Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author "P. Thu\'ery" _publ_contact_author_address ; CEA/Saclay, SCM (CNRS URA 331) B\^at. 125 91191 Gif-sur-Yvette France ; _publ_contact_author_phone '33 01 69 08 63 29' _publ_contact_author_fax '33 1 69 08 66 40' _publ_contact_author_email pierre.thuery@cea.fr _publ_section_title ; Complex-within-complex assemblages from{M([2.2.2]cryptand)(H2O)2}2+ (M = Sr, Ba) and {UO2(p-tert-butyl[3.1.3.1]homooxacalixarene - 4H)}2- ; _publ_contact_author_name 'P. Thuery' loop_ _publ_author_name B.Masci P.Thuery data_1 _database_code_depnum_ccdc_archive 'CCDC 606960' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H162 Ba N2 O22' _chemical_formula_weight 2001.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 15.4801(9) _cell_length_b 18.8355(12) _cell_length_c 18.5273(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.642(3) _cell_angle_gamma 90.00 _cell_volume 5271.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 34140 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method ? _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.447 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 30 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' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 34140 _diffrn_reflns_av_R_equivalents 0.1048 _diffrn_reflns_av_sigmaI/netI 0.1424 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 25.68 _reflns_number_total 17490 _reflns_number_gt 11247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (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)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. Due to the low quality of the crystal and hence of the data, many restraints on bond lengths and/or displacement parameters had to be applied. The phenolic H atoms were found on a Fourier-difference map and all the other ones, except those of the water molecules, 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. 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^)+(0.1502P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.70(2) _refine_ls_number_reflns 17490 _refine_ls_number_parameters 1241 _refine_ls_number_restraints 300 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2604 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.532 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.110 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 Ba Ba 0.92066(5) 0.72617(3) 0.22934(5) 0.04396(17) Uani 1 1 d . . . N1 N 0.7755(8) 0.6528(6) 0.1241(7) 0.065(4) Uani 1 1 d . . . N2 N 1.0675(9) 0.7945(5) 0.3294(7) 0.064(3) Uani 1 1 d . . . O1 O 0.8881(6) 0.5827(5) 0.2496(5) 0.072(3) Uani 1 1 d . . . O2 O 1.0308(7) 0.6479(5) 0.3320(5) 0.065(3) Uani 1 1 d . . . O3 O 0.7510(6) 0.7857(5) 0.1981(5) 0.065(2) Uani 1 1 d . . . O4 O 0.8938(8) 0.8525(6) 0.2929(6) 0.091(4) Uani 1 1 d . . . O5 O 0.9548(7) 0.6661(5) 0.1022(5) 0.071(3) Uani 1 1 d . . . O6 O 1.0939(10) 0.7288(9) 0.1996(8) 0.121(5) Uani 1 1 d . . . O7 O 0.9236(10) 0.8296(6) 0.1282(6) 0.096(4) Uani 1 1 d . . . O8 O 0.8499(7) 0.6919(5) 0.3628(6) 0.066(3) Uani 1 1 d . . . O9 O 0.9663(11) 0.8160(9) -0.0122(9) 0.128(5) Uani 1 1 d U . . O10 O 0.9620(10) 0.9673(8) 0.1528(8) 0.115(4) Uani 1 1 d U . . C1 C 0.7544(15) 0.5896(13) 0.1687(14) 0.133(8) Uani 1 1 d DU . . H1C H 0.7250 0.6083 0.2058 0.159 Uiso 1 1 calc R . . H1D H 0.7111 0.5610 0.1354 0.159 Uiso 1 1 calc R . . C2 C 0.8250(12) 0.5397(10) 0.2080(10) 0.093(5) Uani 1 1 d DU . . H2C H 0.8013 0.5071 0.2393 0.112 Uiso 1 1 calc R . . H2D H 0.8495 0.5124 0.1728 0.112 Uiso 1 1 calc R . . C3 C 0.9675(8) 0.5459(6) 0.2714(6) 0.058(3) Uani 1 1 d D . . H3C H 0.9994 0.5477 0.2318 0.069 Uiso 1 1 calc R . . H3D H 0.9549 0.4965 0.2797 0.069 Uiso 1 1 calc R . . C4 C 1.0245(8) 0.5758(5) 0.3402(6) 0.052(3) Uani 1 1 d D . . H4C H 0.9989 0.5654 0.3824 0.063 Uiso 1 1 calc R . . H4D H 1.0830 0.5546 0.3489 0.063 Uiso 1 1 calc R . . C5 C 1.0845(10) 0.6817(8) 0.3998(9) 0.076(4) Uani 1 1 d . . . H5A H 1.0704 0.6593 0.4429 0.091 Uiso 1 1 calc R . . H5B H 1.1467 0.6733 0.4014 0.091 Uiso 1 1 calc R . . C6 C 1.0701(13) 0.7571(10) 0.4036(11) 0.090(5) Uani 1 1 d U . . H6C H 1.1171 0.7776 0.4411 0.108 Uiso 1 1 calc R . . H6D H 1.0146 0.7654 0.4183 0.108 Uiso 1 1 calc R . . C7 C 0.6985(10) 0.6931(7) 0.1118(9) 0.074(4) Uani 1 1 d DU . . H7A H 0.6639 0.6780 0.1468 0.089 Uiso 1 1 calc R . . H7B H 0.6644 0.6820 0.0626 0.089 Uiso 1 1 calc R . . C8 C 0.7089(15) 0.7724(7) 0.1176(11) 0.096(5) Uani 1 1 d DU . . H8A H 0.6519 0.7958 0.1038 0.116 Uiso 1 1 calc R . . H8B H 0.7467 0.7895 0.0859 0.116 Uiso 1 1 calc R . . C9 C 0.7496(12) 0.8619(10) 0.2113(10) 0.088(5) Uani 1 1 d U . . H9A H 0.6896 0.8781 0.2089 0.105 Uiso 1 1 calc R . . H9B H 0.7737 0.8875 0.1747 0.105 Uiso 1 1 calc R . . C10 C 0.8059(9) 0.8734(8) 0.2874(8) 0.064(3) Uani 1 1 d U . . H10A H 0.8046 0.9233 0.3000 0.076 Uiso 1 1 calc R . . H10B H 0.7812 0.8467 0.3228 0.076 Uiso 1 1 calc R . . C11 C 0.9559(13) 0.8840(12) 0.3473(12) 0.102(6) Uani 1 1 d U . . H11A H 0.9486 0.8672 0.3951 0.122 Uiso 1 1 calc R . . H11B H 0.9463 0.9349 0.3455 0.122 Uiso 1 1 calc R . . C12 C 1.0507(15) 0.8687(13) 0.3397(13) 0.117(7) Uani 1 1 d U . . H12A H 1.0623 0.8952 0.2980 0.140 Uiso 1 1 calc R . . H12B H 1.0916 0.8855 0.3838 0.140 Uiso 1 1 calc R . . C13 C 0.801(2) 0.6398(19) 0.0666(19) 0.163(11) Uani 1 1 d U . . H13A H 0.7807 0.6799 0.0344 0.195 Uiso 1 1 calc R . . H13B H 0.7654 0.5997 0.0448 0.195 Uiso 1 1 calc R . . C14 C 0.9003(19) 0.6228(17) 0.0540(18) 0.155(10) Uani 1 1 d U . . H14A H 0.9156 0.5734 0.0646 0.186 Uiso 1 1 calc R . . H14B H 0.9040 0.6331 0.0035 0.186 Uiso 1 1 calc R . . C15 C 1.0468(11) 0.6507(8) 0.1056(10) 0.085(5) Uani 1 1 d DU . . H15A H 1.0528 0.6328 0.0578 0.102 Uiso 1 1 calc R . . H15B H 1.0657 0.6133 0.1416 0.102 Uiso 1 1 calc R . . C16 C 1.1074(11) 0.7135(8) 0.1259(10) 0.085(4) Uani 1 1 d DU . . H16A H 1.1685 0.7013 0.1268 0.102 Uiso 1 1 calc R . . H16B H 1.0896 0.7530 0.0924 0.102 Uiso 1 1 calc R . . C17 C 1.1453(17) 0.7885(13) 0.2267(11) 0.121(7) Uani 1 1 d DU . . H17A H 1.1150 0.8322 0.2085 0.146 Uiso 1 1 calc R . . H17B H 1.2022 0.7872 0.2129 0.146 Uiso 1 1 calc R . . C18 C 1.1559(16) 0.7814(14) 0.3104(11) 0.118(7) Uani 1 1 d DU . . H18A H 1.1769 0.7342 0.3263 0.142 Uiso 1 1 calc R . . H18B H 1.1988 0.8157 0.3357 0.142 Uiso 1 1 calc R . . O1A O 0.8091(6) 1.0630(6) 0.3779(5) 0.072(3) Uani 1 1 d . . . H1A H 0.8591 1.0605 0.3613 0.086 Uiso 1 1 d R . . O2A O 0.9239(6) 1.0565(5) 0.2722(5) 0.061(2) Uani 1 1 d . . . O3A O 0.9962(6) 1.0506(5) 0.4376(4) 0.055(2) Uani 1 1 d . . . H3A H 0.9891 1.0229 0.4738 0.067 Uiso 1 1 d R . . O4A O 0.9799(6) 0.9577(5) 0.5304(6) 0.068(3) Uani 1 1 d . . . O5A O 0.8930(7) 0.8100(6) 0.5281(6) 0.086(3) Uani 1 1 d D . . O6A O 0.7843(7) 0.9475(5) 0.5079(5) 0.065(2) Uani 1 1 d U . . H6A H 0.8381 0.9342 0.5387 0.078 Uiso 1 1 d R . . O1B O 0.8758(5) 0.4479(4) 0.3786(5) 0.056(2) Uani 1 1 d . . . H1B H 0.8731 0.4766 0.4118 0.067 Uiso 1 1 d R . . O2B O 0.9669(7) 0.3051(6) 0.3788(6) 0.074(3) Uani 1 1 d U . . O3B O 1.0718(6) 0.4303(5) 0.4032(5) 0.056(2) Uani 1 1 d . . . H3B H 1.0168 0.4040 0.3909 0.068 Uiso 1 1 d R . . O4B O 1.0588(5) 0.5518(4) 0.5239(4) 0.0502(19) Uani 1 1 d . . . H4B H 1.0394 0.5072 0.5003 0.060 Uiso 1 1 d R . . O5B O 0.9452(5) 0.5676(4) 0.6187(5) 0.0486(19) Uani 1 1 d . . . O6B O 0.8609(5) 0.5606(4) 0.4520(5) 0.0486(18) Uani 1 1 d . . . C1A C 0.6662(8) 1.0233(6) 0.3186(6) 0.046(3) Uani 1 1 d . . . C1B C 0.7178(7) 0.4292(6) 0.3624(5) 0.036(2) Uani 1 1 d . . . C2A C 0.7462(8) 1.0504(7) 0.3138(7) 0.054(3) Uani 1 1 d . . . C2B C 0.8041(7) 0.4050(6) 0.3633(7) 0.046(3) Uani 1 1 d . . . C3A C 0.7627(8) 1.0654(9) 0.2428(8) 0.068(4) Uani 1 1 d . . . C3B C 0.8180(9) 0.3341(9) 0.3461(9) 0.079(4) Uani 1 1 d DU . . C4A C 0.6971(10) 1.0565(8) 0.1819(9) 0.065(4) Uani 1 1 d U . . H4A1 H 0.7076 1.0698 0.1363 0.077 Uiso 1 1 calc R . . C4B C 0.7471(9) 0.2875(8) 0.3375(8) 0.068(4) Uani 1 1 d U . . H4B1 H 0.7560 0.2406 0.3251 0.081 Uiso 1 1 calc R . . C5A C 0.6167(8) 1.0290(7) 0.1840(6) 0.054(3) Uani 1 1 d . . . C5B C 0.6629(7) 0.3071(6) 0.3466(7) 0.050(3) Uani 1 1 d . . . C6A C 0.6015(7) 1.0147(6) 0.2553(6) 0.047(3) Uani 1 1 d . . . H6A1 H 0.5458 0.9990 0.2594 0.056 Uiso 1 1 calc R . . C6B C 0.6522(7) 0.3792(6) 0.3550(6) 0.040(2) Uani 1 1 d . . . H6B1 H 0.5956 0.3952 0.3557 0.048 Uiso 1 1 calc R . . C7A C 0.5466(9) 1.0166(9) 0.1109(6) 0.062(4) Uani 1 1 d . . . C7B C 0.5858(10) 0.2504(8) 0.3368(9) 0.059(4) Uani 1 1 d . . . C8B C 0.6079(9) 0.1997(8) 0.4019(8) 0.067(4) Uani 1 1 d . . . H8B1 H 0.5623 0.1645 0.3975 0.101 Uiso 1 1 calc R . . H8B2 H 0.6121 0.2257 0.4471 0.101 Uiso 1 1 calc R . . H8B3 H 0.6635 0.1769 0.4022 0.101 Uiso 1 1 calc R . . C8A C 0.5756(11) 0.9625(9) 0.0632(9) 0.076(4) Uani 1 1 d U . . H8A1 H 0.5955 0.9208 0.0919 0.115 Uiso 1 1 calc R . . H8A2 H 0.6232 0.9812 0.0433 0.115 Uiso 1 1 calc R . . H8A3 H 0.5269 0.9503 0.0233 0.115 Uiso 1 1 calc R . . C9A C 0.4575(10) 0.9989(9) 0.1250(8) 0.072(4) Uani 1 1 d . . . H9A1 H 0.4164 0.9914 0.0787 0.108 Uiso 1 1 calc R . . H9A2 H 0.4373 1.0374 0.1510 0.108 Uiso 1 1 calc R . . H9A3 H 0.4617 0.9565 0.1543 0.108 Uiso 1 1 calc R . . C9B C 0.4966(9) 0.2873(7) 0.3333(8) 0.065(3) Uani 1 1 d . . . H9B1 H 0.4817 0.3155 0.2891 0.098 Uiso 1 1 calc R . . H9B2 H 0.5008 0.3173 0.3758 0.098 Uiso 1 1 calc R . . H9B3 H 0.4515 0.2522 0.3327 0.098 Uiso 1 1 calc R . . C10A C 0.5330(10) 1.0889(9) 0.0709(8) 0.075(4) Uani 1 1 d . . . H10C H 0.5852 1.1009 0.0536 0.113 Uiso 1 1 calc R . . H10D H 0.5221 1.1247 0.1047 0.113 Uiso 1 1 calc R . . H10E H 0.4833 1.0860 0.0297 0.113 Uiso 1 1 calc R . . C10B C 0.5830(9) 0.2079(7) 0.2655(7) 0.062(4) Uani 1 1 d . . . H10F H 0.6405 0.1881 0.2666 0.093 Uiso 1 1 calc R . . H10G H 0.5665 0.2387 0.2235 0.093 Uiso 1 1 calc R . . H10H H 0.5405 0.1702 0.2619 0.093 Uiso 1 1 calc R . . C11A C 0.8451(11) 1.0955(10) 0.2335(10) 0.084(4) Uani 1 1 d U . . H11C H 0.8490 1.1440 0.2515 0.101 Uiso 1 1 calc R . . H11D H 0.8449 1.0970 0.1812 0.101 Uiso 1 1 calc R . . C11B C 0.9037(9) 0.3136(9) 0.3229(9) 0.077(4) Uani 1 1 d DU . . H11E H 0.8944 0.2699 0.2945 0.093 Uiso 1 1 calc R . . H11F H 0.9192 0.3504 0.2914 0.093 Uiso 1 1 calc R . . C12B C 1.0508(8) 0.2843(7) 0.3593(8) 0.058(3) Uani 1 1 d . . . H12C H 1.0540 0.3048 0.3120 0.069 Uiso 1 1 calc R . . H12D H 1.0534 0.2330 0.3551 0.069 Uiso 1 1 calc R . . C12A C 0.9947(11) 1.0997(10) 0.2916(8) 0.085(5) Uani 1 1 d . . . H12E H 0.9790 1.1398 0.3190 0.102 Uiso 1 1 calc R . . H12F H 1.0104 1.1180 0.2472 0.102 Uiso 1 1 calc R . . C13B C 1.1274(7) 0.3099(6) 0.4180(7) 0.050(3) Uani 1 1 d . . . C13A C 1.0730(9) 1.0631(7) 0.3376(7) 0.061(3) Uani 1 1 d . . . C14A C 1.0729(7) 1.0449(6) 0.4127(7) 0.044(3) Uani 1 1 d . . . C14B C 1.1356(7) 0.3830(6) 0.4354(6) 0.043(2) Uani 1 1 d . . . C15A C 1.1517(7) 1.0216(5) 0.4572(5) 0.036(2) Uani 1 1 d . . . C15B C 1.2100(7) 0.4084(6) 0.4862(6) 0.041(2) Uani 1 1 d . . . C16A C 1.2237(7) 1.0126(6) 0.4269(6) 0.043(2) Uani 1 1 d . . . H16C H 1.2768 0.9990 0.4581 0.051 Uiso 1 1 calc R . . C16B C 1.2755(8) 0.3572(7) 0.5162(6) 0.050(3) Uani 1 1 d . . . H16D H 1.3262 0.3724 0.5493 0.060 Uiso 1 1 calc R . . C17A C 1.2228(7) 1.0225(6) 0.3521(6) 0.046(3) Uani 1 1 d . . . C17B C 1.2675(8) 0.2882(6) 0.4989(7) 0.051(3) Uani 1 1 d . . . C18B C 1.1922(7) 0.2644(6) 0.4514(7) 0.050(3) Uani 1 1 d . . . H18C H 1.1853 0.2160 0.4418 0.060 Uiso 1 1 calc R . . C18A C 1.1470(8) 1.0494(7) 0.3093(7) 0.054(3) Uani 1 1 d . . . H18D H 1.1449 1.0588 0.2596 0.065 Uiso 1 1 calc R . . C19B C 1.3415(10) 0.2337(7) 0.5331(9) 0.071(4) Uani 1 1 d . . . C19A C 1.3023(9) 1.0133(8) 0.3166(7) 0.059(4) Uani 1 1 d . . . C20B C 1.3108(13) 0.1837(10) 0.5878(10) 0.092(5) Uani 1 1 d U . . H20A H 1.3580 0.1519 0.6089 0.138 Uiso 1 1 calc R . . H20B H 1.2606 0.1568 0.5623 0.138 Uiso 1 1 calc R . . H20C H 1.2944 0.2110 0.6264 0.138 Uiso 1 1 calc R . . C20A C 1.2770(9) 0.9627(9) 0.2506(8) 0.072(4) Uani 1 1 d . . . H20D H 1.2330 0.9848 0.2126 0.109 Uiso 1 1 calc R . . H20E H 1.2535 0.9196 0.2662 0.109 Uiso 1 1 calc R . . H20F H 1.3285 0.9521 0.2316 0.109 Uiso 1 1 calc R . . C21B C 1.3607(11) 0.1848(9) 0.4706(8) 0.078(4) Uani 1 1 d . . . H21A H 1.3807 0.2132 0.4345 0.117 Uiso 1 1 calc R . . H21B H 1.3075 0.1602 0.4475 0.117 Uiso 1 1 calc R . . H21C H 1.4056 0.1510 0.4914 0.117 Uiso 1 1 calc R . . C21A C 1.3816(14) 0.9775(12) 0.3744(12) 0.108(6) Uani 1 1 d U . . H21D H 1.3599 0.9593 0.4155 0.161 Uiso 1 1 calc R . . H21E H 1.4267 1.0122 0.3917 0.161 Uiso 1 1 calc R . . H21F H 1.4059 0.9393 0.3508 0.161 Uiso 1 1 calc R . . C22B C 1.4295(15) 0.2691(12) 0.5670(13) 0.114(6) Uani 1 1 d U . . H22A H 1.4694 0.2345 0.5941 0.171 Uiso 1 1 calc R . . H22B H 1.4200 0.3063 0.5998 0.171 Uiso 1 1 calc R . . H22C H 1.4546 0.2888 0.5283 0.171 Uiso 1 1 calc R . . C22A C 1.3349(13) 1.0828(11) 0.2893(11) 0.102(6) Uani 1 1 d U . . H22D H 1.3759 1.0725 0.2586 0.153 Uiso 1 1 calc R . . H22E H 1.3639 1.1107 0.3309 0.153 Uiso 1 1 calc R . . H22F H 1.2854 1.1087 0.2612 0.153 Uiso 1 1 calc R . . C23B C 1.2206(8) 0.4859(6) 0.5072(6) 0.044(3) Uani 1 1 d . . . H23A H 1.2815 0.4999 0.5097 0.053 Uiso 1 1 calc R . . H23B H 1.1832 0.5140 0.4687 0.053 Uiso 1 1 calc R . . C23A C 1.1570(9) 1.0097(6) 0.5373(6) 0.046(3) Uani 1 1 d . . . H23C H 1.1157 1.0413 0.5536 0.055 Uiso 1 1 calc R . . H23D H 1.2161 1.0218 0.5645 0.055 Uiso 1 1 calc R . . C24B C 1.1970(7) 0.5023(5) 0.5801(6) 0.038(2) Uani 1 1 d . . . C24A C 1.1362(7) 0.9326(6) 0.5560(5) 0.042(2) Uani 1 1 d . . . C25A C 1.0480(8) 0.9122(5) 0.5519(7) 0.047(3) Uani 1 1 d D . . C25B C 1.1188(8) 0.5334(6) 0.5860(5) 0.040(2) Uani 1 1 d . . . C26B C 1.1030(7) 0.5513(6) 0.6559(6) 0.047(3) Uani 1 1 d . . . C26A C 1.0325(9) 0.8424(6) 0.5703(8) 0.071(4) Uani 1 1 d DU . . C27B C 1.1659(7) 0.5353(6) 0.7188(5) 0.039(2) Uani 1 1 d . . . H27B H 1.1547 0.5468 0.7647 0.047 Uiso 1 1 calc R . . C27A C 1.1020(9) 0.7949(7) 0.5922(7) 0.066(4) Uani 1 1 d D . . H27A H 1.0887 0.7490 0.6047 0.079 Uiso 1 1 calc R . . C28B C 1.2461(7) 0.5022(6) 0.7160(6) 0.044(2) Uani 1 1 d . . . C28A C 1.1893(10) 0.8120(7) 0.5964(7) 0.059(3) Uani 1 1 d . . . C29A C 1.2042(8) 0.8849(6) 0.5785(7) 0.054(3) Uani 1 1 d . . . H29A H 1.2621 0.9003 0.5823 0.064 Uiso 1 1 calc R . . C29B C 1.2603(7) 0.4881(6) 0.6463(6) 0.045(2) Uani 1 1 d . . . H29B H 1.3141 0.4681 0.6426 0.054 Uiso 1 1 calc R . . C30A C 1.2588(13) 0.7563(11) 0.6215(11) 0.073(5) Uani 1 1 d U . . C30B C 1.3154(8) 0.4846(7) 0.7874(6) 0.050(3) Uani 1 1 d . . . C31B C 1.3249(11) 0.5503(9) 0.8393(9) 0.077(4) Uani 1 1 d U . . H31A H 1.3601 0.5380 0.8870 0.116 Uiso 1 1 calc R . . H31B H 1.2674 0.5655 0.8444 0.116 Uiso 1 1 calc R . . H31C H 1.3532 0.5882 0.8185 0.116 Uiso 1 1 calc R . . C31A C 1.250(2) 0.7345(15) 0.7015(16) 0.146(9) Uani 1 1 d U . . H31D H 1.1910 0.7185 0.7001 0.220 Uiso 1 1 calc R . . H31E H 1.2631 0.7748 0.7338 0.220 Uiso 1 1 calc R . . H31F H 1.2913 0.6970 0.7195 0.220 Uiso 1 1 calc R . . C32B C 1.2806(12) 0.4255(10) 0.8285(10) 0.093(5) Uani 1 1 d U . . H32A H 1.2732 0.3832 0.7989 0.139 Uiso 1 1 calc R . . H32B H 1.2246 0.4393 0.8384 0.139 Uiso 1 1 calc R . . H32C H 1.3219 0.4166 0.8744 0.139 Uiso 1 1 calc R . . C32A C 1.2472(12) 0.6961(10) 0.5713(10) 0.088(5) Uani 1 1 d U . . H32D H 1.2830 0.6572 0.5942 0.132 Uiso 1 1 calc R . . H32E H 1.2648 0.7093 0.5265 0.132 Uiso 1 1 calc R . . H32F H 1.1861 0.6821 0.5599 0.132 Uiso 1 1 calc R . . C33B C 1.4037(9) 0.4662(8) 0.7734(8) 0.067(3) Uani 1 1 d U . . H33A H 1.4291 0.5074 0.7556 0.100 Uiso 1 1 calc R . . H33B H 1.3973 0.4292 0.7370 0.100 Uiso 1 1 calc R . . H33C H 1.4418 0.4503 0.8185 0.100 Uiso 1 1 calc R . . C33A C 1.3540(12) 0.7875(10) 0.6283(11) 0.097(5) Uani 1 1 d U . . H33D H 1.3955 0.7494 0.6295 0.145 Uiso 1 1 calc R . . H33E H 1.3702 0.8148 0.6729 0.145 Uiso 1 1 calc R . . H33F H 1.3548 0.8175 0.5865 0.145 Uiso 1 1 calc R . . C34B C 1.0238(7) 0.5968(6) 0.6613(6) 0.045(2) Uani 1 1 d . . . H34A H 1.0192 0.6000 0.7126 0.054 Uiso 1 1 calc R . . H34B H 1.0320 0.6444 0.6439 0.054 Uiso 1 1 calc R . . C34A C 0.9497(11) 0.8218(18) 0.5971(8) 0.157(10) Uani 1 1 d DU . . H34C H 0.9585 0.7792 0.6273 0.189 Uiso 1 1 calc R . . H34D H 0.9289 0.8600 0.6241 0.189 Uiso 1 1 calc R . . C35B C 0.8804(7) 0.6220(6) 0.5937(7) 0.048(3) Uani 1 1 d . . . H35A H 0.9022 0.6545 0.5612 0.057 Uiso 1 1 calc R . . H35B H 0.8702 0.6487 0.6358 0.057 Uiso 1 1 calc R . . C35A C 0.8041(8) 0.7981(10) 0.5417(8) 0.089(5) Uani 1 1 d DU . . H35C H 0.8002 0.8207 0.5879 0.107 Uiso 1 1 calc R . . H35D H 0.7952 0.7475 0.5469 0.107 Uiso 1 1 calc R . . C36B C 0.7951(7) 0.5892(6) 0.5531(6) 0.036(2) Uani 1 1 d . . . C36A C 0.7310(6) 0.8268(6) 0.4803(6) 0.045(3) Uani 1 1 d D . . C37B C 0.7892(7) 0.5620(6) 0.4821(5) 0.041(2) Uani 1 1 d . . . C37A C 0.7260(7) 0.9012(6) 0.4652(6) 0.046(3) Uani 1 1 d . . . C38B C 0.7077(6) 0.5361(5) 0.4449(5) 0.034(2) Uani 1 1 d . . . C38A C 0.6576(7) 0.9256(5) 0.4106(6) 0.040(2) Uani 1 1 d . . . C39A C 0.5997(8) 0.8788(6) 0.3714(7) 0.057(3) Uani 1 1 d . . . H39A H 0.5545 0.8964 0.3341 0.068 Uiso 1 1 calc R . . C39B C 0.6358(7) 0.5375(6) 0.4760(6) 0.035(2) Uani 1 1 d . . . H39B H 0.5824 0.5208 0.4479 0.042 Uiso 1 1 calc R . . C40B C 0.6369(7) 0.5623(6) 0.5471(6) 0.045(3) Uani 1 1 d . . . C40A C 0.6034(10) 0.8055(8) 0.3834(9) 0.077(5) Uani 1 1 d . . . C41B C 0.7216(7) 0.5909(5) 0.5858(6) 0.039(2) Uani 1 1 d . . . H41B H 0.7272 0.6104 0.6327 0.047 Uiso 1 1 calc R . . C41A C 0.6706(8) 0.7840(6) 0.4386(7) 0.052(3) Uani 1 1 d . . . H41A H 0.6755 0.7356 0.4485 0.062 Uiso 1 1 calc R . . C42A C 0.5382(11) 0.7541(9) 0.3355(11) 0.101(6) Uani 1 1 d DU . . C42B C 0.5551(8) 0.5619(7) 0.5797(7) 0.068(4) Uani 1 1 d D . . C43B C 0.5132(15) 0.4870(7) 0.5725(11) 0.133(8) Uani 1 1 d DU . . H43A H 0.4844 0.4790 0.6127 0.199 Uiso 1 1 calc R . . H43B H 0.5586 0.4520 