# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Pierre Thuery' _publ_contact_author_email thuery@drecam.cea.fr _publ_author_name P.Thuery data_1 _database_code_depnum_ccdc_archive 'CCDC 877725' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H45 N2 O18.50 S4 U' _chemical_formula_weight 1168.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7485(10) _cell_length_b 11.7636(12) _cell_length_c 16.8054(18) _cell_angle_alpha 73.176(5) _cell_angle_beta 89.985(7) _cell_angle_gamma 89.854(7) _cell_volume 2223.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 122894 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1158 _exptl_absorpt_coefficient_mu 3.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.390 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and twelve \w scans with 2\% steps (765 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 122894 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8425 _reflns_number_gt 7232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The solvent water molecule was given an occupancy factor of 0.5 in order to retain an acceptable displacement parameter. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to the phenolic O atoms were found on a Fourier-difference map, but not those of the water molecule; the C-bound H atoms were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom (1.5 for CH~3~). Some voids in the lattice likely indicate the presence of other, unresolved solvent molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+45.6804P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8425 _refine_ls_number_parameters 566 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.2207 _refine_ls_wR_factor_gt 0.2138 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.253 _refine_diff_density_min -2.408 _refine_diff_density_rms 0.209 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 U U 0.24916(5) 0.15778(4) 0.26547(3) 0.04184(19) Uani 1 1 d . . . S1 S -0.0139(3) 0.2290(3) 0.2830(3) 0.0625(13) Uani 1 1 d . . . S2 S -0.6512(3) 0.4265(5) 0.2959(2) 0.0620(12) Uani 1 1 d . . . S3 S -0.4629(4) 1.0439(4) 0.2725(4) 0.0695(14) Uani 1 1 d . . . S4 S 0.1713(2) 0.8673(2) 0.25581(19) 0.0307(6) Uani 1 1 d . . . O1 O 0.2265(13) 0.2503(10) 0.1638(8) 0.083(4) Uani 1 1 d . . . O2 O 0.2412(8) 0.0760(9) 0.3691(6) 0.049(2) Uani 1 1 d . . . O3 O 0.0298(12) 0.1353(11) 0.2568(9) 0.080(4) Uani 1 1 d U . . O4 O 0.0878(12) 0.2745(10) 0.3200(8) 0.073(3) Uani 1 1 d U . . O5 O -0.0993(11) 0.1957(13) 0.3526(9) 0.087(4) Uani 1 1 d . . . O6 O -0.1897(8) 0.5996(8) -0.0083(6) 0.046(2) Uani 1 1 d . . . H6 H -0.1429 0.6650 -0.0054 0.055 Uiso 1 1 d R . . O7 O -0.6558(12) 0.3083(12) 0.3060(8) 0.076(3) Uani 1 1 d U . . O8 O -0.7698(13) 0.4916(14) 0.2771(9) 0.093(4) Uani 1 1 d . . . O9 O -0.6129(11) 0.4564(9) 0.3657(6) 0.065(3) Uani 1 1 d . . . O10 O -0.4018(8) 0.6685(8) -0.0066(6) 0.045(2) Uani 1 1 d . . . H10 H -0.3393 0.6176 -0.0049 0.054 Uiso 1 1 d R . . O11 O -0.5745(10) 1.1182(12) 0.2355(9) 0.078(4) Uani 1 1 d . . . O12 O -0.4900(15) 0.9526(14) 0.3341(9) 0.097(5) Uani 1 1 d . . . O13 O -0.3810(8) 1.1284(10) 0.2820(7) 0.057(3) Uani 1 1 d . . . O14 O -0.3322(8) 0.8882(8) -0.0149(6) 0.045(2) Uani 1 1 d . . . H14 H -0.3522 0.8084 -0.0066 0.053 Uiso 1 1 d R . . O15 O 0.2149(7) 0.9909(7) 0.2218(6) 0.040(2) Uani 1 1 d . . . O16 O 0.1054(8) 0.8567(9) 0.3292(6) 0.049(2) Uani 1 1 d . . . O17 O 0.2600(7) 0.7830(8) 0.2651(6) 0.045(2) Uani 1 1 d . . . O18 O -0.1186(8) 0.8188(8) -0.0187(5) 0.040(2) Uani 1 1 d . . . H18 H -0.1822 0.8447 -0.0024 0.048 Uiso 1 1 d R . . O19 O -0.875(3) 0.565(3) 0.3860(19) 0.094(8) Uani 0.50 1 d PU . . N1 N 0.650(2) 0.2735(16) 0.4709(13) 0.115(9) Uani 1 1 d . . . N2 N -0.1661(19) -0.183(3) 0.4320(12) 0.118(9) Uani 1 1 d . . . C1 C -0.0409(10) 0.5291(11) 0.0924(9) 0.037(3) Uani 1 1 d . . . C2 C -0.0029(11) 0.4412(11) 0.1611(9) 0.042(3) Uani 1 1 d . . . H2 H 0.0703 0.4447 0.1813 0.050 Uiso 1 1 calc R . . C3 C -0.0739(11) 0.3478(10) 0.1999(10) 0.049(4) Uani 1 1 d . . . C4 C -0.1836(11) 0.3388(11) 0.1718(10) 0.045(3) Uani 1 1 d . . . H4 H -0.2299 0.2754 0.1987 0.054 Uiso 1 1 calc R . . C5 C -0.2227(10) 0.4261(11) 0.1032(9) 0.040(3) Uani 1 1 d . . . C6 C -0.1522(10) 0.5190(11) 0.0635(8) 0.037(3) Uani 1 1 d . . . C7 C -0.3423(10) 0.4197(11) 0.0712(9) 0.037(3) Uani 1 1 d . . . H7A H -0.3653 0.3371 0.0855 0.045 Uiso 1 1 calc R . . H7B H -0.3419 0.4504 0.0111 0.045 Uiso 1 1 calc R . . C8 C -0.4305(9) 0.4891(10) 0.1059(7) 0.028(2) Uani 1 1 d . . . C9 C -0.4894(10) 0.4281(11) 0.1770(8) 0.035(3) Uani 1 1 d . . . H9 H -0.4767 0.3477 0.2026 0.042 Uiso 1 1 calc R . . C10 C -0.5679(10) 0.4922(11) 0.2080(8) 0.038(3) Uani 1 1 d . . . C11 C -0.5878(10) 0.6146(11) 0.1715(9) 0.039(3) Uani 1 1 d . . . H11 H -0.6400 0.6549 0.1951 0.046 Uiso 1 1 calc R . . C12 C -0.5293(10) 0.6738(10) 0.1010(8) 0.035(3) Uani 1 1 d . . . C13 C -0.4533(9) 0.6088(10) 0.0675(8) 0.032(3) Uani 1 1 d . . . C14 C -0.5499(11) 0.8071(10) 0.0611(10) 0.047(4) Uani 1 1 d . . . H14A H -0.5425 0.8251 0.0013 0.056 Uiso 1 1 calc R . . H14B H -0.6270 0.8266 0.0732 0.056 Uiso 1 1 calc R . . C15 C -0.4668(10) 0.8837(10) 0.0925(10) 0.041(3) Uani 1 1 d . . . C16 C -0.4951(11) 0.9209(11) 0.1602(11) 0.052(4) Uani 1 1 d . . . H16 H -0.5647 0.8983 0.1862 0.062 Uiso 1 1 calc R . . C17 C -0.4221(11) 0.9917(12) 0.1910(11) 0.050(4) Uani 1 1 d . . . C18 C -0.3153(10) 1.0203(10) 0.1544(9) 0.037(3) Uani 1 1 d . . . H18A H -0.2644 1.0639 0.1761 0.045 Uiso 1 1 calc R . . C19 C -0.2854(10) 0.9844(10) 0.0870(8) 0.034(3) Uani 1 1 d . . . C20 C -0.3620(10) 0.9176(10) 0.0563(8) 0.035(3) Uani 1 1 d . . . C21 C -0.1674(10) 1.0169(10) 0.0473(8) 0.035(3) Uani 1 1 d . . . H21A H -0.1737 1.0294 -0.0121 0.042 Uiso 1 1 calc R . . H21B H -0.1433 1.0912 0.0560 0.042 Uiso 1 1 calc R . . C22 C -0.0776(9) 0.9242(10) 0.0814(7) 0.031(2) Uani 1 1 d . . . C23 C -0.0064(10) 0.9356(10) 0.1457(8) 0.032(3) Uani 1 1 d . . . H23 H -0.0153 0.9993 0.1676 0.038 Uiso 1 1 calc R . . C24 C 0.0772(9) 0.8509(10) 0.1764(7) 0.029(2) Uani 1 1 d . . . C25 C 0.0915(10) 0.7528(10) 0.1473(8) 0.032(3) Uani 1 1 d . . . H25 H 0.1470 0.6962 0.1702 0.039 Uiso 1 1 calc R . . C26 C 0.0222(10) 0.7400(10) 0.0837(8) 0.034(3) Uani 1 1 d . . . C27 C -0.0584(10) 0.8279(10) 0.0506(7) 0.032(2) Uani 1 1 d . . . C28 C 0.0386(11) 0.6316(11) 0.0509(8) 0.037(3) Uani 1 1 d . . . H28A H 0.0252 0.6555 -0.0086 0.045 Uiso 1 1 calc R . . H28B H 0.1168 0.6044 0.0603 0.045 Uiso 1 1 calc R . . C29 C 0.748(4) 0.191(3) 0.501(3) 0.28(4) Uani 1 1 d . . . H29A H 0.8113 0.2349 0.5126 0.425 Uiso 1 1 calc R . . H29B H 0.7686 0.1541 0.4592 0.425 Uiso 1 1 calc R . . H29C H 0.7261 0.1312 0.5510 0.425 Uiso 1 1 calc R . . C30 C 0.6726(16) 0.354(2) 0.3890(17) 0.105(9) Uani 1 1 d . . . H30A H 0.7486 0.3845 0.3874 0.158 Uiso 1 1 calc R . . H30B H 0.6192 0.4186 0.3774 0.158 Uiso 1 1 calc R . . H30C H 0.6650 0.3121 0.3481 0.158 Uiso 1 1 calc R . . C31 C 0.606(6) 0.334(3) 0.528(2) 0.34(5) Uani 1 1 d . . . H31A H 0.6079 0.2816 0.5838 0.517 Uiso 1 1 d R . . H31B H 0.5285 0.3575 0.5132 0.517 Uiso 1 1 d R . . H31C H 0.6504 0.4036 0.5256 0.517 Uiso 1 1 d R . . C32 C 0.555(2) 0.196(2) 0.4587(18) 0.115(9) Uani 1 1 d . . . H32A H 0.5830 0.1413 0.4307 0.173 Uiso 1 1 calc R . . H32B H 0.4962 0.2446 0.4258 0.173 Uiso 1 1 calc R . . H32C H 0.5243 0.1529 0.5118 0.173 Uiso 1 1 calc R . . C33 C -0.081(5) -0.287(3) 0.472(2) 0.21(2) Uani 1 1 d . . . H33A H -0.0166 -0.2814 0.4361 0.313 Uiso 1 1 calc R . . H33B H -0.1190 -0.3615 0.4784 0.313 Uiso 1 1 calc R . . H33C H -0.0571 -0.2817 0.5251 0.313 Uiso 1 1 calc R . . C34 C -0.104(3) -0.096(3) 0.451(3) 0.178(19) Uani 1 1 d . . . H34A H -0.0257 -0.1032 0.4379 0.267 Uiso 1 1 calc R . . H34B H -0.1116 -0.1036 0.5093 0.267 Uiso 1 1 calc R . . H34C H -0.1324 -0.0193 0.4194 0.267 Uiso 1 1 calc R . . C35 C -0.176(2) -0.175(6) 0.3449(16) 0.28(4) Uani 1 1 d . . . H35A H -0.2550 -0.1821 0.3314 0.418 Uiso 1 1 calc R . . H35B H -0.1337 -0.2387 0.3336 0.418 Uiso 1 1 calc R . . H35C H -0.1472 -0.1005 0.3117 0.418 Uiso 1 1 calc R . . C36 C -0.267(3) -0.219(6) 0.481(2) 0.31(4) Uani 1 1 d . . . H36A H -0.2480 -0.2371 0.5393 0.462 Uiso 1 1 calc R . . H36B H -0.2987 -0.2878 0.4703 0.462 Uiso 1 1 calc R . . H36C H -0.3220 -0.1554 0.4675 0.462 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.0679(4) 0.0265(2) 0.0307(3) -0.00767(18) -0.0053(2) -0.0068(2) S1 0.0273(17) 0.0248(15) 0.121(4) 0.0020(19) 0.0108(19) 0.0018(13) S2 0.0324(19) 0.106(3) 0.040(2) -0.009(2) -0.0026(15) -0.021(2) S3 0.056(2) 0.053(2) 0.116(4) -0.050(3) 0.044(3) -0.0181(19) S4 0.0310(15) 0.0284(13) 0.0337(16) -0.0105(12) -0.0042(12) -0.0015(11) O1 0.135(12) 0.052(7) 0.060(8) -0.010(6) -0.026(8) -0.010(7) O2 0.046(6) 0.057(6) 0.042(6) -0.009(5) 0.007(4) -0.023(5) O3 0.085(7) 0.077(7) 0.085(7) -0.035(6) -0.023(6) 0.018(6) O4 0.097(7) 0.061(6) 0.063(6) -0.024(5) -0.015(6) 0.002(5) O5 0.069(9) 0.102(10) 0.079(10) -0.007(8) 0.004(7) 0.014(7) O6 0.041(5) 0.052(5) 0.049(6) -0.025(5) 0.010(4) -0.018(4) O7 0.093(7) 0.083(7) 0.058(6) -0.032(5) 0.019(5) -0.027(6) O8 0.093(11) 0.102(11) 0.075(10) -0.014(8) 0.019(8) -0.031(8) O9 0.108(9) 0.048(6) 0.039(6) -0.015(5) 0.010(6) 0.021(6) O10 0.050(6) 0.044(5) 0.034(5) -0.001(4) -0.002(4) -0.011(4) O11 0.054(7) 0.083(8) 0.115(11) -0.055(8) -0.007(7) 0.006(6) O12 0.130(13) 0.101(11) 0.067(9) -0.035(8) 0.020(9) 0.030(10) O13 0.028(5) 0.080(7) 0.074(8) -0.042(6) 0.000(5) -0.016(5) O14 0.050(6) 0.045(5) 0.032(5) -0.002(4) -0.012(4) -0.010(4) O15 0.042(5) 0.033(4) 0.047(6) -0.015(4) -0.004(4) -0.007(4) O16 0.038(5) 0.075(7) 0.037(5) -0.021(5) 0.005(4) -0.018(5) O17 0.035(5) 0.041(5) 0.065(7) -0.025(5) -0.009(4) 0.011(4) O18 0.040(5) 0.051(5) 0.030(5) -0.016(4) -0.002(4) -0.011(4) O19 0.120(12) 0.084(11) 0.083(11) -0.031(9) 0.024(9) 0.005(9) N1 0.19(2) 0.070(11) 0.087(14) -0.029(10) -0.082(15) 0.046(13) N2 0.101(15) 0.20(3) 0.053(11) -0.040(14) 0.022(10) -0.070(17) C1 0.030(6) 0.034(6) 0.055(8) -0.025(6) 0.009(6) -0.009(5) C2 0.027(6) 0.035(6) 0.071(10) -0.028(7) 0.012(6) 0.000(5) C3 0.038(7) 0.023(6) 0.092(12) -0.029(7) 0.023(7) 0.003(5) C4 0.030(7) 0.028(6) 0.083(11) -0.023(7) 0.018(6) -0.011(5) C5 0.026(6) 0.038(7) 0.067(10) -0.032(7) 0.004(6) -0.002(5) C6 0.034(7) 0.037(6) 0.047(8) -0.024(6) 0.005(5) -0.002(5) C7 0.025(6) 0.035(6) 0.059(9) -0.026(6) 0.008(5) -0.007(5) C8 0.024(6) 0.028(5) 0.034(6) -0.015(5) -0.004(5) -0.003(4) C9 0.038(7) 0.031(6) 0.041(7) -0.017(5) 0.006(5) 0.003(5) C10 0.029(6) 0.044(7) 0.038(7) -0.009(6) -0.001(5) -0.019(5) C11 0.024(6) 0.041(7) 0.058(9) -0.025(6) 0.000(5) 0.001(5) C12 0.026(6) 0.027(6) 0.052(8) -0.013(5) -0.005(5) -0.003(5) C13 0.021(6) 0.033(6) 0.040(7) -0.010(5) -0.004(5) -0.004(5) C14 0.033(7) 0.027(6) 0.079(11) -0.014(6) -0.016(7) 0.003(5) C15 0.026(6) 0.027(6) 0.069(10) -0.009(6) -0.003(6) 0.000(5) C16 0.023(6) 0.036(7) 0.101(13) -0.026(8) 0.006(7) -0.007(5) C17 0.034(7) 0.035(7) 0.093(12) -0.037(8) 0.017(7) -0.011(5) C18 0.025(6) 0.031(6) 0.058(9) -0.015(6) 0.006(5) -0.008(5) C19 0.035(7) 0.021(5) 0.040(7) -0.001(5) 0.000(5) 0.001(5) C20 0.035(7) 0.021(5) 0.045(8) -0.003(5) -0.012(5) 0.004(5) C21 0.030(6) 0.028(6) 0.043(7) -0.004(5) -0.003(5) -0.008(5) C22 0.026(6) 