# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'F. Cloke' 'P. B. Hitchcock' 'Christopher P. Larch' _publ_contact_author_name 'F. Cloke' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Sussex School of Life Sciences BRIGHTON Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email F.G.CLOKE@SUSSEX.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Activation and reduction of diethylether by low valent uranium: formation of the trimetallic, mixed valence uranium oxo species [U(CpR)(? I)2]3(?3 O) (CpR = C5Me5, C5Me4H, C5H4SiMe3) ; _publ_requested_category FM data_dec705 _database_code_depnum_ccdc_archive 'CCDC 661103' _audit_creation_date 2005-12-13T09:32:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H39 I6 O Si3 U3' _chemical_formula_sum 'C24 H39 I6 O Si3 U3' _chemical_formula_weight 1903.31 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 16.7070(3) _cell_length_b 8.3748(1) _cell_length_c 31.3762(4) _cell_angle_alpha 90 _cell_angle_beta 102.745(1) _cell_angle_gamma 90 _cell_volume 4281.92(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 173999 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3308 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.01 -1 0 0 0.01 0 1 0 0.2 0 -1 0 0.2 0 0 1 0.2 0 0 -1 0.2 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 15.745 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (see. N.W. Alcock (1970). Cryst. Computing, p271) ; _exptl_absorpt_correction_T_min 0.0354 _exptl_absorpt_correction_T_max 0.7279 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.322147E-1 _diffrn_orient_matrix_ub_12 0.614807E-1 _diffrn_orient_matrix_ub_13 0.253842E-1 _diffrn_orient_matrix_ub_21 0.518921E-1 _diffrn_orient_matrix_ub_22 -0.268517E-1 _diffrn_orient_matrix_ub_23 -0.93344E-2 _diffrn_orient_matrix_ub_31 -0.59446E-2 _diffrn_orient_matrix_ub_32 0.987768E-1 _diffrn_orient_matrix_ub_33 -0.183372E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1254 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_number 61341 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 25.97 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 8349 _reflns_number_gt 6849 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0655P)^2^+20.2028P] 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_number_reflns 8349 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.11 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.959 _refine_diff_density_min -2.543 _refine_diff_density_rms 0.333 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 0.48441(2) 0.71560(4) 0.140502(12) 0.02728(11) Uani 1 1 d . . . U2 U 0.33225(2) 0.72149(4) 0.031384(12) 0.03115(11) Uani 1 1 d . . . U3 U 0.27679(2) 0.93461(4) 0.129011(13) 0.03310(12) Uani 1 1 d . . . I1 I 0.42157(5) 0.42196(8) 0.08002(2) 0.03857(18) Uani 1 1 d . A 1 I2 I 0.52014(4) 0.84249(8) 0.05153(2) 0.03783(17) Uani 1 1 d . A 1 I3 I 0.26834(5) 1.06860(8) 0.03158(3) 0.0482(2) Uani 1 1 d . A 1 I4 I 0.17936(4) 0.64705(9) 0.07148(3) 0.04560(19) Uani 1 1 d . A 1 I5 I 0.45720(4) 1.06742(7) 0.16961(2) 0.03688(17) Uani 1 1 d . A 1 I6 I 0.35479(4) 0.65666(9) 0.19845(2) 0.04105(18) Uani 1 1 d . A 1 Si1 Si 0.72514(19) 0.8803(4) 0.16637(11) 0.0394(7) Uani 1 1 d . A 1 Si2 Si 0.1170(2) 0.6420(6) -0.06400(13) 0.0676(11) Uani 1 1 d . A 1 Si3 Si 0.1138(3) 0.8703(6) 0.20842(17) 0.0780(14) Uani 1 1 d . A 1 O1 O 0.3683(4) 0.7882(8) 0.0993(2) 0.0358(16) Uani 1 1 d . A 1 C1 C 0.6489(6) 0.7279(11) 0.1747(3) 0.031(2) Uani 1 1 d . A 1 C2 C 0.6105(6) 0.7127(12) 0.2106(4) 0.037(2) Uani 1 1 d . A 1 H2 H 0.6095 0.7933 0.2318 0.045 Uiso 1 1 calc R A 1 C3 C 0.5740(6) 0.5605(13) 0.2103(4) 0.040(3) Uani 1 1 d . A 1 H3 H 0.5442 0.5218 0.2307 0.049 Uiso 1 1 calc R A 1 C4 C 0.5898(7) 0.4771(13) 0.1743(4) 0.041(3) Uani 1 1 d . A 1 H4 H 0.5728 0.371 0.1661 0.049 Uiso 1 1 calc R A 1 C5 C 0.6347(6) 0.5767(11) 0.1526(4) 0.035(2) Uani 1 1 d . A 1 H5 H 0.6531 0.5488 0.127 0.043 Uiso 1 1 calc R A 1 C6 C 0.6784(8) 1.0828(12) 0.1584(4) 0.048(3) Uani 1 1 d . A 1 H6A H 0.72 1.1603 0.1542 0.072 Uiso 1 1 calc R A 1 H6B H 0.6576 1.1124 0.1842 0.072 Uiso 1 1 calc R A 1 H6C H 0.6331 1.0825 0.1325 0.072 Uiso 1 1 calc R A 1 C7 C 0.8079(9) 0.878(2) 0.2171(6) 0.086(6) Uani 1 1 d . A 1 H7A H 0.8497 0.9574 0.2147 0.13 Uiso 1 1 calc R A 1 H7B H 0.8331 0.7716 0.221 0.13 Uiso 1 1 calc R A 1 H7C H 0.7845 0.9031 0.2423 0.13 Uiso 1 1 calc R A 1 C8 C 0.7674(9) 0.8210(15) 0.1191(6) 0.067(4) Uani 1 1 d . A 1 H8A H 0.8073 0.9011 0.1143 0.1 Uiso 1 1 calc R A 1 H8B H 0.7228 0.8135 0.093 0.1 Uiso 1 1 calc R A 1 H8C H 0.7946 0.7171 0.1249 0.1 Uiso 1 1 calc R A 1 C9 C 0.2325(7) 0.6474(14) -0.0475(3) 0.043(3) Uani 1 1 d . A 1 C10 C 0.2846(8) 0.7740(12) -0.0563(3) 0.045(3) Uani 1 1 d . A 1 H10 H 0.2672 0.8788 -0.0656 0.054 Uiso 1 1 calc R A 1 C11 C 0.3644(8) 0.7178(15) -0.0491(4) 0.049(3) Uani 1 1 d . A 1 H11 H 0.4106 0.7787 -0.0523 0.058 Uiso 1 1 calc R A 1 C12 C 0.3665(8) 0.5596(13) -0.0364(4) 0.045(3) Uani 1 1 d . A 1 H12 H 0.4138 0.4935 -0.0296 0.054 Uiso 1 1 calc R A 1 C13 C 0.2855(8) 0.5141(13) -0.0354(4) 0.047(3) Uani 1 1 d . A 1 H13 H 0.2691 0.4112 -0.0279 0.057 Uiso 1 1 calc R A 1 C14 C 0.0686(11) 0.816(2) -0.0444(6) 0.103(7) Uani 1 1 d . A 1 H14A H 0.0088 0.8068 -0.0538 0.155 Uiso 1 1 calc R A 1 H14B H 0.0869 0.9136 -0.0565 0.155 Uiso 1 1 calc R A 1 H14C H 0.0842 0.8199 -0.0124 0.155 Uiso 1 1 calc R A 1 C15 C 0.0938(12) 0.653(3) -0.1259(5) 0.115(7) Uani 1 1 d . A 1 H15A H 0.0342 0.6506 -0.1372 0.172 Uiso 1 1 calc R A 1 H15B H 0.119 0.5619 -0.1374 0.172 Uiso 1 1 calc R A 1 H15C H 0.1161 0.7526 -0.1349 0.172 Uiso 1 1 calc R A 1 C16 C 0.0801(10) 0.451(2) -0.0451(6) 0.086(5) Uani 1 1 d . A 1 H16A H 0.0201 0.4467 -0.0536 0.128 Uiso 1 1 calc R A 1 H16B H 0.0978 0.443 -0.0133 0.128 Uiso 1 1 calc R A 1 H16C H 0.1031 0.361 -0.0586 0.128 Uiso 1 1 calc R A 1 C17 C 0.1606(7) 1.0054(14) 0.1749(4) 0.043(3) Uani 1 1 d . A 1 