# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _publ_contact_author_name 'Berryman, Orion' _publ_contact_author_email orion@scripps.edu _publ_section_title ; Encapsulation of the uranyl dication ; loop_ _publ_author_name S.Beer O.Berryman D.Ajami 'J.Rebek Jr.' # Attachment '760897.cif.txt' data_steb _database_code_depnum_ccdc_archive 'CCDC 760897' #TrackingRef '760897.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64.50 H58 Cl3 N O8 U' _chemical_formula_weight 1319.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.258(3) _cell_length_b 18.699(4) _cell_length_c 23.046(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.19(3) _cell_angle_gamma 90.00 _cell_volume 5901(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6034 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 14.5 _exptl_crystal_description Parallalepiped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2636 _exptl_absorpt_coefficient_mu 2.941 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5511 _exptl_absorpt_correction_T_max 0.6667 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 20725 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9618 _reflns_number_gt 6514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The thermal paprameters of carbon atoms C40 > C57 C58 > C63 C64 and C65 were restrained to avoid excesive ADP max/min ratio. One of the solvent C2H2Cl2 molecules (C 65 Cl3 Cl4) was reduced to 0.5 occupancy factor. Because of the solvent molecules in the lattice, high angle data was cut to avoid instability in the refinement. This resulted in low data completeness. ; _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^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9618 _refine_ls_number_parameters 668 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1765 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 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 0.89871(3) 0.148445(17) 0.223268(17) 0.03826(16) Uani 1 1 d . . . O1 O 0.8320(4) 0.1198(3) 0.1520(3) 0.0437(17) Uani 1 1 d . . . O2 O 0.9640(6) 0.1768(3) 0.2942(3) 0.057(2) Uani 1 1 d . . . O3 O 1.0392(4) 0.0801(3) 0.2127(3) 0.0452(17) Uani 1 1 d . . . O4 O 0.9381(4) 0.0215(3) 0.2519(3) 0.0379(15) Uani 1 1 d . . . O5 O 0.8821(5) 0.2781(3) 0.1926(3) 0.0440(16) Uani 1 1 d . . . O6 O 1.0037(5) 0.2181(3) 0.1754(3) 0.0449(17) Uani 1 1 d . . . O7 O 0.7468(5) 0.2035(3) 0.2328(3) 0.053(2) Uani 1 1 d . . . O8 O 0.7758(6) 0.0956(3) 0.2698(3) 0.061(2) Uani 1 1 d . . . C1 C 1.0149(7) 0.0231(5) 0.2350(4) 0.038(2) Uani 1 1 d . . . C2 C 1.0772(7) -0.0430(4) 0.2408(4) 0.036(2) Uani 1 1 d . . . C3 C 1.0478(7) -0.0989(5) 0.1985(5) 0.044(3) Uani 1 1 d . . . C4 C 1.1010(8) -0.1633(4) 0.2101(5) 0.045(3) Uani 1 1 d . . . H4 H 1.0834 -0.2015 0.1819 0.054 Uiso 1 1 calc R . . C5 C 1.1779(8) -0.1723(5) 0.2611(5) 0.046(3) Uani 1 1 d . . . H5 H 1.2121 -0.2165 0.2680 0.055 Uiso 1 1 calc R . . C6 C 1.2054(7) -0.1180(5) 0.3018(5) 0.041(2) Uani 1 1 d . . . H6 H 1.2581 -0.1248 0.3371 0.050 Uiso 1 1 calc R . . C7 C 1.1563(7) -0.0518(5) 0.2920(4) 0.036(2) Uani 1 1 d . . . C8 C 1.1901(7) 0.0063(5) 0.3382(5) 0.044(2) Uani 1 1 d . . . C9 C 1.2001(10) -0.0080(7) 0.3970(6) 0.083(4) Uani 1 1 d . . . H9 H 1.1814 -0.0534 0.4084 0.100 Uiso 1 1 calc R . . C10 C 1.2383(14) 0.0442(10) 0.4417(7) 0.127(7) Uani 1 1 d . . . H10 H 1.2474 0.0345 0.4834 0.152 Uiso 1 1 calc R . . C11 C 1.2626(12) 0.1120(9) 0.4217(9) 0.102(5) Uani 1 1 d . . . H11 H 1.2897 0.1477 0.4509 0.123 Uiso 1 1 calc R . . C12 C 1.2484(8) 0.1271(7) 0.3626(8) 0.072(4) Uani 1 1 d . . . H12 H 1.2618 0.1735 0.3501 0.086 Uiso 1 1 calc R . . C13 C 1.2139(7) 0.0736(5) 0.3209(5) 0.047(3) Uani 1 1 d . . . H13 H 1.2063 0.0830 0.2793 0.056 Uiso 1 1 calc R . . C14 C 0.9660(8) -0.0909(6) 0.1418(5) 0.049(3) Uani 1 1 d . . . C15 C 0.8964(8) -0.1461(6) 0.1238(5) 0.052(3) Uani 1 1 d . . . H15 H 0.8994 -0.1874 0.1483 0.063 Uiso 1 1 calc R . . C16 C 0.8236(10) -0.1394(7) 0.0699(6) 0.074(4) Uani 1 1 d . . . H16 H 0.7780 -0.1770 0.0566 0.088 Uiso 1 1 calc R . . C17 C 0.8167(10) -0.0778(9) 0.0348(6) 0.082(4) Uani 1 1 d . . . H17 H 0.7650 -0.0731 -0.0013 0.098 Uiso 1 1 calc R . . C18 C 0.8843(13) -0.0237(8) 0.0522(6) 0.089(5) Uani 1 1 d . . . H18 H 0.8802 0.0178 0.0278 0.107 Uiso 1 1 calc R . . C19 C 0.9581(10) -0.0305(6) 0.1054(5) 0.073(4) Uani 1 1 d . . . H19 H 1.0046 0.0069 0.1174 0.088 Uiso 1 1 calc R . . C20 C 0.9569(7) 0.2755(5) 0.1720(4) 0.041(2) Uani 1 1 d . . . C21 C 0.9889(7) 0.3415(5) 0.1473(6) 0.048(3) Uani 1 1 d . . . C22 C 0.9738(7) 0.3438(5) 0.0842(5) 0.048(3) Uani 1 1 d . . . C23 C 1.0017(8) 0.4084(7) 0.0605(6) 0.068(4) Uani 1 1 d . . . H23 H 0.9910 0.4128 0.0181 0.082 Uiso 1 1 calc R . . C24 C 1.0439(9) 0.4650(7) 0.0975(8) 0.081(4) Uani 1 1 d . . . H24 H 1.0619 0.5072 0.0802 0.097 Uiso 1 1 calc R . . C25 C 1.0600(8) 0.4602(5) 0.1594(7) 0.072(4) Uani 1 1 d . . . H25 H 1.0895 0.4991 0.1844 0.086 Uiso 1 1 calc R . . C26 C 1.0331(7) 0.3983(5) 0.1858(7) 0.058(3) Uani 1 1 d . . . C27 C 1.0577(7) 0.3941(6) 0.2523(6) 0.056(3) Uani 1 1 d . . . C28 C 1.0451(8) 0.4546(6) 0.2879(7) 0.071(4) Uani 1 1 d . . . H28 H 1.0187 0.4977 0.2682 0.085 Uiso 1 1 calc R . . C29 C 1.0707(9) 0.4510(8) 0.3495(8) 0.094(5) Uani 1 1 d . . . H29 H 1.0623 0.4919 0.3720 0.113 Uiso 1 1 calc R . . C30 C 1.1072(9) 0.3912(7) 0.3788(6) 0.078(4) Uani 1 1 d . . . H30 H 1.1229 0.3891 0.4216 0.094 Uiso 1 1 calc R . . C31 C 1.1222(8) 0.3308(6) 0.3454(7) 0.068(4) Uani 1 1 d . . . H31 H 1.1496 0.2884 0.3659 0.082 Uiso 1 1 calc R . . C32 C 1.0977(7) 0.3335(5) 0.2846(6) 0.052(3) Uani 1 1 d . . . H32 H 1.1082 0.2923 0.2630 0.063 Uiso 1 1 calc R . . C33 C 0.9312(7) 0.2850(6) 0.0441(5) 0.052(3) Uani 1 1 d . . . C34 C 0.9783(8) 0.2602(7) 0.0016(5) 0.065(3) Uani 1 1 d . . . H34 H 1.0376 0.2823 0.0002 0.078 Uiso 1 1 calc R . . C35 C 0.9422(9) 0.2062(8) -0.0371(6) 0.076(4) Uani 1 1 d . . . H35 H 0.9740 0.1921 -0.0664 0.091 Uiso 1 1 calc R . . C36 C 0.8593(11) 0.1719(8) -0.0335(6) 0.084(5) Uani 1 1 d . . . H36 H 0.8348 0.1330 -0.0598 0.101 Uiso 1 1 calc R . . C37 C 0.8086(8) 0.1938(7) 0.0092(5) 0.062(3) Uani 1 1 d . . . H37 H 0.7505 0.1704 0.0113 0.074 Uiso 1 1 calc R . . C38 C 0.8471(7) 0.2500(5) 0.0471(5) 0.047(3) Uani 1 1 d . . . H38 H 0.8150 0.2651 0.0760 0.056 Uiso 1 1 calc R . . C39 C 0.7208(10) 0.1493(6) 0.2565(6) 0.069(4) Uani 1 1 d . . . C40 C 0.6071(4) 0.1468(2) 0.2596(3) 0.097(3) Uani 1 1 d GU . . C41 C 0.5322(4) 0.1420(2) 0.2062(3) 0.104(3) Uani 1 1 d GU . . C42 C 0.4354(4) 0.1428(3) 0.2077(3) 0.111(4) Uani 1 1 d GU . . H42 H 0.3842 0.1395 0.1712 0.133 Uiso 1 1 calc R . . C43 C 0.4136(4) 0.1483(3) 0.2626(4) 0.110(4) Uani 1 1 d GU . . H43 H 0.3474 0.1489 0.2637 0.132 Uiso 1 1 calc R . . C44 C 0.4885(5) 0.1532(3) 0.3161(3) 0.094(3) Uani 1 1 d GU . . H44 H 0.4735 0.1570 0.3536 0.113 Uiso 1 1 calc R . . C45 C 0.5852(4) 0.1524(2) 0.3145(3) 0.109(3) Uani 1 1 d GU . . C46 C 0.5385(4) 0.1298(3) 0.1491(3) 0.138(4) Uani 1 1 d GU . . C47 C 0.4742(5) 0.1628(3) 0.0998(3) 0.154(5) Uani 1 1 d GU . . H47 H 0.4277 0.1963 0.1059 0.185 Uiso 1 1 calc R . . C48 C 0.4779(7) 0.1468(4) 0.0416(3) 0.176(6) Uani 1 1 d GU . . H48 H 0.4340 0.1694 0.0079 0.212 Uiso 1 1 calc R . . C49 C 0.5459(7) 0.0979(5) 0.0327(3) 0.191(6) Uani 1 1 d GU . . H49 H 0.5485 0.0870 -0.0071 0.229 Uiso 1 1 calc R . . C50 C 0.6103(6) 0.0649(5) 0.0820(3) 0.175(6) Uani 1 1 d GU . . H50 H 0.6567 0.0314 0.0759 0.211 Uiso 1 1 calc R . . C51 C 0.6065(5) 0.0808(4) 0.1402(3) 0.151(5) Uani 1 1 d GU . . H51 H 0.6505 0.0583 0.1739 0.182 Uiso 1 1 calc R . . C52 C 0.6684(5) 0.1591(3) 0.3678(3) 0.112(4) Uani 1 1 d GU . . C53 C 0.6553(6) 0.1284(3) 0.4199(3) 0.152(5) Uani 1 1 d GU . . H53 H 0.5972 0.1026 0.4182 0.182 Uiso 1 1 calc R . . C54 