#------------------------------------------------------------------------------ #$Date: 2017-11-14 10:20:52 +0200 (Tue, 14 Nov 2017) $ #$Revision: 203156 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/80/1548031.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_1548031 loop_ _publ_author_name 'Elizabeth P. Wildman' 'Gabor Balazs' 'Ashley J. Wooles' 'Manfred Scheer' 'Stephen T. Liddle' _publ_section_title ; Thorium-phosphorus triamidoamine complexes containing Th-P single- and multiple-bond interactions ; _journal_name_full 'Nature Communications' _journal_page_first 12884 _journal_paper_doi 10.1038/ncomms12884 _journal_volume 7 _journal_year 2016 _chemical_formula_moiety 'C43 H98 N5 O Si3 Th, C24 H20 B, 2(C4 H8 O)' _chemical_formula_sum 'C75 H134 B N5 O3 Si3 Th' _chemical_formula_weight 1480.98 _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 _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 108.190(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.4228(13) _cell_length_b 21.7375(13) _cell_length_c 20.5577(13) _cell_measurement_reflns_used 8364 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 73.8680 _cell_measurement_theta_min 4.3640 _cell_volume 7821.2(9) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment 'N2 gas' _diffrn_ambient_temperature 120(2) _diffrn_crystal_treatment 'flash frozen in gaseous N2' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1806 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -69.00 -22.00 1.0000 65.0000 omega____ theta____ kappa____ phi______ frames - -38.5000 -38.0000 60.0000 47 #__ type_ start__ end____ width___ exp.time_ 2 omega -49.00 17.00 1.0000 65.0000 omega____ theta____ kappa____ phi______ frames - -38.5000 38.0000 -60.0000 66 #__ type_ start__ end____ width___ exp.time_ 3 omega -43.00 31.00 1.0000 65.0000 omega____ theta____ kappa____ phi______ frames - -38.5000 38.0000 0.0000 74 #__ type_ start__ end____ width___ exp.time_ 4 omega -36.00 33.00 1.0000 65.0000 omega____ theta____ kappa____ phi______ frames - -38.5000 38.0000 -120.0000 69 #__ type_ start__ end____ width___ exp.time_ 5 omega 32.00 86.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 -30.0000 0.0000 54 #__ type_ start__ end____ width___ exp.time_ 6 omega 56.00 91.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 -30.0000 -150.0000 35 #__ type_ start__ end____ width___ exp.time_ 7 omega 40.00 107.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 -95.0000 -120.0000 67 #__ type_ start__ end____ width___ exp.time_ 8 omega 135.00 178.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 125.0000 90.0000 43 #__ type_ start__ end____ width___ exp.time_ 9 omega 96.00 169.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 125.0000 -60.0000 73 #__ type_ start__ end____ width___ exp.time_ 10 omega 32.00 87.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 -30.0000 -90.0000 55 #__ type_ start__ end____ width___ exp.time_ 11 omega 52.00 89.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 -30.0000 -180.0000 37 #__ type_ start__ end____ width___ exp.time_ 12 omega 120.00 149.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 77.0000 -60.0000 29 #__ type_ start__ end____ width___ exp.time_ 13 omega 39.00 151.00 1.0000 260.0000 omega____ theta____ kappa____ phi______ frames - 106.1322 -15.0000 -30.0000 112 #__ type_ start__ end____ width___ exp.time_ 14 omega 16.00 113.00 1.0000 65.0000 omega____ theta____ kappa____ phi______ frames - 43.1277 57.0000 -30.0000 97 #__ type_ start__ end____ width___ exp.time_ 15 omega 1.00 27.00 1.0000 65.0000 omega____ theta____ kappa____ phi______ frames - 43.1277 -99.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 16 omega 12.00 117.00 1.0000 65.0000 omega____ theta____ kappa____ phi______ frames - 43.1277 77.0000 -150.0000 105 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_orient_matrix_UB_11 -0.0518530000 _diffrn_orient_matrix_UB_12 -0.0029472000 _diffrn_orient_matrix_UB_13 0.0460208000 _diffrn_orient_matrix_UB_21 -0.0339010000 _diffrn_orient_matrix_UB_22 -0.0612409000 _diffrn_orient_matrix_UB_23 -0.0339496000 _diffrn_orient_matrix_UB_31 0.0623691000 _diffrn_orient_matrix_UB_32 -0.0355992000 _diffrn_orient_matrix_UB_33 0.0543806000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1812 _diffrn_reflns_av_unetI/netI 0.1910 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 43946 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.965 _diffrn_reflns_theta_min 4.383 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 6.933 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.258 _exptl_crystal_description block _exptl_crystal_F_000 3120 _exptl_crystal_size_max 0.3219 _exptl_crystal_size_mid 0.042 _exptl_crystal_size_min 0.0297 _refine_diff_density_max 3.834 _refine_diff_density_min -3.188 _refine_diff_density_rms 0.185 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 789 _refine_ls_number_reflns 15597 _refine_ls_number_restraints 221 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.1460 _refine_ls_R_factor_gt 0.0888 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+13.3083P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1983 _refine_ls_wR_factor_ref 0.2472 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8954 _reflns_number_total 15597 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ncomms12884-s7.cif _cod_data_source_block SI-1 _cod_database_code 1548031 _chemical_oxdiff_formula 'C75 H134 N5 Th B Si3 O3' _chemical_oxdiff_usercomment 'THEPWA #15096 SN-689 FOR EPW/STL ON MICROMOUNT IN FOMBLIN OIL' _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. ; _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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. Restrained distances O2-C71 \\sim O2-C68 with sigma of 0.02 C71-C70 \\sim C69-C68 with sigma of 0.02 O2-C71 \\sim O2-C68 with sigma of 0.02 C71-C70 \\sim C69-C68 with sigma of 0.02 3. Rigid body (RIGU) restrains C16, C17, C15, Si2, C20, C19, C18, C14, C13, C12 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 Si2, C17, C15, C16, C12, C14, C13, C18, C20, C19 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 Si1, Si3, C1, C2, C3, C6, C4, C5, C7, C9, C8, C23, C24, C25, C26, C27, C28, C29, C30, C31, O2, C68, C69, C70, C71 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Ternary CH refined with riding coordinates: C3(H3), C5(H5), C8(H8), C14(H14), C17(H17), C20(H20), C25(H25), C28(H28), C31(H31) 4.b Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A, H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C42(H42A,H42B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C1AA(H1AA,H1AB), C2AA(H2AA, H2AB), C4AA(H4AA,H4AB), C3AA(H3AA,H3AB) 4.c Aromatic/amide H refined with riding coordinates: C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67) 4.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C7(H7A, H7B,H7C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A, H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B, H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C41(H41A, H41B,H41C), C43(H43A,H43B,H43C) ; _shelx_res_file ; thepwa.res created by SHELXL-2014/7 TITL thepwa_a.res in P2(1)/n REM Old TITL THEPWA in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.186, Rweak 0.022, Alpha 0.114, Orientation as input REM Formula found by SHELXT: C65 B N16 O2 Si3 Th CELL 1.54184 18.422786 21.737475 20.557736 90 108.1905 90 ZERR 4 0.001308 0.001288 0.001336 0 0.0068 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H B N O Si Th UNIT 300 536 4 20 12 12 4 SADI O2 C71 O2 C68 SADI C71 C70 C69 C68 SADI O2 C71 O2 C68 SADI C71 C70 C69 C68 RIGU Si1 Si3 C1 C2 C3 C6 C4 C5 C7 C9 C8 C23 C24 C25 C26 C27 C28 C29 C30 C31 = O2 C68 C69 C70 C71 RIGU C16 C17 C15 Si2 C20 C19 C18 C14 C13 C12 RIGU Si2 C17 C15 C16 C12 C14 C13 C18 C20 C19 L.S. 16 PLAN 40 TEMP -153(2) BOND $H LIST 6 MORE -1 CONF fmap 2 acta OMIT 1 0 1 OMIT -1 1 1 OMIT 1 1 0 OMIT 0 1 1 OMIT 0 2 0 OMIT -16 17 4 REM REM REM WGHT 0.064800 13.308301 FVAR 0.17836 TH1 7 0.162969 0.319022 0.818215 11.00000 0.03980 0.02658 = 0.03749 -0.00223 0.01680 -0.00184 SI1 6 0.297440 0.399450 0.962871 11.00000 0.05358 0.03519 = 0.03990 -0.00018 0.00368 -0.00094 SI2 6 0.128114 0.152904 0.801681 11.00000 0.04816 0.02602 = 0.05085 -0.00343 0.01426 -0.00213 SI3 6 0.053644 0.415360 0.675845 11.00000 0.05150 0.03323 = 0.04417 -0.00021 0.00480 -0.00294 O1 5 0.257813 0.301912 0.779849 11.00000 0.03536 0.04731 = 0.06089 -0.00696 0.03380 -0.00805 N1 4 0.203249 0.384520 0.914672 11.00000 0.03811 0.04035 = 0.03903 -0.00475 0.01511 0.00971 N2 4 0.121888 0.221723 0.842750 11.00000 0.04151 0.03398 = 0.03788 0.00148 0.02165 -0.00363 N3 4 0.058771 0.366494 0.743439 11.00000 0.01729 0.03071 = 0.07907 -0.00251 0.00676 -0.01519 N4 4 0.054553 0.330330 0.878468 11.00000 0.05492 0.03588 = 0.03775 -0.00439 0.03152 -0.00607 N5 4 0.544366 0.287097 0.708196 11.00000 0.03534 0.04891 = 0.02164 -0.00698 0.00043 -0.00569 C1 1 0.328370 0.459780 0.850530 11.00000 0.10342 0.10856 = 0.10322 0.02030 0.05630 -0.00558 AFIX 137 H1A 2 0.272399 0.459521 0.833579 11.00000 -1.50000 H1B 2 0.348486 0.454471 0.812025 11.00000 -1.50000 H1C 2 0.346196 0.499076 0.873284 11.00000 -1.50000 AFIX 0 C2 1 0.442214 0.417658 0.935795 11.00000 0.07211 0.21333 = 0.12861 -0.00972 0.02029 -0.02790 AFIX 137 H2A 2 0.452416 0.461962 0.940234 11.00000 -1.50000 H2B 2 0.470702 0.399269 0.907624 11.00000 -1.50000 H2C 2 0.458338 0.398647 0.981293 11.00000 -1.50000 AFIX 0 C3 1 0.356650 0.406882 0.901819 11.00000 0.06425 0.07466 = 0.05412 -0.01892 0.01563 -0.01373 AFIX 13 H3 2 0.350653 0.367780 0.875027 11.00000 -1.20000 AFIX 0 C6 1 0.281802 0.527378 0.987134 11.00000 0.09459 0.05068 = 0.10406 -0.01760 0.03873 -0.01493 AFIX 137 H6A 2 0.315752 0.539308 0.960883 11.00000 -1.50000 H6B 2 0.283424 0.558891 1.021651 11.00000 -1.50000 H6C 2 0.229430 0.523421 0.956146 11.00000 -1.50000 AFIX 0 C4 1 0.388260 0.472407 1.075053 11.00000 0.09384 0.10703 = 0.09555 -0.05109 0.00894 -0.00145 AFIX 137 H4A 2 0.398975 0.434932 1.102932 11.00000 -1.50000 H4B 2 0.390316 0.508116 1.104675 11.00000 -1.50000 H4C 2 0.426483 0.477094 1.051264 11.00000 -1.50000 AFIX 0 C5 1 0.307171 0.467761 1.021443 11.00000 0.07917 0.05056 = 0.07641 -0.02428 0.02099 -0.01882 AFIX 13 H5 2 0.271805 0.459292 1.048690 11.00000 -1.20000 AFIX 0 C7 1 0.306247 0.317620 1.072821 11.00000 0.13865 0.08838 = 0.06447 0.01525 0.01612 0.00122 AFIX 137 H7A 2 0.328388 0.346146 1.110754 11.00000 -1.50000 H7B 2 0.317989 0.275231 1.088898 11.00000 -1.50000 H7C 2 0.250716 0.323242 1.055848 11.00000 -1.50000 AFIX 0 C9 1 0.326351 0.273606 0.969062 11.00000 0.13377 0.06776 = 0.09205 0.00190 0.00871 0.01521 AFIX 137 H9A 2 0.271352 0.266593 0.948671 11.00000 -1.50000 H9B 2 0.349900 0.237509 0.995989 11.00000 -1.50000 H9C 2 0.349370 0.280524 0.932666 11.00000 -1.50000 AFIX 0 C8 1 0.339554 0.330298 1.015833 11.00000 0.10627 0.05910 = 0.05828 0.01166 -0.00022 0.01107 AFIX 13 H8 2 0.395841 0.336792 1.036343 11.00000 -1.20000 AFIX 0 C10 1 0.143432 0.409608 0.937790 11.00000 0.05988 0.04366 = 0.05045 -0.02507 0.03018 -0.00975 AFIX 23 H10A 2 0.115906 0.441675 0.905185 11.00000 -1.20000 H10B 2 0.166434 0.429458 0.982891 11.00000 -1.20000 AFIX 0 C11 1 0.088279 0.362371 0.943985 11.00000 0.05649 0.06319 = 0.05258 -0.01694 0.02218 -0.01238 AFIX 23 H11A 2 0.114566 0.332203 0.979635 11.00000 -1.20000 H11B 2 0.047252 0.382113 0.958262 11.00000 -1.20000 AFIX 0 C12 1 0.148175 0.124047 0.669528 11.00000 0.12623 0.04582 = 0.06095 -0.00097 0.04611 0.01201 AFIX 137 H12A 2 0.198431 0.108283 0.696393 11.00000 -1.50000 H12B 2 0.151037 0.140848 0.626159 11.00000 -1.50000 H12C 2 0.110760 0.090523 0.660196 11.00000 -1.50000 AFIX 0 C13 1 0.045484 0.198540 0.667314 11.00000 0.08693 0.03851 = 0.04824 -0.01558 0.00154 0.00014 AFIX 137 H13A 2 0.007109 0.166345 0.663372 11.00000 -1.50000 H13B 2 0.046820 0.209844 0.621553 11.00000 -1.50000 H13C 2 0.032224 0.234750 0.689665 11.00000 -1.50000 AFIX 0 C14 1 0.123678 0.174728 0.709832 11.00000 0.07445 0.04218 = 0.04290 -0.00663 0.01512 0.00420 AFIX 13 H14 2 0.160348 0.209517 0.713887 11.00000 -1.20000 AFIX 0 C15 1 0.053601 0.033005 0.773020 11.00000 0.08553 0.03509 = 0.09613 -0.01982 0.02454 -0.00580 AFIX 137 H15A 2 0.031308 0.036347 0.723197 11.00000 -1.50000 H15B 2 0.024003 0.003542 0.790565 11.00000 -1.50000 H15C 2 0.106574 0.018773 0.784360 11.00000 -1.50000 AFIX 0 C16 1 -0.032274 0.120736 0.780996 11.00000 0.04774 0.02800 = 0.13835 -0.01024 0.02555 -0.02576 AFIX 137 H16A 2 -0.035150 0.160368 0.802783 11.00000 -1.50000 H16B 2 -0.065746 0.090996 0.793346 11.00000 -1.50000 H16C 2 -0.048676 0.125938 0.731161 11.00000 -1.50000 AFIX 0 C17 1 0.051895 0.096653 0.806045 11.00000 0.05747 0.03886 = 0.05659 -0.01322 0.02156 -0.01318 AFIX 13 H17 2 0.062624 0.088048 0.855950 11.00000 -1.20000 AFIX 0 C18 1 0.230530 0.096916 0.921621 11.00000 0.05981 0.06522 = 0.07129 0.00719 0.01235 0.00380 AFIX 137 H18A 2 0.227784 0.135553 0.945306 11.00000 -1.50000 H18B 2 0.280055 0.077228 0.943308 11.00000 -1.50000 H18C 2 0.189449 0.069413 0.924394 11.00000 -1.50000 AFIX 0 C19 1 0.291439 0.145643 0.837124 11.00000 0.05671 0.06291 = 0.08201 0.00493 0.01373 -0.00458 AFIX 137 H19A 2 0.292900 0.143154 0.789951 11.00000 -1.50000 H19B 2 0.337874 0.127104 0.868152 11.00000 -1.50000 H19C 2 0.288409 0.188861 0.849601 11.00000 -1.50000 AFIX 0 C20 1 0.221208 0.110909 0.842867 11.00000 0.05337 0.03733 = 0.06238 -0.00298 0.00912 0.00202 AFIX 13 H20 2 0.218620 0.070562 0.818879 11.00000 -1.20000 AFIX 0 C21 1 0.092963 0.222829 0.900125 11.00000 0.06529 0.03093 = 0.06004 0.00533 0.01232 -0.00311 AFIX 23 H21A 2 0.134477 0.234684 0.941951 11.00000 -1.20000 H21B 2 0.075158 0.181175 0.907370 11.00000 -1.20000 AFIX 0 C22 1 0.027136 0.268240 0.888016 11.00000 0.05648 0.02939 = 0.07033 -0.01298 0.03696 -0.01460 AFIX 23 H22A 2 -0.015068 0.256109 0.846823 11.00000 -1.20000 H22B 2 0.007573 0.268123 0.927728 11.00000 -1.20000 AFIX 0 C23 1 0.133265 0.515710 0.757983 11.00000 0.10993 0.04938 = 0.08631 -0.02399 0.01226 0.00455 AFIX 137 H23A 2 0.134647 0.493539 0.799860 11.00000 -1.50000 H23B 2 0.135865 0.560075 0.766897 11.00000 -1.50000 H23C 2 0.176902 0.503202 0.743407 11.00000 -1.50000 AFIX 0 C24 1 -0.009434 0.518839 0.727738 11.00000 0.12275 0.04997 = 0.08970 0.01458 0.03667 0.02300 AFIX 137 H24A 2 -0.057633 0.506634 0.693709 11.00000 -1.50000 H24B 2 -0.009246 0.563444 0.734716 11.00000 -1.50000 H24C 2 -0.004198 0.497813 0.771135 11.00000 -1.50000 AFIX 0 C25 1 0.059075 0.500622 0.701558 11.00000 0.09430 0.04252 = 0.06752 0.00061 0.01838 0.00575 AFIX 13 H25 2 0.056470 0.526164 0.660433 11.00000 -1.20000 AFIX 0 C26 1 -0.040704 0.443204 0.540960 11.00000 0.09241 0.12145 = 0.08054 0.03010 -0.02303 -0.01952 AFIX 137 H26A 2 -0.033172 0.487025 0.552249 11.00000 -1.50000 H26B 2 -0.090661 0.437163 0.506423 11.00000 -1.50000 H26C 2 -0.000414 0.428758 0.522862 11.00000 -1.50000 AFIX 0 C27 1 -0.059979 0.342510 0.580654 11.00000 0.08457 0.08505 = 0.07567 -0.00261 -0.01630 -0.02582 AFIX 137 H27A 2 -0.027769 0.327675 0.553966 11.00000 -1.50000 H27B 2 -0.113663 0.341728 0.552110 11.00000 -1.50000 H27C 2 -0.053140 0.315913 0.620616 11.00000 -1.50000 AFIX 0 C28 1 -0.037441 0.407525 0.604174 11.00000 0.07763 0.08233 = 0.07417 0.00837 -0.01278 -0.01269 AFIX 13 H28 2 -0.078811 0.424166 0.621167 11.00000 -1.20000 AFIX 0 C29 1 0.167772 0.451908 0.612018 11.00000 0.05458 0.05179 = 0.06435 0.01014 0.00960 -0.00078 AFIX 137 H29A 2 0.132163 0.452026 0.565268 11.00000 -1.50000 H29B 2 0.220000 0.446148 0.610557 11.00000 -1.50000 H29C 2 0.164287 0.491205 0.634220 11.00000 -1.50000 AFIX 0 C30 1 0.145670 0.337006 0.619282 11.00000 0.09776 0.04801 = 0.04177 -0.00308 0.02297 -0.00586 AFIX 137 H30A 2 0.139099 0.305055 0.650608 11.00000 -1.50000 H30B 2 0.193776 0.330167 0.609441 11.00000 -1.50000 H30C 2 0.102989 0.335304 0.576538 11.00000 -1.50000 AFIX 0 C31 1 0.147449 0.399829 0.652267 11.00000 0.06700 0.05034 = 0.03974 -0.00305 0.01403 -0.00850 AFIX 13 H31 2 0.189704 0.398002 0.696774 11.00000 -1.20000 AFIX 0 C32 1 -0.014814 0.353321 0.757489 11.00000 0.05556 0.03443 = 0.04729 0.00276 0.02126 0.00322 AFIX 23 H32A 2 -0.029287 0.309789 0.746473 11.00000 -1.20000 H32B 2 -0.055834 0.379542 0.727826 11.00000 -1.20000 AFIX 0 C33 1 -0.007079 0.365567 0.831500 11.00000 0.05199 0.02514 = 0.09292 -0.00123 0.04081 -0.00380 AFIX 23 H33A 2 0.002570 0.409975 0.841035 11.00000 -1.20000 H33B 2 -0.055792 0.355123 0.839715 11.00000 -1.20000 AFIX 0 C34 1 0.314992 0.285332 0.749344 11.00000 0.05815 0.05417 = 0.04957 0.02359 0.02200 0.00269 AFIX 23 H34A 2 0.291069 0.263309 0.705746 11.00000 -1.20000 H34B 2 0.352819 0.257527 0.780361 11.00000 -1.20000 AFIX 0 C35 1 0.354931 0.343266 0.735874 11.00000 0.06942 0.05956 = 0.05673 0.00193 0.03536 0.00278 AFIX 23 H35A 2 0.316022 0.372997 0.709710 11.00000 -1.20000 H35B 2 0.383276 0.362575 0.780134 11.00000 -1.20000 AFIX 0 C36 1 0.409076 0.329717 0.696821 11.00000 0.03170 0.06130 = 0.06267 -0.00891 0.00994 0.00186 AFIX 23 H36A 2 0.432394 0.368827 0.688686 11.00000 -1.20000 H36B 2 0.379807 0.312596 0.651614 11.00000 -1.20000 AFIX 0 C37 1 0.472921 0.284768 0.732234 11.00000 0.04791 0.05435 = 0.03463 0.00280 0.01472 -0.00996 AFIX 23 H37A 2 0.451897 0.242506 0.725018 11.00000 -1.20000 H37B 2 0.489034 0.293001 0.782076 11.00000 -1.20000 AFIX 0 C38 1 0.575890 0.351363 0.718331 11.00000 0.03761 0.04815 = 0.04109 -0.00552 0.00474 -0.00183 AFIX 23 H38A 2 0.625094 0.351120 0.708342 11.00000 -1.20000 H38B 2 0.540450 0.378055 0.683675 11.00000 -1.20000 AFIX 0 C39 1 0.589208 0.380610 0.786639 11.00000 0.06454 0.05078 = 0.04351 -0.00761 0.01437 -0.00109 AFIX 137 H39A 2 0.615089 0.420175 0.787816 11.00000 -1.50000 H39B 2 0.621186 0.353590 0.822325 11.00000 -1.50000 H39C 2 0.540104 0.387297 0.794693 11.00000 -1.50000 AFIX 0 C40 1 0.518984 0.271748 0.632236 11.00000 0.04680 0.04276 = 0.03246 -0.00136 0.00130 -0.00150 AFIX 23 H40A 2 0.491821 0.231802 0.625050 11.00000 -1.20000 H40B 2 0.482489 0.303534 0.607056 11.00000 -1.20000 AFIX 0 C41 1 0.584279 0.268153 0.603050 11.00000 0.06117 0.09581 = 0.03208 -0.01305 0.01448 0.01989 AFIX 137 H41A 2 0.565041 0.255104 0.555079 11.00000 -1.50000 H41B 2 0.622012 0.238315 0.629260 11.00000 -1.50000 H41C 2 0.608313 0.308699 0.605802 11.00000 -1.50000 AFIX 0 C42 1 0.603867 0.242742 0.750352 11.00000 0.06939 0.02950 = 0.03894 -0.00361 0.00212 -0.00382 AFIX 23 H42A 2 0.614538 0.252842 0.799408 11.00000 -1.20000 H42B 2 0.651796 0.248809 0.739003 11.00000 -1.20000 AFIX 0 C43 1 0.581069 0.175423 0.739567 11.00000 0.07372 0.04536 = 0.04621 -0.00987 -0.00389 0.00520 AFIX 137 H43A 2 0.574667 0.163904 0.692012 11.00000 -1.50000 H43B 2 0.532823 0.169050 0.749308 11.00000 -1.50000 H43C 