0.031(6) 0.033(7) -0.003(5) 0.006(5) -0.008(5) C23 0.029(6) 0.031(6) 0.037(7) -0.011(5) 0.005(5) -0.011(5) C24 0.025(6) 0.033(6) 0.034(6) -0.017(5) 0.002(5) -0.009(5) C25 0.024(6) 0.028(6) 0.044(7) -0.010(5) -0.002(5) -0.003(4) C26 0.029(6) 0.030(6) 0.048(8) -0.018(5) 0.008(5) -0.010(5) C27 0.030(6) 0.034(6) 0.032(6) -0.011(5) 0.006(5) -0.011(5) C28 0.034(7) 0.039(6) 0.044(8) -0.019(6) 0.009(5) -0.009(5) C29 0.26(5) 0.11(2) 0.41(7) 0.03(3) -0.28(5) 0.02(3) C30 0.041(10) 0.111(17) 0.14(2) 0.008(16) -0.002(12) 0.004(11) C31 0.83(14) 0.11(3) 0.12(3) -0.08(2) -0.21(6) 0.14(5) C32 0.11(2) 0.093(17) 0.13(2) -0.012(16) 0.056(17) 0.019(15) C33 0.37(7) 0.14(3) 0.11(3) -0.04(2) 0.09(4) -0.12(4) C34 0.19(3) 0.11(2) 0.26(4) -0.08(3) 0.16(3) -0.07(2) C35 0.063(16) 0.72(11) 0.050(16) -0.11(3) 0.002(12) 0.01(3) C36 0.13(3) 0.72(12) 0.14(3) -0.23(5) 0.10(2) -0.24(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O2 1.731(10) . ? U O1 1.760(12) . ? U O11 2.212(12) 1_645 ? U O15 2.322(8) 1_545 ? U O7 2.357(12) 1_655 ? U O3 2.600(14) . ? U O4 2.652(13) . ? S1 O3 1.396(13) . ? S1 O5 1.506(15) . ? S1 O4 1.516(13) . ? S1 C3 1.807(16) . ? S2 O7 1.352(13) . ? S2 O9 1.393(12) . ? S2 O8 1.575(17) . ? S2 C10 1.755(13) . ? S3 O12 1.298(16) . ? S3 O13 1.427(10) . ? S3 O11 1.596(13) . ? S3 C17 1.723(15) . ? S4 O17 1.413(9) . ? S4 O16 1.430(10) . ? S4 O15 1.492(9) . ? S4 C24 1.785(11) . ? O6 C6 1.373(16) . ? O6 H6 0.9587 . ? O7 U 2.357(12) 1_455 ? O10 C13 1.381(15) . ? O10 H10 0.9414 . ? O11 U 2.212(12) 1_465 ? O14 C20 1.382(16) . ? O14 H14 0.9391 . ? O15 U 2.322(8) 1_565 ? O18 C27 1.393(14) . ? O18 H18 0.8791 . ? N1 C31 1.45(4) . ? N1 C30 1.45(3) . ? N1 C29 1.49(3) . ? N1 C32 1.49(3) . ? N2 C34 1.37(3) . ? N2 C36 1.44(3) . ? N2 C35 1.45(3) . ? N2 C33 1.57(5) . ? C1 C2 1.38(2) . ? C1 C6 1.412(17) . ? C1 C28 1.527(16) . ? C2 C3 1.385(18) . ? C2 H2 0.9300 . ? C3 C4 1.387(19) . ? C4 C5 1.38(2) . ? C4 H4 0.9300 . ? C5 C6 1.381(18) . ? C5 C7 1.514(17) . ? C7 C8 1.533(16) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.388(17) . ? C8 C13 1.394(16) . ? C9 C10 1.383(18) . ? C9 H9 0.9300 . ? C10 C11 1.411(18) . ? C11 C12 1.374(19) . ? C11 H11 0.9300 . ? C12 C13 1.394(17) . ? C12 C14 1.534(16) . ? C14 C15 1.524(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.37(2) . ? C15 C20 1.380(18) . ? C16 C17 1.396(18) . ? C16 H16 0.9300 . ? C17 C18 1.395(18) . ? C18 C19 1.365(18) . ? C18 H18A 0.9300 . ? C19 C20 1.391(16) . ? C19 C21 1.538(17) . ? C21 C22 1.504(16) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.393(16) . ? C22 C23 1.404(16) . ? C23 C24 1.386(17) . ? C23 H23 0.9300 . ? C24 C25 1.389(16) . ? C25 C26 1.386(17) . ? C25 H25 0.9300 . ? C26 C27 1.393(17) . ? C26 C28 1.540(16) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U O1 167.4(6) . . ? O2 U O11 100.8(5) . 1_645 ? O1 U O11 91.8(7) . 1_645 ? O2 U O15 92.0(4) . 1_545 ? O1 U O15 90.5(4) . 1_545 ? O11 U O15 80.7(4) 1_645 1_545 ? O2 U O7 88.9(4) . 1_655 ? O1 U O7 92.7(5) . 1_655 ? O11 U O7 81.1(4) 1_645 1_655 ? O15 U O7 161.7(4) 1_545 1_655 ? O2 U O3 88.0(4) . . ? O1 U O3 80.9(6) . . ? O11 U O3 152.1(4) 1_645 . ? O15 U O3 72.5(4) 1_545 . ? O7 U O3 125.8(4) 1_655 . ? O2 U O4 78.8(4) . . ? O1 U O4 89.6(6) . . ? O11 U O4 155.6(4) 1_645 . ? O15 U O4 123.6(3) 1_545 . ? O7 U O4 74.5(4) 1_655 . ? O3 U O4 51.9(4) . . ? O3 S1 O5 115.9(9) . . ? O3 S1 O4 104.2(7) . . ? O5 S1 O4 104.5(8) . . ? O3 S1 C3 113.8(8) . . ? O5 S1 C3 108.1(7) . . ? O4 S1 C3 109.8(6) . . ? O7 S2 O9 114.1(8) . . ? O7 S2 O8 114.2(8) . . ? O9 S2 O8 103.2(8) . . ? O7 S2 C10 108.4(7) . . ? O9 S2 C10 111.8(7) . . ? O8 S2 C10 104.7(7) . . ? O12 S3 O13 121.4(10) . . ? O12 S3 O11 109.9(9) . . ? O13 S3 O11 106.1(7) . . ? O12 S3 C17 107.5(8) . . ? O13 S3 C17 108.7(6) . . ? O11 S3 C17 101.4(8) . . ? O17 S4 O16 114.8(6) . . ? O17 S4 O15 111.2(6) . . ? O16 S4 O15 110.5(6) . . ? O17 S4 C24 108.3(5) . . ? O16 S4 C24 107.9(5) . . ? O15 S4 C24 103.4(5) . . ? S1 O3 U 104.0(7) . . ? S1 O4 U 98.2(6) . . ? C6 O6 H6 97.6 . . ? S2 O7 U 144.6(9) . 1_455 ? C13 O10 H10 99.3 . . ? S3 O11 U 143.7(9) . 1_465 ? C20 O14 H14 107.3 . . ? S4 O15 U 139.3(6) . 1_565 ? C27 O18 H18 93.1 . . ? C31 N1 C30 113(2) . . ? C31 N1 C29 116(3) . . ? C30 N1 C29 111(3) . . ? C31 N1 C32 105(3) . . ? C30 N1 C32 105.3(18) . . ? C29 N1 C32 105(2) . . ? C34 N2 C36 115(3) . . ? C34 N2 C35 117(3) . . ? C36 N2 C35 116(2) . . ? C34 N2 C33 96(3) . . ? C36 N2 C33 102(3) . . ? C35 N2 C33 107(3) . . ? C2 C1 C6 117.9(11) . . ? C2 C1 C28 119.1(11) . . ? C6 C1 C28 123.0(12) . . ? C1 C2 C3 119.9(13) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 122.0(14) . . ? C2 C3 S1 117.4(11) . . ? C4 C3 S1 120.4(10) . . ? C5 C4 C3 118.7(12) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C6 C5 C4 119.8(12) . . ? C6 C5 C7 120.1(13) . . ? C4 C5 C7 120.1(12) . . ? O6 C6 C5 118.7(11) . . ? O6 C6 C1 119.5(11) . . ? C5 C6 C1 121.7(13) . . ? C5 C7 C8 113.9(10) . . ? C5 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C5 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C13 120.4(11) . . ? C9 C8 C7 117.7(10) . . ? C13 C8 C7 122.0(11) . . ? C10 C9 C8 117.0(11) . . ? C10 C9 H9 121.5 . . ? C8 C9 H9 121.5 . . ? C9 C10 C11 123.0(12) . . ? C9 C10 S2 122.2(10) . . ? C11 C10 S2 114.8(10) . . ? C12 C11 C10 119.4(11) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 117.9(11) . . ? C11 C12 C14 119.8(12) . . ? C13 C12 C14 122.3(12) . . ? O10 C13 C8 121.1(11) . . ? O10 C13 C12 116.7(11) . . ? C8 C13 C12 122.2(12) . . ? C15 C14 C12 112.4(10) . . ? C15 C14 H14A 109.1 . . ? C12 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C12 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C20 117.4(12) . . ? C16 C15 C14 119.6(12) . . ? C20 C15 C14 123.0(14) . . ? C15 C16 C17 121.8(13) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 118.9(14) . . ? C18 C17 S3 120.2(10) . . ? C16 C17 S3 120.8(11) . . ? C19 C18 C17 120.3(12) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C20 119.0(12) . . ? C18 C19 C21 119.6(11) . . ? C20 C19 C21 121.4(12) . . ? C15 C20 O14 119.6(11) . . ? C15 C20 C19 122.5(13) . . ? O14 C20 C19 117.8(12) . . ? C22 C21 C19 113.8(10) . . ? C22 C21 H21A 108.8 . . ? C19 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? C19 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C27 C22 C23 117.4(11) . . ? C27 C22 C21 123.2(11) . . ? C23 C22 C21 119.4(11) . . ? C24 C23 C22 119.4(10) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 122.3(10) . . ? C23 C24 S4 119.7(8) . . ? C25 C24 S4 118.1(9) . . ? C26 C25 C24 119.3(11) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 118.2(10) . . ? C25 C26 C28 119.3(11) . . ? C27 C26 C28 122.5(11) . . ? C26 C27 O18 116.8(10) . . ? C26 C27 C22 123.4(11) . . ? O18 C27 C22 119.8(11) . . ? C1 C28 C26 112.8(10) . . ? C1 C28 H28A 109.0 . . ? C26 C28 H28A 109.0 . . ? C1 C28 H28B 109.0 . . ? C26 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? N1 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 H31A 109.4 . . ? N1 C31 H31B 108.6 . . ? H31A C31 H31B 109.5 . . ? N1 C31 H31C 110.4 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N1 C32 H32A 109.5 . . ? N1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 H35A 109.5 . . ? N2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N2 C36 H36A 109.5 . . ? N2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 O18 0.96 1.78 2.669(12) 152.6 . O18 H18 O14 0.88 1.83 2.643(13) 153.1 . O14 H14 O10 0.94 1.75 2.678(13) 170.6 . O10 H10 O6 0.94 1.77 2.621(14) 148.3 . #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 877726' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H100 Ce2 O64 S8 U' _chemical_formula_weight 2572.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6416(11) _cell_length_b 32.870(3) _cell_length_c 12.0455(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.578(6) _cell_angle_gamma 90.00 _cell_volume 4609.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 96766 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 3.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.566 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and seven \w scans with 2\% steps (530 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 96766 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.68 _reflns_number_total 17345 _reflns_number_gt 14821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Four solvent water molecules were given 0.5 occupancy factors in order to retain acceptable displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some badly behaving atoms. The H atoms bound to the phenolic O atoms were found on a Fourier-difference map, but not those of the water molecules. The C-bound H atoms were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+72.9212P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.238(7) _chemical_absolute_configuration unk _refine_ls_number_reflns 17345 _refine_ls_number_parameters 1199 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1803 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.502 _refine_diff_density_min -2.237 _refine_diff_density_rms 0.182 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 U U 0.46208(4) 0.427060(17) 0.55794(4) 0.03146(14) Uani 1 1 d . . . Ce1 Ce 0.54023(7) 0.28190(3) 0.17099(7) 0.0336(2) Uani 1 1 d . . . Ce2 Ce 1.07202(7) 0.24272(3) 0.78229(7) 0.0325(2) Uani 1 1 d . . . S1 S 0.2137(3) 0.41435(12) 0.6490(3) 0.0354(9) Uani 1 1 d . . . S2 S 0.3827(3) 0.43053(14) 1.2704(3) 0.0335(8) Uani 1 1 d . . . S3 S -0.2479(3) 0.42607(14) 1.4440(3) 0.0340(7) Uani 1 1 d . . . S4 S -0.4132(5) 0.40302(18) 0.8330(4) 0.0639(16) Uani 1 1 d . . . S5 S 0.7095(3) 0.19956(12) 0.0219(3) 0.0317(8) Uani 1 1 d . . . S6 S 0.8173(3) 0.22631(13) 0.5819(3) 0.0357(9) Uani 1 1 d . . . S7 S 0.2932(3) 0.16433(12) 0.8819(3) 0.0325(8) Uani 1 1 d . . . S8 S 0.1254(3) 0.19065(12) 0.2872(3) 0.0326(8) Uani 1 1 d . . . O1 O 0.4476(10) 0.4764(4) 0.6084(10) 0.051(3) Uani 1 1 d . . . O2 O 0.4703(9) 0.3780(4) 0.5084(10) 0.046(3) Uani 1 1 d U . . O3 O 0.3248(9) 0.4024(4) 0.7010(9) 0.042(3) Uani 1 1 d . . . O4 O 0.2476(8) 0.4293(4) 0.5370(8) 0.035(2) Uani 1 1 d . . . O5 O 0.1256(9) 0.3837(3) 0.6485(10) 0.042(3) Uani 1 1 d . . . O6 O 0.0408(9) 0.5571(3) 0.8857(9) 0.037(2) Uani 1 1 d . . . H6 H 0.0460 0.5557 0.9578 0.045 Uiso 1 1 d R . . O7 O 0.4224(9) 0.4484(3) 1.3737(9) 0.038(2) Uani 1 1 d . . . O8 O 0.4750(8) 0.4236(4) 1.1946(8) 0.039(2) Uani 1 1 d . . . O9 O 0.3158(10) 0.3944(3) 1.2896(9) 0.041(3) Uani 1 1 d . . . O10 O 0.1039(9) 0.5652(3) 1.0999(9) 0.042(3) Uani 1 1 d . . . H10 H 0.0338 0.5673 1.1256 0.050 Uiso 1 1 d R . . O11 O -0.3520(8) 0.4429(4) 1.4985(10) 0.041(3) Uani 1 1 d . . . O12 O -0.1559(8) 0.4202(4) 1.5225(9) 0.042(3) Uani 1 1 d . . . O13 O -0.2768(10) 0.3901(4) 1.3783(10) 0.045(3) Uani 1 1 d . . . O14 O -0.1153(9) 0.5610(3) 1.1539(9) 0.039(3) Uani 1 1 d . . . H14 H -0.1371 0.5614 1.0838 0.047 Uiso 1 1 d R . . O15 O -0.4315(9) 0.4057(4) 0.7086(9) 0.044(3) Uani 1 1 d . . . O16 O -0.3466(16) 0.3689(5) 0.8623(15) 0.084(5) Uani 1 1 d U . . O17 O -0.5261(14) 0.4075(5) 0.8936(14) 0.081(5) Uani 1 1 d U . . O18 O -0.1782(9) 0.5560(3) 0.9412(8) 0.037(2) Uani 1 1 d . . . H18 H -0.1118 0.5521 0.9017 0.044 Uiso 1 1 d R . . O19 O 0.6131(8) 0.2279(3) 