 0.081(7) -0.004(6) -0.032(8) 0.045(8) C12 0.131(8) 0.084(6) 0.057(5) -0.009(4) 0.008(5) 0.040(6) C13 0.155(11) 0.136(9) 0.045(5) -0.022(5) 0.009(6) 0.057(8) C14 0.172(13) 0.107(9) 0.143(12) -0.043(8) 0.028(10) 0.040(9) C15 0.120(7) 0.091(6) 0.077(6) -0.038(5) -0.012(5) 0.069(6) C16 0.138(8) 0.086(6) 0.058(5) 0.000(4) -0.011(5) 0.058(6) C17 0.128(8) 0.070(5) 0.062(5) 0.012(4) -0.012(5) 0.058(5) C18 0.241(13) 0.140(8) 0.109(7) 0.022(6) 0.036(8) 0.134(9) C21 0.126(10) 0.130(10) 0.167(13) 0.048(10) 0.020(9) 0.068(9) C22 0.211(14) 0.094(7) 0.074(6) -0.001(5) 0.041(8) 0.081(9) C23 0.35(3) 0.171(16) 0.087(9) -0.084(10) -0.074(13) 0.145(19) C24 0.29(3) 0.084(12) 0.70(8) -0.15(3) -0.01(4) 0.046(17) C25 0.227(13) 0.089(8) 0.147(13) 0.021(8) 0.005(10) 0.072(9) C26 0.189(10) 0.180(10) 0.174(11) -0.007(8) -0.016(7) 0.155(10) C27 0.189(10) 0.180(10) 0.174(11) -0.007(8) -0.016(7) 0.155(10) C29 0.103(7) 0.111(7) 0.066(5) 0.003(5) -0.001(5) 0.074(6) C30 0.128(8) 0.097(6) 0.053(4) 0.003(4) 0.001(5) 0.070(6) C31 0.103(8) 0.096(6) 0.060(5) -0.001(4) -0.015(5) 0.053(6) C32 0.124(9) 0.099(7) 0.064(5) -0.002(5) -0.005(5) 0.054(6) C33 0.112(8) 0.125(9) 0.078(7) 0.003(6) 0.030(6) 0.047(7) C34 0.167(15) 0.121(12) 0.141(14) -0.023(10) 0.080(12) -0.023(11) C35 0.201(14) 0.120(9) 0.134(10) 0.011(7) 0.005(10) 0.119(11) C36 0.169(11) 0.137(9) 0.081(6) 0.025(6) 0.027(7) 0.119(9) C37 0.176(14) 0.207(16) 0.102(9) 0.032(9) 0.036(8) 0.159(14) C38 0.094(7) 0.140(11) 0.147(11) 0.039(9) 0.031(7) 0.068(8) C39 0.122(9) 0.130(9) 0.095(8) -0.014(7) -0.017(6) 0.080(8) C40 0.112(8) 0.138(9) 0.084(7) 0.014(6) -0.003(6) 0.076(7) C41 0.166(12) 0.191(14) 0.079(7) 0.023(8) 0.018(7) 0.121(12) C42 0.173(14) 0.165(13) 0.166(14) -0.001(10) -0.019(11) 0.120(12) C45 0.102(6) 0.087(5) 0.055(5) -0.010(4) 0.002(4) 0.046(5) C46 0.109(8) 0.106(7) 0.059(5) 0.011(5) 0.011(5) 0.065(6) C47 0.099(8) 0.132(9) 0.106(8) -0.004(7) 0.001(7) 0.067(8) C48 0.082(7) 0.159(11) 0.094(8) -0.024(8) 0.014(6) 0.029(8) C49 0.102(9) 0.112(8) 0.094(8) 0.010(6) -0.017(7) 0.014(7) C50 0.112(8) 0.096(6) 0.074(6) 0.020(5) 0.021(5) 0.046(6) C51 0.094(6) 0.070(5) 0.072(5) 0.001(4) 0.003(4) 0.040(4) C52 0.173(11) 0.097(7) 0.061(5) 0.006(5) 0.002(6) 0.088(8) C53 0.208(15) 0.089(7) 0.111(10) 0.002(6) 0.000(9) 0.088(9) C54 0.164(12) 0.135(11) 0.145(13) 0.049(10) -0.012(10) 0.097(10) C55 0.198(14) 0.131(10) 0.086(8) 0.021(7) -0.002(8) 0.105(10) C56 0.149(9) 0.113(8) 0.079(6) 0.003(5) -0.012(6) 0.087(7) C57 0.080(6) 0.052(4) 0.053(6) -0.004(3) 0.001(4) 0.035(4) C58 0.093(7) 0.098(6) 0.062(5) -0.009(5) 0.007(5) 0.035(5) C59 0.148(10) 0.123(9) 0.071(6) -0.017(6) 0.029(6) 0.070(9) C60 0.134(10) 0.098(9) 0.087(8) -0.033(6) -0.012(7) 0.043(8) C61 0.113(9) 0.102(8) 0.108(9) -0.021(7) 0.007(7) 0.010(6) C62 0.118(9) 0.136(10) 0.087(8) -0.030(7) 0.014(7) 0.043(9) C63 0.082(7) 0.089(7) 0.053(6) -0.018(4) -0.003(6) 0.045(6) C64 0.085(7) 0.106(7) 0.070(6) 0.019(5) 0.008(5) 0.050(6) C65 0.123(9) 0.134(11) 0.083(7) 0.020(7) 0.000(6) 0.068(8) C66 0.168(12) 0.149(11) 0.072(7) 0.005(7) -0.011(7) 0.101(10) C67 0.114(9) 0.28(2) 0.084(8) 0.005(9) -0.004(7) 0.134(12) C68 0.106(8) 0.145(11) 0.078(7) 0.039(6) 0.030(6) 0.069(8) C69 0.096(5) 0.073(5) 0.060(4) -0.013(4) 0.001(4) 0.050(4) C70 0.159(11) 0.102(7) 0.069(6) -0.004(5) -0.005(6) 0.083(8) C71 0.244(18) 0.112(9) 0.106(10) 0.006(7) -0.001(10) 0.121(11) C72 0.227(17) 0.073(7) 0.149(14) -0.015(8) 0.053(12) 0.064(9) C73 0.27(2) 0.111(9) 0.112(10) -0.041(8) -0.044(11) 0.118(12) C74 0.177(11) 0.108(7) 0.049(5) -0.004(4) -0.008(5) 0.087(7) C75 0.097(6) 0.082(5) 0.040(4) -0.004(3) -0.009(4) 0.051(4) C76 0.093(7) 0.089(6) 0.056(5) 0.000(4) -0.003(4) 0.036(5) C77 0.116(9) 0.101(7) 0.066(6) -0.005(5) -0.008(6) 0.034(7) C78 0.096(8) 0.111(8) 0.091(8) 0.029(7) -0.011(6) 0.022(7) C79 0.094(8) 0.157(12) 0.126(10) 0.022(9) 0.013(7) 0.074(8) C80 0.102(7) 0.117(8) 0.085(7) -0.002(6) -0.014(5) 0.061(6) F1 0.289(11) 0.320(12) 0.253(10) 0.138(9) 0.151(9) 0.220(10) F2 0.266(9) 0.226(8) 0.119(5) -0.028(5) -0.018(5) 0.127(7) F3 0.172(7) 0.176(7) 0.083(4) -0.013(4) -0.003(4) 0.112(6) F4 0.127(5) 0.147(6) 0.163(7) 0.076(5) 0.050(5) 0.074(5) F5 0.130(7) 0.339(17) 0.244(13) 0.098(12) 0.035(8) 0.143(10) F6 0.191(9) 0.296(14) 0.192(11) 0.105(10) 0.046(8) 0.173(10) F7 0.260(15) 0.298(17) 0.238(14) -0.022(11) -0.022(10) 0.227(15) F8 0.43(3) 0.285(18) 0.34(2) 0.139(17) 0.23(2) 0.24(2) F9 0.240(11) 0.127(7) 0.186(9) 0.045(6) -0.014(8) 0.083(7) F15 0.315(11) 0.127(5) 0.179(7) 0.056(5) 0.044(7) 0.069(6) F16 0.086(4) 0.139(5) 0.099(4) -0.005(4) 0.022(3) 0.042(3) F17 0.132(6) 0.154(7) 0.134(6) -0.023(5) 0.035(5) 0.053(5) F18 0.172(7) 0.118(5) 0.096(5) 0.004(4) 0.000(4) 0.060(5) F19 0.132(7) 0.194(10) 0.187(10) -0.032(8) 0.027(7) 0.022(7) F20 0.260(13) 0.151(8) 0.144(8) -0.031(6) 0.022(8) 0.058(8) F21 0.335(19) 0.097(6) 0.153(9) 0.007(6) 0.053(9) 0.034(8) O1 0.121(5) 0.057(4) 0.081(4) 0.006(3) 0.001(4) 0.042(4) O2 0.104(5) 0.081(4) 0.066(4) -0.004(3) -0.007(3) 0.051(4) O3 0.123(5) 0.067(3) 0.073(4) -0.008(3) -0.008(3) 0.063(3) O4 0.133(5) 0.064(3) 0.048(3) 0.001(2) -0.008(3) 0.056(3) O5 0.115(5) 0.094(4) 0.065(3) -0.003(3) -0.011(3) 0.075(4) O6 0.106(5) 0.075(4) 0.082(4) -0.002(3) -0.018(3) 0.050(3) O11 0.122(5) 0.091(4) 0.044(3) 0.013(3) 0.003(3) 0.069(4) O22 0.117(4) 0.077(3) 0.047(3) -0.005(2) 0.006(3) 0.056(3) P1 0.0937(14) 0.0726(12) 0.0423(10) 0.0062(8) 0.0031(9) 0.0462(11) P2 0.0928(14) 0.0715(11) 0.0429(10) -0.0030(8) 0.0025(9) 0.0468(11) Yb1 0.0930(2) 0.0632(2) 0.04091(15) 0.00011(18) 0.00071(10) 0.04698(18) C19 0.39(3) 0.159(10) 0.071(7) 0.001(7) -0.066(10) 0.174(16) F11 0.33(2) 0.31(2) 0.34(3) 0.015(19) -0.02(2) 0.20(2) F10 0.266(9) 0.226(8) 0.119(5) -0.028(5) -0.018(5) 0.127(7) F13 0.315(11) 0.127(5) 0.179(7) 0.056(5) 0.044(7) 0.069(6) F12 0.289(11) 0.320(12) 0.253(10) 0.138(9) 0.151(9) 0.220(10) C20 0.241(13) 0.140(8) 0.109(7) 0.022(6) 0.036(8) 0.134(9) F14 0.68(6) 0.37(3) 0.56(5) 0.17(3) -0.31(4) 0.20(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.261(11) . ? C1 C2 1.429(13) . ? C1 C8 1.559(13) . ? C2 C3 1.371(13) . ? C2 C11 1.624(15) . ? C3 O2 1.288(11) . ? C3 C4 1.638(17) . ? C4 F1 1.330(18) . ? C4 F2 1.420(15) . ? C4 C5 1.451(19) . ? C5 F3 1.330(16) . ? C5 F4 1.429(15) . ? C5 C6 1.55(2) . ? C6 F7 1.23(2) . ? C6 F6 1.318(19) . ? C6 F5 1.37(2) . ? C7 C8 1.501(17) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C12 1.554(16) . ? C8 C9 1.551(17) . ? C9 C10 1.49(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.597(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.48(2) . ? C11 H11 0.9800 . ? C12 C14 1.563(16) . ? C12 C13 1.568(15) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O3 1.280(11) . ? C15 C16 1.382(14) . ? C15 C22 1.561(13) . ? C16 C17 1.385(14) . ? C16 C25 1.505(18) . ? C17 O4 1.212(10) . ? C17 C18 1.574(16) . ? C18 F9 1.393(17) . ? C18 F8 1.40(2) . ? C18 C19 1.49(3) . ? C21 C22 1.416(17) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C26 1.484(18) . ? C22 C23 1.631(16) . ? C23 C24 1.589(18) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.676(18) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.660(16) . ? C25 H25 0.9800 . ? C26 C27 1.40(2) . ? C26 C28 1.592(17) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C29 O5 1.198(11) . ? C29 C30 1.478(15) . ? C29 C36 1.615(13) . ? C30 C31 1.356(13) . ? C30 C39 1.504(15) . ? C31 O6 1.322(12) . ? C31 C32 1.573(15) . ? C32 F16 1.341(13) . ? C32 F15 1.400(15) . ? C32 C33 1.547(15) . ? C33 F18 1.372(15) . ? C33 F17 1.387(14) . ? C33 C34 1.48(2) . ? C34 F19 1.22(2) . ? C34 F20 1.308(17) . ? C34 F21 1.49(3) . ? C35 C36 1.578(18) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.534(16) . ? C36 C40 1.566(18) . ? C37 C38 1.66(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.508(18) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.550(18) . ? C39 H39 0.9800 . ? C40 C42 1.494(16) . ? C40 C41 1.585(16) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C45 C46 1.354(13) . ? C45 C50 1.483(13) . ? C45 P1 1.781(10) . ? C46 C47 1.401(15) . ? C46 H46 0.9300 . ? C47 C48 1.402(18) . ? C47 H47 0.9300 . ? C48 C49 1.345(19) . ? C48 H48 0.9300 . ? C49 C50 1.340(16) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.315(13) . ? C51 C56 1.392(13) . ? C51 P1 1.834(9) . ? C52 C53 1.403(15) . ? C52 H52 0.9300 . ? C53 C54 1.40(2) . ? C53 H53 0.9300 . ? C54 C55 1.37(2) . ? C54 H54 0.9300 . ? C55 C56 1.342(15) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.359(15) . ? C57 C62 1.367(18) . ? C57 P1 1.853(11) . ? C58 C59 1.429(15) . ? C58 H58 0.9300 . ? C59 C60 1.325(16) . ? C59 H59 0.9300 . ? C60 C61 1.378(18) . ? C60 H60 0.9300 . ? C61 C62 1.365(17) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C64 1.394(16) . ? C63 C68 1.490(19) . ? C63 P2 1.733(13) . ? C64 C65 1.393(14) . ? C64 H64 0.9300 . ? C65 C66 1.441(18) . ? C65 H65 0.9300 . ? C66 C67 1.314(18) . ? C66 H66 0.9300 . ? C67 C68 1.308(16) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C70 1.386(13) . ? C69 C74 1.402(12) . ? C69 P2 1.809(8) . ? C70 C71 1.416(15) . ? C70 H70 0.9300 . ? C71 C72 1.42(2) . ? C71 H71 0.9300 . ? C72 C73 1.30(2) . ? C72 H72 0.9300 . ? C73 C74 1.389(16) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 C80 1.279(14) . ? C75 C76 1.399(12) . ? C75 P2 1.848(9) . ? C76 C77 1.396(15) . ? C76 H76 0.9300 . ? C77 C78 1.290(18) . ? C77 H77 0.9300 . ? C78 C79 1.322(19) . ? C78 H78 0.9300 . ? C79 C80 1.493(17) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? O1 Yb1 2.418(6) . ? O2 Yb1 2.311(7) . ? O3 Yb1 2.330(5) . ? O4 Yb1 2.352(5) . ? O5 Yb1 2.433(6) . ? O6 