# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Trevor Hayton' _publ_contact_author_email HAYTON@CHEM.UCSB.EDU _publ_section_title ; Reactivity of UI4(OEt2)2 with phenols: Probing the chemistry of the U-I bond ; loop_ _publ_author_name 'Trevor Hayton' 'David D. Schnaars' 'Guang Wu.' # Attachment 'Combined_CIF_01-26-09.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 715605' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31 I5 O3 U' _chemical_formula_weight 1095.90 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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 14.141(3) _cell_length_b 18.184(4) _cell_length_c 10.585(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2721.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Orange_Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 11.640 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.14096 _exptl_absorpt_correction_T_max 0.46166 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11975 _diffrn_reflns_av_R_equivalents 0.1304 _diffrn_reflns_av_sigmaI/netI 0.1543 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.73 _reflns_number_total 2800 _reflns_number_gt 1038 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^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 2800 _refine_ls_number_parameters 75 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1534 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 0.788 _refine_ls_restrained_S_all 0.788 _refine_ls_shift/su_max 0.004 _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 O2 O 0.7500 1.0000 0.9178(19) 0.115(7) Uiso 1 2 d SD . . O3 O 0.7500 0.0000 0.684(2) 0.175(10) Uiso 1 2 d SD . . O1 O 0.7392(10) 0.2500 0.2500 0.045(3) Uani 1 2 d S . . U1 U 0.91102(6) 0.2500 0.2500 0.0472(3) Uani 1 2 d S . . I2 I 0.90862(8) 0.21529(6) -0.02685(9) 0.0583(3) Uani 1 1 d . . . I3 I 0.90023(10) 0.41065(6) 0.19428(11) 0.0748(4) Uani 1 1 d . . . I1 I 1.12063(12) 0.2500 0.2500 0.0935(7) Uani 1 2 d S . . C1 C 0.6877(12) 0.2778(9) 0.1435(13) 0.061(5) Uani 1 1 d . . . H1A H 0.6500 0.2383 0.1080 0.073 Uiso 1 1 calc R . . H1B H 0.7323 0.2935 0.0794 0.073 Uiso 1 1 calc R . . C2 C 0.6232(12) 0.3416(8) 0.1760(16) 0.072(5) Uani 1 1 d . . . H2A H 0.5957 0.3337 0.2578 0.107 Uiso 1 1 calc R . . H2B H 0.5739 0.3452 0.1139 0.107 Uiso 1 1 calc R . . H2C H 0.6591 0.3864 0.1767 0.107 Uiso 1 1 calc R . . C6 C 0.8893(14) 0.0690(12) 0.675(2) 0.116(8) Uiso 1 1 d D . . H6A H 0.9065 0.0775 0.7617 0.175 Uiso 1 1 calc R . . H6B H 0.9193 0.1051 0.6224 0.175 Uiso 1 1 calc R . . H6C H 0.9097 0.0208 0.6503 0.175 Uiso 1 1 calc R . . C4 C 0.8832(16) 0.9439(15) 0.987(2) 0.135(9) Uiso 1 1 d D . . H4A H 0.9045 0.9243 0.9082 0.202 Uiso 1 1 calc R . . H4B H 0.9110 0.9164 1.0554 0.202 Uiso 1 1 calc R . . H4C H 0.9018 0.9945 0.9940 0.202 Uiso 1 1 calc R . . C5 C 0.7844(15) 0.0747(8) 0.661(3) 0.218(15) Uiso 1 1 d D . . H5A H 0.7583 0.1088 0.7225 0.261 Uiso 1 1 calc R . . H5B H 0.7675 0.0912 0.5770 0.261 Uiso 1 1 calc R . . C3 C 0.7786(17) 0.9384(17) 0.995(3) 0.33(3) Uiso 1 1 d D . . H3A H 0.7560 0.8922 0.9603 0.401 Uiso 1 1 calc R . . H3B H 0.7563 0.9436 1.0811 0.401 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 O1 0.069(10) 0.031(7) 0.033(7) -0.001(7) 0.000 0.000 U1 0.0486(5) 0.0473(5) 0.0457(5) -0.0002(4) 0.000 0.000 I2 0.0643(8) 0.0641(7) 0.0465(6) -0.0061(5) 0.0053(6) 0.0002(6) I3 0.1133(11) 0.0447(6) 0.0664(7) 0.0048(5) -0.0118(8) -0.0209(7) I1 0.0470(10) 0.151(2) 0.0826(13) -0.0086(14) 0.000 0.000 C1 0.055(12) 0.066(12) 0.061(11) -0.001(9) -0.009(9) -0.002(9) C2 0.085(14) 0.059(11) 0.071(12) 0.002(10) -0.013(10) 0.018(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 O2 C3 1.443(10) 2_675 ? O2 C3 1.443(10) . ? O3 C5 1.463(10) . ? O3 C5 1.463(10) 2_655 ? O1 C1 1.434(15) . ? O1 C1 1.434(15) 4 ? O1 U1 2.430(13) . ? U1 I1 2.964(2) . ? U1 I3 2.9841(13) 4 ? U1 I3 2.9841(13) . ? U1 I2 2.9979(12) . ? U1 I2 2.9979(12) 4 ? C1 C2 1.516(19) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C6 C5 1.495(10) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C4 C3 1.485(10) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 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 C3 O2 C3 111(4) 2_675 . ? C5 O3 C5 161(4) . 2_655 ? C1 O1 C1 118.9(16) . 4 ? C1 O1 U1 120.5(8) . . ? C1 O1 U1 120.5(8) 4 . ? O1 U1 I1 180.0 . . ? O1 U1 I3 87.07(3) . 4 ? I1 U1 I3 92.93(3) . 4 ? O1 U1 I3 87.07(3) . . ? I1 U1 I3 92.93(3) . . ? I3 U1 I3 174.14(7) 4 . ? O1 U1 I2 89.35(3) . . ? I1 U1 I2 90.65(3) . . ? I3 U1 I2 89.23(3) 4 . ? I3 U1 I2 90.71(3) . . ? O1 U1 I2 89.35(3) . 4 ? I1 U1 I2 90.65(3) . 4 ? I3 U1 I2 90.71(3) 4 4 ? I3 U1 I2 89.23(3) . 4 ? I2 U1 I2 178.70(5) . 4 ? O1 C1 C2 113.4(12) . . ? O1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 104.4(14) . . ? O3 C5 H5A 110.9 . . ? C6 C5 H5A 110.9 . . ? O3 C5 H5B 110.9 . . ? C6 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? O2 C3 C4 101.4(17) . . ? O2 C3 H3A 111.5 . . ? C4 C3 H3A 111.5 . . ? O2 C3 H3B 111.5 . . ? C4 C3 H3B 111.5 . . ? H3A C3 H3B 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 U1 I1 0(42) . . . . ? C1 O1 U1 I1 0(58) 4 . . . ? C1 O1 U1 I3 -125.5(7) . . . 4 ? C1 O1 U1 I3 54.5(7) 4 . . 4 ? C1 O1 U1 I3 54.5(7) . . . . ? C1 O1 U1 I3 -125.5(7) 4 . . . ? C1 O1 U1 I2 -36.3(7) . . . . ? C1 O1 U1 I2 143.7(7) 4 . . . ? C1 O1 U1 I2 143.7(7) . . . 4 ? C1 O1 U1 I2 -36.3(7) 4 . . 4 ? C1 O1 C1 C2 59.6(12) 4 . . . ? U1 O1 C1 C2 -120.4(12) . . . . ? C5 O3 C5 C6 -98(2) 2_655 . . . ? C3 O2 C3 C4 -102(3) 2_675 . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.919 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.223 #===END=== data_2 _database_code_depnum_ccdc_archive 'CCDC 715606' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37 I3 O4 U' _chemical_formula_weight 1020.28 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 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, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.166(3) _cell_length_b 12.357(2) _cell_length_c 29.580(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6274.7(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3760 _exptl_absorpt_coefficient_mu 8.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5272 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD are detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27765 _diffrn_reflns_av_R_equivalents 0.1400 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5352 _reflns_number_gt 2258 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^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 5352 _refine_ls_number_parameters 258 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1966 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1889 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.254 _refine_ls_shift/su_max 0.003 _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 C1 C 0.4254(10) 0.6971(16) 0.4423(7) 0.051(5) Uani 1 1 d . . . C2 C 0.3563(12) 0.7535(16) 0.4495(6) 0.062(5) Uani 1 1 d . . . H2 H 0.3363 0.8014 0.4282 0.074 Uiso 1 1 calc R . . C3 C 0.3192(11) 0.7341(19) 0.4901(8) 0.073(7) Uani 1 1 d . . . H3 H 0.2715 0.7678 0.4950 0.088 Uiso 1 1 calc R . . C4 C 0.3467(13) 0.6705(19) 0.5229(8) 0.078(7) Uani 1 1 d . . . H4 H 0.3183 0.6587 0.5492 0.094 Uiso 1 1 calc R . . C5 C 0.4170(15) 0.624(2) 0.5168(8) 0.099(8) Uani 1 1 d . . . H5 H 0.4394 0.5834 0.5399 0.119 Uiso 1 1 calc R . . C6 C 0.4563(11) 0.6366(19) 0.4754(8) 0.074(7) Uani 1 1 d . . . H6 H 0.5041 0.6029 0.4710 0.089 Uiso 1 1 calc R . . C7 C 0.5177(12) 0.4730(17) 0.3488(8) 0.073(7) Uani 1 1 d . . . H7A H 0.4670 0.4669 0.3345 0.088 Uiso 1 1 calc R . . H7B H 0.5099 0.4872 0.3807 0.088 Uiso 1 1 calc R . . C8 C 0.5615(19) 0.372(2) 0.3428(11) 0.136(12) Uani 1 1 d . . . H8A H 0.5383 0.3278 0.3192 0.163 Uiso 1 1 calc R . . H8B H 0.5622 0.3304 0.3707 0.163 Uiso 1 1 calc R . . C9 C 0.6403(19) 0.405(2) 0.3302(12) 0.140(12) Uani 1 1 d . . . H9A H 0.6613 0.3572 0.3072 0.168 Uiso 1 1 calc R . . H9B H 0.6745 0.4037 0.3563 0.168 Uiso 1 1 calc R . . C10 C 0.6330(12) 0.516(2) 0.3125(7) 0.072(7) Uani 1 1 d . . . H10A H 0.6762 0.5598 0.3229 0.087 Uiso 1 1 calc R . . H10B H 0.6333 0.5149 0.2797 0.087 Uiso 1 1 calc R . . C11 C 0.5479(14) 0.931(2) 0.4390(8) 0.101(9) Uani 1 1 d . . . H11A H 0.5539 0.8696 0.4591 0.122 Uiso 1 1 calc R . . H11B H 0.4935 0.9522 0.4388 0.122 Uiso 1 1 calc R . . C12 C 0.5967(16) 1.022(2) 0.4545(9) 0.117(7) Uani 1 1 d . . . H12A H 0.6461 0.9967 0.4665 0.140 Uiso 1 1 calc R . . H12B H 0.5703 1.0652 0.4771 0.140 Uiso 1 1 calc R . . C13 C 0.6074(16) 1.085(2) 0.4092(9) 0.117(7) Uani 1 1 d . . . H13A H 0.6498 1.1366 0.4106 0.140 Uiso 1 1 calc R . . H13B H 0.5599 1.1205 0.3995 0.140 Uiso 1 1 calc R . . C14 C 0.6274(14) 0.985(2) 0.3798(10) 0.135(13) Uani 1 1 d . . . H14A H 0.6206 1.0008 0.3479 0.163 Uiso 1 1 calc R . . H14B H 0.6807 0.9617 0.3849 0.163 Uiso 1 1 calc R . . C15 C 0.3457(10) 0.6585(19) 0.3227(10) 0.103(10) Uani 1 1 d . . . H15A H 0.3233 0.7299 0.3268 0.124 Uiso 1 1 calc R . . H15B H 0.3414 0.6192 0.3509 0.124 Uiso 1 1 calc R . . C16 C 0.3042(11) 0.6002(17) 0.2864(7) 0.070(6) Uani 1 1 d . . . H16A H 0.2500 0.6221 0.2845 0.084 Uiso 1 1 calc R . . H16B H 0.3070 0.5224 0.2906 0.084 Uiso 1 1 calc R . . C17 C 0.3494(12) 0.636(2) 0.2456(9) 0.105(9) Uani 1 1 d . . . H17A H 0.3446 0.5836 0.2213 0.125 Uiso 1 1 calc R . . H17B H 0.3312 0.7057 0.2349 0.125 Uiso 1 1 calc R . . C18 C 0.4311(10) 0.6432(18) 0.2613(8) 0.076(7) Uani 1 1 d . . . H18A H 0.4579 0.5752 0.2563 0.091 Uiso 1 1 calc R . . H18B H 0.4585 0.6999 0.2452 0.091 Uiso 1 1 calc R . . C19 C 0.2395(16) 1.0025(18) 0.4212(13) 0.222(19) Uiso 1 1 d D . . H19A H 0.2596 0.9985 0.4514 0.334 Uiso 1 1 calc R . . H19B H 0.2069 1.0653 0.4183 0.334 Uiso 1 1 calc R . . H19C H 0.2820 1.0075 0.4002 0.334 Uiso 1 1 calc R . . C20 C 0.1947(11) 0.9072(13) 0.4117(8) 0.153(12) Uiso 1 1 d D . . C21 C 0.1469(14) 0.864(2) 0.4449(6) 0.123(10) Uiso 1 1 d D . . H21 H 0.1404 0.9010 0.4721 0.148 Uiso 1 1 calc R . . C22 C 0.1084(17) 0.767(2) 0.4376(8) 0.25(2) Uiso 1 1 d D . . H22 H 0.0857 0.7293 0.4615 0.295 Uiso 1 1 calc R . . C23 C 0.1046(18) 0.726(2) 0.3938(10) 0.27(3) Uiso 1 1 d D . . H23 H 0.0672 0.6745 