#------------------------------------------------------------------------------ #$Date: 2015-10-09 16:07:17 +0300 (Fri, 09 Oct 2015) $ #$Revision: 162082 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/48/7054811.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7054811 loop_ _publ_author_name 'Kahan, Rachel J.' 'Cloke, F. Geoffrey N.' 'Roe, S. Mark' 'Nief, Fran\,cois' _publ_section_title ; Activation of carbon dioxide by new mixed sandwich uranium(iii) complexes incorporating cyclooctatetraenyl and pyrrolide, phospholide, or arsolide ligands ; _journal_issue 10 _journal_name_full 'New J. Chem.' _journal_page_first 7602 _journal_paper_doi 10.1039/C5NJ00590F _journal_volume 39 _journal_year 2015 _chemical_formula_moiety 'C38 H68 O P Si2 U' _chemical_formula_sum 'C38 H68 O P Si2 U' _chemical_formula_weight 866.10 _chemical_name_common 2THF _chemical_properties_physical 'Air-sensitive, Moisture-sensitive, Oxygen-sensitive' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2015-03-02 _audit_creation_method ; Olex2 1.2-beta (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _audit_update_record ; 2015-04-16 deposited with the CCDC. 2015-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 89.568(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8847(7) _cell_length_b 14.9475(8) _cell_length_c 22.5236(14) _cell_measurement_reflns_used 9724 _cell_measurement_temperature 173 _cell_measurement_theta_max 28.7710 _cell_measurement_theta_min 3.6600 _cell_volume 4001.1(4) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 173 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1033 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.872 _diffrn_measurement_details ; 1 omega -46.00 55.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -16.1295 19.0000 -120.0000 101 2 omega -88.00 -49.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -16.1295 -178.0000 -60.0000 39 3 omega -53.00 6.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -16.1295 -77.0000 -150.0000 59 4 omega -26.00 53.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -16.1295 38.0000 120.0000 79 5 omega -79.00 1.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -16.1295 -57.0000 -60.0000 80 6 omega -26.00 -1.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 16.7545 105.0000 171.0000 25 7 omega 27.00 56.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 16.7545 -99.0000 120.0000 29 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0515873000 _diffrn_orient_matrix_UB_12 -0.0014749000 _diffrn_orient_matrix_UB_13 0.0159227000 _diffrn_orient_matrix_UB_21 -0.0276183000 _diffrn_orient_matrix_UB_22 -0.0151540000 _diffrn_orient_matrix_UB_23 -0.0259925000 _diffrn_orient_matrix_UB_31 0.0110264000 _diffrn_orient_matrix_UB_32 -0.0449511000 _diffrn_orient_matrix_UB_33 0.0082602000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type Mo/Ka _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_unetI/netI 0.0419 _diffrn_reflns_laue_measured_fraction_full 0.997 _diffrn_reflns_laue_measured_fraction_max 0.872 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 34897 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.872 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.374 _diffrn_reflns_theta_min 3.429 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 4.183 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.52799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.438 _exptl_crystal_description needle _exptl_crystal_F_000 1756 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: pentane' _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.051 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.103 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 490 _refine_ls_number_reflns 9625 _refine_ls_number_restraints 615 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0298 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+2.1311P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.0700 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7914 _reflns_number_total 9625 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5nj00590f2.cif _cod_data_source_block 2THF _cod_depositor_comments 'Adding full bibliography for 7054809--7054814.cif.' _cod_database_code 7054811 _chemical_oxdiff_formula 'C38 H68 O1 P1 Si2 U1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.787 _shelx_estimated_absorpt_t_min 0.181 _reflns_odcompleteness_completeness 99.69 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints P1, C30, C29, C28, C27, C34, C33, C32, C31 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 P1A, C30A, C29A, C28A, C27A, C34A, C33A, C32A, C31A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints P1 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C34 \\sim C33 \\sim C32 \\sim C31: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 P1A \\sim C30A \\sim C29A \\sim C28A \\sim C27A \\sim C34A \\sim C33A \\sim C32A \\sim C31A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2 4. Rigid body (RIGU) restrains P1A, C30A, C29A, C28A, C27A, C34A, C33A, C32A, C31A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 P1, C27, C28, C29, C30, C31, C32, C33, C34 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C35, C36, C37, C38, O1, Si1, Si2, U1 