# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # Attachment 'Kiplinger_-_Dalton_global.cif' _publ_section_title ; Organometallic Uranium(IV) Fluoride Complexes: Preparation Using Protonolysis Chemistry and Reactivity with Trimethylsilyl Reagents ; _publ_contact_author ; Jaqueline L. Kiplinger MSJ514 Los Alamos National Laboratory Los Alamos, NM 87544 ; _publ_contact_author_email kiplinger@lanl.gov _publ_contact_author_name 'Jaqueline L. Kiplinger' loop_ _publ_author_name R.K.Thomson C.R.Graves B.L.Scott J.L.Kiplinger #compound 2 data_apx745a _database_code_depnum_ccdc_archive 'CCDC 763865' #TrackingRef 'Kiplinger_-_Dalton_global.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 F2 N U' _chemical_formula_weight 625.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 18.7527(17) _cell_length_b 13.4677(13) _cell_length_c 9.4862(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2395.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 6.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2195 _exptl_absorpt_correction_T_max 0.7726 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21187 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.09 _reflns_number_total 2929 _reflns_number_gt 2340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _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^)+(0.0254P)^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 2929 _refine_ls_number_parameters 143 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.799 _refine_ls_restrained_S_all 1.894 _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 0.911917(18) 0.2500 0.07524(4) 0.02164(14) Uani 1 2 d S . . F1 F 0.9383(3) 0.4043(4) 0.0538(5) 0.0410(12) Uani 1 1 d . . . N1 N 1.0383(4) 0.2500 -0.0327(9) 0.028(2) Uani 1 2 d S . . C1 C 0.7837(5) 0.2023(8) -0.0426(11) 0.059(3) Uani 1 1 d U . . C2 C 0.8311(6) 0.1671(9) -0.1373(12) 0.064(3) Uani 1 1 d U . . C3 C 0.8656(6) 0.2500 -0.1984(13) 0.066(5) Uani 1 2 d SU . . C4 C 0.7302(9) 0.1385(16) 0.0427(16) 0.181(10) Uani 1 1 d U . . H4A H 0.7400 0.0694 0.0270 0.272 Uiso 1 1 calc R . . H4B H 0.6825 0.1533 0.0127 0.272 Uiso 1 1 calc R . . H4C H 0.7351 0.1532 0.1412 0.272 Uiso 1 1 calc R . . C5 C 0.8413(11) 0.0569(15) -0.163(2) 0.212(12) Uani 1 1 d U . . H5A H 0.8773 0.0472 -0.2335 0.318 Uiso 1 1 calc R . . H5B H 0.7972 0.0284 -0.1945 0.318 Uiso 1 1 calc R . . H5C H 0.8558 0.0254 -0.0768 0.318 Uiso 1 1 calc R . . C6 C 0.9222(10) 0.2500 -0.3059(16) 0.185(14) Uani 1 2 d SU . . H6A H 0.9350 0.1828 -0.3283 0.277 Uiso 0.50 1 calc PR . . H6B H 0.9633 0.2844 -0.2702 0.277 Uiso 0.50 1 calc PR . . H6C H 0.9054 0.2828 -0.3894 0.277 Uiso 0.50 1 calc PR . . C7 C 0.8600(7) 0.2500 0.3431(15) 0.068(5) Uani 1 2 d SU . . C8 C 0.9048(7) 0.1646(11) 0.3375(11) 0.076(4) Uani 1 1 d U . . C9 C 0.9705(6) 0.2038(9) 0.3313(9) 0.060(3) Uani 1 1 d U . . C10 C 0.7838(11) 0.2500 0.381(2) 0.229(16) Uani 1 2 d SU . . H10A H 0.7651 0.1839 0.3722 0.344 Uiso 0.50 1 calc PR . . H10B H 0.7583 0.2936 0.3184 0.344 Uiso 0.50 1 calc PR . . H10C H 0.7783 0.2725 0.4761 0.344 Uiso 0.50 1 calc PR . . C11 C 0.8888(16) 0.0584(16) 0.3549(17) 0.262(15) Uani 1 1 d U . . H11A H 0.8381 0.0491 0.3587 0.393 Uiso 1 1 calc R . . H11B H 0.9099 0.0348 0.4408 0.393 Uiso 1 1 calc R . . H11C H 0.9080 0.0220 0.2765 0.393 Uiso 1 1 calc R . . C12 C 1.0416(11) 0.1447(18) 0.3272(15) 0.222(12) Uani 1 1 d U . . H12A H 1.0316 0.0748 0.3280 0.333 Uiso 1 1 calc R . . H12B H 1.0699 0.1616 0.4081 0.333 Uiso 1 1 calc R . . H12C H 1.0674 0.1613 0.2430 0.333 Uiso 1 1 calc R . . C13 C 1.0726(5) 0.1661(9) -0.0638(9) 0.046(3) Uani 1 1 d . . . H13 H 1.0518 0.1057 -0.0396 0.056 Uiso 1 1 calc R . . C14 C 1.1379(6) 0.1658(13) -0.1308(14) 0.090(6) Uani 1 1 d . . . H14 H 1.1592 0.1055 -0.1528 0.108 Uiso 1 1 calc R . . C15 C 1.1710(10) 0.2500 -0.165(2) 0.125(12) Uani 1 2 d S . . H15 H 1.2150 0.2500 -0.2097 0.150 Uiso 1 2 calc SR . . 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 0.0160(2) 0.0210(3) 0.0279(2) 0.000 0.00414(19) 0.000 F1 0.054(3) 0.030(3) 0.039(3) -0.003(2) -0.006(2) -0.004(2) N1 0.017(4) 0.041(7) 0.025(5) 0.000 0.000(4) 0.000 C1 0.042(5) 0.067(8) 0.067(7) -0.002(5) -0.014(5) -0.025(5) C2 0.070(7) 0.070(8) 0.052(6) -0.038(5) -0.039(5) 0.024(6) C3 0.011(5) 0.163(15) 0.024(7) 0.000 -0.004(5) 0.000 C4 0.129(13) 0.28(2) 0.136(14) 0.035(15) -0.020(11) -0.156(15) C5 0.27(2) 0.15(2) 0.216(19) -0.119(16) -0.193(18) 0.061(17) C6 0.079(14) 0.46(4) 0.019(9) 0.000 -0.006(9) 0.000 C7 0.031(7) 0.140(15) 0.033(7) 0.000 0.008(6) 0.000 C8 0.122(9) 0.073(9) 0.033(5) 0.010(5) -0.010(6) -0.055(7) C9 0.082(7) 0.073(8) 0.026(5) -0.003(4) -0.003(5) 0.037(6) C10 0.070(14) 0.54(5) 0.075(15) 0.000 0.005(12) 0.000 C11 0.59(4) 0.14(2) 0.056(9) 0.023(11) -0.061(17) -0.21(2) C12 0.25(2) 0.36(3) 0.062(10) -0.024(13) -0.051(12) 0.23(2) C13 0.034(5) 0.068(8) 0.037(5) -0.007(5) -0.004(4) 0.013(5) C14 0.040(7) 0.162(18) 0.068(8) -0.032(10) 0.004(6) 0.043(8) C15 0.041(12) 0.25(4) 0.084(16) 