Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Chen Jie-Sheng' 'Jiang yu-Sheng' 'Li Guanghua' 'Xu Jin-Jie' 'Yu Zhen-Tao' _publ_contact_author_name 'Professor Jie-Sheng Chen' _publ_contact_author_address ; College of Chemistry Jilin University State Key Laboratory of Inorganic S Changchun 130023 CHINA ; _publ_contact_author_phone 86-431-5671974 _publ_contact_author_fax 86-431-5671974 _publ_contact_author_email chemcj@mail.jlu.edu.cn _publ_requested_coeditor_name ? _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A Uranium-Zinc-Organic Molecular Compound Containing Planar Tetranuclear Uranyl Units ; data_sad _database_code_CSD 213349 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H26 N6 O13 U2 Zn' _chemical_formula_sum 'C39 H26 N6 O13 U2 Zn' _chemical_formula_weight 1328.09 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 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 12.9751(6) _cell_length_b 20.3412(8) _cell_length_c 14.6543(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.2870(10) _cell_angle_gamma 90.00 _cell_volume 3864.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Yellow Green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 9.053 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1819 _exptl_absorpt_correction_T_max 0.4062 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 18371 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 23.29 _reflns_number_total 5563 _reflns_number_gt 4709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; 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^)+(0.0367P)^2^+0.0000P] 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 5563 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.422433(16) 0.437808(9) -0.443862(13) 0.02479(8) Uani 1 1 d . . . U2 U 0.720209(17) 0.410337(10) -0.429590(15) 0.03173(8) Uani 1 1 d . . . Zn1 Zn 0.25058(5) 0.36220(3) -0.09851(4) 0.03107(16) Uani 1 1 d . . . O1 O 0.3386(3) 0.34858(18) -0.3660(2) 0.0320(9) Uani 1 1 d . . . O2 O 0.2446(3) 0.36139(18) -0.2438(3) 0.0343(9) Uani 1 1 d . . . O3 O 0.5557(3) 0.36064(19) -0.3768(3) 0.0378(10) Uani 1 1 d . . . O4 O 0.5489(4) 0.2514(2) -0.3965(3) 0.0443(11) Uani 1 1 d . . . O5 O 0.7553(4) 0.3086(2) -0.3367(3) 0.0580(13) Uani 1 1 d . . . O6 O 0.8897(3) 0.3595(2) -0.3855(3) 0.0540(13) Uani 1 1 d . . . O7 O 0.2463(4) 0.4733(3) -0.4536(4) 0.0789(17) Uani 1 1 d . . . O8 O 0.1316(4) 0.5436(3) -0.4922(4) 0.0704(15) Uani 1 1 d . . . O9 O 0.5843(3) 