# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- ChemComm.cif' _audit_creation_method SHELXL-97 # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #========================================================================= # SUBMISSION DETAILS _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 202-994-6959 _publ_requested_category ? #========================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Combining coordination and supramolecular chemistry for the formation of uranyl-organic hybrid materials ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address N.P.Deifel . ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 United States of America ; C.L.Cahill . ; Department of Chemistry The George Washington University 725 21st Street, NW Washington, DC 20052 United States of America ; #========================================================================== # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 813278' #TrackingRef '- ChemComm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Cl4 O14 U2' _chemical_formula_weight 1198.32 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' 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5222(9) _cell_length_b 10.2842(11) _cell_length_c 37.821(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3314.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9606 _cell_measurement_theta_min 6.302 _cell_measurement_theta_max 56.540 _exptl_crystal_description plate _exptl_crystal_colour yellow _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 2.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 10.149 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.486 _exptl_absorpt_correction_T_max 0.666 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 50125 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3383 _reflns_number_gt 2811 _reflns_threshold_expression >2\s(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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0462P)^2^+20.5316P] 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 3383 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.315 _refine_ls_restrained_S_all 1.315 _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 0.94964(3) 0.28127(3) 0.464107(8) 0.01115(12) Uani 1 1 d . . . Cl2 Cl 0.8231(4) 0.0014(3) 0.24745(6) 0.0410(7) Uani 1 1 d . . . Cl1 Cl 1.1285(3) 0.8080(2) 0.30618(6) 0.0308(6) Uani 1 1 d . . . O3 O 0.8505(7) 0.0913(5) 0.49650(15) 0.0172(13) Uani 1 1 d . . . O2 O 1.1314(7) 0.1982(5) 0.46368(15) 0.0143(12) Uani 1 1 d . . . O1 O 0.7705(7) 0.3684(6) 0.46468(14) 0.0160(12) Uani 1 1 d . . . O7 O 0.8414(7) 0.1318(6) 0.42090(15) 0.0185(13) Uani 1 1 d . . . O6 O 0.9624(8) 0.3048(6) 0.40105(16) 