# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 _publ_contact_author_name 'Dr Lionel Salmon' _publ_contact_author_address ; DSM/DRECAM/SCM CEA Saclay Service de Chimie Moleculaire Bat 125 p 26 CEA Saclay Gif-sur-Yvette 91191 FRANCE ; _publ_contact_author_email SALMON@DRECAM.CEA.FR _publ_requested_journal 'New J. Chem.' _publ_section_title ; Synthesis, structure and magnetic behaviour of dinuclear uranium(IV) complexes with a 'calixsalophen' type macrocycle ; loop_ _publ_author_name L.Salmon P.Thuery E.Riviere S.Miyamoto, T.Yamato M.Ephritikhine data_1.4thf _database_code_depnum_ccdc_archive 'CCDC 609879' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H88 Cl4 N4 O8 U2' _chemical_formula_weight 1755.32 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8168(5) _cell_length_b 12.6942(7) _cell_length_c 12.9752(7) _cell_angle_alpha 86.737(2) _cell_angle_beta 65.501(3) _cell_angle_gamma 79.661(4) _cell_volume 1742.02(16) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 53669 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method ? _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 4.853 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.328 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53669 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6616 _reflns_number_gt 5735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+2.9719P] 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 6616 _refine_ls_number_parameters 412 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.738 _refine_diff_density_min -1.361 _refine_diff_density_rms 0.115 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.823129(17) 0.960460(16) 0.561586(15) 0.02408(6) Uani 1 1 d . . . Cl1 Cl 1.05789(11) 0.88131(10) 0.39340(9) 0.0276(3) Uani 1 1 d . . . Cl2 Cl 0.60210(12) 1.03764(11) 0.71959(10) 0.0355(3) Uani 1 1 d . . . N1 N 0.7601(4) 0.7785(3) 0.6002(3) 0.0263(9) Uani 1 1 d . . . N2 N 0.6962(4) 0.9078(3) 0.4566(3) 0.0258(9) Uani 1 1 d . . . O1 O 0.9167(3) 0.8681(3) 0.6594(3) 0.0254(7) Uani 1 1 d . . . O2 O 0.8252(3) 1.0716(3) 0.4293(3) 0.0261(7) Uani 1 1 d . . . O3 O 0.7630(4) 0.4465(3) 0.6447(4) 0.0530(11) Uani 1 1 d . . . O4 O 0.6694(4) 0.6848(3) 0.8805(3) 0.0493(10) Uani 1 1 d . . . C1 C 1.0679(4) 0.7497(4) 0.7093(4) 0.0257(10) Uani 1 1 d . . . C2 C 0.9727(4) 0.7700(4) 0.6694(4) 0.0274(11) Uani 1 1 d . . . C3 C 0.9321(4) 0.6802(4) 0.6439(4) 0.0265(10) Uani 1 1 d . . . C4 C 0.9853(5) 0.5754(4) 0.6587(4) 0.0283(11) Uani 1 1 d . . . H4 H 0.9569 0.5183 0.6406 0.034 Uiso 1 1 calc R . . C5 C 1.0778(4) 0.5542(4) 0.6990(4) 0.0266(10) Uani 1 1 d . . . C6 C 1.1172(4) 0.6441(4) 0.7234(4) 0.0264(10) Uani 1 1 d . . . H6 H 1.1798 0.6327 0.7505 0.032 Uiso 1 1 calc R . . C7 C 1.1315(5) 0.4415(4) 0.7242(4) 0.0311(11) Uani 1 1 d . . . C8 C 1.2761(5) 0.4199(5) 0.6636(6) 0.0510(16) Uani 1 1 d . . . H8A H 1.3012 0.4268 0.5834 0.076 Uiso 1 1 calc R . . H8B H 1.3077 0.3486 0.6795 0.076 Uiso 1 1 calc R . . H8C H 1.3098 0.4706 0.6901 0.076 Uiso 1 1 calc R . . C9 C 1.0914(6) 0.4336(5) 0.8534(5) 0.0435(14) Uani 1 1 d . . . H9A H 1.1340 0.4788 0.8765 0.065 Uiso 1 1 calc R . . H9B H 1.1135 0.3608 0.8721 0.065 Uiso 1 1 calc R . . H9C H 1.0018 0.4563 0.8918 0.065 Uiso 1 1 calc R . . C10 C 1.0811(5) 0.3547(4) 0.6870(5) 0.0373(12) Uani 1 1 d . . . H10A H 0.9911 0.3639 0.7280 0.056 Uiso 1 1 calc R . . H10B H 1.1187 0.2855 0.7022 0.056 Uiso 1 1 calc R . . H10C H 1.1020 0.3602 0.6073 0.056 Uiso 1 1 calc R . . C11 C 0.8239(4) 0.6900(4) 0.6178(4) 0.0255(10) Uani 1 1 d . . . H11 H 0.7967 0.6268 0.6131 0.031 Uiso 1 1 calc R . . C12 C 0.6458(4) 0.7681(4) 0.5915(4) 0.0271(11) Uani 1 1 d . . . C13 C 0.6131(4) 0.8339(4) 0.5144(4) 0.0262(10) Uani 1 1 d . . . C14 C 0.5043(4) 0.8264(4) 0.5019(4) 0.0291(11) Uani 1 1 d . . . H14 H 0.4810 0.8710 0.4521 0.035 Uiso 1 1 calc R . . C15 C 0.4300(4) 0.7528(4) 0.5634(4) 0.0295(11) Uani 1 1 d . . . H15 H 0.3589 0.7459 0.5522 0.035 Uiso 1 1 calc R . . C16 C 0.4609(5) 0.6890(4) 0.6419(4) 0.0331(12) Uani 1 1 d . . . H16 H 0.4096 0.6407 0.6842 0.040 Uiso 1 1 calc R . . C17 C 0.5684(5) 0.6977(4) 0.6567(4) 0.0307(11) Uani 1 1 d . . . H17 H 0.5886 0.6563 0.7102 0.037 Uiso 1 1 calc R . . C18 C 0.7024(4) 0.9382(4) 0.3576(4) 0.0275(10) Uani 1 1 d . . . H18 H 0.6584 0.9039 0.3285 0.033 Uiso 1 1 calc R . . C19 C 0.7685(4) 1.0179(4) 0.2873(4) 0.0260(10) Uani 1 1 d . . . C20 C 0.8297(4) 1.0830(4) 0.3250(4) 0.0240(10) Uani 1 1 d . . . C21 C 0.8830(4) 1.1649(4) 0.2543(4) 0.0239(10) Uani 1 1 d . . . C22 C 0.8775(4) 1.1763(4) 0.1484(4) 0.0293(11) Uani 1 1 d . . . H22 H 0.9173 1.2282 0.1005 0.035 Uiso 1 1 calc R . . C23 C 0.8152(5) 1.1137(4) 0.1110(4) 0.0284(11) Uani 1 1 d . . . C24 C 0.7609(5) 1.0351(4) 0.1823(4) 0.0272(11) Uani 1 1 d . . . H24 H 0.7182 0.9924 0.1604 0.033 Uiso 1 1 calc R . . C25 C 0.8069(5) 1.1388(4) -0.0028(4) 0.0325(11) Uani 1 1 d . . . C26 C 0.7458(6) 1.0574(5) -0.0352(5) 0.0450(14) Uani 1 1 d . . . H26A H 0.7963 0.9876 -0.0434 0.068 Uiso 1 1 calc R . . H26B H 0.7398 1.0772 -0.1055 0.068 Uiso 1 1 calc R . . H26C H 0.6628 1.0563 0.0231 0.068 Uiso 1 1 calc R . . C27 C 0.9387(5) 1.1388(5) -0.0971(4) 0.0436(14) Uani 1 1 d . . . H27A H 0.9894 1.0693 -0.1032 0.065 Uiso 1 1 calc R . . H27B H 0.9775 1.1915 -0.0796 0.065 Uiso 1 1 calc R . . H27C H 0.9320 1.1557 -0.1676 0.065 Uiso 1 1 calc R . . C28 C 0.7264(6) 1.2510(5) 0.0070(5) 0.0456(14) Uani 1 1 d . . . H28A H 0.7178 1.2672 -0.0628 0.068 Uiso 1 1 calc R . . H28B H 0.7668 1.3034 0.0224 0.068 Uiso 1 1 calc R . . H28C H 0.6443 1.2520 0.0675 0.068 Uiso 1 1 calc R . . C29 C 0.7126(6) 0.3768(5) 0.5989(5) 0.0491(15) Uani 1 1 d . . . H29A H 0.7781 0.3181 0.5568 0.059 Uiso 1 1 calc R . . H29B H 0.6796 0.4156 0.5480 0.059 Uiso 1 1 calc R . . C30 C 0.6097(7) 0.3348(7) 0.6953(7) 0.078(2) Uani 1 1 d U . . H30A H 0.6383 0.2621 0.7122 0.094 Uiso 1 1 calc R . . H30B H 0.5368 0.3360 0.6785 0.094 Uiso 1 1 calc R . . C31 C 0.5782(6) 0.4109(5) 0.7937(5) 0.0546(16) Uani 1 1 d . . . H31A H 0.5174 0.4736 0.7944 0.066 Uiso 1 1 calc R . . H31B H 0.5467 0.3757 0.8660 0.066 Uiso 1 1 calc R . . C32 C 0.7050(7) 0.4383(6) 0.7652(5) 0.064(2) Uani 1 1 d . . . H32A H 0.6970 0.5057 0.8014 0.077 Uiso 1 1 calc R . . H32B H 0.7551 0.3829 0.7907 0.077 Uiso 1 1 calc R . . C33 C 0.7334(6) 0.6595(5) 0.9539(5) 0.0534(16) Uani 1 1 d . . . H33A H 0.8238 0.6543 0.9113 0.064 Uiso 1 1 calc R . . H33B H 0.7165 0.5917 0.9905 0.064 Uiso 1 1 calc R . . C34 C 0.6828(6) 0.7501(5) 1.0418(5) 0.0496(15) Uani 1 1 d . . . H34A H 0.6455 0.7229 1.1178 0.060 Uiso 1 1 calc R . . H34B H 0.7496 0.7876 1.0364 0.060 Uiso 1 1 calc R . . C35 C 0.5839(5) 0.8235(5) 1.0135(5) 0.0438(14) Uani 1 1 d . . . H35A H 0.5003 0.8066 1.0570 0.053 Uiso 1 1 calc R . . H35B H 0.5832 0.8982 1.0265 0.053 Uiso 1 1 calc R . . C36 C 0.6284(6) 0.7986(5) 0.8898(5) 0.0445(14) Uani 1 1 d . . . H36A H 0.5603 0.8192 0.8655 0.053 Uiso 1 1 calc R . . H36B H 0.6975 0.8356 0.8445 0.053 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 U 0.02445(10) 0.02794(10) 0.02187(9) 0.00159(6) -0.01128(7) -0.00547(7) Cl1 0.0290(6) 0.0313(7) 0.0245(6) -0.0011(5) -0.0121(5) -0.0064(5) Cl2 0.0295(6) 0.0459(8) 0.0262(6) -0.0021(6) -0.0091(5) 0.0008(6) N1 0.027(2) 0.031(2) 0.024(2) 0.0046(17) -0.0106(18) -0.0117(18) N2 0.027(2) 0.027(2) 0.024(2) -0.0010(17) -0.0107(17) -0.0049(17) O1 0.0260(17) 0.0246(18) 0.0274(17) 0.0049(14) -0.0134(14) -0.0040(14) O2 0.0256(17) 0.0281(19) 0.0252(17) 0.0000(14) -0.0107(14) -0.0053(14) O3 0.062(3) 0.052(3) 0.052(3) 0.010(2) -0.025(2) -0.024(2) O4 0.054(3) 0.052(3) 0.041(2) -0.004(2) -0.021(2) -0.004(2) C1 0.024(2) 0.029(3) 0.023(2) 0.000(2) -0.009(2) -0.004(2) C2 0.026(2) 0.033(3) 0.020(2) 0.003(2) -0.006(2) -0.006(2) C3 0.024(2) 0.036(3) 0.022(2) 0.001(2) -0.012(2) -0.005(2) C4 0.032(3) 0.027(3) 0.027(2) 0.001(2) -0.012(2) -0.008(2) C5 0.023(2) 0.034(3) 0.022(2) -0.001(2) -0.008(2) -0.005(2) C6 0.024(2) 0.035(3) 0.024(2) 0.003(2) -0.014(2) -0.006(2) C7 0.033(3) 0.029(3) 0.034(3) 0.001(2) -0.016(2) -0.004(2) C8 0.039(3) 0.035(3) 0.073(4) 0.001(3) -0.019(3) -0.002(3) C9 0.067(4) 0.034(3) 0.038(3) 0.004(2) -0.031(3) -0.006(3) C10 0.043(3) 0.030(3) 0.044(3) 0.001(2) -0.023(3) -0.005(2) C11 0.032(3) 0.024(3) 0.024(2) 0.0040(19) -0.014(2) -0.009(2) C12 0.029(2) 0.034(3) 0.024(2) -0.002(2) -0.015(2) -0.008(2) C13 0.027(2) 0.032(3) 0.023(2) -0.004(2) -0.012(2) -0.005(2) C14 0.029(3) 0.028(3) 0.027(3) -0.001(2) -0.010(2) -0.002(2) C15 0.022(2) 0.037(3) 0.030(3) -0.006(2) -0.010(2) -0.005(2) C16 0.031(3) 0.037(3) 0.033(3) 0.006(2) -0.012(2) -0.014(2) C17 0.032(3) 0.032(3) 0.030(3) 0.006(2) -0.014(2) -0.008(2) C18 0.024(2) 0.033(3) 0.025(2) -0.003(2) -0.011(2) -0.002(2) C19 0.025(2) 0.031(3) 0.023(2) 0.002(2) -0.011(2) -0.005(2) C20 0.023(2) 0.029(3) 0.021(2) 0.0013(19) -0.009(2) -0.006(2) C21 0.021(2) 0.025(3) 0.025(2) -0.0030(19) -0.010(2) -0.0008(19) C22 0.026(2) 0.032(3) 0.027(3) 0.006(2) -0.009(2) -0.005(2) C23 0.029(3) 0.036(3) 0.024(2) -0.001(2) -0.014(2) -0.006(2) C24 0.029(3) 0.028(3) 0.028(3) 0.001(2) -0.014(2) -0.006(2) C25 0.035(3) 0.039(3) 0.028(3) 0.005(2) -0.015(2) -0.011(2) C26 0.058(4) 0.058(4) 0.035(3) 0.005(3) -0.030(3) -0.021(3) C27 0.043(3) 0.066(4) 0.025(3) 0.010(3) -0.014(3) -0.019(3) C28 0.053(4) 0.052(4) 0.041(3) 0.010(3) -0.030(3) -0.007(3) C29 0.051(4) 0.041(4) 0.058(4) 0.004(3) -0.022(3) -0.015(3) C30 0.064(4) 0.081(5) 0.080(5) -0.021(4) -0.008(4) -0.035(4) C31 0.058(4) 0.050(4) 0.049(4) 0.008(3) -0.013(3) -0.017(3) C32 0.080(5) 0.085(5) 0.050(4) 0.022(4) -0.040(4) -0.044(4) C33 0.051(4) 0.056(4) 0.049(4) 0.007(3) -0.021(3) 0.000(3) C34 0.049(4) 0.063(4) 0.042(3) 0.008(3) -0.023(3) -0.014(3) C35 0.039(3) 0.054(4) 0.039(3) 0.003(3) -0.016(3) -0.009(3) C36 0.040(3) 0.053(4) 0.038(3) 0.004(3) -0.015(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O2 2.154(3) . ? U O1 2.177(3) . ? U N1 2.514(4) . ? U N2 2.590(4) . ? U Cl2 2.6180(12) . ? U Cl1 2.7741(12) . ? U Cl1 2.8602(12) 2_776 ? U U 4.1010(4) 2_776 ? Cl1 U 2.8602(11) 2_776 ? N1 C11 1.301(6) . ? N1 C12 1.431(6) . ? N1 N2 2.666(5) . ? N1 O1 2.711(5) . ? N2 C18 1.297(6) . ? N2 C13 1.431(6) . ? N2 O2 2.716(5) . ? O1 C2 1.327(6) . ? O1 O2 3.005(4) 2_776 ? O1 O2 4.190(4) . ? O2 C20 1.333(5) . ? O3 C29 1.425(7) . ? O3 C32 1.430(7) . ? O4 C36 1.434(7) . ? O4 C33 1.435(7) . ? C1 C6 1.396(7) . ? C1 C2 1.402(7) . ? C1 C21 1.499(6) 2_776 ? C2 C3 1.418(7) . ? C3 C4 1.404(7) . ? C3 C11 1.436(6) . ? C4 C5 1.377(7) . ? C4 H4 0.9300 . ? C5 C6 1.405(7) . ? C5 C7 1.532(7) . ? C6 H6 0.9300 . ? C7 C10 1.529(7) . ? C7 C8 1.535(7) . ? C7 C9 1.543(7) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11 0.9300 . ? C12 C17 1.384(7) . ? C12 C13 1.400(7) . ? C13 C14 1.380(7) . ? C14 C15 1.382(7) . ? C14 H14 0.9300 . ? C15 C16 1.391(7) . ? C15 H15 0.9300 . ? C16 C17 1.385(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.433(7) . ? C18 H18 0.9300 . ? C19 C24 1.404(6) . ? C19 C20 1.414(6) . ? C20 C21 1.402(6) . ? C21 C22 1.400(6) . ? C21 C1 1.499(6) 2_776 ? C22 C23 1.400(7) . ? C22 H22 0.9300 . ? C23 C24 1.377(7) . ? C23 C25 1.532(6) . ? C24 H24 0.9300 . ? C25 C26 1.528(7) . ? C25 C27 1.531(7) . ? C25 C28 1.543(8) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.491(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.522(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.488(9) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.523(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.515(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.500(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U O1 150.68(12) . . ? O2 U N1 130.76(12) . . ? O1 U N1 70.18(12) . . ? O2 U N2 69.16(12) . . ? O1 U N2 132.28(12) . . ? N1 U N2 62.97(12) . . ? O2 U Cl2 99.29(9) . . ? O1 U Cl2 102.07(9) . . ? N1 U Cl2 87.88(10) . . ? N2 U Cl2 85.22(9) . . ? O2 U Cl1 80.16(9) . . ? O1 U Cl1 78.29(9) . . ? N1 U Cl1 92.84(9) . . ? N2 U Cl1 95.01(9) . . ? Cl2 U Cl1 179.27(4) . . ? O2 U Cl1 79.84(9) . 2_776 ? O1 U Cl1 79.27(9) . 2_776 ? N1 U Cl1 148.86(9) . 