Yb1 2.295(6) . ? O11 P1 1.482(6) . ? O11 Yb1 2.293(5) . ? O22 P2 1.487(5) . ? O22 Yb1 2.287(5) . ? C19 F11 1.37(3) . ? C19 F10 1.389(15) . ? C19 C20 1.659(15) . ? F13 C20 1.378(13) . ? F12 C20 1.363(14) . ? C20 F14 1.359(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 128.5(8) . . ? O1 C1 C8 124.8(9) . . ? C2 C1 C8 106.2(9) . . ? C3 C2 C1 121.8(9) . . ? C3 C2 C11 134.3(10) . . ? C1 C2 C11 103.9(8) . . ? O2 C3 C2 127.2(9) . . ? O2 C3 C4 113.0(9) . . ? C2 C3 C4 119.6(9) . . ? F1 C4 F2 103.7(12) . . ? F1 C4 C5 109.7(13) . . ? F2 C4 C5 110.7(11) . . ? F1 C4 C3 111.5(11) . . ? F2 C4 C3 104.0(10) . . ? C5 C4 C3 116.4(9) . . ? F3 C5 F4 107.5(10) . . ? F3 C5 C4 108.0(12) . . ? F4 C5 C4 107.1(11) . . ? F3 C5 C6 116.7(15) . . ? F4 C5 C6 101.5(12) . . ? C4 C5 C6 115.3(11) . . ? F7 C6 F6 117.0(18) . . ? F7 C6 F5 107.6(14) . . ? F6 C6 F5 98.5(18) . . ? F7 C6 C5 120.2(18) . . ? F6 C6 C5 106.2(13) . . ? F5 C6 C5 104.3(15) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 C12 121.0(9) . . ? C7 C8 C9 118.3(11) . . ? C12 C8 C9 98.6(10) . . ? C7 C8 C1 112.8(10) . . ? C12 C8 C1 99.2(8) . . ? C9 C8 C1 103.9(9) . . ? C10 C9 C8 110.0(11) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C11 98.7(11) . . ? C9 C10 H10A 112.0 . . ? C11 C10 H10A 112.0 . . ? C9 C10 H10B 112.0 . . ? C11 C10 H10B 112.0 . . ? H10A C10 H10B 109.7 . . ? C12 C11 C10 104.2(10) . . ? C12 C11 C2 101.4(12) . . ? C10 C11 C2 102.0(9) . . ? C12 C11 H11 115.7 . . ? C10 C11 H11 115.7 . . ? C2 C11 H11 115.7 . . ? C11 C12 C8 96.3(8) . . ? C11 C12 C14 112.2(11) . . ? C8 C12 C14 114.9(10) . . ? C11 C12 C13 112.0(10) . . ? C8 C12 C13 111.4(10) . . ? C14 C12 C13 109.6(9) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 127.4(8) . . ? O3 C15 C22 115.0(9) . . ? C16 C15 C22 117.5(8) . . ? C15 C16 C17 121.1(8) . . ? C15 C16 C25 95.7(9) . . ? C17 C16 C25 143.1(9) . . ? O4 C17 C16 130.5(8) . . ? O4 C17 C18 119.0(9) . . ? C16 C17 C18 110.4(8) . . ? F9 C18 F8 112.0(19) . . ? F9 C18 C19 105.4(12) . . ? F8 C18 C19 116.0(16) . . ? F9 C18 C17 107.6(10) . . ? F8 C18 C17 109.5(11) . . ? C19 C18 C17 105.9(14) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 C22 C26 113.0(14) . . ? C21 C22 C15 112.9(11) . . ? C26 C22 C15 100.3(9) . . ? C21 C22 C23 122.0(13) . . ? C26 C22 C23 104.2(12) . . ? C15 C22 C23 101.9(10) . . ? C24 C23 C22 99.1(12) . . ? C24 C23 H23A 111.9 . . ? C22 C23 H23A 111.9 . . ? C24 C23 H23B 112.0 . . ? C22 C23 H23B 112.0 . . ? H23A C23 H23B 109.6 . . ? C23 C24 C25 103.7(12) . . ? C23 C24 H24A 111.0 . . ? C25 C24 H24A 111.0 . . ? C23 C24 H24B 111.0 . . ? C25 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? C16 C25 C26 110.1(10) . . ? C16 C25 C24 108.9(14) . . ? C26 C25 C24 93.7(15) . . ? C16 C25 H25 114.1 . . ? C26 C25 H25 114.1 . . ? C24 C25 H25 114.1 . . ? C27 C26 C22 119.8(14) . . ? C27 C26 C28 103.9(14) . . ? C22 C26 C28 119.1(16) . . ? C27 C26 C25 103.9(15) . . ? C22 C26 C25 91.5(9) . . ? C28 C26 C25 117.9(17) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O5 C29 C30 133.3(9) . . ? O5 C29 C36 126.3(10) . . ? C30 C29 C36 100.3(9) . . ? C31 C30 C29 117.2(9) . . ? C31 C30 C39 134.2(11) . . ? C29 C30 C39 108.4(8) . . ? O6 C31 C30 126.3(10) . . ? O6 C31 C32 112.7(8) . . ? C30 C31 C32 120.9(10) . . ? F16 C32 F15 112.1(10) . . ? F16 C32 C33 108.3(9) . . ? F15 C32 C33 101.6(10) . . ? F16 C32 C31 109.5(9) . . ? F15 C32 C31 112.4(10) . . ? C33 C32 C31 112.8(9) . . ? F18 C33 F17 106.1(9) . . ? F18 C33 C34 103.5(15) . . ? F17 C33 C34 111.9(14) . . ? F18 C33 C32 107.3(10) . . ? F17 C33 C32 106.9(10) . . ? C34 C33 C32 120.2(10) . . ? F19 C34 F20 115(2) . . ? F19 C34 C33 117.2(17) . . ? F20 C34 C33 113.0(11) . . ? F19 C34 F21 103.5(13) . . ? F20 C34 F21 102.6(18) . . ? C33 C34 F21 102.4(19) . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C40 104.5(12) . . ? C37 C36 C35 111.9(11) . . ? C40 C36 C35 120.2(9) . . ? C37 C36 C29 106.8(8) . . ? C40 C36 C29 101.1(8) . . ? C35 C36 C29 111.0(11) . . ? C36 C37 C38 100.0(10) . . ? C36 C37 H37A 111.8 . . ? C38 C37 H37A 111.8 . . ? C36 C37 H37B 111.8 . . ? C38 C37 H37B 111.8 . . ? H37A C37 H37B 109.5 . . ? C39 C38 C37 102.0(10) . . ? C39 C38 H38A 111.4 . . ? C37 C38 H38A 111.4 . . ? C39 C38 H38B 111.4 . . ? C37 C38 H38B 111.4 . . ? H38A C38 H38B 109.2 . . ? C30 C39 C38 109.3(10) . . ? C30 C39 C40 101.8(10) . . ? C38 C39 C40 102.9(10) . . ? C30 C39 H39 113.9 . . ? C38 C39 H39 113.9 . . ? C40 C39 H39 113.9 . . ? C42 C40 C39 118.1(12) . . ? C42 C40 C36 114.9(11) . . ? C39 C40 C36 92.3(8) . . ? C42 C40 C41 102.9(11) . . ? C39 C40 C41 117.4(10) . . ? C36 C40 C41 111.6(11) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C46 C45 C50 115.0(10) . . ? C46 C45 P1 123.3(8) . . ? C50 C45 P1 121.7(8) . . ? C45 C46 C47 123.3(10) . . ? C45 C46 H46 118.4 . . ? C47 C46 H46 118.4 . . ? C46 C47 C48 118.6(12) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C49 C48 C47 120.2(12) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C50 C49 C48 121.7(12) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C49 C50 C45 121.2(11) . . ? C49 C50 H50 119.4 . . ? C45 C50 H50 119.4 . . ? C52 C51 C56 119.3(9) . . ? C52 C51 P1 117.6(7) . . ? C56 C51 P1 123.0(7) . . ? C51 C52 C53 121.5(10) . . ? C51 C52 H52 119.3 . . ? C53 C52 H52 119.3 . . ? C54 C53 C52 117.0(12) . . ? C54 C53 H53 121.5 . . ? C52 C53 H53 121.5 . . ? C55 C54 C53 121.8(11) . . ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C56 C55 C54 117.5(12) . . ? C56 C55 H55 121.3 . . ? C54 C55 H55 121.3 . . ? C55 C56 C51 122.7(11) . . ? C55 C56 H56 118.6 . . ? C51 C56 H56 118.6 . . ? C58 C57 C62 124.0(10) . . ? C58 C57 P1 119.9(8) . . ? C62 C57 P1 116.1(8) . . ? C57 C58 C59 116.7(10) . . ? C57 C58 H58 121.6 . . ? C59 C58 H58 121.6 . . ? C60 C59 C58 121.7(10) . . ? C60 C59 H59 119.1 . . ? C58 C59 H59 119.2 . . ? C59 C60 C61 117.3(10) . . ? C59 C60 H60 121.4 . . ? C61 C60 H60 121.4 . . ? C62 C61 C60 124.8(12) . . ? C62 C61 H61 117.6 . . ? C60 C61 H61 117.6 . . ? C61 C62 C57 115.1(11) . . ? C61 C62 H62 122.5 . . ? C57 C62 H62 122.5 . . ? C64 C63 C68 112.4(10) . . ? C64 C63 P2 127.6(10) . . ? C68 C63 P2 119.5(8) . . ? C65 C64 C63 125.9(11) . . ? C65 C64 H64 117.0 . . ? C63 C64 H64 117.0 . . ? C64 C65 C66 114.5(10) . . ? C64 C65 H65 122.8 . . ? C66 C65 H65 122.8 . . ? C67 C66 C65 121.7(11) . . ? C67 C66 H66 119.2 . . ? C65 C66 H66 119.2 . . ? C68 C67 C66 123.2(12) . . ? C68 C67 H67 118.4 . . ? C66 C67 H67 118.4 . . ? C67 C68 C63 121.7(10) . . ? C67 C68 H68 119.2 . . ? C63 C68 H68 119.2 . . ? C70 C69 C74 120.8(8) . . ? C70 C69 P2 115.6(6) . . ? C74 C69 P2 123.5(7) . . ? C69 C70 C71 117.2(10) . . ? C69 C70 H70 121.4 . . ? C71 C70 H70 121.4 . . ? C70 C71 C72 119.0(12) . . ? C70 C71 H71 120.5 . . ? C72 C71 H71 120.5 . . ? C73 C72 C71 122.0(11) . . ? C73 C72 H72 119.0 . . ? C71 C72 H72 119.0 . . ? C72 C73 C74 119.8(13) . . ? C72 C73 H73 120.1 . . ? C74 C73 H73 120.1 . . ? C73 C74 C69 119.8(10) . . ? C73 C74 H74 120.1 . . ? C69 C74 H74 120.1 . . ? C80 C75 C76 121.3(10) . . ? C80 C75 P2 121.8(8) . . ? C76 C75 P2 117.0(7) . . ? C77 C76 C75 117.1(10) . . ? C77 C76 H76 121.5 . . ? C75 C76 H76 121.5 . . ? C78 C77 C76 121.6(11) . . ? C78 C77 H77 119.2 . . ? C76 C77 H77 119.2 . . ? C77 C78 C79 123.0(12) . . ? C77 C78 H78 118.5 . . ? C79 C78 H78 118.5 . . ? C78 C79 C80 116.1(12) . . ? C78 C79 H79 122.0 . . ? C80 C79 H79 122.0 . . ? C75 C80 C79 120.0(12) . . ? C75 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C1 O1 Yb1 131.5(6) . . ? C3 O2 Yb1 136.4(6) . . ? C15 O3 Yb1 133.5(6) . . ? C17 O4 Yb1 132.9(6) . . ? C29 O5 Yb1 131.1(6) . . ? C31 O6 Yb1 139.5(6) . . ? P1 O11 Yb1 163.8(4) . . ? P2 O22 Yb1 164.0(4) . . ? O11 P1 C45 111.6(4) . . ? O11 P1 C51 110.5(4) . . ? C45 P1 C51 108.7(4) . . ? O11 P1 C57 111.9(5) . . ? C45 P1 C57 108.1(4) . . ? C51 P1 C57 105.8(4) . . ? O22 P2 C63 112.6(5) . . ? O22 P2 C69 111.3(4) . . ? C63 P2 C69 107.5(4) . . ? O22 P2 C75 113.1(4) . . ? C63 P2 C75 105.7(5) . . ? C69 P2 C75 106.2(4) . . ? O22 Yb1 O11 142.89(17) . . ? O22 Yb1 O6 102.1(2) . . ? O11 Yb1 O6 88.5(2) . . ? O22 Yb1 O2 89.5(2) . . ? O11 Yb1 O2 101.7(2) . . ? O6 Yb1 O2 145.4(2) . . ? O22 Yb1 O3 144.2(2) . . ? O11 Yb1 O3 72.4(2) . . ? O6 Yb1 O3 79.4(2) . . ? O2 Yb1 O3 72.6(2) . . ? O22 Yb1 O4 72.11(19) . . ? O11 Yb1 O4 144.5(2) . . ? O6 Yb1 O4 73.7(2) . . ? O2 Yb1 O4 79.4(2) . . ? O3 Yb1 O4 74.18(19) . . ? O22 Yb1 O1 76.1(2) . . ? O11 Yb1 O1 73.5(2) . . ? O6 Yb1 O1 140.5(2) . . ? O2 Yb1 O1 73.8(2) . . ? O3 Yb1 O1 125.1(2) . . ? O4 Yb1 O1 138.1(2) . . ? O22 Yb1 O5 73.2(2) . . ? O11 Yb1 O5 76.6(2) . . ? O6 Yb1 O5 72.0(2) . . ? O2 Yb1 O5 142.3(2) . . ? O3 Yb1 O5 138.1(2) . . ? O4 Yb1 O5 123.8(2) . . ? O1 Yb1 O5 69.7(2) . . ? F11 C19 F10 114(2) . . ? F11 C19 C18 106.2(14) . . ? F10 C19 C18 111.8(14) . . ? F11 C19 C20 121.0(15) . . ? F10 C19 C20 96.7(11) . . ? C18 C19 C20 106.5(16) . . ? F14 C20 F12 98.7(14) . . ? F14 C20 F13 106.1(11) . . ? F12 C20 F13 92.0(11) . . ? F14 C20 C19 126.7(17) . . ? F12 C20 C19 120.6(13) . . ? F13 C20 C19 106.8(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 1.3(15) . . . . ? C8 C1 C2 C3 173.8(9) . . . . ? O1 C1 C2 C11 -178.6(9) . . . . ? C8 C1 C2 C11 -6.1(10) . . . . ? C1 C2 C3 O2 6.4(15) . . . . ? C11 C2 C3 O2 -173.7(10) . . . . ? C1 C2 C3 C4 -177.8(8) . . . . ? C11 C2 C3 C4 2.0(16) . . . . ? O2 C3 C4 F1 -152.3(11) . . . . ? C2 C3 C4 F1 31.3(15) . . . . ? O2 C3 C4 F2 -41.2(11) . . . . ? C2 C3 C4 F2 142.4(10) . . . . ? O2 C3 C4 C5 80.8(12) . . . . ? C2 C3 C4 C5 -95.5(12) . . . . ? F1 C4 C5 F3 -70.3(14) . . . . ? F2 C4 C5 F3 175.9(11) . . . . ? C3 C4 C5 F3 57.4(13) . . . . ? F1 C4 C5 F4 