0.000 0.037(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 F1 2.146(5) 7_565 ? U1 F1 2.146(5) . ? U1 N1 2.581(8) . ? U1 C7 2.721(14) . ? U1 C1 2.729(9) 7_565 ? U1 C1 2.729(9) . ? U1 C9 2.737(9) 7_565 ? U1 C9 2.737(9) . ? U1 C3 2.737(12) . ? U1 C8 2.744(11) . ? U1 C8 2.744(11) 7_565 ? U1 C2 2.758(9) 7_565 ? N1 C13 1.334(11) . ? N1 C13 1.334(11) 7_565 ? C1 C1 1.28(2) 7_565 ? C1 C2 1.350(14) . ? C1 C4 1.549(16) . ? C2 C3 1.415(14) . ? C2 C5 1.52(2) . ? C3 C2 1.414(14) 7_565 ? C3 C6 1.47(2) . ? C7 C8 1.426(16) . ? C7 C8 1.426(16) 7_565 ? C7 C10 1.47(2) . ? C8 C9 1.341(15) . ? C8 C11 1.47(2) . ? C9 C9 1.24(2) 7_565 ? C9 C12 1.554(17) . ? C13 C14 1.380(13) . ? C14 C15 1.332(16) . ? C15 C14 1.332(16) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 U1 F1 151.1(3) 7_565 . ? F1 U1 N1 75.58(14) 7_565 . ? F1 U1 N1 75.58(14) . . ? F1 U1 C7 99.83(14) 7_565 . ? F1 U1 C7 99.83(14) . . ? N1 U1 C7 134.3(4) . . ? F1 U1 C1 113.1(3) 7_565 7_565 ? F1 U1 C1 86.4(3) . 7_565 ? N1 U1 C1 130.3(3) . 7_565 ? C7 U1 C1 93.9(4) . 7_565 ? F1 U1 C1 86.4(3) 7_565 . ? F1 U1 C1 113.1(3) . . ? N1 U1 C1 130.3(3) . . ? C7 U1 C1 93.9(4) . . ? C1 U1 C1 27.2(5) 7_565 . ? F1 U1 C9 102.2(3) 7_565 7_565 ? F1 U1 C9 76.8(3) . 7_565 ? N1 U1 C9 89.1(3) . 7_565 ? C7 U1 C9 46.8(4) . 7_565 ? C1 U1 C9 131.6(3) 7_565 7_565 ? C1 U1 C9 140.4(3) . 7_565 ? F1 U1 C9 76.8(3) 7_565 . ? F1 U1 C9 102.2(3) . . ? N1 U1 C9 89.1(3) . . ? C7 U1 C9 46.8(4) . . ? C1 U1 C9 140.4(3) 7_565 . ? C1 U1 C9 131.6(3) . . ? C9 U1 C9 26.3(5) 7_565 . ? F1 U1 C3 89.05(14) 7_565 . ? F1 U1 C3 89.05(14) . . ? N1 U1 C3 85.1(3) . . ? C7 U1 C3 140.5(4) . . ? C1 U1 C3 48.1(3) 7_565 . ? C1 U1 C3 48.1(3) . . ? C9 U1 C3 165.7(2) 7_565 . ? C9 U1 C3 165.7(2) . . ? F1 U1 C8 72.0(3) 7_565 . ? F1 U1 C8 120.2(3) . . ? N1 U1 C8 113.8(4) . . ? C7 U1 C8 30.2(3) . . ? C1 U1 C8 115.3(4) 7_565 . ? C1 U1 C8 103.3(3) . . ? C9 U1 C8 46.4(3) 7_565 . ? C9 U1 C8 28.3(3) . . ? C3 U1 C8 147.6(3) . . ? F1 U1 C8 120.2(3) 7_565 7_565 ? F1 U1 C8 72.0(3) . 7_565 ? N1 U1 C8 113.8(4) . 7_565 ? C7 U1 C8 30.2(3) . 7_565 ? C1 U1 C8 103.3(3) 7_565 7_565 ? C1 U1 C8 115.3(4) . 7_565 ? C9 U1 C8 28.3(3) 7_565 7_565 ? C9 U1 C8 46.4(3) . 7_565 ? C3 U1 C8 147.6(3) . 7_565 ? C8 U1 C8 49.6(6) . 7_565 ? F1 U1 C2 116.7(3) 7_565 7_565 ? F1 U1 C2 70.4(3) . 7_565 ? N1 U1 C2 102.4(3) . 7_565 ? C7 U1 C2 119.1(4) . 7_565 ? C1 U1 C2 28.5(3) 7_565 7_565 ? C1 U1 C2 46.5(3) . 7_565 ? C9 U1 C2 141.0(4) 7_565 7_565 ? C9 U1 C2 163.9(4) . 7_565 ? C3 U1 C2 29.8(3) . 7_565 ? C8 U1 C2 143.7(4) . 7_565 ? C8 U1 C2 117.8(4) 7_565 7_565 ? C13 N1 C13 115.9(11) . 7_565 ? C13 N1 U1 122.0(5) . . ? C13 N1 U1 122.0(5) 7_565 . ? C1 C1 C2 110.6(8) 7_565 . ? C1 C1 C4 123.7(10) 7_565 . ? C2 C1 C4 125.4(14) . . ? C1 C1 U1 76.4(2) 7_565 . ? C2 C1 U1 77.0(6) . . ? C4 C1 U1 119.1(8) . . ? C1 C2 C3 107.2(11) . . ? C1 C2 C5 122.2(16) . . ? C3 C2 C5 130.5(14) . . ? C1 C2 U1 74.6(5) . . ? C3 C2 U1 74.3(7) . . ? C5 C2 U1 116.4(8) . . ? C2 C3 C2 104.3(12) 7_565 . ? C2 C3 C6 127.8(6) 7_565 . ? C2 C3 C6 127.8(6) . . ? C2 C3 U1 75.9(6) 7_565 . ? C2 C3 U1 75.9(6) . . ? C6 C3 U1 115.3(9) . . ? C8 C7 C8 107.6(13) . 7_565 ? C8 C7 C10 125.5(7) . . ? C8 C7 C10 125.5(7) 7_565 . ? C8 C7 U1 75.8(7) . . ? C8 C7 U1 75.8(7) 7_565 . ? C10 C7 U1 125.0(12) . . ? C9 C8 C7 103.0(12) . . ? C9 C8 C11 125.1(18) . . ? C7 C8 C11 131.3(16) . . ? C9 C8 U1 75.6(6) . . ? C7 C8 U1 74.0(8) . . ? C11 C8 U1 121.3(9) . . ? C9 C9 C8 113.2(8) 7_565 . ? C9 C9 C12 120.8(12) 7_565 . ? C8 C9 C12 126.0(16) . . ? C9 C9 U1 76.9(2) 7_565 . ? C8 C9 U1 76.1(6) . . ? C12 C9 U1 116.0(7) . . ? N1 C13 C14 122.2(11) . . ? C15 C14 C13 121.5(15) . . ? C14 C15 C14 116.7(18) 7_565 . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.360 _refine_diff_density_min -4.222 _refine_diff_density_rms 0.224 #==============END================== #compound 4 data_apx737s _database_code_depnum_ccdc_archive 'CCDC 763866' #TrackingRef 'Kiplinger_-_Dalton_global.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H68 F2 O U2' _chemical_formula_weight 1163.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 27.007(3) _cell_length_b 9.6398(10) _cell_length_c 17.0651(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.6900(10) _cell_angle_gamma 90.00 _cell_volume 4334.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 7.