Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Michel Ephritikhine' 'Jean-Jacques Girerd' 'Eric Riviere' 'Lionel Salmon' 'Pierre Thuery' _publ_contact_author_name 'Dr Michel Ephritikhine' _publ_contact_author_address ; Service de Chimie Moleculaire CEA Saclay SCM, DRECAM, CNRS URA 331, Bat 125, Gif-sur-Yvette 91191 FRANCE ; _publ_contact_author_phone '33 01 69 08 64 36' _publ_contact_author_fax '33 1 69 08 66 40' _publ_contact_author_email ephri@drecam.cea.fr _publ_section_title ; Versatility of the nature of the magnetic Cu(II)-U(IV) interaction. Syntheses, crystal structures and magnetic properties of Cu2U and CuU compounds ; data_[(CuL^2^(py))U(CuL^2^)].py _database_code_CSD 208958 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H38 Cu2 N6 O8 U' _chemical_formula_weight 1143.91 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4972(12) _cell_length_b 26.2608(11) _cell_length_c 17.3250(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.654(3) _cell_angle_gamma 90.00 _cell_volume 7957.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 53131 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method ? _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 5.184 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.345 _exptl_absorpt_correction_T_max 0.537 _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_special_details 'crystal-to-detector distance 28 mm' _diffrn_ambient_temperature 110(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 53131 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.68 _reflns_number_total 14860 _reflns_number_gt 8753 _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 with some constraints for some atoms of the solvent pyridine molecules. All H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. The highest residual electron density peak is located near the U atom, as a result of imperfect absorption corrections. 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^)+(0.0530P)^2^+23.8583P] 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 14860 _refine_ls_number_parameters 1099 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.371 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.110 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 0.13375(2) 0.870573(15) 0.36005(2) 0.05739(12) Uani 1 1 d . . . Cu1 Cu 0.31175(8) 0.80405(5) 0.40853(8) 0.0643(4) Uani 1 1 d . . . Cu2 Cu -0.04016(7) 0.94523(5) 0.31938(8) 0.0590(3) Uani 1 1 d . . . O1A O 0.0619(4) 0.7974(3) 0.3395(4) 0.0590(17) Uani 1 1 d . . . O2A O 0.2075(4) 0.7918(2) 0.3699(4) 0.0629(18) Uani 1 1 d . . . O3A O 0.2723(4) 0.8726(2) 0.3898(4) 0.0603(17) Uani 1 1 d . . . O4A O 0.1831(4) 0.9508(3) 0.3813(4) 0.0646(19) Uani 1 1 d . . . O5A O 0.1110(4) 0.8613(2) 0.4869(4) 0.0593(17) Uani 1 1 d . . . O6A O 0.0209(4) 0.9173(3) 0.4023(4) 0.0611(18) Uani 1 1 d . . . O7A O 0.0405(4) 0.9099(3) 0.2687(4) 0.0625(18) Uani 1 1 d . . . O8A O 0.1673(4) 0.8656(3) 0.2334(4) 0.0623(18) Uani 1 1 d . . . N1A N 0.3387(6) 0.7318(4) 0.3937(5) 0.069(3) Uani 1 1 d . . . N2A N 0.4164(6) 0.8308(4) 0.4361(8) 0.094(4) Uani 1 1 d . . . N3A N -0.1059(5) 0.9844(3) 0.3894(6) 0.061(2) Uani 1 1 d . . . N4A N -0.0916(5) 0.9619(3) 0.2198(5) 0.062(2) Uani 1 1 d . . . N5A N 0.2742(5) 0.7971(4) 0.5330(6) 0.072(3) Uani 1 1 d . . . C1A C 0.0925(6) 0.7516(4) 0.3418(6) 0.057(3) Uani 1 1 d . . . C2A C 0.1733(7) 0.7472(4) 0.3606(6) 0.058(3) Uani 1 1 d . . . C3A C 0.2105(8) 0.7010(4) 0.3640(7) 0.074(3) Uani 1 1 d . . . C4A C 0.1673(8) 0.6568(5) 0.3520(8) 0.082(4) Uani 1 1 d . . . H4A H 0.1914 0.6252 0.3549 0.098 Uiso 1 1 calc R . . C5A C 0.0900(9) 0.6589(4) 0.3359(7) 0.080(4) Uani 1 1 d . . . H5A H 0.0619 0.6291 0.3297 0.096 Uiso 1 1 calc R . . C6A C 0.0540(8) 0.7062(4) 0.3289(6) 0.073(3) Uani 1 1 d . . . H6A H 0.0022 0.7072 0.3152 0.087 Uiso 1 1 calc R . . C7A C 0.2919(8) 0.6954(5) 0.3780(7) 0.078(3) Uani 1 1 d . . . H7A H 0.3120 0.6627 0.3755 0.093 Uiso 1 1 calc R . . C8A C 0.4189(8) 0.7173(5) 0.4041(9) 0.098(5) Uani 1 1 d . . . H8A1 H 0.4452 0.7248 0.3569 0.117 Uiso 1 1 calc R . . H8A2 H 0.4217 0.6808 0.4124 0.117 Uiso 1 1 calc R . . C9A C 0.4603(8) 0.7435(6) 0.4700(8) 0.097(5) Uani 1 1 d . . . H9A1 H 0.4279 0.7441 0.5145 0.117 Uiso 1 1 calc R . . H9A2 H 0.5062 0.7245 0.4839 0.117 Uiso 1 1 calc R . . C10A C 0.4813(8) 0.7963(7) 0.4493(12) 0.130(7) Uani 1 1 d . . . H10A H 0.5139 0.8101 0.4904 0.157 Uiso 1 1 calc R . . H10B H 0.5110 0.7953 0.4028 0.157 Uiso 1 1 calc R . . C11A C 0.4283(8) 0.8768(6) 0.4495(11) 0.109(5) Uani 1 1 d . . . H11A H 0.4781 0.8848 0.4654 0.130 Uiso 1 1 calc R . . C12A C 0.3756(6) 0.9199(4) 0.4440(8) 0.073(3) Uani 1 1 d . . . C13A C 0.3024(6) 0.9171(4) 0.4142(6) 0.061(3) Uani 1 1 d . . . C14A C 0.2540(6) 0.9589(4) 0.4103(6) 0.060(3) Uani 1 1 d . . . C15A C 0.2815(7) 1.0062(4) 0.4373(8) 0.077(3) Uani 1 1 d . . . H15A H 0.2503 1.0348 0.4354 0.093 Uiso 1 1 calc R . . C16A C 0.3554(8) 1.0095(5) 0.4667(8) 0.081(4) Uani 1 1 d . . . H16A H 0.3736 1.0406 0.4852 0.097 Uiso 1 1 calc R . . C17A C 0.4023(8) 0.9679(5) 0.4690(9) 0.093(4) Uani 1 1 d . . . H17A H 0.4525 0.9714 0.4872 0.111 Uiso 1 1 calc R . . C18A C 0.0555(6) 0.8848(4) 0.5230(6) 0.055(2) Uani 1 1 d . . . C19A C 0.0062(6) 0.9173(4) 0.4773(6) 0.056(2) Uani 1 1 d . . . C20A C -0.0510(6) 0.9469(4) 0.5089(7) 0.058(3) Uani 1 1 d . . . C21A C -0.0623(6) 0.9429(4) 0.5898(7) 0.065(3) Uani 1 1 d . . . H21A H -0.1000 0.9624 0.6125 0.077 Uiso 1 1 calc R . . C22A C -0.0190(6) 0.9111(4) 0.6340(7) 0.064(3) Uani 1 1 d . . . H22A H -0.0276 0.9085 0.6866 0.077 Uiso 1 1 calc R . . C23A C 0.0401(6) 0.8813(4) 0.6005(7) 0.064(3) Uani 1 1 d . . . H23A H 0.0688 0.8592 0.6316 0.077 Uiso 1 1 calc R . . C24A C -0.0995(6) 0.9802(4) 0.4643(7) 0.062(3) Uani 1 1 d . . . H24A H -0.1306 1.0016 0.4924 0.074 Uiso 1 1 calc R . . C25A C -0.1653(6) 1.0199(4) 0.3621(7) 0.067(3) Uani 1 1 d . . . H25A H -0.1625 1.0505 0.3933 0.081 Uiso 1 1 calc R . . H25B H -0.2150 1.0045 0.3693 0.081 Uiso 1 1 calc R . . C26A C -0.1584(6) 1.0343(4) 0.2780(6) 0.066(3) Uani 1 1 d . . . H26A H -0.1097 1.0512 0.2715 0.079 Uiso 1 1 calc R . . H26B H -0.1984 1.0586 0.2644 0.079 Uiso 1 1 calc R . . C27A C -0.1642(6) 0.9891(4) 0.2219(7) 0.064(3) Uani 1 1 d . . . H27A H -0.2040 0.9661 0.2381 0.076 Uiso 1 1 calc R . . H27B H -0.1780 1.0014 0.1706 0.076 Uiso 1 1 calc R . . C28A C -0.0658(7) 0.9513(4) 0.1531(7) 0.072(3) Uani 1 1 d . . . H28A H -0.0958 0.9618 0.1108 0.086 Uiso 1 1 calc R . . C29A C 0.0034(6) 0.9253(4) 0.1359(7) 0.068(3) Uani 1 1 d . . . C30A C 0.0549(6) 0.9066(4) 0.1926(7) 0.062(3) Uani 1 1 d . . . C31A C 0.1240(5) 0.8820(4) 0.1730(7) 0.056(3) Uani 1 1 d . . . C32A C 0.1424(7) 0.8794(4) 0.0960(7) 0.072(3) Uani 1 1 d . . . H32A H 0.1886 0.8649 0.0824 0.087 Uiso 1 1 calc R . . C33A C 0.0927(7) 0.8981(5) 0.0383(8) 0.078(3) Uani 1 1 d . . . H33A H 0.1060 0.8954 -0.0131 0.094 Uiso 1 1 calc R . . C34A C 0.0252(8) 0.9204(5) 0.0558(7) 0.085(4) Uani 1 1 d . . . H34A H -0.0072 0.9325 0.0164 0.101 Uiso 1 1 calc R . . C35A C 0.2325(7) 0.7575(4) 0.5537(8) 0.075(3) Uani 1 1 d . . . H35A H 0.2308 0.7293 0.5211 0.089 Uiso 1 1 calc R . . C36A C 0.1917(7) 0.7552(5) 0.6199(7) 0.074(3) Uani 1 1 d . . . H36A H 0.1621 0.7269 0.6310 0.089 Uiso 1 1 calc R . . C37A C 0.1958(7) 0.7956(5) 0.6688(7) 0.070(3) Uani 1 1 d . . . H37A H 0.1693 0.7953 0.7145 0.084 Uiso 1 1 calc R . . C38A C 0.2398(7) 0.8369(4) 0.6496(7) 0.075(3) Uani 1 1 d . . . H38A H 0.2431 0.8650 0.6821 0.090 Uiso 1 1 calc R . . C39A C 0.2784(7) 0.8361(4) 0.5828(7) 0.070(3) Uani 1 1 d . . . H39A H 0.3091 0.8638 0.5710 0.085 Uiso 1 1 calc R . . U2 U 0.64129(2) 0.629708(16) 0.60737(3) 0.06355(13) Uani 1 1 d . . . Cu3 Cu 0.81674(8) 0.70459(5) 0.58955(9) 0.0699(4) Uani 1 1 d . . . Cu4 Cu 0.46367(8) 0.56063(5) 0.64129(8) 0.0626(3) Uani 1 1 d . . . O1B O 0.5965(4) 0.6430(3) 0.4832(4) 0.0636(19) Uani 1 1 d . . . O2B O 0.7278(4) 0.6799(3) 0.5297(4) 0.0647(19) Uani 1 1 d . . . O3B O 0.7645(4) 0.6589(3) 0.6600(5) 0.070(2) Uani 1 1 d . . . O4B O 0.6609(5) 0.6121(3) 0.7368(4) 0.071(2) Uani 1 1 d . . . O5B O 0.5927(4) 0.7075(3) 0.6356(5) 0.069(2) Uani 1 1 d . . . O6B O 0.5072(4) 0.6274(3) 0.6467(4) 0.0682(19) Uani 1 1 d . . . O7B O 0.5646(4) 0.5514(3) 0.6017(4) 0.0626(18) Uani 1 1 d . . . O8B O 0.7077(4) 0.5580(3) 0.5704(4) 0.069(2) Uani 1 1 d . . . N1B N 0.8606(5) 0.7354(3) 0.4950(6) 0.064(2) Uani 1 1 d . . . N2B N 0.9100(6) 0.7071(4) 0.6591(6) 0.080(3) Uani 1 1 d . . . N3B N 0.3685(5) 0.5844(4) 0.6865(5) 0.066(2) Uani 1 1 d . . . N4B N 0.4390(5) 0.4881(3) 0.6290(5) 0.064(2) Uani 1 1 d . . . N5B N 0.7664(7) 0.7838(4) 0.6251(7) 0.084(3) Uani 1 1 d . . . C1B C 0.6342(6) 0.6720(4) 0.4330(7) 0.064(3) Uani 1 1 d . . . C2B C 0.7053(6) 0.6918(4) 0.4582(7) 0.063(3) Uani 