# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Christopher Cahill' 'Nicholas Deifel' _publ_contact_author_name 'Christopher Cahill' _publ_contact_author_email CAHILL@GWU.EDU _publ_section_title ; The Uranyl Tetrachloride Anion as a Tecton in the Assembly of U(VI) Hybrid Materials ; # Attachment 'CIF.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 735930' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cl4 N2 O2 U1' _chemical_formula_weight 570.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.5670(7) _cell_length_b 8.5723(10) _cell_length_c 8.8394(11) _cell_angle_alpha 71.139(2) _cell_angle_beta 73.078(2) _cell_angle_gamma 86.534(2) _cell_volume 381.64(8) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 226 _exptl_absorpt_coefficient_mu 11.329 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_T_max 0.516 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _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 II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7117 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 30.17 _reflns_number_total 2059 _reflns_number_gt 2059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.2924P] 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 2059 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.02686(8) Uani 1 2 d S . . Cl2 Cl 0.1590(7) 0.3052(2) -0.0555(3) 0.1049(11) Uani 1 1 d . . . Cl1 Cl 0.0279(5) -0.0662(2) 0.31072(19) 0.0657(5) Uani 1 1 d . . . O1 O -0.3046(9) 0.0620(10) 0.0644(8) 0.082(2) Uani 1 1 d . . . N1 N 0.3790(12) 0.2892(9) 0.2514(8) 0.0625(16) Uani 1 1 d . . . H1 H 0.3530 0.2386 0.1877 0.075 Uiso 1 1 calc R . . C1 C 0.5264(16) 0.2232(10) 0.3465(9) 0.0618(18) Uani 1 1 d . . . H1A H 0.5971 0.1222 0.3458 0.074 Uiso 1 1 calc R . . C2 C 0.5756(14) 0.3037(10) 0.4467(9) 0.0563(16) Uani 1 1 d . . . H2 H 0.6791 0.2567 0.5140 0.068 Uiso 1 1 calc R . . C3 C 0.4721(11) 0.4540(9) 0.4478(8) 0.0497(14) Uani 1 1 d . . . C4 C 0.3125(14) 0.5154(12) 0.3501(11) 0.068(2) Uani 1 1 d . . . H4 H 0.2337 0.6140 0.3514 0.081 Uiso 1 1 calc R . . C5 C 0.2693(15) 0.4314(12) 0.2508(11) 0.070(2) Uani 1 1 d . . . H5 H 0.1640 0.4740 0.1837 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02855(12) 0.03192(12) 0.02821(12) -0.01540(8) -0.01470(8) 0.00591(8) Cl2 0.221(3) 0.0472(9) 0.0625(11) 0.0006(8) -0.0736(17) -0.0488(14) Cl1 0.1177(16) 0.0540(8) 0.0376(7) -0.0115(6) -0.0429(9) -0.0026(9) O1 0.037(2) 0.159(6) 0.104(4) -0.106(5) -0.037(3) 0.040(3) N1 0.065(4) 0.086(4) 0.056(3) -0.048(3) -0.015(3) -0.012(3) C1 0.076(5) 0.069(4) 0.054(4) -0.038(3) -0.016(3) -0.006(4) C2 0.058(4) 0.072(4) 0.053(3) -0.038(3) -0.017(3) -0.001(3) C3 0.034(2) 0.077(4) 0.055(3) -0.047(3) -0.007(2) -0.005(3) C4 0.051(4) 0.098(6) 0.089(5) -0.068(5) -0.033(4) 0.015(4) C5 0.056(4) 0.106(6) 0.081(5) -0.062(5) -0.032(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 O1 1.734(4) 2 ? U1 O1 1.734(4) . ? U1 Cl2 2.6581(17) . ? U1 Cl2 2.6581(17) 2 ? U1 Cl1 2.6683(14) . ? U1 Cl1 2.6683(14) 2 ? N1 C1 1.318(11) . ? N1 C5 1.329(11) . ? N1 H1 0.8600 . ? C1 C2 1.377(8) . ? C1 H1A 0.9300 . ? C2 C3 1.381(10) . ? C2 H2 0.9300 . ? C3 C4 1.382(10) . ? C3 C3 1.495(10) 2_666 ? C4 C5 1.379(9) . ? C4 H4 0.9300 . ? C5 H5 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 O1 U1 O1 180.0(5) 2 . ? O1 U1 Cl2 91.9(3) 2 . ? O1 U1 Cl2 88.1(3) . . ? O1 U1 Cl2 88.1(3) 2 2 ? O1 U1 Cl2 91.9(3) . 2 ? Cl2 U1 Cl2 180.00(3) . 2 ? O1 U1 Cl1 91.2(2) 2 . ? O1 U1 Cl1 88.8(2) . . ? Cl2 U1 Cl1 86.78(6) . . ? Cl2 U1 Cl1 93.22(6) 2 . ? O1 U1 Cl1 88.8(2) 2 2 ? O1 U1 Cl1 91.2(2) . 2 ? Cl2 U1 Cl1 93.22(6) . 2 ? Cl2 U1 Cl1 86.78(6) 2 2 ? Cl1 U1 Cl1 180.0 . 2 ? C1 N1 C5 122.2(6) . . ? C1 N1 H1 118.9 . . ? C5 N1 H1 118.9 . . ? N1 C1 C2 120.0(7) . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C1 C2 C3 120.4(7) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 117.4(6) . . ? C2 C3 C3 121.4(8) . 2_666 ? C4 C3 C3 121.2(8) . 2_666 ? C5 C4 C3 120.4(8) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? N1 C5 C4 119.6(8) . . ? N1 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl2 0.86 2.57 3.249(6) 136.7 . N1 H1 O1 0.86 2.57 3.099(8) 120.4 1_655 N1 H1 Cl1 0.86 2.98 3.531(6) 123.9 . _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 30.17 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.909 _refine_diff_density_min -1.531 _refine_diff_density_rms 0.162 #===END # Attachment '2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 735931' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Cl4 N2 O2 U' _chemical_formula_weight 598.1 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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' _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 7.0295(2) _cell_length_b 8.2438(2) _cell_length_c 8.7676(2) _cell_angle_alpha 82.81 _cell_angle_beta 