0.3861 0.328 Uiso 1 1 calc R . . C24 C 0.1578(15) 0.7627(17) 0.3619(7) 0.123(10) Uiso 1 1 d D . . H24 H 0.1662 0.7231 0.3356 0.147 Uiso 1 1 calc R . . C25 C 0.1983(10) 0.8579(17) 0.3691(6) 0.086(7) Uiso 1 1 d D . . H25 H 0.2275 0.8888 0.3459 0.103 Uiso 1 1 calc R . . I1 I 0.64010(8) 0.80494(13) 0.27115(6) 0.0818(5) Uani 1 1 d . . . I2 I 0.43047(8) 0.94195(12) 0.31914(5) 0.0750(5) Uani 1 1 d . . . I3 I 0.67093(8) 0.67499(16) 0.41072(6) 0.0972(7) Uani 1 1 d . . . O1 O 0.4654(7) 0.7150(11) 0.4021(4) 0.061(4) Uani 1 1 d . . . O2 O 0.5603(8) 0.5593(10) 0.3288(5) 0.063(4) Uani 1 1 d . . . O3 O 0.5727(7) 0.9035(11) 0.3947(5) 0.069(4) Uani 1 1 d . . . O4 O 0.4280(6) 0.6675(11) 0.3091(4) 0.062(4) Uani 1 1 d . . . U1 U 0.53469(4) 0.74954(7) 0.34946(2) 0.0527(3) 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 C1 0.045(11) 0.057(14) 0.050(15) 0.009(11) 0.004(10) 0.000(10) C2 0.083(14) 0.072(15) 0.031(13) 0.009(12) -0.001(10) -0.003(13) C3 0.052(12) 0.10(2) 0.066(17) -0.015(16) -0.010(12) 0.009(12) C4 0.086(17) 0.09(2) 0.059(18) 0.012(14) 0.032(13) 0.020(14) C5 0.12(2) 0.11(2) 0.059(19) 0.012(15) -0.009(16) 0.042(18) C6 0.065(13) 0.10(2) 0.054(16) 0.017(14) 0.014(12) 0.027(13) C7 0.084(15) 0.045(16) 0.091(19) 0.000(13) 0.003(13) 0.011(13) C8 0.17(3) 0.09(3) 0.14(3) 0.01(2) -0.03(2) 0.02(2) C9 0.14(3) 0.09(3) 0.19(4) 0.00(2) 0.03(3) 0.04(2) C10 0.077(15) 0.10(2) 0.041(14) 0.003(13) -0.004(12) 0.018(14) C11 0.12(2) 0.13(3) 0.052(17) -0.010(16) 0.022(15) -0.043(17) C12 0.128(15) 0.12(2) 0.101(18) -0.050(15) 0.012(15) -0.028(13) C13 0.128(15) 0.12(2) 0.101(18) -0.050(15) 0.012(15) -0.028(13) C14 0.094(18) 0.15(3) 0.16(3) -0.08(2) 0.08(2) -0.061(19) C15 0.033(11) 0.10(2) 0.18(3) -0.037(19) 0.008(14) -0.025(11) C16 0.057(12) 0.063(16) 0.091(19) 0.000(14) -0.005(13) -0.005(11) C17 0.066(14) 0.12(2) 0.12(2) 0.065(19) -0.034(15) -0.021(14) C18 0.062(13) 0.086(18) 0.079(19) 0.026(14) -0.017(12) 0.006(12) I1 0.0750(9) 0.0852(12) 0.0851(12) 0.0006(10) 0.0312(9) 0.0011(8) I2 0.0650(8) 0.0769(11) 0.0830(12) 0.0107(9) -0.0005(8) 0.0062(8) I3 0.0667(9) 0.1329(17) 0.0921(14) -0.0373(12) -0.0313(9) 0.0285(10) O1 0.056(8) 0.081(11) 0.045(9) -0.009(7) -0.010(7) 0.002(7) O2 0.075(9) 0.045(9) 0.068(10) 0.001(8) -0.005(8) -0.003(7) O3 0.063(8) 0.083(12) 0.061(11) -0.009(8) 0.002(7) -0.003(8) O4 0.029(6) 0.102(12) 0.054(10) -0.019(8) -0.001(6) 0.002(7) U1 0.0446(4) 0.0660(6) 0.0475(5) -0.0066(5) 0.0021(4) 0.0002(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 C1 C6 1.34(3) . ? C1 O1 1.39(2) . ? C1 C2 1.39(2) . ? C2 C3 1.38(3) . ? C2 H2 0.9300 . ? C3 C4 1.34(3) . ? C3 H3 0.9300 . ? C4 C5 1.35(3) . ? C4 H4 0.9300 . ? C5 C6 1.41(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O2 1.42(2) . ? C7 C8 1.47(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.46(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.47(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O2 1.44(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O3 1.42(2) . ? C11 C12 1.47(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.56(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.55(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O3 1.45(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O4 1.473(19) . ? C15 C16 1.48(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.50(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.48(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.45(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.435(10) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.385(8) . ? C20 C25 1.401(8) . ? C21 C22 1.395(9) . ? C21 H21 0.9300 . ? C22 C23 1.390(9) . ? C22 H22 0.9300 . ? C23 C24 1.391(9) . ? C23 H23 0.9300 . ? C24 C25 1.383(8) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? I1 U1 3.0180(16) . ? I2 U1 3.1079(16) . ? I3 U1 3.0987(17) . ? O1 U1 2.006(13) . ? O2 U1 2.468(13) . ? O3 U1 2.415(14) . ? O4 U1 2.409(11) . ? 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 C6 C1 O1 121.1(17) . . ? C6 C1 C2 120.3(19) . . ? O1 C1 C2 118.2(18) . . ? C3 C2 C1 116.0(19) . . ? C3 C2 H2 122.0 . . ? C1 C2 H2 122.0 . . ? C4 C3 C2 125(2) . . ? C4 C3 H3 117.5 . . ? C2 C3 H3 117.5 . . ? C3 C4 C5 118(2) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C4 C5 C6 120(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 120.5(19) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O2 C7 C8 109(2) . . ? O2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C7 C8 C9 105(3) . . ? C7 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8B 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? C8 C9 C10 106(2) . . ? C8 C9 H9A 110.6 . . ? C10 C9 H9A 110.6 . . ? C8 C9 H9B 110.6 . . ? C10 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? O2 C10 C9 107.6(19) . . ? O2 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O2 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O3 C11 C12 107.5(19) . . ? O3 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O3 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 C12 C13 100(2) . . ? C11 C12 H12A 111.7 . . ? C13 C12 H12A 111.7 . . ? C11 C12 H12B 111.7 . . ? C13 C12 H12B 111.7 . . ? H12A C12 H12B 109.5 . . ? C12 C13 C14 96(2) . . ? C12 C13 H13A 112.5 . . ? C14 C13 H13A 112.5 . . ? C12 C13 H13B 112.5 . . ? C14 C13 H13B 112.5 . . ? H13A C13 H13B 110.0 . . ? O3 C14 C13 103.9(18) . . ? O3 C14 H14A 111.0 . . ? C13 C14 H14A 111.0 . . ? O3 C14 H14B 111.0 . . ? C13 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? O4 C15 C16 107.6(18) . . ? O4 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O4 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C15 C16 C17 101.0(18) . . ? C15 C16 H16A 111.6 . . ? C17 C16 H16A 111.6 . . ? C15 C16 H16B 111.6 . . ? C17 C16 H16B 111.6 . . ? H16A C16 H16B 109.4 . . ? C18 C17 C16 104.8(18) . . ? C18 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? C18 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? O4 C18 C17 106.6(18) . . ? O4 C18 H18A 110.4 . . ? C17 C18 H18A 110.4 . . ? O4 C18 H18B 110.4 . . ? C17 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 119.9(7) . . ? C21 C20 C19 119(2) . . ? C25 C20 C19 121(2) . . ? C20 C21 C22 120.1(8) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 118.8(9) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 118.8(9) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 120.4(8) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 119.0(7) . . ? C24 C25 H25 120.5 . . ? C20 C25 H25 120.5 . . ? C1 O1 U1 172.2(11) . . ? C7 O2 C10 107.7(16) . . ? C7 O2 U1 121.3(12) . . ? C10 O2 U1 126.4(13) . . ? C11 O3 C14 107.9(17) . . ? C11 O3 U1 128.3(13) . . ? C14 O3 U1 123.7(13) . . ? C18 O4 C15 106.6(15) . . ? C18 O4 U1 122.9(10) . . ? C15 O4 U1 128.8(12) . . ? O1 U1 O4 81.1(4) . . ? O1 U1 O3 84.1(5) . . ? O4 U1 O3 144.2(4) . . ? O1 U1 O2 95.4(5) . . ? O4 U1 O2 67.2(4) . . ? O3 U1 O2 147.0(4) . . ? O1 U1 I1 179.0(4) . . ? O4 U1 I1 99.9(3) . . ? O3 U1 I1 94.9(3) . . ? O2 U1 I1 85.4(3) . . ? O1 U1 I3 86.0(3) . . ? O4 U1 I3 137.6(3) . . ? O3 U1 I3 72.9(3) . . ? O2 U1 I3 74.1(3) . . ? I1 U1 I3 93.66(5) . . ? O1 U1 I2 92.6(4) . . ? O4 U1 I2 75.0(3) . . ? O3 U1 I2 73.3(3) . . ? O2 U1 I2 139.5(3) . . ? I1 U1 I2 87.14(5) . . ? I3 U1 I2 146.17(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -6(3) . . . . ? O1 C1 C2 C3 -179.2(17) . . . . ? C1 C2 C3 C4 3(3) . . . . ? C2 C3 C4 C5 2(4) . . . . ? C3 C4 C5 C6 -5(4) . . . . ? O1 C1 C6 C5 177(2) . . . . ? C2 C1 C6 C5 4(3) . . . . ? C4 C5 C6 C1 2(4) . . . . ? O2 C7 C8 C9 15(3) . . . . ? C7 C8 C9 C10 -21(3) . . . . ? C8 C9 C10 O2 20(3) . . . . ? O3 C11 C12 C13 36(3) . . . . ? C11 C12 C13 C14 -46(3) . . . . ? C12 C13 C14 O3 42(3) . . . . ? O4 C15 C16 C17 -32(2) . . . . ? C15 C16 C17 C18 36(2) . . . . ? C16 C17 C18 O4 -28(2) . . . . ? C25 C20 C21 C22 6(3) . . . . ? C19 C20 C21 C22 -174.2(19) . . . . ? C20 C21 C22 C23 -14(4) . . . . ? C21 C22 C23 C24 20(5) . . . . ? C22 C23 C24 C25 -18(5) . . . . ? C23 C24 C25 C20 10(4) . . . . ? C21 C20 C25 C24 -4(3) . . . . ? C19 C20 C25 C24 176.3(17) . . . . ? C6 C1 O1 U1 -59(10) . . . . ? C2 C1 O1 U1 114(9) . . . . ? C8 C7 O2 C10 -3(2) . . . . ? C8 C7 O2 U1 -160.7(16) . . . . ? C9 C10 O2 C7 -10(2) . . . . ? C9 C10 O2 U1 145.7(18) . . . . ? C12 C11 O3 C14 -8(3) . . . . ? C12 C11 O3 U1 171.1(15) . . . . ? C13 C14 O3 C11 -23(3) . . . . ? C13 C14 O3 U1 157.5(16) . . . . ? C17 C18 O4 C15 8(2) . . . . ? C17 C18 O4 U1 -158.1(13) . . . . ? C16 C15 O4 C18 15(2) . . . . ? C16 C15 O4 U1 -179.4(13) . . . . ? C1 O1 U1 O4 179(100) . . . . ? C1 O1 U1 O3 -33(9) . . . . ? C1 O1 U1 O2 114(9) . . . . ? C1 O1 U1 I1 -29(27) . . . . ? C1 O1 U1 I3 40(9) . . . . ? C1 O1 U1 I2 -106(9) . . . . ? C18 O4 U1 O1 -172.1(14) . . . . ? C15 O4 U1 O1 24.9(16) . . . . ? C18 O4 U1 O3 121.2(14) . . . . ? C15 O4 U1 O3 -41.8(19) . . . . ? C18 O4 U1 O2 -72.3(13) . . . . ? C15 O4 U1 O2 124.7(17) . . . . ? C18 O4 U1 I1 8.4(14) . . . . ? C15 O4 U1 I1 -154.6(16) . . . . ? C18 O4 U1 I3 -98.2(14) . . . . ? C15 O4 U1 I3 98.7(16) . . . . ? C18 O4 U1 I2 92.8(13) . . . . ? C15 O4 U1 I2 -70.3(16) . . . . ? C11 O3 U1 O1 2.2(17) . . . . ? C14 O3 U1 O1 -178.3(18) . . . . ? C11 O3 U1 O4 68(2) . . . . ? C14 O3 U1 O4 -112.5(18) . . . . ? C11 O3 U1 O2 -88.7(19) . . . . ? C14 O3 U1 O2 91(2) . . . . ? C11 O3 U1 I1 -177.7(17) . . . . ? C14 O3 U1 I1 1.8(18) . . . . ? C11 O3 U1 I3 -85.4(17) . . . . ? C14 O3 U1 I3 94.2(18) . . . . ? C11 O3 U1 I2 96.8(17) . . . . ? C14 O3 U1 I2 -83.7(18) . . . . ? C7 O2 U1 O1 10.3(14) . . . . ? C10 O2 U1 O1 -142.7(14) . . . . ? C7 O2 U1 O4 -67.6(13) . . . . ? C10 O2 U1 O4 139.4(15) . . . . ? C7 O2 U1 O3 97.9(15) . . . . ? C10 O2 U1 O3 -55.1(17) . . . . ? C7 O2 U1 I1 -170.3(13) . . . . ? C10 O2 U1 I1 36.7(13) . . . . ? C7 O2 U1 I3 94.6(13) . . . . ? C10 O2 U1 I3 -58.4(13) . . . . ? C7 O2 U1 I2 -90.2(14) . . . . ? C10 O2 U1 I2 116.8(13) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.725 _refine_diff_density_min -1.340 _refine_diff_density_rms 0.260 #===END=== data_3 _database_code_depnum_ccdc_archive 'CCDC 715607' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H29 I3 O3 U' _chemical_formula_weight 1008.22 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 