# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Bernardo Masci' 'Pierre Thuery' _publ_contact_author_name 'Prof Bernardo Masci' _publ_contact_author_address ; Dipartimento di Chimica Universita La Sapienza P.le Aldo Moro 5 Box 34 - Roma 62 Roma 00185 ITALY ; _publ_contact_author_email BERNARDO.MASCI@UNIROMA1.IT _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis of homooxacalixarenes with 5 and 10 phenol units and crystal structure of their complexes with uranyl ions ; data_18 _database_code_depnum_ccdc_archive 'CCDC 255525' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C141.50 H183.50 N7.50 O14 U' _chemical_formula_weight 2451.49 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.0169(17) _cell_length_b 16.2046(10) _cell_length_c 27.024(3) _cell_angle_alpha 96.325(6) _cell_angle_beta 96.207(5) _cell_angle_gamma 108.071(6) _cell_volume 6552.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39820 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method ? _exptl_crystal_F_000 2578 _exptl_absorpt_coefficient_mu 1.302 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _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 39820 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.68 _reflns_number_total 21721 _reflns_number_gt 11742 _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 Patterson map interpretation and subsequent Fourier-difference synthesis. One pyridine molecule has been affected with a 0.5 occupancy factor so as to keep a physically acceptable displacement parameter. All non-hydrogen atoms were refined with anisotropic displacement parameters, with some restraints for some tert-butyl groups and pyridine molecules. The H atoms bound to N and O were found on a Fourier-difference map and all the other ones were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (NH, OH, CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Some short H...H contacts involve the protons of the pyridine solvent molecules, likely as a result of their imperfect location. A void of 72 A^3^ indicates the presence of another unresolved solvent molecule. 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1017P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _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 21721 _refine_ls_number_parameters 1522 _refine_ls_number_restraints 342 _refine_ls_R_factor_all 0.1717 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.873 _refine_diff_density_max 0.930 _refine_diff_density_min -1.623 _refine_diff_density_rms 0.118 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 0.81384(3) 0.02282(2) 0.241918(17) 0.03851(13) Uani 1 1 d . . . O1 O 0.7658(4) 0.1088(4) 0.2371(3) 0.0409(17) Uani 1 1 d . . . O2 O 0.8613(5) -0.0626(4) 0.2475(3) 0.0467(18) Uani 1 1 d . . . O1A O 0.9151(5) 0.0856(4) 0.1946(3) 0.0472(18) Uani 1 1 d . . . O2A O 0.9049(4) 0.1038(4) 0.3116(3) 0.0457(18) Uani 1 1 d . . . O3A O 0.6164(5) 0.0672(4) 0.3186(3) 0.0481(18) Uani 1 1 d . . . H3A H 0.6656 0.0514 0.3085 0.058 Uiso 1 1 d R . . O4A O 0.4710(5) -0.0028(4) 0.2456(3) 0.0465(18) Uani 1 1 d . . . H4A H 0.5153 0.0000 0.2703 0.056 Uiso 1 1 d R . . O5A O 0.5760(5) -0.0002(4) 0.1475(3) 0.053(2) Uani 1 1 d . . . H5A H 0.6186 -0.0127 0.1516 0.063 Uiso 1 1 d R . . O6A O 0.7671(5) 0.1251(5) 0.1058(3) 0.054(2) Uani 1 1 d . . . C1A C 0.9227(7) 0.1883(6) 0.1359(4) 0.045(3) Uani 1 1 d . . . C2A C 0.9512(7) 0.1692(6) 0.1835(4) 0.045(3) Uani 1 1 d . . . C3A C 1.0177(7) 0.2329(7) 0.2175(5) 0.050(3) Uani 1 1 d . . . C4A C 1.0526(7) 0.3159(7) 0.2021(5) 0.057(3) Uani 1 1 d . . . H4C H 1.0958 0.3599 0.2247 0.069 Uiso 1 1 calc R . . C5A C 1.0265(8) 0.3360(7) 0.1554(5) 0.051(3) Uani 1 1 d . . . C6A C 0.9615(7) 0.2709(7) 0.1225(5) 0.054(3) Uani 1 1 d . . . H6A H 0.9433 0.2821 0.0909 0.065 Uiso 1 1 calc R . . C7A C 1.0711(8) 0.4280(7) 0.1419(5) 0.061(3) Uani 1 1 d . . . C8A C 1.0490(10) 0.4969(9) 0.1760(6) 0.083(4) Uani 1 1 d U . . H8A1 H 1.0727 0.4977 0.2103 0.125 Uiso 1 1 calc R . . H8A2 H 0.9857 0.4829 0.1729 0.125 Uiso 1 1 calc R . . H8A3 H 1.0746 0.5536 0.1664 0.125 Uiso 1 1 calc R . . C9A C 1.0393(10) 0.4332(9) 0.0870(6) 0.089(5) Uani 1 1 d U . . H9A1 H 0.9769 0.4258 0.0828 0.134 Uiso 1 1 calc R . . H9A2 H 1.0494 0.3876 0.0651 0.134 Uiso 1 1 calc R . . H9A3 H 1.0715 0.4894 0.0789 0.134 Uiso 1 1 calc R . . C10A C 1.1713(9) 0.4456(9) 0.1460(6) 0.080(4) Uani 1 1 d U . . H10A H 1.1974 0.4951 0.1297 0.119 Uiso 1 1 calc R . . H10B H 1.1822 0.3948 0.1300 0.119 Uiso 1 1 calc R . . H10C H 1.1971 0.4579 0.1809 0.119 Uiso 1 1 calc R . . C11A C 1.0441(7) 0.2207(7) 0.2701(4) 0.051(3) Uani 1 1 d . . . H11A H 1.1065 0.2541 0.2808 0.061 Uiso 1 1 calc R . . H11B H 1.0370 0.1592 0.2708 0.061 Uiso 1 1 calc R . . C12A C 0.9902(6) 0.2495(6) 0.3069(4) 0.043(3) Uani 1 1 d . . . C13A C 0.9238(7) 0.1920(6) 0.3242(4) 0.044(3) Uani 1 1 d . . . C14A C 0.8701(7) 0.2227(6) 0.3565(4) 0.042(2) Uani 1 1 d . . . C15A C 0.8934(7) 0.3142(6) 0.3692(4) 0.045(3) Uani 1 1 d . . . H15A H 0.8597 0.3350 0.3902 0.054 Uiso 1 1 calc R . . C16A C 0.9629(7) 0.3770(7) 0.3532(4) 0.048(3) Uani 1 1 d . . . C17A C 1.0116(7) 0.3407(7) 0.3231(4) 0.049(3) Uani 1 1 d . . . H17A H 1.0612 0.3786 0.3131 0.059 Uiso 1 1 calc R . . C18A C 0.9862(8) 0.4732(7) 0.3728(5) 0.055(3) Uani 1 1 d . . . C19A C 0.9008(9) 0.5019(7) 0.3688(5) 0.069(4) Uani 1 1 d . . . H19A H 0.8632 0.4751 0.3919 0.103 Uiso 1 1 calc R . . H19B H 0.8691 0.4836 0.3351 0.103 Uiso 1 1 calc R . . H19C H 0.9178 0.5647 0.3769 0.103 Uiso 1 1 calc R . . C20A C 1.0264(10) 0.4914(9) 0.4268(6) 0.080(4) Uani 1 1 d U . . H20A H 0.9844 0.4584 0.4460 0.120 Uiso 1 1 calc R . . H20B H 1.0417 0.5530 0.4389 0.120 Uiso 1 1 calc R . . H20C H 1.0789 0.4745 0.4302 0.120 Uiso 1 1 calc R . . C21A C 1.0468(9) 0.5294(8) 0.3417(6) 0.078(4) Uani 1 1 d U . . H21A H 1.0522 0.5899 0.3513 0.118 Uiso 1 1 calc R . . H21B H 1.0224 0.5115 0.3067 0.118 Uiso 1 1 calc R . . H21C H 1.1043 0.5226 0.3473 0.118 Uiso 1 1 calc R . . C22A C 0.7985(6) 0.1590(7) 0.3778(4) 0.044(3) Uani 1 1 d . . . H22A H 0.8246 0.1501 0.4100 0.053 Uiso 1 1 calc R . . H22B H 0.7803 0.1032 0.3556 0.053 Uiso 1 1 calc R . . C23A C 0.7155(6) 0.1816(6) 0.3857(4) 0.041(2) Uani 1 1 d . . . C24A C 0.6345(7) 0.1373(7) 0.3582(4) 0.047(3) Uani 1 1 d . . . C25A C 0.5588(7) 0.1605(7) 0.3664(4) 0.047(3) Uani 1 1 d . . . C26A C 0.5673(7) 0.2298(7) 0.4044(4) 0.050(3) Uani 1 1 d . . . H26A H 0.5177 0.2458 0.4098 0.060 Uiso 1 1 calc R . . C27A C 0.6502(7) 0.2761(6) 0.4349(4) 0.041(2) Uani 1 1 d . . . C28A C 0.7201(7) 0.2493(7) 0.4244(4) 0.045(3) Uani 1 1 d . . . H28A H 0.7749 0.2779 0.4443 0.054 Uiso 1 1 calc R . . C29A C 0.6578(7) 0.3553(7) 0.4726(5) 0.051(3) Uani 1 1 d . . . C30A C 0.7494(8) 0.3919(8) 0.5043(5) 0.069(4) Uani 1 1 d . . . H30A H 0.7620 0.3464 0.5206 0.104 Uiso 1 1 calc R . . H30B H 0.7508 0.4394 0.5294 0.104 Uiso 1 1 calc R . . H30C H 0.7933 0.4129 0.4831 0.104 Uiso 1 1 calc R . . C31A C 0.6406(9) 0.4273(7) 0.4468(5) 0.070(4) Uani 1 1 d . . . H31A H 0.6832 0.4450 0.4244 0.106 Uiso 1 1 calc R . . H31B H 0.6459 0.4766 0.4716 0.106 Uiso 1 1 calc R . . H31C H 0.5818 0.4062 0.4280 0.106 Uiso 1 1 calc R . . C32A C 0.5896(8) 0.3265(9) 0.5099(5) 0.073(4) Uani 1 1 d . . . H32A H 0.5303 0.3125 0.4924 0.109 Uiso 1 1 calc R . . H32B H 0.6004 0.3736 0.5372 0.109 Uiso 1 1 calc R . . H32C H 0.5962 0.2758 0.5230 0.109 Uiso 1 1 calc R . . C33A C 0.4663(6) 0.1078(6) 0.3373(4) 0.045(3) Uani 1 1 d . . . H33A H 0.4586 0.0457 0.3354 0.053 Uiso 1 1 calc R . . H33B H 0.4219 0.1195 0.3561 0.053 Uiso 1 1 calc R . . C34A C 0.4494(7) 0.1279(6) 0.2841(5) 0.048(3) Uani 1 1 d . . . C35A C 0.4502(7) 0.0741(6) 0.2415(4) 0.043(2) Uani 1 1 d . . . C36A C 0.4232(7) 0.0878(7) 0.1934(4) 0.044(3) Uani 1 1 d . . . C37A C 0.3992(7) 0.1622(7) 0.1884(5) 0.050(3) Uani 1 1 d . . . H37A H 0.3830 0.1729 0.1563 0.060 Uiso 1 1 calc R . . C38A C 0.3984(7) 0.2216(7) 0.2300(5) 0.048(3) Uani 1 1 d . . . C39A C 0.4258(7) 0.2021(6) 0.2780(4) 0.045(3) Uani 1 1 d . . . H39A H 0.4279 0.2407 0.3066 0.054 Uiso 1 1 calc R . . C40A C 0.3673(7) 0.3008(7) 0.2252(5) 0.052(3) Uani 1 1 d . . . C41A C 0.4325(9) 0.3841(8) 0.2582(6) 0.078(4) Uani 1 1 d . . . H41A H 0.4110 0.4327 0.2550 0.117 Uiso 1 1 calc R . . H41B H 0.4898 0.3968 0.2476 0.117 Uiso 1 1 calc R . . H41C H 0.4374 0.3749 0.2928 0.117 Uiso 1 1 calc R . . C42A C 0.3592(8) 0.3204(8) 0.1715(5) 0.062(3) Uani 1 1 d . . . H42A H 0.3141 0.2721 0.1504 0.093 Uiso 1 1 calc R . . H42B H 0.4150 0.3288 0.1594 0.093 Uiso 1 1 calc R . . H42C H 0.3433 0.3728 0.1707 0.093 Uiso 1 1 calc R . . C43A C 0.2787(8) 0.2807(8) 0.2413(6) 0.075(4) Uani 1 1 d . . . H43A H 0.2535 0.3253 0.2340 0.112 Uiso 1 1 calc R . . H43B H 0.2845 0.2789 0.2769 0.112 Uiso 1 1 calc R . . H43C H 0.2406 0.2247 0.2236 0.112 Uiso 1 1 calc R . . C44A C 0.4163(7) 0.0257(6) 0.1471(4) 0.044(3) Uani 1 1 d . . . H44A H 0.3554 0.0061 0.1302 0.052 Uiso 1 1 calc R . . H44B H 0.4288 -0.0255 0.1571 0.052 Uiso 1 1 calc R . . C45A C 0.4762(7) 0.0607(6) 0.1098(4) 0.042(2) Uani 1 1 d . . . C46A C 0.5577(7) 0.0461(6) 0.1113(4) 0.049(3) Uani 1 1 d . . . C47A C 0.6139(7) 0.0744(7) 0.0755(5) 0.049(3) Uani 1 1 d . . . C48A C 0.5885(8) 0.1245(7) 0.0419(4) 0.055(3) Uani 1 1 d . . . H48A H 0.6252 0.1456 0.0185 0.066 Uiso 1 1 calc R . . C49A C 0.5102(8) 0.1440(7) 0.0422(5) 0.053(3) Uani 1 1 d . . . C50A C 0.4541(7) 0.1094(6) 0.0752(4) 0.043(3) Uani 1 1 d . . . H50A H 0.3998 0.1192 0.0741 0.052 Uiso 1 1 calc R . . C51A C 0.4913(8) 0.2069(7) 0.0075(5) 0.054(3) Uani 1 1 d . . . C52A C 0.4090(11) 0.2288(11) 0.0129(7) 0.109(6) Uani 1 1 d U . . H52A H 0.4050 0.2721 -0.0080 0.163 Uiso 1 1 calc R . . H52B H 0.4105 0.2517 0.0474 0.163 Uiso 1 1 calc R . . H52C H 0.3583 0.1768 0.0028 0.163 Uiso 1 1 calc