# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- CCDC_886104.cif' #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Prof. Dr. K. Meyer Department of Chemistry and Pharmacy Inorganic Chemistry Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; _publ_contact_author_phone '049 9131 852-7360' _publ_contact_author_fax '049 9131 852-7367' _publ_contact_author_email Karsten.Meyer@chemie.uni-erlangen.de _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for data deposition. ; #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Uranium-Mediated Reductive Conversion of CO2 to CO and Carbonate in a Single-Vessel, Closed Synthetic Cycle ; loop_ _publ_author_name _publ_author_address A.-C.Schmidt ; Department of Chemistry and Pharmacy Inorganic Chemistry Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; A.V.Nizovtsev ; Department of Chemistry and Pharmacy Inorganic Chemistry Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; A.Scheurer ; Department of Chemistry and Pharmacy Inorganic Chemistry Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; F.W.Heinemann ; Department of Chemistry and Pharmacy Inorganic Chemistry Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; K.Meyer ; Department of Chemistry and Pharmacy Inorganic Chemistry Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; #============================================================================== # 3. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; source of material: see actual publication ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; _publ_contact_author_name 'Prof. Dr. K. Meyer' #============================================================================== # 4.1 RESULTS FOR 4 * 2 n-hexane data_acs1003 _database_code_depnum_ccdc_archive 'CCDC 886104' #TrackingRef '- CCDC_886104.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H132 N6 O7 U2, 2(C6 H14)' _chemical_formula_sum 'C102 H160 N6 O7 U2' _chemical_formula_weight 2058.42 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 C2/c _symmetry_space_group_name_Hall -C2yc 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' '-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 23.955(2) _cell_length_b 20.947(2) _cell_length_c 23.302(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.653(2) _cell_angle_gamma 90.00 _cell_volume 10357(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7194 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 24.71 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4216 _exptl_absorpt_coefficient_mu 3.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2008' _exptl_special_details ; ? ; _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 'Bruker Smart APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43578 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10559 _reflns_number_gt 6169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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 compound crystallized with a total of four molecules of n-hexane per complex molecule. Two of the independent solvent molecules were situated on crystallographic inversion centres, a third one was located on a crystallographic twofold axis. All of the hexane molecules were disordered. Therefore, no hydrogen atoms were included in the structure model. ; _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^)+(0.0595P)^2^+7.8524P] 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 10559 _refine_ls_number_parameters 710 _refine_ls_number_restraints 544 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.329 _refine_ls_restrained_S_all 1.344 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.964129(17) 0.140539(13) 0.649349(13) 0.04285(13) Uani 1 1 d . A . O1 O 1.0393(3) 0.0703(3) 0.6638(3) 0.0618(19) Uani 1 1 d . . . O2 O 0.9844(3) 0.2437(2) 0.6588(2) 0.0442(15) Uani 1 1 d . . . O3 O 0.8722(3) 0.1093(3) 0.6401(3) 0.0622(17) Uani 1 1 d U . . O4 O 1.0000 0.1377(4) 0.7500 0.080(4) Uani 1 2 d S . . N1 N 0.9993(3) 0.1565(3) 0.5548(3) 0.0333(15) Uani 1 1 d . . . N2 N 0.8799(3) 0.2014(3) 0.5394(3) 0.0334(15) Uani 1 1 d . . . N3 N 0.9042(3) 0.0664(3) 0.5429(3) 0.0324(15) Uani 1 1 d . . . C1 C 0.9752(3) 0.2198(3) 0.5250(3) 0.0330(18) Uani 1 1 d . A . H1A H 0.9878 0.2276 0.4907 0.040 Uiso 1 1 calc R . . H1B H 0.9948 0.2533 0.5584 0.040 Uiso 1 1 calc R . . C2 C 0.9046(3) 0.2249(3) 0.4960(3) 0.0310(18) Uani 1 1 d . A . H2A H 0.8921 0.2701 0.4852 0.037 Uiso 1 1 calc R . . H2B H 0.8851 0.2002 0.4551 0.037 Uiso 1 1 calc R . . C3 C 0.8272(4) 0.1570(4) 0.5057(4) 0.041(2) Uani 1 1 d . A . H3A H 0.7956 0.1775 0.4654 0.049 Uiso 1 1 calc R . . H3B H 0.8068 0.1490 0.5335 0.049 Uiso 1 1 calc R . . C4 C 0.8463(4) 0.0934(4) 0.4887(4) 0.0370(19) Uani 1 1 d . A . H4B H 0.8113 0.0626 0.4767 0.044 Uiso 1 1 calc R . . H4C H 0.8537 0.0993 0.4506 0.044 Uiso 1 1 calc R . . C5 C 0.9509(4) 0.0492(3) 0.5203(4) 0.0357(19) Uani 1 1 d . A . H5A H 0.9302 0.0216 0.4815 0.043 Uiso 1 1 calc R . . H5B H 0.9853 0.0242 0.5546 0.043 Uiso 1 1 calc R . . C6 C 0.9787(4) 0.1065(4) 0.5038(4) 0.0374(19) Uani 1 1 d . A . H6A H 1.0152 0.0928 0.4980 0.045 Uiso 1 1 calc R . . H6B H 0.9468 0.1249 0.4623 0.045 Uiso 1 1 calc R . . C7 C 1.0692(4) 0.1611(4) 0.5920(5) 0.055(3) Uani 1 1 d . A . H7A H 1.0800 0.1889 0.6300 0.066 Uiso 1 1 calc R . . H7B H 1.0849 0.1823 0.5643 0.066 Uiso 1 1 calc R . . C8 C 1.1037(4) 0.0983(4) 0.6155(5) 0.060(3) Uani 1 1 d U . . C9 C 1.0891(5) 0.0568(4) 0.6541(5) 0.061(3) Uani 1 1 d U A . C10 C 1.1287(6) 0.0040(5) 0.6833(4) 0.073(3) Uani 1 1 d U . . C11 C 1.1812(5) -0.0044(5) 0.6717(5) 0.081(4) Uani 1 1 d U A . H11A H 1.2080 -0.0400 0.6909 0.097 Uiso 1 1 calc R . . C12 C 1.1952(5) 0.0359(5) 0.6343(6) 0.074(3) Uani 1 1 d U . . C13 C 1.1553(4) 0.0871(5) 0.6044(5) 0.067(3) Uani 1 1 d U A . H13A H 1.1632 0.1145 0.5765 0.081 Uiso 1 1 calc R . . C14 C 1.1219(6) -0.0348(6) 0.7325(6) 0.095(4) Uani 1 1 d U A . H14A H 1.0956 -0.0105 0.7474 0.114 Uiso 1 1 calc R . . H14B H 1.1642 -0.0395 0.7701 0.114 Uiso 1 1 calc R . . C15 C 1.0932(6) -0.1019(6) 0.7127(5) 0.078(3) Uani 1 1 d U . . C16 C 1.1311(5) -0.1451(5) 0.6904(5) 0.067(3) Uani 1 1 d U A . H16A H 1.1282 -0.1287 0.6497 0.100 Uiso 1 1 calc R . . H16B H 1.1140 -0.1885 0.6836 0.100 Uiso 1 1 calc R . . H16C H 1.1754 -0.1457 0.7236 0.100 Uiso 1 1 calc R . . C17 C 1.0929(7) -0.1341(7) 0.7713(7) 0.118(5) Uani 1 1 d U A . H17A H 1.1363 -0.1392 0.8057 0.177 Uiso 1 1 calc R . . H17B H 1.0729 -0.1762 0.7587 0.177 Uiso 1 1 calc R . . H17C H 1.0692 -0.1078 0.7872 0.177 Uiso 1 1 calc R . . C18 C 1.0264(5) -0.0986(6) 0.6582(6) 0.088(4) Uani 1 1 d U A . H18A H 1.0257 -0.0736 0.6223 0.131 Uiso 1 1 calc R . . H18B H 0.9992 -0.0783 0.6739 0.131 Uiso 1 1 calc R . . H18C H 1.0111 -0.1419 0.6431 0.131 Uiso 1 1 calc R . . C19 C 1.2538(5) 0.0260(5) 0.6260(6) 0.092(4) Uani 1 1 d U A . H19A H 1.2441 0.0357 0.5812 0.137 Uiso 1 1 calc R . . H19B H 1.2677 -0.0184 0.6360 0.137 Uiso 1 1 calc R . . H19C H 1.2873 0.0545 0.6555 0.137 Uiso 1 1 calc R . . C20 C 0.8571(4) 0.2556(4) 0.5651(4) 0.045(2) Uani 1 1 d . A . H20A H 0.8168 0.2711 0.5297 0.054 Uiso 1 1 calc R . . H20B H 0.8481 0.2387 0.5996 0.054 Uiso 1 1 calc R . . C21 C 0.9002(5) 0.3115(4) 0.5919(4) 0.047(2) Uani 1 1 d . . . C22 C 0.9628(4) 0.3033(4) 0.6404(4) 0.040(2) Uani 1 1 d . A . C23 C 1.0004(5) 0.3574(4) 0.6698(5) 0.050(2) Uani 1 1 d . . . C24 C 0.9737(6) 0.4170(5) 0.6504(6) 0.067(3) Uani 1 1 d . A . H24A H 0.9987 0.4535 0.6704 0.081 Uiso 1 1 calc R . . C25 C 0.9135(6) 0.4259(4) 0.6040(7) 0.071(3) Uani 1 1 d . . . C26 C 0.8763(5) 0.3726(4) 0.5728(5) 0.058(3) Uani 1 1 d . A . H26A H 0.8347 0.3783 0.5387 0.069 Uiso 1 1 calc R . . C27 C 1.0650(5) 0.3512(4) 0.7266(5) 0.059(3) Uani 1 1 d . A . H27A H 1.0695 0.3067 0.7426 0.071 Uiso 1 1 calc R . . H27B H 1.0664 0.3791 0.7615 0.071 Uiso 1 1 calc R . . C28 C 1.1232(5) 0.3665(4) 0.7178(5) 0.055(3) Uani 1 1 d . . . C29 C 1.1241(5) 0.4356(4) 0.6993(5) 0.062(3) Uani 1 1 d . A . H29A H 1.1626 0.4438 0.6956 0.093 Uiso 1 1 calc R . . H29B H 1.1232 0.4634 0.7326 0.093 Uiso 1 1 calc R . . H29C H 1.0872 0.4443 0.6576 0.093 Uiso 1 1 calc R . . C30 C 1.1811(6) 0.3538(4) 0.7825(6) 0.075(3) Uani 1 1 d . A . H30A H 1.2192 0.3651 0.7790 0.112 Uiso 1 1 calc R . . H30B H 1.1826 0.3085 0.7936 0.112 Uiso 1 1 calc R . . H30C H 1.1789 0.3798 0.8163 0.112 Uiso 1 1 calc R . . C31 C 1.1236(6) 0.3229(5) 0.6648(6) 0.082(4) Uani 1 1 d . A . H31A H 1.1628 0.3294 0.6620 0.123 Uiso 1 1 calc R . . H31B H 1.0875 0.3334 0.6230 0.123 Uiso 1 1 calc R . . H31C H 1.1206 0.2782 0.6755 0.123 Uiso 1 1 calc R . . C32 C 0.8845(6) 0.4936(5) 0.5840(7) 0.104(4) Uani 1 1 d U A . H32A H 0.8991 0.5207 0.6226 0.156 Uiso 1 1 calc R . . H32B H 0.8384 0.4906 0.5631 0.156 Uiso 1 1 calc R . . H32C H 0.8977 0.5124 0.5537 0.156 Uiso 1 1 calc R . . C33 C 0.8913(4) 0.0082(4) 0.5716(4) 0.040(2) Uani 1 1 d . A . H33A H 0.8801 -0.0269 0.5396 0.048 Uiso 0.536(6) 1 calc PR A 1 H33B H 0.9309 -0.0042 0.6100 0.048 Uiso 0.536(6) 1 calc PR A 1 H33C H 0.9271 0.0031 0.6156 0.048 Uiso 0.464(6) 1 d PR A 2 H33D H 0.8919 -0.0292 0.5459 0.048 Uiso 0.464(6) 1 d PR A 2 C34 C 0.8431(10) 0.0128(13) 0.5908(11) 0.034(3) Uani 0.536(6) 1 d PU A 1 C35 C 0.8402(8) 0.0594(8) 0.6296(8) 0.034(3) Uani 0.536(6) 1 d PU A 1 C36 C 0.7942(7) 0.0601(7) 0.6520(7) 0.040(3) Uani 0.536(6) 1 d PU A 1 C37 C 0.7527(7) 0.0085(7) 0.6320(7) 0.041(3) Uani 0.536(6) 1 d PU A 1 H37A H 0.7222 0.0060 0.6473 0.049 Uiso 0.536(6) 1 calc PR A 1 C38 C 0.7531(8) -0.0390(9) 0.5911(9) 0.041(3) Uani 0.536(6) 1 d PU A 1 C39 C 0.8011(9) -0.0368(12) 0.5717(10) 0.034(3) Uani 0.536(6) 1 d PU A 1 H39A H 0.8040 -0.0698 0.5453 0.040 Uiso 0.536(6) 1 calc PR A 1 C40 C 0.7930(7) 0.1047(7) 0.7004(7) 0.041(3) Uani 0.536(6) 1 d PU A 1 H40A H 0.7943 0.0790 0.7367 0.049 Uiso 0.536(6) 1 calc PR A 1 H40B H 0.8322 0.1302 0.7179 0.049 Uiso 0.536(6) 1 calc PR A 1 C41 C 0.740(2) 0.1496(16) 0.680(2) 0.039(3) Uani 0.536(6) 1 d PU A 1 C42 C 0.7517(7) 0.1957(7) 0.7370(7) 0.041(3) Uani 0.536(6) 1 d PU A 1 H42A H 0.7487 0.1718 0.7717 0.062 Uiso 0.536(6) 1 calc PR A 1 H42B H 0.7201 0.2298 0.7216 0.062 Uiso 0.536(6) 1 calc PR A 1 H42C H 0.7939 0.2144 0.7537 0.062 Uiso 0.536(6) 1 calc PR A 1 C43 C 0.6767(8) 0.1308(8) 0.6449(9) 0.054(4) Uani 0.536(6) 1 d PU A 1 H43A H 0.6650 0.1047 0.6726 0.081 Uiso 0.536(6) 1 calc PR A 1 H43B H 0.6711 0.1058 0.6071 0.081 Uiso 0.536(6) 1 calc PR A 1 H43C H 0.6497 0.1688 0.6306 0.081 Uiso 0.536(6) 1 calc PR A 1 C44 C 0.7502(7) 0.2025(7) 0.6304(7) 0.043(4) Uani 0.536(6) 1 d PU A 1 H44A H 0.7403 0.1818 0.5891 0.065 Uiso 0.536(6) 1 calc PR A 1 H44B H 0.7941 0.2169 0.6510 0.065 Uiso 0.536(6) 1 calc PR A 1 H44C H 0.7223 0.2392 0.6227 0.065 Uiso 0.536(6) 1 calc PR A 1 C45 C 0.7084(11) -0.0934(12) 0.5737(11) 0.057(6) Uani 0.536(6) 1 d PU A 1 H45A H 0.6672 -0.0779 0.5667 0.086 Uiso 0.536(6) 1 calc PR A 1 H45B H 0.7244 -0.1248 0.6089 0.086 Uiso 0.536(6) 1 calc PR A 1 H45C H 0.7042 -0.1136 0.5339 0.086 Uiso 0.536(6) 1 calc PR A 1 C34A C 0.8276(12) 0.0100(15) 0.5775(12) 0.032(3) Uani 0.464(6) 1 d PU A 2 C35A C 0.8134(10) 0.0648(9) 0.6039(9) 0.036(3) Uani 0.464(6) 1 d PU A 2 C36A C 0.7549(8) 0.0707(8) 0.6026(8) 0.039(3) Uani 0.464(6) 1 d PU A 2 C37A C 0.7152(9) 0.0172(8) 0.5843(8) 0.038(3) Uani 0.464(6) 1 d PU A 2 H37B H 0.6765 0.0202 0.5862 0.045 Uiso 0.464(6) 1 calc PR A 2 C38A C 0.7293(9) -0.0406(10) 0.5634(9) 0.036(3) Uani 0.464(6) 1 d PU A 2 C39A C 0.7834(11) -0.0423(14) 0.5578(13) 0.036(3) Uani 0.464(6) 1 d PU A 2 H39C H 0.7924 -0.0795 0.5402 0.043 Uiso 0.464(6) 1 calc PR A 2 C40A C 0.7318(8) 0.1359(8) 0.6126(8) 0.036(3) Uani 0.464(6) 1 d PU A 2 H40C H 0.7508 0.1684 0.5961 0.043 Uiso 0.464(6) 1 calc PR A 2 H40D H 0.6858 0.1372 0.5839 0.043 Uiso 0.464(6) 1 calc PR A 2 C41A C 0.743(3) 0.1584(19) 0.679(3) 0.040(3) Uani 0.464(6) 1 d PU A 2 C42A C 0.7099(9) 0.0937(9) 0.7036(9) 0.048(4) Uani 0.464(6) 1 d PU A 2 H42D H 0.6655 0.0879 0.6719 0.073 Uiso 0.464(6) 1 calc PR A 2 H42E H 0.7129 0.1033 0.7461 0.073 Uiso 0.464(6) 1 calc PR A 2 H42F H 0.7333 0.0544 0.7064 0.073 Uiso 0.464(6) 1 calc PR A 2 C43A C 0.7027(8) 0.2106(8) 0.6755(8) 0.040(4) Uani 0.464(6) 1 d PU A 2 H43D H 0.7110 0.2471 0.6542 0.059 Uiso 0.464(6) 1 calc PR A 2 H43E H 0.7114 0.2227 0.7195 0.059 Uiso 0.464(6) 1 calc PR A 2 H43F H 0.6585 0.1978 0.6508 0.059 Uiso 0.464(6) 1 calc PR A 2 C44A C 0.8077(8) 0.1555(8) 0.7282(8) 0.041(4) Uani 0.464(6) 1 d PU A 2 H44D H 0.8319 0.1893 0.7206 0.062 Uiso 0.464(6) 1 calc PR A 2 H44E H 0.8255 0.1138 0.7266 0.062 Uiso 0.464(6) 1 calc PR A 2 H44F H 0.8098 0.1616 0.7708 0.062 Uiso 0.464(6) 1 calc PR A 2 C45A C 0.6850(11) -0.0964(11) 0.5456(11) 0.041(6) Uani 0.464(6) 1 d P A 2 H45D H 0.6733 -0.1098 0.5012 0.062 Uiso 0.464(6) 1 calc PR A 2 H45E H 0.6471 -0.0839 0.5487 0.062 Uiso 0.464(6) 1 calc PR A 2 H45F H 0.7058 -0.1318 0.5754 0.062 Uiso 0.464(6) 1 calc PR A 2 C101 C 1.0058(14) 0.4274(5) 0.5052(17) 0.135(9) Uani 0.50 1 d PDU . . C102 C 1.0000 0.5000 0.5000 0.138(7) Uani 1 2 d SDU . . C103 C 1.0416(11) 0.5454(10) 0.5516(11) 0.159(8) Uani 0.50 1 d PDU . . C104 C 1.0195(9) 0.6148(11) 0.5356(10) 0.169(7) Uani 1 1 d DU . . C105 C 1.0048(18) 0.6382(14) 0.5902(17) 0.180(12) Uani 0.50 1 d PDU . . C201 C 0.7210(11) 0.7337(18) 0.4978(17) 0.181(11) Uani 0.549(15) 1 d PDU . 1 C202 C 0.6648(14) 0.7563(15) 0.4339(15) 0.171(11) Uani 0.549(15) 1 d PDU . 1 C203 C 0.6043(11) 0.7299(16) 0.4334(14) 0.147(10) Uani 0.549(15) 1 d PDU . 1 C301 C 0.5000 0.889(2) 0.2500 0.160(13) Uani 0.451(15) 2 d SPDU . 2 C302 C 0.5511(10) 0.8463(16) 0.2993(12) 0.157(12) Uani 0.451(15) 1 d PDU . 2 C303 C 0.613(2) 0.833(4) 0.302(3) 0.147(12) Uani 0.225(7) 1 d PDU . 2 C304 C 0.653(2) 0.794(3) 0.363(3) 0.148(13) Uani 0.225(7) 1 d PDU . 2 C305 C 0.718(2) 0.791(3) 0.364(3) 0.118(15) Uani 0.225(7) 1 d PDU . 2 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 0.0823(3) 0.02654(17) 0.01918(15) 0.00202(13) 0.02306(15) 0.00967(18) O1 0.092(5) 0.034(3) 0.030(3) -0.003(3) 0.004(3) 0.023(3) O2 0.083(4) 0.026(3) 0.029(3) 0.003(2) 0.030(3) 0.007(3) O3 0.081(3) 0.058(3) 0.062(3) -0.005(2) 0.046(2) 0.003(2) O4 0.181(11) 0.031(5) 0.025(4) 0.000 0.045(6) 0.000 N1 0.036(4) 0.032(4) 0.022(3) 0.000(3) 0.005(3) 0.010(3) N2 0.046(4) 0.027(3) 0.033(3) 0.007(3) 0.024(3) 0.012(3) N3 0.042(4) 0.032(4) 0.022(3) 0.001(3) 0.014(3) 0.010(3) C1 0.036(5) 0.037(4) 0.028(4) 0.005(3) 0.017(4) 0.007(4) C2 0.045(5) 0.030(4) 0.026(4) 0.006(3) 0.023(4) 0.010(3) C3 0.044(5) 0.040(5) 0.047(5) 0.012(4) 0.028(4) 0.010(4) C4 0.038(5) 0.043(5) 0.029(4) 0.003(3) 0.014(4) 0.006(4) C5 0.043(5) 0.031(4) 0.029(4) -0.008(3) 0.013(4) 0.010(4) C6 0.048(5) 0.036(4) 0.027(4) -0.009(3) 0.016(4) 0.005(4) C7 0.041(6) 0.038(5) 0.057(6) -0.023(4) -0.002(5) 0.007(4) C8 0.046(5) 0.037(5) 0.058(5) -0.020(4) -0.008(4) 0.012(4) C9 0.059(6) 0.043(5) 0.045(5) -0.019(4) -0.006(4) 0.023(4) C10 0.094(7) 0.057(5) 0.034(5) -0.010(4) 0.001(5) 0.029(5) C11 0.075(7) 0.059(6) 0.062(6) -0.033(5) -0.009(5) 0.034(5) C12 0.043(5) 0.050(5) 0.088(7) -0.033(5) -0.005(5) 0.012(5) C13 0.045(5) 0.044(5) 0.082(6) -0.025(5) 0.003(5) 0.007(4) C14 0.102(5) 0.092(5) 0.089(5) -0.005(3) 0.041(3) 0.018(3) C15 0.097(7) 0.097(7) 0.053(5) 0.033(5) 0.047(5) 0.055(6) C16 0.082(7) 0.069(7) 0.049(5) 0.008(5) 0.030(5) 0.037(6) C17 0.137(7) 0.128(7) 0.106(7) 0.015(5) 0.070(5) 0.043(5) C18 0.094(6) 0.106(6) 0.084(6) 0.022(5) 0.059(5) 0.031(5) C19 0.072(6) 0.065(5) 0.107(6) -0.023(5) 0.016(4) 0.011(4) C20 0.067(6) 0.035(5) 0.050(5) 0.008(4) 0.043(5) 0.013(4) C21 0.078(7) 0.030(5) 0.056(6) 0.005(4) 0.050(6) 0.011(4) C22 0.069(6) 0.029(4) 0.039(5) -0.001(4) 0.039(5) 0.004(4) C23 0.084(7) 0.036(5) 0.053(5) -0.001(4) 0.052(5) -0.001(5) C24 0.100(10) 0.032(5) 0.112(9) -0.005(6) 0.085(9) 0.000(6) C25 0.095(9) 0.024(5) 0.132(10) 0.007(6) 0.084(9) 0.008(6) C26 0.081(7) 0.036(6) 0.084(7) 0.009(5) 0.062(6) 0.013(5) C27 0.104(8) 0.038(5) 0.051(6) -0.010(4) 0.050(6) -0.020(5) C28 0.093(8) 0.033(5) 0.063(6) -0.015(4) 0.055(6) -0.024(5) C29 0.085(8) 0.038(5) 0.072(7) -0.004(5) 0.043(6) -0.018(5) C30 0.094(9) 0.048(6) 0.095(9) -0.004(6) 0.055(8) -0.009(6) C31 0.124(10) 0.050(6) 0.126(10) -0.030(6) 0.103(9) -0.032(6) C32 0.099(9) 0.048(6) 0.186(13) 0.010(7) 0.083(9) 0.014(6) C33 0.053(6) 0.028(4) 0.041(5) -0.001(4) 0.022(4) 0.008(4) C34 0.038(6) 0.026(4) 0.038(6) 0.005(4) 0.016(5) 0.002(5) C35 0.040(6) 0.029(5) 0.034(6) 0.007(5) 0.019(5) 0.002(5) C36 0.047(5) 0.034(5) 0.036(5) 0.008(4) 0.018(4) 0.003(4) C37 0.044(6) 0.039(5) 0.040(5) 0.008(5) 0.020(5) -0.001(5) C38 0.043(6) 0.033(4) 0.043(6) 0.007(5) 0.017(5) -0.009(5) C39 0.038(7) 0.027(5) 0.037(6) 0.004(5) 0.019(5) 0.001(5) C40 0.047(5) 0.040(5) 0.036(5) 0.012(5) 0.021(4) 0.007(5) C41 0.043(5) 0.041(5) 0.035(4) 0.005(5) 0.019(4) 0.005(5) C42 0.053(7) 0.048(7) 0.034(6) 0.008(6) 0.030(6) 0.010(6) C43 0.049(8) 0.052(8) 0.057(8) 0.007(7) 0.022(7) 0.002(7) C44 0.048(8) 0.043(7) 0.036(7) 0.008(6) 0.016(6) 0.004(6) C45 0.051(12) 0.044(10) 0.061(11) -0.003(10) 0.013(9) -0.012(9) C34A 0.038(6) 0.025(4) 0.035(5) 0.004(4) 0.018(4) 0.001(5) C35A 0.040(6) 0.031(5) 0.035(5) 0.006(5) 0.017(5) 0.001(5) C36A 0.043(5) 0.034(5) 0.037(5) 0.002(4) 0.018(4) 0.003(5) C37A 0.040(6) 0.036(5) 0.039(5) -0.001(5) 0.020(5) -0.003(5) C38A 0.038(7) 0.028(5) 0.039(6) 0.005(5) 0.015(5) -0.002(5) C39A 0.039(7) 0.027(5) 0.040(6) 0.002(5) 0.017(5) 0.001(6) C40A 0.039(5) 0.038(5) 0.035(5) 0.003(5) 0.020(4) 0.004(5) C41A 0.042(5) 0.042(5) 0.036(5) 0.004(5) 0.019(4) 0.005(5) C42A 0.055(10) 0.052(9) 0.047(9) 0.001(8) 0.031(8) 0.002(8) C43A 0.040(8) 0.048(8) 0.038(7) -0.001(7) 0.024(6) 0.006(7) C44A 0.055(8) 0.044(8) 0.027(7) -0.002(6) 0.021(6) 0.006(7) C45A 0.034(15) 0.024(10) 0.047(14) -0.012(11) 0.003(11) -0.015(10) C101 0.075(13) 0.20(2) 0.141(17) 0.024(18) 0.060(12) 0.003(15) C102 0.083(11) 0.198(19) 0.142(15) 0.050(15) 0.060(10) -0.014(12) C103 0.110(12) 0.196(19) 0.157(16) 0.046(15) 0.051(11) -0.012(11) C104 0.111(11) 0.201(18) 0.175(17) 0.030(15) 0.050(11) -0.008(11) C105 0.118(18) 0.22(2) 0.19(2) 0.00(2) 0.064(17) -0.034(17) C201 0.187(13) 0.167(13) 0.182(13) -0.035(8) 0.079(8) 0.011(8) C202 0.179(12) 0.162(12) 0.172(12) -0.031(8) 0.082(8) 0.004(8) C203 0.154(15) 0.171(16) 0.170(15) -0.033(12) 0.121(12) -0.029(12) C301 0.163(14) 0.156(14) 0.155(14) 0.000 0.069(9) 0.000 C302 0.163(13) 0.148(13) 0.156(13) -0.005(6) 0.070(8) 0.002(6) C303 0.150(13) 0.144(13) 0.149(13) -0.005(7) 0.071(8) -0.004(7) C304 0.150(14) 0.141(14) 0.149(14) -0.006(8) 0.066(9) -0.004(8) C305 0.128(19) 0.116(19) 0.128(19) -0.001(14) 0.076(14) -0.002(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O4 2.0909(4) . ? U1 O2 2.203(5) . ? U1 O3 2.209(7) . ? U1 O1 2.227(6) . ? U1 N3 2.705(6) . ? U1 N1 2.720(6) . ? U1 N2 2.732(6) . ? O1 C9 1.343(12) . ? O2 C22 1.343(9) . ? O3 C35 1.252(17) . ? O3 C35A 1.57(2) . ? O4 U1 2.0909(4) 2_756 ? N1 C6 1.484(9) . ? N1 C1 1.485(9) . ? N1 C7 1.489(10) . ? N2 C3 1.469(10) . ? N2 C2 1.472(8) . ? N2 C20 1.500(9) . ? N3 C4 1.487(9) . ? N3 C5 1.487(9) . ? N3 C33 1.489(9) . ? C1 C2 1.506(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4B 0.9900 . ? C4 H4C 0.9900 . ? C5 C6 1.507(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.394(14) . ? C8 C9 1.407(14) . ? C9 C10 1.410(12) . ? C10 C11 1.415(16) . ? C10 C14 1.474(15) . ? C11 C12 1.362(16) . ? C11 H11A 0.9500 . ? C12 C13 1.390(13) . ? C12 C19 1.516(15) . ? C13 H13A 0.9500 . ? C14 C15 1.537(17) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.514(15) . ? C15 C17 1.528(16) . ? C15 C16 1.534(13) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.493(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.388(11) . ? C21 C22 1.408(12) . ? C22 C23 1.412(12) . ? C23 C24 1.379(13) . ? C23 C27 1.506(14) . ? C24 C25 1.354(15) . ? C24 H24A 0.9500 . ? C25 C26 1.403(14) . ? C25 C32 1.553(14) . ? C26 H26A 0.9500 . ? C27 C28 1.533(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.515(11) . ? C28 C30 1.525(15) . ? C28 C31 1.540(12) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.42(3) . ? C33 C34A 1.59(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 H33C 0.9900 . ? C33 H33D 0.9899 . ? C34 C35 1.35(3) . ? C34 C39 1.37(3) . ? C35 C36 1.42(2) . ? C36 C37 1.39(2) . ? C36 C40 1.47(2) . ? C37 C38 1.38(2) . ? C37 H37A 0.9500 . ? C38 C39 1.42(3) . ? C38 C45 1.49(3) . ? C39 H39A 0.9500 . ? C40 C41 1.47(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C43 1.40(5) . ? C41 C42 1.56(5) . ? C41 C44 1.70(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C34A C35A 1.42(3) . ? C34A C39A 1.44(3) . ? C35A C36A 1.39(3) . ? C36A C37A 1.40(2) . ? C36A C40A 1.53(2) . ? C37A C38A 1.40(3) . ? C37A H37B 0.9500 . ? C38A C39A 1.36(3) . ? C38A C45A 1.50(3) . ? C39A H39C 0.9500 . ? C40A C41A 1.51(6) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41A C43A 1.43(6) . ? C41A C44A 1.45(6) . ? C41A C42A 1.79(5) . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C45A H45D 0.9800 . ? C45A H45E 0.9800 . ? C45A H45F 0.9800 . ? C101 C104 1.23(3) 5_766 ? C101 C103 1.40(4) 5_766 ? C102 C103 1.494(10) 5_766 ? C102 C101 1.526(10) 5_766 ? C103 C101 1.40(4) 5_766 ? C103 C104 1.532(10) . ? C104 C101 1.23(3) 5_766 ? C104 C105 1.549(10) . ? C201 C201 1.51(6) 7_666 ? C201 C202 1.547(10) . ? C202 C203 1.547(10) . ? C301 C302 1.53(2) 2_655 ? C301 C302 1.53(2) . ? C302 C303 1.48(2) . ? C303 C304 1.53(2) . ? C304 C305 1.54(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 U1 O2 87.6(2) . . ? O4 U1 O3 88.45(18) . . ? O2 U1 O3 117.6(2) . . ? O4 U1 O1 85.9(2) . . ? O2 U1 O1 120.5(2) . . ? O3 U1 O1 121.2(2) . . ? O4 U1 N3 141.2(2) . . ? O2 U1 N3 130.79(17) . . ? O3 U1 N3 70.1(2) . . ? O1 U1 N3 78.92(19) . . ? O4 U1 N1 142.32(13) . . ? O2 U1 N1 79.85(18) . . ? O3 U1 N1 128.8(2) . . ? O1 U1 N1 70.8(2) . . ? N3 U1 N1 63.92(18) . . ? O4 U1 N2 143.6(2) . . ? O2 U1 N2 70.65(19) . . ? O3 U1 N2 77.2(2) . . ? O1 U1 N2 130.08(19) . . ? N3 U1 N2 63.98(18) . . ? N1 U1 N2 63.54(17) . . ? C9 O1 U1 146.3(6) . . ? C22 O2 U1 147.7(6) . . ? C35 O3 U1 139.3(9) . . ? C35A O3 U1 146.5(8) . . ? U1 O4 U1 176.8(4) 2_756 . ? C6 N1 C1 110.1(6) . . ? C6 N1 C7 112.2(6) . . ? C1 N1 C7 107.6(6) . . ? C6 N1 U1 116.6(5) . . ? C1 N1 U1 106.8(4) . . ? C7 N1 U1 102.9(5) . . ? C3 N2 C2 111.4(6) . . ? C3 N2 C20 108.0(6) . . ? C2 N2 C20 111.0(6) . . ? C3 N2 U1 106.4(4) . . ? C2 N2 U1 116.3(4) . . ? C20 N2 U1 103.1(4) . . ? C4 N3 C5 110.4(5) . . ? C4 N3 C33 112.8(6) . . ? C5 N3 C33 107.8(5) . . ? C4 N3 U1 116.7(4) . . ? C5 N3 U1 107.3(4) . . ? C33 N3 U1 101.0(4) . . ? N1 C1 C2 112.7(6) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 113.1(6) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 113.9(6) . . ? N2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 112.8(6) . . ? N3 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? N3 C4 H4C 109.0 . . ? C3 C4 H4C 109.0 . . ? H4B C4 H4C 107.8 . . ? N3 C5 C6 113.0(6) . . ? N3 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N3 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 C6 C5 112.4(6) . . ? N1 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? N1 C7 C8 115.6(7) . . ? N1 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? N1 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C13 C8 C9 121.3(9) . . ? C13 C8 C7 117.4(10) . . ? C9 C8 C7 120.7(9) . . ? O1 C9 C8 118.9(8) . . ? O1 C9 C10 122.3(11) . . ? C8 C9 C10 118.7(11) . . ? C9 C10 C11 117.7(11) . . ? C9 C10 C14 121.0(12) . . ? C11 C10 C14 120.6(10) . . ? C12 C11 C10 123.4(10) . . ? C12 C11 H11A 118.3 . . ? C10 C11 H11A 118.3 . . ? C11 C12 C13 118.8(11) . . ? C11 C12 C19 121.0(10) . . ? C13 C12 C19 120.2(12) . . ? C12 C13 C8 120.0(12) . . ? C12 C13 H13A 120.0 . . ? C8 C13 H13A 120.0 . . ? C10 C14 C15 117.8(10) . . ? C10 C14 H14A 107.9 . . ? C15 C14 H14A 107.9 . . ? C10 C14 H14B 107.9 . . ? C15 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C18 C15 C17 109.1(11) . . ? C18 C15 C16 107.7(9) . . ? C17 C15 C16 106.9(9) . . ? C18 C15 C14 111.2(9) . . ? C17 C15 C14 108.9(11) . . ? C16 C15 C14 112.9(10) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N2 116.8(7) . . ? C21 C20 H20A 108.1 . . ? N2 C20 H20A 108.1 . . ? C21 C20 H20B 108.1 . . ? N2 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C26 C21 C22 119.9(9) . . ? C26 C21 C20 119.1(9) . . ? C22 C21 C20 120.8(7) . . ? O2 C22 C21 118.6(7) . . ? O2 C22 C23 121.9(8) . . ? C21 C22 C23 119.5(8) . . ? C24 C23 C22 118.3(10) . . ? C24 C23 C27 119.9(9) . . ? C22 C23 C27 121.3(8) . . ? C25 C24 C23 123.0(10) . . ? C25 C24 H24A 118.5 . . ? C23 C24 H24A 118.5 . . ? C24 C25 C26 119.3(9) . . ? C24 C25 C32 121.8(10) . . ? C26 C25 C32 118.9(12) . . ? C21 C26 C25 119.9(11) . . ? C21 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C23 C27 C28 119.4(8) . . ? C23 C27 H27A 107.5 . . ? C28 C27 H27A 107.5 . . ? C23 C27 H27B 107.5 . . ? C28 C27 H27B 107.5 . . ? H27A C27 H27B 107.0 . . ? C29 C28 C30 108.7(8) . . ? C29 C28 C27 112.0(8) . . ? C30 C28 C27 107.4(8) . . ? C29 C28 C31 109.3(8) . . ? C30 C28 C31 110.4(9) . . ? C27 C28 C31 109.1(7) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C32 H32A 109.5 . . ? C25 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C25 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N3 116.9(12) . . ? N3 C33 C34A 115.0(12) . . ? C34 C33 H33A 108.1 . . ? N3 C33 H33A 108.1 . . ? C34A C33 H33A 98.4 . . ? C34 C33 H33B 108.1 . . ? N3 C33 H33B 108.1 . . ? C34A C33 H33B 118.8 . . ? H33A C33 H33B 107.3 . . ? C34 C33 H33C 96.9 . . ? N3 C33 H33C 107.1 . . ? C34A C33 H33C 108.4 . . ? H33A C33 H33C 120.0 . . ? C34 C33 H33D 119.0 . . ? N3 C33 H33D 108.2 . . ? C34A C33 H33D 110.7 . . ? H33B C33 H33D 93.7 . . ? H33C C33 H33D 107.0 . . ? C35 C34 C39 120(2) . . ? C35 C34 C33 123.9(18) . . ? C39 C34 C33 115(2) . . ? O3 C35 C34 121.2(16) . . ? O3 C35 C36 115.3(14) . . ? C34 C35 C36 122.7(17) . . ? C37 C36 C35 115.0(14) . . ? C37 C36 C40 118.9(14) . . ? C35 C36 C40 125.6(14) . . ? C38 C37 C36 123.9(15) . . ? C38 C37 H37A 118.1 . . ? C36 C37 H37A 118.1 . . ? C37 C38 C39 117.6(16) . . ? C37 C38 C45 120.4(18) . . ? C39 C38 C45 121.8(19) . . ? C34 C39 C38 120(2) . . ? C34 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C41 C40 C36 119(2) . . ? C41 C40 H40A 107.7 . . ? C36 C40 H40A 107.7 . . ? C41 C40 H40B 107.7 . . ? C36 C40 H40B 107.7 . . ? H40A C40 H40B 107.1 . . ? C43 C41 C40 123(3) . . ? C43 C41 C42 113(4) . . ? C40 C41 C42 109(3) . . ? C43 C41 C44 104(3) . . ? C40 C41 C44 105(3) . . ? C42 C41 C44 98.6(19) . . ? C35A C34A C39A 118(2) . . ? C35A C34A C33 119(2) . . ? C39A C34A C33 123(2) . . ? C36A C35A C34A 120.3(19) . . ? C36A C35A O3 127.0(16) . . ? C34A C35A O3 112.2(16) . . ? C35A C36A C37A 118.1(16) . . ? C35A C36A C40A 120.5(16) . . ? C37A C36A C40A 121.1(15) . . ? C36A C37A C38A 123.7(17) . . ? C36A C37A H37B 118.2 . . ? C38A C37A H37B 118.2 . . ? C39A C38A C37A 116.8(19) . . ? C39A C38A C45A 122(2) . . ? C37A C38A C45A 120.8(18) . . ? C38A C39A C34A 123(2) . . ? C38A C39A H39C 118.6 . . ? C34A C39A H39C 118.6 . . ? C41A C40A C36A 122(2) . . ? C41A C40A H40C 106.8 . . ? C36A C40A H40C 106.8 . . ? C41A C40A H40D 106.8 . . ? C36A C40A H40D 106.8 . . ? H40C C40A H40D 106.7 . . ? C43A C41A C44A 121(4) . . ? C43A C41A C40A 113(4) . . ? C44A C41A C40A 114(4) . . ? C43A C41A C42A 102(4) . . ? C44A C41A C42A 100(3) . . ? C40A C41A C42A 102(2) . . ? C41A C42A H42D 109.5 . . ? C41A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C41A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C41A C43A H43D 109.5 . . ? C41A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C41A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C41A C44A H44D 109.5 . . ? C41A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C41A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C38A C45A H45D 109.5 . . ? C38A C45A H45E 109.5 . . ? H45D C45A H45E 109.5 . . ? C38A C45A H45F 109.5 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? C104 C101 C103 70.7(19) 5_766 5_766 ? C103 C102 C101 124.6(17) 5_766 5_766 ? C101 C103 C104 49.4(13) 5_766 . ? C101 C104 C103 59.9(19) 5_766 . ? C101 C104 C105 130(3) 5_766 . ? C103 C104 C105 106.5(9) . . ? C201 C201 C202 107(4) 7_666 . ? C203 C202 C201 106.9(9) . . ? C302 C301 C302 107(2) 2_655 . ? C303 C302 C301 126(3) . . ? C302 C303 C304 110(3) . . ? C303 C304 C305 104(3) . . ? 