0.0408(9) 0.035(2) Uani 1 1 d . . . O20 O 0.7077(9) 0.1852(3) -0.0906(8) 0.037(2) Uani 1 1 d . . . O21 O 0.8181(8) 0.2165(3) 0.0568(9) 0.034(2) Uani 1 1 d . . . O22 O 0.6108(9) 0.0574(4) 0.3026(9) 0.041(3) Uani 1 1 d . . . H22 H 0.6583 0.0529 0.3594 0.049 Uiso 1 1 d R . . O23 O 0.9345(8) 0.2299(3) 0.6194(9) 0.037(2) Uani 1 1 d . . . O24 O 0.7369(8) 0.2409(4) 0.6643(9) 0.042(3) Uani 1 1 d . . . O25 O 0.8028(10) 0.2447(4) 0.4727(9) 0.043(3) Uani 1 1 d . . . O26 O 0.7168(9) 0.0523(3) 0.5049(9) 0.037(2) Uani 1 1 d . . . H26 H 0.6460 0.0472 0.5345 0.044 Uiso 1 1 d R . . O27 O 0.1903(9) 0.1814(3) 0.8340(8) 0.037(3) Uani 1 1 d . . . O28 O 0.2652(10) 0.1369(4) 0.9743(9) 0.042(3) Uani 1 1 d . . . O29 O 0.3768(9) 0.1946(4) 0.9089(8) 0.038(3) Uani 1 1 d . . . O30 O 0.4946(9) 0.0476(3) 0.5716(9) 0.038(2) Uani 1 1 d . . . H30 H 0.4588 0.0457 0.5075 0.045 Uiso 1 1 d R . . O31 O 0.2051(9) 0.2218(3) 0.2485(9) 0.042(3) Uani 1 1 d . . . O32 O 0.0729(9) 0.2016(4) 0.3913(9) 0.042(3) Uani 1 1 d . . . O33 O 0.0424(10) 0.1797(4) 0.2036(10) 0.047(3) Uani 1 1 d . . . O34 O 0.3964(10) 0.0413(3) 0.3682(10) 0.043(3) Uani 1 1 d . . . H34 H 0.4592 0.0409 0.3314 0.052 Uiso 1 1 d R . . O35 O 0.3808(8) 0.2363(4) 0.1041(9) 0.043(3) Uani 1 1 d . . . O36 O 0.5287(11) 0.3012(4) -0.0332(10) 0.050(3) Uani 1 1 d . . . O37 O 0.7552(9) 0.2876(4) 0.1628(11) 0.050(3) Uani 1 1 d . . . O38 O 0.6276(9) 0.2285(4) 0.3000(9) 0.045(3) Uani 1 1 d . . . O39 O 0.3993(10) 0.2639(3) 0.3266(9) 0.039(3) Uani 1 1 d . . . O40 O 0.3600(8) 0.3275(3) 0.1495(8) 0.035(2) Uani 1 1 d . . . O41 O 0.5962(9) 0.3546(4) 0.1394(11) 0.048(3) Uani 1 1 d . . . O42 O 0.5829(10) 0.3191(4) 0.3481(10) 0.046(3) Uani 1 1 d . . . O43 O 1.2799(9) 0.2641(4) 0.7980(10) 0.041(3) Uani 1 1 d . . . O44 O 1.0933(9) 0.3124(4) 0.8722(10) 0.042(3) Uani 1 1 d . . . O45 O 1.0728(11) 0.2375(5) 0.9919(10) 0.058(3) Uani 1 1 d . . . O46 O 0.9479(9) 0.1817(4) 0.8346(9) 0.039(3) Uani 1 1 d . . . O47 O 1.1668(10) 0.2131(4) 0.6096(9) 0.051(3) Uani 1 1 d . . . O48 O 1.0840(13) 0.3000(4) 0.6387(10) 0.061(4) Uani 1 1 d . . . O49 O 0.8813(9) 0.2708(4) 0.8404(12) 0.055(3) Uani 1 1 d . . . O50 O 0.0549(11) 0.3911(5) 0.3969(12) 0.062(4) Uani 1 1 d . . . O51 O 0.380(2) 0.3011(8) 0.625(2) 0.055(6) Uani 0.50 1 d PU . . O52 O 0.622(2) 0.3101(8) 0.588(2) 0.050(6) Uani 0.50 1 d PU . . O53 O 0.2744(11) 0.3251(4) 0.4344(11) 0.054(3) Uani 1 1 d . . . O54 O 0.2818(11) 0.3616(4) 0.9357(11) 0.059(4) Uani 1 1 d . . . O55 O -0.0312(10) 0.6325(3) 0.9956(9) 0.042(3) Uani 1 1 d . . . O56 O -0.176(2) 0.3532(8) 1.679(2) 0.127(8) Uani 1 1 d . . . O57 O -0.1442(11) 0.3167(5) 1.3617(14) 0.073(4) Uani 1 1 d . . . O58 O -0.075(2) 0.3698(8) 0.874(2) 0.055(6) Uani 0.50 1 d PU . . O59 O -0.193(2) 0.3829(9) 1.088(2) 0.054(6) Uani 0.50 1 d PU . . O60 O 0.5379(9) 0.2398(4) 0.7910(9) 0.045(3) Uani 1 1 d . . . O61 O 0.1396(10) 0.2984(4) 0.1511(10) 0.046(3) Uani 1 1 d . . . O62 O 0.0620(11) 0.2884(4) 0.4118(11) 0.056(3) Uani 1 1 d . . . O63 O 0.5062(12) 0.1696(5) 0.4115(12) 0.066(4) Uani 1 1 d . . . O64 O 0.4047(10) 0.2139(4) 0.5861(11) 0.054(3) Uani 1 1 d . . . O65 O 0.0213(12) 0.3703(5) 0.1766(10) 0.066(4) Uani 1 1 d . . . O66 O 0.1064(16) 0.4142(5) -0.0014(14) 0.084(5) Uani 1 1 d . . . C1 C 0.0078(13) 0.5024(5) 0.7599(13) 0.037(4) Uani 1 1 d . . . C2 C 0.0513(12) 0.4688(4) 0.7050(12) 0.030(3) Uani 1 1 d . . . H2 H 0.0051 0.4548 0.6544 0.036 Uiso 1 1 calc R . . C3 C 0.1601(13) 0.4562(5) 0.7241(12) 0.033(3) Uani 1 1 d . . . C4 C 0.2333(11) 0.4751(5) 0.8020(11) 0.030(3) Uani 1 1 d . . . H4 H 0.3078 0.4656 0.8138 0.036 Uiso 1 1 calc R . . C5 C 0.1909(12) 0.5088(5) 0.8617(12) 0.031(3) Uani 1 1 d . . . C6 C 0.0778(12) 0.5219(4) 0.8378(11) 0.025(3) Uani 1 1 d . . . C7 C 0.2623(12) 0.5290(5) 0.9473(13) 0.033(3) Uani 1 1 d . . . H7A H 0.2463 0.5580 0.9454 0.040 Uiso 1 1 calc R . . H7B H 0.3425 0.5253 0.9288 0.040 Uiso 1 1 calc R . . C8 C 0.2439(12) 0.5139(5) 1.0630(13) 0.035(3) Uani 1 1 d . . . C9 C 0.3115(13) 0.4824(5) 1.1076(12) 0.031(3) Uani 1 1 d . . . H9 H 0.3696 0.4711 1.0651 0.038 Uiso 1 1 calc R . . C10 C 0.2929(11) 0.4681(5) 1.2133(12) 0.029(3) Uani 1 1 d . . . C11 C 0.2091(11) 0.4851(4) 1.2804(12) 0.027(3) Uani 1 1 d . . . H11 H 0.1974 0.4752 1.3517 0.033 Uiso 1 1 calc R . . C12 C 0.1429(13) 0.5172(5) 1.2396(11) 0.031(3) Uani 1 1 d . . . C13 C 0.1614(12) 0.5315(5) 1.1353(11) 0.029(3) Uani 1 1 d . . . C14 C 0.0509(11) 0.5346(4) 1.3139(11) 0.028(3) Uani 1 1 d . . . H14A H 0.0428 0.5634 1.2984 0.033 Uiso 1 1 calc R . . H14B H 0.0756 0.5317 1.3907 0.033 Uiso 1 1 calc R . . C15 C -0.0653(12) 0.5142(5) 1.2993(14) 0.036(4) Uani 1 1 d . . . C16 C -0.0966(12) 0.4827(5) 1.3649(12) 0.031(3) Uani 1 1 d U . . H16 H -0.0453 0.4727 1.4179 0.038 Uiso 1 1 calc R . . C17 C -0.2050(12) 0.4652(4) 1.3537(12) 0.030(3) Uani 1 1 d . . . C18 C -0.2807(13) 0.4768(4) 1.2686(12) 0.030(3) Uani 1 1 d . . . H18A H -0.3506 0.4635 1.2592 0.036 Uiso 1 1 calc R . . C19 C -0.2504(13) 0.5089(5) 1.1972(14) 0.036(4) Uani 1 1 d . . . C20 C -0.1428(12) 0.5282(5) 1.2159(12) 0.030(3) Uani 1 1 d . . . C21 C -0.3305(13) 0.5221(5) 1.1065(13) 0.038(4) Uani 1 1 d . . . H21A H -0.3261 0.5514 1.0988 0.046 Uiso 1 1 calc R . . H21B H -0.4085 0.5152 1.1271 0.046 Uiso 1 1 calc R . . C22 C -0.3037(13) 0.5021(6) 0.9930(13) 0.043(4) Uani 1 1 d . . . C23 C -0.3604(12) 0.4657(5) 0.9670(14) 0.038(4) Uani 1 1 d . . . H23 H -0.4122 0.4541 1.0160 0.045 Uiso 1 1 calc R . . C24 C -0.3369(13) 0.4475(6) 0.8661(13) 0.043(4) Uani 1 1 d . . . C25 C -0.2574(13) 0.4639(5) 0.7906(13) 0.035(3) Uani 1 1 d . . . H25 H -0.2441 0.4510 0.7232 0.042 Uiso 1 1 calc R . . C26 C -0.2005(12) 0.4986(5) 0.8176(12) 0.031(3) Uani 1 1 d . . . C27 C -0.2278(13) 0.5188(5) 0.9199(14) 0.039(4) Uani 1 1 d . . . C28 C -0.1161(13) 0.5159(5) 0.7368(13) 0.036(3) Uani 1 1 d . . . H28A H -0.1198 0.5454 0.7399 0.043 Uiso 1 1 calc R . . H28B H -0.1381 0.5076 0.6623 0.043 Uiso 1 1 calc R . . C29 C 0.5480(13) 0.1047(5) 0.1672(12) 0.034(3) Uani 1 1 d . . . C30 C 0.5760(13) 0.1385(5) 0.0999(12) 0.033(3) Uani 1 1 d . . . H30A H 0.5219 0.1487 0.0499 0.039 Uiso 1 1 calc R . . C31 C 0.6833(13) 0.1563(5) 0.1078(13) 0.037(4) Uani 1 1 d . . . C32 C 0.7644(11) 0.1426(5) 0.1807(11) 0.030(3) Uani 1 1 d . . . H32 H 0.8354 0.1556 0.1855 0.036 Uiso 1 1 calc R . . C33 C 0.7418(11) 0.1099(5) 0.2471(12) 0.029(3) Uani 1 1 d . . . C34 C 0.6364(13) 0.0912(5) 0.2393(14) 0.038(4) Uani 1 1 d . . . C35 C 0.8342(13) 0.0971(5) 0.3373(13) 0.037(3) Uani 1 1 d . . . H35A H 0.8382 0.0677 0.3420 0.044 Uiso 1 1 calc R . . H35B H 0.9092 0.1072 0.3164 0.044 Uiso 1 1 calc R . . C36 C 0.8018(11) 0.1142(5) 0.4470(12) 0.031(3) Uani 1 1 d . . . C37 C 0.8276(13) 0.1544(6) 0.4630(15) 0.045(4) Uani 1 1 d . . . H37 H 0.8683 0.1692 0.4105 0.054 Uiso 1 1 calc R . . C38 C 0.7889(12) 0.1732(5) 0.5650(12) 0.032(3) Uani 1 1 d . . . C39 C 0.7338(12) 0.1522(5) 0.6469(12) 0.036(4) Uani 1 1 d . . . H39 H 0.7138 0.1651 0.7127 0.043 Uiso 1 1 calc R . . C40 C 0.7083(11) 0.1112(5) 0.6299(12) 0.031(3) Uani 1 1 d . . . C41 C 0.7413(12) 0.0931(5) 0.5263(11) 0.029(3) Uani 1 1 d . . . C42 C 0.6497(13) 0.0868(5) 0.7200(12) 0.037(4) Uani 1 1 d . . . H42A H 0.6804 0.0944 0.7922 0.044 Uiso 1 1 calc R . . H42B H 0.6638 0.0580 0.7089 0.044 Uiso 1 1 calc R . . C43 C 0.5186(13) 0.0955(5) 0.7148(11) 0.031(3) Uani 1 1 d . . . C44 C 0.4721(13) 0.1248(5) 0.7870(11) 0.032(3) Uani 1 1 d . . . H44 H 0.5191 0.1382 0.8381 0.039 Uiso 1 1 calc R . . C45 C 0.3549(13) 0.1336(5) 0.7811(13) 0.035(3) Uani 1 1 d . . . C46 C 0.2824(12) 0.1145(5) 0.7015(12) 0.033(3) Uani 1 1 d . . . H46 H 0.2046 0.1209 0.6977 0.040 Uiso 1 1 calc R . . C47 C 0.3286(12) 0.0864(5) 0.6299(12) 0.032(3) Uani 1 1 d . . . C48 C 0.4472(11) 0.0774(5) 0.6375(11) 0.031(3) Uani 1 1 d . . . C49 C 0.2516(11) 0.0681(5) 0.5408(11) 0.027(3) Uani 1 1 d . . . H49A H 0.1725 0.0693 0.5649 0.032 Uiso 1 1 calc R . . H49B H 0.2717 0.0397 0.5308 0.032 Uiso 1 1 calc R . . C50 C 0.2623(13) 0.0905(5) 0.4290(13) 0.035(3) Uani 1 1 d . . . C51 C 0.1960(14) 0.1256(5) 0.4124(13) 0.034(3) Uani 1 1 d . . . H51 H 0.1444 0.1345 0.4656 0.041 Uiso 1 1 calc R . . C52 C 0.2104(11) 0.1469(5) 0.3125(13) 0.032(3) Uani 1 1 d . . . C53 C 0.2864(13) 0.1341(5) 0.2353(12) 0.035(4) Uani 1 1 d . . . H53 H 0.2958 0.1492 0.1707 0.042 Uiso 1 1 calc R . . C54 C 0.3504(11) 0.0990(5) 0.2510(11) 0.029(3) Uani 1 1 d . . . C55 C 0.3380(13) 0.0771(5) 0.3473(14) 0.038(4) Uani 1 1 d . . . C56 C 0.4351(13) 0.0849(5) 0.1594(11) 0.032(3) Uani 1 1 d . . . H56A H 0.4454 0.0556 0.1650 0.038 Uiso 1 1 calc R . . H56B H 0.4014 0.0906 0.0871 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.0252(2) 0.0399(3) 0.0293(3) -0.0009(3) 0.00117(19) -0.0007(2) Ce1 0.0266(4) 0.0403(5) 0.0338(5) -0.0020(4) -0.0004(3) 0.0005(3) Ce2 0.0244(4) 0.0416(5) 0.0314(4) -0.0006(4) 0.0003(3) -0.0009(3) S1 0.0271(17) 0.041(2) 0.039(2) -0.0021(15) 0.0051(15) -0.0017(14) S2 0.0282(16) 0.041(2) 0.0315(17) 0.0014(18) -0.0021(13) 0.0024(17) S3 0.0260(15) 0.039(2) 0.0368(18) 0.004(2) -0.0009(13) -0.0010(18) S4 0.079(4) 0.075(4) 0.038(3) 0.017(2) -0.024(2) -0.042(3) S5 0.0229(17) 0.042(2) 0.0307(19) -0.0010(16) 0.0026(14) -0.0009(15) S6 0.0283(18) 0.042(2) 0.036(2) 0.0009(17) -0.0050(16) -0.0025(16) S7 0.0240(17) 0.046(2) 0.0270(19) -0.0021(16) 0.0005(14) 0.0003(15) S8 0.0254(17) 0.037(2) 0.035(2) 0.0006(16) -0.0003(14) 0.0028(14) O1 0.033(6) 0.071(9) 0.050(7) 0.027(6) 0.000(5) 0.009(6) O2 0.025(5) 0.063(7) 0.049(6) 0.025(5) -0.013(4) 0.003(4) O3 0.036(6) 0.052(7) 0.038(6) -0.004(5) 0.014(5) -0.001(5) O4 0.036(5) 0.042(6) 0.027(5) 0.000(5) 0.002(4) 0.002(5) O5 0.037(6) 0.030(6) 0.061(8) -0.002(5) 0.008(5) -0.004(5) O6 0.039(6) 0.035(6) 0.038(6) -0.003(5) -0.005(5) 0.006(5) O7 0.036(6) 0.044(6) 0.033(6) 0.007(5) 0.000(5) 0.001(5) O8 0.031(5) 0.041(6) 0.046(6) 0.004(6) 0.003(4) 0.009(5) O9 0.046(6) 0.038(6) 0.038(6) -0.001(5) -0.008(5) 0.000(5) O10 0.035(6) 0.044(7) 0.045(7) 0.007(5) -0.005(5) 0.010(5) O11 0.019(5) 0.057(7) 0.047(7) 0.003(5) 0.008(5) -0.004(4) O12 0.029(5) 0.049(8) 0.049(6) 0.008(6) 0.001(5) -0.008(5) O13 0.043(6) 0.045(7) 0.046(7) -0.009(5) 0.027(5) -0.009(5) O14 0.032(6) 0.044(7) 0.040(6) 0.005(5) -0.001(5) -0.003(5) O15 0.027(5) 0.068(8) 0.037(6) -0.001(5) -0.006(5) -0.012(5) O16 0.093(8) 0.072(8) 0.086(8) 0.007(7) -0.026(7) -0.013(7) O17 0.065(7) 0.102(8) 0.078(8) 0.000(7) 0.005(6) -0.037(7) O18 0.029(5) 0.050(7) 0.030(6) -0.002(5) 0.001(4) -0.003(5) O19 0.017(5) 0.045(7) 0.044(6) 0.000(5) -0.001(4) 0.006(4) O20 0.028(5) 0.052(7) 0.031(6) 0.002(5) -0.001(4) 0.006(5) O21 0.013(4) 0.045(7) 0.044(6) -0.001(5) -0.005(4) 0.003(4) O22 0.032(6) 0.054(7) 0.036(6) 0.000(5) -0.003(5) -0.001(5) O23 0.024(5) 0.037(6) 0.051(7) -0.004(5) 0.000(5) -0.005(4) O24 0.023(5) 0.049(7) 0.053(7) 0.002(6) 0.001(5) 0.004(5) O25 0.053(7) 0.040(6) 0.035(6) 0.003(5) 0.003(5) -0.001(6) O26 0.035(6) 0.036(6) 0.038(6) 0.006(5) -0.004(5) 0.009(5) O27 0.031(5) 0.051(7) 0.030(6) -0.001(5) -0.011(4) 0.012(5) O28 0.039(6) 0.060(8) 0.026(6) -0.007(5) 0.002(5) 0.003(5) O29 0.035(6) 0.055(7) 0.024(5) -0.007(5) 0.005(4) -0.003(5) O30 0.042(6) 0.041(6) 0.030(6) -0.003(5) -0.004(5) 0.006(5) O31 0.039(6) 0.043(7) 0.043(6) 0.014(5) 0.012(5) 0.006(5) O32 0.034(6) 0.049(7) 