Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Christopher L. Cahill' _publ_contact_author_address ; The George Washington University Department of Chemistry 725 21st Street NW Washington, DC 20052 United States of America ; _publ_contact_author_email cahill@gwu.edu _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_category EM #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Frisch, Mark' . ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 United States of America ; 'Cahill, Christopher L.' . ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 United States of America and Geophysical Laboratory Carnegie Institution of Washington Washington, DC 20015 United States of America ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, Structure, and Fluorescent Studies of Novel Uranium Coordination Polymers in the Pyridinedicarboxylic Acid System ; #========================================================================== data_p21onn _database_code_depnum_ccdc_archive 'CCDC 610438' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H3 N O6 U' _chemical_formula_sum 'C7 H3 N O6 U' _chemical_formula_weight 435.13 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5288(7) _cell_length_b 15.4692(15) _cell_length_c 9.5211(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.512(2) _cell_angle_gamma 90.00 _cell_volume 957.14(17) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1376 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.01 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.020 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 16.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.447 _exptl_absorpt_correction_T_max 0.712 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7207 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.01 _reflns_number_total 2102 _reflns_number_gt 1532 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0292P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2102 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.04666(6) 0.335450(19) 0.95875(4) 0.02424(12) Uani 1 1 d . . . N1 N -0.0084(12) 0.1778(4) 0.8616(7) 0.0253(17) Uani 1 1 d . . . C1 C 0.2231(16) 0.5262(5) 0.8671(10) 0.027(2) Uani 1 1 d . . . C2 C 0.2257(15) 0.2259(5) 0.7005(10) 0.025(2) Uani 1 1 d . . . C3 C 0.1171(15) 0.0640(5) 0.7207(9) 0.025(2) Uani 1 1 d . . . C4 C -0.0229(15) 0.0081(6) 0.7690(10) 0.033(2) Uani 1 1 d . . . H4 H -0.0269 -0.0492 0.7392 0.040 Uiso 1 1 calc R . . C5 C 0.1142(14) 0.1505(5) 0.7617(9) 0.024(2) Uani 1 1 d . . . C6 C -0.1579(16) 0.0366(6) 0.8618(11) 0.037(3) Uani 1 1 d . . . H6 H -0.2577 0.0001 0.8924 0.044 Uiso 1 1 calc R . . C7 C -0.1399(15) 0.1211(6) 0.9076(10) 0.031(2) Uani 1 1 d . . . H7 H -0.2248 0.1395 0.9748 0.037 Uiso 1 1 calc R . . O1 O 0.2682(11) 0.4531(4) 0.9207(7) 0.0356(17) Uani 1 1 d . . . O2 O 0.2314(11) 0.2938(4) 1.0866(7) 0.0392(18) Uani 1 1 d . . . O3 O -0.1376(10) 0.3736(4) 0.8287(7) 0.0346(16) Uani 1 1 d . . . O4 O -0.2217(10) 0.2800(4) 1.0790(7) 0.0331(17) Uani 1 1 d . . . O5 O -0.0552(10) 0.4349(4) 1.1269(7) 0.0317(16) Uani 1 1 d . . . O6 O 0.2450(11) 0.2930(4) 0.7726(7) 0.0426(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0321(2) 0.01663(16) 0.02573(19) 0.00092(16) 0.01164(15) 0.00060(17) N1 0.033(5) 0.026(4) 0.018(4) 0.006(3) 0.010(4) -0.002(4) C1 0.040(6) 0.018(4) 0.025(5) -0.010(4) 0.007(5) -0.009(4) C2 0.029(6) 0.022(4) 0.027(5) 0.002(4) 0.022(5) 0.004(4) C3 0.040(6) 0.023(5) 0.012(4) -0.001(4) 0.003(4) 0.001(4) C4 0.041(6) 0.025(5) 0.036(6) -0.007(4) 0.013(5) -0.008(5) C5 0.022(5) 0.029(5) 0.023(5) 0.005(4) 0.008(4) 0.000(4) C6 0.042(7) 0.027(5) 0.043(6) -0.005(5) 0.021(5) -0.015(5) C7 0.037(6) 0.028(5) 0.028(5) -0.006(4) 0.009(5) 0.001(4) O1 0.047(5) 0.019(3) 0.043(4) 0.006(3) 0.019(4) -0.004(3) O2 0.051(5) 0.030(4) 0.036(4) 0.002(3) 0.000(4) -0.003(3) O3 0.039(4) 0.028(3) 0.038(4) 0.003(3) 0.012(3) 0.000(3) O4 0.049(5) 0.024(3) 0.030(4) -0.007(3) 0.025(3) -0.011(3) O5 0.032(4) 0.020(3) 0.046(4) -0.008(3) 0.019(3) -0.001(3) O6 0.059(5) 0.024(3) 0.051(5) -0.010(3) 0.039(4) -0.009(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 O3 1.745(6) . ? U1 O2 1.752(6) . ? U1 O4 2.346(7) . ? U1 O5 2.362(6) . ? U1 O1 2.375(6) . ? U1 O6 2.385(7) . ? U1 N1 2.621(7) . ? N1 C7 1.331(11) . ? N1 C5 1.368(12) . ? C1 O5 1.256(11) 3_567 ? C1 O1 1.264(10) . ? C1 C3 1.516(13) 2_556 ? C2 O4 1.242(10) 4_665 ? C2 O6 1.244(10) . ? C2 C5 1.520(12) . ? C3 C4 1.369(12) . ? C3 C5 1.395(11) . ? C3 C1 1.516(13) 2_546 ? C4 C6 1.378(13) . ? C4 H4 0.9300 . ? C6 C7 1.380(12) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? O4 C2 1.242(10) 4_566 ? O5 C1 1.256(11) 3_567 ? 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 O3 U1 O2 178.1(3) . . ? O3 U1 O4 88.5(3) . . ? O2 U1 O4 91.3(3) . . ? O3 U1 O5 92.3(3) . . ? O2 U1 O5 89.4(3) . . ? O4 U1 O5 68.6(2) . . ? O3 U1 O1 91.2(3) . . ? O2 U1 O1 90.0(3) . . ? O4 U1 O1 148.1(2) . . ? O5 U1 O1 79.6(2) . . ? O3 U1 O6 87.2(3) . . ? O2 U1 O6 91.6(3) . . ? O4 U1 O6 138.3(2) . . ? O5 U1 O6 153.0(2) . . ? O1 U1 O6 73.5(2) . . ? O3 U1 N1 90.2(3) . . ? O2 U1 N1 88.0(3) . . ? O4 U1 N1 75.4(2) . . ? O5 U1 N1 143.9(2) . . ? O1 U1 N1 136.4(2) . . ? O6 U1 N1 63.1(2) . . ? C7 N1 C5 117.7(8) . . ? C7 N1 U1 124.6(6) . . ? C5 N1 U1 117.6(6) . . ? O5 C1 O1 125.5(10) 3_567 . ? O5 C1 C3 119.4(8) 3_567 2_556 ? O1 C1 C3 114.9(9) . 2_556 ? O4 C2 O6 123.6(8) 4_665 . ? O4 C2 C5 119.0(8) 4_665 . ? O6 C2 C5 117.1(8) . . ? C4 C3 C5 119.0(9) . . ? C4 C3 C1 117.3(8) . 2_546 ? C5 C3 C1 123.6(9) . 2_546 ? C3 C4 C6 120.1(9) . . ? C3 C4 H4 119.9 . . ? C6 C4 H4 119.9 . . ? N1 C5 C3 121.0(9) . . ? N1 C5 C2 111.3(7) . . ? C3 C5 C2 127.6(9) . . ? C4 C6 C7 117.7(10) . . ? C4 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? N1 C7 C6 124.0(10) . . ? N1 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? C1 O1 U1 128.7(6) . . ? C2 O4 U1 140.2(6) 4_566 . ? C1 O5 U1 130.3(6) 3_567 . ? C2 O6 U1 127.3(6) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.266 _refine_diff_density_min -2.059 _refine_diff_density_rms 0.297 #====================================================================== data_pca21 _database_code_depnum_ccdc_archive 'CCDC 610439' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H3 N O6 U' _chemical_formula_sum 'C7 H3 N O6 U' _chemical_formula_weight 435.13 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 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 13.4877(10) _cell_length_b 6.9699(5) _cell_length_c 9.4739(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 890.62(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2099 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 26.36 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 18.