2 0.621013 0.149897 0.770428 11.00000 -1.50000 AFIX 0 C44 1 0.342029 0.332639 0.480826 11.00000 0.04856 0.02905 = 0.04692 0.00552 -0.00233 0.01302 C45 1 0.321840 0.373741 0.524698 11.00000 0.06619 0.03776 = 0.04124 -0.00538 0.00627 0.00301 AFIX 43 H45 2 0.275319 0.367062 0.534420 11.00000 -1.20000 AFIX 0 C46 1 0.366954 0.424176 0.554885 11.00000 0.10011 0.04803 = 0.03397 -0.00238 -0.00575 0.00538 AFIX 43 H46 2 0.350645 0.450866 0.584179 11.00000 -1.20000 AFIX 0 C47 1 0.435955 0.435447 0.542103 11.00000 0.08955 0.03239 = 0.04593 -0.00340 -0.01455 -0.00642 AFIX 43 H47 2 0.467267 0.469293 0.562865 11.00000 -1.20000 AFIX 0 C48 1 0.457840 0.395728 0.498023 11.00000 0.07222 0.04211 = 0.05020 -0.00854 -0.00320 0.00151 AFIX 43 H48 2 0.503407 0.403304 0.486973 11.00000 -1.20000 AFIX 0 C49 1 0.412272 0.344813 0.470318 11.00000 0.03124 0.04124 = 0.05495 0.01728 0.00338 -0.00347 AFIX 43 H49 2 0.429852 0.316979 0.442906 11.00000 -1.20000 AFIX 0 C50 1 0.293960 0.253731 0.375904 11.00000 0.03404 0.03504 = 0.03180 0.00378 0.00069 -0.00274 C51 1 0.283704 0.192217 0.347519 11.00000 0.04064 0.04178 = 0.03761 -0.00426 0.00396 -0.00666 AFIX 43 H51 2 0.277635 0.159351 0.375839 11.00000 -1.20000 AFIX 0 C52 1 0.282278 0.178835 0.281943 11.00000 0.02841 0.04262 = 0.03960 -0.01015 -0.00711 -0.00166 AFIX 43 H52 2 0.274198 0.137523 0.266269 11.00000 -1.20000 AFIX 0 C53 1 0.292009 0.222616 0.239272 11.00000 0.04355 0.06317 = 0.03883 0.00858 0.02309 0.00031 AFIX 43 H53 2 0.291403 0.211905 0.194304 11.00000 -1.20000 AFIX 0 C54 1 0.302720 0.282200 0.260231 11.00000 0.04882 0.04909 = 0.04270 -0.01228 0.00606 -0.00513 AFIX 43 H54 2 0.309659 0.313182 0.230121 11.00000 -1.20000 AFIX 0 C55 1 0.303432 0.297521 0.326797 11.00000 0.05508 0.04052 = 0.03914 -0.00409 0.00897 -0.00865 AFIX 43 H55 2 0.310628 0.339476 0.340210 11.00000 -1.20000 AFIX 0 C56 1 0.199557 0.278569 0.442007 11.00000 0.06218 0.05197 = 0.03430 -0.00459 0.01014 -0.00571 C57 1 0.153623 0.229787 0.447059 11.00000 0.05741 0.07312 = 0.04889 -0.01179 0.01600 -0.00611 AFIX 43 H57 2 0.176329 0.190345 0.458152 11.00000 -1.20000 AFIX 0 C58 1 0.073172 0.235912 0.436328 11.00000 0.07532 0.09703 = 0.04479 -0.01344 0.03329 -0.03677 AFIX 43 H58 2 0.044175 0.201320 0.441932 11.00000 -1.20000 AFIX 0 C59 1 0.037714 0.292585 0.417707 11.00000 0.05058 0.13714 = 0.04791 -0.00647 0.01306 0.00092 AFIX 43 H59 2 -0.015336 0.297589 0.411092 11.00000 -1.20000 AFIX 0 C60 1 0.082018 0.341523 0.409090 11.00000 0.06657 0.09179 = 0.03727 -0.01017 0.00142 0.03063 AFIX 43 H60 2 0.058469 0.380182 0.394592 11.00000 -1.20000 AFIX 0 C61 1 0.160731 0.335176 0.421300 11.00000 0.05566 0.06143 = 0.04337 -0.00917 0.00294 0.01412 AFIX 43 H61 2 0.189250 0.370012 0.415528 11.00000 -1.20000 AFIX 0 C62 1 0.329988 0.215624 0.506741 11.00000 0.04634 0.03834 = 0.02915 -0.00404 0.00934 0.00666 C63 1 0.310469 0.207636 0.565824 11.00000 0.05037 0.02143 = 0.04475 0.00263 0.02010 -0.00208 AFIX 43 H63 2 0.272404 0.233484 0.573568 11.00000 -1.20000 AFIX 0 C64 1 0.344619 0.162967 0.614609 11.00000 0.04006 0.06595 = 0.03292 0.02277 0.00128 0.00329 AFIX 43 H64 2 0.329568 0.158567 0.654553 11.00000 -1.20000 AFIX 0 C65 1 0.400509 0.125160 0.604402 11.00000 0.05498 0.05542 = 0.04405 0.01382 0.00656 0.00195 AFIX 43 H65 2 0.422710 0.093601 0.636394 11.00000 -1.20000 AFIX 0 C66 1 0.423557 0.133576 0.547877 11.00000 0.05359 0.03462 = 0.04461 -0.00218 0.02030 0.00363 AFIX 43 H66 2 0.462724 0.108093 0.541586 11.00000 -1.20000 AFIX 0 C67 1 0.390631 0.179088 0.498814 11.00000 0.04347 0.04020 = 0.03231 -0.00020 0.01145 -0.00308 AFIX 43 H67 2 0.408757 0.185304 0.460826 11.00000 -1.20000 AFIX 0 B1 3 0.292202 0.270702 0.450876 11.00000 0.02997 0.03782 = 0.03306 0.00227 0.00558 0.01180 O2 5 0.687885 0.418374 0.645650 11.00000 0.09763 0.07702 = 0.14524 0.04219 0.04337 0.00824 C68 1 0.751062 0.419349 0.620255 11.00000 0.12511 0.08154 = 0.17304 0.04532 0.06734 0.01311 AFIX 23 H68A 2 0.745133 0.386999 0.585076 11.00000 -1.20000 H68B 2 0.798908 0.411397 0.657911 11.00000 -1.20000 AFIX 0 C69 1 0.754341 0.480710 0.589997 11.00000 0.11701 0.07651 = 0.13691 0.03296 0.05377 0.00549 AFIX 23 H69A 2 0.807769 0.493638 0.596990 11.00000 -1.20000 H69B 2 0.725911 0.481172 0.540414 11.00000 -1.20000 AFIX 0 C70 1 0.717484 0.519917 0.628395 11.00000 0.11283 0.07292 = 0.08967 0.03817 0.02897 0.01262 AFIX 23 H70A 2 0.695467 0.557345 0.602198 11.00000 -1.20000 H70B 2 0.753725 0.532052 0.673210 11.00000 -1.20000 AFIX 0 C71 1 0.656917 0.478668 0.636874 11.00000 0.10884 0.08418 = 0.12815 0.04880 0.04009 0.01782 AFIX 23 H71A 2 0.642190 0.491019 0.677378 11.00000 -1.20000 H71B 2 0.611068 0.480535 0.595914 11.00000 -1.20000 AFIX 0 O0AA 5 0.127552 0.425479 1.112171 11.00000 0.11988 C1AA 1 0.147170 0.530816 1.107656 11.00000 0.10570 AFIX 23 H1AA 2 0.124861 0.568492 1.120684 11.00000 -1.20000 H1AB 2 0.165878 0.540363 1.068579 11.00000 -1.20000 AFIX 0 C2AA 1 0.091412 0.481101 1.090577 11.00000 0.10551 AFIX 23 H2AA 2 0.051877 0.488248 1.113119 11.00000 -1.20000 H2AB 2 0.065971 0.480041 1.040463 11.00000 -1.20000 AFIX 0 C4AA 1 0.196403 0.438082 1.170693 11.00000 0.12384 AFIX 23 H4AA 2 0.240602 0.414222 1.166729 11.00000 -1.20000 H4AB 2 0.187666 0.427417 1.214472 11.00000 -1.20000 AFIX 0 C3AA 1 0.210028 0.506256 1.166783 11.00000 0.10280 AFIX 23 H3AA 2 0.209735 0.526732 1.209716 11.00000 -1.20000 H3AB 2 0.260151 0.513729 1.159931 11.00000 -1.20000 AFIX 0 HKLF 4 REM thepwa_a.res in P2(1)/n REM R1 = 0.0888 for 8954 Fo > 4sig(Fo) and 0.1460 for all 15597 data REM 789 parameters refined using 221 restraints END WGHT 0.0648 13.3176 REM Highest difference peak 3.834, deepest hole -3.188, 1-sigma level 0.185 Q1 1 0.1303 0.3209 0.7897 11.00000 0.05 3.83 Q2 1 0.1761 0.3175 0.8847 11.00000 0.05 2.49 Q3 1 0.5109 0.3184 0.5502 11.00000 0.05 1.98 Q4 1 0.1639 0.0441 0.8200 11.00000 0.05 1.92 Q5 1 0.2168 0.3426 0.8625 11.00000 0.05 1.73 Q6 1 0.1668 0.3163 0.7559 11.00000 0.05 1.61 Q7 1 0.2150 0.2993 0.8648 11.00000 0.05 1.51 Q8 1 0.1514 0.3617 0.8536 11.00000 0.05 1.31 Q9 1 0.1994 0.2714 0.8571 11.00000 0.05 1.19 Q10 1 0.0607 0.2596 0.7732 11.00000 0.05 1.17 Q11 1 0.2309 0.3532 0.8308 11.00000 0.05 1.15 Q12 1 0.1926 0.3724 0.8598 11.00000 0.05 1.10 Q13 1 0.1438 0.2855 0.8599 11.00000 0.05 1.06 Q14 1 0.1576 0.2740 0.8484 11.00000 0.05 1.06 Q15 1 0.0701 0.3188 0.8217 11.00000 0.05 1.06 Q16 1 0.1807 0.2891 0.7697 11.00000 0.05 1.04 Q17 1 0.1904 0.3527 0.7775 11.00000 0.05 1.04 Q18 1 0.1991 0.3755 0.8247 11.00000 0.05 1.03 Q19 1 0.1314 0.3147 0.8408 11.00000 0.05 1.03 Q20 1 0.1107 0.2192 0.7905 11.00000 0.05 1.02 Q21 1 0.2627 0.3179 0.8300 11.00000 0.05 0.99 Q22 1 0.2732 0.3197 0.8506 11.00000 0.05 0.93 Q23 1 0.0942 0.2892 0.8075 11.00000 0.05 0.92 Q24 1 0.0686 0.3899 0.7807 11.00000 0.05 0.91 Q25 1 0.1265 0.2599 0.8036 11.00000 0.05 0.91 Q26 1 0.0328 0.3208 0.7255 11.00000 0.05 0.89 Q27 1 0.2676 0.2578 0.8583 11.00000 0.05 0.89 Q28 1 0.2316 0.2881 0.8294 11.00000 0.05 0.87 Q29 1 0.2652 0.3800 0.8563 11.00000 0.05 0.87 Q30 1 0.1270 0.3814 0.8081 11.00000 0.05 0.85 Q31 1 0.2810 0.3203 0.7204 11.00000 0.05 0.82 Q32 1 0.0703 0.2579 0.8286 11.00000 0.05 0.81 Q33 1 0.0937 0.3526 0.8068 11.00000 0.05 0.81 Q34 1 0.3726 0.2903 0.7502 11.00000 0.05 0.80 Q35 1 0.1919 0.3152 0.9333 11.00000 0.05 0.80 Q36 1 0.2500 0.3655 0.9144 11.00000 0.05 0.79 Q37 1 0.2174 0.3010 0.7392 11.00000 0.05 0.78 Q38 1 0.1667 0.4118 1.1190 11.00000 0.05 0.76 Q39 1 0.1693 0.3981 0.9175 11.00000 0.05 0.76 Q40 1 0.2254 0.3355 0.7381 11.00000 0.05 0.76 ; _shelx_res_checksum 54213 _shelx_hkl_file ; 0 0 2 2697.66 118.36 0 0 3 17.90 16.62 0 0 4 112.86 38.85 0 0 -5 81.13 37.38 0 0 5 6.67 23.53 0 0 6 179.85 58.35 0 0 -6 128.87 16.69 0 0 7 3.27 3.36 0 0 -7 -29.07 34.07 0 0 7 -8.56 16.19 0 0 -8 2052.83 217.73 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72.49 33.74 10 -12 12 99.19 31.82 10 12 13 76.10 26.68 10 12 14 29.70 12.21 10 12 15 2.61 4.74 10 -13 -21 73.75 24.58 10 -13 -20 165.19 46.22 10 -13 -19 161.68 50.00 10 -13 -18 34.64 35.23 10 -13 -17 15.05 24.90 10 -13 -16 50.33 56.52 10 -13 -15 47.87 27.54 10 -13 -14 309.70 101.87 10 -13 -13 144.39 73.02 10 -13 -12 414.53 78.40 10 -13 -12 332.18 101.01 10 -13 -11 246.46 72.79 -10 -13 11 112.83 160.93 10 -13 -11 140.91 75.02 10 -13 -10 121.10 49.31 -10 -13 10 -74.46 90.46 -10 -13 10 79.27 147.92 10 -13 -10 44.90 34.38 10 -13 -9 6.18 13.66 -10 -13 9 58.62 133.35 10 -13 -9 17.45 30.14 10 13 -8 130.08 59.25 10 -13 -8 266.94 73.28 -10 13 8 136.84 101.20 -10 -13 8 302.68 211.09 10 -13 -8 190.03 76.54 10 13 -7 121.93 82.62 10 -13 -7 73.59 32.18 -10 13 7 89.99 79.58 -10 -13 7 48.49 62.66 10 -13 -7 134.49 53.82 10 -13 -6 724.77 134.59 -10 13 6 594.30 193.34 10 -13 -6 770.67 133.64 -10 -13 6 577.89 264.74 10 13 -6 634.01 173.38 10 -13 -5 499.22 124.59 -10 13 5 625.92 199.83 10 -13 -5 666.14 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20 -7 -12 21.68 20.26 20 -7 -11 11.58 11.62 20 -7 -10 24.10 14.77 20 -7 -9 5.88 8.26 20 -7 -8 240.25 59.73 20 -7 -7 4.65 16.77 20 -7 -6 90.24 37.33 20 -7 -5 -22.79 22.19 20 -7 -4 24.94 26.44 20 -7 -3 23.27 21.66 20 7 -2 128.96 27.22 20 -7 -2 43.81 19.72 20 7 -1 15.89 14.20 20 -7 -1 -7.29 13.90 20 -7 0 85.90 31.55 20 7 0 186.08 31.91 20 7 1 13.93 8.67 20 7 1 68.87 23.62 20 7 2 44.81 12.71 20 -8 -16 54.41 19.22 -20 -8 15 73.22 30.91 20 -8 -15 28.59 18.69 -20 -8 14 0.00 13.39 20 -8 -14 25.48 13.67 -20 -8 13 0.00 19.00 20 -8 -13 48.53 20.71 -20 -8 12 67.42 31.34 20 -8 -12 234.28 51.81 20 -8 -11 39.49 22.84 20 -8 -10 158.75 41.98 20 -8 -9 36.16 26.42 20 -8 -8 53.74 27.87 20 -8 -7 2.90 10.89 20 -8 -6 33.64 20.74 20 -8 -5 6.75 9.15 20 -8 -4 139.79 44.70 20 -8 -3 11.96 7.57 20 8 -2 110.93 27.72 20 -8 -2 78.38 32.20 20 8 -1 -5.41 4.41 20 -8 -1 6.67 15.28 20 8 0 1.85 5.40 20 -8 0 28.88 17.98 20 8 1 -0.78 2.92 20 8 1 -15.03 10.92 20 8 2 112.78 20.13 20 -9 -15 127.42 29.79 -20 -9 14 23.55 17.80 20 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183.36 44.84 20 -11 -6 -20.05 15.17 20 -11 -5 12.74 5.50 20 -11 -4 -11.75 4.98 20 11 -3 82.57 18.23 20 -11 -3 47.10 22.91 20 11 -2 14.01 5.49 20 -11 -2 3.27 7.08 20 11 -1 12.48 12.05 20 -12 -11 97.01 28.13 20 -12 -10 27.24 14.71 20 -12 -9 26.87 13.18 20 -12 -8 -6.85 8.62 20 -12 -7 10.66 3.33 20 -12 -6 13.91 12.94 20 -12 -5 78.55 30.08 20 -12 -4 12.41 10.04 20 -12 -3 60.39 23.17 20 12 -2 -16.68 10.83 20 -13 -8 85.29 25.81 20 -13 -7 96.96 25.52 20 -13 -6 65.07 22.03 20 -13 -5 -18.30 12.44 21 0 -16 -11.58 10.83 21 0 -15 39.17 16.54 21 0 -14 -12.79 7.06 21 0 -13 0.64 3.56 21 0 -12 -8.52 9.72 21 0 -11 108.28 29.63 21 0 -10 -19.65 13.40 21 0 -9 126.60 32.02 21 0 -8 -2.01 9.04 21 0 -7 28.62 15.82 21 0 -6 6.35 3.73 21 0 -6 -8.42 10.96 21 0 -5 97.92 23.97 21 0 -4 8.60 7.71 21 0 -3 246.47 36.50 21 0 -2 -0.19 5.64 21 0 -1 138.34 26.88 21 0 0 -9.25 5.62 21 0 1 11.54 9.73 21 -1 -16 21.14 9.88 21 1 -15 62.20 20.48 21 -1 -15 60.64 22.61 21 1 -14 19.21 10.44 21 -1 -14 23.88 12.35 21 1 -13 103.05 27.36 21 -1 -13 95.12 30.61 21 1 -12 30.10 14.85 21 -1 -12 32.55 16.71 21 1 -11 50.51 21.49 21 -1 -11 17.08 11.89 21 1 -10 -1.46 7.02 21 -1 -10 6.45 9.02 21 1 -9 4.68 11.70 21 -1 -9 11.36 13.14 21 -1 -8 14.64 12.79 21 -1 -7 68.76 24.86 21 -1 -7 142.86 25.85 21 -1 -6 26.31 12.87 21 -1 -6 39.42 17.73 21 -1 -5 90.61 21.99 21 1 -5 106.31 26.27 21 -1 -5 36.95 14.90 21 -1 -4 4.95 6.22 21 1 -4 -2.33 5.79 21 -1 -4 1.55 7.22 21 -1 -3 6.23 9.47 21 1 -3 5.96 7.90 21 -1 -2 6.60 4.74 21 1 -2 -8.34 12.66 21 -1 -1 99.00 22.07 21 1 -1 113.71 24.00 21 -1 0 34.65 11.37 21 1 0 15.04 10.42 21 -1 1 153.86 23.91 21 1 1 171.35 29.05 21 1 2 18.59 6.49 21 -2 -16 39.57 13.95 21 -2 -15 2.68 3.36 21 -2 -14 -1.88 4.56 21 -2 -13 12.26 12.80 21 -2 -12 45.76 16.15 21 -2 -11 34.04 15.61 21 -2 -10 74.42 26.43 21 -2 -9 51.19 27.42 21 -2 -8 50.18 20.60 21 -2 -7 11.87 10.94 21 -2 -6 -6.37 13.06 21 -2 -5 -0.16 3.81 21 -2 -4 96.34 20.29 21 2 -4 119.52 25.48 21 -2 -4 48.94 24.83 21 -2 -3 83.17 18.91 21 2 -3 88.92 23.11 21 -2 -3 47.54 20.45 21 -2 -2 74.19 23.98 21 -2 -2 137.04 23.84 21 2 -2 140.24 27.06 21 -2 -1 25.92 9.93 21 2 -1 48.96 16.36 21 -2 0 57.99 16.10 21 2 0 55.48 15.33 21 2 1 -2.51 4.23 21 2 2 13.51 6.82 21 -3 -16 47.85 19.17 21 -3 -15 31.70 15.86 21 -3 -14 169.47 36.56 21 -3 -13 9.23 11.99 21 -3 -12 121.64 36.31 21 -3 -11 9.40 6.93 21 -3 -10 -3.16 13.80 21 -3 -9 -11.88 11.77 21 -3 -8 63.71 24.64 21 -3 -7 17.16 13.00 21 -3 -6 167.53 42.48 21 -3 -5 17.41 14.53 21 3 -4 68.75 19.32 21 -3 -4 27.69 16.39 21 3 -3 16.83 11.69 21 -3 -3 17.24 12.65 21 3 -2 16.58 10.67 21 -3 -2 18.84 14.69 21 3 -1 39.30 12.66 21 3 0 168.27 27.16 21 3 1 11.56 7.56 21 3 2 122.77 19.70 21 -4 -16 117.67 26.07 21 -4 -15 29.66 17.15 21 -4 -14 4.64 8.16 21 -4 -13 -11.88 12.06 21 -4 -12 44.27 19.31 21 -4 -11 19.28 16.69 21 -4 -10 161.98 39.75 21 -4 -9 -0.72 14.29 21 -4 -8 65.45 22.76 21 -4 -7 0.80 5.50 21 -4 -6 15.08 10.80 21 -4 -5 14.42 14.35 21 4 -4 133.28 26.94 21 -4 -4 99.69 29.16 21 4 -3 31.96 12.44 21 -4 -3 7.56 10.68 21 -4 -2 100.12 29.09 21 4 -2 201.82 31.09 21 4 -1 15.54 9.23 21 -4 -1 7.54 8.23 21 4 0 23.37 8.99 21 4 1 10.05 7.01 21 -5 -16 9.99 14.61 21 -5 -15 18.33 10.81 21 -5 -14 126.41 33.11 21 -5 -13 71.62 25.07 21 -5 -12 67.46 21.89 21 -5 -11 7.57 12.62 21 -5 -10 -9.45 12.31 21 -5 -9 5.22 12.50 21 -5 -8 56.14 24.15 21 -5 -7 33.40 17.65 21 -5 -6 87.18 30.14 21 -5 -5 14.61 11.67 21 -5 -4 40.31 20.33 21 5 -3 33.25 16.23 21 -5 -3 11.57 10.00 21 5 -2 29.50 11.33 21 -5 -2 0.26 4.43 21 5 -1 6.34 2.56 21 -5 -1 7.10 7.61 21 5 0 117.80 22.92 21 5 1 42.00 12.39 21 -6 -15 20.43 14.26 21 -6 -14 3.24 7.94 21 -6 -13 26.01 18.30 21 -6 -12 4.57 10.48 21 -6 -11 73.66 25.89 21 -6 -10 41.32 21.32 21 -6 -9 68.49 28.83 21 -6 -8 18.03 14.61 21 -6 -7 -1.39 9.81 21 -6 -6 7.47 5.47 21 -6 -5 42.54 23.82 21 -6 -4 26.97 15.81 21 -6 -3 34.08 15.31 21 6 -3 138.35 26.33 21 6 -2 40.96 13.92 21 -6 -2 11.80 9.80 21 6 -1 54.54 15.71 21 -6 -1 29.11 15.09 21 6 0 12.24 7.40 21 -7 -15 77.85 23.06 21 -7 -14 8.19 8.94 21 -7 -13 109.55 28.24 21 -7 -12 6.86 4.29 21 -7 -11 47.58 20.72 21 -7 -10 23.66 15.13 21 -7 -9 29.67 15.85 21 -7 -8 10.13 15.97 21 -7 -7 117.95 33.53 21 -7 -6 -3.65 8.34 21 -7 -5 67.63 24.85 21 7 -4 -3.68 2.75 21 -7 -4 6.67 6.28 21 7 -3 20.94 11.68 21 -7 -3 -1.04 4.83 21 7 -2 9.46 8.12 21 -7 -2 16.65 13.40 21 7 -1 98.78 20.43 21 -8 -14 -27.47 13.77 21 -8 -13 -0.84 5.57 21 -8 -12 -3.44 8.78 21 -8 -11 100.66 31.33 21 -8 -10 20.71 16.62 21 -8 -9 79.58 26.65 21 -8 -8 -13.12 10.67 21 -8 -7 15.03 11.82 21 -8 -6 2.77 10.70 21 -8 -5 28.83 21.68 21 8 -4 21.42 8.21 21 -8 -4 14.39 14.41 21 -8 -3 61.98 24.03 21 8 -3 123.64 21.58 21 8 -2 14.30 4.33 21 -8 -2 -0.88 9.51 21 -9 -13 46.35 15.95 21 -9 -12 70.58 21.82 21 -9 -11 10.64 5.81 21 -9 -10 1.79 5.49 21 -9 -9 6.48 6.89 21 -9 -8 38.20 16.81 21 -9 -7 75.41 22.51 21 -9 -6 50.90 23.21 21 -9 -5 27.38 11.89 21 9 -4 54.44 13.34 21 -9 -4 38.76 17.19 21 9 -3 -1.13 4.66 21 -9 -3 -0.21 7.07 21 -9 -2 -3.69 6.80 21 -10 -11 41.10 15.82 21 -10 -10 120.76 30.86 21 -10 -9 12.54 9.70 21 -10 -8 75.51 25.13 21 -10 -7 11.50 10.49 21 -10 -6 4.81 8.23 21 10 -5 7.92 5.83 21 -10 -5 -0.56 6.33 21 -10 -4 43.53 18.12 21 -10 -3 -11.04 6.71 21 -11 -8 46.78 17.92 21 -11 -7 -17.87 12.82 21 -11 -6 92.52 21.80 22 0 -4 65.90 15.13 22 -1 -12 85.98 23.83 22 -1 -11 -0.10 4.81 22 -1 -10 25.22 10.76 22 -1 -9 8.53 6.20 22 -1 -8 5.30 10.18 22 1 -7 4.34 5.86 22 1 -6 107.06 18.13 22 1 -5 11.42 4.65 22 1 -4 99.38 18.38 22 1 -3 18.96 8.16 22 -2 -13 14.71 11.21 22 -2 -12 -4.11 7.15 22 -2 -11 13.34 7.69 22 -2 -10 6.25 3.88 22 -2 -9 44.98 15.82 22 2 -8 51.90 12.88 22 -2 -8 15.31 7.37 22 2 -7 45.18 11.88 22 -2 -7 23.30 16.77 22 2 -6 11.73 3.93 22 -2 -6 29.96 14.30 22 2 -5 8.10 5.90 22 2 -4 17.79 7.41 22 2 -3 57.49 13.84 22 2 -2 43.54 12.73 22 -3 -13 119.95 27.32 22 -3 -12 -0.52 8.90 22 -3 -11 114.57 27.12 22 -3 -10 -3.09 9.69 22 -3 -9 10.34 5.82 22 -3 -8 -4.67 7.99 22 3 -7 82.56 17.25 22 -3 -7 27.92 13.03 22 3 -6 -2.98 6.88 22 -3 -6 6.54 6.81 22 -3 -5 86.91 22.63 22 3 -5 127.89 21.31 22 3 -4 16.83 11.44 22 3 -3 51.55 13.66 22 3 -2 -9.77 7.56 22 -4 -13 14.59 10.17 22 -4 -12 20.34 13.00 22 -4 -11 2.73 5.23 22 -4 -10 10.42 8.50 22 -4 -9 88.06 25.77 22 -4 -8 13.35 8.21 22 -4 -7 50.35 19.27 22 4 -6 0.87 5.17 22 -4 -6 11.29 9.43 22 4 -5 1.11 3.26 22 -4 -5 1.13 4.50 22 4 -4 4.80 6.61 22 4 -3 58.05 14.17 22 -5 -12 37.37 14.70 22 -5 -11 77.62 21.87 22 -5 -10 13.99 7.14 22 -5 -9 -18.35 11.32 22 -5 -8 15.10 5.55 22 -5 -7 31.12 15.30 22 5 -6 35.86 10.67 22 -5 -6 -14.30 12.57 22 -5 -5 56.46 19.64 22 5 -5 125.86 22.30 22 5 -4 38.14 11.84 22 5 -3 41.99 11.16 22 -6 -12 17.10 11.38 22 -6 -11 3.16 4.96 22 -6 -10 54.17 20.38 22 -6 -9 10.43 6.60 22 -6 -8 35.15 14.39 22 -6 -7 -1.77 8.12 22 6 -6 27.54 10.19 22 -6 -6 18.59 12.50 22 6 -5 4.02 2.71 22 -6 -5 4.51 6.90 22 6 -4 4.63 2.53 22 -7 -11 1.03 8.30 22 -7 -10 57.88 20.08 22 -7 -9 18.24 13.12 22 -7 -8 6.57 6.79 22 7 -7 -13.50 6.25 22 -7 -7 -7.33 9.66 22 -7 -6 48.76 18.30 22 7 -6 117.89 18.47 22 -8 -8 50.11 17.83 0 0 0 0.00 0.00 TITL THEPWA in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 18.422786 21.737475 20.557736 90.0000 108.1905 90.0000 ZERR 4.00 0.001308 0.001288 0.001336 0.0000 0.0068 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H B N O Si Th UNIT 300.00 536.00 4.00 20.00 12.00 12.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 9125 _olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount' _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 Th1 Th 0.16297(2) 0.31902(2) 0.81822(2) 0.03353(13) Uani 1 1 d . . . . . Si1 Si 0.2974(2) 0.39945(17) 0.96287(18) 0.0454(9) Uani 1 1 d . U . . . Si2 Si 0.1281(2) 0.15290(16) 0.80168(19) 0.0420(8) Uani 1 1 d . U . . . Si3 Si 0.0536(2) 0.41536(17) 0.67585(18) 0.0453(9) Uani 1 1 d . U . . . O1 O 0.2578(5) 0.3019(4) 0.7798(5) 0.044(2) Uani 1 1 d . . . . . N1 N 0.2032(6) 0.3845(5) 0.9147(5) 0.038(2) Uani 1 1 d . . . . . N2 N 0.1219(6) 0.2217(5) 0.8427(5) 0.036(2) Uani 1 1 d . . . . . N3 N 0.0588(5) 0.3665(5) 0.7434(6) 0.044(3) Uani 1 1 d . . . . . N4 N 0.0546(6) 0.3303(5) 0.8785(5) 0.039(2) Uani 1 1 d . . . . . N5 N 0.5444(6) 0.2871(5) 0.7082(4) 0.037(2) Uani 1 1 d . . . . . C1 C 0.3284(13) 0.4598(11) 0.8505(11) 0.100(6) Uani 1 1 d . U . . . H1A H 0.2724 0.4595 0.8336 0.149 Uiso 1 1 calc GR . . . . H1B H 0.3485 0.4545 0.8120 0.149 Uiso 1 1 calc GR . . . . H1C H 0.3462 0.4991 0.8733 0.149 Uiso 1 1 calc GR . . . . C2 C 0.4422(13) 0.4177(15) 0.9358(13) 0.141(10) Uani 1 1 d . U . . . H2A H 0.4524 0.4620 0.9402 0.211 Uiso 1 1 calc GR . . . . H2B H 0.4707 0.3993 0.9076 0.211 Uiso 1 1 calc GR . . . . H2C H 0.4583 0.3986 0.9813 0.211 Uiso 1 1 calc GR . . . . C3 C 0.3566(10) 0.4069(9) 0.9018(8) 0.065(4) Uani 1 1 d . U . . . H3 H 0.3507 0.3678 0.8750 0.078 Uiso 1 1 calc R . . . . C6 C 