Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M. Ephritikhine' _publ_contact_author_address ; CEA/Saclay, DSM/DRECAM/SCM (CNRS URA 331) Batiment 125 91191 Gif-sur-Yvette France ; _publ_contact_author_phone '33 1 69 08 64 36' _publ_contact_author_fax '33 1 69 08 66 40' _publ_contact_author_email ephri@drecam.cea.fr _publ_section_title ; Synthesis and crystal structure of uranium(IV) complexes with calix[n]arenes (n = 4, 6 and 8): mononuclear, polynuclear and 1D polymeric species ; loop_ _publ_author_name _publ_author_address L.Salmon ; CEA/Saclay, DSM/DRECAM/SCM (CNRS URA 331) Batiment 125 91191 Gif-sur-Yvette France ; P.Thuery ; CEA/Saclay, DSM/DRECAM/SCM (CNRS URA 331) Batiment 125 91191 Gif-sur-Yvette France ; M.Ephritikhine ; CEA/Saclay, DSM/DRECAM/SCM (CNRS URA 331) Batiment 125 91191 Gif-sur-Yvette France ; # # The CIFs relative to the three compounds reported in the # preliminary communication [Chem. Comm., 2006, 856] have # been deposited with CCDC numbers 290602-290604. # data_4.py _database_code_depnum_ccdc_archive 'CCDC 603334' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H38 Cl3 N3 O4 U' _chemical_formula_weight 1005.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '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 11.8531(2) _cell_length_b 18.9402(4) _cell_length_c 17.8786(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.0440(10) _cell_angle_gamma 90.00 _cell_volume 3939.41(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 76916 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method ? _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 4.370 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.229 _exptl_absorpt_correction_T_max 0.705 _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 one \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 76916 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7390 _reflns_number_gt 6593 _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 bound to N and O were found on a Fourier-difference map and all the other ones were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. The highest residual electron density peak is located near atom C36, in a pyridine molecule which is seemingly slightly disordered. 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^)+(0.0468P)^2^+9.4511P] 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 7390 _refine_ls_number_parameters 487 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.215 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.129 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 0.020731(13) 0.204205(9) 0.866022(9) 0.01590(7) Uani 1 1 d . . . Cl1 Cl -0.16687(9) 0.16592(7) 0.75511(6) 0.0234(2) Uani 1 1 d . . . Cl2 Cl -0.09174(10) 0.11889(7) 0.95351(7) 0.0249(2) Uani 1 1 d . . . Cl3 Cl -0.13697(10) 0.30038(6) 0.89792(8) 0.0267(3) Uani 1 1 d . . . O1 O 0.1055(3) 0.23829(17) 0.77697(18) 0.0198(7) Uani 1 1 d . . . O2 O 0.0713(3) 0.09586(16) 0.82777(18) 0.0187(7) Uani 1 1 d . . . O3 O 0.1660(3) 0.18462(17) 0.95394(18) 0.0203(7) Uani 1 1 d . . . O4 O 0.1193(3) 0.32393(17) 0.91049(19) 0.0205(7) Uani 1 1 d . . . H4 H 0.0878 0.3693 0.9015 0.025 Uiso 1 1 d R . . C1 C 0.2171(4) 0.3174(3) 0.7188(3) 0.0229(10) Uani 1 1 d . . . C2 C 0.1703(4) 0.2503(3) 0.7238(3) 0.0200(10) Uani 1 1 d . . . C3 C 0.1860(4) 0.1958(3) 0.6738(3) 0.0227(10) Uani 1 1 d . . . C4 C 0.2498(4) 0.2104(3) 0.6175(3) 0.0270(11) Uani 1 1 d . . . H4A H 0.2603 0.1750 0.5834 0.032 Uiso 1 1 calc R . . C5 C 0.2983(5) 0.2769(3) 0.6112(3) 0.0331(13) Uani 1 1 d . . . H5 H 0.3415 0.2856 0.5739 0.040 Uiso 1 1 calc R . . C6 C 0.2807(4) 0.3303(3) 0.6621(3) 0.0295(12) Uani 1 1 d . . . H6 H 0.3117 0.3749 0.6580 0.035 Uiso 1 1 calc R . . C7 C 0.1424(4) 0.1227(3) 0.6844(3) 0.0236(10) Uani 1 1 d . . . H7A H 0.1426 0.0951 0.6387 0.028 Uiso 1 1 calc R . . H7B H 0.0639 0.1254 0.6924 0.028 Uiso 1 1 calc R . . C8 C 0.2174(4) 0.0861(2) 0.7527(3) 0.0188(9) Uani 1 1 d . . . C9 C 0.1800(4) 0.0762(2) 0.8216(3) 0.0188(9) Uani 1 1 d . . . C10 C 0.2534(4) 0.0456(2) 0.8849(3) 0.0187(9) Uani 1 1 d . . . C11 C 0.3623(4) 0.0238(2) 0.8769(3) 0.0214(10) Uani 1 1 d . . . H11 H 0.4103 0.0023 0.9178 0.026 Uiso 1 1 calc R . . C12 C 0.4009(4) 0.0335(3) 0.8089(3) 0.0235(10) Uani 1 1 d . . . H12 H 0.4746 0.0197 0.8046 0.028 Uiso 1 1 calc R . . C13 C 0.3269(4) 0.0645(3) 0.7472(3) 0.0230(10) Uani 1 1 d . . . H13 H 0.3520 0.0707 0.7014 0.028 Uiso 1 1 calc R . . C14 C 0.2166(4) 0.0389(2) 0.9615(3) 0.0200(10) Uani 1 1 d . . . H14A H 0.1343 0.0463 0.9546 0.024 Uiso 1 1 calc R . . H14B H 0.2329 -0.0086 0.9809 0.024 Uiso 1 1 calc R . . C15 C 0.2777(4) 0.0913(3) 1.0192(3) 0.0205(10) Uani 1 1 d . . . C16 C 0.2491(4) 0.1632(3) 1.0116(3) 0.0189(9) Uani 1 1 d . . . C17 C 0.3043(4) 0.2134(3) 1.0633(3) 0.0233(10) Uani 1 1 d . . . C18 C 0.3897(4) 0.1910(3) 1.1228(3) 0.0253(11) Uani 1 1 d . . . H18 H 0.4276 0.2238 1.1574 0.030 Uiso 1 1 calc R . . C19 C 0.4195(5) 0.1200(3) 1.1313(3) 0.0301(12) Uani 1 1 d . . . H19 H 0.4776 0.1057 1.1710 0.036 Uiso 1 1 calc R . . C20 C 0.3623(4) 0.0708(3) 1.0804(3) 0.0253(11) Uani 1 1 d . . . H20 H 0.3808 0.0232 1.0873 0.030 Uiso 1 1 calc R . . C21 C 0.2696(5) 0.2901(2) 1.0528(3) 0.0241(11) Uani 1 1 d . . . H21A H 0.3014 0.3161 1.0988 0.029 Uiso 1 1 calc R . . H21B H 0.1865 0.2937 1.0449 0.029 Uiso 1 1 calc R . . C22 C 0.3111(4) 0.3233(3) 0.9856(3) 0.0225(10) Uani 1 1 d . . . C23 C 0.2373(4) 0.3370(2) 0.9157(3) 0.0212(10) Uani 1 1 d . . . C24 C 0.2779(4) 0.3641(3) 0.8530(3) 0.0252(11) Uani 1 1 d . . . C25 C 0.3946(5) 0.3802(3) 0.8625(3) 0.0334(12) Uani 1 1 d . . . H25 H 0.4233 0.3984 0.8216 0.040 Uiso 1 1 calc R . . C26 C 0.4684(4) 0.3694(3) 0.9316(3) 0.0336(13) Uani 1 1 d . . . H26 H 0.5457 0.3814 0.9371 0.040 Uiso 1 1 calc R . . C27 C 0.4272(4) 0.3410(3) 0.9924(3) 0.0311(12) Uani 1 1 d . . . H27 H 0.4775 0.3335 1.0385 0.037 Uiso 1 1 calc R . . C28 C 0.2012(4) 0.3739(3) 0.7756(3) 0.0249(11) Uani 1 1 d . . . H28A H 0.1216 0.3739 0.7816 0.030 Uiso 1 1 calc R . . H28B H 0.2171 0.4196 0.7554 0.030 Uiso 1 1 calc R . . N1 N -0.0558(3) -0.0154(2) 0.8091(2) 0.0257(9) Uani 1 1 d . . . H1 H -0.0192 0.0293 0.8129 0.031 Uiso 1 1 d R . . C29 C -0.0494(4) -0.0644(3) 0.8630(3) 0.0286(11) Uani 1 1 d . . . H29 H -0.0070 -0.0555 0.9115 0.034 Uiso 1 1 calc R . . C30 C -0.1048(5) -0.1281(3) 0.8480(3) 0.0330(12) Uani 1 1 d . . . H30 H -0.0993 -0.1626 0.8855 0.040 Uiso 1 1 calc R . . C31 C -0.1693(4) -0.1397(3) 0.7754(4) 0.0343(13) Uani 1 1 d . . . H31 H -0.2100 -0.1816 0.7643 0.041 Uiso 1 1 calc R . . C32 C -0.1725(4) -0.0883(3) 0.7198(3) 0.0347(13) Uani 1 1 d . . . H32 H -0.2133 -0.0960 0.6706 0.042 Uiso 1 1 calc R . . C33 C -0.1144(5) -0.0258(3) 0.7383(3) 0.0323(12) Uani 1 1 d . . . H33 H -0.1159 0.0091 0.7016 0.039 Uiso 1 1 calc R . . N2 N 0.0441(4) 0.4562(2) 0.8933(3) 0.0276(9) Uani 1 1 d . . . C34 C 0.1068(6) 0.4993(3) 0.9446(3) 0.0400(14) Uani 1 1 d . . . H34 H 0.1718 0.4809 0.9759 0.048 Uiso 1 1 calc R . . C35 C 0.0809(7) 0.5682(4) 0.9534(5) 0.0612(19) Uani 1 1 d U . . H35 H 0.1265 0.5959 0.9902 0.073 Uiso 1 1 calc R . . C36 C -0.0092(7) 0.5946(4) 0.9091(5) 0.065(2) Uani 1 1 d U . . H36 H -0.0274 0.6418 0.9147 0.077 Uiso 1 1 calc R . . C37 C -0.0796(6) 0.5542(4) 0.8531(5) 0.063(2) Uani 1 1 d U . . H37 H -0.1441 0.5733 0.8217 0.076 Uiso 1 1 calc R . . C38 C -0.0472(5) 0.4826(3) 0.8470(4) 0.0407(15) Uani 1 1 d . . . H38 H -0.0904 0.4538 0.8102 0.049 Uiso 1 1 calc R . . N3 N 0.6513(3) 0.1737(2) 0.8705(3) 0.0293(10) Uani 1 1 d . . . H3 H 0.7225 0.1620 0.8700 0.035 Uiso 1 1 d R . . C39 C 0.6212(5) 0.1629(3) 0.9373(3) 0.0323(12) Uani 1 1 d . . . H39 H 0.6750 0.1475 0.9790 0.039 Uiso 1 1 calc R . . C40 C 0.5079(5) 0.1751(3) 0.9440(3) 0.0327(12) Uani 1 1 d . . . H40 H 0.4842 0.1678 0.9901 0.039 Uiso 1 1 calc R . . C41 C 0.4324(5) 0.1982(3) 0.8812(3) 0.0318(12) Uani 1 1 d . . . H41 H 0.3563 0.2065 0.8848 0.038 Uiso 1 1 calc R . . C42 C 0.4662(4) 0.2093(3) 0.8130(3) 0.0300(12) Uani 1 1 d . . . H42 H 0.4141 0.2252 0.7708 0.036 Uiso 1 1 calc R . . C43 C 0.5778(4) 0.1964(3) 0.8085(3) 0.0289(12) Uani 1 1 d . . . H43 H 0.6029 0.2033 0.7628 0.035 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 0.01319(11) 0.01781(10) 0.01628(10) 0.00093(7) 0.00180(7) 0.00130(6) Cl1 0.0171(5) 0.0336(7) 0.0190(5) -0.0010(5) 0.0025(4) -0.0014(4) Cl2 0.0215(6) 0.0294(6) 0.0252(6) 0.0076(5) 0.0081(4) 0.0030(5) Cl3 0.0218(6) 0.0234(6) 0.0347(7) -0.0032(5) 0.0052(5) 0.0043(4) O1 0.0185(16) 0.0214(17) 0.0212(17) 0.0026(14) 0.0077(13) 0.0006(13) O2 0.0180(16) 0.0184(17) 0.0196(16) -0.0001(13) 0.0037(12) 0.0031(12) O3 0.0179(17) 0.0199(17) 0.0193(16) 0.0008(13) -0.0058(13) 0.0029(13) O4 0.0126(16) 0.0191(17) 0.0291(18) -0.0006(14) 0.0022(13) 0.0015(12) C1 0.013(2) 0.028(3) 0.026(3) 0.008(2) -0.0008(18) 0.0031(18) C2 0.016(2) 0.025(3) 0.018(2) 0.0074(19) 0.0012(17) 0.0023(18) C3 0.016(2) 0.033(3) 0.019(2) 0.006(2) 0.0032(18) 0.0077(19) C4 0.025(3) 0.035(3) 0.023(3) 0.006(2) 0.010(2) 0.009(2) C5 0.028(3) 0.043(3) 0.032(3) 0.011(3) 0.016(2) 0.007(2) C6 0.029(3) 0.031(3) 0.031(3) 0.013(2) 0.010(2) 0.002(2) C7 0.023(2) 0.029(3) 0.018(2) -0.002(2) 0.0004(18) 0.008(2) C8 0.014(2) 0.020(2) 0.022(2) -0.0003(19) 0.0030(18) 0.0041(17) C9 0.024(2) 0.012(2) 0.020(2) -0.0010(18) 0.0034(18) 0.0020(17) C10 0.018(2) 0.018(2) 0.020(2) -0.0026(18) 0.0038(18) -0.0014(17) C11 0.021(2) 0.019(2) 0.023(2) -0.0014(19) 0.0017(19) 0.0054(18) C12 0.016(2) 0.025(3) 0.029(3) -0.001(2) 0.0038(19) 0.0071(18) C13 0.027(3) 0.021(2) 0.022(2) -0.004(2) 0.0075(19) -0.0016(19) C14 0.015(2) 0.019(2) 0.025(2) 0.0022(19) 0.0019(18) 0.0017(17) C15 0.021(2) 0.024(3) 0.017(2) 0.0020(19) 0.0061(18) 0.0035(18) C16 0.011(2) 0.026(3) 0.020(2) 0.0024(19) 0.0029(17) 0.0028(17) C17 0.027(3) 0.024(3) 0.019(2) 0.0000(19) 0.005(2) 0.0019(19) C18 0.018(3) 0.037(3) 0.020(2) -0.005(2) 0.0011(19) 0.000(2) C19 0.031(3) 0.036(3) 0.020(2) 0.000(2) -0.002(2) 0.011(2) C20 0.025(3) 0.026(3) 0.025(3) 0.002(2) 0.0039(19) 0.009(2) C21 0.031(3) 0.021(3) 0.019(2) -0.0049(19) 0.000(2) 0.0030(19) C22 0.017(2) 0.022(2) 0.027(3) -0.002(2) 0.0015(19) 0.0006(18) C23 0.017(2) 0.015(2) 0.030(3) -0.0002(19) 0.0021(19) 0.0034(17) C24 0.027(3) 0.017(2) 0.029(3) 0.000(2) 0.001(2) -0.0027(19) C25 0.039(3) 0.029(3) 0.032(3) 0.005(2) 0.007(2) -0.008(2) C26 0.018(3) 0.040(3) 0.042(3) 0.001(3) 0.002(2) -0.012(2) C27 0.026(3) 0.033(3) 0.031(3) -0.005(2) -0.002(2) -0.005(2) C28 0.023(3) 0.023(3) 0.029(3) 0.007(2) 0.003(2) -0.0013(19) N1 0.020(2) 0.025(2) 0.032(2) -0.0032(18) 0.0053(17) 0.0011(17) C29 0.024(3) 0.032(3) 0.030(3) -0.003(2) 0.007(2) 0.003(2) C30 0.031(3) 0.028(3) 0.043(3) 0.001(2) 0.018(2) -0.002(2) C31 0.023(3) 0.025(3) 0.057(4) -0.012(3) 0.012(2) -0.005(2) C32 0.021(3) 0.037(3) 0.043(3) -0.013(3) -0.003(2) 0.001(2) C33 0.034(3) 0.029(3) 0.034(3) 0.001(2) 0.003(2) 0.002(2) N2 0.034(2) 0.023(2) 0.028(2) 0.0009(18) 0.0130(19) 0.0005(18) C34 0.060(4) 0.035(3) 0.029(3) -0.004(2) 0.019(3) -0.018(3) C35 0.086(4) 0.051(3) 0.058(4) -0.012(3) 0.043(3) -0.025(3) C36 0.075(4) 0.048(3) 0.089(4) 0.003(3) 0.064(3) 0.004(3) C37 0.046(3) 0.069(4) 0.083(4) 0.037(3) 0.034(3) 0.023(3) C38 0.027(3) 0.041(3) 0.058(4) 0.024(3) 0.017(3) 0.004(2) N3 0.015(2) 0.032(2) 0.042(3) -0.001(2) 0.0068(18) 0.0008(17) C39 0.033(3) 0.031(3) 0.032(3) -0.005(2) 0.004(2) 0.003(2) C40 0.037(3) 0.030(3) 0.031(3) -0.003(2) 0.009(2) -0.001(2) C41 0.023(3) 0.028(3) 0.047(3) -0.005(2) 0.012(2) 0.002(2) C42 0.019(3) 0.026(3) 0.043(3) 0.000(2) 0.001(2) 0.0017(19) C43 0.019(3) 0.032(3) 0.037(3) 0.001(2) 0.008(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O3 2.130(3) . ? U O1 2.139(3) . ? U O2 2.279(3) . ? U O4 2.605(3) . ? U Cl3 2.7470(12) . ? U Cl2 2.7629(11) . ? U Cl1 2.7772(11) . ? O1 C2 1.351(5) . ? O1 O4 2.865(5) . ? O1 O2 2.900(4) . ? O2 C9 1.365(5) . ? O2 O3 2.864(4) . ? O3 C16 1.344(5) . ? O3 O4 2.776(5) . ? O4 C23 1.405(6) . ? C1 C6 1.396(7) . ? C1 C2 1.397(7) . ? C1 C28 1.511(7) . ? C2 C3 1.402(7) . ? C3 C4 1.397(7) . ? C3 C7 1.502(7) . ? C4 C5 1.399(8) . ? C5 C6 1.402(8) . ? C7 C8 1.531(6) . ? C8 C13 1.382(6) . ? C8 C9 1.400(6) . ? C9 C10 1.413(6) . ? C10 C11 1.388(6) . ? C10 C14 1.521(6) . ? C11 C12 1.390(7) . ? C12 C13 1.400(7) . ? C14 C15 1.512(7) . ? C15 C20 1.390(7) . ? C15 C16 1.404(7) . ? C16 C17 1.399(7) . ? C17 C18 1.386(7) . ? C17 C21 1.511(7) . ? C18 C19 1.390(7) . ? C19 C20 1.386(7) . ? C21 C22 1.520(7) . ? C22 C27 1.399(7) . ? C22 C23 1.406(7) . ? C23 C24 1.399(7) . ? C24 C25 1.394(7) . ? C24 C28 1.516(7) . ? C25 C26 1.385(8) . ? C26 C27 1.384(8) . ? N1 C29 1.331(7) . ? N1 C33 1.336(7) . ? C29 C30 1.375(8) . ? C30 C31 1.392(8) . ? C31 C32 1.387(9) . ? C32 C33 1.378(8) . ? N2 C38 1.327(7) . ? N2 C34 1.341(7) . ? C34 C35 1.356(10) . ? C35 C36 1.302(12) . ? C36 C37 1.400(12) . ? C37 C38 1.421(10) . ? N3 C39 1.326(7) . ? N3 C43 1.343(7) . ? C39 C40 1.391(8) . ? C40 C41 1.367(8) . ? C41 C42 1.370(8) . ? C42 C43 1.364(7) . ? 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 O3 U O1 99.97(12) . . ? O3 U O2 80.94(12) . . ? O1 U O2 81.96(12) . . ? O3 U O4 70.99(11) . . ? O1 U O4 73.57(11) . . ? O2 U O4 138.32(10) . . ? O3 U Cl3 116.64(9) . . ? O1 U Cl3 112.94(9) . . ? O2 U Cl3 152.62(8) . . ? O4 U Cl3 69.06(7) . . ? O3 U Cl2 83.68(9) . . ? O1 U Cl2 160.81(9) . . ? O2 U Cl2 80.02(8) . . ? O4 U Cl2 124.98(8) . . ? Cl3 U Cl2 81.31(4) . . ? O3 U Cl1 154.82(9) . . ? O1 U Cl1 88.48(9) . . ? O2 U Cl1 76.79(8) . . ? O4 U Cl1 134.13(7) . . ? Cl3 U Cl1 80.66(4) . . ? Cl2 U Cl1 81.04(3) . . ? C2 O1 U 170.4(3) . . ? C9 O2 U 125.2(3) . . ? C16 O3 U 171.2(3) . . ? C23 O4 U 123.7(3) . . ? C6 C1 C2 118.8(5) . . ? C6 C1 C28 121.2(5) . . ? C2 C1 C28 120.0(4) . . ? O1 C2 C1 118.9(4) . . ? O1 C2 C3 119.3(4) . . ? C1 C2 C3 121.8(4) . . ? C4 C3 C2 118.1(5) . . ? C4 C3 C7 121.4(5) . . ? C2 C3 C7 120.4(4) . . ? C3 C4 C5 121.6(5) . . ? C4 C5 C6 118.9(5) . . ? C1 C6 C5 120.9(5) . . ? C3 C7 C8 110.9(4) . . ? C13 C8 C9 118.9(4) . . ? C13 C8 C7 119.1(4) . . ? C9 C8 C7 121.9(4) . . ? O2 C9 C8 119.8(4) . . ? O2 C9 C10 119.6(4) . . ? C8 C9 C10 120.6(4) . . ? C11 C10 C9 118.9(4) . . ? C11 C10 C14 120.0(4) . . ? C9 C10 C14 121.1(4) . . ? C12 C11 C10 121.2(4) . . ? C11 C12 C13 118.9(4) . . ? C8 C13 C12 121.5(4) . . ? C15 C14 C10 112.1(4) . . ? C20 C15 C16 118.1(4) . . ? C20 C15 C14 122.1(4) . . ? C16 C15 C14 119.8(4) . . ? O3 C16 C17 118.9(4) . . ? O3 C16 C15 119.6(4) . . ? C17 C16 C15 121.5(4) . . ? C18 C17 C16 118.6(5) . . ? C18 C17 C21 122.1(5) . . ? C16 C17 C21 119.3(4) . . ? C17 C18 C19 120.9(5) . . ? C20 C19 C18 119.8(5) . . ? C19 C20 C15 121.1(5) . . ? C17 C21 C22 112.0(4) . . ? C27 C22 C23 117.9(5) . . ? C27 C22 C21 119.5(4) . . ? C23 C22 C21 122.6(4) . . ? C24 C23 C22 121.9(4) . . ? C24 C23 O4 120.2(4) . . ? C22 C23 O4 117.9(4) . . ? C25 C24 C23 118.0(5) . . ? C25 C24 C28 119.4(5) . . ? C23 C24 C28 122.5(4) . . ? C26 C25 C24 121.3(5) . . ? C27 C26 C25 120.0(5) . . ? C26 C27 C22 120.9(5) . . ? C1 C28 C24 113.3(4) . . ? C29 N1 C33 122.0(5) . . ? N1 C29 C30 120.8(5) . . ? C29 C30 C31 118.5(5) . . ? C32 C31 C30 119.5(5) . . ? C33 C32 C31 119.1(5) . . ? N1 C33 C32 120.0(5) . . ? C38 N2 C34 118.4(5) . . ? N2 C34 C35 123.9(7) . . ? C36 C35 C34 118.4(8) . . ? C35 C36 C37 122.2(7) . . ? C36 C37 C38 116.3(7) . . ? N2 C38 C37 120.8(7) . . ? C39 N3 C43 123.3(4) . . ? N3 C39 C40 118.9(5) . . ? C41 C40 C39 118.3(5) . . ? C40 C41 C42 121.5(5) . . ? C43 C42 C41 118.6(5) . . ? N3 C43 C42 119.4(5) . . ? 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 N2 0.94 1.72 2.658(5) 172.9 . N1 H1 O2 0.95 1.64 2.575(5) 166.5 . N3 H3 Cl1 0.87 2.64 3.259(4) 128.7 1_655 N3 H3 Cl2 0.87 2.55 3.290(4) 143.4 1_655 N3 H3 Cl3 0.87 3.09 3.439(4) 106.0 1_655 #===END data_5.3py _database_code_depnum_ccdc_archive 'CCDC 603335' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H69 Cl6 N7 O6 U2' _chemical_formula_weight 1877.15 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.0764(8) _cell_length_b 12.8301(4) _cell_length_c 24.7114(7) _cell_angle_alpha 90.00 _cell_angle_beta 118.024(2) _cell_angle_gamma 90.00 _cell_volume 7298.