Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Pierre Thuery' _publ_contact_author_address ; Service de Chimie Moleculaire DSM DRECAM, CNRA URA 331 CEA Saclay Bat 125 Gif-sur-Yvette 91191 FRANCE ; _publ_contact_author_email THUERY@DRECAM.CEA.FR _publ_section_title ; Uranyl citrate dimers as guests in a copper-bipyridine framework: a novel heterometallic inorganic-organic hybrid compound ; _publ_author_name 'Pierre Thuery' data_1 _database_code_depnum_ccdc_archive 'CCDC 635249' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H44 Cu N4 O27 U2' _chemical_formula_weight 1456.31 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 orthorhombic _symmetry_space_group_name_H-M 'P c a 21' 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 16.5938(7) _cell_length_b 15.1034(6) _cell_length_c 18.0112(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4514.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 92739 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.67 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2772 _exptl_absorpt_coefficient_mu 7.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.366 _exptl_absorpt_correction_T_max 0.499 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and four \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 92739 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.67 _reflns_number_total 8233 _reflns_number_gt 7381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some badly behaving atoms. The O-bound H atoms have been found on Fourier-difference maps, except for four water molecules. The C-bound H atoms were introduced at calculated positions. All were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0581P)^2^+50.8587P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.491(11) _refine_ls_number_reflns 8233 _refine_ls_number_parameters 596 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.008 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.276 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 0.83229(2) 0.32499(2) -0.00121(2) 0.02426(11) Uani 1 1 d . . . U2 U 0.64106(2) 0.17746(2) 0.00384(2) 0.02177(11) Uani 1 1 d . . . Cu Cu 0.76270(8) 0.75044(8) 0.75024(13) 0.0233(3) Uani 1 1 d . . . O1 O 0.8243(6) 0.2997(6) -0.0984(5) 0.035(2) Uani 1 1 d . . . O2 O 0.8404(5) 0.3564(7) 0.0934(5) 0.032(2) Uani 1 1 d . . . O3 O 0.6501(6) 0.1907(6) -0.0959(5) 0.031(2) Uani 1 1 d . . . O4 O 0.6306(6) 0.1575(6) 0.0998(5) 0.031(2) Uani 1 1 d . . . O5 O 0.7811(4) 0.1802(4) 0.0217(4) 0.0178(16) Uani 1 1 d . . . O6 O 0.9342(5) 0.2210(5) 0.0107(8) 0.048(3) Uani 1 