174.3(11) . . . . ? F2 C4 C5 F4 60.5(14) . . . . ? C3 C4 C5 F4 -58.0(14) . . . . ? F1 C4 C5 C6 62.2(18) . . . . ? F2 C4 C5 C6 -51.6(18) . . . . ? C3 C4 C5 C6 -170.1(14) . . . . ? F3 C5 C6 F7 -174.7(16) . . . . ? F4 C5 C6 F7 -58(2) . . . . ? C4 C5 C6 F7 57(2) . . . . ? F3 C5 C6 F6 -39(2) . . . . ? F4 C5 C6 F6 77.6(18) . . . . ? C4 C5 C6 F6 -167.2(15) . . . . ? F3 C5 C6 F5 64.6(17) . . . . ? F4 C5 C6 F5 -179.0(14) . . . . ? C4 C5 C6 F5 -64(2) . . . . ? O1 C1 C8 C7 -20.1(13) . . . . ? C2 C1 C8 C7 167.1(9) . . . . ? O1 C1 C8 C12 -149.5(9) . . . . ? C2 C1 C8 C12 37.7(10) . . . . ? O1 C1 C8 C9 109.2(11) . . . . ? C2 C1 C8 C9 -63.7(10) . . . . ? C7 C8 C9 C10 -163.6(11) . . . . ? C12 C8 C9 C10 -31.3(12) . . . . ? C1 C8 C9 C10 70.5(12) . . . . ? C8 C9 C10 C11 -0.8(13) . . . . ? C9 C10 C11 C12 35.2(13) . . . . ? C9 C10 C11 C2 -69.9(12) . . . . ? C3 C2 C11 C12 150.8(11) . . . . ? C1 C2 C11 C12 -29.3(10) . . . . ? C3 C2 C11 C10 -101.9(13) . . . . ? C1 C2 C11 C10 78.0(12) . . . . ? C10 C11 C12 C8 -54.7(11) . . . . ? C2 C11 C12 C8 51.0(9) . . . . ? C10 C11 C12 C14 65.5(13) . . . . ? C2 C11 C12 C14 171.2(10) . . . . ? C10 C11 C12 C13 -170.8(10) . . . . ? C2 C11 C12 C13 -65.1(11) . . . . ? C7 C8 C12 C11 -178.5(10) . . . . ? C9 C8 C12 C11 51.0(10) . . . . ? C1 C8 C12 C11 -54.8(10) . . . . ? C7 C8 C12 C14 63.5(14) . . . . ? C9 C8 C12 C14 -67.1(12) . . . . ? C1 C8 C12 C14 -172.8(10) . . . . ? C7 C8 C12 C13 -61.9(13) . . . . ? C9 C8 C12 C13 167.5(10) . . . . ? C1 C8 C12 C13 61.8(11) . . . . ? O3 C15 C16 C17 6.1(18) . . . . ? C22 C15 C16 C17 -178.7(10) . . . . ? O3 C15 C16 C25 -176.9(12) . . . . ? C22 C15 C16 C25 -1.7(14) . . . . ? C15 C16 C17 O4 1.2(19) . . . . ? C25 C16 C17 O4 -173.8(17) . . . . ? C15 C16 C17 C18 -177.3(12) . . . . ? C25 C16 C17 C18 8(2) . . . . ? O4 C17 C18 F9 -149.0(11) . . . . ? C16 C17 C18 F9 29.7(17) . . . . ? O4 C17 C18 F8 -27(2) . . . . ? C16 C17 C18 F8 151.6(16) . . . . ? O4 C17 C18 C19 98.7(14) . . . . ? C16 C17 C18 C19 -82.6(13) . . . . ? O3 C15 C22 C21 -29.6(16) . . . . ? C16 C15 C22 C21 154.6(12) . . . . ? O3 C15 C22 C26 -150.1(11) . . . . ? C16 C15 C22 C26 34.1(15) . . . . ? O3 C15 C22 C23 102.9(12) . . . . ? C16 C15 C22 C23 -72.9(14) . . . . ? C21 C22 C23 C24 -165.1(16) . . . . ? C26 C22 C23 C24 -35.8(17) . . . . ? C15 C22 C23 C24 68.1(17) . . . . ? C22 C23 C24 C25 -8(2) . . . . ? C15 C16 C25 C26 -28.9(14) . . . . ? C17 C16 C25 C26 146.8(17) . . . . ? C15 C16 C25 C24 72.5(15) . . . . ? C17 C16 C25 C24 -112(2) . . . . ? C23 C24 C25 C16 -70(2) . . . . ? C23 C24 C25 C26 43.1(19) . . . . ? C21 C22 C26 C27 -55.5(19) . . . . ? C15 C22 C26 C27 64.9(17) . . . . ? C23 C22 C26 C27 170.0(15) . . . . ? C21 C22 C26 C28 74(2) . . . . ? C15 C22 C26 C28 -165.5(17) . . . . ? C23 C22 C26 C28 -60(2) . . . . ? C21 C22 C26 C25 -162.4(12) . . . . ? C15 C22 C26 C25 -42.1(12) . . . . ? C23 C22 C26 C25 63.1(12) . . . . ? C16 C25 C26 C27 -72.6(14) . . . . ? C24 C25 C26 C27 175.7(12) . . . . ? C16 C25 C26 C22 48.6(14) . . . . ? C24 C25 C26 C22 -63.0(13) . . . . ? C16 C25 C26 C28 173.1(16) . . . . ? C24 C25 C26 C28 61.4(19) . . . . ? O5 C29 C30 C31 0.0(16) . . . . ? C36 C29 C30 C31 175.3(8) . . . . ? O5 C29 C30 C39 -175.9(10) . . . . ? C36 C29 C30 C39 -0.6(10) . . . . ? C29 C30 C31 O6 5.7(14) . . . . ? C39 C30 C31 O6 -179.7(10) . . . . ? C29 C30 C31 C32 -169.9(8) . . . . ? C39 C30 C31 C32 4.7(16) . . . . ? O6 C31 C32 F16 -154.3(8) . . . . ? C30 C31 C32 F16 21.9(12) . . . . ? O6 C31 C32 F15 -29.0(13) . . . . ? C30 C31 C32 F15 147.1(10) . . . . ? O6 C31 C32 C33 85.1(11) . . . . ? C30 C31 C32 C33 -98.7(12) . . . . ? F16 C32 C33 F18 -66.7(12) . . . . ? F15 C32 C33 F18 175.1(11) . . . . ? C31 C32 C33 F18 54.6(13) . . . . ? F16 C32 C33 F17 179.8(9) . . . . ? F15 C32 C33 F17 61.6(13) . . . . ? C31 C32 C33 F17 -58.9(13) . . . . ? F16 C32 C33 C34 51(2) . . . . ? F15 C32 C33 C34 -67(2) . . . . ? C31 C32 C33 C34 172.2(17) . . . . ? F18 C33 C34 F19 77(2) . . . . ? F17 C33 C34 F19 -169.4(19) . . . . ? C32 C33 C34 F19 -43(3) . . . . ? F18 C33 C34 F20 -61(2) . . . . ? F17 C33 C34 F20 53(3) . . . . ? C32 C33 C34 F20 179.2(17) . . . . ? F18 C33 C34 F21 -170.8(11) . . . . ? F17 C33 C34 F21 -57.0(14) . . . . ? C32 C33 C34 F21 69.6(19) . . . . ? O5 C29 C36 C37 102.7(14) . . . . ? C30 C29 C36 C37 -73.1(12) . . . . ? O5 C29 C36 C40 -148.2(10) . . . . ? C30 C29 C36 C40 36.0(10) . . . . ? O5 C29 C36 C35 -19.6(14) . . . . ? C30 C29 C36 C35 164.6(9) . . . . ? C40 C36 C37 C38 -32.8(10) . . . . ? C35 C36 C37 C38 -164.4(10) . . . . ? C29 C36 C37 C38 73.9(12) . . . . ? C36 C37 C38 C39 -4.1(11) . . . . ? C31 C30 C39 C38 -102.1(13) . . . . ? C29 C30 C39 C38 72.9(12) . . . . ? C31 C30 C39 C40 149.6(11) . . . . ? C29 C30 C39 C40 -35.5(11) . . . . ? C37 C38 C39 C30 -67.5(12) . . . . ? C37 C38 C39 C40 40.1(11) . . . . ? C30 C39 C40 C42 174.7(11) . . . . ? C38 C39 C40 C42 61.5(14) . . . . ? C30 C39 C40 C36 54.8(9) . . . . ? C38 C39 C40 C36 -58.4(10) . . . . ? C30 C39 C40 C41 -61.0(12) . . . . ? C38 C39 C40 C41 -174.3(11) . . . . ? C37 C36 C40 C42 -66.6(14) . . . . ? C35 C36 C40 C42 60.0(16) . . . . ? C29 C36 C40 C42 -177.5(11) . . . . ? C37 C36 C40 C39 55.9(10) . . . . ? C35 C36 C40 C39 -177.4(10) . . . . ? C29 C36 C40 C39 -54.9(9) . . . . ? C37 C36 C40 C41 176.7(10) . . . . ? C35 C36 C40 C41 -56.6(14) . . . . ? C29 C36 C40 C41 65.9(12) . . . . ? C50 C45 C46 C47 3.7(14) . . . . ? P1 C45 C46 C47 -176.9(8) . . . . ? C45 C46 C47 C48 -3.4(17) . . . . ? C46 C47 C48 C49 1.0(18) . . . . ? C47 C48 C49 C50 1(2) . . . . ? C48 C49 C50 C45 -0.2(19) . . . . ? C46 C45 C50 C49 -1.9(15) . . . . ? P1 C45 C50 C49 178.6(9) . . . . ? C56 C51 C52 C53 -0.2(19) . . . . ? P1 C51 C52 C53 179.4(11) . . . . ? C51 C52 C53 C54 2(2) . . . . ? C52 C53 C54 C55 -5(2) . . . . ? C53 C54 C55 C56 5(3) . . . . ? C54 C55 C56 C51 -3(2) . . . . ? C52 C51 C56 C55 0.7(19) . . . . ? P1 C51 C56 C55 -178.9(11) . . . . ? C62 C57 C58 C59 -0.8(17) . . . . ? P1 C57 C58 C59 178.8(9) . . . . ? C57 C58 C59 C60 0.3(19) . . . . ? C58 C59 C60 C61 4(2) . . . . ? C59 C60 C61 C62 -8(2) . . . . ? C60 C61 C62 C57 7(2) . . . . ? C58 C57 C62 C61 -3(2) . . . . ? P1 C57 C62 C61 177.6(11) . . . . ? C68 C63 C64 C65 6.9(15) . . . . ? P2 C63 C64 C65 178.5(10) . . . . ? C63 C64 C65 C66 -7.1(18) . . . . ? C64 C65 C66 C67 6(2) . . . . ? C65 C66 C67 C68 -6(3) . . . . ? C66 C67 C68 C63 6(3) . . . . ? C64 C63 C68 C67 -6.1(17) . . . . ? P2 C63 C68 C67 -178.4(13) . . . . ? C74 C69 C70 C71 3.8(18) . . . . ? P2 C69 C70 C71 -178.2(11) . . . . ? C69 C70 C71 C72 -4(2) . . . . ? C70 C71 C72 C73 -5(3) . . . . ? C71 C72 C73 C74 13(3) . . . . ? C72 C73 C74 C69 -13(3) . . . . ? C70 C69 C74 C73 4.2(19) . . . . ? P2 C69 C74 C73 -173.6(12) . . . . ? C80 C75 C76 C77 0.3(13) . . . . ? P2 C75 C76 C77 179.3(7) . . . . ? C75 C76 C77 C78 5.7(16) . . . . ? C76 C77 C78 C79 -11.6(19) . . . . ? C77 C78 C79 C80 10.5(18) . . . . ? C76 C75 C80 C79 -0.8(15) . . . . ? P2 C75 C80 C79 -179.7(8) . . . . ? C78 C79 C80 C75 -4.3(17) . . . . ? C2 C1 O1 Yb1 -10.1(13) . . . . ? C8 C1 O1 Yb1 178.7(6) . . . . ? C2 C3 O2 Yb1 -4.6(14) . . . . ? C4 C3 O2 Yb1 179.4(6) . . . . ? C16 C15 O3 Yb1 -8.8(16) . . . . ? C22 C15 O3 Yb1 175.8(7) . . . . ? C16 C17 O4 Yb1 -5.3(18) . . . . ? C18 C17 O4 Yb1 173.1(9) . . . . ? C30 C29 O5 Yb1 -8.1(15) . . . . ? C36 C29 O5 Yb1 177.6(6) . . . . ? C30 C31 O6 Yb1 -2.9(16) . . . . ? C32 C31 O6 Yb1 173.0(6) . . . . ? Yb1 O11 P1 C45 14.7(16) . . . . ? Yb1 O11 P1 C51 135.7(14) . . . . ? Yb1 O11 P1 C57 -106.6(15) . . . . ? C46 C45 P1 O11 -32.3(9) . . . . ? C50 C45 P1 O11 147.1(7) . . . . ? C46 C45 P1 C51 -154.3(8) . . . . ? C50 C45 P1 C51 25.1(8) . . . . ? C46 C45 P1 C57 91.2(8) . . . . ? C50 C45 P1 C57 -89.4(8) . . . . ? C52 C51 P1 O11 -43.7(10) . . . . ? C56 C51 P1 O11 135.9(9) . . . . ? C52 C51 P1 C45 79.1(10) . . . . ? C56 C51 P1 C45 -101.4(9) . . . . ? C52 C51 P1 C57 -165.0(9) . . . . ? C56 C51 P1 C57 14.5(10) . . . . ? C58 C57 P1 O11 153.0(8) . . . . ? C62 C57 P1 O11 -27.3(10) . . . . ? C58 C57 P1 C45 29.7(9) . . . . ? C62 C57 P1 C45 -150.6(9) . . . . ? C58 C57 P1 C51 -86.6(9) . . . . ? C62 C57 P1 C51 93.1(10) . . . . ? Yb1 O22 P2 C63 -104.3(14) . . . . ? Yb1 O22 P2 C69 134.9(13) . . . . ? Yb1 O22 P2 C75 15.5(15) . . . . ? C64 C63 P2 O22 156.9(8) . . . . ? C68 C63 P2 O22 -32.1(9) . . . . ? C64 C63 P2 C69 -80.2(10) . . . . ? C68 C63 P2 C69 90.8(8) . . . . ? C64 C63 P2 C75 32.9(10) . . . . ? C68 C63 P2 C75 -156.1(8) . . . . ? C70 C69 P2 O22 -43.6(9) . . . . ? C74 C69 P2 O22 134.3(9) . . . . ? C70 C69 P2 C63 -167.3(9) . . . . ? C74 C69 P2 C63 10.6(10) . . . . ? C70 C69 P2 C75 79.9(9) . . . . ? C74 C69 P2 C75 -102.2(9) . . . . ? C80 C75 P2 O22 146.4(8) . . . . ? C76 C75 P2 O22 -32.6(7) . . . . ? C80 C75 P2 C63 -90.0(9) . . . . ? C76 C75 P2 C63 91.0(7) . . . . ? C80 C75 P2 C69 24.0(9) . . . . ? C76 C75 P2 C69 -155.0(6) . . . . ? P2 O22 Yb1 O11 -113.0(13) . . . . ? P2 O22 Yb1 O6 -9.2(14) . . . . ? P2 O22 Yb1 O2 138.0(14) . . . . ? P2 O22 Yb1 O3 79.5(15) . . . . ? P2 O22 Yb1 O4 59.0(14) . . . . ? P2 O22 Yb1 O1 -148.6(14) . . . . ? P2 O22 Yb1 O5 -76.0(14) . . . . ? P1 O11 Yb1 O22 -113.4(13) . . . . ? P1 O11 Yb1 O6 138.4(15) . . . . ? P1 O11 Yb1 O2 -8.3(15) . . . . ? P1 O11 Yb1 O3 59.0(14) . . . . ? P1 O11 Yb1 O4 79.8(16) . . . . ? P1 O11 Yb1 O1 -77.2(15) . . . . ? P1 O11 Yb1 O5 -149.7(15) . . . . ? C31 O6 Yb1 O22 -70.2(9) . . . . ? C31 O6 Yb1 O11 73.9(9) . . . . ? C31 O6 Yb1 O2 -177.5(8) . . . . ? C31 O6 Yb1 O3 146.3(9) . . . . ? C31 O6 Yb1 O4 -137.2(9) . . . . ? C31 O6 Yb1 O1 12.6(11) . . . . ? C31 O6 Yb1 O5 -2.5(9) . . . . ? C3 O2 Yb1 O22 74.0(8) . . . . ? C3 O2 Yb1 O11 -70.3(8) . . . . ? C3 