Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michel Ephritikhine' 'Lionel Salmon' 'Pierre Thuery' _publ_contact_author_name 'M. Ephritikhine' _publ_contact_author_address ; CEA/Saclay, SCM (CNRS URA 331) Bat. 125 91191 Gif-sur-Yvette France ; _publ_contact_author_phone '33 (0) 1 69 08 64 36' _publ_contact_author_fax '33 (0) 1 69 08 66 40' _publ_contact_author_email ephri@drecam.cea.fr _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and crystal structure of tetra- and hexanuclear uranium(IV) complexes with hexadentate compartmental Schiff-base ligands ; data_4 _database_code_depnum_ccdc_archive 'CCDC 250666' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Cl2 N2 O5 U' _chemical_formula_weight 735.43 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' 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 '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 9.9047(6) _cell_length_b 22.5476(15) _cell_length_c 11.8755(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.804(4) _cell_angle_gamma 90.00 _cell_volume 2564.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8699 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method ? _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 6.576 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.178 _exptl_absorpt_correction_T_max 0.272 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 8699 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2269 _reflns_number_gt 2127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. The bridge linking the two N of the Schiff base and the C atoms of the THF molecule were found to be disordered over two positions which were refined with occupancy factors fixed to 0.5 (necessary to account for the relation between the disordered parts) and some restraints on bond lengths. Refinement in the non-centrosymmetric space group Cc was not satisfying, resulting in unstable bond lengths and displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters, except the disordered ones. The H atoms were introduced at calculated positions (except those of the disordered parts) and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH) or 1.5 (CH3) 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^)+(0.0452P)^2^+19.7204P] 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 2269 _refine_ls_number_parameters 163 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 1.633 _refine_diff_density_min -1.482 _refine_diff_density_rms 0.136 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 0.5000 0.630175(14) 0.7500 0.03219(15) Uani 1 2 d S . . Cl Cl 0.64755(19) 0.63106(8) 0.97052(17) 0.0448(4) Uani 1 1 d . . . N N 0.6123(8) 0.5308(3) 0.7041(9) 0.082(3) Uani 1 1 d D . . O1 O 0.8509(5) 0.7316(2) 0.6351(4) 0.0393(11) Uani 1 1 d . . . O2 O 0.6853(4) 0.6509(2) 0.6935(4) 0.0339(10) Uani 1 1 d . . . O3 O 0.5000 0.7386(3) 0.7500 0.0425(17) Uani 1 2 d S . . C1 C 0.9295(8) 0.7750(4) 0.5905(7) 0.0477(18) Uani 1 1 d . . . H1A H 1.0254 0.7736 0.6343 0.072 Uiso 1 1 calc R . . H1B H 0.8921 0.8137 0.5973 0.072 Uiso 1 1 calc R . . H1C H 0.9235 0.7667 0.5101 0.072 Uiso 1 1 calc R . . C2 C 0.8798(7) 0.6735(3) 0.6184(6) 0.0342(14) Uani 1 1 d . . . C3 C 0.7888(7) 0.6321(3) 0.6492(6) 0.0339(14) Uani 1 1 d . . . C4 C 0.8112(7) 0.5726(3) 0.6331(6) 0.0401(16) Uani 1 1 d D . . C5 C 0.9227(8) 0.5531(4) 0.5908(8) 0.0503(19) Uani 1 1 d . . . H5 H 0.9363 0.5128 0.5811 0.060 Uiso 1 1 calc R . . C6 C 1.0113(8) 0.5937(4) 0.5639(7) 0.053(2) Uani 1 1 d . . . H6 H 1.0860 0.5810 0.5360 0.064 Uiso 1 1 calc R . . C7 C 0.9909(7) 0.6541(4) 0.5779(6) 0.0446(17) Uani 1 1 d . . . H7 H 1.0524 0.6814 0.5598 0.053 Uiso 1 1 calc R . . C8 C 0.7139(8) 0.5280(3) 0.6536(8) 0.059(2) Uani 1 1 d D . . H8 H 0.7270 0.4906 0.6251 0.071 Uiso 1 1 calc R . . C9A C 0.5461(11) 0.4767(4) 0.7395(9) 0.039(3) Uiso 0.50 1 d PD . . C9B C 0.5036(15) 0.4886(7) 0.6505(11) 0.056(4) Uiso 0.50 1 d PD . . C10 C 0.4179(10) 0.4622(6) 0.6346(12) 0.053(4) Uani 0.50 1 d PD . . C11 C 0.6306(15) 0.4205(6) 0.7807(18) 0.084(7) Uani 0.50 1 d PD . . C12 C 0.6245(8) 0.7755(3) 0.7975(8) 0.052(2) Uani 1 1 d D . . C13A C 0.6023(13) 0.8355(5) 0.7430(14) 0.048(4) Uiso 0.50 1 d PD . . C13B C 0.5530(12) 0.8371(5) 0.7639(14) 0.046(4) Uiso 0.50 1 d PD . . 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 0.0299(2) 0.0345(2) 0.0350(2) 0.000 0.01350(14) 0.000 Cl 0.0408(9) 0.0567(11) 0.0371(11) 0.0020(7) 0.0103(7) 0.0062(7) N 0.061(5) 0.052(4) 0.153(9) -0.035(5) 0.064(6) -0.011(4) O1 0.035(2) 0.050(3) 0.037(3) 0.000(2) 0.015(2) -0.007(2) O2 0.030(2) 0.041(2) 0.033(3) -0.0023(19) 0.0125(18) 0.0002(19) O3 0.032(3) 0.034(4) 0.066(5) 0.000 0.022(3) 0.000 C1 0.042(4) 0.057(5) 0.045(5) 0.008(3) 0.013(3) -0.009(3) C2 0.032(3) 0.050(4) 0.020(3) -0.003(3) 0.006(2) -0.001(3) C3 0.027(3) 0.049(4) 0.025(4) -0.006(3) 0.006(2) 0.000(3) C4 0.043(4) 0.051(4) 0.029(4) -0.009(3) 0.014(3) 0.002(3) C5 0.053(5) 0.056(5) 0.050(5) -0.008(4) 0.026(4) 0.008(4) C6 0.045(4) 0.074(6) 0.049(5) -0.013(4) 0.027(4) 0.005(4) C7 0.037(4) 0.068(5) 0.031(4) -0.002(3) 0.014(3) -0.004(3) C8 0.053(5) 0.048(5) 0.086(7) -0.022(4) 0.035(5) -0.003(4) C10 0.047(9) 0.052(10) 0.063(12) -0.017(8) 0.019(8) -0.017(7) C11 0.074(13) 0.044(11) 0.13(2) 0.032(11) 0.021(13) 0.014(9) C12 0.049(4) 0.046(4) 0.065(6) -0.011(4) 0.024(4) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O2 2.160(4) . ? U O2 2.160(4) 2_656 ? U O3 2.444(7) . ? U N 2.621(7) 2_656 ? U N 2.621(7) . ? U Cl 2.6530(19) . ? U Cl 2.6531(19) 2_656 ? N C8 1.298(10) . ? N C9B 1.455(10) . ? N C9A 1.495(9) . ? N N 2.717(14) 2_656 ? N O2 2.815(8) . ? O1 C2 1.365(9) . ? O1 C1 1.434(8) . ? O2 C3 1.336(8) . ? O2 O2 4.218(8) 2_656 ? O3 C12 1.475(8) . ? O3 C12 1.475(8) 2_656 ? C2 C7 1.380(10) . ? C2 C3 1.410(10) . ? C3 C4 1.380(10) . ? C4 C5 1.396(10) . ? C4 C8 1.456(8) . ? C5 C6 1.362(12) . ? C6 C7 1.392(13) . ? C9A C11 1.528(9) . ? C9A C9B 1.533(10) 2_656 ? C9A C10 1.570(9) . ? C9B C9A 1.533(10) 2_656 ? C10 C9A 1.48(2) 2_656 ? C10 C11 1.54(3) 2_656 ? C11 C10 1.54(3) 2_656 ? C12 C13A 1.491(10) . ? C12 C13B 1.564(10) . ? C13A C13B 1.520(11) 2_656 ? C13B C13A 1.520(11) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U O2 155.0(3) . 2_656 ? O2 U O3 77.49(13) . . ? O2 U O3 77.49(13) 2_656 . ? O2 U N 133.58(19) . 2_656 ? O2 U N 71.40(19) 2_656 2_656 ? O3 U N 148.78(15) . 2_656 ? O2 U N 71.40(19) . . ? O2 U N 133.58(19) 2_656 . ? O3 U N 148.78(15) . . ? N U N 62.4(3) 2_656 . ? O2 U Cl 90.44(13) . . ? O2 U Cl 89.37(13) 2_656 . ? O3 U Cl 89.57(4) . . ? N U Cl 87.5(2) 2_656 . ? N U Cl 93.2(2) . . ? O2 U Cl 89.37(13) . 2_656 ? O2 U Cl 90.44(13) 2_656 2_656 ? O3 U Cl 89.57(4) . 2_656 ? N U Cl 93.2(2) 2_656 2_656 ? N U Cl 87.5(2) . 2_656 ? Cl U Cl 179.14(8) . 2_656 ? C8 N C9B 109.9(9) . . ? C8 N C9A 122.6(7) . . ? C2 O1 C1 116.6(6) . . ? C12 O3 C12 111.3(7) . 2_656 ? O1 C2 C7 124.8(7) . . ? O1 C2 C3 115.2(6) . . ? C7 C2 C3 120.0(7) . . ? O2 C3 C4 122.0(6) . . ? O2 C3 C2 119.8(6) . . ? C4 C3 C2 118.2(6) . . ? C3 C4 C5 121.7(7) . . ? C3 C4 C8 120.8(6) . . ? C5 C4 C8 117.4(7) . . ? C6 C5 C4 119.3(7) . . ? C5 C6 C7 120.5(7) . . ? C2 C7 C6 120.4(7) . . ? N C8 C4 131.9(7) . . ? C10 C9A N 117.0(10) 2_656 . ? N C9A C11 121.5(8) . . ? N C9A C9B 110.9(10) . 2_656 ? C11 C9A C9B 98.2(11) . 2_656 ? N C9A C10 105.7(7) . . ? C11 C9A C10 110.3(8) . . ? C9B C9A C10 110.0(10) 2_656 . ? N C9B C9A 96.0(8) . 2_656 ? O3 C12 C13A 109.3(8) . . ? O3 C12 C13B 97.1(7) . . ? C12 C13A C13B 94.6(9) . 2_656 ? C13A C13B C12 112.2(10) 2_656 . ? #===END data_6a.2HpyCl.2py _database_code_depnum_ccdc_archive 'CCDC 250667' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H94 Cl8 N14 O16 U4' _chemical_formula_weight 2959.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.233(3) _cell_length_b 13.0849(19) _cell_length_c 17.421(4) _cell_angle_alpha 80.235(15) _cell_angle_beta 83.042(11) _cell_angle_gamma 70.043(12) _cell_volume 2577.1(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16587 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method ? _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 6.542 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.384 _exptl_absorpt_correction_T_max 0.762 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 16587 _diffrn_reflns_av_R_equivalents 0.1197 _diffrn_reflns_av_sigmaI/netI 0.1826 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8797 _reflns_number_gt 5210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The pyridine molecule and the two pyridinium ions have been refined as idealized hexagons with some restraints on displacement parameters. The H atoms were introduced at calculated positions (except those bound to O2B and O3B, which were not found, nor introduced) and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Some voids in the lattice indicate the presence of another, unresolved, solvent molecule, to which corresponds also the highest residual electron density peak. 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^)+(0.0207P)^2^+31.3650P] 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 8797 _refine_ls_number_parameters 595 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1481 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 1.966 _refine_diff_density_min -1.739 _refine_diff_density_rms 0.225 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 0.16384(6) 0.17747(5) 0.82928(4) 0.0308(2) Uani 1 1 d . . . U2 U 0.30132(6) 0.27942(5) 0.63848(4) 0.0314(2) Uani 1 1 d . . . Cl1 Cl -0.0325(4) 0.1631(4) 0.7809(3) 0.0426(12) Uani 1 1 d . . . Cl2 Cl 0.3335(5) 0.4609(4) 0.6772(3) 0.0523(14) Uani 1 1 d . . . Cl3 Cl 0.4008(4) 0.3422(4) 0.4920(3) 0.0397(11) Uani 1 1 d . . . Cl4 Cl 0.3290(5) 0.4496(4) 1.0347(4) 0.0657(18) Uani 1 1 d . . . O1A O 0.1335(11) 0.3937(10) 0.5899(7) 0.037(3) Uani 1 1 d . . . O2A O 0.1363(10) 0.3341(9) 0.7388(7) 0.030(3) Uani 1 1 d . . . O3A O 0.3330(10) 0.2203(9) 0.7798(7) 0.029(3) Uani 1 1 d . . . O4A O 0.4925(11) 0.1895(10) 0.6646(7) 0.036(3) Uani 1 1 d . . . N1A N 0.0172(14) 0.3392(13) 0.8869(10) 0.038(4) Uani 1 1 d . . . N2A N 0.2684(14) 0.2005(11) 0.9426(9) 0.034(4) Uani 1 1 d . . . C1A C 0.0390(14) 0.4424(16) 0.6335(11) 0.036(5) Uani 1 1 d . . . C2A C 0.0410(15) 0.4078(14) 0.7145(9) 0.028(4) Uani 1 1 d . . . C3A C -0.0568(17) 0.4564(15) 0.7668(11) 0.035(4) Uani 1 1 d U . . C4A C -0.1555(16) 0.5338(16) 0.7336(13) 0.045(5) Uani 1 1 d . . . H4A H -0.2212 0.5643 0.7657 0.054 Uiso 1 1 calc R . . C5A C -0.1566(19) 0.5655(16) 0.6536(13) 0.046(5) Uani 1 1 d . . . H5A H -0.2228 0.6187 0.6335 0.055 Uiso 1 1 calc R . . C6A C -0.0634(16) 0.5215(16) 0.6027(12) 0.041(5) Uani 1 1 d . . . H6A H -0.0675 0.5432 0.5491 0.050 Uiso 1 1 calc R . . C7A C -0.0596(16) 0.4242(15) 0.8505(10) 0.031(4) Uani 1 1 d . . . H7A H -0.1206 0.4670 0.8806 0.038 Uiso 1 1 calc R . . C8A C -0.0019(16) 0.3268(15) 0.9721(11) 0.037(5) Uani 1 1 d . . . H8A1 H -0.0147 0.2573 0.9907 0.045 Uiso 1 1 calc R . . H8A2 H -0.0713 0.3851 0.9870 0.045 Uiso 1 1 calc R . . C9A C 0.1021(16) 0.3308(16) 1.0105(11) 0.039(5) Uani 1 1 d . . . H9A1 H 0.0762 0.3519 1.0622 0.046 Uiso 1 1 calc R . . H9A2 H 0.1308 0.3869 0.9801 0.046 Uiso 1 1 calc R . . C10A C 0.2036(17) 0.2199(18) 1.0180(12) 0.045(5) Uani 1 1 d . . . H10C H 0.2560 0.2206 1.0553 0.054 Uiso 1 1 calc R . . H10D H 0.1726 0.1606 1.0373 0.054 Uiso 1 1 calc R . . C11A C 0.3848(19) 0.1738(14) 0.9427(11) 0.039(5) Uani 1 1 d . . . H11A H 0.4142 0.1690 0.9904 0.047 Uiso 1 1 calc R . . C12A C 0.4688(15) 0.1517(15) 0.8770(12) 0.036(5) Uani 1 1 d . . . C13A C 0.4404(16) 0.1744(14) 0.8006(11) 0.031(4) Uani 1 1 d . . . C14A C 0.5279(16) 0.1612(14) 0.7380(11) 0.034(4) Uani 1 1 d . . . C15A C 0.6440(17) 0.1179(14) 0.7555(10) 0.034(4) Uani 1 1 d . . . H15A H 0.7020 0.1063 0.7150 0.041 Uiso 1 1 calc R . . C16A C 0.6753(18) 0.0910(15) 0.8334(11) 0.039(5) Uani 1 1 d . . . H16A H 0.7531 0.0635 0.8452 0.046 Uiso 1 1 calc R . . C17A C 0.5865(17) 0.1071(14) 0.8918(10) 0.035(4) Uani 1 1 d . . . H17A H 0.6060 0.0873 0.9434 0.042 Uiso 1 1 calc R . . O1B O 0.2302(11) 0.1300(10) 0.7007(7) 0.033(3) Uani 1 1 d . . . O2B O 0.3239(10) 0.1446(10) 0.5581(7) 0.031(3) Uani 1 1 d . . . O3B O 0.6889(10) -0.0005(9) 0.1545(6) 0.025(3) Uani 1 1 d . . . O4B O 0.8786(12) -0.0673(10) 0.0672(8) 0.042(3) Uani 1 1 d . . . N1B N 0.4002(15) 0.0665(13) 0.4266(8) 0.039(4) Uani 1 1 d . . . N2B N 0.4801(16) 0.1475(13) 0.1765(10) 0.044(4) Uani 1 1 d . . . C1B C 0.2494(17) 0.0408(15) 0.6598(11) 0.034(4) Uani 1 1 d . . . C2B C 0.3009(17) 0.0549(15) 0.5854(10) 0.035(4) Uani 1 1 d . . . C3B C 0.3302(16) -0.0346(15) 0.5388(11) 0.032(4) Uani 1 1 d U . . C4B C 0.3043(19) -0.1321(18) 0.5729(13) 0.049(6) Uani 1 1 d . . . H4B H 0.3202 -0.1902 0.5444 0.059 Uiso 1 1 calc R . . C5B C 0.255(2) -0.1389(18) 0.6497(13) 0.051(6) Uani 1 1 d . . . H5B H 0.2401 -0.2029 0.6726 0.062 Uiso 1 1 calc R . . C6B C 0.2274(16) -0.0515(15) 0.6921(12) 0.042(5) Uani 1 1 d . . . H6B H 0.1938 -0.0569 0.7428 0.050 Uiso 1 1 calc R . . C7B C 0.379(2) -0.0259(16) 0.4604(13) 0.049(6) Uani 1 1 d . . . H7B H 0.3958 -0.0844 0.4322 0.059 Uiso 1 1 calc R . . C8B C 0.4365(18) 0.0811(16) 0.3447(10) 0.041(5) Uani 1 1 d . . . H8B1 H 0.4427 0.0160 0.3225 0.049 Uiso 1 1 calc R . . H8B2 H 0.5131 0.0891 0.3390 0.049 Uiso 1 1 calc R . . C9B C 0.3550(18) 0.1779(15) 0.3005(11) 0.039(5) Uani 1 1 d . . . H9B1 H 0.3706 0.2432 0.3083 0.047 Uiso 1 1 calc R . . H9B2 H 0.2760 0.1849 0.3215 0.047 Uiso 1 1 calc R . . C10B C 0.3631(19) 0.1726(17) 0.2131(13) 0.047(5) Uani 1 1 d . . . H10A H 0.3312 0.1172 0.2049 0.056 Uiso 1 1 calc R . . H10B H 0.3152 0.2426 0.1875 0.056 Uiso 1 1 calc R . . C11B C 0.5186(18) 0.2138(14) 0.1231(10) 0.036(5) Uani 1 1 d . . . H11B H 0.4707 0.2859 0.1106 0.043 Uiso 1 1 calc R . . C12B C 0.6310(16) 0.1782(17) 0.0843(10) 0.037(5) Uani 1 1 d . . . C13B C 0.7075(13) 0.0697(12) 0.0976(9) 0.019(3) Uani 1 1 d U . . C14B C 0.8118(16) 0.0404(15) 0.0515(11) 0.036(4) Uani 1 1 d . . . C15B C 0.8369(17) 0.1115(17) -0.0068(10) 0.037(5) Uani 1 1 d . . . H15B H 0.9049 0.0872 -0.0385 0.045 Uiso 1 1 calc R . . C16B C 0.7639(16) 0.2231(17) -0.0225(11) 0.038(5) Uani 1 1 d . . . H16B H 0.7841 0.2717 -0.0624 0.046 Uiso 1 1 calc R . . C17B C 0.6610(19) 0.2561(15) 0.0246(11) 0.039(5) Uani 1 1 d . . . H17B H 0.6118 0.3285 0.0174 0.047 Uiso 1 1 calc R . . N1 N 0.247(2) 0.6065(14) 0.5255(9) 0.098(8) Uani 1 1 d GU . . H1A H 0.2578 0.5723 0.5721 0.118 Uiso 1 1 calc R . . C1 C 0.1365(17) 0.6430(18) 0.4975(12) 0.123(13) Uani 1 1 d GU . . H1B H 0.0743 0.6305 0.5292 0.148 Uiso 1 1 calc R . . C2 C 0.1191(14) 0.6983(18) 0.4221(13) 0.121(13) Uani 1 1 d GU . . H2B H 0.0452 0.7228 0.4034 0.145 Uiso 1 1 calc R . . C3 C 0.2122(19) 0.7171(15) 0.3748(9) 0.075(8) Uani 1 1 d GU . . H3A H 0.2005 0.7541 0.3244 0.090 Uiso 1 1 calc R . . C4 C 0.3227(15) 0.6806(16) 0.4027(10) 