0.46688(17) -0.4767(3) 0.0319(9) Uani 1 1 d . . . O10 O 0.4345(3) 0.48059(19) -0.3380(2) 0.0399(10) Uani 1 1 d . . . O11 O 0.4027(3) 0.38964(19) -0.5440(3) 0.0362(10) Uani 1 1 d . . . O12 O 0.7369(4) 0.4600(2) -0.3314(3) 0.0557(12) Uani 1 1 d . . . O13 O 0.7108(3) 0.3601(2) -0.5274(3) 0.0459(11) Uani 1 1 d . . . N1 N 0.3867(4) 0.3079(2) -0.1340(3) 0.0295(11) Uani 1 1 d . . . N2 N 1.0870(6) 0.2106(4) -0.2925(5) 0.081(2) Uani 1 1 d . . . N3 N 0.0928(4) 0.4013(2) -0.0992(3) 0.0390(12) Uani 1 1 d . . . N4 N 0.1610(4) 0.2770(2) -0.0730(3) 0.0373(12) Uani 1 1 d . . . N5 N 0.3035(4) 0.3795(2) 0.0434(3) 0.0372(12) Uani 1 1 d . . . N6 N 0.3093(4) 0.4614(2) -0.1013(3) 0.0308(11) Uani 1 1 d . . . C1 C 0.4105(4) 0.3153(2) -0.2224(3) 0.0243(12) Uani 1 1 d . . . C2 C 0.5024(4) 0.2927(2) -0.2549(3) 0.0272(12) Uani 1 1 d . . . C3 C 0.5688(5) 0.2574(3) -0.1956(4) 0.0347(14) Uani 1 1 d . . . H3 H 0.6301 0.2404 -0.2162 0.080 Uiso 1 1 calc . . . C4 C 0.5428(5) 0.2479(3) -0.1067(4) 0.0384(15) Uani 1 1 d . . . H4 H 0.5854 0.2239 -0.0665 0.080 Uiso 1 1 calc . . . C5 C 0.4518(5) 0.2748(3) -0.0783(4) 0.0376(15) Uani 1 1 d . . . H5 H 0.4352 0.2697 -0.0176 0.080 Uiso 1 1 calc . . . C6 C 0.3250(4) 0.3448(2) -0.2815(4) 0.0269(13) Uani 1 1 d . . . C7 C 0.5360(4) 0.3002(3) -0.3520(4) 0.0300(13) Uani 1 1 d . . . C8 C 1.0233(6) 0.2616(3) -0.3142(5) 0.0517(18) Uani 1 1 d . . . H8 H 1.0516 0.3030 -0.3230 0.080 Uiso 1 1 calc . . . C9 C 0.9175(5) 0.2539(3) -0.3235(4) 0.0439(16) Uani 1 1 d . . . C10 C 0.8782(7) 0.1927(4) -0.3100(6) 0.071(2) Uani 1 1 d . . . H10 H 0.8071 0.1867 -0.3144 0.080 Uiso 1 1 calc . . . C11 C 0.9400(9) 0.1399(4) -0.2901(7) 0.088(3) Uani 1 1 d . . . H11 H 0.9129 0.0979 -0.2830 0.080 Uiso 1 1 calc . . . C12 C 1.0418(9) 0.1515(5) -0.2813(7) 0.090(3) Uani 1 1 d . . . H12 H 1.0845 0.1161 -0.2664 0.080 Uiso 1 1 calc . . . C13 C 0.8500(5) 0.3102(3) -0.3490(4) 0.0421(16) Uani 1 1 d . . . C14 C 0.0916(6) 0.4696(4) -0.3755(5) 0.059(2) Uani 1 1 d . . . H14A H 0.0287 0.4945 -0.3762 0.080 Uiso 1 1 calc . . . H14B H 0.1246 0.4719 -0.3158 0.080 Uiso 1 1 calc . . . H14C H 0.0762 0.4246 -0.3903 0.080 Uiso 1 1 calc . . . C15 C 0.1608(5) 0.4968(3) -0.4432(4) 0.0349(14) Uani 1 1 d . . . C16 C 0.0598(6) 0.4618(3) -0.1134(5) 0.0568(19) Uani 1 1 d . . . H16 H 0.1082 0.4953 -0.1166 0.080 Uiso 1 1 calc . . . C17 C -0.0453(7) 0.4781(4) -0.1238(7) 0.079(3) Uani 1 1 d . . . H17 H -0.0657 0.5213 -0.1342 0.080 Uiso 1 1 calc . . . C18 C -0.1150(6) 0.4305(4) -0.1186(6) 