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2660 _exptl_absorpt_correction_T_max 0.7534 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47738 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.42 _reflns_number_total 10298 _reflns_number_gt 8406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _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. ; # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 203 95 toluene 2 0.500 0.000 0.000 182 85 toluene 3 1.000 0.500 0.000 203 93 toluene 4 0.500 0.500 0.500 182 88 toluene _platon_squeeze_details ; 4 lattice toluene molecules per unit cell disordered across inversion centers. ; _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^)+(0.0328P)^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 10298 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.171472(6) 0.073265(16) 0.253919(9) 0.01008(5) Uani 1 1 d . . . U2 U 0.327541(6) -0.007156(16) 0.329743(9) 0.01040(5) Uani 1 1 d . . . F1 F 0.15575(10) 0.0256(3) 0.36730(15) 0.0201(6) Uani 1 1 d . . . F2 F 0.34304(10) 0.1934(2) 0.38060(14) 0.0182(6) Uani 1 1 d . . . O1 O 0.24924(11) 0.0183(3) 0.27653(17) 0.0145(6) Uani 1 1 d . . . C1 C 0.13819(16) 0.3218(4) 0.3024(2) 0.0128(9) Uani 1 1 d . . . C2 C 0.12032(17) 0.3256(4) 0.2184(3) 0.0147(9) Uani 1 1 d . . . C3 C 0.16300(16) 0.3319(4) 0.1822(2) 0.0140(9) Uani 1 1 d . . . C4 C 0.20755(17) 0.3355(4) 0.2451(2) 0.0131(9) Uani 1 1 d . . . C5 C 0.19202(16) 0.3295(4) 0.3195(2) 0.0130(9) Uani 1 1 d . . . C6 C 0.10591(17) 0.3204(5) 0.3635(3) 0.0210(10) Uani 1 1 d . . . H6A H 0.0995 0.4140 0.3778 0.032 Uiso 1 1 calc R . . H6B H 0.1233 0.2714 0.4105 0.032 Uiso 1 1 calc R . . H6C H 0.0743 0.2750 0.3414 0.032 Uiso 1 1 calc R . . C7 C 0.06579(17) 0.3471(5) 0.1774(3) 0.0217(10) Uani 1 1 d . . . H7A H 0.0455 0.2750 0.1931 0.033 Uiso 1 1 calc R . . H7B H 0.0625 0.3446 0.1202 0.033 Uiso 1 1 calc R . . H7C H 0.0545 0.4356 0.1926 0.033 Uiso 1 1 calc R . . C8 C 0.16239(17) 0.3505(5) 0.0941(2) 0.0181(10) Uani 1 1 d . . . H8A H 0.1800 0.2746 0.0760 0.027 Uiso 1 1 calc R . . H8B H 0.1789 0.4361 0.0865 0.027 Uiso 1 1 calc R . . H8C H 0.1279 0.3526 0.0640 0.027 Uiso 1 1 calc R . . C9 C 0.26028(16) 0.3589(5) 0.2335(3) 0.0173(9) Uani 1 1 d . . . H9A H 0.2663 0.3003 0.1911 0.026 Uiso 1 1 calc R . . H9B H 0.2843 0.3373 0.2824 0.026 Uiso 1 1 calc R . . H9C H 0.2641 0.4543 0.2197 0.026 Uiso 1 1 calc R . . C10 C 0.22633(17) 0.3362(5) 0.4021(2) 0.0176(10) Uani 1 1 d . . . H10A H 0.2291 0.4306 0.4205 0.026 Uiso 1 1 calc R . . H10B H 0.2594 0.3019 0.3999 0.026 Uiso 1 1 calc R . . H10C H 0.2124 0.2804 0.4386 0.026 Uiso 1 1 calc R . . C11 C 0.09802(17) -0.0173(5) 0.1232(3) 0.0179(10) Uani 1 1 d . . . C12 C 0.08368(17) -0.0713(5) 0.1920(3) 0.0179(10) Uani 1 1 d . . . C13 C 0.11893(18) -0.1754(5) 0.2264(3) 0.0182(10) Uani 1 1 d . . . C14 C 0.15681(17) -0.1833(5) 0.1794(3) 0.0180(10) Uani 1 1 d . . . C15 C 0.14427(16) -0.0841(4) 0.1170(3) 0.0150(9) Uani 1 1 d . . . C16 C 0.06651(18) 0.0683(5) 0.0575(3) 0.0220(10) Uani 1 1 d . . . H16A H 0.0516 0.0092 0.0132 0.033 Uiso 1 1 calc R . . H16B H 0.0876 0.1364 0.0398 0.033 Uiso 1 1 calc R . . H16C H 0.0401 0.1140 0.0772 0.033 Uiso 1 1 calc R . . C17 C 0.03631(18) -0.0366(6) 0.2216(3) 0.0267(12) Uani 1 1 d . . . H17A H 0.0172 0.0330 0.1875 0.040 Uiso 1 1 calc R . . H17B H 0.0457 -0.0021 0.2756 0.040 Uiso 1 1 calc R . . H17C H 0.0160 -0.1185 0.2204 0.040 Uiso 1 1 calc R . . C18 C 0.11365(19) -0.2678(5) 0.2951(3) 0.0267(11) Uani 1 1 d . . . H18A H 0.1181 -0.2138 0.3434 0.040 Uiso 1 1 calc R . . H18B H 0.1390 -0.3393 0.3020 0.040 Uiso 1 1 calc R . . H18C H 0.0805 -0.3093 0.2837 0.040 Uiso 1 1 calc R . . C19 C 0.19906(18) -0.2870(5) 0.1897(3) 0.0231(11) Uani 1 1 d . . . H19A H 0.2033 -0.3169 0.1379 0.035 Uiso 1 1 calc R . . H19B H 0.1910 -0.3655 0.2192 0.035 Uiso 1 1 calc R . . H19C H 0.2300 -0.2451 0.2186 0.035 Uiso 1 1 calc R . . C20 C 0.16995(18) -0.0685(5) 0.0481(3) 0.0213(10) Uani 1 1 d . . . H20A H 0.2046 -0.0988 0.0642 0.032 Uiso 1 1 calc R . . H20B H 0.1691 0.0272 0.0321 0.032 Uiso 1 1 calc R . . H20C H 0.1526 -0.1238 0.0037 0.032 Uiso 1 1 calc R . . C21 C 0.38153(17) 0.1195(5) 0.2304(3) 0.0174(10) Uani 1 1 d . . . C22 C 0.34422(17) 0.0395(5) 0.1776(3) 0.0153(9) Uani 1 1 d . . . C23 C 0.35547(17) -0.1025(5) 0.1927(3) 0.0188(10) Uani 1 1 d . . . C24 C 0.40131(18) -0.1108(5) 0.2526(3) 0.0207(10) Uani 1 1 d . . . C25 C 0.41663(17) 0.0254(5) 0.2775(3) 0.0194(10) Uani 1 1 d . . . C26 C 0.38717(19) 0.2736(5) 0.2335(3) 0.0262(11) Uani 1 1 d . . . H26A H 0.3587 0.3154 0.1977 0.039 Uiso 1 1 calc R . . H26B H 0.4179 0.2992 0.2176 0.039 Uiso 1 1 calc R . . H26C H 0.3886 0.3053 0.2873 0.039 Uiso 1 1 calc R . . C27 C 0.30290(19) 0.0931(5) 0.1102(3) 0.0240(11) Uani 1 1 d . . . H27A H 0.3080 0.1903 0.1026 0.036 Uiso 1 1 calc R . . H27B H 0.2705 0.0792 0.1234 0.036 Uiso 1 1 calc R . . H27C H 0.3039 0.0440 0.0616 0.036 Uiso 1 1 calc R . . C28 C 0.3298(2) -0.2216(5) 0.1437(3) 0.0288(12) Uani 1 1 d . . . H28A H 0.3464 -0.2400 0.1005 0.043 Uiso 1 1 calc R . . H28B H 0.2949 -0.1987 0.1221 0.043 Uiso 1 1 calc R . . H28C H 0.3317 -0.3024 0.1771 0.043 Uiso 1 1 calc R . . C29 C 0.4330(2) -0.2395(6) 0.2711(3) 0.0347(13) Uani 1 1 d . . . H29A H 0.4479 -0.2612 0.2264 0.052 Uiso 1 1 calc R . . H29B H 0.4119 -0.3152 0.2804 0.052 Uiso 1 1 calc R . . H29C H 0.4593 -0.2243 0.3181 0.052 Uiso 1 1 calc R . . C30 C 0.46381(18) 0.0709(6) 0.3361(3) 0.0297(12) Uani 1 1 d . . . H30A H 0.4547 0.1114 0.3824 0.045 Uiso 1 1 calc R . . H30B H 0.4815 0.1384 0.3111 0.045 Uiso 1 1 calc R . . H30C H 0.4854 -0.0078 0.3523 0.045 Uiso 1 1 calc R . . C31 C 