Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Pierre Thuery' 'Bernardo Masci' _publ_contact_author_name 'Pierre Thuery ' _publ_contact_author_address ; Service de Chimie Moleculaire DSM DRECAM, CNRA URA 331 CEA Saclay Bat 125 Gif-sur-Yvette 91191 FRANCE ; _publ_contact_author_email THUERY@DRECAM.CEA.FR _publ_requested_journal CrystEngComm _publ_section_title ; Versatility of {M(30-crown-10)} (M = K+, Ba2+) as a guest in UO22+ complexes of [3.1.3.1]- and [3.3.3]homooxacalixarenes ; data_1 _database_code_depnum_ccdc_archive 'CCDC 638697' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H103 Ba Cl9 O20 U' _chemical_formula_weight 1946.93 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' Ba Ba -0.3244 2.2819 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 25.5120(5) _cell_length_b 25.5120(5) _cell_length_c 12.9978(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8459.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 134219 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method ? _exptl_crystal_F_000 3912 _exptl_absorpt_coefficient_mu 2.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.804 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 50 mm' _diffrn_ambient_temperature 100(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 'one \f and five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 134219 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8005 _reflns_number_gt 7051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Two positions of the water solvent molecule (O11 and O12) have been refined with occupancy parameters constrained to sum to unity. One of the solvent chloroform molecules is also disordered over two positions. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some atoms of the solvent molecules. The H atoms bound to the water O atoms were not found. All other H atoms were introduced at calculated positions, except that of the disordered chloroform molecule. All were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0874P)^2^+10.9194P] 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 0.011(6) _refine_ls_number_reflns 8005 _refine_ls_number_parameters 479 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.007 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.127 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 0.139333(8) 0.139333(8) 0.0000 0.02673(11) Uani 1 2 d S . . Ba Ba 0.343652(15) 0.343652(15) 0.0000 0.04109(17) Uani 1 2 d S . . O1 O 0.08835(19) 0.18910(18) 0.1083(4) 0.0317(11) Uani 1 1 d . . . O2 O 0.09693(18) 0.17863(18) -0.1301(4) 0.0311(10) Uani 1 1 d . . . O3 O 0.19442(17) 0.17532(18) -0.2779(4) 0.0342(12) Uani 1 1 d . . . O4 O 0.08929(17) 0.08929(17) 0.0000 0.0361(14) Uani 1 2 d S . . O5 O 0.18919(16) 0.18919(16) 0.0000 0.0305(13) Uani 1 2 d S . . O6 O 0.3852(3) 0.4304(3) 0.1171(6) 0.0661(18) Uani 1 1 d . . . O7 O 0.3240(3) 0.3572(3) 0.2189(5) 0.0733(19) Uani 1 1 d . . . O8 O 0.2966(3) 0.2663(3) 0.1276(6) 0.075(2) Uani 1 1 d . . . O9 O 0.3734(3) 0.2370(2) -0.0102(6) 0.0701(18) Uani 1 1 d . . . O10 O 0.4467(2) 0.3144(3) 0.0496(5) 0.0647(17) Uani 1 1 d . . . O11 O 0.0055(4) 0.1402(4) 0.1936(8) 0.060(3) Uani 0.642(16) 1 d PU . . O12 O 0.0402(5) 0.1254(5) 0.2488(12) 0.035(4) Uani 0.358(16) 1 d PU . . C1 C 0.1106(3) 0.2565(3) 0.2293(6) 0.0346(17) Uani 1 1 d . . . C2 C 0.0903(3) 0.2400(3) 0.1315(5) 0.0285(15) Uani 1 1 d . . . C3 C 0.0705(3) 0.2790(2) 0.0654(6) 0.0302(16) Uani 1 1 d . . . C4 C 0.0722(3) 0.3311(3) 0.0931(5) 0.0314(15) Uani 1 1 d . . . H4 H 0.0589 0.3558 0.0476 0.038 Uiso 1 1 calc R . . C5 C 0.0930(2) 0.3483(2) 0.1869(5) 0.0288(15) Uani 1 1 d . . . C6 C 0.1111(3) 0.3092(3) 0.2514(7) 0.0346(15) Uani 1 1 d . . . H6 H 0.1246 0.3193 0.3148 0.042 Uiso 1 1 calc R . . C7 C 0.0914(3) 0.4058(3) 0.2204(6) 0.0381(18) Uani 1 1 d . . . C8 C 0.0841(4) 0.4437(3) 0.1299(7) 0.052(2) Uani 1 1 d . . . H8A H 0.0520 0.4355 0.0945 0.078 Uiso 1 1 calc R . . H8B H 0.1130 0.4403 0.0833 0.078 Uiso 1 1 calc R . . H8C H 0.0825 0.4790 0.1552 0.078 Uiso 1 1 calc R . . C9 C 0.0451(3) 0.4126(3) 0.2950(7) 0.053(2) Uani 1 1 d . . . H9A H 0.0135 0.4003 0.2628 0.079 Uiso 1 1 calc R . . H9B H 0.0413 0.4490 0.3122 0.079 Uiso 1 1 calc R . . H9C H 0.0515 0.3928 0.3564 0.079 Uiso 1 1 calc R . . C10 C 0.1411(3) 0.4205(3) 0.2774(7) 0.053(2) Uani 1 1 d . . . H10A H 0.1384 0.4561 0.3012 0.079 Uiso 1 1 calc R . . H10B H 0.1706 0.4173 0.2320 0.079 Uiso 1 1 calc R . . H10C H 0.1456 0.3976 0.3353 0.079 Uiso 1 1 calc R . . C11 C 0.0420(3) 0.2628(3) -0.0325(5) 0.0309(16) Uani 1 1 d . . . H11A H 0.0100 0.2832 -0.0372 0.037 Uiso 1 1 calc R . . H11B H 0.0319 0.2263 -0.0257 0.037 Uiso 1 1 calc R . . C12 C 0.0716(3) 0.2689(3) -0.1330(6) 0.0329(16) Uani 1 1 d . . . C13 C 0.0965(2) 0.2258(3) -0.1788(6) 0.0281(15) Uani 1 1 d . . . C14 C 0.1186(3) 0.2306(3) -0.2752(5) 0.0290(16) Uani 1 1 d . . . C15 C 0.1181(3) 0.2797(3) -0.3275(6) 0.0356(16) Uani 1 1 d . . . H15 H 0.1342 0.2832 -0.3913 0.043 Uiso 1 1 calc R . . C16 C 0.0929(3) 0.3228(3) -0.2818(5) 0.0327(17) Uani 1 1 d . . . C17 C 0.0705(3) 0.3159(3) -0.1879(6) 0.0352(17) Uani 1 1 d . . . H17 H 0.0533 0.3443 -0.1584 0.042 Uiso 1 1 calc R . . C18 C 0.0909(3) 0.3760(3) -0.3365(6) 0.0386(17) Uani 1 1 d . . . C19 C 0.1111(5) 0.4192(4) -0.2750(9) 0.085(4) Uani 1 1 d . . . H19A H 0.1058 0.4516 -0.3111 0.128 Uiso 1 1 calc R . . H19B H 0.1479 0.4141 -0.2631 0.128 Uiso 1 1 calc R . . H19C H 0.0930 0.4203 -0.2103 0.128 Uiso 1 1 calc R . . C20 C 0.1202(4) 0.3745(4) -0.4427(8) 0.072(3) Uani 1 1 d . . . H20A H 0.1052 0.4002 -0.4881 0.107 Uiso 1 1 calc R . . H20B H 0.1167 0.3403 -0.4727 0.107 Uiso 1 1 calc R . . H20C H 0.1567 0.3823 -0.4324 0.107 Uiso 1 1 calc R . . C21 C 0.0329(4) 0.3881(4) -0.3641(9) 0.071(3) Uani 1 1 d . . . H21A H 0.0119 0.3872 -0.3028 0.106 Uiso 1 1 calc R . . H21B H 0.0202 0.3624 -0.4119 0.106 Uiso 1 1 calc R . . H21C H 0.0306 0.4223 -0.3947 0.106 Uiso 1 1 calc R . . C22 C 0.1441(3) 0.1845(3) -0.3255(5) 0.0327(15) Uani 1 1 d . . . H22A H 0.1220 0.1538 -0.3179 0.039 Uiso 1 1 calc R . . H22B H 0.1486 0.1913 -0.3984 0.039 Uiso 1 1 calc R . . C23 C 0.2164(3) 0.1272(3) -0.3067(6) 0.0369(17) Uani 1 1 d . . . H23A H 0.2327 0.1305 -0.3738 0.044 Uiso 1 1 calc R . . H23B H 0.1891 0.1009 -0.3113 0.044 Uiso 1 1 calc R . . C24 C 0.3695(5) 0.4808(4) 0.0880(12) 0.086(4) Uani 1 1 d . . . H24A H 0.3985 0.5048 0.0984 0.103 Uiso 1 1 calc R . . H24B H 0.3410 0.4920 0.1325 0.103 Uiso 1 1 calc R . . C25 C 0.3860(5) 0.4245(6) 0.2220(9) 0.088(4) Uani 1 1 d . . . H25A H 0.3952 0.4577 0.2536 0.105 Uiso 1 1 calc R . . H25B H 0.4128 0.3992 0.2403 0.105 Uiso 1 1 calc R . . C26 C 0.3348(6) 0.4067(5) 0.2634(12) 0.103(5) Uani 1 1 d . . . H26A H 0.3364 0.4037 0.3377 0.123 Uiso 1 1 calc R . . H26B H 0.3075 0.4315 0.2457 0.123 Uiso 1 1 calc R . . C27 C 0.2753(4) 0.3355(4) 0.2490(11) 0.077(3) Uani 1 1 d . . . H27A H 0.2470 0.3510 0.2094 0.092 Uiso 1 1 calc R . . H27B H 0.2689 0.3422 0.3213 0.092 Uiso 1 1 calc R . . C28 C 0.2781(5) 0.2763(4) 0.2289(9) 0.083(3) Uani 1 1 d . . . H28A H 0.3014 0.2601 0.2785 0.100 Uiso 1 1 calc R . . H28B H 0.2435 0.2610 0.2374 0.100 Uiso 1 1 calc R . . C29 C 0.3049(6) 0.2121(4) 0.1140(11) 0.099(5) Uani 1 1 d . . . H29A H 0.2717 0.1935 0.1183 0.119 Uiso 1 1 calc R . . H29B H 0.3278 0.1989 0.1676 0.119 Uiso 1 1 calc R . . C30 C 0.3300(5) 0.2029(5) 0.0076(12) 0.097(4) Uani 1 1 d . . . H30A H 0.3417 0.1668 0.0029 0.116 Uiso 1 1 calc R . . H30B H 0.3039 0.2085 -0.0454 0.116 Uiso 1 1 calc R . . C31 C 0.4196(5) 0.2255(5) 0.0623(10) 0.090(4) Uani 1 1 d . . . H31A H 0.4317 0.1897 0.0540 0.108 Uiso 1 1 calc R . . H31B H 0.4096 0.2310 0.1335 0.108 Uiso 1 1 calc R . . C32 C 0.4635(4) 0.2661(4) 0.0282(8) 0.070(3) Uani 1 1 d . . . H32A H 0.4959 0.2590 0.0648 0.085 Uiso 1 1 calc R . . H32B H 0.4702 0.2628 -0.0450 0.085 Uiso 1 1 calc R . . C33 C 0.4844(4) 0.3522(6) 0.0190(10) 0.103(5) Uani 1 1 d . . . H33A H 0.5190 0.3377 0.0303 0.124 Uiso 1 1 calc R . . H33B H 0.4808 0.3827 0.0631 0.124 Uiso 1 1 calc R . . C34 C 0.4710(4) 0.2735(4) 0.4115(9) 0.068(3) Uani 1 1 d . . . H34 H 0.4913 0.3038 0.4355 0.082 Uiso 1 1 calc R . . C35 C 0.5649(11) 0.4324(9) 0.2970(15) 0.079(6) Uani 0.50 1 d P . . Cl1 Cl 0.41302(16) 0.29642(16) 0.3572(3) 0.1168(13) Uani 1 1 d U . . Cl2 Cl 0.50774(12) 0.24112(12) 0.3126(3) 0.0882(9) Uani 1 1 d U . . Cl3 Cl 0.46109(12) 0.23136(15) 0.5154(3) 0.0962(10) Uani 1 1 d U . . Cl4 Cl 0.5209(3) 0.4841(3) 0.2789(4) 0.0710(18) Uani 0.50 1 d PU . . Cl5 Cl 0.54642(13) 0.37346(11) 0.2496(3) 0.0859(8) Uani 1 1 d U . . 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 0.02098(12) 0.02098(12) 0.03822(18) -0.00176(12) 0.00176(12) -0.00131(12) Ba 0.02410(18) 0.02410(18) 0.0751(4) 0.0031(2) -0.0031(2) 0.0021(2) O1 0.029(3) 0.024(2) 0.042(3) 0.001(2) 0.009(2) 0.0009(19) O2 0.026(2) 0.029(3) 0.038(3) -0.004(2) -0.001(2) 0.0030(19) O3 0.024(2) 0.034(3) 0.045(3) -0.003(2) -0.0056(19) 0.005(2) O4 0.029(2) 0.029(2) 0.049(4) -0.004(3) 0.004(3) 0.000(3) O5 0.0285(19) 0.0285(19) 0.034(3) 0.001(2) -0.001(2) -0.001(2) O6 0.059(4) 0.049(4) 0.090(5) -0.011(4) 0.000(4) -0.004(3) O7 0.061(4) 0.072(5) 0.087(5) 0.013(4) 0.004(3) 0.006(3) O8 0.078(5) 0.054(4) 0.094(6) 0.026(4) -0.018(4) -0.019(3) O9 0.063(4) 0.044(3) 0.103(5) -0.002(4) -0.010(4) 0.003(3) O10 0.039(3) 0.074(5) 0.081(4) -0.011(4) 0.000(3) 0.006(3) O11 0.050(5) 0.072(5) 0.059(5) -0.004(4) 0.011(4) 0.000(4) O12 0.035(6) 0.040(6) 0.030(6) 0.004(4) 0.004(4) -0.002(4) C1 0.027(3) 0.032(4) 0.045(5) 0.002(3) 0.006(3) 0.003(3) C2 0.021(3) 0.030(4) 0.034(4) 0.001(3) 0.006(3) 0.000(3) C3 0.023(3) 0.021(3) 0.047(4) 0.000(3) 0.009(3) 0.000(3) C4 0.030(4) 0.025(3) 0.040(4) 0.002(3) 0.004(3) 0.000(3) C5 0.025(3) 0.021(3) 0.041(4) -0.005(3) 0.007(3) 0.000(3) C6 0.034(4) 0.035(4) 0.034(4) -0.003(4) 0.001(4) 0.006(3) C7 0.041(4) 0.025(4) 0.049(5) -0.006(3) 0.002(3) -0.004(3) C8 0.068(6) 0.022(4) 0.066(6) -0.007(4) 0.000(5) -0.006(4) C9 0.050(5) 0.027(4) 0.082(6) -0.018(4) 0.028(4) -0.002(3) C10 0.045(5) 0.051(5) 0.063(6) -0.010(4) -0.004(4) -0.012(4) C11 0.021(3) 0.030(4) 0.042(4) -0.001(3) 0.003(3) 0.003(3) C12 0.026(4) 0.034(4) 0.039(4) -0.014(3) -0.005(3) -0.003(3) C13 0.018(3) 0.028(4) 0.039(4) -0.004(3) -0.004(3) 0.000(3) C14 0.025(3) 0.031(4) 0.032(4) -0.005(3) -0.008(3) 0.006(3) C15 0.026(3) 0.039(4) 0.042(4) 0.000(3) -0.003(3) 0.004(3) C16 0.027(4) 0.029(4) 0.042(4) 0.002(3) -0.004(3) 0.003(3) C17 0.034(4) 0.023(4) 0.049(5) -0.007(3) -0.015(3) 0.006(3) C18 0.033(4) 0.030(4) 0.052(5) 0.005(3) -0.009(3) 0.001(3) C19 0.114(7) 0.060(5) 0.081(7) 0.013(5) -0.021(6) -0.018(5) C20 0.078(6) 0.054(5) 0.083(6) 0.023(4) 0.023(5) 0.011(4) C21 0.053(6) 0.071(7) 0.089(8) 0.034(6) -0.009(5) 0.012(5) C22 0.029(4) 0.037(4) 0.031(3) -0.003(3) -0.003(3) 0.002(3) C23 0.032(4) 0.045(5) 0.034(4) -0.001(3) -0.011(3) 0.012(3) C24 0.075(8) 0.046(6) 0.136(12) -0.004(6) 0.007(8) -0.009(5) C25 0.067(7) 0.124(11) 0.071(9) -0.031(7) 0.009(6) -0.023(7) C26 0.130(11) 0.067(7) 0.111(11) -0.021(8) 0.047(10) -0.014(7) C27 0.059(6) 0.067(6) 0.105(8) 0.020(7) 0.022(7) 0.006(5) C28 0.076(8) 0.068(7) 0.105(9) 0.047(7) 0.002(7) -0.008(5) C29 0.145(12) 0.039(6) 0.114(11) 0.019(6) -0.026(10) -0.040(7) C30 0.109(10) 0.069(7) 0.113(10) -0.003(8) -0.021(10) -0.029(7) C31 0.101(10) 0.087(9) 0.083(8) 0.001(7) -0.020(7) 0.046(8) C32 0.055(6) 0.081(7) 0.075(7) -0.011(6) -0.003(5) 0.033(6) C33 0.044(6) 0.167(14) 0.098(10) -0.062(10) 0.006(6) -0.027(7) C34 0.066(6) 0.053(6) 0.086(7) -0.020(5) -0.027(6) -0.002(5) C35 0.103(18) 0.065(14) 0.068(11) 0.016(12) 0.014(13) 0.020(11) Cl1 0.100(2) 0.114(3) 0.137(3) -0.015(2) -0.048(2) 0.047(2) Cl2 0.0774(18) 0.0768(18) 0.110(2) -0.0114(16) -0.0319(17) -0.0023(15) Cl3 0.0694(17) 0.110(2) 0.109(2) 0.009(2) -0.0234(18) -0.0092(16) Cl4 0.071(4) 0.052(3) 0.089(5) -0.001(4) 0.002(4) 0.011(2) Cl5 0.111(2) 0.0636(14) 0.0833(17) -0.0020(16) 0.019(2) 0.0107(14) _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 O5 1.799(6) . ? U O4 1.806(6) . ? U O2 2.244(5) . ? U O2 2.244(5) 7 ? U O1 2.299(4) . ? U O1 2.299(4) 7 ? Ba O10 2.809(6) . ? Ba O10 2.809(6) 7 ? Ba O9 2.828(6) 7 ? Ba O9 2.828(6) . ? Ba O8 2.844(7) 7 ? Ba O8 2.844(7) . ? Ba O6 2.889(6) . ? Ba O6 2.889(6) 7 ? Ba O7 2.910(7) 7 ? Ba O7 2.910(7) . ? O1 C2 1.335(8) . ? O1 O11 2.694(11) . ? O1 O12 2.737(14) . ? O2 C13 1.359(8) . ? O3 C23 1.400(9) . ? O3 C22 1.445(8) . ? O6 C25 1.373(13) . ? O6 C24 1.398(13) . ? O7 C26 1.416(13) . ? O7 C27 1.414(11) . ? O8 C29 1.411(13) . ? O8 C28 1.422(14) . ? O9 C30 1.427(13) . ? O9 C31 1.536(13) . ? O10 C32 1.334(11) . ? O10 C33 1.417(14) . ? C1 C6 1.374(10) . ? C1 C2 1.436(10) . ? C1 C23 1.496(10) 7 ? C2 C3 1.407(10) . ? C3 C4 1.377(9) . ? C3 C11 1.523(10) . ? C4 C5 1.401(10) . ? C5 C6 1.383(10) . ? C5 C7 1.530(9) . ? C7 C10 1.516(11) . ? C7 C8 1.534(11) . ? C7 C9 1.538(11) . ? C11 C12 1.517(10) . ? C12 C17 1.396(10) . ? C12 C13 1.403(10) . ? C13 C14 1.380(10) . ? C14 C15 1.427(10) . ? C14 C22 1.493(10) . ? C15 C16 1.404(10) . ? C16 C17 1.359(10) . ? C16 C18 1.532(10) . ? C18 C19 1.456(13) . ? C18 C21 1.555(11) . ? C18 C20 1.570(12) . ? C23 C1 1.496(10) 7 ? C24 C33 1.462(18) 7 ? C25 C26 1.484(17) . ? C27 C28 1.535(15) . ? C29 C30 1.542(19) . ? C31 C32 1.590(18) . ? C33 C24 1.462(18) 7 ? C34 Cl3 1.745(12) . ? C34 Cl1 1.739(10) . ? C34 Cl2 1.793(12) . ? C35 C35 1.23(4) 8_665 ? C35 Cl5 1.69(3) . ? C35 Cl4 1.75(2) . ? C35 Cl5 1.77(3) 8_665 ? C35 Cl4 1.99(2) 8_665 ? Cl4 Cl4 0.771(9) 8_665 ? Cl4 C35 1.99(2) 8_665 ? Cl5 C35 1.77(3) 8_665 ? 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 O5 U O4 180 . . ? O5 U O2 91.43(13) . . ? O4 U O2 88.57(13) . . ? O5 U O2 91.43(13) . 7 ? O4 U O2 88.57(13) . 7 ? O2 U O2 177.1(3) . 7 ? O5 U O1 90.55(12) . . ? O4 U O1 89.45(12) . . ? O2 U O1 86.68(17) . . ? O2 U O1 93.29(17) 7 . ? O5 U O1 90.55(12) . 7 ? O4 U O1 89.45(12) . 7 ? O2 U O1 93.29(17) . 7 ? O2 U O1 86.68(17) 7 7 ? O1 U O1 178.9(2) . 7 ? O10 Ba O10 123.3(3) . 7 ? O10 Ba O9 164.0(2) . 7 ? O10 Ba O9 60.27(19) 7 7 ? O10 Ba O9 60.26(19) . . ? O10 Ba O9 164.0(2) 7 . ? O9 Ba O9 121.3(3) 7 . ? O10 Ba O8 132.2(2) . 7 ? O10 Ba O8 94.4(2) 7 7 ? O9 Ba O8 58.2(2) 7 7 ? O9 Ba O8 75.7(2) . 7 ? O10 Ba O8 94.4(2) . . ? O10 Ba O8 132.2(2) 7 . ? O9 Ba O8 75.7(2) 7 . ? O9 Ba O8 58.2(2) . . ? O8 Ba O8 75.8(3) 7 . ? O10 Ba O6 74.85(19) . . ? O10 Ba O6 60.0(2) 7 . ? O9 Ba O6 97.1(2) 7 . ? O9 Ba O6 131.6(2) . . ? O8 Ba O6 152.3(2) 7 . ? O8 Ba O6 112.3(2) . . ? O10 Ba O6 60.0(2) . 7 ? O10 Ba O6 74.85(19) 7 7 ? O9 Ba O6 131.6(2) 7 7 ? O9 Ba O6 97.1(2) . 7 ? O8 Ba O6 112.3(2) 7 7 ? O8 Ba O6 152.3(2) . 