C2/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 19.332(7) _cell_length_b 12.547(4) _cell_length_c 24.785(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.953(5) _cell_angle_gamma 90.00 _cell_volume 5750(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(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 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3680 _exptl_absorpt_coefficient_mu 8.890 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_T_max 0.533 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22838 _diffrn_reflns_av_R_equivalents 0.0795 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.73 _reflns_number_total 5827 _reflns_number_gt 4322 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+9.9856P] 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 5827 _refine_ls_number_parameters 298 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1421 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.234064(18) 1.06010(3) 0.365668(13) 0.02557(14) Uani 1 1 d . . . I1 I 0.34259(4) 1.12529(6) 0.47480(3) 0.0417(2) Uani 1 1 d . . . I2 I 0.11887(4) 1.01067(6) 0.25673(3) 0.0407(2) Uani 1 1 d . . . I3 I 0.20165(4) 1.29297(6) 0.34089(3) 0.0433(2) Uani 1 1 d . . . O1 O 0.2530(3) 0.8978(5) 0.3821(3) 0.0279(14) Uani 1 1 d . . . O3 O 0.1464(4) 1.0666(5) 0.4160(3) 0.0322(15) Uani 1 1 d U . . O2 O 0.3178(4) 1.0826(6) 0.3128(3) 0.0334(15) Uani 1 1 d U . . C7 C 0.3927(5) 0.8222(7) 0.3702(4) 0.029(2) Uani 1 1 d . . . C1 C 0.2671(5) 0.7950(7) 0.3848(3) 0.026(2) Uani 1 1 d . . . C19 C 0.3733(5) 1.1656(9) 0.3222(4) 0.042(3) Uani 1 1 d U . . H19A H 0.4156 1.1462 0.3528 0.050 Uiso 1 1 calc R . . H19B H 0.3548 1.2332 0.3311 0.050 Uiso 1 1 calc R . . C13 C 0.1486(5) 0.7553(7) 0.4074(4) 0.030(2) Uani 1 1 d . . . C2 C 0.3326(5) 0.7533(8) 0.3765(3) 0.029(2) Uani 1 1 d . . . C23 C 0.1550(6) 1.0168(9) 0.4708(4) 0.036(2) Uani 1 1 d U . . H23A H 0.2030 1.0299 0.4960 0.043 Uiso 1 1 calc R . . H23B H 0.1473 0.9405 0.4668 0.043 Uiso 1 1 calc R . . C18 C 0.0962(5) 0.8106(8) 0.3663(4) 0.032(2) Uani 1 1 d . . . H18 H 0.1060 0.8319 0.3333 0.038 Uiso 1 1 calc R . . C6 C 0.2180(5) 0.7202(8) 0.3980(4) 0.031(2) Uani 1 1 d . . . C5 C 0.2344(6) 0.6118(8) 0.3998(4) 0.038(2) Uani 1 1 d . . . H5 H 0.2022 0.5647 0.4087 0.046 Uiso 1 1 calc R . . C4 C 0.2931(5) 0.5714(9) 0.3898(4) 0.036(2) Uani 1 1 d . . . H4 H 0.3012 0.4983 0.3908 0.044 Uiso 1 1 calc R . . C16 C 0.0131(5) 0.8019(9) 0.4209(4) 0.040(3) Uani 1 1 d . . . H16 H -0.0323 0.8171 0.4248 0.048 Uiso 1 1 calc R . . C12 C 0.4285(6) 0.7995(9) 0.3306(4) 0.038(2) Uani 1 1 d . . . H12 H 0.4100 0.7469 0.3039 0.046 Uiso 1 1 calc R . . C8 C 0.4200(5) 0.9046(8) 0.4089(4) 0.035(2) Uani 1 1 d . . . H8 H 0.3960 0.9228 0.4351 0.042 Uiso 1 1 calc R . . C11 C 0.4901(5) 0.8518(10) 0.3296(5) 0.044(3) Uani 1 1 d . . . H11 H 0.5137 0.8342 0.3031 0.053 Uiso 1 1 calc R . . C3 C 0.3424(6) 0.6431(8) 0.3774(4) 0.037(2) Uani 1 1 d . . . H3 H 0.3832 0.6159 0.3695 0.044 Uiso 1 1 calc R . . C17 C 0.0309(5) 0.8340(8) 0.3738(4) 0.037(2) Uani 1 1 d . . . H17 H -0.0026 0.8728 0.3462 0.045 Uiso 1 1 calc R . . C9 C 0.4817(6) 0.9587(9) 0.4084(4) 0.042(3) Uani 1 1 d . . . H9 H 0.4995 1.0128 0.4344 0.051 Uiso 1 1 calc R . . C21 C 0.3791(6) 1.0649(10) 0.2434(4) 0.045(3) Uani 1 1 d U . . H21A H 0.4213 1.0201 0.2581 0.054 Uiso 1 1 calc R . . H21B H 0.3676 1.0681 0.2026 0.054 Uiso 1 1 calc R . . C10 C 0.5171(6) 0.9324(9) 0.3693(5) 0.045(3) Uani 1 1 d . . . H10 H 0.5591 0.9685 0.3693 0.054 Uiso 1 1 calc R . . C26 C 0.0815(6) 1.1327(10) 0.4010(5) 0.048(3) Uani 1 1 d U . . H26A H 0.0527 1.1187 0.3625 0.058 Uiso 1 1 calc R . . H26B H 0.0942 1.2077 0.4045 0.058 Uiso 1 1 calc R . . C14 C 0.1308(6) 0.7227(8) 0.4561(4) 0.037(2) Uani 1 1 d . . . H14 H 0.1641 0.6850 0.4843 0.044 Uiso 1 1 calc R . . C15 C 0.0625(7) 0.7475(9) 0.4616(5) 0.047(3) Uani 1 1 d . . . H15 H 0.0508 0.7262 0.4938 0.056 Uiso 1 1 calc R . . C22 C 0.3164(6) 1.0251(10) 0.2610(4) 0.044(3) Uani 1 1 d U . . H22A H 0.2715 1.0389 0.2318 0.053 Uiso 1 1 calc R . . H22B H 0.3206 0.9490 0.2680 0.053 Uiso 1 1 calc R . . C24 C 0.0997(7) 1.0669(10) 0.4923(5) 0.049(3) Uani 1 1 d U . . H24A H 0.1199 1.1272 0.5162 0.059 Uiso 1 1 calc R . . H24B H 0.0811 1.0162 0.5141 0.059 Uiso 1 1 calc R . . C25 C 0.0408(7) 1.1029(11) 0.4415(5) 0.055(3) Uani 1 1 d U . . H25A H 0.0067 1.0458 0.4267 0.066 Uiso 1 1 calc R . . H25B H 0.0150 1.1636 0.4504 0.066 Uiso 1 1 calc R . . C20 C 0.3908(8) 1.1717(11) 0.2683(5) 0.061(3) Uani 1 1 d U . . H20A H 0.3598 1.2231 0.2434 0.073 Uiso 1 1 calc R . . H20B H 0.4407 1.1933 0.2747 0.073 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 0.0285(2) 0.0238(2) 0.0235(2) 0.00110(14) 0.00624(15) -0.00151(14) I1 0.0392(4) 0.0460(5) 0.0338(4) -0.0121(3) 0.0009(3) -0.0030(3) I2 0.0405(4) 0.0454(5) 0.0286(3) 0.0081(3) -0.0018(3) -0.0130(3) I3 0.0472(5) 0.0256(4) 0.0581(4) 0.0072(3) 0.0167(3) 0.0007(3) O1 0.026(3) 0.020(4) 0.035(3) -0.005(3) 0.007(3) -0.006(3) O3 0.037(4) 0.033(4) 0.027(3) 0.006(3) 0.010(3) 0.006(3) O2 0.032(4) 0.040(4) 0.027(3) -0.007(3) 0.007(3) -0.005(3) C7 0.025(5) 0.025(5) 0.032(5) 0.003(4) 0.002(4) 0.003(4) C1 0.031(5) 0.029(6) 0.012(4) -0.001(4) -0.003(3) 0.002(4) C19 0.027(5) 0.051(7) 0.052(6) -0.016(5) 0.020(5) -0.021(5) C13 0.045(6) 0.021(5) 0.024(4) -0.002(4) 0.010(4) -0.005(4) C2 0.031(5) 0.031(6) 0.019(4) -0.006(4) -0.002(4) 0.002(4) C23 0.037(5) 0.043(6) 0.030(5) 0.006(4) 0.012(4) 0.003(4) C18 0.035(6) 0.031(6) 0.026(5) -0.001(4) 0.005(4) -0.013(4) C6 0.044(6) 0.023(5) 0.020(4) 0.001(4) -0.001(4) -0.002(4) C5 0.041(6) 0.034(6) 0.027(5) 0.000(4) -0.009(4) -0.002(5) C4 0.034(6) 0.034(6) 0.034(5) -0.008(4) -0.002(4) -0.004(5) C16 0.027(6) 0.048(7) 0.044(6) -0.012(5) 0.011(5) -0.003(5) C12 0.043(6) 0.035(6) 0.035(5) 0.002(5) 0.008(5) 0.009(5) C8 0.037(6) 0.029(6) 0.039(6) 0.004(5) 0.010(5) 0.005(5) C11 0.027(6) 0.055(8) 0.052(7) 0.009(6) 0.015(5) 0.004(5) C3 0.039(6) 0.032(6) 0.031(5) -0.002(4) -0.002(4) 0.011(5) C17 0.031(6) 0.038(6) 0.039(6) -0.002(5) 0.005(4) 0.003(5) C9 0.047(7) 0.033(6) 0.039(6) -0.004(5) 0.000(5) -0.005(5) C21 0.035(6) 0.070(8) 0.029(5) -0.009(5) 0.006(4) 0.004(5) C10 0.030(6) 0.045(7) 0.058(7) 0.019(6) 0.010(5) -0.003(5) C26 0.049(7) 0.060(8) 0.042(6) 0.015(5) 0.021(5) 0.018(5) C14 0.045(6) 0.031(6) 0.033(5) 0.007(4) 0.009(5) -0.006(5) C15 0.063(8) 0.038(7) 0.044(6) -0.001(5) 0.023(6) -0.012(6) C22 0.052(7) 0.049(7) 0.033(5) -0.009(5) 0.013(5) -0.004(5) C24 0.063(7) 0.049(8) 0.042(5) 0.005(5) 0.027(5) 0.008(5) C25 0.052(7) 0.063(8) 0.059(7) 0.013(6) 0.031(5) 0.015(6) C20 0.067(8) 0.060(7) 0.070(7) -0.008(6) 0.042(7) -0.015(6) _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 2.088(7) . ? U1 O2 2.378(6) . ? U1 O3 2.382(6) . ? U1 I1 3.0128(10) . ? U1 I3 3.0137(13) . ? U1 I2 3.0211(10) . ? O1 C1 1.315(11) . ? O3 C26 1.458(12) . ? O3 C23 1.459(11) . ? O2 C19 1.464(11) . ? O2 C22 1.465(11) . ? C7 C12 1.385(13) . ? C7 C8 1.403(13) . ? C7 C2 1.493(13) . ? C1 C2 1.439(13) . ? C1 C6 1.440(13) . ? C19 C20 1.473(15) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C13 C18 1.395(13) . ? C13 C14 1.409(12) . ? C13 C6 1.492(14) . ? C2 C3 1.395(14) . ? C23 C24 1.467(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C18 C17 1.360(13) . ? C18 H18 0.9300 . ? C6 C5 1.394(14) . ? C5 C4 1.332(14) . ? C5 H5 0.9300 . ? C4 C3 1.408(14) . ? C4 H4 0.9300 . ? C16 C15 1.354(16) . ? C16 C17 1.370(14) . ? C16 H16 0.9300 . ? C12 C11 1.366(14) . ? C12 H12 0.9300 . ? C8 C9 1.375(15) . ? C8 H8 0.9300 . ? C11 C10 1.400(16) . ? C11 H11 0.9300 . ? C3 H3 0.9300 . ? C17 H17 0.9300 . ? C9 C10 1.380(15) . ? C9 H9 0.9300 . ? C21 C20 1.465(16) . ? C21 C22 1.490(15) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C10 H10 0.9300 . ? C26 C25 1.493(14) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C14 C15 1.402(15) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C24 C25 1.500(17) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 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 O2 96.6(2) . . ? O1 U1 O3 92.4(2) . . ? O2 U1 O3 171.0(2) . . ? O1 U1 I1 93.01(17) . . ? O2 U1 I1 93.14(16) . . ? O3 U1 I1 86.32(16) . . ? O1 U1 I3 178.20(16) . . ? O2 U1 I3 84.66(17) . . ? O3 U1 I3 86.33(16) . . ? I1 U1 I3 88.21(3) . . ? O1 U1 I2 90.93(17) . . ? O2 U1 I2 88.55(16) . . ? O3 U1 I2 91.36(16) . . ? I1 U1 I2 175.51(2) . . ? I3 U1 I2 87.80(2) . . ? C1 O1 U1 170.9(6) . . ? C26 O3 C23 109.7(7) . . ? C26 O3 U1 125.2(5) . . ? C23 O3 U1 124.6(5) . . ? C19 O2 C22 108.4(7) . . ? C19 O2 U1 125.5(5) . . ? C22 O2 U1 125.6(6) . . ? C12 C7 C8 118.0(9) . . ? C12 C7 C2 121.3(9) . . ? C8 C7 C2 120.3(8) . . ? O1 C1 C2 121.8(8) . . ? O1 C1 C6 120.7(8) . . ? C2 C1 C6 117.5(9) . . ? O2 C19 C20 104.1(8) . . ? O2 C19 H19A 110.9 . . ? C20 C19 H19A 110.9 . . ? O2 C19 H19B 110.9 . . ? C20 C19 H19B 110.9 . . ? H19A C19 H19B 109.0 . . ? C18 C13 C14 117.6(9) . . ? C18 C13 C6 121.9(8) . . ? C14 C13 C6 120.1(9) . . ? C3 C2 C1 118.7(9) . . ? C3 C2 C7 118.0(9) . . ? C1 C2 C7 123.2(9) . . ? O3 C23 C24 104.9(8) . . ? O3 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? O3 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.8 . . ? C17 C18 C13 120.9(9) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C5 C6 C1 119.0(9) . . ? C5 C6 C13 119.3(9) . . ? C1 C6 C13 121.7(9) . . ? C4 C5 C6 124.3(11) . . ? C4 C5 H5 117.8 . . ? C6 C5 H5 117.8 . . ? C5 C4 C3 117.7(10) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C15 C16 C17 119.0(10) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C11 C12 C7 122.1(10) . . ? C11 C12 H12 118.9 . . ? C7 C12 H12 118.9 . . ? C9 C8 C7 120.8(9) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C12 C11 C10 118.8(10) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C2 C3 C4 122.6(10) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C18 C17 C16 121.8(10) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C8 C9 C10 119.8(10) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C20 C21 C22 102.8(9) . . ? C20 C21 H21A 111.2 . . ? C22 C21 H21A 111.2 . . ? C20 C21 H21B 111.2 . . ? C22 C21 H21B 111.2 . . ? H21A C21 H21B 109.1 . . ? C9 C10 C11 120.4(10) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? O3 