0.069(2) Uani 1 1 d . . . H18 H -0.1847 0.4408 -0.1260 0.080 Uiso 1 1 calc . . . C19 C -0.0857(5) 0.3655(3) -0.1023(5) 0.0500(17) Uani 1 1 d . . . C20 C 0.0202(5) 0.3532(3) -0.0930(4) 0.0359(14) Uani 1 1 d . . . C21 C 0.0576(5) 0.2868(3) -0.0776(4) 0.0368(14) Uani 1 1 d . . . C22 C -0.0139(5) 0.2358(3) -0.0699(4) 0.0465(17) Uani 1 1 d . . . C23 C 0.0260(7) 0.1728(4) -0.0551(5) 0.062(2) Uani 1 1 d . . . H23 H -0.0185 0.1374 -0.0492 0.080 Uiso 1 1 calc . . . C24 C 0.1300(7) 0.1630(3) -0.0491(5) 0.064(2) Uani 1 1 d . . . H24 H 0.1570 0.1213 -0.0380 0.080 Uiso 1 1 calc . . . C25 C 0.1952(5) 0.2167(3) -0.0598(4) 0.0477(17) Uani 1 1 d . . . H25 H 0.2661 0.2095 -0.0575 0.080 Uiso 1 1 calc . . . C26 C -0.1556(5) 0.3118(4) -0.0940(5) 0.064(2) Uani 1 1 d . . . H26 H -0.2262 0.3195 -0.0998 0.080 Uiso 1 1 calc . . . C27 C -0.1214(6) 0.2507(4) -0.0780(5) 0.063(2) Uani 1 1 d . . . H27 H -0.1690 0.2170 -0.0720 0.080 Uiso 1 1 calc . . . C28 C 0.3029(6) 0.3391(3) 0.1131(4) 0.0515(18) Uani 1 1 d . . . H28 H 0.2787 0.2965 0.1035 0.080 Uiso 1 1 calc . . . C29 C 0.3373(6) 0.3574(4) 0.2019(4) 0.057(2) Uani 1 1 d . . . H29 H 0.3364 0.3270 0.2493 0.080 Uiso 1 1 calc . . . C30 C 0.3722(6) 0.4200(4) 0.2183(4) 0.0530(19) Uani 1 1 d . . . H30 H 0.3940 0.4329 0.2768 0.080 Uiso 1 1 calc . . . C31 C 0.3743(5) 0.4640(3) 0.1453(4) 0.0394(15) Uani 1 1 d . . . C32 C 0.3393(4) 0.4416(3) 0.0584(4) 0.0323(14) Uani 1 1 d . . . C33 C 0.3422(4) 0.4852(3) -0.0190(4) 0.0315(13) Uani 1 1 d . . . C34 C 0.3773(5) 0.5501(3) -0.0067(5) 0.0414(16) Uani 1 1 d . . . C35 C 0.3790(6) 0.5910(3) -0.0852(5) 0.0494(18) Uani 1 1 d . . . H35 H 0.4018 0.6343 -0.0802 0.080 Uiso 1 1 calc . . . C36 C 0.3472(6) 0.5666(3) -0.1667(5) 0.0476(17) Uani 1 1 d . . . H36 H 0.3489 0.5929 -0.2186 0.080 Uiso 1 1 calc . . . C37 C 0.3115(5) 0.5014(3) -0.1737(4) 0.0370(15) Uani 1 1 d . . . H37 H 0.2886 0.4856 -0.2305 0.080 Uiso 1 1 calc . . . C38 C 0.4104(5) 0.5302(4) 0.1553(5) 0.0508(18) Uani 1 1 d . . . H38 H 0.4333 0.5451 0.2126 0.080 Uiso 1 1 calc . . . C39 C 0.4116(5) 0.5715(3) 0.0828(5) 0.0493(18) Uani 1 1 d . . . H39 H 0.4351 0.6144 0.0911 0.080 Uiso 1 1 calc . . . 