data_apr206 _audit_creation_date 2006-04-04T10:50:18-00:00 _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 _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H69 O Si2 U' _chemical_formula_sum 'C39 H69 O Si2 U' _chemical_formula_weight 848.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8533(2) _cell_length_b 14.8390(2) _cell_length_c 22.5090(3) _cell_angle_alpha 90 _cell_angle_beta 90.652(1) _cell_angle_gamma 90 _cell_volume 3958.88(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45751 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.187 _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 0.5300 _exptl_absorpt_correction_T_max 0.6615 #----------------------------------------------------------------------------# # 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 0.340156E-1 _diffrn_orient_matrix_ub_12 0.50741E-2 _diffrn_orient_matrix_ub_13 -0.403142E-1 _diffrn_orient_matrix_ub_21 -0.556911E-1 _diffrn_orient_matrix_ub_22 -0.449051E-1 _diffrn_orient_matrix_ub_23 -0.157414E-1 _diffrn_orient_matrix_ub_31 -0.534767E-1 _diffrn_orient_matrix_ub_32 0.49992E-1 _diffrn_orient_matrix_ub_33 -0.100478E-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 0.073 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_number 58842 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 7771 _reflns_number_gt 6512 _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^)+(0.0344P)^2^+16.1434P] 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 7771 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.156 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.134 #----------------------------------------------------------------------------# # 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' 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 U U 0.540424(16) 0.652259(12) 0.236651(8) 0.02073(7) Uani 1 1 d . . . Si1 Si 0.75557(14) 0.70433(10) 0.08519(6) 0.0260(3) Uani 1 1 d . A 1 Si2 Si 0.75382(14) 0.68502(10) 0.39463(6) 0.0259(3) Uani 1 1 d . A 1 O O 0.5117(3) 0.8348(3) 0.24491(19) 0.0347(10) Uani 1 1 d . B 1 C1 C 0.7185(4) 0.6538(3) 0.1604(2) 0.0218(10) Uani 1 1 d . A 1 C2 C 0.7512(4) 0.7099(3) 0.2086(2) 0.0209(11) Uani 1 1 d . A 1 H2 H 0.7823 0.7651 0.195 0.025 Uiso 1 1 calc R A 1 C3 C 0.7501(4) 0.7062(4) 0.2712(2) 0.0225(11) Uani 1 1 d . A 1 H3 H 0.7812 0.7596 0.2879 0.027 Uiso 1 1 calc R A 1 C4 C 