2_776 ? N2 U Cl1 148.12(9) . 2_776 ? Cl2 U Cl1 92.84(4) . 2_776 ? Cl1 U Cl1 86.60(3) . 2_776 ? U Cl1 U 93.40(3) . 2_776 ? C11 N1 C12 115.4(4) . . ? C11 N1 U 127.9(3) . . ? C12 N1 U 116.4(3) . . ? C18 N2 C13 117.1(4) . . ? C18 N2 U 127.6(3) . . ? C13 N2 U 115.3(3) . . ? C2 O1 U 142.0(3) . . ? C20 O2 U 145.6(3) . . ? C29 O3 C32 107.1(5) . . ? C36 O4 C33 106.0(4) . . ? C6 C1 C2 119.6(4) . . ? C6 C1 C21 116.1(4) . 2_776 ? C2 C1 C21 124.2(4) . 2_776 ? O1 C2 C1 123.0(4) . . ? O1 C2 C3 119.6(4) . . ? C1 C2 C3 117.3(5) . . ? C4 C3 C2 121.0(4) . . ? C4 C3 C11 115.8(4) . . ? C2 C3 C11 122.6(5) . . ? C5 C4 C3 122.4(5) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C4 C5 C6 115.8(5) . . ? C4 C5 C7 123.9(4) . . ? C6 C5 C7 120.2(4) . . ? C1 C6 C5 124.0(4) . . ? C1 C6 H6 118.0 . . ? C5 C6 H6 118.0 . . ? C10 C7 C5 112.1(4) . . ? C10 C7 C8 108.2(4) . . ? C5 C7 C8 110.8(4) . . ? C10 C7 C9 108.1(4) . . ? C5 C7 C9 108.2(4) . . ? C8 C7 C9 109.4(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C3 126.4(4) . . ? N1 C11 H11 116.8 . . ? C3 C11 H11 116.8 . . ? C17 C12 C13 120.4(4) . . ? C17 C12 N1 122.5(4) . . ? C13 C12 N1 117.1(4) . . ? C14 C13 C12 119.5(4) . . ? C14 C13 N2 125.1(4) . . ? C12 C13 N2 115.4(4) . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.4(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 119.8(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C12 C17 C16 119.7(5) . . ? C12 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? N2 C18 C19 128.2(4) . . ? N2 C18 H18 115.9 . . ? C19 C18 H18 115.9 . . ? C24 C19 C20 120.9(4) . . ? C24 C19 C18 116.9(4) . . ? C20 C19 C18 122.0(4) . . ? O2 C20 C21 122.0(4) . . ? O2 C20 C19 119.6(4) . . ? C21 C20 C19 118.1(4) . . ? C20 C21 C22 119.0(4) . . ? C20 C21 C1 123.7(4) . 2_776 ? C22 C21 C1 117.0(4) . 2_776 ? C23 C22 C21 123.4(4) . . ? C23 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? C24 C23 C22 116.9(4) . . ? C24 C23 C25 124.2(4) . . ? C22 C23 C25 118.9(4) . . ? C23 C24 C19 121.6(4) . . ? C23 C24 H24 119.2 . . ? C19 C24 H24 119.2 . . ? C26 C25 C23 112.0(4) . . ? C26 C25 C27 108.3(5) . . ? C23 C25 C27 110.4(4) . . ? C26 C25 C28 108.7(5) . . ? C23 C25 C28 108.3(4) . . ? C27 C25 C28 109.1(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 107.8(5) . . ? O3 C29 H29A 110.1 . . ? C30 C29 H29A 110.1 . . ? O3 C29 H29B 110.1 . . ? C30 C29 H29B 110.1 . . ? H29A C29 H29B 108.5 . . ? C29 C30 C31 104.1(5) . . ? C29 C30 H30A 110.9 . . ? C31 C30 H30A 110.9 . . ? C29 C30 H30B 110.9 . . ? C31 C30 H30B 110.9 . . ? H30A C30 H30B 109.0 . . ? C32 C31 C30 100.1(6) . . ? C32 C31 H31A 111.7 . . ? C30 C31 H31A 111.7 . . ? C32 C31 H31B 111.7 . . ? C30 C31 H31B 111.7 . . ? H31A C31 H31B 109.5 . . ? O3 C32 C31 106.4(5) . . ? O3 C32 H32A 110.4 . . ? C31 C32 H32A 110.4 . . ? O3 C32 H32B 110.4 . . ? C31 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? O4 C33 C34 106.4(5) . . ? O4 C33 H33A 110.4 . . ? C34 C33 H33A 110.4 . . ? O4 C33 H33B 110.4 . . ? C34 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C35 C34 C33 104.7(5) . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34B 110.8 . . ? C33 C34 H34B 110.8 . . ? H34A C34 H34B 108.9 . . ? C36 C35 C34 101.5(5) . . ? C36 C35 H35A 111.5 . . ? C34 C35 H35A 111.5 . . ? C36 C35 H35B 111.5 . . ? C34 C35 H35B 111.5 . . ? H35A C35 H35B 109.3 . . ? O4 C36 C35 104.2(5) . . ? O4 C36 H36A 110.9 . . ? C35 C36 H36A 110.9 . . ? O4 C36 H36B 110.9 . . ? C35 C36 H36B 110.9 . . ? H36A C36 H36B 108.9 . . ? #===END data_2.3py _database_code_depnum_ccdc_archive 'CCDC 609880' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H81 Cl4 N9 O4 U2' _chemical_formula_weight 1862.41 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' Cl Cl 0.1484 0.1585 '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 14.2822(9) _cell_length_b 12.0928(3) _cell_length_c 21.8206(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.604(3) _cell_angle_gamma 90.00 _cell_volume 3767.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 115077 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method ? _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 4.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.698 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and four \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 115077 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7153 _reflns_number_gt 5783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. One of the tert-butyl groups was found to be rotationally disordered over two positions which were refined with occupancy parameters constrained to sum to unity and restraints on displacement parameters. One of the pyridine solvent molecules is disordered around an inversion centre. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions (except in the disordered pyridine molecule) and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH~3~) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+25.7376P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7153 _refine_ls_number_parameters 488 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.374 _refine_diff_density_min -1.561 _refine_diff_density_rms 0.227 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.949314(18) 0.84467(2) 0.956519(11) 0.02485(10) Uani 1 1 d . . . Cl1 Cl 1.11229(12) 0.96159(15) 0.97145(8) 0.0299(4) Uani 1 1 d . . . Cl2 Cl 0.84254(13) 0.66075(16) 0.94723(9) 0.0364(4) Uani 1 1 d . . . O1 O 0.9437(3) 0.9668(4) 0.8829(2) 0.0237(10) Uani 1 1 d . . . O2 O 0.9938(3) 0.8039(4) 1.0499(2) 0.0231(10) Uani 1 1 d . . . N1 N 1.0201(4) 0.7720(4) 0.8556(3) 0.0243(12) Uani 1 1 d . . . N2 N 1.0600(4) 0.6713(5) 0.9599(3) 0.0255(12) Uani 1 1 d . . . N3 N 0.7628(4) 0.9074(5) 0.9380(3) 0.0351(15) Uani 1 1 d . . . N4 N 0.9180(5) 0.3367(6) 0.3482(3) 0.0447(17) Uani 1 1 d . . . C1 C 0.9858(5) 1.1236(5) 0.8226(3) 0.0229(14) Uani 1 1 d . . . C2 C 0.9935(5) 1.0103(6) 0.8381(3) 0.0234(14) Uani 1 1 d . . . C3 C 1.0515(5) 0.9445(5) 0.8019(3) 0.0235(14) Uani 1 1 d . . . C4 C 1.0999(5) 0.9904(6) 0.7527(3) 0.0261(15) Uani 1 1 d . . . H4 H 1.1380 0.9448 0.7298 0.031 Uiso 1 1 calc R . . C5 C 1.0929(5) 1.0994(6) 0.7376(3) 0.0251(14) Uani 1 1 d . . . C6 C 1.0339(5) 1.1643(6) 0.7735(3) 0.0259(14) Uani 1 1 d . . . H6 H 1.0268 1.2387 0.7636 0.031 Uiso 1 1 calc R . . C7 C 1.1445(5) 1.1555(6) 0.6843(3) 0.0314(16) Uani 1 1 d . . . C8 C 1.0710(6) 1.2103(7) 0.6408(4) 0.0396(19) Uani 1 1 d . . . H8A H 1.0360 1.2639 0.6631 0.059 Uiso 1 1 calc R . . H8B H 1.0293 1.1548 0.6244 0.059 Uiso 1 1 calc R . . H8C H 1.1022 1.2462 0.6078 0.059 Uiso 1 1 calc R . . C9 C 1.2010(6) 1.0722(7) 0.6481(4) 0.042(2) Uani 1 1 d . . . H9A H 1.2324 1.1096 0.6158 0.062 Uiso 1 1 calc R . . H9B H 1.1596 1.0172 0.6308 0.062 Uiso 1 1 calc R . . H9C H 1.2464 1.0372 0.6750 0.062 Uiso 1 1 calc R . . C10 C 1.2111(6) 1.2435(7) 0.7104(4) 0.0400(19) Uani 1 1 d . . . H10A H 1.2443 1.2771 0.6776 0.060 Uiso 1 1 calc R . . H10B H 1.2550 1.2099 0.7388 0.060 Uiso 1 1 calc R . . H10C H 1.1758 1.2990 0.7311 0.060 Uiso 1 1 calc R . . C11 C 1.0547(5) 0.8269(6) 0.8112(3) 0.0246(14) Uani 1 1 d . . . H11 H 1.0853 0.7859 0.7818 0.030 Uiso 1 1 calc R . . C12 C 1.0304(5) 0.6541(6) 0.8524(3) 0.0252(14) Uani 1 1 d . . . C13 C 1.0524(5) 0.6000(6) 0.9069(3) 0.0264(15) Uani 1 1 d . . . C14 C 1.0672(5) 0.4863(6) 0.9081(3) 0.0288(16) Uani 1 1 d . . . H14 H 1.0830 0.4505 0.9447 0.035 Uiso 1 1 calc R . . C15 C 1.0578(5) 0.4274(6) 0.8536(3) 0.0282(16) Uani 1 1 d . . . H15 H 1.0686 0.3515 0.8537 0.034 Uiso 1 1 calc R . . C16 C 1.0325(5) 0.4801(6) 0.7989(4) 0.0331(17) Uani 1 1 d . . . H16 H 1.0249 0.4392 0.7630 0.040 Uiso 1 1 calc R . . C17 C 1.0186(5) 0.5943(6) 0.7980(3) 0.0306(16) Uani 1 1 d . . . H17 H 1.0016 0.6301 0.7617 0.037 Uiso 1 1 calc R . . C18 C 1.1197(5) 0.6391(6) 1.0026(3) 0.0274(15) Uani 1 1 d . . . H18 H 1.1589 0.5803 0.9935 0.033 Uiso 1 1 calc R . . C19 C 1.1300(5) 0.6875(6) 1.0629(3) 0.0259(15) Uani 1 1 d . . . C20 C 1.0677(5) 0.7675(6) 1.0852(3) 0.0260(15) Uani 1 1 d . . . C21 C 1.0802(5) 0.8002(6) 1.1466(3) 0.0257(15) Uani 1 1 d . . . C22 C 1.1509(5) 0.7535(6) 1.1830(3) 0.0263(15) Uani 1 1 d . . . H22 H 1.1577 0.7770 1.2234 0.032 Uiso 1 1 calc R . . C23 C 1.2123(5) 0.6729(6) 1.1619(3) 0.0298(16) Uani 1 1 d . A . C24 C 1.1994(5) 0.6412(6) 1.1008(3) 0.0294(16) Uani 1 1 d . . . H24 H 1.2384 0.5875 1.0849 0.035 Uiso 1 1 calc R . . C25 C 1.2849(6) 0.6155(7) 1.2054(4) 0.0374(18) Uani 1 1 d . . . C26A C 1.2531(13) 0.5067(14) 1.2151(9) 0.060(5) Uani 0.618(18) 1 d PU A 1 H26A H 1.2298 0.4762 1.1770 0.090 Uiso 0.618(18) 1 calc PR A 1 H26B H 1.2039 0.5075 1.2442 0.090 Uiso 0.618(18) 1 calc PR A 1 H26C H 1.3041 0.4621 1.2307 0.090 Uiso 0.618(18) 1 calc PR A 1 C27A C 1.3823(11) 0.6239(16) 1.1741(7) 0.058(5) Uani 0.618(18) 1 d PU A 1 H27A H 1.4253 0.5726 1.1931 0.087 Uiso 0.618(18) 1 calc PR A 1 H27B H 1.4063 0.6977 1.1786 0.087 Uiso 0.618(18) 1 calc PR A 1 H27C H 1.3748 0.6066 1.1313 0.087 Uiso 0.618(18) 1 calc PR A 1 C28A C 1.2939(13) 0.6757(13) 1.2669(7) 0.047(4) Uani 0.618(18) 1 d PU A 1 H28A H 1.2389 0.6623 1.2901 0.071 Uiso 0.618(18) 1 calc PR A 1 H28B H 1.3003 0.7537 1.2598 0.071 Uiso 0.618(18) 1 calc PR A 1 H28C H 1.3480 0.6489 1.2893 0.071 Uiso 0.618(18) 1 calc PR A 1 C26B C 1.3439(17) 0.533(2) 1.1759(11) 0.047(7) Uani 0.382(18) 1 d PU A 2 H26D H 1.3894 0.5055 1.2052 0.071 Uiso 0.382(18) 1 calc PR A 2 H26E H 1.3754 0.5673 1.1424 0.071 Uiso 0.382(18) 1 calc PR A 2 H26F H 1.3056 0.4736 1.1607 0.071 Uiso 0.382(18) 1 calc PR A 2 C27B C 1.339(2) 0.698(2) 1.2415(15) 0.055(7) Uani 0.382(18) 1 d PU A 2 H27D H 1.3089 0.7107 1.2798 0.083 Uiso 0.382(18) 1 calc PR A 2 H27E H 1.3412 0.7664 1.2190 0.083 Uiso 0.382(18) 1 calc PR A 2 H27F H 1.4013 0.6715 1.2493 0.083 Uiso 0.382(18) 1 calc PR A 2 C28B C 1.2263(18) 0.545(3) 1.2528(14) 0.056(7) Uani 0.382(18) 1 d PU A 2 H28D H 1.1809 0.5009 1.2308 0.085 Uiso 0.382(18) 1 calc PR A 2 H28E H 1.1948 0.5944 1.2799 0.085 Uiso 0.382(18) 1 calc PR A 2 H28F H 1.2679 0.4981 1.2761 0.085 Uiso 0.382(18) 1 calc PR A 2 C29 C 0.7424(6) 1.0037(7) 0.9099(4) 0.042(2) Uani 1 1 d . . . H29 H 0.7914 1.0425 0.8928 0.051 Uiso 1 1 calc R . . C30 C 0.6557(6) 1.0480(8) 0.9049(5) 0.055(2) Uani 1 1 d . . . H30 H 0.6456 1.1148 0.8846 0.066 Uiso 1 1 calc R . . C31 C 0.5822(7) 0.9914(9) 0.9307(5) 0.061(3) Uani 1 1 d . . . H31 H 0.5216 1.0195 0.9285 0.073 Uiso 1 1 calc R . . C32 C 0.6013(7) 0.8923(9) 0.9599(5) 0.059(3) Uani 1 1 d . . . H32 H 0.5538 0.8525 0.9781 0.071 Uiso 1 1 calc R . . C33 C 0.6920(6) 0.8531(8) 0.9617(4) 0.045(2) Uani 1 1 d . . . H33 H 0.7040 0.7853 0.9804 0.054 Uiso 1 1 calc R . . C34 C 0.8781(6) 0.2443(7) 0.3660(4) 0.041(2) Uani 1 1 d . . . H34 H 0.9146 0.1806 0.3665 0.049 Uiso 1 1 calc R . . C35 C 0.7865(6) 0.2347(7) 0.3839(4) 0.043(2) Uani 1 1 d . . . H35 H 0.7621 0.1668 0.3956 0.051 Uiso 1 1 calc R . . C36 C 0.7321(6) 0.3296(7) 0.3840(4) 0.0410(19) Uani 1 1 d . . . H36 H 0.6702 0.3274 0.3961 0.049 Uiso 1 1 calc R . . C37 C 0.7722(6) 0.4273(8) 0.3658(4) 0.044(2) Uani 1 1 d . . . H37 H 0.7380 0.4927 0.3655 0.053 Uiso 1 1 calc R . . C38 C 0.8634(7) 0.4266(8) 0.3481(4) 0.050(2) Uani 1 1 d . . . H38 H 0.8891 0.4930 0.3351 0.060 Uiso 1 1 calc R . . C39 C 0.9340(10) -0.0774(14) 0.5123(5) 0.084(4) Uani 1 1 d . . . C40 C 0.9101(10) 0.0320(14) 0.5081(5) 0.084(4) Uani 1 1 d . . . C41 C 0.9740(10) 0.1131(12) 0.4950(5) 0.073(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02736(15) 0.02032(14) 0.02675(15) 0.00071(11) -0.00111(9) 0.00079(11) Cl1 0.0272(9) 0.0276(9) 0.0349(9) 0.0001(7) -0.0013(7) -0.0022(7) Cl2 0.0302(9) 0.0290(9) 0.0499(11) 0.0011(8) -0.0025(8) -0.0040(8) O1 0.024(2) 0.020(2) 0.027(2) 0.0007(19) 0.0023(19) 0.001(2) O2 0.024(2) 0.016(2) 0.030(3) 0.0013(18) -0.0013(19) 0.0002(18) N1 0.027(3) 0.014(3) 0.032(3) 0.002(2) 0.002(2) 0.000(2) N2 0.031(3) 0.020(3) 0.025(3) 0.000(2) 0.002(2) 0.001(2) N3 0.031(4) 0.033(4) 0.041(4) -0.003(3) 0.000(3) 0.001(3) N4 0.040(4) 0.045(4) 0.049(4) 0.002(3) 0.003(3) 0.001(3) C1 0.025(4) 