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 0.02466(13) 0.02466(12) 0.02505(12) 0.00343(8) 0.00114(9) 0.00300(8) U2 0.02500(14) 0.03365(14) 0.03635(14) 0.00130(9) -0.00095(10) 0.00666(9) Zn1 0.0295(4) 0.0292(4) 0.0347(4) 0.0001(3) 0.0034(3) -0.0030(3) O1 0.029(2) 0.038(2) 0.028(2) 0.0074(17) -0.0004(17) -0.0003(17) O2 0.029(2) 0.041(2) 0.033(2) 0.0029(17) 0.0017(19) 0.0032(18) O3 0.028(2) 0.039(2) 0.046(2) 0.0204(19) 0.0043(19) 0.0057(18) O4 0.061(3) 0.042(3) 0.031(2) -0.007(2) 0.004(2) 0.005(2) O5 0.031(3) 0.066(3) 0.076(3) 0.030(3) 0.003(2) 0.010(2) O6 0.031(3) 0.053(3) 0.077(3) 0.027(3) 0.001(2) 0.007(2) O7 0.028(3) 0.069(4) 0.140(5) -0.004(3) 0.008(3) 0.011(3) O8 0.064(4) 0.068(3) 0.079(4) 0.040(3) 0.000(3) -0.005(3) O9 0.025(2) 0.030(2) 0.042(2) 0.0116(17) 0.0061(18) 0.0044(17) O10 0.044(3) 0.045(2) 0.031(2) -0.0068(18) 0.0070(19) -0.001(2) O11 0.042(3) 0.034(2) 0.033(2) -0.0006(17) 0.0019(19) 0.0000(19) O12 0.052(3) 0.062(3) 0.052(3) -0.016(2) -0.009(2) 0.013(2) O13 0.041(3) 0.044(3) 0.053(3) -0.008(2) 0.004(2) 0.007(2) N1 0.031(3) 0.031(3) 0.027(2) 0.000(2) 0.003(2) -0.004(2) N2 0.066(5) 0.089(6) 0.087(5) -0.005(4) -0.009(4) 0.035(4) N3 0.030(3) 0.038(3) 0.049(3) 0.003(2) 0.009(2) 0.000(2) N4 0.038(3) 0.034(3) 0.040(3) 0.008(2) 0.001(2) -0.006(2) N5 0.042(3) 0.035(3) 0.035(3) 0.000(2) 0.005(2) -0.002(2) N6 0.024(3) 0.032(3) 0.036(3) -0.001(2) 0.005(2) -0.004(2) C1 0.029(3) 0.019(3) 0.025(3) 0.000(2) 0.000(2) -0.002(2) C2 0.034(3) 0.020(3) 0.027(3) 0.003(2) -0.005(3) -0.004(2) C3 0.038(4) 0.034(3) 0.031(3) 0.004(3) -0.004(3) 0.009(3) C4 0.042(4) 0.042(4) 0.032(3) 0.009(3) -0.001(3) 0.005(3) C5 0.041(4) 0.046(4) 0.025(3) 0.004(3) 0.000(3) -0.001(3) C6 0.025(3) 0.020(3) 0.036(3) 0.004(2) -0.004(3) -0.010(2) C7 0.025(3) 0.035(4) 0.030(3) 0.007(3) -0.004(2) 0.004(3) C8 0.045(5) 0.060(5) 0.049(4) 0.012(3) -0.003(3) 0.020(4) C9 0.048(5) 0.040(4) 0.043(4) 0.007(3) -0.002(3) 0.008(3) C10 0.064(6) 0.054(5) 0.095(6) 0.018(4) -0.022(5) 0.001(4) C11 0.110(9) 0.027(4) 0.125(8) 0.006(4) -0.031(7) 0.003(5) C12 0.114(9) 0.062(6) 0.090(7) -0.010(5) -0.025(6) 0.048(6) C13 0.031(4) 0.046(4) 0.050(4) 0.013(3) -0.001(3) 0.007(3) C14 0.048(5) 0.072(5) 0.056(4) 0.012(4) 0.007(4) -0.014(4) C15 0.025(4) 0.033(3) 0.046(4) 0.003(3) 0.002(3) -0.003(3) C16 0.044(5) 0.048(4) 0.080(5) 0.011(4) 0.017(4) 0.004(3) C17 0.050(6) 0.063(5) 0.126(8) 0.021(5) 0.014(5) 0.013(4) C18 0.040(5) 0.073(6) 0.094(6) 0.018(5) 0.009(4) 0.017(4) C19 0.031(4) 0.063(5) 0.056(4) 0.001(3) 0.006(3) 0.004(3) C20 0.031(4) 0.044(4) 0.033(3) 0.002(3) 0.006(3) -0.002(3) C21 0.034(4) 0.048(4) 0.028(3) 0.006(3) 0.000(3) -0.011(3) C22 0.044(4) 0.046(4) 0.049(4) 0.009(3) -0.002(3) -0.017(3) C23 0.072(6) 0.049(5) 0.067(5) 0.009(4) 0.008(4) -0.032(4) C24 0.075(6) 0.036(4) 0.081(6) 