0.0176(13) Uani 1 1 d . . . O5 O 1.0913(7) 0.4723(6) 0.45725(15) 0.0161(13) Uani 1 1 d . . . O4 O 0.9860(7) 0.3333(6) 0.52388(16) 0.0167(13) Uani 1 1 d . . . C8 C 0.8924(10) 0.1971(8) 0.3953(2) 0.0152(18) Uani 1 1 d . . . C9 C 0.8672(10) 0.1534(9) 0.3579(2) 0.0166(18) Uani 1 1 d . . . C10 C 0.7578(11) 0.0574(8) 0.3504(2) 0.0186(19) Uani 1 1 d . . . H3 H 0.6959 0.0223 0.3682 0.022 Uiso 1 1 calc R . . C11 C 0.7425(12) 0.0148(10) 0.3157(2) 0.029(2) Uani 1 1 d . . . H4 H 0.6672 -0.0471 0.3101 0.035 Uiso 1 1 calc R . . C12 C 0.8386(13) 0.0641(9) 0.2898(2) 0.025(2) Uani 1 1 d . . . C13 C 0.9441(12) 0.1597(10) 0.2965(2) 0.025(2) Uani 1 1 d . . . H6 H 1.0058 0.1939 0.2785 0.030 Uiso 1 1 calc R . . C14 C 0.9577(10) 0.2055(8) 0.3311(2) 0.0157(18) Uani 1 1 d . . . H7 H 1.0285 0.2718 0.3361 0.019 Uiso 1 1 calc R . . C1 C 1.0602(9) 0.5925(8) 0.4521(2) 0.0111(16) Uani 1 1 d . . . C2 C 1.0761(9) 0.6459(7) 0.4151(2) 0.0106(16) Uani 1 1 d . . . C3 C 1.1440(10) 0.5690(8) 0.3889(2) 0.0146(17) Uani 1 1 d . . . H10 H 1.1786 0.4853 0.3940 0.018 Uiso 1 1 calc R . . C4 C 1.1591(11) 0.6189(9) 0.3551(2) 0.0197(19) Uani 1 1 d . . . H11 H 1.2019 0.5684 0.3371 0.024 Uiso 1 1 calc R . . C5 C 1.1098(11) 0.7446(9) 0.3483(2) 0.0191(19) Uani 1 1 d . . . C6 C 1.0451(10) 0.8236(9) 0.3749(3) 0.020(2) Uani 1 1 d . . . H13 H 1.0145 0.9087 0.3702 0.024 Uiso 1 1 calc R . . C7 C 1.0285(10) 0.7709(8) 0.4082(2) 0.0144(18) Uani 1 1 d . . . H14 H 0.9846 0.8206 0.4262 0.017 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 0.01137(18) 0.01030(18) 0.01179(18) -0.00048(12) -0.00019(12) 0.00024(12) Cl2 0.069(2) 0.0380(14) 0.0163(12) -0.0082(10) -0.0072(13) -0.0104(13) Cl1 0.0453(16) 0.0313(13) 0.0159(11) 0.0104(9) 0.0046(11) 0.0024(12) O3 0.018(3) 0.010(3) 0.023(3) 0.000(2) 0.001(3) 0.001(3) O2 0.012(3) 0.004(3) 0.027(3) 0.000(2) 0.000(3) 0.002(2) O1 0.013(3) 0.018(3) 0.017(3) 0.000(2) -0.003(2) 0.005(2) O7 0.023(3) 0.014(3) 0.018(3) -0.001(2) -0.002(3) -0.004(3) O6 0.028(4) 0.012(3) 0.013(3) -0.001(2) -0.001(3) -0.003(3) O5 0.019(3) 0.018(3) 0.012(3) 0.001(2) -0.002(2) -0.005(3) O4 0.017(3) 0.016(3) 0.017(3) -0.002(3) 0.001(2) 0.000(3) C8 0.017(4) 0.014(4) 0.014(4) -0.003(3) -0.004(3) 0.004(3) C9 0.015(4) 0.024(5) 0.011(4) -0.002(3) 0.000(3) 0.004(4) C10 0.017(5) 0.015(4) 0.023(5) 0.000(3) -0.004(4) 0.000(4) C11 0.025(5) 0.040(6) 0.020(5) -0.001(4) -0.008(4) -0.012(5) C12 0.042(6) 0.021(5) 0.013(4) -0.005(4) -0.008(4) 0.001(4) C13 0.032(6) 0.024(5) 0.018(5) 0.001(4) 0.005(4) -0.001(4) C14 0.021(5) 0.004(4) 0.023(5) -0.005(3) -0.004(4) -0.003(3) C1 0.008(4) 0.011(4) 0.014(4) 0.001(3) -0.002(3) -0.008(3) C2 0.009(4) 0.002(3) 0.020(4) 0.001(3) 0.002(3) 0.001(3) C3 0.015(4) 0.009(4) 0.020(4) 0.000(3) 0.005(4) 