O2 Yb1 O6 -175.0(6) . . . . ? C3 O2 Yb1 O3 -137.5(8) . . . . ? C3 O2 Yb1 O4 145.9(8) . . . . ? C3 O2 Yb1 O1 -1.6(7) . . . . ? C3 O2 Yb1 O5 12.9(9) . . . . ? C15 O3 Yb1 O22 -16.2(11) . . . . ? C15 O3 Yb1 O11 171.7(9) . . . . ? C15 O3 Yb1 O6 80.0(9) . . . . ? C15 O3 Yb1 O2 -79.5(9) . . . . ? C15 O3 Yb1 O4 4.1(9) . . . . ? C15 O3 Yb1 O1 -134.2(8) . . . . ? C15 O3 Yb1 O5 127.4(8) . . . . ? C17 O4 Yb1 O22 170.3(9) . . . . ? C17 O4 Yb1 O11 -18.0(11) . . . . ? C17 O4 Yb1 O6 -80.8(9) . . . . ? C17 O4 Yb1 O2 77.3(9) . . . . ? C17 O4 Yb1 O3 2.6(9) . . . . ? C17 O4 Yb1 O1 127.9(9) . . . . ? C17 O4 Yb1 O5 -135.2(9) . . . . ? C1 O1 Yb1 O22 -85.1(7) . . . . ? C1 O1 Yb1 O11 116.3(8) . . . . ? C1 O1 Yb1 O6 -177.4(7) . . . . ? C1 O1 Yb1 O2 8.5(7) . . . . ? C1 O1 Yb1 O3 62.7(8) . . . . ? C1 O1 Yb1 O4 -43.8(9) . . . . ? C1 O1 Yb1 O5 -162.1(7) . . . . ? C29 O5 Yb1 O22 116.5(8) . . . . ? C29 O5 Yb1 O11 -85.4(8) . . . . ? C29 O5 Yb1 O6 7.4(8) . . . . ? C29 O5 Yb1 O2 -177.3(7) . . . . ? C29 O5 Yb1 O3 -42.2(9) . . . . ? C29 O5 Yb1 O4 62.5(8) . . . . ? C29 O5 Yb1 O1 -162.5(8) . . . . ? F9 C18 C19 F11 -42.7(18) . . . . ? F8 C18 C19 F11 -167.1(16) . . . . ? C17 C18 C19 F11 71.2(16) . . . . ? F9 C18 C19 F10 -168.0(14) . . . . ? F8 C18 C19 F10 68(2) . . . . ? C17 C18 C19 F10 -54.1(17) . . . . ? F9 C18 C19 C20 87.5(14) . . . . ? F8 C18 C19 C20 -36.9(18) . . . . ? C17 C18 C19 C20 -158.6(10) . . . . ? F11 C19 C20 F14 -77(2) . . . . ? F10 C19 C20 F14 46(2) . . . . ? C18 C19 C20 F14 161.5(18) . . . . ? F11 C19 C20 F12 151(2) . . . . ? F10 C19 C20 F12 -84.8(18) . . . . ? C18 C19 C20 F12 30.3(18) . . . . ? F11 C19 C20 F13 49(2) . . . . ? F10 C19 C20 F13 172.3(14) . . . . ? C18 C19 C20 F13 -72.5(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7C O1 0.96 2.68 2.912(12) 94.0 . C25 H25 F11 0.98 2.04 2.69(3) 121.9 . C27 H27A F2 0.96 2.46 3.26(2) 141.2 . C39 H39 F16 0.98 2.41 2.799(15) 102.7 . C23 H23A F14 0.97 2.19 3.04(3) 145.6 2_765 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.697 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.144 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_III _database_code_depnum_ccdc_archive 'CCDC 777709' #TrackingRef '- CIF-R.cif' # start Validation Reply Form _vrf_PLAT241_III ; PROBLEM: Check High Ueq as Compared to Neighbors for C24 RESPONSE: Many crystals tried, best presented - the static/positional disorder of the ligand lead to this anomalous value. ; _vrf_PLAT242_III ; PROBLEM: Check Low Ueq as Compared to Neighbors for C20 RESPONSE: Many crystals tried, best presented - the static/positional disorder of the ligand lead to this anomalous value. ; _vrf_PLAT602_III ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The lattice contains large solvent accessible voids, but the solvent was highly disordered and therefore could not be modeled. Instead, the disordered solvent was accounted for using the program SQUEEZE, which estimated that 216 electrons were located in the voids of 1182.5 A3, which is equivalent to 1 molecules of CHCl3 and 3 molecules of hexane; these were included in the formula in Table 2. ; _vrf_PLAT112_III ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 RESPONSE: see comments under _refine_special_details ; _vrf_PLAT860_III ; PROBLEM: Note: Number of Least-Squares Restraints ....... 26 RESPONSE: Owing to the static/positional disorder of the ligand, 26 least-squares restraints were used to refine the structure.The restraints are listed under _refine_special_details ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84.33 H78.33 Cl F21 N0 O8 P2 Yb' _chemical_formula_weight 1889.23 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 14.800(3) _cell_length_b 14.800(3) _cell_length_c 34.447(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6535(3) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7050 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.08 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2863 _exptl_absorpt_coefficient_mu 1.238 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34806 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.99 _reflns_number_total 13049 _reflns_number_gt 11283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There is one crystallographically independent molecule on a general position in this structure. Increasing the space group symmetry from P32 to P3221 effectively adds a 2-fold rotation axis through the Yb center and C16 with the Yb located on the rotation axis. While the belta-diketone ligands containing O1O2 and O5O6 and TPPO ligands are compatible with this symmetry element the belta-diketone ligands containing O3O4 are not. The ligands suffer from the static/positional disorder which is incompatible with the 2-fold axis. It is thus proposed that this rotation is a pseudo-symmetry element only, rather than a genuine symmetry element. This is supported by the ADDSYM-EXT routine in PLATON, which does not detect missed symmetry in space group P32. For these reasons, we are convinced that P32 is the correct space group for this complex. dfix 2.10 0.02 F12 F13 F13 F14 F14 F12 dfix 1.35 0.02 C20 F12 C20 F13 C20 F14 dfix 1.35 C19 F11 C19 F10 C20 F12 dfix 1.52 0.02 C19 C20 dfix 1.54 0.02 C23 C24 C25 C24 C25 C26 dfix 1.50 0.02 C16 C25 dfix 2.40 0.02 C22 C25 isor 0.01 F13 delu 0.01 F12 C20 delu 0.01 C23 C24 delu 0.01 C26 C27 delu 0.01 F14 C20 ; _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^)+(0.1109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.052(10) _refine_ls_number_reflns 13049 _refine_ls_number_parameters 963 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.166 _refine_ls_shift/su_mean 0.010 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 F11 F 0.9782(16) 0.9366(15) 0.0149(6) 0.278(9) Uani 1 1 d D . . F10 F 0.8575(11) 0.9395(11) -0.0207(4) 0.190(3) Uani 1 1 d D . . C19 C 0.9607(10) 1.0019(14) -0.0068(4) 0.115(3) Uani 1 1 d D . . C34 C 1.0510(13) 1.4252(19) 0.1707(6) 0.189(11) Uani 1 1 d . . . F21 F 1.1240(8) 1.4025(14) 0.1473(4) 0.229(8) Uani 1 1 d . . . F19 F 1.0740(10) 1.5141(8) 0.1607(4) 0.204(6) Uani 1 1 d . . . F20 F 1.0679(8) 1.4123(9) 0.2061(4) 0.183(5) Uani 1 1 d . . . C1 C 0.4132(7) 0.8057(9) 0.0624(2) 0.078(2) Uani 1 1 d . . . C2 C 0.4403(7) 0.7297(8) 0.0509(3) 0.079(2) Uani 1 1 d . . . C3 C 0.5407(9) 0.7499(9) 0.0539(3) 0.078(3) Uani 1 1 d . . . C4 C 0.5689(9) 0.6623(9) 0.0433(3) 0.095(3) Uani 1 1 d . . . C5 C 0.6058(11) 0.6606(9) 0.0033(4) 0.098(3) Uani 1 1 d . . . C6 C 0.6410(16) 0.5866(13) -0.0062(6) 0.135(6) Uani 1 1 d . . . C7 C 0.2492(8) 0.8248(10) 0.0615(4) 0.101(2) Uani 1 1 d . . . H7A H 0.1752 0.7871 0.0573 0.151 Uiso 1 1 calc R . . H7B H 0.2823 0.8770 0.0418 0.151 Uiso 1 1 calc R . . H7C H 0.2638 0.8577 0.0866 0.151 Uiso 1 1 calc R . . C8 C 0.2908(8) 0.7502(11) 0.0600(4) 0.101(2) Uani 1 1 d . . . C9 C 0.2538(10) 0.6666(11) 0.0920(4) 0.113(4) Uani 1 1 d . . . H9A H 0.1795 0.6366 0.0964 0.135 Uiso 1 1 calc R . . H9B H 0.2902 0.6973 0.1161 0.135 Uiso 1 1 calc R . . C10 C 0.2780(10) 0.5810(11) 0.0780(5) 0.117(4) Uani 1 1 d . . . H10A H 0.2149 0.5142 0.0746 0.141 Uiso 1 1 calc R . . H10B H 0.3246 0.5731 0.0957 0.141 Uiso 1 1 calc R . . C11 C 0.3330(9) 0.6306(11) 0.0377(4) 0.110(4) Uani 1 1 d . . . H11 H 0.3388 0.5831 0.0194 0.132 Uiso 1 1 calc R . . C12 C 0.2751(8) 0.6824(10) 0.0236(3) 0.094(3) Uani 1 1 d . . . C13 C 0.3239(11) 0.7441(11) -0.0133(3) 0.113(4) Uani 1 1 d . . . H13A H 0.3976 0.7884 -0.0095 0.170 Uiso 1 1 calc R . . H13B H 0.2931 0.7860 -0.0193 0.170 Uiso 1 1 calc R . . H13C H 0.3119 0.6968 -0.0343 0.170 Uiso 1 1 calc R . . C14 C 0.1561(11) 0.6018(13) 0.0153(5) 0.154(7) Uani 1 1 d . . . H14A H 0.1237 0.6375 0.0037 0.231 Uiso 1 1 calc R . . H14B H 0.1215 0.5701 0.0392 0.231 Uiso 1 1 calc R . . H14C H 0.1509 0.5488 -0.0022 0.231 Uiso 1 1 calc R . . C15 C 0.8468(7) 0.9618(8) 0.1117(3) 0.077(2) Uani 1 1 d . . . C16 C 0.9115(7) 1.0024(9) 0.0802(3) 0.079(2) Uani 1 1 d D . . C17 C 0.8834(8) 1.0399(9) 0.0483(3) 0.087(3) Uani 1 1 d . . . C18 C 0.9691(10) 1.0849(13) 0.0178(4) 0.115(3) Uani 1 1 d . . . C21 C 0.8014(11) 0.8414(11) 0.1669(6) 0.133(5) Uani 1 1 d . . . H21A H 0.7843 0.7737 0.1574 0.199 Uiso 1 1 calc R . . H21B H 0.7425 0.8512 0.1635 0.199 Uiso 1 1 calc R . . H21C H 0.8190 0.8467 0.1939 0.199 Uiso 1 1 calc R . . C22 C 0.8846(10) 0.9164(13) 0.1465(3) 0.116(4) Uani 1 1 d D . . C23 C 0.9808(17) 1.0314(19) 0.1655(4) 0.193(10) Uani 1 1 d DU . . H23A H 0.9568 1.0804 0.1705 0.232 Uiso 1 1 calc R . . H23B H 1.0108 1.0210 0.1889 0.232 Uiso 1 1 calc R . . C24 C 1.0578(14) 1.065(2) 0.1301(8) 0.264(16) Uani 1 1 d DU . . H1C H 1.1209 1.0645 0.1372 0.316 Uiso 1 1 calc R . . H1D H 1.0766 1.1349 0.1215 0.316 Uiso 1 1 calc R . . C25 C 0.9947(11) 0.9791(15) 0.0953(5) 0.178(9) Uani 1 1 d D . . H25 H 1.0405 0.9781 0.0749 0.214 Uiso 1 1 calc R . . C26 C 0.9395(11) 0.8730(11) 0.1218(5) 0.119(5) Uani 1 1 d DU . . C27 C 0.8858(16) 0.7950(17) 0.0967(8) 0.186(10) Uani 1 1 d U . . H27A H 0.8826 0.7324 0.1062 0.279 Uiso 1 1 calc R . . H27B H 0.9200 0.8128 0.0719 0.279 Uiso 1 1 calc R . . H27C H 0.8163 0.7837 0.0940 0.279 Uiso 1 1 calc R . . C28 C 1.0220(12) 0.8512(13) 0.1451(5) 0.127(3) Uani 1 1 d . . . C29 C 0.6078(13) 1.1932(14) 0.0987(5) 0.127(3) Uani 1 1 d . . . C30 C 0.7125(8) 1.2744(9) 0.1105(3) 0.083(3) Uani 1 1 d . . . C31 C 0.7911(8) 1.2516(9) 0.1093(3) 0.081(3) Uani 1 1 d . . . C32 C 0.9077(15) 1.3397(15) 0.1162(5) 0.137(4) Uani 1 1 d . . . C33 C 0.9462(11) 1.3398(11) 0.1575(4) 0.112(4) Uani 1 1 d . . . C35 C 0.4244(10) 1.1811(13) 0.0998(5) 0.127(5) Uani 1 1 d . . . H35A H 0.3924 1.2211 0.0924 