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 58951 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method ? _exptl_crystal_F_000 3656 _exptl_absorpt_coefficient_mu 4.710 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.451 _exptl_absorpt_correction_T_max 0.568 _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 two \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 58951 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6923 _reflns_number_gt 5851 _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. One of the pyridine solvent molecules (corresponding to N4) is disordered around a binary axis and has been refined as an idealized hexagon with an occupancy factor of 0.5. The H atoms bound N atoms were found on a Fourier-difference map and all the other ones were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0334P)^2^+31.1376P] 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 6923 _refine_ls_number_parameters 481 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.139 _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 0.655 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.107 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 0.133498(6) -0.004531(11) 0.162300(6) 0.01992(6) Uani 1 1 d . . . Cl1 Cl 0.17733(5) -0.14129(8) 0.25618(5) 0.0295(2) Uani 1 1 d . . . Cl2 Cl 0.03380(5) 0.02221(10) 0.16457(6) 0.0370(3) Uani 1 1 d . . . Cl3 Cl 0.18357(5) 0.14823(8) 0.24573(5) 0.0287(2) Uani 1 1 d . . . O1 O 0.10475(12) -0.1303(2) 0.09687(13) 0.0233(6) Uani 1 1 d . . . O2 O 0.21877(12) -0.0248(2) 0.16232(13) 0.0222(6) Uani 1 1 d . . . O3 O 0.11687(12) 0.1043(2) 0.08980(13) 0.0234(6) Uani 1 1 d . . . N1 N 0.31037(16) -0.0045(3) 0.27228(17) 0.0264(8) Uani 1 1 d . . . H1 H 0.2779 -0.0202 0.2320 0.032 Uiso 1 1 d R . . N2 N 0.11695(18) -0.0928(3) -0.12735(19) 0.0396(10) Uani 1 1 d . . . H2 H 0.1145 -0.1635 -0.1439 0.048 Uiso 1 1 d R . . N3 N 0.0995(2) -0.2765(4) -0.1867(2) 0.0504(13) Uani 1 1 d . . . C1 C 0.03840(18) -0.2250(3) 0.00947(19) 0.0227(9) Uani 1 1 d . . . C2 C 0.09611(18) -0.1988(3) 0.05271(17) 0.0203(9) Uani 1 1 d . . . C3 C 0.14354(19) -0.2463(3) 0.04999(19) 0.0244(9) Uani 1 1 d . . . C4 C 0.13283(19) -0.3202(3) 0.0052(2) 0.0269(10) Uani 1 1 d . . . H4 H 0.1640 -0.3526 0.0036 0.032 Uiso 1 1 calc R . . C5 C 0.07617(19) -0.3473(4) -0.0377(2) 0.0286(10) Uani 1 1 d . . . H5 H 0.0696 -0.3968 -0.0677 0.034 Uiso 1 1 calc R . . C6 C 0.03014(19) -0.2995(3) -0.03471(19) 0.0260(9) Uani 1 1 d . . . H6 H -0.0075 -0.3176 -0.0632 0.031 Uiso 1 1 calc R . . C7 C 0.20556(18) -0.2169(3) 0.0964(2) 0.0242(9) Uani 1 1 d . . . H7A H 0.2318 -0.2717 0.0980 0.029 Uiso 1 1 calc R . . H7B H 0.2082 -0.2112 0.1368 0.029 Uiso 1 1 calc R . . C8 C 0.22441(17) -0.1139(3) 0.08018(19) 0.0228(9) Uani 1 1 d . . . C9 C 0.22728(18) -0.0214(3) 0.1123(2) 0.0238(9) Uani 1 1 d . . . C10 C 0.23854(17) 0.0748(3) 0.09309(18) 0.0233(9) Uani 1 1 d . . . C11 C 0.25359(18) 0.0759(3) 0.0459(2) 0.0269(10) Uani 1 1 d . . . H11 H 0.2628 0.1388 0.0338 0.032 Uiso 1 1 calc R . . C12 C 0.25491(19) -0.0157(3) 0.0168(2) 0.0275(10) Uani 1 1 d . . . H12 H 0.2665 -0.0146 -0.0135 0.033 Uiso 1 1 calc R . . C13 C 0.23890(18) -0.1086(3) 0.0329(2) 0.0266(10) Uani 1 1 d . . . H13 H 0.2378 -0.1691 0.0116 0.032 Uiso 1 1 calc R . . C14 C 0.22948(17) 0.1775(3) 0.11819(18) 0.0221(9) Uani 1 1 d . . . H14A H 0.2274 0.1646 0.1558 0.026 Uiso 1 1 calc R . . H14B H 0.2624 0.2230 0.1278 0.026 Uiso 1 1 calc R . . C15 C 0.17423(18) 0.2309(3) 0.07238(18) 0.0212(9) Uani 1 1 d . . . C16 C 0.11911(18) 0.1872(3) 0.05771(18) 0.0203(9) Uani 1 1 d . . . C17 C 0.06809(18) 0.2277(3) 0.01017(19) 0.0228(9) Uani 1 1 d . . . C18 C 0.07206(19) 0.3165(3) -0.0200(2) 0.0282(10) Uani 1 1 d . . . H18 H 0.0384 0.3449 -0.0514 0.034 Uiso 1 1 calc R . . C19 C 0.1255(2) 0.3637(4) -0.0041(2) 0.0313(10) Uani 1 1 d . . . H19 H 0.1273 0.4242 -0.0239 0.038 Uiso 1 1 calc R . . C20 C 0.17602(19) 0.3197(3) 0.0416(2) 0.0264(10) Uani 1 1 d . . . H20 H 0.2117 0.3504 0.0516 0.032 Uiso 1 1 calc R . . C21 C 0.01098(17) 0.1691(3) -0.01249(19) 0.0234(9) Uani 1 1 d . . . H21A H -0.0018 0.1493 -0.0548 0.028 Uiso 1 1 calc R . . H21B H 0.0185 0.1054 0.0111 0.028 Uiso 1 1 calc R . . C22 C 0.3300(2) 0.0939(4) 0.2853(2) 0.0314(10) Uani 1 1 d . . . H22 H 0.3132 0.1458 0.2559 0.038 Uiso 1 1 calc R . . C23 C 0.3743(2) 0.1177(4) 0.3412(2) 0.0324(11) Uani 1 1 d . . . H23 H 0.3889 0.1852 0.3500 0.039 Uiso 1 1 calc R . . C24 C 0.3973(2) 0.0404(4) 0.3851(2) 0.0315(10) Uani 1 1 d . . . H24 H 0.4270 0.0560 0.4240 0.038 Uiso 1 1 calc R . . C25 C 0.37634(19) -0.0603(4) 0.3711(2) 0.0297(10) Uani 1 1 d . . . H25 H 0.3918 -0.1129 0.4003 0.036 Uiso 1 1 calc R . . C26 C 0.33211(19) -0.0813(4) 0.3132(2) 0.0304(10) Uani 1 1 d . . . H26 H 0.3176 -0.1486 0.3027 0.037 Uiso 1 1 calc R . . C27 C 0.1030(2) -0.0822(4) -0.0819(2) 0.0329(11) Uani 1 1 d . . . H27 H 0.0899 -0.1396 -0.0689 0.040 Uiso 1 1 calc R . . C28 C 0.1079(2) 0.0131(4) -0.0542(2) 0.0324(11) Uani 1 1 d . . . H28 H 0.0997 0.0201 -0.0216 0.039 Uiso 1 1 calc R . . C29 C 0.1254(2) 0.0982(4) -0.0758(2) 0.0367(11) Uani 1 1 d . . . H29 H 0.1277 0.1638 -0.0588 0.044 Uiso 1 1 calc R . . C30 C 0.1396(2) 0.0853(4) -0.1230(2) 0.0424(13) Uani 1 1 d . . . H30 H 0.1520 0.1416 -0.1375 0.051 Uiso 1 1 calc R . . C31 C 0.1350(3) -0.0115(4) -0.1476(3) 0.0437(13) Uani 1 1 d . . . H31 H 0.1445 -0.0210 -0.1791 0.052 Uiso 1 1 calc R . . C32 C 0.0643(3) -0.2688(6) -0.2474(3) 0.0570(17) Uani 1 1 d . . . H32 H 0.0515 -0.2033 -0.2646 0.068 Uiso 1 1 calc R . . C33 C 0.0467(3) -0.3561(6) -0.2851(3) 0.0604(17) Uani 1 1 d U . . H33 H 0.0226 -0.3494 -0.3270 0.073 Uiso 1 1 calc R . . C34 C 0.0650(3) -0.4504(7) -0.2597(3) 0.073(2) Uani 1 1 d U . . H34 H 0.0527 -0.5098 -0.2841 0.088 Uiso 1 1 calc R . . C35 C 0.1027(3) -0.4597(7) -0.1967(4) 0.078(2) Uani 1 1 d . . . H35 H 0.1167 -0.5242 -0.1785 0.093 Uiso 1 1 calc R . . C36 C 0.1179(2) -0.3698(6) -0.1632(3) 0.0573(17) Uani 1 1 d . . . H36 H 0.1427 -0.3747 -0.1213 0.069 Uiso 1 1 calc R . . N4 N 0.0755(3) 0.6878(6) 0.2879(4) 0.053(3) Uani 0.50 1 d PG . . C37 C 0.0517(4) 0.6745(7) 0.3273(3) 0.067(4) Uani 0.50 1 d PG . . H37A H 0.0710 0.6312 0.3630 0.076 Uiso 0.50 1 d P . . C38 C -0.0001(4) 0.7239(8) 0.3151(4) 0.072(4) Uani 0.50 1 d PGU . . H38A H -0.0165 0.7148 0.3423 0.087 Uiso 0.50 1 d PR . . C39 C -0.0280(3) 0.7866(7) 0.2635(5) 0.069(5) Uani 0.50 1 d PG . . H39A H -0.0638 0.8208 0.2550 0.106 Uiso 0.50 1 d PR . . C40 C -0.0042(3) 0.7999(6) 0.2241(4) 0.061(4) Uani 0.50 1 d PG . . H40A H -0.0235 0.8433 0.1884 0.070 Uiso 0.50 1 d PR . . C41 C 0.0476(4) 0.7505(7) 0.2363(4) 0.065(5) Uani 0.50 1 d PG . . H41A H 0.0641 0.7597 0.2091 0.070 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02017(9) 0.01960(9) 0.01903(10) -0.00028(6) 0.00842(7) -0.00021(6) Cl1 0.0352(6) 0.0266(5) 0.0248(5) 0.0040(4) 0.0126(5) 0.0057(5) Cl2 0.0244(5) 0.0457(7) 0.0426(7) -0.0029(5) 0.0172(5) 0.0008(5) Cl3 0.0308(6) 0.0259(5) 0.0296(6) -0.0057(4) 0.0142(5) -0.0036(4) O1 0.0237(15) 0.0216(15) 0.0237(15) -0.0048(12) 0.0103(13) -0.0001(12) O2 0.0181(14) 0.0254(15) 0.0215(15) 0.0009(12) 0.0080(12) 0.0004(12) O3 0.0218(15) 0.0223(15) 0.0235(15) 0.0076(12) 0.0086(12) 0.0010(12) N1 0.0214(18) 0.031(2) 0.0242(19) -0.0018(15) 0.0086(15) -0.0015(15) N2 0.042(3) 0.043(3) 0.035(2) -0.0078(19) 0.020(2) -0.005(2) N3 0.046(3) 0.074(4) 0.038(3) -0.013(2) 0.025(2) -0.017(3) C1 0.025(2) 0.019(2) 0.027(2) 0.0056(17) 0.0140(19) 0.0022(17) C2 0.023(2) 0.017(2) 0.019(2) 0.0023(15) 0.0079(18) -0.0009(16) C3 0.027(2) 0.021(2) 0.029(2) 0.0018(17) 0.0155(19) 0.0020(17) C4 0.027(2) 0.023(2) 0.037(3) -0.0029(18) 0.020(2) 0.0032(18) C5 0.031(2) 0.028(2) 0.028(2) -0.0089(19) 0.015(2) -0.0024(19) C6 0.028(2) 0.026(2) 0.024(2) -0.0023(17) 0.0117(19) -0.0034(18) C7 0.022(2) 0.020(2) 0.032(2) 0.0014(17) 0.0137(19) 0.0019(17) C8 0.015(2) 0.026(2) 0.026(2) -0.0009(17) 0.0092(18) 0.0024(17) C9 0.016(2) 0.027(2) 0.031(2) -0.0003(17) 0.0130(18) -0.0014(17) C10 0.018(2) 0.027(2) 0.021(2) 0.0027(17) 0.0059(17) 0.0007(17) C11 0.021(2) 0.024(2) 0.038(3) 0.0039(19) 0.015(2) 0.0022(18) C12 0.025(2) 0.032(3) 0.031(2) 0.0019(18) 0.017(2) 0.0044(18) C13 0.024(2) 0.025(2) 0.031(2) -0.0063(18) 0.014(2) 0.0003(18) C14 0.017(2) 0.025(2) 0.017(2) -0.0010(16) 0.0020(17) -0.0049(17) C15 0.020(2) 0.020(2) 0.023(2) -0.0042(16) 0.0099(18) -0.0024(17) C16 0.021(2) 0.019(2) 0.016(2) -0.0021(15) 0.0052(17) 0.0017(16) C17 0.020(2) 0.022(2) 0.024(2) -0.0042(17) 0.0076(18) 0.0011(17) C18 0.024(2) 0.029(2) 0.028(2) 0.0099(18) 0.010(2) 0.0066(19) C19 0.032(3) 0.026(2) 0.039(3) 0.009(2) 0.020(2) -0.001(2) C20 0.025(2) 0.022(2) 0.032(2) -0.0008(18) 0.014(2) -0.0024(18) C21 0.021(2) 0.020(2) 0.025(2) -0.0019(17) 0.0074(18) 0.0000(17) C22 0.034(3) 0.026(2) 0.038(3) 0.004(2) 0.019(2) 0.004(2) C23 0.040(3) 0.024(2) 0.038(3) -0.0056(19) 0.022(2) -0.005(2) C24 0.028(2) 0.042(3) 0.022(2) -0.002(2) 0.009(2) -0.005(2) C25 0.026(2) 0.031(3) 0.030(2) 0.0108(19) 0.011(2) 0.0047(19) C26 0.027(2) 0.026(2) 0.037(3) 0.000(2) 0.014(2) -0.0014(19) C27 0.026(2) 0.043(3) 0.030(2) 0.000(2) 0.012(2) -0.005(2) C28 0.024(2) 0.047(3) 0.023(2) -0.001(2) 0.0080(19) 0.003(2) C29 0.033(3) 0.043(3) 0.031(3) 0.001(2) 0.013(2) 0.003(2) C30 0.046(3) 0.047(3) 0.036(3) -0.001(2) 0.021(3) -0.010(3) C31 0.052(3) 0.054(4) 0.035(3) -0.007(2) 0.028(3) -0.011(3) C32 0.057(4) 0.082(5) 0.042(3) 0.001(3) 0.032(3) -0.023(3) C33 0.053(3) 0.089(4) 0.048(3) -0.011(3) 0.031(3) -0.012(3) C34 0.065(3) 0.087(4) 0.079(4) -0.031(3) 0.045(3) -0.002(3) C35 0.058(4) 0.087(5) 0.076(5) -0.011(4) 0.022(4) 0.030(4) C36 0.030(3) 0.099(6) 0.039(3) -0.015(3) 0.013(3) 0.004(3) N4 0.042(5) 0.051(6) 0.059(6) 0.006(5) 0.017(5) 0.004(5) C37 0.074(9) 0.077(10) 0.066(9) -0.028(7) 0.046(8) -0.010(8) C38 0.072(6) 0.079(6) 0.073(5) -0.013(4) 0.039(4) -0.001(4) C39 0.041(11) 0.065(11) 0.108(14) -0.033(10) 0.040(9) -0.004(9) C40 0.042(8) 0.044(7) 0.095(11) 0.009(6) 0.031(10) 0.004(7) C41 0.037(8) 0.061(10) 0.090(11) 0.021(8) 0.026(7) 0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O3 2.149(3) . ? U O1 2.154(3) . ? U O2 2.238(3) . ? U Cl2 2.6488(12) . ? U Cl3 2.6958(10) . ? U Cl1 2.6973(10) . ? U U 7.7685(4) 5 ? O1 C2 1.336(5) . ? O2 C9 1.355(5) . ? O3 C16 1.344(5) . ? N1 C26 1.333(6) . ? N1 C22 1.343(6) . ? N2 C31 1.335(7) . ? N2 C27 1.341(6) . ? N3 C36 1.318(8) . ? N3 C32 1.345(7) . ? C1 C6 1.389(6) . ? C1 C2 1.417(6) . ? C1 C21 1.506(6) 5 ? C2 C3 1.408(6) . ? C3 C4 1.382(6) . ? C3 C7 1.527(6) . ? C4 C5 1.399(6) . ? C5 C6 1.380(6) . ? C7 C8 1.528(6) . ? C8 C13 1.387(6) . ? C8 C9 1.410(6) . ? C9 C10 1.402(6) . ? C10 C11 1.395(6) . ? C10 C14 1.521(6) . ? C11 C12 1.387(6) . ? C12 C13 1.383(6) . ? C14 C15 1.515(6) . ? C15 C20 1.382(6) . ? C15 C16 1.422(6) . ? C16 C17 1.397(6) . ? C17 C18 1.391(6) . ? C17 C21 1.521(6) . ? C18 C19 1.396(6) . ? C19 C20 1.390(6) . ? C21 C1 1.506(6) 5 ? C22 C23 1.354(6) . ? C23 C24 1.381(7) . ? C24 C25 1.382(7) . ? C25 C26 1.380(6) . ? C27 C28 1.377(7) . ? C28 C29 1.384(7) . ? C29 C30 1.387(7) . ? C30 C31 1.363(7) . ? C32 C33 1.390(9) . ? C33 C34 1.342(10) . ? C34 C35 1.404(10) . ? C35 C36 1.365(9) . ? N4 C37 1.3900 . ? N4 C41 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 U O1 89.89(11) . . ? O3 U O2 83.50(11) . . ? O1 U O2 84.76(11) . . ? O3 U Cl2 96.77(8) . . ? O1 U Cl2 96.54(8) . . ? O2 U Cl2 178.66(8) . . ? O3 U Cl3 90.05(8) . . ? O1 U Cl3 172.43(8) . . ? O2 U Cl3 87.71(8) . . ? Cl2 U Cl3 90.98(4) . . ? O3 U Cl1 167.89(8) . . ? O1 U Cl1 90.89(8) . . ? O2 U Cl1 84.54(8) . . ? Cl2 U Cl1 95.14(4) . . ? Cl3 U Cl1 87.59(3) . . ? C26 N1 C22 122.3(4) . . ? C31 N2 C27 121.1(5) . . ? C36 N3 C32 118.3(6) . . ? C6 C1 C2 118.2(4) . . ? C6 C1 C21 123.1(4) . 5 ? C2 C1 C21 118.7(4) . 5 ? O1 C2 C3 120.6(4) . . ? O1 C2 C1 118.9(4) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 118.9(4) . . ? C4 C3 C7 121.0(4) . . ? C2 C3 C7 120.1(4) . . ? C3 C4 C5 121.4(4) . . ? C6 C5 C4 119.0(4) . . ? C5 C6 C1 122.0(4) . . ? C3 C7 C8 112.0(3) . . ? C13 C8 C9 118.0(4) . . ? C13 C8 C7 120.8(4) . . ? C9 C8 C7 121.2(4) . . ? O2 C9 C10 119.2(4) . . ? O2 C9 C8 119.9(4) . . ? C10 C9 C8 121.0(4) . . ? C11 C10 C9 118.6(4) . . ? C11 C10 C14 119.4(4) . . ? C9 C10 C14 121.8(4) . . ? C12 C11 C10 120.7(4) . . ? C13 C12 C11 119.8(4) . . ? C12 C13 C8 121.6(4) . . ? C15 C14 C10 111.3(3) . . ? C20 C15 C16 118.4(4) . . ? C20 C15 C14 121.2(4) . . ? C16 C15 C14 120.3(4) . . ? O3 C16 C17 120.2(4) . . ? O3 C16 C15 118.7(3) . . ? C17 C16 C15 121.1(4) . . ? C18 C17 C16 118.3(4) . . ? C18 C17 C21 120.9(4) . . ? C16 C17 C21 120.4(4) . . ? C17 C18 C19 121.3(4) . . ? C20 C19 C18 119.5(4) . . ? C15 C20 C19 121.2(4) . . ? C1 C21 C17 117.3(4) 5 . ? N1 C22 C23 120.2(4) . . ? C22 C23 C24 119.1(4) . . ? C25 C24 C23 120.0(4) . . ? C26 C25 C24 118.8(4) . . ? N1 C26 C25 119.5(4) . . ? N2 C27 C28 120.6(5) . . ? C27 C28 C29 118.6(5) . . ? C28 C29 C30 119.8(5) . . ? C31 C30 C29 118.7(5) . . ? N2 C31 C30 121.2(5) . . ? N3 C32 C33 121.7(7) . . ? C34 C33 C32 118.8(6) . . ? C33 C34 C35 120.3(7) . . ? C36 C35 C34 117.0(8) . . ? N3 C36 C35 123.9(6) . . ? C37 N4 C41 120.0 . . ? C38 C37 N4 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 N4 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.98 1.69 2.657(5) 169.8 . N2 H2 N3 0.98 1.73 2.699(7) 168.4 . #===END data_6.py _database_code_depnum_ccdc_archive 'CCDC 603336' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H58 Cl5 N5 O6 U2' _chemical_formula_weight 1682.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/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 14.6847(5) _cell_length_b 21.1309(7) _cell_length_c 20.9186(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.721(2) _cell_angle_gamma 90.00 _cell_volume 6216.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 102896 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method ? _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 5.475 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.364 _exptl_absorpt_correction_T_max 0.518 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 40 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 two \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 102896 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.68 _reflns_number_total 11793 _reflns_number_gt 9791 _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 bound to N atoms were found on a Fourier-difference map and all the other ones were introduced at calculated positions. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 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^)+(0.0441P)^2^+5.7398P] 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 11793 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 1.008 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.133 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 0.501860(12) 0.503153(8) 0.276378(8) 0.01436(6) Uani 1 1 d . . . U2 U 0.033380(13) 0.659972(8) 0.211511(8) 0.01472(6) Uani 1 1 d . . . Cl1 Cl 0.54938(9) 0.38562(6) 0.32352(6) 0.0220(3) Uani 1 1 d . . . Cl2 Cl 0.45401(9) 0.53843(6) 0.38497(6) 0.0208(3) Uani 1 1 d . . . Cl3 Cl 0.68342(9) 0.54171(6) 0.33123(6) 0.0223(3) Uani 1 1 d . . . Cl4 Cl -0.01968(9) 0.76576(6) 0.14123(6) 0.0247(3) Uani 1 1 d . . . Cl5 Cl -0.13993(9) 0.61294(6) 0.14780(6) 0.0247(3) Uani 1 1 d . . . O1 O 0.3625(2) 0.46781(15) 0.23262(15) 0.0187(7) Uani 1 1 d . . . O2 O 0.5250(2) 0.47491(15) 0.17922(15) 0.0180(7) Uani 1 1 d . . . O3 O 0.4679(2) 0.59282(15) 0.22904(15) 0.0179(7) Uani 1 1 d . . . O4 O 0.1625(2) 0.70512(15) 0.26544(15) 0.0176(7) Uani 1 1 d . . . O5 O -0.0284(2) 0.69860(16) 0.28760(15) 0.0196(8) Uani 1 1 d . . . O6 O 0.0639(2) 0.57630(15) 0.27172(14) 0.0163(7) Uani 1 1 d . . . N1 N 0.0916(3) 0.61258(19) 0.1166(2) 0.0221(10) Uani 1 1 d . . . N2 N 0.7094(3) 0.43787(19) 0.21823(19) 0.0196(9) Uani 1 1 d . . . H2 H 0.6350 0.4482 0.1966 0.024 Uiso 1 1 d R . . N3 N -0.2138(3) 0.7277(2) 0.25029(19) 0.0218(9) Uani 1 1 d . . . H3 H -0.1534 0.7134 0.2642 0.026 Uiso 1 1 d R . . N4 N 0.4137(3) 0.6391(2) 0.49171(19) 0.0217(9) Uani 1 1 d . . . H4 H 0.4696 0.6616 0.4925 0.026 Uiso 1 1 d R . . N5 N 0.5880(3) 0.6942(2) 0.4952(2) 0.0306(11) Uani 1 1 d . . . C1 C 0.2056(3) 0.4386(2) 0.2291(2) 0.0138(10) Uani 1 1 d . . . C2 C 0.2861(3) 0.4309(2) 0.2060(2) 0.0158(10) Uani 1 1 d . . . C3 C 0.2896(3) 0.3855(2) 0.1584(2) 0.0170(10) Uani 1 1 d . . . C4 C 0.2079(4) 0.3496(2) 0.1307(2) 0.0204(11) Uani 1 1 d . . . H4A H 0.2084 0.3192 0.0986 0.025 Uiso 1 1 calc R . . C5 C 0.1261(4) 0.3584(2) 0.1501(2) 0.0228(12) Uani 1 1 d . . . H5A H 0.0715 0.3353 0.1298 0.027 Uiso 1 1 calc R . . C6 C 0.1262(4) 0.4020(2) 0.2004(2) 0.0210(11) Uani 1 1 d . . . H6 H 0.0722 0.4065 0.2148 0.025 Uiso 1 1 calc R . . C7 C 0.3802(4) 0.3759(2) 0.1380(2) 0.0194(11) Uani 1 1 d . . . H7A H 0.4342 0.3740 0.1776 0.023 Uiso 1 1 calc R . . H7B H 0.3765 0.3359 0.1145 0.023 Uiso 1 1 calc R . . C8 C 0.3948(3) 0.4293(2) 0.0931(2) 0.0166(10) Uani 1 1 d . . . C9 C 0.4602(3) 0.4792(2) 0.1175(2) 0.0159(10) Uani 1 1 d . . . C10 C 0.4561(3) 0.5336(2) 0.0778(2) 0.0171(11) Uani 1 1 d . . . C11 C 0.3985(4) 0.5328(2) 0.0133(2) 0.0225(12) Uani 1 1 d . . . H11 H 0.3986 0.5676 -0.0139 0.027 Uiso 1 1 calc R . . C12 C 0.3406(4) 0.4820(3) -0.0128(3) 0.0252(12) Uani 1 1 d . . . H12 H 0.3040 0.4822 -0.0572 0.030 Uiso 1 1 calc R . . C13 C 0.3376(4) 0.4312(2) 0.0278(2) 0.0197(11) Uani 1 1 d . . . H13 H 0.2966 0.3977 0.0110 0.024 Uiso 1 1 calc R . . C14 C 0.5103(4) 0.5944(2) 0.1055(2) 0.0195(11) Uani 1 1 d . . . H14A H 0.5620 0.5844 0.1449 0.023 Uiso 1 1 calc R . . H14B H 0.5376 0.6122 0.0724 0.023 Uiso 1 1 calc R . . C15 C 0.4455(3) 0.6424(2) 0.1231(2) 0.0172(11) Uani 1 1 d . . . C16 C 0.4268(3) 0.6390(2) 0.1859(2) 0.0148(10) Uani 1 1 d . . . C17 C 0.3675(3) 0.6827(2) 0.2048(2) 0.0171(10) Uani 1 1 d . . . C18 C 0.3246(4) 0.7291(2) 0.1600(2) 0.0192(11) Uani 1 1 d . . . H18 H 0.2842 0.7580 0.1715 0.023 Uiso 1 1 calc R . . C19 C 0.3406(4) 0.7333(2) 0.0983(2) 0.0208(11) Uani 1 1 d . . . H19 H 0.3112 0.7649 0.0686 0.025 Uiso 1 1 calc R . . C20 C 0.4008(4) 0.6902(2) 0.0805(2) 0.0233(12) Uani 1 1 d . . . H20 H 0.4111 0.6937 0.0388 0.028 Uiso 1 1 calc R . . C21 C 0.3551(3) 0.6748(2) 0.2745(2) 0.0153(10) Uani 1 1 d . . . H21A H 0.3079 0.6420 0.2720 0.018 Uiso 1 1 calc R . . H21B H 0.4148 0.6594 0.3038 0.018 Uiso 1 1 calc R . . C22 C 0.3261(3) 0.7319(2) 0.3067(2) 0.0151(10) Uani 1 1 d . . . C23 C 0.2314(3) 0.7420(2) 0.3054(2) 0.0135(10) Uani 1 1 d . . . C24 C 0.2063(3) 0.7883(2) 0.3457(2) 0.0168(10) Uani 1 1 d . . . C25 C 0.2787(4) 0.8252(2) 0.3859(2) 0.0195(11) Uani 1 1 d . . . H25 H 0.2636 0.8553 0.4137 0.023 Uiso 1 1 calc R . . C26 C 0.3727(3) 0.8187(2) 0.3859(2) 0.0196(11) Uani 1 1 d . . . H26 H 0.4195 0.8452 0.4118 0.023 Uiso 1 1 calc R . . C27 C 0.3956(3) 0.7722(2) 0.3469(2) 0.0185(11) Uani 1 1 d . . . H27 H 0.4587 0.7673 0.3471 0.022 Uiso 1 1 calc R . . C28 C 0.1038(3) 0.7973(2) 0.3465(2) 0.0172(11) Uani 1 1 d . . . H28A H 0.0975 0.8386 0.3651 0.021 Uiso 1 1 calc R . . H28B H 0.0626 0.7964 0.3010 0.021 Uiso 1 1 calc R . . C29 C 0.0718(3) 0.7467(2) 0.3871(2) 0.0160(10) Uani 1 1 d . . . C30 C 0.0121(3) 0.6967(2) 0.3557(2) 0.0166(11) Uani 1 1 d . . . C31 C -0.0078(3) 0.6452(2) 0.3916(2) 0.0162(10) Uani 1 1 d . . . C32 C 0.0263(4) 0.6482(2) 0.4622(2) 0.0213(11) Uani 1 1 d . . . H32 H 0.0133 0.6151 0.4876 0.026 Uiso 1 1 calc R . . C33 C 0.0786(4) 0.6995(2) 0.4939(2) 0.0237(12) Uani 1 1 d . . . H33 H 0.0976 0.7020 0.5402 0.028 Uiso 1 1 calc R . . C34 C 0.1027(4) 0.7474(2) 0.4563(2) 0.0225(11) Uani 1 1 d . . . H34 H 0.1405 0.7808 0.4780 0.027 Uiso 1 1 calc R . . C35 C -0.0562(3) 0.5861(2) 0.3576(2) 0.0184(11) Uani 1 1 d . . . H35A H -0.0882 0.5955 0.3112 0.022 Uiso 1 1 calc R . . H35B H -0.1040 0.5729 0.3786 0.022 Uiso 1 1 calc R . . C36 C 0.0138(3) 0.5321(2) 0.3612(2) 0.0145(10) Uani 1 1 d . . . C37 C 0.0733(3) 0.5308(2) 0.3189(2) 0.0157(10) Uani 1 1 d . . . C38 C 0.1424(3) 0.4833(2) 0.3249(2) 0.0174(11) Uani 1 1 d . . . C39 C 0.1483(4) 0.4359(2) 0.3720(2) 0.0194(11) Uani 1 1 d . . . H39 H 0.1933 0.4039 0.3765 0.023 Uiso 1 1 calc R . . C40 C 0.0882(4) 0.4354(2) 0.4122(2) 0.0219(11) Uani 1 1 d . . . H40 H 0.0918 0.4027 0.4426 0.026 Uiso 1 1 calc R . . C41 C 0.0227(4) 0.4834(2) 0.4071(2) 0.0189(11) Uani 1 1 d . . . H41 H -0.0163 0.4831 0.4351 0.023 Uiso 1 1 calc R . . C42 C 0.2137(4) 0.4859(2) 0.2856(2) 0.0186(11) Uani 1 1 d . . . H42A H 0.2764 0.4810 0.3170 0.022 Uiso 1 1 calc R . . H42B H 0.2110 0.5281 0.2668 0.022 Uiso 1 1 calc R . . C43 C 0.1758(4) 0.5836(2) 0.1268(2) 0.0231(12) Uani 1 1 d . . . H43 H 0.2190 0.5853 0.1691 0.028 Uiso 1 1 calc R . . C44 C 0.2011(4) 0.5513(3) 0.0769(2) 0.0288(13) Uani 1 1 d . . . H44 H 0.2600 0.5315 0.0854 0.035 Uiso 1 1 calc R . . C45 C 0.1365(4) 0.5493(3) 0.0143(3) 0.0319(14) Uani 1 1 d . . . H45 H 0.1511 0.5274 -0.0200 0.038 Uiso 1 1 calc R . . C46 C 0.0511(4) 0.5794(3) 0.0028(3) 0.0364(15) Uani 1 1 d . . . H46 H 0.0074 0.5788 -0.0394 0.044 Uiso 1 1 calc R . . C47 C 0.0306(4) 0.6108(3) 0.0549(2) 0.0298(13) Uani 1 1 d . . . H47 H -0.0275 0.6314 0.0470 0.036 Uiso 1 1 calc R . . C48 C 0.7362(4) 0.3888(2) 0.2591(2) 0.0221(11) Uani 1 1 d . . . H48 H 0.6904 0.3635 0.2692 0.027 Uiso 1 1 calc R . . C49 C 0.8305(4) 0.3753(2) 0.2864(2) 0.0211(11) Uani 1 1 d . . . H49 H 0.8492 0.3415 0.3158 0.025 Uiso 1 1 calc R . . C50 C 0.8976(4) 0.4126(2) 0.2698(2) 0.0212(11) Uani 1 1 d . . . H50 H 0.9620 0.4037 0.2873 0.025 Uiso 1 1 calc R . . C51 C 0.8687(4) 0.4631(2) 0.2272(2) 0.0240(12) Uani 1 1 d . . . H51 H 0.9134 0.4883 0.2155 0.029 Uiso 1 1 calc R . . C52 C 0.7733(4) 0.4759(2) 