0.001(3) C4 0.024(5) 0.023(5) 0.012(4) 0.002(3) 0.000(4) -0.008(4) C5 0.018(5) 0.024(5) 0.016(4) 0.005(4) 0.005(4) -0.006(4) C6 0.013(4) 0.015(4) 0.032(5) 0.014(4) 0.003(4) 0.003(4) C7 0.020(5) 0.005(4) 0.019(4) -0.003(3) 0.006(4) -0.004(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.769(6) . ? U1 O1 1.770(6) . ? U1 O5 2.321(6) . ? U1 O4 2.344(6) . ? U1 O6 2.400(6) . ? U1 O7 2.425(6) . ? U1 O3 2.456(6) . ? U1 C8 2.787(8) . ? Cl2 C12 1.733(9) . ? Cl1 C5 1.731(9) . ? O7 C8 1.257(10) . ? O6 C8 1.276(10) . ? O5 C1 1.279(10) . ? O4 C1 1.249(10) 5_766 ? C8 C9 1.499(11) . ? C9 C14 1.383(12) . ? C9 C10 1.387(12) . ? C10 C11 1.386(13) . ? C11 C12 1.374(14) . ? C12 C13 1.356(14) . ? C13 C14 1.395(13) . ? C1 O4 1.249(10) 5_766 ? C1 C2 1.509(11) . ? C2 C7 1.372(11) . ? C2 C3 1.396(11) . ? C3 C4 1.382(11) . ? C4 C5 1.383(13) . ? C5 C6 1.405(13) . ? C6 C7 1.380(12) . ? 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 178.5(3) . . ? O2 U1 O5 87.3(2) . . ? O1 U1 O5 91.2(2) . . ? O2 U1 O4 90.2(2) . . ? O1 U1 O4 89.2(2) . . ? O5 U1 O4 81.1(2) . . ? O2 U1 O6 90.0(2) . . ? O1 U1 O6 90.0(2) . . ? O5 U1 O6 77.3(2) . . ? O4 U1 O6 158.4(2) . . ? O2 U1 O7 91.2(2) . . ? O1 U1 O7 90.1(2) . . ? O5 U1 O7 131.2(2) . . ? O4 U1 O7 147.7(2) . . ? O6 U1 O7 53.9(2) . . ? O2 U1 O3 85.5(2) . . ? O1 U1 O3 95.7(2) . . ? O5 U1 O3 155.3(2) . . ? O4 U1 O3 75.3(2) . . ? O6 U1 O3 126.3(2) . . ? O7 U1 O3 72.6(2) . . ? O2 U1 C8 89.7(3) . . ? O1 U1 C8 91.0(3) . . ? O5 U1 C8 104.5(2) . . ? O4 U1 C8 174.4(2) . . ? O6 U1 C8 27.2(2) . . ? O7 U1 C8 26.8(2) . . ? O3 U1 C8 99.1(2) . . ? C8 O7 U1 92.8(5) . . ? C8 O6 U1 93.5(5) . . ? C1 O5 U1 136.6(5) . . ? C1 O4 U1 143.0(6) 5_766 . ? O7 C8 O6 119.5(8) . . ? O7 C8 C9 121.2(8) . . ? O6 C8 C9 119.3(8) . . ? O7 C8 U1 60.4(4) . . ? O6 C8 U1 59.3(4) . . ? C9 C8 U1 178.0(6) . . ? C14 C9 C10 120.0(8) . . ? C14 C9 C8 119.7(8) . . ? C10 C9 C8 120.2(8) . . ? C11 C10 C9 118.8(9) . . ? C12 C11 C10 120.0(9) . . ? C13 C12 C11 122.0(9) . . ? C13 C12 Cl2 119.5(8) . . ? C11 C12 Cl2 118.5(8) . . ? C12 C13 C14 118.3(9) . . ? C9 C14 C13 120.7(8) . . ? O4 C1 O5 123.0(8) 5_766 . ? O4 C1 C2 118.6(7) 5_766 . ? O5 C1 C2 118.3(7) . . ? C7 C2 C3 121.2(8) . . ? C7 C2 C1 119.4(7) . . ? C3 C2 C1 119.4(7) . . ? C4 C3 C2 119.1(8) . . ? C3 C4 C5 119.3(8) . . ? C4 C5 C6 121.9(8) . . ? C4 C5 Cl1 119.7(7) . . ? C6 C5 Cl1 118.5(7) . . ? C7 C6 C5 117.8(8) . . ? C2 C7 C6 120.8(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.232 _refine_diff_density_min -1.852 _refine_diff_density_rms 0.319 #===END # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 813279' #TrackingRef '- ChemComm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Br4 O14 U2' _chemical_formula_weight 1376.