Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Christopher L. Cahill' _publ_contact_author_address ; Department of Chemistry George Washington University 725 21st Street, NW Washington, DC 20052 ; _publ_contact_author_email cahill@gwu.edu _publ_contact_author_phone 202-994-6959 _publ_contact_author_fax 202-994-5873 _publ_section_title ; Syntheses, Structures and Fluorescent Properties of Two Novel Coordination Polymers in the U-Cu-H3pdc System ; loop_ _publ_author_name _publ_author_address M.Frisch ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 ; C.L.Cahill ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 AND Carnegie Insitution of Washington Geophysical Laboratory 5251 Broad Branch Road, NW Washington, DC 20015 ; data_03187 _database_code_depnum_ccdc_archive 'CCDC 259763' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 03187 _chemical_melting_point ? _chemical_formula_moiety 'C5 H4 N2 O7 U' _chemical_formula_sum 'C5 H4 N2 O7 U' _chemical_formula_weight 442.13 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' _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 6.9556(6) _cell_length_b 11.302(1) _cell_length_c 10.5288(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.057(2) _cell_angle_gamma 90.00 _cell_volume 827.7(1) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1023 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 19.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.511570 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8132 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2397 _reflns_number_gt 2276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _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^)+(0.0175P)^2^+8.3561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2397 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _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 0.25142(2) 0.148101(14) 0.322140(16) 0.00749(6) Uani 1 1 d . . . O1 O 0.3531(5) 0.1239(3) 0.4728(4) 0.0139(7) Uani 1 1 d . . . O2 O 0.1623(5) 0.1719(3) 0.1671(4) 0.0138(7) Uani 1 1 d . . . O3 O 0.0177(5) -0.0153(3) 0.3065(3) 0.0127(7) Uani 1 1 d . . . H3B H -0.0206 -0.0215 0.2301 0.019 Uiso 1 1 d R . . H3D H 0.0711 -0.0795 0.3293 0.019 Uiso 1 1 d R . . O4 O 0.3976(5) -0.0470(3) 0.2760(4) 0.0135(7) Uani 1 1 d . . . O5 O 0.5950(5) -0.1676(3) 0.1705(4) 0.0151(7) Uani 1 1 d . . . O6 O 0.9496(6) 0.3511(3) -0.0189(4) 0.0148(7) Uani 1 1 d . . . O7 O 1.0140(5) 0.1896(3) -0.1268(4) 0.0144(7) Uani 1 1 d . . . N1 N 0.5693(6) 0.1438(3) 0.1909(4) 0.0109(8) Uani 1 1 d . . . N2 N 0.6685(6) 0.2246(4) 0.1263(4) 0.0100(7) Uani 1 1 d . . . H2 H 0.6600 0.3013 0.1395 0.012 Uiso 1 1 calc R . . C1 C 0.5357(6) -0.0669(4) 0.1992(5) 0.0099(8) Uani 1 1 d . . . C2 C 0.6241(6) 0.0385(4) 0.1428(5) 0.0096(8) Uani 1 1 d . . . C3 C 0.7583(7) 0.0533(4) 0.0442(5) 0.0105(8) Uani 1 1 d . . . H3C H 0.8173 -0.0062 -0.0062 0.013 Uiso 1 1 calc R . . C4 C 0.7844(7) 0.1746(4) 0.0375(5) 0.0091(8) Uani 1 1 d . . . C5 C 0.9214(7) 0.2437(4) -0.0407(5) 0.0109(8) 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 U1 0.00665(9) 0.00576(9) 0.01007(9) -0.00006(6) 0.00091(6) 0.00006(6) O1 0.0148(17) 0.0147(17) 0.0123(17) 0.0020(14) -0.0057(13) -0.0007(14) O2 0.0125(16) 0.0156(17) 0.0134(17) 0.0020(14) -0.0051(13) 0.0020(14) O3 0.0152(17) 0.0112(16) 0.0118(16) -0.0020(13) 0.0020(13) -0.0036(13) O4 0.0114(15) 0.0098(16) 0.0193(18) 0.0010(14) 0.0075(14) -0.0007(13) O5 0.0126(16) 0.0081(16) 0.024(2) 0.0029(14) 0.0051(15) 0.0024(13) O6 0.0159(17) 0.0105(17) 0.0181(19) -0.0006(13) 0.0034(14) -0.0022(13) O7 0.0120(16) 0.0149(17) 0.0163(17) -0.0029(14) 0.0066(13) -0.0031(14) N1 0.0103(18) 0.0066(18) 0.016(2) 0.0007(15) 0.0041(15) 0.0007(14) N2 0.0100(18) 0.0055(17) 0.0146(19) 0.0000(14) 0.0050(15) 0.0003(14) C1 0.0067(18) 0.008(2) 0.016(2) 0.0001(17) 0.0006(16) 0.0011(16) C2 0.0063(19) 0.0044(19) 0.018(2) 0.0014(17) 0.0019(16) -0.0010(15) C3 0.0096(19) 0.009(2) 0.013(2) -0.0020(17) 0.0016(16) 0.0004(17) C4 0.009(2) 0.007(2) 0.011(2) 0.0015(16) 0.0008(16) 0.0003(16) C5 0.010(2) 0.012(2) 0.011(2) 0.0014(18) -0.0007(16) -0.0011(17) _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 O1 1.757(4) . ? U1 O2 1.766(4) . ? U1 O5 2.342(4) 2_655 ? U1 O3 2.465(3) . ? U1 O4 2.477(4) . ? U1 O7 2.526(4) 4_466 ? U1 N1 2.608(4) . ? U1 O6 2.686(4) 4_466 ? U1 C5 2.976(5) 4_466 ? O3 H3B 0.8497 . ? O3 H3D 0.8499 . ? O4 C1 1.276(6) . ? O5 C1 1.248(6) . ? O5 U1 2.342(4) 2_645 ? O6 C5 1.251(6) . ? O6 U1 2.686(4) 4_665 ? O7 C5 1.270(6) . ? O7 U1 2.526(4) 4_665 ? N1 N2 1.333(6) . ? N1 C2 1.349(6) . ? N2 C4 1.358(6) . ? N2 H2 0.8800 . ? C1 C2 1.466(6) . ? C2 C3 1.407(6) . ? C3 C4 1.385(6) . ? C3 H3C 0.9500 . ? C4 C5 1.482(6) . ? C5 U1 2.976(5) 4_665 ? 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 O1 U1 O2 176.80(17) . . ? O1 U1 O5 85.72(16) . 2_655 ? O2 U1 O5 93.14(16) . 2_655 ? O1 U1 O3 102.04(15) . . ? O2 U1 O3 79.72(15) . . ? O5 U1 O3 165.68(13) 2_655 . ? O1 U1 O4 82.74(15) . . ? O2 U1 O4 95.63(15) . . ? O5 U1 O4 127.66(12) 2_655 . ? O3 U1 O4 65.85(12) . . ? O1 U1 O7 100.57(15) . 4_466 ? O2 U1 O7 81.79(15) . 4_466 ? O5 U1 O7 69.24(12) 2_655 4_466 ? O3 U1 O7 97.29(12) . 4_466 ? O4 U1 O7 163.10(12) . 4_466 ? O1 U1 N1 97.73(16) . . ? O2 U1 N1 79.06(16) . . ? O5 U1 N1 69.35(13) 2_655 . ? O3 U1 N1 120.65(12) . . ? O4 U1 N1 62.04(12) . . ? O7 U1 N1 132.91(12) 4_466 . ? O1 U1 O6 75.66(15) . 4_466 ? O2 U1 O6 107.54(15) . 4_466 ? O5 U1 O6 109.47(12) 2_655 4_466 ? O3 U1 O6 61.86(12) . 4_466 ? O4 U1 O6 116.52(11) . 4_466 ? O7 U1 O6 49.73(11) 4_466 4_466 ? N1 U1 O6 173.39(13) . 4_466 ? O1 U1 C5 86.31(16) . 