0.190 Uiso 1 1 calc R . . H35B H 0.3995 1.1512 0.1250 0.190 Uiso 1 1 calc R . . H35C H 0.4069 1.1264 0.0813 0.190 Uiso 1 1 calc R . . C36 C 0.5434(10) 1.2526(10) 0.1012(3) 0.095(3) Uani 1 1 d . . . C37 C 0.5808(13) 1.3316(12) 0.0690(4) 0.125(5) Uani 1 1 d . . . H37A H 0.5362 1.3618 0.0662 0.150 Uiso 1 1 calc R . . H37B H 0.5841 1.3011 0.0445 0.150 Uiso 1 1 calc R . . C38 C 0.7027(12) 1.4223(10) 0.0849(5) 0.120(5) Uani 1 1 d . . . H38A H 0.7563 1.4316 0.0665 0.144 Uiso 1 1 calc R . . H38B H 0.7077 1.4891 0.0899 0.144 Uiso 1 1 calc R . . C39 C 0.7099(11) 1.3732(10) 0.1209(4) 0.099(3) Uani 1 1 d . . . H39 H 0.7653 1.4203 0.1386 0.119 Uiso 1 1 calc R . . C40 C 0.5937(11) 1.3219(11) 0.1386(4) 0.102(3) Uani 1 1 d . . . C41 C 0.5734(14) 1.2528(13) 0.1769(4) 0.128(5) Uani 1 1 d . . . H41A H 0.6203 1.2954 0.1971 0.192 Uiso 1 1 calc R . . H41B H 0.5852 1.1960 0.1713 0.192 Uiso 1 1 calc R . . H41C H 0.5027 1.2257 0.1854 0.192 Uiso 1 1 calc R . . C42 C 0.5600(13) 1.3964(13) 0.1481(5) 0.136(5) Uani 1 1 d . . . H42A H 0.6199 1.4629 0.1540 0.205 Uiso 1 1 calc R . . H42B H 0.5146 1.3719 0.1703 0.205 Uiso 1 1 calc R . . H42C H 0.5233 1.4036 0.1264 0.205 Uiso 1 1 calc R . . C43 C 0.6731(7) 1.0339(12) -0.0563(4) 0.072(3) Uani 1 1 d . . . C44 C 0.7192(9) 1.0841(9) -0.0905(3) 0.087(3) Uani 1 1 d . . . H44 H 0.7291 1.1506 -0.0943 0.105 Uiso 1 1 calc R . . C45 C 0.7527(12) 1.0416(11) -0.1203(4) 0.109(4) Uani 1 1 d . . . H45 H 0.7866 1.0800 -0.1423 0.131 Uiso 1 1 calc R . . C46 C 0.7330(12) 0.9407(13) -0.1152(4) 0.117(4) Uani 1 1 d . . . H46 H 0.7530 0.9099 -0.1344 0.140 Uiso 1 1 calc R . . C47 C 0.6839(15) 0.8848(11) -0.0821(4) 0.133(6) Uani 1 1 d . . . H47 H 0.6717 0.8172 -0.0792 0.159 Uiso 1 1 calc R . . C48 C 0.6543(11) 0.9263(9) -0.0549(3) 0.097(4) Uani 1 1 d . . . H48 H 0.6194 0.8854 -0.0335 0.116 Uiso 1 1 calc R . . C49 C 0.7088(7) 1.2217(7) -0.0192(2) 0.067(2) Uani 1 1 d . . . C50 C 0.6870(11) 1.2790(10) -0.0396(4) 0.102(3) Uani 1 1 d . . . H50 H 0.6271 1.2491 -0.0549 0.123 Uiso 1 1 calc R . . C51 C 0.7563(14) 1.3937(11) -0.0393(5) 0.126(5) Uani 1 1 d . . . H51 H 0.7416 1.4385 -0.0533 0.151 Uiso 1 1 calc R . . C52 C 0.8418(12) 1.4280(10) -0.0173(5) 0.118(5) Uani 1 1 d . . . H52 H 0.8922 1.4983 -0.0186 0.141 Uiso 1 1 calc R . . C53 C 0.8575(10) 1.3698(12) 0.0051(3) 0.104(4) Uani 1 1 d . . . H53 H 0.9128 1.4008 0.0225 0.125 Uiso 1 1 calc R . . C54 C 0.7957(7) 1.2606(8) 0.0051(3) 0.077(3) Uani 1 1 d . . . H54 H 0.8113 1.2178 0.0200 0.093 Uiso 1 1 calc R . . C55 C 0.4971(7) 1.0511(7) -0.0349(3) 0.072(2) Uani 1 1 d . . . C56 C 0.4392(10) 1.0643(14) -0.0055(3) 0.110(4) Uani 1 1 d . . . H56 H 0.4661 1.0860 0.0193 0.132 Uiso 1 1 calc R . . C57 C 0.3381(11) 1.0428(15) -0.0156(4) 0.131(6) Uani 1 1 d . . . H57 H 0.2958 1.0493 0.0029 0.157 Uiso 1 1 calc R . . C58 C 0.3013(10) 1.0113(16) -0.0540(5) 0.143(6) Uani 1 1 d . . . H58 H 0.2370 1.0031 -0.0611 0.171 Uiso 1 1 calc R . . C59 C 0.3551(11) 0.9938(14) -0.0794(5) 0.129(5) Uani 1 1 d . . . H59 H 0.3248 0.9626 -0.1029 0.155 Uiso 1 1 calc R . . C60 C 0.4607(9) 1.0220(11) -0.0715(3) 0.101(4) Uani 1 1 d . . . H60 H 0.5033 1.0204 -0.0909 0.121 Uiso 1 1 calc R . . C61 C 0.4915(7) 0.7829(8) 0.1795(3) 0.077(2) Uani 1 1 d . . . C62 C 0.4034(8) 0.7160(10) 0.2033(3) 0.095(3) Uani 1 1 d . . . H62 H 0.3741 0.7441 0.2198 0.114 Uiso 1 1 calc R . . C63 C 0.3633(10) 0.6104(11) 0.2014(4) 0.108(4) Uani 1 1 d . . . H63 H 0.3028 0.5672 0.2152 0.130 Uiso 1 1 calc R . . C64 C 0.4059(13) 0.5687(10) 0.1814(4) 0.126(5) Uani 1 1 d . . . H64 H 0.3803 0.4972 0.1832 0.152 Uiso 1 1 calc R . . C65 C 0.4920(12) 0.6303(11) 0.1563(4) 0.110(4) Uani 1 1 d . . . H65 H 0.5194 0.5998 0.1400 0.132 Uiso 1 1 calc R . . C66 C 0.5328(9) 0.7365(10) 0.1570(3) 0.086(3) Uani 1 1 d . . . H66 H 0.5907 0.7784 0.1417 0.103 Uiso 1 1 calc R . . C67 C 0.4464(7) 0.9503(8) 0.1958(3) 0.078(2) Uani 1 1 d . . . C68 C 0.4388(10) 0.9777(11) 0.2332(4) 0.106(4) Uani 1 1 d . . . H68 H 0.4869 0.9843 0.2520 0.127 Uiso 1 1 calc R . . C69 C 0.3568(12) 0.9956(15) 0.2423(5) 0.138(6) Uani 1 1 d . . . H69 H 0.3480 1.0120 0.2676 0.165 Uiso 1 1 calc R . . C70 C 0.2924(12) 0.9890(13) 0.2147(5) 0.122(5) Uani 1 1 d . . . H70 H 0.2402 1.0040 0.2210 0.147 Uiso 1 1 calc R . . C71 C 0.2976(10) 0.9621(14) 0.1786(4) 0.128(5) Uani 1 1 d . . . H71 H 0.2502 0.9577 0.1599 0.153 Uiso 1 1 calc R . . C72 C 0.3769(9) 0.9403(11) 0.1694(3) 0.097(3) Uani 1 1 d . . . H72 H 0.3808 0.9186 0.1444 0.117 Uiso 1 1 calc R . . C73 C 0.6457(8) 0.9738(10) 0.2203(4) 0.061(3) Uani 1 1 d . . . C74 C 0.6335(9) 0.9144(10) 0.2524(3) 0.092(3) Uani 1 1 d . . . H74 H 0.5760 0.8480 0.2553 0.110 Uiso 1 1 calc R . . C75 C 0.7130(11) 0.9593(11) 0.2811(3) 0.103(4) Uani 1 1 d . . . H75 H 0.7111 0.9202 0.3025 0.124 Uiso 1 1 calc R . . C76 C 0.7912(10) 1.0584(11) 0.2772(4) 0.106(4) Uani 1 1 d . . . H76 H 0.8386 1.0913 0.2972 0.127 Uiso 1 1 calc R . . C77 C 0.7998(10) 1.1094(10) 0.2437(5) 0.121(5) Uani 1 1 d . . . H77 H 0.8590 1.1748 0.2410 0.145 Uiso 1 1 calc R . . C78 C 0.7309(11) 1.0754(11) 0.2132(4) 0.118(5) Uani 1 1 d . . . H78 H 0.7390 1.1138 0.1909 0.142 Uiso 1 1 calc R . . F1 F 0.6462(11) 0.6719(11) 0.0694(4) 0.190(3) Uani 1 1 d . . . F2 F 0.4892(14) 0.5661(13) 0.0501(5) 0.240(5) Uani 1 1 d . . . F3 F 0.5293(7) 0.6541(8) -0.0204(2) 0.129(3) Uani 1 1 d . . . F4 F 0.6940(7) 0.7587(6) -0.0029(3) 0.138(3) Uani 1 1 d . . . F5 F 0.7210(13) 0.5954(12) 0.0135(4) 0.210(6) Uani 1 1 d . . . F6 F 0.6580(11) 0.5857(9) -0.0432(4) 0.188(5) Uani 1 1 d . . . F7 F 0.5619(13) 0.4881(8) 0.0014(4) 0.207(6) Uani 1 1 d . . . F8 F 0.9661(15) 1.1685(18) -0.0040(6) 0.293(11) Uani 1 1 d . . . F9 F 1.0643(7) 1.1253(11) 0.0375(4) 0.183(5) Uani 1 1 d . . . F15 F 0.9181(6) 1.4335(5) 0.1093(2) 0.111(2) Uani 1 1 d . . . F16 F 0.9776(6) 1.3247(8) 0.0929(2) 0.132(3) Uani 1 1 d . . . F17 F 0.8776(6) 1.3502(7) 0.1824(2) 0.125(2) Uani 1 1 d . . . F18 F 0.9356(7) 1.2439(7) 0.1635(3) 0.146(3) Uani 1 1 d . . . O1 O 0.4683(5) 0.8952(6) 0.0749(2) 0.0836(18) Uani 1 1 d . . . O2 O 0.6207(5) 0.8377(6) 0.0617(2) 0.0787(17) Uani 1 1 d . . . O3 O 0.7606(5) 0.9595(6) 0.1189(2) 0.0802(17) Uani 1 1 d . . . O4 O 0.8030(5) 1.0430(6) 0.04278(18) 0.0779(17) Uani 1 1 d . . . O5 O 0.5765(5) 1.1073(5) 0.08526(18) 0.0760(16) Uani 1 1 d . . . O6 O 0.7815(5) 1.1625(5) 0.0999(2) 0.0808(17) Uani 1 1 d . . . O11 O 0.6211(5) 1.0293(6) 0.01897(15) 0.0744(16) Uani 1 1 d . . . O22 O 0.5921(5) 0.9710(6) 0.14283(16) 0.0747(16) Uani 1 1 d . . . P1 P 0.62587(17) 1.07847(19) -0.01947(6) 0.0650(5) Uani 1 1 d . . . P2 P 0.54803(17) 0.92191(19) 0.18077(6) 0.0644(5) Uani 1 1 d . . . Yb1 Yb 0.65593(3) 1.00032(4) 0.08072(3) 0.06090(13) Uani 1 1 d . . . F14 F 1.1282(12) 1.099(2) -0.0369(7) 0.55(3) Uani 1 1 d DU . . F12 F 1.0269(13) 1.1326(12) -0.0637(5) 0.240(5) Uani 1 1 d DU . . F13 F 1.013(2) 0.9871(18) -0.0771(8) 0.389(14) Uani 1 1 d DU . . C20 C 1.0242(13) 1.0509(12) -0.0462(4) 0.137(4) Uani 1 1 d DU . . 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 F11 0.29(2) 0.29(2) 0.31(3) -0.024(17) 0.035(17) 0.192(19) F10 0.222(9) 0.233(9) 0.148(7) -0.020(6) -0.018(6) 0.138(8) C19 0.100(6) 0.174(10) 0.091(6) 0.007(6) 0.016(5) 0.082(7) C34 0.096(10) 0.21(2) 0.145(16) 0.096(15) -0.030(10) -0.012(11) F21 0.084(6) 0.34(2) 0.169(11) 0.055(11) 0.001(6) 0.039(8) F19 0.201(11) 0.107(6) 0.205(12) 0.036(7) -0.050(9) 0.002(7) F20 0.143(8) 0.190(10) 0.149(9) 0.030(7) -0.042(7) 0.034(7) C1 0.078(5) 0.113(8) 0.036(4) 0.011(4) 0.001(4) 0.042(6) C2 0.072(5) 0.093(6) 0.073(6) -0.002(5) -0.003(4) 0.043(5) C3 0.101(7) 0.093(8) 0.045(5) 0.012(5) 0.006(4) 0.052(6) C4 0.089(7) 0.089(7) 0.082(7) 0.013(5) 0.001(5) 0.027(6) C5 0.127(9) 0.093(7) 0.079(7) 0.014(6) 0.005(6) 0.058(7) C6 0.176(15) 0.124(12) 0.140(15) 0.038(10) 0.041(12) 0.100(12) C7 0.062(4) 0.139(7) 0.093(6) 0.007(5) -0.003(4) 0.043(4) C8 0.062(4) 0.139(7) 0.093(6) 0.007(5) -0.003(4) 0.043(4) C9 0.094(8) 0.126(10) 0.068(7) 0.002(6) 0.009(6) 0.017(7) C10 0.096(8) 0.104(8) 0.121(11) 0.033(8) 0.017(7) 0.027(7) C11 0.092(7) 0.136(10) 0.075(7) -0.016(7) 0.005(6) 0.036(7) C12 0.079(6) 0.119(8) 0.062(6) 0.007(5) -0.017(5) 0.031(6) C13 0.116(9) 0.131(10) 0.058(6) 0.010(6) -0.026(6) 0.036(8) C14 0.090(8) 0.168(14) 0.134(13) 0.000(10) -0.046(8) 0.013(9) C15 0.064(5) 0.107(7) 0.074(6) -0.007(5) -0.024(4) 0.053(5) C16 0.075(5) 0.108(7) 0.070(6) -0.021(5) -0.012(5) 0.058(5) C17 0.076(6) 0.124(8) 0.078(7) -0.024(6) -0.004(5) 0.063(6) C18 0.100(6) 0.174(10) 0.091(6) 0.007(6) 0.016(5) 0.082(7) C21 0.112(10) 0.114(10) 0.169(15) 0.038(10) 0.050(10) 0.054(8) C22 0.099(8) 0.193(14) 0.077(7) 0.024(8) -0.005(6) 0.089(9) C23 0.26(2) 0.32(3) 0.084(10) -0.084(14) -0.107(11) 0.20(2) C24 0.096(12) 0.34(4) 0.31(3) -0.14(3) -0.052(14) 0.074(18) C25 0.101(11) 0.25(3) 0.154(18) -0.024(17) 0.029(11) 0.064(14) C26 0.117(9) 0.140(10) 0.159(13) -0.008(8) -0.023(8) 0.109(9) C27 0.166(16) 0.20(2) 0.24(3) -0.071(16) 0.013(14) 0.120(16) C28 0.140(8) 0.161(9) 0.127(8) 0.004(7) -0.002(6) 0.109(8) C29 0.140(8) 0.161(9) 0.127(8) 0.004(7) -0.002(6) 0.109(8) C30 0.088(6) 0.115(8) 0.062(5) 0.011(5) 0.011(5) 0.063(6) C31 0.086(6) 0.100(8) 0.059(5) -0.021(5) -0.008(4) 0.047(6) C32 0.180(10) 0.170(10) 0.093(7) 0.004(6) 0.013(7) 0.112(9) C33 0.108(9) 0.112(9) 0.089(9) 0.026(7) 0.006(7) 0.036(7) C35 0.110(9) 0.181(14) 0.136(12) 0.011(10) 0.010(8) 0.107(10) C36 0.123(8) 0.128(9) 0.076(7) 0.017(6) 0.023(6) 0.094(8) C37 0.178(14) 0.157(13) 0.097(9) 0.044(9) 0.026(9) 0.126(12) C38 0.143(12) 0.091(8) 0.137(12) 0.024(8) 0.048(10) 0.067(8) C39 0.125(9) 0.104(8) 0.082(7) -0.001(6) -0.007(6) 0.067(7) C40 0.134(10) 0.119(9) 