# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 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 ; 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_requested_journal 'Chemical Communications' _publ_section_title ; Structure and magnetism of the first strictly dinuclear compound containing paramagnetic 3d and 5f metal ions. Major influence of the CuII ion coordination on the CuII-UIV interaction ; data_1.1.5py _database_code_CSD 200802 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.50 H42.50 Cu N4.50 O8 U' _chemical_formula_weight 1021.86 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' Cu Cu 0.3201 1.2651 '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 10.6528(5) _cell_length_b 13.4546(7) _cell_length_c 16.1262(9) _cell_angle_alpha 102.667(3) _cell_angle_beta 107.410(3) _cell_angle_gamma 109.447(3) _cell_volume 1944.64(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13267 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepipedic _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method ? _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 4.764 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.376 _exptl_absorpt_correction_T_max 0.683 _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 13267 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0904 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6798 _reflns_number_gt 4989 _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 from Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. One pyridine solvent molecule is disordered around the symmetry centre. All H atoms (except those in the disordered pyridine) were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. The highest residual density peak is located near the U 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^)+(0.0379P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6798 _refine_ls_number_parameters 503 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.003 _refine_diff_density_min -1.160 _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 0.26388(3) 0.28664(2) 0.25481(2) 0.04986(13) Uani 1 1 d . . . Cu Cu -0.04940(10) 0.34349(8) 0.21594(7) 0.0518(3) Uani 1 1 d . . . O1 O 0.3015(6) 0.3245(4) 0.1309(4) 0.0546(13) Uani 1 1 d . . . O2 O 0.1026(5) 0.3599(4) 0.1729(3) 0.0500(13) Uani 1 1 d . . . O3 O 0.0728(5) 0.3055(4) 0.3080(4) 0.0520(13) Uani 1 1 d . . . O4 O 0.2283(6) 0.2016(4) 0.3577(4) 0.0553(14) Uani 1 1 d . . . N1 N -0.1909(7) 0.3314(5) 0.1010(5) 0.0570(17) Uani 1 1 d . . . N2 N -0.2155(7) 0.2898(5) 0.2476(5) 0.0548(17) Uani 1 1 d . . . C1 C 0.2023(9) 0.3381(6) 0.0640(6) 0.057(2) Uani 1 1 d . . . C2 C 0.0886(8) 0.3515(6) 0.0862(6) 0.053(2) Uani 1 1 d . . . C3 C -0.0306(8) 0.3537(6) 0.0179(5) 0.0496(19) Uani 1 1 d . . . C4 C -0.0259(9) 0.3522(6) -0.0678(6) 0.056(2) Uani 1 1 d . . . H4 H -0.1033 0.3526 -0.1136 0.067 Uiso 1 1 calc R . . C5 C 0.0924(9) 0.3502(7) -0.0852(6) 0.059(2) Uani 1 1 d . . . H5 H 0.0977 0.3555 -0.1407 0.070 Uiso 1 1 calc R . . C6 C 0.2061(9) 0.3402(7) -0.0195(6) 0.059(2) Uani 1 1 d . . . H6 H 0.2830 0.3350 -0.0333 0.070 Uiso 1 1 calc R . . C7 C -0.1664(9) 0.3405(7) 0.0304(7) 0.058(2) Uani 1 1 d . . . H7A H -0.2415 0.3386 -0.0186 0.070 Uiso 1 1 calc R . . C8 C -0.3455(9) 0.2928(7) 0.0969(7) 0.064(2) Uani 1 1 d . . . C9 C -0.3313(9) 0.3158(8) 0.1967(6) 0.063(2) Uani 1 1 d . . . H9A H -0.3088 0.3944 0.2258 0.076 Uiso 1 1 calc R . . H9B H -0.4225 0.2696 0.1976 0.076 Uiso 1 1 calc R . . C10 C -0.2327(9) 0.2278(7) 0.2955(6) 0.058(2) Uani 1 1 d . . . H10A H -0.3208 0.2030 0.3016 0.070 Uiso 1 1 calc R . . C11 C -0.1248(9) 0.1924(6) 0.3418(6) 0.054(2) Uani 1 1 d . . . C12 C 0.0155(9) 0.2264(6) 0.3401(5) 0.053(2) Uani 1 1 d . . . C13 C 0.1072(9) 0.1737(6) 0.3717(5) 0.052(2) Uani 1 1 d . . . C14 C 0.0590(9) 0.0941(7) 0.4111(6) 0.058(2) Uani 1 1 d . . . H14 H 0.1177 0.0600 0.4338 0.069 Uiso 1 1 calc R . . C15 C -0.0748(10) 0.0649(7) 0.4171(6) 0.062(2) Uani 1 1 d . . . H15 H -0.1029 0.0133 0.4456 0.075 Uiso 1 1 calc R . . C16 C -0.1660(9) 0.1105(6) 0.3818(6) 0.058(2) Uani 1 1 d . . . H16 H -0.2570 0.0872 0.3842 0.069 Uiso 1 1 calc R . . C17 C -0.4242(9) 0.1647(7) 0.0433(7) 0.072(3) Uani 1 1 d . . . H17A H -0.4308 0.1496 -0.0193 0.108 Uiso 1 1 calc R . . H17B H -0.5202 0.1361 0.0424 0.108 Uiso 1 1 calc R . . H17C H -0.3705 0.1285 0.0734 0.108 Uiso 1 1 calc R . . C18 C -0.4226(10) 0.3557(9) 0.0522(7) 0.081(3) Uani 1 1 d . . . H18A H -0.3602 0.4350 0.0794 0.121 Uiso 1 1 calc R . . H18B H -0.5104 0.3416 0.0621 0.121 Uiso 1 1 calc R . . H18C H -0.4461 0.3303 -0.0133 0.121 Uiso 1 1 calc R . . O5 O 0.0436(5) 0.1321(4) 0.1515(4) 0.0539(13) Uani 1 1 d . . . O6 O 0.3151(5) 0.1341(4) 0.1983(4) 0.0542(13) Uani 1 1 d . . . C19 C -0.1647(10) -0.0409(7) 0.0712(7) 0.076(3) Uani 1 1 d . . . H19A H -0.2024 -0.0615 0.1152 0.114 Uiso 1 1 calc R . . H19B H -0.1887 -0.1078 0.0218 0.114 Uiso 1 1 calc R . . H19C H -0.2068 0.0046 0.0463 0.114 Uiso 1 1 calc R . . C20 C 0.0001(9) 0.0257(7) 0.1197(6) 0.062(2) Uani 1 1 d . . . C21 C 0.0909(10) -0.0283(7) 0.1229(7) 0.068(2) Uani 1 1 d . . . H21A H 0.0490 -0.1066 0.0983 0.082 Uiso 1 1 calc R . . C22 C 0.2400(10) 0.0286(7) 0.1607(6) 0.064(2) Uani 1 1 d . . . C23 C 0.3281(10) -0.0390(8) 0.1575(8) 0.081(3) Uani 1 1 d . . . H23A H 0.3667 -0.0310 0.1114 0.122 Uiso 1 1 calc R . . H23B H 0.2667 -0.1171 0.1418 0.122 Uiso 1 1 calc R . . H23C H 0.4067 -0.0120 0.2172 0.122 Uiso 1 1 calc R . . O7 O 0.5085(6) 0.3383(4) 0.3521(4) 0.0563(14) Uani 1 1 d . . . O8 O 0.3812(5) 0.4827(4) 0.3378(4) 0.0500(13) Uani 1 1 d . . . C24 C 0.7412(9) 0.4084(7) 0.4744(6) 0.061(2) Uani 1 1 d . . . H24A H 0.7054 0.3367 0.4817 0.091 Uiso 1 1 calc R . . H24B H 0.7927 0.4673 0.5344 0.091 Uiso 1 1 calc R . . H24C H 0.8059 0.4102 0.4436 0.091 Uiso 1 1 calc R . . C25 C 0.6168(8) 0.4254(7) 0.4178(6) 0.054(2) Uani 1 1 d . . . C26 C 0.6211(8) 0.5321(7) 0.4378(6) 0.055(2) Uani 1 1 d . . . H26A H 0.7080 0.5919 0.4814 0.066 Uiso 1 1 calc R . . C27 C 0.5053(9) 0.5568(6) 0.3977(5) 0.0507(19) Uani 1 1 d . . . C28 C 0.5260(9) 0.6769(6) 0.4237(6) 0.057(2) Uani 1 1 d . . . H28A H 0.5757 0.7135 0.3905 0.086 Uiso 1 1 calc R . . H28B H 0.5827 0.7153 0.4894 0.086 Uiso 1 1 calc R . . H28C H 0.4327 0.6789 0.4080 0.086 Uiso 1 1 calc R . . N3 N 0.0280(7) 0.5332(5) 0.2964(4) 0.0518(16) Uani 1 1 d . . . C29 C 0.1355(9) 0.6067(6) 0.2845(6) 0.0530(19) Uani 1 1 d . . . H29 H 0.1802 0.5790 0.2498 0.064 Uiso 1 1 calc R . . C30 C 0.1829(9) 0.7216(7) 0.3215(6) 0.061(2) Uani 1 1 d . . . H30 H 0.2564 0.7705 0.3106 0.073 Uiso 1 1 calc R . . C31 C 0.1200(9) 0.7623(7) 0.3742(6) 0.067(3) Uani 1 1 d . . . H31 H 0.1508 0.8396 0.4002 0.081 Uiso 1 1 calc R . . C32 C 0.0109(9) 0.6886(7) 0.3889(6) 0.063(2) Uani 1 1 d . . . H32 H -0.0322 0.7154 0.4254 0.076 Uiso 1 1 calc R . . C33 C -0.0333(8) 0.5754(7) 0.3490(5) 0.0532(19) Uani 1 1 d . . . H33 H -0.1080 0.5256 0.3583 0.064 Uiso 1 1 calc R . . N4 N 0.5623(8) 0.2663(6) 0.8060(5) 0.0651(19) Uani 1 1 d . . . C34 C 0.4255(10) 0.1887(7) 0.7757(6) 0.066(2) Uani 1 1 d . . . H34 H 0.4099 0.1139 0.7648 0.079 Uiso 1 1 calc R . . C35 C 0.3072(10) 0.2126(8) 0.7597(6) 0.071(3) Uani 1 1 d . . . H35 H 0.2142 0.1555 0.7387 0.085 Uiso 1 1 calc R . . C36 C 0.3282(10) 0.3221(8) 0.7752(6) 0.064(2) Uani 1 1 d . . . H36 H 0.2502 0.3413 0.7654 0.077 Uiso 1 1 calc R . . C37 C 0.4677(10) 0.4030(7) 0.8058(6) 0.063(2) Uani 1 1 d . . . H37 H 0.4861 0.4783 0.8168 0.075 Uiso 1 1 calc R . . C38 C 0.5791(10) 0.3711(8) 0.8196(6) 0.064(2) Uani 1 1 d . . . H38 H 0.6728 0.4269 0.8399 0.077 Uiso 1 1 calc R . . C39 C 0.5704(9) 0.9475(7) 0.5490(7) 0.065(2) Uani 1 1 d . . . C40 C 0.5026(9) 1.0033(7) 0.5877(6) 0.057(2) Uani 1 1 d . . . C41 C 0.4339(9) 1.0537(7) 0.5399(7) 0.066(2) 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 0.0504(2) 0.04326(17) 0.04613(19) 0.01363(12) 0.01179(12) 0.01708(13) Cu 0.0498(6) 0.0453(5) 0.0509(6) 0.0158(4) 0.0133(4) 0.0167(4) O1 0.055(3) 0.051(3) 0.053(3) 0.019(3) 0.023(3) 0.017(3) O2 0.053(3) 0.050(3) 0.041(3) 0.015(2) 0.014(2) 0.020(2) O3 0.050(3) 0.042(3) 0.051(3) 0.013(2) 0.015(2) 0.011(2) O4 0.052(3) 0.050(3) 0.057(3) 0.020(3) 0.019(3) 0.016(3) N1 0.061(4) 0.053(4) 0.050(4) 0.016(3) 0.020(3) 0.020(3) N2 0.044(4) 0.053(4) 0.064(5) 0.025(4) 0.020(3) 0.017(3) C1 0.053(5) 0.040(4) 0.053(5) 0.016(4) 0.001(4) 0.010(4) C2 0.056(5) 0.040(4) 0.057(5) 0.018(4) 0.017(4) 