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.8826(19) _cell_length_b 8.8238(8) _cell_length_c 10.1004(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.7130(10) _cell_angle_gamma 90.00 _cell_volume 1770.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7872 _cell_measurement_theta_min 6.134 _cell_measurement_theta_max 53.058 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 13.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.303 _exptl_absorpt_correction_T_max 0.587 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 29979 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4393 _reflns_number_gt 3550 _reflns_threshold_expression >2\s(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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^+3.3311P] 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 4393 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.069127(9) 0.96143(2) 0.224502(18) 0.02653(6) Uani 1 1 d . . . O1 O 0.07020(19) 0.7889(4) 0.1358(4) 0.0386(9) Uani 1 1 d . . . O2 O 0.06803(18) 1.1356(4) 0.3106(4) 0.0396(9) Uani 1 1 d . . . O3 O 0.01037(19) 0.8519(4) 0.4118(4) 0.0403(9) Uani 1 1 d . . . O4 O -0.04640(18) 0.9876(4) 0.1701(4) 0.0371(9) Uani 1 1 d . . . O5 O 0.08035(18) 1.0930(4) 0.0295(4) 0.0384(9) Uani 1 1 d . . . O6 O 0.18941(19) 0.9788(5) 0.2162(4) 0.0453(10) Uani 1 1 d . . . O7 O 0.15087(18) 0.8547(5) 0.3844(4) 0.0420(9) Uani 1 1 d . . . Br1 Br 0.37790(3) 1.13339(12) -0.27910(9) 0.0778(3) Uani 1 1 d . . . Br2 Br 0.48906(4) 0.74572(14) 0.50784(13) 0.1169(4) Uani 1 1 d . . . C1 C 0.0915(3) 1.0608(5) -0.0903(5) 0.0307(11) Uani 1 1 d . . . C2 C 0.1607(3) 1.0786(6) -0.1366(5) 0.0316(11) Uani 1 1 d . . . C3 C 0.2096(3) 1.1519(6) -0.0564(6) 0.0361(12) Uani 1 1 d . . . H3 H 0.1987 1.1897 0.0259 0.043 Uiso 1 1 calc R . . C4 C 0.2738(3) 1.1683(7) -0.0990(6) 0.0460(15) Uani 1 1 d . . . H4 H 0.3066 1.2171 -0.0459 0.055 Uiso 1 1 calc R . . C5 C 0.2891(3) 1.1121(7) -0.2206(6) 0.0450(14) Uani 1 1 d . . . C6 C 0.2421(3) 1.0410(8) -0.3018(7) 0.0521(16) Uani 1 1 d . . . H6 H 0.2534 1.0048 -0.3843 0.063 Uiso 1 1 calc R . . C7 C 0.1769(3) 1.0235(7) -0.2589(6) 0.0435(14) Uani 1 1 d . . . H7 H 0.1444 0.9747 -0.3127 0.052 Uiso 1 1 calc R . . C8 C 0.1997(3) 0.8992(7) 0.3205(6) 0.0372(12) Uani 1 1 d . . . C9 C 0.2702(3) 0.8616(6) 0.3654(5) 0.0356(12) Uani 1 1 d . . . C10 C 0.2825(3) 0.7465(7) 0.4549(6) 0.0474(15) Uani 1 1 d . . . H10 H 0.2468 0.6933 0.4886 0.057 Uiso 1 1 calc R . . C11 C 0.3478(3) 0.7093(8) 0.4948(7) 0.0606(19) Uani 1 1 d . . . H11 H 0.3564 0.6286 0.5522 0.073 Uiso 1 1 calc R . . C12 C 0.3998(3) 0.7938(9) 0.4483(8) 0.063(2) Uani 1 1 d . . . C13 C 0.3885(3) 0.9104(10) 0.3614(8) 0.066(2) Uani 1 1 d . . . H13 H 0.4243 0.9667 0.3316 0.079 