1 d . . . O7 O 0.9777(6) 0.0859(6) 0.0396(6) 0.043(2) Uani 1 1 d . . . O8 O 0.6825(5) 0.0308(5) -0.0141(6) 0.039(2) Uani 1 1 d . . . O9 O 0.7523(6) -0.0897(6) -0.0414(6) 0.043(2) Uani 1 1 d . . . O10 O 0.8699(6) 0.1820(7) 0.1758(6) 0.048(3) Uani 1 1 d . . . H10 H 0.8552 0.2220 0.2034 0.057 Uiso 1 1 d R . . O11 O 0.7582(7) 0.1149(7) 0.2166(6) 0.048(2) Uani 1 1 d . . . O12 O 0.6909(5) 0.3238(4) 0.0155(4) 0.030(2) Uani 1 1 d . . . O13 O 0.5375(4) 0.2822(5) 0.0048(7) 0.0351(18) Uani 1 1 d . . . O14 O 0.4916(5) 0.4193(6) 0.0296(6) 0.041(2) Uani 1 1 d . . . O15 O 0.7894(5) 0.4692(5) -0.0314(6) 0.038(2) Uani 1 1 d . . . O16 O 0.7227(5) 0.5902(6) -0.0580(5) 0.034(2) Uani 1 1 d . . . O17 O 0.7077(6) 0.4006(7) 0.2094(5) 0.050(3) Uani 1 1 d D . . H17 H 0.7387 0.3501 0.2094 0.060 Uiso 1 1 d R . . O18 O 0.5957(6) 0.3345(6) 0.1665(5) 0.041(2) Uani 1 1 d D . . O19 O 0.9544(5) 0.4115(5) -0.0238(5) 0.035(2) Uani 1 1 d . . . H19A H 0.9534 0.4664 -0.0049 0.042 Uiso 1 1 d R . . H19B H 1.0016 0.3901 -0.0164 0.042 Uiso 1 1 d R . . O20 O 0.5189(5) 0.0877(5) -0.0137(5) 0.032(2) Uani 1 1 d . . . H20A H 0.4727 0.1066 0.0067 0.038 Uiso 1 1 d R . . H20B H 0.5222 0.0353 0.0025 0.038 Uiso 1 1 d R . . O21 O 0.7649(6) 0.7423(6) 0.6245(6) 0.033(2) Uani 1 1 d . . . H21A H 0.7327 0.7172 0.5859 0.040 Uiso 1 1 d R . . H21B H 0.8093 0.7571 0.6019 0.040 Uiso 1 1 d R . . O22 O 0.7594(5) 0.7539(5) 0.8801(7) 0.033(3) Uani 1 1 d . . . H22A H 0.7273 0.7876 0.9039 0.040 Uiso 1 1 d R . . H22B H 0.7842 0.7234 0.9105 0.040 Uiso 1 1 d R . . O23 O 0.8330(8) 0.3049(8) 0.2792(7) 0.064(3) Uani 1 1 d U . . O24 O 0.6533(5) 0.6575(6) 0.5350(5) 0.035(2) Uani 1 1 d . . . H24A H 0.6680 0.6209 0.5002 0.042 Uiso 1 1 d R . . H24B H 0.6053 0.6429 0.5391 0.042 Uiso 1 1 d R . . O25 O 0.3858(6) 0.1675(5) 0.0185(6) 0.044(3) Uani 1 1 d . . . O26 O 1.1227(6) 0.1664(6) 0.0354(5) 0.038(2) Uani 1 1 d . . . O27 O 0.5888(6) 0.6648(7) 0.0055(11) 0.069(3) Uani 1 1 d U . . N1 N 0.8486(8) 0.8458(9) 0.7555(8) 0.033(3) Uani 1 1 d . . . N2 N 0.8534(6) 0.6569(7) 0.7519(6) 0.019(2) Uani 1 1 d . . . N3 N 0.6785(6) 0.6542(7) 0.7573(6) 0.023(2) Uani 1 1 d . . . N4 N 0.6705(7) 0.8450(8) 0.7460(7) 0.024(2) Uani 1 1 d . . . C1 C 0.8355(8) 0.1073(8) 0.0316(8) 0.032(3) Uani 1 1 d U . . C2 C 0.9238(9) 0.1392(9) 0.0303(7) 0.039(3) Uani 1 1 d . . . C3 C 0.8250(7) 0.0435(9) -0.0340(8) 0.033(3) Uani 1 1 d U . . H3A H 0.8243 0.0774 -0.0797 0.040 Uiso 1 1 calc R . . H3B H 0.8711 0.0040 -0.0358 0.040 Uiso 1 1 calc R . . C4 C 0.7513(7) -0.0096(8) -0.0297(7) 0.029(3) Uani 1 1 d . . . C5 C 0.8207(9) 0.0602(8) 0.1061(8) 