0.2021(2) 0.0213(11) Uani 1 1 d . . . H52 H 0.7529 0.5105 0.1742 0.026 Uiso 1 1 calc R . . C53 C -0.2699(4) 0.6901(3) 0.2738(3) 0.0260(12) Uani 1 1 d . . . H53 H -0.2445 0.6549 0.2994 0.031 Uiso 1 1 calc R . . C54 C -0.3651(4) 0.7035(2) 0.2602(3) 0.0293(13) Uani 1 1 d . . . H54 H -0.4049 0.6776 0.2762 0.035 Uiso 1 1 calc R . . C55 C -0.4011(4) 0.7567(3) 0.2219(3) 0.0279(12) Uani 1 1 d . . . H55 H -0.4654 0.7665 0.2115 0.034 Uiso 1 1 calc R . . C56 C -0.3401(4) 0.7948(2) 0.1995(3) 0.0256(12) Uani 1 1 d . . . H56 H -0.3630 0.8311 0.1750 0.031 Uiso 1 1 calc R . . C57 C -0.2466(4) 0.7793(2) 0.2135(2) 0.0230(12) Uani 1 1 d . . . H57 H -0.2056 0.8042 0.1976 0.028 Uiso 1 1 calc R . . C58 C 0.3312(4) 0.6610(2) 0.4512(2) 0.0237(12) Uani 1 1 d . . . H58 H 0.3291 0.7003 0.4308 0.028 Uiso 1 1 calc R . . C59 C 0.2505(4) 0.6254(2) 0.4401(2) 0.0240(12) Uani 1 1 d . . . H59 H 0.1935 0.6400 0.4116 0.029 Uiso 1 1 calc R . . C60 C 0.2542(4) 0.5681(2) 0.4713(2) 0.0252(12) Uani 1 1 d . . . H60 H 0.1995 0.5437 0.4647 0.030 Uiso 1 1 calc R . . C61 C 0.3399(4) 0.5466(3) 0.5128(2) 0.0264(12) Uani 1 1 d . . . H61 H 0.3434 0.5079 0.5346 0.032 Uiso 1 1 calc R . . C62 C 0.4195(4) 0.5833(2) 0.5214(2) 0.0235(12) Uani 1 1 d . . . H62 H 0.4779 0.5689 0.5481 0.028 Uiso 1 1 calc R . . C63 C 0.6324(4) 0.6602(3) 0.4594(3) 0.0337(14) Uani 1 1 d . . . H63 H 0.5986 0.6283 0.4319 0.040 Uiso 1 1 calc R . . C64 C 0.7264(4) 0.6701(3) 0.4612(3) 0.0345(14) Uani 1 1 d . . . H64 H 0.7552 0.6448 0.4362 0.041 Uiso 1 1 calc R . . C65 C 0.7761(4) 0.7175(3) 0.5002(3) 0.0310(13) Uani 1 1 d . . . H65 H 0.8392 0.7250 0.5022 0.037 Uiso 1 1 calc R . . C66 C 0.7307(4) 0.7548(3) 0.5372(2) 0.0315(14) Uani 1 1 d . . . H66 H 0.7627 0.7877 0.5639 0.038 Uiso 1 1 calc R . . C67 C 0.6378(4) 0.7413(3) 0.5331(2) 0.0286(13) Uani 1 1 d . . . H67 H 0.6075 0.7660 0.5576 0.034 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 0.01119(10) 0.01484(10) 0.01653(11) -0.00036(7) 0.00314(7) 0.00034(7) U2 0.01246(10) 0.01643(11) 0.01489(10) 0.00147(7) 0.00335(7) -0.00006(7) Cl1 0.0216(7) 0.0165(6) 0.0278(7) 0.0017(5) 0.0069(5) 0.0010(5) Cl2 0.0210(7) 0.0235(7) 0.0185(6) -0.0018(5) 0.0065(5) 0.0014(5) Cl3 0.0142(6) 0.0223(7) 0.0285(7) -0.0028(5) 0.0032(5) -0.0036(5) Cl4 0.0239(7) 0.0211(7) 0.0249(7) 0.0072(5) 0.0002(5) -0.0007(5) Cl5 0.0169(7) 0.0251(7) 0.0279(7) 0.0040(5) -0.0004(5) -0.0060(5) O1 0.0111(18) 0.0229(19) 0.0227(18) -0.0035(14) 0.0058(14) -0.0010(15) O2 0.0135(19) 0.0194(18) 0.0206(18) -0.0008(14) 0.0040(14) 0.0016(15) O3 0.0136(18) 0.0195(18) 0.0212(18) -0.0004(14) 0.0060(14) 0.0026(15) O4 0.0142(19) 0.0165(18) 0.0242(18) -0.0008(13) 0.0090(14) 0.0004(14) O5 0.0126(18) 0.0235(19) 0.0232(19) 0.0027(14) 0.0059(14) 0.0016(15) O6 0.0170(19) 0.0191(18) 0.0133(17) -0.0001(13) 0.0051(14) 0.0010(14) N1 0.026(3) 0.019(2) 0.024(2) -0.0022(17) 0.011(2) 0.0025(19) N2 0.012(2) 0.023(2) 0.024(2) -0.0063(18) 0.0060(18) 0.0020(18) N3 0.011(2) 0.026(2) 0.027(2) -0.0039(18) 0.0042(18) 0.0033(19) N4 0.014(2) 0.026(2) 0.025(2) -0.0026(18) 0.0059(18) -0.0014(19) N5 0.021(3) 0.030(3) 0.037(3) 0.002(2) 0.002(2) -0.004(2) C1 0.014(3) 0.014(2) 0.012(2) 0.0042(18) 0.0010(19) 0.001(2) C2 0.015(3) 0.017(3) 0.013(2) 0.0033(19) 0.0004(19) -0.003(2) C3 0.013(3) 0.016(3) 0.021(3) 0.0027(19) 0.003(2) 0.004(2) C4 0.025(3) 0.022(3) 0.014(3) -0.0041(19) 0.003(2) -0.006(2) C5 0.015(3) 0.032(3) 0.021(3) -0.001(2) 0.004(2) -0.007(2) C6 0.013(3) 0.027(3) 0.024(3) 0.002(2) 0.008(2) -0.002(2) C7 0.016(3) 0.018(3) 0.026(3) -0.001(2) 0.009(2) 0.001(2) C8 0.014(3) 0.022(3) 0.016(3) -0.0058(19) 0.007(2) 0.004(2) C9 0.011(3) 0.021(3) 0.017(3) -0.0039(19) 0.006(2) 0.006(2) C10 0.014(3) 0.019(3) 0.022(3) -0.001(2) 0.011(2) 0.005(2) C11 0.024(3) 0.022(3) 0.027(3) 0.000(2) 0.016(2) 0.004(2) C12 0.020(3) 0.032(3) 0.023(3) 0.000(2) 0.005(2) 0.008(2) C13 0.021(3) 0.024(3) 0.016(3) -0.009(2) 0.009(2) 0.001(2) C14 0.021(3) 0.022(3) 0.018(3) 0.001(2) 0.009(2) -0.001(2) C15 0.016(3) 0.013(2) 0.021(3) -0.0004(19) 0.003(2) -0.004(2) C16 0.010(3) 0.012(2) 0.021(3) 0.0012(19) 0.001(2) 0.001(2) C17 0.019(3) 0.020(3) 0.012(2) -0.0038(19) 0.004(2) -0.005(2) C18 0.018(3) 0.015(3) 0.026(3) 0.001(2) 0.008(2) 0.004(2) C19 0.029(3) 0.019(3) 0.013(3) -0.0002(19) 0.003(2) 0.001(2) C20 0.028(3) 0.025(3) 0.018(3) -0.004(2) 0.008(2) -0.005(2) C21 0.013(3) 0.018(3) 0.015(2) 0.0052(19) 0.0041(19) 0.000(2) C22 0.018(3) 0.017(3) 0.010(2) 0.0033(18) 0.0034(19) -0.001(2) C23 0.015(3) 0.015(2) 0.010(2) 0.0030(18) 0.0030(19) -0.001(2) C24 0.017(3) 0.019(3) 0.017(3) 0.0002(19) 0.008(2) -0.002(2) C25 0.027(3) 0.015(3) 0.016(3) -0.0042(19) 0.006(2) 0.002(2) C26 0.015(3) 0.021(3) 0.022(3) -0.002(2) 0.004(2) -0.003(2) C27 0.009(3) 0.021(3) 0.025(3) 0.000(2) 0.003(2) -0.001(2) C28 0.013(3) 0.018(3) 0.022(3) 0.0017(19) 0.007(2) 0.003(2) C29 0.013(3) 0.021(3) 0.015(3) 0.0043(19) 0.0050(19) 0.009(2) C30 0.011(3) 0.023(3) 0.019(3) -0.0005(19) 0.008(2) 0.006(2) C31 0.017(3) 0.021(3) 0.013(2) 0.0029(19) 0.008(2) 0.004(2) C32 0.023(3) 0.021(3) 0.024(3) 0.004(2) 0.013(2) 0.006(2) C33 0.028(3) 0.028(3) 0.017(3) -0.001(2) 0.009(2) 0.005(2) C34 0.023(3) 0.021(3) 0.026(3) -0.005(2) 0.011(2) 0.002(2) C35 0.016(3) 0.022(3) 0.020(3) 0.001(2) 0.008(2) 0.000(2) C36 0.014(3) 0.015(3) 0.016(2) -0.0022(19) 0.007(2) 0.001(2) C37 0.013(3) 0.010(2) 0.024(3) 0.0008(19) 0.005(2) -0.002(2) C38 0.012(3) 0.019(3) 0.020(3) 0.000(2) 0.002(2) -0.002(2) C39 0.016(3) 0.019(3) 0.024(3) -0.002(2) 0.006(2) 0.003(2) C40 0.029(3) 0.015(3) 0.023(3) 0.005(2) 0.008(2) 0.001(2) C41 0.019(3) 0.022(3) 0.018(3) 0.000(2) 0.010(2) -0.004(2) C42 0.015(3) 0.016(3) 0.026(3) -0.001(2) 0.006(2) -0.003(2) C43 0.023(3) 0.030(3) 0.016(3) -0.001(2) 0.005(2) -0.002(2) C44 0.026(3) 0.036(3) 0.025(3) 0.003(2) 0.009(2) 0.005(3) C45 0.034(4) 0.044(4) 0.021(3) -0.006(2) 0.011(2) 0.003(3) C46 0.035(4) 0.056(4) 0.015(3) -0.006(3) 0.002(2) 0.002(3) C47 0.023(3) 0.040(3) 0.023(3) 0.007(2) 0.001(2) 0.006(3) C48 0.022(3) 0.023(3) 0.022(3) -0.003(2) 0.008(2) 0.001(2) C49 0.020(3) 0.017(3) 0.027(3) -0.006(2) 0.007(2) 0.002(2) C50 0.016(3) 0.021(3) 0.024(3) -0.005(2) 0.002(2) 0.000(2) C51 0.021(3) 0.024(3) 0.028(3) -0.006(2) 0.008(2) -0.010(2) C52 0.024(3) 0.022(3) 0.017(3) 0.002(2) 0.004(2) 0.002(2) C53 0.021(3) 0.022(3) 0.032(3) 0.004(2) 0.002(2) -0.001(2) C54 0.024(3) 0.022(3) 0.041(3) 0.005(2) 0.008(3) -0.005(2) C55 0.016(3) 0.029(3) 0.036(3) 0.000(2) 0.003(2) 0.003(2) C56 0.025(3) 0.020(3) 0.030(3) -0.005(2) 0.005(2) 0.001(2) C57 0.021(3) 0.026(3) 0.022(3) 0.000(2) 0.006(2) -0.001(2) C58 0.031(3) 0.021(3) 0.022(3) 0.003(2) 0.011(2) 0.008(2) C59 0.016(3) 0.031(3) 0.023(3) -0.003(2) 0.003(2) 0.003(2) C60 0.027(3) 0.028(3) 0.023(3) -0.005(2) 0.012(2) -0.007(2) C61 0.027(3) 0.026(3) 0.022(3) 0.007(2) 0.003(2) 0.000(3) C62 0.027(3) 0.025(3) 0.016(3) 0.003(2) 0.003(2) 0.005(2) C63 0.033(4) 0.027(3) 0.037(3) -0.009(2) 0.003(3) -0.006(3) C64 0.032(4) 0.035(3) 0.036(3) 0.000(3) 0.009(3) 0.001(3) C65 0.021(3) 0.033(3) 0.034(3) 0.010(2) -0.001(2) -0.009(3) C66 0.034(4) 0.030(3) 0.022(3) 0.000(2) -0.005(2) -0.009(3) C67 0.031(3) 0.034(3) 0.016(3) 0.001(2) 0.001(2) 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 U1 O1 2.123(3) . ? U1 O3 2.129(3) . ? U1 O2 2.236(3) . ? U1 Cl2 2.6699(11) . ? U1 Cl1 2.6891(12) . ? U1 Cl3 2.7072(12) . ? U2 O4 2.133(3) . ? U2 O6 2.142(3) . ? U2 O5 2.203(3) . ? U2 N1 2.579(4) . ? U2 Cl4 2.6658(12) . ? U2 Cl5 2.6999(12) . ? O1 C2 1.349(6) . ? O2 C9 1.369(5) . ? O3 C16 1.348(5) . ? O4 C23 1.358(5) . ? O5 C30 1.377(5) . ? O6 C37 1.355(5) . ? N1 C43 1.341(7) . ? N1 C47 1.343(6) . ? N2 C48 1.330(6) . ? N2 C52 1.349(6) . ? N3 C53 1.335(7) . ? N3 C57 1.341(6) . ? N4 C62 1.325(6) . ? N4 C58 1.345(6) . ? N5 C63 1.336(7) . ? N5 C67 1.350(7) . ? C1 C6 1.383(7) . ? C1 C2 1.410(7) . ? C1 C42 1.526(6) . ? C2 C3 1.394(7) . ? C3 C4 1.397(7) . ? C3 C7 1.523(7) . ? C4 C5 1.387(7) . ? C5 C6 1.400(7) . ? C7 C8 1.521(7) . ? C8 C13 1.385(7) . ? C8 C9 1.418(7) . ? C9 C10 1.409(7) . ? C10 C11 1.373(7) . ? C10 C14 1.534(7) . ? C11 C12 1.379(7) . ? C12 C13 1.377(7) . ? C14 C15 1.507(7) . ? C15 C20 1.383(7) . ? C15 C16 1.418(7) . ? C16 C17 1.402(7) . ? C17 C18 1.378(7) . ? C17 C21 1.528(6) . ? C18 C19 1.379(7) . ? C19 C20 1.392(7) . ? C21 C22 1.503(6) . ? C22 C23 1.400(7) . ? C22 C27 1.407(7) . ? C23 C24 1.407(6) . ? C24 C25 1.390(7) . ? C24 C28 1.522(7) . ? C25 C26 1.387(7) . ? C26 C27 1.380(7) . ? C28 C29 1.522(6) . ? C29 C34 1.387(6) . ? C29 C30 1.409(7) . ? C30 C31 1.400(7) . ? C31 C32 1.416(7) . ? C31 C35 1.510(7) . ? C32 C33 1.384(7) . ? C33 C34 1.388(7) . ? C35 C36 1.523(6) . ? C36 C41 1.388(6) . ? C36 C37 1.412(6) . ? C37 C38 1.406(7) . ? C38 C39 1.391(7) . ? C38 C42 1.507(7) . ? C39 C40 1.384(7) . ? C40 C41 1.381(7) . ? C43 C44 1.383(7) . ? C44 C45 1.380(7) . ? C45 C46 1.365(8) . ? C46 C47 1.382(8) . ? C48 C49 1.367(7) . ? C49 C50 1.383(7) . ? C50 C51 1.375(7) . ? C51 C52 1.374(7) . ? C53 C54 1.374(8) . ? C54 C55 1.393(7) . ? C55 C56 1.382(7) . ? C56 C57 1.360(7) . ? C58 C59 1.365(7) . ? C59 C60 1.370(7) . ? C60 C61 1.383(7) . ? C61 C62 1.371(7) . ? C63 C64 1.386(8) . ? C64 C65 1.365(8) . ? C65 C66 1.400(8) . ? C66 C67 1.372(8) . ? 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 O3 92.58(12) . . ? O1 U1 O2 83.92(12) . . ? O3 U1 O2 83.75(12) . . ? O1 U1 Cl2 90.46(9) . . ? O3 U1 Cl2 93.65(9) . . ? O2 U1 Cl2 173.68(9) . . ? O1 U1 Cl1 87.10(9) . . ? O3 U1 Cl1 173.49(9) . . ? O2 U1 Cl1 89.74(9) . . ? Cl2 U1 Cl1 92.86(4) . . ? O1 U1 Cl3 176.78(9) . . ? O3 U1 Cl3 89.97(9) . . ? O2 U1 Cl3 94.40(9) . . ? Cl2 U1 Cl3 91.35(4) . . ? Cl1 U1 Cl3 90.14(4) . . ? O4 U2 O6 93.13(12) . . ? O4 U2 O5 86.59(12) . . ? O6 U2 O5 86.61(12) . . ? O4 U2 N1 98.03(13) . . ? O6 U2 N1 94.15(12) . . ? O5 U2 N1 175.26(13) . . ? O4 U2 Cl4 89.48(9) . . ? O6 U2 Cl4 174.22(9) . . ? O5 U2 Cl4 88.39(9) . . ? N1 U2 Cl4 90.59(9) . . ? O4 U2 Cl5 173.86(9) . . ? O6 U2 Cl5 89.67(9) . . ? O5 U2 Cl5 88.12(9) . . ? N1 U2 Cl5 87.21(10) . . ? Cl4 U2 Cl5 87.25(4) . . ? C2 O1 U1 165.0(3) . . ? C9 O2 U1 126.3(3) . . ? C16 O3 U1 162.7(3) . . ? C23 O4 U2 167.0(3) . . ? C30 O5 U2 126.2(3) . . ? C37 O6 U2 166.8(3) . . ? C43 N1 C47 117.9(4) . . ? C43 N1 U2 123.4(3) . . ? C47 N1 U2 118.3(3) . . ? C48 N2 C52 121.8(4) . . ? C53 N3 C57 122.5(4) . . ? C62 N4 C58 121.8(5) . . ? C63 N5 C67 117.2(5) . . ? C6 C1 C2 118.1(4) . . ? C6 C1 C42 124.8(4) . . ? C2 C1 C42 117.1(4) . . ? O1 C2 C3 119.7(4) . . ? O1 C2 C1 118.2(4) . . ? C3 C2 C1 122.2(4) . . ? C2 C3 C4 117.8(4) . . ? C2 C3 C7 120.5(4) . . ? C4 C3 C7 121.7(4) . . ? C5 C4 C3 121.2(4) . . ? C4 C5 C6 119.7(5) . . ? C1 C6 C5 120.9(5) . . ? C8 C7 C3 111.3(4) . . ? C13 C8 C9 119.3(4) . . ? C13 C8 C7 118.5(4) . . ? C9 C8 C7 122.1(4) . . ? O2 C9 C10 120.6(4) . . ? O2 C9 C8 120.3(4) . . ? C10 C9 C8 119.0(4) . . ? C11 C10 C9 118.6(5) . . ? C11 C10 C14 119.2(4) . . ? C9 C10 C14 122.1(4) . . ? C10 C11 C12 122.3(5) . . ? C11 C12 C13 119.2(5) . . ? C12 C13 C8 120.9(5) . . ? C15 C14 C10 111.1(4) . . ? C20 C15 C16 116.8(4) . . ? C20 C15 C14 123.4(4) . . ? C16 C15 C14 119.8(4) . . ? O3 C16 C17 118.8(4) . . ? O3 C16 C15 119.2(4) . . ? C17 C16 C15 122.0(4) . . ? C18 C17 C16 118.4(4) . . ? C18 C17 C21 124.8(4) . . ? C16 C17 C21 116.8(4) . . ? C17 C18 C19 121.0(5) . . ? C18 C19 C20 120.0(5) . . ? C15 C20 C19 121.7(5) . . ? C22 C21 C17 117.9(4) . . ? C23 C22 C27 117.7(4) . . ? C23 C22 C21 121.5(4) . . ? C27 C22 C21 120.2(4) . . ? O4 C23 C22 119.0(4) . . ? O4 C23 C24 119.4(4) . . ? C22 C23 C24 121.6(4) . . ? C25 C24 C23 117.8(4) . . ? C25 C24 C28 120.6(4) . . ? C23 C24 C28 121.6(4) . . ? C24 C25 C26 122.1(4) . . ? C27 C26 C25 118.9(5) . . ? C26 C27 C22 121.7(5) . . ? C29 C28 C24 112.5(4) . . ? C34 C29 C30 117.9(4) . . ? C34 C29 C28 120.9(4) . . ? C30 C29 C28 121.2(4) . . ? O5 C30 C31 118.9(4) . . ? O5 C30 C29 119.1(4) . . ? C31 C30 C29 122.0(4) . . ? C30 C31 C32 117.3(4) . . ? C30 C31 C35 122.1(4) . . ? C32 C31 C35 120.3(4) . . ? C33 C32 C31 121.0(5) . . ? C32 C33 C34 119.8(5) . . ? C33 C34 C29 121.5(5) . . ? C31 C35 C36 112.1(4) . . ? C41 C36 C37 117.9(4) . . ? C41 C36 C35 121.1(4) . . ? C37 C36 C35 121.0(4) . . ? O6 C37 C38 119.4(4) . . ? O6 C37 C36 119.4(4) . . ? C38 C37 C36 121.2(4) . . ? C39 C38 C37 118.4(4) . . ? C39 C38 C42 120.0(4) . . ? C37 C38 C42 121.4(4) . . ? C40 C39 C38 121.0(5) . . ? C41 C40 C39 120.0(4) . . ? C40 C41 C36 121.5(4) . . ? C38 C42 C1 119.1(4) . . ? N1 C43 C44 122.8(5) . . ? C43 C44 C45 118.1(5) . . ? C46 C45 C44 120.0(5) . . ? C45 C46 C47 118.8(5) . . ? N1 C47 C46 122.4(5) . . ? N2 C48 C49 120.5(5) . . ? C48 C49 C50 119.0(5) . . ? C51 C50 C49 119.8(5) . . ? C52 C51 C50 119.3(5) . . ? N2 C52 C51 119.6(5) . . ? N3 C53 C54 119.9(5) . . ? C53 C54 C55 118.7(5) . . ? C56 C55 C54 119.3(5) . . ? C57 C56 C55 119.9(5) . . ? N3 C57 C56 119.6(5) . . ? N4 C58 C59 119.9(5) . . ? C58 C59 C60 119.5(5) . . ? C59 C60 C61 119.5(5) . . ? C62 C61 C60 119.0(5) . . ? N4 C62 C61 120.3(5) . . ? N5 C63 C64 123.2(5) . . ? C65 C64 C63 118.9(6) . . ? C64 C65 C66 119.1(6) . . ? C67 C66 C65 118.1(5) . . ? N5 C67 C66 123.4(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O2 1.08 1.65 2.709(5) 166.4 . N3 H3 O5 0.90 1.79 2.679(5) 170.0 . N4 H4 N5 0.94 1.86 2.793(6) 171.6 . #===END data_7.8py _database_code_depnum_ccdc_archive 'CCDC 603337' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C202 H172 Cl6 N18 O16 U5' _chemical_formula_weight 4510.43 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' O O 0.0106 0.0060 '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' 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/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 21.4083(15) _cell_length_b 27.4775(13) _cell_length_c 18.5799(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.243(4) _cell_angle_gamma 90.00 _cell_volume 10438.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 148163 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method ? _exptl_crystal_F_000 4400 _exptl_absorpt_coefficient_mu 4.002 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.505 _exptl_absorpt_correction_T_max 0.619 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 50 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 'one \f and five \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 148163 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.1468 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.68 _reflns_number_total 19622 _reflns_number_gt 9919 _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. The crystal being very weakly diffracting, the rather low data quality did not permit to get a very satisfying structure determination. The pyridine solvent molecules in particular are very badly resolved. Three pyridine molecules were refined as idealized hexagons. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for the most badly behaving ones. The H atoms were introduced at calculated positions (except for the hydroxylic one (O5), which was not found, nor introduced) 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. Some short H...H contacts involving the solvent molecules are likely due to their imperfect location. Some voids in the lattice indicate the presence of other, unresolved solvent molecules. 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^)+(0.1177P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19622 _refine_ls_number_parameters 1078 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1644 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2096 _refine_ls_wR_factor_gt 0.1781 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.675 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.171 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 0.0000 0.0000 0.0000 0.0518(2) Uani 1 2 d S . . U2 U 0.32519(2) -0.130390(14) -0.00165(3) 0.04662(16) Uani 1 1 d . . . U3 U 0.35795(2) -0.041349(17) 0.27671(3) 0.05683(18) Uani 1 1 d . . . Cl1 Cl 0.30547(14) -0.08398(10) 0.12223(17) 0.0549(8) Uani 1 1 d . . . Cl2 Cl 0.46273(16) 0.00712(12) 0.2635(2) 0.0698(9) Uani 1 1 d . . . Cl3 Cl 0.3158(2) 0.02384(18) 0.3589(3) 0.0752(14) Uani 1 1 d . . . O1 O 0.0603(4) -0.0064(3) 0.1123(5) 0.054(2) Uani 1 1 d . . . O2 O -0.0270(4) 0.0700(3) 0.0316(5) 0.054(2) Uani 1 1 d . . . O3 O 0.0749(4) 0.0368(2) -0.0341(5) 0.054(2) Uani 1 1 d . . . O4 O 0.2567(3) -0.0870(2) -0.0815(4) 0.0460(18) Uani 1 1 d . . . O5 O 0.3320(4) -0.1812(2) -0.0927(4) 0.049(2) Uani 1 1 d . . . O6 O 0.4261(4) -0.1450(2) 0.0522(4) 0.0481(19) Uani 1 1 d . . . O7 O 0.4106(4) -0.1041(3) 0.2759(4) 0.060(2) Uani 1 1 d . . . O8 O 0.2783(4) -0.0845(3) 0.2803(4) 0.055(2) Uani 1 1 d . . . C1 C 0.1184(6) -0.0488(4) 0.2230(7) 0.057(3) Uani 1 1 d . . . C2 C 0.0748(6) -0.0119(4) 0.1885(8) 0.058(3) Uani 1 1 d . . . C3 C 0.0445(6) 0.0202(5) 0.2288(7) 0.059(3) Uani 1 1 d . . . C4 C 0.0601(8) 0.0130(6) 0.3055(10) 0.092(5) Uani 1 1 d . . . H4 H 0.0411 0.0336 0.3328 0.110 Uiso 1 1 calc R . . C5 C 0.1033(8) -0.0237(6) 0.3458(9) 0.092(5) Uani 1 1 d . . . H5 H 0.1128 -0.0277 0.3977 0.110 Uiso 1 1 calc R . . C6 C 0.1312(8) -0.0541(6) 0.3010(9) 0.090(5) Uani 1 1 d . . . H6 H 0.1594 -0.0788 0.3250 0.108 Uiso 1 1 calc R . . C7 C -0.0037(6) 0.0598(5) 0.1876(8) 0.067(4) Uani 1 1 d . . . H7A H -0.0384 0.0443 0.1484 0.080 Uiso 1 1 calc R . . H7B H -0.0235 0.0743 0.2232 0.080 Uiso 1 1 calc R . . C8 C 0.0250(6) 0.0994(4) 0.1527(9) 0.065(4) Uani 1 1 d . . . C9 C 0.0157(6) 0.1023(4) 0.0765(8) 0.055(3) Uani 1 1 d . . . C10 C 0.0464(6) 0.1373(4) 0.0429(9) 0.063(4) Uani 1 1 d . . . C11 C 0.0863(7) 0.1715(5) 0.0908(9) 0.070(4) Uani 1 1 d . . . H11 H 0.1055 0.1961 0.0704 0.084 Uiso 1 1 calc R . . C12 C 0.0972(7) 0.1694(5) 0.1638(10) 0.086(4) Uani 1 1 d . . . H12 H 0.1241 0.1927 0.1941 0.103 Uiso 1 1 calc R . . C13 C 0.0691(7) 0.1328(5) 0.1980(9) 0.079(4) Uani 1 1 d . . . H13 H 0.0799 0.1309 0.2502 0.095 Uiso 1 1 calc R . . C14 C 0.0379(6) 0.1379(5) -0.0376(8) 0.068(4) Uani 1 1 d . . . H14A H 0.0292 0.1710 -0.0560 0.082 Uiso 1 1 calc R . . H14B H 0.0002 0.1183 -0.0629 0.082 Uiso 1 1 calc R . . C15 C 0.0984(7) 0.1185(5) -0.0577(9) 0.076(4) Uani 1 1 d . . . C16 C 0.1138(6) 0.0689(4) -0.0516(7) 0.060(3) Uani 1 1 d . . . C17 C 0.1720(6) 0.0530(5) -0.0644(8) 0.067(4) Uani 1 1 d . . . C18 C 0.2144(7) 0.0888(5) -0.0820(9) 0.086(4) Uani 1 1 d . . . H18 H 0.2535 0.0786 -0.0892 0.103 Uiso 1 1 calc R . . C19 C 0.1993(8) 0.1373(5) -0.0884(10) 0.090(5) Uani 1 1 d . . . H19 H 0.2274 0.1598 -0.0997 0.108 Uiso 1 1 calc R . . C20 C 0.1391(7) 0.1522(5) -0.0770(9) 0.082(4) Uani 1 1 d . . . H20 H 0.1270 0.1848 -0.0826 0.098 Uiso 1 1 calc R . . C21 C 0.1910(6) 0.0005(4) -0.0603(7) 0.054(3) Uani 1 1 d . . . H21A H 0.2361 -0.0027 -0.0294 0.064 Uiso 1 1 calc R . . H21B H 0.1640 -0.0174 -0.0356 0.064 Uiso 1 1 calc R . . C22 C 0.1839(6) -0.0219(4) -0.1352(7) 0.056(3) Uani 1 1 d . . . C23 C 0.2169(6) -0.0650(4) -0.1427(7) 