1 1 d . . . C3B C 0.7490(6) 0.7220(4) 0.4096(7) 0.063(3) Uani 1 1 d . . . C4B C 0.7183(6) 0.7343(4) 0.3352(8) 0.069(3) Uani 1 1 d . . . H4B H 0.7458 0.7552 0.3028 0.083 Uiso 1 1 calc R . . C5B C 0.6486(7) 0.7156(4) 0.3104(7) 0.072(3) Uani 1 1 d . . . H5B H 0.6289 0.7241 0.2617 0.086 Uiso 1 1 calc R . . C6B C 0.6076(6) 0.6840(4) 0.3586(7) 0.067(3) Uani 1 1 d . . . H6B H 0.5612 0.6706 0.3407 0.080 Uiso 1 1 calc R . . C7B C 0.8249(6) 0.7410(4) 0.4308(7) 0.065(3) Uani 1 1 d . . . H7B H 0.8500 0.7593 0.3932 0.078 Uiso 1 1 calc R . . C8B C 0.9382(7) 0.7614(5) 0.4999(9) 0.087(4) Uani 1 1 d . . . H8B1 H 0.9583 0.7646 0.4485 0.105 Uiso 1 1 calc R . . H8B2 H 0.9327 0.7953 0.5210 0.105 Uiso 1 1 calc R . . C9B C 0.9928(7) 0.7315(5) 0.5496(8) 0.085(4) Uani 1 1 d . . . H9B1 H 1.0441 0.7436 0.5405 0.103 Uiso 1 1 calc R . . H9B2 H 0.9904 0.6962 0.5333 0.103 Uiso 1 1 calc R . . C10B C 0.9801(7) 0.7335(6) 0.6344(9) 0.095(4) Uani 1 1 d . . . H10C H 1.0239 0.7183 0.6612 0.115 Uiso 1 1 calc R . . H10D H 0.9775 0.7689 0.6501 0.115 Uiso 1 1 calc R . . C11B C 0.9129(7) 0.6857(4) 0.7275(8) 0.074(3) Uani 1 1 d . . . H11B H 0.9601 0.6869 0.7535 0.089 Uiso 1 1 calc R . . C12B C 0.8523(7) 0.6606(4) 0.7677(7) 0.072(3) Uani 1 1 d . . . C13B C 0.7830(7) 0.6484(4) 0.7325(8) 0.070(3) Uani 1 1 d . . . C14B C 0.7250(7) 0.6242(4) 0.7764(7) 0.067(3) Uani 1 1 d . . . C15B C 0.7404(8) 0.6138(4) 0.8536(8) 0.079(3) Uani 1 1 d . . . H15B H 0.7030 0.5988 0.8832 0.094 Uiso 1 1 calc R . . C16B C 0.8121(9) 0.6257(4) 0.8876(8) 0.084(4) Uani 1 1 d . . . H16B H 0.8223 0.6175 0.9392 0.101 Uiso 1 1 calc R . . C17B C 0.8656(8) 0.6486(4) 0.8466(7) 0.075(3) Uani 1 1 d . . . H17B H 0.9123 0.6567 0.8702 0.090 Uiso 1 1 calc R . . C18B C 0.5230(7) 0.7154(4) 0.6600(7) 0.067(3) Uani 1 1 d . . . C19B C 0.4744(6) 0.6716(4) 0.6675(6) 0.062(3) Uani 1 1 d . . . C20B C 0.4015(7) 0.6751(4) 0.6923(6) 0.064(3) Uani 1 1 d . . . C21B C 0.3719(7) 0.7243(5) 0.7104(7) 0.069(3) Uani 1 1 d . . . H21B H 0.3225 0.7277 0.7280 0.083 Uiso 1 1 calc R . . C22B C 0.4173(8) 0.7668(5) 0.7014(7) 0.077(3) Uani 1 1 d . . . H22B H 0.3978 0.7989 0.7119 0.093 Uiso 1 1 calc R . . C23B C 0.4906(7) 0.7621(5) 0.6773(7) 0.073(3) Uani 1 1 d . . . H23B H 0.5200 0.7913 0.6722 0.088 Uiso 1 1 calc R . . C24B C 0.3533(7) 0.6317(5) 0.7019(7) 0.069(3) Uani 1 1 d . . . H24B H 0.3053 0.6381 0.7216 0.083 Uiso 1 1 calc R . . C25B C 0.3052(6) 0.5488(4) 0.6971(7) 0.070(3) Uani 1 1 d . . . H25C H 0.2759 0.5457 0.6490 0.084 Uiso 1 1 calc R . . H25D H 0.2716 0.5623 0.7357 0.084 Uiso 1 1 calc R . . C26B C 0.3324(7) 0.4968(4) 0.7220(7) 0.074(3) Uani 1 1 d . . . H26C H 0.2898 0.4781 0.7427 0.089 Uiso 1 1 calc R . . H26D H 0.3709 0.5006 0.7631 0.089 Uiso 1 1 calc R . . C27B C 0.3657(7) 0.4666(4) 0.6570(8) 0.077(3) Uani 1 1 d . . . H27C H 0.3747 0.4319 0.6744 0.093 Uiso 1 1 calc R . . H27D H 0.3287 0.4653 0.6142 0.093 Uiso 1 1 calc R . . C28B C 0.4807(6) 0.4555(4) 0.5902(6) 0.060(3) Uani 1 1 d . . . H28B H 0.4592 0.4237 0.5801 0.072 Uiso 1 1 calc R . . C29B C 0.5543(6) 0.4641(4) 0.5627(6) 0.059(3) Uani 1 1 d . . . C30B C 0.5956(6) 0.5092(4) 0.5733(6) 0.055(2) Uani 1 1 d . . . C31B C 0.6737(7) 0.5135(4) 0.5556(6) 0.065(3) Uani 1 1 d . . . C32B C 0.7097(7) 0.4694(4) 0.5266(7) 0.071(3) Uani 1 1 d . . . H32B H 0.7619 0.4695 0.5180 0.085 Uiso 1 1 calc R . . C33B C 0.6667(8) 0.4262(4) 0.5113(7) 0.073(3) Uani 1 1 d . . . H33B H 0.6901 0.3986 0.4880 0.088 Uiso 1 1 calc R . . C34B C 0.5913(7) 0.4222(4) 0.5289(7) 0.067(3) Uani 1 1 d . . . H34B H 0.5645 0.3923 0.5186 0.081 Uiso 1 1 calc R . . C35B C 0.7991(9) 0.8162(5) 0.6727(10) 0.104(5) Uani 1 1 d . . . H35B H 0.8443 0.8058 0.6973 0.124 Uiso 1 1 calc R . . C36B C 0.7739(9) 0.8635(6) 0.6899(10) 0.105(5) Uani 1 1 d . . . H36B H 0.8018 0.8858 0.7216 0.126 Uiso 1 1 calc R . . C37B C 0.7014(9) 0.8767(5) 0.6560(9) 0.096(4) Uani 1 1 d . . . H37B H 0.6780 0.9072 0.6688 0.115 Uiso 1 1 calc R . . C38B C 0.6673(9) 0.8450(6) 0.6059(9) 0.097(4) Uani 1 1 d . . . H38B H 0.6221 0.8542 0.5801 0.116 Uiso 1 1 calc R . . C39B C 0.7018(9) 0.7964(5) 0.5924(9) 0.093(4) Uani 1 1 d . . . H39B H 0.6771 0.7734 0.5594 0.112 Uiso 1 1 calc R . . N1 N 0.6169(8) 0.0117(5) 0.2635(9) 0.113(4) Uani 1 1 d U . . C1 C 0.5546(10) 0.0059(6) 0.3135(9) 0.102(5) Uani 1 1 d . . . H1 H 0.5424 -0.0253 0.3354 0.122 Uiso 1 1 calc R . . C2 C 0.5117(9) 0.0510(6) 0.3281(9) 0.099(4) Uani 1 1 d . . . H2 H 0.4700 0.0507 0.3603 0.119 Uiso 1 1 calc R . . C3 C 0.5349(9) 0.0947(5) 0.2924(9) 0.094(4) Uani 1 1 d . . . H3 H 0.5082 0.1244 0.3033 0.112 Uiso 1 1 calc R . . C4 C 0.5900(8) 0.0985(5) 0.2455(8) 0.079(4) Uani 1 1 d . . . H4 H 0.6004 0.1295 0.2221 0.095 Uiso 1 1 calc R . . C5 C 0.6301(8) 0.0594(6) 0.2314(9) 0.097(4) Uani 1 1 d . . . H5 H 0.6704 0.0629 0.1979 0.116 Uiso 1 1 calc R . . N2 N 0.0706(9) 0.0918(6) 0.1800(9) 0.132(5) Uani 1 1 d U . . C6 C 0.0964(8) 0.0422(5) 0.1779(9) 0.090(4) Uani 1 1 d U . . H6 H 0.0819 0.0204 0.2172 0.108 Uiso 1 1 calc R . . C7 C 0.1395(8) 0.0237(5) 0.1249(9) 0.095(4) Uani 1 1 d U . . H7 H 0.1523 -0.0107 0.1251 0.114 Uiso 1 1 calc R . . C8 C 0.1653(8) 0.0545(5) 0.0702(9) 0.093(4) Uani 1 1 d U . . H8 H 0.1950 0.0413 0.0313 0.111 Uiso 1 1 calc R . . C9 C 0.1493(8) 0.1025(5) 0.0711(8) 0.085(4) Uani 1 1 d U . . H9 H 0.1722 0.1244 0.0364 0.102 Uiso 1 1 calc R . . C10 C 0.1002(11) 0.1209(7) 0.1213(11) 0.126(6) Uani 1 1 d U . . H10 H 0.0851 0.1547 0.1168 0.151 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 0.0550(2) 0.0577(2) 0.0594(3) -0.0014(2) 0.00017(18) 0.00428(18) Cu1 0.0653(8) 0.0643(8) 0.0630(9) -0.0006(6) -0.0027(7) 0.0101(6) Cu2 0.0567(8) 0.0600(7) 0.0601(8) 0.0023(6) -0.0004(6) 0.0042(6) O1A 0.062(4) 0.062(4) 0.053(4) -0.005(3) -0.001(3) -0.001(3) O2A 0.072(5) 0.054(4) 0.062(5) -0.001(3) -0.004(4) 0.011(3) O3A 0.056(4) 0.056(4) 0.069(5) 0.002(4) 0.001(3) 0.008(3) O4A 0.054(4) 0.058(4) 0.082(5) -0.001(4) -0.004(4) 0.004(3) O5A 0.062(4) 0.062(4) 0.054(4) -0.001(3) 0.000(3) 0.005(3) O6A 0.057(4) 0.066(4) 0.061(5) 0.003(3) -0.001(4) 0.005(3) O7A 0.059(4) 0.065(4) 0.064(5) 0.001(4) 0.004(4) 0.005(3) O8A 0.057(4) 0.063(4) 0.066(5) -0.002(4) 0.003(4) 0.006(3) N1A 0.075(7) 0.077(6) 0.055(6) -0.010(5) 0.001(5) 0.020(5) N2A 0.062(7) 0.087(8) 0.133(11) -0.025(7) -0.014(6) 0.023(6) N3A 0.064(6) 0.047(5) 0.072(7) 0.001(4) 0.000(5) -0.004(4) N4A 0.057(6) 0.066(5) 0.063(6) 0.000(4) 0.000(5) 0.003(4) N5A 0.070(6) 0.071(6) 0.074(7) -0.002(5) -0.011(5) 0.009(5) C1A 0.066(7) 0.066(7) 0.039(6) 0.004(4) 0.000(5) -0.006(5) C2A 0.078(8) 0.046(6) 0.050(7) -0.004(4) 0.006(5) 0.004(5) C3A 0.094(9) 0.070(7) 0.057(7) -0.004(6) -0.003(6) -0.003(7) C4A 0.100(11) 0.064(7) 0.081(9) -0.006(6) -0.005(8) 0.003(7) C5A 0.126(12) 0.047(7) 0.066(8) -0.011(5) 0.001(8) -0.008(7) C6A 0.091(9) 0.072(7) 0.055(7) -0.001(6) -0.002(6) -0.015(6) C7A 0.094(10) 0.063(7) 0.076(9) -0.001(6) 0.000(7) 0.013(7) C8A 0.087(10) 0.100(10) 0.103(11) -0.018(8) -0.030(8) 0.035(8) C9A 0.088(10) 0.135(13) 0.068(9) -0.026(8) -0.019(7) 0.047(9) C10A 0.067(10) 0.120(13) 0.20(2) -0.031(13) -0.006(11) 0.026(9) C11A 0.068(9) 0.096(11) 0.160(16) -0.001(10) -0.029(9) 0.012(8) C12A 0.051(7) 0.067(7) 0.100(10) 0.011(6) 0.005(6) 0.002(5) C13A 0.063(7) 0.071(7) 0.050(6) 0.008(5) 0.003(5) -0.005(5) C14A 0.057(7) 0.061(6) 0.063(7) -0.003(5) 0.003(5) 0.001(5) C15A 0.083(9) 0.057(7) 0.092(10) -0.003(6) 0.002(7) -0.008(6) C16A 0.090(10) 0.067(7) 0.086(9) 0.000(6) -0.006(8) -0.021(7) C17A 0.078(9) 0.074(8) 0.126(13) 0.007(8) -0.004(8) -0.015(7) C18A 0.055(6) 0.054(6) 0.056(6) -0.008(5) 0.000(5) -0.004(4) C19A 0.055(6) 0.048(5) 0.064(7) 0.004(5) 0.002(5) -0.003(4) C20A 0.051(6) 0.056(6) 0.067(7) -0.002(5) -0.004(5) 0.000(5) C21A 0.057(6) 0.066(7) 0.070(8) -0.007(6) 0.002(6) 0.005(5) C22A 0.056(7) 0.079(7) 0.057(7) 0.005(6) 0.006(5) -0.004(5) C23A 0.062(7) 0.068(7) 0.063(7) 0.003(5) -0.004(5) 0.000(5) C24A 0.056(6) 0.060(6) 0.069(8) -0.001(5) 0.004(6) 0.000(5) C25A 0.054(7) 0.065(7) 0.083(9) 0.013(6) -0.004(6) 0.003(5) C26A 0.059(7) 0.072(7) 0.067(8) 0.008(6) -0.006(6) 0.003(5) C27A 0.059(7) 0.070(7) 0.062(7) 0.004(5) 0.000(5) 0.006(5) C28A 0.070(8) 0.077(8) 0.068(8) 0.000(6) -0.004(6) -0.006(6) C29A 0.063(7) 0.071(7) 0.070(8) -0.004(6) -0.003(6) 0.009(5) C30A 0.062(7) 0.066(7) 0.057(7) -0.006(5) 0.005(5) -0.001(5) C31A 0.041(5) 0.059(6) 0.069(7) 0.004(5) -0.002(5) -0.005(4) C32A 0.077(8) 0.084(8) 0.055(7) 0.000(6) 0.002(6) 0.005(6) C33A 0.074(8) 0.098(9) 0.064(8) -0.012(7) 0.010(7) 0.006(7) C34A 0.094(10) 0.109(10) 0.050(7) -0.024(7) -0.014(7) 0.019(8) C35A 0.087(9) 0.064(7) 0.072(9) -0.008(6) -0.012(7) 0.002(6) C36A 0.084(9) 0.079(8) 0.060(8) 0.002(6) 0.005(7) 0.002(6) C37A 0.071(8) 0.090(8) 0.049(7) 0.012(6) 0.005(6) 0.017(6) C38A 0.099(10) 0.060(7) 