C 0.7273(7) 0.1353(4) 0.4745(3) 0.179(6) Uani 1 1 d GU . . H54 H 0.7184 0.1143 0.5101 0.215 Uiso 1 1 calc R . . C55 C 0.8123(7) 0.1731(5) 0.4769(3) 0.188(6) Uani 1 1 d GU . . H55 H 0.8615 0.1778 0.5143 0.226 Uiso 1 1 calc R . . C56 C 0.8254(6) 0.2038(5) 0.4248(3) 0.174(5) Uani 1 1 d GU . . H56 H 0.8835 0.2296 0.4265 0.209 Uiso 1 1 calc R . . C57 C 0.7534(5) 0.1968(4) 0.3703(3) 0.151(5) Uani 1 1 d GU . . H57 H 0.7624 0.2179 0.3347 0.181 Uiso 1 1 calc R . . N1 N 0.7190(7) 0.3691(5) 0.1952(4) 0.059(3) Uani 1 1 d . . . H1 H 0.7737 0.3423 0.1947 0.071 Uiso 1 1 calc R . . C58 C 0.7381(13) 0.4435(7) 0.1781(7) 0.102(5) Uani 1 1 d U . . H58A H 0.7980 0.4624 0.2070 0.123 Uiso 1 1 calc R . . H58B H 0.6828 0.4750 0.1792 0.123 Uiso 1 1 calc R . . C59 C 0.7509(10) 0.4420(7) 0.1133(6) 0.086(4) Uani 1 1 d U . . H59A H 0.7929 0.4017 0.1097 0.103 Uiso 1 1 calc R . . H59B H 0.7810 0.4868 0.1056 0.103 Uiso 1 1 calc R . . H59C H 0.6869 0.4365 0.0837 0.103 Uiso 1 1 calc R . . C60 C 0.7137(10) 0.3690(8) 0.2595(6) 0.080(4) Uani 1 1 d U . . H60A H 0.6868 0.3225 0.2678 0.096 Uiso 1 1 calc R . . H60B H 0.6679 0.4068 0.2641 0.096 Uiso 1 1 calc R . . C61 C 0.8104(9) 0.3808(9) 0.3055(7) 0.091(4) Uani 1 1 d U . . H61A H 0.8579 0.3460 0.2992 0.109 Uiso 1 1 calc R . . H61B H 0.8027 0.3749 0.3462 0.109 Uiso 1 1 calc R . . H61C H 0.8335 0.4293 0.3011 0.109 Uiso 1 1 calc R . . C62 C 0.6355(9) 0.3338(7) 0.1538(7) 0.073(4) Uani 1 1 d U . . H62A H 0.6452 0.3340 0.1129 0.088 Uiso 1 1 calc R . . H62B H 0.6343 0.2833 0.1664 0.088 Uiso 1 1 calc R . . C63 C 0.5394(9) 0.3662(8) 0.1501(7) 0.090(4) Uani 1 1 d U . . H63A H 0.5224 0.3574 0.1878 0.108 Uiso 1 1 calc R . . H63B H 0.4896 0.3449 0.1163 0.108 Uiso 1 1 calc R . . H63C H 0.5424 0.4179 0.1436 0.108 Uiso 1 1 calc R . . Cl1 Cl 0.2007(2) 0.21468(17) 0.10386(15) 0.0733(9) Uani 1 1 d D . . Cl2 Cl 0.2112(3) 0.06013(19) 0.13021(16) 0.0838(11) Uani 1 1 d D . . C64 C 0.1353(8) 0.1343(4) 0.1034(5) 0.060(3) Uani 1 1 d D . . H64A H 0.0954 0.1245 0.0617 0.072 Uiso 1 1 calc R . . H64B H 0.0902 0.1407 0.1288 0.072 Uiso 1 1 calc R . . Cl3 Cl 0.0823(4) 0.1922(3) 0.4781(3) 0.0598(15) Uani 0.50 1 d PD . . Cl4 Cl -0.0016(5) 0.0515(4) 0.4703(4) 0.096(2) Uani 0.50 1 d PD . . C65 C 0.0234(14) 0.1240(8) 0.4289(8) 0.068(7) Uani 0.50 1 d PD . . H65A H 0.0657 0.1081 0.4038 0.081 Uiso 0.50 1 calc PR . . H65B H -0.0383 0.1424 0.4016 0.081 Uiso 0.50 1 calc PR . . 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 0.0574(2) 0.0212(2) 0.0463(3) 0.00553(17) 0.03114(19) 0.00697(16) O1 0.054(4) 0.038(4) 0.047(5) 0.023(3) 0.026(3) 0.013(3) O2 0.099(6) 0.027(4) 0.055(5) 0.023(3) 0.038(4) 0.011(4) O3 0.056(4) 0.021(3) 0.074(5) 0.006(3) 0.043(4) 0.006(3) O4 0.049(4) 0.024(3) 0.050(4) 0.001(3) 0.031(3) 0.005(3) O5 0.061(4) 0.028(3) 0.058(5) 0.004(3) 0.041(4) 0.010(3) O6 0.059(4) 0.026(4) 0.062(5) 0.010(3) 0.038(4) 0.009(3) O7 0.076(5) 0.025(4) 0.083(6) 0.013(4) 0.060(4) 0.006(3) O8 0.098(5) 0.034(4) 0.077(6) 0.020(4) 0.066(5) 0.022(4) C1 0.052(6) 0.021(5) 0.047(7) 0.002(4) 0.021(5) 0.004(4) C2 0.057(6) 0.025(5) 0.037(6) 0.005(4) 0.031(5) 0.000(4) C3 0.069(7) 0.024(5) 0.051(7) 0.000(5) 0.035(6) 0.003(5) C4 0.071(7) 0.017(5) 0.050(7) -0.004(4) 0.023(6) 0.000(4) C5 0.065(7) 0.030(5) 0.047(7) 0.002(5) 0.024(6) 0.007(5) C6 0.047(5) 0.035(5) 0.044(7) 0.001(5) 0.015(5) -0.001(4) C7 0.046(5) 0.031(5) 0.038(6) 0.002(4) 0.021(5) -0.004(4) C8 0.054(6) 0.037(6) 0.047(8) -0.009(5) 0.023(5) -0.005(4) C9 0.130(12) 0.071(9) 0.059(10) -0.017(7) 0.042(9) -0.014(8) C10 0.197(19) 0.131(17) 0.057(11) -0.042(11) 0.044(11) -0.044(14) C11 0.112(12) 0.081(11) 0.119(16) -0.059(11) 0.040(11) -0.003(10) C12 0.056(7) 0.054(8) 0.105(12) -0.022(8) 0.024(8) -0.004(6) C13 0.046(5) 0.028(5) 0.067(8) -0.014(5) 0.017(5) 0.000(4) C14 0.072(7) 0.047(6) 0.027(7) -0.004(5) 0.015(6) 0.020(6) C15 0.063(7) 0.063(7) 0.031(7) -0.009(5) 0.013(6) 0.014(6) C16 0.083(9) 0.085(10) 0.057(10) -0.017(8) 0.026(8) 0.015(7) C17 0.087(10) 0.108(12) 0.044(9) -0.006(8) 0.006(7) 0.045(9) C18 0.149(14) 0.060(9) 0.050(10) 0.006(7) 0.015(9) 0.028(9) C19 0.116(11) 0.054(8) 0.040(8) 0.006(6) 0.005(8) 0.017(7) C20 0.057(6) 0.026(5) 0.051(7) 0.004(4) 0.034(5) 0.005(4) C21 0.048(6) 0.023(5) 0.082(9) 0.019(5) 0.032(6) 0.014(4) C22 0.052(6) 0.040(6) 0.064(8) 0.023(6) 0.036(6) 0.010(5) C23 0.063(7) 0.062(8) 0.089(10) 0.043(7) 0.039(7) 0.017(6) C24 0.065(8) 0.048(8) 0.133(14) 0.044(9) 0.033(8) 0.006(6) C25 0.062(7) 0.024(6) 0.127(13) 0.030(7) 0.022(8) 0.005(5) C26 0.050(6) 0.019(5) 0.110(11) 0.017(6) 0.034(7) 0.011(4) C27 0.042(6) 0.036(7) 0.089(10) -0.001(6) 0.018(6) 0.003(5) C28 0.047(6) 0.026(6) 0.129(13) -0.007(7) 0.006(8) 0.004(5) C29 0.065(8) 0.069(10) 0.124(15) -0.040(10) -0.012(9) 0.016(7) C30 0.077(8) 0.065(9) 0.079(10) -0.018(8) -0.001(7) 0.024(7) C31 0.065(7) 0.046(7) 0.078(11) -0.011(6) -0.007(7) 0.012(6) C32 0.060(7) 0.026(6) 0.071(10) 0.000(5) 0.018(6) 0.008(5) C33 0.061(6) 0.050(7) 0.064(8) 0.031(6) 0.047(6) 0.024(5) C34 0.056(7) 0.105(11) 0.035(8) 0.012(7) 0.015(6) 0.029(7) C35 0.064(8) 0.127(13) 0.044(9) 0.011(8) 0.028(7) 0.046(8) C36 0.101(11) 0.083(10) 0.053(9) -0.010(7) -0.003(8) 0.049(8) C37 0.063(7) 0.073(9) 0.052(8) -0.003(6) 0.021(6) 0.021(6) C38 0.065(7) 0.036(6) 0.051(7) 0.009(5) 0.036(6) 0.011(5) C39 0.121(10) 0.033(6) 0.087(10) 0.017(6) 0.084(9) 0.022(6) C40 0.130(7) 0.034(5) 0.161(9) 0.019(6) 0.098(6) 0.009(5) C41 0.102(6) 0.058(6) 0.178(9) 0.011(6) 0.080(6) -0.017(5) C42 0.113(7) 0.067(6) 0.178(10) 0.001(7) 0.081(7) -0.006(6) C43 0.124(8) 0.053(6) 0.176(10) 0.004(7) 0.080(7) 0.003(6) C44 0.102(7) 0.035(5) 0.175(9) 0.012(6) 0.087(6) 0.016(6) C45 0.133(7) 0.057(6) 0.163(8) 0.019(6) 0.083(6) 0.022(6) C46 0.112(7) 0.111(8) 0.204(10) 0.027(8) 0.064(7) -0.063(6) C47 0.127(8) 0.135(9) 0.205(12) 0.040(9) 0.055(9) -0.072(7) C48 0.138(9) 0.162(11) 0.226(12) 0.036(10) 0.045(10) -0.064(8) C49 0.148(10) 0.187(11) 0.235(12) 0.037(10) 0.050(10) -0.076(9) C50 0.128(9) 0.178(10) 0.225(12) 0.047(10) 0.057(9) -0.089(8) C51 0.112(8) 0.149(9) 0.210(11) 0.023(9) 0.073(8) -0.075(7) C52 0.141(8) 0.094(7) 0.135(8) 0.030(7) 0.093(7) 0.034(7) C53 0.168(10) 0.145(9) 0.161(10) 0.020(9) 0.077(8) 0.029(9) C54 0.185(11) 0.180(11) 0.176(11) 0.026(10) 0.055(10) 0.036(10) C55 0.187(11) 0.195(11) 0.181(11) 0.041(10) 0.048(10) 0.030(10) C56 0.185(11) 0.177(10) 0.163(11) 0.040(10) 0.050(9) 0.050(10) C57 0.171(10) 0.151(9) 0.144(10) 0.021(9) 0.066(8) 0.045(9) N1 0.074(6) 0.045(6) 0.063(7) 0.002(5) 0.028(5) 0.012(5) C58 0.163(12) 0.050(8) 0.114(11) -0.002(8) 0.074(10) -0.002(8) C59 0.121(10) 0.074(8) 0.082(10) 0.020(7) 0.059(8) 0.019(8) C60 0.087(8) 0.081(9) 0.090(10) 0.009(7) 0.055(7) 0.020(7) C61 0.076(8) 0.113(11) 0.082(10) 0.012(9) 0.020(8) 0.014(8) C62 0.064(7) 0.067(8) 0.090(10) 0.001(7) 0.022(7) 0.000(6) C63 0.065(7) 0.109(10) 0.099(11) -0.035(8) 0.026(7) 0.008(7) Cl1 0.0620(18) 0.074(2) 0.078(2) 0.0029(17) 0.0100(16) -0.0088(15) Cl2 0.108(2) 0.079(2) 0.079(2) 0.0173(19) 0.051(2) 0.043(2) C64 0.069(7) 0.057(7) 0.059(8) 0.003(6) 0.026(6) 0.005(6) Cl3 0.053(3) 0.063(4) 0.058(4) 0.007(3) 0.007(3) -0.006(3) Cl4 0.070(4) 0.086(5) 0.144(7) -0.011(5) 0.050(4) -0.020(4) C65 0.043(12) 0.12(2) 0.040(16) -0.022(14) 0.011(11) 0.015(13) _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 O2 1.724(8) . ? U1 O1 1.737(7) . ? U1 O3 2.444(6) . ? U1 O7 2.463(6) . ? U1 O6 2.464(6) . ? U1 O4 2.485(6) . ? U1 O8 2.499(6) . ? U1 O5 2.518(6) . ? U1 C1 2.840(8) . ? U1 C39 2.848(11) . ? U1 C20 2.877(9) . ? O3 C1 1.274(10) . ? O4 C1 1.260(10) . ? O5 C20 1.283(10) . ? O6 C20 1.255(10) . ? O7 C39 1.256(11) . ? O8 C39 1.259(12) . ? C1 C2 1.506(12) . ? C2 C7 1.396(13) . ? C2 C3 1.410(12) . ? C3 C4 1.408(13) . ? C3 C14 1.497(14) . ? C4 C5 1.377(14) . ? C5 C6 1.364(13) . ? C6 C7 1.408(13) . ? C7 C8 1.504(13) . ? C8 C9 1.348(15) . ? C8 C13 1.392(13) . ? C9 C10 1.414(18) . ? C10 C11 1.42(2) . ? C11 C12 1.35(2) . ? C12 C13 1.380(15) . ? C14 C15 1.413(15) . ? C14 C19 1.394(15) . ? C15 C16 1.384(17) . ? C16 C17 1.394(18) . ? C17 C18 1.377(19) . ? C18 C19 1.381(17) . ? C20 C21 1.483(12) . ? C21 C26 1.414(16) . ? C21 C22 1.412(16) . ? C22 C23 1.426(14) . ? C22 C33 1.456(15) . ? C23 C24 1.387(18) . ? C24 C25 1.384(18) . ? C25 C26 1.410(14) . ? C26 C27 1.474(16) . ? C27 C32 1.388(15) . ? C27 C28 1.438(16) . ? C28 C29 1.367(19) . ? C29 C30 1.335(18) . ? C30 C31 1.416(16) . ? C31 C32 1.348(16) . ? C33 C34 1.410(14) . ? C33 C38 1.385(13) . ? C34 C35 1.351(17) . ? C35 C36 1.367(19) . ? C36 C37 1.433(16) . ? C37 C38 1.378(15) . ? C39 C40 1.643(13) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C46 1.3614 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C52 1.4549 . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3899 . ? C56 C57 1.3900 . ? N1 C62 1.459(15) . ? N1 C60 1.503(15) . ? N1 C58 1.493(15) . ? C58 C59 1.556(17) . ? C60 C61 1.503(18) . ? C62 C63 1.479(16) . ? Cl1 C64 1.766(9) . ? Cl2 C64 1.762(9) . ? Cl3 C65 1.757(14) . ? Cl4 C65 1.751(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 O2 U1 O1 179.5(3) . . ? O2 U1 O3 90.8(3) . . ? O1 U1 O3 89.6(3) . . ? O2 U1 O7 92.5(3) . . ? O1 U1 O7 87.1(3) . . ? O3 U1 O7 173.2(2) . . ? O2 U1 O6 91.5(3) . . ? O1 U1 O6 88.9(3) . . ? O3 U1 O6 67.33(19) . . ? O7 U1 O6 118.56(19) . . ? O2 U1 O4 91.1(3) . . ? O1 U1 O4 88.9(2) . . ? O3 U1 O4 52.89(18) . . ? O7 U1 O4 120.99(18) . . ? O6 U1 O4 120.18(18) . . ? O2 U1 O8 88.5(3) . . ? O1 U1 O8 91.1(3) . . ? O3 U1 O8 121.9(2) . . ? O7 U1 O8 52.3(2) . . ? O6 U1 O8 170.8(2) . . ? O4 U1 O8 69.01(19) . . ? O2 U1 O5 87.4(3) . . ? O1 U1 O5 92.7(3) . . ? O3 U1 O5 119.37(19) . . ? O7 U1 O5 66.82(19) . . ? O6 U1 O5 52.18(18) . . ? O4 U1 O5 172.12(18) . . ? O8 U1 O5 118.64(19) . . ? O2 U1 C1 91.0(3) . . ? O1 U1 C1 89.2(3) . . ? O3 U1 C1 26.6(2) . . ? O7 U1 C1 147.2(2) . . ? O6 U1 C1 93.9(2) . . ? O4 U1 C1 26.3(2) . . ? O8 U1 C1 95.3(2) . . ? O5 U1 C1 145.9(2) . . ? O2 U1 C39 91.7(4) . . ? O1 U1 C39 87.8(4) . . ? O3 U1 C39 147.8(2) . . ? O7 U1 C39 26.1(2) . . ? O6 U1 C39 144.6(2) . . ? O4 U1 C39 94.9(2) . . ? O8 U1 C39 26.2(2) . . ? O5 U1 C39 92.8(2) . . ? C1 U1 C39 121.2(3) . . ? O2 U1 C20 89.7(3) . . ? O1 U1 C20 90.6(3) . . ? O3 U1 C20 93.0(2) . . ? O7 U1 C20 93.0(2) . . ? O6 U1 C20 25.7(2) . . ? O4 U1 C20 145.9(2) . . ? O8 U1 C20 145.1(2) . . ? O5 U1 C20 26.5(2) . . ? C1 U1 C20 119.6(3) . . ? C39 U1 C20 119.1(3) . . ? C1 O3 U1 94.3(5) . . ? C1 O4 U1 92.7(5) . . ? C20 O5 U1 92.5(5) . . ? C20 O6 U1 95.8(5) . . ? C39 O7 U1 94.3(6) . . ? C39 O8 U1 92.6(6) . . ? O4 C1 O3 120.1(8) . . ? O4 C1 C2 119.7(8) . . ? O3 C1 C2 120.2(8) . . ? O4 C1 U1 61.0(4) . . ? O3 C1 U1 59.1(4) . . ? C2 C1 U1 179.4(6) . . ? C7 C2 C3 120.7(8) . . ? C7 C2 C1 119.3(8) . . ? C3 C2 C1 119.5(9) . . ? C4 C3 C2 117.5(10) . . ? C4 C3 C14 119.9(9) . . ? C2 C3 C14 122.6(8) . . ? C5 C4 C3 121.7(9) . . ? C4 C5 C6 120.3(9) . . ? C5 C6 C7 120.6(10) . . ? C6 C7 C2 119.2(8) . . ? C6 C7 C8 118.3(9) . . ? C2 C7 C8 122.5(8) . . ? C9 C8 C13 120.0(10) . . ? C9 C8 C7 119.5(10) . . ? C13 C8 C7 120.4(9) . . ? C8 C9 C10 120.5(14) . . ? C11 C10 C9 117.2(15) . . ? C12 C11 C10 122.1(14) . . ? C11 C12 C13 118.4(14) . . ? C12 C13 C8 121.6(12) . . ? C15 C14 C19 118.9(11) . . ? C15 C14 C3 119.7(9) . . ? C19 C14 C3 121.3(11) . . ? C14 C15 C16 119.1(11) . . ? C15 C16 C17 120.6(13) . . ? C18 C17 C16 120.5(13) . . ? C17 C18 C19 119.3(13) . . ? C14 C19 C18 121.5(13) . . ? O6 C20 O5 119.4(8) . . ? O6 C20 C21 121.4(8) . . ? O5 C20 C21 119.1(8) . . ? O6 C20 U1 58.5(4) . . ? O5 C20 U1 61.0(4) . . ? C21 C20 U1 178.3(8) . . ? C26 C21 C22 122.5(9) . . ? C26 C21 C20 121.1(10) . . ? C22 C21 C20 116.5(10) . . ? C23 C22 C21 116.2(11) . . ? C23 C22 C33 120.5(11) . . ? C21 C22 C33 123.3(9) . . ? C24 C23 C22 122.1(12) . . ? C25 C24 C23 120.2(11) . . ? C24 C25 C26 120.8(13) . . ? C21 C26 C25 118.2(13) . . ? C21 C26 C27 123.1(9) . . ? C25 C26 C27 118.6(12) . . ? C32 C27 C28 115.7(12) . . ? C32 C27 C26 123.0(10) . . ? C28 C27 C26 121.2(11) . . ? C29 C28 C27 121.0(12) . . ? C30 C29 C28 121.4(13) . . ? C29 C30 C31 119.3(14) . . ? C32 C31 C30 120.1(12) . . ? C31 C32 C27 122.5(11) . . ? C34 C33 C38 117.8(12) . . ? C34 C33 C22 119.6(10) . . ? C38 C33 C22 122.6(9) . . ? C35 C34 C33 122.4(12) . . ? C34 C35 C36 119.2(11) . . ? C35 C36 C37 121.2(13) . . ? C38 C37 C36 117.7(12) . . ? C37 C38 C33 121.7(10) . . ? O8 C39 O7 120.7(10) . . ? O8 C39 C40 121.6(8) . . ? O7 C39 C40 117.1(9) . . ? O8 C39 U1 61.2(5) . . ? O7 C39 U1 59.6(5) . . ? C40 C39 U1 167.3(8) . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 119.2(5) . . ? C45 C40 C39 120.8(5) . . ? C46 C41 C42 111.1 . . ? C46 C41 C40 128.6 . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 C52 124.0 . . ? C40 C45 C52 116.0 . . ? C41 C46 C47 120.6 . . ? C41 C46 C51 119.3 . . ? C47 C46 C51 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C49 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C51 120.0 . . ? C50 C51 C46 120.0 . . ? C53 C52 C57 120.0 . . ? C53 C52 C45 114.8 . . ? C57 C52 C45 125.1 . . ? C52 C53 C54 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C57 120.0 . . ? C56 C57 C52 120.0 . . ? C62 N1 C60 112.9(10) . . ? C62 N1 C58 115.1(11) . . ? C60 N1 C58 108.9(10) . . ? N1 C58 C59 108.4(11) . . ? N1 C60 C61 114.1(11) . . ? C63 C62 N1 115.3(11) . . ? Cl1 C64 Cl2 113.4(6) . . ? Cl3 C65 Cl4 110.1(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 U1 O3 C1 90.6(6) . . . . ? O1 U1 O3 C1 -89.1(6) . . . . ? O7 U1 O3 C1 -28(2) . . . . ? O6 U1 O3 C1 -178.1(6) . . . . ? O4 U1 O3 C1 -0.2(5) . . . . ? O8 U1 O3 C1 1.9(7) . . . . ? O5 U1 O3 C1 178.0(5) . . . . ? C39 U1 O3 C1 -3.9(9) . . . . ? C20 U1 O3 C1 -179.7(6) . . . . ? O2 U1 O4 C1 -89.9(6) . . . . ? O1 U1 O4 C1 90.5(6) . . . . ? O3 U1 O4 C1 0.2(5) . . . . ? O7 U1 O4 C1 176.5(5) . . . . ? O6 U1 O4 C1 2.5(6) . . . . ? O8 U1 O4 C1 -177.9(6) . . . . ? O5 U1 O4 C1 -11.2(18) . . . . ? C39 U1 O4 C1 178.3(6) . . . . ? C20 U1 O4 C1 1.1(8) . . . . ? O2 U1 O5 C20 94.5(6) . . . . ? O1 U1 O5 C20 -85.9(6) . . . . ? O3 U1 O5 C20 5.1(7) . . . . ? O7 U1 O5 C20 -171.6(6) . . . . ? O6 U1 O5 C20 0.6(6) . . . . ? O4 U1 O5 C20 15.6(18) . . . . ? O8 U1 O5 C20 -178.6(6) . . . . ? C1 U1 O5 C20 6.7(8) . . . . ? C39 U1 O5 C20 -173.9(6) . . . . ? O2 U1 O6 C20 -86.1(6) . . . . ? O1 U1 O6 C20 93.7(6) . . . . ? O3 U1 O6 C20 -176.3(7) . . . . ? O7 U1 O6 C20 7.6(7) . . . . ? O4 U1 O6 C20 -178.2(6) . . . . ? O8 U1 O6 C20 3.8(18) . . . . ? O5 U1 O6 C20 -0.6(6) . . . . ? C1 U1 O6 C20 -177.1(6) . . . . ? C39 U1 O6 C20 9.0(9) . . . . ? O2 U1 O7 C39 -88.8(8) . . . . ? O1 U1 O7 C39 90.9(8) . . . . ? O3 U1 O7 C39 30(2) . . . . ? O6 U1 O7 C39 178.1(7) . . . . ? O4 U1 O7 C39 4.0(9) . . . . ? O8 U1 O7 C39 -2.7(7) . . . . ? O5 U1 O7 C39 -174.9(8) . . . . ? C1 U1 O7 C39 6.8(10) . . . . ? C20 U1 O7 C39 -178.6(8) . . . . ? O2 U1 O8 C39 97.0(8) . . . . ? O1 U1 O8 C39 -82.9(8) . . . . ? O3 U1 O8 C39 -173.0(7) . . . . ? O7 U1 O8 C39 2.7(7) . . . . ? O6 U1 O8 C39 7(2) . . . . ? O4 U1 O8 C39 -171.3(8) . . . . ? O5 U1 O8 C39 10.8(8) . . . . ? C1 U1 O8 C39 -172.2(8) . . . . ? C20 U1 O8 C39 9.8(10) . . . . ? U1 O4 C1 O3 -0.4(10) . . . . ? U1 O4 C1 C2 -179.9(8) . . . . ? U1 O3 C1 O4 0.4(10) . . . . ? U1 O3 C1 C2 179.9(8) . . . . ? O2 U1 C1 O4 90.5(6) . . . . ? O1 U1 C1 O4 -89.0(6) . . . . ? O3 U1 C1 O4 -179.6(10) . . . . ? O7 U1 C1 O4 -5.5(9) . . . . ? O6 U1 C1 O4 -177.9(5) . . . . ? O8 U1 C1 O4 2.0(6) . . . . ? O5 U1 C1 O4 177.3(4) . . . . ? C39 U1 C1 O4 -2.0(7) . . . . ? C20 U1 C1 O4 -179.3(5) . . . . ? O2 