# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Massi, Massimiliano' _publ_contact_author_email m.massi@curtin.edu.au _publ_section_title ; Multifunctional Hybrid Materials Based on Transparent Poly(methyl methacrylate) Reinforced by Lanthanoid Hydroxo Clusters ; loop_ _publ_author_name M.Massi D.Brown P.Andrews B.Fraser N.Gorham P.Junk ; T.St Pierre ; B.Skelton R.Woodward #===END # Attachment '- mxm14.cif' data_mxm14 _database_code_depnum_ccdc_archive 'CCDC 779681' #TrackingRef '- mxm14.cif' _audit_creation_date 2010-06-03T12:08:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C238 H227 Eu5 O45' _chemical_formula_moiety 'C210 H195 Eu5 O45, 4(C7 H8)' _chemical_formula_weight 4567 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall -C_2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.8542(9) _cell_length_b 17.7867(4) _cell_length_c 32.6504(5) _cell_angle_alpha 90 _cell_angle_beta 95.338(2) _cell_angle_gamma 90 _cell_volume 20731.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 41139 _cell_measurement_theta_min 3.4535 _cell_measurement_theta_max 34.4527 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9320 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0678 -1 0 0 0.0173 -1 -1 0 0.0449 -1 1 0 0.0209 -44 -1 26 0.0958 0 0 -1 0.9596 9 19 28 0.1673 -10 -24 14 0.1037 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.569 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.909 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0196682157 _diffrn_orient_matrix_ub_12 0.0034762048 _diffrn_orient_matrix_ub_13 0.000366313 _diffrn_orient_matrix_ub_21 -0.0019213087 _diffrn_orient_matrix_ub_22 -0.0395130842 _diffrn_orient_matrix_ub_23 -0.0020355398 _diffrn_orient_matrix_ub_31 0.0020351749 _diffrn_orient_matrix_ub_32 -0.0037615639 _diffrn_orient_matrix_ub_33 0.0217326655 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_unetI/netI 0.0887 _diffrn_reflns_number 192070 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 34.56 _diffrn_reflns_theta_full 33.75 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.954 _reflns_number_total 42124 _reflns_number_gt 24086 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. The terminal groups on many of the long chains were modelled as being disordered over two sets of sites with all occupancies refined to 0.589(2) and its complement after trial refinement found these to be not significantly different, except for C(28),C(29) and C(28'),C(29') where occupancies refined to 0.846(7) and its complement. Geometries of the disordered atoms were restrained to ideal values with ADP's also restrained. Geometries of the two toluene solvent molecules were restrained to ideal values. ; _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^)+(0.0559P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 42124 _refine_ls_number_parameters 1561 _refine_ls_number_restraints 565 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.989 _refine_diff_density_min -2.485 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Eu1 Eu 0.011894(4) 0.945839(7) 0.330144(3) 0.01803(3) Uani 1 1 d . . . Eu2 Eu 0.069088(3) 0.943575(7) 0.245114(4) 0.01867(3) Uani 1 1 d . . . Eu3 Eu 0 1.112234(10) 0.25 0.01878(4) Uani 1 2 d S . . O1 O 0 0.92109(14) 0.25 0.0184(5) Uani 1 2 d SD . . H1O H 0 0.8757 0.25 0.022 Uiso 1 1 calc R . . O2 O 0.04531(5) 1.03048(10) 0.29030(5) 0.0194(4) Uani 1 1 d . B . H2O H 0.0653 1.0591 0.3071 0.023 Uiso 1 1 calc R . . O3 O -0.03123(5) 1.03089(10) 0.29651(5) 0.0195(4) Uani 1 1 d . . . H3O H -0.0458 1.0596 0.316 0.023 Uiso 1 1 calc R . . C1 C 0.17163(8) 0.90667(19) 0.27523(9) 0.0346(7) Uani 1 1 d . . . H1 H 0.198 0.8995 0.2796 0.041 Uiso 1 1 calc R . . C10 C 0.15686(8) 0.97823(19) 0.28349(9) 0.0334(7) Uani 1 1 d D . . O10 O 0.12197(5) 0.99411(12) 0.28043(6) 0.0314(5) Uani 1 1 d D . . C11 C 0.18233(8) 1.04008(19) 0.29938(10) 0.0379(8) Uani 1 1 d D . . C12 C 0.16834(10) 1.0966(2) 0.32288(14) 0.0679(13) Uani 1 1 d D . . H12 H 0.1428 1.0953 0.3285 0.081 Uiso 1 1 calc R . . C13 C 0.19111(11) 1.1548(3) 0.33831(15) 0.0803(15) Uani 1 1 d D . . H13 H 0.1814 1.1918 0.3554 0.096 Uiso 1 1 calc R . . C14 C 0.22789(10) 1.1592(2) 0.32893(11) 0.0529(10) Uani 1 1 d D . . O14 O 0.24780(7) 1.22013(17) 0.34474(8) 0.0654(8) Uani 1 1 d D . . C15 C 0.24216(9) 1.1044(2) 0.30519(10) 0.0445(9) Uani 1 1 d D . . H15 H 0.2674 1.1073 0.2985 0.053 Uiso 1 1 calc R . . C16 C 0.21959(9) 1.0449(2) 0.29101(11) 0.0413(8) Uani 1 1 d D . . H16 H 0.2298 1.0065 0.2752 0.05 Uiso 1 1 calc R . . C17 C 0.28375(10) 1.2328(2) 0.33138(12) 0.0524(10) Uani 1 1 d . . . H17A H 0.282 1.2357 0.301 0.063 Uiso 1 1 calc R . . H17B H 0.3007 1.1908 0.3403 0.063 Uiso 1 1 calc R . . C18 C 0.29860(12) 1.3038(2) 0.34930(14) 0.0616(12) Uani 1 1 d . . . H18 H 0.3227 1.319 0.3426 0.074 Uiso 1 1 calc R . . C19 C 0.28165(14) 1.3478(3) 0.37353(17) 0.0892(17) Uani 1 1 d . . . H19A H 0.2575 1.3349 0.381 0.107 Uiso 1 1 calc R . . H19B H 0.2934 1.3928 0.3837 0.107 Uiso 1 1 calc R . . C20 C 0.14931(8) 0.84579(17) 0.26090(8) 0.0280(6) Uani 1 1 d . . . O20 O 0.11501(5) 0.85062(11) 0.24757(5) 0.0263(4) Uani 1 1 d . . . C21 C 0.16529(8) 0.76830(19) 0.26115(9) 0.0329(7) Uani 1 1 d . . . C22 C 0.14534(9) 0.71156(18) 0.23858(9) 0.0340(7) Uani 1 1 d . . . H22 H 0.1233 0.7245 0.2216 0.041 Uiso 1 1 calc R . . C23 C 0.15686(10) 0.6376(2) 0.24034(10) 0.0433(8) Uani 1 1 d . . . H23 H 0.1429 0.6004 0.2246 0.052 Uiso 1 1 calc R . . C24 C 0.18865(11) 0.6178(2) 0.26502(11) 0.0483(9) Uani 1 1 d . . . O24 O 0.20130(8) 0.54537(16) 0.26913(9) 0.0619(8) Uani 1 1 d U A . C25 C 0.20940(10) 0.6724(2) 0.28707(11) 0.0503(9) Uani 1 1 d U . . H25 H 0.2316 0.6588 0.3036 0.06 Uiso 1 1 calc R . . C26 C 0.19797(9) 0.7470(2) 0.28510(10) 0.0426(8) Uani 1 1 d U . . H26 H 0.2125 0.7841 0.3002 0.051 Uiso 1 1 calc R . . C27 C 0.17867(18) 0.4847(3) 0.25045(19) 0.1010(17) Uani 1 1 d DU . . H27A H 0.1765 0.4897 0.2201 0.121 Uiso 0.846(7) 1 calc PRD A 1 H27B H 0.1532 0.4865 0.2598 0.121 Uiso 0.846(7) 1 calc PR A 1 H27C H 0.175 0.4991 0.2211 0.121 Uiso 0.154(7) 1 calc PRD A 2 H27D H 0.154 0.4923 0.2611 0.121 Uiso 0.154(7) 1 calc PR A 2 C28 C 0.1978(3) 0.4090(4) 0.2634(3) 0.112(2) Uani 0.846(7) 1 d PDU A 1 H28 H 0.184 0.3637 0.259 0.134 Uiso 0.846(7) 1 calc PR A 1 C29 C 0.2280(3) 0.4061(5) 0.2779(3) 0.141(3) Uani 0.846(7) 1 d PDU A 1 H29A H 0.2422 0.4509 0.2825 0.211 Uiso 0.846(7) 1 calc PR A 1 H29B H 0.2389 0.3588 0.2855 0.211 Uiso 0.846(7) 1 calc PR A 1 C28' C 0.1825(14) 0.4017(10) 0.2491(11) 0.107(7) Uiso 0.154(7) 1 d PDU A 2 H28' H 0.1821 0.3841 0.2216 0.128 Uiso 0.154(7) 1 calc PR A 2 C29' C 0.1859(7) 0.3488(14) 0.2741(7) 0.048(6) Uiso 0.154(7) 1 d PDU A 2 H29C H 0.1867 0.3585 0.3027 0.072 Uiso 0.154(7) 1 calc PR A 2 H29D H 0.1879 0.2987 0.2644 0.072 Uiso 0.154(7) 1 calc PR A 2 C2 C 0.10445(9) 0.85366(17) 0.35535(9) 0.0301(6) Uani 1 1 d . . . H2 H 0.1243 0.8232 0.3673 0.036 Uiso 1 1 calc R . . C30 C 0.10207(8) 0.92916(17) 0.36997(8) 0.0276(6) Uani 1 1 d . . . O30 O 0.07278(6) 0.96771(11) 0.36556(5) 0.0258(4) Uani 1 1 d . . . C31 C 0.13563(8) 0.96411(17) 0.39296(9) 0.0314(7) Uani 1 1 d . . . C32 C 0.13140(9) 1.02757(18) 0.41712(9) 0.0345(7) Uani 1 1 d . . . H32 H 0.107 1.0469 0.4192 0.041 Uiso 1 1 calc R . . C33 C 0.16163(10) 1.0632(2) 0.43809(11) 0.0458(9) Uani 1 1 d . . . H33 H 0.158 1.1055 0.455 0.055 Uiso 1 1 calc R . . C34 C 0.19725(11) 1.0364(2) 0.43412(12) 0.0538(10) Uani 1 1 d . . . O34 O 0.22971(8) 1.06589(17) 0.45408(10) 0.0738(10) Uani 1 1 d . . . C35 C 0.20247(10) 0.9750(2) 0.40944(12) 0.0550(11) Uani 1 1 d . . . H35 H 0.2271 0.9574 0.4065 0.066 Uiso 1 1 calc R . . C36 C 0.17217(9) 0.9391(2) 0.38907(11) 0.0424(8) Uani 1 1 d . . . H36 H 0.1761 0.8969 0.3722 0.051 Uiso 1 1 calc R . . C37 C 0.22853(13) 1.1371(3) 0.47524(15) 0.0773(15) Uani 1 1 d . . . H37A H 0.2515 1.1427 0.4943 0.093 Uiso 1 1 calc R . . H37B H 0.2067 1.1378 0.4917 0.093 Uiso 1 1 calc R . . C38 C 0.22569(13) 1.2015(3) 0.44574(16) 0.0728(14) Uani 1 1 d . . . H38 H 0.2411 1.2008 0.4236 0.087 Uiso 1 1 calc R . . C39 C 0.20319(13) 1.2591(3) 0.44864(16) 0.0744(14) Uani 1 1 d . . . H39A H 0.1874 1.2614 0.4705 0.089 Uiso 1 1 calc R . . H39B H 0.2026 1.2984 0.4289 0.089 Uiso 1 1 calc R . . C40 C 0.08001(8) 0.82207(15) 0.32517(8) 0.0235(6) Uani 1 1 d . . . O40 O 0.05452(5) 0.86110(10) 0.30326(5) 0.0219(4) Uani 1 1 d . . . C41 C 0.08095(8) 0.74033(16) 0.31470(8) 0.0277(6) Uani 1 1 d . . . C42 C 0.06205(8) 0.71508(17) 0.27814(9) 0.0301(6) Uani 1 1 d . . . H42 H 0.0493 0.7505 0.2601 0.036 Uiso 1 1 calc R . . C43 C 0.06126(9) 0.63973(18) 0.26736(10) 0.0374(8) Uani 1 1 d . . . H43 H 0.0483 0.6241 0.2421 0.045 Uiso 1 1 calc R . . C44 C 0.07944(10) 0.58723(19) 0.29352(11) 0.0437(9) Uani 1 1 d . . . O44 O 0.07984(8) 0.51165(14) 0.28555(9) 0.0632(8) Uani 1 1 d . B . C45 C 0.09892(11) 0.61151(19) 0.33016(11) 0.0475(9) Uani 1 1 d . . . H45 H 0.1117 0.576 0.3481 0.057 Uiso 1 1 calc R . . C46 C 0.09969(10) 0.68669(18) 0.34048(10) 0.0410(8) Uani 1 1 d . . . H46 H 0.1131 0.7024 0.3655 0.049 Uiso 1 1 calc R . . C47 C 0.05966(17) 0.4846(2) 0.25009(16) 0.0857(16) Uani 1 1 d DU . . H47A H 0.0698 0.5064 0.2255 0.103 Uiso 0.5890(17) 1 calc PR B 1 H47B H 0.0331 0.4999 0.2499 0.103 Uiso 0.5890(17) 1 calc PR B 1 H47C H 0.064 0.5181 0.2267 0.103 Uiso 0.4110(17) 1 d PR B 2 H47D H 0.0323 0.4845 0.2533 0.103 Uiso 0.4110(17) 1 d PR B 2 C48 C 0.0623(4) 0.4004(6) 0.2488(6) 0.1060(19) Uani 0.5890(17) 1 d PDU B 1 H48 H 0.0523 0.3776 0.2239 0.127 Uiso 0.5890(17) 1 calc PR B 1 C49 C 0.0765(3) 0.3546(5) 0.2770(3) 0.096(3) Uani 0.5890(17) 1 d PDU B 1 H49A H 0.0871 0.3736 0.3027 0.115 Uiso 0.5890(17) 1 calc PR B 1 H49B H 0.0764 0.302 0.272 0.115 Uiso 0.5890(17) 1 calc PR B 1 C48' C 0.0595(6) 0.4021(8) 0.2491(9) 0.1060(19) Uani 0.4110(17) 1 d PDU B 2 H48' H 0.0828 0.3768 0.2541 0.127 Uiso 0.4110(17) 1 calc PR B 2 C49' C 0.0305(5) 0.3630(8) 0.2421(6) 0.143(5) Uani 0.4110(17) 1 d PDU B 2 H49C H 0.0068 0.3866 0.2369 0.172 Uiso 0.4110(17) 1 calc PR B 2 H49D H 0.0323 0.3097 0.2418 0.172 Uiso 0.4110(17) 1 calc PR B 2 C3 C -0.01296(9) 0.91057(17) 0.43863(8) 0.0300(7) Uani 1 1 d . . . H3 H -0.0191 0.9019 0.4659 0.036 Uiso 1 1 calc R . . C50 C -0.02510(7) 0.97839(16) 0.41952(8) 0.0238(6) Uani 1 1 d . . . O50 O -0.01740(5) 0.99774(11) 0.38389(5) 0.0249(4) Uani 1 1 d . . . C51 C -0.04932(8) 1.03144(17) 0.44076(8) 0.0282(6) Uani 1 1 d . . . C52 C -0.06705(9) 1.0894(2) 0.41805(9) 0.0375(8) Uani 1 1 d . . . H52 H -0.0627 1.0954 0.39 0.045 Uiso 1 1 calc R . . C53 C -0.09097(11) 1.1388(2) 0.43558(11) 0.0512(10) Uani 1 1 d . . . H53 H -0.103 1.1777 0.4194 0.061 Uiso 1 1 calc R . . C54 C -0.09732(10) 1.1318(2) 0.47654(10) 0.0470(9) Uani 1 1 d . . . O54 O -0.12124(9) 1.18594(19) 0.49092(8) 0.0722(9) Uani 1 1 d . . . C55 C -0.08035(10) 1.0745(2) 0.49962(10) 0.0407(8) Uani 1 1 d . . . H55 H -0.0848 1.0691 0.5277 0.049 Uiso 1 1 calc R . . C56 C -0.05663(9) 1.02456(19) 0.48206(9) 0.0337(7) Uani 1 1 d . . . H56 H -0.0452 0.9851 0.4983 0.04 Uiso 1 1 calc R . . C57 C -0.12443(12) 1.1885(3) 0.53362(12) 0.0628(12) Uani 1 1 d . B . H57A H -0.0993 1.1912 0.5489 0.075 Uiso 1 1 calc R . . H57B H -0.1373 1.1429 0.5425 0.075 Uiso 1 1 calc R . . C58 C -0.14690(17) 1.2579(4) 0.54166(17) 0.1015(19) Uani 1 1 d DU . . H58 H -0.1406 1.302 0.5275 0.122 Uiso 0.5890(17) 1 calc PR B 1 H58' H -0.1721 1.2436 0.5331 0.122 Uiso 0.4110(17) 1 d PR B 2 C59 C -0.1727(2) 1.2648(6) 0.5645(2) 0.083(3) Uani 0.5890(17) 1 d PDU B 1 H59A H -0.179 1.3131 0.5741 0.099 Uiso 0.5890(17) 1 calc PR B 1 H59B H -0.186 1.2217 0.5723 0.099 Uiso 0.5890(17) 1 calc PR B 1 C59' C -0.1504(5) 1.3162(8) 0.5497(5) 0.101(4) Uani 0.4110(17) 1 d PDU B 2 H59C H -0.1691 1.3301 0.5671 0.121 Uiso 0.4110(17) 1 calc PR B 2 H59D H -0.1348 1.3535 0.5395 0.121 Uiso 0.4110(17) 1 calc PR B 2 C60 C 0.00742(8) 0.85527(16) 0.42021(8) 0.0260(6) Uani 1 1 d . . . O60 O 0.01587(6) 0.85817(11) 0.38325(5) 0.0274(4) Uani 1 1 d . . . C61 C 0.02033(10) 0.78636(18) 0.44379(9) 0.0347(7) Uani 1 1 d U . . C62 C 0.03360(10) 0.72611(18) 0.42308(10) 0.0398(8) Uani 1 1 d U . . H62 H 0.0352 0.73 0.3943 0.048 Uiso 1 1 calc R . . C63 C 0.04462(12) 0.6600(2) 0.44301(12) 0.0524(10) Uani 1 1 d U . . H63 H 0.0533 0.6187 0.428 0.063 Uiso 1 1 calc R . . C64 C 0.04279(16) 0.6548(2) 0.48494(13) 0.0743(14) Uani 1 1 d U . . C65 C 0.03208(17) 0.7160(2) 0.50668(12) 0.0800(16) Uani 1 1 d U . . H65 H 0.0327 0.7136 0.5358 0.096 Uiso 1 1 calc R . . C66 C 0.02056(14) 0.7805(2) 0.48644(10) 0.0580(11) Uani 1 1 d U . . H66 H 0.0126 0.822 0.5017 0.07 Uiso 1 1 calc R . . O64 O 0.05135(13) 0.59102(18) 0.50764(11) 0.1030(13) Uani 1 1 d U . . C67 C 0.05817(18) 0.5255(3) 0.48735(18) 0.0926(16) Uani 1 1 d U . . H67A H 0.0822 0.5283 0.4747 0.111 Uiso 1 1 calc R . . H67B H 0.0377 0.5144 0.4657 0.111 Uiso 1 1 calc R . . C68 C 0.05997(16) 0.4656(3) 0.52205(19) 0.0910(16) Uani 1 1 d DU . . H68 H 0.0743 0.4755 0.5475 0.109 Uiso 1 1 calc R . . C69 C 0.04308(15) 0.4051(3) 0.5171(2) 0.0937(17) Uani 1 1 d DU . . H69A H 0.0287 0.3947 0.4918 0.112 Uiso 1 1 calc R . . H69B H 0.0445 0.369 0.5386 0.112 Uiso 1 1 calc R . . C4 C 0.0863(2) 1.2018(4) 0.3005(2) 0.0357(19) Uani 0.4110(17) 1 d P B 1 H4 H 0.11 1.2135 0.3147 0.043 Uiso 0.4110(17) 1 calc PR B 1 C70 C 0.0551(2) 1.1915(4) 0.32294(18) 0.0312(17) Uani 0.4110(17) 1 d PD B 1 O70 O 0.0212(3) 1.1790(5) 0.3091(2) 0.0261(5) Uani 0.4110(17) 1 d PD B 1 C71 C 0.0608(2) 1.1916(4) 0.3695(2) 0.030(2) Uani 0.4110(17) 1 d PD B 1 C72 C 0.0375(2) 1.1471(4) 0.39103(17) 0.0297(16) Uani 0.4110(17) 1 d PD B 1 H72 H 0.0175 1.1203 0.3764 0.036 Uiso 0.4110(17) 1 calc PR B 1 C73 C 0.0427(2) 1.1413(4) 0.4330(2) 0.0340(17) Uani 0.4110(17) 1 d PD B 1 H73 H 0.026 1.1113 0.4469 0.041 Uiso 0.4110(17) 1 calc PR B 1 C74 C 0.0721(2) 1.1781(4) 0.45581(19) 0.0326(18) Uani 0.4110(17) 1 d PD B 1 O74 O 0.07473(17) 1.1665(3) 0.49740(13) 0.0446(15) Uani 0.4110(17) 1 d PD B 1 C75 C 0.0948(3) 1.2238(5) 0.4350(2) 0.037(2) Uani 0.4110(17) 1 d PD B 1 H75 H 0.1144 1.2512 0.4498 0.045 Uiso 0.4110(17) 1 calc PR B 1 C76 C 0.0892(3) 1.2304(5) 0.3921(2) 0.039(2) Uani 0.4110(17) 1 d PD B 1 H76 H 0.1053 1.262 0.3782 0.047 Uiso 0.4110(17) 1 calc PR B 1 C77 C 0.0855(3) 1.2256(5) 0.5242(3) 0.045(2) Uani 0.4110(17) 1 d PD B 1 H77A H 0.072 1.2211 0.5491 0.054 Uiso 0.4110(17) 1 calc PR B 1 H77B H 0.0781 1.2738 0.5106 0.054 Uiso 0.4110(17) 1 calc PR B 1 C78 C 0.1273(3) 1.2272(7) 0.5368(3) 0.053(3) Uani 0.4110(17) 1 d PD B 1 H78 H 0.1398 1.1803 0.5407 0.064 Uiso 0.4110(17) 1 calc PR B 1 C79 C 0.1469(4) 1.2867(8) 0.5427(3) 0.075(4) Uani 0.4110(17) 1 d PD B 1 H79A H 0.1354 1.3347 0.5391 0.09 Uiso 0.4110(17) 1 calc PR B 1 H79B H 0.173 1.2831 0.5506 0.09 Uiso 0.4110(17) 1 calc PR B 1 C80 C 0.08304(18) 1.1948(3) 0.25684(18) 0.0243(14) Uani 0.4110(17) 1 d PD B 1 O80 O 0.0532(2) 1.1787(4) 0.2348(2) 0.0280(7) Uani 0.4110(17) 1 d PD B 1 C81 C 0.11654(18) 1.2110(4) 0.2345(2) 0.0308(16) Uani 0.4110(17) 1 d PD B 1 C82 C 0.1122(3) 1.2215(7) 0.1923(2) 0.048(3) Uani 0.4110(17) 1 d PD B 1 H82 H 0.0877 1.2181 0.1785 0.058 Uiso 0.4110(17) 1 calc PR B 1 C83 C 0.1417(2) 1.2365(5) 0.1691(2) 0.042(2) Uani 0.4110(17) 1 d PD B 1 H83 H 0.1375 1.2449 0.1404 0.051 Uiso 0.4110(17) 1 calc PR B 1 C84 C 0.1771(2) 1.2389(7) 0.1888(2) 0.046(3) Uani 0.4110(17) 1 d PD B 1 O84 O 0.2073(2) 1.2593(5) 0.1688(3) 0.068(3) Uani 0.4110(17) 1 d PD B 1 C85 C 0.1826(2) 1.2263(7) 0.2307(2) 0.074(4) Uani 0.4110(17) 1 d PD B 1 H85 H 0.2073 1.2264 0.2441 0.089 Uiso 0.4110(17) 1 calc PR B 1 C86 C 0.1531(2) 1.2139(6) 0.2527(2) 0.063(3) Uani 0.4110(17) 1 d PD B 1 H86 H 0.1576 1.2069 0.2816 0.076 Uiso 0.4110(17) 1 calc PR B 1 C87 C 0.2037(3) 1.2778(6) 0.1266(3) 0.051(3) Uani 0.4110(17) 1 d PD B 1 H87A H 0.1844 1.317 0.1206 0.062 Uiso 0.4110(17) 1 calc PR B 1 H87B H 0.1968 1.2329 0.1096 0.062 Uiso 0.4110(17) 1 calc PR B 1 C88 C 0.2403(3) 1.3053(8) 0.1186(4) 0.068(4) Uani 0.4110(17) 1 d PD B 1 H88 H 0.2473 1.3542 0.1281 0.081 Uiso 0.4110(17) 1 calc PR B 1 C89 C 0.2635(3) 1.2683(8) 0.0997(4) 0.090(4) Uani 0.4110(17) 1 d PD B 1 H89A H 0.2573 1.2192 0.0898 0.108 Uiso 0.4110(17) 1 calc PR B 1 H89B H 0.2871 1.2896 0.0954 0.108 Uiso 0.4110(17) 1 calc PR B 1 C5 C 0.09324(8) 0.86496(16) 0.14587(8) 0.0245(6) Uani 1 1 d . . . H5 H 0.1039 0.838 0.1247 0.029 Uiso 1 1 calc R . . C90 C 0.10827(8) 0.93753(16) 0.15638(8) 0.0261(6) Uani 1 1 d . . . O90 O 0.10113(5) 0.97420(11) 0.18757(6) 0.0266(4) Uani 1 1 d . . . C91 C 0.13539(8) 0.97294(17) 0.13031(8) 0.0267(6) Uani 1 1 d . . . C92 C 0.13527(9) 0.95923(18) 0.08856(9) 0.0323(7) Uani 1 1 d . . . H92 H 0.1184 0.9232 0.0759 0.039 Uiso 1 1 calc R . . C93 C 0.15950(9) 0.9976(2) 0.06487(10) 0.0422(8) Uani 1 1 d . . . H93 H 0.1589 0.9884 0.0362 0.051 Uiso 1 1 calc R . . C94 C 0.18424(11) 1.0488(2) 0.08368(11) 0.0480(9) Uani 1 1 d . . . O94 O 0.20897(8) 1.09143(19) 0.06383(8) 0.0699(9) Uani 1 1 d . . . C95 C 0.18521(11) 1.0624(2) 0.12558(12) 0.0486(9) Uani 1 1 d . . . H95 H 0.2028 1.0969 0.1384 0.058 Uiso 1 1 calc R . . C96 C 0.16043(9) 1.02541(19) 0.14852(10) 0.0359(7) Uani 1 1 d . . . H96 H 0.1605 1.036 0.1771 0.043 Uiso 1 1 calc R . . C97 C 0.20896(13) 1.0817(3) 0.02029(13) 0.0832(16) Uani 1 1 d . . . H97A H 0.184 1.0919 0.0058 0.1 Uiso 1 1 calc R . . H97B H 0.2171 1.0305 0.0133 0.1 Uiso 1 1 calc R . . C98 C 0.23873(17) 1.1435(4) 0.00978(16) 0.124(2) Uani 1 1 d DU . . H98 H 0.2369 1.1921 0.0215 0.149 Uiso 1 1 calc R . . C99 C 0.26389(15) 1.1323(4) -0.01249(16) 0.115(2) Uani 1 1 d DU . . H99A H 0.2665 1.0842 -0.0247 0.138 Uiso 1 1 calc R . . H99B H 0.2808 1.1716 -0.0176 0.138 Uiso 1 1 calc R . . C100 C 0.06416(7) 0.83075(15) 0.16422(7) 0.0207(5) Uani 1 1 d . . . O100 O 0.04375(5) 0.86590(10) 0.18921(5) 0.0210(4) Uani 1 1 d . . . C101 C 0.05471(8) 0.75093(17) 0.15608(8) 0.0285(6) Uani 1 1 d . . . C102 C 0.02222(9) 0.72083(17) 0.16966(9) 0.0307(7) Uani 1 1 d . . . H102 H 0.0064 0.7524 0.184 0.037 Uiso 1 1 calc R . . C103 C 0.01211(10) 0.64590(17) 0.16295(10) 0.0384(8) Uani 1 1 d . . . H103 H -0.01 0.6266 0.173 0.046 Uiso 1 1 calc R . . C104 C 0.03445(12) 0.60016(19) 0.14171(10) 0.0469(9) Uani 1 1 d . . . O104 O 0.02616(10) 0.52647(14) 0.13202(9) 0.0679(9) Uani 1 1 d . B . C105 C 0.06754(14) 0.6279(2) 0.12899(13) 0.0634(12) Uani 1 1 d . . . H105 H 0.0836 0.5955 0.1155 0.076 Uiso 1 1 calc R . . C106 C 0.07758(11) 0.70255(18) 0.13573(11) 0.0441(9) Uani 1 1 d . . . H106 H 0.1002 0.721 0.1264 0.053 Uiso 1 1 calc R . . C107 C -0.00677(14) 0.4951(2) 0.14504(16) 0.0694(13) Uani 1 1 d DU . . H10A H -0.0289 0.5271 0.1373 0.083 Uiso 0.4110(17) 1 calc PR B 1 H10B H -0.0045 0.4861 0.1751 0.083 Uiso 0.4110(17) 1 calc PR B 1 H10F H -0.0292 0.519 0.1302 0.083 Uiso 0.5890(17) 1 d PR B 2 H10G H -0.0083 0.5004 0.1752 0.083 Uiso 0.5890(17) 1 d PR B 2 C108 C -0.0083(6) 0.4233(7) 0.1214(6) 0.092(4) Uani 0.4110(17) 1 d PDU B 1 H108 H -0.011 0.4339 0.0927 0.111 Uiso 0.4110(17) 1 calc PR B 1 C109 C -0.0073(5) 0.3579(7) 0.1266(6) 0.123(4) Uani 0.4110(17) 1 d PDU B 1 H10C H -0.0047 0.3381 0.1537 0.147 Uiso 0.4110(17) 1 calc PR B 1 H10D H -0.0091 0.3249 0.1036 0.147 Uiso 0.4110(17) 1 calc PR B 1 C10A C -0.0135(4) 0.4140(5) 0.1316(4) 0.079(3) Uani 0.5890(17) 1 d PDU B 2 H10E H -0.0295 0.3814 0.145 0.095 Uiso 0.5890(17) 1 calc PR B 2 C10B C 0.0044(2) 0.3913(4) 0.1000(2) 0.066(2) Uani 0.5890(17) 1 d PDU B 2 H10H H 0.0202 0.4252 0.0872 0.079 Uiso 0.5890(17) 1 calc PR B 2 H10I H 0.0013 0.3413 0.0901 0.079 Uiso 0.5890(17) 1 calc PR B 2 C6 C -0.03075(14) 1.2078(3) 0.34295(14) 0.0275(10) Uani 0.5890(17) 1 d P B 2 H6 H -0.0391 1.2196 0.369 0.033 Uiso 0.5890(17) 1 calc PR B 2 C110 C 0.00792(13) 1.1963(2) 0.34058(13) 0.0229(10) Uani 0.5890(17) 1 d PD B 2 O110 O 0.02318(19) 1.1839(4) 0.30749(18) 0.0261(5) Uani 0.5890(17) 1 d PD B 2 C111 C 0.03479(14) 1.2011(3) 0.37839(13) 0.0258(10) Uani 0.5890(17) 1 d PD B 2 C112 C 0.02461(14) 1.1937(3) 0.41844(13) 0.0287(11) Uani 0.5890(17) 1 d PD B 2 H112 H -0.001 1.1864 0.4228 0.034 Uiso 0.5890(17) 1 calc PR B 2 C113 C 0.05153(15) 1.1970(3) 0.45204(15) 0.0305(12) Uani 0.5890(17) 1 d PD B 2 H113 H 0.0442 1.1912 0.4791 0.037 Uiso 0.5890(17) 1 calc PR B 2 C114 C 0.08845(17) 1.2085(4) 0.44640(17) 0.0280(14) Uani 0.5890(17) 1 d PD B 2 O114 O 0.11673(10) 1.2143(2) 0.47764(10) 0.0382(9) Uani 0.5890(17) 1 d PD B 2 C115 C 0.09894(15) 1.2163(4) 0.40648(17) 0.0309(13) Uani 0.5890(17) 1 d PD B 2 H115 H 0.1244 1.2256 0.4022 0.037 Uiso 0.5890(17) 1 calc PR B 2 C116 C 0.07256(15) 1.2105(4) 0.37338(16) 0.0267(13) Uani 0.5890(17) 1 d PD B 2 H116 H 0.0803 1.2129 0.3464 0.032 Uiso 0.5890(17) 1 calc PR B 2 C117 C 0.10633(18) 1.2246(4) 0.51869(16) 0.0373(14) Uani 0.5890(17) 1 d PD B 2 H11A H 0.0932 1.1794 0.5278 0.045 Uiso 0.5890(17) 1 calc PR B 2 H11B H 0.0895 1.2685 0.5199 0.045 Uiso 0.5890(17) 1 calc PR B 2 C118 C 0.1423(2) 1.2373(5) 0.5456(2) 0.046(2) Uani 0.5890(17) 1 d PD B 2 H118 H 0.1594 1.1966 0.5497 0.055 Uiso 0.5890(17) 1 calc PR B 2 C119 C 0.1511(2) 1.3002(4) 0.5632(2) 0.057(2) Uani 0.5890(17) 1 d PD B 2 H11C H 0.1345 1.3418 0.5596 0.069 Uiso 0.5890(17) 1 calc PR B 2 H11D H 0.1741 1.3052 0.5798 0.069 Uiso 0.5890(17) 1 calc PR B 2 C120 C -0.05789(13) 1.2027(3) 0.30843(13) 0.0245(10) Uani 0.5890(17) 1 d PD B 2 O120 O -0.05123(16) 1.1828(3) 0.27221(15) 0.0280(7) Uani 0.5890(17) 1 d PD B 2 C121 C -0.09845(15) 1.2161(4) 0.31427(17) 0.0269(13) Uani 0.5890(17) 1 d PD B 2 C122 C -0.12605(13) 1.1853(3) 0.28625(17) 0.0310(12) Uani 0.5890(17) 1 d PD B 2 H122 H -0.1188 1.1594 0.2628 0.037 Uiso 0.5890(17) 1 calc PR B 2 C123 C -0.16371(14) 1.1916(3) 0.29195(16) 0.0388(13) Uani 0.5890(17) 1 d PD B 2 H123 H -0.1822 1.1703 0.2726 0.047 Uiso 0.5890(17) 1 calc PR B 2 C124 C -0.17417(16) 1.2295(4) 0.32622(18) 0.0358(16) Uani 0.5890(17) 1 d PD B 2 O124 O -0.21253(13) 1.2285(3) 0.33083(14) 0.0336(11) Uani 0.5890(17) 1 d PD B 2 C125 C -0.14746(15) 1.2649(3) 0.35290(16) 0.0383(13) Uani 0.5890(17) 1 d PD B 2 H125 H -0.1549 1.2937 0.3753 0.046 Uiso 0.5890(17) 1 calc PR B 2 C126 C -0.11005(14) 1.2582(3) 0.34695(15) 0.0344(12) Uani 0.5890(17) 1 d PD B 2 H126 H -0.0918 1.2826 0.3654 0.041 Uiso 0.5890(17) 1 calc PR B 2 C127 C -0.22348(19) 1.2518(4) 0.37011(18) 0.0456(16) Uani 0.5890(17) 1 d PD B 2 H12A H -0.2038 1.2374 0.392 0.055 Uiso 0.5890(17) 1 calc PR B 2 H12B H -0.2469 1.2257 0.3756 0.055 Uiso 0.5890(17) 1 calc PR B 2 C128 C -0.2294(3) 1.3343(4) 0.3713(2) 0.057(2) Uani 0.5890(17) 1 d PD B 2 H128 H -0.2348 1.3543 0.397 0.068 Uiso 0.5890(17) 1 calc PR B 2 C129 C -0.22831(17) 1.3819(4) 0.34207(18) 0.0488(16) Uani 0.5890(17) 1 d PD B 2 H12C H -0.2231 1.3656 0.3155 0.059 Uiso 0.5890(17) 1 calc PR B 2 H12D H -0.2327 1.4337 0.347 0.059 Uiso 0.5890(17) 1 calc PR B 2 C211 C 0.18267(18) 0.4808(4) 0.40074(17) 0.111(2) Uani 1 1 d D . . C212 C 0.15641(17) 0.4392(4) 0.37457(18) 0.100(2) Uani 1 1 d D . . H212 H 0.1596 0.4312 0.3463 0.12 Uiso 1 1 calc R . . C213 C 0.1268(2) 0.4118(4) 0.3921(2) 0.133(3) Uani 1 1 d D . . H213 H 0.1068 0.3926 0.374 0.16 Uiso 1 1 calc R . . C214 C 0.1227(2) 0.4086(5) 0.4325(2) 0.164(4) Uani 1 1 d D . . H214 H 0.1019 0.3846 0.4431 0.197 Uiso 1 1 calc R . . C215 C 0.1503(2) 0.4424(4) 0.4573(2) 0.117(2) Uani 1 1 d D . . H215 H 0.1494 0.4388 0.4862 0.14 Uiso 1 1 calc R . . C216 C 0.1795(2) 0.4816(4) 0.44266(18) 0.130(3) Uani 1 1 d D . . H216 H 0.1969 0.5083 0.4609 0.156 Uiso 1 1 calc R . . C217 C 0.2112(3) 0.5277(6) 0.3837(3) 0.229(6) Uani 1 1 d D . . H21A H 0.2027 0.5411 0.3553 0.344 Uiso 1 1 calc R . . H21B H 0.2348 0.4996 0.3843 0.344 Uiso 1 1 calc RD . . H21C H 0.2151 0.5735 0.4002 0.344 Uiso 1 1 calc R . . C311 C 0.13617(18) 0.5307(4) 0.6252(2) 0.133(2) Uani 1 1 d DU . . C312 C 0.1665(2) 0.4785(5) 0.6326(2) 0.166(2) Uani 1 1 d DU . . H312 H 0.1699 0.4532 0.6583 0.199 Uiso 1 1 calc R . . C313 C 0.1906(2) 0.4644(5) 0.6036(2) 0.156(2) Uani 1 1 d DU . . H313 H 0.2113 0.4313 0.6086 0.187 Uiso 1 1 calc R . . C314 C 0.1830(2) 0.5012(5) 0.5663(2) 0.150(2) Uani 1 1 d DU . . H314 H 0.1985 0.4904 0.545 0.18 Uiso 1 1 calc R . . C315 C 0.1548(2) 0.5518(5) 0.5582(2) 0.150(2) Uani 1 1 d DU . . H315 H 0.1513 0.5764 0.5323 0.18 Uiso 1 1 calc R . . C316 C 0.1307(2) 0.5670(5) 0.5893(2) 0.152(2) Uani 1 1 d DU . . H316 H 0.1109 0.6024 0.5846 0.182 Uiso 1 1 calc R . . C317 C 0.1124(2) 0.5461(4) 0.6606(2) 0.152(3) Uani 1 1 d DU . . H31A H 0.1034 0.4984 0.671 0.228 Uiso 1 1 calc R . . H31B H 0.091 0.5777 0.6509 0.228 Uiso 1 1 calc RD . . H31C H 0.1276 0.572 0.6828 0.228 Uiso 1 1 calc RD . . 