0.065(8) -0.009(6) -0.002(7) 0.015(6) C39A 0.076(8) 0.069(7) 0.065(8) 0.010(6) -0.010(6) 0.002(6) U2 0.0626(3) 0.0611(2) 0.0669(3) -0.0007(2) 0.0018(2) 0.0021(2) Cu3 0.0611(8) 0.0767(9) 0.0718(10) -0.0037(7) -0.0004(7) -0.0030(7) Cu4 0.0644(8) 0.0593(7) 0.0642(9) 0.0001(6) 0.0034(6) 0.0042(6) O1B 0.063(5) 0.059(4) 0.069(5) -0.002(4) 0.004(4) -0.002(3) O2B 0.056(4) 0.068(4) 0.069(5) 0.007(4) -0.010(4) 0.001(3) O3B 0.064(5) 0.077(5) 0.068(5) 0.000(4) 0.003(4) 0.000(4) O4B 0.084(6) 0.068(5) 0.063(5) -0.001(4) 0.003(4) 0.003(4) O5B 0.065(5) 0.071(5) 0.071(5) -0.004(4) 0.007(4) 0.006(4) O6B 0.069(5) 0.063(4) 0.074(5) -0.003(4) 0.004(4) 0.003(4) O7B 0.063(5) 0.059(4) 0.067(5) -0.004(3) 0.007(4) 0.005(3) O8B 0.064(5) 0.070(5) 0.072(5) 0.000(4) 0.004(4) 0.002(4) N1B 0.057(5) 0.069(6) 0.064(6) -0.004(5) 0.001(5) -0.002(4) N2B 0.070(7) 0.092(7) 0.077(8) -0.003(6) -0.003(5) 0.009(5) N3B 0.068(6) 0.069(6) 0.062(6) 0.003(5) -0.001(5) 0.006(5) N4B 0.060(6) 0.064(5) 0.068(6) 0.004(5) -0.002(5) 0.002(4) N5B 0.091(8) 0.075(7) 0.085(8) -0.006(6) 0.000(7) 0.005(6) C1B 0.067(7) 0.053(6) 0.073(8) -0.006(5) -0.001(6) 0.004(5) C2B 0.056(7) 0.058(6) 0.073(8) -0.001(5) -0.008(6) 0.006(5) C3B 0.064(7) 0.061(6) 0.065(7) 0.009(5) -0.006(6) -0.004(5) C4B 0.059(7) 0.055(6) 0.095(10) 0.005(6) 0.010(6) -0.001(5) C5B 0.082(8) 0.067(7) 0.067(8) 0.010(6) -0.008(6) 0.003(6) C6B 0.054(6) 0.069(7) 0.078(8) 0.003(6) -0.007(6) 0.006(5) C7B 0.063(7) 0.047(6) 0.084(9) 0.004(5) -0.001(6) 0.003(5) C8B 0.065(8) 0.103(10) 0.095(11) -0.020(8) 0.013(7) -0.022(7) C9B 0.060(8) 0.106(10) 0.090(11) 0.002(8) -0.008(7) -0.007(7) C10B 0.065(8) 0.131(12) 0.090(11) 0.001(9) 0.001(7) -0.018(8) C11B 0.067(8) 0.075(8) 0.081(9) -0.002(7) -0.012(7) 0.009(6) C12B 0.079(8) 0.064(7) 0.072(8) -0.004(6) -0.010(7) 0.013(6) C13B 0.070(8) 0.047(6) 0.093(10) -0.003(6) -0.001(7) 0.014(5) C14B 0.080(8) 0.062(7) 0.060(7) -0.002(6) -0.001(6) 0.004(6) C15B 0.089(9) 0.065(7) 0.082(9) 0.000(6) -0.006(7) 0.003(6) C16B 0.112(11) 0.059(7) 0.078(9) 0.002(6) -0.023(8) 0.018(7) C17B 0.091(9) 0.065(7) 0.067(8) -0.003(6) -0.024(7) 0.014(6) C18B 0.083(8) 0.051(6) 0.067(8) -0.006(5) -0.007(6) 0.008(5) C19B 0.067(7) 0.064(7) 0.056(7) -0.011(5) 0.001(5) 0.012(5) C20B 0.069(7) 0.067(7) 0.056(7) 0.003(5) 0.001(6) 0.006(6) C21B 0.057(7) 0.088(8) 0.062(8) 0.008(6) 0.000(5) 0.012(6) C22B 0.089(9) 0.076(8) 0.066(8) -0.012(6) -0.004(7) 0.013(7) C23B 0.069(8) 0.082(8) 0.069(8) -0.002(6) -0.009(6) 0.002(6) C24B 0.065(7) 0.082(8) 0.060(7) 0.005(6) -0.002(5) 0.013(6) C25B 0.057(7) 0.074(7) 0.081(9) -0.006(6) 0.010(6) 0.005(5) C26B 0.083(9) 0.075(8) 0.065(8) -0.003(6) -0.001(6) 0.000(6) C27B 0.073(8) 0.070(7) 0.089(10) -0.001(6) 0.000(7) 0.000(6) C28B 0.067(7) 0.058(6) 0.055(7) 0.010(5) 0.004(5) 0.003(5) C29B 0.072(7) 0.062(6) 0.044(6) 0.005(5) 0.002(5) 0.009(5) C30B 0.053(6) 0.055(6) 0.055(6) 0.000(5) -0.009(5) 0.009(5) C31B 0.084(8) 0.057(6) 0.055(7) 0.001(5) -0.004(6) 0.010(6) C32B 0.067(8) 0.080(8) 0.067(8) 0.000(6) 0.005(6) 0.018(6) C33B 0.097(10) 0.053(6) 0.070(8) -0.006(5) 0.000(7) 0.012(6) C34B 0.073(8) 0.059(6) 0.070(8) 0.002(5) -0.002(6) 0.015(5) C35B 0.094(11) 0.077(9) 0.141(15) -0.023(9) 0.019(10) -0.021(8) C36B 0.100(12) 0.095(11) 0.120(13) -0.011(9) -0.004(10) -0.007(9) C37B 0.111(12) 0.074(9) 0.105(12) -0.015(8) 0.023(9) -0.001(8) C38B 0.087(10) 0.100(10) 0.105(12) 0.001(9) 0.011(9) 0.009(8) C39B 0.119(12) 0.064(8) 0.097(11) -0.013(7) 0.003(9) 0.002(8) N1 0.114(8) 0.109(7) 0.113(8) -0.018(7) -0.019(7) 0.002(6) C1 0.144(15) 0.083(10) 0.078(10) 0.018(8) -0.017(10) -0.015(9) C2 0.102(11) 0.096(11) 0.100(12) 0.006(9) 0.004(9) -0.007(9) C3 0.118(12) 0.074(9) 0.089(11) -0.019(8) 0.005(9) -0.002(8) C4 0.101(10) 0.060(7) 0.077(9) -0.017(6) 0.021(8) -0.009(7) C5 0.086(10) 0.107(11) 0.097(11) 0.005(9) -0.020(8) -0.011(9) N2 0.153(9) 0.120(8) 0.124(8) 0.007(7) 0.032(7) 0.006(7) C6 0.107(8) 0.070(6) 0.095(8) -0.002(6) 0.017(7) -0.003(6) C7 0.097(8) 0.077(7) 0.113(8) 0.008(6) 0.022(7) 0.009(6) C8 0.103(8) 0.088(7) 0.089(8) -0.005(6) 0.016(6) 0.005(6) C9 0.083(7) 0.083(7) 0.089(7) -0.002(6) 0.019(6) -0.002(6) C10 0.139(9) 0.121(9) 0.119(9) 0.018(8) 0.040(8) -0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O5A 2.259(7) . ? U1 O8A 2.291(7) . ? U1 O4A 2.301(7) . ? U1 O1A 2.319(7) . ? U1 O2A 2.442(6) . ? U1 O6A 2.455(7) . ? U1 O7A 2.466(7) . ? U1 O3A 2.465(7) . ? U1 Cu1 3.6478(14) . ? U1 Cu2 3.6709(13) . ? Cu1 O2A 1.952(7) . ? Cu1 O3A 1.951(6) . ? Cu1 N1A 1.974(9) . ? Cu1 N2A 2.005(11) . ? Cu1 N5A 2.280(10) . ? Cu2 O6A 1.912(7) . ? Cu2 O7A 1.923(7) . ? Cu2 N4A 1.971(9) . ? Cu2 N3A 1.983(9) . ? O1A C1A 1.316(12) . ? O2A C2A 1.322(11) . ? O2A O3A 2.427(10) . ? O2A N1A 2.805(11) . ? O3A C13A 1.345(12) . ? O3A N2A 2.843(12) . ? O4A C14A 1.343(12) . ? O5A C18A 1.322(12) . ? O6A C19A 1.332(12) . ? O6A O7A 2.358(11) . ? O6A N3A 2.836(11) . ? O7A C30A 1.352(12) . ? O7A N4A 2.794(11) . ? O8A C31A 1.344(12) . ? N1A C7A 1.282(15) . ? N1A C8A 1.460(15) . ? N1A N2A 3.015(16) . ? N2A C11A 1.246(16) . ? N2A C10A 1.467(16) . ? N3A C24A 1.304(14) . ? N3A C25A 1.464(13) . ? N3A N4A 3.014(14) . ? N4A C28A 1.284(14) . ? N4A C27A 1.460(13) . ? N5A C35A 1.325(15) . ? N5A C39A 1.339(14) . ? C1A C6A 1.385(14) . ? C1A C2A 1.447(15) . ? C2A C3A 1.377(15) . ? C3A C4A 1.396(16) . ? C3A C7A 1.445(17) . ? C4A C5A 1.374(18) . ? C5A C6A 1.396(16) . ? C8A C9A 1.500(17) . ? C9A C10A 1.48(2) . ? C11A C12A 1.461(17) . ? C12A C13A 1.369(15) . ? C12A C17A 1.409(16) . ? C13A C14A 1.388(14) . ? C14A C15A 1.407(15) . ? C15A C16A 1.378(17) . ? C16A C17A 1.366(17) . ? C18A C23A 1.380(15) . ? C18A C19A 1.434(14) . ? C19A C20A 1.392(14) . ? C20A C24A 1.430(14) . ? C20A C21A 1.426(15) . ? C21A C22A 1.350(14) . ? C22A C23A 1.434(15) . ? C25A C26A 1.515(15) . ? C26A C27A 1.535(15) . ? C28A C29A 1.429(16) . ? C29A C30A 1.404(15) . ? C29A C34A 1.455(16) . ? C30A C31A 1.420(14) . ? C31A C32A 1.384(15) . ? C32A C33A 1.396(16) . ? C33A C34A 1.360(16) . ? C35A C36A 1.370(17) . ? C36A C37A 1.357(16) . ? C37A C38A 1.376(16) . ? C38A C39A 1.357(16) . ? U2 O5B 2.272(7) . ? U2 O1B 2.295(8) . ? U2 O4B 2.305(8) . ? U2 O8B 2.313(7) . ? U2 O3B 2.440(8) . ? U2 O2B 2.441(7) . ? U2 O7B 2.457(7) . ? U2 O6B 2.463(7) . ? U2 Cu4 3.6607(14) . ? U2 Cu3 3.6662(15) . ? Cu3 O2B 1.955(7) . ? Cu3 O3B 1.957(8) . ? Cu3 N1B 2.000(10) . ? Cu3 N2B 2.001(10) . ? Cu3 N5B 2.348(10) . ? Cu4 O6B 1.913(7) . ? Cu4 O7B 1.928(7) . ? Cu4 N3B 1.963(9) . ? Cu4 N4B 1.962(9) . ? O1B C1B 1.342(13) . ? O2B C2B 1.326(13) . ? O2B O3B 2.394(11) . ? O2B N1B 2.822(11) . ? O3B C13B 1.317(14) . ? O3B N2B 2.844(13) . ? O4B C14B 1.337(13) . ? O5B C18B 1.318(13) . ? O6B C19B 1.347(11) . ? O6B O7B 2.378(10) . ? O6B N3B 2.782(12) . ? O7B C30B 1.334(11) . ? O7B N4B 2.805(11) . ? O8B C31B 1.333(12) . ? N1B C7B 1.268(14) . ? N1B C8B 1.520(14) . ? N1B N2B 3.040(15) . ? N2B C11B 1.311(15) . ? N2B C10B 1.483(16) . ? N3B C24B 1.300(13) . ? N3B C25B 1.465(14) . ? N3B N4B 2.996(13) . ? N4B C28B 1.321(13) . ? N4B C27B 1.495(14) . ? N5B C39B 1.293(17) . ? N5B C35B 1.306(17) . ? C1B C6B 1.394(15) . ? C1B C2B 1.407(15) . ? C2B C3B 1.401(15) . ? C3B C4B 1.418(16) . ? C3B C7B 1.457(15) . ? C4B C5B 1.371(15) . ? C5B C6B 1.392(16) . ? C8B C9B 1.490(17) . ? C9B C10B 1.494(18) . ? C11B C12B 1.445(17) . ? C12B C13B 1.378(16) . ? C12B C17B 1.416(16) . ? C13B C14B 1.434(17) . ? C14B C15B 1.384(16) . ? C15B C16B 1.405(17) . ? C16B C17B 1.335(18) . ? C18B C23B 1.387(15) . ? C18B C19B 1.437(15) . ? C19B C20B 1.362(15) . ? C20B C24B 1.431(15) . ? C20B C21B 1.430(15) . ? C21B C22B 1.380(16) . ? C22B C23B 1.368(16) . ? C25B C26B 1.504(15) . ? C26B C27B 1.510(16) . ? C28B C29B 1.405(15) . ? C29B C30B 1.395(14) . ? C29B C34B 1.412(14) . ? C30B C31B 1.415(15) . ? C31B C32B 1.417(15) . ? C32B C33B 1.384(16) . ? C33B C34B 1.367(16) . ? C35B C36B 1.354(18) . ? C36B C37B 1.42(2) . ? C37B C38B 1.331(19) . ? C38B C39B 1.433(18) . ? N1 C5 1.392(19) . ? N1 C1 1.422(19) . ? C1 C2 1.43(2) . ? C2 C3 1.372(19) . ? C3 C4 1.283(18) . ? C4 C5 1.272(18) . ? N2 C10 1.383(19) . ? N2 C6 1.380(17) . ? C6 C7 1.299(18) . ? C7 C8 1.333(18) . ? C8 C9 1.293(17) . ? C9 C10 1.33(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 O5A U1 O8A 169.5(2) . . ? O5A U1 O4A 91.1(3) . . ? O8A U1 O4A 95.7(3) . . ? O5A U1 O1A 87.1(2) . . ? O8A U1 O1A 87.6(2) . . ? O4A U1 O1A 169.2(2) . . ? O5A U1 O2A 87.0(2) . . ? O8A U1 O2A 82.5(2) . . ? O4A U1 O2A 124.7(2) . . ? O1A U1 O2A 65.9(2) . . ? O5A U1 O6A 66.2(2) . . ? O8A U1 O6A 123.0(2) . . ? O4A U1 O6A 78.3(2) . . ? O1A U1 O6A 91.3(2) . . ? O2A U1 O6A 146.1(2) . . ? O5A U1 O7A 122.5(2) . . ? O8A U1 O7A 65.9(2) . . ? O4A U1 O7A 87.6(2) . . ? O1A U1 O7A 84.4(2) . . ? O2A U1 O7A 137.5(2) . . ? O6A U1 O7A 