C18 C 0.1274(8) 1.0561(16) 0.1315(4) 0.055(3) Uani 1 1 d . A 1 H18 H 0.082 1.0058 0.1127 0.066 Uiso 1 1 calc R A 1 C19 C 0.1667(10) 1.1819(19) 0.1197(6) 0.072(4) Uani 1 1 d . A 1 H19 H 0.1531 1.2339 0.0921 0.087 Uiso 1 1 calc R A 1 C20 C 0.2272(11) 1.2222(16) 0.1525(7) 0.078(5) Uani 1 1 d . A 1 H20 H 0.265 1.3068 0.1521 0.093 Uiso 1 1 calc R A 1 C21 C 0.2269(8) 1.114(2) 0.1901(5) 0.078(5) Uani 1 1 d . A 1 H21 H 0.263 1.1162 0.2181 0.094 Uiso 1 1 calc R A 1 C22 C 0.1894(12) 0.851(2) 0.2657(6) 0.097(6) Uani 1 1 d . A 1 H22A H 0.2008 0.9577 0.2786 0.145 Uiso 1 1 calc R A 1 H22B H 0.2407 0.8021 0.2622 0.145 Uiso 1 1 calc R A 1 H22C H 0.1643 0.7848 0.2849 0.145 Uiso 1 1 calc R A 1 C23 C 0.0262(13) 0.975(3) 0.2214(9) 0.140(10) Uani 1 1 d . A 1 H23A H 0.044 1.0793 0.2343 0.211 Uiso 1 1 calc R A 1 H23B H 0.0037 0.9117 0.2423 0.211 Uiso 1 1 calc R A 1 H23C H -0.0162 0.9903 0.1947 0.211 Uiso 1 1 calc R A 1 C24 C 0.0930(15) 0.676(3) 0.1845(7) 0.132(9) Uani 1 1 d . A 1 H24A H 0.0689 0.6079 0.2039 0.198 Uiso 1 1 calc R A 1 H24B H 0.1443 0.6274 0.1805 0.198 Uiso 1 1 calc R A 1 H24C H 0.0545 0.685 0.1561 0.198 Uiso 1 1 calc R A 1 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 0.0246(2) 0.0331(2) 0.0223(2) 0.00209(14) 0.00142(15) -0.00280(14) U2 0.0316(2) 0.0361(2) 0.0230(2) 0.00156(14) -0.00008(16) -0.00600(15) U3 0.0274(2) 0.0358(2) 0.0354(2) -0.00024(16) 0.00526(16) -0.00062(15) I1 0.0442(4) 0.0323(3) 0.0342(4) 0.0019(3) -0.0020(3) -0.0067(3) I2 0.0373(4) 0.0463(4) 0.0291(4) 0.0050(3) 0.0057(3) -0.0124(3) I3 0.0546(5) 0.0375(4) 0.0451(5) 0.0099(3) -0.0048(4) -0.0050(3) I4 0.0323(4) 0.0519(4) 0.0488(5) 0.0056(3) 0.0008(3) -0.0148(3) I5 0.0361(4) 0.0361(3) 0.0356(4) -0.0010(3) 0.0019(3) -0.0076(3) I6 0.0383(4) 0.0492(4) 0.0378(4) 0.0113(3) 0.0131(3) -0.0025(3) Si1 0.0286(16) 0.0449(16) 0.0432(18) 0.0029(13) 0.0044(13) -0.0069(13) Si2 0.041(2) 0.106(3) 0.045(2) -0.006(2) -0.0125(17) -0.010(2) Si3 0.068(3) 0.092(3) 0.089(3) 0.031(3) 0.049(3) 0.025(2) O1 0.028(4) 0.046(4) 0.030(4) 0.003(3) -0.003(3) -0.001(3) C1 0.027(5) 0.039(5) 0.025(5) 0.000(4) 0.000(4) 0.004(4) C2 0.027(6) 0.040(6) 0.040(6) 0.002(5) -0.005(5) -0.001(4) C3 0.022(5) 0.064(7) 0.029(6) 0.021(5) -0.007(4) -0.007(5) C4 0.039(6) 0.038(5) 0.037(6) 0.006(5) -0.011(5) 0.000(5) C5 0.028(6) 0.041(6) 0.034(6) 0.007(4) 0.001(4) 0.004(4) C6 0.048(7) 0.045(6) 0.055(8) -0.006(5) 0.020(6) -0.015(5) C7 0.048(9) 0.103(12) 0.087(12) 0.039(9) -0.031(8) -0.043(8) C8 0.052(9) 0.053(7) 0.110(13) 0.001(7) 0.049(9) 0.006(6) C9 0.038(6) 0.056(7) 0.027(6) -0.005(5) -0.010(5) -0.012(5) C10 0.074(9) 0.037(6) 0.019(5) 0.008(4) 0.000(5) -0.003(5) C11 0.049(8) 0.069(8) 0.024(6) -0.008(5) 0.001(5) -0.014(6) C12 0.048(8) 0.053(7) 0.033(6) -0.002(5) 0.004(5) 0.001(5) C13 0.067(9) 0.038(6) 0.033(6) -0.006(5) 0.002(6) -0.009(6) C14 0.067(12) 0.141(16) 0.079(13) 0.016(11) -0.032(10) 0.027(11) C15 0.087(14) 0.21(2) 0.032(9) 0.002(11) -0.027(9) -0.010(14) C16 0.050(9) 0.126(14) 0.074(12) -0.018(10) 0.000(8) -0.034(9) C17 0.030(6) 0.062(7) 0.034(6) 0.003(5) 0.002(5) 0.008(5) C18 0.037(7) 0.075(9) 0.055(8) 0.018(6) 0.014(6) 0.018(6) C19 0.062(10) 0.077(10) 0.089(13) 0.022(9) 0.039(10) 0.024(8) C20 0.058(10) 0.048(8) 0.141(18) -0.008(9) 0.054(11) -0.002(7) C21 0.038(8) 0.117(13) 0.077(11) -0.066(10) 0.006(7) 0.020(8) C22 0.102(15) 0.110(14) 0.081(13) 0.004(10) 0.029(11) 0.027(11) C23 0.079(15) 0.19(2) 0.18(3) 0.049(19) 0.082(17) 0.051(15) C24 0.13(2) 0.18(2) 0.098(16) 0.001(15) 0.046(14) -0.089(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.168(7) . ? U1 C2 2.689(10) . ? U1 C3 2.697(10) . ? U1 C5 2.717(10) . ? U1 C4 2.718(10) . ? U1 C1 2.722(10) . ? U1 I1 3.1420(7) . ? U1 I5 3.1473(7) . ? U1 I6 3.1586(8) . ? U1 I2 3.1644(7) . ? U2 O1 2.156(7) . ? U2 C12 2.688(11) . ? U2 C11 2.694(11) . ? U2 C13 2.701(11) . ? U2 C10 2.726(10) . ? U2 C9 2.734(10) . ? U2 I3 3.0973(8) . ? U2 I1 3.1375(8) . ? U2 I4 3.1486(8) . ? U2 I2 3.2256(8) . ? U3 O1 2.311(7) . ? U3 C20 2.702(13) . ? U3 C21 2.706(12) . ? U3 C18 2.712(12) . ? U3 C17 2.726(11) . ? U3 C19 2.743(14) . ? U3 I5 3.2017(8) . ? U3 I4 3.2266(8) . ? U3 I3 3.2302(9) . ? U3 I6 3.2574(8) . ? Si1 C8 1.846(14) . ? Si1 C6 1.861(12) . ? Si1 C1 1.862(11) . ? Si1 C7 1.864(14) . ? Si2 C14 1.84(2) . ? Si2 C16 1.861(17) . ? Si2 C9 1.884(12) . ? Si2 C15 1.896(16) . ? Si3 C24 1.80(2) . ? Si3 C23 1.828(18) . ? Si3 C17 1.832(12) . ? Si3 C22 1.96(2) . ? C1 C2 1.419(15) . ? C1 C5 1.438(14) . ? C2 C3 1.413(14) . ? C2 H2 0.95 . ? C3 C4 1.401(16) . ? C3 H3 0.95 . ? C4 C5 1.397(15) . ? C4 H4 0.95 . ? C5 H5 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C13 1.424(17) . ? C9 C10 1.437(16) . ? C10 C11 1.384(18) . ? C10 H10 0.95 . ? C11 C12 1.381(16) . ? C11 H11 0.95 . ? C12 C13 1.412(17) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.419(17) . ? C17 C21 1.431(19) . ? C18 C19 1.335(19) . ? C18 H18 0.95 . ? C19 C20 1.32(2) . ? C19 H19 0.95 . ? C20 C21 1.49(2) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? 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 C2 158.0(3) . . ? O1 U1 C3 152.0(3) . . ? C2 U1 C3 30.4(3) . . ? O1 U1 C5 151.8(3) . . ? C2 U1 C5 49.4(3) . . ? C3 U1 C5 49.5(3) . . ? O1 U1 C4 148.9(3) . . ? C2 U1 C4 49.5(3) . . ? C3 U1 C4 30.0(3) . . ? C5 U1 C4 29.8(3) . . ? O1 U1 C1 156.5(3) . . ? C2 U1 C1 30.4(3) . . ? C3 U1 C1 50.7(3) . . ? C5 U1 C1 30.7(3) . . ? C4 U1 C1 50.5(3) . . ? O1 U1 I1 73.94(18) . . ? C2 U1 I1 125.7(2) . . ? C3 U1 I1 99.5(2) . . ? C5 U1 I1 85.7(2) . . ? C4 U1 I1 76.2(2) . . ? C1 U1 I1 116.2(2) . . ? O1 U1 I5 75.11(18) . . ? C2 U1 I5 84.7(2) . . ? C3 U1 I5 107.8(3) . . ? C5 U1 I5 123.3(2) . . ? C4 U1 I5 134.2(2) . . ? C1 U1 I5 92.7(2) . . ? I1 U1 I5 149.05(2) . . ? O1 U1 I6 75.54(19) . . ? C2 U1 I6 92.3(2) . . ? C3 U1 I6 77.6(2) . . ? C5 U1 I6 125.6(2) . . ? C4 U1 I6 97.3(3) . . ? C1 U1 I6 122.6(2) . . ? I1 U1 I6 92.59(2) . . ? I5 U1 I6 