0.5739 0.199 Uiso 1 1 calc R . . H43C H 0.4706 0.4834 0.5265 0.199 Uiso 1 1 calc R . . C43A C 0.481(2) 0.7279(18) 0.3873(16) 0.241(18) Uani 1 1 d DU . . H43D H 0.4446 0.7661 0.3978 0.361 Uiso 1 1 calc R . . H43E H 0.5185 0.7114 0.4326 0.361 Uiso 1 1 calc R . . H43F H 0.4442 0.6896 0.3642 0.361 Uiso 1 1 calc R . . C44A C 0.4723(18) 0.7890(16) 0.2727(13) 0.173(11) Uani 1 1 d DU . . H44A H 0.4609 0.8367 0.2865 0.259 Uiso 1 1 calc R . . H44B H 0.4181 0.7625 0.2628 0.259 Uiso 1 1 calc R . . H44C H 0.4964 0.7900 0.2292 0.259 Uiso 1 1 calc R . . C44B C 0.4806(15) 0.6062(10) 0.5335(15) 0.157(10) Uani 1 1 d DU . . H44D H 0.4986 0.6551 0.5344 0.235 Uiso 1 1 calc R . . H44E H 0.4287 0.6022 0.5536 0.235 Uiso 1 1 calc R . . H44F H 0.4676 0.5893 0.4834 0.235 Uiso 1 1 calc R . . C45B C 0.5703(14) 0.5775(10) 0.6618(7) 0.103(6) Uani 1 1 d DU . . H45A H 0.5153 0.5910 0.6738 0.154 Uiso 1 1 calc R . . H45B H 0.6121 0.6155 0.6742 0.154 Uiso 1 1 calc R . . H45C H 0.5930 0.5358 0.6893 0.154 Uiso 1 1 calc R . . C45A C 0.5881(18) 0.6883(13) 0.3200(16) 0.163(10) Uani 1 1 d DU . . H45D H 0.6115 0.6639 0.3656 0.244 Uiso 1 1 calc R . . H45E H 0.6358 0.7020 0.2975 0.244 Uiso 1 1 calc R . . H45F H 0.5485 0.6574 0.2872 0.244 Uiso 1 1 calc R . . C46A C 0.6510(8) 1.0055(5) 0.3953(6) 0.037(2) Uani 1 1 d . . . H46A H 0.5929 1.0222 0.3990 0.044 Uiso 1 1 calc R . . H46B H 0.6947 1.0301 0.4324 0.044 Uiso 1 1 calc R . . C46B C 0.6965(9) 0.5063(6) 0.3669(6) 0.043(3) Uani 1 1 d . . . H46C H 0.6357 0.5139 0.3407 0.051 Uiso 1 1 calc R . . H46D H 0.7341 0.5332 0.3412 0.051 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 Ba 0.0483(3) 0.0405(3) 0.0414(3) -0.0094(4) 0.0060(2) 0.0023(4) N1 0.064(8) 0.040(6) 0.068(7) 0.002(5) -0.034(6) 0.019(5) N2 0.082(8) 0.037(5) 0.073(7) -0.021(5) 0.016(6) -0.011(5) O1 0.069(7) 0.061(5) 0.074(6) -0.010(5) -0.009(5) -0.014(5) O2 0.071(7) 0.058(6) 0.051(5) 0.014(4) -0.017(5) -0.023(5) O3 0.074(6) 0.057(5) 0.061(5) 0.003(4) 0.009(5) 0.010(4) O4 0.112(9) 0.061(6) 0.077(7) -0.038(5) -0.029(6) 0.010(6) O5 0.102(8) 0.066(6) 0.046(5) -0.018(4) 0.020(5) 0.017(5) O6 0.127(11) 0.156(13) 0.101(9) -0.024(9) 0.072(8) -0.068(10) O7 0.182(13) 0.054(6) 0.055(6) 0.013(5) 0.033(7) -0.001(7) O8 0.075(7) 0.055(5) 0.077(6) 0.001(5) 0.037(5) 0.001(5) O9 0.129(5) 0.128(5) 0.128(5) 0.0000(10) 0.0281(15) -0.0001(10) O10 0.116(4) 0.115(4) 0.115(4) 0.0000(10) 0.0254(14) 0.0000(10) C1 0.133(8) 0.132(8) 0.133(8) 0.0001(10) 0.029(2) 0.0000(10) C2 0.093(5) 0.093(5) 0.093(5) 0.0000(10) 0.0203(15) -0.0004(10) C3 0.077(9) 0.044(6) 0.062(8) -0.002(6) 0.037(7) -0.014(6) C4 0.070(8) 0.027(5) 0.055(7) 0.004(5) 0.000(6) -0.001(5) C5 0.062(9) 0.070(9) 0.080(10) -0.012(8) -0.019(7) 0.009(7) C6 0.090(5) 0.090(5) 0.090(5) -0.0002(10) 0.0196(15) 0.0001(10) C7 0.074(4) 0.074(4) 0.074(4) -0.0001(10) 0.0155(13) -0.0002(10) C8 0.096(5) 0.096(5) 0.096(5) 0.0001(10) 0.0206(15) 0.0000(10) C9 0.088(5) 0.087(5) 0.088(5) 0.0000(10) 0.0191(14) 0.0003(10) C10 0.064(3) 0.063(3) 0.064(3) -0.0005(10) 0.0142(12) 0.0006(10) C11 0.102(6) 0.101(6) 0.102(6) -0.0005(10) 0.0220(16) 0.0002(10) C12 0.117(7) 0.116(7) 0.117(7) -0.0005(10) 0.0250(18) 0.0001(10) C13 0.163(11) 0.163(11) 0.163(11) -0.0001(10) 0.035(3) 0.0001(10) C14 0.155(10) 0.155(10) 0.155(10) -0.0005(10) 0.034(2) 0.0002(10) C15 0.085(5) 0.085(5) 0.085(5) -0.0001(10) 0.0189(14) 0.0004(10) C16 0.085(5) 0.085(5) 0.085(5) 0.0002(10) 0.0193(14) 0.0000(10) C17 0.121(7) 0.122(7) 0.122(7) -0.0001(10) 0.0268(19) -0.0004(10) C18 0.118(7) 0.118(7) 0.118(7) -0.0001(10) 0.0258(19) 0.0000(10) O1A 0.042(5) 0.114(9) 0.059(6) 0.026(6) 0.013(4) 0.005(5) O2A 0.054(5) 0.066(6) 0.059(5) -0.002(4) 0.007(4) 0.001(4) O3A 0.062(5) 0.068(6) 0.045(4) -0.001(4) 0.032(4) 0.007(4) O4A 0.062(6) 0.058(5) 0.095(7) -0.016(5) 0.046(5) 0.001(4) O5A 0.094(8) 0.077(7) 0.071(6) 0.018(5) -0.020(6) -0.009(6) O6A 0.065(3) 0.065(3) 0.065(3) 0.0008(10) 0.0132(11) -0.0008(10) O1B 0.050(5) 0.034(4) 0.091(7) -0.008(4) 0.030(4) -0.001(3) O2B 0.074(3) 0.074(3) 0.075(3) -0.0008(10) 0.0152(11) 0.0000(10) O3B 0.046(5) 0.053(5) 0.068(6) 0.012(4) 0.007(4) -0.011(4) O4B 0.044(4) 0.062(5) 0.040(4) 0.013(4) 0.001(3) 0.003(4) O5B 0.035(4) 0.045(4) 0.059(5) -0.002(4) -0.005(3) 0.000(3) O6B 0.043(4) 0.048(4) 0.062(5) -0.003(4) 0.027(4) -0.002(3) C1A 0.057(7) 0.042(6) 0.046(6) 0.015(5) 0.026(5) 0.011(5) C1B 0.042(6) 0.038(6) 0.027(5) -0.004(4) 0.006(4) 0.004(5) C2A 0.044(7) 0.074(8) 0.050(7) 0.025(6) 0.022(5) 0.024(6) C2B 0.039(6) 0.039(6) 0.058(7) -0.002(5) 0.005(5) 0.001(5) C3A 0.037(7) 0.103(11) 0.072(8) 0.045(8) 0.027(6) 0.018(7) C3B 0.079(4) 0.078(4) 0.079(4) -0.0002(10) 0.0172(13) -0.0001(10) C4A 0.064(4) 0.065(4) 0.065(4) 0.0006(10) 0.0143(13) 0.0006(10) C4B 0.067(4) 0.067(4) 0.068(4) -0.0002(10) 0.0149(13) -0.0002(10) C5A 0.061(8) 0.073(8) 0.036(6) 0.018(6) 0.027(5) 0.027(6) C5B 0.036(6) 0.033(5) 0.070(8) 0.003(5) -0.011(5) -0.009(5) C6A 0.037(6) 0.053(6) 0.053(7) 0.000(5) 0.016(5) 0.014(5) C6B 0.042(6) 0.041(6) 0.040(5) 0.003(5) 0.015(4) -0.002(5) C7A 0.060(8) 0.104(11) 0.022(5) 0.006(6) 0.008(5) 0.009(7) C7B 0.040(7) 0.049(6) 0.072(9) 0.017(6) -0.022(6) -0.020(5) C8B 0.060(8) 0.061(8) 0.071(9) 0.013(7) -0.005(7) -0.019(6) C8A 0.077(4) 0.077(4) 0.076(4) -0.0003(10) 0.0167(13) 0.0005(10) C9A 0.075(10) 0.086(10) 0.055(8) -0.025(8) 0.016(7) -0.015(8) C9B 0.055(8) 0.064(9) 0.077(9) -0.004(7) 0.016(6) -0.002(6) C10A 0.073(10) 0.100(12) 0.051(7) 0.017(8) 0.009(7) 0.015(8) C10B 0.049(7) 0.057(7) 0.066(8) -0.002(6) -0.019(6) -0.006(5) C11A 0.084(4) 0.084(4) 0.084(4) 0.0005(10) 0.0182(14) 0.0002(10) C11B 0.078(4) 0.077(4) 0.077(4) 0.0001(10) 0.0169(13) 0.0002(10) C12B 0.047(7) 0.061(8) 0.066(8) -0.001(6) 0.015(5) 0.013(6) C12A 0.077(11) 0.126(14) 0.050(7) -0.004(8) 0.010(7) 0.057(10) C13B 0.045(6) 0.039(6) 0.066(7) -0.010(5) 0.017(5) -0.006(5) C13A 0.069(9) 0.065(8) 0.049(7) 0.005(6) 0.011(6) 0.025(7) C14A 0.035(6) 0.042(6) 0.059(7) -0.002(5) 0.015(5) -0.003(5) C14B 0.040(6) 0.041(6) 0.053(6) -0.004(5) 0.018(5) -0.007(5) C15A 0.048(6) 0.038(5) 0.024(4) 0.002(4) 0.010(4) -0.006(4) C15B 0.048(6) 0.042(6) 0.036(5) -0.002(5) 0.017(4) -0.013(5) C16A 0.037(6) 0.045(6) 0.044(6) 0.001(5) 0.003(4) -0.006(4) C16B 0.051(7) 0.058(7) 0.042(6) 0.007(5) 0.013(5) 0.016(5) C17A 0.037(6) 0.049(6) 0.051(6) -0.003(5) 0.005(5) -0.007(5) C17B 0.062(7) 0.041(6) 0.053(7) -0.004(5) 0.017(6) -0.003(5) C18B 0.048(6) 0.041(6) 0.060(7) -0.002(5) 0.012(5) 0.007(5) C18A 0.055(7) 0.053(7) 0.053(7) 0.017(6) 0.012(6) 0.008(5) C19B 0.063(8) 0.050(7) 0.091(10) -0.015(7) -0.004(7) 0.016(7) C19A 0.059(8) 0.072(9) 0.050(8) 0.005(7) 0.022(6) -0.027(7) C20B 0.092(5) 0.093(5) 0.092(5) 0.0002(10) 0.0204(15) 0.0006(10) C20A 0.058(8) 0.100(11) 0.066(8) -0.026(8) 0.028(7) -0.009(8) C21B 0.085(11) 0.098(12) 0.055(8) -0.010(8) 0.023(7) 0.022(9) C21A 0.107(6) 0.108(6) 0.107(6) 0.0000(10) 0.0235(17) 0.0001(10) C22B 0.114(7) 0.114(7) 0.114(7) -0.0002(10) 0.0246(17) 0.0002(10) C22A 0.102(6) 0.102(6) 0.102(6) -0.0003(10) 0.0232(16) -0.0002(10) C23B 0.044(6) 0.041(6) 0.049(7) -0.009(5) 0.015(5) -0.012(5) C23A 0.066(8) 0.041(6) 0.025(5) -0.001(4) -0.002(5) -0.016(6) C24B 0.038(6) 0.036(5) 0.044(6) 0.001(4) 0.018(4) -0.006(4) C24A 0.054(7) 0.045(6) 0.026(5) -0.001(4) 0.004(4) -0.018(5) C25A 0.053(7) 0.049(6) 0.051(7) -0.001(5) 0.034(5) 0.004(5) C25B 0.054(7) 0.037(6) 0.026(5) -0.006(5) 0.003(4) -0.007(5) C26B 0.039(6) 0.051(6) 0.055(7) -0.004(5) 0.016(5) -0.007(5) C26A 0.071(4) 0.071(4) 0.072(4) -0.0002(10) 0.0167(13) -0.0003(10) C27B 0.033(5) 0.048(6) 0.032(5) 0.001(4) 0.001(4) -0.001(4) C27A 0.096(11) 0.055(7) 0.059(8) -0.007(6) 0.041(7) -0.010(7) C28B 0.043(6) 0.044(6) 0.045(6) -0.008(5) 0.012(5) -0.012(5) C28A 0.080(9) 0.048(7) 0.046(7) 0.003(6) 0.006(6) -0.028(7) C29A 0.041(6) 0.047(6) 0.062(7) 0.009(5) -0.014(5) -0.021(5) C29B 0.049(6) 0.045(6) 0.045(6) 0.001(5) 0.020(5) -0.005(5) C30A 0.073(5) 0.073(5) 0.073(5) 0.0002(10) 0.0154(14) -0.0003(10) C30B 0.049(7) 0.062(7) 0.042(6) -0.009(5) 0.015(5) -0.004(5) C31B 0.077(4) 0.078(4) 0.077(4) -0.0001(10) 0.0166(13) 0.0003(10) C31A 0.147(9) 0.146(9) 0.146(9) 0.0002(10) 0.032(2) -0.0002(10) C32B 0.093(5) 0.093(5) 0.093(5) 0.0004(10) 0.0201(15) 0.0000(10) C32A 0.088(5) 0.087(5) 0.088(5) 0.0001(10) 0.0187(14) 0.0001(10) C33B 0.067(4) 0.068(4) 0.067(4) -0.0001(10) 0.0148(12) 0.0003(10) C33A 0.097(5) 0.097(5) 0.097(5) 0.0003(10) 0.0207(15) 0.0000(10) C34B 0.042(6) 0.052(6) 0.045(6) -0.011(5) 0.019(5) -0.002(5) C34A 0.158(10) 0.157(10) 0.157(10) 0.0001(10) 0.034(2) -0.0002(10) C35B 0.035(6) 0.046(6) 0.058(7) -0.002(5) 0.003(5) -0.002(5) C35A 0.089(5) 0.089(5) 0.089(5) 0.0002(10) 0.0192(14) -0.0002(10) C36B 0.028(6) 0.038(6) 0.039(5) 0.005(5) 0.004(4) 0.004(4) C36A 0.030(5) 0.045(6) 0.060(7) 0.016(5) 0.009(5) 0.007(4) C37B 0.050(6) 0.041(5) 0.030(5) -0.003(4) 0.007(4) 0.007(5) C37A 0.033(6) 0.047(6) 0.054(7) 0.009(5) 0.003(5) -0.003(5) C38B 0.033(5) 0.033(5) 0.034(5) 0.007(4) 0.006(4) 0.000(4) C38A 0.034(5) 0.038(5) 0.049(6) 0.002(5) 0.010(4) 0.004(4) C39A 0.058(7) 0.046(6) 0.057(7) 0.014(5) -0.008(6) -0.003(5) C39B 0.027(5) 0.036(6) 0.041(6) -0.003(5) 0.005(4) -0.006(4) C40B 0.030(5) 0.055(7) 0.046(6) -0.002(5) 0.004(4) 0.005(5) C40A 0.071(9) 0.056(8) 0.089(11) 0.022(7) -0.015(8) -0.027(7) C41B 0.039(6) 0.042(6) 0.036(5) -0.001(4) 0.006(4) 0.009(4) C41A 0.061(7) 0.035(6) 0.058(7) 0.009(5) 0.009(6) -0.004(5) C42A 0.101(6) 0.100(6) 0.100(6) 0.0003(10) 0.0215(16) -0.0003(10) C42B 0.055(8) 0.089(10) 0.068(8) -0.011(8) 0.029(7) 0.012(7) C43B 0.133(8) 0.133(8) 0.133(8) -0.0001(10) 0.029(2) 0.0000(10) C43A 0.241(18) 0.241(18) 0.241(18) 0.0000(10) 0.053(4) -0.0002(10) C44A 0.173(11) 0.173(11) 0.173(11) 0.0000(10) 0.037(3) 0.0000(10) C44B 0.157(10) 0.157(10) 0.157(10) -0.0001(10) 0.034(2) 0.0002(10) C45B 0.103(6) 0.103(6) 0.103(6) -0.0002(10) 0.0226(16) -0.0003(10) C45A 0.163(10) 0.162(10) 0.163(10) -0.0001(10) 0.035(2) -0.0001(10) C46A 0.057(7) 0.031(5) 0.031(5) 0.014(4) 0.031(5) 0.014(5) C46B 0.067(8) 0.029(5) 0.034(5) -0.001(4) 0.016(5) 0.010(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 Ba O2 2.698(9) . ? Ba O7 2.710(10) . ? Ba O4 2.727(10) . ? Ba O5 2.767(8) . ? Ba O1 2.790(10) . ? Ba O3 2.798(9) . ? Ba O6 2.854(13) . ? Ba N2 2.901(11) . ? Ba N1 2.974(12) . ? Ba O8 2.986(9) . ? N1 C13 1.24(3) . ? N1 C7 1.388(18) . ? N1 C1 1.52(3) . ? N2 C12 1.44(2) . ? N2 C18 1.50(3) . ? N2 C6 1.54(2) . ? O1 C2 1.37(2) . ? O1 C3 1.391(16) . ? O2 C4 1.372(14) . ? O2 C5 1.490(16) . ? O3 C9 1.456(19) . ? O3 C8 1.51(2) . ? O4 C11 1.37(2) . ? O4 C10 1.397(18) . ? O5 C14 1.36(3) . ? O5 C15 1.442(19) . ? O6 C17 1.41(3) . ? O6 C16 1.45(2) . ? O7 O10 2.678(19) . ? O7 O9 2.83(2) . ? O9 O3A 2.753(19) 2_574 ? O10 O4A 2.736(17) 2_574 ? C1 C2 1.50(3) . ? C3 C4 1.494(9) . ? C5 C6 1.44(2) . ? C7 C8 1.504(19) . ? C9 C10 1.50(2) . ? C11 C12 1.53(3) . ? C13 C14 1.64(4) . ? C15 C16 1.51(2) . ? C17 C18 1.53(3) . ? O1A C2A 1.381(16) . ? O2A C12A 1.35(2) . ? O2A C11A 1.469(19) . ? O3A C14A 1.368(13) . ? O4A C25A 1.350(15) . ? O5A C34A 1.401(10) . ? O5A C35A 1.470(9) . ? O6A C37A 1.373(15) . ? O1B C2B 1.352(13) . ? O2B C11B 1.270(17) . ? O2B C12B 1.476(16) . ? O3B C14B 1.367(14) . ? O4B C25B 1.357(13) . ? O5B C34B 1.408(13) . ? O5B C35B 1.437(13) . ? O6B C37B 1.347(13) . ? C1A C2A 1.361(17) . ? C1A C6A 1.374(17) . ? C1A C46A 1.527(14) . ? C1B C6B 1.369(15) . ? C1B C2B 1.408(15) . ? C1B C46B 1.496(14) . ? C2A C3A 1.423(17) . ? C2B C3B 1.401(19) . ? C3A C4A 1.35(2) . ? C3A C11A 1.44(2) . ? C3B C4B 1.39(2) . ? C3B C11B 1.53(2) . ? C4A C5A 1.35(2) . ? C4B C5B 1.400(19) . ? C5A C6A 1.419(15) . ? C5A C7A 1.557(17) . ? C5B C6B 1.382(15) . ? C5B C7B 1.582(17) . ? C7A C8A 1.48(2) . ? C7A C9A 1.50(2) . ? C7A C10A 1.54(2) . ? C7B C8B 1.52(2) . ? C7B C9B 1.53(2) . ? C7B C10B 1.54(2) . ? C12B C13B 1.502(17) . ? C12A C13A 1.488(18) . ? C13B C18B 1.361(16) . ? C13B C14B 1.413(15) . ? C13A C18A 1.386(18) . ? C13A C14A 1.435(18) . ? C14A C15A 1.385(15) . ? C14B C15B 1.402(15) . ? C15A C16A 1.364(15) . ? C15A C23A 1.485(13) . ? C15B C16B 1.420(16) . ? C15B C23B 1.511(14) . ? C16A C17A 1.396(16) . ? C16B C17B 1.337(16) . ? C17A C18A 1.362(16) . ? C17A C19A 1.526(17) . ? C17B C18B 1.374(17) . ? C17B C19B 1.566(18) . ? C19B C22B 1.52(3) . ? C19B C20B 1.53(2) . ? C19B C21B 1.56(2) . ? C19A C22A 1.53(2) . ? C19A C20A 1.532(19) . ? C19A C21A 1.59(2) . ? C23B C24B 1.507(15) . ? C23A C24A 1.544(15) . ? C24B C25B 1.370(16) . ? C24B C29B 1.418(15) . ? C24A C29A 1.378(17) . ? C24A C25A 1.404(16) . ? C25A C26A 1.392(9) . ? C25B C26B 1.410(15) . ? C26B C27B 1.379(15) . ? C26B C34B 1.517(15) . ? C26A C27A 1.390(19) . ? C26A C34A 1.524(10) . ? C27B C28B 1.400(15) . ? C27A C28A 1.375(19) . ? C28B C29B 1.382(15) . ? C28B C30B 1.547(16) . ? C28A C29A 1.442(16) . ? C28A C30A 1.50(2) . ? C30A C32A 1.45(3) . ? C30A C33A 1.57(3) . ? C30A C31A 1.57(3) . ? C30B C33B 1.487(18) . ? C30B C32B 1.51(2) . ? C30B C31B 1.555(19) . ? C35B C36B 1.502(15) . ? C35A C36A 1.518(9) . ? C36B C37B 1.395(15) . ? C36B C41B 1.401(15) . ? C36A C41A 1.343(16) . ? C36A C37A 1.428(15) . ? C37B C38B 1.388(14) . ? C37A C38A 1.375(15) . ? C38B C39B 1.361(14) . ? C38B C46B 1.524(14) . ? C38A C39A 1.351(16) . ? C38A C46A 1.531(14) . ? C39A C40A 1.398(18) . ? C39B C40B 1.394(16) . ? C40B C41B 1.453(15) . ? C40B C42B 1.517(16) . ? C40A C41A 1.350(18) . ? C40A C42A 1.53(2) . ? C42A C44A 1.52(3) . ? C42A C45A 1.52(3) . ? C42A C43A 1.52(4) . ? C42B C45B 1.516(9) . ? C42B C44B 1.53(3) . ? C42B C43B 1.55(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ba O7 140.9(4) . . ? O2 Ba O4 107.8(3) . . ? O7 Ba O4 72.5(4) . . ? O2 Ba O5 99.6(3) . . ? O7 Ba O5 70.7(3) . . ? O4 Ba O5 143.2(4) . . ? O2 Ba O1 58.7(3) . . ? O7 Ba O1 145.1(3) . . ? O4 Ba O1 137.6(4) . . ? O5 Ba O1 78.0(3) . . ? O2 Ba O3 141.7(3) . . ? O7 Ba O3 74.1(4) . . ? O4 Ba O3 60.9(3) . . ? O5 Ba O3 109.5(3) . . ? O1 Ba O3 103.1(3) . . ? O2 Ba O6 70.7(4) . . ? O7 Ba O6 72.2(5) . . ? O4 Ba O6 107.9(4) . . ? O5 Ba O6 58.7(4) . . ? O1 Ba O6 104.3(4) . . ? O3 Ba O6 146.3(4) . . ? O2 Ba N2 60.4(3) . . ? O7 Ba N2 89.6(4) . . ? O4 Ba N2 60.6(3) . . ? O5 Ba N2 117.2(3) . . ? O1 Ba N2 118.9(3) . . ? O3 Ba N2 121.5(3) . . ? O6 Ba N2 58.5(4) . . ? O2 Ba N1 118.6(3) . . ? O7 Ba N1 90.3(4) . . ? O4 Ba N1 121.6(3) . . ? O5 Ba N1 60.6(4) . . ? O1 Ba N1 60.3(3) . . ? O3 Ba N1 60.7(3) . . ? O6 Ba N1 119.3(4) . . ? N2 Ba N1 177.6(4) . . ? O2 Ba O8 65.7(3) . . ? O7 Ba O8 142.4(3) . . ? O4 Ba O8 73.3(4) . . ? O5 Ba O8 142.2(3) . . ? O1 Ba O8 64.5(3) . . ? O3 Ba O8 76.1(3) . . ? O6 Ba O8 134.0(4) . . ? N2 Ba O8 86.8(3) . . ? N1 Ba O8 94.6(4) . . ? C13 N1 C7 112.9(18) . . ? C13 N1 C1 117(2) . . ? C7 N1 C1 103.8(14) . . ? C13 N1 Ba 108.5(18) . . ? C7 N1 Ba 110.6(9) . . ? C1 N1 Ba 103.2(11) . . ? C12 N2 C18 112.9(15) . . ? C12 N2 C6 107.2(14) . . ? C18 N2 C6 106.7(14) . . ? C12 N2 Ba 112.1(11) . . ? C18 N2 Ba 113.8(10) . . ? C6 N2 Ba 103.4(9) . . ? C2 O1 C3 110.2(11) . . ? C2 O1 Ba 128.7(9) . . ? C3 O1 Ba 110.3(7) . . ? C4 O2 C5 111.7(10) . . ? C4 O2 Ba 124.8(7) . . ? C5 O2 Ba 120.7(8) . . ? C9 O3 C8 108.1(11) . . ? C9 O3 Ba 114.0(9) . . ? C8 O3 Ba 108.6(9) . . ? C11 O4 C10 116.7(13) . . ? C11 O4 Ba 123.2(11) . . ? C10 O4 Ba 116.9(8) . . ? C14 O5 C15 111.9(16) . . ? C14 O5 Ba 126.7(15) . . ? C15 O5 Ba 114.6(9) . . ? C17 O6 C16 108.0(12) . . ? C17 O6 Ba 115.3(13) . . ? C16 O6 Ba 120.8(10) . . ? O10 O7 Ba 127.9(5) . . ? O10 O7 O9 99.0(6) . . ? Ba O7 O9 127.8(6) . . ? O3A O9 O7 108.6(6) 2_574 . ? O7 O10 O4A 114.7(6) . 