C26 C25 105.6(8) . . ? O3 C26 H26A 110.6 . . ? C25 C26 H26A 110.6 . . ? O3 C26 H26B 110.6 . . ? C25 C26 H26B 110.6 . . ? H26A C26 H26B 108.8 . . ? C15 C14 C13 119.4(9) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 121.3(10) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? O2 C22 C21 106.4(9) . . ? O2 C22 H22A 110.4 . . ? C21 C22 H22A 110.4 . . ? O2 C22 H22B 110.4 . . ? C21 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? C23 C24 C25 106.2(9) . . ? C23 C24 H24A 110.5 . . ? C25 C24 H24A 110.5 . . ? C23 C24 H24B 110.5 . . ? C25 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? C26 C25 C24 102.7(9) . . ? C26 C25 H25A 111.2 . . ? C24 C25 H25A 111.2 . . ? C26 C25 H25B 111.2 . . ? C24 C25 H25B 111.2 . . ? H25A C25 H25B 109.1 . . ? C21 C20 C19 106.7(10) . . ? C21 C20 H20A 110.4 . . ? C19 C20 H20A 110.4 . . ? C21 C20 H20B 110.4 . . ? C19 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 U1 O1 C1 -32(4) . . . . ? O3 U1 O1 C1 149(4) . . . . ? I1 U1 O1 C1 -125(4) . . . . ? I3 U1 O1 C1 102(6) . . . . ? I2 U1 O1 C1 57(4) . . . . ? O1 U1 O3 C26 -145.0(8) . . . . ? O2 U1 O3 C26 35.3(17) . . . . ? I1 U1 O3 C26 122.1(8) . . . . ? I3 U1 O3 C26 33.7(8) . . . . ? I2 U1 O3 C26 -54.0(8) . . . . ? O1 U1 O3 C23 44.2(7) . . . . ? O2 U1 O3 C23 -135.5(13) . . . . ? I1 U1 O3 C23 -48.6(7) . . . . ? I3 U1 O3 C23 -137.1(7) . . . . ? I2 U1 O3 C23 135.2(7) . . . . ? O1 U1 O2 C19 -129.8(8) . . . . ? O3 U1 O2 C19 49.9(16) . . . . ? I1 U1 O2 C19 -36.4(7) . . . . ? I3 U1 O2 C19 51.5(7) . . . . ? I2 U1 O2 C19 139.5(7) . . . . ? O1 U1 O2 C22 58.8(8) . . . . ? O3 U1 O2 C22 -121.5(14) . . . . ? I1 U1 O2 C22 152.2(8) . . . . ? I3 U1 O2 C22 -119.9(8) . . . . ? I2 U1 O2 C22 -32.0(8) . . . . ? U1 O1 C1 C2 52(4) . . . . ? U1 O1 C1 C6 -130(4) . . . . ? C22 O2 C19 C20 13.4(12) . . . . ? U1 O2 C19 C20 -159.2(8) . . . . ? O1 C1 C2 C3 -177.2(8) . . . . ? C6 C1 C2 C3 4.9(12) . . . . ? O1 C1 C2 C7 6.4(12) . . . . ? C6 C1 C2 C7 -171.5(8) . . . . ? C12 C7 C2 C3 45.4(12) . . . . ? C8 C7 C2 C3 -127.1(10) . . . . ? C12 C7 C2 C1 -138.2(9) . . . . ? C8 C7 C2 C1 49.3(12) . . . . ? C26 O3 C23 C24 -8.2(12) . . . . ? U1 O3 C23 C24 163.8(7) . . . . ? C14 C13 C18 C17 1.4(14) . . . . ? C6 C13 C18 C17 174.4(9) . . . . ? O1 C1 C6 C5 179.3(8) . . . . ? C2 C1 C6 C5 -2.7(12) . . . . ? O1 C1 C6 C13 2.1(12) . . . . ? C2 C1 C6 C13 -180.0(8) . . . . ? C18 C13 C6 C5 -119.1(10) . . . . ? C14 C13 C6 C5 53.7(12) . . . . ? C18 C13 C6 C1 58.1(12) . . . . ? C14 C13 C6 C1 -129.0(9) . . . . ? C1 C6 C5 C4 -0.3(14) . . . . ? C13 C6 C5 C4 177.0(9) . . . . ? C6 C5 C4 C3 1.1(14) . . . . ? C8 C7 C12 C11 2.4(15) . . . . ? C2 C7 C12 C11 -170.3(9) . . . . ? C12 C7 C8 C9 -2.0(14) . . . . ? C2 C7 C8 C9 170.7(9) . . . . ? C7 C12 C11 C10 -1.2(16) . . . . ? C1 C2 C3 C4 -4.3(13) . . . . ? C7 C2 C3 C4 172.3(8) . . . . ? C5 C4 C3 C2 1.3(14) . . . . ? C13 C18 C17 C16 -1.9(15) . . . . ? C15 C16 C17 C18 1.6(16) . . . . ? C7 C8 C9 C10 0.5(16) . . . . ? C8 C9 C10 C11 0.7(16) . . . . ? C12 C11 C10 C9 -0.3(16) . . . . ? C23 O3 C26 C25 -12.8(12) . . . . ? U1 O3 C26 C25 175.3(7) . . . . ? C18 C13 C14 C15 -0.6(14) . . . . ? C6 C13 C14 C15 -173.7(9) . . . . ? C17 C16 C15 C14 -0.7(17) . . . . ? C13 C14 C15 C16 0.3(16) . . . . ? C19 O2 C22 C21 7.7(12) . . . . ? U1 O2 C22 C21 -179.7(6) . . . . ? C20 C21 C22 O2 -25.6(12) . . . . ? O3 C23 C24 C25 26.0(13) . . . . ? O3 C26 C25 C24 27.9(13) . . . . ? C23 C24 C25 C26 -33.5(13) . . . . ? C22 C21 C20 C19 34.6(13) . . . . ? O2 C19 C20 C21 -30.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 5.918 _refine_diff_density_min -1.783 _refine_diff_density_rms 0.330 #===END=== data_5 _database_code_depnum_ccdc_archive 'CCDC 715608' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H50 I2 O5 U' _chemical_formula_weight 1006.55 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 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, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.0285(16) _cell_length_b 13.3321(9) _cell_length_c 23.6112(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7249.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 6.216 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.187 _exptl_absorpt_correction_T_max 0.314 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57858 _diffrn_reflns_av_R_equivalents 0.1855 _diffrn_reflns_av_sigmaI/netI 0.1489 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.73 _reflns_number_total 7636 _reflns_number_gt 4042 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^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 7636 _refine_ls_number_parameters 362 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1670 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.982 _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 0.07956(2) 0.07630(4) 0.34578(2) 0.02448(15) Uani 1 1 d . . . I1 I 0.08772(4) 0.25502(7) 0.25918(4) 0.0385(3) Uani 1 1 d . . . I2 I 0.13825(5) -0.02363(9) 0.45187(4) 0.0512(3) Uani 1 1 d . . . O1 O 0.1226(4) -0.0150(7) 0.2899(3) 0.032(2) Uani 1 1 d . . . C14 C -0.0785(5) 0.3940(8) 0.4634(5) 0.021(3) Uani 1 1 d . . . O5 O -0.0100(4) 0.0683(7) 0.2862(4) 0.034(2) Uani 1 1 d U . . O4 O 0.0186(4) -0.0703(7) 0.3694(4) 0.044(2) Uani 1 1 d U . . O2 O 0.0278(4) 0.1682(7) 0.3963(3) 0.028(2) Uani 1 1 d . . . O3 O 0.1666(4) 0.1722(7) 0.3697(4) 0.035(2) Uani 1 1 d U . . C11 C -0.0070(5) 0.2433(9) 0.4181(5) 0.019(3) Uiso 1 1 d . . . C1 C 0.1528(6) -0.0810(9) 0.2541(5) 0.026(3) Uani 1 1 d . . . C7 C 0.2439(6) -0.2881(11) 0.1440(5) 0.033(3) Uani 1 1 d . . . C17 C -0.1195(6) 0.4731(10) 0.4887(5) 0.028(3) Uani 1 1 d . . . C16 C -0.0487(6) 0.2204(9) 0.4574(6) 0.028(3) Uani 1 1 d . . . H16 H -0.0534 0.1543 0.4691 0.034 Uiso 1 1 calc R . . C15 C -0.0834(6) 0.2933(10) 0.4797(5) 0.027(3) Uani 1 1 d . . . H15 H -0.1112 0.2756 0.5065 0.032 Uiso 1 1 calc R . . C4 C 0.2112(6) -0.2146(9) 0.1823(5) 0.026(3) Uani 1 1 d . . . C13 C -0.0359(6) 0.4141(9) 0.4226(5) 0.027(3) Uani 1 1 d . . . H13 H -0.0318 0.4796 0.4096 0.032 Uiso 1 1 calc R . . C19 C -0.1024(7) 0.5784(11) 0.4694(6) 0.049(4) Uani 1 1 d . . . H19A H -0.1234 0.6273 0.4911 0.073 Uiso 1 1 calc R . . H19B H -0.1115 0.5863 0.4300 0.073 Uiso 1 1 calc R . . H19C H -0.0614 0.5879 0.4750 0.073 Uiso 1 1 calc R . . C12 C 0.0001(6) 0.3416(10) 0.4009(5) 0.027(3) Uani 1 1 d . . . H12 H 0.0290 0.3584 0.3750 0.032 Uiso 1 1 calc R . . C3 C 0.1545(6) -0.1838(11) 0.1718(6) 0.035(4) Uani 1 1 d . . . H3 H 0.1357 -0.2090 0.1400 0.042 Uiso 1 1 calc R . . C20 C -0.1828(6) 0.4516(11) 0.4711(6) 0.039(4) Uani 1 1 d . . . H20A H -0.2081 0.4993 0.4888 0.059 Uiso 1 1 calc R . . H20B H -0.1933 0.3850 0.4827 0.059 Uiso 1 1 calc R . . H20C H -0.1862 0.4570 0.4307 0.059 Uiso 1 1 calc R . . C18 C -0.1153(6) 0.4671(10) 0.5535(5) 0.033(3) Uani 1 1 d . . . H18A H -0.0767 0.4851 0.5653 0.049 Uiso 1 1 calc R . . H18B H -0.1236 0.3999 0.5657 0.049 Uiso 1 1 calc R . . H18C H -0.1427 0.5125 0.5702 0.049 Uiso 1 1 calc R . . C6 C 0.2075(6) -0.1096(12) 0.2646(6) 0.040(4) Uani 1 1 d . . . H6 H 0.2260 -0.0860 0.2970 0.048 Uiso 1 1 calc R . . C2 C 0.1251(6) -0.1189(10) 0.2056(6) 0.033(4) Uani 1 1 d . . . H2 H 0.0874 -0.0998 0.1968 0.040 Uiso 1 1 calc R . . C9 C 0.2678(7) -0.3744(11) 0.1801(7) 0.049(4) Uani 1 1 d . . . H9A H 0.2954 -0.4122 0.1583 0.073 Uiso 1 1 calc R . . H9B H 0.2365 -0.4174 0.1914 0.073 Uiso 1 1 calc R . . H9C H 0.2866 -0.3476 0.2131 0.073 Uiso 1 1 calc R . . C29 C -0.0109(6) 0.0240(12) 0.2306(6) 0.044(4) Uani 1 1 d U . . H29A H -0.0094 -0.0486 0.2330 0.053 Uiso 1 1 calc R . . H29B H 0.0217 0.0472 0.2081 0.053 Uiso 1 1 calc R . . C24 C 0.2269(6) 0.1500(13) 0.3564(7) 0.051(4) Uani 1 1 d U . . H24A H 0.2342 0.1602 0.3163 0.061 Uiso 1 1 calc R . . H24B H 0.2359 0.0809 0.3657 0.061 Uiso 1 1 calc R . . C5 C 0.2366(6) -0.1720(11) 0.2294(6) 0.040(4) Uani 1 1 d . . . H5 H 0.2753 -0.1866 0.2372 0.049 Uiso 1 1 calc R . . C30 C -0.0692(7) 0.0589(12) 0.2042(7) 0.055(4) Uani 1 1 d U . . H30A H -0.0633 0.1145 0.1783 0.066 Uiso 1 1 calc R . . H30B H -0.0882 0.0045 0.1842 0.066 Uiso 1 1 calc R . . C25 C 0.0328(7) -0.1731(11) 0.3592(7) 0.051(4) Uani 1 1 d U . . H25A H 0.0725 -0.1865 0.3706 0.061 Uiso 1 1 calc R . . H25B H 0.0290 -0.1883 0.3192 0.061 Uiso 1 1 calc R . . C23 C 0.2628(7) 0.2191(13) 0.3905(8) 0.060(5) Uani 1 1 d U . . H23A H 0.2851 0.1824 0.4186 0.073 Uiso 1 1 calc R . . H23B H 0.2894 0.2564 0.3666 0.073 Uiso 1 1 calc R . . C10 C 0.2935(7) -0.2298(13) 0.1172(7) 0.058(5) Uani 1 1 d . . . H10A H 0.3175 -0.2747 0.0956 0.087 Uiso 1 1 calc R . . H10B H 0.3164 -0.1989 0.1464 0.087 Uiso 1 1 calc R . . H10C H 0.2781 -0.1790 0.0927 0.087 Uiso 1 1 calc R . . C8 C 0.2068(7) -0.3328(12) 0.0972(6) 0.054(5) Uani 1 1 d . . . H8A H 0.1960 -0.2811 0.0710 0.081 Uiso 1 1 calc R . . H8B H 0.1724 -0.3618 0.1134 0.081 Uiso 1 1 calc R . . H8C H 0.2284 -0.3838 0.0778 0.081 Uiso 1 1 calc R . . C31 C -0.1032(7) 0.0902(13) 0.2536(7) 0.059(4) Uani 1 1 d U . . H31A H -0.1319 0.1402 0.2431 0.070 Uiso 1 1 calc R . . H31B H -0.1230 0.0333 0.2705 0.070 Uiso 1 1 calc R . . C32 C -0.0604(6) 0.1320(15) 0.2923(7) 0.059(5) Uani 1 1 d U . . H32A H -0.0512 0.2007 0.2823 0.071 Uiso 1 1 calc R . . H32B H -0.0746 0.1305 0.3310 0.071 Uiso 1 1 calc R . . C21 C 0.1674(7) 0.2542(13) 0.4084(8) 0.064(5) Uani 1 1 d U . . H21A H 0.1446 0.3090 0.3933 0.077 Uiso 1 1 calc R . . H21B H 0.1502 0.2337 0.4441 0.077 Uiso 1 1 calc R . . C27 C -0.0493(8) -0.1622(14) 0.4174(8) 0.068(5) Uani 1 1 d U . . H27A H -0.0886 -0.1770 0.4053 0.081 Uiso 1 1 calc R . . H27B H -0.0479 -0.1650 0.4584 0.081 Uiso 1 1 calc R . . C28 C -0.0331(9) -0.0697(14) 0.3990(11) 0.096(7) Uani 1 1 d U . . H28A H -0.0293 -0.0254 0.4314 0.115 Uiso 1 1 calc R . . H28B H -0.0634 -0.0429 0.3748 0.115 Uiso 1 1 calc R . . C22 C 0.2220(8) 0.2851(17) 0.4173(10) 0.103(7) Uani 1 1 d U . . H22A H 0.2296 0.2874 0.4577 0.123 Uiso 1 1 calc R . . H22B H 0.2267 0.3524 0.4023 0.123 Uiso 1 1 calc R . . C26 C -0.0082(8) -0.2356(12) 0.3928(7) 0.054(4) Uani 1 1 d U . . H26A H -0.0284 -0.2832 0.3687 0.065 Uiso 1 1 calc R . . H26B H 0.0121 -0.2720 0.4223 0.065 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 0.0266(3) 0.0220(3) 0.0248(2) -0.0035(2) 0.0013(2) 