0.7159(4) 0.6455(3) 0.3166(2) 0.0213(11) Uani 1 1 d . A 1 C5 C 0.6699(4) 0.5570(3) 0.3118(2) 0.0240(11) Uani 1 1 d . A 1 H5 H 0.6517 0.5325 0.3495 0.029 Uiso 1 1 calc R A 1 C6 C 0.6446(4) 0.4969(4) 0.2653(2) 0.0244(11) Uani 1 1 d . A 1 H6 H 0.6202 0.4399 0.2795 0.029 Uiso 1 1 calc R A 1 C7 C 0.6465(4) 0.5001(3) 0.2028(2) 0.0239(11) Uani 1 1 d . A 1 H7 H 0.6242 0.4445 0.1854 0.029 Uiso 1 1 calc R A 1 C8 C 0.6732(5) 0.5651(4) 0.1597(2) 0.0267(12) Uani 1 1 d . A 1 H8 H 0.6569 0.5448 0.1205 0.032 Uiso 1 1 calc R A 1 C9 C 0.9130(5) 0.7264(4) 0.0820(3) 0.0365(14) Uani 1 1 d . A 1 H9 H 0.9299 0.7403 0.0396 0.044 Uiso 1 1 calc R A 1 C10 C 0.9806(7) 0.6417(5) 0.0977(4) 0.063(2) Uani 1 1 d . A 1 H10A H 0.9522 0.5908 0.0742 0.095 Uiso 1 1 calc R A 1 H10B H 0.9724 0.6284 0.1401 0.095 Uiso 1 1 calc R A 1 H10C H 1.0604 0.6517 0.0889 0.095 Uiso 1 1 calc R A 1 C11 C 0.9575(6) 0.8068(5) 0.1186(3) 0.054(2) Uani 1 1 d . A 1 H11A H 0.9148 0.8611 0.1079 0.081 Uiso 1 1 calc R A 1 H11B H 1.0375 0.8161 0.1101 0.081 Uiso 1 1 calc R A 1 H11C H 0.9484 0.7943 0.161 0.081 Uiso 1 1 calc R A 1 C12 C 0.6794(5) 0.8161(4) 0.0734(2) 0.0316(13) Uani 1 1 d . A 1 H12 H 0.7109 0.8588 0.1037 0.038 Uiso 1 1 calc R A 1 C13 C 0.7034(7) 0.8576(4) 0.0123(3) 0.0475(17) Uani 1 1 d . A 1 H13A H 0.7851 0.8603 0.0064 0.071 Uiso 1 1 calc R A 1 H13B H 0.6718 0.9185 0.0105 0.071 Uiso 1 1 calc R A 1 H13C H 0.6687 0.8203 -0.0188 0.071 Uiso 1 1 calc R A 1 C14 C 0.5519(6) 0.8123(5) 0.0835(3) 0.0423(16) Uani 1 1 d . A 1 H14A H 0.5372 0.7861 0.1226 0.063 Uiso 1 1 calc R A 1 H14B H 0.5163 0.7749 0.0526 0.063 Uiso 1 1 calc R A 1 H14C H 0.5205 0.8733 0.0816 0.063 Uiso 1 1 calc R A 1 C15 C 0.7247(6) 0.6201(4) 0.0234(2) 0.0366(15) Uani 1 1 d . A 1 H15 H 0.7479 0.56 0.0394 0.044 Uiso 1 1 calc R A 1 C16 C 0.7956(8) 0.6348(5) -0.0338(3) 0.058(2) Uani 1 1 d . A 1 H16A H 0.8756 0.6403 -0.0228 0.087 Uiso 1 1 calc R A 1 H16B H 0.7705 0.6899 -0.0539 0.087 Uiso 1 1 calc R A 1 H16C H 0.7853 0.5832 -0.0605 0.087 Uiso 1 1 calc R A 1 C17 C 0.6005(6) 0.6108(5) 0.0058(3) 0.0479(18) Uani 1 1 d . A 1 H17A H 0.5555 0.601 0.0414 0.072 Uiso 1 1 calc R A 1 H17B H 0.5912 0.5594 -0.0212 0.072 Uiso 1 1 calc R A 1 H17C H 0.5752 0.6659 -0.0142 0.072 Uiso 1 1 calc R A 1 C18 C 0.9116(5) 0.6722(4) 0.4056(3) 0.0348(14) Uani 1 1 d . A 1 H18 H 0.9297 0.6933 0.4468 0.042 Uiso 1 1 calc R A 1 C19 C 0.9805(6) 0.7306(6) 0.3632(3) 