2_574 ? C2 C1 N1 122.1(18) . . ? O1 C2 C1 104.8(16) . . ? O1 C3 C4 112.3(10) . . ? O2 C4 C3 108.7(9) . . ? C6 C5 O2 113.5(13) . . ? C5 C6 N2 112.4(15) . . ? N1 C7 C8 117.2(14) . . ? C7 C8 O3 104.6(13) . . ? O3 C9 C10 105.8(13) . . ? O4 C10 C9 112.6(13) . . ? O4 C11 C12 112.6(18) . . ? N2 C12 C11 113.5(18) . . ? N1 C13 C14 130(3) . . ? O5 C14 C13 105(2) . . ? O5 C15 C16 114.1(14) . . ? O6 C16 C15 100.5(13) . . ? O6 C17 C18 102.7(18) . . ? N2 C18 C17 108.7(19) . . ? C12A O2A C11A 111.6(11) . . ? C34A O5A C35A 106.8(11) . . ? C11B O2B C12B 113.3(11) . . ? C34B O5B C35B 111.1(8) . . ? C2A C1A C6A 119.6(11) . . ? C2A C1A C46A 118.0(11) . . ? C6A C1A C46A 122.4(10) . . ? C6B C1B C2B 117.4(10) . . ? C6B C1B C46B 120.4(10) . . ? C2B C1B C46B 122.2(10) . . ? C1A C2A O1A 119.3(11) . . ? C1A C2A C3A 119.0(12) . . ? O1A C2A C3A 121.7(11) . . ? O1B C2B C3B 117.2(10) . . ? O1B C2B C1B 122.9(10) . . ? C3B C2B C1B 119.9(11) . . ? C4A C3A C2A 119.5(12) . . ? C4A C3A C11A 118.2(14) . . ? C2A C3A C11A 122.1(14) . . ? C4B C3B C2B 118.2(12) . . ? C4B C3B C11B 121.4(14) . . ? C2B C3B C11B 119.4(13) . . ? C3A C4A C5A 123.4(14) . . ? C3B C4B C5B 123.6(13) . . ? C4A C5A C6A 116.1(12) . . ? C4A C5A C7A 120.2(11) . . ? C6A C5A C7A 123.7(12) . . ? C6B C5B C4B 114.2(11) . . ? C6B C5B C7B 124.8(12) . . ? C4B C5B C7B 120.5(12) . . ? C1A C6A C5A 122.2(11) . . ? C1B C6B C5B 125.7(10) . . ? C8A C7A C9A 111.2(14) . . ? C8A C7A C10A 110.4(11) . . ? C9A C7A C10A 104.3(13) . . ? C8A C7A C5A 112.2(12) . . ? C9A C7A C5A 112.1(10) . . ? C10A C7A C5A 106.3(13) . . ? C8B C7B C9B 111.4(14) . . ? C8B C7B C10B 108.3(13) . . ? C9B C7B C10B 110.1(11) . . ? C8B C7B C5B 107.4(10) . . ? C9B C7B C5B 110.4(12) . . ? C10B C7B C5B 109.2(13) . . ? C3A C11A O2A 114.0(13) . . ? O2B C11B C3B 111.2(14) . . ? O2B C12B C13B 109.6(10) . . ? O2A C12A C13A 112.7(15) . . ? C18B C13B C14B 119.3(11) . . ? C18B C13B C12B 120.9(10) . . ? C14B C13B C12B 119.7(11) . . ? C18A C13A C14A 119.9(11) . . ? C18A C13A C12A 120.5(12) . . ? C14A C13A C12A 119.5(12) . . ? O3A C14A C15A 122.8(11) . . ? O3A C14A C13A 119.5(11) . . ? C15A C14A C13A 117.7(10) . . ? O3B C14B C15B 118.6(10) . . ? O3B C14B C13B 121.0(10) . . ? C15B C14B C13B 120.4(11) . . ? C16A C15A C14A 119.2(9) . . ? C16A C15A C23A 121.3(10) . . ? C14A C15A C23A 119.4(10) . . ? C14B C15B C16B 116.2(10) . . ? C14B C15B C23B 121.9(10) . . ? C16B C15B C23B 121.8(10) . . ? C15A C16A C17A 124.1(10) . . ? C17B C16B C15B 123.0(12) . . ? C18A C17A C16A 116.6(11) . . ? C18A C17A C19A 117.7(11) . . ? C16A C17A C19A 125.3(11) . . ? C16B C17B C18B 119.5(11) . . ? C16B C17B C19B 121.3(11) . . ? C18B C17B C19B 119.2(10) . . ? C13B C18B C17B 121.5(11) . . ? C17A C18A C13A 121.9(12) . . ? C22B C19B C20B 112.1(15) . . ? C22B C19B C21B 105.4(15) . . ? C20B C19B C21B 105.4(13) . . ? C22B C19B C17B 112.9(13) . . ? C20B C19B C17B 111.4(13) . . ? C21B C19B C17B 109.2(12) . . ? C17A C19A C22A 113.7(14) . . ? C17A C19A C20A 109.0(10) . . ? C22A C19A C20A 108.2(12) . . ? C17A C19A C21A 109.6(12) . . ? C22A C19A C21A 108.9(14) . . ? C20A C19A C21A 107.3(14) . . ? C24B C23B C15B 113.3(9) . . ? C15A C23A C24A 113.5(9) . . ? C25B C24B C29B 117.8(10) . . ? C25B C24B C23B 123.4(10) . . ? C29B C24B C23B 118.7(10) . . ? C29A C24A C25A 120.5(10) . . ? C29A C24A C23A 119.9(10) . . ? C25A C24A C23A 119.5(10) . . ? O4A C25A C26A 120.4(11) . . ? O4A C25A C24A 122.0(10) . . ? C26A C25A C24A 117.6(11) . . ? O4B C25B C24B 119.6(10) . . ? O4B C25B C26B 119.6(11) . . ? C24B C25B C26B 120.6(10) . . ? C27B C26B C25B 119.4(11) . . ? C27B C26B C34B 120.0(10) . . ? C25B C26B C34B 120.1(10) . . ? C27A C26A C25A 121.0(12) . . ? C27A C26A C34A 113.1(15) . . ? C25A C26A C34A 121.6(16) . . ? C26B C27B C28B 122.3(10) . . ? C28A C27A C26A 123.6(13) . . ? C29B C28B C27B 116.4(10) . . ? C29B C28B C30B 122.4(10) . . ? C27B C28B C30B 121.2(10) . . ? C27A C28A C29A 114.5(13) . . ? C27A C28A C30A 118.8(12) . . ? C29A C28A C30A 126.6(14) . . ? C24A C29A C28A 122.7(11) . . ? C28B C29B C24B 123.4(11) . . ? C32A C30A C28A 111.5(16) . . ? C32A C30A C33A 109.1(16) . . ? C28A C30A C33A 111.1(15) . . ? C32A C30A C31A 112.1(18) . . ? C28A C30A C31A 105.8(17) . . ? C33A C30A C31A 107.1(18) . . ? C33B C30B C32B 111.1(12) . . ? C33B C30B C28B 113.1(10) . . ? C32B C30B C28B 109.4(11) . . ? C33B C30B C31B 109.1(11) . . ? C32B C30B C31B 105.7(12) . . ? C28B C30B C31B 108.1(11) . . ? O5B C34B C26B 110.7(9) . . ? O5A C34A C26A 98.3(12) . . ? O5B C35B C36B 110.1(9) . . ? O5A C35A C36A 112.9(10) . . ? C37B C36B C41B 121.6(10) . . ? C37B C36B C35B 119.5(10) . . ? C41B C36B C35B 118.8(10) . . ? C41A C36A C37A 118.4(9) . . ? C41A C36A C35A 121.9(11) . . ? C37A C36A C35A 119.7(12) . . ? O6B C37B C38B 121.9(9) . . ? O6B C37B C36B 120.5(10) . . ? C38B C37B C36B 117.6(10) . . ? O6A C37A C38A 121.0(10) . . ? O6A C37A C36A 120.7(10) . . ? C38A C37A C36A 118.1(10) . . ? C39B C38B C37B 121.4(9) . . ? C39B C38B C46B 118.3(9) . . ? C37B C38B C46B 120.2(9) . . ? C39A C38A C37A 119.4(10) . . ? C39A C38A C46A 122.3(10) . . ? C37A C38A C46A 118.3(10) . . ? C38A C39A C40A 124.1(11) . . ? C38B C39B C40B 124.4(10) . . ? C39B C40B C41B 114.4(10) . . ? C39B C40B C42B 122.4(10) . . ? C41B C40B C42B 123.2(10) . . ? C41A C40A C39A 114.5(12) . . ? C41A C40A C42A 123.4(13) . . ? C39A C40A C42A 122.1(13) . . ? C36B C41B C40B 120.5(10) . . ? C36A C41A C40A 125.4(11) . . ? C44A C42A C45A 119(2) . . ? C44A C42A C43A 103.7(19) . . ? C45A C42A C43A 104.1(19) . . ? C44A C42A C40A 114.6(17) . . ? C45A C42A C40A 109.0(17) . . ? C43A C42A C40A 104(2) . . ? C45B C42B C40B 116.0(12) . . ? C45B C42B C44B 112.9(16) . . ? C40B C42B C44B 111.6(14) . . ? C45B C42B C43B 103.5(8) . . ? C40B C42B C43B 110.0(13) . . ? C44B C42B C43B 101.5(8) . . ? C1A C46A C38A 111.7(8) . . ? C1B C46B C38B 115.4(9) . . ? 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 O1A H1A O2A 0.89 2.11 2.921(13) 149.9 . O1A H1A O3A 0.89 2.28 2.873(12) 123.2 . O3A H3A O4A 0.88 1.64 2.506(13) 168.3 . O6A H6A O4A 0.93 2.28 2.970(14) 130.5 . O1B H1B O6B 0.83 1.78 2.559(11) 157.3 . O3B H3B O2B 0.97 2.01 2.844(14) 142.8 . O3B H3B O1B 0.97 2.30 2.987(12) 127.4 . O4B H4B O3B 0.96 2.45 3.236(13) 139.1 . #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 606961' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H114 N2 O21 Sr U' _chemical_formula_weight 1621.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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 16.1945(6) _cell_length_b 22.5902(9) _cell_length_c 20.9304(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.591(2) _cell_angle_gamma 90.00 _cell_volume 7442.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 49067 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method ? _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 2.960 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 30 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' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 49067 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.68 _reflns_number_total 13853 _reflns_number_gt 10370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (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)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. One tert-butyl group is disordered with two positions of the terminal C atoms which have been refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, except the disordered ones. Some restraints on bond lengths and/or displacement parameters were applied for the disordered group and the atoms of the solvent methanol and water molecules. The O-bound H atoms of the methanol and water molecules have been found on a Fourier difference map, except those of O17 and O21. All the other H atoms 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. 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^)+(0.0471P)^2^+13.4333P] 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 13853 _refine_ls_number_parameters 855 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.711 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.121 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 0.306941(14) 0.375715(9) 0.685979(10) 0.02558(7) Uani 1 1 d . . . Sr Sr 0.41332(4) 0.17695(2) 0.91185(3) 0.02927(13) Uani 1 1 d . . . O1 O 0.4020(3) 0.44574(16) 0.72770(19) 0.0282(9) Uani 1 1 d . . . O2 O 0.3130(3) 0.46312(16) 0.8379(2) 0.0288(9) Uani 1 1 d . . . O3 O 0.1900(3) 0.41961(17) 0.70873(19) 0.0303(9) Uani 1 1 d . . . O4 O 0.2139(3) 0.30424(18) 0.6395(2) 0.0311(9) Uani 1 1 d . . . O5 O 0.3507(3) 0.20369(18) 0.66282(19) 0.0300(9) Uani 1 1 d . . . O6 O 0.4134(2) 0.32844(17) 0.65208(18) 0.0269(9) Uani 1 1 d . . . O7 O 0.2825(3) 0.41447(18) 0.6082(2) 0.0323(9) Uani 1 1 d . . . O8 O 0.3302(3) 0.33644(17) 0.76285(19) 0.0307(9) Uani 1 1 d . . . O9 O 0.3636(3) 0.28986(18) 0.9084(2) 0.0360(10) Uani 1 1 d . . . O10 O 0.2458(3) 0.20277(19) 0.8818(2) 0.0370(10) Uani 1 1 d . . . O11 O 0.5275(3) 0.17395(18) 1.0270(2) 0.0324(9) Uani 1 1 d . . . O12 O 0.4381(3) 0.07132(18) 0.9747(2) 0.0338(10) Uani 1 1 d . . . O13 O 0.5755(3) 0.1541(2) 0.9002(2) 0.0411(11) Uani 1 1 d . . . O14 O 0.4436(3) 0.0958(2) 0.8213(2) 0.0414(11) Uani 1 1 d . . . O15 O 0.3829(3) 0.22006(19) 0.7966(2) 0.0410(11) Uani 1 1 d . . . H15A H 0.3697 0.2599 0.7925 0.049 Uiso 1 1 d R . . H15B H 0.3502 0.2007 0.7628 0.049 Uiso 1 1 d R . . O16 O 0.3437(3) 0.18369(18) 1.0104(2) 0.0342(10) Uani 1 1 d . . . H16A H 0.3767 0.1754 1.0499 0.041 Uiso 1 1 d R . . H16B H 0.2856 0.1776 0.9952 0.041 Uiso 1 1 d R . . N1 N 0.5411(4) 0.2699(2) 0.9366(2) 0.0364(12) Uani 1 1 d . . . N2 N 0.2970(4) 0.0850(2) 0.8606(3) 0.0398(13) Uani 1 1 d . . . C1 C 0.5478(4) 0.4265(3) 0.7779(3) 0.0266(12) Uani 1 1 d . . . C2 C 0.4672(4) 0.4495(2) 0.7794(3) 0.0268(12) Uani 1 1 d . . . C3 C 0.4591(4) 0.4807(2) 0.8360(3) 0.0273(12) Uani 1 1 d . . . C4 C 0.5293(4) 0.4895(2) 0.8881(3) 0.0298(13) Uani 1 1 d . . . H4 H 0.5222 0.5107 0.9246 0.036 Uiso 1 1 calc R . . C5 C 0.6096(4) 0.4681(3) 0.8878(3) 0.0281(13) Uani 1 1 d . . . C6 C 0.6156(4) 0.4357(3) 0.8316(3) 0.0298(13) Uani 1 1 d . . . H6 H 0.6679 0.4194 0.8304 0.036 Uiso 1 1 calc R . . C7 C 0.6875(4) 0.4795(3) 0.9435(3) 0.0331(14) Uani 1 1 d . . . C8 C 0.7141(5) 0.4225(3) 0.9818(4) 0.060(2) Uani 1 1 d . . . H8A H 0.6686 0.4089 1.0003 0.089 Uiso 1 1 calc R . . H8B H 0.7636 0.4298 1.0164 0.089 Uiso 1 1 calc R . . H8C H 0.7269 0.3928 0.9527 0.089 Uiso 1 1 calc R . . C9 C 0.6710(4) 0.5276(3) 0.9901(3) 0.0448(17) Uani 1 1 d . . . H9A H 0.6540 0.5634 0.9658 0.067 Uiso 1 1 calc R . . H9B H 0.7219 0.5348 1.0234 0.067 Uiso 1 1 calc R . . H9C H 0.6266 0.5150 1.0104 0.067 Uiso 1 1 calc R . . C10 C 0.7617(4) 0.5015(3) 0.9151(4) 0.0452(17) Uani 1 1 d . . . H10A H 0.7763 0.4716 0.8871 0.068 Uiso 1 1 calc R . . H10B H 0.8100 0.5097 0.9505 0.068 Uiso 1 1 calc R . . H10C H 0.7450 0.5369 0.8901 0.068 Uiso 1 1 calc R . . C11 C 0.3743(4) 0.5084(3) 0.8356(3) 0.0293(13) Uani 1 1 d . . . H11A H 0.3799 0.5343 0.8733 0.035 Uiso 1 1 calc R . . H11B H 0.3554 0.5319 0.7961 0.035 Uiso 1 1 calc R . . C12 C 0.2286(4) 0.4868(3) 0.8240(3) 0.0303(13) Uani 1 1 d . . . H12A H 0.2187 0.5105 0.7844 0.036 Uiso 1 1 calc R . . H12B H 0.2218 0.5120 0.8600 0.036 Uiso 1 1 calc R . . C13 C 0.1660(4) 0.4374(3) 0.8152(3) 0.0291(13) Uani 1 1 d . . . C14 C 0.1490(4) 0.4053(3) 0.7566(3) 0.0304(13) Uani 1 1 d . . . C15 C 0.0864(4) 0.3605(3) 0.7457(3) 0.0303(13) Uani 1 1 d . . . C16 C 0.0454(4) 0.3485(3) 0.7963(3) 0.0339(14) Uani 1 1 d . . . H16 H 0.0040 0.3192 0.7893 0.041 Uiso 1 1 calc R . . C17 C 0.0630(4) 0.3778(3) 0.8560(3) 0.0366(14) Uani 1 1 d . A . C18 C 0.1237(4) 0.4235(3) 0.8638(3) 0.0318(13) Uani 1 1 d . . . H18A H 0.1358 0.4450 0.9028 0.038 Uiso 1 1 calc R . . C19 C 0.0185(4) 0.3630(3) 0.9117(3) 0.0447(17) Uani 1 1 d D . . C20A C -0.0758(7) 0.3790(8) 0.8858(8) 0.052(5) Uiso 0.451(11) 1 d PD A 1 H20A H -0.0957 0.3636 0.8421 0.078 Uiso 0.451(11) 1 calc PR A 1 H20B H -0.0821 0.4213 0.8849 0.078 Uiso 0.451(11) 1 calc PR A 1 H20C H -0.1084 0.3622 0.9141 0.078 Uiso 0.451(11) 1 calc PR A 1 C21A C 0.0545(13) 0.3957(8) 0.9749(7) 0.067(6) Uiso 0.451(11) 1 d PD A 1 H21A H 0.0254 0.3835 1.0077 0.100 Uiso 0.451(11) 1 calc PR A 1 H21B H 0.0471 0.4375 0.9675 0.100 Uiso 0.451(11) 1 calc PR A 1 H21C H 0.1139 0.3869 0.9897 0.100 Uiso 0.451(11) 1 calc PR A 1 C22A C 0.0165(12) 0.2956(4) 0.9195(8) 0.050(5) Uiso 0.451(11) 1 d PD A 1 H22A H -0.0214 0.2854 0.9468 0.075 Uiso 0.451(11) 1 calc PR A 1 H22B H 0.0726 0.2815 0.9394 0.075 Uiso 0.451(11) 1 calc PR A 1 H22C H -0.0030 0.2776 0.8770 0.075 Uiso 0.451(11) 1 calc PR A 1 C20B C -0.0258(10) 0.4183(5) 0.9302(8) 0.061(4) Uiso 0.549(11) 1 d PD A 2 H20D H -0.0674 0.4320 0.8925 0.092 Uiso 0.549(11) 1 calc PR A 2 H20E H 0.0156 0.4489 0.9448 0.092 Uiso 0.549(11) 1 calc PR A 2 H20F H -0.0533 0.4088 0.9648 0.092 Uiso 0.549(11) 1 calc PR A 2 C21B C 0.0851(8) 0.3494(7) 0.9764(6) 0.057(4) Uiso 0.549(11) 1 d PD A 2 H21D H 0.0574 0.3473 1.0122 0.085 Uiso 0.549(11) 1 calc PR A 2 H21E H 0.1270 0.3803 0.9848 0.085 Uiso 0.549(11) 1 calc PR A 2 H21F H 0.1123 0.3123 0.9723 0.085 Uiso 0.549(11) 1 calc PR A 2 C22B C -0.0414(10) 0.3114(6) 0.8995(8) 0.066(5) Uiso 0.549(11) 1 d PD A 2 H22D H -0.0641 0.3050 0.9373 0.099 Uiso 0.549(11) 1 calc PR A 2 H22E H -0.0116 0.2767 0.8911 0.099 Uiso 0.549(11) 1 calc PR A 2 H22F H -0.0870 0.3196 0.8620 0.099 Uiso 0.549(11) 1 calc PR A 2 C23 C 0.0597(4) 0.3295(3) 0.6800(3) 0.0340(14) Uani 1 1 d . . . H23A H 0.0774 0.3537 0.6474 0.041 Uiso 1 1 calc R . . H23B H -0.0019 0.3280 0.6681 0.041 Uiso 1 1 calc R . . C24 C 0.0927(4) 0.2672(3) 0.6750(3) 0.0336(14) Uani 1 1 d . . . C25 C 0.1699(4) 0.2579(3) 0.6550(3) 0.0291(13) Uani 1 1 d . . . C26 C 0.1964(4) 0.1998(3) 0.6463(3) 0.0287(13) Uani 1 1 d . . . C27 C 0.1455(4) 0.1518(3) 0.6557(3) 0.0314(13) Uani 1 1 d . . . H27 H 0.1632 0.1136 0.6490 0.038 Uiso 1 1 calc R . . C28 C 0.0692(4) 0.1598(3) 0.6746(3) 0.0328(14) Uani 1 1 d . . . C29 C 0.0449(4) 0.2181(3) 0.6839(3) 0.0335(14) Uani 1 1 d . . . H29 H -0.0057 0.2242 0.6967 0.040 Uiso 1 1 calc R . . C30 C 0.0089(4) 0.1078(3) 0.6793(3) 0.0370(15) Uani 1 1 d . . . C31 C 0.0505(5) 0.0476(3) 0.6740(5) 0.061(2) Uani 1 1 d . . . H31A H 0.1010 0.0439 0.7085 0.092 Uiso 1 1 calc R . . H31B H 0.0650 0.0447 0.6322 0.092 Uiso 1 1 calc R . . H31C H 0.0115 0.0166 0.6778 0.092 Uiso 1 1 calc R . . C32 C -0.0713(4) 0.1132(3) 0.6224(3) 0.0469(18) Uani 1 1 d . . . H32A H -0.1105 0.0822 0.6259 0.070 Uiso 1 1 calc R . . H32B H -0.0554 0.1099 0.5811 0.070 Uiso 1 1 calc R . . H32C H -0.0976 0.1510 0.6247 0.070 Uiso 1 1 calc R . . C33 C -0.0191(5) 0.1096(3) 0.7440(3) 0.0451(17) Uani 1 1 d . . . H33A H -0.0445 0.1473 0.7485 0.068 Uiso 1 1 calc R . . H33B H 0.0293 0.1039 0.7800 0.068 Uiso 1 1 calc R . . H33C H -0.0598 0.0788 0.7443 0.068 Uiso 1 1 calc R . . C34 C 0.2719(4) 0.1894(3) 0.6172(3) 0.0324(14) Uani 1 1 d . . . H34A H 0.2729 0.1482 0.6043 0.039 Uiso 1 1 calc R . . H34B H 0.2662 0.2135 0.5780 0.039 Uiso 1 1 calc R . . C35 C 0.4191(4) 0.2048(3) 0.6301(3) 0.0306(13) Uani 1 1 d . . . H35A H 0.3994 0.2228 0.5871 0.037 Uiso 1 1 calc R . . H35B H 0.4362 0.1645 0.6237 0.037 Uiso 1 1 calc R . . C36 C 0.4945(4) 0.2388(2) 0.6685(3) 0.0263(12) Uani 1 1 d . . . C37 C 0.4865(4) 0.3005(3) 0.6775(3) 0.0287(13) Uani 1 1 d . . . C38 C 0.5612(4) 0.3321(2) 0.7091(3) 0.0266(13) Uani 1 1 d . . . C39 C 0.6381(4) 0.3022(3) 0.7287(3) 0.0292(13) Uani 1 1 d . . . H39 H 0.6858 0.3235 0.7498 0.035 Uiso 1 1 calc R . . C40 C 0.6473(4) 0.2420(3) 0.7184(3) 0.0296(13) Uani 1 1 d . . . C41 C 0.5730(4) 0.2111(3) 0.6890(3) 0.0311(13) Uani 1 1 d . . . H41 H 0.5763 0.1705 0.6828 0.037 Uiso 1 1 calc R . . C42 C 0.7367(4) 0.2143(3) 0.7316(3) 0.0368(15) Uani 1 1 d . . . C43 C 0.7925(5) 0.2337(4) 0.7972(4) 0.057(2) Uani 1 1 d . . . H43A H 0.7975 0.2760 0.7981 0.086 Uiso 1 1 calc R . . H43B H 0.8478 0.2162 0.8029 0.086 Uiso 1 1 calc R . . H43C H 0.7673 0.2210 0.8321 0.086 Uiso 1 1 calc R . . C44 C 0.7795(5) 0.2364(4) 0.6778(4) 0.060(2) Uani 1 1 d . . . H44A H 0.7519 0.2191 0.6365 0.089 Uiso 1 1 calc R . . H44B H 0.8383 0.2253 0.6888 0.089 Uiso 1 1 calc R . . H44C H 0.7750 0.2788 0.6747 0.089 Uiso 1 1 calc R . . C45 C 0.7338(4) 0.1472(3) 0.7298(4) 0.0450(17) Uani 1 1 d . . . H45A H 0.6975 0.1332 0.7569 0.067 Uiso 1 1 calc R . . H45B H 0.7900 0.1317 0.7460 0.067 Uiso 1 1 calc R . . H45C H 0.7119 0.1341 0.6854 0.067 Uiso 1 1 calc R . . C46 C 0.5603(4) 0.3992(2) 0.7150(3) 0.0269(12) Uani 1 1 d . . . H46A H 0.6138 0.4139 0.7079 0.032 Uiso 1 1 calc R . . H46B H 0.5157 0.4141 0.6793 0.032 Uiso 1 1 calc R . . C47 C 0.5004(5) 0.3257(3) 0.9076(3) 0.0430(16) Uani 1 1 d . . . H47A H 0.4904 0.3231 0.8601 0.052 Uiso 1 1 calc R . . H47B H 0.5396 0.3581 0.9219 0.052 Uiso 1 1 calc R . . C48 C 0.4187(5) 0.3399(3) 0.9249(3) 0.0416(16) Uani 1 1 d . . . H48A H 0.4284 0.3483 0.9715 0.050 Uiso 1 1 calc R . . H48B H 0.3930 0.3744 0.9007 0.050 Uiso 1 1 calc R . . C49 C 0.2775(5) 0.3030(3) 0.9101(4) 0.0443(17) Uani 1 1 d . . . H49A H 0.2640 0.3437 0.8970 0.053 Uiso 1 1 calc R . . H49B H 0.2697 0.2977 0.9543 0.053 Uiso 1 1 calc R . . C50 C 0.2204(5) 0.2618(3) 0.8638(3) 0.0431(17) Uani 1 1 d . . . H50A H 0.1619 0.2678 0.8662 0.052 Uiso 1 1 calc R . . H50B H 0.2246 0.2695 0.8190 0.052 Uiso 1 1 calc R . . C51 C 0.1840(5) 0.1619(3) 0.8481(4) 0.0479(18) Uani 1 1 d . . . H51A H 0.1785 0.1649 0.8010 0.057 Uiso 1 1 calc R . . H51B H 0.1292 0.1704 0.8572 0.057 Uiso 1 1 calc R . . C52 C 0.2127(5) 0.1007(3) 0.8716(4) 0.0454(17) Uani 1 1 d . . . H52A H 0.2149 0.0980 0.9182 0.054 Uiso 1 1 calc R . . H52B H 0.1712 0.0722 0.8490 0.054 Uiso 1 1 calc R . . C53 C 0.5678(4) 0.2739(3) 1.0092(3) 0.0359(15) Uani 1 1 d . . . H53A H 0.5206 0.2883 1.0259 0.043 Uiso 1 1 calc R . . H53B H 0.6137 0.3023 1.0212 0.043 Uiso 1 1 calc R . . C54 C 0.5971(4) 0.2150(3) 1.0415(3) 0.0354(14) Uani 1 1 d . . . H54A H 0.6442 0.1999 1.0250 0.042 Uiso 1 1 calc R . . H54B H 0.6163 0.2202 1.0887 0.042 Uiso 1 1 calc R . . C55 C 0.5574(4) 0.1161(3) 1.0484(3) 0.0352(14) Uani 1 1 d . . . H55A H 0.5897 0.1175 1.0937 0.042 Uiso 1 1 calc R . . H55B H 0.5941 0.1012 1.0215 0.042 Uiso 1 1 calc R . . C56 C 0.4818(4) 0.0760(3) 1.0425(3) 0.0346(14) Uani 1 1 d . . . H56A H 0.5004 0.0372 1.0598 0.041 Uiso 1 1 calc R . . H56B H 0.4439 0.0920 1.0678 0.041 Uiso 1 1 calc R . . C57 C 0.3622(4) 0.0382(3) 0.9674(3) 0.0390(15) Uani 1 1 d . . . H57A H 0.3221 0.0595 0.9868 0.047 Uiso 1 1 calc R . . H57B H 0.3742 0.0004 0.9896 0.047 Uiso 1 1 calc R . . C58 C 0.3249(5) 0.0287(3) 0.8952(3) 0.0405(16) Uani 1 1 d . . . H58A H 0.3671 0.0102 0.8756 0.049 Uiso 1 1 calc R . . H58B H 0.2767 0.0021 0.8896 0.049 Uiso 1 1 calc R . . C59 C 0.6149(4) 0.2559(3) 0.9078(3) 0.0431(17) Uani 1 1 d . . . H59A H 0.6641 0.2467 0.9428 0.052 Uiso 1 1 calc R . . H59B H 0.6284 0.2901 0.8841 0.052 Uiso 1 1 calc R . . C60 C 0.5948(5) 0.2040(3) 0.8616(3) 0.0436(17) Uani 1 1 d . . . H60A H 0.5464 0.2129 0.8258 0.052 Uiso 1 1 calc R . . H60B H 0.6431 0.1948 0.8434 0.052 Uiso 1 1 calc R . . C61 C 0.5899(5) 0.0977(3) 0.8739(4) 0.0506(19) Uani 1 1 d . . . H61A H 0.5857 0.0670 0.9054 0.061 Uiso 1 1 calc R . . H61B H 0.6469 0.0966 0.8667 0.061 Uiso 1 1 calc R . . C62 C 0.5260(5) 0.0855(3) 0.8096(4) 0.0484(19) Uani 1 1 d . . . H62A H 0.5358 0.1117 0.7754 0.058 Uiso 1 1 calc R . . H62B H 0.5309 0.0449 0.7959 0.058 Uiso 1 1 calc R . . C63 C 0.3776(5) 0.0663(3) 0.7749(3) 0.0462(18) Uani 1 1 d . . . H63A H 0.3863 0.0238 0.7780 0.055 Uiso 1 1 calc R . . H63B H 0.3780 0.0786 0.7306 0.055 Uiso 1 1 calc R . . C64 C 0.2951(5) 0.0818(3) 0.7900(3) 0.0479(18) Uani 1 1 d . . . H64A H 0.2766 0.1198 0.7701 0.058 Uiso 1 1 calc R . . H64B H 0.2531 0.0526 0.7698 0.058 Uiso 1 1 calc R . . O17 O 0.1099(5) 0.5093(3) 0.6358(4) 0.098(2) Uani 1 1 d U . . C65 C 0.0188(9) 0.4919(6) 0.6176(7) 0.127(5) Uani 1 1 d U . . H65A H -0.0154 0.5258 0.6011 0.191 Uiso 1 1 calc R . . H65B H 0.0023 0.4767 0.6556 0.191 Uiso 1 1 calc R . . H65C H 0.0105 0.4619 0.5842 0.191 Uiso 1 1 calc R . . O18 O 0.1652(3) 0.3167(2) 0.5072(3) 0.0544(13) Uani 1 1 d U . . H18 H 0.1891 0.3154 0.5517 0.065 Uiso 1 1 d R . . C66 C 0.0929(7) 0.3533(5) 