70.63 _cell_angle_gamma 66.07 _cell_volume 438.111(19) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 30.47 _exptl_crystal_description plate _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 338 _exptl_absorpt_coefficient_mu 9.875 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_T_max 0.467 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _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 II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8701 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 30.47 _reflns_number_total 2434 _reflns_number_gt 2430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.1653P] 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 2434 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_ref 0.0437 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _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 0.5000 0.0000 0.5000 0.02743(5) Uani 1 2 d S . . Cl1 Cl 0.24066(14) -0.01734(11) 0.79574(9) 0.04422(17) Uani 1 1 d . . . Cl2 Cl 0.34390(15) -0.19669(13) 0.39170(10) 0.0503(2) Uani 1 1 d . . . O1 O 0.2919(4) 0.1973(3) 0.4668(3) 0.0451(5) Uani 1 1 d . . . N1 N 0.9777(4) 0.2853(4) 0.2747(3) 0.0386(5) Uani 1 1 d . . . H1 H 0.8934 0.2345 0.3342 0.046 Uiso 1 1 calc R . . C1 C 1.1370(5) 0.1993(4) 0.1438(4) 0.0412(7) Uani 1 1 d . . . H1A H 1.1567 0.0862 0.1183 0.049 Uiso 1 1 calc R . . C2 C 1.2710(5) 0.2792(5) 0.0474(4) 0.0406(7) Uani 1 1 d . . . H2 H 1.3816 0.2203 -0.0445 0.049 Uiso 1 1 calc R . . C3 C 0.9440(5) 0.4469(5) 0.3169(4) 0.0426(7) Uani 1 1 d . . . H3 H 0.8322 0.5024 0.4096 0.051 Uiso 1 1 calc R . . C4 C 1.0751(5) 0.5306(4) 0.2231(4) 0.0431(7) Uani 1 1 d . . . H4 H 1.0516 0.6438 0.2515 0.052 Uiso 1 1 calc R . . C5 C 1.2433(5) 0.4466(4) 0.0855(4) 0.0345(6) Uani 1 1 d . . . C6 C 1.3933(5) 0.5334(5) -0.0191(4) 0.0453(7) Uani 1 1 d . . . H6A H 1.3212 0.6609 -0.0022 0.054 Uiso 1 1 calc R . . H6B H 1.4229 0.5091 -0.1319 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02853(7) 0.02532(7) 0.02893(8) 0.00217(5) -0.00702(5) -0.01298(5) Cl1 0.0546(4) 0.0511(4) 0.0320(3) -0.0009(3) -0.0017(3) -0.0344(4) Cl2 0.0622(5) 0.0668(5) 0.0378(4) -0.0063(4) -0.0042(3) -0.0475(5) O1 0.0442(12) 0.0341(11) 0.0514(13) 0.0056(9) -0.0187(10) -0.0083(9) N1 0.0379(13) 0.0466(15) 0.0387(13) 0.0059(11) -0.0088(10) -0.0276(12) C1 0.0465(16) 0.0409(16) 0.0431(16) -0.0018(13) -0.0080(13) -0.0279(14) C2 0.0423(16) 0.0484(18) 0.0339(14) -0.0007(12) -0.0054(12) -0.0251(14) C3 0.0377(15) 0.0436(17) 0.0423(16) -0.0032(13) -0.0037(12) -0.0178(13) C4 0.0431(16) 0.0316(14) 0.0546(19) 0.0014(13) -0.0126(14) -0.0170(13) C5 0.0326(13) 0.0373(14) 0.0404(15) 0.0110(11) -0.0148(11) -0.0206(12) C6 0.0413(16) 0.0491(18) 0.0529(19) 0.0202(15) -0.0169(14) -0.0288(15) _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 1.762(2) . ? U1 O1 1.762(2) 2_656 ? U1 Cl1 2.6554(7) 2_656 ? U1 Cl1 2.6554(7) . ? U1 Cl2 2.6934(8) . ? U1 Cl2 2.6934(8) 2_656 ? N1 C3 1.333(4) . ? N1 C1 1.335(4) . ? N1 H1 0.8600 . ? C1 C2 1.368(4) . ? C1 H1A 0.9300 . ? C2 C5 1.382(4) . ? C2 H2 0.9300 . ? C3 C4 1.368(5) . ? C3 H3 0.9300 . ? C4 C5 1.390(5) . ? C4 H4 0.9300 . ? C5 C6 1.506(4) . ? C6 C6 1.511(6) 2_865 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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(2) . 2_656 ? O1 U1 Cl1 90.17(8) . 2_656 ? O1 U1 Cl1 89.83(8) 2_656 2_656 ? O1 U1 Cl1 89.83(8) . . ? O1 U1 Cl1 90.17(8) 2_656 . ? Cl1 U1 Cl1 180.0 2_656 . ? O1 U1 Cl2 91.02(9) . . ? O1 U1 Cl2 88.98(9) 2_656 . ? Cl1 U1 Cl2 91.24(2) 2_656 . ? Cl1 U1 Cl2 88.76(2) . . ? O1 U1 Cl2 88.98(9) . 2_656 ? O1 U1 Cl2 91.02(9) 2_656 2_656 ? Cl1 U1 Cl2 88.76(2) 2_656 2_656 ? Cl1 U1 Cl2 91.24(2) . 2_656 ? Cl2 U1 Cl2 180.0 . 2_656 ? C3 N1 C1 122.6(3) . . ? C3 N1 H1 118.7 . . ? C1 N1 H1 118.7 . . ? N1 C1 C2 119.3(3) . . ? N1 C1 H1A 120.3 . . ? C2 C1 H1A 120.3 . . ? C1 C2 C5 120.5(3) . . ? C1 C2 H2 119.8 . . ? C5 C2 H2 119.8 . . ? N1 C3 C4 119.6(3) . . ? N1 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C2 C5 C4 118.0(3) . . ? C2 C5 C6 120.5(3) . . ? C4 C5 C6 121.5(3) . . ? C5 C6 C6 111.5(3) . 2_865 ? C5 C6 H6A 109.3 . . ? C6 C6 H6A 109.3 2_865 . ? C5 C6 H6B 109.3 . . ? C6 C6 H6B 109.3 2_865 . ? H6A C6 H6B 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl2 0.86 2.50 3.259(3) 148.1 2_656 N1 H1 Cl1 0.86 2.83 3.367(3) 122.6 2_656 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 30.47 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.011 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.098 #===END # Attachment '3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 735932' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cl4 N2 O2 U' _chemical_formula_weight 596.07 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' Cl Cl 0.1484 0.1585 '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 