4_466 ? O2 U1 C5 96.65(15) . 4_466 ? O5 U1 C5 88.30(13) 2_655 4_466 ? O3 U1 C5 80.30(13) . 4_466 ? O4 U1 C5 141.10(12) . 4_466 ? O7 U1 C5 25.00(13) 4_466 4_466 ? N1 U1 C5 156.80(13) . 4_466 ? O6 U1 C5 24.86(12) 4_466 4_466 ? U1 O3 H3B 109.3 . . ? U1 O3 H3D 109.5 . . ? H3B O3 H3D 109.5 . . ? C1 O4 U1 126.2(3) . . ? C1 O5 U1 162.6(4) . 2_645 ? C5 O6 U1 90.7(3) . 4_665 ? C5 O7 U1 97.8(3) . 4_665 ? N2 N1 C2 105.4(4) . . ? N2 N1 U1 134.2(3) . . ? C2 N1 U1 117.1(3) . . ? N1 N2 C4 112.0(4) . . ? N1 N2 H2 124.0 . . ? C4 N2 H2 124.0 . . ? O5 C1 O4 124.3(4) . . ? O5 C1 C2 120.3(4) . . ? O4 C1 C2 115.4(4) . . ? N1 C2 C3 111.1(4) . . ? N1 C2 C1 116.5(4) . . ? C3 C2 C1 132.4(4) . . ? C4 C3 C2 104.0(4) . . ? C4 C3 H3C 128.0 . . ? C2 C3 H3C 128.0 . . ? N2 C4 C3 107.4(4) . . ? N2 C4 C5 123.0(4) . . ? C3 C4 C5 129.4(4) . . ? O6 C5 O7 121.2(5) . . ? O6 C5 C4 120.7(4) . . ? O7 C5 C4 118.1(4) . . ? O6 C5 U1 64.5(3) . 4_665 ? O7 C5 U1 57.2(2) . 4_665 ? C4 C5 U1 169.3(3) . 4_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 U1 O4 C1 -113.3(4) . . . . ? O2 U1 O4 C1 63.9(4) . . . . ? O5 U1 O4 C1 -34.5(5) 2_655 . . . ? O3 U1 O4 C1 140.0(4) . . . . ? O7 U1 O4 C1 144.1(4) 4_466 . . . ? N1 U1 O4 C1 -10.6(4) . . . . ? O6 U1 O4 C1 176.7(4) 4_466 . . . ? C5 U1 O4 C1 171.8(4) 4_466 . . . ? O1 U1 N1 N2 -112.0(5) . . . . ? O2 U1 N1 N2 68.1(5) . . . . ? O5 U1 N1 N2 -29.6(4) 2_655 . . . ? O3 U1 N1 N2 139.0(4) . . . . ? O4 U1 N1 N2 170.5(5) . . . . ? O7 U1 N1 N2 0.3(6) 4_466 . . . ? O6 U1 N1 N2 -110.4(10) 4_466 . . . ? C5 U1 N1 N2 -13.2(7) 4_466 . . . ? O1 U1 N1 C2 91.7(4) . . . . ? O2 U1 N1 C2 -88.2(4) . . . . ? O5 U1 N1 C2 174.2(4) 2_655 . . . ? O3 U1 N1 C2 -17.2(4) . . . . ? O4 U1 N1 C2 14.2(3) . . . . ? O7 U1 N1 C2 -156.0(3) 4_466 . . . ? O6 U1 N1 C2 93.3(11) 4_466 . . . ? C5 U1 N1 C2 -169.5(3) 4_466 . . . ? C2 N1 N2 C4 0.4(6) . . . . ? U1 N1 N2 C4 -157.8(4) . . . . ? U1 O5 C1 O4 -76.4(12) 2_645 . . . ? U1 O5 C1 C2 104.2(11) 2_645 . . . ? U1 O4 C1 O5 -173.8(4) . . . . ? U1 O4 C1 C2 5.7(6) . . . . ? N2 N1 C2 C3 -1.1(6) . . . . ? U1 N1 C2 C3 161.5(3) . . . . ? N2 N1 C2 C1 179.6(4) . . . . ? U1 N1 C2 C1 -17.8(6) . . . . ? O5 C1 C2 N1 -171.6(5) . . . . ? O4 C1 C2 N1 8.9(7) . . . . ? O5 C1 C2 C3 9.2(8) . . . . ? O4 C1 C2 C3 -170.3(5) . . . . ? N1 C2 C3 C4 1.3(6) . . . . ? C1 C2 C3 C4 -179.5(5) . . . . ? N1 N2 C4 C3 0.4(6) . . . . ? N1 N2 C4 C5 -175.1(4) . . . . ? C2 C3 C4 N2 -1.0(5) . . . . ? C2 C3 C4 C5 174.1(5) . . . . ? U1 O6 C5 O7 -8.0(5) 4_665 . . . ? U1 O6 C5 C4 169.4(4) 4_665 . . . ? U1 O7 C5 O6 8.6(5) 4_665 . . . ? U1 O7 C5 C4 -168.8(4) 4_665 . . . ? N2 C4 C5 O6 7.2(7) . . . . ? C3 C4 C5 O6 -167.3(5) . . . . ? N2 C4 C5 O7 -175.4(5) . . . . ? C3 C4 C5 O7 10.2(8) . . . . ? N2 C4 C5 U1 123.4(17) . . . 4_665 ? C3 C4 C5 U1 -51(2) . . . 4_665 ? 