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(P1A)=Sof(C30A)=Sof(C29A)=Sof(C28A)=Sof(C27A)=Sof(C34A)=Sof(H34A)= Sof(H34B)=Sof(H34C)=Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C32A)= Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=1-FVAR(1) Sof(P1)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(H31D)=Sof(H31E)= Sof(H31F)=Sof(C32)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33)=Sof(H33D)=Sof(H33E)= Sof(H33F)=Sof(C34)=Sof(H34D)=Sof(H34E)=Sof(H34F)=FVAR(1) 6.a Ternary CH refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C15(H15), C18(H18), C21(H21), C24(H24) 6.b Secondary CH2 refined with riding coordinates: C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B) 6.c Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B, H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A, H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C31(H31D,H31E,H31F), C32(H32D,H32E,H32F), C33(H33D,H33E, H33F), C34(H34D,H34E,H34F), C34A(H34A,H34B,H34C), C33A(H33A,H33B,H33C), C32A(H32A,H32B,H32C), C31A(H31A,H31B,H31C) ; _shelx_res_file ; rjk568.res created by SHELXL-2014/7 TITL rjk568_a.res in P2(1)/n CELL 0.71073 11.884709 14.947505 22.523607 90 89.5677 90 ZERR 4 0.000695 0.00083 0.001444 0 0.005 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O P Si U UNIT 152 272 4 4 8 4 DELU P1 C30 C29 C28 C27 C34 C33 C32 C31 DELU P1A C30A C29A C28A C27A C34A C33A C32A C31A SIMU 0.04 0.08 1.7 P1 C30 C29 C28 C27 C34 C33 C32 C31 SIMU 0.04 0.08 1.7 P1A C30A C29A C28A C27A C34A C33A C32A C31A RIGU P1A > C31A RIGU P1 > C34 RIGU C1 > C26 C35 > U1 ISOR 0.01 0.2 C35 L.S. 20 PLAN 5 SIZE 0.06 0.12 0.62 TEMP -100 MORE -1 BOND $H CONF LIST 6 fmap 2 ACTA 52 MERG 2 OMIT 0 1 6 REM REM REM WGHT 0.028700 2.131100 FVAR 1.28047 0.79662 C1 1 0.715505 0.664510 0.658343 11.00000 0.02165 0.03013 = 0.02294 -0.00057 0.00292 0.00001 C2 1 0.750143 0.719169 0.706904 11.00000 0.02057 0.02392 = 0.02548 0.00334 0.00271 0.00110 AFIX 13 H2 2 0.745520 0.783417 0.694788 11.00000 -1.20000 AFIX 0 C3 1 0.753045 0.714294 0.769627 11.00000 0.02205 0.02573 = 0.02321 0.00036 0.00078 0.00045 AFIX 13 H3 2 0.748895 0.776555 0.785741 11.00000 -1.20000 AFIX 0 C4 1 0.719927 0.653329 0.816065 11.00000 0.01958 0.02783 = 0.02373 0.00061 0.00196 0.00243 C5 1 0.674001 0.565605 0.811542 11.00000 0.02394 0.03013 = 0.02373 0.00405 0.00246 0.00371 AFIX 13 H5 2 0.632781 0.548964 0.848803 11.00000 -1.20000 AFIX 0 C6 1 0.645862 0.506746 0.764627 11.00000 0.02133 0.02350 = 0.03458 0.00408 0.00402 0.00251 AFIX 13 H6 2 0.589410 0.461856 0.778868 11.00000 -1.20000 AFIX 0 C7 1 0.644179 0.511428 0.701874 11.00000 0.02640 0.02173 = 0.03230 -0.00261 0.00088 -0.00064 AFIX 13 H7 2 0.586896 0.468843 0.686010 11.00000 -1.20000 AFIX 0 C8 1 0.670998 0.576455 0.658358 11.00000 0.02276 0.02801 = 0.02817 -0.00392 0.00012 0.00012 AFIX 13 H8 2 0.627229 0.565443 0.621325 11.00000 -1.20000 AFIX 0 C9 1 0.909844 0.736564 0.579747 11.00000 0.03637 0.04045 = 0.02724 -0.00120 0.00750 -0.01036 AFIX 13 H9 2 0.927197 0.750545 0.537237 11.00000 -1.20000 AFIX 0 C10 1 0.954726 0.816770 0.615871 11.00000 0.03716 0.06392 = 0.04704 -0.01395 0.00712 -0.01778 AFIX 137 H10A 2 0.948933 0.803347 0.658372 11.00000 -1.50000 H10B 2 0.910050 0.870134 0.606924 11.00000 -1.50000 H10C 2 1.033642 0.827668 0.605214 11.00000 -1.50000 AFIX 0 C11 1 0.977496 0.652496 0.594318 11.00000 0.03522 0.05804 = 0.07809 0.01067 0.00921 -0.00110 AFIX 137 H11A 2 1.057451 0.663468 0.586233 11.00000 -1.50000 H11B 2 0.951337 0.602697 0.569716 11.00000 -1.50000 H11C 2 0.967068 0.637434 0.636347 11.00000 -1.50000 AFIX 0 C12 1 0.722595 0.632076 0.520827 11.00000 0.04446 0.03686 = 0.02904 -0.00567 0.00441 -0.01022 AFIX 13 H12 2 0.745959 0.572188 0.536215 11.00000 -1.20000 AFIX 0 C13 1 0.792868 0.647283 0.463414 11.00000 0.06260 0.06532 = 0.03450 -0.01836 0.01274 -0.02362 AFIX 137 H13A 2 0.773269 0.601725 0.433961 11.00000 -1.50000 H13B 2 0.873151 0.642917 0.472596 11.00000 -1.50000 H13C 2 0.776589 0.706818 0.447405 11.00000 -1.50000 AFIX 0 C14 1 0.598281 0.622696 0.504773 11.00000 0.05161 0.05328 = 0.03782 -0.01002 -0.00323 -0.01228 AFIX 137 H14A 2 0.573821 0.676083 0.483161 11.00000 -1.50000 H14B 2 0.553271 0.616248 0.541156 11.00000 -1.50000 H14C 2 0.588133 0.569748 0.479718 11.00000 -1.50000 AFIX 0 C15 1 0.677695 0.825854 0.572682 11.00000 0.04231 0.03143 = 0.02943 0.00024 -0.00351 -0.00249 AFIX 13 H15 2 0.709657 0.867999 0.602629 11.00000 -1.20000 AFIX 0 C16 1 0.700998 0.868082 0.511047 11.00000 0.07988 0.03967 = 0.03683 0.00731 -0.00303 -0.00034 AFIX 137 H16A 2 0.671095 0.828991 0.480002 11.00000 -1.50000 H16B 2 0.782307 0.875283 0.505273 11.00000 -1.50000 H16C 2 0.664344 0.926705 0.508847 11.00000 -1.50000 AFIX 0 C17 1 0.551317 0.821508 0.585067 11.00000 0.04384 0.04340 = 0.04965 -0.00327 -0.00737 0.00614 AFIX 137 H17A 2 0.520243 0.882232 0.585709 11.00000 -1.50000 H17B 2 0.537929 0.792835 0.623605 11.00000 -1.50000 H17C 2 0.514671 0.786666 0.553834 11.00000 -1.50000 AFIX 0 C18 1 0.918419 0.678061 0.900617 11.00000 0.03133 0.04386 = 0.03094 -0.00210 -0.00473 -0.00038 AFIX 13 H18 2 0.938389 0.699304 0.941298 11.00000 -1.20000 AFIX 0 C19 1 0.986503 0.735565 0.856401 11.00000 0.03246 0.09422 = 0.05771 0.01887 -0.00211 -0.00990 AFIX 137 H19A 2 1.066965 0.729478 0.864706 