7 ? O6 Ba O6 73.4(3) . 7 ? O10 Ba O7 93.9(2) . 7 ? O10 Ba O7 88.20(19) 7 7 ? O9 Ba O7 101.9(2) 7 7 ? O9 Ba O7 75.9(2) . 7 ? O8 Ba O7 55.9(2) 7 7 ? O8 Ba O7 120.0(2) . 7 ? O6 Ba O7 127.2(2) . 7 ? O6 Ba O7 57.1(2) 7 7 ? O10 Ba O7 88.20(19) . . ? O10 Ba O7 93.88(19) 7 . ? O9 Ba O7 75.9(2) 7 . ? O9 Ba O7 101.9(2) . . ? O8 Ba O7 120.0(2) 7 . ? O8 Ba O7 55.9(2) . . ? O6 Ba O7 57.1(2) . . ? O6 Ba O7 127.2(2) 7 . ? O7 Ba O7 175.6(3) 7 . ? C2 O1 U 130.8(4) . . ? C13 O2 U 138.6(4) . . ? C23 O3 C22 112.6(5) . . ? C25 O6 C24 112.0(10) . . ? C25 O6 Ba 116.3(7) . . ? C24 O6 Ba 117.2(7) . . ? C26 O7 C27 114.0(9) . . ? C26 O7 Ba 118.1(7) . . ? C27 O7 Ba 112.0(7) . . ? C29 O8 C28 110.0(9) . . ? C29 O8 Ba 123.0(8) . . ? C28 O8 Ba 123.8(6) . . ? C30 O9 C31 112.3(9) . . ? C30 O9 Ba 111.8(7) . . ? C31 O9 Ba 111.2(6) . . ? C32 O10 C33 110.6(9) . . ? C32 O10 Ba 119.8(6) . . ? C33 O10 Ba 112.9(7) . . ? C6 C1 C2 118.3(7) . . ? C6 C1 C23 121.7(7) . 7 ? C2 C1 C23 119.9(6) . 7 ? O1 C2 C3 122.4(6) . . ? O1 C2 C1 119.9(6) . . ? C3 C2 C1 117.6(6) . . ? C4 C3 C2 120.7(7) . . ? C4 C3 C11 119.6(6) . . ? C2 C3 C11 119.4(6) . . ? C3 C4 C5 122.8(7) . . ? C6 C5 C4 115.3(6) . . ? C6 C5 C7 121.9(7) . . ? C4 C5 C7 122.6(6) . . ? C1 C6 C5 125.2(8) . . ? C10 C7 C8 108.7(7) . . ? C10 C7 C5 110.8(6) . . ? C8 C7 C5 112.9(6) . . ? C10 C7 C9 107.8(7) . . ? C8 C7 C9 108.6(7) . . ? C5 C7 C9 108.0(6) . . ? C3 C11 C12 116.9(6) . . ? C17 C12 C13 117.7(7) . . ? C17 C12 C11 121.3(6) . . ? C13 C12 C11 120.7(6) . . ? O2 C13 C14 119.8(6) . . ? O2 C13 C12 120.0(6) . . ? C14 C13 C12 120.1(7) . . ? C13 C14 C15 120.4(6) . . ? C13 C14 C22 120.4(6) . . ? C15 C14 C22 119.1(6) . . ? C16 C15 C14 119.4(7) . . ? C17 C16 C15 118.0(7) . . ? C17 C16 C18 121.2(7) . . ? C15 C16 C18 120.8(6) . . ? C16 C17 C12 124.3(7) . . ? C19 C18 C16 113.7(7) . . ? C19 C18 C21 108.3(9) . . ? C16 C18 C21 108.4(6) . . ? C19 C18 C20 109.4(8) . . ? C16 C18 C20 111.8(6) . . ? C21 C18 C20 104.8(7) . . ? O3 C22 C14 109.1(5) . . ? O3 C23 C1 110.1(6) . 7 ? O6 C24 C33 113.6(10) . 7 ? O6 C25 C26 112.4(11) . . ? O7 C26 C25 107.3(10) . . ? O7 C27 C28 107.3(8) . . ? O8 C28 C27 110.4(8) . . ? O8 C29 C30 108.9(10) . . ? O9 C30 C29 112.1(10) . . ? O9 C31 C32 104.2(9) . . ? O10 C32 C31 108.5(8) . . ? O10 C33 C24 115.5(9) . 7 ? Cl3 C34 Cl1 113.5(7) . . ? Cl3 C34 Cl2 110.2(6) . . ? Cl1 C34 Cl2 108.0(6) . . ? Cl5 C35 Cl4 116.3(17) . . ? Cl5 C35 Cl5 113.2(11) . 8_665 ? Cl4 C35 Cl5 107.1(13) . 8_665 ? Cl5 C35 Cl4 101.9(10) 8_665 8_665 ? #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 638698' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H80 Ba O18 U' _chemical_formula_weight 1632.75 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' Ba Ba -0.3244 2.2819 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.3580(10) _cell_length_b 12.3410(9) _cell_length_c 23.8660(15) _cell_angle_alpha 90.00 _cell_angle_beta 114.062(4) _cell_angle_gamma 90.00 _cell_volume 6819.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 252644 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method ? _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 3.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 0.740 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 50 mm' _diffrn_ambient_temperature 100(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 'one \f and thirteen \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 252644 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12899 _reflns_number_gt 10382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on displacement parameters for some badly behaving atoms in one phenyl substituent and in the 30-crown-10 moiety. The badly resolved phenyl substituent was refined as an idealized hexagon and restraints were applied for two C-C bond lengths in the crown ether. The H atoms were introduced at calculated positions and 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^)+(0.0696P)^2^+64.3221P] 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 12899 _refine_ls_number_parameters 835 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.524 _refine_diff_density_min -1.348 _refine_diff_density_rms 0.307 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 0.751375(11) 0.68041(2) 0.257296(13) 0.02216(10) Uani 1 1 d . . . Ba Ba 0.74259(2) 1.05781(4) 0.26120(2) 0.03299(15) Uani 1 1 d . . . O1 O 0.8462(2) 0.6810(5) 0.3227(2) 0.0267(12) Uani 1 1 d . . . O2 O 0.7851(2) 0.6810(5) 0.1821(2) 0.0286(12) Uani 1 1 d . . . O3 O 0.6792(2) 0.5445(5) 0.0956(3) 0.0306(13) Uani 1 1 d . . . O4 O 0.6565(2) 0.6840(5) 0.1912(2) 0.0273(12) Uani 1 1 d . . . O5 O 0.7192(2) 0.6841(4) 0.3337(2) 0.0274(12) Uani 1 1 d . . . O6 O 0.8221(2) 0.5445(5) 0.4207(3) 0.0290(13) Uani 1 1 d . . . O7 O 0.7531(2) 0.8254(5) 0.2576(2) 0.0305(13) Uani 1 1 d . . . O8 O 0.7506(2) 0.5336(4) 0.2582(2) 0.0287(13) Uani 1 1 d . . . O9 O 0.8483(3) 0.9937(6) 0.2566(3) 0.0452(17) Uani 1 1 d . . . O10 O 0.8371(3) 0.9861(7) 0.3693(4) 0.064(2) Uani 1 1 d . . . O11 O 0.7302(3) 0.9891(6) 0.3719(3) 0.0505(18) Uani 1 1 d . . . O12 O 0.7335(3) 1.2099(6) 0.3485(4) 0.0566(19) Uani 1 1 d . . . O13 O 0.8337(3) 1.2184(6) 0.3241(3) 0.0530(18) Uani 1 1 d . . . O14 O 0.7692(3) 1.2344(6) 0.1982(4) 0.056(2) Uani 1 1 d . . . O15 O 0.6581(3) 1.2216(6) 0.1976(3) 0.0504(18) Uani 1 1 d . . . O16 O 0.6235(3) 1.0584(6) 0.2498(3) 0.0515(18) Uani 1 1 d . . . O17 O 0.6498(3) 0.9478(6) 0.1650(3) 0.061(2) Uani 1 1 d . . . O18 O 0.7433(4) 1.0109(6) 0.1432(3) 0.056(2) Uani 1 1 d . . . C1 C 0.9054(3) 0.5589(7) 0.3995(4) 0.0270(18) Uani 1 1 d . . . C2 C 0.8888(3) 0.6083(7) 0.3417(4) 0.0268(18) Uani 1 1 d . . . C3 C 0.9196(3) 0.5823(7) 0.3057(3) 0.0255(17) Uani 1 1 d . . . C4 C 0.9618(3) 0.5028(7) 0.3260(4) 0.0283(18) Uani 1 1 d . . . H4 H 0.9819 0.4862 0.3020 0.034 Uiso 1 1 calc R . . C5 C 0.9754(3) 0.4468(7) 0.3809(4) 0.0297(19) Uani 1 1 d . . . C6 C 0.9478(3) 0.4794(7) 0.4177(4) 0.0274(18) Uani 1 1 d . . . H6 H 0.9581 0.4469 0.4558 0.033 Uiso 1 1 calc R . . C7 C 1.0173(4) 0.3565(8) 0.3987(4) 0.034(2) Uani 1 1 d . . . C8 C 1.0671(4) 0.3595(9) 0.3870(4) 0.040(2) Uani 1 1 d . . . H8 H 1.0737 0.4195 0.3672 0.048 Uiso 1 1 calc R . . C9 C 1.1071(5) 0.2750(10) 0.4042(4) 0.049(3) Uani 1 1 d . . . H9 H 1.1403 0.2797 0.3967 0.059 Uiso 1 1 calc R . . C10 C 1.0973(5) 0.1848(9) 0.4322(5) 0.055(3) Uani 1 1 d . . . H10 H 1.1235 0.1276 0.4435 0.065 Uiso 1 1 calc R . . C11 C 1.0479(5) 0.1800(9) 0.4436(5) 0.055(3) Uani 1 1 d . . . H11 H 1.0412 0.1190 0.4626 0.066 Uiso 1 1 calc R . . C12 C 1.0087(4) 0.2638(8) 0.4274(4) 0.042(2) Uani 1 1 d . . . H12 H 0.9759 0.2585 0.4357 0.050 Uiso 1 1 calc R . . C13 C 0.9079(3) 0.6408(7) 0.2463(4) 0.0274(18) Uani 1 1 d . . . H13A H 0.9443 0.6544 0.2433 0.033 Uiso 1 1 calc R . . H13B H 0.8905 0.7104 0.2471 0.033 Uiso 1 1 calc R . . C14 C 0.8683(3) 0.5789(7) 0.1893(4) 0.0260(17) Uani 1 1 d . . . C15 C 0.8087(4) 0.6054(7) 0.1594(4) 0.0285(18) Uani 1 1 d . . . C16 C 0.7761(3) 0.5521(7) 0.1036(4) 0.0281(18) Uani 1 1 d . . . C17 C 0.8000(4) 0.4702(7) 0.0826(4) 0.0300(19) Uani 1 1 d . . . H17 H 0.7769 0.4343 0.0467 0.036 Uiso 1 1 calc R . . C18 C 0.8577(4) 0.4391(7) 0.1134(4) 0.0306(19) Uani 1 1 d . . . C19 C 0.8909(3) 0.4973(7) 0.1660(4) 0.0289(18) Uani 1 1 d . . . H19 H 0.9299 0.4806 0.1864 0.035 Uiso 1 1 calc R . . C20 C 0.8827(4) 0.3477(8) 0.0913(4) 0.036(2) Uani 1 1 d . . . C21 C 0.9410(4) 0.3498(8) 0.0994(4) 0.041(2) Uani 1 1 d . . . H21 H 0.9636 0.4103 0.1169 0.049 Uiso 1 1 calc R . . C22 C 0.9648(5) 0.2624(11) 0.0816(5) 0.059(3) Uani 1 1 d . . . H22 H 1.0034 0.2648 0.0875 0.071 Uiso 1 1 calc R . . C23 C 0.9326(5) 0.1724(9) 0.0553(5) 0.055(3) Uani 1 1 d . . . H23 H 0.9490 0.1144 0.0432 0.065 Uiso 1 1 calc R . . C24 C 0.8756(5) 0.1689(9) 0.0469(5) 0.056(3) Uani 1 1 d . . . H24 H 0.8534 0.1082 0.0289 0.067 Uiso 1 1 calc R . . C25 C 0.8508(5) 0.2553(8) 0.0651(4) 0.044(2) Uani 1 1 d . . . H25 H 0.8124 0.2511 0.0597 0.053 Uiso 1 1 calc R . . C26 C 0.7152(4) 0.5884(7) 0.0677(4) 0.0318(19) Uani 1 1 d . . . H26A H 0.7133 0.6669 0.0674 0.038 Uiso 1 1 calc R . . H26B H 0.7019 0.5634 0.0256 0.038 Uiso 1 1 calc R . . C27 C 0.6244(3) 0.5966(8) 0.0733(4) 0.0316(19) Uani 1 1 d . . . H27A H 0.6015 0.5745 0.0313 0.038 Uiso 1 1 calc R . . H27B H 0.6294 0.6746 0.0739 0.038 Uiso 1 1 calc R . . C28 C 0.5947(3) 0.5656(7) 0.1131(4) 0.0294(18) Uani 1 1 d . . . C29 C 0.6137(3) 0.6143(7) 0.1722(4) 0.0281(18) Uani 1 1 d . . . C30 C 0.5819(3) 0.5883(7) 0.2078(4) 0.0310(19) Uani 1 1 d . . . C31 C 0.5378(3) 0.5137(7) 0.1872(4) 0.0307(19) Uani 1 1 d . . . H31 H 0.5185 0.4969 0.2119 0.037 Uiso 1 1 calc R . . C32 C 0.5209(4) 0.4623(8) 0.1306(4) 0.037(2) Uani 1 1 d . . . C33 C 0.5500(3) 0.4920(7) 0.0939(4) 0.0302(19) Uani 1 1 d . . . H33 H 0.5387 0.4609 0.0552 0.036 Uiso 1 1 calc R . . C34 C 0.4742(4) 0.3800(7) 0.1091(4) 0.036(2) Uani 1 1 d . . . C35 C 0.4241(4) 0.3909(9) 0.1200(4) 0.043(2) Uani 1 1 d . . . H35 H 0.4202 0.4505 0.1419 0.051 Uiso 1 1 calc R . . C36 C 0.3800(4) 0.3144(9) 0.0986(5) 0.050(3) Uani 1 1 d . . . H36 H 0.3471 0.3233 0.1061 0.060 Uiso 1 1 calc R . . C37 C 0.3851(5) 0.2270(10) 0.0669(4) 0.050(3) Uani 1 1 d . . . H37 H 0.3552 0.1768 0.0522 0.060 Uiso 1 1 calc R . . C38 C 0.4338(5) 0.2112(9) 0.0562(4) 0.050(3) Uani 1 1 d . . . H38 H 0.4373 0.1499 0.0353 0.060 Uiso 1 1 calc R . . C39 C 0.4785(4) 0.2890(8) 0.0771(4) 0.043(2) Uani 1 1 d . . . H39 H 0.5113 0.2791 0.0694 0.052 Uiso 1 1 calc R . . C40 C 0.5966(3) 0.6461(8) 0.2683(4) 0.0316(19) Uani 1 1 d . . . H40A H 0.5610 0.6632 0.2723 0.038 Uiso 1 1 calc R . . H40B H 0.6154 0.7141 0.2673 0.038 Uiso 1 1 calc R . . C41 C 0.6356(3) 0.5830(7) 0.3251(4) 0.0291(18) Uani 1 1 d . . . C42 C 0.6947(3) 0.6101(7) 0.3562(4) 0.0268(18) Uani 1 1 d . . . C43 C 0.7264(3) 0.5603(7) 0.4131(4) 0.0257(17) Uani 1 1 d . . . C44 C 0.7014(3) 0.4820(7) 0.4354(4) 0.0296(18) Uani 1 1 d . . . H44 H 0.7232 0.4505 0.4732 0.036 Uiso 1 1 calc R . . C45 C 0.6444(4) 0.4483(7) 0.4032(4) 0.033(2) Uani 1 1 d . . . C46 C 0.6126(4) 0.5028(7) 0.3483(4) 0.032(2) Uani 1 1 d . . . H46 H 0.5740 0.4839 0.3266 0.038 Uiso 1 1 calc R . . C47 C 0.6172(3) 0.3595(6) 0.4262(4) 0.045(3) Uani 1 1 d G . . C48 C 0.6453(4) 0.3171(9) 0.4849(4) 0.150(6) Uani 1 1 d GU . . H48 H 0.6802 0.3467 0.5118 0.180 Uiso 1 1 calc R . . C49 C 0.6213(5) 0.2304(10) 0.5035(4) 0.150(5) Uani 1 1 d GU . . H49 H 0.6401 0.2020 0.5428 0.180 Uiso 1 1 calc R . . C50 C 0.5691(5) 0.1861(8) 0.4633(5) 0.121(4) Uani 1 1 d GU . . H50 H 0.5531 0.1281 0.4757 0.145 Uiso 1 1 calc R . . C51 C 0.5410(4) 0.2286(8) 0.4046(5) 0.104(4) Uani 1 1 d GU . . H51 H 0.5061 0.1989 0.3777 0.125 Uiso 1 1 calc R . . C52 C 0.5650(4) 0.3152(8) 0.3860(3) 0.094(4) Uani 1 1 d GU . . H52 H 0.5462 0.3436 0.3467 0.113 Uiso 1 1 calc R . . C53 C 0.7881(3) 0.5948(7) 0.4486(4) 0.0276(18) Uani 1 1 d . . . H53A H 0.7914 0.6730 0.4475 0.033 Uiso 1 1 calc R . . H53B H 0.8014 0.5724 0.4911 0.033 Uiso 1 1 calc R . . C54 C 0.8777(3) 0.5942(8) 0.4410(4) 0.0290(18) Uani 1 1 d . . . H54A H 0.9013 0.5726 0.4829 0.035 Uiso 1 1 calc R . . H54B H 0.8737 0.6724 0.4399 0.035 Uiso 1 1 calc R . . C55 C 0.8881(4) 0.9329(9) 0.3085(5) 0.048(3) Uani 1 1 d . . . H55A H 0.9260 0.9314 0.3075 0.058 Uiso 1 1 calc R . . H55B H 0.8747 0.8589 0.3068 0.058 Uiso 1 1 calc R . . C56 C 0.8916(4) 0.9857(11) 0.3653(5) 0.059(3) Uani 1 1 d . . . H56A H 0.9195 0.9477 0.4005 0.071 Uiso 1 1 calc R . . H56B H 0.9049 1.0597 0.3665 0.071 Uiso 1 1 calc R . . C57 C 0.8297(6) 0.9224(16) 0.4062(8) 0.107(5) Uani 1 1 d DU . . H57A H 0.8622 0.9311 0.4455 0.128 Uiso 1 1 calc R . . H57B H 0.8317 0.8493 0.3922 0.128 Uiso 1 1 calc R . . C58 C 0.7756(5) 0.9311(11) 0.4169(6) 0.073(4) Uani 1 1 d DU . . H58A H 0.7620 0.8585 0.4193 0.087 Uiso 1 1 calc R . . H58B H 0.7850 0.9657 0.4563 0.087 Uiso 1 1 calc R . . C59 C 0.7035(6) 1.0670(10) 0.3952(6) 0.068(3) Uani 1 1 d U . . H59A H 0.7034 1.0411 0.4336 0.081 Uiso 1 1 calc R . . H59B H 0.6637 1.0767 0.3664 0.081 Uiso 1 1 calc R . . C60 C 0.7347(6) 1.1756(12) 0.4060(6) 0.079(4) Uani 1 1 d U . . H60A H 0.7155 1.2283 0.4213 0.094 Uiso 1 1 calc R . . H60B H 0.7743 1.1677 0.4359 0.094 Uiso 1 1 calc R . . C61 C 0.7652(5) 1.3061(11) 0.3541(7) 0.078(4) Uani 1 1 d DU . . H61A H 0.7628 1.3493 0.3869 0.094 Uiso 1 1 calc R . . H61B H 0.7472 1.3472 0.3164 0.094 Uiso 1 1 calc R . . C62 C 0.8276(5) 1.2895(13) 0.3669(7) 0.085(4) Uani 1 1 d DU . . H62A H 0.8450 1.3587 0.3652 0.102 Uiso 1 1 calc R . . H62B H 0.8476 1.2601 0.4079 0.102 Uiso 1 1 calc R . . C63 C 0.8584(5) 1.2612(11) 0.2842(5) 0.061(3) Uani 1 1 d U . . H63A H 0.8765 1.2031 0.2710 0.073 Uiso 1 1 calc R . . H63B H 0.8879 1.3141 0.3063 0.073 Uiso 1 1 calc R . . C64 C 0.8126(5) 1.3136(9) 0.2294(6) 0.060(3) Uani 1 1 d U . . H64A H 0.7956 1.3739 0.2422 0.072 Uiso 1 1 calc R . . H64B H 0.8293 1.3410 0.2021 0.072 Uiso 1 1 calc R . . C65 C 0.7206(5) 1.2803(10) 0.1520(5) 0.059(3) Uani 1 1 d . . . H65A H 0.7037 1.2280 0.1191 0.070 Uiso 1 1 calc R . . H65B H 0.7324 1.3428 0.1353 0.070 Uiso 1 1 calc R . . C66 C 0.6752(5) 1.3151(9) 0.1749(6) 0.059(3) Uani 1 1 d . . . H66A H 0.6912 1.3687 0.2072 0.071 Uiso 1 1 calc R . . H66B H 0.6422 1.3467 0.1416 0.071 Uiso 1 1 calc R . . C67 C 0.6181(5) 1.2439(9) 0.2247(6) 0.056(3) Uani 1 1 d . . . H67A H 0.5931 1.3039 0.2037 0.067 Uiso 1 1 calc R . . H67B H 0.6387 1.2631 0.2676 0.067 Uiso 1 1 calc R . . C68 C 0.5832(4) 1.1439(9) 0.2188(6) 0.058(3) Uani 1 1 d . . . H68A H 0.5561 1.1546 0.2375 0.069 Uiso 1 1 calc R . . H68B H 0.5617 1.1258 0.1759 0.069 Uiso 1 1 calc R . . C69 C 0.6031(6) 0.9513(10) 0.2320(7) 0.071(4) Uani 1 1 d . . . H69A H 0.5661 0.9425 0.2345 0.085 Uiso 1 1 calc R . . H69B H 0.6300 0.9004 0.2603 0.085 Uiso 1 1 calc R . . C70 C 0.5963(5) 0.9253(10) 0.1676(6) 0.064(3) Uani 1 1 d . . . H70A H 0.5862 0.8496 0.1583 0.076 Uiso 1 1 calc R . . H70B H 0.5660 0.9694 0.1381 0.076 Uiso 1 1 calc R . . C71 C 0.6504(5) 0.9329(10) 0.1066(5) 0.062(3) Uani 1 1 d U . . H71A H 0.6328 0.9950 0.0809 0.075 Uiso 1 1 calc R . . H71B H 0.6279 0.8692 0.0873 0.075 Uiso 1 1 calc R . . C72 C 0.7107(5) 0.9192(9) 0.1121(5) 0.059(3) Uani 1 1 d . . . H72A H 0.7274 0.8537 0.1348 0.071 Uiso 1 1 calc R . . H72B H 0.7109 0.9133 0.0716 0.071 Uiso 1 1 calc R . . C73 C 0.8002(6) 1.0105(10) 0.1460(6) 0.066(4) Uani 1 1 d . . . H73A H 0.8140 1.0846 0.1496 0.079 Uiso 1 1 calc R . . H73B H 0.7993 0.9813 0.1079 0.079 Uiso 1 1 calc R . . C74 C 0.8429(5) 0.9439(9) 0.1997(5) 0.058(3) Uani 1 1 d U . . H74A H 0.8290 0.8701 0.1976 0.070 Uiso 1 1 calc R . . H74B H 0.8802 0.9417 0.1976 0.070 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 