0.017(3) 0.026(3) -0.001(3) -0.006(3) 0.001(3) C2 0.025(3) 0.022(3) 0.023(3) 0.000(3) -0.004(3) 0.000(3) C3 0.025(3) 0.020(3) 0.026(3) 0.001(3) -0.004(3) 0.000(3) C4 0.021(3) 0.027(4) 0.031(4) -0.004(3) 0.001(3) -0.001(3) C5 0.025(4) 0.026(4) 0.024(3) -0.001(3) -0.001(3) -0.003(3) C6 0.026(3) 0.019(3) 0.032(4) 0.001(3) -0.002(3) -0.002(3) C7 0.036(4) 0.027(4) 0.032(4) 0.003(3) 0.006(3) 0.000(3) C8 0.043(5) 0.040(5) 0.036(4) 0.005(4) 0.004(4) 0.004(4) C9 0.046(5) 0.038(5) 0.042(5) 0.007(4) 0.019(4) 0.004(4) C10 0.039(5) 0.037(5) 0.044(5) 0.005(4) 0.006(4) -0.007(4) C11 0.020(3) 0.023(4) 0.030(4) -0.001(3) -0.001(3) 0.005(3) C12 0.025(3) 0.019(3) 0.032(4) -0.004(3) 0.002(3) 0.000(3) C13 0.026(4) 0.025(4) 0.029(4) -0.005(3) 0.003(3) -0.004(3) C14 0.026(4) 0.028(4) 0.033(4) 0.004(3) 0.002(3) -0.002(3) C15 0.034(4) 0.013(3) 0.038(4) -0.001(3) 0.007(3) -0.002(3) C16 0.038(4) 0.025(4) 0.037(4) -0.007(3) 0.000(3) -0.004(3) C17 0.040(4) 0.025(4) 0.027(4) 0.003(3) -0.003(3) -0.004(3) C18 0.023(3) 0.026(4) 0.033(4) -0.002(3) 0.003(3) 0.003(3) C19 0.028(4) 0.022(3) 0.028(4) 0.003(3) -0.002(3) 0.002(3) C20 0.023(4) 0.024(3) 0.030(4) 0.002(3) -0.003(3) -0.006(3) C21 0.024(4) 0.024(3) 0.030(4) -0.001(3) 0.002(3) -0.001(3) C22 0.029(4) 0.021(4) 0.029(4) 0.001(3) 0.002(3) 0.001(3) C23 0.027(4) 0.030(4) 0.033(4) 0.001(3) -0.002(3) 0.002(3) C24 0.027(4) 0.025(4) 0.037(4) -0.002(3) 0.005(3) 0.004(3) C25 0.037(4) 0.037(4) 0.037(4) -0.002(3) -0.012(3) 0.014(3) C26A 0.063(8) 0.054(8) 0.062(8) 0.006(6) -0.024(7) -0.001(6) C27A 0.049(7) 0.076(9) 0.049(7) 0.007(6) -0.002(6) 0.011(7) C28A 0.052(7) 0.044(7) 0.044(7) -0.002(6) -0.022(6) 0.028(6) C26B 0.048(10) 0.048(10) 0.045(9) -0.001(8) -0.011(7) 0.013(8) C27B 0.055(11) 0.048(10) 0.062(11) 0.000(8) -0.019(8) 0.011(8) C28B 0.049(10) 0.064(11) 0.056(10) 0.015(8) 0.000(8) 0.007(8) C29 0.035(4) 0.035(5) 0.056(5) 0.003(4) 0.001(4) 0.007(3) C30 0.039(5) 0.045(5) 0.080(7) 0.011(5) -0.005(5) 0.006(4) C31 0.036(5) 0.064(7) 0.083(8) 0.002(6) 0.001(5) 0.012(5) C32 0.032(5) 0.061(6) 0.085(8) 0.007(6) 0.004(5) 0.004(4) C33 0.037(4) 0.050(5) 0.048(5) 0.004(4) 0.006(4) 0.000(4) C34 0.038(5) 0.042(5) 0.043(5) -0.004(4) 0.000(4) 0.007(4) C35 0.047(5) 0.035(4) 0.047(5) -0.007(4) 0.006(4) -0.004(4) C36 0.035(4) 0.049(5) 0.039(4) -0.007(4) 0.001(3) 0.004(4) C37 0.047(5) 0.049(5) 0.036(4) 0.001(4) -0.002(4) 0.017(4) C38 0.056(6) 0.048(5) 0.048(5) 0.009(4) 0.013(4) 0.003(4) C39 0.087(9) 0.125(12) 0.041(6) -0.008(7) 0.003(6) 0.026(9) C40 0.086(9) 0.118(12) 0.048(6) -0.014(7) -0.011(6) 0.030(9) C41 0.078(9) 0.100(10) 0.041(6) -0.001(6) -0.009(5) 0.023(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O2 2.173(5) . ? U O1 2.183(5) . ? U N1 2.602(6) . ? U N2 2.625(6) . ? U Cl2 2.7011(19) . ? U Cl1 2.7351(17) . ? U N3 2.789(6) . ? U Cl1 2.9683(18) 3_777 ? U U 4.4335(5) 3_777 ? Cl1 U 2.9683(18) 3_777 ? O1 C2 1.333(8) . ? O1 N1 2.670(7) . ? O1 O2 3.250(6) 3_777 ? O1 O2 4.187(6) . ? O2 C20 1.363(8) . ? O2 N2 2.725(7) . ? N1 C11 1.284(9) . ? N1 C12 1.436(9) . ? N1 N2 2.630(8) . ? N2 C18 1.306(9) . ? N2 C13 1.444(9) . ? N3 C33 1.322(11) . ? N3 C29 1.343(10) . ? N4 C34 1.317(11) . ? N4 C38 1.338(12) . ? C1 C6 1.380(10) . ? C1 C2 1.414(9) . ? C1 C21 1.492(10) 3_777 ? C2 C3 1.407(9) . ? C3 C4 1.406(10) . ? C3 C11 1.438(9) . ? C4 C5 1.361(10) . ? C4 H4 0.9300 . ? C5 C6 1.406(10) . ? C5 C7 1.551(10) . ? C6 H6 0.9300 . ? C7 C9 1.524(10) . ? C7 C10 1.527(11) . ? C7 C8 1.545(11) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11 0.9300 . ? C12 C13 1.385(10) . ? C12 C17 1.395(10) . ? C13 C14 1.391(10) . ? C14 C15 1.391(10) . ? C14 H14 0.9300 . ? C15 C16 1.391(11) . ? C15 H15 0.9300 . ? C16 C17 1.396(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.443(10) . ? C18 H18 0.9300 . ? C19 C24 1.391(10) . ? C19 C20 1.410(10) . ? C20 C21 1.403(10) . ? C21 C22 1.387(10) . ? C21 C1 1.492(10) 3_777 ? C22 C23 1.398(10) . ? C22 H22 0.9300 . ? C23 C24 1.395(10) . ? C23 C25 1.548(10) . ? C24 H24 0.9300 . ? C25 C26A 1.410(19) . ? C25 C26B 1.46(2) . ? C25 C27B 1.48(3) . ? C25 C28A 1.528(16) . ? C25 C27A 1.571(18) . ? C25 C28B 1.59(3) . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29 C30 1.351(12) . ? C29 H29 0.9300 . ? C30 C31 1.386(14) . ? C30 H30 0.9300 . ? C31 C32 1.382(14) . ? C31 H31 0.9300 . ? C32 C33 1.378(12) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.381(12) . ? C34 H34 0.9300 . ? C35 C36 1.386(12) . ? C35 H35 0.9300 . ? C36 C37 1.377(12) . ? C36 H36 0.9300 . ? C37 C38 1.368(13) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.37(2) . ? C39 C41 1.397(17) 3_756 ? C40 C41 1.38(2) . ? C41 C39 1.397(17) 3_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U O1 147.91(17) . . ? O2 U N1 127.33(17) . . ? O1 U N1 67.19(17) . . ? O2 U N2 68.44(17) . . ? O1 U N2 124.80(17) . . ? N1 U N2 60.41(17) . . ? O2 U Cl2 91.90(13) . . ? O1 U Cl2 119.55(13) . . ? N1 U Cl2 83.72(13) . . ? N2 U Cl2 71.50(13) . . ? O2 U Cl1 77.30(13) . . ? O1 U Cl1 75.59(13) . . ? N1 U Cl1 85.73(13) . . ? N2 U Cl1 84.25(13) . . ? Cl2 U Cl1 155.70(6) . . ? O2 U N3 116.78(18) . . ? O1 U N3 72.19(18) . . ? N1 U N3 111.21(18) . . ? N2 U N3 142.50(19) . . ? Cl2 U N3 71.23(14) . . ? Cl1 U N3 133.07(14) . . ? O2 U Cl1 76.47(12) . 3_777 ? O1 U Cl1 81.39(12) . 3_777 ? N1 U Cl1 147.42(13) . 3_777 ? N2 U Cl1 143.38(13) . 3_777 ? Cl2 U Cl1 120.97(5) . 3_777 ? Cl1 U Cl1 78.04(5) . 3_777 ? N3 U Cl1 64.26(14) . 3_777 ? U Cl1 U 101.96(5) . 3_777 ? C2 O1 U 142.9(4) . . ? C2 O1 N1 87.4(4) . . ? U O1 N1 63.91(17) . . ? C20 O2 U 143.6(4) . . ? C11 N1 C12 115.8(6) . . ? C11 N1 U 129.1(5) . . ? C12 N1 U 114.8(4) . . ? C18 N2 C13 115.3(6) . . ? C18 N2 U 129.7(5) . . ? C13 N2 U 115.0(4) . . ? C33 N3 C29 116.8(7) . . ? C33 N3 U 123.1(6) . . ? C29 N3 U 119.7(5) . . ? C34 N4 C38 115.7(8) . . ? C6 C1 C2 119.6(6) . . ? C6 C1 C21 117.7(6) . 3_777 ? C2 C1 C21 122.4(6) . 3_777 ? O1 C2 C3 121.5(6) . . ? O1 C2 C1 121.2(6) . . ? C3 C2 C1 117.2(6) . . ? C4 C3 C2 121.0(6) . . ? C4 C3 C11 119.0(6) . . ? C2 C3 C11 119.8(6) . . ? C5 C4 C3 122.2(7) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 116.5(6) . . ? C4 C5 C7 124.9(6) . . ? C6 C5 C7 118.6(6) . . ? C1 C6 C5 123.5(6) . . ? C1 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? C9 C7 C10 108.7(7) . . ? C9 C7 C8 109.0(6) . . ? C10 C7 C8 109.6(6) . . ? C9 C7 C5 111.7(6) . . ? C10 C7 C5 109.3(6) . . ? C8 C7 C5 108.6(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C3 127.4(6) . . ? N1 C11 H11 116.3 . . ? C3 C11 H11 116.3 . . ? C13 C12 C17 120.3(7) . . ? C13 C12 N1 116.6(6) . . ? C17 C12 N1 123.1(6) . . ? C12 C13 C14 120.9(7) . . ? C12 C13 N2 114.6(6) . . ? C14 C13 N2 124.5(7) . . ? C15 C14 C13 118.6(7) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 121.0(7) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 119.9(7) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C12 C17 C16 119.2(7) . . ? C12 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N2 C18 C19 125.3(6) . . ? N2 C18 H18 117.4 . . ? C19 C18 H18 117.4 . . ? C24 C19 C20 121.1(6) . . ? C24 C19 C18 115.6(6) . . ? C20 C19 C18 122.9(6) . . ? O2 C20 C21 121.7(6) . . ? O2 C20 C19 120.8(6) . . ? C21 C20 C19 117.3(6) . . ? C22 C21 C20 120.2(6) . . ? C22 C21 C1 116.9(6) . 3_777 ? C20 C21 C1 122.6(6) . 3_777 ? C21 C22 C23 123.3(7) . . ? C21 C22 H22 118.3 . . ? C23 C22 H22 118.3 . . ? C24 C23 C22 116.0(6) . . ? C24 C23 C25 122.0(7) . . ? C22 C23 C25 121.8(7) . . ? C19 C24 C23 122.1(7) . . ? C19 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C26B C25 C27B 113.3(17) . . ? C26A C25 C28A 109.4(12) . . ? C26A C25 C23 107.3(9) . . ? C26B C25 C23 114.8(10) . . ? C27B C25 C23 110.7(12) . . ? C28A C25 C23 111.2(7) . . ? C26A C25 C27A 114.7(12) . . ? C28A C25 C27A 107.3(11) . . ? C23 C25 C27A 106.9(8) . . ? C26B C25 C28B 104.0(16) . . ? C27B C25 C28B 106.9(18) . . ? C23 C25 C28B 106.4(11) . . ? N3 C29 C30 124.6(9) . . ? N3 C29 H29 117.7 . . ? C30 C29 H29 117.7 . . ? C29 C30 C31 118.3(9) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C32 C31 C30 118.3(9) . . ? C32 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C33 C32 C31 118.9(10) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? N3 C33 C32 123.1(9) . . ? N3 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? N4 C34 C35 125.2(8) . . ? N4 C34 H34 117.4 . . ? C35 C34 H34 117.4 . . ? C34 C35 C36 117.8(8) . . ? C34 C35 H35 121.1 . . ? C36 C35 H35 121.1 . . ? C37 C36 C35 118.1(8) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C38 C37 C36 118.9(8) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? N4 C38 C37 124.3(9) . . ? N4 C38 H38 117.8 . . ? C37 C38 H38 117.8 . . ? C40 C39 C41 121.7(15) . 3_756 ? C39 C40 C41 122.5(13) . . ? C40 C41 C39 115.8(13) . 3_756 ? #===END data_3.5thf _database_code_depnum_ccdc_archive 'CCDC 609881' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H124 N4 O17 U2' _chemical_formula_weight 2082.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 16.2734(4) _cell_length_b 29.7951(10) _cell_length_c 20.3134(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.161(2) _cell_angle_gamma 90.00 _cell_volume 9185.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 171065 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method ? _exptl_crystal_F_000 4192 _exptl_absorpt_coefficient_mu 3.589 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 171065 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.68 _reflns_number_total 16467 _reflns_number_gt 12106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. Some restraints on bond lengths and/or displacement parameters were applied for some badly behaving atoms, particularly in the solvent molecules. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+22.3297P] 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 16467 _refine_ls_number_parameters 1092 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.297 _refine_diff_density_min -1.699 _refine_diff_density_rms 0.131 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 0.895513(16) 0.492792(9) 0.824951(13) 0.02286(7) Uani 1 1 d . . . U2 U 0.867304(16) 0.529255(9) 0.627161(13) 0.02447(8) Uani 1 1 d . . . O1 O 0.7907(3) 0.50333(15) 0.7147(2) 0.0266(11) Uani 1 1 d . . . O2 O 0.9669(3) 0.52100(15) 0.7549(2) 0.0228(10) Uani 1 1 d . . . O3 O 0.9484(3) 0.59064(15) 0.6598(2) 0.0272(11) Uani 1 1 d . . . O4 O 0.7538(3) 0.57125(16) 0.6180(2) 0.0279(11) Uani 1 1 d . . . O5 O 0.8691(3) 0.56906(15) 0.8364(2) 0.0267(11) Uani 1 1 d . . . O6 O 0.7706(3) 0.49793(16) 0.8536(2) 0.0295(11) Uani 1 1 d . . . O7 O 0.9292(3) 0.44511(15) 0.9229(2) 0.0254(10) Uani 1 1 d . . . O8 O 1.0285(3) 0.51466(16) 0.9075(2) 0.0268(11) Uani 1 1 d . . . O9 O 0.9901(3) 0.51577(17) 0.5954(2) 0.0304(11) Uani 1 1 d . . . O10 O 0.8431(3) 0.56332(16) 0.5171(2) 0.0286(11) Uani 1 1 d . . . O11 O 0.7580(3) 0.48197(16) 0.5543(2) 0.0300(11) Uani 1 1 d . . . O12 O 0.9135(3) 0.45155(16) 0.6472(2) 0.0298(11) Uani 1 1 d . . . N1 N 0.8325(3) 0.41603(19) 0.7729(3) 0.0241(12) Uani 1 1 d . . . N2 N 1.0021(3) 0.43294(18) 0.8092(3) 0.0230(12) Uani 1 1 d . . . N3 N 0.8758(4) 0.71799(19) 0.6061(3) 0.0277(13) Uani 1 1 d . . . N4 N 0.6902(4) 0.6993(2) 0.5480(3) 0.0300(14) Uani 1 1 d . . . C1 C 0.6337(4) 0.5179(2) 0.6668(3) 0.0233(15) Uani 1 1 d . . . C2 C 0.7064(4) 0.4882(2) 0.6913(3) 0.0243(15) Uani 1 1 d . . . C3 C 0.6894(4) 0.4418(2) 0.6931(3) 0.0243(15) Uani 1 1 d . . . C4 C 0.6039(4) 0.4249(2) 0.6682(3) 0.0286(16) Uani 1 1 d . . . H4 H 0.5953 0.3941 0.6689 0.034 Uiso 1 1 calc R . . C5 C 0.5306(4) 0.4531(2) 0.6422(3) 0.0275(16) Uani 1 1 d . . . C6 C 0.5484(5) 0.4990(2) 0.6421(3) 0.0285(16) Uani 1 1 d . . . H6 H 0.5008 0.5184 0.6246 0.034 Uiso 1 1 calc R . . C7 C 0.4367(4) 0.4355(3) 0.6135(4) 0.0350(18) Uani 1 1 d . . . C8 C 0.4312(6) 0.3868(3) 0.6362(6) 0.074(3) Uani 1 1 d U . . H8A H 0.4690 0.3682 0.6208 0.111 Uiso 1 1 calc R . . H8B H 0.3715 0.3763 0.6153 0.111 Uiso 1 1 calc R . . H8C H 0.4496 0.3853 0.6867 0.111 Uiso 1 1 calc R . . C9 C 0.3748(5) 0.4638(3) 0.6369(5) 