0.29451(17) -0.1899(4) 0.4295(3) 0.0158(9) Uani 1 1 d . . . C32 C 0.30696(18) -0.0675(4) 0.4748(3) 0.0168(10) Uani 1 1 d . . . C33 C 0.36072(17) -0.0520(4) 0.4918(2) 0.0144(9) Uani 1 1 d . . . C34 C 0.38151(16) -0.1647(4) 0.4566(2) 0.0136(9) Uani 1 1 d . . . C35 C 0.34046(17) -0.2506(4) 0.4175(3) 0.0160(9) Uani 1 1 d . . . C36 C 0.24316(18) -0.2532(5) 0.4060(3) 0.0230(11) Uani 1 1 d . . . H36A H 0.2368 -0.3083 0.4496 0.034 Uiso 1 1 calc R . . H36B H 0.2414 -0.3108 0.3596 0.034 Uiso 1 1 calc R . . H36C H 0.2181 -0.1812 0.3937 0.034 Uiso 1 1 calc R . . C37 C 0.27051(19) 0.0203(5) 0.5078(3) 0.0234(11) Uani 1 1 d . . . H37A H 0.2368 0.0075 0.4760 0.035 Uiso 1 1 calc R . . H37B H 0.2800 0.1161 0.5064 0.035 Uiso 1 1 calc R . . H37C H 0.2714 -0.0065 0.5623 0.035 Uiso 1 1 calc R . . C38 C 0.39160(19) 0.0590(5) 0.5425(3) 0.0223(11) Uani 1 1 d . . . H38A H 0.4024 0.0264 0.5967 0.033 Uiso 1 1 calc R . . H38B H 0.3713 0.1409 0.5417 0.033 Uiso 1 1 calc R . . H38C H 0.4208 0.0804 0.5213 0.033 Uiso 1 1 calc R . . C39 C 0.43687(18) -0.1968(5) 0.4732(3) 0.0234(11) Uani 1 1 d . . . H39A H 0.4489 -0.2158 0.5294 0.035 Uiso 1 1 calc R . . H39B H 0.4549 -0.1188 0.4583 0.035 Uiso 1 1 calc R . . H39C H 0.4424 -0.2765 0.4425 0.035 Uiso 1 1 calc R . . C40 C 0.34384(19) -0.3897(5) 0.3783(3) 0.0255(11) Uani 1 1 d . . . H40A H 0.3788 -0.4130 0.3819 0.038 Uiso 1 1 calc R . . H40B H 0.3266 -0.3852 0.3228 0.038 Uiso 1 1 calc R . . H40C H 0.3283 -0.4592 0.4051 0.038 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 0.00882(8) 0.01073(8) 0.01056(8) 0.00014(6) 0.00184(6) 0.00014(6) U2 0.00955(8) 0.01199(8) 0.00964(8) 0.00077(6) 0.00207(6) 0.00158(6) F1 0.0232(15) 0.0192(14) 0.0187(14) 0.0026(11) 0.0064(12) 0.0010(11) F2 0.0215(14) 0.0155(13) 0.0182(13) 0.0024(11) 0.0058(11) 0.0003(11) O1 0.0161(16) 0.0141(15) 0.0138(15) 0.0012(12) 0.0044(13) 0.0006(13) C1 0.015(2) 0.011(2) 0.013(2) 0.0041(17) 0.0049(17) 0.0093(17) C2 0.017(2) 0.014(2) 0.013(2) -0.0020(17) 0.0029(18) 0.0011(18) C3 0.017(2) 0.012(2) 0.012(2) 0.0004(17) 0.0024(18) 0.0014(18) C4 0.019(2) 0.0053(19) 0.015(2) -0.0002(16) 0.0035(18) 0.0016(17) C5 0.016(2) 0.008(2) 0.014(2) -0.0004(16) 0.0019(18) 0.0015(17) C6 0.019(3) 0.026(3) 0.020(2) 0.002(2) 0.007(2) 0.008(2) C7 0.017(2) 0.031(3) 0.017(2) 0.005(2) 0.0041(19) 0.008(2) C8 0.018(2) 0.022(2) 0.016(2) 0.0038(19) 0.0064(19) 0.001(2) C9 0.018(2) 0.015(2) 0.021(2) 0.0002(19) 0.0070(19) -0.0031(19) C10 0.021(2) 0.014(2) 0.017(2) -0.0036(18) 0.0026(19) 0.0026(19) C11 0.016(2) 0.022(2) 0.015(2) -0.0005(19) 0.0000(18) -0.005(2) C12 0.013(2) 0.022(2) 0.019(2) -0.0054(19) 0.0036(18) -0.0107(19) C13 0.022(3) 0.017(2) 0.014(2) -0.0005(18) 0.0008(19) -0.008(2) C14 0.015(2) 0.018(2) 0.021(2) -0.0073(19) 0.0026(19) -0.0053(19) C15 0.012(2) 0.017(2) 0.016(2) -0.0032(18) 0.0026(18) -0.0038(18) C16 0.016(2) 0.032(3) 0.015(2) -0.002(2) -0.0029(19) 0.000(2) C17 0.013(2) 0.043(3) 0.024(3) -0.004(2) 0.007(2) -0.004(2) C18 0.031(3) 0.028(3) 0.022(3) 0.006(2) 0.007(2) -0.009(2) C19 0.028(3) 0.013(2) 0.028(3) -0.004(2) 0.005(2) 0.002(2) C20 0.023(3) 0.028(3) 0.014(2) -0.003(2) 0.007(2) -0.003(2) C21 0.014(2) 0.026(3) 0.014(2) 0.0006(19) 0.0075(18) -0.005(2) C22 0.014(2) 0.023(2) 0.011(2) -0.0010(18) 0.0067(18) -0.0016(19) C23 0.015(2) 0.027(3) 0.017(2) -0.0042(19) 0.0086(19) 0.001(2) C24 0.019(2) 0.030(3) 0.014(2) -0.002(2) 0.0068(19) 0.007(2) C25 0.015(2) 0.032(3) 0.012(2) 0.0028(19) 0.0041(18) -0.002(2) C26 0.022(3) 0.034(3) 0.023(3) 0.006(2) 0.006(2) -0.007(2) C27 0.025(3) 0.034(3) 0.014(2) 0.003(2) 0.007(2) 0.003(2) C28 0.031(3) 0.030(3) 0.025(3) -0.011(2) 0.006(2) 0.002(2) C29 0.033(3) 0.041(3) 0.034(3) -0.001(3) 0.015(3) 0.018(3) C30 0.014(3) 0.042(3) 0.031(3) 0.009(2) 0.001(2) -0.006(2) C31 0.018(2) 0.016(2) 0.013(2) 0.0042(17) 0.0010(18) -0.0008(19) C32 0.024(3) 0.015(2) 0.013(2) 0.0060(18) 0.0055(19) 0.006(2) C33 0.018(2) 0.016(2) 0.007(2) 0.0021(17) -0.0020(17) 0.0024(18) C34 0.015(2) 0.013(2) 0.012(2) 0.0029(17) 0.0001(17) 0.0027(18) C35 0.020(2) 0.011(2) 0.015(2) 0.0040(17) 0.0003(19) 0.0001(18) C36 0.023(3) 0.024(3) 0.022(3) 0.006(2) 0.006(2) -0.001(2) C37 0.028(3) 0.028(3) 0.018(2) 0.001(2) 0.012(2) 0.006(2) C38 0.030(3) 0.021(2) 0.015(2) -0.0034(19) 0.003(2) 0.004(2) C39 0.021(3) 0.020(2) 0.027(3) -0.003(2) 0.000(2) 0.000(2) C40 0.025(3) 0.018(2) 0.031(3) -0.003(2) 0.001(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.118(3) . ? U1 F1 2.121(2) . ? U1 C5 2.718(4) . ? U1 C4 2.725(4) . ? U1 C15 2.746(4) . ? U1 C1 2.749(4) . ? U1 C12 2.753(4) . ? U1 C3 2.765(4) . ? U1 C14 2.769(4) . ? U1 C13 2.773(4) . ? U1 C11 2.780(4) . ? U1 C2 2.797(4) . ? U2 F2 2.123(2) . ? U2 O1 2.124(3) . ? U2 C32 2.716(4) . ? U2 C31 2.732(4) . ? U2 C33 2.747(4) . ? U2 C21 2.753(4) . ? U2 C25 2.761(4) . ? U2 C35 2.764(4) . ? U2 C22 2.767(4) . ? U2 C23 2.768(4) . ? U2 C34 2.780(4) . ? U2 C24 2.802(4) . ? C1 C2 1.409(6) . ? C1 C5 1.420(6) . ? C1 C6 1.499(6) . ? C2 C3 1.423(6) . ? C2 C7 1.499(6) . ? C3 