0.018(4) C3 0.054(5) 0.041(4) 0.043(4) 0.016(3) 0.009(4) 0.019(4) C4 0.052(5) 0.055(5) 0.052(5) 0.021(4) 0.012(4) 0.021(4) C5 0.059(5) 0.058(5) 0.046(5) 0.020(4) 0.010(4) 0.020(4) C6 0.049(5) 0.056(5) 0.066(6) 0.023(4) 0.023(4) 0.016(4) C7 0.055(5) 0.053(5) 0.067(6) 0.020(4) 0.018(4) 0.029(4) C8 0.047(5) 0.066(5) 0.070(6) 0.009(5) 0.021(4) 0.027(4) C9 0.064(6) 0.069(5) 0.059(6) 0.034(5) 0.026(4) 0.024(5) C10 0.055(5) 0.048(4) 0.064(6) 0.012(4) 0.026(4) 0.016(4) C11 0.059(5) 0.044(4) 0.050(5) 0.013(4) 0.020(4) 0.016(4) C12 0.059(5) 0.035(4) 0.041(4) 0.007(3) 0.007(4) 0.010(4) C13 0.052(5) 0.046(4) 0.043(4) 0.014(4) 0.008(4) 0.016(4) C14 0.069(6) 0.059(5) 0.047(5) 0.027(4) 0.020(4) 0.029(4) C15 0.078(6) 0.056(5) 0.053(5) 0.024(4) 0.024(4) 0.029(5) C16 0.059(5) 0.051(4) 0.052(5) 0.022(4) 0.021(4) 0.010(4) C17 0.053(5) 0.067(5) 0.073(6) 0.000(5) 0.030(5) 0.011(4) C18 0.057(6) 0.112(8) 0.085(7) 0.033(6) 0.033(5) 0.046(6) O5 0.051(3) 0.044(3) 0.049(3) 0.012(2) 0.008(2) 0.014(2) O6 0.052(3) 0.047(3) 0.057(3) 0.016(3) 0.018(3) 0.018(3) C19 0.072(6) 0.056(5) 0.083(7) 0.016(5) 0.023(5) 0.020(5) C20 0.060(5) 0.045(5) 0.056(5) 0.014(4) 0.015(4) 0.007(4) C21 0.063(6) 0.045(4) 0.086(7) 0.018(5) 0.026(5) 0.019(4) C22 0.078(6) 0.052(5) 0.062(6) 0.018(4) 0.027(5) 0.030(5) C23 0.074(6) 0.064(6) 0.116(9) 0.024(6) 0.046(6) 0.040(5) O7 0.054(3) 0.052(3) 0.052(3) 0.014(3) 0.013(3) 0.021(3) O8 0.041(3) 0.043(3) 0.047(3) 0.012(2) 0.006(2) 0.010(2) C24 0.066(5) 0.070(5) 0.058(5) 0.030(4) 0.028(4) 0.035(5) C25 0.041(5) 0.065(5) 0.055(5) 0.023(4) 0.020(4) 0.023(4) C26 0.043(5) 0.056(5) 0.052(5) 0.012(4) 0.017(4) 0.011(4) C27 0.058(5) 0.048(4) 0.039(4) 0.017(4) 0.021(4) 0.014(4) C28 0.058(5) 0.051(4) 0.046(5) 0.007(4) 0.008(4) 0.021(4) N3 0.059(4) 0.047(3) 0.041(4) 0.014(3) 0.012(3) 0.020(3) C29 0.061(5) 0.050(4) 0.048(5) 0.019(4) 0.019(4) 0.025(4) C30 0.062(5) 0.050(5) 0.061(6) 0.024(4) 0.015(4) 0.019(4) C31 0.063(6) 0.045(4) 0.066(6) 0.011(4) 0.006(5) 0.015(4) C32 0.057(5) 0.061(5) 0.054(5) 0.008(4) 0.011(4) 0.023(4) C33 0.049(5) 0.060(5) 0.047(5) 0.016(4) 0.016(4) 0.025(4) N4 0.065(5) 0.070(5) 0.057(5) 0.020(4) 0.019(4) 0.031(4) C34 0.071(6) 0.051(5) 0.057(6) 0.010(4) 0.016(5) 0.019(5) C35 0.052(6) 0.063(6) 0.061(6) 0.010(5) 0.009(4) 0.002(4) C36 0.056(5) 0.071(6) 0.061(6) 0.016(5) 0.016(4) 0.033(5) C37 0.069(6) 0.057(5) 0.060(6) 0.019(4) 0.025(4) 0.027(5) C38 0.066(6) 0.064(5) 0.052(5) 0.016(4) 0.026(4) 0.018(4) C39 0.051(5) 0.047(5) 0.073(6) 0.011(4) 0.020(4) 0.002(4) C40 0.051(5) 0.047(4) 0.069(6) 0.022(4) 0.027(4) 0.013(4) C41 0.052(5) 0.054(5) 0.079(7) 0.015(5) 0.023(5) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O4 2.264(5) . ? U O1 2.282(5) . ? U O5 2.345(5) . ? U O6 2.359(5) . ? U O8 2.359(5) . ? U O7 2.367(5) . ? U O2 2.452(5) . ? U O3 2.497(5) . ? U Cu 3.5741(10) . ? U Cu 7.3295(11) 1_655 ? U U 7.6064(8) 2_666 ? Cu O2 1.912(5) . ? Cu N2 1.940(6) . ? Cu N1 1.941(7) . ? Cu O3 1.944(5) . ? Cu N3 2.320(6) . ? Cu Cu 8.783(2) 2_566 ? O1 C1 1.359(9) . ? O2 C2 1.335(9) . ? O3 C12 1.332(9) . ? O4 C13 1.321(9) . ? N1 C7 1.262(10) . ? N1 C8 1.529(10) . ? N2 C10 1.262(10) . ? N2 C9 1.459(10) . ? C1 C6 1.365(12) . ? C1 C2 1.416(12) . ? C2 C3 1.425(10) . ? C3 C4 1.394(11) . ? C3 C7 1.478(11) . ? C4 C5 1.378(11) . ? C5 C6 1.419(11) . ? C8 C18 1.513(12) . ? C8 C9 1.520(12) . ? C8 C17 1.540(11) . ? C10 C11 1.453(12) . ? C11 C16 1.407(11) . ? C11 C12 1.420(11) . ? C12 C13 1.428(11) . ? C13 C14 1.394(11) . ? C14 C15 1.386(12) . ? C15 C16 1.366(12) . ? O5 C20 1.274(9) . ? O6 C22 1.264(9) . ? C19 C20 1.523(12) . ? C20 C21 1.386(12) . ? C21 C22 1.374(12) . ? C22 C23 1.513(12) . ? O7 C25 1.284(9) . ? O8 C27 1.269(8) . ? C24 C25 1.488(11) . ? C25 C26 1.381(11) . ? C26 C27 1.393(11) . ? C27 C28 1.500(10) . ? N3 C29 1.337(10) . ? N3 C33 1.355(10) . ? C29 C30 1.378(11) . ? C30 C31 1.361(12) . ? C31 C32 1.376(12) . ? C32 C33 1.367(11) . ? N4 C38 1.320(11) . ? N4 C34 1.338(11) . ? C34 C35 1.368(13) . ? C35 C36 1.367(12) . ? C36 C37 1.373(12) . ? C37 C38 1.365(12) . ? C39 C40 1.377(12) . ? C39 C41 1.418(13) 2_676 ? C40 C41 1.346(12) . ? C41 C39 1.418(13) 2_676 ? 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 O4 U O1 163.25(18) . . ? O4 U O5 82.82(18) . . ? O1 U O5 89.20(18) . . ? O4 U O6 82.19(19) . . ? O1 U O6 81.32(19) . . ? O5 U O6 71.62(18) . . ? O4 U O8 106.92(19) . . ? O1 U O8 87.88(18) . . ? O5 U O8 145.97(18) . . ? O6 U O8 140.98(18) . . ? O4 U O7 80.06(19) . . ? O1 U O7 98.21(19) . . ? O5 U O7 143.44(18) . . ? O6 U O7 74.21(18) . . ? O8 U O7 70.41(17) . . ? O4 U O2 125.04(19) . . ? O1 U O2 65.44(18) . . ? O5 U O2 72.40(17) . . ? O6 U O2 130.59(18) . . ? O8 U O2 75.59(16) . . ? O7 U O2 142.79(17) . . ? O4 U O3 65.00(18) . . ? O1 U O3 126.55(18) . . ? O5 U O3 73.29(18) . . ? O6 U O3 134.22(17) . . ? O8 U O3 81.43(17) . . ? O7 U O3 125.87(18) . . ? O2 U O3 61.16(17) . . ? O2 Cu N2 166.7(2) . . ? O2 Cu N1 95.3(3) . . ? N2 Cu N1 84.6(3) . . ? O2 Cu O3 81.6(2) . . ? N2 Cu O3 94.3(3) . . ? N1 Cu O3 161.6(2) . . ? O2 Cu N3 97.4(2) . . ? N2 Cu N3 95.8(3) . . ? N1 Cu N3 97.8(2) . . ? O3 Cu N3 100.6(2) . . ? C7 N1 C8 120.8(7) . . ? C10 N2 C9 122.6(7) . . ? O1 C1 C6 125.2(8) . . ? O1 C1 C2 115.0(8) . . ? C6 C1 C2 119.8(7) . . ? O2 C2 C1 115.2(7) . . ? O2 C2 C3 124.6(7) . . ? C1 C2 C3 120.2(8) . . ? C4 C3 C2 118.4(7) . . ? C4 C3 C7 119.4(7) . . ? C2 C3 C7 121.6(8) . . ? C5 C4 C3 120.6(7) . . ? C4 C5 C6 120.8(8) . . ? C1 C6 C5 119.8(8) . . ? N1 C7 C3 126.6(8) . . ? C18 C8 C9 110.4(7) . . ? C18 C8 N1 111.3(8) . . ? C9 C8 N1 106.6(7) . . ? C18 C8 C17 112.4(8) . . ? C9 C8 C17 109.2(8) . . ? N1 C8 C17 106.7(6) . . ? N2 C9 C8 109.1(7) . . ? N2 C10 C11 124.8(8) . . ? C16 C11 C12 117.6(8) . . ? C16 C11 C10 118.5(8) . . ? C12 C11 C10 123.5(8) . . ? O3 C12 C11 125.0(7) . . ? O3 C12 C13 113.7(8) . . ? C11 C12 C13 121.2(7) . . ? O4 C13 C14 125.5(7) . . ? O4 C13 C12 117.0(7) . . ? C14 C13 C12 117.5(8) . . ? C15 C14 C13 121.3(8) . . ? C16 C15 C14 121.0(8) . . ? C15 C16 C11 121.2(9) . . ? C20 O5 U 135.5(5) . . ? C22 O6 U 133.8(6) . . ? O5 C20 C21 124.7(8) . . ? O5 C20 C19 114.3(8) . . ? C21 C20 C19 120.9(8) . . ? C22 C21 C20 123.0(8) . . ? O6 C22 C21 127.1(8) . . ? O6 C22 C23 114.5(8) . . ? C21 C22 C23 118.4(8) . . ? C25 O7 U 138.2(5) . . ? C27 O8 U 139.0(5) . . ? O7 C25 C26 123.0(7) . . ? O7 C25 C24 117.5(7) . . ? C26 C25 C24 119.6(7) . . ? C25 C26 C27 125.0(7) . . ? O8 C27 C26 123.6(7) . . ? O8 C27 C28 116.9(7) . . ? C26 C27 C28 119.5(7) . . ? C29 N3 C33 117.6(7) . . ? C29 N3 Cu 116.9(5) . . ? C33 N3 Cu 125.3(6) . . ? N3 C29 C30 122.8(8) . . ? C31 C30 C29 118.6(9) . . ? C30 C31 C32 119.7(8) . . ? C33 C32 C31 118.9(9) . . ? N3 C33 C32 122.2(8) . . ? C38 N4 C34 115.9(8) . . ? N4 C34 C35 124.0(8) . . ? C34 C35 C36 118.8(8) . . ? C35 C36 C37 118.1(8) . . ? C38 C37 C36 119.0(8) . . ? N4 C38 C37 124.2(8) . . ? C40 C39 C41 118.4(9) . 2_676 ? C41 C40 C39 119.3(9) . . ? C40 C41 C39 122.3(9) . 2_676 ? #===END data_2 _database_code_CSD 200803 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H35 N3 O8 U Zn' _chemical_formula_weight 905.04 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.1052(7) _cell_length_b 16.7914(5) _cell_length_c 26.9961(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6393.