0.055(2) Uani 1 1 d . . . H9A H 0.3921 0.4621 0.6873 0.082 Uiso 1 1 calc R . . H9B H 0.3158 0.4527 0.6151 0.082 Uiso 1 1 calc R . . H9C H 0.3774 0.4944 0.6232 0.082 Uiso 1 1 calc R . . C10 C 0.4048(6) 0.4358(4) 0.5332(5) 0.065(3) Uani 1 1 d U . . H10A H 0.4067 0.4658 0.5168 0.098 Uiso 1 1 calc R . . H10B H 0.3453 0.4248 0.5142 0.098 Uiso 1 1 calc R . . H10C H 0.4421 0.4168 0.5179 0.098 Uiso 1 1 calc R . . C11 C 0.7577(4) 0.4087(2) 0.7247(3) 0.0276(15) Uani 1 1 d . . . H11 H 0.7459 0.3794 0.7081 0.033 Uiso 1 1 calc R . . C12 C 0.8899(5) 0.3785(2) 0.8008(3) 0.0276(16) Uani 1 1 d . . . C13 C 0.9797(4) 0.3878(2) 0.8198(3) 0.0249(15) Uani 1 1 d . . . C14 C 1.0410(5) 0.3544(2) 0.8484(3) 0.0294(16) Uani 1 1 d . . . H14 H 1.1009 0.3607 0.8625 0.035 Uiso 1 1 calc R . . C15 C 1.0131(5) 0.3114(2) 0.8559(4) 0.0322(17) Uani 1 1 d . . . H15 H 1.0541 0.2886 0.8734 0.039 Uiso 1 1 calc R . . C16 C 0.9233(5) 0.3025(3) 0.8371(4) 0.0356(18) Uani 1 1 d . . . H16 H 0.9049 0.2738 0.8432 0.043 Uiso 1 1 calc R . . C17 C 0.8620(4) 0.3358(2) 0.8096(4) 0.0294(16) Uani 1 1 d . . . H17 H 0.8023 0.3296 0.7969 0.035 Uiso 1 1 calc R . . C18 C 1.0703(4) 0.4393(2) 0.7924(3) 0.0246(15) Uani 1 1 d . . . H18 H 1.0985 0.4142 0.7832 0.030 Uiso 1 1 calc R . . C19 C 1.1058(4) 0.4834(2) 0.7868(3) 0.0252(15) Uani 1 1 d . . . C20 C 1.0550(4) 0.5230(2) 0.7732(3) 0.0246(15) Uani 1 1 d . . . C21 C 1.1003(4) 0.5638(2) 0.7806(3) 0.0264(15) Uani 1 1 d . . . C22 C 1.1916(4) 0.5638(2) 0.8004(3) 0.0273(15) Uani 1 1 d . . . H22 H 1.2202 0.5914 0.8066 0.033 Uiso 1 1 calc R . . C23 C 1.2428(4) 0.5248(2) 0.8115(4) 0.0276(15) Uani 1 1 d . . . C24 C 1.1970(4) 0.4850(2) 0.8037(4) 0.0283(16) Uani 1 1 d . . . H24 H 1.2281 0.4582 0.8100 0.034 Uiso 1 1 calc R . . C25 C 1.3426(5) 0.5275(3) 0.8341(4) 0.0361(18) Uani 1 1 d . . . C26 C 1.3664(5) 0.5536(3) 0.7783(5) 0.056(2) Uani 1 1 d . . . H26A H 1.3441 0.5379 0.7341 0.084 Uiso 1 1 calc R . . H26B H 1.4293 0.5561 0.7932 0.084 Uiso 1 1 calc R . . H26C H 1.3407 0.5830 0.7728 0.084 Uiso 1 1 calc R . . C27 C 1.3842(5) 0.4808(3) 0.8417(5) 0.049(2) Uani 1 1 d . . . H27A H 1.3727 0.4646 0.8783 0.074 Uiso 1 1 calc R . . H27B H 1.4466 0.4837 0.8537 0.074 Uiso 1 1 calc R . . H27C H 1.3592 0.4649 0.7979 0.074 Uiso 1 1 calc R . . C28 C 1.3801(5) 0.5519(4) 0.9048(5) 0.068(3) Uani 1 1 d . . . H28A H 1.3538 0.5811 0.9006 0.102 Uiso 1 1 calc R . . H28B H 1.4427 0.5549 0.9182 0.102 Uiso 1 1 calc R . . H28C H 1.3672 0.5350 0.9402 0.102 Uiso 1 1 calc R . . C29 C 1.0560(4) 0.6088(2) 0.7720(3) 0.0255(15) Uani 1 1 d . . . C30 C 0.9866(4) 0.6208(2) 0.7090(3) 0.0255(15) Uani 1 1 d . . . C31 C 0.9638(4) 0.6667(2) 0.6972(3) 0.0245(15) Uani 1 1 d . . . C32 C 1.0000(4) 0.6984(2) 0.7507(3) 0.0267(15) Uani 1 1 d . . . H32 H 0.9818 0.7281 0.7428 0.032 Uiso 1 1 calc R . . C33 C 1.0637(4) 0.6860(2) 0.8164(4) 0.0297(16) Uani 1 1 d . . . C34 C 1.0907(4) 0.6418(2) 0.8241(3) 0.0251(15) Uani 1 1 d . . . H34 H 1.1346 0.6334 0.8662 0.030 Uiso 1 1 calc R . . C35 C 1.1035(5) 0.7218(2) 0.8741(3) 0.0302(16) Uani 1 1 d . . . C36 C 1.0306(5) 0.7395(3) 0.8987(4) 0.0405(19) Uani 1 1 d . . . H36A H 0.9857 0.7538 0.8598 0.061 Uiso 1 1 calc R . . H36B H 1.0552 0.7608 0.9361 0.061 Uiso 1 1 calc R . . H36C H 1.0053 0.7149 0.9153 0.061 Uiso 1 1 calc R . . C37 C 1.1418(5) 0.7605(3) 0.8437(4) 0.0392(19) Uani 1 1 d . . . H37A H 1.1859 0.7489 0.8271 0.059 Uiso 1 1 calc R . . H37B H 1.1680 0.7824 0.8798 0.059 Uiso 1 1 calc R . . H37C H 1.0955 0.7743 0.8052 0.059 Uiso 1 1 calc R . . C38 C 1.1789(5) 0.7019(3) 0.9379(4) 0.0378(19) Uani 1 1 d . . . H38A H 1.1558 0.6788 0.9593 0.057 Uiso 1 1 calc R . . H38B H 1.2045 0.7252 0.9719 0.057 Uiso 1 1 calc R . . H38C H 1.2231 0.6895 0.9223 0.057 Uiso 1 1 calc R . . C39 C 0.9087(4) 0.6790(2) 0.6245(3) 0.0284(16) Uani 1 1 d . . . H39 H 0.8970 0.6570 0.5899 0.034 Uiso 1 1 calc R . . C40 C 0.8254(4) 0.7244(2) 0.5325(3) 0.0266(15) Uani 1 1 d . . . C41 C 0.7349(5) 0.7157(2) 0.5053(3) 0.0291(16) Uani 1 1 d . . . C42 C 0.6870(5) 0.7262(2) 0.4341(4) 0.0317(17) Uani 1 1 d . . . H42 H 0.6266 0.7210 0.4156 0.038 Uiso 1 1 calc R . . C43 C 0.7286(5) 0.7440(3) 0.3911(4) 0.0352(18) Uani 1 1 d . . . H43 H 0.6960 0.7504 0.3441 0.042 Uiso 1 1 calc R . . C44 C 0.8190(5) 0.7523(3) 0.4181(4) 0.0379(18) Uani 1 1 d . . . H44 H 0.8473 0.7639 0.3895 0.045 Uiso 1 1 calc R . . C45 C 0.8660(5) 0.7427(2) 0.4889(4) 0.0332(17) Uani 1 1 d . . . H45 H 0.9261 0.7487 0.5075 0.040 Uiso 1 1 calc R . . C46 C 0.7108(4) 0.6592(2) 0.5719(3) 0.0276(16) Uani 1 1 d . . . H46 H 0.7526 0.6436 0.5596 0.033 Uiso 1 1 calc R . . C47 C 0.6711(4) 0.6372(2) 0.6177(3) 0.0264(15) Uani 1 1 d . . . C48 C 0.6904(4) 0.5916(2) 0.6338(3) 0.0257(15) Uani 1 1 d . . . C49 C 0.6373(4) 0.5676(2) 0.6645(3) 0.0266(15) Uani 1 1 d . . . C50 C 0.5780(4) 0.5926(2) 0.6861(3) 0.0260(15) Uani 1 1 d . . . H50 H 0.5449 0.5773 0.7079 0.031 Uiso 1 1 calc R . . C51 C 0.5656(4) 0.6390(2) 0.6766(4) 0.0293(16) Uani 1 1 d . . . C52 C 0.6103(4) 0.6604(2) 0.6391(3) 0.0271(15) Uani 1 1 d . . . H52 H 0.5998 0.6906 0.6279 0.032 Uiso 1 1 calc R . . C53 C 0.5000(5) 0.6630(3) 0.7031(4) 0.0340(17) Uani 1 1 d . . . C54 C 0.4979(6) 0.7135(3) 0.6901(5) 0.059(3) Uani 1 1 d . . . H54A H 0.5565 0.7254 0.7100 0.088 Uiso 1 1 calc R . . H54B H 0.4612 0.7277 0.7119 0.088 Uiso 1 1 calc R . . H54C H 0.4745 0.7192 0.6402 0.088 Uiso 1 1 calc R . . C55 C 0.4079(5) 0.6442(3) 0.6657(4) 0.048(2) Uani 1 1 d . . . H55A H 0.3881 0.6519 0.6165 0.072 Uiso 1 1 calc R . . H55B H 0.3684 0.6567 0.6862 0.072 Uiso 1 1 calc R . . H55C H 0.4092 0.6121 0.6707 0.072 Uiso 1 1 calc R . . C56 C 0.5263(5) 0.6561(3) 0.7828(4) 0.044(2) Uani 1 1 d . . . H56A H 0.5236 0.6247 0.7926 0.067 Uiso 1 1 calc R . . H56B H 0.4866 0.6724 0.7992 0.067 Uiso 1 1 calc R . . H56C H 0.5853 0.6669 0.8065 0.067 Uiso 1 1 calc R . . C57 C 0.8064(6) 0.6411(3) 0.8185(4) 0.049(2) Uani 1 1 d . . . H57A H 0.8664 0.6496 0.8279 0.073 Uiso 1 1 calc R . . H57B H 0.7831 0.6587 0.8474 0.073 Uiso 1 1 calc R . . H57C H 0.7721 0.6463 0.7696 0.073 Uiso 1 1 calc R . . C58 C 0.8026(5) 0.5922(2) 0.8352(3) 0.0331(17) Uani 1 1 d . . . C59 C 0.7296(5) 0.5745(3) 0.8472(4) 0.0347(18) Uani 1 1 d . . . H59 H 0.6879 0.5945 0.8513 0.042 Uiso 1 1 calc R . . C60 C 0.7157(4) 0.5297(3) 0.8533(3) 0.0342(18) Uani 1 1 d . . . C61 C 0.6296(5) 0.5130(3) 0.8561(5) 0.047(2) Uani 1 1 d . . . H61A H 0.5938 0.5013 0.8108 0.070 Uiso 1 1 calc R . . H61B H 0.5992 0.5373 0.8685 0.070 Uiso 1 1 calc R . . H61C H 0.6409 0.4897 0.8909 0.070 Uiso 1 1 calc R . . C62 C 0.9963(5) 0.3892(3) 1.0083(4) 0.0365(18) Uani 1 1 d . . . H62A H 0.9740 0.3965 1.0448 0.055 Uiso 1 1 calc R . . H62B H 1.0539 0.3762 1.0291 0.055 Uiso 1 1 calc R . . H62C H 0.9575 0.3681 0.9762 0.055 Uiso 1 1 calc R . . C63 C 1.0019(5) 0.4312(2) 0.9690(3) 0.0296(16) Uani 1 1 d . . . C64 C 1.0821(5) 0.4528(2) 0.9832(4) 0.0302(16) Uani 1 1 d . . . H64 H 1.1324 0.4390 1.0143 0.036 Uiso 1 1 calc R . . C65 C 1.0924(4) 0.4932(2) 0.9542(3) 0.0261(15) Uani 1 1 d . . . C66 C 1.1813(4) 0.5168(3) 0.9765(4) 0.0328(18) Uani 1 1 d . . . H66A H 1.1855 0.5332 0.9372 0.049 Uiso 1 1 calc R . . H66B H 1.2276 0.4948 0.9917 0.049 Uiso 1 1 calc R . . H66C H 1.1869 0.5371 1.0146 0.049 Uiso 1 1 calc R . . C67 C 1.1255(5) 0.5315(3) 0.5813(4) 0.0392(19) Uani 1 1 d . . . H67A H 1.1562 0.5354 0.6311 0.059 Uiso 1 1 calc R . . H67B H 1.1481 0.5524 0.5560 0.059 Uiso 1 1 calc R . . H67C H 1.1340 0.5014 0.5682 0.059 Uiso 1 1 calc R . . C68 C 1.0290(4) 0.5400(2) 0.5637(3) 0.0288(16) Uani 1 1 d . . . C69 C 0.9859(5) 0.5728(2) 0.5129(4) 0.0316(17) Uani 1 1 d . . . H69 H 1.0192 0.5895 0.4929 0.038 Uiso 1 1 calc R . . C70 C 0.8960(5) 0.5814(2) 0.4911(3) 0.0279(16) Uani 1 1 d . . . C71 C 0.8542(5) 0.6140(3) 0.4314(4) 0.042(2) Uani 1 1 d . . . H71A H 0.8276 0.5978 0.3881 0.063 Uiso 1 1 calc R . . H71B H 0.8985 0.6339 0.4272 0.063 Uiso 1 1 calc R . . H71C H 0.8099 0.6312 0.4410 0.063 Uiso 1 1 calc R . . C72 C 0.6460(5) 0.4293(3) 0.4983(4) 0.054(2) Uani 1 1 d . . . H72A H 0.6063 0.4447 0.5158 0.081 Uiso 1 1 calc R . . H72B H 0.6368 0.3975 0.4994 0.081 Uiso 1 1 calc R . . H72C H 0.6352 0.4386 0.4507 0.081 Uiso 1 1 calc R . . C73 C 0.7397(5) 0.4404(3) 0.5440(4) 0.0351(18) Uani 1 1 d . . . C74 C 0.8007(5) 0.4061(2) 0.5712(4) 0.0364(18) Uani 1 1 d . . . H74 H 0.7838 0.3768 0.5568 0.044 Uiso 1 1 calc R . . C75 C 0.8864(5) 0.4136(2) 0.6193(4) 0.0299(16) Uani 1 1 d . . . C76 C 0.9500(5) 0.3752(2) 0.6418(4) 0.0380(19) Uani 1 1 d . . . H76A H 1.0091 0.3863 0.6542 0.057 Uiso 1 1 calc R . . H76B H 0.9378 0.3542 0.6036 0.057 Uiso 1 1 calc R . . H76C H 0.9439 0.3605 0.6818 0.057 Uiso 1 1 calc R . . O13 O 0.7120(7) 0.6084(4) 0.0295(6) 0.136(4) Uani 1 1 d U . . C77 C 0.7194(6) 0.6584(3) 0.0205(5) 0.064(3) Uani 1 1 d . . . H77A H 0.7480 0.6647 -0.0129 0.077 Uiso 1 1 calc R . . H77B H 0.7528 0.6725 0.0653 0.077 Uiso 1 1 calc R . . C78 C 0.6251(6) 0.6751(4) -0.0071(6) 0.075(3) Uani 1 1 d DU . . H78A H 0.6192 0.7012 0.0194 0.091 Uiso 1 1 calc R . . H78B H 0.6074 0.6833 -0.0564 0.091 Uiso 1 1 calc R . . C79 C 0.5696(7) 0.6378(4) 0.0017(7) 0.090(4) Uani 1 1 d DU . . H79A H 0.5606 0.6403 0.0463 0.108 Uiso 1 1 calc R . . H79B H 0.5128 0.6374 -0.0365 0.108 Uiso 1 1 calc R . . C80 C 0.6209(7) 0.5978(4) 0.0003(6) 0.080(3) Uani 1 1 d DU . . H80A H 0.6076 0.5739 0.0274 0.097 Uiso 1 1 calc R . . H80B H 0.6057 0.5874 -0.0479 0.097 Uiso 1 1 calc R . . O14 O 0.7654(3) 0.28152(19) 0.3239(3) 0.0447(14) Uani 1 1 d . . . C81 C 0.7995(6) 0.2828(3) 0.4000(4) 0.055(2) Uani 1 1 d . . . H81A H 0.8262 0.2543 0.4192 0.066 Uiso 1 1 calc R . . H81B H 0.7526 0.2891 0.4176 0.066 Uiso 1 1 calc R . . C82 C 0.8677(6) 0.3200(3) 0.4205(5) 0.060(3) Uani 1 1 d . . . H82A H 0.8700 0.3346 0.4638 0.072 Uiso 1 1 calc R . . H82B H 0.9258 0.3085 0.4265 0.072 Uiso 1 1 calc R . . C83 C 0.8350(6) 0.3516(3) 0.3588(4) 0.051(2) Uani 1 1 d . . . H83A H 0.7901 0.3717 0.3628 0.061 Uiso 1 1 calc R . . H83B H 0.8828 0.3692 0.3540 0.061 Uiso 1 1 calc R . . C84 C 0.7977(6) 0.3195(3) 0.2985(4) 0.043(2) Uani 1 1 d . . . H84A H 0.7504 0.3337 0.2604 0.051 Uiso 1 1 calc R . . H84B H 0.8431 0.3104 0.2807 0.051 Uiso 1 1 calc R . . O15 O 0.2036(4) 0.1466(2) 0.2770(4) 0.0611(17) Uani 1 1 d . . . C85 C 0.1707(6) 0.1897(3) 0.2489(5) 0.064(3) Uani 1 1 d . . . H85A H 0.1182 0.1972 0.2587 0.077 Uiso 1 1 calc R . . H85B H 0.1567 0.1905 0.1983 0.077 Uiso 1 1 calc R . . C86 C 0.2456(7) 0.2218(3) 0.2867(5) 0.066(3) Uani 1 1 d . . . H86A H 0.2422 0.2321 0.3309 0.080 Uiso 1 1 calc R . . H86B H 0.2451 0.2476 0.2574 0.080 Uiso 1 1 calc R . . C87 C 0.3273(7) 0.1930(4) 0.2992(6) 0.072(3) Uani 1 1 d U . . H87A H 0.3585 0.2025 0.2689 0.086 Uiso 1 1 calc R . . H87B H 0.3670 0.1949 0.3480 0.086 Uiso 1 1 calc R . . C88 C 0.2924(7) 0.1460(4) 0.2813(6) 0.069(3) Uani 1 1 d U . . H88A H 0.2957 0.1367 0.2366 0.083 Uiso 1 1 calc R . . H88B H 0.3266 0.1252 0.3176 0.083 Uiso 1 1 calc R . . O16 O 0.6357(6) 0.3126(3) 0.6295(5) 0.108(3) Uani 1 1 d U . . C89 C 0.6021(10) 0.3081(5) 0.5579(7) 0.110(5) Uani 1 1 d U . . H89A H 0.6485 0.3123 0.5391 0.133 Uiso 1 1 calc R . . H89B H 0.5575 0.3308 0.5375 0.133 Uiso 1 1 calc R . . C90 C 0.5632(7) 0.2636(4) 0.5387(5) 0.074(3) Uani 1 1 d U . . H90A H 0.5858 0.2488 0.5061 0.089 Uiso 1 1 calc R . . H90B H 0.4995 0.2654 0.5173 0.089 Uiso 1 1 calc R . . C91 C 0.5915(7) 0.2389(3) 0.6089(5) 0.063(3) Uani 1 1 d U . . H91A H 0.5449 0.2194 0.6113 0.076 Uiso 1 1 calc R . . H91B H 0.6440 0.2211 0.6162 0.076 Uiso 1 1 calc R . . C92 C 0.6094(7) 0.2758(4) 0.6617(6) 0.081(4) Uani 1 1 d . . . H92A H 0.5569 0.2832 0.6715 0.097 Uiso 1 1 calc R . . H92B H 0.6560 0.2674 0.7055 0.097 Uiso 1 1 calc R . . O17 O 0.3430(6) 0.6430(4) 0.1827(5) 0.115(3) Uani 1 1 d U . . C93 C 0.3026(10) 0.6153(6) 0.1200(8) 0.123(5) Uani 1 1 d U . . H93A H 0.2439 0.6267 0.0941 0.148 Uiso 1 1 calc R . . H93B H 0.2964 0.5850 0.1349 0.148 Uiso 1 1 calc R . . C94 C 0.3532(11) 0.6139(6) 0.0714(8) 0.131(6) Uani 1 1 d U . . H94A H 0.3153 0.6157 0.0221 0.157 Uiso 1 1 calc R . . H94B H 0.3911 