C4 1.426(6) . ? C3 C8 1.511(6) . ? C4 C5 1.423(6) . ? C4 C9 1.497(6) . ? C5 C10 1.509(6) . ? C11 C12 1.414(6) . ? C11 C15 1.429(6) . ? C11 C16 1.498(6) . ? C12 C13 1.419(6) . ? C12 C17 1.513(6) . ? C13 C14 1.434(6) . ? C13 C18 1.503(6) . ? C14 C15 1.416(6) . ? C14 C19 1.499(6) . ? C15 C20 1.499(6) . ? C21 C22 1.422(6) . ? C21 C25 1.426(6) . ? C21 C26 1.493(7) . ? C22 C23 1.414(6) . ? C22 C27 1.507(6) . ? C23 C24 1.424(6) . ? C23 C28 1.497(6) . ? C24 C25 1.414(7) . ? C24 C29 1.500(7) . ? C25 C30 1.502(6) . ? C31 C32 1.410(6) . ? C31 C35 1.427(6) . ? C31 C36 1.487(6) . ? C32 C33 1.425(6) . ? C32 C37 1.499(6) . ? C33 C34 1.415(6) . ? C33 C38 1.507(6) . ? C34 C35 1.427(6) . ? C34 C39 1.492(6) . ? C35 C40 1.510(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 O1 U1 F1 99.72(10) . . ? O1 U1 C5 92.74(12) . . ? F1 U1 C5 83.40(11) . . ? O1 U1 C4 83.68(12) . . ? F1 U1 C4 113.40(11) . . ? C5 U1 C4 30.31(12) . . ? O1 U1 C15 94.94(12) . . ? F1 U1 C15 125.92(11) . . ? C5 U1 C15 147.59(13) . . ? C4 U1 C15 119.82(13) . . ? O1 U1 C1 122.68(12) . . ? F1 U1 C1 76.72(11) . . ? C5 U1 C1 30.11(12) . . ? C4 U1 C1 49.66(13) . . ? C15 U1 C1 133.87(13) . . ? O1 U1 C12 132.78(13) . . ? F1 U1 C12 84.96(12) . . ? C5 U1 C12 134.33(13) . . ? C4 U1 C12 137.44(13) . . ? C15 U1 C12 49.24(13) . . ? C1 U1 C12 104.23(13) . . ? O1 U1 C3 106.78(12) . . ? F1 U1 C3 125.85(11) . . ? C5 U1 C3 49.62(12) . . ? C4 U1 C3 30.09(12) . . ? C15 U1 C3 98.11(12) . . ? C1 U1 C3 49.18(12) . . ? C12 U1 C3 107.83(13) . . ? O1 U1 C14 84.05(12) . . ? F1 U1 C14 100.85(12) . . ? C5 U1 C14 175.03(13) . . ? C4 U1 C14 145.07(13) . . ? C15 U1 C14 29.74(13) . . ? C1 U1 C14 153.27(13) . . ? C12 U1 C14 49.26(13) . . ? C3 U1 C14 127.78(13) . . ? O1 U1 C13 105.35(13) . . ? F1 U1 C13 76.67(11) . . ? C5 U1 C13 154.96(13) . . ? C4 U1 C13 165.58(13) . . ? C15 U1 C13 49.25(13) . . ? C1 U1 C13 127.98(13) . . ? C12 U1 C13 29.75(13) . . ? C3 U1 C13 135.67(13) . . ? C14 U1 C13 29.99(13) . . ? O1 U1 C11 124.88(12) . . ? F1 U1 C11 114.42(12) . . ? C5 U1 C11 131.37(13) . . ? C4 U1 C11 116.60(13) . . ? C15 U1 C11 29.97(13) . . ? C1 U1 C11 107.00(13) . . ? C12 U1 C11 29.61(13) . . ? C3 U1 C11 87.31(13) . . ? C14 U1 C11 49.17(14) . . ? C13 U1 C11 49.02(13) . . ? O1 U1 C2 132.83(12) . . ? F1 U1 C2 101.43(11) . . ? C5 U1 C2 49.13(12) . . ? C4 U1 C2 49.23(13) . . ? C15 U1 C2 105.58(13) . . ? C1 U1 C2 29.42(12) . . ? C12 U1 C2 90.82(13) . . ? C3 U1 C2 29.63(12) . . ? C14 U1 C2 131.52(13) . . ? C13 U1 C2 120.34(14) . . ? C11 U1 C2 82.40(13) . . ? F2 U2 O1 99.09(10) . . ? F2 U2 C32 83.33(11) . . ? O1 U2 C32 91.74(12) . . ? F2 U2 C31 113.23(11) . . ? O1 U2 C31 84.84(12) . . ? C32 U2 C31 29.99(13) . . ? F2 U2 C33 74.94(11) . . ? O1 U2 C33 121.50(12) . . ? C32 U2 C33 30.23(13) . . ? C31 U2 C33 49.49(13) . . ? F2 U2 C21 76.37(12) . . ? O1 U2 C21 107.32(12) . . ? C32 U2 C21 153.94(14) . . ? C31 U2 C21 163.63(14) . . ? C33 U2 C21 126.14(13) . . ? F2 U2 C25 85.47(12) . . ? O1 U2 C25 134.83(12) . . ? C32 U2 C25 133.30(14) . . ? C31 U2 C25 134.54(13) . . ? C33 U2 C25 103.18(13) . . ? C21 U2 C25 29.98(13) . . ? F2 U2 C35 124.16(11) . . ? O1 U2 C35 108.96(12) . . ? C32 U2 C35 49.56(13) . . ? C31 U2 C35 30.09(13) . . ? C33 U2 C35 49.22(13) . . ? C21 U2 C35 133.58(14) . . ? C25 U2 C35 104.84(13) . . ? F2 U2 C22 100.21(11) . . ? O1 U2 C22 86.11(12) . . ? C32 U2 C22 176.10(13) . . ? C31 U2 C22 146.32(13) . . ? C33 U2 C22 152.30(13) . . ? C21 U2 C22 29.86(13) . . ? C25 U2 C22 49.14(13) . . ? C35 U2 C22 128.25(13) . . ? F2 U2 C23 125.60(12) . . ? O1 U2 C23 96.18(12) . . ? C32 U2 C23 147.92(14) . . ? C31 U2 C23 119.96(13) . . ? C33 U2 C23 135.17(13) . . ? C21 U2 C23 49.26(14) . . ? C25 U2 C23 49.18(14) . . ? C35 U2 C23 98.65(13) . . ? C22 U2 C23 29.60(13) . . ? F2 U2 C34 99.00(11) . . ? O1 U2 C34 134.29(12) . . ? C32 U2 C34 49.52(13) . . ? C31 U2 C34 49.45(13) . . ? C33 U2 C34 29.67(12) . . ? C21 U2 C34 117.63(13) . . ? C25 U2 C34 88.19(13) . . ? C35 U2 C34 29.82(12) . . ? C22 U2 C34 130.82(13) . . ? C23 U2 C34 106.44(13) . . ? F2 U2 C24 114.84(12) . . ? O1 U2 C24 125.74(12) . . ? C32 U2 C24 131.35(13) . . ? C31 U2 C24 115.22(14) . . ? C33 U2 C24 107.96(13) . . ? C21 U2 C24 48.81(14) . . ? C25 U2 C24 29.43(14) . . ? C35 U2 C24 86.20(14) . . ? C22 U2 C24 48.57(13) . . ? C23 U2 C24 29.63(13) . . ? C34 U2 C24 82.29(13) . . ? U1 O1 U2 163.96(15) . . ? C2 C1 C5 108.3(4) . . ? C2 C1 C6 125.9(4) . . ? C5 C1 C6 125.7(4) . . ? C2 C1 U1 77.2(2) . . ? C5 C1 U1 73.7(2) . . ? C6 C1 U1 118.7(3) . . ? C1 C2 C3 108.2(4) . . ? C1 C2 C7 124.0(4) . . ? C3 C2 C7 126.7(4) . . ? C1 C2 U1 73.4(2) . . ? C3 C2 U1 73.9(2) . . ? C7 C2 U1 127.5(3) . . ? C2 C3 C4 107.8(4) . . ? C2 C3 C8 127.1(4) . . ? C4 C3 C8 124.7(4) . . ? C2 C3 U1 76.5(2) . . ? C4 C3 U1 73.4(2) . . ? C8 C3 U1 121.9(3) . . ? C5 C4 C3 107.8(4) . . ? C5 C4 C9 126.8(4) . . ? C3 C4 C9 125.0(4) . . ? C5 C4 U1 74.6(2) . . ? C3 C4 U1 76.5(2) . . ? C9 C4 U1 120.6(3) . . ? C1 C5 C4 107.9(4) . . ? C1 C5 C10 