# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author ; Dr Marinella Mazzanti LCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; loop_ _publ_author_name _publ_author_address V.Mougel ; SCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; J.Pecaut ; sCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; M.Mazzanti ; sCIB (UMR-E 3 CEA-UJF) DRFMC, CEA Grenoble 17, rue des Martyrs 38054 Grenoble cedex 9 ; _publ_section_title ; New Polynuclear U(IV)-U(V) Complexes from U(IV) Mediated Uranyl(V) Disproportionation ; _publ_contact_author_name 'Dr Marinella Mazzanti' _publ_contact_author_email marinella.mazzanti@cea.fr data_1 _database_code_depnum_ccdc_archive 'CCDC 851298' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21.50 H23.50 K N3.50 O4 U' _chemical_formula_weight 672.07 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.925(4) _cell_length_b 14.316(3) _cell_length_c 14.0547(19) _cell_angle_alpha 90.00 _cell_angle_beta 101.946(15) _cell_angle_gamma 90.00 _cell_volume 4512.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1997 _cell_measurement_theta_min 3.3509 _cell_measurement_theta_max 29.0273 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 3 1 0 0.0036 2.9973 1.0006 0.0036 0.1002 -0.0364 -0.0079 -3 -1 0 0.0036 -2.9973 -1.0006 -0.0036 -0.1002 0.0364 0.0079 1 0 0 0.0059 0.9997 0.0002 0.0009 0.0218 -0.0229 0.0021 -1 0 0 0.0059 -0.9997 -0.0002 -0.0009 -0.0218 0.0229 -0.0021 0 0 1 0.2195 -0.0044 0.0006 1.0016 0.0155 0.0046 0.0489 0 0 -1 0.2195 0.0044 -0.0006 -1.0016 -0.0155 -0.0046 -0.0489 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 7.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1349 _exptl_absorpt_correction_T_max 0.9499 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12681 _diffrn_reflns_av_R_equivalents 0.1018 _diffrn_reflns_av_sigmaI/netI 0.1942 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6438 _reflns_number_gt 2989 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -25.00 16.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - 17.3113 102.0000 9.0000 41 #__ type_ start__ end____ width___ exp.time_ 2 omega 37.00 93.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - 17.3113 179.0000 -180.0000 56 #__ type_ start__ end____ width___ exp.time_ 3 omega -74.00 35.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - -19.0300 0.0000 90.0000 109 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0702P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6438 _refine_ls_number_parameters 546 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.1720 _refine_ls_R_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.2419 _refine_ls_wR_factor_gt 0.1986 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.003 _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 0.40895(5) 0.75529(8) 0.64394(6) 0.0637(4) Uani 1 1 d . . . O1U1 O 0.3538(9) 0.7959(16) 0.5350(12) 0.092(6) Uani 1 1 d . . . O2U1 O 0.4651(9) 0.7093(16) 0.7399(13) 0.101(7) Uani 1 1 d . . . U2 U 0.14516(5) 0.68269(10) 0.79940(8) 0.0844(5) Uani 1 1 d . . . O1U2 O 0.1970(8) 0.7018(16) 0.7183(12) 0.090(6) Uani 1 1 d . . . O2U2 O 0.0918(9) 0.666(2) 0.8743(14) 0.117(8) Uani 1 1 d . . . K1 K 0.2398(3) 0.7944(6) 0.5781(4) 0.088(2) Uani 1 1 d . . . K2 K 0.3092(3) 0.7100(5) 0.8469(4) 0.0775(18) Uani 1 1 d . . . O1 O 0.3568(8) 0.8427(13) 0.7457(12) 0.072(5) Uani 1 1 d . . . O2 O 0.3440(8) 0.6381(14) 0.6692(11) 0.070(5) Uani 1 1 d . . . N1 N 0.4643(11) 0.9160(17) 0.6857(14) 0.072(6) Uani 1 1 d . . . N2 N 0.4917(12) 0.795(2) 0.5432(17) 0.089(7) Uani 1 1 d U . . N3 N 0.4242(9) 0.6184(18) 0.5333(13) 0.068(6) Uani 1 1 d . . . C1 C 0.3446(14) 0.927(2) 0.757(2) 0.085(9) Uani 1 1 d . . . C2 C 0.2936(15) 0.955(2) 0.7904(19) 0.089(10) Uani 1 1 d . . . H2 H 0.2648 0.9104 0.7998 0.107 Uiso 1 1 calc R . . C3 C 0.2856(12) 1.047(3) 0.809(2) 0.085(10) Uani 1 1 d . . . H3 H 0.2497 1.0647 0.8274 0.102 Uiso 1 1 calc R . . C4 C 0.3280(18) 1.116(2) 0.802(2) 0.107(12) Uani 1 1 d . . . H4 H 0.3217 1.1792 0.8181 0.129 Uiso 1 1 calc R . . C5 C 0.3778(17) 1.090(3) 0.772(2) 0.107(13) Uani 1 1 d . . . H5 H 0.4065 1.1371 0.7671 0.129 Uiso 1 1 calc R . . C6 C 0.3889(14) 1.002(2) 0.749(2) 0.072(8) Uani 1 1 d . . . C7 C 0.4412(14) 0.990(2) 0.7195(17) 0.076(8) Uani 1 1 d . . . H7 H 0.4653 1.0446 0.7239 0.092 Uiso 1 1 calc R . . C8 C 0.5203(12) 0.920(2) 0.657(2) 0.085(9) Uani 1 1 d . . . H8A H 0.5516 0.9361 0.7141 0.101 Uiso 1 1 calc R . . H8B H 0.5188 0.9707 0.6084 0.101 Uiso 1 1 calc R . . C9 C 0.5386(14) 0.827(3) 0.612(3) 0.111(11) Uani 1 1 d U . . H9A H 0.5732 0.8389 0.5814 0.134 Uiso 1 1 calc R . . H9B H 0.5503 0.7799 0.6634 0.134 Uiso 1 1 calc R . . C10 C 0.5062(16) 0.700(3) 0.502(3) 0.124(13) Uani 1 1 d . . . H10A H 0.5304 0.7117 0.4527 0.149 Uiso 1 1 calc R . . H10B H 0.5314 0.6643 0.5557 0.149 Uiso 1 1 calc R . . C11 C 0.4592(12) 0.645(2) 0.4612(15) 0.072(8) Uani 1 1 d U . . H11A H 0.4741 0.5880 0.4341 0.086 Uiso 1 1 calc R . . H11B H 0.4334 0.6792 0.4071 0.086 Uiso 1 1 calc R . . C12 C 0.4042(13) 0.535(2) 0.535(2) 0.077(8) Uani 1 1 d U . . H12 H 0.4118 0.4941 0.4860 0.093 Uiso 1 1 calc R . . C13 C 0.3721(13) 0.495(3) 0.602(2) 0.092(10) Uani 1 1 d . . . C14 C 0.3657(14) 0.398(2) 0.599(2) 0.086(9) Uani 1 1 d U . . H14 H 0.3783 0.3647 0.5484 0.103 Uiso 1 1 calc R . . C15 C 0.3430(15) 0.350(2) 0.664(2) 0.095(10) Uani 1 1 d . . . H15 H 0.3423 0.2835 0.6629 0.114 Uiso 1 1 calc R . . C16 C 0.3199(16) 0.400(2) 0.735(2) 0.100(11) Uani 1 1 d . . . H16 H 0.3051 0.3669 0.7837 0.120 Uiso 1 1 calc R . . C17 C 0.3188(13) 0.492(3) 0.7337(16) 0.080(9) Uani 1 1 d . . . H17 H 0.2995 0.5235 0.7782 0.096 Uiso 1 1 calc R . . C18 C 0.3449(13) 0.547(2) 0.6697(18) 0.074(8) Uani 1 1 d . . . C19 C 0.4717(17) 0.859(3) 0.466(3) 0.140(15) Uani 1 1 d U . . H19A H 0.4470 0.9075 0.4882 0.210 Uiso 1 1 calc R . . H19B H 0.4481 0.8263 0.4103 0.210 Uiso 1 1 calc R . . H19C H 0.5062 0.8889 0.4475 0.210 Uiso 1 1 calc R . . O21 O 0.1915(10) 0.8022(19) 0.8990(15) 0.109(7) Uani 1 1 d . . . O22 O 0.2194(8) 0.5899(15) 0.8984(12) 0.080(5) Uani 1 1 d U . . N21 N 0.0912(15) 0.841(3) 0.7331(19) 0.152(15) Uani 1 1 d U . . N22 N 0.0572(11) 0.660(3) 0.6421(15) 0.095(9) Uani 1 1 d . . . N23 N 0.1258(12) 0.507(2) 0.7505(17) 0.099(9) Uani 1 1 d . . . C21 C 0.1802(12) 0.890(2) 0.917(2) 0.077(9) Uani 1 1 d . . . C22 C 0.2172(14) 0.935(3) 0.999(2) 0.103(11) Uani 1 1 d . . . H22 H 0.2494 0.9019 1.0380 0.124 Uiso 1 1 calc R . . C23 C 0.2053(15) 1.026(2) 1.019(2) 0.086(9) Uani 1 1 d . . . H23 H 0.2275 1.0535 1.0769 0.103 Uiso 1 1 calc R . . C24 C 0.1618(14) 1.082(3) 0.958(2) 0.094(11) Uani 1 1 d . . . H24 H 0.1558 1.1460 0.9724 0.113 Uiso 1 1 calc R . . C25 C 0.1300(15) 1.041(3) 0.880(2) 0.100(11) Uani 1 1 d . . . H25 H 0.1018 1.0790 0.8377 0.120 Uiso 1 1 calc R . . C26 C 0.1335(14) 0.948(3) 0.852(2) 0.093(10) Uani 1 1 d U . . C27 C 0.0911(17) 0.916(3) 0.768(3) 0.113(12) Uani 1 1 d U . . H27 H 0.0608 0.9589 0.7392 0.136 Uiso 1 1 calc R . . C28 C 0.0366(19) 0.829(4) 0.649(3) 0.150(14) Uani 1 1 d U . . H28A H 0.0484 0.8430 0.5869 0.180 Uiso 1 1 calc R . . H28B H 0.0056 0.8747 0.6577 0.180 Uiso 1 1 calc R . . C29 C 0.0080(19) 0.721(4) 0.645(2) 0.15(2) Uani 1 1 d . . . H29A H -0.0088 0.7080 0.7030 0.179 Uiso 1 1 calc R . . H29B H -0.0238 0.7126 0.5860 0.179 Uiso 1 1 calc R . . C30 C 0.0361(18) 0.563(4) 0.657(3) 0.139(15) Uani 1 1 d U . . H30A H 0.0165 0.5660 0.7130 0.167 Uiso 1 1 calc R . . H30B H 0.0043 0.5489 0.5991 0.167 Uiso 1 1 calc R . . C31 C 0.0729(17) 0.486(3) 0.671(3) 0.122(13) Uani 1 1 d U . . H31A H 0.0862 0.4713 0.6101 0.146 Uiso 1 1 calc R . . H31B H 0.0509 0.4319 0.6890 0.146 Uiso 1 1 calc R . . C32 C 0.1504(16) 0.433(3) 0.796(2) 0.103(11) Uani 1 1 d U . . H32 H 0.1321 0.3746 0.7765 0.123 Uiso 1 1 calc R . . C33 C 0.2015(15) 0.431(2) 0.872(2) 0.087(9) Uani 1 1 d . . . C34 C 0.2200(17) 0.338(3) 0.904(2) 0.108(11) Uani 1 1 d U . . H34 H 0.1977 0.2852 0.8755 0.129 Uiso 1 1 calc R . . C35 C 0.2680(18) 0.325(3) 0.973(2) 0.121(13) Uani 1 1 d . . . H35 H 0.2769 0.2631 0.9955 0.146 Uiso 1 1 calc R . . C36 C 0.3063(14) 0.3946(19) 1.0154(18) 0.077(9) Uani 1 1 d . . . H36 H 0.3429 0.3820 1.0593 0.092 Uiso 1 1 calc R . . C37 C 0.2872(13) 0.483(2) 0.9890(17) 0.074(8) Uani 1 1 d . . . H37 H 0.3116 0.5335 1.0180 0.088 Uiso 1 1 calc R . . C38 C 0.2363(15) 0.505(2) 0.925(2) 0.082(9) Uani 1 1 d . . . C39 C 0.0762(8) 0.6655(15) 0.5523(10) 0.18(3) Uani 1 1 d . . . H40A H 0.0457 0.6380 0.5006 0.275 Uiso 1 1 calc R . . H40B H 0.1137 0.6311 0.5574 0.275 Uiso 1 1 calc R . . H40C H 0.0824 0.7310 0.5369 0.275 Uiso 1 1 calc R . . N41 N 0.1578(8) 0.1876(15) 0.6535(10) 0.159(14) Uani 1 1 d R . . C41 C 0.1631(8) 0.1036(15) 0.6061(10) 0.123(14) Uani 1 1 d R . . H41A H 0.2015 0.0796 0.6040 0.147 Uiso 1 1 calc R . . C42 C 0.1123(8) 0.0547(15) 0.5621(10) 0.160(18) Uani 1 1 d RU . . H42A H 0.1159 -0.0026 0.5297 0.192 Uiso 1 1 calc R . . C43 C 0.0562(8) 0.0898(15) 0.5654(10) 0.17(2) Uani 1 1 d R . . H43A H 0.0215 0.0565 0.5352 0.206 Uiso 1 1 calc R . . C44 C 0.0509(8) 0.1738(15) 0.6127(10) 0.128(18) Uani 1 1 d R . . H44 H 0.0126 0.1978 0.6149 0.153 Uiso 1 1 calc R . . C45 C 0.1017(8) 0.2227(15) 0.6568(10) 0.110(11) Uani 1 1 d RU . . H45 H 0.0981 0.2800 0.6891 0.132 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 0.0795(8) 0.0559(7) 0.0575(6) 0.0005(5) 0.0181(4) 0.0039(6) O1U1 0.117(16) 0.104(18) 0.067(11) -0.013(11) 0.044(10) -0.026(14) O2U1 0.112(16) 0.101(18) 0.085(13) 0.004(12) 0.009(10) -0.062(15) U2 0.0752(8) 0.0933(11) 0.0846(8) -0.0084(7) 0.0161(5) -0.0002(8) O1U2 0.089(14) 0.092(17) 0.086(12) 0.009(12) 0.010(9) 0.015(13) O2U2 0.104(16) 0.15(3) 0.094(14) -0.011(15) 0.003(11) -0.009(17) K1 0.094(5) 0.101(6) 0.072(4) 0.003(4) 0.023(3) 0.004(4) K2 0.088(4) 0.080(5) 0.065(3) 0.006(3) 0.017(3) -0.012(4) O1 0.087(14) 0.044(12) 0.095(13) -0.015(10) 0.038(10) 0.008(11) O2 0.081(13) 0.074(15) 0.062(10) -0.025(10) 0.030(8) -0.009(12) N1 0.093(18) 0.060(17) 0.066(14) 0.012(12) 0.023(11) -0.006(15) N2 0.107(15) 0.091(15) 0.070(12) 0.004(12) 0.018(11) 0.036(14) N3 0.076(15) 0.085(19) 0.046(11) -0.010(12) 0.019(10) 0.014(15) C1 0.08(2) 0.05(2) 0.11(2) -0.010(18) -0.004(17) 0.00(2) C2 0.12(3) 0.07(2) 0.09(2) 0.006(17) 0.034(18) 0.04(2) C3 0.060(19) 0.10(3) 0.11(2) -0.01(2) 0.045(15) 0.02(2) C4 0.19(4) 0.023(15) 0.13(3) 0.022(16) 0.07(3) -0.01(2) C5 0.13(3) 0.13(4) 0.068(19) -0.01(2) 0.045(18) 0.01(3) C6 0.09(2) 0.040(17) 0.09(2) 0.012(15) 0.030(17) -0.017(19) C7 0.11(3) 0.06(2) 0.061(17) 0.020(15) 0.008(15) 0.00(2) C8 0.08(2) 0.050(19) 0.13(2) -0.008(18) 0.031(17) -0.017(18) C9 0.074(16) 0.14(2) 0.142(18) -0.002(16) 0.061(14) -0.005(15) C10 0.12(3) 0.11(3) 0.15(3) 0.00(3) 0.04(2) -0.05(3) C11 0.090(15) 0.088(17) 0.041(11) -0.008(12) 0.019(10) 0.003(14) C12 0.084(16) 0.069(16) 0.070(14) -0.014(13) -0.004(12) -0.011(14) C13 0.09(2) 0.10(3) 0.09(2) -0.03(2) 0.007(17) 0.01(2) C14 0.097(16) 0.062(16) 0.099(16) 0.002(14) 0.021(13) 0.004(15) C15 0.15(3) 0.06(2) 0.08(2) -0.007(17) 0.032(19) 0.01(2) C16 0.14(3) 0.06(2) 0.10(2) 0.05(2) 0.04(2) 0.00(2) C17 0.09(2) 0.11(3) 0.034(14) 0.007(15) 0.006(12) 0.01(2) C18 0.10(2) 0.07(2) 0.056(16) -0.009(15) 0.026(14) -0.02(2) C19 0.16(3) 0.13(3) 0.15(3) 0.01(2) 0.09(2) 0.01(2) O21 0.105(17) 0.10(2) 0.114(16) -0.005(15) 0.007(12) 0.012(16) O22 0.085(12) 0.067(12) 0.085(10) -0.012(10) 0.014(8) -0.038(11) N21 0.18(3) 0.16(4) 0.085(19) 0.01(2) -0.028(16) 0.11(3) N22 0.080(18) 0.14(3) 0.062(14) -0.004(16) 0.018(12) -0.03(2) N23 0.10(2) 0.09(2) 0.085(17) -0.003(16) -0.019(13) -0.032(19) C21 0.056(18) 0.06(2) 0.11(2) -0.041(18) 0.005(15) -0.014(17) C22 0.08(2) 0.10(3) 0.13(3) -0.03(2) 0.012(18) -0.03(2) C23 0.13(3) 0.05(2) 0.070(18) -0.003(16) 0.020(18) 0.00(2) C24 0.10(2) 0.12(3) 0.069(19) 0.01(2) 0.027(16) 0.03(2) C25 0.12(3) 0.11(3) 0.07(2) 0.00(2) 0.020(18) 0.02(3) C26 0.083(16) 0.094(18) 0.095(16) -0.002(15) 0.005(13) 0.029(15) C27 0.130(19) 0.094(19) 0.112(18) -0.020(16) 0.014(15) 0.033(17) C28 0.15(2) 0.15(2) 0.136(19) 0.000(18) -0.005(14) 0.011(18) C29 0.14(4) 0.23(7) 0.09(3) -0.02(3) 0.05(2) 0.00(4) C30 0.12(2) 0.15(2) 0.14(2) -0.005(18) 0.025(16) 0.012(18) C31 0.117(19) 0.10(2) 0.136(19) -0.011(16) 0.008(15) -0.030(17) C32 0.110(18) 0.098(19) 0.104(17) 0.015(15) 0.033(14) -0.031(16) C33 0.10(2) 0.05(2) 0.10(2) 0.008(17) 0.004(18) -0.02(2) C34 0.122(19) 0.096(19) 0.102(17) -0.008(15) 0.016(14) -0.024(17) C35 0.16(4) 0.09(3) 0.10(3) 0.00(2) 0.02(2) -0.03(3) C36 0.12(3) 0.041(17) 0.067(17) 0.001(14) 0.016(15) -0.023(19) C37 0.10(2) 0.07(2) 0.049(15) -0.011(15) -0.001(14) 0.00(2) C38 0.11(3) 0.07(2) 0.08(2) -0.013(18) 0.043(18) -0.01(2) C39 0.08(3) 0.36(9) 0.11(3) 0.02(4) 0.03(2) 0.02(4) N41 0.20(4) 0.15(4) 0.13(3) 0.02(3) 0.04(2) 0.00(3) C41 0.15(3) 0.12(4) 0.09(2) -0.04(2) 0.01(2) -0.01(3) C42 0.16(2) 0.16(3) 0.16(2) 0.007(18) 0.031(17) 0.008(18) C43 0.24(6) 0.14(5) 0.15(4) 0.01(3) 0.07(3) -0.02(5) C44 0.07(2) 0.25(6) 0.067(19) 0.09(3) 0.023(14) 0.05(3) C45 0.108(18) 0.13(2) 0.097(16) -0.007(15) 0.034(14) 0.032(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2U1 1.79(2) . ? U1 O1U1 1.86(2) . ? U1 O2 2.318(19) . ? U1 O1 2.398(15) . ? U1 N3 2.57(2) . ? U1 N1 2.63(2) . ? U1 N2 2.65(3) . ? U1 K1 3.837(7) . ? U1 K2 4.061(6) . ? U1 K2 4.353(6) 4_575 ? O1U1 K2 2.631(18) 4_575 ? O1U1 K1 2.804(19) . ? U2 O2U2 1.79(2) . ? U2 O1U2 1.830(18) . ? U2 O21 2.32(2) . ? U2 O22 2.37(2) . ? U2 N23 2.62(3) . ? U2 N21 2.65(3) . ? U2 N22 2.69(2) . ? U2 K2 3.701(6) . ? U2 K1 4.079(6) 4_576 ? U2 K1 4.442(6) . ? O1U2 K1 2.72(2) . ? O1U2 K2 2.824(18) . ? K1 O21 2.88(2) 4_575 ? K1 O22 2.975(19) 4_575 ? K1 O1 3.26(2) . ? K1 O2 3.33(2) . ? K1 C22 3.47(4) 4_575 ? K1 K2 3.903(8) 4_575 ? K1 K2 3.972(8) . ? K1 U2 4.079(6) 4_575 ? K2 O1U1 2.631(18) 4_576 ? K2 O1 2.733(19) . ? K2 O22 2.887(19) . ? K2 O2 2.961(16) . ? K2 O21 3.22(2) . ? K2 C1 3.51(3) . ? K2 C17 3.53(4) . ? K2 K1 3.903(8) 4_576 ? O1 C1 1.26(4) . ? O2 C18 1.31(3) . ? N1 C7 1.32(3) . ? N1 C8 1.43(3) . ? N2 C9 1.37(4) . ? N2 C19 1.42(4) . ? N2 C10 1.54(5) . ? N3 C12 1.28(4) . ? N3 C11 1.47(3) . ? C1 C2 1.40(4) . ? C1 C6 1.50(4) . ? C2 C3 1.35(4) . ? C3 C4 1.41(4) . ? C4 C5 1.35(4) . ? C5 C6 1.34(4) . ? C6 C7 1.36(4) . ? C8 C9 1.56(4) . ? C10 C11 1.36(4) . ? C12 C13 1.43(4) . ? C13 C14 1.40(5) . ? C13 C18 1.44(4) . ? C14 C15 1.33(4) . ? C15 C16 1.41(4) . ? C16 C17 1.32(4) . ? C17 C18 1.41(4) . ? O21 C21 1.32(4) . ? O21 K1 2.88(2) 4_576 ? O22 C38 1.31(4) . ? O22 K1 2.975(19) 4_576 ? N21 C27 1.19(4) . ? N21 C28 1.54(4) . ? N22 C39 1.42(2) . ? N22 C29 1.43(5) . ? N22 C30 1.50(5) . ? N23 C32 1.30(4) . ? N23 C31 1.50(4) . ? C21 C22 1.43(4) . ? C21 C26 1.50(4) . ? C22 C23 1.38(4) . ? C22 K1 3.47(4) 4_576 ? C23 C24 1.42(4) . ? C24 C25 1.33(4) . ? C25 C26 1.40(5) . ? C26 C27 1.43(4) . ? C28 C29 1.68(6) . ? C30 C31 1.37(5) . ? C32 C33 1.42(4) . ? C33 C34 1.45(5) . ? C33 C38 1.43(4) . ? C34 C35 1.32(4) . ? C35 C36 1.38(4) . ? C36 C37 1.37(4) . ? C37 C38 1.35(4) . ? N41 C45 1.3904 . ? N41 C41 1.3918 . ? C41 C42 1.3892 . ? C42 C43 1.3904 . ? C43 C44 1.3918 . ? C44 C45 1.3892 . ? 