0.081(8) Uani 1 1 d GU . . H4C H 0.3849 0.6932 0.3711 0.097 Uiso 1 1 calc R . . C5 C 0.3401(15) 0.6253(15) 0.4781(11) 0.080(8) Uani 1 1 d GU . . H5C H 0.4140 0.6009 0.4968 0.096 Uiso 1 1 calc R . . N2 N 0.4454(12) 0.4758(11) 0.8700(7) 0.064(6) Uani 1 1 d G . . H2A H 0.4069 0.4608 0.9126 0.077 Uiso 1 1 calc R . . C6 C 0.4031(11) 0.5766(10) 0.8238(9) 0.066(7) Uani 1 1 d GU . . H6 H 0.3333 0.6280 0.8390 0.079 Uiso 1 1 calc R . . C7 C 0.4653(14) 0.6008(10) 0.7550(8) 0.069(7) Uani 1 1 d GU . . H7 H 0.4370 0.6683 0.7240 0.083 Uiso 1 1 calc R . . C8 C 0.5697(13) 0.5241(13) 0.7323(7) 0.065(7) Uani 1 1 d GU . . H8 H 0.6112 0.5403 0.6862 0.078 Uiso 1 1 calc R . . C9 C 0.6119(11) 0.4232(11) 0.7785(9) 0.073(8) Uani 1 1 d G . . H9 H 0.6818 0.3719 0.7633 0.087 Uiso 1 1 calc R . . C10 C 0.5498(12) 0.3991(9) 0.8473(8) 0.044(5) Uani 1 1 d G . . H10 H 0.5781 0.3316 0.8783 0.052 Uiso 1 1 calc R . . N3 N 0.0144(19) 0.6985(16) 0.7394(11) 0.099(8) Uani 1 1 d GU . . C11 C 0.0967(17) 0.6672(12) 0.7948(12) 0.089(9) Uani 1 1 d GU . . H11 H 0.1481 0.5956 0.8015 0.107 Uiso 1 1 calc R . . C12 C 0.1022(16) 0.7429(16) 0.8401(11) 0.094(10) Uani 1 1 d GU . . H12 H 0.1573 0.7219 0.8771 0.112 Uiso 1 1 calc R . . C13 C 0.0253(18) 0.8498(14) 0.8301(11) 0.065(7) Uani 1 1 d GU . . H13 H 0.0290 0.9005 0.8604 0.078 Uiso 1 1 calc R . . C14 C -0.0570(18) 0.8811(13) 0.7747(13) 0.137(15) Uani 1 1 d GU . . H14 H -0.1085 0.9527 0.7680 0.165 Uiso 1 1 calc R . . C15 C -0.0625(18) 0.8054(18) 0.7294(12) 0.104(11) Uani 1 1 d GU . . H15 H -0.1176 0.8264 0.6924 0.124 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 0.0326(4) 0.0291(4) 0.0285(4) -0.0031(3) -0.0035(3) -0.0073(3) U2 0.0329(4) 0.0301(4) 0.0288(4) -0.0030(3) -0.0030(3) -0.0072(3) Cl1 0.042(3) 0.048(3) 0.040(3) -0.005(2) -0.010(2) -0.015(2) Cl2 0.075(4) 0.047(3) 0.047(3) -0.012(2) -0.009(3) -0.031(3) Cl3 0.042(3) 0.038(3) 0.034(3) 0.000(2) 0.000(2) -0.010(2) Cl4 0.040(3) 0.039(3) 0.113(5) -0.013(3) -0.010(3) -0.003(2) O1A 0.025(7) 0.043(7) 0.036(8) 0.009(6) -0.012(6) -0.006(6) O2A 0.020(6) 0.027(6) 0.035(7) 0.004(5) -0.007(5) 0.001(5) O3A 0.030(7) 0.031(6) 0.026(6) 0.005(5) -0.004(5) -0.013(5) O4A 0.043(8) 0.036(7) 0.028(7) -0.008(5) -0.010(6) -0.005(6) N1A 0.038(9) 0.037(9) 0.044(10) 0.001(7) 0.004(8) -0.024(7) N2A 0.043(10) 0.024(8) 0.038(9) -0.007(7) -0.004(7) -0.013(7) C1A 0.007(8) 0.059(13) 0.034(10) -0.014(9) -0.003(7) 0.003(8) C2A 0.027(9) 0.039(10) 0.011(8) 0.004(7) -0.002(7) -0.004(7) C3A 0.039(6) 0.030(6) 0.038(6) -0.004(4) -0.002(4) -0.015(4) C4A 0.023(10) 0.049(13) 0.056(14) -0.027(10) -0.011(9) 0.009(8) C5A 0.045(13) 0.030(11) 0.062(15) -0.010(10) -0.010(11) -0.009(9) C6A 0.030(11) 0.041(12) 0.048(12) -0.020(9) -0.005(9) 0.002(8) C7A 0.028(10) 0.043(11) 0.024(9) -0.008(8) 0.008(7) -0.015(8) C8A 0.033(11) 0.036(10) 0.035(11) -0.001(8) -0.014(9) 0.001(8) C9A 0.036(11) 0.042(12) 0.036(11) -0.016(9) 0.002(9) -0.007(9) C10A 0.035(11) 0.069(15) 0.037(12) -0.020(10) -0.009(9) -0.015(10) C11A 0.057(14) 0.028(10) 0.031(11) -0.004(8) -0.001(9) -0.012(9) C12A 0.020(9) 0.038(11) 0.054(13) -0.009(9) -0.013(9) -0.008(8) C13A 0.028(10) 0.033(10) 0.034(10) 0.005(8) -0.022(8) -0.009(8) C14A 0.033(10) 0.035(10) 0.047(12) -0.001(8) -0.020(9) -0.025(8) C15A 0.040(11) 0.037(10) 0.023(9) 0.008(8) -0.005(8) -0.014(8) C16A 0.041(11) 0.034(10) 0.043(12) -0.001(9) -0.024(10) -0.010(8) C17A 0.048(12) 0.035(10) 0.011(8) 0.009(7) 0.004(8) -0.006(8) O1B 0.035(7) 0.036(7) 0.027(7) -0.003(5) 0.013(5) -0.018(5) O2B 0.033(7) 0.038(7) 0.024(6) -0.007(5) -0.009(5) -0.011(6) O3B 0.032(7) 0.029(6) 0.011(6) 0.009(5) -0.004(5) -0.012(5) O4B 0.039(8) 0.033(7) 0.047(8) 0.002(6) -0.005(6) -0.008(6) N1B 0.058(11) 0.047(10) 0.011(7) -0.012(7) 0.002(7) -0.013(8) N2B 0.061(12) 0.035(9) 0.042(10) 0.000(8) -0.004(9) -0.027(8) C1B 0.040(11) 0.036(11) 0.035(11) 0.000(8) 0.003(8) -0.028(9) C2B 0.044(12) 0.035(11) 0.020(9) 0.000(8) 0.004(8) -0.008(8) C3B 0.031(6) 0.033(6) 0.036(6) -0.004(4) -0.001(4) -0.016(4) C4B 0.044(12) 0.050(13) 0.056(14) -0.028(11) -0.011(10) -0.008(10) C5B 0.061(15) 0.049(14) 0.049(14) 0.002(11) -0.021(12) -0.022(11) C6B 0.031(10) 0.030(10) 0.046(12) 0.021(9) 0.013(9) -0.004(8) C7B 0.064(15) 0.019(10) 0.056(14) -0.004(9) -0.001(11) -0.005(9) C8B 0.046(12) 0.046(12) 0.019(9) -0.003(8) 0.006(8) -0.005(9) C9B 0.043(12) 0.036(11) 0.036(11) -0.003(8) -0.007(9) -0.009(9) C10B 0.050(13) 0.037(12) 0.057(14) -0.007(10) 0.002(11) -0.020(10) C11B 0.051(12) 0.025(9) 0.029(10) 0.000(8) -0.023(9) -0.004(8) C12B 0.027(10) 0.062(13) 0.026(10) -0.016(9) -0.002(8) -0.014(9) C13B 0.017(5) 0.022(5) 0.018(5) -0.002(4) -0.007(4) -0.006(4) C14B 0.033(10) 0.030(10) 0.043(12) -0.003(8) -0.011(9) -0.005(8) C15B 0.032(10) 0.065(14) 0.019(10) -0.012(9) -0.005(8) -0.018(9) C16B 0.032(11) 0.064(14) 0.029(10) -0.015(9) 0.000(8) -0.024(10) C17B 0.068(14) 0.024(10) 0.028(10) -0.008(8) -0.003(9) -0.018(9) N1 0.103(9) 0.096(9) 0.098(9) -0.012(5) -0.007(5) -0.035(5) C1 0.124(14) 0.122(14) 0.125(14) -0.016(5) -0.008(5) -0.042(6) C2 0.122(14) 0.121(14) 0.122(14) -0.018(5) -0.009(5) -0.042(6) C3 0.073(9) 0.078(9) 0.073(9) -0.008(5) -0.010(5) -0.025(5) C4 0.081(9) 0.080(9) 0.081(9) -0.009(5) -0.007(5) -0.025(5) C5 0.081(9) 0.079(9) 0.082(9) -0.014(5) -0.013(5) -0.024(5) N2 0.077(15) 0.082(14) 0.051(12) -0.002(10) 0.009(10) -0.056(12) C6 0.067(8) 0.064(8) 0.067(8) -0.011(5) -0.007(5) -0.019(5) C7 0.069(8) 0.067(8) 0.072(8) -0.008(5) -0.009(5) -0.024(5) C8 0.064(8) 0.069(8) 0.066(8) -0.006(5) -0.009(5) -0.026(5) C9 0.049(15) 0.086(18) 0.060(17) 0.008(14) 0.003(13) -0.001(13) C10 0.045(12) 0.033(11) 0.058(14) -0.014(10) 0.003(10) -0.016(9) N3 0.098(9) 0.100(9) 0.101(9) -0.014(5) -0.006(5) -0.035(5) C11 0.089(10) 0.084(10) 0.089(10) -0.009(5) 0.000(5) -0.025(5) C12 0.091(11) 0.100(11) 0.090(11) -0.009(5) -0.007(5) -0.032(6) C13 0.067(8) 0.065(8) 0.066(8) -0.013(5) -0.003(5) -0.023(5) C14 0.137(16) 0.139(15) 0.136(16) -0.021(5) -0.009(5) -0.045(7) C15 0.103(12) 0.103(12) 0.106(12) -0.014(5) -0.006(5) -0.036(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 U1 O4B 2.237(13) 2_656 ? U1 O2A 2.316(11) . ? U1 O3A 2.352(12) . ? U1 O3B 2.396(11) 2_656 ? U1 O1B 2.397(12) . ? U1 N1A 2.530(16) . ? U1 N2A 2.589(15) . ? U1 Cl1 2.714(5) . ? U1 U2 3.7854(13) . ? U2 O1A 2.251(11) . ? U2 O4A 2.293(12) . ? U2 O2B 2.358(11) . ? U2 O1B 2.444(12) . ? U2 O3A 2.489(11) . ? U2 O2A 2.495(12) . ? U2 Cl2 2.738(5) . ? U2 Cl3 2.808(5) . ? O1A C1A 1.33(2) . ? O2A C2A 1.297(19) . ? O3A C13A 1.31(2) . ? O4A C14A 1.35(2) . ? N1A C7A 1.31(2) . ? N1A C8A 1.46(2) . ? N2A C11A 1.35(3) . ? N2A C10A 1.46(2) . ? C1A C2A 1.41(2) . ? C1A C6A 1.42(2) . ? C2A C3A 1.44(3) . ? C3A C4A 1.40(2) . ? C3A C7A 1.45(2) . ? C4A C5A 1.39(3) . ? C5A C6A 1.38(3) . ? C8A C9A 1.53(3) . ? C9A C10A 1.55(3) . ? C11A C12A 1.44(3) . ? C12A C13A 1.37(2) . ? C12A C17A 1.40(3) . ? C13A C14A 1.42(3) . ? C14A C15A 1.39(2) . ? C15A C16A 1.41(2) . ? C16A C17A 1.38(3) . ? O1B C1B 1.41(2) . ? O2B C2B 1.30(2) . ? O3B C13B 1.288(18) . ? O3B U1 2.396(11) 2_656 ? O4B C14B 1.37(2) . ? O4B U1 2.237(13) 2_656 ? N1B C7B 1.35(3) . ? N1B C8B 1.44(2) . ? N2B C11B 1.32(2) . ? N2B C10B 1.45(3) . ? C1B C6B 1.34(2) . ? C1B C2B 1.38(2) . ? C2B C3B 1.46(2) . ? C3B C7B 1.42(3) . ? C3B C4B 1.43(3) . ? C4B C5B 1.40(3) . ? C5B C6B 1.39(3) . ? C8B C9B 1.48(2) . ? C9B C10B 1.53(3) . ? C11B C12B 1.42(3) . ? C12B C13B 1.41(2) . ? C12B C17B 1.43(3) . ? C13B C14B 1.39(3) . ? C14B C15B 1.34(3) . ? C15B C16B 1.43(3) . ? C16B C17B 1.39(3) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? N2 C6 1.3900 . ? N2 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? N3 C11 1.3900 . ? N3 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 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 O4B U1 O2A 157.4(4) 2_656 . ? O4B U1 O3A 134.1(4) 2_656 . ? O2A U1 O3A 64.1(4) . . ? O4B U1 O3B 67.7(4) 2_656 2_656 ? O2A U1 O3B 134.8(4) . 2_656 ? O3A U1 O3B 78.3(4) . 2_656 ? O4B U1 O1B 126.3(4) 2_656 . ? O2A U1 O1B 69.5(4) . . ? O3A U1 O1B 66.9(4) . . ? O3B U1 O1B 73.5(4) 2_656 . ? O4B U1 N1A 88.5(5) 2_656 . ? O2A U1 N1A 70.6(5) . . ? O3A U1 N1A 109.8(4) . . ? O3B U1 N1A 150.3(4) 2_656 . ? O1B U1 N1A 136.2(5) . . ? O4B U1 N2A 74.5(5) 2_656 . ? O2A U1 N2A 107.3(4) . . ? O3A U1 N2A 70.0(5) . . ? O3B U1 N2A 80.2(4) 2_656 . ? O1B U1 N2A 133.0(5) . . ? N1A U1 N2A 76.3(5) . . ? O4B U1 Cl1 81.6(4) 2_656 . ? O2A U1 Cl1 86.9(3) . . ? O3A U1 Cl1 140.9(3) . . ? O3B U1 Cl1 110.6(3) 2_656 . ? O1B U1 Cl1 79.0(3) . . ? N1A U1 Cl1 81.6(4) . . ? N2A U1 Cl1 147.6(4) . . ? O1A U2 O4A 165.5(5) . . ? O1A U2 O2B 94.6(4) . . ? O4A U2 O2B 86.6(4) . . ? O1A U2 O1B 97.9(4) . . ? O4A U2 O1B 95.7(4) . . ? O2B U2 O1B 65.9(4) . . ? O1A U2 O3A 125.0(4) . . ? O4A U2 O3A 65.9(4) . . ? O2B U2 O3A 118.7(4) . . ? O1B U2 O3A 64.2(4) . . ? O1A U2 O2A 65.6(4) . . ? O4A U2 O2A 125.2(4) . . ? O2B U2 O2A 123.8(4) . . ? O1B U2 O2A 65.9(4) . . ? O3A U2 O2A 59.6(4) . . ? O1A U2 Cl2 86.9(4) . . ? O4A U2 Cl2 86.0(3) . . ? O2B U2 Cl2 154.9(3) . . ? O1B U2 Cl2 138.8(3) . . ? O3A U2 Cl2 79.5(3) . . ? O2A U2 Cl2 79.5(3) . . ? O1A U2 Cl3 83.8(4) . . ? O4A U2 Cl3 82.9(3) . . ? O2B U2 Cl3 71.7(3) . . ? O1B U2 Cl3 137.5(3) . . ? O3A U2 Cl3 145.2(3) . . ? O2A U2 Cl3 145.6(3) . . ? Cl2 U2 Cl3 83.65(16) . . ? C1A O1A U2 124.0(11) . . ? C2A O2A U1 130.4(11) . . ? C2A O2A U2 116.5(10) . . ? U1 O2A U2 103.7(4) . . ? C13A O3A U1 129.8(11) . . ? C13A O3A U2 118.3(11) . . ? U1 O3A U2 102.9(4) . . ? C14A O4A U2 122.5(12) . . ? C7A N1A C8A 114.5(15) . . ? C7A N1A U1 127.7(13) . . ? C8A N1A U1 116.4(11) . . ? C11A N2A C10A 115.5(15) . . ? C11A N2A U1 123.8(12) . . ? C10A N2A U1 119.2(11) . . ? O1A C1A C2A 116.6(14) . . ? O1A C1A C6A 123.8(17) . . ? C2A C1A C6A 119.5(16) . . ? O2A C2A C1A 116.4(15) . . ? O2A C2A C3A 122.7(14) . . ? C1A C2A C3A 120.8(15) . . ? C4A C3A C2A 117.5(17) . . ? C4A C3A C7A 119.2(18) . . ? C2A C3A C7A 123.2(16) . . ? C5A C4A C3A 120.8(18) . . ? C6A C5A C4A 122.6(19) . . ? C5A C6A C1A 118.7(19) . . ? N1A C7A C3A 124.9(17) . . ? N1A C8A C9A 111.4(17) . . ? C8A C9A C10A 113.4(15) . . ? N2A C10A C9A 111.0(16) . . ? N2A C11A C12A 127.1(17) . . ? C13A C12A C17A 118.0(18) . . ? C13A C12A C11A 124.1(17) . . ? C17A C12A C11A 117.8(17) . . ? O3A C13A C12A 123.1(18) . . ? O3A C13A C14A 115.2(15) . . ? C12A C13A C14A 121.3(16) . . ? O4A C14A C15A 123.8(18) . . ? O4A C14A C13A 117.6(15) . . ? C15A C14A C13A 118.6(16) . . ? C14A C15A C16A 121.1(19) . . ? C17A C16A C15A 117.6(18) . . ? C16A C17A C12A 123.2(17) . . ? C1B O1B U1 138.5(10) . . ? C1B O1B U2 118.1(10) . . ? U1 O1B U2 102.9(4) . . ? C2B O2B U2 121.1(10) . . ? C13B O3B U1 116.7(10) . 2_656 ? C14B O4B U1 121.8(12) . 2_656 ? C7B N1B C8B 120.9(16) . . ? C11B N2B C10B 125.7(17) . . ? C6B C1B C2B 123.7(18) . . ? C6B C1B O1B 123.0(17) . . ? C2B C1B O1B 113.1(15) . . ? O2B C2B C1B 121.1(16) . . ? O2B C2B C3B 120.9(16) . . ? C1B C2B C3B 118.0(17) . . ? C7B C3B C4B 119.8(17) . . ? C7B C3B C2B 122.1(17) . . ? C4B C3B C2B 118.1(17) . . ? C5B C4B C3B 119.2(18) . . ? C4B C5B C6B 121(2) . . ? C1B C6B C5B 120.0(19) . . ? N1B C7B C3B 120.5(18) . . ? N1B C8B C9B 112.7(16) . . ? C8B C9B C10B 113.7(16) . . ? N2B C10B C9B 114.4(18) . . ? N2B C11B C12B 121.8(18) . . ? C13B C12B C11B 122.9(18) . . ? C13B C12B C17B 120.2(17) . . ? C11B C12B C17B 116.7(18) . . ? O3B C13B C14B 119.0(14) . . ? O3B C13B C12B 122.3(15) . . ? C14B C13B C12B 118.5(16) . . ? C15B C14B O4B 124.4(19) . . ? C15B C14B C13B 121.2(17) . . ? O4B C14B C13B 114.2(17) . . ? C14B C15B C16B 122.9(19) . . ? C17B C16B C15B 117.1(19) . . ? C16B C17B C12B 119.9(18) . . ? C1 N1 C5 120.0 . . ? C2 C1 N1 120.0 . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C4 C5 N1 120.0 . . ? C6 N2 C10 120.0 . . ? N2 C6 C7 120.0 . . ? C6 C7 C8 120.0 . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C9 C10 N2 120.0 . . ? C11 N3 C15 120.0 . . ? N3 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 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 N1 H1A Cl2 0.86 2.22 3.054(16) 164.5 . N2 H2A Cl4 0.86 2.22 3.063(13) 164.8 . #===END data_6b.6py _database_code_depnum_ccdc_archive 'CCDC 250668' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H100 Cl4 N16 O16 U4' _chemical_formula_weight 2971.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.3462(8) _cell_length_b 21.4191(13) _cell_length_c 16.8848(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.245(3) _cell_angle_gamma 90.00 _cell_volume 5137.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 35118 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method ? _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 6.465 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.195 _exptl_absorpt_correction_T_max 0.524 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 35118 _diffrn_reflns_av_R_equivalents 0.1023 _diffrn_reflns_av_sigmaI/netI 0.1018 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9710 _reflns_number_gt 5588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. Two C atoms of the diimino bridge of the Schiff base B molecule are disordered over two sites which have been refined with occupancy parameters constrained to sum to unity and some restraints on bond lengths and displacement parameters. One pyridine solvent molecule is disordered over two positions (sharing two C atoms) which have been refined with an occupancy parameter fixed to 0.5. Two solvent pyridine molecules were refined as idealized hexagons. Some restraints on displacement parameters were applied for all solvent molecules. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms bound to O atoms were not found. All the other protons were introduced at calculated positions, except in the disordered parts, and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. Some short contacts involving pyridine hydrogen atoms likely indicate an imperfect location of these rather badly resolved 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^)+(0.0672P)^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 9710 _refine_ls_number_parameters 699 _refine_ls_number_restraints 175 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.199 _refine_diff_density_min -2.029 _refine_diff_density_rms 0.186 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 0.21678(3) 0.38668(2) 0.90293(2) 0.03175(13) Uani 1 1 d . . . U2 U -0.01482(3) 0.38782(2) 0.71384(3) 0.03456(14) Uani 1 1 d . . . Cl1 Cl 0.3199(2) 0.31471(14) 0.83927(19) 0.0431(7) Uani 1 1 d . . . Cl2 Cl -0.1867(2) 0.39561(15) 0.5853(2) 0.0497(8) Uani 1 1 d . . . O1A O -0.0120(5) 0.2865(4) 0.6778(5) 0.041(2) Uani 1 1 d . . . O2A O 0.0892(5) 0.3208(3) 0.8298(4) 0.0339(18) Uani 1 1 d . . . O3A O 0.0628(5) 0.4272(3) 0.8604(5) 0.0318(17) Uani 1 1 d . . . O4A O -0.0522(5) 0.4885(3) 0.7292(4) 0.0352(19) Uani 1 1 d . . . N1A N 0.2275(6) 0.2899(4) 0.9917(6) 0.033(2) Uani 1 1 d . . . N2A N 0.1883(6) 0.4302(4) 1.0331(6) 0.032(2) Uani 1 1 d . . . C1A C 0.0387(8) 0.2416(5) 0.7279(7) 0.032(3) Uani 1 1 d . . . C2A C 0.0924(7) 0.2594(5) 0.8130(7) 0.034(3) Uani 1 1 d . . . C3A C 0.1482(8) 0.2161(6) 0.8742(8) 0.043(3) Uani 1 1 d . . . C4A C 0.1471(8) 0.1535(6) 0.8464(8) 0.045(3) Uani 1 1 d . . . H4A H 0.1831 0.1237 0.8850 0.054 Uiso 1 1 calc R . . C5A C 0.0952(9) 0.1365(6) 0.7659(9) 0.050(3) Uani 1 1 d . . . H5A H 0.0944 0.0947 0.7505 0.061 Uiso 1 1 calc R . . C6A C 0.0415(8) 0.1804(6) 0.7036(7) 0.044(3) Uani 1 1 d . . . H6A H 0.0088 0.1682 0.6472 0.052 Uiso 1 1 calc R . . C7A C 0.2030(8) 0.2341(6) 0.9635(7) 0.040(3) Uani 1 1 d . . . H7A H 0.2219 0.2021 1.0035 0.048 Uiso 1 1 calc R . . C8A C 0.2824(8) 0.2942(5) 1.0826(7) 0.037(3) Uani 1 1 d . . . H8A1 H 0.3441 0.3109 1.0914 0.045 Uiso 1 1 calc R . . H8A2 H 0.2910 0.2526 1.1073 0.045 Uiso 1 1 calc R . . C9A C 0.2349(9) 0.3363(6) 1.1296(7) 0.043(3) Uani 1 1 d . . . H9A1 H 0.1684 0.3261 1.1087 0.051 Uiso 1 1 calc R . . H9A2 H 0.2617 0.3263 1.1901 0.051 Uiso 1 1 calc R . . C10A C 0.2444(8) 0.4062(5) 1.1197(7) 0.037(3) Uani 1 1 d . . . H10A H 0.2250 0.4278 1.1609 0.044 Uiso 1 1 calc R . . H10B H 0.3102 0.4160 1.1332 0.044 Uiso 1 1 calc R . . C11A C 0.1405(8) 0.4791(6) 1.0324(7) 0.041(3) Uani 1 1 d . . . H11A H 0.1430 0.4938 1.0850 0.049 Uiso 1 1 calc R . . C12A C 0.0822(7) 0.5144(5) 0.9566(7) 0.029(2) Uani 1 1 d . . . C13A C 0.0440(7) 0.4870(5) 0.8748(7) 0.031(3) Uani 1 1 d . . . C14A C -0.0171(8) 0.5197(6) 0.8043(7) 0.035(3) Uani 1 1 d . . . C15A C -0.0390(8) 0.5819(5) 0.8135(7) 0.035(3) Uani 1 1 d . . . H15A H -0.0791 0.6040 0.7664 0.042 Uiso 1 1 calc R . . C16A C -0.0002(8) 0.6114(6) 0.8944(7) 0.038(3) Uani 1 1 d . . . H16A H -0.0129 0.6532 0.9008 0.045 Uiso 1 1 calc R . . C17A C 0.0575(8) 0.5767(6) 0.9644(7) 0.036(3) Uani 1 1 d . . . H17A H 0.0806 0.5954 1.0181 0.043 Uiso 1 1 calc R . . O1B O 0.1485(5) 0.4140(4) 0.7533(4) 0.0360(19) Uani 1 1 d . . . O2B O 0.0248(6) 0.4172(4) 0.5967(5) 0.042(2) Uani 1 1 d . . . O3B O -0.2530(5) 0.5066(3) 0.1098(4) 0.0348(18) Uani 1 1 d . . . O4B O -0.3539(5) 0.5866(4) -0.0027(5) 0.0335(18) Uani 1 1 d . . . N1B N -0.0127(8) 0.4262(5) 0.4312(6) 0.046(3) Uani 1 1 d . . . N2B N -0.2268(8) 0.3898(5) 0.1717(6) 0.053(3) Uani 1 1 d D . . C1B C 0.1781(8) 0.4358(6) 0.6923(7) 0.036(3) Uani 1 1 d . . . C2B C 0.1116(8) 0.4356(5) 0.6096(7) 0.036(3) Uani 1 1 d . . . C3B C 0.1379(9) 0.4559(6) 0.5417(7) 0.044(3) Uani 1 1 d . . . C4B C 0.2298(9) 0.4768(6) 0.5598(8) 0.047(3) Uani 1 1 d . . . H4B H 0.2466 0.4901 0.5151 0.056 Uiso 1 1 calc R . . C5B C 0.2953(9) 0.4780(6) 0.6410(7) 0.042(3) Uani 1 1 d . . . H5B H 0.3556 0.4931 0.6523 0.050 Uiso 1 1 calc R . . C6B C 0.2695(9) 0.4560(5) 0.7075(7) 0.040(3) Uani 1 1 d . . . H6B H 0.3145 0.4549 0.7630 0.048 Uiso 1 1 calc R . . C7B C 0.0729(10) 0.4486(6) 0.4553(7) 0.051(4) Uani 1 1 d . . . H7B H 0.0932 0.4608 0.4123 0.061 Uiso 1 1 calc R . . C8B C -0.0684(10) 0.4158(6) 0.3371(8) 0.058(4) Uani 1 1 d D . . C9B C -0.1515(14) 0.3760(12) 0.3317(13) 0.047(6) Uani 0.57(2) 1 d PDU . . C9C C -0.123(2) 0.3545(11) 0.3154(16) 0.045(6) Uani 0.43(2) 1 d PDU . . C10B C -0.1885(17) 0.3449(9) 0.2438(10) 0.044(5) Uani 0.57(2) 1 d PDU . . C10C C -0.1553(18) 0.3427(11) 0.2198(15) 0.045(6) Uani 0.43(2) 1 d PDU . . C11B C -0.3010(9) 0.3779(6) 0.1037(7) 0.046(3) Uani 1 1 d . . . H11B H -0.3239 0.3372 0.0979 0.055 Uiso 1 1 calc R . . C12B C -0.3504(7) 0.4202(6) 0.0377(6) 0.034(3) Uani 1 1 d . . . C13B C -0.3260(7) 0.4839(5) 0.0468(7) 0.029(3) Uani 1 1 d . . . C14B C -0.3812(7) 0.5257(5) -0.0169(7) 0.030(2) Uani 1 1 d . . . C15B C -0.4567(8) 0.5042(6) -0.0873(7) 0.043(3) Uani 1 1 d . . . H15B H -0.4911 0.5321 -0.1298 0.052 Uiso 1 1 calc R . . C16B C -0.4818(9) 0.4401(6) -0.0949(8) 0.047(3) Uani 1 1 d . . . H16B H -0.5329 0.4260 -0.1419 0.057 Uiso 1 1 calc R . . C17B C -0.4299(9) 0.3992(5) -0.0324(7) 0.042(3) Uani 1 1 d . . . H17B H -0.4471 0.3574 -0.0362 0.050 Uiso 1 1 calc R . . N1 N -0.1286(7) 0.3600(5) 0.7913(6) 0.045(3) Uani 1 1 d . . . C1 C -0.1187(11) 0.3078(7) 0.8361(9) 0.064(4) Uani 1 1 d U . . H1 H -0.0706 0.2804 0.8390 0.077 Uiso 1 1 calc R . . C2 C -0.1784(13) 0.2921(9) 0.8795(11) 0.084(5) Uani 1 1 d U . . H2 H -0.1700 0.2551 0.9103 0.101 Uiso 1 1 calc R . . C3 C -0.2484(11) 0.3326(8) 0.8751(10) 0.069(4) Uani 1 1 d U . . H3 H -0.2883 0.3243 0.9038 0.083 Uiso 1 1 calc R . . C4 C -0.2592(9) 0.3871(7) 0.8265(10) 0.062(4) Uani 1 1 d . . . H4 H -0.3074 0.4150 0.8214 0.074 Uiso 1 1 calc R . . C5 C -0.1982(9) 0.3988(7) 0.7867(9) 0.055(4) Uani 1 1 d . . . H5 H -0.2056 0.4353 0.7550 0.066 Uiso 1 1 calc R . . N2 N 0.0696(14) 0.2786(10) 0.5217(14) 0.137(7) Uani 1 1 d U . . C6 C 0.0805(15) 0.2800(9) 0.4481(14) 0.103(6) Uani 1 1 d U . . H6 H 0.0286 0.2686 0.3999 0.124 Uiso 1 1 calc R . . C7 C 0.1571(16) 0.2958(10) 0.4355(14) 0.113(7) Uani 1 1 d U . . H7 H 0.1590 0.2976 0.3812 0.136 Uiso 1 1 calc R . . C8 C 0.2381(19) 0.3103(12) 0.5118(16) 0.143(9) Uani 1 1 d U . . H8 H 0.2926 0.3245 0.5059 0.172 Uiso 1 1 calc R . . C9 C 0.2379(15) 0.3040(9) 0.5929(13) 0.093(6) Uani 1 1 d U . . H9 H 0.2915 0.3077 0.6427 0.111 Uiso 1 1 calc R . . C10 C 0.1497(15) 0.2916(9) 0.5920(14) 0.105(7) Uani 1 1 d U . . H10 H 0.1434 0.2921 0.6447 0.127 Uiso 1 1 calc R . . N3 N 0.0714(10) 0.2380(6) 0.2181(10) 0.151(8) Uani 1 1 d GU . . C11 C 0.0947(10) 0.2185(8) 0.1501(11) 0.128(8) Uani 1 1 d GU . . H11 H 0.1382 0.2411 0.1354 0.153 Uiso 1 1 calc R . . C12 C 0.0530(13) 0.1654(8) 0.1040(9) 0.144(9) Uani 1 1 d GU . . H12 H 0.0686 0.1524 0.0585 0.173 Uiso 1 1 calc R . . C13 C -0.0120(13) 0.1318(6) 0.1259(11) 0.194(14) Uani 1 1 d GU . . H13 H -0.0399 0.0962 0.0951 0.233 Uiso 1 1 calc R . . C14 C -0.0353(10) 0.1512(8) 0.1940(12) 0.152(10) Uani 1 1 d GU . . H14 H -0.0788 0.1287 0.2086 0.182 Uiso 1 1 calc R . . C15 C 0.0063(11) 0.2043(8) 0.2401(8) 0.111(7) Uani 1 1 d GU . . H15 H -0.0093 0.2173 0.2856 0.133 Uiso 1 1 calc R . . C16 C 0.7005(9) 0.5438(7) 0.6354(9) 0.072(5) Uani 1 1 d GU . . C17 C 0.6330(13) 0.4998(6) 0.5915(11) 0.074(9) Uani 0.50 1 d PGU . . C18 C 0.5379(11) 0.5136(8) 0.5674(14) 0.122(15) Uani 0.50 1 d PGU . . C19 C 0.5104(8) 0.5714(9) 0.5873(12) 0.090(11) Uani 0.50 1 d PGU . . C20 C 0.5780(11) 0.6154(6) 0.6312(10) 0.079(5) Uani 1 1 d GU . . C21 C 0.6730(9) 0.6016(6) 0.6553(10) 0.058(8) Uani 0.50 1 d PGU . . C22 C 0.639(2) 0.5134(16) 0.657(2) 0.073(9) Uani 0.50 1 d PU . . C23 C 0.566(3) 0.5569(18) 0.663(2) 0.086(11) Uani 0.50 1 d PU . . C24 C 0.651(2) 0.6372(13) 0.6284(17) 0.051(7) Uani 0.50 1 d PU . . C25 C 0.714(3) 0.6003(18) 0.629(2) 0.086(11) Uani 0.50 1 d PU . . 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 0.0291(2) 0.0321(3) 0.0317(2) -0.0033(2) 0.00896(18) 0.0001(2) U2 0.0323(3) 0.0330(3) 0.0329(2) -0.0043(2) 0.00609(18) 0.0023(2) Cl1 0.0427(17) 0.0406(18) 0.0491(17) -0.0111(14) 0.0210(14) -0.0014(14) Cl2 0.0448(17) 0.0432(19) 0.0456(17) -0.0082(15) -0.0004(14) 0.0022(15) O1A 0.033(5) 0.028(4) 0.051(5) -0.001(4) 0.005(4) 0.010(4) O2A 0.035(4) 0.029(4) 0.036(4) -0.001(3) 0.012(3) 0.006(3) O3A 0.028(4) 0.028(4) 0.040(4) -0.003(3) 0.014(3) 0.000(3) O4A 0.039(5) 0.032(5) 0.031(4) 0.000(3) 0.010(4) 0.005(4) N1A 0.027(5) 0.025(5) 0.045(6) -0.007(4) 0.013(4) -0.004(4) N2A 0.029(5) 0.028(5) 0.038(5) 0.004(4) 0.013(4) 0.009(4) C1A 0.031(6) 0.030(6) 0.034(6) -0.014(5) 0.012(5) -0.005(5) C2A 0.018(6) 0.033(6) 0.043(6) 0.000(6) 0.004(5) 0.007(5) C3A 0.032(7) 0.039(7) 0.062(8) -0.001(6) 0.022(6) -0.003(6) C4A 0.031(7) 0.047(8) 0.045(7) -0.003(6) 0.000(6) 0.005(6) C5A 0.040(8) 0.036(7) 0.067(9) 0.001(7) 0.011(7) 0.006(6) C6A 0.034(7) 0.053(8) 0.038(7) -0.018(6) 0.008(5) -0.001(6) C7A 0.029(6) 0.044(8) 0.044(7) 0.009(6) 0.012(5) 0.004(6) C8A 0.035(7) 0.025(6) 0.046(7) -0.003(5) 0.009(5) 0.004(5) C9A 0.055(8) 0.033(7) 0.041(7) 0.001(6) 0.018(6) 0.004(6) C10A 0.043(7) 0.039(7) 0.025(6) 0.000(5) 0.009(5) 0.007(5) C11A 0.033(7) 0.059(9) 0.027(6) -0.005(6) 0.007(5) -0.002(6) C12A 0.031(6) 0.024(6) 0.036(6) 0.000(5) 0.016(5) -0.007(5) C13A 0.023(6) 0.026(6) 0.049(7) 0.004(5) 0.018(5) -0.002(5) C14A 0.041(7) 0.040(7) 0.031(6) 0.005(5) 0.020(5) 0.010(6) C15A 0.043(7) 0.030(6) 0.042(7) 0.003(5) 0.027(6) 0.002(5) C16A 0.032(6) 0.037(7) 0.046(7) -0.013(6) 0.018(5) 0.000(6) C17A 0.032(6) 0.051(8) 0.025(6) -0.008(5) 0.011(5) 0.001(6) O1B 0.034(4) 0.048(5) 0.028(4) 0.000(4) 0.014(3) -0.001(4) O2B 0.035(5) 0.052(5) 0.033(4) 0.003(4) 0.007(4) 0.005(4) O3B 0.034(4) 0.033(5) 0.033(4) -0.002(3) 0.008(3) 0.000(4) O4B 0.025(4) 0.032(4) 0.039(4) -0.006(4) 0.008(3) 0.005(3) N1B 0.058(7) 0.041(6) 0.032(5) -0.003(5) 0.008(5) 0.007(6) N2B 0.062(7) 0.046(7) 0.035(5) 0.001(5) 0.002(5) -0.012(6) C1B 0.040(7) 0.038(7) 0.037(6) -0.004(5) 0.021(5) 0.003(6) C2B 0.042(7) 0.030(6) 0.031(6) -0.003(5) 0.009(5) 0.013(6) C3B 0.055(9) 0.048(8) 0.035(7) 0.011(6) 0.022(6) 0.012(7) C4B 0.058(9) 0.044(8) 0.035(7) 0.004(6) 0.015(6) 0.002(7) C5B 0.042(7) 0.045(8) 0.039(7) -0.001(6) 0.015(6) 0.007(6) C6B 0.051(8) 0.031(7) 0.035(6) 0.001(5) 0.012(6) 0.007(6) C7B 0.069(10) 0.049(8) 0.031(7) 0.004(6) 0.015(7) 0.019(7) C8B 0.082(11) 0.049(8) 0.030(7) -0.001(6) 0.006(7) -0.002(8) C9B 0.046(12) 0.075(13) 0.022(9) 0.002(9) 0.017(8) -0.008(10) C9C 0.046(12) 0.073(12) 0.020(9) 0.010(9) 0.016(8) -0.016(10) C10B 0.053(12) 0.061(10) 0.016(9) 0.005(8) 0.012(7) -0.026(9) C10C 0.059(14) 0.053(11) 0.017(11) -0.002(10) 0.008(9) -0.036(11) C11B 0.064(9) 0.036(8) 0.041(7) -0.002(6) 0.024(7) -0.011(7) C12B 0.026(6) 0.046(7) 0.025(6) -0.002(5) 0.005(5) 0.005(5) C13B 0.019(6) 0.038(7) 0.036(6) -0.009(5) 0.016(5) -0.005(5) C14B 0.028(6) 0.026(6) 0.042(6) 0.000(5) 0.022(5) 0.005(5) C15B 0.039(7) 0.046(8) 0.037(6) 0.005(6) 0.007(5) 0.003(6) C16B 0.050(8) 0.043(8) 0.039(7) -0.008(6) 0.006(6) -0.005(6) C17B 0.052(8) 0.029(7) 0.043(7) -0.009(5) 0.018(6) 0.011(6) N1 0.034(6) 0.057(7) 0.036(5) -0.009(5) 0.005(4) -0.003(5) C1 0.064(5) 0.064(5) 0.068(5) 0.000(3) 0.028(3) -0.002(3) C2 0.084(6) 0.083(6) 0.086(6) 0.002(3) 0.033(3) -0.002(3) C3 0.067(5) 0.070(5) 0.072(5) -0.001(3) 0.028(3) -0.003(3) C4 0.038(7) 0.071(10) 0.081(10) -0.002(9) 0.027(7) 0.016(8) C5 0.049(8) 0.061(10) 0.058(9) -0.004(7) 0.022(7) -0.002(7) N2 0.138(7) 0.133(8) 0.137(7) 0.000(3) 0.050(4) 0.001(3) C6 0.103(7) 0.100(7) 0.104(7) -0.004(3) 0.037(4) 0.002(3) C7 0.114(8) 0.114(8) 0.114(8) -0.005(3) 0.046(4) 0.004(3) C8 0.143(10) 0.143(10) 0.143(10) 0.000(3) 0.055(4) 0.001(3) C9 0.093(6) 0.093(6) 0.095(6) -0.002(3) 0.038(4) 0.001(3) C10 0.105(7) 0.104(7) 0.108(7) -0.002(3) 0.040(4) 0.001(3) N3 0.152(8) 0.148(8) 0.151(8) 0.001(3) 0.056(4) 0.000(3) C11 0.128(9) 0.128(9) 0.129(9) 0.002(3) 0.051(4) -0.004(3) C12 0.144(9) 0.145(10) 0.145(9) -0.002(3) 0.057(4) -0.001(3) C13 0.194(14) 0.194(14) 0.194(14) 0.000(3) 0.074(6) -0.001(3) C14 0.152(10) 0.153(10) 0.151(10) 0.002(3) 0.058(5) -0.001(3) C15 0.111(7) 0.113(8) 0.111(7) 0.001(3) 0.044(4) 0.002(3) C16 0.073(5) 0.074(5) 0.071(5) -0.002(3) 0.029(3) 0.001(3) C17 0.074(10) 0.073(10) 0.074(10) 0.000(3) 0.028(4) 0.001(3) C18 0.121(15) 0.121(15) 0.122(15) 0.000(3) 0.046(6) 0.000(3) C19 0.090(11) 0.090(11) 0.090(11) 0.000(3) 0.035(5) 0.000(3) C20 0.080(5) 0.079(6) 0.080(5) 0.003(3) 0.030(3) -0.002(3) C21 0.059(8) 0.058(8) 0.058(8) 0.001(3) 0.023(4) 0.000(3) C22 0.072(10) 0.072(10) 0.074(9) 0.000(3) 0.027(4) 0.000(3) C23 0.086(11) 0.086(11) 0.086(11) 0.000(3) 0.033(5) 0.000(3) C24 0.049(7) 0.051(7) 0.052(7) 0.001(3) 0.018(4) 0.001(3) C25 0.086(11) 0.086(11) 0.086(11) 0.000(3) 0.034(5) 0.000(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 O4B 2.215(7) 3_566 ? U1 O2A 2.350(7) . ? U1 O3A 2.360(7) . ? U1 O3B 2.382(8) 3_566 ? U1 O1B 2.412(7) . ? U1 N1A 2.526(9) . ? U1 N2A 2.573(9) . ? U1 Cl1 2.706(3) . ? U1 U2 3.7730(6) . ? U2 O1A 2.259(7) . ? U2 O4A 2.271(7) . ? U2 O2B 2.364(8) . ? U2 O1B 2.403(7) . ? U2 O3A 2.454(7) . ? U2 O2A 2.465(7) . ? U2 N1 2.617(11) . ? U2 Cl2 2.713(3) . ? O1A C1A 1.322(13) . ? O2A C2A 1.350(13) . ? O3A C13A 1.354(13) . ? O4A C14A 1.352(13) . ? N1A C7A 1.288(14) . ? N1A C8A 1.448(13) . ? N2A C11A 1.277(14) . ? N2A C10A 1.479(13) . ? C1A C6A 1.379(16) . ? C1A C2A 1.412(14) . ? C2A C3A 1.411(16) . ? C3A C4A 1.416(17) . ? C3A C7A 1.474(16) . ? C4A C5A 1.340(17) . ? C5A C6A 1.421(17) . ? C8A C9A 1.554(16) . ? C9A C10A 1.519(16) . ? C11A C12A 1.463(15) . ? C12A C17A 1.408(15) . ? C12A C13A 1.408(14) . ? C13A C14A 1.393(15) . ? C14A C15A 1.397(16) . ? C15A C16A 1.416(15) . ? C16A C17A 1.393(16) . ? O1B C1B 1.357(13) . ? O2B C2B 1.325(14) . ? O3B C13B 1.311(12) . ? O3B U1 2.382(8) 3_566 ? O4B C14B 1.363(13) . ? O4B U1 2.215(7) 3_566 ? N1B C7B 1.311(16) . ? N1B C8B 1.509(15) . ? N2B C11B 1.300(15) . ? N2B C10C 1.485(10) . ? N2B C10B 1.487(10) . ? C1B C2B 1.383(15) . ? C1B C6B 1.396(16) . ? C2B C3B 1.421(16) . ? C3B C4B 1.398(17) . ? C3B C7B 1.430(17) . ? C4B C5B 1.359(16) . ? C5B C6B 1.406(16) . ? C8B C9B 1.507(10) . ? C8B C9C 1.526(10) . ? C9B C10B 1.527(10) . ? C9C C10C 1.521(10) . ? C11B C12B 1.414(16) . ? C12B C13B 1.409(16) . ? C12B C17B 1.413(15) . ? C13B C14B 1.409(15) . ? C14B C15B 1.387(15) . ? C15B C16B 1.419(17) . ? C16B C17B 1.371(16) . ? N1 C1 1.326(17) . ? N1 C5 1.331(16) . ? C1 C2 1.41(2) . ? C2 C3 1.36(2) . ? C3 C4 1.40(2) . ? C4 C5 1.367(18) . ? N2 C6 1.32(2) . ? N2 C10 1.38(2) . ? C6 C7 1.31(3) . ? C7 C8 1.45(3) . ? C8 C9 1.38(3) . ? C9 C10 1.37(2) . ? N3 C11 1.3900 . ? N3 C15 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C16 C25 1.24(4) . ? C16 C22 1.30(3) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C22 C23 1.50(5) . ? C24 C25 1.25(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 O4B U1 O2A 156.5(3) 3_566 . ? O4B U1 O3A 133.6(3) 3_566 . ? O2A U1 O3A 61.4(2) . . ? O4B U1 O3B 68.5(3) 3_566 3_566 ? O2A U1 O3B 134.9(2) . 3_566 ? O3A U1 O3B 82.0(3) . 