0.020(4) -0.002(5) -0.007(4) C25 0.043(4) 0.046(4) 0.053(4) 0.010(3) -0.008(3) -0.003(3) C26 0.027(4) 0.091(6) 0.076(5) 0.006(5) 0.005(4) -0.013(4) C27 0.044(5) 0.077(6) 0.069(5) 0.008(4) 0.007(4) -0.032(4) C28 0.075(6) 0.039(4) 0.042(4) -0.001(3) 0.014(4) -0.003(4) C29 0.080(6) 0.056(5) 0.036(4) 0.013(3) 0.009(4) 0.014(4) C30 0.063(5) 0.063(5) 0.033(4) -0.008(3) 0.001(3) 0.016(4) C31 0.034(4) 0.041(4) 0.043(4) -0.008(3) 0.002(3) 0.007(3) C32 0.022(3) 0.037(3) 0.038(3) -0.007(3) 0.001(3) 0.004(3) C33 0.023(3) 0.030(3) 0.042(3) -0.007(3) 0.001(3) -0.002(2) C34 0.033(4) 0.035(4) 0.057(4) -0.005(3) 0.010(3) -0.001(3) C35 0.048(4) 0.028(3) 0.074(5) -0.005(3) 0.009(4) -0.007(3) C36 0.048(4) 0.040(4) 0.055(4) 0.010(3) 0.009(4) 0.003(3) C37 0.035(4) 0.037(4) 0.039(3) 0.001(3) 0.010(3) 0.000(3) C38 0.037(4) 0.065(5) 0.050(4) -0.022(4) -0.005(3) 0.000(3) C39 0.039(4) 0.045(4) 0.064(5) -0.022(4) -0.002(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O11 1.775(4) . ? U1 O10 1.780(4) . ? U1 O9 2.253(4) . ? U1 O9 2.262(3) 3_664 ? U1 O7 2.395(5) . ? U1 O1 2.425(4) . ? U1 O3 2.507(4) . ? U1 U1 3.6640(4) 3_664 ? U1 U2 3.9012(4) . ? U1 U2 4.0165(3) 3_664 ? U2 O13 1.760(4) . ? U2 O12 1.765(4) . ? U2 O9 2.193(4) . ? U2 O8 2.462(5) 3_664 ? U2 O6 2.492(4) . ? U2 O5 2.509(4) . ? U2 O3 2.511(4) . ? U2 C13 2.866(6) . ? U2 U1 4.0165(3) 3_664 ? Zn1 O2 2.128(4) . ? Zn1 N4 2.128(5) . ? Zn1 N6 2.158(5) . ? Zn1 N1 2.164(5) . ? Zn1 N5 2.192(5) . ? Zn1 N3 2.196(5) . ? O1 C6 1.260(6) . ? O2 C6 1.246(7) . ? O3 C7 1.311(7) . ? O4 C7 1.203(7) . ? O5 C13 1.249(7) . ? O6 C13 1.256(7) . ? O7 C15 1.224(7) . ? O8 C15 1.242(7) . ? O8 U2 2.462(5) 3_664 ? O9 U1 2.262(3) 3_664 ? N1 C5 1.333(7) . ? N1 C1 1.351(6) . ? N2 C12 1.351(13) . ? N2 C8 1.356(9) . ? N3 C16 1.317(8) . ? N3 C20 1.365(8) . ? N4 C25 1.316(8) . ? N4 C21 1.355(8) . ? N5 C28 1.312(8) . ? N5 C32 1.361(7) . ? N6 C37 1.339(7) . ? N6 C33 1.352(7) . ? C1 C2 1.380(8) . ? C1 C6 1.504(8) . ? C2 C3 1.398(8) . ? C2 C7 1.512(7) . ? C3 C4 1.372(8) . ? C3 H3 0.9300 . ? C4 C5 1.380(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C8 C9 1.383(9) . ? C8 H8 0.9300 . ? C9 C10 1.363(10) . ? C9 C13 1.480(8) . ? C10 C11 1.365(11) . ? C10 H10 0.9300 . ? C11 C12 1.343(14) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 C15 1.474(9) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 C17 1.405(11) . ? C16 H16 0.9300 . ? C17 C18 1.329(12) . ? C17 H17 0.9300 . ? C18 C19 1.394(10) . ? C18 H18 0.9300 . ? C19 