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 O2U1 U1 O1U1 174.1(9) . . ? O2U1 U1 O2 90.2(8) . . ? O1U1 U1 O2 90.2(8) . . ? O2U1 U1 O1 96.4(8) . . ? O1U1 U1 O1 89.4(7) . . ? O2 U1 O1 82.6(6) . . ? O2U1 U1 N3 90.5(9) . . ? O1U1 U1 N3 84.0(8) . . ? O2 U1 N3 73.3(6) . . ? O1 U1 N3 155.0(7) . . ? O2U1 U1 N1 85.1(8) . . ? O1U1 U1 N1 97.1(8) . . ? O2 U1 N1 153.2(6) . . ? O1 U1 N1 71.8(7) . . ? N3 U1 N1 132.9(7) . . ? O2U1 U1 N2 89.9(8) . . ? O1U1 U1 N2 86.2(7) . . ? O2 U1 N2 142.1(8) . . ? O1 U1 N2 135.0(8) . . ? N3 U1 N2 68.7(8) . . ? N1 U1 N2 64.4(8) . . ? O2U1 U1 K1 140.4(6) . . ? O1U1 U1 K1 43.7(5) . . ? O2 U1 K1 59.6(5) . . ? O1 U1 K1 57.6(5) . . ? N3 U1 K1 102.9(5) . . ? N1 U1 K1 110.0(6) . . ? N2 U1 K1 129.7(5) . . ? O2U1 U1 K2 80.4(6) . . ? O1U1 U1 K2 104.0(5) . . ? O2 U1 K2 45.9(4) . . ? O1 U1 K2 40.7(5) . . ? N3 U1 K2 118.1(5) . . ? N1 U1 K2 107.3(5) . . ? N2 U1 K2 168.0(6) . . ? K1 U1 K2 60.31(12) . . ? O2U1 U1 K2 156.9(7) . 4_575 ? O1U1 U1 K2 17.3(6) . 4_575 ? O2 U1 K2 90.2(4) . 4_575 ? O1 U1 K2 106.5(5) . 4_575 ? N3 U1 K2 67.5(5) . 4_575 ? N1 U1 K2 104.3(4) . 4_575 ? N2 U1 K2 75.8(5) . 4_575 ? K1 U1 K2 56.50(12) . 4_575 ? K2 U1 K2 115.56(15) . 4_575 ? U1 O1U1 K2 150.6(10) . 4_575 ? U1 O1U1 K1 108.9(7) . . ? K2 O1U1 K1 91.7(6) 4_575 . ? O2U2 U2 O1U2 177.4(9) . . ? O2U2 U2 O21 91.5(10) . . ? O1U2 U2 O21 89.5(9) . . ? O2U2 U2 O22 94.3(9) . . ? O1U2 U2 O22 88.3(7) . . ? O21 U2 O22 82.9(7) . . ? O2U2 U2 N23 85.9(11) . . ? O1U2 U2 N23 94.4(9) . . ? O21 U2 N23 153.6(8) . . ? O22 U2 N23 71.2(7) . . ? O2U2 U2 N21 89.7(12) . . ? O1U2 U2 N21 88.3(10) . . ? O21 U2 N21 72.9(10) . . ? O22 U2 N21 155.5(10) . . ? N23 U2 N21 133.3(10) . . ? O2U2 U2 N22 88.9(8) . . ? O1U2 U2 N22 88.8(7) . . ? O21 U2 N22 139.2(10) . . ? O22 U2 N22 137.8(9) . . ? N23 U2 N22 67.1(10) . . ? N21 U2 N22 66.3(11) . . ? O2U2 U2 K2 134.5(6) . . ? O1U2 U2 K2 47.9(5) . . ? O21 U2 K2 59.5(6) . . ? O22 U2 K2 51.3(4) . . ? N23 U2 K2 105.0(6) . . ? N21 U2 K2 110.8(9) . . ? N22 U2 K2 136.3(5) . . ? O2U2 U2 K1 74.8(6) . 4_576 ? O1U2 U2 K1 107.5(6) . 4_576 ? O21 U2 K1 43.6(6) . 4_576 ? O22 U2 K1 46.1(5) . 4_576 ? N23 U2 K1 110.9(5) . 4_576 ? N21 U2 K1 112.7(7) . 4_576 ? N22 U2 K1 163.7(5) . 4_576 ? K2 U2 K1 59.99(12) . 4_576 ? O2U2 U2 K1 162.4(8) . . ? O1U2 U2 K1 15.3(6) . . ? O21 U2 K1 85.9(6) . . ? O22 U2 K1 102.6(4) . . ? N23 U2 K1 104.0(6) . . ? N21 U2 K1 72.9(8) . . ? N22 U2 K1 81.9(5) . . ? K2 U2 K1 57.54(12) . . ? K1 U2 K1 113.82(14) 4_576 . ? U2 O1U2 K1 154.4(10) . . ? U2 O1U2 K2 103.3(7) . . ? K1 O1U2 K2 91.5(6) . . ? O1U2 K1 O1U1 130.7(6) . . ? O1U2 K1 O21 105.5(7) . 4_575 ? O1U1 K1 O21 91.3(6) . 4_575 ? O1U2 K1 O22 150.4(6) . 4_575 ? O1U1 K1 O22 78.6(6) . 4_575 ? O21 K1 O22 64.0(7) 4_575 4_575 ? O1U2 K1 O1 86.9(5) . . ? O1U1 K1 O1 59.3(5) . . ? O21 K1 O1 147.4(6) 4_575 . ? O22 K1 O1 117.2(6) 4_575 . ? O1U2 K1 O2 74.4(5) . . ? O1U1 K1 O2 57.4(5) . . ? O21 K1 O2 97.4(6) 4_575 . ? O22 K1 O2 132.4(5) 4_575 . ? O1 K1 O2 56.4(5) . . ? O1U2 K1 C22 73.8(7) . 4_575 ? O1U1 K1 C22 91.2(7) . 4_575 ? O21 K1 C22 42.3(7) 4_575 4_575 ? O22 K1 C22 105.4(7) 4_575 4_575 ? O1 K1 C22 118.7(6) . 4_575 ? O2 K1 C22 62.4(6) . 4_575 ? O1U2 K1 U1 104.6(4) . . ? O1U1 K1 U1 27.4(4) . . ? O21 K1 U1 109.1(5) 4_575 . ? O22 K1 U1 105.0(4) 4_575 . ? O1 K1 U1 38.4(3) . . ? O2 K1 U1 36.9(3) . . ? C22 K1 U1 90.9(5) 4_575 . ? O1U2 K1 K2 149.9(5) . 4_575 ? O1U1 K1 K2 42.4(4) . 4_575 ? O21 K1 K2 54.2(5) 4_575 4_575 ? O22 K1 K2 47.3(4) 4_575 4_575 ? O1 K1 K2 100.9(3) . 4_575 ? O2 K1 K2 85.7(3) . 4_575 ? C22 K1 K2 77.0(5) 4_575 4_575 ? U1 K1 K2 68.44(14) . 4_575 ? O1U2 K1 K2 45.3(4) . . ? O1U1 K1 K2 90.0(4) . . ? O21 K1 K2 133.6(6) 4_575 . ? O22 K1 K2 159.8(5) 4_575 . ? O1 K1 K2 43.0(3) . . ? O2 K1 K2 46.8(3) . . ? C22 K1 K2 91.3(5) 4_575 . ? U1 K1 K2 62.63(13) . . ? K2 K1 K2 129.4(2) 4_575 . ? O1U2 K1 U2 122.3(4) . 4_575 ? O1U1 K1 U2 97.3(4) . 4_575 ? O21 K1 U2 33.8(5) 4_575 4_575 ? O22 K1 U2 35.0(4) 4_575 4_575 ? O1 K1 U2 150.7(4) . 4_575 ? O2 K1 U2 128.3(3) . 4_575 ? C22 K1 U2 75.6(5) 4_575 4_575 ? U1 K1 U2 123.59(15) . 4_575 ? K2 K1 U2 55.20(12) 4_575 4_575 ? K2 K1 U2 165.1(2) . 4_575 ? O1U2 K1 U2 10.3(4) . . ? O1U1 K1 U2 140.0(5) . . ? O21 K1 U2 106.5(5) 4_575 . ? O22 K1 U2 141.4(4) 4_575 . ? O1 K1 U2 91.1(3) . . ? O2 K1 U2 84.5(3) . . ? C22 K1 U2 79.8(5) 4_575 . ? U1 K1 U2 113.22(15) . . ? K2 K1 U2 156.8(2) 4_575 . ? K2 K1 U2 51.83(11) . . ? U2 K1 U2 117.49(16) 4_575 . ? O1U1 K2 O1 115.5(6) 4_576 . ? O1U1 K2 O1U2 139.1(6) 4_576 . ? O1 K2 O1U2 96.0(6) . . ? O1U1 K2 O22 83.0(6) 4_576 . ? O1 K2 O22 157.9(6) . . ? O1U2 K2 O22 62.2(6) . . ? O1U1 K2 O2 136.0(6) 4_576 . ? O1 K2 O2 66.2(5) . . ? O1U2 K2 O2 79.3(5) . . ? O22 K2 O2 109.6(6) . . ? O1U1 K2 O21 87.4(6) 4_576 . ? O1 K2 O21 106.1(6) . . ? O1U2 K2 O21 57.8(6) . . ? O22 K2 O21 60.8(7) . . ? O2 K2 O21 136.0(6) . . ? O1U1 K2 C1 108.5(7) 4_576 . ? O1 K2 C1 18.4(6) . . ? O1U2 K2 C1 93.2(7) . . ? O22 K2 C1 147.9(7) . . ? O2 K2 C1 83.2(7) . . ? O21 K2 C1 89.2(8) . . ? O1U1 K2 C17 112.2(7) 4_576 . ? O1 K2 C17 108.1(6) . . ? O1U2 K2 C17 78.9(6) . . ? O22 K2 C17 72.6(7) . . ? O2 K2 C17 42.2(6) . . ? O21 K2 C17 126.7(7) . . ? C1 K2 C17 125.4(7) . . ? O1U1 K2 U2 110.3(4) 4_576 . ? O1 K2 U2 118.7(4) . . ? O1U2 K2 U2 28.8(4) . . ? O22 K2 U2 39.8(4) . . ? O2 K2 U2 104.6(4) . . ? O21 K2 U2 38.4(4) . . ? C1 K2 U2 109.3(5) . . ? C17 K2 U2 88.9(5) . . ? O1U1 K2 K1 45.9(4) 4_576 4_576 ? O1 K2 K1 136.1(4) . 4_576 ? O1U2 K2 K1 93.3(4) . 4_576 ? O22 K2 K1 49.2(4) . 4_576 ? O2 K2 K1 157.6(5) . 4_576 ? O21 K2 K1 46.6(4) . 4_576 ? C1 K2 K1 118.5(6) . 4_576 ? C17 K2 K1 115.8(5) . 4_576 ? U2 K2 K1 64.81(14) . 4_576 ? O1U1 K2 K1 164.0(6) 4_576 . ? O1 K2 K1 54.4(4) . . ? O1U2 K2 K1 43.2(4) . . ? O22 K2 K1 104.7(4) . . ? O2 K2 K1 55.1(4) . . ? O21 K2 K1 84.4(4) . . ? C1 K2 K1 57.8(5) . . ? C17 K2 K1 83.7(4) . . ? U2 K2 K1 70.63(14) . . ? K1 K2 K1 130.1(2) 4_576 . ? O1U1 K2 U1 123.5(4) 4_576 . ? O1 K2 U1 34.9(3) . . ? O1U2 K2 U1 97.3(4) . . ? O22 K2 U1 143.7(4) . . ? O2 K2 U1 34.2(4) . . ? O21 K2 U1 135.6(5) . . ? C1 K2 U1 53.2(6) . . ? C17 K2 U1 74.2(5) . . ? U2 K2 U1 126.08(15) . . ? K1 K2 U1 166.7(2) 4_576 . ? K1 K2 U1 57.06(12) . . ? C1 O1 U1 137(2) . . ? C1 O1 K2 118.4(19) . . ? U1 O1 K2 104.5(7) . . ? C1 O1 K1 97.3(18) . . ? U1 O1 K1 84.0(5) . . ? K2 O1 K1 82.6(5) . . ? C18 O2 U1 135.7(18) . . ? C18 O2 K2 110.4(15) . . ? U1 O2 K2 99.9(6) . . ? C18 O2 K1 133.0(18) . . ? U1 O2 K1 83.5(6) . . ? K2 O2 K1 78.1(4) . . ? C7 N1 C8 122(3) . . ? C7 N1 U1 125(2) . . ? C8 N1 U1 113.0(18) . . ? C9 N2 C19 113(3) . . ? C9 N2 C10 111(3) . . ? C19 N2 C10 110(3) . . ? C9 N2 U1 104.0(17) . . ? C19 N2 U1 113(2) . . ? C10 N2 U1 104(2) . . ? C12 N3 C11 120(2) . . ? C12 N3 U1 127.1(19) . . ? C11 N3 U1 112.5(18) . . ? O1 C1 C2 123(3) . . ? O1 C1 C6 120(3) . . ? C2 C1 C6 116(3) . . ? O1 C1 K2 43.3(15) . . ? C2 C1 K2 82(2) . . ? C6 C1 K2 151(2) . . ? C3 C2 C1 120(3) . . ? C2 C3 C4 123(3) . . ? C5 C4 C3 118(3) . . ? C6 C5 C4 123(4) . . ? C5 C6 C7 115(3) . . ? C5 C6 C1 120(3) . . ? C7 C6 C1 126(3) . . ? N1 C7 C6 131(3) . . ? N1 C8 C9 115(2) . . ? N2 C9 C8 110(3) . . ? C11 C10 N2 117(3) . . ? C10 C11 N3 111(2) . . ? N3 C12 C13 128(3) . . ? C14 C13 C12 116(3) . . ? C14 C13 C18 118(3) . . ? C12 C13 C18 126(3) . . ? C15 C14 C13 123(3) . . ? C14 C15 C16 119(3) . . ? C17 C16 C15 120(3) . . ? C16 C17 C18 124(3) . . ? C16 C17 K2 152(2) . . ? C18 C17 K2 83(2) . . ? O2 C18 C17 123(3) . . ? O2 C18 C13 121(3) . . ? C17 C18 C13 116(3) . . ? C21 O21 U2 137(2) . . ? C21 O21 K1 110.2(19) . 4_576 ? U2 O21 K1 102.6(10) . 4_576 ? C21 O21 K2 130(2) . . ? U2 O21 K2 82.0(7) . . ? K1 O21 K2 79.3(6) 4_576 . ? C38 O22 U2 145(2) . . ? C38 O22 K2 116.1(19) . . ? U2 O22 K2 89.0(6) . . ? C38 O22 K1 106.8(17) . 4_576 ? U2 O22 K1 98.9(7) . 4_576 ? K2 O22 K1 83.5(5) . 4_576 ? C27 N21 C28 110(4) . . ? C27 N21 U2 132(3) . . ? C28 N21 U2 115(3) . . ? C39 N22 C29 112(3) . . ? C39 N22 C30 110(3) . . ? C29 N22 C30 106(3) . . ? C39 N22 U2 114.2(15) . . ? C29 N22 U2 111(2) . . ? C30 N22 U2 102(2) . . ? C32 N23 C31 114(3) . . ? C32 N23 U2 128(2) . . ? C31 N23 U2 117(2) . . ? O21 C21 C22 118(3) . . ? O21 C21 C26 123(3) . . ? C22 C21 C26 118(3) . . ? C23 C22 C21 119(3) . . ? C23 C22 K1 149(2) . 4_576 ? C21 C22 K1 82(2) . 4_576 ? C22 C23 C24 124(3) . . ? C25 C24 C23 116(4) . . ? C24 C25 C26 127(4) . . ? C25 C26 C27 117(3) . . ? C25 C26 C21 116(3) . . ? C27 C26 C21 127(3) . . ? N21 C27 C26 124(4) . . ? N21 C28 C29 112(4) . . ? N22 C29 C28 105(3) . . ? C31 C30 N22 124(4) . . ? C30 C31 N23 109(4) . . ? N23 C32 C33 126(3) . . ? C32 C33 C34 113(3) . . ? C32 C33 C38 131(3) . . ? C34 C33 C38 115(3) . . ? C35 C34 C33 120(4) . . ? C34 C35 C36 125(4) . . ? C37 C36 C35 114(3) . . ? C38 C37 C36 125(3) . . ? O22 C38 C37 125(3) . . ? O22 C38 C33 116(3) . . ? C37 C38 C33 119(3) . . ? C45 N41 C41 120.1 . . ? C42 C41 N41 120.0 . . ? C41 C42 C43 119.9 . . ? C42 C43 C44 120.1 . . ? C45 C44 C43 120.0 . . ? C44 C45 N41 119.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.894 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.199 data_2 _database_code_depnum_ccdc_archive 'CCDC 851299' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H104 N16 O13 U4' _chemical_formula_weight 2642.07 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 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 27.5621(19) _cell_length_b 10.9547(8) _cell_length_c 30.626(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9246.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1075 _cell_measurement_theta_min 3.3227 _cell_measurement_theta_max 28.8525 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1 0 0 0.0046 1.0000 0.0000 -0.0000 -0.0055 -0.0005 0.0251 -1 0 0 0.0106 -1.0000 -0.0000 0.0000 0.0055 0.0005 -0.0251 -1 -1 0 0.0958 -1.0000 -1.0000 -0.0000 -0.0453 0.0393 -0.0354 1 1 0 0.0948 1.0000 1.0000 0.0000 0.0453 -0.0393 0.0354 -1 0 1 0.0097 -1.0000 -0.0000 1.0000 0.0190 0.0190 -0.0219 1 0 -1 0.0017 1.0000 0.0000 -1.0000 -0.0190 -0.0190 0.0219 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5056 _exptl_absorpt_coefficient_mu 7.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3175 _exptl_absorpt_correction_T_max 0.9264 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14335 _diffrn_reflns_av_R_equivalents 0.1045 _diffrn_reflns_av_sigmaI/netI 0.2274 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8400 _reflns_number_gt 4068 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 7.00 34.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - 16.8425 37.