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39762 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepipedic _exptl_crystal_colour 'translucent dark yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.880 _exptl_crystal_density_method ? _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 5.866 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.359 _exptl_absorpt_correction_T_max 0.625 _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 39762 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5870 _reflns_number_gt 4049 _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. The bridge between the two N atoms of the Schiff base was found disordered over two positions sharing one of the methyl substituents. These positions were refined with occupancy factors constrained to sum to unity and some restraints on bond lengths, angles and displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters, except the disordered atoms C8 and C9. The H atoms were introduced (except in the disordered parts) at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH2) 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^)+105.2896P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5870 _refine_ls_number_parameters 428 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.905 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.175 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 0.78221(3) 0.86330(2) 0.378752(15) 0.02440(12) Uani 1 1 d . . . Zn Zn 1.04098(8) 0.85564(8) 0.36736(5) 0.0324(3) Uani 1 1 d . . . O1 O 0.7765(5) 0.8035(4) 0.4556(3) 0.0289(17) Uani 1 1 d . . . O2 O 0.9356(5) 0.8267(4) 0.4125(3) 0.034(2) Uani 1 1 d . . . O3 O 0.9267(5) 0.8933(4) 0.3325(3) 0.0262(17) Uani 1 1 d . . . O4 O 0.7587(5) 0.9265(4) 0.3050(3) 0.0258(17) Uani 1 1 d . . . O5 O 0.8275(6) 0.7406(5) 0.3394(3) 0.034(2) Uani 1 1 d . . . O6 O 0.6464(5) 0.7879(4) 0.3580(3) 0.0271(17) Uani 1 1 d . . . O7 O 0.6464(5) 0.9325(4) 0.4064(3) 0.0278(18) Uani 1 1 d . . . O8 O 0.8298(5) 0.9863(4) 0.4165(3) 0.0255(17) Uani 1 1 d . . . N1 N 1.1151(7) 0.7559(6) 0.3933(3) 0.059(3) Uani 1 1 d DU . . N2 N 1.1051(7) 0.8310(5) 0.3004(4) 0.054(3) Uani 1 1 d DU . . N3 N 1.1097(7) 0.9455(5) 0.4047(4) 0.030(2) Uani 1 1 d . . . C1 C 0.8530(9) 0.7683(7) 0.4771(4) 0.030(3) Uani 1 1 d . . . C2 C 0.9396(9) 0.7772(7) 0.4512(5) 0.033(3) Uani 1 1 d . . . C3 C 1.0213(11) 0.7347(8) 0.4664(5) 0.046(3) Uani 1 1 d U . . C4 C 1.0187(11) 0.6941(8) 0.5116(5) 0.050(4) Uani 1 1 d U . . H4 H 1.0726 0.6682 0.5233 0.060 Uiso 1 1 calc R . . C5 C 0.9367(11) 0.6923(8) 0.5387(5) 0.049(4) Uani 1 1 d U . . H5 H 0.9369 0.6671 0.5694 0.059 Uiso 1 1 calc R . . C6 C 0.8525(11) 0.7273(7) 0.5218(5) 0.041(3) Uani 1 1 d . . . H6 H 0.7971 0.7231 0.5403 0.049 Uiso 1 1 calc R . . C7 C 1.1027(10) 0.7248(9) 0.4321(4) 0.064(4) Uani 1 1 d DU . . H7 H 1.1498 0.6897 0.4423 0.077 Uiso 1 1 calc R . . C8A C 1.1608(8) 0.7176(6) 0.3479(3) 0.067(5) Uiso 0.697(15) 1 d PDU . . C8B C 1.2001(6) 0.7594(8) 0.3603(4) 0.061(5) Uiso 0.303(15) 1 d PDU . . C9A C 1.1896(7) 0.7821(10) 0.3129(4) 0.064(4) Uiso 0.697(15) 1 d PDU . . C9B C 1.1582(8) 0.7528(5) 0.3079(3) 0.068(6) Uiso 0.303(15) 1 d PDU . . C10 C 1.0801(8) 0.8560(7) 0.2601(5) 0.051(3) Uani 1 1 d DU . . H10 H 1.1206 0.8462 0.2336 0.061 Uiso 1 1 calc R . . C11 C 0.9916(9) 0.9006(7) 0.2489(5) 0.038(3) Uani 1 1 d . . . C12 C 0.9192(9) 0.9095(6) 0.2847(4) 0.030(3) Uani 1 1 d . . . C13 C 0.8244(9) 0.9330(6) 0.2697(4) 0.029(3) Uani 1 1 d . . . C14 C 0.8092(10) 0.9582(7) 0.2215(5) 0.039(3) Uani 1 1 d . . . H14 H 0.7507 0.9783 0.2117 0.046 Uiso 1 1 calc R . . C15 C 0.8850(10) 0.9526(8) 0.1877(5) 0.040(3) Uani 1 1 d U . . H15 H 0.8755 0.9705 0.1555 0.048 Uiso 1 1 calc R . . C16 C 0.9707(10) 0.9226(8) 0.1998(5) 0.046(3) Uani 1 1 d U . . H16 H 1.0165 0.9165 0.1753 0.056 Uiso 1 1 calc R . . C17A C 1.2590(9) 0.6838(11) 0.3535(8) 0.050(5) Uani 0.697(15) 1 d PDU . . C17B C 1.2391(10) 0.7509(9) 0.2727(5) 0.068(6) Uani 0.303(15) 1 d PDU . . C18 C 1.1107(10) 0.6716(6) 0.3076(4) 0.045(3) Uani 1 1 d DU . . C19 C 0.8544(8) 0.6131(7) 0.3061(5) 0.039(3) Uani 1 1 d . . . H19A H 0.8772 0.6288 0.2741 0.058 Uiso 1 1 calc R . . H19B H 0.8207 0.5637 0.3034 0.058 Uiso 1 1 calc R . . H19C H 0.9071 0.6066 0.3283 0.058 Uiso 1 1 calc R . . C20 C 0.7894(10) 0.6759(7) 0.3258(4) 0.035(3) Uani 1 1 d . . . C21 C 0.6912(8) 0.6638(7) 0.3267(4) 0.028(3) Uani 1 1 d . . . H21 H 0.6687 0.6145 0.3163 0.034 Uiso 1 1 calc R . . C22 C 0.6243(8) 0.7201(7) 0.3420(4) 0.026(3) Uani 1 1 d . . . C23 C 0.5209(8) 0.6994(7) 0.3388(5) 0.035(3) Uani 1 1 d . . . H23A H 0.4929 0.7030 0.3711 0.053 Uiso 1 1 calc R . . H23B H 0.5141 0.6461 0.3265 0.053 Uiso 1 1 calc R . . H23C H 0.4897 0.7358 0.3168 0.053 Uiso 1 1 calc R . . C24 C 0.5207(8) 1.0191(7) 0.4292(4) 0.032(3) Uani 1 1 d . . . H24A H 0.4917 1.0223 0.3971 0.048 Uiso 1 1 calc R . . H24B H 0.5129 1.0690 0.4462 0.048 Uiso 1 1 calc R . . H24C H 0.4912 0.9775 0.4481 0.048 Uiso 1 1 calc R . . C25 C 0.6269(8) 1.0010(7) 0.4234(4) 0.026(3) Uani 1 1 d . . . C26 C 0.6914(8) 1.0603(7) 0.4353(4) 0.032(3) Uani 1 1 d . . . H26 H 0.6684 1.1093 0.4460 0.038 Uiso 1 1 calc R . . C27 C 0.7905(8) 1.0496(6) 0.4319(4) 0.027(2) Uani 1 1 d . . . C28 C 0.8525(8) 1.1146(6) 0.4511(4) 0.030(3) Uani 1 1 d . . . H28A H 0.9063 1.1209 0.4297 0.045 Uiso 1 1 calc R . . H28B H 0.8738 1.1013 0.4839 0.045 Uiso 1 1 calc R . . H28C H 0.8172 1.1635 0.4522 0.045 Uiso 1 1 calc R . . C29 C 1.2038(9) 0.9450(8) 0.4106(5) 0.046(4) Uani 1 1 d . . . H29 H 1.2389 0.9068 0.3937 0.056 Uiso 1 1 calc R . . C30 C 1.2501(8) 0.9968(8) 0.4397(5) 0.046(4) Uani 1 1 d . . . H30 H 1.3155 0.9931 0.4434 0.055 Uiso 1 1 calc R . . C31 C 1.1985(9) 1.0575(7) 0.4649(4) 0.035(3) Uani 1 1 d . . . H31 H 1.2288 1.0948 0.4848 0.042 Uiso 1 1 calc R . . C32 C 1.1035(9) 1.0582(7) 0.4584(5) 0.046(4) Uani 1 1 d . . . H32 H 1.0670 1.0965 0.4743 0.056 Uiso 1 1 calc R . . C33 C 1.0597(9) 1.0020(7) 0.4279(5) 0.041(3) Uani 1 1 d . . . H33 H 0.9943 1.0038 0.4237 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.02235(18) 0.02600(19) 0.02485(19) -0.0027(2) -0.00021(19) -0.00052(18) Zn 0.0235(6) 0.0264(6) 0.0474(9) -0.0049(6) 0.0002(6) -0.0004(6) O1 0.026(4) 0.024(4) 0.037(4) -0.002(3) -0.001(4) -0.004(4) O2 0.026(4) 0.019(4) 0.058(6) 0.001(4) 0.000(4) 0.002(3) O3 0.022(4) 0.024(4) 0.033(5) -0.003(3) 0.001(3) -0.001(3) O4 0.021(4) 0.033(4) 0.023(4) 0.002(3) 0.003(3) 0.003(3) O5 0.029(5) 0.029(5) 0.043(5) -0.003(4) 0.006(4) -0.004(4) O6 0.033(4) 0.026(4) 0.023(4) -0.005(3) -0.001(3) -0.004(3) O7 0.022(4) 0.022(4) 0.039(5) -0.007(3) 0.005(3) -0.003(3) O8 0.021(4) 0.019(4) 0.036(5) -0.003(3) 0.006(3) 0.000(3) N1 0.043(5) 0.051(5) 0.083(7) 0.004(5) 0.000(5) 0.009(5) N2 0.038(5) 0.059(6) 0.065(6) -0.018(5) 0.004(5) -0.002(5) N3 0.032(6) 0.023(5) 0.035(6) 0.009(4) 0.003(5) -0.003(4) C1 0.040(7) 0.029(6) 0.021(6) -0.005(5) -0.011(5) -0.008(5) C2 0.033(7) 0.018(6) 0.050(8) -0.002(5) -0.007(6) 0.002(5) C3 0.050(7) 0.030(6) 0.059(7) 0.003(5) -0.019(6) -0.003(6) C4 0.058(7) 0.034(6) 0.058(7) 0.007(6) -0.034(6) -0.001(6) C5 0.066(8) 0.036(6) 0.046(7) 0.001(5) -0.017(6) 0.009(6) C6 0.063(9) 0.030(7) 0.030(7) -0.001(5) -0.006(6) -0.009(7) C7 0.044(7) 0.056(7) 0.091(9) 0.025(7) 0.000(7) 0.001(6) C10 0.038(6) 0.057(7) 0.057(7) -0.016(6) 0.010(6) -0.008(6) C11 0.046(8) 0.032(7) 0.038(7) -0.021(6) 0.011(6) -0.015(6) C12 0.040(7) 0.017(6) 0.034(7) -0.010(5) -0.002(5) -0.011(5) C13 0.045(7) 0.017(6) 0.024(6) -0.009(5) 0.000(5) -0.010(5) C14 0.052(9) 0.022(6) 0.041(8) -0.003(5) 0.009(6) -0.020(6) C15 0.058(7) 0.041(6) 0.021(6) -0.005(5) 0.004(5) -0.016(6) C16 0.049(7) 0.048(7) 0.042(7) -0.008(6) 0.015(6) -0.015(6) C17A 0.049(9) 0.048(9) 0.052(9) -0.003(7) 0.002(7) 0.005(7) C17B 0.068(7) 0.067(7) 0.069(7) 0.043(6) 0.049(6) 0.041(6) C18 0.057(7) 0.037(6) 0.041(6) -0.016(5) -0.004(6) -0.002(6) C19 0.027(6) 0.034(7) 0.056(9) -0.006(6) 0.009(6) -0.003(5) C20 0.047(8) 0.023(6) 0.036(7) 0.003(5) -0.003(6) 0.001(6) C21 0.029(6) 0.030(6) 0.024(6) -0.008(5) -0.002(5) -0.006(5) C22 0.026(6) 0.034(7) 0.019(6) 0.008(5) -0.006(5) -0.005(5) C23 0.030(7) 0.026(6) 0.049(8) -0.002(6) -0.007(6) -0.006(5) C24 0.029(6) 0.032(6) 0.036(7) -0.016(5) -0.004(5) 0.003(5) C25 0.030(6) 0.031(7) 0.018(6) 0.000(5) 0.005(5) -0.003(5) C26 0.033(7) 0.028(6) 0.034(7) 0.001(5) 0.000(5) 0.005(5) C27 0.026(6) 0.026(6) 0.030(6) -0.001(5) -0.008(5) 0.001(5) C28 0.033(6) 0.026(6) 0.031(6) -0.012(5) -0.007(5) -0.003(5) C29 0.035(8) 0.060(9) 0.044(8) -0.026(7) 0.012(6) -0.003(7) C30 0.014(6) 0.068(10) 0.057(9) -0.034(7) 0.000(5) 0.000(6) C31 0.038(8) 0.039(7) 0.029(7) -0.007(5) 0.001(5) -0.014(6) C32 0.037(8) 0.024(7) 0.078(11) -0.024(7) 0.003(7) -0.008(6) C33 0.027(7) 0.029(7) 0.066(10) -0.014(6) -0.008(6) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O4 2.280(7) . ? U O1 2.305(7) . ? U O7 2.361(7) . ? U O6 2.364(7) . ? U O8 2.398(7) . ? U O5 2.404(8) . ? U O2 2.428(8) . ? U O3 2.442(7) . ? U Zn 3.6653(13) . ? Zn O3 1.971(7) . ? Zn O2 1.983(8) . ? Zn N3 2.057(10) . ? Zn N2 2.063(11) . ? Zn N1 2.094(11) . ? O1 C1 1.360(14) . ? O1 O2 2.557(11) . ? O2 C2 1.336(14) . ? O2 O3 2.436(11) . ? O2 N1 2.845(13) . ? O3 C12 1.323(13) . ? O3 O4 2.545(10) . ? O3 N2 2.861(12) . ? O4 C13 1.334(13) . ? O5 C20 1.267(14) . ? O6 C22 1.258(13) . ? O7 C25 1.268(13) . ? O8 C27 1.269(13) . ? N1 C7 1.185(11) . ? N1 C8B 1.495(5) . ? N1 C8A 1.526(5) . ? N1 N2 2.809(12) . ? N2 C10 1.218(11) . ? N2 C9A 1.486(5) . ? N2 C9B 1.525(5) . ? N3 C33 1.338(15) . ? N3 C29 1.337(16) . ? C1 C6 1.391(16) . ? C1 C2 1.414(17) . ? C2 C3 1.417(17) . ? C3 C4 1.399(18) . ? C3 C7 1.485(18) . ? C4 C5 1.37(2) . ? C5 C6 1.401(19) . ? C8A C9A 1.494(5) . ? C8A C17A 1.505(5) . ? C8A C18 1.510(5) . ? C8B C9B 1.536(5) . ? C9B C17B 1.486(5) . ? C9B C18 1.520(5) . ? C10 C11 1.487(16) . ? C11 C16 1.407(19) . ? C11 C12 1.415(17) . ? C12 C13 1.452(17) . ? C13 C14 1.385(16) . ? C14 C15 1.407(17) . ? C15 C16 1.349(19) . ? C19 C20 1.494(16) . ? C20 C21 1.401(17) . ? C21 C22 1.397(16) . ? C22 C23 1.502(15) . ? C24 C25 1.537(15) . ? C25 C26 1.387(16) . ? C26 C27 1.413(16) . ? C27 C28 1.492(14) . ? C29 C30 1.342(17) . ? C30 C31 1.425(16) . ? C31 C32 1.352(17) . ? C32 C33 1.397(16) . ? 