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 O4 U1 O1 C9 -123.8(9) . . . . ? O2 U1 O1 C9 -38.9(10) . . . . ? O3 U1 O1 C9 150.5(9) . . . . ? N3 U1 O1 C9 92.1(9) . . . . ? N1 U1 O1 C9 26.1(9) . . . . ? N2 U1 O1 C9 50.7(10) . . . . ? O4 U1 O2 C22 -126.3(8) . . . . ? O3 U1 O2 C22 -39.2(9) . . . . ? O1 U1 O2 C22 149.9(8) . . . . ? N3 U1 O2 C22 47.6(9) . . . . ? N1 U1 O2 C22 89.4(8) . . . . ? N2 U1 O2 C22 24.1(8) . . . . ? O4 U1 O3 C35 -100.0(13) . . . . ? O2 U1 O3 C35 173.5(13) . . . . ? O1 U1 O3 C35 -15.7(14) . . . . ? N3 U1 O3 C35 47.0(13) . . . . ? N1 U1 O3 C35 74.0(14) . . . . ? N2 U1 O3 C35 113.7(13) . . . . ? O4 U1 O3 C35A -137.6(15) . . . . ? O2 U1 O3 C35A 135.9(14) . . . . ? O1 U1 O3 C35A -53.3(15) . . . . ? N3 U1 O3 C35A 9.4(14) . . . . ? N1 U1 O3 C35A 36.3(15) . . . . ? N2 U1 O3 C35A 76.0(15) . . . . ? O4 U1 N1 C6 127.6(6) . . . . ? O2 U1 N1 C6 -159.9(5) . . . . ? O3 U1 N1 C6 -42.4(6) . . . . ? O1 U1 N1 C6 72.7(5) . . . . ? N3 U1 N1 C6 -14.1(5) . . . . ? N2 U1 N1 C6 -86.5(5) . . . . ? O4 U1 N1 C1 -108.9(5) . . . . ? O2 U1 N1 C1 -36.4(4) . . . . ? O3 U1 N1 C1 81.0(5) . . . . ? O1 U1 N1 C1 -163.8(5) . . . . ? N3 U1 N1 C1 109.4(5) . . . . ? N2 U1 N1 C1 37.0(4) . . . . ? O4 U1 N1 C7 4.3(6) . . . . ? O2 U1 N1 C7 76.8(4) . . . . ? O3 U1 N1 C7 -165.8(4) . . . . ? O1 U1 N1 C7 -50.7(4) . . . . ? N3 U1 N1 C7 -137.5(5) . . . . ? N2 U1 N1 C7 150.1(5) . . . . ? O4 U1 N2 C3 -106.0(5) . . . . ? O2 U1 N2 C3 -162.6(5) . . . . ? O3 U1 N2 C3 -36.9(4) . . . . ? O1 U1 N2 C3 83.4(5) . . . . ? N3 U1 N2 C3 37.0(4) . . . . ? N1 U1 N2 C3 109.4(5) . . . . ? O4 U1 N2 C2 129.2(5) . . . . ? O2 U1 N2 C2 72.6(5) . . . . ? O3 U1 N2 C2 -161.7(5) . . . . ? O1 U1 N2 C2 -41.4(6) . . . . ? N3 U1 N2 C2 -87.8(5) . . . . ? N1 U1 N2 C2 -15.4(4) . . . . ? O4 U1 N2 C20 7.5(6) . . . . ? O2 U1 N2 C20 -49.0(4) . . . . ? O3 U1 N2 C20 76.7(5) . . . . ? O1 U1 N2 C20 -163.1(4) . . . . ? N3 U1 N2 C20 150.6(5) . . . . ? N1 U1 N2 C20 -137.1(5) . . . . ? O4 U1 N3 C4 128.6(4) . . . . ? O2 U1 N3 C4 -41.5(6) . . . . ? O3 U1 N3 C4 68.3(5) . . . . ? O1 U1 N3 C4 -162.4(5) . . . . ? N1 U1 N3 C4 -88.5(5) . . . . ? N2 U1 N3 C4 -16.8(5) . . . . ? O4 U1 N3 C5 -106.9(4) . . . . ? O2 U1 N3 C5 83.0(5) . . . . ? O3 U1 N3 C5 -167.2(5) . . . . ? O1 U1 N3 C5 -37.9(4) . . . . ? N1 U1 N3 C5 36.0(4) . . . . ? N2 U1 N3 C5 107.7(4) . . . . ? O4 U1 N3 C33 5.9(5) . . . . ? O2 U1 N3 C33 -164.2(4) . . . . ? O3 U1 N3 C33 -54.4(4) . . . . ? O1 U1 N3 C33 74.8(4) . . . . ? N1 U1 N3 C33 148.7(5) . . . . ? N2 U1 N3 C33 -139.5(5) . . . . ? C6 N1 C1 C2 67.7(8) . . . . ? C7 N1 C1 C2 -169.7(6) . . . . ? U1 N1 C1 C2 -59.7(6) . . . . ? C3 N2 C2 C1 -130.9(6) . . . . ? C20 N2 C2 C1 108.7(7) . . . . ? U1 N2 C2 C1 -8.6(7) . . . . ? N1 C1 C2 N2 47.0(8) . . . . ? C2 N2 C3 C4 69.4(8) . . . . ? C20 N2 C3 C4 -168.5(6) . . . . ? U1 N2 C3 C4 -58.4(7) . . . . ? C5 N3 C4 C3 -128.6(7) . . . . ? C33 N3 C4 C3 110.7(7) . . . . ? U1 N3 C4 C3 -5.7(8) . . . . ? N2 C3 C4 N3 44.5(9) . . . . ? C4 N3 C5 C6 69.0(8) . . . . ? C33 N3 C5 C6 -167.3(6) . . . . ? U1 N3 C5 C6 -59.2(6) . . . . ? C1 N1 C6 C5 -131.8(7) . . . . ? C7 N1 C6 C5 108.4(8) . . . . ? U1 N1 C6 C5 -10.0(8) . . . . ? N3 C5 C6 N1 47.3(9) . . . . ? C6 N1 C7 C8 -47.6(11) . . . . ? C1 N1 C7 C8 -168.8(8) . . . . ? U1 N1 C7 C8 78.6(8) . . . . ? N1 C7 C8 C13 132.1(9) . . . . ? N1 C7 C8 C9 -55.9(11) . . . . ? U1 O1 C9 C8 -6.7(14) . . . . ? U1 O1 C9 C10 170.7(6) . . . . ? C13 C8 C9 O1 179.2(8) . . . . ? C7 C8 C9 O1 7.4(12) . . . . ? C13 C8 C9 C10 1.6(13) . . . . ? C7 C8 C9 C10 -170.1(8) . . . . ? O1 C9 C10 C11 -177.7(8) . . . . ? C8 C9 C10 C11 -0.3(13) . . . . ? O1 C9 C10 C14 -7.5(14) . . . . ? C8 C9 C10 C14 170.0(10) . . . . ? C9 C10 C11 C12 0.4(15) . . . . ? C14 C10 C11 C12 -169.9(10) . . . . ? C10 C11 C12 C13 -1.7(15) . . . . ? C10 C11 C12 C19 177.2(9) . . . . ? C11 C12 C13 C8 3.0(14) . . . . ? C19 C12 C13 C8 -175.9(9) . . . . ? C9 C8 C13 C12 -3.0(13) . . . . ? C7 C8 C13 C12 169.0(8) . . . . ? C9 C10 C14 C15 107.2(12) . . . . ? C11 C10 C14 C15 -82.8(14) . . . . ? C10 C14 C15 C18 -61.8(14) . . . . ? C10 C14 C15 C17 178.0(11) . . . . ? C10 C14 C15 C16 59.4(14) . . . . ? C3 N2 C20 C21 -170.5(7) . . . . ? C2 N2 C20 C21 -48.1(9) . . . . ? U1 N2 C20 C21 77.1(7) . . . . ? N2 C20 C21 C26 132.2(8) . . . . ? N2 C20 C21 C22 -53.9(10) . . . . ? U1 O2 C22 C21 -3.5(12) . . . . ? U1 O2 C22 C23 174.4(6) . . . . ? C26 C21 C22 O2 178.7(7) . . . . ? C20 C21 C22 O2 4.9(11) . . . . ? C26 C21 C22 C23 0.7(11) . . . . ? C20 C21 C22 C23 -173.1(7) . . . . ? O2 C22 C23 C24 -176.8(7) . . . . ? C21 C22 C23 C24 1.1(11) . . . . ? O2 C22 C23 C27 -4.5(11) . . . . ? C21 C22 C23 C27 173.4(7) . . . . ? C22 C23 C24 C25 -0.8(13) . . . . ? C27 C23 C24 C25 -173.2(9) . . . . ? C23 C24 C25 C26 -1.4(15) . . . . ? C23 C24 C25 C32 179.0(9) . . . . ? C22 C21 C26 C25 -2.9(13) . . . . ? C20 C21 C26 C25 171.0(8) . . . . ? C24 C25 C26 C21 3.3(15) . . . . ? C32 C25 C26 C21 -177.1(9) . . . . ? C24 C23 C27 C28 -77.3(10) . . . . ? C22 C23 C27 C28 110.6(9) . . . . ? C23 C27 C28 C29 62.5(10) . . . . ? C23 C27 C28 C30 -178.2(7) . . . . ? C23 C27 C28 C31 -58.6(11) . . . . ? C4 N3 C33 C34 -52.0(12) . . . . ? C5 N3 C33 C34 -174.2(11) . . . . ? U1 N3 C33 C34 73.4(11) . . . . ? C4 N3 C33 C34A -38.7(13) . . . . ? C5 N3 C33 C34A -160.9(11) . . . . ? U1 N3 C33 C34A 86.7(11) . . . . ? N3 C33 C34 C35 -52(2) . . . . ? C34A C33 C34 C35 -136(12) . . . . ? N3 C33 C34 C39 133.6(16) . . . . ? C34A C33 C34 C39 49(9) . . . . ? C35A O3 C35 C34 90(3) . . . . ? U1 O3 C35 C34 -32(2) . . . . ? C35A O3 C35 C36 -80(3) . . . . ? U1 O3 C35 C36 157.3(9) . . . . ? C39 C34 C35 O3 -169.9(17) . . . . ? C33 C34 C35 O3 15(3) . . . . ? C39 C34 C35 C36 0(3) . . . . ? C33 C34 C35 C36 -175.0(17) . . . . ? O3 C35 C36 C37 171.0(13) . . . . ? C34 C35 C36 C37 1(2) . . . . ? O3 C35 C36 C40 -18(2) . . . . ? C34 C35 C36 C40 172.2(17) . . . . ? C35 C36 C37 C38 -3(2) . . . . ? C40 C36 C37 C38 -174.5(15) . . . . ? C36 C37 C38 C39 4(3) . . . . ? C36 C37 C38 C45 178.1(17) . . . . ? C35 C34 C39 C38 1(3) . . . . ? C33 C34 C39 C38 176.5(17) . . . . ? C37 C38 C39 C34 -3(3) . . . . ? C45 C38 C39 C34 -177.3(19) . . . . ? C37 C36 C40 C41 -73(3) . . . . ? C35 C36 C40 C41 116(2) . . . . ? C36 C40 C41 C43 49(5) . . . . ? C36 C40 C41 C42 -174.9(18) . . . . ? C36 C40 C41 C44 -70(3) . . . . ? C34 C33 C34A C35A 54(9) . . . . ? N3 C33 C34A C35A -47(2) . . . . ? C34 C33 C34A C39A -125(11) . . . . ? N3 C33 C34A C39A 133(2) . . . . ? C39A C34A C35A C36A -8(3) . . . . ? C33 C34A C35A C36A 172.5(17) . . . . ? C39A C34A C35A O3 164.4(17) . . . . ? C33 C34A C35A O3 -15(3) . . . . ? C35 O3 C35A C36A 109(4) . . . . ? U1 O3 C35A C36A -162.6(12) . . . . ? C35 O3 C35A C34A -63(3) . . . . ? U1 O3 C35A C34A 25(2) . . . . ? C34A C35A C36A C37A 10(3) . . . . ? O3 C35A C36A C37A -161.5(15) . . . . ? C34A C35A C36A C40A -162.5(18) . . . . ? O3 C35A C36A C40A 26(3) . . . . ? C35A C36A C37A C38A -4(3) . . . . ? C40A C36A C37A C38A 168.4(16) . . . . ? C36A C37A C38A C39A -4(3) . . . . ? C36A C37A C38A C45A 179.0(18) . . . . ? C37A C38A C39A C34A 5(3) . . . . ? C45A C38A C39A C34A -177(2) . . . . ? C35A C34A C39A C38A 0(3) . . . . ? C33 C34A C39A C38A 179(2) . . . . ? C35A C36A C40A C41A -93(3) . . . . ? C37A C36A C40A C41A 94(3) . . . . ? C36A C40A C41A C43A -163(2) . . . . ? C36A C40A C41A C44A 53(4) . . . . ? C36A C40A C41A C42A -54(4) . . . . ? C101 C103 C104 C105 127(3) 5_766 . . . ? C201 C201 C202 C203 -173(3) 7_666 . . . ? C302 C301 C302 C303 104(5) 2_655 . . . ? C301 C302 C303 C304 174(4) . . . . ? C302 C303 C304 C305 -173(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.394 _refine_diff_density_min -2.467 _refine_diff_density_rms 0.148 #===END OF DATA FOR 4 * 2 n-hexane # Attachment '- CCDC_886105.cif' data_acs1103 _database_code_depnum_ccdc_archive 'CCDC 886105' #TrackingRef '- CCDC_886105.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H132 N6 O7 U2, C6 H6' _chemical_formula_sum 'C96 H138 N6 O7 U2' _chemical_formula_weight 1964.18 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 orthorhombic _symmetry_space_group_name_H-M Pnna _symmetry_space_group_name_Hall -P2a2bc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y, z' '-x, -y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' 'x-1/2, y, -z' _cell_length_a 16.300(2) _cell_length_b 21.497(3) _cell_length_c 25.420(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8907.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9914 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 3.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.627 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS micro-focus tube' _diffrn_radiation_monochromator 'Quazar focussing montel optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 148203 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.41 _reflns_number_total 11173 _reflns_number_gt 8160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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. ; _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^)+(0.0160P)^2^+12.8625P] 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 11173 _refine_ls_number_parameters 513 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0484 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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 0.006289(6) 0.845153(4) 0.766272(4) 0.01223(3) Uani 1 1 d . . . O1 O -0.04728(13) 0.81568(9) 0.84311(8) 0.0186(4) Uani 1 1 d . . . O2 O -0.07934(12) 0.86067(9) 0.70044(8) 0.0173(4) Uani 1 1 d . . . O3 O 0.13917(11) 0.84264(9) 0.74554(8) 0.0158(4) Uani 1 1 d . . . O4 O 0.00632(17) 0.7500 0.7500 0.0170(6) Uani 1 2 d S . . N1 N -0.08272(14) 0.94122(11) 0.80752(9) 0.0149(5) Uani 1 1 d . . . N2 N 0.03540(14) 0.96072(11) 0.72543(9) 0.0150(5) Uani 1 1 d . . . N3 N 0.08983(14) 0.92462(11) 0.82820(10) 0.0153(5) Uani 1 1 d . . . C1 C -0.10272(16) 0.98366(13) 0.76359(12) 0.0160(6) Uani 1 1 d . . . H1A H -0.1362 1.0186 0.7771 0.019 Uiso 1 1 calc R . . H1B H -0.1360 0.9609 0.7373 0.019 Uiso 1 1 calc R . . C2 C -0.02698(17) 1.00949(12) 0.73707(12) 0.0173(6) Uani 1 1 d . . . H2A H -0.0432 1.0300 0.7038 0.021 Uiso 1 1 calc R . . H2B H -0.0021 1.0415 0.7601 0.021 Uiso 1 1 calc R . . C3 C 0.11805(17) 0.98025(13) 0.74345(12) 0.0169(6) Uani 1 1 d . . . H3A H 0.1300 1.0224 0.7297 0.020 Uiso 1 1 calc R . . H3B H 0.1596 0.9514 0.7289 0.020 Uiso 1 1 calc R . . C4 C 0.12512(18) 0.98102(12) 0.80297(12) 0.0166(6) Uani 1 1 d . . . H4B H 0.1837 0.9844 0.8128 0.020 Uiso 1 1 calc R . . H4C H 0.0965 1.0183 0.8167 0.020 Uiso 1 1 calc R . . C5 C 0.03373(18) 0.94283(14) 0.87148(11) 0.0167(6) Uani 1 1 d . . . H5A H 0.0632 0.9708 0.8960 0.020 Uiso 1 1 calc R . . H5B H 0.0174 0.9052 0.8913 0.020 Uiso 1 1 calc R . . C6 C -0.04291(18) 0.97552(13) 0.85134(11) 0.0169(6) Uani 1 1 d . . . H6A H -0.0825 0.9800 0.8806 0.020 Uiso 1 1 calc R . . H6B H -0.0280 1.0178 0.8391 0.020 Uiso 1 1 calc R . . C7 C 0.04034(18) 0.94793(14) 0.66779(12) 0.0171(6) Uani 1 1 d . . . H7A H 0.0737 0.9100 0.6626 0.021 Uiso 1 1 calc R . . H7B H 0.0699 0.9828 0.6509 0.021 Uiso 1 1 calc R . . C8 C -0.04019(18) 0.93919(14) 0.63974(12) 0.0170(6) Uani 1 1 d . . . C9 C -0.09546(18) 0.89289(13) 0.65617(12) 0.0166(6) Uani 1 1 d . . . C10 C -0.16419(18) 0.87935(14) 0.62477(12) 0.0189(6) Uani 1 1 d . . . C11 C -0.17515(19) 0.91331(14) 0.57827(12) 0.0208(7) Uani 1 1 d . . . H11A H -0.2209 0.9037 0.5566 0.025 Uiso 1 1 calc R . . C12 C -0.12278(19) 0.96009(15) 0.56240(12) 0.0216(7) Uani 1 1 d . . . C13 C -0.05507(19) 0.97234(14) 0.59385(11) 0.0194(6) Uani 1 1 d . . . H13A H -0.0180 1.0042 0.5837 0.023 Uiso 1 1 calc R . . C14 C -0.21808(18) 0.82344(14) 0.63621(13) 0.0210(7) Uani 1 1 d . . . H14A H -0.1869 0.7953 0.6597 0.025 Uiso 1 1 calc R . . H14B H -0.2266 0.8010 0.6027 0.025 Uiso 1 1 calc R . . C15 C -0.30324(19) 0.83421(14) 0.66131(13) 0.0214(7) Uani 1 1 d . . . C16 C -0.3566(2) 0.87621(16) 0.62698(14) 0.0304(8) Uani 1 1 d . . . H16A H -0.4118 0.8789 0.6421 0.046 Uiso 1 1 calc R . . H16B H -0.3600 0.8588 0.5914 0.046 Uiso 1 1 calc R . . H16C H -0.3323 0.9179 0.6254 0.046 Uiso 1 1 calc R . . C17 C -0.3450(2) 0.77088(16) 0.66730(15) 0.0321(8) Uani 1 1 d . . . H17A H -0.3983 0.7763 0.6845 0.048 Uiso 1 1 calc R . . H17B H -0.3104 0.7436 0.6888 0.048 Uiso 1 1 calc R . . H17C H -0.3529 0.7522 0.6325 0.048 Uiso 1 1 calc R . . C18 C -0.2936(2) 0.86332(17) 0.71569(13) 0.0307(8) Uani 1 1 d . . . H18A H -0.3477 0.8685 0.7318 0.046 Uiso 1 1 calc R . . H18B H -0.2669 0.9040 0.7123 0.046 Uiso 1 1 calc R . . H18C H -0.2599 0.8361 0.7378 0.046 Uiso 1 1 calc R . . C19 C -0.1353(2) 0.99573(16) 0.51159(12) 0.0284(8) Uani 1 1 d . . . H19A H -0.1625 0.9688 0.4858 0.043 Uiso 1 1 calc R . . H19B H -0.0820 1.0091 0.4978 0.043 Uiso 1 1 calc R . . H19C H -0.1696 1.0323 0.5183 0.043 Uiso 1 1 calc R . . C20 C -0.16071(17) 0.91152(14) 0.82523(12) 0.0175(6) Uani 1 1 d . . . H20A H -0.1789 0.8820 0.7977 0.021 Uiso 1 1 calc R . . H20B H -0.2032 0.9442 0.8282 0.021 Uiso 1 1 calc R . . C21 C -0.15606(18) 0.87730(14) 0.87677(12) 0.0181(6) Uani 1 1 d . . . C22 C -0.10003(18) 0.82731(14) 0.88212(12) 0.0172(6) Uani 1 1 d . . . C23 C -0.10252(18) 0.79046(14) 0.92813(12) 0.0190(6) Uani 1 1 d . . . C24 C -0.1572(2) 0.80790(15) 0.96756(12) 0.0234(7) Uani 1 1 d . . . H24A H -0.1596 0.7831 0.9985 0.028 Uiso 1 1 calc R . . C25 C -0.20828(19) 0.85916(15) 0.96443(13) 0.0244(7) Uani 1 1 d . . . C26 C -0.20794(19) 0.89282(14) 0.91766(13) 0.0219(7) Uani 1 1 d . . . H26A H -0.2441 0.9272 0.9138 0.026 Uiso 1 1 calc R . . C27 C -0.0536(2) 0.73123(14) 0.93315(12) 0.0220(7) Uani 1 1 d . . . H27A H -0.0363 0.7188 0.8973 0.026 Uiso 1 1 calc R . . H27B H -0.0913 0.6985 0.9461 0.026 Uiso 1 1 calc R . . C28 C 0.02350(19) 0.73032(14) 0.96858(12) 0.0214(7) Uani 1 1 d . . . C29 C 0.0047(2) 0.74978(16) 1.02510(12) 0.0317(8) Uani 1 1 d . . . H29A H 0.0549 0.7474 1.0462 0.048 Uiso 1 1 calc R . . H29B H -0.0368 0.7219 1.0400 0.048 Uiso 1 1 calc R . . H29C H -0.0161 0.7926 1.0254 0.048 Uiso 1 1 calc R . . C30 C 0.0564(2) 0.66362(15) 0.96872(14) 0.0315(8) Uani 1 1 d . . . H30A H 0.1077 0.6620 0.9887 0.047 Uiso 1 1 calc R . . H30B H 0.0665 0.6502 0.9325 0.047 Uiso 1 1 calc R . . H30C H 0.0159 0.6360 0.9851 0.047 Uiso 1 1 calc R . . C31 C 0.0876(2) 0.77358(16) 0.94626(16) 0.0343(9) Uani 1 1 d . . . H31A H 0.1365 0.7727 0.9686 0.051 Uiso 1 1 calc R . . H31B H 0.0657 0.8160 0.9450 0.051 Uiso 1 1 calc R . . H31C H 0.1021 0.7601 0.9106 0.051 Uiso 1 1 calc R . . C32 C -0.2589(2) 0.87981(18) 1.01113(14) 0.0356(9) Uani 1 1 d . . . H32A H -0.2560 0.8482 1.0388 0.053 Uiso 1 1 calc R . . H32B H -0.3162 0.8853 1.0002 0.053 Uiso 1 1 calc R . . H32C H -0.2375 0.9193 1.0246 0.053 Uiso 1 1 calc R . . C33 C 0.15443(18) 0.88364(14) 0.85095(12) 0.0190(6) Uani 1 1 d . . . H33A H 0.1284 0.8438 0.8612 0.023 Uiso 1 1 calc R . . H33B H 0.1750 0.9034 0.8835 0.023 Uiso 1 1 calc R . . C34 C 0.22711(18) 0.86908(13) 0.81641(12) 0.0168(6) Uani 1 1 d . . . C35 C 0.21550(16) 0.84729(13) 0.76465(12) 0.0158(5) Uani 1 1 d . . . C36 C 0.28491(17) 0.83051(12) 0.73440(12) 0.0158(6) Uani 1 1 d . . . C37 C 0.36151(18) 0.83139(12) 0.75866(13) 0.0186(6) Uani 1 1 d . . . H37A H 0.4078 0.8181 0.7389 0.022 Uiso 1 1 calc R . . C38 C 0.37388(18) 0.85066(13) 0.81029(12) 0.0185(6) Uani 1 1 d . . . C39 C 0.30548(18) 0.87043(13) 0.83780(12) 0.0179(6) Uani 1 1 d . . . H39A H 0.3124 0.8855 0.8727 0.021 Uiso 1 1 calc R . . C40 C 0.27511(18) 0.80676(14) 0.67865(12) 0.0190(6) Uani 1 1 d . . . H40A H 0.2160 0.7991 0.6724 0.023 Uiso 1 1 calc R . . H40B H 0.3034 0.7661 0.6762 0.023 Uiso 1 1 calc R . . C41 C 0.30750(17) 0.84887(14) 0.63330(12) 0.0195(6) Uani 1 1 d . . . C42 C 0.39984(18) 0.86072(15) 0.63726(13) 0.0236(7) Uani 1 1 d . . . H42A H 0.4183 0.8839 0.6063 0.035 Uiso 1 1 calc R . . H42B H 0.4289 0.8209 0.6390 0.035 Uiso 1 1 calc R . . H42C H 0.4115 0.8849 0.6691 0.035 Uiso 1 1 calc R . . C43 C 0.2908(2) 0.81424(16) 0.58182(13) 0.0286(8) Uani 1 1 d . . . H43A H 0.3091 0.8397 0.5521 0.043 Uiso 1 1 calc R . . H43B H 0.2318 0.8061 0.5786 0.043 Uiso 1 1 calc R . . H43C H 0.3207 0.7747 0.5818 0.043 Uiso 1 1 calc R . . C44 C 0.2620(2) 0.91093(14) 0.63235(13) 0.0241(7) Uani 1 1 d . . . H44A H 0.2831 0.9366 0.6035 0.036 Uiso 1 1 calc R . . H44B H 0.2705 0.9326 0.6658 0.036 Uiso 1 1 calc R . . H44C H 0.2033 0.9035 0.6271 0.036 Uiso 1 1 calc R . . C45 C 0.45727(18) 0.84604(15) 0.83630(13) 0.0238(7) Uani 1 1 d . . . H45A H 0.4620 0.8781 0.8635 0.036 Uiso 1 1 calc R . . H45B H 0.5003 0.8522 0.8099 0.036 Uiso 1 1 calc R . . H45C H 0.4635 0.8048 0.8523 0.036 Uiso 1 1 calc R . . C101 C 0.5821(2) 0.00138(18) 0.98735(14) 0.0361(9) Uani 1 1 d . . . H10A H 0.6388 0.0021 0.9786 0.043 Uiso 1 1 calc R . . C102 C 0.5361(2) -0.05190(18) 0.97817(15) 0.0362(9) Uani 1 1 d . . . H10B H 0.5613 -0.0875 0.9631 0.043 Uiso 1 1 calc R . . C103 C 0.4542(2) -0.05310(18) 0.99094(15) 0.0370(9) Uani 1 1 d . . . H10C H 0.4228 -0.0896 0.9848 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01407(5) 0.01063(5) 0.01200(5) -0.00077(4) -0.00057(4) 0.00017(4) O1 0.0239(11) 0.0166(10) 0.0152(11) 0.0003(9) 0.0001(9) 0.0022(9) O2 0.0199(10) 0.0151(10) 0.0168(11) 0.0017(8) -0.0018(8) -0.0014(8) O3 0.0158(9) 0.0158(10) 0.0159(10) -0.0021(8) -0.0010(7) -0.0011(8) O4 0.0201(15) 0.0134(13) 0.0175(13) -0.0035(10) 0.000 0.000 N1 0.0185(12) 0.0142(12) 0.0121(13) 0.0003(10) 0.0001(10) -0.0015(10) N2 0.0157(11) 0.0140(11) 0.0154(13) -0.0014(10) 0.0003(9) -0.0010(9) N3 0.0169(12) 0.0151(12) 0.0138(13) -0.0008(10) 0.0004(10) -0.0002(10) C1 0.0164(13) 0.0146(13) 0.0169(15) 0.0019(12) 0.0014(12) 0.0036(11) C2 0.0234(14) 0.0099(12) 0.0186(15) 0.0008(12) -0.0004(12) -0.0008(11) C3 0.0156(13) 0.0150(14) 0.0201(17) -0.0014(12) 0.0011(12) -0.0023(11) C4 0.0178(14) 0.0124(14) 0.0197(16) -0.0014(12) -0.0015(12) -0.0020(11) C5 0.0208(15) 0.0178(14) 0.0116(14) -0.0024(12) 0.0000(11) -0.0011(12) C6 0.0212(15) 0.0152(14) 0.0143(15) -0.0022(12) 0.0022(12) -0.0001(12) C7 0.0176(14) 0.0180(15) 0.0156(15) 0.0019(12) 0.0017(12) 0.0003(12) C8 0.0188(14) 0.0182(15) 0.0140(15) -0.0024(12) 0.0008(11) 0.0048(12) C9 0.0215(15) 0.0147(14) 0.0136(15) -0.0004(12) 0.0004(12) 0.0043(12) C10 0.0181(15) 0.0188(15) 0.0198(16) -0.0038(13) 0.0010(12) 0.0033(12) C11 0.0198(15) 0.0282(17) 0.0145(15) -0.0017(13) -0.0039(12) 0.0049(13) C12 0.0230(16) 0.0263(17) 0.0156(16) 0.0002(13) 0.0005(12) 0.0073(13) C13 0.0246(16) 0.0190(15) 0.0145(15) -0.0004(12) 0.0045(12) 0.0019(13) C14 0.0219(16) 0.0185(15) 0.0225(17) -0.0037(13) -0.0050(13) 0.0017(12) C15 0.0202(15) 0.0232(17) 0.0208(17) -0.0008(13) -0.0016(12) -0.0023(12) C16 0.0210(17) 0.034(2) 0.036(2) 0.0034(16) -0.0041(15) 0.0035(15) C17 0.0295(19) 0.0317(19) 0.035(2) 0.0026(16) -0.0050(16) -0.0086(15) C18 0.0274(18) 0.038(2) 0.0267(19) -0.0059(16) 0.0025(14) -0.0068(15) C19 0.0281(18) 0.039(2) 0.0181(19) 0.0071(16) -0.0021(13) 0.0020(15) C20 0.0143(14) 0.0209(15) 0.0172(15) -0.0010(13) 0.0014(11) 0.0017(12) C21 0.0171(15) 0.0203(16) 0.0170(16) 0.0012(13) -0.0004(12) -0.0024(12) C22 0.0201(15) 0.0186(15) 0.0129(15) -0.0025(12) -0.0003(11) -0.0054(11) C23 0.0232(16) 0.0190(15) 0.0149(15) -0.0028(13) -0.0002(12) -0.0024(12) C24 0.0286(17) 0.0264(17) 0.0150(16) 0.0041(13) 0.0024(13) -0.0038(14) C25 0.0246(16) 0.0294(18) 0.0193(17) 0.0022(13) 0.0048(13) -0.0034(13) C26 0.0204(16) 0.0228(16) 0.0225(17) 0.0011(13) 0.0025(13) 0.0032(13) C27 0.0315(18) 0.0172(15) 0.0173(16) 0.0022(13) -0.0018(13) -0.0012(13) C28 0.0257(16) 0.0207(15) 0.0178(15) 0.0023(12) 0.0007(12) 0.0016(13) C29 0.0334(19) 0.044(2) 0.0177(15) -0.0024(14) -0.0029(17) 0.0049(18) C30 0.040(2) 0.0238(18) 0.031(2) 0.0032(15) -0.0066(16) 0.0046(15) C31 0.0254(18) 0.0303(19) 0.047(2) 0.0084(17) 0.0038(16) 0.0000(15) C32 0.038(2) 0.039(2) 0.029(2) 0.0063(16) 0.0139(17) 0.0056(17) C33 0.0228(15) 0.0203(15) 0.0139(15) 0.0023(12) -0.0034(12) 0.0003(12) C34 0.0188(14) 0.0123(13) 0.0192(16) 0.0009(12) 0.0002(12) 0.0017(11) C35 0.0167(12) 0.0115(12) 0.0193(14) 0.0002(13) 0.0003(12) -0.0002(11) C36 0.0183(13) 0.0102(13) 0.0188(15) -0.0002(12) 0.0001(12) -0.0007(10) C37 0.0181(14) 0.0117(14) 0.0259(18) 0.0005(12) 0.0025(12) 0.0003(10) C38 0.0192(14) 0.0121(14) 0.0241(16) 0.0023(13) -0.0041(12) -0.0008(12) C39 0.0218(15) 0.0144(14) 0.0174(16) -0.0005(12) -0.0040(12) -0.0008(12) C40 0.0184(15) 0.0168(15) 0.0217(17) -0.0053(13) 0.0016(12) -0.0009(12) C41 0.0178(14) 0.0196(15) 0.0212(16) -0.0041(13) 0.0021(12) -0.0024(13) C42 0.0204(16) 0.0276(18) 0.0230(17) -0.0027(14) 0.0031(13) -0.0028(13) C43 0.0252(17) 0.038(2) 0.0230(18) -0.0084(15) 0.0047(14) -0.0072(15) C44 0.0264(17) 0.0252(17) 0.0208(17) 0.0032(14) 0.0044(13) 0.0036(14) C45 0.0206(15) 0.0232(16) 0.0276(17) 0.0008(15) -0.0067(13) 0.0033(14) C101 0.037(2) 0.041(2) 0.030(2) 0.0138(19) -0.0020(16) -0.0019(17) C102 0.047(2) 0.033(2) 0.029(2) 0.0073(16) -0.0046(17) 0.0002(17) C103 0.045(2) 0.032(2) 0.034(2) 0.0093(17) -0.0057(18) -0.0070(18) _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 O4 2.0869(2) . ? U1 O2 2.204(2) . ? U1 O3 2.2298(19) . ? U1 O1 2.231(2) . ? U1 N3 2.693(2) . ? U1 N1 2.733(2) . ? U1 N2 2.734(2) . ? O1 C22 1.336(3) . ? O2 C9 1.347(3) . ? O3 C35 1.339(3) . ? O4 U1 2.0869(3) 2_566 ? N1 C1 1.479(4) . ? N1 C6 1.485(4) . ? N1 C20 1.492(4) . ? N2 C3 1.484(3) . ? N2 C2 1.490(4) . ? N2 C7 1.493(4) . ? N3 C5 1.483(4) . ? N3 C4 1.487(4) . ? N3 C33 1.490(4) . ? C1 C2 1.512(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.517(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4B 0.9900 . ? C4 H4C 0.9900 . ? C5 C6 1.522(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.506(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.388(4) . ? C8 C9 1.406(4) . ? C9 C10 1.406(4) . ? C10 C11 1.401(4) . ? C10 C14 1.517(4) . ? C11 C12 1.379(4) . ? C11 H11A 0.9500 . ? C12 C13 1.388(4) . ? C12 C19 1.516(4) . ? C13 H13A 0.9500 . ? C14 C15 1.545(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.525(4) . ? C15 C16 1.528(4) . ? C15 C17 1.530(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.504(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.381(4) . ? C21 C22 1.417(4) . ? C22 C23 1.413(4) . ? C23 C24 1.393(4) . ? C23 C27 1.508(4) . ? C24 C25 1.383(4) . ? C24 H24A 0.9500 . ? C25 C26 1.392(4) . ? C25 C32 1.513(4) . ? C26 H26A 0.9500 . ? C27 C28 1.546(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C31 1.509(4) . ? C28 C29 1.528(4) . ? C28 C30 1.531(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.507(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.389(4) . ? C34 C35 1.409(4) . ? C35 C36 1.415(4) . ? C36 C37 1.393(4) . ? C36 C40 1.515(4) . ? C37 C38 1.391(4) . ? C37 H37A 0.9500 . ? C38 C39 1.383(4) . ? C38 C45 1.515(4) . ? C39 H39A 0.9500 . ? C40 C41 1.558(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C44 1.526(4) . ? C41 C42 1.530(4) . ? C41 C43 1.530(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C101 C103 1.376(5) 5_657 ? C101 C102 1.389(5) . ? C101 H10A 0.9500 . ? C102 C103 1.374(5) . ? C102 H10B 0.9500 . ? C103 C101 1.376(5) 5_657 ? C103 H10C 0.9500 . ? 