0.0029(3) I1 0.0394(6) 0.0388(6) 0.0372(5) 0.0116(4) 0.0043(5) 0.0018(5) I2 0.0532(7) 0.0581(7) 0.0425(6) 0.0217(6) -0.0117(5) -0.0096(6) O1 0.031(6) 0.040(6) 0.024(5) -0.009(4) 0.006(4) 0.002(5) C14 0.020(7) 0.018(7) 0.023(6) 0.004(5) -0.005(6) 0.002(6) O5 0.028(5) 0.047(6) 0.028(5) -0.002(4) -0.002(4) -0.002(5) O4 0.036(6) 0.034(5) 0.063(7) 0.011(5) 0.004(5) -0.001(5) O2 0.026(5) 0.032(6) 0.026(5) -0.006(4) 0.005(4) -0.003(4) O3 0.036(5) 0.022(5) 0.047(6) -0.003(4) -0.009(5) 0.001(4) C1 0.033(8) 0.017(7) 0.028(7) -0.014(6) 0.017(6) -0.007(6) C7 0.033(9) 0.044(9) 0.021(7) -0.006(6) 0.001(6) 0.007(7) C17 0.035(9) 0.031(8) 0.017(6) 0.005(6) 0.005(6) 0.003(7) C16 0.035(9) 0.016(7) 0.033(8) 0.000(6) 0.001(7) -0.006(6) C15 0.031(8) 0.036(8) 0.013(6) 0.002(5) 0.007(6) 0.005(7) C4 0.023(8) 0.028(8) 0.027(7) -0.004(6) 0.008(6) 0.002(6) C13 0.032(8) 0.015(7) 0.033(7) 0.011(6) -0.011(6) -0.005(6) C19 0.070(12) 0.032(9) 0.045(9) -0.007(8) 0.007(8) 0.023(9) C12 0.018(8) 0.028(8) 0.033(8) 0.004(6) 0.006(6) 0.007(6) C3 0.031(9) 0.044(9) 0.029(8) -0.017(7) 0.000(6) -0.006(7) C20 0.029(9) 0.042(10) 0.046(9) -0.020(7) 0.011(7) 0.005(7) C18 0.043(9) 0.029(8) 0.027(7) 0.003(6) 0.007(7) 0.017(7) C6 0.024(9) 0.063(11) 0.034(8) -0.005(8) -0.001(7) 0.008(8) C2 0.025(8) 0.040(9) 0.035(8) -0.015(7) -0.001(7) 0.002(7) C9 0.041(10) 0.043(10) 0.063(11) -0.018(9) -0.001(8) 0.026(8) C29 0.047(8) 0.045(9) 0.040(8) -0.013(7) -0.013(7) 0.006(7) C24 0.032(7) 0.058(10) 0.063(11) -0.011(7) 0.004(7) -0.016(7) C5 0.025(9) 0.058(11) 0.039(9) 0.002(8) 0.003(7) 0.002(8) C30 0.063(10) 0.052(10) 0.050(8) -0.014(8) -0.030(7) 0.002(8) C25 0.068(10) 0.030(7) 0.053(10) -0.009(7) 0.001(7) -0.024(7) C23 0.037(7) 0.053(11) 0.091(13) -0.007(9) -0.021(8) -0.006(7) C10 0.054(11) 0.078(13) 0.043(10) -0.015(9) 0.008(9) 0.023(10) C8 0.050(11) 0.062(12) 0.049(10) -0.029(9) -0.001(9) 0.015(9) C31 0.035(7) 0.077(12) 0.064(10) -0.012(9) -0.024(7) 0.005(8) C32 0.024(8) 0.108(14) 0.045(9) -0.024(8) -0.015(7) 0.018(8) C21 0.052(8) 0.050(10) 0.090(13) -0.036(8) -0.015(9) -0.008(8) C27 0.062(11) 0.067(10) 0.075(12) 0.022(9) 0.010(8) -0.020(8) C28 0.073(12) 0.052(8) 0.162(18) 0.020(12) 0.058(11) -0.006(10) C22 0.055(10) 0.124(16) 0.130(17) -0.079(12) 0.020(12) -0.030(10) C26 0.074(11) 0.042(7) 0.046(9) 0.014(7) -0.014(8) -0.022(7) _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 2.051(8) . ? U1 O2 2.084(8) . ? U1 O3 2.443(9) . ? U1 O4 2.470(10) . ? U1 O5 2.499(9) . ? U1 I2 3.1428(11) . ? U1 I1 3.1454(10) . ? O1 C1 1.403(14) . ? C14 C13 1.400(17) . ? C14 C15 1.402(17) . ? C14 C17 1.537(17) . ? O5 C29 1.440(15) . ? O5 C32 1.445(17) . ? O4 C28 1.379(19) . ? O4 C25 1.430(17) . ? O2 C11 1.383(14) . ? O3 C21 1.425(17) . ? O3 C24 1.455(16) . ? C11 C16 1.369(17) . ? C11 C12 1.382(17) . ? C1 C6 1.340(18) . ? C1 C2 1.405(17) . ? C7 C8 1.519(18) . ? C7 C10 1.52(2) . ? C7 C4 1.532(18) . ? C7 C9 1.533(19) . ? C17 C19 1.529(19) . ? C17 C18 1.536(17) . ? C17 C20 1.541(18) . ? C16 C15 1.363(17) . ? C16 H16 0.9300 . ? C15 H15 0.9300 . ? C4 C5 1.379(18) . ? C4 C3 1.391(18) . ? C13 C12 1.373(17) . ? C13 H13 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C12 H12 0.9300 . ? C3 C2 1.357(17) . ? C3 H3 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C6 C5 1.354(19) . ? C6 H6 0.9300 . ? C2 H2 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C29 C30 1.551(19) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C24 C23 1.48(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C5 H5 0.9300 . ? C30 C31 1.46(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C25 C26 1.49(2) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C23 C22 1.44(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C31 C32 1.46(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C21 C22 1.34(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C27 C28 1.36(2) . ? C27 C26 1.48(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 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 O2 173.5(3) . . ? O1 U1 O3 93.6(3) . . ? O2 U1 O3 91.7(3) . . ? O1 U1 O4 87.2(3) . . ? O2 U1 O4 90.6(3) . . ? O3 U1 O4 145.9(3) . . ? O1 U1 O5 90.7(3) . . ? O2 U1 O5 82.8(3) . . ? O3 U1 O5 146.0(3) . . ? O4 U1 O5 67.9(3) . . ? O1 U1 I2 93.0(2) . . ? O2 U1 I2 92.3(2) . . ? O3 U1 I2 71.6(2) . . ? O4 U1 I2 74.3(2) . . ? O5 U1 I2 141.8(2) . . ? O1 U1 I1 90.2(3) . . ? O2 U1 I1 87.7(2) . . ? O3 U1 I1 72.9(2) . . ? O4 U1 I1 141.3(2) . . ? O5 U1 I1 73.5(2) . . ? I2 U1 I1 144.44(3) . . ? C1 O1 U1 176.9(8) . . ? C13 C14 C15 115.4(11) . . ? C13 C14 C17 124.6(11) . . ? C15 C14 C17 120.0(11) . . ? C29 O5 C32 108.7(10) . . ? C29 O5 U1 122.9(8) . . ? C32 O5 U1 125.5(8) . . ? C28 O4 C25 106.8(13) . . ? C28 O4 U1 126.9(10) . . ? C25 O4 U1 126.1(9) . . ? C11 O2 U1 166.2(8) . . ? C21 O3 C24 106.4(11) . . ? C21 O3 U1 124.1(9) . . ? C24 O3 U1 128.8(8) . . ? C16 C11 C12 119.7(12) . . ? C16 C11 O2 119.8(11) . . ? C12 C11 O2 120.5(11) . . ? C6 C1 O1 122.2(12) . . ? C6 C1 C2 118.3(12) . . ? O1 C1 C2 119.5(12) . . ? C8 C7 C10 108.8(12) . . ? C8 C7 C4 113.8(12) . . ? C10 C7 C4 106.8(12) . . ? C8 C7 C9 108.1(13) . . ? C10 C7 C9 110.2(12) . . ? C4 C7 C9 109.1(11) . . ? C19 C17 C18 109.2(12) . . ? C19 C17 C14 110.8(11) . . ? C18 C17 C14 108.2(10) . . ? C19 C17 C20 109.5(12) . . ? C18 C17 C20 108.7(11) . . ? C14 C17 C20 110.4(11) . . ? C15 C16 C11 120.8(12) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C16 C15 C14 122.0(12) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C5 C4 C3 114.9(12) . . ? C5 C4 C7 122.0(12) . . ? C3 C4 C7 123.1(12) . . ? C12 C13 C14 123.0(12) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C12 C11 119.1(12) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C2 C3 C4 123.4(13) . . ? C2 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 C6 C5 121.8(14) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C3 C2 C1 118.9(13) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O5 C29 C30 104.8(11) . . ? O5 C29 H29A 110.8 . . ? C30 C29 H29A 110.8 . . ? O5 C29 H29B 110.8 . . ? C30 C29 H29B 110.8 . . ? H29A C29 H29B 108.9 . . ? O3 C24 C23 106.8(13) . . ? O3 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? O3 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C6 C5 C4 122.6(14) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C31 C30 C29 103.3(12) . . ? C31 C30 H30A 111.1 . . ? C29 C30 H30A 111.1 . . ? C31 C30 H30B 111.1 . . ? C29 C30 H30B 111.1 . . ? H30A C30 H30B 109.1 . . ? O4 C25 C26 107.6(13) . . ? O4 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O4 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C22 C23 C24 104.8(14) . . ? C22 C23 H23A 110.8 . . ? C24 C23 H23A 110.8 . . ? C22 C23 H23B 110.8 . . ? C24 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C32 C31 C30 104.3(13) . . ? C32 C31 H31A 110.9 . . ? C30 C31 H31A 110.9 . . ? C32 C31 H31B 110.9 . . ? C30 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? O5 C32 C31 104.8(13) . . ? O5 C32 H32A 110.8 . . ? C31 C32 H32A 110.8 . . ? O5 C32 H32B 110.8 . . ? C31 C32 H32B 110.8 . . ? H32A C32 H32B 108.9 . . ? C22 C21 O3 110.5(15) . . ? C22 C21 H21A 109.6 . . ? O3 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? O3 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C28 C27 C26 107.4(16) . . ? C28 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? C28 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C27 C28 O4 113.2(17) . . ? C27 C28 H28A 108.9 . . ? O4 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? O4 C28 H28B 108.9 . . ? H28A C28 H28B 107.8 . . ? C21 C22 C23 110.9(16) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.0 . . ? C27 C26 C25 104.1(13) . . ? C27 C26 H26A 110.9 . . ? C25 C26 H26A 110.9 . . ? C27 C26 H26B 110.9 . . ? C25 C26 H26B 110.9 . . ? H26A C26 H26B 109.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 U1 O1 C1 -128(14) . . . . ? O3 U1 O1 C1 88(15) . . . . ? O4 U1 O1 C1 -58(15) . . . . ? O5 U1 O1 C1 -126(15) . . . . ? I2 U1 O1 C1 16(15) . . . . ? I1 U1 O1 C1 161(15) . . . . ? O1 U1 O5 C29 -9.0(10) . . . . ? O2 U1 O5 C29 170.8(10) . . . . ? O3 U1 O5 C29 88.5(11) . . . . ? O4 U1 O5 C29 -95.7(10) . . . . ? I2 U1 O5 C29 -104.7(10) . . . . ? I1 U1 O5 C29 81.0(10) . . . . ? O1 U1 O5 C32 -167.7(12) . . . . ? O2 U1 O5 C32 12.0(11) . . . . ? O3 U1 O5 C32 -70.2(13) . . . . ? O4 U1 O5 C32 105.6(12) . . . . ? I2 U1 O5 C32 96.5(12) . . . . ? I1 U1 O5 C32 -77.7(11) . . . . ? O1 U1 O4 C28 -166.2(16) . . . . ? O2 U1 O4 C28 7.7(16) . . . . ? O3 U1 O4 C28 101.6(16) . . . . ? O5 U1 O4 C28 -74.3(15) . . . . ? I2 U1 O4 C28 99.9(15) . . . . ? I1 U1 O4 C28 -79.5(16) . . . . ? O1 U1 O4 C25 19.7(11) . . . . ? O2 U1 O4 C25 -166.5(11) . . . . ? O3 U1 O4 C25 -72.6(13) . . . . ? O5 U1 O4 C25 111.5(11) . . . . ? I2 U1 O4 C25 -74.3(11) . . . . ? I1 U1 O4 C25 106.4(10) . . . . ? O1 U1 O2 C11 -59(5) . . . . ? O3 U1 O2 C11 85(3) . . . . ? O4 U1 O2 C11 -129(3) . . . . ? O5 U1 O2 C11 -61(3) . . . . ? I2 U1 O2 C11 157(3) . . . . ? I1 U1 O2 C11 13(3) . . . . ? O1 U1 O3 C21 179.1(12) . . . . ? O2 U1 O3 C21 2.9(12) . . . . ? O4 U1 O3 C21 -90.6(13) . . . . ? O5 U1 O3 C21 82.5(13) . . . . ? I2 U1 O3 C21 -88.9(12) . . . . ? I1 U1 O3 C21 90.0(12) . . . . ? O1 U1 O3 C24 -11.8(12) . . . . ? O2 U1 O3 C24 172.0(11) . . . . ? O4 U1 O3 C24 78.5(13) . . . . ? O5 U1 O3 C24 -108.4(11) . . . . ? I2 U1 O3 C24 80.2(11) . . . . ? I1 U1 O3 C24 -100.9(11) . . . . ? U1 O2 C11 C16 147(3) . . . . ? U1 O2 C11 C12 -33(4) . . . . ? U1 O1 C1 C6 -54(16) . . . . ? U1 O1 C1 C2 126(15) . . . . ? C13 C14 C17 C19 -7.5(17) . . . . ? C15 C14 C17 C19 174.4(12) . . . . ? C13 C14 C17 C18 -127.2(13) . . . . ? C15 C14 C17 C18 54.7(16) . . . . ? C13 C14 C17 C20 114.0(14) . . . . ? C15 C14 C17 C20 -64.1(15) . . . . ? C12 C11 C16 C15 0.3(19) . . . . ? O2 C11 C16 C15 179.9(11) . . . . ? C11 C16 C15 C14 0(2) . . . . ? C13 C14 C15 C16 0.4(18) . . . . ? C17 C14 C15 C16 178.7(12) . . . . ? C8 C7 C4 C5 175.4(14) . . . . ? C10 C7 C4 C5 -64.6(16) . . . . ? C9 C7 C4 C5 54.6(17) . . . . ? C8 C7 C4 C3 -6(2) . . . . ? C10 C7 C4 C3 113.7(15) . . . . ? C9 C7 C4 C3 -127.2(14) . . . . ? C15 C14 C13 C12 -1.9(18) . . . . ? C17 C14 C13 C12 179.9(12) . . . . ? C14 C13 C12 C11 2.6(19) . . . . ? C16 C11 C12 C13 -1.7(19) . . . . ? O2 C11 C12 C13 178.7(11) . . . . ? C5 C4 C3 C2 -2(2) . . . . ? C7 C4 C3 C2 179.9(13) . . . . ? O1 C1 C6 C5 -178.9(13) . . . . ? C2 C1 C6 C5 1(2) . . . . ? C4 C3 C2 C1 -1(2) . . . . ? C6 C1 C2 C3 1(2) . . . . ? O1 C1 C2 C3 -179.0(12) . . . . ? C32 O5 C29 C30 -4.4(16) . . . . ? U1 O5 C29 C30 -166.3(9) . . . . ? C21 O3 C24 C23 2.4(18) . . . . ? U1 O3 C24 C23 -168.2(10) . . . . ? C1 C6 C5 C4 -4(2) . . . . ? C3 C4 C5 C6 4(2) . . . . ? C7 C4 C5 C6 -177.8(14) . . . . ? O5 C29 C30 C31 -18.5(17) . . . . ? C28 O4 C25 C26 -9.4(19) . . . . ? U1 O4 C25 C26 165.7(9) . . . . ? O3 C24 C23 C22 -6(2) . . . . ? C29 C30 C31 C32 34.3(18) . . . . ? C29 O5 C32 C31 26.1(17) . . . . ? U1 O5 C32 C31 -172.7(10) . . . . ? C30 C31 C32 O5 -37.8(18) . . . . ? C24 O3 C21 C22 3(2) . . . . ? U1 O3 C21 C22 173.8(16) . . . . ? C26 C27 C28 O4 -7(3) . . . . ? C25 O4 C28 C27 10(3) . . . . ? U1 O4 C28 C27 -164.7(14) . . . . ? O3 C21 C22 C23 -7(3) . . . . ? C24 C23 C22 C21 8(3) . . . . ? C28 C27 C26 C25 0(2) . . . . ? O4 C25 C26 C27 5.