R . . C53A C 0.5697(11) 0.3001(9) 0.0214(7) 0.098(5) Uani 1 1 d U . . H53A H 0.5605 0.3385 -0.0017 0.146 Uiso 1 1 calc R . . H53B H 0.6259 0.2915 0.0191 0.146 Uiso 1 1 calc R . . H53C H 0.5694 0.3260 0.0551 0.146 Uiso 1 1 calc R . . C54A C 0.4900(10) 0.1748(9) -0.0468(6) 0.087(4) Uani 1 1 d U . . H54A H 0.4450 0.1184 -0.0566 0.130 Uiso 1 1 calc R . . H54B H 0.5469 0.1696 -0.0515 0.130 Uiso 1 1 calc R . . H54C H 0.4774 0.2156 -0.0672 0.130 Uiso 1 1 calc R . . C55A C 0.6973(7) 0.0557(7) 0.0745(5) 0.054(3) Uani 1 1 d . . . H55A H 0.6924 0.0004 0.0866 0.064 Uiso 1 1 calc R . . H55B H 0.7102 0.0508 0.0402 0.064 Uiso 1 1 calc R . . C56A C 0.8521(7) 0.1186(7) 0.1002(5) 0.050(3) Uani 1 1 d . . . H56A H 0.8629 0.1245 0.0659 0.059 Uiso 1 1 calc R . . H56B H 0.8537 0.0613 0.1066 0.059 Uiso 1 1 calc R . . O1B O 0.7111(4) -0.0644(4) 0.1784(3) 0.0432(17) Uani 1 1 d . . . O2B O 0.7215(4) -0.0300(4) 0.2962(3) 0.0461(18) Uani 1 1 d . . . O3B O 0.9925(5) 0.0131(5) 0.3617(3) 0.0524(19) Uani 1 1 d . . . H3B H 0.9471 0.0320 0.3490 0.063 Uiso 1 1 d R . . O4B O 1.1424(6) 0.0584(5) 0.3182(4) 0.070(2) Uani 1 1 d . . . H4B H 1.0850 0.0389 0.3210 0.084 Uiso 1 1 d R . . O5B O 1.0490(5) 0.0101(5) 0.2033(3) 0.060(2) Uani 1 1 d . . . H5B H 1.0690 0.0164 0.2388 0.072 Uiso 1 1 d R . . O6B O 0.8670(5) -0.1410(5) 0.1307(3) 0.062(2) Uani 1 1 d . . . C1B C 0.7087(8) -0.1958(7) 0.1274(4) 0.051(3) Uani 1 1 d . . . C2B C 0.6763(7) -0.1518(6) 0.1652(4) 0.042(3) Uani 1 1 d . . . C3B C 0.6061(7) -0.2000(7) 0.1868(4) 0.047(3) Uani 1 1 d . . . C4B C 0.5664(8) -0.2900(7) 0.1714(5) 0.055(3) Uani 1 1 d . . . H4D H 0.5186 -0.3209 0.1860 0.066 Uiso 1 1 calc R . . C5B C 0.5972(9) -0.3340(7) 0.1347(5) 0.058(3) Uani 1 1 d . . . C6B C 0.6677(9) -0.2862(7) 0.1133(5) 0.061(3) Uani 1 1 d . . . H6B H 0.6886 -0.3154 0.0885 0.073 Uiso 1 1 calc R . . C7B C 0.5521(9) -0.4360(8) 0.1182(5) 0.070(4) Uani 1 1 d U . . C8B C 0.4460(11) -0.4589(11) 0.1073(7) 0.112(6) Uani 1 1 d U . . H8B1 H 0.4310 -0.4291 0.0807 0.168 Uiso 1 1 calc R . . H8B2 H 0.4253 -0.4402 0.1372 0.168 Uiso 1 1 calc R . . H8B3 H 0.4184 -0.5211 0.0976 0.168 Uiso 1 1 calc R . . C9B C 0.5694(13) -0.4655(12) 0.0665(8) 0.130(7) Uani 1 1 d U . . H9B1 H 0.6263 -0.4741 0.0691 0.194 Uiso 1 1 calc R . . H9B2 H 0.5690 -0.4215 0.0455 0.194 Uiso 1 1 calc R . . H9B3 H 0.5239 -0.5197 0.0519 0.194 Uiso 1 1 calc R . . C10B C 0.5659(11) -0.4823(10) 0.1605(6) 0.094(5) Uani 1 1 d U . . H10D H 0.5356 -0.5441 0.1507 0.141 Uiso 1 1 calc R . . H10E H 0.5428 -0.4610 0.1887 0.141 Uiso 1 1 calc R . . H10F H 0.6283 -0.4721 0.1696 0.141 Uiso 1 1 calc R . . C11B C 0.5752(7) -0.1592(7) 0.2312(5) 0.056(3) Uani 1 1 d . . . H11C H 0.5910 -0.0964 0.2310 0.067 Uiso 1 1 calc R . . H11D H 0.5110 -0.1832 0.2278 0.067 Uiso 1 1 calc R . . C12B C 0.6141(7) -0.1747(6) 0.2798(4) 0.046(3) Uani 1 1 d . . . C13B C 0.6910(6) -0.1113(6) 0.3103(4) 0.040(2) Uani 1 1 d . . . C14B C 0.7328(8) -0.1312(7) 0.3529(5) 0.051(3) Uani 1 1 d . . . C15B C 0.6960(8) -0.2157(7) 0.3657(5) 0.055(3) Uani 1 1 d . . . H15B H 0.7252 -0.2312 0.3929 0.066 Uiso 1 1 calc R . . C16B C 0.6181(8) -0.2767(6) 0.3395(5) 0.051(3) Uani 1 1 d . . . C17B C 0.5796(8) -0.2550(6) 0.2963(4) 0.049(3) Uani 1 1 d . . . H17B H 0.5285 -0.2961 0.2776 0.059 Uiso 1 1 calc R . . C18B C 0.5794(8) -0.3675(7) 0.3573(5) 0.059(3) Uani 1 1 d . . . C19B C 0.6193(10) -0.4318(7) 0.3325(6) 0.073(4) Uani 1 1 d . . . H19D H 0.6127 -0.4314 0.2968 0.109 Uiso 1 1 calc R . . H19E H 0.5892 -0.4897 0.3392 0.109 Uiso 1 1 calc R . . H19F H 0.6812 -0.4150 0.3458 0.109 Uiso 1 1 calc R . . C20B C 0.5968(11) -0.3591(9) 0.4159(6) 0.092(5) Uani 1 1 d . . . H20D H 0.5618 -0.4123 0.4262 0.138 Uiso 1 1 calc R . . H20E H 0.5807 -0.3106 0.4307 0.138 Uiso 1 1 calc R . . H20F H 0.6587 -0.3492 0.4268 0.138 Uiso 1 1 calc R . . C21B C 0.4782(9) -0.4023(8) 0.3416(7) 0.088(5) Uani 1 1 d . . . H21D H 0.4643 -0.4047 0.3060 0.132 Uiso 1 1 calc R . . H21E H 0.4520 -0.3639 0.3589 0.132 Uiso 1 1 calc R . . H21F H 0.4550 -0.4601 0.3503 0.132 Uiso 1 1 calc R . . C22B C 0.8100(7) -0.0616(7) 0.3869(4) 0.049(3) Uani 1 1 d . . . H22C H 0.8304 -0.0127 0.3686 0.059 Uiso 1 1 calc R . . H22D H 0.7867 -0.0405 0.4156 0.059 Uiso 1 1 calc R . . C23B C 0.8896(8) -0.0833(7) 0.4070(5) 0.050(3) Uani 1 1 d . . . C24B C 0.9739(8) -0.0440(7) 0.3968(4) 0.054(3) Uani 1 1 d . . . C25B C 1.0497(8) -0.0616(8) 0.4191(5) 0.056(3) Uani 1 1 d . . . C26B C 1.0390(9) -0.1231(8) 0.4510(5) 0.063(3) Uani 1 1 d . . . H26B H 1.0884 -0.1355 0.4653 0.076 Uiso 1 1 calc R . . C27B C 0.9536(9) -0.1685(7) 0.4627(5) 0.059(3) Uani 1 1 d . . . C28B C 0.8834(8) -0.1440(7) 0.4421(5) 0.056(3) Uani 1 1 d . . . H28B H 0.8283 -0.1688 0.4519 0.068 Uiso 1 1 calc R . . C29B C 0.9429(9) -0.2357(8) 0.4997(5) 0.068(4) Uani 1 1 d . . . C30B C 1.0098(10) -0.2852(9) 0.4941(6) 0.086(4) Uani 1 1 d U . . H30D H 1.0690 -0.2441 0.5007 0.129 Uiso 1 1 calc R . . H30E H 0.9988 -0.3163 0.4604 0.129 Uiso 1 1 calc R . . H30F H 1.0034 -0.3262 0.5176 0.129 Uiso 1 1 calc R . . C31B C 0.8487(9) -0.3056(8) 0.4874(6) 0.078(4) Uani 1 1 d U . . H31D H 0.8473 -0.3541 0.5051 0.117 Uiso 1 1 calc R . . H31E H 0.8350 -0.3260 0.4518 0.117 Uiso 1 1 calc R . . H31F H 0.8057 -0.2797 0.4977 0.117 Uiso 1 1 calc R . . C32B C 0.9615(9) -0.1879(9) 0.5537(5) 0.070(4) Uani 1 1 d . . . H32D H 1.0206 -0.1464 0.5601 0.105 Uiso 1 1 calc R . . H32E H 0.9562 -0.2297 0.5767 0.105 Uiso 1 1 calc R . . H32F H 0.9195 -0.1575 0.5583 0.105 Uiso 1 1 calc R . . C33B C 1.1426(7) -0.0112(7) 0.4120(5) 0.058(3) Uani 1 1 d . . . H33C H 1.1828 -0.0100 0.4418 0.070 Uiso 1 1 calc R . . H33D H 1.1458 0.0490 0.4096 0.070 Uiso 1 1 calc R . . C34B C 1.1758(7) -0.0464(7) 0.3662(5) 0.054(3) Uani 1 1 d . . . C35B C 1.1743(7) -0.0111(8) 0.3228(5) 0.055(3) Uani 1 1 d . . . C36B C 1.2116(8) -0.0392(7) 0.2828(5) 0.056(3) Uani 1 1 d . . . C37B C 1.2492(8) -0.1071(8) 0.2874(5) 0.060(3) Uani 1 1 d . . . H37B H 1.2752 -0.1249 0.2608 0.072 Uiso 1 1 calc R . . C38B C 1.2489(8) -0.1474(8) 0.3295(5) 0.063(3) Uani 1 1 d . . . C39B C 1.2119(8) -0.1170(7) 0.3693(5) 0.059(3) Uani 1 1 d . . . H39B H 1.2105 -0.1430 0.3983 0.071 Uiso 1 1 calc R . . C40B C 1.2904(9) -0.2181(8) 0.3342(6) 0.068(4) Uani 1 1 d . . . C41B C 1.2527(11) -0.2903(10) 0.2894(7) 0.102(5) Uani 1 1 d U . . H41D H 1.1891 -0.3062 0.2838 0.153 Uiso 1 1 calc R . . H41E H 1.2693 -0.3406 0.2959 0.153 Uiso 1 1 calc R . . H41F H 1.2758 -0.2698 0.2600 0.153 Uiso 1 1 calc R . . C42B C 1.2776(9) -0.2590(8) 0.3817(5) 0.075(4) Uani 1 1 d U . . H42D H 1.3046 -0.2147 0.4105 0.112 Uiso 1 1 calc R . . H42E H 1.3048 -0.3041 0.3818 0.112 Uiso 1 1 calc R . . H42F H 1.2153 -0.2842 0.3828 0.112 Uiso 1 1 calc R . . C43B C 1.3935(10) -0.1734(10) 0.3373(6) 0.090(5) Uani 1 1 d U . . H43D H 1.4057 -0.1488 0.3071 0.135 Uiso 1 1 calc R . . H43E H 1.4227 -0.2164 0.3408 0.135 Uiso 1 1 calc R . . H43F H 1.4150 -0.1276 0.3658 0.135 Uiso 1 1 calc R . . C44B C 1.2172(7) 0.0049(8) 0.2357(5) 0.060(3) Uani 1 1 d . . . H44C H 1.1990 0.0565 0.2413 0.072 Uiso 1 1 calc R . . H44D H 1.2786 0.0242 0.2299 0.072 Uiso 1 1 calc R . . C45B C 1.1608(8) -0.0541(7) 0.1896(5) 0.050(3) Uani 1 1 d . . . C46B C 1.0754(8) -0.0476(7) 0.1740(4) 0.052(3) Uani 1 1 d . . . C47B C 1.0256(8) -0.0972(7) 0.1288(4) 0.051(3) Uani 1 1 d . . . C48B C 1.0568(9) -0.1562(7) 0.1014(5) 0.057(3) Uani 1 1 d . . . H48B H 1.0224 -0.1903 0.0718 0.068 Uiso 1 1 calc R . . C49B C 1.1389(9) -0.1652(8) 0.1175(6) 0.070(4) Uani 1 1 d . . . C50B C 1.1874(9) -0.1130(8) 0.1616(6) 0.063(3) Uani 1 1 d . . . H50B H 1.2421 -0.1187 0.1727 0.076 Uiso 1 1 calc R . . C51B C 1.1707(9) -0.2299(7) 0.0851(6) 0.069(4) Uani 1 1 d . . . C52B C 1.2434(16) -0.2596(15) 0.1189(10) 0.167(9) Uani 1 1 d U . . H52D H 1.2371 -0.2498 0.1538 0.251 Uiso 1 1 calc R . . H52E H 1.3021 -0.2257 0.1142 0.251 Uiso 1 1 calc R . . H52F H 1.2340 -0.3208 0.1086 0.251 Uiso 1 1 calc R . . C53B C 1.0993(14) -0.3119(13) 0.0641(9) 0.139(7) Uani 1 1 d U . . H53D H 1.0594 -0.3008 0.0386 0.209 Uiso 1 1 calc R . . H53E H 1.0674 -0.3348 0.0904 0.209 Uiso 1 1 calc R . . H53F H 1.1243 -0.3540 0.0497 0.209 Uiso 1 1 calc R . . C54B C 1.2187(13) -0.1864(12) 0.0462(8) 0.119(6) Uani 1 1 d U . . H54D H 1.2477 -0.2236 0.0304 0.178 Uiso 1 1 calc R . . H54E H 1.2622 -0.1315 0.0617 0.178 Uiso 1 1 calc R . . H54F H 1.1772 -0.1759 0.0213 0.178 Uiso 1 1 calc R . . C55B C 0.9399(8) -0.0860(8) 0.1086(5) 0.060(3) Uani 1 1 d . . . H55C H 0.9439 -0.0249 0.1165 0.072 Uiso 1 1 calc R . . H55D H 0.9285 -0.1021 0.0723 0.072 Uiso 1 1 calc R . . C56B C 0.7831(8) -0.1470(7) 0.1039(5) 0.053(3) Uani 1 1 d . . . H56C H 0.7774 -0.1759 0.0697 0.064 Uiso 1 1 calc R . . H56D H 0.7807 -0.0883 0.1022 0.064 Uiso 1 1 calc R . . N1 N 0.7212(9) 0.2504(8) 0.2213(6) 0.095(4) Uani 1 1 d U . . H1 H 0.7244 0.1958 0.2236 0.114 Uiso 1 1 calc R . . N2 N 0.7098(7) 0.3982(6) 0.2196(5) 0.074(3) Uani 1 1 d . . . C1 C 0.8141(7) 0.3137(8) 0.2246(6) 0.066(4) Uani 1 1 d . . . H1A H 0.8440 0.2949 0.1983 0.079 Uiso 1 1 calc R . . H1B H 0.8487 0.3179 0.2570 0.079 Uiso 1 1 calc R . . C2 C 0.8025(9) 0.4015(8) 0.2176(7) 0.087(5) Uani 1 1 d . . . H2A H 0.8417 0.4469 0.2439 0.104 Uiso 1 1 calc R . . H2B H 0.8186 0.4166 0.1854 0.104 Uiso 1 1 calc R . . C3 C 0.6673(13) 0.2467(12) 0.1767(8) 0.116(6) Uani 1 1 d U . . H3D H 0.6115 0.1992 0.1735 0.139 Uiso 1 1 calc R . . H3E H 0.6964 0.2373 0.1480 0.139 Uiso 1 1 calc R . . C4 C 0.6508(11) 0.3357(10) 0.1793(6) 0.091(5) Uani 1 1 d U . . H4E H 0.6594 0.3579 0.1477 0.109 Uiso 1 1 calc R . . H4F H 0.5898 0.3277 0.1842 0.109 Uiso 1 1 calc R . . C5 C 0.6834(16) 0.2801(15) 0.2661(10) 0.154(8) Uani 1 1 d U . . H5D H 0.6240 0.2401 0.2660 0.184 Uiso 1 1 calc R . . H5E H 0.7201 0.2794 0.2970 0.184 Uiso 1 1 calc R . . C6 C 0.6803(13) 0.3679(12) 