79.51(2) . . ? O1 U1 I2 72.40(19) . . ? C2 U1 I2 117.3(2) . . ? C3 U1 I2 134.4(2) . . ? C5 U1 I2 85.3(2) . . ? C4 U1 I2 111.1(3) . . ? C1 U1 I2 88.0(2) . . ? I1 U1 I2 80.39(2) . . ? I5 U1 I2 90.52(2) . . ? I6 U1 I2 147.89(2) . . ? O1 U2 C12 148.3(3) . . ? O1 U2 C11 149.2(3) . . ? C12 U2 C11 29.7(3) . . ? O1 U2 C13 154.6(3) . . ? C12 U2 C13 30.4(4) . . ? C11 U2 C13 49.4(4) . . ? O1 U2 C10 155.7(3) . . ? C12 U2 C10 49.3(4) . . ? C11 U2 C10 29.6(4) . . ? C13 U2 C10 49.5(3) . . ? O1 U2 C9 159.3(3) . . ? C12 U2 C9 50.4(4) . . ? C11 U2 C9 50.0(4) . . ? C13 U2 C9 30.4(4) . . ? C10 U2 C9 30.5(3) . . ? O1 U2 I3 77.05(18) . . ? C12 U2 I3 127.5(2) . . ? C11 U2 I3 98.8(3) . . ? C13 U2 I3 124.3(3) . . ? C10 U2 I3 80.0(2) . . ? C9 U2 I3 94.2(2) . . ? O1 U2 I1 74.18(18) . . ? C12 U2 I1 79.6(3) . . ? C11 U2 I1 106.0(3) . . ? C13 U2 I1 83.6(3) . . ? C10 U2 I1 128.4(2) . . ? C9 U2 I1 112.9(2) . . ? I3 U2 I1 151.24(2) . . ? O1 U2 I4 74.38(19) . . ? C12 U2 I4 123.3(3) . . ? C11 U2 I4 136.0(3) . . ? C13 U2 I4 93.5(3) . . ? C10 U2 I4 110.7(3) . . ? C9 U2 I4 86.0(3) . . ? I3 U2 I4 82.80(2) . . ? I1 U2 I4 89.32(2) . . ? O1 U2 I2 71.18(19) . . ? C12 U2 I2 86.9(3) . . ? C11 U2 I2 78.5(3) . . ? C13 U2 I2 117.1(3) . . ? C10 U2 I2 101.7(3) . . ? C9 U2 I2 128.4(3) . . ? I3 U2 I2 91.48(2) . . ? I1 U2 I2 79.51(2) . . ? I4 U2 I2 145.49(2) . . ? O1 U3 C20 148.5(4) . . ? O1 U3 C21 156.1(4) . . ? C20 U3 C21 32.0(5) . . ? O1 U3 C18 154.9(4) . . ? C20 U3 C18 47.0(5) . . ? C21 U3 C18 48.9(4) . . ? O1 U3 C17 160.1(3) . . ? C20 U3 C17 50.6(4) . . ? C21 U3 C17 30.5(4) . . ? C18 U3 C17 30.3(4) . . ? O1 U3 C19 147.7(4) . . ? C20 U3 C19 28.0(5) . . ? C21 U3 C19 49.6(5) . . ? C18 U3 C19 28.3(4) . . ? C17 U3 C19 49.7(4) . . ? O1 U3 I5 72.33(17) . . ? C20 U3 I5 84.3(4) . . ? C21 U3 I5 86.3(3) . . ? C18 U3 I5 130.5(3) . . ? C17 U3 I5 115.6(2) . . ? C19 U3 I5 109.3(4) . . ? O1 U3 I4 71.04(17) . . ? C20 U3 I4 132.1(4) . . ? C21 U3 I4 127.9(3) . . ? C18 U3 I4 86.7(3) . . ? C17 U3 I4 97.3(3) . . ? C19 U3 I4 105.1(4) . . ? I5 U3 I4 142.78(2) . . ? O1 U3 I3 72.35(17) . . ? C20 U3 I3 89.8(5) . . ? C21 U3 I3 121.4(4) . . ? C18 U3 I3 92.8(3) . . ? C17 U3 I3 122.5(2) . . ? C19 U3 I3 75.4(3) . . ? I5 U3 I3 95.54(2) . . ? I4 U3 I3 79.54(2) . . ? O1 U3 I6 71.84(17) . . ? C20 U3 I6 123.8(5) . . ? C21 U3 I6 93.6(4) . . ? C18 U3 I6 118.9(3) . . ? C17 U3 I6 91.6(2) . . ? C19 U3 I6 140.4(3) . . ? I5 U3 I6 77.265(19) . . ? I4 U3 I6 85.35(2) . . ? I3 U3 I6 143.98(2) . . ? U2 I1 U1 74.197(17) . . ? U1 I2 U2 72.697(17) . . ? U2 I3 U3 74.498(18) . . ? U2 I4 U3 73.869(18) . . ? U1 I5 U3 75.099(17) . . ? U1 I6 U3 74.169(17) . . ? C8 Si1 C6 111.1(6) . . ? C8 Si1 C1 108.9(6) . . ? C6 Si1 C1 111.4(5) . . ? C8 Si1 C7 109.9(8) . . ? C6 Si1 C7 109.6(7) . . ? C1 Si1 C7 105.9(5) . . ? C14 Si2 C16 112.1(9) . . ? C14 Si2 C9 112.9(7) . . ? C16 Si2 C9 108.9(7) . . ? C14 Si2 C15 107.4(9) . . ? C16 Si2 C15 111.1(9) . . ? C9 Si2 C15 104.2(7) . . ? C24 Si3 C23 116.0(12) . . ? C24 Si3 C17 112.9(7) . . ? C23 Si3 C17 107.2(9) . . ? C24 Si3 C22 109.6(10) . . ? C23 Si3 C22 102.7(11) . . ? C17 Si3 C22 107.8(7) . . ? U2 O1 U1 122.3(3) . . ? U2 O1 U3 118.1(3) . . ? U1 O1 U3 119.5(3) . . ? C2 C1 C5 104.4(9) . . ? C2 C1 Si1 128.0(8) . . ? C5 C1 Si1 125.5(8) . . ? C2 C1 U1 73.5(6) . . ? C5 C1 U1 74.5(6) . . ? Si1 C1 U1 129.3(5) . . ? C3 C2 C1 110.2(10) . . ? C3 C2 U1 75.1(6) . . ? C1 C2 U1 76.1(6) . . ? C3 C2 H2 124.9 . . ? C1 C2 H2 124.9 . . ? U1 C2 H2 115.8 . . ? C4 C3 C2 107.3(10) . . ? C4 C3 U1 75.8(6) . . ? C2 C3 U1 74.5(6) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? U1 C3 H3 115.6 . . ? C5 C4 C3 108.2(9) . . ? C5 C4 U1 75.0(6) . . ? C3 C4 U1 74.2(6) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? U1 C4 H4 116.9 . . ? C4 C5 C1 109.8(10) . . ? C4 C5 U1 75.2(6) . . ? C1 C5 U1 74.9(6) . . ? C4 C5 H5 125.1 . . ? C1 C5 H5 125.1 . . ? U1 C5 H5 116.7 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 C9 C10 105.2(11) . . ? C13 C9 Si2 126.5(9) . . ? C10 C9 Si2 126.3(9) . . ? C13 C9 U2 73.6(6) . . ? C10 C9 U2 74.4(6) . . ? Si2 C9 U2 129.6(6) . . ? C11 C10 C9 108.7(10) . . ? C11 C10 U2 73.9(6) . . ? C9 C10 U2 75.0(6) . . ? C11 C10 H10 125.7 . . ? C9 C10 H10 125.7 . . ? U2 C10 H10 117.3 . . ? C12 C11 C10 109.6(11) . . ? C12 C11 U2 74.9(7) . . ? C10 C11 U2 76.5(7) . . ? C12 C11 H11 125.2 . . ? C10 C11 H11 125.2 . . ? U2 C11 H11 115.4 . . ? C11 C12 C13 107.5(11) . . ? C11 C12 U2 75.4(7) . . ? C13 C12 U2 75.3(7) . . ? C11 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? U2 C12 H12 115.3 . . ? C12 C13 C9 109.0(10) . . ? C12 C13 U2 74.3(6) . . ? C9 C13 U2 76.1(6) . . ? C12 C13 H13 125.5 . . ? C9 C13 H13 125.5 . . ? U2 C13 H13 116.1 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C21 103.8(12) . . ? C18 C17 Si3 127.6(9) . . ? C21 C17 Si3 126.8(11) . . ? C18 C17 U3 74.3(7) . . ? C21 C17 U3 74.0(7) . . ? Si3 C17 U3 127.8(6) . . ? C19 C18 C17 113.0(14) . . ? C19 C18 U3 77.1(8) . . ? C17 C18 U3 75.4(7) . . ? C19 C18 H18 123.5 . . ? C17 C18 H18 123.5 . . ? U3 C18 H18 115.5 . . ? C20 C19 C18 109.0(15) . . ? C20 C19 U3 74.3(9) . . ? C18 C19 U3 74.6(8) . . ? C20 C19 H19 125.5 . . ? C18 C19 H19 125.5 . . ? U3 C19 H19 117.6 . . ? C19 C20 C21 109.0(13) . . ? C19 C20 U3 77.7(9) . . ? C21 C20 U3 74.2(7) . . ? C19 C20 H20 125.5 . . ? C21 C20 H20 125.5 . . ? U3 C20 H20 114.7 . . ? C17 C21 C20 105.1(13) . . ? C17 C21 U3 75.5(7) . . ? C20 C21 U3 73.8(8) . . ? C17 C21 H21 127.4 . . ? C20 C21 H21 127.4 . . ? U3 C21 H21 115.8 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? #===END # Attachment 'jan703.cif' data_jan703 _database_code_depnum_ccdc_archive 'CCDC 661104' _audit_creation_date 2007-07-31T13:45:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H45 I6 O U3' _chemical_formula_sum 'C30 H45 I6 O U3' _chemical_formula_weight 1897.