57.3(2) . . ? O5A U1 O3A 89.9(2) . . ? O8A U1 O3A 85.6(2) . . ? O4A U1 O3A 65.5(2) . . ? O1A U1 O3A 125.1(2) . . ? O2A U1 O3A 59.3(2) . . ? O6A U1 O3A 136.2(2) . . ? O7A U1 O3A 138.9(2) . . ? O2A Cu1 O3A 76.9(3) . . ? O2A Cu1 N1A 91.2(4) . . ? O3A Cu1 N1A 161.7(4) . . ? O2A Cu1 N2A 167.7(4) . . ? O3A Cu1 N2A 91.9(4) . . ? N1A Cu1 N2A 98.5(4) . . ? O2A Cu1 N5A 91.1(3) . . ? O3A Cu1 N5A 97.0(3) . . ? N1A Cu1 N5A 97.0(4) . . ? N2A Cu1 N5A 95.1(5) . . ? O6A Cu2 O7A 75.9(3) . . ? O6A Cu2 N4A 166.8(3) . . ? O7A Cu2 N4A 91.7(3) . . ? O6A Cu2 N3A 93.5(3) . . ? O7A Cu2 N3A 167.5(3) . . ? N4A Cu2 N3A 99.3(4) . . ? Cu1 O2A U1 111.7(3) . . ? Cu1 O3A U1 110.8(3) . . ? Cu2 O6A U1 113.8(3) . . ? Cu2 O7A U1 112.9(3) . . ? C7A N1A C8A 116.1(10) . . ? C11A N2A C10A 116.4(12) . . ? C24A N3A C25A 114.5(10) . . ? C28A N4A C27A 117.1(10) . . ? C35A N5A C39A 116.5(11) . . ? O1A C1A C6A 125.8(11) . . ? O1A C1A C2A 118.4(9) . . ? C6A C1A C2A 115.8(10) . . ? O2A C2A C3A 124.4(11) . . ? O2A C2A C1A 113.0(8) . . ? C3A C2A C1A 122.5(10) . . ? C2A C3A C4A 118.2(12) . . ? C2A C3A C7A 123.9(11) . . ? C4A C3A C7A 117.9(12) . . ? C5A C4A C3A 121.4(12) . . ? C4A C5A C6A 119.6(11) . . ? C5A C6A C1A 122.3(12) . . ? N1A C7A C3A 125.6(11) . . ? N1A C8A C9A 114.6(11) . . ? C10A C9A C8A 111.2(14) . . ? N2A C10A C9A 114.8(13) . . ? N2A C11A C12A 129.5(13) . . ? C13A C12A C17A 117.5(11) . . ? C13A C12A C11A 124.4(12) . . ? C17A C12A C11A 118.1(12) . . ? O3A C13A C12A 121.3(10) . . ? O3A C13A C14A 116.1(9) . . ? C12A C13A C14A 122.6(10) . . ? O4A C14A C13A 116.6(9) . . ? O4A C14A C15A 124.7(10) . . ? C13A C14A C15A 118.7(11) . . ? C16A C15A C14A 119.2(11) . . ? C17A C16A C15A 121.1(12) . . ? C16A C17A C12A 120.9(12) . . ? O5A C18A C23A 126.5(10) . . ? O5A C18A C19A 117.1(9) . . ? C23A C18A C19A 116.4(10) . . ? O6A C19A C20A 122.9(9) . . ? O6A C19A C18A 114.1(9) . . ? C20A C19A C18A 122.9(10) . . ? C19A C20A C24A 123.6(11) . . ? C19A C20A C21A 117.8(10) . . ? C24A C20A C21A 118.6(10) . . ? C22A C21A C20A 120.8(10) . . ? C21A C22A C23A 120.5(11) . . ? C18A C23A C22A 121.4(10) . . ? N3A C24A C20A 128.4(11) . . ? N3A C25A C26A 113.3(10) . . ? C25A C26A C27A 114.2(9) . . ? N4A C27A C26A 110.7(9) . . ? N4A C28A C29A 127.7(12) . . ? C30A C29A C28A 123.6(11) . . ? C30A C29A C34A 117.1(10) . . ? C28A C29A C34A 119.2(11) . . ? O7A C30A C29A 121.7(10) . . ? O7A C30A C31A 116.5(10) . . ? C29A C30A C31A 121.7(10) . . ? O8A C31A C32A 126.4(10) . . ? O8A C31A C30A 115.0(10) . . ? C32A C31A C30A 118.5(10) . . ? C31A C32A C33A 121.0(11) . . ? C34A C33A C32A 121.3(12) . . ? C33A C34A C29A 120.2(11) . . ? N5A C35A C36A 124.4(12) . . ? C37A C36A C35A 118.0(12) . . ? C36A C37A C38A 119.0(12) . . ? C39A C38A C37A 119.3(11) . . ? N5A C39A C38A 122.8(12) . . ? O5B U2 O1B 86.8(3) . . ? O5B U2 O4B 91.0(3) . . ? O1B U2 O4B 168.4(3) . . ? O5B U2 O8B 170.4(3) . . ? O1B U2 O8B 91.4(3) . . ? O4B U2 O8B 92.6(3) . . ? O5B U2 O3B 88.3(3) . . ? O1B U2 O3B 125.2(3) . . ? O4B U2 O3B 66.1(3) . . ? O8B U2 O3B 85.0(3) . . ? O5B U2 O2B 82.8(3) . . ? O1B U2 O2B 66.5(2) . . ? O4B U2 O2B 124.5(3) . . ? O8B U2 O2B 87.8(3) . . ? O3B U2 O2B 58.7(3) . . ? O5B U2 O7B 123.7(3) . . ? O1B U2 O7B 85.3(2) . . ? O4B U2 O7B 86.4(3) . . ? O8B U2 O7B 65.5(2) . . ? O3B U2 O7B 138.9(2) . . ? O2B U2 O7B 141.0(2) . . ? O5B U2 O6B 66.2(3) . . ? O1B U2 O6B 87.8(3) . . ? O4B U2 O6B 80.9(3) . . ? O8B U2 O6B 123.2(2) . . ? O3B U2 O6B 138.0(3) . . ? O2B U2 O6B 141.0(2) . . ? O7B U2 O6B 57.8(2) . . ? O2B Cu3 O3B 75.5(3) . . ? O2B Cu3 N1B 91.1(3) . . ? O3B Cu3 N1B 163.0(4) . . ? O2B Cu3 N2B 162.3(4) . . ? O3B Cu3 N2B 91.8(4) . . ? N1B Cu3 N2B 98.9(4) . . ? O2B Cu3 N5B 97.7(4) . . ? O3B Cu3 N5B 101.2(4) . . ? N1B Cu3 N5B 90.7(4) . . ? N2B Cu3 N5B 96.8(4) . . ? O6B Cu4 O7B 76.5(3) . . ? O6B Cu4 N3B 91.7(4) . . ? O7B Cu4 N3B 168.1(4) . . ? O6B Cu4 N4B 168.7(4) . . ? O7B Cu4 N4B 92.3(3) . . ? N3B Cu4 N4B 99.5(4) . . ? Cu3 O2B U2 112.6(3) . . ? Cu3 O3B U2 112.5(4) . . ? Cu4 O6B U2 112.9(3) . . ? Cu4 O7B U2 112.6(3) . . ? C7B N1B C8B 114.4(11) . . ? C11B N2B C10B 116.7(11) . . ? C24B N3B C25B 115.1(10) . . ? C28B N4B C27B 114.2(9) . . ? C39B N5B C35B 118.1(13) . . ? O1B C1B C6B 124.8(10) . . ? O1B C1B C2B 117.0(10) . . ? C6B C1B C2B 118.2(11) . . ? O2B C2B C3B 122.9(10) . . ? O2B C2B C1B 116.1(10) . . ? C3B C2B C1B 121.1(11) . . ? C2B C3B C4B 118.4(10) . . ? C2B C3B C7B 123.5(10) . . ? C4B C3B C7B 118.1(10) . . ? C5B C4B C3B 120.9(11) . . ? C4B C5B C6B 119.7(11) . . ? C5B C6B C1B 121.7(11) . . ? N1B C7B C3B 127.2(11) . . ? C9B C8B N1B 110.6(11) . . ? C8B C9B C10B 116.1(12) . . ? N2B C10B C9B 114.5(11) . . ? N2B C11B C12B 128.4(12) . . ? C13B C12B C17B 119.5(13) . . ? C13B C12B C11B 122.8(12) . . ? C17B C12B C11B 117.7(12) . . ? O3B C13B C12B 124.2(12) . . ? O3B C13B C14B 116.1(11) . . ? C12B C13B C14B 119.7(12) . . ? O4B C14B C15B 125.9(11) . . ? O4B C14B C13B 115.4(10) . . ? C15B C14B C13B 118.6(12) . . ? C14B C15B C16B 120.5(13) . . ? C17B C16B C15B 120.5(13) . . ? C16B C17B C12B 121.1(12) . . ? O5B C18B C23B 126.5(11) . . ? O5B C18B C19B 117.3(9) . . ? C23B C18B C19B 116.2(11) . . ? O6B C19B C20B 123.5(10) . . ? O6B C19B C18B 114.1(10) . . ? C20B C19B C18B 122.4(10) . . ? C19B C20B C24B 122.9(10) . . ? C19B C20B C21B 118.6(10) . . ? C24B C20B C21B 118.4(11) . . ? C22B C21B C20B 119.5(11) . . ? C23B C22B C21B 120.6(12) . . ? C22B C23B C18B 122.6(12) . . ? N3B C24B C20B 127.8(11) . . ? N3B C25B C26B 112.4(9) . . ? C25B C26B C27B 112.9(10) . . ? N4B C27B C26B 113.3(10) . . ? N4B C28B C29B 126.4(10) . . ? C30B C29B C28B 124.6(10) . . ? C30B C29B C34B 118.3(10) . . ? C28B C29B C34B 116.8(10) . . ? O7B C30B C29B 122.6(10) . . ? O7B C30B C31B 114.7(9) . . ? C29B C30B C31B 122.7(9) . . ? O8B C31B C30B 117.3(9) . . ? O8B C31B C32B 125.8(11) . . ? C30B C31B C32B 116.9(10) . . ? C33B C32B C31B 119.7(11) . . ? C32B C33B C34B 122.8(11) . . ? C33B C34B C29B 119.3(11) . . ? N5B C35B C36B 126.8(16) . . ? C35B C36B C37B 115.0(15) . . ? C38B C37B C36B 119.6(14) . . ? C37B C38B C39B 118.6(15) . . ? N5B C39B C38B 121.6(14) . . ? C5 N1 C1 118.6(14) . . ? N1 C1 C2 115.8(13) . . ? C3 C2 C1 116.8(15) . . ? C4 C3 C2 126.1(14) . . ? C5 C4 C3 119.2(14) . . ? C4 C5 N1 123.4(16) . . ? C10 N2 C6 111.7(15) . . ? C7 C6 N2 124.7(14) . . ? C6 C7 C8 119.4(14) . . ? C9 C8 C7 120.3(15) . . ? C8 C9 C10 120.4(15) . . ? N2 C10 C9 123.0(17) . . ? #===END data_[(ZnL^2^(py))~2~U].2.5py _database_code_CSD 208959 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56.50 H50.50 N8.50 O8 U Zn2' _chemical_formula_weight 1345.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7915(10) _cell_length_b 13.6115(10) _cell_length_c 16.3246(10) _cell_angle_alpha 95.631(5) _cell_angle_beta 93.623(5) _cell_angle_gamma 97.892(4) _cell_volume 2574.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17748 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light brown' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method ? _exptl_crystal_F_000 1330 _exptl_absorpt_coefficient_mu 4.127 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.370 _exptl_absorpt_correction_T_max 0.780 _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 17748 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9029 _reflns_number_gt 7518 _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. One pyridine molecule is disordered over a symmetry centre and two atoms in each Schiff base bridge are disordered over two positions which have been refined with occupancy parameters constrained to sum to unity and some restraints on 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 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 involve some atoms of the disordered bridges (C9B, C26A, C27B), which may indicate an imperfect description of the disorder. 