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega 17.00 74.00 1.0000 300.0000 omega____ theta____ kappa____ phi______ frames - 16.8425 37.0000 -60.0000 57 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8400 _refine_ls_number_parameters 585 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1989 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.1823 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N22 N 0.3169(6) 0.4320(15) 0.1299(6) 0.032(4) Uani 1 1 d . . . U1 U 0.45331(3) 0.55829(7) 0.04933(3) 0.0270(2) Uani 1 1 d . . . U2 U 0.35522(3) 0.65562(7) 0.14624(3) 0.0293(2) Uani 1 1 d . . . O1U O 0.4075(4) 0.6340(11) 0.1014(5) 0.031(4) Uani 1 1 d . . . O2U O 0.5000 0.5000 0.0000 0.032(5) Uani 1 2 d S . . O3U O 0.3062(5) 0.6666(12) 0.1856(5) 0.040(4) Uani 1 1 d . . . O1 O 0.3900(5) 0.4708(12) 0.0152(5) 0.038(4) Uani 1 1 d . . . O2 O 0.4611(5) 0.3772(12) 0.0836(5) 0.036(4) Uani 1 1 d . . . N1 N 0.4203(6) 0.7077(16) -0.0106(7) 0.041(5) Uani 1 1 d . . . N2 N 0.5025(6) 0.7685(14) 0.0459(6) 0.034(5) Uani 1 1 d . . . N3 N 0.5325(5) 0.5623(14) 0.0983(5) 0.024(4) Uani 1 1 d U . . C1 C 0.3586(7) 0.4787(17) -0.0185(8) 0.030(5) Uani 1 1 d . . . C2 C 0.3265(7) 0.385(2) -0.0257(8) 0.043(7) Uani 1 1 d . . . H2 H 0.3272 0.3147 -0.0076 0.051 Uiso 1 1 calc R . . C3 C 0.2929(7) 0.393(2) -0.0598(9) 0.052(8) Uani 1 1 d . . . H3 H 0.2721 0.3258 -0.0654 0.062 Uiso 1 1 calc R . . C4 C 0.2890(7) 0.500(2) -0.0862(9) 0.055(8) Uani 1 1 d . . . H4 H 0.2655 0.5072 -0.1087 0.067 Uiso 1 1 calc R . . C5 C 0.3213(8) 0.592(2) -0.0770(8) 0.046(7) Uani 1 1 d . . . H5 H 0.3199 0.6644 -0.0937 0.055 Uiso 1 1 calc R . . C6 C 0.3557(7) 0.5825(18) -0.0443(7) 0.029(5) Uani 1 1 d . . . C7 C 0.3874(7) 0.689(2) -0.0412(8) 0.040(6) Uani 1 1 d . . . H7 H 0.3839 0.7505 -0.0629 0.048 Uiso 1 1 calc R . . C8 C 0.4440(7) 0.829(2) -0.0145(8) 0.043(6) Uani 1 1 d . . . H8A H 0.4276 0.8893 0.0047 0.052 Uiso 1 1 calc R . . H8B H 0.4422 0.8589 -0.0449 0.052 Uiso 1 1 calc R . . C9 C 0.4983(7) 0.8136(19) -0.0003(8) 0.045(7) Uani 1 1 d . . . H9A H 0.5144 0.7550 -0.0201 0.054 Uiso 1 1 calc R . . H9B H 0.5152 0.8930 -0.0030 0.054 Uiso 1 1 calc R . . C10 C 0.4798(8) 0.8554(19) 0.0758(9) 0.059(8) Uani 1 1 d . . . H10A H 0.4723 0.8144 0.1034 0.088 Uiso 1 1 calc R . . H10B H 0.4498 0.8867 0.0627 0.088 Uiso 1 1 calc R . . H10C H 0.5021 0.9234 0.0813 0.088 Uiso 1 1 calc R . . C11 C 0.5531(7) 0.7436(18) 0.0536(9) 0.049(7) Uani 1 1 d . . . H11A H 0.5717 0.8209 0.0537 0.059 Uiso 1 1 calc R . . H11B H 0.5660 0.6912 0.0299 0.059 Uiso 1 1 calc R . . C12 C 0.5591(7) 0.6774(18) 0.0988(8) 0.039(6) Uani 1 1 d . . . H12A H 0.5939 0.6616 0.1045 0.047 Uiso 1 1 calc R . . H12B H 0.5465 0.7302 0.1224 0.047 Uiso 1 1 calc R . . C13 C 0.5509(8) 0.471(2) 0.1220(7) 0.042(6) Uani 1 1 d . . . H13 H 0.5803 0.4872 0.1371 0.051 Uiso 1 1 calc R . . C14 C 0.5314(7) 0.3513(19) 0.1269(7) 0.033(5) Uani 1 1 d . . . C15 C 0.5583(7) 0.2781(16) 0.1552(8) 0.039(6) Uani 1 1 d . . . H15 H 0.5874 0.3092 0.1676 0.046 Uiso 1 1 calc R . . C16 C 0.5439(8) 0.164(2) 0.1654(8) 0.051(7) Uani 1 1 d . . . H16 H 0.5631 0.1137 0.1838 0.061 Uiso 1 1 calc R . . C17 C 0.4994(7) 0.1200(18) 0.1480(8) 0.035(6) Uani 1 1 d . . . H17 H 0.4877 0.0416 0.1560 0.043 Uiso 1 1 calc R . . C18 C 0.4732(7) 0.1916(18) 0.1194(7) 0.031(5) Uani 1 1 d U . . H18 H 0.4445 0.1602 0.1065 0.037 Uiso 1 1 calc R . . C19 C 0.4883(8) 0.309(2) 0.1093(8) 0.039(6) Uani 1 1 d . . . O21 O 0.3439(4) 0.8499(12) 0.1217(4) 0.029(3) Uani 1 1 d U . . O22 O 0.4091(5) 0.7323(12) 0.1936(5) 0.043(4) Uani 1 1 d . . . N21 N 0.3009(5) 0.6543(14) 0.0787(6) 0.027(4) Uani 1 1 d U . . N23 N 0.4013(6) 0.4784(14) 0.1843(6) 0.037(5) Uani 1 1 d . . . C21 C 0.3424(6) 0.9040(17) 0.0845(6) 0.018(4) Uani 1 1 d U . . C22 C 0.3605(7) 1.0243(18) 0.0804(8) 0.033(5) Uani 1 1 d . . . H22 H 0.3733 1.0631 0.1057 0.040 Uiso 1 1 calc R . . C23 C 0.3605(8) 1.087(2) 0.0424(8) 0.040(6) Uani 1 1 d . . . H23 H 0.3740 1.1665 0.0413 0.048 Uiso 1 1 calc R . . C24 C 0.3408(8) 1.035(2) 0.0049(8) 0.046(7) Uani 1 1 d . . . H24 H 0.3409 1.0788 -0.0219 0.056 Uiso 1 1 calc R . . C25 C 0.3210(7) 0.9190(19) 0.0069(9) 0.040(6) Uani 1 1 d . . . H25 H 0.3053 0.8859 -0.0180 0.048 Uiso 1 1 calc R . . C26 C 0.3237(6) 0.8499(18) 0.0452(7) 0.024(5) Uani 1 1 d U . . C27 C 0.3000(6) 0.7305(17) 0.0465(8) 0.031(5) Uani 1 1 d U . . H27 H 0.2824 0.7066 0.0212 0.038 Uiso 1 1 calc R . . C28 C 0.2714(7) 0.5389(17) 0.0712(7) 0.032(5) Uani 1 1 d U . . H28A H 0.2413 0.5414 0.0888 0.038 Uiso 1 1 calc R . . H28B H 0.2623 0.5323 0.0400 0.038 Uiso 1 1 calc R . . C29 C 0.3015(8) 0.432(2) 0.0842(9) 0.054(8) Uani 1 1 d . . . H29A H 0.2827 0.3567 0.0785 0.065 Uiso 1 1 calc R . . H29B H 0.3307 0.4298 0.0654 0.065 Uiso 1 1 calc R . . C30 C 0.2746(6) 0.4090(17) 0.1597(7) 0.034(6) Uani 1 1 d U . . H30A H 0.2612 0.3278 0.1538 0.051 Uiso 1 1 calc R . . H30B H 0.2496 0.4709 0.1546 0.051 Uiso 1 1 calc R . . H30C H 0.2854 0.4132 0.1902 0.051 Uiso 1 1 calc R . . C31 C 0.3556(7) 0.3422(19) 0.1387(8) 0.044(6) Uani 1 1 d . . . H31A H 0.3804 0.3488 0.1154 0.053 Uiso 1 1 calc R . . H31B H 0.3415 0.2593 0.1371 0.053 Uiso 1 1 calc R . . C32 C 0.3802(8) 0.3564(19) 0.1821(8) 0.046(7) Uani 1 1 d . . . H32A H 0.3565 0.3453 0.2060 0.055 Uiso 1 1 calc R . . H32B H 0.4060 0.2941 0.1853 0.055 Uiso 1 1 calc R . . C33 C 0.4467(8) 0.4833(18) 0.1973(7) 0.033(5) Uani 1 1 d U . . H33 H 0.4626 0.4079 0.2030 0.039 Uiso 1 1 calc R . . C34 C 0.4749(9) 0.595(2) 0.2038(8) 0.046(7) Uani 1 1 d . . . C35 C 0.5241(9) 0.581(2) 0.2134(8) 0.049(7) Uani 1 1 d . . . H35 H 0.5369 0.5006 0.2154 0.059 Uiso 1 1 calc R . . C36 C 0.5554(9) 0.679(2) 0.2201(9) 0.055(7) Uani 1 1 d . . . H36 H 0.5887 0.6679 0.2269 0.066 Uiso 1 1 calc R . . C37 C 0.5348(8) 0.796(2) 0.2164(6) 0.040(6) Uani 1 1 d . . . H37 H 0.5553 0.8649 0.2195 0.048 Uiso 1 1 calc R . . C38 C 0.4872(8) 0.814(2) 0.2087(8) 0.044(7) Uani 1 1 d . . . H38 H 0.4748 0.8949 0.2080 0.053 Uiso 1 1 calc R . . C39 C 0.4553(7) 0.7143(18) 0.2015(6) 0.027(5) Uani 1 1 d U . . C53 C 0.6971(9) 0.597(2) 0.2708(10) 0.060(9) Uani 1 1 d . . . H53 H 0.7131 0.6388 0.2940 0.072 Uiso 1 1 calc R . . C52 C 0.6998(9) 0.631(3) 0.2285(8) 0.052(7) Uani 1 1 d . . . H52 H 0.7175 0.7029 0.2221 0.063 Uiso 1 1 calc R . . C51 C 0.6793(10) 0.571(2) 0.1942(9) 0.064(9) Uani 1 1 d . . . H51 H 0.6848 0.5988 0.1652 0.076 Uiso 1 1 calc R . . C54 C 0.6681(8) 0.495(2) 0.2765(8) 0.043(6) Uani 1 1 d U . . H54 H 0.6624 0.4651 0.3051 0.052 Uiso 1 1 calc R . . C55 C 0.6473(9) 0.437(2) 0.2410(9) 0.052(7) Uani 1 1 d . . . H55 H 0.6286 0.3660 0.2462 0.062 Uiso 1 1 calc R . . N51 N 0.6521(7) 0.475(2) 0.2011(7) 0.055(6) Uani 1 1 d . . . C44 C 0.6730(9) 0.082(4) 0.2061(11) 0.084(12) Uani 1 1 d . . . H44 H 0.6807 0.1132 0.2341 0.101 Uiso 1 1 calc R . . N41 N 0.6701(9) 0.113(3) 0.1284(10) 0.088(10) Uani 1 1 d . . . C41 C 0.6591(11) 0.000(3) 0.1253(11) 0.071(9) Uani 1 1 d . . . H41 H 0.6541 -0.0323 0.0968 0.085 Uiso 1 1 calc R . . C45 C 0.6760(10) 0.152(3) 0.1684(11) 0.064(8) Uani 1 1 d . . . H45 H 0.6828 0.2363 0.1722 0.077 Uiso 1 1 calc R . . C42 C 0.6539(10) -0.080(3) 0.1596(11) 0.069(9) Uani 1 1 d . . . H42 H 0.6472 -0.1636 0.1550 0.083 Uiso 1 1 calc R . . C43 C 0.6587(11) -0.034(4) 0.2001(12) 0.086(13) Uani 1 1 d . . . H43 H 0.6519 -0.0839 0.2247 0.104 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 N22 0.042(11) 0.024(10) 0.029(10) 0.009(10) 0.006(10) -0.018(8) U1 0.0273(4) 0.0216(4) 0.0321(4) -0.0015(5) 0.0039(4) 0.0007(3) U2 0.0300(4) 0.0228(4) 0.0350(4) -0.0026(5) 0.0048(5) 0.0003(4) O1U 0.034(8) 0.017(7) 0.042(9) 0.008(8) 0.007(7) 0.004(6) O2U 0.026(11) 0.026(11) 0.045(14) 0.011(12) 0.007(11) -0.008(9) O3U 0.041(9) 0.024(8) 0.055(10) 0.015(9) 0.003(8) 0.003(7) O1 0.039(9) 0.027(9) 0.046(10) 0.012(8) -0.023(8) 0.007(7) O2 0.028(8) 0.038(9) 0.042(9) 0.002(8) 0.005(8) -0.003(6) N1 0.029(11) 0.035(12) 0.059(14) -0.010(12) 0.006(11) 0.008(8) N2 0.043(11) 0.013(9) 0.047(12) 0.001(10) 0.030(11) 0.003(8) N3 0.028(7) 0.011(6) 0.034(8) -0.009(7) 0.005(7) -0.003(6) C1 0.030(12) 0.016(11) 0.044(14) 0.007(12) 0.005(13) -0.005(9) C2 0.033(13) 0.044(15) 0.051(16) 0.000(14) -0.007(13) -0.018(11) C3 0.014(12) 0.068(18) 0.07(2) -0.021(17) -0.013(14) -0.001(11) C4 0.015(12) 0.08(2) 0.07(2) 0.005(19) -0.020(14) 0.014(12) C5 0.039(15) 0.063(19) 0.035(14) -0.007(15) 0.018(14) 0.012(12) C6 0.028(11) 0.030(13) 0.028(12) -0.002(12) 0.002(12) 0.011(9) C7 0.029(12) 0.041(15) 0.049(16) -0.014(14) 0.003(13) 0.017(10) C8 0.024(12) 0.050(16) 0.056(15) 0.000(15) 0.011(12) 0.011(11) C9 0.037(13) 0.024(13) 0.075(19) 0.024(15) 0.005(14) -0.013(10) C10 0.068(17) 0.025(13) 0.08(2) 0.006(16) 0.039(17) -0.022(12) C11 0.024(12) 0.030(12) 0.09(2) 0.000(16) -0.001(15) -0.022(10) C12 0.022(11) 0.028(13) 0.067(17) -0.020(14) -0.021(12) 0.011(9) C13 0.028(12) 0.054(16) 0.044(14) 0.022(14) -0.019(13) -0.002(11) C14 0.043(13) 0.027(12) 0.028(12) 0.014(12) 0.002(11) -0.012(10) C15 0.039(13) 0.007(10) 0.070(18) -0.006(13) 0.004(14) -0.001(9) C16 0.053(15) 0.049(16) 0.052(16) 0.017(15) -0.022(14) -0.021(13) C17 0.035(12) 0.022(12) 0.049(14) 0.010(13) 0.001(13) 0.000(9) C18 0.028(8) 0.032(9) 0.032(9) 0.013(8) -0.001(7) -0.005(7) C19 0.044(15) 0.034(14) 0.037(14) 0.004(13) -0.007(13) -0.003(11) O21 0.038(7) 0.023(6) 0.027(6) 0.015(6) 0.001(6) -0.007(5) O22 0.056(10) 0.026(9) 0.048(10) -0.001(9) -0.012(9) 0.014(7) N21 0.028(7) 0.020(7) 0.032(8) 0.006(7) -0.001(7) 0.002(6) N23 0.052(12) 0.020(10) 0.040(11) 0.000(10) 0.021(11) 0.002(8) C21 0.015(6) 0.021(6) 0.018(6) -0.004(5) 0.003(5) 0.005(4) C22 0.031(12) 0.026(12) 0.041(13) -0.010(12) -0.008(12) 0.003(9) C23 0.043(14) 0.033(14) 0.044(15) -0.007(13) 0.009(14) -0.008(10) C24 0.053(16) 0.055(18) 0.031(13) -0.003(14) -0.017(13) 0.013(13) C25 0.032(13) 0.028(13) 0.060(17) -0.017(14) -0.011(13) 0.005(10) C26 0.016(7) 0.031(8) 0.026(8) -0.002(8) 0.010(7) 0.005(7) C27 0.021(8) 0.031(8) 0.042(9) -0.008(8) 0.005(8) -0.004(7) C28 0.035(8) 0.027(8) 0.034(9) -0.001(8) 0.001(8) -0.015(7) C29 0.035(14) 0.036(15) 0.09(2) -0.018(18) -0.008(16) 0.006(11) C30 0.024(8) 0.031(9) 0.048(10) -0.007(8) 0.014(8) 0.004(7) C31 0.033(12) 0.028(12) 0.071(18) -0.009(16) -0.009(14) -0.005(11) C32 0.056(16) 0.017(12) 0.065(18) 0.015(15) 0.004(15) -0.011(11) C33 0.035(9) 0.026(8) 0.037(9) 0.001(8) 0.011(8) 0.010(7) C34 0.064(17) 0.028(14) 0.048(16) -0.005(14) -0.009(15) 0.014(12) C35 0.056(16) 0.043(16) 0.048(16) -0.024(15) 0.005(15) -0.002(12) C36 0.046(15) 0.050(17) 0.068(19) -0.010(17) -0.013(15) -0.010(13) C37 0.045(16) 0.060(17) 0.015(11) 0.001(13) 0.010(12) -0.012(12) C38 0.041(14) 0.035(14) 0.057(16) 0.017(14) -0.023(14) -0.014(11) C39 0.028(8) 0.032(9) 0.020(8) 0.002(8) 0.010(8) -0.005(7) C53 0.044(16) 0.055(19) 0.08(2) -0.020(18) -0.039(17) 0.005(13) C52 0.065(18) 0.06(2) 0.032(14) -0.016(16) 0.017(14) 0.004(14) C51 0.11(2) 0.029(15) 0.052(18) 0.001(16) 0.049(18) 0.006(15) C54 0.044(9) 0.045(10) 0.041(10) 0.002(8) -0.021(8) 0.001(8) C55 0.068(17) 0.025(13) 0.063(17) 0.020(15) -0.009(17) -0.008(13) N51 0.053(14) 0.053(15) 0.060(15) 0.024(14) -0.020(14) 0.000(11) C44 0.036(17) 0.15(4) 0.06(2) 0.02(3) -0.022(17) 0.004(19) N41 0.075(19) 0.10(3) 0.09(2) 0.04(2) -0.025(18) 0.022(16) C41 0.12(3) 0.036(16) 0.055(19) 0.008(19) -0.01(2) 0.012(18) C45 0.058(19) 0.07(2) 0.07(2) 0.01(2) 0.011(18) 0.019(16) C42 0.07(2) 0.046(18) 0.09(2) -0.01(2) -0.01(2) 0.013(14) C43 0.07(2) 0.13(4) 0.06(2) 0.06(3) 0.01(2) -0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N22 C29 1.46(3) . ? N22 C31 1.48(2) . ? N22 C30 1.50(2) . ? N22 U2 2.714(16) . ? U1 O2U 2.0848(8) . ? U1 O1U 2.198(13) . ? U1 O1 2.250(14) . ? U1 O2 2.254(14) . ? U1 N1 2.62(2) . ? U1 N3 2.648(15) . ? U1 N2 2.675(15) . ? U2 O3U 1.816(14) . ? U2 O1U 2.003(13) . ? U2 O22 2.240(15) . ? U2 O21 2.278(13) . ? U2 N21 2.552(16) . ? U2 N23 2.596(17) . ? O2U U1 2.0848(8) 5_665 ? O1 C1 1.35(2) . ? O2 C19 1.32(2) . ? N1 C7 1.32(3) . ? N1 C8 1.49(2) . ? N2 C11 1.44(2) . ? N2 C10 1.46(3) . ? N2 C9 1.50(3) . ? N3 C13 1.34(2) . ? N3 C12 1.46(2) . ? C1 C2 1.37(3) . ? C1 C6 1.39(3) . ? C2 C3 1.40(3) . ? C3 C4 1.43(3) . ? C4 C5 1.37(3) . ? C5 C6 1.38(3) . ? C6 C7 1.46(3) . ? C8 C9 1.57(3) . ? C11 C12 1.57(3) . ? C13 C14 1.42(3) . ? C14 C19 1.39(3) . ? C14 C15 1.39(3) . ? C15 C16 1.35(3) . ? C16 C17 1.42(3) . ? C17 C18 1.38(3) . ? C18 C19 1.38(3) . ? O21 C21 1.28(2) . ? O22 C39 1.31(2) . ? N21 C27 1.29(2) . ? N21 C28 1.52(2) . ? N23 C33 1.32(2) . ? N23 C32 1.46(2) . ? C21 C22 1.41(2) . ? C21 C26 1.44(2) . ? C22 C23 1.35(3) . ? C23 C24 1.39(3) . ? C24 C25 1.38(3) . ? C25 C26 1.40(3) . ? C26 C27 1.46(2) . ? C28 C29 1.49(3) . ? C31 C32 1.50(3) . ? C33 C34 1.46(3) . ? C34 C35 1.40(3) . ? C34 C39 1.42(3) . ? C35 C36 1.40(3) . ? C36 C37 1.40(3) . ? C37 C38 1.35(3) . ? C38 C39 1.42(3) . ? C53 C52 1.35(3) . ? C53 C54 1.38(3) . ? C52 C51 1.36(3) . ? C51 N51 1.31(3) . ? C54 C55 1.38(3) . ? C55 N51 1.30(3) . ? C44 C43 1.34(4) . ? C44 C45 1.39(4) . ? N41 C41 1.29(3) . ? N41 C45 1.31(4) . ? C41 C42 1.37(4) . ? C42 C43 1.34(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C29 N22 C31 112.7(18) . . ? C29 N22 C30 110.8(17) . . ? C31 N22 C30 109.8(16) . . ? C29 N22 U2 106.8(13) . . ? C31 N22 U2 106.7(12) . . ? C30 N22 U2 110.0(12) . . ? O2U U1 O1U 175.3(3) . . ? O2U U1 O1 90.7(4) . . ? O1U U1 O1 93.0(5) . . ? O2U U1 O2 90.5(3) . . ? O1U U1 O2 92.8(5) . . ? O1 U1 O2 85.1(5) . . ? O2U U1 N1 84.1(4) . . ? O1U U1 N1 94.2(5) . . ? O1 U1 N1 70.8(5) . . ? O2 U1 N1 155.2(6) . . ? O2U U1 N3 84.6(3) . . ? O1U U1 N3 93.2(5) . . ? O1 U1 N3 155.5(5) . . ? O2 U1 N3 70.9(5) . . ? N1 U1 N3 132.2(5) . . ? O2U U1 N2 85.5(4) . . ? O1U U1 N2 89.7(5) . . ? O1 U1 N2 137.9(5) . . ? O2 U1 N2 136.7(5) . . ? N1 U1 N2 67.1(6) . . ? N3 U1 N2 65.8(5) . . ? O3U U2 O1U 176.5(6) . . ? O3U U2 O22 92.2(6) . . ? O1U U2 O22 90.7(5) . . ? O3U U2 O21 93.2(5) . . ? O1U U2 O21 89.0(5) . . ? O22 U2 O21 87.4(5) . . ? O3U U2 N21 95.9(6) . . ? O1U U2 N21 82.3(5) . . ? O22 U2 N21 156.3(5) . . ? O21 U2 N21 70.0(5) . . ? O3U U2 N23 96.6(6) . . ? O1U U2 N23 82.4(5) . . ? O22 U2 N23 70.5(5) . . ? O21 U2 N23 156.0(5) . . ? N21 U2 N23 130.2(5) . . ? O3U U2 N22 83.8(6) . . ? O1U U2 N22 92.7(5) . . ? O22 U2 N22 135.7(5) . . ? O21 