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 24.5979(5) _cell_length_b 21.5504(4) _cell_length_c 16.6282(3) _cell_angle_alpha 90 _cell_angle_beta 109.891(1) _cell_angle_gamma 90 _cell_volume 8288.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 167899 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.713 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 3.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6616 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.2226 _exptl_absorpt_correction_T_max 0.3167 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_unetI/netI 0.0617 _diffrn_reflns_number 55482 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 24.67 _diffrn_reflns_theta_full 24.67 _diffrn_measured_fraction_theta_full 0.95 _diffrn_measured_fraction_theta_max 0.95 _reflns_number_total 13374 _reflns_number_gt 11825 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The crystal is twinned with matrix (1 0 1 0 -1 0 0 0 -1), BASF=0.457 The U and I atoms were anisotropic; other non-H atoms were left isotropic. 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^)+(0.0499P)^2^+114.3734P] 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_number_reflns 13374 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.257 _refine_diff_density_min -2.546 _refine_diff_density_rms 0.355 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 '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' 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 0.13546(3) 0.64783(3) 0.32905(5) 0.0200(2) Uani 1 1 d . . . U2 U 0.13068(3) 0.82675(3) 0.31589(4) 0.0204(2) Uani 1 1 d . . . U3 U 0.26974(4) 0.74429(3) 0.44949(5) 0.01928(18) Uani 1 1 d . A . U1B U 0.36951(3) 0.32929(4) 0.68329(5) 0.0207(2) Uani 1 1 d . . . U2B U 0.36347(3) 0.14997(4) 0.68382(5) 0.0213(2) Uani 1 1 d . . . U3B U 0.23009(4) 0.24766(4) 0.67379(5) 0.01886(18) Uani 1 1 d . B . I1 I 0.09834(6) 0.73236(6) 0.15971(9) 0.0320(3) Uani 1 1 d . A 1 I2 I 0.04376(6) 0.73473(6) 0.36982(10) 0.0332(4) Uani 1 1 d . A 1 I3 I 0.20084(6) 0.84646(6) 0.51441(8) 0.0282(3) Uani 1 1 d . A 1 I4 I 0.25621(6) 0.84477(6) 0.30436(9) 0.0297(3) Uani 1 1 d . A 1 I5 I 0.26290(6) 0.63853(6) 0.31529(9) 0.0306(3) Uani 1 1 d . A 1 I6 I 0.21208(6) 0.63862(6) 0.52725(8) 0.0321(3) Uani 1 1 d . A 1 O1 O 0.1790(6) 0.7396(5) 0.3661(8) 0.020(3) Uiso 1 1 d . A 1 C1 C 0.1079(9) 0.5477(9) 0.2263(13) 0.030(5) Uiso 1 1 d . A 1 C2 C 0.1401(8) 0.5229(8) 0.3111(11) 0.024(4) Uiso 1 1 d . A 1 C3 C 0.1061(8) 0.5302(8) 0.3634(12) 0.024(4) Uiso 1 1 d . A 1 C4 C 0.0512(8) 0.5574(8) 0.3133(12) 0.023(4) Uiso 1 1 d . A 1 C5 C 0.0549(8) 0.5674(9) 0.2311(12) 0.029(4) Uiso 1 1 d . A 1 C6 C 0.1286(11) 0.5460(11) 0.1517(15) 0.050(6) Uiso 1 1 d . A 1 H6A H 0.1173 0.5844 0.1186 0.075 Uiso 1 1 calc R A 1 H6B H 0.1112 0.5104 0.1152 0.075 Uiso 1 1 calc R A 1 H6C H 0.1708 0.542 0.1721 0.075 Uiso 1 1 calc R A 1 C7 C 0.1988(9) 0.4899(9) 0.3412(13) 0.032(5) Uiso 1 1 d . A 1 H7A H 0.1945 0.4487 0.3633 0.048 Uiso 1 1 calc R A 1 H7B H 0.2265 0.5143 0.3866 0.048 Uiso 1 1 calc R A 1 H7C H 0.2129 0.4855 0.2931 0.048 Uiso 1 1 calc R A 1 C8 C 0.1182(9) 0.5017(9) 0.4502(12) 0.034(5) Uiso 1 1 d . A 1 H8A H 0.1589 0.5082 0.4847 0.051 Uiso 1 1 calc R A 1 H8B H 0.11 0.4571 0.444 0.051 Uiso 1 1 calc R A 1 H8C H 0.0935 0.5212 0.4786 0.051 Uiso 1 1 calc R A 1 C9 C -0.0002(10) 0.5651(11) 0.3364(16) 0.050(6) Uiso 1 1 d . A 1 H9A H -0.0229 0.5267 0.3239 0.075 Uiso 1 1 calc R A 1 H9B H -0.0235 0.5993 0.3033 0.075 Uiso 1 1 calc R A 1 H9C H 0.0111 0.5744 0.3976 0.075 Uiso 1 1 calc R A 1 C10 C 0.0052(9) 0.5929(10) 0.1525(13) 0.040(5) Uiso 1 1 d . A 1 H10A H -0.0274 0.5639 0.1371 0.061 Uiso 1 1 calc R A 1 H10B H 0.019 0.5976 0.104 0.061 Uiso 1 1 calc R A 1 H10C H -0.0074 0.6333 0.1667 0.061 Uiso 1 1 calc R A 1 C11 C 0.1163(8) 0.9409(8) 0.2380(12) 0.023(4) Uiso 1 1 d . A 1 C12 C 0.0693(9) 0.9078(9) 0.1917(13) 0.032(5) Uiso 1 1 d . A 1 C13 C 0.0353(8) 0.8967(8) 0.2427(12) 0.026(4) Uiso 1 1 d . A 1 C14 C 0.0619(8) 0.9232(8) 0.3260(12) 0.023(4) Uiso 1 1 d . A 1 C15 C 0.1142(9) 0.9529(9) 0.3249(13) 0.031(5) Uiso 1 1 d . A 1 C16 C 0.1615(9) 0.9726(10) 0.2066(14) 0.043(5) Uiso 1 1 d . A 1 H16A H 0.1434 1.0071 0.1685 0.064 Uiso 1 1 calc R A 1 H16B H 0.1767 0.9424 0.1755 0.064 Uiso 1 1 calc R A 1 H16C H 0.1933 0.9884 0.2558 0.064 Uiso 1 1 calc R A 1 C17 C 0.0534(9) 0.8949(10) 0.0966(13) 0.039(5) Uiso 1 1 d . A 1 H17A H 0.0886 0.8922 0.0819 0.059 Uiso 1 1 calc R A 1 H17B H 0.029 0.9287 0.064 0.059 Uiso 1 1 calc R A 1 H17C H 0.0321 0.8557 0.0826 0.059 Uiso 1 1 calc R A 1 C18 C -0.0232(10) 0.8663(11) 0.2133(16) 0.050(6) Uiso 1 1 d . A 1 H18A H -0.0254 0.8362 0.1682 0.075 Uiso 1 1 calc R A 1 H18B H -0.0532 0.898 0.191 0.075 Uiso 1 1 calc R A 1 H18C H -0.0292 0.845 0.2617 0.075 Uiso 1 1 calc R A 1 C19 C 0.0383(9) 0.9227(10) 0.3985(13) 0.035(5) Uiso 1 1 d . A 1 H19A H 0.0663 0.9419 0.4491 0.053 Uiso 1 1 calc R A 1 H19B H 0.0313 0.8797 0.4118 0.053 Uiso 1 1 calc R A 1 H19C H 0.0019 0.946 0.3818 0.053 Uiso 1 1 calc R A 1 C20 C 0.1529(10) 0.9947(10) 0.3891(14) 0.044(6) Uiso 1 1 d . A 1 H20A H 0.1469 0.9891 0.4439 0.066 Uiso 1 1 calc R A 1 H20B H 0.1446 1.0378 0.3702 0.066 Uiso 1 1 calc R A 1 H20C H 0.1932 0.9849 0.3959 0.066 Uiso 1 1 calc R A 1 C21 C 0.3539(8) 0.7728(8) 0.5988(12) 0.023(4) Uiso 1 1 d . A 1 C22 C 0.3642(8) 0.7116(9) 0.5844(12) 0.027(4) Uiso 1 1 d . A 1 C23 C 0.3840(8) 0.7070(9) 0.5133(12) 0.025(4) Uiso 1 1 d . A 1 C24 C 0.3852(9) 0.7680(9) 0.4836(13) 0.030(5) Uiso 1 1 d . A 1 C25 C 0.3667(7) 0.8101(8) 0.5363(12) 0.022(4) Uiso 1 1 d . A 1 C26 C 0.3384(10) 0.7958(11) 0.6741(13) 0.040(5) Uiso 1 1 d . A 1 H26A H 0.371 0.7889 0.727 0.059 Uiso 1 1 calc R A 1 H26B H 0.3045 0.7731 0.6768 0.059 Uiso 1 1 calc R A 1 H26C H 0.3296 0.8402 0.6673 0.059 Uiso 1 1 calc R A 1 C27 C 0.3665(9) 0.6575(9) 0.6459(13) 0.034(5) Uiso 1 1 d . A 1 H27A H 0.3302 0.6558 0.658 0.05 Uiso 1 1 calc R A 1 H27B H 0.3989 0.6637 0.6994 0.05 Uiso 1 1 calc R A 1 H27C H 0.3719 0.6184 