0.039(3) Uani 1 1 d . . . H5A H 0.7714 0.0260 0.1024 0.047 Uiso 1 1 calc R . . H5B H 0.8645 0.0192 0.1151 0.047 Uiso 1 1 calc R . . C6 C 0.8140(8) 0.1222(8) 0.1714(7) 0.034(3) Uani 1 1 d . . . C7 C 0.6372(7) 0.3978(8) 0.0228(6) 0.027(3) Uani 1 1 d . . . C8 C 0.5477(7) 0.3635(8) 0.0218(7) 0.031(3) Uani 1 1 d . . . C9 C 0.6431(9) 0.4560(10) -0.0481(8) 0.041(4) Uani 1 1 d . . . H9A H 0.5977 0.4963 -0.0503 0.049 Uiso 1 1 calc R . . H9B H 0.6418 0.4187 -0.0919 0.049 Uiso 1 1 calc R . . C10 C 0.7255(8) 0.5109(9) -0.0461(7) 0.034(3) Uani 1 1 d . . . C11 C 0.6516(8) 0.4497(8) 0.0930(7) 0.030(3) Uani 1 1 d . . . H11A H 0.6091 0.4931 0.0989 0.036 Uiso 1 1 calc R . . H11B H 0.7023 0.4813 0.0888 0.036 Uiso 1 1 calc R . . C12 C 0.6542(6) 0.3908(7) 0.1615(6) 0.029(3) Uani 1 1 d D . . C13 C 0.8532(8) 0.9114(9) 0.7046(9) 0.033(4) Uani 1 1 d . . . H13 H 0.8134 0.9123 0.6682 0.040 Uiso 1 1 calc R . . C14 C 0.9089(10) 0.9750(10) 0.7010(9) 0.038(4) Uani 1 1 d . . . H14 H 0.9055 1.0196 0.6655 0.046 Uiso 1 1 calc R . . C15 C 0.9729(8) 0.9731(8) 0.7523(8) 0.025(3) Uani 1 1 d . . . C16 C 0.9695(10) 0.9073(10) 0.8058(8) 0.036(4) Uani 1 1 d . . . H16 H 1.0090 0.9041 0.8424 0.043 Uiso 1 1 calc R . . C17 C 0.9072(9) 0.8462(11) 0.8049(8) 0.036(4) Uani 1 1 d . . . H17A H 0.9067 0.8027 0.8415 0.043 Uiso 1 1 calc R . . C18 C 0.9150(9) 0.6635(9) 0.7026(8) 0.031(3) Uani 1 1 d . . . H18 H 0.9138 0.7077 0.6667 0.037 Uiso 1 1 calc R . . C19 C 0.9805(8) 0.6048(10) 0.7050(7) 0.031(3) Uani 1 1 d . . . H19 H 1.0221 0.6110 0.6708 0.037 Uiso 1 1 calc R . . C20 C 0.9843(7) 0.5377(7) 0.7573(7) 0.024(2) Uani 1 1 d . . . C21 C 0.9209(8) 0.5349(9) 0.8084(8) 0.036(3) Uani 1 1 d . . . H21 H 0.9208 0.4924 0.8457 0.043 Uiso 1 1 calc R . . C22 C 0.8600(8) 0.5938(8) 0.8037(8) 0.027(3) Uani 1 1 d . . . H22 H 0.8194 0.5903 0.8392 0.033 Uiso 1 1 calc R . . C23 C 0.6806(7) 0.5810(8) 0.7146(7) 0.026(3) Uani 1 1 d . . . H23 H 0.7250 0.5729 0.6838 0.031 Uiso 1 1 calc R . . C24 C 0.6197(9) 0.5161(9) 0.7138(8) 0.034(3) Uani 1 1 d . . . H24 H 0.6257 0.4660 0.6842 0.041 Uiso 1 1 calc R . . C25 C 0.5508(6) 0.5263(7) 0.7569(6) 0.019(2) Uani 1 1 d . . . C26 C 0.5486(7) 0.6031(9) 0.8019(7) 0.024(3) Uani 1 1 d . . . H26 H 0.5051 0.6135 0.8334 0.029 Uiso 1 1 calc R . . C27 C 0.6109(9) 0.6617(9) 0.7986(8) 0.028(3) Uani 1 1 d . . . H27 H 0.6065 0.7121 0.8280 0.034 Uiso 1 1 calc R . . C28 C 0.6075(8) 0.8345(8) 0.7013(7) 0.021(3) Uani 1 1 d . . . H28 H 0.6075 0.7875 0.6679 0.025 Uiso 1 1 calc R . . C29 C 0.5418(7) 0.8913(8) 0.7028(7) 0.020(3) Uani 1 1 d . . . H29 H 0.4978 0.8808 0.6720 0.024 Uiso 1 1 calc