11.00000 -1.50000 H19B 2 0.964290 0.798407 0.860550 11.00000 -1.50000 H19C 2 0.971567 0.715390 0.815819 11.00000 -1.50000 AFIX 0 C20 1 0.955370 0.579691 0.896596 11.00000 0.04905 0.05394 = 0.07190 -0.01318 -0.01505 0.01526 AFIX 137 H20A 2 0.931820 0.554674 0.858439 11.00000 -1.50000 H20B 2 0.920415 0.545657 0.929028 11.00000 -1.50000 H20C 2 1.037437 0.576021 0.899756 11.00000 -1.50000 AFIX 0 C21 1 0.694911 0.615743 0.951527 11.00000 0.04873 0.03826 = 0.02765 0.00200 0.00345 -0.00494 AFIX 13 H21 2 0.716503 0.553485 0.939850 11.00000 -1.20000 AFIX 0 C22 1 0.742331 0.629239 1.014118 11.00000 0.09197 0.07493 = 0.02728 0.00908 -0.00110 -0.02486 AFIX 137 H22A 2 0.722021 0.688983 1.028562 11.00000 -1.50000 H22B 2 0.824448 0.623432 1.012821 11.00000 -1.50000 H22C 2 0.710790 0.583917 1.040917 11.00000 -1.50000 AFIX 0 C23 1 0.566091 0.616310 0.953817 11.00000 0.05720 0.06340 = 0.05198 0.00181 0.02062 -0.01213 AFIX 137 H23A 2 0.539287 0.563364 0.975335 11.00000 -1.50000 H23B 2 0.536575 0.615516 0.913311 11.00000 -1.50000 H23C 2 0.539980 0.670414 0.974271 11.00000 -1.50000 AFIX 0 C24 1 0.726215 0.814593 0.905298 11.00000 0.05346 0.03019 = 0.03050 0.00018 0.00470 0.00558 AFIX 13 H24 2 0.757068 0.847304 0.870034 11.00000 -1.20000 AFIX 0 C25 1 0.782862 0.855012 0.959587 11.00000 0.11627 0.04344 = 0.07651 -0.02592 -0.03698 0.01364 AFIX 137 H25A 2 0.763807 0.918666 0.962405 11.00000 -1.50000 H25B 2 0.864630 0.848314 0.955808 11.00000 -1.50000 H25C 2 0.756550 0.824028 0.995435 11.00000 -1.50000 AFIX 0 C26 1 0.601017 0.834642 0.907404 11.00000 0.07271 0.05816 = 0.08640 -0.00143 0.00291 0.02867 AFIX 137 H26A 2 0.567748 0.807562 0.943061 11.00000 -1.50000 H26B 2 0.565031 0.809765 0.872050 11.00000 -1.50000 H26C 2 0.589456 0.899539 0.908460 11.00000 -1.50000 AFIX 0 PART 1 P1 4 0.306051 0.680050 0.784599 21.00000 0.02080 0.04363 = 0.04239 -0.00974 0.00519 -0.00098 C27 1 0.348258 0.568140 0.787662 21.00000 0.01536 0.03635 = 0.04493 0.00897 0.00537 -0.00550 C28 1 0.364687 0.530283 0.731639 21.00000 0.02303 0.02920 = 0.05856 -0.00318 0.00750 -0.00695 C29 1 0.346913 0.592435 0.683818 21.00000 0.01979 0.04083 = 0.04555 -0.01040 0.00238 -0.01075 C30 1 0.300563 0.697566 0.712236 21.00000 0.01509 0.03329 = 0.03757 -0.00412 -0.00240 -0.00372 C31 1 0.353145 0.516139 0.846138 21.00000 0.04229 0.08214 = 0.07067 0.04165 -0.00190 -0.02090 AFIX 137 H31D 2 0.346449 0.557898 0.879521 21.00000 -1.50000 H31E 2 0.425003 0.484234 0.848541 21.00000 -1.50000 H31F 2 0.291110 0.472995 0.847788 21.00000 -1.50000 AFIX 0 C32 1 0.383023 0.432343 0.722007 21.00000 0.03235 0.03571 = 0.13952 -0.01930 0.00410 -0.00868 AFIX 137 H32D 2 0.429063 0.408289 0.754199 21.00000 -1.50000 H32E 2 0.421794 0.423002 0.683956 21.00000 -1.50000 H32F 2 0.310227 0.401564 0.721555 21.00000 -1.50000 AFIX 0 C33 1 0.348733 0.568415 0.619336 21.00000 0.05102 0.09701 = 0.05255 -0.02789 0.00226 -0.02593 AFIX 137 H33D 2 0.405548 0.522044 0.612223 21.00000 -1.50000 H33E 2 0.367237 0.621577 0.595744 21.00000 -1.50000 H33F 2 0.274607 0.545891 0.607803 21.00000 -1.50000 AFIX 0 C34 1 0.279184 0.754628 0.665787 21.00000 0.04494 0.06959 = 0.07202 0.02884 -0.01592 -0.00181 AFIX 137 H34D 2 0.209329 0.787499 0.673726 21.00000 -1.50000 H34E 2 0.271400 0.720015 0.629095 21.00000 -1.50000 H34F 2 0.341586 0.797039 0.661435 21.00000 -1.50000 AFIX 0 PART 0 C35 1 0.417925 0.889816 0.771800 11.00000 0.04184 0.04928 = 0.18101 -0.03014 0.01411 0.00717 AFIX 23 H35A 2 0.353701 0.876105 0.745583 11.00000 -1.20000 H35B 2 0.397914 0.870710 0.812619 11.00000 -1.20000 AFIX 0 C36 1 0.440349 0.984374 0.770946 11.00000 0.04256 0.03927 = 0.15535 -0.02622 0.01166 0.00185 AFIX 23 H36A 2 0.408104 1.013402 0.806731 11.00000 -1.20000 H36B 2 0.406893 1.012273 0.735337 11.00000 -1.20000 AFIX 0 C37 1 0.564365 0.994315 0.769798 11.00000 0.03769 0.03049 = 0.06913 -0.01007 0.01184 -0.00151 AFIX 23 H37A 2 0.594483 1.000863 0.810428 11.00000 -1.20000 H37B 2 0.587440 1.046731 0.745754 11.00000 -1.20000 AFIX 0 C38 1 0.603841 0.908294 0.741587 11.00000 0.03825 0.02902 = 0.05108 -0.00050 0.00326 -0.00024 AFIX 23 H38A 2 0.616563 0.916981 0.698483 11.00000 -1.20000 H38B 2 0.675313 0.888533 0.759682 11.00000 -1.20000 AFIX 0 O1 3 0.516811 0.842123 0.751610 11.00000 0.02510 0.02645 = 0.06090 -0.00904 -0.00066 0.00112 SI1 5 0.753133 0.715138 0.583342 11.00000 0.02941 0.02901 = 0.02173 -0.00142 0.00232 -0.00535 SI2 5 0.761202 0.691399 0.893332 11.00000 0.02953 0.02796 = 0.02152 0.00090 0.00050 -0.00054 U1 6 0.542155 0.662350 0.739878 11.00000 0.01742 0.02253 = 0.02833 0.00000 0.00124 0.00002 PART 2 P1A 4 0.318845 0.675749 0.704399 -21.00000 0.02548 0.05735 = 0.03974 -0.00231 0.00168 -0.00095 C30A 1 0.339051 0.607814 0.681687 -21.00000 0.02886 0.05321 = 0.03546 -0.00204 0.00207 -0.00103 C29A 1 0.367083 0.536491 0.713361 -21.00000 0.01143 0.04886 = 0.03171 -0.00529 0.00497 -0.00610 C28A 1 0.357179 0.554581 0.773788 -21.00000 0.01709 0.04909 = 0.03460 -0.00287 0.00353 0.00225 C27A 1 0.323882 0.642740 0.783754 -21.00000 0.07372 0.06147 = 0.03293 -0.00765 -0.00236 0.02662 C34A 1 0.341884 0.597744 0.611592 -21.00000 0.04184 0.03716 = 0.03521 -0.00102 0.00296 -0.00728 AFIX 137 H34A 2 0.348546 0.657025 0.593316 -21.00000 -1.50000 H34B 2 0.272319 0.569052 0.598329 -21.00000 -1.50000 H34C 2 0.406535 