0.2818(12) 0.5274(8) 0.9871(10) 0.081(5) Uani 1 1 d . U . . . H6A H 0.3158 0.5393 0.9609 0.122 Uiso 1 1 calc GR . . . . H6B H 0.2834 0.5589 1.0217 0.122 Uiso 1 1 calc GR . . . . H6C H 0.2294 0.5234 0.9561 0.122 Uiso 1 1 calc GR . . . . C4 C 0.3883(12) 0.4724(11) 1.0751(10) 0.104(7) Uani 1 1 d . U . . . H4A H 0.3990 0.4349 1.1029 0.155 Uiso 1 1 calc GR . . . . H4B H 0.3903 0.5081 1.1047 0.155 Uiso 1 1 calc GR . . . . H4C H 0.4265 0.4771 1.0513 0.155 Uiso 1 1 calc GR . . . . C5 C 0.3072(11) 0.4678(8) 1.0214(9) 0.069(4) Uani 1 1 d . U . . . H5 H 0.2718 0.4593 1.0487 0.083 Uiso 1 1 calc R . . . . C7 C 0.3062(15) 0.3176(10) 1.0728(10) 0.101(6) Uani 1 1 d . U . . . H7A H 0.3284 0.3461 1.1108 0.151 Uiso 1 1 calc GR . . . . H7B H 0.3180 0.2752 1.0889 0.151 Uiso 1 1 calc GR . . . . H7C H 0.2507 0.3232 1.0558 0.151 Uiso 1 1 calc GR . . . . C9 C 0.3264(15) 0.2736(9) 0.9691(11) 0.104(7) Uani 1 1 d . U . . . H9A H 0.2714 0.2666 0.9487 0.156 Uiso 1 1 calc GR . . . . H9B H 0.3499 0.2375 0.9960 0.156 Uiso 1 1 calc GR . . . . H9C H 0.3494 0.2805 0.9327 0.156 Uiso 1 1 calc GR . . . . C8 C 0.3396(13) 0.3303(8) 1.0158(9) 0.081(5) Uani 1 1 d . U . . . H8 H 0.3958 0.3368 1.0363 0.097 Uiso 1 1 calc R . . . . C10 C 0.1434(8) 0.4096(7) 0.9378(7) 0.048(3) Uani 1 1 d . . . . . H10A H 0.1159 0.4417 0.9052 0.058 Uiso 1 1 calc R . . . . H10B H 0.1664 0.4295 0.9829 0.058 Uiso 1 1 calc R . . . . C11 C 0.0883(9) 0.3624(8) 0.9440(7) 0.056(4) Uani 1 1 d . . . . . H11A H 0.1146 0.3322 0.9796 0.067 Uiso 1 1 calc R . . . . H11B H 0.0473 0.3821 0.9583 0.067 Uiso 1 1 calc R . . . . C12 C 0.1482(13) 0.1240(7) 0.6695(8) 0.074(5) Uani 1 1 d . U . . . H12A H 0.1984 0.1083 0.6964 0.111 Uiso 1 1 calc GR . . . . H12B H 0.1510 0.1408 0.6262 0.111 Uiso 1 1 calc GR . . . . H12C H 0.1108 0.0905 0.6602 0.111 Uiso 1 1 calc GR . . . . C13 C 0.0455(10) 0.1985(7) 0.6673(7) 0.062(4) Uani 1 1 d . U . . . H13A H 0.0071 0.1663 0.6634 0.094 Uiso 1 1 calc GR . . . . H13B H 0.0468 0.2098 0.6216 0.094 Uiso 1 1 calc GR . . . . H13C H 0.0322 0.2347 0.6897 0.094 Uiso 1 1 calc GR . . . . C14 C 0.1237(10) 0.1747(7) 0.7098(7) 0.054(3) Uani 1 1 d . U . . . H14 H 0.1603 0.2095 0.7139 0.065 Uiso 1 1 calc R . . . . C15 C 0.0536(11) 0.0330(7) 0.7730(9) 0.073(5) Uani 1 1 d . U . . . H15A H 0.0313 0.0363 0.7232 0.110 Uiso 1 1 calc GR . . . . H15B H 0.0240 0.0035 0.7906 0.110 Uiso 1 1 calc GR . . . . H15C H 0.1066 0.0188 0.7844 0.110 Uiso 1 1 calc GR . . . . C16 C -0.0323(9) 0.1207(6) 0.7810(10) 0.072(5) Uani 1 1 d . U . . . H16A H -0.0352 0.1604 0.8028 0.108 Uiso 1 1 calc GR . . . . H16B H -0.0657 0.0910 0.7933 0.108 Uiso 1 1 calc GR . . . . H16C H -0.0487 0.1259 0.7312 0.108 Uiso 1 1 calc GR . . . . C17 C 0.0519(9) 0.0967(6) 0.8060(7) 0.050(3) Uani 1 1 d . U . . . H17 H 0.0626 0.0880 0.8560 0.060 Uiso 1 1 calc R . . . . C18 C 0.2305(10) 0.0969(8) 0.9216(8) 0.067(4) Uani 1 1 d . U . . . H18A H 0.2278 0.1356 0.9453 0.101 Uiso 1 1 calc GR . . . . H18B H 0.2801 0.0772 0.9433 0.101 Uiso 1 1 calc GR . . . . H18C H 0.1894 0.0694 0.9244 0.101 Uiso 1 1 calc GR . . . . C19 C 0.2914(10) 0.1456(8) 0.8371(9) 0.069(4) Uani 1 1 d . U . . . H19A H 0.2929 0.1432 0.7900 0.104 Uiso 1 1 calc GR . . . . H19B H 0.3379 0.1271 0.8682 0.104 Uiso 1 1 calc GR . . . . H19C H 0.2884 0.1889 0.8496 0.104 Uiso 1 1 calc GR . . . . C20 C 0.2212(9) 0.1109(7) 0.8429(8) 0.053(3) Uani 1 1 d . U . . . H20 H 0.2186 0.0706 0.8189 0.064 Uiso 1 1 calc R . . . . C21 C 0.0930(9) 0.2228(6) 0.9001(8) 0.054(4) Uani 1 1 d . . . . . H21A H 0.1345 0.2347 0.9420 0.065 Uiso 1 1 calc R . . . . H21B H 0.0752 0.1812 0.9074 0.065 Uiso 1 1 calc R . . . . C22 C 0.0271(8) 0.2682(6) 0.8880(8) 0.048(3) Uani 1 1 d . . . . . H22A H -0.0151 0.2561 0.8468 0.058 Uiso 1 1 calc R . . . . H22B H 0.0076 0.2681 0.9277 0.058 Uiso 1 1 calc R . . . . C23 C 0.1333(12) 0.5157(8) 0.7580(10) 0.086(6) Uani 1 1 d . U . . . H23A H 0.1346 0.4935 0.7999 0.129 Uiso 1 1 calc GR . . . . H23B H 0.1359 0.5601 0.7669 0.129 Uiso 1 1 calc GR . . . . H23C H 0.1769 0.5032 0.7434 0.129 Uiso 1 1 calc GR . . . . C24 C -0.0094(13) 0.5188(8) 0.7277(10) 0.087(5) Uani 1 1 d . U . . . H24A H -0.0576 0.5066 0.6937 0.130 Uiso 1 1 calc GR . . . . H24B H -0.0092 0.5634 0.7347 0.130 Uiso 1 1 calc GR . . . . H24C H -0.0042 0.4978 0.7711 0.130 Uiso 1 1 calc GR . . . . C25 C 0.0591(12) 0.5006(7) 0.7016(9) 0.070(4) Uani 1 1 d . U . . . H25 H 0.0565 0.5262 0.6604 0.084 Uiso 1 1 calc R . . . . C26 C -0.0407(13) 0.4432(11) 0.5410(10) 0.110(8) Uani 1 1 d . U . . . H26A H -0.0332 0.4870 0.5522 0.165 Uiso 1 1 calc GR . . . . H26B H -0.0907 0.4372 0.5064 0.165 Uiso 1 1 calc GR . . . . H26C H -0.0004 0.4288 0.5229 0.165 Uiso 1 1 calc GR . . . . C27 C -0.0600(12) 0.3425(9) 0.5807(10) 0.091(7) Uani 1 1 d . U . . . H27A H -0.0278 0.3277 0.5540 0.137 Uiso 1 1 calc GR . . . . H27B H -0.1137 0.3417 0.5521 0.137 Uiso 1 1 calc GR . . . . H27C H -0.0531 0.3159 0.6206 0.137 Uiso 1 1 calc GR . . . . C28 C -0.0374(12) 0.4075(9) 0.6042(9) 0.086(5) Uani 1 1 d . U . . . H28 H -0.0788 0.4242 0.6212 0.104 Uiso 1 1 calc R . . . . C29 C 0.1678(9) 0.4519(7) 0.6120(8) 0.059(4) Uani 1 1 d . U . . . H29A H 0.1322 0.4520 0.5653 0.088 Uiso 1 1 calc GR . . . . H29B H 0.2200 0.4461 0.6106 0.088 Uiso 1 1 calc GR . . . . H29C H 0.1643 0.4912 0.6342 0.088 Uiso 1 1 calc GR . . . . C30 C 0.1457(11) 0.3370(7) 0.6193(7) 0.062(4) Uani 1 1 d . U . . . H30A H 0.1391 0.3051 0.6506 0.093 Uiso 1 1 calc GR . . . . H30B H 0.1938 0.3302 0.6094 0.093 Uiso 1 1 calc GR . . . . H30C H 0.1030 0.3353 0.5765 0.093 Uiso 1 1 calc GR . . . . C31 C 0.1474(9) 0.3998(7) 0.6523(7) 0.053(3) Uani 1 1 d . U . . . H31 H 0.1897 0.3980 0.6968 0.064 Uiso 1 1 calc R . . . . C32 C -0.0148(8) 0.3533(6) 0.7575(7) 0.045(3) Uani 1 1 d . . . . . H32A H -0.0293 0.3098 0.7465 0.053 Uiso 1 1 calc R . . . . H32B H -0.0558 0.3795 0.7278 0.053 Uiso 1 1 calc R . . . . C33 C -0.0071(8) 0.3656(6) 0.8315(8) 0.052(4) Uani 1 1 d . . . . . H33A H 0.0026 0.4100 0.8410 0.063 Uiso 1 1 calc R . . . . H33B H -0.0558 0.3551 0.8397 0.063 Uiso 1 1 calc R . . . . C34 C 0.3150(9) 0.2853(7) 0.7493(7) 0.053(4) Uani 1 1 d . . . . . H34A H 0.2911 0.2633 0.7057 0.063 Uiso 1 1 calc R . . . . H34B H 0.3528 0.2575 0.7804 0.063 Uiso 1 1 calc R . . . . C35 C 0.3549(10) 0.3433(8) 0.7359(8) 0.058(4) Uani 1 1 d . . . . . H35A H 0.3160 0.3730 0.7097 0.070 Uiso 1 1 calc R . . . . H35B H 0.3833 0.3626 0.7801 0.070 Uiso 1 1 calc R . . . . C36 C 0.4091(8) 0.3297(7) 0.6968(8) 0.053(4) Uani 1 1 d . . . . . H36A H 0.4324 0.3688 0.6887 0.064 Uiso 1 1 calc R . . . . H36B H 0.3798 0.3126 0.6516 0.064 Uiso 1 1 calc R . . . . C37 C 0.4729(8) 0.2848(7) 0.7322(6) 0.045(3) Uani 1 1 d . . . . . H37A H 0.4519 0.2425 0.7250 0.054 Uiso 1 1 calc R . . . . H37B H 0.4890 0.2930 0.7821 0.054 Uiso 1 1 calc R . . . . C38 C 0.5759(8) 0.3514(6) 0.7183(6) 0.044(3) Uani 1 1 d . . . . . H38A H 0.6251 0.3511 0.7083 0.053 Uiso 1 1 calc R . . . . H38B H 0.5404 0.3781 0.6837 0.053 Uiso 1 1 calc R . . . . C39 C 0.5892(9) 0.3806(7) 0.7866(6) 0.054(4) Uani 1 1 d . . . . . H39A H 0.6151 0.4202 0.7878 0.080 Uiso 1 1 calc GR . . . . H39B H 0.6212 0.3536 0.8223 0.080 Uiso 1 1 calc GR . . . . H39C H 0.5401 0.3873 0.7947 0.080 Uiso 1 1 calc GR . . . . C40 C 0.5190(8) 0.2717(6) 0.6322(6) 0.043(3) Uani 1 1 d . . . . . H40A H 0.4918 0.2318 0.6250 0.052 Uiso 1 1 calc R . . . . H40B H 0.4825 0.3035 0.6071 0.052 Uiso 1 1 calc R . . . . C41 C 0.5843(9) 0.2682(9) 0.6031(7) 0.063(5) Uani 1 1 d . . . . . H41A H 0.5650 0.2551 0.5551 0.095 Uiso 1 1 calc GR . . . . H41B H 0.6220 0.2383 0.6293 0.095 Uiso 1 1 calc GR . . . . H41C H 0.6083 0.3087 0.6058 0.095 Uiso 1 1 calc GR . . . . C42 C 0.6039(9) 0.2427(6) 0.7504(7) 0.049(4) Uani 1 1 d . . . . . H42A H 0.6145 0.2528 0.7994 0.059 Uiso 1 1 calc R . . . . H42B H 0.6518 0.2488 0.7390 0.059 Uiso 1 1 calc R . . . . C43 C 0.5811(10) 0.1754(7) 0.7396(7) 0.060(4) Uani 1 1 d . . . . . H43A H 0.5747 0.1639 0.6920 0.090 Uiso 1 1 calc GR . . . . H43B H 0.5328 0.1691 0.7493 0.090 Uiso 1 1 calc GR . . . . H43C H 0.6210 0.1499 0.7704 0.090 Uiso 1 1 calc GR . . . . C44 C 0.3420(8) 0.3326(6) 0.4808(7) 0.045(3) Uani 1 1 d . . . . . C45 C 0.3218(9) 0.3737(6) 0.5247(6) 0.051(4) Uani 1 1 d . . . . . H45 H 0.2753 0.3671 0.5344 0.061 Uiso 1 1 calc R . . . . C46 C 0.3670(12) 0.4242(7) 0.5549(7) 0.067(5) Uani 1 1 d . . . . . H46 H 0.3506 0.4509 0.5842 0.080 Uiso 1 1 calc R . . . . C47 C 0.4360(11) 0.4354(7) 0.5421(7) 0.064(5) Uani 1 1 d . . . . . H47 H 0.4673 0.4693 0.5629 0.077 Uiso 1 1 calc R . . . . C48 C 0.4578(10) 0.3957(7) 0.4980(7) 0.060(4) Uani 1 1 d . . . . . H48 H 0.5034 0.4033 0.4870 0.072 Uiso 1 1 calc R . . . . C49 C 0.4123(7) 0.3448(6) 0.4703(7) 0.045(3) Uani 1 1 d . . . . . H49 H 0.4299 0.3170 0.4429 0.054 Uiso 1 1 calc R . . . . C50 C 0.2940(7) 0.2537(6) 0.3759(6) 0.036(3) Uani 1 1 d . . . . . C51 C 0.2837(7) 0.1922(6) 0.3475(6) 0.042(3) Uani 1 1 d . . . . . H51 H 0.2776 0.1594 0.3758 0.050 Uiso 1 1 calc R . . . . C52 C 0.2823(7) 0.1788(6) 0.2819(6) 0.041(3) Uani 1 1 d . . . . . H52 H 0.2742 0.1375 0.2663 0.049 Uiso 1 1 calc R . . . . C53 C 0.2920(8) 0.2226(7) 0.2393(6) 0.046(3) Uani 1 1 d . . . . . H53 H 0.2914 0.2119 0.1943 0.055 Uiso 1 1 calc R . . . . C54 C 0.3027(8) 0.2822(7) 0.2602(7) 0.049(3) Uani 1 1 d . . . . . H54 H 0.3097 0.3132 0.2301 0.059 Uiso 1 1 calc R . . . . C55 C 0.3034(8) 0.2975(7) 0.3268(6) 0.046(3) Uani 1 1 d . . . . . H55 