0.02410(16) 0.01522(17) 0.02687(17) -0.00075(12) 0.01009(12) -0.00002(12) Ba 0.0386(3) 0.0208(3) 0.0338(3) -0.0005(2) 0.0088(2) 0.0001(2) O1 0.020(3) 0.027(3) 0.029(3) -0.003(2) 0.006(2) 0.002(2) O2 0.034(3) 0.026(3) 0.028(3) -0.002(2) 0.015(2) 0.001(3) O3 0.024(3) 0.030(3) 0.034(3) 0.006(3) 0.008(2) 0.003(2) O4 0.019(3) 0.025(3) 0.028(3) 0.000(2) 0.000(2) -0.002(2) O5 0.028(3) 0.023(3) 0.031(3) -0.001(2) 0.012(2) -0.003(2) O6 0.023(3) 0.032(3) 0.034(3) -0.006(3) 0.014(2) 0.000(2) O7 0.031(3) 0.030(4) 0.030(3) -0.002(2) 0.011(2) 0.003(2) O8 0.040(3) 0.004(2) 0.038(3) 0.003(2) 0.012(2) -0.003(2) O9 0.041(4) 0.045(4) 0.057(4) -0.001(3) 0.028(3) 0.003(3) O10 0.056(5) 0.080(6) 0.061(5) 0.030(4) 0.028(4) 0.018(4) O11 0.069(5) 0.036(4) 0.049(4) -0.001(3) 0.026(4) 0.000(4) O12 0.068(5) 0.035(4) 0.071(5) -0.004(4) 0.032(4) -0.005(4) O13 0.054(4) 0.044(4) 0.060(5) -0.011(4) 0.022(4) -0.014(4) O14 0.052(4) 0.031(4) 0.072(5) 0.010(4) 0.012(4) -0.001(3) O15 0.050(4) 0.031(4) 0.063(5) 0.009(3) 0.015(4) 0.009(3) O16 0.040(4) 0.051(5) 0.056(4) -0.004(4) 0.011(3) -0.001(3) O17 0.053(4) 0.054(5) 0.053(5) -0.013(4) -0.001(4) -0.006(4) O18 0.086(6) 0.039(4) 0.043(4) 0.000(3) 0.025(4) -0.001(4) C1 0.026(4) 0.028(5) 0.026(4) -0.002(3) 0.009(3) -0.005(3) C2 0.019(4) 0.020(4) 0.033(4) -0.002(3) 0.002(3) 0.001(3) C3 0.024(4) 0.030(5) 0.024(4) -0.005(3) 0.012(3) -0.009(3) C4 0.022(4) 0.027(5) 0.034(5) -0.007(4) 0.010(4) -0.006(3) C5 0.022(4) 0.033(5) 0.030(4) -0.001(4) 0.006(3) 0.004(4) C6 0.022(4) 0.034(5) 0.023(4) 0.002(3) 0.006(3) -0.004(4) C7 0.031(4) 0.038(5) 0.025(4) -0.007(4) 0.002(4) 0.002(4) C8 0.032(5) 0.050(6) 0.032(5) -0.009(4) 0.007(4) 0.007(4) C9 0.050(6) 0.058(7) 0.040(5) -0.007(5) 0.018(5) 0.021(5) C10 0.058(7) 0.053(7) 0.039(5) -0.013(5) 0.006(5) 0.029(6) C11 0.060(7) 0.039(6) 0.045(6) -0.005(5) 0.001(5) 0.006(5) C12 0.039(5) 0.042(6) 0.034(5) -0.002(4) 0.005(4) 0.002(4) C13 0.025(4) 0.028(5) 0.033(4) -0.002(4) 0.015(3) -0.004(3) C14 0.029(4) 0.022(4) 0.030(4) 0.000(3) 0.015(3) -0.004(3) C15 0.034(4) 0.026(5) 0.028(4) 0.002(3) 0.016(4) -0.004(4) C16 0.027(4) 0.034(5) 0.024(4) -0.003(3) 0.011(3) -0.004(4) C17 0.033(4) 0.033(5) 0.024(4) -0.003(4) 0.012(4) -0.004(4) C18 0.035(4) 0.025(5) 0.033(5) 0.006(4) 0.016(4) 0.006(4) C19 0.027(4) 0.031(5) 0.030(5) 0.004(3) 0.013(4) 0.001(4) C20 0.043(5) 0.032(5) 0.030(5) 0.002(4) 0.014(4) 0.011(4) C21 0.039(5) 0.044(6) 0.042(5) -0.005(4) 0.019(4) 0.003(4) C22 0.054(6) 0.082(9) 0.042(6) 0.004(6) 0.021(5) 0.029(6) C23 0.073(8) 0.049(7) 0.044(6) -0.002(5) 0.025(5) 0.027(6) C24 0.082(8) 0.035(6) 0.048(6) -0.007(5) 0.025(6) 0.009(6) C25 0.056(6) 0.033(6) 0.046(6) -0.002(4) 0.025(5) 0.002(5) C26 0.036(5) 0.026(5) 0.032(5) 0.000(4) 0.012(4) -0.002(4) C27 0.027(4) 0.034(5) 0.029(4) -0.002(4) 0.006(3) 0.004(4) C28 0.026(4) 0.026(5) 0.030(4) 0.002(3) 0.006(3) 0.002(4) C29 0.025(4) 0.021(4) 0.033(4) 0.002(3) 0.007(3) 0.002(3) C30 0.024(4) 0.031(5) 0.038(5) 0.000(4) 0.013(4) 0.001(4) C31 0.025(4) 0.030(5) 0.036(5) 0.004(4) 0.011(4) 0.001(4) C32 0.029(4) 0.035(5) 0.038(5) 0.009(4) 0.006(4) 0.002(4) C33 0.023(4) 0.028(4) 0.031(4) -0.001(3) 0.002(3) 0.006(3) C34 0.035(5) 0.032(5) 0.027(4) 0.004(4) -0.002(4) -0.002(4) C35 0.033(5) 0.056(7) 0.034(5) 0.003(4) 0.009(4) -0.007(5) C36 0.045(6) 0.061(8) 0.040(5) 0.007(5) 0.012(4) -0.011(5) C37 0.051(6) 0.058(7) 0.036(5) 0.012(5) 0.012(5) -0.023(5) C38 0.066(7) 0.034(6) 0.034(5) 0.001(4) 0.005(5) -0.001(5) C39 0.043(5) 0.044(6) 0.033(5) 0.004(4) 0.008(4) -0.005(5) C40 0.021(4) 0.041(5) 0.030(4) -0.004(4) 0.008(3) -0.001(4) C41 0.033(4) 0.027(5) 0.027(4) -0.004(4) 0.013(4) -0.002(4) C42 0.032(4) 0.023(4) 0.033(4) -0.001(3) 0.021(4) -0.002(4) C43 0.027(4) 0.025(4) 0.027(4) -0.003(3) 0.013(3) 0.000(3) C44 0.028(4) 0.036(5) 0.027(4) -0.002(3) 0.013(3) 0.001(3) C45 0.032(4) 0.029(5) 0.040(5) -0.008(4) 0.017(4) -0.005(4) C46 0.027(4) 0.035(5) 0.035(5) -0.007(4) 0.013(4) -0.001(4) C47 0.046(6) 0.053(7) 0.029(5) 0.006(4) 0.009(4) -0.020(5) C48 0.146(8) 0.157(8) 0.133(8) 0.043(7) 0.042(6) -0.063(7) C49 0.143(7) 0.152(7) 0.133(7) 0.036(6) 0.035(6) -0.060(6) C50 0.118(6) 0.122(7) 0.106(6) 0.030(6) 0.030(5) -0.057(6) C51 0.096(6) 0.095(6) 0.101(6) 0.030(5) 0.018(5) -0.037(5) C52 0.083(6) 0.085(7) 0.095(7) 0.033(6) 0.016(5) -0.029(6) C53 0.029(4) 0.026(5) 0.030(4) 0.001(3) 0.014(3) 0.002(3) C54 0.017(4) 0.038(5) 0.026(4) -0.005(4) 0.003(3) -0.009(4) C55 0.038(5) 0.036(6) 0.065(7) -0.002(5) 0.016(5) 0.003(5) C56 0.041(6) 0.066(8) 0.060(7) 0.003(6) 0.010(5) 0.005(6) C57 0.104(7) 0.110(7) 0.107(7) 0.017(5) 0.043(5) -0.002(5) C58 0.091(7) 0.072(7) 0.063(6) 0.021(6) 0.041(6) 0.024(6) C59 0.076(7) 0.064(7) 0.077(7) 0.002(6) 0.046(6) 0.004(6) C60 0.092(7) 0.084(8) 0.072(7) -0.009(6) 0.045(6) 0.001(6) C61 0.085(7) 0.058(7) 0.099(8) -0.016(6) 0.044(6) -0.008(6) C62 0.086(7) 0.082(8) 0.093(8) -0.033(6) 0.042(6) -0.013(6) C63 0.054(6) 0.061(7) 0.067(6) 0.005(5) 0.023(5) -0.013(5) C64 0.058(6) 0.048(6) 0.076(6) 0.008(5) 0.028(5) -0.012(5) C65 0.061(7) 0.054(7) 0.054(7) 0.020(6) 0.016(6) 0.007(6) C66 0.055(7) 0.034(6) 0.081(8) 0.011(6) 0.022(6) 0.000(5) C67 0.056(6) 0.039(6) 0.077(8) -0.011(6) 0.031(6) 0.000(5) C68 0.037(6) 0.047(7) 0.086(9) 0.003(6) 0.022(6) 0.010(5) C69 0.066(8) 0.043(7) 0.100(11) 0.011(7) 0.031(7) 0.006(6) C70 0.042(6) 0.042(7) 0.089(9) -0.003(6) 0.008(6) 0.004(5) C71 0.064(6) 0.059(6) 0.045(6) -0.005(5) 0.002(5) 0.009(5) C72 0.095(9) 0.034(6) 0.035(6) -0.006(5) 0.014(6) 0.007(6) C73 0.113(11) 0.038(7) 0.073(8) 0.006(6) 0.064(8) 0.013(7) C74 0.073(6) 0.048(6) 0.070(6) -0.005(5) 0.046(5) 0.003(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 O7 1.789(6) . ? U O8 1.813(5) . ? U O1 2.271(5) . ? U O4 2.277(5) . ? U O2 2.282(5) . ? U O5 2.283(5) . ? Ba O9 2.840(6) . ? Ba O10 2.854(7) . ? Ba O17 2.872(7) . ? Ba O14 2.879(7) . ? Ba O12 2.882(8) . ? Ba O18 2.882(7) . ? Ba O7 2.886(6) . ? Ba O15 2.886(7) . ? Ba O11 2.913(7) . ? Ba O16 2.920(7) . ? Ba O13 2.949(7) . ? O1 C2 1.333(9) . ? O2 C15 1.336(10) . ? O3 C27 1.423(9) . ? O3 C26 1.436(10) . ? O4 C29 1.312(10) . ? O5 C42 1.333(9) . ? O6 C53 1.428(9) . ? O6 C54 1.428(9) . ? O9 C74 1.444(12) . ? O9 C55 1.447(12) . ? O10 C57 1.249(17) . ? O10 C56 1.422(12) . ? O11 C59 1.413(13) . ? O11 C58 1.407(13) . ? O12 C61 1.410(14) . ? O12 C60 1.424(15) . ? O13 C62 1.403(14) . ? O13 C63 1.436(13) . ? O14 C65 1.395(12) . ? O14 C64 1.432(13) . ? O15 C66 1.416(12) . ? O15 C67 1.435(13) . ? O16 C69 1.420(14) . ? O16 C68 1.444(12) . ? O17 C70 1.411(14) . ? O17 C71 1.410(13) . ? O18 C73 1.417(14) . ? O18 C72 1.420(13) . ? C1 C6 1.387(11) . ? C1 C2 1.406(11) . ? C1 C54 1.496(11) . ? C2 C3 1.414(11) . ? C3 C4 1.385(12) . ? C3 C13 1.510(11) . ? C4 C5 1.394(12) . ? C5 C6 1.387(11) . ? C5 C7 1.478(12) . ? C7 C12 1.396(14) . ? C7 C8 1.401(13) . ? C8 C9 1.395(13) . ? C9 C10 1.372(16) . ? C10 C11 1.387(16) . ? C11 C12 1.377(14) . ? C13 C14 1.526(11) . ? C14 C19 1.383(11) . ? C14 C15 1.420(11) . ? C15 C16 1.412(11) . ? C16 C17 1.373(12) . ? C16 C26 1.497(11) . ? C17 C18 1.398(11) . ? C18 C19 1.394(12) . ? C18 C20 1.491(12) . ? C20 C25 1.390(13) . ? C20 C21 1.410(13) . ? C21 C22 1.385(14) . ? C22 C23 1.370(16) . ? C23 C24 1.375(16) . ? C24 C25 1.395(14) . ? C27 C28 1.484(12) . ? C28 C33 1.376(12) . ? C28 C29 1.424(12) . ? C29 C30 1.429(12) . ? C30 C31 1.375(12) . ? C30 C40 1.514(12) . ? C31 C32 1.394(13) . ? C32 C33 1.404(12) . ? C32 C34 1.483(12) . ? C34 C39 1.387(14) . ? C34 C35 1.404(13) . ? C35 C36 1.392(14) . ? C36 C37 1.353(16) . ? C37 C38 1.374(15) . ? C38 C39 1.412(14) . ? C40 C41 1.525(12) . ? C41 C46 1.375(12) . ? C41 C42 1.415(11) . ? C42 C43 1.406(11) . ? C43 C44 1.377(11) . ? C43 C53 1.507(11) . ? C44 C45 1.394(11) . ? C45 C46 1.400(13) . ? C45 C47 1.512(10) . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C55 C56 1.476(15) . ? C57 C58 1.50(2) . ? C59 C60 1.523(18) . ? C61 C62 1.50(2) . ? C63 C64 1.496(16) . ? C65 C66 1.524(16) . ? C67 C68 1.490(15) . ? C69 C70 1.509(18) . ? C71 C72 1.490(16) . ? C73 C74 1.537(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 U O8 179.1(3) . . ? O7 U O1 88.7(2) . . ? O8 U O1 90.5(2) . . ? O7 U O4 90.1(2) . . ? O8 U O4 90.8(2) . . ? O1 U O4 178.6(2) . . ? O7 U O2 89.1(2) . . ? O8 U O2 91.3(2) . . ? O1 U O2 84.74(19) . . ? O4 U O2 94.8(2) . . ? O7 U O5 89.6(2) . . ? O8 U O5 90.1(2) . . ? O1 U O5 94.28(19) . . ? O4 U O5 86.10(19) . . ? O2 U O5 178.4(2) . . ? O9 Ba O10 59.4(2) . . ? O9 Ba O17 108.4(2) . . ? O10 Ba O17 133.5(3) . . ? O9 Ba O14 76.4(2) . . ? O10 Ba O14 114.7(2) . . ? O17 Ba O14 103.3(2) . . ? O9 Ba O12 124.3(2) . . ? O10 Ba O12 80.4(2) . . ? O17 Ba O12 127.2(2) . . ? O14 Ba O12 89.4(2) . . ? O9 Ba O18 61.6(2) . . ? O10 Ba O18 118.9(2) . . ? O17 Ba O18 56.8(2) . . ? O14 Ba O18 63.0(2) . . ? O12 Ba O18 150.6(2) . . ? O9 Ba O7 67.77(17) . . ? O10 Ba O7 70.4(2) . . ? O17 Ba O7 64.01(19) . . ? O14 Ba O7 133.84(19) . . ? O12 Ba O7 134.77(19) . . ? O18 Ba O7 74.57(18) . . ? O9 Ba O15 133.2(2) . . ? O10 Ba O15 149.6(2) . . ? O17 Ba O15 73.8(2) . . ? O14 Ba O15 58.5(2) . . ? O12 Ba O15 70.3(2) . . ? O18 Ba O15 85.8(2) . . ? O7 Ba O15 137.62(18) . . ? O9 Ba O11 114.0(2) . . ? O10 Ba O11 56.7(2) . . ? O17 Ba O11 103.4(2) . . ? O14 Ba O11 146.0(2) . . ? O12 Ba O11 57.5(2) . . ? O18 Ba O11 151.0(2) . . ? O7 Ba O11 77.47(18) . . ? O15 Ba O11 110.4(2) . . ? O9 Ba O16 162.6(2) . . ? O10 Ba O16 122.7(2) . . ? O17 Ba O16 56.5(2) . . ? O14 Ba O16 113.8(2) . . ? O12 Ba O16 71.4(2) . . ? O18 Ba O16 109.1(2) . . ? O7 Ba O16 96.00(18) . . ? O15 Ba O16 55.3(2) . . ? O11 Ba O16 66.1(2) . . ? O9 Ba O13 69.5(2) . . ? O10 Ba O13 63.4(2) . . ? O17 Ba O13 160.3(2) . . ? O14 Ba O13 57.0(2) . . ? O12 Ba O13 58.1(2) . . ? O18 Ba O13 108.5(2) . . ? O7 Ba O13 128.35(18) . . ? O15 Ba O13 93.2(2) . . ? O11 Ba O13 94.9(2) . . ? O16 Ba O13 127.7(2) . . ? C2 O1 U 135.7(5) . . ? C15 O2 U 133.6(5) . . ? C27 O3 C26 111.4(6) . . ? C29 O4 U 135.9(5) . . ? C42 O5 U 133.2(5) . . ? C53 O6 C54 110.8(6) . . ? U O7 Ba 172.6(3) . . ? C74 O9 C55 110.5(8) . . ? C74 O9 Ba 115.1(6) . . ? C55 O9 Ba 116.8(5) . . ? C57 O10 C56 118.2(10) . . ? C57 O10 Ba 121.4(9) . . ? C56 O10 Ba 114.9(6) . . ? C59 O11 C58 114.9(9) . . ? C59 O11 Ba 113.9(6) . . ? C58 O11 Ba 118.8(6) . . ? C61 O12 C60 111.8(10) . . ? C61 O12 Ba 114.0(7) . . ? C60 O12 Ba 121.8(7) . . ? C62 O13 C63 117.4(10) . . ? C62 O13 Ba 119.6(7) . . ? C63 O13 Ba 111.9(6) . . ? C65 O14 C64 112.2(8) . . ? C65 O14 Ba 113.6(6) . . ? C64 O14 Ba 122.6(6) . . ? C66 O15 C67 113.6(8) . . ? C66 O15 Ba 119.6(6) . . ? C67 O15 Ba 114.0(6) . . ? C69 O16 C68 115.6(8) . . ? C69 O16 Ba 105.1(6) . . ? C68 O16 Ba 122.5(6) . . ? C70 O17 C71 114.5(9) . . ? C70 O17 Ba 123.1(7) . . ? C71 O17 Ba 121.1(7) . . ? C73 O18 C72 112.7(9) . . ? C73 O18 Ba 111.6(6) . . ? C72 O18 Ba 115.9(6) . . ? C6 C1 C2 119.9(7) . . ? C6 C1 C54 120.8(7) . . ? C2 C1 C54 119.3(7) . . ? O1 C2 C1 120.3(7) . . ? O1 C2 C3 121.2(7) . . ? C1 C2 C3 118.5(7) . . ? C4 C3 C2 119.3(7) . . ? C4 C3 C13 119.7(7) . . ? C2 C3 C13 121.0(7) . . ? C3 C4 C5 122.5(8) . . ? C6 C5 C4 117.2(8) . . ? C6 C5 C7 121.7(8) . . ? C4 C5 C7 121.1(8) . . ? C1 C6 C5 122.2(8) . . ? C12 C7 C8 117.0(9) . . ? C12 C7 C5 121.4(8) . . ? C8 C7 C5 121.6(9) . . ? C9 C8 C7 121.9(10) . . ? C10 C9 C8 119.7(10) . . ? C9 C10 C11 119.2(10) . . ? C12 C11 C10 121.3(11) . . ? C11 C12 C7 120.9(10) . . ? C3 C13 C14 113.9(7) . . ? C19 C14 C15 119.9(8) . . ? C19 C14 C13 119.5(7) . . ? C15 C14 C13 120.7(7) . . ? O2 C15 C16 121.4(7) . . ? O2 C15 C14 121.2(7) . . ? C16 C15 C14 117.3(8) . . ? C17 C16 C15 120.8(8) . . ? C17 C16 C26 121.1(7) . . ? C15 C16 C26 118.1(7) . . ? C16 C17 C18 122.3(8) . . ? C19 C18 C17 116.7(8) . . ? C19 C18 C20 121.4(8) . . ? C17 C18 C20 121.9(8) . . ? C14 C19 C18 122.7(8) . . ? C25 C20 C21 117.5(9) . . ? C25 C20 C18 121.7(8) . . ? C21 C20 C18 120.7(8) . . ? C22 C21 C20 120.5(10) . . ? C23 C22 C21 121.2(11) . . ? C22 C23 C24 119.2(10) . . ? C23 C24 C25 120.7(11) . . ? C20 C25 C24 120.9(10) . . ? O3 C26 C16 108.9(7) . . ? O3 C27 C28 108.5(7) . . ? C33 C28 C29 120.6(8) . . ? C33 C28 C27 121.4(8) . . ? C29 C28 C27 118.0(7) . . ? O4 C29 C28 121.2(8) . . ? O4 C29 C30 121.9(8) . . ? C28 C29 C30 116.7(7) . . ? C31 C30 C29 120.7(8) . . ? C31 C30 C40 120.4(8) . . ? C29 C30 C40 118.9(7) . . ? C30 C31 C32 122.4(8) . . ? C31 C32 C33 117.0(8) . . ? C31 C32 C34 122.1(8) . . ? C33 C32 C34 120.8(8) . . ? C28 C33 C32 122.4(8) . . ? C39 C34 C35 117.3(9) . . ? C39 C34 C32 120.9(9) . . ? C35 C34 C32 121.8(9) . . ? C36 C35 C34 121.3(10) . . ? C37 C36 C35 120.0(10) . . ? C36 C37 C38 121.0(10) . . ? C37 C38 C39 119.3(10) . . ? C34 C39 C38 121.0(10) . . ? C30 C40 C41 115.2(7) . . ? C46 C41 C42 119.5(8) . . ? C46 C41 C40 119.9(7) . . ? C42 C41 C40 120.6(7) . . ? O5 C42 C43 120.8(7) . . ? O5 C42 C41 121.2(7) . . ? C43 C42 C41 118.0(7) . . ? C44 C43 C42 120.6(7) . . ? C44 C43 C53 121.2(7) . . ? C42 C43 C53 118.3(7) . . ? C43 C44 C45 122.2(8) . . ? C44 C45 C46 116.4(8) . . ? C44 C45 C47 122.7(8) . . ? C46 C45 C47 120.8(7) . . ? C41 C46 C45 123.1(8) . . ? C48 C47 C52 120.0 . . ? C48 C47 C45 121.0(6) . . ? C52 C47 C45 118.8(6) . . ? C47 C48 C49 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C47 120.0 . . ? O6 C53 C43 107.5(6) . . ? O6 C54 C1 108.5(6) . . ? O9 C55 C56 108.5(8) . . ? O10 C56 C55 111.6(9) . . ? O10 C57 C58 119.0(14) . . ? O11 C58 C57 115.4(11) . . ? O11 C59 C60 111.4(10) . . ? O12 C60 C59 107.0(10) . . ? O12 C61 C62 114.7(11) . . ? O13 C62 C61 111.0(11) . . ? O13 C63 C64 110.2(9) . . ? O14 C64 C63 108.5(9) . . ? O14 C65 C66 112.6(10) . . ? O15 C66 C65 107.6(9) . . ? O15 C67 C68 107.4(9) . . ? O16 C68 C67 106.8(8) . . ? O16 C69 C70 112.3(10) . . ? O17 C70 C69 106.9(9) . . ? O17 C71 C72 110.6(9) . . ? O18 C72 C71 108.3(9) . . ? O18 C73 C74 113.4(9) . . ? O9 C74 C73 108.8(9) . . ? #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 638699' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H78 Ba Br6 Cl6 O26 U2' _chemical_formula_weight 2640.88 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' Ba Ba -0.3244 2.2819 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4804(6) _cell_length_b 29.3642(17) _cell_length_c 21.7965(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.601(3) _cell_angle_gamma 90.00 _cell_volume 8619.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 189756 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5032 _exptl_absorpt_coefficient_mu 7.