3_566 ? O4B U1 O1B 130.1(3) 3_566 . ? O2A U1 O1B 69.5(3) . . ? O3A U1 O1B 66.7(2) . . ? O3B U1 O1B 72.3(3) 3_566 . ? O4B U1 N1A 86.0(3) 3_566 . ? O2A U1 N1A 70.9(3) . . ? O3A U1 N1A 108.4(3) . . ? O3B U1 N1A 151.2(3) 3_566 . ? O1B U1 N1A 136.5(3) . . ? O4B U1 N2A 71.1(3) 3_566 . ? O2A U1 N2A 106.8(3) . . ? O3A U1 N2A 69.7(3) . . ? O3B U1 N2A 81.4(3) 3_566 . ? O1B U1 N2A 131.3(3) . . ? N1A U1 N2A 77.5(3) . . ? O4B U1 Cl1 85.4(2) 3_566 . ? O2A U1 Cl1 86.88(19) . . ? O3A U1 Cl1 139.23(18) . . ? O3B U1 Cl1 108.6(2) 3_566 . ? O1B U1 Cl1 79.02(19) . . ? N1A U1 Cl1 81.5(2) . . ? N2A U1 Cl1 149.3(2) . . ? O4B U1 U2 163.9(2) 3_566 . ? O2A U1 U2 39.51(17) . . ? O3A U1 U2 39.29(17) . . ? O3B U1 U2 95.43(17) 3_566 . ? O1B U1 U2 38.34(18) . . ? N1A U1 U2 109.6(2) . . ? N2A U1 U2 108.09(19) . . ? Cl1 U1 U2 99.94(7) . . ? O1A U2 O4A 167.0(3) . . ? O1A U2 O2B 89.6(3) . . ? O4A U2 O2B 89.9(3) . . ? O1A U2 O1B 100.0(3) . . ? O4A U2 O1B 91.6(3) . . ? O2B U2 O1B 66.3(3) . . ? O1A U2 O3A 123.4(3) . . ? O4A U2 O3A 66.8(2) . . ? O2B U2 O3A 124.9(3) . . ? O1B U2 O3A 65.4(2) . . ? O1A U2 O2A 65.3(3) . . ? O4A U2 O2A 125.3(2) . . ? O2B U2 O2A 121.7(3) . . ? O1B U2 O2A 67.8(3) . . ? O3A U2 O2A 58.6(2) . . ? O1A U2 N1 90.0(3) . . ? O4A U2 N1 85.1(3) . . ? O2B U2 N1 155.6(3) . . ? O1B U2 N1 137.5(3) . . ? O3A U2 N1 74.6(3) . . ? O2A U2 N1 79.9(3) . . ? O1A U2 Cl2 87.5(2) . . ? O4A U2 Cl2 79.74(19) . . ? O2B U2 Cl2 78.2(2) . . ? O1B U2 Cl2 143.47(19) . . ? O3A U2 Cl2 137.65(18) . . ? O2A U2 Cl2 144.31(19) . . ? N1 U2 Cl2 77.5(2) . . ? C1A O1A U2 126.4(6) . . ? C2A O2A U1 127.3(6) . . ? C2A O2A U2 117.7(6) . . ? U1 O2A U2 103.2(3) . . ? C13A O3A U1 123.3(6) . . ? C13A O3A U2 116.8(6) . . ? U1 O3A U2 103.2(3) . . ? C14A O4A U2 123.3(6) . . ? C7A N1A C8A 114.9(10) . . ? C7A N1A U1 126.7(8) . . ? C8A N1A U1 117.3(7) . . ? C11A N2A C10A 114.3(9) . . ? C11A N2A U1 124.9(7) . . ? C10A N2A U1 119.7(7) . . ? O1A C1A C6A 125.3(10) . . ? O1A C1A C2A 115.5(10) . . ? C6A C1A C2A 119.2(11) . . ? O2A C2A C3A 123.2(10) . . ? O2A C2A C1A 115.0(9) . . ? C3A C2A C1A 121.7(11) . . ? C2A C3A C4A 116.9(11) . . ? C2A C3A C7A 121.9(11) . . ? C4A C3A C7A 121.2(11) . . ? C5A C4A C3A 121.4(12) . . ? C4A C5A C6A 121.7(12) . . ? C1A C6A C5A 119.0(11) . . ? N1A C7A C3A 126.6(11) . . ? N1A C8A C9A 112.4(9) . . ? C10A C9A C8A 115.7(10) . . ? N2A C10A C9A 114.0(9) . . ? N2A C11A C12A 126.2(11) . . ? C17A C12A C13A 117.4(10) . . ? C17A C12A C11A 120.3(10) . . ? C13A C12A C11A 122.2(10) . . ? O3A C13A C14A 116.2(10) . . ? O3A C13A C12A 122.1(10) . . ? C14A C13A C12A 121.6(10) . . ? O4A C14A C13A 116.9(10) . . ? O4A C14A C15A 123.3(10) . . ? C13A C14A C15A 119.8(11) . . ? C14A C15A C16A 120.1(11) . . ? C17A C16A C15A 118.7(11) . . ? C16A C17A C12A 122.3(10) . . ? C1B O1B U2 118.9(7) . . ? C1B O1B U1 137.9(7) . . ? U2 O1B U1 103.2(3) . . ? C2B O2B U2 120.2(6) . . ? C13B O3B U1 116.0(7) . 3_566 ? C14B O4B U1 121.4(6) . 3_566 ? C7B N1B C8B 118.8(11) . . ? C11B N2B C10C 124.6(14) . . ? C11B N2B C10B 122.6(12) . . ? O1B C1B C2B 115.7(11) . . ? O1B C1B C6B 124.7(10) . . ? C2B C1B C6B 119.6(11) . . ? O2B C2B C1B 118.6(11) . . ? O2B C2B C3B 122.2(10) . . ? C1B C2B C3B 119.2(12) . . ? C4B C3B C2B 119.5(11) . . ? C4B C3B C7B 121.0(12) . . ? C2B C3B C7B 119.2(13) . . ? C5B C4B C3B 121.8(12) . . ? C4B C5B C6B 118.3(12) . . ? C1B C6B C5B 121.6(11) . . ? N1B C7B C3B 125.9(12) . . ? C9B C8B N1B 106.0(12) . . ? N1B C8B C9C 114.8(13) . . ? C8B C9B C10B 107.5(15) . . ? C10C C9C C8B 109.0(19) . . ? N2B C10B C9B 113.5(16) . . ? N2B C10C C9C 110(2) . . ? N2B C11B C12B 126.9(11) . . ? C13B C12B C17B 120.6(10) . . ? C13B C12B C11B 119.6(10) . . ? C17B C12B C11B 119.5(11) . . ? O3B C13B C14B 117.8(10) . . ? O3B C13B C12B 123.9(10) . . ? C14B C13B C12B 118.3(9) . . ? O4B C14B C15B 124.7(10) . . ? O4B C14B C13B 114.7(9) . . ? C15B C14B C13B 120.6(10) . . ? C14B C15B C16B 120.6(11) . . ? C17B C16B C15B 119.3(11) . . ? C16B C17B C12B 120.5(11) . . ? C1 N1 C5 118.5(13) . . ? C1 N1 U2 121.5(9) . . ? C5 N1 U2 120.0(9) . . ? N1 C1 C2 122.6(15) . . ? C3 C2 C1 118.3(17) . . ? C2 C3 C4 118.6(16) . . ? C5 C4 C3 119.4(14) . . ? N1 C5 C4 122.7(14) . . ? C6 N2 C10 115(2) . . ? C7 C6 N2 127(2) . . ? C6 C7 C8 116(2) . . ? C9 C8 C7 123(2) . . ? C10 C9 C8 112(2) . . ? C9 C10 N2 127(2) . . ? C11 N3 C15 120.0 . . ? N3 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C14 C13 C12 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 N3 120.0 . . ? C25 C16 C22 133(3) . . ? C17 C16 C21 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C24 C20 C23 128(2) . . ? C20 C21 C16 120.0 . . ? C16 C22 C23 111(3) . . ? C20 C23 C22 108(3) . . ? C20 C24 C25 118(3) . . ? C16 C25 C24 117(3) . . ? #===END data_7.16py _database_code_depnum_ccdc_archive 'CCDC 250669' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C268 H222 Cl10 N36 O32 U8' _chemical_formula_weight 6717.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.244(2) _cell_length_b 17.3019(18) _cell_length_c 23.439(2) _cell_angle_alpha 80.542(5) _cell_angle_beta 79.928(5) _cell_angle_gamma 72.362(5) _cell_volume 6137.5(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 46385 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.68 _exptl_crystal_description needle _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method ? _exptl_crystal_F_000 3244 _exptl_absorpt_coefficient_mu 5.444 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.567 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 46385 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.1061 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.68 _reflns_number_total 21529 _reflns_number_gt 4966 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. Some restraints on displacement parameters have been applied. Two pyridine rings were refined as idealized hexagons. The H atoms bound to O and N (pyridinium ion) atoms were not found, nor introduced. All other H atoms were introduced at calculated positions 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0002P)^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 21529 _refine_ls_number_parameters 1570 _refine_ls_number_restraints 762 _refine_ls_R_factor_all 0.2282 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.887 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.137 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 0.29070(5) 0.20723(4) 0.01555(3) 0.0316(2) Uani 1 1 d . . . U2 U 0.45911(5) 0.25722(4) 0.08556(3) 0.0296(2) Uani 1 1 d . . . Cl1A Cl 0.1343(4) 0.3038(3) 0.0560(2) 0.0494(15) Uani 1 1 d . . . Cl2A Cl 0.5557(3) 0.1101(2) 0.13132(17) 0.0418(14) Uani 1 1 d . . . Cl3A Cl 0.5730(3) 0.3134(2) 0.12866(17) 0.0375(13) Uani 1 1 d . . . O1A O 0.5590(7) 0.2504(5) 0.0037(4) 0.028(3) Uani 1 1 d . . . O2A O 0.4421(7) 0.1717(5) 0.0166(4) 0.021(3) Uani 1 1 d . . . O3A O 0.3342(8) 0.1946(6) 0.1055(5) 0.042(3) Uani 1 1 d . . . O4A O 0.3909(8) 0.2572(6) 0.1768(4) 0.042(3) Uani 1 1 d . . . N1A N 0.3670(10) 0.0715(8) -0.0221(5) 0.029(4) Uani 1 1 d . . . N2A N 0.2311(10) 0.1019(7) 0.0845(6) 0.035(4) Uani 1 1 d . . . C1A C 0.5657(12) 0.2004(9) -0.0383(7) 0.029(4) Uani 1 1 d . . . C2A C 0.4996(11) 0.1597(8) -0.0296(6) 0.018(4) Uani 1 1 d . . . C3A C 0.5014(12) 0.1050(9) -0.0686(7) 0.029(4) Uani 1 1 d . . . C4A C 0.5700(13) 0.0911(10) -0.1166(7) 0.039(5) Uani 1 1 d . . . H4A H 0.5728 0.0534 -0.1414 0.047 Uiso 1 1 calc R . . C5A C 0.6331(12) 0.1338(9) -0.1265(7) 0.035(5) Uani 1 1 d . . . H5A H 0.6747 0.1281 -0.1594 0.042 Uiso 1 1 calc R . . C6A C 0.6325(12) 0.1864(9) -0.0851(6) 0.030(4) Uani 1 1 d . . . H6A H 0.6768 0.2114 -0.0895 0.036 Uiso 1 1 calc R . . C7A C 0.4438(14) 0.0540(11) -0.0558(7) 0.045(5) Uani 1 1 d U . . H7A H 0.4613 0.0052 -0.0723 0.054 Uiso 1 1 calc R . . C8A C 0.3233(13) 0.0044(10) -0.0087(7) 0.039(5) Uani 1 1 d U . . H8A1 H 0.3457 -0.0317 0.0248 0.047 Uiso 1 1 calc R . . H8A2 H 0.3396 -0.0272 -0.0415 0.047 Uiso 1 1 calc R . . C9A C 0.2239(12) 0.0318(9) 0.0040(7) 0.030(5) Uani 1 1 d . . . C10A C 0.1754(12) 0.0165(9) -0.0334(7) 0.026(4) Uani 1 1 d . . . H10A H 0.2038 -0.0119 -0.0650 0.031 Uiso 1 1 calc R . . C11A C 0.0887(16) 0.0419(11) -0.0251(9) 0.062(6) Uani 1 1 d . . . H11A H 0.0575 0.0311 -0.0511 0.075 Uiso 1 1 calc R . . C12A C 0.0449(16) 0.0833(11) 0.0206(8) 0.067(7) Uani 1 1 d . . . H12A H -0.0156 0.1015 0.0256 0.080 Uiso 1 1 calc R . . C13A C 0.0940(14) 0.0989(10) 0.0616(8) 0.048(5) Uani 1 1 d . . . H13A H 0.0660 0.1256 0.0941 0.057 Uiso 1 1 calc R . . C14A C 0.1854(13) 0.0718(10) 0.0503(7) 0.038(5) Uani 1 1 d . . . C15A C 0.2195(13) 0.0907(11) 0.1406(8) 0.049(5) Uani 1 1 d U . . H15A H 0.1826 0.0589 0.1577 0.059 Uiso 1 1 calc R . . C16A C 0.2572(12) 0.1219(10) 0.1801(7) 0.035(5) Uani 1 1 d . . . C17A C 0.3088(13) 0.1743(10) 0.1626(7) 0.038(5) Uani 1 1 d . . . C18A C 0.3388(13) 0.2080(10) 0.2009(7) 0.038(5) Uani 1 1 d . . . C19A C 0.3181(14) 0.1851(11) 0.2603(8) 0.056(6) Uani 1 1 d . . . H19A H 0.3394 0.2055 0.2872 0.067 Uiso 1 1 calc R . . C20A C 0.2673(12) 0.1339(9) 0.2800(7) 0.034(5) Uani 1 1 d . . . H20A H 0.2526 0.1207 0.3198 0.041 Uiso 1 1 calc R . . C21A C 0.2389(12) 0.1026(10) 0.2404(7) 0.044(5) Uani 1 1 d . . . H21A H 0.2055 0.0665 0.2540 0.052 Uiso 1 1 calc R . . O1B O 0.3371(7) 0.3212(6) 0.0265(4) 0.031(3) Uani 1 1 d . . . O2B O 0.4237(7) 0.4027(6) 0.0631(4) 0.027(3) Uani 1 1 d . . . O3B O 0.6545(8) 0.7409(6) 0.0813(4) 0.035(3) Uani 1 1 d . . . O4B O 0.7844(8) 0.7991(6) 0.0522(4) 0.036(3) Uani 1 1 d . . . N1B N 0.4577(9) 0.5405(7) 0.0672(5) 0.030(4) Uani 1 1 d . . . N2B N 0.5404(10) 0.6915(7) 0.1625(5) 0.029(4) Uani 1 1 d . . . C1B C 0.3213(11) 0.4010(9) 0.0060(6) 0.024(4) Uani 1 1 d . . . C2B C 0.3705(11) 0.4438(9) 0.0261(7) 0.025(4) Uani 1 1 d . . . C3B C 0.3585(11) 0.5270(9) 0.0049(7) 0.026(4) Uani 1 1 d . . . C4B C 0.2995(12) 0.5669(10) -0.0361(7) 0.038(5) Uani 1 1 d . . . H4B H 0.2925 0.6215 -0.0507 0.045 Uiso 1 1 calc R . . C5B C 0.2542(12) 0.5235(9) -0.0534(7) 0.036(5) Uani 1 1 d . . . H5B H 0.2149 0.5499 -0.0797 0.043 Uiso 1 1 calc R . . C6B C 0.2630(12) 0.4397(9) -0.0338(7) 0.033(5) Uani 1 1 d . . . H6B H 0.2308 0.4117 -0.0470 0.040 Uiso 1 1 calc R . . C7B C 0.4038(12) 0.5733(9) 0.0283(7) 0.032(5) Uani 1 1 d U . . H7B H 0.3940 0.6286 0.0152 0.039 Uiso 1 1 calc R . . C8B C 0.4962(12) 0.5871(9) 0.0974(6) 0.033(5) Uani 1 1 d U . . H8B1 H 0.5080 0.6329 0.0708 0.040 Uiso 1 1 calc R . . H8B2 H 0.5511 0.5523 0.1093 0.040 Uiso 1 1 calc R . . C9B C 0.4353(11) 0.6180(9) 0.1502(6) 0.021(4) Uani 1 1 d . . . C10B C 0.3572(13) 0.5998(10) 0.1662(7) 0.038(5) Uani 1 1 d . . . H10B H 0.3406 0.5689 0.1438 0.046 Uiso 1 1 calc R . . C11B C 0.3029(14) 0.6275(10) 0.2160(8) 0.053(6) Uani 1 1 d . . . H11B H 0.2495 0.6160 0.2262 0.064 Uiso 1 1 calc R . . C12B C 0.3281(13) 0.6727(10) 0.2511(7) 0.042(5) Uani 1 1 d . . . H12B H 0.2942 0.6878 0.2859 0.051 Uiso 1 1 calc R . . C13B C 0.4028(12) 0.6934(9) 0.2328(7) 0.032(5) Uani 1 1 d . . . H13B H 0.4176 0.7260 0.2549 0.038 Uiso 1 1 calc R . . C14B C 0.4594(12) 0.6691(9) 0.1826(6) 0.025(4) Uani 1 1 d . . . C15B C 0.5747(12) 0.7124(9) 0.1999(7) 0.032(5) Uani 1 1 d U . . H15B H 0.5514 0.7081 0.2390 0.039 Uiso 1 1 calc R . . C16B C 0.6491(14) 0.7428(11) 0.1820(8) 0.045(5) Uani 1 1 d . . . C17B C 0.6822(13) 0.7548(10) 0.1255(8) 0.040(5) Uani 1 1 d . . . C18B C 0.7523(13) 0.7920(10) 0.1099(7) 0.040(5) Uani 1 1 d . . . C19B C 0.7868(13) 0.8190(11) 0.1522(8) 0.050(6) Uani 1 1 d . . . H19B H 0.8306 0.8450 0.1414 0.059 Uiso 1 1 calc R . . C20B C 0.7516(14) 0.8045(11) 0.2119(8) 0.050(5) Uani 1 1 d . . . H20B H 0.7735 0.8198 0.2411 0.060 Uiso 1 1 calc R . . C21B C 0.6862(15) 0.7684(11) 0.2259(9) 0.061(6) Uani 1 1 d . . . H21B H 0.6639 0.7596 0.2650 0.073 Uiso 1 1 calc R . . U3 U 0.73431(6) 0.11259(4) 0.46620(3) 0.0375(2) Uani 1 1 d . . . U4 U 0.57952(6) 0.23661(4) 0.57870(3) 0.0335(2) Uani 1 1 d . . . Cl1C Cl 0.8793(4) 0.1583(3) 0.46250(19) 0.0477(15) Uani 1 1 d . . . Cl2C Cl 0.4543(3) 0.3316(2) 0.65116(17) 0.0391(13) Uani 1 1 d . . . O1C O 0.4644(8) 0.2693(6) 0.5266(4) 0.035(3) Uani 1 1 d . . . O2C O 0.5914(8) 0.1350(6) 0.5135(4) 0.032(3) Uani 1 1 d . . . O3C O 0.7123(8) 0.1150(6) 0.5657(4) 0.038(3) Uani 1 1 d . . . O4C O 0.6687(9) 0.2078(7) 0.6479(4) 0.038(3) Uani 1 1 d . . . N1C N 0.6644(12) -0.0008(8) 0.4597(6) 0.042(4) Uani 1 1 d . . . N2C N 0.8293(11) -0.0193(8) 0.5154(6) 0.042(4) Uani 1 1 d . . . C1C C 0.4587(13) 0.2212(11) 0.4890(7) 0.035(5) Uani 1 1 d . . . C2C C 0.5256(13) 0.1526(10) 0.4825(7) 0.031(5) Uani 1 1 d . . . C3C C 0.5199(13) 0.0946(10) 0.4441(7) 0.036(5) Uani 1 1 d . . . C4C C 0.4511(15) 0.1181(12) 0.4107(8) 0.055(6) Uani 1 1 d . . . H4C H 0.4484 0.0831 0.3853 0.066 Uiso 1 1 calc R . . C5C C 0.3852(15) 0.1934(11) 0.4143(8) 0.055(6) Uani 1 1 d . . . H5C H 0.3395 0.2085 0.3920 0.066 Uiso 1 1 calc R . . C6C C 0.3924(13) 0.2442(10) 0.4533(7) 0.040(5) Uani 1 1 d . . . H6C H 0.3515 0.2950 0.4554 0.048 Uiso 1 1 calc R . . C7C C 0.5890(14) 0.0148(11) 0.4474(7) 0.043(5) Uani 1 1 d U . . H7C H 0.5737 -0.0294 0.4391 0.051 Uiso 1 1 calc R . . C8C C 0.7168(14) -0.0878(10) 0.4726(8) 0.043(5) Uani 1 1 d U . . H8C1 H 0.7108 -0.1021 0.5146 0.052 Uiso 1 1 calc R . . H8C2 H 0.6916 -0.1223 0.4566 0.052 Uiso 1 1 calc R . . C9C C 0.8071(13) -0.1067(9) 0.4511(7) 0.027(4) Uani 1 1 d . . . C10C C 0.8442(16) -0.1561(11) 0.4072(8) 0.058(6) Uani 1 1 d . . . H10C H 0.8081 -0.1760 0.3904 0.069 Uiso 1 1 calc R . . C11C C 0.9309(14) -0.1771(11) 0.3876(7) 0.045(5) Uani 1 1 d . . . H11C H 0.9533 -0.2128 0.3594 0.054 Uiso 1 1 calc R . . C12C C 0.9836(16) -0.1465(12) 0.4086(8) 0.066(7) Uani 1 1 d . . . H12C H 1.0427 -0.1600 0.3944 0.079 Uiso 1 1 calc R . . C13C C 0.9511(15) -0.0939(11) 0.4523(8) 0.054(6) Uani 1 1 d . . . H13C H 0.9872 -0.0716 0.4671 0.065 Uiso 1 1 calc R . . C14C C 0.8609(13) -0.0764(9) 0.4727(7) 0.033(5) Uani 1 1 d . . . C15C C 0.8652(14) -0.0287(11) 0.5611(8) 0.045(5) Uani 1 1 d U . . H15C H 0.9123 -0.0746 0.5662 0.054 Uiso 1 1 calc R . . C16C C 0.8385(13) 0.0271(10) 0.6070(7) 0.036(5) Uani 1 1 d . . . C17C C 0.7667(13) 0.0940(11) 0.6080(7) 0.036(5) Uani 1 1 d . . . C18C C 0.7422(12) 0.1468(10) 0.6520(7) 0.028(4) Uani 1 1 d . . . C19C C 0.7938(13) 0.1231(11) 0.6975(7) 0.040(5) Uani 1 1 d . . . H19C H 0.7767 0.1528 0.7293 0.048 Uiso 1 1 calc R . . C20C C 0.8670(13) 0.0596(10) 0.6977(7) 0.039(5) Uani 1 1 d . . . H20C H 0.9001 0.0485 0.7282 0.047 Uiso 1 1 calc R . . C21C C 0.8931(13) 0.0109(10) 0.6526(7) 0.036(5) Uani 1 1 d . . . H21C H 0.9447 -0.0314 0.6518 0.043 Uiso 1 1 calc R . . O1D O 0.3280(8) 0.7490(6) 0.5136(4) 0.038(3) Uani 1 1 d . . . O2D O 0.4103(8) 0.6283(6) 0.4514(5) 0.038(3) Uani 1 1 d . . . O3D O 0.6651(8) 0.1834(6) 0.3811(5) 0.038(3) Uani 1 1 d . . . O4D O 0.8009(8) 0.0608(7) 0.3853(4) 0.044(3) Uani 1 1 d . . . N1D N 0.4533(10) 0.4762(7) 0.4376(5) 0.028(4) Uani 1 1 d . . . N2D N 0.5417(10) 0.2846(7) 0.3228(5) 0.025(4) Uani 1 1 d . . . C1D C 0.3157(13) 0.6733(11) 0.5360(7) 0.038(5) Uani 1 1 d . . . C2D C 0.3600(12) 0.6094(10) 0.5027(7) 0.031(5) Uani 1 1 d . . . C3D C 0.3622(13) 0.5298(10) 0.5216(8) 0.037(5) Uani 1 1 d . . . C4D C 0.3147(12) 0.5158(9) 0.5762(7) 0.032(5) Uani 1 1 d . . . H4D H 0.3145 0.4626 0.5911 0.039 Uiso 1 1 calc R . . C5D C 0.2685(12) 0.5781(10) 0.6086(7) 0.038(5) Uani 1 1 d . . . H5D H 0.2383 0.5666 0.6449 0.046 Uiso 1 1 calc R . . C6D C 0.2667(12) 0.6581(10) 0.5874(7) 0.036(5) Uani 1 1 d . . . H6D H 0.2324 0.7008 0.6080 0.044 Uiso 1 1 calc R . . C7D C 0.4096(12) 0.4642(10) 0.4877(7) 0.036(5) Uani 1 1 d U . . H7D H 0.4085 0.4112 0.5027 0.043 Uiso 1 1 calc R . . C8D C 0.4927(13) 0.4089(10) 0.4015(7) 0.046(6) Uani 1 1 d U . . H8D1 H 0.5034 0.3571 0.4263 0.056 Uiso 1 1 calc R . . H8D2 H 0.5481 0.4141 0.3805 0.056 Uiso 1 1 calc R . . C9D C 0.4325(14) 0.4105(11) 0.3586(7) 0.038(5) Uani 1 1 d . . . C10D C 0.3603(13) 0.4677(10) 0.3530(7) 0.034(5) Uani 1 1 d . . . H10D