0.063(2) Uani 1 1 d . A 1 H19A H 0.956 0.7935 0.3664 0.094 Uiso 1 1 calc R A 1 H19B H 0.9689 0.7095 0.3224 0.094 Uiso 1 1 calc R A 1 H19C H 1.0608 0.7262 0.3739 0.094 Uiso 1 1 calc R A 1 C20 C 0.9486(7) 0.5733(5) 0.4020(4) 0.059(2) Uani 1 1 d . A 1 H20A H 0.9038 0.5372 0.4295 0.089 Uiso 1 1 calc R A 1 H20B H 1.0287 0.5685 0.4129 0.089 Uiso 1 1 calc R A 1 H20C H 0.9371 0.5511 0.3614 0.089 Uiso 1 1 calc R A 1 C21 C 0.7198(6) 0.8088(4) 0.4046(3) 0.0383(15) Uani 1 1 d . A 1 H21 H 0.7575 0.8416 0.3714 0.046 Uiso 1 1 calc R A 1 C22 C 0.7677(11) 0.8479(5) 0.4622(4) 0.093(4) Uani 1 1 d . A 1 H22A H 0.8484 0.834 0.4652 0.139 Uiso 1 1 calc R A 1 H22B H 0.7284 0.8213 0.496 0.139 Uiso 1 1 calc R A 1 H22C H 0.757 0.9133 0.4624 0.139 Uiso 1 1 calc R A 1 C23 C 0.5940(8) 0.8312(5) 0.3997(4) 0.069(3) Uani 1 1 d . A 1 H23A H 0.5633 0.8067 0.3625 0.104 Uiso 1 1 calc R A 1 H23B H 0.5839 0.8967 0.4002 0.104 Uiso 1 1 calc R A 1 H23C H 0.5543 0.8044 0.4334 0.104 Uiso 1 1 calc R A 1 C24 C 0.6850(6) 0.6098(4) 0.4522(3) 0.0371(14) Uani 1 1 d . A 1 H24 H 0.7037 0.5466 0.4405 0.045 Uiso 1 1 calc R A 1 C25 C 0.7322(8) 0.6215(6) 0.5152(3) 0.065(2) Uani 1 1 d . A 1 H25A H 0.8148 0.6177 0.5145 0.097 Uiso 1 1 calc R A 1 H25B H 0.7026 0.5738 0.5408 0.097 Uiso 1 1 calc R A 1 H25C H 0.7097 0.6804 0.5307 0.097 Uiso 1 1 calc R A 1 C26 C 0.5565(6) 0.6147(5) 0.4531(3) 0.0525(19) Uani 1 1 d . A 1 H26A H 0.5265 0.6068 0.4127 0.079 Uiso 1 1 calc R A 1 H26B H 0.5331 0.6736 0.4684 0.079 Uiso 1 1 calc R A 1 H26C H 0.5272 0.567 0.4788 0.079 Uiso 1 1 calc R A 1 C27 C 0.3149(5) 0.6771(4) 0.2194(3) 0.0377(15) Uani 1 1 d . B 1 H27 H 0.2963 0.7367 0.2075 0.045 Uiso 1 1 calc R B 1 C28 C 0.3231(5) 0.6458(5) 0.2787(3) 0.0416(17) Uani 1 1 d . B 1 C29 C 0.3518(5) 0.5538(5) 0.2746(3) 0.0377(15) Uani 1 1 d . B 1 C30 C 0.3630(5) 0.5302(4) 0.2151(3) 0.0344(14) Uani 1 1 d . B 1 C31 C 0.3386(5) 0.6060(4) 0.1814(3) 0.0356(14) Uani 1 1 d . B 1 C32 C 0.3012(7) 0.6944(7) 0.3357(4) 0.076(3) Uani 1 1 d . B 1 H32A H 0.2746 0.6515 0.3655 0.114 Uiso 1 1 calc R B 1 H32B H 0.2435 0.7408 0.329 0.114 Uiso 1 1 calc R B 1 H32C H 0.3711 0.7229 0.3499 0.114 Uiso 1 1 calc R B 1 C33 C 0.3624(6) 0.4892(6) 0.3268(3) 0.062(2) Uani 1 1 d . B 1 H33A H 0.2897 0.4594 0.3332 0.093 Uiso 1 1 calc R B 1 H33B H 0.3843 0.5227 0.3626 0.093 Uiso 1 1 calc R B 1 H33C H 0.4199 0.4437 0.3182 0.093 Uiso 1 1 calc R B 1 C34 C 