R . . C30 C 0.5418(8) 0.9617(8) 0.7488(8) 0.024(3) Uani 1 1 d U . . C31 C 0.6096(10) 0.9715(11) 0.7948(9) 0.039(4) Uani 1 1 d . . . H31 H 0.6106 1.0174 0.8292 0.047 Uiso 1 1 calc R . . C32 C 0.6732(8) 0.9163(10) 0.7905(8) 0.029(3) Uani 1 1 d U . . H32 H 0.7191 0.9276 0.8184 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0253(2) 0.0220(2) 0.0255(2) -0.0004(3) 0.0018(3) -0.00487(14) U2 0.0187(2) 0.02190(19) 0.0247(2) 0.0008(3) -0.0007(3) -0.00146(13) Cu 0.0180(7) 0.0178(6) 0.0341(7) 0.0008(6) -0.0001(7) 0.0020(6) O1 0.046(5) 0.028(4) 0.030(5) -0.014(4) -0.003(4) -0.001(4) O2 0.035(5) 0.036(5) 0.027(5) -0.009(4) -0.004(4) -0.002(4) O3 0.048(6) 0.023(5) 0.022(4) 0.007(4) 0.006(4) -0.009(4) O4 0.037(6) 0.027(5) 0.028(5) 0.005(4) 0.005(4) -0.007(4) O5 0.0168(18) 0.0181(18) 0.0185(18) -0.0002(10) -0.0009(10) 0.0002(10) O6 0.024(4) 0.033(4) 0.087(8) 0.010(6) -0.012(6) -0.011(3) O7 0.035(5) 0.025(5) 0.070(7) -0.004(4) -0.004(5) 0.009(4) O8 0.031(5) 0.029(4) 0.057(7) 0.006(4) -0.010(4) 0.001(3) O9 0.038(5) 0.030(5) 0.062(6) -0.008(4) 0.004(5) 0.015(4) O10 0.039(6) 0.052(7) 0.053(7) -0.004(5) -0.001(5) -0.009(5) O11 0.050(6) 0.048(6) 0.046(6) 0.002(5) 0.003(5) -0.009(5) O12 0.047(4) 0.016(3) 0.028(5) -0.003(3) 0.001(4) 0.006(3) O13 0.022(4) 0.023(4) 0.060(5) -0.002(6) 0.005(6) -0.001(3) O14 0.027(5) 0.029(5) 0.067(7) 0.006(4) 0.002(4) -0.005(4) O15 0.028(5) 0.016(4) 0.069(6) 0.003(4) 0.010(4) -0.005(3) O16 0.028(5) 0.028(5) 0.045(5) 0.004(4) 0.008(4) 0.001(4) O17 0.044(6) 0.055(6) 0.050(6) -0.006(5) -0.001(5) -0.005(5) O18 0.044(6) 0.039(5) 0.041(6) -0.008(4) 0.003(4) -0.010(4) O19 0.031(5) 0.027(4) 0.048(6) 0.003(3) 0.004(4) 0.005(4) O20 0.020(4) 0.031(4) 0.044(6) 0.001(4) -0.008(4) 0.002(3) O21 0.029(5) 0.040(6) 0.029(5) 0.005(4) -0.007(4) -0.001(4) O22 0.037(5) 0.026(5) 0.037(6) -0.005(4) 0.000(4) -0.010(4) O23 0.076(9) 0.047(7) 0.068(8) 0.005(6) -0.020(6) -0.008(6) O24 0.027(4) 0.035(4) 0.043(4) -0.004(3) -0.006(3) -0.003(3) O25 0.040(5) 0.030(5) 0.063(8) 0.003(4) 0.000(5) -0.001(4) O26 0.042(6) 0.030(5) 0.042(5) 0.007(4) -0.004(4) 0.003(4) O27 0.055(4) 0.060(4) 0.092(5) 0.000(4) 0.000(5) -0.006(4) N1 0.036(7) 0.025(6) 0.039(7) 0.002(5) 0.004(6) 0.005(5) N2 0.019(2) 0.020(2) 0.020(2) 0.0001(10) 0.0001(10) -0.0001(10) N3 0.020(4) 0.021(4) 0.027(4) 0.002(3) -0.002(3) -0.001(3) N4 0.024(6) 0.020(5) 0.030(6) 0.003(4) -0.006(5) -0.007(4) C1 0.039(6) 0.021(5) 0.038(6) 0.004(5) -0.001(5) -0.008(5) C2 0.037(8) 0.039(8) 0.041(7) -0.009(6) 0.010(6) -0.011(6) C3 0.016(5) 0.039(6) 0.044(6) -0.004(5) 0.008(5) 0.006(5) C4 0.023(6) 0.034(7) 