0.053(3) Uani 1 1 d . . . C24 C 0.2096(6) -0.0864(4) -0.2136(7) 0.050(3) Uani 1 1 d . . . C25 C 0.1656(7) -0.0636(6) -0.2774(8) 0.071(4) Uani 1 1 d . . . H25 H 0.1585 -0.0774 -0.3249 0.085 Uiso 1 1 calc R . . C26 C 0.1339(7) -0.0224(6) -0.2701(8) 0.072(4) Uani 1 1 d . . . H26 H 0.1060 -0.0081 -0.3131 0.086 Uiso 1 1 calc R . . C27 C 0.1413(7) -0.0012(5) -0.2023(9) 0.075(4) Uani 1 1 d . . . H27 H 0.1185 0.0272 -0.1995 0.089 Uiso 1 1 calc R . . C28 C 0.2455(6) -0.1306(4) -0.2229(7) 0.055(3) Uani 1 1 d . . . H28A H 0.2318 -0.1394 -0.2758 0.066 Uiso 1 1 calc R . . H28B H 0.2328 -0.1569 -0.1954 0.066 Uiso 1 1 calc R . . C29 C 0.3198(6) -0.1268(4) -0.1968(8) 0.055(3) Uani 1 1 d . . . C30 C 0.3590(6) -0.1540(4) -0.1349(7) 0.050(3) Uani 1 1 d . . . C31 C 0.4287(7) -0.1519(4) -0.1185(7) 0.059(3) Uani 1 1 d . . . C32 C 0.4554(7) -0.1209(4) -0.1619(8) 0.058(3) Uani 1 1 d . . . H32 H 0.5006 -0.1189 -0.1513 0.069 Uiso 1 1 calc R . . C33 C 0.4167(7) -0.0940(4) -0.2190(7) 0.059(3) Uani 1 1 d . . . H33 H 0.4361 -0.0731 -0.2454 0.071 Uiso 1 1 calc R . . C34 C 0.3497(7) -0.0966(4) -0.2392(8) 0.063(4) Uani 1 1 d . . . H34 H 0.3243 -0.0788 -0.2800 0.075 Uiso 1 1 calc R . . C35 C 0.4706(6) -0.1887(4) -0.0636(8) 0.061(4) Uani 1 1 d . . . H35A H 0.4414 -0.2125 -0.0522 0.073 Uiso 1 1 calc R . . H35B H 0.4971 -0.2059 -0.0897 0.073 Uiso 1 1 calc R . . C36 C 0.5149(6) -0.1713(4) 0.0088(8) 0.059(4) Uani 1 1 d . . . C37 C 0.4896(7) -0.1519(4) 0.0680(8) 0.055(3) Uani 1 1 d . . . C38 C 0.5333(6) -0.1418(4) 0.1407(8) 0.050(3) Uani 1 1 d . . . C39 C 0.5986(6) -0.1468(4) 0.1533(8) 0.064(4) Uani 1 1 d . . . H39 H 0.6265 -0.1385 0.2004 0.076 Uiso 1 1 calc R . . C40 C 0.6256(7) -0.1637(5) 0.0987(9) 0.078(4) Uani 1 1 d . . . H40 H 0.6706 -0.1670 0.1088 0.093 Uiso 1 1 calc R . . C41 C 0.5839(7) -0.1755(5) 0.0292(9) 0.071(4) Uani 1 1 d . . . H41 H 0.6022 -0.1872 -0.0070 0.085 Uiso 1 1 calc R . . C42 C 0.5033(6) -0.1248(4) 0.2010(7) 0.059(3) Uani 1 1 d . . . H42A H 0.4718 -0.0993 0.1801 0.071 Uiso 1 1 calc R . . H42B H 0.5374 -0.1109 0.2425 0.071 Uiso 1 1 calc R . . C43 C 0.4691(6) -0.1653(4) 0.2314(7) 0.051(3) Uani 1 1 d . . . C44 C 0.4240(6) -0.1528(5) 0.2690(7) 0.058(3) Uani 1 1 d . . . C45 C 0.3929(6) -0.1864(4) 0.2995(8) 0.062(4) Uani 1 1 d . . . C46 C 0.4068(7) -0.2358(5) 0.2928(8) 0.074(4) Uani 1 1 d . . . H46 H 0.3870 -0.2593 0.3147 0.089 Uiso 1 1 calc R . . C47 C 0.4491(6) -0.2496(5) 0.2545(8) 0.067(4) Uani 1 1 d . . . H47 H 0.4569 -0.2823 0.2476 0.081 Uiso 1 1 calc R . . C48 C 0.4809(6) -0.2128(5) 0.2254(7) 0.060(3) Uani 1 1 d . . . H48 H 0.5112 -0.2219 0.2010 0.072 Uiso 1 1 calc R . . C49 C 0.3460(7) -0.1729(5) 0.3450(8) 0.073(4) Uani 1 1 d . . . H49A H 0.3505 -0.1965 0.3851 0.088 Uiso 1 1 calc R . . H49B H 0.3582 -0.1413 0.3682 0.088 Uiso 1 1 calc R . . C50 C 0.2751(6) -0.1713(4) 0.2968(7) 0.051(3) Uani 1 1 d . . . C51 C 0.2442(7) -0.1269(5) 0.2643(7) 0.060(3) Uani 1 1 d . . . C52 C 0.1778(6) -0.1274(4) 0.2142(7) 0.058(3) Uani 1 1 d . . . C53 C 0.1457(6) -0.1727(5) 0.2068(8) 0.066(4) Uani 1 1 d . . . H53 H 0.1025 -0.1743 0.1767 0.080 Uiso 1 1 calc R . . C54 C 0.1740(8) -0.2141(5) 0.2410(8) 0.068(4) Uani 1 1 d . . . H54 H 0.1500 -0.2428 0.2356 0.081 Uiso 1 1 calc R . . C55 C 0.2391(6) -0.2133(5) 0.2842(7) 0.061(3) Uani 1 1 d . . . H55 H 0.2589 -0.2422 0.3052 0.073 Uiso 1 1 calc R . . C56 C 0.1476(6) -0.0815(4) 0.1785(7) 0.054(3) Uani 1 1 d . . . H56A H 0.1808 -0.0632 0.1640 0.065 Uiso 1 1 calc R . . H56B H 0.1137 -0.0898 0.1325 0.065 Uiso 1 1 calc R . . N1 N 0.3288(5) -0.2142(3) 0.0694(6) 0.055(3) Uani 1 1 d . . . C57 C 0.2917(7) -0.2244(5) 0.1165(7) 0.068(4) Uani 1 1 d . . . H57 H 0.2709 -0.1993 0.1340 0.081 Uiso 1 1 calc R . . C58 C 0.2853(7) -0.2719(5) 0.1381(8) 0.075(4) Uani 1 1 d . . . H58 H 0.2589 -0.2787 0.1686 0.089 Uiso 1 1 calc R . . C59 C 0.3180(7) -0.3095(5) 0.1144(8) 0.077(4) Uani 1 1 d . . . H59 H 0.3138 -0.3415 0.1290 0.092 Uiso 1 1 calc R . . C60 C 0.3552(6) -0.2991(5) 0.0706(7) 0.061(3) Uani 1 1 d . . . H60 H 0.3785 -0.3234 0.0548 0.074 Uiso 1 1 calc R . . C61 C 0.3585(6) -0.2500(4) 0.0486(8) 0.067(4) Uani 1 1 d . . . H61 H 0.3838 -0.2431 0.0169 0.081 Uiso 1 1 calc R . . N2 N 0.2103(5) -0.1718(3) -0.0264(6) 0.055(3) Uani 1 1 d . . . C62 C 0.1659(6) -0.1532(5) 0.0060(7) 0.063(3) Uani 1 1 d . . . H62 H 0.1760 -0.1246 0.0339 0.075 Uiso 1 1 calc R . . C63 C 0.1072(6) -0.1752(5) -0.0013(7) 0.066(4) Uani 1 1 d . . . H63 H 0.0793 -0.1633 0.0246 0.080 Uiso 1 1 calc R . . C64 C 0.0895(6) -0.2162(5) -0.0486(8) 0.067(4) Uani 1 1 d . . . H64 H 0.0490 -0.2312 -0.0563 0.081 Uiso 1 1 calc R . . C65 C 0.1340(6) -0.2335(5) -0.0830(7) 0.065(4) Uani 1 1 d . . . H65 H 0.1239 -0.2604 -0.1146 0.078 Uiso 1 1 calc R . . C66 C 0.1931(6) -0.2107(4) -0.0704(7) 0.057(3) Uani 1 1 d . . . H66 H 0.2227 -0.2230 -0.0936 0.068 Uiso 1 1 calc R . . N3 N 0.3840(5) -0.0472(3) -0.0070(6) 0.049(2) Uani 1 1 d . . . C67 C 0.3699(6) -0.0215(4) -0.0723(7) 0.055(3) Uani 1 1 d . . . H67 H 0.3433 -0.0350 -0.1167 0.067 Uiso 1 1 calc R . . C68 C 0.3956(6) 0.0260(4) -0.0726(8) 0.056(3) Uani 1 1 d . . . H68 H 0.3860 0.0440 -0.1169 0.068 Uiso 1 1 calc R . . C69 C 0.4336(7) 0.0445(4) -0.0086(9) 0.065(4) Uani 1 1 d . . . H69 H 0.4508 0.0755 -0.0092 0.077 Uiso 1 1 calc R . . C70 C 0.4484(6) 0.0200(4) 0.0577(7) 0.052(3) Uani 1 1 d . . . H70 H 0.4743 0.0339 0.1022 0.062 Uiso 1 1 calc R . . C71 C 0.4232(6) -0.0267(5) 0.0563(8) 0.060(3) Uani 1 1 d . . . H71 H 0.4338 -0.0445 0.1008 0.072 Uiso 1 1 calc R . . N4 N 0.2977(5) 0.0255(4) 0.1837(6) 0.063(3) Uani 1 1 d . . . C72 C 0.2343(7) 0.0368(5) 0.1774(8) 0.071(4) Uani 1 1 d . . . H72 H 0.2125 0.0167 0.2023 0.085 Uiso 1 1 calc R . . C73 C 0.2018(7) 0.0728(5) 0.1403(8) 0.074(4) Uani 1 1 d . . . H73 H 0.1592 0.0785 0.1412 0.089 Uiso 1 1 calc R . . C74 C 0.2292(8) 0.1026(6) 0.0998(10) 0.101(5) Uani 1 1 d . . . H74 H 0.2068 0.1288 0.0722 0.121 Uiso 1 1 calc R . . C75 C 0.2942(10) 0.0911(8) 0.1022(12) 0.132(7) Uani 1 1 d . . . H75 H 0.3151 0.1084 0.0730 0.159 Uiso 1 1 calc R . . C76 C 0.3254(7) 0.0549(6) 0.1475(9) 0.085(4) Uani 1 1 d . . . H76 H 0.3697 0.0506 0.1532 0.102 Uiso 1 1 calc R . . N5 N 0.4263(6) -0.0520(4) 0.4177(6) 0.060(4) Uani 1 1 d GU . . C77 C 0.4892(7) -0.0656(5) 0.4192(7) 0.061(7) Uani 1 1 d GU . . H77 H 0.5000 -0.0683 0.3745 0.073 Uiso 1 1 calc R . . C78 C 0.5360(6) -0.0751(6) 0.4876(9) 0.077(8) Uani 1 1 d GU . . H78 H 0.5781 -0.0842 0.4886 0.092 Uiso 1 1 calc R . . C79 C 0.5198(7) -0.0710(5) 0.5545(6) 0.084(7) Uani 1 1 d GU . . H79 H 0.5511 -0.0774 0.6003 0.101 Uiso 1 1 calc R . . C80 C 0.4569(8) -0.0575(6) 0.5530(6) 0.068(7) Uani 1 1 d GU . . H80 H 0.4461 -0.0547 0.5978 0.082 Uiso 1 1 calc R . . C81 C 0.4101(6) -0.0480(5) 0.4846(8) 0.098(10) Uani 1 1 d GU . . H81 H 0.3680 -0.0389 0.4836 0.117 Uiso 1 1 calc R . . N6 N 0.0033(6) 0.7579(4) 0.6009(7) 0.087(5) Uani 1 1 d GU . . C82 C 0.0388(7) 0.7967(5) 0.5852(6) 0.092(7) Uani 1 1 d GU . . H82 H 0.0440 0.7999 0.5375 0.110 Uiso 1 1 calc R . . C83 C 0.0666(6) 0.8307(4) 0.6409(8) 0.118(6) Uani 1 1 d GU . . H83 H 0.0903 0.8567 0.6304 0.142 Uiso 1 1 calc R . . C84 C 0.0588(5) 0.8259(4) 0.7122(6) 0.101(5) Uani 1 1 d GU . . H84 H 0.0774 0.8486 0.7495 0.122 Uiso 1 1 calc R . . C85 C 0.0233(6) 0.7871(5) 0.7279(6) 0.089(5) Uani 1 1 d GU . . H85 H 0.0181 0.7838 0.7756 0.107 Uiso 1 1 calc R . . C86 C -0.0044(5) 0.7530(4) 0.6722(8) 0.079(6) Uani 1 1 d GU . . H86 H -0.0282 0.7271 0.6827 0.095 Uiso 1 1 calc R . . N7 N 0.1788(6) -0.1089(5) 0.5553(7) 0.098(4) Uani 1 1 d U . . C87 C 0.1742(8) -0.1419(6) 0.4997(10) 0.097(5) Uani 1 1 d U . . H87 H 0.1454 -0.1678 0.4958 0.116 Uiso 1 1 calc R . . C88 C 0.2087(8) -0.1398(6) 0.4496(9) 0.092(5) Uani 1 1 d U . . H88 H 0.2031 -0.1631 0.4119 0.110 Uiso 1 1 calc R . . C89 C 0.2531(9) -0.1014(7) 0.4561(10) 0.104(5) Uani 1 1 d U . . H89 H 0.2775 -0.0988 0.4223 0.125 Uiso 1 1 calc R . . C90 C 0.2608(7) -0.0674(5) 0.5128(7) 0.093(4) Uani 1 1 d U . . H90 H 0.2916 -0.0426 0.5200 0.112 Uiso 1 1 calc R . . C91 C 0.2201(8) -0.0721(7) 0.5584(9) 0.098(5) Uani 1 1 d U . . H91 H 0.2217 -0.0477 0.5937 0.117 Uiso 1 1 calc R . . N8 N 0.6533(7) -0.0317(5) 0.2943(9) 0.061(5) Uani 1 1 d GU . . C92 C 0.7121(8) -0.0393(5) 0.2787(8) 0.075(6) Uani 1 1 d GU . . H92 H 0.7179 -0.0273 0.2343 0.091 Uiso 1 1 calc R . . C93 C 0.7623(7) -0.0649(7) 0.3293(11) 0.136(10) Uani 1 1 d GU . . H93 H 0.8016 -0.0700 0.3188 0.164 Uiso 1 1 calc R . . C94 C 0.7536(10) -0.0828(9) 0.3956(11) 0.13(2) Uani 1 1 d GU . . H94 H 0.7872 -0.0999 0.4295 0.155 Uiso 1 1 calc R . . C95 C 0.6948(11) -0.0752(8) 0.4113(9) 0.100(17) Uani 1 1 d GU . . H95 H 0.6890 -0.0872 0.4557 0.119 Uiso 1 1 calc R . . C96 C 0.6446(8) -0.0497(7) 0.3607(10) 0.124(9) Uani 1 1 d GU . . H96 H 0.6053 -0.0446 0.3712 0.149 Uiso 1 1 calc R . . N9 N 0.9930(12) 0.3213(8) 0.1186(13) 0.078(7) Uani 1 1 d U . . C97 C 0.9756(14) 0.3546(10) 0.1638(16) 0.117(9) Uani 1 1 d U . . H97 H 0.9319 0.3586 0.1615 0.140 Uiso 1 1 calc R . . C98 C 1.0225(10) 0.3819(7) 0.2121(11) 0.072(5) Uani 1 1 d U . . H98 H 1.0102 0.4104 0.2313 0.087 Uiso 1 1 calc R . . C99 C 1.0841(18) 0.3696(12) 0.233(2) 0.097(10) Uani 1 1 d U . . H99 H 1.1140 0.3849 0.2730 0.117 Uiso 1 1 calc R . . C100 C 1.1046(19) 0.3326(13) 0.192(2) 0.111(11) Uani 1 1 d U . . H100 H 1.1481 0.3234 0.2023 0.133 Uiso 1 1 calc R . . C101 C 1.0561(13) 0.3115(8) 0.1360(14) 0.101(7) Uani 1 1 d U . . H101 H 1.0687 0.2878 0.1073 0.121 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 0.0564(4) 0.0384(4) 0.0707(5) 0.0008(3) 0.0341(4) 0.0026(3) U2 0.0523(3) 0.0356(3) 0.0580(3) -0.0013(2) 0.0256(2) -0.0005(2) U3 0.0602(3) 0.0525(3) 0.0615(3) -0.0007(2) 0.0237(3) -0.0032(2) Cl1 0.0589(19) 0.0525(18) 0.0579(19) -0.0035(15) 0.0246(16) -0.0007(15) Cl2 0.063(2) 0.066(2) 0.081(2) -0.0021(18) 0.0232(19) -0.0114(17) Cl3 0.075(3) 0.076(3) 0.081(3) -0.019(3) 0.031(3) 0.002(3) O1 0.065(5) 0.046(5) 0.064(6) 0.001(4) 0.036(5) -0.001(4) O2 0.059(5) 0.042(5) 0.072(6) 0.004(4) 0.039(5) 0.018(4) O3 0.053(5) 0.037(4) 0.084(6) 0.010(4) 0.038(5) 0.000(4) O4 0.052(5) 0.043(4) 0.046(5) 0.005(4) 0.019(4) 0.005(4) O5 0.063(5) 0.037(4) 0.055(5) -0.015(4) 0.029(4) -0.016(4) O6 0.037(5) 0.041(4) 0.067(5) -0.005(4) 0.017(4) 0.008(3) O7 0.072(6) 0.049(5) 0.060(5) 0.005(4) 0.020(5) 0.002(4) O8 0.071(5) 0.043(5) 0.056(5) -0.002(4) 0.027(4) -0.009(4) C1 0.048(8) 0.064(9) 0.061(9) 0.000(7) 0.020(7) 0.004(7) C2 0.063(9) 0.052(8) 0.069(10) -0.014(7) 0.033(8) -0.004(7) C3 0.061(8) 0.077(9) 0.042(8) -0.011(7) 0.020(7) 0.008(7) C4 0.092(8) 0.090(8) 0.101(9) -0.016(7) 0.041(7) 0.022(7) C5 0.102(8) 0.106(8) 0.076(8) 0.002(7) 0.039(7) 0.033(7) C6 0.094(8) 0.090(8) 0.088(8) -0.004(7) 0.029(7) 0.014(7) C7 0.073(7) 0.062(7) 0.081(7) -0.011(6) 0.047(6) 0.008(6) C8 0.060(9) 0.038(7) 0.100(12) -0.016(8) 0.030(8) -0.002(6) C9 0.055(8) 0.043(8) 0.077(10) -0.009(7) 0.035(8) -0.001(6) C10 0.042(7) 0.048(8) 0.103(12) 0.013(8) 0.026(8) 0.012(6) C11 0.070(7) 0.050(6) 0.093(8) 0.000(6) 0.031(6) -0.001(6) C12 0.077(8) 0.064(7) 0.107(9) -0.021(7) 0.012(7) -0.001(6) C13 0.082(8) 0.072(7) 0.084(8) -0.015(7) 0.028(7) 0.004(6) C14 0.067(7) 0.055(7) 0.091(8) 0.012(6) 0.036(6) 0.005(5) C15 0.064(7) 0.076(8) 0.096(8) 0.006(6) 0.037(6) -0.009(6) C16 0.078(10) 0.042(7) 0.071(9) 0.011(6) 0.039(8) 0.013(7) C17 0.056(8) 0.059(9) 0.098(11) 0.000(8) 0.042(8) 0.002(7) C18 0.082(8) 0.077(8) 0.110(9) 0.000(7) 0.046(7) 0.012(7) C19 0.084(8) 0.072(8) 0.126(9) 0.014(7) 0.050(7) 0.001(6) C20 0.074(7) 0.069(7) 0.112(9) 0.013(7) 0.044(7) 0.006(6) C21 0.062(8) 0.041(7) 0.074(9) 0.009(6) 0.046(7) 0.007(6) C22 0.053(8) 0.053(8) 0.070(10) 0.025(7) 0.032(7) 0.005(6) C23 0.060(8) 0.045(7) 0.064(10) 0.009(7) 0.035(7) -0.002(6) C24 0.059(8) 0.051(7) 0.050(8) 0.005(7) 0.033(7) -0.007(6) C25 0.082(10) 0.086(11) 0.055(9) -0.001(8) 0.034(8) -0.015(9) C26 0.066(10) 0.089(11) 0.059(10) 0.018(9) 0.018(8) 0.014(8) C27 0.063(9) 0.094(11) 0.070(11) 0.010(9) 0.024(8) 0.006(8) C28 0.060(8) 0.053(8) 0.057(8) -0.013(6) 0.027(7) -0.015(6) C29 0.060(9) 0.046(7) 0.070(9) -0.024(7) 0.034(8) -0.019(7) C30 0.055(8) 0.044(7) 0.061(9) -0.009(7) 0.032(7) -0.004(6) C31 0.082(10) 0.033(7) 0.070(9) -0.020(7) 0.034(8) 0.005(7) C32 0.068(9) 0.048(8) 0.071(10) -0.009(7) 0.040(8) -0.014(7) C33 0.082(11) 0.050(8) 0.055(9) -0.011(7) 0.036(8) -0.019(7) C34 0.074(10) 0.053(8) 0.078(10) -0.025(7) 0.047(8) -0.025(7) C35 0.064(9) 0.041(7) 0.092(11) -0.024(7) 0.045(8) -0.013(6) C36 0.051(8) 0.036(7) 0.100(11) 0.005(7) 0.039(8) 0.007(6) C37 0.061(9) 0.036(7) 0.077(10) 0.005(7) 0.034(8) 0.008(6) C38 0.038(7) 0.030(6) 0.084(10) 0.002(6) 0.020(7) -0.005(5) C39 0.055(9) 0.054(8) 0.079(10) -0.003(7) 0.016(8) -0.023(6) C40 0.056(9) 0.087(11) 0.100(12) 0.000(9) 0.039(9) 0.017(8) C41 0.067(7) 0.068(7) 0.088(8) 0.006(6) 0.035(6) 0.000(6) C42 0.054(8) 0.051(8) 0.072(9) 0.000(7) 0.017(7) 0.004(6) C43 0.059(8) 0.042(8) 0.052(8) 0.005(6) 0.017(7) -0.003(6) C44 0.062(8) 0.055(8) 0.055(8) 0.021(7) 0.014(7) -0.010(7) C45 0.056(8) 0.049(8) 0.089(10) 0.024(7) 0.033(8) 0.006(6) C46 0.072(7) 0.079(8) 0.077(8) 0.017(6) 0.030(6) 0.007(6) C47 0.061(9) 0.046(8) 0.095(11) 0.006(7) 0.023(8) -0.007(6) C48 0.047(8) 0.065(9) 0.070(9) 0.006(7) 0.022(7) 0.004(7) C49 0.093(12) 0.053(8) 0.085(10) 0.036(7) 0.044(9) 0.001(7) C50 0.059(8) 0.050(8) 0.055(8) 0.015(6) 0.034(7) 0.002(7) C51 0.067(9) 0.064(9) 0.058(9) -0.003(7) 0.035(7) -0.002(8) C52 0.062(7) 0.059(7) 0.063(7) 0.005(6) 0.035(6) -0.006(6) C53 0.061(9) 0.066(9) 0.082(10) -0.001(8) 0.036(8) -0.012(7) C54 0.089(12) 0.046(8) 0.078(10) 0.007(7) 0.041(9) -0.009(8) C55 0.057(9) 0.068(9) 0.067(9) 0.030(7) 0.033(8) 0.003(7) C56 0.046(7) 0.056(8) 0.061(8) -0.010(7) 0.019(6) 0.000(6) N1 0.062(7) 0.045(6) 0.068(7) 0.013(5) 0.034(6) 0.001(5) C57 0.080(10) 0.053(8) 0.066(9) 0.014(7) 0.015(8) -0.002(7) C58 0.108(12) 0.051(9) 0.078(10) 0.011(8) 0.048(9) -0.024(8) C59 0.105(12) 0.065(10) 0.068(10) 0.000(8) 0.038(9) -0.021(9) C60 0.058(7) 0.055(7) 0.071(7) -0.002(6) 0.020(6) -0.007(5) C61 0.075(10) 0.036(7) 0.110(12) 0.007(7) 0.058(9) -0.006(7) N2 0.053(6) 0.051(6) 0.070(7) 0.014(6) 0.032(6) 0.005(5) C62 0.054(9) 0.065(8) 0.075(10) -0.007(7) 0.027(7) 0.008(7) C63 0.041(8) 0.094(11) 0.069(9) -0.009(8) 0.024(7) 0.003(7) C64 0.055(8) 0.057(8) 0.093(11) -0.006(8) 0.026(8) -0.007(7) C65 0.056(9) 0.071(9) 0.077(10) -0.025(7) 0.035(8) -0.012(7) C66 0.081(10) 0.045(7) 0.058(8) -0.024(6) 0.040(7) -0.016(7) N3 0.057(6) 0.037(5) 0.056(7) 0.003(5) 0.020(6) 0.006(5) C67 0.064(8) 0.052(8) 0.059(9) -0.008(7) 0.032(7) -0.002(7) C68 0.058(8) 0.043(7) 0.065(9) 0.005(7) 0.012(7) -0.011(6) C69 0.080(10) 0.037(7) 0.097(12) 0.004(8) 0.058(10) -0.003(7) C70 0.060(8) 0.045(7) 0.051(8) -0.013(7) 0.018(6) -0.015(6) C71 0.069(9) 0.053(8) 0.054(9) 0.011(7) 0.014(7) 0.010(7) N4 0.067(8) 0.051(6) 0.077(8) -0.001(6) 0.032(6) -0.003(6) C72 0.062(7) 0.060(7) 0.087(8) -0.002(6) 0.016(6) -0.012(6) C73 0.071(7) 0.068(7) 0.084(8) 0.004(6) 0.024(6) 0.004(6) C74 0.085(8) 0.099(8) 0.127(9) 0.026(7) 0.044(7) 0.010(7) C75 0.126(10) 0.134(10) 0.138(10) 0.030(8) 0.042(8) -0.003(8) C76 0.070(7) 0.088(8) 0.102(8) 0.021(7) 0.032(7) 0.023(7) N5 0.059(7) 0.055(7) 0.045(7) 0.021(6) -0.014(6) -0.045(6) C77 0.067(10) 0.062(10) 0.047(10) 0.000(8) 0.008(8) -0.013(8) C78 0.076(11) 0.072(11) 0.085(12) -0.003(9) 0.028(9) -0.007(8) C79 0.095(11) 0.073(10) 0.068(10) -0.005(8) -0.002(8) -0.015(8) C80 0.074(11) 0.069(10) 0.059(10) -0.007(8) 0.016(8) -0.005(8) C81 0.086(13) 0.093(13) 0.114(13) -0.019(9) 0.029(9) -0.008(9) N6 0.097(9) 0.070(8) 0.089(9) -0.024(7) 0.022(7) 0.001(7) C82 0.098(10) 0.088(10) 0.089(10) -0.022(8) 0.028(8) -0.003(8) C83 0.115(9) 0.108(9) 0.125(10) 0.006(8) 0.025(8) -0.001(8) C84 0.097(9) 0.089(8) 0.115(9) -0.003(7) 0.027(7) 0.019(7) C85 0.083(8) 0.095(9) 0.098(9) 0.000(7) 0.040(7) 0.017(7) C86 0.082(9) 0.065(9) 0.089(10) -0.005(8) 0.025(8) -0.001(7) N7 0.100(7) 0.105(7) 0.096(7) -0.013(6) 0.042(6) 0.004(6) C87 0.103(9) 0.101(9) 0.096(9) -0.012(7) 0.047(7) -0.001(7) C88 0.101(9) 0.093(8) 0.086(8) -0.004(7) 0.033(7) -0.004(7) C89 0.117(9) 0.119(9) 0.091(9) -0.013(8) 0.054(7) 0.006(8) C90 0.100(7) 0.107(7) 0.083(7) -0.019(6) 0.043(6) 0.003(6) C91 0.107(9) 0.108(9) 0.089(8) -0.008(7) 0.047(7) 0.012(7) N8 0.060(9) 0.057(9) 0.061(9) -0.002(7) 0.008(7) -0.008(7) C92 0.091(10) 0.067(9) 0.064(9) 0.011(7) 0.017(8) 0.000(8) C93 0.119(12) 0.146(13) 0.150(13) 0.010(9) 0.048(9) 0.003(9) C94 0.13(2) 0.13(2) 0.13(2) 0.017(10) 0.037(12) 0.006(10) C95 0.100(19) 0.107(19) 0.095(19) 0.017(10) 0.033(11) 0.002(10) C96 0.106(12) 0.128(12) 0.142(13) -0.012(9) 0.042(9) -0.009(9) N9 0.077(10) 0.065(9) 0.084(10) -0.020(8) 0.013(8) -0.010(8) C97 0.107(11) 0.124(12) 0.122(12) -0.018(9) 0.039(9) -0.003(9) C98 0.074(9) 0.068(9) 0.073(9) -0.026(7) 0.018(7) -0.009(7) C99 0.100(13) 0.095(13) 0.096(13) -0.010(9) 0.027(9) -0.006(9) C100 0.108(14) 0.108(14) 0.118(14) -0.004(9) 0.033(10) 0.004(9) C101 0.105(11) 0.089(10) 0.112(11) -0.026(8) 0.038(9) 0.010(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 U1 O1 2.111(9) 3 ? U1 O1 2.111(9) . ? U1 O2 2.141(7) 3 ? U1 O2 2.141(7) . ? U1 O3 2.144(7) 3 ? U1 O3 2.145(7) . ? U1 U2 7.8377(6) . ? U1 U3 7.9428(7) . ? U2 O4 2.117(7) . ? U2 O6 2.134(7) . ? U2 O5 2.231(7) . ? U2 N2 2.625(9) . ? U2 N3 2.627(9) . ? U2 N1 2.644(9) . ? U2 Cl1 2.771(3) . ? U2 C30 2.852(11) . ? U2 U3 5.5746(7) . ? U3 O7 2.062(8) . ? U3 O8 2.094(8) . ? U3 N4 2.588(11) . ? U3 N5 2.611(10) . ? U3 Cl3 2.677(5) . ? U3 Cl2 2.682(3) . ? U3 Cl1 2.993(3) . ? O1 C2 1.364(14) . ? O2 C9 1.366(14) . ? O3 C16 1.317(13) . ? O4 C23 1.346(14) . ? O4 O5 3.087(10) . ? O5 C30 1.332(13) . ? O5 O6 3.014(10) . ? O6 C37 1.316(13) . ? O7 C44 1.384(14) . ? O8 C51 1.360(14) . ? C1 C6 1.401(19) . ? C1 C2 1.400(16) . ? C1 C56 1.478(16) . ? C2 C3 1.432(16) . ? C3 C4 1.379(19) . ? C3 C7 1.537(17) . ? C4 C5 1.42(2) . ? C5 C6 1.428(19) . ? C7 C8 1.490(17) . ? C8 C9 1.373(18) . ? C8 C13 1.404(18) . ? C9 C10 1.411(17) . ? C10 C11 1.397(18) . ? C10 C14 1.451(18) . ? C11 C12 1.307(19) . ? C12 C13 1.42(2) . ? C14 C15 1.545(18) . ? C15 C20 1.391(18) . ? C15 C16 1.400(17) . ? C16 C17 1.407(16) . ? C17 C18 1.439(18) . ? C17 C21 1.496(15) . ? C18 C19 1.366(18) . ? C19 C20 1.426(19) . ? C21 C22 1.488(17) . ? C22 C23 1.406(16) . ? C22 C27 1.428(18) . ? C23 C24 1.408(16) . ? C24 C25 1.422(18) . ? C24 C28 1.475(15) . ? C25 C26 1.347(19) . ? C26 C27 1.355(19) . ? C28 C29 1.523(17) . ? C29 C30 1.420(17) . ? C29 C34 1.420(16) . ? C30 C31 1.432(17) . ? C31 C32 1.405(17) . ? C31 C35 1.527(17) . ? C32 C33 1.357(17) . ? C33 C34 1.371(16) . ? C35 C36 1.476(17) . ? C36 C41 1.416(17) . ? C36 C37 1.463(17) . ? C37 C38 1.424(17) . ? C38 C39 1.354(16) . ? C38 C42 1.521(17) . ? C39 C40 1.388(18) . ? C40 C41 1.373(19) . ? C42 C43 1.529(16) . ? C43 C48 1.340(15) . ? C43 C44 1.392(16) . ? C44 C45 1.357(16) . ? C45 C46 1.403(17) . ? C45 C49 1.538(17) . ? C46 C47 1.361(17) . ? C47 C48 1.412(16) . ? C49 C50 1.516(17) . ? C50 C55 1.369(16) . ? C50 C51 1.434(16) . ? C51 C52 1.451(18) . ? C52 C53 1.408(16) . ? C52 C56 1.481(16) . ? C53 C54 1.355(17) . ? C54 C55 1.386(17) . ? N1 C61 1.290(14) . ? N1 C57 1.374(15) . ? C57 C58 1.384(16) . ? C58 C59 1.391(18) . ? C59 C60 1.327(16) . ? C60 C61 1.418(16) . ? N2 C66 1.329(13) . ? N2 C62 1.366(14) . ? C62 C63 1.364(16) . ? C63 C64 1.411(17) . ? C64 C65 1.379(16) . ? C65 C66 1.368(16) . ? N3 C71 1.349(15) . ? N3 C67 1.357(14) . ? C67 C68 1.419(16) . ? C68 C69 1.325(17) . ? C69 C70 1.356(17) . ? C70 C71 1.389(16) . ? N4 C76 1.303(17) . ? N4 C72 1.363(16) . ? C72 C73 1.287(17) . ? C73 C74 1.357(19) . ? C74 C75 1.41(2) . ? C75 C76 1.35(2) . ? N5 C77 1.3900 . ? N5 C81 1.3900 . ? C77 C78 1.3900 . ? C78 C79 1.3900 . ? C79 C80 1.3900 . ? C80 C81 1.3900 . ? N6 C82 1.3900 . ? N6 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C85 C86 1.3900 . ? N7 C91 1.332(19) . ? N7 C87 1.358(19) . ? C87 C88 1.35(2) . ? C88 C89 1.40(2) . ? C89 C90 1.381(19) . ? C90 C91 1.391(18) . ? N8 C92 1.3900 . ? N8 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? N9 C101 1.32(3) . ? N9 C97 1.37(3) . ? C97 C98 1.36(3) . ? C98 C99 1.31(4) . ? C99 C100 1.41(4) . ? C100 C101 1.36(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O1 180.0(3) 3 . ? O1 U1 O2 86.6(3) 3 3 ? O1 U1 O2 93.4(3) . 