data_1 _nottingham_internal_coll_name THBGLE _nottingham_internal_coll_number 11755 _nottingham_internal_coll_client BMG/STL _nottingham_internal_coll_type sphere _nottingham_internal_coll_frame_method \w _nottingham_internal_coll_frame_time 90 _nottingham_internal_coll_frame_width 0.3 _nottingham_internal_coll_user BMG _nottingham_internal_coll_date 10/08/2012 _nottingham_internal_coll_location NOTTS _nottingham_internal_NCS_number ? _nottingham_internal_process_date 15/08/2012 _nottingham_internal_process_user BMG _nottingham_internal_solution_date 15/08/2012 _nottingham_internal_solution_user BMG _nottingham_internal_refinement_date 10/11/2012 _nottingham_internal_refinement_user BMG/WL _nottingham_internal_validation_date 21/11/2014 _nottingham_internal_validation_user pczwl _nottingham_internal_archive_date 21/11/2014 _refine_special_details ; Disordered solvent molecules could not be sensibly modelled, and so the dataset was treated with PLATON SQUEEZE. The removed contribution was assigned as 6 hexane molecules (the solvent used for crystallisation) per unit cell, and these solvent molecules were included in the formula, and the calculation of derived parameters. ; _vrf_CHEMW03_1 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The molecular weight was calculated from the formula, which includes solvent molecules accounted for by PLATON SQUEEZE. ; _vrf_PLAT342_1 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0277 Ang. RESPONSE: This refelcts the relatively poor quality of the dataset. ; _vrf_PLAT976_1 ; PROBLEM: Check Calcd Residual Density 0.98A From N10 -1.60 eA-3 RESPONSE: This refelcts the relatively poor quality of the dataset. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 8 0 ' ' 2 0.214 0.801 -0.005 267 62 '2(C6 H14) ' 3 0.500 0.500 0.500 326 71 '2(C6 H14) ' 4 0.401 -0.054 0.429 19 2 ' ' 5 0.599 0.054 0.571 20 2 ' ' 6 0.786 0.199 0.005 268 62 '2(C6 H14) ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? _audit_creation_date 2014-11-10 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C28 H65 Cl N4 O Si3 Th, C6 H14' _chemical_formula_sum 'C34 H79 Cl N4 O Si3 Th' _chemical_formula_weight 911.77 _chemical_melting_point ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Th' 'Th' -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.481(5) _cell_length_b 20.964(7) _cell_length_c 22.540(7) _cell_angle_alpha 71.861(5) _cell_angle_beta 74.644(5) _cell_angle_gamma 81.898(5) _cell_volume 6257(3) _cell_formula_units_Z 6 _cell_measurement_reflns_used 10738 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 27.07 _cell_measurement_theta_min 2.25 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 3.755 _exptl_absorpt_correction_T_max 0.4306 _exptl_absorpt_correction_T_min 0.2667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2007/2 (Bruker,2007) was used for absorption correction. wR2(int) was 0.0894 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.6194. The \l/2 correction factor is 0.0015. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2808 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_unetI/netI 0.2022 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.917 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 54396 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.917 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 28.086 _diffrn_reflns_theta_min 1.556 _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.366 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.917 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_standards_number . _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 13920 _reflns_number_total 27954 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _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 ? _refine_diff_density_max 2.216 _refine_diff_density_min -3.082 _refine_diff_density_rms 0.248 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1092 _refine_ls_number_reflns 27954 _refine_ls_number_restraints 1107 _refine_ls_R_factor_all 0.1808 _refine_ls_R_factor_gt 0.0838 _refine_ls_restrained_S_all 1.000 _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^)+(0.0795P)^2^+100.6395P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1949 _refine_ls_wR_factor_ref 0.2306 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O3-C81A \\sim O3-C81 with sigma of 0.02 C82A-C81A \\sim C82-C81 with sigma of 0.02 C83-C82A \\sim C83-C82 with sigma of 0.02 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(C81A)=Sof(H81C)=Sof(H81D)=1-FVAR(1) Sof(C81)=Sof(H81A)=Sof(H81B)=FVAR(1) Sof(H83C)=Sof(H83D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=1-FVAR(2) Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H83A)=Sof(H83B)=FVAR(2) 5.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C35(H35A,H35B), C36(H36A,H36B), C43(H43A,H43B), C44(H44A,H44B), C51(H51A, H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C63(H63A,H63B), C64(H64A,H64B), C71(H71A,H71B), C72(H72A,H72B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A, H83B), C83(H83C,H83D), C84(H84A,H84B), C81A(H81C,H81D), C82A(H82C,H82D) 5.