U1 C1 O3 -89.9(6) . . . . ? O1 U1 C1 O3 90.6(6) . . . . ? O7 U1 C1 O3 174.1(5) . . . . ? O6 U1 C1 O3 1.7(6) . . . . ? O4 U1 C1 O3 179.6(10) . . . . ? O8 U1 C1 O3 -178.4(6) . . . . ? O5 U1 C1 O3 -3.1(8) . . . . ? C39 U1 C1 O3 177.6(6) . . . . ? C20 U1 C1 O3 0.3(7) . . . . ? O2 U1 C1 C2 -97(80) . . . . ? O1 U1 C1 C2 83(80) . . . . ? O3 U1 C1 C2 -7(79) . . . . ? O7 U1 C1 C2 167(100) . . . . ? O6 U1 C1 C2 -6(80) . . . . ? O4 U1 C1 C2 172(100) . . . . ? O8 U1 C1 C2 174(100) . . . . ? O5 U1 C1 C2 -11(80) . . . . ? C39 U1 C1 C2 170(100) . . . . ? C20 U1 C1 C2 -7(80) . . . . ? O4 C1 C2 C7 -94.6(11) . . . . ? O3 C1 C2 C7 85.9(11) . . . . ? U1 C1 C2 C7 93(80) . . . . ? O4 C1 C2 C3 77.5(12) . . . . ? O3 C1 C2 C3 -101.9(11) . . . . ? U1 C1 C2 C3 -95(80) . . . . ? C7 C2 C3 C4 0.1(13) . . . . ? C1 C2 C3 C4 -171.9(8) . . . . ? C7 C2 C3 C14 -177.4(8) . . . . ? C1 C2 C3 C14 10.5(13) . . . . ? C2 C3 C4 C5 1.1(14) . . . . ? C14 C3 C4 C5 178.7(9) . . . . ? C3 C4 C5 C6 -0.8(15) . . . . ? C4 C5 C6 C7 -0.7(14) . . . . ? C5 C6 C7 C2 1.8(13) . . . . ? C5 C6 C7 C8 -179.6(8) . . . . ? C3 C2 C7 C6 -1.5(12) . . . . ? C1 C2 C7 C6 170.5(8) . . . . ? C3 C2 C7 C8 180.0(8) . . . . ? C1 C2 C7 C8 -8.0(12) . . . . ? C6 C7 C8 C9 -51.5(13) . . . . ? C2 C7 C8 C9 127.0(11) . . . . ? C6 C7 C8 C13 126.4(10) . . . . ? C2 C7 C8 C13 -55.1(12) . . . . ? C13 C8 C9 C10 -2(2) . . . . ? C7 C8 C9 C10 175.5(13) . . . . ? C8 C9 C10 C11 2(2) . . . . ? C9 C10 C11 C12 1(3) . . . . ? C10 C11 C12 C13 -3(2) . . . . ? C11 C12 C13 C8 2.7(17) . . . . ? C9 C8 C13 C12 0.2(16) . . . . ? C7 C8 C13 C12 -177.7(9) . . . . ? C4 C3 C14 C15 46.5(13) . . . . ? C2 C3 C14 C15 -136.0(10) . . . . ? C4 C3 C14 C19 -132.1(11) . . . . ? C2 C3 C14 C19 45.4(14) . . . . ? C19 C14 C15 C16 1.4(15) . . . . ? C3 C14 C15 C16 -177.2(9) . . . . ? C14 C15 C16 C17 -2.4(16) . . . . ? C15 C16 C17 C18 2.3(19) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C15 C14 C19 C18 -0.3(18) . . . . ? C3 C14 C19 C18 178.3(11) . . . . ? C17 C18 C19 C14 0(2) . . . . ? U1 O6 C20 O5 1.0(10) . . . . ? U1 O6 C20 C21 178.0(9) . . . . ? U1 O5 C20 O6 -1.0(10) . . . . ? U1 O5 C20 C21 -178.0(9) . . . . ? O2 U1 C20 O6 94.2(6) . . . . ? O1 U1 C20 O6 -86.2(6) . . . . ? O3 U1 C20 O6 3.4(6) . . . . ? O7 U1 C20 O6 -173.3(6) . . . . ? O4 U1 C20 O6 2.7(9) . . . . ? O8 U1 C20 O6 -179.0(5) . . . . ? O5 U1 C20 O6 179.0(10) . . . . ? C1 U1 C20 O6 3.3(7) . . . . ? C39 U1 C20 O6 -174.0(6) . . . . ? O2 U1 C20 O5 -84.8(6) . . . . ? O1 U1 C20 O5 94.9(6) . . . . ? O3 U1 C20 O5 -175.5(6) . . . . ? O7 U1 C20 O5 7.7(6) . . . . ? O6 U1 C20 O5 -179.0(10) . . . . ? O4 U1 C20 O5 -176.2(4) . . . . ? O8 U1 C20 O5 2.1(9) . . . . ? C1 U1 C20 O5 -175.7(5) . . . . ? C39 U1 C20 O5 7.0(7) . . . . ? O2 U1 C20 C21 9(21) . . . . ? O1 U1 C20 C21 -172(21) . . . . ? O3 U1 C20 C21 -82(21) . . . . ? O7 U1 C20 C21 101(21) . . . . ? O6 U1 C20 C21 -85(21) . . . . ? O4 U1 C20 C21 -83(21) . . . . ? O8 U1 C20 C21 96(21) . . . . ? O5 U1 C20 C21 94(21) . . . . ? C1 U1 C20 C21 -82(21) . . . . ? C39 U1 C20 C21 101(21) . . . . ? O6 C20 C21 C26 -105.7(11) . . . . ? O5 C20 C21 C26 71.3(13) . . . . ? U1 C20 C21 C26 -21(22) . . . . ? O6 C20 C21 C22 73.6(13) . . . . ? O5 C20 C21 C22 -109.4(11) . . . . ? U1 C20 C21 C22 158(21) . . . . ? C26 C21 C22 C23 -2.8(14) . . . . ? C20 C21 C22 C23 177.9(8) . . . . ? C26 C21 C22 C33 178.0(9) . . . . ? C20 C21 C22 C33 -1.3(13) . . . . ? C21 C22 C23 C24 1.8(15) . . . . ? C33 C22 C23 C24 -178.9(10) . . . . ? C22 C23 C24 C25 -0.2(17) . . . . ? C23 C24 C25 C26 -0.6(17) . . . . ? C22 C21 C26 C25 2.1(14) . . . . ? C20 C21 C26 C25 -178.7(9) . . . . ? C22 C21 C26 C27 -174.2(9) . . . . ? C20 C21 C26 C27 5.1(14) . . . . ? C24 C25 C26 C21 -0.3(15) . . . . ? C24 C25 C26 C27 176.1(10) . . . . ? C21 C26 C27 C32 41.2(15) . . . . ? C25 C26 C27 C32 -135.0(11) . . . . ? C21 C26 C27 C28 -141.6(10) . . . . ? C25 C26 C27 C28 42.2(14) . . . . ? C32 C27 C28 C29 -0.6(16) . . . . ? C26 C27 C28 C29 -178.1(11) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C28 C29 C30 C31 2(2) . . . . ? C29 C30 C31 C32 -2(2) . . . . ? C30 C31 C32 C27 0.2(18) . . . . ? C28 C27 C32 C31 0.9(16) . . . . ? C26 C27 C32 C31 178.2(10) . . . . ? C23 C22 C33 C34 50.6(14) . . . . ? C21 C22 C33 C34 -130.2(10) . . . . ? C23 C22 C33 C38 -131.7(10) . . . . ? C21 C22 C33 C38 47.4(14) . . . . ? C38 C33 C34 C35 2.6(16) . . . . ? C22 C33 C34 C35 -179.6(11) . . . . ? C33 C34 C35 C36 -2.9(19) . . . . ? C34 C35 C36 C37 1.9(19) . . . . ? C35 C36 C37 C38 -0.8(18) . . . . ? C36 C37 C38 C33 0.6(16) . . . . ? C34 C33 C38 C37 -1.5(15) . . . . ? C22 C33 C38 C37 -179.2(10) . . . . ? U1 O8 C39 O7 -4.8(13) . . . . ? U1 O8 C39 C40 165.6(9) . . . . ? U1 O7 C39 O8 4.9(13) . . . . ? U1 O7 C39 C40 -165.9(8) . . . . ? O2 U1 C39 O8 -83.1(7) . . . . ? O1 U1 C39 O8 96.9(7) . . . . ? O3 U1 C39 O8 11.1(12) . . . . ? O7 U1 C39 O8 -175.2(13) . . . . ? O6 U1 C39 O8 -178.1(5) . . . . ? O4 U1 C39 O8 8.2(8) . . . . ? O5 U1 C39 O8 -170.5(7) . . . . ? C1 U1 C39 O8 9.1(9) . . . . ? C20 U1 C39 O8 -173.6(6) . . . . ? O2 U1 C39 O7 92.1(8) . . . . ? O1 U1 C39 O7 -87.9(8) . . . . ? O3 U1 C39 O7 -173.6(5) . . . . ? O6 U1 C39 O7 -2.9(11) . . . . ? O4 U1 C39 O7 -176.6(7) . . . . ? O8 U1 C39 O7 175.2(13) . . . . ? O5 U1 C39 O7 4.7(8) . . . . ? C1 U1 C39 O7 -175.7(6) . . . . ? C20 U1 C39 O7 1.6(9) . . . . ? O2 U1 C39 C40 171(3) . . . . ? O1 U1 C39 C40 -9(3) . . . . ? O3 U1 C39 C40 -95(3) . . . . ? O7 U1 C39 C40 79(3) . . . . ? O6 U1 C39 C40 76(3) . . . . ? O4 U1 C39 C40 -98(3) . . . . ? O8 U1 C39 C40 -106(3) . . . . ? O5 U1 C39 C40 83(3) . . . . ? C1 U1 C39 C40 -97(3) . . . . ? C20 U1 C39 C40 80(3) . . . . ? O8 C39 C40 C41 -104.1(11) . . . . ? O7 C39 C40 C41 66.6(11) . . . . ? U1 C39 C40 C41 -5(3) . . . . ? O8 C39 C40 C45 78.5(12) . . . . ? O7 C39 C40 C45 -110.8(10) . . . . ? U1 C39 C40 C45 177(2) . . . . ? C45 C40 C41 C46 -173.4 . . . . ? C39 C40 C41 C46 9.2(5) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C39 C40 C41 C42 -177.4(5) . . . . ? C46 C41 C42 C43 174.5 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C43 C44 C45 C52 178.3 . . . . ? C41 C40 C45 C44 0.0 . . . . ? C39 C40 C45 C44 177.4(5) . . . . ? C41 C40 C45 C52 -178.4 . . . . ? C39 C40 C45 C52 -1.0(5) . . . . ? C42 C41 C46 C47 41.7 . . . . ? C40 C41 C46 C47 -144.4 . . . . ? C42 C41 C46 C51 -134.7 . . . . ? C40 C41 C46 C51 39.1 . . . . ? C41 C46 C47 C48 -176.4 . . . . ? C51 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C46 0.0 . . . . ? C41 C46 C51 C50 176.5 . . . . ? C47 C46 C51 C50 0.0 . . . . ? C44 C45 C52 C53 33.9 . . . . ? C40 C45 C52 C53 -147.8 . . . . ? C44 C45 C52 C57 -141.8 . . . . ? C40 C45 C52 C57 36.6 . . . . ? C57 C52 C53 C54 0.0 . . . . ? C45 C52 C53 C54 -175.9 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C52 0.0 . . . . ? C53 C52 C57 C56 0.0 . . . . ? C45 C52 C57 C56 175.4 . . . . ? C62 N1 C58 C59 -56.2(15) . . . . ? C60 N1 C58 C59 175.9(11) . . . . ? C62 N1 C60 C61 160.0(11) . . . . ? C58 N1 C60 C61 -70.9(15) . . . . ? C60 N1 C62 C63 60.7(15) . . . . ? C58 N1 C62 C63 -65.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.645 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.146 # Attachment '760898.cif.txt' data_sbee _database_code_depnum_ccdc_archive 'CCDC 760898' #TrackingRef '760898.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H86 N2 O18 U' _chemical_formula_weight 1517.