0.4947(6) 0.094(3) Uani 1 1 d U . . H66A H 0.0546 0.3402 0.5205 0.142 Uiso 1 1 calc R . . H66B H 0.0650 0.3513 0.4489 0.142 Uiso 1 1 calc R . . H66C H 0.1098 0.3934 0.5061 0.142 Uiso 1 1 calc R . . O19 O 0.2125(8) 0.6055(5) 0.4635(6) 0.081(4) Uani 1 1 d DU . . H19 H 0.2284 0.5761 0.4889 0.097 Uiso 1 1 d R . . C68 C 0.1757(12) 0.6593(6) 0.4805(9) 0.073(5) Uani 1 1 d DU . . H68A H 0.2004 0.6689 0.5256 0.110 Uiso 1 1 calc R . . H68B H 0.1155 0.6542 0.4745 0.110 Uiso 1 1 calc R . . H68C H 0.1864 0.6908 0.4528 0.110 Uiso 1 1 calc R . . O20 O 0.2373(7) 0.6054(4) 0.3450(5) 0.136(3) Uani 1 1 d U . . H20 H 0.2005 0.6063 0.3765 0.163 Uiso 1 1 d R . . C69 C 0.1623(8) 0.5881(6) 0.2946(6) 0.113(4) Uani 1 1 d U . . H69A H 0.1255 0.5646 0.3143 0.170 Uiso 1 1 calc R . . H69B H 0.1796 0.5654 0.2612 0.170 Uiso 1 1 calc R . . H69C H 0.1326 0.6229 0.2754 0.170 Uiso 1 1 calc R . . O21 O 0.2009(9) 0.5186(6) 0.5417(7) 0.085(4) 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 0.02647(12) 0.02388(11) 0.02700(11) 0.00137(9) 0.00752(8) 0.00147(10) Sr 0.0350(3) 0.0252(3) 0.0283(3) 0.0012(2) 0.0089(2) 0.0033(2) O1 0.032(2) 0.024(2) 0.029(2) -0.0008(16) 0.0079(18) 0.0018(17) O2 0.026(2) 0.023(2) 0.039(2) -0.0001(17) 0.0104(18) 0.0026(17) O3 0.030(2) 0.031(2) 0.030(2) 0.0042(17) 0.0080(18) 0.0065(18) O4 0.026(2) 0.031(2) 0.037(2) -0.0045(18) 0.0094(19) -0.0017(18) O5 0.026(2) 0.033(2) 0.032(2) -0.0047(17) 0.0074(18) -0.0018(18) O6 0.026(2) 0.027(2) 0.028(2) -0.0027(16) 0.0063(17) 0.0034(17) O7 0.031(2) 0.032(2) 0.033(2) 0.0012(18) 0.0057(19) 0.0009(18) O8 0.033(2) 0.028(2) 0.032(2) 0.0000(17) 0.0095(19) 0.0029(18) O9 0.043(3) 0.025(2) 0.041(2) 0.0019(18) 0.014(2) 0.0046(19) O10 0.036(3) 0.038(2) 0.035(2) 0.0021(19) 0.004(2) 0.004(2) O11 0.036(2) 0.030(2) 0.033(2) 0.0036(18) 0.0102(19) 0.0034(19) O12 0.038(3) 0.030(2) 0.034(2) 0.0026(18) 0.008(2) 0.0015(19) O13 0.045(3) 0.044(3) 0.038(3) -0.001(2) 0.017(2) 0.003(2) O14 0.054(3) 0.036(2) 0.033(2) -0.0054(19) 0.008(2) 0.007(2) O15 0.059(3) 0.030(2) 0.034(2) -0.0008(19) 0.009(2) 0.007(2) O16 0.030(2) 0.041(2) 0.030(2) 0.0022(18) 0.0027(19) 0.0011(19) N1 0.041(3) 0.038(3) 0.031(3) 0.002(2) 0.011(2) -0.001(2) N2 0.049(4) 0.030(3) 0.036(3) -0.001(2) 0.001(3) 0.000(2) C1 0.026(3) 0.027(3) 0.028(3) 0.002(2) 0.008(2) -0.001(2) C2 0.033(3) 0.018(3) 0.029(3) 0.003(2) 0.007(3) -0.003(2) C3 0.029(3) 0.022(3) 0.030(3) -0.001(2) 0.006(3) -0.002(2) C4 0.036(4) 0.023(3) 0.031(3) -0.002(2) 0.010(3) 0.000(3) C5 0.024(3) 0.025(3) 0.034(3) 0.006(2) 0.004(3) -0.001(2) C6 0.029(3) 0.027(3) 0.035(3) 0.001(2) 0.011(3) 0.000(3) C7 0.033(4) 0.031(3) 0.034(3) -0.002(3) 0.005(3) -0.002(3) C8 0.060(5) 0.047(4) 0.054(5) 0.005(4) -0.022(4) -0.012(4) C9 0.031(4) 0.066(5) 0.036(4) -0.012(3) 0.002(3) -0.003(3) C10 0.033(4) 0.053(4) 0.050(4) -0.012(3) 0.010(3) -0.006(3) C11 0.024(3) 0.031(3) 0.035(3) -0.002(2) 0.010(3) 0.001(2) C12 0.023(3) 0.027(3) 0.041(3) -0.002(3) 0.008(3) 0.008(2) C13 0.026(3) 0.025(3) 0.037(3) 0.000(2) 0.007(3) 0.006(2) C14 0.027(3) 0.031(3) 0.035(3) 0.002(3) 0.010(3) 0.008(3) C15 0.022(3) 0.034(3) 0.035(3) 0.004(3) 0.008(3) 0.010(2) C16 0.026(3) 0.035(3) 0.042(4) 0.001(3) 0.012(3) -0.001(3) C17 0.029(3) 0.043(4) 0.039(3) 0.001(3) 0.010(3) 0.009(3) C18 0.032(3) 0.030(3) 0.032(3) 0.000(3) 0.005(3) 0.006(3) C19 0.037(4) 0.053(5) 0.049(4) 0.006(3) 0.020(3) 0.001(3) C23 0.029(3) 0.037(3) 0.035(3) 0.004(3) 0.005(3) -0.001(3) C24 0.036(4) 0.034(3) 0.033(3) -0.006(3) 0.012(3) -0.001(3) C25 0.028(3) 0.032(3) 0.026(3) -0.003(2) 0.005(3) -0.007(3) C26 0.021(3) 0.032(3) 0.032(3) -0.005(2) 0.005(3) 0.000(2) C27 0.025(3) 0.032(3) 0.037(3) -0.007(3) 0.008(3) -0.004(3) C28 0.024(3) 0.038(4) 0.036(3) 0.000(3) 0.007(3) 0.001(3) C29 0.029(3) 0.036(3) 0.036(3) -0.006(3) 0.009(3) -0.001(3) C30 0.030(3) 0.040(4) 0.043(4) -0.007(3) 0.013(3) -0.005(3) C31 0.043(5) 0.042(4) 0.106(7) -0.007(4) 0.032(5) -0.012(4) C32 0.035(4) 0.062(5) 0.043(4) -0.005(3) 0.008(3) -0.018(3) C33 0.035(4) 0.051(5) 0.049(4) 0.001(3) 0.010(3) -0.014(3) C34 0.029(3) 0.033(3) 0.035(3) -0.004(3) 0.008(3) -0.003(3) C35 0.029(3) 0.029(3) 0.038(3) -0.003(3) 0.016(3) -0.001(3) C36 0.026(3) 0.026(3) 0.030(3) 0.002(2) 0.014(3) -0.001(2) C37 0.029(3) 0.033(3) 0.027(3) 0.002(2) 0.013(3) 0.000(3) C38 0.031(3) 0.024(3) 0.028(3) 0.001(2) 0.014(3) -0.002(2) C39 0.026(3) 0.030(3) 0.032(3) 0.000(2) 0.008(3) -0.001(3) C40 0.026(3) 0.027(3) 0.037(3) -0.001(2) 0.009(3) -0.004(2) C41 0.032(3) 0.027(3) 0.037(3) -0.002(3) 0.013(3) 0.001(3) C42 0.029(4) 0.027(3) 0.054(4) 0.000(3) 0.009(3) 0.003(3) C43 0.041(5) 0.054(5) 0.070(5) -0.010(4) 0.001(4) 0.011(4) C44 0.041(4) 0.059(5) 0.088(6) 0.016(4) 0.034(4) 0.012(4) C45 0.030(4) 0.032(3) 0.073(5) -0.001(3) 0.012(4) 0.004(3) C46 0.022(3) 0.023(3) 0.037(3) -0.003(2) 0.009(3) -0.003(2) C47 0.051(4) 0.029(3) 0.047(4) 0.010(3) 0.007(3) -0.006(3) C48 0.054(5) 0.022(3) 0.047(4) 0.005(3) 0.007(3) 0.004(3) C49 0.048(4) 0.041(4) 0.047(4) 0.004(3) 0.018(3) 0.016(3) C50 0.041(4) 0.039(4) 0.049(4) 0.014(3) 0.011(3) 0.008(3) C51 0.037(4) 0.043(4) 0.057(5) -0.001(3) -0.001(3) 0.002(3) C52 0.040(4) 0.038(4) 0.053(4) -0.005(3) 0.000(3) -0.008(3) C53 0.041(4) 0.031(3) 0.040(4) 0.003(3) 0.017(3) 0.002(3) C54 0.031(4) 0.038(4) 0.036(3) 0.001(3) 0.007(3) -0.003(3) C55 0.040(4) 0.033(4) 0.034(3) 0.002(3) 0.012(3) 0.005(3) C56 0.044(4) 0.032(3) 0.029(3) 0.007(3) 0.010(3) 0.010(3) C57 0.045(4) 0.025(3) 0.046(4) 0.007(3) 0.009(3) 0.000(3) C58 0.052(4) 0.028(3) 0.037(4) -0.002(3) 0.002(3) -0.007(3) C59 0.039(4) 0.052(4) 0.044(4) 0.005(3) 0.019(3) -0.004(3) C60 0.046(4) 0.050(4) 0.039(4) -0.001(3) 0.019(3) -0.001(3) C61 0.062(5) 0.050(4) 0.047(4) 0.002(3) 0.025(4) 0.019(4) C62 0.066(5) 0.035(4) 0.051(4) 0.000(3) 0.029(4) 0.008(3) C63 0.065(5) 0.035(4) 0.036(4) -0.009(3) 0.006(3) 0.007(3) C64 0.060(5) 0.039(4) 0.039(4) -0.001(3) -0.002(3) -0.002(4) O17 0.097(2) 0.098(2) 0.098(2) 0.0027(10) 0.0235(11) 0.0007(10) C65 0.127(5) 0.127(5) 0.127(5) 0.0002(10) 0.0294(15) -0.0001(10) O18 0.0538(16) 0.0564(16) 0.0531(15) 0.0004(9) 0.0125(10) -0.0005(10) C66 0.094(3) 0.095(3) 0.094(3) -0.0001(10) 0.0224(13) 0.0006(10) O19 0.081(4) 0.081(4) 0.081(4) 0.0006(10) 0.0198(13) -0.0005(10) C68 0.073(5) 0.073(5) 0.073(5) -0.0002(10) 0.0174(16) 0.0004(10) O20 0.135(3) 0.135(3) 0.137(3) 0.0009(10) 0.0314(13) -0.0001(10) C69 0.113(4) 0.113(4) 0.114(4) 0.0003(10) 0.0260(14) -0.0001(10) O21 0.085(4) 0.086(4) 0.086(4) 0.0007(10) 0.0211(14) 0.0009(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O8 1.798(4) . ? U O7 1.808(4) . ? U O1 2.237(4) . ? U O4 2.266(4) . ? U O6 2.278(4) . ? U O3 2.285(4) . ? Sr O15 2.539(4) . ? Sr O16 2.577(4) . ? Sr O9 2.670(4) . ? Sr O11 2.671(4) . ? Sr O10 2.701(4) . ? Sr O12 2.709(4) . ? Sr O13 2.743(5) . ? Sr O14 2.763(4) . ? Sr N2 2.840(6) . ? Sr N1 2.909(6) . ? Sr C60 3.401(7) . ? O1 C2 1.326(7) . ? O2 C12 1.433(7) . ? O2 C11 1.434(7) . ? O3 C14 1.365(7) . ? O3 O17 2.682(9) . ? O4 C25 1.347(7) . ? O5 C35 1.431(6) . ? O5 C34 1.439(7) . ? O6 C37 1.337(7) . ? O7 O21 2.891(15) . ? O9 C48 1.430(8) . ? O9 C49 1.436(8) . ? O10 C50 1.420(7) . ? O10 C51 1.422(8) . ? O11 C55 1.429(7) . ? O11 C54 1.437(7) . ? O12 C57 1.417(8) . ? O12 C56 1.433(7) . ? O13 C61 1.428(8) . ? O13 C60 1.462(8) . ? O14 C63 1.429(8) . ? O14 C62 1.430(8) . ? N1 C53 1.482(8) . ? N1 C47 1.484(8) . ? N1 C59 1.493(8) . ? N2 C64 1.473(8) . ? N2 C52 1.479(9) . ? N2 C58 1.481(8) . ? C1 C6 1.391(8) . ? C1 C2 1.411(8) . ? C1 C46 1.509(8) . ? C2 C3 1.409(8) . ? C3 C4 1.394(8) . ? C3 C11 1.507(8) . ? C4 C5 1.389(8) . ? C5 C6 1.407(8) . ? C5 C7 1.526(8) . ? C7 C8 1.524(9) . ? C7 C9 1.526(9) . ? C7 C10 1.542(9) . ? C12 C13 1.489(8) . ? C13 C18 1.390(8) . ? C13 C14 1.395(8) . ? C14 C15 1.412(9) . ? C15 C16 1.403(8) . ? C15 C23 1.512(8) . ? C16 C17 1.382(9) . ? C17 C18 1.408(9) . ? C17 C19 1.546(9) . ? C19 C22B 1.498(9) . ? C19 C21A 1.507(9) . ? C19 C22A 1.531(9) . ? C19 C20B 1.536(9) . ? C19 C20A 1.539(9) . ? C19 C21B 1.550(9) . ? C23 C24 1.516(8) . ? C24 C29 1.391(9) . ? C24 C25 1.426(8) . ? C25 C26 1.406(8) . ? C26 C27 1.403(8) . ? C26 C34 1.508(8) . ? C27 C28 1.396(8) . ? C28 C29 1.401(9) . ? C28 C30 1.544(9) . ? C30 C33 1.527(9) . ? C30 C31 1.532(10) . ? C30 C32 1.548(10) . ? C35 C36 1.506(8) . ? C36 C41 1.391(8) . ? C36 C37 1.416(8) . ? C37 C38 1.427(8) . ? C38 C39 1.391(8) . ? C38 C46 1.522(8) . ? C39 C40 1.389(8) . ? C40 C41 1.403(8) . ? C40 C42 1.541(8) . ? C42 C45 1.518(9) . ? C42 C43 1.519(10) . ? C42 C44 1.537(9) . ? C47 C48 1.487(10) . ? C49 C50 1.497(10) . ? C51 C52 1.503(10) . ? C53 C54 1.516(8) . ? C55 C56 1.503(9) . ? C57 C58 1.506(9) . ? C59 C60 1.505(9) . ? C61 C62 1.518(11) . ? C63 C64 1.486(10) . ? O17 C65 1.488(15) . ? O17 O21 2.732(15) . ? O18 C66 1.406(12) . ? O19 C68 1.435(19) . ? O20 C69 1.462(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 179.3(2) . . ? O8 U O1 91.10(17) . . ? O7 U O1 89.65(16) . . ? O8 U O4 90.63(17) . . ? O7 U O4 88.63(17) . . ? O1 U O4 177.14(13) . . ? O8 U O6 91.85(16) . . ? O7 U O6 88.19(16) . . ? O1 U O6 87.21(14) . . ? O4 U O6 90.45(14) . . ? O8 U O3 92.16(16) . . ? O7 U O3 87.74(16) . . ? O1 U O3 98.04(14) . . ? O4 U O3 84.17(14) . . ? O6 U O3 173.33(14) . . ? O15 Sr O16 135.52(14) . . ? O15 Sr O9 67.53(13) . . ? O16 Sr O9 77.27(13) . . ? O15 Sr O11 143.60(14) . . ? O16 Sr O11 67.68(13) . . ? O9 Sr O11 100.90(13) . . ? O15 Sr O10 74.67(14) . . ? O16 Sr O10 64.49(13) . . ? O9 Sr O10 60.50(13) . . ? O11 Sr O10 131.33(12) . . ? O15 Sr O12 140.60(13) . . ? O16 Sr O12 72.92(13) . . ? O9 Sr O12 149.76(12) . . ? O11 Sr O12 63.08(13) . . ? O10 Sr O12 109.26(13) . . ? O15 Sr O13 87.92(14) . . ? O16 Sr O13 133.68(14) . . ? O9 Sr O13 117.78(14) . . ? O11 Sr O13 66.50(13) . . ? O10 Sr O13 161.83(13) . . ? O12 Sr O13 80.88(13) . . ? O15 Sr O14 68.22(13) . . ? O16 Sr O14 140.36(14) . . ? O9 Sr O14 135.74(13) . . ? O11 Sr O14 113.89(13) . . ? O10 Sr O14 108.30(14) . . ? O12 Sr O14 73.67(13) . . ? O13 Sr O14 59.05(14) . . ? O15 Sr N2 87.62(15) . . ? O16 Sr N2 88.22(15) . . ? O9 Sr N2 121.28(15) . . ? O11 Sr N2 125.41(14) . . ? O10 Sr N2 61.89(15) . . ? O12 Sr N2 63.19(14) . . ? O13 Sr N2 113.13(15) . . ? O14 Sr N2 57.64(16) . . ? O15 Sr N1 82.13(15) . . ? O16 Sr N1 104.00(14) . . ? O9 Sr N1 60.81(15) . . ? O11 Sr N1 62.93(14) . . ? O10 Sr N1 121.28(14) . . ? O12 Sr N1 122.11(15) . . ? O13 Sr N1 59.72(15) . . ? O14 Sr N1 111.57(15) . . ? N2 Sr N1 167.58(15) . . ? O15 Sr C60 68.07(17) . . ? O16 Sr C60 144.01(16) . . ? O9 Sr C60 95.55(15) . . ? O11 Sr C60 79.50(15) . . ? O10 Sr C60 141.52(16) . . ? O12 Sr C60 105.54(15) . . ? O13 Sr C60 24.68(15) . . ? O14 Sr C60 66.51(16) . . ? N2 Sr C60 124.03(16) . . ? N1 Sr C60 45.16(15) . . ? C2 O1 U 135.0(3) . . ? C12 O2 C11 111.3(4) . . ? C14 O3 U 128.3(3) . . ? C14 O3 O17 110.1(4) . . ? U O3 O17 121.6(2) . . ? C25 O4 U 141.8(4) . . ? C35 O5 C34 110.6(4) . . ? C37 O6 U 139.6(3) . . ? U O7 O21 143.8(3) . . ? C48 O9 C49 112.6(5) . . ? C48 O9 Sr 125.5(4) . . ? C49 O9 Sr 119.0(4) . . ? C50 O10 C51 110.6(5) . . ? C50 O10 Sr 118.5(4) . . ? C51 O10 Sr 121.8(4) . . ? C55 O11 C54 109.5(5) . . ? C55 O11 Sr 114.7(3) . . ? C54 O11 Sr 121.2(3) . . ? C57 O12 C56 111.1(5) . . ? C57 O12 Sr 112.7(3) . . ? C56 O12 Sr 113.4(3) . . ? C61 O13 C60 113.6(5) . . ? C61 O13 Sr 116.7(4) . . ? C60 O13 Sr 103.7(4) . . ? C63 O14 C62 112.8(5) . . ? C63 O14 Sr 123.4(4) . . ? C62 O14 Sr 123.2(4) . . ? C53 N1 C47 111.3(5) . . ? C53 N1 C59 111.0(5) . . ? C47 N1 C59 109.7(5) . . ? C53 N1 Sr 104.5(3) . . ? C47 N1 Sr 108.1(4) . . ? C59 N1 Sr 112.2(4) . . ? C64 N2 C52 111.4(6) . . ? C64 N2 C58 112.3(5) . . ? C52 N2 C58 108.5(5) . . ? C64 N2 Sr 105.7(4) . . ? C52 N2 Sr 108.7(4) . . ? C58 N2 Sr 110.1(4) . . ? C6 C1 C2 119.0(5) . . ? C6 C1 C46 121.5(5) . . ? C2 C1 C46 119.0(5) . . ? O1 C2 C3 120.3(5) . . ? O1 C2 C1 121.4(5) . . ? C3 C2 C1 118.2(5) . . ? C4 C3 C2 120.6(6) . . ? C4 C3 C11 121.2(5) . . ? C2 C3 C11 118.0(5) . . ? C5 C4 C3 122.6(5) . . ? C4 C5 C6 115.7(6) . . ? C4 C5 C7 123.0(5) . . ? C6 C5 C7 121.3(5) . . ? C1 C6 C5 123.8(6) . . ? C8 C7 C5 109.9(5) . . ? C8 C7 C9 109.7(6) . . ? C5 C7 C9 111.8(5) . . ? C8 C7 C10 109.0(6) . . ? C5 C7 C10 109.8(5) . . ? C9 C7 C10 106.6(5) . . ? O2 C11 C3 109.9(5) . . ? O2 C12 C13 109.6(5) . . ? C18 C13 C14 119.8(6) . . ? C18 C13 C12 121.2(5) . . ? C14 C13 C12 119.1(5) . . ? O3 C14 C13 119.6(5) . . ? O3 C14 C15 120.3(5) . . ? C13 C14 C15 120.1(5) . . ? C16 C15 C14 117.6(6) . . ? C16 C15 C23 120.7(6) . . ? C14 C15 C23 121.5(5) . . ? C17 C16 C15 123.8(6) . . ? C16 C17 C18 116.5(6) . . ? C16 C17 C19 123.0(6) . . ? C18 C17 C19 120.5(6) . . ? C13 C18 C17 122.1(6) . . ? C21A C19 C22A 114.1(11) . . ? C22B C19 C20B 110.7(10) . . ? C21A C19 C20A 109.9(11) . . ? C22A C19 C20A 103.2(10) . . ? C22B C19 C17 115.9(8) . . ? C21A C19 C17 113.8(9) . . ? C22A C19 C17 108.7(8) . . ? C20B C19 C17 109.9(7) . . ? C20A C19 C17 106.4(8) . . ? C22B C19 C21B 106.7(10) . . ? C20B C19 C21B 102.2(9) . . ? C17 C19 C21B 110.5(7) . . ? C15 C23 C24 117.5(5) . . ? C29 C24 C25 118.4(6) . . ? C29 C24 C23 121.0(6) . . ? C25 C24 C23 120.3(5) . . ? O4 C25 C26 120.0(5) . . ? O4 C25 C24 120.4(5) . . ? C26 C25 C24 119.4(5) . . ? C27 C26 C25 119.8(5) . . ? C27 C26 C34 119.6(5) . . ? C25 C26 C34 119.9(5) . . ? C28 C27 C26 121.9(6) . . ? C27 C28 C29 117.2(6) . . ? C27 C28 C30 122.3(6) . . ? C29 C28 C30 120.3(5) . . ? C24 C29 C28 123.3(6) . . ? C33 C30 C31 108.4(6) . . ? C33 C30 C28 111.1(5) . . ? C31 C30 C28 112.0(5) . . ? C33 C30 C32 108.1(6) . . ? C31 C30 C32 108.5(6) . . ? C28 C30 C32 108.6(5) . . ? O5 C34 C26 112.0(5) . . ? O5 C35 C36 112.0(5) . . ? C41 C36 C37 120.5(6) . . ? C41 C36 C35 120.2(5) . . ? C37 C36 C35 119.0(5) . . ? O6 C37 C36 120.8(5) . . ? O6 C37 C38 121.6(5) . . ? C36 C37 C38 117.3(5) . . ? C39 C38 C37 119.8(5) . . ? C39 C38 C46 119.0(5) . . ? C37 C38 C46 120.9(5) . . ? C40 C39 C38 123.5(6) . . ? C39 C40 C41 116.2(6) . . ? C39 C40 C42 120.0(5) . . ? C41 C40 C42 123.4(5) . . ? C36 C41 C40 122.6(6) . . ? C45 C42 C43 108.5(6) . . ? C45 C42 C44 108.9(6) . . ? C43 C42 C44 107.1(6) . . ? C45 C42 C40 112.2(5) . . ? C43 C42 C40 112.3(5) . . ? C44 C42 C40 107.7(5) . . ? C1 C46 C38 118.9(5) . . ? N1 C47 C48 114.8(5) . . ? O9 C48 C47 108.1(5) . . ? O9 C49 C50 108.1(5) . . ? O10 C50 C49 108.4(6) . . ? O10 C51 C52 107.9(6) . . ? N2 C52 C51 113.3(6) . . ? N1 C53 C54 113.0(5) . . ? O11 C54 C53 108.9(5) . . ? O11 C55 C56 108.4(5) . . ? O12 C56 C55 109.2(5) . . ? O12 C57 C58 108.5(5) . . ? N2 C58 C57 111.8(5) . . ? N1 C59 C60 110.6(6) . . ? O13 C60 C59 106.8(5) . . ? O13 C60 Sr 51.6(3) . . ? C59 C60 Sr 90.8(4) . . ? O13 C61 C62 111.3(6) . . ? O14 C62 C61 106.7(5) . . ? O14 C63 C64 108.2(5) . . ? N2 C64 C63 114.7(6) . . ? C65 O17 O3 105.3(7) . . ? C65 O17 O21 120.4(8) . . ? O3 O17 O21 101.4(4) . . ? O17 O21 O7 81.5(4) . . ? 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 O15 H15A O8 0.92 1.90 2.803(6) 166.1 . O15 H15B O5 0.89 2.10 2.751(6) 129.4 . O16 H16A O6 0.89 2.08 2.928(6) 157.7 4_566 O16 H16B O18 0.93 2.03 2.876(7) 150.9 4_566 O18 H18 O4 0.92 1.80 2.711(7) 167.0 . O19 H19 O21 0.85 1.83 2.590(19) 148.3 . O20 H20 O19 0.99 1.78 2.604(16) 138.0 . #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 606962' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H120 Ba N2 O24 U' _chemical_formula_weight 1725.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.8244(3) _cell_length_b 22.0852(5) _cell_length_c 29.4456(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.3120(10) _cell_angle_gamma 90.00 _cell_volume 8337.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 46962 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method ? _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 2.477 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.411 _exptl_absorpt_correction_T_max 0.609 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 30 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' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 46962 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14524 _reflns_number_gt 11614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (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)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The methanol and water solvent molecules are badly resolved and some of the methanol molecules were affected with a 0.5 occupancy factor so as both to keep acceptable displacement parameters and to account for some short contacts which indicate that some disordered components cannot be occupied simultaneously (molecules containing O18 and O22 in particular). All non-hydrogen atoms were refined with anisotropic displacement parameters, with some restraints for the displacement parameters of the solvent molecules. Only some of the H atoms bound to O atoms were found on Fourier-difference maps and the other ones were not introduced. The H atoms bound to C atoms 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. 