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A, H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A, H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C29(H29A,H29B, H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A, H34B,H34C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C46(H46A,H46B, H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C57(H57A, H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B, H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C74(H74A, H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 0.20080(4) 0.33119(3) 0.20442(3) 0.02518(15) Uani 1 1 d . . . . . Cl1 Cl 0.2137(3) 0.2913(2) 0.09787(17) 0.0338(9) Uani 1 1 d . . . . . N1 N 0.0406(9) 0.3380(6) 0.2525(6) 0.027(2) Uani 1 1 d . . . . . Si1 Si -0.0541(3) 0.3576(3) 0.2166(2) 0.0371(11) Uani 1 1 d . . . . . C1 C -0.0083(12) 0.3934(9) 0.1288(8) 0.040(4) Uani 1 1 d . . . . . H1A H 0.0196 0.4362 0.1203 0.060 Uiso 1 1 calc GR . . . . H1B H -0.0612 0.4009 0.1074 0.060 Uiso 1 1 calc GR . . . . H1C H 0.0410 0.3619 0.1124 0.060 Uiso 1 1 calc GR . . . . C2 C -0.1412(14) 0.4232(10) 0.2460(10) 0.056(5) Uani 1 1 d . . . . . H2A H -0.1085 0.4645 0.2355 0.084 Uiso 1 1 calc GR . . . . H2B H -0.1654 0.4065 0.2926 0.084 Uiso 1 1 calc GR . . . . H2C H -0.1950 0.4326 0.2251 0.084 Uiso 1 1 calc GR . . . . C3 C -0.1225(13) 0.2834(10) 0.2318(9) 0.046(3) Uani 1 1 d . . . . . C4 C -0.1707(14) 0.2526(10) 0.3026(9) 0.055(5) Uani 1 1 d . . . . . H4A H -0.1930 0.2885 0.3234 0.083 Uiso 1 1 calc GR . . . . H4B H -0.1244 0.2215 0.3240 0.083 Uiso 1 1 calc GR . . . . H4C H -0.2255 0.2282 0.3056 0.083 Uiso 1 1 calc GR . . . . C5 C -0.0558(13) 0.2273(9) 0.2069(8) 0.048(4) Uani 1 1 d . . . . . H5A H 0.0033 0.2201 0.2222 0.072 Uiso 1 1 calc GR . . . . H5B H -0.0398 0.2412 0.1598 0.072 Uiso 1 1 calc GR . . . . H5C H -0.0889 0.1854 0.2230 0.072 Uiso 1 1 calc GR . . . . C6 C -0.2023(14) 0.3018(11) 0.1950(10) 0.063(5) Uani 1 1 d . . . . . H6A H -0.2466 0.3370 0.2090 0.095 Uiso 1 1 calc GR . . . . H6B H -0.2374 0.2619 0.2037 0.095 Uiso 1 1 calc GR . . . . H6C H -0.1739 0.3182 0.1489 0.095 Uiso 1 1 calc GR . . . . C7 C 0.0236(11) 0.3403(8) 0.3200(7) 0.030(3) Uani 1 1 d . . . . . H7A H 0.0577 0.3009 0.3447 0.036 Uiso 1 1 calc R . . . . H7B H -0.0458 0.3385 0.3406 0.036 Uiso 1 1 calc R . . . . C8 C 0.0594(11) 0.4045(8) 0.3204(8) 0.033(3) Uani 1 1 d . . . . . H8A H 0.0231 0.4442 0.2980 0.040 Uiso 1 1 calc R . . . . H8B H 0.0518 0.4056 0.3651 0.040 Uiso 1 1 calc R . . . . N2 N 0.3223(9) 0.3165(6) 0.2586(6) 0.028(3) Uani 1 1 d . . . . . Si2 Si 0.4344(3) 0.2781(2) 0.2330(2) 0.0340(10) Uani 1 1 d . . . . . C9 C 0.5291(12) 0.3413(9) 0.1992(9) 0.044(4) Uani 1 1 d . . . . . H9A H 0.5909 0.3192 0.1835 0.066 Uiso 1 1 calc GR . . . . H9B H 0.5343 0.3600 0.2330 0.066 Uiso 1 1 calc GR . . . . H9C H 0.5113 0.3776 0.1638 0.066 Uiso 1 1 calc GR . . . . C10 C 0.4254(11) 0.2385(9) 0.1720(8) 0.040(4) Uani 1 1 d . . . . . H10A H 0.3939 0.2708 0.1403 0.060 Uiso 1 1 calc GR . . . . H10B H 0.3877 0.1988 0.1930 0.060 Uiso 1 1 calc GR . . . . H10C H 0.4899 0.2249 0.1503 0.060 Uiso 1 1 calc GR . . . . C11 C 0.4760(12) 0.2028(9) 0.3036(9) 0.041(3) Uani 1 1 d . . . . . C12 C 0.5168(14) 0.2358(10) 0.3437(9) 0.054(5) Uani 1 1 d . . . . . H12A H 0.4682 0.2680 0.3594 0.081 Uiso 1 1 calc GR . . . . H12B H 0.5741 0.2592 0.3167 0.081 Uiso 1 1 calc GR . . . . H12C H 0.5339 0.2008 0.3804 0.081 Uiso 1 1 calc GR . . . . C13 C 0.3965(14) 0.1623(11) 0.3383(10) 0.061(5) Uani 1 1 d . . . . . H13A H 0.3627 0.1567 0.3080 0.091 Uiso 1 1 calc GR . . . . H13B H 0.3525 0.1843 0.3683 0.091 Uiso 1 1 calc GR . . . . H13C H 0.4199 0.1181 0.3622 0.091 Uiso 1 1 calc GR . . . . C14 C 0.5643(13) 0.1683(9) 0.2664(8) 0.046(4) Uani 1 1 d . . . . . H14A H 0.6160 0.1993 0.2470 0.069 Uiso 1 1 calc GR . . . . H14B H 0.5462 0.1560 0.2327 0.069 Uiso 1 1 calc GR . . . . H14C H 0.5866 0.1276 0.2962 0.069 Uiso 1 1 calc GR . . . . C15 C 0.3220(11) 0.3589(8) 0.3017(7) 0.028(3) Uani 1 1 d . . . . . H15A H 0.3577 0.3336 0.3346 0.033 Uiso 1 1 calc R . . . . H15B H 0.3556 0.4002 0.2758 0.033 Uiso 1 1 calc R . . . . C16 C 0.2252(11) 0.3777(8) 0.3335(7) 0.034(3) Uani 1 1 d . . . . . H16A H 0.2279 0.4125 0.3542 0.040 Uiso 1 1 calc R . . . . H16B H 0.1972 0.3379 0.3675 0.040 Uiso 1 1 calc R . . . . N3 N 0.2193(9) 0.4450(7) 0.1474(6) 0.031(2) Uani 1 1 d . . . . . Si3 Si 0.3027(3) 0.4795(2) 0.0800(2) 0.0308(10) Uani 1 1 d . . . . . C17 C 0.3718(11) 0.5393(9) 0.0971(7) 0.035(3) Uani 1 1 d . . . . . H17A H 0.3836 0.5200 0.1402 0.052 Uiso 1 1 calc GR . . . . H17B H 0.3343 0.5824 0.0948 0.052 Uiso 1 1 calc GR . . . . H17C H 0.4332 0.5465 0.0653 0.052 Uiso 1 1 calc GR . . . . C18 C 0.3920(11) 0.4140(8) 0.0568(7) 0.034(3) Uani 1 1 d . . . . . H18A H 0.3593 0.3802 0.0494 0.051 Uiso 1 1 calc GR . . . . H18B H 0.4252 0.3923 0.0913 0.051 Uiso 1 1 calc GR . . . . H18C H 0.4387 0.4346 0.0173 0.051 Uiso 1 1 calc GR . . . . C19 C 0.2518(11) 0.5265(8) 0.0072(7) 0.030(3) Uani 1 1 d . . . . . C20 C 0.2208(12) 0.4759(9) -0.0177(7) 0.039(4) Uani 1 1 d . . . . . H20A H 0.1689 0.4509 0.0151 0.059 Uiso 1 1 calc GR . . . . H20B H 0.2754 0.4444 -0.0277 0.059 Uiso 1 1 calc GR . . . . H20C H 0.1980 0.4993 -0.0566 0.059 Uiso 1 1 calc GR . . . . C21 C 0.3304(12) 0.5668(9) -0.0474(7) 0.040(4) Uani 1 1 d . . . . . H21A H 0.3873 0.5368 -0.0562 0.061 Uiso 1 1 calc GR . . . . H21B H 0.3475 0.6031 -0.0341 0.061 Uiso 1 1 calc GR . . . . H21C H 0.3060 0.5862 -0.0863 0.061 Uiso 1 1 calc GR . . . . C22 C 0.1669(12) 0.5746(9) 0.0250(8) 0.042(4) Uani 1 1 d . . . . . H22A H 0.1109 0.5489 0.0502 0.064 Uiso 1 1 calc GR . . . . H22B H 0.1521 0.6061 -0.0142 0.064 Uiso 1 1 calc GR . . . . H22C H 0.1833 0.5997 0.0506 0.064 Uiso 1 1 calc GR . . . . C23 C 0.1621(12) 0.4915(8) 0.1817(7) 0.031(3) Uani 1 1 d . . . . . H23A H 0.0929 0.4863 0.1882 0.038 Uiso 1 1 calc R . . . . H23B H 0.1758 0.5384 0.1561 0.038 Uiso 1 1 calc R . . . . C24 C 0.1873(12) 0.4763(8) 0.2474(7) 0.032(3) Uani 1 1 d . . . . . H24A H 0.2566 0.4811 0.2411 0.039 Uiso 1 1 calc R . . . . H24B H 0.1505 0.5085 0.2706 0.039 Uiso 1 1 calc R . . . . N4 N 0.1622(9) 0.4044(7) 0.2865(5) 0.029(2) Uani 1 1 d . . . . . O1 O 0.1859(8) 0.2000(5) 0.2539(5) 0.030(2) Uani 1 1 d . . . . . C25 C 0.1980(12) 0.1440(7) 0.2272(7) 0.033(3) Uani 1 1 d . . . . . H25A H 0.2669 0.1298 0.2152 0.040 Uiso 1 1 calc R . . . . H25B H 0.1719 0.1569 0.1885 0.040 Uiso 1 1 calc R . . . . C26 C 0.1440(15) 0.0875(9) 0.2788(8) 0.048(4) Uani 1 1 d . . . . . H26A H 0.1749 0.0430 0.2758 0.057 Uiso 1 1 calc R . . . . H26B H 0.0765 0.0899 0.2760 0.057 Uiso 1 1 calc R . . . . C27 C 0.1507(15) 0.1007(9) 0.3405(8) 0.045(4) Uani 1 1 d . . . . . H27A H 0.0980 0.0807 0.3771 0.054 Uiso 1 1 calc R . . . . H27B H 0.2130 0.0827 0.3514 0.054 Uiso 1 1 calc R . . . . C28 C 0.1416(13) 0.1762(8) 0.3231(7) 0.037(4) Uani 1 1 d . . . . . H28A H 0.0732 0.1926 0.3322 0.045 Uiso 1 1 calc R . . . . H28B H 0.1752 0.1925 0.3480 0.045 Uiso 1 1 calc R . . . . Th2 Th 0.09511(4) 0.20593(3) 0.59312(3) 0.02821(16) Uani 1 1 d . . . . . Cl2 Cl 0.1426(3) 0.2207(2) 0.46350(17) 0.0349(9) Uani 1 1 d . . . . . N5 N -0.0591(10) 0.1762(7) 0.6088(6) 0.037(3) Uani 1 1 d . . . . . Si4 Si -0.1464(3) 0.2157(3) 0.5664(2) 0.0351(11) Uani 1 1 d . . . . . C29 C -0.2594(13) 0.2401(10) 0.6204(8) 0.046(4) Uani 1 1 d . . . . . H29A H -0.2449 0.2706 0.6416 0.069 Uiso 1 1 calc GR . . . . H29B H -0.2861 0.1997 0.6530 0.069 Uiso 1 1 calc GR . . . . H29C H -0.3061 0.2628 0.5949 0.069 Uiso 1 1 calc GR . . . . C30 C -0.1013(13) 0.2946(9) 0.5060(8) 0.044(4) Uani 1 1 d . . . . . H30A H -0.0395 0.2845 0.4787 0.067 Uiso 1 1 calc GR . . . . H30B H -0.0930 0.3262 0.5280 0.067 Uiso 1 1 calc GR . . . . H30C H -0.1475 0.3146 0.4794 0.067 Uiso 1 1 calc GR . . . . C31 C -0.1786(12) 0.1607(9) 0.5222(7) 0.035(3) Uani 1 1 d . . . . . C32 C -0.2042(14) 0.0914(9) 0.5672(8) 0.048(4) Uani 1 1 d . . . . . H32A H -0.2631 0.0956 0.5997 0.072 Uiso 1 1 calc GR . . . . H32B H -0.1518 0.0709 0.5883 0.072 Uiso 1 1 calc GR . . . . H32C H -0.2144 0.0630 0.5425 0.072 Uiso 1 1 calc GR . . . . C33 C -0.2657(12) 0.1958(10) 0.4929(8) 0.044(4) Uani 1 1 d . . . . . H33A H -0.3193 0.2048 0.5269 0.066 Uiso 1 1 calc GR . . . . H33B H -0.2856 0.1663 0.4729 0.066 Uiso 1 1 calc GR . . . . H33C H -0.2469 0.2383 0.4604 0.066 Uiso 1 1 calc GR . . . . C34 C -0.0941(12) 0.1534(9) 0.4666(7) 0.037(4) Uani 1 1 d . . . . . H34A H -0.0456 0.1202 0.4833 0.056 Uiso 1 1 calc GR . . . . H34B H -0.0659 0.1969 0.4447 0.056 Uiso 1 1 calc GR . . . . H34C H -0.1169 0.1386 0.4361 0.056 Uiso 1 1 calc GR . . . . C35 C -0.0946(13) 0.1268(9) 0.6715(7) 0.043(4) Uani 1 1 d . . . . . H35A H -0.0551 0.0839 0.6739 0.051 Uiso 1 1 calc R . . . . H35B H -0.1617 0.1179 0.6756 0.051 Uiso 1 1 calc R . . . . C36 C -0.0899(13) 0.1536(10) 0.7272(8) 0.045(4) Uani 1 1 d . . . . . H36A H -0.1292 0.1965 0.7252 0.054 Uiso 1 1 calc R . . . . H36B H -0.1151 0.1207 0.7690 0.054 Uiso 1 1 calc R . . . . N6 N 0.0595(9) 0.2963(7) 0.6373(6) 0.032(3) Uani 1 1 d . . . . . Si5 Si 0.0626(4) 0.3789(3) 0.5915(2) 0.0426(12) Uani 1 1 d . . . . . C37 C 0.1084(13) 0.3803(8) 0.5053(7) 0.036(4) Uani 1 1 d . . . . . H37A H 0.0570 0.3700 0.4896 0.053 Uiso 1 1 calc GR . . . . H37B H 0.1623 0.3467 0.5014 0.053 Uiso 1 1 calc GR . . . . H37C H 0.1301 0.4251 0.4797 0.053 Uiso 1 1 calc GR . . . . C38 C -0.0622(15) 0.4230(10) 0.6027(9) 0.058(5) Uani 1 1 d . . . . . H38A H -0.0727 0.4441 0.6373 0.087 Uiso 1 1 calc GR . . . . H38B H -0.1104 0.3901 0.6138 0.087 Uiso 1 1 calc GR . . . . H38C H -0.0680 0.4576 0.5627 0.087 Uiso 1 1 calc GR . . . . C39 C 0.1446(15) 0.4293(9) 0.6090(9) 0.049(3) Uani 1 1 d . . . . . C40 C 0.2478(14) 0.4011(9) 0.5941(9) 0.050(4) Uani 1 1 d . . . . . H40A H 0.2638 0.3942 0.5514 0.075 Uiso 1 1 calc GR . . . . H40B H 0.2556 0.3581 0.6263 0.075 Uiso 1 1 calc GR . . . . H40C H 0.2907 0.4329 0.5950 0.075 Uiso 1 1 calc GR . . . . C41 C 0.1195(17) 0.4264(10) 0.6810(9) 0.063(5) Uani 1 1 d . . . . . H41A H 0.1231 0.3795 0.7072 0.095 Uiso 1 1 calc GR . . . . H41B H 0.0544 0.4464 0.6926 0.095 Uiso 1 1 calc GR . . . . H41C H 0.1652 0.4516 0.6886 0.095 Uiso 1 1 calc GR . . . . C42 C 0.1352(16) 0.5048(9) 0.5699(9) 0.053(5) Uani 1 1 d . . . . . H42A H 0.0686 0.5225 0.5813 0.080 Uiso 1 1 calc GR . . . . H42B H 0.1535 0.5088 0.5238 0.080 Uiso 1 1 calc GR . . . . H42C H 0.1775 0.5305 0.5799 0.080 Uiso 1 1 calc GR . . . . C43 C 0.0000(13) 0.2851(9) 0.7034(8) 0.044(4) Uani 1 1 d . . . . . H43A H -0.0685 0.2891 0.7023 0.052 Uiso 1 1 calc R . . . . H43B H 0.0104 0.3207 0.7209 0.052 Uiso 1 1 calc R . . . . C44 C 0.0215(13) 0.2185(9) 0.7470(8) 0.042(4) Uani 1 1 d . . . . . H44A H 0.0874 0.2162 0.7528 0.051 Uiso 1 1 calc R . . . . H44B H -0.0236 0.2126 0.7896 0.051 Uiso 1 1 calc R . . . . N7 N 0.1619(10) 0.1052(7) 0.6439(6) 0.034(3) Uani 1 1 d . . . . . Si6 Si 0.1840(4) 0.0328(2) 0.6194(2) 0.0379(11) Uani 1 1 d . . . . . C45 C 0.1413(16) -0.0409(9) 0.6862(9) 0.060(5) Uani 1 1 d . . . . . H45A H 0.0717 -0.0348 0.7021 0.090 Uiso 1 1 calc GR . . . . H45B H 0.1731 -0.0461 0.7209 0.090 Uiso 1 1 calc GR . . . . H45C H 0.1562 -0.0812 0.6713 0.090 Uiso 1 1 calc GR . . . . C46 C 0.1166(14) 0.0425(9) 0.5566(8) 0.045(4) Uani 1 1 d . . . . . H46A H 0.1455 0.0763 0.5172 0.068 Uiso 1 1 calc GR . . . . H46B H 0.0495 0.0569 0.5721 0.068 Uiso 1 1 calc GR . . . . H46C H 0.1195 -0.0006 0.5476 0.068 Uiso 1 1 calc GR . . . . C47 C 0.3167(13) 0.0162(9) 0.5827(9) 