0.3781(6) 0.4372(5) 0.1902(4) 0.062(2) Uani 1 1 d . B 1 H34A H 0.4186 0.3997 0.2193 0.093 Uiso 1 1 calc R B 1 H34B H 0.4217 0.4406 0.1535 0.093 Uiso 1 1 calc R B 1 H34C H 0.3041 0.4106 0.1816 0.093 Uiso 1 1 calc R B 1 C35 C 0.3272(7) 0.6116(6) 0.1143(3) 0.063(2) Uani 1 1 d . B 1 H35A H 0.2571 0.582 0.1015 0.095 Uiso 1 1 calc R B 1 H35B H 0.3915 0.5814 0.0959 0.095 Uiso 1 1 calc R B 1 H35C H 0.3256 0.675 0.1021 0.095 Uiso 1 1 calc R B 1 C36 C 0.6007(6) 0.9001(4) 0.2394(3) 0.0378(14) Uani 1 1 d . B 1 H36A H 0.62 0.9083 0.1971 0.045 Uiso 1 1 calc R B 1 H36B H 0.669 0.8793 0.2611 0.045 Uiso 1 1 calc R B 1 C37 C 0.5598(6) 0.9873(4) 0.2651(3) 0.0445(16) Uani 1 1 d . B 1 H37A H 0.5902 0.9961 0.3059 0.053 Uiso 1 1 calc R B 1 H37B H 0.5829 1.0389 0.2402 0.053 Uiso 1 1 calc R B 1 C38 C 0.4366(7) 0.9784(5) 0.2657(6) 0.098(4) Uani 1 1 d . B 1 H38A H 0.4076 0.9931 0.3056 0.117 Uiso 1 1 calc R B 1 H38B H 0.4019 1.0203 0.2365 0.117 Uiso 1 1 calc R B 1 C39 C 0.4090(7) 0.8863(6) 0.2504(7) 0.116(5) Uani 1 1 d . B 1 H39A H 0.3612 0.8596 0.2816 0.139 Uiso 1 1 calc R B 1 H39B H 0.3663 0.8848 0.2123 0.139 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 U 0.01898(11) 0.02037(10) 0.02287(11) 0.00047(8) 0.00074(7) 0.00001(8) Si1 0.0325(9) 0.0267(8) 0.0189(7) -0.0016(6) 0.0032(6) -0.0050(6) Si2 0.0340(9) 0.0250(7) 0.0186(7) 0.0024(6) -0.0001(6) 0.0006(6) O 0.029(2) 0.026(2) 0.049(3) -0.0044(18) -0.0060(19) -0.0001(17) C1 0.021(3) 0.022(2) 0.023(3) 0.000(2) 0.000(2) -0.003(2) C2 0.022(3) 0.018(2) 0.023(3) 0.000(2) 0.000(2) -0.002(2) C3 0.024(3) 0.026(3) 0.018(3) -0.002(2) -0.001(2) -0.003(2) C4 0.023(3) 0.021(3) 0.019(2) 0.001(2) 0.003(2) 0.003(2) C5 0.025(3) 0.025(3) 0.021(3) 0.004(2) 0.003(2) 0.002(2) C6 0.025(3) 0.022(3) 0.026(3) 0.004(2) 0.003(2) 0.000(2) C7 0.023(3) 0.020(3) 0.029(3) -0.006(2) 0.000(2) 0.001(2) C8 0.026(3) 0.029(3) 0.025(3) -0.001(2) 0.005(2) -0.001(2) C9 0.038(4) 0.039(3) 0.032(3) 0.002(3) 0.009(3) -0.008(3) C10 0.038(4) 0.067(5) 0.085(6) 0.018(4) 0.008(4) 0.005(4) C11 0.046(5) 0.075(5) 0.040(4) -0.016(4) 0.009(3) -0.022(4) C12 0.047(4) 0.023(3) 0.025(3) 0.002(2) 0.000(3) -0.001(3) C13 0.071(5) 0.039(4) 0.032(3) 0.011(3) 0.001(3) -0.001(3) C14 0.045(4) 0.044(4) 0.037(4) 0.000(3) -0.005(3) 0.004(3) C15 0.057(4) 0.033(3) 0.020(3) -0.007(2) 0.007(3) -0.012(3) C16 0.095(6) 0.054(5) 0.027(3) -0.018(3) 0.020(4) -0.021(4) C17 