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.567 _refine_diff_density_min -2.139 _refine_diff_density_rms 0.241 #===END=== data_6 _database_code_depnum_ccdc_archive 'CCDC 715609' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;Uranium(IV) diiodo bis(2,6-dimethylphenol) tris(tetrahydrofuran) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H58 I2 O7 U' _chemical_formula_weight 1094.65 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.6892(18) _cell_length_b 11.8797(15) _cell_length_c 24.995(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.130(3) _cell_angle_gamma 90.00 _cell_volume 4058.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 5.562 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.20432 _exptl_absorpt_correction_T_max 0.30886 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14998 _diffrn_reflns_av_R_equivalents 0.1242 _diffrn_reflns_av_sigmaI/netI 0.1377 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.51 _reflns_number_total 4075 _reflns_number_gt 2525 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^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 4075 _refine_ls_number_parameters 211 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.915 _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 C1 C 0.3978(8) 0.8603(10) 0.8729(4) 0.031(3) Uani 1 1 d . . . C2 C 0.3160(8) 0.7963(9) 0.8849(4) 0.028(3) Uani 1 1 d . . . C3 C 0.2720(9) 0.8182(11) 0.9330(5) 0.043(3) Uani 1 1 d . . . H3 H 0.2181 0.7758 0.9419 0.052 Uiso 1 1 calc R . . C4 C 0.3067(10) 0.9009(11) 0.9674(5) 0.044(3) Uani 1 1 d . . . H4 H 0.2760 0.9153 0.9990 0.053 Uiso 1 1 calc R . . C5 C 0.3862(10) 0.9614(11) 0.9548(5) 0.046(3) Uani 1 1 d . . . H5 H 0.4088 1.0178 0.9781 0.055 Uiso 1 1 calc R . . C6 C 0.4356(8) 0.9421(9) 0.9080(5) 0.033(3) Uani 1 1 d . . . C7 C 0.2765(8) 0.7048(10) 0.8475(5) 0.037(3) Uani 1 1 d . . . H7A H 0.2489 0.7383 0.8151 0.056 Uiso 1 1 calc R . . H7B H 0.2269 0.6631 0.8646 0.056 Uiso 1 1 calc R . . H7C H 0.3287 0.6550 0.8390 0.056 Uiso 1 1 calc R . . C8 C 0.5270(8) 1.0115(11) 0.8970(5) 0.044(3) Uani 1 1 d . . . H8A H 0.5306 1.0758 0.9202 0.066 Uiso 1 1 calc R . . H8B H 0.5232 1.0361 0.8603 0.066 Uiso 1 1 calc R . . H8C H 0.5843 0.9659 0.9034 0.066 Uiso 1 1 calc R . . C9 C 0.3795(8) 0.5639(10) 0.7220(5) 0.039(3) Uani 1 1 d . . . H9A H 0.4104 0.5257 0.7527 0.047 Uiso 1 1 calc R . . H9B H 0.3200 0.5996 0.7327 0.047 Uiso 1 1 calc R . . C10 C 0.3581(11) 0.4849(12) 0.6785(6) 0.063(4) Uani 1 1 d . . . H10A H 0.2951 0.4490 0.6821 0.076 Uiso 1 1 calc R . . H10B H 0.4083 0.4275 0.6775 0.076 Uiso 1 1 calc R . . C11 C 0.3569(11) 0.5579(12) 0.6294(5) 0.059(4) Uani 1 1 d . . . H11A H 0.3706 0.5141 0.5980 0.071 Uiso 1 1 calc R . . H11B H 0.2942 0.5950 0.6234 0.071 Uiso 1 1 calc R . . C12 C 0.4367(9) 0.6422(10) 0.6421(5) 0.039(3) Uani 1 1 d . . . H12A H 0.4976 0.6178 0.6278 0.046 Uiso 1 1 calc R . . H12B H 0.4193 0.7151 0.6271 0.046 Uiso 1 1 calc R . . C13 C 0.4214(7) 1.1052(9) 0.7686(6) 0.035(3) Uani 1 1 d . . . H13A H 0.4006 1.0802 0.8032 0.042 Uiso 1 1 calc R . . H13B H 0.3654 1.1052 0.7431 0.042 Uiso 1 1 calc R . . C14 C 0.4681(8) 1.2215(9) 0.7728(5) 0.043(3) Uani 1 1 d . . . H14A H 0.4191 1.2805 0.7692 0.052 Uiso 1 1 calc R . . H14B H 0.5057 1.2308 0.8066 0.052 Uiso 1 1 calc R . . C15 C 0.4098(18) 0.621(3) 0.4194(11) 0.186(10) Uani 1 1 d U . . H15A H 0.3938 0.5417 0.4211 0.224 Uiso 1 1 calc R . . H15B H 0.4053 0.6446 0.3822 0.224 Uiso 1 1 calc R . . C16 C 0.3466(18) 0.683(3) 0.4484(10) 0.158(9) Uani 1 1 d U . . H16A H 0.3340 0.7552 0.4317 0.190 Uiso 1 1 calc R . . H16B H 0.2850 0.6431 0.4507 0.190 Uiso 1 1 calc R . . C17 C 0.3892(17) 0.695(2) 0.4961(9) 0.136(8) Uani 1 1 d U . . H17A H 0.3615 0.6429 0.5209 0.163 Uiso 1 1 calc R . . H17B H 0.3778 0.7712 0.5089 0.163 Uiso 1 1 calc R . . C18 C 0.4878(18) 0.677(2) 0.4944(10) 0.148(8) Uani 1 1 d U . . H18A H 0.5092 0.6197 0.5202 0.177 Uiso 1 1 calc R . . H18B H 0.5242 0.7454 0.5022 0.177 Uiso 1 1 calc R . . I1 I 0.71114(5) 0.87295(7) 0.79931(3) 0.0376(3) Uani 1 1 d . . . O1 O 0.4397(5) 0.8427(6) 0.8246(3) 0.0264(17) Uani 1 1 d . . . O2 O 0.4464(5) 0.6482(6) 0.7007(3) 0.0287(18) Uani 1 1 d . . . O3 O 0.5000 1.0329(9) 0.7500 0.032(3) Uani 1 2 d S . . O4 O 0.5015(12) 0.640(2) 0.4412(8) 0.190(8) Uani 1 1 d U . . U1 U 0.5000 0.82468(5) 0.7500 0.02357(19) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(6) 0.047(8) 0.018(6) 0.006(5) 0.001(5) 0.008(5) C2 0.030(6) 0.029(7) 0.027(6) 0.006(5) 0.007(5) 0.004(5) C3 0.036(7) 0.058(9) 0.036(8) 0.010(7) 0.008(6) 0.007(6) C4 0.053(8) 0.048(9) 0.033(8) -0.002(7) 0.011(7) 0.016(7) C5 0.064(9) 0.042(8) 0.030(8) -0.004(6) -0.003(7) 0.015(7) C6 0.037(6) 0.032(7) 0.030(7) -0.001(6) -0.008(6) 0.003(5) C7 0.040(7) 0.028(7) 0.044(8) -0.005(6) 0.008(6) -0.007(5) C8 0.032(7) 0.063(9) 0.036(8) -0.022(7) -0.004(6) -0.003(6) C9 0.042(7) 0.024(7) 0.051(9) 0.008(6) -0.004(6) -0.009(5) C10 0.079(11) 0.044(9) 0.068(11) -0.008(8) 0.000(9) -0.041(8) C11 0.090(11) 0.051(9) 0.036(8) -0.003(7) -0.001(8) -0.036(8) C12 0.054(8) 0.029(7) 0.032(7) -0.005(5) -0.001(6) -0.007(6) C13 0.018(5) 0.027(7) 0.061(9) -0.005(6) 0.003(6) -0.003(5) C14 0.040(7) 0.011(5) 0.078(11) -0.007(6) 0.000(6) 0.002(5) C15 0.104(13) 0.33(3) 0.123(16) -0.087(17) -0.051(13) 0.076(16) C16 0.105(11) 0.26(2) 0.106(15) -0.037(17) -0.027(12) 0.065(16) C17 0.124(14) 0.20(2) 0.086(12) -0.008(14) -0.008(11) 0.030(16) C18 0.109(12) 0.21(2) 0.114(14) -0.028(16) -0.041(12) -0.005(16) I1 0.0243(4) 0.0372(5) 0.0506(6) 0.0014(4) -0.0032(4) 0.0001(3) O1 0.030(4) 0.018(4) 0.031(5) 0.003(3) -0.003(3) 0.000(3) O2 0.036(4) 0.018(4) 0.032(5) -0.005(3) 0.005(4) -0.008(3) O3 0.019(5) 0.026(6) 0.053(8) 0.000 0.005(5) 0.000 O4 0.083(9) 0.34(2) 0.141(13) -0.063(15) -0.015(10) 0.029(12) U1 0.0203(3) 0.0211(3) 0.0293(4) 0.000 0.0012(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 C1 O1 1.379(13) . ? C1 C6 1.391(15) . ? C1 C2 1.399(15) . ? C2 C3 1.400(16) . ? C2 C7 1.514(15) . ? C3 C4 1.374(17) . ? C3 H3 0.9300 . ? C4 C5 1.355(18) . ? C4 H4 0.9300 . ? C5 C6 1.401(17) . ? C5 H5 0.9300 . ? C6 C8 1.536(16) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.452(17) . ? C9 O2 1.475(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.503(19) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.503(16) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.464(14) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O3 1.472(12) . ? C13 C14 1.524(15) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C14 1.48(2) 2_656 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O4 1.36(3) . ? C15 C16 1.37(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.31(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.37(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.42(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? I1 U1 3.1326(8) . ? O1 U1 2.092(8) . ? O2 U1 2.521(7) . ? O3 C13 1.472(12) 2_656 ? O3 U1 2.473(10) . ? U1 O1 2.092(8) 2_656 ? U1 O2 2.521(7) 2_656 ? U1 I1 3.1326(8) 2_656 ? 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 C1 C6 120.0(10) . . ? O1 C1 C2 118.7(10) . . ? C6 C1 C2 121.3(11) . . ? C1 C2 C3 118.1(11) . . ? C1 C2 C7 121.4(10) . . ? C3 C2 C7 120.5(11) . . ? C4 C3 C2 121.3(12) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.3(13) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.5(12) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 117.5(11) . . ? C1 C6 C8 122.7(11) . . ? C5 C6 C8 119.9(11) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 O2 105.9(10) . . ? C10 C9 H9A 110.6 . . ? O2 C9 H9A 110.6 . . ? C10 C9 H9B 110.6 . . ? O2 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C9 C10 C11 103.3(11) . . ? C9 C10 H10A 111.1 . . ? C11 C10 H10A 111.1 . . ? C9 C10 H10B 111.1 . . ? C11 C10 H10B 111.1 . . ? H10A C10 H10B 109.1 . . ? C12 C11 C10 103.7(10) . . ? C12 C11 H11A 111.0 . . ? C10 C11 H11A 111.0 . . ? C12 C11 H11B 111.0 . . ? C10 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? O2 C12 C11 105.6(10) . . ? O2 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? O2 C12 H12B 110.6 . . ? C11 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? O3 C13 C14 103.9(8) . . ? O3 C13 H13A 111.0 . . ? C14 C13 H13A 111.0 . . ? O3 C13 H13B 111.0 . . ? C14 C13 H13B 111.0 . . ? H13A C13 H13B 109.0 . . ? C14 C14 C13 102.2(8) 2_656 . ? C14 C14 H14A 111.3 2_656 . ? C13 C14 H14A 111.3 . . ? C14 C14 H14B 111.3 2_656 . ? C13 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? O4 C15 C16 107(2) . . ? O4 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O4 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C17 C16 C15 106(2) . . ? C17 C16 H16A 110.4 . . ? C15 C16 H16A 110.4 . . ? C17 C16 H16B 110.4 . . ? C15 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? C16 C17 C18 110(2) . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.2 . . ? C17 C18 O4 105.1(19) . . ? C17 C18 H18A 110.7 . . ? O4 C18 H18A 110.7 . . ? C17 C18 H18B 110.7 . . ? O4 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? C1 O1 U1 176.8(6) . . ? C12 O2 C9 107.6(8) . . ? C12 O2 U1 122.5(6) . . ? C9 O2 U1 123.9(7) . . ? C13 O3 C13 108.6(11) 2_656 . ? C13 O3 U1 125.7(5) 2_656 . ? C13 O3 U1 125.7(5) . . ? C15 O4 C18 105(2) . . ? O1 U1 O1 168.2(4) 2_656 . ? O1 U1 O3 84.12(18) 2_656 . ? O1 U1 O3 84.12(18) . . ? O1 U1 O2 76.6(3) 2_656 . ? O1 U1 O2 113.7(3) . . ? O3 U1 O2 146.28(17) . . ? O1 U1 O2 113.7(3) 2_656 2_656 ? O1 U1 O2 76.6(2) . 