0.044(3) Uani 1 1 d . . . . . C48 C 0.3750(14) 0.0174(9) 0.6290(9) 0.052(4) Uani 1 1 d . . . . . H48A H 0.3675 0.0622 0.6351 0.077 Uiso 1 1 calc GR . . . . H48B H 0.4428 0.0065 0.6114 0.077 Uiso 1 1 calc GR . . . . H48C H 0.3524 -0.0159 0.6703 0.077 Uiso 1 1 calc GR . . . . C49 C 0.3492(14) 0.0728(9) 0.5207(9) 0.051(4) Uani 1 1 d . . . . . H49A H 0.3300 0.1164 0.5291 0.076 Uiso 1 1 calc GR . . . . H49B H 0.3193 0.0696 0.4876 0.076 Uiso 1 1 calc GR . . . . H49C H 0.4192 0.0684 0.5058 0.076 Uiso 1 1 calc GR . . . . C50 C 0.3327(15) -0.0514(10) 0.5688(10) 0.060(5) Uani 1 1 d . . . . . H50A H 0.2879 -0.0538 0.5439 0.090 Uiso 1 1 calc GR . . . . H50B H 0.3220 -0.0874 0.6094 0.090 Uiso 1 1 calc GR . . . . H50C H 0.3987 -0.0565 0.5442 0.090 Uiso 1 1 calc GR . . . . C51 C 0.1659(12) 0.0983(9) 0.7121(8) 0.038(3) Uani 1 1 d . . . . . H51A H 0.2002 0.1353 0.7131 0.045 Uiso 1 1 calc R . . . . H51B H 0.1998 0.0550 0.7301 0.045 Uiso 1 1 calc R . . . . C52 C 0.0599(13) 0.1011(10) 0.7514(8) 0.048(4) Uani 1 1 d . . . . . H52A H 0.0267 0.0626 0.7520 0.058 Uiso 1 1 calc R . . . . H52B H 0.0581 0.0987 0.7962 0.058 Uiso 1 1 calc R . . . . N8 N 0.0128(10) 0.1642(7) 0.7207(6) 0.038(3) Uani 1 1 d . . . . . O2 O 0.2756(8) 0.2406(6) 0.5573(5) 0.034(2) Uani 1 1 d . . . . . C53 C 0.3270(12) 0.2229(9) 0.6070(7) 0.035(4) Uani 1 1 d . . . . . H53A H 0.3364 0.1734 0.6236 0.042 Uiso 1 1 calc R . . . . H53B H 0.2914 0.2408 0.6430 0.042 Uiso 1 1 calc R . . . . C54 C 0.4224(13) 0.2540(10) 0.5764(8) 0.046(4) Uani 1 1 d . . . . . H54A H 0.4731 0.2281 0.5979 0.056 Uiso 1 1 calc R . . . . H54B H 0.4183 0.3012 0.5773 0.056 Uiso 1 1 calc R . . . . C55 C 0.4406(14) 0.2496(12) 0.5085(9) 0.059(5) Uani 1 1 d . . . . . H55A H 0.4850 0.2836 0.4784 0.071 Uiso 1 1 calc R . . . . H55B H 0.4683 0.2043 0.5058 0.071 Uiso 1 1 calc R . . . . C56 C 0.3437(12) 0.2631(10) 0.4937(7) 0.047(4) Uani 1 1 d . . . . . H56A H 0.3314 0.3115 0.4731 0.056 Uiso 1 1 calc R . . . . H56B H 0.3382 0.2373 0.4649 0.056 Uiso 1 1 calc R . . . . Th3 Th 0.34638(4) 0.22050(3) 0.87057(3) 0.02665(15) Uani 1 1 d . . . . . Cl3 Cl 0.2723(3) 0.2287(2) 0.76880(18) 0.0375(10) Uani 1 1 d . . . . . N9 N 0.4719(9) 0.1401(7) 0.8528(6) 0.030(2) Uani 1 1 d . . . . . Si7 Si 0.4649(3) 0.0665(2) 0.8394(2) 0.0324(10) Uani 1 1 d . . . . . C57 C 0.4988(14) -0.0055(9) 0.9049(8) 0.047(4) Uani 1 1 d . . . . . H57A H 0.4647 0.0009 0.9467 0.070 Uiso 1 1 calc GR . . . . H57B H 0.5682 -0.0075 0.9008 0.070 Uiso 1 1 calc GR . . . . H57C H 0.4814 -0.0475 0.9016 0.070 Uiso 1 1 calc GR . . . . C58 C 0.3390(12) 0.0591(9) 0.8386(8) 0.044(4) Uani 1 1 d . . . . . H58A H 0.3196 0.0968 0.8048 0.065 Uiso 1 1 calc GR . . . . H58B H 0.2968 0.0600 0.8803 0.065 Uiso 1 1 calc GR . . . . H58C H 0.3340 0.0167 0.8304 0.065 Uiso 1 1 calc GR . . . . C59 C 0.5452(12) 0.0578(9) 0.7613(7) 0.036(3) Uani 1 1 d . . . . . C60 C 0.6511(12) 0.0644(10) 0.7574(8) 0.044(4) Uani 1 1 d . . . . . H60A H 0.6712 0.0302 0.7933 0.066 Uiso 1 1 calc GR . . . . H60B H 0.6590 0.1092 0.7596 0.066 Uiso 1 1 calc GR . . . . H60C H 0.6906 0.0581 0.7168 0.066 Uiso 1 1 calc GR . . . . C61 C 0.5365(15) -0.0101(9) 0.7524(9) 0.052(4) Uani 1 1 d . . . . . H61A H 0.4692 -0.0155 0.7553 0.077 Uiso 1 1 calc GR . . . . H61B H 0.5592 -0.0462 0.7861 0.077 Uiso 1 1 calc GR . . . . H61C H 0.5754 -0.0123 0.7102 0.077 Uiso 1 1 calc GR . . . . C62 C 0.5197(13) 0.1146(8) 0.7037(8) 0.039(4) Uani 1 1 d . . . . . H62A H 0.5581 0.1068 0.6634 0.059 Uiso 1 1 calc GR . . . . H62B H 0.5336 0.1581 0.7060 0.059 Uiso 1 1 calc GR . . . . H62C H 0.4514 0.1149 0.7053 0.059 Uiso 1 1 calc GR . . . . C63 C 0.5583(11) 0.1472(8) 0.8739(7) 0.030(3) Uani 1 1 d . . . . . H63A H 0.5886 0.1893 0.8462 0.036 Uiso 1 1 calc R . . . . H63B H 0.6057 0.1090 0.8696 0.036 Uiso 1 1 calc R . . . . C64 C 0.5293(11) 0.1487(8) 0.9443(7) 0.029(3) Uani 1 1 d . . . . . H64A H 0.4990 0.1067 0.9720 0.035 Uiso 1 1 calc R . . . . H64B H 0.5870 0.1519 0.9586 0.035 Uiso 1 1 calc R . . . . N10 N 0.4301(9) 0.3151(6) 0.8456(6) 0.032(3) Uani 1 1 d . . . . . Si8 Si 0.4946(4) 0.3594(3) 0.7709(2) 0.0410(12) Uani 1 1 d . . . . . C65 C 0.4991(14) 0.3138(10) 0.7123(8) 0.051(5) Uani 1 1 d . . . . . H65A H 0.4337 0.3057 0.7131 0.076 Uiso 1 1 calc GR . . . . H65B H 0.5361 0.2707 0.7234 0.076 Uiso 1 1 calc GR . . . . H65C H 0.5298 0.3408 0.6692 0.076 Uiso 1 1 calc GR . . . . C66 C 0.6232(13) 0.3615(9) 0.7717(9) 0.051(4) Uani 1 1 d . . . . . H66A H 0.6525 0.3155 0.7816 0.077 Uiso 1 1 calc GR . . . . H66B H 0.6266 0.3823 0.8043 0.077 Uiso 1 1 calc GR . . . . H66C H 0.6579 0.3878 0.7294 0.077 Uiso 1 1 calc GR . . . . C67 C 0.4404(15) 0.4479(10) 0.7432(10) 0.057(4) Uani 1 1 d . . . . . C68 C 0.4147(15) 0.4815(10) 0.7985(10) 0.057(5) Uani 1 1 d . . . . . H68A H 0.4735 0.4868 0.8097 0.085 Uiso 1 1 calc GR . . . . H68B H 0.3724 0.4533 0.8361 0.085 Uiso 1 1 calc GR . . . . H68C H 0.3819 0.5258 0.7844 0.085 Uiso 1 1 calc GR . . . . C69 C 0.5099(19) 0.4900(12) 0.6861(12) 0.090(6) Uani 1 1 d . . . . . H69A H 0.4959 0.5376 0.6841 0.135 Uiso 1 1 calc GR . . . . H69B H 0.5029 0.4831 0.6465 0.135 Uiso 1 1 calc GR . . . . H69C H 0.5758 0.4764 0.6908 0.135 Uiso 1 1 calc GR . . . . C70 C 0.3482(15) 0.4448(10) 0.7260(11) 0.063(5) Uani 1 1 d . . . . . H70A H 0.3357 0.4865 0.6936 0.094 Uiso 1 1 calc GR . . . . H70B H 0.2954 0.4391 0.7644 0.094 Uiso 1 1 calc GR . . . . H70C H 0.3532 0.4066 0.7087 0.094 Uiso 1 1 calc GR . . . . C71 C 0.4490(12) 0.3268(8) 0.9028(8) 0.037(3) Uani 1 1 d . . . . . H71A H 0.3878 0.3305 0.9344 0.044 Uiso 1 1 calc