0.062(5) 0.051(4) 0.030(3) -0.006(3) -0.003(3) -0.018(4) C18 0.039(4) 0.039(3) 0.026(3) -0.001(2) -0.011(3) -0.004(3) C19 0.025(4) 0.106(7) 0.057(5) 0.025(4) -0.003(3) -0.013(4) C20 0.054(5) 0.058(5) 0.065(5) -0.013(4) -0.016(4) 0.015(4) C21 0.063(5) 0.031(3) 0.021(3) 0.002(2) 0.001(3) -0.001(3) C22 0.187(12) 0.037(4) 0.053(5) -0.020(4) -0.046(6) 0.018(6) C23 0.077(6) 0.045(5) 0.086(6) 0.006(4) 0.020(5) 0.025(4) C24 0.053(4) 0.031(3) 0.028(3) 0.003(3) 0.007(3) -0.005(3) C25 0.094(7) 0.075(5) 0.025(4) 0.016(3) 0.003(4) -0.020(5) C26 0.056(5) 0.057(4) 0.045(4) -0.001(3) 0.025(3) -0.005(4) C27 0.029(3) 0.030(3) 0.054(4) 0.007(3) -0.009(3) 0.000(2) C28 0.009(3) 0.078(5) 0.038(3) -0.021(3) 0.002(2) -0.005(3) C29 0.022(3) 0.050(4) 0.041(4) 0.016(3) -0.008(3) -0.011(3) C30 0.025(3) 0.033(3) 0.046(4) -0.009(3) 0.003(3) -0.001(2) C31 0.025(3) 0.049(4) 0.033(3) 0.000(3) -0.003(2) -0.014(3) C32 0.048(5) 0.114(8) 0.067(6) -0.040(5) 0.008(4) 0.005(5) C33 0.044(5) 0.089(6) 0.053(5) 0.031(4) -0.001(4) -0.015(4) C34 0.043(4) 0.045(4) 0.097(6) -0.019(4) 0.007(4) -0.012(3) C35 0.053(5) 0.101(7) 0.036(4) 0.002(4) -0.007(3) -0.028(5) C36 0.041(4) 0.025(3) 0.048(4) -0.002(3) 0.004(3) -0.005(3) C37 0.043(4) 0.029(3) 0.062(4) -0.003(3) 0.007(3) -0.001(3) C38 0.036(5) 0.035(4) 0.223(13) -0.044(6) 0.015(6) 0.001(3) C39 0.036(5) 0.038(5) 0.275(16) -0.035(7) -0.003(7) 0.014(4) #----------------------------------------------------------------------------# # 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 U C5 2.675(5) . ? U C8 2.685(5) . ? U C6 2.691(5) . ? U C7 2.698(5) . ? U C3 2.717(5) . ? U C27 2.722(6) . ? U C2 2.722(5) . ? U C1 2.736(5) . ? U O 2.737(4) . ? U C4 2.737(5) . ? U C28 2.756(6) . ? U C31 2.770(6) . ? U C29 2.812(6) . ? U C30 2.814(6) . ? Si1 C9 1.897(6) . ? Si1 C15 1.902(6) . ? Si1 C12 1.906(6) . ? Si1 C1 1.907(5) . ? Si2 C18 1.894(7) . ? Si2 C21 1.895(6) . ? Si2 C4 1.900(5) . ? Si2 C24 1.901(6) . ? O C36 1.438(7) . ? O C39 1.443(9) . ? C1 C2 1.420(7) . ? C1 C8 1.421(7) . ? C2 C3 1.410(7) . ? C2 H2 0.95 . ? C3 C4 1.425(7) . ? C3 H3 0.95 . ? C4 C5 1.426(7) . ? C5 C6 1.406(7) . ? C5 H5 0.95 . ? C6 C7 1.408(7) . ? C6 H6 0.95 . ? C7 C8 1.408(7) . ? C7 H7 0.95 . ? C8 H8 0.95 . ? C9 C10 1.530(10) . ? C9 C11 1.538(9) . ? C9 H9 1 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C14 1.532(9) . ? C12 C13 1.535(8) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C17 1.526(9) . ? C15 C16 1.561(9) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.531(9) . ? C18 C20 1.533(9) . ? C18 H18 1 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.524(9) . ? C21 C23 1.530(11) . ? C21 H21 1 . ? 