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 O4 U1 O2 89.89(7) . . ? O4 U1 O3 85.94(9) . . ? O2 U1 O3 116.06(7) . . ? O4 U1 O1 83.99(6) . . ? O2 U1 O1 117.37(8) . . ? O3 U1 O1 125.46(7) . . ? O4 U1 N3 137.53(8) . . ? O2 U1 N3 131.91(7) . . ? O3 U1 N3 70.26(7) . . ? O1 U1 N3 82.32(7) . . ? O4 U1 N1 144.77(9) . . ? O2 U1 N1 80.84(7) . . ? O3 U1 N1 128.66(7) . . ? O1 U1 N1 70.79(7) . . ? N3 U1 N1 64.20(7) . . ? O4 U1 N2 144.62(6) . . ? O2 U1 N2 71.59(7) . . ? O3 U1 N2 76.33(7) . . ? O1 U1 N2 131.18(7) . . ? N3 U1 N2 63.75(7) . . ? N1 U1 N2 63.34(7) . . ? C22 O1 U1 148.03(19) . . ? C9 O2 U1 146.65(18) . . ? C35 O3 U1 144.57(18) . . ? U1 O4 U1 179.97(15) 2_566 . ? C1 N1 C6 110.9(2) . . ? C1 N1 C20 107.7(2) . . ? C6 N1 C20 111.0(2) . . ? C1 N1 U1 107.07(16) . . ? C6 N1 U1 115.53(16) . . ? C20 N1 U1 104.17(16) . . ? C3 N2 C2 111.1(2) . . ? C3 N2 C7 107.8(2) . . ? C2 N2 C7 111.2(2) . . ? C3 N2 U1 107.30(16) . . ? C2 N2 U1 116.45(16) . . ? C7 N2 U1 102.39(16) . . ? C5 N3 C4 110.1(2) . . ? C5 N3 C33 107.7(2) . . ? C4 N3 C33 112.1(2) . . ? C5 N3 U1 106.81(16) . . ? C4 N3 U1 117.43(17) . . ? C33 N3 U1 102.07(16) . . ? N1 C1 C2 112.5(2) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 112.8(2) . . ? N2 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N2 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N2 C3 C4 112.3(2) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 113.1(2) . . ? N3 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? N3 C4 H4C 109.0 . . ? C3 C4 H4C 109.0 . . ? H4B C4 H4C 107.8 . . ? N3 C5 C6 112.2(2) . . ? N3 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N3 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N1 C6 C5 112.4(2) . . ? N1 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 116.2(2) . . ? N2 C7 H7A 108.2 . . ? C8 C7 H7A 108.2 . . ? N2 C7 H7B 108.2 . . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? C13 C8 C9 120.1(3) . . ? C13 C8 C7 119.1(3) . . ? C9 C8 C7 120.4(3) . . ? O2 C9 C8 119.2(3) . . ? O2 C9 C10 121.5(3) . . ? C8 C9 C10 119.2(3) . . ? C11 C10 C9 118.2(3) . . ? C11 C10 C14 120.1(3) . . ? C9 C10 C14 121.1(3) . . ? C12 C11 C10 123.2(3) . . ? C12 C11 H11A 118.4 . . ? C10 C11 H11A 118.4 . . ? C11 C12 C13 117.5(3) . . ? C11 C12 C19 122.3(3) . . ? C13 C12 C19 120.2(3) . . ? C12 C13 C8 121.7(3) . . ? C12 C13 H13A 119.1 . . ? C8 C13 H13A 119.1 . . ? C10 C14 C15 118.7(3) . . ? C10 C14 H14A 107.6 . . ? C15 C14 H14A 107.6 . . ? C10 C14 H14B 107.6 . . ? C15 C14 H14B 107.6 . . ? H14A C14 H14B 107.1 . . ? C18 C15 C16 109.5(3) . . ? C18 C15 C17 108.7(3) . . ? C16 C15 C17 109.3(3) . . ? C18 C15 C14 110.1(3) . . ? C16 C15 C14 111.4(3) . . ? C17 C15 C14 107.9(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 C21 115.4(2) . . ? N1 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? N1 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? C26 C21 C22 120.4(3) . . ? C26 C21 C20 120.4(3) . . ? C22 C21 C20 119.1(3) . . ? O1 C22 C23 121.9(3) . . ? O1 C22 C21 119.0(3) . . ? C23 C22 C21 119.1(3) . . ? C24 C23 C22 117.6(3) . . ? C24 C23 C27 120.3(3) . . ? C22 C23 C27 121.9(3) . . ? C25 C24 C23 123.9(3) . . ? C25 C24 H24A 118.0 . . ? C23 C24 H24A 118.0 . . ? C24 C25 C26 117.4(3) . . ? C24 C25 C32 121.1(3) . . ? C26 C25 C32 121.3(3) . . ? C21 C26 C25 121.3(3) . . ? C21 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C23 C27 C28 119.3(3) . . ? C23 C27 H27A 107.5 . . ? C28 C27 H27A 107.5 . . ? C23 C27 H27B 107.5 . . ? C28 C27 H27B 107.5 . . ? H27A C27 H27B 107.0 . . ? C31 C28 C29 108.9(3) . . ? C31 C28 C30 109.6(3) . . ? C29 C28 C30 108.9(3) . . ? C31 C28 C27 109.6(3) . . ? C29 C28 C27 112.4(3) . . ? C30 C28 C27 107.3(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C32 H32A 109.5 . . ? C25 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C25 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 C34 116.9(2) . . ? N3 C33 H33A 108.1 . . ? C34 C33 H33A 108.1 . . ? N3 C33 H33B 108.1 . . ? C34 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C39 C34 C35 119.7(3) . . ? C39 C34 C33 119.4(3) . . ? C35 C34 C33 120.5(3) . . ? O3 C35 C34 119.2(2) . . ? O3 C35 C36 121.8(3) . . ? C34 C35 C36 119.0(2) . . ? C37 C36 C35 118.2(3) . . ? C37 C36 C40 120.9(3) . . ? C35 C36 C40 120.7(3) . . ? C38 C37 C36 123.5(3) . . ? C38 C37 H37A 118.3 . . ? C36 C37 H37A 118.3 . . ? C39 C38 C37 116.9(3) . . ? C39 C38 C45 121.5(3) . . ? C37 C38 C45 121.5(3) . . ? C38 C39 C34 122.5(3) . . ? C38 C39 H39A 118.8 . . ? C34 C39 H39A 118.8 . . ? C36 C40 C41 117.4(2) . . ? C36 C40 H40A 107.9 . . ? C41 C40 H40A 107.9 . . ? C36 C40 H40B 107.9 . . ? C41 C40 H40B 107.9 . . ? H40A C40 H40B 107.2 . . ? C44 C41 C42 109.5(3) . . ? C44 C41 C43 109.0(3) . . ? C42 C41 C43 108.2(3) . . ? C44 C41 C40 110.8(2) . . ? C42 C41 C40 112.4(3) . . ? C43 C41 C40 106.8(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C38 C45 H45A 109.5 . . ? C38 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C38 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C103 C101 C102 120.1(4) 5_657 . ? C103 C101 H10A 120.0 5_657 . ? C102 C101 H10A 120.0 . . ? C103 C102 C101 120.0(4) . . ? C103 C102 H10B 120.0 . . ? C101 C102 H10B 120.0 . . ? C102 C103 C101 119.9(4) . 5_657 ? C102 C103 H10C 120.1 . . ? C101 C103 H10C 120.1 5_657 . ? 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 O4 U1 O1 C22 -142.8(4) . . . . ? O2 U1 O1 C22 -56.1(4) . . . . ? O3 U1 O1 C22 136.5(3) . . . . ? N3 U1 O1 C22 77.5(3) . . . . ? N1 U1 O1 C22 12.2(3) . . . . ? N2 U1 O1 C22 32.8(4) . . . . ? O4 U1 O2 C9 -128.2(3) . . . . ? O3 U1 O2 C9 -42.8(3) . . . . ? O1 U1 O2 C9 148.6(3) . . . . ? N3 U1 O2 C9 43.4(4) . . . . ? N1 U1 O2 C9 85.9(3) . . . . ? N2 U1 O2 C9 21.1(3) . . . . ? O4 U1 O3 C35 -110.5(3) . . . . ? O2 U1 O3 C35 161.6(3) . . . . ? O1 U1 O3 C35 -30.8(3) . . . . ? N3 U1 O3 C35 33.7(3) . . . . ? N1 U1 O3 C35 62.2(3) . . . . ? N2 U1 O3 C35 100.3(3) . . . . ? O4 U1 N1 C1 -112.99(16) . . . . ? O2 U1 N1 C1 -36.39(16) . . . . ? O3 U1 N1 C1 79.76(18) . . . . ? O1 U1 N1 C1 -159.71(18) . . . . ? N3 U1 N1 C1 109.65(17) . . . . ? N2 U1 N1 C1 37.52(16) . . . . ? O4 U1 N1 C6 122.96(17) . . . . ? O2 U1 N1 C6 -160.44(19) . . . . ? O3 U1 N1 C6 -44.3(2) . . . . ? O1 U1 N1 C6 76.24(18) . . . . ? N3 U1 N1 C6 -14.40(18) . . . . ? N2 U1 N1 C6 -86.53(19) . . . . ? O4 U1 N1 C20 0.9(2) . . . . ? O2 U1 N1 C20 77.53(17) . . . . ? O3 U1 N1 C20 -166.31(15) . . . . ? O1 U1 N1 C20 -45.79(16) . . . . ? N3 U1 N1 C20 -136.43(18) . . . . ? N2 U1 N1 C20 151.44(18) . . . . ? O4 U1 N2 C3 -100.0(2) . . . . ? O2 U1 N2 C3 -161.79(18) . . . . ? O3 U1 N2 C3 -37.91(16) . . . . ? O1 U1 N2 C3 87.57(18) . . . . ? N3 U1 N2 C3 36.57(16) . . . . ? N1 U1 N2 C3 109.39(18) . . . . ? O4 U1 N2 C2 134.9(2) . . . . ? O2 U1 N2 C2 73.09(19) . . . . ? O3 U1 N2 C2 -163.0(2) . . . . ? O1 U1 N2 C2 -37.6(2) . . . . ? N3 U1 N2 C2 -88.55(19) . . . . ? N1 U1 N2 C2 -15.73(18) . . . . ? O4 U1 N2 C7 13.4(2) . . . . ? O2 U1 N2 C7 -48.40(16) . . . . ? O3 U1 N2 C7 75.48(16) . . . . ? O1 U1 N2 C7 -159.04(15) . . . . ? N3 U1 N2 C7 149.96(18) . . . . ? N1 U1 N2 C7 -137.22(17) . . . . ? O4 U1 N3 C5 -107.32(18) . . . . ? O2 U1 N3 C5 85.14(19) . . . . ? O3 U1 N3 C5 -167.09(18) . . . . ? O1 U1 N3 C5 -35.01(17) . . . . ? N1 U1 N3 C5 37.32(16) . . . . ? N2 U1 N3 C5 108.82(18) . . . . ? O4 U1 N3 C4 128.57(18) . . . . ? O2 U1 N3 C4 -39.0(2) . . . . ? O3 U1 N3 C4 68.79(18) . . . . ? O1 U1 N3 C4 -159.12(19) . . . . ? N1 U1 N3 C4 -86.79(19) . . . . ? N2 U1 N3 C4 -15.30(17) . . . . ? O4 U1 N3 C33 5.6(2) . . . . ? O2 U1 N3 C33 -161.96(15) . . . . ? O3 U1 N3 C33 -54.19(16) . . . . ? O1 U1 N3 C33 77.89(17) . . . . ? N1 U1 N3 C33 150.22(18) . . . . ? N2 U1 N3 C33 -138.28(18) . . . . ? C6 N1 C1 C2 66.7(3) . . . . ? C20 N1 C1 C2 -171.7(2) . . . . ? U1 N1 C1 C2 -60.2(2) . . . . ? C3 N2 C2 C1 -131.3(3) . . . . ? C7 N2 C2 C1 108.6(3) . . . . ? U1 N2 C2 C1 -8.2(3) . . . . ? N1 C1 C2 N2 46.8(3) . . . . ? C2 N2 C3 C4 70.3(3) . . . . ? C7 N2 C3 C4 -167.6(2) . . . . ? U1 N2 C3 C4 -58.0(2) . . . . ? C5 N3 C4 C3 -130.5(2) . . . . ? C33 N3 C4 C3 109.7(3) . . . . ? U1 N3 C4 C3 -8.0(3) . . . . ? N2 C3 C4 N3 45.4(3) . . . . ? C4 N3 C5 C6 67.4(3) . . . . ? C33 N3 C5 C6 -170.1(2) . . . . ? U1 N3 C5 C6 -61.1(2) . . . . ? C1 N1 C6 C5 -132.5(2) . . . . ? C20 N1 C6 C5 107.8(3) . . . . ? U1 N1 C6 C5 -10.5(3) . . . . ? N3 C5 C6 N1 48.9(3) . . . . ? C3 N2 C7 C8 -168.8(2) . . . . ? C2 N2 C7 C8 -46.9(3) . . . . ? U1 N2 C7 C8 78.2(2) . . . . ? N2 C7 C8 C13 130.2(3) . . . . ? N2 C7 C8 C9 -57.2(4) . . . . ? U1 O2 C9 C8 -1.5(5) . . . . ? U1 O2 C9 C10 175.5(2) . . . . ? C13 C8 C9 O2 179.1(3) . . . . ? C7 C8 C9 O2 6.6(4) . . . . ? C13 C8 C9 C10 2.0(4) . . . . ? C7 C8 C9 C10 -170.5(3) . . . . ? O2 C9 C10 C11 -177.6(3) . . . . ? C8 C9 C10 C11 -0.6(4) . . . . ? O2 C9 C10 C14 -6.6(4) . . . . ? C8 C9 C10 C14 170.4(3) . . . . ? C9 C10 C11 C12 -1.3(5) . . . . ? C14 C10 C11 C12 -172.4(3) . . . . ? C10 C11 C12 C13 1.7(5) . . . . ? C10 C11 C12 C19 179.3(3) . . . . ? C11 C12 C13 C8 -0.2(4) . . . . ? C19 C12 C13 C8 -177.8(3) . . . . ? C9 C8 C13 C12 -1.6(4) . . . . ? C7 C8 C13 C12 171.0(3) . . . . ? C11 C10 C14 C15 -83.6(4) . . . . ? C9 C10 C14 C15 105.6(3) . . . . ? C10 C14 C15 C18 -62.8(4) . . . . ? C10 C14 C15 C16 58.8(4) . . . . ? C10 C14 C15 C17 178.7(3) . . . . ? C1 N1 C20 C21 -167.5(2) . . . . ? C6 N1 C20 C21 -46.0(3) . . . . ? U1 N1 C20 C21 79.0(3) . . . . ? N1 C20 C21 C26 123.4(3) . . . . ? N1 C20 C21 C22 -59.1(4) . . . . ? U1 O1 C22 C23 -173.9(2) . . . . ? U1 O1 C22 C21 7.3(5) . . . . ? C26 C21 C22 O1 -176.1(3) . . . . ? C20 C21 C22 O1 6.4(4) . . . . ? C26 C21 C22 C23 5.1(4) . . . . ? C20 C21 C22 C23 -172.4(3) . . . . ? O1 C22 C23 C24 177.3(3) . . . . ? C21 C22 C23 C24 -3.9(4) . . . . ? O1 C22 C23 C27 -7.9(4) . . . . ? C21 C22 C23 C27 170.9(3) . . . . ? C22 C23 C24 C25 -0.6(5) . . . . ? C27 C23 C24 C25 -175.5(3) . . . . ? C23 C24 C25 C26 4.0(5) . . . . ? C23 C24 C25 C32 -172.8(3) . . . . ? C22 C21 C26 C25 -1.7(5) . . . . ? C20 C21 C26 C25 175.8(3) . . . . ? C24 C25 C26 C21 -2.8(5) . . . . ? C32 C25 C26 C21 173.9(3) . . . . ? C24 C23 C27 C28 -79.1(4) . . . . ? C22 C23 C27 C28 106.2(3) . . . . ? C23 C27 C28 C31 -64.7(4) . . . . ? C23 C27 C28 C29 56.5(4) . . . . ? C23 C27 C28 C30 176.3(3) . . . . ? C5 N3 C33 C34 -168.9(2) . . . . ? C4 N3 C33 C34 -47.7(3) . . . . ? U1 N3 C33 C34 78.8(3) . . . . ? N3 C33 C34 C39 137.0(3) . . . . ? N3 C33 C34 C35 -50.4(4) . . . . ? U1 O3 C35 C34 -11.4(5) . . . . ? U1 O3 C35 C36 168.1(2) . . . . ? C39 C34 C35 O3 176.0(3) . . . . ? C33 C34 C35 O3 3.3(4) . . . . ? C39 C34 C35 C36 -3.6(4) . . . . ? C33 C34 C35 C36 -176.2(3) . . . . ? O3 C35 C36 C37 -174.3(3) . . . . ? C34 C35 C36 C37 5.2(4) . . . . ? O3 C35 C36 C40 0.3(4) . . . . ? C34 C35 C36 C40 179.9(3) . . . . ? C35 C36 C37 C38 -3.1(4) . . . . ? C40 C36 C37 C38 -177.8(3) . . . . ? C36 C37 C38 C39 -0.8(4) . . . . ? C36 C37 C38 C45 175.1(3) . . . . ? C37 C38 C39 C34 2.6(4) . . . . ? C45 C38 C39 C34 -173.3(3) . . . . ? C35 C34 C39 C38 -0.4(5) . . . . ? C33 C34 C39 C38 172.3(3) . . . . ? C37 C36 C40 C41 -73.2(4) . . . . ? C35 C36 C40 C41 112.3(3) . . . . ? C36 C40 C41 C44 -61.8(3) . . . . ? C36 C40 C41 C42 61.0(3) . . . . ? C36 C40 C41 C43 179.6(3) . . . . ? C103 C101 C102 C103 -0.2(6) 5_657 . . . ? C101 C102 C103 C101 0.2(6) . . . 5_657 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.103 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.103 #===END OF DATA FOR 4 * benzene # Attachment '- CCDC_886106.cif' data_acs1105a _database_code_depnum_ccdc_archive 'CCDC 886106' #TrackingRef '- CCDC_886106.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C91 H132 N6 O9 U2, 2.5(C6 H6)' _chemical_formula_sum 'C106 H147 N6 O9 U2' _chemical_formula_weight 2125.36 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 P2(1)/n _symmetry_space_group_name_Hall -P2yn 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 17.0385(2) _cell_length_b 23.9304(3) _cell_length_c 24.1626(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.9860(10) _cell_angle_gamma 90.00 _cell_volume 9798.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9858 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.81 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4324 _exptl_absorpt_coefficient_mu 3.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2008' _exptl_special_details ; ? ; _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 'Bruker Smart APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 150266 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.10 _reflns_number_total 21565 _reflns_number_gt 16522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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. One large residual electron density maximum (> 7.0) is located very close to U1 (< 0.81 ). The next highest maximum (2.20) is located close to U2 (< 0.77 ). ; _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^)+(0.0250P)^2^+38.8149P] 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 21565 _refine_ls_number_parameters 1132 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 -0.099433(10) 0.175181(7) 0.239493(7) 0.01830(5) Uani 1 1 d . . . O1 O -0.09678(19) 0.12251(13) 0.16561(13) 0.0230(7) Uani 1 1 d . . . O2 O -0.09121(19) 0.19260(13) 0.32718(13) 0.0211(7) Uani 1 1 d . . . O3 O -0.15790(19) 0.09769(13) 0.26706(14) 0.0242(7) Uani 1 1 d . . . N1 N -0.1266(3) 0.23885(18) 0.14703(19) 0.0352(11) Uani 1 1 d . . . N2 N -0.1569(2) 0.28020(16) 0.25740(17) 0.0231(9) Uani 1 1 d . . . N3 N -0.2513(3) 0.1890(2) 0.2024(2) 0.0423(12) Uani 1 1 d U . . C1 C -0.1075(4) 0.2975(2) 0.1651(3) 0.0441(15) Uani 1 1 d . . . H1A H -0.0511 0.2996 0.1798 0.053 Uiso 1 1 calc R . . H1B H -0.1157 0.3225 0.1324 0.053 Uiso 1 1 calc R . . C2 C -0.1558(4) 0.3174(2) 0.2080(2) 0.0355(13) Uani 1 1 d . . . H2A H -0.2107 0.3223 0.1909 0.043 Uiso 1 1 calc R . . H2B H -0.1360 0.3546 0.2210 0.043 Uiso 1 1 calc R . . C3 C -0.2400(3) 0.2689(3) 0.2695(2) 0.0394(14) Uani 1 1 d . . . H3A H -0.2659 0.3049 0.2765 0.047 Uiso 1 1 calc R . . H3B H -0.2388 0.2462 0.3038 0.047 Uiso 1 1 calc R . . C4 C -0.2896(3) 0.2380(3) 0.2216(3) 0.0502(16) Uani 1 1 d U . . H4A H -0.3406 0.2268 0.2345 0.060 Uiso 1 1 calc R . . H4B H -0.3010 0.2641 0.1900 0.060 Uiso 1 1 calc R . . C5 C -0.2517(3) 0.1911(3) 0.1383(2) 0.0417(14) Uani 1 1 d U . . H5A H -0.2322 0.1548 0.1256 0.050 Uiso 1 1 calc R . . H5B H -0.3069 0.1954 0.1216 0.050 Uiso 1 1 calc R . . C6 C -0.2051(4) 0.2351(3) 0.1174(3) 0.0465(16) Uani 1 1 d . . . H6A H -0.2326 0.2712 0.1207 0.056 Uiso 1 1 calc R . . H6B H -0.2004 0.2283 0.0775 0.056 Uiso 1 1 calc R . . C7 C -0.0657(4) 0.2227(2) 0.1104(2) 0.0363(14) Uani 1 1 d . . . H7A H -0.0139 0.2213 0.1332 0.044 Uiso 1 1 calc R . . H7B H -0.0625 0.2524 0.0822 0.044 Uiso 1 1 calc R . . C8 C -0.0786(3) 0.1683(2) 0.0810(2) 0.0267(11) Uani 1 1 d . . . C9 C -0.0895(3) 0.1187(2) 0.11105(19) 0.0222(10) Uani 1 1 d . . . C10 C -0.0899(3) 0.0666(2) 0.0841(2) 0.0216(10) Uani 1 1 d . . . C11 C -0.0778(3) 0.0662(2) 0.0279(2) 0.0265(11) Uani 1 1 d . . . H11A H -0.0757 0.0311 0.0097 0.032 Uiso 1 1 calc R . . C12 C -0.0687(3) 0.1143(2) -0.0029(2) 0.0288(11) Uani 1 1 d . . . C13 C -0.0700(3) 0.1650(2) 0.0250(2) 0.0295(12) Uani 1 1 d . . . H13A H -0.0648 0.1986 0.0047 0.035 Uiso 1 1 calc R . . C14 C -0.0973(3) 0.01247(19) 0.1153(2) 0.0231(10) Uani 1 1 d . . . H14A H -0.0852 0.0203 0.1555 0.028 Uiso 1 1 calc R . . H14B H -0.0563 -0.0134 0.1045 0.028 Uiso 1 1 calc R . . C15 C -0.1774(3) -0.0182(2) 0.1070(2) 0.0288(12) Uani 1 1 d . . . C16 C -0.2027(3) -0.0301(3) 0.0460(2) 0.0369(14) Uani 1 1 d . . . H16A H -0.2519 -0.0517 0.0426 0.055 Uiso 1 1 calc R . . H16B H -0.1614 -0.0515 0.0301 0.055 Uiso 1 1 calc R . . H16C H -0.2113 0.0053 0.0258 0.055 Uiso 1 1 calc R . . C17 C -0.1676(4) -0.0736(2) 0.1385(2) 0.0366(14) Uani 1 1 d . . . H17A H -0.2177 -0.0940 0.1345 0.055 Uiso 1 1 calc R . . H17B H -0.1518 -0.0662 0.1780 0.055 Uiso 1 1 calc R . . H17C H -0.1269 -0.0961 0.1232 0.055 Uiso 1 1 calc R . . C18 C -0.2392(3) 0.0175(2) 0.1313(3) 0.0393(14) Uani 1 1 d . . . H18A H -0.2892 -0.0030 0.1291 0.059 Uiso 1 1 calc R . . H18B H -0.2466 0.0523 0.1100 0.059 Uiso 1 1 calc R . . H18C H -0.2215 0.0261 0.1702 0.059 Uiso 1 1 calc R . . C19 C -0.0548(3) 0.1118(2) -0.0636(2) 0.0352(13) Uani 1 1 d . . . H19A H -0.0801 0.0783 -0.0806 0.053 Uiso 1 1 calc R . . H19B H 0.0020 0.1104 -0.0668 0.053 Uiso 1 1 calc R . . H19C H -0.0774 0.1451 -0.0828 0.053 Uiso 1 1 calc R . . C20 C -0.1119(3) 0.30834(19) 0.3059(2) 0.0241(11) Uani 1 1 d . . . H20A H -0.1310 0.3473 0.3074 0.029 Uiso 1 1 calc R . . H20B H -0.0557 0.3100 0.2989 0.029 Uiso 1 1 calc R . . C21 C -0.1160(3) 0.28256(19) 0.3622(2) 0.0199(10) Uani 1 1 d . . . C22 C -0.0998(3) 0.22574(19) 0.3714(2) 0.0189(10) Uani 1 1 d . . . C23 C -0.0953(3) 0.20383(18) 0.42529(19) 0.0176(9) Uani 1 1 d . . . C24 C -0.1134(3) 0.2390(2) 0.4683(2) 0.0225(10) Uani 1 1 d . . . H24A H -0.1124 0.2239 0.5048 0.027 Uiso 1 1 calc R . . C25 C -0.1329(3) 0.2952(2) 0.4601(2) 0.0212(10) Uani 1 1 d . . . C26 C -0.1324(3) 0.31601(19) 0.4069(2) 0.0223(10) Uani 1 1 d . . . H26A H -0.1436 0.3545 0.4004 0.027 Uiso 1 1 calc R . . C27 C -0.0729(3) 0.14398(19) 0.43728(19) 0.0201(10) Uani 1 1 d . . . H27A H -0.0903 0.1214 0.4039 0.024 Uiso 1 1 calc R . . H27B H -0.1023 0.1306 0.4679 0.024 Uiso 1 1 calc R . . C28 C 0.0156(3) 0.13300(19) 0.4534(2) 0.0215(10) Uani 1 1 d . . . C29 C 0.0628(3) 0.1473(2) 0.4047(2) 0.0331(12) Uani 1 1 d . . . H29A H 0.0418 0.1262 0.3717 0.050 Uiso 1 1 calc R . . H29B H 0.1184 0.1374 0.4145 0.050 Uiso 1 1 calc R . . H29C H 0.0585 0.1874 0.3968 0.050 Uiso 1 1 calc R . . C30 C 0.0267(3) 0.0709(2) 0.4665(2) 0.0281(11) Uani 1 1 d . . . H30A H -0.0043 0.0607 0.4970 0.042 Uiso 1 1 calc R . . H30B H 0.0827 0.0634 0.4777 0.042 Uiso 1 1 calc R . . H30C H 0.0090 0.0488 0.4334 0.042 Uiso 1 1 calc R . . C31 C 0.0471(3) 0.1668(2) 0.5047(2) 0.0312(12) Uani 1 1 d . . . H31A H 0.0164 0.1579 0.5356 0.047 Uiso 1 1 calc R . . H31B H 0.0425 0.2068 0.4962 0.047 Uiso 1 1 calc R . . H31C H 0.1027 0.1573 0.5151 0.047 Uiso 1 1 calc R . . C32 C -0.1557(3) 0.3306(2) 0.5075(2) 0.0281(11) Uani 1 1 d . . . H32A H -0.1979 0.3564 0.4937 0.042 Uiso 1 1 calc R . . H32B H -0.1097 0.3520 0.5235 0.042 Uiso 1 1 calc R . . H32C H -0.1742 0.3064 0.5362 0.042 Uiso 1 1 calc R . . C33 C -0.2980(3) 0.1380(2) 0.2159(3) 0.0419(15) Uani 1 1 d . . . H33A H -0.3544 0.1452 0.2037 0.050 Uiso 1 1 calc R . . H33B H -0.2811 0.1063 0.1937 0.050 Uiso 1 1 calc R . . C34 C -0.2909(3) 0.1206(2) 0.2763(3) 0.0396(15) Uani 1 1 d . . . C35 C -0.2201(3) 0.0942(2) 0.2967(2) 0.0274(12) Uani 1 1 d . . . C36 C -0.2173(3) 0.0640(2) 0.3469(2) 0.0319(13) Uani 1 1 d . . . C37 C -0.2830(4) 0.0681(3) 0.3779(3) 0.0498(19) Uani 1 1 d . . . H37A H -0.2808 0.0498 0.4129 0.060 Uiso 1 1 calc R . . C38 C -0.3507(4) 0.0980(3) 0.3591(4) 0.063(2) Uani 1 1 d . . . C39 C -0.3538(4) 0.1220(3) 0.3072(3) 0.055(2) Uani 1 1 d . . . H39A H -0.4009 0.1401 0.2923 0.066 Uiso 1 1 calc R . . C40 C -0.1489(3) 0.0265(2) 0.3652(2) 0.0321(13) Uani 1 1 d . . . H40A H -0.1372 0.0300 0.4060 0.039 Uiso 1 1 calc R . . H40B H -0.1021 0.0403 0.3482 0.039 Uiso 1 1 calc R . . C41 C -0.1594(4) -0.0367(2) 0.3509(2) 0.0328(13) Uani 1 1 d . . . C42 C -0.1823(4) -0.0437(2) 0.2885(2) 0.0353(13) Uani 1 1 d . . . H42A H -0.1833 -0.0835 0.2790 0.053 Uiso 1 1 calc R . . H42B H -0.1435 -0.0245 0.2680 0.053 Uiso 1 1 calc R . . H42C H -0.2346 -0.0275 0.2784 0.053 Uiso 1 1 calc R . . C43 C -0.0811(4) -0.0650(3) 0.3668(3) 0.0518(18) Uani 1 1 d . . . H43A H -0.0873 -0.1056 0.3623 0.078 Uiso 1 1 calc R . . H43B H -0.0627 -0.0564 0.4056 0.078 Uiso 1 1 calc R . . H43C H -0.0424 -0.0515 0.3426 0.078 Uiso 1 1 calc R . . C44 C -0.2224(5) -0.0629(3) 0.3834(3) 0.059(2) Uani 1 1 d . . . H44A H -0.2246 -0.1032 0.3765 0.088 Uiso 1 1 calc R . . H44B H -0.2738 -0.0462 0.3712 0.088 Uiso 1 1 calc R . . H44C H -0.2091 -0.0559 0.4232 0.088 Uiso 1 1 calc R . . C45 C -0.4189(5) 0.1003(4) 0.3948(4) 0.095(3) Uani 1 1 d U . . H45A H -0.4686 0.1039 0.3708 0.142 Uiso 1 1 calc R . . H45B H -0.4123 0.1326 0.4198 0.142 Uiso 1 1 calc R . . H45C H -0.4197 0.0660 0.4168 0.142 Uiso 1 1 calc R . . U2 U 0.203365(10) 0.146060(7) 0.220090(7) 0.01608(5) Uani 1 1 d . . . O4 O 0.22764(17) 0.11474(13) 0.30386(13) 0.0188(7) Uani 1 1 d . . . O5 O 0.1872(2) 0.20322(13) 0.15008(13) 0.0233(7) Uani 1 1 d . . . O6 O 0.32082(18) 0.18584(13) 0.23605(14) 0.0232(7) Uani 1 1 d . . . O7 O 0.05090(17) 0.15793(13) 0.23280(13) 0.0191(7) Uani 1 1 d . . . O8 O 0.00913(18) 0.24150(13) 0.24988(14) 0.0235(7) Uani 1 1 d . . . O9 O 0.13900(18) 0.22169(13) 0.26020(13) 0.0212(7) Uani 1 1 d . . . N4 N 0.1473(2) 0.04040(15) 0.22977(16) 0.0196(8) Uani 1 1 d . . . N5 N 0.1665(2) 0.08897(15) 0.12075(16) 0.0195(8) Uani 1 1 d . . . N6 N 0.3071(2) 0.06455(15) 0.19870(16) 0.0179(8) Uani 1 1 d . . . C46 C 0.0881(3) 0.03184(19) 0.18102(19) 0.0206(10) Uani 1 1 d . . . H46A H 0.0464 0.0606 0.1813 0.025 Uiso 1 1 calc R . . H46B H 0.0631 -0.0052 0.1840 0.025 Uiso 1 1 calc R . . C47 C 0.1247(3) 0.0352(2) 0.1264(2) 0.0239(11) Uani 1 1 d . . . H47A H 0.1623 0.0039 0.1244 0.029 Uiso 1 1 calc R . . H47B H 0.0827 0.0311 0.0951 0.029 Uiso 1 1 calc R . . C48 C 0.2455(3) 0.0811(2) 0.10130(19) 0.0212(10) Uani 1 1 d . . . H48A H 0.2701 0.1182 0.0975 0.025 Uiso 1 1 calc R . . H48B H 0.2390 0.0636 0.0640 0.025 Uiso 1 1 calc R . . C49 C 0.3002(3) 0.04535(19) 0.13980(19) 0.0222(10) Uani 1 1 d . . . H49A H 0.2807 0.0064 0.1381 0.027 Uiso 1 1 calc R . . H49B H 0.3533 0.0455 0.1266 0.027 Uiso 1 1 calc R . . C50 C 0.2931(3) 0.01773(18) 0.23724(19) 0.0181(9) Uani 1 1 d . . . H50A H 0.3063 0.0307 0.2760 0.022 Uiso 1 1 calc R . . H50B H 0.3295 -0.0133 0.2307 0.022 Uiso 1 1 calc R . . C51 C 0.2093(3) -0.00439(19) 0.23098(19) 0.0203(10) Uani 1 1 d . . . H51A H 0.2008 -0.0263 0.1961 0.024 Uiso 1 1 calc R . . H51B H 0.2027 -0.0301 0.2623 0.024 Uiso 1 1 calc R . . C52 C 0.1045(3) 0.0382(2) 0.28028(19) 0.0202(10) Uani 1 1 d . . . H52A H 0.0707 0.0044 0.2783 0.024 Uiso 1 1 calc R . . H52B H 0.0695 0.0712 0.2805 0.024 Uiso 1 1 calc R . . C53 C 0.1576(3) 0.03692(19) 0.33323(19) 0.0194(10) Uani 1 1 d . . . C54 C 0.2190(3) 0.07587(18) 0.34328(18) 0.0170(9) Uani 1 1 d . . . C55 C 0.2723(3) 0.07218(19) 0.39084(19) 0.0201(10) Uani 1 1 d . . . C56 C 0.2588(3) 0.0310(2) 0.4300(2) 0.0240(11) Uani 1 1 d . . . H56A H 0.2944 0.0284 0.4629 0.029 Uiso 1 1 calc R . . C57 C 0.1963(3) -0.0060(2) 0.4230(2) 0.0245(11) Uani 1 1 d . . . C58 C 0.1470(3) -0.00300(19) 0.37342(19) 0.0215(10) Uani 1 1 d . . . H58A H 0.1050 -0.0291 0.3669 0.026 Uiso 1 1 calc R . . C59 C 0.3447(3) 0.10892(19) 0.3997(2) 0.0221(10) Uani 1 1 d . . . H59A H 0.3606 0.1190 0.3628 0.027 Uiso 1 1 calc R . . H59B H 0.3880 0.0865 0.4191 0.027 Uiso 1 1 calc R . . C60 C 0.3375(3) 0.1633(2) 0.4329(2) 0.0355(13) Uani 1 1 d . . . C61 C 0.3094(4) 0.1514(3) 0.4895(2) 0.0550(19) Uani 1 1 d . . . H61A H 0.2564 0.1351 0.4844 0.082 Uiso 1 1 calc R . . H61B H 0.3080 0.1864 0.5105 0.082 Uiso 1 1 calc R . . H61C H 0.3457 0.1252 0.5100 0.082 Uiso 1 1 calc R . . C62 C 0.4205(4) 0.1888(3) 0.4410(3) 0.056(2) Uani 1 1 d . . . H62A H 0.4395 0.1951 0.4046 0.084 Uiso 1 1 calc R . . H62B H 0.4564 0.1631 0.4628 0.084 Uiso 1 1 calc R . . H62C H 0.4187 0.2245 0.4608 0.084 Uiso 1 1 calc R . . C63 C 0.2812(3) 0.2039(2) 0.4003(3) 0.0433(16) Uani 1 1 d . . . H63A H 0.2992 0.2109 0.3638 0.065 Uiso 1 1 calc R . . H63B H 0.2800 0.2392 0.4208 0.065 Uiso 1 1 calc R . . H63C H 0.2280 0.1878 0.3955 0.065 Uiso 1 1 calc R . . C64 C 0.1812(3) -0.0488(2) 0.4666(2) 0.0320(12) Uani 1 1 d . . . H64A H 0.2316 -0.0606 0.4865 0.048 Uiso 1 1 calc R . . H64B H 0.1545 -0.0813 0.4486 0.048 Uiso 1 1 calc R . . H64C H 0.1478 -0.0324 0.4930 0.048 Uiso 1 1 calc R . . C65 C 0.1142(3) 0.1225(2) 0.07932(19) 0.0216(10) Uani 1 1 d . . . H65A H 0.0982 0.0981 0.0470 0.026 Uiso 1 1 calc R . . H65B H 0.0658 0.1322 0.0965 0.026 Uiso 1 1 calc R . . C66 C 0.1473(3) 0.1755(2) 0.0579(2) 0.0223(10) Uani 1 1 d . . . C67 C 0.1777(3) 0.21601(19) 0.0953(2) 0.0211(10) Uani 1 1 d . . . C68 C 0.1994(3) 0.26864(19) 0.0747(2) 0.0220(10) Uani 1 1 d . . . C69 C 0.1928(3) 0.2767(2) 0.0177(2) 0.0251(11) Uani 1 1 d . . . H69A H 0.2084 0.3118 0.0040 0.030 Uiso 1 1 calc R . . C70 C 0.1644(3) 0.2362(2) -0.0206(2) 0.0264(11) Uani 1 1 d . . . C71 C 0.1404(3) 0.1858(2) 0.0009(2) 0.0239(11) Uani 1 1 d . . . H71A H 0.1187 0.1577 -0.0240 0.029 Uiso 1 1 calc R . . C72 C 0.2258(3) 0.3152(2) 0.1144(2) 0.0267(11) Uani 1 1 d . . . H72A H 0.2671 0.3371 0.0982 0.032 Uiso 1 1 calc R . . H72B H 0.2502 0.2984 0.1495 0.032 Uiso 1 1 calc R . . C73 C 0.1605(3) 0.3556(2) 0.1285(2) 0.0303(12) Uani 1 1 d . . . C74 C 0.1228(4) 0.3867(2) 0.0766(2) 0.0394(14) Uani 1 1 d . . . H74A H 0.0976 0.3597 0.0499 0.059 Uiso 1 1 calc R . . H74B H 0.1637 0.4072 0.0593 0.059 Uiso 1 1 calc R . . H74C H 0.0831 0.4131 0.0875 0.059 Uiso 1 1 calc R . . C75 C 0.1976(4) 0.3982(2) 0.1702(2) 0.0413(15) Uani 1 1 d . . . H75A H 0.2213 0.3788 0.2035 0.062 Uiso 1 1 calc R . . H75B H 0.1569 0.4241 0.1804 0.062 Uiso 1 1 calc R . . H75C H 0.2385 0.4192 0.1534 0.062 Uiso 1 1 calc R . . C76 C 0.0969(4) 0.3239(2) 0.1549(3) 0.0442(15) Uani 1 1 d . . . H76A H 0.0722 0.2966 0.1282 0.066 Uiso 1 1 calc R . . H76B H 0.0569 0.3502 0.1653 0.066 Uiso 1 1 calc R . . H76C H 0.1205 0.3043 0.1882 0.066 Uiso 1 1 calc R . . C77 C 0.1613(3) 0.2463(2) -0.0822(2) 0.0336(13) Uani 1 1 d . . . H77A H 0.2037 0.2721 -0.0897 0.050 Uiso 1 1 calc R . . H77B H 0.1102 0.2628 -0.0957 0.050 Uiso 1 1 calc R . . H77C H 0.1680 0.2108 -0.1014 0.050 Uiso 1 1 calc R . . C78 C 0.3896(3) 0.08476(18) 0.2153(2) 0.0187(10) Uani 1 1 d . . . H78A H 0.4270 0.0548 0.2076 0.022 Uiso 1 1 calc R . . H78B H 0.3959 0.0918 0.2559 0.022 Uiso 1 1 calc R . . C79 C 0.4111(3) 0.13702(18) 0.1858(2) 0.0198(10) Uani 1 1 d . . . C80 C 0.3792(3) 0.18741(19) 0.2026(2) 0.0210(10) Uani 1 1 d . . . C81 C 0.4096(3) 0.2385(2) 0.1849(2) 0.0234(11) Uani 1 1 d . . . C82 C 0.4624(3) 0.2363(2) 0.1445(2) 0.0251(11) Uani 1 1 d . . . H82A H 0.4807 0.2705 0.1306 0.030 Uiso 1 1 calc R . . C83 C 0.4893(3) 0.1867(2) 0.1235(2) 0.0264(11) Uani 1 1 d . . . C84 C 0.4652(3) 0.1369(2) 0.1470(2) 0.0231(10) Uani 1 1 d . . . H84A H 0.4864 0.1024 0.1360 0.028 Uiso 1 1 calc R . . C85 C 0.3898(3) 0.2933(2) 0.2107(2) 0.0262(11) Uani 1 1 d . . . H85A H 0.3361 0.2905 0.2226 0.031 Uiso 1 1 calc R . . H85B H 0.3885 0.3226 0.1817 0.031 Uiso 1 1 calc R . . C86 C 0.4469(3) 0.3123(2) 0.2612(2) 0.0293(12) Uani 1 1 d . . . C87 C 0.4449(4) 0.2717(3) 0.3091(3) 0.061(2) Uani 1 1 d . . . H87A H 0.4767 0.2865 0.3420 0.091 Uiso 1 1 calc R . . H87B H 0.4663 0.2356 0.2989 0.091 Uiso 1 1 calc R . . H87C H 0.3902 0.2668 0.3175 0.091 Uiso 1 1 calc R . . C88 C 0.5304(3) 0.3182(3) 0.2458(3) 0.067(2) Uani 1 1 d . . . H88A H 0.5648 0.3314 0.2782 0.100 Uiso 1 1 calc R . . H88B H 