0.031(6) -0.001(5) 0.000(5) 0.010(5) C5 0.056(9) 0.022(7) 0.040(8) 0.009(5) -0.008(6) 0.000(6) C6 0.040(8) 0.030(7) 0.034(7) 0.019(5) -0.012(6) -0.006(6) C7 0.024(6) 0.031(6) 0.027(7) 0.010(5) 0.003(4) 0.003(5) C8 0.026(6) 0.022(6) 0.046(9) -0.001(5) 0.009(5) -0.008(5) C9 0.056(10) 0.039(8) 0.027(7) 0.014(6) 0.009(6) -0.004(7) C10 0.026(7) 0.052(9) 0.025(7) -0.007(6) 0.010(5) -0.007(6) C11 0.030(7) 0.013(6) 0.048(8) -0.005(5) 0.005(6) 0.002(5) C12 0.029(7) 0.027(7) 0.032(7) -0.011(5) 0.016(5) 0.000(5) C13 0.021(7) 0.021(7) 0.057(9) 0.011(6) -0.004(6) -0.002(6) C14 0.042(9) 0.022(7) 0.050(9) 0.007(6) -0.015(7) -0.019(6) C15 0.031(7) 0.023(6) 0.022(6) 0.002(5) 0.000(5) -0.013(5) C16 0.051(9) 0.030(8) 0.027(7) 0.003(6) -0.009(6) -0.021(7) C17 0.027(8) 0.045(9) 0.034(8) 0.013(6) -0.008(6) -0.017(7) C18 0.036(9) 0.027(7) 0.029(7) 0.004(5) 0.003(6) -0.005(6) C19 0.024(7) 0.040(8) 0.028(7) 0.006(6) -0.003(5) 0.002(6) C20 0.025(6) 0.025(5) 0.021(5) -0.010(4) 0.000(4) -0.006(4) C21 0.035(8) 0.033(7) 0.041(8) 0.017(6) 0.008(6) -0.004(6) C22 0.022(7) 0.025(7) 0.035(8) 0.008(5) 0.003(5) 0.001(5) C23 0.020(7) 0.016(6) 0.041(8) -0.006(5) 0.011(6) -0.004(5) C24 0.035(8) 0.026(7) 0.040(8) 0.001(6) 0.012(6) -0.003(6) C25 0.019(4) 0.016(4) 0.020(4) 0.002(3) -0.005(4) 0.004(3) C26 0.020(5) 0.022(4) 0.030(5) 0.000(4) 0.002(4) -0.001(4) C27 0.024(8) 0.022(7) 0.039(8) -0.002(5) 0.004(6) 0.009(5) C28 0.022(5) 0.015(4) 0.026(4) 0.002(3) 0.003(4) -0.004(4) C29 0.013(6) 0.019(7) 0.028(6) 0.004(5) 0.001(5) -0.004(5) C30 0.017(5) 0.023(6) 0.033(6) 0.013(5) 0.003(5) 0.007(4) C31 0.048(10) 0.029(8) 0.040(8) -0.019(6) -0.010(7) -0.002(7) C32 0.020(6) 0.029(6) 0.039(6) -0.008(5) -0.011(5) 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 U1 O2 1.775(8) . ? U1 O1 1.797(9) . ? U1 O6 2.318(8) . ? U1 O15 2.355(8) . ? U1 O12 2.366(9) . ? U1 O5 2.383(7) . ? U1 O19 2.446(9) . ? U1 U2 3.8785(5) . ? U2 O4 1.763(9) . ? U2 O3 1.814(9) . ? U2 O13 2.336(7) . ? U2 O8 2.342(8) . ? U2 O5 2.346(7) . ? U2 O12 2.369(7) . ? U2 O20 2.459(8) . ? Cu N3 2.021(10) . ? Cu N1 2.028(14) . ? Cu N2 2.064(11) . ? Cu N4 2.094(12) . ? Cu O21 2.268(11) . ? Cu O22 2.340(12) . ? O5 C1 1.435(15) . ? O6 C2 1.296(16) . ? O7 C2 1.214(17) . ? O8 C4 1.324(14) . ? O9 C4 1.228(15) . ? O10 C6 1.297(16) . ? O11 C6 1.237(17) . ? O12 C7 1.435(14) . ? O13 C8 1.277(14) . ? O14 C8 1.264(15) . ? O15 C10 1.261(16) . ? O16 C10 1.218(16) . ? O16 O27 2.740(15) . ? O17 C12 1.247(9) . ? O18 C12 1.293(9) . ? O23 O3 2.849(15) 4_655 ? O24 O25 2.738(12) 2_665 ? O26 O27 2.665(13) 3_565 ? N1 C17 1.32(2) . ? N1 C13 