0.042(6) -0.002(5) 0.014(5) 0.003(5) O33 0.043(7) 0.049(7) 0.047(7) -0.008(6) -0.004(5) 0.009(5) O34 0.043(6) 0.036(6) 0.051(7) 0.002(5) 0.008(5) 0.003(5) O35 0.025(5) 0.062(8) 0.043(6) -0.012(6) 0.006(4) -0.004(5) O36 0.067(8) 0.039(7) 0.043(7) 0.002(5) -0.005(6) -0.001(6) O37 0.036(6) 0.051(8) 0.064(8) -0.017(6) 0.013(6) -0.007(5) O38 0.036(6) 0.059(8) 0.039(6) -0.008(5) -0.007(5) -0.007(5) O39 0.042(6) 0.049(7) 0.028(6) -0.002(5) 0.002(5) 0.001(5) O40 0.028(5) 0.046(7) 0.032(6) -0.004(5) 0.002(4) 0.005(4) O41 0.032(6) 0.045(7) 0.066(8) -0.014(6) -0.006(6) 0.002(5) O42 0.046(7) 0.050(7) 0.042(7) -0.013(5) 0.006(5) -0.003(5) O43 0.024(5) 0.056(7) 0.044(7) 0.002(5) -0.005(5) -0.003(5) O44 0.033(6) 0.051(7) 0.043(7) -0.011(5) -0.003(5) 0.009(5) O45 0.050(7) 0.083(10) 0.041(7) 0.004(7) 0.014(6) 0.009(7) O46 0.026(5) 0.063(8) 0.028(6) 0.002(5) 0.000(4) -0.004(5) O47 0.045(7) 0.081(9) 0.027(6) -0.008(6) -0.005(5) 0.009(6) O48 0.087(10) 0.061(9) 0.034(7) 0.011(6) -0.014(7) -0.011(7) O49 0.019(5) 0.070(9) 0.077(9) -0.021(7) 0.007(5) 0.000(5) O50 0.041(7) 0.078(10) 0.067(9) -0.006(7) -0.010(6) 0.010(6) O51 0.037(9) 0.071(10) 0.057(10) 0.038(8) -0.008(8) -0.016(8) O52 0.050(9) 0.049(10) 0.052(10) 0.012(8) 0.002(8) 0.003(8) O53 0.047(7) 0.056(8) 0.059(8) 0.001(6) 0.021(6) 0.008(6) O54 0.042(7) 0.080(10) 0.054(8) 0.017(7) 0.002(6) -0.006(6) O55 0.047(7) 0.037(6) 0.042(6) 0.006(5) 0.002(5) 0.006(5) O56 0.098(16) 0.124(18) 0.16(2) -0.016(16) -0.017(15) -0.001(13) O57 0.032(7) 0.092(12) 0.094(12) 0.005(9) -0.011(7) 0.000(7) O58 0.052(9) 0.048(10) 0.065(10) -0.008(8) -0.009(8) 0.014(8) O59 0.039(9) 0.075(10) 0.048(9) 0.007(8) 0.011(8) -0.003(8) O60 0.031(6) 0.059(8) 0.045(6) 0.008(6) -0.008(5) -0.001(5) O61 0.039(6) 0.056(8) 0.042(7) 0.012(6) -0.005(5) -0.006(5) O62 0.047(7) 0.058(9) 0.064(8) 0.001(7) 0.008(6) -0.001(6) O63 0.056(8) 0.074(10) 0.068(9) -0.008(7) 0.005(7) -0.017(7) O64 0.040(7) 0.071(9) 0.053(8) -0.003(6) 0.007(6) -0.003(6) O65 0.060(8) 0.106(12) 0.032(7) 0.001(7) 0.008(6) -0.006(8) O66 0.094(12) 0.082(13) 0.076(11) -0.006(8) 0.001(9) 0.002(9) C1 0.034(8) 0.044(10) 0.033(8) 0.006(7) -0.010(7) -0.003(7) C2 0.030(7) 0.028(8) 0.031(8) 0.005(6) 0.004(6) -0.010(6) C3 0.032(8) 0.041(9) 0.027(8) 0.002(6) 0.012(6) -0.007(6) C4 0.018(6) 0.058(10) 0.014(6) 0.006(6) -0.004(5) 0.000(6) C5 0.021(7) 0.045(9) 0.026(8) 0.004(6) -0.011(6) -0.004(6) C6 0.029(7) 0.032(8) 0.014(6) 0.008(6) -0.003(5) -0.002(6) C7 0.028(7) 0.033(9) 0.038(8) 0.005(6) -0.009(6) -0.007(6) C8 0.027(7) 0.043(9) 0.035(8) 0.010(7) 0.000(6) -0.004(6) C9 0.033(8) 0.038(9) 0.023(7) 0.000(6) -0.007(6) 0.004(6) C10 0.014(6) 0.042(9) 0.032(8) 0.002(6) -0.005(5) -0.003(6) C11 0.018(6) 0.040(9) 0.024(7) 0.004(6) -0.005(5) -0.006(6) C12 0.031(7) 0.043(9) 0.019(7) 0.000(6) 0.000(6) 0.000(6) C13 0.029(7) 0.041(9) 0.017(7) -0.001(6) -0.003(5) 0.002(6) C14 0.027(7) 0.034(8) 0.022(7) 0.011(6) -0.002(5) 0.005(6) C15 0.017(6) 0.042(9) 0.049(10) -0.016(7) 0.002(6) -0.008(6) C16 0.024(6) 0.041(7) 0.029(6) 0.004(5) -0.015(5) 0.002(5) C17 0.029(7) 0.028(8) 0.035(8) -0.001(6) 0.013(6) -0.006(6) C18 0.034(7) 0.027(8) 0.029(8) -0.005(6) 0.007(6) -0.003(6) C19 0.026(7) 0.050(10) 0.033(8) 0.002(7) 0.006(6) 0.004(6) C20 0.029(7) 0.035(9) 0.028(8) -0.008(6) 0.009(6) -0.002(6) C21 0.029(8) 0.052(10) 0.033(8) -0.011(7) 0.007(6) 0.004(7) C22 0.028(8) 0.070(12) 0.031(9) 0.010(8) 0.004(6) -0.005(7) C23 0.020(7) 0.046(10) 0.047(10) 0.006(8) -0.008(6) -0.008(6) C24 0.030(8) 0.068(12) 0.029(8) -0.012(7) 0.003(6) -0.024(7) C25 0.032(8) 0.039(9) 0.034(8) 0.005(7) 0.002(6) 0.001(7) C26 0.025(7) 0.045(9) 0.022(7) 0.003(6) 0.006(6) 0.011(6) C27 0.027(7) 0.036(9) 0.054(10) 0.022(8) 0.008(7) 0.002(6) C28 0.036(8) 0.041(9) 0.031(8) 0.008(7) -0.001(6) -0.008(7) C29 0.032(8) 0.042(9) 0.030(8) 0.004(7) 0.003(6) 0.009(7) C30 0.033(8) 0.037(9) 0.029(8) -0.002(6) 0.000(6) 0.007(6) C31 0.031(8) 0.054(11) 0.025(8) 0.005(7) 0.002(6) -0.008(7) C32 0.019(6) 0.057(10) 0.014(6) -0.004(6) -0.002(5) 0.002(6) C33 0.010(6) 0.047(10) 0.031(8) -0.002(7) 0.004(5) 0.000(6) C34 0.037(8) 0.026(8) 0.050(10) 0.001(7) 0.008(7) 0.002(6) C35 0.030(8) 0.044(9) 0.035(8) 0.008(7) 0.001(6) 0.002(7) C36 0.017(6) 0.044(10) 0.032(8) -0.001(6) -0.005(6) 0.010(6) C37 0.028(8) 0.055(12) 0.051(10) 0.021(8) 0.005(7) 0.008(7) C38 0.023(7) 0.048(10) 0.026(8) -0.005(6) -0.006(6) 0.000(6) C39 0.026(7) 0.059(11) 0.024(8) 0.005(7) 0.000(6) 0.001(7) C40 0.017(6) 0.044(10) 0.033(8) 0.002(7) -0.007(6) 0.008(6) C41 0.032(7) 0.036(9) 0.018(7) 0.001(6) -0.013(6) 0.006(6) C42 0.040(9) 0.047(10) 0.023(8) 0.003(7) -0.003(6) -0.009(7) C43 0.039(8) 0.035(8) 0.018(7) 0.010(6) -0.010(6) -0.004(6) C44 0.042(8) 0.044(9) 0.011(6) 0.002(6) -0.005(6) -0.010(7) C45 0.032(8) 0.041(9) 0.032(8) 0.010(7) -0.009(6) -0.001(6) C46 0.022(7) 0.053(10) 0.024(7) 0.014(7) -0.008(6) 0.001(6) C47 0.027(8) 0.036(9) 0.033(8) 0.005(6) 0.005(6) -0.001(6) C48 0.021(7) 0.050(10) 0.022(7) 0.004(6) 0.001(5) 0.005(6) C49 0.015(6) 0.045(9) 0.021(7) -0.003(6) -0.003(5) 0.006(6) C50 0.039(8) 0.029(8) 0.035(8) -0.007(6) -0.003(7) -0.003(6) C51 0.038(8) 0.032(9) 0.033(8) -0.006(7) -0.001(7) -0.002(7) C52 0.016(6) 0.047(9) 0.034(8) 0.004(7) 0.006(6) 0.006(6) C53 0.042(9) 0.046(10) 0.018(7) 0.000(6) 0.011(6) 0.002(7) C54 0.017(6) 0.046(9) 0.024(7) 0.000(6) 0.000(5) 0.004(6) C55 0.032(8) 0.036(9) 0.045(9) -0.011(7) -0.018(7) 0.000(6) C56 0.041(8) 0.038(9) 0.017(7) -0.003(6) -0.004(6) 0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O2 1.723(13) . ? U O1 1.741(14) . ? U O15 2.297(11) 1_655 ? U O11 2.345(10) 1_654 ? U O7 2.369(10) 1_554 ? U O3 2.498(11) . ? U O4 2.508(9) . ? Ce1 O42 2.504(11) . ? Ce1 O41 2.508(12) . ? Ce1 O35 2.512(11) . ? Ce1 O37 2.513(11) . ? Ce1 O19 2.521(11) . ? Ce1 O36 2.542(12) . ? Ce1 O38 2.551(12) . ? Ce1 O39 2.573(11) . ? Ce1 O40 2.589(10) . ? Ce2 O49 2.511(11) . ? Ce2 O27 2.515(10) 1_655 ? Ce2 O43 2.525(10) . ? Ce2 O45 2.531(12) . ? Ce2 O44 2.545(11) . ? Ce2 O23 2.555(10) . ? Ce2 O46 2.556(11) . ? Ce2 O47 2.557(11) . ? Ce2 O48 2.562(12) . ? S1 O5 1.437(11) . ? S1 O3 1.484(12) . ? S1 O4 1.494(10) . ? S1 C3 1.763(16) . ? S2 O8 1.435(10) . ? S2 O9 1.441(12) . ? S2 O7 1.448(12) . ? S2 C10 1.754(15) . ? S3 O12 1.434(11) . ? S3 O13 1.459(12) . ? S3 O11 1.490(11) . ? S3 C17 1.761(15) . ? S4 O16 1.405(18) . ? S4 O15 1.514(12) . ? S4 O17 1.517(17) . ? S4 C24 1.755(16) . ? S5 O20 1.435(11) . ? S5 O21 1.441(10) . ? S5 O19 1.477(10) . ? S5 C31 1.785(16) . ? S6 O23 1.437(10) . ? S6 O24 1.454(11) . ? S6 O25 1.456(12) . ? S6 C38 1.789(17) . ? S7 O29 1.426(12) . ? S7 O27 1.439(10) . ? S7 O28 1.470(12) . ? S7 C45 1.740(17) . ? S8 O33 1.435(12) . ? S8 O32 1.445(11) . ? S8 O31 1.461(11) . ? S8 C52 1.771(15) . ? O6 C6 1.365(18) . ? O6 H6 0.8709 . ? O7 U 2.369(10) 1_556 ? O10 C13 1.362(18) . ? O10 H10 0.8776 . ? O11 U 2.345(10) 1_456 ? O14 C20 1.351(19) . ? O14 H14 0.8788 . ? O15 U 2.297(11) 1_455 ? O18 C27 1.38(2) . ? O18 H18 0.9204 . ? O22 C34 1.38(2) . ? O22 H22 0.8878 . ? O26 C41 1.395(18) . ? O26 H26 0.9171 . ? O27 Ce2 2.515(10) 1_455 ? O30 C48 1.379(18) . ? O30 H30 0.8770 . ? O34 C55 1.38(2) . ? O34 H34 0.8589 . ? C1 C2 1.39(2) . ? C1 C6 1.39(2) . ? C1 C28 1.53(2) . ? C2 C3 1.35(2) . ? C2 H2 0.9300 . ? C3 C4 1.41(2) . ? C4 C5 1.41(2) . ? C4 H4 0.9300 . ? C5 C6 1.412(19) . ? C5 C7 1.48(2) . ? C7 C8 1.50(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.40(2) . ? C8 C13 1.43(2) . ? C9 C10 1.38(2) . ? C9 H9 0.9300 . ? C10 C11 1.39(2) . ? C11 C12 1.39(2) . ? C11 H11 0.9300 . ? C12 C13 1.36(2) . ? C12 C14 1.515(19) . ? C14 C15 1.518(19) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.36(2) . ? C15 C20 1.42(2) . ? C16 C17 1.39(2) . ? C16 H16 0.9300 . ? C17 C18 1.40(2) . ? C18 C19 1.41(2) . ? C18 H18A 0.9300 . ? C19 C20 1.42(2) . ? C19 C21 1.49(2) . ? C21 C22 1.55(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.37(2) . ? C22 C23 1.40(2) . ? C23 C24 1.38(2) . ? C23 H23 0.9300 . ? C24 C25 1.41(2) . ? C25 C26 1.36(2) . ? C25 H25 0.9300 . ? C26 C27 1.44(2) . ? C26 C28 1.50(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.41(2) . ? C29 C30 1.42(2) . ? C29 C56 1.47(2) . ? C30 C31 1.38(2) . ? C30 H30A 0.9300 . ? C31 C32 1.36(2) . ? C32 C33 1.37(2) . ? C32 H32 0.9300 . ? C33 C34 1.37(2) . ? C33 C35 1.58(2) . ? C35 C36 1.49(2) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.37(2) . ? C36 C41 1.38(2) . ? C37 C38 1.45(2) . ? C37 H37 0.9300 . ? C38 C39 1.37(2) . ? C39 C40 1.40(2) . ? C39 H39 0.9300 . ? C40 C41 1.44(2) . ? C40 C42 1.52(2) . ? C42 C43 1.55(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C48 1.38(2) . ? C43 C44 1.41(2) . ? C44 C45 1.40(2) . ? C44 H44 0.9300 . ? C45 C46 1.42(2) . ? C46 C47 1.38(2) . ? C46 H46 0.9300 . ? C47 C48 1.415(19) . ? C47 C49 1.51(2) . ? C49 C50 1.54(2) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C55 1.40(2) . ? C50 C51 1.40(2) . ? C51 C52 1.40(2) . ? C51 H51 0.9300 . ? C52 C53 1.36(2) . ? C53 C54 1.39(2) . ? C53 H53 0.9300 . ? C54 C55 1.37(2) . ? C54 C56 1.558(19) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U O1 177.6(5) . . ? O2 U O15 87.4(5) . 1_655 ? O1 U O15 93.6(5) . 1_655 ? O2 U O11 92.7(5) . 1_654 ? O1 U O11 89.6(5) . 1_654 ? O15 U O11 79.5(4) 1_655 1_654 ? O2 U O7 88.0(5) . 1_554 ? O1 U O7 91.8(5) . 1_554 ? O15 U O7 158.3(4) 1_655 1_554 ? O11 U O7 79.6(4) 1_654 1_554 ? O2 U O3 88.4(5) . . ? O1 U O3 89.8(5) . . ? O15 U O3 72.5(4) 1_655 . ? O11 U O3 151.9(4) 1_654 . ? O7 U O3 128.5(4) 1_554 . ? O2 U O4 93.0(4) . . ? O1 U O4 84.7(5) . . ? O15 U O4 128.1(4) 1_655 . ? O11 U O4 152.1(4) 1_654 . ? O7 U O4 73.3(3) 1_554 . ? O3 U O4 55.6(4) . . ? O42 Ce1 O41 67.3(4) . . ? O42 Ce1 O35 134.7(4) . . ? O41 Ce1 O35 135.4(4) . . ? O42 Ce1 O37 78.9(4) . . ? O41 Ce1 O37 70.3(4) . . ? O35 Ce1 O37 139.9(4) . . ? O42 Ce1 O19 143.9(4) . . ? O41 Ce1 O19 119.2(4) . . ? O35 Ce1 O19 68.5(3) . . ? O37 Ce1 O19 71.7(3) . . ? O42 Ce1 O36 135.3(4) . . ? O41 Ce1 O36 68.1(4) . . ? O35 Ce1 O36 78.8(4) . . ? O37 Ce1 O36 89.2(4) . . ? O19 Ce1 O36 65.7(4) . . ? O42 Ce1 O38 75.1(4) . . ? O41 Ce1 O38 130.3(4) . . ? O35 Ce1 O38 94.2(4) . . ? O37 Ce1 O38 71.6(4) . . ? O19 Ce1 O38 76.1(4) . . ? O36 Ce1 O38 141.1(4) . . ? O42 Ce1 O39 67.3(4) . . ? O41 Ce1 O39 119.9(4) . . ? O35 Ce1 O39 67.8(3) . . ? O37 Ce1 O39 133.5(4) . . ? O19 Ce1 O39 120.8(3) . . ? O36 Ce1 O39 137.3(4) . . ? O38 Ce1 O39 69.6(4) . . ? O42 Ce1 O40 87.5(4) . . ? O41 Ce1 O40 69.2(3) . . ? O35 Ce1 O40 73.6(4) . . ? O37 Ce1 O40 139.4(4) . . ? O19 Ce1 O40 128.5(3) . . ? O36 Ce1 O40 74.0(4) . . ? O38 Ce1 O40 141.0(4) . . ? O39 Ce1 O40 71.6(3) . . ? O49 Ce2 O27 135.2(4) . 