0.6195 0.05 Uiso 1 1 calc R A 1 C28 C 0.4090(9) 0.6515(9) 0.4831(14) 0.039(5) Uiso 1 1 d . A 1 H28A H 0.3902 0.6136 0.4932 0.059 Uiso 1 1 calc R A 1 H28B H 0.4506 0.6492 0.5147 0.059 Uiso 1 1 calc R A 1 H28C H 0.4025 0.6556 0.4219 0.059 Uiso 1 1 calc R A 1 C29 C 0.4093(10) 0.7887(10) 0.4103(14) 0.043(5) Uiso 1 1 d . A 1 H29A H 0.4013 0.7561 0.3667 0.065 Uiso 1 1 calc R A 1 H29B H 0.4511 0.7955 0.4349 0.065 Uiso 1 1 calc R A 1 H29C H 0.3903 0.8273 0.3841 0.065 Uiso 1 1 calc R A 1 C30 C 0.3657(9) 0.8778(10) 0.5285(14) 0.041(5) Uiso 1 1 d . A 1 H30A H 0.3611 0.8964 0.5797 0.062 Uiso 1 1 calc R A 1 H30B H 0.3333 0.8903 0.4779 0.062 Uiso 1 1 calc R A 1 H30C H 0.402 0.8921 0.5229 0.062 Uiso 1 1 calc R A 1 I1B I 0.45570(6) 0.23649(6) 0.82021(10) 0.0331(4) Uani 1 1 d . B 1 I2B I 0.40229(7) 0.23913(7) 0.55623(10) 0.0339(4) Uani 1 1 d . B 1 I3B I 0.29204(6) 0.14378(6) 0.81003(9) 0.0283(3) Uani 1 1 d . B 1 I4B I 0.23595(6) 0.14587(6) 0.53923(8) 0.0294(3) Uani 1 1 d . B 1 I5B I 0.24298(6) 0.35534(7) 0.55206(9) 0.0311(3) Uani 1 1 d . B 1 I6B I 0.29887(6) 0.34606(6) 0.81255(8) 0.0308(3) Uani 1 1 d . B 1 O1B O 0.3200(7) 0.2436(6) 0.6761(9) 0.028(3) Uiso 1 1 d . B 1 C1B C 0.4318(8) 0.4125(8) 0.6242(12) 0.026(4) Uiso 1 1 d . B 1 C2B C 0.3830(9) 0.4470(9) 0.6273(13) 0.026(5) Uiso 1 1 d . B 1 C3B C 0.3876(9) 0.4539(9) 0.7120(13) 0.030(5) Uiso 1 1 d . B 1 C4B C 0.4393(9) 0.4238(9) 0.7627(13) 0.028(5) Uiso 1 1 d . B 1 C5B C 0.4670(9) 0.3986(9) 0.7108(12) 0.030(4) Uiso 1 1 d . B 1 C6B C 0.4494(10) 0.4028(11) 0.5480(15) 0.049(6) Uiso 1 1 d . B 1 H6B1 H 0.4653 0.4414 0.5343 0.074 Uiso 1 1 calc R B 1 H6B2 H 0.4156 0.3904 0.4992 0.074 Uiso 1 1 calc R B 1 H6B3 H 0.4788 0.3701 0.5601 0.074 Uiso 1 1 calc R B 1 C7B C 0.3424(9) 0.4783(9) 0.5490(13) 0.035(5) Uiso 1 1 d . B 1 H7B1 H 0.3618 0.514 0.5341 0.053 Uiso 1 1 calc R B 1 H7B2 H 0.3079 0.4925 0.5607 0.053 Uiso 1 1 calc R B 1 H7B3 H 0.331 0.4489 0.5013 0.053 Uiso 1 1 calc R B 1 C8B C 0.3479(10) 0.4937(11) 0.7452(15) 0.049(6) Uiso 1 1 d . B 1 H8B1 H 0.3075 0.4868 0.7094 0.073 Uiso 1 1 calc R B 1 H8B2 H 0.3576 0.5377 0.743 0.073 Uiso 1 1 calc R B 1 H8B3 H 0.3532 0.4821 0.8044 0.073 Uiso 1 1 calc R B 1 C9B C 0.4614(12) 0.4233(12) 0.8618(15) 0.057(7) Uiso 1 1 d . B 1 H9B1 H 0.4831 0.4615 0.8833 0.085 Uiso 1 1 calc R B 1 H9B2 H 0.4867 0.3873 0.8826 0.085 Uiso 1 1 calc R B 1 H9B3 H 0.4285 0.4207 0.882 0.085 Uiso 1 1 calc R B 1 C10B C 0.5257(9) 0.3676(10) 0.7372(14) 0.040(5) Uiso 1 1 d . B 1 H10D H 0.537 0.3546 0.7971 0.06 Uiso 1 1 calc R B 1 H10E H 0.5543 0.397 0.7306 0.06 Uiso 1 1 calc R B 1 H10F H 0.5238 0.3313 0.701 0.06 Uiso 1 1 calc R B 1 C11B C 0.4437(8) 0.0570(9) 0.7484(12) 0.025(4) Uiso 1 1 d . B 1 C12B C 0.3914(9) 0.0304(9) 0.7473(13) 0.032(5) Uiso 1 1 d . B 1 C13B C 0.3552(8) 0.0246(9) 0.6619(12) 0.027(4) Uiso 1 1 d . B 1 C14B C 0.3839(9) 0.0462(9) 0.6099(13) 0.027(4) Uiso 1 1 d . B 1 C15B C 0.4410(9) 0.0667(10) 0.6635(13) 0.035(5) Uiso 1 1 d . B 1 C16B C 0.4987(9) 0.0656(9) 0.8296(13) 0.035(5) Uiso 1 1 d . B 1 H16D H 0.5227 0.0282 0.8386 0.052 Uiso 1 1 calc R B 1 H16E H 0.487 0.0727 0.8796 0.052 Uiso 1 1 calc R B 1 H16F H 0.5209 0.1014 0.8215 0.052 Uiso 1 1 calc R B 1 C17B C 0.3792(9) 0.0039(10) 0.8255(13) 0.035(5) Uiso 1 1 d . B 1 H17D H 0.3933 0.0329 0.8735 0.053 Uiso 1 1 calc R B 1 H17E H 0.399 -0.036 0.8416 0.053 Uiso 1 1 calc R B 1 H17F H 0.3375 -0.0021 0.8113 0.053 Uiso 1 1 calc R B 1 C18B C 0.2966(8) -0.0071(9) 0.6347(12) 0.033(5) Uiso 1 1 d . B 1 H18D H 0.276 0.001 0.5739 0.049 Uiso 1 1 calc R B 1 H18E H 0.274 0.0093 0.6685 0.049 Uiso 1 1 calc R B 1 H18F H 0.3019 -0.0519 0.6442 0.049 Uiso 1 1 calc R B 1 C19B C 0.3647(9) 0.0462(10) 0.5111(13) 0.040(5) Uiso 1 1 d . B 1 H19D H 0.3237 0.035 0.487 0.06 Uiso 1 1 calc R B 1 H19E H 0.3878 0.016 0.4926 0.06 Uiso 1 1 calc R B 1 H19F H 0.3704 0.0877 0.4911 0.06 Uiso 1 1 calc R B 1 C20B C 0.4892(10) 0.0894(11) 0.6323(15) 0.048(6) Uiso 1 1 d . B 1 H20D H 0.5121 0.0539 0.6252 0.072 Uiso 1 1 calc R B 1 H20E H 0.5143 0.1182 0.6743 0.072 Uiso 1 1 calc R B 1 H20F H 0.4723 0.1107 0.5773 0.072 Uiso 1 1 calc R B 1 C21B C 0.1444(9) 0.2287(9) 0.7394(12) 0.026(4) Uiso 1 1 d . B 1 C22B C 0.1381(8) 0.2934(8) 0.7142(11) 0.024(4) Uiso 1 1 d . B 1 C23B C 0.1198(8) 0.2936(9) 0.6247(12) 0.027(4) Uiso 1 1 d . B 1 C24B C 0.1154(9) 0.2331(9) 0.5935(13) 0.027(4) Uiso 1 1 d . B 1 C25B C 0.1295(8) 0.1922(9) 0.6638(12) 0.027(4) Uiso 1 1 d . B 1 C26B C 0.1602(10) 0.2092(11) 0.8320(13) 0.043(6) Uiso 1 1 d . B 1 H26D H 0.171 0.1653 0.8377 0.065 Uiso 1 1 calc R B 1 H26E H 0.1269 0.2155 0.8508 0.065 Uiso 1 1 calc R B 1 H26F H 0.1927 0.2342 0.8675 0.065 Uiso 1 1 calc R B 1 C27B C 0.1425(9) 0.3456(9) 0.7739(13) 0.035(5) Uiso 1 1 d . B 1 H27D H 0.1039 0.3562 0.7745 0.052 Uiso 1 1 calc R B 1 H27E H 0.1592 0.3818 0.7551 0.052 Uiso 1 1 calc R B 1 H27F H 0.1673 0.3336 0.8315 0.052 Uiso 1 1 calc R B 1 C28B C 0.0986(9) 0.3493(10) 0.5668(13) 0.039(5) Uiso 1 1 d . B 1 H28D H 0.0569 0.3542 0.5538 0.058 Uiso 1 1 calc R B 1 H28E H 0.1066 0.343 0.5135 0.058 Uiso 1 1 calc R B 1 H28F H 0.1186 0.3867 0.5956 0.058 Uiso 1 1 calc R B 1 C29B C 0.0863(10) 0.2138(11) 0.4993(14) 0.046(6) Uiso 1 1 d . B 1 H29D H 0.0443 0.2177 0.4834 0.069 Uiso 1 1 calc R B 1 H29E H 0.0962 0.1707 0.4919 0.069 Uiso 1 1 calc R B 1 H29F H 0.0999 0.2408 0.4626 0.069 Uiso 1 1 calc R B 1 C30B C 0.1263(9) 0.1213(9) 0.6630(13) 0.036(5) Uiso 1 1 d . B 1 H30D H 0.1534 0.105 0.7167 0.054 Uiso 1 1 calc R B 1 H30E H 0.1364 0.1052 0.6148 0.054 Uiso 1 1 calc R B 1 H30F H 0.0869 0.1083 0.657 0.054 Uiso 1 1 calc R B 1 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 0.0181(4) 0.0170(5) 0.0238(4) -0.0004(3) 0.0056(3) 0.0005(3) U2 0.0174(4) 0.0177(5) 0.0248(4) -0.0006(3) 0.0054(3) 0.0005(3) U3 0.0166(5) 0.0184(4) 0.0230(4) 0.0006(3) 0.0070(4) -0.0002(2) U1B 0.0182(4) 0.0185(5) 0.0251(4) 0.0010(3) 0.0071(3) -0.0014(3) U2B 0.0194(4) 0.0177(5) 0.0272(4) 