0.560932 0.599819 -21.00000 -1.50000 AFIX 0 C33A 1 0.377951 0.435389 0.694339 -21.00000 0.01425 0.04793 = 0.04377 -0.00610 0.00824 -0.00422 AFIX 137 H33A 2 0.302859 0.408557 0.692154 -21.00000 -1.50000 H33B 2 0.422895 0.403077 0.723671 -21.00000 -1.50000 H33C 2 0.414857 0.431659 0.655362 -21.00000 -1.50000 AFIX 0 C32A 1 0.359941 0.496589 0.827066 -21.00000 0.02399 0.05808 = 0.03307 -0.00171 0.00213 0.00338 AFIX 137 H32A 2 0.359518 0.433680 0.814817 -21.00000 -1.50000 H32B 2 0.293760 0.508738 0.852001 -21.00000 -1.50000 H32C 2 0.428373 0.508974 0.849636 -21.00000 -1.50000 AFIX 0 C31A 1 0.300612 0.699786 0.841065 -21.00000 0.04000 0.07029 = 0.04183 -0.01566 0.00932 0.01298 AFIX 137 H31A 2 0.372007 0.722147 0.856712 -21.00000 -1.50000 H31B 2 0.263444 0.662392 0.871091 -21.00000 -1.50000 H31C 2 0.251859 0.750430 0.831169 -21.00000 -1.50000 AFIX 0 HKLF 4 REM rjk568_a.res in P2(1)/n REM R1 = 0.0298 for 7914 Fo > 4sig(Fo) and 0.0429 for all 9625 data REM 490 parameters refined using 615 restraints END WGHT 0.0287 2.1311 REM Highest difference peak 1.051, deepest hole -0.965, 1-sigma level 0.103 Q1 1 0.5570 0.6035 0.7306 11.00000 0.05 1.05 Q2 1 0.4950 0.7250 0.7504 11.00000 0.05 0.91 Q3 1 0.6225 0.6613 0.7446 11.00000 0.05 0.86 Q4 1 0.4600 0.6553 0.7387 11.00000 0.05 0.80 Q5 1 0.5582 0.6566 0.7052 11.00000 0.05 0.70 ; _shelx_res_checksum 64062 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7155(3) 0.6645(2) 0.65834(14) 0.0249(7) Uani 1 1 d . U . . . C2 C 0.7501(3) 0.7192(2) 0.70690(14) 0.0233(6) Uani 1 1 d . U . . . H2 H 0.7455 0.7834 0.6948 0.028 Uiso 1 1 calc R . . . . C3 C 0.7530(3) 0.7143(2) 0.76963(14) 0.0237(7) Uani 1 1 d . U . . . H3 H 0.7489 0.7766 0.7857 0.028 Uiso 1 1 calc R . . . . C4 C 0.7199(3) 0.6533(2) 0.81607(14) 0.0237(7) Uani 1 1 d . U . . . C5 C 0.6740(3) 0.5656(2) 0.81154(14) 0.0259(7) Uani 1 1 d . U . . . H5 H 0.6328 0.5490 0.8488 0.031 Uiso 1 1 calc R . . . . C6 C 0.6459(3) 0.5067(2) 0.76463(15) 0.0265(7) Uani 1 1 d . U . . . H6 H 0.5894 0.4619 0.7789 0.032 Uiso 1 1 calc R . . . . C7 C 0.6442(3) 0.5114(2) 0.70187(15) 0.0268(7) Uani 1 1 d . U . . . H7 H 0.5869 0.4688 0.6860 0.032 Uiso 1 1 calc R . . . . C8 C 0.6710(3) 0.5765(2) 0.65836(15) 0.0263(7) Uani 1 1 d . U . . . H8 H 0.6272 0.5654 0.6213 0.032 Uiso 1 1 calc R . . . . C9 C 0.9098(3) 0.7366(2) 0.57975(16) 0.0347(8) Uani 1 1 d . U . . . H9 H 0.9272 0.7505 0.5372 0.042 Uiso 1 1 calc R . . . . C10 C 0.9547(4) 0.8168(3) 0.61587(19) 0.0494(11) Uani 1 1 d . U . . . H10A H 0.9489 0.8033 0.6584 0.074 Uiso 1 1 calc GR . . . . H10B H 0.9101 0.8701 0.6069 0.074 Uiso 1 1 calc GR . . . . H10C H 1.0336 0.8277 0.6052 0.074 Uiso 1 1 calc GR . . . . C11 C 0.9775(4) 0.6525(3) 0.5943(2) 0.0572(12) Uani 1 1 d . U . . . H11A H 1.0575 0.6635 0.5862 0.086 Uiso 1 1 calc GR . . . . H11B H 0.9513 0.6027 0.5697 0.086 Uiso 1 1 calc GR . . . . H11C H 0.9671 0.6374 0.6363 0.086 Uiso 1 1 calc GR . . . . C12 C 0.7226(3) 0.6321(3) 0.52083(16) 0.0368(8) Uani 1 1 d . U . . . H12 H 0.7460 0.5722 0.5362 0.044 Uiso 1 1 calc R . . . . C13 C 0.7929(4) 0.6473(3) 0.46341(19) 0.0542(12) Uani 1 1 d . U . . . H13A H 0.7733 0.6017 0.4340 0.081 Uiso 1 1 calc GR . . . . H13B H 0.8732 0.6429 0.4726 0.081 Uiso 1 1 calc GR . . . . H13C H 0.7766 0.7068 0.4474 0.081 Uiso 1 1 calc GR . . . . C14 C 0.5983(4) 0.6227(3) 0.50477(18) 0.0476(10) Uani 1 1 d . U . . . H14A H 0.5738 0.6761 0.4832 0.071 Uiso 1 1 calc GR . . . . H14B H 0.5533 0.6162 0.5412 0.071 Uiso 1 1 calc GR . . . . H14C H 0.5881 0.5697 0.4797 0.071 Uiso 1 1 calc GR . . . . C15 C 0.6777(3) 0.8259(2) 0.57268(16) 0.0344(8) Uani 1 1 d . U . . . H15 H 0.7097 0.8680 0.6026 0.041 Uiso 1 1 calc R . . . . C16 C 0.7010(4) 0.8681(3) 0.51105(18) 0.0521(11) Uani 1 1 d . U . . . H16A H 0.6711 0.8290 0.4800 0.078 Uiso 1 1 calc GR . . . . H16B H 0.7823 0.8753 0.5053 0.078 Uiso 1 1 calc GR . . . . H16C H 0.6643 0.9267 0.5088 0.078 Uiso 1 1 calc GR . . . . C17 C 0.5513(4) 0.8215(3) 0.5851(2) 0.0456(10) Uani 1 1 d . U . . . H17A H 0.5202 0.8822 0.5857 0.068 Uiso 1 1 calc GR . . . . H17B H 0.5379 0.7928 0.6236 0.068 Uiso 1 1 calc GR . . . . H17C H 0.5147 0.7867 0.5538 0.068 Uiso 1 1 calc GR . . . . C18 C 0.9184(3) 0.6781(2) 0.90062(17) 0.0354(8) Uani 1 1 d . U . . . H18 H 0.9384 0.6993 0.9413 0.042 Uiso 1 1 calc R . . . . C19 C 0.9865(4) 0.7356(3) 0.8564(2) 0.0615(13) Uani 1 1 d . U . . . H19A H 1.0670 0.7295 0.8647 0.092 Uiso 1 1 calc GR . . . . H19B H 0.9643 0.7984 0.8606 0.092 Uiso 1 1 calc GR . . . . H19C H 0.9716 0.7154 0.8158 0.092 Uiso 1 1 calc GR . . . . C20 C 0.9554(4) 0.5797(3) 0.8966(2) 0.0582(12) Uani 1 1 d . U . . . H20A H 0.9318 0.5547 0.8584 0.087 Uiso 1 1 calc GR . . . . H20B H 0.9204 0.5457 0.9290 0.087 Uiso 1 1 calc GR . . . . H20C H 1.0374 0.5760 0.8998 0.087 Uiso 1 1 calc GR . . . . C21 C 0.6949(3) 0.6157(3) 0.95153(16) 0.0382(9) Uani 1 1 d . U . . . H21 H 0.7165 0.5535 0.9399 0.046 Uiso 1 1 calc R . . . . C22 C 0.7423(5) 0.6292(3) 1.01412(18) 0.0647(14) Uani 1 1 d . U . . . H22A H 0.7220 0.6890 1.0286 0.097 Uiso 1 1 calc GR . . . . H22B H 0.8244 0.6234 1.0128 0.097 Uiso 1 1 calc GR . . . . H22C H 0.7108 0.5839 1.0409 0.097 Uiso 1 1 calc GR . . . . C23 C 0.5661(4) 0.6163(3) 0.9538(2) 0.0576(12) Uani 1 1 d . U . . . H23A H 0.5393 0.5634 0.9753 0.086 Uiso 1 1 calc GR . . . . H23B