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 Eu1 0.02022(6) 0.01810(6) 0.01554(5) 0.00155(5) 0.00039(4) 0.00121(5) Eu2 0.01628(6) 0.01984(6) 0.01971(5) -0.00509(5) 0.00068(4) -0.00128(5) Eu3 0.02348(9) 0.01585(8) 0.01699(7) 0 0.00174(6) 0 O1 0.0200(12) 0.0162(11) 0.0185(11) 0 0.0001(9) 0 O2 0.0200(9) 0.0189(8) 0.0190(8) -0.0026(6) 0.0007(7) -0.0041(7) O3 0.0219(9) 0.0176(8) 0.0192(8) 0.0012(6) 0.0031(7) 0.0027(7) C1 0.0199(14) 0.0452(19) 0.0381(16) -0.0102(14) -0.0002(12) -0.0002(13) C10 0.0241(14) 0.0458(19) 0.0295(14) -0.0121(13) -0.0012(11) -0.0068(14) O10 0.0172(9) 0.0373(12) 0.0389(11) -0.0157(9) -0.0016(8) -0.0034(9) C11 0.0230(15) 0.047(2) 0.0431(17) -0.0140(14) 0.0005(12) -0.0115(14) C12 0.0301(18) 0.081(3) 0.096(3) -0.056(2) 0.0234(19) -0.028(2) C13 0.044(2) 0.092(3) 0.109(3) -0.072(3) 0.031(2) -0.036(2) C14 0.0363(19) 0.070(3) 0.052(2) -0.0214(19) 0.0041(16) -0.0284(19) O14 0.0438(15) 0.085(2) 0.0693(17) -0.0351(15) 0.0158(13) -0.0411(15) C15 0.0268(16) 0.057(2) 0.0503(19) -0.0042(17) 0.0040(14) -0.0155(16) C16 0.0261(16) 0.049(2) 0.0489(19) -0.0058(15) 0.0031(14) -0.0073(15) C17 0.0317(18) 0.062(3) 0.063(2) -0.0072(19) 0.0025(16) -0.0231(18) C18 0.039(2) 0.066(3) 0.079(3) -0.011(2) 0.004(2) -0.027(2) C19 0.066(3) 0.095(4) 0.109(4) -0.042(3) 0.019(3) -0.051(3) C20 0.0214(13) 0.0384(17) 0.0243(13) -0.0036(11) 0.0024(10) 0.0054(12) O20 0.0202(9) 0.0318(11) 0.0264(9) -0.0080(8) -0.0011(7) 0.0018(8) C21 0.0232(14) 0.0433(18) 0.0319(14) -0.0054(13) 0.0011(11) 0.0099(13) C22 0.0305(16) 0.0392(18) 0.0317(14) -0.0055(13) -0.0011(12) 0.0122(14) C23 0.044(2) 0.046(2) 0.0395(17) -0.0087(15) 0.0041(15) 0.0159(17) C24 0.051(2) 0.052(2) 0.0437(18) 0.0024(16) 0.0095(16) 0.0274(18) O24 0.0607(18) 0.0496(17) 0.0762(19) 0.0004(14) 0.0105(15) 0.0243(14) C25 0.0368(19) 0.064(2) 0.0486(19) 0.0045(18) -0.0037(15) 0.0233(18) C26 0.0293(16) 0.058(2) 0.0389(16) -0.0039(15) -0.0041(13) 0.0127(16) C27 0.114(4) 0.073(3) 0.117(4) 0.004(3) 0.016(3) 0.030(3) C28 0.131(5) 0.075(3) 0.129(5) 0.001(4) 0.012(4) 0.037(4) C29 0.133(6) 0.137(6) 0.150(6) 0.035(5) 0.003(5) 0.087(5) C2 0.0296(15) 0.0285(15) 0.0301(14) -0.0022(11) -0.0079(11) 0.0044(12) C30 0.0278(14) 0.0342(16) 0.0195(12) -0.0025(10) -0.0053(10) 0.0036(12) O30 0.0281(10) 0.0272(10) 0.0208(9) -0.0011(7) -0.0052(7) 0.0035(8) C31 0.0263(15) 0.0346(16) 0.0310(14) -0.0068(12) -0.0095(11) 0.0035(12) C32 0.0316(16) 0.0373(17) 0.0328(15) -0.0081(13) -0.0070(12) 0.0050(14) C33 0.0413(19) 0.046(2) 0.0466(19) -0.0216(15) -0.0113(15) -0.0001(16) C34 0.0354(19) 0.056(2) 0.066(2) -0.0265(19) -0.0195(17) 0.0006(17) O34 0.0403(15) 0.074(2) 0.100(2) -0.0484(17) -0.0321(15) 0.0023(14) C35 0.0316(18) 0.060(2) 0.069(2) -0.0303(19) -0.0190(17) 0.0106(18) C36 0.0306(16) 0.045(2) 0.0483(18) -0.0172(15) -0.0112(14) 0.0050(15) C37 0.055(3) 0.079(3) 0.091(3) -0.042(3) -0.029(2) -0.009(2) C38 0.047(2) 0.084(3) 0.087(3) -0.042(3) 0.003(2) -0.019(2) C39 0.062(3) 0.079(3) 0.082(3) -0.026(3) 0.009(2) -0.020(3) C40 0.0236(13) 0.0212(13) 0.0251(12) -0.0007(10) -0.0016(10) 0.0042(11) O40 0.0231(9) 0.0212(9) 0.0205(8) -0.0012(7) -0.0031(7) 0.0054(8) C41 0.0262(14) 0.0244(14) 0.0315(14) -0.0044(11) -0.0037(11) 0.0058(12) C42 0.0277(15) 0.0270(15) 0.0348(15) -0.0033(12) -0.0023(12) 0.0046(12) C43 0.0363(18) 0.0303(16) 0.0436(17) -0.0063(13) -0.0066(14) 0.0051(14) C44 0.045(2) 0.0257(16) 0.058(2) -0.0082(15) -0.0066(16) 0.0109(15) O44 0.074(2) 0.0280(13) 0.0830(19) -0.0176(13) -0.0191(15) 0.0115(13) C45 0.052(2) 0.0266(17) 0.059(2) -0.0021(15) -0.0194(17) 0.0125(16) C46 0.045(2) 0.0281(16) 0.0457(18) -0.0041(13) -0.0164(15) 0.0121(15) C47 0.110(4) 0.046(2) 0.094(3) -0.026(2) -0.027(3) 0.013(3) C48 0.133(5) 0.050(3) 0.125(4) -0.024(3) -0.043(4) 0.014(3) C49 0.131(7) 0.068(5) 0.087(6) -0.017(4) 0.003(5) 0.032(5) C48' 0.133(5) 0.050(3) 0.125(4) -0.024(3) -0.043(4) 0.014(3) C49' 0.160(9) 0.054(6) 0.201(11) -0.039(8) -0.059(10) 0.003(6) C3 0.0362(16) 0.0344(16) 0.0196(12) 0.0029(11) 0.0036(11) -0.0054(13) C50 0.0202(12) 0.0305(15) 0.0204(11) -0.0032(10) 0.0006(9) -0.0114(11) O50 0.0297(10) 0.0262(10) 0.0193(8) 0.0006(7) 0.0047(7) 0.0002(8) C51 0.0253(14) 0.0364(16) 0.0234(12) -0.0060(11) 0.0043(11) -0.0061(12) C52 0.0359(17) 0.048(2) 0.0290(14) -0.0045(13) 0.0045(13) 0.0063(15) C53 0.051(2) 0.063(2) 0.0405(18) -0.0021(17) 0.0097(16) 0.0254(19) C54 0.0348(18) 0.067(3) 0.0395(17) -0.0141(17) 0.0076(14) 0.0120(18) O54 0.072(2) 0.101(2) 0.0459(15) -0.0203(15) 0.0204(14) 0.0232(18) C55 0.0366(18) 0.059(2) 0.0283(15) -0.0109(14) 0.0106(13) -0.0029(16) C56 0.0313(16) 0.0422(18) 0.0280(14) -0.0068(12) 0.0056(12) -0.0075(14) C57 0.050(2) 0.088(3) 0.050(2) -0.005(2) 0.0035(18) 0.020(2) C58 0.112(4) 0.114(4) 0.085(3) 0.013(3) 0.041(3) 0.066(4) C59 0.100(6) 0.106(6) 0.043(4) -0.013(4) 0.007(4) 0.063(5) C59' 0.106(9) 0.110(9) 0.086(8) 0.004(8) 0.013(7) 0.027(8) C60 0.0304(15) 0.0255(14) 0.0214(12) 0.0038(10) -0.0020(10) -0.0078(12) O60 0.0368(11) 0.0246(10) 0.0205(9) 0.0033(7) 0.0002(8) 0.0021(9) C61 0.0478(19) 0.0297(16) 0.0250(13) 0.0085(11) -0.0054(12) -0.0051(14) C62 0.047(2) 0.0331(17) 0.0368(16) 0.0094(13) -0.0074(14) 0.0019(15) C63 0.068(3) 0.0342(19) 0.053(2) 0.0098(16) -0.0063(18) 0.0074(18) C64 0.114(4) 0.046(2) 0.058(2) 0.0316(19) -0.024(2) -0.006(2) C65 0.152(5) 0.049(2) 0.0369(19) 0.0199(18) -0.006(2) 0.000(3) C66 0.110(3) 0.0337(19) 0.0290(16) 0.0120(14) 0.0002(19) -0.004(2) O64 0.165(4) 0.0495(18) 0.088(2) 0.0421(16) -0.026(2) 0.009(2) C67 0.117(4) 0.056(3) 0.102(3) 0.028(2) -0.005(3) 0.019(3) C68 0.103(4) 0.058(3) 0.108(4) 0.016(3) -0.017(3) 0.010(3) C69 0.087(4) 0.074(3) 0.117(4) 0.020(3) -0.002(3) 0.017(3) C4 0.058(5) 0.027(4) 0.020(3) -0.003(3) -0.010(3) -0.014(4) C70 0.051(5) 0.014(3) 0.027(3) 0.000(2) -0.004(3) -0.003(3) O70 0.0331(12) 0.0223(12) 0.0226(9) -0.0064(8) 0.0002(8) -0.0020(9) C71 0.045(6) 0.021(4) 0.023(3) -0.003(3) -0.011(4) -0.011(4) C72 0.045(4) 0.025(4) 0.018(3) 0.000(2) -0.002(3) -0.009(3) C73 0.038(4) 0.029(4) 0.035(4) -0.001(3) 0.003(3) -0.007(3) C74 0.043(5) 0.032(4) 0.021(3) 0.003(3) -0.007(3) -0.006(4) O74 0.062(4) 0.052(4) 0.018(2) -0.001(2) -0.005(2) -0.015(3) C75 0.047(5) 0.036(5) 0.027(5) 0.006(4) -0.008(4) -0.019(4) C76 0.064(6) 0.036(5) 0.017(4) 0.009(3) -0.004(4) -0.017(4) C77 0.049(6) 0.055(6) 0.030(4) -0.002(4) -0.007(4) -0.014(5) C78 0.073(8) 0.060(7) 0.029(5) 0.009(4) 0.013(5) -0.023(6) C79 0.093(10) 0.084(10) 0.047(7) -0.003(7) -0.001(7) -0.031(8) C80 0.039(4) 0.012(3) 0.021(3) 0.005(2) 0.001(3) -0.004(3) O80 0.0382(13) 0.0221(11) 0.0239(16) 0.0045(16) 0.0046(11) 0.016(2) C81 0.036(4) 0.028(4) 0.027(3) 0.003(3) -0.002(3) -0.007(3) C82 0.041(6) 0.065(7) 0.039(5) -0.013(5) 0.003(4) 0.004(6) C83 0.044(5) 0.061(6) 0.023(3) -0.003(4) 0.003(3) 0.004(4) C84 0.048(6) 0.049(6) 0.037(5) 0.015(5) -0.018(4) -0.015(5) O84 0.040(4) 0.092(7) 0.074(5) 0.054(5) 0.009(3) -0.007(4) C85 0.058(6) 0.116(9) 0.043(5) 0.038(5) -0.025(4) -0.049(6) C86 0.058(6) 0.100(8) 0.027(4) 0.023(4) -0.020(4) -0.049(6) C87 0.040(5) 0.069(7) 0.042(5) 0.009(4) -0.010(4) 0.005(5) C88 0.062(8) 0.085(10) 0.057(7) 0.028(6) 0.011(6) -0.018(7) C89 0.066(8) 0.100(10) 0.110(10) -0.022(8) 0.047(7) -0.019(7) C5 0.0249(14) 0.0270(14) 0.0219(12) -0.0050(10) 0.0034(10) 0.0054(11) C90 0.0246(13) 0.0271(15) 0.0271(13) 0.0028(11) 0.0049(10) 0.0092(12) O90 0.0229(10) 0.0274(10) 0.0306(10) -0.0055(8) 0.0091(8) -0.0017(8) C91 0.0209(13) 0.0295(15) 0.0300(13) 0.0031(11) 0.0044(11) 0.0051(12) C92 0.0266(15) 0.0441(19) 0.0261(13) 0.0036(12) 0.0019(11) 0.0048(13) C93 0.0376(18) 0.059(2) 0.0307(15) 0.0116(15) 0.0090(13) 0.0100(17) C94 0.043(2) 0.055(2) 0.0485(19) 0.0159(17) 0.0188(16) 0.0022(18) O94 0.0674(19) 0.089(2) 0.0577(16) 0.0240(15) 0.0298(14) -0.0153(17) C95 0.043(2) 0.051(2) 0.054(2) 0.0036(17) 0.0197(16) -0.0105(18) C96 0.0312(16) 0.0425(18) 0.0354(16) 0.0022(13) 0.0104(13) -0.0050(14) C97 0.055(3) 0.148(5) 0.049(2) 0.048(3) 0.016(2) -0.003(3) C98 0.188(6) 0.126(5) 0.069(3) 0.039(3) 0.072(4) -0.014(5) C99 0.108(5) 0.167(7) 0.068(3) 0.016(4) -0.002(3) -0.046(5) C100 0.0218(12) 0.0186(12) 0.0210(11) -0.0053(9) -0.0023(9) 0.0048(10) O100 0.0183(9) 0.0215(9) 0.0234(8) -0.0059(7) 0.0025(7) 0.0000(7) C101 0.0293(15) 0.0296(15) 0.0253(13) -0.0021(11) -0.0035(11) 0.0032(12) C102 0.0307(15) 0.0248(14) 0.0352(15) -0.0065(11) -0.0040(12) -0.0003(12) C103 0.0432(19) 0.0260(16) 0.0433(17) -0.0063(13) -0.0097(14) -0.0063(14) C104 0.074(3) 0.0247(17) 0.0404(17) -0.0115(13) -0.0022(17) -0.0026(17) O104 0.112(3) 0.0247(13) 0.0686(18) -0.0192(12) 0.0159(17) -0.0126(15) C105 0.098(3) 0.0289(19) 0.068(2) -0.0180(17) 0.031(2) 0.008(2) C106 0.059(2) 0.0257(16) 0.0513(19) -0.0099(14) 0.0237(17) 0.0030(16) C107 0.078(3) 0.0239(18) 0.101(3) -0.009(2) -0.020(3) -0.010(2) C108 0.118(8) 0.033(5) 0.119(8) -0.004(6) -0.022(7) -0.012(6) C109 0.164(9) 0.068(6) 0.137(9) -0.031(7) 0.022(8) -0.022(8) C10A 0.111(6) 0.021(4) 0.102(6) 0.000(4) -0.004(5) -0.008(4) C10B 0.103(6) 0.014(3) 0.081(5) -0.014(3) 0.012(4) -0.008(3) C6 0.028(2) 0.031(3) 0.024(2) -0.0051(18) 0.0053(18) -0.001(2) C110 0.034(3) 0.0091(19) 0.025(2) -0.0065(15) 0.0032(18) -0.0063(18) O110 0.0331(12) 0.0223(12) 0.0226(9) -0.0064(8) 0.0002(8) -0.0020(9) C111 0.029(3) 0.024(2) 0.024(2) -0.0025(18) 0.0025(19) -0.002(2) C112 0.024(2) 0.032(3) 0.031(2) 0.004(2) 0.0052(19) -0.001(2) C113 0.034(3) 0.035(3) 0.023(2) 0.004(2) 0.003(2) 0.001(2) C114 0.030(3) 0.030(3) 0.023(3) -0.001(2) 0.001(2) 0.001(3) O114 0.034(2) 0.051(2) 0.0284(17) -0.0059(16) -0.0005(15) 0.0018(18) C115 0.022(3) 0.045(4) 0.027(3) -0.007(3) 0.004(2) -0.008(2) C116 0.022(3) 0.039(4) 0.019(2) -0.007(2) 0.000(2) -0.003(2) C117 0.035(3) 0.055(4) 0.021(2) 0.004(2) -0.004(2) 0.002(3) C118 0.046(5) 0.060(5) 0.032(4) 0.012(3) 0.006(3) -0.003(4) C119 0.064(5) 0.066(5) 0.042(4) 0.004(4) 0.004(4) -0.016(4) C120 0.027(2) 0.018(2) 0.029(2) -0.0015(17) 0.0047(18) 0.0033(18) O120 0.0382(13) 0.0221(11) 0.0239(16) 0.0045(16) 0.0046(11) 0.016(2) C121 0.028(3) 0.029(3) 0.024(2) -0.002(2) 0.005(2) 0.005(2) C122 0.023(2) 0.036(3) 0.034(3) -0.009(2) 0.002(2) 0.006(2) C123 0.026(3) 0.049(4) 0.040(3) -0.004(2) 0.002(2) 0.009(3) C124 0.027(3) 0.047(4) 0.033(3) -0.002(3) 0.003(3) 0.014(3) O124 0.020(2) 0.049(3) 0.031(2) -0.0125(19) -0.0007(15) 0.010(2) C125 0.037(3) 0.045(3) 0.034(3) -0.005(2) 0.009(2) 0.013(3) C126 0.029(3) 0.039(3) 0.034(3) -0.006(2) -0.003(2) 0.011(2) C127 0.035(3) 0.060(4) 0.042(3) 0.002(3) 0.009(3) 0.014(3) C128 0.067(6) 0.064(5) 0.040(4) -0.012(3) 0.003(4) 0.030(4) C129 0.047(4) 0.055(4) 0.044(3) -0.001(3) 0.000(3) 0.019(3) C211 0.115(5) 0.119(5) 0.102(5) 0.024(4) 0.018(4) -0.006(5) C212 0.088(4) 0.120(5) 0.091(4) -0.001(4) -0.005(3) -0.010(4) C213 0.137(7) 0.099(5) 0.164(8) -0.006(5) 0.019(6) 0.003(5) C214 0.235(11) 0.133(7) 0.121(6) -0.035(6) 0.005(7) -0.023(7) C215 0.148(7) 0.096(5) 0.109(5) -0.024(4) 0.022(5) -0.023(5) C216 0.160(7) 0.133(6) 0.097(5) -0.031(4) 0.010(5) -0.044(6) C217 0.137(8) 0.283(14) 0.274(14) -0.082(11) 0.057(9) -0.058(9) C311 0.086(4) 0.152(5) 0.162(4) 0.012(4) 0.029(3) -0.040(3) C312 0.109(4) 0.207(6) 0.187(5) 0.025(5) 0.049(4) 0.006(4) C313 0.100(4) 0.209(6) 0.162(5) 0.042(5) 0.030(4) -0.013(4) C314 0.107(4) 0.204(6) 0.132(4) 0.013(5) -0.027(4) -0.023(4) C315 0.107(5) 0.207(6) 0.131(4) -0.048(4) -0.009(4) -0.001(4) C316 0.115(4) 0.188(5) 0.148(5) -0.008(4) -0.017(4) -0.063(4) C317 0.127(5) 0.140(6) 0.196(6) 0.016(5) 0.053(5) -0.006(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Eu1 O50 2.3190(18) . ? Eu1 O60 2.3265(18) . ? Eu1 O3 2.3599(17) . ? Eu1 O40 2.3721(18) . ? Eu1 O2 2.3843(17) . ? Eu1 O30 2.4050(19) . ? Eu1 O100 2.4832(18) 2 ? Eu1 O1 2.6487(4) . ? Eu2 O10 2.3078(18) . ? Eu2 O20 2.3294(19) . ? Eu2 O2 2.3509(17) . ? Eu2 O90 2.3555(19) . ? Eu2 O100 2.3994(17) . ? Eu2 O3 2.3997(18) 2 ? Eu2 O40 2.4928(18) . ? Eu2 O1 2.5288(4) . ? Eu3 O70 2.331(8) . ? Eu3 O70 2.331(8) 2 ? Eu3 O80 2.335(8) . ? Eu3 O80 2.335(8) 2 ? Eu3 O110 2.355(6) . ? Eu3 O110 2.355(6) 2 ? Eu3 O120 2.393(5) 2 ? Eu3 O120 2.393(5) . ? Eu3 O3 2.4433(17) 2 ? Eu3 O3 2.4433(17) . ? Eu3 O2 2.4674(17) 2 ? Eu3 O2 2.4674(17) . ? O1 Eu2 2.5288(4) 2 ? O1 Eu1 2.6487(4) 2 ? O1 H1O 0.807 . ? O2 H2O 1 . ? O3 Eu2 2.3997(18) 2 ? O3 H3O 1 . ? C1 C20 1.401(4) . ? C1 C10 1.414(5) . ? C1 H1 0.95 . ? C10 O10 1.277(3) . ? C10 C11 1.492(4) . ? C11 C12 1.386(5) . ? C11 C16 1.391(4) . ? C12 C13 1.384(5) . ? C12 H12 0.95 . ? C13 C14 1.383(5) . ? C13 H13 0.95 . ? C14 O14 1.372(4) . ? C14 C15 1.373(5) . ? O14 C17 1.417(4) . ? C15 C16 1.385(4) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C17 C18 1.471(5) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.303(6) . ? C18 H18 0.95 . ? C19 H19A 0.95 . ? C19 H19B 0.95 . ? C20 O20 1.269(3) . ? C20 C21 1.492(4) . ? C21 C26 1.399(4) . ? C21 C22 1.406(4) . ? C22 C23 1.378(5) . ? C22 H22 0.95 . ? C23 C24 1.379(5) . ? C23 H23 0.95 . ? C24 O24 1.368(4) . ? C24 C25 1.385(6) . ? O24 C27 1.450(7) . ? C25 C26 1.389(5) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C27 C28' 1.483(17) . ? C27 C28 1.551(8) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C27 H27C 0.99 . ? C27 H27D 0.99 . ? C28 C29 1.143(10) . ? C28 H28 0.95 . ? C29 H29A 0.95 . ? C29 H29B 0.95 . ? C28' C29' 1.243(18) . ? C28' H28' 0.95 . ? C29' H29C 0.95 . ? C29' H29D 0.95 . ? C2 C40 1.376(4) . ? C2 C30 1.430(4) . ? C2 H2 0.95 . ? C30 O30 1.251(3) . ? C30 C31 1.493(4) . ? C31 C32 1.393(4) . ? C31 C36 1.400(4) . ? C32 C33 1.381(4) . ? C32 H32 0.95 . ? C33 C34 1.380(5) . ? C33 H33 0.95 . ? C34 C35 1.380(5) . ? C34 O34 1.383(4) . ? O34 C37 1.445(5) . ? C35 C36 1.377(5) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.495(7) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.312(7) . ? C38 H38 0.95 . ? C39 H39A 0.95 . ? C39 H39B 0.95 . ? C40 O40 1.307(3) . ? C40 C41 1.495(4) . ? C41 C42 1.391(4) . ? C41 C46 1.402(4) . ? C42 C43 1.385(4) . ? C42 H42 0.95 . ? C43 C44 1.387(5) . ? C43 H43 0.95 . ? C44 O44 1.370(4) . ? C44 C45 1.396(5) . ? O44 C47 1.392(5) . ? C45 C46 1.379(5) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 C48' 1.468(14) . ? C47 C48 1.501(11) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C47 H47C 0.9923 . ? C47 H47D 0.9948 . ? C48 C49 1.299(14) . ? C48 H48 0.95 . ? C49 H49A 0.95 . ? C49 H49B 0.95 . ? C48' C49' 1.254(17) . ? C48' H48' 0.95 . ? C49' H49C 0.95 . ? C49' H49D 0.95 . ? C3 C60 1.395(4) . ? C3 C50 1.408(4) . ? C3 H3 0.95 . ? C50 O50 1.268(3) . ? C50 C51 1.496(4) . ? C51 C52 1.389(4) . ? C51 C56 1.403(4) . ? C52 C53 1.388(5) . ? C52 H52 0.95 . ? C53 C54 1.383(5) . ? C53 H53 0.95 . ? C54 C55 1.375(5) . ? C54 O54 1.399(4) . ? O54 C57 1.410(5) . ? C55 C56 1.390(5) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 C58 1.510(7) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 C59' 1.079(12) . ? C58 C59 1.246(9) . ? C58 H58 0.95 . ? C58 H58' 0.9556 . ? C59 H59A 0.95 . ? C59 H59B 0.95 . ? C59' H59C 0.95 . ? C59' H59D 0.95 . ? C60 O60 1.272(3) . ? C60 C61 1.498(4) . ? C61 C62 1.375(5) . ? C61 C66 1.396(4) . ? C62 C63 1.384(5) . ? C62 H62 0.95 . ? C63 C64 1.380(6) . ? C63 H63 0.95 . ? C64 O64 1.373(4) . ? C64 C65 1.374(6) . ? C65 C66 1.368(5) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? O64 C67 1.373(6) . ? C67 C68 1.553(7) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? C68 C69 1.238(4) . ? C68 H68 0.95 . ? C69 H69A 0.95 . ? C69 H69B 0.95 . ? C4 C70 1.408(11) . ? C4 C80 1.425(9) . ? C4 H4 0.95 . ? C70 O70 1.277(10) . ? C70 C71 1.514(8) . ? C71 C76 1.385(9) . ? C71 C72 1.390(9) . ? C72 C73 1.369(8) . ? C72 H72 0.95 . ? C73 C74 1.394(9) . ? C73 H73 0.95 . ? C74 O74 1.368(7) . ? C74 C75 1.376(9) . ? O74 C77 1.398(9) . ? C75 C76 1.401(9) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? C77 C78 1.516(12) . ? C77 H77A 0.99 . ? C77 H77B 0.99 . ? C78 C79 1.275(11) . ? C78 H78 0.95 . ? C79 H79A 0.95 . ? C79 H79B 0.95 . ? C80 O80 1.267(9) . ? C80 C81 1.490(8) . ? C81 C82 1.386(9) . ? C81 C86 1.389(9) . ? C82 C83 1.379(10) . ? C82 H82 0.95 . ? C83 C84 1.371(9) . ? C83 H83 0.95 . ? C84 O84 1.365(10) . ? C84 C85 1.380(9) . ? O84 C87 1.410(10) . ? C85 C86 1.350(10) . ? C85 H85 0.95 . ? C86 H86 0.95 . ? C87 C88 1.445(12) . ? C87 H87A 0.99 . ? C87 H87B 0.99 . ? C88 C89 1.265(11) . ? C88 H88 0.95 . ? C89 H89A 0.95 . ? C89 H89B 0.95 . ? C5 C100 1.390(4) . ? C5 C90 1.428(4) . ? C5 H5 0.95 . ? C90 O90 1.256(3) . ? C90 C91 1.490(4) . ? C91 C92 1.385(4) . ? C91 C96 1.390(4) . ? C92 C93 1.394(4) . ? C92 H92 0.95 . ? C93 C94 1.376(5) . ? C93 H93 0.95 . ? C94 O94 1.374(4) . ? C94 C95 1.387(5) . ? O94 C97 1.432(5) . ? C95 C96 1.381(5) . ? C95 H95 0.95 . ? C96 H96 0.95 . ? C97 C98 1.592(7) . ? C97 H97A 0.99 . ? C97 H97B 0.99 . ? C98 C99 1.227(4) . ? C98 H98 0.95 . ? C99 H99A 0.95 . ? C99 H99B 0.95 . ? C100 O100 1.305(3) . ? C100 C101 1.478(4) . ? O100 Eu1 2.4832(18) 2 ? C101 C102 1.391(4) . ? C101 C106 1.399(4) . ? C102 C103 1.393(4) . ? C102 H102 0.95 . ? C103 C104 1.374(5) . ? C103 H103 0.95 . ? C104 O104 1.374(4) . ? C104 C105 1.384(6) . ? O104 C107 1.406(6) . ? C105 C106 1.388(5) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C107 C108 1.491(13) . ? C107 C10A 1.522(9) . ? C107 H10A 0.99 . ? C107 H10B 0.99 . ? C107 H10F 0.9956 . ? C107 H10G 0.9946 . ? C108 C109 1.175(14) . ? C108 H108 0.95 . ? C109 H10C 0.95 . ? C109 H10D 0.95 . ? C10A C10B 1.326(12) . ? C10A H10E 0.95 . ? C10B H10H 0.95 . ? C10B H10I 0.95 . ? C6 C110 1.411(7) . ? C6 C120 1.422(6) . ? C6 H6 0.95 . ? C110 O110 1.275(7) . ? C110 C111 1.496(6) . ? C111 C116 1.389(7) . ? C111 C112 1.396(6) . ? C112 C113 1.394(6) . ? C112 H112 0.95 . ? C113 C114 1.368(7) . ? C113 H113 0.95 . ? C114 O114 1.374(6) . ? C114 C115 1.397(7) . ? O114 C117 1.436(6) . ? C115 C116 1.372(7) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C117 C118 1.509(8) . ? C117 H11A 0.99 . ? C117 H11B 0.99 . ? C118 C119 1.284(9) . ? C118 H118 0.95 . ? C119 H11C 0.95 . ? C119 H11D 0.95 . ? C120 O120 1.278(6) . ? C120 C121 1.503(7) . ? C121 C122 1.396(7) . ? C121 C126 1.398(7) . ? C122 C123 1.385(6) . ? C122 H122 0.95 . ? C123 C124 1.387(7) . ? C123 H123 0.95 . ? C124 C125 1.385(8) . ? C124 O124 1.397(7) . ? O124 C127 1.437(7) . ? C125 C126 1.378(7) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C127 C128 1.484(9) . ? C127 H12A 0.99 . ? C127 H12B 0.99 . ? C128 C129 1.279(8) . ? C128 H128 0.95 . ? C129 H12C 0.95 . ? C129 H12D 0.95 . ? C211 C216 1.384(6) . ? C211 C212 1.420(6) . ? C211 C217 1.467(7) . ? C212 C213 1.342(7) . ? C212 H212 0.95 . ? C213 C214 1.345(7) . ? C213 H213 0.95 . ? C214 C215 1.358(7) . ? C214 H214 0.95 . ? C215 C216 1.380(7) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C217 H21A 0.98 . ? C217 H21B 0.98 . ? C217 H21C 0.98 . ? C311 C316 1.339(7) . ? C311 C312 1.432(7) . ? C311 C317 1.522(7) . ? C312 C313 1.366(7) . ? C312 H312 0.95 . ? C313 C314 1.386(7) . ? C313 H313 0.95 . ? C314 C315 1.362(7) . ? C314 H314 0.95 . ? C315 C316 1.418(7) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C317 H31A 0.98 . ? C317 H31B 0.98 . ? C317 H31C 0.98 . ? 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 O50 Eu1 O60 72.75(7) . . ? O50 Eu1 O3 76.92(6) . . ? O60 Eu1 O3 140.23(7) . . ? O50 Eu1 O40 152.33(6) . . ? O60 Eu1 O40 81.55(6) . . ? O3 Eu1 O40 130.69(6) . . ? O50 Eu1 O2 116.58(6) . . ? O60 Eu1 O2 146.18(7) . . ? O3 Eu1 O2 71.46(6) . . ? O40 Eu1 O2 79.95(6) . . ? O50 Eu1 O30 91.51(6) . . ? O60 Eu1 O30 76.12(7) . . ? O3 Eu1 O30 130.25(6) . . ? O40 Eu1 O30 72.15(6) . . ? O2 Eu1 O30 71.36(6) . . ? O50 Eu1 O100 90.62(6) . 2 ? O60 Eu1 O100 78.35(6) . 2 ? O3 Eu1 O100 76.85(6) . 2 ? O40 Eu1 O100 94.13(6) . 2 ? O2 Eu1 O100 130.95(6) . 2 ? O30 Eu1 O100 152.47(6) . 2 ? O50 Eu1 O1 140.46(5) . . ? O60 Eu1 O1 128.17(7) . . ? O3 Eu1 O1 66.96(6) . . ? O40 Eu1 O1 65.10(5) . . ? O2 Eu1 O1 66.97(6) . . ? O30 Eu1 O1 123.88(5) . . ? O100 Eu1 O1 66.53(5) 2 . ? O10 Eu2 O20 73.39(7) . . ? O10 Eu2 O2 76.07(6) . . ? O20 Eu2 O2 137.86(6) . . ? O10 Eu2 O90 82.51(7) . . ? O20 Eu2 O90 78.23(7) . . ? O2 Eu2 O90 125.50(6) . . ? O10 Eu2 O100 147.11(6) . . ? O20 Eu2 O100 80.43(6) . . ? O2 Eu2 O100 136.24(6) . . ? O90 Eu2 O100 72.82(6) . . ? O10 Eu2 O3 115.22(7) . 2 ? O20 Eu2 O3 147.09(6) . 2 ? O2 Eu2 O3 73.20(6) . 2 ? O90 Eu2 O3 71.98(6) . 2 ? O100 Eu2 O3 77.74(6) . 2 ? O10 Eu2 O40 93.97(7) . . ? O20 Eu2 O40 75.74(6) . . ? O2 Eu2 O40 78.17(6) . . ? O90 Eu2 O40 153.63(6) . . ? O100 Eu2 O40 98.58(6) . . ? O3 Eu2 O40 131.66(6) 2 . ? O10 Eu2 O1 142.57(5) . . ? O20 Eu2 O1 125.37(7) . . ? O2 Eu2 O1 69.51(6) . . ? O90 Eu2 O1 129.80(5) . . ? O100 Eu2 O1 69.70(5) . . ? O3 Eu2 O1 68.43(6) 2 . ? O40 Eu2 O1 65.35(5) . . ? O70 Eu3 O70 118.8(5) . 2 ? O70 Eu3 O80 73.1(3) . . ? O70 Eu3 O80 77.0(3) 2 . ? O70 Eu3 O80 77.0(3) . 2 ? O70 Eu3 O80 73.1(3) 2 2 ? O80 Eu3 O80 119.2(3) . 2 ? O70 Eu3 O110 3.1(4) . . ? O70 Eu3 O110 116.59(12) 2 . ? O80 Eu3 O110 70.2(2) . . ? O80 Eu3 O110 77.9(2) 2 . ? O70 Eu3 O110 116.59(12) . 