U2 N22 136.8(5) . . ? N21 U2 N22 67.5(5) . . ? N23 U2 N22 66.3(6) . . ? U2 O1U U1 162.8(7) . . ? U1 O2U U1 180.00(4) 5_665 . ? C1 O1 U1 145.7(12) . . ? C19 O2 U1 146.2(13) . . ? C7 N1 C8 112.5(19) . . ? C7 N1 U1 129.8(15) . . ? C8 N1 U1 117.5(14) . . ? C11 N2 C10 115.9(19) . . ? C11 N2 C9 106.9(17) . . ? C10 N2 C9 110.0(17) . . ? C11 N2 U1 108.7(11) . . ? C10 N2 U1 108.6(11) . . ? C9 N2 U1 106.3(12) . . ? C13 N3 C12 116.9(17) . . ? C13 N3 U1 127.4(13) . . ? C12 N3 U1 115.7(12) . . ? O1 C1 C2 119(2) . . ? O1 C1 C6 121.7(18) . . ? C2 C1 C6 119(2) . . ? C1 C2 C3 120(2) . . ? C2 C3 C4 122(2) . . ? C5 C4 C3 116(2) . . ? C4 C5 C6 123(2) . . ? C5 C6 C1 121(2) . . ? C5 C6 C7 114(2) . . ? C1 C6 C7 126(2) . . ? N1 C7 C6 125(2) . . ? N1 C8 C9 107.4(16) . . ? N2 C9 C8 111.8(17) . . ? N2 C11 C12 109.4(17) . . ? N3 C12 C11 109.7(17) . . ? N3 C13 C14 127(2) . . ? C19 C14 C15 120.2(19) . . ? C19 C14 C13 126(2) . . ? C15 C14 C13 113.2(19) . . ? C16 C15 C14 121(2) . . ? C15 C16 C17 119(2) . . ? C18 C17 C16 119.8(19) . . ? C19 C18 C17 121(2) . . ? O2 C19 C18 119(2) . . ? O2 C19 C14 122(2) . . ? C18 C19 C14 119(2) . . ? C21 O21 U2 136.8(12) . . ? C39 O22 U2 135.0(13) . . ? C27 N21 C28 114.2(17) . . ? C27 N21 U2 128.8(13) . . ? C28 N21 U2 116.2(12) . . ? C33 N23 C32 115.5(18) . . ? C33 N23 U2 124.8(13) . . ? C32 N23 U2 118.1(14) . . ? O21 C21 C22 119.9(18) . . ? O21 C21 C26 124.3(17) . . ? C22 C21 C26 115.8(18) . . ? C23 C22 C21 123(2) . . ? C22 C23 C24 120(2) . . ? C25 C24 C23 119(2) . . ? C24 C25 C26 121(2) . . ? C25 C26 C21 119.9(18) . . ? C25 C26 C27 119(2) . . ? C21 C26 C27 120.4(19) . . ? N21 C27 C26 126(2) . . ? C29 C28 N21 108.3(16) . . ? N22 C29 C28 115(2) . . ? N22 C31 C32 114.8(19) . . ? N23 C32 C31 108.4(19) . . ? N23 C33 C34 125.6(19) . . ? C35 C34 C39 119(2) . . ? C35 C34 C33 117(2) . . ? C39 C34 C33 124(2) . . ? C36 C35 C34 123(2) . . ? C35 C36 C37 116(2) . . ? C38 C37 C36 123(2) . . ? C37 C38 C39 121(2) . . ? O22 C39 C34 121.2(19) . . ? O22 C39 C38 120.9(19) . . ? C34 C39 C38 118(2) . . ? C52 C53 C54 112(3) . . ? C53 C52 C51 126(3) . . ? N51 C51 C52 120(3) . . ? C53 C54 C55 121(2) . . ? N51 C55 C54 124(2) . . ? C55 N51 C51 118(2) . . ? C43 C44 C45 115(3) . . ? C41 N41 C45 114(3) . . ? N41 C41 C42 126(3) . . ? N41 C45 C44 126(4) . . ? C43 C42 C41 117(3) . . ? C44 C43 C42 121(3) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 2.427 _refine_diff_density_min -1.438 _refine_diff_density_rms 0.249 data_3 _database_code_depnum_ccdc_archive 'CCDC 851300' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 N6 O8 U2' _chemical_formula_weight 1186.84 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3093(7) _cell_length_b 10.8301(2) _cell_length_c 22.1561(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.356(3) _cell_angle_gamma 90.00 _cell_volume 3773.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6433 _cell_measurement_theta_min 3.3054 _cell_measurement_theta_max 32.3061 _exptl_crystal_description bloc _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 8.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2571 _exptl_absorpt_correction_T_max 0.5873 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18306 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 30.51 _reflns_number_total 11399 _reflns_number_gt 8853 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -26.00 75.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 0.0000 -120.0000 101 #__ type_ start__ end____ width___ exp.time_ 2 omega -5.00 96.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 25.4051 77.0000 -150.0000 101 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0192P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11399 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 0.100812(12) 0.425262(15) 0.222647(7) 0.01964(5) Uani 1 1 d . . . O1U1 O 0.1739(2) 0.4565(3) 0.17724(14) 0.0281(8) Uani 1 1 d . . . O2U1 O 0.0345(2) 0.3777(3) 0.27049(14) 0.0298(8) Uani 1 1 d . . . O1 O 0.1372(2) 0.6001(3) 0.27501(14) 0.0303(8) Uani 1 1 d . . . O2 O -0.0036(2) 0.5355(3) 0.16199(14) 0.0324(9) Uani 1 1 d . . . N1 N 0.2279(3) 0.3847(4) 0.32005(17) 0.0254(9) Uani 1 1 d . . . N2 N 0.1544(3) 0.1974(3) 0.22806(18) 0.0245(9) Uani 1 1 d . . . N3 N 0.0166(3) 0.2891(4) 0.13180(19) 0.0295(10) Uani 1 1 d . . . C1 C 0.1827(3) 0.6539(4) 0.32594(19) 0.0211(10) Uani 1 1 d . . . C2 C 0.1736(3) 0.7809(4) 0.3340(2) 0.0238(10) Uani 1 1 d . . . H2 H 0.1349 0.8275 0.3026 0.029 Uiso 1 1 calc R . . C3 C 0.2213(3) 0.8387(5) 0.3880(2) 0.0290(11) Uani 1 1 d . . . H3 H 0.2149 0.9249 0.3932 0.035 Uiso 1 1 calc R . . C4 C 0.2777(4) 0.7727(5) 0.4343(2) 0.0344(13) Uani 1 1 d . . . H4 H 0.3093 0.8129 0.4713 0.041 Uiso 1 1 calc R . . C5 C 0.2877(3) 0.6478(5) 0.4262(2) 0.0303(12) Uani 1 1 d . . . H5 H 0.3272 0.6029 0.4578 0.036 Uiso 1 1 calc R . . C6 C 0.2417(3) 0.5855(4) 0.37280(19) 0.0211(10) Uani 1 1 d . . . C7 C 0.2592(3) 0.4561(5) 0.3661(2) 0.0278(11) Uani 1 1 d . . . H7 H 0.2992 0.4195 0.4005 0.033 Uiso 1 1 calc R . . C8 C 0.2629(4) 0.2580(5) 0.3245(2) 0.0397(14) Uani 1 1 d . . . H8A H 0.2861 0.2357 0.3691 0.048 Uiso 1 1 calc R . . H8B H 0.3101 0.2550 0.3042 0.048 Uiso 1 1 calc R . . C9 C 0.1958(5) 0.1665(5) 0.2937(2) 0.0485(17) Uani 1 1 d . . . H9A H 0.2220 0.0836 0.2955 0.058 Uiso 1 1 calc R . . H9B H 0.1521 0.1628 0.3174 0.058 Uiso 1 1 calc R . . C10 C 0.0763(4) 0.1215(5) 0.2054(3) 0.0474(16) Uani 1 1 d . . . H10A H 0.0383 0.1347 0.2330 0.057 Uiso 1 1 calc R . . H10B H 0.0920 0.0330 0.2073 0.057 Uiso 1 1 calc R . . C11 C 0.0294(4) 0.1554(5) 0.1382(3) 0.0434(15) Uani 1 1 d . . . H11A H 0.0628 0.1270 0.1094 0.052 Uiso 1 1 calc R . . H11B H -0.0264 0.1132 0.1264 0.052 Uiso 1 1 calc R . . C12 C -0.0334(4) 0.3253(5) 0.0794(2) 0.0342(13) Uani 1 1 d . . . H12 H -0.0551 0.2624 0.0496 0.041 Uiso 1 1 calc R . . C13 C -0.0602(3) 0.4492(5) 0.0605(2) 0.0292(12) Uani 1 1 d . . . C14 C -0.1092(3) 0.4683(6) -0.0014(2) 0.0377(14) Uani 1 1 d . . . H14 H -0.1209 0.4004 -0.0295 0.045 Uiso 1 1 calc R . . C15 C -0.1404(4) 0.5833(6) -0.0220(2) 0.0402(15) Uani 1 1 d . . . H15 H -0.1721 0.5950 -0.0642 0.048 Uiso 1 1 calc R . . C16 C -0.1249(3) 0.6817(5) 0.0193(2) 0.0334(13) Uani 1 1 d . . . H16 H -0.1459 0.7614 0.0052 0.040 Uiso 1 1 calc R . . C17 C -0.0793(3) 0.6654(5) 0.0811(2) 0.0293(11) Uani 1 1 d . . . H17 H -0.0707 0.7332 0.1092 0.035 Uiso 1 1 calc R . . C18 C -0.0459(3) 0.5501(5) 0.1021(2) 0.0250(11) Uani 1 1 d . . . C19 C 0.2128(4) 0.1725(5) 0.1882(3) 0.0465(16) Uani 1 1 d . . . H19A H 0.2673 0.2138 0.2060 0.070 Uiso 1 1 calc R . . H19B H 0.1875 0.2039 0.1458 0.070 Uiso 1 1 calc R . . H19C H 0.2220 0.0833 0.1864 0.070 Uiso 1 1 calc R . . U2 U 0.426349(11) 0.701056(15) 0.123007(7) 0.01704(4) Uani 1 1 d . B . O1U2 O 0.5141(2) 0.7820(3) 0.17249(14) 0.0277(8) Uani 1 1 d . . . O2U2 O 0.3426(2) 0.6076(3) 0.07909(13) 0.0235(7) Uani 1 1 d . . . O21 O 0.3421(2) 0.8675(3) 0.11083(14) 0.0247(7) Uani 1 1 d . . . O22 O 0.4608(2) 0.7596(3) 0.03682(14) 0.0274(8) Uani 1 1 d . . . N21 N 0.3431(3) 0.7000(3) 0.20614(16) 0.0235(9) Uani 1 1 d . B . N22 N 0.4637(3) 0.5200(4) 0.20384(16) 0.0257(9) Uani 1 1 d . . . N23 N 0.5366(3) 0.5493(3) 0.10062(16) 0.0211(8) Uani 1 1 d . . . C21 C 0.2589(3) 0.8705(4) 0.1016(2) 0.0206(10) Uani 1 1 d . . . C22 C 0.2080(3) 0.9431(4) 0.0530(2) 0.0261(11) Uani 1 1 d . . . H22 H 0.2344 0.9914 0.0276 0.031 Uiso 1 1 calc R . . C23 C 0.1215(4) 0.9454(4) 0.0417(2) 0.0292(12) Uani 1 1 d . . . H23 H 0.0887 0.9928 0.0078 0.035 Uiso 1 1 calc R . . C24 C 0.0807(4) 0.8790(5) 0.0794(2) 0.0332(12) Uani 1 1 d . . . H24 H 0.0206 0.8808 0.0713 0.040 Uiso 1 1 calc R . . C25 C 0.1290(3) 0.8112(4) 0.1281(2) 0.0277(11) Uani 1 1 d . . . H25 H 0.1017 0.7680 0.1547 0.033 Uiso 1 1 calc R . . C26 C 0.2173(3) 0.8037(4) 0.1398(2) 0.0227(10) Uani 1 1 d . . . C27 C 0.2633(3) 0.7311(4) 0.1929(2) 0.0231(10) Uani 1 1 d . . . H27 H 0.2320 0.7033 0.2209 0.028 Uiso 1 1 calc R . . C28 C 0.3761(4) 0.6277(5) 0.2634(2) 0.0305(12) Uani 1 1 d . . . H28A H 0.3355 0.5606 0.2652 0.037 Uiso 1 1 calc R A 1 H28B H 0.3812 0.6815 0.3003 0.037 Uiso 1 1 calc R A 1 C29 C 0.4624(5) 0.5722(6) 0.2656(3) 0.0253(17) Uani 0.703(7) 1 d P B 1 H29A H 0.5067 0.6368 0.2777 0.030 Uiso 0.703(7) 1 calc PR B 1 H29B H 0.4756 0.5063 0.2976 0.030 Uiso 0.703(7) 1 calc PR B 1 C30 C 0.5436(5) 0.4650(7) 0.2038(3) 0.0272(17) Uani 0.703(7) 1 d P B 1 H30A H 0.5511 0.3883 0.2290 0.033 Uiso 0.703(7) 1 calc PR B 1 H30B H 0.5900 0.5223 0.2240 0.033 Uiso 0.703(7) 1 calc PR B 1 C31 C 0.5508(3) 0.4345(4) 0.1385(2) 0.0264(11) Uani 1 1 d . B . H31A H 0.6080 0.4007 0.1407 0.032 Uiso 1 1 calc R C 1 H31B H 0.5079 0.3717 0.1189 0.032 Uiso 1 1 calc R C 1 C32 C 0.5832(3) 0.5623(4) 0.0623(2) 0.0228(10) Uani 1 1 d . B . H32 H 0.6210 0.4962 0.0608 0.027 Uiso 1 1 calc R . . C33 C 0.5849(3) 0.6655(4) 0.02114(19) 0.0199(9) Uani 1 1 d . . . C34 C 0.6500(3) 0.6694(4) -0.0091(2) 0.0249(10) Uani 1 1 d . B . H34 H 0.6902 0.6041 -0.0028 0.030 Uiso 1 1 calc R . . C35 C 0.6572(3) 0.7665(5) -0.0482(2) 0.0288(11) Uani 1 1 d . . . H35 H 0.7030 0.7692 -0.0672 0.035 Uiso 1 1 calc R B . C36 C 0.5975(3) 0.8579(4) -0.0591(2) 0.0266(11) Uani 1 1 d . B . H36 H 0.6018 0.9239 -0.0864 0.032 Uiso 1 1 calc R . . C37 C 0.5303(3) 0.8565(4) -0.03104(19) 0.0228(10) Uani 1 1 d . . . H37 H 0.4891 0.9206 -0.0397 0.027 Uiso 1 1 calc R B . C38 C 0.5236(3) 0.7609(4) 0.00976(19) 0.0206(10) Uani 1 1 d . B . C39 C 0.3932(5) 0.4177(6) 0.1877(3) 0.0223(16) Uani 0.703(7) 1 d P B 1 H39A H 0.4053 0.3545 0.2206 0.034 Uiso 0.703(7) 1 calc PR B 1 H39B H 0.3927 0.3797 0.1475 0.034 Uiso 0.703(7) 1 calc PR B 1 H39C H 0.3376 0.4549 0.1851 0.034 Uiso 0.703(7) 1 calc PR B 1 C39B C 0.5526(10) 0.5553(14) 0.2558(7) 0.023(4) Uani 0.297(7) 1 d P B 2 H39D H 0.5446 0.6311 0.2777 0.034 Uiso 0.297(7) 1 calc PR B 2 H39E H 0.5976 0.5683 0.2346 0.034 Uiso 0.297(7) 1 calc PR B 2 H39F H 0.5688 0.4878 0.2860 0.034 Uiso 0.297(7) 1 calc PR B 2 C30B C 0.4824(14) 0.4150(15) 0.1717(8) 0.034(5) Uani 0.297(7) 1 d P B 2 H30C H 0.4297 0.3888 0.1405 0.041 Uiso 0.297(7) 1 calc PR B 2 H30D H 0.5000 0.3468 0.2021 0.041 Uiso 0.297(7) 1 calc PR B 2 C29B C 0.4043(12) 0.5096(17) 0.2374(8) 0.033(5) Uani 0.297(7) 1 d P B 2 H29C H 0.4274 0.4531 0.2729 0.040 Uiso 0.297(7) 1 calc PR B 2 H29D H 0.3532 0.4696 0.2102 0.040 Uiso 0.297(7) 1 calc PR B 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 0.02264(10) 0.01838(8) 0.01755(8) -0.00092(6) 0.00467(7) 0.00018(7) O1U1 0.033(2) 0.0286(18) 0.0241(16) -0.0019(14) 0.0101(15) -0.0074(17) O2U1 0.032(2) 0.0287(18) 0.0330(18) 0.0005(15) 0.0166(16) 0.0031(17) O1 0.038(2) 0.0231(18) 0.0230(17) -0.0022(14) -0.0046(15) 0.0034(16) O2 0.036(2) 0.0262(18) 0.0275(18) 0.0001(15) -0.0057(15) 0.0052(17) N1 0.030(2) 0.024(2) 0.021(2) 0.0049(16) 0.0045(17) 0.0061(19) N2 0.027(2) 0.021(2) 0.031(2) 0.0023(17) 0.0159(18) -0.0011(18) N3 0.028(2) 0.027(2) 0.033(2) -0.0105(18) 0.0057(19) 0.000(2) C1 0.019(2) 0.029(2) 0.014(2) -0.0039(18) 0.0035(18) -0.007(2) C2 0.019(3) 0.032(3) 0.019(2) -0.0065(19) 0.0023(18) 0.003(2) C3 0.032(3) 0.032(3) 0.024(2) -0.008(2) 0.009(2) -0.009(2) C4 0.034(3) 0.048(3) 0.018(2) -0.005(2) 0.001(2) -0.013(3) C5 0.027(3) 0.042(3) 0.020(2) 0.006(2) 0.004(2) -0.009(3) C6 0.026(3) 0.026(2) 0.014(2) 0.0024(18) 0.0090(18) -0.001(2) C7 0.026(3) 0.037(3) 0.019(2) 0.010(2) 0.003(2) 0.007(2) C8 0.045(4) 0.036(3) 0.034(3) 0.003(2) 0.003(3) 0.016(3) C9 0.077(5) 0.031(3) 0.039(3) 0.009(3) 0.018(3) 0.014(3) C10 0.042(4) 0.024(3) 0.085(5) -0.003(3) 0.031(3) -0.005(3) C11 0.040(4) 0.028(3) 0.056(4) -0.018(3) 0.002(3) 0.001(3) C12 0.029(3) 0.038(3) 0.035(3) -0.022(2) 0.008(2) -0.003(3) C13 0.024(3) 0.045(3) 0.019(2) -0.009(2) 0.007(2) -0.004(2) C14 0.026(3) 0.063(4) 0.024(3) -0.015(3) 0.008(2) -0.005(3) C15 0.030(3) 0.071(4) 0.017(2) 0.004(3) 0.004(2) 0.000(3) C16 0.022(3) 0.049(3) 0.028(3) 0.013(2) 0.004(2) -0.003(3) C17 0.020(3) 0.038(3) 0.026(2) 0.000(2) -0.002(2) -0.007(2) C18 0.017(2) 0.034(3) 0.025(2) 0.003(2) 0.0069(19) -0.003(2) C19 0.051(4) 0.038(3) 0.059(4) -0.001(3) 0.028(3) 0.015(3) U2 0.01922(9) 0.01524(8) 0.01609(8) 0.00205(6) 0.00370(6) 0.00027(7) O1U2 0.026(2) 0.0271(18) 0.0275(17) -0.0042(14) 0.0038(15) -0.0043(16) O2U2 0.0255(19) 0.0205(16) 0.0221(16) 0.0025(13) 0.0021(14) -0.0037(15) O21 0.026(2) 0.0175(16) 0.0344(18) 0.0071(14) 0.0139(15) 0.0041(15) O22 0.028(2) 0.0295(18) 0.0276(17) 0.0117(14) 0.0126(15) 0.0103(16) N21 0.034(3) 0.0199(19) 0.0206(19) 0.0037(16) 0.0143(18) -0.0025(19) N22 0.034(3) 0.022(2) 0.0187(19) 0.0048(16) 0.0032(17) 0.0028(19) N23 0.023(2) 0.0163(19) 0.0209(18) 0.0049(15) 0.0005(16) 0.0052(17) C21 0.027(3) 0.013(2) 0.024(2) -0.0032(17) 0.010(2) 0.0006(19) C22 0.029(3) 0.023(2) 0.029(2) 0.000(2) 0.011(2) 0.004(2) C23 0.034(3) 0.021(2) 0.029(3) -0.003(2) 0.002(2) 0.008(2) C24 0.025(3) 0.023(3) 0.050(3) -0.004(2) 0.008(2) -0.002(2) C25 0.033(3) 0.018(2) 0.037(3) -0.002(2) 0.018(2) 0.000(2) C26 0.028(3) 0.014(2) 0.028(2) -0.0011(18) 0.011(2) -0.001(2) C27 0.027(3) 0.021(2) 0.024(2) -0.0012(18) 0.012(2) -0.006(2) C28 0.046(4) 0.025(3) 0.026(2) 0.005(2) 0.019(2) 0.002(2) C29 0.036(5) 0.023(3) 0.014(3) 0.002(3) 0.002(3) 0.001(3) C30 0.024(4) 0.025(4) 0.030(4) 0.005(3) 0.003(3) 0.000(3) C31 0.025(3) 0.021(2) 0.035(3) 0.004(2) 0.012(2) 0.006(2) C32 