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^)+(0.0783P)^2^+27.2674P] 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 14524 _refine_ls_number_parameters 919 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1511 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.586 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.116 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 0.34799(2) 0.641783(12) 0.831846(9) 0.04767(10) Uani 1 1 d . . . O1 O 0.2062(4) 0.5975(2) 0.79810(17) 0.0513(12) Uani 1 1 d . . . O2 O 0.0757(4) 0.7064(2) 0.82933(18) 0.0567(13) Uani 1 1 d . . . O3 O 0.2606(4) 0.6762(2) 0.89328(17) 0.0514(12) Uani 1 1 d . . . O4 O 0.4939(4) 0.6781(2) 0.86772(18) 0.0530(12) Uani 1 1 d . . . O5 O 0.5947(4) 0.7077(2) 0.77835(17) 0.0504(12) Uani 1 1 d . . . O6 O 0.4398(4) 0.6006(2) 0.77480(17) 0.0506(12) Uani 1 1 d . . . O7 O 0.3680(4) 0.5724(2) 0.86276(18) 0.0540(13) Uani 1 1 d . . . O8 O 0.3297(4) 0.7115(2) 0.80067(17) 0.0507(12) Uani 1 1 d . . . C1 C 0.1839(6) 0.5941(3) 0.7166(3) 0.0499(17) Uani 1 1 d . . . C2 C 0.1504(6) 0.6114(3) 0.7603(3) 0.0500(17) Uani 1 1 d . . . C3 C 0.0536(6) 0.6419(3) 0.7640(3) 0.0491(17) Uani 1 1 d . . . C4 C -0.0064(7) 0.6543(4) 0.7253(3) 0.0542(18) Uani 1 1 d . . . H4 H -0.0697 0.6743 0.7283 0.065 Uiso 1 1 calc R . . C5 C 0.0252(6) 0.6378(4) 0.6820(3) 0.0535(18) Uani 1 1 d . . . C6 C 0.1194(7) 0.6073(3) 0.6796(3) 0.0540(18) Uani 1 1 d . . . H6 H 0.1407 0.5947 0.6511 0.065 Uiso 1 1 calc R . . C7 C -0.0386(7) 0.6521(4) 0.6388(3) 0.062(2) Uani 1 1 d . . . C8 C -0.1437(8) 0.6810(6) 0.6497(3) 0.092(4) Uani 1 1 d . . . H8A H -0.1327 0.7218 0.6599 0.137 Uiso 1 1 calc R . . H8B H -0.1764 0.6581 0.6732 0.137 Uiso 1 1 calc R . . H8C H -0.1878 0.6811 0.6229 0.137 Uiso 1 1 calc R . . C9 C -0.0621(9) 0.5925(5) 0.6131(3) 0.081(3) Uani 1 1 d . . . H9A H -0.1130 0.5999 0.5893 0.122 Uiso 1 1 calc R . . H9B H -0.0886 0.5630 0.6338 0.122 Uiso 1 1 calc R . . H9C H 0.0009 0.5775 0.6001 0.122 Uiso 1 1 calc R . . C10 C 0.0232(7) 0.6939(4) 0.6080(3) 0.065(2) Uani 1 1 d . . . H10A H 0.0360 0.7317 0.6232 0.098 Uiso 1 1 calc R . . H10B H -0.0161 0.7010 0.5804 0.098 Uiso 1 1 calc R . . H10C H 0.0884 0.6752 0.6010 0.098 Uiso 1 1 calc R . . C11 C 0.0150(6) 0.6572(3) 0.8105(3) 0.0510(17) Uani 1 1 d . . . H11A H -0.0579 0.6688 0.8084 0.061 Uiso 1 1 calc R . . H11B H 0.0210 0.6221 0.8301 0.061 Uiso 1 1 calc R . . C12 C 0.0540(6) 0.7147(4) 0.8768(3) 0.0571(19) Uani 1 1 d . . . H12A H 0.0533 0.6757 0.8918 0.069 Uiso 1 1 calc R . . H12B H -0.0143 0.7329 0.8797 0.069 Uiso 1 1 calc R . . C13 C 0.1346(6) 0.7545(4) 0.8991(3) 0.0546(19) Uani 1 1 d . . . C14 C 0.2363(6) 0.7316(3) 0.9071(2) 0.0501(17) Uani 1 1 d . . . C15 C 0.3075(6) 0.7677(4) 0.9317(3) 0.0521(18) Uani 1 1 d . . . C16 C 0.2778(6) 0.8243(4) 0.9468(2) 0.0502(17) Uani 1 1 d . . . H16 H 0.3260 0.8471 0.9635 0.060 Uiso 1 1 calc R . . C17 C 0.1794(6) 0.8489(3) 0.9381(3) 0.0505(17) Uani 1 1 d . . . C18 C 0.1092(6) 0.8126(4) 0.9143(2) 0.0532(18) Uani 1 1 d . . . H18 H 0.0425 0.8274 0.9081 0.064 Uiso 1 1 calc R . . C19 C 0.1491(6) 0.9109(4) 0.9577(3) 0.0531(18) Uani 1 1 d . . . C20 C 0.0526(8) 0.9378(4) 0.9350(4) 0.075(3) Uani 1 1 d . . . H20A H 0.0634 0.9415 0.9029 0.112 Uiso 1 1 calc R . . H20B H 0.0394 0.9771 0.9476 0.112 Uiso 1 1 calc R . . H20C H -0.0061 0.9119 0.9400 0.112 Uiso 1 1 calc R . . C21 C 0.1287(9) 0.9033(4) 1.0091(3) 0.077(3) Uani 1 1 d . . . H21A H 0.0692 0.8776 1.0130 0.115 Uiso 1 1 calc R . . H21B H 0.1156 0.9422 1.0223 0.115 Uiso 1 1 calc R . . H21C H 0.1888 0.8854 1.0238 0.115 Uiso 1 1 calc R . . C22 C 0.2381(7) 0.9566(4) 0.9524(3) 0.060(2) Uani 1 1 d . . . H22A H 0.2981 0.9432 0.9697 0.091 Uiso 1 1 calc R . . H22B H 0.2165 0.9955 0.9632 0.091 Uiso 1 1 calc R . . H22C H 0.2555 0.9596 0.9209 0.091 Uiso 1 1 calc R . . C23 C 0.4159(6) 0.7434(4) 0.9443(3) 0.0542(19) Uani 1 1 d . . . H23A H 0.4317 0.7540 0.9757 0.065 Uiso 1 1 calc R . . H23B H 0.4140 0.6996 0.9424 0.065 Uiso 1 1 calc R . . C24 C 0.5031(6) 0.7660(3) 0.9155(2) 0.0484(17) Uani 1 1 d . . . C25 C 0.5377(6) 0.7325(3) 0.8778(2) 0.0489(17) Uani 1 1 d . . . C26 C 0.6231(6) 0.7530(3) 0.8534(3) 0.0519(18) Uani 1 1 d . . . C27 C 0.6751(6) 0.8063(3) 0.8658(3) 0.0508(17) Uani 1 1 d . . . H27 H 0.7309 0.8195 0.8488 0.061 Uiso 1 1 calc R . . C28 C 0.6447(6) 0.8400(3) 0.9034(3) 0.0499(17) Uani 1 1 d . . . C29 C 0.5588(6) 0.8186(4) 0.9276(3) 0.0508(17) Uani 1 1 d . . . H29 H 0.5378 0.8404 0.9528 0.061 Uiso 1 1 calc R . . C30 C 0.7091(6) 0.8936(3) 0.9222(3) 0.0509(17) Uani 1 1 d . . . C31 C 0.6361(7) 0.9472(4) 0.9349(3) 0.060(2) Uani 1 1 d . . . H31A H 0.5915 0.9350 0.9590 0.089 Uiso 1 1 calc R . . H31B H 0.5943 0.9585 0.9088 0.089 Uiso 1 1 calc R . . H31C H 0.6776 0.9812 0.9447 0.089 Uiso 1 1 calc R . . C32 C 0.7696(7) 0.8731(4) 0.9642(3) 0.058(2) Uani 1 1 d . . . H32A H 0.8166 0.8412 0.9563 0.087 Uiso 1 1 calc R . . H32B H 0.7219 0.8585 0.9864 0.087 Uiso 1 1 calc R . . H32C H 0.8086 0.9066 0.9767 0.087 Uiso 1 1 calc R . . C33 C 0.7883(6) 0.9164(4) 0.8868(3) 0.0568(19) Uani 1 1 d . . . H33A H 0.8269 0.9500 0.8991 0.085 Uiso 1 1 calc R . . H33B H 0.7513 0.9289 0.8596 0.085 Uiso 1 1 calc R . . H33C H 0.8356 0.8842 0.8796 0.085 Uiso 1 1 calc R . . C34 C 0.6670(6) 0.7143(4) 0.8159(3) 0.0558(19) Uani 1 1 d . . . H34A H 0.7308 0.7326 0.8053 0.067 Uiso 1 1 calc R . . H34B H 0.6843 0.6746 0.8280 0.067 Uiso 1 1 calc R . . C35 C 0.6268(6) 0.6589(4) 0.7506(3) 0.0527(18) Uani 1 1 d . . . H35A H 0.6431 0.6241 0.7697 0.063 Uiso 1 1 calc R . . H35B H 0.6896 0.6703 0.7350 0.063 Uiso 1 1 calc R . . C36 C 0.5430(6) 0.6418(3) 0.7161(3) 0.0507(17) Uani 1 1 d . . . C37 C 0.4528(6) 0.6124(3) 0.7307(2) 0.0496(17) Uani 1 1 d . . . C38 C 0.3787(6) 0.5922(3) 0.6972(2) 0.0471(16) Uani 1 1 d . . . C39 C 0.3987(6) 0.6007(3) 0.6516(3) 0.0517(18) Uani 1 1 d . . . H39 H 0.3500 0.5870 0.6300 0.062 Uiso 1 1 calc R . . C40 C 0.4892(7) 0.6291(3) 0.6365(3) 0.0520(18) Uani 1 1 d . . . C41 C 0.5593(7) 0.6496(3) 0.6704(3) 0.0534(18) Uani 1 1 d . . . H41 H 0.6196 0.6694 0.6616 0.064 Uiso 1 1 calc R . . C42 C 0.5182(7) 0.6314(3) 0.5859(3) 0.0528(18) Uani 1 1 d . . . C43 C 0.4241(7) 0.6210(4) 0.5543(3) 0.065(2) Uani 1 1 d . . . H43A H 0.3704 0.6496 0.5612 0.097 Uiso 1 1 calc R . . H43B H 0.3983 0.5806 0.5585 0.097 Uiso 1 1 calc R . . H43C H 0.4444 0.6262 0.5234 0.097 Uiso 1 1 calc R . . C44 C 0.5998(7) 0.5809(4) 0.5772(3) 0.063(2) Uani 1 1 d . . . H44A H 0.6213 0.5828 0.5462 0.095 Uiso 1 1 calc R . . H44B H 0.5692 0.5420 0.5829 0.095 Uiso 1 1 calc R . . H44C H 0.6593 0.5866 0.5971 0.095 Uiso 1 1 calc R . . C45 C 0.5662(7) 0.6935(4) 0.5738(3) 0.059(2) Uani 1 1 d . . . H45A H 0.5833 0.6939 0.5422 0.088 Uiso 1 1 calc R . . H45B H 0.6283 0.7000 0.5919 0.088 Uiso 1 1 calc R . . H45C H 0.5168 0.7250 0.5796 0.088 Uiso 1 1 calc R . . C46 C 0.2821(6) 0.5581(3) 0.7121(3) 0.0538(18) Uani 1 1 d . . . H46A H 0.2684 0.5258 0.6905 0.065 Uiso 1 1 calc R . . H46B H 0.2980 0.5393 0.7412 0.065 Uiso 1 1 calc R . . Ba Ba 0.36525(4) 0.90204(2) 0.705093(15) 0.05013(13) Uani 1 1 d . . . N1 N 0.3278(5) 0.9307(3) 0.8027(2) 0.0542(16) Uani 1 1 d . . . N2 N 0.3890(6) 0.8748(3) 0.6056(2) 0.0591(17) Uani 1 1 d . . . O9 O 0.5359(5) 0.9342(2) 0.76029(18) 0.0585(14) Uani 1 1 d . . . O10 O 0.5661(5) 0.8950(3) 0.67052(19) 0.0604(14) Uani 1 1 d . . . O11 O 0.2422(4) 0.8279(2) 0.75636(18) 0.0557(13) Uani 1 1 d . . . O12 O 0.2632(4) 0.8001(2) 0.66465(19) 0.0580(13) Uani 1 1 d . . . O13 O 0.2037(5) 0.9839(2) 0.73039(18) 0.0585(14) Uani 1 1 d . . . O14 O 0.2427(5) 0.9639(3) 0.63873(19) 0.0605(14) Uani 1 1 d . . . O15 O 0.4559(4) 0.7973(2) 0.74507(19) 0.0591(14) Uani 1 1 d . . . H15A H 0.4828 0.7563 0.7508 0.071 Uiso 1 1 d R . . H15B H 0.3975 0.7834 0.7583 0.071 Uiso 1 1 d R . . O16 O 0.4239(5) 1.0176(2) 0.68618(19) 0.0588(14) Uani 1 1 d . . . H16A H 0.4798 1.0405 0.6923 0.071 Uiso 1 1 d R . . H16B H 0.4116 1.0330 0.6575 0.071 Uiso 1 1 d R . . C47 C 0.4255(7) 0.9573(4) 0.8224(3) 0.061(2) Uani 1 1 d . . . H47C H 0.4224 0.9562 0.8552 0.073 Uiso 1 1 calc R . . H47D H 0.4301 0.9994 0.8132 0.073 Uiso 1 1 calc R . . C48 C 0.5222(7) 0.9244(4) 0.8077(3) 0.063(2) Uani 1 1 d . . . H48C H 0.5825 0.9394 0.8248 0.076 Uiso 1 1 calc R . . H48D H 0.5153 0.8815 0.8137 0.076 Uiso 1 1 calc R . . C49 C 0.6325(7) 0.9091(4) 0.7456(3) 0.063(2) Uani 1 1 d . . . H49C H 0.6320 0.8655 0.7491 0.075 Uiso 1 1 calc R . . H49D H 0.6901 0.9254 0.7637 0.075 Uiso 1 1 calc R . . C50 C 0.6444(7) 0.9254(4) 0.6973(3) 0.062(2) Uani 1 1 d . . . H50C H 0.6373 0.9689 0.6935 0.075 Uiso 1 1 calc R . . H50D H 0.7131 0.9137 0.6873 0.075 Uiso 1 1 calc R . . C51 C 0.5723(8) 0.9090(5) 0.6234(3) 0.070(2) Uani 1 1 d . . . H51C H 0.6434 0.9043 0.6135 0.084 Uiso 1 1 calc R . . H51D H 0.5510 0.9506 0.6180 0.084 Uiso 1 1 calc R . . C52 C 0.5007(8) 0.8662(4) 0.5974(3) 0.071(2) Uani 1 1 d . . . H52C H 0.5124 0.8712 0.5651 0.086 Uiso 1 1 calc R . . H52D H 0.5195 0.8249 0.6054 0.086 Uiso 1 1 calc R . . C53 C 0.3047(7) 0.8723(3) 0.8256(3) 0.0564(19) Uani 1 1 d . . . H53C H 0.2873 0.8802 0.8569 0.068 Uiso 1 1 calc R . . H53D H 0.3668 0.8472 0.8257 0.068 Uiso 1 1 calc R . . C54 C 0.2170(7) 0.8384(4) 0.8030(3) 0.062(2) Uani 1 1 d . . . H54C H 0.2065 0.8001 0.8184 0.075 Uiso 1 1 calc R . . H54D H 0.1531 0.8618 0.8046 0.075 Uiso 1 1 calc R . . C55 C 0.1732(7) 0.7856(4) 0.7337(3) 0.065(2) Uani 1 1 d . . . H55C H 0.1129 0.8069 0.7211 0.078 Uiso 1 1 calc R . . H55D H 0.1489 0.7559 0.7553 0.078 Uiso 1 1 calc R . . C56 C 0.2291(7) 0.7551(4) 0.6970(3) 0.061(2) Uani 1 1 d . . . H56C H 0.2890 0.7335 0.7096 0.073 Uiso 1 1 calc R . . H56D H 0.1834 0.7260 0.6819 0.073 Uiso 1 1 calc R . . C57 C 0.3257(7) 0.7735(4) 0.6301(3) 0.062(2) Uani 1 1 d . . . H57C H 0.2942 0.7362 0.6191 0.075 Uiso 1 1 calc R . . H57D H 0.3951 0.7646 0.6420 0.075 Uiso 1 1 calc R . . C58 C 0.3311(8) 0.8197(4) 0.5918(3) 0.067(2) Uani 1 1 d . . . H58C H 0.3648 0.8014 0.5660 0.080 Uiso 1 1 calc R . . H58D H 0.2608 0.8309 0.5822 0.080 Uiso 1 1 calc R . . C59 C 0.2430(7) 0.9741(4) 0.8095(3) 0.060(2) Uani 1 1 d . . . H59C H 0.2572 0.9969 0.8371 0.072 Uiso 1 1 calc R . . H59D H 0.1782 0.9522 0.8133 0.072 Uiso 1 1 calc R . . C60 C 0.2306(7) 1.0178(4) 0.7699(3) 0.060(2) Uani 1 1 d . . . H60C H 0.1763 1.0470 0.7761 0.072 Uiso 1 1 calc R . . H60D H 0.2953 1.0395 0.7655 0.072 Uiso 1 1 calc R . . C61 C 0.1611(7) 1.0221(4) 0.6955(3) 0.064(2) Uani 1 1 d . . . H61C H 0.2090 1.0551 0.6897 0.077 Uiso 1 1 calc R . . H61D H 0.0958 1.0394 0.7053 0.077 Uiso 1 1 calc R . . C62 C 0.1429(7) 0.9863(4) 0.6528(3) 0.069(2) Uani 1 1 d . . . H62C H 0.0960 0.9528 0.6584 0.083 Uiso 1 1 calc R . . H62D H 0.1119 1.0118 0.6293 0.083 Uiso 1 1 calc R . . C63 C 0.2416(8) 0.9466(4) 0.5920(3) 0.075(3) Uani 1 1 d . . . H63C H 0.2180 0.9803 0.5733 0.090 Uiso 1 1 calc R . . H63D H 0.1938 0.9131 0.5871 0.090 Uiso 1 1 calc R . . C64 C 0.3507(8) 0.9281(4) 0.5787(3) 0.069(2) Uani 1 1 d . . . H64A H 0.3495 0.9176 0.5470 0.082 Uiso 1 1 calc R . . H64B H 0.3972 0.9615 0.5838 0.082 Uiso 1 1 calc R . . O17 O 0.2710(6) 0.5989(3) 0.9640(3) 0.091(2) Uani 1 1 d U . . H17 H 0.2112 0.6240 0.9659 0.109 Uiso 1 1 d R . . O18 O 0.930(2) 0.5677(13) 0.9951(10) 0.101(8) Uani 0.50 1 d PU . . O19 O 0.1334(15) 0.4176(9) 0.9009(7) 0.116(6) Uani 1 1 d U . . O20 O 0.8067(13) 0.6332(8) 0.9231(6) 0.104(5) Uani 0.50 1 d PU . . H20 H 0.7894 0.6062 0.9401 0.125 Uiso 0.50 1 d PR . . O21 O 0.0550(10) 0.4586(6) 0.7249(5) 0.073(3) Uani 0.50 1 d PU . . H21 H 0.0319 0.4478 0.6965 0.088 Uiso 0.50 1 d PR . . O22 O 0.1117(8) 0.6402(4) 1.0146(3) 0.114(3) Uani 0.50 1 d PU . . C65 C 0.2276(16) 0.5405(9) 0.9491(7) 0.078(5) Uani 1 1 d U . . H65A H 0.1769 0.5272 0.9704 0.116 Uiso 1 1 calc R . . H65B H 0.2826 0.5112 0.9476 0.116 Uiso 1 1 calc R . . H65C H 0.1948 0.5450 0.9197 0.116 Uiso 1 1 calc R . . C66 C 0.992(2) 0.5482(14) 1.0215(10) 0.077(9) Uani 0.50 1 d PU . . H66A H 1.0608 0.5546 1.0103 0.116 Uiso 0.50 1 calc PR . . H66B H 0.9803 0.5056 1.0254 0.116 Uiso 0.50 1 calc PR . . H66C H 0.9852 0.5684 1.0501 0.116 Uiso 0.50 1 calc PR . . C67 C 0.086(2) 0.3656(10) 0.8864(9) 0.099(7) Uani 1 1 d U . . H67A H 0.1291 0.3315 0.8943 0.148 Uiso 1 1 calc R . . H67B H 0.0757 0.3671 0.8540 0.148 Uiso 1 1 calc R . . H67C H 0.0197 0.3617 0.9006 0.148 Uiso 1 1 calc R . . C68 C 0.7957(16) 0.6888(9) 0.9428(7) 0.079(5) Uani 0.50 1 d PU . . H68A H 0.7566 0.6848 0.9701 0.119 Uiso 0.50 1 calc PR . . H68B H 0.7594 0.7154 0.9221 0.119 Uiso 0.50 1 calc PR . . H68C H 0.8633 0.7052 0.9502 0.119 Uiso 0.50 1 calc PR . . C69 C 0.064(2) 0.4155(12) 0.7520(9) 0.111(8) Uani 0.50 1 d PU . . H69A H 0.1224 0.3910 0.7439 0.167 Uiso 0.50 1 calc PR . . H69B H 0.0015 0.3915 0.7506 0.167 Uiso 0.50 1 calc PR . . H69C H 0.0744 0.4309 0.7822 0.167 Uiso 0.50 1 calc PR . . C70 C 0.0893(9) 0.7015(5) 1.0117(4) 0.092(3) Uani 0.50 1 d PU . . H70A H 0.0687 0.7161 1.0408 0.138 Uiso 0.50 1 calc PR . . H70B H 0.0336 0.7078 0.9899 0.138 Uiso 0.50 1 calc PR . . H70C H 0.1502 0.7230 1.0023 0.138 Uiso 0.50 1 calc PR . . O23 O 0.1122(9) 0.5006(6) 0.8347(4) 0.155(4) Uani 1 1 d U . . O24 O -0.0859(9) 0.8009(6) 0.7963(4) 0.156(4) Uani 1 1 d U . . O25 O 0.6075(5) 0.5843(3) 0.8997(2) 0.0785(18) Uani 1 1 d U . . O26 O 0.4939(13) 0.5551(7) 0.9692(5) 0.093(4) 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 0.05242(18) 0.04235(16) 0.04817(16) -0.00151(11) -0.00028(11) -0.00002(13) O1 0.054(3) 0.048(3) 0.051(3) 0.000(2) -0.004(2) -0.004(2) O2 0.062(3) 0.056(3) 0.052(3) -0.008(2) 0.005(2) -0.014(3) O3 0.058(3) 0.049(3) 0.048(3) -0.007(2) 0.004(2) 0.001(3) O4 0.055(3) 0.047(3) 0.057(3) -0.002(2) -0.003(2) 0.000(3) O5 0.052(3) 0.049(3) 0.050(3) -0.007(2) -0.001(2) 0.006(2) O6 0.051(3) 0.047(3) 0.053(3) -0.004(2) 0.002(2) 0.008(2) O7 0.067(4) 0.039(3) 0.055(3) 0.004(2) -0.007(2) 0.004(3) O8 0.056(3) 0.045(3) 0.051(3) 0.002(2) 0.002(2) 0.002(2) C1 0.053(4) 0.047(4) 0.050(4) -0.004(3) -0.004(3) -0.002(4) C2 0.049(4) 0.044(4) 0.057(4) 0.002(3) 0.002(3) -0.010(4) C3 0.051(4) 0.047(4) 0.050(4) 0.000(3) 0.002(3) -0.012(4) C4 0.052(5) 0.056(5) 0.055(5) -0.002(3) -0.002(3) -0.004(4) C5 0.054(5) 0.053(4) 0.054(4) -0.004(3) 0.003(3) -0.009(4) C6 0.060(5) 0.047(4) 0.055(4) -0.008(3) 0.003(4) 0.002(4) C7 0.056(5) 0.071(6) 0.060(5) 0.000(4) -0.007(4) 0.000(4) C8 0.067(6) 0.148(11) 0.059(6) 0.004(6) -0.003(5) 0.013(7) C9 0.093(8) 0.092(7) 0.059(5) -0.001(5) -0.008(5) -0.028(6) C10 0.061(5) 0.070(6) 0.065(5) 0.002(4) 0.002(4) 0.003(5) C11 0.052(4) 0.048(4) 0.053(4) -0.004(3) 0.004(3) -0.010(4) C12 0.052(5) 0.061(5) 0.058(5) -0.009(4) 0.003(4) -0.005(4) C13 0.055(5) 0.060(5) 0.049(4) -0.006(3) 0.005(3) -0.006(4) C14 0.055(5) 0.047(4) 0.048(4) 0.000(3) 0.007(3) -0.006(4) C15 0.051(4) 0.053(4) 0.053(4) -0.003(3) 0.003(3) 0.000(4) C16 0.048(4) 0.055(4) 0.048(4) -0.001(3) 0.002(3) -0.006(4) C17 0.051(4) 0.054(4) 0.047(4) -0.001(3) 0.003(3) 0.001(4) C18 0.050(4) 0.061(5) 0.049(4) 0.001(3) 0.001(3) -0.003(4) C19 0.055(5) 0.051(4) 0.053(4) -0.001(3) -0.002(3) -0.004(4) C20 0.073(6) 0.060(5) 0.090(7) -0.005(5) -0.017(5) 0.007(5) C21 0.107(8) 0.063(5) 0.062(5) -0.007(4) 0.015(5) 0.022(6) C22 0.066(5) 0.051(5) 0.064(5) -0.010(4) 0.004(4) 0.002(4) C23 0.060(5) 0.054(4) 0.049(4) -0.005(3) -0.004(3) -0.003(4) C24 0.051(4) 0.045(4) 0.048(4) -0.004(3) -0.005(3) 0.003(3) C25 0.052(4) 0.044(4) 0.050(4) 0.000(3) -0.002(3) 0.001(4) C26 0.056(5) 0.051(4) 0.048(4) -0.005(3) -0.006(3) 0.002(4) C27 0.049(4) 0.052(4) 0.051(4) -0.001(3) 0.001(3) 0.002(4) C28 0.054(4) 0.046(4) 0.049(4) -0.003(3) -0.006(3) 0.004(4) C29 0.051(4) 0.053(4) 0.049(4) -0.002(3) -0.001(3) 0.002(4) C30 0.047(4) 0.051(4) 0.054(4) -0.003(3) -0.005(3) -0.001(4) C31 0.068(5) 0.053(5) 0.057(5) -0.007(4) -0.004(4) -0.004(4) C32 0.064(5) 0.051(4) 0.059(5) -0.006(3) 0.002(4) -0.001(4) C33 0.055(5) 0.061(5) 0.055(5) -0.002(4) -0.002(4) -0.006(4) C34 0.056(5) 0.056(5) 0.055(5) -0.010(3) -0.003(4) 0.002(4) C35 0.054(5) 0.049(4) 0.055(4) -0.008(3) 0.000(3) 0.002(4) C36 0.053(4) 0.049(4) 0.050(4) -0.004(3) 0.001(3) 0.001(4) C37 0.056(5) 0.044(4) 0.049(4) -0.006(3) -0.001(3) 0.009(4) C38 0.050(4) 0.039(4) 0.053(4) -0.002(3) -0.002(3) 0.003(3) C39 0.052(4) 0.048(4) 0.055(4) -0.004(3) -0.006(3) 0.004(4) C40 0.058(5) 0.041(4) 0.056(4) -0.002(3) -0.004(3) 0.007(4) C41 0.057(5) 0.049(4) 0.054(4) -0.006(3) 0.001(3) -0.002(4) C42 0.062(5) 0.050(4) 0.047(4) -0.002(3) -0.006(3) 0.006(4) C43 0.072(6) 0.068(5) 0.055(5) 0.007(4) 0.001(4) -0.007(5) C44 0.069(6) 0.064(5) 0.057(5) -0.001(4) 0.003(4) 0.017(4) C45 0.068(5) 0.055(5) 0.053(5) -0.004(3) 0.004(4) -0.004(4) C46 0.064(5) 0.045(4) 0.052(4) -0.005(3) -0.002(4) 0.000(4) Ba 0.0528(3) 0.0448(2) 0.0528(3) 0.00089(18) -0.00012(19) -0.0017(2) N1 0.061(4) 0.048(4) 0.054(4) 0.006(3) 0.005(3) 0.001(3) N2 0.068(5) 0.053(4) 0.057(4) 0.002(3) 0.003(3) 0.001(3) O9 0.064(4) 0.057(3) 0.055(3) 0.004(2) -0.004(3) 0.000(3) O10 0.060(3) 0.060(3) 0.061(3) -0.001(3) 0.006(3) -0.015(3) O11 0.062(3) 0.044(3) 0.061(3) 0.001(2) 0.003(3) -0.008(3) O12 0.062(3) 0.046(3) 0.066(3) 0.001(2) 0.004(3) -0.004(3) O13 0.070(4) 0.050(3) 0.056(3) 0.002(2) -0.003(3) 0.005(3) O14 0.063(4) 0.063(3) 0.055(3) -0.001(3) -0.002(3) 0.006(3) O15 0.059(3) 0.048(3) 0.071(4) 0.005(2) 0.005(3) 0.003(3) O16 0.064(4) 0.051(3) 0.061(3) -0.001(2) -0.005(3) -0.009(3) C47 0.068(6) 0.058(5) 0.056(5) 0.000(4) -0.005(4) -0.009(4) C48 0.062(5) 0.069(5) 0.058(5) 0.006(4) -0.006(4) -0.006(4) C49 0.052(5) 0.061(5) 0.074(6) -0.002(4) -0.002(4) -0.002(4) C50 0.047(5) 0.059(5) 0.081(6) -0.001(4) 0.007(4) -0.009(4) C51 0.070(6) 0.075(6) 0.066(6) -0.007(4) 0.013(4) -0.008(5) C52 0.085(7) 0.065(6) 0.064(5) -0.010(4) 0.015(5) -0.008(5) C53 0.070(5) 0.044(4) 0.055(5) 0.003(3) 0.008(4) 0.002(4) C54 0.062(5) 0.057(5) 0.067(5) 0.003(4) 0.015(4) -0.003(4) C55 0.058(5) 0.061(5) 0.075(6) 0.008(4) -0.004(4) -0.010(4) C56 0.066(5) 0.046(4) 0.070(5) -0.002(4) -0.009(4) -0.011(4) C57 0.067(6) 0.057(5) 0.062(5) -0.006(4) -0.003(4) -0.004(4) C58 0.079(6) 0.056(5) 0.065(5) -0.012(4) -0.004(4) -0.001(5) C59 0.076(6) 0.045(4) 0.059(5) 0.000(3) 0.010(4) 0.002(4) C60 0.068(5) 0.048(4) 0.064(5) -0.001(4) 0.008(4) -0.001(4) C61 0.066(6) 0.063(5) 0.062(5) 0.000(4) -0.002(4) 0.007(4) C62 0.069(6) 0.063(5) 0.075(6) 0.004(4) -0.012(5) 0.012(5) C63 0.095(7) 0.067(6) 0.063(6) -0.003(4) -0.014(5) 0.016(5) C64 0.089(7) 0.062(5) 0.055(5) 0.005(4) 0.001(4) 0.002(5) O17 0.095(3) 0.089(3) 0.088(3) 0.005(2) 0.004(2) 0.001(3) O18 0.100(8) 0.100(8) 0.103(8) 0.002(3) 0.002(3) -0.001(3) O19 0.116(6) 0.114(6) 0.116(6) 0.001(3) 0.003(3) -0.003(3) O20 0.103(6) 0.103(6) 0.107(6) -0.004(3) -0.001(3) 0.001(3) O21 0.073(4) 0.069(4) 0.078(4) -0.001(3) 0.009(3) 0.000(3) O22 0.116(4) 0.113(4) 0.113(4) 0.008(3) 0.007(3) 0.003(3) C65 