125.8(4) . . ? C4 C5 C10 126.3(4) . . ? C1 C5 U1 76.2(2) . . ? C4 C5 U1 75.1(2) . . ? C10 C5 U1 116.9(3) . . ? C12 C11 C15 107.4(4) . . ? C12 C11 C16 127.6(4) . . ? C15 C11 C16 123.7(4) . . ? C12 C11 U1 74.1(2) . . ? C15 C11 U1 73.7(2) . . ? C16 C11 U1 128.0(3) . . ? C11 C12 C13 108.8(4) . . ? C11 C12 C17 127.0(4) . . ? C13 C12 C17 123.9(4) . . ? C11 C12 U1 76.3(2) . . ? C13 C12 U1 75.9(2) . . ? C17 C12 U1 118.7(3) . . ? C12 C13 C14 107.6(4) . . ? C12 C13 C18 124.9(4) . . ? C14 C13 C18 127.3(4) . . ? C12 C13 U1 74.4(2) . . ? C14 C13 U1 74.8(2) . . ? C18 C13 U1 120.8(3) . . ? C15 C14 C13 107.6(4) . . ? C15 C14 C19 126.1(4) . . ? C13 C14 C19 126.0(4) . . ? C15 C14 U1 74.3(2) . . ? C13 C14 U1 75.2(2) . . ? C19 C14 U1 120.9(3) . . ? C14 C15 C11 108.5(4) . . ? C14 C15 C20 125.6(4) . . ? C11 C15 C20 125.1(4) . . ? C14 C15 U1 76.0(2) . . ? C11 C15 U1 76.3(2) . . ? C20 C15 U1 121.9(3) . . ? C22 C21 C25 107.6(4) . . ? C22 C21 C26 127.9(4) . . ? C25 C21 C26 124.3(4) . . ? C22 C21 U2 75.6(2) . . ? C25 C21 U2 75.3(2) . . ? C26 C21 U2 118.9(3) . . ? C23 C22 C21 108.4(4) . . ? C23 C22 C27 124.3(4) . . ? C21 C22 C27 126.9(4) . . ? C23 C22 U2 75.2(2) . . ? C21 C22 U2 74.5(2) . . ? C27 C22 U2 121.7(3) . . ? C22 C23 C24 107.6(4) . . ? C22 C23 C28 125.9(4) . . ? C24 C23 C28 125.5(4) . . ? C22 C23 U2 75.2(2) . . ? C24 C23 U2 76.5(2) . . ? C28 C23 U2 123.2(3) . . ? C25 C24 C23 108.3(4) . . ? C25 C24 C29 126.1(4) . . ? C23 C24 C29 124.2(4) . . ? C25 C24 U2 73.7(3) . . ? C23 C24 U2 73.9(2) . . ? C29 C24 U2 128.9(3) . . ? C24 C25 C21 107.9(4) . . ? C24 C25 C30 128.4(4) . . ? C21 C25 C30 123.4(4) . . ? C24 C25 U2 76.9(3) . . ? C21 C25 U2 74.7(2) . . ? C30 C25 U2 119.3(3) . . ? C32 C31 C35 108.2(4) . . ? C32 C31 C36 125.9(4) . . ? C35 C31 C36 125.6(4) . . ? C32 C31 U2 74.4(2) . . ? C35 C31 U2 76.2(2) . . ? C36 C31 U2 120.6(3) . . ? C31 C32 C33 108.0(4) . . ? C31 C32 C37 125.5(4) . . ? C33 C32 C37 126.0(4) . . ? C31 C32 U2 75.6(2) . . ? C33 C32 U2 76.1(2) . . ? C37 C32 U2 120.3(3) . . ? C34 C33 C32 108.3(4) . . ? C34 C33 C38 124.6(4) . . ? C32 C33 C38 127.0(4) . . ? C34 C33 U2 76.5(2) . . ? C32 C33 U2 73.7(2) . . ? C38 C33 U2 118.9(3) . . ? C33 C34 C35 107.7(4) . . ? C33 C34 C39 123.6(4) . . ? C35 C34 C39 127.7(4) . . ? C33 C34 U2 73.9(2) . . ? C35 C34 U2 74.5(2) . . ? C39 C34 U2 126.4(3) . . ? C34 C35 C31 107.8(4) . . ? C34 C35 C40 127.3(4) . . ? C31 C35 C40 124.5(4) . . ? C34 C35 U2 75.7(2) . . ? C31 C35 U2 73.7(2) . . ? C40 C35 U2 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.122 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.166 #===============END=================== #compound 15 data_apx869a _database_code_depnum_ccdc_archive 'CCDC 763867' #TrackingRef 'Kiplinger_-_Dalton_global.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H44 O Se U' _chemical_formula_weight 737.64 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' 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 17.830(7) _cell_length_b 14.973(6) _cell_length_c 21.254(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5674(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 7.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2835 _exptl_absorpt_correction_T_max 0.4862 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34068 _diffrn_reflns_av_R_equivalents 0.1351 _diffrn_reflns_av_sigmaI/netI 0.0919 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5181 _reflns_number_gt 3095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _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^)+(0.0390P)^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 5181 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.048586(18) 0.71837(3) 0.357640(15) 0.01617(12) Uani 1 1 d . . . Se1 Se 0.03936(6) 0.90320(7) 0.38378(5) 0.0345(3) Uani 1 1 d . . . O1 O -0.0237(3) 0.7099(4) 0.2842(3) 0.0229(16) Uani 1 1 d . . . C1 C 0.1723(5) 0.6458(7) 0.3036(4) 0.024(2) Uani 1 1 d . . . C2 C 0.2001(5) 0.6784(7) 0.3610(4) 0.0201(13) Uani 1 1 d . . . C3 C 0.1995(5) 0.7700(7) 0.3584(4) 0.0201(13) Uani 1 1 d . . . C4 C 0.1713(5) 0.7971(7) 0.3002(4) 0.0201(13) Uani 1 1 d . . . C5 C 0.1561(5) 0.7199(8) 0.2654(4) 0.025(2) Uani 1 1 d . . . C6 C 0.1682(6) 0.5513(7) 0.2824(5) 0.045(3) Uani 1 1 d . . . H6A H 0.2014 0.5427 0.2473 0.068 Uiso 1 1 calc R . . H6B H 0.1178 0.5376 0.2698 0.068 Uiso 1 1 calc R . . H6C H 0.1828 0.5126 0.3162 0.068 Uiso 1 1 calc R . . C7 C 0.2431(5) 0.6264(9) 0.4082(5) 0.055(4) Uani 1 1 d . . . H7A H 0.2957 0.6380 0.4031 0.082 Uiso 1 1 calc R . . H7B H 0.2336 0.5638 0.4022 0.082 Uiso 1 1 calc R . . H7C H 0.2277 0.6436 0.4497 0.082 Uiso 1 1 calc R . . C8 C 0.2316(5) 0.8333(8) 0.4082(5) 0.049(4) Uani 1 1 d . . . H8A H 0.2813 0.8510 0.3962 0.073 Uiso 1 1 calc R . . H8B H 0.2334 0.8033 0.4481 0.073 Uiso 1 1 calc R . . H8C H 0.2002 0.8852 0.4115 0.073 Uiso 1 1 calc R . . C9 C 0.1719(6) 0.8905(8) 0.2729(5) 0.051(4) Uani 1 1 d . . . H9A H 0.1657 0.9333 0.3061 0.076 Uiso 1 1 calc R . . H9B H 