3 ? O1 U1 O2 93.4(3) 3 . ? O1 U1 O2 86.6(3) . . ? O2 U1 O2 179.998(1) 3 . ? O1 U1 O3 92.3(3) 3 3 ? O1 U1 O3 87.7(3) . 3 ? O2 U1 O3 86.8(3) 3 3 ? O2 U1 O3 93.2(3) . 3 ? O1 U1 O3 87.7(3) 3 . ? O1 U1 O3 92.3(3) . . ? O2 U1 O3 93.2(3) 3 . ? O2 U1 O3 86.8(3) . . ? O3 U1 O3 179.997(1) 3 . ? O4 U2 O6 146.1(3) . . ? O4 U2 O5 90.4(3) . . ? O6 U2 O5 87.3(3) . . ? O4 U2 N2 72.7(3) . . ? O6 U2 N2 140.1(3) . . ? O5 U2 N2 82.2(3) . . ? O4 U2 N3 74.0(3) . . ? O6 U2 N3 75.6(3) . . ? O5 U2 N3 112.1(3) . . ? N2 U2 N3 143.7(3) . . ? O4 U2 N1 138.7(3) . . ? O6 U2 N1 74.1(3) . . ? O5 U2 N1 80.5(3) . . ? N2 U2 N1 66.3(3) . . ? N3 U2 N1 146.5(3) . . ? O4 U2 Cl1 94.5(2) . . ? O6 U2 Cl1 94.5(2) . . ? O5 U2 Cl1 167.97(19) . . ? N2 U2 Cl1 88.8(2) . . ? N3 U2 Cl1 79.8(2) . . ? N1 U2 Cl1 88.6(2) . . ? O7 U3 O8 88.8(3) . . ? O7 U3 N4 138.9(3) . . ? O8 U3 N4 100.0(3) . . ? O7 U3 N5 76.6(4) . . ? O8 U3 N5 97.1(3) . . ? N4 U3 N5 140.3(3) . . ? O7 U3 Cl3 147.2(2) . . ? O8 U3 Cl3 86.9(2) . . ? N4 U3 Cl3 73.8(3) . . ? N5 U3 Cl3 71.7(3) . . ? O7 U3 Cl2 86.6(2) . . ? O8 U3 Cl2 174.4(2) . . ? N4 U3 Cl2 81.5(2) . . ? N5 U3 Cl2 85.0(3) . . ? Cl3 U3 Cl2 98.74(13) . . ? O7 U3 Cl1 73.5(2) . . ? O8 U3 Cl1 74.4(2) . . ? N4 U3 Cl1 70.5(2) . . ? N5 U3 Cl1 149.0(3) . . ? Cl3 U3 Cl1 135.59(13) . . ? Cl2 U3 Cl1 101.14(9) . . ? U2 Cl1 U3 150.48(11) . . ? C2 O1 U1 156.9(7) . . ? C9 O2 U1 124.3(7) . . ? C16 O3 U1 166.1(7) . . ? C23 O4 U2 168.3(7) . . ? C30 O5 U2 103.5(6) . . ? C37 O6 U2 165.3(8) . . ? C44 O7 U3 159.8(7) . . ? C51 O8 U3 150.1(7) . . ? C6 C1 C2 116.5(12) . . ? C6 C1 C56 122.1(12) . . ? C2 C1 C56 121.3(11) . . ? O1 C2 C1 118.0(10) . . ? O1 C2 C3 118.4(11) . . ? C1 C2 C3 123.5(12) . . ? C4 C3 C2 116.3(12) . . ? C4 C3 C7 122.5(11) . . ? C2 C3 C7 121.2(11) . . ? C3 C4 C5 124.5(14) . . ? C4 C5 C6 115.2(14) . . ? C1 C6 C5 123.9(14) . . ? C8 C7 C3 115.5(11) . . ? C9 C8 C13 116.5(13) . . ? C9 C8 C7 122.6(12) . . ? C13 C8 C7 120.5(14) . . ? O2 C9 C8 117.3(11) . . ? O2 C9 C10 119.2(13) . . ? C8 C9 C10 123.5(13) . . ? C11 C10 C9 116.9(14) . . ? C11 C10 C14 121.0(12) . . ? C9 C10 C14 122.1(13) . . ? C12 C11 C10 121.3(14) . . ? C11 C12 C13 121.9(14) . . ? C8 C13 C12 119.7(15) . . ? C10 C14 C15 112.8(11) . . ? C20 C15 C16 121.3(13) . . ? C20 C15 C14 117.9(12) . . ? C16 C15 C14 120.7(11) . . ? O3 C16 C15 121.5(11) . . ? O3 C16 C17 119.4(10) . . ? C15 C16 C17 119.2(12) . . ? C16 C17 C18 118.4(12) . . ? C16 C17 C21 122.1(11) . . ? C18 C17 C21 119.5(11) . . ? C19 C18 C17 122.5(13) . . ? C18 C19 C20 117.9(14) . . ? C15 C20 C19 120.6(13) . . ? C22 C21 C17 113.6(11) . . ? C23 C22 C27 117.3(13) . . ? C23 C22 C21 121.8(11) . . ? C27 C22 C21 120.9(12) . . ? O4 C23 C22 120.4(11) . . ? O4 C23 C24 118.0(11) . . ? C22 C23 C24 121.6(12) . . ? C23 C24 C25 117.3(12) . . ? C23 C24 C28 122.4(12) . . ? C25 C24 C28 120.3(12) . . ? C26 C25 C24 121.0(13) . . ? C25 C26 C27 122.1(14) . . ? C26 C27 C22 120.6(14) . . ? C24 C28 C29 116.0(9) . . ? C30 C29 C34 120.1(12) . . ? C30 C29 C28 122.2(11) . . ? C34 C29 C28 117.6(13) . . ? O5 C30 C29 121.1(11) . . ? O5 C30 C31 120.3(12) . . ? C29 C30 C31 118.6(11) . . ? C32 C31 C30 118.6(12) . . ? C32 C31 C35 121.7(12) . . ? C30 C31 C35 118.9(11) . . ? C33 C32 C31 121.3(12) . . ? C32 C33 C34 122.2(12) . . ? C33 C34 C29 119.0(13) . . ? C36 C35 C31 119.0(9) . . ? C41 C36 C37 114.6(13) . . ? C41 C36 C35 123.6(12) . . ? C37 C36 C35 121.6(11) . . ? O6 C37 C38 121.9(11) . . ? O6 C37 C36 118.2(12) . . ? C38 C37 C36 119.9(11) . . ? C39 C38 C37 119.9(12) . . ? C39 C38 C42 123.0(12) . . ? C37 C38 C42 117.1(10) . . ? C38 C39 C40 122.6(13) . . ? C41 C40 C39 118.1(13) . . ? C40 C41 C36 124.6(13) . . ? C38 C42 C43 113.7(10) . . ? C48 C43 C44 117.2(11) . . ? C48 C43 C42 123.8(11) . . ? C44 C43 C42 119.0(10) . . ? C45 C44 O7 118.6(12) . . ? C45 C44 C43 122.8(12) . . ? O7 C44 C43 118.6(10) . . ? C44 C45 C46 118.5(12) . . ? C44 C45 C49 123.1(11) . . ? C46 C45 C49 118.3(11) . . ? C47 C46 C45 120.4(13) . . ? C46 C47 C48 118.2(12) . . ? C43 C48 C47 122.7(12) . . ? C50 C49 C45 112.5(11) . . ? C55 C50 C51 118.6(12) . . ? C55 C50 C49 119.4(11) . . ? C51 C50 C49 121.9(11) . . ? O8 C51 C50 119.1(12) . . ? O8 C51 C52 120.6(11) . . ? C50 C51 C52 120.3(12) . . ? C53 C52 C51 115.2(12) . . ? C53 C52 C56 125.1(12) . . ? C51 C52 C56 119.6(11) . . ? C54 C53 C52 124.1(13) . . ? C53 C54 C55 119.4(12) . . ? C50 C55 C54 122.1(12) . . ? C1 C56 C52 117.8(10) . . ? C61 N1 C57 117.6(10) . . ? C61 N1 U2 117.3(8) . . ? C57 N1 U2 124.0(8) . . ? N1 C57 C58 120.2(13) . . ? C57 C58 C59 120.4(13) . . ? C60 C59 C58 118.9(13) . . ? C59 C60 C61 118.1(13) . . ? N1 C61 C60 124.7(12) . . ? C66 N2 C62 118.0(10) . . ? C66 N2 U2 122.0(8) . . ? C62 N2 U2 119.9(8) . . ? C63 C62 N2 122.1(12) . . ? C62 C63 C64 119.0(12) . . ? C65 C64 C63 117.9(12) . . ? C66 C65 C64 119.7(12) . . ? N2 C66 C65 123.1(11) . . ? C71 N3 C67 118.6(10) . . ? C71 N3 U2 120.8(8) . . ? C67 N3 U2 120.2(8) . . ? N3 C67 C68 119.9(11) . . ? C69 C68 C67 119.0(12) . . ? C68 C69 C70 122.7(12) . . ? C69 C70 C71 117.2(12) . . ? N3 C71 C70 122.6(11) . . ? C76 N4 C72 114.0(12) . . ? C76 N4 U3 124.9(9) . . ? C72 N4 U3 120.5(9) . . ? C73 C72 N4 126.1(14) . . ? C72 C73 C74 120.4(15) . . ? C73 C74 C75 115.6(16) . . ? C76 C75 C74 119.0(18) . . ? N4 C76 C75 124.4(16) . . ? C77 N5 C81 120.0 . . ? C77 N5 U3 107.6(7) . . ? C81 N5 U3 132.4(7) . . ? N5 C77 C78 120.0 . . ? C79 C78 C77 120.0 . . ? C78 C79 C80 120.0 . . ? C79 C80 C81 120.0 . . ? C80 C81 N5 120.0 . . ? C82 N6 C86 120.0 . . ? C83 C82 N6 120.0 . . ? C82 C83 C84 120.0 . . ? C83 C84 C85 120.0 . . ? C86 C85 C84 120.0 . . ? C85 C86 N6 120.0 . . ? C91 N7 C87 115.9(14) . . ? C88 C87 N7 124.5(17) . . ? C87 C88 C89 118.0(16) . . ? C90 C89 C88 119.9(15) . . ? C89 C90 C91 116.6(15) . . ? N7 C91 C90 124.8(15) . . ? C92 N8 C96 120.0 . . ? N8 C92 C93 120.0 . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C96 C95 C94 120.0 . . ? C95 C96 N8 120.0 . . ? C101 N9 C97 116(2) . . ? C98 C97 N9 120(2) . . ? C99 C98 C97 122(2) . . ? C98 C99 C100 119(3) . . ? C101 C100 C99 115(3) . . ? N9 C101 C100 126(3) . . ? #===END data_8.4py _database_code_depnum_ccdc_archive 'CCDC 603338' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H56 N4 O8 U' _chemical_formula_weight 1175.10 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.3919(5) _cell_length_b 17.0589(5) _cell_length_c 17.0640(5) _cell_angle_alpha 90.00 _cell_angle_beta 120.446(2) _cell_angle_gamma 90.00 _cell_volume 5368.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39725 _cell_measurement_theta_min 3.47 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method ? _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 3.080 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 40 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 one \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 39725 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4943 _reflns_number_gt 3752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO and SCALEPACK (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, with restraints for some badly behaving atoms in the solvent pyridine molecules. One of these molecules (containing N3) was refined as an idealized hexagon and was affected with an occupancy factor of 0.5 so as to keep reasonable displacement parameters. The H atom bound to O2 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^)+(0.0978P)^2^+62.5699P] 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 4943 _refine_ls_number_parameters 339 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1725 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.118 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.203 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 0.0000 0.07612(3) 0.7500 0.0489(2) Uani 1 2 d S . . O1 O 0.0030(3) 0.1627(3) 0.8431(4) 0.0396(14) Uani 1 1 d . . . O2 O 0.1268(4) 0.1314(4) 0.8262(4) 0.0475(16) Uani 1 1 d . . . H2 H 0.1612 0.1015 0.8181 0.057 Uiso 1 1 d R . . O3 O -0.0704(5) 0.0008(4) 0.7947(5) 0.070(2) Uani 1 1 d . . . O4 O 0.0772(5) -0.0033(4) 0.8770(5) 0.070(2) Uani 1 1 d . . . N1 N 0.2409(6) 0.0571(6) 0.8410(7) 0.067(3) Uani 1 1 d . . . N2 N 0.0000 0.3722(7) 0.7500 0.053(3) Uani 1 2 d S . . C1 C -0.0599(5) 0.2367(6) 0.8999(6) 0.041(2) Uani 1 1 d . . . C2 C 0.0044(5) 0.2123(5) 0.9063(6) 0.041(2) Uani 1 1 d . . . C3 C 0.0729(5) 0.2378(5) 0.9792(6) 0.037(2) Uani 1 1 d . . . C4 C 0.0737(6) 0.2872(6) 1.0444(6) 0.045(2) Uani 1 1 d . . . H4 H 0.1178 0.3049 1.0922 0.054 Uiso 1 1 calc R . . C5 C 0.0100(5) 0.3101(6) 1.0387(6) 0.047(2) Uani 1 1 d . . . H5 H 0.0111 0.3430 1.0829 0.057 Uiso 1 1 calc R . . C6 C -0.0550(6) 0.2849(6) 0.9686(7) 0.052(3) Uani 1 1 d . . . H6 H -0.0974 0.3004 0.9668 0.063 Uiso 1 1 calc R . . C7 C 0.1415(5) 0.2110(5) 0.9833(6) 0.041(2) Uani 1 1 d . . . H7A H 0.1393 0.1547 0.9742 0.050 Uiso 1 1 calc R . . H7B H 0.1824 0.2220 1.0433 0.050 Uiso 1 1 calc R . . C8 C 0.1538(5) 0.2506(5) 0.9125(6) 0.041(2) Uani 1 1 d . . . C9 C 0.1433(5) 0.2115(5) 0.8344(6) 0.042(2) Uani 1 1 d . . . C10 C 0.1503(5) 0.2482(6) 0.7674(6) 0.046(2) Uani 1 1 d . . . C11 C 0.1702(5) 0.3267(6) 0.7791(6) 0.043(2) Uani 1 1 d . . . H11 H 0.1744 0.3528 0.7342 0.052 Uiso 1 1 calc R . . C12 C 0.1837(5) 0.3667(6) 0.8568(7) 0.048(2) Uani 1 1 d . . . H12 H 0.1995 0.4184 0.8655 0.058 Uiso 1 1 calc R . . C13 C 0.1737(5) 0.3294(5) 0.9215(6) 0.042(2) Uani 1 1 d . . . H13 H 0.1803 0.3574 0.9719 0.050 Uiso 1 1 calc R . . C14 C 0.1311(6) 0.2077(7) 0.6782(7) 0.055(3) Uani 1 1 d . . . H14A H 0.1693 0.2172 0.6646 0.066 Uiso 1 1 calc R . . H14B H 0.1280 0.1516 0.6849 0.066 Uiso 1 1 calc R . . C15 C -0.1205(11) -0.0756(10) 0.8639(14) 0.088(5) Uani 1 1 d . . . H15A H -0.1199 -0.0525 0.9155 0.132 Uiso 1 1 calc R . . H15B H -0.1162 -0.1315 0.8711 0.132 Uiso 1 1 calc R . . H15C H -0.1652 -0.0628 0.8097 0.132 Uiso 1 1 calc R . . C16 C -0.0612(10) -0.0459(9) 0.8568(11) 0.068(4) Uani 1 1 d . . . C17 C 0.0047(9) -0.0708(7) 0.9110(12) 0.083(4) Uani 1 1 d . . . H17 H 0.0050 -0.1162 0.9413 0.099 Uiso 1 1 calc R . . C18 C 0.0700(9) -0.0490(8) 0.9340(9) 0.084(4) Uani 1 1 d . . . C19 C 0.1414(12) -0.0782(12) 1.0082(15) 0.105(7) Uani 1 1 d . . . H19A H 0.1363 -0.0969 1.0577 0.158 Uiso 1 1 calc R . . H19B H 0.1762 -0.0363 1.0290 0.158 Uiso 1 1 calc R . . H19C H 0.1578 -0.1203 0.9856 0.158 Uiso 1 1 calc R . . C20 C 0.2660(9) 0.0088(9) 0.9108(10) 0.094(4) Uani 1 1 d U . . H20 H 0.2405 0.0037 0.9414 0.113 Uiso 1 1 calc R . . C21 C 0.3288(10) -0.0347(11) 0.9403(13) 0.115(6) Uani 1 1 d U . . H21 H 0.3436 -0.0712 0.9868 0.138 Uiso 1 1 calc R . . C22 C 0.3693(9) -0.0217(10) 0.8976(12) 0.105(5) Uani 1 1 d U . . H22 H 0.4129 -0.0478 0.9174 0.125 Uiso 1 1 calc R . . C23 C 0.3432(7) 0.0304(7) 0.8256(9) 0.073(3) Uani 1 1 d U . . H23 H 0.3682 0.0396 0.7951 0.088 Uiso 1 1 calc R . . C24 C 0.2798(7) 0.0676(7) 0.8013(10) 0.072(3) Uani 1 1 d U . . H24 H 0.2624 0.1030 0.7532 0.087 Uiso 1 1 calc R . . C25 C 0.0089(6) 0.4119(6) 0.8249(8) 0.054(3) Uani 1 1 d . . . H25 H 0.0147 0.3851 0.8757 0.065 Uiso 1 1 calc R . . C26 C 0.0088(6) 0.4921(7) 0.8227(9) 0.066(3) Uani 1 1 d . . . H26 H 0.0149 0.5203 0.8729 0.079 Uiso 1 1 calc R . . C27 C 0.0000 0.5303(10) 0.7500 0.065(4) Uani 1 2 d SU . . H27 H 0.0000 0.5848 0.7500 0.078 Uiso 1 2 calc SR . . N3 N 0.2961(7) 0.2024(7) 0.6714(11) 0.076(6) Uani 0.50 1 d PGU . . C28 C 0.3063(7) 0.2830(7) 0.6814(11) 0.080(7) Uani 0.50 1 d PGU . . H28 H 0.2754 0.3139 0.6917 0.096 Uiso 0.50 1 calc PR . . C29 C 0.3628(8) 0.3176(6) 0.6758(10) 0.055(5) Uani 0.50 1 d PGU . . H29 H 0.3696 0.3716 0.6825 0.066 Uiso 0.50 1 calc PR . . C30 C 0.4091(6) 0.2715(7) 0.6604(10) 0.044(4) Uani 0.50 1 d PGU . . H30 H 0.4469 0.2947 0.6567 0.052 Uiso 0.50 1 calc PR . . C31 C 0.3989(7) 0.1909(7) 0.6504(11) 0.072(7) Uani 0.50 1 d PGU . . H31 H 0.4298 0.1600 0.6401 0.086 Uiso 0.50 1 calc PR . . C32 C 0.3424(7) 0.1563(6) 0.6559(11) 0.051(5) Uani 0.50 1 d PGU . . H32 H 0.3355 0.1023 0.6493 0.061 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.0924(5) 0.0219(3) 0.0389(3) 0.000 0.0380(3) 0.000 O1 0.053(4) 0.034(3) 0.036(3) -0.005(3) 0.025(3) -0.005(3) O2 0.064(4) 0.037(3) 0.048(4) 0.008(3) 0.034(3) 0.021(3) O3 0.111(6) 0.041(4) 0.066(4) 0.006(3) 0.049(4) -0.012(4) O4 0.109(6) 0.042(4) 0.056(4) 0.019(3) 0.040(4) 0.015(4) N1 0.065(5) 0.053(4) 0.058(5) -0.012(4) 0.013(4) 0.020(4) N2 0.043(7) 0.051(7) 0.053(7) 0.000 0.016(6) 0.000 C1 0.040(6) 0.054(5) 0.035(5) -0.002(4) 0.023(4) -0.010(4) C2 0.053(6) 0.037(5) 0.038(5) 0.002(4) 0.028(5) -0.007(4) C3 0.050(6) 0.029(4) 0.039(5) 0.002(4) 0.028(5) 0.002(4) C4 0.050(6) 0.049(5) 0.032(5) -0.011(4) 0.016(4) -0.004(4) C5 0.037(6) 0.065(6) 0.036(5) -0.014(5) 0.016(5) 0.003(5) C6 0.053(7) 0.065(7) 0.046(6) -0.010(5) 0.030(5) -0.002(5) C7 0.053(6) 0.037(5) 0.034(4) 0.006(4) 0.022(4) 0.016(4) C8 0.037(5) 0.043(5) 0.043(5) 0.016(4) 0.021(4) 0.020(4) C9 0.037(5) 0.043(5) 0.044(5) 0.012(4) 0.019(4) 0.022(4) C10 0.044(6) 0.056(6) 0.043(5) 0.010(4) 0.026(5) 0.019(4) C11 0.026(5) 0.061(6) 0.044(5) 0.017(5) 0.018(4) 0.014(4) C12 0.028(5) 0.056(6) 0.053(6) 0.013(5) 0.015(4) 0.007(4) C13 0.029(5) 0.046(5) 0.044(5) 0.004(4) 0.014(4) 0.008(4) C14 0.058(7) 0.061(7) 0.054(6) 0.004(5) 0.035(6) 0.014(5) C15 0.105(9) 0.080(9) 0.098(9) 0.018(7) 0.066(7) -0.001(7) C16 0.101(9) 0.051(6) 0.063(7) 0.008(6) 0.050(6) 0.000(6) C17 0.104(8) 0.036(5) 0.119(9) 0.016(5) 0.065(7) 0.005(6) C18 0.112(9) 0.059(6) 0.061(6) 0.018(5) 0.029(6) 0.021(6) C19 0.119(10) 0.098(10) 0.091(9) 0.029(7) 0.047(8) 0.006(8) C20 0.099(8) 0.085(7) 0.084(7) -0.003(6) 0.036(6) 0.040(6) C21 0.109(9) 0.105(9) 0.105(9) 0.005(7) 0.035(7) 0.046(7) C22 0.087(8) 0.099(9) 0.103(9) -0.009(7) 0.031(7) 0.026(7) C23 0.058(6) 0.060(6) 0.078(7) -0.019(5) 0.018(5) 0.008(5) C24 0.064(7) 0.056(6) 0.072(7) -0.010(5) 0.017(5) 0.011(5) C25 0.052(6) 0.053(6) 0.060(6) -0.003(5) 0.031(5) 0.007(5) C26 0.037(6) 0.070(8) 0.090(9) -0.029(7) 0.032(6) -0.002(5) C27 0.055(8) 0.048(7) 0.090(9) 0.000 0.036(7) 0.000 N3 0.073(7) 0.079(8) 0.080(8) -0.004(5) 0.043(6) -0.001(5) C28 0.076(11) 0.086(11) 0.083(11) -0.012(8) 0.044(8) 0.004(8) C29 0.058(9) 0.050(8) 0.049(8) -0.006(7) 0.020(7) -0.027(7) C30 0.028(8) 0.043(7) 0.050(8) 0.012(7) 0.014(6) 0.000(6) C31 0.054(10) 0.065(10) 0.088(11) 0.016(8) 0.030(8) 0.001(8) C32 0.038(8) 0.047(8) 0.069(9) -0.017(7) 0.028(7) -0.002(6) _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 O1 2.146(6) . ? U O1 2.146(6) 2_556 ? U O4 2.374(7) 2_556 ? U O4 2.374(7) . ? U O3 2.381(8) . ? U O3 2.381(8) 2_556 ? U O2 2.522(7) . ? U O2 2.522(7) 2_556 ? O1 C2 1.360(11) . ? O2 C9 1.400(11) . ? O3 C16 1.259(16) . ? O4 C18 1.314(16) . ? N1 C20 1.319(18) . ? N1 C24 1.324(18) . ? N2 C25 1.373(12) 2_556 ? N2 C25 1.373(12) . ? C1 C2 1.387(14) . ? C1 C6 1.393(13) . ? C1 C14 1.510(14) 2_556 ? C2 C3 1.428(14) . ? C3 C4 1.389(12) . ? C3 C7 1.504(13) . ? C4 C5 1.375(14) . ? C5 C6 1.365(14) . ? C7 C8 1.518(12) . ? C8 C13 1.395(13) . ? C8 C9 1.403(13) . ? C9 C10 1.377(13) . ? C10 C11 1.389(14) . ? C10 C14 1.526(14) . ? C11 C12 1.385(14) . ? C12 C13 1.382(13) . ? C14 C1 1.510(14) 2_556 ? C15 C16 1.43(2) . ? C16 C17 1.30(2) . ? C17 C18 1.30(2) . ? C18 C19 1.49(3) . ? C20 C21 1.39(2) . ? C21 C22 1.40(3) . ? C22 C23 1.38(2) . ? C23 C24 1.358(17) . ? C25 C26 1.369(15) . ? C26 C27 1.328(15) . ? C27 C26 1.328(15) 2_556 ? N3 C28 1.3900 . ? N3 C32 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U O1 93.0(3) . 2_556 ? O1 U O4 144.5(3) . 2_556 ? O1 U O4 88.4(3) 2_556 2_556 ? O1 U O4 88.4(2) . . ? O1 U O4 144.5(3) 2_556 . ? O4 U O4 110.4(4) 2_556 . ? O1 U O3 85.5(2) . . ? O1 U O3 145.3(3) 2_556 . ? O4 U O3 74.0(3) 2_556 . ? O4 U O3 70.1(3) . . ? O1 U O3 145.3(3) . 2_556 ? O1 U O3 85.5(2) 2_556 2_556 ? O4 U O3 70.1(3) 2_556 2_556 ? O4 U O3 74.0(3) . 2_556 ? O3 U O3 114.7(4) . 2_556 ? O1 U O2 74.9(2) . . ? O1 U O2 75.2(2) 2_556 . ? O4 U O2 138.9(3) 2_556 . ? O4 U O2 70.9(3) . . ? O3 U O2 136.6(2) . . ? O3 U O2 71.2(3) 2_556 . ? O1 U O2 75.2(2) . 2_556 ? O1 U O2 74.9(2) 2_556 2_556 ? O4 U O2 70.9(3) 2_556 2_556 ? O4 U O2 138.9(3) . 2_556 ? O3 U O2 71.2(3) . 2_556 ? O3 U O2 136.6(2) 2_556 2_556 ? O2 U O2 136.1(3) . 2_556 ? C2 O1 U 175.0(5) . . ? C9 O2 U 124.5(5) . . ? C16 O3 U 139.2(11) . . ? C18 O4 U 136.5(9) . . ? C20 N1 C24 118.3(12) . . ? C25 N2 C25 120.8(13) 2_556 . ? C2 C1 C6 117.5(9) . . ? C2 C1 C14 119.2(8) . 2_556 ? C6 C1 C14 123.3(9) . 2_556 ? O1 C2 C1 120.1(8) . . ? O1 C2 C3 118.8(8) . . ? C1 C2 C3 121.2(8) . . ? C4 C3 C2 118.2(8) . . ? C4 C3 C7 122.1(9) . . ? C2 C3 C7 119.7(8) . . ? C5 C4 C3 120.5(9) . . ? C6 C5 C4 120.4(9) . . ? C5 C6 C1 122.2(10) . . ? C3 C7 C8 112.6(7) . . ? C13 C8 C9 117.1(8) . . ? C13 C8 C7 120.5(8) . . ? C9 C8 C7 122.3(8) . . ? C10 C9 O2 119.3(8) . . ? C10 C9 C8 122.7(9) . . ? O2 C9 C8 118.0(8) . . ? C9 C10 C11 118.3(9) . . ? C9 C10 C14 122.3(10) . . ? C11 C10 C14 119.2(9) . . ? C12 C11 C10 120.8(9) . . ? C13 C12 C11 119.8(10) . . ? C12 C13 C8 121.2(9) . . ? C1 C14 C10 111.9(8) 2_556 . ? O3 C16 C17 117.0(15) . . ? O3 C16 C15 122.0(17) . . ? C17 C16 C15 120.8(14) . . ? C18 C17 C16 137.0(14) . . ? C17 C18 O4 117.2(13) . . ? C17 C18 C19 130.0(15) . . ? O4 C18 C19 111.9(16) . . ? N1 C20 C21 122.5(17) . . ? C20 C21 C22 117.8(18) . . ? C23 C22 C21 119.0(15) . . ? C24 C23 C22 117.5(15) . . ? N1 C24 C23 124.7(14) . . ? C26 C25 N2 118.1(11) . . ? C27 C26 C25 120.9(12) . . ? C26 C27 C26 121.3(16) . 