0.078(6) 0.078(6) 0.077(6) 0.001(3) 0.005(3) -0.001(3) C66 0.077(9) 0.077(9) 0.078(9) 0.000(3) 0.004(3) -0.002(3) C67 0.100(8) 0.098(8) 0.099(8) -0.001(3) 0.003(3) -0.001(3) C68 0.078(6) 0.080(6) 0.079(6) 0.000(3) -0.002(3) 0.000(3) C69 0.111(9) 0.112(9) 0.110(9) -0.002(3) 0.005(3) 0.003(3) C70 0.094(4) 0.093(4) 0.090(4) -0.001(3) 0.004(3) 0.002(3) O23 0.149(5) 0.152(5) 0.163(5) 0.013(3) 0.007(3) 0.001(3) O24 0.153(5) 0.157(5) 0.160(5) -0.001(3) 0.007(3) 0.002(3) O25 0.079(3) 0.072(3) 0.084(3) -0.001(2) -0.009(2) 0.002(2) O26 0.095(5) 0.092(5) 0.093(5) 0.002(3) 0.000(3) 0.005(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 O7 1.799(5) . ? U O8 1.806(5) . ? U O6 2.264(5) . ? U O1 2.274(5) . ? U O4 2.274(5) . ? U O3 2.280(5) . ? U O2 3.771(6) . ? U O5 3.852(5) . ? O1 C2 1.346(9) . ? O1 O23 2.693(13) . ? O1 O2 3.082(8) . ? O1 O6 3.089(7) . ? O1 O3 3.358(7) . ? O2 C11 1.440(9) . ? O2 C12 1.442(9) . ? O2 O3 3.067(8) . ? O3 C14 1.329(9) . ? O3 O4 3.102(8) . ? O4 C25 1.356(9) . ? O4 O5 3.030(7) . ? O4 O6 3.288(7) . ? O5 C35 1.418(9) . ? O5 C34 1.434(9) . ? O5 O6 3.089(7) . ? O6 C37 1.340(9) . ? C1 C6 1.385(11) . ? C1 C2 1.417(11) . ? C1 C46 1.497(11) . ? C2 C3 1.419(11) . ? C3 C4 1.388(11) . ? C3 C11 1.504(10) . ? C4 C5 1.396(11) . ? C5 C6 1.386(11) . ? C5 C7 1.530(11) . ? C7 C10 1.528(12) . ? C7 C8 1.531(13) . ? C7 C9 1.545(13) . ? C12 C13 1.497(11) . ? C13 C18 1.400(11) . ? C13 C14 1.413(11) . ? C14 C15 1.402(11) . ? C15 C16 1.382(11) . ? C15 C23 1.527(11) . ? C16 C17 1.393(11) . ? C17 C18 1.384(11) . ? C17 C19 1.539(11) . ? C19 C20 1.514(12) . ? C19 C22 1.534(11) . ? C19 C21 1.550(12) . ? C23 C24 1.503(11) . ? C24 C29 1.407(11) . ? C24 C25 1.414(10) . ? C25 C26 1.399(11) . ? C26 C27 1.397(11) . ? C26 C34 1.514(10) . ? C27 C28 1.397(10) . ? C28 C29 1.406(11) . ? C28 C30 1.540(11) . ? C30 C32 1.514(11) . ? C30 C33 1.557(11) . ? C30 C31 1.560(11) . ? C35 C36 1.510(11) . ? C36 C41 1.378(11) . ? C36 C37 1.401(11) . ? C37 C38 1.425(10) . ? C38 C39 1.387(11) . ? C38 C46 1.524(11) . ? C39 C40 1.399(11) . ? C40 C41 1.403(11) . ? C40 C42 1.545(11) . ? C42 C43 1.524(12) . ? C42 C45 1.548(11) . ? C42 C44 1.556(11) . ? Ba O16 2.722(5) . ? Ba O11 2.749(5) . ? Ba O9 2.788(6) . ? Ba O10 2.796(6) . ? Ba O14 2.831(6) . ? Ba O15 2.832(5) . ? Ba O12 2.851(5) . ? Ba O13 2.862(6) . ? Ba N1 2.992(6) . ? Ba N2 3.014(7) . ? N1 C59 1.467(10) . ? N1 C53 1.488(10) . ? N1 C47 1.489(11) . ? N1 N2 6.003(10) . ? N2 C52 1.471(12) . ? N2 C58 1.477(11) . ? N2 C64 1.494(11) . ? O9 C48 1.429(10) . ? O9 C49 1.432(10) . ? O10 C51 1.425(11) . ? O10 C50 1.430(10) . ? O11 C54 1.438(10) . ? O11 C55 1.440(10) . ? O12 C57 1.436(10) . ? O12 C56 1.451(10) . ? O13 C60 1.420(10) . ? O13 C61 1.429(10) . ? O14 C63 1.428(10) . ? O14 C62 1.442(11) . ? C47 C48 1.508(12) . ? C49 C50 1.480(12) . ? C51 C52 1.514(13) . ? C53 C54 1.493(12) . ? C55 C56 1.474(12) . ? C57 C58 1.524(12) . ? C59 C60 1.517(11) . ? C61 C62 1.497(12) . ? C63 C64 1.518(14) . ? O17 C65 1.467(19) . ? O17 O26 3.019(18) . ? O18 C66 1.18(4) . ? O19 C67 1.36(3) . ? O19 O23 2.69(2) . ? O20 C68 1.37(2) . ? O20 O25 2.844(18) . ? O21 C69 1.24(3) . ? O22 C70 1.386(13) . ? O25 O26 2.619(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 U O8 179.2(3) . . ? O7 U O6 87.8(2) . . ? O8 U O6 91.7(2) . . ? O7 U O1 87.6(2) . . ? O8 U O1 93.0(2) . . ? O6 U O1 85.82(19) . . ? O7 U O4 87.7(2) . . ? O8 U O4 91.8(2) . . ? O6 U O4 92.86(19) . . ? O1 U O4 175.11(18) . . ? O7 U O3 87.1(2) . . ? O8 U O3 93.4(2) . . ? O6 U O3 174.83(18) . . ? O1 U O3 95.02(19) . . ? O4 U O3 85.87(19) . . ? O7 U O2 117.0(2) . . ? O8 U O2 63.77(19) . . ? O6 U O2 129.39(15) . . ? O1 U O2 54.79(15) . . ? O4 U O2 128.85(15) . . ? O3 U O2 54.40(15) . . ? O7 U O5 114.8(2) . . ? O8 U O5 64.40(19) . . ? O6 U O5 53.31(15) . . ? O1 U O5 129.80(15) . . ? O4 U O5 51.81(15) . . ? O3 U O5 128.45(15) . . ? O2 U O5 128.16(11) . . ? C11 O2 C12 110.8(6) . . ? C35 O5 C34 109.2(6) . . ? C6 C1 C2 117.9(8) . . ? C6 C1 C46 122.0(7) . . ? C2 C1 C46 119.8(7) . . ? O1 C2 C1 121.5(7) . . ? O1 C2 C3 119.6(7) . . ? C1 C2 C3 118.9(7) . . ? C4 C3 C2 119.9(7) . . ? C4 C3 C11 121.0(8) . . ? C2 C3 C11 119.0(7) . . ? C3 C4 C5 122.2(8) . . ? C6 C5 C4 116.4(8) . . ? C6 C5 C7 120.6(7) . . ? C4 C5 C7 123.0(8) . . ? C1 C6 C5 124.7(8) . . ? C10 C7 C5 110.1(7) . . ? C10 C7 C8 110.1(8) . . ? C5 C7 C8 111.6(8) . . ? C10 C7 C9 108.7(8) . . ? C5 C7 C9 109.0(7) . . ? C8 C7 C9 107.2(8) . . ? O2 C11 C3 109.5(6) . . ? O2 C12 C13 110.7(6) . . ? C18 C13 C14 119.7(7) . . ? C18 C13 C12 121.0(8) . . ? C14 C13 C12 119.2(7) . . ? O3 C14 C15 121.8(7) . . ? O3 C14 C13 120.0(7) . . ? C15 C14 C13 118.1(7) . . ? C16 C15 C14 119.9(7) . . ? C16 C15 C23 119.7(7) . . ? C14 C15 C23 120.3(7) . . ? C15 C16 C17 123.3(7) . . ? C18 C17 C16 116.3(7) . . ? C18 C17 C19 122.6(7) . . ? C16 C17 C19 120.9(7) . . ? C17 C18 C13 122.7(8) . . ? C20 C19 C22 107.4(7) . . ? C20 C19 C17 113.2(7) . . ? C22 C19 C17 110.6(7) . . ? C20 C19 C21 108.7(8) . . ? C22 C19 C21 108.2(7) . . ? C17 C19 C21 108.6(6) . . ? C24 C23 C15 115.6(7) . . ? C29 C24 C25 117.6(7) . . ? C29 C24 C23 120.7(7) . . ? C25 C24 C23 121.4(7) . . ? O4 C25 C26 119.9(7) . . ? O4 C25 C24 119.9(7) . . ? C26 C25 C24 119.9(7) . . ? C27 C26 C25 120.7(7) . . ? C27 C26 C34 119.0(7) . . ? C25 C26 C34 120.0(7) . . ? C28 C27 C26 121.1(8) . . ? C27 C28 C29 117.3(7) . . ? C27 C28 C30 122.5(7) . . ? C29 C28 C30 119.7(7) . . ? C28 C29 C24 123.3(7) . . ? C32 C30 C28 108.9(6) . . ? C32 C30 C33 108.4(7) . . ? C28 C30 C33 111.1(6) . . ? C32 C30 C31 109.3(7) . . ? C28 C30 C31 110.5(6) . . ? C33 C30 C31 108.6(7) . . ? O5 C34 C26 112.0(6) . . ? O5 C35 C36 111.5(6) . . ? C41 C36 C37 120.1(7) . . ? C41 C36 C35 120.3(7) . . ? C37 C36 C35 119.3(7) . . ? O6 C37 C36 120.5(7) . . ? O6 C37 C38 120.9(7) . . ? C36 C37 C38 118.4(7) . . ? C39 C38 C37 119.5(7) . . ? C39 C38 C46 121.1(7) . . ? C37 C38 C46 119.3(7) . . ? C38 C39 C40 122.7(7) . . ? C39 C40 C41 116.3(7) . . ? C39 C40 C42 122.6(7) . . ? C41 C40 C42 120.7(8) . . ? C36 C41 C40 123.0(8) . . ? C43 C42 C40 112.3(7) . . ? C43 C42 C45 107.8(7) . . ? C40 C42 C45 111.0(6) . . ? C43 C42 C44 108.5(7) . . ? C40 C42 C44 108.2(6) . . ? C45 C42 C44 108.9(7) . . ? C1 C46 C38 117.0(6) . . ? O16 Ba O11 146.65(17) . . ? O16 Ba O9 70.34(16) . . ? O11 Ba O9 106.53(16) . . ? O16 Ba O10 73.56(17) . . ? O11 Ba O10 135.39(17) . . ? O9 Ba O10 60.59(17) . . ? O16 Ba O14 63.74(17) . . ? O11 Ba O14 110.48(17) . . ? O9 Ba O14 134.05(16) . . ? O10 Ba O14 106.10(17) . . ? O16 Ba O15 137.57(17) . . ? O11 Ba O15 61.37(16) . . ? O9 Ba O15 69.92(16) . . ? O10 Ba O15 74.51(17) . . ? O14 Ba O15 153.77(17) . . ? O16 Ba O12 141.38(16) . . ? O11 Ba O12 59.69(16) . . ? O9 Ba O12 142.32(16) . . ? O10 Ba O12 102.82(16) . . ? O14 Ba O12 81.41(16) . . ? O15 Ba O12 73.07(16) . . ? O16 Ba O13 70.47(17) . . ? O11 Ba O13 78.76(16) . . ? O9 Ba O13 104.52(16) . . ? O10 Ba O13 143.98(16) . . ? O14 Ba O13 58.72(16) . . ? O15 Ba O13 134.46(16) . . ? O12 Ba O13 106.23(16) . . ? C59 N1 C53 110.4(6) . . ? C59 N1 C47 107.9(7) . . ? C53 N1 C47 109.9(6) . . ? C52 N2 C58 109.5(7) . . ? C52 N2 C64 108.9(7) . . ? C58 N2 C64 110.2(7) . . ? C48 O9 C49 111.3(6) . . ? C51 O10 C50 112.3(6) . . ? C54 O11 C55 113.5(6) . . ? C57 O12 C56 111.6(6) . . ? C60 O13 C61 111.2(6) . . ? C63 O14 C62 112.4(7) . . ? N1 C47 C48 112.9(7) . . ? O9 C48 C47 109.1(7) . . ? O9 C49 C50 107.8(7) . . ? O10 C50 C49 109.2(7) . . ? O10 C51 C52 108.1(7) . . ? N2 C52 C51 114.7(7) . . ? N1 C53 C54 112.8(7) . . ? O11 C54 C53 108.8(7) . . ? O11 C55 C56 109.4(7) . . ? O12 C56 C55 109.1(7) . . ? O12 C57 C58 106.7(7) . . ? N2 C58 C57 112.3(7) . . ? N1 C59 C60 112.0(7) . . ? O13 C60 C59 108.4(6) . . ? O13 C61 C62 110.0(7) . . ? O14 C62 C61 107.5(7) . . ? O14 C63 C64 109.4(8) . . ? N2 C64 C63 111.7(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O15 H15A O5 0.98 1.95 2.823(7) 146.0 . O15 H15B O8 0.91 2.21 3.002(7) 145.7 . O16 H16A O6 0.89 1.93 2.764(7) 155.4 2_656 O16 H16B O14 0.92 2.70 2.934(8) 95.8 . O16 H16B O25 0.92 2.04 2.946(9) 167.7 2_656 O17 H17 O22 0.95 1.97 2.713(13) 133.3 . O20 H20 O18 0.81 2.54 2.99(3) 116.0 . #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 606963' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H194 Ba N4 O29 U2' _chemical_formula_weight 2794.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.8808(13) _cell_length_b 19.0624(19) _cell_length_c 22.4431(19) _cell_angle_alpha 66.304(5) _cell_angle_beta 73.525(6) _cell_angle_gamma 66.252(5) _cell_volume 6698.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 43147 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method ? _exptl_crystal_F_000 2852 _exptl_absorpt_coefficient_mu 2.771 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 30 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' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 43147 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.1450 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.68 _reflns_number_total 22608 _reflns_number_gt 14956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (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)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Due to low crystal quality, the structure determination is not quite satisfactory, but it gives unambiguously the main features of the complex. All non-hydrogen atoms were refined with anisotropic displacement parameters, with some restraints for some badly behaving atoms. The H atoms bound to O atoms were not found, nor introduced. All the other H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (NH, CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Some voids in the lattice 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^)+(0.0868P)^2^+135.5044P] 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 22608 _refine_ls_number_parameters 1477 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1451 _refine_ls_R_factor_gt 0.0982 _refine_ls_wR_factor_ref 0.2515 _refine_ls_wR_factor_gt 0.2242 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 1.738 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.340 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 0.39847(3) 0.45057(3) 0.36529(3) 0.02798(16) Uani 1 1 d . . . U2 U 1.12303(3) 0.19256(3) 0.13760(3) 0.02805(16) Uani 1 1 d . . . Ba Ba 0.77321(5) 0.39105(6) 0.25382(4) 0.0306(2) Uani 1 1 d . . . O1A O 0.3178(6) 0.4933(6) 0.4493(5) 0.031(2) Uani 1 1 d . . . O2A O 0.1824(7) 0.5763(6) 0.3601(5) 0.041(3) Uani 1 1 d U . . O3A O 0.3506(6) 0.5673(6) 0.2840(5) 0.031(2) Uani 1 1 d . . . O4A O 0.4890(5) 0.4083(6) 0.2828(5) 0.028(2) Uani 1 1 d . . . O5A O 0.4854(6) 0.2331(6) 0.3586(5) 0.033(2) Uani 1 1 d . . . O6A O 0.4522(6) 0.3355(6) 0.4471(5) 0.030(2) Uani 1 1 d . . . O7A O 0.4631(6) 0.4950(6) 0.3705(5) 0.038(3) Uani 1 1 d . . . O8A O 0.3336(5) 0.4061(6) 0.3598(5) 0.031(2) Uani 1 1 d . . . O1B O 1.2156(6) 0.2340(7) 0.0566(5) 0.037(3) Uani 1 1 d . . . O2B O 1.3449(5) 0.0927(6) 0.1381(5) 0.024(2) Uani 1 1 d U . . O3B O 1.1887(6) 0.1658(7) 0.2193(5) 0.035(2) Uani 1 1 d . . . O4B O 1.0258(6) 0.1637(6) 0.2204(5) 0.029(2) Uani 1 1 d . . . O5B O 0.9929(6) 0.0901(6) 0.1370(5) 0.034(2) Uani 1 1 d . . . O6B O 1.0536(5) 0.2327(6) 0.0557(5) 0.029(2) Uani 1 1 d . . . O7B O 1.0807(7) 0.2936(7) 0.1398(6) 0.043(3) Uani 1 1 d . . . O8B O 1.1647(6) 0.0896(6) 0.1357(5) 0.034(2) Uani 1 1 d . . . C1A C 0.2648(10) 0.4076(9) 0.5508(7) 0.034(4) Uani 1 1 d . . . C1B C 1.2430(8) 0.2238(9) -0.0511(7) 0.028(3) Uani 1 1 d . . . C2B C 1.2675(8) 0.2063(9) 0.0072(7) 0.029(3) Uani 1 1 d . . . C2A C 0.2560(9) 0.4742(9) 0.4928(7) 0.032(3) Uani 1 1 d . . . C3B C 1.3450(9) 0.1642(10) 0.0159(7) 0.036(4) Uani 1 1 d . . . C3A C 0.1787(9) 0.5277(9) 0.4810(7) 0.031(3) Uani 1 1 d . . . C4A C 0.1157(9) 0.5126(10) 0.5252(7) 0.037(4) Uani 1 1 d . . . H4A H 0.0658 0.5476 0.5167 0.044 Uiso 1 1 calc R . . C4B C 1.3987(9) 0.1381(10) -0.0343(8) 0.041(4) Uani 1 1 d . . . H4B H 1.4506 0.1093 -0.0281 0.049 Uiso 1 1 calc R . . C5A C 0.1243(10) 0.4444(12) 0.5842(9) 0.046(4) Uani 1 1 d . . . C5B C 1.3756(9) 0.1546(10) -0.0946(8) 0.037(4) Uani 1 1 d . . . C6B C 1.2981(9) 0.1978(10) -0.1004(7) 0.037(4) Uani 1 1 d . . . H6B H 1.2815 0.2103 -0.1398 0.044 Uiso 1 1 calc R . . C6A C 0.2002(10) 0.3946(10) 0.5944(8) 0.042(4) Uani 1 1 d . . . H6A H 0.2076 0.3501 0.6327 0.050 Uiso 1 1 calc R . . C7B C 1.4345(10) 0.1270(12) -0.1509(9) 0.048(4) Uani 1 1 d . . . C7A C 0.0532(12) 0.4266(12) 0.6342(9) 0.053(5) Uani 1 1 d . . . C8B C 1.4160(19) 0.060(2) -0.1614(16) 0.113(10) Uani 1 1 d U . . H8B1 H 1.4002 0.0246 -0.1195 0.169 Uiso 1 1 calc R . . H8B2 H 1.4620 0.0291 -0.1834 0.169 Uiso 1 1 calc R . . H8B3 H 1.3746 0.0851 -0.1877 0.169 Uiso 1 1 calc R . . C8A C 0.0675(13) 0.4089(17) 0.7056(10) 0.075(7) Uani 1 1 d . . . H8A1 H 0.1226 0.3860 0.7078 0.112 Uiso 1 1 calc R . . H8A2 H 0.0419 0.3714 0.7370 0.112 Uiso 1 1 calc R . . H8A3 H 0.0466 0.4586 0.7155 0.112 Uiso 1 1 calc R . . C9A C 0.0467(12) 0.3489(12) 0.6325(10) 0.056(5) Uani 1 1 d U . . H9A1 H 0.0514 0.3526 0.5877 0.084 Uiso 1 1 calc R . . H9A2 H -0.0031 0.3436 0.6557 0.084 Uiso 1 1 calc R . . H9A3 H 0.0877 0.3024 0.6532 0.084 Uiso 1 1 calc R . . C9B C 1.4273(18) 0.2026(19) -0.2148(14) 0.106(9) Uani 1 1 d U . . H9B1 H 1.3929 0.2040 -0.2399 0.160 Uiso 1 1 calc R . . H9B2 H 1.4780 0.1992 -0.2406 0.160 Uiso 1 1 calc R . . H9B3 H 1.4065 0.2511 -0.2030 0.160 Uiso 1 1 calc R . . C10B C 1.5187(16) 0.0905(18) -0.1404(14) 0.097(9) Uani 1 1 d U . . H10A H 1.5488 0.0620 -0.1711 0.146 Uiso 1 1 calc R . . H10B H 1.5227 0.0533 -0.0963 0.146 Uiso 1 1 calc R . . H10C H 1.5383 0.1327 -0.1470 0.146 Uiso 1 1 calc R . . C10A C -0.0253(13) 0.4972(14) 0.6193(12) 0.074(7) Uani 1 1 d . . . H10D H -0.0247 0.5436 0.6262 0.112 Uiso 1 1 calc R . . H10E H -0.0681 0.4803 0.6481 0.112 Uiso 1 1 calc R . . H10F H -0.0314 0.5114 0.5745 0.112 Uiso 1 1 calc R . . C11A C 0.1701(9) 0.6001(10) 0.4216(7) 0.038(4) Uani 1 1 d . . . H11A H 0.2083 0.6251 0.4163 0.045 Uiso 1 1 calc R . . H11B H 0.1184 0.6393 0.4262 0.045 Uiso 1 1 calc R . . C11B C 1.3728(10) 0.1488(12) 0.0777(8) 0.047(4) Uani 1 1 d . . . H11C H 1.4295 0.1281 0.0709 0.056 Uiso 1 1 calc R . . H11D H 1.3574 0.2004 0.0845 0.056 Uiso 1 1 calc R . . C12B C 1.3541(10) 0.1004(12) 0.1898(8) 0.052(5) Uani 1 1 d . . . H12A H 1.3372 0.1576 0.1844 0.063 Uiso 1 1 calc R . . H12B H 1.4091 0.0773 0.1944 0.063 Uiso 1 1 calc R . . C12A C 0.1905(10) 0.6450(10) 0.3060(8) 0.042(4) Uani 1 1 d . . . H12C H 0.2237 0.6674 0.3137 0.050 Uiso 1 1 calc R . . H12D H 0.1398 0.6864 0.2991 0.050 Uiso 1 1 calc R . . C13B C 1.3077(9) 0.0586(11) 0.2521(8) 0.037(4) Uani 1 1 d . . . C13A C 0.2256(9) 0.6180(9) 0.2489(8) 0.036(4) Uani 1 1 d . . . C14A C 0.3079(9) 0.5811(9) 0.2382(7) 0.031(3) Uani 1 1 d . . . C14B C 1.2258(8) 0.0956(9) 0.2626(7) 0.029(3) Uani 1 1 d . . . C15B C 1.1832(8) 0.0588(9) 0.3227(7) 0.027(3) Uani 1 1 d . . . C15A C 0.3436(9) 0.5649(9) 0.1793(7) 0.033(4) Uani 1 1 d . . . C16B C 1.2224(9) -0.0122(11) 0.3674(7) 0.037(4) Uani 1 1 d . . . H16B H 1.1942 -0.0353 0.4066 0.044 Uiso 1 1 calc R . . C16A C 0.3000(9) 0.5790(9) 0.1348(8) 0.035(4) Uani 1 1 d . . . H16A H 0.3255 0.5675 0.0961 0.042 Uiso 1 1 calc R . . C17A C 0.2172(10) 0.6105(10) 0.1444(7) 0.036(4) Uani 1 1 d . . . C17B C 1.3036(10) -0.0509(12) 0.3555(9) 0.047(4) Uani 1 1 d . . . C18A C 0.1842(9) 0.6297(10) 0.2003(8) 0.040(4) Uani 1 1 d . . . H18A H 0.1300 0.6523 0.2072 0.048 Uiso 1 1 calc R . . C18B C 1.3438(9) -0.0140(9) 0.2979(7) 0.032(3) Uani 1 1 d . . . H18B H 1.3974 -0.0388 0.2891 0.039 Uiso 1 1 calc R . . C19A C 0.1716(10) 0.6232(12) 0.0937(8) 0.047(5) Uani 1 1 d . . . C19B C 1.3421(11) -0.1319(13) 0.4065(8) 0.052(5) Uani 1 1 d . . . C20B C 1.4304(10) -0.1658(13) 0.3887(10) 0.063(6) Uani 1 1 d . . . H20A H 1.4539 -0.1287 0.3871 0.094 Uiso 1 1 calc R . . H20B H 1.4424 -0.1728 0.3465 0.094 Uiso 1 1 calc R . . H20C H 1.4505 -0.2172 0.4213 0.094 Uiso 1 1 calc R . . C20A C 0.2013(15) 0.5542(16) 0.0674(13) 0.085(7) Uani 1 1 d U . . H20D H 0.1989 0.5053 0.1029 0.127 Uiso 1 1 calc R . . H20E H 0.2545 0.5476 0.0466 0.127 Uiso 1 1 calc R . . H20F H 0.1696 0.5654 0.0359 0.127 Uiso 1 1 calc R . . C21B C 1.3040(12) -0.1940(13) 0.4131(11) 0.070(6) Uani 1 1 d . . . H21A H 1.3295 -0.2180 0.3790 0.104 Uiso 1 1 calc R . . H21B H 1.2495 -0.1666 0.4091 0.104 Uiso 1 1 calc R . . H21C H 1.3096 -0.2356 0.4552 0.104 Uiso 1 1 calc R . . C21A C 0.0846(12) 0.6411(16) 0.1173(10) 0.071(7) Uani 1 1 d . . . H21D H 0.0576 0.6594 0.0806 0.107 Uiso 1 1 calc R . . H21E H 0.0658 0.6824 0.1374 0.107 Uiso 1 1 calc R . . H21F H 0.0751 0.5926 0.1489 0.107 Uiso 1 1 calc R . . C22A C 0.1807(14) 0.6974(16) 0.0314(11) 0.086(8) Uani 1 1 d . . . H22A H 0.2351 0.6888 0.0144 0.130 Uiso 1 1 calc R . . H22B H 0.1586 0.7459 0.0432 0.130 Uiso 1 1 calc R . . H22C H 0.1539 0.7029 -0.0016 0.130 Uiso 1 1 calc R . . C22B C 1.3263(12) -0.1219(14) 0.4732(9) 0.066(6) Uani 1 1 d . . . H22D H 1.3479 -0.1736 0.5050 0.099 Uiso 1 1 calc R . . H22E H 1.2709 -0.1014 0.4862 0.099 Uiso 1 1 calc R . . H22F H 1.3500 -0.0846 0.4707 0.099 Uiso 1 1 calc R . . C23A C 0.4335(8) 0.5312(9) 0.1656(7) 0.031(3) Uani 1 1 d . . . H23A H 0.4509 0.5601 0.1206 0.037 Uiso 1 1 calc R . . H23B H 0.4552 0.5416 0.1944 0.037 Uiso 1 1 calc R . . C23B C 1.0965(9) 0.0985(9) 0.3386(7) 0.030(3) Uani 1 1 d . . . H23C H 1.0822 0.1557 0.3128 0.037 Uiso 1 1 calc R . . H23D H 1.0837 0.0942 0.3847 0.037 Uiso 1 1 calc R . . C24A C 0.4648(9) 0.4423(10) 0.1756(7) 0.033(4) Uani 1 1 d . . . C24B C 1.0493(9) 0.0597(11) 0.3245(8) 0.038(4) Uani 1 1 d . . . C25A C 0.4871(8) 0.3842(10) 0.2356(7) 0.033(3) Uani 1 1 d . . . C25B C 1.0171(8) 0.0928(9) 0.2656(7) 0.029(3) Uani 1 1 d . . . C26A C 0.5174(8) 0.3010(9) 0.2427(7) 0.031(3) Uani 1 1 d . . . C26B C 0.9752(9) 0.0556(10) 0.2556(7) 