C20 1.397(9) . ? C19 C26 1.428(10) . ? C20 C21 1.449(9) . ? C21 C22 1.400(8) . ? C22 C23 1.397(10) . ? C22 C27 1.428(11) . ? C23 C24 1.364(11) . ? C23 H23 0.9300 . ? C24 C25 1.393(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.336(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.409(10) . ? C28 H28 0.9300 . ? C29 C30 1.369(10) . ? C29 H29 0.9300 . ? C30 C31 1.396(9) . ? C30 H30 0.9300 . ? C31 C32 1.410(8) . ? C31 C38 1.430(9) . ? C32 C33 1.441(8) . ? C33 C34 1.406(8) . ? C34 C35 1.421(9) . ? C34 C39 1.435(9) . ? C35 C36 1.343(10) . ? C35 H35 0.9300 . ? C36 C37 1.407(9) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.356(10) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? 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 O11 U1 O10 174.45(18) . . ? O11 U1 O9 94.21(16) . . ? O10 U1 O9 90.42(17) . . ? O11 U1 O9 92.65(15) . 3_664 ? O10 U1 O9 91.71(16) . 3_664 ? O9 U1 O9 71.49(15) . 3_664 ? O11 U1 O7 90.6(2) . . ? O10 U1 O7 87.4(2) . . ? O9 U1 O7 143.50(16) . . ? O9 U1 O7 72.17(16) 3_664 . ? O11 U1 O1 85.59(15) . . ? O10 U1 O1 88.93(15) . . ? O9 U1 O1 137.45(13) . . ? O9 U1 O1 151.05(13) 3_664 . ? O7 U1 O1 78.96(17) . . ? O11 U1 O3 93.04(16) . . ? O10 U1 O3 85.94(17) . . ? O9 U1 O3 67.26(12) . . ? O9 U1 O3 138.65(13) 3_664 . ? O7 U1 O3 148.60(17) . . ? O1 U1 O3 70.27(13) . . ? O11 U1 U1 94.23(12) . 3_664 ? O10 U1 U1 91.32(13) . 3_664 ? O9 U1 U1 35.82(9) . 3_664 ? O9 U1 U1 35.66(9) 3_664 3_664 ? O7 U1 U1 107.77(14) . 3_664 ? O1 U1 U1 173.27(9) . 3_664 ? O3 U1 U1 103.04(9) . 3_664 ? O11 U1 U2 94.31(13) . . ? O10 U1 U2 88.33(14) . . ? O9 U1 U2 28.24(9) . . ? O9 U1 U2 99.70(9) 3_664 . ? O7 U1 U2 170.70(13) . . ? O1 U1 U2 109.25(9) . . ? O3 U1 U2 39.02(9) . . ? U1 U1 U2 64.044(7) 3_664 . ? O11 U1 U2 89.67(12) . 3_664 ? O10 U1 U2 92.82(13) . 3_664 ? O9 U1 U2 96.66(9) . 3_664 ? O9 U1 U2 25.21(9) 3_664 3_664 ? O7 U1 U2 47.15(14) . 3_664 ? O1 U1 U2 125.86(9) . 3_664 ? O3 U1 U2 163.84(9) . 3_664 ? U1 U1 U2 60.848(7) 3_664 3_664 ? U2 U1 U2 124.893(6) . 3_664 ? O13 U2 O12 176.9(2) . . ? O13 U2 O9 91.09(18) . . ? O12 U2 O9 91.59(18) . . ? O13 U2 O8 82.7(2) . 3_664 ? O12 U2 O8 95.1(2) . 3_664 ? O9 U2 O8 106.68(15) . 