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.294 _exptl_absorpt_correction_T_max 0.521 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 50 mm' _diffrn_ambient_temperature 100(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 'one \f and eight \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 189756 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.68 _reflns_number_total 16311 _reflns_number_gt 9939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with some restraints on bond lengths and/or displacement parameters for the atoms of the badly resolved crown ether and solvent molecules. The H atoms were introduced at calculated positions and 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^)+(0.1349P)^2^+17.7025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 16311 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 141 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2441 _refine_ls_wR_factor_gt 0.2277 _refine_ls_goodness_of_fit_ref 1.081 _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 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.392 _refine_diff_density_min -2.117 _refine_diff_density_rms 0.199 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 U1 U 0.19739(4) 0.294451(18) 1.07953(2) 0.0598(2) Uani 1 1 d . . . Br1A Br -0.02759(12) 0.05939(6) 1.04924(9) 0.0879(5) Uani 1 1 d . . . Br2A Br 0.69672(12) 0.19101(7) 1.05908(10) 0.0922(6) Uani 1 1 d . . . Br3A Br 0.2102(5) 0.3246(2) 0.7365(4) 0.0741(17) Uani 1 1 d . . . O1A O 0.0736(6) 0.2537(3) 1.1131(4) 0.060(2) Uani 1 1 d . . . O2A O 0.2618(6) 0.2137(3) 1.1417(4) 0.060(2) Uani 1 1 d . . . O3A O 0.3455(6) 0.3024(3) 1.1287(4) 0.058(2) Uani 1 1 d . . . O4A O 0.3619(8) 0.3305(3) 1.0038(5) 0.082(3) Uani 1 1 d . . . O5A O 0.1450(7) 0.3435(3) 1.0076(4) 0.062(2) Uani 1 1 d . . . O6A O 0.0212(7) 0.2605(4) 0.9799(5) 0.077(3) Uani 1 1 d . . . O7A O 0.1594(8) 0.3376(3) 1.1326(4) 0.074(3) Uani 1 1 d . . . O8A O 0.2323(6) 0.2525(3) 1.0248(4) 0.052(2) Uani 1 1 d . . . C1A C -0.0174(9) 0.2017(5) 1.0481(7) 0.062(4) Uani 1 1 d . . . C2A C 0.0530(9) 0.2120(6) 1.0958(6) 0.063(4) Uani 1 1 d . . . C3A C 0.1044(9) 0.1763(5) 1.1263(7) 0.064(4) Uani 1 1 d . . . C4A C 0.0804(9) 0.1307(6) 1.1122(7) 0.067(4) Uani 1 1 d . . . H4A H 0.1133 0.1069 1.1325 0.081 Uiso 1 1 calc R . . C5A C 0.0061(10) 0.1222(5) 1.0671(7) 0.065(4) Uani 1 1 d . . . C6A C -0.0428(10) 0.1543(6) 1.0366(7) 0.071(4) Uani 1 1 d . . . H6A H -0.0932 0.1468 1.0079 0.085 Uiso 1 1 calc R . . C7A C 0.1875(9) 0.1882(5) 1.1750(7) 0.063(4) Uani 1 1 d . . . H7A1 H 0.1616 0.2066 1.2075 0.076 Uiso 1 1 calc R . . H7A2 H 0.2164 0.1607 1.1929 0.076 Uiso 1 1 calc R . . C8A C 0.3555(8) 0.2142(5) 1.1771(6) 0.058(3) Uani 1 1 d . . . H8A1 H 0.3725 0.1838 1.1916 0.070 Uiso 1 1 calc R . . H8A2 H 0.3517 0.2343 1.2123 0.070 Uiso 1 1 calc R . . C9A C 0.4340(10) 0.2319(5) 1.1325(6) 0.060(4) Uani 1 1 d . . . C10A C 0.4209(10) 0.2757(5) 1.1104(6) 0.054(3) Uani 1 1 d . . . C11A C 0.4820(10) 0.2938(4) 1.0677(7) 0.060(4) Uani 1 1 d . . . C12A C 0.5653(11) 0.2670(6) 1.0488(7) 0.070(4) Uani 1 1 d . . . H12A H 0.6064 0.2769 1.0184 0.084 Uiso 1 1 calc R . . C13A C 0.5803(10) 0.2258(6) 1.0787(7) 0.072(4) Uani 1 1 d . . . C14A C 0.5141(9) 0.2083(5) 1.1189(6) 0.058(3) Uani 1 1 d . . . H14A H 0.5256 0.1799 1.1367 0.070 Uiso 1 1 calc R . . C15A C 0.4527(11) 0.3376(5) 1.0349(7) 0.067(4) Uani 1 1 d . . . H15A H 0.4473 0.3621 1.0644 0.080 Uiso 1 1 calc R . . H15B H 0.5025 0.3458 1.0062 0.080 Uiso 1 1 calc R . . C16A C 0.3301(11) 0.3673(5) 0.9631(6) 0.063(4) Uani 1 1 d . . . H16A H 0.3845 0.3767 0.9384 0.075 Uiso 1 1 calc R . . H16B H 0.3094 0.3933 0.9869 0.075 Uiso 1 1 calc R . . C17A C 0.2447(16) 0.3503(5) 0.9225(7) 0.088(6) Uani 1 1 d . . . C18A C 0.1549(11) 0.3372(5) 0.9462(6) 0.062(4) Uani 1 1 d . . . C19A C 0.0802(12) 0.3172(5) 0.9118(7) 0.069(4) Uani 1 1 d . . . C20A C 0.0941(13) 0.3112(5) 0.8489(7) 0.086(5) Uani 1 1 d . . . H20A H 0.0450 0.2977 0.8237 0.104 Uiso 1 1 calc R . . C21A C 0.1818(12) 0.3256(6) 0.8250(7) 0.084(5) Uani 1 1 d . . . C22A C 0.2608(13) 0.3449(6) 0.8585(8) 0.086(5) Uani 1 1 d . . . H22A H 0.3194 0.3536 0.8408 0.103 Uiso 1 1 calc R . . C23A C -0.0067(14) 0.2997(5) 0.9399(8) 0.085(5) Uani 1 1 d . . . H23A H -0.0553 0.2902 0.9084 0.102 Uiso 1 1 calc R . . H23B H -0.0362 0.3235 0.9641 0.102 Uiso 1 1 calc R . . C24A C -0.0604(12) 0.2391(6) 1.0124(8) 0.088(6) Uani 1 1 d . . . H24A H -0.0905 0.2610 1.0392 0.105 Uiso 1 1 calc R . . H24B H -0.1111 0.2279 0.9832 0.105 Uiso 1 1 calc R . . U2 U 0.75087(5) -0.024060(19) 0.73945(3) 0.0745(2) Uani 1 1 d . . . Br1B Br 0.37568(15) 0.07461(6) 0.52544(8) 0.0900(5) Uani 1 1 d . . . Br2B Br 0.76363(14) 0.21400(5) 0.84827(8) 0.0825(5) Uani 1 1 d . . . Br3B Br 0.3211(2) -0.05590(9) 0.94533(16) 0.0889(8) Uani 1 1 d . . . O1B O 0.7052(7) -0.0368(3) 0.6424(5) 0.070(3) Uani 1 1 d . . . O2B O 0.7830(8) 0.0511(3) 0.6698(4) 0.070(3) Uani 1 1 d . . . O3B O 0.8694(8) 0.0218(4) 0.7843(5) 0.078(3) Uani 1 1 d . . . O4B O 0.7284(8) 0.0125(3) 0.8868(4) 0.077(3) Uani 1 1 d . . . O5B O 0.6999(8) -0.0730(3) 0.8087(4) 0.069(3) Uani 1 1 d . . . O6B O 0.5367(9) -0.0634(3) 0.7107(5) 0.089(3) Uani 1 1 d . . . O7B O 0.8504(9) -0.0620(4) 0.7253(5) 0.092(4) Uani 1 1 d . . . O8B O 0.6531(7) 0.0142(3) 0.7553(4) 0.064(2) Uani 1 1 d . . . C1B C 0.5340(13) -0.0275(5) 0.6154(8) 0.076(4) Uani 1 1 d . . . C2B C 0.6318(11) -0.0097(5) 0.6156(7) 0.067(4) Uani 1 1 d . . . C3B C 0.6524(12) 0.0318(4) 0.5938(6) 0.058(4) Uani 1 1 d . . . C4B C 0.5745(12) 0.0571(5) 0.5668(6) 0.064(4) Uani 1 1 d . . . H4B H 0.5865 0.0862 0.5520 0.077 Uiso 1 1 calc R . . C5B C 0.4805(13) 0.0395(5) 0.5618(7) 0.071(4) Uani 1 1 d . . . C6B C 0.4619(13) -0.0018(6) 0.5865(7) 0.082(5) Uani 1 1 d . . . H6B H 0.3973 -0.0130 0.5835 0.099 Uiso 1 1 calc R . . C7B C 0.7565(12) 0.0482(5) 0.6040(6) 0.072(4) Uani 1 1 d . . . H7B1 H 0.8014 0.0275 0.5845 0.086 Uiso 1 1 calc R . . H7B2 H 0.7632 0.0780 0.5854 0.086 Uiso 1 1 calc R . . C8B C 0.8499(10) 0.0836(5) 0.6877(6) 0.064(4) Uani 1 1 d . . . H8B1 H 0.8419 0.1099 0.6610 0.077 Uiso 1 1 calc R . . H8B2 H 0.9167 0.0719 0.6840 0.077 Uiso 1 1 calc R . . C9B C 0.8356(9) 0.0976(5) 0.7534(7) 0.061(4) Uani 1 1 d . . . C10B C 0.8445(10) 0.0646(5) 0.7983(7) 0.060(4) Uani 1 1 d . . . C11B C 0.8259(10) 0.0747(5) 0.8611(7) 0.061(4) Uani 1 1 d . . . C12B C 0.8005(9) 0.1196(5) 0.8757(7) 0.061(4) Uani 1 1 d . . . H12B H 0.7862 0.1275 0.9156 0.074 Uiso 1 1 calc R . . C13B C 0.7970(10) 0.1517(5) 0.8296(8) 0.065(4) Uani 1 1 d . . . C14B C 0.8121(10) 0.1413(5) 0.7674(7) 0.061(4) Uani 1 1 d . . . H14B H 0.8062 0.1635 0.7370 0.073 Uiso 1 1 calc R . . C15B C 0.8175(11) 0.0369(5) 0.9036(7) 0.071(4) Uani 1 1 d . . . H15C H 0.8746 0.0170 0.9013 0.085 Uiso 1 1 calc R . . H15D H 0.8148 0.0481 0.9453 0.085 Uiso 1 1 calc R . . C16B C 0.7170(15) -0.0318(5) 0.9208(8) 0.090(5) Uani 1 1 d . . . H16C H 0.7702 -0.0527 0.9119 0.108 Uiso 1 1 calc R . . H16D H 0.7173 -0.0267 0.9647 0.108 Uiso 1 1 calc R . . C17B C 0.6198(13) -0.0498(5) 0.8976(7) 0.076(4) Uani 1 1 d . . . C18B C 0.6143(16) -0.0699(5) 0.8394(8) 0.083(5) Uani 1 1 d . . . C19B C 0.5241(16) -0.0851(5) 0.8152(9) 0.089(5) Uani 1 1 d . . . C20B C 0.4413(14) -0.0820(6) 0.8464(8) 0.094(5) Uani 1 1 d . . . H20B H 0.3807 -0.0923 0.8297 0.113 Uiso 1 1 calc R . . C21B C 0.4490(16) -0.0625(6) 0.9057(8) 0.103(6) Uani 1 1 d . . . C22B C 0.5365(14) -0.0467(5) 0.9310(8) 0.086(5) Uani 1 1 d . . . H22B H 0.5396 -0.0341 0.9702 0.103 Uiso 1 1 calc R . . C23B C 0.5180(12) -0.1024(5) 0.7478(8) 0.078(4) Uani 1 1 d . . . H23C H 0.5673 -0.1259 0.7418 0.094 Uiso 1 1 calc R . . H23D H 0.4527 -0.1149 0.7374 0.094 Uiso 1 1 calc R . . C24B C 0.5164(13) -0.0734(5) 0.6447(8) 0.079(5) Uani 1 1 d . . . H24C H 0.4486 -0.0836 0.6368 0.095 Uiso 1 1 calc R . . H24D H 0.5616 -0.0963 0.6301 0.095 Uiso 1 1 calc R . . Ba Ba 0.30816(6) 0.13789(3) 0.81027(4) 0.0584(2) Uani 1 1 d . . . O1 O 0.1351(9) 0.1912(4) 0.8162(6) 0.091(3) Uani 1 1 d . . . O2 O 0.1622(11) 0.1393(4) 0.7093(6) 0.073(4) Uani 1 1 d D . . O3 O 0.3395(15) 0.1728(8) 0.6888(10) 0.097(7) Uani 1 1 d D . . O4 O 0.3967(16) 0.2290(8) 0.8007(9) 0.103(7) Uani 1 1 d D . . O5 O 0.3494(12) 0.1968(5) 0.9080(7) 0.097(5) Uani 1 1 d D . . O6 O 0.4324(10) 0.1132(4) 0.9148(6) 0.063(3) Uani 1 1 d . . . O7 O 0.5111(9) 0.1161(4) 0.8076(6) 0.106(4) Uani 1 1 d D . . O8 O 0.3612(15) 0.0692(8) 0.7295(11) 0.084(7) Uani 1 1 d D . . O9 O 0.232(2) 0.0529(10) 0.8318(12) 0.075(9) Uani 1 1 d D . . O10 O 0.1921(16) 0.1285(8) 0.9137(11) 0.104(7) Uani 1 1 d D . . C1 C 0.079(2) 0.1954(8) 0.7595(12) 0.104(8) Uani 1 1 d D . . H1A H 0.0118 0.2037 0.7683 0.125 Uiso 1 1 calc R . . H1B H 0.1070 0.2202 0.7364 0.125 Uiso 1 1 calc R . . C2 C 0.0756(14) 0.1543(7) 0.7198(9) 0.075(6) Uani 1 1 d D . . H2A H 0.0410 0.1616 0.6810 0.090 Uiso 1 1 calc R . . H2B H 0.0383 0.1306 0.7395 0.090 Uiso 1 1 calc R . . C3 C 0.2069(16) 0.1223(7) 0.6561(10) 0.09(2) Uani 1 1 d DU . . H3A H 0.1584 0.1145 0.6236 0.107 Uiso 1 1 calc R . . H3B H 0.2503 0.0966 0.6651 0.107 Uiso 1 1 calc R . . C4 C 0.263(2) 0.1651(8) 0.6422(11) 0.072(8) Uani 1 1 d D . . H4C H 0.2930 0.1621 0.6027 0.087 Uiso 1 1 calc R . . H4D H 0.2184 0.1908 0.6402 0.087 Uiso 1 1 calc R . . C5 C 0.379(3) 0.2175(11) 0.6872(10) 0.081(15) Uani 1 1 d DU . . H5A H 0.3246 0.2379 0.6773 0.097 Uiso 1 1 calc R . . H5B H 0.4228 0.2185 0.6529 0.097 Uiso 1 1 calc R . . C6 C 0.4370(19) 0.2377(10) 0.7421(9) 0.072(8) Uani 1 1 d D . . H6C H 0.5043 0.2259 0.7427 0.087 Uiso 1 1 calc R . . H6D H 0.4409 0.2704 0.7364 0.087 Uiso 1 1 calc R . . C7 C 0.429(3) 0.2586(10) 0.8493(11) 0.106(15) Uani 1 1 d DU . . H7A H 0.4201 0.2903 0.8380 0.128 Uiso 1 1 calc R . . H7B H 0.4972 0.2531 0.8623 0.128 Uiso 1 1 calc R . . C8 C 0.3579(19) 0.2445(6) 0.8982(11) 0.065(7) Uani 1 1 d D . . H8A H 0.3796 0.2586 0.9367 0.078 Uiso 1 1 calc R . . H8B H 0.2925 0.2564 0.8869 0.078 Uiso 1 1 calc R . . C9 C 0.4101(18) 0.1852(7) 0.9603(9) 0.058(7) Uani 1 1 d D . . H9A H 0.4771 0.1966 0.9561 0.069 Uiso 1 1 calc R . . H9B H 0.3837 0.1984 0.9970 0.069 Uiso 1 1 calc R . . C10 C 0.410(3) 0.1342(8) 0.9645(16) 0.090(10) Uani 1 1 d DU . . H10A H 0.3453 0.1242 0.9760 0.108 Uiso 1 1 calc R . . H10B H 0.4577 0.1252 0.9971 0.108 Uiso 1 1 calc R . . C11 C 0.536(2) 0.1037(11) 0.9091(11) 0.096(9) Uani 1 1 d DU . . H11A H 0.5741 0.1317 0.9084 0.115 Uiso 1 1 calc R . . H11B H 0.5614 0.0848 0.9427 0.115 Uiso 1 1 calc R . . C12 C 0.5396(15) 0.0790(7) 0.8488(9) 0.111(6) Uani 1 1 d DU . . H12C H 0.4926 0.0540 0.8460 0.134 Uiso 1 1 calc R . . H12D H 0.6058 0.0678 0.8416 0.134 Uiso 1 1 calc R . . C13 C 0.5371(17) 0.1064(7) 0.7456(8) 0.096(7) Uani 1 1 d DU . . H13A H 0.6042 0.0945 0.7454 0.115 Uiso 1 1 calc R . . H13B H 0.5341 0.1340 0.7212 0.115 Uiso 1 1 calc R . . C14 C 0.4645(16) 0.0717(13) 0.7187(19) 0.070(12) Uani 1 1 d D . . H14C H 0.4689 0.0739 0.6745 0.084 Uiso 1 1 calc R . . H14D H 0.4917 0.0421 0.7303 0.084 Uiso 1 1 calc R . . C15 C 0.304(2) 0.0294(8) 0.7339(11) 0.092(10) Uani 1 1 d DU . . H15E H 0.3461 0.0041 0.7233 0.110 Uiso 1 1 calc R . . H15F H 0.2513 0.0312 0.7021 0.110 Uiso 1 1 calc R . . C16 C 0.256(6) 0.0166(8) 0.792(2) 0.12(3) Uani 1 1 d DU . . H16E H 0.1958 -0.0002 0.7815 0.148 Uiso 1 1 calc R . . H16F H 0.3004 -0.0040 0.8150 0.148 Uiso 1 1 calc R . . C17 C 0.147(2) 0.0624(17) 0.8663(18) 0.124(18) Uani 1 1 d DU . . H17A H 0.1099 0.0344 0.8708 0.148 Uiso 1 1 calc R . . H17B H 0.1045 0.0834 0.8429 0.148 Uiso 1 1 calc R . . C18 C 0.169(5) 0.0825(8) 0.9299(15) 0.11(3) Uani 1 1 d DU . . H18A H 0.1118 0.0810 0.9551 0.132 Uiso 1 1 calc R . . H18B H 0.2251 0.0675 0.9508 0.132 Uiso 1 1 calc R . . C19 C 0.137(3) 0.1693(10) 0.9236(15) 0.073(13) Uani 1 1 d D . . H19A H 0.0898 0.1635 0.9548 0.087 Uiso 1 1 calc R . . H19B H 0.1827 0.1926 0.9392 0.087 Uiso 1 1 calc R . . C20 C 0.082(2) 0.1874(11) 0.8665(13) 0.096(9) Uani 1 1 d DU . . H20C H 0.0259 0.1674 0.8570 0.115 Uiso 1 1 calc R . . H20D H 0.0553 0.2171 0.8760 0.115 Uiso 1 1 calc R . . Cl1 Cl 0.7218(4) 0.34771(19) 0.9572(2) 0.1044(15) Uani 1 1 d . . . Cl2 Cl 0.5686(4) 0.3531(2) 0.8616(3) 0.1202(19) Uani 1 1 d . . . Cl3 Cl 0.7705(4) 0.33719(15) 0.8335(2) 0.0963(14) Uani 1 1 d . . . C21 C 0.6902(11) 0.3665(6) 0.8820(7) 0.075(4) Uani 1 1 d . . . H21 H 0.7005 0.3994 0.8789 0.090 Uiso 1 1 calc R . . Cl4 Cl -0.0272(9) -0.0293(5) 0.5838(9) 0.100(5) Uani 1 1 d DU . . Cl5 Cl 0.1778(9) -0.0303(4) 0.6046(8) 0.090(4) Uani 1 1 d DU . . Cl6 Cl 0.0806(10) 0.0524(4) 0.5902(7) 0.082(4) Uani 1 1 d DU . . C22 C 0.0707(11) -0.0006(5) 0.6196(13) 0.08(2) Uani 1 1 d DU . . H22 H 0.0622 0.0010 0.6640 0.095 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 U1 0.0686(4) 0.0594(3) 0.0510(3) -0.0113(2) -0.0006(2) 0.0161(3) Br1A 0.0657(9) 0.0887(12) 0.1074(14) -0.0023(10) -0.0173(9) -0.0203(9) Br2A 0.0612(9) 0.1039(13) 0.1130(14) 0.0117(11) 0.0196(9) 0.0199(9) Br3A 0.079(2) 0.092(4) 0.051(2) -0.007(3) 0.0034(17) 0.021(3) O1A 0.041(5) 0.066(6) 0.073(6) -0.013(5) -0.006(4) 0.013(4) O2A 0.058(5) 0.063(6) 0.060(6) -0.003(4) -0.003(4) 0.000(4) O3A 0.054(5) 0.058(5) 0.062(6) -0.013(4) 0.000(4) -0.003(4) O4A 0.102(8) 0.058(6) 0.082(7) 0.006(5) -0.024(6) 0.003(6) O5A 0.076(6) 0.049(5) 0.060(6) -0.007(4) -0.005(5) 0.026(4) O6A 0.046(5) 0.093(8) 0.090(8) 0.014(6) -0.001(5) 0.019(5) O7A 0.096(7) 0.061(6) 0.064(6) -0.013(5) -0.004(5) 0.018(5) O8A 0.057(5) 0.054(5) 0.045(5) -0.009(4) -0.003(4) 0.006(4) C1A 0.040(7) 0.066(9) 0.080(10) -0.002(8) 0.000(7) 0.013(7) C2A 0.039(7) 0.092(11) 0.058(9) -0.012(8) 0.007(6) 0.016(7) C3A 0.041(7) 0.087(11) 0.063(9) -0.003(8) 0.004(6) 0.005(7) C4A 0.036(7) 0.098(12) 0.069(9) -0.008(8) 0.002(6) -0.016(7) C5A 0.049(8) 0.072(9) 0.074(10) -0.003(8) 0.002(7) -0.008(7) C6A 0.042(8) 0.093(12) 0.078(11) -0.014(9) -0.003(7) -0.009(8) C7A 0.045(7) 0.081(10) 0.065(9) 0.007(8) 0.015(7) 0.004(7) C8A 0.038(7) 0.082(10) 0.054(8) -0.002(7) -0.006(6) 0.002(6) C9A 0.058(8) 0.070(9) 0.049(8) -0.006(7) -0.018(6) -0.019(7) C10A 0.055(8) 0.062(8) 0.044(7) 0.005(6) -0.012(6) 0.002(7) C11A 0.051(8) 0.051(8) 0.076(10) -0.003(7) -0.017(7) -0.005(6) C12A 0.062(9) 0.089(11) 0.058(9) 0.010(8) 0.007(7) -0.004(8) C13A 0.048(8) 0.093(12) 0.074(10) -0.001(9) 0.003(7) 0.005(8) C14A 0.038(7) 0.069(9) 0.067(9) 0.008(7) 0.004(6) 0.002(6) C15A 0.068(9) 0.063(9) 0.068(10) 0.010(7) -0.001(8) -0.012(7) C16A 0.083(10) 0.058(8) 0.046(8) 0.009(7) -0.005(7) -0.014(7) C17A 0.153(18) 0.063(10) 0.048(9) 0.006(7) 0.005(10) 0.058(11) C18A 0.077(10) 0.064(9) 0.045(8) -0.007(7) 0.010(7) 0.017(8) C19A 0.081(11) 0.070(10) 0.055(9) 0.006(8) -0.007(8) 0.018(9) C20A 0.131(16) 0.062(10) 0.062(11) -0.003(8) -0.039(10) 0.022(10) C21A 0.106(10) 0.087(10) 0.058(8) -0.005(8) -0.004(8) 0.032(9) C22A 