2_656 ? O3 U1 O2 146.28(17) . 2_656 ? O2 U1 O2 67.4(3) . 2_656 ? O1 U1 I1 86.06(18) 2_656 . ? O1 U1 I1 91.79(18) . . ? O3 U1 I1 79.451(19) . . ? O2 U1 I1 125.61(17) . . ? O2 U1 I1 73.88(17) 2_656 . ? O1 U1 I1 91.79(18) 2_656 2_656 ? O1 U1 I1 86.06(18) . 2_656 ? O3 U1 I1 79.451(19) . 2_656 ? O2 U1 I1 73.88(17) . 2_656 ? O2 U1 I1 125.61(17) 2_656 2_656 ? I1 U1 I1 158.90(4) . 2_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -177.5(9) . . . . ? C6 C1 C2 C3 1.1(16) . . . . ? O1 C1 C2 C7 3.3(15) . . . . ? C6 C1 C2 C7 -178.1(10) . . . . ? C1 C2 C3 C4 0.8(17) . . . . ? C7 C2 C3 C4 -179.9(11) . . . . ? C2 C3 C4 C5 -1.0(18) . . . . ? C3 C4 C5 C6 -0.7(19) . . . . ? O1 C1 C6 C5 175.9(10) . . . . ? C2 C1 C6 C5 -2.7(16) . . . . ? O1 C1 C6 C8 -3.3(16) . . . . ? C2 C1 C6 C8 178.1(10) . . . . ? C4 C5 C6 C1 2.6(17) . . . . ? C4 C5 C6 C8 -178.3(11) . . . . ? O2 C9 C10 C11 -34.6(14) . . . . ? C9 C10 C11 C12 36.7(16) . . . . ? C10 C11 C12 O2 -24.9(15) . . . . ? O3 C13 C14 C14 35.8(13) . . . 2_656 ? O4 C15 C16 C17 -26(4) . . . . ? C15 C16 C17 C18 19(4) . . . . ? C16 C17 C18 O4 -6(4) . . . . ? C6 C1 O1 U1 -71(12) . . . . ? C2 C1 O1 U1 108(12) . . . . ? C11 C12 O2 C9 4.0(13) . . . . ? C11 C12 O2 U1 -149.7(8) . . . . ? C10 C9 O2 C12 19.4(13) . . . . ? C10 C9 O2 U1 172.7(8) . . . . ? C14 C13 O3 C13 -13.4(6) . . . 2_656 ? C14 C13 O3 U1 166.6(6) . . . . ? C16 C15 O4 C18 22(4) . . . . ? C17 C18 O4 C15 -10(4) . . . . ? C1 O1 U1 O1 27(12) . . . 2_656 ? C1 O1 U1 O3 27(12) . . . . ? C1 O1 U1 O2 -123(12) . . . . ? C1 O1 U1 O2 179(100) . . . 2_656 ? C1 O1 U1 I1 106(12) . . . . ? C1 O1 U1 I1 -53(12) . . . 2_656 ? C13 O3 U1 O1 -40.6(7) 2_656 . . 2_656 ? C13 O3 U1 O1 139.4(7) . . . 2_656 ? C13 O3 U1 O1 139.4(7) 2_656 . . . ? C13 O3 U1 O1 -40.6(7) . . . . ? C13 O3 U1 O2 -95.6(7) 2_656 . . . ? C13 O3 U1 O2 84.4(7) . . . . ? C13 O3 U1 O2 84.4(7) 2_656 . . 2_656 ? C13 O3 U1 O2 -95.6(7) . . . 2_656 ? C13 O3 U1 I1 46.4(6) 2_656 . . . ? C13 O3 U1 I1 -133.6(6) . . . . ? C13 O3 U1 I1 -133.6(6) 2_656 . . 2_656 ? C13 O3 U1 I1 46.4(6) . . . 2_656 ? C12 O2 U1 O1 -25.1(8) . . . 2_656 ? C9 O2 U1 O1 -174.5(8) . . . 2_656 ? C12 O2 U1 O1 149.0(8) . . . . ? C9 O2 U1 O1 -0.5(8) . . . . ? C12 O2 U1 O3 31.7(10) . . . . ? C9 O2 U1 O3 -117.7(7) . . . . ? C12 O2 U1 O2 -148.3(10) . . . 2_656 ? C9 O2 U1 O2 62.3(7) . . . 2_656 ? C12 O2 U1 I1 -100.1(8) . . . . ? C9 O2 U1 I1 110.4(7) . . . . ? C12 O2 U1 I1 70.8(8) . . . 2_656 ? C9 O2 U1 I1 -78.7(7) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.166 _refine_diff_density_min -3.350 _refine_diff_density_rms 0.305 #===END=== data_7 _database_code_depnum_ccdc_archive 'CCDC 715610' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 F10 I2 O5.50 U' _chemical_formula_weight 1110.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.613(3) _cell_length_b 10.9881(16) _cell_length_c 14.154(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.465(3) _cell_angle_gamma 90.00 _cell_volume 3339.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green_Blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 6.799 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.22701 _exptl_absorpt_correction_T_max 0.31183 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14985 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 23.96 _reflns_number_total 4916 _reflns_number_gt 3326 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^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 4916 _refine_ls_number_parameters 394 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0698 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _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 O6 O 0.033(3) 0.041(4) 0.438(4) 0.27(3) Uiso 0.50 1 d PD A -1 C25 C 0.055(2) -0.039(5) 0.512(5) 0.15(3) Uiso 0.50 1 d PD A -1 C26 C 0.013(4) -0.001(6) 0.585(3) 0.16(3) Uiso 0.50 1 d PD A -1 C27 C -0.046(3) 0.024(8) 0.522(5) 0.14(2) Uiso 0.50 1 d PD A -1 C28 C -0.032(3) 0.036(5) 0.421(4) 0.14(2) Uiso 0.50 1 d PD A -1 C1 C 0.1385(5) 0.9283(9) 0.9979(8) 0.032(3) Uani 1 1 d . . . C2 C 0.0831(5) 0.8921(9) 0.9496(9) 0.040(3) Uani 1 1 d . . . C3 C 0.0336(6) 0.8625(10) 0.9972(10) 0.049(3) Uani 1 1 d . . . C4 C 0.0374(5) 0.8717(10) 1.0963(10) 0.045(3) Uani 1 1 d . . . C5 C 0.0925(5) 0.9090(10) 1.1433(9) 0.039(3) Uani 1 1 d . . . C6 C 0.1425(4) 0.9379(9) 1.0950(9) 0.032(3) Uani 1 1 d . . . C7 C 0.3906(4) 1.0441(9) 0.7508(7) 0.030(3) Uani 1 1 d . . . C8 C 0.4258(5) 0.9538(9) 0.7150(7) 0.031(3) Uani 1 1 d . . . C9 C 0.4744(5) 0.9763(9) 0.6604(8) 0.037(3) Uani 1 1 d . . . C10 C 0.4872(5) 1.0936(11) 0.6368(8) 0.043(3) Uani 1 1 d . . . C11 C 0.4520(5) 1.1853(9) 0.6679(8) 0.035(3) Uani 1 1 d . . . C12 C 0.4057(5) 1.1622(9) 0.7251(8) 0.035(3) Uani 1 1 d . . . C13 C 0.4201(4) 0.9496(8) 1.0014(8) 0.031(3) Uani 1 1 d . . . H13A H 0.4247 1.0364 0.9919 0.037 Uiso 1 1 calc R . . H13B H 0.4405 0.9064 0.9537 0.037 Uiso 1 1 calc R . . C14 C 0.4469(4) 0.9129(10) 1.1001(8) 0.037(3) Uani 1 1 d . . . H14A H 0.4597 0.8282 1.1020 0.045 Uiso 1 1 calc R . . H14B H 0.4824 0.9633 1.1227 0.045 Uiso 1 1 calc R . . C15 C 0.3938(5) 0.9330(9) 1.1579(8) 0.036(3) Uani 1 1 d . . . H15A H 0.3883 1.0188 1.1710 0.043 Uiso 1 1 calc R . . H15B H 0.3996 0.8884 1.2173 0.043 Uiso 1 1 calc R . . C16 C 0.3376(5) 0.8813(10) 1.0894(8) 0.041(3) Uani 1 1 d . . . H16A H 0.3344 0.7937 1.0954 0.049 Uiso 1 1 calc R . . H16B H 0.2986 0.9183 1.1020 0.049 Uiso 1 1 calc R . . C17 C 0.3201(5) 0.6795(9) 0.8910(9) 0.048(3) Uani 1 1 d . . . H17A H 0.3515 0.6757 0.9456 0.058 Uiso 1 1 calc R . . H17B H 0.3390 0.7122 0.8375 0.058 Uiso 1 1 calc R . . C18 C 0.2944(7) 0.5581(11) 0.8684(12) 0.089(5) Uani 1 1 d . . . H18A H 0.3232 0.4957 0.8946 0.107 Uiso 1 1 calc R . . H18B H 0.2870 0.5470 0.8001 0.107 Uiso 1 1 calc R . . C19 C 0.2346(6) 0.5500(9) 0.9116(9) 0.050(3) Uani 1 1 d . . . H19A H 0.2413 0.5167 0.9754 0.060 Uiso 1 1 calc R . . H19B H 0.2046 0.4996 0.8733 0.060 Uiso 1 1 calc R . . C20 C 0.2129(5) 0.6803(9) 0.9131(8) 0.038(3) Uani 1 1 d . . . H20A H 0.1834 0.6973 0.8578 0.046 Uiso 1 1 calc R . . H20B H 0.1929 0.6961 0.9699 0.046 Uiso 1 1 calc R . . C21 C 0.1437(5) 1.1687(11) 0.8128(9) 0.055(4) Uani 1 1 d . . . H21A H 0.1443 1.2030 0.8760 0.066 Uiso 1 1 calc R . . H21B H 0.1156 1.0997 0.8071 0.066 Uiso 1 1 calc R . . C22 C 0.1241(6) 1.2627(11) 0.7381(8) 0.060(4) Uani 1 1 d . . . H22A H 0.0796 1.2587 0.7192 0.072 Uiso 1 1 calc R . . H22B H 0.1347 1.3439 0.7614 0.072 Uiso 1 1 calc R . . C23 C 0.1597(5) 1.2307(10) 0.6564(9) 0.050(3) Uani 1 1 d . . . H23A H 0.1630 1.2997 0.6145 0.059 Uiso 1 1 calc R . . H23B H 0.1409 1.1627 0.6200 0.059 Uiso 1 1 calc R . . C24 C 0.2223(4) 1.1967(8) 0.7090(7) 0.028(2) Uiso 1 1 d . . . H24A H 0.2454 1.1440 0.6705 0.034 Uiso 1 1 calc R . . H24B H 0.2470 1.2687 0.7263 0.034 Uiso 1 1 calc R . . F1 F 0.0767(3) 0.8777(6) 0.8544(5) 0.0564(18) Uani 1 1 d . . . F2 F -0.0217(3) 0.8276(7) 0.9494(5) 0.067(2) Uani 1 1 d . . . F3 F -0.0116(3) 0.8468(7) 1.1419(6) 0.074(2) Uani 1 1 d . . . F4 F 0.0983(3) 0.9181(6) 1.2399(5) 0.0592(19) Uani 1 1 d . . . F5 F 0.1955(3) 0.9749(5) 1.1449(4) 0.0444(16) Uani 1 1 d . . . F6 F 0.4143(3) 0.8364(5) 0.7394(5) 0.0510(17) Uani 1 1 d . . . F7 F 0.5079(3) 0.8845(6) 0.6318(5) 0.0595(19) Uani 1 1 d . . . F8 F 0.5333(3) 1.1188(6) 0.5843(5) 0.0576(19) Uani 1 1 d . . . F9 F 0.4651(3) 1.3023(5) 0.6464(5) 0.0541(18) Uani 1 1 d . . . F10 F 0.3734(3) 1.2544(5) 0.7578(5) 0.0490(17) Uani 1 1 d . . . I1 I 0.21904(4) 0.85574(7) 0.68719(5) 0.0478(2) Uani 1 1 d . . . I2 I 0.29955(4) 1.20919(6) 0.99753(6) 0.0434(2) Uani 1 1 d . . . O1 O 0.1887(3) 0.9526(6) 0.9501(5) 0.0341(17) Uani 1 1 d . . . O2 O 0.3461(3) 1.0204(6) 0.8049(5) 0.0315(17) Uani 1 1 d . . . O3 O 0.3540(3) 0.9156(5) 0.9962(5) 0.0281(16) Uani 1 1 d . . . O4 O 0.2681(3) 0.7554(6) 0.9120(5) 0.0338(17) Uani 1 1 d . . . O5 O 0.2059(3) 1.1322(6) 0.7946(5) 0.0337(17) Uani 1 1 d . . . U1 U 0.268272(17) 0.97730(3) 0.87795(3) 0.02813(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(7) 0.037(6) 0.028(8) 0.003(5) 0.011(6) 0.004(5) C2 0.040(7) 0.040(7) 0.040(9) 0.007(6) 0.002(6) 0.001(5) C3 0.039(8) 0.042(7) 0.064(10) 0.003(6) -0.005(7) -0.007(6) C4 0.039(8) 0.043(7) 0.055(10) 0.016(6) 0.012(7) 0.005(6) C5 0.041(7) 0.046(7) 0.031(8) 0.002(6) 0.007(6) 0.007(6) C6 0.014(6) 0.037(6) 0.045(9) 0.011(5) -0.001(5) 0.004(4) C7 0.020(5) 0.046(7) 0.022(7) 0.005(5) -0.005(5) -0.005(5) C8 0.037(6) 0.033(6) 0.024(7) 0.003(5) 0.005(5) -0.002(5) C9 0.034(6) 0.036(6) 0.043(8) 0.000(6) 0.012(6) 0.001(5) C10 0.037(7) 0.061(8) 0.033(8) 0.010(6) 0.007(6) -0.008(6) C11 0.024(6) 0.036(6) 0.042(8) 0.015(5) -0.005(5) -0.012(5) C12 0.030(6) 0.033(6) 0.040(8) 0.001(5) -0.001(6) 0.002(5) C13 0.027(6) 0.027(6) 0.039(7) 0.006(5) 0.008(5) -0.005(4) C14 0.023(6) 0.043(7) 0.045(8) 0.003(6) -0.003(5) -0.006(5) C15 0.035(6) 0.040(6) 0.032(7) 0.002(5) -0.005(6) -0.007(5) C16 0.038(7) 0.044(7) 0.043(8) 0.025(6) 0.015(6) 0.020(5) C17 0.044(7) 0.038(7) 0.060(9) 0.002(6) -0.005(6) 0.012(5) C18 0.110(12) 0.036(8) 0.134(16) 0.001(8) 0.064(12) -0.005(8) C19 0.066(8) 0.029(7) 0.059(9) -0.003(6) 0.024(7) 0.003(6) C20 0.047(7) 0.039(6) 0.028(7) 0.007(5) 0.004(6) -0.009(5) C21 0.031(7) 0.061(8) 0.076(10) 0.024(7) 0.014(7) 0.014(6) C22 0.087(10) 0.056(8) 0.038(9) 0.019(6) 0.013(8) 0.035(7) C23 0.050(8) 0.050(7) 0.045(9) 0.008(6) -0.008(7) 0.004(6) F1 0.056(4) 0.070(5) 0.041(5) -0.006(4) -0.004(4) -0.003(4) F2 0.031(4) 0.087(5) 0.080(6) -0.003(4) -0.003(4) -0.014(4) F3 0.039(4) 0.098(6) 0.091(6) 0.018(5) 0.032(4) -0.008(4) F4 0.061(5) 0.072(5) 0.048(5) 0.009(4) 0.025(4) 0.002(4) F5 0.039(4) 0.050(4) 0.044(4) 0.002(3) 0.003(3) 0.001(3) F6 0.056(4) 0.034(4) 0.065(5) -0.005(3) 0.016(4) -0.003(3) F7 0.062(5) 0.058(4) 0.062(5) -0.016(4) 0.026(4) 0.010(4) F8 0.043(4) 0.078(5) 0.056(5) 0.005(4) 0.023(4) -0.014(4) F9 0.055(4) 0.047(4) 0.062(5) 0.015(3) 0.014(4) -0.005(3) F10 