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 O4 U O1 169.4(3) . . ? O4 U O7 85.9(3) . . ? O1 U O7 84.4(3) . . ? O4 U O6 85.7(3) . . ? O1 U O6 87.2(3) . . ? O7 U O6 71.4(2) . . ? O4 U O8 90.6(3) . . ? O1 U O8 90.2(3) . . ? O7 U O8 70.7(2) . . ? O6 U O8 142.1(2) . . ? O4 U O5 93.0(3) . . ? O1 U O5 91.9(3) . . ? O7 U O5 141.0(3) . . ? O6 U O5 69.6(3) . . ? O8 U O5 148.3(3) . . ? O4 U O2 125.1(3) . . ? O1 U O2 65.3(3) . . ? O7 U O2 136.8(3) . . ? O6 U O2 132.5(3) . . ? O8 U O2 79.0(3) . . ? O5 U O2 73.3(3) . . ? O4 U O3 65.1(2) . . ? O1 U O3 125.4(3) . . ? O7 U O3 137.4(2) . . ? O6 U O3 131.8(2) . . ? O8 U O3 78.8(2) . . ? O5 U O3 74.3(3) . . ? O2 U O3 60.0(3) . . ? O3 Zn O2 76.1(3) . . ? O3 Zn N3 112.6(3) . . ? O2 Zn N3 103.4(4) . . ? O3 Zn N2 90.3(3) . . ? O2 Zn N2 144.9(4) . . ? N3 Zn N2 111.7(4) . . ? O3 Zn N1 145.5(4) . . ? O2 Zn N1 88.5(3) . . ? N3 Zn N1 100.8(4) . . ? N2 Zn N1 85.0(3) . . ? C7 N1 C8B 131.5(11) . . ? C7 N1 C8A 125.9(10) . . ? C10 N2 C9A 128.8(10) . . ? C10 N2 C9B 123.9(9) . . ? O1 C1 C6 125.6(11) . . ? O1 C1 C2 115.3(10) . . ? C6 C1 C2 119.0(12) . . ? O2 C2 C1 114.6(10) . . ? O2 C2 C3 125.0(12) . . ? C1 C2 C3 120.4(12) . . ? C4 C3 C2 118.5(14) . . ? C4 C3 C7 120.7(13) . . ? C2 C3 C7 120.3(13) . . ? C5 C4 C3 119.9(13) . . ? C4 C5 C6 122.2(13) . . ? C1 C6 C5 119.1(13) . . ? N1 C7 C3 128.1(15) . . ? C9A C8A C17A 95.0(11) . . ? C9A C8A C18 92.5(9) . . ? C17A C8A C18 108.1(11) . . ? C9A C8A N1 108.4(5) . . ? C17A C8A N1 117.9(10) . . ? C18 C8A N1 126.6(9) . . ? N1 C8B C9B 103.7(4) . . ? N2 C9A C8A 109.0(5) . . ? C17B C9B C18 108.5(4) . . ? C17B C9B N2 108.1(4) . . ? C18 C9B N2 123.7(9) . . ? C17B C9B C8B 107.1(5) . . ? C18 C9B C8B 103.8(4) . . ? N2 C9B C8B 104.4(4) . . ? N2 C10 C11 126.8(13) . . ? C16 C11 C12 117.7(13) . . ? C16 C11 C10 120.1(12) . . ? C12 C11 C10 121.3(12) . . ? O3 C12 C11 126.0(12) . . ? O3 C12 C13 113.7(10) . . ? C11 C12 C13 120.1(11) . . ? O4 C13 C14 126.1(11) . . ? O4 C13 C12 114.7(10) . . ? C14 C13 C12 119.2(11) . . ? C13 C14 C15 118.0(13) . . ? C16 C15 C14 123.3(13) . . ? C15 C16 C11 120.9(12) . . ? O5 C20 C21 122.6(11) . . ? O5 C20 C19 116.6(12) . . ? C21 C20 C19 120.7(11) . . ? C22 C21 C20 125.1(11) . . ? O6 C22 C21 123.2(10) . . ? O6 C22 C23 118.0(10) . . ? C21 C22 C23 118.8(10) . . ? O7 C25 C26 126.3(11) . . ? O7 C25 C24 115.4(10) . . ? C26 C25 C24 118.2(10) . . ? C25 C26 C27 122.9(11) . . ? O8 C27 C26 124.1(11) . . ? O8 C27 C28 118.1(10) . . ? C26 C27 C28 117.6(10) . . ? N3 C29 C30 123.3(12) . . ? C29 C30 C31 119.6(11) . . ? C32 C31 C30 116.8(11) . . ? C31 C32 C33 120.6(12) . . ? N3 C33 C32 121.5(12) . . ? #===END data_3.1.5py _database_code_CSD 200804 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.50 H39.50 Cu2 N5.50 O8 U' _chemical_formula_weight 1132.42 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 P2~1~/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 10.3373(5) _cell_length_b 13.4223(11) _cell_length_c 31.0552(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.315(5) _cell_angle_gamma 90.00 _cell_volume 4308.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25869 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'translucent dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method ? _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 4.786 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_T_max 0.787 _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 25869 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.0950 _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 -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7837 _reflns_number_gt 5201 _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. The bridge C27-C26 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. One pyridine molecule was refined as an idealized hexagon with some restraints on displacement parameters and an occupation factor of 0.5. All non-hydrogen atoms were refined with anisotropic displacement parameters, except for C35 and C36, which behave badly and were refined with a fixed isotropic displacement parameter. The H atoms were introduced at calculated positions as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH2) or 1.5 (CH3) times that of the parent atom. A void of 72 A^3^ likely indicates the presence of an unresolved solvent molecule. The highest residual electron density peak is located near Cu1, 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^)+(0.0577P)^2^+57.3693P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7837 _refine_ls_number_parameters 548 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.246 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.627 _refine_diff_density_min -1.238 _refine_diff_density_rms 0.176 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 -1.01655(5) -0.49353(4) 0.142821(17) 0.02934(18) Uani 1 1 d . . . Cu1 Cu -0.84968(18) -0.57743(16) 0.23568(6) 0.0404(5) Uani 1 1 d . . . Cu2 Cu -1.17826(18) -0.38237(15) 0.05430(6) 0.0396(5) Uani 1 1 d D . . O1 O -0.9811(9) -0.3260(7) 0.1569(3) 0.037(2) Uani 1 1 d . . . O2 O -0.9001(10) -0.4604(8) 0.2082(3) 0.040(3) Uani 1 1 d . . . O3 O -0.9370(9) -0.6277(9) 0.1876(3) 0.043(3) Uani 1 1 d . . . O4 O -1.0623(9) -0.6565(7) 0.1186(3) 0.034(2) Uani 1 1 d . . . N1 N -0.7575(13) -0.5207(11) 0.2826(4) 0.046(4) Uani 1 1 d . . . N2 N -0.8076(12) -0.7069(12) 0.2589(4) 0.045(4) Uani 1 1 d . . . C1 C -0.9127(14) -0.2932(13) 0.1919(6) 0.045(4) Uani 1 1 d . . . C2 C -0.8682(15) -0.3671(13) 0.2205(5) 0.039(4) Uani 1 1 d . . . C3 C -0.7966(16) -0.3471(12) 0.2588(6) 0.044(4) Uani 1 1 d . . . C4 C -0.7746(17) -0.2471(13) 0.2682(6) 0.047(4) Uani 1 1 d . . . H4 H -0.7313 -0.2305 0.2936 0.056 Uiso 1 1 calc R . . C5 C -0.8140(16) -0.1748(13) 0.2420(6) 0.048(5) Uani 1 1 d . . . H5 H -0.7929 -0.1093 0.2488 0.058 Uiso 1 1 calc R . . C6 C -0.8894(16) -0.1947(14) 0.2029(6) 0.049(4) Uani 1 1 d . . . H6 H -0.9208 -0.1428 0.1860 0.059 Uiso 1 1 calc R . . C7 C -0.7458(15) -0.4276(14) 0.2857(5) 0.042(4) Uani 1 1 d . . . H7 H -0.6965 -0.4064 0.3091 0.051 Uiso 1 1 calc R . . C8 C -0.6885(14) -0.5997(13) 0.3084(5) 0.043(4) Uani 1 1 d . . . C9 C -0.7581(18) -0.6944(14) 0.3038(6) 0.056(5) Uani 1 1 d . . . H9A H -0.8300 -0.6960 0.3237 0.068 Uiso 1 1 calc R . . H9B H -0.7006 -0.7492 0.3109 0.068 Uiso 1 1 calc R . . C10 C -0.8413(15) -0.7904(13) 0.2420(6) 0.043(4) Uani 1 1 d . . . H10 H -0.8250 -0.8480 0.2577 0.052 Uiso 1 1 calc R . . C11 C -0.8994(16) -0.8008(13) 0.2025(6) 0.046(4) Uani 1 1 d . . . C12 C -0.9514(15) -0.7245(12) 0.1761(5) 0.039(4) Uani 1 1 d . . . C13 C -1.0183(14) -0.7371(11) 0.1382(5) 0.035(3) Uani 1 1 d . . . C14 C -1.0347(15) -0.8356(12) 0.1232(6) 0.049(4) Uani 1 1 d . . . H14 H -1.0794 -0.8478 0.0977 0.059 Uiso 1 1 calc R . . C15 C -0.9822(18) -0.9165(14) 0.1476(6) 0.053(5) Uani 1 1 d . . . H15 H -0.9912 -0.9809 0.1369 0.064 Uiso 1 1 calc R . . C16 C -0.9218(17) -0.9031(12) 0.1843(7) 0.052(5) Uani 1 1 d . . . H16 H -0.8922 -0.9583 0.1996 0.062 Uiso 1 1 calc R . . C17 C -0.684(2) -0.5661(17) 0.3565(6) 0.070(6) Uani 1 1 d . . . H17A H -0.7695 -0.5461 0.3653 0.105 Uiso 1 1 calc R . . H17B H -0.6260 -0.5109 0.3596 0.105 Uiso 1 1 calc R . . H17C H -0.6554 -0.6204 0.3741 0.105 Uiso 1 1 calc R . . C18 C -0.5520(16) -0.6098(13) 0.2901(6) 0.050(4) Uani 1 1 d . . . H18A H -0.5049 -0.6590 0.3063 0.075 Uiso 1 1 calc R . . H18B H -0.5082 -0.5468 0.2922 0.075 Uiso 1 1 calc R . . H18C H -0.5571 -0.6298 0.2605 0.075 Uiso 1 1 calc R . . O5 O -1.1978(9) -0.4872(7) 0.1867(3) 0.032(2) Uani 1 1 d . . . O6 O -1.2161(9) -0.4369(8) 0.1078(3) 0.036(2) Uani 1 1 d . . . O7 O -1.0170(9) -0.4359(8) 0.0691(3) 0.034(2) Uani 1 1 d . . . O8 O -0.8202(8) -0.5034(8) 