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 O3 H3B O7 0.85 2.19 2.740(5) 122.3 3_655 O3 H3D O6 0.85 2.15 2.708(5) 123.0 2_645 N2 H2 O4 0.88 1.97 2.817(5) 160.2 2_655 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.729 _refine_diff_density_min -1.693 _refine_diff_density_rms 0.224 #===END data_sad2 _database_code_depnum_ccdc_archive 'CCDC 259764' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H4 Cu N4 O12 U' _chemical_formula_weight 673.74 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.1014(7) _cell_length_b 7.6067(11) _cell_length_c 10.2910(15) _cell_angle_alpha 72.380(3) _cell_angle_beta 86.796(3) _cell_angle_gamma 84.447(3) _cell_volume 378.67(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2862 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 30.44 _exptl_crystal_description blade _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 309 _exptl_absorpt_coefficient_mu 12.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.374 _exptl_absorpt_correction_T_max 0.615 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2510 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 30.44 _reflns_number_total 1502 _reflns_number_gt 1502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.05 (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0463P)^2^+0.5087P] 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 1502 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _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 0.0000 0.0000 0.0000 0.01700(10) Uani 1 2 d S . . Cu1 Cu -0.5000 0.0000 -0.5000 0.01785(17) Uani 1 2 d S . . O1 O 0.2451(8) -0.0308(6) 0.1220(4) 0.0249(8) Uani 1 1 d . . . O2 O 0.1718(8) 0.2604(6) -0.1338(4) 0.0262(8) Uani 1 1 d . . . O3 O 0.3118(9) 0.3986(6) -0.3467(5) 0.0292(9) Uani 1 1 d . . . O4 O -0.7391(8) 0.8088(6) -0.1075(4) 0.0236(8) Uani 1 1 d . . . O5 O -0.7311(8) 0.9685(5) -0.3293(4) 0.0207(7) Uani 1 1 d . . . C1 C 0.1596(9) 0.3858(7) -0.2482(5) 0.0174(9) Uani 1 1 d . . . C2 C -0.0669(10) 0.5316(7) -0.2638(5) 0.0166(8) Uani 1 1 d . . . C3 C -0.2646(10) 0.5656(7) -0.1747(5) 0.0189(9) Uani 1 1 d . . . H3 H -0.2940 0.4987 -0.0839 0.023 Uiso 1 1 calc R . . C4 C -0.4096(10) 0.7233(7) -0.2526(5) 0.0160(8) Uani 1 1 d . . . C5 C -0.6464(9) 0.8405(7) -0.2278(5) 0.0154(8) Uani 1 1 d . . . N1 N -0.3052(9) 0.7810(6) -0.3798(4) 0.0173(8) Uani 1 1 d . . . N2 N -0.0950(9) 0.6644(6) -0.3846(4) 0.0177(8) Uani 1 1 d . . . H2 H 0.0081 0.6726 -0.4549 0.021 Uiso 1 1 calc R . . OW1 O -0.2596(8) 1.2013(6) -0.4119(4) 0.0239(8) 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 U1 0.02005(14) 0.01644(13) 0.01177(14) -0.00214(9) 0.00030(9) 0.00464(8) Cu1 0.0197(4) 0.0166(4) 0.0122(4) 0.0002(3) 0.0024(3) 0.0065(3) O1 0.0263(18) 0.030(2) 0.0165(18) -0.0042(15) -0.0055(15) 0.0034(15) O2 0.0259(19) 0.0204(18) 0.025(2) 