R . . . . H71B H 0.4810 0.3694 0.8901 0.044 Uiso 1 1 calc R . . . . C72 C 0.5119(12) 0.2695(8) 0.9321(8) 0.035(3) Uani 1 1 d . . . . . H72A H 0.5738 0.2663 0.9010 0.042 Uiso 1 1 calc R . . . . H72B H 0.5249 0.2761 0.9707 0.042 Uiso 1 1 calc R . . . . N11 N 0.2741(9) 0.1616(6) 0.9742(6) 0.029(2) Uani 1 1 d . . . . . Si9 Si 0.1595(3) 0.1332(3) 1.0009(2) 0.0374(11) Uani 1 1 d . . . . . C73 C 0.0727(12) 0.1857(10) 1.0459(8) 0.047(4) Uani 1 1 d . . . . . H73A H 0.0553 0.2278 1.0157 0.070 Uiso 1 1 calc GR . . . . H73B H 0.1020 0.1957 1.0762 0.070 Uiso 1 1 calc GR . . . . H73C H 0.0150 0.1612 1.0695 0.070 Uiso 1 1 calc GR . . . . C74 C 0.1146(13) 0.1353(11) 0.9286(8) 0.052(5) Uani 1 1 d . . . . . H74A H 0.1442 0.0967 0.9130 0.078 Uiso 1 1 calc GR . . . . H74B H 0.1318 0.1771 0.8946 0.078 Uiso 1 1 calc GR . . . . H74C H 0.0447 0.1331 0.9409 0.078 Uiso 1 1 calc GR . . . . C75 C 0.1531(16) 0.0435(10) 1.0562(9) 0.057(4) Uani 1 1 d . . . . . C76 C 0.2357(18) -0.0037(11) 1.0274(10) 0.073(5) Uani 1 1 d . . . . . H76A H 0.2299 -0.0500 1.0553 0.110 Uiso 1 1 calc GR . . . . H76B H 0.2981 0.0116 1.0244 0.110 Uiso 1 1 calc GR . . . . H76C H 0.2304 -0.0020 0.9845 0.110 Uiso 1 1 calc GR . . . . C77 C 0.1598(16) 0.0384(11) 1.1261(8) 0.060(5) Uani 1 1 d . . . . . H77A H 0.1497 -0.0077 1.1536 0.091 Uiso 1 1 calc GR . . . . H77B H 0.1105 0.0693 1.1434 0.091 Uiso 1 1 calc GR . . . . H77C H 0.2234 0.0505 1.1248 0.091 Uiso 1 1 calc GR . . . . C78 C 0.0559(18) 0.0166(13) 1.0629(10) 0.081(6) Uani 1 1 d . . . . . H78A H 0.0562 0.0061 1.0234 0.122 Uiso 1 1 calc GR . . . . H78B H 0.0042 0.0508 1.0703 0.122 Uiso 1 1 calc GR . . . . H78C H 0.0455 -0.0242 1.0993 0.122 Uiso 1 1 calc GR . . . . C79 C 0.3209(10) 0.1465(8) 1.0303(7) 0.027(3) Uani 1 1 d . . . . . H79A H 0.3519 0.1004 1.0382 0.033 Uiso 1 1 calc R . . . . H79B H 0.2715 0.1490 1.0696 0.033 Uiso 1 1 calc R . . . . C80 C 0.3959(11) 0.1973(8) 1.0156(7) 0.030(3) Uani 1 1 d . . . . . H80A H 0.3627 0.2410 1.0191 0.036 Uiso 1 1 calc R . . . . H80B H 0.4349 0.1816 1.0480 0.036 Uiso 1 1 calc R . . . . N12 N 0.4611(8) 0.2072(6) 0.9500(6) 0.027(2) Uani 1 1 d . . . . . O3 O 0.1958(7) 0.3005(6) 0.8853(5) 0.035(2) Uani 1 1 d . . . . . C81 C 0.134(4) 0.337(3) 0.838(2) 0.034(10) Uani 0.42(9) 1 d . . P A 1 H81A H 0.1136 0.3059 0.8194 0.040 Uiso 0.42(9) 1 calc R . P A 1 H81B H 0.1686 0.3734 0.8023 0.040 Uiso 0.42(9) 1 calc R . P A 1 C82 C 0.046(5) 0.367(7) 0.880(5) 0.054(18) Uani 0.35(15) 1 d . . P A 1 H82A H 0.0209 0.4107 0.8546 0.065 Uiso 0.35(15) 1 calc R . P A 1 H82B H -0.0062 0.3358 0.8985 0.065 Uiso 0.35(15) 1 calc R . P A 1 C83 C 0.0853(13) 0.3770(10) 0.9324(9) 0.047(4) Uani 1 1 d . . . . . H83A H 0.0431 0.3574 0.9750 0.057 Uiso 0.35(15) 1 calc R . P A 1 H83B H 0.0884 0.4255 0.9264 0.057 Uiso 0.35(15) 1 calc R . P A 1 H83C H 0.0371 0.3493 0.9671 0.057 Uiso 0.65(15) 1 calc R . P A 2 H83D H 0.0834 0.4215 0.9395 0.057 Uiso 0.65(15) 1 calc R . P A 2 C84 C 0.1855(12) 0.3419(10) 0.9283(9) 0.047(5) Uani 1 1 d . . . . . H84A H 0.2349 0.3754 0.9110 0.056 Uiso 1 1 calc R . . . . H84B H 0.1926 0.3136 0.9713 0.056 Uiso 1 1 calc R . . . . C81A C 0.106(3) 0.313(3) 0.858(3) 0.041(9) Uani 0.58(9) 1 d . . P A 2 H81C H 0.0591 0.2790 0.8826 0.049 Uiso 0.58(9) 1 calc R . P A 2 H81D H 0.1231 0.3141 0.8120 0.049 Uiso 0.58(9) 1 calc R . P A 2 C82A C 0.069(5) 0.384(2) 0.867(2) 0.049(9) Uani 0.65(15) 1 d . . P A 2 H82C H 0.1067 0.4198 0.8330 0.059 Uiso 0.65(15) 1 calc R . P A 2 H82D H 0.0005 0.3933 0.8663 0.059 Uiso 0.65(15) 1 calc R . 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 Th1 0.0269(3) 0.0325(3) 0.0183(3) -0.0103(2) -0.0078(2) 0.0028(3) Cl1 0.038(2) 0.048(3) 0.0201(18) -0.0155(17) -0.0100(16) 0.0047(19) N1 0.029(5) 0.023(6) 0.028(5) -0.003(4) -0.011(4) 0.004(4) Si1 0.028(2) 0.048(3) 0.033(2) -0.007(2) -0.0127(19) 0.002(2) C1 0.039(8) 0.042(9) 0.040(6) -0.007(5) -0.020(5) 0.004(7) C2 0.049(9) 0.059(9) 0.059(10) -0.018(8) -0.019(8) 0.014(7) C3 0.040(7) 0.051(7) 0.044(7) -0.005(5) -0.016(5) -0.003(5) C4 0.058(10) 0.053(10) 0.047(7) -0.002(6) -0.009(6) -0.012(8) C5 0.051(9) 0.051(8) 0.038(9) -0.002(7) -0.017(7) -0.002(7) C6 0.052(9) 0.068(12) 0.073(11) -0.006(9) -0.035(8) -0.005(8) C7 0.027(7) 0.033(7) 0.028(5) -0.009(5) -0.007(5) 0.003(5) C8 0.035(6) 0.033(7) 0.032(7) -0.010(5) -0.008(5) 0.002(5) N2 0.035(5) 0.032(6) 0.023(5) -0.013(5) -0.017(4) 0.007(4) Si2 0.036(2) 0.036(3) 0.035(2) -0.014(2) -0.016(2) 0.003(2) C9 0.033(7) 0.049(8) 0.052(9) -0.012(7) -0.017(6) -0.003(6) C10 0.023(8) 0.056(10) 0.049(8) -0.024(7) -0.019(6) 0.009(7) C11 0.037(7) 0.044(7) 0.049(6) -0.019(5) -0.024(5) 0.014(5) C12 0.052(10) 0.071(11) 0.053(9) -0.030(8) -0.031(8) 0.017(8) C13 0.054(8) 0.067(10) 0.055(9) -0.003(8) -0.020(7) -0.001(7) C14 0.050(8) 0.051(9) 0.041(8) -0.015(7) -0.024(6) 0.013(7) C15 0.040(6) 0.024(7) 0.028(6) -0.014(6) -0.021(5) 0.011(5) C16 0.041(6) 0.038(8) 0.029(6) -0.016(5) -0.019(5) 0.013(5) N3 0.037(6) 0.036(5) 0.020(4) -0.009(4) -0.008(4) -0.002(4) Si3 0.033(2) 0.037(3) 0.023(2) -0.0089(18) -0.0079(18) 0.0012(19) C17 0.036(8) 0.048(8) 0.019(7) -0.011(6) -0.002(6) -0.006(6) C18 0.031(7) 0.040(7) 0.025(7) -0.008(6) 0.001(6) -0.003(6) C19 0.029(6) 0.042(6) 0.015(5) -0.006(4) -0.002(4) -0.003(5) C20 0.043(9) 0.051(8) 0.024(7) -0.011(6) -0.009(6) -0.003(7) C21 0.040(7) 0.048(9) 0.022(6) 0.000(6) -0.001(5) 0.000(6) C22 0.043(7) 0.060(9) 0.024(7) -0.015(7) -0.011(6) 0.011(6) C23 0.044(8) 0.034(7) 0.018(5) -0.009(5) -0.008(5) 0.000(5) C24 0.035(8) 0.043(6) 0.020(5) -0.013(4) -0.006(5) 