0.1078(3) 0.033(2) Uani 1 1 d . . . N3 N -1.3419(9) -0.3159(7) 0.0450(3) 0.069(4) Uani 1 1 d DU . . N4 N -1.1202(9) -0.3300(10) -0.0006(2) 0.055(3) Uani 1 1 d DU . . C19 C -1.3100(14) -0.4487(11) 0.1751(5) 0.035(4) Uani 1 1 d . . . C20 C -1.3218(13) -0.4181(12) 0.1313(5) 0.036(4) Uani 1 1 d . . . C21 C -1.4284(15) -0.3643(13) 0.1148(6) 0.045(4) Uani 1 1 d . . . C22 C -1.5350(16) -0.3505(14) 0.1444(6) 0.052(5) Uani 1 1 d . . . H22 H -1.6090 -0.3169 0.1353 0.063 Uiso 1 1 calc R . . C23 C -1.5274(17) -0.3858(15) 0.1848(7) 0.059(5) Uani 1 1 d . . . H23 H -1.5985 -0.3779 0.2027 0.070 Uiso 1 1 calc R . . C24 C -1.4171(15) -0.4340(12) 0.2012(6) 0.042(4) Uani 1 1 d . . . H24 H -1.4158 -0.4562 0.2295 0.051 Uiso 1 1 calc R . . C25 C -1.4303(15) -0.3170(12) 0.0720(4) 0.055(5) Uani 1 1 d D . . H25 H -1.5062 -0.2843 0.0643 0.066 Uiso 1 1 calc R . . C26 C -1.3317(6) -0.2385(5) 0.0106(2) 0.070(4) Uani 1 1 d DU . . C27 C -1.2315(9) -0.2757(8) -0.02087(19) 0.056(3) Uani 1 1 d DU . . H27A H -1.2735 -0.3198 -0.0414 0.067 Uiso 1 1 calc R . . H27B H -1.1979 -0.2193 -0.0368 0.067 Uiso 1 1 calc R . . C28 C -1.0086(8) -0.3452(11) -0.0160(5) 0.042(4) Uani 1 1 d D . . H28 H -0.9948 -0.3231 -0.0440 0.050 Uiso 1 1 calc R . . C29 C -0.9073(14) -0.3902(12) 0.0039(5) 0.036(4) Uani 1 1 d . . . C30 C -0.9089(14) -0.4314(11) 0.0461(5) 0.033(3) Uani 1 1 d . . . C31 C -0.7989(15) -0.4699(11) 0.0675(5) 0.038(4) Uani 1 1 d . . . C32 C -0.6833(15) -0.4736(12) 0.0453(6) 0.041(4) Uani 1 1 d . . . H32 H -0.6098 -0.5002 0.0583 0.049 Uiso 1 1 calc R . . C33 C -0.6777(17) -0.4368(13) 0.0029(6) 0.048(4) Uani 1 1 d . . . H33 H -0.5994 -0.4393 -0.0116 0.058 Uiso 1 1 calc R . . C34 C -0.7844(17) -0.3972(13) -0.0178(6) 0.049(4) Uani 1 1 d . . . H34 H -0.7771 -0.3749 -0.0461 0.058 Uiso 1 1 calc R . . C35 C -1.2828(14) -0.1416(6) 0.0292(5) 0.080 Uiso 1 1 d D . . H35A H -1.3471 -0.0908 0.0253 0.120 Uiso 1 1 calc R . . H35B H -1.2047 -0.1224 0.0148 0.120 Uiso 1 1 calc R . . H35C H -1.2655 -0.1500 0.0594 0.120 Uiso 1 1 calc R . . C36 C -1.4582(8) -0.2287(12) -0.0135(4) 0.080 Uiso 1 1 d D . . H36A H -1.4991 -0.2928 -0.0154 0.120 Uiso 1 1 calc R . . H36B H -1.4423 -0.2038 -0.0420 0.120 Uiso 1 1 calc R . . H36C H -1.5138 -0.1834 0.0015 0.120 Uiso 1 1 calc R . . N5 N -0.5205(15) -0.3369(12) 0.3681(5) 0.056(4) Uani 1 1 d . . . C37 C -0.410(3) -0.298(2) 0.3529(9) 0.096(8) Uani 1 1 d U . . H37 H -0.3510 -0.3414 0.3403 0.115 Uiso 1 1 calc R . . C38 C -0.379(3) -0.197(2) 0.3547(8) 0.094(8) Uani 1 1 d U . . H38 H -0.2955 -0.1742 0.3489 0.113 Uiso 1 1 calc R . . C39 C -0.4738(16) -0.1335(13) 0.3654(6) 0.050(5) Uani 1 1 d . . . H39 H -0.4610 -0.0651 0.3631 0.060 Uiso 1 1 calc R . . C40 C -0.5864(18) -0.1688(16) 0.3792(6) 0.054(5) Uani 1 1 d . . . H40 H -0.6509 -0.1251 0.3880 0.065 Uiso 1 1 calc R . . C41 C -0.6069(17) -0.2690(17) 0.3804(6) 0.058(5) Uani 1 1 d . . . H41 H -0.6863 -0.2915 0.3904 0.069 Uiso 1 1 calc R . . N6 N -0.710(3) -0.102(2) 0.1108(6) 0.074(4) Uani 0.50 1 d PGU . . C42 C -0.797(2) -0.166(2) 0.0913(8) 0.074(4) Uani 0.50 1 d PGU . . H42 H -0.8547 -0.2028 0.1080 0.088 Uiso 0.50 1 calc PR . . C43 C -0.800(2) -0.176(2) 0.0467(8) 0.074(4) Uani 0.50 1 d PGU . . H43 H -0.8582 -0.2193 0.0336 0.088 Uiso 0.50 1 calc PR . . C44 C -0.714(3) -0.122(2) 0.0217(6) 0.074(4) Uani 0.50 1 d PGU . . H44 H -0.7153 -0.1282 -0.0081 0.088 Uiso 0.50 1 calc PR . . C45 C -0.626(2) -0.057(2) 0.0412(8) 0.074(4) Uani 0.50 1 d PGU . . H45 H -0.5690 -0.0205 0.0244 0.088 Uiso 0.50 1 calc PR . . C46 C -0.624(2) -0.0472(19) 0.0857(8) 0.073(4) Uani 0.50 1 d PGU . . H46 H -0.5656 -0.0040 0.0988 0.088 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 0.0281(3) 0.0322(3) 0.0277(3) 0.0006(3) 0.00056(17) 0.0016(3) Cu1 0.0341(10) 0.0547(13) 0.0325(10) 0.0037(9) -0.0025(8) 0.0023(9) Cu2 0.0383(11) 0.0477(12) 0.0329(10) 0.0068(9) -0.0002(8) 0.0070(9) O1 0.035(6) 0.030(6) 0.045(6) -0.003(5) 0.001(5) -0.001(5) O2 0.042(6) 0.042(6) 0.035(6) -0.006(5) -0.009(5) -0.006(5) O3 0.029(6) 0.058(8) 0.043(7) 0.018(6) 0.001(5) 0.006(5) O4 0.033(6) 0.031(6) 0.039(6) 0.000(5) 0.001(4) -0.002(5) N1 0.046(8) 0.050(10) 0.042(8) -0.004(7) 0.002(6) 0.000(7) N2 0.030(7) 0.065(10) 0.040(8) 0.012(7) 0.004(6) 0.005(7) C1 0.022(8) 0.054(11) 0.060(12) -0.012(9) 0.016(7) -0.009(8) C2 0.034(9) 0.053(11) 0.031(9) -0.001(8) 0.003(7) -0.002(8) C3 0.044(10) 0.035(9) 0.054(11) -0.009(8) 0.013(8) -0.013(8) C4 0.059(11) 0.037(10) 0.044(10) 0.011(8) 0.003(8) 0.010(8) C5 0.054(11) 0.039(10) 0.052(11) -0.030(8) 0.011(8) -0.020(8) C6 0.048(10) 0.048(11) 0.051(12) 0.004(9) 0.017(8) -0.004(8) C7 0.030(9) 0.070(13) 0.027(8) 0.005(8) 0.003(6) 0.005(8) C8 0.030(8) 0.050(11) 0.048(10) 0.018(8) -0.009(7) -0.006(7) C9 0.048(11) 0.053(12) 0.069(13) 0.006(10) -0.006(9) -0.001(9) C10 0.038(9) 0.043(10) 0.049(11) -0.003(8) 0.006(8) -0.002(8) C11 0.041(10) 0.039(10) 0.059(12) 0.016(9) 0.010(8) -0.004(8) C12 0.038(9) 0.031(9) 0.048(10) 0.004(7) 0.017(7) -0.004(7) C13 0.038(9) 0.033(8) 0.035(9) 0.001(7) 0.010(7) -0.004(7) C14 0.034(9) 0.036(10) 0.077(13) 0.002(9) 0.003(8) 0.004(7) C15 0.057(11) 0.042(11) 0.060(12) -0.010(9) -0.001(9) 0.001(9) C16 0.045(10) 0.025(9) 0.086(15) 0.007(9) 0.021(10) -0.001(8) C17 0.092(16) 0.072(15) 0.045(11) 0.010(10) -0.020(11) -0.006(12) C18 0.046(10) 0.040(10) 0.062(12) 0.017(9) -0.010(8) -0.004(8) O5 0.029(5) 0.029(6) 0.039(6) -0.001(5) 0.002(4) 0.005(4) O6 0.031(6) 0.046(7) 0.032(6) -0.004(5) -0.001(4) 0.008(5) O7 0.031(5) 0.044(6) 0.026(5) 0.002(5) 0.007(4) 0.003(5) O8 0.027(5) 0.035(6) 0.038(5) -0.004(5) 0.001(4) 0.002(5) N3 0.069(4) 0.070(4) 0.069(4) 0.0005(17) 0.0003(17) 0.0011(17) N4 0.056(3) 0.056(3) 0.055(3) 0.0010(17) -0.0011(17) -0.0009(17) C19 0.034(9) 0.029(8) 0.043(9) 0.003(7) 0.011(7) -0.011(7) C20 0.019(7) 0.047(10) 0.041(9) -0.002(7) 0.005(6) -0.003(7) C21 0.032(9) 0.043(10) 0.060(12) -0.021(8) 0.001(8) 0.005(7) C22 0.031(9) 0.062(12) 0.065(13) -0.003(10) 0.008(8) 0.002(8) C23 0.033(10) 0.070(14) 0.073(14) -0.004(11) 0.014(9) 0.001(9) C24 0.034(9) 0.040(10) 0.053(10) -0.010(8) 0.013(7) -0.009(7) C25 0.060(12) 0.050(11) 0.054(11) -0.001(9) -0.025(9) 0.029(9) C26 0.070(4) 0.070(4) 0.070(4) 0.0003(12) 0.0003(12) 0.0008(12) C27 0.056(3) 0.056(3) 0.055(3) 0.0008(12) -0.0006(12) -0.0007(12) C28 0.044(10) 0.051(11) 0.031(8) 0.002(7) -0.007(7) -0.015(8) C29 0.032(8) 0.039(9) 0.037(9) -0.007(7) 0.006(6) -0.011(7) C30 0.032(8) 0.031(9) 0.036(8) -0.002(7) 0.006(6) -0.007(6) C31 0.034(8) 0.031(9) 0.047(10) -0.005(7) 0.016(7) -0.006(6) C32 0.030(8) 0.041(10) 0.052(10) -0.005(7) 0.004(7) -0.009(7) C33 0.044(10) 0.045(11) 0.057(11) -0.014(9) 0.024(8) -0.005(8) C34 0.059(12) 0.043(10) 0.044(10) -0.002(8) 0.014(8) -0.021(9) N5 0.052(9) 0.052(10) 0.065(11) -0.012(8) 0.001(8) -0.014(8) C37 0.096(8) 0.096(8) 0.096(8) -0.0001(13) 0.0010(13) 0.0001(13) C38 0.094(8) 0.094(8) 0.094(8) 0.0001(13) 0.0008(13) -0.0001(13) C39 0.040(10) 0.040(10) 0.069(13) -0.014(9) -0.013(9) 0.009(8) C40 0.058(12) 0.065(14) 0.040(11) -0.001(9) 0.010(8) 0.015(10) C41 0.030(9) 0.083(16) 0.059(12) 0.005(11) 0.002(8) -0.003(10) N6 0.073(4) 0.074(4) 0.074(4) 0.0000(8) 0.0003(8) 0.0001(8) C42 0.074(4) 0.073(4) 0.074(4) 0.0000(8) 0.0003(8) 0.0000(8) C43 0.074(4) 0.074(4) 0.074(4) 0.0000(8) 0.0003(8) 0.0000(8) C44 0.074(4) 0.074(4) 0.074(4) 0.0000(8) 0.0003(8) 0.0000(8) C45 0.074(4) 0.074(4) 0.074(4) 0.0001(8) 0.0004(8) 0.0000(8) C46 0.074(4) 0.073(4) 0.074(4) 0.0000(8) 0.0003(8) 0.0000(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 2.311(9) . ? U O1 2.320(10) . ? U O5 2.325(9) . ? U O4 2.360(10) . ? U O2 2.395(10) . ? U O3 2.417(10) . ? U O7 2.417(9) . ? U O6 2.448(10) . ? U Cu1 3.536(2) . ? U Cu2 3.5394(19) . ? Cu1 O2 1.862(11) . ? Cu1 O3 1.867(12) . ? Cu1 N1 1.897(14) . ? Cu1 N2 1.930(15) . ? Cu2 O6 1.858(10) . ? Cu2 O7 1.870(10) . ? Cu2 N3 1.933(7) . ? Cu2 N4 1.942(8) . ? O1 C1 1.36(2) . ? O2 C2 1.350(19) . ? O2 O3 2.365(16) . ? O2 N1 2.853(17) . ? O3 C12 1.355(19) . ? O3 N2 2.792(17) . ? O4 C13 1.321(18) . ? N1 C7 1.26(2) . ? N1 C8 1.51(2) . ? N1 N2 2.65(2) . ? N2 C10 1.29(2) . ? N2 C9 1.49(2) . ? C1 C6 1.39(2) . ? C1 C2 1.41(2) . ? C2 C3 1.42(2) . ? C3 C4 1.39(2) . ? C3 C7 1.46(2) . ? C4 C5 1.33(2) . ? C5 C6 1.46(2) . ? C8 C9 1.47(2) . ? C8 C18 1.53(2) . ? C8 C17 1.56(2) . ? C10 C11 1.37(2) . ? C11 C12 1.42(2) . ? C11 C16 1.50(2) . ? C12 C13 1.37(2) . ? C13 C14 1.41(2) . ? C14 C15 1.43(2) . ? C15 C16 1.31(3) . ? O5 C19 1.318(18) . ? O6 C20 1.342(16) . ? O6 O7 2.388(13) . ? O6 N3 2.846(12) . ? O7 C30 1.331(16) . ? O7 N4 2.795(12) . ? O8 C31 1.349(18) . ? N3 C25 1.243(10) . ? N3 C26 1.494(11) . ? N3 N4 2.708(8) . ? N4 C28 1.267(10) . ? N4 C27 1.498(13) . ? C19 C24 1.39(2) . ? C19 C20 1.43(2) . ? C20 C21 1.41(2) . ? C21 C22 1.45(2) . ? C21 C25 1.47(2) . ? C22 C23 1.34(3) . ? C23 C24 1.40(2) . ? C26 C36 1.509(11) . ? C26 C35 1.509(12) . ? C26 C27 1.513(10) . ? C28 C29 1.355(18) . ? C29 C30 1.42(2) . ? C29 C34 1.45(2) . ? C30 C31 1.41(2) . ? C31 C32 1.38(2) . ? C32 C33 1.41(2) . ? C33 C34 1.38(2) . ? N5 C41 1.33(2) . ? N5 C37 1.34(3) . ? C37 C38 1.40(4) . ? C38 C39 1.34(3) . ? C39 C40 1.33(2) . ? C40 C41 1.36(3) . ? 