2 ? O70 Eu3 O110 3.1(4) 2 2 ? O80 Eu3 O110 77.9(2) . 2 ? O80 Eu3 O110 70.2(2) 2 2 ? O110 Eu3 O110 114.5(3) . 2 ? O70 Eu3 O120 77.5(3) . 2 ? O70 Eu3 O120 71.4(3) 2 2 ? O80 Eu3 O120 5.7(3) . 2 ? O80 Eu3 O120 117.63(13) 2 2 ? O110 Eu3 O120 74.5(2) . 2 ? O110 Eu3 O120 72.5(2) 2 2 ? O70 Eu3 O120 71.4(3) . . ? O70 Eu3 O120 77.5(3) 2 . ? O80 Eu3 O120 117.63(12) . . ? O80 Eu3 O120 5.7(3) 2 . ? O110 Eu3 O120 72.5(2) . . ? O110 Eu3 O120 74.5(2) 2 . ? O120 Eu3 O120 116.7(3) 2 . ? O70 Eu3 O3 133.1(2) . 2 ? O70 Eu3 O3 85.4(2) 2 2 ? O80 Eu3 O3 74.76(19) . 2 ? O80 Eu3 O3 149.57(17) 2 2 ? O110 Eu3 O3 131.88(18) . 2 ? O110 Eu3 O3 88.47(17) 2 2 ? O120 Eu3 O3 73.34(14) 2 2 ? O120 Eu3 O3 155.27(13) . 2 ? O70 Eu3 O3 85.4(2) . . ? O70 Eu3 O3 133.1(2) 2 . ? O80 Eu3 O3 149.57(17) . . ? O80 Eu3 O3 74.76(19) 2 . ? O110 Eu3 O3 88.47(17) . . ? O110 Eu3 O3 131.88(18) 2 . ? O120 Eu3 O3 155.27(13) 2 . ? O120 Eu3 O3 73.34(14) . . ? O3 Eu3 O3 107.38(8) 2 . ? O70 Eu3 O2 152.7(2) . 2 ? O70 Eu3 O2 73.2(2) 2 2 ? O80 Eu3 O2 134.01(19) . 2 ? O80 Eu3 O2 84.36(17) 2 2 ? O110 Eu3 O2 155.50(17) . 2 ? O110 Eu3 O2 74.21(18) 2 2 ? O120 Eu3 O2 129.32(13) 2 2 ? O120 Eu3 O2 89.13(13) . 2 ? O3 Eu3 O2 68.69(6) 2 2 ? O3 Eu3 O2 70.45(6) . 2 ? O70 Eu3 O2 73.2(2) . . ? O70 Eu3 O2 152.7(2) 2 . ? O80 Eu3 O2 84.36(17) . . ? O80 Eu3 O2 134.01(19) 2 . ? O110 Eu3 O2 74.21(18) . . ? O110 Eu3 O2 155.50(17) 2 . ? O120 Eu3 O2 89.13(13) 2 . ? O120 Eu3 O2 129.32(13) . . ? O3 Eu3 O2 70.45(6) 2 . ? O3 Eu3 O2 68.69(6) . . ? O2 Eu3 O2 107.78(8) 2 . ? Eu2 O1 Eu2 161.80(11) . 2 ? Eu2 O1 Eu1 88.855(18) . 2 ? Eu2 O1 Eu1 88.133(18) 2 2 ? Eu2 O1 Eu1 88.133(18) . . ? Eu2 O1 Eu1 88.855(18) 2 . ? Eu1 O1 Eu1 160.87(10) 2 . ? Eu2 O1 H1O 99.10 . . ? Eu2 O1 H1O 99.10 2 . ? Eu1 O1 H1O 99.57 2 . ? Eu1 O1 H1O 99.57 . . ? Eu2 O2 Eu1 99.04(7) . . ? Eu2 O2 Eu3 108.18(6) . . ? Eu1 O2 Eu3 108.89(7) . . ? Eu2 O2 H2O 113.2 . . ? Eu1 O2 H2O 113.2 . . ? Eu3 O2 H2O 113.2 . . ? Eu1 O3 Eu2 99.22(7) . 2 ? Eu1 O3 Eu3 110.52(7) . . ? Eu2 O3 Eu3 107.39(6) 2 . ? Eu1 O3 H3O 112.9 . . ? Eu2 O3 H3O 112.9 2 . ? Eu3 O3 H3O 112.9 . . ? C20 C1 C10 123.1(3) . . ? C20 C1 H1 118.4 . . ? C10 C1 H1 118.4 . . ? O10 C10 C1 124.5(3) . . ? O10 C10 C11 115.3(3) . . ? C1 C10 C11 120.1(3) . . ? C10 O10 Eu2 134.91(18) . . ? C12 C11 C16 117.9(3) . . ? C12 C11 C10 119.1(3) . . ? C16 C11 C10 123.1(3) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.3(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? O14 C14 C15 124.4(3) . . ? O14 C14 C13 115.8(3) . . ? C15 C14 C13 119.8(3) . . ? C14 O14 C17 117.8(3) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C11 121.6(3) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? O14 C17 C18 108.7(3) . . ? O14 C17 H17A 110 . . ? C18 C17 H17A 110 . . ? O14 C17 H17B 110 . . ? C18 C17 H17B 110 . . ? H17A C17 H17B 108.3 . . ? C19 C18 C17 125.8(4) . . ? C19 C18 H18 117.1 . . ? C17 C18 H18 117.1 . . ? C18 C19 H19A 120 . . ? C18 C19 H19B 120 . . ? H19A C19 H19B 120 . . ? O20 C20 C1 124.6(3) . . ? O20 C20 C21 115.1(3) . . ? C1 C20 C21 120.3(3) . . ? C20 O20 Eu2 135.99(18) . . ? C26 C21 C22 117.3(3) . . ? C26 C21 C20 123.6(3) . . ? C22 C21 C20 118.9(3) . . ? C23 C22 C21 121.8(3) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? O24 C24 C23 123.1(4) . . ? O24 C24 C25 116.9(3) . . ? C23 C24 C25 120.0(3) . . ? C24 O24 C27 119.5(3) . . ? C24 C25 C26 120.3(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 120.8(3) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? O24 C27 C28' 134.7(18) . . ? O24 C27 C28 108.3(5) . . ? O24 C27 H27A 110 . . ? C28 C27 H27A 110 . . ? O24 C27 H27B 110 . . ? C28 C27 H27B 110 . . ? H27A C27 H27B 108.4 . . ? O24 C27 H27C 103.5 . . ? C28' C27 H27C 103.5 . . ? C28 C27 H27C 120.2 . . ? H27B C27 H27C 104.3 . . ? O24 C27 H27D 103.5 . . ? C28' C27 H27D 103.5 . . ? C28 C27 H27D 114.2 . . ? H27C C27 H27D 105.3 . . ? C29 C28 C27 122.1(9) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C28 C29 H29A 120 . . ? C28 C29 H29B 120 . . ? H29A C29 H29B 120 . . ? C29' C28' C27 138(3) . . ? C29' C28' H28' 111.2 . . ? C27 C28' H28' 111.2 . . ? C28' C29' H29C 120 . . ? C28' C29' H29D 120 . . ? H29C C29' H29D 120 . . ? C40 C2 C30 124.6(3) . . ? C40 C2 H2 117.7 . . ? C30 C2 H2 117.7 . . ? O30 C30 C2 123.5(3) . . ? O30 C30 C31 117.3(3) . . ? C2 C30 C31 119.2(3) . . ? C30 O30 Eu1 132.94(18) . . ? C32 C31 C36 117.4(3) . . ? C32 C31 C30 119.8(3) . . ? C36 C31 C30 122.6(3) . . ? C33 C32 C31 122.0(3) . . ? C33 C32 H32 119 . . ? C31 C32 H32 119 . . ? C34 C33 C32 119.0(3) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 120.3(3) . . ? C33 C34 O34 124.8(3) . . ? C35 C34 O34 114.9(3) . . ? C34 O34 C37 119.8(3) . . ? C36 C35 C34 120.3(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 120.8(3) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? O34 C37 C38 111.6(4) . . ? O34 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? O34 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 108 . . ? C39 C38 C37 123.9(5) . . ? C39 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? C38 C39 H39A 120 . . ? C38 C39 H39B 120 . . ? H39A C39 H39B 120 . . ? O40 C40 C2 122.8(3) . . ? O40 C40 C41 114.9(2) . . ? C2 C40 C41 122.3(2) . . ? C40 O40 Eu1 125.24(15) . . ? C40 O40 Eu2 122.96(17) . . ? Eu1 O40 Eu2 95.50(6) . . ? C42 C41 C46 117.6(3) . . ? C42 C41 C40 119.4(2) . . ? C46 C41 C40 123.0(2) . . ? C43 C42 C41 121.8(3) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 C44 119.8(3) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? O44 C44 C43 123.8(3) . . ? O44 C44 C45 117.0(3) . . ? C43 C44 C45 119.2(3) . . ? C44 O44 C47 118.9(3) . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 121.0(3) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? O44 C47 C48' 111.3(10) . . ? O44 C47 C48 109.8(7) . . ? O44 C47 H47A 109.7 . . ? C48' C47 H47A 111.9 . . ? C48 C47 H47A 109.7 . . ? O44 C47 H47B 109.7 . . ? C48' C47 H47B 105.8 . . ? C48 C47 H47B 109.7 . . ? H47A C47 H47B 108.2 . . ? O44 C47 H47C 109 . . ? C48' C47 H47C 125.7 . . ? C48 C47 H47C 124.2 . . ? O44 C47 H47D 110.7 . . ? C48' C47 H47D 89.9 . . ? C48 C47 H47D 93.8 . . ? H47C C47 H47D 108.1 . . ? C49 C48 C47 128.9(13) . . ? C49 C48 H48 115.5 . . ? C47 C48 H48 115.5 . . ? C48 C49 H49A 120 . . ? C48 C49 H49B 120 . . ? H49A C49 H49B 120 . . ? C49' C48' C47 124.0(17) . . ? C49' C48' H48' 118 . . ? C47 C48' H48' 118 . . ? C48' C49' H49C 120 . . ? C48' C49' H49D 120 . . ? H49C C49' H49D 120 . . ? C60 C3 C50 124.5(2) . . ? C60 C3 H3 117.8 . . ? C50 C3 H3 117.8 . . ? O50 C50 C3 123.7(3) . . ? O50 C50 C51 116.1(3) . . ? C3 C50 C51 120.2(2) . . ? C50 O50 Eu1 137.64(18) . . ? C52 C51 C56 117.4(3) . . ? C52 C51 C50 118.5(2) . . ? C56 C51 C50 124.0(3) . . ? C53 C52 C51 121.3(3) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C54 C53 C52 120.3(3) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C55 C54 C53 119.5(3) . . ? C55 C54 O54 125.4(3) . . ? C53 C54 O54 115.0(3) . . ? C54 O54 C57 117.6(3) . . ? C54 C55 C56 120.3(3) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C55 C56 C51 121.1(3) . . ? C55 C56 H56 119.4 . . ? C51 C56 H56 119.4 . . ? O54 C57 C58 107.0(4) . . ? O54 C57 H57A 110.3 . . ? C58 C57 H57A 110.3 . . ? O54 C57 H57B 110.3 . . ? C58 C57 H57B 110.3 . . ? H57A C57 H57B 108.6 . . ? C59 C58 C57 128.4(7) . . ? C59 C58 H58 115.8 . . ? C57 C58 H58 115.8 . . ? C59' C58 H58' 101.5 . . ? C57 C58 H58' 103.7 . . ? C58 C59 H59A 120 . . ? C58 C59 H59B 120 . . ? H59A C59 H59B 120 . . ? C58 C59' H59C 120 . . ? C58 C59' H59D 120 . . ? H59C C59' H59D 120 . . ? O60 C60 C3 124.1(3) . . ? O60 C60 C61 115.5(3) . . ? C3 C60 C61 120.3(2) . . ? C60 O60 Eu1 136.94(18) . . ? C62 C61 C66 117.5(3) . . ? C62 C61 C60 119.3(3) . . ? C66 C61 C60 123.2(3) . . ? C61 C62 C63 121.9(3) . . ? C61 C62 H62 119.1 . . ? C63 C62 H62 119.1 . . ? C64 C63 C62 119.1(4) . . ? C64 C63 H63 120.5 . . ? C62 C63 H63 120.5 . . ? O64 C64 C65 115.8(4) . . ? O64 C64 C63 124.2(4) . . ? C65 C64 C63 120.0(4) . . ? C66 C65 C64 120.1(4) . . ? C66 C65 H65 120 . . ? C64 C65 H65 120 . . ? C65 C66 C61 121.2(4) . . ? C65 C66 H66 119.4 . . ? C61 C66 H66 119.4 . . ? C67 O64 C64 118.8(4) . . ? O64 C67 C68 103.2(4) . . ? O64 C67 H67A 111.1 . . ? C68 C67 H67A 111.1 . . ? O64 C67 H67B 111.1 . . ? C68 C67 H67B 111.1 . . ? H67A C67 H67B 109.1 . . ? C69 C68 C67 121.0(6) . . ? C69 C68 H68 119.5 . . ? C67 C68 H68 119.5 . . ? C68 C69 H69A 120 . . ? C68 C69 H69B 120 . . ? H69A C69 H69B 120 . . ? C70 C4 C80 120.9(7) . . ? C70 C4 H4 119.6 . . ? C80 C4 H4 119.6 . . ? O70 C70 C4 128.1(7) . . ? O70 C70 C71 113.1(7) . . ? C4 C70 C71 118.8(6) . . ? C70 O70 Eu3 127.5(7) . . ? C76 C71 C72 117.4(6) . . ? C76 C71 C70 124.1(7) . . ? C72 C71 C70 118.4(6) . . ? C73 C72 C71 121.1(6) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C74 121.7(7) . . ? C72 C73 H73 119.1 . . ? C74 C73 H73 119.1 . . ? O74 C74 C75 126.1(7) . . ? O74 C74 C73 116.1(7) . . ? C75 C74 C73 117.8(6) . . ? C74 O74 C77 119.8(6) . . ? C74 C75 C76 120.5(8) . . ? C74 C75 H75 119.8 . . ? C76 C75 H75 119.8 . . ? C71 C76 C75 121.5(7) . . ? C71 C76 H76 119.3 . . ? C75 C76 H76 119.3 . . ? O74 C77 C78 113.2(8) . . ? O74 C77 H77A 108.9 . . ? C78 C77 H77A 108.9 . . ? O74 C77 H77B 108.9 . . ? C78 C77 H77B 108.9 . . ? H77A C77 H77B 107.8 . . ? C79 C78 C77 124.9(12) . . ? C79 C78 H78 117.5 . . ? C77 C78 H78 117.5 . . ? C78 C79 H79A 120 . . ? C78 C79 H79B 120 . . ? H79A C79 H79B 120 . . ? O80 C80 C4 125.1(7) . . ? O80 C80 C81 116.3(6) . . ? C4 C80 C81 118.5(6) . . ? C80 O80 Eu3 131.1(5) . . ? C82 C81 C86 115.6(7) . . ? C82 C81 C80 119.5(6) . . ? C86 C81 C80 124.8(6) . . ? C83 C82 C81 123.4(8) . . ? C83 C82 H82 118.3 . . ? C81 C82 H82 118.3 . . ? C84 C83 C82 118.2(7) . . ? C84 C83 H83 120.9 . . ? C82 C83 H83 120.9 . . ? O84 C84 C83 121.7(7) . . ? O84 C84 C85 118.2(7) . . ? C83 C84 C85 119.9(8) . . ? C84 O84 C87 121.7(8) . . ? C86 C85 C84 120.5(8) . . ? C86 C85 H85 119.7 . . ? C84 C85 H85 119.7 . . ? C85 C86 C81 122.3(7) . . ? C85 C86 H86 118.9 . . ? C81 C86 H86 118.9 . . ? O84 C87 C88 104.7(8) . . ? O84 C87 H87A 110.8 . . ? C88 C87 H87A 110.8 . . ? O84 C87 H87B 110.8 . . ? C88 C87 H87B 110.8 . . ? H87A C87 H87B 108.9 . . ? C89 C88 C87 124.1(13) . . ? C89 C88 H88 118 . . ? C87 C88 H88 118 . . ? C88 C89 H89A 120 . . ? C88 C89 H89B 120 . . ? H89A C89 H89B 120 . . ? C100 C5 C90 125.0(2) . . ? C100 C5 H5 117.5 . . ? C90 C5 H5 117.5 . . ? O90 C90 C5 124.3(3) . . ? O90 C90 C91 115.9(3) . . ? C5 C90 C91 119.8(2) . . ? C90 O90 Eu2 132.71(18) . . ? C92 C91 C96 118.8(3) . . ? C92 C91 C90 123.1(3) . . ? C96 C91 C90 118.0(3) . . ? C91 C92 C93 121.0(3) . . ? C91 C92 H92 119.5 . . ? C93 C92 H92 119.5 . . ? C94 C93 C92 119.1(3) . . ? C94 C93 H93 120.5 . . ? C92 C93 H93 120.5 . . ? O94 C94 C93 124.9(3) . . ? O94 C94 C95 114.3(4) . . ? C93 C94 C95 120.8(3) . . ? C94 O94 C97 117.5(4) . . ? C96 C95 C94 119.6(4) . . ? C96 C95 H95 120.2 . . ? C94 C95 H95 120.2 . . ? C95 C96 C91 120.7(3) . . ? C95 C96 H96 119.7 . . ? C91 C96 H96 119.7 . . ? O94 C97 C98 101.1(4) . . ? O94 C97 H97A 111.6 . . ? C98 C97 H97A 111.6 . . ? O94 C97 H97B 111.6 . . ? C98 C97 H97B 111.6 . . ? H97A C97 H97B 109.4 . . ? C99 C98 C97 124.1(7) . . ? C99 C98 H98 118 . . ? C97 C98 H98 118 . . ? C98 C99 H99A 120 . . ? C98 C99 H99B 120 . . ? H99A C99 H99B 120 . . ? O100 C100 C5 123.1(2) . . ? O100 C100 C101 116.1(2) . . ? C5 C100 C101 120.8(2) . . ? C100 O100 Eu2 123.83(15) . . ? C100 O100 Eu1 126.81(15) . 2 ? Eu2 O100 Eu1 95.87(6) . 2 ? C102 C101 C106 117.4(3) . . ? C102 C101 C100 119.8(3) . . ? C106 C101 C100 122.8(3) . . ? C101 C102 C103 122.1(3) . . ? C101 C102 H102 119 . . ? C103 C102 H102 119 . . ? C104 C103 C102 119.4(3) . . ? C104 C103 H103 120.3 . . ? C102 C103 H103 120.3 . . ? C103 C104 O104 123.9(4) . . ? C103 C104 C105 119.8(3) . . ? O104 C104 C105 116.3(3) . . ? C104 O104 C107 118.6(3) . . ? C104 C105 C106 120.7(4) . . ? C104 C105 H105 119.7 . . ? C106 C105 H105 119.7 . . ? C105 C106 C101 120.6(4) . . ? C105 C106 H106 119.7 . . ? C101 C106 H106 119.7 . . ? O104 C107 C108 100.1(9) . . ? O104 C107 C10A 113.7(6) . . ? O104 C107 H10A 111.8 . . ? C108 C107 H10A 111.8 . . ? C10A C107 H10A 111.8 . . ? O104 C107 H10B 111.8 . . ? C108 C107 H10B 111.8 . . ? C10A C107 H10B 97.4 . . ? H10A C107 H10B 109.5 . . ? O104 C107 H10F 110.2 . . ? C108 C107 H10F 97.1 . . ? C10A C107 H10F 99.5 . . ? O104 C107 H10G 112.8 . . ? C108 C107 H10G 126.2 . . ? C10A C107 H10G 110.8 . . ? H10F C107 H10G 109 . . ? C109 C108 C107 140.7(19) . . ? C109 C108 H108 109.7 . . ? C107 C108 H108 109.7 . . ? C108 C109 H10C 120 . . ? C108 C109 H10D 120 . . ? H10C C109 H10D 120 . . ? C10B C10A C107 116.0(9) . . ? C10B C10A H10E 122 . . ? C107 C10A H10E 122 . . ? C10A C10B H10H 120 . . ? C10A C10B H10I 120 . . ? H10H C10B H10I 120 . . ? C110 C6 C120 123.4(4) . . ? C110 C6 H6 118.3 . . ? C120 C6 H6 118.3 . . ? O110 C110 C6 125.0(5) . . ? O110 C110 C111 114.5(5) . . ? C6 C110 C111 120.5(4) . . ? C110 O110 Eu3 128.4(5) . . ? C116 C111 C112 117.7(4) . . ? C116 C111 C110 118.0(4) . . ? C112 C111 C110 124.2(4) . . ? C113 C112 C111 120.7(4) . . ? C113 C112 H112 119.6 . . ? C111 C112 H112 119.6 . . ? C114 C113 C112 120.5(5) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C113 C114 O114 124.6(5) . . ? C113 C114 C115 119.2(5) . . ? O114 C114 C115 116.2(5) . . ? C114 O114 C117 117.7(4) . . ? C116 C115 C114 120.1(5) . . ? C116 C115 H115 119.9 . . ? C114 C115 H115 119.9 . . ? C115 C116 C111 121.6(5) . . ? C115 C116 H116 119.2 . . ? C111 C116 H116 119.2 . . ? O114 C117 C118 106.3(5) . . ? O114 C117 H11A 110.5 . . ? C118 C117 H11A 110.5 . . ? O114 C117 H11B 110.5 . . ? C118 C117 H11B 110.5 . . ? H11A C117 H11B 108.7 . . ? C119 C118 C117 123.4(8) . . ? C119 C118 H118 118.3 . . ? C117 C118 H118 118.3 . . ? C118 C119 H11C 120 . . ? C118 C119 H11D 120 . . ? H11C C119 H11D 120 . . ? O120 C120 C6 125.3(5) . . ? O120 C120 C121 115.3(5) . . ? C6 C120 C121 119.2(4) . . ? C120 O120 Eu3 129.8(4) . . ? C122 C121 C126 117.9(5) . . ? C122 C121 C120 119.3(5) . . ? C126 C121 C120 122.8(5) . . ? C123 C122 C121 121.4(5) . . ? C123 C122 H122 119.3 . . ? C121 C122 H122 119.3 . . ? C122 C123 C124 119.2(5) . . ? C122 C123 H123 120.4 . . ? C124 C123 H123 120.4 . . ? C125 C124 C123 120.3(5) . . ? C125 C124 O124 124.6(5) . . ? C123 C124 O124 115.0(5) . . ? C124 O124 C127 116.5(5) . . ? C126 C125 C124 119.8(5) . . ? C126 C125 H125 120.1 . . ? C124 C125 H125 120.1 . . ? C125 C126 C121 121.1(5) . . ? C125 C126 H126 119.5 . . ? C121 C126 H126 119.5 . . ? O124 C127 C128 111.1(6) . . ? O124 C127 H12A 109.4 . . ? C128 C127 H12A 109.4 . . ? O124 C127 H12B 109.4 . . ? C128 C127 H12B 109.4 . . ? H12A C127 H12B 108 . . ? C129 C128 C127 128.5(7) . . ? C129 C128 H128 115.8 . . ? C127 C128 H128 115.8 . . ? C128 C129 H12C 120 . . ? C128 C129 H12D 120 . . ? H12C C129 H12D 120 . . ? C216 C211 C212 119.3(5) . . ? C216 C211 C217 119.6(7) . . ? C212 C211 C217 121.0(6) . . ? C213 C212 C211 116.1(6) . . ? C213 C212 H212 122 . . ? C211 C212 H212 122 . . ? C212 C213 C214 126.7(7) . . ? C212 C213 H213 116.6 . . ? C214 C213 H213 116.6 . . ? C213 C214 C215 115.1(7) . . ? C213 C214 H214 122.4 . . ? C215 C214 H214 122.4 . . ? C214 C215 C216 123.5(6) . . ? C214 C215 H215 118.3 . . ? C216 C215 H215 118.3 . . ? C215 C216 C211 118.2(6) . . ? C215 C216 H216 120.9 . . ? C211 C216 H216 120.9 . . ? C211 C217 H21A 109.5 . . ? C211 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? C211 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C316 C311 C312 120.5(6) . . ? C316 C311 C317 122.2(7) . . ? C312 C311 C317 117.2(6) . . ? C313 C312 C311 121.4(7) . . ? C313 C312 H312 119.3 . . ? C311 C312 H312 119.3 . . ? C312 C313 C314 115.9(7) . . ? C312 C313 H313 122.1 . . ? C314 C313 H313 122.1 . . ? C315 C314 C313 124.5(7) . . ? C315 C314 H314 117.8 . . ? C313 C314 H314 117.8 . . ? C314 C315 C316 118.4(7) . . ? C314 C315 H315 120.8 . . ? C316 C315 H315 120.8 . . ? C311 C316 C315 119.2(7) . . ? C311 C316 H316 120.4 . . ? C315 C316 H316 120.4 . . ? C311 C317 H31A 109.5 . . ? C311 C317 H31B 109.5 . . ? H31A C317 H31B 109.5 . . ? C311 C317 H31C 109.5 . . ? H31A C317 H31C 109.5 . . ? H31B C317 H31C 109.5 . . ? #===END # Attachment '- mxm15.cif' data_mxm15 _database_code_depnum_ccdc_archive 'CCDC 779682' #TrackingRef '- mxm15.cif' _audit_creation_date 2010-03-29T08:35:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C238 H227 O45 Tb5' _chemical_formula_moiety 'C210 H195 Tb5 O45, 4(C7 H8)' _chemical_formula_weight 4601.8 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall -C_2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.7195(10) _cell_length_b 17.7608(6) _cell_length_c 32.6347(6) _cell_angle_alpha 90 _cell_angle_beta 95.464(2) _cell_angle_gamma 90 _cell_volume 20609.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25052 _cell_measurement_theta_min 3.3908 _cell_measurement_theta_max 32.0807 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description slab _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9360 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.0895 -1 0 0 0.0825 0 0 1 0.2629 0 0 -1 0.0637 0 -1 0 0.0415 0 1 0 0.0677 41 -2 23 0.112 49 2 -15 0.1066 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.773 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.834 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0193397309 _diffrn_orient_matrix_ub_12 0.0034299385 _diffrn_orient_matrix_ub_13 -0.0069030204 _diffrn_orient_matrix_ub_21 0.0013584242 _diffrn_orient_matrix_ub_22 0.0397153984 _diffrn_orient_matrix_ub_23 0.0018650627 _diffrn_orient_matrix_ub_31 0.004558821 _diffrn_orient_matrix_ub_32 0.00247516 _diffrn_orient_matrix_ub_33 -0.0206448571 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_unetI/netI 0.1343 _diffrn_reflns_number 118092 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 32.17 _diffrn_reflns_theta_full 31 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.937 _reflns_number_total 34029 _reflns_number_gt 17226 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. The terminal groups on many of the long chains were modelled as being disordered over two sets of sites with all occupancies set at 0.5 after trial refinement found these to be not significantly different. Geometries of the disordered atoms were restrained to ideal values with ADP's also restrained. Geometries of the two toluene solvent molecules were restrained to ideal values. ; _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^)+(0.0489P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 34029 _refine_ls_number_parameters 1547 _refine_ls_number_restraints 522 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 3.261 _refine_diff_density_min -2.288 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Tb1 Tb 0.011806(5) 0.942100(12) 0.329275(5) 0.02348(4) Uani 1 1 d . . . Tb2 Tb 0.068546(5) 0.940309(12) 0.245128(5) 0.02360(4) Uani 1 1 d . . . Tb3 Tb 0 1.107213(16) 0.25 0.02302(6) Uani 1 2 d S . . O1 O 0 0.9165(2) 0.25 0.0242(9) Uani 1 2 d SD . . O2 O 0.04489(6) 1.02596(15) 0.28990(7) 0.0241(6) Uani 1 1 d . . . H2O H 0.065 1.0546 0.3067 0.029 Uiso 1 1 calc R . . O3 O -0.03117(7) 1.02704(15) 0.29603(7) 0.0244(6) Uani 1 1 d . . . H3O H -0.0458 1.0558 0.3155 0.029 Uiso 1 1 calc R . . C1 C 0.17063(11) 0.9058(3) 0.27509(12) 0.0378(11) Uani 1 1 d . . . H1 H 0.1971 0.8993 0.2794 0.045 Uiso 1 1 calc R . . C10 C 0.15580(11) 0.9760(3) 0.28362(12) 0.0359(10) Uani 1 1 d D . . O10 O 0.12079(7) 0.99171(17) 0.28041(8) 0.0366(7) Uani 1 1 d D . . C11 C 0.18101(11) 1.0387(3) 0.29955(13) 0.0403(12) Uani 1 1 d D . . C12 C 0.16703(13) 1.0954(3) 0.32258(18) 0.0736(18) Uani 1 1 d D . . H12 H 0.1413 1.0942 0.3276 0.088 Uiso 1 1 calc R . . C13 C 0.18944(14) 1.1538(4) 0.33867(19) 0.089(2) Uani 1 1 d D . . H13 H 0.1796 1.1909 0.3557 0.107 Uiso 1 1 calc R . . C14 C 0.22666(13) 1.1573(3) 0.32953(15) 0.0595(15) Uani 1 1 d D . . O14 O 0.24662(9) 1.2190(2) 0.34581(11) 0.0747(12) Uani 1 1 d D . . C15 C 0.24117(12) 1.1025(3) 0.30578(14) 0.0518(13) Uani 1 1 d D . . H15 H 0.2664 1.1054 0.2991 0.062 Uiso 1 1 calc R . . C16 C 0.21840(12) 1.0432(3) 0.29179(14) 0.0454(12) Uani 1 1 d D . . H16 H 0.2287 1.0043 0.2764 0.054 Uiso 1 1 calc RD . . C17 C 0.28297(13) 1.2308(3) 0.33245(17) 0.0601(15) Uani 1 1 d . . . H17A H 0.2813 1.2328 0.302 0.072 Uiso 1 1 calc R . . H17B H 0.2999 1.1889 0.3419 0.072 Uiso 1 1 calc R . . C18 C 0.29767(16) 1.3026(4) 0.3500(2) 0.078(2) Uani 1 1 d . . . H18 H 0.3214 1.3186 0.3422 0.094 Uiso 1 1 calc R . . C19 C 0.28169(18) 1.3458(4) 0.3747(2) 0.104(3) Uani 1 1 d . . . H19A H 0.2579 1.3323 0.3834 0.125 Uiso 1 1 calc R . . H19B H 0.2936 1.3911 0.3842 0.125 Uiso 1 1 calc R . . C20 C 0.14869(11) 0.8440(3) 0.26049(11) 0.0336(10) Uani 1 1 d . . . O20 O 0.11399(7) 0.84849(16) 0.24766(7) 0.0303(7) Uani 1 1 d . . . C21 C 0.16515(11) 0.7663(3) 0.26058(12) 0.0363(11) Uani 1 1 d . . . C22 C 0.14547(12) 0.7099(3) 0.23821(13) 0.0404(11) Uani 1 1 d . . . H22 H 0.1233 0.7226 0.2212 0.048 Uiso 1 1 calc R . . C23 C 0.15744(14) 0.6354(3) 0.24005(14) 0.0482(13) Uani 1 1 d . . . H23 H 0.1435 0.5976 0.2246 0.058 Uiso 1 1 calc R . . C24 C 0.18980(14) 0.6169(3) 0.26456(15) 0.0526(14) Uani 1 1 d . A . O24 O 0.20164(11) 0.5437(2) 0.26726(12) 0.0695(11) Uani 1 1 d . . . C25 C 0.20983(14) 0.6713(3) 0.28624(16) 0.0570(15) Uani 1 1 d . . . H25 H 0.2321 0.6582 0.3029 0.068 Uiso 1 1 calc R A . C26 C 0.19799(12) 0.7455(3) 0.28422(14) 0.0483(13) Uani 1 1 d . A . H26 H 0.2125 0.7828 0.2992 0.058 Uiso 1 1 calc R . . C27 C 0.1815(3) 0.4822(6) 0.2522(3) 0.062(3) Uani 0.5 1 d PDU A 1 H27A H 0.1781 0.4885 0.222 0.075 Uiso 0.5 1 calc PRD A 1 H27B H 0.1563 0.4869 0.262 0.075 Uiso 0.5 1 calc PR A 1 C28 C 0.1932(4) 0.4027(8) 0.2597(5) 0.102(4) Uani 0.5 1 d PDU A 1 H28 H 0.1754 0.3629 0.2593 0.123 Uiso 0.5 1 calc PR A 1 C29 C 0.2285(4) 0.3909(12) 0.2667(7) 0.124(4) Uani 0.5 1 d PDU A 1 H29A H 0.2457 0.4318 0.2669 0.149 Uiso 0.5 1 calc PR A 1 H29B H 0.2376 0.3411 0.2717 0.149 Uiso 0.5 1 calc PR A 1 C27' C 0.2344(5) 0.5278(7) 0.2918(4) 0.114(5) Uani 0.5 1 d PDU A 2 H27C H 0.2316 0.5426 0.3206 0.137 Uiso 0.5 1 calc PRD A 2 H27D H 0.2556 0.5567 0.2821 0.137 Uiso 0.5 1 calc PR A 2 C28' C 0.2426(5) 0.4436(8) 0.2898(5) 0.120(5) Uani 0.5 1 d PDU A 2 H28' H 0.2668 0.4243 0.299 0.144 Uiso 0.5 1 calc PR A 2 C29' C 0.2162(5) 0.3998(12) 0.2754(7) 0.124(4) Uani 0.5 1 d PDU A 2 H29C H 0.1921 0.4199 0.2663 0.149 Uiso 0.5 1 calc PR A 2 H29D H 0.2205 0.3472 0.2738 0.149 Uiso 0.5 1 calc PR A 2 C2 C 0.10402(12) 0.8506(3) 0.35574(12) 0.0362(10) Uani 1 1 d . . . H2 H 0.1239 0.8203 0.3682 0.043 Uiso 1 1 calc R . . C30 C 0.10137(11) 0.9260(3) 0.36993(11) 0.0332(10) Uani 1 1 d . . . O30 O 0.07178(7) 0.96511(16) 0.36522(7) 0.0304(7) Uani 1 1 d . . . C31 C 0.13473(12) 0.9621(3) 0.39333(12) 0.0382(11) Uani 1 1 d . . . C32 C 0.13027(13) 1.0256(3) 0.41737(13) 0.0411(11) Uani 1 1 d . . . H32 H 0.1057 1.0446 0.4194 0.049 Uiso 1 1 calc R . . C33 C 0.16029(14) 1.0616(3) 0.43825(14) 0.0517(13) Uani 1 1 d . . . H33 H 0.1564 1.1038 0.4552 0.062 Uiso 1 1 calc R . . C34 C 0.19638(14) 1.0357(3) 0.43431(17) 0.0585(15) Uani 1 1 d . . . O34 O 0.22891(11) 1.0647(2) 0.45389(13) 0.0833(13) Uani 1 1 d . . . C35 C 0.20153(14) 0.9725(3) 0.41040(16) 0.0628(16) Uani 1 1 d . . . H35 H 0.2262 0.954 0.4082 0.075 Uiso 1 1 calc R . . C36 C 0.17121(12) 0.9362(3) 0.38984(14) 0.0484(13) Uani 1 1 d . . . H36 H 0.1751 0.8935 0.3732 0.058 Uiso 1 1 calc R . . C37 C 0.2278(2) 1.1350(4) 0.4756(2) 0.093(2) Uani 1 1 d . . . H37A H 0.2507 1.1401 0.495 0.112 Uiso 1 1 calc R . . H37B H 0.2056 1.136 0.4916 0.112 Uiso 1 1 calc R . . C38 C 0.22566(18) 1.1990(5) 0.4456(2) 0.094(2) Uani 1 1 d . . . H38 H 0.241 1.1972 0.4234 0.113 Uiso 1 1 calc R . . C39 C 0.2026(2) 1.2600(5) 0.4486(2) 0.110(3) Uani 1 1 d . . . H39A H 0.1869 1.263 0.4705 0.132 Uiso 1 1 calc R . . H39B H 0.2022 1.2992 0.4288 0.132 Uiso 1 1 calc R . . C40 C 0.07978(10) 0.8180(3) 0.32504(11) 0.0318(10) Uani 1 1 d . . . O40 O 0.05414(7) 0.85816(15) 0.30285(7) 0.0257(6) Uani 1 1 d . . . C41 C 0.08101(11) 0.7372(3) 0.31468(12) 0.0340(10) Uani 1 1 d . . . C42 C 0.06158(11) 0.7108(2) 0.27800(12) 0.0337(10) Uani 1 1 d . . . H42 H 0.0483 0.7457 0.26 0.04 Uiso 1 1 calc R . . C43 C 0.06129(12) 0.6368(3) 0.26756(13) 0.0407(11) Uani 1 1 d . . . H43 H 0.0485 0.6208 0.2422 0.049 Uiso 1 1 calc R . . C44 C 0.07971(14) 0.5843(3) 0.29391(16) 0.0512(13) Uani 1 1 d . . . O44 O 0.07991(11) 0.5080(2) 0.28614(12) 0.0753(12) Uani 1 1 d . C . C45 C 0.09886(15) 0.6085(3) 0.33083(16) 0.0596(15) Uani 1 1 d . . . H45 H 0.1114 0.5732 0.3492 0.072 Uiso 1 1 calc R . . C46 C 0.09945(13) 0.6834(3) 0.34033(14) 0.0463(12) Uani 1 1 d . . . H46 H 0.1129 0.6994 0.3653 0.056 Uiso 1 1 calc R . . C47 C 0.0595(2) 0.4823(4) 0.2497(2) 0.107(2) Uani 1 1 d DU . . H47A H 0.0726 0.4962 0.2254 0.128 Uiso 0.5 1 calc PR B 1 H47B H 0.034 0.5048 0.2467 0.128 Uiso 0.5 1 calc PR B 1 H47C H 0.0639 0.5158 0.2263 0.128 Uiso 0.5 1 d PR B 2 H47D H 0.0322 0.4822 0.253 0.128 Uiso 0.5 1 d PR B 2 C48 C 0.0572(5) 0.3998(7) 0.2536(5) 0.097(3) Uiso 0.5 1 d PDU C 1 H48 H 0.078 0.3816 0.2712 0.116 Uiso 0.5 1 calc PR C 1 C49 C 0.0392(3) 0.3531(12) 0.2426(6) 0.177(6) Uiso 0.5 1 d PDU . 