1_655 ? O49 Ce2 O43 136.5(4) . . ? O27 Ce2 O43 71.5(4) 1_655 . ? O49 Ce2 O45 75.0(4) . . ? O27 Ce2 O45 72.7(4) 1_655 . ? O43 Ce2 O45 87.2(4) . . ? O49 Ce2 O44 68.4(4) . . ? O27 Ce2 O44 124.4(3) 1_655 . ? O43 Ce2 O44 68.2(4) . . ? O45 Ce2 O44 68.8(4) . . ? O49 Ce2 O23 74.1(4) . . ? O27 Ce2 O23 113.3(3) 1_655 . ? O43 Ce2 O23 134.1(4) . . ? O45 Ce2 O23 138.6(4) . . ? O44 Ce2 O23 122.2(3) . . ? O49 Ce2 O46 73.5(4) . . ? O27 Ce2 O46 67.6(4) 1_655 . ? O43 Ce2 O46 138.1(4) . . ? O45 Ce2 O46 72.3(4) . . ? O44 Ce2 O46 130.9(4) . . ? O23 Ce2 O46 73.0(3) . . ? O49 Ce2 O47 139.2(4) . . ? O27 Ce2 O47 69.9(4) 1_655 . ? O43 Ce2 O47 75.3(4) . . ? O45 Ce2 O47 142.0(4) . . ? O44 Ce2 O47 130.4(4) . . ? O23 Ce2 O47 65.4(3) . . ? O46 Ce2 O47 98.7(4) . . ? O49 Ce2 O48 88.4(5) . . ? O27 Ce2 O48 136.3(4) 1_655 . ? O43 Ce2 O48 77.7(4) . . ? O45 Ce2 O48 136.4(5) . . ? O44 Ce2 O48 67.6(4) . . ? O23 Ce2 O48 69.0(4) . . ? O46 Ce2 O48 141.1(4) . . ? O47 Ce2 O48 72.8(5) . . ? O5 S1 O3 115.8(7) . . ? O5 S1 O4 115.0(7) . . ? O3 S1 O4 103.4(6) . . ? O5 S1 C3 107.0(7) . . ? O3 S1 C3 107.6(7) . . ? O4 S1 C3 107.7(7) . . ? O8 S2 O9 112.4(7) . . ? O8 S2 O7 112.1(7) . . ? O9 S2 O7 111.4(7) . . ? O8 S2 C10 108.0(7) . . ? O9 S2 C10 108.8(7) . . ? O7 S2 C10 103.6(7) . . ? O12 S3 O13 114.6(8) . . ? O12 S3 O11 111.4(7) . . ? O13 S3 O11 110.8(6) . . ? O12 S3 C17 106.9(7) . . ? O13 S3 C17 108.8(7) . . ? O11 S3 C17 103.8(7) . . ? O16 S4 O15 111.5(10) . . ? O16 S4 O17 115.7(11) . . ? O15 S4 O17 110.9(8) . . ? O16 S4 C24 109.3(10) . . ? O15 S4 C24 104.1(8) . . ? O17 S4 C24 104.5(9) . . ? O20 S5 O21 114.0(6) . . ? O20 S5 O19 110.4(6) . . ? O21 S5 O19 112.2(6) . . ? O20 S5 C31 106.6(7) . . ? O21 S5 C31 107.0(7) . . ? O19 S5 C31 106.1(7) . . ? O23 S6 O24 112.0(7) . . ? O23 S6 O25 110.6(7) . . ? O24 S6 O25 114.2(7) . . ? O23 S6 C38 106.8(7) . . ? O24 S6 C38 106.3(7) . . ? O25 S6 C38 106.5(7) . . ? O29 S7 O27 112.5(7) . . ? O29 S7 O28 114.2(7) . . ? O27 S7 O28 110.6(7) . . ? O29 S7 C45 106.2(7) . . ? O27 S7 C45 107.1(7) . . ? O28 S7 C45 105.6(7) . . ? O33 S8 O32 112.5(7) . . ? O33 S8 O31 112.2(7) . . ? O32 S8 O31 112.3(7) . . ? O33 S8 C52 106.7(7) . . ? O32 S8 C52 107.0(7) . . ? O31 S8 C52 105.6(7) . . ? S1 O3 U 100.6(6) . . ? S1 O4 U 99.9(5) . . ? C6 O6 H6 111.0 . . ? S2 O7 U 137.9(7) . 1_556 ? C13 O10 H10 114.1 . . ? S3 O11 U 144.1(7) . 1_456 ? C20 O14 H14 118.4 . . ? S4 O15 U 150.3(8) . 1_455 ? C27 O18 H18 97.7 . . ? S5 O19 Ce1 143.2(6) . . ? C34 O22 H22 115.1 . . ? S6 O23 Ce2 147.2(7) . . ? C41 O26 H26 106.6 . . ? S7 O27 Ce2 149.8(7) . 1_455 ? C48 O30 H30 111.6 . . ? C55 O34 H34 109.8 . . ? C2 C1 C6 118.3(14) . . ? C2 C1 C28 119.5(14) . . ? C6 C1 C28 122.2(15) . . ? C3 C2 C1 120.6(15) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 122.7(15) . . ? C2 C3 S1 119.2(12) . . ? C4 C3 S1 118.1(12) . . ? C3 C4 C5 118.3(13) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C6 C5 C4 117.7(13) . . ? C6 C5 C7 121.4(14) . . ? C4 C5 C7 120.8(13) . . ? O6 C6 C1 119.3(13) . . ? O6 C6 C5 118.1(13) . . ? C1 C6 C5 122.4(14) . . ? C5 C7 C8 114.6(13) . . ? C5 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C5 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C13 116.4(13) . . ? C9 C8 C7 121.1(14) . . ? C13 C8 C7 122.5(14) . . ? C10 C9 C8 120.9(14) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 121.2(14) . . ? C9 C10 S2 120.3(11) . . ? C11 C10 S2 118.3(11) . . ? C10 C11 C12 119.3(13) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.7(14) . . ? C13 C12 C14 122.3(13) . . ? C11 C12 C14 118.0(12) . . ? C12 C13 O10 119.3(13) . . ? C12 C13 C8 122.5(14) . . ? O10 C13 C8 118.1(13) . . ? C12 C14 C15 113.5(13) . . ? C12 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? C12 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C20 119.2(13) . . ? C16 C15 C14 120.9(14) . . ? C20 C15 C14 119.9(14) . . ? C15 C16 C17 120.5(13) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 121.5(13) . . ? C16 C17 S3 120.3(12) . . ? C18 C17 S3 118.2(11) . . ? C17 C18 C19 119.5(14) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C18 C19 C20 117.6(14) . . ? C18 C19 C21 120.3(14) . . ? C20 C19 C21 122.0(15) . . ? O14 C20 C15 119.8(13) . . ? O14 C20 C19 118.8(14) . . ? C15 C20 C19 121.4(14) . . ? C19 C21 C22 113.1(13) . . ? C19 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C19 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C27 C22 C23 120.4(17) . . ? C27 C22 C21 122.3(17) . . ? C23 C22 C21 117.4(14) . . ? C24 C23 C22 117.9(15) . . ? C24 C23 H23 121.1 . . ? C22 C23 H23 121.1 . . ? C23 C24 C25 122.5(15) . . ? C23 C24 S4 117.1(12) . . ? C25 C24 S4 120.4(12) . . ? C26 C25 C24 119.2(15) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 118.8(13) . . ? C25 C26 C28 119.0(13) . . ? C27 C26 C28 122.1(14) . . ? C22 C27 O18 120.7(16) . . ? C22 C27 C26 121.1(16) . . ? O18 C27 C26 118.3(13) . . ? C26 C28 C1 113.1(13) . . ? C26 C28 H28A 109.0 . . ? C1 C28 H28A 109.0 . . ? C26 C28 H28B 109.0 . . ? C1 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C34 C29 C30 115.3(14) . . ? C34 C29 C56 123.2(14) . . ? C30 C29 C56 121.5(13) . . ? C31 C30 C29 120.5(14) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C32 C31 C30 121.6(15) . . ? C32 C31 S5 121.1(12) . . ? C30 C31 S5 117.2(12) . . ? C31 C32 C33 120.1(14) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C34 119.2(14) . . ? C32 C33 C35 118.6(12) . . ? C34 C33 C35 122.0(14) . . ? C33 C34 O22 121.2(15) . . ? C33 C34 C29 123.2(15) . . ? O22 C34 C29 115.6(14) . . ? C36 C35 C33 109.5(12) . . ? C36 C35 H35A 109.8 . . ? C33 C35 H35A 109.8 . . ? C36 C35 H35B 109.8 . . ? C33 C35 H35B 109.8 . . ? H35A C35 H35B 108.2 . . ? C37 C36 C41 120.1(14) . . ? C37 C36 C35 115.7(14) . . ? C41 C36 C35 124.0(15) . . ? C36 C37 C38 117.4(15) . . ? C36 C37 H37 121.3 . . ? C38 C37 H37 121.3 . . ? C39 C38 C37 123.3(16) . . ? C39 C38 S6 119.8(12) . . ? C37 C38 S6 116.9(12) . . ? C38 C39 C40 118.8(15) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? C39 C40 C41 117.9(14) . . ? C39 C40 C42 120.2(13) . . ? C41 C40 C42 121.8(14) . . ? C36 C41 O26 117.4(13) . . ? C36 C41 C40 122.4(14) . . ? O26 C41 C40 120.2(13) . . ? C40 C42 C43 108.8(12) . . ? C40 C42 H42A 109.9 . . ? C43 C42 H42A 109.9 . . ? C40 C42 H42B 109.9 . . ? C43 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? C48 C43 C44 118.6(14) . . ? C48 C43 C42 122.3(14) . . ? C44 C43 C42 119.0(13) . . ? C45 C44 C43 119.4(14) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 121.2(15) . . ? C44 C45 S7 119.6(12) . . ? C46 C45 S7 118.8(12) . . ? C47 C46 C45 119.2(13) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C48 119.1(14) . . ? C46 C47 C49 118.6(12) . . ? C48 C47 C49 122.2(13) . . ? C43 C48 O30 116.9(12) . . ? C43 C48 C47 122.5(14) . . ? O30 C48 C47 120.5(13) . . ? C47 C49 C50 112.2(12) . . ? C47 C49 H49A 109.2 . . ? C50 C49 H49A 109.2 . . ? C47 C49 H49B 109.2 . . ? C50 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? C55 C50 C51 120.5(15) . . ? C55 C50 C49 121.6(14) . . ? C51 C50 C49 117.9(13) . . ? C50 C51 C52 117.6(14) . . ? C50 C51 H51 121.2 . . ? C52 C51 H51 121.2 . . ? C53 C52 C51 121.2(14) . . ? C53 C52 S8 120.0(12) . . ? C51 C52 S8 118.8(11) . . ? C52 C53 C54 121.1(14) . . ? C52 C53 H53 119.4 . . ? C54 C53 H53 119.4 . . ? C55 C54 C53 119.4(13) . . ? C55 C54 C56 121.0(13) . . ? C53 C54 C56 119.6(13) . . ? C54 C55 O34 123.0(15) . . ? C54 C55 C50 120.2(15) . . ? O34 C55 C50 116.8(15) . . ? C29 C56 C54 113.3(12) . . ? C29 C56 H56A 108.9 . . ? C54 C56 H56A 108.9 . . ? C29 C56 H56B 108.9 . . ? C54 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 O10 0.87 1.86 2.689(15) 158.3 . O10 H10 O14 0.88 1.79 2.643(15) 165.3 . O14 H14 O18 0.88 1.79 2.662(15) 173.4 . O18 H18 O6 0.92 1.80 2.642(15) 151.6 . O22 H22 O26 0.89 1.87 2.725(16) 160.2 . O26 H26 O30 0.92 1.82 2.721(15) 165.8 . O30 H30 O34 0.88 1.83 2.701(16) 175.0 . O34 H34 O22 0.86 1.88 2.679(16) 153.6 . #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 877727' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H97 Eu2 O62.50 S8 U' _chemical_formula_weight 2568.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9431(2) _cell_length_b 19.8987(4) _cell_length_c 20.4792(4) _cell_angle_alpha 71.2552(9) _cell_angle_beta 78.0759(10) _cell_angle_gamma 77.8533(8) _cell_volume 4454.53(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 232308 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 28.70 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2558 _exptl_absorpt_coefficient_mu 3.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.505 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and twelve \w scans with 1\% steps (1780 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 232308 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 28.70 _reflns_number_total 22979 _reflns_number_gt 18960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Two sulfonate groups (S3, S4) were found to be rotationally disordered over two positions which were given occupancy parameters constrained to sum to unity. Three water molecules bound to Eu1 are also disordered over two positions which were given occupancy parameters constrained to sum to unity, while two water molecules bound to Eu2 (O45A, O50) are disordered with a third one (O45B), all having been given occupancy parameters of 0.5, and the coordination number of Eu2 is 9 or 8, respectively. Several solvent water molecules are also disordered over two positions. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths, angles and/or displacement parameters for some badly behaving atoms, particularly in the disordered parts and the solvent molecules. The H atoms bound to the phenolic O atoms and those of three coordinated water molecules were found on a Fourier-difference map, but not those of the other water molecules. The C-bound H atoms were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+28.5423P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22979 _refine_ls_number_parameters 1312 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.225 _refine_diff_density_min -4.493 _refine_diff_density_rms 0.198 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 U U 1.138534(18) 0.272687(12) 0.981142(12) 0.02151(7) Uani 1 1 d . . . Eu1 Eu 0.87804(5) 0.11716(2) 1.36009(2) 0.04754(12) Uani 1 1 d . . . Eu2 Eu 0.55611(3) 0.64609(2) 0.82232(2) 0.03972(10) Uani 1 1 d . . . S1 S 1.04030(14) 0.40821(9) 0.87165(9) 0.0290(3) Uani 1 1 d . . . S2 S 0.43873(13) 0.30166(9) 0.94467(8) 0.0277(3) Uani 1 1 d . . . S3 S 0.25080(19) 0.59610(13) 0.6623(2) 0.1062(15) Uani 1 1 d DU . . S4 S 0.83781(16) 0.72371(9) 0.57691(9) 0.0323(4) Uani 1 1 d . . . S5 S 0.84370(13) 0.22756(9) 1.05927(8) 0.0259(3) Uani 1 1 d . . . S6 S 0.24219(14) 0.13639(8) 1.12805(9) 0.0266(3) Uani 1 1 d . . . S7 S 0.49656(18) -0.06725(12) 1.43724(14) 0.0559(6) Uani 1 1 d . . . S8 S 1.0761(2) -0.05800(11) 1.36129(10) 0.0426(5) Uani 1 1 d . . . O1 O 1.1339(5) 0.2250(3) 0.9230(3) 0.0360(11) Uani 1 1 d . . . O2 O 1.1407(4) 0.3203(2) 1.0397(2) 0.0284(9) Uani 1 1 d . . . O3 O 1.1641(4) 0.3780(3) 0.8745(3) 0.0320(10) Uani 1 1 d . . . O4 O 0.9773(4) 0.3674(3) 0.9381(3) 0.0310(10) Uani 1 1 d . . . O5 O 1.0171(5) 0.4849(3) 0.8582(3) 0.0407(12) Uani 1 1 d . . . O6 O 0.9135(5) 0.3311(3) 0.6463(3) 0.0359(11) Uani 1 1 d . . . H6 H 0.8498 0.3094 0.6598 0.043 Uiso 1 1 d R . . O7 O 0.3374(4) 0.2681(3) 0.9465(3) 0.0339(11) Uani 1 1 d . . . O8 O 0.4025(4) 0.3758(3) 0.9453(3) 0.0363(11) Uani 1 1 d . . . O9 O 0.5083(4) 0.2573(3) 0.9976(3) 0.0360(11) Uani 1 1 d . . . O10 O 0.7140(4) 0.2788(3) 0.6776(3) 0.0335(11) Uani 1 1 d . . . H10 H 0.6786 0.3081 0.6403 0.040 Uiso 1 1 d R . . O11A O 0.3037(8) 0.6412(5) 0.6937(7) 0.086(3) Uani 0.564(11) 1 d PDU A 1 O12A O 0.1903(8) 0.6414(5) 0.6120(5) 0.086(3) Uani 0.564(11) 1 d PDU A 1 O13A O 0.1818(8) 0.5543(5) 0.7236(5) 0.072(3) Uani 