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 18.534(4) _cell_length_b 19.636(4) _cell_length_c 19.425(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.62(3) _cell_angle_gamma 90.00 _cell_volume 7007(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8830 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.1 _exptl_crystal_description Parallalepiped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 2.387 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5650 _exptl_absorpt_correction_T_max 0.7160 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 25087 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12156 _reflns_number_gt 9066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The systematic absences (hkl, h+k=2n+1; h0l, l=2n+1) indicated a choice between the space groups Cc and C2/c. The former space group was chosen based on the fact that Z=4 and the compound cannot exhibit a two-fold or center of inversion local symmetry. 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. The thermal paprameters of carbon atoms were restrained to avoid excesive ADP max/min ratio. The large residual factors are the result of disorderd water solvent molecules, the model for which could not be improved despite best efforts. This disorder also leaves solvent accessible voids in the structure. The program SQUEEZE however was not used. ; _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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 0.498(9) _refine_ls_number_reflns 12156 _refine_ls_number_parameters 864 _refine_ls_number_restraints 445 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.128 _refine_ls_shift/su_mean 0.045 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 0.60834(6) 0.701034(12) 0.54475(6) 0.04129(7) Uani 1 1 d . . . O1 O 0.6371(3) 0.7026(3) 0.4717(5) 0.063(2) Uani 1 1 d . . . O2 O 0.5794(4) 0.6996(4) 0.6302(3) 0.049(2) Uani 1 1 d . . . O3 O 0.5389(3) 0.5955(4) 0.5035(4) 0.058(2) Uani 1 1 d . . . O4 O 0.4740(4) 0.6916(3) 0.4994(4) 0.047(2) Uani 1 1 d . . . O5 O 0.6666(5) 0.8162(3) 0.5686(5) 0.063(3) Uani 1 1 d . . . O6 O 0.5526(3) 0.8102(3) 0.5214(4) 0.041(2) Uani 1 1 d . . . O7 O 0.6749(4) 0.5987(4) 0.5765(4) 0.048(2) Uani 1 1 d . . . O8 O 0.7425(4) 0.6839(4) 0.5932(4) 0.056(3) Uani 1 1 d . . . O9 O 0.6045(8) 0.6183(7) 0.2123(8) 0.162(6) Uani 1 1 d . . . H9 H 0.5762 0.6224 0.1763 0.194 Uiso 1 1 calc R . . O10 O 0.3821(6) 0.6742(7) 0.7844(6) 0.134(4) Uani 1 1 d . . . H10 H 0.4180 0.6990 0.7894 0.160 Uiso 1 1 calc R . . O11 O 0.6054(5) 0.8251(5) 0.8719(4) 0.074(3) Uani 1 1 d . . . H11 H 0.5798 0.7909 0.8677 0.089 Uiso 1 1 calc R . . O12 O 0.6052(7) 0.8427(6) 0.2241(6) 0.102(4) Uani 1 1 d . . . H12 H 0.6270 0.8062 0.2266 0.123 Uiso 1 1 calc R . . O13 O 0.8774(5) 0.6543(6) 0.3162(5) 0.118(4) Uani 1 1 d . . . H13 H 0.8717 0.6237 0.2872 0.141 Uiso 1 1 calc R . . O14 O 0.5965(8) 0.6098(6) 0.8798(6) 0.127(4) Uani 1 1 d . . . H14 H 0.6046 0.5932 0.9188 0.153 Uiso 1 1 calc R . . N1 N 0.3594(4) 0.8027(4) 0.4878(5) 0.059(3) Uani 1 1 d . . . N2 N 0.8489(8) 0.8038(6) 0.6047(7) 0.094(5) Uani 1 1 d . . . H2 H 0.8120 0.7743 0.6090 0.113 Uiso 1 1 calc R . . C1 C 0.4779(6) 0.6283(6) 0.4935(6) 0.057(3) Uani 1 1 d U . . C2 C 0.4160(6) 0.5790(6) 0.4656(6) 0.056(2) Uani 1 1 d U . . C3 C 0.4115(6) 0.5541(6) 0.4027(6) 0.064(2) Uani 1 1 d U . . C4 C 0.3471(6) 0.5164(6) 0.3797(7) 0.075(3) Uani 1 1 d U . . H4 H 0.3389 0.5033 0.3333 0.090 Uiso 1 1 calc R . . C5 C 0.2962(6) 0.4982(6) 0.4222(6) 0.070(3) Uani 1 1 d U . . H5 H 0.2571 0.4702 0.4060 0.084 Uiso 1 1 calc R . . C6 C 0.3046(5) 0.5219(6) 0.4871(6) 0.062(2) Uani 1 1 d U . . H6 H 0.2714 0.5094 0.5169 0.074 Uiso 1 1 calc R . . C7 C 0.3597(6) 0.5631(6) 0.5100(6) 0.061(2) Uani 1 1 d U . . C8 C 0.4648(8) 0.5723(7) 0.3540(7) 0.074(2) Uani 1 1 d U . . C9 C 0.4951(7) 0.6397(6) 0.3489(6) 0.069(3) Uani 1 1 d U . . H9A H 0.4819 0.6758 0.3755 0.082 Uiso 1 1 calc R . . C10 C 0.5449(8) 0.6474(7) 0.3022(6) 0.076(3) Uani 1 1 d U . . H10A H 0.5638 0.6909 0.2980 0.092 Uiso 1 1 calc R . . C11 C 0.5686(8) 0.5986(7) 0.2625(7) 0.085(3) Uani 1 1 d U . . C12 C 0.5459(8) 0.5348(7) 0.2657(6) 0.089(3) Uani 1 1 d U . . H12A H 0.5647 0.5009 0.2399 0.107 Uiso 1 1 calc R . . C13 C 0.4929(8) 0.5193(7) 0.3087(7) 0.086(3) Uani 1 1 d U . . H13A H 0.4747 0.4752 0.3090 0.103 Uiso 1 1 calc R . . C14 C 0.3669(6) 0.5949(6) 0.5808(7) 0.064(2) Uani 1 1 d U . . C15 C 0.3019(6) 0.6149(6) 0.6101(7) 0.077(3) Uani 1 1 d U . . H15 H 0.2562 0.6119 0.5838 0.093 Uiso 1 1 calc R . . C16 C 0.3087(7) 0.6367(7) 0.6727(8) 0.088(3) Uani 1 1 d U . . H16 H 0.2658 0.6472 0.6902 0.106 Uiso 1 1 calc R . . C17 C 0.3733(7) 0.6466(7) 0.7178(7) 0.083(3) Uani 1 1 d U . . C18 C 0.4371(7) 0.6247(6) 0.6945(6) 0.078(3) Uani 1 1 d U . . H18 H 0.4820 0.6290 0.7218 0.094 Uiso 1 1 calc R . . C19 C 0.4303(7) 0.5944(6) 0.6243(6) 0.066(3) Uani 1 1 d U . . H19 H 0.4710 0.5742 0.6095 0.079 Uiso 1 1 calc R . . C20 C 0.6112(10) 0.8456(3) 0.5480(10) 0.0448(17) Uani 1 1 d U . . C21 C 0.6131(7) 0.9223(3) 0.5529(7) 0.0481(17) Uani 1 1 d U . . C22 C 0.6096(5) 0.9576(6) 0.6122(6) 0.055(2) Uani 1 1 d U . . C23 C 0.6129(6) 1.0269(6) 0.6120(7) 0.063(2) Uani 1 1 d U . . H23 H 0.6191 1.0495 0.6544 0.076 Uiso 1 1 calc R . . C24 C 0.6081(8) 1.0618(4) 0.5575(7) 0.068(2) Uani 1 1 d U . . H24 H 0.6061 1.1090 0.5608 0.081 Uiso 1 1 calc R . . C25 C 0.6055(7) 1.0310(7) 0.4901(8) 0.071(3) Uani 1 1 d U . . H25 H 0.6065 1.0578 0.4508 0.086 Uiso 1 1 calc R . . C26 C 0.6014(7) 0.9578(6) 0.4845(6) 0.061(2) Uani 1 1 d DU . . C27 C 0.6125(6) 0.9237(6) 0.6758(7) 0.061(2) Uani 1 1 d U . . C28 C 0.5649(6) 0.8669(6) 0.6856(7) 0.064(3) Uani 1 1 d U . . H28 H 0.5314 0.8529 0.6484 0.077 Uiso 1 1 calc R . . C29 C 0.5671(7) 0.8353(7) 0.7440(7) 0.073(3) Uani 1 1 d U . . H29 H 0.5388 0.7963 0.7455 0.087 Uiso 1 1 calc R . . C30 C 0.6085(7) 0.8556(6) 0.8033(7) 0.072(3) Uani 1 1 d U . . C31 C 0.6557(7) 0.9091(7) 0.8025(7) 0.078(3) Uani 1 1 d U . . H31 H 0.6847 0.9239 0.8425 0.093 Uiso 1 1 calc R . . C32 C 0.6580(7) 0.9438(7) 0.7305(7) 0.074(3) Uani 1 1 d U . . H32 H 0.6913 0.9784 0.7260 0.089 Uiso 1 1 calc R . . C33 C 0.6030(7) 0.9202(7) 0.4143(6) 0.064(2) Uani 1 1 d DU . . C34 C 0.5601(7) 0.9420(7) 0.3486(7) 0.074(3) Uani 1 1 d U . . H34 H 0.5297 0.9796 0.3498 0.088 Uiso 1 1 calc R . . C35 C 0.5617(8) 0.9149(8) 0.2944(8) 0.075(3) Uani 1 1 d U . . H35 H 0.5289 0.9293 0.2568 0.090 Uiso 1 1 calc R . . C36 C 0.6058(8) 0.8670(7) 0.2842(7) 0.071(3) Uani 1 1 d U . . C37 C 0.6565(8) 0.8392(8) 0.3406(7) 0.069(3) Uani 1 1 d U . . H37 H 0.6906 0.8056 0.3349 0.083 Uiso 1 1 calc R . . C38 C 0.6475(7) 0.8700(7) 0.4068(7) 0.066(3) Uani 1 1 d U . . H38 H 0.6751 0.8529 0.4465 0.079 Uiso 1 1 calc R . . C39 C 0.7340(6) 0.6218(5) 0.5995(6) 0.045(3) Uani 1 1 d U . . C40 C 0.8005(6) 0.5822(6) 0.6295(7) 0.054(2) Uani 1 1 d U . . C41 C 0.8486(6) 0.5644(6) 0.5883(7) 0.062(2) Uani 1 1 d U . . C42 C 0.9062(7) 0.5181(7) 0.6218(7) 0.074(3) Uani 1 1 d U . . H42 H 0.9437 0.5056 0.5970 0.089 Uiso 1 1 calc R . . C43 C 0.9066(7) 0.4928(6) 0.6886(7) 0.072(3) Uani 1 1 d U . . H43 H 0.9429 0.4624 0.7064 0.086 Uiso 1 1 calc R . . C44 C 0.8588(7) 0.5100(6) 0.7256(7) 0.067(3) Uani 1 1 d U . . H44 H 0.8596 0.4913 0.7697 0.081 Uiso 1 1 calc R . . C45 C 0.8040(6) 0.5574(6) 0.7007(6) 0.054(2) Uani 1 1 d U . . C46 C 0.8537(7) 0.5841(6) 0.5152(8) 0.067(2) Uani 1 1 d U . . C47 C 0.9200(7) 0.5976(6) 0.4967(8) 0.082(3) Uani 1 1 d U . . H47 H 0.9609 0.5917 0.5295 0.099 Uiso 1 1 calc R . . C48 C 0.9297(7) 0.6203(6) 0.4295(8) 0.085(3) Uani 1 1 d U . . H48 H 0.9760 0.6298 0.4186 0.102 Uiso 1 1 calc R . . C49 C 0.8701(7) 0.6282(6) 0.3809(8) 0.080(3) Uani 1 1 d U . . C50 C 0.8009(6) 0.6126(6) 0.3995(7) 0.073(3) Uani 1 1 d U . . H50 H 0.7604 0.6154 0.3657 0.088 Uiso 1 1 calc R . . C51 C 0.7917(8) 0.5948(7) 0.4614(8) 0.069(3) Uani 1 1 d U . . H51 H 0.7447 0.5886 0.4722 0.083 Uiso 1 1 calc R . . C52 C 0.7502(7) 0.5724(6) 0.7460(6) 0.060(2) Uani 1 1 d U . . C53 C 0.7209(7) 0.6344(6) 0.7519(6) 0.063(3) Uani 1 1 d U . . H53 H 0.7331 0.6681 0.7218 0.075 Uiso 1 1 calc R . . C54 C 