0.020(3) 0.018(2) 0.028(2) -0.0021(19) 0.002(2) 0.003(2) C33 0.021(3) 0.017(2) 0.020(2) -0.0034(17) 0.0036(18) -0.0050(19) C34 0.024(3) 0.022(2) 0.028(2) -0.003(2) 0.007(2) 0.001(2) C35 0.027(3) 0.030(3) 0.032(3) -0.003(2) 0.013(2) -0.007(2) C36 0.034(3) 0.024(2) 0.023(2) -0.0017(19) 0.009(2) -0.009(2) C37 0.026(3) 0.018(2) 0.024(2) -0.0007(18) 0.006(2) 0.003(2) C38 0.027(3) 0.018(2) 0.017(2) -0.0046(17) 0.0065(19) -0.004(2) C39 0.026(4) 0.020(3) 0.020(3) -0.003(3) 0.004(3) -0.005(3) C39B 0.018(8) 0.027(9) 0.018(7) 0.011(6) -0.004(6) -0.003(7) C30B 0.059(15) 0.015(8) 0.027(9) 0.008(7) 0.008(9) 0.000(9) C29B 0.020(9) 0.043(11) 0.037(10) 0.017(9) 0.007(8) 0.017(9) _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 O2U1 1.779(3) . ? U1 O1U1 1.784(3) . ? U1 O1 2.218(3) . ? U1 O2 2.218(3) . ? U1 N3 2.578(4) . ? U1 N1 2.604(4) . ? U1 N2 2.609(4) . ? O1 C1 1.311(5) . ? O2 C18 1.333(5) . ? N1 C7 1.274(6) . ? N1 C8 1.478(6) . ? N2 C9 1.471(6) . ? N2 C10 1.486(7) . ? N2 C19 1.486(6) . ? N3 C12 1.290(6) . ? N3 C11 1.464(7) . ? C1 C2 1.400(6) . ? C1 C6 1.422(6) . ? C2 C3 1.392(6) . ? C3 C4 1.382(7) . ? C4 C5 1.380(7) . ? C5 C6 1.395(6) . ? C6 C7 1.446(6) . ? C8 C9 1.500(8) . ? C10 C11 1.527(8) . ? C12 C13 1.439(7) . ? C13 C14 1.407(7) . ? C13 C18 1.408(7) . ? C14 C15 1.377(8) . ? C15 C16 1.384(8) . ? C16 C17 1.384(6) . ? C17 C18 1.392(7) . ? U2 O2U2 1.770(3) . ? U2 O1U2 1.786(3) . ? U2 O22 2.221(3) . ? U2 O21 2.239(3) . ? U2 N21 2.561(4) . ? U2 N23 2.580(4) . ? U2 N22 2.616(4) . ? O21 C21 1.319(6) . ? O22 C38 1.318(6) . ? N21 C27 1.302(6) . ? N21 C28 1.466(6) . ? N22 C29B 1.372(17) . ? N22 C30B 1.418(17) . ? N22 C30 1.434(8) . ? N22 C29 1.485(7) . ? N22 C39 1.568(7) . ? N22 C39B 1.640(15) . ? N23 C32 1.289(6) . ? N23 C31 1.484(5) . ? C21 C22 1.413(6) . ? C21 C26 1.416(6) . ? C22 C23 1.365(7) . ? C23 C24 1.396(7) . ? C24 C25 1.370(7) . ? C25 C26 1.396(7) . ? C26 C27 1.448(6) . ? C28 C29 1.519(9) . ? C28 C29B 1.523(19) . ? C30 C31 1.518(8) . ? C31 C30B 1.51(2) . ? C32 C33 1.447(6) . ? C33 C34 1.398(6) . ? C33 C38 1.413(6) . ? C34 C35 1.386(6) . ? C35 C36 1.364(7) . ? C36 C37 1.397(7) . ? C37 C38 1.398(6) . ? 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 O2U1 U1 O1U1 173.30(15) . . ? O2U1 U1 O1 93.24(14) . . ? O1U1 U1 O1 90.37(14) . . ? O2U1 U1 O2 91.52(15) . . ? O1U1 U1 O2 94.41(15) . . ? O1 U1 O2 85.05(12) . . ? O2U1 U1 N3 91.00(15) . . ? O1U1 U1 N3 88.02(14) . . ? O1 U1 N3 155.51(13) . . ? O2 U1 N3 70.73(13) . . ? O2U1 U1 N1 86.18(14) . . ? O1U1 U1 N1 89.72(14) . . ? O1 U1 N1 70.52(12) . . ? O2 U1 N1 155.26(12) . . ? N3 U1 N1 133.87(13) . . ? O2U1 U1 N2 86.99(14) . . ? O1U1 U1 N2 86.56(14) . . ? O1 U1 N2 138.01(13) . . ? O2 U1 N2 136.94(13) . . ? N3 U1 N2 66.28(13) . . ? N1 U1 N2 67.59(12) . . ? C1 O1 U1 147.3(3) . . ? C18 O2 U1 141.1(3) . . ? C7 N1 C8 116.4(4) . . ? C7 N1 U1 128.5(3) . . ? C8 N1 U1 114.9(3) . . ? C9 N2 C10 109.6(4) . . ? C9 N2 C19 110.4(5) . . ? C10 N2 C19 108.9(4) . . ? C9 N2 U1 108.7(3) . . ? C10 N2 U1 105.1(3) . . ? C19 N2 U1 113.8(3) . . ? C12 N3 C11 115.3(4) . . ? C12 N3 U1 127.4(3) . . ? C11 N3 U1 117.2(3) . . ? O1 C1 C2 119.4(4) . . ? O1 C1 C6 121.1(4) . . ? C2 C1 C6 119.6(4) . . ? C3 C2 C1 119.8(4) . . ? C4 C3 C2 121.1(5) . . ? C5 C4 C3 119.2(5) . . ? C4 C5 C6 121.9(5) . . ? C5 C6 C1 118.4(4) . . ? C5 C6 C7 118.6(4) . . ? C1 C6 C7 122.9(4) . . ? N1 C7 C6 128.5(4) . . ? N1 C8 C9 111.1(5) . . ? N2 C9 C8 112.8(5) . . ? N2 C10 C11 111.1(5) . . ? N3 C11 C10 110.7(4) . . ? N3 C12 C13 128.1(5) . . ? C14 C13 C18 118.4(5) . . ? C14 C13 C12 118.1(5) . . ? C18 C13 C12 123.2(4) . . ? C15 C14 C13 121.4(5) . . ? C14 C15 C16 119.3(5) . . ? C15 C16 C17 120.8(5) . . ? C16 C17 C18 120.4(5) . . ? O2 C18 C17 119.5(4) . . ? O2 C18 C13 120.8(5) . . ? C17 C18 C13 119.6(4) . . ? O2U2 U2 O1U2 174.13(14) . . ? O2U2 U2 O22 91.42(13) . . ? O1U2 U2 O22 92.49(14) . . ? O2U2 U2 O21 91.98(14) . . ? O1U2 U2 O21 92.58(14) . . ? O22 U2 O21 87.31(11) . . ? O2U2 U2 N21 85.06(14) . . ? O1U2 U2 N21 92.98(14) . . ? O22 U2 N21 157.30(12) . . ? O21 U2 N21 70.45(12) . . ? O2U2 U2 N23 90.36(14) . . ? O1U2 U2 N23 86.81(14) . . ? O22 U2 N23 70.65(12) . . ? O21 U2 N23 157.89(11) . . ? N21 U2 N23 131.66(12) . . ? O2U2 U2 N22 87.34(13) . . ? O1U2 U2 N22 86.81(14) . . ? O22 U2 N22 137.46(12) . . ? O21 U2 N22 135.23(12) . . ? N21 U2 N22 64.90(13) . . ? N23 U2 N22 66.84(12) . . ? C21 O21 U2 127.7(3) . . ? C38 O22 U2 143.0(3) . . ? C27 N21 C28 116.7(4) . . ? C27 N21 U2 121.7(3) . . ? C28 N21 U2 118.8(3) . . ? C29B N22 C30B 118.9(12) . . ? C29B N22 C30 137.6(8) . . ? C30B N22 C30 49.4(9) . . ? C29B N22 C29 49.3(9) . . ? C30B N22 C29 145.7(8) . . ? C30 N22 C29 113.2(5) . . ? C29B N22 C39 59.1(9) . . ? C30B N22 C39 63.9(9) . . ? C30 N22 C39 108.5(5) . . ? C29 N22 C39 106.9(5) . . ? C29B N22 C39B 105.0(10) . . ? C30B N22 C39B 105.7(11) . . ? C30 N22 C39B 57.5(7) . . ? C29 N22 C39B 59.4(6) . . ? C39 N22 C39B 141.6(6) . . ? C29B N22 U2 111.3(7) . . ? C30B N22 U2 107.4(7) . . ? C30 N22 U2 110.9(3) . . ? C29 N22 U2 106.7(3) . . ? C39 N22 U2 110.5(3) . . ? C39B N22 U2 107.9(5) . . ? C32 N23 C31 115.7(4) . . ? C32 N23 U2 128.3(3) . . ? C31 N23 U2 116.0(3) . . ? O21 C21 C22 120.3(4) . . ? O21 C21 C26 122.1(4) . . ? C22 C21 C26 117.6(5) . . ? C23 C22 C21 121.3(5) . . ? C22 C23 C24 120.9(5) . . ? C25 C24 C23 118.8(5) . . ? C24 C25 C26 121.8(5) . . ? C25 C26 C21 119.5(4) . . ? C25 C26 C27 118.0(4) . . ? C21 C26 C27 122.4(5) . . ? N21 C27 C26 126.6(4) . . ? N21 C28 C29 111.3(4) . . ? N21 C28 C29B 101.5(7) . . ? C29 C28 C29B 46.4(7) . . ? N22 C29 C28 111.1(5) . . ? N22 C30 C31 113.1(5) . . ? N23 C31 C30B 111.6(7) . . ? N23 C31 C30 108.4(4) . . ? C30B C31 C30 46.4(7) . . ? N23 C32 C33 127.7(4) . . ? C34 C33 C38 118.9(4) . . ? C34 C33 C32 118.0(4) . . ? C38 C33 C32 123.1(4) . . ? C35 C34 C33 121.6(5) . . ? C36 C35 C34 119.1(5) . . ? C35 C36 C37 121.4(4) . . ? C36 C37 C38 120.0(5) . . ? O22 C38 C37 120.3(4) . . ? O22 C38 C33 120.7(4) . . ? C37 C38 C33 119.0(4) . . ? N22 C30B C31 114.8(12) . . ? N22 C29B C28 117.6(14) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.45 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.747 _refine_diff_density_min -1.197 _refine_diff_density_rms 0.181 data_4 _database_code_depnum_ccdc_archive 'CCDC 851301' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H147 N14 O16 U5' _chemical_formula_weight 3327.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.8481(5) _cell_length_b 31.3059(14) _cell_length_c 24.9946(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.442(3) _cell_angle_gamma 90.00 _cell_volume 12766.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8610 _cell_measurement_theta_min 3.3340 _cell_measurement_theta_max 32.3734 _exptl_crystal_description 'long block' _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6404 _exptl_absorpt_coefficient_mu 6.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2228 _exptl_absorpt_correction_T_max 0.4953 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44348 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 24.71 _reflns_number_total 21558 _reflns_number_gt 14486 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -33.00 51.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 -37.0000 90.0000 84 #__ type_ start__ end____ width___ exp.time_ 2 omega -93.00 -1.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 -77.0000 30.0000 92 #__ type_ start__ end____ width___ exp.time_ 3 omega -80.00 -32.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 179.0000 150.0000 48 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0863P)^2^+470.6426P] 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 21558 _refine_ls_number_parameters 1459 _refine_ls_number_restraints 154 _refine_ls_R_factor_all 0.1425 _refine_ls_R_factor_gt 0.1038 _refine_ls_wR_factor_ref 0.2766 _refine_ls_wR_factor_gt 0.2539 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.002 _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 0.40918(5) 0.23136(3) 0.50795(3) 0.0496(2) Uani 1 1 d . . . U2 U 0.02772(5) 0.24026(3) 0.64099(3) 0.0427(2) Uani 1 1 d . . . U3 U 0.39952(5) 0.22889(3) 0.65223(3) 0.0492(2) Uani 1 1 d . . . U4 U 0.18102(5) 0.23601(3) 0.53733(3) 0.0529(3) Uani 1 1 d . . . U5 U 0.24041(5) 0.27342(3) 0.69940(4) 0.0560(3) Uani 1 1 d . . . O345 O 0.2631(8) 0.2464(5) 0.6225(5) 0.045(4) Uani 1 1 d . . . O13U O 0.4273(9) 0.1990(5) 0.5860(5) 0.048(4) Uani 1 1 d . . . O14U O 0.2727(9) 0.2358(6) 0.4999(6) 0.059(4) Uani 1 1 d . . . O24U O 0.0845(8) 0.2333(5) 0.5683(6) 0.049(4) Uani 1 1 d . . . O25U O 0.1200(9) 0.2904(5) 0.6715(7) 0.060(4) Uani 1 1 d . . . O35U O 0.3675(11) 0.2571(7) 0.7208(6) 0.077(6) Uani 1 1 d . . . O1 O 0.3922(9) 0.1793(5) 0.4452(7) 0.056(4) Uani 1 1 d . . . O2 O 0.4103(10) 0.2825(6) 0.4439(7) 0.063(5) Uani 1 1 d . . . N1 N 0.5454(13) 0.1885(8) 0.5185(8) 0.066(6) Uani 1 1 d . . . N2 N 0.5506(13) 0.2712(8) 0.5326(7) 0.066(6) Uani 1 1 d . . . C1 C 0.4225(15) 0.1490(9) 0.4194(10) 0.059(7) Uani 1 1 d . . . C2 C 0.3796(16) 0.1303(8) 0.3707(9) 0.055(6) Uani 1 1 d . . . C3 C 0.4186(17) 0.1007(8) 0.3469(12) 0.065(7) Uani 1 1 d . . . H3 H 0.3879 0.0874 0.3141 0.078 Uiso 1 1 calc R . . C4 C 0.5026(17) 0.0875(9) 0.3671(11) 0.066(7) Uani 1 1 d . . . C5 C 0.5438(16) 0.1066(9) 0.4135(11) 0.062(7) Uani 1 1 d . . . H5 H 0.5992 0.0987 0.4290 0.074 Uiso 1 1 calc R . . C6 C 0.5079(15) 0.1385(9) 0.4406(11) 0.060(6) Uani 1 1 d . . . C7 C 0.5593(17) 0.1564(10) 0.4885(12) 0.071(8) Uani 1 1 d . . . H7 H 0.6116 0.1434 0.5008 0.086 Uiso 1 1 calc R . . C8 C 0.6076(14) 0.2054(10) 0.5609(12) 0.066(7) Uani 1 1 d . . . C9 C 0.6656(14) 0.1771(12) 0.5968(12) 0.080(9) Uani 1 1 d . . . H9 H 0.6608 0.1469 0.5944 0.096 Uiso 1 1 calc R . . C10 C 0.7312(15) 0.1982(14) 0.6367(11) 0.087(11) Uani 1 1 d . . . H10 H 0.7733 0.1808 0.6584 0.104 Uiso 1 1 calc R . . C11 C 0.7374(17) 0.2459(15) 0.6461(16) 0.107(13) Uani 1 1 d . . . H11 H 0.7804 0.2580 0.6739 0.128 Uiso 1 1 calc R . . C12 C 0.676(2) 0.2719(12) 0.6113(14) 0.095(10) Uani 1 1 d U . . H12 H 0.6762 0.3021 0.6153 0.114 Uiso 1 1 calc R . . C13 C 0.6137(12) 0.2503(11) 0.5700(9) 0.063(8) Uani 1 1 d . . . C14 C 0.5646(13) 0.3097(9) 0.5163(10) 0.055(6) Uani 1 1 d . . . H14 H 0.6133 0.3231 0.5368 0.066 Uiso 1 1 calc R . . C15 C 0.5143(12) 0.3350(9) 0.4701(10) 0.059(7) Uani 1 1 d . . . C16 C 0.5421(15) 0.3755(8) 0.4622(11) 0.059(6) Uani 1 1 d . . . H16 H 0.5901 0.3855 0.4878 0.070 Uiso 1 1 calc R . . C17 C 0.5056(17) 0.4020(9) 0.4205(12) 0.069(8) Uani 1 1 d . . . C18 C 0.4325(15) 0.3844(8) 0.3857(10) 0.055(6) Uani 1 1 d . . . H18 H 0.4042 0.4017 0.3557 0.067 Uiso 1 1 calc R . . C19 C 0.3985(13) 0.3451(8) 0.3910(9) 0.049(6) Uani 1 1 d . . . C20 C 0.4408(14) 0.3202(8) 0.4363(11) 0.054(6) Uani 1 1 d . . . C21 C 0.2885(16) 0.1405(9) 0.3472(12) 0.066(7) Uani 1 1 d . . . C22 C 0.2780(14) 0.1877(8) 0.3324(11) 0.063(7) Uani 1 1 d . . . H22A H 0.3109 0.1949 0.3064 0.094 Uiso 1 1 calc R . . H22B H 0.2962 0.2049 0.3660 0.094 Uiso 1 1 calc R . . H22C H 0.2201 0.1936 0.3154 0.094 Uiso 1 1 calc R . . C23 C 0.2401(16) 0.1299(9) 0.3912(11) 0.069(7) Uani 1 1 d . . . H23A H 0.1814 0.1284 0.3733 0.104 Uiso 1 1 calc R . . H23B H 0.2498 0.1523 0.4195 0.104 Uiso 1 1 calc R . . H23C H 0.2586 0.1024 0.4086 0.104 Uiso 1 1 calc R . . C24 C 0.2502(14) 0.1150(9) 0.2955(11) 0.063(7) Uani 1 1 d . . . H24A H 0.2728 0.1246 0.2650 0.094 Uiso 1 1 calc R . . H24B H 0.1907 0.1193 0.2856 0.094 Uiso 1 1 calc R . . H24C H 0.2623 0.0846 0.3025 0.094 Uiso 1 1 calc R . . C25 C 0.5388(17) 0.0537(10) 0.3346(10) 0.066(7) Uani 1 1 d . . . C26 C 0.494(2) 0.0123(11) 0.3317(13) 0.100(12) Uani 1 1 d . . . H26A H 0.4381 0.0157 0.3083 0.151 Uiso 1 1 calc R . . H26B H 0.4912 0.0037 0.3689 0.151 Uiso 1 1 calc R . . H26C H 0.5226 -0.0097 0.3159 0.151 Uiso 1 1 calc R . . C27 C 0.5393(18) 0.0699(11) 0.2785(12) 0.085(9) Uani 1 1 d . . . H27A H 0.5609 0.0477 0.2583 0.128 Uiso 1 1 calc R . . H27B H 0.5742 0.0954 0.2820 0.128 Uiso 1 1 calc R . . H27C H 0.4834 0.0773 0.2583 0.128 Uiso 1 1 calc R . . C28 C 0.627(2) 0.0447(11) 0.3643(12) 0.106(13) Uani 1 1 d . . . H28A H 0.6304 0.0368 0.4027 0.159 Uiso 1 1 calc R . . H28B H 0.6604 0.0702 0.3635 0.159 Uiso 1 1 calc R . . H28C H 0.6479 0.0211 0.3458 0.159 Uiso 1 1 calc R . . C29 C 0.5355(16) 0.4448(9) 0.4075(14) 0.071(8) Uani 1 1 d . . . C30 C 0.559(2) 0.4436(11) 0.3520(17) 0.116(14) Uani 1 1 d . . . H30A H 0.6110 0.4282 0.3565 0.174 Uiso 1 1 calc R . . H30B H 0.5651 0.4728 0.3396 0.174 Uiso 1 1 calc R . . H30C H 0.5160 0.4289 0.3245 0.174 Uiso 1 1 calc R . . C31 C 0.6115(17) 0.4594(10) 0.4556(14) 0.092(11) Uani 1 1 d . . . H31A H 0.5961 0.4589 0.4909 0.137 Uiso 1 1 calc R . . H31B H 0.6278 0.4884 0.4481 0.137 Uiso 1 1 calc R . . H31C H 0.6574 0.4398 0.4573 0.137 Uiso 1 1 calc R . . C32 C 0.471(2) 0.4779(11) 0.4027(19) 0.14(2) Uani 1 1 d . . . H32A H 0.4238 0.4706 0.3722 0.212 Uiso 1 1 calc R . . H32B H 0.4926 0.5058 0.3957 0.212 Uiso 1 1 calc R . . H32C H 0.4532 0.4791 0.4372 0.212 Uiso 1 1 calc R . . C33 C 0.3209(13) 0.3299(8) 0.3498(10) 0.053(6) Uani 1 1 d . . . C34 C 0.2845(14) 0.3644(9) 0.3040(10) 0.060(7) Uani 1 1 d . . . H34A H 0.2835 0.3924 0.3215 0.090 Uiso 1 1 calc R . . H34B H 0.2286 0.3563 0.2844 0.090 Uiso 1 1 calc R . . H34C H 0.3188 0.3660 