0.001(5) N4 0.029(5) 0.040(5) 0.019(4) -0.008(4) -0.008(4) 0.002(4) O1 0.044(6) 0.027(4) 0.021(4) -0.011(3) -0.010(4) 0.004(4) C25 0.049(9) 0.022(6) 0.029(6) -0.012(5) -0.009(6) 0.008(5) C26 0.076(12) 0.036(7) 0.034(7) -0.014(5) -0.012(7) -0.008(7) C27 0.070(12) 0.035(7) 0.029(6) -0.008(5) -0.010(6) -0.003(6) C28 0.058(10) 0.033(6) 0.020(5) -0.009(4) -0.008(5) 0.000(6) Th2 0.0407(4) 0.0291(3) 0.0183(3) -0.0076(2) -0.0126(3) -0.0008(3) Cl2 0.055(3) 0.038(2) 0.0182(18) -0.0119(16) -0.0129(17) -0.005(2) N5 0.043(5) 0.043(6) 0.027(5) -0.011(4) -0.014(4) -0.004(4) Si4 0.040(3) 0.048(3) 0.025(2) -0.016(2) -0.0144(19) 0.002(2) C29 0.051(7) 0.060(11) 0.033(7) -0.018(7) -0.017(6) 0.007(7) C30 0.057(10) 0.044(7) 0.041(7) -0.019(6) -0.019(7) -0.001(6) C31 0.037(6) 0.046(7) 0.025(6) -0.013(5) -0.012(5) 0.004(5) C32 0.063(10) 0.051(7) 0.034(7) -0.011(6) -0.021(7) -0.004(6) C33 0.040(7) 0.062(10) 0.033(8) -0.016(7) -0.017(6) 0.008(7) C34 0.041(7) 0.049(10) 0.030(6) -0.019(6) -0.015(5) 0.001(6) C35 0.050(8) 0.055(8) 0.025(5) -0.003(5) -0.016(5) -0.011(7) C36 0.048(6) 0.062(10) 0.023(6) -0.004(6) -0.013(5) -0.008(6) N6 0.046(6) 0.035(5) 0.025(4) -0.017(3) -0.023(4) 0.008(4) Si5 0.070(3) 0.036(3) 0.033(2) -0.018(2) -0.030(2) 0.015(2) C37 0.059(10) 0.022(8) 0.034(6) -0.014(5) -0.019(6) -0.001(7) C38 0.078(8) 0.061(11) 0.040(9) -0.021(8) -0.029(7) 0.025(7) C39 0.080(8) 0.036(7) 0.045(7) -0.020(5) -0.037(6) 0.013(5) C40 0.083(8) 0.027(8) 0.059(10) -0.026(8) -0.041(7) 0.010(6) C41 0.106(13) 0.056(11) 0.046(7) -0.024(7) -0.038(7) -0.004(9) C42 0.090(13) 0.036(7) 0.043(8) -0.021(6) -0.029(8) 0.014(6) C43 0.056(9) 0.052(7) 0.033(5) -0.020(5) -0.019(5) 0.001(6) C44 0.043(9) 0.058(6) 0.030(6) -0.017(5) -0.014(6) 0.004(5) N7 0.044(6) 0.033(5) 0.028(5) -0.008(4) -0.016(4) -0.004(4) Si6 0.059(3) 0.024(2) 0.042(3) -0.010(2) -0.031(2) 0.001(2) C45 0.078(12) 0.039(8) 0.059(8) -0.006(6) -0.019(8) -0.005(7) C46 0.066(10) 0.032(9) 0.051(8) -0.017(7) -0.035(8) 0.003(8) C47 0.055(6) 0.035(7) 0.056(7) -0.025(5) -0.026(5) 0.003(5) C48 0.065(10) 0.038(10) 0.069(9) -0.023(8) -0.042(8) 0.008(8) C49 0.057(10) 0.047(8) 0.060(8) -0.025(6) -0.024(6) 0.003(7) C50 0.069(11) 0.051(8) 0.084(12) -0.042(8) -0.038(9) 0.009(7) C51 0.051(7) 0.031(8) 0.038(6) -0.009(5) -0.022(5) 0.001(6) C52 0.054(7) 0.058(7) 0.039(7) -0.016(5) -0.023(5) 0.003(5) N8 0.042(5) 0.048(6) 0.025(5) -0.009(4) -0.011(4) -0.002(4) O2 0.044(5) 0.044(6) 0.019(4) -0.009(4) -0.009(3) -0.012(4) C53 0.044(7) 0.040(9) 0.028(6) -0.012(5) -0.013(5) -0.006(6) C54 0.049(7) 0.065(12) 0.030(7) -0.013(7) -0.011(5) -0.018(7) C55 0.051(7) 0.099(16) 0.038(7) -0.028(8) -0.009(5) -0.024(7) C56 0.047(7) 0.076(12) 0.023(5) -0.014(6) -0.005(5) -0.030(7) Th3 0.0287(3) 0.0338(4) 0.0238(3) -0.0136(3) -0.0129(2) 0.0027(3) Cl3 0.044(2) 0.050(3) 0.026(2) -0.0169(19) -0.0151(18) 0.001(2) N9 0.031(5) 0.042(5) 0.023(5) -0.013(4) -0.013(4) 0.003(4) Si7 0.041(3) 0.035(3) 0.025(2) -0.0088(19) -0.0152(19) 0.000(2) C57 0.067(11) 0.039(7) 0.043(7) -0.008(6) -0.031(8) -0.004(7) C58 0.046(7) 0.045(10) 0.041(9) -0.007(8) -0.019(6) -0.002(6) C59 0.043(6) 0.038(7) 0.026(5) -0.005(5) -0.016(4) 0.007(5) C60 0.047(7) 0.060(11) 0.025(8) -0.010(7) -0.013(5) 0.003(6) C61 0.069(11) 0.045(7) 0.043(9) -0.015(6) -0.019(8) 0.004(7) C62 0.053(10) 0.037(8) 0.031(6) -0.009(5) -0.019(6) 0.003(6) C63 0.026(6) 0.041(8) 0.030(6) -0.021(6) -0.010(5) 0.008(5) C64 0.027(6) 0.038(7) 0.029(6) -0.017(5) -0.010(5) -0.001(5) N10 0.035(6) 0.031(5) 0.038(5) -0.014(4) -0.016(4) -0.001(4) Si8 0.047(3) 0.038(3) 0.042(3) -0.014(2) -0.014(2) -0.004(2) C65 0.064(11) 0.049(10) 0.039(8) -0.018(7) 0.002(7) -0.021(8) C66 0.058(7) 0.038(10) 0.060(11) -0.011(8) -0.017(7) -0.009(6) C67 0.067(8) 0.049(7) 0.062(8) -0.017(5) -0.031(6) 0.003(5) C68 0.063(11) 0.048(10) 0.072(9) -0.025(8) -0.030(8) 0.001(8) C69 0.108(13) 0.068(11) 0.086(10) -0.016(8) -0.014(9) -0.015(9) C70 0.079(9) 0.038(10) 0.088(13) -0.025(9) -0.047(9) 0.014(7) C71 0.037(8) 0.035(6) 0.050(6) -0.020(5) -0.021(6) -0.005(5) C72 0.032(7) 0.038(6) 0.041(7) -0.013(5) -0.014(6) -0.007(5) N11 0.030(5) 0.030(6) 0.030(5) -0.011(4) -0.011(4) 0.001(4) Si9 0.037(3) 0.057(3) 0.022(2) -0.012(2) -0.0073(19) -0.013(2) C73 0.035(8) 0.067(10) 0.040(8) -0.018(8) -0.004(6) -0.011(7) C74 0.040(9) 0.090(13) 0.027(7) -0.012(7) -0.002(6) -0.032(9) C75 0.088(10) 0.058(7) 0.030(6) -0.012(5) -0.018(6) -0.016(6) C76 0.116(12) 0.053(10) 0.044(10) -0.007(8) -0.008(8) -0.017(8) C77 0.080(13) 0.073(12) 0.027(6) 0.000(7) -0.018(7) -0.024(10) C78 0.109(11) 0.097(14) 0.044(10) -0.010(10) -0.022(8) -0.043(9) C79 0.019(6) 0.042(8) 0.022(5) -0.014(5) -0.002(4) 0.000(5) C80 0.029(6) 0.037(7) 0.028(5) -0.016(5) -0.005(4) -0.001(5) N12 0.025(5) 0.035(5) 0.024(4) -0.014(4) -0.005(4) -0.001(4) O3 0.034(5) 0.051(6) 0.030(5) -0.017(4) -0.019(4) 0.002(4) C81 0.029(14) 0.039(19) 0.043(11) -0.014(12) -0.024(11) -0.003(15) C82 0.040(13) 0.08(4) 0.06(2) -0.04(3) -0.027(15) 0.012(19) C83 0.042(8) 0.051(10) 0.061(9) -0.027(8) -0.025(6) 0.008(7) C84 0.038(7) 0.067(10) 0.052(9) -0.037(8) -0.025(7) 0.014(7) C81A 0.037(11) 0.050(15) 0.046(19) -0.019(15) -0.026(13) 0.009(11) C82A 0.042(16) 0.056(14) 0.062(12) -0.028(11) -0.028(12) 0.012(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 Cl1 2.733(4) . ? Th1 N1 2.291(12) . ? Th1 N2 2.332(11) . ? Th1 N3 2.346(13) . ? Th1 N4 2.660(12) . ? Th1 O1 2.642(10) . ? N1 Si1 1.710(12) . ? N1 C7 1.491(18) . ? Si1 C1 1.856(17) . ? Si1 C2 1.886(19) . ? Si1 C3 