0.5313 0.3451 0.2154 0.100 Uiso 1 1 calc R . . H88C H 0.5492 0.2818 0.2340 0.100 Uiso 1 1 calc R . . C89 C 0.4198(4) 0.3695(2) 0.2788(3) 0.0392(14) Uani 1 1 d . . . H89A H 0.4564 0.3835 0.3097 0.059 Uiso 1 1 calc R . . H89B H 0.3668 0.3664 0.2909 0.059 Uiso 1 1 calc R . . H89C H 0.4186 0.3954 0.2473 0.059 Uiso 1 1 calc R . . C90 C 0.5411(3) 0.1864(2) 0.0767(2) 0.0322(13) Uani 1 1 d . . . H90A H 0.5757 0.2192 0.0798 0.048 Uiso 1 1 calc R . . H90B H 0.5081 0.1873 0.0410 0.048 Uiso 1 1 calc R . . H90C H 0.5733 0.1524 0.0789 0.048 Uiso 1 1 calc R . . C91 C 0.0668(3) 0.2079(2) 0.24825(18) 0.0194(10) Uani 1 1 d . . . C101 C 0.1812(3) 0.3300(2) 0.3468(2) 0.0342(13) Uani 1 1 d . . . H10A H 0.1885 0.3245 0.3087 0.041 Uiso 1 1 calc R . . C102 C 0.2338(3) 0.3620(2) 0.3794(3) 0.0386(14) Uani 1 1 d . . . H10B H 0.2767 0.3791 0.3639 0.046 Uiso 1 1 calc R . . C103 C 0.2245(3) 0.3694(3) 0.4352(3) 0.0450(16) Uani 1 1 d . . . H10C H 0.2613 0.3913 0.4582 0.054 Uiso 1 1 calc R . . C104 C 0.1612(3) 0.3448(2) 0.4574(2) 0.0388(14) Uani 1 1 d . . . H10D H 0.1546 0.3494 0.4957 0.047 Uiso 1 1 calc R . . C105 C 0.1076(3) 0.3134(2) 0.4236(2) 0.0346(13) Uani 1 1 d . . . H10E H 0.0635 0.2972 0.4386 0.042 Uiso 1 1 calc R . . C106 C 0.1177(3) 0.3056(2) 0.3683(2) 0.0327(13) Uani 1 1 d . . . H10F H 0.0812 0.2836 0.3452 0.039 Uiso 1 1 calc R . . C201 C 0.4876(3) 0.9345(2) 0.1748(3) 0.0349(13) Uani 1 1 d . . . H20C H 0.4589 0.9167 0.1439 0.042 Uiso 1 1 calc R . . C202 C 0.5439(3) 0.9751(2) 0.1664(3) 0.0435(16) Uani 1 1 d . . . H20D H 0.5534 0.9853 0.1297 0.052 Uiso 1 1 calc R . . C203 C 0.5855(3) 1.0001(2) 0.2116(3) 0.0452(17) Uani 1 1 d . . . H20E H 0.6239 1.0276 0.2058 0.054 Uiso 1 1 calc R . . C204 C 0.5722(3) 0.9858(2) 0.2652(3) 0.0435(16) Uani 1 1 d . . . H20F H 0.6015 1.0032 0.2961 0.052 Uiso 1 1 calc R . . C205 C 0.5158(3) 0.9460(2) 0.2734(3) 0.0388(14) Uani 1 1 d . . . H20G H 0.5056 0.9362 0.3101 0.047 Uiso 1 1 calc R . . C206 C 0.4740(3) 0.9203(2) 0.2279(3) 0.0340(13) Uani 1 1 d . . . H20H H 0.4355 0.8928 0.2336 0.041 Uiso 1 1 calc R . . C301 C 0.0040(4) 0.5555(2) 0.5151(3) 0.0450(16) Uani 1 1 d . . . H30D H 0.0072 0.5935 0.5266 0.054 Uiso 1 1 calc R . . C302 C 0.0673(4) 0.5298(3) 0.4956(3) 0.0499(17) Uani 1 1 d . . . H30E H 0.1138 0.5506 0.4914 0.060 Uiso 1 1 calc R . . C303 C 0.0642(4) 0.4743(3) 0.4821(3) 0.058(2) Uani 1 1 d . . . H30F H 0.1095 0.4563 0.4706 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02133(9) 0.01368(8) 0.01881(9) 0.00186(7) -0.00299(7) 0.00026(7) O1 0.0312(18) 0.0196(17) 0.0158(17) 0.0020(14) -0.0081(14) -0.0039(14) O2 0.0282(18) 0.0155(16) 0.0195(17) -0.0010(13) 0.0026(14) 0.0038(13) O3 0.0256(18) 0.0205(17) 0.0269(19) 0.0013(14) 0.0051(15) -0.0033(14) N1 0.051(3) 0.020(2) 0.030(3) 0.0038(19) -0.013(2) 0.000(2) N2 0.023(2) 0.017(2) 0.029(2) 0.0060(17) 0.0013(18) 0.0056(16) N3 0.022(2) 0.031(2) 0.072(3) 0.005(2) -0.005(2) -0.0028(19) C1 0.064(4) 0.029(3) 0.038(4) 0.011(3) -0.002(3) 0.000(3) C2 0.052(4) 0.017(3) 0.038(3) 0.008(2) 0.007(3) 0.006(2) C3 0.022(3) 0.061(4) 0.035(3) -0.002(3) -0.001(2) 0.013(3) C4 0.027(3) 0.037(3) 0.085(5) -0.002(3) -0.002(3) -0.003(3) C5 0.030(3) 0.051(4) 0.041(3) -0.005(3) -0.012(3) 0.008(3) C6 0.047(4) 0.043(4) 0.045(4) -0.003(3) -0.012(3) 0.012(3) C7 0.064(4) 0.026(3) 0.017(3) 0.005(2) -0.003(3) -0.007(3) C8 0.033(3) 0.024(3) 0.021(3) 0.003(2) -0.007(2) -0.007(2) C9 0.022(2) 0.027(3) 0.016(2) 0.002(2) -0.0049(19) -0.007(2) C10 0.018(2) 0.024(3) 0.021(3) 0.002(2) -0.0034(19) -0.0051(19) C11 0.021(2) 0.033(3) 0.025(3) -0.003(2) 0.001(2) -0.009(2) C12 0.024(3) 0.039(3) 0.023(3) 0.002(2) -0.002(2) -0.009(2) C13 0.033(3) 0.028(3) 0.025(3) 0.008(2) -0.007(2) -0.009(2) C14 0.027(3) 0.018(2) 0.024(3) 0.000(2) 0.002(2) -0.003(2) C15 0.031(3) 0.031(3) 0.025(3) -0.006(2) 0.005(2) -0.016(2) C16 0.037(3) 0.045(3) 0.028(3) -0.003(3) 0.000(2) -0.022(3) C17 0.053(4) 0.031(3) 0.026(3) -0.005(2) 0.006(3) -0.018(3) C18 0.028(3) 0.044(4) 0.047(4) 0.000(3) 0.006(3) -0.014(3) C19 0.035(3) 0.043(3) 0.027(3) 0.005(3) 0.002(2) -0.014(3) C20 0.026(3) 0.012(2) 0.035(3) -0.001(2) 0.007(2) 0.0009(19) C21 0.016(2) 0.017(2) 0.027(3) -0.001(2) 0.0035(19) 0.0008(18) C22 0.014(2) 0.017(2) 0.026(3) -0.0040(19) 0.0005(19) 0.0001(18) C23 0.014(2) 0.015(2) 0.024(2) -0.0025(19) 0.0023(18) -0.0006(17) C24 0.017(2) 0.028(3) 0.021(3) -0.002(2) -0.0009(19) 0.000(2) C25 0.016(2) 0.023(2) 0.025(3) -0.009(2) 0.0000(19) 0.0024(19) C26 0.016(2) 0.015(2) 0.036(3) -0.007(2) 0.001(2) 0.0005(18) C27 0.024(2) 0.017(2) 0.020(2) -0.0023(19) 0.0044(19) 0.0028(19) C28 0.022(2) 0.020(2) 0.023(3) -0.0009(19) 0.002(2) 0.0047(19) C29 0.030(3) 0.030(3) 0.042(3) 0.006(3) 0.015(2) 0.008(2) C30 0.036(3) 0.019(2) 0.030(3) 0.001(2) 0.002(2) 0.006(2) C31 0.030(3) 0.025(3) 0.037(3) -0.003(2) -0.009(2) 0.006(2) C32 0.024(3) 0.024(3) 0.036(3) -0.007(2) -0.001(2) 0.005(2) C33 0.020(3) 0.030(3) 0.073(5) 0.000(3) -0.008(3) -0.005(2) C34 0.027(3) 0.020(3) 0.073(4) -0.016(3) 0.011(3) -0.007(2) C35 0.027(3) 0.016(2) 0.040(3) -0.011(2) 0.009(2) -0.007(2) C36 0.040(3) 0.027(3) 0.030(3) -0.014(2) 0.012(2) -0.016(2) C37 0.052(4) 0.060(4) 0.042(4) -0.030(3) 0.029(3) -0.037(3) C38 0.042(4) 0.065(5) 0.090(6) -0.056(5) 0.041(4) -0.031(4) C39 0.034(3) 0.038(4) 0.097(6) -0.034(4) 0.021(4) -0.009(3) C40 0.052(4) 0.031(3) 0.013(2) 0.001(2) 0.003(2) -0.020(3) C41 0.055(4) 0.025(3) 0.017(3) -0.002(2) 0.001(2) -0.018(3) C42 0.056(4) 0.026(3) 0.023(3) -0.004(2) 0.001(3) -0.007(3) C43 0.080(5) 0.033(3) 0.037(4) 0.007(3) -0.021(3) -0.010(3) C44 0.097(6) 0.039(4) 0.045(4) -0.008(3) 0.024(4) -0.043(4) C45 0.073(5) 0.098(7) 0.123(7) -0.060(6) 0.063(5) -0.036(5) U2 0.01790(8) 0.01305(8) 0.01701(9) 0.00108(7) 0.00050(6) -0.00290(7) O4 0.0188(16) 0.0167(16) 0.0201(17) 0.0019(13) -0.0011(13) 0.0004(13) O5 0.035(2) 0.0191(17) 0.0152(17) 0.0017(13) 0.0025(14) -0.0052(15) O6 0.0208(17) 0.0152(16) 0.034(2) -0.0012(14) 0.0036(15) -0.0029(13) O7 0.0154(15) 0.0232(17) 0.0180(16) 0.0030(13) -0.0018(13) -0.0016(13) O8 0.0192(17) 0.0222(17) 0.0302(19) 0.0039(15) 0.0073(14) 0.0035(14) O9 0.0190(17) 0.0220(17) 0.0223(18) -0.0046(14) 0.0006(14) 0.0012(14) N4 0.023(2) 0.0160(19) 0.019(2) 0.0011(16) -0.0024(16) -0.0026(16) N5 0.023(2) 0.016(2) 0.018(2) 0.0004(16) -0.0009(16) -0.0049(16) N6 0.020(2) 0.0121(18) 0.022(2) 0.0005(15) 0.0019(16) -0.0016(15) C46 0.021(2) 0.016(2) 0.023(3) 0.0030(19) -0.0019(19) -0.0080(19) C47 0.030(3) 0.020(2) 0.021(3) -0.001(2) -0.001(2) -0.012(2) C48 0.027(3) 0.021(2) 0.016(2) -0.0018(19) 0.001(2) -0.007(2) C49 0.030(3) 0.016(2) 0.022(3) -0.0036(19) 0.006(2) -0.005(2) C50 0.021(2) 0.014(2) 0.019(2) 0.0023(18) 0.0032(19) 0.0029(18) C51 0.026(2) 0.015(2) 0.021(2) 0.0002(19) 0.005(2) -0.0047(19) C52 0.018(2) 0.019(2) 0.025(3) 0.002(2) 0.0069(19) -0.0037(19) C53 0.021(2) 0.018(2) 0.020(2) 0.0012(19) 0.0046(19) 0.0029(19) C54 0.019(2) 0.016(2) 0.016(2) 0.0000(18) 0.0059(18) 0.0043(18) C55 0.022(2) 0.019(2) 0.020(2) -0.0031(19) 0.0046(19) 0.0058(19) C56 0.030(3) 0.026(3) 0.017(2) -0.004(2) 0.002(2) 0.011(2) C57 0.030(3) 0.023(3) 0.022(3) 0.008(2) 0.011(2) 0.008(2) C58 0.027(3) 0.017(2) 0.023(3) 0.0012(19) 0.013(2) 0.0017(19) C59 0.023(2) 0.021(2) 0.021(2) -0.004(2) -0.001(2) 0.005(2) C60 0.032(3) 0.034(3) 0.038(3) -0.017(3) -0.006(2) 0.004(2) C61 0.075(5) 0.057(4) 0.031(3) -0.030(3) -0.003(3) 0.018(4) C62 0.046(4) 0.033(3) 0.082(5) -0.029(3) -0.025(4) 0.006(3) C63 0.038(3) 0.022(3) 0.068(4) -0.014(3) -0.006(3) 0.007(2) C64 0.042(3) 0.032(3) 0.023(3) 0.011(2) 0.009(2) 0.010(2) C65 0.022(2) 0.025(2) 0.016(2) 0.002(2) -0.0032(19) -0.005(2) C66 0.020(2) 0.023(2) 0.024(3) 0.005(2) -0.0002(19) -0.003(2) C67 0.024(2) 0.019(2) 0.021(2) 0.0013(19) 0.002(2) 0.0000(19) C68 0.020(2) 0.019(2) 0.027(3) 0.004(2) 0.001(2) -0.0004(19) C69 0.024(3) 0.024(3) 0.026(3) 0.011(2) 0.001(2) -0.001(2) C70 0.023(3) 0.033(3) 0.022(3) 0.008(2) 0.000(2) 0.004(2) C71 0.022(2) 0.026(3) 0.022(3) 0.001(2) -0.007(2) -0.002(2) C72 0.030(3) 0.022(3) 0.028(3) 0.008(2) 0.001(2) -0.006(2) C73 0.039(3) 0.019(2) 0.033(3) -0.001(2) 0.003(2) -0.010(2) C74 0.048(4) 0.024(3) 0.045(4) 0.000(3) -0.002(3) 0.005(3) C75 0.059(4) 0.028(3) 0.037(3) 0.001(3) 0.005(3) -0.019(3) C76 0.052(4) 0.024(3) 0.060(4) -0.009(3) 0.023(3) -0.006(3) C77 0.043(3) 0.038(3) 0.019(3) 0.010(2) -0.001(2) -0.002(3) C78 0.017(2) 0.017(2) 0.021(2) -0.0020(19) 0.0013(19) 0.0010(18) C79 0.018(2) 0.016(2) 0.025(3) 0.0018(19) -0.0006(19) -0.0021(18) C80 0.018(2) 0.020(2) 0.024(3) 0.000(2) -0.0032(19) -0.0064(19) C81 0.018(2) 0.020(2) 0.031(3) 0.007(2) -0.005(2) -0.0045(19) C82 0.021(2) 0.022(3) 0.031(3) 0.008(2) -0.001(2) -0.006(2) C83 0.016(2) 0.041(3) 0.022(3) 0.009(2) 0.000(2) -0.006(2) C84 0.023(2) 0.024(3) 0.022(3) -0.002(2) -0.001(2) -0.004(2) C85 0.019(2) 0.017(2) 0.042(3) 0.006(2) 0.000(2) -0.0012(19) C86 0.022(3) 0.014(2) 0.050(3) -0.004(2) -0.006(2) 0.0015(19) C87 0.080(5) 0.026(3) 0.068(5) 0.010(3) -0.038(4) -0.011(3) C88 0.024(3) 0.068(5) 0.107(6) -0.055(5) 0.005(4) -0.005(3) C89 0.047(4) 0.026(3) 0.046(4) -0.001(3) 0.014(3) 0.005(3) C90 0.024(3) 0.046(3) 0.026(3) 0.005(2) 0.001(2) -0.012(2) C91 0.020(2) 0.025(3) 0.013(2) 0.0030(19) 0.0039(18) 0.003(2) C101 0.040(3) 0.034(3) 0.029(3) 0.000(2) 0.007(2) 0.013(3) C102 0.032(3) 0.035(3) 0.052(4) 0.001(3) 0.017(3) 0.000(2) C103 0.034(3) 0.041(4) 0.060(4) -0.024(3) 0.007(3) -0.006(3) C104 0.042(3) 0.043(3) 0.034(3) -0.009(3) 0.014(3) 0.004(3) C105 0.031(3) 0.029(3) 0.046(4) -0.002(3) 0.011(3) -0.002(2) C106 0.029(3) 0.023(3) 0.044(3) -0.005(2) -0.004(2) 0.005(2) C201 0.029(3) 0.026(3) 0.050(4) -0.012(3) 0.010(3) -0.004(2) C202 0.041(3) 0.029(3) 0.065(4) -0.014(3) 0.028(3) -0.004(3) C203 0.030(3) 0.034(3) 0.075(5) -0.024(3) 0.024(3) -0.012(3) C204 0.026(3) 0.036(3) 0.068(5) -0.023(3) -0.001(3) -0.001(2) C205 0.038(3) 0.026(3) 0.051(4) -0.003(3) -0.003(3) 0.002(2) C206 0.028(3) 0.017(2) 0.057(4) -0.008(3) 0.006(3) -0.005(2) C301 0.054(4) 0.026(3) 0.056(4) -0.003(3) 0.007(3) -0.002(3) C302 0.035(3) 0.034(3) 0.080(5) -0.001(3) 0.008(3) -0.005(3) C303 0.045(4) 0.036(4) 0.097(6) 0.006(4) 0.031(4) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 2.149(3) . ? U1 O1 2.190(3) . ? U1 O3 2.239(3) . ? U1 O8 2.430(3) . ? U1 O7 2.616(3) . ? U1 N3 2.669(4) . ? U1 N1 2.704(4) . ? U1 N2 2.748(4) . ? U1 C91 2.926(5) . ? O1 C9 1.340(5) . ? O2 C22 1.351(5) . ? O3 C35 1.342(6) . ? N1 C6 1.452(7) . ? N1 C7 1.483(7) . ? N1 C1 1.496(7) . ? N2 C2 1.490(6) . ? N2 C20 1.493(6) . ? N2 C3 1.500(6) . ? N3 C4 1.443(8) . ? N3 C33 1.511(7) . ? N3 C5 1.547(8) . ? C1 C2 1.469(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.548(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.441(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.490(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.379(7) . ? C8 C9 1.415(7) . ? C9 C10 1.407(7) . ? C10 C11 1.395(7) . ? C10 C14 1.510(6) . ? C11 C12 1.388(7) . ? C11 H11A 0.9500 . ? C12 C13 1.388(7) . ? C12 C19 1.511(7) . ? C13 H13A 0.9500 . ? C14 C15 1.544(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.519(8) . ? C15 C16 1.520(7) . ? C15 C17 1.529(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.502(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.394(6) . ? C21 C22 1.401(6) . ? C22 C23 1.399(6) . ? C23 C24 1.396(6) . ? C23 C27 1.502(6) . ? C24 C25 1.396(7) . ? C24 H24A 0.9500 . ? C25 C26 1.381(7) . ? C25 C32 1.506(6) . ? C26 H26A 0.9500 . ? C27 C28 1.540(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C30 1.527(6) . ? C28 C31 1.530(7) . ? C28 C29 1.531(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.510(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.368(8) . ? C34 C35 1.405(8) . ? C35 C36 1.409(8) . ? C36 C37 1.414(7) . ? C36 C40 1.502(8) . ? C37 C38 1.393(11) . ? C37 H37A 0.9500 . ? C38 C39 1.376(11) . ? C38 C45 1.517(9) . ? C39 H39A 0.9500 . ? C40 C41 1.557(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C43 1.510(9) . ? C41 C44 1.527(8) . ? C41 C42 1.528(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? U2 O4 2.158(3) . ? U2 O5 2.171(3) . ? U2 O6 2.213(3) . ? U2 O9 2.375(3) . ? U2 O7 2.663(3) . ? U2 N6 2.717(4) . ? U2 N4 2.722(4) . ? U2 N5 2.776(4) . ? U2 C91 2.898(4) . ? O4 C54 1.350(5) . ? O5 C67 1.351(5) . ? O6 C80 1.346(5) . ? O7 C91 1.274(5) . ? O8 C91 1.274(5) . ? O9 C91 1.277(5) . ? N4 C46 1.483(6) . ? N4 C52 1.486(6) . ? N4 C51 1.503(6) . ? N5 C48 1.482(6) . ? N5 C47 1.485(6) . ? N5 C65 1.501(6) . ? N6 C49 1.488(6) . ? N6 C50 1.492(5) . ? N6 C78 1.501(6) . ? C46 C47 1.519(6) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.513(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.516(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.488(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C58 1.387(6) . ? C53 C54 1.404(6) . ? C54 C55 1.391(6) . ? C55 C56 1.401(7) . ? C55 C59 1.512(6) . ? C56 C57 1.382(7) . ? C56 H56A 0.9500 . ? C57 C58 1.391(7) . ? C57 C64 1.511(6) . ? C58 H58A 0.9500 . ? C59 C60 1.540(7) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.522(8) . ? C60 C63 1.526(8) . ? C60 C62 1.535(8) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.501(6) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.390(7) . ? C66 C71 1.391(7) . ? C67 C68 1.418(6) . ? C68 C69 1.383(7) . ? C68 C72 1.508(7) . ? C69 C70 1.392(7) . ? C69 H69A 0.9500 . ? C70 C71 1.392(7) . ? C70 C77 1.505(7) . ? C71 H71A 0.9500 . ? C72 C73 1.537(7) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C76 1.518(7) . ? C73 C75 1.524(7) . ? C73 C74 1.540(7) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.503(6) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C84 1.383(6) . ? C79 C80 1.400(6) . ? C80 C81 1.411(6) . ? C81 C82 1.395(7) . ? C81 C85 1.506(7) . ? C82 C83 1.387(7) . ? C82 H82A 0.9500 . ? C83 C84 1.400(7) . ? C83 C90 1.506(7) . ? C84 H84A 0.9500 . ? C85 C86 1.547(7) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C88 1.513(8) . ? C86 C87 1.515(8) . ? C86 C89 1.520(7) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C101 C102 1.365(8) . ? C101 C106 1.378(8) . ? C101 H10A 0.9500 . ? C102 C103 1.385(8) . ? C102 H10B 0.9500 . ? C103 C104 1.385(8) . ? C103 H10C 0.9500 . ? C104 C105 1.380(8) . ? C104 H10D 0.9500 . ? C105 C106 1.379(8) . ? C105 H10E 0.9500 . ? C106 H10F 0.9500 . ? C201 C206 1.369(8) . ? C201 C202 1.394(7) . ? C201 H20C 0.9500 . ? C202 C203 1.375(9) . ? C202 H20D 0.9500 . ? C203 C204 1.381(9) . ? C203 H20E 0.9500 . ? C204 C205 1.382(8) . ? C204 H20F 0.9500 . ? C205 C206 1.390(8) . ? C205 H20G 0.9500 . ? C206 H20H 0.9500 . ? C301 C302 1.368(8) . ? C301 C303 1.371(9) 3_566 ? C301 H30D 0.9500 . ? C302 C303 1.367(8) . ? C302 H30E 0.9500 . ? C303 C301 1.371(9) 3_566 ? C303 H30F 0.9500 . ? 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 155.57(11) . . ? O2 U1 O3 81.53(12) . . ? O1 U1 O3 79.25(12) . . ? O2 U1 O8 78.52(12) . . ? O1 U1 O8 112.33(11) . . ? O3 U1 O8 150.18(12) . . ? O2 U1 O7 97.35(11) . . ? O1 U1 O7 75.83(11) . . ? O3 U1 O7 110.89(11) . . ? O8 U1 O7 50.94(10) . . ? O2 U1 N3 105.59(15) . . ? O1 U1 N3 84.20(14) . . ? O3 U1 N3 75.93(13) . . ? O8 U1 N3 130.88(12) . . ? O7 U1 N3 156.88(14) . . ? O2 U1 N1 133.87(12) . . ? O1 U1 N1 70.55(13) . . ? O3 U1 N1 132.02(13) . . ? O8 U1 N1 77.30(13) . . ? O7 U1 N1 97.02(13) . . ? N3 U1 N1 64.91(15) . . ? O2 U1 N2 69.82(12) . . ? O1 U1 N2 133.86(12) . . ? O3 U1 N2 122.26(12) . . ? O8 U1 N2 70.51(11) . . ? O7 U1 N2 121.42(11) . . ? N3 U1 N2 65.85(13) . . ? N1 U1 N2 65.27(13) . . ? O2 U1 C91 85.05(12) . . ? O1 U1 C91 96.37(12) . . ? O3 U1 C91 131.13(12) . . ? O8 U1 C91 25.42(12) . . ? O7 U1 C91 25.81(11) . . ? N3 U1 C91 152.69(14) . . ? N1 U1 C91 89.42(14) . . ? N2 U1 C91 95.85(12) . . ? C9 O1 U1 148.6(3) . . ? C22 O2 U1 153.2(3) . . ? C35 O3 U1 127.6(3) . . ? C6 N1 C7 110.9(5) . . ? C6 N1 C1 111.3(5) . . ? C7 N1 C1 105.9(4) . . ? C6 N1 U1 116.2(4) . . ? C7 N1 U1 106.0(3) . . ? C1 N1 U1 105.9(3) . . ? C2 N2 C20 108.1(4) . . ? C2 N2 C3 110.8(4) . . ? C20 N2 C3 110.2(4) . . ? C2 N2 U1 112.7(3) . . ? C20 N2 U1 112.0(3) . . ? C3 N2 U1 103.0(3) . . ? C4 N3 C33 108.6(5) . . ? C4 N3 C5 110.0(5) . . ? C33 N3 C5 107.2(5) . . ? C4 N3 U1 116.6(4) . . ? C33 N3 U1 110.0(3) . . ? C5 N3 U1 104.1(3) . . ? C2 C1 N1 112.9(5) . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? N1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C1 C2 N2 115.2(4) . . ? C1 C2 H2A 108.5 . . ? N2 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? N2 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N2 C3 C4 113.2(5) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? N3 C4 C3 113.6(5) . . ? N3 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? N3 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 N3 115.3(5) . . ? C6 C5 H5A 108.4 . . ? N3 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? N3 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C5 C6 N1 112.7(5) . . ? C5 C6 H6A 109.0 . . ? N1 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? N1 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N1 C7 C8 115.7(5) . . ? N1 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C13 C8 C9 119.3(5) . . ? C13 C8 C7 119.6(5) . . ? C9 C8 C7 120.6(4) . . ? O1 C9 C10 121.3(4) . . ? O1 C9 C8 118.6(4) . . ? C10 C9 C8 120.0(4) . . ? C11 C10 C9 117.6(4) . . ? C11 C10 C14 120.6(4) . . ? C9 C10 C14 121.7(4) . . ? C12 C11 C10 123.6(5) . . ? C12 C11 H11A 118.2 . . ? C10 C11 H11A 118.2 . . ? C11 C12 C13 117.1(5) . . ? C11 C12 C19 121.7(5) . . ? C13 C12 C19 121.2(5) . . ? C8 C13 C12 122.3(5) . . ? C8 C13 H13A 118.8 . . ? C12 C13 H13A 118.8 . . ? C10 C14 C15 117.6(4) . . ? C10 C14 H14A 107.9 . . ? C15 C14 H14A 107.9 . . ? C10 C14 H14B 107.9 . . ? C15 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C18 C15 C16 110.0(5) . . ? C18 C15 C17 109.8(4) . . ? C16 C15 C17 109.1(4) . . ? C18 C15 C14 108.7(4) . . ? C16 C15 C14 111.9(4) . . ? C17 C15 C14 107.3(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C21 117.2(4) . . ? N2 C20 H20A 108.0 . . ? C21 C20 H20A 108.0 . . ? N2 C20 H20B 108.0 . . ? C21 C20 H20B 108.0 . . ? H20A C20 H20B 107.2 . . ? C26 C21 C22 119.1(4) . . ? C26 C21 C20 119.8(4) . . ? C22 C21 C20 121.0(4) . . ? O2 C22 C23 121.1(4) . . ? O2 C22 C21 118.7(4) . . ? C23 C22 C21 120.1(4) . . ? C24 C23 C22 118.2(4) . . ? C24 C23 C27 120.1(4) . . ? C22 C23 C27 121.7(4) . . ? C25 C24 C23 122.9(4) . . ? C25 C24 H24A 118.5 . . ? C23 C24 H24A 118.5 . . ? C26 C25 C24 117.0(4) . . ? C26 C25 C32 122.2(4) . . ? C24 C25 C32 120.7(4) . . ? C25 C26 C21 122.4(4) . . ? C25 C26 H26A 118.8 . . ? C21 C26 H26A 118.8 . . ? C23 C27 C28 115.7(4) . . ? C23 C27 H27A 108.4 . . ? C28 C27 H27A 108.4 . . ? C23 C27 H27B 108.4 . . ? C28 C27 H27B 108.4 . . ? H27A C27 H27B 107.4 . . ? C30 C28 C31 108.7(4) . . ? C30 C28 C29 108.3(4) . . ? C31 C28 C29 109.6(4) . . ? C30 C28 C27 108.4(4) . . ? C31 C28 C27 111.5(4) . . ? C29 C28 C27 110.3(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C32 H32A 109.5 . . ? C25 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C25 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N3 116.3(5) . . ? C34 C33 H33A 108.2 . . ? N3 C33 H33A 108.2 . . ? C34 C33 H33B 108.2 . . ? N3 C33 H33B 108.2 . . ? H33A C33 H33B 107.4 . . ? C39 C34 C35 120.8(7) . . ? C39 C34 C33 122.2(6) . . ? C35 C34 C33 116.2(5) . . ? O3 C35 C34 118.9(5) . . ? O3 C35 C36 122.2(5) . . ? C34 C35 C36 118.9(5) . . ? C35 C36 C37 117.6(6) . . ? C35 C36 C40 121.1(5) . . ? C37 C36 C40 121.2(6) . . ? C38 C37 C36 122.5(7) . . ? C38 C37 H37A 118.7 . . ? C36 C37 H37A 118.7 . . ? C39 C38 C37 117.6(6) . . ? C39 C38 C45 123.0(8) . . ? C37 C38 C45 119.4(8) . . ? C34 C39 C38 122.0(7) . . ? C34 C39 H39A 119.0 . . ? C38 C39 H39A 119.0 . . ? C36 C40 C41 116.6(4) . . ? C36 C40 H40A 108.1 . . ? C41 C40 H40A 108.1 . . ? C36 C40 H40B 108.1 . . ? C41 C40 H40B 108.1 . . ? H40A C40 H40B 107.3 . . ? C43 C41 C44 109.6(5) . . ? C43 C41 C42 109.2(5) . . ? C44 C41 C42 110.0(5) . . ? C43 C41 C40 107.5(5) . . ? C44 C41 C40 110.8(5) . . ? C42 C41 C40 109.7(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C38 C45 H45A 109.5 . . ? C38 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C38 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O4 U2 O5 161.15(12) . . ? O4 U2 O6 84.52(12) . . ? O5 U2 O6 84.46(12) . . ? O4 U2 O9 86.18(11) . . ? O5 U2 O9 79.13(12) . . ? O6 U2 O9 92.80(11) . . ? O4 U2 O7 91.31(10) . . ? O5 U2 O7 88.67(11) . . ? O6 U2 O7 144.03(11) . . ? O9 U2 O7 51.25(10) . . ? O4 U2 N6 82.20(11) . . ? O5 U2 N6 109.64(12) . . ? O6 U2 N6 75.39(11) . . ? O9 U2 N6 164.12(11) . . ? O7 U2 N6 139.47(10) . . ? O4 U2 N4 68.36(11) . . ? O5 U2 N4 129.45(12) . . ? O6 U2 N4 134.73(11) . . ? O9 U2 N4 119.46(11) . . ? O7 U2 N4 74.56(11) . . ? N6 U2 N4 65.83(11) . . ? O4 U2 N5 130.10(11) . . ? O5 U2 N5 68.75(11) . . ? O6 U2 N5 118.75(12) . . ? O9 U2 N5 130.96(11) . . ? O7 U2 N5 90.97(10) . . ? N6 U2 N5 64.85(11) . . ? N4 U2 N5 64.37(11) . . ? O4 U2 C91 92.13(12) . . ? O5 U2 C91 79.72(12) . . ? O6 U2 C91 118.22(13) . . ? O9 U2 C91 25.65(12) . . ? O7 U2 C91 26.05(11) . . ? N6 U2 C91 164.85(12) . . ? N4 U2 C91 99.02(12) . . ? N5 U2 C91 109.87(12) . . ? C54 O4 U2 151.2(3) . . ? C67 O5 U2 154.0(3) . . ? C80 O6 U2 128.2(3) . . ? C91 O7 U1 90.8(3) . . ? C91 O7 U2 87.3(2) . . ? U1 O7 U2 175.77(13) . . ? C91 O8 U1 99.6(3) . . ? C91 O9 U2 100.7(3) . . ? C46 N4 C52 107.2(3) . . ? C46 N4 C51 109.6(4) . . ? C52 N4 C51 111.2(3) . . ? C46 N4 U2 106.0(3) . . ? C52 N4 U2 108.1(3) . . ? C51 N4 U2 114.3(3) . . ? C48 N5 C47 112.3(4) . . ? C48 N5 C65 110.6(3) . . ? C47 N5 C65 105.5(4) . . ? C48 N5 U2 101.9(3) . . ? C47 N5 U2 114.5(3) . . ? C65 N5 U2 112.2(3) . . ? C49 N6 C50 111.3(3) . . ? C49 N6 C78 109.4(3) . . ? C50 N6 C78 106.3(3) . . ? C49 N6 U2 114.6(3) . . ? C50 N6 U2 105.8(2) . . ? C78 N6 U2 109.1(2) . . ? N4 C46 C47 112.1(4) . . ? N4 C46 H46A 109.2 . . ? C47 C46 H46A 109.2 . . ? N4 C46 H46B 109.2 . . ? C47 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? N5 C47 C46 111.7(4) . . ? N5 C47 H47A 109.3 . . ? C46 C47 H47A 109.3 . . ? N5 C47 H47B 109.3 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? N5 C48 C49 113.5(4) . . ? N5 C48 H48A 108.9 . . ? C49 C48 H48A 108.9 . . ? N5 C48 H48B 108.9 . . ? C49 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? N6 C49 C48 113.3(4) . . ? N6 C49 H49A 108.9 . . ? C48 C49 H49A 108.9 . . ? N6 C49 H49B 108.9 . . ? C48 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? N6 C50 C51 114.2(4) . . ? N6 C50 H50A 108.7 . . ? C51 C50 H50A 108.7 . . ? N6 C50 H50B 108.7 . . ? C51 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? N4 C51 C50 114.0(4) . . ? N4 C51 H51A 108.8 . . ? C50 C51 H51A 108.8 . . ? N4 C51 H51B 108.8 . . ? C50 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? N4 C52 C53 113.6(4) . . ? N4 C52 H52A 108.8 . . ? C53 C52 H52A 108.8 . . ? N4 C52 H52B 108.8 . . ? C53 C52 H52B 108.8 . . ? H52A C52 H52B 107.7 . . ? C58 C53 C54 119.0(4) . . ? C58 C53 C52 120.3(4) . . ? C54 C53 C52 120.7(4) . . ? O4 C54 C55 121.1(4) . . ? O4 C54 C53 118.0(4) . . ? C55 C54 C53 120.8(4) . . ? C54 C55 C56 117.6(4) . . ? C54 C55 C59 122.2(4) . . ? C56 C55 C59 120.1(4) . . ? C57 C56 C55 123.2(5) . . ? C57 C56 H56A 118.4 . . ? C55 C56 H56A 118.4 . . ? C56 C57 C58 117.4(4) . . ? C56 C57 C64 122.3(5) . . ? C58 C57 C64 120.3(5) . . ? C53 C58 C57 121.9(5) . . ? C53 C58 H58A 119.1 . . ? C57 C58 H58A 119.1 . . ? C55 C59 C60 117.2(4) . . ? C55 C59 H59A 108.0 . . ? C60 C59 H59A 108.0 . . ? C55 C59 H59B 108.0 . . ? C60 C59 H59B 108.0 . . ? H59A C59 H59B 107.2 . . ? C61 C60 C63 110.0(5) . . ? C61 C60 C62 109.4(5) . . ? C63 C60 C62 109.5(5) . . ? C61 C60 C59 111.1(5) . . ? C63 C60 C59 110.5(4) . . ? C62 C60 C59 106.3(4) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C57 C64 H64A 109.5 . . ? C57 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C57 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 N5 117.6(4) . . ? C66 C65 H65A 107.9 . . ? N5 C65 H65A 107.9 . . ? C66 C65 H65B 107.9 . . ? N5 C65 H65B 107.9 . . ? H65A C65 H65B 107.2 . . ? C67 C66 C71 120.5(4) . . ? C67 C66 C65 119.5(4) . . ? C71 C66 C65 119.7(4) . . ? O5 C67 C66 118.6(4) . . ? O5 C67 C68 122.4(4) . . ? C66 C67 C68 119.0(4) . . ? C69 C68 C67 118.5(4) . . ? C69 C68 C72 121.2(4) . . ? C67 C68 C72 120.3(4) . . ? C68 C69 C70 123.5(5) . . ? C68 C69 H69A 118.3 . . ? C70 C69 H69A 118.3 . . ? C71 C70 C69 116.8(4) . . ? C71 C70 C77 121.8(5) . . ? C69 C70 C77 121.3(5) . . ? C66 C71 C70 121.7(5) . . ? C66 C71 H71A 119.2 . . ? C70 C71 H71A 119.2 . . ? C68 C72 C73 115.5(4) . . ? C68 C72 H72A 108.4 . . ? C73 C72 H72A 108.4 . . ? C68 C72 H72B 108.4 . . ? C73 C72 H72B 108.4 . . ? H72A C72 H72B 107.5 . . ? C76 C73 C75 108.8(5) . . ? C76 C73 C72 110.1(4) . . ? C75 C73 C72 107.8(5) . . ? C76 C73 C74 109.2(5) . . ? C75 C73 C74 108.9(4) . . ? C72 C73 C74 112.0(4) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C70 C77 H77A 109.5 . . ? C70 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C70 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N6 C78 C79 114.2(4) . . ? N6 C78 H78A 108.7 . . ? C79 C78 H78A 108.7 . . ? N6 C78 H78B 108.7 . . ? C79 C78 H78B 108.7 . . ? H78A C78 H78B 107.6 . . ? C84 C79 C80 120.3(4) . . ? C84 C79 C78 122.2(4) . . ? C80 C79 C78 117.3(4) . . ? O6 C80 C79 118.9(4) . . ? O6 C80 C81 121.6(4) . . ? C79 C80 C81 119.5(4) . . ? C82 C81 C80 117.6(5) . . ? C82 C81 C85 120.7(4) . . ? C80 C81 C85 121.6(4) . . ? C83 C82 C81 123.3(4) . . ? C83 C82 H82A 118.3 . . ? C81 C82 H82A 118.3 . . ? C82 C83 C84 117.3(4) . . ? C82 C83 C90 121.5(5) . . ? C84 C83 C90 121.2(5) . . ? C79 C84 C83 121.2(5) . . ? C79 C84 H84A 119.4 . . ? C83 C84 H84A 119.4 . . ? C81 C85 C86 115.6(4) . . ? C81 C85 H85A 108.4 . . ? C86 C85 H85A 108.4 . . ? C81 C85 H85B 108.4 . . ? C86 C85 H85B 108.4 . . ? H85A C85 H85B 107.4 . . ? C88 C86 C87 110.1(6) . . ? C88 C86 C89 107.8(5) . . ? C87 C86 C89 109.3(5) . . ? C88 C86 C85 111.4(5) . . ? C87 C86 C85 110.6(4) . . ? C89 C86 C85 107.5(4) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C86 C89 H89A 109.5 . . ? C86 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C86 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C83 C90 H90A 109.5 . . ? C83 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C83 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? O8 C91 O7 117.4(4) . . ? O8 C91 O9 124.0(4) . . ? O7 C91 O9 118.6(4) . . ? O8 C91 U2 166.1(3) . . ? O7 C91 U2 66.6(2) . . ? O9 C91 U2 53.6(2) . . ? O8 C91 U1 55.0(2) . . ? O7 C91 U1 63.4(2) . . ? O9 C91 U1 171.1(3) . . ? U2 C91 U1 129.89(17) . . ? C102 C101 C106 120.9(5) . . ? C102 C101 H10A 119.6 . . ? C106 C101 H10A 119.6 . . ? C101 C102 C103 120.1(5) . . ? C101 C102 H10B 120.0 . . ? C103 C102 H10B 120.0 . . ? C102 C103 C104 119.6(6) . . ? C102 C103 H10C 120.2 . . ? C104 C103 H10C 120.2 . . ? C105 C104 C103 119.8(5) . . ? C105 C104 H10D 120.1 . . ? C103 C104 H10D 120.1 . . ? C106 C105 C104 120.3(5) . . ? C106 C105 H10E 119.8 . . ? C104 C105 H10E 119.8 . . ? C101 C106 C105 119.4(5) . . ? C101 C106 H10F 120.3 . . ? C105 C106 H10F 120.3 . . ? C206 C201 C202 119.7(6) . . ? C206 C201 H20C 120.1 . . ? C202 C201 H20C 120.1 . . ? C203 C202 C201 119.5(6) . . ? C203 C202 H20D 120.3 . . ? C201 C202 H20D 120.3 . . ? C202 C203 C204 121.1(5) . . ? C202 C203 H20E 119.5 . . ? C204 C203 H20E 119.5 . . ? C203 C204 C205 119.3(6) . . ? C203 C204 H20F 120.4 . . ? C205 C204 H20F 120.4 . . ? C204 C205 C206 119.9(6) . . ? C204 C205 H20G 120.1 . . ? C206 C205 H20G 120.1 . . ? C201 C206 C205 120.6(5) . . ? C201 C206 H20H 119.7 . . ? C205 C206 H20H 119.7 . . ? C302 C301 C303 119.1(6) . 