0.2776 0.090 Uiso 1 1 calc R . . C35 C 0.2529(14) 0.3197(9) 0.3786(10) 0.060(7) Uani 1 1 d . . . H35A H 0.2595 0.2903 0.3927 0.090 Uiso 1 1 calc R . . H35B H 0.1994 0.3227 0.3522 0.090 Uiso 1 1 calc R . . H35C H 0.2564 0.3395 0.4095 0.090 Uiso 1 1 calc R . . C36 C 0.3414(15) 0.2915(8) 0.3184(12) 0.064(7) Uani 1 1 d . . . H36A H 0.3678 0.2695 0.3447 0.097 Uiso 1 1 calc R . . H36B H 0.3787 0.3003 0.2960 0.097 Uiso 1 1 calc R . . H36C H 0.2909 0.2800 0.2943 0.097 Uiso 1 1 calc R . . O41 O -0.0512(9) 0.1824(5) 0.6141(6) 0.050(4) Uani 1 1 d . . . O42 O -0.0728(9) 0.2842(5) 0.6026(7) 0.056(4) Uani 1 1 d . . . N41 N 0.0026(11) 0.1997(6) 0.7257(8) 0.048(4) Uani 1 1 d . . . N42 N -0.0205(10) 0.2801(6) 0.7203(6) 0.043(4) Uani 1 1 d . . . C41 C -0.0784(14) 0.1455(8) 0.6267(11) 0.053(6) Uani 1 1 d . . . C42 C -0.1214(16) 0.1166(8) 0.5854(12) 0.063(7) Uani 1 1 d . . . C43 C -0.1496(19) 0.0787(10) 0.6015(14) 0.081(9) Uani 1 1 d . . . H43 H -0.1812 0.0603 0.5740 0.098 Uiso 1 1 calc R . . C44 C -0.1327(18) 0.0658(10) 0.6592(17) 0.085(10) Uani 1 1 d . . . C45 C -0.0929(15) 0.0947(9) 0.6977(12) 0.064(7) Uani 1 1 d . . . H45 H -0.0836 0.0877 0.7357 0.077 Uiso 1 1 calc R . . C46 C -0.0652(14) 0.1344(8) 0.6832(11) 0.058(6) Uani 1 1 d . . . C47 C -0.0291(12) 0.1627(7) 0.7266(9) 0.045(5) Uani 1 1 d . . . H47A H -0.0718 0.1669 0.7471 0.054 Uiso 1 1 calc R . . H47B H 0.0145 0.1457 0.7513 0.054 Uiso 1 1 calc R . . C48 C 0.0262(12) 0.2246(7) 0.7722(8) 0.044(5) Uani 1 1 d . . . C49 C 0.0656(16) 0.2038(10) 0.8276(11) 0.068(7) Uani 1 1 d . . . H49 H 0.0738 0.1738 0.8302 0.081 Uiso 1 1 calc R . . C50 C 0.0893(13) 0.2293(10) 0.8740(9) 0.059(7) Uani 1 1 d . . . H50 H 0.1183 0.2174 0.9083 0.071 Uiso 1 1 calc R . . C51 C 0.0704(19) 0.2719(10) 0.8700(11) 0.074(8) Uani 1 1 d . . . H51 H 0.0833 0.2884 0.9029 0.089 Uiso 1 1 calc R . . C52 C 0.0332(14) 0.2928(9) 0.8203(12) 0.064(7) Uani 1 1 d . . . H52 H 0.0230 0.3227 0.8191 0.077 Uiso 1 1 calc R . . C53 C 0.0111(12) 0.2664(8) 0.7706(8) 0.044(5) Uani 1 1 d . . . C54 C -0.0683(15) 0.3151(8) 0.7127(9) 0.055(6) Uani 1 1 d . . . H54 H -0.0758 0.3277 0.7456 0.066 Uiso 1 1 calc R . . C55 C -0.1103(12) 0.3369(7) 0.6619(9) 0.043(5) Uani 1 1 d . . . C56 C -0.1464(13) 0.3756(9) 0.6674(10) 0.058(6) Uani 1 1 d . . . H56 H -0.1429 0.3861 0.7035 0.069 Uiso 1 1 calc R . . C57 C -0.1883(14) 0.4003(8) 0.6221(11) 0.058(6) Uani 1 1 d . . . C58 C -0.1930(14) 0.3820(8) 0.5720(10) 0.053(6) Uani 1 1 d . . . H58 H -0.2221 0.3975 0.5405 0.064 Uiso 1 1 calc R . . C59 C -0.1598(13) 0.3435(8) 0.5622(10) 0.053(6) Uani 1 1 d . . . C60 C -0.1135(15) 0.3210(7) 0.6085(11) 0.056(6) Uani 1 1 d . . . C61 C -0.1382(17) 0.1273(9) 0.5230(11) 0.067(7) Uani 1 1 d . . . C62 C -0.1863(18) 0.1673(10) 0.5083(12) 0.080(9) Uani 1 1 d . . . H62A H -0.1650 0.1893 0.5361 0.120 Uiso 1 1 calc R . . H62B H -0.2440 0.1618 0.5070 0.120 Uiso 1 1 calc R . . H62C H -0.1817 0.1773 0.4720 0.120 Uiso 1 1 calc R . . C63 C -0.190(2) 0.0928(11) 0.4884(14) 0.094(10) Uani 1 1 d . . . H63A H -0.2467 0.0952 0.4917 0.141 Uiso 1 1 calc R . . H63B H -0.1682 0.0647 0.5014 0.141 Uiso 1 1 calc R . . H63C H -0.1891 0.0964 0.4496 0.141 Uiso 1 1 calc R . . C64 C -0.0563(18) 0.1303(12) 0.5082(14) 0.096(11) Uani 1 1 d . . . H64A H -0.0640 0.1438 0.4719 0.145 Uiso 1 1 calc R . . H64B H -0.0335 0.1016 0.5073 0.145 Uiso 1 1 calc R . . H64C H -0.0184 0.1476 0.5360 0.145 Uiso 1 1 calc R . . C65 C -0.159(3) 0.0216(9) 0.6770(16) 0.096(11) Uani 1 1 d . . . C66 C -0.104(5) -0.0103(17) 0.662(3) 0.23(4) Uani 1 1 d . . . H66A H -0.1070 -0.0369 0.6824 0.348 Uiso 1 1 calc R . . H66B H -0.0477 0.0006 0.6723 0.348 Uiso 1 1 calc R . . H66C H -0.1207 -0.0158 0.6225 0.348 Uiso 1 1 calc R . . C67 C -0.247(3) 0.0107(15) 0.642(2) 0.21(3) Uani 1 1 d . . . H67A H -0.2693 -0.0128 0.6599 0.308 Uiso 1 1 calc R . . H67B H -0.2445 0.0021 0.6050 0.308 Uiso 1 1 calc R . . H67C H -0.2820 0.0359 0.6400 0.308 Uiso 1 1 calc R . . C68 C -0.147(3) 0.0155(13) 0.7334(19) 0.15(2) Uani 1 1 d . . . H68A H -0.1426 -0.0151 0.7417 0.226 Uiso 1 1 calc R . . H68B H -0.1939 0.0273 0.7454 0.226 Uiso 1 1 calc R . . H68C H -0.0969 0.0300 0.7531 0.226 Uiso 1 1 calc R . . C69 C -0.2279(16) 0.4430(9) 0.6323(12) 0.065(7) Uani 1 1 d . . . C70 C -0.2249(19) 0.4748(10) 0.5856(12) 0.082(9) Uani 1 1 d . . . H70A H -0.2485 0.4613 0.5497 0.122 Uiso 1 1 calc R . . H70B H -0.1679 0.4827 0.5880 0.122 Uiso 1 1 calc R . . H70C H -0.2565 0.5004 0.5894 0.122 Uiso 1 1 calc R . . C71 C -0.3174(18) 0.4332(10) 0.6307(16) 0.092(10) Uani 1 1 d . . . H71A H -0.3433 0.4188 0.5958 0.138 Uiso 1 1 calc R . . H71B H -0.3465 0.4599 0.6334 0.138 Uiso 1 1 calc R . . H71C H -0.3197 0.4145 0.6617 0.138 Uiso 1 1 calc R . . C72 C -0.188(2) 0.4648(9) 0.6859(14) 0.097(11) Uani 1 1 d . . . H72A H -0.2195 0.4904 0.6900 0.145 Uiso 1 1 calc R . . H72B H -0.1320 0.4729 0.6859 0.145 Uiso 1 1 calc R . . H72C H -0.1871 0.4453 0.7167 0.145 Uiso 1 1 calc R . . C73 C -0.1699(16) 0.3262(10) 0.5033(9) 0.066(8) Uani 1 1 d . . . C74 C -0.2220(19) 0.3520(11) 0.4609(12) 0.088(10) Uani 1 1 d . . . H74A H -0.2237 0.3397 0.4246 0.132 Uiso 1 1 calc R . . H74B H -0.2003 0.3811 0.4627 0.132 Uiso 1 1 calc R . . H74C H -0.2775 0.3526 0.4665 0.132 Uiso 1 1 calc R . . C75 C -0.0812(18) 0.3245(12) 0.4885(12) 0.093(11) Uani 1 1 d . . . H75A H -0.0866 0.3095 0.4534 0.140 Uiso 1 1 calc R . . H75B H -0.0418 0.3094 0.5179 0.140 Uiso 1 1 calc R . . H75C H -0.0616 0.3537 0.4854 0.140 Uiso 1 1 calc R . . C76 C -0.207(2) 0.2824(10) 0.4978(10) 0.078(9) Uani 1 1 d . . . H76A H -0.2540 0.2815 0.4655 0.117 Uiso 1 1 calc R . . H76B H -0.2252 0.2755 0.5311 0.117 Uiso 1 1 calc R . . H76C H -0.1659 0.2614 0.4932 0.117 Uiso 1 1 calc R . . O81 O 0.3765(10) 0.1662(6) 0.6877(8) 0.071(5) Uani 1 1 d . . . O82 O 0.4022(9) 0.2801(5) 0.5816(5) 0.043(3) Uani 1 1 d . . . N81 N 0.5330(13) 0.2014(9) 0.7211(9) 0.072(7) Uani 1 1 d . . . N82 N 0.5128(12) 0.2887(10) 0.6832(8) 0.081(8) Uani 1 1 d . . . C81 C 0.4049(15) 0.1334(9) 0.7199(10) 0.061(7) Uani 1 1 d . . . C82 C 0.3604(17) 0.0986(10) 0.7262(12) 0.073(8) Uani 1 1 d . . . H82 H 0.3044 0.0980 0.7065 0.088 Uiso 1 1 calc R . . C83 C 0.391(2) 0.0642(9) 0.7591(13) 0.079(8) Uani 1 1 d . . . H83 H 0.3555 0.0409 0.7614 0.095 Uiso 1 1 calc R . . C84 C 0.469(2) 0.0629(11) 0.7879(14) 0.089(10) Uani 1 1 d . . . H84 H 0.4909 0.0395 0.8111 0.107 Uiso 1 1 calc R . . C85 C 0.514(2) 0.0957(12) 0.7823(13) 0.089(10) Uani 1 1 d . . . H85 H 0.5697 0.0947 0.8019 0.106 Uiso 1 1 calc R . . C86 C 0.4880(15) 0.1332(10) 0.7500(11) 0.067(7) Uani 1 1 d . . . C87 C 0.5430(16) 0.1677(13) 0.7472(11) 0.083(10) Uani 1 1 d . . . H87 H 0.5970 0.1638 0.7696 0.100 Uiso 1 1 calc R . . C88 C 0.5983(18) 0.2315(16) 0.7300(15) 0.123(18) Uani 1 1 d . . . H88A H 0.6273 0.2274 0.7004 0.147 Uiso 1 1 calc R . . H88B H 0.6375 0.2242 0.7654 0.147 Uiso 1 1 calc R . . C89 C 0.579(2) 0.2761(14) 0.7316(12) 0.114(16) Uani 1 1 d . . . H89A H 0.6284 0.2933 0.7324 0.137 Uiso 1 1 calc R . . H89B H 0.5614 0.2822 0.7658 0.137 Uiso 1 1 calc R . . C90 C 0.518(2) 0.3271(11) 0.6642(15) 0.092(11) Uani 1 1 d . . . H90 H 0.5624 0.3444 0.6839 0.110 Uiso 1 1 calc R . . C91 C 0.4652(16) 0.3453(9) 0.6169(14) 0.072(8) Uani 1 1 d . . . C92 C 0.472(2) 0.3908(12) 0.6058(17) 0.103(11) Uani 1 1 d U . . H92 H 0.5117 0.4072 0.6311 0.124 Uiso 1 1 calc R . . C93 C 0.424(2) 0.4104(10) 0.5612(16) 0.091(9) Uani 1 1 d U . . H93 H 0.4316 0.4397 0.5540 0.109 Uiso 1 1 calc R . . C94 C 0.3676(18) 0.3875(9) 0.5283(13) 0.072(8) Uani 1 1 d . . . H94 H 0.3314 0.4017 0.4984 0.087 Uiso 1 1 calc R . . C95 C 0.3569(16) 0.3454(8) 0.5338(11) 0.058(6) Uani 1 1 d . . . H95 H 0.3148 0.3310 0.5077 0.069 Uiso 1 1 calc R . . C96 C 0.4060(13) 0.3228(9) 0.5767(10) 0.053(6) Uani 1 1 d . . . O101 O 0.1732(9) 0.3057(8) 0.5386(7) 0.078(6) Uani 1 1 d . . . O102 O 0.2213(10) 0.1697(6) 0.5636(7) 0.062(5) Uani 1 1 d . . . N101 N 0.1028(14) 0.2690(12) 0.4449(13) 0.104(10) Uani 1 1 d . . . N102 N 0.0979(13) 0.1793(11) 0.4670(8) 0.077(8) Uani 1 1 d . . . C101 C 0.1501(18) 0.3441(14) 0.5142(16) 0.092(12) Uani 1 1 d . . . C102 C 0.170(3) 0.3812(14) 0.5440(18) 0.111(13) Uani 1 1 d . . . H102 H 0.1980 0.3819 0.5821 0.133 Uiso 1 1 calc R . . C103 C 0.145(3) 0.4174(16) 0.513(3) 0.16(3) Uani 1 1 d . . . H103 H 0.1595 0.4421 0.5355 0.192 Uiso 1 1 calc R . . C104 C 0.114(5) 0.427(2) 0.470(4) 0.20(4) Uani 1 1 d . . . H104 H 0.1056 0.4556 0.4572 0.241 Uiso 1 1 calc R . . C105 C 0.087(3) 0.387(2) 0.4372(19) 0.15(2) Uani 1 1 d . . . H105 H 0.0574 0.3892 0.3997 0.175 Uiso 1 1 calc R . . C106 C 0.108(2) 0.3463(16) 0.4623(16) 0.114(14) Uani 1 1 d U . . C107 C 0.085(2) 0.3075(17) 0.4286(16) 0.116(14) Uani 1 1 d U . . H107 H 0.0552 0.3113 0.3914 0.139 Uiso 1 1 calc R . . C108 C 0.066(3) 0.2397(14) 0.3993(18) 0.114(8) Uani 1 1 d U . . H10A H 0.1082 0.2310 0.3799 0.137 Uiso 1 1 calc R . . H10B H 0.0214 0.2544 0.3725 0.137 Uiso 1 1 calc R . . C109 C 0.033(2) 0.2004(14) 0.4215(17) 0.114(8) Uani 1 1 d U . . H10C H 0.0129 0.1798 0.3911 0.137 Uiso 1 1 calc R . . H10D H -0.0145 0.2087 0.4363 0.137 Uiso 1 1 calc R . . C110 C 0.1053(18) 0.1375(15) 0.4676(12) 0.085(11) Uani 1 1 d . . . H110 H 0.0667 0.1226 0.4396 0.102 Uiso 1 1 calc R . . C111 C 0.161(2) 0.1127(11) 0.5031(14) 0.085(10) Uani 1 1 d . . . C112 C 0.163(3) 0.0667(15) 0.4950(18) 0.122(16) Uani 1 1 d . . . H112 H 0.1260 0.0530 0.4652 0.146 Uiso 1 1 calc R . . C113 C 0.221(4) 0.044(2) 0.532(3) 0.152(19) Uani 1 1 d U . . H113 H 0.2217 0.0138 0.5272 0.183 Uiso 1 1 calc R . . C114 C 0.275(3) 0.0602(12) 0.5714(18) 0.115(13) Uani 1 1 d . . . H114 H 0.3152 0.0424 0.5940 0.138 Uiso 1 1 calc R . . C115 C 0.274(2) 0.1011(11) 0.5818(13) 0.086(9) Uani 1 1 d . . . H115 H 0.3139 0.1118 0.6130 0.103 Uiso 1 1 calc R . . C116 C 0.2196(18) 0.1300(11) 0.5498(12) 0.073(8) Uani 1 1 d . . . O121 O 0.2779(11) 0.3394(6) 0.6870(12) 0.106(9) Uani 1 1 d . . . O122 O 0.1567(8) 0.2095(6) 0.6837(6) 0.059(4) Uani 1 1 d . . . N121 N 0.2632(19) 0.3196(15) 0.7893(15) 0.137(16) Uani 1 1 d . . . N122 N 0.2598(9) 0.2264(10) 0.7848(9) 0.111(13) Uani 1 1 d . . . C121 C 0.2883(9) 0.3789(10) 0.7000(9) 0.208(13) Uani 1 1 d RU . . C122 C 0.2884(9) 0.4109(10) 0.6614(9) 0.213(13) Uani 1 1 d RU . . H122 H 0.2884 0.4035 0.6246 0.256 Uiso 1 1 calc R . . C123 C 0.2884(9) 0.4535(10) 0.6768(9) 0.219(13) Uani 1 1 d RU . . H123 H 0.2885 0.4754 0.6504 0.263 Uiso 1 1 calc R . . C124 C 0.2884(9) 0.4643(10) 0.7307(9) 0.227(14) Uani 1 1 d RU . . H124 H 0.2884 0.4935 0.7412 0.272 Uiso 1 1 calc R . . C125 C 0.2882(9) 0.4323(10) 0.7693(9) 0.225(13) Uani 1 1 d RU . . H125 H 0.2882 0.4397 0.8062 0.270 Uiso 1 1 calc R . . C126 C 0.2882(9) 0.3897(10) 0.7540(9) 0.216(13) Uani 1 1 d RU . . C127 C 0.279(4) 0.361(2) 0.793(3) 0.206(14) Uani 1 1 d U . . H127 H 0.2858 0.3724 0.8295 0.247 Uiso 1 1 calc R . . C128 C 0.269(4) 0.2915(19) 0.837(2) 0.16(2) Uani 1 1 d U . . H12A H 0.2120 0.2863 0.8401 0.197 Uiso 1 1 calc R . . H12B H 0.2968 0.3078 0.8703 0.197 Uiso 1 1 calc R . . C129 C 0.312(3) 0.2465(16) 0.841(2) 0.140(16) Uani 1 1 d U . . H12C H 0.3066 0.2300 0.8735 0.168 Uiso 1 1 calc R . . H12D H 0.3708 0.2491 0.8411 0.168 Uiso 1 1 calc R . . C130 C 0.244(3) 0.187(2) 0.7940(19) 0.14(3) Uani 1 1 d . . . H130 H 0.2640 0.1768 0.8309 0.170 Uiso 1 1 calc R . . C131 C 0.201(2) 0.1566(15) 0.756(2) 0.110(16) Uani 1 1 d . . . C132 C 0.196(2) 0.1153(19) 0.773(2) 0.15(2) Uani 1 1 d . . . H132 H 0.2199 0.1084 0.8102 0.175 Uiso 1 1 calc R . . C133 C 0.157(3) 0.0834(17) 0.738(4) 0.19(4) Uani 1 1 d . . . H133 H 0.1552 0.0549 0.7505 0.233 Uiso 1 1 calc R . . C134 C 0.121(3) 0.0946(12) 0.685(3) 0.15(2) Uani 1 1 d . . . H134 H 0.0925 0.0734 0.6603 0.176 Uiso 1 1 calc R . . C135 C 0.1253(17) 0.1351(8) 0.6647(19) 0.100(13) Uani 1 1 d . . . H135 H 0.1032 0.1413 0.6267 0.120 Uiso 1 1 calc R . . C136 C 0.1630(17) 0.1675(10) 0.7018(16) 0.086(11) Uani 1 1 d . . . N141 N 0.107(4) 0.4593(17) 0.022(2) 0.21(2) Uani 1 1 d DU . . C141 C 0.103(4) 0.4960(17) 0.022(3) 0.18(2) Uani 1 1 d DU . . C142 C 0.098(4) 0.5403(17) 0.029(3) 0.20(3) Uani 1 1 d DU . . H14A H 0.0446 0.5475 0.0352 0.307 Uiso 1 1 calc R . . H14B H 0.1050 0.5549 -0.0042 0.307 Uiso 1 1 calc R . . H14C H 0.1416 0.5494 0.0609 0.307 Uiso 1 1 calc R . . N142 N 0.215(4) 0.542(2) 0.6213(19) 0.28(4) Uani 1 1 d . . . C143 C 0.160(3) 0.5412(15) 0.586(2) 0.124(15) Uani 1 1 d . . . C144 C 0.092(3) 0.5366(18) 0.538(2) 0.17(2) Uani 1 1 d . . . H14D H 0.1039 0.5525 0.5070 0.262 Uiso 1 1 calc R . . H14E H 0.0423 0.5478 0.5461 0.262 Uiso 1 1 calc R . . H14F H 0.0847 0.5063 0.5281 0.262 Uiso 1 1 calc R . . N143 N 0.005(2) 0.4641(17) 0.607(2) 0.143(16) Uani 1 1 d . . . C145 C 0.030(3) 0.4322(19) 0.6238(19) 0.105(13) Uani 1 1 d . . . C146 C 0.064(2) 0.3917(13) 0.6446(19) 0.115(14) Uani 1 1 d . . . H14G H 0.0758 0.3750 0.6145 0.172 Uiso 1 1 calc R . . H14H H 0.0243 0.3763 0.6603 0.172 Uiso 1 1 calc R . . H14I H 0.1146 0.3963 0.6734 0.172 Uiso 1 1 calc R . . N144 N 0.646(4) 0.088(2) 0.687(3) 0.28(3) Uani 1 1 d DU . . C147 C 0.583(4) 0.095(2) 0.657(2) 0.19(2) Uani 1 1 d DU . . C148 C 0.511(3) 0.099(2) 0.615(2) 0.19(2) Uani 1 1 d DU . . H14J H 0.5188 0.1213 0.5885 0.280 Uiso 1 1 calc R . . H14K H 0.4652 0.1074 0.6302 0.280 Uiso 1 1 calc R . . H14L H 0.4988 0.0720 0.5953 0.280 