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^)+(0.0167P)^2^+2.6156P] 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 9029 _refine_ls_number_parameters 685 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.719 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.107 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U U 0.107185(18) 0.731780(15) 0.281688(12) 0.02818(7) Uani 1 1 d . . . Zn1 Zn -0.01872(5) 0.68437(4) 0.47732(4) 0.02947(14) Uani 1 1 d . . . Zn2 Zn 0.18981(6) 0.80843(5) 0.08058(4) 0.03646(16) Uani 1 1 d . . . O1 O -0.0375(3) 0.6345(3) 0.1954(2) 0.0337(9) Uani 1 1 d . . . O2 O -0.0400(3) 0.6411(3) 0.3532(2) 0.0295(8) Uani 1 1 d . . . O3 O 0.1295(3) 0.7382(3) 0.4309(2) 0.0316(8) Uani 1 1 d . . . O4 O 0.2776(3) 0.8221(3) 0.3406(2) 0.0332(8) Uani 1 1 d . . . O5 O -0.0029(3) 0.8575(3) 0.3110(2) 0.0353(9) Uani 1 1 d . . . O6 O 0.1152(3) 0.8545(3) 0.1832(2) 0.0326(8) Uani 1 1 d . . . O7 O 0.2171(3) 0.7097(3) 0.1618(2) 0.0346(9) Uani 1 1 d . . . O8 O 0.2036(3) 0.5954(3) 0.2791(2) 0.0345(9) Uani 1 1 d . . . N1 N -0.1386(4) 0.5628(4) 0.4923(3) 0.0398(12) Uani 1 1 d D . . N2 N 0.0670(4) 0.6994(3) 0.5935(3) 0.0323(10) Uani 1 1 d . . . N3 N 0.1976(5) 0.9516(4) 0.0464(3) 0.0473(13) Uani 1 1 d . . . N4 N 0.3284(5) 0.7671(4) 0.0206(3) 0.0555(15) Uani 1 1 d D . . C1 C -0.1201(5) 0.5720(4) 0.2235(4) 0.0328(12) Uani 1 1 d . . . C2 C -0.1217(4) 0.5756(4) 0.3095(3) 0.0273(11) Uani 1 1 d . . . C3 C -0.2045(5) 0.5123(4) 0.3465(4) 0.0328(12) Uani 1 1 d . . . C4 C -0.2846(5) 0.4442(4) 0.2933(4) 0.0372(13) Uani 1 1 d . . . H4 H -0.3399 0.4014 0.3158 0.045 Uiso 1 1 calc R . . C5 C -0.2819(5) 0.4402(4) 0.2095(4) 0.0383(14) Uani 1 1 d . . . H5 H -0.3348 0.3943 0.1757 0.046 Uiso 1 1 calc R . . C6 C -0.2005(5) 0.5044(4) 0.1735(4) 0.0357(13) Uani 1 1 d . . . H6 H -0.2004 0.5017 0.1164 0.043 Uiso 1 1 calc R . . C7 C -0.2063(5) 0.5090(4) 0.4346(4) 0.0351(13) Uani 1 1 d . . . H7 H -0.2628 0.4626 0.4519 0.042 Uiso 1 1 calc R . . C8A C -0.1456(8) 0.5264(7) 0.5756(4) 0.036(2) Uiso 0.623(12) 1 d PDU . . C9A C -0.1233(7) 0.6179(6) 0.6395(5) 0.038(2) Uiso 0.623(12) 1 d PDU . . C8B C -0.1732(13) 0.5695(12) 0.5806(6) 0.033(3) Uiso 0.377(12) 1 d PDU . . C9B C -0.0695(12) 0.5686(8) 0.6407(9) 0.035(4) Uiso 0.377(12) 1 d PDU . . C10 C 0.0022(5) 0.6674(5) 0.6635(4) 0.0421(14) Uani 1 1 d D . . C11 C 0.1720(5) 0.7378(4) 0.6109(3) 0.0328(12) Uani 1 1 d . . . H11 H 0.1990 0.7408 0.6660 0.039 Uiso 1 1 calc R . . C12 C 0.2549(5) 0.7777(4) 0.5557(3) 0.0305(12) Uani 1 1 d . . . C13 C 0.2297(4) 0.7781(4) 0.4704(3) 0.0287(11) Uani 1 1 d . . . C14 C 0.3117(5) 0.8224(4) 0.4196(3) 0.0307(12) Uani 1 1 d . . . C15 C 0.4193(5) 0.8640(4) 0.4568(4) 0.0355(13) Uani 1 1 d . . . H15 H 0.4743 0.8930 0.4246 0.043 Uiso 1 1 calc R . . C16 C 0.4468(5) 0.8634(4) 0.5411(4) 0.0388(14) Uani 1 1 d . . . H16 H 0.5197 0.8910 0.5643 0.047 Uiso 1 1 calc R . . C17 C 0.3668(5) 0.8222(4) 0.5899(4) 0.0358(13) Uani 1 1 d . . . H17 H 0.3856 0.8231 0.6462 0.043 Uiso 1 1 calc R . . C18 C -0.0108(5) 0.9301(4) 0.2633(3) 0.0343(13) Uani 1 1 d . . . C19 C 0.0541(5) 0.9295(4) 0.1937(3) 0.0349(13) Uani 1 1 d . . . C20 C 0.0568(6) 1.0052(4) 0.1406(4) 0.0443(15) Uani 1 1 d . . . C21 C -0.0143(7) 1.0798(5) 0.1573(4) 0.0558(19) Uani 1 1 d . . . H21 H -0.0154 1.1303 0.1229 0.067 Uiso 1 1 calc R . . C22 C -0.0807(6) 1.0792(5) 0.2225(4) 0.0520(17) Uani 1 1 d . . . H22 H -0.1265 1.1290 0.2319 0.062 Uiso 1 1 calc R . . C23 C -0.0807(5) 1.0038(4) 0.2759(4) 0.0419(14) Uani 1 1 d . . . H23 H -0.1276 1.0033 0.3196 0.050 Uiso 1 1 calc R . . C24 C 0.1314(7) 1.0130(5) 0.0741(4) 0.0528(18) Uani 1 1 d . . . H24 H 0.1319 1.0704 0.0475 0.063 Uiso 1 1 calc R . . C25 C 0.2742(7) 0.9827(5) -0.0200(4) 0.068(2) Uani 1 1 d D . . C26A C 0.3809(10) 0.9337(8) -0.0250(9) 0.062(4) Uiso 0.554(13) 1 d PDU . . C27A C 0.3505(14) 0.8231(8) -0.0538(7) 0.059(3) Uiso 0.554(13) 1 d PDU . . C26B C 0.3086(13) 0.8901(9) -0.0703(9) 0.055(4) Uiso 0.446(13) 1 d PDU . . C27B C 0.3959(12) 0.8314(11) -0.0330(10) 0.059(4) Uiso 0.446(13) 1 d PDU . . C28 C 0.3810(6) 0.6950(5) 0.0356(4) 0.0490(17) Uani 1 1 d . . . H28 H 0.4394 0.6839 0.0015 0.059 Uiso 1 1 calc R . . C29 C 0.3633(5) 0.6282(5) 0.0976(4) 0.0437(15) Uani 1 1 d . . . C30 C 0.2841(5) 0.6394(4) 0.1587(3) 0.0339(13) Uani 1 1 d . . . C31 C 0.2770(5) 0.5765(4) 0.2231(4) 0.0354(13) Uani 1 1 d . . . C32 C 0.3468(5) 0.5018(5) 0.2253(4) 0.0427(15) Uani 1 1 d . . . H32 H 0.3418 0.4599 0.2670 0.051 Uiso 1 1 calc R . . C33 C 0.4248(5) 0.4897(5) 0.1645(4) 0.0473(16) Uani 1 1 d . . . H33 H 0.4708 0.4396 0.1660 0.057 Uiso 1 1 calc R . . C34 C 0.4332(5) 0.5517(5) 0.1031(4) 0.0501(18) Uani 1 1 d . . . H34 H 0.4861 0.5434 0.0640 0.060 Uiso 1 1 calc R . . N5 N -0.1126(4) 0.8011(3) 0.4846(3) 0.0310(10) Uani 1 1 d . . . C35 C -0.2041(5) 0.7977(4) 0.4297(4) 0.0381(14) Uani 1 1 d . . . H35 H -0.2254 0.7404 0.3930 0.046 Uiso 1 1 calc R . . C36 C -0.2666(5) 0.8745(4) 0.4257(4) 0.0389(14) Uani 1 1 d . . . H36 H -0.3289 0.8695 0.3869 0.047 Uiso 1 1 calc R . . C37 C -0.2360(5) 0.9605(4) 0.4807(4) 0.0365(13) Uani 1 1 d . . . H37 H -0.2782 1.0133 0.4800 0.044 Uiso 1 1 calc R . . C38 C -0.1414(5) 0.9655(4) 0.5363(4) 0.0376(13) Uani 1 1 d . . . H38 H -0.1176 1.0224 0.5730 0.045 Uiso 1 1 calc R . . C39 C -0.0834(5) 0.8850(4) 0.5362(4) 0.0391(14) Uani 1 1 d . . . H39 H -0.0203 0.8886 0.5741 0.047 Uiso 1 1 calc R . . N6 N 0.0442(4) 0.7280(3) 0.0131(3) 0.0351(11) Uani 1 1 d . . . C40 C -0.0611(5) 0.7419(4) 0.0346(4) 0.0385(14) Uani 1 1 d . . . H40 H -0.0678 0.7946 0.0740 0.046 Uiso 1 1 calc R . . C41 C -0.1589(5) 0.6817(5) 0.0009(4) 0.0446(15) Uani 1 1 d . . . H41 H -0.2305 0.6935 0.0170 0.053 Uiso 1 1 calc R . . C42 C -0.1495(5) 0.6033(5) -0.0574(4) 0.0444(15) Uani 1 1 d . . . H42 H -0.2149 0.5616 -0.0811 0.053 Uiso 1 1 calc R . . C43 C -0.0427(6) 0.5874(5) -0.0801(4) 0.0550(18) Uani 1 1 d . . . H43 H -0.0342 0.5343 -0.1185 0.066 Uiso 1 1 calc R . . C44 C 0.0521(6) 0.6526(5) -0.0442(4) 0.0469(16) Uani 1 1 d . . . H44 H 0.1243 0.6434 -0.0607 0.056 Uiso 1 1 calc R . . N7 N 0.3284(6) 0.0630(5) 0.2694(4) 0.0669(17) Uani 1 1 d . . . C45 C 0.4120(7) 0.0775(6) 0.2141(5) 0.068(2) Uani 1 1 d . . . H45 H 0.4629 0.0311 0.2091 0.082 Uiso 1 1 calc R . . C46 C 0.4249(7) 0.1510(5) 0.1686(5) 0.069(2) Uani 1 1 d U . . H46 H 0.4826 0.1568 0.1324 0.082 Uiso 1 1 calc R . . C47 C 0.3530(8) 0.2172(6) 0.1757(6) 0.082(3) Uani 1 1 d U . . H47 H 0.3604 0.2691 0.1425 0.098 Uiso 1 1 calc R . . C48 C 0.2690(7) 0.2134(6) 0.2290(5) 0.073(2) Uani 1 1 d U . . H48 H 0.2218 0.2628 0.2336 0.088 Uiso 1 1 calc R . . C49 C 0.2552(6) 0.1349(5) 0.2759(4) 0.0566(18) Uani 1 1 d . . . H49 H 0.1972 0.1298 0.3120 0.068 Uiso 1 1 calc R . . N8 N 0.5866(5) 0.8833(4) 0.1895(3) 0.0473(13) Uani 1 1 d . . . C50 C 0.5096(5) 0.8328(4) 0.2326(4) 0.0405(14) Uani 1 1 d . . . H50 H 0.4421 0.8587 0.2422 0.049 Uiso 1 1 calc R . . C51 C 0.5251(5) 0.7451(4) 0.2633(3) 0.0353(13) Uani 1 1 d . . . H51 H 0.4701 0.7132 0.2938 0.042 Uiso 1 1 calc R . . C52 C 0.6246(5) 0.7046(4) 0.2479(4) 0.0370(13) Uani 1 1 d . . . H52 H 0.6360 0.6438 0.2662 0.044 Uiso 1 1 calc R . . C53 C 0.7057(5) 0.7558(4) 0.2053(4) 0.0402(14) Uani 1 1 d . . . H53 H 0.7743 0.7317 0.1958 0.048 Uiso 1 1 calc R . . C54 C 0.6836(6) 0.8431(5) 0.1772(4) 0.0496(17) Uani 1 1 d . . . H54 H 0.7386 0.8770 0.1478 0.060 Uiso 1 1 calc R . . C55 C 0.4824(6) 0.5410(6) 0.4294(5) 0.0578(18) Uani 1 1 d . . . C56 C 0.4647(6) 0.4399(5) 0.4254(4) 0.0517(17) Uani 1 1 d . . . C57 C 0.4829(6) 0.3977(5) 0.4978(5) 0.0587(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02816(12) 0.02742(11) 0.02929(12) 0.00307(8) 0.00382(7) 0.00440(8) Zn1 0.0271(3) 0.0326(3) 0.0296(3) 0.0041(3) 0.0034(2) 0.0067(3) Zn2 0.0395(4) 0.0375(4) 0.0298(3) 0.0042(3) 0.0056(3) -0.0052(3) O1 0.034(2) 0.033(2) 0.033(2) 0.0016(17) -0.0001(16) 0.0044(17) O2 0.028(2) 0.0310(19) 0.029(2) 0.0024(16) 0.0033(15) 0.0040(16) O3 0.028(2) 0.0320(19) 0.034(2) 0.0021(17) 0.0002(16) 0.0013(16) O4 0.030(2) 0.033(2) 0.035(2) -0.0008(18) 0.0064(16) 0.0002(16) O5 0.040(2) 0.032(2) 0.036(2) 0.0035(18) 0.0057(17) 0.0103(17) O6 0.042(2) 0.0256(18) 0.030(2) 0.0037(16) 0.0028(16) 0.0028(17) O7 0.033(2) 0.037(2) 0.035(2) 0.0049(18) 0.0062(16) 0.0052(17) O8 0.036(2) 0.034(2) 0.034(2) 0.0026(18) 0.0022(17) 0.0101(17) N1 0.032(3) 0.050(3) 0.037(3) 0.013(2) 0.004(2) -0.004(2) N2 0.034(3) 0.034(2) 0.031(2) 0.003(2) 0.002(2) 0.009(2) N3 0.057(4) 0.045(3) 0.036(3) 0.012(3) 0.001(2) -0.008(3) N4 0.059(4) 0.060(4) 0.046(3) 0.005(3) 0.023(3) -0.004(3) C1 0.028(3) 0.027(3) 0.043(3) -0.002(3) 0.001(2) 0.007(2) C2 0.025(3) 0.024(3) 0.034(3) 0.000(2) 0.001(2) 0.009(2) C3 0.029(3) 0.029(3) 0.043(3) 0.005(3) 0.003(2) 0.013(2) C4 0.029(3) 0.028(3) 0.054(4) 0.003(3) 0.002(3) 0.004(2) C5 0.029(3) 0.031(3) 0.052(4) -0.005(3) -0.006(3) 0.008(2) C6 0.033(3) 0.037(3) 0.037(3) -0.003(3) 0.001(2) 0.011(3) C7 0.029(3) 0.031(3) 0.048(4) 0.016(3) 0.007(3) 0.004(2) C10 0.033(3) 0.057(4) 0.039(3) 0.009(3) 0.012(3) 0.008(3) C11 0.036(3) 0.031(3) 0.032(3) -0.003(2) -0.001(2) 0.014(2) C12 0.029(3) 0.025(3) 0.038(3) -0.001(2) 0.002(2) 0.009(2) C13 0.029(3) 0.023(3) 0.034(3) 0.000(2) 0.003(2) 0.006(2) C14 0.029(3) 0.028(3) 0.035(3) -0.001(2) 0.003(2) 0.007(2) C15 0.029(3) 0.032(3) 0.045(3) -0.001(3) 0.004(2) 0.008(2) C16 0.025(3) 0.038(3) 0.052(4) -0.002(3) -0.001(3) 0.005(2) C17 0.039(3) 0.033(3) 0.035(3) 0.003(3) -0.003(2) 0.011(3) C18 0.039(3) 0.027(3) 0.033(3) -0.003(3) -0.004(2) 0.003(2) C19 0.039(3) 0.029(3) 0.033(3) -0.003(3) -0.009(2) 0.002(2) C20 0.054(4) 0.030(3) 0.045(4) 0.002(3) -0.013(3) -0.002(3) C21 0.080(5) 0.033(3) 0.054(4) 0.008(3) -0.019(4) 0.014(3) C22 0.061(5) 0.038(3) 