2_556 ? C28 N3 C32 120.0 . . ? C29 C28 N3 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C31 120.0 . . ? C32 C31 C30 120.0 . . ? C31 C32 N3 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 N1 0.96 1.72 2.648(12) 160.8 . #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 603339' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H104 N4 Na4 O20 U2' _chemical_formula_weight 2321.95 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' Na Na 0.0362 0.0249 '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 12.4838(4) _cell_length_b 12.7588(5) _cell_length_c 33.6497(14) _cell_angle_alpha 81.021(4) _cell_angle_beta 79.732(4) _cell_angle_gamma 70.613(2) _cell_volume 4947.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 102502 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method ? _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 3.358 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.499 _exptl_absorpt_correction_T_max 0.715 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2003)' _exptl_special_details 'crystal-to-detector distance 60 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 six \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 102502 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.68 _reflns_number_total 18745 _reflns_number_gt 13051 _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 pyridine molecule is disordered over two positions (corresponding to atoms N3 and N4, bound to Na1 and Na2, respectively) which were refined as idealized hexagons, with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some badly behaving ones, in the acac groups and pyridine molecules. The H atoms bound to O4 and O8 were found on a Fourier-difference map and all the other ones were introduced at calculated positions (except in the disordered parts). 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^)+(0.0797P)^2^+5.7355P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18745 _refine_ls_number_parameters 1268 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.624 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.159 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 -0.13582(2) 0.34818(2) 0.414631(8) 0.02710(10) Uani 1 1 d . . . U2 U 0.26918(2) 0.24067(2) 0.108767(8) 0.02550(10) Uani 1 1 d . . . Na1 Na -0.2631(3) 0.3173(3) 0.32600(9) 0.0456(9) Uani 1 1 d . . . Na2 Na 0.1479(3) 0.0477(3) 0.18396(9) 0.0390(8) Uani 1 1 d . . . Na3 Na -0.3604(3) 0.4291(3) 0.49086(9) 0.0399(8) Uani 1 1 d . . . Na4 Na 0.4298(2) 0.1192(2) 0.02117(8) 0.0311(7) Uani 1 1 d . . . O1 O -0.1306(4) 0.2251(4) 0.37195(15) 0.0322(13) Uani 1 1 d . . . O2 O -0.3088(4) 0.3223(4) 0.43544(14) 0.0313(13) Uani 1 1 d . . . O3 O -0.2363(4) 0.4589(4) 0.36238(14) 0.0307(13) Uani 1 1 d . . . O4 O -0.1113(5) 0.4049(5) 0.28508(15) 0.0385(14) Uani 1 1 d . . . H4 H -0.1588 0.4345 0.3082 0.046 Uiso 1 1 d R . . O5 O 0.1007(4) 0.2173(4) 0.14174(14) 0.0307(13) Uani 1 1 d . . . O6 O 0.2580(4) 0.1054(4) 0.07480(14) 0.0284(12) Uani 1 1 d . . . O7 O 0.3245(4) 0.0942(4) 0.15789(13) 0.0269(12) Uani 1 1 d . . . O8 O 0.1930(5) 0.1477(5) 0.23489(15) 0.0374(14) Uani 1 1 d . . . H8 H 0.2346 0.1442 0.2100 0.045 Uiso 1 1 d R . . O9 O 0.0086(4) 0.3853(4) 0.36602(14) 0.0299(12) Uani 1 1 d . . . O10 O -0.0051(5) 0.4017(5) 0.44669(15) 0.0395(14) Uani 1 1 d . . . O11 O 0.0025(5) 0.1825(5) 0.43561(15) 0.0416(15) Uani 1 1 d . . . O12 O -0.1716(4) 0.3058(5) 0.48949(15) 0.0383(14) Uani 1 1 d . . . O13 O -0.2446(4) 0.5183(5) 0.44378(15) 0.0343(13) Uani 1 1 d . . . O14 O -0.4727(5) 0.6124(5) 0.48558(17) 0.0413(15) Uani 1 1 d . . . O15 O 0.3612(4) 0.3869(4) 0.09479(13) 0.0297(12) Uani 1 1 d . . . O16 O 0.2545(4) 0.3251(4) 0.16779(14) 0.0312(13) Uani 1 1 d . . . O17 O 0.1238(4) 0.4074(4) 0.09074(15) 0.0337(13) Uani 1 1 d . . . O18 O 0.2935(4) 0.2911(4) 0.03473(14) 0.0298(12) Uani 1 1 d . . . O19 O 0.4663(4) 0.1481(4) 0.08475(14) 0.0270(12) Uani 1 1 d . . . O20 O 0.5933(4) -0.0343(4) 0.03180(15) 0.0298(12) Uani 1 1 d . . . C1 C -0.0027(8) 0.0675(7) 0.3400(2) 0.043(2) Uani 1 1 d . . . C2 C -0.0947(7) 0.1123(7) 0.3687(2) 0.036(2) Uani 1 1 d . . . C3 C -0.1536(7) 0.0450(7) 0.3935(2) 0.038(2) Uani 1 1 d . . . C4 C -0.1164(8) -0.0705(8) 0.3902(3) 0.049(2) Uani 1 1 d . . . H4A H -0.1550 -0.1161 0.4066 0.059 Uiso 1 1 calc R . . C5 C -0.0227(8) -0.1161(7) 0.3627(3) 0.048(2) Uani 1 1 d . . . H5 H 0.0021 -0.1926 0.3608 0.058 Uiso 1 1 calc R . . C6 C 0.0351(8) -0.0495(7) 0.3378(2) 0.051(3) Uani 1 1 d . . . H6 H 0.0988 -0.0815 0.3195 0.061 Uiso 1 1 calc R . . C7 C -0.2572(7) 0.0940(7) 0.4243(3) 0.042(2) Uani 1 1 d . . . H7A H -0.2328 0.1233 0.4448 0.051 Uiso 1 1 calc R . . H7B H -0.2879 0.0350 0.4377 0.051 Uiso 1 1 calc R . . C8 C -0.3513(7) 0.1870(7) 0.4048(2) 0.0337(19) Uani 1 1 d . . . C9 C -0.3702(7) 0.2983(7) 0.4113(2) 0.035(2) Uani 1 1 d . . . C10 C -0.4537(7) 0.3876(7) 0.3916(2) 0.035(2) Uani 1 1 d . . . C11 C -0.5183(7) 0.3619(8) 0.3662(3) 0.051(2) Uani 1 1 d . . . H11 H -0.5738 0.4189 0.3535 0.061 Uiso 1 1 calc R . . C12 C -0.4990(8) 0.2516(8) 0.3603(3) 0.058(3) Uani 1 1 d . . . H12 H -0.5429 0.2344 0.3442 0.069 Uiso 1 1 calc R . . C13 C -0.4159(9) 0.1683(9) 0.3781(3) 0.061(3) Uani 1 1 d U . . H13 H -0.4013 0.0955 0.3723 0.074 Uiso 1 1 calc R . . C14 C -0.4759(7) 0.5060(7) 0.3999(2) 0.034(2) Uani 1 1 d . . . H14A H -0.5583 0.5401 0.4054 0.041 Uiso 1 1 calc R . . H14B H -0.4449 0.5031 0.4247 0.041 Uiso 1 1 calc R . . C15 C -0.4301(7) 0.5830(7) 0.3683(2) 0.035(2) Uani 1 1 d . . . C16 C -0.3126(6) 0.5596(6) 0.3529(2) 0.0280(18) Uani 1 1 d . . . C17 C -0.2750(7) 0.6416(7) 0.3270(2) 0.0325(19) Uani 1 1 d . . . C18 C -0.3546(7) 0.7429(7) 0.3163(2) 0.040(2) Uani 1 1 d . . . H18 H -0.3294 0.7964 0.2987 0.048 Uiso 1 1 calc R . . C19 C -0.4703(8) 0.7678(8) 0.3308(3) 0.048(2) Uani 1 1 d . . . H19 H -0.5224 0.8366 0.3236 0.057 Uiso 1 1 calc R . . C20 C -0.5052(7) 0.6856(7) 0.3567(3) 0.044(2) Uani 1 1 d . . . H20 H -0.5826 0.7005 0.3667 0.052 Uiso 1 1 calc R . . C21 C -0.1496(7) 0.6218(7) 0.3093(2) 0.0340(19) Uani 1 1 d . . . H21A H -0.1288 0.6872 0.3116 0.041 Uiso 1 1 calc R . . H21B H -0.1027 0.5592 0.3253 0.041 Uiso 1 1 calc R . . C22 C -0.1228(7) 0.5986(7) 0.2659(2) 0.0309(18) Uani 1 1 d . . . C23 C -0.1028(7) 0.4902(7) 0.2557(2) 0.038(2) Uani 1 1 d . . . C24 C -0.0748(6) 0.4673(7) 0.2145(2) 0.035(2) Uani 1 1 d . . . C25 C -0.0677(8) 0.5524(10) 0.1846(2) 0.054(3) Uani 1 1 d . . . H25 H -0.0480 0.5374 0.1576 0.064 Uiso 1 1 calc R . . C26 C -0.0898(7) 0.6606(9) 0.1941(3) 0.052(3) Uani 1 1 d . . . H26 H -0.0876 0.7180 0.1735 0.062 Uiso 1 1 calc R . . C27 C -0.1153(7) 0.6829(8) 0.2349(2) 0.043(2) Uani 1 1 d . . . H27 H -0.1273 0.7546 0.2413 0.052 Uiso 1 1 calc R . . C28 C -0.0400(7) 0.3515(8) 0.2034(2) 0.048(3) Uani 1 1 d . . . H28A H -0.0651 0.3051 0.2264 0.058 Uiso 1 1 calc R . . H28B H 0.0431 0.3236 0.1986 0.058 Uiso 1 1 calc R . . C29 C -0.0851(7) 0.3377(7) 0.1668(2) 0.039(2) Uani 1 1 d . . . C30 C -0.0129(7) 0.2649(7) 0.1373(2) 0.0323(19) Uani 1 1 d . . . C31 C -0.0577(7) 0.2435(7) 0.1059(2) 0.033(2) Uani 1 1 d . . . C32 C -0.1714(7) 0.2957(7) 0.1026(2) 0.041(2) Uani 1 1 d . . . H32 H -0.2008 0.2815 0.0812 0.049 Uiso 1 1 calc R . . C33 C -0.2442(7) 0.3679(7) 0.1291(2) 0.038(2) Uani 1 1 d . . . H33 H -0.3207 0.4028 0.1256 0.046 Uiso 1 1 calc R . . C34 C -0.1993(7) 0.3873(7) 0.1618(2) 0.042(2) Uani 1 1 d . . . H34 H -0.2477 0.4346 0.1805 0.051 Uiso 1 1 calc R . . C35 C 0.0183(6) 0.1632(7) 0.0754(2) 0.037(2) Uani 1 1 d . . . H35A H -0.0300 0.1501 0.0583 0.044 Uiso 1 1 calc R . . H35B H 0.0699 0.1988 0.0580 0.044 Uiso 1 1 calc R . . C36 C 0.0879(7) 0.0529(7) 0.0940(2) 0.038(2) Uani 1 1 d . . . C37 C 0.2087(7) 0.0291(7) 0.0938(2) 0.0291(18) Uani 1 1 d . . . C38 C 0.2732(7) -0.0721(6) 0.1139(2) 0.0293(18) Uani 1 1 d . . . C39 C 0.2174(7) -0.1488(7) 0.1327(3) 0.041(2) Uani 1 1 d . . . H39 H 0.2599 -0.2158 0.1456 0.049 Uiso 1 1 calc R . . C40 C 0.1040(8) -0.1299(8) 0.1329(3) 0.052(3) Uani 1 1 d . . . H40 H 0.0702 -0.1836 0.1456 0.062 Uiso 1 1 calc R . . C41 C 0.0377(7) -0.0300(8) 0.1140(3) 0.045(2) Uani 1 1 d . . . H41 H -0.0403 -0.0174 0.1144 0.055 Uiso 1 1 calc R . . C42 C 0.4008(7) -0.0990(6) 0.1107(2) 0.0323(19) Uani 1 1 d . . . H42A H 0.4245 -0.0489 0.0888 0.039 Uiso 1 1 calc R . . H42B H 0.4361 -0.1743 0.1030 0.039 Uiso 1 1 calc R . . C43 C 0.4490(7) -0.0916(7) 0.1486(2) 0.0307(18) Uani 1 1 d . . . C44 C 0.4129(7) 0.0053(6) 0.1686(2) 0.0295(18) Uani 1 1 d . . . C45 C 0.4693(7) 0.0080(7) 0.2014(2) 0.0334(19) Uani 1 1 d . . . C46 C 0.5571(8) -0.0823(7) 0.2124(3) 0.050(2) Uani 1 1 d . . . H46 H 0.5932 -0.0801 0.2340 0.060 Uiso 1 1 calc R . . C47 C 0.5945(8) -0.1771(8) 0.1926(3) 0.056(3) Uani 1 1 d . . . H47 H 0.6560 -0.2372 0.2003 0.067 Uiso 1 1 calc R . . C48 C 0.5405(7) -0.1819(7) 0.1616(3) 0.042(2) Uani 1 1 d . . . H48 H 0.5648 -0.2467 0.1486 0.051 Uiso 1 1 calc R . . C49 C 0.4338(7) 0.1135(7) 0.2239(2) 0.0343(19) Uani 1 1 d . . . H49A H 0.5023 0.1295 0.2271 0.041 Uiso 1 1 calc R . . H49B H 0.3889 0.1763 0.2073 0.041 Uiso 1 1 calc R . . C50 C 0.3648(8) 0.1032(7) 0.2653(3) 0.043(2) Uani 1 1 d . . . C51 C 0.2454(8) 0.1202(7) 0.2688(2) 0.037(2) Uani 1 1 d . . . C52 C 0.1787(9) 0.1131(7) 0.3065(2) 0.046(2) Uani 1 1 d . . . C53 C 0.2342(9) 0.0847(8) 0.3403(3) 0.054(3) Uani 1 1 d U . . H53 H 0.1914 0.0780 0.3657 0.065 Uiso 1 1 calc R . . C54 C 0.3526(10) 0.0654(9) 0.3385(3) 0.064(3) Uani 1 1 d U . . H54 H 0.3881 0.0462 0.3618 0.077 Uiso 1 1 calc R . . C55 C 0.4146(9) 0.0764(7) 0.2999(3) 0.051(3) Uani 1 1 d . . . H55 H 0.4929 0.0649 0.2978 0.062 Uiso 1 1 calc R . . C56 C 0.0507(8) 0.1426(8) 0.3094(3) 0.056(3) Uani 1 1 d U . . H56A H 0.0319 0.1406 0.2828 0.067 Uiso 1 1 calc R . . H56B H 0.0162 0.2187 0.3163 0.067 Uiso 1 1 calc R . . C57 C 0.1795(7) 0.3913(7) 0.3232(2) 0.041(2) Uani 1 1 d . . . H57A H 0.1835 0.3264 0.3113 0.061 Uiso 1 1 calc R . . H57B H 0.2556 0.3906 0.3251 0.061 Uiso 1 1 calc R . . H57C H 0.1424 0.4573 0.3066 0.061 Uiso 1 1 calc R . . C58 C 0.1122(7) 0.3909(7) 0.3650(2) 0.035(2) Uani 1 1 d . . . C59 C 0.1575(7) 0.3974(8) 0.3984(2) 0.046(2) Uani 1 1 d . . . H59 H 0.2327 0.3986 0.3949 0.056 Uiso 1 1 calc R . . C60 C 0.0962(8) 0.4024(8) 0.4379(3) 0.043(2) Uani 1 1 d . . . C61 C 0.1577(8) 0.4095(9) 0.4726(3) 0.061(3) Uani 1 1 d U . . H61A H 0.1226 0.4811 0.4828 0.091 Uiso 1 1 calc R . . H61B H 0.2370 0.4001 0.4627 0.091 Uiso 1 1 calc R . . H61C H 0.1519 0.3516 0.4941 0.091 Uiso 1 1 calc R . . C62 C 0.1595(9) 0.0510(9) 0.4616(3) 0.071(3) Uani 1 1 d U . . H62A H 0.1524 -0.0091 0.4493 0.107 Uiso 1 1 calc R . . H62B H 0.1877 0.0226 0.4871 0.107 Uiso 1 1 calc R . . H62C H 0.2119 0.0838 0.4440 0.107 Uiso 1 1 calc R . . C63 C 0.0444(8) 0.1378(9) 0.4683(3) 0.058(3) Uani 1 1 d U . . C64 C -0.0070(9) 0.1638(9) 0.5071(3) 0.063(3) Uani 1 1 d U . . H64 H 0.0314 0.1249 0.5288 0.076 Uiso 1 1 calc R . . C65 C -0.1121(8) 0.2440(9) 0.5154(3) 0.055(3) Uani 1 1 d . . . C66 C -0.1659(9) 0.2568(9) 0.5597(3) 0.069(3) Uani 1 1 d U . . H66A H -0.1733 0.3299 0.5661 0.103 Uiso 1 1 calc R . . H66B H -0.1179 0.2013 0.5773 0.103 Uiso 1 1 calc R . . H66C H -0.2403 0.2471 0.5637 0.103 Uiso 1 1 calc R . . C67 C -0.1509(7) 0.6500(7) 0.4116(2) 0.043(2) Uani 1 1 d . . . H67A H -0.1098 0.6700 0.4292 0.065 Uiso 1 1 calc R . . H67B H -0.1756 0.7112 0.3913 0.065 Uiso 1 1 calc R . . H67C H -0.1016 0.5856 0.3987 0.065 Uiso 1 1 calc R . . C68 C -0.2532(7) 0.6237(7) 0.4360(2) 0.036(2) Uani 1 1 d . . . C69 C -0.3477(8) 0.7098(7) 0.4490(2) 0.044(2) Uani 1 1 d . . . H69 H -0.3431 0.7817 0.4419 0.053 Uiso 1 1 calc R . . C70 C -0.4504(8) 0.7002(8) 0.4720(3) 0.047(2) Uani 1 1 d . . . C71 C -0.5465(8) 0.8112(8) 0.4787(3) 0.065(3) Uani 1 1 d U . . H71A H -0.5912 0.8322 0.4566 0.097 Uiso 1 1 calc R . . H71B H -0.5133 0.8684 0.4799 0.097 Uiso 1 1 calc R . . H71C H -0.5949 0.8023 0.5037 0.097 Uiso 1 1 calc R . . C72 C 0.4069(7) 0.5540(7) 0.0875(2) 0.041(2) Uani 1 1 d . . . H72A H 0.4748 0.5443 0.0992 0.062 Uiso 1 1 calc R . . H72B H 0.3574 0.6296 0.0888 0.062 Uiso 1 1 calc R . . H72C H 0.4277 0.5383 0.0597 0.062 Uiso 1 1 calc R . . C73 C 0.3463(7) 0.4762(6) 0.1105(2) 0.0305(19) Uani 1 1 d . . . C74 C 0.2854(7) 0.4983(7) 0.1491(2) 0.037(2) Uani 1 1 d . . . H74 H 0.2688 0.5697 0.1566 0.044 Uiso 1 1 calc R . . C75 C 0.2487(7) 0.4215(7) 0.1764(2) 0.0329(19) Uani 1 1 d . . . C76 C 0.2047(7) 0.4465(7) 0.2199(2) 0.039(2) Uani 1 1 d . . . H76A H 0.1479 0.4105 0.2309 0.058 Uiso 1 1 calc R . . H76B H 0.1712 0.5258 0.2207 0.058 Uiso 1 1 calc R . . H76C H 0.2672 0.4193 0.2357 0.058 Uiso 1 1 calc R . . C77 C -0.0081(7) 0.5751(8) 0.0683(2) 0.048(2) Uani 1 1 d . . . H77A H -0.0711 0.5521 0.0832 0.072 Uiso 1 1 calc R . . H77B H -0.0297 0.6167 0.0431 0.072 Uiso 1 1 calc R . . H77C H 0.0114 0.6211 0.0840 0.072 Uiso 1 1 calc R . . C78 C 0.0939(7) 0.4733(7) 0.0599(2) 0.0306(18) Uani 1 1 d . . . C79 C 0.1508(7) 0.4607(7) 0.0205(2) 0.038(2) Uani 1 1 d . . . H79 H 0.1222 0.5152 -0.0001 0.046 Uiso 1 1 calc R . . C80 C 0.2483(7) 0.3710(7) 0.0099(2) 0.0303(19) Uani 1 1 d . . . C81 C 0.3021(7) 0.3689(7) -0.0346(2) 0.0327(19) Uani 1 1 d . . . H81A H 0.3784 0.3731 -0.0371 0.049 Uiso 1 1 calc R . . H81B H 0.2568 0.4316 -0.0506 0.049 Uiso 1 1 calc R . . H81C H 0.3048 0.3009 -0.0441 0.049 Uiso 1 1 calc R . . C82 C 0.5793(7) 0.1895(7) 0.1261(2) 0.036(2) Uani 1 1 d . . . H82A H 0.5643 0.2663 0.1152 0.054 Uiso 1 1 calc R . . H82B H 0.6560 0.1603 0.1329 0.054 Uiso 1 1 calc R . . H82C H 0.5258 0.1840 0.1500 0.054 Uiso 1 1 calc R . . C83 C 0.5664(7) 0.1227(6) 0.0947(2) 0.0276(18) Uani 1 1 d . . . C84 C 0.6629(7) 0.0415(7) 0.0790(2) 0.034(2) Uani 1 1 d . . . H84 H 0.7300 0.0315 0.0895 0.041 Uiso 1 1 calc R . . C85 C 0.6722(7) -0.0295(7) 0.0482(2) 0.037(2) Uani 1 1 d . . . C86 C 0.7897(6) -0.1066(7) 0.0356(3) 0.043(2) Uani 1 1 d . . . H86A H 0.8127 -0.1635 0.0574 0.065 Uiso 1 1 calc R . . H86B H 0.8430 -0.0649 0.0289 0.065 Uiso 1 1 calc R . . H86C H 0.7885 -0.1407 0.0122 0.065 Uiso 1 1 calc R . . N1 N -0.3886(8) 0.4120(8) 0.2745(3) 0.075(3) Uani 1 1 d U . . C87 C -0.4027(8) 0.5122(8) 0.2604(3) 0.049(2) Uani 1 1 d . . . H87 H -0.3702 0.5532 0.2724 0.059 Uiso 1 1 calc R . . C88 C -0.4620(8) 0.5652(9) 0.2287(3) 0.053(3) Uani 1 1 d . . . H88 H -0.4721 0.6404 0.2203 0.063 Uiso 1 1 calc R . . C89 C -0.5074(8) 0.5027(9) 0.2094(3) 0.053(3) Uani 1 1 d . . . H89 H -0.5479 0.5358 0.1876 0.063 Uiso 1 1 calc R . . C90 C -0.4920(10) 0.3961(10) 0.2226(3) 0.074(3) Uani 1 1 d . . . H90 H -0.5175 0.3514 0.2097 0.089 Uiso 1 1 calc R . . C91 C -0.4374(11) 0.3547(12) 0.2559(4) 0.097(4) Uani 1 1 d U . . H91 H -0.4328 0.2820 0.2668 0.116 Uiso 1 1 calc R . . N2 N 0.1854(7) -0.1247(6) 0.2312(2) 0.0440(19) Uani 1 1 d . . . C92 C 0.2770(8) -0.1585(8) 0.2510(3) 0.047(2) Uani 1 1 d . . . H92 H 0.3265 -0.1157 0.2453 0.056 Uiso 1 1 calc R . . C93 C 0.3042(7) -0.2496(8) 0.2787(3) 0.047(2) Uani 1 1 d . . . H93 H 0.3708 -0.2682 0.2906 0.056 Uiso 1 1 calc R . . C94 C 0.2333(8) -0.3136(7) 0.2889(3) 0.056(3) Uani 1 1 d . . . H94 H 0.2467 -0.3734 0.3090 0.067 Uiso 1 1 calc R . . C95 C 0.1375(8) -0.2846(8) 0.2672(3) 0.049(2) Uani 1 1 d . . . H95 H 0.0897 -0.3289 0.2711 0.059 Uiso 1 1 calc R . . C96 C 0.1181(8) -0.1907(8) 0.2409(2) 0.043(2) Uani 1 1 d . . . H96 H 0.0524 -0.1700 0.2283 0.051 Uiso 1 1 calc R . . N3 N -0.2299(7) 0.1623(7) 0.2818(2) 0.037(3) Uani 0.564(7) 1 d PG . 1 C97 C -0.2149(8) 0.1961(6) 0.2404(2) 0.043(4) Uani 0.564(7) 1 d PG . 1 C98 C -0.1941(9) 0.1197(8) 0.21248(19) 0.040(4) Uani 0.564(7) 1 d PG . 1 C99 C -0.1881(9) 0.0095(7) 0.2259(3) 0.039(4) Uani 0.564(7) 1 d PG . 1 C100 C -0.2031(10) -0.0243(6) 0.2673(3) 0.039(5) Uani 0.564(7) 1 d PG . 1 C101 C -0.2240(8) 0.0521(8) 0.2952(2) 0.044(5) Uani 0.564(7) 1 d PG . 1 N4 N -0.0566(8) 0.0666(9) 0.2128(3) 0.034(4) Uani 0.436(7) 1 d PG . 2 C102 C -0.1466(10) 0.0707(10) 0.1929(3) 0.041(5) Uani 0.436(7) 1 d PG . 2 C103 C -0.2445(9) 0.0509(12) 0.2150(4) 0.048(7) Uani 0.436(7) 1 d PG . 2 C104 C -0.2524(8) 0.0270(11) 0.2569(4) 0.038(6) Uani 0.436(7) 1 d PG . 2 C105 C -0.1624(10) 0.0229(11) 0.2768(3) 0.034(5) Uani 0.436(7) 1 d PG . 2 C106 C -0.0645(8) 0.0427(10) 0.2548(3) 0.035(5) Uani 0.436(7) 1 d PG . 