0.2641(8) 0.110(6) Uani 1 1 d U . . H6C H 0.6199 0.3680 0.2648 0.132 Uiso 1 1 calc R . . H6D H 0.7177 0.4073 0.2933 0.132 Uiso 1 1 calc R . . N3 N 0.8996(7) -0.2149(6) 0.2338(4) 0.060(3) Uani 1 1 d U . . H3 H 0.8788 -0.1652 0.2261 0.072 Uiso 1 1 d R . . N4 N 0.9142(8) -0.3464(7) 0.2722(5) 0.071(3) Uani 1 1 d U . . C7 C 0.8111(9) -0.2684(9) 0.2405(6) 0.077(4) Uani 1 1 d U . . H7A H 0.7722 -0.2885 0.2084 0.092 Uiso 1 1 calc R . . H7B H 0.7853 -0.2353 0.2628 0.092 Uiso 1 1 calc R . . C8 C 0.8254(12) -0.3478(11) 0.2643(7) 0.109(6) Uani 1 1 d U . . H8A H 0.8034 -0.3489 0.2963 0.130 Uiso 1 1 calc R . . H8B H 0.7901 -0.4018 0.2424 0.130 Uiso 1 1 calc R . . C9 C 0.9615(15) -0.1845(14) 0.2782(9) 0.148(8) Uani 1 1 d U . . H9A H 0.9447 -0.1432 0.3006 0.177 Uiso 1 1 calc R . . H9B H 1.0201 -0.1550 0.2704 0.177 Uiso 1 1 calc R . . C10 C 0.9622(16) -0.2648(15) 0.3036(10) 0.156(9) Uani 1 1 d U . . H10G H 1.0233 -0.2625 0.3128 0.187 Uiso 1 1 calc R . . H10H H 0.9364 -0.2621 0.3344 0.187 Uiso 1 1 calc R . . C11 C 0.9284(14) -0.2732(12) 0.1972(8) 0.122(6) Uani 1 1 d U . . H11E H 0.8822 -0.2995 0.1684 0.146 Uiso 1 1 calc R . . H11F H 0.9818 -0.2397 0.1853 0.146 Uiso 1 1 calc R . . C12 C 0.9459(11) -0.3431(10) 0.2247(6) 0.089(5) Uani 1 1 d U . . H12A H 0.9178 -0.3997 0.2036 0.107 Uiso 1 1 calc R . . H12B H 1.0093 -0.3329 0.2301 0.107 Uiso 1 1 calc R . . N5 N 0.6239(9) 0.0446(8) 0.5234(6) 0.096(4) Uani 1 1 d U . . C13 C 0.6128(10) 0.0436(10) 0.4744(7) 0.087(4) Uani 1 1 d U . . H13 H 0.6153 0.0960 0.4627 0.104 Uiso 1 1 calc R . . C14 C 0.5980(9) -0.0286(9) 0.4398(6) 0.077(4) Uani 1 1 d U . . H14 H 0.5902 -0.0256 0.4055 0.093 Uiso 1 1 calc R . . C15 C 0.5949(9) -0.1050(9) 0.4565(6) 0.080(4) Uani 1 1 d U . . H15 H 0.5852 -0.1554 0.4336 0.096 Uiso 1 1 calc R . . C16 C 0.6062(9) -0.1086(9) 0.5076(6) 0.078(4) Uani 1 1 d U . . H16 H 0.6046 -0.1603 0.5200 0.094 Uiso 1 1 calc R . . C17 C 0.6198(9) -0.0322(9) 0.5387(6) 0.081(4) Uani 1 1 d U . . H17 H 0.6268 -0.0335 0.5732 0.098 Uiso 1 1 calc R . . N6 N 1.1713(10) 0.1085(10) 0.1136(6) 0.113(5) Uani 1 1 d U . . C18 C 1.1850(10) 0.0634(9) 0.0728(6) 0.078(4) Uani 1 1 d U . . H18 H 1.2099 0.0194 0.0768 0.094 Uiso 1 1 calc R . . C19 C 1.1647(14) 0.0787(13) 0.0274(9) 0.129(7) Uani 1 1 d U . . H19 H 1.1769 0.0468 -0.0001 0.155 Uiso 1 1 calc R . . C20 C 1.1240(12) 0.1440(11) 0.0195(8) 0.106(5) Uani 1 1 d U . . H20 H 1.1087 0.1546 -0.0128 0.127 Uiso 1 1 calc R . . C21 C 1.1083(13) 0.1895(13) 0.0598(8) 0.118(6) Uani 1 1 d U . . H21 H 1.0850 0.2349 0.0564 0.141 Uiso 1 1 calc R . . C22 C 1.1275(10) 0.1676(10) 0.1059(7) 0.086(4) Uani 1 1 d U . . H22 H 1.1102 0.1941 0.1334 0.103 Uiso 1 1 calc R . . N7 N 1.3153(10) 0.4111(9) 0.4118(6) 0.109(5) Uani 1 1 d U . . C23 C 1.2391(10) 0.3484(9) 0.3863(6) 0.081(4) Uani 1 1 d U . . H23 H 1.1924 0.3662 0.3733 0.097 Uiso 1 1 calc R . . C24 C 1.2298(10) 0.2627(9) 0.3794(6) 0.077(4) Uani 1 1 d U . . H24 H 1.1781 0.2221 0.3611 0.093 Uiso 1 1 calc R . . C25 C 1.2959(10) 0.2361(9) 0.3991(6) 0.078(4) Uani 1 1 d U . . H25 H 1.2889 0.1765 0.3951 0.093 Uiso 1 1 calc R . . C26 C 1.3696(10) 0.2920(9) 0.4237(6) 0.081(4) Uani 1 1 d U . . H26 H 1.4158 0.2726 0.4356 0.097 Uiso 1 1 calc R . . C27 C 1.3789(12) 0.3767(11) 0.4320(7) 0.098(5) Uani 1 1 d U . . H27 H 1.4301 0.4148 0.4520 0.117 Uiso 1 1 calc R . . N8 N 0.7730(11) 0.4750(8) 0.0141(7) 0.078(6) Uani 0.50 1 d PGU . . C28 C 0.7749(12) 0.5477(11) -0.0092(5) 0.088(9) Uani 0.50 1 d PGU . . H28 H 0.7512 0.5402 -0.0430 0.105 Uiso 0.50 1 calc PR . . C29 C 0.8121(12) 0.6317(9) 0.0181(7) 0.064(7) Uani 0.50 1 d PGU . . H29 H 0.8134 0.6804 0.0025 0.077 Uiso 0.50 1 calc PR . . C30 C 0.8475(12) 0.6430(9) 0.0686(7) 0.091(9) Uani 0.50 1 d PGU . . H30 H 0.8724 0.6992 0.0868 0.110 Uiso 0.50 1 calc PR . . C31 C 0.8456(13) 0.5702(13) 0.0918(6) 0.094(10) Uani 0.50 1 d PGU . . H31 H 0.8693 0.5777 0.1257 0.112 Uiso 0.50 1 calc PR . . C32 C 0.8084(13) 0.4862(10) 0.0646(7) 0.094(10) Uani 0.50 1 d PGU . . H32 H 0.8072 0.4375 0.0801 0.113 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 U 0.0395(2) 0.03584(19) 0.0426(2) 0.00765(14) 0.00568(15) 0.01525(15) O1 0.038(4) 0.029(3) 0.057(5) 0.006(3) 0.013(3) 0.011(3) O2 0.051(5) 0.048(4) 0.046(5) 0.005(3) 0.001(4) 0.025(3) O1A 0.066(5) 0.053(4) 0.033(4) 0.015(3) 0.018(4) 0.027(4) O2A 0.047(4) 0.045(4) 0.045(5) 0.001(3) -0.005(3) 0.021(3) O3A 0.043(4) 0.061(4) 0.045(5) -0.005(3) 0.004(3) 0.029(4) O4A 0.048(4) 0.049(4) 0.046(5) 0.012(3) 0.003(3) 0.021(3) O5A 0.048(5) 0.060(4) 0.061(6) 0.026(4) 0.013(4) 0.025(4) O6A 0.045(5) 0.067(5) 0.056(5) 0.006(4) 0.016(4) 0.025(4) C1A 0.035(6) 0.044(6) 0.052(8) 0.001(5) 0.013(5) 0.009(5) C2A 0.053(7) 0.043(6) 0.041(7) 0.009(5) 0.005(5) 0.022(5) C3A 0.033(6) 0.049(6) 0.072(9) 0.017(6) 0.015(6) 0.014(5) C4A 0.037(6) 0.054(7) 0.081(10) 0.008(6) 0.021(6) 0.012(5) C5A 0.052(7) 0.060(7) 0.051(8) 0.015(6) 0.021(6) 0.026(6) C6A 0.051(7) 0.048(6) 0.071(9) 0.019(6) 0.022(6) 0.020(5) C7A 0.063(8) 0.049(7) 0.071(10) 0.016(6) 0.008(7) 0.018(6) C8A 0.088(6) 0.077(5) 0.087(6) 0.015(4) 0.023(4) 0.028(4) C9A 0.095(6) 0.085(6) 0.089(6) 0.022(4) 0.013(4) 0.027(4) C10A 0.074(6) 0.080(5) 0.081(6) 0.011(4) 0.017(4) 0.019(4) C11A 0.050(7) 0.051(6) 0.045(8) 0.005(5) 0.005(5) 0.008(5) C12A 0.025(5) 0.049(6) 0.059(8) 0.007(5) 0.007(5) 0.015(4) C13A 0.041(6) 0.040(6) 0.053(8) 0.007(5) 0.007(5) 0.017(5) C14A 0.036(6) 0.047(6) 0.043(7) 0.003(5) -0.008(5) 0.019(5) C15A 0.049(6) 0.042(6) 0.041(7) 0.002(5) 0.010(5) 0.011(5) C16A 0.052(7) 0.048(6) 0.044(7) 0.002(5) 0.009(5) 0.017(5) C17A 0.040(6) 0.048(6) 0.057(8) -0.006(5) 0.002(5) 0.018(5) C18A 0.058(7) 0.040(6) 0.057(8) -0.001(5) 0.006(6) 0.006(5) C19A 0.082(9) 0.045(7) 0.082(11) 0.010(6) 0.021(8) 0.022(6) C20A 0.083(6) 0.075(5) 0.079(6) 0.012(4) 0.002(4) 0.027(4) C21A 0.079(6) 0.073(5) 0.082(6) 0.011(4) 0.018(4) 0.021(4) C22A 0.028(5) 0.056(6) 0.045(7) -0.003(5) 0.002(5) 0.013(5) C23A 0.025(5) 0.044(6) 0.052(7) 0.007(5) 0.005(5) 0.009(4) C24A 0.048(7) 0.049(6) 0.051(8) 0.014(5) 0.014(5) 0.021(5) C25A 0.045(6) 0.053(6) 0.046(7) 0.011(5) 0.011(5) 0.020(5) C26A 0.051(7) 0.066(7) 0.045(7) 0.013(5) 0.015(5) 0.033(6) C27A 0.035(6) 0.046(6) 0.038(7) 0.003(4) 0.008(5) 0.009(4) C28A 0.043(6) 0.058(6) 0.035(7) 0.005(5) 0.000(5) 0.020(5) C29A 0.044(7) 0.058(7) 0.057(8) 0.002(5) 0.005(6) 0.027(5) C30A 0.056(8) 0.078(8) 0.070(10) -0.019(7) 0.008(7) 0.028(7) C31A 0.085(10) 0.043(6) 0.089(11) -0.002(6) 0.012(8) 0.034(7) C32A 0.047(7) 0.098(10) 0.058(9) -0.006(7) 0.007(6) 0.008(7) C33A 0.034(6) 0.047(6) 0.052(7) 0.010(5) 0.004(5) 0.013(5) C34A 0.037(6) 0.042(6) 0.064(9) 0.002(5) 0.004(5) 0.015(5) C35A 0.036(6) 0.041(6) 0.040(7) 0.002(5) 0.002(5) 0.001(4) C36A 0.036(6) 0.050(6) 0.038(7) -0.002(5) 0.003(5) 0.007(5) C37A 0.036(6) 0.058(7) 0.057(8) 0.009(5) -0.003(5) 0.017(5) C38A 0.037(6) 0.058(6) 0.054(8) 0.009(5) 0.009(5) 0.022(5) C39A 0.043(6) 0.045(6) 0.040(7) 0.000(5) 0.002(5) 0.009(5) C40A 0.048(7) 0.062(7) 0.057(8) 0.017(6) 0.008(6) 0.031(6) C41A 0.064(9) 0.067(8) 0.098(12) 0.001(7) 0.007(8) 0.020(7) C42A 0.058(8) 0.070(8) 0.072(10) 0.030(7) 0.018(7) 0.032(6) C43A 0.064(9) 0.076(8) 0.113(13) 0.044(8) 0.043(8) 0.045(7) C44A 0.037(6) 0.054(6) 0.039(7) 0.013(5) 0.000(5) 0.014(5) C45A 0.043(6) 0.047(6) 0.034(6) 0.008(5) 0.003(5) 0.013(5) C46A 0.049(7) 0.044(6) 0.056(8) 0.011(5) 0.002(6) 0.020(5) C47A 0.043(6) 0.058(7) 0.054(8) 0.015(5) 0.014(5) 0.024(5) C48A 0.068(8) 0.059(7) 0.038(7) 0.010(5) 0.012(6) 0.018(6) C49A 0.050(7) 0.051(6) 0.054(8) 0.007(5) 0.003(6) 0.012(5) C50A 0.041(6) 0.050(6) 0.032(6) -0.003(5) -0.007(5) 0.013(5) C51A 0.052(7) 0.058(7) 0.057(8) 0.007(6) 0.008(6) 0.027(6) C52A 0.109(7) 0.113(7) 0.109(7) 0.026(5) 0.014(5) 0.042(5) C53A 0.105(6) 0.090(6) 0.096(7) 0.021(5) 0.004(5) 0.030(5) C54A 0.089(6) 0.087(6) 0.084(6) 0.019(4) 0.006(4) 0.031(4) C55A 0.056(7) 0.051(6) 0.047(8) 0.005(5) 0.001(6) 0.012(5) C56A 0.040(6) 0.061(7) 0.056(8) 0.014(5) 0.009(5) 0.026(5) O1B 0.043(4) 0.032(4) 0.048(5) 0.009(3) -0.001(3) 0.005(3) O2B 0.035(4) 0.029(4) 0.070(6) 0.006(3) 0.007(4) 0.006(3) O3B 0.048(5) 0.062(5) 0.055(5) 0.017(4) 0.004(4) 0.027(4) O4B 0.065(6) 0.067(5) 0.085(7) 0.019(5) 0.015(5) 0.026(5) O5B 0.063(5) 0.063(5) 0.049(5) -0.002(4) 0.008(4) 0.018(4) O6B 0.060(5) 0.066(5) 0.060(6) 0.016(4) 0.012(4) 0.018(4) C1B 0.059(7) 0.059(7) 0.038(7) 0.010(5) -0.009(6) 0.028(6) C2B 0.045(6) 0.035(5) 0.040(7) 0.009(4) -0.008(5) 0.008(5) C3B 0.043(6) 0.053(6) 0.044(7) 0.002(5) -0.008(5) 0.022(5) C4B 0.060(7) 0.041(6) 0.058(8) 0.010(5) -0.003(6) 0.012(5) C5B 0.083(9) 0.038(6) 0.049(8) -0.006(5) 0.003(7) 0.019(6) C6B 0.076(9) 0.045(7) 0.057(9) -0.001(5) 0.009(7) 0.016(6) C7B 0.078(5) 0.062(5) 0.065(5) 0.009(4) 0.008(4) 0.018(4) C8B 0.112(7) 0.108(7) 0.113(7) 0.016(5) 0.011(5) 0.033(5) C9B 0.132(8) 0.125(8) 0.128(8) 0.011(5) 0.026(5) 0.037(5) C10B 0.098(6) 0.087(6) 0.097(7) 0.016(4) 0.009(5) 0.033(4) C11B 0.033(6) 0.049(6) 0.086(10) 0.025(6) 0.011(6) 0.010(5) C12B 0.049(7) 0.037(5) 0.062(8) 0.015(5) 0.020(6) 0.020(5) C13B 0.034(6) 0.030(5) 0.053(7) 0.002(4) 0.014(5) 0.007(4) C14B 0.061(7) 0.052(6) 0.052(8) 0.024(5) 0.017(6) 0.026(6) C15B 0.067(8) 0.048(7) 0.050(8) 0.015(5) 0.015(6) 0.016(6) C16B 0.060(7) 0.039(6) 0.060(8) 0.010(5) 0.025(6) 0.019(5) C17B 0.057(7) 0.038(6) 0.049(8) 0.007(5) 0.000(6) 0.014(5) C18B 0.062(8) 0.044(6) 0.067(9) 0.015(6) 0.018(6) 0.007(6) C19B 0.095(10) 0.047(7) 0.087(11) 0.024(7) 0.044(9) 0.024(7) C20B 0.130(14) 0.075(9) 0.073(12) 0.021(8) 0.044(10) 0.023(9) C21B 0.073(10) 0.052(8) 0.137(15) 0.047(8) 0.020(9) 0.003(7) C22B 0.055(7) 0.047(6) 0.044(7) 0.001(5) 0.002(5) 0.019(5) C23B 0.051(7) 0.046(6) 0.060(8) 0.004(5) 0.009(6) 0.026(5) C24B 0.061(8) 0.062(7) 0.042(7) 0.005(5) -0.004(6) 0.030(6) C25B 