0.055(4) -0.004(3) -0.015(3) 0.017(3) C23 0.046(4) 0.037(3) 0.040(3) -0.002(3) -0.007(3) 0.007(3) C24 0.073(5) 0.043(4) 0.040(4) 0.021(3) -0.015(3) -0.005(4) C25 0.096(6) 0.057(4) 0.040(4) 0.015(4) 0.010(4) -0.028(4) C28 0.037(4) 0.067(5) 0.039(4) -0.008(3) 0.015(3) 0.001(3) C29 0.035(3) 0.052(4) 0.038(3) -0.013(3) -0.001(3) 0.000(3) C30 0.028(3) 0.035(3) 0.034(3) -0.009(3) -0.001(2) 0.000(2) C31 0.027(3) 0.035(3) 0.041(3) -0.009(3) -0.005(2) 0.007(2) C32 0.037(3) 0.045(3) 0.043(4) -0.010(3) -0.009(3) 0.012(3) C33 0.033(3) 0.050(4) 0.057(4) -0.010(3) -0.006(3) 0.015(3) C34 0.025(3) 0.067(4) 0.052(4) -0.031(4) 0.000(3) 0.008(3) N5 0.030(3) 0.030(2) 0.032(2) 0.003(2) 0.0041(19) 0.0024(19) C35 0.036(3) 0.034(3) 0.043(3) -0.009(3) -0.004(3) 0.011(3) C36 0.027(3) 0.041(3) 0.049(4) 0.002(3) -0.004(3) 0.011(3) C37 0.035(3) 0.031(3) 0.046(4) 0.001(3) 0.007(3) 0.013(2) C38 0.041(4) 0.033(3) 0.037(3) 0.000(3) 0.000(3) 0.003(3) C39 0.036(3) 0.046(3) 0.033(3) 0.001(3) -0.005(2) 0.005(3) N6 0.044(3) 0.032(2) 0.028(2) 0.007(2) 0.001(2) 0.000(2) C40 0.041(4) 0.036(3) 0.036(3) -0.003(3) -0.002(3) 0.003(3) C41 0.035(3) 0.052(4) 0.045(4) -0.002(3) -0.002(3) 0.006(3) C42 0.042(4) 0.047(4) 0.040(4) -0.005(3) -0.004(3) 0.000(3) C43 0.054(4) 0.057(4) 0.048(4) -0.022(4) 0.002(3) 0.007(3) C44 0.041(4) 0.048(4) 0.048(4) -0.009(3) 0.006(3) 0.000(3) N7 0.064(4) 0.067(4) 0.066(4) 0.007(3) -0.005(3) 0.003(3) C45 0.077(6) 0.059(5) 0.080(6) 0.014(4) 0.032(4) 0.031(4) C46 0.075(5) 0.058(4) 0.090(5) 0.026(4) 0.056(4) 0.032(4) C47 0.097(6) 0.058(4) 0.098(6) 0.027(4) 0.041(5) 0.011(4) C48 0.077(5) 0.058(4) 0.094(6) 0.013(4) 0.038(4) 0.021(4) C49 0.064(5) 0.050(4) 0.058(4) 0.002(4) 0.025(4) 0.008(4) N8 0.044(3) 0.042(3) 0.059(3) 0.017(3) 0.000(3) 0.011(3) C50 0.029(3) 0.044(3) 0.047(4) 0.002(3) 0.000(3) 0.006(3) C51 0.034(3) 0.035(3) 0.035(3) 0.006(3) -0.003(2) -0.005(2) C52 0.041(3) 0.029(3) 0.040(3) 0.003(3) -0.009(3) 0.006(3) C53 0.041(4) 0.046(3) 0.035(3) 0.003(3) 0.000(3) 0.016(3) C54 0.041(4) 0.056(4) 0.061(4) 0.032(4) 0.021(3) 0.015(3) C55 0.051(4) 0.061(4) 0.058(4) 0.008(4) -0.008(3) 0.001(4) C56 0.054(4) 0.045(4) 0.054(4) -0.006(3) 0.002(3) 0.009(3) C57 0.043(4) 0.056(4) 0.073(5) -0.006(4) 0.003(4) 0.004(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 O8 2.304(4) . ? U O4 2.306(4) . ? U O1 2.315(4) . ? U O5 2.317(4) . ? U O2 2.418(3) . ? U O3 2.426(4) . ? U O6 2.427(3) . ? U O7 2.432(4) . ? U Zn1 3.6824(7) . ? U Zn2 3.6896(7) . ? Zn1 O3 2.022(4) . ? Zn1 O2 2.044(3) . ? Zn1 N5 2.056(4) . ? Zn1 N1 2.068(5) . ? Zn1 N2 2.071(4) . ? Zn2 O7 2.020(4) . ? Zn2 O6 2.025(4) . ? Zn2 N3 2.071(5) . ? Zn2 N4 2.071(6) . ? Zn2 N6 2.090(5) . ? O1 C1 1.337(6) . ? O2 C2 1.336(6) . ? O2 O3 2.444(5) . ? O2 N1 2.848(6) . ? O3 C13 1.329(6) . ? O3 N2 2.878(6) . ? O4 C14 1.326(6) . ? O5 C18 1.326(6) . ? O6 C19 1.332(7) . ? O6 O7 2.453(5) . ? O6 N3 2.859(6) . ? O7 C30 1.321(7) . ? O7 N4 2.846(6) . ? O8 C31 1.329(7) . ? N1 C7 1.292(7) . ? N1 C8A 1.497(7) . ? N1 C8B 1.521(9) . ? N1 N2 3.118(7) . ? N2 C11 1.279(7) . ? N2 C10 1.482(7) . ? N3 C24 1.288(9) . ? N3 C25 1.510(8) . ? N3 N4 3.131(9) . ? N4 C28 1.267(9) . ? N4 C27B 1.488(9) . ? N4 C27A 1.514(9) . ? C1 C6 1.387(8) . ? C1 C2 1.402(8) . ? C2 C3 1.417(7) . ? C3 C4 1.415(8) . ? C3 C7 1.445(8) . ? C4 C5 1.367(8) . ? C5 C6 1.404(8) . ? C8A C9A 1.526(8) . ? C9A C10 1.550(8) . ? C8B C9B 1.52(2) . ? C9B C10 1.487(9) . ? C11 C12 1.458(8) . ? C12 C13 1.406(7) . ? C12 C17 1.428(8) . ? C13 C14 1.423(7) . ? C14 C15 1.392(8) . ? C15 C16 1.396(8) . ? C16 C17 1.370(8) . ? C18 C23 1.391(8) . ? C18 C19 1.409(8) . ? C19 C20 1.409(8) . ? C20 C21 1.420(9) . ? C20 C24 1.443(10) . ? C21 C22 1.361(10) . ? C22 C23 1.410(9) . ? C25 C26A 1.506(9) . ? C25 C26B 1.551(9) . ? C26A C27A 1.519(9) . ? C26B C27B 1.520(10) . ? C28 C29 1.432(9) . ? C29 C34 1.420(9) . ? C29 C30 1.420(8) . ? C30 C31 1.419(8) . ? C31 C32 1.394(8) . ? C32 C33 1.408(9) . ? C33 C34 1.372(10) . ? N5 C39 1.342(7) . ? N5 C35 1.350(7) . ? C35 C36 1.364(8) . ? C36 C37 1.394(8) . ? C37 C38 1.383(8) . ? C38 C39 1.369(8) . ? N6 C44 1.337(7) . ? N6 C40 1.344(8) . ? C40 C41 1.370(8) . ? C41 C42 1.379(8) . ? C42 C43 1.374(9) . ? C43 C44 1.386(9) . ? N7 C45 1.386(9) . ? N7 C49 1.392(9) . ? C45 C46 1.301(10) . ? C46 C47 1.320(10) . ? C47 C48 1.359(11) . ? C48 C49 1.372(10) . ? N8 C50 1.340(8) . ? N8 C54 1.351(8) . ? C50 C51 1.369(8) . ? C51 C52 1.389(8) . ? C52 C53 1.371(8) . ? C53 C54 1.367(8) . ? C55 C56 1.358(9) . ? C55 C57 1.387(10) 2_666 ? C56 C57 1.381(10) . ? C57 C55 1.387(10) 2_666 ? 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 O8 U O4 85.69(13) . . ? O8 U O1 88.01(13) . . ? O4 U O1 165.99(13) . . ? O8 U O5 167.56(13) . . ? O4 U O5 95.36(13) . . ? O1 U O5 93.49(13) . . ? O8 U O2 88.60(13) . . ? O4 U O2 126.47(12) . . ? O1 U O2 65.76(12) . . ? O5 U O2 80.79(12) . . ? O8 U O3 86.34(12) . . ? O4 U O3 65.92(12) . . ? O1 U O3 126.16(12) . . ? O5 U O3 82.81(13) . . ? O2 U O3 60.61(12) . . ? O8 U O6 126.56(13) . . ? O4 U O6 85.34(13) . . ? O1 U O6 88.40(12) . . ? O5 U O6 65.86(13) . . ? O2 U O6 136.52(12) . . ? O3 U O6 135.29(12) . . ? O8 U O7 66.01(13) . . ? O4 U O7 83.33(13) . . ? O1 U O7 82.67(13) . . ? O5 U O7 126.43(13) . . ? O2 U O7 140.36(12) . . ? O3 U O7 140.28(12) . . ? O6 U O7 60.64(12) . . ? Zn1 U Zn2 169.172(15) . . ? O3 Zn1 O2 73.92(14) . . ? O3 Zn1 N5 105.19(16) . . ? O2 Zn1 N5 100.27(16) . . ? O3 Zn1 N1 148.44(18) . . ? O2 Zn1 N1 87.68(16) . . ? N5 Zn1 N1 103.15(19) . . ? O3 Zn1 N2 89.36(17) . . ? O2 Zn1 N2 154.50(16) . . ? N5 Zn1 N2 102.66(17) . . ? N1 Zn1 N2 97.76(18) . . ? O7 Zn2 O6 74.65(14) . . ? O7 Zn2 N3 152.80(18) . . ? O6 Zn2 N3 88.51(18) . . ? O7 Zn2 N4 88.1(2) . . ? O6 Zn2 N4 152.2(2) . . ? N3 Zn2 N4 98.2(2) . . ? O7 Zn2 N6 98.80(16) . . ? O6 Zn2 N6 98.65(17) . . ? N3 Zn2 N6 104.83(19) . . ? N4 Zn2 N6 105.5(2) . . ? Zn1 O2 U 110.96(15) . . ? Zn1 O3 U 111.46(15) . . ? Zn2 O6 U 111.61(15) . . ? Zn2 O7 U 111.61(16) . . ? C7 N1 C8A 114.4(5) . . ? C7 N1 C8B 119.6(7) . . ? C11 N2 C10 116.4(5) . . ? C24 N3 C25 117.8(6) . . ? C28 N4 C27B 109.5(7) . . ? C28 N4 C27A 121.6(8) . . ? O1 C1 C6 124.4(5) . . ? O1 C1 C2 116.2(5) . . ? C6 C1 C2 119.4(5) . . ? O2 C2 C1 115.7(5) . . ? O2 C2 C3 123.0(5) . . ? C1 C2 C3 121.3(5) . . ? C4 C3 C2 117.5(5) . . ? C4 C3 C7 118.8(5) . . ? C2 C3 C7 123.6(5) . . ? C5 C4 C3 121.0(6) . . ? C4 C5 C6 121.0(5) . . ? C1 C6 C5 119.8(5) . . ? N1 C7 C3 127.7(5) . . ? N1 C8A C9A 107.4(7) . . ? C8A C9A C10 118.8(7) . . ? C9B C8B N1 110.4(11) . . ? C10 C9B C8B 114.8(11) . . ? N2 C10 C9B 111.0(7) . . ? N2 C10 C9A 114.8(5) . . ? N2 C11 C12 128.5(5) . . ? C13 C12 C17 117.8(5) . . ? C13 C12 C11 123.6(5) . . ? C17 C12 C11 118.6(5) . . ? O3 C13 C12 123.6(5) . . ? O3 C13 C14 114.9(5) . . ? C12 C13 C14 121.5(5) . . ? O4 C14 C15 125.5(5) . . ? O4 C14 C13 116.6(5) . . ? C15 C14 C13 117.9(5) . . ? C14 C15 C16 121.6(5) . . ? C17 C16 C15 120.2(5) . . ? C16 C17 C12 121.0(5) . . ? O5 C18 C23 124.7(5) . . ? O5 C18 C19 116.7(5) . . ? C23 C18 C19 118.6(5) . . ? O6 C19 C18 115.6(5) . . ? O6 C19 C20 122.4(5) . . ? C18 C19 C20 121.9(5) . . ? C19 C20 C21 117.1(6) . . ? C19 C20 C24 123.5(6) . . ? C21 C20 C24 119.3(6) . . ? C22 C21 C20 121.5(6) . . ? C21 C22 C23 120.6(6) . . ? C18 C23 C22 120.2(6) . . ? N3 C24 C20 129.1(6) . . ? C26A C25 N3 115.4(7) . . ? N3 C25 C26B 110.8(8) . . ? C25 C26A C27A 110.8(10) . . ? N4 C27A C26A 108.8(9) . . ? C27B C26B C25 120.5(12) . . ? N4 C27B C26B 103.9(10) . . ? N4 C28 C29 129.0(6) . . ? C34 C29 C30 117.7(6) . . ? C34 C29 C28 119.4(6) . . ? C30 C29 C28 122.8(6) . . ? O7 C30 C31 116.0(5) . . ? O7 C30 C29 123.4(5) . . ? C31 C30 C29 120.5(5) . . ? O8 C31 C32 124.4(6) . . ? O8 C31 C30 116.0(5) . . ? C32 C31 C30 119.6(6) . . ? C31 C32 C33 120.2(6) . . ? C34 C33 C32 120.2(6) . . ? C33 C34 C29 121.8(6) . . ? C39 N5 C35 117.2(5) . . ? N5 C35 C36 122.9(5) . . ? C35 C36 C37 119.1(5) . . ? C38 C37 C36 118.6(5) . . ? C39 C38 C37 118.6(5) . . ? N5 C39 C38 123.7(5) . . ? C44 N6 C40 117.8(5) . . ? N6 C40 C41 122.7(6) . . ? C40 C41 C42 118.9(6) . . ? C43 C42 C41 119.4(6) . . ? C42 C43 C44 118.3(6) . . ? N6 C44 C43 122.8(6) . . ? C45 N7 C49 115.6(6) . . ? C46 C45 N7 125.0(7) . . ? C45 C46 C47 117.7(7) . . ? C46 C47 C48 123.4(8) . . ? C47 C48 C49 118.4(7) . . ? C48 C49 N7 119.8(7) . . ? C50 N8 C54 116.3(5) . . ? N8 C50 C51 123.4(6) . . ? C50 C51 C52 118.8(6) . . ? C53 C52 C51 118.8(5) . . ? C54 C53 C52 118.6(6) . . ? N8 C54 C53 124.0(6) . . ? C56 C55 C57 123.0(7) . 2_666 ? C55 C56 C57 117.4(7) . . ? C56 C57 C55 119.6(7) . 2_666 ? #===END data_[(NiL^3^)~2~U].1.5py _database_code_CSD 208960 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.50 H39.50 N5.50 Ni2 O8 U' _chemical_formula_weight 1122.76 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3441(4) _cell_length_b 13.4866(10) _cell_length_c 31.0091(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.119(4) _cell_angle_gamma 90.00 _cell_volume 4326.