0.046(4) 0.033(3) 0.069(5) 0.004(3) 0.010(4) 0.006(3) I1 0.0686(6) 0.0447(5) 0.0292(5) -0.0035(3) 0.0014(4) -0.0048(4) I2 0.0527(5) 0.0345(4) 0.0426(5) -0.0093(3) 0.0026(4) 0.0055(3) O1 0.037(4) 0.039(4) 0.028(5) 0.006(3) 0.010(3) -0.005(3) O2 0.022(4) 0.034(4) 0.038(5) 0.003(3) 0.007(3) -0.004(3) O3 0.026(4) 0.030(4) 0.028(5) 0.011(3) 0.005(3) -0.003(3) O4 0.025(4) 0.026(4) 0.049(5) -0.002(3) 0.001(4) 0.002(3) O5 0.034(4) 0.042(4) 0.027(5) 0.006(3) 0.014(3) 0.005(3) U1 0.0281(2) 0.0289(2) 0.0279(3) 0.00132(19) 0.00515(17) 0.00091(18) _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 O6 C25 1.398(10) . ? O6 C28 1.400(10) . ? C25 C26 1.501(10) . ? C26 C27 1.505(10) . ? C27 C28 1.507(10) . ? C1 O1 1.368(11) . ? C1 C2 1.368(14) . ? C1 C6 1.372(14) . ? C2 F1 1.349(13) . ? C2 C3 1.366(15) . ? C3 F2 1.359(12) . ? C3 C4 1.400(17) . ? C4 F3 1.329(12) . ? C4 C5 1.360(15) . ? C5 F4 1.363(12) . ? C5 C6 1.378(14) . ? C6 F5 1.339(11) . ? C7 O2 1.321(11) . ? C7 C8 1.381(14) . ? C7 C12 1.397(13) . ? C8 F6 1.366(11) . ? C8 C9 1.395(14) . ? C9 F7 1.331(11) . ? C9 C10 1.367(15) . ? C10 F8 1.337(12) . ? C10 C11 1.366(15) . ? C11 F9 1.358(11) . ? C11 C12 1.380(14) . ? C12 F10 1.341(11) . ? C13 O3 1.470(10) . ? C13 C14 1.507(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.499(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.572(14) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O3 1.455(11) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O4 1.456(11) . ? C17 C18 1.466(16) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.493(17) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.508(13) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O4 1.453(11) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 O5 1.453(11) . ? C21 C22 1.504(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.501(15) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.516(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O5 1.481(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? I1 U1 3.0918(9) . ? I2 U1 3.0914(9) . ? O1 U1 2.114(7) . ? O2 U1 2.125(6) . ? O3 U1 2.449(6) . ? O4 U1 2.486(6) . ? O5 U1 2.398(6) . ? 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 C25 O6 C28 111.0(11) . . ? O6 C25 C26 99.2(9) . . ? C25 C26 C27 101(2) . . ? C26 C27 C28 108.6(11) . . ? O6 C28 C27 98.5(9) . . ? O1 C1 C2 120.6(10) . . ? O1 C1 C6 121.1(9) . . ? C2 C1 C6 118.3(10) . . ? F1 C2 C3 117.8(10) . . ? F1 C2 C1 121.2(11) . . ? C3 C2 C1 120.9(11) . . ? F2 C3 C2 121.0(12) . . ? F2 C3 C4 117.9(12) . . ? C2 C3 C4 121.0(11) . . ? F3 C4 C5 121.8(12) . . ? F3 C4 C3 120.7(11) . . ? C5 C4 C3 117.5(11) . . ? C4 C5 F4 119.2(11) . . ? C4 C5 C6 121.3(11) . . ? F4 C5 C6 119.5(10) . . ? F5 C6 C1 120.3(10) . . ? F5 C6 C5 118.7(10) . . ? C1 C6 C5 121.0(10) . . ? O2 C7 C8 122.6(9) . . ? O2 C7 C12 122.7(9) . . ? C8 C7 C12 114.7(10) . . ? F6 C8 C7 117.5(9) . . ? F6 C8 C9 118.5(9) . . ? C7 C8 C9 123.9(9) . . ? F7 C9 C10 120.5(10) . . ? F7 C9 C8 120.3(9) . . ? C10 C9 C8 119.2(10) . . ? F8 C10 C11 120.2(10) . . ? F8 C10 C9 121.0(11) . . ? C11 C10 C9 118.8(10) . . ? F9 C11 C10 119.2(10) . . ? F9 C11 C12 119.3(10) . . ? C10 C11 C12 121.4(10) . . ? F10 C12 C11 120.2(9) . . ? F10 C12 C7 117.8(9) . . ? C11 C12 C7 122.0(10) . . ? O3 C13 C14 104.4(8) . . ? O3 C13 H13A 110.9 . . ? C14 C13 H13A 110.9 . . ? O3 C13 H13B 110.9 . . ? C14 C13 H13B 110.9 . . ? H13A C13 H13B 108.9 . . ? C15 C14 C13 103.2(8) . . ? C15 C14 H14A 111.1 . . ? C13 C14 H14A 111.1 . . ? C15 C14 H14B 111.1 . . ? C13 C14 H14B 111.1 . . ? H14A C14 H14B 109.1 . . ? C14 C15 C16 101.4(8) . . ? C14 C15 H15A 111.5 . . ? C16 C15 H15A 111.5 . . ? C14 C15 H15B 111.5 . . ? C16 C15 H15B 111.5 . . ? H15A C15 H15B 109.3 . . ? O3 C16 C15 102.4(8) . . ? O3 C16 H16A 111.3 . . ? C15 C16 H16A 111.3 . . ? O3 C16 H16B 111.3 . . ? C15 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? O4 C17 C18 106.5(10) . . ? O4 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O4 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 C19 106.8(11) . . ? C17 C18 H18A 110.4 . . ? C19 C18 H18A 110.4 . . ? C17 C18 H18B 110.4 . . ? C19 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C18 C19 C20 103.5(9) . . ? C18 C19 H19A 111.1 . . ? C20 C19 H19A 111.1 . . ? C18 C19 H19B 111.1 . . ? C20 C19 H19B 111.1 . . ? H19A C19 H19B 109.0 . . ? O4 C20 C19 106.3(8) . . ? O4 C20 H20A 110.5 . . ? C19 C20 H20A 110.5 . . ? O4 C20 H20B 110.5 . . ? C19 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? O5 C21 C22 105.0(9) . . ? O5 C21 H21A 110.7 . . ? C22 C21 H21A 110.7 . . ? O5 C21 H21B 110.7 . . ? C22 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C23 C22 C21 104.6(9) . . ? C23 C22 H22A 110.8 . . ? C21 C22 H22A 110.8 . . ? C23 C22 H22B 110.8 . . ? C21 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? C22 C23 C24 100.7(10) . . ? C22 C23 H23A 111.6 . . ? C24 C23 H23A 111.6 . . ? C22 C23 H23B 111.6 . . ? C24 C23 H23B 111.6 . . ? H23A C23 H23B 109.4 . . ? O5 C24 C23 103.7(8) . . ? O5 C24 H24A 111.0 . . ? C23 C24 H24A 111.0 . . ? O5 C24 H24B 111.0 . . ? C23 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? C1 O1 U1 176.0(6) . . ? C7 O2 U1 173.8(6) . . ? C16 O3 C13 110.8(7) . . ? C16 O3 U1 116.7(5) . . ? C13 O3 U1 128.3(5) . . ? C20 O4 C17 109.3(7) . . ? C20 O4 U1 125.3(5) . . ? C17 O4 U1 120.3(6) . . ? C21 O5 C24 108.9(7) . . ? C21 O5 U1 126.1(6) . . ? C24 O5 U1 124.7(5) . . ? O1 U1 O2 174.4(2) . . ? O1 U1 O5 83.4(2) . . ? O2 U1 O5 92.0(2) . . ? O1 U1 O3 103.2(2) . . ? O2 U1 O3 79.3(2) . . ? O5 U1 O3 150.8(2) . . ? O1 U1 O4 76.2(2) . . ? O2 U1 O4 109.3(2) . . ? O5 U1 O4 141.2(2) . . ? O3 U1 O4 67.2(2) . . ? O1 U1 I2 88.90(18) . . ? O2 U1 I2 86.95(18) . . ? O5 U1 I2 76.14(16) . . ? O3 U1 I2 75.64(15) . . ? O4 U1 I2 135.02(16) . . ? O1 U1 I1 98.50(18) . . ? O2 U1 I1 83.36(18) . . ? O5 U1 I1 75.99(16) . . ? O3 U1 I1 129.55(15) . . ? O4 U1 I1 74.80(16) . . ? I2 U1 I1 150.08(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C28 O6 C25 C26 -50(3) . . . . ? O6 C25 C26 C27 37(5) . . . . ? C25 C26 C27 C28 -17(8) . . . . ? C25 O6 C28 C27 38(5) . . . . ? C26 C27 C28 O6 -10(7) . . . . ? O1 C1 C2 F1 0.9(15) . . . . ? C6 C1 C2 F1 -178.2(9) . . . . ? O1 C1 C2 C3 177.1(9) . . . . ? C6 C1 C2 C3 -2.0(16) . . . . ? F1 C2 C3 F2 -4.4(16) . . . . ? C1 C2 C3 F2 179.3(9) . . . . ? F1 C2 C3 C4 178.1(10) . . . . ? C1 C2 C3 C4 1.8(17) . . . . ? F2 C3 C4 F3 0.1(16) . . . . ? C2 C3 C4 F3 177.7(10) . . . . ? F2 C3 C4 C5 -178.7(9) . . . . ? C2 C3 C4 C5 -1.1(17) . . . . ? F3 C4 C5 F4 1.8(16) . . . . ? C3 C4 C5 F4 -179.4(9) . . . . ? F3 C4 C5 C6 -178.1(10) . . . . ? C3 C4 C5 C6 0.7(16) . . . . ? O1 C1 C6 F5 1.9(14) . . . . ? C2 C1 C6 F5 -179.0(9) . . . . ? O1 C1 C6 C5 -177.5(9) . . . . ? C2 C1 C6 C5 1.6(15) . . . . ? C4 C5 C6 F5 179.6(9) . . . . ? F4 C5 C6 F5 -0.3(14) . . . . ? C4 C5 C6 C1 -0.9(16) . . . . ? F4 C5 C6 C1 179.2(9) . . . . ? O2 C7 C8 F6 -1.7(14) . . . . ? C12 C7 C8 F6 178.5(9) . . . . ? O2 C7 C8 C9 -177.8(9) . . . . ? C12 C7 C8 C9 2.4(15) . . . . ? F6 C8 C9 F7 1.0(15) . . . . ? C7 C8 C9 F7 177.1(9) . . . . ? F6 C8 C9 C10 -178.8(10) . . . . ? C7 C8 C9 C10 -2.7(16) . . . . ? F7 C9 C10 F8 0.4(17) . . . . ? C8 C9 C10 F8 -179.8(9) . . . . ? F7 C9 C10 C11 -179.6(10) . . . . ? C8 C9 C10 C11 0.2(16) . . . . ? F8 C10 C11 F9 -1.2(15) . . . . ? C9 C10 C11 F9 178.8(9) . . . . ? F8 C10 C11 C12 -177.6(9) . . . . ? C9 C10 C11 C12 2.4(16) . . . . ? F9 C11 C12 F10 0.9(14) . . . . ? C10 C11 C12 F10 177.3(10) . . . . ? F9 C11 C12 C7 -179.1(9) . . . . ? C10 C11 C12 C7 -2.7(16) . . . . ? O2 C7 C12 F10 0.5(14) . . . . ? C8 C7 C12 F10 -179.7(8) . . . . ? O2 C7 C12 C11 -179.5(9) . . . . ? C8 C7 C12 C11 0.3(14) . . . . ? O3 C13 C14 C15 -32.9(10) . . . . ? C13 C14 C15 C16 42.0(10) . . . . ? C14 C15 C16 O3 -35.6(9) . . . . ? O4 C17 C18 C19 -21.5(15) . . . . ? C17 C18 C19 C20 27.8(15) . . . . ? C18 C19 C20 O4 -23.7(13) . . . . ? O5 C21 C22 C23 27.3(13) . . . . ? C21 C22 C23 C24 -40.2(12) . . . . ? C22 C23 C24 O5 37.9(10) . . . . ? C2 C1 O1 U1 -92(9) . . . . ? C6 C1 O1 U1 87(9) . . . . ? C8 C7 O2 U1 -79(6) . . . . ? C12 C7 O2 U1 101(6) . . . . ? C15 C16 O3 C13 15.9(9) . . . . ? C15 C16 O3 U1 -143.0(6) . . . . ? C14 C13 O3 C16 9.9(10) . . . . ? C14 C13 O3 U1 165.8(6) . . . . ? C19 C20 O4 C17 11.2(11) . . . . ? C19 C20 O4 U1 165.8(7) . . . . ? C18 C17 O4 C20 6.3(13) . . . . ? C18 C17 O4 U1 -149.8(9) . . . . ? C22 C21 O5 C24 -2.9(12) . . . . ? C22 C21 O5 U1 -176.7(7) . . . . ? C23 C24 O5 C21 -22.3(10) . . . . ? C23 C24 O5 U1 151.7(6) . . . . ? C1 O1 U1 O2 -173(8) . . . . ? C1 O1 U1 O5 153(9) . . . . ? C1 O1 U1 O3 -56(9) . . . . ? C1 O1 U1 O4 6(9) . . . . ? C1 O1 U1 I2 -131(9) . . . . ? C1 O1 U1 I1 78(9) . . . . ? C7 O2 U1 O1 -95(6) . . . . ? C7 O2 U1 O5 -61(6) . . . . ? C7 O2 U1 O3 147(6) . . . . ? C7 O2 U1 O4 86(6) . . . . ? C7 O2 U1 I2 -137(6) . . . . ? C7 O2 U1 I1 15(6) . . . . ? C21 O5 U1 O1 2.9(8) . . . . ? C24 O5 U1 O1 -170.0(7) . . . . ? C21 O5 U1 O2 -173.9(8) . . . . ? C24 O5 U1 O2 13.2(7) . . . . ? C21 O5 U1 O3 -102.5(9) . . . . ? C24 O5 U1 O3 84.6(8) . . . . ? C21 O5 U1 O4 61.2(9) . . . . ? C24 O5 U1 O4 -111.6(7) . . . . ? C21 O5 U1 I2 -87.6(8) . . . . ? C24 O5 U1 I2 99.6(6) . . . . ? C21 O5 U1 I1 103.4(8) . . . . ? C24 O5 U1 I1 -69.5(6) . . . . ? C16 O3 U1 O1 -2.8(7) . . . . ? C13 O3 U1 O1 -157.4(7) . . . . ? C16 O3 U1 O2 172.2(7) . . . . ? C13 O3 U1 O2 17.5(7) . . . . ? C16 O3 U1 O5 97.6(7) . . . . ? C13 O3 U1 O5 -57.0(9) . . . . ? C16 O3 U1 O4 -71.4(6) . . . . ? C13 O3 U1 O4 133.9(7) . . . . ? C16 O3 U1 I2 82.6(6) . . . . ? C13 O3 U1 I2 -72.0(7) . . . . ? C16 O3 U1 I1 -115.8(6) . . . . ? C13 O3 U1 I1 89.6(7) . . . . ? C20 O4 U1 O1 34.4(7) . . . . ? C17 O4 U1 O1 -173.6(7) . . . . ? C20 O4 U1 O2 -145.8(7) . . . . ? C17 O4 U1 O2 6.2(7) . . . . ? C20 O4 U1 O5 -26.1(9) . . . . ? C17 O4 U1 O5 125.8(7) . . . . ? C20 O4 U1 O3 145.4(8) . . . . ? C17 O4 U1 O3 -62.6(7) . . . . ? C20 O4 U1 I2 108.5(7) . . . . ? C17 O4 U1 I2 -99.5(7) . . . . ? C20 O4 U1 I1 -68.6(7) . . . . ? C17 O4 U1 I1 83.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 23.96 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 2.382 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.193