0.055(7) 0.064(7) 0.050(8) 0.003(6) 0.001(6) 0.028(6) C26B 0.065(9) 0.060(7) 0.058(9) -0.007(6) -0.007(7) 0.022(6) C27B 0.087(10) 0.057(7) 0.041(8) 0.009(5) 0.004(6) 0.036(7) C28B 0.066(8) 0.054(7) 0.061(9) 0.017(6) 0.009(6) 0.033(6) C29B 0.082(10) 0.055(7) 0.076(10) 0.025(6) 0.009(8) 0.031(7) C30B 0.094(6) 0.082(6) 0.088(6) 0.013(4) 0.014(4) 0.036(4) C31B 0.084(6) 0.074(5) 0.072(6) 0.025(4) 0.008(4) 0.017(4) C32B 0.080(10) 0.084(9) 0.046(9) 0.003(7) 0.002(7) 0.031(7) C33B 0.048(7) 0.052(7) 0.072(10) 0.006(6) -0.003(6) 0.017(5) C34B 0.046(7) 0.052(7) 0.052(8) 0.002(5) -0.004(6) 0.003(5) C35B 0.036(6) 0.069(8) 0.055(9) 0.014(6) -0.002(6) 0.013(6) C36B 0.044(7) 0.051(7) 0.068(9) 0.010(6) 0.010(6) 0.009(5) C37B 0.055(8) 0.073(8) 0.059(9) 0.012(6) 0.013(6) 0.029(6) C38B 0.053(8) 0.060(7) 0.069(10) 0.007(6) 0.008(7) 0.008(6) C39B 0.076(9) 0.046(6) 0.062(9) 0.017(6) 0.006(7) 0.029(6) C40B 0.068(9) 0.070(8) 0.085(11) 0.026(7) 0.011(7) 0.043(7) C41B 0.106(7) 0.102(6) 0.101(7) 0.017(5) 0.011(5) 0.040(5) C42B 0.079(6) 0.075(5) 0.075(6) 0.017(4) 0.014(4) 0.029(4) C43B 0.088(6) 0.091(6) 0.094(6) 0.018(4) 0.019(4) 0.032(4) C44B 0.032(6) 0.073(8) 0.083(10) 0.023(7) 0.016(6) 0.021(6) C45B 0.046(7) 0.046(6) 0.067(9) 0.014(5) 0.021(6) 0.018(5) C46B 0.066(8) 0.040(6) 0.047(8) 0.005(5) 0.016(6) 0.009(5) C47B 0.069(8) 0.060(7) 0.030(7) 0.004(5) 0.011(6) 0.027(6) C48B 0.070(9) 0.061(7) 0.050(8) 0.019(6) 0.025(6) 0.028(6) C49B 0.062(9) 0.064(8) 0.089(12) 0.028(8) 0.021(8) 0.020(7) C50B 0.051(8) 0.072(8) 0.081(11) 0.030(7) 0.024(7) 0.030(7) C51B 0.065(8) 0.047(7) 0.096(12) 0.009(6) 0.035(8) 0.013(6) C52B 0.168(10) 0.167(10) 0.168(10) 0.025(3) 0.025(3) 0.058(4) C53B 0.139(8) 0.138(8) 0.141(8) 0.017(3) 0.024(3) 0.045(4) C54B 0.119(7) 0.119(7) 0.119(7) 0.017(3) 0.022(3) 0.038(3) C55B 0.055(8) 0.078(8) 0.045(8) 0.007(6) 0.011(6) 0.020(6) C56B 0.067(8) 0.053(7) 0.047(8) 0.018(5) 0.007(6) 0.028(6) N1 0.097(5) 0.089(4) 0.102(5) 0.019(3) 0.010(3) 0.035(3) N2 0.062(7) 0.046(6) 0.107(11) 0.010(6) -0.005(7) 0.014(5) C1 0.030(6) 0.078(8) 0.088(11) 0.002(7) 0.008(6) 0.020(6) C2 0.059(9) 0.059(9) 0.123(15) 0.005(8) 0.005(9) -0.002(7) C3 0.115(7) 0.115(6) 0.117(7) 0.010(3) 0.019(3) 0.038(3) C4 0.090(5) 0.092(5) 0.091(5) 0.013(3) 0.011(3) 0.031(3) C5 0.152(9) 0.155(9) 0.153(9) 0.029(3) 0.022(3) 0.048(4) C6 0.108(6) 0.112(6) 0.110(6) 0.014(3) 0.017(3) 0.036(3) N3 0.061(4) 0.056(3) 0.062(4) 0.007(3) 0.005(3) 0.020(3) N4 0.073(4) 0.071(4) 0.074(4) 0.012(3) 0.009(3) 0.029(3) C7 0.077(5) 0.076(5) 0.080(5) 0.016(3) 0.008(3) 0.027(3) C8 0.108(6) 0.108(6) 0.111(6) 0.020(3) 0.017(3) 0.035(3) C9 0.148(8) 0.146(8) 0.150(9) 0.022(3) 0.018(3) 0.051(4) C10 0.157(9) 0.155(9) 0.156(9) 0.025(3) 0.021(3) 0.052(4) C11 0.124(7) 0.122(7) 0.122(7) 0.020(3) 0.021(3) 0.042(4) C12 0.091(5) 0.088(5) 0.091(5) 0.014(3) 0.015(3) 0.033(3) N5 0.098(5) 0.097(5) 0.095(5) 0.017(3) 0.012(3) 0.031(3) C13 0.087(5) 0.087(5) 0.085(5) 0.014(3) 0.013(3) 0.028(3) C14 0.079(5) 0.076(5) 0.077(5) 0.015(3) 0.012(3) 0.024(3) C15 0.081(5) 0.078(5) 0.079(5) 0.010(3) 0.014(3) 0.025(3) C16 0.078(5) 0.078(5) 0.080(5) 0.015(3) 0.010(3) 0.025(3) C17 0.079(5) 0.083(5) 0.080(5) 0.017(3) 0.010(3) 0.024(3) N6 0.113(5) 0.112(5) 0.114(5) 0.018(3) 0.019(3) 0.035(3) C18 0.078(5) 0.079(5) 0.078(5) 0.013(3) 0.013(3) 0.025(3) C19 0.130(7) 0.130(7) 0.129(7) 0.020(3) 0.019(3) 0.044(4) C20 0.108(6) 0.106(6) 0.105(6) 0.015(3) 0.014(3) 0.039(3) C21 0.119(7) 0.119(7) 0.116(7) 0.017(3) 0.017(3) 0.042(3) C22 0.085(5) 0.088(5) 0.085(5) 0.013(3) 0.014(3) 0.030(3) N7 0.108(5) 0.108(5) 0.109(5) 0.016(3) 0.018(3) 0.034(3) C23 0.080(5) 0.080(5) 0.083(5) 0.012(3) 0.008(3) 0.028(3) C24 0.077(5) 0.077(5) 0.075(5) 0.012(3) 0.009(3) 0.024(3) C25 0.078(5) 0.077(5) 0.080(5) 0.011(3) 0.013(3) 0.027(3) C26 0.079(5) 0.080(5) 0.085(5) 0.011(3) 0.009(3) 0.029(3) C27 0.096(6) 0.097(6) 0.099(6) 0.015(3) 0.014(3) 0.030(3) N8 0.076(7) 0.078(7) 0.078(7) 0.007(3) 0.017(3) 0.024(3) C28 0.086(9) 0.090(9) 0.087(9) 0.012(3) 0.015(3) 0.029(4) C29 0.064(7) 0.065(7) 0.065(7) 0.011(3) 0.014(3) 0.020(4) C30 0.091(10) 0.091(10) 0.092(10) 0.013(3) 0.014(3) 0.029(4) C31 0.092(10) 0.095(10) 0.093(10) 0.013(3) 0.013(3) 0.031(4) C32 0.093(10) 0.094(10) 0.096(10) 0.016(3) 0.014(3) 0.032(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O2 1.787(6) . ? U O1 1.799(6) . ? U O1A 2.238(7) . ? U O2B 2.243(7) . ? U O1B 2.251(6) . ? U O2A 2.251(7) . ? U O6B 4.123(8) . ? U O6A 4.285(8) . ? O1A C2A 1.379(11) . ? O1A O2A 3.169(10) . ? O1A O6A 3.441(11) . ? O1A O5A 5.145(10) . ? O2A C13A 1.361(11) . ? O2A O3A 4.500(10) . ? O3A C24A 1.407(12) . ? O3A O4A 2.734(10) . ? O4A C35A 1.398(12) . ? O4A O5A 3.286(11) . ? O5A C46A 1.358(12) . ? O5A O6A 3.488(10) . ? O6A C56A 1.420(12) . ? O6A C55A 1.428(12) . ? C1A C6A 1.395(14) . ? C1A C2A 1.418(15) . ? C1A C56A 1.489(14) . ? C2A C3A 1.393(15) . ? C3A C4A 1.414(14) . ? C3A C11A 1.492(16) . ? C4A C5A 1.390(16) . ? C5A C6A 1.378(16) . ? C5A C7A 1.545(15) . ? C7A C8A 1.519(17) . ? C7A C10A 1.529(17) . ? C7A C9A 1.535(19) . ? C11A C12A 1.511(15) . ? C12A C13A 1.344(14) . ? C12A C17A 1.416(13) . ? C13A C14A 1.444(14) . ? C14A C15A 1.404(13) . ? C14A C22A 1.501(14) . ? C15A C16A 1.400(14) . ? C16A C17A 1.389(14) . ? C16A C18A 1.506(14) . ? C18A C20A 1.488(17) . ? C18A C21A 1.508(17) . ? C18A C19A 1.572(16) . ? C22A C23A 1.515(13) . ? C23A C24A 1.358(14) . ? C23A C28A 1.409(14) . ? C24A C25A 1.408(14) . ? C25A C26A 1.399(15) . ? C25A C33A 1.536(14) . ? C26A C27A 1.420(14) . ? C27A C28A 1.365(14) . ? C27A C29A 1.514(14) . ? C29A C31A 1.502(15) . ? C29A C30A 1.521(16) . ? C29A C32A 1.567(16) . ? C33A C34A 1.525(15) . ? C34A C35A 1.370(14) . ? C34A C39A 1.387(14) . ? C35A C36A 1.388(14) . ? C36A C37A 1.390(14) . ? C36A C44A 1.489(14) . ? C37A C38A 1.400(15) . ? C38A C39A 1.426(15) . ? C38A C40A 1.526(14) . ? C40A C43A 1.480(16) . ? C40A C42A 1.520(16) . ? C40A C41A 1.539(16) . ? C44A C45A 1.501(14) . ? C45A C50A 1.373(14) . ? C45A C46A 1.395(14) . ? C46A C47A 1.410(15) . ? C47A C48A 1.393(15) . ? C47A C55A 1.460(15) . ? C48A C49A 1.385(15) . ? C49A C50A 1.374(15) . ? C49A C51A 1.535(15) . ? C51A C52A 1.485(19) . ? C51A C54A 1.497(18) . ? C51A C53A 1.611(17) . ? O1B C2B 1.342(11) . ? O1B O2B 3.149(11) . ? O1B O6B 3.421(11) . ? O1B O5B 5.117(10) . ? O2B C13B 1.367(11) . ? O2B O3B 4.317(10) . ? O3B C24B 1.388(13) . ? O3B O4B 2.720(12) . ? O4B C35B 1.385(13) . ? O4B O5B 3.196(12) . ? O5B C46B 1.354(13) . ? O5B O6B 3.409(11) . ? O6B C56B 1.426(13) . ? O6B C55B 1.463(13) . ? C1B C6B 1.395(15) . ? C1B C2B 1.415(15) . ? C1B C56B 1.464(16) . ? C2B C3B 1.384(15) . ? C3B C4B 1.393(14) . ? C3B C11B 1.510(16) . ? C4B C5B 1.378(16) . ? C5B C6B 1.381(17) . ? C5B C7B 1.575(16) . ? C7B C10B 1.466(19) . ? C7B C9B 1.51(2) . ? C7B C8B 1.61(2) . ? C11B C12B 1.472(16) . ? C12B C17B 1.390(13) . ? C12B C13B 1.436(14) . ? C13B C14B 1.388(15) . ? C14B C15B 1.411(14) . ? C14B C22B 1.519(15) . ? C15B C16B 1.387(16) . ? C16B C17B 1.391(15) . ? C16B C18B 1.560(14) . ? C18B C19B 1.515(16) . ? C18B C21B 1.534(17) . ? C18B C20B 1.562(19) . ? C22B C23B 1.487(14) . ? C23B C24B 1.376(16) . ? C23B C28B 1.429(15) . ? C24B C25B 1.418(15) . ? C25B C26B 1.372(17) . ? C25B C33B 1.504(16) . ? C26B C27B 1.425(18) . ? C27B C28B 1.386(16) . ? C27B C29B 1.542(16) . ? C29B C32B 1.527(18) . ? C29B C30B 1.535(18) . ? C29B C31B 1.554(18) . ? C33B C34B 1.521(17) . ? C34B C35B 1.362(16) . ? C34B C39B 1.439(15) . ? C35B C36B 1.389(17) . ? C36B C37B 1.420(16) . ? C36B C44B 1.524(17) . ? C37B C38B 1.373(17) . ? C38B C39B 1.397(17) . ? C38B C40B 1.503(16) . ? C40B C42B 1.512(18) . ? C40B C41B 1.51(2) . ? C40B C43B 1.572(19) . ? C44B C45B 1.496(16) . ? C45B C50B 1.352(16) . ? C45B C46B 1.427(16) . ? C46B C47B 1.396(15) . ? C47B C48B 1.391(15) . ? C47B C55B 1.493(16) . ? C48B C49B 1.396(17) . ? C49B C50B 1.382(19) . ? C49B C51B 1.532(18) . ? C51B C53B 1.47(2) . ? C51B C54B 1.48(2) . ? C51B C52B 1.62(3) . ? N1 C3 1.39(2) . ? N1 C5 1.51(2) . ? N1 C1 1.509(16) . ? N2 C6 1.42(2) . ? N2 C4 1.431(18) . ? N2 C2 1.475(17) . ? C1 C2 1.520(17) . ? C3 C4 1.54(2) . ? C5 C6 1.45(2) . ? N3 C9 1.41(2) . ? N3 C7 1.456(16) . ? N3 C11 1.50(2) . ? N4 C8 1.408(18) . ? N4 C10 1.43(2) . ? N4 C12 1.430(18) . ? C7 C8 1.568(19) . ? C9 C10 1.54(3) . ? C11 C12 1.50(2) . ? N5 C13 1.315(18) . ? N5 C17 1.340(17) . ? C13 C14 1.356(19) . ? C14 C15 1.353(18) . ? C15 C16 1.382(19) . ? C16 C17 1.360(18) . ? N6 C18 1.332(19) . ? N6 C22 1.371(19) . ? C18 C19 1.31(2) . ? C19 C20 1.43(2) . ? C20 C21 1.34(2) . ? C21 C22 1.36(2) . ? N7 C23 1.376(18) . ? N7 C27 1.394(19) . ? C23 C24 1.339(17) . ? C24 C25 1.343(18) . ? C25 C26 1.300(18) . ? C26 C27 1.323(19) . ? N8 C28 1.3900 . ? N8 C32 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U O1 179.3(4) . . ? O2 U O1A 90.7(3) . . ? O1 U O1A 89.9(3) . . ? O2 U O2B 90.1(2) . . ? O1 U O2B 89.3(2) . . ? O1A U O2B 174.00(19) . . ? O2 U O1B 90.0(2) . . ? O1 U O1B 90.4(2) . . ? O1A U O1B 96.98(19) . . ? O2B U O1B 89.0(2) . . ? O2 U O2A 90.3(3) . . ? O1 U O2A 89.3(3) . . ? O1A U O2A 89.8(3) . . ? O2B U O2A 84.24(19) . . ? O1B U O2A 173.21(19) . . ? C2A O1A U 135.3(6) . . ? C13A O2A U 124.4(6) . . ? C56A O6A C55A 112.0(8) . . ? C6A C1A C2A 120.2(10) . . ? C6A C1A C56A 120.7(11) . . ? C2A C1A C56A 119.0(9) . . ? O1A C2A C3A 120.8(9) . . ? O1A C2A C1A 119.0(9) . . ? C3A C2A C1A 120.2(9) . . ? C2A C3A C4A 116.7(11) . . ? C2A C3A C11A 123.0(9) . . ? C4A C3A C11A 119.8(11) . . ? C5A C4A C3A 124.2(12) . . ? C6A C5A C4A 117.5(10) . . ? C6A C5A C7A 122.6(11) . . ? C4A C5A C7A 119.9(11) . . ? C5A C6A C1A 121.2(11) . . ? C8A C7A C10A 112.0(11) . . ? C8A C7A C9A 108.5(11) . . ? C10A C7A C9A 106.0(12) . . ? C8A C7A C5A 109.9(11) . . ? C10A C7A C5A 109.1(10) . . ? C9A