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25784 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepipedic _exptl_crystal_colour 'translucent dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method ? _exptl_crystal_F_000 2204 _exptl_absorpt_coefficient_mu 4.654 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_T_max 0.498 _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_detector_area_resol_mean 18 _diffrn_standards_decay_% none _diffrn_reflns_number 25784 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7381 _reflns_number_gt 5849 _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. The bridge C26-C27 of the second Schiff base molecule and its two methyl substituents C35 and C36 are much disordered but, the two (or more) positions being unresolved, the main component only has been kept and refined with restraints on bond lengths, angles and displacement parameters. The pyridine molecules were refined as idealized hexagons with some restraints on displacement parameters. One of them was given an occupancy factor of 0.5 in order to keep physically acceptable displacement factors. The H atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. A void of 91 A^3^ likely indicates the presence of an unresolved solvent molecule. The highest residual electron density peak is located near C26, in the badly resolved bridge of the second Schiff base molecule. Furthermore, some short contacts involving C35 and its hydrogen atoms indicate that the description of this bridge is not perfect, but can only be considered as an average of several disordered positions. 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^)+(0.0647P)^2^+45.6159P] 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 SHELXL _refine_ls_extinction_coef 0.0017(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7381 _refine_ls_number_parameters 548 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.286 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 1.396 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.106 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 0.00919(5) 0.02653(4) 0.356161(14) 0.0404(2) Uani 1 1 d . . . Ni1 Ni -0.15487(18) -0.05375(17) 0.26293(5) 0.0548(6) Uani 1 1 d . . . Ni2 Ni 0.17058(18) 0.13077(14) 0.44567(5) 0.0476(5) Uani 1 1 d . . . O1 O -0.0286(10) 0.1934(9) 0.3427(3) 0.060(3) Uani 1 1 d . . . O2 O -0.1125(9) 0.0616(9) 0.2908(3) 0.057(3) Uani 1 1 d . . . O3 O -0.0675(9) -0.1056(8) 0.3085(3) 0.052(3) Uani 1 1 d . . . O4 O 0.0559(9) -0.1341(8) 0.3776(3) 0.051(2) Uani 1 1 d . . . N1 N -0.2439(14) -0.0005(13) 0.2184(4) 0.069(4) Uani 1 1 d . . . N2 N -0.1885(12) -0.1798(14) 0.2385(4) 0.068(4) Uani 1 1 d . . . C1 C -0.0961(16) 0.2246(13) 0.3086(6) 0.063(4) Uani 1 1 d . . . C2 C -0.1408(14) 0.1543(14) 0.2796(5) 0.057(4) Uani 1 1 d . . . C3 C -0.2125(16) 0.1699(13) 0.2405(6) 0.067(5) Uani 1 1 d . . . C4 C -0.2352(17) 0.2700(15) 0.2325(6) 0.071(5) Uani 1 1 d . . . H4 H -0.2809 0.2867 0.2077 0.085 Uiso 1 1 calc R . . C5 C -0.1963(18) 0.3420(14) 0.2576(6) 0.069(5) Uani 1 1 d . . . H5 H -0.2167 0.4071 0.2503 0.083 Uiso 1 1 calc R . . C6 C -0.1192(18) 0.3225(16) 0.2980(7) 0.082(6) Uani 1 1 d . . . H6 H -0.0886 0.3742 0.3151 0.099 Uiso 1 1 calc R . . C7 C -0.2573(15) 0.0889(15) 0.2141(4) 0.058(4) Uani 1 1 d . . . H7 H -0.3041 0.1079 0.1898 0.069 Uiso 1 1 calc R . . C8 C -0.3083(15) -0.0819(16) 0.1915(5) 0.068(5) Uani 1 1 d . . . C9 C -0.2342(18) -0.1729(14) 0.1932(5) 0.071(5) Uani 1 1 d . . . H9A H -0.1617 -0.1703 0.1734 0.085 Uiso 1 1 calc R . . H9B H -0.2879 -0.2295 0.1858 0.085 Uiso 1 1 calc R . . C10 C -0.1558(18) -0.2630(14) 0.2554(6) 0.071(5) Uani 1 1 d . . . H10 H -0.1751 -0.3189 0.2390 0.085 Uiso 1 1 calc R . . C11 C -0.0965(16) -0.2812(16) 0.2941(5) 0.069(5) Uani 1 1 d . . . C12 C -0.0496(14) -0.2005(12) 0.3191(5) 0.053(4) Uani 1 1 d . . . C13 C 0.0178(14) -0.2161(12) 0.3577(5) 0.057(4) Uani 1 1 d . . . C14 C 0.0358(17) -0.3128(13) 0.3718(7) 0.071(5) Uani 1 1 d . . . H14 H 0.0794 -0.3251 0.3975 0.085 Uiso 1 1 calc R . . C15 C -0.011(2) -0.3903(19) 0.3476(8) 0.094(6) Uani 1 1 d U . . H15 H 0.0001 -0.4547 0.3577 0.113 Uiso 1 1 calc R . . C16 C -0.0700(18) -0.3774(14) 0.3119(6) 0.073(5) Uani 1 1 d U . . H16 H -0.0970 -0.4331 0.2967 0.087 Uiso 1 1 calc R . . C17 C -0.314(2) -0.0461(16) 0.1426(6) 0.087(6) Uani 1 1 d U . . H17A H -0.2279 -0.0377 0.1319 0.131 Uiso 1 1 calc R . . H17B H -0.3596 0.0158 0.1409 0.131 Uiso 1 1 calc R . . H17C H -0.3584 -0.0950 0.1256 0.131 Uiso 1 1 calc R . . C18 C -0.4467(15) -0.0958(14) 0.2090(6) 0.067(5) Uani 1 1 d . . . H18A H -0.4912 -0.1445 0.1919 0.100 Uiso 1 1 calc R . . H18B H -0.4923 -0.0339 0.2075 0.100 Uiso 1 1 calc R . . H18C H -0.4428 -0.1176 0.2384 0.100 Uiso 1 1 calc R . . O5 O 0.1904(9) 0.0335(7) 0.3127(3) 0.045(2) Uani 1 1 d . . . O6 O 0.2061(9) 0.0844(8) 0.3919(3) 0.048(2) Uani 1 1 d . . . O7 O 0.0151(9) 0.0766(8) 0.4316(3) 0.049(2) Uani 1 1 d . . . O8 O -0.1839(8) 0.0124(7) 0.3920(3) 0.044(2) Uani 1 1 d . . . N3 N 0.3285(11) 0.1916(7) 0.4550(3) 0.071(3) Uani 1 1 d DU . . N4 N 0.1225(8) 0.1715(8) 0.5004(2) 0.054(2) Uani 1 1 d DU . . C19 C 0.3029(14) 0.0691(12) 0.3258(4) 0.048(3) Uani 1 1 d . . . C20 C 0.3147(13) 0.1005(12) 0.3691(4) 0.050(3) Uani 1 1 d . . . C21 C 0.4229(13) 0.1487(12) 0.3865(3) 0.059(4) Uani 1 1 d D . . C22 C 0.5297(16) 0.1598(16) 0.3572(6) 0.075(5) Uani 1 1 d . . . H22 H 0.6046 0.1914 0.3666 0.090 Uiso 1 1 calc R . . C23 C 0.5232(17) 0.1251(16) 0.3162(7) 0.081(6) Uani 1 1 d . . . H23 H 0.5952 0.1314 0.2985 0.097 Uiso 1 1 calc R . . C24 C 0.4126(15) 0.0806(14) 0.2997(5) 0.062(4) Uani 1 1 d . . . H24 H 0.4113 0.0583 0.2714 0.074 Uiso 1 1 calc R . . C25 C 0.4241(14) 0.1912(11) 0.4293(3) 0.072(3) Uani 1 1 d DU . . H25 H 0.5005 0.2204 0.4388 0.086 Uiso 1 1 calc R . . C26 C 0.3156(8) 0.2593(8) 0.4945(3) 0.085(8) Uani 1 1 d DU . . C27 C 0.2351(8) 0.2060(11) 0.5276(2) 0.078(7) Uani 1 1 d DU . . H27A H 0.2073 0.2504 0.5504 0.094 Uiso 1 1 calc R . . H27B H 0.2815 0.1506 0.5401 0.094 Uiso 1 1 calc R . . C28 C 0.0119(8) 0.1554(10) 0.5170(4) 0.054(2) Uani 1 1 d DU . . H28 H 0.0008 0.1774 0.5451 0.064 Uiso 1 1 calc R . . C29 C -0.0954(8) 0.1085(11) 0.4980(4) 0.054(4) Uani 1 1 d D . . C30 C -0.0923(13) 0.0753(12) 0.4552(4) 0.048(3) Uani 1 1 d . . . C31 C -0.2028(13) 0.0389(10) 0.4331(4) 0.044(3) Uani 1 1 d . . . C32 C -0.3170(16) 0.0319(14) 0.4560(5) 0.062(4) Uani 1 1 d . . . H32 H -0.3915 0.0076 0.4429 0.074 Uiso 1 1 calc R . . C33 C -0.3193(18) 0.0623(14) 0.5003(5) 0.068(5) Uani 1 1 d . . . H33 H -0.3958 0.0551 0.5157 0.082 Uiso 1 1 calc R . . C34 C -0.2122(17) 0.1022(12) 0.5213(5) 0.061(4) Uani 1 1 d . . . H34 H -0.2174 0.1240 0.5497 0.073 Uiso 1 1 calc R . . C35 C 0.4512(9) 0.2756(14) 0.5128(4) 0.083(11) Uani 1 1 d DU . . H35A H 0.4485 0.3263 0.5345 0.125 Uiso 1 1 calc R . . H35B H 0.5083 0.2956 0.4900 0.125 Uiso 1 1 calc R . . H35C H 0.4822 0.2150 0.5253 0.125 Uiso 1 1 calc R . . C36 C 0.2441(15) 0.3528(8) 0.4801(6) 0.091(9) Uani 1 1 d DU . . H36A H 0.1913 0.3378 0.4554 0.137 Uiso 1 1 calc R . . H36B H 0.3056 0.4032 0.4726 0.137 Uiso 1 1 calc R . . H36C H 0.1903 0.3761 0.5032 0.137 Uiso 1 1 calc R . . N5 N 0.5179(13) 0.1801(7) 0.1343(4) 0.087(4) Uani 1 1 d GU . . C37 C 0.4020(11) 0.2157(9) 0.1508(4) 0.102(5) Uani 1 1 d GU . . H37 H 0.3402 0.1717 0.1611 0.122 Uiso 1 1 calc R . . C38 C 0.3784(10) 0.3172(10) 0.1518(5) 0.101(5) Uani 1 1 d GU . . H38 H 0.3008 0.3410 0.1628 0.121 Uiso 1 1 calc R . . C39 C 0.4707(13) 0.3830(7) 0.1363(4) 0.080(4) Uani 1 1 d GU . . H39 H 0.4550 0.4508 0.1370 0.096 Uiso 1 1 calc R . . C40 C 0.5867(11) 0.3474(9) 0.1199(4) 0.078(4) Uani 1 1 d GU . . H40 H 0.6484 0.3914 0.1095 0.093 Uiso 1 1 calc R . . C41 C 0.6103(10) 0.2459(10) 0.1189(4) 0.079(4) Uani 1 1 d GU . . H41 H 0.6878 0.2221 0.1078 0.095 Uiso 1 1 calc R . . N6 N 0.376(2) 0.9671(17) 0.0876(8) 0.090(6) Uani 0.50 1 d PGU . . C42 C 0.284(3) 0.909(2) 0.1083(6) 0.088(7) Uani 0.50 1 d PGU . . H42 H 0.2652 0.9200 0.1373 0.106 Uiso 0.50 1 calc PR . . C43 C 0.219(2) 0.835(2) 0.0858(9) 0.093(7) Uani 0.50 1 d PGU . . H43 H 0.1576 0.7962 0.0996 0.111 Uiso 0.50 1 calc PR . . C44 C 0.247(3) 0.8188(19) 0.0425(9) 0.096(7) Uani 0.50 1 d PGU . . H44 H 0.2036 0.7692 0.0274 0.115 Uiso 0.50 1 calc PR . . C45 C 0.339(3) 0.877(2) 0.0217(7) 0.099(7) Uani 0.50 1 d PGU . . H45 H 0.3572 0.8660 -0.0072 0.118 Uiso 0.50 1 calc PR . . C46 C 0.403(2) 0.951(2) 0.0443(8) 0.094(7) Uani 0.50 1 d PGU . . H46 H 0.4647 0.9897 0.0305 0.113 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.0400(3) 