H 0.5366 0.6155 0.9133 0.086 Uiso 1 1 calc GR . . . . H23C H 0.5400 0.6704 0.9743 0.086 Uiso 1 1 calc GR . . . . C24 C 0.7262(3) 0.8146(2) 0.90530(16) 0.0381(9) Uani 1 1 d . U . . . H24 H 0.7571 0.8473 0.8700 0.046 Uiso 1 1 calc R . . . . C25 C 0.7829(6) 0.8550(3) 0.9596(3) 0.0786(18) Uani 1 1 d . U . . . H25A H 0.7638 0.9187 0.9624 0.118 Uiso 1 1 calc GR . . . . H25B H 0.8646 0.8483 0.9558 0.118 Uiso 1 1 calc GR . . . . H25C H 0.7566 0.8240 0.9954 0.118 Uiso 1 1 calc GR . . . . C26 C 0.6010(5) 0.8346(3) 0.9074(3) 0.0724(15) Uani 1 1 d . U . . . H26A H 0.5677 0.8076 0.9431 0.109 Uiso 1 1 calc GR . . . . H26B H 0.5650 0.8098 0.8720 0.109 Uiso 1 1 calc GR . . . . H26C H 0.5895 0.8995 0.9085 0.109 Uiso 1 1 calc GR . . . . P1 P 0.30605(12) 0.68005(11) 0.78460(7) 0.0356(4) Uani 0.797(4) 1 d . U P A 1 C27 C 0.3483(8) 0.5681(5) 0.7877(3) 0.0322(17) Uani 0.797(4) 1 d . U P A 1 C28 C 0.3647(8) 0.5303(5) 0.7316(3) 0.0370(17) Uani 0.797(4) 1 d . U P A 1 C29 C 0.3469(12) 0.5924(7) 0.6838(7) 0.0354(19) Uani 0.797(4) 1 d . U P A 1 C30 C 0.3006(10) 0.6976(6) 0.7122(5) 0.0286(17) Uani 0.797(4) 1 d . U P A 1 C31 C 0.3531(9) 0.5161(7) 0.8461(4) 0.065(3) Uani 0.797(4) 1 d . U P A 1 H31D H 0.3464 0.5579 0.8795 0.098 Uiso 0.797(4) 1 calc GR . P A 1 H31E H 0.4250 0.4842 0.8485 0.098 Uiso 0.797(4) 1 calc GR . P A 1 H31F H 0.2911 0.4730 0.8478 0.098 Uiso 0.797(4) 1 calc GR . P A 1 C32 C 0.3830(8) 0.4323(5) 0.7220(4) 0.069(3) Uani 0.797(4) 1 d . U P A 1 H32D H 0.4291 0.4083 0.7542 0.104 Uiso 0.797(4) 1 calc GR . P A 1 H32E H 0.4218 0.4230 0.6840 0.104 Uiso 0.797(4) 1 calc GR . P A 1 H32F H 0.3102 0.4016 0.7216 0.104 Uiso 0.797(4) 1 calc GR . P A 1 C33 C 0.3487(13) 0.5684(7) 0.6193(4) 0.067(3) Uani 0.797(4) 1 d . U P A 1 H33D H 0.4055 0.5220 0.6122 0.100 Uiso 0.797(4) 1 calc GR . P A 1 H33E H 0.3672 0.6216 0.5957 0.100 Uiso 0.797(4) 1 calc GR . P A 1 H33F H 0.2746 0.5459 0.6078 0.100 Uiso 0.797(4) 1 calc GR . P A 1 C34 C 0.2792(5) 0.7546(4) 0.6658(3) 0.0621(17) Uani 0.797(4) 1 d . U P A 1 H34D H 0.2093 0.7875 0.6737 0.093 Uiso 0.797(4) 1 calc GR . P A 1 H34E H 0.2714 0.7200 0.6291 0.093 Uiso 0.797(4) 1 calc GR . P A 1 H34F H 0.3416 0.7970 0.6614 0.093 Uiso 0.797(4) 1 calc GR . P A 1 C35 C 0.4179(4) 0.8898(3) 0.7718(3) 0.0908(19) Uani 1 1 d . U . . . H35A H 0.3537 0.8761 0.7456 0.109 Uiso 1 1 calc R . . . . H35B H 0.3979 0.8707 0.8126 0.109 Uiso 1 1 calc R . . . . C36 C 0.4403(4) 0.9844(3) 0.7709(3) 0.0791(18) Uani 1 1 d . U . . . H36A H 0.4081 1.0134 0.8067 0.095 Uiso 1 1 calc R . . . . H36B H 0.4069 1.0123 0.7353 0.095 Uiso 1 1 calc R . . . . C37 C 0.5644(3) 0.9943(2) 0.7698(2) 0.0458(10) Uani 1 1 d . U . . . H37A H 0.5945 1.0009 0.8104 0.055 Uiso 1 1 calc R . . . . H37B H 0.5874 1.0467 0.7458 0.055 Uiso 1 1 calc R . . . . C38 C 0.6038(3) 0.9083(2) 0.74159(18) 0.0395(9) Uani 1 1 d . U . . . H38A H 0.6166 0.9170 0.6985 0.047 Uiso 1 1 calc R . . . . H38B H 0.6753 0.8885 0.7597 0.047 Uiso 1 1 calc R . . . . O1 O 0.5168(2) 0.84212(14) 0.75161(13) 0.0375(6) Uani 1 1 d . U . . . Si1 Si 0.75313(8) 0.71514(6) 0.58334(4) 0.0267(2) Uani 1 1 d . U . . . Si2 Si 0.76120(8) 0.69140(6) 0.89333(4) 0.0263(2) Uani 1 1 d . U . . . U1 U 0.54216(2) 0.66235(2) 0.73988(2) 0.02277(5) Uani 1 1 d . U . . . P1A P 0.3188(12) 0.6757(8) 0.7044(5) 0.041(2) Uani 0.203(4) 1 d . U P A 2 C30A C 0.339(6) 0.608(4) 0.682(3) 0.039(7) Uani 0.203(4) 1 d . U P A 2 C29A C 0.367(3) 0.536(3) 0.7134(12) 0.031(4) Uani 0.203(4) 1 d . U P A 2 C28A C 0.357(4) 0.555(3) 0.7738(17) 0.034(5) Uani 0.203(4) 1 d . U P A 2 C27A C 0.324(3) 0.643(2) 0.7838(12) 0.056(7) Uani 0.203(4) 1 d . U P A 2 C34A C 0.342(5) 0.598(2) 0.6116(16) 0.038(6) Uani 0.203(4) 1 d . U P A 2 H34A H 0.3485 0.6570 0.5933 0.057 Uiso 0.203(4) 1 calc GR . P A 2 H34B H 0.2723 0.5691 0.5983 0.057 Uiso 0.203(4) 1 calc GR . P A 2 H34C H 0.4065 0.5609 0.5998 0.057 Uiso 0.203(4) 1 calc GR . P A 2 C33A C 0.378(3) 0.435(2) 0.6943(11) 0.035(5) Uani 0.203(4) 1 d . U P A 2 H33A H 0.3029 0.4086 0.6922 0.053 Uiso 0.203(4) 1 calc GR . P A 2 H33B H 0.4229 0.4031 0.7237 0.053 Uiso 0.203(4) 1 calc GR . P A 2 H33C H 0.4149 0.4317 0.6554 0.053 Uiso 0.203(4) 1 calc GR . P A 2 C32A C 0.360(4) 0.497(3) 0.8271(12) 0.038(5) Uani 0.203(4) 1 d . U P A 2 H32A H 0.3595 0.4337 0.8148 0.058 Uiso 0.203(4) 1 calc GR . P A 2 H32B H 0.2938 0.5087 0.8520 0.058 Uiso 0.203(4) 1 calc GR . P A 2 H32C H 0.4284 0.5090 0.8496 0.058 Uiso 0.203(4) 1 calc GR . P A 2 C31A C 0.3006(18) 0.6998(15) 0.8411(9) 0.051(5) Uani 0.203(4) 1 d . U P A 2 H31A H 0.3720 0.7221 0.8567 0.076 Uiso 0.203(4) 1 calc GR . P A 2 H31B H 0.2634 0.6624 0.8711 0.076 Uiso 0.203(4) 1 calc GR . P A 2 H31C H 0.2519 0.7504 0.8312 0.076 Uiso 0.203(4) 1 calc GR . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0216(17) 0.0301(16) 0.0229(16) -0.0006(12) 0.0029(12) 0.0000(13) C2 0.0206(17) 0.0239(15) 0.0255(16) 0.0033(12) 0.0027(12) 0.0011(12) C3 0.0221(17) 0.0257(16) 0.0232(16) 0.0004(12) 0.0008(12) 0.0004(12) C4 0.0196(16) 0.0278(16) 0.0237(16) 0.0006(12) 0.0020(12) 0.0024(12) C5 0.0239(18) 0.0301(16) 0.0237(16) 0.0041(13) 0.0025(12) 0.0037(13) C6 0.0213(17) 0.0235(15) 0.0346(18) 0.0041(13) 0.0040(12) 0.0025(13) C7 0.0264(18) 0.0217(15) 0.0323(17) -0.0026(13) 0.0009(13) -0.0006(13) C8 0.0228(17) 0.0280(16) 0.0282(17) -0.0039(13) 0.0001(12) 0.0001(13) C9 0.036(2) 0.0405(19) 0.0272(19) -0.0012(15) 0.0075(14) -0.0104(15) C10 0.037(2) 0.064(3) 0.047(3) -0.014(2) 0.0071(18) -0.0178(19) C11 0.035(3) 0.058(3) 0.078(4) 0.011(2) 0.009(2) -0.0011(19) C12 0.044(2) 0.0369(19) 0.0290(19) -0.0057(15) 0.0044(15) -0.0102(16) C13 0.063(3) 0.065(3) 0.034(2) -0.018(2) 0.0127(19) -0.024(2) C14 0.052(3) 0.053(2) 0.038(2) -0.0100(19) -0.0032(18) -0.012(2) C15 0.042(2) 0.0314(18) 0.0294(19) 0.0002(14) -0.0035(15) -0.0025(15) C16 0.080(3) 0.040(2) 0.037(2) 0.0073(18) -0.003(2) 0.000(2) C17 0.044(2) 0.043(2) 0.050(3) -0.0033(18) -0.0074(18) 0.0061(18) C18 0.031(2) 0.044(2) 0.031(2) -0.0021(15) -0.0047(14) -0.0004(15) C19 0.032(2) 0.094(3) 0.058(3) 0.019(3) -0.0021(19) -0.010(2) C20 0.049(3) 0.054(2) 0.072(3) -0.013(2) -0.015(2) 0.015(2) C21 0.049(2) 0.038(2) 0.0276(19) 0.0020(15) 0.0034(15) -0.0049(17) C22 0.092(4) 0.075(3) 0.027(2) 0.009(2) -0.001(2) -0.025(3) C23 0.057(3) 0.063(3) 0.052(3) 0.002(2) 0.021(2) -0.012(2) C24 0.053(2) 0.0302(18) 0.030(2) 0.0002(15) 0.0047(16) 0.0056(16) C25 0.116(5) 0.043(3) 0.077(4) -0.026(2) -0.037(3) 0.014(3) C26 0.073(3) 0.058(3) 0.086(4) -0.001(3) 0.003(3) 0.029(2) P1 0.0208(7) 0.0436(9) 0.0424(8) -0.0097(7) 0.0052(5) -0.0010(6) C27 0.015(3) 0.036(3) 0.045(4) 0.009(2) 0.005(3) -0.006(2) C28 0.023(3) 0.029(2) 0.059(4) -0.003(3) 0.007(3) -0.0070(19) C29 0.020(4) 0.041(4) 0.046(3) -0.010(3) 0.002(2) -0.011(3) C30 0.015(4) 0.033(3) 0.038(3) -0.004(2) -0.002(3) -0.004(3) C31 0.042(4) 0.082(6) 0.071(5) 0.042(5) -0.002(5) -0.021(5) C32 0.032(4) 0.036(3) 0.140(8) -0.019(4) 0.004(6) -0.009(2) C33 0.051(6) 0.097(9) 0.053(4) -0.028(4) 0.002(4) -0.026(7) C34 0.045(4) 0.070(4) 0.072(4) 0.029(3) -0.016(3) -0.002(3) C35 0.042(3) 0.049(3) 0.181(6) -0.030(3) 0.014(3) 0.007(2) C36 0.043(3) 0.039(2) 0.155(6) -0.026(3) 0.012(3) 0.0019(19) C37 0.038(2) 0.0305(19) 0.069(3) -0.0101(19) 0.0118(19) -0.0015(16) C38 0.038(2) 0.0290(18) 0.051(2) -0.0005(16) 0.0033(17) -0.0002(15) O1 0.0251(14) 0.0265(12) 0.0609(18) -0.0090(11) -0.0007(11) 0.0011(10) Si1 0.0294(5) 0.0290(5) 0.0217(5) -0.0014(4) 0.0023(4) -0.0053(4) Si2 0.0295(5) 0.0280(4) 0.0215(5) 0.0009(4) 0.0005(4) -0.0005(4) U1 0.01742(7) 0.02253(7) 0.02833(7) 0.00000(5) 0.00124(4) 0.00002(5) P1A 0.025(5) 0.057(6) 0.040(4) -0.002(4) 0.002(3) -0.001(4) C30A 0.029(16) 0.053(7) 0.035(6) -0.002(5) 0.002(6) -0.001(7) C29A 0.011(10) 0.049(6) 0.032(7) -0.005(5) 0.005(6) -0.006(5) C28A 0.017(12) 0.049(7) 0.035(6) -0.003(5) 0.004(6) 0.002(6) C27A 0.074(18) 0.061(8) 0.033(6) -0.008(5) -0.002(6) 0.027(8) C34A 0.042(16) 0.037(12) 0.035(6) -0.001(6) 0.003(6) -0.007(12) C33A 0.014(10) 0.048(7) 0.044(11) -0.006(6) 0.008(9) -0.004(6) C32A 0.024(12) 0.058(10) 0.033(8) -0.002(7) 0.002(8) 0.003(9) C31A 0.040(12) 0.070(11) 0.042(7) -0.016(8) 0.009(7) 0.013(9) 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' P P 0.1023 0.0942 '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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 Si1 112.7(2) C2 C1 U1 73.39(18) C8 C1 C2 129.8(3) C8 C1 Si1 117.0(2) C8 C1 U1 73.23(18) Si1 C1 U1 140.18(16) C1 C2 H2 108.9 C1 C2 U1 76.30(18) C3 C2 C1 138.1(3) C3 C2 H2 108.9 C3 C2 U1 74.90(17) U1 C2 H2 108.9 C2 C3 H3 108.2 C2 C3 C4 138.5(3) C2 C3 U1 74.85(18) C4 C3 H3 108.2 C4 C3 U1 75.54(18) U1 C3 H3 108.2 C3 C4 Si2 113.9(2) C3 C4 U1 73.82(18) C5 C4 C3 129.3(3) C5 C4 Si2 116.3(2) C5 C4 U1 72.68(18) Si2 C4 U1 140.02(15) C4 C5 H5 110.8 C4 C5 U1 76.85(18) C6 C5 C4 135.9(3) C6 C5 H5 110.8 C6 C5 U1 75.15(18) U1 C5 H5 110.8 C5 C6 H6 109.8 C5 C6 U1 74.28(17) C7 C6 C5 136.0(3) C7 C6 H6 109.8 C7 C6 U1 74.97(18) U1 C6 H6 109.8 C6 C7 H7 109.9 C6 C7 U1 74.58(18) C8 C7 C6 136.1(3) C8 C7 H7 109.9 C8 C7 U1 75.15(18) U1 C7 H7 109.9 C1 C8 H8 110.4 C1 C8 U1 76.64(18) C7 C8 C1 136.0(3) C7 C8 H8 110.4 C7 C8 U1 74.49(18) U1 C8 H8 110.4 C10 C9 H9 105.8 C10 C9 Si1 116.9(3) C11 C9 H9 105.8 C11 C9 C10 109.9(4) C11 C9 Si1 111.8(3) Si1 C9 H9 105.8 C9 C10 H10A 109.5 C9 C10 H10B 109.5 C9 C10 H10C 109.5 H10A C10 H10B 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C9 C11 H11A 109.5 C9 C11 H11B 109.5 C9 C11 H11C 109.5 H11A C11 H11B 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C13 C12 H12 105.7 C13 C12 Si1 114.5(3) C14 C12 H12 105.7 C14 C12 C13 109.3(3) C14 C12 Si1 115.0(3) Si1 C12 H12 105.7 C12 C13 H13A 109.5 C12 C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C12 C14 H14A 109.5 C12 C14 H14B 109.5 C12 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C16 C15 H15 106.4 C16 C15 Si1 112.8(3) C17 C15 H15 106.4 C17 C15 C16 110.5(3) C17 C15 Si1 113.9(2) Si1 C15 H15 106.4 C15 C16 H16A 109.5 C15 C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C15 C17 H17A 109.5 C15 C17 H17B 109.5 C15 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C19 C18 H18 106.7 C19 C18 Si2 113.6(3) C20 C18 H18 106.7 C20 C18 C19 110.3(4) C20 C18 Si2 112.2(3) Si2 C18 H18 106.7 C18 C19 H19A 109.5 C18 C19 H19B 109.5 C18 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C18 C20 H20A 109.5 C18 C20 H20B 109.5 C18 C20 H20C 109.5 H20A C20 H20B 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C22 C21 H21 105.6 C22 C21 Si2 113.7(3) C23 C21 H21 105.6 C23 C21 C22 110.0(3) C23 C21 Si2 115.4(3) Si2 C21 H21 105.6 C21 C22 H22A 109.5 C21 C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C21 