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.280 _exptl_absorpt_correction_T_max 0.482 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6335 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 28.01 _reflns_number_total 1994 _reflns_number_gt 1683 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0000P)^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 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 0.015(11) _refine_ls_number_reflns 1994 _refine_ls_number_parameters 136 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0398 _refine_ls_wR_factor_gt 0.0367 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _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 1.079619(12) 0.46240(3) -0.01857(7) 0.01932(7) Uani 1 1 d . . . O1 O 1.0838(4) 0.6274(10) 0.1221(6) 0.0335(15) Uani 1 1 d . . . O2 O 1.0793(4) 0.2950(9) -0.1559(5) 0.0438(15) Uani 1 1 d . . . O3 O 0.9848(4) 0.2424(7) 0.1139(5) 0.0334(13) Uani 1 1 d . . . O4 O 1.0915(5) 0.7097(12) -0.1838(8) 0.055(2) Uani 1 1 d . . . O5 O 1.2517(3) 0.5216(7) -0.0563(6) 0.043(2) Uani 1 1 d . . . O6 O 0.9107(3) 0.5543(7) -0.0577(4) 0.0279(15) Uani 1 1 d . . . N1 N 1.2045(4) 0.2192(9) 0.1002(6) 0.0246(14) Uani 1 1 d . . . C1 C 1.1809(5) 0.0734(12) 0.1790(8) 0.032(2) Uani 1 1 d . . . H1 H 1.1159 0.0634 0.2109 0.039 Uiso 1 1 calc R . . C2 C 1.2490(11) -0.0700(9) 0.2182(17) 0.027(2) Uani 1 1 d . . . H2 H 1.2306 -0.1681 0.2794 0.033 Uiso 1 1 calc R . . C3 C 1.3426(4) -0.0615(10) 0.1642(7) 0.0195(16) Uani 1 1 d . . . C4 C 1.3684(5) 0.0906(10) 0.0792(6) 0.0171(15) Uani 1 1 d . . . H4 H 1.4319 0.0993 0.0417 0.021 Uiso 1 1 calc R . . C5 C 1.2980(5) 0.2310(11) 0.0503(6) 0.0202(16) Uani 1 1 d . . . C6 C 0.9181(5) 0.2104(10) 0.2017(8) 0.0254(16) Uani 1 1 d . . . C7 C 0.8228(4) 0.5899(9) -0.0260(16) 0.0209(15) 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 0.01101(10) 0.02086(12) 0.02609(11) 0.0015(5) 0.0008(5) 0.00035(9) O1 0.032(3) 0.034(4) 0.034(4) -0.011(3) -0.007(2) -0.008(3) O2 0.045(4) 0.054(4) 0.032(3) -0.018(3) -0.002(3) 0.014(3) O3 0.022(3) 0.031(4) 0.047(3) 0.012(3) 0.008(2) -0.003(2) O4 0.025(3) 0.064(6) 0.075(5) 0.055(4) -0.006(3) -0.014(3) O5 0.019(2) 0.033(3) 0.076(6) 0.031(3) 0.007(2) 0.003(2) O6 0.011(2) 0.031(3) 0.042(4) -0.008(2) 0.0026(18) 0.002(2) N1 0.015(3) 0.025(4) 0.034(4) 0.006(3) -0.001(2) 0.000(2) C1 0.010(3) 0.037(6) 0.050(5) 0.009(4) 0.002(3) 0.005(3) C2 0.025(3) 0.027(4) 0.029(6) 0.008(5) 0.006(3) -0.014(6) C3 0.017(3) 0.025(5) 0.016(3) -0.005(3) -0.005(2) -0.007(3) C4 0.012(3) 0.021(5) 0.018(3) -0.002(3) 0.001(2) 0.001(3) C5 0.011(3) 0.026(5) 0.023(4) 0.004(3) -0.003(3) -0.001(3) C6 0.019(4) 0.017(4) 0.040(4) -0.005(3) -0.004(3) 0.002(3) C7 0.017(3) 0.020(3) 0.026(4) -0.008(6) -0.003(5) -0.001(2) _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 1.748(5) . yes U1 O1 1.761(6) . yes U1 O4 2.334(6) . yes U1 O3 2.358(5) . yes U1 O5 2.385(5) . yes U1 O6 2.395(4) . yes U1 N1 2.641(6) . yes O3 C6 1.245(8) . ? O4 C6 1.227(9) 2_764 ? O5 C7 1.268(7) 3_565 ? O6 C7 1.248(7) . ? N1 C1 1.301(9) . ? N1 C5 1.350(8) . ? C1 C2 1.408(14) . ? C1 H1 0.9300 . ? C2 C3 1.364(16) . ? C2 H2 0.9300 . ? C3 C4 1.376(9) . ? C3 C6 1.496(9) 3 ? C4 C5 1.390(9) . ? C4 H4 0.9300 . ? C5 C7 1.481(11) 3_565 ? C6 O4 1.227(9) 2_765 ? C6 C3 1.496(9) 3_455 ? C7 O5 1.268(7) 3_465 ? C7 C5 1.481(11) 3_465 ? 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 178.0(3) . . yes O2 U1 O4 89.6(3) . . ? O1 U1 O4 91.3(2) . . ? O2 U1 O3 87.7(2) . . ? O1 U1 O3 92.3(3) . . ? O4 U1 O3 151.0(2) . . ? O2 U1 O5 90.4(2) . . ? O1 U1 O5 88.2(2) . . ? O4 U1 O5 72.8(2) . . ? O3 U1 O5 136.08(17) . . ? O2 U1 O6 93.5(2) . . ? O1 U1 O6 88.5(2) . . ? O4 U1 O6 76.36(19) . . yes O3 U1 O6 74.95(16) . . yes O5 U1 O6 148.90(16) . . ? O2 U1 N1 83.7(2) . . ? O1 U1 N1 94.4(2) . . ? O4 U1 N1 135.7(2) . . ? O3 U1 N1 72.66(17) . . ? O5 U1 N1 63.53(17) . . yes O6 U1 N1 147.57(16) . . ? C6 O3 U1 149.7(5) . . ? C6 O4 U1 157.1(7) 2_764 . ? C7 O5 U1 126.6(5) 3_565 . ? C7 O6 U1 156.8(7) . . ? C1 N1 C5 118.5(6) . . ? C1 N1 U1 126.1(4) . . ? C5 N1 U1 114.1(4) . . ? N1 C1 C2 123.1(8) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.3(10) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.1(7) . . ? C2 C3 C6 120.7(7) . 3 ? C4 C3 C6 120.1(6) . 3 ? C3 C4 C5 119.1(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.7(6) . . ? N1 C5 C7 115.7(6) . 3_565 ? C4 C5 C7 122.4(6) . 3_565 ? O4 C6 O3 125.9(7) 2_765 . ? O4 C6 C3 116.9(7) 2_765 3_455 ? O3 C6 C3 117.2(6) . 3_455 ? O6 C7 O5 122.8(8) . 3_465 ? O6 C7 C5 120.0(6) . 3_465 ? O5 C7 C5 117.2(6) 3_465 3_465 ? _refine_diff_density_max 0.770 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.159 #====================================================================== data_p212121 _database_code_depnum_ccdc_archive 'CCDC 610440' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H3 N O6 U' _chemical_formula_sum 'C7 H3 N O6 U' _chemical_formula_weight 435.13 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 orthorhombic _symmetry_space_group_name_H-M 'P 212121' 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' _cell_length_a 5.5685(4) _cell_length_b 8.4635(5) _cell_length_c 19.7227(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 929.51(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4052 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.92 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 17.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.296 _exptl_absorpt_correction_T_max 0.497 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7093 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.92 _reflns_number_total 2037 _reflns_number_gt 1940 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0352P)^2^+2.4724P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(6) _refine_ls_number_reflns 2037 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _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 0.46057(5) 0.24132(3) 0.127013(11) 0.01730(9) Uani 1 1 d . . . N1 N 0.2326(12) 0.4995(7) 0.1243(3) 0.0200(11) Uani 1 1 d . . . O1 O 0.1987(12) 0.1364(7) 0.1480(3) 0.0327(14) Uani 1 1 d . . . O2 O 0.7823(11) 0.6447(6) 0.6094(3) 0.0286(13) Uani 1 1 d . . . O3 O 0.4240(13) 0.3817(7) 0.2336(2) 0.0328(14) Uani 1 1 d . . . O4 O 0.3196(12) 0.5881(7) 0.2968(2) 0.0294(14) Uani 1 1 d . . . O5 O 0.2855(12) 0.3169(6) 0.0219(3) 0.0314(14) Uani 1 1 d . . . O6 O 0.0619(11) 0.4663(6) -0.0469(2) 0.0251(12) Uani 1 1 d . . . C1 C 0.3301(16) 0.5150(9) 0.2409(3) 0.0236(17) Uani 1 1 d . . . C2 C 0.2091(16) 0.5884(9) 0.1802(3) 0.0221(16) Uani 1 1 d . . . C3 C 0.0887(18) 0.7291(10) 0.1806(4) 0.038(2) Uani 1 1 d . . . H3 H 0.0801 0.7871 0.2205 0.046 Uiso 1 1 calc R . . C4 C -0.020(2) 0.7865(11) 0.1232(5) 0.052(3) Uani 1 1 d . . . H4 H -0.1024 0.8819 0.1227 0.062 Uiso 1 1 calc R . . C5 C 0.0034(19) 0.6887(9) 0.0633(4) 0.036(2) Uani 1 1 d . . . H5 H -0.0672 0.7200 0.0227 0.043 Uiso 1 1 calc R . . C6 C 0.1280(15) 0.5518(8) 0.0666(3) 0.0211(15) Uani 1 1 d . . . C7 C 0.1620(17) 0.4365(9) 0.0089(3) 0.0239(18) 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 0.02209(15) 0.01690(12) 0.01293(12) 0.00020(10) 0.00040(9) 0.00051(11) N1 0.022(3) 0.020(2) 0.018(3) -0.003(2) -0.002(3) -0.002(2) O1 0.031(4) 0.030(3) 0.036(3) -0.003(2) 0.005(3) -0.005(3) O2 0.032(3) 0.028(3) 0.027(3) -0.005(2) -0.004(2) -0.010(2) O3 0.048(4) 0.033(3) 0.017(2) -0.002(2) -0.004(3) 0.004(3) O4 0.039(4) 0.033(3) 0.016(2) -0.008(2) 0.002(2) -0.011(3) O5 0.049(4) 0.028(3) 0.017(2) -0.007(2) -0.006(3) 0.012(3) O6 0.034(4) 0.023(3) 0.018(2) 0.0017(19) -0.008(2) -0.004(3) C1 0.025(5) 0.029(4) 0.017(3) -0.007(3) -0.002(3) -0.001(3) C2 0.022(4) 0.023(4) 0.021(3) -0.006(3) -0.002(3) -0.001(3) C3 0.050(6) 0.032(4) 0.033(4) -0.014(4) -0.011(4) 0.011(5) C4 0.062(7) 0.040(5) 0.054(6) -0.019(4) 0.000(6) 0.024(5) C5 0.049(7) 0.028(4) 0.030(4) -0.007(3) -0.016(4) 0.005(4) C6 0.024(4) 0.017(3) 0.022(3) -0.004(3) -0.005(3) -0.001(3) C7 0.033(5) 0.023(4) 0.017(3) -0.002(3) -0.004(3) -0.003(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 O1 1.757(6) . ? U1 O2 1.761(6) 2_664 ? U1 O4 2.332(5) 3_645 ? U1 O5 2.379(5) . ? U1 O3 2.423(5) . ? U1 O6 2.429(5) 4 ? U1 N1 2.528(6) . ? N1 C2 1.341(9) . ? N1 C6 1.353(9) . ? O2 U1 1.761(6) 2_665 ? O3 C1 1.252(9) . ? O4 C1 1.266(8) . ? O4 U1 2.332(5) 3_655 ? O5 C7 1.251(10) . ? O6 C7 1.258(8) . ? O6 U1 2.429(5) 4_455 ? C1 C2 1.508(10) . ? C2 C3 1.366(11) . ? C3 C4 1.372(13) . ? C3 H3 0.9300 . ? C4 C5 1.447(11) . ? C4 H4 0.9300 . ? C5 C6 1.352(11) . ? C5 H5 0.9300 . ? C6 C7 1.512(10) . ? 