1 H49A H 0.0171 0.3624 0.2247 0.212 Uiso 0.5 1 calc PR . 1 H49B H 0.0455 0.3031 0.251 0.212 Uiso 0.5 1 calc PR . 1 C48' C 0.0702(5) 0.3986(8) 0.2447(5) 0.140(6) Uiso 0.5 1 d PDU C 2 H48' H 0.0704 0.3779 0.2179 0.168 Uiso 0.5 1 calc PR C 2 C49' C 0.0793(4) 0.3547(10) 0.2779(5) 0.121(5) Uiso 0.5 1 d PDU C 2 H49C H 0.0792 0.3751 0.3048 0.145 Uiso 0.5 1 calc PR C 2 H49D H 0.0858 0.3034 0.2743 0.145 Uiso 0.5 1 calc PR C 2 C3 C -0.01221(11) 0.9089(3) 0.43737(11) 0.0352(11) Uani 1 1 d . . . H3 H -0.0178 0.9012 0.465 0.042 Uiso 1 1 calc R . . C50 C -0.02464(10) 0.9760(3) 0.41793(11) 0.0309(10) Uani 1 1 d . . . O50 O -0.01714(7) 0.99505(16) 0.38217(7) 0.0307(7) Uani 1 1 d . . . C51 C -0.04870(11) 1.0304(3) 0.43916(12) 0.0323(10) Uani 1 1 d . . . C52 C -0.06620(12) 1.0882(3) 0.41669(13) 0.0443(12) Uani 1 1 d . . . H52 H -0.0616 1.0944 0.3887 0.053 Uiso 1 1 calc R . . C53 C -0.09024(14) 1.1376(3) 0.43383(14) 0.0585(15) Uani 1 1 d . . . H53 H -0.1025 1.1761 0.4174 0.07 Uiso 1 1 calc R . . C54 C -0.09651(14) 1.1312(3) 0.47446(15) 0.0561(15) Uani 1 1 d . . . O54 O -0.12050(11) 1.1851(3) 0.48926(11) 0.0806(13) Uani 1 1 d . . . C55 C -0.07936(13) 1.0746(3) 0.49790(13) 0.0453(13) Uani 1 1 d . . . H55 H -0.0836 1.0701 0.5261 0.054 Uiso 1 1 calc R . . C56 C -0.05574(12) 1.0236(3) 0.48057(12) 0.0390(11) Uani 1 1 d . . . H56 H -0.0443 0.9841 0.4969 0.047 Uiso 1 1 calc R . . C57 C -0.12456(18) 1.1877(4) 0.53148(18) 0.087(2) Uani 1 1 d . E . H57A H -0.0996 1.191 0.5474 0.104 Uiso 1 1 calc R . . H57B H -0.1374 1.1418 0.5401 0.104 Uiso 1 1 calc R . . C58 C -0.1474(2) 1.2556(5) 0.5389(2) 0.115(3) Uani 1 1 d DU . . H58 H -0.143 1.2987 0.5228 0.137 Uiso 0.5 1 calc PR D 1 H58' H -0.1726 1.2413 0.5304 0.137 Uiso 0.5 1 d PR D 2 C59 C -0.1720(4) 1.2630(10) 0.5642(3) 0.099(4) Uani 0.5 1 d PDU E 1 H59A H -0.1766 1.3111 0.5754 0.119 Uiso 0.5 1 calc PR E 1 H59B H -0.1858 1.2204 0.5719 0.119 Uiso 0.5 1 calc PR E 1 C59' C -0.1490(5) 1.3155(9) 0.5489(5) 0.121(5) Uani 0.5 1 d PDU E 2 H59C H -0.1663 1.3298 0.5679 0.145 Uiso 0.5 1 calc PR E 2 H59D H -0.1331 1.3522 0.5383 0.145 Uiso 0.5 1 calc PR E 2 C60 C 0.00779(11) 0.8523(3) 0.41903(11) 0.0319(10) Uani 1 1 d . . . O60 O 0.01592(8) 0.85465(16) 0.38184(7) 0.0327(7) Uani 1 1 d . . . C61 C 0.02077(13) 0.7840(3) 0.44267(12) 0.0422(11) Uani 1 1 d U . . C62 C 0.03443(14) 0.7238(3) 0.42249(14) 0.0490(13) Uani 1 1 d U . . H62 H 0.0367 0.7278 0.3938 0.059 Uiso 1 1 calc R . . C63 C 0.04509(16) 0.6574(3) 0.44246(16) 0.0637(15) Uani 1 1 d U . . H63 H 0.0537 0.6162 0.4274 0.076 Uiso 1 1 calc R . . C64 C 0.0432(2) 0.6512(4) 0.48424(18) 0.086(2) Uani 1 1 d U . . C65 C 0.0321(2) 0.7133(4) 0.50585(17) 0.093(2) Uani 1 1 d U . . H65 H 0.0323 0.711 0.535 0.111 Uiso 1 1 calc R . . C66 C 0.02098(17) 0.7782(3) 0.48532(14) 0.0647(16) Uani 1 1 d U . . H66 H 0.0132 0.8201 0.5005 0.078 Uiso 1 1 calc R . . O64 O 0.05155(18) 0.5884(3) 0.50683(15) 0.124(2) Uani 1 1 d U . . C67 C 0.0576(2) 0.5235(5) 0.4875(2) 0.113(3) Uani 1 1 d U . . H67A H 0.0817 0.5249 0.4749 0.135 Uiso 1 1 calc R . . H67B H 0.037 0.513 0.4657 0.135 Uiso 1 1 calc R . . C68 C 0.0586(3) 0.4635(5) 0.5219(4) 0.141(3) Uani 1 1 d U . . H68 H 0.0733 0.4746 0.547 0.169 Uiso 1 1 calc R . . C69 C 0.0430(3) 0.4059(6) 0.5198(4) 0.154(4) Uani 1 1 d U . . H69A H 0.0279 0.3925 0.4953 0.185 Uiso 1 1 calc R . . H69B H 0.0452 0.3724 0.5426 0.185 Uiso 1 1 calc R . . C4 C 0.0854(3) 1.1985(5) 0.3003(3) 0.043(2) Uani 0.5 1 d P F 1 H4 H 0.1092 1.2105 0.3145 0.051 Uiso 0.5 1 calc PR F 1 C70 C 0.0544(2) 1.1880(5) 0.3234(2) 0.043(2) Uani 0.5 1 d PD F 1 O70 O 0.0217(2) 1.1649(4) 0.3093(2) 0.0267(11) Uani 0.5 1 d PD F 1 C71 C 0.0611(3) 1.1915(6) 0.3697(2) 0.038(3) Uani 0.5 1 d PD F 1 C72 C 0.0372(3) 1.1483(6) 0.3910(2) 0.050(3) Uani 0.5 1 d PD F 1 H72 H 0.0174 1.121 0.3762 0.06 Uiso 0.5 1 calc PR F 1 C73 C 0.0417(3) 1.1443(6) 0.4337(2) 0.054(3) Uani 0.5 1 d PD F 1 H73 H 0.0249 1.1147 0.4479 0.064 Uiso 0.5 1 calc PR F 1 C74 C 0.0703(3) 1.1830(7) 0.4555(2) 0.048(3) Uani 0.5 1 d PD F 1 O74 O 0.0735(2) 1.1703(5) 0.49786(17) 0.074(2) Uani 0.5 1 d PD F 1 C75 C 0.0944(3) 1.2264(7) 0.4354(3) 0.050(4) Uani 0.5 1 d PD F 1 H75 H 0.1137 1.2545 0.4504 0.06 Uiso 0.5 1 calc PR F 1 C76 C 0.0900(3) 1.2287(7) 0.3922(3) 0.054(4) Uani 0.5 1 d PD F 1 H76 H 0.1075 1.2567 0.378 0.065 Uiso 0.5 1 calc PR F 1 C77 C 0.0858(4) 1.2303(9) 0.5237(3) 0.097(4) Uani 0.5 1 d PDU F 1 H77A H 0.0724 1.2284 0.5489 0.116 Uiso 0.5 1 calc PR F 1 H77B H 0.0792 1.2784 0.5095 0.116 Uiso 0.5 1 calc PR F 1 C78 C 0.1275(4) 1.2285(9) 0.5358(4) 0.102(4) Uani 0.5 1 d PDU F 1 H78 H 0.1401 1.1815 0.538 0.122 Uiso 0.5 1 calc PR F 1 C79 C 0.1458(5) 1.2880(10) 0.5430(4) 0.114(4) Uani 0.5 1 d PDU F 1 H79A H 0.1334 1.3354 0.5409 0.137 Uiso 0.5 1 calc PR F 1 H79B H 0.1722 1.2857 0.5506 0.137 Uiso 0.5 1 calc PR F 1 C80 C 0.0829(2) 1.1921(5) 0.2568(2) 0.041(2) Uani 0.5 1 d PD F 1 O80 O 0.05393(19) 1.1694(4) 0.2331(2) 0.0297(9) Uani 0.5 1 d PD F 1 C81 C 0.1161(2) 1.2072(6) 0.2335(2) 0.041(2) Uani 0.5 1 d PD F 1 C82 C 0.1102(3) 1.2156(10) 0.1914(3) 0.065(5) Uani 0.5 1 d PD F 1 H82 H 0.0857 1.2084 0.1779 0.078 Uiso 0.5 1 calc PR F 1 C83 C 0.1400(2) 1.2348(8) 0.1684(3) 0.072(4) Uani 0.5 1 d PD F 1 H83 H 0.1356 1.2474 0.1401 0.086 Uiso 0.5 1 calc PR F 1 C84 C 0.1756(3) 1.2348(11) 0.1879(4) 0.074(6) Uani 0.5 1 d PD F 1 O84 O 0.2072(2) 1.2584(6) 0.1694(3) 0.069(4) Uani 0.5 1 d PD F 1 C85 C 0.1819(3) 1.2228(9) 0.2295(3) 0.085(4) Uani 0.5 1 d PD F 1 H85 H 0.2068 1.2216 0.2426 0.102 Uiso 0.5 1 calc PR F 1 C86 C 0.1520(2) 1.2127(7) 0.2519(3) 0.070(4) Uani 0.5 1 d PD F 1 H86 H 0.1562 1.2093 0.2811 0.084 Uiso 0.5 1 calc PR F 1 C87 C 0.2035(3) 1.2768(8) 0.1273(3) 0.069(4) Uani 0.5 1 d PD F 1 H87A H 0.184 1.3159 0.1215 0.083 Uiso 0.5 1 calc PR F 1 H87B H 0.1962 1.2317 0.1105 0.083 Uiso 0.5 1 calc PR F 1 C88 C 0.2397(3) 1.3045(9) 0.1175(4) 0.089(6) Uani 0.5 1 d PD F 1 H88 H 0.2467 1.3543 0.1256 0.107 Uiso 0.5 1 calc PR F 1 C89 C 0.2625(4) 1.2659(9) 0.0986(5) 0.119(6) Uani 0.5 1 d PD F 1 H89A H 0.2561 1.2159 0.0902 0.143 Uiso 0.5 1 calc PR F 1 H89B H 0.2859 1.2869 0.093 0.143 Uiso 0.5 1 calc PR F 1 C5 C 0.09310(10) 0.8626(2) 0.14661(11) 0.0283(9) Uani 1 1 d . . . H5 H 0.1038 0.8357 0.1254 0.034 Uiso 1 1 calc R . . C90 C 0.10854(10) 0.9355(2) 0.15738(11) 0.0283(9) Uani 1 1 d . . . O90 O 0.10120(7) 0.97212(16) 0.18871(8) 0.0308(7) Uani 1 1 d . . . C91 C 0.13550(10) 0.9717(2) 0.13168(12) 0.0305(9) Uani 1 1 d . . . C92 C 0.13527(12) 0.9577(3) 0.08936(12) 0.0376(11) Uani 1 1 d . . . H92 H 0.1185 0.9214 0.0765 0.045 Uiso 1 1 calc R . . C93 C 0.15960(13) 0.9969(3) 0.06611(13) 0.0490(13) Uani 1 1 d . . . H93 H 0.1591 0.988 0.0374 0.059 Uiso 1 1 calc R . . C94 C 0.18411(14) 1.0479(3) 0.08451(15) 0.0545(14) Uani 1 1 d . . . O94 O 0.20884(10) 1.0914(3) 0.06443(11) 0.0756(12) Uani 1 1 d . . . C95 C 0.18509(13) 1.0618(3) 0.12652(15) 0.0534(13) Uani 1 1 d . . . H95 H 0.2025 1.0971 0.1393 0.064 Uiso 1 1 calc R . . C96 C 0.16055(12) 1.0238(3) 0.14970(13) 0.0424(12) Uani 1 1 d . . . H96 H 0.161 1.0339 0.1783 0.051 Uiso 1 1 calc R . . C97 C 0.20917(18) 1.0811(5) 0.02122(17) 0.094(3) Uani 1 1 d U . . H97A H 0.1842 1.0916 0.0066 0.113 Uiso 1 1 calc R . . H97B H 0.2169 1.0292 0.0147 0.113 Uiso 1 1 calc R . . C98 C 0.2389(2) 1.1398(5) 0.0097(2) 0.130(3) Uani 1 1 d U . . H98 H 0.2379 1.1884 0.0218 0.156 Uiso 1 1 calc R . . C99 C 0.2622(2) 1.1295(6) -0.0124(2) 0.144(4) Uani 1 1 d U . . H99A H 0.2642 1.0818 -0.0251 0.173 Uiso 1 1 calc R . . H99B H 0.2792 1.1687 -0.0176 0.173 Uiso 1 1 calc R . . C100 C 0.06434(11) 0.8287(2) 0.16428(11) 0.0294(9) Uani 1 1 d . . . O100 O 0.04340(7) 0.86286(15) 0.18941(7) 0.0252(6) Uani 1 1 d . . . C101 C 0.05519(11) 0.7488(2) 0.15637(11) 0.0320(10) Uani 1 1 d . . . C102 C 0.02249(12) 0.7165(3) 0.16969(12) 0.0366(10) Uani 1 1 d . . . H102 H 0.0063 0.7472 0.1841 0.044 Uiso 1 1 calc R . . C103 C 0.01301(14) 0.6423(3) 0.16273(13) 0.0449(12) Uani 1 1 d . . . H103 H -0.0092 0.6226 0.1726 0.054 Uiso 1 1 calc R . . C104 C 0.03522(17) 0.5971(3) 0.14186(15) 0.0559(14) Uani 1 1 d . . . O104 O 0.02791(13) 0.5226(2) 0.13209(12) 0.0818(13) Uani 1 1 d . H . C105 C 0.06818(19) 0.6262(3) 0.12921(17) 0.0768(19) Uani 1 1 d . . . H105 H 0.0844 0.5943 0.1156 0.092 Uiso 1 1 calc R . . C106 C 0.07797(15) 0.7004(3) 0.13597(15) 0.0564(14) Uani 1 1 d . . . H106 H 0.1006 0.719 0.1266 0.068 Uiso 1 1 calc R . . C107 C -0.0050(2) 0.4909(3) 0.1442(2) 0.083(2) Uani 1 1 d D . . H10A H -0.0258 0.5266 0.1368 0.099 Uiso 0.5 1 calc PR G 1 H10B H -0.0021 0.4865 0.1745 0.099 Uiso 0.5 1 calc PR G 1 H10F H -0.0274 0.5148 0.1293 0.099 Uiso 0.5 1 d PR G 2 H10G H -0.0065 0.4962 0.1743 0.099 Uiso 0.5 1 d PR G 2 C108 C -0.0166(5) 0.4161(8) 0.1270(5) 0.102(3) Uiso 0.5 1 d PD H 1 H108 H -0.0419 0.4003 0.128 0.122 Uiso 0.5 1 calc PR H 1 C109 C 0.0047(6) 0.3754(11) 0.1121(5) 0.132(5) Uiso 0.5 1 d PD H 1 H10C H 0.0301 0.3902 0.1108 0.159 Uiso 0.5 1 calc PR H 1 H10D H -0.0037 0.3279 0.1014 0.159 Uiso 0.5 1 calc PR H 1 C10A C -0.0076(5) 0.4093(8) 0.1312(5) 0.102(3) Uiso 0.5 1 d PD H 2 H10E H -0.0171 0.3704 0.1473 0.122 Uiso 0.5 1 calc PR H 2 C10B C 0.0043(5) 0.3990(13) 0.0967(5) 0.132(5) Uiso 0.5 1 d PD H 2 H10H H 0.0135 0.4403 0.0821 0.159 Uiso 0.5 1 calc PR H 2 H10I H 0.0041 0.3498 0.0852 0.159 Uiso 0.5 1 calc PR H 2 C6 C -0.0307(2) 1.2057(4) 0.3424(2) 0.0231(17) Uani 0.5 1 d P F 2 H6 H -0.0393 1.2184 0.3682 0.028 Uiso 0.5 1 calc PR F 2 C110 C 0.0074(2) 1.1939(4) 0.34081(19) 0.0277(18) Uani 0.5 1 d PDU F 2 O110 O 0.0223(2) 1.1843(4) 0.3067(2) 0.0267(11) Uani 0.5 1 d PDU F 2 C111 C 0.0350(2) 1.1990(4) 0.3783(2) 0.0212(16) Uani 0.5 1 d PDU F 2 C112 C 0.02432(19) 1.1916(4) 0.4179(2) 0.0241(17) Uani 0.5 1 d PD F 2 H112 H -0.0014 1.1834 0.4218 0.029 Uiso 0.5 1 calc PR F 2 C113 C 0.05079(19) 1.1961(5) 0.4517(2) 0.026(2) Uani 0.5 1 d PD F 2 H113 H 0.0431 1.1914 0.4787 0.032 Uiso 0.5 1 calc PR F 2 C114 C 0.0880(2) 1.2074(6) 0.4464(3) 0.024(2) Uani 0.5 1 d PD F 2 O114 O 0.11664(14) 1.2142(3) 0.47809(14) 0.0314(14) Uani 0.5 1 d PD F 2 C115 C 0.0993(3) 1.2145(6) 0.4071(3) 0.028(2) Uani 0.5 1 d PD F 2 H115 H 0.1249 1.2232 0.4033 0.033 Uiso 0.5 1 calc PR F 2 C116 C 0.0731(2) 1.2089(7) 0.3736(3) 0.032(3) Uani 0.5 1 d PD F 2 H116 H 0.081 1.2119 0.3467 0.038 Uiso 0.5 1 calc PR F 2 C117 C 0.1067(3) 1.2256(6) 0.5179(2) 0.038(2) Uani 0.5 1 d PDU F 2 H11A H 0.0927 1.1813 0.5268 0.045 Uiso 0.5 1 calc PR F 2 H11B H 0.0902 1.2703 0.5185 0.045 Uiso 0.5 1 calc PR F 2 C118 C 0.1414(3) 1.2369(6) 0.5461(3) 0.045(2) Uani 0.5 1 d PDU F 2 H118 H 0.1578 1.1951 0.5514 0.054 Uiso 0.5 1 calc PR F 2 C119 C 0.1507(3) 1.2995(6) 0.5638(3) 0.056(3) Uani 0.5 1 d PDU F 2 H11C H 0.135 1.3424 0.5592 0.067 Uiso 0.5 1 calc PR F 2 H11D H 0.1733 1.303 0.5816 0.067 Uiso 0.5 1 calc PR F 2 C120 C -0.05746(17) 1.2000(4) 0.3078(2) 0.0195(15) Uani 0.5 1 d PD F 2 O120 O -0.0495(2) 1.1813(5) 0.2710(2) 0.0297(9) Uani 0.5 1 d PD F 2 C121 C -0.0979(2) 1.2161(7) 0.3125(3) 0.028(2) Uani 0.5 1 d PD F 2 C122 C -0.12602(19) 1.1835(5) 0.2858(2) 0.0247(18) Uani 0.5 1 d PD F 2 H122 H -0.1191 1.1547 0.2632 0.03 Uiso 0.5 1 calc PR F 2 C123 C -0.1633(2) 1.1917(5) 0.2910(2) 0.034(2) Uani 0.5 1 d PD F 2 H123 H -0.1819 1.1683 0.2724 0.041 Uiso 0.5 1 calc PR F 2 C124 C -0.1738(2) 1.2340(9) 0.3233(4) 0.041(3) Uani 0.5 1 d PD F 2 O124 O -0.2125(2) 1.2287(6) 0.3303(2) 0.041(2) Uani 0.5 1 d PD F 2 C125 C -0.1474(2) 1.2668(6) 0.3513(3) 0.041(2) Uani 0.5 1 d PD F 2 H125 H -0.155 1.2938 0.3743 0.049 Uiso 0.5 1 calc PR F 2 C126 C -0.10898(19) 1.2598(5) 0.3452(2) 0.033(2) Uani 0.5 1 d PD F 2 H126 H -0.0905 1.2846 0.3633 0.04 Uiso 0.5 1 calc PR F 2 C127 C -0.2234(3) 1.2516(6) 0.3697(3) 0.052(3) Uani 0.5 1 d PD F 2 H12A H -0.2038 1.2363 0.3916 0.063 Uiso 0.5 1 calc PR F 2 H12B H -0.2472 1.2263 0.3749 0.063 Uiso 0.5 1 calc PR F 2 C128 C -0.2286(4) 1.3353(7) 0.3709(4) 0.069(4) Uani 0.5 1 d PD F 2 H128 H -0.233 1.3552 0.397 0.082 Uiso 0.5 1 calc PR F 2 C129 C -0.2281(3) 1.3836(6) 0.3423(3) 0.058(3) Uani 0.5 1 d PD F 2 H12C H -0.2238 1.3679 0.3153 0.07 Uiso 0.5 1 calc PR F 2 H12D H -0.2319 1.4353 0.3479 0.07 Uiso 0.5 1 calc PR F 2 C211 C 0.1845(2) 0.4775(5) 0.3981(2) 0.156(4) Uani 1 1 d D I . C212 C 0.1569(2) 0.4334(5) 0.3742(2) 0.142(4) Uani 1 1 d D . . C213 C 0.1256(2) 0.4099(6) 0.3933(3) 0.175(5) Uani 1 1 d D I . H213 H 0.1055 0.3886 0.3759 0.21 Uiso 1 1 calc RD . . C214 C 0.1207(4) 0.4142(10) 0.4336(3) 0.379(15) Uani 1 1 d D . . H214 H 0.0984 0.3982 0.4449 0.454 Uiso 1 1 calc R I . C215 C 0.1515(3) 0.4442(6) 0.4570(3) 0.184(6) Uani 1 1 d D I . H215 H 0.1533 0.4376 0.486 0.22 Uiso 1 1 calc R . . C216 C 0.1797(4) 0.4836(8) 0.4399(3) 0.276(10) Uani 1 1 d D . . H216 H 0.1961 0.5151 0.4569 0.332 Uiso 1 1 calc R I . C217 C 0.2098(4) 0.5309(8) 0.3804(4) 0.113(5) Uiso 0.5 1 d PD . . H21A H 0.2051 0.53 0.3503 0.169 Uiso 0.5 1 calc PR I . H21B H 0.2359 0.5166 0.3885 0.169 Uiso 0.5 1 calc PRD . . H21C H 0.2051 0.5817 0.3905 0.169 Uiso 0.5 1 calc PR . . C218 C 0.1513(6) 0.3908(13) 0.3335(5) 0.269(15) Uiso 0.5 1 d PD I 1 H21D H 0.1732 0.3987 0.318 0.404 Uiso 0.5 1 calc PR I 1 H21E H 0.1286 0.4096 0.3173 0.404 Uiso 0.5 1 calc PRD I 1 H21F H 0.1484 0.337 0.3389 0.404 Uiso 0.5 1 calc PRD I 1 C311 C 0.1367(2) 0.5344(7) 0.6299(3) 0.207(3) Uani 1 1 d DU . . C312 C 0.1684(3) 0.4876(7) 0.6357(3) 0.219(3) Uani 1 1 d DU . . H312 H 0.1742 0.4657 0.6621 0.263 Uiso 1 1 calc R . . C313 C 0.1914(3) 0.4715(7) 0.6058(3) 0.202(3) Uani 1 1 d DU . . H313 H 0.2127 0.4396 0.6107 0.242 Uiso 1 1 calc R . . C314 C 0.1817(3) 0.5045(7) 0.5677(3) 0.197(3) Uani 1 1 d DU . . H314 H 0.1962 0.494 0.5454 0.236 Uiso 1 1 calc R . . C315 C 0.1515(3) 0.5523(7) 0.5620(3) 0.204(3) Uani 1 1 d DU . . H315 H 0.1467 0.5763 0.536 0.245 Uiso 1 1 calc R . . C316 C 0.1277(3) 0.5673(7) 0.5919(3) 0.206(3) Uani 1 1 d DU . . H316 H 0.1062 0.5986 0.5867 0.247 Uiso 1 1 calc R . . C317 C 0.1120(3) 0.5507(7) 0.6641(3) 0.227(4) Uani 1 1 d DU . . H31A H 0.1253 0.5367 0.6906 0.34 Uiso 1 1 calc R . . H31B H 0.0887 0.5214 0.6595 0.34 Uiso 1 1 calc RD . . H31C H 0.1059 0.6045 0.6642 0.34 Uiso 1 1 calc RD . . H1O H 0 0.8709(11) 0.25 0.272 Uiso 1 2 d SD . . H211 H 0.2037(6) 0.496(2) 0.3868(5) 0.272 Uiso 0.5 1 d PD J 1 H212 H 0.1607(7) 0.421(2) 0.3490(5) 0.272 Uiso 0.5 1 d PD K 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02311(9) 0.02776(10) 0.01964(8) 0.00154(8) 0.00234(7) 0.00198(9) Tb2 0.01877(8) 0.02803(10) 0.02411(9) -0.00513(8) 0.00270(7) -0.00107(9) Tb3 0.02317(12) 0.02497(15) 0.02117(12) 0 0.00343(10) 0 O1 0.0180(17) 0.036(2) 0.0188(16) 0 0.0013(14) 0 O2 0.0199(13) 0.0269(14) 0.0252(12) -0.0008(11) -0.0001(10) -0.0022(11) O3 0.0254(13) 0.0239(14) 0.0248(13) 0.0018(11) 0.0069(11) 0.0043(12) C1 0.024(2) 0.048(3) 0.041(2) -0.005(2) 0.0019(18) 0.001(2) C10 0.029(2) 0.045(3) 0.035(2) -0.008(2) 0.0030(18) -0.007(2) O10 0.0221(13) 0.0449(19) 0.0420(15) -0.0155(14) -0.0011(12) -0.0052(14) C11 0.025(2) 0.053(3) 0.043(2) -0.012(2) 0.0019(18) -0.008(2) C12 0.034(2) 0.086(4) 0.105(4) -0.057(4) 0.029(3) -0.031(3) C13 0.041(3) 0.112(5) 0.119(5) -0.079(4) 0.033(3) -0.033(3) C14 0.035(3) 0.083(4) 0.059(3) -0.020(3) -0.002(2) -0.028(3) O14 0.047(2) 0.093(3) 0.086(3) -0.041(2) 0.0182(19) -0.043(2) C15 0.026(2) 0.067(4) 0.063(3) -0.007(3) 0.008(2) -0.012(3) C16 0.031(2) 0.046(3) 0.059(3) -0.005(2) 0.005(2) -0.006(2) C17 0.032(2) 0.066(4) 0.082(4) -0.011(3) 0.001(2) -0.022(3) C18 0.039(3) 0.088(5) 0.107(5) -0.026(4) 0.010(3) -0.021(3) C19 0.072(4) 0.108(6) 0.135(6) -0.046(5) 0.024(4) -0.057(4) C20 0.028(2) 0.046(3) 0.028(2) -0.0040(19) 0.0071(17) 0.002(2) O20 0.0213(13) 0.0374(17) 0.0319(14) -0.0077(12) 0.0011(11) 0.0018(13) C21 0.027(2) 0.046(3) 0.036(2) -0.003(2) 0.0062(18) 0.008(2) C22 0.032(2) 0.049(3) 0.040(2) -0.007(2) 0.0033(19) 0.006(2) C23 0.054(3) 0.042(3) 0.050(3) -0.004(2) 0.012(2) 0.014(2) C24 0.056(3) 0.045(3) 0.058(3) 0.006(2) 0.017(3) 0.025(3) O24 0.065(2) 0.052(3) 0.092(3) 0.008(2) 0.007(2) 0.028(2) C25 0.041(3) 0.066(4) 0.063(3) 0.002(3) -0.001(2) 0.022(3) C26 0.033(2) 0.061(4) 0.050(3) -0.004(2) -0.001(2) 0.005(2) C27 0.063(6) 0.047(6) 0.080(7) -0.007(6) 0.024(6) 0.018(6) C28 0.084(8) 0.093(8) 0.132(9) -0.020(8) 0.023(8) 0.061(7) C29 0.130(9) 0.076(7) 0.173(10) -0.016(7) 0.048(9) 0.048(7) C27' 0.172(13) 0.071(8) 0.105(9) 0.010(8) 0.042(10) 0.043(9) C28' 0.141(10) 0.086(9) 0.136(10) 0.025(8) 0.027(9) 0.060(8) C29' 0.130(9) 0.076(7) 0.173(10) -0.016(7) 0.048(9) 0.048(7) C2 0.031(2) 0.039(3) 0.035(2) -0.0003(19) -0.0101(18) 0.007(2) C30 0.031(2) 0.045(3) 0.0233(19) -0.0009(18) -0.0029(16) 0.006(2) O30 0.0297(14) 0.0339(17) 0.0264(13) -0.0027(11) -0.0028(11) 0.0051(13) C31 0.035(2) 0.047(3) 0.030(2) -0.0066(19) -0.0096(18) 0.004(2) C32 0.038(2) 0.041(3) 0.041(2) -0.010(2) -0.009(2) 0.010(2) C33 0.052(3) 0.048(3) 0.052(3) -0.017(2) -0.011(2) 0.003(3) C34 0.039(3) 0.059(4) 0.072(3) -0.023(3) -0.023(3) 0.006(3) O34 0.056(2) 0.078(3) 0.108(3) -0.044(3) -0.032(2) 0.000(2) C35 0.037(3) 0.076(4) 0.071(3) -0.021(3) -0.019(3) 0.012(3) C36 0.039(2) 0.054(3) 0.049(3) -0.019(2) -0.014(2) 0.012(3) C37 0.080(5) 0.088(6) 0.104(5) -0.024(4) -0.031(4) -0.003(4) C38 0.059(4) 0.098(6) 0.124(6) -0.043(5) 0.001(4) -0.010(4) C39 0.089(5) 0.123(7) 0.117(6) -0.044(5) 0.009(4) -0.025(5) C40 0.0233(19) 0.046(3) 0.026(2) -0.0004(18) 0.0021(16) 0.0084(19) O40 0.0248(13) 0.0298(16) 0.0219(12) 0.0006(11) -0.0012(11) 0.0040(12) C41 0.025(2) 0.038(3) 0.038(2) 0.003(2) -0.0020(17) 0.0067(19) C42 0.030(2) 0.034(3) 0.037(2) -0.0019(19) 0.0008(18) 0.004(2) C43 0.038(2) 0.040(3) 0.043(2) -0.007(2) -0.002(2) 0.005(2) C44 0.055(3) 0.029(3) 0.069(3) -0.012(2) 0.001(3) 0.008(2) O44 0.091(3) 0.042(2) 0.087(3) -0.023(2) -0.018(2) 0.014(2) C45 0.066(3) 0.043(3) 0.065(3) -0.002(3) -0.020(3) 0.020(3) C46 0.049(3) 0.040(3) 0.047(3) -0.007(2) -0.010(2) 0.013(2) C47 0.130(5) 0.057(4) 0.127(5) -0.011(4) -0.018(4) 0.014(4) C3 0.036(2) 0.049(3) 0.0214(19) 0.0043(18) 0.0073(17) -0.006(2) C50 0.0220(18) 0.043(3) 0.028(2) -0.0032(18) 0.0022(16) -0.0074(19) O50 0.0327(14) 0.0379(18) 0.0220(13) 0.0006(12) 0.0050(11) 0.0000(14) C51 0.027(2) 0.042(3) 0.029(2) -0.0083(18) 0.0058(17) -0.0057(19) C52 0.041(2) 0.057(3) 0.036(2) -0.004(2) 0.008(2) 0.010(2) C53 0.065(3) 0.071(4) 0.041(3) 0.004(3) 0.012(2) 0.031(3) C54 0.050(3) 0.074(4) 0.046(3) -0.011(3) 0.014(2) 0.013(3) O54 0.082(3) 0.111(4) 0.054(2) -0.020(2) 0.029(2) 0.027(3) C55 0.043(3) 0.063(4) 0.032(2) -0.010(2) 0.013(2) -0.002(2) C56 0.035(2) 0.052(3) 0.030(2) -0.005(2) 0.0053(18) -0.003(2) C57 0.071(4) 0.117(6) 0.074(4) -0.010(4) 0.009(3) 0.027(4) C58 0.115(5) 0.125(7) 0.110(5) 0.010(5) 0.046(4) 0.075(5) C59 0.120(9) 0.116(10) 0.063(7) -0.004(7) 0.021(6) 0.058(8) C59' 0.124(10) 0.131(11) 0.108(9) 0.008(9) 0.007(8) 0.030(10) C60 0.030(2) 0.040(3) 0.0243(19) 0.0035(18) -0.0049(16) -0.004(2) O60 0.0400(16) 0.0363(17) 0.0221(13) 0.0038(12) 0.0040(12) 0.0016(14) C61 0.053(3) 0.042(3) 0.030(2) 0.008(2) -0.004(2) -0.005(2) C62 0.056(3) 0.047(3) 0.041(2) 0.011(2) -0.008(2) 0.002(3) C63 0.079(4) 0.053(3) 0.056(3) 0.009(3) -0.006(3) 0.016(3) C64 0.131(5) 0.061(4) 0.061(3) 0.034(3) -0.017(4) 0.012(4) C65 0.162(6) 0.070(4) 0.044(3) 0.021(3) 0.003(4) 0.010(5) C66 0.111(4) 0.048(3) 0.034(2) 0.011(2) 0.002(3) -0.001(3) O64 0.192(5) 0.072(3) 0.099(3) 0.040(3) -0.027(4) 0.024(4) C67 0.127(6) 0.084(5) 0.125(6) 0.039(5) 0.004(5) 0.021(5) C68 0.140(7) 0.081(6) 0.194(8) 0.040(6) -0.022(6) 0.001(5) C69 0.120(7) 0.130(8) 0.208(9) 0.041(8) -0.009(7) 0.010(7) C4 0.049(5) 0.039(6) 0.038(5) -0.001(4) -0.006(4) -0.011(5) C70 0.062(6) 0.022(5) 0.045(5) 0.003(4) 0.014(5) 0.009(5) O70 0.0309(15) 0.021(3) 0.0289(15) -0.0013(17) 0.0042(12) -0.0012(19) C71 0.051(7) 0.029(6) 0.030(5) -0.008(4) -0.013(5) 0.001(6) C72 0.050(6) 0.066(8) 0.032(5) -0.010(5) -0.007(4) -0.005(6) C73 0.056(6) 0.061(8) 0.046(6) -0.006(5) 0.017(5) -0.012(6) C74 0.049(7) 0.071(9) 0.022(5) -0.007(5) -0.006(5) -0.006(7) O74 0.081(5) 0.106(7) 0.033(4) -0.003(4) -0.003(4) -0.020(5) C75 0.043(6) 0.065(9) 0.040(6) -0.004(6) -0.005(5) -0.027(6) C76 0.067(8) 0.059(9) 0.039(7) -0.001(6) 0.016(6) -0.018(7) C77 0.116(7) 0.141(9) 