3_664 ? O13 U2 O6 90.13(18) . . ? O12 U2 O6 87.00(19) . . ? O9 U2 O6 171.58(14) . . ? O8 U2 O6 65.23(15) 3_664 . ? O13 U2 O5 88.18(18) . . ? O12 U2 O5 90.9(2) . . ? O9 U2 O5 136.85(14) . . ? O8 U2 O5 115.98(16) 3_664 . ? O6 U2 O5 51.53(14) . . ? O13 U2 O3 89.13(17) . . ? O12 U2 O3 93.29(19) . . ? O9 U2 O3 68.02(12) . . ? O8 U2 O3 170.23(16) 3_664 . ? O6 U2 O3 120.33(13) . . ? O5 U2 O3 68.82(13) . . ? O13 U2 C13 86.80(19) . . ? O12 U2 C13 91.1(2) . . ? O9 U2 C13 162.50(16) . . ? O8 U2 C13 90.30(18) 3_664 . ? O6 U2 C13 25.93(16) . . ? O5 U2 C13 25.78(16) . . ? O3 U2 C13 94.56(16) . . ? O13 U2 U1 90.16(14) . . ? O12 U2 U1 92.93(16) . . ? O9 U2 U1 29.08(9) . . ? O8 U2 U1 135.29(12) 3_664 . ? O6 U2 U1 159.26(10) . . ? O5 U2 U1 107.77(10) . . ? O3 U2 U1 38.94(8) . . ? C13 U2 U1 133.47(13) . . ? O13 U2 U1 93.12(14) . 3_664 ? O12 U2 U1 88.62(15) . 3_664 ? O9 U2 U1 26.05(9) . 3_664 ? O8 U2 U1 81.18(12) 3_664 3_664 ? O6 U2 U1 145.54(10) . 3_664 ? O5 U2 U1 162.79(10) . 3_664 ? O3 U2 U1 94.03(8) . 3_664 ? C13 U2 U1 171.41(13) . 3_664 ? U1 U2 U1 55.107(6) . 3_664 ? O2 Zn1 N4 99.85(17) . . ? O2 Zn1 N6 89.27(16) . . ? N4 Zn1 N6 163.88(18) . . ? O2 Zn1 N1 75.68(15) . . ? N4 Zn1 N1 94.77(18) . . ? N6 Zn1 N1 100.39(17) . . ? O2 Zn1 N5 161.45(17) . . ? N4 Zn1 N5 96.71(18) . . ? N6 Zn1 N5 76.71(18) . . ? N1 Zn1 N5 94.73(18) . . ? O2 Zn1 N3 90.10(17) . . ? N4 Zn1 N3 77.31(19) . . ? N6 Zn1 N3 89.50(18) . . ? N1 Zn1 N3 162.45(18) . . ? N5 Zn1 N3 101.69(19) . . ? C6 O1 U1 126.2(3) . . ? C6 O2 Zn1 116.6(4) . . ? C7 O3 U1 123.8(3) . . ? C7 O3 U2 129.9(3) . . ? U1 O3 U2 102.04(13) . . ? C13 O5 U2 93.3(4) . . ? C13 O6 U2 93.9(4) . . ? C15 O7 U1 168.0(5) . . ? C15 O8 U2 109.5(4) . 3_664 ? U2 O9 U1 122.68(15) . . ? U2 O9 U1 128.74(17) . 3_664 ? U1 O9 U1 108.51(15) . 3_664 ? C5 N1 C1 118.7(5) . . ? C5 N1 Zn1 127.8(4) . . ? C1 N1 Zn1 113.2(3) . . ? C12 N2 C8 116.4(8) . . ? C16 N3 C20 117.4(6) . . ? C16 N3 Zn1 129.5(4) . . ? C20 N3 Zn1 112.7(4) . . ? C25 N4 C21 118.2(5) . . ? C25 N4 Zn1 127.0(4) . . ? C21 N4 Zn1 114.6(4) . . ? C28 N5 C32 118.0(5) . . ? C28 N5 Zn1 128.8(4) . . ? C32 N5 Zn1 113.2(4) . . ? C37 N6 C33 118.2(5) . . ? C37 N6 Zn1 127.0(4) . . ? C33 N6 Zn1 114.7(4) . . ? N1 C1 C2 121.8(5) . . ? N1 C1 C6 113.9(5) . . ? C2 C1 C6 124.1(5) . . ? C1 C2 C3 118.4(5) . . ? C1 C2 C7 125.2(5) . . ? C3 C2 C7 116.3(5) . . ? C4 C3 C2 119.6(5) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.4(5) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 122.9(5) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? O2 C6 O1 124.8(5) . . ? O2 C6 C1 117.6(5) . . ? O1 C6 C1 117.5(5) . . ? O4 C7 O3 126.2(5) . . ? O4 C7 C2 118.6(5) . . ? O3 C7 C2 115.0(5) . . ? N2 C8 C9 122.0(7) . . ? N2 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 