C7A C5A 111.3(10) . . ? C3A C11A C12A 112.9(9) . . ? C13A C12A C17A 119.8(10) . . ? C13A C12A C11A 122.4(9) . . ? C17A C12A C11A 117.7(9) . . ? C12A C13A O2A 121.3(10) . . ? C12A C13A C14A 120.5(9) . . ? O2A C13A C14A 118.2(9) . . ? C15A C14A C13A 116.0(9) . . ? C15A C14A C22A 123.1(10) . . ? C13A C14A C22A 120.7(8) . . ? C16A C15A C14A 125.9(10) . . ? C17A C16A C15A 113.5(9) . . ? C17A C16A C18A 125.2(10) . . ? C15A C16A C18A 120.9(10) . . ? C16A C17A C12A 124.0(10) . . ? C20A C18A C16A 109.9(10) . . ? C20A C18A C21A 111.4(11) . . ? C16A C18A C21A 111.4(10) . . ? C20A C18A C19A 107.9(11) . . ? C16A C18A C19A 110.8(9) . . ? C21A C18A C19A 105.3(10) . . ? C14A C22A C23A 118.5(8) . . ? C24A C23A C28A 117.3(9) . . ? C24A C23A C22A 123.1(9) . . ? C28A C23A C22A 119.5(9) . . ? C23A C24A O3A 125.7(9) . . ? C23A C24A C25A 121.6(10) . . ? O3A C24A C25A 112.7(9) . . ? C26A C25A C24A 118.9(10) . . ? C26A C25A C33A 119.1(10) . . ? C24A C25A C33A 121.8(10) . . ? C25A C26A C27A 121.2(10) . . ? C28A C27A C26A 116.1(9) . . ? C28A C27A C29A 124.5(9) . . ? C26A C27A C29A 119.2(9) . . ? C27A C28A C23A 124.9(10) . . ? C31A C29A C27A 111.3(10) . . ? C31A C29A C30A 108.4(10) . . ? C27A C29A C30A 111.5(9) . . ? C31A C29A C32A 110.1(10) . . ? C27A C29A C32A 108.8(9) . . ? C30A C29A C32A 106.6(10) . . ? C34A C33A C25A 114.4(9) . . ? C35A C34A C39A 117.6(11) . . ? C35A C34A C33A 123.9(10) . . ? C39A C34A C33A 118.3(10) . . ? C34A C35A C36A 122.8(10) . . ? C34A C35A O4A 119.8(10) . . ? C36A C35A O4A 117.1(9) . . ? C35A C36A C37A 118.2(10) . . ? C35A C36A C44A 123.3(10) . . ? C37A C36A C44A 118.4(10) . . ? C36A C37A C38A 122.6(11) . . ? C37A C38A C39A 115.6(10) . . ? C37A C38A C40A 123.1(10) . . ? C39A C38A C40A 121.3(10) . . ? C34A C39A C38A 123.0(10) . . ? C43A C40A C42A 108.4(10) . . ? C43A C40A C38A 107.5(9) . . ? C42A C40A C38A 112.6(10) . . ? C43A C40A C41A 109.9(11) . . ? C42A C40A C41A 107.2(10) . . ? C38A C40A C41A 111.1(10) . . ? C36A C44A C45A 116.2(9) . . ? C50A C45A C46A 118.8(10) . . ? C50A C45A C44A 121.7(10) . . ? C46A C45A C44A 119.4(9) . . ? O5A C46A C45A 115.5(10) . . ? O5A C46A C47A 123.4(10) . . ? C45A C46A C47A 121.1(10) . . ? C48A C47A C46A 117.1(10) . . ? C48A C47A C55A 120.7(11) . . ? C46A C47A C55A 122.2(10) . . ? C49A C48A C47A 122.0(11) . . ? C50A C49A C48A 118.9(11) . . ? C50A C49A C51A 122.3(11) . . ? C48A C49A C51A 118.8(10) . . ? C45A C50A C49A 121.8(10) . . ? C52A C51A C54A 109.1(12) . . ? C52A C51A C49A 115.0(11) . . ? C54A C51A C49A 112.2(10) . . ? C52A C51A C53A 104.3(11) . . ? C54A C51A C53A 106.5(11) . . ? C49A C51A C53A 109.0(10) . . ? O6A C55A C47A 109.1(9) . . ? O6A C56A C1A 110.5(9) . . ? C2B O1B U 133.4(6) . . ? C13B O2B U 132.3(6) . . ? C56B O6B C55B 110.9(9) . . ? C6B C1B C2B 118.3(11) . . ? C6B C1B C56B 121.3(11) . . ? C2B C1B C56B 120.3(10) . . ? O1B C2B C3B 120.7(10) . . ? O1B C2B C1B 120.4(10) . . ? C3B C2B C1B 118.9(9) . . ? C2B C3B C4B 121.1(11) . . ? C2B C3B C11B 121.5(9) . . ? C4B C3B C11B 117.2(11) . . ? C5B C4B C3B 120.8(12) . . ? C4B C5B C6B 118.2(10) . . ? C4B C5B C7B 120.1(12) . . ? C6B C5B C7B 121.7(11) . . ? C5B C6B C1B 122.7(12) . . ? C10B C7B C9B 120.8(14) . . ? C10B C7B C5B 109.9(12) . . ? C9B C7B C5B 111.6(12) . . ? C10B C7B C8B 103.8(13) . . ? C9B C7B C8B 100.0(13) . . ? C5B C7B C8B 109.4(11) . . ? C12B C11B C3B 112.8(9) . . ? C17B C12B C13B 117.5(10) . . ? C17B C12B C11B 120.0(10) . . ? C13B C12B C11B 122.4(9) . . ? O2B C13B C14B 120.9(9) . . ? O2B C13B C12B 117.7(9) . . ? C14B C13B C12B 121.4(9) . . ? C13B C14B C15B 117.5(11) . . ? C13B C14B C22B 120.9(9) . . ? C15B C14B C22B 121.3(10) . . ? C16B C15B C14B 123.0(11) . . ? C15B C16B C17B 117.5(9) . . ? C15B C16B C18B 120.0(11) . . ? C17B C16B C18B 122.4(11) . . ? C12B C17B C16B 122.9(10) . . ? C19B C18B C21B 109.0(11) . . ? C19B C18B C16B 109.2(10) . . ? C21B C18B C16B 109.6(10) . . ? C19B C18B C20B 111.2(11) . . ? C21B C18B C20B 106.6(12) . . ? C16B C18B C20B 111.2(10) . . ? C23B C22B C14B 120.3(9) . . ? C24B C23B C28B 115.0(10) . . ? C24B C23B C22B 124.3(10) . . ? C28B C23B C22B 120.6(10) . . ? C23B C24B O3B 123.4(10) . . ? C23B C24B C25B 123.1(11) . . ? O3B C24B C25B 113.4(11) . . ? C26B C25B C24B 119.2(12) . . ? C26B C25B C33B 118.1(11) . . ? C24B C25B C33B 122.6(11) . . ? C25B C26B C27B 121.3(12) . . ? C28B C27B C26B 116.4(11) . . ? C28B C27B C29B 122.7(12) . . ? C26B C27B C29B 120.8(11) . . ? C27B C28B C23B 124.8(12) . . ? C32B C29B C30B 108.1(11) . . ? C32B C29B C27B 109.6(10) . . ? C30B C29B C27B 109.9(12) . . ? C32B C29B C31B 112.0(12) . . ? C30B C29B C31B 106.8(10) . . ? C27B C29B C31B 110.3(11) . . ? C25B C33B C34B 115.9(9) . . ? C35B C34B C39B 119.1(12) . . ? C35B C34B C33B 121.5(11) . . ? C39B C34B C33B 119.3(11) . . ? C34B C35B O4B 121.6(12) . . ? C34B C35B C36B 120.8(12) . . ? O4B C35B C36B 117.4(11) . . ? C35B C36B C37B 118.8(12) . . ? C35B C36B C44B 121.4(11) . . ? C37B C36B C44B 119.7(12) . . ? C38B C37B C36B 122.6(12) . . ? C37B C38B C39B 117.1(12) . . ? C37B C38B C40B 122.1(13) . . ? C39B C38B C40B 120.7(12) . . ? C38B C39B C34B 121.4(12) . . ? C38B C40B C42B 114.2(12) . . ? C38B C40B C41B 109.7(12) . . ? C42B C40B C41B 108.4(12) . . ? C38B C40B C43B 106.9(11) . . ? C42B C40B C43B 105.9(12) . . ? C41B C40B C43B 111.7(13) . . ? C45B C44B C36B 113.2(10) . . ? C50B C45B C46B 118.2(12) . . ? C50B C45B C44B 123.0(11) . . ? C46B C45B C44B 118.9(10) . . ? O5B C46B C47B 123.7(11) . . ? O5B C46B C45B 117.2(10) . . ? C47B C46B C45B 119.0(11) . . ? C48B C47B C46B 120.0(12) . . ? C48B C47B C55B 119.3(11) . . ? C46B C47B C55B 120.7(10) . . ? C47B C48B C49B 121.1(13) . . ? C50B C49B C48B 117.1(13) . . ? C50B C49B C51B 124.1(13) . . ? C48B C49B C51B 118.8(13) . . ? C45B C50B C49B 124.5(13) . . ? C53B C51B C54B 112.9(16) . . ? C53B C51B C49B 113.0(13) . . ? C54B C51B C49B 110.2(12) . . ? C53B C51B C52B 105.0(14) . . ? C54B C51B C52B 104.8(14) . . ? C49B C51B C52B 110.6(14) . . ? O6B C55B C47B 110.2(10) . . ? O6B C56B C1B 112.3(9) . . ? C3 N1 C5 110.7(16) . . ? C3 N1 C1 112.8(14) . . ? C5 N1 C1 106.8(14) . . ? C6 N2 C4 104.7(13) . . ? C6 N2 C2 111.4(13) . . ? C4 N2 C2 110.8(12) . . ? N1 C1 C2 105.4(10) . . ? N2 C2 C1 110.9(10) . . ? N1 C3 C4 106.4(15) . . ? N2 C4 C3 110.9(13) . . ? C6 C5 N1 109.8(18) . . ? N2 C6 C5 110.8(17) . . ? C9 N3 C7 115.0(14) . . ? C9 N3 C11 110.8(14) . . ? C7 N3 C11 104.4(11) . . ? C8 N4 C10 105.4(14) . . ? C8 N4 C12 107.6(13) . . ? C10 N4 C12 107.4(14) . . ? N3 C7 C8 104.8(12) . . ? N4 C8 C7 114.8(13) . . ? N3 C9 C10 107.6(17) . . ? N4 C10 C9 113.0(19) . . ? C12 C11 N3 106.9(15) . . ? N4 C12 C11 113.8(14) . . ? C13 N5 C17 115.7(14) . . ? N5 C13 C14 124.6(15) . . ? C15 C14 C13 118.1(16) . . ? C14 C15 C16 120.4(14) . . ? C17 C16 C15 116.2(14) . . ? N5 C17 C16 125.0(16) . . ? C18 N6 C22 116.8(16) . . ? C19 C18 N6 122.4(18) . . ? C18 C19 C20 121(2) . . ? C21 C20 C19 118(2) . . ? C20 C21 C22 118(2) . . ? C21 C22 N6 123.3(18) . . ? C23 N7 C27 113.8(14) . . ? C24 C23 N7 122.4(15) . . ? C23 C24 C25 119.3(15) . . ? C26 C25 C24 121.3(14) . . ? C25 C26 C27 120.0(16) . . ? C26 C27 N7 122.9(17) . . ? C28 N8 C32 120.0 . . ? N8 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C31 C32 N8 120.0 . . ? 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 O3A H3A O2B 0.96 1.83 2.710(7) 151.0 . O4A H4A O3A 0.91 1.91 2.734(10) 150.2 . O5A H5A O1B 0.77 2.02 2.766(7) 162.5 . O3B H3B O2A 0.92 1.85 2.697(7) 151.2 . O4B H4B O3B 0.89 1.91 2.720(12) 150.4 . O5B H5B O4B 0.96 2.26 3.196(12) 166.2 . N1 H1 O1 0.91 1.79 2.668(13) 161.8 . N3 H3 O2 1.00 1.81 2.718(10) 149.3 . #===END data_19 _database_code_depnum_ccdc_archive 'CCDC 255526' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C178 H244 N20 O28 U4' _chemical_formula_weight 4064.05 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4500(14) _cell_length_b 19.1428(16) _cell_length_c 20.2899(18) _cell_angle_alpha 117.130(6) _cell_angle_beta 102.485(7) _cell_angle_gamma 96.117(7) _cell_volume 4411.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23830 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method ? _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 3.734 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 0.688 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 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_decay_% none _diffrn_reflns_number 23830 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.1087 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14405 _reflns_number_gt 4660 _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. Some constraints on bond lengths were applied for one tert-butyl group and some parts of DABCO and pyridine molecules. Some restraints on displacement parameters (ISOR) were applied for the tert-butyl terminal carbon atoms and the DABCO, pyridine and water molecules. The H atoms were introduced at calculated positions (except those of the water molecule) 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. 