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 176.6(2) . 2_664 ? O1 U1 O4 90.2(3) . 3_645 ? O2 U1 O4 90.3(2) 2_664 3_645 ? O1 U1 O5 90.1(3) . . ? O2 U1 O5 90.8(2) 2_664 . ? O4 U1 O5 157.86(18) 3_645 . ? O1 U1 O3 88.5(2) . . ? O2 U1 O3 88.3(2) 2_664 . ? O4 U1 O3 75.97(18) 3_645 . ? O5 U1 O3 126.17(18) . . ? O1 U1 O6 88.9(2) . 4 ? O2 U1 O6 94.5(2) 2_664 4 ? O4 U1 O6 83.97(18) 3_645 4 ? O5 U1 O6 73.89(18) . 4 ? O3 U1 O6 159.76(18) . 4 ? O1 U1 N1 91.4(3) . . ? O2 U1 N1 86.0(2) 2_664 . ? O4 U1 N1 139.29(18) 3_645 . ? O5 U1 N1 62.84(18) . . ? O3 U1 N1 63.41(19) . . ? O6 U1 N1 136.73(18) 4 . ? C2 N1 C6 117.7(7) . . ? C2 N1 U1 121.1(5) . . ? C6 N1 U1 121.1(5) . . ? C1 O3 U1 125.2(5) . . ? C1 O4 U1 144.0(6) . 3_655 ? C7 O5 U1 128.5(5) . . ? C7 O6 U1 121.8(5) . 4_455 ? O3 C1 O4 124.0(7) . . ? O3 C1 C2 117.8(6) . . ? O4 C1 C2 118.0(7) . . ? N1 C2 C3 122.8(7) . . ? N1 C2 C1 112.2(7) . . ? C3 C2 C1 125.0(7) . . ? C2 C3 C4 121.3(7) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C3 C4 C5 115.6(8) . . ? C3 C4 H4 122.2 . . ? C5 C4 H4 122.2 . . ? C6 C5 C4 119.8(8) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 N1 122.8(7) . . ? C5 C6 C7 125.5(7) . . ? N1 C6 C7 111.6(6) . . ? O5 C7 O6 125.8(7) . . ? O5 C7 C6 115.9(6) . . ? O6 C7 C6 118.3(7) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.078 _refine_diff_density_min -2.307 _refine_diff_density_rms 0.259 #====================================================================== data_pbar1 _database_code_depnum_ccdc_archive 'CCDC 610441' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H3 N O10 U2' _chemical_formula_sum 'C7 H3 N O10 U2' _chemical_formula_weight 737.16 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7478(10) _cell_length_b 9.1757(11) _cell_length_c 9.3460(12) _cell_angle_alpha 86.151(2) _cell_angle_beta 71.627(2) _cell_angle_gamma 77.395(2) _cell_volume 615.35(13) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3348 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.11 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 26.335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.092 _exptl_absorpt_correction_T_max 0.591 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _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 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11904 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 30.11 _reflns_number_total 3336 _reflns_number_gt 2209 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. The water molecule, O8, which is bound to U1, was left as isotropic. When it is taken anisotropic, O8 becomes a non-positive definite. Atoms O1, N1, C3 and C7 have large ADP max/min ratios which are probably due to static disorder of the 2,6-pydc organic side chains. ; _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^)+(0.0305P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3336 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 0.28490(6) 0.95934(5) 0.13822(5) 0.00912(14) Uani 1 1 d . . . U2 U 0.72281(6) 0.63879(5) 0.07009(5) 0.00891(13) Uani 1 1 d . . . O1 O 0.1523(11) 0.6455(10) 0.4165(10) 0.016(2) Uani 1 1 d . . . O2 O 0.5898(12) 0.8606(9) 0.0144(10) 0.014(2) Uani 1 1 d . . . O3 O 0.7936(12) 0.7165(10) 0.2084(10) 0.016(2) Uani 1 1 d . . . O4 O 0.3935(11) 0.6961(9) 0.2249(9) 0.0115(13) Uani 1 1 d . . . O5 O 0.9503(12) 0.4009(9) 0.0875(9) 0.0115(13) Uani 1 1 d . . . O6 O 0.6739(12) 0.5518(10) -0.0735(10) 0.014(2) Uani 1 1 d . . . O7 O 0.3366(12) 1.0123(10) 0.2958(10) 0.015(2) Uani 1 1 d . . . O9 O 0.2164(12) 0.8991(9) -0.0064(10) 0.013(2) Uani 1 1 d . . . O10 O 0.0374(13) 1.1819(9) 0.1824(11) 0.019(2) Uani 1 1 d . . . N1 N 0.6064(13) 0.4397(11) 0.2621(11) 0.009(2) Uani 1 1 d . . . C1 C 0.3114(19) 0.6145(14) 0.3305(14) 0.012(2) Uani 1 1 d . . . C2 C 0.9136(19) 0.2951(13) 0.1774(14) 0.012(2) Uani 1 1 d . . . C3 C 0.3543(18) 0.3555(13) 0.4503(14) 0.0137(19) Uani 1 1 d . . . H3 H 0.2295 0.3747 0.5077 0.016 Uiso 1 1 calc R . . C4 C 0.4712(17) 0.2217(13) 0.4630(14) 0.0116(19) Uani 1 1 d . . . H4 H 0.4244 0.1484 0.5280 0.014 Uiso 1 1 calc R . . C5 C 0.7175(16) 0.3075(13) 0.2764(13) 0.007(2) Uani 1 1 d . . . C6 C 0.4290(17) 0.4614(13) 0.3487(14) 0.0116(19) Uani 1 1 d . . . C7 C 0.6596(18) 0.1955(14) 0.3787(13) 0.0137(19) Uani 1 1 d . . . H7 H 0.7422 0.1085 0.3898 0.016 Uiso 1 1 calc R . . O8 O -0.0052(12) 0.8859(9) 0.3074(10) 0.0138(19) Uiso 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 0.0093(3) 0.0046(2) 0.0119(3) 0.0000(2) -0.0027(2) 0.0010(2) U2 0.0088(3) 0.0046(2) 0.0111(3) 0.00017(19) -0.0017(2) 0.00105(19) O1 0.004(4) 0.015(5) 0.020(5) 0.000(4) 0.005(4) 0.003(4) O2 0.020(5) 0.010(4) 0.016(5) 0.000(4) -0.008(4) -0.004(4) O3 0.016(5) 0.014(5) 0.018(5) -0.003(4) -0.004(4) 0.000(4) O4 0.011(3) 0.004(3) 0.015(3) 0.000(2) 0.000(3) 0.001(2) O5 0.011(3) 0.004(3) 0.015(3) 0.000(2) 0.000(3) 0.001(2) O6 0.017(5) 0.016(5) 0.016(5) 0.001(4) -0.011(4) -0.007(4) O7 0.009(5) 0.019(5) 0.013(5) 0.001(4) 0.001(4) 0.000(4) O9 0.016(5) 0.010(4) 0.015(5) -0.001(4) -0.009(4) 0.003(4) O10 0.017(5) 0.008(5) 0.030(6) 0.009(4) -0.007(4) -0.002(4) N1 0.004(5) 0.006(5) 0.010(5) 0.001(4) 0.003(4) 0.003(4) C1 0.021(5) 0.006(4) 0.010(5) 0.002(4) -0.009(4) 0.000(4) C2 0.021(5) 0.006(4) 0.010(5) 0.002(4) -0.009(4) 0.000(4) C3 0.018(5) 0.010(4) 0.008(4) -0.007(3) -0.001(4) 0.005(4) C4 0.013(5) 0.008(4) 0.012(5) -0.004(3) -0.003(4) 0.001(4) C5 0.006(6) 0.006(6) 0.008(6) -0.003(5) -0.001(5) 0.003(5) C6 0.013(5) 0.008(4) 0.012(5) -0.004(3) -0.003(4) 0.001(4) C7 0.018(5) 0.010(4) 0.008(4) -0.007(3) -0.001(4) 0.005(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 U1 O9 1.760(9) . ? U1 O7 1.766(9) . ? U1 O2 2.284(9) 2_675 ? U1 O2 2.286(9) . ? U1 O10 2.434(9) . ? U1 O8 2.507(9) . ? U1 O4 2.545(8) . ? U1 U1 3.7067(10) 2_675 ? U1 U2 3.8862(7) . ? U1 U2 4.0503(7) 2_675 ? U2 O6 1.783(8) . ? U2 O3 1.794(9) . ? U2 O2 2.181(8) . ? U2 O5 2.456(8) 2_765 ? U2 O4 2.464(8) . ? U2 O5 2.520(8) . ? U2 N1 2.575(10) . ? U2 U1 4.0503(7) 2_675 ? O1 C1 1.225(15) . ? O2 U1 2.284(9) 2_675 ? O4 C1 1.286(14) . ? O5 C2 1.260(14) . ? O5 U2 2.456(8) 2_765 ? O10 C2 1.260(14) 1_465 ? N1 C6 1.336(15) . ? N1 C5 1.351(14) . ? C1 C6 1.529(17) . ? C2 O10 1.260(14) 1_645 ? C2 C5 1.494(18) . ? C3 C4 1.380(16) . ? C3 C6 1.399(17) . ? C3 H3 0.9300 . ? C4 C7 1.399(17) . ? C4 H4 0.9300 . ? C5 C7 1.404(17) . ? C7 H7 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 O9 U1 O7 174.5(4) . . ? O9 U1 O2 91.2(4) . 