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 0.0367(4) 0.0741(6) 0.0386(5) 0.0004(4) 0.0104(3) 0.0058(4) U2 0.0379(4) 0.0533(5) 0.0386(4) -0.0017(4) 0.0126(3) 0.0001(4) U3 0.0368(4) 0.0712(6) 0.0396(5) 0.0008(4) 0.0097(3) -0.0009(4) U4 0.0369(4) 0.0870(7) 0.0362(4) 0.0008(4) 0.0114(3) 0.0064(4) U5 0.0419(5) 0.0775(7) 0.0515(5) -0.0173(5) 0.0169(4) -0.0085(4) O345 0.036(7) 0.077(10) 0.028(7) 0.019(7) 0.019(6) 0.010(7) O13U 0.050(8) 0.068(10) 0.024(7) 0.000(7) 0.005(6) -0.001(7) O14U 0.043(8) 0.097(13) 0.039(8) 0.001(8) 0.015(7) 0.004(8) O24U 0.032(7) 0.079(11) 0.039(8) -0.005(8) 0.016(6) 0.003(7) O25U 0.041(8) 0.057(10) 0.090(13) 0.012(9) 0.033(8) 0.001(7) O35U 0.071(12) 0.121(16) 0.025(8) -0.021(9) -0.011(8) -0.007(11) O1 0.035(8) 0.077(11) 0.055(10) -0.009(8) 0.010(7) 0.011(8) O2 0.048(9) 0.092(14) 0.051(10) 0.011(9) 0.019(8) 0.007(9) N1 0.059(13) 0.101(18) 0.039(11) 0.009(12) 0.014(10) 0.017(12) N2 0.067(14) 0.12(2) 0.017(9) -0.008(10) 0.019(9) -0.027(13) C1 0.061(15) 0.076(17) 0.048(14) 0.005(12) 0.028(12) 0.028(13) C2 0.069(16) 0.063(15) 0.041(13) -0.004(11) 0.032(12) 0.005(12) C3 0.077(18) 0.053(15) 0.070(17) 0.013(13) 0.028(14) 0.011(13) C4 0.067(16) 0.078(19) 0.061(17) 0.016(14) 0.035(14) 0.032(14) C5 0.058(15) 0.081(19) 0.052(15) 0.015(14) 0.025(13) 0.028(13) C6 0.053(14) 0.074(18) 0.058(16) 0.004(13) 0.021(13) 0.011(13) C7 0.058(16) 0.08(2) 0.071(19) 0.010(16) 0.012(14) 0.023(14) C8 0.037(13) 0.08(2) 0.080(19) 0.000(16) 0.023(13) 0.001(13) C9 0.035(13) 0.13(3) 0.072(18) -0.016(18) 0.016(13) 0.028(15) C10 0.040(14) 0.17(4) 0.050(16) 0.032(19) 0.005(12) 0.044(19) C11 0.031(14) 0.17(4) 0.11(3) 0.05(3) -0.005(15) -0.002(19) C12 0.099(13) 0.098(13) 0.090(13) 0.009(9) 0.029(9) -0.012(9) C13 0.022(10) 0.13(3) 0.035(12) -0.018(14) 0.011(9) -0.021(13) C14 0.031(11) 0.09(2) 0.048(13) -0.013(13) 0.024(10) 0.002(12) C15 0.025(11) 0.09(2) 0.055(15) 0.007(14) 0.008(10) 0.016(12) C16 0.047(13) 0.061(16) 0.075(18) -0.014(14) 0.027(13) 0.008(12) C17 0.067(17) 0.063(17) 0.078(19) -0.024(15) 0.017(15) 0.010(14) C18 0.062(15) 0.056(15) 0.046(13) -0.005(11) 0.009(11) 0.005(12) C19 0.038(11) 0.069(16) 0.043(13) -0.015(11) 0.018(10) 0.001(11) C20 0.045(13) 0.055(15) 0.074(17) -0.009(13) 0.037(13) 0.000(11) C21 0.057(15) 0.065(17) 0.084(19) -0.011(15) 0.035(14) -0.006(13) C22 0.046(13) 0.058(15) 0.066(16) 0.010(13) -0.021(12) 0.002(11) C23 0.057(15) 0.081(19) 0.069(18) 0.009(15) 0.017(13) 0.016(14) C24 0.047(13) 0.071(17) 0.070(17) -0.011(14) 0.013(12) -0.005(12) C25 0.076(17) 0.08(2) 0.037(13) 0.003(13) 0.009(12) 0.027(15) C26 0.14(3) 0.10(3) 0.06(2) -0.008(18) 0.01(2) 0.04(2) C27 0.073(19) 0.11(2) 0.08(2) 0.003(18) 0.028(16) 0.041(18) C28 0.15(3) 0.11(3) 0.055(18) 0.012(17) 0.017(19) 0.08(2) C29 0.056(15) 0.052(16) 0.09(2) -0.013(15) -0.008(15) 0.001(12) C30 0.11(3) 0.08(2) 0.13(3) 0.01(2) -0.02(3) -0.04(2) C31 0.057(17) 0.08(2) 0.11(3) -0.022(19) -0.016(17) 0.012(15) C32 0.11(3) 0.08(2) 0.18(4) -0.03(3) -0.08(3) 0.03(2) C33 0.042(12) 0.064(15) 0.051(14) 0.009(12) 0.010(10) -0.004(11) C34 0.043(13) 0.082(18) 0.046(14) -0.004(13) -0.006(11) -0.005(12) C35 0.044(13) 0.088(19) 0.048(14) 0.014(13) 0.008(11) -0.006(12) C36 0.049(14) 0.067(17) 0.086(19) -0.017(15) 0.034(13) 0.003(12) O41 0.045(8) 0.062(10) 0.042(8) -0.009(7) 0.007(7) -0.012(7) O42 0.054(9) 0.054(10) 0.054(10) 0.019(8) -0.001(7) 0.003(8) N41 0.044(10) 0.049(11) 0.047(11) 0.009(9) 0.003(8) -0.002(9) N42 0.050(10) 0.062(12) 0.011(8) -0.011(7) -0.002(7) -0.005(9) C41 0.046(13) 0.050(14) 0.067(16) -0.009(12) 0.022(12) -0.003(11) C42 0.066(16) 0.056(16) 0.074(18) -0.018(13) 0.029(14) -0.013(13) C43 0.09(2) 0.07(2) 0.08(2) -0.026(17) 0.034(18) -0.031(17) C44 0.062(17) 0.068(19) 0.14(3) -0.03(2) 0.042(19) -0.020(15) C45 0.058(15) 0.071(18) 0.067(17) 0.013(14) 0.022(13) -0.007(13) C46 0.046(13) 0.062(16) 0.069(17) 0.004(13) 0.018(12) -0.001(12) C47 0.032(10) 0.058(14) 0.051(13) 0.000(11) 0.021(10) 0.013(10) C48 0.040(11) 0.053(14) 0.028(11) 0.016(10) -0.013(9) -0.015(10) C49 0.060(15) 0.075(19) 0.070(18) 0.017(15) 0.021(14) 0.000(14) C50 0.040(12) 0.11(2) 0.018(10) 0.002(12) -0.002(9) 0.001(13) C51 0.09(2) 0.09(2) 0.049(16) -0.020(15) 0.047(16) 0.002(17) C52 0.048(14) 0.069(17) 0.079(19) -0.016(15) 0.022(13) 0.001(12) C53 0.027(10) 0.075(17) 0.031(11) 0.007(11) 0.007(8) -0.010(10) C54 0.071(16) 0.060(15) 0.039(13) -0.014(11) 0.024(12) -0.009(13) C55 0.035(11) 0.054(13) 0.043(12) -0.011(10) 0.014(9) 0.011(10) C56 0.035(12) 0.085(19) 0.049(14) -0.009(13) 0.003(10) -0.015(12) C57 0.041(12) 0.071(17) 0.060(16) 0.009(13) 0.012(11) 0.006(12) C58 0.048(13) 0.058(15) 0.060(15) 0.023(12) 0.025(12) 0.021(11) C59 0.035(11) 0.077(17) 0.049(14) 0.008(12) 0.013(10) -0.002(11) C60 0.056(14) 0.042(13) 0.085(18) -0.017(13) 0.044(14) -0.015(11) C61 0.074(18) 0.070(18) 0.065(17) -0.024(14) 0.034(14) -0.011(14) C62 0.08(2) 0.10(2) 0.064(18) -0.016(16) 0.022(15) -0.045(18) C63 0.09(2) 0.11(3) 0.08(2) -0.023(19) 0.024(19) -0.04(2) C64 0.08(2) 0.12(3) 0.10(3) -0.05(2) 0.051(19) -0.027(19) C65 0.14(3) 0.044(17) 0.10(3) -0.021(17) 0.03(2) -0.027(18) C66 0.36(10) 0.11(4) 0.31(9) 0.00(5) 0.24(8) -0.07(5) C67 0.15(4) 0.15(4) 0.26(6) 0.12(4) -0.05(4) -0.11(4) C68 0.24(6) 0.10(3) 0.12(4) -0.01(3) 0.05(4) -0.09(3) C69 0.063(16) 0.065(17) 0.075(18) 0.005(14) 0.030(14) 0.005(13) C70 0.09(2) 0.070(19) 0.08(2) 0.019(16) 0.011(17) -0.012(16) C71 0.08(2) 0.08(2) 0.14(3) 0.01(2) 0.06(2) 0.027(16) C72 0.16(3) 0.053(18) 0.09(2) -0.006(16) 0.05(2) 0.004(19) C73 0.067(16) 0.10(2) 0.035(13) 0.033(13) 0.019(12) 0.031(15) C74 0.09(2) 0.11(3) 0.07(2) -0.004(18) 0.030(17) 0.024(19) C75 0.08(2) 0.15(3) 0.053(17) 0.035(19) 0.028(15) 0.04(2) C76 0.12(2) 0.09(2) 0.030(13) 0.009(13) 0.028(14) 0.033(19) O81 0.054(10) 0.084(13) 0.074(12) 0.020(11) 0.013(9) 0.000(9) O82 0.051(8) 0.051(9) 0.029(7) -0.014(7) 0.016(6) 0.004(7) N81 0.053(13) 0.11(2) 0.053(13) 0.019(14) 0.011(10) 0.000(13) N82 0.038(11) 0.16(3) 0.043(12) -0.004(14) 0.006(9) -0.023(14) C81 0.057(15) 0.075(18) 0.048(15) -0.007(13) 0.008(12) 0.000(13) C82 0.055(16) 0.08(2) 0.08(2) 0.013(16) 0.010(14) 0.012(15) C83 0.09(2) 0.062(18) 0.09(2) 0.014(16) 0.028(18) 0.012(16) C84 0.10(3) 0.07(2) 0.09(2) 0.008(18) 0.00(2) 0.019(19) C85 0.10(2) 0.10(3) 0.07(2) 0.019(19) 0.023(18) 0.05(2) C86 0.049(14) 0.10(2) 0.052(15) 0.020(14) 0.012(12) 0.009(14) C87 0.047(15) 0.15(3) 0.046(16) 0.015(19) 0.001(12) 0.018(18) C88 0.041(16) 0.23(5) 0.09(3) 0.07(3) 0.006(16) -0.04(2) C89 0.11(3) 0.16(4) 0.044(17) 0.03(2) -0.042(17) -0.08(3) C90 0.08(2) 0.09(2) 0.10(2) -0.01(2) 0.008(19) -0.057(19) C91 0.047(14) 0.070(18) 0.10(2) 0.013(17) 0.028(16) -0.007(13) C92 0.10(3) 0.10(3) 0.12(3) 0.00(2) 0.030(19) -0.03(2) C93 0.11(3) 0.055(18) 0.12(3) 0.002(17) 0.05(2) -0.013(17) C94 0.072(18) 0.065(19) 0.08(2) -0.001(16) 0.024(16) 0.009(15) C95 0.068(16) 0.052(15) 0.061(16) 0.000(12) 0.031(13) 0.023(12) C96 0.029(11) 0.087(19) 0.054(14) -0.006(13) 0.028(10) -0.005(12) O101 0.033(8) 0.16(2) 0.045(9) 0.029(11) 0.023(7) 0.020(10) O102 0.060(10) 0.075(12) 0.047(10) -0.018(9) 0.004(8) 0.011(9) N101 0.039(12) 0.17(3) 0.10(2) 0.03(2) 0.016(13) 0.007(16) N102 0.052(13) 0.15(3) 0.021(10) -0.022(13) 0.003(9) 0.011(15) C101 0.056(17) 0.13(3) 0.10(3) 0.05(3) 0.045(18) 0.05(2) C102 0.13(3) 0.11(3) 0.11(3) 0.01(3) 0.05(3) 0.04(3) C103 0.14(4) 0.10(3) 0.29(8) 0.08(5) 0.14(5) 0.05(3) C104 0.23(7) 0.15(5) 0.26(9) 0.13(6) 0.13(7) 0.14(5) C105 0.12(3) 0.23(6) 0.10(3) 0.11(4) 0.06(3) 0.09(4) C106 0.079(19) 0.19(4) 0.09(2) 0.07(2) 0.056(19) 0.06(2) C107 0.083(19) 0.21(4) 0.08(2) 0.07(2) 0.057(19) 0.06(2) C108 0.110(11) 0.126(12) 0.107(11) 0.000(9) 0.027(8) 0.004(9) C109 0.110(11) 0.126(12) 0.107(11) 0.000(9) 0.027(9) 0.004(9) C110 0.054(17) 0.15(4) 0.048(17) -0.05(2) 0.014(14) -0.04(2) C111 0.09(2) 0.10(3) 0.07(2) -0.032(19) 0.035(19) -0.04(2) C112 0.13(3) 0.14(4) 0.11(3) -0.08(3) 0.05(3) -0.07(3) C113 0.15(2) 0.15(2) 0.15(2) -0.002(10) 0.041(11) -0.001(10) C114 0.15(4) 0.08(3) 0.11(3) -0.04(2) 0.04(3) -0.02(2) C115 0.10(2) 0.09(2) 0.07(2) -0.016(18) 0.022(18) 0.020(19) C116 0.070(18) 0.09(2) 0.067(18) -0.001(17) 0.029(15) -0.004(16) O121 0.056(11) 0.046(11) 0.22(3) -0.036(14) 0.050(15) -0.018(9) O122 0.031(7) 0.100(14) 0.045(9) -0.004(9) 0.008(7) 0.014(8) N121 0.10(2) 0.20(4) 0.13(3) -0.09(3) 0.08(2) -0.08(2) N122 0.016(10) 0.25(4) 0.068(18) 0.00(2) 0.011(11) 0.006(17) C121 0.20(2) 0.210(19) 0.23(2) -0.011(13) 0.09(2) -0.02(2) C122 0.20(2) 0.21(2) 0.24(2) -0.008(13) 0.08(2) -0.02(2) C123 0.22(2) 0.210(19) 0.240(18) -0.008(13) 0.077(17) -0.021(18) C124 0.230(16) 0.222(15) 0.230(16) -0.007(8) 0.062(9) -0.003(9) C125 0.230(15) 0.220(15) 0.230(15) -0.011(8) 0.067(9) -0.003(9) C126 0.213(19) 0.217(16) 0.235(19) -0.022(12) 0.085(18) -0.023(17) C127 0.21(3) 0.208(19) 0.22(2) -0.042(18) 0.09(2) -0.02(2) C128 0.17(2) 0.17(2) 0.16(2) -0.009(10) 0.041(11) 0.001(10) C129 0.142(18) 0.149(19) 0.131(18) 0.005(10) 0.039(10) 0.000(10) C130 0.06(3) 0.28(8) 0.09(3) 0.10(4) 0.03(2) 0.05(4) C131 0.052(19) 0.15(4) 0.14(4) 0.09(3) 0.05(2) 0.03(2) C132 0.07(3) 0.19(5) 0.20(5) 0.14(5) 0.07(3) 0.05(3) C133 0.11(4) 0.11(4) 0.41(12) 0.16(6) 0.15(6) 0.05(3) C134 0.11(3) 0.06(2) 0.30(8) 0.01(3) 0.11(4) 0.00(2) C135 0.057(17) 0.027(14) 0.22(4) 0.00(2) 0.05(2) 0.013(12) C136 0.062(17) 0.07(2) 0.15(3) 0.07(2) 0.06(2) 0.024(15) N141 0.21(3) 0.20(3) 0.21(3) -0.025(19) 0.036(18) 0.007(19) C141 0.18(2) 0.18(3) 0.18(2) 0.000(10) 0.045(11) -0.001(10) C142 0.20(3) 0.20(3) 0.21(3) 0.006(19) 0.05(2) 0.004(19) N142 0.33(8) 0.39(9) 0.09(3) -0.01(4) 0.02(4) -0.26(7) C143 0.15(4) 0.12(3) 0.10(3) -0.03(3) 0.03(3) -0.04(3) C144 0.12(4) 0.17(5) 0.21(6) 0.05(4) -0.02(4) -0.03(3) N143 0.10(3) 0.17(4) 0.17(4) 0.02(3) 0.04(3) 0.00(3) C145 0.08(3) 0.14(4) 0.10(3) 0.00(3) 0.03(2) -0.03(3) C146 0.10(3) 0.10(3) 0.16(4) -0.04(3) 0.07(3) -0.05(2) N144 0.28(4) 0.28(4) 0.27(4) 0.00(2) 0.07(2) -0.01(2) C147 0.19(3) 0.19(3) 0.19(3) -0.001(10) 0.046(11) 0.001(10) C148 0.18(3) 0.19(3) 0.19(3) 0.007(19) 0.045(19) 0.002(19) _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 O13U 2.152(14) . ? U1 O1 2.231(16) . ? U1 O14U 2.262(15) . ? U1 O2 2.267(17) . ? U1 O82 2.416(13) . ? U1 N1 2.61(2) . ? U1 N2 2.62(2) . ? U1 U3 3.6510(12) . ? U1 U4 4.0922(11) . ? U2 O42 2.206(15) . ? U2 O25U 2.207(16) . ? U2 O41 2.248(15) . ? U2 O24U 2.265(13) . ? U2 O122 2.374(14) . ? U2 N41 2.593(18) . ? U2 N42 2.636(16) . ? U2 U5 3.6662(12) . ? U2 U4 4.0913(11) . ? U3 O13U 2.055(14) . ? U3 O35U 2.115(17) . ? U3 O81 2.227(19) . ? U3 O345 2.299(13) . ? U3 O82 2.394(15) . ? U3 N81 2.61(2) . ? U3 N82 2.65(3) . ? U3 U5 3.4781(12) . ? U3 U4 4.0713(12) . ? U4 O24U 1.970(13) . ? U4 O14U 1.996(15) . ? U4 O101 2.19(2) . ? U4 O102 2.231(18) . ? U4 O345 2.254(14) . ? U4 N101 2.57(3) . ? U4 N102 2.64(3) . ? U4 U5 4.0940(12) . ? U5 O25U 2.043(15) . ? U5 O35U 2.135(19) . ? U5 O121 2.205(19) . ? U5 O345 2.218(14) . ? U5 O122 2.423(18) . ? U5 N122 2.55(3) . ? U5 N121 2.62(3) . ? O1 C1 1.32(3) . ? O2 C20 1.32(3) . ? N1 C7 1.31(3) . ? N1 C8 1.39(3) . ? N2 C14 1.31(3) . ? N2 C13 1.39(3) . ? C1 C2 1.38(3) . ? C1 C6 1.44(3) . ? C2 C3 1.36(3) . ? C2 C21 1.53(4) . ? C3 C4 1.44(4) . ? C4 C5 1.33(4) . ? C4 C25 1.55(3) . ? C5 C6 1.42(3) . ? C6 C7 1.41(4) . ? C8 C13 1.42(4) . ? C8 C9 1.45(4) . ? C9 C10 1.45(4) . ? C10 C11 1.51(5) . ? C11 C12 1.43(5) . ? C12 C13 1.45(4) . ? C14 C15 1.48(3) . ? C15 C16 1.38(4) . ? C15 C20 1.39(3) . ? C16 C17 1.35(4) . ? C17 C18 1.43(4) . ? C17 C29 1.50(4) . ? C18 C19 1.38(3) . ? C19 C20 1.41(3) . ? C19 C33 1.52(3) . ? C21 C24 1.52(4) . ? C21 C22 1.52(4) . ? C21 C23 1.56(4) . ? C25 C27 1.49(4) . ? C25 C26 1.50(5) . ? C25 C28 1.51(4) . ? C29 C32 1.49(4) . ? C29 C30 1.54(5) . ? C29 C31 1.59(4) . ? C33 C36 1.52(3) . ? C33 C35 1.53(3) . ? C33 C34 1.58(3) . ? O41 C41 1.31(3) . ? O42 C60 1.37(3) . ? N41 C47 1.28(3) . ? N41 C48 1.37(3) . ? N42 C53 1.31(3) . ? N42 C54 1.35(3) . ? C41 C46 1.41(4) . ? C41 C42 1.43(3) . ? C42 C43 1.38(4) . ? C42 C61 1.55(4) . ? C43 C44 1.46(5) . ? C44 C45 1.37(4) . ? C44 C65 1.55(4) . ? C45 C46 1.41(3) . ? C46 C47 1.41(3) . ? C48 C53 1.33(3) . ? C48 C49 1.52(3) . ? C49 C50 1.38(4) . ? C50 C51 1.37(4) . ? C51 C52 1.41(4) . ? C52 C53 1.46(3) . ? C54 C55 1.46(3) . ? C55 C56 1.38(3) . ? C55 C60 1.41(3) . ? C56 C57 1.41(3) . ? C57 C58 1.36(3) . ? C57 C69 1.54(4) . ? C58 C59 1.38(3) . ? C59 C60 1.41(3) . ? C59 C73 1.54(3) . ? C61 C62 1.49(4) . ? C61 C63 1.52(4) . ? C61 C64 1.52(4) . ? C65 C68 1.39(5) . ? C65 C66 1.47(7) . ? C65 C67 1.55(5) . ? C69 C72 1.50(4) . ? C69 C71 1.53(4) . ? C69 C70 1.54(4) . ? C73 C74 1.44(4) . ? C73 C76 1.50(4) . ? C73 C75 1.63(4) . ? O81 C81 1.32(3) . ? O82 C96 1.34(3) . ? N81 C87 1.23(4) . ? N81 C88 1.42(4) . ? N82 C90 1.31(4) . ? N82 C89 1.48(4) . ? C81 C82 1.35(4) . ? C81 C86 1.41(3) . ? C82 C83 1.38(4) . ? C83 C84 1.34(4) . ? C84 C85 1.30(5) . ? C85 C86 1.43(4) . ? C86 C87 1.44(4) . ? C88 C89 1.44(6) . ? C90 C91 1.41(4) . ? C91 C96 1.41(4) . ? C91 C92 1.46(4) . ? C92 C93 1.35(5) . ? C93 C94 1.31(4) . ? C94 C95 1.34(4) . ? C95 C96 1.37(3) . ? O101 C101 1.36(4) . ? O102 C116 1.29(3) . ? N101 C107 1.28(5) . ? N101 C108 1.47(5) . ? N102 C110 1.32(4) . ? N102 C109 1.52(4) . ? C101 C106 1.32(5) . ? C101 C102 1.38(5) . ? C102 C103 1.38(6) . ? C103 C104 1.10(9) . ? C104 C105 1.50(9) . ? C105 C106 1.43(6) . ? C106 C107 1.48(6) . ? C108 C109 1.51(5) . ? C110 C111 1.36(5) . ? C111 C116 1.44(4) . ? C111 C112 1.46(5) . ? C112 C113 1.36(6) . ? C113 C114 1.27(6) . ? C114 C115 1.31(4) . ? C115 C116 1.39(4) . ? O121 C121 1.28(3) . ? O122 C136 1.39(3) . ? N121 C127 1.32(7) . ? N121 C128 1.47(6) . ? N122 C130 1.31(6) . ? N122 C129 1.59(5) . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C124 C125 1.3900 . ? C125 C126 1.3900 . ? C126 C127 1.37(7) . ? C128 C129 1.58(7) . ? C130 C131 1.41(7) . ? C131 C132 1.37(6) . ? C131 C136 1.38(5) . ? C132 C133 1.38(9) . ? C133 C134 1.36(9) . ? C134 C135 1.37(5) . ? C135 C136 1.41(5) . ? N141 C141 1.152(10) . ? C141 C142 1.403(10) . ? N142 C143 1.12(6) . ? C143 C144 1.43(6) . ? N143 C145 1.13(5) . ? C145 C146 1.43(6) . ? N144 C147 1.154(10) . ? C147 C148 1.403(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13U U1 O1 104.9(6) . . ? O13U U1 O14U 91.2(6) . . ? O1 U1 O14U 91.9(6) . . ? O13U U1 O2 161.6(6) . . ? O1 U1 O2 92.4(7) . . ? O14U U1 O2 94.6(6) . . ? O13U U1 O82 68.3(5) . . ? O1 U1 O82 167.2(5) . . ? O14U U1 O82 77.7(5) . . ? O2 U1 O82 95.8(6) . . ? O13U U1 N1 75.2(6) . . ? O1 U1 N1 69.6(6) . . ? O14U U1 N1 152.6(7) . . ? O2 U1 N1 105.8(6) . . ? O82 U1 N1 117.1(6) . . ? O13U U1 N2 95.5(6) . . ? O1 U1 N2 117.6(6) . . ? O14U U1 N2 146.6(7) . . ? O2 U1 N2 70.3(6) . . ? O82 U1 N2 74.6(6) . . ? N1 U1 N2 59.8(8) . . ? O13U U1 U3 29.0(4) . . ? O1 U1 U3 130.5(4) . . ? O14U U1 U3 78.2(4) . . ? O2 U1 U3 136.2(5) . . ? O82 U1 U3 40.4(4) . . ? N1 U1 U3 98.3(4) . . ? N2 U1 U3 92.3(4) . . ? O13U U1 U4 77.3(4) . . ? O1 U1 U4 101.0(4) . . ? O14U U1 U4 15.0(4) . . ? O2 U1 U4 106.0(4) . . ? O82 U1 U4 67.3(3) . . ? N1 U1 U4 147.2(5) . . ? N2 U1 U4 141.2(5) . . ? U3 U1 U4 63.14(2) . . ? O42 U2 O25U 96.0(6) . . ? O42 U2 O41 92.3(6) . . ? O25U U2 O41 171.6(6) . . ? O42 U2 O24U 98.2(6) . . ? O25U U2 O24U 86.7(6) . . ? O41 U2 O24U 91.1(5) . . ? O42 U2 O122 165.0(6) . . ? O25U U2 O122 69.3(6) . . ? O41 U2 O122 102.4(6) . . ? O24U U2 O122 78.4(5) . . ? O42 U2 N41 113.4(6) . . ? O25U U2 N41 108.1(6) . . ? O41 U2 N41 69.2(6) . . ? O24U U2 N41 142.7(6) . . ? O122 U2 N41 75.6(6) . . ? O42 U2 N42 71.7(6) . . ? O25U U2 N42 74.1(6) . . ? O41 U2 N42 109.6(5) . . ? O24U U2 N42 156.8(6) . . ? O122 U2 N42 105.9(5) . . ? N41 U2 N42 58.3(6) . . ? O42 U2 U5 124.4(4) . . ? O25U U2 U5 29.1(4) . . ? O41 U2 U5 142.5(4) . . ? O24U U2 U5 77.3(4) . . ? O122 U2 U5 40.7(5) . . ? N41 U2 U5 99.0(4) . . ? N42 U2 U5 91.2(4) . . ? O42 U2 U4 106.4(4) . . ? O25U U2 U4 74.9(4) . . ? O41 U2 U4 101.8(4) . . ? O24U U2 U4 13.9(4) . . ? O122 U2 U4 67.6(4) . . ? N41 U2 U4 139.4(4) . . ? N42 U2 U4 148.6(4) . . ? U5 U2 U4 63.43(2) . . ? O13U U3 O35U 177.2(7) . . ? O13U U3 O81 90.9(7) . . ? O35U U3 O81 86.5(8) . . ? O13U U3 O345 105.0(5) . . ? O35U U3 O345 74.1(6) . . ? O81 U3 O345 94.6(6) . . ? O13U U3 O82 70.2(5) . . ? O35U U3 O82 112.0(7) . . ? O81 U3 O82 157.1(6) . . ? O345 U3 O82 78.6(5) . . ? O13U U3 N81 92.8(7) . . ? O35U U3 N81 87.4(7) . . ? O81 U3 N81 69.8(7) . . ? O345 U3 N81 156.7(6) . . ? O82 U3 N81 122.3(6) . . ? O13U U3 N82 105.4(6) . . ? O35U U3 N82 77.2(7) . . ? O81 U3 N82 133.7(7) . . ? O345 U3 N82 121.0(7) . . ? O82 U3 N82 66.3(6) . . ? N81 U3 N82 66.5(8) . . ? O13U U3 U5 143.6(4) . . ? O35U U3 U5 35.3(5) . . ? O81 U3 U5 89.6(5) . . ? O345 U3 U5 38.8(3) . . ? O82 U3 U5 98.0(3) . . ? N81 U3 U5 121.2(5) . . ? N82 U3 U5 100.2(6) . . ? O13U U3 U1 30.6(4) . . ? O35U U3 U1 151.1(6) . . ? O81 U3 U1 117.8(5) . . ? O345 U3 U1 87.9(3) . . ? O82 U3 U1 40.8(3) . . ? N81 U3 U1 114.5(5) . . ? N82 U3 U1 93.9(5) . . ? U5 U3 U1 123.67(3) . . ? O13U U3 U4 78.7(4) . . ? O35U U3 U4 100.4(5) . . ? O81 U3 U4 96.5(4) . . ? O345 U3 U4 26.3(3) . . ? O82 U3 U4 67.9(3) . . ? N81 U3 U4 163.9(6) . . ? N82 U3 U4 128.8(6) . . ? U5 U3 U4 65.13(2) . . ? U1 U3 U4 63.73(2) . . ? O24U U4 O14U 174.7(6) . . ? O24U U4 O101 88.7(6) . . ? O14U U4 O101 93.8(6) . . ? O24U U4 O102 93.7(6) . . ? O14U U4 O102 85.5(7) . . ? O101 U4 O102 159.9(6) . . ? O24U U4 O345 90.4(5) . . ? O14U U4 O345 94.6(5) . . ? O101 U4 O345 82.3(6) . . ? O102 U4 O345 77.7(6) . . ? O24U U4 N101 94.7(7) . . ? O14U U4 N101 82.1(7) . . ? O101 U4 N101 66.0(9) . . ? O102 U4 N101 133.4(9) . . ? O345 U4 N101 147.8(9) . . ? O24U U4 N102 83.1(6) . . ? O14U U4 N102 91.7(7) . . ? O101 U4 N102 131.0(8) . . ? O102 U4 N102 69.1(7) . . ? O345 U4 N102 145.6(7) . . ? N101 U4 N102 66.6(10) . . ? O24U U4 U3 114.2(4) . . ? O14U U4 U3 70.2(4) . . ? O101 U4 U3 95.3(4) . . ? O102 U4 U3 65.6(4) . . ? O345 U4 U3 26.9(3) . . ? N101 U4 U3 145.7(6) . . ? N102 U4 U3 132.0(6) . . ? O24U U4 U2 16.0(4) . . ? O14U U4 U2 169.0(4) . . ? O101 U4 U2 84.8(4) . . ? O102 U4 U2 92.2(4) . . ? O345 U4 U2 74.5(3) . . ? N101 U4 U2 107.0(6) . . ? N102 U4 U2 97.5(5) . . ? U3 U4 U2 99.07(2) . . ? O24U U4 U1 166.9(4) . . ? O14U U4 U1 17.1(4) . . ? O101 U4 U1 95.8(4) . . ? O102 U4 U1 77.8(4) . . ? O345 U4 U1 78.0(3) . . ? N101 U4 U1 98.4(5) . . ? N102 U4 U1 102.9(5) . . ? U3 U4 U1 53.132(19) . . ? U2 U4 U1 152.18(3) . . ? O24U U4 U5 69.2(4) . . ? O14U U4 U5 116.0(5) . . ? O101 U4 U5 72.6(4) . . ? O102 U4 U5 89.6(4) . . ? O345 U4 U5 23.5(3) . . ? N101 U4 U5 135.9(8) . . ? N102 U4 U5 144.0(5) . . ? U3 U4 U5 50.42(2) . . ? U2 U4 U5 53.22(2) . . ? U1 U4 U5 100.31(2) . . ? O25U U5 O35U 174.5(7) . . ? O25U U5 O121 90.2(7) . . ? O35U U5 O121 87.5(8) . . ? O25U U5 O345 100.0(6) . . ? O35U U5 O345 75.4(5) . . ? O121 U5 O345 96.8(8) . . ? O25U U5 O122 70.8(6) . . ? O35U U5 O122 110.4(7) . . ? O121 U5 O122 157.9(7) . . ? O345 U5 O122 76.3(5) . . ? O25U U5 N122 110.2(6) . . ? O35U U5 N122 74.9(6) . . ? O121 U5 N122 132.7(9) . . ? O345 U5 N122 119.5(7) . . ? O122 U5 N122 66.8(6) . . ? O25U U5 N121 94.0(10) . . ? O35U U5 N121 89.7(9) . . ? O121 U5 N121 67.5(12) . . ? O345 U5 N121 159.1(7) . . ? O122 U5 N121 123.4(9) . . ? N122 U5 N121 68.9(13) . . ? O25U U5 U3 140.5(5) . . ? O35U U5 U3 34.9(4) . . ? O121 U5 U3 93.2(5) . . ? O345 U5 U3 40.5(3) . . ? O122 U5 U3 94.6(3) . . ? N122 U5 U3 96.0(4) . . ? N121 U5 U3 123.5(7) . . ? O25U U5 U2 31.7(5) . . ? O35U U5 U2 148.3(5) . . ? O121 U5 U2 119.7(6) . . ? O345 U5 U2 84.8(4) . . ? O122 U5 U2 39.7(4) . . ? N122 U5 U2 94.5(4) . . ? N121 U5 U2 114.7(6) . . ? U3 U5 U2 120.72(3) . . ? O25U U5 U4 76.1(5) . . ? O35U U5 U4 99.3(4) . . ? O121 U5 U4 97.9(8) . . ? O345 U5 U4 23.9(3) . . ? O122 U5 U4 67.3(4) . . ? N122 U5 U4 127.8(6) . . ? N121 U5 U4 162.6(12) . . ? U3 U5 U4 64.45(2) . . ? U2 U5 U4 63.35(2) . . ? U5 O345 U4 132.5(6) . . ? U5 O345 U3 100.7(5) . . ? U4 O345 U3 126.8(6) . . ? U3 O13U U1 120.4(7) . . ? U4 O14U U1 147.9(8) . . ? U4 O24U U2 150.1(8) . . ? U5 O25U U2 119.1(8) . . ? U3 O35U U5 109.8(6) . . ? C1 O1 U1 150.6(15) . . ? C20 O2 U1 143.6(17) . . ? C7 N1 C8 121(2) . . ? C7 N1 U1 127.9(18) . . ? C8 N1 U1 110.9(17) . . ? C14 N2 C13 118(2) . . ? C14 N2 U1 125.9(17) . . ? C13 N2 U1 115.5(17) . . ? O1 C1 C2 124(2) . . ? O1 C1 C6 117(2) . . ? C2 C1 C6 119(2) . . ? C3 C2 C1 118(2) . . ? C3 C2 C21 122(2) . . ? C1 C2 C21 120(2) . . ? C2 C3 C4 126(3) . . ? C5 C4 C3 115(2) . . ? C5 C4 C25 125(2) . . ? C3 C4 C25 120(3) . . ? C4 C5 C6 122(2) . . ? C7 C6 C5 116(2) . . ? C7 C6 C1 125(2) . . ? C5 C6 C1 119(2) . . ? N1 C7 C6 129(2) . . ? N1 C8 C13 120(2) . . ? N1 C8 C9 120(3) . . ? C13 C8 C9 119(3) . . ? C10 C9 C8 115(3) . . ? C9 C10 C11 125(3) . . ? C12 C11 C10 117(3) . . ? C11 C12 C13 117(3) . . ? N2 C13 C8 110(2) . . ? N2 C13 C12 124(3) . . ? C8 C13 C12 126(3) . . ? N2 C14 C15 128(2) . . ? C16 C15 C20 120(2) . . ? C16 C15 C14 117(2) . . ? C20 C15 C14 123(3) . . ? C17 C16 C15 124(3) . . ? C16 C17 C18 113(3) . . ? C16 C17 C29 127(3) . . ? C18 C17 C29 120(3) . . ? C19 C18 C17 127(2) . . ? C18 C19 C20 116(2) . . ? C18 C19 C33 121(2) . . ? C20 C19 C33 123(2) . . ? O2 C20 C15 122(2) . . ? O2 C20 C19 118(2) . . ? C15 C20 C19 120(2) . . ? C24 C21 C22 108(2) . . ? C24 C21 C2 113(2) . . ? C22 C21 C2 110(2) . . ? C24 C21 C23 108(2) . . ? C22 C21 C23 109(2) . . ? C2 C21 C23 109(2) . . ? C27 C25 C26 112(3) . . ? C27 C25 C28 107(2) . . ? C26 C25 C28 107(3) . . ? C27 C25 C4 111(2) . . ? C26 C25 C4 111(2) . . ? C28 C25 C4 110(2) . . ? C32 C29 C17 111(3) . . ? C32 C29 C30 107(3) . . ? C17 C29 C30 111(2) . . ? C32 C29 C31 107(2) . . ? C17 C29 C31 110(3) . . ? C30 C29 C31 110(3) . . ? C36 C33 C19 109.2(19) . . ? C36 C33 C35 112(2) . . ? C19 C33 C35 111.3(19) . . ? C36 C33 C34 105(2) . . ? C19 C33 C34 113(2) . . ? C35 C33 C34 106.4(19) . . ? C41 O41 U2 148.7(15) . . ? C60 O42 U2 146.0(16) . . ? C47 N41 C48 122.3(19) . . ? C47 N41 U2 127.7(15) . . ? C48 N41 U2 109.9(13) . . ? C53 N42 C54 119.2(19) . . ? C53 N42 U2 116.1(15) . . ? C54 N42 U2 124.4(13) . . ? O41 C41 C46 119(2) . . ? O41 C41 C42 122(2) . . ? C46 C41 C42 119(2) . . ? C43 C42 C41 119(3) . . ? C43 C42 C61 119(2) . . ? C41 C42 C61 122(2) . . ? C42 C43 C44 122(3) . . ? C45 C44 C43 117(3) . . ? C45 C44 C65 121(3) . . ? C43 C44 C65 122(3) . . ? C44 C45 C46 123(3) . . ? C45 C46 C47 118(2) . . ? C45 C46 C41 120(2) . . ? C47 C46 C41 123(2) . . ? N41 C47 C46 131(2) . . ? C53 C48 N41 121.3(18) . . ? C53 C48 C49 119(2) . . ? N41 C48 C49 120(2) . . ? C50 C49 C48 119(2) . . ? C51 C50 C49 119(2) . . ? C50 C51 C52 124(2) . . ? C51 C52 C53 117(2) . . ? N42 C53 C48 112(2) . . ? N42 C53 C52 126(2) . . ? C48 C53 C52 122(2) . . ? N42 C54 C55 130.3(19) . . ? C56 C55 C60 119(2) . . ? C56 C55 C54 117(2) . . ? C60 C55 C54 124(2) . . ? C55 C56 C57 123(2) . . ? C58 C57 C56 114(2) . . ? C58 C57 C69 126(2) . . ? C56 C57 C69 120(2) . . ? C57 C58 C59 127(2) . . ? C58 C59 C60 117(2) . . ? C58 C59 C73 122(2) . . ? C60 C59 C73 121(2) . . ? O42 C60 C59 121(2) . . ? O42 C60 C55 120(2) . . ? C59 C60 C55 119(2) . . ? C62 C61 C63 105(3) . . ? C62 C61 C64 111(3) . . ? C63 C61 C64 110(2) . . ? C62 C61 C42 112(2) . . ? C63 C61 C42 111(2) . . ? C64 C61 C42 108(2) . . ? C68 C65 C66 103(4) . . ? C68 C65 C67 114(4) . . ? C66 C65 C67 106(4) . . ? C68 C65 C44 116(3) . . ? C66 C65 C44 107(3) . . ? C67 C65 C44 110(3) . . ? C72 C69 C71 109(3) . . ? C72 C69 C70 107(2) . . ? C71 C69 C70 109(2) . . ? C72 C69 C57 115(2) . . ? C71 C69 C57 107(2) . . ? C70 C69 C57 110(2) . . ? C74 C73 C76 106(3) . . ? C74 C73 C59 114(2) . . ? C76 C73 C59 111(2) . . ? C74 C73 C75 106(2) . . ? C76 C73 C75 110(2) . . ? C59 C73 C75 110(2) . . ? C81 O81 U3 148.9(16) . . ? C96 O82 U3 137.9(13) . . ? C96 O82 U1 123.1(13) . . ? U3 O82 U1 98.7(5) . . ? C87 N81 C88 119(3) . . ? C87 N81 U3 128(2) . . ? C88 N81 U3 113(2) . . ? C90 N82 C89 116(3) . . ? C90 N82 U3 131.1(19) . . ? C89 N82 U3 113(2) . . ? O81 C81 C82 125(2) . . ? O81 C81 C86 119(3) . . ? C82 C81 C86 116(3) . . ? C81 C82 C83 125(3) . . ? C84 C83 C82 121(3) . . ? C85 C84 C83 116(3) . . ? C84 C85 C86 128(3) . . ? C81 C86 C85 115(3) . . ? C81 C86 C87 122(3) . . ? C85 C86 C87 123(3) . . ? N81 C87 C86 132(3) . . ? N81 C88 C89 118(3) . . ? C88 C89 N82 112(3) . . ? N82 C90 C91 126(3) . . ? C96 C91 C90 126(3) . . ? C96 C91 C92 115(3) . . ? C90 C91 C92 119(3) . . ? C93 C92 C91 123(3) . . ? C94 C93 C92 118(3) . . ? C93 C94 C95 125(3) . . ? C94 C95 C96 121(3) . . ? O82 C96 C95 123(2) . . ? O82 C96 C91 118(2) . . ? C95 C96 C91 119(3) . . ? C101 O101 U4 153(2) . . ? C116 O102 U4 146.5(18) . . ? C107 N101 C108 109(4) . . ? C107 N101 U4 133(3) . . ? C108 N101 U4 118(3) . . ? C110 N102 C109 119(3) . . ? C110 N102 U4 128.9(19) . . ? C109 N102 U4 112(2) . . ? C106 C101 O101 121(4) . . ? C106 C101 C102 119(4) . . ? O101 C101 C102 120(3) . . ? C101 C102 C103 113(5) . . ? C104 C103 C102 141(8) . . ? C103 C104 C105 108(6) . . ? C106 C105 C104 120(5) . . ? C101 C106 C105 120(5) . . ? C101 C106 C107 121(4) . . ? C105 C106 C107 119(4) . . ? N101 C107 C106 126(4) . . ? N101 C108 C109 110(4) . . ? C108 C109 N102 111(3) . . ? N102 C110 C111 129(3) . . ? C110 C111 C116 123(3) . . ? C110 C111 C112 121(3) . . ? C116 C111 C112 117(4) . . ? C113 C112 C111 118(4) . . ? C114 C113 C112 124(6) . . ? C113 C114 C115 121(5) . . ? C114 C115 C116 124(4) . . ? O102 C116 C115 120(3) . . ? O102 C116 C111 123(3) . . ? C115 C116 C111 117(3) . . ? C121 O121 U5 154(2) . . ? C136 O122 U2 121.2(16) . . ? C136 O122 U5 137.5(17) . . ? U2 O122 U5 99.7(7) . . ? C127 N121 C128 124(5) . . ? C127 N121 U5 126(4) . . ? C128 N121 U5 109(3) . . ? C130 N122 C129 108(4) . . ? C130 N122 U5 135(3) . . ? C129 N122 U5 116(2) . . ? O121 C121 C122 122.8(18) . . ? O121 C121 C126 116.6(17) . . ? C122 C121 C126 120.0 . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C123 C124 C125 120.0 . . ? C126 C125 C124 120.0 . . ? C127 C126 C125 115(3) . . ? C127 C126 C121 124(3) . . ? C125 C126 C121 120.0 . . ? N121 C127 C126 130(6) . . ? N121 C128 C129 121(5) . . ? C128 C129 N122 99(4) . . ? N122 C130 C131 128(3) . . ? C132 C131 C136 119(5) . . ? C132 C131 C130 119(5) . . ? C136 C131 C130 122(4) . . ? C131 C132 C133 123(5) . . ? C134 C133 C132 117(4) . . ? C133 C134 C135 123(5) . . ? C134 C135 C136 119(5) . . ? C131 C136 O122 122(4) . . ? C131 C136 C135 119(3) . . ? O122 C136 C135 119(3) . . ? N141 C141 C142 172(8) . . ? N142 C143 C144 174(7) . . ? N143 C145 C146 179(5) . . ? N144 C147 C148 169(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.103 _refine_diff_density_min -3.148 _refine_diff_density_rms 0.250