0.033(5) -0.020(6) -0.001(6) -0.058(7) C78 0.115(7) 0.148(8) 0.045(6) -0.014(6) 0.013(6) -0.062(7) C79 0.119(8) 0.158(10) 0.067(7) -0.009(8) 0.015(7) -0.064(8) C80 0.042(5) 0.040(6) 0.040(5) -0.012(4) -0.008(4) -0.023(4) O80 0.0276(18) 0.026(2) 0.0361(17) -0.009(3) 0.0045(14) -0.017(3) C81 0.043(5) 0.040(6) 0.039(5) 0.004(4) -0.001(4) -0.005(5) C82 0.060(8) 0.082(11) 0.059(8) -0.014(7) 0.032(7) -0.010(8) C83 0.056(7) 0.107(12) 0.057(7) -0.023(7) 0.025(6) -0.010(7) C84 0.055(9) 0.070(11) 0.092(12) 0.012(9) -0.024(8) 0.017(8) O84 0.036(4) 0.096(9) 0.076(6) 0.045(5) 0.015(4) -0.004(5) C85 0.049(6) 0.143(13) 0.059(7) 0.042(8) -0.012(6) -0.033(8) C86 0.059(7) 0.097(10) 0.053(6) 0.016(6) -0.002(5) -0.037(7) C87 0.063(7) 0.085(10) 0.062(7) 0.011(7) 0.026(6) 0.020(8) C88 0.071(9) 0.115(14) 0.085(10) 0.035(9) 0.030(8) -0.025(10) C89 0.108(11) 0.119(15) 0.142(13) -0.013(11) 0.071(10) -0.033(11) C5 0.0233(19) 0.037(2) 0.0249(18) -0.0084(17) 0.0044(15) 0.0045(18) C90 0.0249(18) 0.033(2) 0.0272(18) 0.0024(18) 0.0053(15) 0.0111(19) O90 0.0268(14) 0.0351(17) 0.0319(14) -0.0051(12) 0.0094(12) -0.0003(13) C91 0.0210(18) 0.037(2) 0.034(2) 0.0004(18) 0.0047(16) 0.0061(18) C92 0.033(2) 0.048(3) 0.033(2) 0.0035(19) 0.0056(18) 0.005(2) C93 0.042(3) 0.072(4) 0.033(2) 0.010(2) 0.010(2) 0.006(3) C94 0.044(3) 0.069(4) 0.053(3) 0.014(3) 0.020(2) -0.004(3) O94 0.075(2) 0.096(3) 0.061(2) 0.018(2) 0.034(2) -0.020(2) C95 0.044(3) 0.061(4) 0.058(3) -0.002(3) 0.021(2) -0.015(3) C96 0.038(2) 0.052(3) 0.040(2) -0.001(2) 0.014(2) -0.005(2) C97 0.073(4) 0.161(7) 0.052(3) 0.041(4) 0.023(3) -0.007(4) C98 0.183(8) 0.141(8) 0.079(4) 0.042(5) 0.076(5) -0.021(6) C99 0.136(7) 0.228(12) 0.067(5) 0.010(6) -0.003(5) -0.072(8) C100 0.027(2) 0.041(3) 0.0187(18) -0.0059(17) -0.0043(15) 0.0008(19) O100 0.0221(12) 0.0276(15) 0.0268(13) -0.0044(11) 0.0069(11) 0.0008(12) C101 0.032(2) 0.036(3) 0.0275(19) 0.0027(18) 0.0017(17) 0.002(2) C102 0.035(2) 0.037(3) 0.037(2) -0.0013(19) -0.0019(19) -0.002(2) C103 0.048(3) 0.042(3) 0.044(3) -0.003(2) -0.001(2) -0.014(2) C104 0.086(4) 0.033(3) 0.048(3) -0.011(2) 0.007(3) -0.010(3) O104 0.127(4) 0.034(2) 0.089(3) -0.022(2) 0.040(3) -0.024(2) C105 0.113(5) 0.039(3) 0.087(4) -0.025(3) 0.050(4) 0.003(3) C106 0.068(3) 0.037(3) 0.069(3) -0.017(2) 0.036(3) -0.003(3) C107 0.107(5) 0.038(4) 0.098(5) -0.009(3) -0.019(4) -0.023(4) C6 0.025(4) 0.022(4) 0.023(4) 0.003(3) 0.008(3) 0.004(3) C110 0.037(4) 0.020(4) 0.028(4) -0.010(3) 0.008(3) 0.001(3) O110 0.0309(15) 0.021(3) 0.0289(15) -0.0013(17) 0.0042(12) -0.0012(19) C111 0.024(4) 0.011(4) 0.029(4) -0.002(3) 0.004(3) 0.003(3) C112 0.020(4) 0.022(4) 0.031(4) 0.004(3) 0.003(3) -0.001(3) C113 0.015(4) 0.039(6) 0.025(4) 0.005(4) 0.003(3) 0.001(4) C114 0.019(4) 0.021(5) 0.033(5) -0.003(4) 0.008(4) -0.007(4) O114 0.024(3) 0.048(4) 0.022(3) -0.002(2) 0.000(2) 0.001(3) C115 0.030(5) 0.032(6) 0.022(5) -0.011(4) 0.003(4) -0.010(4) C116 0.021(5) 0.047(7) 0.029(5) -0.018(5) 0.005(4) -0.011(5) C117 0.039(5) 0.046(5) 0.027(4) 0.009(4) 0.000(4) -0.002(4) C118 0.051(5) 0.052(5) 0.030(4) 0.006(4) 0.001(4) -0.009(5) C119 0.063(6) 0.069(6) 0.034(5) -0.001(4) -0.003(4) -0.011(5) C120 0.018(3) 0.014(4) 0.027(4) 0.002(3) 0.004(3) 0.003(3) O120 0.0276(18) 0.026(2) 0.0361(17) -0.009(3) 0.0045(14) -0.017(3) C121 0.032(5) 0.031(6) 0.024(5) -0.003(4) 0.014(4) 0.004(4) C122 0.032(4) 0.024(5) 0.019(4) -0.005(3) 0.003(3) 0.005(4) C123 0.024(4) 0.049(6) 0.028(4) -0.012(4) -0.006(3) 0.008(4) C124 0.021(5) 0.060(9) 0.044(5) -0.012(5) 0.014(4) 0.011(6) O124 0.025(4) 0.064(6) 0.035(4) -0.010(4) 0.003(3) 0.006(4) C125 0.031(5) 0.056(7) 0.038(5) -0.008(4) 0.012(4) 0.014(5) C126 0.016(4) 0.046(6) 0.038(4) -0.005(4) -0.001(3) 0.007(4) C127 0.029(5) 0.072(9) 0.058(6) 0.021(6) 0.015(5) 0.010(6) C128 0.077(10) 0.082(11) 0.048(7) -0.018(7) 0.014(7) 0.031(8) C129 0.055(6) 0.064(8) 0.056(6) 0.011(6) 0.008(5) 0.011(6) C211 0.146(8) 0.175(11) 0.146(8) 0.073(8) 0.007(7) -0.014(8) C212 0.126(8) 0.163(10) 0.132(8) -0.015(7) -0.027(6) -0.037(7) C213 0.110(8) 0.128(10) 0.283(15) -0.015(10) -0.003(9) -0.003(7) C214 0.68(4) 0.31(2) 0.119(10) -0.012(12) -0.104(18) -0.15(2) C215 0.314(17) 0.112(9) 0.118(8) -0.020(7) -0.011(10) 0.031(10) C216 0.47(3) 0.212(15) 0.143(11) -0.004(10) 0.008(14) -0.193(16) C311 0.107(5) 0.230(6) 0.291(6) 0.069(6) 0.044(5) -0.024(5) C312 0.127(5) 0.267(7) 0.272(6) 0.087(6) 0.063(5) 0.004(5) C313 0.117(5) 0.264(7) 0.230(6) 0.093(6) 0.047(5) -0.017(5) C314 0.130(5) 0.241(7) 0.210(6) 0.054(6) -0.029(5) -0.035(5) C315 0.131(6) 0.239(7) 0.230(6) 0.012(6) -0.042(5) -0.033(6) C316 0.120(5) 0.228(7) 0.260(6) 0.030(6) -0.024(5) -0.062(5) C317 0.136(7) 0.229(9) 0.324(8) 0.061(8) 0.065(6) -0.011(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Tb1 O50 2.296(2) . ? Tb1 O60 2.308(3) . ? Tb1 O3 2.344(2) . ? Tb1 O40 2.346(2) . ? Tb1 O2 2.357(2) . ? Tb1 O30 2.378(3) . ? Tb1 O100 2.452(2) 2 ? Tb1 O1 2.6212(7) . ? Tb2 O10 2.287(3) . ? Tb2 O20 2.297(3) . ? Tb2 O2 2.324(2) . ? Tb2 O90 2.341(2) . ? Tb2 O3 2.370(3) 2 ? Tb2 O100 2.386(2) . ? Tb2 O40 2.475(2) . ? Tb2 O1 2.5048(7) . ? Tb3 O70 2.261(7) . ? Tb3 O70 2.261(7) 2 ? Tb3 O80 2.331(7) . ? Tb3 O80 2.331(7) 2 ? Tb3 O120 2.358(8) 2 ? Tb3 O120 2.358(8) . ? Tb3 O110 2.379(7) . ? Tb3 O110 2.379(7) 2 ? Tb3 O3 2.417(2) 2 ? Tb3 O3 2.417(2) . ? Tb3 O2 2.440(2) 2 ? Tb3 O2 2.440(2) . ? O1 Tb2 2.5048(7) 2 ? O1 Tb1 2.6212(7) 2 ? O1 H1O 0.810(19) . ? O2 H2O 1 . ? O3 Tb2 2.370(3) 2 ? O3 H3O 1 . ? C1 C10 1.394(6) . ? C1 C20 1.405(6) . ? C1 H1 0.95 . ? C10 O10 1.276(4) . ? C10 C11 1.493(5) . ? C11 C12 1.378(6) . ? C11 C16 1.385(5) . ? C12 C13 1.384(6) . ? C12 H12 0.95 . ? C13 C14 1.391(6) . ? C13 H13 0.95 . ? C14 C15 1.376(6) . ? C14 O14 1.386(5) . ? O14 C17 1.424(5) . ? C15 C16 1.381(6) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C17 C18 1.474(8) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.285(8) . ? C18 H18 0.95 . ? C19 H19A 0.95 . ? C19 H19B 0.95 . ? C20 O20 1.273(4) . ? C20 C21 1.499(6) . ? C21 C22 1.391(6) . ? C21 C26 1.391(6) . ? C22 C23 1.390(6) . ? C22 H22 0.95 . ? C23 C24 1.381(7) . ? C23 H23 0.95 . ? C24 C25 1.360(7) . ? C24 O24 1.368(6) . ? O24 C27 1.372(11) . ? O24 C27' 1.384(17) . ? C25 C26 1.384(7) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C27 C28 1.485(13) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.278(15) . ? C28 H28 0.95 . ? C29 H29A 0.95 . ? C29 H29B 0.95 . ? C27' C28' 1.526(14) . ? C27' H27C 0.99 . ? C27' H27D 0.99 . ? C28' C29' 1.279(16) . ? C28' H28' 0.95 . ? C29' H29C 0.95 . ? C29' H29D 0.95 . ? C2 C40 1.386(5) . ? C2 C30 1.424(6) . ? C2 H2 0.95 . ? C30 O30 1.262(5) . ? C30 C31 1.497(6) . ? C31 C32 1.392(6) . ? C31 C36 1.396(6) . ? C32 C33 1.373(6) . ? C32 H32 0.95 . ? C33 C34 1.386(7) . ? C33 H33 0.95 . ? C34 O34 1.372(6) . ? C34 C35 1.390(7) . ? O34 C37 1.437(7) . ? C35 C36 1.378(7) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.498(10) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.371(10) . ? C38 H38 0.95 . ? C39 H39A 0.95 . ? C39 H39B 0.95 . ? C40 O40 1.321(4) . ? C40 C41 1.476(6) . ? C41 C46 1.394(6) . ? C41 C42 1.406(5) . ? C42 C43 1.358(6) . ? C42 H42 0.95 . ? C43 C44 1.390(6) . ? C43 H43 0.95 . ? C44 O44 1.378(6) . ? C44 C45 1.395(7) . ? O44 C47 1.409(7) . ? C45 C46 1.365(7) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 C48 1.474(13) . ? C47 C48' 1.548(15) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C47 H47C 0.9916 . ? C47 H47D 0.9914 . ? C48 C49 1.090(15) . ? C48 H48 0.95 . ? C49 H49A 0.95 . ? C49 H49B 0.95 . ? C48' C49' 1.349(15) . ? C48' H48' 0.95 . ? C49' H49C 0.95 . ? C49' H49D 0.95 . ? C3 C60 1.399(6) . ? C3 C50 1.403(6) . ? C3 H3 0.95 . ? C50 O50 1.268(4) . ? C50 C51 1.505(6) . ? C51 C52 1.377(6) . ? C51 C56 1.403(5) . ? C52 C53 1.382(6) . ? C52 H52 0.95 . ? C53 C54 1.371(6) . ? C53 H53 0.95 . ? C54 C55 1.372(7) . ? C54 O54 1.401(6) . ? O54 C57 1.400(6) . ? C55 C56 1.393(6) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 C58 1.489(9) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 C59' 1.115(14) . ? C58 C59 1.266(11) . ? C58 H58 0.95 . ? C58 H58' 0.9518 . ? C59 H58' 1.1661 . ? C59 H59A 0.95 . ? C59 H59B 0.95 . ? C59' H59C 0.95 . ? C59' H59D 0.95 . ? C60 O60 1.275(4) . ? C60 C61 1.488(6) . ? C61 C62 1.370(7) . ? C61 C66 1.395(6) . ? C62 C63 1.383(7) . ? C62 H62 0.95 . ? C63 C64 1.376(7) . ? C63 H63 0.95 . ? C64 O64 1.355(7) . ? C64 C65 1.386(9) . ? C65 C66 1.372(8) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? O64 C67 1.342(9) . ? C67 C68 1.546(11) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? C68 C69 1.165(12) . ? C68 H68 0.95 . ? C69 H69A 0.95 . ? C69 H69B 0.95 . ? C4 C70 1.413(12) . ? C4 C80 1.418(11) . ? C4 H4 0.95 . ? C70 O70 1.279(10) . ? C70 C71 1.509(10) . ? C71 C76 1.378(11) . ? C71 C72 1.382(11) . ? C72 C73 1.391(10) . ? C72 H72 0.95 . ? C73 C74 1.374(11) . ? C73 H73 0.95 . ? C74 C75 1.366(11) . ? C74 O74 1.394(9) . ? O74 C77 1.403(12) . ? C75 C76 1.404(11) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? C77 C78 1.503(14) . ? C77 H77A 0.99 . ? C77 H77B 0.99 . ? C78 C79 1.254(12) . ? C78 H78 0.95 . ? C79 H79A 0.95 . ? C79 H79B 0.95 . ? C80 O80 1.294(9) . ? C80 C81 1.494(9) . ? C81 C86 1.367(10) . ? C81 C82 1.376(10) . ? C82 C83 1.402(11) . ? C82 H82 0.95 . ? C83 C84 1.368(11) . ? C83 H83 0.95 . ? C84 C85 1.370(12) . ? C84 O84 1.396(11) . ? O84 C87 1.406(12) . ? C85 C86 1.361(10) . ? C85 H85 0.95 . ? C86 H86 0.95 . ? C87 C88 1.445(13) . ? C87 H87A 0.99 . ? C87 H87B 0.99 . ? C88 C89 1.268(12) . ? C88 H88 0.95 . ? C89 H89A 0.95 . ? C89 H89B 0.95 . ? C5 C100 1.365(5) . ? C5 C90 1.439(6) . ? C5 H5 0.95 . ? C90 O90 1.260(4) . ? C90 C91 1.482(5) . ? C91 C96 1.380(6) . ? C91 C92 1.402(5) . ? C92 C93 1.393(6) . ? C92 H92 0.95 . ? C93 C94 1.359(7) . ? C93 H93 0.95 . ? C94 O94 1.384(6) . ? C94 C95 1.390(7) . ? O94 C97 1.423(6) . ? C95 C96 1.386(6) . ? C95 H95 0.95 . ? C96 H96 0.95 . ? C97 C98 1.560(10) . ? C97 H97A 0.99 . ? C97 H97B 0.99 . ? C98 C99 1.168(10) . ? C98 H98 0.95 . ? C99 H99A 0.95 . ? C99 H99B 0.95 . ? C100 O100 1.310(4) . ? C100 C101 1.474(6) . ? O100 Tb1 2.452(2) 2 ? C101 C106 1.395(6) . ? C101 C102 1.407(6) . ? C102 C103 1.373(6) . ? C102 H102 0.95 . ? C103 C104 1.357(7) . ? C103 H103 0.95 . ? C104 O104 1.379(6) . ? C104 C105 1.384(8) . ? O104 C107 1.393(7) . ? C105 C106 1.377(7) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C107 C108 1.485(14) . ? C107 C10A 1.510(14) . ? C107 H10A 0.99 . ? C107 H10B 0.99 . ? C107 H10F 0.9921 . ? C107 H10G 0.9942 . ? C108 C109 1.186(16) . ? C108 H108 0.95 . ? C109 H10C 0.95 . ? C109 H10D 0.95 . ? C10A C10B 1.253(16) . ? C10A H10E 0.95 . ? C10B H10H 0.95 . ? C10B H10I 0.95 . ? C6 C110 1.383(10) . ? C6 C120 1.412(9) . ? C6 H6 0.95 . ? C110 O110 1.288(9) . ? C110 C111 1.498(9) . ? C111 C112 1.388(9) . ? C111 C116 1.393(9) . ? C112 C113 1.386(9) . ? C112 H112 0.95 . ? C113 C114 1.370(9) . ? C113 H113 0.95 . ? C114 C115 1.389(10) . ? C114 O114 1.389(9) . ? O114 C117 1.393(9) . ? C115 C116 1.372(10) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C117 C118 1.488(11) . ? C117 H11A 0.99 . ? C117 H11B 0.99 . ? C118 C119 1.281(11) . ? C118 H118 0.95 . ? C119 H11C 0.95 . ? C119 H11D 0.95 . ? C120 O120 1.303(9) . ? C120 C121 1.495(9) . ? C121 C122 1.392(10) . ? C121 C126 1.406(10) . ? C122 C123 1.367(9) . ? C122 H122 0.95 . ? C123 C124 1.377(11) . ? C123 H123 0.95 . ? C124 C125 1.376(11) . ? C124 O124 1.424(9) . ? O124 C127 1.437(11) . ? C125 C126 1.412(9) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C127 C128 1.500(13) . ? C127 H12A 0.99 . ? C127 H12B 0.99 . ? C128 C129 1.267(11) . ? C128 H128 0.95 . ? C129 H12C 0.95 . ? C129 H12D 0.95 . ? C211 C216 1.394(7) . ? C211 C212 1.433(7) . ? C211 C217 1.464(8) . ? C211 H211 0.872(8) . ? C212 C213 1.394(7) . ? C212 C218 1.526(9) . ? C212 H212 0.877(8) . ? C213 C214 1.347(8) . ? C213 H213 0.95 . ? C214 C215 1.384(12) . ? C214 H214 0.95 . ? C215 C216 1.388(12) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C217 H21A 0.98 . ? C217 H21B 0.98 . ? C217 H21C 0.98 . ? C217 H211 0.70(3) . ? C218 H21D 0.98 . ? C218 H21E 0.98 . ? C218 H21F 0.98 . ? C218 H212 0.79(2) . ? C311 C316 1.379(8) . ? C311 C312 1.403(8) . ? C311 C317 1.515(8) . ? C312 C313 1.367(8) . ? C312 H312 0.95 . ? C313 C314 1.387(8) . ? C313 H313 0.95 . ? C314 C315 1.372(8) . ? C314 H314 0.95 . ? C315 C316 1.382(8) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C317 H31A 0.98 . ? C317 H31B 0.98 . ? C317 H31C 0.98 . ? 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 O50 Tb1 O60 73.64(9) . . ? O50 Tb1 O3 76.26(8) . . ? O60 Tb1 O3 140.33(9) . . ? O50 Tb1 O40 152.74(9) . . ? O60 Tb1 O40 81.25(9) . . ? O3 Tb1 O40 130.97(8) . . ? O50 Tb1 O2 115.85(9) . . ? O60 Tb1 O2 146.16(9) . . ? O3 Tb1 O2 71.40(8) . . ? O40 Tb1 O2 80.04(9) . . ? O50 Tb1 O30 90.45(9) . . ? O60 Tb1 O30 76.02(9) . . ? O3 Tb1 O30 129.60(9) . . ? O40 Tb1 O30 73.05(9) . . ? O2 Tb1 O30 71.66(8) . . ? O50 Tb1 O100 90.75(9) . 2 ? O60 Tb1 O100 77.97(9) . 2 ? O3 Tb1 O100 77.20(9) . 2 ? O40 Tb1 O100 94.31(9) . 2 ? O2 Tb1 O100 131.32(8) . 2 ? O30 Tb1 O100 152.48(9) . 2 ? O50 Tb1 O1 140.49(7) . . ? O60 Tb1 O1 127.55(10) . . ? O3 Tb1 O1 67.55(8) . . ? O40 Tb1 O1 64.87(8) . . ? O2 Tb1 O1 67.27(8) . . ? O30 Tb1 O1 124.71(6) . . ? O100 Tb1 O1 66.72(7) 2 . ? O10 Tb2 O20 74.06(10) . . ? O10 Tb2 O2 75.54(9) . . ? O20 Tb2 O2 137.76(8) . . ? O10 Tb2 O90 81.71(9) . . ? O20 Tb2 O90 78.25(9) . . ? O2 Tb2 O90 125.10(9) . . ? O10 Tb2 O3 114.48(10) . 2 ? O20 Tb2 O3 147.12(8) . 2 ? O2 Tb2 O3 73.25(8) . 2 ? O90 Tb2 O3 72.14(8) . 2 ? O10 Tb2 O100 147.51(9) . . ? O20 Tb2 O100 80.30(9) . . ? O2 Tb2 O100 136.35(8) . . ? O90 Tb2 O100 73.70(9) . . ? O3 Tb2 O100 77.99(9) 2 . ? O10 Tb2 O40 94.07(9) . . ? O20 Tb2 O40 75.61(9) . . ? O2 Tb2 O40 78.05(8) . . ? O90 Tb2 O40 153.66(9) . . ? O3 Tb2 O40 131.89(8) 2 . ? O100 Tb2 O40 98.60(8) . . ? O10 Tb2 O1 142.29(7) . . ? O20 Tb2 O1 124.70(11) . . ? O2 Tb2 O1 69.79(9) . . ? O90 Tb2 O1 130.85(7) . . ? O3 Tb2 O1 69.18(9) 2 . ? O100 Tb2 O1 69.60(7) . . ? O40 Tb2 O1 64.96(7) . . ? O70 Tb3 O70 126.1(3) . 2 ? O70 Tb3 O80 76.3(3) . . ? O70 Tb3 O80 78.9(3) 2 . ? O70 Tb3 O80 78.9(3) . 2 ? O70 Tb3 O80 76.3(3) 2 2 ? O80 Tb3 O80 123.5(4) . 2 ? O70 Tb3 O120 77.9(3) . 2 ? O70 Tb3 O120 72.8(3) 2 2 ? O80 Tb3 O120 7.1(3) . 2 ? O80 Tb3 O120 117.63(16) 2 2 ? O70 Tb3 O120 72.8(3) . . ? O70 Tb3 O120 77.9(3) 2 . ? O80 Tb3 O120 117.63(16) . . ? O80 Tb3 O120 7.1(3) 2 . ? O120 Tb3 O120 112.1(4) 2 . ? O70 Tb3 O110 8.3(3) . . ? O70 Tb3 O110 117.88(15) 2 . ? O80 Tb3 O110 71.9(3) . . ? O80 Tb3 O110 76.5(3) 2 . ? O120 Tb3 O110 72.6(3) 2 . ? O120 Tb3 O110 69.9(3) . . ? O70 Tb3 O110 117.88(15) . 2 ? O70 Tb3 O110 8.3(3) 2 2 ? O80 Tb3 O110 76.5(3) . 2 ? O80 Tb3 O110 71.9(3) 2 2 ? O120 Tb3 O110 69.9(3) 2 2 ? O120 Tb3 O110 72.6(3) . 2 ? O110 Tb3 O110 109.7(4) . 2 ? O70 Tb3 O3 131.1(2) . 2 ? O70 Tb3 O3 82.87(19) 2 2 ? O80 Tb3 O3 72.1(2) . 2 ? O80 Tb3 O3 149.96(18) 2 2 ? O120 Tb3 O3 75.3(2) 2 2 ? O120 Tb3 O3 155.80(19) . 2 ? O110 Tb3 O3 133.1(2) . 2 ? O110 Tb3 O3 89.72(19) 2 2 ? O70 Tb3 O3 82.87(19) . . ? O70 Tb3 O3 131.1(2) 2 . ? O80 Tb3 O3 149.96(18) . . ? O80 Tb3 O3 72.1(2) 2 . ? O120 Tb3 O3 155.80(19) 2 . ? O120 Tb3 O3 75.3(2) . . ? O110 Tb3 O3 89.7(2) . . ? O110 Tb3 O3 133.1(2) 2 . ? O3 Tb3 O3 107.81(12) 2 . ? O70 Tb3 O2 151.6(2) . 2 ? O70 Tb3 O2 69.91(19) 2 2 ? O80 Tb3 O2 132.1(2) . 2 ? O80 Tb3 O2 83.70(18) 2 2 ? O120 Tb3 O2 130.4(2) 2 2 ? O120 Tb3 O2 90.71(18) . 2 ? O110 Tb3 O2 155.6(2) . 2 ? O110 Tb3 O2 76.8(2) 2 2 ? O3 Tb3 O2 68.78(8) 2 2 ? O3 Tb3 O2 70.43(8) . 2 ? O70 Tb3 O2 69.91(19) . . ? O70 Tb3 O2 151.6(2) 2 . ? O80 Tb3 O2 83.70(18) . . ? O80 Tb3 O2 132.1(2) 2 . ? O120 Tb3 O2 90.71(18) 2 . ? O120 Tb3 O2 130.4(2) . . ? O110 Tb3 O2 76.8(2) . . ? O110 Tb3 O2 155.6(2) 2 . ? O3 Tb3 O2 70.43(8) 2 . ? O3 Tb3 O2 68.78(8) . . ? O2 Tb3 O2 107.47(12) 2 . ? Tb2 O1 Tb2 160.52(17) . 2 ? Tb2 O1 Tb1 88.53(3) . 2 ? Tb2 O1 Tb1 88.10(3) 2 2 ? Tb2 O1 Tb1 88.10(3) . . ? Tb2 O1 Tb1 88.53(3) 2 . ? Tb1 O1 Tb1 159.98(16) 2 . ? Tb2 O1 H1O 99.74(9) . . ? Tb2 O1 H1O 99.74(8) 2 . ? Tb1 O1 H1O 100.01(8) 2 . ? Tb1 O1 H1O 100.01(8) . . ? Tb2 O2 Tb1 99.23(10) . . ? Tb2 O2 Tb3 108.15(9) . . ? Tb1 O2 Tb3 109.07(9) . . ? Tb2 O2 H2O 113.1 . . ? Tb1 O2 H2O 113.1 . . ? Tb3 O2 H2O 113.1 . . ? Tb1 O3 Tb2 98.79(10) . 2 ? Tb1 O3 Tb3 110.29(9) . . ? Tb2 O3 Tb3 107.38(9) 2 . ? Tb1 O3 H3O 113.1 . . ? Tb2 O3 H3O 113.1 2 . ? Tb3 O3 H3O 113.1 . . ? C10 C1 C20 123.8(4) . . ? C10 C1 H1 118.1 . . ? C20 C1 H1 118.1 . . ? O10 C10 C1 124.6(4) . . ? O10 C10 C11 114.8(4) . . ? C1 C10 C11 120.6(4) . . ? C10 O10 Tb2 134.5(3) . . ? C12 C11 C16 117.5(4) . . ? C12 C11 C10 119.8(4) . . ? C16 C11 C10 122.7(4) . . ? C11 C12 C13 121.9(4) . . ? C11 C12 H12 119 . . ? C13 C12 H12 119 . . ? C12 C13 C14 118.8(5) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 O14 124.6(4) . . ? C15 C14 C13 120.6(4) . . ? O14 C14 C13 114.8(5) . . ? C14 O14 C17 116.7(4) . . ? C14 C15 C16 118.9(4) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C15 C16 C11 122.1(4) . . ? C15 C16 H16 118.9 . . ? C11 C16 H16 118.9 . . ? O14 C17 C18 108.0(5) . . ? O14 C17 H17A 110.1 . . ? C18 C17 H17A 110.1 . . ? O14 C17 H17B 110.1 . . ? C18 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? C19 C18 C17 126.6(6) . . ? C19 C18 H18 116.7 . . ? C17 C18 H18 116.7 . . ? C18 C19 H19A 120 . . ? C18 C19 H19B 120 . . ? H19A C19 H19B 120 . . ? O20 C20 C1 123.9(4) . . ? O20 C20 C21 115.3(4) . . ? C1 C20 C21 120.8(4) . . ? C20 O20 Tb2 136.0(3) . . ? C22 C21 C26 117.2(4) . . ? C22 C21 C20 118.9(4) . . ? C26 C21 C20 123.8(4) . . ? C23 C22 C21 121.7(4) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 119.2(5) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 O24 119.8(5) . . ? C25 C24 C23 120.2(5) . . ? O24 C24 C23 120.0(5) . . ? C24 O24 C27 125.9(6) . . ? C24 O24 C27' 118.1(7) . . ? C27 O24 C27' 115.5(8) . . ? C24 C25 C26 120.6(5) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 121.2(5) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? O24 C27 C28 124.7(9) . . ? O24 C27 H27A 106.2 . . ? C28 C27 H27A 106.2 . . ? O24 C27 H27B 106.2 . . ? C28 C27 H27B 106.2 . . ? H27A C27 H27B 106.4 . . ? C29 C28 C27 116.3(15) . . ? C29 C28 H28 121.8 . . ? C27 C28 H28 121.8 . . ? C28 C29 H29A 120 . . ? C28 C29 H29B 120 . . ? H29A C29 H29B 120 . . ? O24 C27' C28' 109.3(13) . . ? O24 C27' H27C 109.8 . . ? C28' C27' H27C 109.8 . . ? O24 C27' H27D 109.8 . . ? C28' C27' H27D 109.8 . . ? H27C C27' H27D 108.3 . . ? C29' C28' C27' 118.3(17) . . ? C29' C28' H28' 120.9 . . ? C27' C28' H28' 120.9 . . ? C28' C29' H29C 120 . . ? C28' C29' H29D 120 . . ? H29C C29' H29D 120 . . ? C40 C2 C30 124.8(4) . . ? C40 C2 H2 117.6 . . ? C30 C2 H2 117.6 . . ? O30 C30 C2 124.0(4) . . ? O30 C30 C31 116.3(4) . . ? C2 C30 C31 119.6(4) . . ? C30 O30 Tb1 132.1(3) . . ? C32 C31 C36 118.1(4) . . ? C32 C31 C30 120.4(4) . . ? C36 C31 C30 121.4(4) . . ? C33 C32 C31 122.1(4) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 119.3(5) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? O34 C34 C33 125.9(5) . . ? O34 C34 C35 114.4(5) . . ? C33 C34 C35 119.6(5) . . ? C34 O34 C37 119.6(5) . . ? C36 C35 C34 120.7(5) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C31 120.2(5) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? O34 C37 C38 109.8(6) . . ? O34 C37 H37A 109.7 . . ? C38 C37 H37A 109.7 . . ? O34 C37 H37B 109.7 . . ? C38 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? C39 C38 C37 123.1(7) . . ? C39 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? C38 C39 H39A 120 . . ? C38 C39 H39B 120 . . ? H39A C39 H39B 120 . . ? O40 C40 C2 121.6(4) . . ? O40 C40 C41 115.7(3) . . ? C2 C40 C41 122.7(4) . . ? C40 O40 Tb1 125.4(2) . . ? C40 O40 Tb2 123.5(2) . . ? Tb1 O40 Tb2 95.35(9) . . ? C46 C41 C42 116.6(4) . . ? C46 C41 C40 123.5(4) . . ? C42 C41 C40 119.8(4) . . ? C43 C42 C41 121.9(4) . . ? C43 C42 H42 119 . . ? C41 C42 H42 119 . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? O44 C44 C43 123.7(4) . . ? O44 C44 C45 116.8(5) . . ? C43 C44 C45 119.4(5) . . ? C44 O44 C47 117.5(4) . . ? C46 C45 C44 119.5(5) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C41 122.4(4) . . ? C45 C46 H46 118.8 . . ? C41 C46 H46 118.8 . . ? O44 C47 C48 106.2(8) . . ? O44 C47 C48' 106.7(8) . . ? O44 C47 H47A 110.5 . . ? C48 C47 H47A 110.5 . . ? O44 C47 H47B 110.5 . . ? C48 C47 H47B 110.5 . . ? H47A C47 H47B 108.7 . . ? O44 C47 H47C 110.3 . . ? C48' C47 H47C 115.9 . . ? O44 C47 H47D 110.2 . . ? C48' C47 H47D 105.3 . . ? H47C C47 H47D 108.2 . . ? C49 C48 C47 140(2) . . ? C49 C48 H48 110.2 . . ? C47 C48 H48 109.9 . . ? C48 C49 H49A 120.2 . . ? C48 C49 H49B 119.8 . . ? H49A C49 H49B 120 . . ? C49' C48' C47 120.9(14) . . ? C49' C48' H48' 119.5 . . ? C47 C48' H48' 119.6 . . ? C48' C49' H49C 119.9 . . ? C48' C49' H49D 120.1 . . ? H49C C49' H49D 120 . . ? C60 C3 C50 124.7(3) . . ? C60 C3 H3 117.7 . . ? C50 C3 H3 117.7 . . ? O50 C50 C3 123.9(4) . . ? O50 C50 C51 115.6(4) . . ? C3 C50 C51 120.5(3) . . ? C50 O50 Tb1 137.1(3) . . ? C52 C51 C56 117.6(4) . . ? C52 C51 C50 118.9(4) . . ? C56 C51 C50 123.4(4) . . ? C51 C52 C53 121.7(4) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C54 C53 C52 120.3(5) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 119.7(5) . . ? C55 C54 O54 124.3(4) . . ? C53 C54 O54 116.0(5) . . ? C54 O54 C57 119.1(5) . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C55 C56 C51 120.4(4) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? O54 C57 C58 107.3(6) . . ? O54 C57 H57A 110.3 . . ? C58 C57 H57A 110.2 . . ? O54 C57 H57B 110.2 . . ? C58 C57 H57B 110.3 . . ? H57A C57 H57B 108.5 . . ? C59 C58 C57 127.9(11) . . ? C59 C58 H58 116 . . ? C57 C58 H58 116 . . ? C59' C58 H58' 105.5 . . ? C57 C58 H58' 104.7 . . ? H58 C58 H58' 104.8 . . ? C58 C59 H59A 120 . . ? C58 C59 H59B 120 . . ? H59A C59 H59B 120 . . ? C58 C59' H59C 120 . . ? C58 C59' H59D 120 . . ? H59C C59' H59D 120 . . ? O60 C60 C3 123.7(4) . . ? O60 C60 C61 115.6(4) . . ? C3 C60 C61 120.7(4) . . ? C60 O60 Tb1 136.5(3) . . ? C62 C61 C66 117.0(5) . . ? C62 C61 C60 119.6(4) . . ? C66 C61 C60 123.3(5) . . ? C61 C62 C63 122.2(5) . . ? C61 C62 H62 118.9 . . ? C63 C62 H62 118.9 . . ? C64 C63 C62 119.8(6) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? O64 C64 C63 125.1(6) . . ? O64 C64 C65 115.9(6) . . ? C63 C64 C65 118.9(5) . . ? C66 C65 C64 120.2(5) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C65 C66 C61 121.5(5) . . ? C65 C66 H66 119.2 . . ? C61 C66 H66 119.2 . . ? C67 O64 C64 119.3(6) . . ? O64 C67 C68 104.1(7) . . ? O64 C67 H67A 110.9 . . ? C68 C67 H67A 110.9 . . ? O64 C67 H67B 110.9 . . ? C68 C67 H67B 110.9 . . ? H67A C67 H67B 108.9 . . ? C69 C68 C67 125.7(12) . . ? C69 C68 H68 117.1 . . ? C67 C68 H68 117.1 . . ? C68 C69 H69A 120 . . ? C68 C69 H69B 120 . . ? H69A C69 H69B 120 . . ? C70 C4 C80 123.0(8) . . ? C70 C4 H4 118.5 . . ? C80 C4 H4 118.5 . . ? O70 C70 C4 125.8(7) . . ? O70 C70 C71 115.2(8) . . ? C4 C70 C71 118.1(8) . . ? C70 O70 Tb3 132.9(6) . . ? C76 C71 C72 117.9(8) . . ? C76 C71 C70 126.3(9) . . ? C72 C71 C70 115.7(7) . . ? C71 C72 C73 120.9(8) . . ? C71 C72 H72 119.5 . . ? C73 C72 H72 119.5 . . ? C74 C73 C72 120.2(8) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C75 C74 C73 120.2(8) . . ? C75 C74 O74 124.9(8) . . ? C73 C74 O74 114.7(8) . . ? C74 O74 C77 117.7(9) . . ? C74 C75 C76 119.1(9) . . ? C74 C75 H75 120.5 . . ? C76 C75 H75 120.5 . . ? C71 C76 C75 121.6(10) . . ? C71 C76 H76 119.2 . . ? C75 C76 H76 119.2 . . ? O74 C77 C78 112.8(12) . . ? O74 C77 H77A 109 . . ? C78 C77 H77A 109 . . ? O74 C77 H77B 109 . . ? C78 C77 H77B 109 . . ? H77A C77 H77B 107.8 . . ? C79 C78 C77 121.3(16) . . ? C79 C78 H78 119.4 . . ? C77 C78 H78 119.4 . . ? C78 C79 H79A 120 . . ? C78 C79 H79B 120 . . ? H79A C79 H79B 120 . . ? O80 C80 C4 126.5(8) . . ? O80 C80 C81 112.3(7) . . ? C4 C80 C81 121.0(7) . . ? C80 O80 Tb3 129.6(6) . . ? C86 C81 C82 118.7(8) . . ? C86 C81 C80 123.1(7) . . ? C82 C81 C80 118.3(7) . . ? C81 C82 C83 120.6(9) . . ? C81 C82 H82 119.7 . . ? C83 C82 H82 119.7 . . ? C84 C83 C82 118.1(10) . . ? C84 C83 H83 121 . . ? C82 C83 H83 121 . . ? C83 C84 C85 121.2(9) . . ? C83 C84 O84 123.6(10) . . ? C85 C84 O84 114.5(9) . . ? C84 O84 C87 119.3(9) . . ? C86 C85 C84 119.4(9) . . ? C86 C85 H85 120.3 . . ? C84 C85 H85 120.3 . . ? C85 C86 C81 121.5(9) . . ? C85 C86 H86 119.3 . . ? C81 C86 H86 119.3 . . ? O84 C87 C88 107.0(10) . . ? O84 C87 H87A 110.3 . . ? C88 C87 H87A 110.3 . . ? O84 C87 H87B 110.3 . . ? C88 C87 H87B 110.3 . . ? H87A C87 H87B 108.6 . . ? C89 C88 C87 123.4(15) . . ? C89 C88 H88 118.3 . . ? C87 C88 H88 118.3 . . ? C88 C89 H89A 120 . . ? C88 C89 H89B 120 . . ? H89A C89 H89B 120 . . ? C100 C5 C90 125.5(3) . . ? C100 C5 H5 117.3 . . ? C90 C5 H5 117.3 . . ? O90 C90 C5 123.9(3) . . ? O90 C90 C91 115.6(4) . . ? C5 C90 C91 120.5(3) . . ? C90 O90 Tb2 132.2(3) . . ? C96 C91 C92 118.8(4) . . ? C96 C91 C90 118.7(4) . . ? C92 C91 C90 122.5(4) . . ? C93 C92 C91 120.1(4) . . ? C93 C92 H92 119.9 . . ? C91 C92 H92 119.9 . . ? C94 C93 C92 120.1(4) . . ? C94 C93 H93 120 . . ? C92 C93 H93 120 . . ? C93 C94 O94 125.2(4) . . ? C93 C94 C95 120.6(4) . . ? O94 C94 C95 114.2(5) . . ? C94 O94 C97 117.6(5) . . ? C96 C95 C94 119.6(5) . . ? C96 C95 H95 120.2 . . ? C94 C95 H95 120.2 . . ? C91 C96 C95 120.8(4) . . ? C91 C96 H96 119.6 . . ? C95 C96 H96 119.6 . . ? O94 C97 C98 102.8(5) . . ? O94 C97 H97A 111.2 . . ? C98 C97 H97A 111.2 . . ? O94 C97 H97B 111.2 . . ? C98 C97 H97B 111.2 . . ? H97A C97 H97B 109.1 . . ? C99 C98 C97 125.8(10) . . ? C99 C98 H98 117.1 . . ? C97 C98 H98 117.1 . . ? C98 C99 H99A 120 . . ? C98 C99 H99B 120 . . ? H99A C99 H99B 120 . . ? O100 C100 C5 123.9(4) . . ? O100 C100 C101 115.2(3) . . ? C5 C100 C101 120.9(4) . . ? C100 O100 Tb2 123.2(2) . . ? C100 O100 Tb1 127.1(2) . 2 ? Tb2 O100 Tb1 95.40(9) . 2 ? C106 C101 C102 115.9(4) . . ? C106 C101 C100 123.1(4) . . ? C102 C101 C100 121.0(4) . . ? C103 C102 C101 122.6(4) . . ? C103 C102 H102 118.7 . . ? C101 C102 H102 118.7 . . ? C104 C103 C102 120.3(5) . . ? C104 C103 H103 119.9 . . ? C102 C103 H103 119.9 . . ? C103 C104 O104 125.2(5) . . ? C103 C104 C105 118.9(5) . . ? O104 C104 C105 115.9(5) . . ? C104 O104 C107 118.0(5) . . ? C106 C105 C104 121.3(5) . . ? C106 C105 H105 119.3 . . ? C104 C105 H105 119.3 . . ? C105 C106 C101 121.0(5) . . ? C105 C106 H106 119.5 . . ? C101 C106 H106 119.5 . . ? O104 C107 C108 117.9(9) . . ? O104 C107 C10A 109.9(8) . . ? O104 C107 H10A 107.8 . . ? C108 C107 H10A 107.8 . . ? O104 C107 H10B 107.8 . . ? C108 C107 H10B 107.8 . . ? C10A C107 H10B 101.7 . . ? H10A C107 H10B 107.2 . . ? O104 C107 H10F 110.6 . . ? O104 C107 H10G 111.6 . . ? C108 C107 H10G 114.7 . . ? C10A C107 H10G 111.1 . . ? H10F C107 H10G 109 . . ? C109 C108 C107 122.3(17) . . ? C109 C108 H108 118.9 . . ? C107 C108 H108 118.9 . . ? C108 C109 H10C 120 . . ? C108 C109 H10D 120 . . ? H10C C109 H10D 120 . . ? C10B C10A C107 112.1(17) . . ? C10B C10A H10E 124 . . ? C107 C10A H10E 124 . . ? C10A C10B H10H 120 . . ? C10A C10B H10I 120 . . ? H10H C10B H10I 120 . . ? C110 C6 C120 123.6(6) . . ? C110 C6 H6 118.2 . . ? C120 C6 H6 118.2 . . ? O110 C110 C6 122.7(7) . . ? O110 C110 C111 114.8(7) . . ? C6 C110 C111 122.3(6) . . ? C110 O110 Tb3 127.8(6) . . ? C112 C111 C116 118.1(7) . . ? C112 C111 C110 122.4(6) . . ? C116 C111 C110 119.4(7) . . ? C113 C112 C111 120.6(6) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C114 C113 C112 120.3(7) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C113 C114 C115 120.0(8) . . ? C113 C114 O114 125.0(7) . . ? C115 C114 O114 114.9(7) . . ? C114 O114 C117 118.1(6) . . ? C116 C115 C114 119.6(8) . . ? C116 C115 H115 120.2 . . ? C114 C115 H115 120.2 . . ? C115 C116 C111 121.4(8) . . ? C115 C116 H116 119.3 . . ? C111 C116 H116 119.3 . . ? O114 C117 C118 109.0(7) . . ? O114 C117 H11A 109.9 . . ? C118 C117 H11A 109.9 . . ? O114 C117 H11B 109.9 . . ? C118 C117 H11B 109.9 . . ? H11A C117 H11B 108.3 . . ? C119 C118 C117 124.2(10) . . ? C119 C118 H118 117.9 . . ? C117 C118 H118 117.9 . . ? C118 C119 H11C 120 . . ? C118 C119 H11D 120 . . ? H11C C119 H11D 120 . . ? O120 C120 C6 124.4(6) . . ? O120 C120 C121 116.1(7) . . ? C6 C120 C121 119.5(6) . . ? C120 O120 Tb3 130.2(6) . . ? C122 C121 C126 117.8(7) . . ? C122 C121 C120 120.2(7) . . ? C126 C121 C120 121.9(7) . . ? C123 C122 C121 122.1(7) . . ? C123 C122 H122 118.9 . . ? C121 C122 H122 118.9 . . ? C122 C123 C124 119.5(7) . . ? C122 C123 H123 120.3 . . ? C124 C123 H123 120.3 . . ? C125 C124 C123 121.4(7) . . ? C125 C124 O124 122.4(8) . . ? C123 C124 O124 115.1(9) . . ? C124 O124 C127 118.2(8) . . ? C124 C125 C126 118.9(7) . . ? C124 C125 H125 120.6 . . ? C126 C125 H125 120.6 . . ? C121 C126 C125 120.2(7) . . ? C121 C126 H126 119.9 . . ? C125 C126 H126 119.9 . . ? O124 C127 C128 110.5(9) . . ? O124 C127 H12A 109.6 . . ? C128 C127 H12A 109.6 . . ? O124 C127 H12B 109.6 . . ? C128 C127 H12B 109.6 . . ? H12A C127 H12B 108.1 . . ? C129 C128 C127 129.8(11) . . ? C129 C128 H128 115.1 . . ? C127 C128 H128 115.1 . . ? C128 C129 H12C 120 . . ? C128 C129 H12D 120 . . ? H12C C129 H12D 120 . . ? C216 C211 C212 115.7(6) . . ? C216 C211 C217 118.3(8) . . ? C212 C211 C217 123.9(7) . . ? C216 C211 H211 124.0(10) . . ? C212 C211 H211 120.2(10) . . ? C213 C212 C211 117.4(6) . . ? C213 C212 C218 101.4(8) . . ? C211 C212 C218 140.6(9) . . ? C213 C212 H212 123.2(10) . . ? C211 C212 H212 119.4(10) . . ? C214 C213 C212 127.2(8) . . ? C214 C213 H213 116.4 . . ? C212 C213 H213 116.4 . . ? C213 C214 C215 112.9(9) . . ? C213 C214 H214 123.6 . . ? C215 C214 H214 123.6 . . ? C214 C215 C216 123.0(9) . . ? C214 C215 H215 118.5 . . ? C216 C215 H215 118.5 . . ? C215 C216 C211 121.0(8) . . ? C215 C216 H216 119.5 . . ? C211 C216 H216 119.5 . . ? C211 C217 H21A 109.5 . . ? C211 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? C211 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C212 C218 H21D 109.5 . . ? C212 C218 H21E 109.4 . . ? C212 C218 H21F 109.5 . . ? C316 C311 C312 119.3(8) . . ? C316 C311 C317 118.5(8) . . ? C312 C311 C317 122.2(8) . . ? C313 C312 C311 124.0(8) . . ? C313 C312 H312 118 . . ? C311 C312 H312 118 . . ? C312 C313 C314 115.9(8) . . ? C312 C313 H313 122.1 . . ? C314 C313 H313 122.1 . . ? C315 C314 C313 120.7(9) . . ? C315 C314 H314 119.7 . . ? C313 C314 H314 119.7 . . ? C314 C315 C316 123.5(9) . . ? C314 C315 H315 118.2 . . ? C316 C315 H315 118.2 . . ? C311 C316 C315 116.6(8) . . ? C311 C316 H316 121.7 . . ? C315 C316 H316 121.7 . . ? C311 C317 H31A 109.5 . . ? C311 C317 H31B 109.5 . . ? H31A C317 H31B 109.5 . . ? C311 C317 H31C 109.5 . . ? H31A C317 H31C 109.5 . . ? H31B C317 H31C 109.5 . . ? #===END # Attachment '- mxm13.cif' data_mxm13 _database_code_depnum_ccdc_archive 'CCDC 779683' #TrackingRef '- mxm13.cif' _audit_creation_date 2010-03-09T20:29:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C238 H227 Ho5 O45' _chemical_formula_moiety 'C210 H195 Ho5 O45, 4(C7 H8)' _chemical_formula_weight 4631.85 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall -C_2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.6653(3) _cell_length_b 17.7996(2) _cell_length_c 32.4926(3) _cell_angle_alpha 90 _cell_angle_beta 95.5600(10) _cell_angle_gamma 90 _cell_volume 20530.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 49684 _cell_measurement_theta_min 3.5071 _cell_measurement_theta_max 34.5018 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic_rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9400 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -1 0 0.1174 1 1 0 0.0623 0 0 1 0.1552 0 0 -1 0.3629 1 0 0 0.0557 -16 -4 44 0.1938 -50 0 10 0.1334 -48 -6 -3 0.1179 -49 -1 -3 0.1042 14 24 2 0.0847 50 0 -4 0.0521 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.984 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.792 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0083790719 _diffrn_orient_matrix_ub_12 -0.0361860237 _diffrn_orient_matrix_ub_13 0.0007617908 _diffrn_orient_matrix_ub_21 0.0162274631 _diffrn_orient_matrix_ub_22 0.0150752143 _diffrn_orient_matrix_ub_23 -0.0079595611 _diffrn_orient_matrix_ub_31 0.0081000049 _diffrn_orient_matrix_ub_32 0.0072325442 _diffrn_orient_matrix_ub_33 0.0204320715 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_number 133526 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 34.57 _diffrn_reflns_theta_full 33.75 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.949 _reflns_number_total 41528 _reflns_number_gt 27184 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+31.7716P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 41528 _refine_ls_number_parameters 1549 _refine_ls_number_restraints 469 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.121 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 4.397 _refine_diff_density_min -2.63 _refine_diff_density_rms 0.142 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ho1 Ho 0.011179(4) 0.939613(8) 0.328381(4) 0.02164(3) Uani 1 1 d . . . Ho2 Ho 0.068017(4) 0.937702(8) 0.246005(4) 0.02163(3) Uani 1 1 d . . . Ho3 Ho 0 1.102724(11) 0.25 0.02111(4) Uani 1 2 d S . . O1 O 0 0.91466(16) 0.25 0.0217(6) Uani 1 2 d SD . . H1O H 0 0.8677(10) 0.25 0.026 Uiso 1 2 d SD . . O2 O 0.04430(6) 1.02244(12) 0.29009(6) 0.0230(4) Uani 1 1 d . . . H2O H 0.0643 1.0509 0.3073 0.028 Uiso 1 1 calc R . . O3 O -0.03100(6) 1.02291(12) 0.29490(6) 0.0229(4) Uani 1 1 d . . . H3O H -0.0457 1.0515 0.3144 0.027 Uiso 1 1 calc R . . C1 C 0.16963(9) 0.9044(2) 0.27569(12) 0.0374(8) Uani 1 1 d . . . H1 H 0.1962 0.8983 0.2795 0.045 Uiso 1 1 calc R . . C10 C 0.15462(9) 0.9751(2) 0.28458(11) 0.0361(8) Uani 1 1 d D . . O10 O 0.11925(6) 0.98985(14) 0.28149(8) 0.0348(5) Uani 1 1 d D . . C11 C 0.18010(10) 1.0368(2) 0.30030(12) 0.0415(9) Uani 1 1 d D . . C12 C 0.16634(12) 1.0911(3) 0.32546(18) 0.0742(16) Uani 1 1 d D . . H12 H 0.1411 1.0881 0.3322 0.089 Uiso 1 1 calc R . . C13 C 0.18934(13) 1.1502(3) 0.3409(2) 0.0862(19) Uani 1 1 d D . . H13 H 0.18 1.1865 0.3588 0.103 Uiso 1 1 calc R . . C14 C 0.22583(11) 1.1556(3) 0.33009(14) 0.0551(12) Uani 1 1 d D . . O14 O 0.24595(9) 1.2168(2) 0.34593(11) 0.0688(10) Uani 1 1 d D . . C15 C 0.23985(11) 1.1025(3) 0.30510(14) 0.0495(10) Uani 1 1 d D . . H15 H 0.2649 1.1066 0.2976 0.059 Uiso 1 1 calc R . . C16 C 0.21702(10) 1.0426(2) 0.29088(14) 0.0450(9) Uani 1 1 d D . . H16 H 0.227 1.0049 0.2744 0.054 Uiso 1 1 calc RD . . C17 C 0.28219(12) 1.2295(3) 0.33193(17) 0.0578(12) Uani 1 1 d . . . H17A H 0.2799 1.2332 0.3014 0.069 Uiso 1 1 calc R . . H17B H 0.2992 1.1871 0.3403 0.069 Uiso 1 1 calc R . . C18 C 0.29768(13) 1.3003(3) 0.35043(19) 0.0695(15) Uani 1 1 d . . . H18 H 0.3216 1.316 0.3431 0.083 Uiso 1 1 calc R . . C19 C 0.28148(17) 1.3429(4) 0.3758(2) 0.096(2) Uani 1 1 d . . . H19A H 0.2575 1.3295 0.384 0.116 Uiso 1 1 calc R . . H19B H 0.2936 1.3876 0.3862 0.116 Uiso 1 1 calc R . . C20 C 0.14781(9) 0.8426(2) 0.26167(10) 0.0317(7) Uani 1 1 d . . . O20 O 0.11292(6) 0.84629(13) 0.24879(7) 0.0298(5) Uani 1 1 d . . . C21 C 0.16459(9) 0.7657(2) 0.26156(11) 0.0362(8) Uani 1 1 d . . . C22 C 0.14547(11) 0.7091(2) 0.23899(12) 0.0399(8) Uani 1 1 d . . . H22 H 0.1231 0.7213 0.222 0.048 Uiso 1 1 calc R . . C23 C 0.15787(12) 0.6356(2) 0.24043(13) 0.0456(9) Uani 1 1 d . . . H23 H 0.1443 0.598 0.2245 0.055 Uiso 1 1 calc R . . C24 C 0.19041(13) 0.6174(3) 0.26552(13) 0.0498(10) Uani 1 1 d . A . O24 O 0.20315(10) 0.54515(19) 0.26837(12) 0.0652(10) Uani 1 1 d . . . C25 C 0.21046(12) 0.6724(3) 0.28744(14) 0.0545(12) Uani 1 1 d . . . H25 H 0.233 0.66 0.304 0.065 Uiso 1 1 calc R A . C26 C 0.19799(11) 0.7462(2) 0.28551(12) 0.0440(9) Uani 1 1 d . A . H26 H 0.2122 0.784 0.3006 0.053 Uiso 1 1 calc R . . C27 C 0.1823(3) 0.4845(5) 0.2524(3) 0.058(2) Uani 0.5 1 d PDU A 1 H27A H 0.1792 0.4899 0.2219 0.07 Uiso 0.5 1 calc PRD A 1 H27B H 0.1569 0.4882 0.2621 0.07 Uiso 0.5 1 calc PR A 1 C28 C 0.1965(4) 0.4087(7) 0.2618(5) 0.104(4) Uani 0.5 1 d PDU A 1 H28 H 0.1787 0.369 0.2603 0.125 Uiso 0.5 1 calc PR A 1 C29 C 0.2308(5) 0.3916(9) 0.2719(6) 0.139(4) Uani 0.5 1 d PDU A 1 H29A H 0.2496 0.4296 0.2739 0.167 Uiso 0.5 1 calc PR A 1 H29B H 0.2376 0.3408 0.2776 0.167 Uiso 0.5 1 calc PR A 1 C27' C 0.2377(5) 0.5289(7) 0.2924(4) 0.101(4) Uani 0.5 1 d PDU A 2 H27C H 0.2358 0.5423 0.3217 0.121 Uiso 0.5 1 calc PRD A 2 H27D H 0.2584 0.5585 0.2822 0.121 Uiso 0.5 1 calc PR A 2 C28' C 0.2456(5) 0.4466(7) 0.2888(5) 0.118(5) Uani 0.5 1 d PDU A 2 H28' H 0.2693 0.426 0.2991 0.141 Uiso 0.5 1 calc PR A 2 C29' C 0.2194(6) 0.4050(11) 0.2714(8) 0.139(4) Uani 0.5 1 d PDU A 2 H29C H 0.1959 0.4266 0.2613 0.167 Uiso 0.5 1 calc PR A 2 H29D H 0.2234 0.3525 0.2686 0.167 Uiso 0.5 1 calc PR A 2 C2 C 0.10262(10) 0.8494(2) 0.35679(11) 0.0356(8) Uani 1 1 d . . . H2 H 0.1223 0.8191 0.3697 0.043 Uiso 1 1 calc R . . C30 C 0.09955(10) 0.9253(2) 0.37118(10) 0.0329(7) Uani 1 1 d . . . O30 O 0.07019(6) 0.96369(14) 0.36558(7) 0.0299(5) Uani 1 1 d . . . C31 C 0.13304(11) 0.9611(2) 0.39450(11) 0.0381(8) Uani 1 1 d . . . C32 C 0.12833(11) 1.0243(2) 0.41857(11) 0.0416(9) Uani 1 1 d . . . H32 H 0.1036 1.043 0.4206 0.05 Uiso 1 1 calc R . . C33 C 0.15873(13) 1.0608(2) 0.43969(13) 0.0495(11) Uani 1 1 d . . . H33 H 0.1549 1.1036 0.4563 0.059 Uiso 1 1 calc R . . C34 C 0.19452(13) 1.0340(3) 0.43626(15) 0.0582(13) Uani 1 1 d . . . O34 O 0.22731(10) 1.0637(2) 0.45621(13) 0.0767(12) Uani 1 1 d . . . C35 C 0.20019(12) 0.9718(3) 0.41185(16) 0.0591(13) Uani 1 1 d . . . H35 H 0.225 0.954 0.4093 0.071 Uiso 1 1 calc R . . C36 C 0.16968(11) 0.9360(2) 0.39136(13) 0.0480(10) Uani 1 1 d . . . H36 H 0.1737 0.8933 0.3748 0.058 Uiso 1 1 calc R . . C37 C 0.22634(17) 1.1350(3) 0.47666(19) 0.0797(18) Uani 1 1 d . . . H37A H 0.2491 1.1404 0.4964 0.096 Uiso 1 1 calc R . . H37B H 0.2041 1.137 0.4926 0.096 Uiso 1 1 calc R . . C38 C 0.22463(16) 1.1978(4) 0.4471(2) 0.0823(19) Uani 1 1 d . . . H38 H 0.2403 1.1956 0.4251 0.099 Uiso 1 1 calc R . . C39 C 0.20198(18) 1.2585(4) 0.4493(2) 0.0823(18) Uani 1 1 d . . . H39A H 0.186 1.2623 0.4709 0.099 Uiso 1 1 calc R . . H39B H 0.2021 1.2973 0.4292 0.099 Uiso 1 1 calc R . . C40 C 0.07906(9) 0.8179(2) 0.32574(10) 0.0317(7) Uani 1 1 d . . . O40 O 0.05355(6) 0.85699(12) 0.30290(6) 0.0259(4) Uani 1 1 d . . . C41 C 0.08046(10) 0.7370(2) 0.31549(11) 0.0343(7) Uani 1 1 d . . . C42 C 0.06142(10) 0.7105(2) 0.27838(11) 0.0340(7) Uani 1 1 d . . . H42 H 0.0486 0.7454 0.2599 0.041 Uiso 1 1 calc R . . C43 C 0.06089(12) 0.6346(2) 0.26803(13) 0.0434(9) Uani 1 1 d . . . H43 H 0.0475 0.6179 0.243 0.052 Uiso 1 1 calc R . . C44 C 0.08002(14) 0.5839(2) 0.29440(15) 0.0533(11) Uani 1 1 d . . . O44 O 0.08070(12) 0.50804(18) 0.28661(13) 0.0805(12) Uani 1 1 d . C . C45 C 0.09876(15) 0.6080(2) 0.33120(15) 0.0594(13) Uani 1 1 d . . . H45 H 0.1115 0.5726 0.3494 0.071 Uiso 1 1 calc R . . C46 C 0.09916(12) 0.6832(2) 0.34169(13) 0.0488(10) Uani 1 1 d . . . H46 H 0.1123 0.6989 0.3671 0.059 Uiso 1 1 calc R . . C47 C 0.0609(2) 0.4816(3) 0.2503(2) 0.102(2) Uani 1 1 d DU . . H47A H 0.0747 0.4951 0.2263 0.122 Uiso 0.5 1 calc PR B 1 H47B H 0.0358 0.5058 0.2466 0.122 Uiso 0.5 1 calc PR B 1 H47C H 0.0653 0.5151 0.2269 0.122 Uiso 0.5 1 d PR B 2 H47D H 0.0336 0.4815 0.2536 0.122 Uiso 0.5 1 d PR B 2 C48 C 0.0561(3) 0.3966(6) 0.2520(4) 0.100(3) Uiso 0.5 1 d PDU C 1 H48 H 0.0791 0.3695 0.2564 0.12 Uiso 0.5 1 calc PR C 1 C49 C 0.0277(5) 0.3567(13) 0.2486(7) 0.105(8) Uiso 0.5 1 d PDU C 1 H49A H 0.0035 0.3791 0.2442 0.126 Uiso 0.5 1 calc PR C 1 H49B H 0.0301 0.3036 0.2505 0.126 Uiso 0.5 1 calc PR C 1 C48' C 0.0717(5) 0.4021(8) 0.2436(5) 0.115(5) Uiso 0.5 1 d PDU C 2 H48' H 0.0756 0.3841 0.2168 0.138 Uiso 0.5 1 calc PR C 2 C49' C 0.0757(5) 0.3576(10) 0.2762(5) 0.116(5) Uiso 0.5 1 d PDU C 2 H49C H 0.0718 0.3767 0.3027 0.14 Uiso 0.5 1 calc PR C 2 H49D H 0.0826 0.3065 0.2731 0.14 Uiso 0.5 1 calc PR C 2 C3 C -0.01247(10) 0.9093(2) 0.43650(10) 0.0316(7) Uani 1 1 d . . . H3 H -0.0178 0.9021 0.4643 0.038 Uiso 1 1 calc R . . C50 C -0.02479(9) 0.97603(19) 0.41669(9) 0.0269(6) Uani 1 1 d . . . O50 O -0.01727(7) 0.99392(13) 0.38019(6) 0.0302(5) Uani 1 1 d . . . C51 C -0.04829(9) 1.0304(2) 0.43767(10) 0.0308(7) Uani 1 1 d . . . C52 C -0.06571(12) 1.0888(2) 0.41463(11) 0.0423(9) Uani 1 1 d . . . H52 H -0.0614 1.094 0.3864 0.051 Uiso 1 1 calc R . . C53 C -0.08908(14) 1.1395(3) 0.43186(13) 0.0589(13) Uani 1 1 d . . . H53 H -0.1006 1.1788 0.4155 0.071 Uiso 1 1 calc R . . C54 C -0.09564(12) 1.1328(3) 0.47295(12) 0.0494(10) Uani 1 1 d . . . O54 O -0.11957(11) 1.1871(2) 0.48732(11) 0.0754(11) Uani 1 1 d . . . C55 C -0.07892(11) 1.0760(2) 0.49652(11) 0.0430(9) Uani 1 1 d . . . H55 H -0.0833 1.0714 0.5248 0.052 Uiso 1 1 calc R . . C56 C -0.05555(10) 1.0249(2) 0.47893(10) 0.0352(8) Uani 1 1 d . . . H56 H -0.0443 0.9854 0.4955 0.042 Uiso 1 1 calc R . . C57 C -0.12341(16) 1.1905(4) 0.53037(16) 0.0758(17) Uani 1 1 d . E . H57A H -0.0983 1.1941 0.5462 0.091 Uiso 1 1 calc R . . H57B H -0.1361 1.1447 0.5393 0.091 Uiso 1 1 calc R . . C58 C -0.1466(2) 1.2591(5) 0.5380(2) 0.109(2) Uani 1 1 d DU . . H58 H -0.1421 1.3016 0.5214 0.13 Uiso 0.5 1 calc PR D 1 H58' H -0.1718 1.2448 0.5294 0.13 Uiso 0.5 1 d PR D 2 C59 C -0.1701(4) 1.2680(9) 0.5621(3) 0.093(4) Uani 0.5 1 d PDU E 1 H59A H -0.1742 1.3165 0.573 0.111 Uiso 0.5 1 calc PR E 1 H59B H -0.1845 1.2265 0.5701 0.111 Uiso 0.5 1 calc PR E 1 C59' C -0.1486(5) 1.3162(8) 0.5481(5) 0.107(4) Uani 0.5 1 d PDU E 2 H59C H -0.1662 1.3292 0.5671 0.128 Uiso 0.5 1 calc PR E 2 H59D H -0.1329 1.3537 0.5382 0.128 Uiso 0.5 1 calc PR E 2 C60 C 0.00727(10) 0.85224(19) 0.41781(9) 0.0299(7) Uani 1 1 d . . . O60 O 0.01470(7) 0.85347(13) 0.38049(7) 0.0320(5) Uani 1 1 d . . . C61 C 0.01985(11) 0.7842(2) 0.44205(10) 0.0368(8) Uani 1 1 d U . . C62 C 0.03358(12) 0.7240(2) 0.42176(12) 0.0448(9) Uani 1 1 d U . . H62 H 0.0357 0.7279 0.3929 0.054 Uiso 1 1 calc R . . C63 C 0.04450(14) 0.6577(3) 0.44205(15) 0.0581(12) Uani 1 1 d U . . H63 H 0.0535 0.6165 0.4272 0.07 Uiso 1 1 calc R . . C64 C 0.04208(18) 0.6525(3) 0.48420(17) 0.0773(16) Uani 1 1 d U . . C65 C 0.0304(2) 0.7139(3) 0.50568(15) 0.0807(18) Uani 1 1 d U . . H65 H 0.0301 0.7112 0.5348 0.097 Uiso 1 1 calc R . . C66 C 0.01938(16) 0.7787(3) 0.48498(12) 0.0598(13) Uani 1 1 d U . . H66 H 0.0113 0.8205 0.5 0.072 Uiso 1 1 calc R . . O64 O 0.05068(16) 0.5895(2) 0.50698(15) 0.1080(17) Uani 1 1 d U . . C67 C 0.0582(2) 0.5236(4) 0.4875(3) 0.103(2) Uani 1 1 d U . . H67A H 0.0827 0.5259 0.4757 0.124 Uiso 1 1 calc R . . H67B H 0.0382 0.5116 0.4652 0.124 Uiso 1 1 calc R . . C68 C 0.0590(2) 0.4644(4) 0.5239(3) 0.103(2) Uani 1 1 d U . . H68 H 0.0722 0.4759 0.55 0.124 Uiso 1 1 calc R . . C69 C 0.0438(2) 0.4074(5) 0.5193(3) 0.109(3) Uani 1 1 d U . . H69A H 0.0305 0.3954 0.4933 0.131 Uiso 1 1 calc R . . H69B H 0.0445 0.3724 0.5414 0.131 Uiso 1 1 calc R . . C4 C 0.08399(18) 1.1966(3) 0.30032(18) 0.0269(13) Uani 0.5 1 d P F 1 H4 H 0.1075 1.2103 0.3145 0.032 Uiso 0.5 1 calc PR F 1 C70 C 0.05355(18) 1.1855(3) 0.32359(16) 0.0263(12) Uani 0.5 1 d PD F 1 O70 O 0.0202(2) 1.1673(5) 0.3084(2) 0.0275(6) Uani 0.5 1 d PD F 1 C71 C 0.05915(19) 1.1884(4) 0.36996(18) 0.0255(13) Uani 0.5 1 d PD F 1 C72 C 0.03581(19) 1.1437(3) 0.39182(16) 0.0282(13) Uani 0.5 1 d PD F 1 H72 H 0.0162 1.1154 0.3772 0.034 Uiso 0.5 1 calc PR F 1 C73 C 0.04076(19) 1.1401(4) 0.43441(18) 0.0337(15) Uani 0.5 1 d PD F 1 H73 H 0.0242 1.1106 0.4489 0.04 Uiso 0.5 1 calc PR F 1 C74 C 0.0701(2) 1.1797(4) 0.45618(18) 0.0330(15) Uani 0.5 1 d PD F 1 O74 O 0.07273(16) 1.1687(3) 0.49851(13) 0.0468(14) Uani 0.5 1 d PD F 1 C75 C 0.0921(3) 1.2260(5) 0.4350(2) 0.040(2) Uani 0.5 1 d PD F 1 H75 H 0.1107 1.2567 0.4497 0.048 Uiso 0.5 1 calc PR F 1 C76 C 0.0875(2) 1.2281(5) 0.3920(2) 0.0354(17) Uani 0.5 1 d PD F 1 H76 H 0.1041 1.2576 0.3776 0.043 Uiso 0.5 1 calc PR F 1 C77 C 0.0842(2) 1.2280(5) 0.5254(2) 0.048(2) Uani 0.5 1 d PD F 1 H77A H 0.071 1.2237 0.5508 0.057 Uiso 0.5 1 calc PR F 1 H77B H 0.0767 1.2763 0.5119 0.057 Uiso 0.5 1 calc PR F 1 C78 C 0.1270(3) 1.2284(6) 0.5375(3) 0.056(3) Uani 0.5 1 d PD F 1 H78 H 0.1398 1.1817 0.5408 0.067 Uiso 0.5 1 calc PR F 1 C79 C 0.1457(4) 1.2880(8) 0.5433(4) 0.079(4) Uani 0.5 1 d PD F 1 H79A H 0.1334 1.3353 0.5402 0.094 Uiso 0.5 1 calc PR F 1 H79B H 0.1721 1.2858 0.5508 0.094 Uiso 0.5 1 calc PR F 1 C80 C 0.08193(15) 1.1889(3) 0.25775(15) 0.0234(12) Uani 0.5 1 d PD F 1 O80 O 0.05398(16) 1.1631(3) 0.23463(18) 0.0248(6) Uani 0.5 1 d PD F 1 C81 C 0.11484(17) 1.2072(4) 0.23465(18) 0.0290(13) Uani 0.5 1 d PD F 1 C82 C 0.1107(2) 1.2130(7) 0.1922(2) 0.051(3) Uani 0.5 1 d PD F 1 H82 H 0.0867 1.2031 0.1779 0.061 Uiso 0.5 1 calc PR F 1 C83 C 0.1400(2) 1.2327(6) 0.1694(2) 0.050(2) Uani 0.5 1 d PD F 1 H83 H 0.1355 1.2416 0.1405 0.06 Uiso 0.5 1 calc PR F 1 C84 C 0.1757(2) 1.2391(7) 0.1893(2) 0.042(3) Uani 0.5 1 d PD F 1 O84 O 0.2062(2) 1.2601(5) 0.1698(2) 0.059(2) Uani 0.5 1 d PD F 1 C85 C 0.1812(2) 1.2289(6) 0.2313(2) 0.056(2) Uani 0.5 1 d PD F 1 H85 H 0.2058 1.2321 0.2452 0.067 Uiso 0.5 1 calc PR F 1 C86 C 0.15122(19) 1.2142(6) 0.2530(2) 0.054(2) Uani 0.5 1 d PD F 1 H86 H 0.1556 1.2086 0.2821 0.064 Uiso 0.5 1 calc PR F 1 C87 C 0.2027(2) 1.2760(6) 0.1271(3) 0.051(2) Uani 0.5 1 d PD F 1 H87A H 0.1836 1.3156 0.1205 0.061 Uiso 0.5 1 calc PR F 1 H87B H 0.1951 1.2304 0.1109 0.061 Uiso 0.5 1 calc PR F 1 C88 C 0.2403(3) 1.3020(7) 0.1174(3) 0.058(3) Uani 