0.0002(3) 0.0084(3) -0.0004(3) U3B 0.0151(4) 0.0189(4) 0.0220(4) 0.0002(3) 0.0055(4) -0.0005(2) I1 0.0386(8) 0.0304(8) 0.0232(7) -0.0012(6) 0.0055(6) 0.0013(6) I2 0.0267(8) 0.0315(8) 0.0473(9) -0.0009(7) 0.0203(7) 0.0000(6) I3 0.0286(7) 0.0296(7) 0.0272(7) -0.0066(6) 0.0104(6) 0.0017(5) I4 0.0243(7) 0.0347(7) 0.0330(7) 0.0110(6) 0.0134(6) 0.0004(5) I5 0.0295(7) 0.0305(7) 0.0376(7) -0.0069(6) 0.0190(6) 0.0009(5) I6 0.0316(8) 0.0375(8) 0.0245(7) 0.0073(6) 0.0061(6) -0.0084(6) I1B 0.0252(8) 0.0324(8) 0.0330(8) 0.0021(6) -0.0013(6) -0.0012(5) I2B 0.0404(9) 0.0323(8) 0.0369(8) -0.0015(6) 0.0232(7) -0.0011(6) I3B 0.0273(7) 0.0283(7) 0.0315(7) 0.0085(6) 0.0128(6) 0.0024(5) I4B 0.0263(7) 0.0314(7) 0.0274(7) -0.0074(6) 0.0051(6) -0.0014(5) I5B 0.0271(8) 0.0304(7) 0.0302(7) 0.0103(6) 0.0026(6) -0.0008(5) I6B 0.0330(8) 0.0344(8) 0.0264(7) -0.0100(6) 0.0120(6) -0.0065(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.234(12) . ? U1 C1 2.69(2) . ? U1 C2 2.715(18) . ? U1 C5 2.718(19) . ? U1 C3 2.748(18) . ? U1 C4 2.791(18) . ? U1 I2 3.1772(15) . ? U1 I6 3.1979(15) . ? U1 I1 3.2143(15) . ? U1 I5 3.2260(16) . ? U1 U3 3.8395(11) . ? U2 O1 2.228(12) . ? U2 C13 2.705(18) . ? U2 C14 2.721(18) . ? U2 C12 2.73(2) . ? U2 C11 2.746(18) . ? U2 C15 2.76(2) . ? U2 I1 3.1794(15) . ? U2 I4 3.1821(16) . ? U2 I3 3.1904(15) . ? U2 I2 3.2576(15) . ? U2 U3 3.8240(11) . ? U3 O1 2.192(13) . ? U3 C21 2.708(19) . ? U3 C22 2.717(19) . ? U3 C25 2.727(17) . ? U3 C24 2.75(2) . ? U3 C23 2.763(18) . ? U3 I5 3.1539(15) . ? U3 I4 3.1744(15) . ? U3 I6 3.1809(15) . ? U3 I3 3.1826(15) . ? U1B O1B 2.192(13) . ? U1B C4B 2.70(2) . ? U1B C5B 2.73(2) . ? U1B C3B 2.74(2) . ? U1B C1B 2.748(18) . ? U1B C2B 2.761(19) . ? U1B I2B 3.1698(16) . ? U1B I5B 3.1849(16) . ? U1B I6B 3.2112(15) . ? U1B I1B 3.2238(16) . ? U1B U3B 3.8095(11) . ? U2B O1B 2.268(13) . ? U2B C14B 2.679(19) . ? U2B C15B 2.72(2) . ? U2B C13B 2.725(19) . ? U2B C11B 2.760(19) . ? U2B C12B 2.78(2) . ? U2B I3B 3.1652(15) . ? U2B I1B 3.2040(16) . ? U2B I2B 3.2377(15) . ? U2B I4B 3.2398(16) . ? U2B U3B 3.8538(11) . ? U3B O1B 2.200(15) . ? U3B C24B 2.70(2) . ? U3B C25B 2.701(19) . ? U3B C21B 2.713(19) . ? U3B C23B 2.739(19) . ? U3B C22B 2.752(18) . ? U3B I5B 3.1654(14) . ? U3B I6B 3.1666(15) . ? U3B I4B 3.1714(14) . ? U3B I3B 3.1806(14) . ? C1 C5 1.40(3) . ? C1 C2 1.46(3) . ? C1 C6 1.49(3) . ? C2 C3 1.41(3) . ? C2 C7 1.53(3) . ? C3 C4 1.45(3) . ? C3 C8 1.50(3) . ? C4 C5 1.42(3) . ? C4 C9 1.45(3) . ? C5 C10 1.56(3) . ? C11 C12 1.35(3) . ? C11 C15 1.49(3) . ? C11 C16 1.54(3) . ? C12 C13 1.40(3) . ? C12 C17 1.52(3) . ? C13 C14 1.43(3) . ? C13 C18 1.50(3) . ? C14 C15 1.44(3) . ? C14 C19 1.51(3) . ? C15 C20 1.47(3) . ? C21 C22 1.38(3) . ? C21 C25 1.43(3) . ? C21 C26 1.51(3) . ? C22 C23 1.43(3) . ? C22 C27 1.54(3) . ? C23 C24 1.41(3) . ? C23 C28 1.51(3) . ? C24 C25 1.44(3) . ? C24 C29 1.59(3) . ? C25 C30 1.47(3) . ? C1B C2B 1.43(3) . ? C1B C5B 1.44(3) . ? C1B C6B 1.49(3) . ? C2B C3B 1.38(3) . ? C2B C7B 1.50(3) . ? C3B C4B 1.42(3) . ? C3B C8B 1.54(3) . ? C4B C5B 1.38(3) . ? C4B C9B 1.55(3) . ? C5B C10B 1.51(3) . ? C11B C12B 1.40(3) . ? C11B C15B 1.41(3) . ? C11B C16B 1.56(3) . ? C12B C13B 1.40(3) . ? C12B C17B 1.54(3) . ? C13B C14B 1.37(3) . ? C13B C18B 1.52(3) . ? C14B C15B 1.45(3) . ? C14B C19B 1.55(3) . ? C15B C20B 1.53(3) . ? C21B C25B 1.42(3) . ? C21B C22B 1.45(3) . ? C21B C26B 1.51(3) . ? C22B C23B 1.40(3) . ? C22B C27B 1.48(3) . ? C23B C24B 1.39(3) . ? C23B C28B 1.52(3) . ? C24B C25B 1.41(3) . ? C24B C29B 1.54(3) . ? C25B C30B 1.53(3) . ? 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 C1 151.4(5) . . ? O1 U1 C2 150.9(5) . . ? C1 U1 C2 31.4(6) . . ? O1 U1 C5 156.0(5) . . ? C1 U1 C5 30.0(6) . . ? C2 U1 C5 49.5(6) . . ? O1 U1 C3 153.5(5) . . ? C1 U1 C3 50.6(6) . . ? C2 U1 C3 29.8(5) . . ? C5 U1 C3 49.2(6) . . ? O1 U1 C4 156.2(5) . . ? C1 U1 C4 50.4(6) . . ? C2 U1 C4 49.8(5) . . ? C5 U1 C4 29.8(6) . . ? C3 U1 C4 30.3(5) . . ? O1 U1 I2 74.2(3) . . ? C1 U1 I2 124.4(4) . . ? C2 U1 I2 131.8(4) . . ? C5 U1 I2 94.5(4) . . ? C3 U1 I2 104.1(4) . . ? C4 U1 I2 82.7(4) . . ? O1 U1 I6 73.2(3) . . ? C1 U1 I6 122.5(4) . . ? C2 U1 I6 91.1(4) . . ? C5 U1 I6 129.2(4) . . ? C3 U1 I6 80.4(4) . . ? C4 U1 I6 102.2(4) . . ? I2 U1 I6 91.66(4) . . ? O1 U1 I1 72.9(3) . . ? C1 U1 I1 87.9(4) . . ? C2 U1 I1 118.4(4) . . ? C5 U1 I1 84.5(4) . . ? C3 U1 I1 133.5(4) . . ? C4 U1 I1 109.5(4) . . ? I2 U1 I1 80.92(4) . . ? I6 U1 I1 146.11(4) . . ? O1 U1 I5 71.8(3) . . ? C1 U1 I5 86.9(4) . . ? C2 U1 I5 81.5(4) . . ? C5 U1 I5 116.5(4) . . ? C3 U1 I5 106.7(4) . . ? C4 U1 I5 131.2(4) . . ? I2 U1 I5 146.02(4) . . ? I6 U1 I5 79.81(4) . . ? I1 U1 I5 88.07(4) . . ? O1 U1 U3 29.5(3) . . ? C1 U1 U3 138.7(4) . . ? C2 U1 U3 122.2(4) . . ? C5 U1 U3 168.6(4) . . ? C3 U1 U3 129.1(4) . . ? C4 U1 U3 155.0(4) . . ? I2 U1 U3 96.71(3) . . ? I6 U1 U3 52.79(3) . . ? I1 U1 U3 95.03(3) . . ? I5 U1 U3 52.15(3) . . ? O1 U2 C13 155.4(5) . . ? O1 U2 C14 152.2(5) . . ? C13 U2 C14 30.7(5) . . ? O1 U2 C12 155.3(5) . . ? C13 U2 C12 29.8(6) . . ? C14 U2 C12 50.5(6) . . ? O1 U2 C11 154.0(5) . . ? C13 U2 C11 48.4(6) . . ? C14 U2 C11 50.3(6) . . ? C12 U2 C11 28.6(6) . . ? O1 U2 C15 151.6(5) . . ? C13 U2 C15 49.8(6) . . ? C14 U2 C15 30.5(6) . . ? C12 U2 C15 50.1(6) . . ? C11 U2 C15 31.3(6) . . ? O1 U2 I1 73.7(3) . . ? C13 U2 I1 92.9(4) . . ? C14 U2 I1 123.5(4) . . ? C12 U2 I1 82.6(4) . . ? C11 U2 I1 103.4(4) . . ? C15 U2 I1 132.4(4) . . ? O1 U2 I4 73.7(3) . . ? C13 U2 I4 128.0(4) . . ? C14 U2 I4 123.2(4) . . ? C12 U2 I4 100.0(4) . . ? C11 U2 I4 80.5(4) . . ? C15 U2 I4 92.7(4) . . ? I1 U2 I4 90.41(4) . . ? O1 U2 I3 72.1(3) . . ? C13 U2 I3 118.2(4) . . ? C14 U2 I3 87.9(4) . . ? C12 U2 I3 131.5(4) . . ? C11 U2 I3 107.8(4) . . ? C15 U2 I3 81.4(4) . . ? I1 U2 I3 145.81(4) . . ? I4 U2 I3 81.47(4) . . ? O1 U2 I2 72.6(3) . . ? C13 U2 I2 85.0(4) . . ? C14 U2 I2 88.2(4) . . ? C12 U2 I2 110.6(4) . . ? C11 