0.033(3) Uani 1 1 d . . . C27A C 0.5229(9) 0.2747(11) 0.1898(7) 0.035(4) Uani 1 1 d . . . H27A H 0.5415 0.2195 0.1956 0.041 Uiso 1 1 calc R . . C27B C 0.9613(8) -0.0141(10) 0.3024(8) 0.036(4) Uani 1 1 d . . . H27B H 0.9324 -0.0379 0.2941 0.044 Uiso 1 1 calc R . . C28B C 0.9912(9) -0.0484(9) 0.3625(8) 0.033(3) Uani 1 1 d . . . C28A C 0.5007(9) 0.3309(10) 0.1293(8) 0.036(4) Uani 1 1 d . . . C29A C 0.4711(9) 0.4146(9) 0.1229(7) 0.032(3) Uani 1 1 d . . . H29A H 0.4552 0.4527 0.0833 0.038 Uiso 1 1 calc R . . C29B C 1.0321(9) -0.0083(10) 0.3726(7) 0.033(3) Uani 1 1 d . . . H29B H 1.0488 -0.0276 0.4132 0.040 Uiso 1 1 calc R . . C30B C 0.9770(11) -0.1254(11) 0.4168(7) 0.046(4) Uani 1 1 d . . . C30A C 0.5113(10) 0.3030(11) 0.0707(8) 0.042(4) Uani 1 1 d . . . C31A C 0.5311(12) 0.2130(11) 0.0879(10) 0.053(5) Uani 1 1 d . . . H31A H 0.5252 0.2019 0.0517 0.080 Uiso 1 1 calc R . . H31B H 0.4965 0.1938 0.1262 0.080 Uiso 1 1 calc R . . H31C H 0.5841 0.1859 0.0966 0.080 Uiso 1 1 calc R . . C31B C 0.9288(14) -0.1007(13) 0.4776(9) 0.065(6) Uani 1 1 d . . . H31D H 0.9186 -0.1470 0.5123 0.098 Uiso 1 1 calc R . . H31E H 0.8801 -0.0591 0.4663 0.098 Uiso 1 1 calc R . . H31F H 0.9576 -0.0804 0.4922 0.098 Uiso 1 1 calc R . . C32B C 0.9309(13) -0.1594(14) 0.3978(11) 0.066(6) Uani 1 1 d U . . H32A H 0.9570 -0.1709 0.3577 0.099 Uiso 1 1 calc R . . H32B H 0.8796 -0.1206 0.3915 0.099 Uiso 1 1 calc R . . H32C H 0.9265 -0.2085 0.4321 0.099 Uiso 1 1 calc R . . C32A C 0.4359(13) 0.3463(14) 0.0404(11) 0.070(6) Uani 1 1 d . . . H32D H 0.4414 0.3294 0.0040 0.105 Uiso 1 1 calc R . . H32E H 0.4254 0.4039 0.0253 0.105 Uiso 1 1 calc R . . H32F H 0.3934 0.3331 0.0729 0.105 Uiso 1 1 calc R . . C33B C 1.0531(12) -0.1869(12) 0.4352(11) 0.065(6) Uani 1 1 d . . . H33A H 1.0816 -0.1630 0.4462 0.098 Uiso 1 1 calc R . . H33B H 1.0829 -0.2056 0.3988 0.098 Uiso 1 1 calc R . . H33C H 1.0442 -0.2318 0.4724 0.098 Uiso 1 1 calc R . . C33A C 0.5774(13) 0.3297(12) 0.0204(9) 0.063(6) Uani 1 1 d . . . H33D H 0.6233 0.3082 0.0410 0.094 Uiso 1 1 calc R . . H33E H 0.5616 0.3879 0.0042 0.094 Uiso 1 1 calc R . . H33F H 0.5887 0.3099 -0.0155 0.094 Uiso 1 1 calc R . . C34B C 0.9375(8) 0.0935(9) 0.1939(7) 0.030(3) Uani 1 1 d . . . H34A H 0.9024 0.0655 0.1981 0.036 Uiso 1 1 calc R . . H34B H 0.9065 0.1497 0.1893 0.036 Uiso 1 1 calc R . . C34A C 0.5475(8) 0.2405(9) 0.3045(7) 0.031(3) Uani 1 1 d . . . H34C H 0.5756 0.1882 0.2983 0.037 Uiso 1 1 calc R . . H34D H 0.5839 0.2569 0.3147 0.037 Uiso 1 1 calc R . . C35B C 0.9577(10) 0.1419(11) 0.0790(8) 0.039(4) Uani 1 1 d . . . H35A H 0.9262 0.1944 0.0841 0.047 Uiso 1 1 calc R . . H35B H 0.9231 0.1189 0.0741 0.047 Uiso 1 1 calc R . . C35A C 0.5175(8) 0.1915(10) 0.4169(7) 0.034(4) Uani 1 1 d . . . H35C H 0.5568 0.2130 0.4154 0.041 Uiso 1 1 calc R . . H35D H 0.5432 0.1347 0.4206 0.041 Uiso 1 1 calc R . . C36B C 1.0154(8) 0.1533(10) 0.0189(7) 0.031(3) Uani 1 1 d . . . C36A C 0.4591(9) 0.1977(8) 0.4749(7) 0.032(3) Uani 1 1 d . . . C37B C 1.0605(9) 0.2026(9) 0.0091(7) 0.027(3) Uani 1 1 d . . . C37A C 0.4280(8) 0.2727(9) 0.4880(7) 0.027(3) Uani 1 1 d . . . C38B C 1.1113(9) 0.2168(9) -0.0487(7) 0.031(3) Uani 1 1 d . . . C38A C 0.3777(9) 0.2770(9) 0.5465(7) 0.031(3) Uani 1 1 d . . . C39B C 1.1159(9) 0.1869(10) -0.0977(8) 0.035(4) Uani 1 1 d . . . H39B H 1.1489 0.1995 -0.1371 0.042 Uiso 1 1 calc R . . C39A C 0.3539(10) 0.2092(10) 0.5889(7) 0.039(4) Uani 1 1 d . . . H39A H 0.3184 0.2140 0.6266 0.047 Uiso 1 1 calc R . . C40B C 1.0716(10) 0.1377(10) -0.0885(8) 0.040(4) Uani 1 1 d . . . C40A C 0.3814(11) 0.1348(9) 0.5766(8) 0.040(4) Uani 1 1 d . . . C41A C 0.4341(10) 0.1318(11) 0.5206(8) 0.043(4) Uani 1 1 d . . . H41A H 0.4550 0.0831 0.5118 0.052 Uiso 1 1 calc R . . C41B C 1.0238(9) 0.1231(11) -0.0305(8) 0.038(4) Uani 1 1 d . . . H41B H 0.9945 0.0904 -0.0232 0.046 Uiso 1 1 calc R . . C42B C 1.0796(11) 0.1046(12) -0.1429(9) 0.047(5) Uani 1 1 d . . . C42A C 0.3608(13) 0.0597(11) 0.6252(9) 0.056(5) Uani 1 1 d . . . C43B C 1.0943(16) 0.1654(16) -0.2120(13) 0.088(8) Uani 1 1 d U . . H43A H 1.0459 0.2076 -0.2231 0.132 Uiso 1 1 calc R . . H43B H 1.1153 0.1376 -0.2438 0.132 Uiso 1 1 calc R . . H43C H 1.1309 0.1886 -0.2118 0.132 Uiso 1 1 calc R . . C43A C 0.3270(13) 0.0304(13) 0.5879(11) 0.068(6) Uani 1 1 d . . . H43D H 0.3671 0.0116 0.5551 0.101 Uiso 1 1 calc R . . H43E H 0.2846 0.0746 0.5670 0.101 Uiso 1 1 calc R . . H43F H 0.3083 -0.0130 0.6183 0.101 Uiso 1 1 calc R . . C44B C 1.0065(10) 0.0852(12) -0.1383(8) 0.045(4) Uani 1 1 d . . . H44A H 0.9612 0.1326 -0.1391 0.067 Uiso 1 1 calc R . . H44B H 1.0008 0.0422 -0.0979 0.067 Uiso 1 1 calc R . . H44C H 1.0117 0.0685 -0.1748 0.067 Uiso 1 1 calc R . . C44A C 0.2987(14) 0.0783(15) 0.6810(11) 0.074(6) Uani 1 1 d U . . H44D H 0.2850 0.0307 0.7086 0.111 Uiso 1 1 calc R . . H44E H 0.2532 0.1211 0.6637 0.111 Uiso 1 1 calc R . . H44F H 0.3181 0.0952 0.7063 0.111 Uiso 1 1 calc R . . C45A C 0.4317(15) -0.0042(12) 0.6505(10) 0.069(6) Uani 1 1 d . . . H45A H 0.4688 -0.0196 0.6149 0.104 Uiso 1 1 calc R . . H45B H 0.4184 -0.0505 0.6823 0.104 Uiso 1 1 calc R . . H45C H 0.4543 0.0158 0.6710 0.104 Uiso 1 1 calc R . . C45B C 1.1497(13) 0.0261(14) -0.1351(12) 0.073(6) Uani 1 1 d U . . H45D H 1.1543 0.0034 -0.1677 0.109 Uiso 1 1 calc R . . H45E H 1.1423 -0.0119 -0.0921 0.109 Uiso 1 1 calc R . . H45F H 1.1966 0.0378 -0.1406 0.109 Uiso 1 1 calc R . . C46B C 1.1577(9) 0.2709(9) -0.0635(7) 0.032(3) Uani 1 1 d . . . H46A H 1.1329 0.3057 -0.0364 0.038 Uiso 1 1 calc R . . H46B H 1.1572 0.3054 -0.1091 0.038 Uiso 1 1 calc R . . C46A C 0.3482(9) 0.3517(10) 0.5657(7) 0.034(4) Uani 1 1 d . . . H46C H 0.3838 0.3825 0.5428 0.041 Uiso 1 1 calc R . . H46D H 0.3489 0.3355 0.6125 0.041 Uiso 1 1 calc R . . O1 O 0.7271(6) 0.4296(6) 0.3696(5) 0.036(2) Uani 1 1 d . . . O2 O 0.6591(7) 0.5435(7) 0.2567(5) 0.042(3) Uani 1 1 d . . . O3 O 0.9149(6) 0.4095(6) 0.2618(5) 0.035(2) Uani 1 1 d . . . O4 O 0.8422(6) 0.4952(6) 0.1486(5) 0.036(2) Uani 1 1 d . . . O5 O 0.8108(6) 0.2193(7) 0.2946(5) 0.037(3) Uani 1 1 d . . . O6 O 0.7043(6) 0.3262(7) 0.2014(5) 0.036(2) Uani 1 1 d . . . O7 O 0.8932(6) 0.3128(6) 0.1741(5) 0.031(2) Uani 1 1 d U . . O8 O 0.6374(6) 0.3625(7) 0.3258(6) 0.039(3) Uani 1 1 d . . . O9 O 0.9636(7) 0.3935(6) 0.0476(5) 0.042(3) Uani 1 1 d . . . O10 O 0.5904(7) 0.3434(8) 0.4582(6) 0.052(3) Uani 1 1 d . . . O11 O 1.2246(7) 0.3618(8) 0.0776(7) 0.053(3) Uani 1 1 d . . . O12 O 1.0663(7) 0.4666(8) 0.0595(6) 0.056(3) Uani 1 1 d . . . O13 O 1.1633(7) 0.3167(8) 0.2207(7) 0.054(3) Uani 1 1 d . . . N1 N 0.8579(8) 0.2860(9) 0.3704(6) 0.039(3) Uani 1 1 d . . . N2 N 0.6887(7) 0.5020(8) 0.1387(6) 0.034(3) Uani 1 1 d . . . N3 N 0.2929(11) 0.2848(12) 0.3520(8) 0.064(5) Uani 1 1 d . . . H3 H 0.3240 0.3065 0.3584 0.077 Uiso 1 1 calc R . . N4 N 1.2359(8) -0.0664(9) 0.1352(7) 0.043(3) Uani 1 1 d . . . H4 H 1.1941 -0.0205 0.1343 0.051 Uiso 1 1 calc R . . C1 C 0.8024(9) 0.2958(10) 0.4280(7) 0.034(4) Uani 1 1 d . . . H1A H 0.8290 0.2643 0.4664 0.041 Uiso 1 1 calc R . . H1B H 0.7622 0.2739 0.4324 0.041 Uiso 1 1 calc R . . C2 C 0.7634(9) 0.3837(10) 0.4269(8) 0.037(4) Uani 1 1 d . . . H2A H 0.7248 0.3865 0.4657 0.044 Uiso 1 1 calc R . . H2B H 0.8022 0.4051 0.4266 0.044 Uiso 1 1 calc R . . C3 C 0.6897(11) 0.5121(12) 0.3636(10) 0.052(5) Uani 1 1 d . . . H3A H 0.7273 0.5408 0.3427 0.062 Uiso 1 1 calc R . . H3B H 0.6689 0.5175 0.4069 0.062 Uiso 1 1 calc R . . C4 C 0.6252(11) 0.5483(11) 0.3237(9) 0.049(5) Uani 1 1 d . . . H4C H 0.5881 0.5189 0.3437 0.059 Uiso 1 1 calc R . . H4D H 0.5978 0.6044 0.3214 0.059 Uiso 1 1 calc R . . C5 C 0.5967(10) 0.5657(11) 0.2210(9) 0.048(4) Uani 1 1 d . . . H5A H 0.5562 0.6154 0.2256 0.058 Uiso 1 1 calc R . . H5B H 0.5736 0.5231 0.2372 0.058 Uiso 1 1 calc R . . C6 C 0.6338(10) 0.5778(10) 0.1498(8) 0.041(4) Uani 1 1 d . . . H6C H 0.5930 0.6010 0.1226 0.049 Uiso 1 1 calc R . . H6D H 0.6615 0.6163 0.1363 0.049 Uiso 1 1 calc R . . C7 C 0.9272(9) 0.3069(11) 0.3670(8) 0.040(4) Uani 1 1 d . . . H7A H 0.9643 0.2597 0.3928 0.048 Uiso 1 1 calc R . . H7B H 0.9108 0.3494 0.3862 0.048 Uiso 1 1 calc R . . C8 C 0.9671(8) 0.3352(10) 0.2972(8) 0.036(4) Uani 1 1 d . . . H8A H 1.0147 0.3432 0.2974 0.043 Uiso 1 1 calc R . . H8B H 0.9810 0.2947 0.2764 0.043 Uiso 1 1 calc R . . C9 C 0.9551(9) 0.4457(9) 0.1984(8) 0.039(4) Uani 1 1 d . . . H9A H 0.9787 0.4077 0.1741 0.047 Uiso 1 1 calc R . . H9B H 0.9962 0.4596 0.2043 0.047 Uiso 1 1 calc R . . C10 C 0.8975(9) 0.5194(10) 0.1619(8) 0.038(4) Uani 1 1 d . . . H10G H 0.8707 0.5554 0.1879 0.046 Uiso 1 1 calc R . . H10H H 0.9237 0.5480 0.1210 0.046 Uiso 1 1 calc R . . C11 C 0.8049(9) 0.5527(11) 0.0915(9) 0.041(4) Uani 1 1 d . . . H11E H 0.8439 0.5603 0.0527 0.050 Uiso 1 1 calc R . . H11F H 0.7758 0.6048 0.0980 0.050 Uiso 1 1 calc R . . C12 C 0.7498(9) 0.5180(9) 0.0827(7) 0.035(4) Uani 1 1 d . . . H12E H 0.7247 0.5555 0.0443 0.042 Uiso 1 1 calc R . . H12F H 0.7808 0.4676 0.0737 0.042 Uiso 1 1 calc R . . C13 C 0.8856(10) 0.2015(9) 0.3714(8) 0.036(4) Uani 1 1 d . . . H13A H 0.9019 0.1659 0.4138 0.043 Uiso 1 1 calc R . . H13B H 0.9314 0.1939 0.3383 0.043 Uiso 1 1 calc R . . C14 C 0.8269(10) 0.1754(10) 0.3593(8) 0.040(4) Uani 1 1 d . . . H14A H 0.8479 0.1178 0.3656 0.048 Uiso 1 1 calc R . . H14B H 0.7793 0.1857 0.3901 0.048 Uiso 1 1 calc R . . C15 C 0.7576(8) 0.1952(10) 0.2789(8) 0.037(4) Uani 1 1 d . . . H15A H 0.7090 0.2042 0.3089 0.045 Uiso 1 1 calc R . . H15B H 0.7796 0.1376 0.2849 0.045 Uiso 1 1 calc R . . C16 C 0.7407(9) 0.2414(9) 0.2092(8) 0.036(4) Uani 1 1 d . . . H16C H 0.7890 0.2330 0.1788 0.043 Uiso 1 1 calc R . . H16D H 0.7062 0.2220 0.1997 0.043 Uiso 1 1 calc R . . C17 C 0.6902(11) 0.3724(11) 0.1341(8) 0.045(4) Uani 1 1 d . . . H17A H 0.6603 0.3509 0.1213 0.055 Uiso 1 1 calc R . . H17B H 0.7396 0.3683 0.1049 0.055 Uiso 1 1 calc R . . C18 C 0.6470(8) 0.4571(9) 0.1291(9) 0.036(4) Uani 1 1 d . . . H18C H 0.6001 0.4589 0.1613 0.043 Uiso 1 1 calc R . . H18D H 0.6305 0.4855 0.0859 0.043 Uiso 1 1 calc R . . C19 C 0.3118(14) 0.2957(17) 0.2786(13) 0.082(7) Uani 1 1 d . . . H19A H 0.3677 0.2706 0.2679 0.099 Uiso 1 1 calc R . . H19B H 0.2856 0.2673 0.2697 0.099 Uiso 1 1 calc R . . C20 C 0.2895(13) 0.3792(15) 0.2360(10) 0.070(7) Uani 1 1 d . . . H20G H 0.2357 0.4066 0.2496 0.105 Uiso 1 1 calc R . . H20H H 0.2959 0.3808 0.1915 0.105 Uiso 1 1 calc R . . H20I H 0.3219 0.4055 0.2386 0.105 Uiso 1 1 calc R . . C21 C 0.2165(14) 0.3268(15) 0.3757(12) 0.071(6) Uani 1 1 d . . . H21G H 0.1797 0.3100 0.3664 0.085 Uiso 1 1 calc R . . H21H H 0.2055 0.3844 0.3522 0.085 Uiso 1 1 calc R . . C22 C 0.2037(15) 0.3124(16) 0.4488(12) 0.081(7) Uani 1 1 d U . . H22G H 0.1936 0.2620 0.4726 0.122 Uiso 1 1 calc R . . H22H H 0.1597 0.3559 0.4591 0.122 Uiso 1 1 calc R . . H22I H 0.2496 0.3102 0.4609 0.122 Uiso 1 1 calc R . . C23 C 0.3242(14) 0.1938(14) 0.3895(12) 0.073(6) Uani 1 1 d U . . H23E H 0.3765 0.1705 0.3688 0.087 Uiso 1 1 calc R . . H23F H 0.3272 0.1858 0.4344 0.087 Uiso 1 1 calc R . . C24 C 0.2709(16) 0.1511(17) 0.3901(14) 0.092(8) Uani 1 1 d U . . H24A H 0.2273 0.1575 0.4245 0.138 Uiso 1 1 calc R . . H24B H 0.2996 0.0945 0.3979 0.138 Uiso 1 1 calc R . . H24C H 0.2523 0.1745 0.3485 0.138 Uiso 1 1 calc R . . C25 C 1.2064(14) -0.1186(14) 0.1248(12) 0.072(6) Uani 1 1 d U . . H25A H 1.1839 -0.0907 0.0842 0.086 Uiso 1 1 calc R . . H25B H 1.1652 -0.1305 0.1605 0.086 Uiso 1 1 calc R . . C26 C 1.2707(16) -0.1982(17) 0.1209(14) 0.097(9) Uani 1 1 d U . . H26A H 1.3203 -0.1961 0.1221 0.145 Uiso 1 1 calc R . . H26B H 1.2724 -0.2057 0.0807 0.145 Uiso 1 1 calc R . . H26C H 1.2597 -0.2426 0.1576 0.145 Uiso 1 1 calc R . . C27 C 1.2628(14) -0.0936(16) 0.2015(13) 0.080(7) Uani 1 1 d . . . H27C H 1.2765 -0.0512 0.2041 0.096 Uiso 1 1 calc R . . H27D H 1.3088 -0.1418 0.2058 0.096 Uiso 1 1 calc R . . C28 C 1.1965(12) -0.1122(12) 0.2580(10) 0.060(5) Uani 1 1 d . . . H28A H 1.1469 -0.0810 0.2426 0.090 Uiso 1 1 calc R . . H28B H 1.1982 -0.0981 0.2940 0.090 Uiso 1 1 calc R . . H28C H 1.2033 -0.1690 0.2725 0.090 Uiso 1 1 calc R . . C29 C 1.2964(16) -0.0384(13) 0.0805(13) 0.081(8) Uani 1 1 d . . . H29C H 1.3441 -0.0841 0.0799 0.097 Uiso 1 1 calc R . . H29D H 1.3084 0.0015 0.0889 0.097 Uiso 1 1 calc R . . C30 C 1.2688(15) -0.0010(13) 0.0133(10) 0.072(7) Uani 1 1 d . . . H30A H 1.2754 -0.0434 -0.0025 0.107 Uiso 1 1 calc R . . H30B H 1.2991 0.0325 -0.0170 0.107 Uiso 1 1 calc R . . H30C H 1.2146 0.0315 0.0174 0.107 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 0.0271(3) 0.0283(3) 0.0288(3) -0.0079(2) -0.0064(2) -0.0093(2) U2 0.0262(3) 0.0307(3) 0.0274(3) -0.0098(2) -0.0045(2) -0.0088(2) Ba 0.0291(5) 0.0322(5) 0.0318(5) -0.0114(4) -0.0025(4) -0.0116(4) O1A 0.025(5) 0.037(6) 0.029(5) -0.015(5) 0.001(5) -0.008(4) O2A 0.044(4) 0.020(4) 0.026(4) -0.005(3) 0.022(3) 0.002(3) O3A 0.035(6) 0.029(6) 0.028(5) -0.010(4) -0.010(5) -0.004(4) O4A 0.025(5) 0.023(5) 0.031(5) -0.011(4) -0.003(4) -0.001(4) O5A 0.035(6) 0.033(6) 0.030(5) -0.006(5) -0.014(5) -0.007(5) O6A 0.027(5) 0.029(6) 0.032(5) -0.011(5) -0.003(5) -0.008(4) O7A 0.039(6) 0.032(6) 0.039(6) -0.008(5) -0.004(5) -0.013(5) O8A 0.021(5) 0.038(6) 0.035(6) -0.015(5) -0.003(5) -0.008(4) O1B 0.035(6) 0.038(6) 0.034(6) -0.014(5) -0.003(5) -0.008(5) O2B 0.025(4) 0.029(4) 0.028(4) -0.017(3) 0.011(3) -0.020(3) O3B 0.031(6) 0.042(7) 0.031(6) -0.008(5) -0.006(5) -0.014(5) O4B 0.033(6) 0.037(6) 0.025(5) -0.015(5) 0.000(4) -0.018(5) O5B 0.038(6) 0.039(6) 0.030(5) -0.010(5) -0.008(5) -0.015(5) O6B 0.026(5) 0.038(6) 0.026(5) -0.010(4) 0.000(4) -0.018(4) O7B 0.047(7) 0.040(7) 0.047(7) -0.019(6) -0.005(6) -0.017(5) O8B 0.031(6) 0.037(6) 0.034(6) -0.016(5) -0.007(5) -0.005(5) C1A 0.047(10) 0.030(9) 0.028(8) -0.012(7) -0.004(8) -0.013(7) C1B 0.028(8) 0.030(8) 0.030(7) -0.009(6) 0.000(7) -0.017(6) C2B 0.028(8) 0.023(8) 0.034(8) -0.004(6) -0.005(7) -0.010(6) C2A 0.036(9) 0.030(8) 0.029(8) -0.009(7) -0.012(7) -0.007(7) C3B 0.037(9) 0.038(9) 0.022(7) 0.001(7) -0.002(7) -0.014(7) C3A 0.044(9) 0.027(8) 0.022(7) -0.010(6) -0.006(7) -0.007(7) C4A 0.033(9) 0.043(10) 0.030(8) -0.013(7) -0.009(7) -0.005(7) C4B 0.030(9) 0.034(9) 0.047(10) -0.001(8) -0.011(8) -0.008(7) C5A 0.041(10) 0.065(13) 0.055(11) -0.033(10) -0.008(9) -0.025(9) C5B 0.029(8) 0.035(9) 0.045(9) -0.013(8) 0.006(8) -0.017(7) C6B 0.040(9) 0.045(10) 0.024(7) -0.009(7) -0.006(7) -0.015(7) C6A 0.059(11) 0.028(9) 0.033(8) -0.013(7) -0.009(9) -0.005(8) C7B 0.036(10) 0.062(13) 0.049(10) -0.026(9) -0.001(9) -0.013(8) C7A 0.064(13) 0.048(11) 0.049(11) -0.021(9) 0.012(10) -0.028(10) C8B 0.113(11) 0.112(11) 0.113(11) -0.042(6) -0.013(5) -0.035(6) C8A 0.056(13) 0.13(2) 0.053(12) -0.048(14) 0.013(11) -0.041(14) C9A 0.058(7) 0.056(6) 0.058(7) -0.019(4) -0.006(4) -0.025(5) C9B 0.105(10) 0.104(10) 0.101(10) -0.034(6) -0.010(5) -0.030(5) C10B 0.098(10) 0.098(10) 0.096(10) -0.037(5) -0.013(5) -0.028(5) C10A 0.059(14) 0.072(16) 0.082(16) -0.045(13) 0.008(13) -0.004(11) C11A 0.036(9) 0.055(11) 0.027(8) -0.025(8) -0.002(7) -0.009(8) C11B 0.033(9) 0.060(12) 0.047(10) -0.019(9) -0.020(8) -0.002(8) C12B 0.037(10) 0.061(12) 0.039(10) 0.016(9) -0.012(8) -0.025(9) C12A 0.043(10) 0.037(10) 0.046(10) -0.018(8) -0.015(8) -0.003(7) C13B 0.031(8) 0.051(11) 0.032(8) -0.010(8) -0.009(7) -0.017(7) C13A 0.031(8) 0.021(8) 0.041(9) -0.003(7) -0.009(7) 0.001(6) C14A 0.031(8) 0.034(9) 0.033(8) -0.011(7) -0.006(7) -0.014(7) C14B 0.030(8) 0.026(8) 0.039(8) -0.018(7) -0.017(7) -0.001(6) C15B 0.029(8) 0.034(8) 0.023(7) -0.011(6) -0.009(6) -0.010(6) C15A 0.035(9) 0.035(9) 0.028(8) 0.001(7) -0.003(7) -0.021(7) C16B 0.033(9) 0.056(11) 0.024(7) -0.010(7) -0.006(7) -0.019(8) C16A 0.027(8) 0.027(8) 0.041(9) -0.005(7) -0.001(7) -0.009(6) C17A 0.041(9) 0.043(10) 0.025(8) -0.014(7) 0.002(7) -0.017(7) C17B 0.031(9) 0.071(13) 0.045(10) -0.020(9) -0.004(8) -0.025(9) C18A 0.025(8) 0.039(10) 0.039(9) -0.002(7) -0.010(7) -0.002(7) C18B 0.030(8) 0.028(8) 0.035(8) -0.005(7) -0.012(7) -0.005(6) C19A 0.036(9) 0.068(13) 0.037(9) -0.023(9) -0.013(8) -0.006(8) C19B 0.048(11) 0.069(13) 0.025(8) 0.001(8) -0.006(8) -0.020(10) C20B 0.036(10) 0.069(14) 0.052(11) -0.008(10) -0.008(9) 0.002(9) C20A 0.085(9) 0.087(9) 0.086(8) -0.031(5) -0.018(5) -0.026(5) C21B 0.060(13) 0.054(13) 0.070(14) 0.009(11) -0.024(12) -0.014(10) C21A 0.058(13) 0.103(19) 0.049(12) -0.022(12) -0.018(11) -0.021(12) C22A 0.071(16) 0.10(2) 0.055(13) 0.017(13) -0.031(12) -0.024(14) C22B 0.054(13) 0.076(15) 0.045(11) -0.023(11) -0.002(10) 0.002(11) C23A 0.025(8) 0.038(9) 0.029(8) -0.004(7) -0.003(7) -0.019(7) C23B 0.038(9) 0.037(9) 0.028(7) -0.018(7) -0.005(7) -0.016(7) C24A 0.030(8) 0.039(9) 0.029(8) 0.004(7) -0.011(7) -0.020(7) C24B 0.026(8) 0.060(11) 0.032(8) -0.013(8) -0.003(7) -0.020(8) C25A 0.025(8) 0.048(10) 0.032(8) -0.021(7) 0.003(7) -0.015(7) C25B 0.028(8) 0.032(8) 0.021(7) -0.011(6) 0.000(6) -0.003(6) C26A 0.026(8) 0.032(9) 0.034(8) -0.010(7) -0.007(7) -0.008(6) C26B 0.024(8) 0.041(9) 0.030(8) -0.016(7) 0.009(7) -0.011(7) C27A 0.027(8) 0.050(10) 0.029(8) -0.013(7) -0.002(7) -0.016(7) C27B 0.020(8) 0.050(10) 0.038(9) -0.011(8) 0.001(7) -0.016(7) C28B 0.026(8) 0.034(9) 0.038(8) -0.009(7) -0.006(7) -0.012(6) C28A 0.026(8) 0.035(9) 0.044(9) -0.007(7) -0.006(7) -0.012(7) C29A 0.039(9) 0.033(9) 0.027(7) -0.007(6) -0.013(7) -0.013(7) C29B 0.034(9) 0.041(9) 0.026(7) -0.006(7) -0.004(7) -0.018(7) C30B 0.062(12) 0.050(11) 0.022(8) 0.007(7) -0.016(8) -0.027(9) C30A 0.047(10) 0.049(11) 0.030(8) -0.011(8) -0.010(8) -0.015(8) C31A 0.065(13) 0.041(11) 0.058(11) -0.017(9) -0.001(10) -0.025(9) C31B 0.108(19) 0.055(13) 0.036(10) -0.018(9) 0.012(11) -0.041(12) C32B 0.068(7) 0.069(7) 0.064(7) -0.017(5) -0.013(5) -0.028(5) C32A 0.084(16) 0.074(15) 0.065(13) -0.041(12) -0.034(12) -0.004(12) C33B 0.069(14) 0.052(13) 0.067(13) 0.005(10) -0.027(12) -0.026(11) C33A 0.081(15) 0.053(12) 0.036(10) -0.014(9) 0.019(10) -0.025(11) C34B 