3_566 ? C302 C301 H30D 120.5 . . ? C303 C301 H30D 120.5 3_566 . ? C303 C302 C301 120.4(6) . . ? C303 C302 H30E 119.8 . . ? C301 C302 H30E 119.8 . . ? C302 C303 C301 120.4(6) . 3_566 ? C302 C303 H30F 119.8 . . ? C301 C303 H30F 119.8 3_566 . ? 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 O1 C9 -160.2(5) . . . . ? O3 U1 O1 C9 161.1(6) . . . . ? O8 U1 O1 C9 -47.6(6) . . . . ? O7 U1 O1 C9 -83.9(6) . . . . ? N3 U1 O1 C9 84.4(6) . . . . ? N1 U1 O1 C9 19.0(5) . . . . ? N2 U1 O1 C9 36.3(6) . . . . ? C91 U1 O1 C9 -68.1(6) . . . . ? O1 U1 O2 C22 -169.6(5) . . . . ? O3 U1 O2 C22 -131.2(6) . . . . ? O8 U1 O2 C22 71.0(6) . . . . ? O7 U1 O2 C22 118.6(6) . . . . ? N3 U1 O2 C22 -58.5(7) . . . . ? N1 U1 O2 C22 11.5(7) . . . . ? N2 U1 O2 C22 -2.2(6) . . . . ? C91 U1 O2 C22 95.9(6) . . . . ? O2 U1 O3 C35 54.9(4) . . . . ? O1 U1 O3 C35 -140.2(4) . . . . ? O8 U1 O3 C35 103.3(4) . . . . ? O7 U1 O3 C35 149.6(4) . . . . ? N3 U1 O3 C35 -53.6(4) . . . . ? N1 U1 O3 C35 -89.1(4) . . . . ? N2 U1 O3 C35 -4.6(4) . . . . ? C91 U1 O3 C35 130.7(4) . . . . ? O2 U1 N1 C6 -103.8(4) . . . . ? O1 U1 N1 C6 76.7(4) . . . . ? O3 U1 N1 C6 22.5(5) . . . . ? O8 U1 N1 C6 -163.8(4) . . . . ? O7 U1 N1 C6 149.0(4) . . . . ? N3 U1 N1 C6 -16.0(4) . . . . ? N2 U1 N1 C6 -89.6(4) . . . . ? C91 U1 N1 C6 173.7(4) . . . . ? O2 U1 N1 C7 132.6(3) . . . . ? O1 U1 N1 C7 -46.9(3) . . . . ? O3 U1 N1 C7 -101.1(3) . . . . ? O8 U1 N1 C7 72.6(3) . . . . ? O7 U1 N1 C7 25.3(3) . . . . ? N3 U1 N1 C7 -139.6(4) . . . . ? N2 U1 N1 C7 146.8(3) . . . . ? C91 U1 N1 C7 50.1(3) . . . . ? O2 U1 N1 C1 20.4(4) . . . . ? O1 U1 N1 C1 -159.1(4) . . . . ? O3 U1 N1 C1 146.6(3) . . . . ? O8 U1 N1 C1 -39.6(4) . . . . ? O7 U1 N1 C1 -86.9(4) . . . . ? N3 U1 N1 C1 108.2(4) . . . . ? N2 U1 N1 C1 34.6(3) . . . . ? C91 U1 N1 C1 -62.1(4) . . . . ? O2 U1 N2 C2 157.7(4) . . . . ? O1 U1 N2 C2 -29.5(4) . . . . ? O3 U1 N2 C2 -137.0(3) . . . . ? O8 U1 N2 C2 73.2(3) . . . . ? O7 U1 N2 C2 71.4(4) . . . . ? N3 U1 N2 C2 -83.7(4) . . . . ? N1 U1 N2 C2 -11.5(3) . . . . ? C91 U1 N2 C2 75.2(3) . . . . ? O2 U1 N2 C20 35.6(3) . . . . ? O1 U1 N2 C20 -151.6(3) . . . . ? O3 U1 N2 C20 100.9(3) . . . . ? O8 U1 N2 C20 -49.0(3) . . . . ? O7 U1 N2 C20 -50.7(3) . . . . ? N3 U1 N2 C20 154.2(3) . . . . ? N1 U1 N2 C20 -133.6(3) . . . . ? C91 U1 N2 C20 -47.0(3) . . . . ? O2 U1 N2 C3 -82.9(3) . . . . ? O1 U1 N2 C3 90.0(3) . . . . ? O3 U1 N2 C3 -17.5(3) . . . . ? O8 U1 N2 C3 -167.4(3) . . . . ? O7 U1 N2 C3 -169.1(3) . . . . ? N3 U1 N2 C3 35.7(3) . . . . ? N1 U1 N2 C3 108.0(3) . . . . ? C91 U1 N2 C3 -165.4(3) . . . . ? O2 U1 N3 C4 44.8(5) . . . . ? O1 U1 N3 C4 -158.0(5) . . . . ? O3 U1 N3 C4 121.7(5) . . . . ? O8 U1 N3 C4 -43.3(5) . . . . ? O7 U1 N3 C4 -127.9(5) . . . . ? N1 U1 N3 C4 -86.8(4) . . . . ? N2 U1 N3 C4 -14.0(4) . . . . ? C91 U1 N3 C4 -65.3(6) . . . . ? O2 U1 N3 C33 -79.3(4) . . . . ? O1 U1 N3 C33 77.8(4) . . . . ? O3 U1 N3 C33 -2.5(4) . . . . ? O8 U1 N3 C33 -167.5(3) . . . . ? O7 U1 N3 C33 107.9(4) . . . . ? N1 U1 N3 C33 149.1(4) . . . . ? N2 U1 N3 C33 -138.2(4) . . . . ? C91 U1 N3 C33 170.5(3) . . . . ? O2 U1 N3 C5 166.1(3) . . . . ? O1 U1 N3 C5 -36.7(3) . . . . ? O3 U1 N3 C5 -117.0(3) . . . . ? O8 U1 N3 C5 78.0(4) . . . . ? O7 U1 N3 C5 -6.6(5) . . . . ? N1 U1 N3 C5 34.5(3) . . . . ? N2 U1 N3 C5 107.3(3) . . . . ? C91 U1 N3 C5 56.0(5) . . . . ? C6 N1 C1 C2 67.5(6) . . . . ? C7 N1 C1 C2 -172.0(5) . . . . ? U1 N1 C1 C2 -59.7(5) . . . . ? N1 C1 C2 N2 52.0(7) . . . . ? C20 N2 C2 C1 109.6(5) . . . . ? C3 N2 C2 C1 -129.5(5) . . . . ? U1 N2 C2 C1 -14.7(6) . . . . ? C2 N2 C3 C4 62.2(6) . . . . ? C20 N2 C3 C4 -178.2(4) . . . . ? U1 N2 C3 C4 -58.5(5) . . . . ? C33 N3 C4 C3 114.1(6) . . . . ? C5 N3 C4 C3 -128.9(5) . . . . ? U1 N3 C4 C3 -10.7(7) . . . . ? N2 C3 C4 N3 50.0(7) . . . . ? C4 N3 C5 C6 66.2(6) . . . . ? C33 N3 C5 C6 -175.9(5) . . . . ? U1 N3 C5 C6 -59.4(5) . . . . ? N3 C5 C6 N1 47.4(7) . . . . ? C7 N1 C6 C5 112.3(6) . . . . ? C1 N1 C6 C5 -130.1(5) . . . . ? U1 N1 C6 C5 -8.8(7) . . . . ? C6 N1 C7 C8 -51.2(6) . . . . ? C1 N1 C7 C8 -172.0(5) . . . . ? U1 N1 C7 C8 75.7(5) . . . . ? N1 C7 C8 C13 133.5(5) . . . . ? N1 C7 C8 C9 -54.8(7) . . . . ? U1 O1 C9 C10 177.1(4) . . . . ? U1 O1 C9 C8 -0.7(8) . . . . ? C13 C8 C9 O1 179.1(4) . . . . ? C7 C8 C9 O1 7.4(7) . . . . ? C13 C8 C9 C10 1.3(7) . . . . ? C7 C8 C9 C10 -170.4(5) . . . . ? O1 C9 C10 C11 -176.6(4) . . . . ? C8 C9 C10 C11 1.1(7) . . . . ? O1 C9 C10 C14 -0.8(7) . . . . ? C8 C9 C10 C14 177.0(4) . . . . ? C9 C10 C11 C12 -2.6(7) . . . . ? C14 C10 C11 C12 -178.5(4) . . . . ? C10 C11 C12 C13 1.6(7) . . . . ? C10 C11 C12 C19 179.3(5) . . . . ? C9 C8 C13 C12 -2.4(8) . . . . ? C7 C8 C13 C12 169.4(5) . . . . ? C11 C12 C13 C8 1.0(8) . . . . ? C19 C12 C13 C8 -176.8(5) . . . . ? C11 C10 C14 C15 -78.9(6) . . . . ? C9 C10 C14 C15 105.3(5) . . . . ? C10 C14 C15 C18 -66.1(6) . . . . ? C10 C14 C15 C16 55.6(6) . . . . ? C10 C14 C15 C17 175.1(4) . . . . ? C2 N2 C20 C21 170.6(4) . . . . ? C3 N2 C20 C21 49.4(5) . . . . ? U1 N2 C20 C21 -64.6(4) . . . . ? N2 C20 C21 C26 -131.5(4) . . . . ? N2 C20 C21 C22 51.7(6) . . . . ? U1 O2 C22 C23 166.4(4) . . . . ? U1 O2 C22 C21 -11.4(9) . . . . ? C26 C21 C22 O2 173.9(4) . . . . ? C20 C21 C22 O2 -9.3(6) . . . . ? C26 C21 C22 C23 -3.9(7) . . . . ? C20 C21 C22 C23 172.9(4) . . . . ? O2 C22 C23 C24 -172.9(4) . . . . ? C21 C22 C23 C24 4.9(6) . . . . ? O2 C22 C23 C27 6.2(7) . . . . ? C21 C22 C23 C27 -176.0(4) . . . . ? C22 C23 C24 C25 -2.4(7) . . . . ? C27 C23 C24 C25 178.5(4) . . . . ? C23 C24 C25 C26 -1.1(7) . . . . ? C23 C24 C25 C32 177.1(4) . . . . ? C24 C25 C26 C21 2.2(7) . . . . ? C32 C25 C26 C21 -176.0(4) . . . . ? C22 C21 C26 C25 0.3(7) . . . . ? C20 C21 C26 C25 -176.6(4) . . . . ? C24 C23 C27 C28 -88.8(5) . . . . ? C22 C23 C27 C28 92.1(5) . . . . ? C23 C27 C28 C30 177.4(4) . . . . ? C23 C27 C28 C31 57.9(5) . . . . ? C23 C27 C28 C29 -64.2(5) . . . . ? C4 N3 C33 C34 -73.9(6) . . . . ? C5 N3 C33 C34 167.3(5) . . . . ? U1 N3 C33 C34 54.7(6) . . . . ? N3 C33 C34 C39 115.2(6) . . . . ? N3 C33 C34 C35 -74.8(6) . . . . ? U1 O3 C35 C34 57.0(6) . . . . ? U1 O3 C35 C36 -124.5(4) . . . . ? C39 C34 C35 O3 -174.7(5) . . . . ? C33 C34 C35 O3 15.2(7) . . . . ? C39 C34 C35 C36 6.8(8) . . . . ? C33 C34 C35 C36 -163.4(5) . . . . ? O3 C35 C36 C37 173.2(4) . . . . ? C34 C35 C36 C37 -8.3(7) . . . . ? O3 C35 C36 C40 -10.0(7) . . . . ? C34 C35 C36 C40 168.5(5) . . . . ? C35 C36 C37 C38 3.6(8) . . . . ? C40 C36 C37 C38 -173.2(5) . . . . ? C36 C37 C38 C39 3.0(9) . . . . ? C36 C37 C38 C45 179.9(6) . . . . ? C35 C34 C39 C38 0.0(9) . . . . ? C33 C34 C39 C38 169.6(6) . . . . ? C37 C38 C39 C34 -4.8(9) . . . . ? C45 C38 C39 C34 178.4(6) . . . . ? C35 C36 C40 C41 -96.3(6) . . . . ? C37 C36 C40 C41 80.4(6) . . . . ? C36 C40 C41 C43 173.3(5) . . . . ? C36 C40 C41 C44 -66.9(6) . . . . ? C36 C40 C41 C42 54.7(6) . . . . ? O5 U2 O4 C54 154.2(5) . . . . ? O6 U2 O4 C54 -151.3(6) . . . . ? O9 U2 O4 C54 115.5(6) . . . . ? O7 U2 O4 C54 64.5(6) . . . . ? N6 U2 O4 C54 -75.4(6) . . . . ? N4 U2 O4 C54 -8.4(5) . . . . ? N5 U2 O4 C54 -27.9(6) . . . . ? C91 U2 O4 C54 90.5(6) . . . . ? O4 U2 O5 C67 168.0(6) . . . . ? O6 U2 O5 C67 113.5(7) . . . . ? O9 U2 O5 C67 -152.6(7) . . . . ? O7 U2 O5 C67 -101.8(7) . . . . ? N6 U2 O5 C67 41.2(7) . . . . ? N4 U2 O5 C67 -33.2(7) . . . . ? N5 U2 O5 C67 -10.3(7) . . . . ? C91 U2 O5 C67 -126.5(7) . . . . ? O4 U2 O6 C80 134.8(4) . . . . ? O5 U2 O6 C80 -60.5(4) . . . . ? O9 U2 O6 C80 -139.3(4) . . . . ? O7 U2 O6 C80 -140.5(3) . . . . ? N6 U2 O6 C80 51.5(4) . . . . ? N4 U2 O6 C80 82.8(4) . . . . ? N5 U2 O6 C80 1.5(4) . . . . ? C91 U2 O6 C80 -135.7(3) . . . . ? O2 U1 O7 C91 -62.2(3) . . . . ? O1 U1 O7 C91 141.7(3) . . . . ? O3 U1 O7 C91 -145.9(3) . . . . ? O8 U1 O7 C91 6.5(2) . . . . ? N3 U1 O7 C91 110.7(4) . . . . ? N1 U1 O7 C91 73.9(3) . . . . ? N2 U1 O7 C91 8.6(3) . . . . ? O4 U2 O7 C91 92.2(3) . . . . ? O5 U2 O7 C91 -69.0(3) . . . . ? O6 U2 O7 C91 9.7(3) . . . . ? O9 U2 O7 C91 8.1(2) . . . . ? N6 U2 O7 C91 171.7(2) . . . . ? N4 U2 O7 C91 159.3(3) . . . . ? N5 U2 O7 C91 -137.7(3) . . . . ? O2 U1 O8 C91 102.8(3) . . . . ? O1 U1 O8 C91 -54.2(3) . . . . ? O3 U1 O8 C91 53.9(4) . . . . ? O7 U1 O8 C91 -6.6(2) . . . . ? N3 U1 O8 C91 -156.4(3) . . . . ? N1 U1 O8 C91 -116.7(3) . . . . ? N2 U1 O8 C91 175.3(3) . . . . ? O4 U2 O9 C91 -103.0(3) . . . . ? O5 U2 O9 C91 88.9(3) . . . . ? O6 U2 O9 C91 172.7(3) . . . . ? O7 U2 O9 C91 -8.3(2) . . . . ? N6 U2 O9 C91 -146.0(4) . . . . ? N4 U2 O9 C91 -40.5(3) . . . . ? N5 U2 O9 C91 39.8(3) . . . . ? O4 U2 N4 C46 161.4(3) . . . . ? O5 U2 N4 C46 -11.4(3) . . . . ? O6 U2 N4 C46 -141.1(3) . . . . ? O9 U2 N4 C46 89.3(3) . . . . ? O7 U2 N4 C46 63.7(3) . . . . ? N6 U2 N4 C46 -107.5(3) . . . . ? N5 U2 N4 C46 -35.1(3) . . . . ? C91 U2 N4 C46 72.7(3) . . . . ? O4 U2 N4 C52 46.7(3) . . . . ? O5 U2 N4 C52 -126.1(3) . . . . ? O6 U2 N4 C52 104.2(3) . . . . ? O9 U2 N4 C52 -25.5(3) . . . . ? O7 U2 N4 C52 -51.0(3) . . . . ? N6 U2 N4 C52 137.7(3) . . . . ? N5 U2 N4 C52 -149.8(3) . . . . ? C91 U2 N4 C52 -42.0(3) . . . . ? O4 U2 N4 C51 -77.8(3) . . . . ? O5 U2 N4 C51 109.5(3) . . . . ? O6 U2 N4 C51 -20.3(4) . . . . ? O9 U2 N4 C51 -149.9(3) . . . . ? O7 U2 N4 C51 -175.5(3) . . . . ? N6 U2 N4 C51 13.3(3) . . . . ? N5 U2 N4 C51 85.7(3) . . . . ? C91 U2 N4 C51 -166.5(3) . . . . ? O4 U2 N5 C48 -92.3(3) . . . . ? O5 U2 N5 C48 87.0(3) . . . . ? O6 U2 N5 C48 16.4(3) . . . . ? O9 U2 N5 C48 139.7(2) . . . . ? O7 U2 N5 C48 175.2(3) . . . . ? N6 U2 N5 C48 -38.5(2) . . . . ? N4 U2 N5 C48 -112.4(3) . . . . ? C91 U2 N5 C48 156.9(3) . . . . ? O4 U2 N5 C47 29.2(4) . . . . ? O5 U2 N5 C47 -151.5(3) . . . . ? O6 U2 N5 C47 137.9(3) . . . . ? O9 U2 N5 C47 -98.8(3) . . . . ? O7 U2 N5 C47 -63.3(3) . . . . ? N6 U2 N5 C47 83.0(3) . . . . ? N4 U2 N5 C47 9.1(3) . . . . ? C91 U2 N5 C47 -81.6(3) . . . . ? O4 U2 N5 C65 149.5(3) . . . . ? O5 U2 N5 C65 -31.3(3) . . . . ? O6 U2 N5 C65 -101.9(3) . . . . ? O9 U2 N5 C65 21.5(3) . . . . ? O7 U2 N5 C65 56.9(3) . . . . ? N6 U2 N5 C65 -156.8(3) . . . . ? N4 U2 N5 C65 129.3(3) . . . . ? C91 U2 N5 C65 38.6(3) . . . . ? O4 U2 N6 C49 157.8(3) . . . . ? O5 U2 N6 C49 -37.3(3) . . . . ? O6 U2 N6 C49 -115.8(3) . . . . ? O9 U2 N6 C49 -158.8(4) . . . . ? O7 U2 N6 C49 75.0(3) . . . . ? N4 U2 N6 C49 88.1(3) . . . . ? N5 U2 N6 C49 16.3(3) . . . . ? C91 U2 N6 C49 89.1(5) . . . . ? O4 U2 N6 C50 34.9(3) . . . . ? O5 U2 N6 C50 -160.3(3) . . . . ? O6 U2 N6 C50 121.2(3) . . . . ? O9 U2 N6 C50 78.2(5) . . . . ? O7 U2 N6 C50 -48.0(3) . . . . ? N4 U2 N6 C50 -34.9(3) . . . . ? N5 U2 N6 C50 -106.6(3) . . . . ? C91 U2 N6 C50 -33.9(6) . . . . ? O4 U2 N6 C78 -79.1(3) . . . . ? O5 U2 N6 C78 85.7(3) . . . . ? O6 U2 N6 C78 7.2(3) . . . . ? O9 U2 N6 C78 -35.8(5) . . . . ? O7 U2 N6 C78 -162.0(2) . . . . ? N4 U2 N6 C78 -148.9(3) . . . . ? N5 U2 N6 C78 139.4(3) . . . . ? C91 U2 N6 C78 -147.9(4) . . . . ? C52 N4 C46 C47 178.1(4) . . . . ? C51 N4 C46 C47 -61.0(5) . . . . ? U2 N4 C46 C47 62.8(4) . . . . ? C48 N5 C47 C46 133.9(4) . . . . ? C65 N5 C47 C46 -105.6(4) . . . . ? U2 N5 C47 C46 18.3(5) . . . . ? N4 C46 C47 N5 -56.2(5) . . . . ? C47 N5 C48 C49 -59.8(5) . . . . ? C65 N5 C48 C49 -177.3(4) . . . . ? U2 N5 C48 C49 63.2(4) . . . . ? C50 N6 C49 C48 128.9(4) . . . . ? C78 N6 C49 C48 -113.9(4) . . . . ? U2 N6 C49 C48 9.0(5) . . . . ? N5 C48 C49 N6 -52.2(5) . . . . ? C49 N6 C50 C51 -67.1(5) . . . . ? C78 N6 C50 C51 173.9(4) . . . . ? U2 N6 C50 C51 57.9(4) . . . . ? C46 N4 C51 C50 129.4(4) . . . . ? C52 N4 C51 C50 -112.2(4) . . . . ? U2 N4 C51 C50 10.6(5) . . . . ? N6 C50 C51 N4 -48.1(5) . . . . ? C46 N4 C52 C53 170.7(4) . . . . ? C51 N4 C52 C53 50.9(5) . . . . ? U2 N4 C52 C53 -75.4(4) . . . . ? N4 C52 C53 C58 -129.9(4) . . . . ? N4 C52 C53 C54 49.9(6) . . . . ? U2 O4 C54 C55 160.8(4) . . . . ? U2 O4 C54 C53 -15.2(8) . . . . ? C58 C53 C54 O4 -179.3(4) . . . . ? C52 C53 C54 O4 0.9(6) . . . . ? C58 C53 C54 C55 4.7(6) . . . . ? C52 C53 C54 C55 -175.1(4) . . . . ? O4 C54 C55 C56 179.5(4) . . . . ? C53 C54 C55 C56 -4.7(6) . . . . ? O4 C54 C55 C59 -3.3(7) . . . . ? C53 C54 C55 C59 172.5(4) . . . . ? C54 C55 C56 C57 0.8(7) . . . . ? C59 C55 C56 C57 -176.4(4) . . . . ? C55 C56 C57 C58 2.9(7) . . . . ? C55 C56 C57 C64 -177.9(4) . . . . ? C54 C53 C58 C57 -0.9(7) . . . . ? C52 C53 C58 C57 179.0(4) . . . . ? C56 C57 C58 C53 -2.8(7) . . . . ? C64 C57 C58 C53 178.0(4) . . . . ? C54 C55 C59 C60 93.9(6) . . . . ? C56 C55 C59 C60 -89.0(6) . . . . ? C55 C59 C60 C61 55.2(6) . . . . ? C55 C59 C60 C63 -67.2(6) . . . . ? C55 C59 C60 C62 174.1(5) . . . . ? C48 N5 C65 C66 -48.4(5) . . . . ? C47 N5 C65 C66 -170.1(4) . . . . ? U2 N5 C65 C66 64.6(5) . . . . ? N5 C65 C66 C67 -54.8(6) . . . . ? N5 C65 C66 C71 131.3(5) . . . . ? U2 O5 C67 C66 23.4(10) . . . . ? U2 O5 C67 C68 -154.8(5) . . . . ? C71 C66 C67 O5 -176.6(4) . . . . ? C65 C66 C67 O5 9.6(7) . . . . ? C71 C66 C67 C68 1.8(7) . . . . ? C65 C66 C67 C68 -172.1(4) . . . . ? O5 C67 C68 C69 175.4(4) . . . . ? C66 C67 C68 C69 -2.8(7) . . . . ? O5 C67 C68 C72 -7.2(7) . . . . ? C66 C67 C68 C72 174.5(4) . . . . ? C67 C68 C69 C70 1.2(7) . . . . ? C72 C68 C69 C70 -176.1(5) . . . . ? C68 C69 C70 C71 1.4(7) . . . . ? C68 C69 C70 C77 -177.6(5) . . . . ? C67 C66 C71 C70 1.0(7) . . . . ? C65 C66 C71 C70 174.8(4) . . . . ? C69 C70 C71 C66 -2.5(7) . . . . ? C77 C70 C71 C66 176.5(5) . . . . ? C69 C68 C72 C73 84.2(6) . . . . ? C67 C68 C72 C73 -93.1(5) . . . . ? C68 C72 C73 C76 59.7(6) . . . . ? C68 C72 C73 C75 178.2(4) . . . . ? C68 C72 C73 C74 -62.0(6) . . . . ? C49 N6 C78 C79 67.2(5) . . . . ? C50 N6 C78 C79 -172.5(4) . . . . ? U2 N6 C78 C79 -58.8(4) . . . . ? N6 C78 C79 C84 -110.7(5) . . . . ? N6 C78 C79 C80 74.6(5) . . . . ? U2 O6 C80 C79 -59.6(6) . . . . ? U2 O6 C80 C81 121.6(4) . . . . ? C84 C79 C80 O6 173.3(4) . . . . ? C78 C79 C80 O6 -11.9(6) . . . . ? C84 C79 C80 C81 -7.9(7) . . . . ? C78 C79 C80 C81 167.0(4) . . . . ? O6 C80 C81 C82 -171.6(4) . . . . ? C79 C80 C81 C82 9.6(7) . . . . ? O6 C80 C81 C85 11.6(7) . . . . ? C79 C80 C81 C85 -167.2(4) . . . . ? C80 C81 C82 C83 -3.8(7) . . . . ? C85 C81 C82 C83 173.0(5) . . . . ? C81 C82 C83 C84 -3.7(7) . . . . ? C81 C82 C83 C90 175.1(5) . . . . ? C80 C79 C84 C83 0.0(7) . . . . ? C78 C79 C84 C83 -174.5(4) . . . . ? C82 C83 C84 C79 5.7(7) . . . . ? C90 C83 C84 C79 -173.1(4) . . . . ? C82 C81 C85 C86 -85.9(6) . . . . ? C80 C81 C85 C86 90.8(6) . . . . ? C81 C85 C86 C88 58.8(6) . . . . ? C81 C85 C86 C87 -64.0(6) . . . . ? C81 C85 C86 C89 176.8(4) . . . . ? U1 O8 C91 O7 11.9(4) . . . . ? U1 O8 C91 O9 -169.3(4) . . . . ? U1 O8 C91 U2 115.5(14) . . . . ? U1 O7 C91 O8 -10.9(4) . . . . ? U2 O7 C91 O8 165.3(4) . . . . ? U1 O7 C91 O9 170.3(4) . . . . ? U2 O7 C91 O9 -13.5(4) . . . . ? U1 O7 C91 U2 -176.21(13) . . . . ? U2 O7 C91 U1 176.21(13) . . . . ? U2 O9 C91 O8 -163.3(4) . . . . ? U2 O9 C91 O7 15.5(4) . . . . ? O4 U2 C91 O8 161.5(15) . . . . ? O5 U2 C91 O8 -1.4(15) . . . . ? O6 U2 C91 O8 76.6(15) . . . . ? O9 U2 C91 O8 84.9(15) . . . . ? O7 U2 C91 O8 -109.9(15) . . . . ? N6 U2 C91 O8 -130.9(13) . . . . ? N4 U2 C91 O8 -130.0(15) . . . . ? N5 U2 C91 O8 -64.1(15) . . . . ? O4 U2 C91 O7 -88.6(3) . . . . ? O5 U2 C91 O7 108.5(3) . . . . ? O6 U2 C91 O7 -173.5(2) . . . . ? O9 U2 C91 O7 -165.2(4) . . . . ? N6 U2 C91 O7 -21.1(6) . . . . ? N4 U2 C91 O7 -20.2(3) . . . . ? N5 U2 C91 O7 45.7(3) . . . . ? O4 U2 C91 O9 76.6(3) . . . . ? O5 U2 C91 O9 -86.3(3) . . . . ? O6 U2 C91 O9 -8.3(3) . . . . ? O7 U2 C91 O9 165.2(4) . . . . ? N6 U2 C91 O9 144.1(4) . . . . ? N4 U2 C91 O9 145.0(3) . . . . ? N5 U2 C91 O9 -149.1(3) . . . . ? O4 U2 C91 U1 -93.0(2) . . . . ? O5 U2 C91 U1 104.1(2) . . . . ? O6 U2 C91 U1 -177.95(17) . . . . ? O9 U2 C91 U1 -169.6(4) . . . . ? O7 U2 C91 U1 -4.41(15) . . . . ? N6 U2 C91 U1 -25.5(6) . . . . ? N4 U2 C91 U1 -24.6(2) . . . . ? N5 U2 C91 U1 41.3(2) . . . . ? O2 U1 C91 O8 -73.5(3) . . . . ? O1 U1 C91 O8 131.0(3) . . . . ? O3 U1 C91 O8 -147.8(3) . . . . ? O7 U1 C91 O8 168.1(4) . . . . ? N3 U1 C91 O8 41.3(5) . . . . ? N1 U1 C91 O8 60.6(3) . . . . ? N2 U1 C91 O8 -4.5(3) . . . . ? O2 U1 C91 O7 118.3(3) . . . . ? O1 U1 C91 O7 -37.2(3) . . . . ? O3 U1 C91 O7 44.1(3) . . . . ? O8 U1 C91 O7 -168.1(4) . . . . ? N3 U1 C91 O7 -126.9(3) . . . . ? N1 U1 C91 O7 -107.5(3) . . . . ? N2 U1 C91 O7 -172.6(2) . . . . ? O2 U1 C91 U2 122.8(2) . . . . ? O1 U1 C91 U2 -32.7(2) . . . . ? O3 U1 C91 U2 48.6(3) . . . . ? O8 U1 C91 U2 -163.6(4) . . . . ? O7 U1 C91 U2 4.53(15) . . . . ? N3 U1 C91 U2 -122.3(3) . . . . ? N1 U1 C91 U2 -103.0(2) . . . . ? N2 U1 C91 U2 -168.1(2) . . . . ? C106 C101 C102 C103 1.2(9) . . . . ? C101 C102 C103 C104 -0.7(9) . . . . ? C102 C103 C104 C105 -0.6(9) . . . . ? C103 C104 C105 C106 1.3(9) . . . . ? C102 C101 C106 C105 -0.4(8) . . . . ? C104 C105 C106 C101 -0.9(8) . . . . ? C206 C201 C202 C203 0.5(8) . . . . ? C201 C202 C203 C204 -0.3(9) . . . . ? C202 C203 C204 C205 -0.4(9) . . . . ? C203 C204 C205 C206 0.8(8) . . . . ? C202 C201 C206 C205 -0.1(8) . . . . ? C204 C205 C206 C201 -0.5(8) . . . . ? C303 C301 C302 C303 -3.7(12) 3_566 . . . ? C301 C302 C303 C301 3.7(13) . . . 3_566 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 7.031 _refine_diff_density_min -2.910 _refine_diff_density_rms 0.129 #===END OF DATA FOR 5 * 2.5 benzene # Attachment '- CCDC_886107.cif' data_acs1121 _database_code_depnum_ccdc_archive 'CCDC 886107' #TrackingRef '- CCDC_886107.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C184 H264 K4 N12 O24 U4, 18(C6 H6)' _chemical_formula_sum 'C292 H372 K4 N12 O24 U4' _chemical_formula_weight 5542.54 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' K K 0.2009 0.2494 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.9925(4) _cell_length_b 20.0409(4) _cell_length_c 21.8950(4) _cell_angle_alpha 71.285(1) _cell_angle_beta 65.118(1) _cell_angle_gamma 63.811(1) _cell_volume 6690.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9156 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.77 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2844 _exptl_absorpt_coefficient_mu 2.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2008' _exptl_special_details ; ? ; _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 'Bruker Smart APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 122215 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.88 _reflns_number_total 31153 _reflns_number_gt 20804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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. ; _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^)+(0.0475P)^2^+3.6650P] 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 31153 _refine_ls_number_parameters 1501 _refine_ls_number_restraints 188 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.206720(11) 0.727198(10) 0.152400(9) 0.01769(5) Uani 1 1 d . . . U2 U -0.192903(11) 0.443001(10) 0.418853(9) 0.02104(6) Uani 1 1 d . . . K1 K -0.00023(7) 0.59758(6) 0.29257(6) 0.0292(3) Uani 1 1 d . . . K2 K 0.10845(7) 0.48826(7) 0.42939(6) 0.0301(3) Uani 1 1 d . . . O1 O 0.11371(19) 0.81075(17) 0.21798(16) 0.0204(7) Uani 1 1 d . . . O2 O 0.1378(2) 0.75130(18) 0.08519(16) 0.0230(8) Uani 1 1 d . . . O3 O 0.30551(19) 0.61940(18) 0.13126(16) 0.0227(8) Uani 1 1 d . . . O4 O 0.12456(19) 0.65288(17) 0.22208(16) 0.0208(7) Uani 1 1 d . . . O5 O 0.2060(2) 0.65947(18) 0.26610(16) 0.0227(8) Uani 1 1 d . . . O6 O 0.1248(2) 0.59037(19) 0.32718(17) 0.0280(8) Uani 1 1 d . . . O7 O -0.1983(2) 0.4375(2) 0.32005(16) 0.0268(8) Uani 1 1 d . . . O8 O -0.2872(2) 0.55472(19) 0.41146(16) 0.0259(8) Uani 1 1 d . . . O9 O -0.0767(2) 0.35334(18) 0.38768(16) 0.0246(8) Uani 1 1 d . . . O10 O -0.1035(2) 0.51579(18) 0.36888(16) 0.0226(8) Uani 1 1 d . . . O11 O -0.1326(2) 0.47218(19) 0.47916(16) 0.0263(8) Uani 1 1 d . . . O12 O -0.0401(2) 0.53039(19) 0.42737(17) 0.0263(8) Uani 1 1 d . . . N1 N 0.2815(2) 0.8026(2) 0.16586(19) 0.0172(8) Uani 1 1 d . . . N2 N 0.1901(2) 0.8761(2) 0.07166(19) 0.0192(9) Uani 1 1 d . . . N3 N 0.3419(2) 0.7443(2) 0.03637(19) 0.0202(9) Uani 1 1 d . . . N4 N -0.3067(2) 0.3784(2) 0.4568(2) 0.0227(9) Uani 1 1 d . . . N5 N -0.3109(2) 0.4662(2) 0.5447(2) 0.0239(9) Uani 1 1 d . . . N6 N -0.1775(2) 0.3196(2) 0.5223(2) 0.0234(9) Uani 1 1 d . . . C1 C 0.2635(3) 0.8843(3) 0.1384(2) 0.0217(11) Uani 1 1 d . . . H1A H 0.3126 0.8910 0.0995 0.026 Uiso 1 1 calc R . . H1B H 0.2539 0.9104 0.1742 0.026 Uiso 1 1 calc R . . C2 C 0.1881(3) 0.9207(3) 0.1146(2) 0.0221(11) Uani 1 1 d . . . H2A H 0.1371 0.9265 0.1550 0.027 Uiso 1 1 calc R . . H2B H 0.1859 0.9717 0.0884 0.027 Uiso 1 1 calc R . . C3 C 0.2555(3) 0.8803(3) 0.0052(2) 0.0207(11) Uani 1 1 d . . . H3A H 0.2911 0.9029 0.0076 0.025 Uiso 1 1 calc R . . H3B H 0.2295 0.9137 -0.0299 0.025 Uiso 1 1 calc R . . C4 C 0.3089(3) 0.8037(3) -0.0159(2) 0.0206(11) Uani 1 1 d . . . H4A H 0.2757 0.7868 -0.0284 0.025 Uiso 1 1 calc R . . H4B H 0.3563 0.8090 -0.0573 0.025 Uiso 1 1 calc R . . C5 C 0.3958(3) 0.7630(3) 0.0566(2) 0.0213(11) Uani 1 1 d . . . H5A H 0.3939 0.8150 0.0345 0.026 Uiso 1 1 calc R . . H5B H 0.4539 0.7284 0.0397 0.026 Uiso 1 1 calc R . . C6 C 0.3702(3) 0.7569(3) 0.1339(2) 0.0212(11) Uani 1 1 d . . . H6A H 0.3801 0.7034 0.1553 0.025 Uiso 1 1 calc R . . H6B H 0.4059 0.7736 0.1435 0.025 Uiso 1 1 calc R . . C7 C 0.2616(3) 0.7896(3) 0.2417(2) 0.0201(10) Uani 1 1 d . . . H7A H 0.3014 0.8007 0.2514 0.024 Uiso 1 1 calc R . . H7B H 0.2694 0.7356 0.2598 0.024 Uiso 1 1 calc R . . C8 C 0.1745(3) 0.8367(3) 0.2790(2) 0.0191(10) Uani 1 1 d . . . C9 C 0.1045(3) 0.8442(3) 0.2658(2) 0.0201(11) Uani 1 1 d . . . C10 C 0.0253(3) 0.8910(3) 0.3008(2) 0.0207(11) Uani 1 1 d . . . C11 C 0.0177(3) 0.9272(3) 0.3486(2) 0.0246(11) Uani 1 1 d . . . H11A H -0.0358 0.9595 0.3716 0.029 Uiso 1 1 calc R . . C12 C 0.0857(3) 0.9181(3) 0.3645(2) 0.0247(11) Uani 1 1 d . . . C13 C 0.1629(3) 0.8734(3) 0.3286(2) 0.0225(11) Uani 1 1 d . . . H13A H 0.2100 0.8672 0.3381 0.027 Uiso 1 1 calc R . . C14 C -0.0497(3) 0.9041(3) 0.2835(2) 0.0252(12) Uani 1 1 d . . . H14A H -0.0300 0.8963 0.2358 0.030 Uiso 1 1 calc R . . H14B H -0.0861 0.9577 0.2851 0.030 Uiso 1 1 calc R . . C15 C -0.1028(3) 0.8553(3) 0.3286(3) 0.0271(12) Uani 1 1 d . . . C16 C -0.0486(3) 0.7714(3) 0.3337(3) 0.0354(14) Uani 1 1 d . . . H16A H -0.0194 0.7580 0.2879 0.053 Uiso 1 1 calc R . . H16B H -0.0838 0.7412 0.3614 0.053 Uiso 1 1 calc R . . H16C H -0.0080 0.7613 0.3551 0.053 Uiso 1 1 calc R . . C17 C -0.1657(4) 0.8703(4) 0.2951(3) 0.0449(16) Uani 1 1 d . . . H17A H -0.1363 0.8527 0.2510 0.067 Uiso 1 1 calc R . . H17B H -0.1973 0.9246 0.2880 0.067 Uiso 1 1 calc R . . H17C H -0.2038 0.8434 0.3248 0.067 Uiso 1 1 calc R . . C18 C -0.1510(3) 0.8764(3) 0.3999(3) 0.0308(13) Uani 1 1 d . . . H18A H -0.1881 0.8478 0.4259 0.046 Uiso 1 1 calc R . . H18B H -0.1838 0.9305 0.3962 0.046 Uiso 1 1 calc R . . H18C H -0.1118 0.8644 0.4235 0.046 Uiso 1 1 calc R . . C19 C 0.0753(3) 0.9582(3) 0.4175(3) 0.0322(13) Uani 1 1 d . . . H19A H 0.1283 0.9403 0.4256 0.048 Uiso 1 1 calc R . . H19B H 0.0328 0.9476 0.4602 0.048 Uiso 1 1 calc R . . H19C H 0.0583 1.0127 0.4009 0.048 Uiso 1 1 calc R . . C20 C 0.1073(3) 0.9072(3) 0.0626(2) 0.0196(10) Uani 1 1 d . . . H20A H 0.0938 0.9618 0.0446 0.024 Uiso 1 1 calc R . . H20B H 0.0651 0.9016 0.1080 0.024 Uiso 1 1 calc R . . C21 C 0.1002(3) 0.8711(3) 0.0158(2) 0.0211(11) Uani 1 1 d . . . C22 C 0.1099(3) 0.7947(3) 0.0333(2) 0.0211(11) Uani 1 1 d . . . C23 C 0.0911(3) 0.7626(3) -0.0035(2) 0.0223(11) Uani 1 1 d . . . C24 C 0.0687(3) 0.8072(3) -0.0606(2) 0.0251(12) Uani 1 1 d . . . H24A H 0.0562 0.7860 -0.0861 0.030 Uiso 1 1 calc R . . C25 C 0.0641(3) 0.8819(3) -0.0815(3) 0.0250(12) Uani 1 1 d . . . C26 C 0.0781(3) 0.9131(3) -0.0421(2) 0.0207(11) Uani 1 1 d . . . H26A H 0.0726 0.9647 -0.0547 0.025 Uiso 1 1 calc R . . C27 C 0.0968(3) 0.6814(3) 0.0197(3) 0.0271(12) Uani 1 1 d . . . H27A H 0.1440 0.6530 0.0375 0.033 Uiso 1 1 calc R . . H27B H 0.1100 0.6605 -0.0207 0.033 Uiso 1 1 calc R . . C28 C 0.0182(3) 0.6671(3) 0.0753(3) 0.0291(13) Uani 1 1 d . . . C29 C -0.0183(3) 0.7111(3) 0.1339(3) 0.0340(13) Uani 1 1 d . . . H29A H -0.0649 0.6972 0.1692 0.051 Uiso 1 1 calc R . . H29B H -0.0380 0.7653 0.1165 0.051 Uiso 1 1 calc R . . H29C H 0.0246 0.6990 0.1535 0.051 Uiso 1 1 calc R . . C30 C 0.0445(4) 0.5832(3) 0.1038(3) 0.0398(15) Uani 1 1 d . . . H30A H -0.0040 0.5714 0.1376 0.060 Uiso 1 1 calc R . . H30B H 0.0858 0.5698 0.1255 0.060 Uiso 1 1 calc R . . H30C H 0.0688 0.5544 0.0666 0.060 Uiso 1 1 calc R . . C31 C -0.0485(4) 0.6897(3) 0.0423(3) 0.0421(15) Uani 1 1 d . . . H31A H -0.0967 0.6775 0.0765 0.063 Uiso 1 1 calc R . . H31B H -0.0254 0.6620 0.0045 0.063 Uiso 1 1 calc R . . H31C H -0.0658 0.7440 0.0250 0.063 Uiso 1 1 calc R . . C32 C 0.0453(3) 0.9275(3) -0.1467(3) 0.0319(13) Uani 1 1 d . . . H32A H 0.0607 0.9722 -0.1607 0.048 Uiso 1 1 calc R . . H32B H -0.0142 0.9433 -0.1387 0.048 Uiso 1 1 calc R . . H32C H 0.0772 0.8965 -0.1829 0.048 Uiso 1 1 calc R . . C33 C 0.3912(3) 0.6753(3) 0.0035(2) 0.0217(11) Uani 1 1 d . . . H33A H 0.4328 0.6871 -0.0402 0.026 Uiso 1 1 calc R . . H33B H 0.3533 0.6627 -0.0073 0.026 Uiso 1 1 calc R . . C34 C 0.4355(3) 0.6071(3) 0.0454(2) 0.0199(10) Uani 1 1 d . . . C35 C 0.3876(3) 0.5800(3) 0.1097(2) 0.0204(11) Uani 1 1 d . . . C36 C 0.4263(3) 0.5143(3) 0.1488(2) 0.0233(11) Uani 1 1 d . . . C37 C 0.5118(3) 0.4789(3) 0.1224(3) 0.0258(12) Uani 1 1 d . . . H37A H 0.5383 0.4343 0.1487 0.031 Uiso 1 1 calc R . . C38 C 0.5604(3) 0.5054(3) 0.0595(3) 0.0252(11) Uani 1 1 d . . . C39 C 0.5201(3) 0.5701(3) 0.0218(2) 0.0240(11) Uani 1 1 d . . . H39A H 0.5516 0.5895 -0.0216 0.029 Uiso 1 1 calc R . . C40 C 0.3756(3) 0.4841(3) 0.2181(2) 0.0264(12) Uani 1 1 d . . . H40A H 0.3288 0.5274 0.2388 0.032 Uiso 1 1 calc R . . H40B H 0.4110 0.4590 0.2476 0.032 Uiso 1 1 calc R . . C41 C 0.3399(3) 0.4279(3) 0.2189(3) 0.0265(12) Uani 1 1 d . . . C42 C 0.4088(3) 0.3553(3) 0.1963(3) 0.0364(14) Uani 1 1 d . . . H42A H 0.4434 0.3332 0.2258 0.055 Uiso 1 1 calc R . . H42B H 0.4431 0.3663 0.1489 0.055 Uiso 1 1 calc R . . H42C H 0.3844 0.3197 0.1997 0.055 Uiso 1 1 calc R . . C43 C 0.2869(4) 0.4088(3) 0.2927(3) 0.0417(15) Uani 1 1 d . . . H43A H 0.3213 0.3878 0.3223 0.063 Uiso 1 1 calc R . . H43B H 0.2648 0.3717 0.2954 0.063 Uiso 1 1 calc R . . H43C H 0.2409 0.4547 0.3077 0.063 Uiso 1 1 calc R . . C44 C 0.2865(3) 0.4624(3) 0.1728(3) 0.0292(12) Uani 1 1 d . . . H44A H 0.2613 0.4271 0.1766 0.044 Uiso 1 1 calc R . . H44B H 0.3211 0.4726 0.1254 0.044 Uiso 1 1 calc R . . H44C H 0.2426 0.5097 0.1868 0.044 Uiso 1 1 calc R . . C45 C 0.6535(3) 0.4662(3) 0.0328(3) 0.0326(13) Uani 1 1 d . . . H45A H 0.6712 0.4227 0.0667 0.049 Uiso 1 1 calc R . . H45B H 0.6810 0.5014 0.0240 0.049 Uiso 1 1 calc R . . H45C H 0.6687 0.4490 -0.0098 0.049 Uiso 1 1 calc R . . C46 C 0.1520(3) 0.6325(3) 0.2744(2) 0.0227(11) Uani 1 1 d . . . C47 C -0.3853(3) 0.4341(3) 0.4928(2) 0.0249(11) Uani 1 1 d . . . H47A H -0.4311 0.4156 0.5060 0.030 Uiso 1 1 calc R . . H47B H -0.3971 0.4822 0.4608 0.030 Uiso 1 1 calc R . . C48 C -0.3848(3) 0.4492(3) 0.5562(2) 0.0264(12) Uani 1 1 d . . . H48A H -0.4356 0.4923 0.5727 0.032 Uiso 1 1 calc R . . H48B H -0.3864 0.4045 0.5924 0.032 Uiso 1 1 calc R . . C49 C -0.2692(3) 0.4183(3) 0.5965(2) 0.0250(11) Uani 1 1 d . . . H49A H -0.3101 0.4258 0.6426 0.030 Uiso 1 1 calc R . . H49B H -0.2246 0.4353 0.5903 0.030 Uiso 1 1 calc R . . C50 C -0.2323(3) 0.3357(3) 0.5928(2) 0.0272(12) Uani 1 1 d . . . H50A H -0.1994 0.3087 0.6242 0.033 Uiso 1 1 calc R . . H50B H -0.2777 0.3161 0.6083 0.033 Uiso 1 1 calc R . . C51 C -0.1990(3) 0.2693(3) 0.5015(3) 0.0267(12) Uani 1 1 d . . . H51A H -0.1909 0.2207 0.5334 0.032 Uiso 1 1 calc R . . H51B H -0.1605 0.2588 0.4553 0.032 Uiso 1 1 calc R . . C52 C -0.2874(3) 0.3026(3) 0.5009(2) 0.0256(12) Uani 1 1 d . . . H52A H -0.2969 0.2677 0.4844 0.031 Uiso 1 1 calc R . . H52B H -0.3260 0.3072 0.5482 0.031 Uiso 1 1 calc R . . C53 C -0.3165(3) 0.3694(3) 0.3960(2) 0.0240(11) Uani 1 1 d . . . H53A H -0.3634 0.3516 0.4123 0.029 Uiso 1 1 calc R . . H53B H -0.2657 0.3291 0.3743 0.029 Uiso 1 1 calc R . . C54 C -0.3315(3) 0.4379(3) 0.3417(2) 0.0246(11) Uani 1 1 d . . . C55 C -0.2657(3) 0.4634(3) 0.3014(2) 0.0238(11) Uani 1 1 d . . . C56 C -0.2702(3) 0.5142(3) 0.2400(3) 0.0290(12) Uani 1 1 d . . . C57 C -0.3456(3) 0.5456(3) 0.2279(3) 0.0302(13) Uani 1 1 d . . . H57A H -0.3505 0.5828 0.1884 0.036 Uiso 1 1 calc R . . C58 C -0.4140(3) 0.5257(3) 0.2703(3) 0.0284(12) Uani 1 1 d . . . C59 C -0.4040(3) 0.4695(3) 0.3259(3) 0.0273(12) Uani 1 1 d . . . H59A H -0.4485 0.4520 0.3541 0.033 Uiso 1 1 calc R . . C60 C -0.1934(3) 0.5262(3) 0.1853(3) 0.0299(13) Uani 1 1 d . . . H60A H -0.1540 0.5197 0.2073 0.036 Uiso 1 1 calc R . . H60B H -0.2089 0.5787 0.1606 0.036 Uiso 1 1 calc R . . C61 C -0.1493(3) 0.4713(3) 0.1334(3) 0.0305(13) Uani 1 1 d . . . C62 C -0.2077(3) 0.4804(3) 0.0972(3) 0.0334(13) Uani 1 1 d . . . H62A H -0.2526 0.4624 0.1299 0.050 Uiso 1 1 calc R . . H62B H -0.1763 0.4508 0.0599 0.050 Uiso 1 1 calc R . . H62C H -0.2314 0.5337 0.0786 0.050 Uiso 1 1 calc R . . C63 C -0.1191(3) 0.3889(3) 0.1683(3) 0.0354(14) Uani 1 1 d . . . H63A H -0.0804 0.3824 0.1903 0.053 Uiso 1 1 calc R . . H63B H -0.0909 0.3556 0.1342 0.053 Uiso 1 1 calc R . . H63C H -0.1668 0.3762 0.2029 0.053 Uiso 1 1 calc R . . C64 C -0.0744(4) 0.4899(3) 0.0796(3) 0.0379(14) Uani 1 1 d . . . H64A H -0.0349 0.4818 0.1014 0.057 Uiso 1 1 calc R . . H64B H -0.0927 0.5427 0.0577 0.057 Uiso 1 1 calc R . . H64C H -0.0474 0.4571 0.0451 0.057 Uiso 1 1 calc R . . C65 C -0.4946(3) 0.5621(3) 0.2552(3) 0.0408(15) Uani 1 1 d . . . H65A H -0.4829 0.5694 0.2059 0.061 Uiso 1 1 calc R . . H65B H -0.5257 0.6110 0.2708 0.061 Uiso 1 1 calc R . . H65C H -0.5276 0.5294 0.2790 0.061 Uiso 1 1 calc R . . C66 C -0.3355(3) 0.5448(3) 0.5533(3) 0.0264(12) Uani 1 1 d . . . H66A H -0.2843 0.5545 0.5424 0.032 Uiso 1 1 calc R . . H66B H -0.3676 0.5488 0.6020 0.032 Uiso 1 1 calc R . . C67 C -0.3865(3) 0.6065(3) 0.5108(3) 0.0252(12) Uani 1 1 d . . . C68 C -0.3548(3) 0.6109(3) 0.4391(3) 0.0251(12) Uani 1 1 d . . . C69 C -0.3959(3) 0.6743(3) 0.3995(3) 0.0285(12) Uani 1 1 d . . . C70 C -0.4671(3) 0.7283(3) 0.4317(3) 0.0294(12) Uani 1 1 d . . . H70A H -0.4952 0.7707 0.4046 0.035 Uiso 1 1 calc R . . C71 C -0.5001(3) 0.7233(3) 0.5034(3) 0.0310(13) Uani 1 1 d . . . C72 C -0.4573(3) 0.6618(3) 0.5409(3) 0.0309(13) Uani 1 1 d . . . H72A H -0.4774 0.6574 0.5892 0.037 Uiso 1 1 calc R . . C73 C -0.3609(3) 0.6845(3) 0.3221(3) 0.0290(12) Uani 1 1 d . . . H73A H -0.4079 0.7087 0.3040 0.035 Uiso 1 1 calc R . . H73B H -0.3290 0.6339 0.3085 0.035 Uiso 1 1 calc R . . C74 C -0.3042(3) 0.7315(3) 0.2877(3) 0.0309(13) Uani 1 1 d . . . C75 C -0.2253(3) 0.6917(4) 0.3084(3) 0.0441(16) Uani 1 1 d . . . H75A H -0.1892 0.7216 0.2852 0.066 Uiso 1 1 calc R . . H75B H -0.1957 0.6416 0.2951 0.066 Uiso 1 1 calc R . . H75C H -0.2408 0.6867 0.3579 0.066 Uiso 1 1 calc R . . C76 C -0.3484(4) 0.8108(3) 0.3071(3) 0.0432(15) Uani 1 1 d . . . H76A H -0.3139 0.8414 0.2790 0.065 Uiso 1 1 calc R . . H76B H -0.3575 0.8069 0.3554 0.065 Uiso 1 1 calc R . . H76C H -0.4020 0.8345 0.2991 0.065 Uiso 1 1 calc R . . C77 C -0.2796(4) 0.7394(3) 0.2103(3) 0.0451(16) Uani 1 1 d . . . H77A H -0.2407 0.7666 0.1874 0.068 Uiso 1 1 calc R . . H77B H -0.3294 0.7676 0.1966 0.068 Uiso 1 1 calc R . . H77C H -0.2530 0.6893 0.1974 0.068 Uiso 1 1 calc R . . C78 C -0.5762(3) 0.7853(3) 0.5356(3) 0.0431(15) Uani 1 1 d . . . H78A H -0.6113 0.7634 0.5774 0.065 Uiso 1 1 calc R . . H78B H -0.6073 0.8142 0.5036 0.065 Uiso 1 1 calc R . . H78C H -0.5598 0.8187 0.5469 0.065 Uiso 1 1 calc R . . C79 C -0.0902(3) 0.2825(3) 0.5243(2) 0.0270(12) Uani 1 1 d . . . H79A H -0.0898 0.2432 0.5655 0.032 Uiso 1 1 calc R . . H79B H -0.0746 0.3209 0.5297 0.032 Uiso 1 1 calc R . . C80 C -0.0239(3) 0.2466(3) 0.4635(3) 0.0261(12) Uani 1 1 d . . . C81 C -0.0177(3) 0.2859(3) 0.3969(3) 0.0272(12) Uani 1 1 d . . . C82 C 0.0471(3) 0.2538(3) 0.3416(3) 0.0241(11) Uani 1 1 d . . . C83 C 0.1058(3) 0.1834(3) 0.3540(3) 0.0293(12) Uani 1 1 d . . . H83A H 0.1498 0.1614 0.3163 0.035 Uiso 1 1 calc R . . C84 C 0.1023(3) 0.1436(3) 0.4202(3) 0.0305(13) Uani 1 1 d . . . C85 C 0.0358(3) 0.1766(3) 0.4736(3) 0.0285(12) Uani 1 1 d . . . H85A H 0.0309 0.1500 0.5189 0.034 Uiso 1 1 calc R . . C86 C 0.0528(3) 0.2957(3) 0.2693(3) 0.0294(12) Uani 1 1 d . . . H86A H -0.0038 0.3301 0.2689 0.035 Uiso 1 1 calc R . . H86B H 0.0726 0.2585 0.2395 0.035 Uiso 1 1 calc R . . C87 C 0.1102(3) 0.3423(3) 0.2380(3) 0.0316(13) Uani 1 1 d . . . C88 C 0.0837(3) 0.4000(3) 0.2822(3) 0.0377(14) Uani 1 1 d . . . H88A H 0.0850 0.3740 0.3282 0.057 Uiso 1 1 calc R . . H88B H 0.0272 0.4353 0.2847 0.057 Uiso 1 1 calc R . . H88C H 0.1218 0.4278 0.2621 0.057 Uiso 1 1 calc R . . C89 C 0.1023(4) 0.3837(4) 0.1679(3) 0.0488(17) Uani 1 1 d . . . H89A H 0.0440 0.4150 0.1730 0.073 Uiso 1 1 calc R . . H89B H 0.1218 0.3469 0.1385 0.073 Uiso 1 1 calc R . . H89C H 0.1360 0.4157 0.1474 0.073 Uiso 1 1 calc R . . C90 C 0.2002(3) 0.2898(3) 0.2299(3) 0.0366(14) Uani 1 1 d . . . H90A H 0.2060 0.2660 0.2750 0.055 Uiso 1 1 calc R . . H90B H 0.2370 0.3189 0.2052 0.055 Uiso 1 1 calc R . . H90C H 0.2154 0.2507 0.2041 0.055 Uiso 1 1 calc R . . C91 C 0.1703(3) 0.0704(3) 0.4327(3) 0.0387(14) Uani 1 1 d . . . H91A H 0.1471 0.0388 0.4741 0.058 Uiso 1 1 calc R . . H91B H 0.2129 0.0807 0.4383 0.058 Uiso 1 1 calc R . . H91C H 0.1952 0.0441 0.3936 0.058 Uiso 1 1 calc R . . C92 C -0.0905(3) 0.5075(3) 0.4248(3) 0.0242(11) Uani 1 1 d . . . C93 C 0.2084(4) 0.3147(3) 0.5104(3) 0.0467(16) Uani 1 1 d . . . H93A H 0.1910 0.3442 0.5440 0.056 Uiso 1 1 calc R . . C94 C 0.2906(4) 0.2737(4) 0.4835(3) 0.0510(18) Uani 1 1 d . . . H94A H 0.3307 0.2743 0.4983 0.061 Uiso 1 1 calc R . . C95 C 0.3152(4) 0.2307(4) 0.4338(4) 0.065(2) Uani 1 1 d . . . H95A H 0.3721 0.2019 0.4143 0.078 Uiso 1 1 calc R . . C96 C 0.2547(5) 0.2311(4) 0.4134(3) 0.0571(19) Uani 1 1 d . . . H96A H 0.2704 0.2019 0.3800 0.069 Uiso 1 1 calc R . . C97 C 0.1738(4) 0.2727(4) 0.4405(3) 0.0492(18) Uani 1 1 d . . . H97A H 0.1332 0.2733 0.4256 0.059 Uiso 1 1 calc R . . C98 C 0.1509(4) 0.3133(3) 0.4890(3) 0.0466(17) Uani 1 1 d . . . H98A H 0.0938 0.3415 0.5086 0.056 Uiso 1 1 calc R . . C101 C 0.4680(5) 0.8606(5) 0.2131(4) 0.092(3) Uani 1 1 d U . . H101 H 0.5005 0.8702 0.1667 0.110 Uiso 1 1 calc R . . C102 C 0.4695(4) 0.7883(5) 0.2430(4) 0.066(2) Uani 1 1 d U . . H102 H 0.5020 0.7481 0.2176 0.079 Uiso 1 1 calc R . . C103 C 0.4222(4) 0.7755(5) 0.3116(4) 0.068(2) Uani 1 1 d U . . H103 H 0.4241 0.7258 0.3338 0.081 Uiso 1 1 calc R . . C104 C 0.3733(4) 0.8347(5) 0.3466(4) 0.068(2) Uani 1 1 d U . . H104 H 0.3388 0.8262 0.3926 0.081 Uiso 1 1 calc R . . C105 C 0.3732(5) 0.9055(5) 0.3166(5) 0.092(3) Uani 1 1 d U . . H105 H 0.3408 0.9460 0.3418 0.111 Uiso 1 1 calc R . . C106 C 0.4209(6) 0.9177(5) 0.2490(5) 0.101(3) Uani 1 1 d U . . H106 H 0.4204 0.9673 0.2275 0.121 Uiso 1 1 calc R . . C201 C 0.7361(4) 0.9497(4) 0.1470(3) 0.0534(18) Uani 1 1 d . . . H201 H 0.7056 0.9659 0.1902 0.064 Uiso 1 1 calc R . . C202 C 0.8199(4) 0.9343(3) 0.1198(3) 0.0504(17) Uani 1 1 d . . . H202 H 0.8471 0.9404 0.1443 0.060 Uiso 1 1 calc R . . C203 C 0.8652(4) 0.9105(3) 0.0584(3) 0.0440(16) Uani 1 1 d . . . H203 H 0.9235 0.8995 0.0406 0.053 Uiso 1 1 calc R . . C204 C 0.8263(4) 0.9026(3) 0.0230(3) 0.0467(17) Uani 1 1 d . . . H204 H 0.8579 0.8862 -0.0200 0.056 Uiso 1 1 calc R . . C205 C 0.7424(4) 0.9175(4) 0.0479(4) 0.0522(18) Uani 1 1 d . . . H205 H 0.7161 0.9117 0.0224 0.063 Uiso 1 1 calc R . . C206 C 0.6964(4) 0.9415(4) 0.1110(4) 0.061(2) Uani 1 1 d . . . H206 H 0.6382 0.9520 0.1291 0.074 Uiso 1 1 calc R . . C301 C 0.8597(4) 0.1111(3) 0.4110(3) 0.0445(16) Uani 1 1 d . . . H301 H 0.8659 0.0793 0.4527 0.053 Uiso 1 1 calc R . . C302 C 0.9080(4) 0.1540(3) 0.3754(3) 0.0406(15) Uani 1 1 d . . . H302 H 0.9488 0.1510 0.3914 0.049 Uiso 1 1 calc R . . C303 C 0.8979(4) 0.2010(4) 0.3170(3) 0.0479(17) Uani 1 1 d . . . H303 H 0.9311 0.2314 0.2926 0.057 Uiso 1 1 calc R . . C304 C 0.8396(4) 0.2050(4) 0.2924(3) 0.0482(17) Uani 1 1 d . . . H304 H 0.8325 0.2383 0.2516 0.058 Uiso 1 1 calc R . . C305 C 0.7923(4) 0.1610(3) 0.3270(3) 0.0451(16) Uani 1 1 d . . . H305 H 0.7530 0.1631 0.3098 0.054 Uiso 1 1 calc R . . C306 C 0.8014(4) 0.1134(3) 0.3871(3) 0.0474(17) Uani 1 1 d . . . H306 H 0.7684 0.0828 0.4116 0.057 Uiso 1 1 calc R . . C401 C 0.7736(4) 0.8581(4) 0.8696(3) 0.0564(19) Uani 1 1 d . . . H401 H 0.7316 0.8387 0.9014 0.068 Uiso 1 1 calc R . . C402 C 0.8512(4) 0.8267(4) 0.8752(3) 0.0520(18) Uani 1 1 d . . . H402 H 0.8636 0.7854 0.9102 0.062 Uiso 1 1 calc R . . C403 C 0.9114(4) 0.8559(4) 0.8293(3) 0.0504(17) Uani 1 1 d . . . H403 H 0.9657 0.8344 0.8325 0.060 Uiso 1 1 calc R . . C404 C 0.8934(4) 0.9152(4) 0.7794(3) 0.0515(18) Uani 1 1 d . . . H404 H 0.9350 0.9353 0.7483 0.062 Uiso 1 1 calc R . . C405 C 0.8161(5) 0.9463(4) 0.7734(3) 0.0529(18) Uani 1 1 d . . . H405 H 0.8042 0.9878 0.7383 0.063 Uiso 1 1 calc R . . C406 C 0.7555(4) 0.9177(4) 0.8182(3) 0.0571(19) Uani 1 1 d . . . H406 H 0.7018 0.9386 0.8139 0.068 Uiso 1 1 calc R . . C501 C 0.3709(3) 0.1196(4) 0.2621(3) 0.106(3) Uani 1 1 d GU . . H501 H 0.3139 0.1253 0.2842 0.127 Uiso 1 1 calc R . . C502 C 0.3989(3) 0.1490(3) 0.1934(3) 0.092(3) Uani 1 1 d GU . . H502 H 0.3611 0.1749 0.1684 0.110 Uiso 1 1 calc R . . C503 C 0.4822(3) 0.1407(3) 0.1611(3) 0.092(3) Uani 1 1 d GU . . H503 H 0.5013 0.1608 0.1141 0.111 Uiso 1 1 calc R . . C504 C 0.5375(3) 0.1029(4) 0.1976(3) 0.105(3) Uani 1 1 d GU . . H504 H 0.5944 0.0972 0.1756 0.126 Uiso 1 1 calc R . . C505 C 0.5095(4) 0.0734(4) 0.2664(3) 0.123(3) Uani 1 1 d GU . . H505 H 0.5472 0.0475 0.2914 0.147 Uiso 1 1 calc R . . C506 C 0.4261(4) 0.0817(4) 0.2987(3) 0.131(4) Uani 1 1 d GU . . H506 H 0.4070 0.0616 0.3457 0.157 Uiso 1 1 calc R . . C601 C 0.3411(3) 0.8024(2) 0.7849(3) 0.073(2) Uani 1 1 d GU . . H601 H 0.3444 0.8482 0.7852 0.088 Uiso 1 1 calc R . . C602 C 0.2760(3) 0.7800(3) 0.8332(2) 0.069(2) Uani 1 1 d GU . . H602 H 0.2349 0.8106 0.8666 0.082 Uiso 1 1 calc R . . C603 C 0.2712(2) 0.7130(3) 0.8328(2) 0.065(2) Uani 1 1 d GU . . H603 H 0.2267 0.6977 0.8658 0.078 Uiso 1 1 calc R . . C604 C 0.3314(3) 0.6683(2) 0.7840(2) 0.069(2) Uani 1 1 d GU . . H604 H 0.3281 0.6225 0.7837 0.083 Uiso 1 1 calc R . . C605 C 0.3965(3) 0.6907(3) 0.7357(2) 0.072(2) Uani 1 1 d GU . . H605 H 0.4376 0.6601 0.7024 0.086 Uiso 1 1 calc R . . C606 C 0.4013(3) 0.7577(3) 0.7362(2) 0.073(2) Uani 1 1 d GU . . H606 H 0.4458 0.7730 0.7031 0.088 Uiso 1 1 calc R . . C701 C 0.7214(3) 0.7416(3) 0.0407(2) 0.081(2) Uani 1 1 d GU . . H701 H 0.7529 0.7485 0.0607 0.097 Uiso 1 1 calc R . . C702 C 0.7562(2) 0.6818(3) 0.0054(3) 0.078(2) Uani 1 1 d GU . . H702 H 0.8115 0.6480 0.0012 0.094 Uiso 1 1 calc R . . C703 C 0.7100(3) 0.6717(2) -0.0238(2) 0.068(2) Uani 1 1 d GU . . H703 H 0.7338 0.6308 -0.0480 0.082 Uiso 1 1 calc R . . C704 C 0.6291(3) 0.7212(3) -0.0178(3) 0.072(2) Uani 1 1 d GU . . H704 H 0.5976 0.7143 -0.0378 0.086 Uiso 1 1 calc R . . C705 C 0.5943(2) 0.7809(3) 0.0175(3) 0.086(3) Uani 1 1 d GU . . H705 H 0.5390 0.8148 0.0217 0.103 Uiso 1 1 calc R . . C706 C 0.6404(3) 0.7911(3) 0.0467(3) 0.085(2) Uani 1 1 d GU . . H706 H 0.6167 0.8319 0.0709 0.103 Uiso 1 1 calc R . . C801 C 0.4228(10) 0.0464(9) 0.5353(8) 0.176(5) Uani 1 1 d DU . . H801 H 0.3694 0.0765 0.5607 0.212 Uiso 1 1 calc R . . C802 C 0.4929(11) 0.0503(9) 0.5368(8) 0.189(5) Uani 1 1 d DU . . H802 H 0.4886 0.0854 0.5600 0.227 Uiso 1 1 calc R . . C803 C 0.5707(10) 0.0008(10) 0.5029(9) 0.198(6) Uani 1 1 d DU . . H803 H 0.6196 -0.0004 0.5061 0.238 Uiso 1 1 calc R . . C901 C 0.4540(4) 0.9735(4) 0.9838(3) 0.0574(19) Uani 1 1 d D . . H901 H 0.4226 0.9554 0.9732 0.069 Uiso 1 1 calc R . . C902 C 0.5284(4) 0.9788(4) 0.9373(4) 0.065(2) Uani 1 1 d D . . H902 H 0.5486 0.9644 0.8940 0.078 Uiso 1 1 calc R . . C903 C 0.5740(4) 1.0050(4) 0.9534(3) 0.069(2) Uani 1 1 d D . . H903 H 0.6253 1.0082 0.9208 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02078(10) 0.01891(10) 0.01314(10) 0.00239(7) -0.00466(8) -0.01121(8) U2 0.02470(11) 0.02635(11) 0.01405(10) 0.00156(8) -0.00496(8) -0.01551(9) K1 0.0337(6) 0.0378(7) 0.0208(6) 0.0079(5) -0.0099(5) -0.0246(6) K2 0.0366(7) 0.0397(7) 0.0175(6) 0.0047(5) -0.0079(5) -0.0241(6) O1 0.0250(18) 0.0237(18) 0.0135(17) 0.0030(14) -0.0058(14) -0.0142(15) O2 0.0294(19) 0.0231(18) 0.0183(19) 0.0071(14) -0.0120(15) -0.0142(15) O3 0.0187(17) 0.0219(18) 0.0190(19) 0.0020(14) -0.0009(14) -0.0088(14) O4 0.0234(17) 0.0218(18) 0.0173(18) 0.0046(14) -0.0058(15) -0.0143(15) O5 0.0268(18) 0.0267(19) 0.0140(18) 0.0066(14) -0.0048(15) -0.0178(16) O6 0.035(2) 0.031(2) 0.0176(19) 0.0105(16) -0.0073(16) -0.0230(17) O7 0.031(2) 0.040(2) 0.0157(19) -0.0010(16) -0.0038(15) -0.0240(17) O8 0.0264(19) 0.036(2) 0.0137(18) -0.0012(15) -0.0030(15) -0.0147(16) O9 0.0277(19) 0.0255(19) 0.0175(19) 0.0027(15) -0.0039(15) -0.0144(16) O10 0.0284(19) 0.0269(19) 0.0150(18) 0.0013(14) -0.0069(15) -0.0156(16) O11 0.035(2) 0.039(2) 0.0130(18) 0.0037(15) -0.0047(15) -0.0279(17) O12 0.031(2) 0.035(2) 0.0206(19) -0.0003(16) -0.0074(16) -0.0223(17) N1 0.021(2) 0.019(2) 0.011(2) 0.0000(16) -0.0027(16) -0.0104(17) N2 0.023(2) 0.018(2) 0.015(2) 0.0004(16) -0.0040(17) -0.0100(17) N3 0.024(2) 0.021(2) 0.017(2) -0.0006(17) -0.0067(18) -0.0110(18) N4 0.028(2) 0.028(2) 0.014(2) 0.0021(18) -0.0066(18) -0.0165(19) N5 0.027(2) 0.031(2) 0.017(2) 0.0004(18) -0.0051(18) -0.0178(19) N6 0.025(2) 0.027(2) 0.016(2) 0.0007(18) -0.0042(18) -0.0134(19) C1 0.031(3) 0.020(2) 0.016(3) 0.000(2) -0.006(2) -0.015(2) C2 0.027(3) 0.019(2) 0.020(3) 0.003(2) -0.008(2) -0.012(2) C3 0.026(3) 0.020(2) 0.016(3) 0.001(2) -0.004(2) -0.013(2) C4 0.025(3) 0.025(3) 0.013(2) 0.003(2) -0.008(2) -0.013(2) C5 0.022(3) 0.024(3) 0.016(3) -0.001(2) -0.003(2) -0.012(2) C6 0.025(3) 0.026(3) 0.016(3) -0.001(2) -0.008(2) -0.013(2) C7 0.023(2) 0.026(3) 0.013(2) 0.000(2) -0.005(2) -0.014(2) C8 0.024(3) 0.022(3) 0.011(2) -0.0009(19) -0.002(2) -0.014(2) C9 0.030(3) 0.019(2) 0.011(2) 0.0044(19) -0.006(2) -0.014(2) C10 0.028(3) 0.017(2) 0.013(3) 0.0062(19) -0.004(2) -0.013(2) C11 0.025(3) 0.023(3) 0.020(3) -0.004(2) 0.000(2) -0.011(2) C12 0.034(3) 0.025(3) 0.014(3) -0.001(2) -0.001(2) -0.017(2) C13 0.028(3) 0.022(3) 0.021(3) 0.000(2) -0.008(2) -0.014(2) C14 0.026(3) 0.024(3) 0.017(3) 0.004(2) -0.005(2) -0.008(2) C15 0.025(3) 0.037(3) 0.019(3) -0.003(2) -0.005(2) -0.014(2) C16 0.032(3) 0.032(3) 0.033(3) -0.004(3) 0.003(3) -0.018(3) C17 0.042(4) 0.071(5) 0.033(4) 0.003(3) -0.017(3) -0.033(3) C18 0.028(3) 0.037(3) 0.026(3) -0.005(2) -0.003(2) -0.016(3) C19 0.040(3) 0.041(3) 0.025(3) -0.011(3) -0.008(3) -0.021(3) C20 0.021(2) 0.018(2) 0.018(3) 0.003(2) -0.007(2) -0.008(2) C21 0.021(2) 0.022(3) 0.019(3) 0.001(2) -0.005(2) -0.011(2) C22 0.022(2) 0.021(2) 0.016(3) 0.003(2) -0.004(2) -0.010(2) C23 0.030(3) 0.021(3) 0.018(3) 0.001(2) -0.009(2) -0.013(2) C24 0.035(3) 0.026(3) 0.020(3) 0.001(2) -0.013(2) -0.015(2) C25 0.029(3) 0.026(3) 0.020(3) 0.002(2) -0.011(2) -0.010(2) C26 0.025(3) 0.015(2) 0.016(3) 0.0035(19) -0.003(2) -0.009(2) C27 0.044(3) 0.025(3) 0.022(3) 0.004(2) -0.016(3) -0.021(2) C28 0.038(3) 0.026(3) 0.031(3) 0.005(2) -0.017(3) -0.019(3) C29 0.039(3) 0.048(4) 0.023(3) 0.004(3) -0.009(3) -0.030(3) C30 0.053(4) 0.037(3) 0.040(4) 0.009(3) -0.022(3) -0.029(3) C31 0.054(4) 0.042(4) 0.048(4) 0.003(3) -0.027(3) -0.030(3) C32 0.049(3) 0.025(3) 0.026(3) 0.006(2) -0.019(3) -0.016(3) C33 0.022(2) 0.023(3) 0.017(3) 0.002(2) -0.004(2) -0.012(2) C34 0.023(3) 0.019(2) 0.018(3) -0.003(2) -0.006(2) -0.008(2) C35 0.023(3) 0.019(2) 0.020(3) -0.007(2) -0.006(2) -0.007(2) C36 0.032(3) 0.022(3) 0.020(3) -0.001(2) -0.010(2) -0.013(2) C37 0.029(3) 0.027(3) 0.026(3) -0.003(2) -0.014(2) -0.009(2) C38 0.024(3) 0.030(3) 0.028(3) -0.007(2) -0.010(2) -0.012(2) C39 0.030(3) 0.027(3) 0.017(3) -0.002(2) -0.004(2) -0.017(2) C40 0.029(3) 0.024(3) 0.019(3) 0.000(2) -0.004(2) -0.009(2) C41 0.034(3) 0.023(3) 0.018(3) 0.004(2) -0.006(2) -0.014(2) C42 0.041(3) 0.029(3) 0.038(4) -0.001(3) -0.015(3) -0.014(3) C43 0.052(4) 0.039(3) 0.027(3) 0.006(3) -0.004(3) -0.026(3) C44 0.033(3) 0.029(3) 0.024(3) 0.002(2) -0.007(2) -0.017(2) C45 0.030(3) 0.032(3) 0.035(3) -0.003(3) -0.011(3) -0.013(2) C46 0.025(3) 0.016(2) 0.021(3) -0.002(2) -0.004(2) -0.007(2) C47 0.027(3) 0.032(3) 0.019(3) 0.002(2) -0.009(2) -0.016(2) C48 0.024(3) 0.033(3) 0.019(3) -0.002(2) 0.000(2) -0.017(2) C49 0.029(3) 0.034(3) 0.013(3) 0.002(2) -0.006(2) -0.017(2) C50 0.030(3) 0.037(3) 0.014(3) 0.006(2) -0.008(2) -0.018(2) C51 0.032(3) 0.028(3) 0.021(3) 0.006(2) -0.007(2) -0.019(2) C52 0.033(3) 0.030(3) 0.015(3) 0.006(2) -0.006(2) -0.021(2) C53 0.027(3) 0.030(3) 0.019(3) -0.004(2) -0.004(2) -0.017(2) C54 0.032(3) 0.028(3) 0.015(3) -0.005(2) -0.002(2) -0.016(2) C55 0.029(3) 0.027(3) 0.020(3) -0.004(2) -0.007(2) -0.015(2) C56 0.040(3) 0.035(3) 0.020(3) -0.006(2) -0.006(2) -0.023(3) C57 0.044(3) 0.027(3) 0.018(3) -0.001(2) -0.011(3) -0.013(3) C58 0.034(3) 0.035(3) 0.022(3) -0.009(2) -0.012(2) -0.010(2) C59 0.026(3) 0.033(3) 0.024(3) -0.011(2) -0.002(2) -0.013(2) C60 0.044(3) 0.038(3) 0.018(3) 0.005(2) -0.010(2) -0.030(3) C61 0.041(3) 0.041(3) 0.015(3) 0.002(2) -0.005(2) -0.028(3) C62 0.043(3) 0.039(3) 0.024(3) -0.007(3) -0.004(3) -0.025(3) C63 0.039(3) 0.041(3) 0.027(3) -0.005(3) -0.004(3) -0.023(3) C64 0.047(4) 0.048(4) 0.022(3) -0.002(3) -0.004(3) -0.029(3) C65 0.038(3) 0.054(4) 0.028(3) -0.011(3) -0.013(3) -0.009(3) C66 0.031(3) 0.032(3) 0.017(3) -0.006(2) -0.002(2) -0.016(2) C67 0.029(3) 0.026(3) 0.025(3) -0.002(2) -0.008(2) -0.017(2) C68 0.026(3) 0.028(3) 0.024(3) -0.002(2) -0.008(2) -0.013(2) C69 0.027(3) 0.032(3) 0.027(3) -0.007(2) -0.008(2) -0.011(2) C70 0.033(3) 0.028(3) 0.031(3) -0.001(2) -0.014(3) -0.014(2) C71 0.027(3) 0.036(3) 0.031(3) -0.012(3) 0.000(2) -0.017(3) C72 0.034(3) 0.038(3) 0.024(3) -0.003(2) -0.004(2) -0.023(3) C73 0.029(3) 0.030(3) 0.026(3) 0.000(2) -0.012(2) -0.008(2) C74 0.036(3) 0.033(3) 0.017(3) 0.000(2) -0.007(2) -0.012(3) C75 0.035(3) 0.054(4) 0.034(4) 0.013(3) -0.012(3) -0.021(3) C76 0.042(4) 0.044(4) 0.042(4) -0.004(3) -0.009(3) -0.021(3) C77 0.058(4) 0.045(4) 0.023(3) 0.004(3) -0.011(3) -0.019(3) C78 0.037(3) 0.040(4) 0.046(4) -0.012(3) -0.002(3) -0.016(3) C79 0.028(3) 0.033(3) 0.018(3) 0.005(2) -0.009(2) -0.014(2) C80 0.030(3) 0.035(3) 0.019(3) 0.004(2) -0.008(2) -0.022(2) C81 0.029(3) 0.033(3) 0.027(3) -0.001(2) -0.010(2) -0.020(2) C82 0.028(3) 0.023(3) 0.026(3) -0.002(2) -0.009(2) -0.016(2) C83 0.031(3) 0.036(3) 0.025(3) -0.004(2) -0.001(2) -0.024(3) C84 0.027(3) 0.034(3) 0.035(3) -0.002(3) -0.011(3) -0.017(2) C85 0.029(3) 0.032(3) 0.029(3) 0.005(2) -0.012(2) -0.020(2) C86 0.037(3) 0.028(3) 0.028(3) -0.005(2) -0.009(3) -0.017(2) C87 0.035(3) 0.030(3) 0.027(3) 0.000(2) -0.001(2) -0.020(3) C88 0.035(3) 0.030(3) 0.044(4) -0.010(3) 0.002(3) -0.020(3) C89 0.061(4) 0.047(4) 0.039(4) 0.012(3) -0.014(3) -0.035(3) C90 0.041(3) 0.033(3) 0.034(3) -0.004(3) -0.001(3) -0.023(3) C91 0.041(3) 0.035(3) 0.040(4) -0.001(3) -0.016(3) -0.015(3) C92 0.025(3) 0.024(3) 0.020(3) -0.003(2) -0.003(2) -0.010(2) C93 0.070(5) 0.041(4) 0.036(4) 0.005(3) -0.022(3) -0.028(3) C94 0.063(5) 0.046(4) 0.057(5) 0.012(3) -0.030(4) -0.035(4) C95 0.044(4) 0.044(4) 0.071(6) 0.000(4) 0.005(4) -0.014(3) C96 0.090(6) 0.050(4) 0.037(4) -0.004(3) -0.012(4) -0.041(4) C97 0.075(5) 0.055(4) 0.035(4) 0.017(3) -0.027(4) -0.046(4) C98 0.054(4) 0.042(4) 0.039(4) 0.012(3) -0.014(3) -0.028(3) C101 0.077(5) 0.094(5) 0.050(4) 0.007(4) -0.011(4) -0.006(4) C102 0.052(4) 0.103(5) 0.051(4) -0.002(4) -0.028(3) -0.032(4) C103 0.057(4) 0.106(5) 0.059(4) 0.003(4) -0.030(3) -0.046(4) C104 0.052(4) 0.098(5) 0.051(4) 0.004(4) -0.022(3) -0.031(4) C105 0.079(4) 0.088(4) 0.074(4) -0.004(3) -0.020(3) -0.011(3) C106 0.094(4) 0.087(4) 0.074(4) 0.003(3) -0.018(3) -0.011(3) C201 0.061(5) 0.057(4) 0.031(4) 0.009(3) -0.009(3) -0.029(4) C202 0.066(5) 0.043(4) 0.042(4) 0.007(3) -0.017(4) -0.029(4) C203 0.054(4) 0.035(3) 0.042(4) 0.009(3) -0.019(3) -0.023(3) C204 0.059(4) 0.030(3) 0.052(4) 0.006(3) -0.025(4) -0.019(3) C205 0.071(5) 0.046(4) 0.055(5) 0.007(3) -0.032(4) -0.033(4) C206 0.053(4) 0.059(5) 0.065(5) 0.017(4) -0.016(4) -0.036(4) C301 0.055(4) 0.032(3) 0.040(4) -0.004(3) -0.017(3) -0.011(3) C302 0.039(3) 0.037(3) 0.055(4) -0.013(3) -0.023(3) -0.012(3) C303 0.053(4) 0.046(4) 0.047(4) -0.008(3) -0.009(3) -0.027(3) C304 0.058(4) 0.048(4) 0.036(4) -0.004(3) -0.017(3) -0.018(3) C305 0.039(3) 0.049(4) 0.054(4) -0.021(3) -0.020(3) -0.008(3) C306 0.041(4) 0.042(4) 0.059(5) -0.020(3) 0.001(3) -0.023(3) C401 0.055(4) 0.078(5) 0.037(4) -0.016(4) 0.011(3) -0.043(4) C402 0.075(5) 0.055(4) 0.033(4) -0.005(3) -0.012(4) -0.036(4) C403 0.062(4) 0.063(5) 0.041(4) -0.015(3) -0.011(3) -0.036(4) C404 0.072(5) 0.059(4) 0.035(4) -0.013(3) 0.000(3) -0.046(4) C405 0.087(5) 0.038(4) 0.042(4) -0.005(3) -0.019(4) -0.032(4) C406 0.058(4) 0.069(5) 0.043(4) -0.018(4) -0.004(4) -0.027(4) C501 0.075(5) 0.123(6) 0.086(6) -0.042(5) -0.010(4) -0.006(5) C502 0.060(4) 0.099(5) 0.102(6) -0.038(5) -0.008(4) -0.019(4) C503 0.062(4) 0.102(6) 0.119(6) -0.029(5) -0.026(4) -0.031(4) C504 0.074(5) 0.119(6) 0.130(7) -0.018(6) -0.043(5) -0.033(5) C505 0.079(5) 0.142(7) 0.124(7) -0.023(6) -0.028(5) -0.025(5) C506 0.089(6) 0.152(7) 0.103(6) -0.044(6) -0.014(5) -0.002(6) C601 0.079(5) 0.097(5) 0.072(5) -0.013(4) -0.040(4) -0.043(4) C602 0.063(4) 0.097(5) 0.058(4) -0.025(4) -0.031(3) -0.020(4) C603 0.062(4) 0.080(5) 0.046(4) -0.010(4) -0.024(3) -0.014(4) C604 0.060(4) 0.078(5) 0.044(4) -0.006(3) -0.012(3) -0.012(4) C605 0.062(4) 0.080(5) 0.052(4) -0.010(4) -0.009(3) -0.017(4) C606 0.061(4) 0.093(5) 0.072(5) -0.011(4) -0.031(4) -0.026(4) C701 0.103(5) 0.094(5) 0.048(4) -0.002(4) -0.020(4) -0.050(4) C702 0.082(5) 0.065(4) 0.078(5) 0.016(4) -0.032(4) -0.031(4) C703 0.072(4) 0.064(4) 0.071(5) -0.018(4) -0.005(4) -0.039(4) C704 0.053(4) 0.085(5) 0.084(5) -0.015(4) -0.007(4) -0.044(4) C705 0.046(4) 0.083(5) 0.106(6) -0.017(4) 0.006(4) -0.033(4) C706 0.080(5) 0.089(5) 0.076(5) -0.031(4) 0.024(4) -0.055(4) C801 0.171(6) 0.168(6) 0.189(6) -0.037(4) -0.053(4) -0.060(4) C802 0.182(6) 0.183(6) 0.198(6) -0.039(4) -0.049(4) -0.069(4) C803 0.154(9) 0.215(10) 0.210(10) -0.038(8) -0.043(8) -0.067(8) C901 0.055(4) 0.056(5) 0.057(5) -0.011(4) -0.011(4) -0.023(4) C902 0.079(6) 0.072(5) 0.047(5) -0.009(4) -0.006(4) -0.044(5) C903 0.065(5) 0.062(5) 0.068(5) -0.018(4) 0.011(4) -0.038(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 U1 O2 2.173(3) . ? U1 O3 2.176(3) . ? U1 O1 2.187(3) . ? U1 O4 2.360(3) . ? U1 O5 2.421(3) . ? U1 N1 2.630(4) . ? U1 N3 2.810(4) . ? U1 C46 2.822(5) . ? U1 N2 2.896(4) . ? U2 O9 2.141(3) . ? U2 O8 2.172(3) . ? U2 O7 