U2 I2 133.1(4) . . ? C15 U2 I2 117.5(4) . . ? I1 U2 I2 80.22(4) . . ? I4 U2 I2 146.32(4) . . ? I3 U2 I2 88.33(4) . . ? O1 U2 U3 29.8(3) . . ? C13 U2 U3 171.1(4) . . ? C14 U2 U3 140.4(4) . . ? C12 U2 U3 152.9(4) . . ? C11 U2 U3 129.5(4) . . ? C15 U2 U3 123.0(4) . . ? I1 U2 U3 95.91(3) . . ? I4 U2 U3 52.93(3) . . ? I3 U2 U3 53.03(3) . . ? I2 U2 U3 95.64(3) . . ? O1 U3 C21 152.5(5) . . ? O1 U3 C22 155.6(5) . . ? C21 U3 C22 29.5(6) . . ? O1 U3 C25 151.3(5) . . ? C21 U3 C25 30.5(5) . . ? C22 U3 C25 49.4(6) . . ? O1 U3 C24 153.8(5) . . ? C21 U3 C24 49.8(6) . . ? C22 U3 C24 49.0(6) . . ? C25 U3 C24 30.4(6) . . ? O1 U3 C23 155.8(5) . . ? C21 U3 C23 49.7(6) . . ? C22 U3 C23 30.1(6) . . ? C25 U3 C23 49.9(5) . . ? C24 U3 C23 29.6(6) . . ? O1 U3 I5 73.8(3) . . ? C21 U3 I5 130.8(4) . . ? C22 U3 I5 102.8(4) . . ? C25 U3 I5 125.2(4) . . ? C24 U3 I5 94.8(4) . . ? C23 U3 I5 82.2(4) . . ? O1 U3 I4 74.3(3) . . ? C21 U3 I4 113.1(4) . . ? C22 U3 I4 130.0(4) . . ? C25 U3 I4 83.9(4) . . ? C24 U3 I4 82.2(4) . . ? C23 U3 I4 108.7(4) . . ? I5 U3 I4 89.34(4) . . ? O1 U3 I6 74.1(3) . . ? C21 U3 I6 95.6(4) . . ? C22 U3 I6 81.6(4) . . ? C25 U3 I6 126.0(4) . . ? C24 U3 I6 128.4(4) . . ? C23 U3 I6 99.9(4) . . ? I5 U3 I6 81.16(4) . . ? I4 U3 I6 148.37(5) . . ? O1 U3 I3 72.7(3) . . ? C21 U3 I3 82.0(4) . . ? C22 U3 I3 107.7(4) . . ? C25 U3 I3 86.1(4) . . ? C24 U3 I3 115.7(4) . . ? C23 U3 I3 131.3(4) . . ? I5 U3 I3 146.46(5) . . ? I4 U3 I3 81.71(4) . . ? I6 U3 I3 89.71(4) . . ? O1 U3 U2 30.4(3) . . ? C21 U3 U2 132.9(4) . . ? C22 U3 U2 160.9(4) . . ? C25 U3 U2 120.9(4) . . ? C24 U3 U2 133.7(4) . . ? C23 U3 U2 161.8(4) . . ? I5 U3 U2 95.91(4) . . ? I4 U3 U2 53.11(3) . . ? I6 U3 U2 97.72(3) . . ? I3 U3 U2 53.22(3) . . ? O1B U1B C4B 155.5(6) . . ? O1B U1B C5B 155.5(6) . . ? C4B U1B C5B 29.5(6) . . ? O1B U1B C3B 152.8(6) . . ? C4B U1B C3B 30.3(6) . . ? C5B U1B C3B 49.6(6) . . ? O1B U1B C1B 153.8(5) . . ? C4B U1B C1B 49.0(6) . . ? C5B U1B C1B 30.4(5) . . ? C3B U1B C1B 49.1(6) . . ? O1B U1B C2B 152.1(6) . . ? C4B U1B C2B 48.9(6) . . ? C5B U1B C2B 49.8(6) . . ? C3B U1B C2B 29.1(6) . . ? C1B U1B C2B 30.0(5) . . ? O1B U1B I2B 73.2(4) . . ? C4B U1B I2B 121.6(4) . . ? C5B U1B I2B 92.2(4) . . ? C3B U1B I2B 130.9(4) . . ? C1B U1B I2B 82.1(4) . . ? C2B U1B I2B 104.6(4) . . ? O1B U1B I5B 73.5(4) . . ? C4B U1B I5B 120.8(4) . . ? C5B U1B I5B 128.1(4) . . ? C3B U1B I5B 90.6(4) . . ? C1B U1B I5B 100.0(4) . . ? C2B U1B I5B 79.0(4) . . ? I2B U1B I5B 93.57(4) . . ? O1B U1B I6B 73.4(4) . . ? C4B U1B I6B 89.2(4) . . ? C5B U1B I6B 118.1(4) . . ? C3B U1B I6B 82.3(4) . . ? C1B U1B I6B 131.3(4) . . ? C2B U1B I6B 106.1(4) . . ? I2B U1B I6B 146.45(4) . . ? I5B U1B I6B 79.25(4) . . ? O1B U1B I1B 74.7(4) . . ? C4B U1B I1B 88.1(4) . . ? C5B U1B I1B 83.8(4) . . ? C3B U1B I1B 117.2(4) . . ? C1B U1B I1B 110.1(4) . . ? C2B U1B I1B 133.0(4) . . ? I2B U1B I1B 80.51(4) . . ? I5B U1B I1B 147.97(4) . . ? I6B U1B I1B 88.44(4) . . ? O1B U1B U3B 29.9(4) . . ? C4B U1B U3B 141.4(4) . . ? C5B U1B U3B 170.8(4) . . ? C3B U1B U3B 123.4(4) . . ? C1B U1B U3B 152.9(4) . . ? C2B U1B U3B 128.3(4) . . ? I2B U1B U3B 96.82(3) . . ? I5B U1B U3B 52.90(3) . . ? I6B U1B U3B 52.79(3) . . ? I1B U1B U3B 96.27(3) . . ? O1B U2B C14B 151.1(6) . . ? O1B U2B C15B 156.5(6) . . ? C14B U2B C15B 31.2(6) . . ? O1B U2B C13B 149.6(6) . . ? C14B U2B C13B 29.4(6) . . ? C15B U2B C13B 49.7(6) . . ? O1B U2B C11B 158.3(5) . . ? C14B U2B C11B 49.6(6) . . ? C15B U2B C11B 29.7(6) . . ? C13B U2B C11B 49.0(6) . . ? O1B U2B C12B 153.8(6) . . ? C14B U2B C12B 48.7(6) . . ? C15B U2B C12B 48.9(6) . . ? C13B U2B C12B 29.5(6) . . ? C11B U2B C12B 29.3(6) . . ? O1B U2B I3B 73.6(4) . . ? C14B U2B I3B 120.1(4) . . ? C15B U2B I3B 128.7(4) . . ? C13B U2B I3B 90.8(4) . . ? C11B U2B I3B 101.3(4) . . ? C12B U2B I3B 80.2(4) . . ? O1B U2B I1B 74.3(4) . . ? C14B U2B I1B 127.7(4) . . ? C15B U2B I1B 96.6(4) . . ? C13B U2B I1B 132.4(4) . . ? C11B U2B I1B 84.6(4) . . ? C12B U2B I1B 104.3(4) . . ? I3B U2B I1B 88.53(4) . . ? O1B U2B I2B 70.9(4) . . ? C14B U2B I2B 93.0(4) . . ? C15B U2B I2B 86.3(4) . . ? C13B U2B I2B 121.7(4) . . ? C11B U2B I2B 110.8(4) . . ? C12B U2B I2B 135.1(4) . . ? I3B U2B I2B 144.43(4) . . ? I1B U2B I2B 79.79(4) . . ? O1B U2B I4B 70.3(4) . . ? C14B U2B I4B 85.5(4) . . ? C15B U2B I4B 115.6(4) . . ? C13B U2B I4B 82.2(4) . . ? C11B U2B I4B 130.7(4) . . ? C12B U2B I4B 108.0(4) . . ? I3B U2B I4B 82.83(4) . . ? I1B U2B I4B 144.56(4) . . ? I2B U2B I4B 87.52(4) . . ? O1B U2B U3B 29.9(4) . . ? C14B U2B U3B 136.5(4) . . ? C15B U2B U3B 167.6(4) . . ? C13B U2B U3B 120.8(4) . . ? C11B U2B U3B 154.0(4) . . ? C12B U2B U3B 128.3(4) . . ? I3B U2B U3B 52.79(3) . . ? I1B U2B U3B 95.74(3) . . ? I2B U2B U3B 94.81(3) . . ? I4B U2B U3B 52.24(3) . . ? O1B U3B C24B 151.6(6) . . ? O1B U3B C25B 151.4(5) . . ? C24B U3B C25B 30.3(6) . . ? O1B U3B C21B 154.2(6) . . ? C24B U3B C21B 50.0(6) . . ? C25B U3B C21B 30.5(6) . . ? O1B U3B C23B 155.1(5) . . ? C24B U3B C23B 29.7(6) . . ? C25B U3B C23B 49.3(6) . . ? C21B U3B C23B 49.3(6) . . ? O1B U3B C22B 156.1(5) . . ? C24B U3B C22B 49.8(6) . . ? C25B U3B C22B 50.3(5) . . ? C21B U3B C22B 30.7(6) . . ? C23B U3B C22B 29.5(5) . . ? O1B U3B I5B 73.8(3) . . ? C24B U3B I5B 94.8(4) . . ? C25B U3B I5B 125.0(4) . . ? C21B U3B I5B 128.9(4) . . ? C23B U3B I5B 81.3(4) . . ? C22B U3B I5B 99.4(4) . . ? O1B U3B I6B 74.3(4) . . ? C24B U3B I6B 130.4(4) . . ? C25B U3B I6B 126.3(4) . . ? C21B U3B I6B 95.9(4) . . ? C23B U3B I6B 101.8(4) . . ? C22B U3B I6B 82.1(4) . . ? I5B U3B I6B 80.22(4) . . ? O1B U3B I4B 72.5(4) . . ? C24B U3B I4B 82.0(4) . . ? C25B U3B I4B 84.9(4) . . ? C21B U3B I4B 114.1(4) . . ? C23B U3B I4B 108.6(4) . . ? C22B U3B I4B 131.2(4) . . ? I5B U3B I4B 91.00(4) . . ? I6B U3B I4B 146.73(5) . . ? O1B U3B I3B 74.0(3) . . ? C24B U3B I3B 116.0(4) . . ? C25B U3B I3B 86.5(4) . . ? C21B U3B I3B 81.8(4) . . ? C23B U3B I3B 130.7(4) . . ? C22B U3B I3B 