0.079(7) -0.001(6) 0.020(6) 0.082(8) C41 0.186(15) 0.161(13) 0.074(8) 0.009(8) 0.021(8) 0.115(12) C42 0.151(13) 0.154(13) 0.129(13) -0.022(10) 0.005(9) 0.095(11) C43 0.078(7) 0.074(7) 0.064(8) -0.001(6) -0.012(4) 0.037(6) C44 0.105(7) 0.084(8) 0.073(7) 0.013(6) 0.018(6) 0.047(6) C45 0.136(12) 0.125(10) 0.078(8) 0.007(7) 0.022(7) 0.074(9) C46 0.144(11) 0.159(13) 0.081(8) -0.018(8) 0.009(7) 0.100(11) C47 0.244(19) 0.112(9) 0.080(8) 0.002(7) 0.024(9) 0.118(12) C48 0.130(10) 0.093(8) 0.068(6) 0.019(5) 0.026(6) 0.056(7) C49 0.086(5) 0.085(5) 0.039(4) -0.006(4) 0.002(4) 0.049(5) C50 0.118(9) 0.106(8) 0.086(8) -0.020(6) 0.009(6) 0.058(7) C51 0.161(13) 0.088(8) 0.141(13) 0.023(8) 0.020(11) 0.073(9) C52 0.119(10) 0.085(8) 0.098(10) -0.007(7) 0.027(8) 0.014(7) C53 0.110(8) 0.120(11) 0.058(6) 0.006(7) 0.003(5) 0.038(8) C54 0.072(5) 0.085(7) 0.059(5) -0.002(5) 0.005(4) 0.027(5) C55 0.071(5) 0.094(6) 0.065(5) 0.001(4) -0.009(4) 0.051(5) C56 0.103(8) 0.190(14) 0.064(7) -0.008(7) -0.012(6) 0.094(9) C57 0.105(9) 0.231(18) 0.104(10) -0.015(10) 0.003(7) 0.119(11) C58 0.081(8) 0.216(17) 0.135(14) 0.058(12) 0.002(8) 0.077(10) C59 0.100(9) 0.204(16) 0.100(10) -0.032(10) -0.037(7) 0.088(10) C60 0.100(7) 0.171(11) 0.054(5) -0.016(6) -0.016(5) 0.083(8) C61 0.077(5) 0.094(6) 0.054(5) 0.001(4) 0.002(4) 0.038(5) C62 0.090(6) 0.112(8) 0.068(6) 0.013(5) 0.021(5) 0.038(6) C63 0.108(8) 0.099(9) 0.088(8) -0.005(7) 0.007(7) 0.029(7) C64 0.160(13) 0.079(7) 0.093(9) 0.011(7) -0.027(9) 0.024(8) C65 0.134(10) 0.092(9) 0.115(10) -0.015(8) -0.012(8) 0.065(8) C66 0.107(7) 0.099(8) 0.068(6) 0.005(5) 0.008(5) 0.063(7) C67 0.072(5) 0.097(6) 0.071(6) -0.002(5) 0.001(4) 0.046(5) C68 0.106(8) 0.150(11) 0.086(8) -0.016(7) 0.011(6) 0.082(8) C69 0.135(11) 0.235(19) 0.088(9) -0.019(10) 0.021(8) 0.126(13) C70 0.125(11) 0.160(13) 0.121(12) 0.002(9) 0.029(9) 0.100(10) C71 0.088(8) 0.213(17) 0.102(10) -0.014(10) -0.010(7) 0.090(10) C72 0.104(8) 0.154(11) 0.066(6) 0.004(7) 0.003(5) 0.088(8) C73 0.055(5) 0.080(6) 0.048(7) 0.003(5) -0.003(4) 0.034(4) C74 0.101(7) 0.092(8) 0.071(7) -0.002(6) -0.009(5) 0.041(6) C75 0.127(9) 0.122(9) 0.074(7) 0.010(6) -0.023(6) 0.073(9) C76 0.089(9) 0.124(10) 0.088(9) -0.013(7) -0.022(7) 0.041(8) C77 0.086(7) 0.101(8) 0.123(11) 0.011(8) -0.021(7) 0.008(6) C78 0.109(9) 0.105(9) 0.090(9) 0.000(7) -0.011(7) 0.016(8) F1 0.222(9) 0.233(9) 0.148(7) -0.020(6) -0.018(6) 0.138(8) F2 0.272(11) 0.259(10) 0.253(11) 0.140(9) 0.118(9) 0.180(10) F3 0.157(7) 0.163(7) 0.097(6) 0.000(5) -0.009(5) 0.101(6) F4 0.148(7) 0.112(5) 0.152(7) 0.037(5) 0.070(6) 0.062(5) F5 0.292(17) 0.255(15) 0.205(13) 0.014(10) 0.031(11) 0.229(15) F6 0.266(13) 0.172(9) 0.181(11) 0.054(8) 0.109(10) 0.151(10) F7 0.311(16) 0.121(7) 0.230(13) 0.030(7) 0.085(12) 0.139(9) F8 0.277(18) 0.41(3) 0.29(2) 0.21(2) 0.111(16) 0.24(2) F9 0.097(6) 0.238(12) 0.187(10) -0.030(9) 0.027(6) 0.063(7) F15 0.126(5) 0.086(4) 0.095(4) 0.024(3) -0.004(4) 0.034(4) F16 0.091(4) 0.193(8) 0.076(4) 0.015(4) 0.026(3) 0.045(5) F17 0.106(5) 0.158(7) 0.089(5) -0.005(4) 0.000(4) 0.050(5) F18 0.148(7) 0.122(6) 0.137(7) 0.047(5) -0.017(5) 0.045(5) O1 0.055(4) 0.098(5) 0.087(5) 0.000(4) 0.009(3) 0.031(3) O2 0.073(4) 0.093(4) 0.073(4) -0.008(3) -0.010(3) 0.044(4) O3 0.076(4) 0.115(5) 0.075(4) -0.007(3) -0.012(3) 0.067(4) O4 0.069(4) 0.124(5) 0.053(3) -0.013(3) -0.009(3) 0.058(4) O5 0.100(4) 0.098(4) 0.059(4) -0.007(3) -0.001(3) 0.071(4) O6 0.070(4) 0.092(4) 0.079(4) -0.021(3) -0.006(3) 0.040(3) O11 0.075(3) 0.109(4) 0.043(3) 0.004(3) -0.005(2) 0.049(3) O22 0.083(4) 0.112(5) 0.047(3) 0.012(3) 0.015(3) 0.062(4) P1 0.0699(12) 0.0876(14) 0.0448(11) 0.0040(9) -0.0019(9) 0.0449(11) P2 0.0665(12) 0.0879(14) 0.0429(10) 0.0020(9) 0.0060(9) 0.0417(11) Yb1 0.0620(2) 0.0893(3) 0.04085(17) 0.00023(10) 0.0004(2) 0.0449(2) F14 0.155(10) 0.99(8) 0.33(3) 0.06(4) 0.084(14) 0.16(3) F12 0.272(11) 0.259(10) 0.253(11) 0.140(9) 0.118(9) 0.180(10) F13 0.393(16) 0.385(16) 0.389(17) -0.041(10) 0.013(10) 0.194(11) C20 0.180(10) 0.170(10) 0.093(7) 0.004(6) 0.013(7) 0.112(9) _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 F11 C19 1.346(16) . ? F10 C19 1.416(14) . ? C19 C18 1.45(2) . ? C19 C20 1.604(14) . ? C34 F19 1.23(2) . ? C34 F20 1.278(18) . ? C34 C33 1.50(2) . ? C34 F21 1.51(3) . ? C1 O1 1.234(12) . ? C1 C2 1.426(15) . ? C1 C8 1.574(14) . ? C2 C3 1.365(14) . ? C2 C11 1.597(15) . ? C3 O2 1.275(13) . ? C3 C4 1.590(17) . ? C4 F2 1.340(19) . ? C4 F1 1.405(16) . ? C4 C5 1.486(18) . ? C5 F3 1.361(15) . ? C5 F4 1.400(14) . ? C5 C6 1.47(2) . ? C6 F6 1.30(2) . ? C6 F5 1.31(2) . ? C6 F7 1.36(2) . ? C7 C8 1.510(18) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.540(18) . ? C8 C12 1.549(19) . ? C9 C10 1.55(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.592(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.49(2) . ? C11 H11 0.9800 . ? C12 C13 1.519(16) . ? C12 C14 1.583(15) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O3 1.283(10) . ? C15 C16 1.373(15) . ? C15 C22 1.606(14) . ? C16 C17 1.385(15) . ? C16 C25 1.527(15) . ? C17 O4 1.229(11) . ? C17 C18 1.519(17) . ? C18 F9 1.399(17) . ? C18 F8 1.47(2) . ? C21 C22 1.369(18) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C26 1.522(18) . ? C22 C23 1.71(3) . ? C23 C24 1.570(18) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.656(17) . ? C24 H1C 0.9700 . ? C24 H1D 0.9700 . ? C25 C26 1.639(16) . ? C25 H25 0.9800 . ? C26 C27 1.34(2) . ? C26 C28 1.622(17) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C29 O5 1.205(18) . ? C29 C30 1.47(2) . ? C29 C36 1.589(16) . ? C30 C31 1.364(14) . ? C30 C39 1.524(16) . ? C31 O6 1.296(12) . ? C31 C32 1.58(2) . ? C32 F15 1.340(18) . ? C32 F16 1.413(17) . ? C32 C33 1.53(2) . ? C33 F18 1.364(16) . ? C33 F17 1.395(17) . ? C35 C36 1.536(19) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.502(16) . ? C36 C40 1.580(18) . ? C37 C38 1.71(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.466(19) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.612(19) . ? C39 H39 0.9800 . ? C40 C42 1.458(18) . ? C40 C41 1.606(18) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.377(18) . ? C43 C48 1.48(2) . ? C43 P1 1.729(15) . ? C44 C45 1.417(16) . ? C44 H44 0.9300 . ? C45 C46 1.381(19) . ? C45 H45 0.9300 . ? C46 C47 1.38(2) . ? C46 H46 0.9300 . ? C47 C48 1.310(17) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.261(16) . ? C49 C54 1.395(13) . ? C49 P1 1.843(10) . ? C50 C51 1.481(19) . ? C50 H50 0.9300 . ? C51 C52 1.34(2) . ? C51 H51 0.9300 . ? C52 C53 1.26(2) . ? C52 H52 0.9300 . ? C53 C54 1.404(17) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C60 1.353(13) . ? C55 C56 1.402(15) . ? C55 P1 1.818(8) . ? C56 C57 1.409(16) . ? C56 H56 0.9300 . ? C57 C58 1.42(2) . ? C57 H57 0.9300 . ? C58 C59 1.29(2) . ? C58 H58 0.9300 . ? C59 C60 1.427(16) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C66 1.365(14) . ? C61 C62 1.435(14) . ? C61 P2 1.793(11) . ? C62 C63 1.368(18) . ? C62 H62 0.9300 . ? C63 C64 1.28(2) . ? C63 H63 0.9300 . ? C64 C65 1.43(2) . ? C64 H64 0.9300 . ? C65 C66 1.374(16) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C72 1.325(15) . ? C67 C68 1.371(15) . ? C67 P2 1.828(9) . ? C68 C69 1.402(16) . ? C68 H68 0.9300 . ? C69 C70 1.32(2) . ? C69 H69 0.9300 . ? C70 C71 1.32(2) . ? C70 H70 0.9300 . ? C71 C72 1.399(16) . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? C73 C74 1.368(18) . ? C73 C78 1.418(18) . ? C73 P2 1.850(13) . ? C74 C75 1.421(16) . ? C74 H74 0.9300 . ? C75 C76 1.346(18) . ? C75 H75 0.9300 . ? C76 C77 1.349(19) . ? C76 H76 0.9300 . ? C77 C78 1.371(18) . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? O1 Yb1 2.419(7) . ? O2 Yb1 2.290(7) . ? O3 Yb1 2.331(6) . ? O4 Yb1 2.338(6) . ? O5 Yb1 2.404(6) . ? O6 Yb1 2.278(6) . ? O11 P1 1.496(6) . ? O11 Yb1 2.279(5) . ? O22 P2 1.479(6) . ? O22 Yb1 2.291(5) . ? F14 C20 1.374(16) . ? F12 C20 1.333(12) . ? F13 C20 1.376(16) . ? 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 F11 C19 F10 104.6(16) . . ? F11 C19 C18 108.6(14) . . ? F10 C19 C18 111.0(12) . . ? F11 C19 C20 121.0(14) . . ? F10 C19 C20 101.9(12) . . ? C18 C19 C20 109.4(13) . . ? F19 C34 F20 117(2) . . ? F19 C34 C33 115.5(16) . . ? F20 C34 C33 111.2(13) . . ? F19 C34 F21 103.9(15) . . ? F20 C34 F21 105.1(19) . . ? C33 C34 F21 102(2) . . ? O1 C1 C2 130.4(9) . . ? O1 C1 C8 123.3(10) . . ? C2 C1 C8 106.1(9) . . ? C3 C2 C1 120.7(10) . . ? C3 C2 C11 134.1(10) . . ? C1 C2 C11 105.1(9) . . ? O2 C3 C2 126.4(10) . . ? O2 C3 C4 113.0(9) . . ? C2 C3 C4 120.3(10) . . ? F2 C4 F1 103.6(12) . . ? F2 C4 C5 106.3(13) . . ? F1 C4 C5 107.8(12) . . ? F2 C4 C3 112.1(11) . . ? F1 C4 C3 107.7(11) . . ? C5 C4 C3 118.4(9) . . ? F3 C5 F4 107.1(10) . . ? F3 C5 C6 114.1(13) . . ? F4 C5 C6 104.2(12) . . ? F3 C5 C4 104.9(11) . . ? F4 C5 C4 106.4(10) . . ? C6 C5 C4 119.4(11) . . ? F6 C6 F5 109.8(16) . . ? F6 C6 F7 104.1(16) . . ? F5 C6 F7 104.9(14) . . ? F6 C6 C5 111.6(13) . . ? F5 C6 C5 116.7(17) . . ? F7 C6 C5 108.7(14) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C8 C9 116.8(11) . . ? C7 C8 C12 121.3(10) . . ? C9 C8 C12 100.5(11) . . ? C7 C8 C1 113.6(10) . . ? C9 C8 C1 103.6(9) . . ? C12 C8 C1 98.2(8) . . ? C8 C9 C10 107.3(11) . . ? C8 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? C8 C9 H9B 110.2 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? C9 C10 C11 99.6(11) . . ? C9 C10 H10A 111.8 . . ? C11 C10 H10A 111.9 . . ? C9 C10 H10B 111.8 . . ? C11 C10 H10B 111.8 . . ? H10A C10 H10B 109.6 . . ? C12 C11 C10 103.3(10) . . ? C12 C11 C2 100.6(10) . . ? C10 C11 C2 102.7(9) . . ? C12 C11 H11 116.0 . . ? C10 C11 H11 116.0 . . ? C2 C11 