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^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14405 _refine_ls_number_parameters 1049 _refine_ls_number_restraints 380 _refine_ls_R_factor_all 0.2695 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.2386 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.860 _refine_diff_density_max 1.066 _refine_diff_density_min -1.123 _refine_diff_density_rms 0.135 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 0.63602(7) 0.84798(6) 0.27396(5) 0.0614(3) Uani 1 1 d . . . U2 U 0.93984(7) 0.88817(6) 0.49212(6) 0.0634(4) Uani 1 1 d . . . O1 O 0.6187(11) 0.9392(9) 0.2319(8) 0.071(5) Uani 1 1 d . . . O2 O 0.5002(11) 0.7845(9) 0.1716(9) 0.068(5) Uani 1 1 d . . . O3 O 0.5973(10) 0.7270(8) 0.2745(8) 0.055(4) Uani 1 1 d . . . O4 O 0.8332(10) 0.7801(9) 0.4587(9) 0.064(4) Uani 1 1 d . . . O5 O 1.0405(11) 0.8477(9) 0.5605(9) 0.068(4) Uani 1 1 d . . . O6 O 1.1846(11) 0.9587(8) 0.7859(8) 0.067(5) Uani 1 1 d . . . O7 O 0.7233(10) 0.8068(9) 0.2194(10) 0.074(5) Uani 1 1 d . . . O8 O 0.5582(10) 0.8907(8) 0.3345(9) 0.057(4) Uani 1 1 d . . . O9 O 0.9918(10) 0.8433(9) 0.4123(8) 0.069(5) Uani 1 1 d . . . O10 O 0.8848(10) 0.9415(10) 0.5693(9) 0.075(5) Uani 1 1 d . . . O11 O 0.7826(12) 0.8816(9) 0.3937(9) 0.072(5) Uani 1 1 d . . . O12 O 0.7741(14) 0.9750(10) 0.3537(10) 0.075(6) Uani 1 1 d . . . O13 O 0.9186(12) 0.9922(10) 0.4521(9) 0.081(6) Uani 1 1 d . . . N1 N 0.827(2) 0.9551(14) 0.3975(15) 0.064(7) Uani 1 1 d . . . C1 C 0.6690(19) 0.9284(13) 0.1220(15) 0.074(7) Uani 1 1 d . . . C2 C 0.5916(17) 0.9256(12) 0.1567(14) 0.059(7) Uani 1 1 d . . . C3 C 0.4826(16) 0.8976(12) 0.1097(13) 0.059(7) Uani 1 1 d . . . C4 C 0.461(2) 0.8734(13) 0.0303(12) 0.072(8) Uani 1 1 d . . . H4A H 0.3912 0.8531 0.0001 0.087 Uiso 1 1 calc R . . C5 C 0.5352(18) 0.8772(13) -0.0068(14) 0.068(7) Uani 1 1 d . . . C6 C 0.6388(18) 0.9073(14) 0.0420(16) 0.071(7) Uani 1 1 d . . . H6 H 0.6915 0.9140 0.0209 0.085 Uiso 1 1 calc R . . C7 C 0.504(2) 0.8489(15) -0.0908(13) 0.070(8) Uani 1 1 d D . . C8 C 0.494(5) 0.7583(18) -0.135(3) 0.13(3) Uani 1 1 d DU . . H8A H 0.5571 0.7457 -0.1162 0.197 Uiso 1 1 calc R . . H8B H 0.4809 0.7408 -0.1894 0.197 Uiso 1 1 calc R . . H8C H 0.4362 0.7312 -0.1280 0.197 Uiso 1 1 calc R . . C9 C 0.405(2) 0.8760(19) -0.1172(18) 0.112(11) Uani 1 1 d U . . H9A H 0.3457 0.8493 -0.1114 0.168 Uiso 1 1 calc R . . H9B H 0.3924 0.8620 -0.1707 0.168 Uiso 1 1 calc R . . H9C H 0.4161 0.9334 -0.0858 0.168 Uiso 1 1 calc R . . C10 C 0.582(2) 0.8915(18) -0.1122(17) 0.116(11) Uani 1 1 d U . . H10A H 0.5566 0.8741 -0.1665 0.174 Uiso 1 1 calc R . . H10B H 0.6482 0.8788 -0.1009 0.174 Uiso 1 1 calc R . . H10C H 0.5894 0.9488 -0.0826 0.174 Uiso 1 1 calc R . . C11 C 0.3983(16) 0.8912(12) 0.1436(12) 0.055(6) Uani 1 1 d . . . H11A H 0.3478 0.9198 0.1322 0.066 Uiso 1 1 calc R . . H11B H 0.4278 0.9176 0.1996 0.066 Uiso 1 1 calc R . . C12 C 0.3418(17) 0.8051(14) 0.1142(14) 0.061(7) Uani 1 1 d . . . C13 C 0.3963(15) 0.7571(17) 0.1320(13) 0.065(7) Uani 1 1 d . . . C14 C 0.3471(17) 0.6783(16) 0.1140(13) 0.063(7) Uani 1 1 d . . . C15 C 0.2441(16) 0.6494(14) 0.0757(13) 0.061(7) Uani 1 1 d . . . H15 H 0.2115 0.5964 0.0592 0.073 Uiso 1 1 calc R . . C16 C 0.1816(17) 0.7047(17) 0.0601(15) 0.071(7) Uani 1 1 d . . . C17 C 0.2351(19) 0.7803(15) 0.0810(13) 0.074(8) Uani 1 1 d . . . H17 H 0.1984 0.8155 0.0726 0.088 Uiso 1 1 calc R . . C18 C 0.0588(19) 0.6721(16) 0.0204(16) 0.071(7) Uani 1 1 d U . . C19 C 0.036(2) 0.6656(17) -0.0592(16) 0.110(10) Uani 1 1 d U . . H19A H 0.0664 0.6243 -0.0913 0.166 Uiso 1 1 calc R . . H19B H 0.0666 0.7164 -0.0538 0.166 Uiso 1 1 calc R . . H19C H -0.0380 0.6519 -0.0829 0.166 Uiso 1 1 calc R . . C20 C 0.018(2) 0.5876(17) 0.0042(17) 0.107(10) Uani 1 1 d U . . H20A H -0.0570 0.5736 -0.0146 0.160 Uiso 1 1 calc R . . H20B H 0.0402 0.5850 0.0512 0.160 Uiso 1 1 calc R . . H20C H 0.0454 0.5504 -0.0342 0.160 Uiso 1 1 calc R . . C21 C 0.012(2) 0.7304(19) 0.0740(18) 0.118(11) Uani 1 1 d U . . H21A H 0.0072 0.7735 0.0625 0.178 Uiso 1 1 calc R . . H21B H 0.0559 0.7520 0.1264 0.178 Uiso 1 1 calc R . . H21C H -0.0562 0.7039 0.0682 0.178 Uiso 1 1 calc R . . C22 C 0.4093(17) 0.6316(14) 0.1362(13) 0.067(7) Uani 1 1 d . . . H22A H 0.4786 0.6438 0.1317 0.080 Uiso 1 1 calc R . . H22B H 0.3782 0.5748 0.0995 0.080 Uiso 1 1 calc R . . C23 C 0.4215(17) 0.6448(12) 0.2175(15) 0.060(7) Uani 1 1 d . . . C24 C 0.5089(17) 0.6927(14) 0.2818(14) 0.066(7) Uani 1 1 d . . . C25 C 0.5065(16) 0.6985(13) 0.3526(13) 0.051(6) Uani 1 1 d . . . C26 C 0.4211(16) 0.6649(13) 0.3623(14) 0.068(7) Uani 1 1 d . . . H26 H 0.4215 0.6741 0.4115 0.081 Uiso 1 1 calc R . . C27 C 0.3265(16) 0.6134(14) 0.2950(13) 0.054(6) Uani 1 1 d . . . C28 C 0.3359(15) 0.6086(13) 0.2284(13) 0.061(7) Uani 1 1 d . . . H28 H 0.2784 0.5775 0.1846 0.073 Uiso 1 1 calc R . . C29 C 0.235(2) 0.5700(17) 0.3051(14) 0.083(9) Uani 1 1 d . . . C30 C 0.201(3) 0.627(2) 0.371(2) 0.138(13) Uani 1 1 d U . . H30A H 0.1458 0.5975 0.3783 0.208 Uiso 1 1 calc R . . H30B H 0.1767 0.6670 0.3605 0.208 Uiso 1 1 calc R . . H30C H 0.2596 0.6530 0.4179 0.208 Uiso 1 1 calc R . . C31 C 0.1439(17) 0.5276(14) 0.2327(14) 0.078(7) Uani 1 1 d U . . H31A H 0.1536 0.4758 0.1986 0.117 Uiso 1 1 calc R . . H31B H 0.1389 0.5594 0.2073 0.117 Uiso 1 1 calc R . . H31C H 0.0805 0.5205 0.2459 0.117 Uiso 1 1 calc R . . C32 C 0.268(2) 0.5094(18) 0.3277(17) 0.101(10) Uani 1 1 d U . . H32A H 0.2079 0.4771 0.3270 0.152 Uiso 1 1 calc R . . H32B H 0.3171 0.5373 0.3790 0.152 Uiso 1 1 calc R . . H32C H 0.3010 0.4752 0.2916 0.152 Uiso 1 1 calc R . . C33 C 0.6058(15) 0.7387(12) 0.4193(12) 0.056(6) Uani 1 1 d . . . H33A H 0.5875 0.7628 0.4674 0.067 Uiso 1 1 calc R . . H33B H 0.6448 0.7820 0.4160 0.067 Uiso 1 1 calc R . . C34 C 0.6789(16) 0.6810(14) 0.4229(14) 0.061(7) Uani 1 1 d . . . C35 C 0.7873(13) 0.7038(12) 0.4421(11) 0.042(5) Uani 1 1 d U . . C36 C 0.8450(14) 0.6491(11) 0.4447(13) 0.047(5) Uani 1 1 d . . . C37 C 0.7972(15) 0.5764(12) 0.4283(12) 0.056(6) Uani 1 1 d . . . H37 H 0.8400 0.5429 0.4332 0.068 Uiso 1 1 calc R . . C38 C 0.6878(17) 0.5444(11) 0.4040(13) 0.066(7) Uani 1 1 d D . . C39 C 0.634(2) 0.6016(16) 0.4068(14) 0.072(8) Uani 1 1 d . . . H39 H 0.5623 0.5879 0.3974 0.086 Uiso 1 1 calc R . . C40 C 0.6470(16) 0.4588(12) 0.3797(13) 0.098(13) Uani 1 1 d DU . . C41 C 0.682(3) 0.4456(19) 0.4462(18) 0.158(19) Uani 1 1 d DU . . H41A H 0.6299 0.4532 0.4731 0.236 Uiso 1 1 calc R . . H41B H 0.7470 0.4835 0.4808 0.236 Uiso 1 1 calc R . . H41C H 0.6912 0.3916 0.4279 0.236 Uiso 1 1 calc R . . C42 C 0.5323(15) 0.4377(18) 0.3501(19) 0.108(14) Uani 1 1 d DU . . H42A H 0.5053 0.3866 0.3454 0.162 Uiso 1 1 calc R . . H42B H 0.5112 0.4342 0.3001 0.162 Uiso 1 1 calc R . . H42C H 0.5051 0.4786 0.3854 0.162 Uiso 1 1 calc R . . C43 C 0.689(3) 0.4073(16) 0.3170(18) 0.105(19) Uani 1 1 d DU . . H43A H 0.6697 0.4177 0.2745 0.158 Uiso 1 1 calc R . . H43B H 0.6609 0.3514 0.2995 0.158 Uiso 1 1 calc R . . H43C H 0.7641 0.4194 0.3365 0.158 Uiso 1 1 calc R . . C44 C 0.9660(16) 0.6767(14) 0.4699(13) 0.065(7) Uani 1 1 d . . . H44A H 0.9955 0.6300 0.4490 0.078 Uiso 1 1 calc R . . H44B H 0.9859 0.7113 0.4495 0.078 Uiso 1 1 calc R . . C45 C 1.0094(15) 0.7232(16) 0.5593(15) 0.072(8) Uani 1 1 d . . . C46 C 1.0355(14) 0.8041(14) 0.5962(14) 0.052(6) Uani 1 1 d . . . C47 C 1.0672(17) 0.8427(13) 0.6787(15) 0.063(7) Uani 1 1 d . . . C48 C 1.0635(19) 0.7972(15) 0.7201(17) 0.081(8) Uani 1 1 d . . . H48 H 1.0765 0.8235 0.7737 0.097 Uiso 1 1 calc R . . C49 C 1.0401(19) 0.7144(17) 0.6771(18) 0.081(8) Uani 1 1 d . . . C50 C 1.0085(15) 0.6762(13) 0.5948(16) 0.065(7) Uani 1 1 d . . . H50 H 0.9875 0.6202 0.5650 0.078 Uiso 1 1 calc R . . C51 C 1.0416(18) 0.6640(15) 0.7199(13) 0.066(7) Uani 1 1 d D . . C52 C 1.147(2) 0.6989(16) 0.7853(16) 0.104(9) Uani 1 1 d U . . H52A H 1.1372 0.6957 0.8293 0.156 Uiso 1 1 calc R . . H52B H 1.1736 0.7543 0.8001 0.156 Uiso 1 1 calc R . . H52C H 1.1971 0.6683 0.7668 0.156 Uiso 1 1 calc R . . C53 C 0.960(2) 0.6842(19) 0.7626(17) 0.122(12) Uani 1 1 d DU . . H53A H 0.9687 0.6639 0.7984 0.183 Uiso 1 1 calc R . . H53B H 0.8916 0.6598 0.7260 0.183 Uiso 1 1 calc R . . H53C H 0.9695 0.7417 0.7906 0.183 Uiso 1 1 calc R . . C54 C 1.0189(19) 0.5756(15) 0.6658(15) 0.091(9) Uani 1 1 d U . . H54A H 1.0706 0.5642 0.6386 0.136 Uiso 1 1 calc R . . H54B H 0.9506 0.5582 0.6292 0.136 Uiso 1 1 calc R . . H54C H 1.0210 0.5474 0.6947 0.136 Uiso 1 1 calc R . . C55 C 1.0928(18) 0.9351(11) 0.7279(13) 0.066(7) Uani 1 1 d . . . H55A H 1.1007 0.9594 0.6960 0.079 Uiso 1 1 calc R . . H55B H 1.0367 0.9522 0.7499 0.079 Uiso 1 1 calc R . . C56 C 1.2165(16) 1.0430(12) 0.8309(13) 0.060(7) Uani 1 1 d . . . H56A H 1.1741 1.0621 0.8658 0.071 Uiso 1 1 calc R . . H56B H 1.2046 1.0663 0.7971 0.071 Uiso 1 1 calc R . . N2 N 0.6191(18) 1.0865(13) 0.3359(14) 0.084(7) Uani 1 1 d U . . H2 H 0.6186 1.0348 0.3021 0.101 Uiso 1 1 calc R . . N3 N 0.622(2) 1.2282(15) 0.4301(15) 0.092(7) Uani 1 1 d U . . C57 C 0.711(2) 1.1348(18) 0.3456(18) 0.108(10) Uani 1 1 d U . . H57A H 0.7092 1.1352 0.2977 0.130 Uiso 1 1 calc R . . H57B H 0.7701 1.1143 0.3594 0.130 Uiso 1 1 calc R . . C58 C 0.721(2) 1.2260(18) 0.4147(18) 0.103(10) Uani 1 1 d U . . H58A H 0.7760 1.2387 0.4610 0.124 Uiso 1 1 calc R . . H58B H 0.7383 1.2651 0.3986 0.124 Uiso 1 1 calc R . . C59 C 0.529(3) 1.104(2) 0.303(2) 0.133(13) Uani 1 1 d U . . H59A H 0.4665 1.0708 0.3005 0.159 Uiso 1 1 calc R . . H59B H 0.5255 1.0930 0.2511 0.159 Uiso 1 1 calc R . . C60 C 0.534(3) 1.196(2) 0.356(2) 0.145(14) Uani 1 1 d U . . H60A H 0.5464 1.2255 0.3296 0.174 Uiso 1 1 calc R . . H60B H 0.4683 1.2021 0.3678 0.174 Uiso 1 1 calc R . . C61 C 0.600(3) 1.087(2) 0.408(2) 0.118(11) Uani 1 1 d U . . H61A H 0.6566 1.0723 0.4336 0.142 Uiso 1 1 calc R . . H61B H 0.5343 1.0499 0.3941 0.142 Uiso 1 1 calc R . . C62 C 0.597(3) 1.177(2) 0.459(2) 0.142(14) Uani 1 1 d U . . H62A H 0.5268 1.1784 0.4645 0.170 Uiso 1 1 calc R . . H62B H 0.6450 1.1982 0.5105 0.170 Uiso 1 1 calc R . . N4 N 0.7225(13) 0.6302(11) 0.2194(10) 0.061(5) Uani 1 1 d U . . H4 H 0.6790 0.6624 0.2383 0.073 Uiso 1 1 calc R . . N5 N 0.852(2) 0.5479(17) 0.1713(17) 0.108(8) Uani 1 1 d U . . C63 C 0.706(2) 0.5619(15) 0.2340(15) 0.075(8) Uani 1 1 d U . . H63A H 0.6348 0.5291 0.2071 0.090 Uiso 1 1 calc R . . H63B H 0.7204 0.5805 0.2891 0.090 Uiso 1 1 calc R . . C64 C 0.783(3) 0.5158(19) 0.2021(18) 0.104(10) Uani 1 1 d U . . H64A H 0.8272 0.5098 0.2431 0.124 Uiso 1 1 calc R . . H64B H 0.7444 0.4620 0.1612 