7.0000(2) _cell_length_b 8.1759(2) _cell_length_c 8.4438(2) _cell_angle_alpha 81.59 _cell_angle_beta 73.86 _cell_angle_gamma 66.80 _cell_volume 426.310(19) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 274 _exptl_absorpt_coefficient_mu 10.148 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.310 _exptl_absorpt_correction_T_max 0.640 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _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 II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8313 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 30.25 _reflns_number_total 2359 _reflns_number_gt 2359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.0483P] 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 2359 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0142 _refine_ls_R_factor_gt 0.0142 _refine_ls_wR_factor_ref 0.0343 _refine_ls_wR_factor_gt 0.0343 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 0.02308(4) Uani 1 2 d S . . Cl1 Cl -0.23476(10) -0.03663(9) 0.30177(7) 0.03806(12) Uani 1 1 d . . . Cl2 Cl 0.15072(12) 0.20506(11) 0.10919(9) 0.04817(16) Uani 1 1 d . . . O1 O -0.2158(3) 0.1934(2) -0.0359(2) 0.0385(4) Uani 1 1 d . . . N1 N 0.4467(3) 0.3093(3) 0.7591(3) 0.0342(4) Uani 1 1 d . . . H1 H 0.3539 0.2616 0.8048 0.041 Uiso 1 1 calc R . . C1 C 0.6120(4) 0.2246(3) 0.6378(3) 0.0352(5) Uani 1 1 d . . . H1A H 0.6249 0.1166 0.6042 0.042 Uiso 1 1 calc R . . C2 C 0.4190(4) 0.4648(3) 0.8125(3) 0.0357(5) Uani 1 1 d . . . H2 H 0.3016 0.5194 0.8973 0.043 Uiso 1 1 calc R . . C3 C 0.7626(4) 0.2975(3) 0.5631(3) 0.0322(4) Uani 1 1 d . . . H3 H 0.8766 0.2402 0.4772 0.039 Uiso 1 1 calc R . . C4 C 0.5651(4) 0.5436(3) 0.7415(3) 0.0325(4) Uani 1 1 d . . . H4 H 0.5455 0.6532 0.7762 0.039 Uiso 1 1 calc R . . C5 C 0.7441(3) 0.4579(3) 0.6164(3) 0.0269(4) Uani 1 1 d . . . C6 C 0.9038(4) 0.5402(3) 0.5486(3) 0.0308(4) Uani 1 1 d . . . H6 H 0.8678 0.6568 0.5754 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02339(6) 0.02229(6) 0.02308(6) -0.00256(4) -0.00285(4) -0.00930(4) Cl1 0.0444(3) 0.0463(3) 0.0266(3) -0.0058(2) 0.0027(2) -0.0262(3) Cl2 0.0593(4) 0.0636(4) 0.0387(3) -0.0149(3) -0.0013(3) -0.0433(4) O1 0.0340(8) 0.0343(9) 0.0359(9) -0.0023(7) -0.0078(7) -0.0009(7) N1 0.0313(9) 0.0397(10) 0.0350(10) -0.0009(8) -0.0018(8) -0.0212(8) C1 0.0375(12) 0.0376(12) 0.0367(12) -0.0070(10) -0.0042(9) -0.0217(10) C2 0.0298(11) 0.0363(12) 0.0356(12) -0.0053(9) 0.0022(9) -0.0122(9) C3 0.0313(10) 0.0377(12) 0.0292(11) -0.0080(9) -0.0002(8) -0.0171(9) C4 0.0318(11) 0.0272(10) 0.0368(12) -0.0046(9) -0.0034(9) -0.0113(8) C5 0.0261(9) 0.0292(10) 0.0260(10) -0.0002(8) -0.0044(7) -0.0125(8) C6 0.0347(11) 0.0298(10) 0.0308(11) -0.0020(8) -0.0020(9) -0.0187(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 1.7624(16) 2 ? U1 O1 1.7624(16) . ? U1 Cl1 2.6683(6) 2 ? U1 Cl1 2.6683(6) . ? U1 Cl2 2.6758(6) . ? U1 Cl2 2.6758(6) 2 ? N1 C2 1.335(3) . ? N1 C1 1.336(3) . ? N1 H1 0.8600 . ? C1 C3 1.371(3) . ? C1 H1A 0.9300 . ? C2 C4 1.373(3) . ? C2 H2 0.9300 . ? C3 C5 1.395(3) . ? C3 H3 0.9300 . ? C4 C5 1.402(3) . ? C4 H4 0.9300 . ? C5 C6 1.468(3) . ? C6 C6 1.329(5) 2_766 ? C6 H6 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 O1 U1 O1 180.00(19) 2 . ? O1 U1 Cl1 89.25(6) 2 2 ? O1 U1 Cl1 90.75(6) . 2 ? O1 U1 Cl1 90.75(6) 2 . ? O1 U1 Cl1 89.25(6) . . ? Cl1 U1 Cl1 180.00(3) 2 . ? O1 U1 Cl2 91.22(7) 2 . ? O1 U1 Cl2 88.78(7) . . ? Cl1 U1 Cl2 88.51(2) 2 . ? Cl1 U1 Cl2 91.49(2) . . ? O1 U1 Cl2 88.78(7) 2 2 ? O1 U1 Cl2 91.22(7) . 2 ? Cl1 U1 Cl2 91.49(2) 2 2 ? Cl1 U1 Cl2 88.51(2) . 2 ? Cl2 U1 Cl2 180.00(3) . 2 ? C2 N1 C1 122.9(2) . . ? C2 N1 H1 118.5 . . ? C1 N1 H1 118.5 . . ? N1 C1 C3 119.8(2) . . ? N1 C1 H1A 120.1 . . ? C3 C1 H1A 120.1 . . ? N1 C2 C4 119.6(2) . . ? N1 C2 H2 120.2 . . ? C4 C2 H2 120.2 . . ? C1 C3 C5 119.7(2) . . ? C1 C3 H3 120.2 . . ? C5 C3 H3 120.2 . . ? C2 C4 C5 119.7(2) . . ? C2 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C3 C5 C4 118.3(2) . . ? C3 C5 C6 123.1(2) . . ? C4 C5 C6 118.6(2) . . ? C6 C6 C5 124.5(3) 2_766 . ? C6 C6 H6 117.7 2_766 . ? C5 C6 H6 117.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl2 0.86 2.64 3.318(2) 136.3 1_556 N1 H1 Cl1 0.86 2.65 3.286(2) 132.3 2_556 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 30.25 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.890 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.087 #===END # Attachment '4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 735933' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 Cl4 N2 O6 U' _chemical_formula_weight 712.14 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' 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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 8.0673(3) _cell_length_b 8.6337(3) _cell_length_c 9.2526(3) _cell_angle_alpha 