H 0.3438 0.5092 0.3769 0.040 Uiso 1 1 calc R . . C11D C 0.3065(16) 0.4689(13) 0.3122(9) 0.070(7) Uani 1 1 d . . . H11D H 0.2529 0.5081 0.3109 0.084 Uiso 1 1 calc R . . C12D C 0.3349(15) 0.4102(12) 0.2737(8) 0.054(6) Uani 1 1 d . . . H12D H 0.3005 0.4129 0.2452 0.065 Uiso 1 1 calc R . . C13D C 0.4080(13) 0.3510(11) 0.2757(7) 0.039(5) Uani 1 1 d . . . H13D H 0.4238 0.3114 0.2503 0.047 Uiso 1 1 calc R . . C14D C 0.4627(13) 0.3490(10) 0.3179(7) 0.034(5) Uani 1 1 d . . . C15D C 0.5823(13) 0.2398(10) 0.2790(7) 0.041(5) Uani 1 1 d U . . H15D H 0.5579 0.2524 0.2444 0.049 Uiso 1 1 calc R . . C16D C 0.6575(12) 0.1764(10) 0.2820(7) 0.026(4) Uani 1 1 d . . . C17D C 0.6940(13) 0.1476(10) 0.3326(7) 0.030(4) Uani 1 1 d . . . C18D C 0.7690(12) 0.0783(10) 0.3358(6) 0.025(4) Uani 1 1 d . . . C19D C 0.8024(12) 0.0366(10) 0.2879(7) 0.036(5) Uani 1 1 d . . . H19D H 0.8508 -0.0089 0.2891 0.043 Uiso 1 1 calc R . . C20D C 0.7608(14) 0.0646(11) 0.2359(8) 0.050(6) Uani 1 1 d . . . H20D H 0.7821 0.0363 0.2035 0.060 Uiso 1 1 calc R . . C21D C 0.6897(13) 0.1331(11) 0.2335(8) 0.044(5) Uani 1 1 d . . . H21D H 0.6634 0.1504 0.1996 0.052 Uiso 1 1 calc R . . N1 N 0.5127(11) 0.1280(8) 0.6480(6) 0.032(4) Uani 1 1 d U . . C1 C 0.4359(14) 0.1306(11) 0.6449(7) 0.043(5) Uani 1 1 d U . . H1 H 0.4057 0.1699 0.6180 0.052 Uiso 1 1 calc R . . C2 C 0.3916(14) 0.0752(11) 0.6812(8) 0.050(6) Uani 1 1 d U . . H2 H 0.3353 0.0763 0.6772 0.060 Uiso 1 1 calc R . . C3 C 0.4395(15) 0.0190(12) 0.7235(8) 0.056(6) Uani 1 1 d U . . H3 H 0.4141 -0.0173 0.7488 0.067 Uiso 1 1 calc R . . C4 C 0.5205(14) 0.0183(10) 0.7267(7) 0.040(5) Uani 1 1 d U . . H4 H 0.5527 -0.0177 0.7541 0.048 Uiso 1 1 calc R . . C5 C 0.5562(16) 0.0750(12) 0.6862(9) 0.064(7) Uani 1 1 d U . . H5 H 0.6135 0.0741 0.6872 0.077 Uiso 1 1 calc R . . N2 N 1.1007(12) 0.7165(10) -0.0115(7) 0.067(4) Uani 1 1 d U . . C6 C 1.1549(15) 0.7439(12) 0.0170(9) 0.069(4) Uani 1 1 d U . . H6 H 1.1515 0.7346 0.0574 0.082 Uiso 1 1 calc R . . C7 C 1.2138(15) 0.7852(12) -0.0154(9) 0.064(4) Uani 1 1 d U . . H7 H 1.2533 0.7990 0.0024 0.076 Uiso 1 1 calc R . . C8 C 1.2108(15) 0.8028(11) -0.0700(9) 0.063(4) Uani 1 1 d U . . H8 H 1.2466 0.8338 -0.0908 0.075 Uiso 1 1 calc R . . C9 C 1.1593(15) 0.7799(12) -0.1008(9) 0.067(4) Uani 1 1 d U . . H9 H 1.1604 0.7937 -0.1409 0.080 Uiso 1 1 calc R . . C10 C 1.1058(15) 0.7355(12) -0.0687(9) 0.064(4) Uani 1 1 d U . . H10 H 1.0712 0.7178 -0.0885 0.077 Uiso 1 1 calc R . . N3 N 1.0118(13) 0.6204(11) 0.0529(7) 0.073(4) Uani 1 1 d U . . C11 C 1.0345(15) 0.5378(13) 0.0563(9) 0.065(4) Uani 1 1 d U . . H11 H 1.0806 0.5107 0.0306 0.078 Uiso 1 1 calc R . . C12 C 0.9893(16) 0.4934(14) 0.0979(9) 0.072(5) Uani 1 1 d U . . H12 H 1.0069 0.4367 0.1008 0.086 Uiso 1 1 calc R . . C13 C 0.9237(16) 0.5295(13) 0.1325(9) 0.069(4) Uani 1 1 d U . . H13 H 0.8956 0.4983 0.1608 0.082 Uiso 1 1 calc R . . C14 C 0.8941(16) 0.6123(13) 0.1289(9) 0.070(5) Uani 1 1 d U . . H14 H 0.8444 0.6395 0.1519 0.085 Uiso 1 1 calc R . . C15 C 0.9455(17) 0.6539(14) 0.0871(9) 0.074(5) Uani 1 1 d U . . H15 H 0.9290 0.7106 0.0845 0.089 Uiso 1 1 calc R . . N4 N 1.0039(13) 0.1785(11) 0.1986(8) 0.075(4) Uani 1 1 d U . . C16 C 0.9589(16) 0.1426(14) 0.2475(10) 0.074(4) Uani 1 1 d U . . H16 H 0.9508 0.0916 0.2476 0.089 Uiso 1 1 calc R . . C17 C 0.9284(15) 0.1836(13) 0.2930(9) 0.074(5) Uani 1 1 d U . . H17 H 0.8989 0.1595 0.3253 0.089 Uiso 1 1 calc R . . C18 C 0.9371(16) 0.2598(14) 0.2965(10) 0.076(5) Uani 1 1 d U . . H18 H 0.9152 0.2866 0.3297 0.091 Uiso 1 1 calc R . . C19 C 0.9809(16) 0.2937(14) 0.2468(10) 0.079(5) Uani 1 1 d U . . H19 H 0.9869 0.3459 0.2451 0.095 Uiso 1 1 calc R . . C20 C 1.0138(16) 0.2509(13) 0.2024(10) 0.076(5) Uani 1 1 d U . . H20 H 1.0465 0.2732 0.1711 0.091 Uiso 1 1 calc R . . N5 N 0.8988(15) 0.5314(12) 0.3085(7) 0.040(5) Uani 1 1 d GU . . C21 C 0.9333(13) 0.4938(10) 0.3596(10) 0.041(5) Uani 1 1 d GU . . H21 H 0.9736 0.4424 0.3603 0.050 Uiso 1 1 calc R . . C22 C 0.9075(15) 0.5328(13) 0.4098(7) 0.042(6) Uani 1 1 d GU . . H22 H 0.9306 0.5076 0.4440 0.050 Uiso 1 1 calc R . . C23 C 0.8472(15) 0.6096(13) 0.4089(7) 0.043(6) Uani 1 1 d GU . . H23 H 0.8300 0.6357 0.4424 0.052 Uiso 1 1 calc R . . C24 C 0.8127(14) 0.6472(10) 0.3577(10) 0.041(6) Uani 1 1 d GU . . H24 H 0.7723 0.6986 0.3571 0.049 Uiso 1 1 calc R . . C25 C 0.8385(15) 0.6082(13) 0.3076(8) 0.042(5) Uani 1 1 d GU . . H25 H 0.8154 0.6334 0.2734 0.050 Uiso 1 1 calc R . . N6 N 0.1304(10) 0.3525(7) 0.4575(6) 0.090(5) Uani 1 1 d GU . . C26 C 0.1759(9) 0.3441(8) 0.4018(7) 0.085(5) Uani 1 1 d GU . . H26 H 0.2205 0.3686 0.3888 0.102 Uiso 1 1 calc R . . C27 C 0.1548(10) 0.2989(9) 0.3656(5) 0.089(5) Uani 1 1 d GU . . H27 H 0.1852 0.2933 0.3283 0.106 Uiso 1 1 calc R . . C28 C 0.0881(11) 0.2623(8) 0.3850(6) 0.092(5) Uani 1 1 d GU . . H28 H 0.0739 0.2321 0.3608 0.110 Uiso 1 1 calc R . . C29 C 0.0426(9) 0.2707(9) 0.4407(7) 0.089(5) Uani 1 1 d GU . . H29 H -0.0020 0.2462 0.4538 0.107 Uiso 1 1 calc R . . C30 C 0.0638(10) 0.3158(9) 0.4770(5) 0.093(5) Uani 1 1 d GU . . H30 H 0.0333 0.3215 0.5142 0.112 Uiso 1 1 calc R . . N7 N 0.0999(15) 0.8992(13) 0.1473(8) 0.088(5) Uani 1 1 d U . . C31 C 0.019(2) 0.9339(15) 0.1634(10) 0.085(5) Uani 1 1 d U . . H31 H -0.0017 0.9885 0.1486 0.102 Uiso 1 1 calc R . . C32 C -0.0358(19) 0.9038(16) 0.1966(10) 0.087(5) Uani 1 1 d U . . H32 H -0.0937 0.9331 0.2058 0.104 Uiso 1 1 calc R . . C33 C -0.0034(19) 0.8258(16) 0.2175(10) 0.092(5) Uani 1 1 d U . . H33 H -0.0421 0.8045 0.2449 0.111 Uiso 1 1 calc R . . C34 C 0.0727(19) 0.7745(16) 0.2063(11) 0.092(5) Uani 1 1 d U . . H34 H 0.0881 0.7198 0.2216 0.110 Uiso 1 1 calc R . . C35 C 0.1282(18) 0.8133(14) 0.1679(10) 0.084(5) Uani 1 1 d U . . H35 H 0.1846 0.7830 0.1555 0.101 Uiso 1 1 calc R . . N8 N 0.162(2) 0.6102(16) 0.4646(12) 0.039(5) Uani 1 1 d U . . C36 C 0.1716(14) 0.6729(11) 0.4198(8) 0.053(4) Uani 1 1 d U . . H36 H 0.1994 0.7090 0.4277 0.064 Uiso 1 1 calc R . . C37 C 0.146(2) 0.686(2) 0.3684(15) 0.045(5) Uani 1 1 d U . . H37 H 0.1515 0.7332 0.3441 0.054 Uiso 1 1 calc R . . C38 C 0.1144(15) 0.6393(12) 0.3508(9) 0.065(5) Uani 1 1 d U . . H38 H 0.0968 0.6477 0.3140 0.077 Uiso 1 1 calc R . . C39 C 0.1083(15) 0.5756(12) 0.3898(9) 0.065(5) Uani 1 1 d U . . H39 H 0.0867 0.5374 0.3784 0.078 Uiso 1 1 calc R . . C40 C 0.130(2) 0.561(2) 0.4424(14) 0.040(5) Uani 1 1 d U . . H40 H 0.1216 0.5144 0.4656 0.048 Uiso 1 1 calc R . . N9 N 0.1993(13) 0.4215(11) 0.1463(8) 0.079(4) Uani 1 1 d U . . C41 C 0.1570(16) 0.3967(14) 0.1991(9) 0.072(4) Uani 1 1 d U . . H41 H 0.1621 0.3416 0.2109 0.087 Uiso 1 1 calc R . . C42 C 0.1085(15) 0.4530(13) 0.2331(9) 0.067(4) Uani 1 1 d U . . H42 H 0.0756 0.4371 0.2671 0.080 Uiso 1 1 calc R . . C43 C 0.1061(15) 0.5318(13) 0.2195(9) 0.065(4) Uani 1 1 d U . . H43 H 0.0762 0.5683 0.2462 0.078 Uiso 1 1 calc R . . C44 C 0.1464(15) 0.5604(12) 0.1672(9) 0.061(4) Uani 1 1 d U . . H44 H 0.1407 0.6158 0.1564 0.073 Uiso 1 1 calc R . . C45 C 0.1942(15) 0.5040(13) 0.1330(9) 0.069(4) Uani 1 1 d U . . H45 H 0.2256 0.5207 0.0985 0.082 Uiso 1 1 calc R . . N10 N 0.7670(12) 0.4686(10) 0.2343(7) 0.058(4) Uani 1 1 d U . . C46 C 0.7640(15) 0.4090(12) 0.2087(8) 0.057(4) Uani 1 1 d U . . H46 H 0.8164 0.3780 0.1906 0.069 Uiso 1 1 calc R . . C47 C 0.6889(15) 0.3871(12) 0.2059(8) 0.058(4) Uani 1 1 d U . . H47 H 0.6915 0.3382 0.1931 0.070 Uiso 1 1 calc R . . C48 C 0.6110(15) 0.4422(11) 0.2232(7) 0.049(4) Uani 1 1 d U . . H48 H 0.5586 0.4373 0.2156 0.059 Uiso 1 1 calc R . . C49 C 0.6125(15) 0.5022(11) 0.2509(7) 0.051(4) Uani 1 1 d U . . H49 H 0.5606 0.5336 0.2693 0.061 Uiso 1 1 calc R . . C50 C 0.6854(15) 0.5182(12) 0.2530(8) 0.050(4) Uani 1 1 d U . . H50 H 0.6824 0.5657 0.2680 0.060 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 0.0435(6) 0.0270(4) 0.0274(4) 0.0011(3) -0.0058(4) -0.0162(4) U2 0.0454(6) 0.0239(4) 0.0221(4) 0.0006(3) -0.0065(4) -0.0142(4) Cl1A 0.046(4) 0.039(3) 0.061(3) -0.011(3) 0.003(3) -0.011(3) Cl2A 0.069(5) 0.029(3) 0.033(3) 0.003(2) -0.022(3) -0.016(3) Cl3A 0.049(4) 0.038(3) 0.033(2) 0.001(2) -0.016(3) -0.020(3) O1A 0.037(7) 0.015(5) 0.025(5) -0.001(4) 0.007(5) -0.002(5) O2A 0.021(7) 0.015(5) 0.029(5) -0.004(4) -0.005(5) -0.007(5) O3A 0.053(8) 0.034(6) 0.032(6) 0.002(5) -0.004(6) -0.008(6) O4A 0.064(8) 0.037(6) 0.037(6) -0.009(5) -0.021(6) -0.021(6) N1A 0.032(8) 0.032(7) 0.030(6) -0.003(5) -0.003(6) -0.019(6) N2A 0.039(8) 0.029(7) 0.046(7) 0.001(6) -0.009(6) -0.023(6) C1A 0.024(9) 0.031(7) 0.033(7) -0.008(6) -0.006(7) -0.008(7) C2A 0.018(4) 0.017(4) 0.018(4) -0.0025(11) -0.0024(11) -0.0050(14) C3A 0.028(9) 0.029(7) 0.031(7) -0.006(6) 0.002(7) -0.010(7) C4A 0.039(10) 0.034(8) 0.040(8) 0.006(7) 0.001(7) -0.012(7) C5A 0.043(9) 0.031(8) 0.027(7) 0.001(6) 0.008(7) -0.014(7) C6A 0.028(9) 0.031(7) 0.026(7) 0.005(6) 0.008(7) -0.011(7) C7A 0.048(10) 0.048(8) 0.047(8) -0.022(7) -0.008(7) -0.016(7) C8A 0.042(10) 0.040(8) 0.038(8) 0.005(7) -0.004(7) -0.021(7) C9A 0.028(9) 0.028(7) 0.021(7) 0.001(6) 0.000(7) 0.008(7) C10A 0.026(9) 0.021(7) 0.036(8) 0.000(6) -0.007(7) -0.013(7) C11A 0.065(11) 0.058(9) 0.069(10) -0.012(8) -0.012(8) -0.021(8) C12A 0.068(11) 0.064(10) 0.069(10) -0.010(8) -0.006(8) -0.021(8) C13A 0.038(10) 0.046(8) 0.057(9) -0.010(7) -0.002(8) -0.009(7) C14A 0.031(9) 0.039(8) 0.048(8) -0.009(7) -0.005(7) -0.015(7) C15A 0.052(10) 0.054(9) 0.046(9) -0.011(7) 0.002(7) -0.025(8) C16A 0.041(9) 0.035(8) 0.028(8) -0.002(6) -0.001(7) -0.014(7) C17A 0.047(10) 0.037(8) 0.030(8) -0.013(7) 0.003(7) -0.012(7) C18A 0.044(10) 0.039(8) 0.039(8) -0.005(7) 0.000(7) -0.026(7) C19A 0.061(10) 0.066(9) 0.057(9) -0.019(8) -0.014(8) -0.032(8) C20A 0.040(9) 0.032(8) 0.029(8) -0.007(6) -0.002(7) -0.009(7) C21A 0.046(10) 0.038(8) 0.043(8) -0.004(7) 0.013(7) -0.017(7) O1B 0.034(7) 0.029(6) 0.022(5) 0.004(5) -0.001(5) -0.003(5) O2B 0.035(7) 0.031(6) 0.024(5) -0.009(5) -0.012(5) -0.014(5) O3B 0.039(8) 0.030(6) 0.031(6) -0.009(5) -0.005(5) 0.003(5) O4B 0.047(8) 0.032(6) 0.030(6) 0.005(5) -0.003(5) -0.018(6) N1B 0.032(8) 0.027(7) 0.034(7) 0.000(6) -0.015(6) -0.010(6) N2B 0.034(8) 0.033(7) 0.028(6) 0.000(5) -0.001(6) -0.023(6) C1B 0.017(9) 0.023(7) 0.024(7) 0.011(6) 0.003(6) -0.006(7) C2B 0.015(9) 0.029(7) 0.033(7) -0.009(6) -0.012(7) -0.002(7) C3B 0.030(9) 0.024(7) 0.033(7) -0.009(6) -0.004(7) -0.018(7) C4B 0.043(10) 0.036(8) 0.034(8) -0.003(7) -0.003(7) -0.014(7) C5B 0.039(9) 0.026(7) 0.037(8) 0.010(6) -0.008(7) -0.008(7) C6B 0.031(9) 0.028(8) 0.040(8) 0.000(6) -0.006(7) -0.009(7) C7B 0.037(9) 0.019(7) 0.037(8) -0.010(6) 0.010(7) -0.004(7) C8B 0.039(9) 0.024(7) 0.034(8) 0.004(6) -0.002(7) -0.013(7) C9B 0.018(9) 0.027(7) 0.013(7) 0.006(6) 0.002(6) -0.005(7) C10B 0.038(10) 0.041(8) 0.036(8) -0.010(7) 0.002(7) -0.011(7) C11B 0.056(10) 0.052(9) 0.056(9) -0.013(7) -0.001(8) -0.021(8) C12B 0.045(10) 0.036(8) 0.046(8) -0.002(7) 0.001(7) -0.016(7) C13B 0.035(9) 0.039(8) 0.028(7) -0.010(6) -0.009(7) -0.015(7) C14B 0.025(9) 0.028(7) 0.017(7) -0.009(6) -0.002(6) -0.001(7) C15B 0.043(9) 0.029(7) 0.028(7) -0.004(6) -0.001(7) -0.016(7) C16B 0.048(10) 0.050(9) 0.039(8) -0.004(7) -0.011(7) -0.014(7) C17B 0.044(10) 0.039(8) 0.034(8) -0.003(7) -0.009(7) -0.009(7) C18B 0.049(10) 0.039(8) 0.031(8) -0.007(7) -0.011(7) -0.005(7) C19B 0.049(10) 0.060(9) 0.047(9) -0.005(7) -0.010(7) -0.024(8) C20B 0.053(10) 0.054(9) 0.042(8) 0.012(7) -0.010(7) -0.022(8) C21B 0.061(11) 0.068(9) 0.053(9) 0.003(8) -0.011(8) -0.019(8) U3 0.0615(7) 0.0288(4) 0.0240(4) -0.0021(3) -0.0019(4) -0.0180(4) U4 0.0562(7) 0.0255(4) 0.0214(4) -0.0002(3) -0.0028(4) -0.0181(4) Cl1C 0.058(5) 0.039(3) 0.047(3) 0.003(2) -0.009(3) -0.017(3) Cl2C 0.049(4) 0.033(3) 0.031(2) -0.001(2) -0.005(3) -0.008(3) O1C 0.046(8) 0.029(6) 0.026(5) -0.004(5) -0.006(5) -0.002(5) O2C 0.047(8) 0.019(5) 0.029(6) 0.003(5) 0.001(5) -0.015(5) O3C 0.053(8) 0.037(6) 0.019(5) -0.002(5) 0.001(5) -0.008(6) O4C 0.051(8) 0.037(6) 0.023(5) 0.002(5) -0.003(5) -0.013(6) N1C 0.051(9) 0.028(7) 0.041(7) -0.003(6) 0.000(7) -0.005(7) N2C 0.047(9) 0.030(7) 0.042(7) -0.010(6) 0.004(7) -0.004(6) C1C 0.033(9) 0.042(8) 0.030(8) -0.008(7) 0.002(7) -0.012(7) C2C 0.038(9) 0.024(7) 0.037(8) 0.000(6) 0.001(7) -0.020(7) C3C 0.042(10) 0.028(8) 0.039(8) -0.005(7) 0.005(7) -0.016(7) C4C 0.059(10) 0.054(9) 0.058(9) -0.009(7) -0.008(8) -0.022(8) C5C 0.057(10) 0.058(9) 0.052(9) -0.007(7) -0.006(8) -0.019(8) C6C 0.048(10) 0.031(8) 0.038(8) 0.004(7) -0.005(7) -0.012(7) C7C 0.053(10) 0.038(8) 0.037(8) -0.013(7) -0.004(7) -0.010(8) C8C 0.058(10) 0.028(8) 0.044(8) -0.001(7) -0.009(7) -0.013(7) C9C 0.030(9) 0.024(7) 0.032(8) -0.001(6) -0.001(7) -0.017(7) C10C 0.063(11) 0.049(9) 0.061(9) -0.003(7) -0.004(8) -0.018(8) C11C 0.050(10) 0.043(8) 0.042(8) -0.018(7) -0.001(8) -0.008(8) C12C 0.073(11) 0.059(9) 0.059(10) -0.005(8) -0.001(8) -0.015(8) C13C 0.062(10) 0.044(9) 0.049(9) 0.002(7) 0.001(8) -0.012(8) C14C 0.038(9) 0.021(7) 0.030(8) 0.001(6) 0.001(7) 0.003(7) C15C 0.047(10) 0.038(8) 0.047(9) 0.004(7) 0.000(7) -0.013(7) C16C 0.035(9) 0.034(8) 0.034(8) 0.000(7) 0.002(7) -0.006(7) C17C 0.041(10) 0.036(8) 0.036(8) -0.004(7) -0.001(7) -0.021(7) C18C 0.021(9) 0.031(8) 0.026(7) 0.000(6) 0.004(7) -0.006(7) C19C 0.049(10) 0.037(8) 0.038(8) 0.002(7) -0.001(7) -0.022(7) C20C 0.038(10) 0.033(8) 0.044(8) 0.008(7) 0.006(7) -0.019(7) C21C 0.037(9) 0.035(8) 0.032(8) 0.007(7) -0.001(7) -0.011(7) O1D 0.048(8) 0.026(6) 0.034(6) -0.003(5) 0.006(5) -0.011(6) O2D 0.049(8) 0.030(6) 0.033(6) -0.003(5) -0.007(6) -0.008(6) O3D 0.044(8) 0.031(6) 0.038(6) -0.009(5) -0.001(5) -0.010(5) O4D 0.057(8) 0.049(6) 0.024(6) 0.003(5) -0.015(6) -0.011(6) N1D 0.030(8) 0.028(7) 0.023(6) -0.006(5) 0.002(6) -0.003(6) N2D 0.031(8) 0.016(6) 0.029(6) -0.008(5) -0.002(6) -0.004(6) C1D 0.036(9) 0.046(8) 0.035(8) -0.008(7) -0.011(7) -0.012(7) C2D 0.034(9) 0.035(8) 0.028(7) -0.018(7) -0.003(7) -0.007(7) C3D 0.035(9) 0.037(8) 0.045(8) 0.007(7) -0.017(7) -0.019(7) C4D 0.040(9) 0.018(7) 0.034(8) 0.002(6) 0.003(7) -0.009(7) C5D 0.031(9) 0.029(8) 0.044(8) 0.010(7) 0.003(7) -0.006(7) C6D 0.034(9) 0.026(7) 0.043(8) 0.007(6) 0.012(7) -0.014(7) C7D 0.035(9) 0.034(8) 0.046(8) -0.003(7) -0.014(7) -0.019(7) C8D 0.053(10) 0.040(8) 0.043(8) -0.009(7) -0.003(7) -0.008(7) C9D 0.041(10) 0.041(8) 0.031(8) -0.008(7) -0.005(7) -0.007(7) C10D 0.039(9) 0.034(8) 0.029(8) 0.000(6) -0.012(7) -0.010(7) C11D 0.068(11) 0.069(10) 0.076(10) -0.013(8) -0.013(8) -0.019(8) C12D 0.050(10) 0.062(9) 0.053(9) 0.002(7) -0.011(8) -0.020(8) C13D 0.042(10) 0.037(8) 0.038(8) -0.007(7) -0.004(7) -0.010(7) C14D 0.038(9) 0.033(8) 0.033(8) -0.007(7) -0.004(7) -0.012(7) C15D 0.051(10) 0.043(8) 0.033(8) -0.007(7) -0.011(7) -0.017(7) C16D 0.035(9) 0.026(7) 0.024(7) -0.004(6) -0.017(7) -0.013(7) C17D 0.035(9) 0.038(8) 0.019(7) -0.002(6) 0.001(7) -0.019(7) C18D 0.033(9) 0.030(7) 0.017(7) -0.004(6) 0.000(6) -0.018(7) C19D 0.040(10) 0.034(8) 