0.0455(3) 0.0357(3) -0.0015(2) 0.00130(17) -0.0037(2) Ni1 0.0457(11) 0.0814(16) 0.0373(9) -0.0054(9) -0.0019(7) -0.0084(9) Ni2 0.0530(11) 0.0519(12) 0.0378(9) -0.0039(8) -0.0054(7) -0.0065(9) O1 0.051(7) 0.062(8) 0.068(7) -0.001(6) 0.004(5) -0.013(5) O2 0.046(6) 0.074(8) 0.050(6) 0.004(5) 0.001(4) 0.006(5) O3 0.053(6) 0.063(7) 0.039(5) -0.009(5) 0.001(4) -0.012(5) O4 0.050(6) 0.047(6) 0.055(6) -0.001(5) 0.014(4) -0.002(5) N1 0.060(10) 0.095(13) 0.053(8) -0.002(7) -0.002(6) 0.009(8) N2 0.042(8) 0.120(14) 0.042(7) -0.022(8) 0.004(5) -0.026(8) C1 0.063(11) 0.051(11) 0.075(11) 0.027(9) 0.022(8) 0.008(8) C2 0.044(9) 0.077(13) 0.048(8) 0.014(8) 0.004(6) 0.005(8) C3 0.052(10) 0.051(11) 0.100(13) 0.028(9) 0.033(8) 0.010(8) C4 0.066(12) 0.072(14) 0.074(11) 0.013(10) 0.014(8) 0.003(9) C5 0.079(13) 0.049(11) 0.079(12) 0.022(9) 0.022(9) 0.018(9) C6 0.069(13) 0.071(14) 0.107(15) 0.025(11) 0.024(10) 0.009(10) C7 0.064(10) 0.072(13) 0.037(7) -0.009(8) 0.009(6) -0.010(9) C8 0.050(10) 0.109(15) 0.043(8) -0.031(9) -0.018(6) 0.026(9) C9 0.082(13) 0.065(12) 0.065(10) -0.007(9) 0.008(8) -0.015(10) C10 0.083(13) 0.045(11) 0.085(13) 0.003(9) 0.027(10) 0.001(9) C11 0.060(11) 0.088(15) 0.059(10) -0.022(9) 0.015(7) -0.004(9) C12 0.045(9) 0.038(9) 0.076(10) -0.002(7) 0.017(7) 0.003(7) C13 0.046(9) 0.048(10) 0.077(10) -0.010(8) 0.019(7) 0.000(7) C14 0.061(11) 0.047(11) 0.106(14) -0.001(10) 0.021(9) 0.017(8) C15 0.086(10) 0.088(11) 0.108(11) -0.001(9) 0.011(9) 0.008(9) C16 0.075(9) 0.053(9) 0.089(9) -0.017(8) 0.026(8) 0.003(7) C17 0.098(10) 0.085(11) 0.079(9) -0.004(8) -0.010(8) 0.005(8) C18 0.058(11) 0.065(12) 0.078(11) -0.021(9) -0.009(8) 0.013(8) O5 0.044(6) 0.048(6) 0.041(5) -0.005(4) 0.007(4) -0.003(4) O6 0.046(6) 0.061(7) 0.039(5) 0.001(4) 0.003(4) -0.015(5) O7 0.043(6) 0.066(7) 0.037(5) -0.008(4) 0.006(4) -0.002(5) O8 0.034(5) 0.051(6) 0.047(5) -0.001(4) 0.002(3) -0.002(4) N3 0.067(8) 0.088(9) 0.059(6) 0.000(6) -0.009(4) -0.037(6) N4 0.071(7) 0.046(6) 0.043(5) -0.009(4) -0.006(4) 0.015(5) C19 0.047(9) 0.050(9) 0.048(7) 0.012(7) 0.003(6) 0.009(7) C20 0.043(9) 0.056(10) 0.050(8) 0.005(7) 0.002(6) -0.005(7) C21 0.044(9) 0.066(11) 0.067(10) 0.008(8) -0.007(7) -0.016(7) C22 0.042(11) 0.096(16) 0.086(13) 0.015(11) 0.005(8) -0.008(9) C23 0.050(12) 0.096(16) 0.096(14) 0.028(12) 0.015(9) -0.005(10) C24 0.047(10) 0.075(12) 0.063(9) -0.002(8) 0.007(7) -0.002(8) C25 0.067(8) 0.088(9) 0.060(6) 0.000(6) -0.009(4) -0.037(6) C26 0.089(12) 0.093(13) 0.074(11) -0.013(10) -0.018(9) -0.034(10) C27 0.082(11) 0.083(12) 0.070(10) -0.042(9) -0.007(9) -0.001(9) C28 0.071(7) 0.046(6) 0.043(5) -0.009(4) -0.006(4) 0.015(5) C29 0.066(10) 0.059(10) 0.037(7) 0.001(6) 0.011(6) 0.018(8) C30 0.049(9) 0.051(9) 0.044(7) 0.008(7) 0.004(6) 0.006(7) C31 0.044(8) 0.035(8) 0.053(8) 0.008(6) 0.005(6) -0.004(6) C32 0.047(10) 0.079(12) 0.059(9) 0.010(8) 0.010(6) 0.003(8) C33 0.072(12) 0.072(12) 0.060(10) 0.012(8) 0.029(8) 0.019(9) C34 0.076(12) 0.048(10) 0.058(9) 0.002(7) 0.019(8) 0.009(8) C35 0.084(14) 0.087(15) 0.078(14) -0.008(11) -0.010(10) 0.001(11) C36 0.098(13) 0.077(13) 0.100(12) 0.002(10) -0.028(10) 0.001(10) N5 0.086(8) 0.085(8) 0.091(8) 0.010(7) 0.001(7) 0.013(7) C37 0.095(8) 0.092(8) 0.118(8) 0.000(7) 0.016(7) -0.002(7) C38 0.091(8) 0.089(8) 0.122(8) -0.002(7) 0.015(7) -0.002(7) C39 0.076(7) 0.077(8) 0.088(7) 0.011(6) -0.002(6) -0.003(6) C40 0.079(8) 0.079(9) 0.075(8) 0.004(7) 0.008(7) -0.013(8) C41 0.074(9) 0.086(9) 0.078(8) 0.003(8) 0.007(7) 0.007(8) N6 0.094(9) 0.086(9) 0.092(9) 0.006(8) -0.007(8) -0.001(8) C42 0.087(9) 0.086(9) 0.091(9) 0.002(8) -0.011(8) -0.006(8) C43 0.093(9) 0.086(10) 0.099(9) 0.004(8) -0.010(8) -0.005(8) C44 0.098(10) 0.089(10) 0.101(9) 0.001(8) -0.008(8) -0.001(8) C45 0.106(10) 0.092(10) 0.098(9) 0.004(8) -0.003(8) 0.005(8) C46 0.098(10) 0.089(10) 0.096(9) 0.009(8) -0.001(8) 0.000(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O8 2.296(9) . ? U O5 2.313(9) . ? U O4 2.317(10) . ? U O1 2.322(12) . ? U O2 2.430(10) . ? U O7 2.436(8) . ? U O6 2.444(9) . ? U O3 2.446(9) . ? U Ni1 3.5199(18) . ? U Ni2 3.5283(17) . ? Ni1 N1 1.807(14) . ? Ni1 O3 1.817(10) . ? Ni1 O2 1.833(12) . ? Ni1 N2 1.892(16) . ? Ni2 O7 1.818(9) . ? Ni2 O6 1.821(9) . ? Ni2 N3 1.850(10) . ? Ni2 N4 1.853(9) . ? O1 C1 1.333(19) . ? O2 C2 1.33(2) . ? O2 O3 2.368(17) . ? O2 N1 2.753(17) . ? O3 C12 1.334(18) . ? O3 N2 2.696(14) . ? O4 C13 1.325(18) . ? N1 C7 1.22(2) . ? N1 C8 1.53(2) . ? N1 N2 2.56(3) . ? N2 C10 1.28(2) . ? N2 C9 1.49(2) . ? C1 C6 1.38(2) . ? C1 C2 1.39(2) . ? C2 C3 1.44(2) . ? C3 C4 1.39(2) . ? C3 C7 1.44(2) . ? C4 C5 1.31(3) . ? C5 C6 1.51(3) . ? C8 C9 1.45(3) . ? C8 C18 1.54(2) . ? C8 C17 1.59(2) . ? C10 C11 1.37(3) . ? C11 C12 1.42(2) . ? C11 C16 1.44(3) . ? C12 C13 1.40(2) . ? C13 C14 1.39(2) . ? C14 C15 1.38(3) . ? C15 C16 1.27(3) . ? O5 C19 1.323(17) . ? O6 C20 1.345(15) . ? O6 O7 2.334(12) . ? O6 N3 2.741(12) . ? O7 C30 1.331(15) . ? O7 N4 2.722(12) . ? O8 C31 1.337(16) . ? N3 C25 1.271(17) . ? N3 C26 1.534(14) . ? N3 N4 2.571(10) . ? N4 C28 1.273(6) . ? N4 C27 1.510(12) . ? C19 C24 1.40(2) . ? C19 C20 1.41(2) . ? C20 C21 1.40(2) . ? C21 C22 1.439(19) . ? C21 C25 1.447(10) . ? C22 C23 1.36(3) . ? C23 C24 1.39(2) . ? C26 C27 1.506(13) . ? C26 C36 1.528(16) . ? C26 C35 1.528(13) . ? C28 C29 1.406(9) . ? C29 C30 1.402(18) . ? C29 C34 1.411(18) . ? C30 C31 1.418(19) . ? C31 C32 1.384(19) . ? C32 C33 1.43(2) . ? C33 C34 1.39(3) . ? N5 C37 1.3900 . ? N5 C41 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? N6 C42 1.3900 . ? N6 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 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 O8 U O5 173.0(3) . . ? O8 U O4 88.0(3) . . ? O5 U O4 92.1(3) . . ? O8 U O1 91.2(4) . . ? O5 U O1 89.6(3) . . ? O4 U O1 173.2(4) . . ? O8 U O2 88.3(3) . . ? O5 U O2 85.7(3) . . ? O4 U O2 121.9(4) . . ? O1 U O2 64.8(4) . . ? O8 U O7 65.0(3) . . ? O5 U O7 122.0(3) . . ? O4 U O7 88.8(3) . . ? O1 U O7 84.7(4) . . ? O2 U O7 139.4(3) . . ? O8 U O6 122.2(3) . . ? O5 U O6 64.9(3) . . ? O4 U O6 89.7(4) . . ? O1 U O6 85.0(4) . . ? O2 U O6 138.2(3) . . ? O7 U O6 57.1(3) . . ? O8 U O3 87.2(3) . . ? O5 U O3 86.5(3) . . ? O4 U O3 63.8(3) . . ? O1 U O3 122.9(4) . . ? O2 U O3 58.1(4) . . ? O7 U O3 142.1(3) . . ? O6 U O3 140.8(3) . . ? Ni1 U Ni2 174.41(5) . . ? N1 Ni1 O3 178.7(6) . . ? N1 Ni1 O2 98.3(6) . . ? O3 Ni1 O2 80.9(5) . . ? N1 Ni1 N2 87.6(7) . . ? O3 Ni1 N2 93.2(6) . . ? O2 Ni1 N2 174.1(6) . . ? O7 Ni2 O6 79.8(4) . . ? O7 Ni2 N3 174.6(4) . . ? O6 Ni2 N3 96.6(4) . . ? O7 Ni2 N4 95.7(3) . . ? O6 Ni2 N4 175.3(4) . . ? N3 Ni2 N4 88.0(3) . . ? C7 N1 C8 126.9(15) . . ? C10 N2 C9 121.6(17) . . ? O1 C1 C6 125.5(19) . . ? O1 C1 C2 118.2(15) . . ? C6 C1 C2 116.2(18) . . ? O2 C2 C1 113.6(13) . . ? O2 C2 C3 118.1(16) . . ? C1 C2 C3 128.3(17) . . ? C4 C3 C2 112.3(18) . . ? C4 C3 C7 125.5(19) . . ? C2 C3 C7 122.3(16) . . ? C5 C4 C3 124.2(19) . . ? C4 C5 C6 121.8(17) . . ? C1 C6 C5 117(2) . . ? N1 C7 C3 130.6(17) . . ? C9 C8 N1 111.1(13) . . ? C9 C8 C18 112.1(18) . . ? N1 C8 C18 107.4(12) . . ? C9 C8 C17 108.1(13) . . ? N1 C8 C17 108.5(17) . . ? C18 C8 C17 109.7(13) . . ? C8 C9 N2 104.7(14) . . ? N2 C10 C11 129.2(19) . . ? C10 C11 C12 119.6(19) . . ? C10 C11 C16 125.8(18) . . ? C12 C11 C16 114.5(16) . . ? O3 C12 C13 115.0(14) . . ? O3 C12 C11 123.6(16) . . ? C13 C12 C11 121.4(16) . . ? O4 C13 C14 126.7(17) . . ? O4 C13 C12 114.8(14) . . ? C14 C13 C12 118.5(16) . . ? C15 C14 C13 120(2) . . ? C16 C15 C14 123(2) . . ? C15 C16 C11 123(2) . . ? C25 N3 C26 124.9(6) . . ? C28 N4 C27 121.3(5) . . ? O5 C19 C24 125.1(13) . . ? O5 C19 C20 118.4(12) . . ? C24 C19 C20 116.5(14) . . ? O6 C20 C21 122.6(11) . . ? O6 C20 C19 112.4(12) . . ? C21 C20 C19 124.9(12) . . ? C20 C21 C22 114.8(12) . . ? C20 C21 C25 122.9(10) . . ? C22 C21 C25 122.2(14) . . ? C23 C22 C21 121.2(16) . . ? C22 C23 C24 122.3(16) . . ? C23 C24 C19 120.1(16) . . ? N3 C25 C21 124.8(12) . . ? C27 C26 C36 109.0(9) . . ? C27 C26 C35 108.9(8) . . ? C36 C26 C35 115.7(11) . . ? C27 C26 N3 108.0(9) . . ? C36 C26 N3 107.5(9) . . ? C35 C26 N3 107.5(9) . . ? C26 C27 N4 101.1(6) . . ? N4 C28 C29 128.1(10) . . ? C30 C29 C28 121.3(9) . . ? C30 C29 C34 119.2(11) . . ? C28 C29 C34 119.3(13) . . ? O7 C30 C29 122.4(12) . . ? O7 C30 C31 114.4(12) . . ? C29 C30 C31 123.2(11) . . ? O8 C31 C32 126.7(13) . . ? O8 C31 C30 115.6(11) . . ? C32 C31 C30 117.6(13) . . ? C31 C32 C33 119.3(15) . . ? C34 C33 C32 123.0(15) . . ? C33 C34 C29 117.7(14) . . ? C37 N5 C41 120.0 . . ? C38 C37 N5 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C41 120.0 . . ? C40 C41 N5 120.0 . . ? C42 N6 C46 120.0 . . ? C43 C42 N6 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 N6 120.0 . . ?