67.9900(10) _cell_angle_beta 71.9850(10) _cell_angle_gamma 77.5720(10) _cell_volume 564.57(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 438 _exptl_absorpt_coefficient_mu 7.694 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.440 _exptl_absorpt_correction_T_max 0.735 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _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 II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10041 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.35 _reflns_number_total 3078 _reflns_number_gt 3066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^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 3078 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0448 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.0000 0.0000 0.0000 0.03093(5) Uani 1 2 d S . . Cl1 Cl 0.33544(10) -0.13230(11) -0.02752(9) 0.05017(18) Uani 1 1 d . . . Cl2 Cl -0.02146(10) -0.06483(12) 0.31077(9) 0.05231(19) Uani 1 1 d . . . O1 O 0.0640(3) 0.1990(3) -0.0458(3) 0.0481(5) Uani 1 1 d . . . N1 N 0.6208(3) 0.2076(3) 0.6593(3) 0.0469(6) Uani 1 1 d . . . H1 H 0.6909 0.1741 0.7215 0.056 Uiso 1 1 calc R . . O2 O 0.0149(3) 0.4309(3) 0.1976(2) 0.0473(5) Uani 1 1 d . . . H4 H -0.0477 0.4595 0.1349 0.071 Uiso 1 1 calc R . . O3 O 0.2261(3) 0.4794(3) -0.0314(2) 0.0463(5) Uani 1 1 d . . . C1 C 0.1743(4) 0.4371(4) 0.1188(3) 0.0380(6) Uani 1 1 d . . . C2 C 0.3108(4) 0.3905(4) 0.2095(4) 0.0457(7) Uani 1 1 d . . . H2 H 0.4281 0.3800 0.1539 0.055 Uiso 1 1 calc R . . C3 C 0.2729(4) 0.3637(4) 0.3641(4) 0.0446(7) Uani 1 1 d . . . H3 H 0.1549 0.3788 0.4162 0.054 Uiso 1 1 calc R . . C4 C 0.3988(4) 0.3120(4) 0.4633(3) 0.0385(6) Uani 1 1 d . . . C5 C 0.3456(4) 0.3254(4) 0.6160(3) 0.0440(7) Uani 1 1 d . . . H5 H 0.2320 0.3715 0.6525 0.053 Uiso 1 1 calc R . . C6 C 0.5715(4) 0.2449(5) 0.4117(4) 0.0510(8) Uani 1 1 d . . . H6 H 0.6122 0.2356 0.3093 0.061 Uiso 1 1 calc R . . C7 C 0.4580(4) 0.2715(4) 0.7131(4) 0.0456(7) Uani 1 1 d . . . H7 H 0.4212 0.2794 0.8160 0.055 Uiso 1 1 calc R . . C8 C 0.6802(4) 0.1932(5) 0.5127(4) 0.0571(9) Uani 1 1 d . . . H8 H 0.7952 0.1481 0.4794 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.03266(8) 0.03279(8) 0.03053(7) -0.01191(5) -0.01337(5) 0.00037(5) Cl1 0.0376(4) 0.0706(5) 0.0474(4) -0.0293(4) -0.0180(3) 0.0122(3) Cl2 0.0445(4) 0.0811(6) 0.0341(3) -0.0241(4) -0.0147(3) 0.0035(4) O1 0.0556(13) 0.0378(11) 0.0554(13) -0.0156(10) -0.0180(11) -0.0081(9) N1 0.0457(14) 0.0595(16) 0.0402(13) -0.0168(12) -0.0253(11) 0.0064(12) O2 0.0418(11) 0.0626(14) 0.0352(10) -0.0128(10) -0.0163(9) 0.0024(10) O3 0.0434(11) 0.0625(13) 0.0375(10) -0.0199(10) -0.0152(9) -0.0016(10) C1 0.0391(14) 0.0407(14) 0.0401(14) -0.0179(12) -0.0198(12) 0.0067(11) C2 0.0363(15) 0.0632(19) 0.0399(15) -0.0211(14) -0.0150(12) 0.0050(13) C3 0.0356(14) 0.0604(19) 0.0400(15) -0.0173(14) -0.0167(12) 0.0018(13) C4 0.0358(14) 0.0485(16) 0.0320(13) -0.0111(12) -0.0152(11) -0.0011(12) C5 0.0355(14) 0.0604(19) 0.0343(14) -0.0160(13) -0.0084(11) -0.0021(13) C6 0.0443(16) 0.076(2) 0.0396(15) -0.0308(16) -0.0175(13) 0.0103(15) C7 0.0452(16) 0.0618(19) 0.0315(13) -0.0150(13) -0.0129(12) -0.0052(14) C8 0.0416(16) 0.083(3) 0.0559(19) -0.0394(19) -0.0237(15) 0.0200(16) _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 1.760(2) 2 ? U1 O1 1.760(2) . ? U1 Cl2 2.6719(7) 2 ? U1 Cl2 2.6719(7) . ? U1 Cl1 2.6747(7) 2 ? U1 Cl1 2.6747(7) . ? N1 C7 1.329(4) . ? N1 C8 1.335(4) . ? N1 H1 0.8600 . ? O2 C1 1.268(4) . ? O2 H4 0.8200 . ? O3 C1 1.251(4) . ? C1 C2 1.486(4) . ? C2 C3 1.306(4) . ? C2 H2 0.9300 . ? C3 C4 1.466(4) . ? C3 H3 0.9300 . ? C4 C5 1.385(4) . ? C4 C6 1.397(4) . ? C5 C7 1.363(4) . ? C5 H5 0.9300 . ? C6 C8 1.366(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8 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 O1 U1 O1 180.00(15) 2 . ? O1 U1 Cl2 89.69(8) 2 2 ? O1 U1 Cl2 90.31(8) . 2 ? O1 U1 Cl2 90.31(8) 2 . ? O1 U1 Cl2 89.69(8) . . ? Cl2 U1 Cl2 180.00(4) 2 . ? O1 U1 Cl1 89.53(8) 2 2 ? O1 U1 Cl1 90.47(8) . 2 ? Cl2 U1 Cl1 86.81(2) 2 2 ? Cl2 U1 Cl1 93.19(2) . 2 ? O1 U1 Cl1 90.47(8) 2 . ? O1 U1 Cl1 89.53(8) . . ? Cl2 U1 Cl1 93.19(2) 2 . ? Cl2 U1 Cl1 86.81(2) . . ? Cl1 U1 Cl1 180.0 2 . ? C7 N1 C8 122.7(3) . . ? C7 N1 H1 118.6 . . ? C8 N1 H1 118.6 . . ? C1 O2 H4 109.5 . . ? O3 C1 O2 124.6(2) . . ? O3 C1 C2 117.0(3) . . ? O2 C1 C2 118.4(3) . . ? C3 C2 C1 122.7(3) . . ? C3 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C2 C3 C4 126.1(3) . . ? C2 C3 H3 117.0 . . ? C4 C3 H3 117.0 . . ? C5 C4 C6 117.9(3) . . ? C5 C4 C3 119.5(3) . . ? C6 C4 C3 122.5(3) . . ? C7 C5 C4 120.6(3) . . ? C7 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C8 C6 C4 119.5(3) . . ? C8 C6 H6 120.2 . . ? C4 C6 H6 120.2 . . ? N1 C7 C5 119.3(3) . . ? N1 C7 H7 120.3 . . ? C5 C7 H7 120.3 . . ? N1 C8 C6 119.8(3) . . ? N1 C8 H8 120.1 . . ? C6 C8 H8 120.