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 C26 1.526(10) . ? C24 C25 1.528(9) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C31 1.389(9) . ? C27 C28 1.416(9) . ? C27 H27 0.95 . ? C28 C29 1.409(9) . ? C28 C32 1.498(9) . ? C29 C30 1.393(9) . ? C29 C33 1.521(9) . ? C30 C31 1.385(9) . ? C30 C34 1.501(9) . ? C31 C35 1.517(9) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 C37 1.500(8) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 C38 1.466(10) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.446(11) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? 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 C5 U C8 79.49(16) . . ? C5 U C6 30.37(15) . . ? C8 U C6 58.09(16) . . ? C5 U C7 58.03(16) . . ? C8 U C7 30.32(16) . . ? C6 U C7 30.28(15) . . ? C5 U C3 57.19(16) . . ? C8 U C3 77.62(16) . . ? C6 U C3 76.58(16) . . ? C7 U C3 84.23(16) . . ? C5 U C27 135.81(18) . . ? C8 U C27 123.68(19) . . ? C6 U C27 126.68(17) . . ? C7 U C27 122.19(17) . . ? C3 U C27 153.51(17) . . ? C5 U C2 77.97(15) . . ? C8 U C2 57.02(16) . . ? C6 U C2 84.56(16) . . ? C7 U C2 76.46(15) . . ? C3 U C2 30.06(15) . . ? C27 U C2 145.78(17) . . ? C5 U C1 87.73(15) . . ? C8 U C1 30.36(15) . . ? C6 U C1 78.60(15) . . ? C7 U C1 57.62(15) . . ? C3 U C1 57.82(15) . . ? C27 U C1 132.26(18) . . ? C2 U C1 30.15(15) . . ? C5 U O 123.44(14) . . ? C8 U O 126.48(15) . . ? C6 U O 152.77(14) . . ? C7 U O 154.98(15) . . ? C3 U O 78.65(14) . . ? C27 U O 75.71(15) . . ? C2 U O 79.62(14) . . ? C1 U O 97.58(14) . . ? C5 U C4 30.51(15) . . ? C8 U C4 87.72(16) . . ? C6 U C4 57.84(15) . . ? C7 U C4 78.57(15) . . ? C3 U C4 30.30(15) . . ? C27 U C4 146.78(18) . . ? C2 U C4 58.10(15) . . ? C1 U C4 80.06(15) . . ? O U C4 94.93(13) . . ? C5 U C28 107.22(19) . . ? C8 U C28 139.60(18) . . ? C6 U C28 108.4(2) . . ? C7 U C28 120.53(19) . . ? C3 U C28 140.16(16) . . ? C27 U C28 29.9(2) . . ? C2 U C28 162.66(18) . . ? C1 U C28 161.15(17) . . ? O U C28 83.90(18) . . ? C4 U C28 118.63(17) . . ? C5 U C31 129.73(17) . . ? C8 U C31 95.74(18) . . ? C6 U C31 106.65(18) . . ? C7 U C31 93.92(18) . . ? C3 U C31 169.81(16) . . ? C27 