0.1316 0.8966 0.2433 0.076 Uiso 1 1 calc R . . H9C H 0.2188 0.9009 0.2520 0.076 Uiso 1 1 calc R . . C10 C 0.1396(5) 0.7163(8) 0.1963(4) 0.042(3) Uani 1 1 d . . . H10A H 0.1104 0.7675 0.1846 0.062 Uiso 1 1 calc R . . H10B H 0.1119 0.6629 0.1870 0.062 Uiso 1 1 calc R . . H10C H 0.1858 0.7162 0.1732 0.062 Uiso 1 1 calc R . . C11 C -0.0662(5) 0.6561(7) 0.4315(4) 0.020(2) Uani 1 1 d . . . C12 C -0.0279(5) 0.5819(7) 0.4106(4) 0.024(3) Uani 1 1 d . . . C13 C 0.0434(5) 0.5788(6) 0.4419(4) 0.022(2) Uani 1 1 d . . . C14 C 0.0459(5) 0.6545(7) 0.4793(4) 0.020(2) Uani 1 1 d . . . C15 C -0.0208(6) 0.7054(7) 0.4744(4) 0.022(2) Uani 1 1 d . . . C16 C -0.0552(6) 0.5093(7) 0.3681(5) 0.039(3) Uani 1 1 d . . . H16A H -0.0704 0.4588 0.3929 0.059 Uiso 1 1 calc R . . H16B H -0.0156 0.4918 0.3401 0.059 Uiso 1 1 calc R . . H16C H -0.0971 0.5305 0.3441 0.059 Uiso 1 1 calc R . . C17 C 0.0928(6) 0.4992(7) 0.4415(5) 0.039(3) Uani 1 1 d . . . H17A H 0.1326 0.5073 0.4714 0.058 Uiso 1 1 calc R . . H17B H 0.1137 0.4914 0.4002 0.058 Uiso 1 1 calc R . . H17C H 0.0641 0.4473 0.4526 0.058 Uiso 1 1 calc R . . C18 C 0.1065(6) 0.6828(7) 0.5252(4) 0.036(3) Uani 1 1 d . . . H18A H 0.0848 0.6917 0.5660 0.054 Uiso 1 1 calc R . . H18B H 0.1290 0.7375 0.5110 0.054 Uiso 1 1 calc R . . H18C H 0.1441 0.6371 0.5276 0.054 Uiso 1 1 calc R . . C19 C -0.0434(6) 0.7804(7) 0.5146(4) 0.039(3) Uani 1 1 d . . . H19A H -0.0634 0.7578 0.5534 0.058 Uiso 1 1 calc R . . H19B H -0.0810 0.8150 0.4934 0.058 Uiso 1 1 calc R . . H19C H -0.0006 0.8173 0.5232 0.058 Uiso 1 1 calc R . . C20 C -0.1476(5) 0.6765(7) 0.4212(5) 0.034(3) Uani 1 1 d . . . H20A H -0.1651 0.6450 0.3847 0.050 Uiso 1 1 calc R . . H20B H -0.1538 0.7396 0.4150 0.050 Uiso 1 1 calc R . . H20C H -0.1759 0.6580 0.4574 0.050 Uiso 1 1 calc R . . C21 C -0.0633(5) 0.9353(7) 0.3969(5) 0.029(3) Uani 1 1 d . . . C22 C -0.0811(7) 1.0027(8) 0.4388(6) 0.050(4) Uani 1 1 d . . . H22 H -0.0432 1.0320 0.4608 0.060 Uiso 1 1 calc R . . C23 C -0.1548(8) 1.0264(9) 0.4480(6) 0.059(4) Uani 1 1 d . . . H23 H -0.1654 1.0742 0.4746 0.071 Uiso 1 1 calc R . . C24 C -0.2121(6) 0.9835(8) 0.4202(5) 0.039(3) Uani 1 1 d . . . H24 H -0.2616 0.9974 0.4299 0.047 Uiso 1 1 calc R . . C25 C -0.1952(6) 0.9195(8) 0.3778(5) 0.044(3) Uani 1 1 d . . . H25 H -0.2335 0.8915 0.3557 0.053 Uiso 1 1 calc R . . C26 C -0.1220(6) 0.8953(7) 0.3668(4) 0.032(3) Uani 1 1 d . . . H26 H -0.1121 0.8501 0.3379 0.038 Uiso 1 1 calc R . . C27 C -0.0744(5) 0.7090(8) 0.2307(4) 0.032(3) Uani 1 1 d . . . C28 C -0.0517(5) 0.6307(7) 0.1889(5) 0.031(3) Uani 1 1 d . . . H28A H -0.0015 0.6395 0.1740 0.047 Uiso 1 1 calc R . . H28B H -0.0854 0.6269 0.1537 0.047 Uiso 1 1 calc R . . H28C H -0.0541 0.5763 0.2128 0.047 Uiso 1 1 calc R . . C29 C -0.1527(5) 0.6929(8) 0.2534(5) 0.044(3) Uani 1 1 d . . . H29A H -0.1557 0.6348 0.2724 0.066 Uiso 1 1 calc R . . H29B H -0.1868 0.6960 0.2185 0.066 Uiso 1 1 calc R . . H29C H -0.1659 0.7375 0.2839 0.066 Uiso 1 1 calc R . . C30 C -0.0674(5) 0.7953(7) 0.1961(5) 0.033(3) Uani 1 1 d . . . H30A H -0.0844 0.8432 0.2226 0.050 Uiso 1 1 calc R . . H30B H -0.0976 0.7933 0.1587 0.050 Uiso 1 1 calc R . . H30C H -0.0160 0.8051 0.1849 0.050 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 0.01671(19) 0.0167(2) 0.01509(18) 0.00103(17) 0.00106(16) -0.00088(18) Se1 0.0325(6) 0.0168(6) 0.0541(7) -0.0023(5) 0.0130(5) -0.0011(5) O1 0.029(4) 0.019(4) 0.021(4) 0.001(3) 0.003(3) -0.004(3) C1 0.020(6) 0.020(6) 0.031(6) -0.007(5) 0.009(4) -0.007(5) C2 0.009(3) 0.029(4) 0.023(3) 0.000(3) 0.001(2) -0.003(3) C3 0.009(3) 0.029(4) 0.023(3) 0.000(3) 0.001(2) -0.003(3) C4 0.009(3) 0.029(4) 0.023(3) 0.000(3) 0.001(2) -0.003(3) C5 0.019(5) 0.035(7) 0.020(5) 0.002(6) 0.009(4) -0.006(6) C6 0.033(7) 0.037(8) 0.066(9) -0.016(7) 0.025(6) -0.003(6) C7 0.015(6) 0.097(13) 0.052(8) 0.022(8) 0.015(5) -0.004(7) C8 0.019(6) 0.066(10) 0.061(8) -0.025(7) -0.002(5) -0.009(6) C9 0.060(9) 0.032(8) 0.061(8) 0.018(7) 0.024(7) 0.007(7) C10 0.024(6) 0.080(10) 0.021(6) -0.005(7) 0.013(5) -0.009(7) C11 0.025(6) 0.016(6) 0.018(5) 0.011(5) 0.007(4) 0.004(5) C12 0.033(6) 0.023(7) 0.018(5) -0.008(5) 0.014(4) -0.005(5) C13 0.033(6) 0.013(6) 0.020(5) -0.002(4) 0.019(5) -0.003(5) C14 0.026(5) 0.025(6) 0.009(4) 0.005(4) 0.006(4) 0.003(5) C15 0.035(6) 0.015(6) 0.016(5) 0.000(5) 0.013(4) -0.008(5) C16 0.059(8) 0.018(7) 0.040(7) -0.001(5) -0.005(6) -0.008(6) C17 0.047(8) 0.025(7) 0.044(7) 0.009(6) 0.025(6) -0.002(6) C18 0.046(7) 0.046(8) 0.016(6) 0.010(5) -0.002(5) -0.014(6) C19 0.063(8) 0.036(7) 0.018(5) 0.004(6) 0.005(5) 0.003(7) C20 0.032(6) 0.029(7) 0.040(7) 0.019(5) 0.008(5) -0.005(6) C21 0.029(7) 0.018(6) 0.039(6) -0.001(5) 0.005(5) 0.005(5) C22 0.038(7) 0.046(9) 0.067(9) -0.019(7) 0.005(6) -0.002(7) C23 0.066(10) 0.032(9) 0.079(10) -0.006(7) 0.019(8) 0.017(8) C24 0.027(7) 0.039(9) 0.051(8) 0.015(7) 0.013(6) 0.003(6) C25 0.026(7) 0.058(9) 0.048(7) 0.003(7) -0.019(6) 0.015(6) C26 0.035(7) 0.027(7) 0.033(6) -0.010(5) -0.005(5) -0.002(5) C27 