Uiso 1 1 calc R . . C14 C 0.3238(3) 0.9439(8) 0.3184(8) 0.0553(17) Uani 1 1 d . . . H14 H 0.3157 1.0218 0.2576 0.066 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 0.02819(10) 0.02630(10) 0.02494(10) -0.00019(8) -0.00034(7) 0.00018(8) O1 0.047(2) 0.0303(19) 0.039(2) -0.0073(17) 0.0014(17) 0.0022(16) O2 0.041(2) 0.035(2) 0.043(2) -0.0128(18) 0.0024(17) -0.0040(17) O3 0.048(2) 0.042(2) 0.031(2) 0.0083(17) 0.0025(17) -0.0039(17) O4 0.0303(19) 0.036(2) 0.045(2) 0.0020(17) -0.0016(17) -0.0034(15) O5 0.038(2) 0.047(2) 0.030(2) 0.0114(17) 0.0050(16) 0.0001(17) O6 0.036(2) 0.060(3) 0.039(2) 0.017(2) 0.0017(17) 0.0011(19) O7 0.035(2) 0.052(3) 0.038(2) 0.0120(19) 0.0003(17) 0.0004(17) Br1 0.0361(3) 0.1125(7) 0.0863(6) -0.0039(5) 0.0189(4) -0.0069(4) Br2 0.0386(4) 0.1532(10) 0.1567(11) 0.0441(9) -0.0188(5) 0.0145(5) C1 0.033(3) 0.026(2) 0.034(3) 0.010(2) 0.001(2) 0.001(2) C2 0.033(3) 0.030(3) 0.032(3) 0.004(2) 0.003(2) 0.000(2) C3 0.033(3) 0.039(3) 0.037(3) -0.002(2) 0.005(2) -0.003(2) C4 0.032(3) 0.058(4) 0.047(4) 0.001(3) -0.003(3) -0.011(3) C5 0.030(3) 0.052(4) 0.054(4) 0.006(3) 0.009(3) -0.002(3) C6 0.040(3) 0.072(5) 0.045(4) -0.003(3) 0.010(3) -0.004(3) C7 0.037(3) 0.054(4) 0.040(3) -0.003(3) 0.001(3) -0.003(3) C8 0.033(3) 0.043(3) 0.036(3) -0.003(3) -0.003(2) 0.000(2) C9 0.030(3) 0.040(3) 0.036(3) -0.002(2) -0.002(2) 0.004(2) C10 0.038(3) 0.049(4) 0.055(4) 0.005(3) -0.005(3) -0.004(3) C11 0.050(4) 0.062(4) 0.069(5) 0.023(4) -0.010(3) 0.005(3) C12 0.034(3) 0.081(5) 0.073(5) 0.008(4) -0.006(3) 0.012(3) C13 0.033(3) 0.086(6) 0.079(5) 0.009(5) 0.009(3) -0.004(3) C14 0.042(3) 0.057(4) 0.067(5) 0.011(3) 0.001(3) 0.000(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.767(4) . ? U1 O1 1.767(4) . ? U1 O5 2.307(4) . ? U1 O4 2.348(4) . ? U1 O6 2.402(4) . ? U1 O7 2.426(4) . ? U1 O3 2.467(4) . ? U1 C8 2.783(5) . ? O4 C1 1.252(6) 3_575 ? O5 C1 1.272(6) . ? O6 C8 1.275(7) . ? O7 C8 1.254(7) . ? Br1 C5 1.898(5) . ? Br2 C12 1.895(6) . ? C1 O4 1.252(6) 3_575 ? C1 C2 1.481(7) . ? C2 C7 1.381(8) . ? C2 C3 1.395(7) . ? C3 C4 1.374(8) . ? C4 C5 1.372(9) . ? C5 C6 1.366(9) . ? C6 C7 1.394(8) . ? C8 C9 1.489(7) . ? C9 C10 1.374(8) . ? C9 C14 1.392(8) . ? C10 C11 1.379(8) . ? C11 C12 1.375(10) . ? C12 C13 1.364(10) . ? C13 C14 1.370(9) . ? 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 179.03(18) . . ? O2 U1 O5 89.23(16) . . ? O1 U1 O5 89.81(16) . . ? O2 U1 O4 89.72(15) . . ? O1 U1 O4 90.07(15) . . ? O5 U1 O4 83.32(13) . . ? O2 U1 O6 89.84(16) . . ? O1 U1 O6 90.07(16) . . ? O5 U1 O6 78.55(13) . . ? O4 U1 O6 161.87(14) . . ? O2 U1 O7 91.90(16) . . ? O1 U1 O7 88.82(15) . . ? O5 U1 O7 132.45(13) . . ? O4 U1 O7 144.20(13) . . ? O6 U1 O7 53.93(13) . . ? O2 U1 O3 86.89(16) . . ? O1 