0.124 Uiso 1 1 calc R . . C65 C 0.7030(18) 0.6056(15) 0.1347(14) 0.073(7) Uani 1 1 d U . . H65A H 0.7116 0.6530 0.1284 0.088 Uiso 1 1 calc R . . H65B H 0.6325 0.5727 0.1047 0.088 Uiso 1 1 calc R . . C66 C 0.787(2) 0.5557(18) 0.1070(18) 0.093(9) Uani 1 1 d U . . H66A H 0.7510 0.5025 0.0636 0.112 Uiso 1 1 calc R . . H66B H 0.8312 0.5828 0.0897 0.112 Uiso 1 1 calc R . . C67 C 0.8329(16) 0.6791(15) 0.2592(14) 0.074(7) Uani 1 1 d U . . H67A H 0.8454 0.7050 0.3149 0.089 Uiso 1 1 calc R . . H67B H 0.8427 0.7213 0.2456 0.089 Uiso 1 1 calc R . . C68 C 0.913(2) 0.6280(16) 0.2373(16) 0.083(8) Uani 1 1 d U . . H68A H 0.9637 0.6528 0.2223 0.099 Uiso 1 1 calc R . . H68B H 0.9496 0.6226 0.2809 0.099 Uiso 1 1 calc R . . N6 N 0.2275(18) 0.9000(15) 0.3028(14) 0.095(7) Uani 1 1 d U . . N7 N 0.321(2) 0.8977(18) 0.4285(17) 0.111(9) Uani 1 1 d U . . C69 C 0.295(2) 0.840(2) 0.2864(17) 0.109(10) Uani 1 1 d U . . H69A H 0.3535 0.8588 0.2727 0.131 Uiso 1 1 calc R . . H69B H 0.2547 0.7886 0.2424 0.131 Uiso 1 1 calc R . . C70 C 0.337(2) 0.829(2) 0.3541(19) 0.108(10) Uani 1 1 d U . . H70A H 0.4105 0.8301 0.3620 0.130 Uiso 1 1 calc R . . H70B H 0.3002 0.7773 0.3442 0.130 Uiso 1 1 calc R . . C71 C 0.149(2) 0.8800(18) 0.3391(16) 0.101(9) Uani 1 1 d DU . . H71A H 0.1051 0.9184 0.3507 0.122 Uiso 1 1 calc R . . H71B H 0.1050 0.8261 0.3044 0.122 Uiso 1 1 calc R . . C72 C 0.216(3) 0.886(2) 0.4135(17) 0.127(12) Uani 1 1 d DU . . H72A H 0.2016 0.9294 0.4568 0.152 Uiso 1 1 calc R . . H72B H 0.1902 0.8362 0.4133 0.152 Uiso 1 1 calc R . . C73 C 0.292(2) 0.9797(18) 0.3667(18) 0.098(10) Uani 1 1 d U . . H73A H 0.2461 1.0144 0.3878 0.118 Uiso 1 1 calc R . . H73B H 0.3345 1.0048 0.3470 0.118 Uiso 1 1 calc R . . C74 C 0.363(2) 0.970(2) 0.4312(19) 0.112(11) Uani 1 1 d U . . H74A H 0.4320 0.9699 0.4250 0.135 Uiso 1 1 calc R . . H74B H 0.3687 1.0154 0.4814 0.135 Uiso 1 1 calc R . . N8 N 0.213(2) 1.1196(18) 0.2873(18) 0.116(9) Uani 1 1 d U . . C75 C 0.209(2) 1.185(2) 0.354(2) 0.095(9) Uani 1 1 d U . . H75 H 0.1745 1.1699 0.3821 0.114 Uiso 1 1 calc R . . C76 C 0.243(2) 1.264(2) 0.3863(18) 0.092(9) Uani 1 1 d U . . H76 H 0.2413 1.3023 0.4349 0.110 Uiso 1 1 calc R . . C77 C 0.282(2) 1.281(2) 0.335(2) 0.117(11) Uani 1 1 d U . . H77 H 0.3096 1.3352 0.3526 0.140 Uiso 1 1 calc R . . C78 C 0.285(2) 1.2263(18) 0.2623(19) 0.097(9) Uani 1 1 d DU . . H78 H 0.3085 1.2408 0.2294 0.116 Uiso 1 1 calc R . . C79 C 0.247(2) 1.1476(18) 0.2438(19) 0.106(10) Uani 1 1 d DU . . H79 H 0.2457 1.1082 0.1946 0.127 Uiso 1 1 calc R . . N9 N 0.098(2) 0.9234(14) 0.0508(14) 0.096(7) Uani 1 1 d U . . C80 C 0.164(2) 0.9352(16) 0.0133(17) 0.087(8) Uani 1 1 d U . . H80 H 0.2356 0.9488 0.0369 0.105 Uiso 1 1 calc R . . C81 C 0.124(3) 0.9269(18) -0.064(2) 0.104(10) Uani 1 1 d U . . H81 H 0.1694 0.9346 -0.0898 0.125 Uiso 1 1 calc R . . C82 C 0.013(3) 0.9062(18) -0.0962(19) 0.105(10) Uani 1 1 d U . . H82 H -0.0189 0.9016 -0.1439 0.126 Uiso 1 1 calc R . . C83 C -0.045(3) 0.8933(19) -0.051(2) 0.103(10) Uani 1 1 d U . . H83 H -0.1176 0.8790 -0.0710 0.124 Uiso 1 1 calc R . . C84 C -0.006(2) 0.8998(17) 0.0154(19) 0.087(9) Uani 1 1 d U . . H84 H -0.0503 0.8878 0.0398 0.105 Uiso 1 1 calc R . . N10 N 0.5036(18) 0.5795(15) -0.0926(15) 0.089(7) Uani 1 1 d U . . C85 C 0.513(2) 0.6451(19) -0.0261(19) 0.094(9) Uani 1 1 d U . . H85 H 0.4527 0.6491 -0.0103 0.113 Uiso 1 1 calc R . . C86 C 0.595(2) 0.7051(18) 0.0205(17) 0.090(9) Uani 1 1 d U . . H86 H 0.5932 0.7501 0.0652 0.108 Uiso 1 1 calc R . . C87 C 0.688(2) 0.6946(18) -0.0038(18) 0.084(9) Uani 1 1 d U . . H87 H 0.7514 0.7318 0.0286 0.101 Uiso 1 1 calc R . . C88 C 0.686(2) 0.636(2) -0.068(2) 0.111(11) Uani 1 1 d U . . H88 H 0.7447 0.6328 -0.0857 0.134 Uiso 1 1 calc R . . C89 C 0.590(2) 0.5758(18) -0.1128(17) 0.088(9) Uani 1 1 d U . . H89 H 0.5887 0.5312 -0.1588 0.106 Uiso 1 1 calc R . . O14 O 0.1468(17) 0.9602(14) 0.2047(13) 0.138(8) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0598(6) 0.0576(7) 0.0591(7) 0.0271(6) 0.0132(5) 0.0012(5) U2 0.0616(6) 0.0583(7) 0.0606(7) 0.0263(6) 0.0140(5) 0.0000(5) O1 0.068(10) 0.082(12) 0.047(10) 0.015(9) 0.039(8) -0.018(8) O2 0.063(9) 0.084(12) 0.063(11) 0.047(10) 0.012(8) 0.009(8) O3 0.042(7) 0.067(10) 0.050(9) 0.022(8) 0.017(7) 0.008(7) O4 0.048(8) 0.071(11) 0.082(12) 0.050(10) 0.013(8) 0.010(8) O5 0.054(9) 0.074(12) 0.062(10) 0.031(9) 0.005(8) 0.005(8) O6 0.079(11) 0.041(10) 0.056(11) 0.016(9) -0.001(9) -0.003(8) O7 0.043(8) 0.049(10) 0.097(13) 0.021(9) 0.004(9) -0.008(7) O8 0.051(8) 0.029(8) 0.082(11) 0.017(8) 0.026(8) 0.004(6) O9 0.046(8) 0.067(11) 0.043(9) -0.015(8) 0.024(7) -0.008(7) O10 0.039(8) 0.070(12) 0.070(12) 0.008(9) 0.007(8) -0.014(8) O11 0.081(10) 0.049(11) 0.075(12) 0.026(10) 0.016(9) 0.006(8) O12 0.092(13) 0.055(12) 0.057(12) 0.029(10) -0.011(10) -0.006(9) O13 0.069(10) 0.084(13) 0.072(12) 0.049(11) -0.009(9) -0.036(10) N1 0.072(17) 0.048(16) 0.054(17) 0.007(13) 0.026(14) 0.014(12) C1 0.084(17) 0.044(15) 0.068(18) 0.008(13) 0.031(15) -0.001(12) C2 0.074(15) 0.042(14) 0.075(17) 0.031(13) 0.048(14) 0.001(11) C3 0.062(13) 0.040(13) 0.072(17) 0.037(13) 0.010(12) -0.022(11) C4 0.102(19) 0.055(15) 0.032(13) 0.021(12) -0.013(13) -0.016(13) C5 0.071(15) 0.049(15) 0.065(17) 0.028(13) -0.001(14) -0.013(12) C6 0.072(16) 0.065(17) 0.10(2) 0.049(16) 0.039(16) 0.016(13) C7 0.09(2) 0.064(16) 0.036(15) 0.023(13) 0.003(15) -0.005(15) C8 0.25(6) 0.09(6) 0.06(6) 0.04(5) 0.04(5) 0.07(5) C9 0.10(2) 0.13(3) 0.06(2) 0.03(2) -0.01(2) 0.007(19) C10 0.10(2) 0.17(3) 0.10(2) 0.08(2) 0.038(19) 0.020(19) C11 0.066(14) 0.045(13) 0.058(14) 0.038(12) 0.004(12) 0.001(10) C12 0.042(13) 0.058(16) 0.078(18) 0.033(14) 0.009(13) 0.013(11) C13 0.026(11) 0.11(2) 0.050(15) 0.027(15) 0.019(11) 0.024(12) C14 0.059(14) 0.09(2) 0.053(15) 0.051(15) 0.005(13) 0.010(13) C15 0.053(13) 0.067(17) 0.068(17) 0.039(14) 0.018(13) 0.015(12) C16 0.050(13) 0.12(2) 0.09(2) 0.071(18) 0.040(14) 0.049(14) C17 0.096(19) 0.060(17) 0.063(17) 0.040(14) 0.008(15) 0.003(14) C18 0.062(15) 0.037(18) 0.097(19) 0.018(15) 0.026(14) 0.012(13) C19 0.08(2) 0.17(2) 0.09(2) 0.09(2) -0.015(19) -0.003(17) C20 0.07(2) 0.12(2) 0.15(3) 0.08(2) 0.027(19) 0.024(18) C21 0.09(2) 0.10(3) 0.15(3) 0.06(2) 0.01(2) 0.01(2) C22 0.065(15) 0.063(17) 0.060(16) 0.034(14) 0.000(13) -0.009(12) C23 0.067(14) 0.033(13) 0.10(2) 0.037(13) 0.049(14) 0.009(11) C24 0.056(14) 0.059(17) 0.063(17) 0.020(14) 0.006(13) 0.012(12) C25 0.049(13) 0.055(15) 0.046(14) 0.027(12) 0.004(11) 0.009(10) C26 0.061(14) 0.046(14) 0.067(16) 0.006(12) 0.025(12) -0.010(11) C27 0.046(12) 0.086(18) 0.054(14) 0.045(13) 0.032(11) 0.023(11) C28 0.044(12) 0.055(15) 0.050(15) 0.015(12) -0.013(11) -0.008(10) C29 0.097(19) 0.066(19) 0.048(15) 0.005(14) 0.024(14) -0.024(15) C30 0.13(3) 0.13(3) 0.12(3) 0.04(3) 0.05(2) -0.01(2) C31 0.064(15) 0.076(17) 0.098(18) 0.052(15) 0.016(14) 0.005(13) C32 0.09(2) 0.10(2) 0.13(2) 0.07(2) 0.042(18) 0.029(17) C33 0.060(13) 0.041(13) 0.057(14) 0.011(11) 0.031(11) 0.011(10) C34 0.049(13) 0.054(16) 0.068(17) 0.026(13) 0.007(12) 0.007(11) C35 0.029(7) 0.054(9) 0.041(8) 0.014(7) 0.029(7) 0.018(6) C36 0.037(10) 0.033(12) 0.080(16) 0.027(12) 0.028(11) 0.017(9) C37 0.048(11) 0.047(14) 0.056(14) 0.027(12) -0.016(11) 0.003(10) C38 0.071(16) 0.056(16) 0.09(2) 0.042(15) 0.030(15) 0.034(13) C39 0.081(17) 0.08(2) 0.069(19) 0.041(17) 0.042(15) 0.012(15) C40 0.08(3) 0.06(3) 0.17(3) 0.06(3) 0.06(3) 0.02(2) C41 0.17(3) 0.13(3) 0.18(3) 0.09(2) 0.04(2) 0.00(2) C42 0.10(2) 0.07(2) 0.16(2) 0.07(2) 0.04(2) 0.004(19) C43 0.09(3) 0.10(3) 0.10(3) 0.02(2) 0.05(2) 0.01(2) C44 0.067(15) 0.069(17) 0.072(18) 0.042(15) 0.027(14) 0.017(12) C45 0.035(12) 0.087(19) 0.087(19) 0.056(16) -0.017(13) 0.000(11) C46 0.037(11) 0.049(15) 0.058(16) 0.024(13) 0.003(11) -0.002(10) C47 0.060(14) 0.032(13) 0.076(18) 0.004(12) 0.037(13) 0.003(10) C48 0.081(18) 0.054(17) 0.09(2) 0.029(17) 0.024(16) 0.007(14) C49 0.061(16) 0.08(2) 0.10(2) 0.033(19) 0.030(17) 0.009(14) C50 0.041(12) 0.037(13) 0.10(2) 0.028(14) 0.012(13) -0.009(10) C51 0.072(15) 0.057(18) 0.037(13) -0.002(12) 0.010(12) 0.026(12) C52 0.09(2) 0.10(2) 0.13(2) 0.082(19) 0.009(18) 0.004(16) C53 0.13(3) 0.13(3) 0.12(3) 0.06(2) 0.08(2) 0.04(2) C54 0.074(18) 0.08(2) 0.12(2) 0.065(18) 0.014(16) 0.014(15) C55 0.086(17) 0.027(12) 0.066(16) 0.016(12) 0.012(14) -0.001(11) C56 0.067(14) 0.042(14) 0.071(16) 0.027(13) 0.029(13) 0.001(11) N2 0.075(16) 0.063(16) 0.110(19) 0.051(14) 0.002(14) 0.008(12) N3 0.079(17) 0.090(19) 0.104(19) 0.037(16) 0.039(15) 0.031(14) C57 0.06(2) 0.12(3) 0.13(2) 0.05(2) 0.051(18) -0.005(18) C58 0.07(2) 0.10(2) 0.12(2) 0.04(2) 0.037(19) 0.018(17) C59 0.15(3) 0.10(3) 0.11(3) 0.03(3) 0.02(3) 0.02(2) C60 0.15(3) 0.15(3) 0.15(3) 0.10(3) 0.02(3) 0.04(3) C61 0.16(3) 0.12(3) 0.08(3) 0.05(2) 0.04(2) 0.03(2) C62 0.18(3) 0.09(3) 0.17(3) 0.07(3) 0.06(3) 0.04(3) N4 0.063(11) 0.061(13) 0.066(13) 0.032(11) 0.033(10) 0.014(9) N5 0.099(19) 0.11(2) 0.12(2) 0.047(18) 0.050(18) 0.073(16) C63 0.086(17) 0.064(18) 0.068(18) 0.038(15) 0.005(14) 0.002(14) C64 0.11(2) 0.09(2) 0.08(2) 0.02(2) 0.00(2) 0.041(19) C65 0.060(15) 0.083(18) 0.076(18) 0.042(15) 0.010(14) 0.018(13) C66 0.09(2) 0.10(2) 0.09(2) 0.041(19) 0.039(19) 0.048(17) C67 0.049(14) 0.082(18) 0.053(17) 0.003(14) 0.021(13) 0.003(13) C68 0.073(17) 0.08(2) 0.07(2) 0.016(17) 0.031(16) 0.015(15) N6 0.076(16) 0.096(19) 0.098(18) 0.040(16) 0.020(14) 0.009(14) N7 0.12(2) 0.09(2) 0.11(2) 0.048(19) 0.018(18) 0.016(17) C69 0.09(2) 0.17(3) 0.08(2) 0.07(2) 0.03(2) -0.008(19) C70 0.11(2) 0.14(3) 0.11(3) 0.09(2) 0.04(2) 0.03(2) C71 0.11(2) 0.11(2) 0.10(2) 0.065(18) 0.041(18) -0.010(16) C72 0.12(3) 0.16(3) 0.10(3) 0.09(2) 0.01(2) 0.01(2) C73 0.09(2) 0.10(2) 0.08(2) 0.03(2) 0.019(18) 0.013(17) C74 0.11(2) 0.12(3) 0.12(2) 