1.35(2) . ? N2 C22 1.338(17) . ? N2 C18 1.359(18) . ? N3 C23 1.346(16) . ? N3 C27 1.351(18) . ? N4 C28 1.329(17) . ? N4 C32 1.343(19) . ? C1 C3 1.534(18) . ? C1 C5 1.538(18) . ? C1 C2 1.544(18) . ? C3 C4 1.465(17) . ? C5 C6 1.508(19) . ? C7 C11 1.506(17) . ? C7 C9 1.554(16) . ? C7 C8 1.573(16) . ? C9 C10 1.599(19) . ? C11 C12 1.521(17) . ? C13 C14 1.33(2) . ? C14 C15 1.41(2) . ? C15 C16 1.386(19) . ? C15 C30 1.510(15) 3_575 ? C16 C17 1.39(2) . ? C18 C19 1.40(2) . ? C19 C20 1.385(18) . ? C20 C21 1.398(18) . ? C20 C25 1.466(16) 3_565 ? C21 C22 1.350(19) . ? C23 C24 1.408(18) . ? C24 C25 1.391(17) . ? C25 C26 1.417(17) . ? C25 C20 1.466(16) 3_465 ? C26 C27 1.36(2) . ? C28 C29 1.388(18) . ? C29 C30 1.348(19) . ? C30 C31 1.41(2) . ? C30 C15 1.511(15) 3_475 ? C31 C32 1.35(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O1 176.7(5) . . ? O2 U1 O6 92.1(5) . . ? O1 U1 O6 90.0(5) . . ? O2 U1 O15 89.9(4) . . ? O1 U1 O15 87.1(4) . . ? O6 U1 O15 150.3(3) . . ? O2 U1 O12 87.4(3) . . ? O1 U1 O12 92.8(4) . . ? O6 U1 O12 135.0(3) . . ? O15 U1 O12 74.7(3) . . ? O2 U1 O5 96.1(4) . . ? O1 U1 O5 87.0(4) . . ? O6 U1 O5 67.8(3) . . ? O15 U1 O5 141.4(3) . . ? O12 U1 O5 67.5(2) . . ? O2 U1 O19 87.4(4) . . ? O1 U1 O19 90.7(4) . . ? O6 U1 O19 76.9(3) . . ? O15 U1 O19 73.6(3) . . ? O12 U1 O19 147.9(3) . . ? O5 U1 O19 144.6(3) . . ? O4 U2 O3 176.3(5) . . ? O4 U2 O13 92.1(5) . . ? O3 U2 O13 89.6(5) . . ? O4 U2 O8 90.1(4) . . ? O3 U2 O8 86.7(4) . . ? O13 U2 O8 149.0(3) . . ? O4 U2 O5 88.0(4) . . ? O3 U2 O5 93.0(4) . . ? O13 U2 O5 135.7(2) . . ? O8 U2 O5 75.2(3) . . ? O4 U2 O12 96.1(4) . . ? O3 U2 O12 87.5(4) . . ? O13 U2 O12 67.9(3) . . ? O8 U2 O12 142.4(3) . . ? O5 U2 O12 68.0(3) . . ? O4 U2 O20 87.2(4) . . ? O3 U2 O20 90.1(4) . . ? O13 U2 O20 76.6(3) . . ? O8 U2 O20 72.7(3) . . ? O5 U2 O20 147.5(2) . . ? O12 U2 O20 144.4(3) . . ? N3 Cu N1 173.7(6) . . ? N3 Cu N2 90.6(4) . . ? N1 Cu N2 88.5(4) . . ? N3 Cu N4 89.3(4) . . ? N1 Cu N4 91.8(4) . . ? N2 Cu N4 178.7(6) . . ? N3 Cu O21 92.0(4) . . ? N1 Cu O21 94.2(5) . . ? N2 Cu O21 88.1(4) . . ? N4 Cu O21 90.7(4) . . ? N3 Cu O22 86.4(4) . . ? N1 Cu O22 87.4(5) . . ? N2 Cu O22 91.0(4) . . ? N4 Cu O22 90.2(4) . . ? O21 Cu O22 178.1(3) . . ? C1 O5 U2 128.8(6) . . ? C1 O5 U1 120.1(6) . . ? U2 O5 U1 110.2(3) . . ? C2 O6 U1 125.1(8) . . ? C4 O8 U2 135.9(8) . . ? C7 O12 U1 128.4(6) . . ? C7 O12 U2 121.2(7) . . ? U1 O12 U2 110.0(3) . . ? C8 O13 U2 123.7(7) . . ? C10 O15 U1 139.8(8) . . ? C10 O16 O27 111.3(8) . . ? Cu O21 O24 126.5(4) . . ? Cu O21 O26 123.5(4) . 2_765 ? O24 O21 O26 109.7(5) . 