2_675 ? O7 U1 O2 93.9(4) . 2_675 ? O9 U1 O2 90.8(4) . . ? O7 U1 O2 92.9(4) . . ? O2 U1 O2 71.6(3) 2_675 . ? O9 U1 O10 91.7(4) . . ? O7 U1 O10 87.5(4) . . ? O2 U1 O10 74.3(3) 2_675 . ? O2 U1 O10 145.8(3) . . ? O9 U1 O8 83.8(4) . . ? O7 U1 O8 90.7(3) . . ? O2 U1 O8 146.4(3) 2_675 . ? O2 U1 O8 141.4(3) . . ? O10 U1 O8 72.7(3) . . ? O9 U1 O4 94.3(3) . . ? O7 U1 O4 83.4(3) . . ? O2 U1 O4 138.4(3) 2_675 . ? O2 U1 O4 67.1(3) . . ? O10 U1 O4 146.5(3) . . ? O8 U1 O4 75.2(3) . . ? O9 U1 U1 91.2(3) . 2_675 ? O7 U1 U1 94.2(3) . 2_675 ? O2 U1 U1 35.8(2) 2_675 2_675 ? O2 U1 U1 35.8(2) . 2_675 ? O10 U1 U1 110.1(2) . 2_675 ? O8 U1 U1 174.45(19) . 2_675 ? O4 U1 U1 102.77(19) . 2_675 ? O9 U1 U2 93.6(3) . . ? O7 U1 U2 87.7(3) . . ? O2 U1 U2 100.2(2) 2_675 . ? O2 U1 U2 28.8(2) . . ? O10 U1 U2 172.4(2) . . ? O8 U1 U2 113.3(2) . . ? O4 U1 U2 38.36(18) . . ? U1 U1 U2 64.425(16) 2_675 . ? O9 U1 U2 87.6(3) . 2_675 ? O7 U1 U2 96.1(3) . 2_675 ? O2 U1 U2 24.3(2) 2_675 2_675 ? O2 U1 U2 95.7(2) . 2_675 ? O10 U1 U2 50.5(2) . 2_675 ? O8 U1 U2 122.1(2) . 2_675 ? O4 U1 U2 162.67(19) . 2_675 ? U1 U1 U2 59.936(14) 2_675 2_675 ? U2 U1 U2 124.361(14) . 2_675 ? O6 U2 O3 174.7(4) . . ? O6 U2 O2 92.7(4) . . ? O3 U2 O2 90.9(4) . . ? O6 U2 O5 88.5(4) . 2_765 ? O3 U2 O5 86.7(3) . 2_765 ? O2 U2 O5 106.3(3) . 2_765 ? O6 U2 O4 92.8(4) . . ? O3 U2 O4 92.1(3) . . ? O2 U2 O4 70.1(3) . . ? O5 U2 O4 176.3(3) 2_765 . ? O6 U2 O5 88.1(3) . . ? O3 U2 O5 87.5(3) . . ? O2 U2 O5 165.2(3) . . ? O5 U2 O5 58.9(3) 2_765 . ? O4 U2 O5 124.6(3) . . ? O6 U2 N1 90.8(4) . . ? O3 U2 N1 89.6(4) . . ? O2 U2 N1 133.1(3) . . ? O5 U2 N1 120.5(3) 2_765 . ? O4 U2 N1 63.0(3) . . ? O5 U2 N1 61.6(3) . . ? O6 U2 U1 94.2(3) . . ? O3 U2 U1 90.9(3) . . ? O2 U2 U1 30.3(2) . . ? O5 U2 U1 136.54(19) 2_765 . ? O4 U2 U1 39.87(18) . . ? O5 U2 U1 164.34(19) . . ? N1 U2 U1 102.8(2) . . ? O6 U2 U1 94.5(3) . 2_675 ? O3 U2 U1 87.0(3) . 2_675 ? O2 U2 U1 25.5(2) . 2_675 ? O5 U2 U1 80.90(19) 2_765 2_675 ? O4 U2 U1 95.49(18) . 2_675 ? O5 U2 U1 139.69(19) . 2_675 ? N1 U2 U1 158.1(2) . 2_675 ? U1 U2 U1 55.639(14) . 2_675 ? U2 O2 U1 130.2(4) . 2_675 ? U2 O2 U1 120.9(4) . . ? U1 O2 U1 108.4(3) 2_675 . ? C1 O4 U2 126.4(8) . . ? C1 O4 U1 131.5(8) . . ? U2 O4 U1 101.8(3) . . ? C2 O5 U2 113.6(8) . 2_765 ? C2 O5 U2 125.3(8) . . ? U2 O5 U2 121.1(3) 2_765 . ? C2 O10 U1 168.5(9) 1_465 . ? C6 N1 C5 117.0(10) . . ? C6 N1 U2 120.6(8) . . ? C5 N1 U2 122.3(7) . . ? O1 C1 O4 127.6(12) . . ? O1 C1 C6 117.3(11) . . ? O4 C1 C6 115.1(11) . . ? O10 C2 O5 121.3(12) 1_645 . ? O10 C2 C5 121.1(11) 1_645 . ? O5 C2 C5 117.7(11) . . ? C4 C3 C6 118.1(12) . . ? C4 C3 H3 121.0 . . ? C6 C3 H3 121.0 . . ? C3 C4 C7 120.4(12) . . ? C3 C4 H4 119.8 . . ? C7 C4 H4 119.8 . . ? N1 C5 C7 124.3(11) . . ? N1 C5 C2 112.9(10) . . ? C7 C5 C2 122.7(11) . . ? N1 C6 C3 123.7(11) . . ? N1 C6 C1 114.6(11) . . ? C3 C6 C1 121.7(11) . . ? C4 C7 C5 116.4(12) . . ? C4 C7 H7 121.8 . . ? C5 C7 H7 121.8 . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.790 _refine_diff_density_min -2.316 _refine_diff_density_rms 0.494 #====================================================================== data_c2onm _database_code_depnum_ccdc_archive 'CCDC 610442' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Cu N2 O18.5 U' _chemical_formula_sum 'C14 H6 Cu N2 O18.5 U' _chemical_formula_weight 800.11 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 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.888(3) _cell_length_b 7.0906(17) _cell_length_c 10.944(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.525(3) _cell_angle_gamma 90.00 _cell_volume 1147.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 548 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 28.01 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 8.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _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 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4436 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.01 _reflns_number_total 1399 _reflns_number_gt 1122 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0313P)^2^+2.1558P] 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 1399 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.0322(2) Uani 1 4 d S . . Cu1 Cu 0.0000 0.0000 0.5000 0.0359(5) Uani 1 4 d S . . O1 O 0.0000 -0.2479(11) 0.0000 0.044(2) Uani 1 2 d S . . O2 O -0.1290(4) 0.0000 -0.1670(6) 0.047(2) Uani 1 2 d S . . O3 O -0.2741(5) 0.0000 -0.2490(6) 0.051(2) Uani 1 2 d S . . O4 O -0.0282(5) 0.0000 0.2126(6) 0.063(3) Uani 1 2 d S . . O5 O -0.1067(4) 0.0000 0.3750(6) 0.042(2) Uani 1 2 d S . . O6A O -0.0612(16) -0.216(3) -0.417(2) 0.095(5) Uani 0.76(4) 1 d P . 1 O6B O -0.097(2) -0.217(5) -0.388(2) 0.051(9) Uani 0.37(6) 1 d P . 2 O7 O -0.2540(9) -0.144(2) 0.5235(12) 0.088(5) Uani 0.50 1 d P . . O8 O -0.4665(6) 0.0000 0.6909(9) 0.075(3) Uani 1 2 d S . . N1 N -0.1689(5) 0.0000 0.0554(7) 0.029(2) Uani 1 2 d S . . C1 C -0.2395(6) 0.0000 -0.0328(9) 0.028(2) Uani 1 2 d S . . C2 C -0.3266(6) 0.0000 -0.0015(9) 0.032(3) Uani 1 2 d S . . H2 H -0.3750 0.0000 -0.0632 0.038 Uiso 1 2 calc SR . . C3 C -0.3430(6) 0.0000 0.1194(10) 0.042(3) Uani 1 2 d S . . H3 H -0.4018 0.0000 0.1404 0.050 Uiso 1 2 calc SR . . C4 C -0.2704(7) 0.0000 0.2083(9) 0.040(3) Uani 1 2 d S . . H4 H -0.2789 0.0000 0.2911 0.048 Uiso 1 2 calc SR . . C5 C -0.1851(7) 0.0000 0.1733(9) 0.032(3) Uani 1 2 d S . . C6 C -0.2136(7) 0.0000 -0.1598(9) 0.035(3) Uani 1 2 d S . . C7 C -0.0995(7) 0.0000 0.2626(9) 0.035(3) Uani 1 2 d S . . 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 0.0207(3) 0.0539(5) 0.0212(3) 0.000 -0.0015(2) 0.000 Cu1 0.0255(9) 0.0576(15) 0.0236(9) 0.000 -0.0016(7) 0.000 O1 0.037(4) 0.043(6) 0.048(5) 0.000 -0.011(3) 0.000 O2 0.024(4) 0.094(7) 0.024(4) 0.000 -0.002(3) 0.000 O3 0.027(4) 0.094(7) 0.029(4) 0.000 -0.009(3) 0.000 O4 0.023(4) 0.140(9) 0.024(4) 0.000 -0.002(3) 0.000 O5 0.023(4) 0.082(6) 0.019(4) 0.000 -0.003(3) 0.000 O6A 0.062(10) 0.092(10) 0.127(14) 0.041(10) -0.012(9) -0.011(10) O6B 0.032(15) 0.081(16) 0.041(12) 0.015(10) 0.015(10) 0.005(13) O7 0.066(8) 0.148(15) 0.052(8) -0.007(9) 0.023(7) -0.013(10) O8 0.058(6) 0.063(7) 0.100(8) 0.000 -0.012(5) 0.000 N1 0.023(4) 0.034(6) 0.029(5) 0.000 -0.002(4) 0.000 C1 0.028(5) 0.031(7) 0.025(5) 0.000 0.006(4) 0.000 C2 0.021(5) 0.040(7) 0.032(6) 0.000 -0.009(4) 0.000 C3 0.016(5) 0.071(9) 0.038(6) 0.000 0.003(5) 0.000 C4 0.030(6) 0.072(9) 0.020(5) 0.000 0.007(5) 0.000 C5 0.029(5) 0.040(7) 0.025(5) 0.000 -0.002(4) 0.000 C6 0.032(6) 0.057(8) 0.017(5) 0.000 0.003(5) 0.000 C7 0.023(5) 0.052(8) 0.031(6) 0.000 0.000(5) 0.000 _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 1.758(8) 5 ? U1 O1 1.758(8) . ? U1 O4 2.411(7) . ? U1 O4 2.411(7) 5 ? U1 O2 2.496(7) 5 ? U1 O2 2.496(7) . ? U1 N1 2.653(8) . ? U1 N1 2.653(8) 5 ? Cu1 O5 1.975(6) . ? Cu1 O5 1.975(6) 5_556 ? Cu1 O6A 2.04(2) 6_556 ? Cu1 O6A 2.04(2) 1_556 ? Cu1 O6A 2.04(2) 5 ? Cu1 O6A 2.04(2) 2 ? O2 C6 1.271(11) . ? O3 C6 1.251(11) . ? O4 C7 1.248(11) . ? O5 C7 1.246(11) . ? O6A Cu1 2.04(2) 1_554 ? O7 O7 1.60(3) 7_446 ? N1 C5 1.339(11) . ? N1 C1 1.344(12) . ? C1 C2 1.378(13) . ? C1 C6 1.485(12) . ? C2 C3 1.372(13) . ? C2 H2 0.9300 . ? C3 C4 1.370(14) . ? C3 H3 0.9300 . ? C4 C5 1.367(13) . ? C4 H4 0.9300 . ? C5 C7 1.516(14) . ? 