C23 H23A 109.5 C21 C23 H23B 109.5 C21 C23 H23C 109.5 H23A C23 H23B 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C25 C24 H24 106.4 C25 C24 Si2 113.5(3) C26 C24 H24 106.4 C26 C24 C25 109.6(4) C26 C24 Si2 114.1(3) Si2 C24 H24 106.4 C24 C25 H25A 109.5 C24 C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25B 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C24 C26 H26A 109.5 C24 C26 H26B 109.5 C24 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C27 P1 U1 70.1(3) C30 P1 C27 101.8(4) C30 P1 U1 74.1(4) P1 C27 U1 75.4(3) C28 C27 P1 113.0(6) C28 C27 C31 124.5(7) C28 C27 U1 75.9(4) C31 C27 P1 122.2(5) C31 C27 U1 122.0(6) C27 C28 C29 113.2(8) C27 C28 C32 123.2(6) C27 C28 U1 76.3(5) C29 C28 C32 123.0(8) C29 C28 U1 73.7(6) C32 C28 U1 124.8(6) C28 C29 C30 110.3(11) C28 C29 C33 124.8(9) C28 C29 U1 77.3(7) C30 C29 U1 76.6(7) C33 C29 C30 124.2(9) C33 C29 U1 120.8(9) P1 C30 C29 101.5(7) P1 C30 U1 73.8(4) C29 C30 U1 68.0(6) C34 C30 P1 149.0(7) C34 C30 C29 109.4(9) C34 C30 U1 116.8(7) C27 C31 H31D 109.5 C27 C31 H31E 109.5 C27 C31 H31F 109.5 H31D C31 H31E 109.5 H31D C31 H31F 109.5 H31E C31 H31F 109.5 C28 C32 H32D 109.5 C28 C32 H32E 109.5 C28 C32 H32F 109.5 H32D C32 H32E 109.5 H32D C32 H32F 109.5 H32E C32 H32F 109.5 C29 C33 H33D 109.5 C29 C33 H33E 109.5 C29 C33 H33F 109.5 H33D C33 H33E 109.5 H33D C33 H33F 109.5 H33E C33 H33F 109.5 C30 C34 H34D 109.5 C30 C34 H34E 109.5 C30 C34 H34F 109.5 H34D C34 H34E 109.5 H34D C34 H34F 109.5 H34E C34 H34F 109.5 H35A C35 H35B 108.3 C36 C35 H35A 109.8 C36 C35 H35B 109.8 C36 C35 O1 109.3(4) O1 C35 H35A 109.8 O1 C35 H35B 109.8 C35 C36 H36A 110.4 C35 C36 H36B 110.4 C35 C36 C37 106.4(4) H36A C36 H36B 108.6 C37 C36 H36A 110.4 C37 C36 H36B 110.4 C36 C37 H37A 111.1 C36 C37 H37B 111.1 C36 C37 C38 103.2(3) H37A C37 H37B 109.1 C38 C37 H37A 111.1 C38 C37 H37B 111.1 C37 C38 H38A 110.3 C37 C38 H38B 110.3 H38A C38 H38B 108.5 O1 C38 C37 107.3(3) O1 C38 H38A 110.3 O1 C38 H38B 110.3 C35 O1 C38 106.9(3) C35 O1 U1 127.4(3) C38 O1 U1 125.6(2) C1 Si1 C12 110.54(15) C9 Si1 C1 109.30(16) C9 Si1 C12 105.70(16) C9 Si1 C15 108.23(17) C15 Si1 C1 110.56(15) C15 Si1 C12 112.34(17) C4 Si2 C24 111.19(15) C18 Si2 C4 108.11(16) C18 Si2 C21 106.44(17) C18 Si2 C24 107.74(17) C21 Si2 C4 110.22(15) C21 Si2 C24 112.89(17) C1 U1 P1A 121.2(3) C1 U1 C28A 139.9(7) C1 U1 C27A 158.4(6) C2 U1 C1 30.31(9) C2 U1 C3 30.25(9) C2 U1 C4 58.70(9) C2 U1 O1 79.46(9) C2 U1 P1A 140.1(3) C2 U1 C28A 163.4(7) C2 U1 C27A 167.1(7) C3 U1 C1 58.17(10) C3 U1 C4 30.65(9) C3 U1 O1 78.16(8) C3 U1 P1A 159.2(3) C3 U1 C28A 144.6(8) C3 U1 C27A 143.4(6) C4 U1 C1 80.86(10) C4 U1 P1A 157.8(3) C4 U1 C28A 113.9(8) C4 U1 C27A 119.6(6) C5 U1 C1 88.29(10) C5 U1 C2 78.36(10) C5 U1 C3 57.35(9) C5 U1 C4 30.47(9) C5 U1 C6 30.58(10) C5 U1 C7 58.44(10) C5 U1 C8 79.76(10) C5 U1 O1 122.67(9) C5 U1 P1A 140.7(3) C5 U1 C28A 89.2(8) C5 U1 C27A 106.1(6) C6 U1 C1 78.85(9) C6 U1 C2 84.81(10) C6 U1 C3 76.76(10) C6 U1 C4 58.03(9) C6 U1 C7 30.45(10) C6 U1 C8 58.20(10) C6 U1 O1 152.24(9) C6 U1 P1A 124.1(3) C6 U1 C28A 78.9(8) C6 U1 C27A 105.2(7) C7 U1 C1 57.67(9) C7 U1 C2 76.61(9) C7 U1 C3 84.48(10) C7 U1 C4 79.07(10) C7 U1 C8 30.36(9) C7 U1 O1 155.14(9) C7 U1 P1A 113.3(2) C7 U1 C28A 87.5(7) C7 U1 C27A 116.1(7) C8 U1 C1 30.13(9) C8 U1 C2 56.83(9) C8 U1 C3 77.54(10) C8 U1 C4 88.08(10) C8 U1 O1 126.66(9) C8 U1 P1A 112.0(2) C8 U1 C28A 110.4(7) C8 U1 C27A 135.4(6) O1 U1 C1 97.78(9) O1 U1 C4 94.21(8) O1 U1 P1A 81.5(2) O1 U1 C28A 116.9(7) O1 U1 C27A 88.1(7) P1A U1 C28A 51.5(9) C27A U1 P1A 38.9(6) C27A U1 C28A 28.8(9) C30A P1A U1 82(4) C30A P1A C29A 32(3) C30A P1A C27A 101(3) C29A P1A U1 69.6(11) C27A P1A U1 70.5(11) C27A P1A C29A 69.2(12) P1A C30A U1 74(4) P1A C30A C29A 121(6) P1A C30A C34A 122(4) C29A C30A U1 77(3) C29A C30A C34A 117(4) C34A C30A U1 118(4) P1A C29A U1 65.4(11) C30A C29A U1 77(3) C30A C29A P1A 27(3) C30A C29A C28A 110(4) C30A C29A C33A 130(4) C28A C29A U1 74(2) C28A C29A P1A 83(2) C28A C29A C33A 117(3) C33A C29A U1 129(2) C33A C29A P1A 156(2) C29A C28A U1 78(2) C29A C28A C27A 111(3) C29A C28A C32A 133(3) C27A C28A U1 74(2) C27A C28A C32A 116(3) C32A C28A U1 122(3) P1A C27A U1 70.5(11) C28A C27A U1 77(2) C28A C27A P1A 96(2) C28A C27A C31A 134(3) C31A C27A U1 113.1(18) C31A C27A P1A 130(2) C30A C34A H34A 109.5 C30A C34A H34B 109.5 C30A C34A H34C 109.5 H34A C34A H34B 109.5 H34A C34A H34C 109.5 H34B C34A H34C 109.5 C29A C33A H33A 109.5 C29A C33A H33B 109.5 C29A C33A H33C 109.5 H33A C33A H33B 109.5 H33A C33A H33C 109.5 H33B C33A H33C 109.5 C28A C32A H32A 109.5 C28A C32A H32B 109.5 C28A C32A H32C 109.5 H32A C32A H32B 109.5 H32A C32A H32C 109.5 H32B C32A H32C 109.5 C27A C31A H31A 109.5 C27A C31A H31B 109.5 C27A C31A H31C 109.5 H31A C31A H31B 109.5 H31A C31A H31C 109.5 H31B C31A H31C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.428(4) C1 C8 1.419(4) C1 Si1 1.901(3) C1 U1 2.750(3) C2 H2 1.0000 C2 C3 1.415(4) C2 U1 2.712(3) C3 H3 1.0000 C3 C4 1.440(4) C3 U1 2.713(3) C4 C5 1.424(4) C4 Si2 1.899(3) C4 U1 2.735(3) C5 H5 1.0000 C5 C6 1.417(4) C5 U1 2.681(3) C6 H6 1.0000 C6 C7 1.415(5) C6 U1 2.693(3) C7 H7 1.0000 C7 C8 1.415(4) C7 U1 2.697(3) C8 H8 1.0000 C8 U1 2.706(3) C9 H9 1.0000 C9 C10 1.546(5) C9 C11 1.529(5) C9 Si1 1.891(4) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 H12 1.0000 C12 C13 