H11 116.0 . . ? C11 C12 C13 111.1(11) . . ? C11 C12 C8 97.5(8) . . ? C13 C12 C8 114.5(11) . . ? C11 C12 C14 112.4(12) . . ? C13 C12 C14 108.5(10) . . ? C8 C12 C14 112.6(11) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.4 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 129.2(8) . . ? O3 C15 C22 113.2(9) . . ? C16 C15 C22 117.4(8) . . ? C15 C16 C17 121.3(8) . . ? C15 C16 C25 95.5(9) . . ? C17 C16 C25 143.0(10) . . ? O4 C17 C16 128.9(10) . . ? O4 C17 C18 119.3(11) . . ? C16 C17 C18 111.8(9) . . ? F9 C18 C19 106.7(11) . . ? F9 C18 F8 109.6(16) . . ? C19 C18 F8 113.0(16) . . ? F9 C18 C17 107.2(11) . . ? C19 C18 C17 109.5(13) . . ? F8 C18 C17 110.7(11) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 C22 C26 113.5(14) . . ? C21 C22 C15 111.1(11) . . ? C26 C22 C15 97.5(9) . . ? C21 C22 C23 125.1(14) . . ? C26 C22 C23 106.2(11) . . ? C15 C22 C23 99.1(11) . . ? C24 C23 C22 97.5(12) . . ? C24 C23 H23A 112.3 . . ? C22 C23 H23A 112.3 . . ? C24 C23 H23B 112.3 . . ? C22 C23 H23B 112.2 . . ? H23A C23 H23B 109.9 . . ? C23 C24 C25 106.1(14) . . ? C23 C24 H1C 110.5 . . ? C25 C24 H1C 110.5 . . ? C23 C24 H1D 110.5 . . ? C25 C24 H1D 110.5 . . ? H1C C24 H1D 108.7 . . ? C16 C25 C26 109.6(10) . . ? C16 C25 C24 106.3(15) . . ? C26 C25 C24 98.7(16) . . ? C16 C25 H25 113.7 . . ? C26 C25 H25 113.7 . . ? C24 C25 H25 113.7 . . ? C27 C26 C22 120.8(13) . . ? C27 C26 C28 109.2(13) . . ? C22 C26 C28 114.9(12) . . ? C27 C26 C25 105.2(18) . . ? C22 C26 C25 91.3(9) . . ? C28 C26 C25 113.8(12) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O5 C29 C30 131.5(12) . . ? O5 C29 C36 125.7(14) . . ? C30 C29 C36 102.2(12) . . ? C31 C30 C29 118.2(11) . . ? C31 C30 C39 132.6(11) . . ? C29 C30 C39 109.2(10) . . ? O6 C31 C30 125.9(10) . . ? O6 C31 C32 113.4(10) . . ? C30 C31 C32 120.5(11) . . ? F15 C32 F16 110.4(14) . . ? F15 C32 C33 108.3(14) . . ? F16 C32 C33 103.1(13) . . ? F15 C32 C31 110.0(13) . . ? F16 C32 C31 111.7(13) . . ? C33 C32 C31 113.2(13) . . ? F18 C33 F17 108.0(10) . . ? F18 C33 C34 111.2(15) . . ? F17 C33 C34 102.9(16) . . ? F18 C33 C32 106.9(13) . . ? F17 C33 C32 106.4(12) . . ? C34 C33 C32 120.7(13) . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C35 111.2(12) . . ? C37 C36 C40 103.0(12) . . ? C35 C36 C40 118.5(10) . . ? C37 C36 C29 107.5(10) . . ? C35 C36 C29 114.6(12) . . ? C40 C36 C29 100.8(10) . . ? C36 C37 C38 102.0(11) . . ? C36 C37 H37A 111.4 . . ? C38 C37 H37A 111.4 . . ? C36 C37 H37B 111.4 . . ? C38 C37 H37B 111.4 . . ? H37A C37 H37B 109.2 . . ? C39 C38 C37 101.0(10) . . ? C39 C38 H38A 111.6 . . ? C37 C38 H38A 111.6 . . ? C39 C38 H38B 111.6 . . ? C37 C38 H38B 111.6 . . ? H38A C38 H38B 109.4 . . ? C38 C39 C30 108.6(10) . . ? C38 C39 C40 103.2(10) . . ? C30 C39 C40 99.8(9) . . ? C38 C39 H39 114.6 . . ? C30 C39 H39 114.6 . . ? C40 C39 H39 114.6 . . ? C42 C40 C36 116.6(12) . . ? C42 C40 C41 105.7(11) . . ? C36 C40 C41 112.3(11) . . ? C42 C40 C39 114.7(12) . . ? C36 C40 C39 92.5(8) . . ? C41 C40 C39 115.2(11) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 112.6(11) . . ? C44 C43 P1 127.4(11) . . ? C48 C43 P1 119.7(9) . . ? C43 C44 C45 124.7(12) . . ? C43 C44 H44 117.6 . . ? C45 C44 H44 117.6 . . ? C46 C45 C44 117.2(12) . . ? C46 C45 H45 121.4 . . ? C44 C45 H45 121.4 . . ? C45 C46 C47 120.9(12) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 120.6(12) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C43 123.8(11) . . ? C47 C48 H48 118.1 . . ? C43 C48 H48 118.1 . . ? C50 C49 C54 123.3(11) . . ? C50 C49 P1 121.6(9) . . ? C54 C49 P1 115.1(7) . . ? C49 C50 C51 120.2(13) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C52 C51 C50 114.9(13) . . ? C52 C51 H51 122.5 . . ? C50 C51 H51 122.5 . . ? C53 C52 C51 123.3(13) . . ? C53 C52 H52 118.3 . . ? C51 C52 H52 118.3 . . ? C52 C53 C54 123.3(13) . . ? C52 C53 H53 118.4 . . ? C54 C53 H53 118.4 . . ? C49 C54 C53 114.3(10) . . ? C49 C54 H54 122.8 . . ? C53 C54 H54 122.8 . . ? C60 C55 C56 122.9(9) . . ? C60 C55 P1 123.3(7) . . ? C56 C55 P1 113.8(7) . . ? C55 C56 C57 116.4(11) . . ? C55 C56 H56 121.8 . . ? C57 C56 H56 121.8 . . ? C56 C57 C58 119.6(12) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? C59 C58 C57 121.5(12) . . ? C59 C58 H58 119.2 . . ? C57 C58 H58 119.2 . . ? C58 C59 C60 120.4(13) . . ? C58 C59 H59 119.8 . . ? C60 C59 H59 119.8 . . ? C55 C60 C59 118.3(11) . . ? C55 C60 H60 120.8 . . ? C59 C60 H60 120.8 . . ? C66 C61 C62 117.2(11) . . ? C66 C61 P2 121.4(8) . . ? C62 C61 P2 121.3(8) . . ? C63 C62 C61 119.1(11) . . ? C63 C62 H62 120.4 . . ? C61 C62 H62 120.4 . . ? C64 C63 C62 122.6(13) . . ? C64 C63 H63 118.7 . . ? C62 C63 H63 118.7 . . ? C63 C64 C65 121.0(13) . . ? C63 C64 H64 119.5 . . ? C65 C64 H64 119.5 . . ? C66 C65 C64 117.4(13) . . ? C66 C65 H65 121.3 . . ? C64 C65 H65 121.3 . . ? C61 C66 C65 122.4(12) . . ? C61 C66 H66 118.8 . . ? C65 C66 H66 118.8 . . ? C72 C67 C68 120.3(10) . . ? C72 C67 P2 117.5(8) . . ? C68 C67 P2 122.2(8) . . ? C67 C68 C69 118.3(12) . . ? C67 C68 H68 120.9 . . ? C69 C68 H68 120.9 . . ? C70 C69 C68 119.1(13) . . ? C70 C69 H69 120.4 . . ? C68 C69 H69 120.4 . . ? C69 C70 C71 123.7(12) . . ? C69 C70 H70 118.2 . . ? C71 C70 H70 118.2 . . ? C70 C71 C72 117.7(12) . . ? C70 C71 H71 121.2 . . ? C72 C71 H71 121.2 . . ? C67 C72 C71 120.8(11) . . ? C67 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? C74 C73 C78 125.5(12) . . ? C74 C73 P2 120.2(9) . . ? C78 C73 P2 114.2(10) . . ? C73 C74 C75 116.7(12) . . ? C73 C74 H74 121.7 . . ? C75 C74 H74 121.6 . . ? C76 C75 C74 120.0(11) . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C75 C76 C77 119.0(12) . . ? C75 C76 H76 120.5 . . ? C77 C76 H76 120.5 . . ? C76 C77 C78 127.1(12) . . ? C76 C77 H77 116.4 . . ? C78 C77 H77 116.4 . . ? C77 C78 C73 111.3(13) . . ? C77 C78 H78 124.4 . . ? C73 C78 H78 124.4 . . ? C1 O1 Yb1 130.4(6) . . ? C3 O2 Yb1 137.7(6) . . ? C15 O3 Yb1 131.6(6) . . ? C17 O4 Yb1 133.8(7) . . ? C29 O5 Yb1 131.5(8) . . ? C31 O6 Yb1 139.6(6) . . ? P1 O11 Yb1 163.3(4) . . ? P2 O22 Yb1 163.1(4) . . ? O11 P1 C43 113.1(6) . . ? O11 P1 C55 111.2(4) . . ? C43 P1 C55 106.2(5) . . ? O11 P1 C49 113.5(4) . . ? C43 P1 C49 106.1(5) . . ? C55 P1 C49 106.2(4) . . ? O22 P2 C61 112.4(4) . . ? O22 P2 C67 110.4(4) . . ? C61 P2 C67 107.8(5) . . ? O22 P2 C73 112.7(5) . . ? C61 P2 C73 108.3(5) . . ? C67 P2 C73 104.9(5) . . ? O6 Yb1 O11 102.4(3) . . ? O6 Yb1 O2 145.9(2) . . ? O11 Yb1 O2 88.6(3) . . ? O6 Yb1 O22 88.3(3) . . ? O11 Yb1 O22 142.79(18) . . ? O2 Yb1 O22 102.3(3) . . ? O6 Yb1 O3 79.1(3) . . ? O11 Yb1 O3 144.9(2) . . ? O2 Yb1 O3 73.8(2) . . ? O22 Yb1 O3 71.9(2) . . ? O6 Yb1 O4 73.7(2) . . ? O11 Yb1 O4 72.2(2) . . ? O2 Yb1 O4 79.4(2) . . ? O22 Yb1 O4 144.4(2) . . ? O3 Yb1 O4 74.7(2) . . ? O6 Yb1 O5 72.4(2) . . ? O11 Yb1 O5 72.9(2) . . ? O2 Yb1 O5 141.5(2) . . ? O22 Yb1 O5 76.8(2) . . ? O3 Yb1 O5 137.9(2) . . ? O4 Yb1 O5 123.6(2) . . ? O6 Yb1 O1 140.4(2) . . ? O11 Yb1 O1 75.4(2) . . ? O2 Yb1 O1 73.5(2) . . ? O22 Yb1 O1 73.9(3) . . ? O3 Yb1 O1 125.3(3) . . ? O4 Yb1 O1 137.8(2) . . ? O5 Yb1 O1 69.3(2) . . ? F12 C20 F14 96.9(14) . . ? F12 C20 F13 102.2(13) . . ? F14 C20 F13 105.0(14) . . ? F12 C20 C19 122.5(13) . . ? F14 C20 C19 106.6(13) . . ? F13 C20 C19 120.1(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 2.1(16) . . . . ? C8 C1 C2 C3 -172.9(9) . . . . ? O1 C1 C2 C11 180.0(10) . . . . ? C8 C1 C2 C11 5.0(10) . . . . ? C1 C2 C3 O2 -9.7(15) . . . . ? C11 C2 C3 O2 173.1(11) . . . . ? C1 C2 C3 C4 176.4(9) . . . . ? C11 C2 C3 C4 -0.8(17) . . . . ? O2 C3 C4 F2 155.3(12) . . . . ? C2 C3 C4 F2 -30.0(16) . . . . ? O2 C3 C4 F1 42.1(12) . . . . ? C2 C3 C4 F1 -143.3(11) . . . . ? O2 C3 C4 C5 -80.4(12) . . . . ? C2 C3 C4 C5 94.3(12) . . . . ? F2 C4 C5 F3 71.0(13) . . . . ? F1 C4 C5 F3 -178.4(11) . . . . ? C3 C4 C5 F3 -56.0(13) . . . . ? F2 C4 C5 F4 -175.7(11) . . . . ? F1 C4 C5 F4 -65.1(13) . . . . ? C3 C4 C5 F4 57.3(14) . . . . ? F2 C4 C5 C6 -58.3(18) . . . . ? F1 C4 C5 C6 52.3(17) . . . . ? C3 C4 C5 C6 174.7(13) . . . . ? F3 C5 C6 F6 47(2) . . . . ? F4 C5 C6 F6 -69.6(18) . . . . ? C4 C5 C6 F6 171.8(14) . . . . ? F3 C5 C6 F5 174.2(14) . . . . ? F4 C5 C6 F5 57.8(18) . . . . ? C4 C5 C6 F5 -61(2) . . . . ? F3 C5 C6 F7 -67.5(18) . . . . ? F4 C5 C6 F7 176.1(14) . . . . ? C4 C5 C6 F7 58(2) . . . . ? O1 C1 C8 C7 18.8(14) . . . . ? C2 C1 C8 C7 -165.8(10) . . . . ? O1 C1 C8 C9 -108.9(12) . . . . ? C2 C1 C8 C9 66.6(11) . . . . ? O1 C1 C8 C12 148.2(9) . . . . ? C2 C1 C8 C12 -36.3(10) . . . . ? C7 C8 C9 C10 163.4(11) . . . . ? C12 C8 C9 C10 30.1(12) . . . . ? C1 C8 C9 C10 -71.0(12) . . . . ? C8 C9 C10 C11 2.0(13) . . . . ? C9 C10 C11 C12 -35.3(12) . . . . ? C9 C10 C11 C2 69.0(12) . . . . ? C3 C2 C11 C12 -152.8(12) . . . . ? C1 C2 C11 C12 29.7(11) . . . . ? C3 C2 C11 C10 100.9(14) . . . . ? C1 C2 C11 C10 -76.6(12) . . . . ? C10 C11 C12 C13 174.4(10) . . . . ? C2 C11 C12 C13 68.5(11) . . . . ? C10 C11 C12 C8 54.5(11) . . . . ? C2 C11 C12 C8 -51.5(10) . . . . ? C10 C11 C12 C14 -63.8(14) . . . . ? C2 C11 C12 C14 -169.8(11) . . . . ? C7 C8 C12 C11 178.1(10) . . . . ? C9 C8 C12 C11 -51.5(10) . . . . ? C1 C8 C12 C11 54.0(10) . . . . ? C7 C8 C12 C13 60.8(14) . . . . ? C9 C8 C12 C13 -168.8(10) . . . . ? C1 C8 C12 C13 -63.3(12) . . . . ? C7 C8 C12 C14 -63.8(15) . . . . ? C9 C8 C12 C14 66.7(13) . . . . ? C1 C8 C12 C14 172.2(10) . . . . ? O3 C15 C16 C17 -6.6(18) . . . . ? C22 C15 C16 C17 177.7(11) . . . . ? O3 C15 C16 C25 177.1(12) . . . . ? C22 C15 C16 C25 1.4(14) . . . . ? C15 C16 C17 O4 -0.2(19) . . . . ? C25 C16 C17 O4 173.6(16) . . . . ? C15 C16 C17 C18 177.6(11) . . . . ? C25 C16 C17 C18 -9(2) . . . . ? F11 C19 C18 F9 