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 5 . ? O1 U1 O4 90.0 5 . ? O1 U1 O4 90.0 . . ? O1 U1 O4 90.0 5 5 ? O1 U1 O4 90.0 . 5 ? O4 U1 O4 180.0(3) . 5 ? O1 U1 O2 90.0 5 5 ? O1 U1 O2 90.0 . 5 ? O4 U1 O2 59.8(2) . 5 ? O4 U1 O2 120.2(2) 5 5 ? O1 U1 O2 90.0 5 . ? O1 U1 O2 90.0 . . ? O4 U1 O2 120.2(2) . . ? O4 U1 O2 59.8(2) 5 . ? O2 U1 O2 180.0(2) 5 . ? O1 U1 N1 90.0 5 . ? O1 U1 N1 90.0 . . ? O4 U1 N1 60.4(2) . . ? O4 U1 N1 119.6(2) 5 . ? O2 U1 N1 120.2(2) 5 . ? O2 U1 N1 59.8(2) . . ? O1 U1 N1 90.0 5 5 ? O1 U1 N1 90.0 . 5 ? O4 U1 N1 119.6(2) . 5 ? O4 U1 N1 60.4(2) 5 5 ? O2 U1 N1 59.8(2) 5 5 ? O2 U1 N1 120.2(2) . 5 ? N1 U1 N1 180.00(7) . 5 ? O5 Cu1 O5 180.000(1) . 5_556 ? O5 Cu1 O6A 86.7(5) . 6_556 ? O5 Cu1 O6A 93.3(5) 5_556 6_556 ? O5 Cu1 O6A 86.7(5) . 1_556 ? O5 Cu1 O6A 93.3(5) 5_556 1_556 ? O6A Cu1 O6A 96.9(18) 6_556 1_556 ? O5 Cu1 O6A 93.3(5) . 5 ? O5 Cu1 O6A 86.7(5) 5_556 5 ? O6A Cu1 O6A 83.1(18) 6_556 5 ? O6A Cu1 O6A 180.0(13) 1_556 5 ? O5 Cu1 O6A 93.3(5) . 2 ? O5 Cu1 O6A 86.7(5) 5_556 2 ? O6A Cu1 O6A 180.000(2) 6_556 2 ? O6A Cu1 O6A 83.1(18) 1_556 2 ? O6A Cu1 O6A 96.9(18) 5 2 ? C6 O2 U1 129.8(6) . . ? C7 O4 U1 132.4(7) . . ? C7 O5 Cu1 122.1(6) . . ? C5 N1 C1 118.7(8) . . ? C5 N1 U1 120.0(6) . . ? C1 N1 U1 121.3(6) . . ? N1 C1 C2 120.2(9) . . ? N1 C1 C6 114.0(8) . . ? C2 C1 C6 125.8(9) . . ? C3 C2 C1 121.0(9) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 118.1(9) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 119.0(9) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 123.0(9) . . ? N1 C5 C7 113.0(8) . . ? C4 C5 C7 124.0(9) . . ? O3 C6 O2 125.6(9) . . ? O3 C6 C1 119.3(9) . . ? O2 C6 C1 115.0(8) . . ? O5 C7 O4 127.3(10) . . ? O5 C7 C5 118.4(8) . . ? O4 C7 C5 114.3(9) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.850 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.216 #====================================================================== data_pbar1_2 _database_code_depnum_ccdc_archive 'CCDC 610443' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Ag2 N2 O10 U' _chemical_formula_sum 'C14 H6 Ag2 N2 O10 U' _chemical_formula_weight 815.98 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' Ag Ag -0.8971 1.1015 '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 8.4579(3) _cell_length_b 9.4393(4) _cell_length_c 11.8454(4) _cell_angle_alpha 72.7230(10) _cell_angle_beta 69.3170(10) _cell_angle_gamma 66.6810(10) _cell_volume 798.76(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3173 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 28.08 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 12.607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.777 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _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 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7549 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.08 _reflns_number_total 3453 _reflns_number_gt 3091 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0182P)^2^+2.8064P] 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 3453 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0542 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.61926(3) 0.27241(2) 0.823233(19) 0.00609(6) Uani 1 1 d . . . Ag1 Ag 0.12124(6) 0.61245(5) 0.91720(4) 0.01541(11) Uani 1 1 d . . . Ag2 Ag 1.00041(6) -0.12329(5) 0.71049(4) 0.01447(11) Uani 1 1 d . . . N1 N 0.6958(6) 0.4325(5) 0.6004(4) 0.0067(7) Uani 1 1 d . . . N2 N 0.5787(6) 0.1396(5) 1.0540(4) 0.0067(7) Uani 1 1 d . . . O1 O 0.1275(5) 0.3500(4) 1.1592(4) 0.0102(8) Uani 1 1 d . . . O2 O 0.8232(5) 0.0013(5) 0.8839(4) 0.0111(9) Uani 1 1 d . . . O3 O 0.3949(5) 0.5293(4) 0.7636(3) 0.0092(8) Uani 1 1 d . . . O4 O 0.9727(5) -0.1793(5) 1.0161(4) 0.0111(9) Uani 1 1 d . . . O5 O 0.8936(5) 0.1566(5) 0.6720(4) 0.0128(9) Uani 1 1 d . . . O6 O 0.3249(5) 0.3643(5) 0.9752(4) 0.0114(9) Uani 1 1 d . . . O7 O 0.5133(5) 0.1751(5) 0.7821(4) 0.0112(9) Uani 1 1 d . . . O8 O 0.7239(5) 0.3734(5) 0.8610(4) 0.0114(9) Uani 1 1 d . . . O9 O 1.2867(5) -0.2615(4) 0.6275(4) 0.0103(9) Uani 1 1 d . . . O10 O 1.0872(6) 0.1397(5) 0.4865(4) 0.0190(10) Uani 1 1 d . . . C1 C 0.7891(8) 0.6121(7) 0.3698(5) 0.0110(12) Uani 1 1 d . . . H1 H 0.8212 0.6720 0.2929 0.013 Uiso 1 1 calc R . . C2 C 0.6246(8) 0.6684(7) 0.4518(5) 0.0096(12) Uani 1 1 d . . . H2 H 0.5442 0.7664 0.4306 0.012 Uiso 1 1 calc R . . C3 C 0.8542(7) -0.0575(7) 0.9898(5) 0.0090(12) Uani 1 1 d . . . C4 C 0.9560(7) 0.2123(7) 0.5585(5) 0.0086(8) Uani 1 1 d . . . C5 C 0.4320(7) 0.1662(7) 1.2639(5) 0.0089(12) Uani 1 1 d . . . H5 H 0.3288 0.2078 1.3229 0.011 Uiso 1 1 calc R . . C6 C 0.8510(7) 0.3793(6) 0.5182(5) 0.0079(8) Uani 1 1 d . . . C8 C 0.9035(8) 0.4667(7) 0.4041(6) 0.0117(12) Uani 1 1 d . . . H8 H 1.0152 0.4275 0.3512 0.014 Uiso 1 1 calc R . . C9 C 0.5828(7) 0.5757(7) 0.5655(5) 0.0079(8) Uani 1 1 d . . . C10 C 0.4058(7) 0.6205(7) 0.6592(5) 0.0086(8) Uani 1 1 d . . . C11 C 0.2812(7) 0.3148(6) 1.0913(5) 0.0074(11) Uani 1 1 d . . . C12 C 0.5882(7) 0.0630(6) 1.2972(5) 0.0086(11) Uani 1 1 d . . . H12 H 0.5936 0.0413 1.3779 0.010 Uiso 1 1 calc R . . C13 C 0.7343(7) -0.0058(6) 1.2076(5) 0.0086(12) Uani 1 1 d . . . H13 H 0.8389 -0.0760 1.2270 0.010 Uiso 1 1 calc R . . C14 C 0.4353(7) 0.2042(6) 1.1413(5) 0.0089(12) Uani 1 1 d . . . C15 C 0.7206(7) 0.0323(6) 1.0887(5) 0.0077(11) 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 0.00440(10) 0.00594(11) 0.00541(11) -0.00126(8) -0.00031(7) 0.00013(7) Ag1 0.0094(2) 0.0144(2) 0.0121(2) -0.00265(18) -0.00134(18) 0.00530(18) Ag2 0.0126(2) 0.0084(2) 0.0124(2) -0.00251(18) 0.00354(18) 0.00103(17) N1 0.0057(16) 0.0079(17) 0.0053(16) -0.0038(13) 0.0001(13) -0.0005(13) N2 0.0057(16) 0.0079(17) 0.0053(16) -0.0038(13) 0.0001(13) -0.0005(13) O1 0.007(2) 0.010(2) 0.011(2) -0.0060(17) 0.0017(16) -0.0008(16) O2 0.009(2) 0.009(2) 0.008(2) -0.0014(16) 0.0010(16) 0.0000(16) O3 0.008(2) 0.008(2) 0.005(2) -0.0015(16) 0.0009(15) 0.0016(15) O4 0.007(2) 0.009(2) 0.014(2) -0.0039(17) -0.0025(17) 0.0022(16) O5 0.008(2) 0.011(2) 0.006(2) 0.0016(16) 0.0043(16) 0.0037(16) O6 0.010(2) 0.014(2) 0.004(2) -0.0027(16) 0.0021(16) -0.0010(16) O7 0.012(2) 0.013(2) 0.009(2) -0.0046(17) -0.0017(17) -0.0035(17) O8 0.009(2) 0.011(2) 0.012(2) -0.0032(17) -0.0023(17) -0.0010(16) O9 0.007(2) 0.008(2) 0.011(2) -0.0007(16) -0.0024(16) 0.0014(16) O10 0.015(2) 0.016(2) 0.013(2) -0.0006(18) 0.0038(18) 0.0015(18) C1 0.014(3) 0.016(3) 0.005(3) -0.001(2) -0.001(2) -0.008(2) C2 0.014(3) 0.008(3) 0.006(3) -0.001(2) -0.001(2) -0.005(2) C3 0.008(3) 0.011(3) 0.010(3) -0.001(2) -0.001(2) -0.007(2) C4 0.006(2) 0.011(2) 0.007(2) -0.0071(16) 0.0012(15) 0.0006(16) C5 0.005(3) 0.010(3) 0.012(3) -0.007(2) 0.002(2) -0.003(2) C6 0.008(2) 0.010(2) 0.007(2) -0.0056(16) 0.0006(15) -0.0029(16) C8 0.012(3) 0.012(3) 0.012(3) -0.005(2) -0.001(2) -0.006(2) C9 0.008(2) 0.010(2) 0.007(2) -0.0056(16) 0.0006(15) -0.0029(16) C10 0.006(2) 0.011(2) 