H 0.3106 0.3395 0.3402 0.055 Uiso 1 1 calc R . . . . C56 C 0.1996(9) 0.2786(7) 0.4420(6) 0.051(4) Uani 1 1 d . . . . . C57 C 0.1536(9) 0.2298(9) 0.4471(7) 0.060(4) Uani 1 1 d . . . . . H57 H 0.1763 0.1903 0.4582 0.072 Uiso 1 1 calc R . . . . C58 C 0.0732(11) 0.2359(10) 0.4363(7) 0.069(5) Uani 1 1 d . . . . . H58 H 0.0442 0.2013 0.4419 0.083 Uiso 1 1 calc R . . . . C59 C 0.0377(11) 0.2926(12) 0.4177(8) 0.079(6) Uani 1 1 d . . . . . H59 H -0.0153 0.2976 0.4111 0.095 Uiso 1 1 calc R . . . . C60 C 0.0820(10) 0.3415(9) 0.4091(7) 0.069(5) Uani 1 1 d . . . . . H60 H 0.0585 0.3802 0.3946 0.082 Uiso 1 1 calc R . . . . C61 C 0.1607(9) 0.3352(8) 0.4213(7) 0.056(4) Uani 1 1 d . . . . . H61 H 0.1893 0.3700 0.4155 0.068 Uiso 1 1 calc R . . . . C62 C 0.3300(8) 0.2156(6) 0.5067(6) 0.039(3) Uani 1 1 d . . . . . C63 C 0.3105(8) 0.2076(5) 0.5658(6) 0.038(3) Uani 1 1 d . . . . . H63 H 0.2724 0.2335 0.5736 0.045 Uiso 1 1 calc R . . . . C64 C 0.3446(8) 0.1630(7) 0.6146(6) 0.049(4) Uani 1 1 d . . . . . H64 H 0.3296 0.1586 0.6546 0.058 Uiso 1 1 calc R . . . . C65 C 0.4005(9) 0.1252(7) 0.6044(7) 0.054(4) Uani 1 1 d . . . . . H65 H 0.4227 0.0936 0.6364 0.064 Uiso 1 1 calc R . . . . C66 C 0.4236(8) 0.1336(6) 0.5479(6) 0.043(3) Uani 1 1 d . . . . . H66 H 0.4627 0.1081 0.5416 0.052 Uiso 1 1 calc R . . . . C67 C 0.3906(7) 0.1791(6) 0.4988(6) 0.039(3) Uani 1 1 d . . . . . H67 H 0.4088 0.1853 0.4608 0.046 Uiso 1 1 calc R . . . . B1 B 0.2922(8) 0.2707(7) 0.4509(7) 0.035(3) Uani 1 1 d . . . . . O2 O 0.6879(9) 0.4184(6) 0.6457(9) 0.105(5) Uani 1 1 d D U . . . C68 C 0.7511(15) 0.4193(10) 0.6203(15) 0.122(8) Uani 1 1 d D U . . . H68A H 0.7451 0.3870 0.5851 0.146 Uiso 1 1 calc R . . . . H68B H 0.7989 0.4114 0.6579 0.146 Uiso 1 1 calc R . . . . C69 C 0.7543(15) 0.4807(9) 0.5900(13) 0.107(7) Uani 1 1 d D U . . . H69A H 0.8078 0.4936 0.5970 0.128 Uiso 1 1 calc R . . . . H69B H 0.7259 0.4812 0.5404 0.128 Uiso 1 1 calc R . . . . C70 C 0.7175(13) 0.5199(9) 0.6284(11) 0.092(5) Uani 1 1 d D U . . . H70A H 0.6955 0.5573 0.6022 0.111 Uiso 1 1 calc R . . . . H70B H 0.7537 0.5321 0.6732 0.111 Uiso 1 1 calc R . . . . C71 C 0.6569(13) 0.4787(9) 0.6369(13) 0.106(6) Uani 1 1 d D U . . . H71A H 0.6422 0.4910 0.6774 0.128 Uiso 1 1 calc R . . . . H71B H 0.6111 0.4805 0.5959 0.128 Uiso 1 1 calc R . . . . O0AA O 0.1276(11) 0.4255(9) 1.1122(9) 0.120(6) Uiso 1 1 d . . . . . C1AA C 0.1472(14) 0.5308(12) 1.1077(12) 0.106(7) Uiso 1 1 d . . . . . H1AA H 0.1249 0.5685 1.1207 0.127 Uiso 1 1 calc R . . . . H1AB H 0.1659 0.5404 1.0686 0.127 Uiso 1 1 calc R . . . . C2AA C 0.0914(14) 0.4811(11) 1.0906(12) 0.106(7) Uiso 1 1 d . . . . . H2AA H 0.0519 0.4882 1.1131 0.127 Uiso 1 1 calc R . . . . H2AB H 0.0660 0.4800 1.0405 0.127 Uiso 1 1 calc R . . . . C4AA C 0.1964(16) 0.4381(13) 1.1707(14) 0.124(9) Uiso 1 1 d . . . . . H4AA H 0.2406 0.4142 1.1667 0.149 Uiso 1 1 calc R . . . . H4AB H 0.1877 0.4274 1.2145 0.149 Uiso 1 1 calc R . . . . C3AA C 0.2100(14) 0.5063(11) 1.1668(12) 0.103(7) Uiso 1 1 d . . . . . H3AA H 0.2097 0.5267 1.2097 0.123 Uiso 1 1 calc R . . . . H3AB H 0.2602 0.5137 1.1599 0.123 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th1 0.0398(2) 0.0266(2) 0.0375(2) -0.00223(18) 0.01680(16) -0.00184(19) Si1 0.054(2) 0.0352(18) 0.0399(17) -0.0002(15) 0.0037(15) -0.0009(17) Si2 0.048(2) 0.0260(16) 0.0508(19) -0.0034(14) 0.0143(15) -0.0021(15) Si3 0.051(2) 0.0332(18) 0.0442(18) -0.0002(15) 0.0048(15) -0.0029(16) O1 0.035(4) 0.047(5) 0.061(5) -0.007(4) 0.034(4) -0.008(4) N1 0.038(6) 0.040(6) 0.039(5) -0.005(5) 0.015(4) 0.010(5) N2 0.042(6) 0.034(5) 0.038(5) 0.001(4) 0.022(4) -0.004(5) N3 0.017(5) 0.031(5) 0.079(8) -0.003(5) 0.007(5) -0.015(4) N4 0.055(7) 0.036(6) 0.038(5) -0.004(4) 0.032(5) -0.006(5) N5 0.035(5) 0.049(6) 0.022(4) -0.007(4) 0.000(4) -0.006(5) C1 0.103(13) 0.109(13) 0.103(11) 0.020(10) 0.056(10) -0.006(11) C2 0.072(9) 0.21(3) 0.129(15) -0.010(16) 0.020(8) -0.028(9) C3 0.064(8) 0.075(9) 0.054(6) -0.019(6) 0.016(5) -0.014(7) C6 0.095(12) 0.051(7) 0.104(11) -0.018(7) 0.039(9) -0.015(7) C4 0.094(11) 0.107(14) 0.096(11) -0.051(10) 0.009(9) -0.001(9) C5 0.079(9) 0.051(6) 0.076(8) -0.024(6) 0.021(7) -0.019(6) C7 0.139(17) 0.088(13) 0.064(8) 0.015(8) 0.016(9) 0.001(12) C9 0.134(19) 0.068(8) 0.092(11) 0.002(8) 0.009(11) 0.015(9) C8 0.106(12) 0.059(7) 0.058(7) 0.012(5) 0.000(7) 0.011(7) C10 0.060(9) 0.044(8) 0.050(7) -0.025(6) 0.030(6) -0.010(7) C11 0.056(9) 0.063(10) 0.053(8) -0.017(7) 0.022(7) -0.012(8) C12 0.126(14) 0.046(8) 0.061(8) -0.001(6) 0.046(8) 0.012(9) C13 0.087(9) 0.039(7) 0.048(7) -0.016(6) 0.002(6) 0.000(7) C14 0.074(8) 0.042(6) 0.043(5) -0.007(5) 0.015(5) 0.004(6) C15 0.086(11) 0.035(6) 0.096(12) -0.020(7) 0.025(9) -0.006(6) C16 0.048(6) 0.028(6) 0.138(15) -0.010(8) 0.026(6) -0.026(5) C17 0.057(6) 0.039(6) 0.057(7) -0.013(5) 0.022(5) -0.013(5) C18 0.060(9) 0.065(10) 0.071(7) 0.007(7) 0.012(6) 0.004(8) C19 0.057(7) 0.063(10) 0.082(10) 0.005(8) 0.014(6) -0.005(7) C20 0.053(6) 0.037(7) 0.062(6) -0.003(5) 0.009(5) 0.002(5) C21 0.065(10) 0.031(7) 0.060(8) 0.005(7) 0.012(7) -0.003(7) C22 0.056(9) 0.029(7) 0.070(9) -0.013(7) 0.037(7) -0.015(6) C23 0.110(10) 0.049(9) 0.086(10) -0.024(8) 0.012(8) 0.005(8) C24 0.123(11) 0.050(9) 0.090(11) 0.015(8) 0.037(9) 0.023(8) C25 0.094(9) 0.043(6) 0.068(8) 0.001(6) 0.018(6) 0.006(6) C26 0.092(15) 0.121(14) 0.081(9) 0.030(9) -0.023(9) -0.020(12) C27 0.085(13) 0.085(9) 0.076(10) -0.003(7) -0.016(10) -0.026(8) C28 0.078(8) 0.082(9) 0.074(8) 0.008(6) -0.013(7) -0.013(7) C29 0.055(8) 0.052(7) 0.064(8) 0.010(6) 0.010(6) -0.001(6) C30 0.098(12) 0.048(6) 0.042(7) -0.003(5) 0.023(7) -0.006(6) C31 0.067(7) 0.050(6) 0.040(6) -0.003(5) 0.014(5) -0.008(5) C32 0.056(8) 0.034(7) 0.047(7) 0.003(6) 0.021(6) 0.003(6) C33 0.052(9) 0.025(6) 0.093(11) -0.001(7) 0.041(8) -0.004(6) C34 0.058(9) 0.054(9) 0.050(7) 0.024(7) 0.022(7) 0.003(8) C35 0.069(10) 0.060(10) 0.057(8) 0.002(7) 0.035(8) 0.003(9) C36 0.032(7) 0.061(10) 0.063(9) -0.009(7) 0.010(6) 0.002(7) C37 0.048(8) 0.054(8) 0.035(6) 0.003(6) 0.015(5) -0.010(7) C38 0.038(7) 0.048(8) 0.041(6) -0.006(6) 0.005(5) -0.002(6) C39 0.065(10) 0.051(9) 0.044(7) -0.008(7) 0.014(7) -0.001(8) C40 0.047(8) 0.043(7) 0.032(6) -0.001(6) 0.001(5) -0.002(6) C41 0.061(10) 0.096(13) 0.032(6) -0.013(8) 0.014(6) 0.020(10) C42 0.069(10) 0.030(7) 0.039(6) -0.004(6) 0.002(6) -0.004(7) C43 0.074(11) 0.045(8) 0.046(7) -0.010(7) -0.004(7) 0.005(8) C44 0.049(8) 0.029(7) 0.047(7) 0.006(6) -0.002(6) 0.013(6) C45 0.066(10) 0.038(7) 0.041(7) -0.005(6) 0.006(6) 0.003(7) C46 0.100(15) 0.048(9) 0.034(7) -0.002(7) -0.006(8) 0.005(10) C47 0.090(13) 0.032(8) 0.046(8) -0.003(6) -0.015(8) -0.006(8) C48 0.072(11) 0.042(8) 0.050(8) -0.009(7) -0.003(7) 0.002(8) C49 0.031(6) 0.041(7) 0.055(8) 0.017(6) 0.003(5) -0.003(6) C50 0.034(6) 0.035(7) 0.032(5) 0.004(5) 0.001(5) -0.003(5) C51 0.041(7) 0.042(7) 0.038(6) -0.004(6) 0.004(5) -0.007(6) C52 0.028(6) 0.043(7) 0.040(6) -0.010(6) -0.007(5) -0.002(6) C53 0.044(7) 0.063(9) 0.039(6) 0.009(6) 0.023(6) 0.000(7) C54 0.049(8) 0.049(8) 0.043(7) -0.012(6) 0.006(6) -0.005(7) C55 0.055(8) 0.041(7) 0.039(6) -0.004(6) 0.009(6) -0.009(7) C56 0.062(9) 0.052(9) 0.034(6) -0.005(6) 0.010(6) -0.006(8) C57 0.057(10) 0.073(11) 0.049(8) -0.012(8) 0.016(7) -0.006(9) C58 0.075(12) 0.097(14) 0.045(8) -0.013(9) 0.033(8) -0.037(11) C59 0.051(10) 0.14(2) 0.048(9) -0.006(11) 0.013(7) 0.001(12) C60 0.067(11) 0.092(13) 0.037(7) -0.010(8) 0.001(7) 0.031(10) C61 0.056(9) 0.061(10) 0.043(7) -0.009(7) 0.003(6) 0.014(8) C62 0.046(7) 0.038(7) 0.029(5) -0.004(5) 0.009(5) 0.007(6) C63 0.050(8) 0.021(6) 0.045(6) 0.003(5) 0.020(6) -0.002(5) C64 0.040(7) 0.066(10) 0.033(6) 0.023(6) 0.001(5) 0.003(7) C65 0.055(9) 0.055(9) 0.044(7) 0.014(7) 0.007(6) 0.002(8) C66 0.054(8) 0.035(7) 0.045(7) -0.002(6) 0.020(6) 0.004(6) C67 0.043(7) 0.040(7) 0.032(5) 0.000(5) 0.011(5) -0.003(6) B1 0.030(7) 0.038(8) 0.033(6) 0.002(6) 0.006(5) 0.012(6) O2 0.098(10) 0.077(7) 0.145(13) 0.042(8) 0.043(9) 0.008(7) C68 0.125(15) 0.082(9) 0.17(2) 0.045(10) 0.067(15) 0.013(9) C69 0.117(15) 0.077(10) 0.137(15) 0.033(10) 0.054(13) 0.005(9) C70 0.113(13) 0.073(8) 0.090(12) 0.038(8) 0.029(10) 0.013(8) C71 0.109(12) 0.084(9) 0.128(16) 0.049(9) 0.040(11) 0.018(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -4.1491 12.3296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 9 4 -10 0.0132 9.0153 4.0066 -9.9762 -0.9384 -0.2123 -0.1229 -7 0 -8 0.1600 -6.9981 -0.0122 -7.9979 -0.0052 0.5095 -0.8710 0 14 2 0.0286 -0.0146 14.0050 2.0085 0.0519 -0.9254 -0.3903 -3 13 3 0.0183 -3.0176 13.0017 3.0035 0.2564 -0.7959 -0.4877 3 -13 -3 0.0183 3.0176 -13.0017 -3.0035 -0.2564 0.7959 0.4877 5 0 9 0.1546 4.9952 0.0103 8.9947 0.1549 -0.4753 0.8003 -9 -2 11 0.0148 -9.0181 -2.0055 10.9766 0.9787 0.0559 0.1059 9 2 -11 0.0148 9.0181 2.0055 -10.9766 -0.9787 -0.0559 -0.1059 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 O1 Th1 N1 109.4(4) . . O1 Th1 N2 105.9(4) . . O1 Th1 N3 115.8(4) . . O1 Th1 N4 172.7(3) . . N1 Th1 N4 68.9(3) . . N2 Th1 N1 113.5(4) . . N2 Th1 N4 69.3(3) . . N3 Th1 N1 105.6(4) . . N3 Th1 N2 106.8(3) . . N3 Th1 N4 71.3(4) . . N1 Si1 C3 108.3(6) . . N1 Si1 C5 113.0(7) . . N1 Si1 C8 109.8(8) . . C5 Si1 C3 113.2(8) . . C8 Si1 C3 103.4(10) . . C8 Si1 C5 108.7(8) . . N2 Si2 C14 106.0(6) . . N2 Si2 C17 111.8(6) . . N2 Si2 C20 112.7(6) . . C17 Si2 C14 113.7(7) . . C17 Si2 C20 