0.5877 0.0792 0.157 Uiso 1 1 calc R . . C95 C 0.4049(12) 0.6570(7) 0.0980(9) 0.163(7) Uani 1 1 d DU . . H95A H 0.4675 0.6513 0.1113 0.196 Uiso 1 1 calc R . . H95B H 0.3880 0.6794 0.0607 0.196 Uiso 1 1 calc R . . C96 C 0.3862(14) 0.6743(7) 0.1605(10) 0.177(8) Uani 1 1 d DU . . H96A H 0.4412 0.6816 0.1983 0.213 Uiso 1 1 calc R . . H96B H 0.3510 0.7014 0.1476 0.213 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 0.01981(13) 0.02307(15) 0.02630(13) 0.00021(10) 0.00903(10) 0.00025(10) U2 0.02429(14) 0.02296(15) 0.02749(14) -0.00066(10) 0.01096(11) -0.00043(10) O1 0.018(2) 0.026(3) 0.032(3) 0.0018(19) 0.005(2) 0.0004(19) O2 0.014(2) 0.029(3) 0.022(2) 0.0038(18) 0.0031(18) 0.0022(18) O3 0.031(3) 0.021(3) 0.028(2) 0.0016(19) 0.009(2) -0.001(2) O4 0.027(3) 0.029(3) 0.029(2) 0.001(2) 0.013(2) 0.000(2) O5 0.027(3) 0.021(3) 0.030(2) -0.0039(19) 0.009(2) 0.006(2) O6 0.024(3) 0.034(3) 0.033(3) 0.000(2) 0.013(2) 0.000(2) O7 0.028(2) 0.022(3) 0.026(2) 0.0005(19) 0.010(2) 0.0006(19) O8 0.024(2) 0.029(3) 0.026(2) -0.0023(19) 0.007(2) 0.000(2) O9 0.026(3) 0.034(3) 0.035(3) 0.000(2) 0.015(2) 0.001(2) O10 0.030(3) 0.033(3) 0.024(2) 0.0043(19) 0.012(2) -0.003(2) O11 0.031(3) 0.026(3) 0.029(3) -0.0049(19) 0.007(2) -0.009(2) O12 0.036(3) 0.017(3) 0.037(3) 0.000(2) 0.014(2) -0.002(2) N1 0.020(3) 0.027(3) 0.027(3) 0.003(2) 0.009(2) 0.002(2) N2 0.019(3) 0.022(3) 0.027(3) -0.003(2) 0.007(2) -0.001(2) N3 0.029(3) 0.023(3) 0.031(3) 0.000(2) 0.010(3) -0.003(2) N4 0.030(3) 0.028(4) 0.032(3) 0.002(2) 0.012(3) 0.001(3) C1 0.023(3) 0.021(4) 0.028(4) 0.000(3) 0.012(3) -0.003(3) C2 0.022(3) 0.032(4) 0.019(3) -0.001(3) 0.008(3) -0.002(3) C3 0.023(4) 0.026(4) 0.021(3) -0.005(3) 0.005(3) 0.003(3) C4 0.027(4) 0.029(4) 0.027(4) 0.000(3) 0.006(3) -0.003(3) C5 0.025(4) 0.030(4) 0.023(3) 0.000(3) 0.004(3) -0.005(3) C6 0.029(4) 0.030(5) 0.027(4) 0.004(3) 0.009(3) -0.001(3) C7 0.023(4) 0.029(4) 0.042(4) 0.000(3) -0.002(3) -0.004(3) C8 0.056(4) 0.063(5) 0.089(5) 0.014(4) 0.010(4) -0.008(4) C9 0.037(5) 0.060(7) 0.066(6) -0.019(5) 0.018(4) -0.016(4) C10 0.056(4) 0.073(5) 0.064(4) -0.017(4) 0.016(3) -0.003(4) C11 0.034(4) 0.027(4) 0.024(3) -0.002(3) 0.014(3) 0.001(3) C12 0.032(4) 0.025(4) 0.027(4) 0.002(3) 0.012(3) -0.001(3) C13 0.028(4) 0.019(4) 0.033(4) 0.000(3) 0.017(3) 0.000(3) C14 0.028(4) 0.029(4) 0.034(4) 0.005(3) 0.014(3) 0.004(3) C15 0.027(4) 0.029(4) 0.040(4) 0.005(3) 0.012(3) 0.005(3) C16 0.041(4) 0.025(4) 0.043(4) 0.001(3) 0.017(4) 0.003(3) C17 0.022(4) 0.028(4) 0.038(4) -0.004(3) 0.010(3) -0.002(3) C18 0.019(3) 0.025(4) 0.027(3) 0.000(3) 0.005(3) 0.005(3) C19 0.025(4) 0.025(4) 0.029(4) -0.001(3) 0.013(3) -0.002(3) C20 0.022(4) 0.027(4) 0.026(4) -0.002(3) 0.010(3) -0.002(3) C21 0.021(3) 0.033(4) 0.024(3) -0.001(3) 0.006(3) -0.003(3) C22 0.023(4) 0.031(4) 0.025(3) -0.001(3) 0.006(3) -0.002(3) C23 0.023(4) 0.030(4) 0.032(4) -0.001(3) 0.013(3) -0.003(3) C24 0.021(4) 0.033(4) 0.034(4) 0.004(3) 0.013(3) 0.008(3) C25 0.021(4) 0.029(4) 0.059(5) 0.003(4) 0.015(3) 0.000(3) C26 0.037(5) 0.046(6) 0.095(7) 0.020(5) 0.035(5) 0.010(4) C27 0.021(4) 0.042(5) 0.082(6) 0.014(4) 0.015(4) 0.009(3) C28 0.031(5) 0.076(8) 0.084(7) -0.017(6) 0.006(5) -0.007(5) C29 0.024(4) 0.021(4) 0.031(4) -0.003(3) 0.010(3) -0.006(3) C30 0.022(4) 0.028(4) 0.030(4) -0.004(3) 0.014(3) -0.001(3) C31 0.014(3) 0.028(4) 0.030(4) -0.003(3) 0.006(3) -0.001(3) C32 0.028(4) 0.021(4) 0.030(4) -0.002(3) 0.010(3) -0.002(3) C33 0.024(4) 0.032(4) 0.033(4) -0.003(3) 0.012(3) -0.001(3) C34 0.020(3) 0.026(4) 0.029(4) 0.000(3) 0.009(3) 0.003(3) C35 0.030(4) 0.029(4) 0.031(4) -0.003(3) 0.010(3) -0.002(3) C36 0.041(5) 0.039(5) 0.041(4) -0.008(3) 0.014(4) 0.002(4) C37 0.034(4) 0.041(5) 0.040(4) -0.005(3) 0.010(3) -0.007(3) C38 0.041(4) 0.034(5) 0.031(4) -0.004(3) 0.005(3) -0.003(3) C39 0.029(4) 0.028(4) 0.030(4) -0.005(3) 0.013(3) -0.005(3) C40 0.024(4) 0.023(4) 0.031(4) -0.002(3) 0.007(3) -0.001(3) C41 0.035(4) 0.021(4) 0.034(4) 0.004(3) 0.015(3) 0.002(3) C42 0.027(4) 0.031(4) 0.036(4) 0.002(3) 0.010(3) 0.000(3) C43 0.035(4) 0.040(5) 0.032(4) 0.001(3) 0.013(3) 0.000(3) C44 0.039(4) 0.034(5) 0.045(5) 0.009(3) 0.021(4) 0.007(3) C45 0.031(4) 0.032(5) 0.035(4) 0.000(3) 0.011(3) 0.001(3) C46 0.027(4) 0.025(4) 0.030(4) 0.000(3) 0.010(3) -0.004(3) C47 0.025(4) 0.030(4) 0.026(3) -0.002(3) 0.011(3) -0.007(3) C48 0.028(4) 0.023(4) 0.025(3) 0.001(3) 0.008(3) 0.004(3) C49 0.026(4) 0.030(4) 0.022(3) 0.001(3) 0.007(3) 0.000(3) C50 0.023(4) 0.029(4) 0.026(4) 0.003(3) 0.008(3) -0.001(3) C51 0.024(4) 0.031(4) 0.032(4) 0.002(3) 0.009(3) 0.004(3) C52 0.030(4) 0.021(4) 0.033(4) 0.004(3) 0.014(3) 0.001(3) C53 0.039(4) 0.030(4) 0.040(4) 0.000(3) 0.022(3) 0.002(3) C54 0.069(6) 0.043(6) 0.087(7) 0.002(5) 0.056(6) 0.009(5) C55 0.037(5) 0.053(6) 0.057(5) 0.000(4) 0.023(4) 0.007(4) C56 0.046(5) 0.044(5) 0.051(5) -0.006(4) 0.027(4) 0.005(4) C57 0.054(5) 0.030(5) 0.052(5) -0.008(4) 0.008(4) 0.007(4) C58 0.039(4) 0.027(4) 0.028(4) -0.001(3) 0.006(3) 0.010(3) C59 0.032(4) 0.041(5) 0.033(4) 0.003(3) 0.012(3) 0.013(3) C60 0.020(4) 0.060(6) 0.023(4) -0.001(3) 0.007(3) 0.009(3) C61 0.023(4) 0.058(6) 0.059(5) 0.006(4) 0.013(4) 0.004(4) C62 0.037(4) 0.036(5) 0.035(4) 0.004(3) 0.013(3) -0.001(3) C63 0.032(4) 0.035(4) 0.022(4) -0.001(3) 0.010(3) 0.000(3) C64 0.034(4) 0.025(4) 0.032(4) 0.005(3) 0.013(3) 0.001(3) C65 0.019(3) 0.038(4) 0.023(3) -0.004(3) 0.011(3) 0.000(3) C66 0.024(4) 0.045(5) 0.026(4) 0.001(3) 0.005(3) 0.001(3) C67 0.030(4) 0.043(5) 0.045(4) -0.003(4) 0.014(3) -0.002(3) C68 0.026(4) 0.035(5) 0.029(4) -0.012(3) 0.014(3) -0.005(3) C69 0.034(4) 0.029(4) 0.036(4) 0.003(3) 0.017(3) -0.007(3) C70 0.032(4) 0.028(4) 0.027(4) -0.002(3) 0.015(3) -0.007(3) C71 0.049(5) 0.041(5) 0.034(4) 0.007(3) 0.014(4) 0.003(4) C72 0.047(5) 0.042(6) 0.061(6) -0.001(4) 0.005(4) -0.013(4) C73 0.041(4) 0.031(5) 0.032(4) -0.002(3) 0.012(3) -0.009(3) C74 0.050(5) 0.014(4) 0.041(4) -0.006(3) 0.011(4) -0.011(3) C75 0.038(4) 0.025(4) 0.035(4) 0.002(3) 0.023(3) 0.000(3) C76 0.051(5) 0.029(4) 0.035(4) -0.004(3) 0.016(4) 0.001(4) O13 0.132(5) 0.133(6) 0.145(5) -0.001(4) 0.050(4) -0.002(4) C77 0.052(6) 0.046(6) 0.088(7) 0.019(5) 0.018(5) -0.002(5) C78 0.067(5) 0.071(5) 0.080(5) 0.011(4) 0.017(4) 0.001(4) C79 0.072(5) 0.096(6) 0.102(5) 0.013(4) 0.032(4) -0.007(4) C80 0.064(5) 0.069(5) 0.104(5) -0.002(4) 0.025(4) -0.018(4) O14 0.046(3) 0.039(4) 0.048(3) 0.002(3) 0.016(3) -0.002(3) C81 0.058(6) 0.058(6) 0.055(5) 0.015(4) 0.027(5) 0.018(5) C82 0.055(6) 0.076(8) 0.043(5) 0.002(5) 0.010(4) 0.009(5) C83 0.044(5) 0.050(6) 0.063(6) -0.008(4) 0.024(4) -0.012(4) C84 0.049(5) 0.044(5) 0.041(4) 0.005(4) 0.023(4) 0.002(4) O15 0.049(4) 0.046(4) 0.097(5) 0.012(3) 0.036(4) -0.007(3) C85 0.066(7) 0.055(7) 0.084(7) 0.029(5) 0.042(6) 0.010(5) C86 0.108(9) 0.046(6) 0.055(6) 0.001(5) 0.043(6) 0.006(6) C87 0.066(5) 0.067(5) 0.077(5) 0.009(4) 0.019(4) -0.011(4) C88 0.065(5) 0.066(5) 0.080(5) 0.005(4) 0.028(4) -0.002(4) O16 0.109(5) 0.085(5) 0.120(5) -0.018(4) 0.031(4) -0.003(4) C89 0.114(6) 0.105(6) 0.114(6) 0.013(4) 0.041(4) -0.001(4) C90 0.077(5) 0.075(5) 0.074(5) 0.002(4) 0.032(4) -0.008(4) C91 0.061(4) 0.060(5) 0.066(4) 0.003(4) 0.021(3) -0.009(4) C92 0.069(8) 0.105(11) 0.075(7) 0.005(7) 0.033(6) 0.022(7) O17 0.110(5) 0.114(5) 0.118(5) -0.003(4) 0.037(4) -0.010(4) C93 0.128(7) 0.124(7) 0.125(6) -0.015(5) 0.056(5) -0.010(5) C94 0.141(7) 0.131(7) 0.132(7) -0.002(5) 0.063(5) 0.005(5) C95 0.160(8) 0.170(9) 0.167(8) 0.004(5) 0.069(5) -0.015(5) C96 0.180(9) 0.175(9) 0.179(9) 0.003(5) 0.067(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.295(4) . ? U1 O2 2.296(4) . ? U1 O8 2.303(4) . ? U1 O6 2.312(5) . ? U1 O5 2.340(4) . ? U1 O7 2.344(4) . ? U1 N1 2.572(6) . ? U1 N2 2.587(5) . ? U1 U2 4.0252(4) . ? U2 O4 2.182(5) . ? U2 O3 2.213(4) . ? U2 O11 2.332(4) . ? U2 O9 2.346(5) . ? U2 O10 2.355(4) . ? U2 O12 2.423(5) . ? U2 O2 2.527(4) . ? U2 O1 2.628(5) . ? O1 C2 1.357(8) . ? O1 O4 2.732(6) . ? O1 O2 2.734(6) . ? O1 N1 2.837(7) . ? O2 C20 1.346(8) . ? O2 O3 2.777(6) . ? O2 N2 2.824(7) . ? O3 C30 1.320(8) . ? O3 O4 3.024(6) . ? O3 N3 4.007(7) . ? O4 C48 1.332(8) . ? O4 N4 4.073(7) . ? O5 C58 1.276(8) . ? O6 C60 1.301(9) . ? O7 C63 1.284(8) . ? O8 C65 1.294(8) . ? O9 C68 1.278(8) . ? O10 C70 1.281(8) . ? O11 C73 1.274(9) . ? O12 C75 1.271(8) . ? N1 C11 1.276(8) . ? N1 C12 1.435(8) . ? N1 N2 2.636(7) . ? N2 C18 1.287(8) . ? N2 C13 1.430(8) . ? N3 C39 1.278(9) . ? N3 C40 1.434(8) . ? N3 N4 2.873(8) . ? N4 C46 1.288(9) . ? N4 C41 1.406(9) . ? C1 C6 1.412(9) . ? C1 C2 1.416(9) . ? C1 C49 1.483(9) . ? C2 C3 1.412(10) . ? C3 C4 1.392(9) . ? C3 C11 1.451(9) . ? C4 C5 1.397(9) . ? C5 C6 1.397(10) . ? C5 C7 1.519(9) . ? C7 C9 1.514(11) . ? C7 C10 1.523(11) . ? C7 C8 1.537(12) . ? C12 C17 1.385(10) . ? C12 C13 1.398(9) . ? C13 C14 1.381(9) . ? C14 C15 1.384(10) . ? C15 C16 1.395(10) . ? C16 C17 1.373(10) . ? C18 C19 1.458(9) . ? C19 C24 1.399(9) . ? C19 C20 1.408(9) . ? C20 C21 1.402(9) . ? C21 C22 1.392(9) . ? C21 C29 1.502(10) . ? C22 C23 1.401(10) . ? C23 C24 1.379(10) . ? C23 C25 1.522(9) . ? C25 C28 1.526(12) . ? C25 C27 1.529(11) . ? C25 C26 1.534(11) . ? C29 C34 1.405(9) . ? C29 C30 1.414(9) . ? C30 C31 1.415(9) . ? C31 C32 1.399(9) . ? C31 C39 1.469(9) . ? C32 C33 1.413(9) . ? C33 C34 1.380(10) . ? C33 C35 1.544(9) . ? C35 C36 1.536(10) . ? C35 C37 1.542(10) . ? C35 C38 1.545(9) . ? C40 C45 1.395(10) . ? C40 C41 1.397(9) . ? C41 C42 1.408(9) . ? C42 C43 1.389(10) . ? C43 C44 1.394(10) . ? C44 C45 1.392(10) . ? C46 C47 1.465(9) . ? C47 C52 1.398(9) . ? C47 C48 1.407(9) . ? C48 C49 1.427(9) . ? C49 C50 1.408(9) . ? C50 C51 1.401(10) . ? C51 C52 1.385(10) . ? C51 C53 1.533(10) . ? C53 C55 1.521(10) . ? C53 C54 1.527(11) . ? C53 C56 1.532(10) . ? C57 C58 1.503(11) . ? C58 C59 1.399(10) . ? C59 C60 1.367(11) . ? C60 C61 1.507(10) . ? C62 C63 1.504(10) . ? C63 C64 1.389(10) . ? C64 C65 1.378(10) . ? C65 C66 1.522(9) . ? C67 C68 1.501(10) . ? C68 C69 1.409(10) . ? C69 C70 1.390(9) . ? C70 C71 1.510(9) . ? C72 C73 1.509(10) . ? C73 C74 1.392(10) . ? C74 C75 1.401(10) . ? C75 C76 1.498(10) . ? O13 C80 1.419(13) . ? O13 C77 1.512(14) . ? C77 C78 1.515(13) . ? C78 C79 1.483(17) . ? C79 C80 1.463(9) . ? O14 C84 1.421(9) . ? O14 C81 1.443(10) . ? C81 C82 1.516(13) . ? C82 C83 1.505(12) . ? C83 C84 1.500(11) . ? O15 C88 1.415(11) . ? O15 C85 1.427(10) . ? C85 C86 1.522(13) . ? C86 C87 1.525(14) . ? C87 C88 1.505(14) . ? O16 C89 1.364(14) . ? O16 C92 1.419(14) . ? C89 C90 1.460(16) . ? C90 C91 1.521(13) . ? C91 C92 1.489(14) . ? O17 C96 1.34(2) . ? O17 C93 1.460(15) . ? C93 C94 1.499(18) . ? C94 C95 1.53(2) . ? C95 C96 1.50(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 73.08(15) . . ? O1 U1 O8 147.57(16) . . ? O2 U1 O8 78.15(15) . . ? O1 U1 O6 79.95(16) . . ? O2 U1 O6 144.96(15) . . ? O8 U1 O6 118.63(16) . . ? O1 U1 O5 82.28(15) . . ? O2 U1 O5 81.84(16) . . ? O8 U1 O5 79.10(16) . . ? O6 U1 O5 72.62(17) . . ? O1 U1 O7 140.86(16) . . ? O2 U1 O7 137.08(15) . . ? O8 U1 O7 71.51(16) . . ? O6 U1 O7 77.54(16) . . ? O5 U1 O7 119.97(15) . . ? O1 U1 N1 71.04(16) . . ? O2 U1 N1 106.67(16) . . ? O8 U1 N1 132.95(16) . . ? O6 U1 N1 84.59(17) . . ? O5 U1 N1 147.57(16) . . ? O7 U1 N1 75.30(16) . . ? O1 U1 N2 105.60(16) . . ? O2 U1 N2 70.37(16) . . ? O8 U1 N2 77.81(16) . . ? O6 U1 N2 140.02(17) . . ? O5 U1 N2 146.84(17) . . ? O7 U1 N2 74.04(16) . . ? N1 U1 N2 61.45(16) . . ? O4 U2 O3 86.95(17) . . ? O4 U2 O11 82.19(17) . . ? O3 U2 O11 157.73(16) . . ? O4 U2 O9 148.58(17) . . ? O3 U2 O9 75.43(17) . . ? O11 U2 O9 104.61(17) . . ? O4 U2 O10 79.94(16) . . ? O3 U2 O10 78.77(16) . . ? O11 U2 O10 80.22(16) . . ? O9 U2 O10 71.32(16) . . ? O4 U2 O12 139.82(17) . . ? O3 U2 O12 128.62(16) . . ? O11 U2 O12 69.43(16) . . ? O9 U2 O12 68.84(16) . . ? O10 U2 O12 120.44(16) . . ? O4 U2 O2 110.67(15) . . ? O3 U2 O2 71.38(15) . . ? O11 U2 O2 130.73(15) . . ? O9 U2 O2 88.38(15) . . ? O10 U2 O2 147.37(15) . . ? O12 U2 O2 71.90(15) . . ? O4 U2 O1 68.48(15) . . ? O3 U2 O1 114.70(15) . . ? O11 