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl2 0.86 2.59 3.259(3) 135.0 2_656 N1 H1 Cl1 0.86 2.66 3.338(3) 136.3 2_656 O2 H4 O3 0.82 1.85 2.656(3) 168.2 2_565 _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 30.35 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 1.016 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.096 #===END # Attachment '5.cif' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 735934' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H16 Cl4 N2 O2 U' _chemical_formula_weight 612.13 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' 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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 12.8370(3) _cell_length_b 11.6971(3) _cell_length_c 12.3740(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.24 _cell_angle_gamma 90.00 _cell_volume 1815.78(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 9.532 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_T_max 0.683 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _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 II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17363 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 30.37 _reflns_number_total 2590 _reflns_number_gt 1965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+2.1400P] 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 2590 _refine_ls_number_parameters 102 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0167 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0361 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.022 _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 0.2500 0.2500 0.5000 0.02993(4) Uani 1 2 d S . . O1 O 0.36398(15) 0.16747(17) 0.49668(17) 0.0472(5) Uani 1 1 d . . . Cl1 Cl 0.19983(6) 0.10827(6) 0.64949(6) 0.04740(17) Uani 1 1 d . . . Cl2 Cl 0.13479(7) 0.11753(7) 0.34254(6) 0.0563(2) Uani 1 1 d . . . N1 N 0.6113(2) 0.2994(3) 0.5913(2) 0.0613(8) Uani 1 1 d D . . H1 H 0.6127 0.3335 0.6532 0.074 Uiso 1 1 calc R . . C1 C 0.6253(3) 0.1868(4) 0.5913(3) 0.0637(10) Uani 1 1 d D . . H1A H 0.6373 0.1464 0.6576 0.076 Uiso 1 1 calc R . . C2 C 0.5953(3) 0.3612(3) 0.4994(3) 0.0583(9) Uani 1 1 d D . . H2 H 0.5860 0.4399 0.5023 0.070 Uiso 1 1 calc R . . C3 C 0.6222(2) 0.1302(3) 0.4936(3) 0.0505(7) Uani 1 1 d D . . H3 H 0.6314 0.0513 0.4932 0.061 Uiso 1 1 calc R . . C4 C 0.5924(2) 0.3085(3) 0.4005(2) 0.0464(7) Uani 1 1 d D . . H4 H 0.5819 0.3517 0.3360 0.056 Uiso 1 1 calc R . . C5 C 0.6052(2) 0.1916(2) 0.3953(2) 0.0364(6) Uani 1 1 d D . . C6 C 0.6009(2) 0.1325(3) 0.2865(2) 0.0488(7) Uani 1 1 d . . . H6A H 0.6627 0.0833 0.2928 0.059 Uiso 1 1 calc R . . H6B H 0.6042 0.1895 0.2303 0.059 Uiso 1 1 calc R . . C7 C 0.5000 0.0612(4) 0.2500 0.0556(12) Uani 1 2 d S . . H7A H 0.4914 0.0123 0.3108 0.067 Uiso 0.50 1 calc PR . . H7B H 0.5086 0.0123 0.1892 0.067 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.03398(7) 0.02884(7) 0.02805(7) -0.00021(6) 0.00903(5) 0.00457(6) O1 0.0433(11) 0.0425(11) 0.0593(12) 0.0034(10) 0.0185(10) 0.0136(9) Cl1 0.0665(5) 0.0416(4) 0.0367(3) 0.0042(3) 0.0168(3) -0.0036(3) Cl2 0.0778(5) 0.0569(5) 0.0328(3) -0.0060(3) 0.0085(3) -0.0202(4) N1 0.0502(16) 0.092(2) 0.0435(16) -0.0225(17) 0.0141(13) -0.0150(16) C1 0.054(2) 0.095(3) 0.0386(17) 0.0158(19) 0.0025(14) -0.013(2) C2 0.0533(19) 0.057(2) 0.065(2) -0.0192(18) 0.0137(16) -0.0035(15) C3 0.0536(18) 0.0478(18) 0.0463(17) 0.0123(14) 0.0019(14) 0.0024(14) C4 0.0541(18) 0.0427(18) 0.0418(16) -0.0014(13) 0.0086(13) -0.0022(14) C5 0.0310(13) 0.0417(16) 0.0368(14) -0.0016(12) 0.0078(10) 0.0006(11) C6 0.0498(17) 0.0528(19) 0.0441(16) -0.0078(14) 0.0104(13) 0.0120(14) C7 0.081(3) 0.034(2) 0.047(2) 0.000 0.000(2) 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 1.7606(18) . ? U1 O1 1.7606(18) 7_556 ? U1 Cl1 2.6627(7) 7_556 ? U1 Cl1 2.6627(7) . ? U1 Cl2 2.6763(7) . ? U1 Cl2 2.6763(7) 7_556 ? N1 C2 1.327(5) . ? N1 C1 1.330(6) . ? N1 H1 0.8600 . ? C1 C3 1.371(5) . ? C1 H1A 0.9300 . ? C2 C4 1.363(4) . ? C2 H2 0.9300 . ? C3 C5 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.380(4) . ? C4 H4 0.9300 . ? C5 C6 1.504(4) . ? C6 C7 1.526(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C6 1.526(4) 2_655 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? 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 180.00(13) . 7_556 ? O1 U1 Cl1 90.03(7) . 7_556 ? O1 U1 Cl1 89.97(7) 7_556 7_556 ? O1 U1 Cl1 89.97(7) . . ? O1 U1 Cl1 90.03(7) 7_556 . ? Cl1 U1 Cl1 180.0 7_556 . ? O1 U1 Cl2 89.96(7) . . ? O1 U1 Cl2 90.04(7) 7_556 . ? Cl1 U1 Cl2 91.86(2) 7_556 . ? Cl1 U1 Cl2 88.14(2) . . ? O1 U1 Cl2 90.04(7) . 7_556 ? O1 U1 Cl2 89.96(7) 7_556 7_556 ? Cl1 U1 Cl2 88.14(2) 7_556 7_556 ? Cl1 U1 Cl2 91.86(2) . 7_556 ? Cl2 U1 Cl2 180.0 . 