0.564(11) 1 d PDU A 1 O11B O 0.2781(10) 0.6665(4) 0.6422(9) 0.085(3) Uani 0.436(11) 1 d PDU A 2 O12B O 0.1690(8) 0.5997(7) 0.6115(7) 0.087(3) Uani 0.436(11) 1 d PDU A 2 O13B O 0.1957(11) 0.5678(7) 0.7296(5) 0.079(3) Uani 0.436(11) 1 d PDU A 2 O14 O 0.6338(5) 0.3950(3) 0.5688(3) 0.0404(12) Uani 1 1 d . A . H14 H 0.6946 0.4145 0.5444 0.048 Uiso 1 1 d R . . O15A O 0.8675(10) 0.7668(4) 0.5071(4) 0.040(3) Uani 0.70(2) 1 d P B 3 O16A O 0.9209(12) 0.7157(5) 0.6228(6) 0.041(3) Uani 0.70(2) 1 d P B 3 O17A O 0.7178(8) 0.7502(5) 0.6077(7) 0.042(2) Uani 0.70(2) 1 d P B 3 O15B O 0.939(2) 0.7537(10) 0.5229(11) 0.037(6) Uani 0.30(2) 1 d P B 4 O16B O 0.863(2) 0.7145(11) 0.6460(11) 0.034(5) Uani 0.30(2) 1 d P B 4 O17B O 0.7326(15) 0.7631(10) 0.5620(17) 0.037(7) Uani 0.30(2) 1 d P B 4 O18 O 0.8386(5) 0.4416(3) 0.5413(3) 0.0427(13) Uani 1 1 d . A . H18 H 0.8842 0.4051 0.5739 0.051 Uiso 1 1 d R . . O19 O 0.9668(4) 0.2361(3) 1.0502(3) 0.0373(12) Uani 1 1 d . . . O20 O 0.7894(5) 0.2301(3) 1.1293(3) 0.0440(13) Uani 1 1 d . . . O21 O 0.7836(4) 0.2766(3) 1.0051(3) 0.0354(11) Uani 1 1 d . . . O22 O 0.8363(4) -0.0638(3) 1.0490(3) 0.0315(10) Uani 1 1 d . . . H22 H 0.8598 -0.0941 1.0829 0.038 Uiso 1 1 d R . . O23 O 0.2091(4) 0.1652(3) 1.0566(2) 0.0295(10) Uani 1 1 d . . . O24 O 0.1497(4) 0.1027(3) 1.1774(3) 0.0359(11) Uani 1 1 d . . . O25 O 0.2808(5) 0.1907(3) 1.1473(3) 0.0393(12) Uani 1 1 d . . . O26 O 0.6245(4) -0.0976(3) 1.0999(3) 0.0409(13) Uani 1 1 d . . . H26 H 0.6862 -0.0821 1.0725 0.049 Uiso 1 1 d R . . O27 O 0.5298(8) -0.1160(4) 1.5002(4) 0.079(3) Uani 1 1 d . . . O28 O 0.5477(10) -0.0031(5) 1.4105(6) 0.120(4) Uani 1 1 d U . . O29 O 0.3745(7) -0.0476(6) 1.4395(4) 0.098(3) Uani 1 1 d U . . O30 O 0.6874(5) -0.2062(3) 1.2141(3) 0.0438(14) Uani 1 1 d . . . H30 H 0.6589 -0.1762 1.1734 0.053 Uiso 1 1 d R . . O31 O 1.0179(6) 0.0154(3) 1.3554(4) 0.0532(16) Uani 1 1 d . . . O32 O 1.0467(10) -0.1044(5) 1.4303(4) 0.090(3) Uani 1 1 d U . . O33 O 1.1969(6) -0.0593(4) 1.3375(5) 0.068(2) Uani 1 1 d . . . O34 O 0.8960(4) -0.1573(3) 1.1682(3) 0.0309(10) Uani 1 1 d . . . H34 H 0.8262 -0.1780 1.1915 0.037 Uiso 1 1 d R . . O35 O 1.0616(10) 0.1609(5) 1.2973(6) 0.109(3) Uani 1 1 d U . . O36 O 0.8393(8) 0.0444(5) 1.4779(4) 0.076(2) Uani 1 1 d . . . O37 O 0.7630(9) 0.0319(6) 1.3638(7) 0.109(3) Uani 1 1 d U . . O38 O 0.8215(10) 0.2402(5) 1.2866(5) 0.102(3) Uani 1 1 d . . . O39A O 0.872(2) 0.2099(10) 1.4161(10) 0.108(8) Uani 0.518(12) 1 d P . . O39B O 0.9598(14) 0.1644(9) 1.4263(7) 0.058(5) Uani 0.482(12) 1 d P . . O40A O 0.9297(10) 0.1150(6) 1.2363(6) 0.048(3) Uani 0.518(12) 1 d P . . O40B O 0.8235(11) 0.1166(7) 1.2495(6) 0.047(4) Uani 0.482(12) 1 d P . . O41A O 0.6844(14) 0.1662(9) 1.3827(8) 0.074(5) Uani 0.518(12) 1 d PU . . O41B O 0.7057(12) 0.1694(8) 1.4289(10) 0.063(5) Uani 0.482(12) 1 d P . . O42 O 0.3519(8) 0.6474(7) 0.8443(6) 0.115(3) Uani 1 1 d U . . H42A H 0.3130 0.6697 0.8815 0.138 Uiso 1 1 d R . . H42B H 0.3400 0.6025 0.8669 0.138 Uiso 1 1 d R . . O43 O 0.4798(5) 0.7489(4) 0.8663(3) 0.0524(16) Uani 1 1 d . . . O44 O 0.6740(8) 0.7369(5) 0.7447(5) 0.089(3) Uani 1 1 d U . . O45A O 0.5315(10) 0.6116(6) 0.7185(6) 0.040(2) Uani 0.50 1 d P . . O45B O 0.5313(11) 0.6825(8) 0.7018(7) 0.056(3) Uani 0.50 1 d P . . O46 O 0.5232(9) 0.5233(6) 0.8386(5) 0.101(3) Uani 1 1 d U . . O47 O 0.5183(6) 0.5894(4) 0.9471(3) 0.0519(15) Uani 1 1 d . . . H47A H 0.5356 0.6179 0.9667 0.062 Uiso 1 1 d R . . H47B H 0.4369 0.5924 0.9634 0.062 Uiso 1 1 d R . . O48 O 0.7030(5) 0.6588(4) 0.8808(4) 0.0578(17) Uani 1 1 d . . . O49 O 0.7341(5) 0.5744(3) 0.7895(4) 0.0539(17) Uani 1 1 d . . . H49A H 0.7997 0.5953 0.7778 0.065 Uiso 1 1 d R . . H49B H 0.7398 0.5347 0.7767 0.065 Uiso 1 1 d R . . O50 O 0.4205(14) 0.7373(7) 0.7490(6) 0.067(4) Uani 0.50 1 d P . . O51 O 0.9479(13) 0.4594(8) 0.0495(8) 0.066(4) Uani 0.50 1 d PU . . O52 O 0.2960(8) 0.5055(5) 0.8496(6) 0.097(3) Uani 1 1 d U . . O53 O 0.8101(7) 0.5277(5) 0.9604(6) 0.093(3) Uani 1 1 d U . . O54 O 0.9452(4) 0.6209(3) 0.7559(3) 0.0405(12) Uani 1 1 d . . . O55 O 0.1306(7) 0.7033(4) 0.4768(4) 0.0206(16) Uani 0.50 1 d PU . . O56 O 0.7074(10) 0.2092(7) 0.5583(7) 0.128(4) Uani 1 1 d U . . O57A O 0.5069(9) 0.7195(7) 0.5974(7) 0.061(5) Uani 0.533(17) 1 d P . . O57B O 0.4600(13) 0.7499(7) 0.5313(8) 0.058(5) Uani 0.467(17) 1 d PU . . O58A O 0.7641(12) 0.9117(6) 0.5017(11) 0.076(6) Uani 0.67(3) 1 d P . . O58B O 0.7276(14) 0.9039(8) 0.5566(12) 0.029(6) Uani 0.33(3) 1 d P . . O59 O 0.4997(10) 0.8613(7) 0.6460(7) 0.053(3) Uani 0.50 1 d P . . O60A O 0.9411(11) 0.3172(6) 0.1722(5) 0.049(4) Uani 0.63(3) 1 d P . . O60B O 1.028(2) 0.2850(13) 0.1870(10) 0.068(9) Uani 0.37(3) 1 d P . . O61 O 0.3128(7) 0.5762(4) 1.0403(4) 0.0633(19) Uani 1 1 d . . . O62 O 0.2698(8) 0.0756(5) 0.3251(5) 0.091(3) Uani 1 1 d U . . O63 O 0.7149(7) 0.0215(5) 0.2280(4) 0.069(2) Uani 1 1 d . . . O64 O 0.5039(7) 0.8930(4) 0.7658(4) 0.070(2) Uani 1 1 d . . . O65 O 0.6795(14) 0.4754(7) 0.7266(7) 0.064(4) Uani 0.50 1 d P . . C1 C 0.9961(5) 0.4088(4) 0.6827(3) 0.0275(13) Uani 1 1 d . A . C2 C 1.0261(5) 0.4262(4) 0.7358(4) 0.0278(13) Uani 1 1 d . . . H2 H 1.0659 0.4647 0.7255 0.033 Uiso 1 1 calc R . . C3 C 0.9975(5) 0.3866(4) 0.8049(3) 0.0277(13) Uani 1 1 d . . . C4 C 0.9350(5) 0.3295(3) 0.8219(3) 0.0267(13) Uani 1 1 d . . . H4 H 0.9146 0.3043 0.8683 0.032 Uiso 1 1 calc R . . C5 C 0.9035(5) 0.3105(3) 0.7693(3) 0.0251(12) Uani 1 1 d . . . C6 C 0.9358(5) 0.3498(3) 0.6998(4) 0.0272(13) Uani 1 1 d . . . C7 C 0.8356(5) 0.2487(3) 0.7890(4) 0.0271(13) Uani 1 1 d . . . H7A H 0.8537 0.2156 0.8333 0.033 Uiso 1 1 calc R . . H7B H 0.8597 0.2230 0.7541 0.033 Uiso 1 1 calc R . . C8 C 0.7055(5) 0.2731(3) 0.7948(3) 0.0231(12) Uani 1 1 d . . . C9 C 0.6408(5) 0.2778(3) 0.8588(3) 0.0252(12) Uani 1 1 d . . . H9 H 0.6772 0.2667 0.8978 0.030 Uiso 1 1 calc R . . C10 C 0.5218(5) 0.2993(4) 0.8635(3) 0.0263(13) Uani 1 1 d . . . C11 C 0.4660(5) 0.3175(3) 0.8054(3) 0.0255(12) Uani 1 1 d . . . H11 H 0.3864 0.3329 0.8095 0.031 Uiso 1 1 calc R . . C12 C 0.5287(5) 0.3128(3) 0.7416(3) 0.0231(12) Uani 1 1 d . . . C13 C 0.6483(5) 0.2890(3) 0.7377(3) 0.0237(12) Uani 1 1 d . . . C14 C 0.4660(6) 0.3359(3) 0.6789(3) 0.0277(13) Uani 1 1 d . . . H14A H 0.3878 0.3247 0.6935 0.033 Uiso 1 1 calc R . . H14B H 0.5059 0.3099 0.6459 0.033 Uiso 1 1 calc R . . C15 C 0.4622(6) 0.4160(4) 0.6444(3) 0.0277(13) Uani 1 1 d . A . C16 C 0.3723(6) 0.4634(4) 0.6667(4) 0.0350(16) Uani 1 1 d . . . H16 H 0.3126 0.4460 0.7012 0.042 Uiso 1 1 calc R A . C17 C 0.3703(5) 0.5372(3) 0.6377(4) 0.045(2) Uani 1 1 d D A . C18 C 0.4592(6) 0.5638(4) 0.5866(5) 0.0412(19) Uani 1 1 d . . . H18A H 0.4573 0.6131 0.5678 0.049 Uiso 1 1 calc R A . C19 C 0.5510(6) 0.5173(4) 0.5633(4) 0.0327(15) Uani 1 1 d . A . C20 C 0.5502(6) 0.4440(4) 0.5920(3) 0.0301(14) Uani 1 1 d . . . C21 C 0.6462(7) 0.5478(4) 0.5068(3) 0.0351(16) Uani 1 1 d . . . H21A H 0.6137 0.5931 0.4765 0.042 Uiso 1 1 calc R A . H21B H 0.6766 0.5150 0.4788 0.042 Uiso 1 1 calc R . . C22 C 0.7459(6) 0.5601(4) 0.5363(3) 0.0314(14) Uani 1 1 d . A . C23 C 0.7461(7) 0.6262(4) 0.5447(3) 0.0324(14) Uani 1 1 d . . . H23 H 0.6861 0.6638 0.5321 0.039 Uiso 1 1 calc R A . C24 C 0.8364(6) 0.6362(4) 0.5721(4) 0.0311(14) Uani 1 1 d . A . C25 C 0.9248(6) 0.5811(4) 0.5926(3) 0.0306(14) Uani 1 1 d . . . H25 H 0.9832 0.5888 0.6119 0.037 Uiso 1 1 calc R A . C26 C 0.9271(6) 0.5138(4) 0.5845(3) 0.0313(14) Uani 1 1 d . A . C27 C 0.8374(6) 0.5045(4) 0.5554(3) 0.0309(14) Uani 1 1 d . . . C28 C 1.0243(6) 0.4533(4) 0.6077(4) 0.0321(14) Uani 1 1 d . . . H28A H 1.0398 0.4224 0.5776 0.039 Uiso 1 1 calc R A . H28B H 1.0940 0.4734 0.6026 0.039 Uiso 1 1 calc R . . C29 C 0.9299(5) 0.0148(4) 1.0807(3) 0.0252(12) Uani 1 1 d . . . C30 C 0.9327(5) 0.0848(4) 1.0807(3) 0.0258(13) Uani 1 1 d . . . H30A H 0.9927 0.0944 1.0973 0.031 Uiso 1 1 calc R . . C31 C 0.8448(5) 0.1400(3) 1.0556(3) 0.0247(12) Uani 1 1 d . . . C32 C 0.7530(5) 0.1269(4) 1.0315(3) 0.0254(12) Uani 1 1 d . . . H32 H 0.6946 0.1644 1.0160 0.030 Uiso 1 1 calc R . . C33 C 0.7481(5) 0.0582(4) 1.0303(3) 0.0249(12) Uani 1 1 d . . . C34 C 0.8396(5) 0.0027(4) 1.0547(3) 0.0261(12) Uani 1 1 d . . . C35 C 0.6487(6) 0.0446(4) 1.0035(4) 0.0299(14) Uani 1 1 d . . . H35A H 0.6750 0.0044 0.9842 0.036 Uiso 1 1 calc R . . H35B H 0.6247 0.0865 0.9662 0.036 Uiso 1 1 calc R . . C36 C 0.5456(6) 0.0284(3) 1.0601(4) 0.0295(14) Uani 1 1 d . . . C37 C 0.4531(6) 0.0824(3) 1.0675(4) 0.0282(13) Uani 1 1 d . . . H37 H 0.4537 0.1286 1.0371 0.034 Uiso 1 1 calc R . . C38 C 0.3607(6) 0.0677(3) 1.1199(4) 0.0283(13) Uani 1 1 d . . . C39 C 0.3581(6) -0.0002(4) 1.1672(4) 0.0334(15) Uani 1 1 d . . . H39 H 0.2955 -0.0086 1.2027 0.040 Uiso 1 1 calc R . . C40 C 0.4485(6) -0.0553(4) 1.1618(5) 0.0366(17) Uani 1 1 d . . . C41 C 0.5408(6) -0.0407(3) 1.1068(4) 0.0332(16) Uani 1 1 d . . . C42 C 0.4492(6) -0.1289(4) 1.2143(5) 0.045(2) Uani 1 1 d . . . H42C H 0.4783 -0.1655 1.1904 0.054 Uiso 1 1 calc R . . H42D H 0.3707 -0.1350 1.2369 0.054 Uiso 1 1 calc R . . C43 C 0.5250(6) -0.1385(4) 1.2692(5) 0.044(2) Uani 1 1 d . . . C44 C 0.4820(6) -0.1060(4) 1.3227(5) 0.051(2) Uani 1 1 d . . . H44 H 0.4083 -0.0790 1.3240 0.061 Uiso 1 1 calc R . . C45 C 0.5479(6) -0.1136(4) 1.3735(5) 0.046(2) Uani 1 1 d . . . C46 C 0.6577(6) -0.1537(4) 1.3726(4) 0.0414(18) Uani 1 1 d . . . H46 H 0.7006 -0.1595 1.4077 0.050 Uiso 1 1 calc R . . C47 C 0.7043(6) -0.1854(4) 1.3189(4) 0.0381(18) Uani 1 1 d . . . C48 C 0.6376(6) -0.1762(4) 1.2678(5) 0.0368(17) Uani 1 1 d . . . C49 C 0.8295(5) -0.2231(4) 1.3161(4) 0.0324(15) Uani 1 1 d . . . H49C H 0.8443 -0.2519 1.3626 0.039 Uiso 1 1 calc R . . H49D H 0.8437 -0.2546 1.2867 0.039 Uiso 1 1 calc R . . C50 C 0.9092(5) -0.1665(3) 1.2867(3) 0.0242(12) Uani 1 1 d . . . C51 C 0.9537(5) -0.1432(4) 1.3318(3) 0.0273(13) Uani 1 1 d . . . H51 H 0.9391 -0.1643 1.3797 0.033 Uiso 1 1 calc R . . C52 C 1.0201(6) -0.0881(4) 1.3049(3) 0.0271(13) Uani 1 1 d . . . C53 C 1.0425(5) -0.0557(3) 1.2331(3) 0.0239(12) Uani 1 1 d . . . H53 H 1.0865 -0.0186 1.2161 0.029 Uiso 1 1 calc R . . C54 C 0.9998(5) -0.0783(3) 1.1873(3) 0.0227(12) Uani 1 1 d . . . C55 C 0.9327(5) -0.1340(3) 1.2154(3) 0.0229(12) Uani 1 1 d . . . C56 C 1.0257(5) -0.0445(4) 1.1092(3) 0.0262(13) Uani 1 1 d . . . H56A H 1.0370 -0.0814 1.0860 0.031 Uiso 1 1 calc R . . H56B H 1.0974 -0.0249 1.0986 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01879(11) 0.02292(11) 0.02255(11) -0.00556(8) -0.00498(8) -0.00251(8) Eu1 0.0866(3) 0.02737(19) 0.02598(19) -0.00960(15) 0.00514(19) -0.01359(19) Eu2 0.03300(19) 0.0481(2) 0.03071(19) -0.01012(16) -0.00034(14) 0.00299(16) S1 0.0268(7) 0.0239(7) 0.0315(8) -0.0009(6) -0.0062(6) -0.0032(6) S2 0.0188(7) 0.0378(9) 0.0228(7) -0.0067(6) -0.0008(5) -0.0020(6) S3 0.0229(10) 0.0297(11) 0.211(4) 0.0121(17) 0.0195(16) 0.0038(8) S4 0.0379(9) 0.0261(8) 0.0331(9) -0.0020(7) -0.0124(7) -0.0087(7) S5 0.0207(7) 0.0289(8) 0.0275(8) -0.0055(6) -0.0028(6) -0.0077(6) S6 0.0269(7) 0.0215(7) 0.0302(8) -0.0040(6) -0.0095(6) -0.0014(6) S7 0.0295(9) 0.0431(11) 0.0673(15) 0.0046(10) 0.0113(9) 0.0036(8) S8 0.0685(13) 0.0360(10) 0.0312(9) -0.0065(8) -0.0228(9) -0.0149(9) O1 0.043(3) 0.031(3) 0.038(3) -0.013(2) -0.015(2) 0.000(2) O2 0.028(2) 0.027(2) 