0.023(6) 0.054(9) 0.019(5) -0.010(6) -0.007(4) 0.006(6) C28 0.019(5) 0.034(7) 0.040(6) -0.005(5) -0.009(5) -0.007(5) C29 0.024(6) 0.070(11) 0.038(7) -0.013(6) -0.002(5) -0.006(6) C30 0.038(7) 0.036(8) 0.027(6) 0.005(5) -0.002(5) 0.014(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 2.029(6) . ? U1 C12 2.702(10) . ? U1 C1 2.714(9) . ? U1 C11 2.743(9) . ? U1 C5 2.742(8) . ? U1 C13 2.754(9) . ? U1 C14 2.757(8) . ? U1 C2 2.768(9) . ? U1 C4 2.769(9) . ? U1 C15 2.779(9) . ? U1 C3 2.799(8) . ? U1 Se1 2.8274(15) . ? Se1 C21 1.914(10) . ? O1 C27 1.453(11) . ? C1 C2 1.404(12) . ? C1 C5 1.405(14) . ? C1 C6 1.487(14) . ? C2 C3 1.372(13) . ? C2 C7 1.483(13) . ? C3 C4 1.394(12) . ? C3 C8 1.532(13) . ? C4 C5 1.399(13) . ? C4 C9 1.515(13) . ? C5 C10 1.498(12) . ? C11 C12 1.378(13) . ? C11 C15 1.426(13) . ? C11 C20 1.498(12) . ? C12 C13 1.436(13) . ? C12 C16 1.495(13) . ? C13 C14 1.385(13) . ? C13 C17 1.482(13) . ? C14 C15 1.416(13) . ? C14 C18 1.516(12) . ? C15 C19 1.467(13) . ? C21 C26 1.365(13) . ? C21 C22 1.383(14) . ? C22 C23 1.375(15) . ? C23 C24 1.344(15) . ? C24 C25 1.350(15) . ? C25 C26 1.374(13) . ? C27 C30 1.491(15) . ? C27 C29 1.498(13) . ? C27 C28 1.525(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 C12 87.3(3) . . ? O1 U1 C1 99.6(3) . . ? C12 U1 C1 106.5(3) . . ? O1 U1 C11 86.8(3) . . ? C12 U1 C11 29.3(3) . . ? C1 U1 C11 135.5(3) . . ? O1 U1 C5 83.9(3) . . ? C12 U1 C5 131.1(3) . . ? C1 U1 C5 29.8(3) . . ? C11 U1 C5 159.0(3) . . ? O1 U1 C13 115.6(3) . . ? C12 U1 C13 30.5(3) . . ? C1 U1 C13 89.9(3) . . ? C11 U1 C13 49.1(3) . . ? C5 U1 C13 119.7(3) . . ? O1 U1 C14 133.6(3) . . ? C12 U1 C14 48.6(3) . . ? C1 U1 C14 105.8(3) . . ? C11 U1 C14 48.1(3) . . ? C5 U1 C14 133.3(3) . . ? C13 U1 C14 29.1(3) . . ? O1 U1 C2 128.8(3) . . ? C12 U1 C2 108.6(3) . . ? C1 U1 C2 29.7(3) . . ? C11 U1 C2 129.8(3) . . ? C5 U1 C2 48.5(3) . . ? C13 U1 C2 81.5(3) . . ? C14 U1 C2 85.3(3) . . ? O1 U1 C4 100.9(3) . . ? C12 U1 C4 154.7(3) . . ? C1 U1 C4 48.8(3) . . ? C11 U1 C4 170.7(3) . . ? C5 U1 C4 29.4(3) . . ? C13 U1 C4 129.5(3) . . ? C14 U1 C4 125.1(3) . . ? C2 U1 C4 48.1(3) . . ? O1 U1 C15 113.6(3) . . ? C12 U1 C15 49.5(3) . . ? C1 U1 C15 135.4(3) . . ? C11 U1 C15 29.9(3) . . ? C5 U1 C15 161.8(3) . . ? C13 U1 C15 49.6(3) . . ? C14 U1 C15 29.6(3) . . ? C2 U1 C15 113.3(3) . . ? C4 U1 C15 140.8(3) . . ? O1 U1 C3 129.2(3) . . ? C12 U1 C3 133.8(3) . . ? C1 U1 C3 48.1(3) . . ? C11 U1 C3 143.9(3) . . ? C5 U1 C3 47.9(3) . . ? C13 U1 C3 103.8(3) . . ? C14 U1 C3 96.1(3) . . ? C2 U1 C3 28.5(3) . . ? C4 U1 C3 29.0(2) . . ? C15 U1 C3 116.2(3) . . ? O1 U1 Se1 100.09(19) . . ? C12 U1 Se1 129.0(2) . . ? C1 U1 Se1 121.5(2) . . ? C11 U1 Se1 100.2(2) . . ? C5 U1 Se1 100.0(2) . . ? C13 U1 Se1 127.81(19) . . ? C14 U1 Se1 98.9(2) . . ? C2 U1 Se1 105.3(2) . . ? C4 U1 Se1 73.5(2) . . ? C15 U1 Se1 82.4(2) . . ? C3 U1 Se1 77.6(2) . . ? C21 Se1 U1 109.3(3) . . ? C27 O1 U1 176.8(7) . . ? C2 C1 C5 107.5(9) . . ? C2 C1 C6 127.7(10) . . ? C5 C1 C6 124.4(10) . . ? C2 C1 U1 77.3(5) . . ? C5 C1 U1 76.2(5) . . ? C6 C1 U1 118.0(6) . . ? C3 C2 C1 108.0(9) . . ? C3 C2 C7 123.8(10) . . ? C1 C2 C7 126.0(10) . . ? C3 C2 U1 77.0(5) . . ? C1 C2 U1 73.0(5) . . ? C7 C2 U1 129.4(6) . . ? C2 C3 C4 109.3(9) . . ? C2 C3 C8 125.9(9) . . ? C4 C3 C8 124.6(10) . . ? C2 C3 U1 74.5(5) . . ? C4 C3 U1 74.3(5) . . ? C8 C3 U1 122.3(6) . . ? C3 C4 C5 107.4(9) . . ? C3 C4 C9 127.3(10) . . ? C5 C4 C9 124.1(10) . . ? C3 C4 U1 76.7(5) . . ? C5 C4 U1 74.2(5) . . ? C9 C4 U1 124.6(6) . . ? C4 C5 C1 107.8(8) . . ? C4 C5 C10 125.9(10) . . ? C1 C5 C10 125.4(10) . . ? C4 C5 U1 76.4(5) . . ? C1 C5 U1 74.0(5) . . ? C10 C5 U1 124.3(6) . . ? C12 C11 C15 110.0(8) . . ? C12 C11 C20 126.7(9) . . ? C15 C11 C20 122.6(9) . . ? C12 C11 U1 73.7(5) . . ? C15 C11 U1 76.5(5) . . ? C20 C11 U1 124.8(6) . . ? C11 C12 C13 108.4(8) . . ? C11 C12 C16 128.3(9) . . ? C13 C12 C16 123.0(9) . . ? C11 C12 U1 77.0(6) . . ? C13 C12 U1 76.8(5) . . ? C16 C12 U1 117.6(6) . . ? C14 C13 C12 105.6(9) . . ? C14 C13 C17 130.0(10) . . ? C12 C13 C17 123.3(9) . . ? C14 C13 U1 75.6(5) . . ? C12 C13 U1 72.7(5) . . ? C17 C13 U1 125.9(6) . . ? C13 C14 C15 111.8(9) . . ? C13 C14 C18 128.4(9) . . ? C15 C14 C18 119.7(9) . . ? C13 C14 U1 75.3(5) . . ? C15 C14 U1 76.0(5) . . ? C18 C14 U1 119.6(6) . . ? C14 C15 C11 104.2(8) . . ? C14 C15 C19 126.9(9) . . ? C11 C15 C19 127.7(9) . . ? C14 C15 U1 74.3(5) . . ? C11 C15 U1 73.6(5) . . ? C19 C15 U1 126.1(7) . . ? C26 C21 C22 116.6(10) . . ? C26 C21 Se1 123.7(8) . . ? C22 C21 Se1 119.7(8) . . ? C23 C22 C21 119.9(12) . . ? C24 C23 C22 122.8(12) . . ? C23 C24 C25 117.5(11) . . ? C24 C25 C26 120.9(11) . . ? C21 C26 C25 122.1(10) . . ? O1 C27 C30 109.0(9) . . ? O1 C27 C29 109.2(8) . . ? C30 C27 C29 112.1(9) . . ? O1 C27 C28 107.4(8) . . ? C30 C27 C28 111.0(9) . . ? C29 C27 C28 108.1(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.905 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.226 #===============END===============