7_556 ? C2 N1 C1 122.4(3) . . ? C2 N1 H1 118.8 . . ? C1 N1 H1 118.8 . . ? N1 C1 C3 120.0(3) . . ? N1 C1 H1A 120.0 . . ? C3 C1 H1A 120.0 . . ? N1 C2 C4 119.5(3) . . ? N1 C2 H2 120.2 . . ? C4 C2 H2 120.2 . . ? C1 C3 C5 119.5(3) . . ? C1 C3 H3 120.3 . . ? C5 C3 H3 120.3 . . ? C2 C4 C5 120.6(3) . . ? C2 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C3 118.0(3) . . ? C4 C5 C6 121.0(2) . . ? C3 C5 C6 121.0(3) . . ? C5 C6 C7 112.5(2) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C6 C7 C6 113.7(4) . 2_655 ? C6 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 2_655 . ? C6 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 2_655 . ? H7A C7 H7B 107.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl2 0.86 2.37 3.209(3) 165.4 8_556 _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 30.37 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.954 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.081 #===END # Attachment '6.cif' data_compound6 _database_code_depnum_ccdc_archive 'CCDC 735935' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 Cl6 N6 O4 U' _chemical_formula_weight 865.21 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' Cl Cl 0.1484 0.1585 '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 7.1290(4) _cell_length_b 9.9708(5) _cell_length_c 11.4392(6) _cell_angle_alpha 71.3090(10) _cell_angle_beta 72.5940(10) _cell_angle_gamma 77.2490(10) _cell_volume 727.92(7) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 538 _exptl_absorpt_coefficient_mu 6.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_T_max 0.685 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _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 II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14294 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 30.33 _reflns_number_total 4015 _reflns_number_gt 4015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.1024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4015 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0155 _refine_ls_R_factor_gt 0.0155 _refine_ls_wR_factor_ref 0.0420 _refine_ls_wR_factor_gt 0.0420 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 1.0000 0.0000 0.0000 0.02816(4) Uani 1 2 d S . . Cl1 Cl 0.62456(8) 0.02961(6) 0.13620(5) 0.04361(11) Uani 1 1 d . . . Cl2 Cl 1.08202(10) -0.23292(6) 0.18413(6) 0.04843(13) Uani 1 1 d . . . O1 O 1.0606(2) 0.10624(17) 0.07802(15) 0.0396(3) Uani 1 1 d . . . N1 N 0.7590(3) -0.0111(2) 0.5659(2) 0.0460(5) Uani 1 1 d . . . H1 H 0.7695 -0.0983 0.6118 0.055 Uiso 1 1 calc R . . N2 N 0.7076(3) 0.40831(19) 0.35303(17) 0.0351(3) Uani 1 1 d . . . N3 N 0.6806(3) 0.6208(2) -0.01528(18) 0.0427(4) Uani 1 1 d . . . H3 H 0.6715 0.6664 -0.0916 0.051 Uiso 1 1 calc R . . C1 C 0.7278(4) 0.0179(2) 0.4498(2) 0.0439(5) Uani 1 1 d . . . H1A H 0.7185 -0.0567 0.4205 0.053 Uiso 1 1 calc R . . C2 C 0.7741(3) 0.0925(3) 0.6117(2) 0.0448(5) Uani 1 1 d . . . H2A H 0.7933 0.0696 0.6932 0.054 Uiso 1 1 calc R . . C3 C 0.7095(3) 0.1550(2) 0.3738(2) 0.0384(4) Uani 1 1 d . . . H3A H 0.6849 0.1742 0.2942 0.046 Uiso 1 1 calc R . . C4 C 0.7616(3) 0.2311(3) 0.5404(2) 0.0390(4) Uani 1 1 d . . . H4 H 0.7749 0.3025 0.5723 0.047 Uiso 1 1 calc R . . C5 C 0.7285(3) 0.2662(2) 0.41790(18) 0.0326(4) Uani 1 1 d . . . C6 C 0.7579(4) 0.4834(3) 0.0093(2) 0.0452(5) Uani 1 1 d . . . H6 H 0.8028 0.4392 -0.0563 0.054 Uiso 1 1 calc R . . C7 C 0.6168(3) 0.6903(2) 0.0749(2) 0.0401(4) Uani 1 1 d . . . H7 H 0.5659 0.7869 0.0545 0.048 Uiso 1 1 calc R . . C8 C 0.7720(4) 0.4062(2) 0.1297(2) 0.0404(4) Uani 1 1 d . . . H8 H 0.8281 0.3107 0.1460 0.048 Uiso 1 1 calc R . . C9 C 0.6265(3) 0.6190(2) 0.1968(2) 0.0356(4) Uani 1 1 d . . . H9 H 0.5836 0.6673 0.2596 0.043 Uiso 1 1 calc R . . C10 C 0.7011(3) 0.4728(2) 0.22800(18) 0.0299(3) Uani 1 1 d . . . OW1 O 0.7533(4) 0.6261(3) 0.4436(2) 0.0713(6) Uani 1 1 d . . . Cl3 Cl 0.76915(10) -0.32914(6) 0.69628(5) 0.04582(12) Uani 1 1 d . . . H2 H 0.699(4) 0.468(3) 0.393(3) 0.043(7) 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 0.03263(5) 0.02710(5) 0.02662(5) -0.01070(3) -0.00793(3) -0.00205(3) Cl1 0.0359(2) 0.0532(3) 0.0402(3) -0.0174(2) -0.00471(19) -0.0026(2) Cl2 0.0604(3) 0.0398(3) 0.0402(3) -0.0021(2) -0.0184(2) -0.0023(2) O1 0.0462(8) 0.0393(7) 0.0419(8) -0.0218(6) -0.0111(6) -0.0071(6) N1 0.0425(9) 0.0396(9) 0.0426(10) 0.0080(8) -0.0107(8) -0.0076(8) N2 0.0455(9) 0.0331(8) 0.0268(8) -0.0071(6) -0.0113(7) -0.0037(7) N3 0.0532(11) 0.0478(10) 0.0277(8) -0.0001(7) -0.0146(7) -0.0175(8) C1 0.0437(11) 0.0367(10) 0.0461(12) -0.0048(9) -0.0096(9) -0.0074(8) C2 0.0418(11) 0.0525(12) 0.0304(10) 0.0032(9) -0.0100(8) -0.0074(9) C3 0.0431(10) 0.0375(10) 0.0339(10) -0.0038(8) -0.0129(8) -0.0083(8) C4 0.0404(10) 0.0460(11) 0.0283(9) -0.0057(8) -0.0099(8) -0.0059(8) C5 0.0316(8) 0.0353(9) 0.0273(8) -0.0038(7) -0.0083(7) -0.0030(7) C6 