U1 O3 93.96(16) . . ? O5 U1 O3 157.00(13) . . ? O4 U1 O3 74.00(13) . . ? O6 U1 O3 124.07(13) . . ? O7 U1 O3 70.39(12) . . ? O2 U1 C8 91.89(17) . . ? O1 U1 C8 88.47(17) . . ? O5 U1 C8 105.70(15) . . ? O4 U1 C8 170.85(16) . . ? O6 U1 C8 27.21(15) . . ? O7 U1 C8 26.75(15) . . ? O3 U1 C8 97.09(15) . . ? C1 O4 U1 141.3(4) 3_575 . ? C1 O5 U1 136.7(3) . . ? C8 O6 U1 93.3(3) . . ? C8 O7 U1 92.7(3) . . ? O4 C1 O5 122.4(5) 3_575 . ? O4 C1 C2 118.7(5) 3_575 . ? O5 C1 C2 118.8(5) . . ? C7 C2 C3 119.8(5) . . ? C7 C2 C1 120.3(5) . . ? C3 C2 C1 119.9(5) . . ? C4 C3 C2 120.0(5) . . ? C5 C4 C3 119.4(5) . . ? C6 C5 C4 122.0(5) . . ? C6 C5 Br1 118.6(5) . . ? C4 C5 Br1 119.4(4) . . ? C5 C6 C7 118.9(6) . . ? C2 C7 C6 120.0(6) . . ? O7 C8 O6 120.0(5) . . ? O7 C8 C9 120.9(5) . . ? O6 C8 C9 119.1(5) . . ? O7 C8 U1 60.6(3) . . ? O6 C8 U1 59.5(3) . . ? C9 C8 U1 177.0(4) . . ? C10 C9 C14 119.6(5) . . ? C10 C9 C8 120.1(5) . . ? C14 C9 C8 120.3(5) . . ? C9 C10 C11 120.3(6) . . ? C12 C11 C10 118.9(6) . . ? C13 C12 C11 121.7(6) . . ? C13 C12 Br2 119.8(5) . . ? C11 C12 Br2 118.6(6) . . ? C12 C13 C14 119.4(7) . . ? C13 C14 C9 120.1(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.732 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.147 #===END # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 813280' #TrackingRef '- ChemComm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 I4 O14 U2' _chemical_formula_weight 1564.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.645(2) _cell_length_b 8.8687(8) _cell_length_c 10.0673(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.429(2) _cell_angle_gamma 90.00 _cell_volume 1841.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7796 _cell_measurement_theta_min 5.925 _cell_measurement_theta_max 59.952 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 12.197 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_T_max 0.614 _exptl_absorpt_process_details 'SADABS, Sheldrick (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 31246 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 30.39 _reflns_number_total 5163 _reflns_number_gt 4019 _reflns_threshold_expression >2\s(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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0468P)^2^+1.1616P] 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 5163 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.066496(9) 0.46206(2) 0.224734(19) 0.02358(7) Uani 1 1 d . . . I1 I 0.37634(2) 0.63008(7) -0.27711(5) 0.05933(16) Uani 1 1 d . . . I2 I 0.48107(3) 0.24537(8) 0.51322(7) 0.0784(2) Uani 1 1 d . . . O1 O 0.0680(2) 0.2900(5) 0.1352(4) 0.0366(10) Uani 1 1 d . . . O2 O 0.0648(2) 0.6354(5) 0.3110(4) 0.0357(10) Uani 1 1 d . . . O3 O 