U2 O1 79.19(15) . . ? O9 U2 O1 142.63(15) . . ? O10 U2 O1 144.18(14) . . ? O12 U2 O1 78.45(15) . . ? O2 U2 O1 64.01(13) . . ? C2 O1 U1 126.7(4) . . ? C2 O1 U2 121.8(4) . . ? U1 O1 U2 109.50(17) . . ? C20 O2 U1 124.8(4) . . ? C20 O2 U2 120.3(4) . . ? U1 O2 U2 113.04(16) . . ? C30 O3 U2 148.8(4) . . ? C48 O4 U2 160.9(4) . . ? C58 O5 U1 135.0(5) . . ? C60 O6 U1 135.4(5) . . ? C63 O7 U1 133.4(4) . . ? C65 O8 U1 133.6(4) . . ? C68 O9 U2 131.9(5) . . ? C70 O10 U2 131.8(4) . . ? C73 O11 U2 140.5(5) . . ? C75 O12 U2 137.7(4) . . ? C11 N1 C12 118.3(6) . . ? C11 N1 U1 126.6(5) . . ? C12 N1 U1 115.1(4) . . ? C18 N2 C13 118.0(6) . . ? C18 N2 U1 127.8(4) . . ? C13 N2 U1 114.2(4) . . ? C39 N3 C40 116.6(6) . . ? C46 N4 C41 115.6(6) . . ? C6 C1 C2 117.7(6) . . ? C6 C1 C49 115.6(6) . . ? C2 C1 C49 126.7(6) . . ? O1 C2 C3 120.0(6) . . ? O1 C2 C1 121.8(6) . . ? C3 C2 C1 118.2(6) . . ? C4 C3 C2 121.6(6) . . ? C4 C3 C11 114.9(6) . . ? C2 C3 C11 123.4(6) . . ? C3 C4 C5 121.7(7) . . ? C6 C5 C4 116.0(6) . . ? C6 C5 C7 121.2(6) . . ? C4 C5 C7 122.8(6) . . ? C5 C6 C1 124.6(6) . . ? C9 C7 C5 112.3(6) . . ? C9 C7 C10 109.0(7) . . ? C5 C7 C10 108.4(7) . . ? C9 C7 C8 108.3(8) . . ? C5 C7 C8 111.8(6) . . ? C10 C7 C8 106.9(7) . . ? N1 C11 C3 126.1(6) . . ? C17 C12 C13 120.3(6) . . ? C17 C12 N1 124.8(6) . . ? C13 C12 N1 114.9(6) . . ? C14 C13 C12 119.9(6) . . ? C14 C13 N2 123.8(6) . . ? C12 C13 N2 116.3(6) . . ? C13 C14 C15 119.8(7) . . ? C14 C15 C16 119.9(7) . . ? C17 C16 C15 120.6(7) . . ? C16 C17 C12 119.5(7) . . ? N2 C18 C19 123.8(6) . . ? C24 C19 C20 121.0(6) . . ? C24 C19 C18 115.3(6) . . ? C20 C19 C18 123.3(6) . . ? O2 C20 C21 122.2(6) . . ? O2 C20 C19 120.6(6) . . ? C21 C20 C19 117.1(6) . . ? C22 C21 C20 119.8(7) . . ? C22 C21 C29 116.7(6) . . ? C20 C21 C29 123.4(6) . . ? C21 C22 C23 123.8(7) . . ? C24 C23 C22 115.4(6) . . ? C24 C23 C25 123.6(6) . . ? C22 C23 C25 120.9(6) . . ? C23 C24 C19 122.7(7) . . ? C23 C25 C28 109.2(7) . . ? C23 C25 C27 111.5(6) . . ? C28 C25 C27 109.0(7) . . ? C23 C25 C26 109.2(6) . . ? C28 C25 C26 109.4(7) . . ? C27 C25 C26 108.3(7) . . ? C34 C29 C30 118.5(6) . . ? C34 C29 C21 119.5(6) . . ? C30 C29 C21 121.6(6) . . ? O3 C30 C29 121.1(6) . . ? O3 C30 C31 120.4(6) . . ? C29 C30 C31 118.2(6) . . ? C32 C31 C30 120.7(6) . . ? C32 C31 C39 123.0(6) . . ? C30 C31 C39 116.0(6) . . ? C31 C32 C33 121.2(6) . . ? C34 C33 C32 116.8(6) . . ? C34 C33 C35 123.0(6) . . ? C32 C33 C35 120.1(6) . . ? C33 C34 C29 124.0(6) . . ? C36 C35 C37 110.3(6) . . ? C36 C35 C33 108.7(6) . . ? C37 C35 C33 109.4(6) . . ? C36 C35 C38 109.3(6) . . ? C37 C35 C38 108.1(6) . . ? C33 C35 C38 111.1(6) . . ? N3 C39 C31 124.1(6) . . ? C45 C40 C41 119.6(6) . . ? C45 C40 N3 119.4(6) . . ? C41 C40 N3 120.8(6) . . ? C40 C41 N4 121.8(6) . . ? C40 C41 C42 118.7(6) . . ? N4 C41 C42 119.5(6) . . ? C43 C42 C41 121.0(7) . . ? C42 C43 C44 120.3(7) . . ? C45 C44 C43 118.6(7) . . ? C44 C45 C40 121.8(7) . . ? N4 C46 C47 122.7(7) . . ? C52 C47 C48 121.9(6) . . ? C52 C47 C46 119.9(6) . . ? C48 C47 C46 117.9(6) . . ? O4 C48 C47 120.7(6) . . ? O4 C48 C49 121.5(6) . . ? C47 C48 C49 117.8(6) . . ? C50 C49 C48 117.5(6) . . ? C50 C49 C1 118.7(6) . . ? C48 C49 C1 123.3(6) . . ? C51 C50 C49 124.1(6) . . ? C52 C51 C50 116.8(6) . . ? C52 C51 C53 123.4(6) . . ? C50 C51 C53 119.7(6) . . ? C51 C52 C47 121.0(6) . . ? C55 C53 C54 108.6(7) . . ? C55 C53 C56 109.2(6) . . ? C54 C53 C56 107.1(7) . . ? C55 C53 C51 109.8(6) . . ? C54 C53 C51 112.0(6) . . ? C56 C53 C51 110.1(6) . . ? O5 C58 C59 124.1(7) . . ? O5 C58 C57 115.1(7) . . ? C59 C58 C57 120.8(7) . . ? C60 C59 C58 124.3(7) . . ? O6 C60 C59 125.0(7) . . ? O6 C60 C61 114.0(7) . . ? C59 C60 C61 120.9(7) . . ? O7 C63 C64 123.4(7) . . ? O7 C63 C62 116.1(6) . . ? C64 C63 C62 120.5(6) . . ? C65 C64 C63 124.5(7) . . ? O8 C65 C64 123.8(6) . . ? O8 C65 C66 114.6(6) . . ? C64 C65 C66 121.6(6) . . ? O9 C68 C69 123.6(6) . . ? O9 C68 C67 116.7(7) . . ? C69 C68 C67 119.6(7) . . ? C70 C69 C68 123.4(7) . . ? O10 C70 C69 125.2(6) . . ? O10 C70 C71 115.3(6) . . ? C69 C70 C71 119.5(6) . . ? O11 C73 C74 123.8(7) . . ? O11 C73 C72 116.0(7) . . ? C74 C73 C72 120.1(7) . . ? C73 C74 C75 123.2(7) . . ? O12 C75 C74 123.3(7) . . ? O12 C75 C76 116.9(6) . . ? C74 C75 C76 119.7(7) . . ? C80 O13 C77 106.6(9) . . ? O13 C77 C78 104.7(8) . . ? C79 C78 C77 106.8(9) . . ? C80 C79 C78 103.4(9) . . ? O13 C80 C79 109.1(10) . . ? C84 O14 C81 108.6(6) . . ? O14 C81 C82 105.8(7) . . ? C83 C82 C81 103.1(7) . . ? C84 C83 C82 101.4(7) . . ? O14 C84 C83 107.8(6) . . ? C88 O15 C85 105.3(7) . . ? O15 C85 C86 104.3(8) . . ? C85 C86 C87 102.9(8) . . ? C88 C87 C86 104.6(8) . . ? O15 C88 C87 107.0(9) . . ? C89 O16 C92 110.1(10) . . ? O16 C89 C90 110.0(11) . . ? C89 C90 C91 103.5(9) . . ? C92 C91 C90 103.5(9) . . ? O16 C92 C91 104.6(9) . . ? C96 O17 C93 103.0(12) . . ? O17 C93 C94 114.2(13) . . ? C93 C94 C95 96.1(13) . . ? C96 C95 C94 109.5(16) . . ? O17 C96 C95 109.9(17) . . ? #===END data_4.2py _database_code_depnum_ccdc_archive 'CCDC 609882' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H102 N6 O14 U2' _chemical_formula_weight 1979.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.5199(4) _cell_length_b 16.7753(6) _cell_length_c 18.1932(8) _cell_angle_alpha 77.591(2) _cell_angle_beta 81.494(3) _cell_angle_gamma 68.004(2) _cell_volume 4277.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 158460 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method ? _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 3.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.421 _exptl_absorpt_correction_T_max 0.707 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and seven \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 158460 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.68 _reflns_number_total 16208 _reflns_number_gt 13016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atom bound to O4 was found on a Fourier-difference map and all the other ones were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (OH, CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+2.2489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 16208 _refine_ls_number_parameters 1040 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.899 _refine_diff_density_min -1.861 _refine_diff_density_rms 0.098 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 -0.044353(10) 0.481509(9) 0.802208(8) 0.02117(5) Uani 1 1 d . . . U2 U 0.290738(10) 0.197125(9) 0.595230(8) 0.02247(5) Uani 1 1 d . . . O1 O 0.05510(18) 0.51893(17) 0.70934(15) 0.0212(6) Uani 1 1 d . . . O2 O 0.02680(18) 0.34664(17) 0.78267(16) 0.0245(6) Uani 1 1 d . . . O3 O 0.21289(18) 0.23717(18) 0.70086(15) 0.0236(6) Uani 1 1 d . . . O4 O 0.23459(19) 0.43332(18) 0.71188(17) 0.0273(6) Uani 1 1 d . . . H4 H 0.1726 0.4515 0.7054 0.033 Uiso 1 1 d R . . O5 O -0.05797(19) 0.62607(18) 0.80782(16) 0.0256(6) Uani 1 1 d . . . O6 O -0.19871(19) 0.56253(19) 0.84646(16) 0.0275(6) Uani 1 1 d . . . O7 O -0.0732(2) 0.4094(2) 0.92284(17) 0.0320(7) Uani 1 1 d . . . O8 O 0.07694(19) 0.46096(19) 0.87431(16) 0.0271(6) Uani 1 1 d . . . O9 O 0.2859(2) 0.33268(18) 0.52834(16) 0.0268(6) Uani 1 1 d . . . O10 O 0.13562(19) 0.28253(18) 0.56669(16) 0.0249(6) Uani 1 1 d . . . O11 O 0.2267(2) 0.08653(18) 0.61867(17) 0.0297(7) Uani 1 1 d . . . O12 O 0.37938(19) 0.07586(18) 0.68373(17) 0.0289(7) Uani 1 1 d . . . O13 O 0.4424(2) 0.14514(19) 0.53307(17) 0.0306(7) Uani 1 1 d . . . O14 O 0.2813(2) 0.16709(19) 0.47564(16) 0.0305(7) Uani 1 1 d . . . N1 N -0.1340(2) 0.5742(2) 0.68333(18) 0.0207(7) Uani 1 1 d . . . N2 N -0.1586(2) 0.4268(2) 0.75332(19) 0.0226(7) Uani 1 1 d . . . N3 N 0.3877(2) 0.2539(2) 0.65983(19) 0.0232(7) Uani 1 1 d . . . N4 N 0.4120(2) 0.3211(2) 0.74518(19) 0.0236(7) Uani 1 1 d . . . N5 N 0.3127(3) 0.8082(3) 0.2379(3) 0.0511(12) Uani 1 1 d . . . N6 N 0.4552(4) 0.6045(4) 0.0582(3) 0.0752(17) Uani 1 1 d . . . C1 C 0.1285(3) 0.6232(3) 0.6580(2) 0.0240(9) Uani 1 1 d . . . C2 C 0.0542(3) 0.5925(3) 0.6644(2) 0.0223(8) Uani 1 1 d . . . C3 C -0.0228(3) 0.6429(3) 0.6201(2) 0.0219(8) Uani 1 1 d . . . C4 C -0.0204(3) 0.7163(3) 0.5672(2) 0.0228(8) Uani 1 1 d . . . H4A H -0.0709 0.7476 0.5382 0.027 Uiso 1 1 calc R . . C5 C 0.0552(3) 0.7439(3) 0.5568(2) 0.0241(9) Uani 1 1 d . . . C6 C 0.1278(3) 0.6963(3) 0.6031(2) 0.0248(9) Uani 1 1 d . . . H6 H 0.1788 0.7140 0.5973 0.030 Uiso 1 1 calc R . . C7 C 0.0552(3) 0.8243(3) 0.4969(3) 0.0291(9) Uani 1 1 d . . . C8 C 0.0552(3) 0.8058(3) 0.4179(3) 0.0365(11) Uani 1 1 d . . . H8A H 0.0576 0.8552 0.3807 0.055 Uiso 1 1 calc R . . H8B H -0.0006 0.7952 0.4143 0.055 Uiso 1 1 calc R . . H8C H 0.1086 0.7553 0.4091 0.055 Uiso 1 1 calc R . . C9 C 0.1412(3) 0.8484(3) 0.4993(3) 0.0335(10) Uani 1 1 d . . . H9A H 0.1377 0.8999 0.4628 0.050 Uiso 1 1 calc R . . H9B H 0.1967 0.8011 0.4878 0.050 Uiso 1 1 calc R . . H9C H 0.1427 0.8591 0.5487 0.050 Uiso 1 1 calc R . . C10 C -0.0332(3) 0.9022(3) 0.5123(3) 0.0358(11) Uani 1 1 d . . . H10A H -0.0338 0.9134 0.5620 0.054 Uiso 1 1 calc R . . H10B H -0.0873 0.8890 0.5088 0.054 Uiso 1 1 calc R . . H10C H -0.0335 0.9530 0.4757 0.054 Uiso 1 1 calc R . . C11 C -0.1083(3) 0.6252(3) 0.6280(2) 0.0218(8) Uani 1 1 d . . . H11 H -0.1486 0.6532 0.5898 0.026 Uiso 1 1 calc R . . C12 C -0.2246(3) 0.5712(3) 0.6837(2) 0.0219(8) Uani 1 1 d . . . C13 C -0.2386(3) 0.4944(3) 0.7209(2) 0.0225(8) Uani 1 1 d . . . C14 C -0.3273(3) 0.4888(3) 0.7262(2) 0.0252(9) Uani 1 1 d . . . H14 H -0.3370 0.4381 0.7516 0.030 Uiso 1 1 calc R . . C15 C -0.4001(3) 0.5584(3) 0.6938(3) 0.0276(9) Uani 1 1 d . . . H15 H -0.4587 0.5542 0.6967 0.033 Uiso 1 1 calc R . . C16 C -0.3863(3) 0.6346(3) 0.6569(2) 0.0260(9) Uani 1 1 d . . . H16 H -0.4356 0.6812 0.6348 0.031 Uiso 1 1 calc R . . C17 C -0.2999(3) 0.6418(3) 0.6526(2) 0.0238(9) Uani 1 1 d . . . H17 H -0.2916 0.6937 0.6290 0.029 Uiso 1 1 calc R . . C18 C -0.1518(3) 0.3462(3) 0.7572(2) 0.0238(9) Uani 1 1 d . . . H18 H -0.2013 0.3375 0.7410 0.029 Uiso 1 1 calc R . . C19 C -0.0752(3) 0.2694(3) 0.7839(2) 0.0243(9) Uani 1 1 d . . . C20 C 0.0131(3) 0.2717(3) 0.7939(2) 0.0229(8) Uani 1 1 d . . . C21 C 0.0848(3) 0.1913(3) 0.8173(2) 0.0228(8) Uani 1 1 d . . . C22 C 0.0655(3) 0.1150(3) 0.8339(2) 0.0254(9) Uani 1 1 d . . . H22 H 0.1127 0.0633 0.8512 0.030 Uiso 1 1 calc R . . C23 C -0.0217(3) 0.1112(3) 0.8259(2) 0.0266(9) Uani 1 1 d . . . C24 C -0.0896(3) 0.1894(3) 0.7989(2) 0.0259(9) Uani 1 1 d . . . H24 H -0.1470 0.1890 0.7902 0.031 Uiso 1 1 calc R . . C25 C -0.0447(3) 0.0275(3) 0.8494(3) 0.0341(10) Uani 1 1 d . . . C26 C 0.0384(4) -0.0518(3) 0.8786(3) 0.0465(13) Uani 1 1 d . . . H26A H 0.0214 -0.1029 0.8899 0.070 Uiso 1 1 calc R . . H26B H 0.0564 -0.0428 0.9235 0.070 Uiso 1 1 calc R . . H26C H 0.0896 -0.0598 0.8407 0.070 Uiso 1 1 calc R . . C27 C -0.1233(4) 0.0422(3) 0.9140(3) 0.0464(13) Uani 1 1 d . . . H27A H -0.1349 -0.0112 0.9330 0.070 Uiso 1 1 calc R . . H27B H -0.1791 0.0868 0.8950 0.070 Uiso 1 1 calc R . . H27C H -0.1046 0.0600 0.9539 0.070 Uiso 1 1 calc R . . C28 C -0.0806(3) 0.0076(3) 0.7838(3) 0.0408(12) Uani 1 1 d . . . H28A H -0.0324 -0.0035 0.7436 0.061 Uiso 1 1 calc R . . H28B H -0.1338 0.0567 0.7658 0.061 Uiso 1 1 calc R . . H28C H -0.0981 -0.0429 0.8009 0.061 Uiso 1 1 calc R . . C29 C 0.1767(3) 0.1919(2) 0.8311(2) 0.0226(8) Uani 1 1 d . . . C30 C 0.2344(3) 0.2204(3) 0.7716(2) 0.0226(8) Uani 1 1 d . . . C31 C 0.3152(3) 0.2286(3) 0.7899(2) 0.0229(8) Uani 1 1 d . . . C32 C 0.3428(3) 0.1996(3) 0.8642(2) 0.0233(9) Uani 1 1 d . . . H32 H 0.3978 0.2035 0.8748 0.028 Uiso 1 1 calc R . . C33 C 0.2909(3) 0.1656(3) 0.9223(2) 0.0259(9) Uani 1 1 d . . . C34 C 0.2070(3) 0.1637(3) 0.9037(2) 0.0246(9) Uani 1 1 d . . . H34 H 0.1699 0.1426 0.9418 0.030 Uiso 1 1 calc R . . C35 C 0.3246(3) 0.1258(3) 1.0013(2) 0.0264(9) Uani 1 1 d . . . C36 C 0.3653(4) 0.0258(3) 1.0081(3) 0.0393(11) Uani 1 1 d . . . H36A H 0.3177 0.0052 1.0010 0.059 Uiso 1 1 calc R . . H36B H 0.3877 0.0000 1.0573 0.059 Uiso 1 1 calc R . . H36C H 0.4159 0.0099 0.9704 0.059 