0.0622(14) 0.0468(11) 0.0290(10) -0.0132(8) -0.0040(9) -0.0179(10) C7 0.0431(10) 0.0353(9) 0.0388(11) -0.0011(8) -0.0156(9) -0.0047(8) C8 0.0526(12) 0.0335(9) 0.0312(10) -0.0103(8) -0.0033(8) -0.0059(8) C9 0.0406(10) 0.0322(9) 0.0328(9) -0.0091(7) -0.0105(8) -0.0006(7) C10 0.0309(8) 0.0313(8) 0.0262(8) -0.0064(6) -0.0073(6) -0.0039(7) OW1 0.0869(16) 0.0929(17) 0.0500(11) -0.0361(11) -0.0044(11) -0.0366(13) Cl3 0.0640(3) 0.0424(3) 0.0275(2) -0.00367(19) -0.0114(2) -0.0088(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 O1 1.7731(14) 2_755 ? U1 O1 1.7731(14) . ? U1 Cl1 2.6701(5) 2_755 ? U1 Cl1 2.6701(5) . ? U1 Cl2 2.6785(5) 2_755 ? U1 Cl2 2.6785(5) . ? N1 C2 1.335(4) . ? N1 C1 1.341(3) . ? N1 H1 0.8600 . ? N2 C5 1.371(3) . ? N2 C10 1.378(2) . ? N2 H2 0.84(3) . ? N3 C6 1.332(3) . ? N3 C7 1.338(3) . ? N3 H3 0.8600 . ? C1 C3 1.368(3) . ? C1 H1A 0.9300 . ? C2 C4 1.361(3) . ? C2 H2A 0.9300 . ? C3 C5 1.404(3) . ? C3 H3A 0.9300 . ? C4 C5 1.410(3) . ? C4 H4 0.9300 . ? C6 C8 1.367(3) . ? C6 H6 0.9300 . ? C7 C9 1.362(3) . ? C7 H7 0.9300 . ? C8 C10 1.397(3) . ? C8 H8 0.9300 . ? C9 C10 1.405(3) . ? C9 H9 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 O1 U1 O1 180.00(8) 2_755 . ? O1 U1 Cl1 89.41(5) 2_755 2_755 ? O1 U1 Cl1 90.59(5) . 2_755 ? O1 U1 Cl1 90.59(5) 2_755 . ? O1 U1 Cl1 89.41(5) . . ? Cl1 U1 Cl1 180.00(3) 2_755 . ? O1 U1 Cl2 89.19(6) 2_755 2_755 ? O1 U1 Cl2 90.81(6) . 2_755 ? Cl1 U1 Cl2 89.465(19) 2_755 2_755 ? Cl1 U1 Cl2 90.535(19) . 2_755 ? O1 U1 Cl2 90.81(6) 2_755 . ? O1 U1 Cl2 89.19(6) . . ? Cl1 U1 Cl2 90.535(19) 2_755 . ? Cl1 U1 Cl2 89.465(19) . . ? Cl2 U1 Cl2 180.00(4) 2_755 . ? C2 N1 C1 121.4(2) . . ? C2 N1 H1 119.3 . . ? C1 N1 H1 119.3 . . ? C5 N2 C10 130.07(19) . . ? C5 N2 H2 118(2) . . ? C10 N2 H2 112(2) . . ? C6 N3 C7 122.14(19) . . ? C6 N3 H3 118.9 . . ? C7 N3 H3 118.9 . . ? N1 C1 C3 121.2(2) . . ? N1 C1 H1A 119.4 . . ? C3 C1 H1A 119.4 . . ? N1 C2 C4 120.6(2) . . ? N1 C2 H2A 119.7 . . ? C4 C2 H2A 119.7 . . ? C1 C3 C5 118.8(2) . . ? C1 C3 H3A 120.6 . . ? C5 C3 H3A 120.6 . . ? C2 C4 C5 119.8(2) . . ? C2 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N2 C5 C3 124.70(19) . . ? N2 C5 C4 117.1(2) . . ? C3 C5 C4 118.09(19) . . ? N3 C6 C8 120.9(2) . . ? N3 C6 H6 119.6 . . ? C8 C6 H6 119.6 . . ? N3 C7 C9 119.7(2) . . ? N3 C7 H7 120.2 . . ? C9 C7 H7 120.2 . . ? C6 C8 C10 119.1(2) . . ? C6 C8 H8 120.4 . . ? C10 C8 H8 120.4 . . ? C7 C9 C10 120.1(2) . . ? C7 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C8 125.14(18) . . ? N2 C10 C9 116.80(18) . . ? C8 C10 C9 117.97(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl3 0.86 2.19 3.036(2) 166.8 . N2 H2 OW1 0.84(3) 1.99(3) 2.802(3) 162(3) . N3 H3 Cl3 0.86 2.30 3.061(2) 147.0 1_564 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 30.33 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.674 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.073 #===END # Attachment '7.cif' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 735936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 Cl6 N4 O4 U' _chemical_formula_weight 835.18 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' Cl Cl 0.1484 0.1585 '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 7.0230(2) _cell_length_b 15.4120(4) _cell_length_c 13.4514(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.76 _cell_angle_gamma 90.00 _cell_volume 1420.00(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow-green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 6.313 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.419 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _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 II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27602 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 30.32 _reflns_number_total 4025 _reflns_number_gt 3333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker AXS, 2005)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2005)' _computing_data_reduction 'SAINTPLUS (Bruker AXS, 2005)' _computing_structure_solution 'SHELXS (Sheldrick, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WINGX (Farrugia, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+0.9335P] 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 4025 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0508 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 0.02803(4) Uani 1 2 d S . . Cl1 Cl -0.02084(9) -0.17288(4) 0.01253(4) 0.03785(13) Uani 1 1 d . . . Cl2 Cl 0.23772(12) 0.45119(4) 0.89536(5) 0.05334(18) Uani 1 1 d . . . Cl3 Cl -0.14592(18) -0.01153(5) -0.19958(6) 0.0619(2) Uani 1 1 d . . . O1 O -0.2399(3) 0.00836(10) 0.0201(2) 0.0472(5) Uani 1 1 d . . . N2 N 0.4658(3) 0.32333(12) 0.04167(14) 0.0326(4) Uani 1 1 d . . . HN2 H 0.4387 0.3613 -0.0062 0.039 Uiso 1 1 