2 N5 N 0.5746(6) 0.2224(5) -0.00370(18) 0.0338(16) Uani 1 1 d . . . C107 C 0.5708(7) 0.3086(7) 0.0154(2) 0.035(2) Uani 1 1 d . . . H107 H 0.5013 0.3472 0.0296 0.042 Uiso 1 1 calc R . . C108 C 0.6661(8) 0.3435(7) 0.0149(2) 0.044(2) Uani 1 1 d . . . H108 H 0.6606 0.4042 0.0282 0.052 Uiso 1 1 calc R . . C109 C 0.7694(8) 0.2838(8) -0.0061(3) 0.050(2) Uani 1 1 d . . . H109 H 0.8348 0.3045 -0.0073 0.060 Uiso 1 1 calc R . . C110 C 0.7741(8) 0.1938(8) -0.0250(3) 0.045(2) Uani 1 1 d . . . H110 H 0.8425 0.1533 -0.0393 0.054 Uiso 1 1 calc R . . C111 C 0.6776(8) 0.1649(7) -0.0224(2) 0.040(2) Uani 1 1 d . . . H111 H 0.6828 0.1018 -0.0342 0.048 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 0.02411(18) 0.03174(19) 0.02345(16) -0.00479(12) -0.00102(12) -0.00637(14) U2 0.02412(17) 0.02888(18) 0.02298(16) -0.00617(12) -0.00093(12) -0.00723(14) Na1 0.050(2) 0.042(2) 0.0356(18) -0.0085(15) -0.0100(16) 0.0026(17) Na2 0.0343(19) 0.041(2) 0.0351(17) -0.0005(15) -0.0008(14) -0.0068(16) Na3 0.0323(18) 0.044(2) 0.0331(17) -0.0056(15) 0.0068(14) -0.0034(16) Na4 0.0300(17) 0.0324(18) 0.0291(16) -0.0082(13) -0.0052(13) -0.0047(14) O1 0.033(3) 0.020(3) 0.037(3) -0.003(2) -0.003(2) -0.001(2) O2 0.026(3) 0.044(3) 0.026(3) -0.005(2) 0.000(2) -0.014(3) O3 0.024(3) 0.033(3) 0.030(3) 0.002(2) 0.000(2) -0.005(3) O4 0.051(4) 0.038(3) 0.030(3) -0.008(3) 0.005(3) -0.022(3) O5 0.024(3) 0.039(3) 0.028(3) -0.005(2) 0.002(2) -0.009(3) O6 0.026(3) 0.030(3) 0.027(3) -0.008(2) -0.004(2) -0.005(3) O7 0.025(3) 0.029(3) 0.024(3) -0.005(2) 0.000(2) -0.004(2) O8 0.043(4) 0.047(4) 0.021(3) -0.007(2) 0.006(2) -0.017(3) O9 0.025(3) 0.035(3) 0.029(3) -0.009(2) -0.001(2) -0.007(3) O10 0.027(3) 0.062(4) 0.035(3) -0.013(3) -0.006(3) -0.016(3) O11 0.038(3) 0.040(4) 0.033(3) 0.005(3) -0.006(3) 0.001(3) O12 0.028(3) 0.049(4) 0.032(3) -0.004(3) 0.002(3) -0.007(3) O13 0.025(3) 0.039(4) 0.040(3) -0.013(3) 0.000(2) -0.009(3) O14 0.037(4) 0.037(4) 0.046(3) -0.012(3) 0.009(3) -0.011(3) O15 0.032(3) 0.037(3) 0.025(3) -0.012(2) 0.003(2) -0.016(3) O16 0.033(3) 0.031(3) 0.028(3) -0.008(2) 0.000(2) -0.008(3) O17 0.031(3) 0.031(3) 0.033(3) 0.002(2) -0.006(2) -0.003(3) O18 0.030(3) 0.029(3) 0.026(3) -0.004(2) -0.004(2) -0.003(3) O19 0.020(3) 0.032(3) 0.028(3) -0.004(2) 0.000(2) -0.007(2) O20 0.027(3) 0.031(3) 0.033(3) -0.007(2) -0.004(2) -0.009(3) C1 0.047(6) 0.038(5) 0.031(5) -0.004(4) 0.003(4) -0.002(4) C2 0.045(5) 0.036(5) 0.031(4) -0.013(4) -0.004(4) -0.013(4) C3 0.044(5) 0.027(5) 0.042(5) -0.007(4) 0.000(4) -0.012(4) C4 0.059(7) 0.048(6) 0.043(5) -0.008(4) -0.015(5) -0.016(5) C5 0.065(7) 0.028(5) 0.046(5) -0.001(4) -0.017(5) -0.005(5) C6 0.072(7) 0.033(5) 0.028(5) -0.006(4) -0.003(4) 0.010(5) C7 0.044(6) 0.031(5) 0.054(5) -0.002(4) -0.001(4) -0.019(4) C8 0.027(5) 0.032(5) 0.038(5) -0.004(4) -0.005(4) -0.003(4) C9 0.029(5) 0.039(5) 0.040(5) -0.007(4) 0.000(4) -0.016(4) C10 0.025(5) 0.041(5) 0.041(5) -0.012(4) -0.007(4) -0.007(4) C11 0.028(5) 0.057(7) 0.066(6) -0.014(5) -0.012(5) -0.006(5) C12 0.046(6) 0.047(6) 0.090(8) -0.021(6) -0.032(6) -0.009(5) C13 0.063(5) 0.055(5) 0.073(5) -0.020(4) -0.001(4) -0.026(4) C14 0.022(4) 0.037(5) 0.036(5) -0.007(4) -0.001(4) -0.002(4) C15 0.038(5) 0.034(5) 0.035(4) -0.009(4) -0.008(4) -0.011(4) C16 0.021(4) 0.021(4) 0.038(4) -0.008(3) -0.004(3) 0.001(3) C17 0.029(5) 0.029(5) 0.040(5) -0.008(4) -0.004(4) -0.007(4) C18 0.041(5) 0.039(5) 0.045(5) 0.009(4) -0.014(4) -0.021(5) C19 0.032(5) 0.038(6) 0.069(6) -0.003(5) -0.014(5) -0.003(4) C20 0.030(5) 0.037(5) 0.059(6) -0.001(4) -0.004(4) -0.007(4) C21 0.032(5) 0.033(5) 0.035(4) 0.004(4) -0.013(4) -0.006(4) C22 0.033(5) 0.035(5) 0.031(4) 0.001(4) -0.008(4) -0.019(4) C23 0.028(5) 0.050(6) 0.036(5) -0.003(4) 0.002(4) -0.017(4) C24 0.020(4) 0.054(6) 0.029(4) -0.003(4) -0.002(3) -0.010(4) C25 0.044(6) 0.094(9) 0.020(4) -0.005(5) 0.006(4) -0.024(6) C26 0.034(5) 0.075(8) 0.045(6) 0.013(5) -0.007(4) -0.024(5) C27 0.033(5) 0.056(6) 0.045(5) 0.009(4) -0.016(4) -0.020(5) C28 0.032(5) 0.073(7) 0.023(4) -0.014(4) 0.000(4) 0.006(5) C29 0.027(5) 0.058(6) 0.032(4) -0.007(4) -0.002(4) -0.013(4) C30 0.026(5) 0.039(5) 0.029(4) -0.004(4) -0.001(3) -0.007(4) C31 0.029(5) 0.036(5) 0.033(4) -0.004(4) -0.006(4) -0.008(4) C32 0.038(5) 0.050(6) 0.037(5) -0.006(4) -0.010(4) -0.015(5) C33 0.021(4) 0.050(6) 0.041(5) -0.005(4) -0.008(4) -0.007(4) C34 0.025(5) 0.054(6) 0.039(5) -0.004(4) -0.010(4) 0.000(4) C35 0.021(4) 0.046(6) 0.040(5) -0.016(4) -0.002(4) -0.004(4) C36 0.025(5) 0.039(5) 0.048(5) -0.019(4) 0.005(4) -0.004(4) C37 0.029(5) 0.036(5) 0.029(4) -0.013(4) -0.001(3) -0.016(4) C38 0.039(5) 0.024(4) 0.028(4) -0.013(3) -0.003(4) -0.011(4) C39 0.039(5) 0.033(5) 0.052(5) -0.013(4) -0.002(4) -0.011(4) C40 0.048(6) 0.047(6) 0.070(7) -0.015(5) 0.006(5) -0.032(5) C41 0.025(5) 0.055(6) 0.063(6) -0.017(5) -0.004(4) -0.017(5) C42 0.038(5) 0.024(4) 0.037(4) -0.006(3) -0.004(4) -0.011(4) C43 0.029(5) 0.034(5) 0.033(4) -0.005(4) 0.002(4) -0.016(4) C44 0.034(5) 0.029(5) 0.024(4) 0.006(3) -0.001(3) -0.013(4) C45 0.034(5) 0.036(5) 0.038(5) 0.005(4) -0.009(4) -0.022(4) C46 0.045(6) 0.031(5) 0.080(7) -0.006(5) -0.030(5) -0.010(5) C47 0.044(6) 0.048(6) 0.076(7) 0.002(5) -0.031(5) -0.005(5) C48 0.030(5) 0.032(5) 0.066(6) -0.010(4) -0.011(4) -0.006(4) C49 0.036(5) 0.034(5) 0.037(5) -0.002(4) -0.012(4) -0.013(4) C50 0.066(7) 0.027(5) 0.042(5) -0.004(4) -0.010(5) -0.019(5) C51 0.056(6) 0.028(5) 0.031(5) -0.005(4) -0.004(4) -0.019(4) C52 0.086(8) 0.027(5) 0.025(4) -0.004(4) 0.000(5) -0.022(5) C53 0.073(5) 0.043(4) 0.041(4) -0.009(3) 0.002(4) -0.013(4) C54 0.089(5) 0.059(5) 0.053(4) -0.010(4) -0.017(4) -0.028(4) C55 0.088(8) 0.040(6) 0.043(5) 0.004(4) -0.028(5) -0.037(6) C56 0.053(4) 0.045(4) 0.044(4) 0.004(3) 0.014(3) 0.003(3) C57 0.030(5) 0.048(6) 0.043(5) -0.006(4) 0.005(4) -0.014(4) C58 0.035(5) 0.036(5) 0.032(4) -0.005(4) 0.004(4) -0.011(4) C59 0.031(5) 0.080(7) 0.038(5) -0.025(5) 0.003(4) -0.026(5) C60 0.036(5) 0.057(6) 0.042(5) -0.007(4) -0.015(4) -0.017(5) C61 0.054(4) 0.080(5) 0.058(4) -0.021(4) -0.011(4) -0.024(4) C62 0.066(5) 0.069(5) 0.056(4) 0.007(4) -0.011(4) 0.006(4) C63 0.050(4) 0.063(5) 0.047(4) 0.000(4) -0.005(4) -0.002(4) C64 0.056(5) 0.070(5) 0.050(4) -0.004(4) -0.004(4) -0.005(4) C65 0.039(6) 0.070(7) 0.036(5) 0.001(5) -0.009(4) 0.008(5) C66 0.066(5) 0.075(5) 0.052(4) -0.003(4) -0.013(4) -0.003(4) C67 0.048(6) 0.042(6) 0.041(5) -0.015(4) 0.004(4) -0.018(5) C68 0.040(5) 0.038(5) 0.039(5) -0.014(4) 0.002(4) -0.024(4) C69 0.049(6) 0.033(5) 0.049(5) -0.009(4) 0.004(4) -0.013(5) C70 0.051(6) 0.047(6) 0.043(5) -0.020(5) 0.010(4) -0.017(5) C71 0.059(5) 0.054(5) 0.071(5) 0.005(4) 0.002(4) -0.016(4) C72 0.044(6) 0.040(5) 0.042(5) 0.000(4) -0.008(4) -0.017(5) C73 0.029(5) 0.024(4) 0.039(5) 0.004(4) -0.019(4) -0.004(4) C74 0.043(5) 0.029(5) 0.031(4) -0.008(4) -0.001(4) -0.002(4) C75 0.030(5) 0.038(5) 0.035(5) -0.014(4) -0.011(4) -0.008(4) C76 0.036(5) 0.047(6) 0.032(4) -0.012(4) -0.003(4) -0.008(4) C77 0.043(6) 0.057(6) 0.034(5) -0.002(4) -0.003(4) -0.003(5) C78 0.028(5) 0.027(5) 0.037(5) -0.004(4) -0.008(4) -0.008(4) C79 0.036(5) 0.034(5) 0.037(5) -0.006(4) -0.005(4) 0.000(4) C80 0.033(5) 0.038(5) 0.021(4) 0.002(4) -0.011(3) -0.012(4) C81 0.032(5) 0.031(5) 0.031(4) -0.001(4) -0.003(4) -0.007(4) C82 0.035(5) 0.042(5) 0.035(5) -0.010(4) -0.002(4) -0.016(4) C83 0.028(5) 0.027(4) 0.022(4) 0.002(3) 0.004(3) -0.006(4) C84 0.027(5) 0.042(5) 0.037(5) -0.004(4) -0.002(4) -0.015(4) C85 0.034(5) 0.037(5) 0.041(5) -0.005(4) 0.005(4) -0.016(4) C86 0.023(5) 0.045(6) 0.064(6) -0.017(5) -0.005(4) -0.008(4) N1 0.091(5) 0.070(4) 0.081(4) 0.003(4) -0.031(4) -0.041(4) C87 0.058(6) 0.052(6) 0.048(6) 0.002(5) -0.013(5) -0.031(5) C88 0.048(6) 0.054(7) 0.045(6) 0.003(5) -0.006(5) -0.004(5) C89 0.045(6) 0.077(8) 0.039(5) -0.005(5) -0.011(4) -0.021(6) C90 0.086(9) 0.079(9) 0.077(8) -0.011(7) -0.051(7) -0.029(7) C91 0.109(6) 0.095(6) 0.098(6) 0.000(4) -0.037(4) -0.040(4) N2 0.050(5) 0.047(5) 0.043(4) -0.001(4) -0.011(4) -0.026(4) C92 0.046(6) 0.052(6) 0.046(5) -0.002(5) 0.003(5) -0.028(5) C93 0.029(5) 0.042(6) 0.065(6) -0.003(5) -0.017(4) 0.000(4) C94 0.050(6) 0.027(5) 0.078(7) -0.006(5) 0.011(5) -0.004(5) C95 0.045(6) 0.050(6) 0.060(6) -0.008(5) -0.014(5) -0.021(5) C96 0.040(5) 0.052(6) 0.040(5) 0.001(4) -0.013(4) -0.018(5) N3 0.033(7) 0.069(10) 0.018(6) -0.007(6) -0.003(5) -0.028(7) C97 0.043(10) 0.057(11) 0.044(9) -0.015(8) -0.001(7) -0.033(9) C98 0.029(9) 0.046(11) 0.043(9) -0.005(8) -0.007(7) -0.006(8) C99 0.055(12) 0.025(10) 0.047(11) -0.013(8) -0.022(9) -0.014(8) C100 0.042(11) 0.034(11) 0.048(11) -0.017(9) -0.001(9) -0.020(9) C101 0.012(8) 0.033(10) 0.077(12) -0.005(8) 0.013(8) -0.005(7) N4 0.019(8) 0.041(10) 0.035(9) -0.004(7) -0.001(7) -0.003(7) C102 0.024(12) 0.043(14) 0.048(13) -0.010(10) 0.003(10) -0.002(10) C103 0.08(2) 0.023(13) 0.040(13) 0.002(10) -0.023(13) -0.005(12) C104 0.052(15) 0.021(12) 0.039(13) -0.008(10) 0.012(11) -0.015(11) C105 0.014(10) 0.036(13) 0.051(13) 0.024(10) -0.014(9) -0.012(9) C106 0.025(10) 0.038(12) 0.046(12) -0.007(9) -0.002(9) -0.017(9) N5 0.042(4) 0.035(4) 0.029(4) -0.011(3) -0.002(3) -0.015(3) C107 0.042(5) 0.040(5) 0.020(4) 0.003(4) -0.002(4) -0.015(4) C108 0.057(6) 0.041(6) 0.036(5) -0.008(4) -0.009(4) -0.016(5) C109 0.039(6) 0.057(7) 0.053(6) 0.008(5) -0.007(5) -0.021(5) C110 0.035(5) 0.049(6) 0.048(5) -0.008(5) 0.002(4) -0.013(5) C111 0.050(6) 0.041(5) 0.030(4) -0.008(4) 0.001(4) -0.016(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 O2 2.264(5) . ? U1 O1 2.267(5) . ? U1 O9 2.329(5) . ? U1 O11 2.344(5) . ? U1 O3 2.344(5) . ? U1 O13 2.398(5) . ? U1 O10 2.427(5) . ? U1 O12 2.484(5) . ? U1 Na3 3.442(3) . ? U1 Na1 3.747(3) . ? U2 O6 2.267(5) . ? U2 O5 2.285(5) . ? U2 O7 2.300(5) . ? U2 O16 2.355(5) . ? U2 O17 2.369(5) . ? U2 O19 2.400(5) . ? U2 O15 2.446(5) . ? U2 O18 2.464(5) . ? U2 Na4 3.517(3) . ? U2 Na2 3.732(3) . ? Na1 O1 2.358(6) . ? Na1 N1 2.446(9) . ? Na1 O3 2.471(6) . ? Na1 N3 2.540(7) . ? Na1 O4 2.594(6) . ? Na1 C10 2.944(8) . ? Na1 C9 2.953(8) . ? Na1 C2 3.095(9) . ? Na2 O5 2.354(6) . ? Na2 O7 2.450(6) . ? Na2 N2 2.464(8) . ? Na2 N4 2.509(9) . ? Na2 O8 2.528(6) . ? Na2 C38 2.926(7) . ? Na2 C37 3.020(8) . ? Na2 C39 3.064(8) . ? Na3 O14 2.291(6) . ? Na3 O14 2.294(7) 2_466 ? Na3 O2 2.352(6) . ? Na3 O12 2.356(6) . ? Na3 O13 2.367(6) . ? Na3 Na3 3.347(6) 2_466 ? Na4 O20 2.330(6) 2_655 ? Na4 O18 2.339(6) . ? Na4 O20 2.349(6) . ? Na4 O19 2.372(5) . ? Na4 N5 2.528(7) . ? Na4 O6 2.581(6) . ? Na4 Na4 3.358(6) 2_655 ? O1 C2 1.374(9) . ? O2 C9 1.339(9) . ? O3 C16 1.352(8) . ? O4 C23 1.369(9) . ? O5 C30 1.370(9) . ? O6 C37 1.342(9) . ? O7 C44 1.348(9) . ? O8 C51 1.357(9) . ? O9 C58 1.313(9) . ? O10 C60 1.250(9) . ? O11 C63 1.273(10) . ? O12 C65 1.251(9) . ? O13 C68 1.301(9) . ? O14 C70 1.243(10) . ? O14 Na3 2.294(7) 2_466 ? O15 C73 1.274(8) . ? O16 C75 1.283(9) . ? O17 C78 1.257(9) . ? O18 C80 1.255(8) . ? O19 C83 1.275(8) . ? O20 C85 1.235(9) . ? O20 Na4 2.330(6) 2_655 ? C1 C2 1.387(11) . ? C1 C6 1.417(11) . ? C1 C56 1.515(12) . ? C2 C3 1.397(11) . ? C3 C4 1.407(11) . ? C3 C7 1.524(11) . ? C4 C5 1.376(12) . ? C5 C6 1.384(13) . ? C7 C8 1.525(11) . ? C8 C13 1.401(12) . ? C8 C9 1.407(11) . ? C9 C10 1.431(11) . ? C10 C11 1.412(11) . ? C10 C14 1.505(11) . ? C11 C12 1.387(12) . ? C12 C13 1.363(13) . ? C14 C15 1.501(11) . ? C15 C20 1.378(11) . ? C15 C16 1.413(10) . ? C16 C17 1.404(11) . ? C17 C18 1.384(11) . ? C17 C21 1.524(10) . ? C18 C19 1.385(11) . ? C19 C20 1.391(12) . ? C21 C22 1.493(10) . ? C22 C27 1.390(11) . ? C22 C23 1.407(11) . ? C23 C24 1.419(10) . ? C24 C25 1.376(12) . ? C24 C28 1.484(12) . ? C25 C26 1.392(13) . ? C26 C27 1.406(11) . ? C28 C29 1.497(11) . ? C29 C34 1.384(10) . ? C29 C30 1.440(10) . ? C30 C31 1.382(11) . ? C31 C32 1.370(11) . ? C31 C35 1.530(10) . ? C32 C33 1.372(10) . ? C33 C34 1.408(11) . ? C35 C36 1.496(11) . ? C36 C41 1.426(12) . ? C36 C37 1.434(11) . ? C37 C38 1.415(11) . ? C38 C39 1.394(11) . ? C38 C42 1.502(10) . ? C39 C40 1.355(12) . ? C40 C41 1.395(12) . ? C42 C43 1.531(10) . ? C43 C44 1.401(10) . ? C43 C48 1.404(11) . ? C44 C45 1.423(10) . ? C45 C46 1.355(11) . ? C45 C49 1.544(11) . ? C46 C47 1.375(12) . ? C47 C48 1.358(12) . ? C49 C50 1.511(11) . ? C50 C55 1.361(11) . ? C50 C51 1.419(12) . ? C51 C52 1.396(11) . ? C52 C53 1.376(12) . ? C52 C56 1.503(13) . ? C53 C54 1.406(14) . ? C54 C55 1.400(13) . ? C57 C58 1.503(10) . ? C58 C59 1.371(11) . ? C59 C60 1.408(11) . ? C60 C61 1.536(11) . ? C62 C63 1.500(13) . ? C63 C64 1.385(12) . ? C64 C65 1.383(12) . ? C65 C66 1.532(12) . ? C67 C68 1.498(11) . ? C68 C69 1.377(11) . ? C69 C70 1.406(12) . ? C70 C71 1.540(12) . ? C72 C73 1.486(11) . ? C73 C74 1.399(10) . ? C74 C75 1.373(11) . ? C75 C76 1.512(10) . ? C77 C78 1.509(11) . ? C78 C79 1.393(10) . ? C79 C80 1.402(10) . ? C80 C81 1.530(10) . ? C82 C83 1.516(10) . ? C83 C84 1.386(10) . ? C84 C85 1.444(11) . ? C85 C86 1.500(11) . ? N1 C87 1.257(11) . ? N1 C91 1.368(14) . ? C87 C88 1.365(12) . ? C88 C89 1.405(13) . ? C89 C90 1.323(14) . ? C90 C91 1.357(14) . ? N2 C92 1.339(11) . ? N2 C96 1.344(11) . ? C92 C93 1.359(12) . ? C93 C94 1.360(12) . ? C94 C95 1.425(12) . ? C95 C96 1.354(12) . ? N3 C97 1.3900 . ? N3 C101 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.3900 . ? C99 C100 1.3900 . ? C100 C101 1.3900 . ? N4 C102 1.3900 . ? N4 C106 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C105 C106 1.3900 . ? N5 C107 1.342(10) . ? N5 C111 1.348(10) . ? C107 C108 1.399(11) . ? C108 C109 1.390(12) . ? C109 C110 1.377(12) . ? C110 C111 1.358(11) . ? 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 79.28(18) . . ? O2 U1 O9 154.07(17) . . ? O1 U1 O9 83.40(18) . . ? O2 U1 O11 106.80(19) . . ? O1 U1 O11 75.38(19) . . ? O9 U1 O11 87.08(18) . . ? O2 U1 O3 80.20(17) . . ? O1 U1 O3 75.56(18) . . ? O9 U1 O3 76.86(17) . . ? O11 U1 O3 148.13(18) . . ? O2 U1 O13 77.91(18) . . ? O1 U1 O13 146.24(18) . . ? O9 U1 O13 107.84(18) . . ? O11 U1 O13 135.34(18) . . ? O3 U1 O13 76.30(17) . . ? O2 U1 O10 134.54(17) . . ? O1 U1 O10 139.39(18) . . ? O9 U1 O10 69.91(17) . . ? O11 U1 O10 73.3(2) . . ? O3 U1 O10 124.24(19) . . ? O13 U1 O10 73.15(18) . . ? O2 U1 O12 67.74(17) . . ? O1 U1 O12 121.33(18) . . ? O9 U1 O12 138.19(17) . . ? O11 U1 O12 70.11(18) . . ? O3 U1 O12 138.12(17) . . ? O13 U1 O12 71.32(18) . . ? O10 U1 O12 70.14(18) . . ? O6 U2 O5 79.83(18) . . ? O6 U2 O7 82.97(17) . . ? O5 U2 O7 75.77(17) . . ? O6 U2 O16 153.77(18) . . ? O5 U2 O16 80.94(17) . . ? O7 U2 O16 75.11(17) . . ? O6 U2 O17 107.49(18) . . ? O5 U2 O17 74.27(18) . . ? O7 U2 O17 145.72(17) . . ? O16 U2 O17 84.07(17) . . ? O6 U2 O19 77.15(17) . . ? O5 U2 O19 145.38(18) . . ? O7 U2 O19 76.05(16) . . ? O16 U2 O19 110.52(17) . . ? O17 U2 O19 137.60(17) . . ? O6 U2 O15 136.45(16) . . ? O5 U2 O15 138.14(17) . . ? O7 U2 O15 120.55(17) . . ? O16 U2 O15 68.78(16) . . ? O17 U2 O15 74.46(18) . . ? O19 U2 O15 74.63(16) . . ? O6 U2 O18 68.50(17) . . ? O5 U2 O18 120.43(17) . . ? O7 U2 O18 142.17(16) . . ? O16 U2 O18 137.39(17) . . ? O17 U2 O18 69.54(17) . . ? O19 U2 O18 73.82(16) . . ? O15 U2 O18 72.15(16) . . ? O1 Na1 N1 175.9(3) . . ? O1 Na1 O3 71.57(19) . . ? N1 Na1 O3 109.1(3) . . ? O1 Na1 N3 100.2(3) . . ? N1 Na1 N3 78.1(3) . . ? O3 Na1 N3 163.6(3) . . ? O1 Na1 O4 88.1(2) . . ? N1 Na1 O4 88.3(3) . . ? O3 Na1 O4 68.20(18) . . ? N3 Na1 O4 97.9(2) . . ? O5 Na2 O7 71.73(19) . . ? O5 Na2 N2 176.2(2) . . ? O7 Na2 N2 111.2(2) . . ? O5 Na2 N4 94.1(3) . . ? O7 Na2 N4 161.4(3) . . ? N2 Na2 N4 82.5(3) . . ? O5 Na2 O8 88.8(2) . . ? O7 Na2 O8 70.07(18) . . ? N2 Na2 O8 90.0(2) . . ? N4 Na2 O8 98.4(3) . . ? O14 Na3 O14 86.2(2) . 2_466 ? O14 Na3 O2 121.6(2) . . ? O14 Na3 O2 95.3(2) 2_466 . ? O14 Na3 O12 145.6(3) . . ? O14 Na3 O12 127.4(2) 2_466 . ? O2 Na3 O12 68.6(2) . . ? O14 Na3 O13 76.7(2) . . ? O14 Na3 O13 153.1(2) 2_466 . ? O2 Na3 O13 76.84(19) . . ? O12 Na3 O13 74.1(2) . . ? O20 Na4 O18 116.9(2) 2_655 . ? O20 Na4 O20 88.3(2) 2_655 . ? O18 Na4 O20 154.8(2) . . ? O20 Na4 O19 162.2(2) 2_655 . ? O18 Na4 O19 76.66(18) . . ? O20 Na4 O19 78.60(19) . . ? O20 Na4 N5 109.7(2) 2_655 . ? O18 Na4 N5 88.0(2) . . ? O20 Na4 N5 83.5(2) . . ? O19 Na4 N5 80.9(2) . . ? O20 Na4 O6 102.3(2) 2_655 . ? O18 Na4 O6 65.44(18) . . ? O20 Na4 O6 110.8(2) . . ? O19 Na4 O6 71.87(17) . . ? N5 Na4 O6 145.3(2) . . ? C2 O1 U1 140.9(5) . . ? C2 O1 Na1 109.2(5) . . ? U1 O1 Na1 108.2(2) . . ? C9 O2 U1 124.5(4) . . ? C9 O2 Na3 132.8(5) . . ? U1 O2 Na3 96.4(2) . . ? C16 O3 U1 143.1(4) . . ? C16 O3 Na1 109.5(4) . . ? U1 O3 Na1 102.2(2) . . ? C23 O4 Na1 140.4(5) . . ? C30 O5 U2 135.7(5) . . ? C30 O5 Na2 116.0(5) . . ? U2 O5 Na2 107.1(2) . . ? C37 O6 U2 120.5(4) . . ? C37 O6 Na4 139.7(4) . . ? U2 O6 Na4 92.78(19) . . ? C44 O7 U2 143.9(4) . . ? C44 O7 Na2 107.4(4) . . ? U2 O7 Na2 103.5(2) . . ? C51 O8 Na2 137.7(5) . . ? C58 O9 U1 137.7(5) . . ? C60 O10 U1 135.6(5) . . ? C63 O11 U1 136.6(6) . . ? C65 O12 Na3 135.4(5) . . ? C65 O12 U1 134.0(5) . . ? Na3 O12 U1 90.6(2) . . ? C68 O13 Na3 130.0(5) . . ? C68 O13 U1 137.1(5) . . ? Na3 O13 U1 92.5(2) . . ? C70 O14 Na3 132.2(6) . . ? C70 O14 Na3 133.8(6) . 2_466 ? Na3 O14 Na3 93.8(2) . 2_466 ? C73 O15 U2 134.2(5) . . ? C75 O16 U2 137.0(5) . . ? C78 O17 U2 139.9(5) . . ? C80 O18 Na4 128.4(5) . . ? C80 O18 U2 137.3(5) . . ? Na4 O18 U2 94.09(19) . . ? C83 O19 Na4 123.9(4) . . ? C83 O19 U2 141.0(4) . . ? Na4 O19 U2 94.94(18) . . ? C85 O20 Na4 138.3(5) . 2_655 ? C85 O20 Na4 123.2(5) . . ? Na4 O20 Na4 91.7(2) 2_655 . ? C2 C1 C6 118.7(8) . . ? C2 C1 C56 120.7(8) . . ? C6 C1 C56 120.4(7) . . ? O1 C2 C1 119.5(8) . . ? O1 C2 C3 119.5(7) . . ? C1 C2 C3 121.0(8) . . ? C2 C3 C4 119.4(8) . . ? C2 C3 C7 121.4(7) . . ? C4 C3 C7 119.2(8) . . ? C5 C4 C3 119.9(9) . . ? C4 C5 C6 120.9(9) . . ? C5 C6 C1 120.1(8) . . ? C3 C7 C8 112.5(7) . . ? C13 C8 C9 117.4(8) . . ? C13 C8 C7 123.2(8) . . ? C9 C8 C7 119.2(7) . . ? O2 C9 C8 120.5(7) . . ? O2 C9 C10 119.2(7) . . ? C8 C9 C10 120.3(7) . . ? C11 C10 C9 119.0(8) . . ? C11 C10 C14 121.2(8) . . ? C9 C10 C14 119.8(7) . . ? C12 C11 C10 119.9(9) . . ? C13 C12 C11 120.1(9) . . ? C12 C13 C8 123.1(9) . . ? C15 C14 C10 119.0(6) . . ? C20 C15 C16 118.8(8) . . ? C20 C15 C14 117.9(7) . . ? C16 C15 C14 123.0(7) . . ? O3 C16 C17 119.7(7) . . ? O3 C16 C15 120.9(7) . . ? C17 C16 C15 119.4(7) . . ? C18 C17 C16 119.1(7) . . ? C18 C17 C21 118.7(7) . . ? C16 C17 C21 122.1(7) . . ? C17 C18 C19 122.6(8) . . ? C18 C19 C20 117.2(8) . . ? C15 C20 C19 122.9(8) . . ? C22 C21 C17 114.1(6) . . ? C27 C22 C23 118.9(7) . . ? C27 C22 C21 120.7(8) . . ? C23 C22 C21 120.3(7) . . ? O4 C23 C22 121.1(7) . . ? O4 C23 C24 118.5(8) . . ? C22 C23 C24 120.4(8) . . ? C25 C24 C23 119.3(8) . . ? C25 C24 C28 119.0(8) . . ? C23 C24 C28 121.3(8) . . ? C24 C25 C26 120.9(8) . . ? C25 C26 C27 119.8(9) . . ? C22 C27 C26 120.6(9) . . ? C24 C28 C29 115.7(7) . . ? C34 C29 C30 117.7(7) . . ? C34 C29 C28 121.4(7) . . ? C30 C29 C28 120.8(7) . . ? O5 C30 C31 121.4(7) . . ? O5 C30 C29 117.9(7) . . ? C31 C30 C29 120.6(7) . . ? C32 C31 C30 118.7(7) . . ? C32 C31 C35 120.6(7) . . ? C30 C31 C35 120.6(7) . . ? C31 C32 C33 123.4(8) . . ? C32 C33 C34 117.8(8) . . ? C29 C34 C33 121.6(8) . . ? C36 C35 C31 114.6(7) . . ? C41 C36 C37 117.5(8) . . ? C41 C36 C35 122.2(7) . . ? C37 C36 C35 120.2(8) . . ? O6 C37 C38 121.2(7) . . ? O6 C37 C36 118.5(7) . . ? C38 C37 C36 120.3(7) . . ? C39 C38 C37 118.5(8) . . ? C39 C38 C42 121.8(7) . . ? C37 C38 C42 119.4(7) . . ? C40 C39 C38 122.7(9) . . ? C39 C40 C41 120.0(9) . . ? C40 C41 C36 120.9(8) . . ? C38 C42 C43 117.2(6) . . ? C44 C43 C48 118.5(7) . . ? C44 C43 C42 122.7(7) . . ? C48 C43 C42 118.4(7) . . ? O7 C44 C43 121.3(7) . . ? O7 C44 C45 119.8(7) . . ? C43 C44 C45 118.9(7) . . ? C46 C45 C44 119.4(8) . . ? C46 C45 C49 119.8(7) . . ? C44 C45 C49 120.8(7) . . ? C45 C46 C47 122.1(9) . . ? C48 C47 C46 119.3(9) . . ? C47 C48 C43 121.7(8) . . ? C50 C49 C45 113.9(7) . . ? C55 C50 C51 118.2(8) . . ? C55 C50 C49 121.6(9) . . ? C51 C50 C49 120.2(7) . . ? O8 C51 C52 118.5(8) . . ? O8 C51 C50 119.7(7) . . ? C52 C51 C50 121.8(8) . . ? C53 C52 C51 117.2(10) . . ? C53 C52 C56 122.3(8) . . ? C51 C52 C56 120.4(8) . . ? C52 C53 C54 123.2(9) . . ? C55 C54 C53 117.0(9) . . ? C50 C55 C54 122.5(10) . . ? C52 C56 C1 115.2(7) . . ? O9 C58 C59 124.3(7) . . ? O9 C58 C57 114.4(7) . . ? C59 C58 C57 121.3(8) . . ? C58 C59 C60 123.5(8) . . ? O10 C60 C59 124.5(8) . . ? O10 C60 C61 117.5(8) . . ? C59 C60 C61 118.0(8) . . ? O11 C63 C64 125.6(9) . . ? O11 C63 C62 113.4(8) . . ? C64 C63 C62 121.0(9) . . ? C65 C64 C63 124.0(9) . . ? O12 C65 C64 125.4(8) . . ? O12 C65 C66 115.4(8) . . ? C64 C65 C66 119.1(8) . . ? O13 C68 C69 124.6(8) . . ? O13 C68 C67 116.1(7) . . ? C69 C68 C67 119.3(8) . . ? C68 C69 C70 126.8(8) . . ? O14 C70 C69 126.9(8) . . ? O14 C70 C71 117.5(8) . . ? C69 C70 C71 115.6(9) . . ? O15 C73 C74 123.5(7) . . ? O15 C73 C72 116.5(7) . . ? C74 C73 C72 119.7(7) . . ? C75 C74 C73 124.2(8) . . ? O16 C75 C74 123.5(7) . . ? O16 C75 C76 116.7(7) . . ? C74 C75 C76 119.6(7) . . ? O17 C78 C79 124.8(7) . . ? O17 C78 C77 115.0(7) . . ? C79 C78 C77 120.1(7) . . ? C78 C79 C80 124.3(8) . . ? O18 C80 C79 123.9(7) . . ? O18 C80 C81 117.7(7) . . ? C79 C80 C81 118.3(7) . . ? O19 C83 C84 125.7(7) . . ? O19 C83 C82 116.1(6) . . ? C84 C83 C82 118.1(7) . . ? C83 C84 C85 128.0(8) . . ? O20 C85 C84 126.7(8) . . ? O20 C85 C86 116.9(7) . . ? C84 C85 C86 116.4(8) . . ? C87 N1 C91 115.7(10) . . ? C87 N1 Na1 122.6(7) . . ? C91 N1 Na1 121.2(8) . . ? N1 C87 C88 124.8(10) . . ? C87 C88 C89 118.0(10) . . ? C90 C89 C88 119.2(9) . . ? C89 C90 C91 117.3(11) . . ? C90 C91 N1 124.8(13) . . ? C92 N2 C96 113.7(8) . . ? C92 N2 Na2 120.7(6) . . ? C96 N2 Na2 125.6(6) . . ? N2 C92 C93 125.9(9) . . ? C92 C93 C94 119.5(9) . . ? C93 C94 C95 116.9(9) . . ? C96 C95 C94 118.0(9) . . ? N2 C96 C95 125.8(8) . . ? C97 N3 C101 120.0 . . ? C97 N3 Na1 113.5(4) . . ? C101 N3 Na1 126.4(4) . . ? C98 C97 N3 120.0 . . ? C97 C98 C99 120.0 . . ? C98 C99 C100 120.0 . . ? C101 C100 C99 120.0 . . ? C100 C101 N3 120.0 . . ? C102 N4 C106 120.0 . . ? C102 N4 Na2 128.8(6) . . ? C106 N4 Na2 109.2(5) . . ? N4 C102 C103 120.0 . . ? C102 C103 C104 120.0 . . ? C105 C104 C103 120.0 . . ? C104 C105 C106 120.0 . . ? C105 C106 N4 120.0 . . ? C107 N5 C111 117.0(7) . . ? C107 N5 Na4 119.4(5) . . ? C111 N5 Na4 117.6(5) . . ? N5 C107 C108 123.3(8) . . ? C109 C108 C107 117.4(8) . . ? C110 C109 C108 119.5(9) . . ? C111 C110 C109 119.1(8) . . ? N5 C111 C110 123.7(8) . . ? 