0.6754(8) 0.6522(7) 0.7975(7) 0.074(3) Uani 1 1 d U . . H54 H 0.6551 0.6954 0.7985 0.089 Uiso 1 1 calc R . . C55 C 0.6612(9) 0.6007(8) 0.8431(7) 0.085(3) Uani 1 1 d U . . C56 C 0.6930(8) 0.5366(7) 0.8397(7) 0.085(3) Uani 1 1 d U . . H56 H 0.6840 0.5023 0.8704 0.102 Uiso 1 1 calc R . . C57 C 0.7371(7) 0.5252(7) 0.7906(7) 0.076(3) Uani 1 1 d U . . H57 H 0.7589 0.4827 0.7885 0.091 Uiso 1 1 calc R . . C58 C 0.3655(6) 0.8394(8) 0.5615(8) 0.093(4) Uani 1 1 d DU . . H58 H 0.4020 0.8754 0.5605 0.111 Uiso 1 1 calc R . . C59 C 0.3979(8) 0.7882(7) 0.6219(8) 0.091(5) Uani 1 1 d U . . H59A H 0.4169 0.8137 0.6624 0.110 Uiso 1 1 calc R . . H59B H 0.4363 0.7617 0.6064 0.110 Uiso 1 1 calc R . . H59C H 0.3601 0.7584 0.6330 0.110 Uiso 1 1 calc R . . C60 C 0.2915(8) 0.8762(8) 0.5594(9) 0.148(6) Uani 1 1 d DU . . H60A H 0.2574 0.8573 0.5229 0.178 Uiso 1 1 calc R . . H60B H 0.2978 0.9239 0.5510 0.178 Uiso 1 1 calc R . . H60C H 0.2734 0.8703 0.6031 0.178 Uiso 1 1 calc R . . C61 C 0.3830(10) 0.8494(7) 0.4293(9) 0.135(5) Uani 1 1 d DU . . H61 H 0.3363 0.8495 0.3989 0.163 Uiso 1 1 calc R . . C62 C 0.4309(10) 0.8248(9) 0.3743(10) 0.140(7) Uani 1 1 d DU . . H62A H 0.4230 0.8538 0.3343 0.167 Uiso 1 1 calc R . . H62B H 0.4180 0.7789 0.3610 0.167 Uiso 1 1 calc R . . H62C H 0.4813 0.8266 0.3938 0.167 Uiso 1 1 calc R . . C64 C 0.2931(11) 0.7562(8) 0.4923(10) 0.159(6) Uani 1 1 d U . . H64A H 0.3038 0.7263 0.5320 0.190 Uiso 1 1 calc R . . H64B H 0.2518 0.7842 0.4998 0.190 Uiso 1 1 calc R . . C63 C 0.3927(10) 0.9254(7) 0.4342(9) 0.123(6) Uani 1 1 d DU . . H63A H 0.4417 0.9357 0.4538 0.147 Uiso 1 1 calc R . . H63B H 0.3595 0.9439 0.4634 0.147 Uiso 1 1 calc R . . H63C H 0.3829 0.9450 0.3887 0.147 Uiso 1 1 calc R . . C65 C 0.2738(12) 0.7154(8) 0.4306(11) 0.169(7) Uani 1 1 d U . . H65A H 0.2996 0.7317 0.3941 0.203 Uiso 1 1 calc R . . H65B H 0.2224 0.7186 0.4161 0.203 Uiso 1 1 calc R . . H65C H 0.2867 0.6688 0.4406 0.203 Uiso 1 1 calc R . . C66 C 0.8599(7) 0.8487(6) 0.6680(6) 0.078(3) Uani 1 1 d U . . H66 H 0.9104 0.8426 0.6896 0.094 Uiso 1 1 calc R . . C67 C 0.8113(8) 0.8168(7) 0.7161(8) 0.086(4) Uani 1 1 d U . . H67A H 0.8101 0.8456 0.7559 0.103 Uiso 1 1 calc R . . H67B H 0.8302 0.7729 0.7309 0.103 Uiso 1 1 calc R . . H67C H 0.7630 0.8118 0.6920 0.103 Uiso 1 1 calc R . . C68 C 0.8505(10) 0.9209(7) 0.6503(9) 0.119(5) Uani 1 1 d U . . H68A H 0.8010 0.9291 0.6305 0.143 Uiso 1 1 calc R . . H68B H 0.8825 0.9331 0.6173 0.143 Uiso 1 1 calc R . . H68C H 0.8619 0.9479 0.6915 0.143 Uiso 1 1 calc R . . C69 C 0.9260(9) 0.7631(10) 0.6201(9) 0.135(5) Uani 1 1 d DU . . H69 H 0.9160 0.7298 0.5825 0.162 Uiso 1 1 calc R . . C70 C 0.9239(10) 0.7122(8) 0.6810(9) 0.130(6) Uani 1 1 d DU . . H70A H 0.9433 0.6691 0.6690 0.156 Uiso 1 1 calc R . . H70B H 0.8745 0.7062 0.6897 0.156 Uiso 1 1 calc R . . H70C H 0.9525 0.7297 0.7220 0.156 Uiso 1 1 calc R . . C71 C 0.9917(7) 0.7952(9) 0.5948(9) 0.132(5) Uani 1 1 d U . . H71A H 1.0076 0.8333 0.6238 0.159 Uiso 1 1 calc R . . H71B H 0.9790 0.8104 0.5478 0.159 Uiso 1 1 calc R . . H71C H 1.0301 0.7622 0.5968 0.159 Uiso 1 1 calc R . . C72 C 0.8359(6) 0.8357(6) 0.5373(6) 0.060(3) Uani 1 1 d U . . H72A H 0.7897 0.8594 0.5338 0.072 Uiso 1 1 calc R . . H72B H 0.8735 0.8697 0.5347 0.072 Uiso 1 1 calc R . . C73 C 0.8346(7) 0.7925(7) 0.4800(7) 0.066(4) Uani 1 1 d U . . H73A H 0.8749 0.7615 0.4874 0.080 Uiso 1 1 calc R . . H73B H 0.8381 0.8190 0.4391 0.080 Uiso 1 1 calc R . . H73C H 0.7899 0.7672 0.4740 0.080 Uiso 1 1 calc R . . O1W O 0.5077(6) 0.7261(4) 0.8660(6) 0.176(4) Uani 1 1 d . . . O3W O 0.7285(7) 0.7038(8) 0.2118(8) 0.211(6) Uani 1 1 d . . . O2W O 0.5901(7) 0.5356(6) 0.9860(7) 0.141(5) Uani 1 1 d . . . O4W O 0.6623(7) 0.5463(6) 0.1075(6) 0.141(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.03296(10) 0.03505(11) 0.05384(14) -0.0046(4) -0.00176(9) -0.0029(4) O1 0.036(3) 0.038(4) 0.126(6) -0.015(4) 0.044(3) -0.012(3) O2 0.058(4) 0.067(5) 0.017(3) 0.004(3) -0.011(3) -0.009(4) O3 0.028(3) 0.065(5) 0.081(5) -0.016(4) 0.007(3) -0.003(3) O4 0.047(4) 0.013(3) 0.083(5) -0.011(3) 0.013(4) -0.009(3) O5 0.078(5) 0.014(3) 0.093(6) -0.001(3) -0.001(5) -0.001(3) O6 0.018(3) 0.040(4) 0.061(5) 0.010(3) -0.003(3) -0.003(3) O7 0.049(4) 0.031(4) 0.057(4) -0.001(3) -0.023(3) -0.002(3) O8 0.036(4) 0.059(5) 0.067(6) -0.013(4) -0.018(4) -0.010(4) O9 0.177(11) 0.122(10) 0.199(12) -0.060(9) 0.067(10) -0.016(9) O10 0.094(7) 0.184(11) 0.129(9) 0.003(8) 0.039(6) 0.004(7) O11 0.089(6) 0.073(5) 0.055(5) 0.000(4) -0.011(4) 0.007(4) O12 0.125(9) 0.081(7) 0.100(8) 0.020(6) 0.014(7) -0.003(6) O13 0.108(7) 0.143(9) 0.111(7) -0.007(6) 0.047(6) -0.034(7) O14 0.213(11) 0.075(7) 0.115(7) -0.003(6) 0.098(7) 0.000(7) N1 0.044(4) 0.043(5) 0.079(6) -0.010(5) -0.036(4) 0.018(4) N2 0.129(11) 0.086(10) 0.069(8) -0.004(7) 0.017(8) 0.020(8) C1 0.039(4) 0.063(6) 0.068(5) 0.026(5) 0.006(4) 0.009(4) C2 0.037(3) 0.053(4) 0.074(4) 0.026(4) -0.006(4) 0.001(3) C3 0.060(4) 0.047(4) 0.078(4) 0.018(4) -0.016(4) -0.004(4) C4 0.068(5) 0.060(5) 0.090(5) 0.007(5) -0.018(4) -0.018(4) C5 0.053(4) 0.057(5) 0.093(5) 0.016(4) -0.012(4) -0.022(4) C6 0.039(4) 0.055(4) 0.088(5) 0.029(4) -0.007(4) -0.013(4) C7 0.042(4) 0.051(4) 0.088(4) 0.028(4) -0.001(4) 0.004(3) C8 0.088(4) 0.052(4) 0.074(4) 0.003(4) -0.022(4) -0.001(4) C9 0.091(5) 0.044(4) 0.062(5) 0.001(4) -0.022(4) -0.012(4) C10 0.108(5) 0.049(5) 0.067(5) 0.002(4) -0.010(5) -0.022(5) C11 0.123(6) 0.063(5) 0.063(5) 0.003(5) -0.006(5) -0.016(5) C12 0.125(6) 0.064(5) 0.072(5) -0.009(5) -0.013(5) -0.005(5) C13 0.118(6) 0.051(5) 0.082(5) -0.006(5) -0.016(5) -0.005(5) C14 0.052(4) 0.048(4) 0.095(4) 0.023(4) 0.018(4) 0.003(4) C15 0.061(4) 0.063(5) 0.113(5) 0.014(5) 0.030(5) 0.006(4) C16 0.072(5) 0.079(5) 0.120(6) 0.013(5) 0.033(5) 0.005(5) C17 0.076(5) 0.077(5) 0.099(5) 0.023(5) 0.023(5) 0.001(5) C18 0.082(5) 0.064(5) 0.089(5) 0.029(4) 0.016(5) -0.001(4) C19 0.067(5) 0.054(4) 0.080(5) 0.026(4) 0.022(4) 0.002(4) C20 0.037(3) 0.030(3) 0.065(4) 0.018(6) -0.002(3) 0.008(6) C21 0.029(3) 0.042(3) 0.070(4) 0.006(4) -0.003(3) -0.009(4) C22 0.032(3) 0.043(4) 0.090(4) -0.008(4) 0.007(3) -0.007(3) C23 0.046(4) 0.041(4) 0.102(5) -0.002(4) 0.011(4) 0.010(4) C24 0.055(4) 0.045(4) 0.104(6) 0.006(5) 0.013(5) 0.013(5) C25 0.060(5) 0.046(5) 0.106(6) 0.020(5) 0.003(5) 0.005(4) C26 0.044(4) 0.049(4) 0.089(4) 0.019(4) 0.006(4) -0.008(4) C27 0.042(4) 0.048(4) 0.091(4) -0.021(4) 0.000(4) -0.006(3) C28 0.051(4) 0.055(5) 0.084(5) -0.011(4) 0.000(4) -0.008(4) C29 0.066(5) 0.061(5) 0.087(5) -0.013(5) -0.002(5) 0.000(4) C30 0.069(5) 0.059(5) 0.083(5) -0.009(5) -0.009(5) 0.018(4) C31 0.070(5) 0.070(5) 0.088(5) -0.020(5) -0.011(5) 0.001(5) C32 0.059(5) 0.064(5) 0.098(5) -0.027(5) 0.000(5) -0.006(4) C33 0.051(4) 0.057(4) 0.084(4) 0.024(4) 0.009(4) -0.006(4) C34 0.065(5) 0.068(5) 0.088(5) 0.041(5) 0.012(5) 0.004(4) C35 0.076(5) 0.073(5) 0.074(5) 0.030(5) 0.007(5) -0.001(5) C36 0.075(5) 0.073(5) 0.065(5) 0.024(5) 0.015(4) -0.016(5) C37 0.071(5) 0.064(5) 0.074(5) 0.017(5) 0.017(4) -0.005(4) C38 0.059(5) 0.061(5) 0.077(5) 0.020(5) 0.006(5) -0.008(4) C39 0.045(5) 0.021(4) 0.067(6) 0.010(4) -0.003(5) 0.010(4) C40 0.047(4) 0.033(4) 0.077(4) 0.003(4) -0.010(4) 0.004(3) C41 0.044(4) 0.041(4) 0.098(5) -0.009(4) -0.002(4) 0.004(4) C42 0.057(5) 0.056(5) 0.105(6) -0.013(5) -0.004(5) 0.016(4) C43 0.062(5) 0.058(5) 0.090(5) -0.003(5) -0.014(5) 0.019(4) C44 0.069(5) 0.051(5) 0.074(5) 0.006(4) -0.023(4) 0.014(4) C45 0.056(4) 0.038(4) 0.063(4) 0.000(4) -0.017(4) 0.009(3) C46 0.049(4) 0.040(4) 0.112(5) -0.010(4) 0.014(4) -0.005(4) C47 0.068(5) 0.054(5) 0.129(6) -0.001(5) 0.027(5) -0.004(4) C48 0.071(5) 0.069(5) 0.124(6) -0.011(5) 0.043(5) 0.000(4) C49 0.079(5) 0.064(5) 0.103(6) -0.011(5) 0.033(5) -0.003(5) C50 