117.6(6) . . ? C10 C9 C13 121.5(7) . . ? C8 C9 C13 120.8(6) . . ? C9 C10 C11 122.0(8) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 116.7(8) . . ? C12 C11 H11 121.7 . . ? C10 C11 H11 121.7 . . ? C11 C12 N2 125.1(8) . . ? C11 C12 H12 117.4 . . ? N2 C12 H12 117.4 . . ? O5 C13 O6 120.4(6) . . ? O5 C13 C9 121.2(6) . . ? O6 C13 C9 118.4(6) . . ? O5 C13 U2 60.9(3) . . ? O6 C13 U2 60.2(3) . . ? C9 C13 U2 170.1(5) . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O7 C15 O8 119.1(6) . . ? O7 C15 C14 121.1(6) . . ? O8 C15 C14 119.8(6) . . ? N3 C16 C17 123.0(7) . . ? N3 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 118.8(7) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 121.2(7) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C20 116.6(6) . . ? C18 C19 C26 124.7(7) . . ? C20 C19 C26 118.7(6) . . ? N3 C20 C19 122.9(6) . . ? N3 C20 C21 116.8(5) . . ? C19 C20 C21 120.3(6) . . ? N4 C21 C22 123.0(6) . . ? N4 C21 C20 118.1(5) . . ? C22 C21 C20 118.9(6) . . ? C23 C22 C21 116.8(7) . . ? C23 C22 C27 124.3(6) . . ? C21 C22 C27 119.0(6) . . ? C24 C23 C22 120.3(6) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 118.8(7) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? N4 C25 C24 123.0(7) . . ? N4 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C27 C26 C19 121.2(7) . . ? C27 C26 H26 119.4 . . ? C19 C26 H26 119.4 . . ? C26 C27 C22 121.9(6) . . ? C26 C27 H27 119.1 . . ? C22 C27 H27 119.1 . . ? N5 C28 C29 122.8(6) . . ? N5 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C30 C29 C28 119.9(6) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 118.6(6) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C30 C31 C32 118.0(6) . . ? C30 C31 C38 122.7(6) . . ? C32 C31 C38 119.3(6) . . ? N5 C32 C31 122.7(5) . . ? N5 C32 C33 117.6(5) . . ? C31 C32 C33 119.6(5) . . ? N6 C33 C34 122.7(5) . . ? N6 C33 C32 117.6(5) . . ? C34 C33 C32 119.6(5) . . ? C33 C34 C35 117.5(6) . . ? C33 C34 C39 119.3(6) . . ? C35 C34 C39 123.2(6) . . ? C36 C35 C34 119.3(6) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.1(6) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? N6 C37 C36 122.2(6) . . ? N6 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C39 C38 C31 121.1(6) . . ? C39 C38 H38 119.4 . . ? C31 C38 H38 119.4 . . ? C38 C39 C34 121.0(6) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.104 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.115 #============================================================END