U C31 29.29(19) . . ? C2 U C31 139.81(16) . . ? C1 U C31 112.85(16) . . ? O U C31 99.70(16) . . ? C4 U C31 158.76(17) . . ? C28 U C31 48.69(18) . . ? C5 U C29 89.18(16) . . ? C8 U C29 114.83(19) . . ? C6 U C29 81.16(18) . . ? C7 U C29 91.48(18) . . ? C3 U C29 142.57(16) . . ? C27 U C29 47.98(18) . . ? C2 U C29 165.69(17) . . ? C1 U C29 144.77(18) . . ? O U C29 113.17(17) . . ? C4 U C29 112.45(16) . . ? C28 U C29 29.3(2) . . ? C31 U C29 47.33(17) . . ? C5 U C30 101.01(17) . . ? C8 U C30 91.21(17) . . ? C6 U C30 80.19(17) . . ? C7 U C30 76.25(16) . . ? C3 U C30 156.74(17) . . ? C27 U C30 48.04(17) . . ? C2 U C30 148.07(16) . . ? C1 U C30 118.52(16) . . ? O U C30 123.75(15) . . ? C4 U C30 130.59(17) . . ? C28 U C30 48.47(18) . . ? C31 U C30 28.72(18) . . ? C29 U C30 28.67(18) . . ? C9 Si1 C15 105.5(3) . . ? C9 Si1 C12 108.0(3) . . ? C15 Si1 C12 112.5(3) . . ? C9 Si1 C1 109.8(3) . . ? C15 Si1 C1 110.2(2) . . ? C12 Si1 C1 110.6(2) . . ? C18 Si2 C21 107.1(3) . . ? C18 Si2 C4 108.2(3) . . ? C21 Si2 C4 111.1(2) . . ? C18 Si2 C24 106.4(3) . . ? C21 Si2 C24 113.3(3) . . ? C4 Si2 C24 110.5(3) . . ? C36 O C39 105.7(5) . . ? C36 O U 124.7(3) . . ? C39 O U 129.4(4) . . ? C2 C1 C8 130.7(5) . . ? C2 C1 Si1 112.6(4) . . ? C8 C1 Si1 116.5(4) . . ? C2 C1 U 74.4(3) . . ? C8 C1 U 72.8(3) . . ? Si1 C1 U 138.4(3) . . ? C3 C2 C1 137.4(5) . . ? C3 C2 U 74.8(3) . . ? C1 C2 U 75.5(3) . . ? C3 C2 H2 111.3 . . ? C1 C2 H2 111.3 . . ? U C2 H2 134.9 . . ? C2 C3 C4 138.4(5) . . ? C2 C3 U 75.2(3) . . ? C4 C3 U 75.7(3) . . ? C2 C3 H3 110.8 . . ? C4 C3 H3 110.8 . . ? U C3 H3 135.1 . . ? C3 C4 C5 129.7(5) . . ? C3 C4 Si2 113.7(4) . . ? C5 C4 Si2 116.2(4) . . ? C3 C4 U 74.0(3) . . ? C5 C4 U 72.3(3) . . ? Si2 C4 U 140.0(2) . . ? C6 C5 C4 136.0(5) . . ? C6 C5 U 75.4(3) . . ? C4 C5 U 77.2(3) . . ? C6 C5 H5 112 . . ? C4 C5 H5 112 . . ? U C5 H5 129.3 . . ? C5 C6 C7 135.8(5) . . ? C5 C6 U 74.2(3) . . ? C7 C6 U 75.2(3) . . ? C5 C6 H6 112.1 . . ? C7 C6 H6 112.1 . . ? U C6 H6 134.6 . . ? C6 C7 C8 136.0(5) . . ? C6 C7 U 74.6(3) . . ? C8 C7 U 74.3(3) . . ? C6 C7 H7 112 . . ? C8 C7 H7 112 . . ? U C7 H7 135.7 . . ? C7 C8 C1 135.7(5) . . ? C7 C8 U 75.4(3) . . ? C1 C8 U 76.8(3) . . ? C7 C8 H8 112.2 . . ? C1 C8 H8 112.2 . . ? U C8 H8 129.6 . . ? C10 C9 C11 109.7(6) . . ? C10 C9 Si1 111.2(5) . . ? C11 C9 Si1 116.5(5) . . ? C10 C9 H9 106.2 . . ? C11 C9 H9 106.2 . . ? Si1 C9 H9 106.