51.3(17) . . . . ? F10 C19 C18 F9 165.7(13) . . . . ? C20 C19 C18 F9 -82.6(15) . . . . ? F11 C19 C18 F8 171.8(15) . . . . ? F10 C19 C18 F8 -73.8(16) . . . . ? C20 C19 C18 F8 37.8(16) . . . . ? F11 C19 C18 C17 -64.3(16) . . . . ? F10 C19 C18 C17 50.0(16) . . . . ? C20 C19 C18 C17 161.7(11) . . . . ? O4 C17 C18 F9 147.3(12) . . . . ? C16 C17 C18 F9 -30.8(16) . . . . ? O4 C17 C18 C19 -97.4(14) . . . . ? C16 C17 C18 C19 84.6(13) . . . . ? O4 C17 C18 F8 28(2) . . . . ? C16 C17 C18 F8 -150.2(15) . . . . ? O3 C15 C22 C21 29.9(17) . . . . ? C16 C15 C22 C21 -153.8(13) . . . . ? O3 C15 C22 C26 148.7(10) . . . . ? C16 C15 C22 C26 -35.0(14) . . . . ? O3 C15 C22 C23 -103.5(12) . . . . ? C16 C15 C22 C23 72.9(13) . . . . ? C21 C22 C23 C24 169.1(18) . . . . ? C26 C22 C23 C24 33.8(18) . . . . ? C15 C22 C23 C24 -66.9(18) . . . . ? C22 C23 C24 C25 7(2) . . . . ? C15 C16 C25 C26 31.7(14) . . . . ? C17 C16 C25 C26 -143.0(16) . . . . ? C15 C16 C25 C24 -74.1(15) . . . . ? C17 C16 C25 C24 111(2) . . . . ? C23 C24 C25 C16 72(2) . . . . ? C23 C24 C25 C26 -41(2) . . . . ? C21 C22 C26 C27 53(2) . . . . ? C15 C22 C26 C27 -64(2) . . . . ? C23 C22 C26 C27 -166.2(19) . . . . ? C21 C22 C26 C28 -81.7(17) . . . . ? C15 C22 C26 C28 161.3(12) . . . . ? C23 C22 C26 C28 59.5(15) . . . . ? C21 C22 C26 C25 161.2(13) . . . . ? C15 C22 C26 C25 44.3(11) . . . . ? C23 C22 C26 C25 -57.6(12) . . . . ? C16 C25 C26 C27 70.0(15) . . . . ? C24 C25 C26 C27 -179.1(13) . . . . ? C16 C25 C26 C22 -52.5(13) . . . . ? C24 C25 C26 C22 58.4(13) . . . . ? C16 C25 C26 C28 -170.5(12) . . . . ? C24 C25 C26 C28 -59.6(15) . . . . ? O5 C29 C30 C31 -5(2) . . . . ? C36 C29 C30 C31 -176.1(9) . . . . ? O5 C29 C30 C39 173.1(16) . . . . ? C36 C29 C30 C39 2.1(13) . . . . ? C29 C30 C31 O6 -2.6(17) . . . . ? C39 C30 C31 O6 179.6(11) . . . . ? C29 C30 C31 C32 171.8(12) . . . . ? C39 C30 C31 C32 -6.0(18) . . . . ? O6 C31 C32 F15 153.6(10) . . . . ? C30 C31 C32 F15 -21.4(16) . . . . ? O6 C31 C32 F16 30.7(16) . . . . ? C30 C31 C32 F16 -144.3(11) . . . . ? O6 C31 C32 C33 -85.1(14) . . . . ? C30 C31 C32 C33 99.9(15) . . . . ? F19 C34 C33 F18 169(2) . . . . ? F20 C34 C33 F18 -55(3) . . . . ? F21 C34 C33 F18 56.7(15) . . . . ? F19 C34 C33 F17 -76(2) . . . . ? F20 C34 C33 F17 61(3) . . . . ? F21 C34 C33 F17 172.2(12) . . . . ? F19 C34 C33 C32 42(3) . . . . ? F20 C34 C33 C32 178.8(19) . . . . ? F21 C34 C33 C32 -70(2) . . . . ? F15 C32 C33 F18 -179.4(12) . . . . ? F16 C32 C33 F18 -62.4(15) . . . . ? C31 C32 C33 F18 58.4(16) . . . . ? F15 C32 C33 F17 65.4(16) . . . . ? F16 C32 C33 F17 -177.6(12) . . . . ? C31 C32 C33 F17 -56.8(15) . . . . ? F15 C32 C33 C34 -51(2) . . . . ? F16 C32 C33 C34 66(2) . . . . ? C31 C32 C33 C34 -173.2(18) . . . . ? O5 C29 C36 C37 -102.0(18) . . . . ? C30 C29 C36 C37 69.7(14) . . . . ? O5 C29 C36 C35 22(2) . . . . ? C30 C29 C36 C35 -166.2(11) . . . . ? O5 C29 C36 C40 150.6(15) . . . . ? C30 C29 C36 C40 -37.7(12) . . . . ? C35 C36 C37 C38 162.6(10) . . . . ? C40 C36 C37 C38 34.6(11) . . . . ? C29 C36 C37 C38 -71.3(14) . . . . ? C36 C37 C38 C39 2.8(13) . . . . ? C37 C38 C39 C30 66.9(12) . . . . ? C37 C38 C39 C40 -38.4(12) . . . . ? C31 C30 C39 C38 103.6(14) . . . . ? C29 C30 C39 C38 -74.4(14) . . . . ? C31 C30 C39 C40 -148.8(11) . . . . ? C29 C30 C39 C40 33.2(12) . . . . ? C37 C36 C40 C42 63.4(15) . . . . ? C35 C36 C40 C42 -59.8(17) . . . . ? C29 C36 C40 C42 174.3(13) . . . . ? C37 C36 C40 C41 -174.5(11) . . . . ? C35 C36 C40 C41 62.3(14) . . . . ? C29 C36 C40 C41 -63.6(13) . . . . ? C37 C36 C40 C39 -55.9(10) . . . . ? C35 C36 C40 C39 -179.1(10) . . . . ? C29 C36 C40 C39 55.0(11) . . . . ? C38 C39 C40 C42 -62.0(15) . . . . ? C30 C39 C40 C42 -173.9(11) . . . . ? C38 C39 C40 C36 58.9(11) . . . . ? C30 C39 C40 C36 -53.0(9) . . . . ? C38 C39 C40 C41 175.0(11) . . . . ? C30 C39 C40 C41 63.1(13) . . . . ? C48 C43 C44 C45 -4.4(17) . . . . ? P1 C43 C44 C45 -177.4(11) . . . . ? C43 C44 C45 C46 3(2) . . . . ? C44 C45 C46 C47 -1(2) . . . . ? C45 C46 C47 C48 0(3) . . . . ? C46 C47 C48 C43 -2(3) . . . . ? C44 C43 C48 C47 3.9(19) . . . . ? P1 C43 C48 C47 177.5(14) . . . . ? C54 C49 C50 C51 1.5(17) . . . . ? P1 C49 C50 C51 -178.9(9) . . . . ? C49 C50 C51 C52 2(2) . . . . ? C50 C51 C52 C53 -8(2) . . . . ? C51 C52 C53 C54 10(2) . . . . ? C50 C49 C54 C53 0.0(14) . . . . ? P1 C49 C54 C53 -179.6(7) . . . . ? C52 C53 C54 C49 -5.9(18) . . . . ? C60 C55 C56 C57 2(2) . . . . ? P1 C55 C56 C57 -179.2(12) . . . . ? C55 C56 C57 C58 -1(3) . . . . ? C56 C57 C58 C59 6(3) . . . . ? C57 C58 C59 C60 -10(3) . . . . ? C56 C55 C60 C59 -6(2) . . . . ? P1 C55 C60 C59 174.7(11) . . . . ? C58 C59 C60 C55 11(3) . . . . ? C66 C61 C62 C63 -2.3(16) . . . . ? P2 C61 C62 C63 -179.7(10) . . . . ? C61 C62 C63 C64 5(2) . . . . ? C62 C63 C64 C65 -7(2) . . . . ? C63 C64 C65 C66 5(2) . . . . ? C62 C61 C66 C65 1.2(16) . . . . ? P2 C61 C66 C65 178.6(9) . . . . ? C64 C65 C66 C61 -2.6(19) . . . . ? C72 C67 C68 C69 -1(2) . . . . ? P2 C67 C68 C69 -178.4(12) . . . . ? C67 C68 C69 C70 -2(3) . . . . ? C68 C69 C70 C71 3(3) . . . . ? C69 C70 C71 C72 0(3) . . . . ? C68 C67 C72 C71 3(2) . . . . ? P2 C67 C72 C71 -179.1(12) . . . . ? C70 C71 C72 C67 -2(2) . . . . ? C78 C73 C74 C75 0.5(19) . . . . ? P2 C73 C74 C75 178.8(9) . . . . ? C73 C74 C75 C76 4.8(19) . . . . ? C74 C75 C76 C77 -8(2) . . . . ? C75 C76 C77 C78 7(3) . . . . ? C76 C77 C78 C73 -2(3) . . . . ? C74 C73 C78 C77 -2(2) . . . . ? P2 C73 C78 C77 179.5(12) . . . . ? C2 C1 O1 Yb1 7.2(15) . . . . ? C8 C1 O1 Yb1 -178.5(7) . . . . ? C2 C3 O2 Yb1 7.8(15) . . . . ? C4 C3 O2 Yb1 -177.9(7) . . . . ? C16 C15 O3 Yb1 9.3(17) . . . . ? C22 C15 O3 Yb1 -174.9(8) . . . . ? C16 C17 O4 Yb1 3.9(18) . . . . ? C18 C17 O4 Yb1 -173.8(8) . . . . ? C30 C29 O5 Yb1 14(2) . . . . ? C36 C29 O5 Yb1 -177.1(8) . . . . ? C30 C31 O6 Yb1 0.6(18) . . . . ? C32 C31 O6 Yb1 -174.1(8) . . . . ? Yb1 O11 P1 C43 103.9(15) . . . . ? Yb1 O11 P1 C55 -136.7(14) . . . . ? Yb1 O11 P1 C49 -17.1(16) . . . . ? C44 C43 P1 O11 -156.6(9) . . . . ? C48 C43 P1 O11 30.9(10) . . . . ? C44 C43 P1 C55 81.1(11) . . . . ? C48 C43 P1 C55 -91.4(9) . . . . ? C44 C43 P1 C49 -31.6(11) . . . . ? C48 C43 P1 C49 155.9(8) . . . . ? C60 C55 P1 O11 -135.6(10) . . . . ? C56 C55 P1 O11 45.3(11) . . . . ? C60 C55 P1 C43 -12.1(12) . . . . ? C56 C55 P1 C43 168.7(10) . . . . ? C60 C55 P1 C49 100.6(10) . . . . ? C56 C55 P1 C49 -78.6(10) . . . . ? C50 C49 P1 O11 -145.8(8) . . . . ? C54 C49 P1 O11 33.8(8) . . . . ? C50 C49 P1 C43 89.4(10) . . . . ? C54 C49 P1 C43 -91.0(7) . . . . ? C50 C49 P1 C55 -23.4(9) . . . . ? C54 C49 P1 C55 156.2(7) . . . . ? Yb1 O22 P2 C61 -16.0(16) . . . . ? Yb1 O22 P2 C67 -136.4(14) . . . . ? Yb1 O22 P2 C73 106.7(15) . . . . ? C66 C61 P2 O22 34.6(10) . . . . ? C62 C61 P2 O22 -148.1(8) . . . . ? C66 C61 P2 C67 156.4(8) . . . . ? C62 C61 P2 C67 -26.3(10) . . . . ? C66 C61 P2 C73 -90.6(9) . . . . ? C62 C61 P2 C73 86.8(9) . . . . ? C72 C67 P2 O22 45.2(11) . . . . ? C68 C67 P2 O22 -136.9(10) . . . . ? C72 C67 P2 C61 -77.9(10) . . . . ? C68 C67 P2 C61 100.0(10) . . . . ? C72 C67 P2 C73 166.8(10) . . . . ? C68 C67 P2 C73 -15.3(11) . . . . ? C74 C73 P2 O22 -154.7(9) . . . . ? C78 C73 P2 O22 23.8(10) . . . . ? C74 C73 P2 C61 -29.8(10) . . . . ? C78 C73 P2 C61 148.8(9) . . . . ? C74 C73 P2 C67 85.1(10) . . . . ? C78 C73 P2 C67 -96.3(10) . . . . ? C31 O6 Yb1 O11 71.4(10) . . . . ? C31 O6 Yb1 O2 177.7(9) . . . . ? C31 O6 Yb1 O22 -72.6(10) . . . . ? C31 O6 Yb1 O3 -144.5(11) . . . . ? C31 O6 Yb1 O4 138.4(11) . . . . ? C31 O6 Yb1 O5 4.1(10) . . . . ? C31 O6 Yb1 O1 -10.7(12) . . . . ? P1 O11 Yb1 O6 10.1(16) . . . . ? P1 O11 Yb1 O2 -137.3(15) . . . . ? P1 O11 Yb1 O22 113.9(13) . . . . ? P1 O11 Yb1 O3 -78.6(16) . . . . ? P1 O11 Yb1 O4 -58.0(15) . . . . ? P1 O11 Yb1 O5 77.0(15) . . . . ? P1 O11 Yb1 O1 149.4(16) . . . . ? C3 O2 Yb1 O6 174.3(7) . . . . ? C3 O2 Yb1 O11 -75.4(9) . . . . ? C3 O2 Yb1 O22 68.7(9) . . . . ? C3 O2 Yb1 O3 135.4(9) . . . . ? C3 O2 Yb1 O4 -147.6(9) . . . . ? C3 O2 Yb1 O5 -15.6(11) . . . . ? C3 O2 Yb1 O1 -0.2(8) . . . . ? P2 O22 Yb1 O6 -138.2(15) . . . . ? P2 O22 Yb1 O11 113.4(13) . . . . ? P2 O22 Yb1 O2 9.0(16) . . . . ? P2 O22 Yb1 O3 -59.1(15) . . . . ? P2 O22 Yb1 O4 -79.9(17) . . . . ? P2 O22 Yb1 O5 149.5(16) . . . . ? P2 O22 Yb1 O1 77.6(15) . . . . ? C15 O3 Yb1 O6 -80.3(9) . . . . ? C15 O3 Yb1 O11 15.9(11) . . . . ? C15 O3 Yb1 O2 78.7(9) . . . . ? C15 O3 Yb1 O22 -172.1(9) . . . . ? C15 O3 Yb1 O4 -4.4(9) . . . . ? C15 O3 Yb1 O5 -128.1(8) . . . . ? C15 O3 Yb1 O1 134.0(8) . . . . ? C17 O4 Yb1 O6 81.2(10) . . . . ? C17 O4 Yb1 O11 -169.5(10) . . . . ? C17 O4 Yb1 O2 -77.6(10) . . . . ? C17 O4 Yb1 O22 18.8(12) . . . . ? C17 O4 Yb1 O3 -1.7(10) . . . . ? C17 O4 Yb1 O5 136.2(10) . . . . ? C17 O4 Yb1 O1 -127.9(9) . . . . ? C29 O5 Yb1 O6 -10.5(12) . . . . ? C29 O5 Yb1 O11 -120.0(12) . . . . ? C29 O5 Yb1 O2 175.3(12) . . . . ? C29 O5 Yb1 O22 81.9(12) . . . . ? C29 O5 Yb1 O3 39.3(13) . . . . ? C29 O5 Yb1 O4 -66.0(12) . . . . ? C29 O5 Yb1 O1 159.5(12) . . . . ? C1 O1 Yb1 O6 178.1(7) . . . . ? C1 O1 Yb1 O11 86.1(8) . . . . ? C1 O1 Yb1 O2 -6.8(8) . . . . ? C1 O1 Yb1 O22 -115.3(8) . . . . ? C1 O1 Yb1 O3 -62.2(9) . . . . ? C1 O1 Yb1 O4 45.3(10) . . . . ? C1 O1 Yb1 O5 163.0(8) . . . . ? F11 C19 C20 F12 -164.4(19) . . . . ? F10 C19 C20 F12 80(2) . . . . ? C18 C19 C20 F12 -37(2) . . . . ? F11 C19 C20 F14 -55(2) . . . . ? F10 C19 C20 F14 -169.8(17) . . . . ? C18 C19 C20 F14 72.7(18) . . . . ? F11 C19 C20 F13 65(2) . . . . ? F10 C19 C20 F13 -51(2) . . . . ? C18 C19 C20 F13 -168.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.308 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.141