0.007(2) -0.0071(16) 0.0012(15) 0.0006(16) C11 0.006(3) 0.008(3) 0.009(3) -0.008(2) -0.001(2) 0.000(2) C12 0.014(3) 0.008(3) 0.004(3) 0.000(2) -0.003(2) -0.005(2) C13 0.005(3) 0.008(3) 0.012(3) -0.001(2) -0.001(2) -0.003(2) C14 0.008(3) 0.008(3) 0.010(3) -0.004(2) -0.001(2) -0.001(2) C15 0.011(3) 0.005(3) 0.007(3) 0.000(2) -0.001(2) -0.005(2) _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 O8 1.759(4) . ? U1 O7 1.764(4) . ? U1 O5 2.451(4) . ? U1 O6 2.498(4) . ? U1 O3 2.503(4) . ? U1 O2 2.516(4) . ? U1 N2 2.609(5) . ? U1 N1 2.620(5) . ? Ag1 O4 2.278(4) 1_465 ? Ag1 O6 2.369(4) . ? Ag1 O3 2.391(4) . ? Ag1 O1 2.436(4) 2_567 ? Ag1 Ag2 3.0633(6) 1_465 ? Ag1 Ag1 3.2699(10) 2_567 ? Ag2 O9 2.261(4) . ? Ag2 O5 2.385(4) . ? Ag2 O2 2.390(4) . ? Ag2 Ag1 3.0633(6) 1_645 ? N1 C6 1.338(7) . ? N1 C9 1.356(7) . ? N2 C15 1.332(7) . ? N2 C14 1.347(7) . ? O1 C11 1.235(7) . ? O1 Ag1 2.436(4) 2_567 ? O2 C3 1.286(7) . ? O3 C10 1.276(7) . ? O4 C3 1.232(7) . ? O4 Ag1 2.278(4) 1_645 ? O5 C4 1.288(7) . ? O6 C11 1.282(7) . ? O9 C10 1.236(6) 1_645 ? O10 C4 1.227(7) . ? C1 C8 1.371(8) . ? C1 C2 1.388(8) . ? C1 H1 0.9300 . ? C2 C9 1.384(8) . ? C2 H2 0.9300 . ? C3 C15 1.505(8) . ? C4 C6 1.499(7) . ? C5 C14 1.382(8) . ? C5 C12 1.404(8) . ? C5 H5 0.9300 . ? C6 C8 1.382(8) . ? C8 H8 0.9300 . ? C9 C10 1.502(8) . ? C10 O9 1.236(6) 1_465 ? C11 C14 1.496(7) . ? C12 C13 1.387(8) . ? C12 H12 0.9300 . ? C13 C15 1.380(8) . ? C13 H13 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 O8 U1 O7 178.51(18) . . ? O8 U1 O5 91.90(17) . . ? O7 U1 O5 87.92(17) . . ? O8 U1 O6 95.40(16) . . ? O7 U1 O6 84.83(16) . . ? O5 U1 O6 172.47(14) . . ? O8 U1 O3 89.34(15) . . ? O7 U1 O3 89.49(16) . . ? O5 U1 O3 121.21(12) . . ? O6 U1 O3 60.87(12) . . ? O8 U1 O2 96.19(15) . . ? O7 U1 O2 85.01(16) . . ? O5 U1 O2 60.45(12) . . ? O6 U1 O2 116.70(12) . . ? O3 U1 O2 174.22(13) . . ? O8 U1 N2 82.96(16) . . ? O7 U1 N2 98.42(16) . . ? O5 U1 N2 118.90(13) . . ? O6 U1 N2 60.42(13) . . ? O3 U1 N2 119.56(13) . . ? O2 U1 N2 59.76(13) . . ? O8 U1 N1 85.81(16) . . ? O7 U1 N1 92.82(16) . . ? O5 U1 N1 60.45(13) . . ? O6 U1 N1 121.89(13) . . ? O3 U1 N1 61.05(13) . . ? O2 U1 N1 120.90(13) . . ? N2 U1 N1 168.73(14) . . ? O4 Ag1 O6 129.94(14) 1_465 . ? O4 Ag1 O3 136.64(14) 1_465 . ? O6 Ag1 O3 64.31(13) . . ? O4 Ag1 O1 94.23(14) 1_465 2_567 ? O6 Ag1 O1 124.18(14) . 2_567 ? O3 Ag1 O1 108.95(13) . 2_567 ? O4 Ag1 Ag2 78.56(10) 1_465 1_465 ? O6 Ag1 Ag2 148.12(10) . 1_465 ? O3 Ag1 Ag2 85.21(9) . 1_465 ? O1 Ag1 Ag2 55.32(9) 2_567 1_465 ? O4 Ag1 Ag1 98.90(10) 1_465 2_567 ? O6 Ag1 Ag1 73.97(10) . 2_567 ? O3 Ag1 Ag1 123.76(10) . 2_567 ? O1 Ag1 Ag1 65.97(9) 2_567 2_567 ? Ag2 Ag1 Ag1 120.65(2) 1_465 2_567 ? O9 Ag2 O5 121.99(13) . . ? O9 Ag2 O2 140.08(14) . . ? O5 Ag2 O2 63.16(13) . . ? O9 Ag2 Ag1 73.90(10) . 1_645 ? O5 Ag2 Ag1 137.15(10) . 1_645 ? O2 Ag2 Ag1 79.79(9) . 1_645 ? C6 N1 C9 117.3(5) . . ? C6 N1 U1 121.4(3) . . ? C9 N1 U1 121.2(4) . . ? C15 N2 C14 118.2(5) . . ? C15 N2 U1 118.5(4) . . ? C14 N2 U1 121.0(3) . . ? C11 O1 Ag1 119.5(4) . 2_567 ? C3 O2 Ag2 121.5(4) . . ? C3 O2 U1 125.7(4) . . ? Ag2 O2 U1 111.85(15) . . ? C10 O3 Ag1 115.2(3) . . ? C10 O3 U1 127.9(3) . . ? Ag1 O3 U1 116.85(15) . . ? C3 O4 Ag1 128.3(4) . 1_645 ? C4 O5 Ag2 111.1(3) . . ? C4 O5 U1 130.1(3) . . ? Ag2 O5 U1 114.33(15) . . ? C11 O6 Ag1 111.7(3) . . ? C11 O6 U1 128.3(3) . . ? Ag1 O6 U1 117.89(15) . . ? C10 O9 Ag2 138.3(4) 1_645 . ? C8 C1 C2 119.0(5) . . ? C8 C1 H1 120.5 . . ? C2 C1 H1 120.5 . . ? C9 C2 C1 118.6(5) . . ? C9 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? O4 C3 O2 126.7(6) . . ? O4 C3 C15 119.8(5) . . ? O2 C3 C15 113.4(5) . . ? O10 C4 O5 125.4(5) . . ? O10 C4 C6 121.0(5) . . ? O5 C4 C6 113.7(5) . . ? C14 C5 C12 118.4(5) . . ? C14 C5 H5 120.8 . . ? C12 C5 H5 120.8 . . ? N1 C6 C8 123.1(5) . . ? N1 C6 C4 113.4(5) . . ? C8 C6 C4 123.4(5) . . ? C1 C8 C6 119.2(6) . . ? C1 C8 H8 120.4 . . ? C6 C8 H8 120.4 . . ? N1 C9 C2 122.8(5) . . ? N1 C9 C10 113.7(5) . . ? C2 C9 C10 123.4(5) . . ? O9 C10 O3 127.1(5) 1_465 . ? O9 C10 C9 117.5(5) 1_465 . ? O3 C10 C9 115.4(5) . . ? O1 C11 O6 125.1(5) . . ? O1 C11 C14 120.9(5) . . ? O6 C11 C14 114.0(5) . . ? C13 C12 C5 118.7(5) . . ? C13 C12 H12 120.6 . . ? C5 C12 H12 120.6 . . ? C15 C13 C12 118.4(5) . . ? C15 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? N2 C14 C5 122.6(5) . . ? N2 C14 C11 112.8(5) . . ? C5 C14 C11 124.6(5) . . ? N2 C15 C13 123.3(5) . . ? N2 C15 C3 113.3(5) . . ? C13 C15 C3 122.9(5) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.312 _refine_diff_density_min -1.135 _refine_diff_density_rms 0.233 #====================================================================== data_cc _database_code_depnum_ccdc_archive 'CCDC 610444' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H6 N2 O16 Pb2 U' _chemical_formula_sum 'C16 H6 N2 O16 Pb2 U' _chemical_formula_weight 1134.66 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' Pb Pb -3.3944 10.1111 '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 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.7087(4) _cell_length_b 19.9618(10) _cell_length_c 12.8850(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.8420(10) _cell_angle_gamma 90.00 _cell_volume 2143.87(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9318 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 30.31 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 23.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.123 _exptl_absorpt_correction_T_max 0.155 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10742 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 30.31 _reflns_number_total 5637 _reflns_number_gt 5523 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0191P)^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 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 0.000(18) _refine_ls_number_reflns 5637 _refine_ls_number_parameters 335 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.76054(2) 0.219196(11) 0.501267(17) 0.00699(5) Uani 1 1 d . . . Pb1 Pb 0.78186(2) 0.436313(11) 0.491118(19) 0.01120(5) Uani 1 1 d . . . Pb2 Pb 0.71022(3) 0.003998(12) 0.47109(2) 0.01303(6) Uani 1 1 d . . . O1 O 0.6224(6) 0.1160(3) 0.5311(4) 0.0160(11) Uani 1 1 d . . . O2 O 0.8683(6) 0.1090(2) 0.4774(4) 0.0149(11) Uani 1 1 d . . . O3 O 0.8944(6) 0.3212(2) 0.4610(5) 0.0141(11) Uani 1 1 d . . . O4 O 0.6644(7) 0.3302(2) 0.5333(5) 0.0152(11) Uani 1 1 d . . . O5 O 0.6310(6) 0.2196(2) 0.3665(4) 0.0158(10) Uani 1 1 d . . . O6 O 0.8848(6) 0.2181(2) 0.6377(4) 0.0136(10) Uani 1 1 d . . . O7 O 0.4335(6) 0.0575(2) 0.5769(4) 0.0151(10) Uani 1 1 d . . . O8 O 1.0564(6) 0.3831(3) 0.3941(4) 0.0164(11) Uani 1 1 d . . . O9 O 0.4763(6) 0.4037(3) 0.5448(4) 0.0188(11) Uani 1 1 d . . . O10 O 1.0226(6) 0.0336(2) 0.4319(4) 0.0156(10) Uani 1 1 d . . . O11 O 0.7834(6) 0.4511(3) 0.6798(4) 0.0215(11) Uani 1 1 d . . . O12 O 1.0576(6) 0.4256(3) 0.6227(4) 0.0211(11) Uani 1 1 d . . . O13 O 1.0873(8) -0.1144(3) 0.2979(5) 0.0404(16) Uani 1 1 d . . . O14 O 0.9312(8) -0.0106(3) 0.1816(5) 0.0279(13) Uani 1 1 d . . . O15 O 0.7032(6) 0.0351(3) 0.2830(4) 0.0232(12) Uani 1 1 d . . . O16 O 0.4339(6) 0.0231(3) 0.3467(4) 0.0198(11) Uani 1 1 d . . . N1 N 0.5088(6) 