0.030(2) -0.0085(19) -0.0048(18) -0.0037(18) O3 0.023(2) 0.034(3) 0.035(3) -0.001(2) -0.0065(19) -0.0091(19) O4 0.027(2) 0.029(2) 0.033(3) -0.003(2) -0.0051(19) -0.0040(18) O5 0.046(3) 0.026(3) 0.045(3) -0.006(2) -0.008(2) -0.003(2) O6 0.043(3) 0.031(3) 0.032(3) -0.011(2) 0.005(2) -0.010(2) O7 0.022(2) 0.048(3) 0.028(2) -0.008(2) 0.0008(18) -0.006(2) O8 0.037(3) 0.040(3) 0.030(3) -0.014(2) 0.000(2) 0.000(2) O9 0.027(2) 0.053(3) 0.024(2) -0.008(2) -0.0045(19) -0.001(2) O10 0.033(2) 0.040(3) 0.027(2) -0.014(2) 0.0006(19) -0.003(2) O11A 0.035(4) 0.035(4) 0.162(8) -0.010(5) -0.002(5) 0.009(4) O12A 0.037(4) 0.034(4) 0.165(7) -0.009(5) -0.010(4) 0.003(3) O13A 0.029(4) 0.025(4) 0.157(7) -0.025(4) -0.007(4) -0.005(3) O11B 0.032(4) 0.030(5) 0.164(8) -0.004(5) -0.002(5) 0.004(4) O12B 0.030(4) 0.036(5) 0.168(8) 0.000(5) -0.009(5) 0.002(4) O13B 0.029(4) 0.034(4) 0.162(7) -0.017(5) -0.008(4) -0.001(4) O14 0.057(3) 0.033(3) 0.030(3) -0.009(2) 0.002(2) -0.015(2) O15A 0.048(6) 0.029(4) 0.037(4) 0.002(3) -0.007(4) -0.010(4) O16A 0.049(7) 0.031(4) 0.045(6) -0.001(4) -0.023(5) -0.012(4) O17A 0.043(5) 0.038(5) 0.047(7) -0.016(4) -0.001(4) -0.012(4) O15B 0.040(13) 0.027(9) 0.041(11) -0.008(8) 0.006(9) -0.009(8) O16B 0.037(12) 0.036(10) 0.029(10) -0.012(8) -0.008(9) -0.003(9) O17B 0.020(8) 0.027(9) 0.070(19) -0.021(10) -0.015(10) 0.005(6) O18 0.064(4) 0.034(3) 0.031(3) -0.012(2) 0.007(2) -0.020(3) O19 0.025(2) 0.031(3) 0.048(3) 0.006(2) -0.013(2) -0.0085(19) O20 0.057(3) 0.048(3) 0.032(3) -0.018(2) 0.008(2) -0.025(3) O21 0.029(2) 0.032(3) 0.045(3) -0.006(2) -0.015(2) -0.001(2) O22 0.036(3) 0.027(2) 0.032(2) -0.011(2) -0.011(2) 0.0049(19) O23 0.028(2) 0.030(2) 0.028(2) -0.0050(19) -0.0125(19) 0.0047(18) O24 0.038(3) 0.026(2) 0.036(3) -0.002(2) -0.001(2) -0.004(2) O25 0.050(3) 0.029(3) 0.045(3) -0.011(2) -0.021(3) -0.005(2) O26 0.031(3) 0.024(2) 0.070(4) -0.013(2) -0.018(3) 0.002(2) O27 0.120(7) 0.044(4) 0.093(6) -0.024(4) -0.083(5) 0.014(4) O28 0.131(6) 0.077(5) 0.134(6) -0.048(5) 0.060(5) -0.025(4) O29 0.049(4) 0.161(7) 0.056(4) -0.024(4) -0.004(3) 0.030(4) O30 0.038(3) 0.025(2) 0.070(4) -0.009(3) -0.025(3) -0.002(2) O31 0.057(4) 0.052(4) 0.064(4) -0.037(3) -0.008(3) -0.007(3) O32 0.158(7) 0.084(5) 0.045(4) -0.006(3) -0.038(4) -0.054(5) O33 0.044(4) 0.078(5) 0.106(6) -0.046(5) -0.045(4) 0.004(3) O34 0.032(2) 0.029(2) 0.035(3) -0.010(2) -0.015(2) -0.0005(19) O35 0.120(6) 0.073(5) 0.104(6) -0.024(4) 0.053(5) -0.018(4) O36 0.101(6) 0.076(5) 0.040(4) -0.012(4) 0.015(4) -0.020(5) O37 0.090(5) 0.102(6) 0.168(7) -0.072(5) -0.040(5) -0.016(4) O38 0.147(9) 0.057(5) 0.098(7) 0.010(5) -0.046(7) -0.034(5) O39A 0.18(2) 0.069(11) 0.086(13) -0.057(10) -0.050(14) 0.035(13) O39B 0.080(10) 0.071(10) 0.036(7) -0.004(6) -0.010(6) -0.052(9) O40A 0.049(7) 0.048(7) 0.038(6) -0.002(5) -0.002(5) -0.007(5) O40B 0.045(7) 0.055(8) 0.030(6) -0.010(5) -0.010(5) 0.014(5) O41A 0.080(8) 0.077(8) 0.049(7) -0.025(6) -0.013(6) 0.034(6) O41B 0.044(8) 0.059(9) 0.078(12) -0.018(8) 0.008(7) -0.008(6) O42 0.076(5) 0.177(7) 0.130(6) -0.115(6) -0.017(5) 0.012(5) O43 0.045(3) 0.073(4) 0.044(3) -0.033(3) -0.011(3) 0.011(3) O44 0.080(5) 0.072(5) 0.073(5) 0.003(4) 0.029(4) 0.003(4) O45A 0.049(6) 0.031(5) 0.043(6) -0.017(5) -0.023(5) 0.009(5) O45B 0.040(6) 0.081(10) 0.050(7) -0.018(7) -0.006(5) -0.015(6) O46 0.098(5) 0.135(6) 0.101(6) -0.073(5) 0.031(4) -0.068(5) O47 0.058(4) 0.064(4) 0.043(3) -0.016(3) -0.001(3) -0.032(3) O48 0.040(3) 0.064(4) 0.081(5) -0.035(4) -0.005(3) -0.016(3) O49 0.032(3) 0.056(4) 0.086(5) -0.041(4) -0.002(3) -0.008(3) O50 0.105(12) 0.046(7) 0.025(6) 0.000(5) -0.006(6) 0.021(7) O51 0.072(7) 0.066(7) 0.063(7) -0.021(5) -0.014(6) -0.004(5) O52 0.071(5) 0.066(4) 0.162(7) -0.026(5) -0.036(5) -0.021(4) O53 0.060(4) 0.063(4) 0.157(7) -0.035(5) -0.014(4) -0.010(3) O54 0.028(2) 0.045(3) 0.043(3) -0.009(3) -0.006(2) -0.002(2) O55 0.028(3) 0.020(3) 0.019(3) -0.011(2) 0.006(2) -0.013(2) O56 0.117(6) 0.129(7) 0.133(7) 0.020(5) -0.053(5) -0.069(5) O57A 0.031(6) 0.064(8) 0.065(9) 0.018(6) -0.006(5) -0.014(5) O57B 0.060(7) 0.042(6) 0.064(7) 0.000(5) -0.011(5) -0.010(5) O58A 0.069(8) 0.042(6) 0.119(18) -0.020(7) -0.030(9) -0.001(5) O58B 0.025(8) 0.019(7) 0.046(13) -0.007(7) -0.019(8) 0.003(5) O59 0.036(6) 0.078(9) 0.073(9) -0.065(8) -0.014(6) 0.004(6) O60A 0.059(8) 0.050(6) 0.040(6) -0.018(5) 0.000(5) -0.012(5) O60B 0.09(2) 0.073(15) 0.043(11) -0.022(10) 0.009(11) -0.029(14) O61 0.083(5) 0.043(4) 0.058(4) -0.015(3) 0.017(4) -0.023(3) O62 0.096(5) 0.081(5) 0.098(5) 0.013(4) -0.058(4) -0.037(4) O63 0.075(5) 0.085(5) 0.051(4) -0.021(4) -0.012(4) -0.016(4) O64 0.066(5) 0.061(4) 0.077(5) -0.007(4) -0.022(4) -0.007(4) O65 0.099(11) 0.042(7) 0.054(8) -0.027(6) -0.013(8) 0.005(7) C1 0.023(3) 0.027(3) 0.025(3) -0.003(2) 0.003(2) -0.001(2) C2 0.020(3) 0.026(3) 0.031(3) -0.001(3) -0.002(2) -0.003(2) C3 0.023(3) 0.027(3) 0.027(3) 0.001(3) -0.006(2) -0.002(2) C4 0.021(3) 0.027(3) 0.025(3) 0.002(2) -0.006(2) -0.002(2) C5 0.015(3) 0.024(3) 0.027(3) -0.001(2) 0.001(2) 0.002(2) C6 0.021(3) 0.027(3) 0.029(3) -0.009(3) 0.003(2) -0.001(2) C7 0.020(3) 0.025(3) 0.030(3) -0.001(3) -0.003(2) -0.002(2) C8 0.021(3) 0.018(3) 0.026(3) -0.001(2) -0.004(2) -0.001(2) C9 0.023(3) 0.027(3) 0.020(3) 0.001(2) -0.005(2) -0.004(2) C10 0.020(3) 0.031(3) 0.025(3) -0.005(3) -0.001(2) -0.005(2) C11 0.021(3) 0.022(3) 0.030(3) -0.003(2) -0.005(2) -0.001(2) C12 0.025(3) 0.019(3) 0.022(3) 0.001(2) -0.004(2) -0.005(2) C13 0.027(3) 0.019(3) 0.022(3) -0.005(2) 0.001(2) -0.002(2) C14 0.029(3) 0.026(3) 0.028(3) -0.003(3) -0.007(3) -0.008(2) C15 0.028(3) 0.028(3) 0.027(3) 0.001(3) -0.015(3) -0.005(2) C16 0.028(3) 0.032(4) 0.041(4) 0.002(3) -0.013(3) -0.008(3) C17 0.023(3) 0.032(4) 0.073(6) 0.000(4) -0.018(4) 0.000(3) C18 0.033(4) 0.030(4) 0.055(5) 0.007(3) -0.025(3) -0.008(3) C19 0.038(4) 0.034(4) 0.029(3) 0.000(3) -0.018(3) -0.014(3) C20 0.040(4) 0.030(3) 0.024(3) -0.004(3) -0.014(3) -0.011(3) C21 0.052(4) 0.038(4) 0.019(3) 0.001(3) -0.014(3) -0.021(3) C22 0.042(4) 0.034(4) 0.018(3) 0.001(3) -0.006(3) -0.017(3) C23 0.042(4) 0.029(3) 0.024(3) 0.001(3) -0.008(3) -0.012(3) C24 0.037(4) 0.026(3) 0.028(3) 0.001(3) -0.009(3) -0.011(3) C25 0.033(3) 0.033(3) 0.023(3) -0.001(3) -0.003(3) -0.011(3) C26 0.038(4) 0.032(3) 0.019(3) 0.001(3) 0.001(3) -0.013(3) C27 0.044(4) 0.029(3) 0.018(3) -0.002(2) 0.002(3) -0.017(3) C28 0.034(3) 0.031(3) 0.024(3) -0.003(3) 0.004(3) -0.007(3) C29 0.021(3) 0.031(3) 0.019(3) -0.005(2) -0.001(2) -0.001(2) C30 0.015(3) 0.035(3) 0.024(3) -0.003(3) -0.002(2) -0.005(2) C31 0.021(3) 0.029(3) 0.023(3) -0.006(2) -0.001(2) -0.004(2) C32 0.019(3) 0.030(3) 0.025(3) -0.007(3) -0.004(2) 0.001(2) C33 0.024(3) 0.031(3) 0.022(3) -0.009(2) -0.007(2) -0.003(2) C34 0.024(3) 0.029(3) 0.025(3) -0.013(3) -0.002(2) 0.002(2) C35 0.027(3) 0.032(3) 0.033(3) -0.010(3) -0.016(3) 0.002(3) C36 0.029(3) 0.024(3) 0.041(4) -0.012(3) -0.017(3) -0.001(2) C37 0.030(3) 0.022(3) 0.035(3) -0.008(3) -0.016(3) -0.001(2) C38 0.027(3) 0.026(3) 0.035(3) -0.007(3) -0.016(3) -0.003(2) C39 0.027(3) 0.024(3) 0.048(4) -0.002(3) -0.017(3) -0.005(3) C40 0.027(3) 0.022(3) 0.060(5) -0.001(3) -0.020(3) -0.005(3) C41 0.026(3) 0.020(3) 0.057(5) -0.009(3) -0.022(3) 0.002(2) C42 0.024(3) 0.022(3) 0.082(6) 0.003(4) -0.020(4) -0.004(3) C43 0.025(3) 0.026(3) 0.069(6) 0.009(4) -0.017(4) -0.004(3) C44 0.020(3) 0.038(4) 0.070(6) 0.017(4) -0.004(3) -0.004(3) C45 0.024(3) 0.039(4) 0.055(5) 0.008(4) 0.000(3) -0.002(3) C46 0.025(3) 0.038(4) 0.045(4) 0.006(3) -0.002(3) -0.001(3) C47 0.019(3) 0.026(3) 0.054(5) 0.005(3) -0.003(3) -0.002(2) C48 0.025(3) 0.020(3) 0.058(5) 0.003(3) -0.013(3) -0.004(2) C49 0.020(3) 0.027(3) 0.041(4) 0.002(3) -0.008(3) 0.000(2) C50 0.018(3) 0.024(3) 0.027(3) -0.008(2) -0.001(2) 0.001(2) C51 0.027(3) 0.030(3) 0.023(3) -0.006(3) -0.005(2) 0.000(2) C52 0.031(3) 0.027(3) 0.023(3) -0.007(2) -0.004(2) -0.004(3) C53 0.024(3) 0.023(3) 0.023(3) -0.001(2) -0.009(2) -0.001(2) C54 0.018(3) 0.028(3) 0.021(3) -0.006(2) -0.002(2) -0.001(2) C55 0.017(3) 0.023(3) 0.028(3) -0.009(2) -0.006(2) 0.005(2) C56 0.021(3) 0.033(3) 0.020(3) -0.004(2) -0.002(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O1 1.759(5) . ? U O2 1.759(5) . ? U O23 2.308(4) 1_655 ? U O7 2.326(5) 1_655 ? U O19 2.346(5) . ? U O4 2.479(5) . ? U O3 2.511(5) . ? Eu1 O41A 2.326(15) . ? Eu1 O39B 2.329(12) . ? Eu1 O31 2.352(6) . ? Eu1 O37 2.373(9) . ? Eu1 O36 2.389(7) . ? Eu1 O39A 2.449(15) . ? Eu1 O38 2.464(9) . ? Eu1 O35 2.477(10) . ? Eu1 O41B 2.478(15) . ? Eu1 O40B 2.487(12) . ? Eu1 O40A 2.494(12) . ? Eu2 O42 2.383(10) . ? Eu2 O49 2.399(6) . ? Eu2 O45B 2.402(13) . ? Eu2 O48 2.413(6) . ? Eu2 O43 2.425(6) . ? Eu2 O47 2.428(6) . ? Eu2 O46 2.462(9) . ? Eu2 O44 2.465(8) . ? Eu2 O50 2.488(13) . ? Eu2 O45A 2.522(10) . ? S1 O5 1.438(5) . ? S1 O3 1.480(5) . ? S1 O4 1.483(5) . ? S1 C3 1.753(7) . ? S2 O9 1.447(5) . ? S2 O8 1.450(6) . ? S2 O7 1.488(5) . ? S2 C10 1.761(7) . ? S3 O12A 1.354(6) . ? S3 O13B 1.390(6) . ? S3 O11B 1.416(6) . ? S3 O13A 1.461(6) . ? S3 O12B 1.543(7) . ? S3 O11A 1.547(6) . ? S3 C17 1.744(5) . ? S4 O17B 1.370(16) . ? S4 O15A 1.426(8) . ? S4 O16B 1.454(19) . ? S4 O16A 1.454(9) . ? S4 O17A 1.501(10) . ? S4 O15B 1.534(18) . ? S4 C24 1.779(7) . ? S5 O21 1.427(5) . ? S5 O20 1.458(6) . ? S5 O19 1.482(5) . ? S5 C31 1.764(7) . ? S6 O25 1.447(5) . ? S6 O24 1.452(5) . ? S6 O23 1.494(5) . ? S6 C38 1.771(7) . ? S7 O27 1.416(7) . ? S7 O29 1.423(8) . ? S7 O28 1.430(10) . ? S7 C45 1.771(10) . ? S8 O33 1.422(7) . ? S8 O32 1.437(8) . ? S8 O31 1.458(7) . ? S8 C52 1.754(7) . ? O6 C6 1.356(8) . ? O6 H6 0.9026 . ? O7 U 2.326(5) 1_455 ? O10 C13 1.365(8) . ? O10 H10 0.9181 . ? O14 C20 1.365(9) . ? O14 H14 0.8778 . ? O18 C27 1.369(8) . ? O18 H18 0.9693 . ? O22 C34 1.374(8) . ? O22 H22 0.8152 . ? O23 U 2.308(4) 1_455 ? O26 C41 1.368(8) . ? O26 H26 0.8750 . ? O30 C48 1.386(11) . ? O30 H30 0.9375 . ? O34 C55 1.374(8) . ? O34 H34 0.9726 . ? O42 H42A 0.9885 . ? O42 H42B 0.8914 . ? O47 H47A 0.8675 . ? O47 H47B 0.9565 . ? O49 H49A 0.9160 . ? O49 H49B 0.8942 . ? C1 C2 1.374(10) . ? C1 C6 1.416(9) . ? C1 C28 1.514(9) . ? C2 C3 1.392(9) . ? C2 H2 0.9300 . ? C3 C4 1.401(9) . ? C4 C5 1.392(10) . ? C4 H4 0.9300 . ? C5 C6 1.403(9) . ? C5 C7 1.515(9) . ? C7 C8 1.519(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.392(9) . ? C8 C9 1.397(9) . ? C9 C10 1.388(8) . ? C9 H9 0.9300 . ? C10 C11 1.392(9) . ? C11 C12 1.386(9) . ? C11 H11 0.9300 . ? C12 C13 1.401(9) . ? C12 C14 1.515(9) . ? C14 C15 1.517(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.378(10) . ? C15 C20 1.402(10) . ? C16 C17 1.393(9) . ? C16 H16 0.9300 . ? C17 C18 1.387(10) . ? C18 C19 1.388(12) . ? C18 H18A 0.9300 . ? C19 C20 1.388(10) . ? C19 C21 1.516(10) . ? C21 C22 1.535(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.382(10) . ? C22 C27 1.400(11) . ? C23 C24 1.390(10) . ? C23 H23 0.9300 . ? C24 C25 1.375(10) . ? C25 C26 1.395(10) . ? C25 H25 0.9300 . ? C26 C27 1.398(10) . ? C26 C28 1.515(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.391(9) . ? C29 C30 1.400(9) . ? C29 C56 1.520(9) . ? C30 C31 1.396(9) . ? C30 H30A 0.9300 . ? C31 C32 1.394(8) . ? C32 C33 1.387(9) . ? C32 H32 0.9300 . ? C33 C34 1.424(9) . ? C33 C35 1.512(8) . ? C35 C36 1.517(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.391(9) . ? C36 C41 1.406(10) . ? C37 C38 1.378(10) . ? C37 H37 0.9300 . ? C38 C39 1.389(9) . ? C39 C40 1.382(10) . ? C39 H39 0.9300 . ? C40 C41 1.406(11) . ? C40 C42 1.513(10) . ? C42 C43 1.528(12) . ? C42 H42C 0.9700 . ? C42 H42D 0.9700 . ? C43 C48 1.394(10) . ? C43 C44 1.402(14) . ? C44 C45 1.382(13) . ? C44 H44 0.9300 . ? C45 C46 1.384(10) . ? C46 C47 1.402(12) . ? C46 H46 0.9300 . ? C47 C48 1.388(11) . ? C47 C49 1.523(9) . ? C49 C50 1.521(9) . ? C49 H49C 0.9700 . ? C49 H49D 0.9700 . ? C50 C55 1.389(9) . ? C50 C51 1.390(9) . ? C51 C52 1.389(9) . ? C51 H51 0.9300 . ? C52 C53 1.395(9) . ? C53 C54 1.382(8) . ? C53 H53 0.9300 . ? C54 C55 1.406(9) . ? C54 C56 1.515(8) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U O2 179.0(2) . . ? O1 U O23 88.3(2) . 