0.068(5) 0.059(5) 0.096(5) -0.014(5) 0.023(5) -0.010(4) C51 0.061(5) 0.050(5) 0.100(6) -0.008(5) 0.021(5) -0.015(4) C52 0.075(4) 0.043(4) 0.055(4) 0.009(4) -0.013(4) 0.008(4) C53 0.086(5) 0.040(4) 0.060(5) 0.013(4) 0.001(4) -0.006(4) C54 0.102(5) 0.048(5) 0.072(5) 0.003(5) 0.007(5) 0.004(5) C55 0.113(6) 0.071(5) 0.070(5) 0.005(5) 0.012(5) 0.008(5) C56 0.115(6) 0.068(5) 0.070(5) 0.018(5) -0.001(5) 0.007(5) C57 0.097(5) 0.051(5) 0.073(5) 0.008(4) -0.010(5) 0.012(5) C58 0.064(6) 0.081(7) 0.132(9) -0.035(7) 0.007(6) -0.005(6) C59 0.056(6) 0.092(9) 0.121(10) -0.016(8) -0.005(7) -0.003(6) C60 0.136(11) 0.128(11) 0.176(12) -0.027(10) 0.002(10) 0.001(10) C61 0.166(11) 0.094(9) 0.137(10) -0.016(9) -0.017(9) 0.025(9) C62 0.159(13) 0.101(10) 0.153(13) -0.013(10) -0.001(11) 0.009(10) C64 0.154(11) 0.091(9) 0.202(13) 0.052(9) -0.083(10) -0.052(9) C63 0.139(11) 0.090(9) 0.137(11) -0.027(9) 0.012(9) -0.021(9) C65 0.162(12) 0.075(9) 0.235(15) 0.060(9) -0.100(11) -0.026(9) C66 0.085(6) 0.053(6) 0.083(7) -0.010(5) -0.038(6) -0.014(5) C67 0.083(8) 0.086(8) 0.089(8) -0.017(7) 0.007(7) -0.006(6) C68 0.163(12) 0.058(7) 0.128(10) -0.035(7) -0.015(9) 0.006(8) C69 0.088(8) 0.174(10) 0.138(9) 0.074(8) -0.006(8) 0.031(8) C70 0.103(10) 0.127(11) 0.150(11) 0.074(9) -0.016(9) 0.029(8) C71 0.045(6) 0.200(13) 0.145(11) 0.036(10) -0.011(7) 0.007(8) C72 0.057(6) 0.054(6) 0.070(7) -0.008(5) 0.018(5) -0.017(5) C73 0.061(7) 0.078(8) 0.057(6) -0.014(6) -0.007(5) 0.002(6) O1W 0.286(9) 0.044(4) 0.251(9) -0.019(5) 0.228(7) -0.028(6) O3W 0.177(8) 0.327(17) 0.146(10) -0.021(10) 0.077(8) -0.188(9) O2W 0.161(10) 0.093(7) 0.169(10) 0.033(7) 0.017(8) -0.036(7) O4W 0.166(10) 0.102(8) 0.131(8) -0.038(6) -0.066(8) 0.041(7) _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 O1 1.581(9) . ? U1 O2 1.811(8) . ? U1 O6 2.396(7) . ? U1 O7 2.396(7) . ? U1 O3 2.515(7) . ? U1 O5 2.523(7) . ? U1 O4 2.535(7) . ? U1 O8 2.561(7) . ? O3 C1 1.294(12) . ? O4 C1 1.252(13) . ? O5 C20 1.199(16) . ? O6 C20 1.335(16) . ? O7 C39 1.215(12) . ? O8 C39 1.238(12) . ? O9 C11 1.309(19) . ? O10 C17 1.393(17) . ? O11 C30 1.470(16) . ? O12 C36 1.259(17) . ? O13 C49 1.381(16) . ? O14 C55 1.49(2) . ? N1 C64 1.54(2) . ? N1 C61 1.568(19) . ? N1 C58 1.594(17) . ? N2 C72 1.442(17) . ? N2 C66 1.504(16) . ? N2 C69 1.63(2) . ? C1 C2 1.543(15) . ? C2 C3 1.310(16) . ? C2 C7 1.472(16) . ? C3 C4 1.425(16) . ? C3 C8 1.498(18) . ? C4 C5 1.382(16) . ? C5 C6 1.334(16) . ? C6 C7 1.333(15) . ? C7 C14 1.501(17) . ? C8 C9 1.446(17) . ? C8 C13 1.499(19) . ? C9 C10 1.387(19) . ? C10 C11 1.34(2) . ? C11 C12 1.326(19) . ? C12 C13 1.40(2) . ? C14 C19 1.353(16) . ? C14 C15 1.453(17) . ? C15 C16 1.279(17) . ? C16 C17 1.400(18) . ? C17 C18 1.389(17) . ? C18 C19 1.478(17) . ? C20 C21 1.508(9) . ? C21 C22 1.353(17) . ? C21 C26 1.490(17) . ? C22 C23 1.362(15) . ? C22 C27 1.398(16) . ? C23 C24 1.254(16) . ? C24 C25 1.436(18) . ? C25 C26 1.443(18) . ? C26 C33 1.555(14) . ? C27 C32 1.326(16) . ? C27 C28 1.451(16) . ? C28 C29 1.289(18) . ? C29 C30 1.356(17) . ? C30 C31 1.368(18) . ? C31 C32 1.562(19) . ? C33 C38 1.305(18) . ? C33 C34 1.477(18) . ? C34 C35 1.18(2) . ? C35 C36 1.28(2) . ? C36 C37 1.451(19) . ? C37 C38 1.452(19) . ? C39 C40 1.508(14) . ? C40 C41 1.322(18) . ? C40 C45 1.460(16) . ? C41 C46 1.49(2) . ? C41 C42 1.484(17) . ? C42 C43 1.389(18) . ? C43 C44 1.257(17) . ? C44 C45 1.415(15) . ? C45 C52 1.445(17) . ? C46 C47 1.351(18) . ? C46 C51 1.462(19) . ? C47 C48 1.415(19) . ? C48 C49 1.363(19) . ? C49 C50 1.412(17) . ? C50 C51 1.286(19) . ? C52 C57 1.313(18) . ? C52 C53 1.345(17) . ? C53 C54 1.348(19) . ? C54 C55 1.39(2) . ? C55 C56 1.40(2) . ? C56 C57 1.355(19) . ? C58 C60 1.545(14) . ? C58 C59 1.60(2) . ? C61 C63 1.503(15) . ? C61 C62 1.553(16) . ? C64 C65 1.45(3) . ? C66 C68 1.463(18) . ? C66 C67 1.517(18) . ? C69 C71 1.51(2) . ? C69 C70 1.554(15) . ? C72 C73 1.399(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 177.5(4) . . ? O1 U1 O6 90.0(3) . . ? O2 U1 O6 90.9(3) . . ? O1 U1 O7 91.4(3) . . ? O2 U1 O7 87.5(3) . . ? O6 U1 O7 173.4(2) . . ? O1 U1 O3 87.1(3) . . ? O2 U1 O3 94.5(3) . . ? O6 U1 O3 119.2(2) . . ? O7 U1 O3 67.34(16) . . ? O1 U1 O5 87.7(3) . . ? O2 U1 O5 91.0(3) . . ? O6 U1 O5 52.85(16) . . ? O7 U1 O5 120.8(3) . . ? O3 U1 O5 170.5(3) . . ? O1 U1 O4 97.0(3) . . ? O2 U1 O4 85.4(3) . . ? O6 U1 O4 67.7(2) . . ? O7 U1 O4 118.5(2) . . ? O3 U1 O4 52.5(2) . . ? O5 U1 O4 120.4(2) . . ? O1 U1 O8 84.6(3) . . ? O2 U1 O8 93.0(3) . . ? O6 U1 O8 124.1(2) . . ? O7 U1 O8 49.7(3) . . ? O3 U1 O8 116.1(2) . . ? O5 U1 O8 71.3(3) . . ? O4 U1 O8 168.20(17) . . ? C1 O3 U1 92.2(7) . . ? C1 O4 U1 92.2(6) . . ? C20 O5 U1 92.5(7) . . ? C20 O6 U1 94.9(5) . . ? C39 O7 U1 100.9(6) . . ? C39 O8 U1 92.1(6) . . ? C64 N1 C61 133.5(11) . . ? C64 N1 C58 100.3(11) . . ? C61 N1 C58 113.2(9) . . ? C72 N2 C66 118.4(11) . . ? C72 N2 C69 114.6(12) . . ? C66 N2 C69 96.7(12) . . ? O4 C1 O3 122.7(10) . . ? O4 C1 C2 127.4(9) . . ? O3 C1 C2 109.5(10) . . ? C3 C2 C7 120.4(11) . . ? C3 C2 C1 120.9(11) . . ? C7 C2 C1 118.7(10) . . ? C2 C3 C4 115.7(12) . . ? C2 C3 C8 122.4(11) . . ? C4 C3 C8 121.4(11) . . ? C5 C4 C3 123.9(12) . . ? C6 C5 C4 118.2(10) . . ? C5 C6 C7 121.0(11) . . ? C6 C7 C2 120.4(11) . . ? C6 C7 C14 121.9(11) . . ? C2 C7 C14 117.7(10) . . ? C9 C8 C13 115.2(13) . . ? C9 C8 C3 123.8(12) . . ? C13 C8 C3 121.0(12) . . ? C10 C9 C8 116.4(12) . . ? C11 C10 C9 126.6(13) . . ? O9 C11 C12 120.7(14) . . ? O9 C11 C10 117.1(14) . . ? C12 C11 C10 121.2(15) . . ? C11 C12 C13 119.0(14) . . ? C12 C13 C8 121.5(12) . . ? C19 C14 C15 117.1(12) . . ? C19 C14 C7 122.2(11) . . ? C15 C14 C7 119.6(10) . . ? C16 C15 C14 118.6(12) . . ? C15 C16 C17 127.6(13) . . ? C18 C17 O10 115.1(11) . . ? C18 C17 C16 116.6(13) . . ? O10 C17 C16 128.4(12) . . ? C17 C18 C19 117.0(11) . . ? C14 C19 C18 122.2(12) . . ? O5 C20 O6 119.6(6) . . ? O5 C20 C21 116.6(12) . . ? O6 C20 C21 123.7(12) . . ? C22 C21 C26 120.0(7) . . ? C22 C21 C20 124.2(12) . . ? C26 C21 C20 114.3(12) . . ? C21 C22 C23 120.2(11) . . ? C21 C22 C27 120.5(10) . . ? C23 C22 C27 118.8(11) . . ? C24 C23 C22 123.3(12) . . ? C23 C24 C25 122.0(8) . . ? C26 C25 C24 118.8(12) . . ? C25 C26 C21 113.5(11) . . ? C25 C26 C33 122.2(11) . . ? C21 C26 C33 122.8(10) . . ? C32 C27 C22 120.9(11) . . ? C32 C27 C28 117.2(12) . . ? C22 C27 C28 121.9(10) . . ? C29 C28 C27 122.4(12) . . ? C28 C29 C30 123.6(14) . . ? C31 C30 C29 120.5(14) . . ? C31 C30 O11 115.1(11) . . ? C29 C30 O11 124.4(12) . . ? C30 C31 C32 116.0(12) . . ? C27 C32 C31 119.9(12) . . ? C38 C33 C34 113.5(13) . . ? C38 C33 C26 122.9(12) . . ? C34 C33 C26 123.3(12) . . ? C35 C34 C33 124.3(15) . . ? C34 C35 C36 124.2(16) . . ? O12 C36 C35 119.6(14) . . ? O12 C36 C37 118.9(14) . . ? C35 C36 C37 121.5(15) . . ? C36 C37 C38 111.9(13) . . ? C33 C38 C37 124.2(13) . . ? O7 C39 O8 116.9(9) . . ? O7 C39 C40 127.0(9) . . ? O8 C39 C40 115.9(10) . . ? C41 C40 C45 122.4(11) . . ? C41 C40 C39 119.0(12) . . ? C45 C40 C39 118.0(11) . . ? C40 C41 C46 130.0(12) . . ? C40 C41 C42 113.6(12) . . ? C46 C41 C42 116.5(11) . . ? C43 C42 C41 122.9(12) . . ? C44 C43 C42 121.4(12) . . ? C43 C44 C45 120.6(12) . . ? C44 C45 C52 116.6(11) . . ? C44 C45 C40 118.9(11) . . ? C52 C45 C40 124.1(10) . . ? C47 C46 C41 118.7(12) . . ? C47 C46 C51 116.0(14) . . ? C41 C46 C51 125.2(12) . . ? C46 C47 C48 122.6(13) . . ? C49 C48 C47 119.0(12) . . ? C48 C49 O13 120.3(12) . . ? C48 C49 C50 118.6(13) . . ? O13 C49 C50 121.0(12) . . ? C51 C50 C49 122.4(13) . . ? C50 C51 C46 121.3(13) . . ? C57 C52 C53 118.0(13) . . ? C57 C52 C45 117.4(12) . . ? C53 C52 C45 123.8(12) . . ? C52 C53 C54 125.9(12) . . ? C53 C54 C55 114.7(14) . . ? C54 C55 C56 120.6(14) . . ? C54 C55 O14 116.8(13) . . ? C56 C55 O14 120.3(13) . . ? C57 