0.0014(16) 0.0031(16) 0.0074(15) O3 0.031(2) 0.027(2) 0.025(2) -0.0055(17) 0.0075(17) 0.0094(16) O4 0.031(2) 0.0236(18) 0.0146(17) -0.0061(14) 0.0074(15) 0.0031(15) O5 0.0203(16) 0.0217(17) 0.0160(17) -0.0015(14) 0.0021(13) 0.0043(13) C1 0.0150(19) 0.014(2) 0.021(2) -0.0034(17) 0.0007(17) 0.0023(16) C2 0.020(2) 0.0144(19) 0.014(2) -0.0045(17) 0.0019(17) 0.0035(16) C3 0.020(2) 0.017(2) 0.016(2) -0.0015(18) 0.0033(18) 0.0038(17) C4 0.019(2) 0.015(2) 0.012(2) -0.0022(16) 0.0017(16) 0.0033(16) C5 0.018(2) 0.0134(19) 0.014(2) -0.0040(16) 0.0027(17) -0.0001(15) N1 0.0204(18) 0.0148(17) 0.0134(19) -0.0018(14) 0.0002(15) 0.0058(15) N2 0.0208(19) 0.0143(18) 0.0143(19) -0.0020(15) 0.0043(15) 0.0062(15) OW1 0.0252(18) 0.0237(18) 0.0188(19) -0.0024(15) 0.0027(15) 0.0021(14) _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 O1 1.771(4) 2 ? U1 O1 1.771(4) . ? U1 O2 2.266(4) 2 ? U1 O2 2.266(4) . ? U1 O4 2.355(4) 2_465 ? U1 O4 2.355(4) 1_645 ? Cu1 N1 1.965(4) 2_464 ? Cu1 N1 1.965(4) 1_545 ? Cu1 O5 2.026(4) 1_545 ? Cu1 O5 2.026(4) 2_464 ? O2 C1 1.271(7) . ? O3 C1 1.228(7) . ? O4 C5 1.260(6) . ? O4 U1 2.355(4) 1_465 ? O5 C5 1.257(6) . ? O5 Cu1 2.026(4) 1_565 ? C1 C2 1.502(7) . ? C2 N2 1.349(6) . ? C2 C3 1.384(7) . ? C3 C4 1.393(7) . ? C4 N1 1.345(6) . ? C4 C5 1.488(6) . ? N1 N2 1.333(6) . ? N1 Cu1 1.965(4) 1_565 ? 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 O1 U1 O1 180.0(3) 2 . ? O1 U1 O2 90.88(18) 2 2 ? O1 U1 O2 89.12(18) . 2 ? O1 U1 O2 89.12(18) 2 . ? O1 U1 O2 90.88(18) . . ? O2 U1 O2 180.00(15) 2 . ? O1 U1 O4 90.66(17) 2 2_465 ? O1 U1 O4 89.34(17) . 2_465 ? O2 U1 O4 92.93(15) 2 2_465 ? O2 U1 O4 87.07(15) . 2_465 ? O1 U1 O4 89.34(17) 2 1_645 ? O1 U1 O4 90.66(17) . 1_645 ? O2 U1 O4 87.07(15) 2 1_645 ? O2 U1 O4 92.93(15) . 1_645 ? O4 U1 O4 180.0 2_465 1_645 ? N1 Cu1 N1 180.0(2) 2_464 1_545 ? N1 Cu1 O5 98.78(16) 2_464 1_545 ? N1 Cu1 O5 81.22(16) 1_545 1_545 ? N1 Cu1 O5 81.22(16) 2_464 2_464 ? N1 Cu1 O5 98.78(16) 1_545 2_464 ? O5 Cu1 O5 180.000(1) 1_545 2_464 ? C1 O2 U1 145.3(4) . . ? C5 O4 U1 131.2(3) . 1_465 ? C5 O5 Cu1 114.1(3) . 1_565 ? O3 C1 O2 126.8(5) . . ? O3 C1 C2 117.1(5) . . ? O2 C1 C2 116.1(4) . . ? N2 C2 C3 108.5(4) . . ? N2 C2 C1 118.7(4) . . ? C3 C2 C1 132.8(5) . . ? C2 C3 C4 103.9(4) . . ? N1 C4 C3 110.7(4) . . ? N1 C4 C5 114.0(4) . . ? C3 C4 C5 135.3(5) . . ? O5 C5 O4 125.5(5) . . ? O5 C5 C4 116.3(4) . . ? O4 C5 C4 118.1(5) . . ? N2 N1 C4 106.6(4) . . ? N2 N1 Cu1 139.4(3) . 1_565 ? C4 N1 Cu1 114.0(3) . 1_565 ? N1 N2 C2 110.4(4) . . ? 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 N2 H2 OW1 0.86 1.92 2.709(6) 151.7 2_574 _diffrn_measured_fraction_theta_max 0.652 _diffrn_reflns_theta_full 30.44 _diffrn_measured_fraction_theta_full 0.652 _refine_diff_density_max 1.474 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.186