Uiso 1 1 calc R . . C37 C 0.3999(3) 0.1577(3) 1.0177(3) 0.0348(11) Uani 1 1 d . . . H37A H 0.4549 0.1370 0.9849 0.052 Uiso 1 1 calc R . . H37B H 0.4149 0.1356 1.0693 0.052 Uiso 1 1 calc R . . H37C H 0.3769 0.2204 1.0092 0.052 Uiso 1 1 calc R . . C38 C 0.2437(3) 0.1492(3) 1.0621(3) 0.0351(11) Uani 1 1 d . . . H38A H 0.2176 0.2114 1.0588 0.053 Uiso 1 1 calc R . . H38B H 0.2664 0.1226 1.1110 0.053 Uiso 1 1 calc R . . H38C H 0.1967 0.1282 1.0543 0.053 Uiso 1 1 calc R . . C39 C 0.3708(3) 0.2670(2) 0.7307(2) 0.0226(8) Uani 1 1 d . . . C40 C 0.4451(3) 0.3020(3) 0.6251(2) 0.0261(9) Uani 1 1 d . . . C41 C 0.4594(3) 0.3440(3) 0.6781(2) 0.0260(9) Uani 1 1 d . . . C42 C 0.5140(3) 0.3966(3) 0.6614(3) 0.0320(10) Uani 1 1 d . . . H42 H 0.5230 0.4240 0.6974 0.038 Uiso 1 1 calc R . . C43 C 0.5537(3) 0.4057(3) 0.5884(3) 0.0388(11) Uani 1 1 d . . . H43 H 0.5906 0.4401 0.5747 0.047 Uiso 1 1 calc R . . C44 C 0.5396(3) 0.3642(3) 0.5343(3) 0.0365(11) Uani 1 1 d . . . H44 H 0.5673 0.3718 0.4856 0.044 Uiso 1 1 calc R . . C45 C 0.4853(3) 0.3121(3) 0.5518(3) 0.0305(10) Uani 1 1 d . . . H45 H 0.4761 0.2848 0.5157 0.037 Uiso 1 1 calc R . . C46 C 0.3814(3) 0.3743(3) 0.8052(2) 0.0238(9) Uani 1 1 d . . . H46A H 0.4355 0.3680 0.8297 0.029 Uiso 1 1 calc R . . H46B H 0.3408 0.3521 0.8426 0.029 Uiso 1 1 calc R . . C47 C 0.3304(3) 0.4703(3) 0.7774(2) 0.0229(8) Uani 1 1 d . . . C48 C 0.2547(3) 0.4971(3) 0.7334(2) 0.0239(9) Uani 1 1 d . . . C49 C 0.2057(3) 0.5865(3) 0.7102(2) 0.0233(9) Uani 1 1 d . . . C50 C 0.2326(3) 0.6459(3) 0.7354(2) 0.0253(9) Uani 1 1 d . . . H50 H 0.1982 0.7050 0.7224 0.030 Uiso 1 1 calc R . . C51 C 0.3077(3) 0.6219(3) 0.7788(2) 0.0236(9) Uani 1 1 d . . . C52 C 0.3570(3) 0.5323(3) 0.7991(2) 0.0232(8) Uani 1 1 d . . . H52 H 0.4084 0.5138 0.8274 0.028 Uiso 1 1 calc R . . C53 C 0.3354(3) 0.6926(3) 0.7992(2) 0.0262(9) Uani 1 1 d . . . C54 C 0.3625(3) 0.7458(3) 0.7258(3) 0.0308(10) Uani 1 1 d . . . H54A H 0.3853 0.7870 0.7377 0.046 Uiso 1 1 calc R . . H54B H 0.3088 0.7765 0.6972 0.046 Uiso 1 1 calc R . . H54C H 0.4102 0.7072 0.6966 0.046 Uiso 1 1 calc R . . C55 C 0.2523(3) 0.7551(3) 0.8417(3) 0.0324(10) Uani 1 1 d . . . H55A H 0.2361 0.7231 0.8886 0.049 Uiso 1 1 calc R . . H55B H 0.1998 0.7798 0.8114 0.049 Uiso 1 1 calc R . . H55C H 0.2695 0.8009 0.8514 0.049 Uiso 1 1 calc R . . C56 C 0.4175(3) 0.6544(3) 0.8494(3) 0.0307(10) Uani 1 1 d . . . H56A H 0.4009 0.6212 0.8955 0.046 Uiso 1 1 calc R . . H56B H 0.4322 0.7009 0.8607 0.046 Uiso 1 1 calc R . . H56C H 0.4707 0.6170 0.8235 0.046 Uiso 1 1 calc R . . C57 C -0.0926(3) 0.7781(3) 0.7740(3) 0.0333(10) Uani 1 1 d . . . H57A H -0.0537 0.7781 0.8104 0.050 Uiso 1 1 calc R . . H57B H -0.1467 0.8306 0.7708 0.050 Uiso 1 1 calc R . . H57C H -0.0584 0.7753 0.7255 0.050 Uiso 1 1 calc R . . C58 C -0.1224(3) 0.7003(3) 0.7978(2) 0.0269(9) Uani 1 1 d . . . C59 C -0.2177(3) 0.7116(3) 0.8084(2) 0.0280(9) Uani 1 1 d . . . H59 H -0.2612 0.7676 0.7967 0.034 Uiso 1 1 calc R . . C60 C -0.2501(3) 0.6427(3) 0.8357(2) 0.0276(9) Uani 1 1 d . . . C61 C -0.3525(3) 0.6612(3) 0.8558(3) 0.0355(11) Uani 1 1 d . . . H61A H -0.3746 0.6323 0.8267 0.053 Uiso 1 1 calc R . . H61B H -0.3859 0.7230 0.8449 0.053 Uiso 1 1 calc R . . H61C H -0.3625 0.6402 0.9086 0.053 Uiso 1 1 calc R . . C62 C -0.0820(4) 0.3371(4) 1.0487(3) 0.0549(15) Uani 1 1 d . . . H62A H -0.1469 0.3727 1.0520 0.082 Uiso 1 1 calc R . . H62B H -0.0557 0.3309 1.0951 0.082 Uiso 1 1 calc R . . H62C H -0.0754 0.2806 1.0400 0.082 Uiso 1 1 calc R . . C63 C -0.0323(3) 0.3793(3) 0.9849(3) 0.0360(11) Uani 1 1 d . . . C64 C 0.0517(3) 0.3851(3) 0.9949(3) 0.0373(11) Uani 1 1 d . . . H64 H 0.0758 0.3608 1.0418 0.045 Uiso 1 1 calc R . . C65 C 0.1026(3) 0.4246(3) 0.9402(3) 0.0299(10) Uani 1 1 d . . . C66 C 0.1938(3) 0.4248(3) 0.9591(3) 0.0358(11) Uani 1 1 d . . . H66A H 0.2382 0.3663 0.9658 0.054 Uiso 1 1 calc R . . H66B H 0.1845 0.4478 1.0048 0.054 Uiso 1 1 calc R . . H66C H 0.2168 0.4606 0.9186 0.054 Uiso 1 1 calc R . . C67 C 0.2625(3) 0.4834(3) 0.5064(3) 0.0334(10) Uani 1 1 d . . . H67A H 0.3078 0.4770 0.5399 0.050 Uiso 1 1 calc R . . H67B H 0.2122 0.5382 0.5077 0.050 Uiso 1 1 calc R . . H67C H 0.2912 0.4819 0.4559 0.050 Uiso 1 1 calc R . . C68 C 0.2257(3) 0.4103(3) 0.5305(2) 0.0280(9) Uani 1 1 d . . . C69 C 0.1323(3) 0.4273(3) 0.5520(2) 0.0286(9) Uani 1 1 d . . . H69 H 0.0943 0.4846 0.5553 0.034 Uiso 1 1 calc R . . C70 C 0.0911(3) 0.3626(3) 0.5693(2) 0.0242(9) Uani 1 1 d . . . C71 C -0.0116(3) 0.3885(3) 0.5897(3) 0.0316(10) Uani 1 1 d . . . H71A H -0.0406 0.3765 0.5523 0.047 Uiso 1 1 calc R . . H71B H -0.0376 0.4498 0.5917 0.047 Uiso 1 1 calc R . . H71C H -0.0225 0.3559 0.6381 0.047 Uiso 1 1 calc R . . C72 C 0.1562(4) -0.0172(3) 0.6663(3) 0.0439(12) Uani 1 1 d . . . H72A H 0.0944 0.0247 0.6715 0.066 Uiso 1 1 calc R . . H72B H 0.1638 -0.0667 0.7060 0.066 Uiso 1 1 calc R . . H72C H 0.1660 -0.0357 0.6183 0.066 Uiso 1 1 calc R . . C73 C 0.2259(3) 0.0237(3) 0.6708(3) 0.0287(9) Uani 1 1 d . . . C74 C 0.2852(3) -0.0095(3) 0.7298(3) 0.0317(10) Uani 1 1 d . . . H74 H 0.2747 -0.0513 0.7691 0.038 Uiso 1 1 calc R . . C75 C 0.3596(3) 0.0175(3) 0.7324(2) 0.0276(9) Uani 1 1 d . . . C76 C 0.4236(3) -0.0261(3) 0.7957(3) 0.0380(11) Uani 1 1 d . . . H76A H 0.4871 -0.0460 0.7749 0.057 Uiso 1 1 calc R . . H76B H 0.4087 -0.0750 0.8244 0.057 Uiso 1 1 calc R . . H76C H 0.4157 0.0150 0.8279 0.057 Uiso 1 1 calc R . . C77 C 0.5848(3) 0.0927(3) 0.4605(3) 0.0431(12) Uani 1 1 d . . . H77A H 0.5985 0.1454 0.4509 0.065 Uiso 1 1 calc R . . H77B H 0.6079 0.0634 0.4179 0.065 Uiso 1 1 calc R . . H77C H 0.6140 0.0553 0.5046 0.065 Uiso 1 1 calc R . . C78 C 0.4809(3) 0.1149(3) 0.4730(3) 0.0329(10) Uani 1 1 d . . . C79 C 0.4324(4) 0.1031(3) 0.4202(3) 0.0389(11) Uani 1 1 d . . . H79 H 0.4666 0.0765 0.3799 0.047 Uiso 1 1 calc R . . C80 C 0.3359(3) 0.1285(3) 0.4239(2) 0.0333(10) Uani 1 1 d . . . C81 C 0.2884(4) 0.1123(3) 0.3654(3) 0.0467(13) Uani 1 1 d . . . H81A H 0.2567 0.0728 0.3887 0.070 Uiso 1 1 calc R . . H81B H 0.3341 0.0872 0.3270 0.070 Uiso 1 1 calc R . . H81C H 0.2441 0.1665 0.3429 0.070 Uiso 1 1 calc R . . C82 C 0.2990(3) 0.8131(4) 0.3109(3) 0.0466(13) Uani 1 1 d . . . H82 H 0.2570 0.7896 0.3402 0.056 Uiso 1 1 calc R . . C83 C 0.3430(3) 0.8506(4) 0.3459(3) 0.0465(13) Uani 1 1 d . . . H83 H 0.3313 0.8515 0.3974 0.056 Uiso 1 1 calc R . . C84 C 0.4050(3) 0.8869(3) 0.3029(3) 0.0400(12) Uani 1 1 d . . . H84 H 0.4363 0.9124 0.3249 0.048 Uiso 1 1 calc R . . C85 C 0.4188(3) 0.8843(3) 0.2271(3) 0.0434(12) Uani 1 1 d . . . H85 H 0.4590 0.9090 0.1965 0.052 Uiso 1 1 calc R . . C86 C 0.3722(3) 0.8444(4) 0.1968(3) 0.0465(13) Uani 1 1 d . . . H86 H 0.3825 0.8426 0.1455 0.056 Uiso 1 1 calc R . . C87 C 0.4182(5) 0.6888(5) 0.0518(4) 0.0731(19) Uani 1 1 d U . . H87 H 0.4571 0.7210 0.0454 0.088 Uiso 1 1 calc R . . C88 C 0.3236(6) 0.7317(6) 0.0542(5) 0.100(3) Uani 1 1 d U . . H88 H 0.2983 0.7922 0.0491 0.120 Uiso 1 1 calc R . . C89 C 0.2656(5) 0.6820(5) 0.0644(4) 0.0719(19) Uani 1 1 d U . . H89 H 0.2011 0.7092 0.0682 0.086 Uiso 1 1 calc R . . C90 C 0.3039(4) 0.5957(5) 0.0687(4) 0.0670(18) Uani 1 1 d U . . H90 H 0.2668 0.5619 0.0740 0.080 Uiso 1 1 calc R . . C91 C 0.3993(5) 0.5578(5) 0.0649(4) 0.0712(19) Uani 1 1 d U . . H91 H 0.4264 0.4977 0.0671 0.085 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 0.02183(8) 0.02135(8) 0.02086(9) -0.00273(6) -0.00319(6) -0.00818(6) U2 0.02360(9) 0.02248(8) 0.02143(9) -0.00425(6) -0.00229(6) -0.00781(6) O1 0.0216(14) 0.0245(15) 0.0187(14) -0.0016(12) 0.0005(11) -0.0116(12) O2 0.0231(14) 0.0207(14) 0.0309(16) -0.0046(12) -0.0026(12) -0.0087(12) O3 0.0226(14) 0.0277(15) 0.0203(15) -0.0044(12) -0.0022(11) -0.0082(12) O4 0.0231(15) 0.0257(15) 0.0354(17) -0.0080(13) -0.0056(12) -0.0086(12) O5 0.0277(15) 0.0240(15) 0.0256(16) -0.0076(12) -0.0027(12) -0.0079(12) O6 0.0259(15) 0.0296(16) 0.0265(16) -0.0091(13) -0.0004(12) -0.0075(13) O7 0.0317(16) 0.0367(17) 0.0249(16) 0.0045(13) -0.0051(13) -0.0132(14) O8 0.0291(15) 0.0318(16) 0.0218(15) -0.0022(13) -0.0080(12) -0.0113(13) O9 0.0303(16) 0.0253(15) 0.0239(16) -0.0022(12) -0.0014(12) -0.0102(13) O10 0.0256(15) 0.0240(15) 0.0246(15) -0.0052(12) -0.0051(12) -0.0064(12) O11 0.0351(17) 0.0256(15) 0.0315(17) -0.0016(13) -0.0072(13) -0.0144(13) O12 0.0261(15) 0.0246(15) 0.0324(17) -0.0020(13) -0.0064(13) -0.0050(12) O13 0.0261(16) 0.0329(17) 0.0308(17) -0.0100(14) 0.0059(13) -0.0086(13) O14 0.0367(17) 0.0290(16) 0.0251(16) -0.0096(13) -0.0040(13) -0.0078(13) N1 0.0187(16) 0.0232(17) 0.0206(17) -0.0069(14) -0.0031(13) -0.0055(14) N2 0.0208(17) 0.0215(17) 0.0243(18) -0.0033(14) -0.0023(14) -0.0064(14) N3 0.0256(18) 0.0239(18) 0.0197(18) -0.0028(14) -0.0016(14) -0.0087(14) N4 0.0209(17) 0.0235(17) 0.0263(19) -0.0042(14) -0.0027(14) -0.0076(14) N5 0.036(2) 0.068(3) 0.055(3) -0.011(2) -0.007(2) -0.023(2) N6 0.050(3) 0.105(5) 0.070(4) 0.002(3) -0.021(3) -0.030(3) C1 0.023(2) 0.026(2) 0.024(2) -0.0050(17) -0.0027(16) -0.0089(17) C2 0.025(2) 0.020(2) 0.022(2) -0.0061(17) -0.0001(16) -0.0080(16) C3 0.022(2) 0.023(2) 0.023(2) -0.0065(17) -0.0005(16) -0.0101(16) C4 0.024(2) 0.023(2) 0.021(2) -0.0043(17) -0.0039(16) -0.0073(17) C5 0.028(2) 0.024(2) 0.021(2) -0.0056(17) -0.0015(17) -0.0095(17) C6 0.023(2) 0.024(2) 0.030(2) -0.0063(18) -0.0017(17) -0.0106(17) C7 0.032(2) 0.025(2) 0.031(2) 0.0023(18) -0.0060(18) -0.0141(18) C8 0.045(3) 0.038(3) 0.029(3) 0.002(2) -0.007(2) -0.020(2) C9 0.035(2) 0.034(2) 0.036(3) 0.002(2) -0.006(2) -0.019(2) C10 0.034(2) 0.028(2) 0.043(3) 0.002(2) -0.008(2) -0.011(2) C11 0.024(2) 0.022(2) 0.019(2) -0.0029(16) -0.0039(16) -0.0069(16) C12 0.021(2) 0.024(2) 0.021(2) -0.0084(17) 0.0002(16) -0.0060(16) C13 0.022(2) 0.027(2) 0.019(2) -0.0042(17) -0.0040(16) -0.0073(17) C14 0.025(2) 0.026(2) 0.027(2) -0.0062(18) -0.0032(17) -0.0100(17) C15 0.021(2) 0.027(2) 0.035(2) -0.0094(19) 0.0010(18) -0.0084(17) C16 0.021(2) 0.025(2) 0.028(2) -0.0035(18) -0.0059(17) -0.0030(17) C17 0.025(2) 0.023(2) 0.023(2) -0.0051(17) -0.0019(17) -0.0088(17) C18 0.019(2) 0.025(2) 0.027(2) -0.0042(17) -0.0010(16) -0.0087(17) C19 0.020(2) 0.026(2) 0.027(2) -0.0049(17) -0.0027(16) -0.0076(17) C20 0.026(2) 0.022(2) 0.021(2) -0.0030(16) -0.0013(16) -0.0091(17) C21 0.022(2) 0.024(2) 0.020(2) -0.0035(17) -0.0026(16) -0.0060(17) C22 0.025(2) 0.024(2) 0.023(2) -0.0013(17) -0.0051(17) -0.0046(17) C23 0.026(2) 0.025(2) 0.028(2) -0.0043(18) -0.0012(17) -0.0094(18) C24 0.026(2) 0.026(2) 0.029(2) -0.0049(18) -0.0038(17) -0.0123(18) C25 0.032(2) 0.024(2) 0.048(3) 0.000(2) -0.006(2) -0.0131(19) C26 0.043(3) 0.027(2) 0.070(4) 0.007(2) -0.015(3) -0.016(2) C27 0.054(3) 0.039(3) 0.050(3) -0.002(2) 0.009(3) -0.028(3) C28 0.042(3) 0.027(2) 0.059(3) -0.007(2) -0.011(2) -0.016(2) C29 0.020(2) 0.0174(19) 0.027(2) -0.0031(16) -0.0012(16) -0.0035(16) C30 0.023(2) 0.020(2) 0.023(2) -0.0043(17) -0.0046(16) -0.0053(16) C31 0.0216(19) 0.023(2) 0.024(2) -0.0067(17) 0.0006(16) -0.0078(16) C32 0.023(2) 0.021(2) 0.028(2) -0.0061(17) -0.0048(17) -0.0076(16) C33 0.025(2) 0.024(2) 0.028(2) -0.0063(18) -0.0041(17) -0.0063(17) C34 0.022(2) 0.024(2) 0.025(2) -0.0024(17) -0.0003(17) -0.0061(17) C35 0.026(2) 0.030(2) 0.023(2) -0.0038(18) -0.0053(17) -0.0093(18) C36 0.049(3) 0.033(3) 0.031(3) -0.002(2) -0.015(2) -0.007(2) C37 0.040(3) 0.044(3) 0.023(2) -0.002(2) -0.0096(19) -0.018(2) C38 0.038(3) 0.043(3) 0.026(2) -0.007(2) -0.003(2) -0.015(2) C39 0.0180(19) 0.0192(19) 0.029(2) -0.0034(17) -0.0043(16) -0.0045(16) C40 0.024(2) 0.020(2) 0.031(2) -0.0021(17) -0.0008(17) -0.0061(17) C41 0.022(2) 0.027(2) 0.029(2) -0.0031(18) -0.0028(17) -0.0090(17) C42 0.026(2) 0.031(2) 0.042(3) -0.006(2) -0.0008(19) -0.0136(19) C43 0.035(3) 0.038(3) 0.050(3) -0.005(2) 0.001(2) -0.023(2) C44 0.034(3) 0.042(3) 0.033(3) -0.002(2) 0.006(2) -0.017(2) C45 0.026(2) 0.030(2) 0.035(3) -0.0056(19) -0.0011(19) -0.0100(19) C46 0.026(2) 0.025(2) 0.024(2) -0.0044(17) -0.0087(17) -0.0098(17) C47 0.020(2) 0.023(2) 0.025(2) -0.0059(17) 0.0003(16) -0.0060(16) C48 0.022(2) 0.023(2) 