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 O1 90.4(4) . . ? O8 U O5 172.1(3) . . ? O1 U O5 88.9(3) . . ? O8 U O4 88.4(3) . . ? O1 U O4 171.8(4) . . ? O5 U O4 93.4(3) . . ? O8 U O2 88.3(3) . . ? O1 U O2 65.3(4) . . ? O5 U O2 84.2(3) . . ? O4 U O2 122.7(4) . . ? O8 U O3 86.0(3) . . ? O1 U O3 124.1(4) . . ? O5 U O3 87.9(3) . . ? O4 U O3 63.9(4) . . ? O2 U O3 58.9(4) . . ? O8 U O7 64.6(3) . . ? O1 U O7 82.4(4) . . ? O5 U O7 123.1(3) . . ? O4 U O7 89.7(3) . . ? O2 U O7 137.9(4) . . ? O3 U O7 141.5(4) . . ? O8 U O6 123.3(3) . . ? O1 U O6 85.1(4) . . ? O5 U O6 64.5(3) . . ? O4 U O6 88.8(3) . . ? O2 U O6 137.5(4) . . ? O3 U O6 140.4(3) . . ? O7 U O6 58.8(3) . . ? Cu1 U Cu2 173.62(5) . . ? O2 Cu1 O3 78.7(5) . . ? O2 Cu1 N1 98.8(5) . . ? O3 Cu1 N1 176.9(6) . . ? O2 Cu1 N2 173.4(6) . . ? O3 Cu1 N2 94.6(6) . . ? N1 Cu1 N2 87.8(6) . . ? O6 Cu2 O7 79.7(4) . . ? O6 Cu2 N3 97.3(3) . . ? O7 Cu2 N3 172.9(5) . . ? O6 Cu2 N4 174.0(3) . . ? O7 Cu2 N4 94.3(3) . . ? N3 Cu2 N4 88.6(4) . . ? C7 N1 C8 127.9(15) . . ? C10 N2 C9 124.9(15) . . ? O1 C1 C6 126.3(17) . . ? O1 C1 C2 116.2(15) . . ? C6 C1 C2 117.4(17) . . ? O2 C2 C1 113.3(14) . . ? O2 C2 C3 122.5(15) . . ? C1 C2 C3 124.2(16) . . ? C4 C3 C2 116.2(17) . . ? C4 C3 C7 122.2(16) . . ? C2 C3 C7 121.5(15) . . ? C5 C4 C3 121.7(18) . . ? C4 C5 C6 122.4(16) . . ? C1 C6 C5 118.0(17) . . ? N1 C7 C3 131.0(16) . . ? C9 C8 N1 109.1(13) . . ? C9 C8 C18 109.9(15) . . ? N1 C8 C18 107.5(13) . . ? C9 C8 C17 110.8(15) . . ? N1 C8 C17 108.4(15) . . ? C18 C8 C17 111.1(14) . . ? C8 C9 N2 110.7(15) . . ? N2 C10 C11 125.0(17) . . ? C10 C11 C12 127.4(17) . . ? C10 C11 C16 119.8(16) . . ? C12 C11 C16 112.7(16) . . ? O3 C12 C13 113.5(14) . . ? O3 C12 C11 120.0(16) . . ? C13 C12 C11 126.5(16) . . ? O4 C13 C12 117.6(14) . . ? O4 C13 C14 125.2(15) . . ? C12 C13 C14 117.2(15) . . ? C13 C14 C15 119.6(17) . . ? C16 C15 C14 122.3(18) . . ? C15 C16 C11 121.7(17) . . ? C25 N3 C26 123.1(7) . . ? C28 N4 C27 128.2(9) . . ? O5 C19 C24 126.7(15) . . ? O5 C19 C20 116.4(12) . . ? C24 C19 C20 116.8(15) . . ? O6 C20 C21 122.4(14) . . ? O6 C20 C19 113.5(13) . . ? C21 C20 C19 123.8(14) . . ? C20 C21 C22 115.4(16) . . ? C20 C21 C25 123.7(14) . . ? C22 C21 C25 120.7(15) . . ? C23 C22 C21 120.4(17) . . ? C22 C23 C24 123.0(16) . . ? C19 C24 C23 120.1(17) . . ? N3 C25 C21 127.4(14) . . ? N3 C26 C36 110.5(8) . . ? N3 C26 C35 110.5(8) . . ? C36 C26 C35 113.7(9) . . ? N3 C26 C27 106.5(6) . . ? C36 C26 C27 107.6(7) . . ? C35 C26 C27 107.6(8) . . ? N4 C27 C26 114.6(5) . . ? N4 C28 C29 127.0(15) . . ? C28 C29 C30 125.5(14) . . ? C28 C29 C34 119.7(15) . . ? C30 C29 C34 114.8(15) . . ? O7 C30 C31 114.1(13) . . ? O7 C30 C29 121.7(13) . . ? C31 C30 C29 124.2(13) . . ? O8 C31 C32 126.6(15) . . ? O8 C31 C30 115.1(12) . . ? C32 C31 C30 118.2(15) . . ? C31 C32 C33 119.6(16) . . ? C34 C33 C32 122.3(15) . . ? C33 C34 C29 120.6(16) . . ? C41 N5 C37 114.1(19) . . ? N5 C37 C38 124(3) . . ? C39 C38 C37 117(3) . . ? C40 C39 C38 120(2) . . ? C39 C40 C41 119.8(18) . . ? N5 C41 C40 124.3(17) . . ? C42 N6 C46 120.0 . . ? N6 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 N6 120.0 . . ? #===END data_4.3py _database_code_CSD 200805 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H57 N9 O8 U Zn2' _chemical_formula_weight 1412.93 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 orthorhombic _symmetry_space_group_name_H-M Pca2~1~ loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 20.1496(19) _cell_length_b 14.6344(15) _cell_length_c 19.2905(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5688.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 33720 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method ? _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 3.741 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.314 _exptl_absorpt_correction_T_max 0.963 _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 33720 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9915 _reflns_number_gt 4595 _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. All non-hydrogen atoms were refined with anisotropic displacement parameters. Some constraints on displacement parameters (ISOR) were applied for several atoms in the Schiff base molecules and for all those of the uncomplexed pyridine molecules. Some constraints on bond lengths were applied for several atoms, in particular the C atoms of the bridges between imine functions and the C atoms of the uncomplexed pyridine molecules. All H atoms were introduced at calculated positions and treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH2) 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^)+(0.0515P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(13) _refine_ls_number_reflns 9915 _refine_ls_number_parameters 736 _refine_ls_number_restraints 273 _refine_ls_R_factor_all 0.1896 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 1.239 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.134 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 0.12809(3) 0.34524(5) 0.16125(5) 0.0503(3) Uani 1 1 d . . . Zn1 Zn 0.00529(12) 0.3988(2) 0.29101(13) 0.0744(9) Uani 1 1 d . . . Zn2 Zn 0.22642(11) 0.30185(16) 0.00509(11) 0.0462(6) Uani 1 1 d . . . O1 O 0.1234(7) 0.1857(9) 0.1823(6) 0.071(5) Uani 1 1 d . . . O2 O 0.0646(7) 0.2983(13) 0.2603(6) 0.065(5) Uani 1 1 d . . . O3 O 0.0731(6) 0.4607(11) 0.2287(7) 0.062(4) Uani 1 1 d . . . O4 O 0.1476(6) 0.5005(9) 0.1284(7) 0.051(4) Uani 1 1 d . . . O5 O 0.0260(6) 0.3342(10) 0.1058(7) 0.059(4) Uani 1 1 d . . . O6 O 0.1347(6) 0.3092(8) 0.0400(7) 0.051(4) Uani 1 1 d . . . O7 O 0.2358(7) 0.3208(9) 0.1084(7) 0.045(4) Uani 1 1 d . . . O8 O 0.2183(7) 0.3525(10) 0.2368(7) 0.056(4) Uani 1 1 d . . . N1 N -0.0067(10) 0.3388(19) 0.3853(10) 0.089(6) Uani 1 1 d U . . N2 N 0.0088(11) 0.5189(17) 0.3522(10) 0.085(7) Uani 1 1 d U . . N3 N 0.2035(9) 0.2006(12) -0.0639(7) 0.052(5) Uani 1 1 d . . . N4 N 0.3139(8) 0.2382(10) 0.0056(8) 0.050(4) Uani 1 1 d . . . C1 C 0.0902(11) 0.1495(19) 0.2384(10) 0.059(5) Uani 1 1 d U . . C2 C 0.0604(10) 0.215(2) 0.2832(12) 0.074(8) Uani 1 1 d D . . C3 C 0.0284(12) 0.191(2) 0.3450(11) 0.077(7) Uani 1 1 d DU . . C4 C 0.0254(13) 0.096(2) 0.3562(15) 0.096(9) Uani 1 1 d U . . H4 H 0.0034 0.0770 0.3959 0.115 Uiso 1 1 calc R . . C5 C 0.0507(13) 0.032(2) 0.3159(14) 0.093(8) Uani 1 1 d U . . H5 H 0.0452 -0.0295 0.3275 0.111 Uiso 1 1 calc R . . C6 C 0.0873(13) 0.057(2) 0.2533(13) 0.082(8) Uani 1 1 d U . . H6 H 0.1073 0.0134 0.2251 0.098 Uiso 1 1 calc R . . C7 C 0.0022(13) 0.253(2) 0.3910(14) 0.088(8) Uani 1 1 d U . . H7 H -0.0113 0.2286 0.4331 0.106 Uiso 1 1 calc R . . C8 C -0.0157(14) 0.4208(19) 0.4411(14) 0.089(9) Uani 1 1 d DU . . C9 C -0.0424(18) 0.511(2) 0.4148(18) 0.086(12) Uani 1 1 d DU . . H9A H -0.0375 0.5602 0.4483 0.103 Uiso 1 1 calc R . . H9B H -0.0881 0.5072 0.3994 0.103 Uiso 1 1 calc R . . C10 C 0.0295(13) 0.600(2) 0.3337(14) 0.087(8) Uani 1 1 d U . . H10 H 0.0185 0.6494 0.3616 0.105 Uiso 1 1 calc R . . C11 C 0.0675(10) 0.6164(16) 0.2740(10) 0.060(6) Uani 1 1 d DU . . C12 C 0.0882(13) 0.5516(19) 0.2249(12) 0.084(8) Uani 1 1 d DU . . C13 C 0.1257(10) 0.5712(16) 0.1718(12) 0.059(6) Uani 1 1 d U . . C14 C 0.1418(8) 0.6581(16) 0.1586(19) 0.064(5) Uani 1 1 d U . . H14 H 0.1661 0.6720 0.1190 0.076 Uiso 1 1 calc R . . C15 C 0.1239(14) 0.724(2) 0.2007(13) 0.114(10) Uani 1 1 d DU . . H15 H 0.1374 0.7833 0.1906 0.136 Uiso 1 1 calc R . . C16 C 0.0860(11) 0.710(2) 0.2591(11) 0.081(8) Uani 1 1 d DU . . H16 H 0.0729 0.7577 0.2876 0.098 Uiso 1 1 calc R . . C17 C -0.071(2) 0.390(3) 0.490(2) 0.138(17) Uani 1 1 d U . . H17A H -0.0897 