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 109.9(5) . . ? C14 C12 Si1 114.4(4) . . ? C13 C12 Si1 112.4(4) . . ? C14 C12 H12 106.5 . . ? C13 C12 H12 106.5 . . ? Si1 C12 H12 106.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 109.0(5) . . ? C17 C15 Si1 115.3(5) . . ? C16 C15 Si1 114.2(4) . . ? C17 C15 H15 105.8 . . ? C16 C15 H15 105.8 . . ? Si1 C15 H15 105.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 110.8(6) . . ? C19 C18 Si2 113.3(4) . . ? C20 C18 Si2 111.8(5) . . ? C19 C18 H18 106.8 . . ? C20 C18 H18 106.8 . . ? Si2 C18 H18 106.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 109.4(7) . . ? C22 C21 Si2 113.0(5) . . ? C23 C21 Si2 114.2(5) . . ? C22 C21 H21 106.6 . . ? C23 C21 H21 106.6 . . ? Si2 C21 H21 106.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 109.8(6) . . ? C26 C24 Si2 114.6(5) . . ? C25 C24 Si2 114.2(5) . . ? C26 C24 H24 105.8 . . ? C25 C24 H24 105.8 . . ? Si2 C24 H24 105.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 C27 C28 108.6(6) . . ? C31 C27 U 77.3(4) . . ? C28 C27 U 76.4(3) . . ? C31 C27 H27 125.7 . . ? C28 C27 H27 125.7 . . ? U C27 H27 113 . . ? C29 C28 C27 105.7(5) . . ? C29 C28 C32 124.5(7) . . ? C27 C28 C32 129.7(7) . . ? C29 C28 U 77.5(3) . . ? C27 C28 U 73.7(3) . . ? C32 C28 U 116.7(4) . . ? C30 C29 C28 109.4(5) . . ? C30 C29 C33 125.2(7) . . ? C28 C29 C33 125.3(7) . . ? C30 C29 U 75.7(3) . . ? C28 C29 U 73.2(3) . . ? C33 C29 U 120.2(4) . . ? C31 C30 C29 107.5(5) . . ? C31 C30 C34 124.5(6) . . ? C29 C30 C34 127.1(6) . . ? C31 C30 U 73.9(3) . . ? C29 C30 U 75.6(3) . . ? C34 C30 U 124.3(4) . . ? C30 C31 C27 108.7(5) . . ? C30 C31 C35 127.3(6) . . ? C27 C31 C35 123.7(6) . . ? C30 C31 U 77.4(3) . . ? C27 C31 U 73.4(3) . . ? C35 C31 U 120.0(4) . . ? O C36 C37 107.9(5) . . ? O C36 H36A 110.1 . . ? C37 C36 H36A 110.1 . . ? O C36 H36B 110.1 . . ? C37 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? C38 C37 C36 104.6(6) . . ? C38 C37 H37A 110.8 . . ? C36 C37 H37A 110.8 . . ? C38 C37 H37B 110.8 . . ? C36 C37 H37B 110.8 . . ? H37A C37 H37B 108.9 . . ? C39 C38 C37 107.8(6) . . ? C39 C38 H38A 110.1 . . ? C37 C38 H38A 110.1 . . ? C39 C38 H38B 110.1 . . ? C37 C38 H38B 110.1 . . ? H38A C38 H38B 108.5 . . ? O C39 C38 109.4(7) . . ? O C39 H39A 109.8 . . ? C38 C39 H39A 109.8 . . ? O C39 H39B 109.8 . . ? C38 C39 H39B 109.8 . . ? H39A C39 H39B 108.2 . . ? #===END