0.103(10) 0.085(9) 0.069(9) 0.009(8) -0.010(8) 0.019(8) C23A 0.091(12) 0.067(10) 0.093(13) -0.021(9) -0.033(10) 0.029(9) C24A 0.063(10) 0.104(13) 0.094(12) -0.039(11) -0.017(9) 0.036(10) U2 0.1001(5) 0.0508(3) 0.0755(4) 0.0076(3) 0.0337(3) 0.0266(3) Br1B 0.1186(14) 0.0818(11) 0.0681(11) 0.0018(9) -0.0144(9) 0.0185(10) Br2B 0.0954(12) 0.0637(9) 0.0880(12) -0.0183(8) 0.0010(9) -0.0119(8) Br3B 0.1065(19) 0.0646(15) 0.099(2) -0.0122(14) 0.0471(16) -0.0066(14) O1B 0.072(6) 0.048(5) 0.092(7) -0.021(5) 0.012(5) 0.000(5) O2B 0.103(7) 0.049(5) 0.060(6) 0.007(5) 0.020(5) -0.014(5) O3B 0.086(7) 0.081(7) 0.066(7) 0.009(5) 0.000(5) 0.022(6) O4B 0.106(8) 0.060(6) 0.062(6) 0.015(5) -0.010(6) -0.009(6) O5B 0.104(8) 0.037(5) 0.070(6) -0.001(4) 0.032(6) 0.010(5) O6B 0.132(10) 0.051(6) 0.082(8) 0.010(5) -0.027(7) -0.025(6) O7B 0.119(9) 0.073(7) 0.085(8) 0.001(6) 0.030(7) 0.058(7) O8B 0.087(7) 0.046(5) 0.062(6) 0.004(4) 0.021(5) 0.021(5) C1B 0.079(11) 0.048(9) 0.101(13) 0.009(8) -0.007(9) 0.005(8) C2B 0.072(10) 0.065(9) 0.065(9) -0.002(7) 0.012(7) 0.029(8) C3B 0.095(11) 0.041(7) 0.040(7) -0.013(6) 0.019(7) -0.011(7) C4B 0.088(10) 0.065(9) 0.039(8) 0.004(7) 0.003(7) -0.005(8) C5B 0.103(12) 0.061(9) 0.052(9) 0.007(7) 0.017(8) -0.013(9) C6B 0.097(12) 0.085(12) 0.067(10) -0.030(9) 0.012(9) 0.029(10) C7B 0.099(12) 0.074(10) 0.044(8) 0.010(7) 0.025(7) -0.009(9) C8B 0.053(8) 0.080(10) 0.060(9) -0.014(7) 0.011(6) -0.012(7) C9B 0.041(7) 0.065(9) 0.077(10) -0.008(8) 0.000(6) -0.006(6) C10B 0.053(8) 0.064(9) 0.063(9) -0.004(7) -0.011(6) 0.019(7) C11B 0.053(8) 0.068(9) 0.062(9) 0.007(7) 0.002(6) 0.007(7) C12B 0.039(7) 0.086(11) 0.059(9) -0.009(8) -0.004(6) -0.008(7) C13B 0.059(8) 0.053(8) 0.083(11) -0.019(8) 0.009(7) -0.007(7) C14B 0.053(8) 0.056(9) 0.073(10) 0.012(7) -0.010(7) -0.012(7) C15B 0.074(10) 0.071(10) 0.067(10) 0.001(8) -0.006(8) 0.005(8) C16B 0.122(11) 0.069(9) 0.079(9) 0.004(8) 0.015(9) 0.015(9) C17B 0.105(13) 0.063(9) 0.062(10) 0.003(8) 0.026(9) 0.002(9) C18B 0.135(16) 0.041(8) 0.076(11) -0.008(8) 0.043(11) 0.010(9) C19B 0.119(11) 0.058(8) 0.093(10) -0.012(8) 0.036(9) -0.017(8) C20B 0.107(11) 0.067(9) 0.111(11) -0.035(8) 0.032(9) -0.006(8) C21B 0.116(11) 0.080(10) 0.115(12) -0.006(9) 0.041(10) 0.005(9) C22B 0.123(11) 0.058(8) 0.080(9) -0.015(7) 0.039(9) -0.015(8) C23B 0.080(9) 0.058(8) 0.098(10) -0.003(8) 0.016(8) -0.008(7) C24B 0.079(10) 0.056(9) 0.101(13) 0.009(9) -0.016(9) -0.005(8) Ba 0.0484(4) 0.0791(6) 0.0475(5) -0.0002(4) 0.0008(3) 0.0155(4) O1 0.084(8) 0.082(7) 0.107(10) -0.009(7) -0.011(7) 0.019(6) O2 0.083(8) 0.057(7) 0.076(8) -0.008(6) -0.042(7) 0.013(7) O3 0.091(11) 0.107(12) 0.095(12) -0.030(10) 0.018(10) 0.033(10) O4 0.087(11) 0.102(12) 0.125(13) -0.001(11) 0.065(10) -0.015(10) O5 0.106(10) 0.088(9) 0.094(10) -0.013(8) -0.040(8) 0.026(8) O6 0.075(8) 0.061(7) 0.051(7) -0.009(6) -0.016(6) -0.002(6) O7 0.094(7) 0.100(8) 0.127(9) -0.001(7) 0.021(7) 0.029(6) O8 0.092(13) 0.094(13) 0.065(12) -0.023(10) -0.010(10) 0.043(11) O9 0.086(14) 0.044(12) 0.094(15) -0.021(11) -0.027(12) 0.003(11) O10 0.090(11) 0.123(13) 0.105(12) 0.052(10) 0.063(10) 0.052(10) C1 0.084(12) 0.097(13) 0.128(15) 0.011(12) -0.029(11) 0.035(11) C2 0.054(10) 0.097(12) 0.074(11) 0.031(10) -0.005(9) -0.006(9) C3 0.09(3) 0.09(2) 0.08(3) -0.001(15) -0.002(16) -0.010(15) C4 0.118(15) 0.059(12) 0.040(11) 0.006(10) -0.005(11) 0.011(11) C5 0.067(18) 0.085(19) 0.09(2) 0.003(14) 0.000(14) 0.013(14) C6 0.084(14) 0.065(13) 0.069(13) 0.001(11) 0.021(11) -0.003(11) C7 0.088(18) 0.115(19) 0.12(2) -0.016(14) 0.009(14) 0.001(14) C8 0.070(12) 0.057(12) 0.067(13) -0.025(10) -0.003(11) 0.006(10) C9 0.052(11) 0.072(13) 0.049(12) -0.009(10) -0.005(10) 0.013(10) C10 0.081(14) 0.094(15) 0.095(16) -0.011(13) 0.002(12) 0.016(12) C11 0.098(14) 0.097(14) 0.092(14) -0.003(12) 0.000(11) 0.016(12) C12 0.088(10) 0.110(11) 0.135(13) -0.003(10) 0.000(9) 0.044(9) C13 0.092(12) 0.066(11) 0.134(14) 0.033(10) 0.058(11) 0.047(10) C14 0.078(17) 0.077(17) 0.055(16) -0.013(13) 0.011(13) 0.043(13) C15 0.085(14) 0.102(15) 0.085(14) -0.035(12) -0.033(11) -0.043(12) C16 0.13(3) 0.12(3) 0.12(3) 0.002(16) 0.004(16) -0.002(16) C17 0.13(2) 0.09(2) 0.14(2) 0.001(14) -0.012(15) -0.014(14) C18 0.11(3) 0.11(3) 0.11(3) 0.001(15) 0.023(15) 0.012(15) C19 0.065(17) 0.087(18) 0.066(18) -0.017(14) 0.012(13) 0.013(14) C20 0.076(12) 0.099(14) 0.114(15) -0.013(12) 0.024(12) 0.048(11) Cl1 0.120(4) 0.121(4) 0.072(3) 0.009(3) 0.001(2) -0.038(3) Cl2 0.078(3) 0.142(4) 0.140(4) 0.049(4) -0.007(3) -0.038(3) Cl3 0.131(4) 0.078(3) 0.081(3) 0.003(2) 0.017(3) 0.015(3) C21 0.081(10) 0.077(10) 0.066(10) 0.005(8) 0.002(8) -0.026(8) Cl4 0.054(6) 0.080(8) 0.167(12) 0.064(8) 0.022(7) 0.007(6) Cl5 0.061(6) 0.068(7) 0.139(10) -0.073(7) -0.003(7) 0.014(5) Cl6 0.089(8) 0.057(6) 0.103(9) -0.005(6) 0.022(7) 0.019(6) C22 0.09(3) 0.08(3) 0.07(2) 0.000(15) 0.005(15) 0.013(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O8A 1.793(8) . ? U1 O7A 1.804(9) . ? U1 O1A 2.205(9) . ? U1 O5A 2.219(9) . ? U1 O3A 2.235(9) . ? U1 O2A 2.847(9) . ? Br1A C5A 1.936(14) . ? Br2A C13A 1.936(15) . ? Br3A C21A 1.983(18) . ? O1A C2A 1.308(17) . ? O2A C8A 1.451(14) . ? O2A C7A 1.469(15) . ? O3A C10A 1.357(15) . ? O4A C15A 1.388(17) . ? O4A C16A 1.450(16) . ? O5A C18A 1.363(16) . ? O6A C24A 1.48(2) . ? O6A C23A 1.482(19) . ? C1A C2A 1.41(2) . ? C1A C6A 1.45(2) . ? C1A C24A 1.45(2) . ? C2A C3A 1.41(2) . ? C3A C4A 1.41(2) . ? C3A C7A 1.55(2) . ? C4A C5A 1.394(19) . ? C5A C6A 1.31(2) . ? C8A C9A 1.560(19) . ? C9A C14A 1.327(19) . ? C9A C10A 1.382(19) . ? C10A C11A 1.377(19) . ? C11A C12A 1.45(2) . ? C11A C15A 1.513(19) . ? C12A C13A 1.38(2) . ? C13A C14A 1.38(2) . ? C16A C17A 1.51(2) . ? C17A C18A 1.39(2) . ? C17A C22A 1.43(2) . ? C18A C19A 1.36(2) . ? C19A C20A 1.40(2) . ? C19A C23A 1.44(2) . ? C20A C21A 1.380(10) . ? C21A C22A 1.384(10) . ? U2 O8B 1.777(8) . ? U2 O7B 1.782(9) . ? U2 O1B 2.208(10) . ? U2 O5B 2.216(9) . ? U2 O3B 2.275(11) . ? U2 O2B 2.725(9) . ? Br1B C5B 1.893(17) . ? Br2B C13B 1.931(14) . ? Br3B C21B 1.973(19) . ? O1B C2B 1.379(16) . ? O2B C8B 1.358(16) . ? O2B C7B 1.464(17) . ? O3B C10B 1.340(16) . ? O4B C15B 1.431(17) . ? O4B C16B 1.509(18) . ? O5B C18B 1.363(19) . ? O6B C23B 1.432(18) . ? O6B C24B 1.481(19) . ? C1B C6B 1.36(2) . ? C1B C2B 1.42(2) . ? C1B C24B 1.52(2) . ? C2B C3B 1.343(19) . ? C3B C4B 1.39(2) . ? C3B C7B 1.49(2) . ? C4B C5B 1.37(2) . ? C5B C6B 1.36(2) . ? C8B C9B 1.512(19) . ? C9B C14B 1.359(19) . ? C9B C10B 1.38(2) . ? C10B C11B 1.434(19) . ? C11B C12B 1.401(19) . ? C11B C15B 1.45(2) . ? C12B C13B 1.38(2) . ? C13B C14B 1.41(2) . ? C16B C17B 1.48(2) . ? C17B C22B 1.37(2) . ? C17B C18B 1.40(2) . ? C18B C19B 1.38(3) . ? C19B C20B 1.34(2) . ? C19B C23B 1.55(2) . ? C20B C21B 1.412(10) . ? C21B C22B 1.36(2) . ? Ba O9 2.75(3) . ? Ba O8 2.79(2) . ? Ba O5 2.780(15) . ? Ba O10 2.815(19) . ? Ba O7 2.812(12) . ? Ba O1 2.816(11) . ? Ba O6 2.860(12) . ? Ba O2 2.886(12) . ? Ba O3 2.89(2) . ? Ba O4 2.94(2) . ? O1 C20 1.34(3) . ? O1 C1 1.42(3) . ? O2 C2 1.278(16) . ? O2 C3 1.42(3) . ? O3 C5 1.42(4) . ? O3 C4 1.43(3) . ? O4 C7 1.42(4) . ? O4 C6 1.43(3) . ? O5 C8 1.421(10) . ? O5 C9 1.41(3) . ? O6 C10 1.29(3) . ? O6 C11 1.43(3) . ? O7 C13 1.441(10) . ? O7 C12 1.45(2) . ? O8 C15 1.41(3) . ? O8 C14 1.43(3) . ? O9 C16 1.42(5) . ? O9 C17 1.43(4) . ? O10 C18 1.43(4) . ? O10 C19 1.43(3) . ? C1 C2 1.49(3) . ? C3 C4 1.51(3) . ? C5 C6 1.52(4) . ? C7 C8 1.52(4) . ? C9 C10 1.50(3) . ? C11 C12 1.50(3) . ? C13 C14 1.51(4) . ? C15 C16 1.50(6) . ? C17 C18 1.52(5) . ? C19 C20 1.52(4) . ? Cl1 C21 1.763(16) . ? Cl2 C21 1.725(16) . ? Cl3 C21 1.771(17) . ? Cl4 C22 1.723(10) . ? Cl5 C22 1.731(10) . ? Cl6 C22 1.690(10) . ? 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 O8A U1 O7A 178.0(4) . . ? O8A U1 O1A 94.2(4) . . ? O7A U1 O1A 85.8(4) . . ? O8A U1 O5A 93.5(3) . . ? O7A U1 O5A 84.6(4) . . ? O1A U1 O5A 111.4(3) . . ? O8A U1 O3A 97.8(3) . . ? O7A U1 O3A 83.8(4) . . ? O1A U1 O3A 124.8(3) . . ? O5A U1 O3A 121.3(3) . . ? O8A U1 O2A 70.2(3) . . ? O7A U1 O2A 111.7(4) . . ? O1A U1 O2A 67.0(3) . . ? O5A U1 O2A 163.0(3) . . ? O3A U1 O2A 67.2(3) . . ? C2A O1A U1 124.5(8) . . ? C8A O2A C7A 109.8(10) . . ? C8A O2A U1 118.9(7) . . ? C7A O2A U1 117.4(7) . . ? C10A O3A U1 117.6(7) . . ? C15A O4A C16A 114.6(11) . . ? C18A O5A U1 124.3(7) . . ? C24A O6A C23A 116.0(11) . . ? C2A C1A C6A 118.5(13) . . ? C2A C1A C24A 118.3(14) . . ? C6A C1A C24A 123.2(14) . . ? O1A C2A C3A 117.8(13) . . ? O1A C2A C1A 122.7(13) . . ? C3A C2A C1A 119.4(14) . . ? C2A C3A C4A 120.2(13) . . ? C2A C3A C7A 118.9(14) . . ? C4A C3A C7A 120.9(13) . . ? C5A C4A C3A 118.2(15) . . ? C6A C5A C4A 123.8(14) . . ? C6A C5A Br1A 118.3(11) . . ? C4A C5A Br1A 117.8(12) . . ? C5A C6A C1A 119.5(13) . . ? O2A C7A C3A 105.3(11) . . ? O2A C8A C9A 105.7(10) . . ? C14A C9A C10A 120.1(13) . . ? C14A C9A C8A 123.1(13) . . ? C10A C9A C8A 116.6(13) . . ? O3A C10A C11A 117.1(12) . . ? O3A C10A C9A 121.3(13) . . ? C11A C10A C9A 121.6(13) . . ? C10A C11A C12A 118.5(13) . . ? C10A C11A C15A 119.7(13) . . ? C12A C11A C15A 121.2(14) . . ? C13A C12A C11A 116.2(13) . . ? C14A C13A C12A 122.6(14) . . ? C14A C13A Br2A 119.9(12) . . ? C12A C13A Br2A 117.5(11) . . ? C9A C14A C13A 120.2(14) . . ? O4A C15A C11A 108.0(11) . . ? O4A C16A C17A 108.0(11) . . ? C18A C17A C22A 120.3(17) . . ? C18A C17A C16A 121.9(13) . . ? C22A C17A C16A 117.7(17) . . ? C19A C18A O5A 119.8(14) . . ? C19A C18A C17A 123.3(14) . . ? O5A C18A C17A 116.9(14) . . ? C18A C19A C20A 117.6(15) . . ? C18A C19A C23A 121.0(14) . . ? C20A C19A C23A 121.3(15) . . ? C21A C20A C19A 119.1(15) . . ? C20A C21A C22A 125.3(16) . . ? C20A C21A Br3A 124.7(12) . . ? C22A C21A Br3A 109.9(13) . . ? C21A C22A C17A 114.4(17) . . ? C19A C23A O6A 109.7(12) . . ? C1A C24A O6A 107.0(11) . . ? O8B U2 O7B 178.6(5) . . ? O8B U2 O1B 96.7(4) . . ? O7B U2 O1B 84.7(5) . . ? O8B U2 O5B 91.3(4) . . ? O7B U2 O5B 88.3(4) . . ? O1B U2 O5B 117.4(4) . . ? O8B U2 O3B 93.2(4) . . ? O7B U2 O3B 85.7(5) . . ? O1B U2 O3B 132.2(4) . . ? O5B U2 O3B 109.0(4) . . ? O8B U2 O2B 74.6(4) . . ? O7B U2 O2B 105.7(4) . . ? O1B U2 O2B 69.4(3) . . ? O5B U2 O2B 165.3(3) . . ? O3B U2 O2B 68.5(3) . . ? C2B O1B U2 118.2(8) . . ? C8B O2B C7B 116.8(10) . . ? C8B O2B U2 121.9(9) . . ? C7B O2B U2 117.5(8) . . ? C10B O3B U2 118.3(8) . . ? C15B O4B C16B 114.1(12) . . ? C18B O5B U2 125.9(9) . . ? C23B O6B C24B 111.1(11) . . ? C6B C1B C2B 116.2(15) . . ? C6B C1B C24B 124.4(16) . . ? C2B C1B C24B 119.3(14) . . ? C3B C2B O1B 121.2(15) . . ? C3B C2B C1B 122.7(14) . . ? O1B C2B C1B 116.0(13) . . ? C2B C3B C4B 118.0(14) . . ? C2B C3B C7B 116.7(14) . . ? C4B C3B C7B 125.2(13) . . ? C5B C4B C3B 120.7(14) . . ? C6B C5B C4B 119.6(16) . . ? C6B C5B Br1B 120.3(13) . . ? C4B C5B Br1B 119.9(11) . . ? C5B C6B C1B 122.5(18) . . ? O2B C7B C3B 110.6(10) . . ? O2B C8B C9B 110.6(11) . . ? C14B C9B C10B 121.2(14) . . ? C14B C9B C8B 120.7(14) . . ? C10B C9B C8B 118.0(13) . . ? O3B C10B C9B 120.7(13) . . ? O3B C10B C11B 118.1(13) . . ? C9B C10B C11B 121.2(13) . . ? C12B C11B C10B 117.8(13) . . ? C12B C11B C15B 123.2(14) . . ? C10B C11B C15B 118.0(13) . . ? C13B C12B C11B 118.6(13) . . ? C12B C13B C14B 123.3(13) . . ? C12B C13B Br2B 119.7(11) . . ? C14B C13B Br2B 116.9(12) . . ? C9B C14B C13B 117.7(13) . . ? O4B C15B C11B 108.0(11) . . ? C17B C16B O4B 104.4(13) . . ? C22B C17B C18B 120.0(18) . . ? C22B C17B C16B 121.9(16) . . ? C18B C17B C16B 118.1(16) . . ? O5B C18B C19B 122.9(15) . . ? O5B C18B C17B 117.6(18) . . ? C19B C18B C17B 119.6(16) . . ? C20B C19B C18B 121.8(17) . . ? C20B C19B C23B 119.6(18) . . ? C18B C19B C23B 118.4(15) . . ? C19B C20B C21B 117.6(18) . . ? C22B C21B C20B 122.4(17) . . ? C22B C21B Br3B 123.2(12) . . ? C20B C21B Br3B 114.2(15) . . ? C21B C22B C17B 118.5(16) . . ? O6B C23B C19B 105.6(12) . . ? O6B C24B C1B 101.9(12) . . ? O9 Ba O8 63.9(6) . . ? O9 Ba O5 119.9(6) . . ? O8 Ba O5 152.2(6) . . ? O9 Ba O10 63.1(8) . . ? O8 Ba O10 127.0(7) . . ? O5 Ba O10 63.0(7) . . ? O9 Ba O7 99.8(7) . . ? O8 Ba O7 63.0(5) . . ? O5 Ba O7 89.8(4) . . ? O10 Ba O7 124.8(6) . . ? O9 Ba O1 100.3(6) . . ? O8 Ba O1 131.8(5) . . ? O5 Ba O1 75.9(4) . . ? O10 Ba O1 61.7(5) . . ? O7 Ba O1 159.3(4) . . ? O9 Ba O6 81.1(7) . . ? O8 Ba O6 99.3(6) . . ? O5 Ba O6 57.2(4) . . ? O10 Ba O6 70.3(6) . . ? O7 Ba O6 54.8(4) . . ? O1 Ba O6 124.1(4) . . ? O9 Ba O2 83.9(7) . . ? O8 Ba O2 73.4(5) . . ? O5 Ba O2 132.9(4) . . ? O10 Ba O2 103.2(6) . . ? O7 Ba O2 128.1(4) . . ? O1 Ba O2 59.3(4) . . ? O6 Ba O2 165.0(4) . . ? O9 Ba O3 123.4(7) . . ? O8 Ba O3 68.0(6) . . ? O5 Ba O3 116.7(5) . . ? O10 Ba O3 151.5(6) . . ? O7 Ba O3 83.0(5) . . ? O1 Ba O3 90.0(5) . . ? O6 Ba O3 135.7(5) . . ? O2 Ba O3 54.4(5) . . ? O9 Ba O4 174.1(7) . . ? O8 Ba O4 119.7(6) . . ? O5 Ba O4 54.6(5) . . ? O10 Ba O4 112.8(7) . . ? O7 Ba O4 78.9(5) . . ? O1 Ba O4 80.6(5) . . ? O6 Ba O4 93.6(5) . . ? O2 Ba O4 101.4(5) . . ? O3 Ba O4 62.3(6) . . ? C20 O1 C1 115.8(19) . . ? C20 O1 Ba 117.8(12) . . ? C1 O1 Ba 114.5(12) . . ? C2 O2 C3 133.8(15) . . ? C2 O2 Ba 117.7(11) . . ? C3 O2 Ba 108.5(13) . . ? C5 O3 C4 113(2) . . ? C5 O3 Ba 114.9(14) . . ? C4 O3 Ba 117.7(16) . . ? C7 O4 C6 116.2(17) . . ? C7 O4 Ba 127.8(13) . . ? C6 O4 Ba 113.4(14) . . ? C8 O5 C9 108.1(18) . . ? C8 O5 Ba 120.8(12) . . ? C9 O5 Ba 123.8(12) . . ? C10 O6 C11 115(2) . . ? C10 O6 Ba 113.5(17) . . ? C11 O6 Ba 121.1(13) . . ? C13 O7 C12 111.2(14) . . ? C13 O7 Ba 110.1(11) . . ? C12 O7 Ba 112.8(11) . . ? C15 O8 C14 127(2) . . ? C15 O8 Ba 113.6(15) . . ? C14 O8 Ba 110.3(17) . . ? C16 O9 C17 133(4) . . ? C16 O9 Ba 119(3) . . ? C17 O9 Ba 103(2) . . ? C18 O10 C19 129(2) . . ? C18 O10 Ba 115.1(17) . . ? C19 O10 Ba 110.4(18) . . ? C2 C1 O1 116.0(17) . . ? C1 C2 O2 112.2(18) . . ? O2 C3 C4 96.3(16) . . ? O3 C4 C3 110.1(18) . . ? O3 C5 C6 122(2) . . ? O4 C6 C5 115.5(11) . . ? O4 C7 C8 100.3(17) . . ? O5 C8 C7 115.6(11) . . ? C10 C9 O5 107(2) . . ? C9 C10 O6 115(3) . . ? C12 C11 O6 104.0(19) . . ? C11 C12 O7 99.2(18) . . ? O7 C13 C14 108(2) . . ? O8 C14 C13 126(2) . . ? O8 C15 C16 122(3) . . ? O9 C16 C15 116.7(12) . . ? O9 C17 C18 115(3) . . ? O10 C18 C17 100(3) . . ? C20 C19 O10 114(3) . . ? O1 C20 C19 116(3) . . ? Cl2 C21 Cl1 110.8(8) . . ? Cl2 C21 Cl3 109.6(9) . . ? Cl1 C21 Cl3 105.9(9) . . ? Cl4 C22 Cl6 110.5(13) . . ? Cl4 C22 Cl5 107.2(12) . . ? Cl6 C22 Cl5 108.2(12) . . ? #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 638700' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H96 Ba2 O22 S4 U2' _chemical_formula_weight 2264.53 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' Ba Ba -0.3244 2.2819 '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.223(3) _cell_length_b 18.754(3) _cell_length_c 16.684(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.362(9) _cell_angle_gamma 90.00 _cell_volume 4570.