0.4427 0.5132 0.206 Uiso 1 1 calc R . . H17B H -0.0533 0.3491 0.5244 0.206 Uiso 1 1 calc R . . H17C H -0.1052 0.3597 0.4644 0.206 Uiso 1 1 calc R . . C18 C 0.0494(10) 0.4293(16) 0.4825(10) 0.068(6) Uani 1 1 d U . . H18A H 0.0859 0.4366 0.4510 0.102 Uiso 1 1 calc R . . H18B H 0.0560 0.3751 0.5097 0.102 Uiso 1 1 calc R . . H18C H 0.0469 0.4814 0.5126 0.102 Uiso 1 1 calc R . . C19 C 0.0205(9) 0.2909(14) 0.0430(9) 0.038(4) Uani 1 1 d U . . C20 C 0.0821(10) 0.2770(14) 0.0099(10) 0.048(5) Uani 1 1 d . . . C21 C 0.0801(11) 0.2207(16) -0.0517(11) 0.061(6) Uani 1 1 d . . . C22 C 0.0172(11) 0.1844(16) -0.0757(11) 0.059(6) Uani 1 1 d U . . H22 H 0.0156 0.1424 -0.1118 0.071 Uiso 1 1 calc R . . C23 C -0.0407(14) 0.214(2) -0.0436(14) 0.096(9) Uani 1 1 d U . . H23 H -0.0813 0.1972 -0.0627 0.115 Uiso 1 1 calc R . . C24 C -0.0400(10) 0.2678(14) 0.0171(10) 0.057(6) Uani 1 1 d . . . H24 H -0.0792 0.2866 0.0383 0.068 Uiso 1 1 calc R . . C25 C 0.1398(11) 0.1776(14) -0.0780(10) 0.056(6) Uani 1 1 d . . . H25 H 0.1336 0.1286 -0.1080 0.068 Uiso 1 1 calc R . . C26 C 0.2611(10) 0.1399(15) -0.0791(12) 0.061(6) Uani 1 1 d DU . . C27 C 0.3246(10) 0.1913(15) -0.0627(11) 0.065(6) Uani 1 1 d D . . H27A H 0.3618 0.1493 -0.0598 0.078 Uiso 1 1 calc R . . H27B H 0.3340 0.2358 -0.0987 0.078 Uiso 1 1 calc R . . C28 C 0.3561(11) 0.2355(16) 0.0544(11) 0.065(6) Uani 1 1 d U . . H28 H 0.3972 0.2104 0.0435 0.078 Uiso 1 1 calc R . . C29 C 0.3478(8) 0.2669(14) 0.1250(10) 0.045(5) Uani 1 1 d . . . C30 C 0.2903(9) 0.3062(15) 0.1479(9) 0.050(6) Uani 1 1 d . . . C31 C 0.2790(11) 0.3265(14) 0.2180(10) 0.047(5) Uani 1 1 d . . . C32 C 0.3342(10) 0.3192(13) 0.2604(11) 0.050(6) Uani 1 1 d . . . H32 H 0.3306 0.3368 0.3066 0.060 Uiso 1 1 calc R . . C33 C 0.3928(11) 0.2878(16) 0.2373(11) 0.060(6) Uani 1 1 d U . . H33 H 0.4285 0.2860 0.2678 0.073 Uiso 1 1 calc R . . C34 C 0.4020(10) 0.2583(14) 0.1711(14) 0.072(7) Uani 1 1 d . . . H34 H 0.4422 0.2335 0.1567 0.086 Uiso 1 1 calc R . . C35 C 0.2520(13) 0.0506(18) -0.0327(12) 0.081(8) Uani 1 1 d U . . H35A H 0.2918 0.0147 -0.0344 0.121 Uiso 1 1 calc R . . H35B H 0.2155 0.0152 -0.0502 0.121 Uiso 1 1 calc R . . H35C H 0.2431 0.0681 0.0144 0.121 Uiso 1 1 calc R . . C36 C 0.2598(12) 0.1166(16) -0.1591(10) 0.074(7) Uani 1 1 d . . . H36A H 0.2622 0.1722 -0.1854 0.111 Uiso 1 1 calc R . . H36B H 0.2195 0.0849 -0.1701 0.111 Uiso 1 1 calc R . . H36C H 0.2971 0.0785 -0.1703 0.111 Uiso 1 1 calc R . . N5 N -0.0820(8) 0.4073(12) 0.2397(8) 0.048(4) Uani 1 1 d . . . C37 C -0.1377(9) 0.3722(16) 0.2616(10) 0.065(7) Uani 1 1 d . . . H37 H -0.1356 0.3360 0.3012 0.077 Uiso 1 1 calc R . . C38 C -0.1988(11) 0.3834(16) 0.2321(11) 0.070(7) Uani 1 1 d . . . H38 H -0.2363 0.3548 0.2500 0.084 Uiso 1 1 calc R . . C39 C -0.2024(11) 0.4414(16) 0.1725(11) 0.067(7) Uani 1 1 d . . . H39 H -0.2426 0.4526 0.1504 0.081 Uiso 1 1 calc R . . C40 C -0.1443(9) 0.4799(14) 0.1488(10) 0.049(6) Uani 1 1 d . . . H40 H -0.1453 0.5200 0.1114 0.059 Uiso 1 1 calc R . . C41 C -0.0847(10) 0.4594(14) 0.1804(11) 0.060(7) Uani 1 1 d . . . H41 H -0.0455 0.4812 0.1611 0.072 Uiso 1 1 calc R . . N6 N 0.2479(7) 0.4250(11) -0.0434(7) 0.031(4) Uani 1 1 d . . . C42 C 0.2455(10) 0.5013(19) -0.0085(10) 0.057(7) Uani 1 1 d . . . H42 H 0.2260 0.5013 0.0352 0.068 Uiso 1 1 calc R . . C43 C 0.2703(12) 0.5801(15) -0.0336(12) 0.069(7) Uani 1 1 d . . . H43 H 0.2695 0.6317 -0.0055 0.082 Uiso 1 1 calc R . . C44 C 0.2968(11) 0.5875(15) -0.0993(11) 0.061(6) Uani 1 1 d . . . H44 H 0.3122 0.6427 -0.1170 0.073 Uiso 1 1 calc R . . C45 C 0.2990(12) 0.5065(15) -0.1374(11) 0.063(7) Uani 1 1 d . . . H45 H 0.3167 0.5050 -0.1819 0.075 Uiso 1 1 calc R . . C46 C 0.2741(9) 0.4289(15) -0.1067(11) 0.048(6) Uani 1 1 d . . . H46 H 0.2757 0.3749 -0.1321 0.057 Uiso 1 1 calc R . . N7 N 0.0111(9) -0.1209(13) 0.0494(9) 0.065(5) Uani 1 1 d U . . C47 C -0.0054(12) -0.0347(18) 0.0468(11) 0.069(6) Uani 1 1 d U . . H47 H -0.0491 -0.0221 0.0345 0.083 Uiso 1 1 calc R . . C48 C 0.0343(12) 0.040(2) 0.0601(12) 0.079(7) Uani 1 1 d U . . H48 H 0.0175 0.0989 0.0576 0.095 Uiso 1 1 calc R . . C49 C 0.1005(14) 0.0241(19) 0.0774(14) 0.085(9) Uani 1 1 d DU . . H49 H 0.1302 0.0720 0.0842 0.102 Uiso 1 1 calc R . . C50 C 0.1198(17) -0.0661(19) 0.0840(17) 0.124(11) Uani 1 1 d DU . . H50 H 0.1620 -0.0836 0.0982 0.149 Uiso 1 1 calc R . . C51 C 0.0699(14) -0.1287(19) 0.0674(14) 0.094(9) Uani 1 1 d U . . H51 H 0.0838 -0.1892 0.0705 0.112 Uiso 1 1 calc R . . N8 N 0.2216(15) 0.822(2) -0.0411(14) 0.111(9) Uani 1 1 d U . . C52 C 0.2778(12) 0.8172(17) -0.0719(13) 0.075(7) Uani 1 1 d U . . H52 H 0.3147 0.8000 -0.0460 0.090 Uiso 1 1 calc R . . C53 C 0.2866(18) 0.836(2) -0.1400(19) 0.126(14) Uani 1 1 d DU . . H53 H 0.3287 0.8362 -0.1598 0.151 Uiso 1 1 calc R . . C54 C 0.2307(16) 0.855(2) -0.1792(17) 0.129(11) Uani 1 1 d DU . . H54 H 0.2356 0.8716 -0.2254 0.155 Uiso 1 1 calc R . . C55 C 0.1679(15) 0.849(2) -0.1513(14) 0.104(9) Uani 1 1 d U . . H55 H 0.1299 0.8533 -0.1784 0.125 Uiso 1 1 calc R . . C56 C 0.1651(14) 0.8365(19) -0.0818(14) 0.092(8) Uani 1 1 d U . . H56 H 0.1238 0.8379 -0.0601 0.111 Uiso 1 1 calc R . . N9 N -0.2184(14) 0.085(2) 0.1355(13) 0.137(10) Uani 1 1 d U . . C57 C -0.1706(14) 0.146(3) 0.1373(14) 0.125(12) Uani 1 1 d DU . . H57 H -0.1807 0.2035 0.1201 0.150 Uiso 1 1 calc R . . C58 C -0.1066(12) 0.134(2) 0.162(2) 0.110(8) Uani 1 1 d DU . . H58 H -0.0752 0.1802 0.1603 0.132 Uiso 1 1 calc R . . C59 C -0.0919(17) 0.047(3) 0.1895(15) 0.129(12) Uani 1 1 d U . . H59 H -0.0502 0.0345 0.2077 0.155 Uiso 1 1 calc R . . C60 C -0.1423(14) -0.021(2) 0.1890(13) 0.100(10) Uani 1 1 d U . . H60 H -0.1329 -0.0798 0.2047 0.119 Uiso 1 1 calc R . . C61 C -0.2053(15) 0.000(2) 0.165(2) 0.125(10) Uani 1 1 d U . . H61 H -0.2393 -0.0426 0.1691 0.150 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U 0.0414(3) 0.0626(5) 0.0468(3) 0.0067(6) 0.0021(6) -0.0058(4) Zn1 0.0420(15) 0.130(3) 0.0512(15) 0.0088(16) 0.0077(11) 0.0025(16) Zn2 0.0528(14) 0.0400(16) 0.0459(12) -0.0006(11) 0.0048(10) -0.0030(12) O1 0.093(10) 0.057(11) 0.063(12) 0.037(7) 0.009(7) -0.025(9) O2 0.046(9) 0.108(15) 0.040(8) 0.015(8) 0.010(6) -0.004(9) O3 0.025(7) 0.064(12) 0.096(10) 0.018(9) 0.008(6) 0.013(7) O4 0.057(9) 0.043(11) 0.052(8) 0.008(6) -0.008(6) -0.015(7) O5 0.031(7) 0.048(10) 0.100(10) 0.031(8) 0.013(7) -0.016(7) O6 0.027(7) 0.036(9) 0.088(10) -0.004(6) -0.006(6) -0.011(6) O7 0.063(10) 0.023(10) 0.049(8) 0.015(6) 0.002(7) 0.008(8) O8 0.039(8) 0.064(12) 0.063(9) 0.007(8) -0.007(6) -0.007(8) N1 0.089(9) 0.095(10) 0.083(9) 0.006(8) -0.001(7) 0.005(9) N2 0.093(10) 0.097(11) 0.064(9) -0.018(8) 0.007(8) -0.007(8) N3 0.079(13) 0.041(12) 0.036(10) 0.006(8) 0.003(8) -0.023(10) N4 0.081(12) 0.025(11) 0.045(9) 0.000(8) 0.019(9) -0.001(9) C1 0.068(9) 0.055(10) 0.054(8) 0.009(8) 0.004(7) -0.016(8) C2 0.044(14) 0.08(2) 0.099(19) 0.036(18) 0.003(12) 0.000(14) C3 0.074(10) 0.079(11) 0.077(10) 0.009(8) 0.002(8) 0.001(9) C4 0.089(11) 0.105(12) 0.093(11) 0.003(9) -0.007(9) -0.011(9) C5 0.099(11) 0.087(12) 0.092(11) 0.016(9) -0.009(9) -0.007(9) C6 0.081(11) 0.082(12) 0.082(10) -0.001(9) 0.007(8) 0.000(9) C7 0.080(11) 0.096(12) 0.089(11) 0.006(9) 0.021(8) -0.009(9) C8 0.084(11) 0.093(12) 0.089(11) -0.003(9) -0.003(8) 0.006(9) C9 0.084(14) 0.080(15) 0.095(14) -0.001(9) -0.007(9) 0.003(9) C10 0.080(11) 0.091(12) 0.091(11) 0.004(9) -0.008(8) 0.000(9) C11 0.058(9) 0.068(10) 0.054(9) -0.009(8) 0.004(7) 0.007(8) C12 0.075(11) 0.091(12) 0.087(11) -0.008(9) -0.002(8) -0.004(9) C13 0.056(8) 0.069(10) 0.053(9) -0.009(8) -0.005(8) 0.006(8) C14 0.065(9) 0.062(9) 0.064(8) -0.001(9) 0.008(9) -0.001(8) C15 0.114(12) 0.109(13) 0.118(12) 0.010(9) 0.000(9) 0.001(9) C16 0.079(10) 0.084(11) 0.081(10) -0.007(9) -0.006(8) 0.011(9) C17 0.138(18) 0.138(18) 0.137(18) 0.000(5) 0.002(5) 0.000(5) C18 0.077(10) 0.068(10) 0.060(9) -0.008(8) -0.016(8) 0.000(8) C19 0.029(8) 0.047(9) 0.038(7) 0.002(7) -0.005(6) -0.011(7) C20 0.057(14) 0.042(15) 0.045(12) 0.023(11) 0.019(10) -0.007(11) C21 0.059(15) 0.056(18) 0.069(15) 0.026(12) 0.002(11) -0.023(13) C22 0.063(9) 0.052(10) 0.062(9) 0.005(7) -0.016(7) -0.006(8) C23 0.094(11) 0.093(12) 0.100(11) 0.008(9) -0.010(9) -0.011(9) C24 0.054(14) 0.057(17) 0.059(13) 0.011(11) -0.011(10) 0.007(11) C25 0.084(17) 0.041(17) 0.044(12) -0.012(9) -0.003(10) -0.009(12) C26 0.069(10) 0.055(10) 0.058(9) -0.003(8) -0.009(8) 0.006(8) C27 0.084(17) 0.027(15) 