104.5(7) . . C20 Si2 C14 108.2(7) . . N3 Si3 C25 112.7(7) . . N3 Si3 C28 112.9(8) . . N3 Si3 C31 105.1(6) . . C25 Si3 C31 105.0(8) . . C28 Si3 C25 105.2(9) . . C28 Si3 C31 115.7(9) . . C34 O1 Th1 173.3(9) . . Si1 N1 Th1 125.9(5) . . C10 N1 Th1 115.7(8) . . C10 N1 Si1 118.2(8) . . Si2 N2 Th1 126.5(5) . . C21 N2 Th1 112.8(8) . . C21 N2 Si2 120.7(9) . . Si3 N3 Th1 129.7(6) . . C32 N3 Th1 113.7(8) . . C32 N3 Si3 116.5(8) . . C11 N4 Th1 107.8(8) . . C11 N4 C22 112.1(11) . . C22 N4 Th1 108.3(7) . . C33 N4 Th1 106.4(7) . . C33 N4 C11 112.1(11) . . C33 N4 C22 109.9(11) . . C38 N5 C37 108.5(10) . . C38 N5 C40 109.2(10) . . C38 N5 C42 109.5(9) . . C40 N5 C37 107.6(9) . . C42 N5 C37 109.5(10) . . C42 N5 C40 112.6(10) . . H1A C1 H1B 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . C3 C1 H1A 109.5 . . C3 C1 H1B 109.5 . . C3 C1 H1C 109.5 . . H2A C2 H2B 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . C3 C2 H2A 109.5 . . C3 C2 H2B 109.5 . . C3 C2 H2C 109.5 . . Si1 C3 H3 107.6 . . C1 C3 Si1 111.9(14) . . C1 C3 H3 107.6 . . C2 C3 Si1 115.6(14) . . C2 C3 C1 106.2(19) . . C2 C3 H3 107.6 . . H6A C6 H6B 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C5 C6 H6A 109.5 . . C5 C6 H6B 109.5 . . C5 C6 H6C 109.5 . . H4A C4 H4B 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . C5 C4 H4A 109.5 . . C5 C4 H4B 109.5 . . C5 C4 H4C 109.5 . . Si1 C5 H5 105.3 . . C6 C5 Si1 115.6(13) . . C6 C5 C4 111.8(16) . . C6 C5 H5 105.3 . . C4 C5 Si1 112.4(14) . . C4 C5 H5 105.3 . . H7A C7 H7B 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C8 C7 H7A 109.5 . . C8 C7 H7B 109.5 . . C8 C7 H7C 109.5 . . H9A C9 H9B 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C8 C9 H9A 109.5 . . C8 C9 H9B 109.5 . . C8 C9 H9C 109.5 . . Si1 C8 H8 108.5 . . C7 C8 Si1 113.7(16) . . C7 C8 C9 108.5(19) . . C7 C8 H8 108.5 . . C9 C8 Si1 108.9(12) . . C9 C8 H8 108.5 . . N1 C10 H10A 109.1 . . N1 C10 H10B 109.1 . . N1 C10 C11 112.6(12) . . H10A C10 H10B 107.8 . . C11 C10 H10A 109.1 . . C11 C10 H10B 109.1 . . N4 C11 C10 110.8(12) . . N4 C11 H11A 109.5 . . N4 C11 H11B 109.5 . . C10 C11 H11A 109.5 . . C10 C11 H11B 109.5 . . H11A C11 H11B 108.1 . . H12A C12 H12B 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . C14 C12 H12A 109.5 . . C14 C12 H12B 109.5 . . C14 C12 H12C 109.5 . . H13A C13 H13B 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . C14 C13 H13A 109.5 . . C14 C13 H13B 109.5 . . C14 C13 H13C 109.5 . . Si2 C14 H14 106.5 . . C12 C14 Si2 115.1(11) . . C12 C14 H14 106.5 . . C13 C14 Si2 112.9(12) . . C13 C14 C12 108.7(13) . . C13 C14 H14 106.5 . . H15A C15 H15B 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . C17 C15 H15A 109.5 . . C17 C15 H15B 109.5 . . C17 C15 H15C 109.5 . . H16A C16 H16B 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C17 C16 H16A 109.5 . . C17 C16 H16B 109.5 . . C17 C16 H16C 109.5 . . Si2 C17 H17 105.0 . . C15 C17 Si2 116.2(12) . . C15 C17 C16 108.0(12) . . C15 C17 H17 105.0 . . C16 C17 Si2 116.4(10) . . C16 C17 H17 105.0 . . H18A C18 H18B 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . C20 C18 H18A 109.5 . . C20 C18 H18B 109.5 . . C20 C18 H18C 109.5 . . H19A C19 H19B 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . C20 C19 H19A 109.5 . . C20 C19 H19B 109.5 . . C20 C19 H19C 109.5 . . Si2 C20 H20 107.8 . . C18 C20 Si2 109.9(11) . . C18 C20 H20 107.8 . . C19 C20 Si2 113.3(10) . . C19 C20 C18 110.1(13) . . C19 C20 H20 107.8 . . N2 C21 H21A 109.5 . . N2 C21 H21B 109.5 . . N2 C21 C22 110.9(11) . . H21A C21 H21B 108.0 . . C22 C21 H21A 109.5 . . C22 C21 H21B 109.5 . . N4 C22 C21 109.1(11) . . N4 C22 H22A 109.9 . . N4 C22 H22B 109.9 . . C21 C22 H22A 109.9 . . C21 C22 H22B 109.9 . . H22A C22 H22B 108.3 . . H23A C23 H23B 109.5 . . H23A C23 H23C 109.5 . . H23B C23 H23C 109.5 . . C25 C23 H23A 109.5 . . C25 C23 H23B 109.5 . . C25 C23 H23C 109.5 . . H24A C24 H24B 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . C25 C24 H24A 109.5 . . C25 C24 H24B 109.5 . . C25 C24 H24C 109.5 . . Si3 C25 H25 108.6 . . C23 C25 Si3 111.9(12) . . C23 C25 C24 108.1(16) . . C23 C25 H25 108.6 . . C24 C25 Si3 111.1(13) . . C24 C25 H25 108.6 . . H26A C26 H26B 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C28 C26 H26A 109.5 . . C28 C26 H26B 109.5 . . C28 C26 H26C 109.5 . . H27A C27 H27B 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C28 C27 H27A 109.5 . . C28 C27 H27B 109.5 . . C28 C27 H27C 109.5 . . Si3 C28 H28 106.7 . . C26 C28 Si3 114.9(15) . . C26 C28 C27 105.9(17) . . C26 C28 H28 106.7 . . C27 C28 Si3 115.4(14) . . C27 C28 H28 106.7 . . H29A C29 H29B 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . C31 C29 H29A 109.5 . . C31 C29 H29B 109.5 . . C31 C29 H29C 109.5 . . H30A C30 H30B 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . C31 C30 H30A 109.5 . . C31 C30 H30B 109.5 . . C31 C30 H30C 109.5 . . Si3 C31 H31 105.9 . . C29 C31 Si3 113.1(11) . . C29 C31 C30 113.7(13) . . C29 C31 H31 105.9 . . C30 C31 Si3 111.5(12) . . C30 C31 H31 105.9 . . N3 C32 H32A 109.5 . . N3 C32 H32B 109.5 . . N3 C32 C33 110.8(11) . . H32A C32 H32B 108.1 . . C33 C32 H32A 109.5 . . C33 C32 H32B 109.5 . . N4 C33 C32 112.6(11) . . N4 C33 H33A 109.1 . . N4 C33 H33B 109.1 . . C32 C33 H33A 109.1 . . C32 C33 H33B 109.1 . . H33A C33 H33B 107.8 . . O1 C34 H34A 109.8 . . O1 C34 H34B 109.8 . . O1 C34 C35 109.5(12) . . H34A C34 H34B 108.2 . . C35 C34 H34A 109.8 . . C35 C34 H34B 109.8 . . C34 C35 H35A 109.2 . . C34 C35 H35B 109.2 . . H35A C35 H35B 107.9 . . C36 C35 C34 112.1(14) . . C36 C35 H35A 109.2 . . C36 C35 H35B 109.2 . . C35 C36 H36A 108.6 . . C35 C36 H36B 108.6 . . C35 C36 C37 114.5(13) . . H36A C36 H36B 107.6 . . C37 C36 H36A 108.6 . . C37 C36 H36B 108.6 . . N5 C37 H37A 108.4 . . N5 C37 H37B 108.4 . . C36 C37 N5 115.6(11) . . C36 C37 H37A 108.4 . . C36 C37 H37B 108.4 . . H37A C37 H37B 107.4 . . N5 C38 H38A 107.8 . . N5 C38 H38B 107.8 . . H38A C38 H38B 107.1 . . C39 C38 N5 118.0(12) . . C39 C38 H38A 107.8 . . C39 C38 H38B 107.8 . . C38 C39 H39A 109.5 . . C38 C39 H39B 109.5 . . C38 C39 H39C 109.5 . . H39A C39 H39B 109.5 . . H39A C39 H39C 109.5 . . H39B C39 H39C 109.5 . . N5 C40 H40A 109.0 . . N5 C40 H40B 108.9 . . H40A C40 H40B 107.8 . . C41 C40 N5 113.1(11) . . C41 C40 H40A 108.9 . . C41 C40 H40B 108.9 . . C40 C41 H41A 109.5 . . C40 C41 H41B 109.5 . . C40 C41 H41C 109.5 . . H41A C41 H41B 109.5 . . H41A C41 H41C 109.5 . . H41B C41 H41C 109.5 . . N5 C42 H42A 108.7 . . N5 C42 H42B 108.7 . . N5 C42 C43 114.3(11) . . H42A C42 H42B 107.6 . . C43 C42 H42A 108.7 . . C43 C42 H42B 108.7 . . C42 C43 H43A 109.5 . . C42 C43 H43B 109.5 . . C42 C43 H43C 109.5 . . H43A C43 H43B 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . C45 C44 C49 115.0(13) . . C45 C44 B1 122.4(14) . . C49 C44 B1 122.2(13) . . C44 C45 H45 118.5 . . C46 C45 C44 123.1(17) . . C46 C45 H45 118.5 . . C45 C46 H46 119.9 . . C47 C46 C45 120.2(16) . . C47 C46 H46 119.9 . . C46 C47 H47 120.8 . . C46 C47 C48 118.5(15) . . C48 C47 H47 120.8 . . C47 C48 H48 120.2 . . C49 C48 C47 119.6(18) . . C49 C48 H48 120.2 . . C44 C49 H49 118.2 . . C48 C49 C44 123.5(16) . . C48 C49 H49 118.2 . . C51 C50 B1 124.3(11) . . C55 C50 C51 111.0(11) . . C55 C50 B1 124.7(11) . . C50 C51 H51 118.2 . . C52 C51 C50 123.5(12) . . C52 C51 H51 118.2 . . C51 C52 H52 119.1 . . C53 C52 C51 121.7(13) . . C53 C52 H52 119.1 . . C52 C53 H53 119.9 . . C52 C53 C54 120.2(13) . . C54 C53 H53 119.9 . . C53 C54 H54 120.3 . . C53 C54 C55 119.4(14) . . C55 C54 H54 120.3 . . C50 C55 H55 117.9 . . C54 C55 C50 124.1(13) . . C54 C55 H55 117.9 . . C57 C56 C61 115.1(15) . . C57 C56 B1 122.9(14) . . C61 C56 B1 121.6(14) . . C56 C57 H57 118.5 . . C56 C57 C58 123.0(18) . . C58 C57 H57 118.5 . . C57 C58 H58 120.1 . . C59 C58 C57 119.9(17) . . C59 C58 H58 120.1 . . C58 C59 H59 121.0 . . C60 C59 C58 118.1(17) . . C60 C59 H59 121.0 . . C59 C60 H60 119.3 . . C59 C60 C61 121.4(18) . . C61 C60 H60 119.3 . . C56 C61 H61 118.8 . . C60 C61 C56 122.4(17) . . C60 C61 H61 118.8 . . C63 C62 C67 117.4(11) . . C63 C62 B1 122.2(11) . . C67 C62 B1 120.0(11) . . C62 C63 H63 118.8 . . C62 C63 C64 122.4(13) . . C64 C63 H63 118.8 . . C63 C64 H64 120.2 . . C65 C64 C63 119.6(13) . . C65 C64 H64 120.2 . . C64 C65 H65 120.3 . . C66 C65 C64 119.5(13) . . C66 C65 H65 120.3 . . C65 C66 H66 119.2 . . C65 C66 C67 121.6(13) . . C67 C66 H66 119.2 . . C62 C67 H67 120.4 . . C66 C67 C62 119.3(12) . . C66 C67 H67 120.4 . . C44 B1 C56 113.0(11) . . C44 B1 C62 105.6(9) . . C50 B1 C44 112.0(11) . . C50 B1 C56 104.3(9) . . C50 B1 C62 111.9(10) . . C62 B1 C56 110.2(11) . . C68 O2 C71 106.5(17) . . O2 C68 H68A 110.0 . . O2 C68 H68B 110.0 . . O2 C68 C69 108.3(19) . . H68A C68 H68B 108.4 . . C69 C68 H68A 110.0 . . C69 C68 H68B 110.0 . . C68 C69 H69A 111.3 . . C68 C69 H69B 111.3 . . H69A C69 H69B 109.2 . . C70 C69 C68 102.2(19) . . C70 C69 H69A 111.3 . . C70 C69 H69B 111.3 . . C69 C70 H70A 111.4 . . C69 C70 H70B 111.4 . . C69 C70 C71 101.8(18) . . H70A C70 H70B 109.3 . . C71 C70 H70A 111.4 . . C71 C70 H70B 111.4 . . O2 C71 C70 106.6(17) . . O2 C71 H71A 110.4 . . O2 C71 H71B 110.4 . . C70 C71 H71A 110.4 . . C70 C71 H71B 110.4 . . H71A C71 H71B 108.6 . . C2AA O0AA C4AA 108(2) . . H1AA C1AA H1AB 109.0 . . C2AA C1AA H1AA 111.0 . . C2AA C1AA H1AB 111.0 . . C2AA C1AA C3AA 104(2) . . C3AA C1AA H1AA 111.0 . . C3AA C1AA H1AB 111.0 . . O0AA C2AA C1AA 110(2) . . O0AA C2AA H2AA 109.7 . . O0AA C2AA H2AB 109.7 . . C1AA C2AA H2AA 109.7 . . C1AA C2AA H2AB 109.7 . . H2AA C2AA H2AB 108.2 . . O0AA C4AA H4AA 110.8 . . O0AA C4AA H4AB 110.8 . . O0AA C4AA C3AA 105(2) . . H4AA C4AA H4AB 108.9 . . C3AA C4AA H4AA 110.8 . . C3AA C4AA H4AB 110.8 . . C1AA C3AA C4AA 107(2) . . C1AA C3AA H3AA 110.3 . . C1AA C3AA H3AB 110.3 . . C4AA C3AA H3AA 110.3 . . C4AA C3AA H3AB 110.3 . . H3AA C3AA H3AB 108.