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 113150 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 4.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.498 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 100(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 five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 113150 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8654 _reflns_number_gt 5584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some C atoms in the DMSO and methanol molecules. The H atom bound to O11 was found on a Fourier-difference map and all the others were introduced at calculated positions. All were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (OH, CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Some voids in the lattice likely indicate the presence of 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^)+(0.0911P)^2^] 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 8654 _refine_ls_number_parameters 496 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.946 _refine_diff_density_min -1.164 _refine_diff_density_rms 0.188 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 0.40865(3) 0.14078(2) 0.46975(2) 0.04192(16) Uani 1 1 d . . . Ba Ba 0.35020(4) -0.04962(4) 0.41295(4) 0.0457(2) Uani 1 1 d . . . S1 S 0.4522(3) -0.1484(2) 0.2396(2) 0.0897(13) Uani 1 1 d . . . S2 S 0.1906(3) -0.1884(2) 0.2637(2) 0.0856(11) Uani 1 1 d . . . O1 O 0.3922(4) 0.1957(4) 0.5827(4) 0.0486(19) Uani 1 1 d . . . O2 O 0.2679(4) 0.0904(4) 0.4499(4) 0.0422(17) Uani 1 1 d . . . O3 O 0.2298(4) 0.0291(4) 0.2807(4) 0.0387(16) Uani 1 1 d . . . O4 O 0.4129(4) 0.0742(4) 0.3575(4) 0.0485(19) Uani 1 1 d . . . O5 O 0.5605(4) 0.1551(4) 0.4792(4) 0.0471(18) Uani 1 1 d . . . O6 O 0.5111(4) 0.3015(4) 0.5282(4) 0.0499(19) Uani 1 1 d . . . O7 O 0.4512(4) 0.0625(4) 0.5332(4) 0.0417(17) Uani 1 1 d . . . O8 O 0.3640(4) 0.2144(4) 0.4025(4) 0.0453(18) Uani 1 1 d . . . O9 O 0.3933(6) -0.1158(6) 0.2880(5) 0.076(3) Uani 1 1 d U . . O10 O 0.2155(6) -0.1411(4) 0.3413(5) 0.065(2) Uani 1 1 d . . . O11 O 0.2433(5) -0.0594(4) 0.5129(5) 0.0593(17) Uani 1 1 d U . . H11 H 0.2809 -0.0329 0.5611 0.071 Uiso 1 1 d R . . C1 C 0.3923(7) 0.3189(6) 0.5948(5) 0.044(3) Uani 1 1 d . . . C2 C 0.3456(7) 0.2560(6) 0.5827(6) 0.040(2) Uani 1 1 d . . . C3 C 0.2517(7) 0.2548(6) 0.5726(6) 0.044(3) Uani 1 1 d . . . C4 C 0.2079(8) 0.3178(6) 0.5787(6) 0.050(3) Uani 1 1 d . . . H4 H 0.1453 0.3164 0.5729 0.060 Uiso 1 1 calc R . . C5 C 0.2526(8) 0.3843(7) 0.5933(7) 0.053(3) Uani 1 1 d . . . C6 C 0.3448(8) 0.3858(7) 0.5996(6) 0.051(3) Uani 1 1 d . . . H6 H 0.3764 0.4289 0.6067 0.062 Uiso 1 1 calc R . . C7 C 0.2024(9) 0.4520(7) 0.5961(9) 0.078(4) Uani 1 1 d . . . H7A H 0.1377 0.4436 0.5755 0.117 Uiso 1 1 calc R . . H7B H 0.2202 0.4871 0.5619 0.117 Uiso 1 1 calc R . . H7C H 0.2168 0.4688 0.6526 0.117 Uiso 1 1 calc R . . C8 C 0.2006(7) 0.1867(7) 0.5596(6) 0.051(3) Uani 1 1 d . . . H8A H 0.1565 0.1883 0.5917 0.061 Uiso 1 1 calc R . . H8B H 0.2434 0.1486 0.5825 0.061 Uiso 1 1 calc R . . C9 C 0.1491(7) 0.1672(7) 0.4685(6) 0.052(3) Uani 1 1 d . . . C10 C 0.1805(7) 0.1160(6) 0.4219(6) 0.046(3) Uani 1 1 d . . . C11 C 0.1211(7) 0.0942(6) 0.3475(6) 0.041(2) Uani 1 1 d . . . C12 C 0.0359(7) 0.1246(7) 0.3156(7) 0.053(3) Uani 1 1 d . . . H12 H -0.0023 0.1073 0.2657 0.063 Uiso 1 1 calc R . . C13 C 0.0047(7) 0.1815(7) 0.3567(7) 0.060(3) Uani 1 1 d . . . C14 C 0.0624(7) 0.1970(7) 0.4345(6) 0.054(3) Uani 1 1 d . . . H14 H 0.0421 0.2299 0.4670 0.065 Uiso 1 1 calc R . . C15 C -0.0885(8) 0.2153(7) 0.3205(8) 0.073(4) Uani 1 1 d . . . H15A H -0.1012 0.2473 0.3607 0.110 Uiso 1 1 calc R . . H15B H -0.1344 0.1787 0.3070 0.110 Uiso 1 1 calc R . . H15C H -0.0889 0.2412 0.2707 0.110 Uiso 1 1 calc R . . C16 C 0.1464(6) 0.0308(6) 0.3019(6) 0.043(2) Uani 1 1 d . . . H16A H 0.1452 -0.0110 0.3358 0.051 Uiso 1 1 calc R . . H16B H 0.0976 0.0249 0.2505 0.051 Uiso 1 1 calc R . . C17 C 0.2424(6) 0.0916(6) 0.2388(6) 0.043(3) Uani 1 1 d . . . H17A H 0.2428 0.1324 0.2746 0.051 Uiso 1 1 calc R . . H17B H 0.1915 0.0972 0.1889 0.051 Uiso 1 1 calc R . . C18 C 0.3316(7) 0.0896(6) 0.2146(6) 0.044(3) Uani 1 1 d . . . C19 C 0.4142(7) 0.0869(6) 0.2778(6) 0.043(3) Uani 1 1 d . . . C20 C 0.4970(7) 0.0934(6) 0.2593(6) 0.046(3) Uani 1 1 d . . . C21 C 0.4958(7) 0.1051(6) 0.1749(6) 0.045(3) Uani 1 1 d . . . H21 H 0.5507 0.1126 0.1621 0.054 Uiso 1 1 calc R . . C22 C 0.4154(7) 0.1057(6) 0.1119(6) 0.049(3) Uani 1 1 d . . . C23 C 0.3335(7) 0.0974(7) 0.1332(6) 0.052(3) Uani 1 1 d . . . H23 H 0.2786 0.0971 0.0909 0.063 Uiso 1 1 calc R . . C24 C 0.4154(9) 0.1203(8) 0.0185(7) 0.071(4) Uani 1 1 d . . . H24A H 0.4414 0.0802 -0.0022 0.107 Uiso 1 1 calc R . . H24B H 0.4511 0.1621 0.0165 0.107 Uiso 1 1 calc R . . H24C H 0.3537 0.1276 -0.0154 0.107 Uiso 1 1 calc R . . C25 C 0.5875(7) 0.0972(6) 0.3251(6) 0.049(3) Uani 1 1 d . . . H25A H 0.6349 0.0794 0.3017 0.059 Uiso 1 1 calc R . . H25B H 0.5855 0.0662 0.3711 0.059 Uiso 1 1 calc R . . C26 C 0.6138(7) 0.1729(6) 0.3593(6) 0.046(3) Uani 1 1 d . . . C27 C 0.5981(6) 0.1981(6) 0.4327(6) 0.041(3) Uani 1 1 d . . . C28 C 0.6214(7) 0.2663(7) 0.4578(6) 0.047(3) Uani 1 1 d . . . C29 C 0.6599(7) 0.3111(6) 0.4102(6) 0.043(3) Uani 1 1 d . . . H29 H 0.6745 0.3577 0.4281 0.052 Uiso 1 1 calc R . . C30 C 0.6769(7) 0.2886(6) 0.3374(6) 0.048(3) Uani 1 1 d . . . C31 C 0.6536(6) 0.2203(6) 0.3119(6) 0.046(3) Uani 1 1 d . . . H31 H 0.6638 0.2042 0.2626 0.056 Uiso 1 1 calc R . . C32 C 0.7155(8) 0.3402(7) 0.2831(7) 0.060(3) Uani 1 1 d . . . H32A H 0.7520 0.3139 0.2549 0.091 Uiso 1 1 calc R . . H32B H 0.7527 0.3758 0.3182 0.091 Uiso 1 1 calc R . . H32C H 0.6657 0.3629 0.2427 0.091 Uiso 1 1 calc R . . C33 C 0.6055(7) 0.2911(7) 0.5382(6) 0.050(3) Uani 1 1 d . . . H33A H 0.6292 0.2559 0.5815 0.060 Uiso 1 1 calc R . . H33B H 0.6381 0.3355 0.5556 0.060 Uiso 1 1 calc R . . C34 C 0.4954(7) 0.3208(7) 0.6058(7) 0.059(3) Uani 1 1 d . . . H34A H 0.5190 0.3682 0.6220 0.071 Uiso 1 1 calc R . . H34B H 0.5264 0.2876 0.6491 0.071 Uiso 1 1 calc R . . C35 C 0.5556(11) -0.0907(10) 0.2631(10) 0.106(5) Uani 1 1 d U . . H35A H 0.5374 -0.0418 0.2527 0.159 Uiso 1 1 calc R . . H35B H 0.5933 -0.1042 0.2282 0.159 Uiso 1 1 calc R . . H35C H 0.5896 -0.0963 0.3207 0.159 Uiso 1 1 calc R . . C36 C 0.4030(12) -0.1152(11) 0.1332(9) 0.110(5) Uani 1 1 d U . . H36A H 0.3642 -0.1512 0.1003 0.165 Uiso 1 1 calc R . . H36B H 0.4513 -0.1039 0.1088 0.165 Uiso 1 1 calc R . . H36C H 0.3675 -0.0732 0.1347 0.165 Uiso 1 1 calc R . . C37 C 0.1573(12) -0.1309(10) 0.1769(10) 0.107(6) Uani 1 1 d U . . H37A H 0.1111 -0.0987 0.1841 0.161 Uiso 1 1 calc R . . H37B H 0.1332 -0.1585 0.1271 0.161 Uiso 1 1 calc R . . H37C H 0.2094 -0.1042 0.1722 0.161 Uiso 1 1 calc R . . C38 C 0.0756(9) -0.2207(8) 0.2576(9) 0.086(5) Uani 1 1 d . . . H38A H 0.0774 -0.2482 0.3066 0.129 Uiso 1 1 calc R . . H38B H 0.0539 -0.2501 0.2089 0.129 Uiso 1 1 calc R . . H38C H 0.0351 -0.1809 0.2542 0.129 Uiso 1 1 calc R . . C39 C 0.1634(7) -0.0854(7) 0.5360(7) 0.0578(18) Uani 1 1 d U . . H39A H 0.1087 -0.0712 0.4943 0.087 Uiso 1 1 calc R . . H39B H 0.1632 -0.0656 0.5890 0.087 Uiso 1 1 calc R . . H39C H 0.1658 -0.1365 0.5399 0.087 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 0.0431(2) 0.0433(3) 0.0349(2) 0.00152(17) 0.00364(16) 0.00136(18) Ba 0.0460(4) 0.0454(4) 0.0389(4) 0.0014(3) 0.0008(3) -0.0007(3) S1 0.118(3) 0.090(3) 0.060(2) -0.007(2) 0.023(2) 0.012(3) S2 0.086(2) 0.075(3) 0.088(3) -0.009(2) 0.011(2) -0.008(2) O1 0.041(4) 0.053(5) 0.047(4) -0.011(4) 0.004(3) -0.005(4) O2 0.039(4) 0.048(5) 0.035(4) 0.000(3) 0.003(3) -0.001(3) O3 0.039(4) 0.044(5) 0.032(3) 0.000(3) 0.009(3) -0.001(3) O4 0.043(4) 0.056(5) 0.040(4) 0.008(3) 0.002(3) -0.003(4) O5 0.039(4) 0.053(5) 0.046(4) 0.005(4) 0.007(3) 0.002(3) O6 0.045(4) 0.056(5) 0.048(4) -0.008(4) 0.013(3) -0.005(4) O7 0.045(4) 0.045(5) 0.030(3) 0.001(3) 0.002(3) 0.003(3) O8 0.045(4) 0.038(5) 0.044(4) 0.006(3) -0.003(3) 0.003(3) O9 0.072(5) 0.104(7) 0.052(4) -0.011(5) 0.019(4) 0.009(5) O10 0.070(5) 0.060(6) 0.056(5) 0.002(4) -0.001(4) -0.012(4) O11 0.052(3) 0.062(3) 0.068(3) 0.002(2) 0.024(2) 0.001(2) C1 0.055(6) 0.042(7) 0.026(5) 0.000(5) -0.001(4) 0.002(5) C2 0.052(6) 0.031(6) 0.038(5) -0.001(5) 0.016(5) -0.011(5) C3 0.055(7) 0.045(7) 0.034(5) 0.005(5) 0.018(5) -0.008(5) C4 0.058(7) 0.047(8) 0.047(6) -0.004(5) 0.017(5) -0.009(6) C5 0.054(7) 0.053(8) 0.055(7) -0.010(6) 0.021(5) 0.010(6) C6 0.060(7) 0.036(7) 0.050(6) 0.003(5) 0.005(5) -0.011(6) C7 0.073(9) 0.063(11) 0.109(11) 0.005(8) 0.044(8) 0.009(8) C8 0.057(6) 0.064(9) 0.029(5) 0.000(5) 0.008(4) -0.009(6) C9 0.037(6) 0.075(9) 0.038(6) -0.004(6) 0.004(4) -0.005(6) C10 0.049(6) 0.046(7) 0.041(6) 0.006(5) 0.011(5) -0.006(5) C11 0.048(6) 0.038(6) 0.034(5) 0.012(5) 0.007(4) -0.002(5) C12 0.044(6) 0.067(9) 0.042(6) -0.006(6) 0.004(5) -0.003(6) C13 0.041(6) 0.072(10) 0.058(7) -0.010(6) 0.000(5) 0.014(6) C14 0.056(7) 0.054(8) 0.046(6) -0.013(6) 0.005(5) 0.014(6) C15 0.061(8) 0.061(10) 0.084(9) -0.005(7) -0.001(6) 0.027(7) C16 0.042(6) 0.039(6) 0.041(5) 0.002(5) 0.001(4) -0.004(5) C17 0.035(5) 0.054(7) 0.035(5) 0.001(5) 0.002(4) 0.014(5) C18 0.050(6) 0.041(7) 0.036(5) 0.005(5) 0.005(4) -0.002(5) C19 0.042(6) 0.045(7) 0.038(6) -0.009(5) 0.004(4) -0.003(5) C20 0.055(6) 0.054(8) 0.030(5) -0.003(5) 0.013(4) -0.006(6) C21 0.051(6) 0.044(7) 0.038(5) -0.014(5) 0.009(4) -0.016(5) C22 0.059(7) 0.041(7) 0.046(6) 0.003(5) 0.014(5) 0.005(6) C23 0.045(6) 0.072(9) 0.029(5) -0.002(5) -0.007(4) 0.014(6) C24 0.073(8) 0.096(11) 0.044(7) 0.001(7) 0.015(6) -0.016(8) C25 0.045(6) 0.053(8) 0.042(6) -0.005(5) 0.002(5) 0.005(6) C26 0.040(6) 0.053(8) 0.040(6) 0.005(5) 0.006(4) -0.001(5) C27 0.032(5) 0.054(8) 0.035(5) -0.006(5) 0.007(4) 0.006(5) C28 0.054(6) 0.051(8) 0.032(5) 0.002(5) 0.006(5) 0.002(6) C29 0.044(6) 0.039(7) 0.041(6) -0.014(5) 0.003(4) -0.005(5) C30 0.044(6) 0.046(7) 0.050(6) 0.013(5) 0.008(5) 0.006(5) C31 0.040(6) 0.052(8) 0.045(6) 0.006(5) 0.010(5) 0.010(5) C32 0.063(7) 0.075(9) 0.043(6) -0.011(6) 0.015(5) -0.020(7) C33 0.048(6) 0.070(9) 0.031(5) -0.004(5) 0.008(4) -0.025(6) C34 0.049(7) 0.058(9) 0.075(8) -0.017(7) 0.023(6) -0.008(6) C35 0.118(9) 0.104(10) 0.110(8) 0.011(7) 0.054(7) 0.009(8) C36 0.116(9) 0.126(10) 0.085(8) -0.009(8) 0.024(7) 0.012(8) C37 0.114(9) 0.109(10) 0.101(9) 0.009(7) 0.032(7) 0.003(7) C38 0.069(9) 0.082(12) 0.098(11) -0.037(9) 0.009(7) -0.015(8) C39 0.050(3) 0.061(3) 0.067(3) 0.002(2) 0.025(2) 0.001(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 O8 1.789(7) . ? U O7 1.819(7) . ? U O1 2.223(7) . ? U O4 2.267(7) . ? U O2 2.279(6) . ? U O5 2.289(7) . ? U Ba 3.7370(9) . ? U Ba 4.0225(9) 3_656 ? Ba O11 2.644(7) . ? Ba O9 2.662(8) . ? Ba O10 2.683(8) . ? Ba O5 2.760(7) 3_656 ? Ba O4 2.767(8) . ? Ba O3 2.851(6) . ? Ba O7 2.911(6) 3_656 ? Ba O7 3.013(7) . ? Ba O2 3.046(7) . ? Ba U 4.0225(9) 3_656 ? S1 O9 1.496(9) . ? S1 C36 1.830(16) . ? S1 C35 1.859(17) . ? S2 O10 1.526(9) . ? S2 C37 1.762(17) . ? S2 C38 1.828(13) . ? O1 C2 1.335(12) . ? O2 C10 1.367(12) . ? O3 C17 1.404(12) . ? O3 C16 1.412(11) . ? O4 C19 1.356(12) . ? O5 C27 1.353(12) . ? O5 Ba 2.760(7) 3_656 ? O6 C33 1.413(11) . ? O6 C34 1.427(13) . ? O7 Ba 2.911(6) 3_656 ? O11 C39 1.459(12) . ? C1 C2 1.362(14) . ? C1 C6 1.463(15) . ? C1 C34 1.528(14) . ? C2 C3 1.391(14) . ? C3 C4 1.375(15) . ? C3 C8 1.478(15) . ? C4 C5 1.409(16) . ? C5 C6 1.378(15) . ? C5 C7 1.490(16) . ? C8 C9 1.546(13) . ? C9 C14 1.398(14) . ? C9 C10 1.401(16) . ? C10 C11 1.376(13) . ? C11 C12 1.379(14) . ? C11 C16 1.517(14) . ? C12 C13 1.420(16) . ? C13 C14 1.378(14) . ? C13 C15 1.516(14) . ? C17 C18 1.523(14) . ? C18 C23 1.374(14) . ? C18 C19 1.396(13) . ? C19 C20 1.386(14) . ? C20 C21 1.420(13) . ? C20 C25 1.502(13) . ? C21 C22 1.371(13) . ? C22 C23 1.398(15) . ? C22 C24 1.581(15) . ? C25 C26 1.540(16) . ? C26 C27 1.394(14) . ? C26 C31 1.434(15) . ? C27 C28 1.362(15) . ? C28 C29 1.394(15) . ? C28 C33 1.503(14) . ? C29 C30 1.377(14) . ? C30 C31 1.365(15) . ? C30 C32 1.550(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 U O7 176.8(3) . . ? O8 U O1 93.5(3) . . ? O7 U O1 89.2(3) . . ? O8 U O4 90.1(3) . . ? O7 U O4 87.1(3) . . ? O1 U O4 172.7(3) . . ? O8 U O2 93.1(3) . . ? O7 U O2 85.2(3) . . ? O1 U O2 89.4(2) . . ? O4 U O2 84.0(2) . . ? O8 U O5 98.7(3) . . ? O7 U O5 82.4(3) . . ? O1 U O5 103.9(2) . . ? O4 U O5 81.8(2) . . ? O2 U O5 161.6(3) . . ? O11 Ba O9 142.4(3) . . ? O11 Ba O10 73.0(3) . . ? O9 Ba O10 71.3(3) . . ? O11 Ba O5 79.4(2) . 3_656 ? O9 Ba O5 89.5(3) . 3_656 ? O10 Ba O5 90.4(2) . 3_656 ? O11 Ba O4 126.9(2) . . ? O9 Ba O4 86.9(3) . . ? O10 Ba O4 132.9(2) . . ? O5 Ba O4 131.8(2) 3_656 . ? O11 Ba O3 98.5(2) . . ? O9 Ba O3 83.2(2) . . ? O10 Ba O3 75.1(2) . . ? O5 Ba O3 165.2(2) 3_656 . ? O4 Ba O3 60.89(18) . . ? O11 Ba O7 124.8(2) . 3_656 ? O9 Ba O7 74.9(2) . 3_656 ? O10 Ba O7 133.0(2) . 3_656 ? O5 Ba O7 57.4(2) 3_656 3_656 ? O4 Ba O7 75.35(19) . 3_656 ? O3 Ba O7 131.83(18) . 3_656 ? O11 Ba O7 85.3(2) . . ? O9 Ba O7 130.9(2) . . ? O10 Ba O7 157.8(2) . . ? O5 Ba O7 90.1(2) 3_656 . ? O4 Ba O7 58.49(18) . . ? O3 Ba O7 104.47(19) . . ? O7 Ba O7 64.0(2) 3_656 . ? O11 Ba O2 64.6(2) . . ? O9 Ba O2 140.0(2) . . ? O10 Ba O2 109.6(2) . . ? O5 Ba O2 129.85(19) 3_656 . ? O4 Ba O2 62.9(2) . . ? O3 Ba O2 59.92(17) . . ? O7 Ba O2 117.38(18) 3_656 . ? O7 Ba O2 54.91(17) . . ? U Ba U 99.396(17) . 3_656 ? O9 S1 C36 104.0(7) . . ? O9 S1 C35 104.4(7) . . ? C36 S1 C35 95.6(8) . . ? O10 S2 C37 106.7(7) . . ? O10 S2 C38 104.2(6) . . ? C37 S2 C38 96.2(8) . . ? C2 O1 U 125.4(6) . . ? C10 O2 U 133.5(7) . . ? C10 O2 Ba 130.5(6) . . ? U O2 Ba 87.9(2) . . ? C17 O3 C16 111.4(7) . . ? C17 O3 Ba 132.0(5) . . ? C16 O3 Ba 104.2(5) . . ? C19 O4 U 136.5(7) . . ? C19 O4 Ba 125.2(6) . . ? U O4 Ba 95.3(2) . . ? C27 O5 U 127.8(6) . . ? C27 O5 Ba 126.3(6) . 3_656 ? U O5 Ba 105.3(3) . 3_656 ? C33 O6 C34 110.6(7) . . ? U O7 Ba 114.5(3) . 