C56 C55 118.7(13) . . ? C52 C57 C56 122.0(13) . . ? C60 C58 C59 124.0(13) . . ? C60 C58 N1 103.3(10) . . ? C59 C58 N1 110.4(10) . . ? C63 C61 C62 106.2(14) . . ? C63 C61 N1 125.2(13) . . ? C62 C61 N1 123.8(12) . . ? C65 C64 N1 113.2(18) . . ? C68 C66 N2 112.2(11) . . ? C68 C66 C67 118.9(13) . . ? N2 C66 C67 103.5(11) . . ? C71 C69 C70 128.3(14) . . ? C71 C69 N2 117.4(12) . . ? C70 C69 N2 110.2(13) . . ? C73 C72 N2 116.3(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 U1 O3 C1 -104.5(7) . . . . ? O2 U1 O3 C1 77.4(7) . . . . ? O6 U1 O3 C1 -16.1(7) . . . . ? O7 U1 O3 C1 162.8(6) . . . . ? O5 U1 O3 C1 -47.4(19) . . . . ? O4 U1 O3 C1 -3.4(6) . . . . ? O8 U1 O3 C1 173.0(6) . . . . ? O1 U1 O4 C1 84.3(7) . . . . ? O2 U1 O4 C1 -95.7(7) . . . . ? O6 U1 O4 C1 171.5(7) . . . . ? O7 U1 O4 C1 -11.1(8) . . . . ? O3 U1 O4 C1 3.5(6) . . . . ? O5 U1 O4 C1 175.8(7) . . . . ? O8 U1 O4 C1 -13(2) . . . . ? O1 U1 O5 C20 93.9(11) . . . . ? O2 U1 O5 C20 -88.2(11) . . . . ? O6 U1 O5 C20 2.2(11) . . . . ? O7 U1 O5 C20 -175.9(10) . . . . ? O3 U1 O5 C20 37(2) . . . . ? O4 U1 O5 C20 -2.9(11) . . . . ? O8 U1 O5 C20 179.0(11) . . . . ? O1 U1 O6 C20 -89.1(10) . . . . ? O2 U1 O6 C20 88.6(10) . . . . ? O7 U1 O6 C20 13(3) . . . . ? O3 U1 O6 C20 -175.7(9) . . . . ? O5 U1 O6 C20 -1.9(10) . . . . ? O4 U1 O6 C20 173.4(10) . . . . ? O8 U1 O6 C20 -5.6(10) . . . . ? O1 U1 O7 C39 85.5(8) . . . . ? O2 U1 O7 C39 -92.3(8) . . . . ? O6 U1 O7 C39 -17(3) . . . . ? O3 U1 O7 C39 171.8(7) . . . . ? O5 U1 O7 C39 -2.7(9) . . . . ? O4 U1 O7 C39 -175.8(7) . . . . ? O8 U1 O7 C39 3.7(7) . . . . ? O1 U1 O8 C39 -100.0(8) . . . . ? O2 U1 O8 C39 80.6(8) . . . . ? O6 U1 O8 C39 173.6(7) . . . . ? O7 U1 O8 C39 -3.6(7) . . . . ? O3 U1 O8 C39 -15.9(8) . . . . ? O5 U1 O8 C39 170.6(8) . . . . ? O4 U1 O8 C39 -1(2) . . . . ? U1 O4 C1 O3 -6.4(12) . . . . ? U1 O4 C1 C2 -178.4(11) . . . . ? U1 O3 C1 O4 6.4(12) . . . . ? U1 O3 C1 C2 179.7(8) . . . . ? O4 C1 C2 C3 102.5(15) . . . . ? O3 C1 C2 C3 -70.3(13) . . . . ? O4 C1 C2 C7 -74.4(15) . . . . ? O3 C1 C2 C7 112.7(11) . . . . ? C7 C2 C3 C4 4.8(16) . . . . ? C1 C2 C3 C4 -172.1(10) . . . . ? C7 C2 C3 C8 176.1(10) . . . . ? C1 C2 C3 C8 -0.8(17) . . . . ? C2 C3 C4 C5 -8.6(18) . . . . ? C8 C3 C4 C5 180.0(11) . . . . ? C3 C4 C5 C6 5.7(18) . . . . ? C4 C5 C6 C7 1.3(17) . . . . ? C5 C6 C7 C2 -4.9(16) . . . . ? C5 C6 C7 C14 174.9(10) . . . . ? C3 C2 C7 C6 1.6(16) . . . . ? C1 C2 C7 C6 178.5(10) . . . . ? C3 C2 C7 C14 -178.3(10) . . . . ? C1 C2 C7 C14 -1.3(14) . . . . ? C2 C3 C8 C9 -38.2(18) . . . . ? C4 C3 C8 C9 132.7(13) . . . . ? C2 C3 C8 C13 139.2(12) . . . . ? C4 C3 C8 C13 -50.0(16) . . . . ? C13 C8 C9 C10 1.2(16) . . . . ? C3 C8 C9 C10 178.7(11) . . . . ? C8 C9 C10 C11 -1(2) . . . . ? C9 C10 C11 O9 167.0(14) . . . . ? C9 C10 C11 C12 -1(2) . . . . ? O9 C11 C12 C13 -164.1(14) . . . . ? C10 C11 C12 C13 4(2) . . . . ? C11 C12 C13 C8 -3.7(19) . . . . ? C9 C8 C13 C12 1.2(18) . . . . ? C3 C8 C13 C12 -176.4(11) . . . . ? C6 C7 C14 C19 132.6(12) . . . . ? C2 C7 C14 C19 -47.6(16) . . . . ? C6 C7 C14 C15 -34.8(16) . . . . ? C2 C7 C14 C15 145.0(10) . . . . ? C19 C14 C15 C16 6.3(17) . . . . ? C7 C14 C15 C16 174.3(11) . . . . ? C14 C15 C16 C17 3(2) . . . . ? C15 C16 C17 C18 -6(2) . . . . ? C15 C16 C17 O10 175.6(14) . . . . ? O10 C17 C18 C19 179.4(11) . . . . ? C16 C17 C18 C19 0.9(17) . . . . ? C15 C14 C19 C18 -11.3(17) . . . . ? C7 C14 C19 C18 -179.0(10) . . . . ? C17 C18 C19 C14 7.8(17) . . . . ? U1 O5 C20 O6 -3.6(17) . . . . ? U1 O5 C20 C21 177.6(14) . . . . ? U1 O6 C20 O5 3.8(18) . . . . ? U1 O6 C20 C21 -177.5(16) . . . . ? O5 C20 C21 C22 -78(2) . . . . ? O6 C20 C21 C22 103.1(18) . . . . ? O5 C20 C21 C26 115.9(16) . . . . ? O6 C20 C21 C26 -63(2) . . . . ? C26 C21 C22 C23 -15.8(19) . . . . ? C20 C21 C22 C23 178.9(12) . . . . ? C26 C21 C22 C27 173.0(9) . . . . ? C20 C21 C22 C27 7.7(19) . . . . ? C21 C22 C23 C24 11.2(19) . . . . ? C27 C22 C23 C24 -177.4(12) . . . . ? C22 C23 C24 C25 -6(2) . . . . ? C23 C24 C25 C26 6(2) . . . . ? C24 C25 C26 C21 -9.9(18) . . . . ? C24 C25 C26 C33 -176.3(12) . . . . ? C22 C21 C26 C25 15.0(19) . . . . ? C20 C21 C26 C25 -178.3(12) . . . . ? C22 C21 C26 C33 -178.7(9) . . . . ? C20 C21 C26 C33 -12.0(18) . . . . ? C21 C22 C27 C32 130.1(13) . . . . ? C23 C22 C27 C32 -41.2(17) . . . . ? C21 C22 C27 C28 -51.9(17) . . . . ? C23 C22 C27 C28 136.8(12) . . . . ? C32 C27 C28 C29 -2(2) . . . . ? C22 C27 C28 C29 180.0(13) . . . . ? C27 C28 C29 C30 7(2) . . . . ? C28 C29 C30 C31 -6(2) . . . . ? C28 C29 C30 O11 172.5(13) . . . . ? C29 C30 C31 C32 0.1(19) . . . . ? O11 C30 C31 C32 -178.1(11) . . . . ? C22 C27 C32 C31 174.8(11) . . . . ? C28 C27 C32 C31 -3.2(18) . . . . ? C30 C31 C32 C27 4.2(19) . . . . ? C25 C26 C33 C38 128.6(15) . . . . ? C21 C26 C33 C38 -36.5(19) . . . . ? C25 C26 C33 C34 -45.0(18) . . . . ? C21 C26 C33 C34 149.9(12) . . . . ? C38 C33 C34 C35 4(2) . . . . ? C26 C33 C34 C35 178.4(15) . . . . ? C33 C34 C35 C36 -7(3) . . . . ? C34 C35 C36 O12 -177.7(16) . . . . ? C34 C35 C36 C37 3(2) . . . . ? O12 C36 C37 C38 -176.8(13) . . . . ? C35 C36 C37 C38 3(2) . . . . ? C34 C33 C38 C37 2(2) . . . . ? C26 C33 C38 C37 -172.4(12) . . . . ? C36 C37 C38 C33 -5(2) . . . . ? U1 O7 C39 O8 -6.6(13) . . . . ? U1 O7 C39 C40 178.9(11) . . . . ? U1 O8 C39 O7 6.1(12) . . . . ? U1 O8 C39 C40 -178.9(9) . . . . ? O7 C39 C40 C41 92.8(16) . . . . ? O8 C39 C40 C41 -81.7(15) . . . . ? O7 C39 C40 C45 -79.0(16) . . . . ? O8 C39 C40 C45 106.5(13) . . . . ? C45 C40 C41 C46 179.8(12) . . . . ? C39 C40 C41 C46 8(2) . . . . ? C45 C40 C41 C42 -1.0(17) . . . . ? C39 C40 C41 C42 -172.4(10) . . . . ? C40 C41 C42 C43 3.9(18) . . . . ? C46 C41 C42 C43 -176.8(12) . . . . ? C41 C42 C43 C44 -3(2) . . . . ? C42 C43 C44 C45 -2(2) . . . . ? C43 C44 C45 C52 178.1(12) . . . . ? C43 C44 C45 C40 4.5(18) . . . . ? C41 C40 C45 C44 -3.0(18) . . . . ? C39 C40 C45 C44 168.5(10) . . . . ? C41 C40 C45 C52 -176.1(12) . . . . ? C39 C40 C45 C52 -4.6(17) . . . . ? C40 C41 C46 C47 139.4(14) . . . . ? C42 C41 C46 C47 -39.8(17) . . . . ? C40 C41 C46 C51 -36(2) . . . . ? C42 C41 C46 C51 144.6(13) . . . . ? C41 C46 C47 C48 -176.4(12) . . . . ? C51 C46 C47 C48 -0.4(19) . . . . ? C46 C47 C48 C49 -0.9(19) . . . . ? C47 C48 C49 O13 176.0(12) . . . . ? C47 C48 C49 C50 -0.5(18) . . . . ? C48 C49 C50 C51 4(2) . . . . ? O13 C49 C50 C51 -172.8(13) . . . . ? C49 C50 C51 C46 -5(2) . . . . ? C47 C46 C51 C50 3.4(19) . . . . ? C41 C46 C51 C50 179.2(13) . . . . ? C44 C45 C52 C57 -26.6(17) . . . . ? C40 C45 C52 C57 146.7(12) . . . . ? C44 C45 C52 C53 143.5(12) . . . . ? C40 C45 C52 C53 -43.3(18) . . . . ? C57 C52 C53 C54 -4(2) . . . . ? C45 C52 C53 C54 -174.0(13) . . . . ? C52 C53 C54 C55 2(2) . . . . ? C53 C54 C55 C56 0(2) . . . . ? C53 C54 C55 O14 -162.7(12) . . . . ? C54 C55 C56 C57 -1(2) . . . . ? O14 C55 C56 C57 161.3(13) . . . . ? C53 C52 C57 C56 3(2) . . . . ? C45 C52 C57 C56 173.6(12) . . . . ? C55 C56 C57 C52 -1(2) . . . . ? C64 N1 C58 C60 -60.4(13) . . . . ? C61 N1 C58 C60 86.7(13) . . . . ? C64 N1 C58 C59 74.2(12) . . . . ? C61 N1 C58 C59 -138.7(11) . . . . ? C64 N1 C61 C63 117.7(19) . . . . ? C58 N1 C61 C63 -14.8(19) . . . . ? C64 N1 C61 C62 -90(2) . . . . ? C58 N1 C61 C62 137.2(14) . . . . ? C61 N1 C64 C65 43(2) . . . . ? C58 N1 C64 C65 179.8(13) . . . . ? C72 N2 C66 C68 4(2) . . . . ? C69 N2 C66 C68 126.6(13) . . . . ? C72 N2 C66 C67 133.3(13) . . . . ? C69 N2 C66 C67 -104.0(11) . . . . ? C72 N2 C69 C71 39(2) . . . . ? C66 N2 C69 C71 -86.1(17) . . . . ? C72 N2 C69 C70 -161.4(14) . . . . ? C66 N2 C69 C70 73.1(16) . . . . ? C66 N2 C72 C73 172.7(12) . . . . ? C69 N2 C72 C73 59.5(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.600 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.129