calc R . . N1 N 0.4967(3) 0.18713(14) -0.28994(14) 0.0379(4) Uani 1 1 d . . . H1 H 0.4913 0.1755 -0.3530 0.046 Uiso 1 1 calc R . . C3 C 0.5539(3) 0.28707(15) -0.15511(17) 0.0330(5) Uani 1 1 d . . . H3 H 0.5893 0.3426 -0.1308 0.040 Uiso 1 1 calc R . . C5 C 0.4608(3) 0.14084(15) -0.12879(18) 0.0346(5) Uani 1 1 d . . . H5 H 0.4319 0.0973 -0.0866 0.041 Uiso 1 1 calc R . . C6 C 0.5097(3) 0.22441(14) -0.09056(16) 0.0276(4) Uani 1 1 d . . . C7 C 0.5117(3) 0.24266(16) 0.01747(15) 0.0286(4) Uani 1 1 d . . . C8 C 0.5556(4) 0.18140(17) 0.09434(18) 0.0383(5) Uani 1 1 d . . . H8 H 0.5893 0.1251 0.0801 0.046 Uiso 1 1 calc R . . C4 C 0.4563(4) 0.12441(16) -0.22934(19) 0.0397(5) Uani 1 1 d . . . H4 H 0.4249 0.0691 -0.2556 0.048 Uiso 1 1 calc R . . C9 C 0.5488(4) 0.20520(19) 0.19324(18) 0.0438(6) Uani 1 1 d . . . H9 H 0.5757 0.1643 0.2453 0.053 Uiso 1 1 calc R . . C10 C 0.4599(4) 0.34764(18) 0.13633(18) 0.0416(6) Uani 1 1 d . . . H10 H 0.4271 0.4044 0.1491 0.050 Uiso 1 1 calc R . . C2 C 0.5452(4) 0.26698(16) -0.25598(18) 0.0371(5) Uani 1 1 d . . . H2 H 0.5731 0.3091 -0.3001 0.044 Uiso 1 1 calc R . . C11 C 0.5024(4) 0.2890(2) 0.21459(18) 0.0460(6) Uani 1 1 d . . . H11 H 0.4999 0.3054 0.2808 0.055 Uiso 1 1 calc R . . OW1 O 0.0851(3) 0.61659(12) 0.97984(14) 0.0537(5) 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 0.03305(7) 0.02317(6) 0.03155(7) 0.00361(4) 0.01504(4) 0.00477(4) Cl1 0.0532(4) 0.0254(2) 0.0368(3) 0.0028(2) 0.0136(2) 0.0035(2) Cl2 0.0742(5) 0.0415(3) 0.0438(3) 0.0076(3) 0.0118(3) 0.0222(3) Cl3 0.1010(7) 0.0453(4) 0.0361(3) 0.0040(3) 0.0077(4) 0.0066(4) O1 0.0411(11) 0.0363(10) 0.0719(15) 0.0083(8) 0.0287(10) 0.0083(7) N2 0.0405(10) 0.0304(9) 0.0270(8) -0.0001(7) 0.0074(8) 0.0054(8) N1 0.0389(11) 0.0470(12) 0.0284(9) -0.0072(8) 0.0086(8) 0.0051(9) C3 0.0403(12) 0.0294(10) 0.0301(10) -0.0018(8) 0.0095(9) -0.0011(9) C5 0.0401(12) 0.0271(11) 0.0366(11) 0.0003(9) 0.0087(10) -0.0005(9) C6 0.0278(10) 0.0294(10) 0.0260(9) -0.0005(8) 0.0065(8) 0.0042(8) C7 0.0281(10) 0.0315(11) 0.0267(10) 0.0018(8) 0.0073(9) 0.0013(8) C8 0.0418(13) 0.0383(13) 0.0353(11) 0.0095(10) 0.0100(10) 0.0091(10) C4 0.0425(13) 0.0337(12) 0.0415(12) -0.0104(10) 0.0064(10) 0.0016(10) C9 0.0433(14) 0.0573(16) 0.0294(11) 0.0128(11) 0.0050(10) 0.0029(12) C10 0.0475(14) 0.0437(13) 0.0355(12) -0.0097(10) 0.0129(11) 0.0025(11) C2 0.0407(13) 0.0406(13) 0.0325(11) 0.0024(10) 0.0139(10) 0.0017(10) C11 0.0438(14) 0.0692(18) 0.0259(11) -0.0049(11) 0.0098(10) -0.0028(13) OW1 0.0823(15) 0.0400(10) 0.0424(10) 0.0044(8) 0.0213(10) 0.0063(10) _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 1.769(2) . ? U1 O1 1.769(2) 3 ? U1 Cl3 2.6597(8) . ? U1 Cl3 2.6597(8) 3 ? U1 Cl1 2.6758(6) 3 ? U1 Cl1 2.6758(6) . ? N2 C10 1.337(3) . ? N2 C7 1.342(3) . ? N2 HN2 0.8600 . ? N1 C2 1.330(3) . ? N1 C4 1.335(3) . ? N1 H1 0.8600 . ? C3 C6 1.379(3) . ? C3 C2 1.380(3) . ? C3 H3 0.9300 . ? C5 C4 1.369(3) . ? C5 C6 1.401(3) . ? C5 H5 0.9300 . ? C6 C7 1.477(3) . ? C7 C8 1.384(3) . ? C8 C9 1.391(3) . ? C8 H8 0.9300 . ? C4 H4 0.9300 . ? C9 C11 1.377(4) . ? C9 H9 0.9300 . ? C10 C11 1.370(4) . ? C10 H10 0.9300 . ? C2 H2 0.9300 . ? C11 H11 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 O1 U1 O1 180.00(16) . 3 ? O1 U1 Cl3 89.50(9) . . ? O1 U1 Cl3 90.50(9) 3 . ? O1 U1 Cl3 90.50(9) . 3 ? O1 U1 Cl3 89.50(9) 3 3 ? Cl3 U1 Cl3 180.00(5) . 3 ? O1 U1 Cl1 90.25(5) . 3 ? O1 U1 Cl1 89.75(5) 3 3 ? Cl3 U1 Cl1 90.983(19) . 3 ? Cl3 U1 Cl1 89.017(19) 3 3 ? O1 U1 Cl1 89.75(5) . . ? O1 U1 Cl1 90.25(5) 3 . ? Cl3 U1 Cl1 89.017(19) . . ? Cl3 U1 Cl1 90.983(19) 3 . ? Cl1 U1 Cl1 180.000(2) 3 . ? C10 N2 C7 123.4(2) . . ? C10 N2 HN2 118.3 . . ? C7 N2 HN2 118.3 . . ? C2 N1 C4 122.2(2) . . ? C2 N1 H1 118.9 . . ? C4 N1 H1 118.9 . . ? C6 C3 C2 119.7(2) . . ? C6 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C4 C5 C6 118.9(2) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C3 C6 C5 118.9(2) . . ? C3 C6 C7 122.1(2) . . ? C5 C6 C7 119.0(2) . . ? N2 C7 C8 118.5(2) . . ? N2 C7 C6 117.67(19) . . ? C8 C7 C6 123.9(2) . . ? C7 C8 C9 119.1(2) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N1 C4 C5 120.5(2) . . ? N1 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C11 C9 C8 120.4(2) . . ? C11 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N2 C10 C11 120.0(2) . . ? N2 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? N1 C2 C3 119.8(2) . . ? N1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C10 C11 C9 118.7(2) . . ? C10 C11 H11 120.7 . . ? C9 C11 H11 120.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 HN2 Cl2 0.86 2.20 2.9880(19) 152.4 1_554 N1 H1 OW1 0.86 1.90 2.718(3) 157.9 2_545 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 30.32 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.200 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.081 #===END