2.248(3) . ? U2 O11 2.398(3) . ? U2 O10 2.410(3) . ? U2 N4 2.703(4) . ? U2 N5 2.745(4) . ? U2 N6 2.767(4) . ? U2 C92 2.830(5) . ? K1 O4 2.715(3) . ? K1 O6 2.716(4) . ? K1 O12 2.751(3) . ? K1 O10 2.766(3) . ? K1 C46 3.107(5) . ? K1 C92 3.127(5) . ? K1 K2 3.8774(15) . ? K2 O6 2.516(3) . ? K2 O12 2.579(3) . ? K2 O11 2.639(4) 2_566 ? K2 O12 2.813(3) 2_566 ? K2 C92 3.091(5) 2_566 ? K2 C98 3.178(6) . ? K2 C93 3.449(6) . ? K2 K2 3.906(2) 2_566 ? O1 C9 1.329(5) . ? O2 C22 1.339(5) . ? O3 C35 1.346(5) . ? O4 C46 1.328(6) . ? O5 C46 1.283(6) . ? O6 C46 1.255(6) . ? O7 C55 1.339(6) . ? O8 C68 1.338(6) . ? O9 C81 1.341(6) . ? O10 C92 1.294(6) . ? O11 C92 1.311(6) . ? O11 K2 2.639(4) 2_566 ? O12 C92 1.258(6) . ? O12 K2 2.813(3) 2_566 ? N1 C1 1.487(6) . ? N1 C6 1.491(6) . ? N1 C7 1.500(6) . ? N2 C3 1.470(6) . ? N2 C2 1.471(6) . ? N2 C20 1.490(6) . ? N3 C4 1.480(5) . ? N3 C5 1.486(6) . ? N3 C33 1.496(6) . ? N4 C47 1.484(6) . ? N4 C53 1.494(6) . ? N4 C52 1.498(6) . ? N5 C66 1.483(6) . ? N5 C49 1.490(6) . ? N5 C48 1.490(6) . ? N6 C51 1.483(6) . ? N6 C50 1.498(6) . ? N6 C79 1.502(6) . ? C1 C2 1.521(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.529(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.508(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.392(7) . ? C8 C9 1.412(6) . ? C9 C10 1.405(7) . ? C10 C11 1.384(7) . ? C10 C14 1.517(7) . ? C11 C12 1.395(7) . ? C11 H11A 0.9500 . ? C12 C13 1.376(7) . ? C12 C19 1.517(7) . ? C13 H13A 0.9500 . ? C14 C15 1.537(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.527(7) . ? C15 C18 1.528(7) . ? C15 C16 1.533(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.507(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.393(6) . ? C21 C22 1.399(6) . ? C22 C23 1.404(7) . ? C23 C24 1.391(6) . ? C23 C27 1.508(6) . ? C24 C25 1.391(7) . ? C24 H24A 0.9500 . ? C25 C26 1.376(7) . ? C25 C32 1.519(6) . ? C26 H26A 0.9500 . ? C27 C28 1.556(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C30 1.521(7) . ? C28 C29 1.531(7) . ? C28 C31 1.543(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.498(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.375(6) . ? C34 C35 1.404(7) . ? C35 C36 1.400(6) . ? C36 C37 1.390(7) . ? C36 C40 1.514(7) . ? C37 C38 1.387(7) . ? C37 H37A 0.9500 . ? C38 C39 1.386(7) . ? C38 C45 1.511(7) . ? C39 H39A 0.9500 . ? C40 C41 1.543(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.520(7) . ? C41 C44 1.523(7) . ? C41 C43 1.531(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C48 1.517(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.499(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.514(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.507(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C59 1.383(7) . ? C54 C55 1.395(7) . ? C55 C56 1.412(7) . ? C56 C57 1.390(7) . ? C56 C60 1.509(7) . ? C57 C58 1.383(7) . ? C57 H57A 0.9500 . ? C58 C59 1.381(7) . ? C58 C65 1.508(7) . ? C59 H59A 0.9500 . ? C60 C61 1.547(7) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C64 1.526(7) . ? C61 C63 1.537(7) . ? C61 C62 1.537(7) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.515(7) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C72 1.371(7) . ? C67 C68 1.414(7) . ? C68 C69 1.401(7) . ? C69 C70 1.376(7) . ? C69 C73 1.518(7) . ? C70 C71 1.412(7) . ? C70 H70A 0.9500 . ? C71 C72 1.371(7) . ? C71 C78 1.500(7) . ? C72 H72A 0.9500 . ? C73 C74 1.540(7) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C77 1.530(7) . ? C74 C76 1.538(8) . ? C74 C75 1.540(7) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.509(7) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C85 1.382(7) . ? C80 C81 1.402(7) . ? C81 C82 1.394(7) . ? C82 C83 1.389(7) . ? C82 C86 1.518(7) . ? C83 C84 1.403(7) . ? C83 H83A 0.9500 . ? C84 C85 1.383(7) . ? C84 C91 1.503(7) . ? C85 H85A 0.9500 . ? C86 C87 1.545(7) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.523(7) . ? C87 C89 1.526(8) . ? C87 C90 1.530(7) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 K2 3.091(5) 2_566 ? C93 C94 1.366(9) . ? C93 C98 1.370(8) . ? C93 H93A 0.9500 . ? C94 C95 1.401(10) . ? C94 H94A 0.9500 . ? C95 C96 1.395(10) . ? C95 H95A 0.9500 . ? C96 C97 1.351(9) . ? C96 H96A 0.9500 . ? C97 C98 1.355(9) . ? C97 H97A 0.9500 . ? C98 H98A 0.9500 . ? C101 C106 1.345(12) . ? C101 C102 1.379(11) . ? C101 H101 0.9500 . ? C102 C103 1.395(10) . ? C102 H102 0.9500 . ? C103 C104 1.368(10) . ? C103 H103 0.9500 . ? C104 C105 1.358(11) . ? C104 H104 0.9500 . ? C105 C106 1.381(11) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C201 C202 1.366(9) . ? C201 C206 1.385(9) . ? C201 H201 0.9500 . ? C202 C203 1.360(8) . ? C202 H202 0.9500 . ? C203 C204 1.355(8) . ? C203 H203 0.9500 . ? C204 C205 1.370(9) . ? C204 H204 0.9500 . ? C205 C206 1.393(9) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C301 C302 1.361(8) . ? C301 C306 1.389(8) . ? C301 H301 0.9500 . ? C302 C303 1.353(8) . ? C302 H302 0.9500 . ? C303 C304 1.384(8) . ? C303 H303 0.9500 . ? C304 C305 1.361(8) . ? C304 H304 0.9500 . ? C305 C306 1.383(9) . ? C305 H305 0.9500 . ? C306 H306 0.9500 . ? C401 C402 1.367(9) . ? C401 C406 1.383(9) . ? C401 H401 0.9500 . ? C402 C403 1.380(9) . ? C402 H402 0.9500 . ? C403 C404 1.359(9) . ? C403 H403 0.9500 . ? C404 C405 1.365(9) . ? C404 H404 0.9500 . ? C405 C406 1.374(9) . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? C501 C502 1.3900 . ? C501 C506 1.3900 . ? C501 H501 0.9500 . ? C502 C503 1.3900 . ? C502 H502 0.9500 . ? C503 C504 1.3900 . ? C503 H503 0.9500 . ? C504 C505 1.3900 . ? C504 H504 0.9500 . ? C505 C506 1.3900 . ? C505 H505 0.9500 . ? C506 H506 0.9500 . ? C601 C602 1.3900 . ? C601 C606 1.3900 . ? C601 H601 0.9500 . ? C602 C603 1.3900 . ? C602 H602 0.9500 . ? C603 C604 1.3900 . ? C603 H603 0.9500 . ? C604 C605 1.3900 . ? C604 H604 0.9500 . ? C605 C606 1.3900 . ? C605 H605 0.9500 . ? C606 H606 0.9500 . ? C701 C702 1.3900 . ? C701 C706 1.3900 . ? C701 H701 0.9500 . ? C702 C703 1.3900 . ? C702 H702 0.9500 . ? C703 C704 1.3900 . ? C703 H703 0.9500 . ? C704 C705 1.3900 . ? C704 H704 0.9500 . ? C705 C706 1.3900 . ? C705 H705 0.9500 . ? C706 H706 0.9500 . ? C801 C802 1.382(9) . ? C801 C803 1.387(7) 2_656 ? C801 H801 0.9500 . ? C802 C803 1.406(9) . ? C802 H802 0.9500 . ? C803 C801 1.387(7) 2_656 ? C803 H803 0.9500 . ? C901 C902 1.377(7) . ? C901 C903 1.387(6) 2_677 ? C901 H901 0.9500 . ? C902 C903 1.388(7) . ? C902 H902 0.9500 . ? C903 C901 1.387(6) 2_677 ? C903 H903 0.9500 . ? 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 O3 103.82(12) . . ? O2 U1 O1 97.27(12) . . ? O3 U1 O1 154.40(12) . . ? O2 U1 O4 82.47(11) . . ? O3 U1 O4 84.30(11) . . ? O1 U1 O4 84.24(11) . . ? O2 U1 O5 137.16(11) . . ? O3 U1 O5 78.08(11) . . ? O1 U1 O5 76.60(11) . . ? O4 U1 O5 54.88(11) . . ? O2 U1 N1 132.27(11) . . ? O3 U1 N1 103.24(12) . . ? O1 U1 N1 71.67(11) . . ? O4 U1 N1 138.84(11) . . ? O5 U1 N1 86.68(11) . . ? O2 U1 N3 88.65(11) . . ? O3 U1 N3 67.98(11) . . ? O1 U1 N3 127.56(11) . . ? O4 U1 N3 147.94(11) . . ? O5 U1 N3 128.99(11) . . ? N1 U1 N3 66.51(11) . . ? O2 U1 C46 110.33(13) . . ? O3 U1 C46 79.93(12) . . ? O1 U1 C46 79.24(12) . . ? O4 U1 C46 27.93(12) . . ? O5 U1 C46 26.95(12) . . ? N1 U1 C46 112.61(13) . . ? N3 U1 C46 146.00(12) . . ? O2 U1 N2 70.02(11) . . ? O3 U1 N2 129.42(11) . . ? O1 U1 N2 71.54(11) . . ? O4 U1 N2 139.98(11) . . ? O5 U1 N2 140.94(11) . . ? N1 U1 N2 62.38(11) . . ? N3 U1 N2 61.84(11) . . ? C46 U1 N2 150.44(12) . . ? O9 U2 O8 157.51(12) . . ? O9 U2 O7 81.46(13) . . ? O8 U2 O7 85.75(12) . . ? O9 U2 O11 87.27(12) . . ? O8 U2 O11 94.86(12) . . ? O7 U2 O11 150.06(11) . . ? O9 U2 O10 81.58(12) . . ? O8 U2 O10 81.51(12) . . ? O7 U2 O10 96.25(11) . . ? O11 U2 O10 54.51(11) . . ? O9 U2 N4 103.60(12) . . ? O8 U2 N4 90.86(12) . . ? O7 U2 N4 75.38(12) . . ? O11 U2 N4 134.45(11) . . ? O10 U2 N4 169.14(11) . . ? O9 U2 N5 131.83(12) . . ? O8 U2 N5 69.81(12) . . ? O7 U2 N5 132.82(12) . . ? O11 U2 N5 74.15(11) . . ? O10 U2 N5 118.03(12) . . ? N4 U2 N5 65.68(12) . . ? O9 U2 N6 68.63(12) . . ? O8 U2 N6 133.74(12) . . ? O7 U2 N6 121.88(12) . . ? O11 U2 N6 78.40(11) . . ? O10 U2 N6 125.20(11) . . ? N4 U2 N6 65.63(12) . . ? N5 U2 N6 64.29(12) . . ? O9 U2 C92 82.39(13) . . ? O8 U2 C92 89.21(13) . . ? O7 U2 C92 122.88(13) . . ? O11 U2 C92 27.48(12) . . ? O10 U2 C92 27.09(12) . . ? N4 U2 C92 161.68(13) . . ? N5 U2 C92 97.28(13) . . ? N6 U2 C92 101.69(13) . . ? O4 K1 O6 48.73(9) . . ? O4 K1 O12 126.75(10) . . ? O6 K1 O12 78.30(10) . . ? O4 K1 O10 169.09(10) . . ? O6 K1 O10 123.81(10) . . ? O12 K1 O10 47.97(9) . . ? O4 K1 C46 25.25(11) . . ? O6 K1 C46 23.68(11) . . ? O12 K1 C46 101.52(12) . . ? O10 K1 C46 147.39(12) . . ? O4 K1 C92 149.77(12) . . ? O6 K1 C92 101.05(12) . . ? O12 K1 C92 23.61(11) . . ? O10 K1 C92 24.38(11) . . ? C46 K1 C92 124.62(13) . . ? O4 K1 K2 88.06(7) . . ? O6 K1 K2 40.22(7) . . ? O12 K1 K2 41.60(7) . . ? O10 K1 K2 83.68(7) . . ? C46 K1 K2 63.71(9) . . ? C92 K1 K2 62.05(9) . . ? O6 K2 O12 85.29(11) . . ? O6 K2 O11 104.10(11) . 2_566 ? O12 K2 O11 119.83(11) . 2_566 ? O6 K2 O12 140.37(12) . 2_566 ? O12 K2 O12 87.25(11) . 2_566 ? O11 K2 O12 48.42(10) 2_566 2_566 ? O6 K2 C92 126.27(13) . 2_566 ? O12 K2 C92 106.47(12) . 2_566 ? O11 K2 C92 24.88(11) 2_566 2_566 ? O12 K2 C92 24.01(11) 2_566 2_566 ? O6 K2 C98 148.43(15) . . ? O12 K2 C98 102.61(14) . . ? O11 K2 C98 98.31(14) 2_566 . ? O12 K2 C98 71.07(14) 2_566 . ? C92 K2 C98 81.25(15) 2_566 . ? O6 K2 C93 145.54(14) . . ? O12 K2 C93 123.76(14) . . ? O11 K2 C93 78.68(14) 2_566 . ? O12 K2 C93 66.27(13) 2_566 . ? C92 K2 C93 67.38(14) 2_566 . ? C98 K2 C93 23.41(15) . . ? O6 K2 K1 44.20(8) . . ? O12 K2 K1 45.10(8) . . ? O11 K2 K1 134.41(9) 2_566 . ? O12 K2 K1 129.73(8) 2_566 . ? C92 K2 K1 140.63(10) 2_566 . ? C98 K2 K1 125.45(13) . . ? C93 K2 K1 146.82(12) . . ? O6 K2 K2 120.03(10) . 2_566 ? O12 K2 K2 45.99(8) . 2_566 ? O11 K2 K2 81.40(8) 2_566 2_566 ? O12 K2 K2 41.26(7) 2_566 2_566 ? C92 K2 K2 61.93(10) 2_566 2_566 ? C98 K2 K2 84.87(12) . 2_566 ? C93 K2 K2 94.42(12) . 2_566 ? K1 K2 K2 89.67(4) . 2_566 ? C9 O1 U1 141.3(3) . . ? C22 O2 U1 150.6(3) . . ? C35 O3 U1 147.8(3) . . ? C46 O4 U1 95.7(3) . . ? C46 O4 K1 94.1(3) . . ? U1 O4 K1 165.73(14) . . ? C46 O5 U1 94.2(3) . . ? C46 O6 K2 165.5(3) . . ? C46 O6 K1 95.9(3) . . ? K2 O6 K1 95.58(11) . . ? C55 O7 U2 127.5(3) . . ? C68 O8 U2 152.3(3) . . ? C81 O9 U2 155.0(3) . . ? C92 O10 U2 94.9(3) . . ? C92 O10 K1 93.7(3) . . ? U2 O10 K1 171.24(14) . . ? C92 O11 U2 94.9(3) . . ? C92 O11 K2 97.2(3) . 2_566 ? U2 O11 K2 163.98(15) . 2_566 ? C92 O12 K2 143.5(3) . . ? C92 O12 K1 95.2(3) . . ? K2 O12 K1 93.30(11) . . ? C92 O12 K2 90.5(3) . 2_566 ? K2 O12 K2 92.75(11) . 2_566 ? K1 O12 K2 161.08(15) . 2_566 ? C1 N1 C6 111.5(3) . . ? C1 N1 C7 109.7(4) . . ? C6 N1 C7 109.4(3) . . ? C1 N1 U1 122.0(3) . . ? C6 N1 U1 100.5(3) . . ? C7 N1 U1 102.7(3) . . ? C3 N2 C2 109.7(4) . . ? C3 N2 C20 110.5(4) . . ? C2 N2 C20 108.4(4) . . ? C3 N2 U1 116.3(3) . . ? C2 N2 U1 105.5(3) . . ? C20 N2 U1 106.1(3) . . ? C4 N3 C5 112.7(4) . . ? C4 N3 C33 104.7(3) . . ? C5 N3 C33 110.2(4) . . ? C4 N3 U1 108.2(3) . . ? C5 N3 U1 108.7(3) . . ? C33 N3 U1 112.4(3) . . ? C47 N4 C53 108.3(4) . . ? C47 N4 C52 111.7(4) . . ? C53 N4 C52 107.5(4) . . ? C47 N4 U2 103.8(3) . . ? C53 N4 U2 111.2(3) . . ? C52 N4 U2 114.2(3) . . ? C66 N5 C49 104.9(4) . . ? C66 N5 C48 111.0(4) . . ? C49 N5 C48 111.4(4) . . ? C66 N5 U2 109.3(3) . . ? C49 N5 U2 106.8(3) . . ? C48 N5 U2 113.0(3) . . ? C51 N6 C50 111.4(4) . . ? C51 N6 C79 110.6(4) . . ? C50 N6 C79 106.1(4) . . ? C51 N6 U2 101.9(3) . . ? C50 N6 U2 115.4(3) . . ? C79 N6 U2 111.6(3) . . ? N1 C1 C2 112.8(4) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 112.2(4) . . ? N2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N2 C3 C4 112.2(4) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 115.3(4) . . ? N3 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? N3 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C6 113.2(4) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.8 . . ? N1 C6 C5 113.6(4) . . ? N1 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? N1 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N1 C7 C8 113.9(4) . . ? N1 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C13 C8 C9 119.1(4) . . ? C13 C8 C7 118.7(4) . . ? C9 C8 C7 122.3(4) . . ? O1 C9 C10 120.1(4) . . ? O1 C9 C8 120.4(4) . . ? C10 C9 C8 119.3(4) . . ? C11 C10 C9 119.0(5) . . ? C11 C10 C14 120.9(4) . . ? C9 C10 C14 120.0(4) . . ? C10 C11 C12 122.5(5) . . ? C10 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C13 C12 C11 117.6(5) . . ? C13 C12 C19 121.0(5) . . ? C11 C12 C19 121.3(5) . . ? C12 C13 C8 122.4(5) . . ? C12 C13 H13A 118.8 . . ? C8 C13 H13A 118.8 . . ? C10 C14 C15 117.4(4) . . ? C10 C14 H14A 107.9 . . ? C15 C14 H14A 107.9 . . ? C10 C14 H14B 107.9 . . ? C15 C14 H14B 107.9 . . ? H14A C14 H14B 107.2 . . ? C17 C15 C18 108.0(4) . . ? C17 C15 C16 109.0(5) . . ? C18 C15 C16 110.0(4) . . ? C17 C15 C14 107.6(4) . . ? C18 C15 C14 111.5(4) . . ? C16 C15 C14 110.7(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C21 115.4(4) . . ? N2 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? N2 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? C26 C21 C22 118.9(5) . . ? C26 C21 C20 121.6(4) . . ? C22 C21 C20 119.3(4) . . ? O2 C22 C21 120.3(4) . . ? O2 C22 C23 119.2(4) . . ? C21 C22 C23 120.5(4) . . ? C24 C23 C22 118.1(4) . . ? C24 C23 C27 122.9(5) . . ? C22 C23 C27 119.0(4) . . ? C25 C24 C23 122.2(5) . . ? C25 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? C26 C25 C24 118.3(4) . . ? C26 C25 C32 120.8(5) . . ? C24 C25 C32 120.9(5) . . ? C25 C26 C21 121.8(4) . . ? C25 C26 H26A 119.1 . . ? C21 C26 H26A 119.1 . . ? C23 C27 C28 116.2(4) . . ? C23 C27 H27A 108.2 . . ? C28 C27 H27A 108.2 . . ? C23 C27 H27B 108.2 . . ? C28 C27 H27B 108.2 . . ? H27A C27 H27B 107.4 . . ? C30 C28 C29 108.8(4) . . ? C30 C28 C31 110.3(4) . . ? C29 C28 C31 109.0(5) . . ? C30 C28 C27 107.0(4) . . ? C29 C28 C27 112.5(4) . . ? C31 C28 C27 109.3(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C32 H32A 109.5 . . ? C25 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C25 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 C34 115.3(4) . . ? N3 C33 H33A 108.5 . . ? C34 C33 H33A 108.5 . . ? N3 C33 H33B 108.5 . . ? C34 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C39 C34 C35 120.2(4) . . ? C39 C34 C33 121.9(4) . . ? C35 C34 C33 117.9(4) . . ? O3 C35 C36 122.7(4) . . ? O3 C35 C34 117.8(4) . . ? C36 C35 C34 119.5(4) . . ? C37 C36 C35 118.0(5) . . ? C37 C36 C40 121.7(4) . . ? C35 C36 C40 120.3(4) . . ? C38 C37 C36 123.4(5) . . ? C38 C37 H37A 118.3 . . ? C36 C37 H37A 118.3 . . ? C39 C38 C37 117.1(4) . . ? C39 C38 C45 120.9(5) . . ? C37 C38 C45 122.0(5) . . ? C34 C39 C38 121.8(5) . . ? C34 C39 H39A 119.1 . . ? C38 C39 H39A 119.1 . . ? C36 C40 C41 116.1(4) . . ? C36 C40 H40A 108.3 . . ? C41 C40 H40A 108.3 . . ? C36 C40 H40B 108.3 . . ? C41 C40 H40B 108.3 . . ? H40A C40 H40B 107.4 . . ? C42 C41 C44 109.4(4) . . ? C42 C41 C43 108.3(4) . . ? C44 C41 C43 109.8(4) . . ? C42 C41 C40 111.2(4) . . ? C44 C41 C40 110.9(4) . . ? C43 C41 C40 107.2(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C38 C45 H45A 109.5 . . ? C38 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C38 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O6 C46 O5 124.6(5) . . ? O6 C46 O4 120.3(4) . . ? O5 C46 O4 115.1(4) . . ? O6 C46 U1 176.6(4) . . ? O5 C46 U1 58.8(2) . . ? O4 C46 U1 56.3(2) . . ? O6 C46 K1 60.4(3) . . ? O5 C46 K1 169.6(3) . . ? O4 C46 K1 60.6(2) . . ? U1 C46 K1 116.22(16) . . ? N4 C47 C48 114.4(4) . . ? N4 C47 H47A 108.7 . . ? C48 C47 H47A 108.7 . . ? N4 C47 H47B 108.7 . . ? C48 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N5 C48 C47 113.6(4) . . ? N5 C48 H48A 108.9 . . ? C47 C48 H48A 108.9 . . ? N5 C48 H48B 108.9 . . ? C47 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? N5 C49 C50 114.0(4) . . ? N5 C49 H49A 108.8 . . ? C50 C49 H49A 108.8 . . ? N5 C49 H49B 108.8 . . ? C50 C49 H49B 108.8 . . ? H49A C49 H49B 107.6 . . ? N6 C50 C49 112.7(4) . . ? N6 C50 H50A 109.1 . . ? C49 C50 H50A 109.1 . . ? N6 C50 H50B 109.1 . . ? C49 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? N6 C51 C52 113.0(4) . . ? N6 C51 H51A 109.0 . . ? C52 C51 H51A 109.0 . . ? N6 C51 H51B 109.0 . . ? C52 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? N4 C52 C51 112.8(4) . . ? N4 C52 H52A 109.0 . . ? C51 C52 H52A 109.0 . . ? N4 C52 H52B 109.0 . . ? C51 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? N4 C53 C54 117.3(4) . . ? N4 C53 H53A 108.0 . . ? C54 C53 H53A 108.0 . . ? N4 C53 H53B 108.0 . . ? C54 C53 H53B 108.0 . . ? H53A C53 H53B 107.2 . . ? C59 C54 C55 119.9(5) . . ? C59 C54 C53 121.7(5) . . ? C55 C54 C53 117.9(4) . . ? O7 C55 C54 119.8(4) . . ? O7 C55 C56 121.0(4) . . ? C54 C55 C56 119.1(5) . . ? C57 C56 C55 117.8(5) . . ? C57 C56 C60 120.8(5) . . ? C55 C56 C60 121.0(5) . . ? C58 C57 C56 123.4(5) . . ? C58 C57 H57A 118.3 . . ? C56 C57 H57A 118.3 . . ? C59 C58 C57 116.9(5) . . ? C59 C58 C65 121.8(5) . . ? C57 C58 C65 121.3(5) . . ? C58 C59 C54 122.2(5) . . ? C58 C59 H59A 118.9 . . ? C54 C59 H59A 118.9 . . ? C56 C60 C61 112.9(4) . . ? C56 C60 H60A 109.0 . . ? C61 C60 H60A 109.0 . . ? C56 C60 H60B 109.0 . . ? C61 C60 H60B 109.0 . . ? H60A C60 H60B 107.8 . . ? C64 C61 C63 108.7(5) . . ? C64 C61 C62 108.2(4) . . ? C63 C61 C62 109.1(4) . . ? C64 C61 C60 108.5(4) . . ? C63 C61 C60 111.4(4) . . ? C62 C61 C60 110.9(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C58 C65 H65A 109.5 . . ? C58 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C58 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N5 C66 C67 116.7(4) . . ? N5 C66 H66A 108.1 . . ? C67 C66 H66A 108.1 . . ? N5 C66 H66B 108.1 . . ? C67 C66 H66B 108.1 . . ? H66A C66 H66B 107.3 . . ? C72 C67 C68 120.7(5) . . ? C72 C67 C66 120.1(5) . . ? C68 C67 C66 118.8(4) . . ? O8 C68 C69 122.4(5) . . ? O8 C68 C67 119.2(4) . . ? C69 C68 C67 118.5(5) . . ? C70 C69 C68 119.0(5) . . ? C70 C69 C73 120.5(5) . . ? C68 C69 C73 120.5(5) . . ? C69 C70 C71 122.8(5) . . ? C69 C70 H70A 118.6 . . ? C71 C70 H70A 118.6 . . ? C72 C71 C70 117.0(5) . . ? C72 C71 C78 122.5(5) . . ? C70 C71 C78 120.4(5) . . ? C71 C72 C67 122.1(5) . . ? C71 C72 H72A 119.0 . . ? C67 C72 H72A 119.0 . . ? C69 C73 C74 115.8(4) . . ? C69 C73 H73A 108.3 . . ? C74 C73 H73A 108.3 . . ? C69 C73 H73B 108.3 . . ? C74 C73 H73B 108.3 . . ? H73A C73 H73B 107.4 . . ? C77 C74 C76 108.6(5) . . ? C77 C74 C73 108.1(5) . . ? C76 C74 C73 111.9(4) . . ? C77 C74 C75 109.2(5) . . ? C76 C74 C75 108.6(5) . . ? C73 C74 C75 110.4(4) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C71 C78 H78A 109.5 . . ? C71 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C71 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N6 C79 C80 116.9(4) . . ? N6 C79 H79A 108.1 . . ? C80 C79 H79A 108.1 . . ? N6 C79 H79B 108.1 . . ? C80 C79 H79B 108.1 . . ? H79A C79 H79B 107.3 . . ? C85 C80 C81 119.2(5) . . ? C85 C80 C79 119.8(4) . . ? C81 C80 C79 120.9(5) . . ? O9 C81 C82 121.2(4) . . ? O9 C81 C80 118.6(5) . . ? C82 C81 C80 120.1(5) . . ? C83 C82 C81 118.8(5) . . ? C83 C82 C86 121.1(5) . . ? C81 C82 C86 120.1(4) . . ? C82 C83 C84 122.4(5) . . ? C82 C83 H83A 118.8 . . ? C84 C83 H83A 118.8 . . ? C85 C84 C83 116.9(5) . . ? C85 C84 C91 121.7(5) . . ? C83 C84 C91 121.3(5) . . ? C80 C85 C84 122.6(5) . . ? C80 C85 H85A 118.7 . . ? C84 C85 H85A 118.7 . . ? C82 C86 C87 115.8(4) . . ? C82 C86 H86A 108.3 . . ? C87 C86 H86A 108.3 . . ? C82 C86 H86B 108.3 . . ? C87 C86 H86B 108.3 . . ? H86A C86 H86B 107.4 . . ? C88 C87 C89 109.0(5) . . ? C88 C87 C90 110.1(5) . . ? C89 C87 C90 109.6(5) . . ? C88 C87 C86 110.9(4) . . ? C89 C87 C86 107.2(5) . . ? C90 C87 C86 109.9(4) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C84 C91 H91A 109.5 . . ? C84 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C84 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? O12 C92 O10 123.0(4) . . ? O12 C92 O11 121.5(4) . . ? O10 C92 O11 115.4(4) . . ? O12 C92 U2 174.9(4) . . ? O10 C92 U2 58.0(2) . . ? O11 C92 U2 57.6(2) . . ? O12 C92 K2 65.5(3) . 2_566 ? O10 C92 K2 165.0(3) . 2_566 ? O11 C92 K2 57.9(2) . 2_566 ? U2 C92 K2 114.74(16) . 2_566 ? O12 C92 K1 61.2(2) . . ? O10 C92 K1 62.0(2) . . ? O11 C92 K1 176.4(3) . . ? U2 C92 K1 119.96(17) . . ? K2 C92 K1 123.92(17) 2_566 . ? C94 C93 C98 120.0(7) . . ? C94 C93 K2 123.2(4) . . ? C98 C93 K2 67.1(3) . . ? C94 C93 H93A 120.0 . . ? C98 C93 H93A 120.0 . . ? K2 C93 H93A 80.9 . . ? C93 C94 C95 119.2(6) . . ? C93 C94 H94A 120.4 . . ? C95 C94 H94A 120.4 . . ? C96 C95 C94 118.8(6) . . ? C96 C95 H95A 120.6 . . ? C94 C95 H95A 120.6 . . ? C97 C96 C95 120.7(7) . . ? C97 C96 H96A 119.6 . . ? C95 C96 H96A 119.6 . . ? C96 C97 C98 119.8(7) . . ? C96 C97 H97A 120.1 . . ? C98 C97 H97A 120.1 . . ? C97 C98 C93 121.4(7) . . ? C97 C98 K2 111.7(4) . . ? C93 C98 K2 89.4(4) . . ? C97 C98 H98A 119.3 . . ? C93 C98 H98A 119.3 . . ? K2 C98 H98A 68.4 . . ? C106 C101 C102 120.6(8) . . ? C106 C101 H101 119.7 . . ? C102 C101 H101 119.7 . . ? C101 C102 C103 118.6(8) . . ? C101 C102 H102 120.7 . . ? C103 C102 H102 120.7 . . ? C104 C103 C102 119.8(8) . . ? C104 C103 H103 120.1 . . ? C102 C103 H103 120.1 . . ? C105 C104 C103 120.8(8) . . ? C105 C104 H104 119.6 . . ? C103 C104 H104 119.6 . . ? C104 C105 C106 119.1(9) . . ? C104 C105 H105 120.4 . . ? C106 C105 H105 120.4 . . ? C101 C106 C105 121.0(10) . . ? C101 C106 H106 119.5 . . ? C105 C106 H106 119.5 . . ? C202 C201 C206 119.1(7) . . ? C202 C201 H201 120.5 . . ? C206 C201 H201 120.5 . . ? C203 C202 C201 121.7(7) . . ? C203 C202 H202 119.2 . . ? C201 C202 H202 119.2 . . ? C204 C203 C202 119.2(7) . . ? C204 C203 H203 120.4 . . ? C202 C203 H203 120.4 . . ? C203 C204 C205 121.5(7) . . ? C203 C204 H204 119.2 . . ? C205 C204 H204 119.2 . . ? C204 C205 C206 119.0(7) . . ? C204 C205 H205 120.5 . . ? C206 C205 H205 120.5 . . ? C201 C206 C205 119.5(7) . . ? C201 C206 H206 120.3 . . ? C205 C206 H206 120.3 . . ? C302 C301 C306 120.6(6) . . ? C302 C301 H301 119.7 . . ? C306 C301 H301 119.7 . . ? C303 C302 C301 120.0(6) . . ? C303 C302 H302 120.0 . . ? C301 C302 H302 120.0 . . ? C302 C303 C304 120.6(6) . . ? C302 C303 H303 119.7 . . ? C304 C303 H303 119.7 . . ? C305 C304 C303 119.8(6) . . ? C305 C304 H304 120.1 . . ? C303 C304 H304 120.1 . . ? C304 C305 C306 120.2(6) . . ? C304 C305 H305 119.9 . . ? C306 C305 H305 119.9 . . ? C305 C306 C301 118.8(6) . . ? C305 C306 H306 120.6 . . ? C301 C306 H306 120.6 . . ? C402 C401 C406 120.6(6) . . ? C402 C401 H401 119.7 . . ? C406 C401 H401 119.7 . . ? C401 C402 C403 119.2(7) . . ? C401 C402 H402 120.4 . . ? C403 C402 H402 120.4 . . ? C404 C403 C402 120.2(7) . . ? C404 C403 H403 119.9 . . ? C402 C403 H403 119.9 . . ? C403 C404 C405 120.7(6) . . ? C403 C404 H404 119.6 . . ? C405 C404 H404 119.6 . . ? C404 C405 C406 119.9(7) . . ? C404 C405 H405 120.0 . . ? C406 C405 H405 120.0 . . ? C405 C406 C401 119.2(7) . . ? C405 C406 H406 120.4 . . ? C401 C406 H406 120.4 . . ? C502 C501 C506 120.0 . . ? C502 C501 H501 120.0 . . ? C506 C501 H501 120.0 . . ? C503 C502 C501 120.0 . . ? C503 C502 H502 120.0 . . ? C501 C502 H502 120.0 . . ? C502 C503 C504 120.0 . . ? C502 C503 H503 120.0 . . ? C504 C503 H503 120.0 . . ? C505 C504 C503 120.0 . . ? C505 C504 H504 120.0 . . ? C503 C504 H504 120.0 . . ? C506 C505 C504 120.0 . . ? C506 C505 H505 120.0 . . ? C504 C505 H505 120.0 . . ? C505 C506 C501 120.0 . . ? C505 C506 H506 120.0 . . ? C501 C506 H506 120.0 . . ? C602 C601 C606 120.0 . . ? C602 C601 H601 120.0 . . ? C606 C601 H601 120.0 . . ? C603 C602 C601 120.0 . . ? C603 C602 H602 120.0 . . ? C601 C602 H602 120.0 . . ? C602 C603 C604 120.0 . . ? C602 C603 H603 120.0 . . ? C604 C603 H603 120.0 . . ? C605 C604 C603 120.0 . . ? C605 C604 H604 120.0 . . ? C603 C604 H604 120.0 . . ? C606 C605 C604 120.0 . . ? C606 C605 H605 120.0 . . ? C604 C605 H605 120.0 . . ? C605 C606 C601 120.0 . . ? C605 C606 H606 120.0 . . ? C601 C606 H606 120.0 . . ? C702 C701 C706 120.0 . . ? C702 C701 H701 120.0 . . ? C706 C701 H701 120.0 . . ? C703 C702 C701 120.0 . . ? C703 C702 H702 120.0 . . ? C701 C702 H702 120.0 . . ? C704 C703 C702 120.0 . . ? C704 C703 H703 120.0 . . ? C702 C703 H703 120.0 . . ? C703 C704 C705 120.0 . . ? C703 C704 H704 120.0 . . ? C705 C704 H704 120.0 . . ? C704 C705 C706 120.0 . . ? C704 C705 H705 120.0 . . ? C706 C705 H705 120.0 . . ? C705 C706 C701 120.0 . . ? C705 C706 H706 120.0 . . ? C701 C706 H706 120.0 . . ? C802 C801 C803 121.0(15) . 2_656 ? C802 C801 H801 119.5 . . ? C803 C801 H801 119.5 2_656 . ? C801 C802 C803 117.9(14) . . ? C801 C802 H802 121.1 . . ? C803 C802 H802 121.1 . . ? C801 C803 C802 121.0(14) 2_656 . ? C801 C803 H803 119.5 2_656 . ? C802 C803 H803 119.5 . . ? C902 C901 C903 118.5(6) . 2_677 ? C902 C901 H901 120.8 . . ? C903 C901 H901 120.8 2_677 . ? C901 C902 C903 120.4(6) . . ? C901 C902 H902 119.8 . . ? C903 C902 H902 119.8 . . ? C901 C903 C902 121.1(6) 2_677 . ? C901 C903 H903 119.4 2_677 . ? C902 C903 H903 119.4 . . ? 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 O4 K1 K2 O6 10.86(14) . . . . ? O12 K1 K2 O6 -149.16(17) . . . . ? O10 K1 K2 O6 -176.29(14) . . . . ? C46 K1 K2 O6 3.93(16) . . . . ? C92 K1 K2 O6 -164.42(16) . . . . ? O4 K1 K2 O12 160.02(14) . . . . ? O6 K1 K2 O12 149.16(17) . . . . ? O10 K1 K2 O12 -27.13(13) . . . . ? C46 K1 K2 O12 153.09(15) . . . . ? C92 K1 K2 O12 -15.26(15) . . . . ? O4 K1 K2 O11 69.63(13) . . . 2_566 ? O6 K1 K2 O11 58.78(16) . . . 2_566 ? O12 K1 K2 O11 -90.38(16) . . . 2_566 ? O10 K1 K2 O11 -117.51(13) . . . 2_566 ? C46 K1 K2 O11 62.71(15) . . . 2_566 ? C92 K1 K2 O11 -105.64(15) . . . 2_566 ? O4 K1 K2 O12 136.44(12) . . . 2_566 ? O6 K1 K2 O12 125.58(16) . . . 2_566 ? O12 K1 K2 O12 -23.6(2) . . . 2_566 ? O10 K1 K2 O12 -50.71(13) . . . 2_566 ? C46 K1 K2 O12 129.51(14) . . . 2_566 ? C92 K1 K2 O12 -38.84(14) . . . 2_566 ? O4 K1 K2 C92 105.71(17) . . . 2_566 ? O6 K1 K2 C92 94.9(2) . . . 2_566 ? O12 K1 K2 C92 -54.30(19) . . . 2_566 ? O10 K1 K2 C92 -81.43(17) . . . 2_566 ? C46 K1 K2 C92 98.79(19) . . . 