2_765 ? O25 O24 O21 77.0(4) 2_665 . ? C17 N1 C13 114.4(13) . . ? C17 N1 Cu 123.6(11) . . ? C13 N1 Cu 121.9(11) . . ? C22 N2 C18 116.5(11) . . ? C22 N2 Cu 123.9(9) . . ? C18 N2 Cu 119.3(9) . . ? C23 N3 C27 114.0(11) . . ? C23 N3 Cu 122.4(8) . . ? C27 N3 Cu 123.2(9) . . ? C28 N4 C32 118.8(12) . . ? C28 N4 Cu 121.0(10) . . ? C32 N4 Cu 120.1(9) . . ? O5 C1 C3 108.4(10) . . ? O5 C1 C5 111.2(11) . . ? C3 C1 C5 111.3(10) . . ? O5 C1 C2 110.9(10) . . ? C3 C1 C2 106.9(11) . . ? C5 C1 C2 108.0(11) . . ? O7 C2 O6 124.9(12) . . ? O7 C2 C1 119.3(12) . . ? O6 C2 C1 115.3(12) . . ? C4 C3 C1 113.4(10) . . ? O9 C4 O8 120.1(11) . . ? O9 C4 C3 121.3(11) . . ? O8 C4 C3 118.6(11) . . ? C6 C5 C1 113.9(10) . . ? O11 C6 O10 123.9(13) . . ? O11 C6 C5 120.8(12) . . ? O10 C6 C5 115.3(12) . . ? O12 C7 C11 112.6(9) . . ? O12 C7 C9 109.0(10) . . ? C11 C7 C9 112.7(11) . . ? O12 C7 C8 109.1(9) . . ? C11 C7 C8 109.4(10) . . ? C9 C7 C8 103.7(10) . . ? O14 C8 O13 124.8(11) . . ? O14 C8 C7 118.3(10) . . ? O13 C8 C7 116.5(10) . . ? C7 C9 C10 109.2(11) . . ? O16 C10 O15 124.1(12) . . ? O16 C10 C9 118.2(12) . . ? O15 C10 C9 117.7(12) . . ? C7 C11 C12 112.3(9) . . ? O17 C12 O18 124.4(11) . . ? O17 C12 C11 120.7(10) . . ? O18 C12 C11 114.8(10) . . ? C14 C13 N1 126.8(15) . . ? C13 C14 C15 118.4(14) . . ? C16 C15 C14 116.1(13) . . ? C16 C15 C30 121.8(11) . 3_575 ? C14 C15 C30 122.1(11) . 3_575 ? C17 C16 C15 120.0(14) . . ? N1 C17 C16 124.1(14) . . ? N2 C18 C19 121.1(13) . . ? C20 C19 C18 121.2(13) . . ? C19 C20 C21 115.8(12) . . ? C19 C20 C25 120.8(11) . 3_565 ? C21 C20 C25 123.3(11) . 3_565 ? C22 C21 C20 120.2(12) . . ? N2 C22 C21 125.1(12) . . ? N3 C23 C24 123.9(11) . . ? C25 C24 C23 120.5(12) . . ? C24 C25 C26 115.5(11) . . ? C24 C25 C20 123.3(11) . 3_465 ? C26 C25 C20 121.1(10) . 3_465 ? C27 C26 C25 119.1(12) . . ? N3 C27 C26 126.9(13) . . ? N4 C28 C29 122.2(13) . . ? C30 C29 C28 119.9(13) . . ? C29 C30 C31 116.5(12) . . ? C29 C30 C15 122.6(11) . 3_475 ? C31 C30 C15 120.9(12) . 3_475 ? C32 C31 C30 121.8(13) . . ? N4 C32 C31 120.4(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10 O23 0.82 1.89 2.701(18) 170.1 . O17 H17 O23 0.92 2.12 2.827(16) 132.9 . O19 H19A O14 0.90 1.94 2.799(12) 159.7 3_565 O19 H19B O27 0.86 1.71 2.566(14) 171.5 3_565 O20 H20B O7 0.84 2.08 2.875(12) 155.5 3_455 O20 H20A O25 0.90 1.72 2.582(12) 159.4 . O21 H21A O24 0.95 1.85 2.764(13) 162.8 . O21 H21B O26 0.88 2.01 2.825(14) 153.4 2_765 O22 H22B O16 0.83 2.33 2.780(13) 115.1 1_556 O22 H22A O9 0.85 2.14 2.755(13) 128.9 1_566 O24 H24B O14 0.83 1.87 2.671(12) 161.9 2_665 O24 H24A O16 0.87 2.15 2.841(13) 136.6 4_655