108.2(4) . . ? I5B U3B I3B 147.52(5) . . ? I6B U3B I3B 86.83(4) . . ? I4B U3B I3B 83.68(4) . . ? O1B U3B U1B 29.8(3) . . ? C24B U3B U1B 148.1(4) . . ? C25B U3B U1B 178.3(4) . . ? C21B U3B U1B 149.8(4) . . ? C23B U3B U1B 129.2(4) . . ? C22B U3B U1B 128.9(4) . . ? I5B U3B U1B 53.37(3) . . ? I6B U3B U1B 53.86(3) . . ? I4B U3B U1B 95.30(3) . . ? I3B U3B U1B 95.11(3) . . ? U2 I1 U1 74.31(3) . . ? U1 I2 U2 73.74(3) . . ? U3 I3 U2 73.74(3) . . ? U3 I4 U2 73.97(4) . . ? U3 I5 U1 73.99(3) . . ? U3 I6 U1 74.01(3) . . ? U3 O1 U2 119.8(5) . . ? U3 O1 U1 120.3(5) . . ? U2 O1 U1 119.9(6) . . ? C5 C1 C2 105.3(17) . . ? C5 C1 C6 130(2) . . ? C2 C1 C6 124.6(19) . . ? C5 C1 U1 76.0(11) . . ? C2 C1 U1 75.2(11) . . ? C6 C1 U1 117.6(14) . . ? C3 C2 C1 108.4(16) . . ? C3 C2 C7 122.8(16) . . ? C1 C2 C7 128.6(16) . . ? C3 C2 U1 76.4(10) . . ? C1 C2 U1 73.5(10) . . ? C7 C2 U1 119.6(12) . . ? C2 C3 C4 108.9(16) . . ? C2 C3 C8 125.7(16) . . ? C4 C3 C8 124.1(17) . . ? C2 C3 U1 73.8(10) . . ? C4 C3 U1 76.5(10) . . ? C8 C3 U1 126.7(13) . . ? C5 C4 C3 105.3(16) . . ? C5 C4 C9 125.9(18) . . ? C3 C4 C9 128.3(18) . . ? C5 C4 U1 72.3(11) . . ? C3 C4 U1 73.2(10) . . ? C9 C4 U1 125.6(14) . . ? C1 C5 C4 112.1(17) . . ? C1 C5 C10 122.8(18) . . ? C4 C5 C10 125.0(17) . . ? C1 C5 U1 74.0(11) . . ? C4 C5 U1 78.0(11) . . ? C10 C5 U1 118.8(13) . . ? C12 C11 C15 109.9(17) . . ? C12 C11 C16 128.0(18) . . ? C15 C11 C16 121.4(17) . . ? C12 C11 U2 75.2(11) . . ? C15 C11 U2 74.9(11) . . ? C16 C11 U2 124.4(13) . . ? C11 C12 C13 108.4(17) . . ? C11 C12 C17 123.9(18) . . ? C13 C12 C17 127.1(18) . . ? C11 C12 U2 76.2(12) . . ? C13 C12 U2 73.9(11) . . ? C17 C12 U2 123.4(13) . . ? C12 C13 C14 110.3(16) . . ? C12 C13 C18 125.5(18) . . ? C14 C13 C18 124.0(18) . . ? C12 C13 U2 76.2(11) . . ? C14 C13 U2 75.3(11) . . ? C18 C13 U2 119.4(13) . . ? C13 C14 C15 106.3(16) . . ? C13 C14 C19 126.6(17) . . ? C15 C14 C19 127.0(17) . . ? C13 C14 U2 74.0(10) . . ? C15 C14 U2 76.3(11) . . ? C19 C14 U2 117.5(12) . . ? C14 C15 C20 128.5(19) . . ? C14 C15 C11 105.1(17) . . ? C20 C15 C11 125.7(19) . . ? C14 C15 U2 73.2(11) . . ? C20 C15 U2 124.8(14) . . ? C11 C15 U2 73.8(11) . . ? C22 C21 C25 108.1(16) . . ? C22 C21 C26 124.8(18) . . ? C25 C21 C26 126.8(17) . . ? C22 C21 U3 75.6(10) . . ? C25 C21 U3 75.5(10) . . ? C26 C21 U3 120.3(13) . . ? C21 C22 C23 110.2(17) . . ? C21 C22 C27 125.2(17) . . ? C23 C22 C27 123.5(17) . . ? C21 C22 U3 74.9(10) . . ? C23 C22 U3 76.7(11) . . ? C27 C22 U3 124.9(12) . . ? C24 C23 C22 106.2(17) . . ? C24 C23 C28 124.3(18) . . ? C22 C23 C28 128.7(18) . . ? C24 C23 U3 74.6(11) . . ? C22 C23 U3 73.1(10) . . ? C28 C23 U3 125.5(13) . . ? C23 C24 C25 109.0(17) . . ? C23 C24 C29 126.0(19) . . ? C25 C24 C29 124.7(17) . . ? C23 C24 U3 75.8(11) . . ? C25 C24 U3 74.0(11) . . ? C29 C24 U3 121.5(13) . . ? C21 C25 C24 106.4(15) . . ? C21 C25 C30 128.4(17) . . ? C24 C25 C30 125.0(18) . . ? C21 C25 U3 74.0(10) . . ? C24 C25 U3 75.6(11) . . ? C30 C25 U3 119.1(13) . . ? U2B I1B U1B 73.98(4) . . ? U1B I2B U2B 74.24(4) . . ? U2B I3B U3B 74.79(3) . . ? U3B I4B U2B 73.89(3) . . ? U3B I5B U1B 73.72(3) . . ? U3B I6B U1B 73.35(3) . . ? U1B O1B U3B 120.3(6) . . ? U1B O1B U2B 120.2(7) . . ? U3B O1B U2B 119.2(6) . . ? C2B C1B C5B 107.5(17) . . ? C2B C1B C6B 126.6(18) . . ? C5B C1B C6B 125.0(18) . . ? C2B C1B U1B 75.5(11) . . ? C5B C1B U1B 74.1(11) . . ? C6B C1B U1B 124.9(14) . . ? C3B C2B C1B 108.3(18) . . ? C3B C2B C7B 129.3(19) . . ? C1B C2B C7B 121.5(17) . . ? C3B C2B U1B 74.5(12) . . ? C1B C2B U1B 74.5(10) . . ? C7B C2B U1B 125.6(13) . . ? C2B C3B C4B 107.6(18) . . ? C2B C3B C8B 125.8(19) . . ? C4B C3B C8B 126.3(18) . . ? C2B C3B U1B 76.4(12) . . ? C4B C3B U1B 73.5(11) . . ? C8B C3B U1B 121.7(14) . . ? C5B C4B C3B 110.0(18) . . ? C5B C4B C9B 126.3(19) . . ? C3B C4B C9B 123.7(19) . . ? C5B C4B U1B 76.4(12) . . ? C3B C4B U1B 76.3(11) . . ? C9B C4B U1B 116.7(14) . . ? C4B C5B C1B 106.6(17) . . ? C4B C5B C10B 128.2(18) . . ? C1B C5B C10B 125.0(18) . . ? C4B C5B U1B 74.2(12) . . ? C1B C5B U1B 75.5(11) . . ? C10B C5B U1B 120.3(13) . . ? C12B C11B C15B 108.5(17) . . ? C12B C11B C16B 125.4(17) . . ? C15B C11B C16B 125.6(18) . . ? C12B C11B U2B 76.2(11) . . ? C15B C11B U2B 73.6(11) . . ? C16B C11B U2B 123.0(12) . . ? C11B C12B C13B 108.3(18) . . ? C11B C12B C17B 125.6(18) . . ? C13B C12B C17B 125.6(18) . . ? C11B C12B U2B 74.5(11) . . ? C13B C12B U2B 73.0(11) . . ? C17B C12B U2B 124.7(13) . . ? C14B C13B C12B 108.7(18) . . ? C14B C13B C18B 127.4(18) . . ? C12B C13B C18B 123.6(18) . . ? C14B C13B U2B 73.5(11) . . ? C12B C13B U2B 77.5(11) . . ? C18B C13B U2B 120.4(13) . . ? C13B C14B C15B 108.4(17) . . ? C13B C14B C19B 129.2(18) . . ? C15B C14B C19B 122.3(17) . . ? C13B C14B U2B 77.2(12) . . ? C15B C14B U2B 76.0(11) . . ? C19B C14B U2B 116.7(13) . . ? C11B C15B C14B 106.1(18) . . ? C11B C15B C20B 127.7(19) . . ? C14B C15B C20B 126.1(18) . . ? C11B C15B U2B 76.7(12) . . ? C14B C15B U2B 72.8(11) . . ? C20B C15B U2B 119.2(14) . . ? C25B C21B C22B 107.8(16) . . ? C25B C21B C26B 130.2(18) . . ? C22B C21B C26B 121.9(18) . . ? C25B C21B U3B 74.3(11) . . ? C22B C21B U3B 76.1(10) . . ? C26B C21B U3B 119.1(14) . . ? C23B C22B C21B 106.0(16) . . ? C23B C22B C27B 129.3(17) . . ? C21B C22B C27B 124.1(17) . . ? C23B C22B U3B 74.7(10) . . ? C21B C22B U3B 73.2(10) . . ? C27B C22B U3B 123.9(13) . . ? C24B C23B C22B 110.4(17) . . ? C24B C23B C28B 122.5(18) . . ? C22B C23B C28B 126.5(17) . . ? C24B C23B U3B 73.5(11) . . ? C22B C23B U3B 75.7(11) . . ? C28B C23B U3B 124.5(13) . . ? C23B C24B C25B 108.0(17) . . ? C23B C24B C29B 125.6(19) . . ? C25B C24B C29B 124.9(18) . . ? C23B C24B U3B 76.8(11) . . ? C25B C24B U3B 75.0(11) . . ? C29B C24B U3B 125.5(13) . . ? C24B C25B C21B 107.8(16) . . ? C24B C25B C30B 128.3(18) . . ? C21B C25B C30B 123.8(17) . . ? C24B C25B U3B 74.8(11) . . ? C21B C25B U3B 75.3(11) . . ? C30B C25B U3B 119.1(12) . . ? #===END