0.07(2) 0.04(2) -0.006(19) N8 0.12(2) 0.14(2) 0.11(2) 0.07(2) 0.048(19) 0.044(18) C75 0.10(2) 0.10(3) 0.11(3) 0.05(2) 0.043(19) 0.052(19) C76 0.093(19) 0.10(2) 0.09(2) 0.04(2) 0.049(17) 0.020(17) C77 0.10(2) 0.15(3) 0.09(3) 0.07(2) 0.00(2) 0.02(2) C78 0.071(19) 0.15(2) 0.09(2) 0.07(2) 0.008(18) 0.053(18) C79 0.12(2) 0.11(3) 0.08(2) 0.05(2) 0.031(19) 0.015(19) N9 0.087(17) 0.104(18) 0.101(19) 0.059(15) 0.017(16) 0.028(14) C80 0.073(19) 0.08(2) 0.09(2) 0.033(17) 0.004(17) 0.025(15) C81 0.11(2) 0.09(2) 0.08(3) 0.03(2) 0.00(2) 0.021(18) C82 0.10(2) 0.13(2) 0.12(2) 0.08(2) 0.03(2) 0.051(19) C83 0.09(2) 0.13(3) 0.10(3) 0.06(2) 0.03(2) 0.040(19) C84 0.12(2) 0.08(2) 0.06(2) 0.035(18) 0.026(19) 0.017(16) N10 0.078(16) 0.101(19) 0.087(18) 0.050(15) 0.020(14) 0.008(14) C85 0.09(2) 0.10(2) 0.09(2) 0.041(19) 0.043(18) 0.004(17) C86 0.090(19) 0.07(2) 0.08(2) 0.019(17) 0.020(17) -0.003(16) C87 0.082(19) 0.06(2) 0.07(2) 0.014(17) 0.008(17) -0.002(15) C88 0.08(2) 0.12(3) 0.10(3) 0.02(2) 0.05(2) 0.02(2) C89 0.090(19) 0.10(2) 0.07(2) 0.035(18) 0.015(17) 0.037(17) O14 0.153(19) 0.16(2) 0.120(19) 0.074(17) 0.057(16) 0.058(16) _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 O8 1.759(15) . ? U1 O7 1.785(17) . ? U1 O2 2.170(14) . ? U1 O1 2.278(17) . ? U1 O3 2.325(14) . ? U1 O12 2.476(15) . ? U1 O11 2.537(16) . ? U1 N1 2.91(3) . ? U1 U2 5.0287(14) . ? U1 U2 6.3930(15) 2_776 ? U1 U1 10.687(2) 2_776 ? U2 O9 1.788(14) . ? U2 O10 1.801(17) . ? U2 O4 2.113(13) . ? U2 O5 2.179(15) . ? U2 O13 2.434(13) 2_776 ? U2 O13 2.491(16) . ? U2 O11 2.523(16) . ? U2 U2 4.2549(18) 2_776 ? O1 C2 1.38(2) . ? O1 O2 2.77(2) . ? O1 O6 11.96(2) . ? O2 C13 1.36(2) . ? O2 O3 2.92(2) . ? O2 O2 15.00(3) 2_776 ? O3 C24 1.37(2) . ? O3 O4 3.973(18) . ? O3 O3 12.49(2) 2_776 ? O4 C35 1.38(2) . ? O4 O5 2.832(18) . ? O5 C46 1.34(2) . ? O5 O6 3.95(2) . ? O5 O1 5.233(19) 2_776 ? O5 O5 7.38(3) 2_776 ? O6 C55 1.37(2) . ? O6 C56 1.40(2) . ? O11 N1 1.43(3) . ? O12 N1 1.24(3) . ? O13 N1 1.33(3) . ? O13 U2 2.434(13) 2_776 ? C1 C2 1.39(3) . ? C1 C6 1.43(3) . ? C1 C56 1.51(3) 2_776 ? C2 C3 1.45(3) . ? C3 C4 1.41(3) . ? C3 C11 1.47(3) . ? C4 C5 1.39(3) . ? C5 C6 1.40(3) . ? C5 C7 1.48(3) . ? C7 C10 1.51(3) . ? C7 C8 1.52(6) . ? C7 C9 1.56(3) . ? C11 C12 1.51(3) . ? C12 C13 1.36(3) . ? C12 C17 1.37(3) . ? C13 C14 1.42(3) . ? C14 C15 1.35(3) . ? C14 C22 1.44(3) . ? C15 C16 1.52(3) . ? C16 C17 1.37(3) . ? C16 C18 1.58(3) . ? C18 C21 1.47(4) . ? C18 C19 1.52(3) . ? C18 C20 1.51(3) . ? C22 C23 1.52(3) . ? C23 C24 1.39(3) . ? C23 C28 1.39(3) . ? C24 C25 1.40(3) . ? C25 C26 1.35(3) . ? C25 C33 1.50(3) . ? C26 C27 1.49(3) . ? C27 C28 1.35(3) . ? C27 C29 1.51(3) . ? C29 C30 1.50(4) . ? C29 C31 1.50(3) . ? C29 C32 1.50(4) . ? C33 C34 1.57(3) . ? C34 C35 1.39(2) . ? C34 C39 1.43(3) . ? C35 C36 1.38(3) . ? C36 C37 1.32(2) . ? C36 C44 1.55(3) . ? C37 C38 1.42(3) . ? C38 C39 1.36(3) . ? C38 C40 1.48(4) . ? C40 C42 1.47(3) . ? C40 C41 1.47(4) . ? C40 C43 1.48(4) . ? C44 C45 1.54(3) . ? C45 C46 1.34(3) . ? C45 C50 1.38(3) . ? C46 C47 1.42(3) . ? C47 C48 1.46(3) . ? C47 C55 1.54(3) . ? C48 C49 1.37(3) . ? C49 C50 1.42(3) . ? C49 C51 1.56(4) . ? C51 C54 1.49(3) . ? C51 C53 1.52(4) . ? C51 C52 1.55(3) . ? C56 C1 1.51(3) 2_776 ? N2 C57 1.38(3) . ? N2 C59 1.40(3) . ? N2 C61 1.53(3) . ? N3 C62 1.40(4) . ? N3 C58 1.44(3) . ? N3 C60 1.50(4) . ? C57 C58 1.63(4) . ? C59 C60 1.57(4) . ? C61 C62 1.57(4) . ? N4 C63 1.47(3) . ? N4 C67 1.49(2) . ? N4 C65 1.51(3) . ? N5 C64 1.45(3) . ? N5 C68 1.48(3) . ? N5 C66 1.49(3) . ? C63 C64 1.50(3) . ? C65 C66 1.58(3) . ? C67 C68 1.53(3) . ? N6 C73 1.48(3) . ? N6 C69 1.50(3) . ? N6 C71 1.52(3) . ? N6 O14 2.81(3) . ? N7 C72 1.36(3) . ? N7 C74 1.41(3) . ? N7 C70 1.56(4) . ? C69 C70 1.48(3) . ? C71 C72 1.53(4) . ? C73 C74 1.54(4) . ? N8 C79 1.35(3) . ? N8 C75 1.37(4) . ? N8 O14 2.65(4) . ? C75 C76 1.33(4) . ? C76 C77 1.40(4) . ? C77 C78 1.38(4) . ? C78 C79 1.38(5) . ? N9 C80 1.35(3) . ? N9 C84 1.34(3) . ? N9 O14 2.77(3) . ? C80 C81 1.46(4) . ? C81 C82 1.43(4) . ? C82 C83 1.41(4) . ? C83 C84 1.28(4) . ? N10 C89 1.31(3) . ? N10 C85 1.33(3) . ? C85 C86 1.31(3) . ? C86 C87 1.45(4) . ? C87 C88 1.26(4) . ? C88 C89 1.43(4) . ? 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 U1 O7 175.4(6) . . ? O8 U1 O2 92.1(6) . . ? O7 U1 O2 92.4(6) . . ? O8 U1 O1 89.3(6) . . ? O7 U1 O1 92.9(6) . . ? O2 U1 O1 76.8(5) . . ? O8 U1 O3 91.6(5) . . ? O7 U1 O3 87.8(6) . . ? O2 U1 O3 80.8(5) . . ? O1 U1 O3 157.7(5) . . ? O8 U1 O12 89.4(6) . . ? O7 U1 O12 87.8(6) . . ? O2 U1 O12 143.5(5) . . ? O1 U1 O12 66.7(5) . . ? O3 U1 O12 135.6(5) . . ? O8 U1 O11 88.7(6) . . ? O7 U1 O11 86.7(6) . . ? O2 U1 O11 162.4(5) . . ? O1 U1 O11 120.8(5) . . ? O3 U1 O11 81.6(5) . . ? O12 U1 O11 54.1(5) . . ? O8 U1 N1 91.4(6) . . ? O7 U1 N1 84.5(6) . . ? O2 U1 N1 167.8(6) . . ? O1 U1 N1 91.6(7) . . ? O3 U1 N1 110.7(6) . . ? O12 U1 N1 24.9(5) . . ? O11 U1 N1 29.4(6) . . ? O9 U2 O10 173.7(8) . . ? O9 U2 O4 94.5(6) . . ? O10 U2 O4 89.2(6) . . ? O9 U2 O5 93.2(7) . . ? O10 U2 O5 92.3(7) . . ? O4 U2 O5 82.6(5) . . ? O9 U2 O13 87.9(6) . 2_776 ? O10 U2 O13 89.3(6) . 2_776 ? O4 U2 O13 169.7(5) . 2_776 ? O5 U2 O13 87.3(5) . 2_776 ? O9 U2 O13 84.8(7) . . ? O10 U2 O13 88.9(7) . . ? O4 U2 O13 129.7(5) . . ? O5 U2 O13 147.7(5) . . ? O13 U2 O13 60.5(6) 2_776 . ? O9 U2 O11 85.3(6) . . ? O10 U2 O11 90.7(6) . . ? O4 U2 O11 75.7(5) . . ? O5 U2 O11 158.1(5) . . ? O13 U2 O11 114.5(5) 2_776 . ? O13 U2 O11 54.0(5) . . ? O12 N1 O13 131(2) . . ? O12 N1 O11 117(2) . . ? O13 N1 O11 111(2) . . ? C2 C1 C6 119(2) . . ? C2 C1 C56 120(2) . 2_776 ? C6 C1 C56 121(2) . 2_776 ? O1 C2 C1 120(2) . . ? O1 C2 C3 120.7(18) . . ? C1 C2 C3 119(2) . . ? C4 C3 C2 118(2) . . ? C4 C3 C11 121.5(19) . . ? C2 C3 C11 120.6(19) . . ? C5 C4 C3 126(2) . . ? C4 C5 C6 114(2) . . ? C4 C5 C7 121(2) . . ? C6 C5 C7 125(3) . . ? C5 C6 C1 125(2) . . ? C5 C7 C10 112(2) . . ? C5 C7 C8 109(3) . . ? C10 C7 C8 110(4) . . ? C5 C7 C9 112(3) . . ? C10 C7 C9 99(2) . . ? C8 C7 C9 114(3) . . ? C3 C11 C12 114(2) . . ? C13 C12 C17 121(2) . . ? C13 C12 C11 118(2) . . ? C17 C12 C11 120(2) . . ? C12 C13 O2 121(2) . . ? C12 C13 C14 122.1(19) . . ? O2 C13 C14 117(2) . . ? C15 C14 C13 119(2) . . ? C15 C14 C22 122(2) . . ? C13 C14 C22 119(2) . . ? C14 C15 C16 119(2) . . ? C17 C16 C15 118(2) . . ? C17 C16 C18 124(2) . . ? C15 C16 C18 119(2) . . ? C12 C17 C16 121(2) . . ? C21 C18 C19 115(3) . . ? C21 C18 C20 112(2) . . ? C19 C18 C20 105(2) . . ? C21 C18 C16 105(2) . . ? C19 C18 C16 107(2) . . ? C20 C18 C16 114(2) . . ? C14 C22 C23 116(2) . . ? C24 C23 C28 118(2) . . ? C24 C23 C22 125.3(19) . . ? C28 C23 C22 117(2) . . ? O3 C24 C23 121(2) . . ? O3 C24 C25 121.0(19) . . ? C23 C24 C25 118(2) . . ? C26 C25 C24 123(2) . . ? C26 C25 C33 118.5(19) . . ? C24 C25 C33 118.3(19) . . ? C25 C26 C27 121(2) . . ? C28 C27 C26 112.8(18) . . ? C28 C27 C29 127(2) . . ? C26 C27 C29 120.2(19) . . ? C27 C28 C23 128(2) . . ? C30 C29 C31 110(3) . . ? C30 C29 C32 104(2) . . ? C31 C29 C32 109(2) . . ? C30 C29 C27 111(2) . . ? C31 C29 C27 112(2) . . ? C32 C29 C27 110(3) . . ? C25 C33 C34 114.7(17) . . ? C35 C34 C39 117(2) . . ? C35 C34 C33 122.7(19) . . ? C39 C34 C33 119.9(19) . . ? O4 C35 C36 122.6(16) . . ? O4 C35 C34 119.1(19) . . ? C36 C35 C34 118.4(19) . . ? C37 C36 C35 120.3(18) . . ? C37 C36 C44 121.8(19) . . ? C35 C36 C44 117.9(17) . . ? C36 C37 C38 127(2) . . ? C39 C38 C37 110.9(18) . . ? C39 C38 C40 129.3(18) . . ? C37 C38 C40 119.8(17) . . ? C38 C39 C34 126(2) . . ? C42 C40 C41 111(3) . . ? C42 C40 C38 110(2) . . ? C41 C40 C38 109(2) . . ? C42 C40 C43 109(2) . . ? C41 C40 C43 109(3) . . ? C38 C40 C43 109(2) . . ? C45 C44 C36 109.9(18) . . ? C46 C45 C50 125(2) . . ? C46 C45 C44 119(2) . . ? C50 C45 C44 116(2) . . ? O5 C46 C45 124(2) . . ? O5 C46 C47 120(2) . . ? C45 C46 C47 115(2) . . ? C46 C47 C48 122(2) . . ? C46 C47 C55 121(2) . . ? C48 C47 C55 117(2) . . ? C49 C48 C47 118(3) . . ? C48 C49 C50 119(3) . . ? C48 C49 C51 119(3) . . ? C50 C49 C51 121(2) . . ? C45 C50 C49 119(2) . . ? C54 C51 C53 111(2) . . ? C54 C51 C52 115(2) . . ? C53 C51 C52 104(2) . . ? C54 C51 C49 113(2) . . ? C53 C51 C49 107(2) . . ? C52 C51 C49 107(2) . . ? O6 C55 C47 107.7(19) . . ? O6 C56 C1 112.1(19) . 2_776 ? C57 N2 C59 113(2) . . ? C57 N2 C61 118(3) . . ? C59 N2 C61 104(3) . . ? C62 N3 C58 113(3) . . ? C62 N3 C60 103(3) . . ? C58 N3 C60 111(3) . . ? N2 C57 C58 108(2) . . ? N3 C58 C57 107(2) . . ? N2 C59 C60 108(3) . . ? N3 C60 C59 109(3) . . ? N2 C61 C62 102(3) . . ? N3 C62 C61 115(3) . . ? C63 N4 C67 111.0(18) . . ? C63 N4 C65 114.2(18) . . ? C67 N4 C65 105.7(17) . . ? C64 N5 C68 105(2) . . ? C64 N5 C66 109(2) . . ? C68 N5 C66 111(3) . . ? N4 C63 C64 103(2) . . ? N5 C64 C63 119(3) . . ? N4 C65 C66 106(2) . . ? N5 C66 C65 111(2) . . ? N4 C67 C68 112(2) . . ? N5 C68 C67 106(2) . . ? C73 N6 C69 109(2) . . ? C73 N6 C71 102(2) . . ? C69 N6 C71 109(2) . . ? C72 N7 C74 110(3) . . ? C72 N7 C70 104(3) . . ? C74 N7 C70 105(3) . . ? N6 C69 C70 112(3) . . ? C69 C70 N7 111(3) . . ? C72 C71 N6 105(2) . . ? N7 C72 C71 119(3) . . ? N6 C73 C74 110(2) . . ? N7 C74 C73 111(2) . . ? C79 N8 C75 108(3) . . ? C76 C75 N8 134(3) . . ? C75 C76 C77 109(3) . . ? C78 C77 C76 127(3) . . ? C79 C78 C77 112(3) . . ? N8 C79 C78 129(3) . . ? C80 N9 C84 119(3) . . ? N9 C80 C81 121(3) . . ? C82 C81 C80 116(3) . . ? C83 C82 C81 115(3) . . ? C84 C83 C82 125(3) . . ? C83 C84 N9 122(3) . . ? C89 N10 C85 114(3) . . ? N10 C85 C86 129(3) . . ? C85 C86 C87 114(3) . . ? C88 C87 C86 122(3) . . ? C87 C88 C89 117(3) . . ? N10 C89 C88 124(3) . . ? N8 O14 N9 105.5(11) . . ? N8 O14 N6 106.6(11) . . ? N9 O14 N6 141.6(12) . . ? 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 N2 H2 O1 0.91 1.73 2.64(3) 175.4 . N4 H4 O3 0.91 1.76 2.67(2) 178.6 .