3_656 ? U O7 Ba 98.3(2) . . ? Ba O7 Ba 116.0(2) 3_656 . ? S1 O9 Ba 158.6(5) . . ? S2 O10 Ba 136.5(5) . . ? C39 O11 Ba 153.7(7) . . ? C2 C1 C6 120.4(10) . . ? C2 C1 C34 120.9(10) . . ? C6 C1 C34 118.7(10) . . ? O1 C2 C1 118.5(9) . . ? O1 C2 C3 121.0(9) . . ? C1 C2 C3 120.5(10) . . ? C4 C3 C2 118.7(10) . . ? C4 C3 C8 120.4(10) . . ? C2 C3 C8 120.8(10) . . ? C3 C4 C5 123.5(11) . . ? C6 C5 C4 117.7(11) . . ? C6 C5 C7 120.0(12) . . ? C4 C5 C7 122.2(10) . . ? C5 C6 C1 119.1(11) . . ? C3 C8 C9 116.7(9) . . ? C14 C9 C10 118.7(9) . . ? C14 C9 C8 117.6(10) . . ? C10 C9 C8 123.4(10) . . ? O2 C10 C11 122.2(10) . . ? O2 C10 C9 120.2(9) . . ? C11 C10 C9 117.7(10) . . ? C10 C11 C12 122.1(10) . . ? C10 C11 C16 119.4(9) . . ? C12 C11 C16 118.3(9) . . ? C11 C12 C13 122.1(10) . . ? C14 C13 C12 113.7(10) . . ? C14 C13 C15 124.3(11) . . ? C12 C13 C15 121.6(10) . . ? C13 C14 C9 125.2(10) . . ? O3 C16 C11 121.0(8) . . ? O3 C17 C18 111.6(8) . . ? C23 C18 C19 119.0(10) . . ? C23 C18 C17 121.9(8) . . ? C19 C18 C17 118.7(8) . . ? O4 C19 C20 120.0(8) . . ? O4 C19 C18 119.2(9) . . ? C20 C19 C18 120.7(9) . . ? C19 C20 C21 118.5(9) . . ? C19 C20 C25 123.1(9) . . ? C21 C20 C25 118.1(9) . . ? C22 C21 C20 121.4(10) . . ? C21 C22 C23 118.1(9) . . ? C21 C22 C24 120.6(10) . . ? C23 C22 C24 121.2(9) . . ? C18 C23 C22 122.2(9) . . ? C20 C25 C26 113.8(9) . . ? C27 C26 C31 118.5(11) . . ? C27 C26 C25 123.2(10) . . ? C31 C26 C25 118.3(9) . . ? O5 C27 C28 119.9(9) . . ? O5 C27 C26 120.4(10) . . ? C28 C27 C26 119.7(10) . . ? C27 C28 C29 120.4(10) . . ? C27 C28 C33 118.2(10) . . ? C29 C28 C33 121.5(11) . . ? C30 C29 C28 122.1(11) . . ? C31 C30 C29 117.7(10) . . ? C31 C30 C32 120.8(10) . . ? C29 C30 C32 121.4(11) . . ? C30 C31 C26 121.6(10) . . ? O6 C33 C28 110.5(8) . . ? O6 C34 C1 108.3(8) . . ? #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 638701' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H216 K4 O48 U2' _chemical_formula_weight 3203.51 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' K K 0.2009 0.2494 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0923(7) _cell_length_b 24.6602(9) _cell_length_c 25.5672(16) _cell_angle_alpha 90.00 _cell_angle_beta 103.061(3) _cell_angle_gamma 90.00 _cell_volume 7426.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 116766 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange-yellow' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method ? _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 2.370 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.433 _exptl_absorpt_correction_T_max 0.752 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 50 mm' _diffrn_ambient_temperature 100(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 'one \f and five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 116766 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14080 _reflns_number_gt 10501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to water O atoms were found on a Fourier-difference map and all the other ones were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (OH, CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Some voids near atom K2 could indicate the presence of a disordered water ligand which could not be located correctly. 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^)+(0.0433P)^2^+33.0564P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 14080 _refine_ls_number_parameters 854 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _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 1.434 _refine_diff_density_min -1.480 _refine_diff_density_rms 0.115 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 0.048024(19) 0.884442(9) 0.084182(9) 0.02675(8) Uani 1 1 d . . . K1 K -0.08827(12) 0.67770(6) 0.28719(6) 0.0383(3) Uani 1 1 d . . . K2 K -0.10947(18) 1.02275(7) 0.05047(7) 0.0612(5) Uani 1 1 d . . . O1 O -0.0569(3) 0.94191(16) 0.12280(15) 0.0295(9) Uani 1 1 d . . . O2 O 0.2018(3) 0.93146(15) 0.13019(15) 0.0287(9) Uani 1 1 d . . . O3 O 0.3370(3) 0.82045(15) 0.14294(16) 0.0287(9) Uani 1 1 d . . . O4 O 0.1491(3) 0.83101(15) 0.03885(15) 0.0292(9) Uani 1 1 d . . . O5 O -0.1079(3) 0.84391(16) 0.03262(16) 0.0323(10) Uani 1 1 d . . . O6 O -0.2358(3) 0.85252(16) 0.12331(16) 0.0322(10) Uani 1 1 d . . . O7 O 0.0334(4) 0.93487(15) 0.03085(16) 0.0328(10) Uani 1 1 d . . . O8 O 0.0621(3) 0.83578(15) 0.13740(16) 0.0300(9) Uani 1 1 d . . . O9 O 0.0045(5) 0.76416(19) 0.23076(19) 0.0535(13) Uani 1 1 d . . . O10 O -0.0201(4) 0.66252(19) 0.18816(19) 0.0514(13) Uani 1 1 d . . . O11 O 0.1216(4) 0.61468(18) 0.27645(17) 0.0410(11) Uani 1 1 d . . . O12 O -0.0458(4) 0.57071(17) 0.32359(19) 0.0428(11) Uani 1 1 d . . . O13 O -0.2709(4) 0.60064(18) 0.27867(19) 0.0451(12) Uani 1 1 d . . . O14 O -0.3217(4) 0.70019(19) 0.22247(19) 0.0464(12) Uani 1 1 d . . . O15 O -0.2699(4) 0.75111(18) 0.32537(19) 0.0451(12) Uani 1 1 d . . . O16 O -0.1439(4) 0.69641(19) 0.42159(19) 0.0472(12) Uani 1 1 d . . . O17 O 0.0599(4) 0.68553(18) 0.38421(18) 0.0429(11) Uani 1 1 d . . . O18 O 0.0791(5) 0.7928(2) 0.3433(2) 0.0663(16) Uani 1 1 d . . . O19 O 0.0265(5) 1.1116(2) 0.1228(2) 0.0606(14) Uani 1 1 d . . . H19A H 0.0582 1.1345 0.1523 0.073 Uiso 1 1 d R . . H19B H -0.0232 1.1250 0.1020 0.073 Uiso 1 1 d R . . O20 O -0.1843(4) 1.13027(18) 0.0541(2) 0.0525(13) Uani 1 1 d . . . H20A H -0.1653 1.1452 0.0223 0.063 Uiso 1 1 d R . . H20B H -0.2389 1.1492 0.0644 0.063 Uiso 1 1 d R . . O21 O -0.2641(5) 1.0014(2) -0.0531(2) 0.0613(15) Uani 1 1 d . . . H21A H -0.2386 0.9680 -0.0621 0.074 Uiso 1 1 d R . . H21B H -0.2405 1.0233 -0.0754 0.074 Uiso 1 1 d R . . O22 O 0.2541(5) 0.7573(2) 0.2219(2) 0.0716(17) Uani 1 1 d . . . H22A H 0.2968 0.7725 0.2034 0.086 Uiso 1 1 d R . . H22B H 0.1671 0.7559 0.2130 0.086 Uiso 1 1 d R . . O23 O 0.1552(4) 1.1647(2) 0.2165(2) 0.0707(16) Uani 1 1 d . . . H23A H 0.1648 1.1947 0.2373 0.085 Uiso 1 1 d R . . H23B H 0.2131 1.1425 0.2186 0.085 Uiso 1 1 d R . . O24 O -0.1872(4) 0.89895(19) -0.06120(19) 0.0496(13) Uani 1 1 d . . . H24A H -0.1670 0.8869 -0.0255 0.059 Uiso 1 1 d R . . H24B H -0.1233 0.8983 -0.0747 0.059 Uiso 1 1 d R . . C1 C -0.1787(5) 0.9267(2) 0.1832(2) 0.0267(13) Uani 1 1 d . . . C2 C -0.0756(5) 0.9459(2) 0.1727(2) 0.0271(13) Uani 1 1 d . . . C3 C 0.0013(5) 0.9716(2) 0.2142(2) 0.0260(13) Uani 1 1 d . . . C4 C -0.0214(5) 0.9739(2) 0.2653(2) 0.0289(14) Uani 1 1 d . . . H4 H 0.0310 0.9910 0.2926 0.035 Uiso 1 1 calc R . . C5 C -0.1183(5) 0.9519(2) 0.2776(2) 0.0289(14) Uani 1 1 d . . . C6 C -0.1965(5) 0.9291(2) 0.2349(2) 0.0298(14) Uani 1 1 d . . . H6 H -0.2634 0.9148 0.2412 0.036 Uiso 1 1 calc R . . C7 C -0.1416(5) 0.9540(3) 0.3339(3) 0.0347(15) Uani 1 1 d . . . C8 C -0.2497(6) 0.9872(3) 0.3320(3) 0.0451(18) Uani 1 1 d . . . H8A H -0.2677 0.9867 0.3667 0.068 Uiso 1 1 calc R . . H8B H -0.3114 0.9717 0.3059 0.068 Uiso 1 1 calc R . . H8C H -0.2376 1.0239 0.3222 0.068 Uiso 1 1 calc R . . C9 C -0.0463(6) 0.9801(3) 0.3751(3) 0.0411(16) Uani 1 1 d . . . H9A H 0.0234 0.9610 0.3760 0.062 Uiso 1 1 calc R . . H9B H -0.0637 0.9783 0.4099 0.062 Uiso 1 1 calc R . . H9C H -0.0382 1.0173 0.3656 0.062 Uiso 1 1 calc R . . C10 C -0.1599(6) 0.8959(3) 0.3523(3) 0.0453(18) Uani 1 1 d . . . H10A H -0.0912 0.8754 0.3553 0.068 Uiso 1 1 calc R . . H10B H -0.2200 0.8790 0.3266 0.068 Uiso 1 1 calc R . . H10C H -0.1797 0.8971 0.3866 0.068 Uiso 1 1 calc R . . C11 C 0.1099(5) 0.9964(2) 0.2046(2) 0.0270(13) Uani 1 1 d . . . H11A H 0.0990 1.0051 0.1667 0.032 Uiso 1 1 calc R . . H11B H 0.1248 1.0300 0.2246 0.032 Uiso 1 1 calc R . . C12 C 0.2124(5) 0.9596(2) 0.2208(2) 0.0267(13) Uani 1 1 d . . . C13 C 0.2534(5) 0.9292(2) 0.1823(2) 0.0262(13) Uani 1 1 d . . . C14 C 0.3530(5) 0.8979(2) 0.2002(2) 0.0266(13) Uani 1 1 d . . . C15 C 0.4033(5) 0.8951(2) 0.2545(2) 0.0275(13) Uani 1 1 d . . . H15 H 0.4676 0.8736 0.2653 0.033 Uiso 1 1 calc R . . C16 C 0.3626(5) 0.9228(2) 0.2936(2) 0.0280(13) Uani 1 1 d . . . C17 C 0.2668(5) 0.9556(2) 0.2750(2) 0.0276(13) Uani 1 1 d . . . H17 H 0.2382 0.9755 0.2999 0.033 Uiso 1 1 calc R . . C18 C 0.4178(5) 0.9216(2) 0.3536(2) 0.0294(14) Uani 1 1 d . . . C19 C 0.3297(5) 0.9070(3) 0.3864(3) 0.0368(15) Uani 1 1 d . . . H19C H 0.3658 0.9065 0.4239 0.055 Uiso 1 1 calc R . . H19D H 0.2986 0.8718 0.3758 0.055 Uiso 1 1 calc R . . H19E H 0.2699 0.9334 0.3800 0.055 Uiso 1 1 calc R . . C20 C 0.4659(5) 0.9775(2) 0.3717(3) 0.0349(15) Uani 1 1 d . . . H20C H 0.5226 0.9871 0.3524 0.052 Uiso 1 1 calc R . . H20D H 0.4995 0.9767 0.4095 0.052 Uiso 1 1 calc R . . H20E H 0.4059 1.0038 0.3646 0.052 Uiso 1 1 calc R . . C21 C 0.5131(6) 0.8795(3) 0.3665(3) 0.0403(16) Uani 1 1 d . . . H21C H 0.5723 0.8892 0.3488 0.060 Uiso 1 1 calc R . . H21D H 0.4835 0.8445 0.3542 0.060 Uiso 1 1 calc R . . H21E H 0.5432 0.8783 0.4046 0.060 Uiso 1 1 calc R . . C22 C 0.4021(5) 0.8686(2) 0.1603(2) 0.0312(14) Uani 1 1 d . . . H22C H 0.4017 0.8919 0.1297 0.037 Uiso 1 1 calc R . . H22D H 0.4801 0.8588 0.1762 0.037 Uiso 1 1 calc R . . C23 C 0.3657(5) 0.7971(2) 0.0963(2) 0.0310(14) Uani 1 1 d . . . H23C H 0.4389 0.7792 0.1066 0.037 Uiso 1 1 calc R . . H23D H 0.3715 0.8255 0.0708 0.037 Uiso 1 1 calc R . . C24 C 0.2776(5) 0.7569(2) 0.0704(2) 0.0294(14) Uani 1 1 d . . . C25 C 0.1717(5) 0.7762(2) 0.0409(2) 0.0276(13) Uani 1 1 d . . . C26 C 0.0931(5) 0.7393(2) 0.0128(2) 0.0249(13) Uani 1 1 d . . . C27 C 0.1190(5) 0.6845(2) 0.0171(2) 0.0290(14) Uani 1 1 d . . . H27 H 0.0662 0.6602 -0.0020 0.035 Uiso 1 1 calc R . . C28 C 0.2201(5) 0.6637(2) 0.0484(2) 0.0296(14) Uani 1 1 d . . . C29 C 0.2987(5) 0.7019(2) 0.0739(2) 0.0300(14) Uani 1 1 d . . . H29 H 0.3682 0.6898 0.0941 0.036 Uiso 1 1 calc R . . C30 C 0.2460(5) 0.6024(2) 0.0510(3) 0.0321(14) Uani 1 1 d . . . C31 C 0.3202(7) 0.5889(3) 0.0111(3) 0.058(2) Uani 1 1 d . . . H31A H 0.3887 0.6099 0.0197 0.086 Uiso 1 1 calc R . . H31B H 0.2793 0.5974 -0.0247 0.086 Uiso 1 1 calc R . . H31C H 0.3387 0.5510 0.0134 0.086 Uiso 1 1 calc R . . C32 C 0.3066(6) 0.5865(3) 0.1075(3) 0.0463(18) Uani 1 1 d . . . H32A H 0.2620 0.5976 0.1323 0.069 Uiso 1 1 calc R . . H32B H 0.3793 0.6040 0.1166 0.069 Uiso 1 1 calc R . . H32C H 0.3167 0.5479 0.1094 0.069 Uiso 1 1 calc R . . C33 C 0.1380(5) 0.5684(2) 0.0350(3) 0.0370(16) Uani 1 1 d . . . H33A H 0.1563 0.5308 0.0420 0.055 Uiso 1 1 calc R . . H33B H 0.1052 0.5733 -0.0025 0.055 Uiso 1 1 calc R . . H33C H 0.0847 0.5796 0.0555 0.055 Uiso 1 1 calc R . . C34 C -0.0191(5) 0.7581(2) -0.0216(2) 0.0275(13) Uani 1 1 d . . . H34A H -0.0354 0.7377 -0.0549 0.033 Uiso 1 1 calc R . . H34B H -0.0132 0.7961 -0.0304 0.033 Uiso 1 1 calc R . . C35 C -0.1162(5) 0.7509(2) 0.0064(2) 0.0284(13) Uani 1 1 d . . . C36 C -0.1571(5) 0.7945(2) 0.0313(2) 0.0296(14) Uani 1 1 d . . . C37 C -0.2526(5) 0.7875(2) 0.0530(2) 0.0307(14) Uani 1 1 d . . . C38 C -0.2993(5) 0.7357(3) 0.0541(2) 0.0334(15) Uani 1 1 d . . . H38 H -0.3610 0.7312 0.0698 0.040 Uiso 1 1 calc R . . C39 C -0.2564(5) 0.6906(2) 0.0325(2) 0.0296(14) Uani 1 1 d . . . C40 C -0.1671(5) 0.7001(2) 0.0073(2) 0.0291(14) Uani 1 1 d . . . H40 H -0.1401 0.6713 -0.0097 0.035 Uiso 1 1 calc R . . C41 C -0.3065(6) 0.6338(3) 0.0343(3) 0.0383(16) Uani 1 1 d . . . C42 C -0.2104(6) 0.5909(3) 0.0454(3) 0.055(2) Uani 1 1 d . . . H42A H -0.1572 0.5997 0.0782 0.082 Uiso 1 1 calc R . . H42B H -0.1722 0.5908 0.0163 0.082 Uiso 1 1 calc R . . H42C H -0.2423 0.5557 0.0485 0.082 Uiso 1 1 calc R . . C43 C -0.3688(7) 0.6289(3) 0.0799(3) 0.055(2) Uani 1 1 d . . . H43A H -0.3173 0.6369 0.1135 0.082 Uiso 1 1 calc R . . H43B H -0.3973 0.5927 0.0809 0.082 Uiso 1 1 calc R . . H43C H -0.4310 0.6541 0.0740 0.082 Uiso 1 1 calc R . . C44 C -0.3852(6) 0.6216(3) -0.0191(3) 0.0508(19) Uani 1 1 d . . . H44A H -0.4134 0.5853 -0.0190 0.076 Uiso 1 1 calc R . . H44B H -0.3447 0.6253 -0.0472 0.076 Uiso 1 1 calc R . . H44C H -0.4477 0.6466 -0.0253 0.076 Uiso 1 1 calc R . . C45 C -0.3038(5) 0.8353(3) 0.0735(3) 0.0341(15) Uani 1 1 d . . . H45A H -0.3111 0.8647 0.0477 0.041 Uiso 1 1 calc R . . H45B H -0.3791 0.8262 0.0780 0.041 Uiso 1 1 calc R . . C46 C -0.2679(5) 0.9051(2) 0.1377(3) 0.0310(14) Uani 1 1 d . . . H46A H -0.3400 0.9031 0.1481 0.037 Uiso 1 1 calc R . . H46B H -0.2767 0.9293 0.1071 0.037 Uiso 1 1 calc R . . C47 C -0.0779(6) 0.7527(3) 0.1816(3) 0.0446(18) Uani 1 1 d . . . H47A H -0.0908 0.7845 0.1587 0.054 Uiso 1 1 calc R . . H47B H -0.1496 0.7416 0.1892 0.054 Uiso 1 1 calc R . . C48 C -0.0290(6) 0.7088(3) 0.1557(3) 0.0504(19) Uani 1 1 d . . . H48A H -0.0770 0.7013 0.1207 0.060 Uiso 1 1 calc R . . H48B H 0.0455 0.7193 0.1510 0.060 Uiso 1 1 calc R . . C49 C 0.0763(7) 0.6300(3) 0.1828(3) 0.062(2) Uani 1 1 d . . . H49A H 0.1436 0.6524 0.1868 0.074 Uiso 1 1 calc R . . H49B H 0.0617 0.6127 0.1479 0.074 Uiso 1 1 calc R . . C50 C 0.0924(8) 0.5889(3) 0.2256(3) 0.059(2) Uani 1 1 d . . . H50A H 0.0230 0.5683 0.2227 0.071 Uiso 1 1 calc R . . H50B H 0.1523 0.5641 0.2218 0.071 Uiso 1 1 calc R . . C51 C 0.1476(6) 0.5784(3) 0.3205(3) 0.0422(17) Uani 1 1 d . . . H51A H 0.1658 0.5992 0.3535 0.051 Uiso 1 1 calc R . . H51B H 0.2145 0.5576 0.3181 0.051 Uiso 1 1 calc R . . C52 C 0.0536(6) 0.5398(3) 0.3232(3) 0.0501(19) Uani 1 1 d . . . H52A H 0.0399 0.5158 0.2924 0.060 Uiso 1 1 calc R . . H52B H 0.0739 0.5180 0.3555 0.060 Uiso 1 1 calc R . . C53 C -0.1384(6) 0.5360(3) 0.3253(3) 0.0486(19) Uani 1 1 d . . . H53A H -0.1197 0.5133 0.3571 0.058 Uiso 1 1 calc R . . H53B H -0.1534 0.5125 0.2941 0.058 Uiso 1 1 calc R . . C54 C -0.2423(6) 0.5691(3) 0.3263(3) 0.0460(18) Uani 1 1 d . . . H54A H -0.3050 0.5453 0.3286 0.055 Uiso 1 1 calc R . . H54B H -0.2276 0.5926 0.3575 0.055 Uiso 1 1 calc R . . C55 C -0.3779(6) 0.6256(3) 0.2732(3) 0.0459(18) Uani 1 1 d . . . H55A H -0.3774 0.6493 0.3036 0.055 Uiso 1 1 calc R . . H55B H -0.4362 0.5984 0.2720 0.055 Uiso 1 1 calc R . . C56 C -0.4018(6) 0.6578(3) 0.2220(3) 0.0509(19) Uani 1 1 d . . . H56A H -0.4007 0.6337 0.1922 0.061 Uiso 1 1 calc R . . H56B H -0.4772 0.6734 0.2164 0.061 Uiso 1 1 calc R . . C57 C -0.3590(6) 0.7537(3) 0.2322(3) 0.0501(19) Uani 1 1 d . . . H57A H -0.4308 0.7608 0.2073 0.060 Uiso 1 1 calc R . . H57B H -0.3042 0.7798 0.2251 0.060 Uiso 1 1 calc R . . C58 C -0.3734(6) 0.7618(3) 0.2880(3) 0.0470(18) Uani 1 1 d . . . H58A H -0.3969 0.7989 0.2923 0.056 Uiso 1 1 calc R . . H58B H -0.4321 0.7377 0.2947 0.056 Uiso 1 1 calc R . . C59 C -0.2777(6) 0.7613(3) 0.3789(3) 0.0486(19) Uani 1 1 d . . . H59A H -0.3343 0.7375 0.3881 0.058 Uiso 1 1 calc R . . H59B H -0.3022 0.7984 0.3818 0.058 Uiso 1 1 calc R . . C60 C -0.1667(6) 0.7525(3) 0.4175(3) 0.0455(18) Uani 1 1 d . . . H60A H -0.1068 0.7712 0.4051 0.055 Uiso 1 1 calc R . . H60B H -0.1698 0.7670 0.4525 0.055 Uiso 1 1 calc R . . C61 C -0.0373(6) 0.6837(3) 0.4571(3) 0.055(2) Uani 1 1 d . . . H61A H -0.0498 0.6616 0.4866 0.066 Uiso 1 1 calc R . . H61B H 0.0004 0.7169 0.4718 0.066 Uiso 1 1 calc R . . C62 C 0.0350(6) 0.6539(3) 0.4270(3) 0.0474(18) Uani 1 1 d . . . H62A H 0.1055 0.6438 0.4515 0.057 Uiso 1 1 calc R . . H62B H -0.0035 0.6209 0.4124 0.057 Uiso 1 1 calc R . . C63 C 0.1555(6) 0.7199(3) 0.4002(3) 