0.083(17) 0.014(12) 0.022(12) -0.017(12) C28 0.059(10) 0.066(10) 0.069(9) -0.005(8) 0.003(8) -0.010(8) C29 0.015(9) 0.041(15) 0.080(14) 0.010(11) 0.004(9) 0.008(9) C30 0.055(12) 0.058(15) 0.037(15) 0.007(10) 0.000(9) 0.006(10) C31 0.045(13) 0.042(16) 0.053(12) 0.003(10) -0.017(10) -0.009(11) C32 0.054(13) 0.034(16) 0.063(13) 0.013(9) -0.008(10) 0.000(10) C33 0.056(9) 0.057(10) 0.068(9) 0.005(8) -0.004(7) 0.001(8) C34 0.060(13) 0.058(16) 0.099(18) -0.030(16) -0.037(15) 0.012(11) C35 0.091(11) 0.068(11) 0.083(10) -0.003(8) -0.011(8) 0.003(9) C36 0.10(2) 0.062(19) 0.058(15) 0.001(12) 0.006(12) 0.010(15) N5 0.045(10) 0.050(13) 0.051(10) 0.003(9) 0.006(7) 0.002(9) C37 0.035(13) 0.11(2) 0.047(12) 0.022(11) 0.004(8) -0.003(12) C38 0.060(16) 0.08(2) 0.068(16) 0.012(12) 0.013(11) -0.016(13) C39 0.078(15) 0.088(19) 0.036(14) -0.002(12) -0.013(10) 0.021(13) C40 0.059(14) 0.049(14) 0.040(15) 0.017(9) -0.009(8) 0.005(10) C41 0.068(15) 0.020(13) 0.09(2) 0.007(11) 0.015(11) -0.003(11) N6 0.033(9) 0.021(11) 0.039(10) 0.001(7) -0.009(7) -0.007(7) C42 0.049(13) 0.10(2) 0.026(11) -0.006(11) 0.016(9) -0.013(13) C43 0.10(2) 0.022(15) 0.083(17) -0.011(12) 0.009(14) -0.029(14) C44 0.100(18) 0.021(15) 0.062(14) 0.003(11) 0.021(12) 0.008(12) C45 0.11(2) 0.034(17) 0.048(13) 0.018(11) 0.038(12) -0.018(13) C46 0.041(12) 0.043(16) 0.060(13) -0.015(11) -0.003(9) 0.008(11) N7 0.059(8) 0.058(9) 0.077(8) 0.000(7) -0.015(7) -0.005(7) C47 0.070(10) 0.067(10) 0.072(9) -0.003(8) -0.006(8) 0.005(9) C48 0.079(10) 0.080(11) 0.077(10) 0.005(8) -0.004(8) -0.009(9) C49 0.087(12) 0.078(12) 0.089(11) 0.003(9) 0.000(8) 0.000(9) C50 0.116(13) 0.123(14) 0.135(13) 0.002(9) -0.002(9) -0.004(10) C51 0.096(11) 0.083(12) 0.101(11) -0.002(9) -0.018(9) 0.003(9) N8 0.110(12) 0.105(13) 0.119(12) 0.006(9) -0.003(9) 0.006(9) C52 0.071(10) 0.068(11) 0.086(10) 0.003(8) -0.004(8) 0.010(8) C53 0.127(16) 0.120(16) 0.130(16) -0.001(9) 0.000(9) 0.008(10) C54 0.137(14) 0.125(14) 0.127(13) -0.003(9) -0.006(9) -0.006(10) C55 0.107(11) 0.107(12) 0.097(11) -0.004(9) -0.008(9) -0.008(9) C56 0.099(11) 0.087(12) 0.091(11) 0.002(9) -0.013(9) -0.006(9) N9 0.142(13) 0.136(13) 0.133(13) 0.006(9) 0.003(9) 0.003(9) C57 0.124(14) 0.130(14) 0.121(14) 0.006(9) 0.002(9) 0.006(10) C58 0.118(11) 0.117(12) 0.095(10) 0.003(10) 0.007(10) 0.006(9) C59 0.132(14) 0.134(15) 0.121(14) -0.002(9) -0.003(9) 0.013(10) C60 0.104(12) 0.095(13) 0.101(13) -0.008(9) 0.003(8) 0.016(9) C61 0.130(13) 0.124(13) 0.121(12) -0.008(10) -0.005(10) 0.004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U O5 2.324(13) . ? U O8 2.332(13) . ? U O1 2.372(13) . ? U O4 2.392(13) . ? U O2 2.400(12) . ? U O3 2.404(15) . ? U O6 2.402(13) . ? U O7 2.425(14) . ? U Zn1 3.606(3) . ? U Zn2 3.661(2) . ? Zn1 O2 1.985(17) . ? Zn1 N5 2.023(16) . ? Zn1 O3 2.032(14) . ? Zn1 N1 2.03(2) . ? Zn1 N2 2.12(2) . ? Zn2 O6 1.970(12) . ? Zn2 N4 1.994(16) . ? Zn2 O7 2.021(13) . ? Zn2 N3 2.044(17) . ? Zn2 N6 2.077(15) . ? O1 C1 1.38(2) . ? O2 C2 1.29(3) . ? O2 O3 2.46(2) . ? O2 N1 2.87(2) . ? O3 C12 1.37(3) . ? O3 N2 2.84(2) . ? O4 C13 1.40(2) . ? O5 C19 1.37(2) . ? O6 C20 1.30(2) . ? O6 O7 2.435(18) . ? O6 N3 2.91(2) . ? O7 C30 1.35(2) . ? O7 N4 2.80(2) . ? O8 C31 1.33(2) . ? N1 C7 1.27(3) . ? N1 C8 1.62(3) . ? N1 N2 2.73(4) . ? N2 C10 1.31(3) . ? N2 C9 1.59(4) . ? N3 C25 1.36(2) . ? N3 C26 1.49(3) . ? N3 N4 2.66(2) . ? N4 C28 1.27(2) . ? N4 C27 1.50(2) . ? C1 C6 1.39(3) . ? C1 C2 1.43(3) . ? C2 C3 1.40(3) . ? C3 C7 1.37(3) . ? C3 C4 1.41(3) . ? C4 C5 1.33(4) . ? C5 C6 1.46(3) . ? C8 C9 1.51(4) . ? C8 C17 1.53(5) . ? C8 C18 1.54(3) . ? C10 C11 1.40(3) . ? C11 C12 1.40(3) . ? C11 C16 1.44(3) . ? C12 C13 1.31(3) . ? C13 C14 1.34(3) . ? C14 C15 1.31(4) . ? C15 C16 1.38(3) . ? C19 C24 1.36(2) . ? C19 C20 1.41(2) . ? C20 C21 1.45(3) . ? C21 C25 1.45(3) . ? C21 C22 1.45(3) . ? C22 C23 1.39(3) . ? C23 C24 1.41(3) . ? C26 C27 1.52(3) . ? C26 C36 1.58(3) . ? C26 C35 1.59(3) . ? C28 C29 1.45(3) . ? C29 C30 1.37(2) . ? C29 C34 1.41(3) . ? C30 C31 1.40(3) . ? C31 C32 1.39(3) . ? C32 C33 1.34(3) . ? C33 C34 1.36(3) . ? N5 C37 1.31(2) . ? N5 C41 1.38(2) . ? C37 C38 1.36(3) . ? C38 C39 1.43(3) . ? C39 C40 1.38(3) . ? C40 C41 1.38(2) . ? N6 C42 1.31(3) . ? N6 C46 1.33(2) . ? C42 C43 1.35(3) . ? C43 C44 1.38(3) . ? C44 C45 1.39(3) . ? C45 C46 1.38(3) . ? N7 C51 1.24(3) . ? N7 C47 1.31(3) . ? C47 C48 1.38(3) . ? C48 C49 1.39(3) . ? C49 C50 1.38(4) . ? C50 C51 1.40(3) . ? N8 C52 1.28(3) . ? N8 C56 1.40(3) . ? C52 C53 1.35(4) . ? C53 C54 1.38(5) . ? C54 C55 1.38(4) . ? C55 C56 1.35(3) . ? N9 C57 1.31(3) . ? N9 C61 1.40(3) . ? C57 C58 1.39(4) . ? C58 C59 1.41(4) . ? C59 C60 1.42(4) . ? C60 C61 1.39(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 U O8 168.7(5) . . ? O5 U O1 88.6(5) . . ? O8 U O1 88.2(5) . . ? O5 U O4 95.1(4) . . ? O8 U O4 89.7(5) . . ? O1 U O4 170.8(5) . . ? O5 U O2 82.8(5) . . ? O8 U O2 86.0(5) . . ? O1 U O2 63.9(5) . . ? O4 U O2 124.8(5) . . ? O5 U O3 83.7(5) . . ? O8 U O3 89.4(5) . . ? O1 U O3 125.5(5) . . ? O4 U O3 63.4(5) . . ? O2 U O3 61.6(6) . . ? O5 U O6 65.5(5) . . ? O8 U O6 125.2(4) . . ? O1 U O6 87.3(4) . . ? O4 U O6 86.6(4) . . ? O2 U O6 137.9(5) . . ? O3 U O6 135.0(4) . . ? O5 U O7 126.1(5) . . ? O8 U O7 64.6(5) . . ? O1 U O7 87.9(5) . . ? O4 U O7 83.2(4) . . ? O2 U O7 140.3(5) . . ? O3 U O7 138.1(5) . . ? O6 U O7 60.6(4) . . ? Zn1 U Zn2 168.59(6) . . ? O2 Zn1 N5 115.0(6) . . ? O2 Zn1 O3 75.5(6) . . ? N5 Zn1 O3 105.5(6) . . ? O2 Zn1 N1 91.1(8) . . ? N5 Zn1 N1 111.1(7) . . ? O3 Zn1 N1 143.2(7) . . ? O2 Zn1 N2 139.6(8) . . ? N5 Zn1 N2 104.5(8) . . ? O3 Zn1 N2 86.4(8) . . ? N1 Zn1 N2 82.2(10) . . ? O6 Zn2 N4 148.6(6) . . ? O6 Zn2 O7 75.2(5) . . ? N4 Zn2 O7 88.6(6) . . ? O6 Zn2 N3 92.9(6) . . ? N4 Zn2 N3 82.2(7) . . ? O7 Zn2 N3 139.7(6) . . ? O6 Zn2 N6 107.6(6) . . ? N4 Zn2 N6 102.9(6) . . ? O7 Zn2 N6 107.8(6) . . ? N3 Zn2 N6 112.5(6) . . ? C7 N1 C8 133(2) . . ? C10 N2 C9 119(2) . . ? C25 N3 C26 123.3(17) . . ? C28 N4 C27 122.7(18) . . ? O1 C1 C6 124(2) . . ? O1 C1 C2 115(2) . . ? C6 C1 C2 121(2) . . ? O2 C2 C3 124(3) . . ? O2 C2 C1 113.5(19) . . ? C3 C2 C1 123(2) . . ? C7 C3 C2 124(3) . . ? C7 C3 C4 122(3) . . ? C2 C3 C4 113(3) . . ? C5 C4 C3 127(3) . . ? C4 C5 C6 120(3) . . ? C1 C6 C5 116(3) . . ? N1 C7 C3 130(3) . . ? C9 C8 C17 102(3) . . ? C9 C8 C18 114(3) . . ? C17 C8 C18 109(3) . . ? C9 C8 N1 118(2) . . ? C17 C8 N1 106(3) . . ? C18 C8 N1 108.0(19) . . ? C8 C9 N2 95(2) . . ? N2 C10 C11 124(3) . . ? C12 C11 C10 127(3) . . ? C12 C11 C16 115(2) . . ? C10 C11 C16 118(2) . . ? C13 C12 O3 112.6(19) . . ? C13 C12 C11 124(3) . . ? O3 C12 C11 124(2) . . ? C12 C13 C14 120(3) . . ? C12 C13 O4 119(2) . . ? C14 C13 O4 121(2) . . ? C15 C14 C13 121(3) . . ? C14 C15 C16 123(3) . . ? C15 C16 C11 117(3) . . ? C24 C19 O5 120.7(17) . . ? C24 C19 C20 126(2) . . ? O5 C19 C20 113.3(16) . . ? O6 C20 C19 117.6(19) . . ? O6 C20 C21 126.7(17) . . ? C19 C20 C21 115.4(19) . . ? C25 C21 C20 120.8(18) . . ? C25 C21 C22 117(2) . . ? C20 C21 C22 120(2) . . ? C23 C22 C21 119(2) . . ? C22 C23 C24 122(2) . . ? C19 C24 C23 117(2) . . ? N3 C25 C21 127.4(19) . . ? N3 C26 C27 108.6(18) . . ? N3 C26 C36 108.0(15) . . ? C27 C26 C36 108.8(19) . . ? N3 C26 C35 106.8(19) . . ? C27 C26 C35 112.8(17) . . ? C36 C26 C35 111.7(19) . . ? N4 C27 C26 106.7(16) . . ? N4 C28 C29 128(2) . . ? C30 C29 C34 119(2) . . ? C30 C29 C28 122.3(18) . . ? C34 C29 C28 118.3(18) . . ? O7 C30 C29 125.0(18) . . ? O7 C30 C31 112.1(18) . . ? C29 C30 C31 122.5(18) . . ? O8 C31 C32 126.8(19) . . ? O8 C31 C30 118.2(16) . . ? C32 C31 C30 115(2) . . ? C33 C32 C31 122(2) . . ? C32 C33 C34 123(2) . . ? C33 C34 C29 117(2) . . ? C37 N5 C41 117.0(18) . . ? N5 C37 C38 126(2) . . ? C37 C38 C39 117(2) . . ? C40 C39 C38 118(2) . . ? C39 C40 C41 120(2) . . ? N5 C41 C40 121.4(19) . . ? C42 N6 C46 116.9(18) . . ? N6 C42 C43 122.1(18) . . ? C42 C43 C44 123(2) . . ? C43 C44 C45 115(2) . . ? C46 C45 C44 118(2) . . ? N6 C46 C45 125(2) . . ? C51 N7 C47 110(2) . . ? N7 C47 C48 128(2) . . ? C47 C48 C49 118(3) . . ? C50 C49 C48 117(3) . . ? C49 C50 C51 114(3) . . ? N7 C51 C50 134(3) . . ? C52 N8 C56 118(3) . . ? N8 C52 C53 124(3) . . ? C52 C53 C54 118(3) . . ? C55 C54 C53 121(3) . . ? C56 C55 C54 116(3) . . ? C55 C56 N8 123(3) . . ? C57 N9 C61 117(3) . . ? N9 C57 C58 128(3) . . ? C57 C58 C59 116(3) . . ? C58 C59 C60 119(3) . . ? C61 C60 C59 120(3) . . ? C60 C61 N9 121(3) . . ?