1_655 ? O2 U O23 91.86(19) . 1_655 ? O1 U O7 90.0(2) . 1_655 ? O2 U O7 90.9(2) . 1_655 ? O23 U O7 78.25(18) 1_655 1_655 ? O1 U O19 91.7(2) . . ? O2 U O19 87.4(2) . . ? O23 U O19 78.63(17) 1_655 . ? O7 U O19 156.76(18) 1_655 . ? O1 U O4 93.1(2) . . ? O2 U O4 86.30(19) . . ? O23 U O4 151.80(16) 1_655 . ? O7 U O4 129.87(17) 1_655 . ? O19 U O4 73.18(16) . . ? O1 U O3 85.8(2) . . ? O2 U O3 94.48(19) . . ? O23 U O3 151.75(16) 1_655 . ? O7 U O3 74.15(16) 1_655 . ? O19 U O3 129.09(16) . . ? O4 U O3 56.27(15) . . ? O41A Eu1 O31 148.8(5) . . ? O39B Eu1 O31 100.0(5) . . ? O41A Eu1 O37 72.0(5) . . ? O39B Eu1 O37 145.2(4) . . ? O31 Eu1 O37 77.8(3) . . ? O41A Eu1 O36 82.5(4) . . ? O39B Eu1 O36 74.1(4) . . ? O31 Eu1 O36 80.4(3) . . ? O37 Eu1 O36 71.3(4) . . ? O41A Eu1 O39A 73.0(7) . . ? O31 Eu1 O39A 129.9(6) . . ? O37 Eu1 O39A 138.6(7) . . ? O36 Eu1 O39A 82.9(5) . . ? O41A Eu1 O38 64.5(5) . . ? O39B Eu1 O38 89.1(5) . . ? O31 Eu1 O38 139.3(3) . . ? O37 Eu1 O38 115.4(4) . . ? O36 Eu1 O38 139.7(4) . . ? O39A Eu1 O38 66.4(5) . . ? O41A Eu1 O35 137.4(5) . . ? O39B Eu1 O35 67.9(4) . . ? O31 Eu1 O35 72.9(3) . . ? O37 Eu1 O35 140.0(4) . . ? O36 Eu1 O35 128.0(4) . . ? O39A Eu1 O35 81.4(7) . . ? O38 Eu1 O35 74.3(4) . . ? O39B Eu1 O41B 77.3(6) . . ? O31 Eu1 O41B 146.4(4) . . ? O37 Eu1 O41B 85.8(5) . . ? O36 Eu1 O41B 66.5(5) . . ? O38 Eu1 O41B 74.3(5) . . ? O35 Eu1 O41B 132.8(4) . . ? O39B Eu1 O40B 153.4(4) . . ? O31 Eu1 O40B 88.7(3) . . ? O37 Eu1 O40B 61.2(4) . . ? O36 Eu1 O40B 132.4(4) . . ? O38 Eu1 O40B 68.7(4) . . ? O35 Eu1 O40B 91.2(4) . . ? O41B Eu1 O40B 108.8(5) . . ? O41A Eu1 O40A 110.4(5) . . ? O31 Eu1 O40A 71.7(3) . . ? O37 Eu1 O40A 80.9(4) . . ? O36 Eu1 O40A 144.1(3) . . ? O39A Eu1 O40A 132.5(6) . . ? O38 Eu1 O40A 72.9(4) . . ? O35 Eu1 O40A 64.4(4) . . ? O42 Eu2 O49 141.2(3) . . ? O42 Eu2 O45B 84.4(4) . . ? O49 Eu2 O45B 86.6(4) . . ? O42 Eu2 O48 137.6(3) . . ? O49 Eu2 O48 71.6(2) . . ? O45B Eu2 O48 132.7(3) . . ? O42 Eu2 O43 76.0(3) . . ? O49 Eu2 O43 142.3(2) . . ? O45B Eu2 O43 107.4(4) . . ? O48 Eu2 O43 73.5(2) . . ? O42 Eu2 O47 76.7(3) . . ? O49 Eu2 O47 101.7(2) . . ? O45B Eu2 O47 158.6(3) . . ? O48 Eu2 O47 68.7(2) . . ? O43 Eu2 O47 78.1(2) . . ? O42 Eu2 O46 72.7(4) . . ? O49 Eu2 O46 70.0(3) . . ? O45B Eu2 O46 91.8(4) . . ? O48 Eu2 O46 117.2(3) . . ? O43 Eu2 O46 141.3(3) . . ? O47 Eu2 O46 73.0(3) . . ? O42 Eu2 O44 130.9(4) . . ? O49 Eu2 O44 77.2(2) . . ? O45B Eu2 O44 65.1(4) . . ? O48 Eu2 O44 69.3(3) . . ? O43 Eu2 O44 77.6(3) . . ? O47 Eu2 O44 135.8(3) . . ? O46 Eu2 O44 140.9(3) . . ? O42 Eu2 O50 56.9(5) . . ? O49 Eu2 O50 130.3(3) . . ? O48 Eu2 O50 131.4(4) . . ? O43 Eu2 O50 67.5(4) . . ? O47 Eu2 O50 126.9(4) . . ? O46 Eu2 O50 111.4(5) . . ? O44 Eu2 O50 74.9(4) . . ? O42 Eu2 O45A 80.2(3) . . ? O49 Eu2 O45A 72.8(3) . . ? O48 Eu2 O45A 141.8(3) . . ? O43 Eu2 O45A 134.6(3) . . ? O47 Eu2 O45A 132.6(3) . . ? O46 Eu2 O45A 60.7(4) . . ? O44 Eu2 O45A 90.0(4) . . ? O50 Eu2 O45A 67.1(4) . . ? O5 S1 O3 113.2(3) . . ? O5 S1 O4 114.8(3) . . ? O3 S1 O4 105.1(3) . . ? O5 S1 C3 108.6(3) . . ? O3 S1 C3 108.3(3) . . ? O4 S1 C3 106.4(3) . . ? O9 S2 O8 115.2(3) . . ? O9 S2 O7 111.1(3) . . ? O8 S2 O7 110.8(3) . . ? O9 S2 C10 106.8(3) . . ? O8 S2 C10 109.4(3) . . ? O7 S2 C10 102.8(3) . . ? O13B S3 O11B 119.2(6) . . ? O12A S3 O13A 115.4(5) . . ? O13B S3 O12B 107.4(6) . . ? O11B S3 O12B 104.2(6) . . ? O12A S3 O11A 108.6(5) . . ? O13A S3 O11A 102.3(5) . . ? O12A S3 C17 117.9(5) . . ? O13B S3 C17 112.6(5) . . ? O11B S3 C17 110.3(5) . . ? O13A S3 C17 107.4(4) . . ? O12B S3 C17 101.1(5) . . ? O11A S3 C17 103.3(4) . . ? O17B S4 O16B 115.7(13) . . ? O15A S4 O16A 114.3(6) . . ? O15A S4 O17A 111.2(5) . . ? O16A S4 O17A 110.9(6) . . ? O17B S4 O15B 112.1(13) . . ? O16B S4 O15B 108.4(12) . . ? O17B S4 C24 106.3(8) . . ? O15A S4 C24 106.5(4) . . ? O16B S4 C24 106.5(9) . . ? O16A S4 C24 106.6(4) . . ? O17A S4 C24 106.9(4) . . ? O15B S4 C24 107.3(7) . . ? O21 S5 O20 114.1(4) . . ? O21 S5 O19 113.3(3) . . ? O20 S5 O19 108.5(3) . . ? O21 S5 C31 107.4(3) . . ? O20 S5 C31 107.1(3) . . ? O19 S5 C31 106.1(3) . . ? O25 S6 O24 114.7(3) . . ? O25 S6 O23 111.2(3) . . ? O24 S6 O23 110.3(3) . . ? O25 S6 C38 109.0(3) . . ? O24 S6 C38 107.5(3) . . ? O23 S6 C38 103.5(3) . . ? O27 S7 O29 113.5(6) . . ? O27 S7 O28 116.5(7) . . ? O29 S7 O28 108.3(7) . . ? O27 S7 C45 105.4(4) . . ? O29 S7 C45 107.5(5) . . ? O28 S7 C45 104.8(5) . . ? O33 S8 O32 114.9(6) . . ? O33 S8 O31 110.6(4) . . ? O32 S8 O31 110.7(5) . . ? O33 S8 C52 107.2(4) . . ? O32 S8 C52 106.4(4) . . ? O31 S8 C52 106.5(3) . . ? S1 O3 U 98.1(2) . . ? S1 O4 U 99.4(2) . . ? C6 O6 H6 110.0 . . ? S2 O7 U 144.1(3) . 1_455 ? C13 O10 H10 109.0 . . ? C20 O14 H14 111.5 . . ? C27 O18 H18 105.3 . . ? S5 O19 U 152.1(3) . . ? C34 O22 H22 108.1 . . ? S6 O23 U 139.8(3) . 1_455 ? C41 O26 H26 109.9 . . ? C48 O30 H30 107.9 . . ? S8 O31 Eu1 163.7(4) . . ? C55 O34 H34 107.2 . . ? Eu2 O42 H42A 112.5 . . ? Eu2 O42 H42B 106.9 . . ? H42A O42 H42B 98.2 . . ? Eu2 O47 H47A 106.0 . . ? Eu2 O47 H47B 111.0 . . ? H47A O47 H47B 100.1 . . ? Eu2 O49 H49A 116.7 . . ? Eu2 O49 H49B 125.3 . . ? H49A O49 H49B 115.8 . . ? C2 C1 C6 118.6(6) . . ? C2 C1 C28 120.3(6) . . ? C6 C1 C28 121.1(6) . . ? C1 C2 C3 120.5(6) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 120.8(6) . . ? C2 C3 S1 119.7(5) . . ? C4 C3 S1 119.5(5) . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 118.2(6) . . ? C4 C5 C7 119.0(6) . . ? C6 C5 C7 122.7(6) . . ? O6 C6 C5 120.8(6) . . ? O6 C6 C1 117.4(6) . . ? C5 C6 C1 121.8(6) . . ? C5 C7 C8 112.9(5) . . ? C5 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C5 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C13 C8 C9 118.9(5) . . ? C13 C8 C7 121.0(6) . . ? C9 C8 C7 120.0(6) . . ? C10 C9 C8 119.3(6) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 121.3(6) . . ? C9 C10 S2 119.6(5) . . ? C11 C10 S2 119.0(5) . . ? C12 C11 C10 120.1(6) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 118.3(6) . . ? C11 C12 C14 118.8(6) . . ? C13 C12 C14 122.9(6) . . ? O10 C13 C8 116.8(6) . . ? O10 C13 C12 121.3(6) . . ? C8 C13 C12 121.9(6) . . ? C12 C14 C15 109.8(5) . . ? C12 C14 H14A 109.7 . . ? C15 C14 H14A 109.7 . . ? C12 C14 H14B 109.7 . . ? C15 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C20 118.4(6) . . ? C16 C15 C14 119.6(6) . . ? C20 C15 C14 122.0(6) . . ? C15 C16 C17 120.3(6) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.4(6) . . ? C18 C17 S3 120.0(5) . . ? C16 C17 S3 119.5(5) . . ? C17 C18 C19 120.5(6) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C18 118.1(7) . . ? C20 C19 C21 122.4(7) . . ? C18 C19 C21 119.4(7) . . ? O14 C20 C19 121.5(7) . . ? O14 C20 C15 116.2(6) . . ? C19 C20 C15 122.2(7) . . ? C19 C21 C22 112.7(5) . . ? C19 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C19 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C27 119.1(6) . . ? C23 C22 C21 120.3(7) . . ? C27 C22 C21 120.6(6) . . ? C22 C23 C24 119.5(7) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 121.4(7) . . ? C25 C24 S4 120.5(5) . . ? C23 C24 S4 118.0(5) . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 118.1(7) . . ? C25 C26 C28 119.9(6) . . ? C27 C26 C28 122.0(7) . . ? O18 C27 C26 121.0(7) . . ? O18 C27 C22 117.3(6) . . ? C26 C27 C22 121.6(6) . . ? C1 C28 C26 112.6(6) . . ? C1 C28 H28A 109.1 . . ? C26 C28 H28A 109.1 . . ? C1 C28 H28B 109.1 . . ? C26 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C34 C29 C30 118.6(6) . . ? C34 C29 C56 123.0(6) . . ? C30 C29 C56 118.4(6) . . ? C31 C30 C29 119.5(6) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C32 C31 C30 121.4(6) . . ? C32 C31 S5 118.7(5) . . ? C30 C31 S5 119.9(5) . . ? C33 C32 C31 120.6(6) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 117.5(6) . . ? C32 C33 C35 120.1(6) . . ? C34 C33 C35 122.4(6) . . ? O22 C34 C29 121.3(6) . . ? O22 C34 C33 116.3(6) . . ? C29 C34 C33 122.4(6) . . ? C33 C35 C36 112.4(6) . . ? C33 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? C33 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C41 118.1(7) . . ? C37 C36 C35 120.4(6) . . ? C41 C36 C35 121.5(6) . . ? C38 C37 C36 120.1(6) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 121.5(6) . . ? C37 C38 S6 119.8(5) . . ? C39 C38 S6 118.6(6) . . ? C40 C39 C38 120.1(7) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 118.2(6) . . ? C39 C40 C42 120.9(7) . . ? C41 C40 C42 120.9(7) . . ? O26 C41 C36 121.4(7) . . ? O26 C41 C40 116.7(6) . . ? C36 C41 C40 121.9(6) . . ? C40 C42 C43 110.9(6) . . ? C40 C42 H42C 109.5 . . ? C43 C42 H42C 109.5 . . ? C40 C42 H42D 109.5 . . ? C43 C42 H42D 109.5 . . ? H42C C42 H42D 108.0 . . ? C48 C43 C44 117.6(8) . . ? C48 C43 C42 123.3(9) . . ? C44 C43 C42 119.1(7) . . ? C45 C44 C43 120.8(7) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 120.6(9) . . ? C44 C45 S7 120.3(6) . . ? C46 C45 S7 119.0(7) . . ? C45 C46 C47 120.0(8) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 118.5(7) . . ? C48 C47 C49 123.0(8) . . ? C46 C47 C49 118.3(7) . . ? O30 C48 C47 117.2(6) . . ? O30 C48 C43 120.4(7) . . ? C47 C48 C43 122.4(8) . . ? C50 C49 C47 108.8(5) . . ? C50 C49 H49C 109.9 . . ? C47 C49 H49C 109.9 . . ? C50 C49 H49D 109.9 . . ? C47 C49 H49D 109.9 . . ? H49C C49 H49D 108.3 . . ? C55 C50 C51 118.9(6) . . ? C55 C50 C49 121.2(6) . . ? C51 C50 C49 119.8(6) . . ? C52 C51 C50 119.6(6) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C53 120.9(6) . . ? C51 C52 S8 120.0(5) . . ? C53 C52 S8 119.1(5) . . ? C54 C53 C52 120.5(6) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 117.8(6) . . ? C53 C54 C56 120.9(6) . . ? C55 C54 C56 121.2(6) . . ? O34 C55 C50 121.4(6) . . ? O34 C55 C54 116.3(6) . . ? C50 C55 C54 122.2(6) . . ? C54 C56 C29 112.9(5) . . ? C54 C56 H56A 109.0 . . ? C29 C56 H56A 109.0 . . ? C54 C56 H56B 109.0 . . ? C29 C56 H56B 109.0 . . ? H56A C56 H56B 107.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 O10 0.90 1.78 2.674(7) 171.1 . O10 H10 O14 0.92 1.93 2.804(8) 158.0 . O14 H14 O18 0.88 1.89 2.685(8) 149.5 . O18 H18 O6 0.97 1.76 2.680(8) 158.1 . O22 H22 O34 0.82 1.87 2.678(7) 171.7 . O26 H26 O22 0.88 1.84 2.667(7) 157.0 . O30 H30 O26 0.94 1.83 2.739(8) 162.2 . O34 H34 O30 0.97 1.78 2.740(7) 166.3 . O42 H42A O20 0.99 2.08 2.797(12) 127.9 2_667 O42 H42B O52 0.89 2.25 3.000(15) 141.5 . O47 H47A O8 0.87 2.13 2.888(8) 145.4 2_667 O47 H47B O61 0.96 1.92 2.783(9) 148.7 . O49 H49A O54 0.92 1.84 2.746(8) 169.7 . O49 H49B O65 0.89 2.10 2.913(15) 150.8 .