1.551(5) C12 C14 1.530(5) C12 Si1 1.914(4) C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 H15 1.0000 C15 C16 1.548(5) C15 C17 1.527(6) C15 Si1 1.898(4) C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 H18 1.0000 C18 C19 1.541(6) C18 C20 1.537(5) C18 Si2 1.887(4) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 H21 1.0000 C21 C22 1.536(5) C21 C23 1.531(6) C21 Si2 1.898(4) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 H24 1.0000 C24 C25 1.525(6) C24 C26 1.518(7) C24 Si2 1.907(4) C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 P1 C27 1.748(8) P1 C30 1.653(11) P1 U1 2.9859(15) C27 C28 1.395(9) C27 C31 1.531(10) C27 U1 2.901(9) C28 C29 1.439(13) C28 C32 1.496(10) C28 U1 2.896(9) C29 C30 1.782(16) C29 C33 1.496(16) C29 U1 2.849(15) C30 C34 1.375(12) C30 U1 2.989(12) C31 H31D 0.9800 C31 H31E 0.9800 C31 H31F 0.9800 C32 H32D 0.9800 C32 H32E 0.9800 C32 H32F 0.9800 C33 H33D 0.9800 C33 H33E 0.9800 C33 H33F 0.9800 C34 H34D 0.9800 C34 H34E 0.9800 C34 H34F 0.9800 C35 H35A 0.9900 C35 H35B 0.9900 C35 C36 1.438(7) C35 O1 1.445(5) C36 H36A 0.9900 C36 H36B 0.9900 C36 C37 1.481(6) C37 H37A 0.9900 C37 H37B 0.9900 C37 C38 1.508(5) C38 H38A 0.9900 C38 H38B 0.9900 C38 O1 1.448(4) O1 U1 2.717(2) U1 P1A 2.785(15) U1 C28A 2.83(4) U1 C27A 2.78(3) P1A C30A 1.16(6) P1A C29A 2.17(4) P1A C27A 1.86(3) C30A C29A 1.33(5) C30A C34A 1.59(7) C29A C28A 1.39(4) C29A C33A 1.58(4) C28A C27A 1.39(4) C28A C32A 1.48(5) C27A C31A 1.57(3) C34A H34A 0.9800 C34A H34B 0.9800 C34A H34C 0.9800 C33A H33A 0.9800 C33A H33B 0.9800 C33A H33C 0.9800 C32A H32A 0.9800 C32A H32B 0.9800 C32A H32C 0.9800 C31A H31A 0.9800 C31A H31B 0.9800 C31A H31C 0.9800 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C1 C2 C3 C4 -2.3(7) C1 C2 C3 U1 -48.1(4) C2 C1 C8 C7 0.1(6) C2 C1 C8 U1 50.2(3) C2 C3 C4 C5 4.7(6) C2 C3 C4 Si2 176.3(3) C2 C3 C4 U1 -45.6(4) C3 C4 C5 C6 1.0(6) C3 C4 C5 U1 -50.7(3) C3 C4 Si2 C18 -72.5(3) C3 C4 Si2 C21 171.5(2) C3 C4 Si2 C24 45.6(3) C4 C5 C6 C7 -5.1(7) C4 C5 C6 U1 -52.3(4) C5 C4 Si2 C18 100.2(3) C5 C4 Si2 C21 -15.7(3) C5 C4 Si2 C24 -141.7(3) C5 C6 C7 C8 0.9(7) C5 C6 C7 U1 -47.0(4) C6 C7 C8 C1 3.0(7) C6 C7 C8 U1 -47.7(4) C8 C1 C2 C3 -2.5(7) C8 C1 C2 U1 -50.2(3) C10 C9 Si1 C1 -74.2(3) C10 C9 Si1 C12 166.8(3) C10 C9 Si1 C15 46.2(3) C11 C9 Si1 C1 53.6(3) C11 C9 Si1 C12 -65.4(3) C11 C9 Si1 C15 174.1(3) C16 C15 Si1 C1 -177.4(3) C16 C15 Si1 C9 63.0(3) C16 C15 Si1 C12 -53.4(3) C17 C15 Si1 C1 -50.4(3) C17 C15 Si1 C9 -170.1(3) C17 C15 Si1 C12 73.6(3) C19 C18 Si2 C4 61.8(3) C19 C18 Si2 C21 -179.8(3) C19 C18 Si2 C24 -58.5(3) C20 C18 Si2 C4 -64.2(3) C20 C18 Si2 C21 54.2(3) C20 C18 Si2 C24 175.5(3) C22 C21 Si2 C4 168.2(3) C22 C21 Si2 C18 51.2(4) C22 C21 Si2 C24 -66.8(4) C23 C21 Si2 C4 -63.3(3) C23 C21 Si2 C18 179.7(3) C23 C21 Si2 C24 61.7(3) P1 C27 C28 C29 1.9(10) P1 C27 C28 C32 -170.0(7) P1 C27 C28 U1 67.1(5) C27 P1 C30 C29 -2.3(9) C27 P1 C30 C34 179.5(18) C27 P1 C30 U1 -65.1(4) C27 C28 C29 C30 -3.6(12) C27 C28 C29 C33 -174.4(12) C27 C28 C29 U1 66.7(7) C28 C29 C30 P1 3.7(12) C28 C29 C30 C34 -177.3(9) C28 C29 C30 U1 70.8(8) C30 P1 C27 C28 0.6(8) C30 P1 C27 C31 -173.0(8) C30 P1 C27 U1 68.0(5) C31 C27 C28 C29 175.4(10) C31 C27 C28 C32 3.5(14) C31 C27 C28 U1 -119.4(9) C32 C28 C29 C30 168.4(9) C32 C28 C29 C33 -2.4(18) C32 C28 C29 U1 -121.3(8) C33 C29 C30 P1 174.6(11) C33 C29 C30 C34 -6.4(17) C33 C29 C30 U1 -118.4(13) C35 C36 C37 C38 25.9(6) C36 C35 O1 C38 3.5(6) C36 C35 O1 U1 -179.6(4) C36 C37 C38 O1 -24.1(5) C37 C38 O1 C35 13.2(5) C37 C38 O1 U1 -163.8(3) O1 C35 C36 C37 -18.9(7) Si1 C1 C2 C3 -174.2(3) Si1 C1 C2 U1 138.08(19) Si1 C1 C8 C7 171.6(3) Si1 C1 C8 U1 -138.3(2) Si2 C4 C5 C6 -170.4(3) Si2 C4 C5 U1 137.8(2) U1 C1 C2 C3 47.7(4) U1 C1 C8 C7 -50.1(4) U1 C2 C3 C4 45.8(4) U1 C3 C4 C5 50.3(3) U1 C3 C4 Si2 -138.08(19) U1 C4 C5 C6 51.8(4) U1 C4 Si2 C18 -165.6(2) U1 C4 Si2 C21 78.4(3) U1 C4 Si2 C24 -47.5(3) U1 C5 C6 C7 47.2(4) U1 C6 C7 C8 47.9(4) U1 C7 C8 C1 50.7(4) U1 P1 C27 C28 -67.4(6) U1 P1 C27 C31 118.9(8) U1 P1 C30 C29 62.7(7) U1 P1 C30 C34 -115.4(19) U1 C27 C28 C29 -65.2(8) U1 C27 C28 C32 122.9(8) U1 C28 C29 C30 -70.3(9) U1 C28 C29 C33 118.9(14) U1 C29 C30 P1 -67.1(6) U1 C29 C30 C34 111.9(8) U1 P1A C30A C29A 63(6) U1 P1A C30A C34A -113(6) U1 P1A C27A C28A -74(2) U1 P1A C27A C31A 104(3) U1 C30A C29A P1A 61(6) U1 C30A C29A C28A 67(3) U1 C30A C29A C33A -130(4) U1 C29A C28A C27A 67(3) U1 C29A C28A C32A -122(5) U1 C28A C27A P1A 68.4(13) U1 C28A C27A C31A -110(4) P1A C30A C29A U1 -61(6) P1A C30A C29A C28A 6(8) P1A C30A C29A C33A 168(5) P1A C29A C28A U1 -66.2(10) P1A C29A C28A C27A 1(3) P1A C29A C28A C32A 171(4) C30A P1A C27A U1 78(4) C30A P1A C27A C28A 4(4) C30A P1A C27A C31A -178(4) C30A C29A C28A U1 -69(4) C30A C29A C28A C27A -2(5) C30A C29A C28A C32A 169(5) C29A P1A C30A U1 -63(6) C29A P1A C30A C34A -176(11) C29A P1A C27A U1 74.8(12) C29A P1A C27A C28A 1(2) C29A P1A C27A C31A 179(3) C29A C28A C27A U1 -69(3) C29A C28A C27A P1A -1(3) C29A C28A C27A C31A -179(3) C27A P1A C30A U1 -68.5(15) C27A P1A C30A C29A -6(7) C27A P1A C30A C34A 178(5) C34A C30A C29A U1 115(5) C34A C30A C29A P1A 176(11) C34A C30A C29A C28A -178(5) C34A C30A C29A C33A -15(8) C33A C29A C28A U1 126(3) C33A C29A C28A C27A -167(3) C33A C29A C28A C32A 3(6) C32A C28A C27A U1 118(3) C32A C28A C27A P1A -173(3) C32A C28A C27A C31A 8(6)