0.0499(19) Uani 1 1 d . . . H63A H 0.2232 0.6983 0.4132 0.060 Uiso 1 1 calc R . . H63B H 0.1450 0.7435 0.4291 0.060 Uiso 1 1 calc R . . C64 C 0.1686(6) 0.7530(3) 0.3532(3) 0.055(2) Uani 1 1 d . . . H64A H 0.2420 0.7708 0.3608 0.066 Uiso 1 1 calc R . . H64B H 0.1632 0.7301 0.3219 0.066 Uiso 1 1 calc R . . C65 C 0.0797(7) 0.8277(3) 0.2999(3) 0.057(2) Uani 1 1 d . . . H65A H 0.1523 0.8249 0.2901 0.069 Uiso 1 1 calc R . . H65B H 0.0711 0.8648 0.3110 0.069 Uiso 1 1 calc R . . C66 C -0.0130(6) 0.8150(3) 0.2520(3) 0.0409(17) Uani 1 1 d . . . H66A H -0.0855 0.8151 0.2623 0.049 Uiso 1 1 calc R . . H66B H -0.0153 0.8427 0.2249 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.03131(13) 0.02368(12) 0.02593(12) 0.00197(11) 0.00791(9) 0.00027(11) K1 0.0361(8) 0.0349(8) 0.0415(8) 0.0084(6) 0.0036(7) -0.0027(6) K2 0.1010(15) 0.0396(9) 0.0524(11) 0.0158(8) 0.0372(10) 0.0213(9) O1 0.032(2) 0.033(2) 0.025(2) 0.0032(18) 0.0085(18) -0.0007(18) O2 0.034(2) 0.026(2) 0.027(2) 0.0029(17) 0.0089(19) -0.0043(18) O3 0.030(2) 0.027(2) 0.031(2) -0.0028(18) 0.0102(19) -0.0027(18) O4 0.031(2) 0.027(2) 0.030(2) 0.0028(18) 0.0085(19) -0.0015(18) O5 0.030(2) 0.030(2) 0.035(2) 0.0021(19) 0.0048(19) 0.0046(19) O6 0.034(2) 0.028(2) 0.034(2) -0.0056(19) 0.0045(19) 0.0027(19) O7 0.042(3) 0.023(2) 0.033(2) 0.0069(18) 0.008(2) 0.0059(19) O8 0.034(2) 0.022(2) 0.035(2) 0.0062(18) 0.0092(19) 0.0018(18) O9 0.070(4) 0.043(3) 0.045(3) 0.002(2) 0.008(3) 0.002(3) O10 0.062(3) 0.046(3) 0.043(3) 0.000(2) 0.008(2) 0.017(3) O11 0.042(3) 0.042(3) 0.038(3) 0.001(2) 0.006(2) 0.007(2) O12 0.039(3) 0.028(2) 0.063(3) 0.002(2) 0.014(2) -0.002(2) O13 0.038(3) 0.046(3) 0.053(3) -0.003(2) 0.016(2) -0.002(2) O14 0.041(3) 0.048(3) 0.051(3) 0.002(2) 0.012(2) 0.003(2) O15 0.044(3) 0.041(3) 0.049(3) -0.001(2) 0.009(2) 0.008(2) O16 0.036(3) 0.048(3) 0.055(3) 0.001(2) 0.004(2) 0.005(2) O17 0.043(3) 0.044(3) 0.040(3) -0.001(2) 0.006(2) -0.003(2) O18 0.060(4) 0.080(4) 0.064(4) 0.022(3) 0.023(3) 0.019(3) O19 0.070(4) 0.060(3) 0.052(3) 0.012(3) 0.015(3) 0.015(3) O20 0.076(4) 0.039(3) 0.053(3) 0.013(2) 0.036(3) 0.015(2) O21 0.075(4) 0.051(3) 0.067(4) 0.009(3) 0.035(3) -0.013(3) O22 0.084(4) 0.071(4) 0.067(4) 0.011(3) 0.031(3) -0.009(3) O23 0.048(3) 0.078(4) 0.089(4) -0.020(3) 0.020(3) 0.006(3) O24 0.047(3) 0.055(3) 0.043(3) 0.008(2) 0.003(2) 0.004(2) C1 0.030(3) 0.020(3) 0.030(3) 0.001(2) 0.008(3) 0.003(3) C2 0.034(3) 0.018(3) 0.030(3) 0.003(2) 0.007(3) 0.005(3) C3 0.028(3) 0.024(3) 0.027(3) 0.002(3) 0.009(3) 0.005(3) C4 0.027(3) 0.026(3) 0.032(3) -0.003(3) 0.002(3) 0.004(3) C5 0.033(4) 0.023(3) 0.031(3) 0.001(3) 0.009(3) 0.005(3) C6 0.029(3) 0.027(3) 0.036(4) 0.003(3) 0.010(3) 0.002(3) C7 0.034(4) 0.037(4) 0.035(4) -0.008(3) 0.012(3) -0.003(3) C8 0.038(4) 0.059(5) 0.041(4) -0.015(4) 0.013(3) 0.000(3) C9 0.044(4) 0.046(4) 0.037(4) -0.005(3) 0.017(3) -0.002(3) C10 0.057(5) 0.044(4) 0.040(4) -0.002(3) 0.022(4) -0.008(3) C11 0.031(3) 0.021(3) 0.029(3) 0.001(3) 0.007(3) 0.000(3) C12 0.028(3) 0.019(3) 0.034(3) 0.001(3) 0.011(3) -0.006(2) C13 0.030(3) 0.023(3) 0.026(3) 0.001(3) 0.007(3) -0.007(3) C14 0.027(3) 0.021(3) 0.032(3) -0.002(2) 0.009(3) -0.004(2) C15 0.027(3) 0.019(3) 0.037(4) 0.000(3) 0.009(3) 0.002(2) C16 0.029(3) 0.022(3) 0.035(3) 0.003(3) 0.011(3) -0.005(3) C17 0.028(3) 0.025(3) 0.031(3) -0.003(3) 0.010(3) -0.004(3) C18 0.030(3) 0.030(3) 0.031(3) 0.001(3) 0.011(3) 0.003(3) C19 0.037(4) 0.040(4) 0.033(4) 0.004(3) 0.008(3) -0.002(3) C20 0.033(4) 0.035(4) 0.037(4) -0.002(3) 0.009(3) -0.004(3) C21 0.049(4) 0.041(4) 0.029(3) 0.001(3) 0.006(3) 0.008(3) C22 0.029(3) 0.031(3) 0.035(4) -0.003(3) 0.009(3) -0.002(3) C23 0.032(3) 0.028(3) 0.035(4) -0.005(3) 0.011(3) 0.000(3) C24 0.032(3) 0.029(3) 0.030(3) -0.003(3) 0.012(3) 0.001(3) C25 0.035(4) 0.026(3) 0.025(3) 0.002(3) 0.014(3) 0.000(3) C26 0.025(3) 0.030(3) 0.022(3) 0.001(2) 0.009(3) 0.002(3) C27 0.032(3) 0.029(3) 0.029(3) -0.003(3) 0.013(3) -0.003(3) C28 0.033(4) 0.031(3) 0.027(3) 0.003(3) 0.012(3) 0.004(3) C29 0.028(3) 0.035(4) 0.027(3) -0.003(3) 0.006(3) 0.004(3) C30 0.037(4) 0.026(3) 0.035(4) -0.001(3) 0.012(3) 0.001(3) C31 0.067(5) 0.033(4) 0.087(6) -0.014(4) 0.049(5) -0.003(4) C32 0.047(4) 0.031(4) 0.058(5) 0.005(3) 0.005(4) 0.006(3) C33 0.042(4) 0.026(3) 0.042(4) 0.009(3) 0.009(3) 0.001(3) C34 0.033(3) 0.025(3) 0.026(3) -0.004(3) 0.009(3) -0.002(3) C35 0.025(3) 0.034(3) 0.025(3) 0.001(3) 0.002(3) -0.001(3) C36 0.032(3) 0.026(3) 0.027(3) -0.001(3) 0.000(3) -0.002(3) C37 0.028(3) 0.034(3) 0.028(3) -0.005(3) 0.002(3) 0.004(3) C38 0.028(3) 0.040(4) 0.032(4) -0.003(3) 0.006(3) -0.002(3) C39 0.029(3) 0.035(3) 0.025(3) -0.003(3) 0.007(3) -0.001(3) C40 0.034(4) 0.026(3) 0.025(3) 0.000(3) 0.004(3) 0.004(3) C41 0.046(4) 0.034(3) 0.039(4) 0.003(3) 0.017(3) -0.002(3) C42 0.056(5) 0.032(4) 0.081(6) 0.010(4) 0.025(4) 0.001(4) C43 0.072(5) 0.046(4) 0.057(5) 0.001(4) 0.039(4) -0.008(4) C44 0.058(5) 0.049(4) 0.049(4) -0.004(4) 0.020(4) -0.020(4) C45 0.028(3) 0.035(4) 0.040(4) -0.007(3) 0.008(3) 0.000(3) C46 0.027(3) 0.026(3) 0.040(4) -0.002(3) 0.008(3) 0.001(3) C47 0.050(4) 0.042(4) 0.040(4) 0.013(3) 0.005(3) -0.007(3) C48 0.043(4) 0.063(5) 0.043(4) 0.011(4) 0.006(3) 0.007(4) C49 0.066(6) 0.071(6) 0.050(5) -0.003(4) 0.015(4) 0.022(4) C50 0.078(6) 0.062(5) 0.036(4) -0.006(4) 0.008(4) 0.019(5) C51 0.046(4) 0.041(4) 0.040(4) -0.001(3) 0.010(3) 0.010(3) C52 0.050(5) 0.043(4) 0.058(5) 0.006(4) 0.012(4) 0.012(4) C53 0.048(4) 0.035(4) 0.063(5) 0.004(4) 0.013(4) -0.010(3) C54 0.047(4) 0.041(4) 0.053(5) 0.001(4) 0.017(4) -0.014(3) C55 0.040(4) 0.043(4) 0.059(5) -0.005(4) 0.019(4) -0.005(3) C56 0.033(4) 0.071(5) 0.049(5) -0.012(4) 0.011(3) 0.004(4) C57 0.046(4) 0.051(5) 0.052(5) 0.003(4) 0.008(4) 0.006(4) C58 0.042(4) 0.039(4) 0.057(5) -0.002(4) 0.005(4) 0.011(3) C59 0.055(5) 0.035(4) 0.057(5) -0.001(3) 0.013(4) 0.007(3) C60 0.054(5) 0.043(4) 0.039(4) -0.003(3) 0.010(4) -0.002(3) C61 0.051(5) 0.074(6) 0.035(4) -0.001(4) 0.001(4) 0.010(4) C62 0.048(4) 0.055(5) 0.039(4) 0.006(4) 0.010(3) 0.008(4) C63 0.047(5) 0.041(4) 0.053(5) -0.003(4) -0.007(4) -0.009(3) C64 0.040(4) 0.045(4) 0.081(6) -0.011(4) 0.014(4) -0.002(4) C65 0.059(5) 0.058(5) 0.058(5) 0.005(4) 0.019(4) 0.010(4) C66 0.045(4) 0.032(4) 0.048(4) 0.009(3) 0.016(4) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O8 1.793(4) . ? U O7 1.824(4) . ? U O1 2.272(4) . ? U O5 2.274(4) . ? U O2 2.280(4) . ? U O4 2.284(4) . ? U K2 3.9066(16) . ? U K2 4.3355(16) 3_575 ? K1 O17 2.719(5) . ? K1 O12 2.806(4) . ? K1 O10 2.859(5) . ? K1 O13 2.884(5) . ? K1 O9 2.936(5) . ? K1 O14 2.984(5) . ? K1 O11 3.041(5) . ? K1 O15 3.166(5) . ? K2 O7 2.669(4) 3_575 ? K2 O1 2.696(4) . ? K2 O20 2.810(5) . ? K2 O7 2.885(4) . ? K2 O21 2.923(6) . ? K2 O19 3.090(6) . ? K2 K2 4.245(3) 3_575 ? K2 U 4.3357(16) 3_575 ? O1 C2 1.348(7) . ? O2 C13 1.339(7) . ? O3 C23 1.437(7) . ? O3 C22 1.438(7) . ? O4 C25 1.377(7) . ? O5 C36 1.352(7) . ? O6 C45 1.415(7) . ? O6 C46 1.425(7) . ? O7 K2 2.669(4) 3_575 ? O9 C66 1.402(8) . ? O9 C47 1.445(8) . ? O10 C48 1.400(8) . ? O10 C49 1.446(9) . ? O11 C51 1.417(8) . ? O11 C50 1.418(8) . ? O12 C53 1.419(8) . ? O12 C52 1.424(8) . ? O13 C55 1.412(8) . ? O13 C54 1.420(8) . ? O14 C56 1.422(8) . ? O14 C57 1.434(8) . ? O15 C59 1.416(8) . ? O15 C58 1.417(8) . ? O16 C60 1.411(8) . ? O16 C61 1.434(8) . ? O17 C63 1.417(8) . ? O17 C62 1.429(8) . ? O18 C65 1.406(9) . ? O18 C64 1.438(9) . ? C1 C6 1.386(8) . ? C1 C2 1.417(8) . ? C1 C46 1.495(8) . ? C2 C3 1.395(8) . ? C3 C4 1.397(8) . ? C3 C11 1.517(8) . ? C4 C5 1.390(8) . ? C5 C6 1.392(8) . ? C5 C7 1.528(8) . ? C7 C9 1.517(9) . ? C7 C8 1.533(9) . ? C7 C10 1.541(9) . ? C11 C12 1.516(8) . ? C12 C17 1.398(8) . ? C12 C13 1.413(8) . ? C13 C14 1.416(8) . ? C14 C15 1.385(8) . ? C14 C22 1.479(8) . ? C15 C16 1.390(8) . ? C16 C17 1.406(8) . ? C16 C18 1.528(8) . ? C18 C20 1.526(8) . ? C18 C21 1.531(8) . ? C18 C19 1.540(8) . ? C23 C24 1.494(8) . ? C24 C29 1.380(8) . ? C24 C25 1.414(8) . ? C25 C26 1.393(8) . ? C26 C27 1.385(8) . ? C26 C34 1.514(8) . ? C27 C28 1.399(8) . ? C28 C29 1.391(8) . ? C28 C30 1.542(8) . ? C30 C32 1.516(9) . ? C30 C33 1.528(9) . ? C30 C31 1.539(9) . ? C34 C35 1.517(8) . ? C35 C36 1.396(8) . ? C35 C40 1.397(8) . ? C36 C37 1.401(8) . ? C37 C38 1.398(8) . ? C37 C45 1.483(8) . ? C38 C39 1.392(8) . ? C39 C40 1.397(8) . ? C39 C41 1.533(9) . ? C41 C44 1.508(10) . ? C41 C43 1.530(9) . ? C41 C42 1.548(10) . ? C47 C48 1.461(10) . ? C49 C50 1.470(11) . ? C51 C52 1.495(10) . ? C53 C54 1.503(10) . ? C55 C56 1.502(10) . ? C57 C58 1.490(10) . ? C59 C60 1.492(10) . ? C61 C62 1.483(10) . ? C63 C64 1.492(10) . ? C65 C66 1.495(10) . ? 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 O8 U O7 179.01(17) . . ? O8 U O1 93.10(16) . . ? O7 U O1 86.00(16) . . ? O8 U O5 94.00(16) . . ? O7 U O5 86.49(17) . . ? O1 U O5 93.13(14) . . ? O8 U O2 91.29(16) . . ? O7 U O2 88.22(16) . . ? O1 U O2 85.94(14) . . ? O5 U O2 174.68(14) . . ? O8 U O4 91.67(16) . . ? O7 U O4 89.23(16) . . ? O1 U O4 175.11(13) . . ? O5 U O4 85.48(14) . . ? O2 U O4 95.01(14) . . ? O17 K1 O12 74.39(14) . . ? O17 K1 O10 123.69(15) . . ? O12 K1 O10 95.90(14) . . ? O17 K1 O13 116.83(14) . . ? O12 K1 O13 59.01(13) . . ? O10 K1 O13 102.47(15) . . ? O17 K1 O9 98.65(14) . . ? O12 K1 O9 141.65(15) . . ? O10 K1 O9 56.02(14) . . ? O13 K1 O9 144.35(15) . . ? O17 K1 O14 146.99(14) . . ? O12 K1 O14 115.97(14) . . ? O10 K1 O14 87.67(14) . . ? O13 K1 O14 57.88(14) . . ? O9 K1 O14 90.65(14) . . ? O17 K1 O11 74.18(13) . . ? O12 K1 O11 57.01(13) . . ? O10 K1 O11 55.90(13) . . ? O13 K1 O11 107.26(13) . . ? O9 K1 O11 84.68(14) . . ? O14 K1 O11 138.52(13) . . ? O17 K1 O15 92.19(13) . . ? O12 K1 O15 121.54(13) . . ? O10 K1 O15 134.99(14) . . ? O13 K1 O15 80.07(13) . . ? O9 K1 O15 96.03(14) . . ? O14 K1 O15 55.21(13) . . ? O11 K1 O15 166.27(13) . . ? O7 K2 O1 138.98(14) 3_575 . ? O7 K2 O20 79.99(13) 3_575 . ? O1 K2 O20 134.69(14) . . ? O7 K2 O7 80.41(13) 3_575 . ? O1 K2 O7 60.41(12) . . ? O20 K2 O7 157.57(15) . . ? O7 K2 O21 68.13(13) 3_575 . ? O1 K2 O21 119.46(14) . . ? O20 K2 O21 93.11(16) . . ? O7 K2 O21 89.61(14) . . ? O7 K2 O19 87.62(14) 3_575 . ? O1 K2 O19 95.87(14) . . ? O20 K2 O19 56.18(15) . . ? O7 K2 O19 112.20(14) . . ? O21 K2 O19 144.55(14) . . ? C2 O1 U 133.3(3) . . ? C2 O1 K2 122.1(3) . . ? U O1 K2 103.38(14) . . ? C13 O2 U 129.4(3) . . ? C23 O3 C22 111.7(4) . . ? C25 O4 U 132.2(3) . . ? C36 O5 U 135.4(3) . . ? C45 O6 C46 111.6(4) . . ? U O7 K2 148.9(2) . 3_575 ? U O7 K2 110.05(17) . . ? K2 O7 K2 99.60(13) 3_575 . ? C66 O9 C47 112.2(5) . . ? C66 O9 K1 110.5(4) . . ? C47 O9 K1 91.2(4) . . ? C48 O10 C49 110.7(6) . . ? C48 O10 K1 114.7(4) . . ? C49 O10 K1 123.8(4) . . ? C51 O11 C50 114.2(5) . . ? C51 O11 K1 106.9(4) . . ? C50 O11 K1 105.8(4) . . ? C53 O12 C52 110.5(5) . . ? C53 O12 K1 119.4(4) . . ? C52 O12 K1 126.3(4) . . ? C55 O13 C54 111.3(5) . . ? C55 O13 K1 112.9(4) . . ? C54 O13 K1 105.2(4) . . ? C56 O14 C57 115.9(5) . . ? C56 O14 K1 115.1(4) . . ? C57 O14 K1 111.7(4) . . ? C59 O15 C58 112.1(5) . . ? C59 O15 K1 127.0(4) . . ? C58 O15 K1 117.9(4) . . ? C60 O16 C61 113.2(6) . . ? C63 O17 C62 113.8(5) . . ? C63 O17 K1 129.2(4) . . ? C62 O17 K1 116.7(4) . . ? C65 O18 C64 114.7(6) . . ? C6 C1 C2 120.0(5) . . ? C6 C1 C46 121.2(5) . . ? C2 C1 C46 118.8(5) . . ? O1 C2 C3 121.9(5) . . ? O1 C2 C1 119.9(5) . . ? C3 C2 C1 118.1(5) . . ? C2 C3 C4 119.5(5) . . ? C2 C3 C11 120.7(5) . . ? C4 C3 C11 119.8(5) . . ? C5 C4 C3 123.4(6) . . ? C4 C5 C6 115.9(5) . . ? C4 C5 C7 123.0(5) . . ? C6 C5 C7 121.1(5) . . ? C1 C6 C5 122.8(6) . . ? C9 C7 C5 113.3(5) . . ? C9 C7 C8 107.7(5) . . ? C5 C7 C8 108.9(5) . . ? C9 C7 C10 108.7(6) . . ? C5 C7 C10 109.0(5) . . ? C8 C7 C10 109.0(6) . . ? C12 C11 C3 113.6(5) . . ? C17 C12 C13 119.5(5) . . ? C17 C12 C11 119.1(5) . . ? C13 C12 C11 121.4(5) . . ? O2 C13 C12 120.8(5) . . ? O2 C13 C14 121.0(5) . . ? C12 C13 C14 118.1(5) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 C22 120.8(5) . . ? C13 C14 C22 119.3(5) . . ? C14 C15 C16 123.4(5) . . ? C15 C16 C17 116.0(5) . . ? C15 C16 C18 124.6(5) . . ? C17 C16 C18 119.3(5) . . ? C12 C17 C16 122.9(5) . . ? C20 C18 C16 109.8(5) . . ? C20 C18 C21 109.3(5) . . ? C16 C18 C21 111.5(5) . . ? C20 C18 C19 108.0(5) . . ? C16 C18 C19 110.6(5) . . ? C21 C18 C19 107.6(5) . . ? O3 C22 C14 109.8(5) . . ? O3 C23 C24 110.6(5) . . ? C29 C24 C25 119.8(6) . . ? C29 C24 C23 121.3(6) . . ? C25 C24 C23 118.8(5) . . ? O4 C25 C26 121.1(5) . . ? O4 C25 C24 119.9(5) . . ? C26 C25 C24 119.0(5) . . ? C27 C26 C25 118.8(5) . . ? C27 C26 C34 120.1(5) . . ? C25 C26 C34 121.1(5) . . ? C26 C27 C28 123.7(6) . . ? C29 C28 C27 115.9(5) . . ? C29 C28 C30 122.2(5) . . ? C27 C28 C30 121.8(5) . . ? C24 C29 C28 122.6(6) . . ? C32 C30 C33 108.2(5) . . ? C32 C30 C31 110.3(6) . . ? C33 C30 C31 107.1(5) . . ? C32 C30 C28 110.1(5) . . ? C33 C30 C28 111.9(5) . . ? C31 C30 C28 109.1(5) . . ? C26 C34 C35 112.2(5) . . ? C36 C35 C40 118.7(5) . . ? C36 C35 C34 121.1(5) . . ? C40 C35 C34 120.2(5) . . ? O5 C36 C35 120.4(5) . . ? O5 C36 C37 120.0(5) . . ? C35 C36 C37 119.6(5) . . ? C38 C37 C36 119.6(5) . . ? C38 C37 C45 121.1(6) . . ? C36 C37 C45 119.2(5) . . ? C39 C38 C37 122.2(6) . . ? C38 C39 C40 116.4(6) . . ? C38 C39 C41 122.3(5) . . ? C40 C39 C41 121.3(5) . . ? C39 C40 C35 123.1(5) . . ? C44 C41 C43 110.9(6) . . ? C44 C41 C39 109.1(5) . . ? C43 C41 C39 111.1(5) . . ? C44 C41 C42 109.0(6) . . ? C43 C41 C42 106.6(6) . . ? C39 C41 C42 110.2(5) . . ? O6 C45 C37 110.6(5) . . ? O6 C46 C1 109.5(5) . . ? O9 C47 C48 105.5(6) . . ? O10 C48 C47 108.8(6) . . ? O10 C49 C50 106.7(6) . . ? O11 C50 C49 109.7(7) . . ? O11 C51 C52 113.9(6) . . ? O12 C52 C51 108.2(6) . . ? O12 C53 C54 109.9(5) . . ? O13 C54 C53 109.0(6) . . ? O13 C55 C56 108.0(6) . . ? O14 C56 C55 112.7(6) . . ? O14 C57 C58 113.6(6) . . ? O15 C58 C57 110.1(6) . . ? O15 C59 C60 111.6(6) . . ? O16 C60 C59 108.8(6) . . ? O16 C61 C62 109.3(6) . . ? O17 C62 C61 112.2(6) . . ? O17 C63 C64 108.8(6) . . ? O18 C64 C63 107.6(6) . . ? O18 C65 C66 112.4(7) . . ? O9 C66 C65 110.8(6) . . ? 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 O19 H19B O20 0.78 2.06 2.789(8) 155.8 . O19 H19A O23 0.95 1.94 2.861(8) 163.4 . O20 H20A O4 0.97 1.72 2.682(6) 172.4 3_575 O20 H20B O16 0.90 1.93 2.819(7) 172.2 2_455 O21 H21B O2 0.88 1.93 2.804(6) 174.0 3_575 O21 H21A O24 0.93 1.81 2.717(7) 164.8 . O22 H22A O3 0.86 2.09 2.902(6) 157.1 . O22 H22B O9 1.03 2.12 3.081(8) 154.3 . O23 H23B O11 0.88 2.09 2.936(7) 160.8 2 O23 H23A O22 0.90 1.99 2.850(8) 157.7 2 O24 H24A O5 0.94 1.83 2.734(6) 160.0 . O24 H24B O19 0.92 1.90 2.777(7) 160.9 3_575