0.2289(3) 0.5732(5) 0.0103(11) Uani 1 1 d . . . N2 N 1.0049(6) 0.2087(3) 0.4172(4) 0.0087(11) Uani 1 1 d . . . C1 C 0.5003(8) 0.1099(4) 0.5685(5) 0.0119(14) Uani 1 1 d . . . C2 C 0.4372(8) 0.1742(3) 0.5982(5) 0.0095(13) Uani 1 1 d . . . C3 C 0.3140(8) 0.1780(4) 0.6462(5) 0.0131(13) Uani 1 1 d . . . H3 H 0.2692 0.1392 0.6648 0.016 Uiso 1 1 calc R . . C4 C 0.2586(7) 0.2402(3) 0.6663(5) 0.0122(12) Uani 1 1 d . . . H4 H 0.1787 0.2435 0.7008 0.015 Uiso 1 1 calc R . . C5 C 0.3229(8) 0.2977(4) 0.6347(5) 0.0134(13) Uani 1 1 d . . . H5 H 0.2831 0.3400 0.6428 0.016 Uiso 1 1 calc R . . C6 C 1.0060(8) 0.3281(3) 0.4150(6) 0.0101(14) Uani 1 1 d . . . C7 C 1.0712(7) 0.2632(4) 0.3877(5) 0.0081(12) Uani 1 1 d . . . C8 C 1.1943(7) 0.2599(3) 0.3373(5) 0.0093(12) Uani 1 1 d . . . H8 H 1.2383 0.2987 0.3179 0.011 Uiso 1 1 calc R . . C9 C 1.1797(7) 0.1401(3) 0.3485(5) 0.0114(12) Uani 1 1 d . . . H9 H 1.2125 0.0974 0.3357 0.014 Uiso 1 1 calc R . . C10 C 1.0624(7) 0.1490(3) 0.3989(5) 0.0064(11) Uani 1 1 d . . . C11 C 0.4503(8) 0.2891(3) 0.5899(6) 0.0111(13) Uani 1 1 d . . . C12 C 0.5318(8) 0.3472(3) 0.5541(5) 0.0108(12) Uani 1 1 d . . . C13 C 1.2484(7) 0.1968(3) 0.3171(5) 0.0111(12) Uani 1 1 d . . . H13 H 1.3290 0.1926 0.2834 0.013 Uiso 1 1 calc R . . C14 C 0.9828(8) 0.0916(3) 0.4382(5) 0.0096(12) Uani 1 1 d . . . C15 C 0.9160(8) 0.4602(4) 0.7507(5) 0.0162(13) Uani 1 1 d . . . C16 C 1.0710(8) 0.4489(4) 0.7143(6) 0.0183(14) 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 0.00675(9) 0.00610(10) 0.00901(10) -0.00036(9) 0.00369(6) -0.00031(8) Pb1 0.01239(11) 0.00839(11) 0.01437(11) 0.00102(9) 0.00633(7) 0.00093(9) Pb2 0.01581(11) 0.00867(11) 0.01723(12) -0.00110(9) 0.00893(8) -0.00153(9) O1 0.017(2) 0.012(3) 0.023(3) -0.004(2) 0.013(2) -0.0016(19) O2 0.014(2) 0.011(3) 0.022(3) 0.001(2) 0.010(2) 0.0009(18) O3 0.015(2) 0.012(2) 0.021(3) -0.0028(19) 0.012(2) -0.0023(18) O4 0.018(3) 0.006(2) 0.028(3) 0.0000(19) 0.017(2) -0.0006(17) O5 0.011(2) 0.022(3) 0.013(2) 0.000(2) -0.0004(18) -0.0026(19) O6 0.013(2) 0.016(3) 0.013(2) -0.0022(18) 0.0054(18) 0.0009(18) O7 0.018(2) 0.011(2) 0.020(3) 0.000(2) 0.012(2) -0.0023(19) O8 0.016(2) 0.015(3) 0.019(3) 0.000(2) 0.0065(19) -0.003(2) O9 0.017(2) 0.016(3) 0.026(3) 0.001(2) 0.010(2) 0.006(2) O10 0.017(2) 0.008(2) 0.023(3) 0.002(2) 0.0071(19) 0.0020(19) O11 0.022(3) 0.028(3) 0.013(2) 0.002(2) 0.0032(19) -0.009(2) O12 0.025(3) 0.021(3) 0.015(3) -0.003(2) 0.001(2) 0.010(2) O13 0.045(4) 0.037(4) 0.030(3) -0.005(3) -0.003(3) 0.007(3) O14 0.042(3) 0.024(3) 0.018(3) 0.000(2) 0.009(2) -0.005(3) O15 0.019(2) 0.036(3) 0.015(3) 0.002(2) 0.0046(19) -0.004(2) O16 0.021(3) 0.023(3) 0.020(3) 0.003(2) 0.013(2) 0.009(2) N1 0.006(2) 0.015(3) 0.011(3) 0.001(2) 0.0037(19) 0.004(2) N2 0.008(2) 0.010(3) 0.008(3) 0.001(2) 0.0017(19) -0.003(2) C1 0.012(3) 0.017(4) 0.007(3) -0.001(3) 0.004(2) 0.000(3) C2 0.011(3) 0.011(3) 0.007(3) -0.001(2) 0.002(2) -0.005(2) C3 0.015(3) 0.019(4) 0.006(3) -0.004(2) 0.005(2) -0.006(3) C4 0.009(3) 0.018(3) 0.010(3) 0.000(3) 0.004(2) -0.004(2) C5 0.010(3) 0.020(3) 0.010(3) 0.000(3) 0.001(2) 0.002(3) C6 0.013(3) 0.003(3) 0.013(3) -0.002(2) 0.001(2) -0.003(2) C7 0.005(2) 0.014(3) 0.004(3) 0.001(2) -0.001(2) 0.000(2) C8 0.009(3) 0.013(3) 0.007(3) 0.000(2) 0.004(2) -0.001(2) C9 0.013(3) 0.011(3) 0.009(3) 0.000(2) 0.002(2) 0.000(2) C10 0.004(3) 0.007(3) 0.007(3) -0.001(2) -0.002(2) 0.000(2) C11 0.009(3) 0.012(3) 0.011(3) 0.002(2) 0.002(2) -0.001(2) C12 0.012(3) 0.009(3) 0.013(3) -0.003(3) 0.007(2) 0.001(3) C13 0.008(3) 0.014(3) 0.011(3) -0.007(2) 0.002(2) 0.000(2) C14 0.011(3) 0.009(3) 0.008(3) 0.001(2) 0.002(2) 0.001(2) C15 0.024(3) 0.011(3) 0.014(3) 0.003(3) 0.007(2) -0.003(3) C16 0.015(3) 0.025(4) 0.013(3) 0.007(3) 0.002(2) 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 O5 1.775(5) . ? U1 O6 1.777(5) . ? U1 O4 2.445(5) . ? U1 O2 2.446(5) . ? U1 O1 2.470(5) . ? U1 O3 2.475(5) . ? U1 N1 2.624(5) . ? U1 N2 2.661(6) . ? Pb1 O11 2.445(5) . ? Pb1 O4 2.481(5) . ? Pb1 O12 2.516(5) . ? Pb1 O3 2.571(5) . ? Pb2 O15 2.485(5) . ? Pb2 O2 2.496(5) . ? Pb2 O16 2.504(5) . ? Pb2 O1 2.555(5) . ? O1 C1 1.294(9) . ? O2 C14 1.289(8) . ? O3 C6 1.284(9) . ? O4 C12 1.304(8) . ? O7 C1 1.217(8) . ? O8 C6 1.242(8) . ? O9 C12 1.219(8) . ? O10 C14 1.218(8) . ? O11 C15 1.261(8) . ? O12 C16 1.242(9) . ? O15 C16 1.273(8) 4_454 ? O16 C15 1.247(8) 4_454 ? N1 C2 1.342(8) . ? N1 C11 1.346(9) . ? N2 C7 1.337(8) . ? N2 C10 1.340(8) . ? C1 C2 1.489(9) . ? C2 C3 1.388(9) . ? C3 C4 1.383(9) . ? C3 H3 0.9300 . ? C4 C5 1.389(10) . ? C4 H4 0.9300 . ? C5 C11 1.401(10) . ? C5 H5 0.9300 . ? C6 C7 1.496(9) . ? C7 C8 1.407(9) . ? C8 C13 1.395(9) . ? C8 H8 0.9300 . ? C9 C10 1.371(9) . ? C9 C13 1.393(9) . ? C9 H9 0.9300 . ? C10 C14 1.502(9) . ? C11 C12 1.501(10) . ? C13 H13 0.9300 . ? C15 O16 1.247(8) 4 ? C15 C16 1.568(9) . ? C16 O15 1.273(8) 4 ? 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 U1 O6 178.1(2) . . ? O5 U1 O4 90.6(2) . . ? O6 U1 O4 89.1(2) . . ? O5 U1 O2 92.2(2) . . ? O6 U1 O2 88.16(19) . . ? O4 U1 O2 177.1(2) . . ? O5 U1 O1 87.4(2) . . ? O6 U1 O1 91.2(2) . . ? O4 U1 O1 121.52(19) . . ? O2 U1 O1 59.44(16) . . ? O5 U1 O3 89.8(2) . . ? O6 U1 O3 91.6(2) . . ? O4 U1 O3 59.67(15) . . ? O2 U1 O3 119.51(18) . . ? O1 U1 O3 177.0(2) . . ? O5 U1 N1 89.2(2) . . ? O6 U1 N1 89.0(2) . . ? O4 U1 N1 60.73(18) . . ? O2 U1 N1 120.10(18) . . ? O1 U1 N1 60.81(18) . . ? O3 U1 N1 120.38(18) . . ? O5 U1 N2 87.6(2) . . ? O6 U1 N2 94.13(19) . . ? O4 U1 N2 119.55(17) . . ? O2 U1 N2 59.81(16) . . ? O1 U1 N2 118.74(17) . . ? O3 U1 N2 59.90(17) . . ? N1 U1 N2 176.82(18) . . ? O11 Pb1 O4 76.66(18) . . ? O11 Pb1 O12 67.10(17) . . ? O4 Pb1 O12 98.81(19) . . ? O11 Pb1 O3 111.43(18) . . ? O4 Pb1 O3 57.93(14) . . ? O12 Pb1 O3 72.20(17) . . ? O15 Pb2 O2 71.32(18) . . ? O15 Pb2 O16 65.82(16) . . ? O2 Pb2 O16 108.15(17) . . ? O15 Pb2 O1 98.73(19) . . ? O2 Pb2 O1 57.70(15) . . ? O16 Pb2 O1 75.14(17) . . ? C1 O1 U1 128.8(4) . . ? C1 O1 Pb2 112.4(4) . . ? U1 O1 Pb2 118.7(2) . . ? C14 O2 U1 131.3(4) . . ? C14 O2 Pb2 104.1(4) . . ? U1 O2 Pb2 122.1(2) . . ? C6 O3 U1 130.5(4) . . ? C6 O3 Pb1 110.3(4) . . ? U1 O3 Pb1 118.7(2) . . ? C12 O4 U1 129.7(4) . . ? C12 O4 Pb1 105.5(4) . . ? U1 O4 Pb1 123.6(2) . . ? C15 O11 Pb1 118.5(4) . . ? C16 O12 Pb1 114.6(4) . . ? C16 O15 Pb2 120.1(5) 4_454 . ? C15 O16 Pb2 119.8(5) 4_454 . ? C2 N1 C11 117.7(6) . . ? C2 N1 U1 121.2(4) . . ? C11 N1 U1 121.1(4) . . ? C7 N2 C10 117.3(6) . . ? C7 N2 U1 120.9(4) . . ? C10 N2 U1 121.7(4) . . ? O7 C1 O1 125.4(7) . . ? O7 C1 C2 119.8(7) . . ? O1 C1 C2 114.8(6) . . ? N1 C2 C3 122.3(6) . . ? N1 C2 C1 114.1(6) . . ? C3 C2 C1 123.5(6) . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.7(6) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C11 117.0(7) . . ? C4 C5 H5 121.5 . . ? C11 C5 H5 121.5 . . ? O8 C6 O3 123.9(6) . . ? O8 C6 C7 122.2(7) . . ? O3 C6 C7 114.0(5) . . ? N2 C7 C8 122.8(6) . . ? N2 C7 C6 114.4(6) . . ? C8 C7 C6 122.8(6) . . ? C13 C8 C7 118.2(6) . . ? C13 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C10 C9 C13 118.3(6) . . ? C10 C9 H9 120.9 . . ? C13 C9 H9 120.9 . . ? N2 C10 C9 124.5(6) . . ? N2 C10 C14 112.8(6) . . ? C9 C10 C14 122.7(6) . . ? N1 C11 C5 123.8(6) . . ? N1 C11 C12 114.0(6) . . ? C5 C11 C12 122.2(6) . . ? O9 C12 O4 124.8(6) . . ? O9 C12 C11 122.4(6) . . ? O4 C12 C11 112.8(6) . . ? C9 C13 C8 118.8(6) . . ? C9 C13 H13 120.6 . . ? C8 C13 H13 120.6 . . ? O10 C14 O2 123.4(6) . . ? O10 C14 C10 122.3(6) . . ? O2 C14 C10 114.3(6) . . ? O16 C15 O11 125.6(7) 4 . ? O16 C15 C16 117.7(6) 4 . ? O11 C15 C16 116.7(6) . . ? O12 C16 O15 124.8(7) . 