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Th1 O1 2.162(8) . Th1 N1 2.365(10) . Th1 N2 2.353(10) . Th1 N3 2.296(10) . Th1 N4 2.670(10) . Si1 N1 1.739(11) . Si1 C3 1.909(18) . Si1 C5 1.885(16) . Si1 C8 1.876(17) . Si2 N2 1.739(11) . Si2 C14 1.924(15) . Si2 C17 1.885(15) . Si2 C20 1.893(15) . Si3 N3 1.728(12) . Si3 C25 1.921(16) . Si3 C28 1.863(17) . Si3 C31 1.964(17) . O1 C34 1.430(17) . N1 C10 1.437(16) . N2 C21 1.438(18) . N3 C32 1.499(17) . N4 C11 1.471(16) . N4 C22 1.476(16) . N4 C33 1.457(18) . N5 C37 1.544(17) . N5 C38 1.502(17) . N5 C40 1.521(14) . N5 C42 1.513(16) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C1 C3 1.54(3) . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 H2C 0.9800 . C2 C3 1.53(3) . C3 H3 1.0000 . C6 H6A 0.9800 . C6 H6B 0.9800 . C6 H6C 0.9800 . C6 C5 1.48(2) . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . C4 C5 1.56(2) . C5 H5 1.0000 . C7 H7A 0.9800 . C7 H7B 0.9800 . C7 H7C 0.9800 . C7 C8 1.51(3) . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C9 C8 1.54(3) . C8 H8 1.0000 . C10 H10A 0.9900 . C10 H10B 0.9900 . C10 C11 1.48(2) . C11 H11A 0.9900 . C11 H11B 0.9900 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . C12 C14 1.53(2) . C13 H13A 0.9800 . C13 H13B 0.9800 . C13 H13C 0.9800 . C13 C14 1.52(2) . C14 H14 1.0000 . C15 H15A 0.9800 . C15 H15B 0.9800 . C15 H15C 0.9800 . C15 C17 1.546(19) . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . C16 C17 1.56(2) . C17 H17 1.0000 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . C18 C20 1.60(2) . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . C19 C20 1.53(2) . C20 H20 1.0000 . C21 H21A 0.9900 . C21 H21B 0.9900 . C21 C22 1.52(2) . C22 H22A 0.9900 . C22 H22B 0.9900 . C23 H23A 0.9800 . C23 H23B 0.9800 . C23 H23C 0.9800 . C23 C25 1.53(2) . C24 H24A 0.9800 . C24 H24B 0.9800 . C24 H24C 0.9800 . C24 C25 1.57(3) . C25 H25 1.0000 . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C26 C28 1.50(3) . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C27 C28 1.51(2) . C28 H28 1.0000 . C29 H29A 0.9800 . C29 H29B 0.9800 . C29 H29C 0.9800 . C29 C31 1.52(2) . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C30 C31 1.52(2) . C31 H31 1.0000 . C32 H32A 0.9900 . C32 H32B 0.9900 . C32 C33 1.507(19) . C33 H33A 0.9900 . C33 H33B 0.9900 . C34 H34A 0.9900 . C34 H34B 0.9900 . C34 C35 1.53(2) . C35 H35A 0.9900 . C35 H35B 0.9900 . C35 C36 1.49(2) . C36 H36A 0.9900 . C36 H36B 0.9900 . C36 C37 1.528(19) . C37 H37A 0.9900 . C37 H37B 0.9900 . C38 H38A 0.9900 . C38 H38B 0.9900 . C38 C39 1.490(17) . C39 H39A 0.9800 . C39 H39B 0.9800 . C39 H39C 0.9800 . C40 H40A 0.9900 . C40 H40B 0.9900 . C40 C41 1.50(2) . C41 H41A 0.9800 . C41 H41B 0.9800 . C41 H41C 0.9800 . C42 H42A 0.9900 . C42 H42B 0.9900 . C42 C43 1.519(18) . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 0.9800 . C44 C45 1.40(2) . C44 C49 1.40(2) . C44 B1 1.64(2) . C45 H45 0.9500 . C45 C46 1.40(2) . C46 H46 0.9500 . C46 C47 1.40(3) . C47 H47 0.9500 . C47 C48 1.40(2) . C48 H48 0.9500 . C48 C49 1.398(19) . C49 H49 0.9500 . C50 C51 1.448(17) . C50 C55 1.437(18) . C50 B1 1.595(18) . C51 H51 0.9500 . C51 C52 1.371(18) . C52 H52 0.9500 . C52 C53 1.344(19) . C53 H53 0.9500 . C53 C54 1.36(2) . C54 H54 0.9500 . C54 C55 1.404(18) . C55 H55 0.9500 . C56 C57 1.38(2) . C56 C61 1.42(2) . C56 B1 1.67(2) . C57 H57 0.9500 . C57 C58 1.43(2) . C58 H58 0.9500 . C58 C59 1.39(3) . C59 H59 0.9500 . C59 C60 1.39(3) . C60 H60 0.9500 . C60 C61 1.40(2) . C61 H61 0.9500 . C62 C63 1.381(17) . C62 C67 1.421(18) . C62 B1 1.655(18) . C63 H63 0.9500 . C63 C64 1.397(17) . C64 H64 0.9500 . C64 C65 1.38(2) . C65 H65 0.9500 . C65 C66 1.368(19) . C66 H66 0.9500 . C66 C67 1.408(18) . C67 H67 0.9500 . O2 C68 1.42(2) . O2 C71 1.418(19) . C68 H68A 0.9900 . C68 H68B 0.9900 . C68 C69 1.48(2) . C69 H69A 0.9900 . C69 H69B 0.9900 . C69 C70 1.46(3) . C70 H70A 0.9900 . C70 H70B 0.9900 . C70 C71 1.48(2) . C71 H71A 0.9900 . C71 H71B 0.9900 . O0AA C2AA 1.38(3) . O0AA C4AA 1.48(3) . C1AA H1AA 0.9900 . C1AA H1AB 0.9900 . C1AA C2AA 1.46(3) . C1AA C3AA 1.49(3) . C2AA H2AA 0.9900 . C2AA H2AB 0.9900 . C4AA H4AA 0.9900 . C4AA H4AB 0.9900 . C4AA C3AA 1.51(3) . C3AA H3AA 0.9900 . C3AA H3AB 0.9900 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Th1 N1 C10 C11 48.0(14) . . . . Th1 N2 C21 C22 57.5(13) . . . . Th1 N3 C32 C33 51.3(13) . . . . Th1 N4 C11 C10 36.2(15) . . . . Th1 N4 C22 C21 32.2(12) . . . . Th1 N4 C33 C32 32.8(12) . . . . Si1 N1 C10 C11 -127.0(11) . . . . Si2 N2 C21 C22 -125.5(10) . . . . Si3 N3 C32 C33 -127.5(10) . . . . O1 C34 C35 C36 -173.5(12) . . . . N1 Si1 C5 C6 -62.2(17) . . . . N1 Si1 C5 C4 167.8(14) . . . . N1 Si1 C8 C7 -69.3(16) . . . . N1 Si1 C8 C9 51.7(19) . . . . N1 C10 C11 N4 -57.0(17) . . . . N2 Si2 C17 C15 -178.2(11) . . . . N2 Si2 C17 C16 52.9(13) . . . . N2 Si2 C20 C18 58.3(12) . . . . N2 Si2 C20 C19 -65.3(13) . . . . N2 C21 C22 N4 -60.1(14) . . . . N3 Si3 C28 C26 -172.8(17) . . . . N3 Si3 C28 C27 -49(2) . . . . N3 C32 C33 N4 -56.8(14) . . . . C3 Si1 N1 Th1 39.8(9) . . . . C3 Si1 N1 C10 -145.7(11) . . . . C3 Si1 C5 C6 61.4(17) . . . . C3 Si1 C5 C4 -68.7(17) . . . . C3 Si1 C8 C7 175.2(15) . . . . C3 Si1 C8 C9 -63.7(19) . . . . C5 Si1 N1 Th1 166.0(8) . . . . C5 Si1 N1 C10 -19.5(13) . . . . C5 Si1 C8 C7 54.7(18) . . . . C5 Si1 C8 C9 175.8(17) . . . . C8 Si1 N1 Th1 -72.4(10) . . . . C8 Si1 N1 C10 102.0(12) . . . . C8 Si1 C5 C6 175.6(16) . . . . C8 Si1 C5 C4 45.6(18) . . . . C11 N4 C22 C21 -86.6(14) . . . . C11 N4 C33 C32 150.4(12) . . . . C14 Si2 N2 Th1 -28.7(9) . . . . C14 Si2 N2 C21 154.7(11) . . . . C14 Si2 C17 C15 61.8(14) . . . . C14 Si2 C17 C16 -67.2(13) . . . . C14 Si2 C20 C18 175.2(10) . . . . C14 Si2 C20 C19 51.5(13) . . . . C17 Si2 N2 Th1 -153.2(7) . . . . C17 Si2 N2 C21 30.2(12) . . . . C17 Si2 C20 C18 -63.3(11) . . . . C17 Si2 C20 C19 173.1(11) . . . . C20 Si2 N2 Th1 89.5(8) . . . . C20 Si2 N2 C21 -87.1(12) . . . . C20 Si2 C17 C15 -56.0(13) . . . . C20 Si2 C17 C16 175.0(12) . . . . C22 N4 C11 C10 155.2(13) . . . . C22 N4 C33 C32 -84.3(13) . . . . C25 Si3 N3 Th1 -93.3(10) . . . . C25 Si3 N3 C32 85.2(11) . . . . C25 Si3 C28 C26 64(2) . . . . C25 Si3 C28 C27 -172.5(18) . . . . C28 Si3 N3 Th1 147.6(10) . . . . C28 Si3 N3 C32 -33.9(13) . . . . C31 Si3 N3 Th1 20.5(9) . . . . C31 Si3 N3 C32 -160.9(9) . . . . C31 Si3 C28 C26 -52(2) . . . . C31 Si3 C28 C27 72(2) . . . . C33 N4 C11 C10 -80.6(15) . . . . C33 N4 C22 C21 148.0(12) . . . . C34 C35 C36 C37 -59.6(18) . . . . C35 C36 C37 N5 -159.0(12) . . . . C37 N5 C38 C39 50.7(14) . . . . C37 N5 C40 C41 -176.1(13) . . . . C37 N5 C42 C43 66.2(15) . . . . C38 N5 C37 C36 57.5(13) . . . . C38 N5 C40 C41 66.4(15) . . . . C38 N5 C42 C43 -175.0(12) . . . . C40 N5 C37 C36 -60.4(14) . . . . C40 N5 C38 C39 167.6(12) . . . . C40 N5 C42 C43 -53.4(17) . . . . C42 N5 C37 C36 176.9(11) . . . . C42 N5 C38 C39 -68.8(15) . . . . C42 N5 C40 C41 -55.4(16) . . . . C44 C45 C46 C47 0(2) . . . . C45 C44 C49 C48 -3.3(18) . . . . C45 C44 B1 C50 147.3(12) . . . . C45 C44 B1 C56 29.8(16) . . . . C45 C44 B1 C62 -90.6(13) . . . . C45 C46 C47 C48 1(2) . . . . C46 C47 C48 C49 -3(2) . . . . C47 C48 C49 C44 4(2) . . . . C49 C44 C45 C46 1.4(19) . . . . C49 C44 B1 C50 -39.7(15) . . . . C49 C44 B1 C56 -157.2(11) . . . . C49 C44 B1 C62 82.3(14) . . . . C50 C51 C52 C53 1(2) . . . . C51 C50 C55 C54 0.0(19) . . . . C51 C50 B1 C44 153.8(12) . . . . C51 C50 B1 C56 -83.6(14) . . . . C51 C50 B1 C62 35.4(17) . . . . C51 C52 C53 C54 -1(2) . . . . C52 C53 C54 C55 0(2) . . . . C53 C54 C55 C50 0(2) . . . . C55 C50 C51 C52 -0.9(19) . . . . C55 C50 B1 C44 -28.3(16) . . . . C55 C50 B1 C56 94.3(15) . . . . C55 C50 B1 C62 -146.7(13) . . . . C56 C57 C58 C59 2(2) . . . . C57 C56 C61 C60 2(2) . . . . C57 C56 B1 C44 -151.0(13) . . . . C57 C56 B1 C50 87.1(15) . . . . C57 C56 B1 C62 -33.1(17) . . . . C57 C58 C59 C60 1(2) . . . . C58 C59 C60 C61 -3(2) . . . . C59 C60 C61 C56 1(2) . . . . C61 C56 C57 C58 -4(2) . . . . C61 C56 B1 C44 36.0(16) . . . . C61 C56 B1 C50 -85.9(14) . . . . C61 C56 B1 C62 153.9(12) . . . . C62 C63 C64 C65 0(2) . . . . C63 C62 C67 C66 5.1(18) . . . . C63 C62 B1 C44 82.9(15) . . . . C63 C62 B1 C50 -155.0(12) . . . . C63 C62 B1 C56 -39.5(16) . . . . C63 C64 C65 C66 2(2) . . . . C64 C65 C66 C67 -1(2) . . . . C65 C66 C67 C62 -2(2) . . . . C67 C62 C63 C64 -4.1(19) . . . . C67 C62 B1 C44 -90.0(14) . . . . C67 C62 B1 C50 32.2(16) . . . . C67 C62 B1 C56 147.7(12) . . . . B1 C44 C45 C46 174.9(12) . . . . B1 C44 C49 C48 -176.8(11) . . . . B1 C50 C51 C52 177.2(11) . . . . B1 C50 C55 C54 -178.1(13) . . . . B1 C56 C57 C58 -177.0(12) . . . . B1 C56 C61 C60 175.6(12) . . . . B1 C62 C63 C64 -177.1(12) . . . . B1 C62 C67 C66 178.2(11) . . . . O2 C68 C69 C70 27(3) . . . . C68 O2 C71 C70 -19(3) . . . . C68 C69 C70 C71 -37(3) . . . . C69 C70 C71 O2 36(2) . . . . C71 O2 C68 C69 -5(3) . . . . O0AA C4AA C3AA C1AA 2(3) . . . . C2AA O0AA C4AA C3AA -17(3) . . . . C2AA C1AA C3AA C4AA 13(3) . . . . C4AA O0AA C2AA C1AA 27(3) . . . . C3AA C1AA C2AA O0AA -25(3) . . . .