0.036(8) -0.001(7) -0.006(7) -0.014(7) C20D 0.059(10) 0.054(9) 0.039(8) -0.009(7) -0.008(8) -0.014(8) C21D 0.052(10) 0.043(8) 0.042(8) -0.004(7) -0.021(7) -0.014(7) N1 0.041(9) 0.024(7) 0.027(7) 0.011(5) -0.004(6) -0.013(6) C1 0.050(10) 0.041(8) 0.043(9) -0.009(7) 0.000(8) -0.022(8) C2 0.055(10) 0.048(9) 0.056(9) -0.008(7) -0.010(8) -0.025(8) C3 0.063(11) 0.058(9) 0.063(9) -0.018(8) -0.019(8) -0.030(8) C4 0.043(10) 0.037(8) 0.033(8) 0.010(7) -0.003(7) -0.010(7) C5 0.062(11) 0.063(10) 0.072(10) -0.014(8) -0.012(8) -0.019(8) N2 0.067(7) 0.066(6) 0.066(6) -0.010(6) -0.013(6) -0.013(5) C6 0.066(7) 0.068(7) 0.067(7) -0.008(6) -0.011(6) -0.010(6) C7 0.061(7) 0.062(6) 0.067(7) -0.009(6) -0.009(6) -0.017(6) C8 0.063(7) 0.057(6) 0.066(7) -0.004(6) -0.006(6) -0.017(6) C9 0.069(7) 0.066(7) 0.065(7) -0.007(6) -0.011(6) -0.016(6) C10 0.068(7) 0.064(6) 0.064(7) -0.013(6) -0.014(6) -0.018(6) N3 0.073(7) 0.072(6) 0.070(6) -0.012(6) -0.009(6) -0.015(6) C11 0.071(7) 0.062(7) 0.066(7) -0.015(6) -0.006(6) -0.022(6) C12 0.069(7) 0.072(7) 0.068(7) -0.009(6) -0.004(6) -0.015(6) C13 0.067(7) 0.068(7) 0.068(7) -0.009(6) -0.004(6) -0.017(6) C14 0.071(7) 0.063(7) 0.069(7) -0.002(6) 0.002(6) -0.017(6) C15 0.073(7) 0.072(7) 0.071(7) -0.008(6) -0.002(6) -0.016(6) N4 0.078(7) 0.080(6) 0.068(6) -0.009(6) -0.009(6) -0.027(6) C16 0.075(7) 0.077(7) 0.073(7) -0.009(6) -0.008(6) -0.027(6) C17 0.074(7) 0.080(7) 0.065(7) -0.002(6) -0.001(6) -0.025(6) C18 0.077(7) 0.080(7) 0.070(7) -0.013(6) -0.005(6) -0.024(6) C19 0.080(7) 0.079(7) 0.076(7) -0.006(6) -0.007(6) -0.023(6) C20 0.076(7) 0.080(7) 0.073(7) -0.004(6) -0.012(6) -0.027(6) N5 0.034(8) 0.045(7) 0.046(7) 0.003(6) -0.008(6) -0.021(6) C21 0.036(8) 0.041(7) 0.051(8) 0.002(6) -0.007(6) -0.021(6) C22 0.036(8) 0.050(8) 0.044(8) 0.003(6) -0.013(6) -0.017(6) C23 0.040(8) 0.046(8) 0.048(8) 0.001(6) -0.011(6) -0.019(6) C24 0.037(8) 0.041(8) 0.047(8) 0.002(6) -0.010(6) -0.018(6) C25 0.036(8) 0.044(7) 0.047(8) 0.008(6) -0.008(6) -0.017(6) N6 0.088(7) 0.094(7) 0.084(7) -0.004(6) -0.007(6) -0.025(6) C26 0.085(7) 0.087(7) 0.082(7) -0.004(6) -0.005(6) -0.030(6) C27 0.090(7) 0.092(7) 0.083(7) -0.006(6) -0.010(6) -0.027(6) C28 0.095(8) 0.088(7) 0.090(7) -0.004(6) -0.009(6) -0.027(6) C29 0.089(7) 0.085(7) 0.093(7) 0.000(6) -0.009(6) -0.031(6) C30 0.091(7) 0.094(7) 0.090(7) -0.003(6) -0.009(6) -0.025(6) N7 0.085(7) 0.087(7) 0.090(7) -0.004(6) -0.012(6) -0.023(6) C31 0.084(8) 0.083(7) 0.087(7) -0.011(6) -0.008(6) -0.023(6) C32 0.082(8) 0.087(7) 0.083(7) -0.008(6) -0.003(6) -0.017(6) C33 0.085(8) 0.091(7) 0.088(7) 0.001(6) 0.002(6) -0.019(6) C34 0.085(8) 0.087(7) 0.092(7) 0.001(6) -0.003(6) -0.018(6) C35 0.081(7) 0.080(7) 0.090(7) -0.004(6) -0.010(6) -0.024(6) N8 0.039(7) 0.034(7) 0.045(7) -0.004(6) 0.000(6) -0.015(6) C36 0.049(7) 0.046(6) 0.063(7) -0.004(6) 0.001(6) -0.016(6) C37 0.045(8) 0.042(7) 0.051(7) -0.005(6) 0.002(6) -0.021(6) C38 0.058(7) 0.062(7) 0.058(7) 0.001(6) 0.003(6) -0.005(6) C39 0.058(7) 0.059(7) 0.070(7) -0.005(6) 0.002(6) -0.012(6) C40 0.040(8) 0.038(7) 0.042(7) -0.007(6) -0.003(6) -0.011(6) N9 0.079(7) 0.082(6) 0.078(6) -0.010(6) -0.008(6) -0.025(6) C41 0.075(7) 0.075(7) 0.071(7) -0.011(6) -0.008(6) -0.026(6) C42 0.070(7) 0.071(7) 0.062(7) -0.010(6) -0.007(6) -0.022(6) C43 0.071(7) 0.066(7) 0.062(7) -0.017(6) -0.009(6) -0.019(6) C44 0.067(7) 0.058(6) 0.064(7) -0.014(6) -0.006(6) -0.024(6) C45 0.073(7) 0.067(7) 0.070(7) -0.011(6) -0.006(6) -0.026(6) N10 0.058(7) 0.061(6) 0.057(6) -0.005(5) -0.007(5) -0.022(5) C46 0.059(7) 0.061(6) 0.053(6) -0.010(5) -0.003(6) -0.019(6) C47 0.058(7) 0.058(6) 0.055(6) -0.003(6) -0.005(6) -0.013(6) C48 0.051(7) 0.050(6) 0.048(6) -0.003(5) -0.006(6) -0.018(5) C49 0.054(7) 0.054(6) 0.045(6) -0.004(5) -0.010(6) -0.017(6) C50 0.052(7) 0.051(6) 0.048(6) -0.008(5) -0.009(6) -0.016(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 U1 O4B 2.199(10) 2_665 ? U1 O3A 2.296(10) . ? U1 O2A 2.351(11) . ? U1 O1B 2.379(10) . ? U1 O3B 2.419(11) 2_665 ? U1 N1A 2.523(13) . ? U1 N2A 2.534(13) . ? U1 Cl1A 2.692(5) . ? U1 U2 3.7940(10) . ? U2 O4A 2.229(11) . ? U2 O1A 2.280(10) . ? U2 O2B 2.395(10) . ? U2 O2A 2.464(8) . ? U2 O1B 2.488(11) . ? U2 O3A 2.519(12) . ? U2 Cl2A 2.714(4) . ? U2 Cl3A 2.731(4) . ? O1A C1A 1.383(15) . ? O1A O2A 2.603(14) . ? O2A C2A 1.299(17) . ? O2A O3A 2.480(16) . ? O2A N1A 2.738(14) . ? O3A C17A 1.351(18) . ? O3A O4A 2.559(13) . ? O3A N2A 2.792(16) . ? O4A C18A 1.369(19) . ? N1A C7A 1.33(2) . ? N1A C8A 1.502(18) . ? N1A N2A 3.03(2) . ? N2A C15A 1.287(19) . ? N2A C14A 1.429(18) . ? C1A C6A 1.40(2) . ? C1A C2A 1.42(2) . ? C2A C3A 1.412(17) . ? C3A C4A 1.43(2) . ? C3A C7A 1.44(2) . ? C4A C5A 1.40(2) . ? C5A C6A 1.430(18) . ? C8A C9A 1.53(2) . ? C9A C14A 1.34(2) . ? C9A C10A 1.38(2) . ? C10A C11A 1.33(2) . ? C11A C12A 1.36(2) . ? C12A C13A 1.45(2) . ? C13A C14A 1.41(2) . ? C15A C16A 1.44(2) . ? C16A C17A 1.38(2) . ? C16A C21A 1.40(2) . ? C17A C18A 1.37(2) . ? C18A C19A 1.39(2) . ? C19A C20A 1.36(2) . ? C20A C21A 1.355(19) . ? O1B C1B 1.346(16) . ? O2B C2B 1.301(17) . ? O3B C17B 1.284(17) . ? O3B U1 2.419(11) 2_665 ? O4B C18B 1.362(18) . ? O4B U1 2.199(10) 2_665 ? N1B C7B 1.314(18) . ? N1B C8B 1.480(16) . ? N2B C15B 1.268(16) . ? N2B C14B 1.46(2) . ? C1B C6B 1.39(2) . ? C1B C2B 1.419(19) . ? C2B C3B 1.41(2) . ? C3B C4B 1.42(2) . ? C3B C7B 1.458(18) . ? C4B C5B 1.344(19) . ? C5B C6B 1.418(19) . ? C8B C9B 1.51(2) . ? C9B C10B 1.37(2) . ? C9B C14B 1.430(18) . ? C10B C11B 1.39(2) . ? C11B C12B 1.406(19) . ? C12B C13B 1.35(2) . ? C13B C14B 1.40(2) . ? C15B C16B 1.43(2) . ? C16B C17B 1.35(2) . ? C16B C21B 1.47(2) . ? C17B C18B 1.44(2) . ? C18B C19B 1.42(2) . ? C19B C20B 1.43(2) . ? C20B C21B 1.36(2) . ? U3 O4D 2.195(11) . ? U3 O3C 2.303(10) . ? U3 O2C 2.337(12) . ? U3 O1D 2.391(10) 2_666 ? U3 O3D 2.427(11) . ? U3 N2C 2.558(15) . ? U3 N1C 2.583(14) . ? U3 Cl1C 2.686(5) . ? U3 U4 3.7618(11) . ? U4 O4C 2.258(11) . ? U4 O1C 2.288(11) . ? U4 O2D 2.375(10) 2_666 ? U4 O1D 2.432(11) 2_666 ? U4 O2C 2.456(9) . ? U4 O3C 2.531(12) . ? U4 N1 2.639(13) . ? U4 Cl2C 2.722(5) . ? O1C C1C 1.340(16) . ? O1C O2C 2.619(16) . ? O2C C2C 1.329(19) . ? O2C O3C 2.400(17) . ? O2C N1C 2.700(16) . ? O3C C17C 1.374(19) . ? O3C O4C 2.577(13) . ? O3C N2C 2.800(17) . ? O4C C18C 1.338(19) . ? N1C C7C 1.25(2) . ? N1C C8C 1.50(2) . ? N1C N2C 3.09(2) . ? N2C C15C 1.270(19) . ? N2C C14C 1.444(18) . ? C1C C2C 1.35(2) . ? C1C C6C 1.40(2) . ? C2C C3C 1.49(2) . ? C3C C4C 1.40(2) . ? C3C C7C 1.49(2) . ? C4C C5C 1.42(2) . ? C5C C6C 1.409(19) . ? C8C C9C 1.42(2) . ? C9C C14C 1.35(2) . ? C9C C10C 1.38(2) . ? C10C C11C 1.36(3) . ? C11C C12C 1.33(2) . ? C12C C13C 1.41(2) . ? C13C C14C 1.41(2) . ? C15C C16C 1.48(2) . ? C16C C17C 1.37(2) . ? C16C C21C 1.45(2) . ? C17C C18C 1.42(2) . ? C18C C19C 1.40(2) . ? C19C C20C 1.35(2) . ? C20C C21C 1.387(19) . ? O1D C1D 1.388(18) . ? O1D U3 2.391(10) 2_666 ? O1D U4 2.432(11) 2_666 ? O2D C2D 1.382(19) . ? O2D U4 2.375(10) 2_666 ? O3D C17D 1.328(16) . ? O4D C18D 1.307(16) . ? N1D C7D 1.283(19) . ? N1D C8D 1.471(17) . ? N2D C15D 1.344(18) . ? N2D C14D 1.43(2) . ? C1D C6D 1.36(2) . ? C1D C2D 1.40(2) . ? C2D C3D 1.37(2) . ? C3D C4D 1.40(2) . ? C3D C7D 1.44(2) . ? C4D C5D 1.37(2) . ? C5D C6D 1.385(19) . ? C8D C9D 1.51(2) . ? C9D C10D 1.30(2) . ? C9D C14D 1.46(2) . ? C10D C11D 1.40(2) . ? C11D C12D 1.39(2) . ? C12D C13D 1.31(2) . ? C13D C14D 1.43(2) . ? C15D C16D 1.38(2) . ? C16D C17D 1.37(2) . ? C16D C21D 1.40(2) . ? C17D C18D 1.43(2) . ? C18D C19D 1.374(19) . ? C19D C20D 1.44(2) . ? C20D C21D 1.38(2) . ? N1 C1 1.25(2) . ? N1 C5 1.30(2) . ? C1 C2 1.45(2) . ? C2 C3 1.42(2) . ? C3 C4 1.33(2) . ? C4 C5 1.43(2) . ? N2 C10 1.32(2) . ? N2 C6 1.42(2) . ? N2 N3 2.65(3) . ? C6 C7 1.41(3) . ? C7 C8 1.27(2) . ? C8 C9 1.37(2) . ? C9 C10 1.38(3) . ? N3 C15 1.27(2) . ? N3 C11 1.36(2) . ? C11 C12 1.39(3) . ? C12 C13 1.28(3) . ? C13 C14 1.36(2) . ? C14 C15 1.42(3) . ? N4 C20 1.33(2) . ? N4 C16 1.41(2) . ? C16 C17 1.32(2) . ? C17 C18 1.38(2) . ? C18 C19 1.40(3) . ? C19 C20 1.32(2) . ? N5 C21 1.3900 . ? N5 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? N6 C26 1.3900 . ? N6 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? N7 C31 1.29(3) . ? N7 C35 1.44(2) . ? C31 C32 1.25(3) . ? C32 C33 1.33(3) . ? C33 C34 1.30(3) . ? C34 C35 1.40(3) . ? N8 C40 1.33(3) . ? N8 C36 1.41(3) . ? C36 C37 1.30(3) . ? C37 C38 1.24(3) . ? C38 C39 1.33(2) . ? C39 C40 1.30(3) . ? N9 C41 1.38(2) . ? N9 C45 1.39(2) . ? C41 C42 1.33(3) . ? C42 C43 1.34(2) . ? C43 C44 1.38(3) . ? C44 C45 1.33(2) . ? N10 C46 1.291(18) . ? N10 C50 1.38(2) . ? C46 C47 1.40(3) . ? C47 C48 1.38(2) . ? C48 C49 1.320(19) . ? C49 C50 1.31(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4B U1 O3A 160.4(4) 2_665 . ? O4B U1 O2A 130.4(4) 2_665 . ? O3A U1 O2A 64.5(4) . . ? O4B U1 O1B 126.1(4) 2_665 . ? O3A U1 O1B 68.5(3) . . ? O2A U1 O1B 68.2(3) . . ? O4B U1 O3B 66.7(4) 2_665 2_665 ? O3A U1 O3B 132.9(4) . 2_665 ? O2A U1 O3B 76.3(4) . 2_665 ? O1B U1 O3B 73.5(3) . 2_665 ? O4B U1 N1A 74.9(4) 2_665 . ? O3A U1 N1A 104.9(4) . . ? O2A U1 N1A 68.3(4) . . ? O1B U1 N1A 133.9(4) . . ? O3B U1 N1A 82.3(4) 2_665 . ? O4B U1 N2A 91.1(4) 2_665 . ? O3A U1 N2A 70.4(4) . . ? O2A U1 N2A 108.4(4) . . ? O1B U1 N2A 135.3(4) . . ? O3B U1 N2A 151.0(4) 2_665 . ? N1A U1 N2A 73.7(4) . . ? O4B U1 Cl1A 81.0(3) 2_665 . ? O3A U1 Cl1A 89.2(3) . . ? O2A U1 Cl1A 145.7(2) . . ? O1B U1 Cl1A 82.1(3) . . ? O3B U1 Cl1A 112.4(3) 2_665 . ? N1A U1 Cl1A 143.8(3) . . ? N2A U1 Cl1A 80.4(4) . . ? O4A U2 O1A 165.6(4) . . ? O4A U2 O2B 96.0(4) . . ? O1A U2 O2B 86.9(3) . . ? O4A U2 O2A 122.7(3) . . ? O1A U2 O2A 66.4(3) . . ? O2B U2 O2A 120.8(3) . . ? O4A U2 O1B 102.7(4) . . ? O1A U2 O1B 91.2(4) . . ? O2B U2 O1B 64.1(3) . . ? O2A U2 O1B 64.8(3) . . ? O4A U2 O3A 64.9(3) . . ? O1A U2 O3A 126.0(3) . . ? O2B U2 O3A 117.0(4) . . ? O2A U2 O3A 59.7(3) . . ? O1B U2 O3A 63.4(3) . . ? O4A U2 Cl2A 81.5(3) . . ? O1A U2 Cl2A 89.6(3) . . ? O2B U2 Cl2A 153.6(3) . . ? O2A U2 Cl2A 81.1(2) . . ? O1B U2 Cl2A 142.2(2) . . ? O3A U2 Cl2A 85.9(3) . . ? O4A U2 Cl3A 84.1(3) . . ? O1A U2 Cl3A 83.6(3) . . ? O2B U2 Cl3A 70.7(2) . . ? O2A U2 Cl3A 145.9(3) . . ? O1B U2 Cl3A 134.8(2) . . ? O3A U2 Cl3A 148.3(2) . . ? Cl2A U2 Cl3A 82.90(13) . . ? C7A N1A C8A 115.3(14) . . ? C15A N2A C14A 121.9(15) . . ? O1A C1A C6A 124.8(15) . . ? O1A C1A C2A 114.7(15) . . ? C6A C1A C2A 120.4(14) . . ? O2A C2A C3A 122.6(15) . . ? O2A C2A C1A 117.6(12) . . ? C3A C2A C1A 119.7(16) . . ? C2A C3A C4A 119.5(16) . . ? C2A C3A C7A 120.6(16) . . ? C4A C3A C7A 119.2(15) . . ? C5A C4A C3A 120.6(16) . . ? C4A C5A C6A 119.0(16) . . ? C1A C6A C5A 120.4(16) . . ? N1A C7A C3A 124.7(16) . . ? N1A C8A C9A 115.8(14) . . ? C14A C9A C10A 121.2(19) . . ? C14A C9A C8A 119.6(16) . . ? C10A C9A C8A 119.2(15) . . ? C11A C10A C9A 121.1(17) . . ? C10A C11A C12A 121.1(19) . . ? C11A C12A C13A 119(2) . . ? C14A C13A C12A 117.2(18) . . ? C9A C14A C13A 120.1(17) . . ? C9A C14A N2A 123.7(19) . . ? C13A C14A N2A 115.4(16) . . ? N2A C15A C16A 127.4(18) . . ? C17A C16A C21A 115.6(15) . . ? C17A C16A C15A 124.3(16) . . ? C21A C16A C15A 120.0(17) . . ? O3A C17A C18A 115.5(16) . . ? O3A C17A C16A 121.1(14) . . ? C18A C17A C16A 123.4(17) . . ? O4A C18A C17A 116.3(16) . . ? O4A C18A C19A 126.3(15) . . ? C17A C18A C19A 117.3(17) . . ? C20A C19A C18A 121.9(16) . . ? C21A C20A C19A 118.5(17) . . ? C20A C21A C16A 123.2(17) . . ? C7B N1B C8B 124.7(13) . . ? C15B N2B C14B 117.4(14) . . ? O1B C1B C6B 123.2(14) . . ? O1B C1B C2B 115.6(15) . . ? C6B C1B C2B 121.1(15) . . ? O2B C2B C3B 124.7(13) . . ? O2B C2B C1B 117.0(14) . . ? C3B C2B C1B 118.3(15) . . ? C2B C3B C4B 120.9(13) . . ? C2B C3B C7B 118.9(15) . . ? C4B C3B C7B 120.1(15) . . ? C5B C4B C3B 118.2(16) . . ? C4B C5B C6B 123.7(17) . . ? C1B C6B C5B 117.7(15) . . ? N1B C7B C3B 123.1(14) . . ? N1B C8B C9B 110.7(14) . . ? C10B C9B C14B 120.5(15) . . ? C10B C9B C8B 121.1(13) . . ? C14B C9B C8B 118.4(15) . . ? C9B C10B C11B 120.0(15) . . ? C10B C11B C12B 120.5(19) . . ? C13B C12B C11B 118.2(18) . . ? C12B C13B C14B 124.1(14) . . ? C13B C14B C9B 116.4(16) . . ? C13B C14B N2B 124.4(13) . . ? C9B C14B N2B 119.2(14) . . ? N2B C15B C16B 120.2(16) . . ? C17B C16B C15B 122.3(16) . . ? C17B C16B C21B 118.3(19) . . ? C15B C16B C21B 119.1(17) . . ? O3B C17B C16B 126.8(19) . . ? O3B C17B C18B 113.3(16) . . ? C16B C17B C18B 119.7(17) . . ? O4B C18B C19B 121.9(18) . . ? O4B C18B C17B 116.0(14) . . ? C19B C18B C17B 122.1(17) . . ? C18B C19B C20B 117.2(18) . . ? C21B C20B C19B 119.7(18) . . ? C20B C21B C16B 122.8(19) . . ? O4D U3 O3C 153.7(4) . . ? O4D U3 O2C 133.1(4) . . ? O3C U3 O2C 62.3(4) . . ? O4D U3 O1D 131.4(4) . 2_666 ? O3C U3 O1D 71.2(4) . 2_666 ? O2C U3 O1D 68.2(4) . 2_666 ? O4D U3 O3D 67.0(4) . . ? O3C U3 O3D 139.1(4) . . ? O2C U3 O3D 84.3(4) . . ? O1D U3 O3D 75.0(3) 2_666 . ? O4D U3 N2C 83.8(4) . . ? O3C U3 N2C 70.1(4) . . ? O2C U3 N2C 108.7(4) . . ? O1D U3 N2C 136.8(4) 2_666 . ? O3D U3 N2C 148.0(4) . . ? O4D U3 N1C 75.0(4) . . ? O3C U3 N1C 100.1(4) . . ? O2C U3 N1C 66.3(4) . . ? O1D U3 N1C 131.9(5) 2_666 . ? O3D U3 N1C 85.8(4) . . ? N2C U3 N1C 73.9(5) . . ? O4D U3 Cl1C 84.2(3) . . ? O3C U3 Cl1C 88.1(3) . . ? O2C U3 Cl1C 141.4(2) . . ? O1D U3 Cl1C 79.5(3) 2_666 . ? O3D U3 Cl1C 107.7(3) . . ? N2C U3 Cl1C 80.7(4) . . ? N1C U3 Cl1C 148.6(4) . . ? O4C U4 O1C 166.8(4) . . ? O4C U4 O2D 95.6(4) . 2_666 ? O1C U4 O2D 87.5(4) . 2_666 ? O4C U4 O1D 105.3(4) . 2_666 ? O1C U4 O1D 87.7(4) . 