0.028(2) -0.0051(17) -0.0034(17) -0.0081(17) C49 0.0186(19) 0.028(2) 0.024(2) -0.0021(17) -0.0009(16) -0.0099(17) C50 0.024(2) 0.023(2) 0.027(2) -0.0019(17) -0.0022(17) -0.0077(17) C51 0.021(2) 0.027(2) 0.024(2) -0.0068(17) -0.0017(16) -0.0090(17) C52 0.0187(19) 0.026(2) 0.023(2) -0.0028(17) -0.0030(16) -0.0060(16) C53 0.024(2) 0.027(2) 0.029(2) -0.0060(18) -0.0063(17) -0.0080(17) C54 0.030(2) 0.032(2) 0.035(3) -0.006(2) -0.0012(19) -0.0167(19) C55 0.028(2) 0.031(2) 0.040(3) -0.012(2) -0.0002(19) -0.0109(19) C56 0.030(2) 0.029(2) 0.039(3) -0.009(2) -0.0107(19) -0.0112(19) C57 0.039(3) 0.029(2) 0.033(3) -0.006(2) -0.005(2) -0.014(2) C58 0.036(2) 0.024(2) 0.023(2) -0.0090(17) -0.0048(18) -0.0094(19) C59 0.030(2) 0.022(2) 0.031(2) -0.0051(18) -0.0062(18) -0.0062(18) C60 0.025(2) 0.032(2) 0.025(2) -0.0122(19) -0.0038(17) -0.0049(18) C61 0.027(2) 0.040(3) 0.042(3) -0.017(2) -0.002(2) -0.009(2) C62 0.050(3) 0.073(4) 0.039(3) 0.018(3) -0.009(3) -0.031(3) C63 0.037(3) 0.034(3) 0.031(3) 0.002(2) -0.003(2) -0.011(2) C64 0.030(2) 0.049(3) 0.026(2) 0.003(2) -0.0083(19) -0.008(2) C65 0.027(2) 0.033(2) 0.028(2) -0.0087(19) -0.0049(18) -0.0069(19) C66 0.027(2) 0.051(3) 0.027(2) -0.008(2) -0.0066(19) -0.008(2) C67 0.040(3) 0.030(2) 0.032(3) -0.004(2) 0.000(2) -0.017(2) C68 0.041(3) 0.027(2) 0.018(2) -0.0003(17) -0.0077(18) -0.015(2) C69 0.030(2) 0.026(2) 0.028(2) -0.0081(18) -0.0022(18) -0.0075(18) C70 0.025(2) 0.026(2) 0.019(2) -0.0048(17) -0.0034(16) -0.0048(17) C71 0.034(2) 0.030(2) 0.030(2) -0.0064(19) -0.0033(19) -0.009(2) C72 0.044(3) 0.036(3) 0.054(3) 0.007(2) -0.016(2) -0.021(2) C73 0.030(2) 0.024(2) 0.033(2) -0.0059(19) -0.0001(18) -0.0110(18) C74 0.037(3) 0.031(2) 0.026(2) -0.0021(19) -0.0045(19) -0.012(2) C75 0.035(2) 0.023(2) 0.024(2) -0.0036(18) -0.0056(18) -0.0075(18) C76 0.042(3) 0.037(3) 0.035(3) 0.000(2) -0.012(2) -0.014(2) C77 0.040(3) 0.044(3) 0.041(3) -0.011(2) 0.008(2) -0.012(2) C78 0.038(3) 0.026(2) 0.030(2) -0.0029(19) 0.006(2) -0.011(2) C79 0.047(3) 0.038(3) 0.029(3) -0.013(2) 0.006(2) -0.011(2) C80 0.052(3) 0.022(2) 0.023(2) -0.0020(18) -0.005(2) -0.010(2) C81 0.056(3) 0.043(3) 0.038(3) -0.021(2) -0.011(2) -0.003(2) C82 0.030(3) 0.060(3) 0.050(3) -0.008(3) 0.002(2) -0.020(2) C83 0.037(3) 0.053(3) 0.042(3) -0.011(3) -0.003(2) -0.006(2) C84 0.026(2) 0.036(3) 0.057(3) -0.015(2) -0.006(2) -0.004(2) C85 0.032(3) 0.041(3) 0.052(3) -0.008(2) 0.003(2) -0.011(2) C86 0.035(3) 0.059(3) 0.040(3) -0.010(3) -0.001(2) -0.011(2) C87 0.067(3) 0.083(4) 0.088(4) -0.039(3) -0.016(3) -0.031(3) C88 0.103(4) 0.100(4) 0.106(5) -0.056(4) -0.013(4) -0.025(4) C89 0.056(3) 0.098(4) 0.060(3) -0.034(3) 0.002(3) -0.018(3) C90 0.054(3) 0.089(4) 0.055(3) 0.013(3) -0.007(3) -0.035(3) C91 0.057(3) 0.073(4) 0.072(4) 0.017(3) -0.013(3) -0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 2.196(3) . ? U1 O1 2.265(2) . ? U1 O8 2.331(3) . ? U1 O7 2.335(3) . ? U1 O5 2.377(3) . ? U1 O6 2.386(3) . ? U1 N2 2.611(3) . ? U1 N1 2.618(3) . ? U1 U2 6.8795(3) . ? U2 O3 2.205(3) . ? U2 O9 2.317(3) . ? U2 O11 2.351(3) . ? U2 O10 2.363(3) . ? U2 O14 2.373(3) . ? U2 O13 2.383(3) . ? U2 O12 2.403(3) . ? U2 N3 2.576(3) . ? O1 C2 1.323(5) . ? O1 O4 2.615(4) . ? O1 N1 2.807(4) . ? O1 O2 3.074(4) . ? O2 C20 1.321(5) . ? O2 N2 2.761(4) . ? O2 O3 3.140(4) . ? O3 C30 1.323(5) . ? O3 N3 2.807(4) . ? O3 O4 3.480(4) . ? O4 C48 1.364(5) . ? O4 N4 2.759(4) . ? O5 C58 1.267(5) . ? O6 C60 1.270(5) . ? O7 C63 1.288(6) . ? O8 C65 1.270(5) . ? O9 C68 1.293(5) . ? O10 C70 1.268(5) . ? O11 C73 1.260(5) . ? O12 C75 1.269(5) . ? O13 C78 1.275(5) . ? O14 C80 1.280(5) . ? N1 C11 1.292(5) . ? N1 C12 1.425(5) . ? N1 N2 2.664(5) . ? N2 C18 1.304(5) . ? N2 C13 1.431(5) . ? N3 C39 1.326(5) . ? N3 C40 1.412(5) . ? N4 C39 1.374(5) . ? N4 C41 1.386(5) . ? N4 C46 1.470(5) . ? N5 C82 1.329(7) . ? N5 C86 1.342(7) . ? N6 C87 1.298(9) . ? N6 C91 1.347(8) . ? C1 C6 1.404(6) . ? C1 C2 1.411(6) . ? C1 C49 1.500(6) . ? C2 C3 1.424(6) . ? C3 C4 1.400(6) . ? C3 C11 1.444(5) . ? C4 C5 1.390(6) . ? C5 C6 1.390(6) . ? C5 C7 1.540(6) . ? C7 C8 1.535(6) . ? C7 C10 1.539(6) . ? C7 C9 1.541(6) . ? C12 C13 1.399(6) . ? C12 C17 1.400(6) . ? C13 C14 1.402(6) . ? C14 C15 1.379(6) . ? C15 C16 1.389(6) . ? C16 C17 1.380(6) . ? C18 C19 1.438(6) . ? C19 C24 1.405(6) . ? C19 C20 1.424(6) . ? C20 C21 1.416(6) . ? C21 C22 1.384(6) . ? C21 C29 1.489(6) . ? C22 C23 1.408(6) . ? C23 C24 1.383(6) . ? C23 C25 1.535(6) . ? C25 C26 1.526(6) . ? C25 C28 1.534(7) . ? C25 C27 1.550(6) . ? C29 C34 1.392(6) . ? C29 C30 1.419(6) . ? C30 C31 1.404(6) . ? C31 C32 1.408(6) . ? C31 C39 1.471(5) . ? C32 C33 1.388(6) . ? C33 C34 1.406(6) . ? C33 C35 1.526(6) . ? C35 C38 1.536(6) . ? C35 C36 1.538(6) . ? C35 C37 1.544(6) . ? C40 C45 1.391(6) . ? C40 C41 1.396(6) . ? C41 C42 1.399(6) . ? C42 C43 1.382(7) . ? C43 C44 1.405(7) . ? C44 C45 1.389(6) . ? C46 C47 1.512(5) . ? C47 C48 1.398(6) . ? C47 C52 1.399(6) . ? C48 C49 1.405(6) . ? C49 C50 1.391(6) . ? C50 C51 1.389(6) . ? C51 C52 1.401(6) . ? C51 C53 1.532(6) . ? C53 C56 1.534(6) . ? C53 C54 1.535(6) . ? C53 C55 1.549(6) . ? C57 C58 1.502(6) . ? C58 C59 1.408(6) . ? C59 C60 1.395(6) . ? C60 C61 1.505(6) . ? C62 C63 1.495(7) . ? C63 C64 1.384(7) . ? C64 C65 1.389(6) . ? C65 C66 1.506(6) . ? C67 C68 1.497(6) . ? C68 C69 1.381(6) . ? C69 C70 1.414(6) . ? C70 C71 1.498(6) . ? C72 C73 1.501(6) . ? C73 C74 1.401(6) . ? C74 C75 1.397(6) . ? C75 C76 1.510(6) . ? C77 C78 1.505(6) . ? C78 C79 1.393(7) . ? C79 C80 1.390(7) . ? C80 C81 1.503(7) . ? C82 C83 1.374(8) . ? C83 C84 1.387(7) . ? C84 C85 1.372(7) . ? C85 C86 1.384(7) . ? C87 C88 1.371(10) . ? C88 C89 1.411(11) . ? C89 C90 1.332(10) . ? C90 C91 1.373(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O1 87.09(10) . . ? O2 U1 O8 88.23(10) . . ? O1 U1 O8 80.77(10) . . ? O2 U1 O7 81.61(11) . . ? O1 U1 O7 150.73(10) . . ? O8 U1 O7 72.02(10) . . ? O2 U1 O5 156.32(10) . . ? O1 U1 O5 72.88(9) . . ? O8 U1 O5 76.43(10) . . ? O7 U1 O5 109.82(10) . . ? O2 U1 O6 134.18(10) . . ? O1 U1 O6 131.55(10) . . ? O8 U1 O6 117.53(10) . . ? O7 U1 O6 72.75(10) . . ? O5 U1 O6 69.48(10) . . ? O2 U1 N2 69.50(10) . . ? O1 U1 N2 112.94(10) . . ? O8 U1 N2 152.38(10) . . ? O7 U1 N2 88.23(11) . . ? O5 U1 N2 129.67(10) . . ? O6 U1 N2 72.32(10) . . ? O2 U1 N1 108.37(10) . . ? O1 U1 N1 69.75(10) . . ? O8 U1 N1 144.84(10) . . ? O7 U1 N1 139.49(10) . . ? O5 U1 N1 76.89(10) . . ? O6 U1 N1 72.87(10) . . ? N2 U1 N1 61.24(10) . . ? O3 U2 O9 99.11(10) . . ? O3 U2 O11 86.68(10) . . ? O9 U2 O11 147.42(10) . . ? O3 U2 O10 72.76(10) . . ? O9 U2 O10 70.92(10) . . ? O11 U2 O10 80.50(10) . . ? O3 U2 O14 145.78(10) . . ? O9 U2 O14 84.56(10) . . ? O11 U2 O14 73.62(10) . . ? O10 U2 O14 76.51(10) . . ? O3 U2 O13 144.32(10) . . ? O9 U2 O13 84.70(10) . . ? O11 U2 O13 109.06(10) . . ? O10 U2 O13 139.91(10) . . ? O14 U2 O13 69.74(10) . . ? O3 U2 O12 81.01(10) . . ? O9 U2 O12 142.32(10) . . ? O11 U2 O12 70.18(10) . . ? O10 U2 O12 141.53(10) . . ? O14 U2 O12 116.32(10) . . ? O13 U2 O12 75.11(10) . . ? O3 U2 N3 71.43(10) . . ? O9 U2 N3 71.22(10) . . ? O11 U2 N3 139.76(10) . . ? O10 U2 N3 121.71(10) . . ? O14 U2 N3 139.92(10) . . ? O13 U2 N3 76.47(10) . . ? O12 U2 N3 73.27(10) . . ? C2 O1 U1 134.6(2) . . ? C20 O2 U1 140.5(2) . . ? C30 O3 U2 134.0(2) . . ? C58 O5 U1 134.9(3) . . ? C60 O6 U1 134.3(3) . . ? C63 O7 U1 137.1(3) . . ? C65 O8 U1 138.0(3) . . ? C68 O9 U2 131.9(3) . . ? C70 O10 U2 129.0(3) . . ? C73 O11 U2 136.7(3) . . ? C75 O12 U2 133.7(3) . . ? C78 O13 U2 138.9(3) . . ? C80 O14 U2 138.6(3) . . ? C11 N1 C12 117.4(3) . . ? C11 N1 U1 128.0(3) . . ? C12 N1 U1 114.4(2) . . ? C18 N2 C13 117.7(3) . . ? C18 N2 U1 127.4(3) . . ? C13 N2 U1 114.9(2) . . ? C39 N3 C40 105.1(3) . . ? C39 N3 U2 124.2(3) . . ? C40 N3 U2 127.8(3) . . ? C39 N4 C41 106.4(3) . . ? C39 N4 C46 126.2(3) . . ? C41 N4 C46 122.6(3) . . ? C82 N5 C86 116.4(5) . . ? C87 N6 C91 119.2(6) . . ? C6 C1 C2 118.7(4) . . ? C6 C1 C49 117.2(4) . . ? C2 C1 C49 124.0(4) . . ? O1 C2 C1 121.8(4) . . ? O1 C2 C3 120.2(3) . . ? C1 C2 C3 118.0(4) . . ? C4 C3 C2 120.4(4) . . ? C4 C3 C11 115.8(4) . . ? C2 C3 C11 123.7(4) . . ? C5 C4 C3 122.0(4) . . ? C6 C5 C4 116.7(4) . . ? C6 C5 C7 123.3(4) . . ? C4 C5 C7 120.0(4) . . ? C5 C6 C1 123.9(4) . . ? C8 C7 C10 109.3(4) . . ? C8 C7 C9 108.6(4) . . ? C10 C7 C9 108.7(4) . . ? C8 C7 C5 109.9(4) . . ? C10 C7 C5 108.7(4) . . ? C9 C7 C5 111.6(4) . . ? N1 C11 C3 126.1(4) . . ? C13 C12 C17 119.3(4) . . ? C13 C12 N1 117.1(3) . . ? C17 C12 N1 123.5(4) . . ? C12 C13 C14 119.8(4) . . ? C12 C13 N2 115.5(3) . . ? C14 C13 N2 124.7(4) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 120.1(4) . . ? C17 C16 C15 120.5(4) . . ? C16 C17 C12 120.1(4) . . ? N2 C18 C19 126.2(4) . . ? C24 C19 C20 120.1(4) . . ? C24 C19 C18 117.1(4) . . ? C20 C19 C18 122.8(4) . . ? O2 C20 C21 121.4(4) . . ? O2 C20 C19 120.8(4) . . ? C21 C20 C19 117.8(4) . . ? C22 C21 C20 119.4(4) . . ? C22 C21 C29 121.2(4) . . ? C20 C21 C29 119.1(4) . . ? C21 C22 C23 123.7(4) . . ? C24 C23 C22 116.2(4) . . ? C24 C23 C25 120.3(4) . . ? C22 C23 C25 123.4(4) . . ? C23 C24 C19 122.5(4) . . ? C26 C25 C28 108.9(4) . . ? C26 C25 C23 112.8(4) . . ? C28 C25 C23 111.3(4) . . ? C26 C25 C27 108.0(4) . . ? C28 C25 C27 107.9(4) . . ? C23 C25 C27 107.8(4) . . ? C34 C29 C30 119.2(4) . . ? C34 C29 C21 119.5(4) . . ? C30 C29 C21 121.2(4) . . ? O3 C30 C31 121.3(4) . . ? O3 C30 C29 120.4(4) . . ? C31 C30 C29 118.3(4) . . ? C30 C31 C32 120.1(4) . . ? C30 C31 C39 119.5(4) . . ? C32 C31 C39 120.4(4) . . ? C33 C32 C31 122.3(4) . . ? C32 C33 C34 116.4(4) . . ? C32 C33 C35 122.9(4) . . ? C34 C33 C35 120.5(4) . . ? C29 C34 C33 123.2(4) . . ? C33 C35 C38 111.1(3) . . ? C33 C35 C36 108.7(3) . . ? C38 C35 C36 108.3(4) . . ? C33 C35 C37 112.2(4) . . ? C38 C35 C37 107.6(4) . . ? C36 C35 C37 109.0(4) . . ? N3 C39 N4 112.9(4) . . ? N3 C39 C31 125.4(4) . . ? N4 C39 C31 121.6(4) . . ? C45 C40 C41 120.1(4) . . ? C45 C40 N3 131.1(4) . . ? C41 C40 N3 108.9(4) . . ? N4 C41 C40 106.7(4) . . ? N4 C41 C42 130.4(4) . . ? C40 C41 C42 122.9(4) . . ? C43 C42 C41 116.3(4) . . ? C42 C43 C44 121.5(4) . . ? C45 C44 C43 121.6(4) . . ? C44 C45 C40 117.7(4) . . ? N4 C46 C47 113.9(3) . . ? C48 C47 C52 120.1(4) . . ? C48 C47 C46 120.5(4) . . ? C52 C47 C46 119.4(4) . . ? O4 C48 C47 117.1(4) . . ? O4 C48 C49 122.9(4) . . ? C47 C48 C49 120.0(4) . . ? C50 C49 C48 117.9(4) . . ? C50 C49 C1 117.2(4) . . ? C48 C49 C1 124.9(4) . . ? C51 C50 C49 123.9(4) . . ? C50 C51 C52 116.9(4) . . ? C50 C51 C53 119.7(4) . . ? C52 C51 C53 123.3(4) . . ? C47 C52 C51 121.2(4) . . ? C51 C53 C56 112.5(3) . . ? C51 C53 C54 108.4(3) . . ? C56 C53 C54 109.0(4) . . ? C51 C53 C55 110.5(3) . . ? C56 C53 C55 107.8(4) . . ? C54 C53 C55 108.5(4) . . ? O5 C58 C59 123.1(4) . . ? O5 C58 C57 116.6(4) . . ? C59 C58 C57 120.3(4) . . ? C60 C59 C58 123.1(4) . . ? O6 C60 C59 124.7(4) . . ? O6 C60 C61 115.3(4) . . ? C59 C60 C61 120.0(4) . . ? O7 C63 C64 124.1(4) . . ? O7 C63 C62 115.8(4) . . ? C64 C63 C62 120.1(5) . . ? C63 C64 C65 124.9(4) . . ? O8 C65 C64 123.8(4) . . ? O8 C65 C66 117.3(4) . . ? C64 C65 C66 118.9(4) . . ? O9 C68 C69 123.4(4) . . ? O9 C68 C67 116.0(4) . . ? C69 C68 C67 120.6(4) . . ? C68 C69 C70 123.8(4) . . ? O10 C70 C69 123.8(4) . . ? O10 C70 C71 116.7(4) . . ? C69 C70 C71 119.5(4) . . ? O11 C73 C74 124.7(4) . . ? O11 C73 C72 115.5(4) . . ? C74 C73 C72 119.8(4) . . ? C75 C74 C73 122.9(4) . . ? O12 C75 C74 124.6(4) . . ? O12 C75 C76 116.2(4) . . ? C74 C75 C76 119.2(4) . . ? O13 C78 C79 123.8(4) . . ? O13 C78 C77 116.1(4) . . ? C79 C78 C77 120.1(4) . . ? C80 C79 C78 124.0(4) . . ? O14 C80 C79 123.8(4) . . ? O14 C80 C81 115.2(4) . . ? C79 C80 C81 121.0(4) . . ? N5 C82 C83 124.3(5) . . ? C82 C83 C84 118.7(5) . . ? C85 C84 C83 118.1(5) . . ? C84 C85 C86 119.2(5) . . ? N5 C86 C85 123.3(5) . . ? N6 C87 C88 121.9(7) . . ? C87 C88 C89 118.4(8) . . ? C90 C89 C88 119.4(7) . . ? C89 C90 C91 118.5(7) . . ? N6 C91 C90 122.4(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O1 0.91 1.75 2.615(4) 157.4 .