0.0104(2) 0.3509(5) 0.4130(4) 0.0382(10) Uani 1 1 d . . . O4 O -0.0453(2) 0.4871(5) 0.1731(4) 0.0351(10) Uani 1 1 d . . . O5 O 0.07594(19) 0.5943(5) 0.0288(4) 0.0344(10) Uani 1 1 d . . . O6 O 0.1826(2) 0.4799(6) 0.2148(5) 0.0416(11) Uani 1 1 d . . . O7 O 0.1457(2) 0.3563(6) 0.3840(4) 0.0390(11) Uani 1 1 d . . . C1 C 0.0878(3) 0.5604(6) -0.0913(6) 0.0286(12) Uani 1 1 d . . . C2 C 0.1550(3) 0.5797(7) -0.1368(6) 0.0282(12) Uani 1 1 d . . . C3 C 0.2016(3) 0.6527(7) -0.0548(6) 0.0333(14) Uani 1 1 d . . . H3 H 0.1904 0.6897 0.0275 0.040 Uiso 1 1 calc R . . C4 C 0.2646(3) 0.6701(8) -0.0963(7) 0.0408(16) Uani 1 1 d . . . H4 H 0.2953 0.7207 -0.0429 0.049 Uiso 1 1 calc R . . C5 C 0.2808(3) 0.6120(9) -0.2163(6) 0.0385(15) Uani 1 1 d . . . C6 C 0.2353(3) 0.5390(8) -0.2975(7) 0.0405(16) Uani 1 1 d . . . H6 H 0.2471 0.5000 -0.3788 0.049 Uiso 1 1 calc R . . C7 C 0.1728(3) 0.5240(8) -0.2586(6) 0.0362(14) Uani 1 1 d . . . H7 H 0.1421 0.4762 -0.3143 0.043 Uiso 1 1 calc R . . C8 C 0.1931(3) 0.4025(8) 0.3203(6) 0.0343(13) Uani 1 1 d . . . C9 C 0.2605(3) 0.3631(7) 0.3640(6) 0.0311(13) Uani 1 1 d . . . C10 C 0.2724(3) 0.2484(8) 0.4542(7) 0.0421(16) Uani 1 1 d . . . H10 H 0.2382 0.1955 0.4893 0.051 Uiso 1 1 calc R . . C11 C 0.3364(4) 0.2127(9) 0.4923(7) 0.0516(19) Uani 1 1 d . . . H11 H 0.3453 0.1322 0.5494 0.062 Uiso 1 1 calc R . . C12 C 0.3862(3) 0.2973(9) 0.4448(7) 0.0431(16) Uani 1 1 d . . . C13 C 0.3749(3) 0.4130(10) 0.3581(8) 0.0501(18) Uani 1 1 d . . . H13 H 0.4093 0.4693 0.3276 0.060 Uiso 1 1 calc R . . C14 C 0.3121(3) 0.4460(8) 0.3157(7) 0.0407(15) Uani 1 1 d . . . H14 H 0.3041 0.5235 0.2549 0.049 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 0.02060(11) 0.02737(12) 0.02263(11) -0.00021(8) -0.00061(7) 0.00023(9) I1 0.0251(2) 0.0863(4) 0.0675(3) -0.0058(3) 0.0126(2) -0.0035(2) I2 0.0301(3) 0.0950(5) 0.1086(5) 0.0187(4) -0.0145(3) 0.0133(3) O1 0.034(2) 0.039(2) 0.036(2) -0.0082(19) 0.0001(18) 0.003(2) O2 0.035(2) 0.031(2) 0.041(2) -0.0074(18) 0.0038(19) -0.0035(19) O3 0.038(2) 0.045(3) 0.032(2) 0.0080(19) 0.0013(19) -0.007(2) O4 0.023(2) 0.045(3) 0.038(2) 0.0013(19) -0.0001(18) -0.0035(19) O5 0.024(2) 0.049(3) 0.030(2) 0.0099(19) 0.0038(17) 0.002(2) O6 0.024(2) 0.060(3) 0.040(2) 0.012(2) -0.0011(19) 0.002(2) O7 0.023(2) 0.057(3) 0.037(2) 0.014(2) -0.0005(18) 0.002(2) C1 0.023(3) 0.028(3) 0.034(3) 0.013(2) -0.002(2) 0.003(2) C2 0.025(3) 0.032(3) 0.027(3) 0.005(2) 0.001(2) -0.002(2) C3 0.025(3) 0.043(4) 0.033(3) -0.002(3) 0.001(2) -0.004(3) C4 0.027(3) 0.050(4) 0.045(4) -0.004(3) -0.002(3) -0.011(3) C5 0.019(3) 0.054(4) 0.043(3) 0.000(3) 0.009(3) 0.003(3) C6 0.033(3) 0.051(4) 0.038(3) -0.012(3) 0.008(3) -0.001(3) C7 0.026(3) 0.048(4) 0.035(3) -0.012(3) 0.001(3) -0.003(3) C8 