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 O3 0.94 1.92 2.841(7) 165.5 . O8 H8 O7 0.90 1.98 2.858(6) 164.3 . #===END data_10.4py _database_code_depnum_ccdc_archive 'CCDC 603340' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H74 F3 N6 O11 S U' _chemical_formula_weight 1706.61 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.448(3) _cell_length_b 10.0747(14) _cell_length_c 29.331(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.737(8) _cell_angle_gamma 90.00 _cell_volume 7744(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 93228 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method ? _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 2.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 50 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 'one \f and nine \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% none _diffrn_reflns_number 93228 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7319 _reflns_number_gt 6253 _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 direct methods and subsequent Fourier-difference synthesis. The triflate counter-ion is highly disordered and only the S, C and some O atoms of two positions appeared at first. These atoms were used to locate two positions of a triflate model, which were then refined as rigid groups with restraints on displacement parameters. The triflate moiety was affected with an overall 0.5 occupancy parameter (refined occupancies for each position: 0.260 and 0.240) so that the displacement parameters retain acceptable values. This 0.5 occupancy factor is in agreement with the +5 valence of U. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to O2 and N2 were found on a Fourier-difference map and all the other ones were introduced at calculated positions. All were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. The highest residual electron density peaks are located near the disordered triflate moiety. 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^)+(0.0823P)^2^+13.5494P] 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 7319 _refine_ls_number_parameters 565 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1312 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.287 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.151 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 0.0000 0.07168(3) 0.7500 0.02319(12) Uani 1 2 d S . . O1 O -0.07153(14) -0.0324(4) 0.73591(13) 0.0276(8) Uani 1 1 d . . . O2 O 0.00926(13) -0.1619(4) 0.69596(12) 0.0275(8) Uani 1 1 d . . . H2 H 0.0439 -0.1827 0.6912 0.033 Uiso 1 1 d R . . O3 O -0.00314(14) 0.1148(4) 0.67820(12) 0.0274(8) Uani 1 1 d . . . O4 O -0.05381(13) 0.2370(4) 0.74688(12) 0.0271(8) Uani 1 1 d . . . N1 N 0.09297(17) -0.2998(5) 0.67886(16) 0.0338(11) Uani 1 1 d . . . N2 N -0.1710(2) 0.1669(6) 0.55639(17) 0.0472(14) Uani 1 1 d . . . H2N H -0.1628 0.2259 0.5330 0.057 Uiso 1 1 d R . . N3 N -0.1460(2) 0.3478(6) 0.49414(18) 0.0454(13) Uani 1 1 d . . . C1 C -0.1582(2) -0.0114(6) 0.74730(18) 0.0282(12) Uani 1 1 d . . . C2 C -0.1184(2) -0.0861(5) 0.73329(18) 0.0260(12) Uani 1 1 d . . . C3 C -0.1267(2) -0.2176(6) 0.71729(18) 0.0299(12) Uani 1 1 d . . . C4 C -0.1761(2) -0.2694(6) 0.71369(19) 0.0355(13) Uani 1 1 d . . . H4 H -0.1823 -0.3549 0.7025 0.043 Uiso 1 1 calc R . . C5 C -0.2154(2) -0.1959(6) 0.7265(2) 0.0398(15) Uani 1 1 d . . . H5 H -0.2480 -0.2322 0.7238 0.048 Uiso 1 1 calc R . . C6 C -0.2073(2) -0.0686(6) 0.7433(2) 0.0375(14) Uani 1 1 d . . . H6 H -0.2344 -0.0203 0.7520 0.045 Uiso 1 1 calc R . . C7 C -0.0830(2) -0.2975(6) 0.70351(18) 0.0308(12) Uani 1 1 d . . . H7A H -0.0926 -0.3904 0.7015 0.037 Uiso 1 1 calc R . . H7B H -0.0538 -0.2890 0.7271 0.037 Uiso 1 1 calc R . . C8 C -0.0678(2) -0.2529(5) 0.65749(18) 0.0293(12) Uani 1 1 d . . . C9 C -0.0232(2) -0.1831(6) 0.65531(18) 0.0295(12) Uani 1 1 d . . . C10 C -0.0104(2) -0.1343(7) 0.61374(19) 0.0363(14) Uani 1 1 d . . . C11 C -0.0440(3) -0.1655(6) 0.5734(2) 0.0444(16) Uani 1 1 d . . . H11 H -0.0363 -0.1360 0.5451 0.053 Uiso 1 1 calc R . . C12 C -0.0869(3) -0.2367(6) 0.5749(2) 0.0452(16) Uani 1 1 d . . . H12 H -0.1078 -0.2580 0.5478 0.054 Uiso 1 1 calc R . . C13 C -0.1002(2) -0.2785(6) 0.6170(2) 0.0382(14) Uani 1 1 d . . . H13 H -0.1307 -0.3235 0.6180 0.046 Uiso 1 1 calc R . . C14 C 0.0342(2) -0.0413(6) 0.6111(2) 0.0382(15) Uani 1 1 d . . . H14A H 0.0570 -0.0445 0.6399 0.046 Uiso 1 1 calc R . . H14B H 0.0532 -0.0703 0.5868 0.046 Uiso 1 1 calc R . . C15 C 0.0161(2) 0.0997(6) 0.6018(2) 0.0361(14) Uani 1 1 d . . . C16 C -0.0020(2) 0.1736(6) 0.63685(18) 0.0282(12) Uani 1 1 d . . . C17 C -0.0190(2) 0.3045(6) 0.62923(19) 0.0309(13) Uani 1 1 d . . . C18 C -0.0195(2) 0.3580(7) 0.5851(2) 0.0390(15) Uani 1 1 d . . . H18 H -0.0313 0.4440 0.5791 0.047 Uiso 1 1 calc R . . C19 C -0.0027(2) 0.2845(7) 0.5502(2) 0.0452(16) Uani 1 1 d . . . H19 H -0.0035 0.3214 0.5210 0.054 Uiso 1 1 calc R . . C20 C 0.0151(2) 0.1585(7) 0.5583(2) 0.0410(15) Uani 1 1 d . . . H20 H 0.0266 0.1108 0.5346 0.049 Uiso 1 1 calc R . . C21 C -0.0377(2) 0.3831(6) 0.6672(2) 0.0308(12) Uani 1 1 d . . . H21A H -0.0384 0.4763 0.6589 0.037 Uiso 1 1 calc R . . H21B H -0.0136 0.3727 0.6950 0.037 Uiso 1 1 calc R . . C22 C -0.0899(2) 0.3434(5) 0.67739(19) 0.0289(12) Uani 1 1 d . . . C23 C -0.0951(2) 0.2674(5) 0.71681(18) 0.0276(12) Uani 1 1 d . . . C24 C -0.14387(19) 0.2235(6) 0.72520(18) 0.0271(12) Uani 1 1 d . . . C25 C -0.1864(2) 0.2639(6) 0.69542(19) 0.0322(13) Uani 1 1 d . . . H25 H -0.2186 0.2367 0.7010 0.039 Uiso 1 1 calc R . . C26 C -0.1821(2) 0.3442(6) 0.6574(2) 0.0343(13) Uani 1 1 d . . . H26 H -0.2110 0.3728 0.6384 0.041 Uiso 1 1 calc R . . C27 C -0.1344(2) 0.3803(6) 0.6484(2) 0.0332(13) Uani 1 1 d . . . H27 H -0.1313 0.4308 0.6224 0.040 Uiso 1 1 calc R . . C28 C -0.1490(2) 0.1295(6) 0.76436(18) 0.0308(12) Uani 1 1 d . . . H28A H -0.1772 0.1576 0.7801 0.037 Uiso 1 1 calc R . . H28B H -0.1181 0.1324 0.7863 0.037 Uiso 1 1 calc R . . C29 C 0.1399(2) -0.2803(8) 0.6692(2) 0.0519(19) Uani 1 1 d . . . H29 H 0.1500 -0.1947 0.6628 0.062 Uiso 1 1 calc R . . C30 C 0.1746(3) -0.3851(10) 0.6683(3) 0.064(2) Uani 1 1 d . . . H30 H 0.2075 -0.3683 0.6619 0.077 Uiso 1 1 calc R . . C31 C 0.1606(3) -0.5079(10) 0.6765(3) 0.070(2) Uani 1 1 d . . . H31 H 0.1834 -0.5780 0.6758 0.084 Uiso 1 1 calc R . . C32 C 0.1119(4) -0.5304(8) 0.6861(2) 0.061(2) Uani 1 1 d . . . H32 H 0.1009 -0.6158 0.6917 0.073 Uiso 1 1 calc R . . C33 C 0.0800(3) -0.4244(6) 0.6871(2) 0.0372(14) Uani 1 1 d . . . H33 H 0.0473 -0.4401 0.6940 0.045 Uiso 1 1 calc R . . C34 C -0.2181(2) 0.1250(9) 0.5606(2) 0.0521(18) Uani 1 1 d . . . H34 H -0.2460 0.1580 0.5412 0.063 Uiso 1 1 calc R . . C35 C -0.2251(2) 0.0350(7) 0.5930(2) 0.0428(16) Uani 1 1 d . . . H35 H -0.2575 0.0020 0.5951 0.051 Uiso 1 1 calc R . . C36 C -0.1831(2) -0.0088(7) 0.6235(2) 0.0418(15) Uani 1 1 d . . . H36 H -0.1875 -0.0699 0.6464 0.050 Uiso 1 1 calc R . . C37 C -0.1353(2) 0.0396(6) 0.6191(2) 0.0387(15) Uani 1 1 d . . . H37 H -0.1071 0.0130 0.6394 0.046 Uiso 1 1 calc R . . C38 C -0.1301(2) 0.1266(7) 0.5849(2) 0.0368(14) Uani 1 1 d . . . H38 H -0.0979 0.1585 0.5812 0.044 Uiso 1 1 calc R . . C39 C -0.1142(3) 0.3089(8) 0.4657(2) 0.0508(17) Uani 1 1 d . . . H39 H -0.1071 0.2187 0.4643 0.061 Uiso 1 1 calc R . . C40 C -0.0918(3) 0.3909(11) 0.4390(3) 0.068(2) Uani 1 1 d . . . H40 H -0.0691 0.3569 0.4204 0.081 Uiso 1 1 calc R . . C41 C -0.1015(3) 0.5219(10) 0.4384(3) 0.067(2) Uani 1 1 d . . . H41 H -0.0857 0.5790 0.4198 0.081 Uiso 1 1 calc R . . C42 C -0.1351(4) 0.5683(8) 0.4658(3) 0.070(2) Uani 1 1 d . . . H42 H -0.1434 0.6580 0.4660 0.084 Uiso 1 1 calc R . . C43 C -0.1569(3) 0.4773(9) 0.4940(3) 0.061(2) Uani 1 1 d . . . H43 H -0.1797 0.5083 0.5131 0.073 Uiso 1 1 calc R . . S1 S -0.2260(2) -0.0662(6) 0.44649(18) 0.0467(13) Uani 0.260(3) 1 d PGU A 1 O5 O -0.1910(3) -0.1147(11) 0.4840(2) 0.0448(19) Uani 0.260(3) 1 d PGU A 1 O6 O -0.2701(3) -0.1504(10) 0.4350(3) 0.059(3) Uani 0.260(3) 1 d PGU A 1 O7 O -0.2343(4) 0.0704(6) 0.4452(3) 0.055(2) Uani 0.260(3) 1 d PGU A 1 C44 C -0.1907(3) -0.0939(8) 0.3989(2) 0.067(2) Uani 0.260(3) 1 d PGU A 1 F1 F -0.1880(5) -0.2128(10) 0.3861(4) 0.070(2) Uani 0.260(3) 1 d PGU A 1 F2 F -0.2156(4) -0.0376(13) 0.3605(2) 0.068(2) Uani 0.260(3) 1 d PGU A 1 F3 F -0.1435(3) -0.0410(13) 0.4085(4) 0.071(2) Uani 0.260(3) 1 d PGU A 1 S2 S -0.1954(3) -0.0396(6) 0.4544(2) 0.0499(14) Uani 0.240(3) 1 d PGU A 2 O8 O -0.2060(4) -0.1459(9) 0.4838(2) 0.0392(19) Uani 0.240(3) 1 d PGU A 2 O9 O -0.2312(4) 0.0688(9) 0.4536(4) 0.0529(19) Uani 0.240(3) 1 d PGU A 2 O10 O -0.1442(3) -0.0070(11) 0.4547(3) 0.062(2) Uani 0.240(3) 1 d PGU A 2 C45 C -0.2125(4) -0.1138(9) 0.3985(2) 0.071(2) Uani 0.240(3) 1 d PGU A 2 F4 F -0.2597(4) -0.1259(14) 0.3854(3) 0.084(3) Uani 0.240(3) 1 d PGU A 2 F5 F -0.1988(5) -0.0321(14) 0.3658(2) 0.070(2) Uani 0.240(3) 1 d PGU A 2 F6 F -0.1888(5) -0.2321(10) 0.3968(4) 0.071(2) Uani 0.240(3) 1 d PGU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.01647(16) 0.02850(18) 0.02475(16) 0.000 0.00328(10) 0.000 O1 0.0221(19) 0.029(2) 0.033(2) -0.0011(16) 0.0058(15) -0.0016(16) O2 0.0263(19) 0.029(2) 0.0282(19) -0.0005(16) 0.0062(15) 0.0023(16) O3 0.0270(19) 0.031(2) 0.0243(19) 0.0013(16) 0.0045(15) 0.0007(17) O4 0.0200(18) 0.029(2) 0.0314(19) -0.0023(16) 0.0007(15) 0.0048(15) N1 0.029(2) 0.035(3) 0.038(3) -0.008(2) 0.006(2) -0.002(2) N2 0.042(3) 0.064(4) 0.035(3) 0.012(3) 0.000(2) -0.012(3) N3 0.045(3) 0.050(4) 0.041(3) 0.005(3) 0.003(2) -0.008(3) C1 0.023(3) 0.030(3) 0.032(3) 0.005(2) 0.005(2) -0.001(2) C2 0.021(3) 0.029(3) 0.028(3) 0.006(2) 0.004(2) -0.001(2) C3 0.028(3) 0.031(3) 0.029(3) 0.005(2) 0.003(2) -0.001(3) C4 0.032(3) 0.034(3) 0.040(3) 0.004(3) 0.001(2) -0.008(3) C5 0.024(3) 0.038(4) 0.057(4) 0.005(3) 0.005(3) -0.010(3) C6 0.024(3) 0.045(4) 0.045(3) 0.010(3) 0.008(2) -0.001(3) C7 0.031(3) 0.028(3) 0.032(3) -0.002(2) 0.002(2) -0.004(2) C8 0.035(3) 0.021(3) 0.031(3) -0.004(2) 0.002(2) -0.001(2) C9 0.033(3) 0.027(3) 0.029(3) -0.007(2) 0.008(2) 0.006(2) C10 0.045(4) 0.035(3) 0.032(3) -0.005(3) 0.013(3) 0.008(3) C11 0.067(4) 0.039(4) 0.028(3) 0.000(3) 0.009(3) 0.002(3) C12 0.064(4) 0.036(4) 0.032(3) -0.004(3) -0.006(3) -0.009(3) C13 0.048(4) 0.027(3) 0.038(3) 0.001(3) -0.002(3) 0.001(3) C14 0.041(4) 0.045(4) 0.031(3) -0.003(3) 0.016(3) 0.002(3) C15 0.034(3) 0.042(4) 0.034(3) 0.005(3) 0.009(3) -0.006(3) C16 0.024(3) 0.034(3) 0.027(3) 0.005(2) 0.005(2) -0.004(2) C17 0.020(3) 0.038(3) 0.035(3) 0.005(3) 0.005(2) -0.005(2) C18 0.029(3) 0.041(4) 0.047(4) 0.013(3) 0.003(3) -0.005(3) C19 0.045(4) 0.059(5) 0.032(3) 0.015(3) 0.009(3) -0.003(3) C20 0.043(4) 0.049(4) 0.032(3) 0.007(3) 0.012(3) -0.002(3) C21 0.026(3) 0.026(3) 0.040(3) 0.001(3) 0.003(2) -0.005(2) C22 0.029(3) 0.022(3) 0.034(3) 0.000(2) 0.001(2) -0.001(2) C23 0.025(3) 0.023(3) 0.035(3) -0.003(2) 0.004(2) 0.003(2) C24 0.021(3) 0.028(3) 0.033(3) -0.004(2) 0.007(2) 0.000(2) C25 0.024(3) 0.031(3) 0.041(3) 0.000(3) 0.002(2) 0.003(2) C26 0.029(3) 0.032(3) 0.041(3) 0.000(3) -0.002(2) 0.003(3) C27 0.033(3) 0.029(3) 0.037(3) 0.000(3) 0.000(2) 0.004(3) C28 0.021(3) 0.042(3) 0.030(3) -0.001(3) 0.004(2) 0.006(3) C29 0.042(4) 0.059(5) 0.059(4) -0.026(4) 0.022(3) -0.021(4) C30 0.042(3) 0.085(4) 0.066(4) -0.026(3) 0.011(3) 0.000(3) C31 0.067(4) 0.075(4) 0.063(4) -0.017(3) -0.009(3) 0.023(4) C32 0.086(6) 0.051(4) 0.041(4) -0.003(3) -0.008(4) 0.015(4) C33 0.038(3) 0.038(4) 0.035(3) -0.001(3) 0.004(3) -0.002(3) C34 0.032(3) 0.082(5) 0.039(4) 0.010(4) -0.006(3) -0.010(4) C35 0.033(3) 0.053(4) 0.042(4) 0.001(3) 0.004(3) -0.009(3) C36 0.038(4) 0.039(4) 0.047(4) 0.003(3) 0.002(3) -0.002(3) C37 0.034(3) 0.036(4) 0.043(4) -0.001(3) -0.004(3) 0.003(3) C38 0.033(3) 0.038(3) 0.040(3) -0.003(3) 0.003(3) -0.003(3) C39 0.059(4) 0.050(4) 0.042(4) -0.006(3) 0.001(3) 0.008(4) C40 0.053(5) 0.113(8) 0.039(4) 0.001(4) 0.015(3) -0.003(5) C41 0.067(4) 0.073(4) 0.058(4) 0.011(3) -0.007(3) -0.021(4) C42 0.079(4) 0.053(4) 0.070(4) -0.001(3) -0.020(3) -0.005(3) C43 0.050(4) 0.080(6) 0.051(4) -0.026(4) -0.002(3) 0.006(4) S1 0.060(3) 0.044(2) 0.038(2) -0.006(2) 0.014(2) 0.008(2) O5 0.063(4) 0.039(3) 0.033(3) -0.006(3) 0.012(3) 0.015(3) O6 0.073(5) 0.058(5) 0.048(5) -0.008(4) 0.014(4) -0.012(5) O7 0.069(4) 0.051(4) 0.046(4) -0.002(4) 0.011(4) 0.010(4) C44 0.081(4) 0.067(3) 0.057(3) 0.001(3) 0.020(3) 0.017(3) F1 0.090(4) 0.068(4) 0.055(4) 0.001(4) 0.020(4) 0.017(4) F2 0.078(4) 0.070(4) 0.058(4) -0.002(3) 0.021(4) 0.019(4) F3 0.079(4) 0.067(4) 0.068(4) 0.006(4) 0.011(4) 0.008(4) S2 0.065(3) 0.043(3) 0.043(2) -0.009(2) 0.013(3) 0.008(3) O8 0.056(4) 0.035(3) 0.029(3) -0.006(3) 0.015(3) 0.009(3) O9 0.067(4) 0.048(3) 0.044(3) -0.004(3) 0.009(3) 0.009(3) O10 0.070(4) 0.055(4) 0.061(4) -0.001(4) 0.015(4) 0.011(4) C45 0.086(4) 0.070(3) 0.059(3) -0.002(3) 0.018(3) 0.018(3) F4 0.098(5) 0.081(5) 0.074(5) -0.008(5) 0.015(5) 0.003(5) F5 0.082(4) 0.071(4) 0.061(4) -0.002(3) 0.021(4) 0.019(4) F6 0.089(4) 0.069(4) 0.057(4) -0.001(4) 0.017(4) 0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O3 2.141(3) . ? U O3 2.141(3) 2_556 ? U O1 2.154(4) . ? U O1 2.154(4) 2_556 ? U O4 2.185(4) 2_556 ? U O4 2.185(3) . ? U O2 2.866(4) 2_556 ? U O2 2.866(4) . ? O1 C2 1.344(7) . ? O2 C9 1.389(6) . ? O3 C16 1.354(6) . ? O4 C23 1.344(6) . ? N1 C29 1.324(7) . ? N1 C33 1.332(8) . ? N2 C34 1.336(8) . ? N2 C38 1.340(8) . ? N3 C39 1.320(9) . ? N3 C43 1.336(11) . ? C1 C2 1.401(8) . ? C1 C6 1.411(8) . ? C1 C28 1.514(9) . ? C2 C3 1.413(8) . ? C3 C4 1.396(8) . ? C3 C7 1.509(8) . ? C4 C5 1.369(9) . ? C5 C6 1.380(8) . ? C7 C8 1.526(8) . ? C8 C9 1.383(8) . ? C8 C13 1.391(8) . ? C9 C10 1.398(8) . ? C10 C11 1.416(9) . ? C10 C14 1.517(9) . ? C11 C12 1.348(9) . ? C12 C13 1.391(9) . ? C14 C15 1.512(8) . ? C15 C16 1.404(8) . ? C15 C20 1.406(8) . ? C16 C17 1.402(8) . ? C17 C18 1.401(8) . ? C17 C21 1.503(8) . ? C18 C19 1.383(9) . ? C19 C20 1.363(9) . ? C21 C22 1.506(8) . ? C22 C27 1.404(8) . ? C22 C23 1.409(8) . ? C23 C24 1.415(7) . ? C24 C25 1.389(8) . ? C24 C28 1.509(8) . ? C25 C26 1.396(8) . ? C26 C27 1.372(8) . ? C29 C30 1.403(11) . ? C30 C31 1.324(13) . ? C31 C32 1.373(12) . ? C32 C33 1.363(10) . ? C34 C35 1.343(10) . ? C35 C36 1.399(9) . ? C36 C37 1.377(9) . ? C37 C38 1.353(9) . ? C39 C40 1.332(11) . ? C40 C41 1.344(13) . ? C41 C42 1.358(13) . ? C42 C43 1.410(13) . ? S1 O7 1.3923 . ? S1 O5 1.4263 . ? S1 O6 1.4432 . ? S1 C44 1.8026 . ? C44 F1 1.2616 . ? C44 F3 1.3512 . ? C44 F2 1.3519 . ? S2 O10 1.3921 . ? S2 O8 1.4262 . ? S2 O9 1.4434 . ? S2 C45 1.8028 . ? C45 F4 1.2614 . ? C45 F6 1.3509 . ? C45 F5 1.3516 . ? 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 O3 U O3 156.6(2) . 2_556 ? O3 U O1 89.62(14) . . ? O3 U O1 101.79(14) 2_556 . ? O3 U O1 101.79(14) . 2_556 ? O3 U O1 89.62(14) 2_556 2_556 ? O1 U O1 121.7(2) . 2_556 ? O3 U O4 79.94(14) . 2_556 ? O3 U O4 82.26(14) 2_556 2_556 ? O1 U O4 158.39(14) . 2_556 ? O1 U O4 79.20(13) 2_556 2_556 ? O3 U O4 82.26(14) . . ? O3 U O4 79.94(14) 2_556 . ? O1 U O4 79.20(13) . . ? O1 U O4 158.39(15) 2_556 . ? O4 U O4 80.66(19) 2_556 . ? O3 U O2 135.70(13) . 2_556 ? O3 U O2 67.51(13) 2_556 2_556 ? O1 U O2 64.41(12) . 2_556 ? O1 U O2 68.43(12) 2_556 2_556 ? O4 U O2 134.95(12) 2_556 2_556 ? O4 U O2 123.05(12) . 2_556 ? O3 U O2 67.51(13) . . ? O3 U O2 135.70(13) 2_556 . ? O1 U O2 68.43(12) . . ? O1 U O2 64.41(12) 2_556 . ? O4 U O2 123.05(12) 2_556 . ? O4 U O2 134.95(12) . . ? O2 U O2 69.62(14) 2_556 . ? C2 O1 U 170.3(4) . . ? C9 O2 U 120.8(3) . . ? C16 O3 U 165.3(4) . . ? C23 O4 U 132.0(3) . . ? C29 N1 C33 116.8(6) . . ? C34 N2 C38 122.1(6) . . ? C39 N3 C43 116.4(6) . . ? C2 C1 C6 118.4(5) . . ? C2 C1 C28 120.5(5) . . ? C6 C1 C28 121.1(5) . . ? O1 C2 C1 119.4(5) . . ? O1 C2 C3 119.9(5) . . ? C1 C2 C3 120.7(5) . . ? C4 C3 C2 118.6(5) . . ? C4 C3 C7 121.6(5) . . ? C2 C3 C7 119.8(5) . . ? C5 C4 C3 121.0(6) . . ? C4 C5 C6 120.8(5) . . ? C5 C6 C1 120.4(6) . . ? C3 C7 C8 112.5(5) . . ? C9 C8 C13 119.0(5) . . ? C9 C8 C7 121.2(5) . . ? C13 C8 C7 119.7(5) . . ? C8 C9 O2 118.1(5) . . ? C8 C9 C10 121.8(5) . . ? O2 C9 C10 120.0(5) . . ? C9 C10 C11 116.9(6) . . ? C9 C10 C14 122.8(5) . . ? C11 C10 C14 120.0(5) . . ? C12 C11 C10 121.8(6) . . ? C11 C12 C13 120.2(6) . . ? C12 C13 C8 120.1(6) . . ? C15 C14 C10 111.1(5) . . ? C16 C15 C20 118.3(6) . . ? C16 C15 C14 119.8(5) . . ? C20 C15 C14 121.8(6) . . ? O3 C16 C17 120.6(5) . . ? O3 C16 C15 118.3(5) . . ? C17 C16 C15 121.1(5) . . ? C18 C17 C16 118.1(5) . . ? C18 C17 C21 121.3(6) . . ? C16 C17 C21 120.5(5) . . ? C19 C18 C17 120.9(6) . . ? C20 C19 C18 120.5(6) . . ? C19 C20 C15 121.0(6) . . ? C17 C21 C22 114.2(5) . . ? C27 C22 C23 118.3(5) . . ? C27 C22 C21 121.6(5) . . ? C23 C22 C21 120.1(5) . . ? O4 C23 C22 120.1(5) . . ? O4 C23 C24 119.6(5) . . ? C22 C23 C24 120.3(5) . . ? C25 C24 C23 118.6(5) . . ? C25 C24 C28 121.0(5) . . ? C23 C24 C28 120.4(5) . . ? C24 C25 C26 121.7(5) . . ? C27 C26 C25 118.9(5) . . ? C26 C27 C22 122.0(6) . . ? C24 C28 C1 111.3(4) . . ? N1 C29 C30 121.8(7) . . ? C31 C30 C29 120.0(7) . . ? C30 C31 C32 119.0(8) . . ? C33 C32 C31 118.3(8) . . ? N1 C33 C32 124.0(7) . . ? N2 C34 C35 119.8(6) . . ? C34 C35 C36 119.5(6) . . ? C37 C36 C35 119.2(6) . . ? C38 C37 C36 119.0(6) . . ? N2 C38 C37 120.3(6) . . ? N3 C39 C40 124.0(8) . . ? C39 C40 C41 121.2(8) . . ? C40 C41 C42 118.0(8) . . ? C41 C42 C43 118.4(8) . . ? N3 C43 C42 122.0(7) . . ? O7 S1 O5 116.2 . . ? O7 S1 O6 117.2 . . ? O5 S1 O6 113.5 . . ? O7 S1 C44 103.2 . . ? O5 S1 C44 101.1 . . ? O6 S1 C44 102.4 . . ? F1 C44 F3 110.4 . . ? F1 C44 F2 101.0 . . ? F3 C44 F2 109.9 . . ? F1 C44 S1 115.8 . . ? F3 C44 S1 109.8 . . ? F2 C44 S1 109.6 . . ? O10 S2 O8 116.3 . . ? O10 S2 O9 117.2 . . ? O8 S2 O9 113.4 . . ? O10 S2 C45 103.2 . . ? O8 S2 C45 101.1 . . ? O9 S2 C45 102.4 . . ? F4 C45 F6 110.4 . . ? F4 C45 F5 101.0 . . ? F6 C45 F5 109.9 . . ? F4 C45 S2 115.8 . . ? F6 C45 S2 109.8 . . ? F5 C45 S2 109.6 . . ? 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 O2 H2 N1 0.97 1.83 2.717(6) 151.7 . N2 H2N N3 0.96 1.77 2.724(7) 174.1 .