0.028(8) 0.029(8) 0.030(8) -0.001(6) 0.003(7) -0.018(6) C34A 0.028(8) 0.022(8) 0.035(8) -0.009(6) -0.002(7) -0.002(6) C35B 0.042(10) 0.045(10) 0.035(8) -0.010(8) -0.009(8) -0.019(8) C35A 0.021(7) 0.041(9) 0.033(8) -0.010(7) -0.014(7) 0.003(6) C36B 0.017(7) 0.041(9) 0.030(8) -0.009(7) 0.000(7) -0.010(6) C36A 0.051(10) 0.013(7) 0.027(7) -0.004(6) -0.015(7) -0.003(6) C37B 0.033(8) 0.026(8) 0.027(7) -0.012(6) -0.007(7) -0.007(6) C37A 0.029(8) 0.025(8) 0.021(7) -0.003(6) -0.004(6) -0.007(6) C38B 0.031(8) 0.028(8) 0.032(8) 0.003(6) -0.015(7) -0.012(6) C38A 0.030(8) 0.033(9) 0.029(8) -0.008(7) -0.003(7) -0.010(6) C39B 0.033(9) 0.042(10) 0.033(8) -0.023(7) 0.001(7) -0.007(7) C39A 0.050(10) 0.040(10) 0.019(7) -0.009(7) -0.002(7) -0.010(8) C40B 0.049(10) 0.036(9) 0.036(9) -0.007(7) -0.005(8) -0.019(8) C40A 0.060(11) 0.024(8) 0.038(9) -0.011(7) -0.004(8) -0.016(8) C41A 0.050(11) 0.041(10) 0.036(9) -0.017(8) -0.005(8) -0.008(8) C41B 0.040(9) 0.051(11) 0.037(9) -0.019(8) -0.004(8) -0.026(8) C42B 0.054(11) 0.068(13) 0.049(10) -0.037(10) 0.017(9) -0.046(10) C42A 0.081(15) 0.036(10) 0.040(10) 0.005(8) -0.010(10) -0.025(10) C43B 0.091(9) 0.091(9) 0.088(9) -0.031(5) -0.014(5) -0.034(5) C43A 0.079(15) 0.061(14) 0.072(14) -0.006(11) 0.001(12) -0.056(12) C44B 0.054(11) 0.067(12) 0.032(8) -0.018(8) -0.007(8) -0.035(9) C44A 0.077(8) 0.069(8) 0.073(8) -0.023(5) -0.004(5) -0.027(5) C45A 0.12(2) 0.042(12) 0.047(11) 0.003(9) -0.014(12) -0.042(13) C45B 0.076(8) 0.073(8) 0.075(8) -0.030(5) -0.008(5) -0.026(5) C46B 0.041(9) 0.033(9) 0.026(7) -0.012(7) -0.009(7) -0.012(7) C46A 0.040(9) 0.038(9) 0.026(7) -0.014(7) -0.004(7) -0.013(7) O1 0.039(6) 0.029(6) 0.045(6) -0.015(5) -0.013(5) -0.008(5) O2 0.048(7) 0.047(7) 0.038(6) -0.018(5) 0.001(6) -0.022(6) O3 0.031(6) 0.036(6) 0.043(6) -0.018(5) 0.001(5) -0.016(5) O4 0.041(6) 0.033(6) 0.029(5) -0.001(5) -0.007(5) -0.015(5) O5 0.032(6) 0.043(7) 0.033(6) -0.007(5) -0.008(5) -0.013(5) O6 0.031(6) 0.038(6) 0.043(6) -0.018(5) -0.003(5) -0.012(5) O7 0.028(4) 0.036(4) 0.029(4) -0.012(3) -0.002(3) -0.009(3) O8 0.038(6) 0.039(7) 0.037(6) -0.005(5) -0.007(5) -0.016(5) O9 0.049(7) 0.029(6) 0.032(6) -0.009(5) 0.003(5) -0.004(5) O10 0.055(8) 0.056(8) 0.047(7) -0.009(6) -0.015(6) -0.024(6) O11 0.045(7) 0.047(8) 0.066(8) -0.017(7) -0.005(7) -0.018(6) O12 0.042(7) 0.063(9) 0.061(8) -0.021(7) -0.001(7) -0.018(6) O13 0.053(8) 0.052(8) 0.076(9) -0.036(7) -0.008(7) -0.021(6) N1 0.035(7) 0.054(9) 0.031(7) -0.021(7) -0.002(6) -0.013(6) N2 0.030(7) 0.045(8) 0.030(7) -0.016(6) 0.008(6) -0.019(6) N3 0.090(14) 0.087(14) 0.040(9) -0.004(9) -0.012(9) -0.069(12) N4 0.038(8) 0.042(9) 0.041(8) -0.011(7) -0.010(7) -0.006(6) C1 0.029(8) 0.053(10) 0.025(7) -0.017(7) -0.002(7) -0.016(7) C2 0.031(8) 0.044(10) 0.047(9) -0.032(8) -0.004(8) -0.008(7) C3 0.056(12) 0.060(12) 0.064(12) -0.048(11) 0.004(10) -0.022(10) C4 0.051(11) 0.045(11) 0.051(11) -0.028(9) 0.005(9) -0.013(9) C5 0.043(10) 0.035(10) 0.065(12) -0.013(9) -0.016(9) -0.009(8) C6 0.047(10) 0.033(9) 0.039(9) -0.009(7) -0.018(8) -0.005(7) C7 0.025(8) 0.060(11) 0.034(8) -0.012(8) -0.012(7) -0.013(7) C8 0.012(7) 0.057(11) 0.047(9) -0.027(8) 0.009(7) -0.017(7) C9 0.040(9) 0.031(9) 0.055(10) -0.020(8) 0.002(8) -0.021(7) C10 0.034(9) 0.040(10) 0.050(10) -0.022(8) 0.008(8) -0.023(7) C11 0.031(9) 0.046(10) 0.051(10) -0.020(8) 0.004(8) -0.019(7) C12 0.040(9) 0.028(8) 0.029(8) 0.005(6) -0.016(7) -0.008(7) C13 0.042(9) 0.032(9) 0.031(8) -0.008(7) -0.007(7) -0.011(7) C14 0.043(10) 0.034(9) 0.034(8) -0.007(7) -0.017(8) -0.001(7) C15 0.017(7) 0.032(9) 0.044(9) -0.001(7) -0.014(7) 0.005(6) C16 0.040(9) 0.019(8) 0.047(9) -0.009(7) -0.013(8) -0.007(6) C17 0.058(11) 0.050(11) 0.035(9) -0.012(8) -0.017(9) -0.018(9) C18 0.021(8) 0.021(8) 0.055(10) -0.003(7) 0.000(8) -0.009(6) C19 0.063(15) 0.10(2) 0.10(2) -0.027(16) -0.025(15) -0.039(14) C20 0.069(14) 0.107(19) 0.057(12) -0.007(13) -0.021(11) -0.063(14) C21 0.079(16) 0.068(15) 0.084(16) -0.025(13) -0.020(14) -0.037(13) C22 0.081(8) 0.080(8) 0.085(8) -0.028(5) -0.009(5) -0.030(5) C23 0.076(8) 0.072(8) 0.074(8) -0.024(5) -0.011(5) -0.028(5) C24 0.094(9) 0.092(9) 0.094(9) -0.030(5) -0.012(5) -0.035(5) C25 0.073(8) 0.072(8) 0.075(8) -0.022(5) -0.011(5) -0.030(5) C26 0.096(10) 0.094(10) 0.096(10) -0.029(5) -0.013(5) -0.031(5) C27 0.069(15) 0.074(17) 0.11(2) -0.046(15) -0.020(15) -0.016(12) C28 0.063(13) 0.042(11) 0.052(11) -0.008(9) -0.012(10) 0.000(9) C29 0.12(2) 0.032(11) 0.11(2) -0.030(13) -0.027(17) -0.032(12) C30 0.106(19) 0.047(13) 0.048(12) -0.003(10) 0.006(12) -0.036(12) _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 O7A 1.792(11) . ? U1 O8A 1.801(10) . ? U1 O3A 2.269(10) . ? U1 O1A 2.269(9) . ? U1 O6A 2.289(10) . ? U1 O4A 2.301(9) . ? U1 O2A 3.817(11) . ? U1 O5A 3.844(10) . ? U2 O7B 1.780(11) . ? U2 O8B 1.811(10) . ? U2 O6B 2.260(9) . ? U2 O1B 2.266(11) . ? U2 O4B 2.278(9) . ? U2 O3B 2.278(10) . ? U2 O5B 3.708(10) . ? U2 O2B 3.842(9) . ? Ba O8 2.747(11) . ? Ba O7 2.771(10) . ? Ba O4 2.790(10) . ? Ba O1 2.790(10) . ? Ba O6 2.817(11) . ? Ba O2 2.850(12) . ? Ba O5 2.854(11) . ? Ba O3 2.896(10) . ? Ba N2 2.987(13) . ? Ba N1 2.999(13) . ? O1A C2A 1.363(18) . ? O2A C12A 1.410(19) . ? O2A C11A 1.550(17) . ? O3A C14A 1.363(17) . ? O4A C25A 1.326(17) . ? O4A O8 2.904(15) . ? O5A C35A 1.392(16) . ? O5A C34A 1.434(18) . ? O6A C37A 1.344(17) . ? O6A O10 2.757(16) . ? O1B C2B 1.381(18) . ? O1B O11 2.736(17) . ? O2B C12B 1.29(2) . ? O2B C11B 1.46(2) . ? O3B C14B 1.347(17) . ? O3B O13 2.731(16) . ? O4B C25B 1.364(18) . ? O4B O7 2.966(14) . ? O5B C34B 1.408(17) . ? O5B C35B 1.429(18) . ? O6B C37B 1.337(16) . ? O6B O9 2.802(15) . ? O7B O13 2.954(17) . ? O7B O9 2.971(16) . ? O7B O12 2.996(18) . ? C1A C6A 1.37(2) . ? C1A C2A 1.40(2) . ? C1A C46A 1.54(2) . ? C1B C2B 1.38(2) . ? C1B C6B 1.39(2) . ? C1B C46B 1.54(2) . ? C2B C3B 1.38(2) . ? C2A C3A 1.43(2) . ? C3B C4B 1.39(2) . ? C3B C11B 1.50(2) . ? C3A C4A 1.36(2) . ? C3A C11A 1.47(2) . ? C4A C5A 1.43(2) . ? C4B C5B 1.42(2) . ? C5A C6A 1.39(2) . ? C5A C7A 1.54(3) . ? C5B C6B 1.37(2) . ? C5B C7B 1.54(2) . ? C7B C10B 1.50(3) . ? C7B C9B 1.56(3) . ? C7B C8B 1.57(4) . ? C7A C9A 1.55(3) . ? C7A C10A 1.56(3) . ? C7A C8A 1.58(3) . ? C12B C13B 1.53(2) . ? C12A C13A 1.46(2) . ? C13B C18B 1.39(2) . ? C13B C14B 1.41(2) . ? C13A C18A 1.41(2) . ? C13A C14A 1.42(2) . ? C14A C15A 1.40(2) . ? C14B C15B 1.43(2) . ? C15B C16B 1.38(2) . ? C15B C23B 1.51(2) . ? C15A C16A 1.35(2) . ? C15A C23A 1.54(2) . ? C16B C17B 1.41(2) . ? C16A C17A 1.42(2) . ? C17A C18A 1.36(2) . ? C17A C19A 1.50(2) . ? C17B C18B 1.37(2) . ? C17B C19B 1.54(3) . ? C19A C20A 1.49(3) . ? C19A C21A 1.52(3) . ? C19A C22A 1.57(3) . ? C19B C22B 1.52(3) . ? C19B C20B 1.52(2) . ? C19B C21B 1.56(3) . ? C23A C24A 1.49(2) . ? C23B C24B 1.52(2) . ? C24A C25A 1.40(2) . ? C24A C29A 1.44(2) . ? C24B C29B 1.40(2) . ? C24B C25B 1.41(2) . ? C25A C26A 1.41(2) . ? C25B C26B 1.36(2) . ? C26A C27A 1.43(2) . ? C26A C34A 1.49(2) . ? C26B C27B 1.39(2) . ? C26B C34B 1.51(2) . ? C27A C28A 1.40(2) . ? C27B C28B 1.41(2) . ? C28B C29B 1.40(2) . ? C28B C30B 1.55(2) . ? C28A C29A 1.42(2) . ? C28A C30A 1.54(2) . ? C30B C33B 1.48(3) . ? C30B C32B 1.50(3) . ? C30B C31B 1.54(2) . ? C30A C31A 1.50(2) . ? C30A C32A 1.52(3) . ? C30A C33A 1.53(2) . ? C35B C36B 1.48(2) . ? C35A C36A 1.46(2) . ? C36B C41B 1.39(2) . ? C36B C37B 1.42(2) . ? C36A C41A 1.42(2) . ? C36A C37A 1.43(2) . ? C37B C38B 1.38(2) . ? C37A C38A 1.40(2) . ? C38B C39B 1.40(2) . ? C38B C46B 1.49(2) . ? C38A C39A 1.42(2) . ? C38A C46A 1.50(2) . ? C39B C40B 1.42(2) . ? C39A C40A 1.41(2) . ? C40B C41B 1.35(2) . ? C40B C42B 1.53(2) . ? C40A C41A 1.37(2) . ? C40A C42A 1.53(2) . ? C42B C44B 1.53(2) . ? C42B C45B 1.53(3) . ? C42B C43B 1.55(3) . ? C42A C45A 1.47(3) . ? C42A C44A 1.50(3) . ? C42A C43A 1.54(3) . ? O1 C3 1.41(2) . ? O1 C2 1.416(19) . ? O2 C5 1.44(2) . ? O2 C4 1.481(19) . ? O3 C8 1.424(19) . ? O3 C9 1.448(19) . ? O4 C10 1.439(18) . ? O4 C11 1.45(2) . ? O5 C14 1.404(18) . ? O5 C15 1.432(19) . ? O6 C16 1.435(18) . ? O6 C17 1.449(19) . ? O7 O9 2.862(14) . ? O8 O10 2.766(17) . ? O9 O12 2.759(17) 2_765 ? O9 O12 2.923(18) . ? O11 O12 2.884(18) . ? O11 O13 2.977(19) . ? N1 C1 1.438(19) . ? N1 C13 1.47(2) . ? N1 C7 1.49(2) . ? N2 C12 1.469(19) . ? N2 C6 1.47(2) . ? N2 C18 1.48(2) . ? N3 C21 1.41(3) . ? N3 C19 1.53(3) . ? N3 C23 1.53(3) . ? N4 C25 1.43(3) . ? N4 C29 1.51(3) . ? N4 C27 1.53(3) . ? C1 C2 1.53(2) . ? C3 C4 1.49(3) . ? C5 C6 1.52(2) . ? C7 C8 1.51(2) . ? C9 C10 1.48(2) . ? C11 C12 1.53(2) . ? C13 C14 1.51(2) . ? C15 C16 1.51(2) . ? C17 C18 1.46(2) . ? C19 C20 1.44(3) . ? C21 C22 1.51(3) . ? C23 C24 1.52(3) . ? C25 C26 1.53(3) . ? C27 C28 1.55(3) . ? C29 C30 1.53(3) . ? 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 O7A U1 O8A 179.8(5) . . ? O7A U1 O3A 87.5(4) . . ? O8A U1 O3A 92.4(4) . . ? O7A U1 O1A 87.0(4) . . ? O8A U1 O1A 93.2(4) . . ? O3A U1 O1A 95.8(4) . . ? O7A U1 O6A 89.2(4) . . ? O8A U1 O6A 90.9(4) . . ? O3A U1 O6A 176.7(4) . . ? O1A U1 O6A 84.5(4) . . ? O7A U1 O4A 88.3(4) . . ? O8A U1 O4A 91.5(4) . . ? O3A U1 O4A 85.7(3) . . ? O1A U1 O4A 175.0(4) . . ? O6A U1 O4A 93.7(3) . . ? O7B U2 O8B 179.1(5) . . ? O7B U2 O6B 87.7(4) . . ? O8B U2 O6B 91.9(4) . . ? O7B U2 O1B 87.4(5) . . ? O8B U2 O1B 93.3(4) . . ? O6B U2 O1B 85.6(4) . . ? O7B U2 O4B 86.7(4) . . ? O8B U2 O4B 92.6(4) . . ? O6B U2 O4B 95.1(3) . . ? O1B U2 O4B 174.1(4) . . ? O7B U2 O3B 86.4(5) . . ? O8B U2 O3B 94.0(4) . . ? O6B U2 O3B 174.1(4) . . ? O1B U2 O3B 93.4(4) . . ? O4B U2 O3B 85.3(3) . . ? O8 Ba O7 131.9(3) . . ? O8 Ba O4 147.3(3) . . ? O7 Ba O4 66.7(3) . . ? O8 Ba O1 66.3(3) . . ? O7 Ba O1 147.2(3) . . ? O4 Ba O1 114.3(3) . . ? O8 Ba O6 64.1(3) . . ? O7 Ba O6 74.0(3) . . ? O4 Ba O6 107.7(3) . . ? O1 Ba O6 130.3(3) . . ? O8 Ba O2 72.5(3) . . ? O7 Ba O2 143.9(3) . . ? O4 Ba O2 80.1(3) . . ? O1 Ba O2 60.0(3) . . ? O6 Ba O2 104.7(3) . . ? O8 Ba O5 75.2(3) . . ? O7 Ba O5 64.0(3) . . ? O4 Ba O5 130.6(3) . . ? O1 Ba O5 105.6(3) . . ? O6 Ba O5 60.7(3) . . ? O2 Ba O5 147.7(3) . . ? O8 Ba O3 143.9(3) . . ? O7 Ba O3 73.1(3) . . ? O4 Ba O3 59.0(3) . . ? O1 Ba O3 80.0(3) . . ? O6 Ba O3 147.1(3) . . ? O2 Ba O3 102.2(3) . . ? O5 Ba O3 103.2(3) . . ? O8 Ba N2 89.9(3) . . ? O7 Ba N2 90.6(3) . . ? O4 Ba N2 60.5(3) . . ? O1 Ba N2 119.2(3) . . ? O6 Ba N2 62.0(3) . . ? O2 Ba N2 59.6(3) . . ? O5 Ba N2 121.6(3) . . ? O3 Ba N2 118.9(3) . . ? O8 Ba N1 90.7(3) . . ? O7 Ba N1 90.8(3) . . ? O4 Ba N1 118.3(3) . . ? O1 Ba N1 58.9(3) . . ? O6 Ba N1 120.4(4) . . ? O2 Ba N1 118.3(3) . . ? O5 Ba N1 60.9(3) . . ? O3 Ba N1 59.6(3) . . ? N2 Ba N1 177.5(4) . . ? C2A O1A U1 134.3(9) . . ? C12A O2A C11A 105.0(12) . . ? C14A O3A U1 128.8(9) . . ? C25A O4A U1 135.0(9) . . ? C25A O4A O8 119.3(8) . . ? U1 O4A O8 103.2(4) . . ? C35A O5A C34A 108.7(11) . . ? C37A O6A U1 133.0(9) . . ? C37A O6A O10 119.9(9) . . ? U1 O6A O10 107.1(4) . . ? C2B O1B U2 135.5(9) . . ? C2B O1B O11 118.9(9) . . ? U2 O1B O11 105.4(5) . . ? C12B O2B C11B 111.6(12) . . ? C14B O3B O13 125.0(9) . . ? U2 O3B O13 103.1(5) . . ? C25B O4B U2 132.9(9) . . ? C25B O4B O7 123.9(9) . . ? U2 O4B O7 99.6(4) . . ? C34B O5B C35B 110.9(11) . . ? C37B O6B O9 122.0(9) . . ? U2 O6B O9 102.8(4) . . ? U2 O7B O13 109.8(6) . . ? U2 O7B O9 110.8(5) . . ? O13 O7B O9 138.7(5) . . ? U2 O7B O12 143.5(6) . . ? O13 O7B O12 84.0(5) . . ? O9 O7B O12 58.7(4) . . ? C6A C1A C2A 119.9(15) . . ? C6A C1A C46A 121.1(14) . . ? C2A C1A C46A 118.9(14) . . ? C2B C1B C6B 118.2(13) . . ? C2B C1B C46B 122.8(13) . . ? C6B C1B C46B 119.0(13) . . ? C1B C2B O1B 120.3(13) . . ? C1B C2B C3B 120.7(14) . . ? O1B C2B C3B 118.9(13) . . ? O1A C2A C1A 122.9(14) . . ? O1A C2A C3A 118.6(13) . . ? C1A C2A C3A 118.4(15) . . ? C2B C3B C4B 119.7(14) . . ? C2B C3B C11B 120.9(14) . . ? C4B C3B C11B 119.4(14) . . ? C4A C3A C2A 120.1(14) . . ? C4A C3A C11A 121.9(14) . . ? C2A C3A C11A 118.0(14) . . ? C3A C4A C5A 121.9(15) . . ? C3B C4B C5B 121.2(14) . . ? C6A C5A C4A 116.4(16) . . ? C6A C5A C7A 121.5(18) . . ? C4A C5A C7A 122.1(16) . . ? C6B C5B C4B 116.2(14) . . ? C6B C5B C7B 122.1(15) . . ? C4B C5B C7B 121.7(14) . . ? C5B C6B C1B 124.0(14) . . ? C1A C6A C5A 123.3(16) . . ? C10B C7B C5B 115.5(17) . . ? C10B C7B C9B 108(2) . . ? C5B C7B C9B 107.9(17) . . ? C10B C7B C8B 105(2) . . ? C5B C7B C8B 110.2(17) . . ? C9B C7B C8B 110(2) . . ? C5A C7A C9A 108.4(15) . . ? C5A C7A C10A 113.0(17) . . ? C9A C7A C10A 108.7(18) . . ? C5A C7A C8A 109.2(16) . . ? C9A C7A C8A 107.7(17) . . ? C10A C7A C8A 109.6(17) . . ? C3A C11A O2A 110.2(12) . . ? O2B C11B C3B 117.0(14) . . ? O2B C12B C13B 112.0(15) . . ? O2A C12A C13A 106.8(13) . . ? C18B C13B C14B 119.9(14) . . ? C18B C13B C12B 122.0(14) . . ? C14B C13B C12B 118.2(14) . . ? C18A C13A C14A 116.4(14) . . ? C18A C13A C12A 124.8(14) . . ? C14A C13A C12A 118.6(14) . . ? O3A C14A C15A 121.7(13) . . ? O3A C14A C13A 118.9(13) . . ? C15A C14A C13A 119.3(14) . . ? O3B C14B C13B 121.6(14) . . ? O3B C14B C15B 120.3(12) . . ? C13B C14B C15B 118.0(13) . . ? C16B C15B C14B 119.6(13) . . ? C16B C15B C23B 120.0(13) . . ? C14B C15B C23B 120.3(13) . . ? C16A C15A C14A 120.6(14) . . ? C16A C15A C23A 120.4(14) . . ? C14A C15A C23A 119.0(13) . . ? C15B C16B C17B 122.3(15) . . ? C15A C16A C17A 122.9(15) . . ? C18A C17A C16A 115.4(15) . . ? C18A C17A C19A 124.1(15) . . ? C16A C17A C19A 120.5(14) . . ? C18B C17B C16B 117.3(16) . . ? C18B C17B C19B 123.7(15) . . ? C16B C17B C19B 119.0(15) . . ? C17A C18A C13A 125.1(15) . . ? C17B C18B C13B 122.8(15) . . ? C20A C19A C17A 113.3(16) . . ? C20A C19A C21A 109.0(19) . . ? C17A C19A C21A 113.5(15) . . ? C20A C19A C22A 103.8(18) . . ? C17A C19A C22A 110.2(17) . . ? C21A C19A C22A 106.3(17) . . ? C22B C19B C20B 107.4(16) . . ? C22B C19B C17B 110.4(17) . . ? C20B C19B C17B 113.6(15) . . ? C22B C19B C21B 107.8(17) . . ? C20B C19B C21B 109.7(18) . . ? C17B C19B C21B 107.9(15) . . ? C24A C23A C15A 113.5(12) . . ? C15B C23B C24B 111.8(12) . . ? C25A C24A C29A 118.3(14) . . ? C25A C24A C23A 122.1(14) . . ? C29A C24A C23A 119.6(13) . . ? C29B C24B C25B 117.6(14) . . ? C29B C24B C23B 120.0(14) . . ? C25B C24B C23B 122.3(15) . . ? O4A C25A C24A 119.4(14) . . ? O4A C25A C26A 119.8(14) . . ? C24A C25A C26A 120.3(14) . . ? C26B C25B O4B 120.9(13) . . ? C26B C25B C24B 119.8(14) . . ? O4B C25B C24B 119.3(14) . . ? C25A C26A C27A 120.5(14) . . ? C25A C26A C34A 119.7(13) . . ? C27A C26A C34A 119.8(14) . . ? C25B C26B C27B 122.3(15) . . ? C25B C26B C34B 119.6(14) . . ? C27B C26B C34B 118.0(14) . . ? C28A C27A C26A 120.8(16) . . ? C26B C27B C28B 119.8(15) . . ? C29B C28B C27B 117.2(14) . . ? C29B C28B C30B 120.5(14) . . ? C27B C28B C30B 122.3(14) . . ? C27A C28A C29A 117.9(15) . . ? C27A C28A C30A 120.9(15) . . ? C29A C28A C30A 121.2(14) . . ? C28A C29A C24A 122.2(14) . . ? C28B C29B C24B 123.1(14) . . ? C33B C30B C32B 111.5(18) . . ? C33B C30B C31B 108.1(16) . . ? C32B C30B C31B 107.2(17) . . ? C33B C30B C28B 109.4(15) . . ? C32B C30B C28B 113.1(14) . . ? C31B C30B C28B 107.3(15) . . ? C31A C30A C32A 108.7(16) . . ? C31A C30A C33A 109.1(15) . . ? C32A C30A C33A 109.1(17) . . ? C31A C30A C28A 114.7(14) . . ? C32A C30A C28A 108.4(14) . . ? C33A C30A C28A 106.7(14) . . ? O5B C34B C26B 112.3(11) . . ? O5A C34A C26A 111.6(11) . . ? O5B C35B C36B 113.1(13) . . ? O5A C35A C36A 112.7(11) . . ? C41B C36B C37B 118.6(14) . . ? C41B C36B C35B 123.0(14) . . ? C37B C36B C35B 118.2(14) . . ? C41A C36A C37A 118.2(14) . . ? C41A C36A C35A 123.3(14) . . ? C37A C36A C35A 118.4(14) . . ? O6B C37B C38B 121.9(13) . . ? O6B C37B C36B 119.9(13) . . ? C38B C37B C36B 118.1(13) . . ? O6A C37A C38A 120.9(13) . . ? O6A C37A C36A 119.9(13) . . ? C38A C37A C36A 118.9(13) . . ? C37B C38B C39B 121.1(14) . . ? C37B C38B C46B 120.9(14) . . ? C39B C38B C46B 117.8(14) . . ? C37A C38A C39A 119.4(14) . . ? C37A C38A C46A 121.5(14) . . ? C39A C38A C46A 119.1(14) . . ? C38B C39B C40B 121.3(15) . . ? C40A C39A C38A 123.2(15) . . ? C41B C40B C39B 116.1(15) . . ? C41B C40B C42B 124.1(15) . . ? C39B C40B C42B 119.8(14) . . ? C41A C40A C39A 115.2(15) . . ? C41A C40A C42A 121.5(16) . . ? C39A C40A C42A 123.0(15) . . ? C40A C41A C36A 124.8(16) . . ? C40B C41B C36B 124.7(15) . . ? C40B C42B C44B 111.6(14) . . ? C40B C42B C45B 108.4(16) . . ? C44B C42B C45B 108.4(16) . . ? C40B C42B C43B 111.4(16) . . ? C44B C42B C43B 108.8(17) . . ? C45B C42B C43B 108.2(17) . . ? C45A C42A C44A 110.3(17) . . ? C45A C42A C40A 109.5(18) . . ? C44A C42A C40A 112.2(17) . . ? C45A C42A C43A 110.1(18) . . ? C44A C42A C43A 106.9(18) . . ? C40A C42A C43A 107.8(15) . . ? C38B C46B C1B 113.0(12) . . ? C38A C46A C1A 114.6(13) . . ? C3 O1 C2 112.9(12) . . ? C5 O2 C4 108.9(13) . . ? C8 O3 C9 110.3(11) . . ? C10 O4 C11 113.4(12) . . ? C14 O5 C15 111.8(12) . . ? C16 O6 C17 110.2(12) . . ? C1 N1 C13 110.8(13) . . ? C1 N1 C7 110.8(12) . . ? C13 N1 C7 107.9(13) . . ? C12 N2 C6 111.0(13) . . ? C12 N2 C18 110.8(12) . . ? C6 N2 C18 111.1(12) . . ? C21 N3 C19 117.3(18) . . ? C21 N3 C23 116.1(16) . . ? C19 N3 C23 107.7(19) . . ? C25 N4 C29 114.6(16) . . ? C25 N4 C27 117.6(17) . . ? C29 N4 C27 109.6(16) . . ? N1 C1 C2 114.1(14) . . ? O1 C2 C1 108.3(11) . . ? O1 C3 C4 110.1(14) . . ? O2 C4 C3 108.4(14) . . ? O2 C5 C6 105.7(14) . . ? N2 C6 C5 112.9(14) . . ? N1 C7 C8 112.6(12) . . ? O3 C8 C7 108.6(12) . . ? O3 C9 C10 108.2(13) . . ? O4 C10 C9 108.2(12) . . ? O4 C11 C12 107.3(13) . . ? N2 C12 C11 115.6(13) . . ? N1 C13 C14 115.4(13) . . ? O5 C14 C13 108.8(14) . . ? O5 C15 C16 112.1(13) . . ? O6 C16 C15 109.1(13) . . ? O6 C17 C18 108.9(14) . . ? C17 C18 N2 116.8(13) . . ? C20 C19 N3 115(2) . . ? N3 C21 C22 113(2) . . ? C24 C23 N3 110.4(19) . . ? N4 C25 C26 112(2) . . ? N4 C27 C28 109.8(17) . . ? N4 C29 C30 112.1(19) . . ? 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 N3 H3 O8A 0.91 1.99 2.792(19) 146.0 . N4 H4 O8B 0.91 1.95 2.729(18) 142.1 .