4 ? O12 C16 C15 119.1(6) . . ? O15 C16 C15 116.1(6) 4 . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.555 _refine_diff_density_min -2.810 _refine_diff_density_rms 0.236 #====================================================================== data_c2onc _database_code_depnum_ccdc_archive 'CCDC 610445' #====================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 N2 O12 Pb U' _chemical_formula_sum 'C14 H6 N2 O12 Pb U' _chemical_formula_weight 839.44 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' Pb Pb -3.3944 10.1111 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.9437(9) _cell_length_b 16.0610(9) _cell_length_c 8.8145(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.9670(10) _cell_angle_gamma 90.00 _cell_volume 1759.37(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6336 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 30.27 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 18.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.268 _exptl_absorpt_correction_T_max 0.471 _exptl_absorpt_process_details 'SADABS, Sheldrick (2004)' _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8601 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 30.27 _reflns_number_total 2439 _reflns_number_gt 2204 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0151P)^2^+6.8491P] 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 2439 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0186 _refine_ls_wR_factor_ref 0.0419 _refine_ls_wR_factor_gt 0.0405 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.2500 0.2500 1.0000 0.00780(5) Uani 1 2 d S . . Pb1 Pb 0.5000 0.433708(10) 1.2500 0.00832(5) Uani 1 2 d S . . O1 O 0.0048(10) 0.4507(5) 0.898(2) 0.264(9) Uani 1 1 d . . . O2 O 0.3224(2) 0.38752(15) 0.9846(3) 0.0108(5) Uani 1 1 d . . . O3 O 0.1093(2) 0.18501(15) 0.7400(3) 0.0123(5) Uani 1 1 d . . . O4 O 0.1445(2) 0.30245(15) 1.0207(3) 0.0126(5) Uani 1 1 d . . . O5 O 0.3673(2) 0.49153(15) 0.8612(3) 0.0107(5) Uani 1 1 d . . . O6 O 0.0190(2) 0.15887(15) 0.4618(3) 0.0143(5) Uani 1 1 d . . . N1 N 0.2018(2) 0.31456(17) 0.7003(4) 0.0085(6) Uani 1 1 d . . . C1 C 0.2511(3) 0.3843(2) 0.6877(5) 0.0100(6) Uani 1 1 d . . . C2 C 0.1277(3) 0.2983(2) 0.3981(5) 0.0112(7) Uani 1 1 d . . . H2 H 0.0872 0.2665 0.3018 0.013 Uiso 1 1 calc R . . C3 C 0.2388(3) 0.4159(2) 0.5339(5) 0.0139(7) Uani 1 1 d . . . H3 H 0.2711 0.4660 0.5294 0.017 Uiso 1 1 calc R . . C4 C 0.1774(3) 0.3713(2) 0.3863(5) 0.0130(7) Uani 1 1 d . . . H4 H 0.1696 0.3900 0.2815 0.016 Uiso 1 1 calc R . . C5 C 0.3196(3) 0.4255(2) 0.8543(5) 0.0097(6) Uani 1 1 d . . . C6 C 0.1400(3) 0.2741(2) 0.5558(5) 0.0100(7) Uani 1 1 d . . . C7 C 0.0837(3) 0.2001(2) 0.5813(5) 0.0108(7) 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 0.01104(9) 0.00677(9) 0.00620(10) -0.00038(6) 0.00444(8) -0.00146(6) Pb1 0.00999(9) 0.00676(8) 0.00810(10) 0.000 0.00401(7) 0.000 O1 0.125(8) 0.102(6) 0.51(3) -0.018(9) 0.099(15) -0.002(6) O2 0.0150(12) 0.0088(11) 0.0077(12) -0.0003(10) 0.0043(10) -0.0027(10) O3 0.0152(13) 0.0109(11) 0.0101(13) 0.0002(10) 0.0052(11) -0.0031(10) O4 0.0144(12) 0.0121(11) 0.0137(14) -0.0024(10) 0.0085(11) -0.0019(10) O5 0.0136(12) 0.0069(10) 0.0132(13) -0.0022(9) 0.0074(11) -0.0023(9) O6 0.0165(13) 0.0131(12) 0.0093(13) -0.0018(10) 0.0023(11) -0.0028(10) N1 0.0105(14) 0.0071(13) 0.0083(14) -0.0009(11) 0.0046(12) 0.0003(10) C1 0.0106(15) 0.0080(14) 0.0107(17) 0.0015(13) 0.0044(14) 0.0022(13) C2 0.0100(16) 0.0141(16) 0.0081(17) 0.0015(13) 0.0029(14) 0.0001(13) C3 0.0167(18) 0.0117(16) 0.0120(19) 0.0019(14) 0.0055(15) -0.0019(14) C4 0.0153(17) 0.0153(17) 0.0087(17) -0.0001(14) 0.0057(14) -0.0013(14) C5 0.0108(16) 0.0110(15) 0.0083(17) -0.0006(13) 0.0052(14) 0.0013(13) C6 0.0114(16) 0.0069(14) 0.0131(18) 0.0009(13) 0.0067(14) 0.0011(12) C7 0.0099(16) 0.0101(15) 0.0117(18) 0.0012(13) 0.0044(14) 0.0026(13) _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 O4 1.775(2) 7_557 ? U1 O4 1.775(2) . ? U1 O2 2.458(2) 7_557 ? U1 O2 2.458(2) . ? U1 O3 2.473(3) . ? U1 O3 2.473(3) 7_557 ? U1 N1 2.626(3) 7_557 ? U1 N1 2.626(3) . ? Pb1 O3 2.467(2) 7_557 ? Pb1 O3 2.467(2) 8_556 ? Pb1 O2 2.627(3) . ? Pb1 O2 2.627(3) 2_657 ? Pb1 O5 2.733(2) 6_566 ? Pb1 O5 2.733(2) 5_667 ? O2 C5 1.286(4) . ? O3 C7 1.300(4) . ? O3 Pb1 2.467(2) 7_557 ? O5 C5 1.238(4) . ? O5 Pb1 2.733(2) 5_667 ? O6 C7 1.225(4) . ? N1 C6 1.339(5) . ? N1 C1 1.345(4) . ? C1 C3 1.384(5) . ? C1 C5 1.495(5) . ? C2 C6 1.377(5) . ? C2 C4 1.390(5) . ? C2 H2 0.9300 . ? C3 C4 1.388(5) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C6 C7 1.496(5) . ? 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 U1 O4 180.00(17) 7_557 . ? O4 U1 O2 87.69(10) 7_557 7_557 ? O4 U1 O2 92.31(10) . 7_557 ? O4 U1 O2 92.31(10) 7_557 . ? O4 U1 O2 87.69(10) . . ? O2 U1 O2 180.0 7_557 . ? O4 U1 O3 92.91(10) 7_557 . ? O4 U1 O3 87.09(10) . . ? O2 U1 O3 59.91(8) 7_557 . ? O2 U1 O3 120.09(8) . . ? O4 U1 O3 87.09(10) 7_557 7_557 ? O4 U1 O3 92.91(10) . 7_557 ? O2 U1 O3 120.09(8) 7_557 7_557 ? O2 U1 O3 59.91(8) . 7_557 ? O3 U1 O3 180.000(1) . 7_557 ? O4 U1 N1 94.03(10) 7_557 7_557 ? O4 U1 N1 85.97(10) . 7_557 ? O2 U1 N1 60.90(9) 7_557 7_557 ? O2 U1 N1 119.10(9) . 7_557 ? O3 U1 N1 119.95(8) . 7_557 ? O3 U1 N1 60.05(8) 7_557 7_557 ? O4 U1 N1 85.97(10) 7_557 . ? O4 U1 N1 94.03(10) . . ? O2 U1 N1 119.10(9) 7_557 . ? O2 U1 N1 60.90(9) . . ? O3 U1 N1 60.05(8) . . ? O3 U1 N1 119.95(8) 7_557 . ? N1 U1 N1 180.0 7_557 . ? O3 Pb1 O3 78.79(12) 7_557 8_556 ? O3 Pb1 O2 57.70(8) 7_557 . ? O3 Pb1 O2 95.62(8) 8_556 . ? O3 Pb1 O2 95.62(8) 7_557 2_657 ? O3 Pb1 O2 57.70(8) 8_556 2_657 ? O2 Pb1 O2 147.20(11) . 2_657 ? O3 Pb1 O5 78.30(8) 7_557 6_566 ? O3 Pb1 O5 151.86(8) 8_556 6_566 ? O2 Pb1 O5 85.73(8) . 6_566 ? O2 Pb1 O5 108.82(8) 2_657 6_566 ? O3 Pb1 O5 151.86(8) 7_557 5_667 ? O3 Pb1 O5 78.30(8) 8_556 5_667 ? O2 Pb1 O5 108.82(8) . 5_667 ? O2 Pb1 O5 85.73(8) 2_657 5_667 ? O5 Pb1 O5 127.88(10) 6_566 5_667 ? C5 O2 U1 129.0(2) . . ? C5 O2 Pb1 107.2(2) . . ? U1 O2 Pb1 116.71(9) . . ? C7 O3 Pb1 108.1(2) . 7_557 ? C7 O3 U1 129.3(2) . . ? Pb1 O3 U1 122.44(10) 7_557 . ? C5 O5 Pb1 142.6(2) . 5_667 ? C6 N1 C1 117.3(3) . . ? C6 N1 U1 121.7(2) . . ? C1 N1 U1 120.3(2) . . ? N1 C1 C3 123.1(3) . . ? N1 C1 C5 114.2(3) . . ? C3 C1 C5 122.7(3) . . ? C6 C2 C4 118.4(3) . . ? C6 C2 H2 120.8 . . ? C4 C2 H2 120.8 . . ? C1 C3 C4 118.5(3) . . ? C1 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C2 118.8(3) . . ? C3 C4 H4 120.6 . . ? C2 C4 H4 120.6 . . ? O5 C5 O2 124.3(3) . . ? O5 C5 C1 121.2(3) . . ? O2 C5 C1 114.5(3) . . ? N1 C6 C2 123.7(3) . . ? N1 C6 C7 113.4(3) . . ? C2 C6 C7 122.9(3) . . ? O6 C7 O3 124.1(3) . . ? O6 C7 C6 122.1(3) . . ? O3 C7 C6 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.051 _refine_diff_density_min -1.459 _refine_diff_density_rms 0.178