0.5 1 d PD F 1 H88 H 0.2476 1.3511 0.1264 0.07 Uiso 0.5 1 calc PR F 1 C89 C 0.2631(3) 1.2665(8) 0.0987(3) 0.079(4) Uani 0.5 1 d PD F 1 H89A H 0.2572 1.2171 0.089 0.095 Uiso 0.5 1 calc PR F 1 H89B H 0.2866 1.2885 0.0941 0.095 Uiso 0.5 1 calc PR F 1 C5 C 0.09341(9) 0.86184(18) 0.14785(9) 0.0275(6) Uani 1 1 d . . . H5 H 0.1042 0.8354 0.1265 0.033 Uiso 1 1 calc R . . C90 C 0.10853(9) 0.93431(18) 0.15894(10) 0.0278(6) Uani 1 1 d . . . O90 O 0.10107(6) 0.96956(13) 0.19072(7) 0.0294(5) Uani 1 1 d . . . C91 C 0.13533(9) 0.97066(19) 0.13328(10) 0.0289(6) Uani 1 1 d . . . C92 C 0.13494(10) 0.9583(2) 0.09115(10) 0.0356(8) Uani 1 1 d . . . H92 H 0.118 0.9223 0.0782 0.043 Uiso 1 1 calc R . . C93 C 0.15888(11) 0.9976(2) 0.06737(12) 0.0432(9) Uani 1 1 d . . . H93 H 0.158 0.9894 0.0384 0.052 Uiso 1 1 calc R . . C94 C 0.18370(12) 1.0484(3) 0.08647(13) 0.0493(10) Uani 1 1 d . . . O94 O 0.20808(11) 1.0923(2) 0.06630(10) 0.0728(11) Uani 1 1 d . . . C95 C 0.18497(13) 1.0608(3) 0.12864(14) 0.0524(11) Uani 1 1 d . . . H95 H 0.2027 1.0953 0.1416 0.063 Uiso 1 1 calc R . . C96 C 0.16067(10) 1.0232(2) 0.15181(12) 0.0394(8) Uani 1 1 d . . . H96 H 0.1611 1.0331 0.1806 0.047 Uiso 1 1 calc R . . C97 C 0.20760(17) 1.0833(4) 0.02268(15) 0.0796(18) Uani 1 1 d . . . H97A H 0.1824 1.0948 0.0086 0.095 Uiso 1 1 calc R . . H97B H 0.2147 1.0316 0.0155 0.095 Uiso 1 1 calc R . . C98 C 0.2375(3) 1.1415(5) 0.0106(2) 0.128(3) Uani 1 1 d . . . H98 H 0.2363 1.1907 0.0217 0.154 Uiso 1 1 calc R . . C99 C 0.2617(2) 1.1297(5) -0.0112(2) 0.110(3) Uani 1 1 d . . . H99A H 0.264 1.0813 -0.0231 0.132 Uiso 1 1 calc R . . H99B H 0.2787 1.1686 -0.0169 0.132 Uiso 1 1 calc R . . C100 C 0.06449(9) 0.82756(18) 0.16561(9) 0.0270(6) Uani 1 1 d . . . O100 O 0.04347(6) 0.86125(12) 0.19100(6) 0.0252(4) Uani 1 1 d . . . C101 C 0.05551(10) 0.74687(19) 0.15707(10) 0.0325(7) Uani 1 1 d . . . C102 C 0.02286(11) 0.7155(2) 0.17031(11) 0.0372(8) Uani 1 1 d . . . H102 H 0.0067 0.7462 0.1846 0.045 Uiso 1 1 calc R . . C103 C 0.01347(13) 0.6409(2) 0.16315(13) 0.0465(10) Uani 1 1 d . . . H103 H -0.0089 0.6208 0.1725 0.056 Uiso 1 1 calc R . . C104 C 0.03685(18) 0.5964(2) 0.14231(14) 0.0622(14) Uani 1 1 d . . . O104 O 0.02912(15) 0.52259(19) 0.13226(12) 0.0922(15) Uani 1 1 d . H . C105 C 0.06963(18) 0.6256(3) 0.13005(16) 0.0722(16) Uani 1 1 d . . . H105 H 0.086 0.594 0.1165 0.087 Uiso 1 1 calc R . . C106 C 0.07916(15) 0.6998(2) 0.13712(14) 0.0550(12) Uani 1 1 d . . . H106 H 0.102 0.7189 0.1284 0.066 Uiso 1 1 calc R . . C107 C -0.0045(2) 0.4902(3) 0.1441(2) 0.095(2) Uani 1 1 d D . . H10A H -0.026 0.5229 0.1343 0.113 Uiso 0.5 1 calc PR G 1 H10B H -0.003 0.4886 0.1747 0.113 Uiso 0.5 1 calc PR G 1 H10F H -0.0269 0.5141 0.1292 0.113 Uiso 0.5 1 d PR G 2 H10G H -0.006 0.4955 0.1742 0.113 Uiso 0.5 1 d PR G 2 C108 C -0.0120(3) 0.4132(5) 0.1279(3) 0.105(2) Uiso 0.5 1 d PD H 1 H108 H -0.0376 0.4067 0.1175 0.126 Uiso 0.5 1 calc PR H 1 C109 C 0.0062(8) 0.3568(13) 0.1245(10) 0.127(14) Uiso 0.5 1 d PD H 1 H10C H 0.0323 0.3561 0.1337 0.152 Uiso 0.5 1 calc PR H 1 H10D H -0.0056 0.313 0.1125 0.152 Uiso 0.5 1 calc PR H 1 C10A C -0.0080(11) 0.4066(11) 0.1333(9) 0.18(2) Uiso 0.5 1 d PD H 2 H10E H -0.0196 0.3705 0.1495 0.216 Uiso 0.5 1 calc PR H 2 C10B C 0.0056(3) 0.3921(7) 0.1016(3) 0.104(3) Uiso 0.5 1 d PD H 2 H10H H 0.0168 0.4309 0.0868 0.125 Uiso 0.5 1 calc PR H 2 H10I H 0.0052 0.342 0.0915 0.125 Uiso 0.5 1 calc PR H 2 C6 C -0.03063(19) 1.2037(4) 0.3415(2) 0.0338(15) Uani 0.5 1 d P F 2 H6 H -0.0394 1.2189 0.3669 0.041 Uiso 0.5 1 calc PR F 2 C110 C 0.0083(2) 1.1892(5) 0.34104(17) 0.0396(17) Uani 0.5 1 d PD F 2 O110 O 0.0229(3) 1.1731(5) 0.3072(2) 0.0275(6) Uani 0.5 1 d PD F 2 C111 C 0.03573(18) 1.1964(4) 0.37782(18) 0.0305(14) Uani 0.5 1 d PD F 2 C112 C 0.02503(19) 1.1908(5) 0.41760(19) 0.0376(16) Uani 0.5 1 d PD F 2 H112 H -0.0007 1.183 0.4216 0.045 Uiso 0.5 1 calc PR F 2 C113 C 0.05158(19) 1.1964(5) 0.4519(2) 0.0359(16) Uani 0.5 1 d PD F 2 H113 H 0.0441 1.1919 0.4791 0.043 Uiso 0.5 1 calc PR F 2 C114 C 0.0887(2) 1.2084(6) 0.4460(2) 0.033(2) Uani 0.5 1 d PD F 2 O114 O 0.11670(15) 1.2147(4) 0.47800(15) 0.0455(14) Uani 0.5 1 d PD F 2 C115 C 0.0994(2) 1.2159(5) 0.4061(2) 0.0379(19) Uani 0.5 1 d PD F 2 H115 H 0.1248 1.2271 0.402 0.045 Uiso 0.5 1 calc PR F 2 C116 C 0.07322(19) 1.2071(5) 0.3727(2) 0.0317(16) Uani 0.5 1 d PD F 2 H116 H 0.0811 1.2085 0.3456 0.038 Uiso 0.5 1 calc PR F 2 C117 C 0.1060(3) 1.2257(5) 0.5193(2) 0.0433(19) Uani 0.5 1 d PD F 2 H11A H 0.0926 1.181 0.5286 0.052 Uiso 0.5 1 calc PR F 2 H11B H 0.0894 1.2701 0.5203 0.052 Uiso 0.5 1 calc PR F 2 C118 C 0.1425(3) 1.2378(6) 0.5463(3) 0.047(2) Uani 0.5 1 d PD F 2 H118 H 0.1599 1.1973 0.5505 0.057 Uiso 0.5 1 calc PR F 2 C119 C 0.1506(4) 1.3009(6) 0.5635(3) 0.066(3) Uani 0.5 1 d PD F 2 H11C H 0.1335 1.3417 0.5596 0.079 Uiso 0.5 1 calc PR F 2 H11D H 0.1737 1.307 0.5803 0.079 Uiso 0.5 1 calc PR F 2 C120 C -0.05749(17) 1.1969(3) 0.30633(19) 0.0290(13) Uani 0.5 1 d PD F 2 O120 O -0.04949(17) 1.1762(4) 0.26959(19) 0.0248(6) Uani 0.5 1 d PD F 2 C121 C -0.0981(2) 1.2153(5) 0.3115(2) 0.0303(17) Uani 0.5 1 d PD F 2 C122 C -0.12561(17) 1.1818(4) 0.2847(2) 0.0366(16) Uani 0.5 1 d PD F 2 H122 H -0.1184 1.1532 0.262 0.044 Uiso 0.5 1 calc PR F 2 C123 C -0.16340(19) 1.1892(5) 0.2901(2) 0.0456(19) Uani 0.5 1 d PD F 2 H123 H -0.182 1.1671 0.271 0.055 Uiso 0.5 1 calc PR F 2 C124 C -0.1739(2) 1.2293(6) 0.3237(3) 0.040(2) Uani 0.5 1 d PD F 2 O124 O -0.21183(17) 1.2309(4) 0.3293(2) 0.0417(17) Uani 0.5 1 d PD F 2 C125 C -0.1467(2) 1.2665(5) 0.3497(3) 0.050(2) Uani 0.5 1 d PD F 2 H125 H -0.154 1.2973 0.3714 0.06 Uiso 0.5 1 calc PR F 2 C126 C -0.10892(18) 1.2584(4) 0.3436(2) 0.0400(17) Uani 0.5 1 d PD F 2 H126 H -0.0903 1.2829 0.3618 0.048 Uiso 0.5 1 calc PR F 2 C127 C -0.2222(3) 1.2513(5) 0.3691(3) 0.055(2) Uani 0.5 1 d PD F 2 H12A H -0.2015 1.2381 0.3905 0.066 Uiso 0.5 1 calc PR F 2 H12B H -0.2449 1.2229 0.375 0.066 Uiso 0.5 1 calc PR F 2 C128 C -0.2299(3) 1.3326(6) 0.3711(3) 0.061(3) Uani 0.5 1 d PD F 2 H128 H -0.2361 1.3514 0.3969 0.073 Uiso 0.5 1 calc PR F 2 C129 C -0.2291(3) 1.3804(6) 0.3421(3) 0.059(3) Uani 0.5 1 d PD F 2 H12C H -0.2231 1.3649 0.3155 0.071 Uiso 0.5 1 calc PR F 2 H12D H -0.2347 1.4317 0.3469 0.071 Uiso 0.5 1 calc PR F 2 C211 C 0.1841(2) 0.4760(6) 0.4000(2) 0.156(4) Uani 1 1 d D K . H211 H 0.2032(5) 0.4974(18) 0.3897(4) 0.187 Uiso 0.5 1 d PD I 1 C212 C 0.1567(2) 0.4353(5) 0.37457(19) 0.115(3) Uani 1 1 d D . . H212 H 0.1590(6) 0.430(2) 0.3480(4) 0.137 Uiso 0.5 1 d PD J 2 C213 C 0.1251(2) 0.4113(5) 0.3931(3) 0.150(4) Uani 1 1 d D K . H213 H 0.1045 0.3945 0.3748 0.179 Uiso 1 1 calc RD . . C214 C 0.1202(3) 0.4089(8) 0.4338(3) 0.218(7) Uani 1 1 d D . . H214 H 0.0992 0.3863 0.4447 0.262 Uiso 1 1 calc R K . C215 C 0.1493(2) 0.4432(5) 0.4574(3) 0.132(4) Uani 1 1 d D K . H215 H 0.1479 0.444 0.4865 0.159 Uiso 1 1 calc R . . C216 C 0.1805(3) 0.4769(7) 0.4429(2) 0.171(5) Uani 1 1 d D . . H216 H 0.1991 0.5002 0.4615 0.206 Uiso 1 1 calc R K . C217 C 0.2110(4) 0.5280(8) 0.3835(4) 0.108(5) Uiso 0.5 1 d PD . . H21A H 0.2045 0.5343 0.3537 0.162 Uiso 0.5 1 calc PR K . H21B H 0.2365 0.5075 0.3885 0.162 Uiso 0.5 1 calc PRD . . H21C H 0.2098 0.5768 0.3972 0.162 Uiso 0.5 1 calc PR . . C218 C 0.1523(6) 0.3926(14) 0.3339(5) 0.265(17) Uiso 0.5 1 d PD K 1 H21D H 0.1751 0.3991 0.3196 0.397 Uiso 0.5 1 calc PR K 1 H21E H 0.1305 0.4119 0.3166 0.397 Uiso 0.5 1 calc PRD K 1 H21F H 0.1487 0.339 0.3394 0.397 Uiso 0.5 1 calc PRD K 1 C311 C 0.1389(2) 0.5341(6) 0.6290(3) 0.188(3) Uani 1 1 d DU . . C312 C 0.1692(3) 0.4835(7) 0.6351(3) 0.206(3) Uani 1 1 d DU . . H312 H 0.1729 0.4579 0.6608 0.247 Uiso 1 1 calc R . . C313 C 0.1938(3) 0.4690(7) 0.6060(3) 0.190(3) Uani 1 1 d DU . . H313 H 0.2162 0.4405 0.6121 0.228 Uiso 1 1 calc R . . C314 C 0.1836(3) 0.4990(6) 0.5669(3) 0.181(3) Uani 1 1 d DU . . H314 H 0.1969 0.4849 0.5441 0.217 Uiso 1 1 calc R . . C315 C 0.1544(3) 0.5489(6) 0.5615(3) 0.182(3) Uani 1 1 d DU . . H315 H 0.1501 0.5727 0.5353 0.218 Uiso 1 1 calc R . . C316 C 0.1309(3) 0.5673(6) 0.5911(3) 0.181(3) Uani 1 1 d DU . . H316 H 0.1103 0.601 0.5856 0.218 Uiso 1 1 calc R . . C317 C 0.1131(3) 0.5508(7) 0.6620(3) 0.205(4) Uani 1 1 d DU . . H31A H 0.1273 0.5465 0.6893 0.307 Uiso 1 1 calc R . . H31B H 0.0922 0.5148 0.66 0.307 Uiso 1 1 calc RD . . H31C H 0.1032 0.6019 0.6583 0.307 Uiso 1 1 calc RD . . 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 Ho1 0.02327(6) 0.02301(6) 0.01846(5) 0.00210(4) 0.00110(4) 0.00244(5) Ho2 0.01853(6) 0.02321(6) 0.02306(6) -0.00497(5) 0.00159(4) -0.00107(5) Ho3 0.02334(8) 0.02068(8) 0.01931(7) 0 0.00203(6) 0 O1 0.0222(13) 0.0179(12) 0.0248(13) 0 0.0008(11) 0 O2 0.0231(10) 0.0234(10) 0.0226(9) -0.0033(7) 0.0027(8) 0.0003(8) O3 0.0235(10) 0.0246(10) 0.0208(9) 0.0018(7) 0.0035(8) 0.0044(8) C1 0.0197(14) 0.046(2) 0.0465(19) -0.0067(16) 0.0026(13) -0.0018(14) C10 0.0244(15) 0.045(2) 0.0387(17) -0.0114(15) -0.0008(13) -0.0076(14) O10 0.0208(10) 0.0394(13) 0.0436(13) -0.0161(10) 0.0002(9) -0.0020(10) C11 0.0243(15) 0.049(2) 0.050(2) -0.0140(17) 0.0017(15) -0.0095(15) C12 0.032(2) 0.083(3) 0.110(4) -0.062(3) 0.020(2) -0.027(2) C13 0.041(2) 0.095(4) 0.127(5) -0.074(3) 0.027(3) -0.033(3) C14 0.035(2) 0.066(3) 0.064(3) -0.021(2) 0.0045(19) -0.024(2) O14 0.0438(16) 0.082(2) 0.082(2) -0.0361(19) 0.0137(16) -0.0371(16) C15 0.0299(18) 0.057(3) 0.061(2) -0.006(2) 0.0040(17) -0.0151(18) C16 0.0277(17) 0.048(2) 0.059(2) -0.0072(18) 0.0042(17) -0.0074(16) C17 0.032(2) 0.061(3) 0.079(3) -0.009(2) 0.001(2) -0.019(2) C18 0.036(2) 0.067(3) 0.105(4) -0.014(3) 0.000(3) -0.022(2) C19 0.063(3) 0.095(4) 0.132(6) -0.043(4) 0.016(4) -0.050(3) C20 0.0243(14) 0.0400(18) 0.0310(15) -0.0070(13) 0.0046(12) 0.0049(13) O20 0.0239(10) 0.0340(12) 0.0310(11) -0.0074(9) -0.0006(9) 0.0019(9) C21 0.0248(15) 0.049(2) 0.0352(16) -0.0048(15) 0.0033(13) 0.0068(15) C22 0.0315(17) 0.046(2) 0.0426(19) -0.0077(16) 0.0037(15) 0.0103(16) C23 0.046(2) 0.045(2) 0.047(2) -0.0083(17) 0.0073(17) 0.0135(18) C24 0.054(2) 0.047(2) 0.048(2) 0.0007(18) 0.0085(19) 0.021(2) O24 0.059(2) 0.0497(19) 0.087(2) 0.0055(17) 0.0061(19) 0.0249(16) C25 0.041(2) 0.067(3) 0.053(2) 0.002(2) -0.0033(19) 0.022(2) C26 0.0314(18) 0.051(2) 0.048(2) -0.0035(17) -0.0038(16) 0.0105(17) C27 0.073(6) 0.034(4) 0.069(5) -0.005(4) 0.016(5) 0.020(4) C28 0.102(8) 0.069(7) 0.138(9) -0.006(7) 0.002(8) 0.050(6) C29 0.157(10) 0.070(6) 0.184(9) -0.004(6) -0.014(9) 0.057(7) C27' 0.146(11) 0.075(7) 0.086(8) 0.021(6) 0.033(8) 0.028(8) C28' 0.145(10) 0.079(7) 0.128(10) 0.036(7) 0.011(9) 0.050(7) C29' 0.157(10) 0.070(6) 0.184(9) -0.004(6) -0.014(9) 0.057(7) C2 0.0328(17) 0.0337(17) 0.0380(17) -0.0007(14) -0.0078(14) 0.0084(14) C30 0.0318(16) 0.0350(17) 0.0296(15) -0.0009(12) -0.0080(13) 0.0050(13) O30 0.0282(11) 0.0344(12) 0.0262(10) -0.0018(9) -0.0030(9) 0.0027(9) C31 0.0359(18) 0.0396(19) 0.0361(17) -0.0051(14) -0.0099(15) 0.0075(15) C32 0.0402(19) 0.046(2) 0.0360(18) -0.0067(15) -0.0101(15) 0.0078(17) C33 0.050(2) 0.047(2) 0.048(2) -0.0179(18) -0.0121(19) 0.0035(19) C34 0.042(2) 0.059(3) 0.068(3) -0.022(2) -0.021(2) 0.003(2) O34 0.0512(19) 0.068(2) 0.103(3) -0.038(2) -0.0331(19) -0.0010(16) C35 0.037(2) 0.061(3) 0.075(3) -0.025(2) -0.019(2) 0.008(2) C36 0.0356(19) 0.048(2) 0.056(2) -0.0191(18) -0.0170(17) 0.0093(17) C37 0.067(3) 0.076(4) 0.090(4) -0.033(3) -0.026(3) -0.008(3) C38 0.058(3) 0.082(4) 0.104(5) -0.038(4) -0.003(3) -0.013(3) C39 0.072(4) 0.077(4) 0.097(4) -0.026(3) 0.008(3) -0.022(3) C40 0.0251(15) 0.0395(18) 0.0298(15) 0.0022(13) -0.0012(12) 0.0082(13) O40 0.0250(10) 0.0265(10) 0.0256(10) -0.0020(8) -0.0008(8) 0.0052(8) C41 0.0328(16) 0.0305(17) 0.0383(17) -0.0010(13) -0.0024(14) 0.0067(14) C42 0.0298(16) 0.0304(16) 0.0414(18) -0.0009(13) 0.0015(14) 0.0074(13) C43 0.044(2) 0.0344(19) 0.050(2) -0.0091(16) -0.0038(17) 0.0068(16) C44 0.064(3) 0.0278(18) 0.067(3) -0.0064(18) -0.002(2) 0.0148(19) O44 0.109(3) 0.0344(17) 0.093(3) -0.0168(17) -0.017(2) 0.0266(18) C45 0.076(3) 0.036(2) 0.062(3) -0.0001(19) -0.016(2) 0.025(2) C46 0.053(2) 0.037(2) 0.052(2) -0.0047(17) -0.0142(19) 0.0192(18) C47 0.133(5) 0.056(3) 0.108(5) -0.032(3) -0.031(4) 0.029(4) C3 0.0346(17) 0.0372(17) 0.0229(13) 0.0038(12) 0.0030(12) -0.0056(14) C50 0.0255(14) 0.0340(16) 0.0210(12) -0.0016(11) 0.0014(11) -0.0087(12) O50 0.0364(12) 0.0334(12) 0.0212(9) 0.0000(8) 0.0050(9) 0.0029(10) C51 0.0275(15) 0.0383(18) 0.0267(14) -0.0070(12) 0.0033(12) -0.0052(13) C52 0.047(2) 0.050(2) 0.0299(16) -0.0030(15) 0.0059(15) 0.0063(18) C53 0.067(3) 0.069(3) 0.041(2) 0.004(2) 0.009(2) 0.029(3) C54 0.045(2) 0.063(3) 0.040(2) -0.0105(18) 0.0071(17) 0.013(2) O54 0.079(2) 0.092(3) 0.059(2) -0.0176(18) 0.0269(18) 0.025(2) C55 0.041(2) 0.060(2) 0.0293(16) -0.0085(16) 0.0098(15) -0.0039(18) C56 0.0339(17) 0.045(2) 0.0275(15) -0.0051(14) 0.0054(13) -0.0051(15) C57 0.063(3) 0.107(5) 0.059(3) -0.013(3) 0.012(3) 0.021(3) C58 0.132(5) 0.114(5) 0.088(4) 0.009(4) 0.048(4) 0.069(4) C59 0.107(8) 0.116(8) 0.054(5) -0.011(6) -0.002(5) 0.061(7) C59' 0.111(9) 0.120(9) 0.090(8) 0.004(8) 0.011(7) 0.045(8) C60 0.0338(16) 0.0314(16) 0.0233(13) 0.0062(11) -0.0033(12) -0.0042(13) O60 0.0397(13) 0.0317(12) 0.0244(10) 0.0053(9) 0.0022(9) 0.0026(10) C61 0.0451(19) 0.0328(17) 0.0308(15) 0.0094(13) -0.0049(14) -0.0043(15) C62 0.048(2) 0.044(2) 0.0400(19) 0.0123(16) -0.0033(17) 0.0089(18) C63 0.068(3) 0.044(2) 0.060(3) 0.014(2) -0.004(2) 0.013(2) C64 0.097(4) 0.059(3) 0.072(3) 0.040(2) -0.013(3) 0.004(3) C65 0.137(5) 0.061(3) 0.043(2) 0.025(2) 0.003(3) 0.010(3) C66 0.098(4) 0.047(2) 0.0337(19) 0.0151(17) 0.004(2) 0.000(2) O64 0.148(4) 0.067(2) 0.104(3) 0.058(2) -0.015(3) 0.019(3) C67 0.108(5) 0.068(4) 0.135(5) 0.038(4) 0.015(4) 0.030(4) C68 0.114(5) 0.063(4) 0.126(5) 0.002(4) -0.027(4) 0.025(4) C69 0.093(5) 0.091(5) 0.141(6) 0.017(5) 0.000(5) 0.023(4) C4 0.033(3) 0.025(3) 0.021(2) 0.000(2) -0.006(2) -0.009(2) C70 0.041(3) 0.019(3) 0.019(2) -0.0002(19) -0.001(2) -0.004(2) O70 0.0325(13) 0.0234(13) 0.0260(10) -0.0064(9) -0.0004(10) -0.0022(11) C71 0.026(3) 0.024(3) 0.026(3) -0.005(2) -0.002(3) -0.005(3) C72 0.042(3) 0.021(3) 0.021(2) -0.005(2) 0.001(2) -0.008(3) C73 0.040(4) 0.035(3) 0.027(3) -0.002(3) 0.002(3) -0.005(3) C74 0.029(3) 0.045(4) 0.024(3) -0.001(3) -0.004(3) -0.006(3) O74 0.056(3) 0.065(4) 0.019(2) -0.002(2) -0.002(2) -0.019(3) C75 0.052(5) 0.041(5) 0.026(4) -0.004(3) -0.008(4) -0.015(4) C76 0.039(4) 0.044(4) 0.022(3) -0.006(3) -0.006(3) -0.017(3) C77 0.049(5) 0.066(6) 0.028(3) -0.009(3) -0.003(3) -0.015(4) C78 0.049(5) 0.084(7) 0.032(4) 0.006(4) -0.004(4) -0.026(5) C79 0.096(9) 0.087(9) 0.053(7) -0.007(6) 0.007(7) -0.030(8) C80 0.021(2) 0.032(3) 0.014(2) -0.001(2) -0.0116(19) -0.009(2) O80 0.0269(14) 0.0173(17) 0.0298(13) -0.0037(15) 0.0010(11) -0.0054(15) C81 0.033(3) 0.029(3) 0.025(3) 0.005(2) 0.003(3) 0.001(3) C82 0.034(5) 0.087(8) 0.033(4) -0.009(4) 0.003(4) 0.001(5) C83 0.035(4) 0.087(7) 0.030(4) -0.007(4) 0.006(3) -0.008(4) C84 0.030(4) 0.055(6) 0.040(5) 0.009(4) -0.002(3) -0.016(4) O84 0.033(3) 0.078(6) 0.067(4) 0.042(4) 0.006(3) 0.000(3) C85 0.033(4) 0.086(6) 0.046(4) 0.034(4) -0.011(3) -0.030(4) C86 0.043(4) 0.091(7) 0.026(3) 0.020(4) -0.003(3) -0.034(4) C87 0.036(4) 0.070(6) 0.047(4) 0.011(4) 0.003(4) -0.003(4) C88 0.056(6) 0.074(7) 0.046(5) 0.017(5) 0.012(4) -0.012(5) C89 0.053(6) 0.115(10) 0.072(7) -0.013(7) 0.019(5) -0.023(6) C5 0.0276(14) 0.0289(15) 0.0267(14) -0.0045(11) 0.0058(11) 0.0014(12) C90 0.0303(15) 0.0264(14) 0.0272(14) 0.0016(11) 0.0052(12) 0.0054(12) O90 0.0249(10) 0.0304(11) 0.0341(11) -0.0059(9) 0.0095(9) -0.0016(9) C91 0.0232(14) 0.0333(16) 0.0306(15) 0.0023(12) 0.0048(12) 0.0026(12) C92 0.0285(16) 0.049(2) 0.0295(15) 0.0033(14) 0.0031(13) 0.0041(15) C93 0.040(2) 0.056(2) 0.0348(17) 0.0108(16) 0.0083(15) 0.0049(18) C94 0.044(2) 0.058(3) 0.049(2) 0.0085(18) 0.0217(18) -0.0055(19) O94 0.078(2) 0.087(3) 0.0584(19) 0.0140(18) 0.0323(17) -0.027(2) C95 0.049(2) 0.062(3) 0.049(2) 0.0002(19) 0.0161(19) -0.020(2) C96 0.0331(17) 0.049(2) 0.0382(18) -0.0011(16) 0.0119(14) -0.0079(16) C97 0.070(3) 0.124(5) 0.047(3) 0.029(3) 0.019(2) -0.012(3) C98 0.203(8) 0.118(6) 0.076(4) 0.027(4) 0.080(5) -0.027(6) C99 0.105(5) 0.163(8) 0.063(4) 0.000(4) 0.007(4) -0.050(5) C100 0.0255(14) 0.0317(15) 0.0235(13) -0.0060(11) 0.0003(11) -0.0033(12) O100 0.0231(10) 0.0255(10) 0.0270(10) -0.0060(8) 0.0029(8) -0.0009(8) C101 0.0375(17) 0.0305(16) 0.0291(15) -0.0057(12) 0.0008(13) 0.0007(14) C102 0.0391(18) 0.0299(17) 0.0417(18) -0.0069(14) -0.0001(15) -0.0061(14) C103 0.058(2) 0.0325(19) 0.047(2) -0.0037(16) -0.0034(19) -0.0146(18) C104 0.116(4) 0.0216(18) 0.050(2) -0.0144(16) 0.011(3) -0.013(2) O104 0.174(4) 0.0333(17) 0.075(2) -0.0249(16) 0.039(3) -0.028(2) C105 0.116(4) 0.029(2) 0.079(3) -0.020(2) 0.049(3) -0.003(3) C106 0.078(3) 0.0305(19) 0.062(2) -0.0124(17) 0.037(2) -0.002(2) C107 0.122(5) 0.041(3) 0.112(5) -0.001(3) -0.034(4) -0.034(3) C6 0.031(3) 0.035(3) 0.036(3) -0.008(3) 0.006(3) 0.003(3) C110 0.051(4) 0.056(5) 0.012(2) -0.007(3) 0.004(3) 0.000(4) O110 0.0325(13) 0.0234(13) 0.0260(10) -0.0064(9) -0.0004(10) -0.0022(11) C111 0.029(3) 0.029(3) 0.032(3) -0.008(2) -0.003(3) -0.003(3) C112 0.028(3) 0.048(4) 0.037(3) -0.001(3) 0.006(3) 0.001(3) C113 0.032(4) 0.047(4) 0.030(3) 0.003(3) 0.009(3) -0.005(3) C114 0.030(4) 0.042(5) 0.027(4) -0.006(3) -0.005(3) 0.005(4) O114 0.035(3) 0.065(4) 0.035(3) -0.007(2) -0.001(2) -0.003(3) C115 0.023(3) 0.053(5) 0.037(4) -0.017(4) 0.000(3) -0.012(3) C116 0.022(3) 0.044(4) 0.030(3) -0.005(3) 0.004(3) -0.004(3) C117 0.049(5) 0.054(5) 0.027(3) 0.007(3) 0.003(4) -0.002(4) C118 0.046(5) 0.061(6) 0.034(4) 0.007(4) 0.001(4) -0.009(5) C119 0.075(7) 0.080(8) 0.045(5) -0.002(5) 0.011(5) -0.012(6) C120 0.030(3) 0.021(3) 0.036(3) 0.001(2) 0.004(3) 0.005(2) O120 0.0269(14) 0.0173(17) 0.0298(13) -0.0037(15) 0.0010(11) -0.0054(15) C121 0.030(4) 0.031(4) 0.031(4) -0.005(3) 0.006(3) -0.004(3) C122 0.025(3) 0.038(4) 0.047(4) -0.011(3) -0.001(3) 0.012(3) C123 0.030(4) 0.057(5) 0.049(4) -0.011(4) 0.001(3) 0.003(4) C124 0.035(4) 0.048(5) 0.037(5) -0.006(4) 0.005(4) 0.008(4) O124 0.024(3) 0.062(5) 0.038(3) -0.019(3) -0.001(2) 0.006(3) C125 0.041(4) 0.066(6) 0.044(4) -0.011(4) 0.004(3) 0.022(4) C126 0.027(3) 0.048(4) 0.044(4) -0.008(3) -0.005(3) 0.013(3) C127 0.050(5) 0.062(6) 0.054(5) 0.010(4) 0.012(5) 0.014(5) C128 0.066(7) 0.074(8) 0.043(5) -0.005(5) 0.009(5) 0.031(6) C129 0.054(5) 0.065(6) 0.058(5) -0.001(5) 0.003(4) 0.021(5) C211 0.124(8) 0.208(11) 0.133(8) 0.060(8) 0.002(7) -0.027(8) C212 0.119(7) 0.138(8) 0.080(5) -0.005(5) -0.021(5) -0.001(6) C213 0.144(9) 0.111(7) 0.201(11) 0.005(8) 0.052(8) 0.007(7) C214 0.34(2) 0.182(12) 0.137(10) -0.016(9) 0.025(12) -0.120(13) C215 0.167(10) 0.089(6) 0.141(8) -0.027(5) 0.008(7) -0.007(6) C216 0.217(12) 0.171(10) 0.122(8) -0.036(7) -0.006(8) -0.086(10) C311 0.100(4) 0.205(6) 0.264(5) 0.078(5) 0.046(5) -0.018(4) C312 0.122(5) 0.254(7) 0.251(6) 0.097(6) 0.063(5) 0.019(5) C313 0.109(5) 0.249(7) 0.217(6) 0.100(6) 0.040(5) 0.003(5) C314 0.113(5) 0.226(7) 0.196(6) 0.062(6) -0.024(5) -0.029(5) C315 0.115(5) 0.213(7) 0.208(6) 0.027(6) -0.038(5) -0.028(5) C316 0.110(5) 0.194(6) 0.232(6) 0.041(6) -0.023(5) -0.060(5) C317 0.131(7) 0.198(8) 0.295(8) 0.064(7) 0.070(6) -0.015(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ho1 O50 2.265(2) . ? Ho1 O60 2.279(2) . ? Ho1 O3 2.308(2) . ? Ho1 O40 2.318(2) . ? Ho1 O2 2.324(2) . ? Ho1 O30 2.362(2) . ? Ho1 O100 2.430(2) 2 ? Ho1 O1 2.5779(5) . ? Ho2 O10 2.263(2) . ? Ho2 O20 2.279(2) . ? Ho2 O2 2.297(2) . ? Ho2 O90 2.313(2) . ? Ho2 O3 2.339(2) 2 ? Ho2 O100 2.347(2) . ? Ho2 O40 2.436(2) . ? Ho2 O1 2.4760(5) . ? Ho3 O70 2.275(7) . ? Ho3 O70 2.275(7) 2 ? Ho3 O80 2.302(6) 2 ? Ho3 O80 2.302(6) . ? Ho3 O110 2.323(8) . ? Ho3 O110 2.323(8) 2 ? Ho3 O120 2.334(7) 2 ? Ho3 O120 2.334(7) . ? Ho3 O3 2.384(2) . ? Ho3 O3 2.384(2) 2 ? Ho3 O2 2.416(2) 2 ? Ho3 O2 2.416(2) . ? O1 Ho2 2.4760(5) 2 ? O1 Ho1 2.5779(5) 2 ? O1 H1O 0.835(18) . ? O2 H2O 1 . ? O3 Ho2 2.339(2) 2 ? O3 H3O 1 . ? C1 C20 1.397(5) . ? C1 C10 1.408(5) . ? C1 H1 0.95 . ? C10 O10 1.283(4) . ? C10 C11 1.484(5) . ? C11 C16 1.384(5) . ? C11 C12 1.386(6) . ? C12 C13 1.398(6) . ? C12 H12 0.95 . ? C13 C14 1.384(6) . ? C13 H13 0.95 . ? C14 C15 1.372(6) . ? C14 O14 1.376(5) . ? O14 C17 1.429(5) . ? C15 C16 1.394(5) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C17 C18 1.481(7) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.296(8) . ? C18 H18 0.95 . ? C19 H19A 0.95 . ? C19 H19B 0.95 . ? C20 O20 1.276(4) . ? C20 C21 1.494(5) . ? C21 C22 1.386(5) . ? C21 C26 1.402(5) . ? C22 C23 1.379(6) . ? C22 H22 0.95 . ? C23 C24 1.391(6) . ? C23 H23 0.95 . ? C24 O24 1.363(5) . ? C24 C25 1.372(7) . ? O24 C27' 1.422(16) . ? O24 C27 1.384(10) . ? C25 C26 1.386(6) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C27 C28 1.463(12) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.273(15) . ? C28 H28 0.95 . ? C29 H29A 0.95 . ? C29 H29B 0.95 . ? C27' C28' 1.499(14) . ? C27' H27C 0.99 . ? C27' H27D 0.99 . ? C28' C29' 1.282(17) . ? C28' H28' 0.95 . ? C29' H29C 0.95 . ? C29' H29D 0.95 . ? C2 C40 1.369(5) . ? C2 C30 1.437(5) . ? C2 H2 0.95 . ? C30 O30 1.249(4) . ? C30 C31 1.494(5) . ? C31 C32 1.389(5) . ? C31 C36 1.394(5) . ? C32 C33 1.388(5) . ? C32 H32 0.95 . ? C33 C34 1.377(6) . ? C33 H33 0.95 . ? C34 O34 1.386(5) . ? C34 C35 1.388(6) . ? O34 C37 1.435(6) . ? C35 C36 1.376(5) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 C38 1.471(9) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.356(9) . ? C38 H38 0.95 . ? C39 H39A 0.95 . ? C39 H39B 0.95 . ? C40 O40 1.316(4) . ? C40 C41 1.479(5) . ? C41 C46 1.406(5) . ? C41 C42 1.407(5) . ? C42 C43 1.392(5) . ? C42 H42 0.95 . ? C43 C44 1.379(6) . ? C43 H43 0.95 . ? C44 O44 1.375(5) . ? C44 C45 1.380(6) . ? O44 C47 1.396(7) . ? C45 C46 1.381(6) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 C48' 1.488(14) . ? C47 C48 1.524(11) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C47 H47C 0.99 . ? C47 H47D 0.99 . ? C48 C49 1.232(15) . ? C48 H48 0.95 . ? C49 H49A 0.95 . ? C49 H49B 0.95 . ? C48' C49' 1.319(15) . ? C48' H48' 0.95 . ? C49' H49C 0.95 . ? C49' H49D 0.95 . ? C3 C50 1.402(5) . ? C3 C60 1.406(5) . ? C3 H3 0.95 . ? C50 O50 1.281(4) . ? C50 C51 1.488(5) . ? C51 C52 1.392(5) . ? C51 C56 1.393(5) . ? C52 C53 1.383(6) . ? C52 H52 0.95 . ? C53 C54 1.383(6) . ? C53 H53 0.95 . ? C54 C55 1.370(6) . ? C54 O54 1.398(5) . ? O54 C57 1.420(6) . ? C55 C56 1.393(5) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 C58 1.508(9) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 C59' 1.073(13) . ? C58 C59 1.215(12) . ? C58 H58 0.95 . ? C58 H58' 