2_566 ? C92 K1 K2 C92 -69.6(2) . . . 2_566 ? O4 K1 K2 C98 -129.32(17) . . . . ? O6 K1 K2 C98 -140.2(2) . . . . ? O12 K1 K2 C98 70.66(19) . . . . ? O10 K1 K2 C98 43.53(17) . . . . ? C46 K1 K2 C98 -136.25(18) . . . . ? C92 K1 K2 C98 55.40(18) . . . . ? O4 K1 K2 C93 -115.2(2) . . . . ? O6 K1 K2 C93 -126.0(2) . . . . ? O12 K1 K2 C93 84.8(2) . . . . ? O10 K1 K2 C93 57.7(2) . . . . ? C46 K1 K2 C93 -122.1(2) . . . . ? C92 K1 K2 C93 69.5(2) . . . . ? O4 K1 K2 K2 147.22(8) . . . 2_566 ? O6 K1 K2 K2 136.36(13) . . . 2_566 ? O12 K1 K2 K2 -12.80(11) . . . 2_566 ? O10 K1 K2 K2 -39.93(8) . . . 2_566 ? C46 K1 K2 K2 140.29(11) . . . 2_566 ? C92 K1 K2 K2 -28.06(11) . . . 2_566 ? O2 U1 O1 C9 -167.6(4) . . . . ? O3 U1 O1 C9 47.0(6) . . . . ? O4 U1 O1 C9 110.8(4) . . . . ? O5 U1 O1 C9 55.6(4) . . . . ? N1 U1 O1 C9 -35.3(4) . . . . ? N3 U1 O1 C9 -73.7(5) . . . . ? C46 U1 O1 C9 83.0(4) . . . . ? N2 U1 O1 C9 -101.5(4) . . . . ? O3 U1 O2 C22 -118.0(6) . . . . ? O1 U1 O2 C22 76.6(6) . . . . ? O4 U1 O2 C22 159.8(6) . . . . ? O5 U1 O2 C22 154.7(6) . . . . ? N1 U1 O2 C22 4.9(7) . . . . ? N3 U1 O2 C22 -51.1(6) . . . . ? C46 U1 O2 C22 157.8(6) . . . . ? N2 U1 O2 C22 9.3(6) . . . . ? O2 U1 O3 C35 119.9(6) . . . . ? O1 U1 O3 C35 -95.6(6) . . . . ? O4 U1 O3 C35 -159.3(6) . . . . ? O5 U1 O3 C35 -104.1(6) . . . . ? N1 U1 O3 C35 -20.4(6) . . . . ? N3 U1 O3 C35 37.1(5) . . . . ? C46 U1 O3 C35 -131.5(6) . . . . ? N2 U1 O3 C35 44.5(6) . . . . ? O2 U1 O4 C46 -176.0(3) . . . . ? O3 U1 O4 C46 79.2(3) . . . . ? O1 U1 O4 C46 -77.9(3) . . . . ? O5 U1 O4 C46 -0.2(2) . . . . ? N1 U1 O4 C46 -24.4(3) . . . . ? N3 U1 O4 C46 108.8(3) . . . . ? N2 U1 O4 C46 -129.9(3) . . . . ? O2 U1 O4 K1 -42.5(6) . . . . ? O3 U1 O4 K1 -147.3(6) . . . . ? O1 U1 O4 K1 55.6(6) . . . . ? O5 U1 O4 K1 133.3(7) . . . . ? N1 U1 O4 K1 109.1(6) . . . . ? N3 U1 O4 K1 -117.7(6) . . . . ? C46 U1 O4 K1 133.5(8) . . . . ? N2 U1 O4 K1 3.6(7) . . . . ? O6 K1 O4 C46 -5.4(2) . . . . ? O12 K1 O4 C46 1.8(3) . . . . ? O10 K1 O4 C46 -55.5(7) . . . . ? C92 K1 O4 C46 -6.4(4) . . . . ? K2 K1 O4 C46 -14.7(3) . . . . ? O6 K1 O4 U1 -139.0(7) . . . . ? O12 K1 O4 U1 -131.9(6) . . . . ? O10 K1 O4 U1 170.9(5) . . . . ? C46 K1 O4 U1 -133.6(8) . . . . ? C92 K1 O4 U1 -140.0(5) . . . . ? K2 K1 O4 U1 -148.3(6) . . . . ? O2 U1 O5 C46 6.4(3) . . . . ? O3 U1 O5 C46 -91.2(3) . . . . ? O1 U1 O5 C46 92.6(3) . . . . ? O4 U1 O5 C46 0.2(3) . . . . ? N1 U1 O5 C46 164.5(3) . . . . ? N3 U1 O5 C46 -139.6(3) . . . . ? N2 U1 O5 C46 128.5(3) . . . . ? O12 K2 O6 C46 -163.8(14) . . . . ? O11 K2 O6 C46 76.6(14) 2_566 . . . ? O12 K2 O6 C46 116.3(14) 2_566 . . . ? C92 K2 O6 C46 89.2(14) 2_566 . . . ? C98 K2 O6 C46 -57.3(15) . . . . ? C93 K2 O6 C46 -13.9(15) . . . . ? K1 K2 O6 C46 -142.4(14) . . . . ? K2 K2 O6 C46 164.7(13) 2_566 . . . ? O12 K2 O6 K1 -21.37(12) . . . . ? O11 K2 O6 K1 -140.96(11) 2_566 . . . ? O12 K2 O6 K1 -101.29(17) 2_566 . . . ? C92 K2 O6 K1 -128.37(14) 2_566 . . . ? C98 K2 O6 K1 85.2(3) . . . . ? C93 K2 O6 K1 128.6(2) . . . . ? K2 K2 O6 K1 -52.85(14) 2_566 . . . ? O4 K1 O6 C46 5.7(3) . . . . ? O12 K1 O6 C46 -168.5(3) . . . . ? O10 K1 O6 C46 175.6(3) . . . . ? C92 K1 O6 C46 -174.8(3) . . . . ? K2 K1 O6 C46 171.2(4) . . . . ? O4 K1 O6 K2 -165.49(18) . . . . ? O12 K1 O6 K2 20.34(11) . . . . ? O10 K1 O6 K2 4.44(17) . . . . ? C46 K1 O6 K2 -171.2(4) . . . . ? C92 K1 O6 K2 13.99(15) . . . . ? O9 U2 O7 C55 159.6(4) . . . . ? O8 U2 O7 C55 -38.9(4) . . . . ? O11 U2 O7 C55 -131.3(4) . . . . ? O10 U2 O7 C55 -119.9(4) . . . . ? N4 U2 O7 C55 53.1(4) . . . . ? N5 U2 O7 C55 18.4(4) . . . . ? N6 U2 O7 C55 101.5(4) . . . . ? C92 U2 O7 C55 -125.2(4) . . . . ? O9 U2 O8 C68 -159.3(6) . . . . ? O7 U2 O8 C68 145.3(7) . . . . ? O11 U2 O8 C68 -64.7(7) . . . . ? O10 U2 O8 C68 -117.7(7) . . . . ? N4 U2 O8 C68 70.0(7) . . . . ? N5 U2 O8 C68 6.4(7) . . . . ? N6 U2 O8 C68 13.9(8) . . . . ? C92 U2 O8 C68 -91.6(7) . . . . ? O8 U2 O9 C81 168.5(7) . . . . ? O7 U2 O9 C81 -135.4(8) . . . . ? O11 U2 O9 C81 72.4(8) . . . . ? O10 U2 O9 C81 126.9(8) . . . . ? N4 U2 O9 C81 -62.8(8) . . . . ? N5 U2 O9 C81 6.6(8) . . . . ? N6 U2 O9 C81 -6.2(7) . . . . ? C92 U2 O9 C81 99.6(8) . . . . ? O9 U2 O10 C92 -89.7(3) . . . . ? O8 U2 O10 C92 105.1(3) . . . . ? O7 U2 O10 C92 -170.1(3) . . . . ? O11 U2 O10 C92 2.9(3) . . . . ? N4 U2 O10 C92 150.9(6) . . . . ? N5 U2 O10 C92 43.5(3) . . . . ? N6 U2 O10 C92 -33.5(3) . . . . ? O4 K1 O10 C92 67.2(6) . . . . ? O6 K1 O10 C92 23.2(3) . . . . ? O12 K1 O10 C92 2.1(3) . . . . ? C46 K1 O10 C92 26.5(4) . . . . ? K2 K1 O10 C92 26.1(3) . . . . ? O9 U2 O11 C92 78.7(3) . . . . ? O8 U2 O11 C92 -78.8(3) . . . . ? O7 U2 O11 C92 11.1(4) . . . . ? O10 U2 O11 C92 -2.9(3) . . . . ? N4 U2 O11 C92 -174.8(3) . . . . ? N5 U2 O11 C92 -146.2(3) . . . . ? N6 U2 O11 C92 147.5(3) . . . . ? O9 U2 O11 K2 -142.0(6) . . . 2_566 ? O8 U2 O11 K2 60.4(6) . . . 2_566 ? O7 U2 O11 K2 150.3(5) . . . 2_566 ? O10 U2 O11 K2 136.4(6) . . . 2_566 ? N4 U2 O11 K2 -35.6(6) . . . 2_566 ? N5 U2 O11 K2 -7.0(5) . . . 2_566 ? N6 U2 O11 K2 -73.3(5) . . . 2_566 ? C92 U2 O11 K2 139.3(7) . . . 2_566 ? O6 K2 O12 C92 124.4(5) . . . . ? O11 K2 O12 C92 -132.0(5) 2_566 . . . ? O12 K2 O12 C92 -94.5(5) 2_566 . . . ? C92 K2 O12 C92 -109.1(5) 2_566 . . . ? C98 K2 O12 C92 -24.6(5) . . . . ? C93 K2 O12 C92 -35.7(6) . . . . ? K1 K2 O12 C92 103.4(5) . . . . ? K2 K2 O12 C92 -94.5(5) 2_566 . . . ? O6 K2 O12 K1 21.02(12) . . . . ? O11 K2 O12 K1 124.58(11) 2_566 . . . ? O12 K2 O12 K1 162.07(15) 2_566 . . . ? C92 K2 O12 K1 147.51(12) 2_566 . . . ? C98 K2 O12 K1 -128.03(15) . . . . ? C93 K2 O12 K1 -139.05(15) . . . . ? K2 K2 O12 K1 162.07(15) 2_566 . . . ? O6 K2 O12 K2 -141.05(12) . . . 2_566 ? O11 K2 O12 K2 -37.49(14) 2_566 . . 2_566 ? O12 K2 O12 K2 0.000(1) 2_566 . . 2_566 ? C92 K2 O12 K2 -14.56(13) 2_566 . . 2_566 ? C98 K2 O12 K2 69.91(15) . . . 2_566 ? C93 K2 O12 K2 58.89(18) . . . 2_566 ? K1 K2 O12 K2 -162.07(15) . . . 2_566 ? O4 K1 O12 C92 -169.7(3) . . . . ? O6 K1 O12 C92 -164.3(3) . . . . ? O10 K1 O12 C92 -2.1(3) . . . . ? C46 K1 O12 C92 -169.0(3) . . . . ? K2 K1 O12 C92 -144.5(3) . . . . ? O4 K1 O12 K2 -25.23(17) . . . . ? O6 K1 O12 K2 -19.76(11) . . . . ? O10 K1 O12 K2 142.39(17) . . . . ? C46 K1 O12 K2 -24.46(13) . . . . ? C92 K1 O12 K2 144.5(3) . . . . ? O4 K1 O12 K2 83.2(4) . . . 2_566 ? O6 K1 O12 K2 88.7(4) . . . 2_566 ? O10 K1 O12 K2 -109.1(4) . . . 2_566 ? C46 K1 O12 K2 84.0(4) . . . 2_566 ? C92 K1 O12 K2 -107.0(5) . . . 2_566 ? K2 K1 O12 K2 108.5(4) . . . 2_566 ? O2 U1 N1 C1 17.5(4) . . . . ? O3 U1 N1 C1 140.5(3) . . . . ? O1 U1 N1 C1 -65.6(3) . . . . ? O4 U1 N1 C1 -122.9(3) . . . . ? O5 U1 N1 C1 -142.5(3) . . . . ? N3 U1 N1 C1 82.0(3) . . . . ? C46 U1 N1 C1 -135.0(3) . . . . ? N2 U1 N1 C1 12.7(3) . . . . ? O2 U1 N1 C6 -106.4(3) . . . . ? O3 U1 N1 C6 16.7(3) . . . . ? O1 U1 N1 C6 170.6(3) . . . . ? O4 U1 N1 C6 113.3(3) . . . . ? O5 U1 N1 C6 93.6(2) . . . . ? N3 U1 N1 C6 -41.8(2) . . . . ? C46 U1 N1 C6 101.2(3) . . . . ? N2 U1 N1 C6 -111.1(3) . . . . ? O2 U1 N1 C7 140.8(2) . . . . ? O3 U1 N1 C7 -96.2(3) . . . . ? O1 U1 N1 C7 57.7(2) . . . . ? O4 U1 N1 C7 0.4(3) . . . . ? O5 U1 N1 C7 -19.3(3) . . . . ? N3 U1 N1 C7 -154.7(3) . . . . ? C46 U1 N1 C7 -11.7(3) . . . . ? N2 U1 N1 C7 136.0(3) . . . . ? O2 U1 N2 C3 -88.8(3) . . . . ? O3 U1 N2 C3 2.9(4) . . . . ? O1 U1 N2 C3 165.9(3) . . . . ? O4 U1 N2 C3 -138.3(3) . . . . ? O5 U1 N2 C3 129.0(3) . . . . ? N1 U1 N2 C3 87.4(3) . . . . ? N3 U1 N2 C3 10.8(3) . . . . ? C46 U1 N2 C3 175.0(3) . . . . ? O2 U1 N2 C2 149.4(3) . . . . ? O3 U1 N2 C2 -118.9(3) . . . . ? O1 U1 N2 C2 44.1(3) . . . . ? O4 U1 N2 C2 99.9(3) . . . . ? O5 U1 N2 C2 7.2(4) . . . . ? N1 U1 N2 C2 -34.4(3) . . . . ? N3 U1 N2 C2 -111.1(3) . . . . ? C46 U1 N2 C2 53.2(4) . . . . ? O2 U1 N2 C20 34.5(3) . . . . ? O3 U1 N2 C20 126.2(3) . . . . ? O1 U1 N2 C20 -70.8(3) . . . . ? O4 U1 N2 C20 -15.0(4) . . . . ? O5 U1 N2 C20 -107.7(3) . . . . ? N1 U1 N2 C20 -149.3(3) . . . . ? N3 U1 N2 C20 134.0(3) . . . . ? C46 U1 N2 C20 -61.7(4) . . . . ? O2 U1 N3 C4 34.6(3) . . . . ? O3 U1 N3 C4 140.1(3) . . . . ? O1 U1 N3 C4 -63.6(3) . . . . ? O4 U1 N3 C4 108.0(3) . . . . ? O5 U1 N3 C4 -167.8(3) . . . . ? N1 U1 N3 C4 -103.5(3) . . . . ? C46 U1 N3 C4 160.5(3) . . . . ? N2 U1 N3 C4 -33.4(3) . . . . ? O2 U1 N3 C5 157.2(3) . . . . ? O3 U1 N3 C5 -97.3(3) . . . . ? O1 U1 N3 C5 59.1(3) . . . . ? O4 U1 N3 C5 -129.3(3) . . . . ? O5 U1 N3 C5 -45.2(3) . . . . ? N1 U1 N3 C5 19.2(3) . . . . ? C46 U1 N3 C5 -76.9(4) . . . . ? N2 U1 N3 C5 89.3(3) . . . . ? O2 U1 N3 C33 -80.6(3) . . . . ? O3 U1 N3 C33 24.9(3) . . . . ? O1 U1 N3 C33 -178.7(3) . . . . ? O4 U1 N3 C33 -7.1(4) . . . . ? O5 U1 N3 C33 77.0(3) . . . . ? N1 U1 N3 C33 141.4(3) . . . . ? C46 U1 N3 C33 45.3(4) . . . . ? N2 U1 N3 C33 -148.6(3) . . . . ? O9 U2 N4 C47 167.6(3) . . . . ? O8 U2 N4 C47 -29.8(3) . . . . ? O7 U2 N4 C47 -115.2(3) . . . . ? O11 U2 N4 C47 67.8(3) . . . . ? O10 U2 N4 C47 -75.0(7) . . . . ? N5 U2 N4 C47 37.5(3) . . . . ? N6 U2 N4 C47 109.0(3) . . . . ? C92 U2 N4 C47 60.3(5) . . . . ? O9 U2 N4 C53 -76.2(3) . . . . ? O8 U2 N4 C53 86.4(3) . . . . ? O7 U2 N4 C53 1.0(3) . . . . ? O11 U2 N4 C53 -175.9(3) . . . . ? O10 U2 N4 C53 41.3(8) . . . . ? N5 U2 N4 C53 153.7(3) . . . . ? N6 U2 N4 C53 -134.8(3) . . . . ? C92 U2 N4 C53 176.5(4) . . . . ? O9 U2 N4 C52 45.7(3) . . . . ? O8 U2 N4 C52 -151.7(3) . . . . ? O7 U2 N4 C52 122.9(3) . . . . ? O11 U2 N4 C52 -54.0(4) . . . . ? O10 U2 N4 C52 163.2(5) . . . . ? N5 U2 N4 C52 -84.4(3) . . . . ? N6 U2 N4 C52 -12.9(3) . . . . ? C92 U2 N4 C52 -61.6(6) . . . . ? O9 U2 N5 C66 133.2(3) . . . . ? O8 U2 N5 C66 -39.5(3) . . . . ? O7 U2 N5 C66 -102.9(3) . . . . ? O11 U2 N5 C66 61.9(3) . . . . ? O10 U2 N5 C66 28.5(3) . . . . ? N4 U2 N5 C66 -140.1(3) . . . . ? N6 U2 N5 C66 146.5(3) . . . . ? C92 U2 N5 C66 46.9(3) . . . . ? O9 U2 N5 C49 20.3(4) . . . . ? O8 U2 N5 C49 -152.5(3) . . . . ? O7 U2 N5 C49 144.2(3) . . . . ? O11 U2 N5 C49 -51.0(3) . . . . ? O10 U2 N5 C49 -84.4(3) . . . . ? N4 U2 N5 C49 107.0(3) . . . . ? N6 U2 N5 C49 33.5(3) . . . . ? C92 U2 N5 C49 -66.0(3) . . . . ? O9 U2 N5 C48 -102.6(3) . . . . ? O8 U2 N5 C48 84.7(3) . . . . ? O7 U2 N5 C48 21.3(4) . . . . ? O11 U2 N5 C48 -173.9(3) . . . . ? O10 U2 N5 C48 152.7(3) . . . . ? N4 U2 N5 C48 -15.9(3) . . . . ? N6 U2 N5 C48 -89.4(3) . . . . ? C92 U2 N5 C48 171.1(3) . . . . ? O9 U2 N6 C51 -80.0(3) . . . . ? O8 U2 N6 C51 102.8(3) . . . . ? O7 U2 N6 C51 -15.5(3) . . . . ? O11 U2 N6 C51 -171.6(3) . . . . ? O10 U2 N6 C51 -142.1(3) . . . . ? N4 U2 N6 C51 37.0(3) . . . . ? N5 U2 N6 C51 110.5(3) . . . . ? C92 U2 N6 C51 -156.9(3) . . . . ? O9 U2 N6 C50 159.1(3) . . . . ? O8 U2 N6 C50 -18.1(4) . . . . ? O7 U2 N6 C50 -136.4(3) . . . . ? O11 U2 N6 C50 67.5(3) . . . . ? O10 U2 N6 C50 97.1(3) . . . . ? N4 U2 N6 C50 -83.8(3) . . . . ? N5 U2 N6 C50 -10.3(3) . . . . ? C92 U2 N6 C50 82.2(3) . . . . ? O9 U2 N6 C79 38.0(3) . . . . ? O8 U2 N6 C79 -139.3(3) . . . . ? O7 U2 N6 C79 102.4(3) . . . . ? O11 U2 N6 C79 -53.7(3) . . . . ? O10 U2 N6 C79 -24.1(4) . . . . ? N4 U2 N6 C79 155.0(3) . . . . ? N5 U2 N6 C79 -131.5(3) . . . . ? C92 U2 N6 C79 -39.0(3) . . . . ? C6 N1 C1 C2 129.2(4) . . . . ? C7 N1 C1 C2 -109.4(4) . . . . ? U1 N1 C1 C2 10.6(5) . . . . ? C3 N2 C2 C1 -70.5(5) . . . . ? C20 N2 C2 C1 168.8(4) . . . . ? U1 N2 C2 C1 55.4(4) . . . . ? N1 C1 C2 N2 -47.3(5) . . . . ? C2 N2 C3 C4 133.0(4) . . . . ? C20 N2 C3 C4 -107.6(4) . . . . ? U1 N2 C3 C4 13.4(5) . . . . ? C5 N3 C4 C3 -60.6(5) . . . . ? C33 N3 C4 C3 179.6(4) . . . . ? U1 N3 C4 C3 59.6(4) . . . . ? N2 C3 C4 N3 -50.2(5) . . . . ? C4 N3 C5 C6 127.7(4) . . . . ? C33 N3 C5 C6 -115.7(4) . . . . ? U1 N3 C5 C6 7.8(4) . . . . ? C1 N1 C6 C5 -61.4(5) . . . . ? C7 N1 C6 C5 177.0(4) . . . . ? U1 N1 C6 C5 69.4(4) . . . . ? N3 C5 C6 N1 -54.5(5) . . . . ? C1 N1 C7 C8 53.9(5) . . . . ? C6 N1 C7 C8 176.5(4) . . . . ? U1 N1 C7 C8 -77.3(4) . . . . ? N1 C7 C8 C13 -134.2(4) . . . . ? N1 C7 C8 C9 46.5(6) . . . . ? U1 O1 C9 C10 -172.2(3) . . . . ? U1 O1 C9 C8 11.5(7) . . . . ? C13 C8 C9 O1 179.1(4) . . . . ? C7 C8 C9 O1 -1.7(7) . . . . ? C13 C8 C9 C10 2.7(7) . . . . ? C7 C8 C9 C10 -178.0(4) . . . . ? O1 C9 C10 C11 -177.8(4) . . . . ? C8 C9 C10 C11 -1.5(7) . . . . ? O1 C9 C10 C14 -0.8(6) . . . . ? C8 C9 C10 C14 175.5(4) . . . . ? C9 C10 C11 C12 -1.1(7) . . . . ? C14 C10 C11 C12 -178.2(4) . . . . ? C10 C11 C12 C13 2.5(7) . . . . ? C10 C11 C12 C19 -179.7(5) . . . . ? C11 C12 C13 C8 -1.1(7) . . . . ? C19 C12 C13 C8 -179.0(5) . . . . ? C9 C8 C13 C12 -1.4(7) . . . . ? C7 C8 C13 C12 179.3(4) . . . . ? C11 C10 C14 C15 -86.1(6) . . . . ? C9 C10 C14 C15 96.9(5) . . . . ? C10 C14 C15 C17 -171.6(5) . . . . ? C10 C14 C15 C18 70.1(6) . . . . ? C10 C14 C15 C16 -52.6(6) . . . . ? C3 N2 C20 C21 55.9(5) . . . . ? C2 N2 C20 C21 176.1(4) . . . . ? U1 N2 C20 C21 -71.0(4) . . . . ? N2 C20 C21 C26 -121.5(5) . . . . ? N2 C20 C21 C22 63.2(6) . . . . ? U1 O2 C22 C21 -24.3(9) . . . . ? U1 O2 C22 C23 155.4(5) . . . . ? C26 C21 C22 O2 174.4(4) . . . . ? C20 C21 C22 O2 -10.2(7) . . . . ? C26 C21 C22 C23 -5.3(7) . . . . ? C20 C21 C22 C23 170.1(4) . . . . ? O2 C22 C23 C24 -174.9(4) . . . . ? C21 C22 C23 C24 4.8(7) . . . . ? O2 C22 C23 C27 4.4(7) . . . . ? C21 C22 C23 C27 -176.0(4) . . . . ? C22 C23 C24 C25 -0.5(8) . . . . ? C27 C23 C24 C25 -179.7(5) . . . . ? C23 C24 C25 C26 -3.3(8) . . . . ? C23 C24 C25 C32 175.8(5) . . . . ? C24 C25 C26 C21 2.9(7) . . . . ? C32 C25 C26 C21 -176.3(5) . . . . ? C22 C21 C26 C25 1.3(7) . . . . ? C20 C21 C26 C25 -173.9(4) . . . . ? C24 C23 C27 C28 -94.5(6) . . . . ? C22 C23 C27 C28 86.3(6) . . . . ? C23 C27 C28 C30 -165.5(4) . . . . ? C23 C27 C28 C29 -46.2(6) . . . . ? C23 C27 C28 C31 75.1(6) . . . . ? C4 N3 C33 C34 176.9(4) . . . . ? C5 N3 C33 C34 55.4(5) . . . . ? U1 N3 C33 C34 -65.9(4) . . . . ? N3 C33 C34 C39 -123.0(5) . . . . ? N3 C33 C34 C35 58.8(6) . . . . ? U1 O3 C35 C36 124.8(5) . . . . ? U1 O3 C35 C34 -54.7(8) . . . . ? C39 C34 C35 O3 178.1(4) . . . . ? C33 C34 C35 O3 -3.6(7) . . . . ? C39 C34 C35 C36 -1.3(7) . . . . ? C33 C34 C35 C36 176.9(4) . . . . ? O3 C35 C36 C37 -178.5(4) . . . . ? C34 C35 C36 C37 1.0(7) . . . . ? O3 C35 C36 C40 0.8(7) . . . . ? C34 C35 C36 C40 -179.8(4) . . . . ? C35 C36 C37 C38 0.0(8) . . . . ? C40 C36 C37 C38 -179.2(5) . . . . ? C36 C37 C38 C39 -0.7(8) . . . . ? C36 C37 C38 C45 179.1(5) . . . . ? C35 C34 C39 C38 0.7(8) . . . . ? C33 C34 C39 C38 -177.5(5) . . . . ? C37 C38 C39 C34 0.3(8) . . . . ? C45 C38 C39 C34 -179.4(5) . . . . ? C37 C36 C40 C41 -91.0(6) . . . . ? C35 C36 C40 C41 89.7(6) . . . . ? C36 C40 C41 C42 65.3(6) . . . . ? C36 C40 C41 C44 -56.6(6) . . . . ? C36 C40 C41 C43 -176.5(4) . . . . ? K2 O6 C46 O5 -48.3(16) . . . . ? K1 O6 C46 O5 169.3(4) . . . . ? K2 O6 C46 O4 132.2(12) . . . . ? K1 O6 C46 O4 -10.2(5) . . . . ? K2 O6 C46 K1 142.4(14) . . . . ? U1 O5 C46 O6 -179.8(4) . . . . ? U1 O5 C46 O4 -0.3(4) . . . . ? U1 O5 C46 K1 -64.0(19) . . . . ? U1 O4 C46 O6 179.8(4) . . . . ? K1 O4 C46 O6 10.2(5) . . . . ? U1 O4 C46 O5 0.3(4) . . . . ? K1 O4 C46 O5 -169.3(4) . . . . ? K1 O4 C46 U1 -169.67(18) . . . . ? U1 O4 C46 K1 169.67(18) . . . . ? O2 U1 C46 O5 -175.4(3) . . . . ? O3 U1 C46 O5 83.5(3) . . . . ? O1 U1 C46 O5 -81.6(3) . . . . ? O4 U1 C46 O5 -179.6(4) . . . . ? N1 U1 C46 O5 -16.8(3) . . . . ? N3 U1 C46 O5 64.3(4) . . . . ? N2 U1 C46 O5 -90.3(3) . . . . ? O2 U1 C46 O4 4.2(3) . . . . ? O3 U1 C46 O4 -96.9(3) . . . . ? O1 U1 C46 O4 98.1(3) . . . . ? O5 U1 C46 O4 179.6(4) . . . . ? N1 U1 C46 O4 162.9(2) . . . . ? N3 U1 C46 O4 -116.0(3) . . . . ? N2 U1 C46 O4 89.3(4) . . . . ? O2 U1 C46 K1 -5.8(2) . . . . ? O3 U1 C46 K1 -106.91(18) . . . . ? O1 U1 C46 K1 88.05(17) . . . . ? O4 U1 C46 K1 -10.03(17) . . . . ? O5 U1 C46 K1 169.6(4) . . . . ? N1 U1 C46 K1 152.84(14) . . . . ? N3 U1 C46 K1 -126.1(2) . . . . ? N2 U1 C46 K1 79.3(3) . . . . ? O4 K1 C46 O6 -169.9(5) . . . . ? O12 K1 C46 O6 11.5(3) . . . . ? O10 K1 C46 O6 -6.7(4) . . . . ? C92 K1 C46 O6 6.2(3) . . . . ? K2 K1 C46 O6 -6.3(3) . . . . ? O4 K1 C46 O5 68.5(18) . . . . ? O6 K1 C46 O5 -122(2) . . . . ? O12 K1 C46 O5 -110.0(19) . . . . ? O10 K1 C46 O5 -128.3(18) . . . . ? C92 K1 C46 O5 -115.4(19) . . . . ? K2 K1 C46 O5 -127.9(19) . . . . ? O6 K1 C46 O4 169.9(5) . . . . ? O12 K1 C46 O4 -178.6(2) . . . . ? O10 K1 C46 O4 163.2(2) . . . . ? C92 K1 C46 O4 176.1(2) . . . . ? K2 K1 C46 O4 163.6(3) . . . . ? O4 K1 C46 U1 9.57(17) . . . . ? O6 K1 C46 U1 179.5(4) . . . . ? O12 K1 C46 U1 -168.98(15) . . . . ? O10 K1 C46 U1 172.75(15) . . . . ? C92 K1 C46 U1 -174.32(14) . . . . ? K2 K1 C46 U1 173.16(19) . . . . ? C53 N4 C47 C48 -180.0(4) . . . . ? C52 N4 C47 C48 61.8(5) . . . . ? U2 N4 C47 C48 -61.8(4) . . . . ? C66 N5 C48 C47 114.6(5) . . . . ? C49 N5 C48 C47 -128.9(4) . . . . ? U2 N5 C48 C47 -8.6(5) . . . . ? N4 C47 C48 N5 49.8(6) . . . . ? C66 N5 C49 C50 -175.0(4) . . . . ? C48 N5 C49 C50 64.8(5) . . . . ? U2 N5 C49 C50 -59.1(4) . . . . ? C51 N6 C50 C49 -130.3(4) . . . . ? C79 N6 C50 C49 109.3(4) . . . . ? U2 N6 C50 C49 -14.8(5) . . . . ? N5 C49 C50 N6 51.2(6) . . . . ? C50 N6 C51 C52 60.2(5) . . . . ? C79 N6 C51 C52 178.0(4) . . . . ? U2 N6 C51 C52 -63.3(4) . . . . ? C47 N4 C52 C51 -131.3(4) . . . . ? C53 N4 C52 C51 110.1(5) . . . . ? U2 N4 C52 C51 -13.8(5) . . . . ? N6 C51 C52 N4 55.7(6) . . . . ? C47 N4 C53 C54 62.6(5) . . . . ? C52 N4 C53 C54 -176.6(4) . . . . ? U2 N4 C53 C54 -50.9(5) . . . . ? N4 C53 C54 C59 -117.2(5) . . . . ? N4 C53 C54 C55 71.0(6) . . . . ? U2 O7 C55 C54 -57.1(6) . . . . ? U2 O7 C55 C56 125.2(4) . . . . ? C59 C54 C55 O7 174.3(4) . . . . ? C53 C54 C55 O7 -13.7(7) . . . . ? C59 C54 C55 C56 -8.0(8) . . . . ? C53 C54 C55 C56 164.0(5) . . . . ? O7 C55 C56 C57 -172.4(5) . . . . ? C54 C55 C56 C57 9.8(8) . . . . ? O7 C55 C56 C60 15.3(8) . . . . ? C54 C55 C56 C60 -162.4(5) . . . . ? C55 C56 C57 C58 -4.7(8) . . . . ? C60 C56 C57 C58 167.5(5) . . . . ? C56 C57 C58 C59 -2.4(8) . . . . ? C56 C57 C58 C65 179.4(5) . . . . ? C57 C58 C59 C54 4.5(8) . . . . ? C65 C58 C59 C54 -177.3(5) . . . . ? C55 C54 C59 C58 0.6(8) . . . . ? C53 C54 C59 C58 -171.0(5) . . . . ? C57 C56 C60 C61 -82.5(6) . . . . ? C55 C56 C60 C61 89.5(6) . . . . ? C56 C60 C61 C64 178.3(4) . . . . ? C56 C60 C61 C63 -62.0(6) . . . . ? C56 C60 C61 C62 59.6(6) . . . . ? C49 N5 C66 C67 -174.9(4) . . . . ? C48 N5 C66 C67 -54.4(5) . . . . ? U2 N5 C66 C67 70.9(4) . . . . ? N5 C66 C67 C72 131.4(5) . . . . ? N5 C66 C67 C68 -55.8(6) . . . . ? U2 O8 C68 C69 -171.3(5) . . . . ? U2 O8 C68 C67 8.4(10) . . . . ? C72 C67 C68 O8 -177.6(5) . . . . ? C66 C67 C68 O8 9.6(7) . . . . ? C72 C67 C68 C69 2.1(8) . . . . ? C66 C67 C68 C69 -170.7(5) . . . . ? O8 C68 C69 C70 177.3(5) . . . . ? C67 C68 C69 C70 -2.4(8) . . . . ? O8 C68 C69 C73 -4.8(8) . . . . ? C67 C68 C69 C73 175.5(5) . . . . ? C68 C69 C70 C71 1.0(8) . . . . ? C73 C69 C70 C71 -176.9(5) . . . . ? C69 C70 C71 C72 0.8(8) . . . . ? C69 C70 C71 C78 177.8(5) . . . . ? C70 C71 C72 C67 -1.2(8) . . . . ? C78 C71 C72 C67 -178.2(5) . . . . ? C68 C67 C72 C71 -0.2(8) . . . . ? C66 C67 C72 C71 172.4(5) . . . . ? C70 C69 C73 C74 84.6(6) . . . . ? C68 C69 C73 C74 -93.3(6) . . . . ? C69 C73 C74 C77 -176.6(4) . . . . ? C69 C73 C74 C76 -57.1(6) . . . . ? C69 C73 C74 C75 64.0(6) . . . . ? C51 N6 C79 C80 47.5(6) . . . . ? C50 N6 C79 C80 168.4(4) . . . . ? U2 N6 C79 C80 -65.1(5) . . . . ? N6 C79 C80 C85 -136.6(5) . . . . ? N6 C79 C80 C81 48.7(7) . . . . ? U2 O9 C81 C82 168.1(5) . . . . ? U2 O9 C81 C80 -9.6(11) . . . . ? C85 C80 C81 O9 178.9(4) . . . . ? C79 C80 C81 O9 -6.3(7) . . . . ? C85 C80 C81 C82 1.1(8) . . . . ? C79 C80 C81 C82 175.9(5) . . . . ? O9 C81 C82 C83 -179.0(4) . . . . ? C80 C81 C82 C83 -1.3(7) . . . . ? O9 C81 C82 C86 1.0(7) . . . . ? C80 C81 C82 C86 178.8(5) . . . . ? C81 C82 C83 C84 -0.3(8) . . . . ? C86 C82 C83 C84 179.6(5) . . . . ? C82 C83 C84 C85 2.0(8) . . . . ? C82 C83 C84 C91 -174.9(5) . . . . ? C81 C80 C85 C84 0.7(8) . . . . ? C79 C80 C85 C84 -174.1(5) . . . . ? C83 C84 C85 C80 -2.2(8) . . . . ? C91 C84 C85 C80 174.7(5) . . . . ? C83 C82 C86 C87 -84.2(6) . . . . ? C81 C82 C86 C87 95.7(6) . . . . ? C82 C86 C87 C88 -57.2(6) . . . . ? C82 C86 C87 C89 -176.2(5) . . . . ? C82 C86 C87 C90 64.8(6) . . . . ? K2 O12 C92 O10 -98.8(6) . . . . ? K1 O12 C92 O10 4.0(5) . . . . ? K2 O12 C92 O10 165.9(4) 2_566 . . . ? K2 O12 C92 O11 80.0(7) . . . . ? K1 O12 C92 O11 -177.2(4) . . . . ? K2 O12 C92 O11 -15.3(5) 2_566 . . . ? K2 O12 C92 K2 95.3(5) . . . 2_566 ? K1 O12 C92 K2 -161.94(16) . . . 2_566 ? K2 O12 C92 K1 -102.8(5) . . . . ? K2 O12 C92 K1 161.94(16) 2_566 . . . ? U2 O10 C92 O12 174.0(4) . . . . ? K1 O10 C92 O12 -4.0(5) . . . . ? U2 O10 C92 O11 -4.8(4) . . . . ? K1 O10 C92 O11 177.2(4) . . . . ? K1 O10 C92 U2 -178.02(17) . . . . ? U2 O10 C92 K2 -64.9(13) . . . 2_566 ? K1 O10 C92 K2 117.1(13) . . . 2_566 ? U2 O10 C92 K1 178.02(17) . . . . ? U2 O11 C92 O12 -174.0(4) . . . . ? K2 O11 C92 O12 16.4(5) 2_566 . . . ? U2 O11 C92 O10 4.8(4) . . . . ? K2 O11 C92 O10 -164.7(4) 2_566 . . . ? K2 O11 C92 U2 -169.5(2) 2_566 . . . ? U2 O11 C92 K2 169.5(2) . . . 2_566 ? O9 U2 C92 O10 86.4(3) . . . . ? O8 U2 C92 O10 -72.7(3) . . . . ? O7 U2 C92 O10 11.7(3) . . . . ? O11 U2 C92 O10 -174.8(5) . . . . ? N4 U2 C92 O10 -163.1(3) . . . . ? N5 U2 C92 O10 -142.2(3) . . . . ? N6 U2 C92 O10 152.6(3) . . . . ? O9 U2 C92 O11 -98.8(3) . . . . ? O8 U2 C92 O11 102.1(3) . . . . ? O7 U2 C92 O11 -173.4(2) . . . . ? O10 U2 C92 O11 174.8(5) . . . . ? N4 U2 C92 O11 11.8(6) . . . . ? N5 U2 C92 O11 32.6(3) . . . . ? N6 U2 C92 O11 -32.6(3) . . . . ? O9 U2 C92 K2 -108.54(17) . . . 2_566 ? O8 U2 C92 K2 92.39(17) . . . 2_566 ? O7 U2 C92 K2 176.81(14) . . . 2_566 ? O11 U2 C92 K2 -9.75(19) . . . 2_566 ? O10 U2 C92 K2 165.1(4) . . . 2_566 ? N4 U2 C92 K2 2.0(5) . . . 2_566 ? N5 U2 C92 K2 22.85(18) . . . 2_566 ? N6 U2 C92 K2 -42.30(18) . . . 2_566 ? O9 U2 C92 K1 84.35(18) . . . . ? O8 U2 C92 K1 -74.72(18) . . . . ? O7 U2 C92 K1 9.7(2) . . . . ? O11 U2 C92 K1 -176.9(4) . . . . ? O10 U2 C92 K1 -2.02(17) . . . . ? N4 U2 C92 K1 -165.1(3) . . . . ? N5 U2 C92 K1 -144.26(17) . . . . ? N6 U2 C92 K1 150.59(17) . . . . ? O4 K1 C92 O12 16.5(4) . . . . ? O6 K1 C92 O12 15.7(3) . . . . ? O10 K1 C92 O12 176.2(5) . . . . ? C46 K1 C92 O12 13.2(3) . . . . ? K2 K1 C92 O12 25.9(2) . . . . ? O4 K1 C92 O10 -159.7(2) . . . . ? O6 K1 C92 O10 -160.5(3) . . . . ? O12 K1 C92 O10 -176.2(5) . . . . ? C46 K1 C92 O10 -163.0(2) . . . . ? K2 K1 C92 O10 -150.3(3) . . . . ? O4 K1 C92 U2 -157.79(17) . . . . ? O6 K1 C92 U2 -158.56(17) . . . . ? O12 K1 C92 U2 -174.3(4) . . . . ? O10 K1 C92 U2 1.94(17) . . . . ? C46 K1 C92 U2 -161.09(15) . . . . ? K2 K1 C92 U2 -148.4(2) . . . . ? O4 K1 C92 K2 36.3(3) . . . 2_566 ? O6 K1 C92 K2 35.6(2) . . . 2_566 ? O12 K1 C92 K2 19.9(2) . . . 2_566 ? O10 K1 C92 K2 -163.9(4) . . . 2_566 ? C46 K1 C92 K2 33.0(3) . . . 2_566 ? K2 K1 C92 K2 45.75(15) . . . 2_566 ? O6 K2 C93 C94 -3.2(7) . . . . ? O12 K2 C93 C94 139.9(5) . . . . ? O11 K2 C93 C94 -101.6(6) 2_566 . . . ? O12 K2 C93 C94 -151.0(6) 2_566 . . . ? C92 K2 C93 C94 -124.9(6) 2_566 . . . ? C98 K2 C93 C94 111.9(7) . . . . ? K1 K2 C93 C94 81.9(6) . . . . ? K2 K2 C93 C94 178.1(5) 2_566 . . . ? O6 K2 C93 C98 -115.1(4) . . . . ? O12 K2 C93 C98 28.0(5) . . . . ? O11 K2 C93 C98 146.4(4) 2_566 . . . ? O12 K2 C93 C98 97.1(4) 2_566 . . . ? C92 K2 C93 C98 123.2(4) 2_566 . . . ? K1 K2 C93 C98 -30.0(5) . . . . ? K2 K2 C93 C98 66.1(4) 2_566 . . . ? C98 C93 C94 C95 0.3(9) . . . . ? K2 C93 C94 C95 -80.6(7) . . . . ? C93 C94 C95 C96 -0.1(10) . . . . ? C94 C95 C96 C97 0.6(10) . . . . ? C95 C96 C97 C98 -1.2(10) . . . . ? C96 C97 C98 C93 1.4(9) . . . . ? C96 C97 C98 K2 104.8(6) . . . . ? C94 C93 C98 C97 -0.9(9) . . . . ? K2 C93 C98 C97 115.3(6) . . . . ? C94 C93 C98 K2 -116.2(5) . . . . ? O6 K2 C98 C97 -22.0(6) . . . . ? O12 K2 C98 C97 79.7(5) . . . . ? O11 K2 C98 C97 -157.1(5) 2_566 . . . ? O12 K2 C98 C97 162.3(5) 2_566 . . . ? C92 K2 C98 C97 -175.3(5) 2_566 . . . ? C93 K2 C98 C97 -123.9(7) . . . . ? K1 K2 C98 C97 36.5(5) . . . . ? K2 K2 C98 C97 122.4(5) 2_566 . . . ? O6 K2 C98 C93 101.8(5) . . . . ? O12 K2 C98 C93 -156.4(4) . . . . ? O11 K2 C98 C93 -33.2(4) 2_566 . . . ? O12 K2 C98 C93 -73.8(4) 2_566 . . . ? C92 K2 C98 C93 -51.4(4) 2_566 . . . ? K1 K2 C98 C93 160.3(4) . . . . ? K2 K2 C98 C93 -113.7(4) 2_566 . . . ? C106 C101 C102 C103 -1.1(13) . . . . ? C101 C102 C103 C104 2.7(10) . . . . ? C102 C103 C104 C105 -3.5(11) . . . . ? C103 C104 C105 C106 2.6(13) . . . . ? C102 C101 C106 C105 0.2(15) . . . . ? C104 C105 C106 C101 -1.0(15) . . . . ? C206 C201 C202 C203 -0.5(10) . . . . ? C201 C202 C203 C204 0.7(9) . . . . ? C202 C203 C204 C205 -0.4(9) . . . . ? C203 C204 C205 C206 0.0(9) . . . . ? C202 C201 C206 C205 0.1(10) . . . . ? C204 C205 C206 C201 0.1(10) . . . . ? C306 C301 C302 C303 1.8(9) . . . . ? C301 C302 C303 C304 -1.0(10) . . . . ? C302 C303 C304 C305 -0.4(10) . . . . ? C303 C304 C305 C306 1.1(10) . . . . ? C304 C305 C306 C301 -0.4(9) . . . . ? C302 C301 C306 C305 -1.1(9) . . . . ? C406 C401 C402 C403 0.8(10) . . . . ? C401 C402 C403 C404 0.3(10) . . . . ? C402 C403 C404 C405 -0.7(10) . . . . ? C403 C404 C405 C406 0.1(10) . . . . ? C404 C405 C406 C401 1.0(10) . . . . ? C402 C401 C406 C405 -1.4(11) . . . . ? C506 C501 C502 C503 0.0 . . . . ? C501 C502 C503 C504 0.0 . . . . ? C502 C503 C504 C505 0.0 . . . . ? C503 C504 C505 C506 0.0 . . . . ? C504 C505 C506 C501 0.0 . . . . ? C502 C501 C506 C505 0.0 . . . . ? C606 C601 C602 C603 0.0 . . . . ? C601 C602 C603 C604 0.0 . . . . ? C602 C603 C604 C605 0.0 . . . . ? C603 C604 C605 C606 0.0 . . . . ? C604 C605 C606 C601 0.0 . . . . ? C602 C601 C606 C605 0.0 . . . . ? C706 C701 C702 C703 0.0 . . . . ? C701 C702 C703 C704 0.0 . . . . ? C702 C703 C704 C705 0.0 . . . . ? C703 C704 C705 C706 0.0 . . . . ? C704 C705 C706 C701 0.0 . . . . ? C702 C701 C706 C705 0.0 . . . . ? C803 C801 C802 C803 -5(3) 2_656 . . . ? C801 C802 C803 C801 5(3) . . . 2_656 ? C903 C901 C902 C903 0.2(13) 2_677 . . . ? C901 C902 C903 C901 -0.2(13) . . . 2_677 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.072 _refine_diff_density_min -1.445 _refine_diff_density_rms 0.139 #===END OF DATA FOR 6 * 18 benzene