0.029(3) 0.041(3) 0.033(3) -0.003(3) -0.002(3) 0.001(3) C9 0.025(3) 0.035(3) 0.033(3) -0.001(2) 0.000(2) 0.006(3) C10 0.028(3) 0.054(4) 0.044(4) 0.010(3) -0.002(3) 0.002(3) C11 0.044(4) 0.054(5) 0.056(5) 0.018(4) -0.004(4) 0.006(4) C12 0.031(3) 0.050(4) 0.048(4) 0.001(3) -0.006(3) 0.008(3) C13 0.022(3) 0.061(5) 0.067(5) 0.003(4) 0.001(3) -0.002(3) C14 0.035(4) 0.044(4) 0.043(4) 0.006(3) -0.003(3) 0.000(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.766(4) . ? U1 O1 1.773(4) . ? U1 O5 2.310(4) . ? U1 O4 2.355(4) . ? U1 O6 2.408(4) . ? U1 O7 2.429(4) . ? U1 O3 2.468(4) . ? U1 C8 2.797(6) . ? I1 C5 2.097(6) . ? I2 C12 2.100(6) . ? O4 C1 1.250(7) 3_565 ? O5 C1 1.280(7) . ? O6 C8 1.276(8) . ? O7 C8 1.261(7) . ? C1 O4 1.250(7) 3_565 ? C1 C2 1.490(8) . ? C2 C7 1.385(8) . ? C2 C3 1.400(8) . ? C3 C4 1.391(8) . ? C4 C5 1.368(9) . ? C5 C6 1.380(9) . ? C6 C7 1.371(9) . ? C8 C9 1.483(8) . ? C9 C10 1.378(9) . ? C9 C14 1.399(9) . ? C10 C11 1.396(9) . ? C11 C12 1.375(10) . ? C12 C13 1.360(10) . ? C13 C14 1.380(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 O2 U1 O1 178.9(2) . . ? O2 U1 O5 88.97(18) . . ? O1 U1 O5 89.95(18) . . ? O2 U1 O4 89.21(18) . . ? O1 U1 O4 90.41(18) . . ? O5 U1 O4 83.18(15) . . ? O2 U1 O6 90.23(19) . . ? O1 U1 O6 89.82(19) . . ? O5 U1 O6 79.11(15) . . ? O4 U1 O6 162.28(16) . . ? O2 U1 O7 92.22(19) . . ? O1 U1 O7 88.70(18) . . ? O5 U1 O7 132.90(14) . . ? O4 U1 O7 143.91(15) . . ? O6 U1 O7 53.81(15) . . ? O2 U1 O3 87.14(18) . . ? O1 U1 O3 93.75(18) . . ? O5 U1 O3 156.62(15) . . ? O4 U1 O3 73.73(15) . . ? O6 U1 O3 123.93(15) . . ? O7 U1 O3 70.33(14) . . ? O2 U1 C8 91.91(19) . . ? O1 U1 C8 88.6(2) . . ? O5 U1 C8 106.15(17) . . ? O4 U1 C8 170.62(17) . . ? O6 U1 C8 27.07(17) . . ? O7 U1 C8 26.75(16) . . ? O3 U1 C8 97.02(17) . . ? C1 O4 U1 140.1(4) 3_565 . ? C1 O5 U1 135.6(4) . . ? C8 O6 U1 93.7(4) . . ? C8 O7 U1 93.1(4) . . ? O4 C1 O5 123.0(5) 3_565 . ? O4 C1 C2 118.2(5) 3_565 . ? O5 C1 C2 118.8(5) . . ? C7 C2 C3 119.1(6) . . ? C7 C2 C1 121.1(6) . . ? C3 C2 C1 119.8(5) . . ? C4 C3 C2 120.1(6) . . ? C5 C4 C3 119.3(6) . . ? C4 C5 C6 121.0(6) . . ? C4 C5 I1 119.8(5) . . ? C6 C5 I1 119.2(5) . . ? C7 C6 C5 120.1(6) . . ? C6 C7 C2 120.4(6) . . ? O7 C8 O6 119.3(6) . . ? O7 C8 C9 120.7(6) . . ? O6 C8 C9 119.9(6) . . ? O7 C8 U1 60.1(3) . . ? O6 C8 U1 59.2(3) . . ? C9 C8 U1 176.2(4) . . ? C10 C9 C14 120.0(6) . . ? C10 C9 C8 120.6(6) . . ? C14 C9 C8 119.4(6) . . ? C9 C10 C11 119.2(6) . . ? C12 C11 C10 119.5(7) . . ? C13 C12 C11 121.7(6) . . ? C13 C12 I2 120.5(5) . . ? C11 C12 I2 117.8(5) . . ? C12 C13 C14 119.4(7) . . ? C13 C14 C9 120.0(6) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.345 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.280 #===END