0.95 . ? C59 H58' 1.1369 . ? C59 H59A 0.95 . ? C59 H59B 0.95 . ? C59' H59C 0.95 . ? C59' H59D 0.95 . ? C60 O60 1.266(4) . ? C60 C61 1.490(5) . ? C61 C62 1.372(6) . ? C61 C66 1.400(5) . ? C62 C63 1.390(6) . ? C62 H62 0.95 . ? C63 C64 1.384(7) . ? C63 H63 0.95 . ? C64 O64 1.362(6) . ? C64 C65 1.381(8) . ? C65 C66 1.375(6) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? O64 C67 1.372(9) . ? C67 C68 1.584(10) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? C68 C69 1.154(10) . ? C68 H68 0.95 . ? C69 H69A 0.95 . ? C69 H69B 0.95 . ? C4 C80 1.385(8) . ? C4 C70 1.396(9) . ? C4 H4 0.95 . ? C70 O70 1.284(9) . ? C70 C71 1.501(7) . ? C71 C76 1.376(8) . ? C71 C72 1.394(8) . ? C72 C73 1.379(7) . ? C72 H72 0.95 . ? C73 C74 1.395(8) . ? C73 H73 0.95 . ? C74 C75 1.371(9) . ? C74 O74 1.383(7) . ? O74 C77 1.406(9) . ? C75 C76 1.389(9) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? C77 C78 1.538(11) . ? C77 H77A 0.99 . ? C77 H77B 0.99 . ? C78 C79 1.258(11) . ? C78 H78 0.95 . ? C79 H79A 0.95 . ? C79 H79B 0.95 . ? C80 O80 1.274(7) . ? C80 C81 1.489(8) . ? C81 C82 1.377(9) . ? C81 C86 1.380(8) . ? C82 C83 1.381(10) . ? C82 H82 0.95 . ? C83 C84 1.376(9) . ? C83 H83 0.95 . ? C84 O84 1.365(9) . ? C84 C85 1.371(9) . ? O84 C87 1.409(10) . ? C85 C86 1.362(9) . ? C85 H85 0.95 . ? C86 H86 0.95 . ? C87 C88 1.480(11) . ? C87 H87A 0.99 . ? C87 H87B 0.99 . ? C88 C89 1.236(11) . ? C88 H88 0.95 . ? C89 H89A 0.95 . ? C89 H89B 0.95 . ? C5 C100 1.373(5) . ? C5 C90 1.431(5) . ? C5 H5 0.95 . ? C90 O90 1.258(4) . ? C90 C91 1.477(5) . ? C91 C92 1.385(5) . ? C91 C96 1.396(5) . ? C92 C93 1.395(5) . ? C92 H92 0.95 . ? C93 C94 1.371(6) . ? C93 H93 0.95 . ? C94 O94 1.380(5) . ? C94 C95 1.384(6) . ? O94 C97 1.425(6) . ? C95 C96 1.375(6) . ? C95 H95 0.95 . ? C96 H96 0.95 . ? C97 C98 1.565(9) . ? C97 H97A 0.99 . ? C97 H97B 0.99 . ? C98 C99 1.187(10) . ? C98 H98 0.95 . ? C99 H99A 0.95 . ? C99 H99B 0.95 . ? C100 O100 1.312(4) . ? C100 C101 1.492(5) . ? O100 Ho1 2.430(2) 2 ? C101 C106 1.393(5) . ? C101 C102 1.396(5) . ? C102 C103 1.383(5) . ? C102 H102 0.95 . ? C103 C104 1.376(7) . ? C103 H103 0.95 . ? C104 C105 1.373(8) . ? C104 O104 1.375(5) . ? O104 C107 1.417(8) . ? C105 C106 1.378(6) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C107 C108 1.483(10) . ? C107 C10A 1.531(18) . ? C107 H10A 0.99 . ? C107 H10B 0.99 . ? C107 H10F 0.99 . ? C107 H10G 0.99 . ? C108 C109 1.207(17) . ? C108 H108 0.95 . ? C109 H10C 0.95 . ? C109 H10D 0.95 . ? C10A C10B 1.210(19) . ? C10A H10E 0.95 . ? C10B H10H 0.95 . ? C10B H10I 0.95 . ? C6 C110 1.414(10) . ? C6 C120 1.423(9) . ? C6 H6 0.95 . ? C110 O110 1.292(9) . ? C110 C111 1.474(8) . ? C111 C116 1.377(8) . ? C111 C112 1.386(8) . ? C112 C113 1.394(8) . ? C112 H112 0.95 . ? C113 C114 1.373(9) . ? C113 H113 0.95 . ? C114 O114 1.375(8) . ? C114 C115 1.393(9) . ? O114 C117 1.444(8) . ? C115 C116 1.370(8) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C117 C118 1.514(11) . ? C117 H11A 0.99 . ? C117 H11B 0.99 . ? C118 C119 1.276(11) . ? C118 H118 0.95 . ? C119 H11C 0.95 . ? C119 H11D 0.95 . ? C120 O120 1.307(8) . ? C120 C121 1.510(8) . ? C121 C126 1.381(9) . ? C121 C122 1.382(8) . ? C122 C123 1.383(8) . ? C122 H122 0.95 . ? C123 C124 1.386(10) . ? C123 H123 0.95 . ? C124 O124 1.383(9) . ? C124 C125 1.389(10) . ? O124 C127 1.426(10) . ? C125 C126 1.389(9) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C127 C128 1.475(12) . ? C127 H12A 0.99 . ? C127 H12B 0.99 . ? C128 C129 1.272(10) . ? C128 H128 0.95 . ? C129 H12C 0.95 . ? C129 H12D 0.95 . ? C211 C216 1.410(7) . ? C211 C212 1.417(7) . ? C211 C217 1.472(8) . ? C211 H211 0.877(8) . ? C212 C213 1.394(7) . ? C212 C218 1.519(9) . ? C212 H212 0.880(8) . ? C213 C214 1.351(8) . ? C213 H213 0.95 . ? C214 C215 1.372(8) . ? C214 H214 0.95 . ? C215 C216 1.387(8) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C217 H211 0.65(2) . ? C217 H21A 0.98 . ? C217 H21B 0.98 . ? C217 H21C 0.98 . ? C218 H212 0.83(3) . ? C218 H21D 0.98 . ? C218 H21E 0.98 . ? C218 H21F 0.98 . ? C311 C316 1.370(8) . ? C311 C312 1.405(8) . ? C311 C317 1.510(8) . ? C312 C313 1.378(8) . ? C312 H312 0.95 . ? C313 C314 1.392(8) . ? C313 H313 0.95 . ? C314 C315 1.367(8) . ? C314 H314 0.95 . ? C315 C316 1.377(8) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C317 H31A 0.98 . ? C317 H31B 0.98 . ? C317 H31C 0.98 . ? 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 O50 Ho1 O60 74.41(8) . . ? O50 Ho1 O3 75.98(7) . . ? O60 Ho1 O3 140.25(8) . . ? O50 Ho1 O40 152.97(8) . . ? O60 Ho1 O40 81.24(8) . . ? O3 Ho1 O40 131.05(7) . . ? O50 Ho1 O2 114.50(8) . . ? O60 Ho1 O2 146.13(8) . . ? O3 Ho1 O2 71.46(7) . . ? O40 Ho1 O2 80.12(8) . . ? O50 Ho1 O30 89.05(8) . . ? O60 Ho1 O30 76.10(8) . . ? O3 Ho1 O30 129.22(8) . . ? O40 Ho1 O30 73.65(8) . . ? O2 Ho1 O30 71.64(7) . . ? O50 Ho1 O100 91.82(8) . 2 ? O60 Ho1 O100 77.95(8) . 2 ? O3 Ho1 O100 77.10(7) . 2 ? O40 Ho1 O100 94.45(7) . 2 ? O2 Ho1 O100 131.46(7) . 2 ? O30 Ho1 O100 152.78(8) . 2 ? O50 Ho1 O1 140.38(6) . . ? O60 Ho1 O1 127.61(9) . . ? O3 Ho1 O1 67.27(7) . . ? O40 Ho1 O1 65.27(6) . . ? O2 Ho1 O1 67.57(7) . . ? O30 Ho1 O1 125.56(6) . . ? O100 Ho1 O1 66.53(6) 2 . ? O10 Ho2 O20 75.11(8) . . ? O10 Ho2 O2 74.98(8) . . ? O20 Ho2 O2 138.07(7) . . ? O10 Ho2 O90 81.26(9) . . ? O20 Ho2 O90 78.27(8) . . ? O2 Ho2 O90 124.72(8) . . ? O10 Ho2 O3 114.02(8) . 2 ? O20 Ho2 O3 147.30(7) . 2 ? O2 Ho2 O3 72.96(7) . 2 ? O90 Ho2 O3 72.65(8) . 2 ? O10 Ho2 O100 148.10(8) . . ? O20 Ho2 O100 79.93(7) . . ? O2 Ho2 O100 136.28(7) . . ? O90 Ho2 O100 74.41(8) . . ? O3 Ho2 O100 78.16(7) 2 . ? O10 Ho2 O40 94.31(8) . . ? O20 Ho2 O40 75.43(8) . . ? O2 Ho2 O40 78.23(7) . . ? O90 Ho2 O40 153.58(8) . . ? O3 Ho2 O40 131.64(7) 2 . ? O100 Ho2 O40 98.35(7) . . ? O10 Ho2 O1 142.00(7) . . ? O20 Ho2 O1 124.61(9) . . ? O2 Ho2 O1 69.77(7) . . ? O90 Ho2 O1 131.08(6) . . ? O3 Ho2 O1 68.61(7) 2 . ? O100 Ho2 O1 69.44(6) . . ? O40 Ho2 O1 65.28(6) . . ? O70 Ho3 O70 119.3(4) . 2 ? O70 Ho3 O80 77.7(3) . 2 ? O70 Ho3 O80 75.0(3) 2 2 ? O70 Ho3 O80 75.0(3) . . ? O70 Ho3 O80 77.7(3) 2 . ? O80 Ho3 O80 124.3(3) 2 . ? O70 Ho3 O110 3.5(4) . . ? O70 Ho3 O110 116.98(12) 2 . ? O80 Ho3 O110 79.1(3) 2 . ? O80 Ho3 O110 71.7(3) . . ? O70 Ho3 O110 116.98(12) . 2 ? O70 Ho3 O110 3.5(4) 2 2 ? O80 Ho3 O110 71.7(3) 2 2 ? O80 Ho3 O110 79.1(3) . 2 ? O110 Ho3 O110 114.7(5) . 2 ? O70 Ho3 O120 76.0(3) . 2 ? O70 Ho3 O120 71.2(2) 2 2 ? O80 Ho3 O120 117.92(14) 2 2 ? O80 Ho3 O120 7.6(2) . 2 ? O110 Ho3 O120 72.6(3) . 2 ? O110 Ho3 O120 72.3(3) 2 2 ? O70 Ho3 O120 71.2(2) . . ? O70 Ho3 O120 76.0(3) 2 . ? O80 Ho3 O120 7.6(2) 2 . ? O80 Ho3 O120 117.92(14) . . ? O110 Ho3 O120 72.3(3) . . ? O110 Ho3 O120 72.6(3) 2 . ? O120 Ho3 O120 111.9(3) 2 . ? O70 Ho3 O3 85.4(2) . . ? O70 Ho3 O3 133.1(2) 2 . ? O80 Ho3 O3 72.43(16) 2 . ? O80 Ho3 O3 149.14(14) . . ? O110 Ho3 O3 88.8(2) . . ? O110 Ho3 O3 131.6(2) 2 . ? O120 Ho3 O3 155.32(15) 2 . ? O120 Ho3 O3 76.06(17) . . ? O70 Ho3 O3 133.1(2) . 2 ? O70 Ho3 O3 85.4(2) 2 2 ? O80 Ho3 O3 149.14(13) 2 2 ? O80 Ho3 O3 72.43(16) . 2 ? O110 Ho3 O3 131.6(2) . 2 ? O110 Ho3 O3 88.8(2) 2 2 ? O120 Ho3 O3 76.06(17) 2 2 ? O120 Ho3 O3 155.32(15) . 2 ? O3 Ho3 O3 106.83(10) . 2 ? O70 Ho3 O2 152.4(2) . 2 ? O70 Ho3 O2 73.2(2) 2 2 ? O80 Ho3 O2 82.88(13) 2 2 ? O80 Ho3 O2 132.56(16) . 2 ? O110 Ho3 O2 155.6(2) . 2 ? O110 Ho3 O2 74.2(2) 2 2 ? O120 Ho3 O2 131.05(17) 2 2 ? O120 Ho3 O2 90.35(13) . 2 ? O3 Ho3 O2 70.10(7) . 2 ? O3 Ho3 O2 68.61(7) 2 2 ? O70 Ho3 O2 73.2(2) . . ? O70 Ho3 O2 152.4(2) 2 . ? O80 Ho3 O2 132.56(16) 2 . ? O80 Ho3 O2 82.88(13) . . ? O110 Ho3 O2 74.2(2) . . ? O110 Ho3 O2 155.6(2) 2 . ? O120 Ho3 O2 90.35(13) 2 . ? O120 Ho3 O2 131.05(17) . . ? O3 Ho3 O2 68.61(7) . . ? O3 Ho3 O2 70.10(7) 2 . ? O2 Ho3 O2 107.47(10) 2 . ? Ho2 O1 Ho2 160.93(13) 2 . ? Ho2 O1 Ho1 88.75(2) 2 . ? Ho2 O1 Ho1 87.98(2) . . ? Ho2 O1 Ho1 87.98(2) 2 2 ? Ho2 O1 Ho1 88.75(2) . 2 ? Ho1 O1 Ho1 160.16(12) . 2 ? Ho2 O1 H1O 99.53(6) 2 . ? Ho2 O1 H1O 99.53(7) . . ? Ho1 O1 H1O 99.92(6) . . ? Ho1 O1 H1O 99.92(6) 2 . ? Ho2 O2 Ho1 98.88(8) . . ? Ho2 O2 Ho3 108.25(7) . . ? Ho1 O2 Ho3 108.91(8) . . ? Ho2 O2 H2O 113.3 . . ? Ho1 O2 H2O 113.3 . . ? Ho3 O2 H2O 113.3 . . ? Ho1 O3 Ho2 99.06(8) . 2 ? Ho1 O3 Ho3 110.58(8) . . ? Ho2 O3 Ho3 107.97(7) 2 . ? Ho1 O3 H3O 112.8 . . ? Ho2 O3 H3O 112.8 2 . ? Ho3 O3 H3O 112.8 . . ? C20 C1 C10 124.0(3) . . ? C20 C1 H1 118 . . ? C10 C1 H1 118 . . ? O10 C10 C1 123.9(3) . . ? O10 C10 C11 116.1(3) . . ? C1 C10 C11 120.0(3) . . ? C10 O10 Ho2 134.0(2) . . ? C16 C11 C12 118.5(3) . . ? C16 C11 C10 122.9(4) . . ? C12 C11 C10 118.6(3) . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 119.6(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 O14 124.0(4) . . ? C15 C14 C13 120.6(4) . . ? O14 C14 C13 115.4(4) . . ? C14 O14 C17 117.5(4) . . ? C14 C15 C16 119.3(4) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C11 C16 C15 121.4(4) . . ? C11 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? O14 C17 C18 108.6(4) . . ? O14 C17 H17A 110 . . ? C18 C17 H17A 110 . . ? O14 C17 H17B 110 . . ? C18 C17 H17B 110 . . ? H17A C17 H17B 108.4 . . ? C19 C18 C17 125.8(5) . . ? C19 C18 H18 117.1 . . ? C17 C18 H18 117.1 . . ? C18 C19 H19A 120 . . ? C18 C19 H19B 120 . . ? H19A C19 H19B 120 . . ? O20 C20 C1 124.1(3) . . ? O20 C20 C21 115.1(3) . . ? C1 C20 C21 120.7(3) . . ? C20 O20 Ho2 135.2(2) . . ? C22 C21 C26 117.6(4) . . ? C22 C21 C20 119.4(3) . . ? C26 C21 C20 122.9(3) . . ? C23 C22 C21 122.1(4) . . ? C23 C22 H22 119 . . ? C21 C22 H22 119 . . ? C22 C23 C24 119.2(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? O24 C24 C25 119.0(4) . . ? O24 C24 C23 120.9(4) . . ? C25 C24 C23 120.0(4) . . ? C24 O24 C27' 119.6(6) . . ? C24 O24 C27 123.1(5) . . ? C27' O24 C27 116.9(7) . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 120.7(4) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? O24 C27 C28 118.5(9) . . ? O24 C27 H27A 107.7 . . ? C28 C27 H27A 107.7 . . ? O24 C27 H27B 107.7 . . ? C28 C27 H27B 107.7 . . ? H27A C27 H27B 107.1 . . ? C29 C28 C27 125.5(15) . . ? C29 C28 H28 117.2 . . ? C27 C28 H28 117.2 . . ? C28 C29 H29A 120 . . ? C28 C29 H29B 120 . . ? H29A C29 H29B 120 . . ? O24 C27' C28' 108.5(12) . . ? O24 C27' H27C 110 . . ? C28' C27' H27C 110 . . ? O24 C27' H27D 110 . . ? C28' C27' H27D 110 . . ? H27C C27' H27D 108.4 . . ? C29' C28' C27' 117.5(16) . . ? C29' C28' H28' 121.2 . . ? C27' C28' H28' 121.2 . . ? C28' C29' H29C 120 . . ? C28' C29' H29D 120 . . ? H29C C29' H29D 120 . . ? C40 C2 C30 124.4(3) . . ? C40 C2 H2 117.8 . . ? C30 C2 H2 117.8 . . ? O30 C30 C2 123.8(3) . . ? O30 C30 C31 117.3(3) . . ? C2 C30 C31 118.9(3) . . ? C30 O30 Ho1 131.9(2) . . ? C32 C31 C36 117.8(3) . . ? C32 C31 C30 119.8(3) . . ? C36 C31 C30 122.3(3) . . ? C33 C32 C31 121.8(4) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C34 C33 C32 118.9(4) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 O34 125.3(4) . . ? C33 C34 C35 120.6(4) . . ? O34 C34 C35 114.1(4) . . ? C34 O34 C37 119.8(4) . . ? C36 C35 C34 119.6(4) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C31 121.2(4) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? O34 C37 C38 111.8(5) . . ? O34 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? O34 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 107.9 . . ? C39 C38 C37 123.9(7) . . ? C39 C38 H38 118 . . ? C37 C38 H38 118 . . ? C38 C39 H39A 120 . . ? C38 C39 H39B 120 . . ? H39A C39 H39B 120 . . ? O40 C40 C2 122.7(3) . . ? O40 C40 C41 115.1(3) . . ? C2 C40 C41 122.2(3) . . ? C40 O40 Ho1 125.0(2) . . ? C40 O40 Ho2 123.7(2) . . ? Ho1 O40 Ho2 95.18(8) . . ? C46 C41 C42 116.9(3) . . ? C46 C41 C40 123.4(3) . . ? C42 C41 C40 119.7(3) . . ? C43 C42 C41 121.8(3) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C44 C43 C42 119.4(4) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? O44 C44 C43 123.0(4) . . ? O44 C44 C45 116.7(4) . . ? C43 C44 C45 120.3(4) . . ? C44 O44 C47 118.0(4) . . ? C44 C45 C46 120.5(4) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C41 121.2(4) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? O44 C47 C48' 109.1(8) . . ? O44 C47 C48 110.7(6) . . ? O44 C47 H47A 109.5 . . ? C48 C47 H47A 109.5 . . ? O44 C47 H47B 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 108.1 . . ? O44 C47 H47C 109.9 . . ? C48' C47 H47C 113.4 . . ? O44 C47 H47D 109.5 . . ? C48' C47 H47D 106.6 . . ? H47C C47 H47D 108.2 . . ? C49 C48 C47 131.4(15) . . ? C49 C48 H48 114.3 . . ? C47 C48 H48 114.3 . . ? C48 C49 H49A 120 . . ? C48 C49 H49B 120 . . ? H49A C49 H49B 120 . . ? C49' C48' C47 117.5(14) . . ? C49' C48' H48' 121.2 . . ? C47 C48' H48' 121.2 . . ? C48' C49' H49C 120 . . ? C48' C49' H49D 120 . . ? H49C C49' H49D 120 . . ? C50 C3 C60 124.2(3) . . ? C50 C3 H3 117.9 . . ? C60 C3 H3 117.9 . . ? O50 C50 C3 123.5(3) . . ? O50 C50 C51 116.1(3) . . ? C3 C50 C51 120.4(3) . . ? C50 O50 Ho1 137.0(2) . . ? C52 C51 C56 117.0(3) . . ? C52 C51 C50 118.8(3) . . ? C56 C51 C50 124.1(3) . . ? C53 C52 C51 121.6(4) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C54 120.0(4) . . ? C52 C53 H53 120 . . ? C54 C53 H53 120 . . ? C55 C54 C53 119.8(4) . . ? C55 C54 O54 124.8(4) . . ? C53 C54 O54 115.4(4) . . ? C54 O54 C57 118.6(4) . . ? C54 C55 C56 119.9(4) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? C55 C56 C51 121.6(4) . . ? C55 C56 H56 119.2 . . ? C51 C56 H56 119.2 . . ? O54 C57 C58 107.6(5) . . ? O54 C57 H57A 110.2 . . ? C58 C57 H57A 110.2 . . ? O54 C57 H57B 110.2 . . ? C58 C57 H57B 110.2 . . ? H57A C57 H57B 108.5 . . ? C59' C58 C57 150.7(13) . . ? C59 C58 C57 129.5(10) . . ? C59 C58 H58 115.3 . . ? C57 C58 H58 115.3 . . ? C59' C58 H58' 104.7 . . ? C57 C58 H58' 104.6 . . ? H58 C58 H58' 104.8 . . ? C58 C59 H59A 120 . . ? C58 C59 H59B 120 . . ? H59A C59 H59B 120 . . ? C58 C59' H59C 120 . . ? C58 C59' H59D 120 . . ? H59C C59' H59D 120 . . ? O60 C60 C3 124.1(3) . . ? O60 C60 C61 116.1(3) . . ? C3 C60 C61 119.8(3) . . ? C60 O60 Ho1 136.2(2) . . ? C62 C61 C66 117.7(4) . . ? C62 C61 C60 118.9(3) . . ? C66 C61 C60 123.4(4) . . ? C61 C62 C63 122.1(4) . . ? C61 C62 H62 119 . . ? C63 C62 H62 119 . . ? C64 C63 C62 119.0(5) . . ? C64 C63 H63 120.5 . . ? C62 C63 H63 120.5 . . ? O64 C64 C65 116.1(5) . . ? O64 C64 C63 124.1(6) . . ? C65 C64 C63 119.9(4) . . ? C66 C65 C64 120.2(5) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C65 C66 C61 121.0(5) . . ? C65 C66 H66 119.5 . . ? C61 C66 H66 119.5 . . ? C64 O64 C67 119.8(5) . . ? O64 C67 C68 102.3(6) . . ? O64 C67 H67A 111.3 . . ? C68 C67 H67A 111.3 . . ? O64 C67 H67B 111.3 . . ? C68 C67 H67B 111.3 . . ? H67A C67 H67B 109.2 . . ? C69 C68 C67 120.9(8) . . ? C69 C68 H68 119.6 . . ? C67 C68 H68 119.6 . . ? C68 C69 H69A 120 . . ? C68 C69 H69B 120 . . ? H69A C69 H69B 120 . . ? C80 C4 C70 123.9(5) . . ? C80 C4 H4 118 . . ? C70 C4 H4 118 . . ? O70 C70 C4 124.5(6) . . ? O70 C70 C71 115.0(6) . . ? C4 C70 C71 120.3(5) . . ? C70 O70 Ho3 131.0(6) . . ? C76 C71 C72 118.1(6) . . ? C76 C71 C70 124.0(6) . . ? C72 C71 C70 117.7(5) . . ? C73 C72 C71 120.8(6) . . ? C73 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? C72 C73 C74 120.1(6) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C75 C74 O74 126.7(6) . . ? C75 C74 C73 119.2(6) . . ? O74 C74 C73 114.1(6) . . ? C74 O74 C77 120.0(6) . . ? C74 C75 C76 120.2(7) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C71 C76 C75 121.3(7) . . ? C71 C76 H76 119.3 . . ? C75 C76 H76 119.3 . . ? O74 C77 C78 112.6(8) . . ? O74 C77 H77A 109.1 . . ? C78 C77 H77A 109.1 . . ? O74 C77 H77B 109.1 . . ? C78 C77 H77B 109.1 . . ? H77A C77 H77B 107.8 . . ? C79 C78 C77 122.7(11) . . ? C79 C78 H78 118.7 . . ? C77 C78 H78 118.7 . . ? C78 C79 H79A 120 . . ? C78 C79 H79B 120 . . ? H79A C79 H79B 120 . . ? O80 C80 C4 126.0(6) . . ? O80 C80 C81 113.0(5) . . ? C4 C80 C81 120.9(5) . . ? C80 O80 Ho3 131.6(4) . . ? C82 C81 C86 115.5(6) . . ? C82 C81 C80 120.6(6) . . ? C86 C81 C80 123.8(5) . . ? C81 C82 C83 122.9(7) . . ? C81 C82 H82 118.5 . . ? C83 C82 H82 118.5 . . ? C84 C83 C82 118.8(7) . . ? C84 C83 H83 120.6 . . ? C82 C83 H83 120.6 . . ? O84 C84 C85 117.0(7) . . ? O84 C84 C83 123.2(7) . . ? C85 C84 C83 119.6(7) . . ? C84 O84 C87 120.9(7) . . ? C86 C85 C84 119.7(6) . . ? C86 C85 H85 120.1 . . ? C84 C85 H85 120.1 . . ? C85 C86 C81 123.1(6) . . ? C85 C86 H86 118.4 . . ? C81 C86 H86 118.4 . . ? O84 C87 C88 106.1(7) . . ? O84 C87 H87A 110.5 . . ? C88 C87 H87A 110.5 . . ? O84 C87 H87B 110.5 . . ? C88 C87 H87B 110.5 . . ? H87A C87 H87B 108.7 . . ? C89 C88 C87 126.7(11) . . ? C89 C88 H88 116.6 . . ? C87 C88 H88 116.6 . . ? C88 C89 H89A 120 . . ? C88 C89 H89B 120 . . ? H89A C89 H89B 120 . . ? C100 C5 C90 125.1(3) . . ? C100 C5 H5 117.4 . . ? C90 C5 H5 117.4 . . ? O90 C90 C5 123.5(3) . . ? O90 C90 C91 116.4(3) . . ? C5 C90 C91 120.1(3) . . ? C90 O90 Ho2 132.8(2) . . ? C92 C91 C96 118.5(3) . . ? C92 C91 C90 122.9(3) . . ? C96 C91 C90 118.5(3) . . ? C91 C92 C93 121.3(4) . . ? C91 C92 H92 119.3 . . ? C93 C92 H92 119.4 . . ? C94 C93 C92 118.9(4) . . ? C94 C93 H93 120.5 . . ? C92 C93 H93 120.5 . . ? C93 C94 O94 124.5(4) . . ? C93 C94 C95 120.7(4) . . ? O94 C94 C95 114.7(4) . . ? C94 O94 C97 117.5(4) . . ? C96 C95 C94 120.2(4) . . ? C96 C95 H95 119.9 . . ? C94 C95 H95 119.9 . . ? C95 C96 C91 120.3(4) . . ? C95 C96 H96 119.8 . . ? C91 C96 H96 119.8 . . ? O94 C97 C98 103.5(5) . . ? O94 C97 H97A 111.1 . . ? C98 C97 H97A 111.1 . . ? O94 C97 H97B 111.1 . . ? C98 C97 H97B 111.1 . . ? H97A C97 H97B 109 . . ? C99 C98 C97 125.8(9) . . ? C99 C98 H98 117.1 . . ? C97 C98 H98 117.1 . . ? C98 C99 H99A 120 . . ? C98 C99 H99B 120 . . ? H99A C99 H99B 120 . . ? O100 C100 C5 124.0(3) . . ? O100 C100 C101 115.6(3) . . ? C5 C100 C101 120.4(3) . . ? C100 O100 Ho2 123.35(18) . . ? C100 O100 Ho1 126.33(18) . 2 ? Ho2 O100 Ho1 95.46(7) . 2 ? C106 C101 C102 117.6(3) . . ? C106 C101 C100 122.5(3) . . ? C102 C101 C100 119.9(3) . . ? C103 C102 C101 121.9(4) . . ? C103 C102 H102 119.1 . . ? C101 C102 H102 119.1 . . ? C104 C103 C102 119.2(4) . . ? C104 C103 H103 120.4 . . ? C102 C103 H103 120.4 . . ? C105 C104 O104 116.7(5) . . ? C105 C104 C103 119.9(4) . . ? O104 C104 C103 123.4(5) . . ? C104 O104 C107 118.7(5) . . ? C104 C105 C106 121.2(5) . . ? C104 C105 H105 119.4 . . ? C106 C105 H105 119.4 . . ? C105 C106 C101 120.2(5) . . ? C105 C106 H106 119.9 . . ? C101 C106 H106 119.9 . . ? O104 C107 C108 114.1(7) . . ? O104 C107 C10A 112.7(13) . . ? O104 C107 H10A 108.7 . . ? C108 C107 H10A 108.7 . . ? C10A C107 H10A 116.9 . . ? O104 C107 H10B 108.7 . . ? C108 C107 H10B 108.7 . . ? C10A C107 H10B 101.4 . . ? H10A C107 H10B 107.6 . . ? O104 C107 H10F 110.9 . . ? C10A C107 H10F 105.1 . . ? H10B C107 H10F 117.6 . . ? O104 C107 H10G 111.1 . . ? C108 C107 H10G 114.5 . . ? C10A C107 H10G 108 . . ? H10F C107 H10G 108.8 . . ? C109 C108 C107 136.2(17) . . ? C109 C108 H108 111.9 . . ? C107 C108 H108 111.9 . . ? C108 C109 H10C 120 . . ? C108 C109 H10D 120 . . ? H10C C109 H10D 120 . . ? C10B C10A C107 111.8(18) . . ? C10B C10A H10E 124.1 . . ? C107 C10A H10E 124.1 . . ? C10A C10B H10H 120 . . ? C10A C10B H10I 120 . . ? H10H C10B H10I 120 . . ? C110 C6 C120 124.2(6) . . ? C110 C6 H6 117.9 . . ? C120 C6 H6 117.9 . . ? O110 C110 C6 121.6(7) . . ? O110 C110 C111 114.8(7) . . ? C6 C110 C111 123.4(6) . . ? C110 O110 Ho3 131.5(7) . . ? C116 C111 C112 118.7(6) . . ? C116 C111 C110 119.3(6) . . ? C112 C111 C110 121.9(6) . . ? C111 C112 C113 120.9(6) . . ? C111 C112 H112 119.6 . . ? C113 C112 H112 119.6 . . ? C114 C113 C112 119.2(6) . . ? C114 C113 H113 120.4 . . ? C112 C113 H113 120.4 . . ? C113 C114 O114 123.1(7) . . ? C113 C114 C115 120.0(6) . . ? O114 C114 C115 116.9(7) . . ? C114 O114 C117 118.5(6) . . ? C116 C115 C114 119.9(7) . . ? C116 C115 H115 120.1 . . ? C114 C115 H115 120.1 . . ? C115 C116 C111 121.1(6) . . ? C115 C116 H116 119.5 . . ? C111 C116 H116 119.5 . . ? O114 C117 C118 105.5(7) . . ? O114 C117 H11A 110.6 . . ? C118 C117 H11A 110.6 . . ? O114 C117 H11B 110.6 . . ? C118 C117 H11B 110.6 . . ? H11A C117 H11B 108.8 . . ? C119 C118 C117 121.6(10) . . ? C119 C118 H118 119.2 . . ? C117 C118 H118 119.2 . . ? C118 C119 H11C 120 . . ? C118 C119 H11D 120 . . ? H11C C119 H11D 120 . . ? O120 C120 C6 124.6(6) . . ? O120 C120 C121 117.3(6) . . ? C6 C120 C121 118.1(6) . . ? C120 O120 Ho3 130.1(5) . . ? C126 C121 C122 118.9(6) . . ? C126 C121 C120 123.1(6) . . ? C122 C121 C120 117.8(6) . . ? C121 C122 C123 121.3(7) . . ? C121 C122 H122 119.4 . . ? C123 C122 H122 119.4 . . ? C122 C123 C124 119.4(7) . . ? C122 C123 H123 120.3 . . ? C124 C123 H123 120.3 . . ? O124 C124 C123 117.2(7) . . ? O124 C124 C125 122.9(7) . . ? C123 C124 C125 119.9(7) . . ? C124 O124 C127 117.8(7) . . ? C124 C125 C126 119.6(7) . . ? C124 C125 H125 120.2 . . ? C126 C125 H125 120.2 . . ? C121 C126 C125 120.7(7) . . ? C121 C126 H126 119.6 . . ? C125 C126 H126 119.6 . . ? O124 C127 C128 110.8(8) . . ? O124 C127 H12A 109.5 . . ? C128 C127 H12A 109.5 . . ? O124 C127 H12B 109.5 . . ? C128 C127 H12B 109.5 . . ? H12A C127 H12B 108.1 . . ? C129 C128 C127 127.4(9) . . ? C129 C128 H128 116.3 . . ? C127 C128 H128 116.3 . . ? C128 C129 H12C 120 . . ? C128 C129 H12D 120 . . ? H12C C129 H12D 120 . . ? C216 C211 C212 117.3(6) . . ? C216 C211 C217 118.6(8) . . ? C212 C211 C217 123.0(7) . . ? C216 C211 H211 121.5(10) . . ? C212 C211 H211 121.1(10) . . ? C213 C212 C211 116.3(6) . . ? C213 C212 C218 101.8(8) . . ? C213 C212 H212 123.0(10) . . ? C211 C212 H212 120.4(10) . . ? C214 C213 C212 128.3(8) . . ? C214 C213 H213 115.8 . . ? C212 C213 H213 115.9 . . ? C213 C214 C215 111.7(8) . . ? C213 C214 H214 124.1 . . ? C215 C214 H214 124.1 . . ? C214 C215 C216 126.1(8) . . ? C214 C215 H215 116.9 . . ? C216 C215 H215 116.9 . . ? C215 C216 C211 119.0(7) . . ? C215 C216 H216 120.5 . . ? C211 C216 H216 120.5 . . ? C211 C217 H21A 109.5 . . ? C211 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? C211 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C212 C218 H21D 109.5 . . ? C212 C218 H21E 109.4 . . ? H212 C218 H21E 101.9 . . ? C212 C218 H21F 109.5 . . ? C316 C311 C312 119.7(8) . . ? C316 C311 C317 117.8(8) . . ? C312 C311 C317 122.5(8) . . ? C313 C312 C311 123.7(8) . . ? C313 C312 H312 118.2 . . ? C311 C312 H312 118.2 . . ? C312 C313 C314 115.3(8) . . ? C312 C313 H313 122.3 . . ? C314 C313 H313 122.3 . . ? C315 C314 C313 119.6(9) . . ? C315 C314 H314 120.2 . . ? C313 C314 H314 120.2 . . ? C314 C315 C316 125.1(9) . . ? C314 C315 H315 117.5 . . ? C316 C315 H315 117.5 . . ? C311 C316 C315 115.8(8) . . ? C311 C316 H316 122.1 . . ? C315 C316 H316 122.1 . . ? C311 C317 H31A 109.5 . . ? C311 C317 H31B 109.5 . . ? H31A C317 H31B 109.5 . . ? C311 C317 H31C 109.5 . . ? H31A C317 H31C 109.5 . . ? H31B C317 H31C 109.5 . . ?