2_666 ? O2D U4 O1D 66.3(4) 2_666 2_666 ? O4C U4 O2C 120.3(4) . . ? O1C U4 O2C 66.9(4) . . ? O2D U4 O2C 125.7(3) 2_666 . ? O1D U4 O2C 65.7(3) 2_666 . ? O4C U4 O3C 64.8(4) . . ? O1C U4 O3C 124.2(3) . . ? O2D U4 O3C 120.7(4) 2_666 . ? O1D U4 O3C 66.8(4) 2_666 . ? O2C U4 O3C 57.5(4) . . ? O4C U4 N1 82.2(4) . . ? O1C U4 N1 89.2(4) . . ? O2D U4 N1 152.5(4) 2_666 . ? O1D U4 N1 140.9(4) 2_666 . ? O2C U4 N1 77.3(4) . . ? O3C U4 N1 83.3(4) . . ? O4C U4 Cl2C 88.4(3) . . ? O1C U4 Cl2C 79.9(3) . . ? O2D U4 Cl2C 74.6(3) 2_666 . ? O1D U4 Cl2C 139.4(3) 2_666 . ? O2C U4 Cl2C 138.4(3) . . ? O3C U4 Cl2C 149.2(2) . . ? N1 U4 Cl2C 77.9(3) . . ? C7C N1C C8C 119.9(17) . . ? C15C N2C C14C 121.8(17) . . ? O1C C1C C2C 116.4(17) . . ? O1C C1C C6C 122.3(17) . . ? C2C C1C C6C 120.9(16) . . ? O2C C2C C1C 120.1(15) . . ? O2C C2C C3C 121.1(17) . . ? C1C C2C C3C 118.6(18) . . ? C4C C3C C2C 118.4(18) . . ? C4C C3C C7C 127.0(16) . . ? C2C C3C C7C 114.6(17) . . ? C3C C4C C5C 122.2(18) . . ? C6C C5C C4C 116.7(19) . . ? C1C C6C C5C 122.6(18) . . ? N1C C7C C3C 128.9(18) . . ? C9C C8C N1C 116.4(16) . . ? C14C C9C C10C 116.7(19) . . ? C14C C9C C8C 120.9(16) . . ? C10C C9C C8C 122.4(16) . . ? C11C C10C C9C 123.0(19) . . ? C12C C11C C10C 120.0(18) . . ? C11C C12C C13C 121(2) . . ? C12C C13C C14C 116.9(19) . . ? C9C C14C C13C 122.5(16) . . ? C9C C14C N2C 122.1(18) . . ? C13C C14C N2C 115.2(16) . . ? N2C C15C C16C 125.9(19) . . ? C17C C16C C21C 118.2(16) . . ? C17C C16C C15C 124.1(17) . . ? C21C C16C C15C 117.8(17) . . ? C16C C17C O3C 122.1(15) . . ? C16C C17C C18C 123.4(18) . . ? O3C C17C C18C 114.5(17) . . ? O4C C18C C19C 128.3(15) . . ? O4C C18C C17C 116.2(16) . . ? C19C C18C C17C 115.1(18) . . ? C20C C19C C18C 123.8(17) . . ? C19C C20C C21C 120.4(19) . . ? C20C C21C C16C 118.7(18) . . ? C7D N1D C8D 120.4(14) . . ? C15D N2D C14D 122.2(14) . . ? C6D C1D O1D 124.5(16) . . ? C6D C1D C2D 119.7(17) . . ? O1D C1D C2D 115.8(16) . . ? C3D C2D O2D 119.8(15) . . ? C3D C2D C1D 122.9(18) . . ? O2D C2D C1D 117.0(15) . . ? C2D C3D C4D 115.8(17) . . ? C2D C3D C7D 122.6(17) . . ? C4D C3D C7D 121.6(16) . . ? C5D C4D C3D 122.0(16) . . ? C4D C5D C6D 120.4(17) . . ? C1D C6D C5D 119.0(17) . . ? N1D C7D C3D 122.2(16) . . ? N1D C8D C9D 110.1(15) . . ? C10D C9D C14D 119.2(17) . . ? C10D C9D C8D 123.0(15) . . ? C14D C9D C8D 117.5(17) . . ? C9D C10D C11D 122.1(17) . . ? C12D C11D C10D 119(2) . . ? C13D C12D C11D 123(2) . . ? C12D C13D C14D 118.4(17) . . ? N2D C14D C13D 120.5(14) . . ? N2D C14D C9D 121.0(15) . . ? C13D C14D C9D 118.4(18) . . ? N2D C15D C16D 124.3(16) . . ? C17D C16D C15D 122.5(16) . . ? C17D C16D C21D 119.3(17) . . ? C15D C16D C21D 117.5(16) . . ? O3D C17D C16D 123.1(17) . . ? O3D C17D C18D 115.2(14) . . ? C16D C17D C18D 121.7(15) . . ? O4D C18D C19D 125.4(17) . . ? O4D C18D C17D 115.5(14) . . ? C19D C18D C17D 119.2(15) . . ? C18D C19D C20D 118.7(17) . . ? C21D C20D C19D 120.9(17) . . ? C20D C21D C16D 119.9(17) . . ? C1 N1 C5 120.2(18) . . ? N1 C1 C2 123(2) . . ? C3 C2 C1 116(2) . . ? C4 C3 C2 120(2) . . ? C3 C4 C5 117(2) . . ? N1 C5 C4 123(2) . . ? C10 N2 C6 116.4(19) . . ? C10 N2 N3 126.3(14) . . ? C6 N2 N3 117.0(14) . . ? C7 C6 N2 121(2) . . ? C8 C7 C6 118(2) . . ? C7 C8 C9 125(2) . . ? C8 C9 C10 116(2) . . ? N2 C10 C9 124(2) . . ? C15 N3 C11 117(2) . . ? C15 N3 N2 117.0(16) . . ? C11 N3 N2 125.9(17) . . ? N3 C11 C12 120(2) . . ? C13 C12 C11 121(2) . . ? C12 C13 C14 122(2) . . ? C13 C14 C15 114(2) . . ? N3 C15 C14 126(2) . . ? C20 N4 C16 117.2(19) . . ? C17 C16 N4 118(2) . . ? C16 C17 C18 125(2) . . ? C17 C18 C19 115(2) . . ? C20 C19 C18 119(2) . . ? C19 C20 N4 125(2) . . ? C21 N5 C25 120.0 . . ? N5 C21 C22 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C24 C25 N5 120.0 . . ? C26 N6 C30 120.0 . . ? N6 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 N6 120.0 . . ? C31 N7 C35 114(2) . . ? C32 C31 N7 128(3) . . ? C31 C32 C33 114(3) . . ? C34 C33 C32 131(3) . . ? C33 C34 C35 110(3) . . ? C34 C35 N7 121(3) . . ? C40 N8 C36 106(3) . . ? C37 C36 N8 128(2) . . ? C38 C37 C36 123(3) . . ? C37 C38 C39 113(3) . . ? C40 C39 C38 127(3) . . ? C39 C40 N8 123(3) . . ? C41 N9 C45 118.0(19) . . ? C42 C41 N9 119(2) . . ? C41 C42 C43 122(2) . . ? C42 C43 C44 122(2) . . ? C45 C44 C43 116(2) . . ? C44 C45 N9 123(2) . . ? C46 N10 C50 113.3(19) . . ? N10 C46 C47 126(2) . . ? C48 C47 C46 115.9(19) . . ? C49 C48 C47 118(2) . . ? C50 C49 C48 121(2) . . ? C49 C50 N10 123.7(19) . . ? #===END data_8.6py _database_code_depnum_ccdc_archive 'CCDC 250670' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H126 Cl10 N20 O16 U6' _chemical_formula_weight 4031.21 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 '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 42.8614(16) _cell_length_b 10.6024(4) _cell_length_c 29.6703(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.342(2) _cell_angle_gamma 90.00 _cell_volume 13471.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 45361 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method ? _exptl_crystal_F_000 7632 _exptl_absorpt_coefficient_mu 7.455 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.201 _exptl_absorpt_correction_T_max 0.551 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 45361 _diffrn_reflns_av_R_equivalents 0.1191 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12714 _reflns_number_gt 8047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. One pyridine molecule is disordered over two positions which have been refined as idealized hexagons with occupancy parameters fixed to 0.5. All non-hydrogen atoms were refined with anisotropic displacement parameters, with some restraints on displacement parameters for some badly behaving atoms, particularly in the disordered molecules. The H atom bound to N in the pyridinium ion was found on a Fourier-difference map and all the other ones were introduced at calculated positions, except in the disordered pyridine molecules. All H atoms were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (NH, CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+52.7644P] 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 12714 _refine_ls_number_parameters 857 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _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 1.120 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.183 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 0.193993(9) 0.46536(3) 0.833544(11) 0.03057(10) Uani 1 1 d . . . U2 U 0.110857(9) 0.53850(3) 0.851621(11) 0.02867(10) Uani 1 1 d . . . U3 U 0.074764(9) 0.51032(3) 0.963733(11) 0.03134(10) Uani 1 1 d . . . Cl1 Cl 0.20817(6) 0.4061(2) 0.92069(8) 0.0365(6) Uani 1 1 d . . . Cl2 Cl 0.25255(6) 0.3666(2) 0.83034(8) 0.0404(6) Uani 1 1 d . . . Cl3 Cl 0.18509(7) 0.2826(3) 0.77217(9) 0.0492(7) Uani 1 1 d . . . Cl4 Cl 0.11983(6) 0.4811(2) 1.02712(8) 0.0371(6) Uani 1 1 d . . . Cl5 Cl 0.06220(7) 0.7469(3) 0.98928(9) 0.0466(7) Uani 1 1 d . . . O1A O 0.11689(17) 0.6200(6) 0.9275(2) 0.0364(17) Uani 1 1 d . . . O2A O 0.16383(15) 0.6035(5) 0.8738(2) 0.0310(16) Uani 1 1 d . . . O3A O 0.15051(15) 0.5444(6) 0.7939(2) 0.0354(16) Uani 1 1 d . . . O4A O 0.09164(16) 0.5929(6) 0.7828(2) 0.0351(17) Uani 1 1 d . . . N1A N 0.2236(2) 0.6718(8) 0.8518(3) 0.038(2) Uani 1 1 d . . . N2A N 0.2106(2) 0.6032(7) 0.7682(3) 0.038(2) Uani 1 1 d . . . C1A C 0.1439(2) 0.6801(9) 0.9410(3) 0.031(2) Uani 1 1 d . . . C2A C 0.1688(2) 0.6711(8) 0.9120(3) 0.031(2) Uani 1 1 d . . . C3A C 0.1974(3) 0.7309(9) 0.9219(3) 0.036(3) Uani 1 1 d . . . C4A C 0.2002(3) 0.8031(9) 0.9623(3) 0.037(3) Uani 1 1 d . . . H4A H 0.2187 0.8460 0.9692 0.045 Uiso 1 1 calc R . . C5A C 0.1763(3) 0.8108(9) 0.9909(3) 0.039(3) Uani 1 1 d . . . H5A H 0.1789 0.8561 1.0176 0.046 Uiso 1 1 calc R . . C6A C 0.1478(2) 0.7511(9) 0.9804(3) 0.032(2) Uani 1 1 d . . . H6A H 0.1314 0.7587 0.9998 0.038 Uiso 1 1 calc R . . C7A C 0.2215(3) 0.7365(9) 0.8886(3) 0.037(3) Uani 1 1 d . . . H7A H 0.2375 0.7941 0.8946 0.044 Uiso 1 1 calc R . . C8A C 0.2469(3) 0.7201(10) 0.8179(4) 0.044(3) Uani 1 1 d . . . C9A C 0.2434(3) 0.6375(10) 0.7762(3) 0.043(3) Uani 1 1 d . . . H9A1 H 0.2508 0.6826 0.7502 0.051 Uiso 1 1 calc R . . H9A2 H 0.2559 0.5618 0.7803 0.051 Uiso 1 1 calc R . . C10A C 0.1954(3) 0.6436(10) 0.7330(3) 0.042(3) Uani 1 1 d . . . H10A H 0.2073 0.6828 0.7117 0.051 Uiso 1 1 calc R . . C11A C 0.1628(3) 0.6370(9) 0.7221(3) 0.038(3) Uani 1 1 d . . . C12A C 0.1419(3) 0.5956(9) 0.7542(3) 0.038(3) Uani 1 1 d . . . C13A C 0.1094(3) 0.6207(9) 0.7480(3) 0.037(3) Uani 1 1 d . . . C14A C 0.0986(3) 0.6716(12) 0.7076(4) 0.061(3) Uani 1 1 d U . . H14A H 0.0773 0.6839 0.7021 0.073 Uiso 1 1 calc R . . C15A C 0.1197(3) 0.7045(13) 0.6750(4) 0.069(4) Uani 1 1 d U . . H15A H 0.1121 0.7355 0.6474 0.083 Uiso 1 1 calc R . . C16A C 0.1510(3) 0.6924(11) 0.6827(4) 0.055(3) Uani 1 1 d . . . H16A H 0.1646 0.7215 0.6613 0.066 Uiso 1 1 calc R . . C17A C 0.2802(3) 0.7090(11) 0.8377(4) 0.050(3) Uani 1 1 d . . . H17A H 0.2845 0.6227 0.8455 0.075 Uiso 1 1 calc R . . H17B H 0.2824 0.7605 0.8643 0.075 Uiso 1 1 calc R . . H17C H 0.2946 0.7370 0.8159 0.075 Uiso 1 1 calc R . . C18A C 0.2382(3) 0.8550(9) 0.8039(3) 0.044(3) Uani 1 1 d . . . H18A H 0.2423 0.9110 0.8288 0.066 Uiso 1 1 calc R . . H18B H 0.2164 0.8584 0.7949 0.066 Uiso 1 1 calc R . . H18C H 0.2505 0.8802 0.7790 0.066 Uiso 1 1 calc R . . O1B O 0.14695(15) 0.3669(5) 0.8567(2) 0.0277(15) Uani 1 1 d . . . O2B O 0.09921(16) 0.3821(5) 0.91047(19) 0.0291(16) Uani 1 1 d . . . O3B O -0.02637(14) 0.5161(6) 1.05865(18) 0.0381(17) Uani 1 1 d . . . O4B O -0.06257(15) 0.4260(6) 1.11911(19) 0.0326(16) Uani 1 1 d . . . N1B N 0.06801(19) 0.2697(8) 0.9847(2) 0.031(2) Uani 1 1 d . . . N2B N 0.04247(18) 0.4665(8) 1.0347(2) 0.0351(19) Uani 1 1 d . . . C1B C 0.1416(2) 0.2671(8) 0.8833(3) 0.032(2) Uani 1 1 d . . . C2B C 0.1160(2) 0.2751(8) 0.9124(3) 0.030(2) Uani 1 1 d . . . C3B C 0.1088(2) 0.1757(9) 0.9400(3) 0.038(3) Uani 1 1 d . . . C4B C 0.1274(3) 0.0661(9) 0.9384(4) 0.045(3) Uani 1 1 d . . . H4B H 0.1226 -0.0021 0.9565 0.054 Uiso 1 1 calc R . . C5B C 0.1523(3) 0.0564(9) 0.9111(3) 0.042(3) Uani 1 1 d . . . H5B H 0.1643 -0.0168 0.9108 0.051 Uiso 1 1 calc R . . C6B C 0.1593(2) 0.1587(8) 0.8839(3) 0.034(2) Uani 1 1 d . . . H6B H 0.1764 0.1538 0.8657 0.041 Uiso 1 1 calc R . . C7B C 0.0844(2) 0.1773(10) 0.9719(3) 0.039(3) Uani 1 1 d . . . H7B H 0.0800 0.0999 0.9850 0.047 Uiso 1 1 calc R . . C8B C 0.0468(2) 0.2393(9) 1.0233(3) 0.035(2) Uani 1 1 d . . . C9B C 0.0244(2) 0.3519(10) 1.0284(3) 0.039(3) Uani 1 1 d . . . H9B1 H 0.0108 0.3593 1.0016 0.046 Uiso 1 1 calc R . . H9B2 H 0.0116 0.3384 1.0541 0.046 Uiso 1 1 calc R . . C10B C 0.0401(2) 0.5328(10) 1.0708(3) 0.038(2) Uani 1 1 d . . . H10B H 0.0527 0.6039 1.0736 0.045 Uiso 1 1 calc R . . C11B C 0.0190(2) 0.5068(10) 1.1083(3) 0.039(3) Uani 1 1 d . . . C12B C -0.0131(2) 0.4895(10) 1.0989(3) 0.041(3) Uani 1 1 d . . . C13B C -0.0322(2) 0.4466(9) 1.1331(3) 0.035(2) Uani 1 1 d . . . C14B C -0.0200(3) 0.4278(11) 1.1762(3) 0.049(3) Uani 1 1 d . . . H14B H -0.0328 0.3993 1.1987 0.059 Uiso 1 1 calc R . . C15B C 0.0115(3) 0.4518(12) 1.1859(3) 0.059(4) Uani 1 1 d . . . H15B H 0.0194 0.4427 1.2154 0.071 Uiso 1 1 calc R . . C16B C 0.0312(3) 0.4886(10) 1.1530(3) 0.046(3) Uani 1 1 d . . . H16B H 0.0524 0.5015 1.1600 0.055 Uiso 1 1 calc R . . C17B C 0.0269(3) 0.1239(11) 1.0126(4) 0.062(4) Uani 1 1 d . . . H17D H 0.0101 0.1198 1.0331 0.092 Uiso 1 1 calc R . . H17E H 0.0395 0.0494 1.0157 0.092 Uiso 1 1 calc R . . H17F H 0.0184 0.1297 0.9822 0.092 Uiso 1 1 calc R . . C18B C 0.0676(3) 0.2217(10) 1.0662(3) 0.048(3) Uani 1 1 d . . . H18D H 0.0547 0.2123 1.0917 0.072 Uiso 1 1 calc R . . H18E H 0.0808 0.2940 1.0705 0.072 Uiso 1 1 calc R . . H18F H 0.0802 0.1476 1.0632 0.072 Uiso 1 1 calc R . . N1 N 0.1171(2) 0.7811(8) 0.8426(3) 0.049(3) Uani 1 1 d . . . C1 C 0.0928(4) 0.8504(12) 0.8514(5) 0.080(4) Uani 1 1 d U . . H1 H 0.0766 0.8149 0.8670 0.095 Uiso 1 1 calc R . . C2 C 0.0905(5) 0.9796(16) 0.8375(7) 0.112(6) Uani 1 1 d U . . H2 H 0.0745 1.0315 0.8467 0.134 Uiso 1 1 calc R . . C3 C 0.1128(5) 1.0225(16) 0.8102(6) 0.104(5) Uani 1 1 d U . . H3A H 0.1098 1.1012 0.7969 0.125 Uiso 1 1 calc R . . C4 C 0.1394(4) 0.9575(12) 0.8010(5) 0.077(4) Uani 1 1 d U . . H4 H 0.1556 0.9912 0.7850 0.093 Uiso 1 1 calc R . . C5 C 0.1395(3) 0.8340(10) 0.8185(3) 0.054(4) Uani 1 1 d . . . H5 H 0.1567 0.7842 0.8128 0.065 Uiso 1 1 calc R . . N2 N 0.0803(2) 0.3477(7) 0.8124(3) 0.036(2) Uani 1 1 d . . . C6 C 0.0552(3) 0.2928(10) 0.8296(4) 0.050(3) Uani 1 1 d . . . H6 H 0.0511 0.3049 0.8599 0.060 Uiso 1 1 calc R . . C7 C 0.0354(3) 0.2185(13) 0.8030(5) 0.076(4) Uani 1 1 d U . . H7 H 0.0179 0.1820 0.8152 0.091 Uiso 1 1 calc R . . C8 C 0.0417(4) 0.1983(14) 0.7573(5) 0.084(5) Uani 1 1 d U . . H8 H 0.0285 0.1481 0.7392 0.101 Uiso 1 1 calc R . . C9 C 0.0678(3) 0.2544(12) 0.7397(5) 0.071(4) Uani 1 1 d U . . H9 H 0.0726 0.2443 0.7096 0.085 Uiso 1 1 calc R . . C10 C 0.0863(3) 0.3260(9) 0.7690(4) 0.044(3) Uani 1 1 d . . . H10 H 0.1043 0.3617 0.7579 0.053 Uiso 1 1 calc R . . N3 N 0.2843(2) 0.3882(7) 0.9764(3) 0.036(2) Uani 1 1 d . . . H3 H 0.2673 0.3974 0.9959 0.043 Uiso 1 1 d R . . C11 C 0.2876(3) 0.4390(10) 0.9360(3) 0.043(3) Uani 1 1 d . . . H11 H 0.2718 0.4896 0.9234 0.051 Uiso 1 1 calc R . . C12 C 0.3136(3) 0.4179(10) 0.9129(4) 0.048(3) Uani 1 1 d . . . H12 H 0.3157 0.4532 0.8845 0.057 Uiso 1 1 calc R . . C13 C 0.3371(3) 0.3435(10) 0.9319(4) 0.053(3) Uani 1 1 d . . . H13 H 0.3553 0.3298 0.9167 0.064 Uiso 1 1 calc R . . C14 C 0.3333(3) 0.2910(11) 0.9726(4) 0.059(4) Uani 1 1 d . . . H14 H 0.3485 0.2381 0.9854 0.071 Uiso 1 1 calc R . . C15 C 0.3067(3) 0.3166(10) 0.9948(4) 0.045(3) Uani 1 1 d . . . H15 H 0.3043 0.2830 1.0234 0.055 Uiso 1 1 calc R . . N4 N 0.2391(2) 0.4399(7) 1.0362(3) 0.039(2) Uani 1 1 d . . . C16 C 0.2438(3) 0.3862(9) 1.0774(4) 0.043(3) Uani 1 1 d . . . H16 H 0.2608 0.3330 1.0829 0.052 Uiso 1 1 calc R . . C17 C 0.2232(3) 0.4103(10) 1.1120(4) 0.055(3) Uani 1 1 d . . . H17 H 0.2258 0.3688 1.1395 0.066 Uiso 1 1 calc R . . C18 C 0.1996(3) 0.4935(10) 1.1054(4) 0.055(3) Uani 1 1 d . . . H18 H 0.1866 0.5121 1.1287 0.066 Uiso 1 1 calc R . . C19 C 0.1951(3) 0.5488(10) 1.0654(4) 0.047(3) Uani 1 1 d . . . H19 H 0.1790 0.6066 1.0606 0.057 Uiso 1 1 calc R . . C20 C 0.2147(3) 0.5194(10) 1.0309(3) 0.047(3) Uani 1 1 d . . . H20 H 0.2108 0.5562 1.0028 0.056 Uiso 1 1 calc R . . N5 N 0.1154(3) 0.0384(12) 0.6252(4) 0.089(4) Uani 1 1 d . . . C21 C 0.1100(4) 0.1355(16) 0.5993(4) 0.081(5) Uani 1 1 d . . . H21 H 0.1004 0.1197 0.5712 0.097 Uiso 1 1 calc R . . C22 C 0.1169(3) 0.2573(15) 0.6091(5) 0.075(4) Uani 1 1 d U . . H22 H 0.1125 0.3220 0.5886 0.090 Uiso 1 1 calc R . . C23 C 0.1312(4) 0.2807(16) 0.6521(6) 0.099(5) Uani 1 1 d U . . H23 H 0.1364 0.3615 0.6620 0.119 Uiso 1 1 calc R . . C24 C 0.1369(4) 0.1725(16) 0.6789(5) 0.079(4) Uani 1 1 d U . . H24 H 0.1475 0.1798 0.7067 0.095 Uiso 1 1 calc R . . C25 C 0.1272(3) 0.0608(15) 0.6644(5) 0.075(4) Uani 1 1 d . . . H25 H 0.1292 -0.0066 0.6843 0.090 Uiso 1 1 calc R . . N6 N -0.0168(3) -0.0765(8) 0.8439(3) 0.063(6) Uani 0.50 1 d PGU . . C26 C -0.0376(3) 0.0236(12) 0.8462(4) 0.061(7) Uani 0.50 1 d PGU . . C27 C -0.0300(4) 0.1280(11) 0.8728(4) 0.069(8) Uani 0.50 1 d PGU . . C28 C -0.0016(4) 0.1323(11) 0.8970(4) 0.057(7) Uani 0.50 1 d PGU . . C29 C 0.0192(3) 0.0323(14) 0.8947(4) 0.070(7) Uani 0.50 1 d PGU . . C30 C 0.0116(3) -0.0722(11) 0.8681(4) 0.075(8) Uani 0.50 1 d PGU . . N7 N -0.0040(6) -0.1513(13) 0.7632(4) 0.134(12) Uani 0.50 1 d PGU . . C31 C -0.0360(6) -0.1291(15) 0.7615(4) 0.146(16) Uani 0.50 1 d PGU . . C32 C -0.0504(4) -0.0839(16) 0.7994(5) 0.145(16) Uani 0.50 1 d PGU . . C33 C -0.0329(3) -0.0608(11) 0.8390(3) 0.119(14) Uani 0.50 1 d PGU . . C34 C -0.0009(3) -0.0830(8) 0.8406(3) 0.127(16) Uani 0.50 1 d PGU . . C35 C 0.0136(4) -0.1282(12) 0.8027(5) 0.118(13) Uani 0.50 1 d PGU . . 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 0.0318(2) 0.0321(2) 0.02815(18) 0.00021(16) 0.00464(15) 0.00203(17) U2 0.0294(2) 0.0308(2) 0.02591(17) 0.00132(16) 0.00241(14) 0.00261(17) U3 0.0269(2) 0.0414(2) 0.02580(17) -0.00063(16) 0.00233(14) 0.00758(17) Cl1 0.0353(16) 0.0452(15) 0.0291(12) 0.0009(11) 0.0038(11) 0.0069(12) Cl2 0.0383(17) 0.0497(15) 0.0334(13) -0.0030(12) 0.0048(12) 0.0100(12) Cl3 0.048(2) 0.0616(19) 0.0388(15) -0.0171(13) 0.0113(13) -0.0063(14) Cl4 0.0307(14) 0.0429(15) 0.0373(12) 0.0045(12) -0.0033(10) 0.0036(12) Cl5 0.0445(19) 0.0479(16) 0.0475(16) -0.0046(13) 0.0025(13) 0.0134(13) O1A 0.044(5) 0.042(4) 0.024(3) -0.005(3) 0.002(3) 0.002(3) O2A 0.031(4) 0.028(4) 0.034(4) -0.001(3) 0.002(3) 0.006(3) O3A 0.035(4) 0.041(4) 0.030(3) 0.007(3) -0.002(3) 0.006(3) O4A 0.038(5) 0.040(4) 0.027(4) 0.005(3) -0.003(3) 0.002(3) N1A 0.032(6) 0.040(5) 0.042(5) 0.008(4) 0.004(4) -0.003(4) N2A 0.031(6) 0.038(5) 0.047(5) 0.005(4) 0.011(4) -0.009(4) C1A 0.030(6) 0.029(5) 0.034(5) -0.004(4) -0.003(5) 0.009(4) C2A 0.034(7) 0.029(5) 0.029(5) -0.004(4) -0.002(5) 0.005(4) C3A 0.042(7) 0.035(6) 0.032(5) 0.001(5) -0.006(5) 0.000(5) C4A 0.038(7) 0.029(6) 0.044(6) -0.006(5) -0.002(5) -0.002(5) C5A 0.058(8) 0.024(5) 0.033(6) -0.004(4) -0.003(5) -0.005(5) C6A 0.036(7) 0.033(5) 0.027(5) -0.006(4) 0.002(4) 0.010(5) C7A 0.038(7) 0.028(5) 0.043(6) -0.002(5) 0.003(5) -0.004(5) C8A 0.044(8) 0.040(6) 0.046(7) 0.000(5) 0.006(6) -0.003(5) C9A 0.042(8) 0.045(6) 0.041(6) 0.026(5) 0.007(5) -0.004(5) C10A 0.042(8) 0.056(7) 0.029(5) 0.001(5) 0.002(5) 0.006(6) C11A 0.035(7) 0.046(6) 0.033(6) 0.002(5) -0.007(5) -0.016(5) C12A 0.038(7) 0.040(6) 0.036(6) -0.001(5) 0.004(5) -0.017(5) C13A 0.037(7) 0.046(6) 0.027(5) 0.004(5) -0.012(5) -0.010(5) C14A 0.044(7) 0.085(7) 0.053(6) 0.018(6) -0.008(5) -0.025(6) C15A 0.073(8) 0.092(8) 0.041(6) 0.028(6) -0.009(6) -0.016(6) C16A 0.046(9) 0.085(9) 0.035(6) 0.013(6) -0.002(6) -0.027(7) C17A 0.038(8) 0.067(8) 0.043(6) 0.001(6) -0.006(6) -0.008(6) C18A 0.046(8) 0.046(7) 0.040(6) 0.010(5) 0.012(5) -0.018(5) O1B 0.031(4) 0.025(3) 0.028(3) 0.002(3) 0.006(3) -0.001(3) O2B 0.042(5) 0.027(3) 0.020(3) 0.008(3) 0.009(3) 0.003(3) O3B 0.027(4) 0.065(5) 0.022(3) -0.002(3) 0.000(3) 0.004(4) O4B 0.022(4) 0.047(4) 0.028(3) 0.004(3) 0.003(3) 0.006(3) N1B 0.025(5) 0.048(5) 0.022(4) 0.004(4) 0.003(4) -0.001(4) N2B 0.023(5) 0.050(5) 0.033(4) 0.003(4) 0.000(3) 0.001(4) C1B 0.032(7) 0.024(5) 0.039(6) -0.007(5) 0.000(5) -0.001(4) C2B 0.040(7) 0.022(5) 0.027(5) 0.001(4) 0.000(5) 0.014(4) C3B 0.031(7) 0.039(6) 0.043(6) 0.009(5) 0.005(5) 0.006(5) C4B 0.055(8) 0.032(6) 0.050(6) 0.019(5) 0.014(6) 0.016(5) C5B 0.047(8) 0.037(6) 0.043(6) 0.005(5) 0.013(5) 0.007(5) C6B 0.043(7) 0.033(6) 0.027(5) -0.003(4) 0.016(5) 0.004(5) C7B 0.031(7) 0.044(6) 0.042(6) 0.007(5) 0.004(5) 0.000(5) C8B 0.027(6) 0.044(6) 0.034(5) 0.006(5) 0.005(5) -0.001(5) C9B 0.020(6) 0.073(8) 0.023(5) 0.003(5) 0.003(4) -0.005(5) C10B 0.028(6) 0.060(7) 0.025(5) -0.004(5) -0.005(4) 0.004(5) C11B 0.042(7) 0.050(6) 0.025(5) -0.003(5) -0.001(4) 0.017(5) C12B 0.018(5) 0.068(8) 0.036(5) -0.001(5) -0.010(4) 0.014(5) C13B 0.027(6) 0.049(6) 0.030(5) -0.007(5) 0.006(4) 0.009(5) C14B 0.042(8) 0.078(8) 0.028(5) 0.003(5) 0.010(5) 0.023(6) C15B 0.051(9) 0.103(11) 0.024(5) 0.005(6) -0.001(5) 0.024(7) C16B 0.034(6) 0.070(8) 0.032(5) -0.005(5) -0.008(5) 0.005(6) C17B 0.034(8) 0.067(8) 0.085(9) -0.014(7) 0.020(7) -0.023(6) C18B 0.051(8) 0.061(8) 0.032(6) 0.015(5) 0.009(5) 0.013(6) N1 0.047(7) 0.038(5) 0.060(6) -0.008(5) -0.019(5) 0.004(5) C1 0.077(8) 0.053(7) 0.107(8) -0.008(6) -0.019(7) -0.001(6) C2 0.103(9) 0.082(8) 0.148(10) -0.014(8) -0.018(8) 0.011(8) C3 0.115(10) 0.082(8) 0.112(9) -0.001(7) -0.031(8) 0.005(8) C4 0.092(8) 0.059(7) 0.080(7) -0.003(6) -0.019(7) -0.009(7) C5 0.098(12) 0.028(6) 0.036(6) 0.012(5) -0.009(7) -0.012(6) N2 0.029(6) 0.031(5) 0.047(5) 0.002(4) 0.002(4) 0.002(4) C6 0.024(7) 0.044(7) 0.081(9) -0.001(6) 0.001(6) 0.004(5) C7 0.049(7) 0.075(7) 0.105(8) -0.011(7) 0.008(7) -0.005(6) C8 0.068(8) 0.082(8) 0.102(8) -0.039(7) -0.005(7) -0.001(6) C9 0.066(8) 0.071(7) 0.075(7) -0.023(6) -0.009(6) 0.012(6) C10 0.043(8) 0.033(6) 0.056(7) -0.006(5) -0.006(6) 0.008(5) N3 0.042(6) 0.033(5) 0.035(5) -0.004(4) 0.010(4) -0.001(4) C11 0.037(7) 0.047(7) 0.044(6) 0.000(5) -0.003(5) -0.001(5) C12 0.043(8) 0.056(7) 0.044(6) -0.004(5) -0.002(6) 0.016(6) C13 0.036(8) 0.052(7) 0.071(9) -0.036(7) 0.004(6) 0.005(6) C14 0.072(10) 0.049(7) 0.055(8) -0.008(6) -0.014(7) 0.034(7) C15 0.063(9) 0.039(6) 0.034(6) 0.007(5) 0.004(6) 0.008(6) N4 0.048(6) 0.037(5) 0.032(4) -0.001(4) 0.005(4) -0.011(4) C16 0.046(8) 0.034(6) 0.051(7) 0.002(5) 0.001(6) 0.001(5) C17 0.092(11) 0.032(6) 0.044(7) 0.014(5) 0.019(7) 0.007(6) C18 0.071(9) 0.042(7) 0.054(7) 0.017(6) 0.027(6) 0.011(6) C19 0.042(7) 0.038(6) 0.063(7) -0.004(6) 0.000(6) 0.002(5) C20 0.058(8) 0.042(6) 0.039(6) -0.003(5) -0.013(5) 0.008(6) N5 0.124(12) 0.085(9) 0.057(7) 0.001(7) 0.006(7) 0.014(8) C21 0.102(14) 0.111(13) 0.029(7) 0.004(8) -0.006(7) 0.001(10) C22 0.062(8) 0.075(7) 0.089(8) 0.017(7) 0.027(7) 0.005(6) C23 0.084(9) 0.097(9) 0.119(9) -0.017(8) 0.025(8) -0.020(7) C24 0.070(8) 0.102(8) 0.064(7) -0.002(7) -0.010(6) -0.023(7) C25 0.044(9) 0.101(12) 0.080(10) 0.013(9) 0.013(7) 0.011(8) N6 0.064(10) 0.066(10) 0.061(9) 0.006(8) 0.029(8) -0.013(8) C26 0.061(10) 0.062(10) 0.061(10) 0.015(8) 0.005(8) 0.001(8) C27 0.070(11) 0.073(11) 0.064(10) -0.003(8) 0.012(9) 0.004(9) C28 0.061(10) 0.055(10) 0.056(10) 0.004(8) 0.009(8) -0.008(8) C29 0.075(11) 0.070(11) 0.065(10) -0.004(8) 0.006(8) 0.005(9) C30 0.080(12) 0.082(11) 0.064(11) 0.010(9) 0.009(9) 0.004(9) N7 0.142(14) 0.125(13) 0.135(15) 0.000(9) 0.012(10) -0.004(10) C31 0.149(19) 0.140(18) 0.149(18) -0.002(10) -0.006(10) 0.006(10) C32 0.145(18) 0.141(18) 0.149(18) 0.008(10) 0.007(10) -0.006(10) C33 0.121(17) 0.119(17) 0.117(16) 0.018(10) 0.015(10) -0.006(10) C34 0.124(18) 0.125(18) 0.132(18) -0.008(10) 0.004(10) -0.004(10) C35 0.117(16) 0.117(15) 0.119(15) 0.000(10) -0.001(10) -0.007(10) _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 O2A 2.318(6) . ? U1 O3A 2.320(6) . ? U1 O1B 2.396(6) . ? U1 N2A 2.553(8) . ? U1 N1A 2.576(8) . ? U1 Cl3 2.676(3) . ? U1 Cl1 2.706(2) . ? U1 Cl2 2.725(3) . ? U1 U2 3.7071(5) . ? U2 O4A 2.244(6) . ? U2 O4B 2.308(6) 5_567 ? U2 O1B 2.389(6) . ? U2 O1A 2.416(6) . ? U2 O2A 2.438(7) . ? U2 O3A 2.463(6) . ? U2 O2B 2.474(5) . ? U2 N1 2.600(9) . ? U2 N2 2.653(8) . ? U2 U3 3.7374(5) . ? U3 O3B 2.170(6) 5_567 ? U3 O2B 2.362(6) . ? U3 O1A 2.434(7) . ? U3 O4B 2.582(6) 5_567 ? U3 N2B 2.608(8) . ? U3 N1B 2.645(8) . ? U3 Cl4 2.658(2) . ? U3 Cl5 2.682(3) . ? O1A C1A 1.368(12) . ? O2A C2A 1.350(10) . ? O3A C12A 1.335(11) . ? O4A C13A 1.342(12) . ? N1A C7A 1.295(12) . ? N1A C8A 1.536(13) . ? N2A C10A 1.280(12) . ? N2A C9A 1.463(13) . ? C1A C6A 1.395(12) . ? C1A C2A 1.401(14) . ? C2A C3A 1.399(14) . ? C3A C4A 1.422(13) . ? C3A C7A 1.459(14) . ? C4A C5A 1.359(14) . ? C5A C6A 1.400(14) . ? C8A C9A 1.519(14) . ? C8A C17A 1.524(15) . ? C8A C18A 1.532(14) . ? C10A C11A 1.421(14) . ? C11A C16A 1.385(14) . ? C11A C12A 1.406(14) . ? C12A C13A 1.421(14) . ? C13A C14A 1.375(14) . ? C14A C15A 1.395(16) . ? C15A C16A 1.359(17) . ? O1B C1B 1.345(11) . ? O2B C2B 1.344(10) . ? O3B C12B 1.334(10) . ? O3B U3 2.170(6) 5_567 ? O4B C13B 1.368(11) . ? O4B U2 2.308(6) 5_567 ? O4B U3 2.582(6) 5_567 ? N1B C7B 1.273(12) . ? N1B C8B 1.524(12) . ? N2B C10B 1.288(11) . ? N2B C9B 1.448(12) . ? C1B C6B 1.377(13) . ? C1B C2B 1.424(13) . ? C2B C3B 1.377(13) . ? C3B C4B 1.411(13) . ? C3B C7B 1.441(14) . ? C4B C5B 1.369(14) . ? C5B C6B 1.392(13) . ? C8B C17B 1.518(14) . ? C8B C18B 1.536(13) . ? C8B C9B 1.542(14) . ? C10B C11B 1.487(13) . ? C11B C12B 1.405(13) . ? C11B C16B 1.419(12) . ? C12B C13B 1.404(13) . ? C13B C14B 1.377(13) . ? C14B C15B 1.393(16) . ? C15B C16B 1.375(15) . ? N1 C1 1.308(16) . ? N1 C5 1.344(15) . ? C1 C2 1.433(19) . ? C2 C3 1.35(2) . ? C3 C4 1.37(2) . ? C4 C5 1.408(15) . ? N2 C6 1.343(13) . ? N2 C10 1.343(13) . ? C6 C7 1.382(17) . ? C7 C8 1.409(19) . ? C8 C9 1.390(19) . ? C9 C10 1.379(16) . ? N3 C15 1.324(13) . ? N3 C11 1.328(12) . ? C11 C12 1.353(15) . ? C12 C13 1.379(15) . ? C13 C14 1.345(16) . ? C14 C15 1.365(16) . ? N4 C20 1.347(13) . ? N4 C16 1.357(12) . ? C16 C17 1.404(15) . ? C17 C18 1.349(15) . ? C18 C19 1.331(14) . ? C19 C20 1.386(15) . ? N5 C25 1.271(17) . ? N5 C21 1.299(17) . ? C21 C22 1.353(19) . ? C22 C23 1.41(2) . ? C23 C24 1.41(2) . ? C24 C25 1.321(18) . ? N6 C26 1.3900 . ? N6 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? N7 C31 1.3900 . ? N7 C35 1.3900 . ? C31 C32 1.3898 . ? C32 C33 1.3901 . ? C33 C34 1.3900 . ? C34 C35 1.3902 . ? 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 O2A U1 O3A 65.2(2) . . ? O2A U1 O1B 68.5(2) . . ? O3A U1 O1B 68.6(2) . . ? O2A U1 N2A 102.0(2) . . ? O3A U1 N2A 69.5(3) . . ? O1B U1 N2A 137.0(2) . . ? O2A U1 N1A 68.6(3) . . ? O3A U1 N1A 100.3(2) . . ? O1B U1 N1A 136.3(2) . . ? N2A U1 N1A 61.6(3) . . ? O2A U1 Cl3 137.87(17) . . ? O3A U1 Cl3 80.04(17) . . ? O1B U1 Cl3 77.37(15) . . ? N2A U1 Cl3 86.2(2) . . ? N1A U1 Cl3 144.5(2) . . ? O2A U1 Cl1 76.24(16) . . ? O3A U1 Cl1 135.50(16) . . ? O1B U1 Cl1 77.49(15) . . ? N2A U1 Cl1 143.2(2) . . ? N1A U1 Cl1 84.65(19) . . ? Cl3 U1 Cl1 120.16(8) . . ? O2A U1 Cl2 142.64(17) . . ? O3A U1 Cl2 147.47(16) . . ? O1B U1 Cl2 129.01(15) . . ? N2A U1 Cl2 84.7(2) . . ? N1A U1 Cl2 83.6(2) . . ? Cl3 U1 Cl2 78.68(9) . . ? Cl1 U1 Cl2 76.87(8) . . ? O4A U2 O4B 89.9(2) . 5_567 ? O4A U2 O1B 117.8(2) . . ? O4B U2 O1B 133.5(2) 5_567 . ? O4A U2 O1A 141.0(2) . . ? O4B U2 O1A 69.8(2) 5_567 . ? O1B U2 O1A 99.7(2) . . ? O4A U2 O2A 118.4(2) . . ? O4B U2 O2A 133.8(2) 5_567 . ? O1B U2 O2A 66.7(2) . . ? O1A U2 O2A 65.4(2) . . ? O4A U2 O3A 66.4(2) . . ? O4B U2 O3A 155.9(2) 5_567 . ? O1B U2 O3A 66.4(2) . . ? O1A U2 O3A 126.1(2) . . ? O2A U2 O3A 61.3(2) . . ? O4A U2 O2B 137.5(2) . . ? O4B U2 O2B 68.5(2) 5_567 . ? O1B U2 O2B 66.0(2) . . ? O1A U2 O2B 66.3(2) . . ? O2A U2 O2B 102.2(2) . . ? O3A U2 O2B 132.3(2) . . ? O4A U2 N1 71.8(3) . . ? O4B U2 N1 88.5(3) 5_567 . ? O1B U2 N1 133.7(3) . . ? O1A U2 N1 74.6(3) . . ? O2A U2 N1 69.5(3) . . ? O3A U2 N1 80.1(3) . . ? O2B U2 N1 139.4(3) . . ? O4A U2 N2 68.9(2) . . ? O4B U2 N2 81.7(2) 5_567 . ? O1B U2 N2 75.7(2) . . ? O1A U2 N2 135.6(2) . . ? O2A U2 N2 140.5(2) . . ? O3A U2 N2 93.2(2) . . ? O2B U2 N2 71.9(2) . . ? N1 U2 N2 139.4(3) . . ? O3B U3 O2B 99.5(2) 5_567 . ? O3B U3 O1A 130.1(2) 5_567 . ? O2B U3 O1A 67.8(2) . . ? O3B U3 O4B 65.7(2) 5_567 5_567 ? O2B U3 O4B 65.9(2) . 5_567 ? O1A U3 O4B 65.2(2) . 5_567 ? O3B U3 N2B 72.1(2) 5_567 . ? O2B U3 N2B 134.6(2) . . ? O1A U3 N2B 150.4(2) . . ? O4B U3 N2B 136.2(2) 5_567 . ? O3B U3 N1B 80.5(3) 5_567 . ? O2B U3 N1B 70.0(2) . . ? O1A U3 N1B 130.9(2) . . ? O4B U3 N1B 117.2(2) 5_567 . ? N2B U3 N1B 64.6(2) . . ? O3B U3 Cl4 149.23(16) 5_567 . ? O2B U3 Cl4 94.42(16) . . ? O1A U3 Cl4 80.63(16) . . ? O4B U3 Cl4 144.78(16) 5_567 . ? N2B U3 Cl4 78.60(17) . . ? N1B U3 Cl4 78.71(18) . . ? O3B U3 Cl5 90.40(19) 5_567 . ? O2B U3 Cl5 145.82(15) . . ? O1A U3 Cl5 80.74(16) . . ? O4B U3 Cl5 89.38(15) 5_567 . ? N2B U3 Cl5 79.58(19) . . ? N1B U3 Cl5 144.15(18) . . ? Cl4 U3 Cl5 93.29(8) . . ? C1A O1A U2 119.8(6) . . ? C1A O1A U3 136.8(6) . . ? U2 O1A U3 100.8(2) . . ? C2A O2A U1 134.0(6) . . ? C2A O2A U2 119.4(6) . . ? U1 O2A U2 102.4(2) . . ? C12A O3A U1 141.5(6) . . ? C12A O3A U2 116.7(6) . . ? U1 O3A U2 101.6(2) . . ? C13A O4A U2 124.0(6) . . ? C7A N1A C8A 116.4(9) . . ? C7A N1A U1 125.2(7) . . ? C8A N1A U1 118.3(6) . . ? C10A N2A C9A 120.2(9) . . ? C10A N2A U1 131.5(8) . . ? C9A N2A U1 108.3(6) . . ? O1A C1A C6A 124.5(9) . . ? O1A C1A C2A 116.5(8) . . ? C6A C1A C2A 119.0(10) . . ? O2A C2A C3A 121.6(9) . . ? O2A C2A C1A 116.9(9) . . ? C3A C2A C1A 121.5(9) . . ? C2A C3A C4A 117.6(10) . . ? C2A C3A C7A 120.9(9) . . ? C4A C3A C7A 120.7(10) . . ? C5A C4A C3A 121.2(10) . . ? C4A C5A C6A 120.5(9) . . ? C1A C6A C5A 120.1(10) . . ? N1A C7A C3A 128.6(10) . . ? C9A C8A C17A 109.4(9) . . ? C9A C8A C18A 107.5(9) . . ? C17A C8A C18A 113.0(9) . . ? C9A C8A N1A 107.2(8) . . ? C17A C8A N1A 110.2(9) . . ? C18A C8A N1A 109.3(9) . . ? N2A C9A C8A 109.8(9) . . ? N2A C10A C11A 129.2(10) . . ? C16A C11A C12A 118.9(11) . . ? C16A C11A C10A 119.6(10) . . ? C12A C11A C10A 120.6(9) . . ? O3A C12A C11A 124.2(10) . . ? O3A C12A C13A 115.2(9) . . ? C11A C12A C13A 120.2(9) . . ? O4A C13A C14A 125.1(11) . . ? O4A C13A C12A 116.2(8) . . ? C14A C13A C12A 118.6(10) . . ? C13A C14A C15A 119.8(12) . . ? C16A C15A C14A 121.7(11) . . ? C15A C16A C11A 120.3(11) . . ? C1B O1B U2 120.7(6) . . ? C1B O1B U1 132.6(6) . . ? U2 O1B U1 101.5(2) . . ? C2B O2B U3 135.2(5) . . ? C2B O2B U2 118.2(5) . . ? U3 O2B U2 101.2(2) . . ? C12B O3B U3 128.0(6) . 5_567 ? C13B O4B U2 135.8(5) . 5_567 ? C13B O4B U3 113.5(5) . 5_567 ? U2 O4B U3 99.5(2) 5_567 5_567 ? C7B N1B C8B 114.5(8) . . ? C7B N1B U3 127.2(7) . . ? C8B N1B U3 117.1(6) . . ? C10B N2B C9B 120.3(8) . . ? C10B N2B U3 129.5(7) . . ? C9B N2B U3 110.1(5) . . ? O1B C1B C6B 123.8(9) . . ? O1B C1B C2B 117.6(8) . . ? C6B C1B C2B 118.6(9) . . ? O2B C2B C3B 122.6(9) . . ? O2B C2B C1B 116.7(8) . . ? C3B C2B C1B 120.7(9) . . ? C2B C3B C4B 118.0(10) . . ? C2B C3B C7B 124.6(9) . . ? C4B C3B C7B 117.3(9) . . ? C5B C4B C3B 122.4(10) . . ? C4B C5B C6B 118.4(10) . . ? C1B C6B C5B 121.8(10) . . ? N1B C7B C3B 129.1(10) . . ? C17B C8B N1B 111.2(8) . . ? C17B C8B C18B 112.2(9) . . ? N1B C8B C18B 107.7(8) . . ? C17B C8B C9B 107.3(9) . . ? N1B C8B C9B 107.6(8) . . ? C18B C8B C9B 110.8(8) . . ? N2B C9B C8B 109.4(8) . . ? N2B C10B C11B 126.3(10) . . ? C12B C11B C16B 119.2(9) . . ? C12B C11B C10B 119.6(8) . . ? C16B C11B C10B 121.0(9) . . ? O3B C12B C13B 118.3(9) . . ? O3B C12B C11B 122.0(9) . . ? C13B C12B C11B 119.7(8) . . ? O4B C13B C14B 125.3(9) . . ? O4B C13B C12B 114.2(8) . . ? C14B C13B C12B 120.5(10) . . ? C13B C14B C15B 119.5(10) . . ? C16B C15B C14B 121.7(9) . . ? C15B C16B C11B 119.2(10) . . ? C1 N1 C5 117.5(11) . . ? C1 N1 U2 116.8(9) . . ? C5 N1 U2 123.1(8) . . ? N1 C1 C2 121.7(16) . . ? C3 C2 C1 116.8(18) . . ? C2 C3 C4 124.3(17) . . ? C3 C4 C5 112.6(16) . . ? N1 C5 C4 126.4(14) . . ? C6 N2 C10 118.7(10) . . ? C6 N2 U2 123.5(7) . . ? C10 N2 U2 116.1(7) . . ? N2 C6 C7 120.8(12) . . ? C6 C7 C8 119.9(14) . . ? C9 C8 C7 119.0(13) . . ? C10 C9 C8 116.8(13) . . ? N2 C10 C9 124.7(12) . . ? C15 N3 C11 120.2(10) . . ? N3 C11 C12 120.7(10) . . ? C11 C12 C13 119.4(11) . . ? C14 C13 C12 119.4(12) . . ? C13 C14 C15 118.9(11) . . ? N3 C15 C14 121.4(10) . . ? C20 N4 C16 117.0(9) . . ? N4 C16 C17 120.4(10) . . ? C18 C17 C16 120.2(10) . . ? C19 C18 C17 119.9(11) . . ? C18 C19 C20 119.3(11) . . ? N4 C20 C19 123.1(10) . . ? C25 N5 C21 116.6(14) . . ? N5 C21 C22 126.7(14) . . ? C21 C22 C23 116.3(14) . . ? C24 C23 C22 115.1(15) . . ? C25 C24 C23 120.0(15) . . ? N5 C25 C24 125.0(16) . . ? C26 N6 C30 120.0 . . ? N6 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 N6 120.0 . . ? C31 N7 C35 120.0 . . ? C32 C31 N7 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? N7 C35 C34 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 N3 H3 N4 0.95 1.79 2.734(12) 169.6 .