1.854(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.53(2) . ? C3 C5 1.56(3) . ? C3 C6 1.53(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.51(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 N4 1.482(19) . ? N2 Si2 1.744(13) . ? N2 C15 1.506(17) . ? Si2 C9 1.883(17) . ? Si2 C10 1.854(16) . ? Si2 C11 2.015(17) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.56(2) . ? C11 C13 1.43(3) . ? C11 C14 1.55(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.46(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N4 1.505(17) . ? N3 Si3 1.698(13) . ? N3 C23 1.462(19) . ? Si3 C17 1.891(16) . ? Si3 C18 1.850(16) . ? Si3 C19 1.906(15) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.51(2) . ? C19 C21 1.55(2) . ? C19 C22 1.53(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.546(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 N4 1.53(2) . ? O1 C25 1.448(17) . ? O1 C28 1.473(17) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.51(2) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.53(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.50(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? Th2 Cl2 2.745(4) . ? Th2 N5 2.310(14) . ? Th2 N6 2.340(12) . ? Th2 N7 2.283(13) . ? Th2 N8 2.713(13) . ? Th2 O2 2.657(11) . ? N5 Si4 1.747(14) . ? N5 C35 1.48(2) . ? Si4 C29 1.875(18) . ? Si4 C30 1.857(18) . ? Si4 C31 1.909(17) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.52(2) . ? C31 C33 1.57(2) . ? C31 C34 1.53(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.55(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 N8 1.50(2) . ? N6 Si5 1.717(14) . ? N6 C43 1.48(2) . ? Si5 C37 1.873(16) . ? Si5 C38 1.902(19) . ? Si5 C39 1.883(19) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.52(3) . ? C39 C41 1.55(2) . ? C39 C42 1.56(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.48(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 N8 1.47(2) . ? N7 Si6 1.733(14) . ? N7 C51 1.512(19) . ? Si6 C45 1.835(19) . ? Si6 C46 1.868(16) . ? Si6 C47 1.91(2) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.51(2) . ? C47 C49 1.54(3) . ? C47 C50 1.52(2) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C51 C52 1.56(2) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52 N8 1.46(2) . ? O2 C53 1.433(17) . ? O2 C56 1.486(18) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C53 C54 1.51(2) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54 C55 1.51(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C55 C56 1.50(2) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? Th3 Cl3 2.728(4) . ? Th3 N9 2.340(13) . ? Th3 N10 2.311(13) . ? Th3 N11 2.313(13) . ? Th3 N12 2.679(11) . ? Th3 O3 2.570(11) . ? N9 Si7 1.683(14) . ? N9 C63 1.491(18) . ? Si7 C57 1.868(17) . ? Si7 C58 1.857(17) . ? Si7 C59 1.880(17) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.54(2) . ? C59 C61 1.52(2) . ? C59 C62 1.55(2) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C63 C64 1.539(19) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C64 N12 1.479(19) . ? N10 Si8 1.734(14) . ? N10 C71 1.484(19) . ? Si8 C65 1.840(17) . ? Si8 C66 1.874(19) . ? Si8 C67 1.89(2) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.55(3) . ? C67 C69 1.52(3) . ? C67 C70 1.50(3) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C71 C72 1.49(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C72 N12 1.480(19) . ? N11 Si9 1.730(13) . ? N11 C79 1.518(17) . ? Si9 C73 1.857(18) . ? Si9 C74 1.894(16) . ? Si9 C75 1.90(2) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.58(3) . ? C75 C77 1.57(2) . ? C75 C78 1.54(3) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C79 C80 1.53(2) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C80 N12 1.498(18) . ? O3 C81 1.54(2) . ? O3 C84 1.458(18) . ? O3 C81A 1.54(2) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C81 C82 1.56(4) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C82 C83 1.52(3) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C83 H83C 0.9900 . ? C83 H83D 0.9900 . ? C83 C84 1.52(2) . ? C83 C82A 1.52(3) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C81A H81C 0.9900 . ? C81A H81D 0.9900 . ? C81A C82A 1.56(4) . ? C82A H82C 0.9900 . ? C82A H82D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Th1 Cl1 106.1(3) . . ? N1 Th1 N2 123.7(4) . . ? N1 Th1 N3 98.9(4) . . ? N1 Th1 N4 67.7(4) . . ? N1 Th1 O1 84.4(4) . . ? N2 Th1 Cl1 125.6(3) . . ? N2 Th1 N3 97.7(4) . . ? N2 Th1 N4 68.3(4) . . ? N2 Th1 O1 85.7(4) . . ? N3 Th1 Cl1 94.6(3) . . ? N3 Th1 N4 70.5(4) . . ? N3 Th1 O1 172.5(4) . . ? N4 Th1 Cl1 161.9(3) . . ? O1 Th1 Cl1 78.1(2) . . ? O1 Th1 N4 117.0(3) . . ? Si1 N1 Th1 127.9(7) . . ? C7 N1 Th1 112.1(9) . . ? C7 N1 Si1 118.4(10) . . ? N1 Si1 C1 108.9(7) . . ? N1 Si1 C2 111.6(8) . . ? N1 Si1 C3 112.4(7) . . ? C1 Si1 C2 107.2(8) . . ? C3 Si1 C1 109.2(8) . . ? C3 Si1 C2 107.3(9) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Si1 114.1(14) . . ? C4 C3 C5 108.1(15) . . ? C4 C3 C6 106.7(16) . . ? C5 C3 Si1 110.5(13) . . ? C6 C3 Si1 110.9(13) . . ? C6 C3 C5 106.1(16) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 109.8 . . ? N1 C7 H7B 109.8 . . ? N1 C7 C8 109.5(12) . . ? H7A C7 H7B 108.2 . . ? C8 C7 H7A 109.8 . . ? C8 C7 H7B 109.8 . . ? C7 C8 H8A 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? N4 C8 C7 106.2(13) . . ? N4 C8 H8A 110.5 . . ? N4 C8 H8B 110.5 . . ? Si2 N2 Th1 121.7(6) . . ? C15 N2 Th1 121.2(8) . . ? C15 N2 Si2 113.9(9) . . ? N2 Si2 C9 110.7(7) . . ? N2 Si2 C10 108.0(6) . . ? N2 Si2 C11 113.1(7) . . ? C9 Si2 C11 108.2(8) . . ? C10 Si2 C9 111.2(8) . . ? C10 Si2 C11 105.7(8) . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Si2 107.1(12) . . ? C13 C11 Si2 108.4(12) . . ? C13 C11 C12 115.8(16) . . ? C13 C11 C14 116.2(17) . . ? C14 C11 Si2 102.8(11) . . ? C14 C11 C12 105.5(14) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.1 . . ? N2 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C16 C15 N2 112.3(12) . . ? C16 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C15 C16 N4 111.2(12) . . ? H16A C16 H16B 108.0 . . ? N4 C16 H16A 109.4 . . ? N4 C16 H16B 109.4 . . ? Si3 N3 Th1 128.9(7) . . ? C23 N3 Th1 113.9(9) . . ? C23 N3 Si3 116.1(10) . . ? N3 Si3 C17 109.2(7) . . ? N3 Si3 C18 110.5(7) . . ? N3 Si3 C19 114.5(7) . . ? C17 Si3 C19 108.8(7) . . ? C18 Si3 C17 106.1(8) . . ? C18 Si3 C19 107.2(7) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Si3 108.8(11) . . ? C20 C19 C21 107.6(13) . . ? C20 C19 C22 110.3(14) . . ? C21 C19 Si3 110.1(10) . . ? C22 C19 Si3 110.6(10) . . ? C22 C19 C21 109.3(14) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 109.8 . . ? N3 C23 H23B 109.8 . . ? N3 C23 C24 109.2(13) . . ? H23A C23 H23B 108.3 . . ? C24 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? C23 C24 H24A 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? N4 C24 C23 108.6(12) . . ? N4 C24 H24A 110.0 . . ? N4 C24 H24B 110.0 . . ? C8 N4 Th1 111.6(9) . . ? C8 N4 C16 111.0(11) . . ? C8 N4 C24 109.3(12) . . ? C16 N4 Th1 109.0(9) . . ? C16 N4 C24 108.8(12) . . ? C24 N4 Th1 107.1(8) . . ? C25 O1 Th1 134.5(8) . . ? C25 O1 C28 108.4(11) . . ? C28 O1 Th1 116.3(8) . . ? O1 C25 H25A 110.4 . . ? O1 C25 H25B 110.4 . . ? O1 C25 C26 106.7(12) . . ? H25A C25 H25B 108.6 . . ? C26 C25 H25A 110.4 . . ? C26 C25 H25B 110.4 . . ? C25 C26 H26A 111.3 . . ? C25 C26 H26B 111.3 . . ? C25 C26 C27 102.4(14) . . ? H26A C26 H26B 109.2 . . ? C27 C26 H26A 111.3 . . ? C27 C26 H26B 111.3 . . ? C26 C27 H27A 111.3 . . ? C26 C27 H27B 111.3 . . ? H27A C27 H27B 109.2 . . ? C28 C27 C26 102.3(13) . . ? C28 C27 H27A 111.3 . . ? C28 C27 H27B 111.3 . . ? O1 C28 C27 105.9(12) . . ? O1 C28 H28A 110.5 . . ? O1 C28 H28B 110.5 . . ? C27 C28 H28A 110.5 . . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? N5 Th2 Cl2 94.8(3) . . ? N5 Th2 N6 99.0(5) . . ? N5 Th2 N8 70.0(4) . . ? N5 Th2 O2 171.6(4) . . ? N6 Th2 Cl2 123.7(3) . . ? N6 Th2 N8 68.9(4) . . ? N6 Th2 O2 86.2(4) . . ? N7 Th2 Cl2 108.7(3) . . ? N7 Th2 N5 99.8(5) . . ? N7 Th2 N6 122.0(4) . . ? N7 Th2 N8 67.3(4) . . ? N7 Th2 O2 82.7(4) . . ? N8 Th2 Cl2 162.6(3) . . ? O2 Th2 Cl2 76.9(2) . . ? O2 Th2 N8 118.1(4) . . ? Si4 N5 Th2 129.1(7) . . ? C35 N5 Th2 114.1(10) . . ? C35 N5 Si4 115.3(11) . . ? N5 Si4 C29 111.7(7) . . ? N5 Si4 C30 109.3(8) . . ? N5 Si4 C31 112.5(7) . . ? C29 Si4 C31 108.3(8) . . ? C30 Si4 C29 106.7(9) . . ? C30 Si4 C31 108.1(7) . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 Si4 111.3(11) . . ? C32 C31 C33 109.5(14) . . ? C32 C31 C34 109.5(14) . . ? C33 C31 Si4 109.1(11) . . ? C34 C31 Si4 109.9(11) . . ? C34 C31 C33 107.5(12) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? N5 C35 C36 110.5(14) . . ? H35A C35 H35B 108.1 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C35 C36 H36A 110.1 . . ? C35 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? N8 C36 C35 108.0(14) . . ? N8 C36 H36A 110.1 . . ? N8 C36 H36B 110.1 . . ? Si5 N6 Th2 123.2(6) . . ? C43 N6 Th2 118.5(10) . . ? C43 N6 Si5 114.8(11) . . ? N6 Si5 C37 107.9(7) . . ? N6 Si5 C38 110.8(9) . . ? N6 Si5 C39 114.2(7) . . ? C37 Si5 C38 109.1(8) . . ? C37 Si5 C39 106.8(8) . . ? C39 Si5 C38 107.9(9) . . ? Si5 C37 H37A 109.5 . . ? Si5 C37 H37B 109.5 . . ? Si5 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si5 C38 H38A 109.5 . . ? Si5 C38 H38B 109.5 . . ? Si5 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 Si5 110.7(12) . . ? C40 C39 C41 106.1(15) . . ? C40 C39 C42 110.7(17) . . ? C41 C39 Si5 111.7(15) . . ? C41 C39 C42 107.2(14) . . ? C42 C39 Si5 110.3(12) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 C43 H43A 108.9 . . ? N6 C43 H43B 108.9 . . ? N6 C43 C44 113.3(14) . . ? H43A C43 H43B 107.7 . . ? C44 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? N8 C44 C43 110.6(13) . . ? N8 C44 H44A 109.5 . . ? N8 C44 H44B 109.5 . . ? Si6 N7 Th2 126.5(6) . . ? C51 N7 Th2 114.6(10) . . ? C51 N7 Si6 117.4(10) . . ? N7 Si6 C45 111.2(8) . . ? N7 Si6 C46 108.7(7) . . ? N7 Si6 C47 112.6(7) . . ? C45 Si6 C46 107.4(9) . . ? C45 Si6 C47 109.1(9) . . ? C46 Si6 C47 107.6(8) . . ? Si6 C45 H45A 109.5 . . ? Si6 C45 H45B 109.5 . . ? Si6 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si6 C46 H46A 109.5 . . ? Si6 C46 H46B 109.5 . . ? Si6 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 Si6 109.0(13) . . ? C48 C47 C49 107.4(15) . . ? C48 C47 C50 110.4(15) . . ? C49 C47 Si6 109.5(12) . . ? C50 C47 Si6 110.0(13) . . ? C50 C47 C49 110.5(16) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N7 C51 H51A 110.4 . . ? N7 C51 H51B 110.4 . . ? N7 C51 C52 106.6(13) . . ? H51A C51 H51B 108.6 . . ? C52 C51 H51A 110.4 . . ? C52 C51 H51B 110.4 . . ? C51 C52 H52A 110.2 . . ? C51 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? N8 C52 C51 107.8(14) . . ? N8 C52 H52A 110.2 . . ? N8 C52 H52B 110.2 . . ? C36 N8 Th2 107.1(9) . . ? C44 N8 Th2 106.3(10) . . ? C44 N8 C36 111.7(14) . . ? C52 N8 Th2 110.7(10) . . ? C52 N8 C36 109.2(14) . . ? C52 N8 C44 111.7(13) . . ? C53 O2 Th2 116.1(8) . . ? C53 O2 C56 109.4(12) . . ? C56 O2 Th2 133.3(8) . . ? O2 C53 H53A 110.6 . . ? O2 C53 H53B 110.6 . . ? O2 C53 C54 105.9(12) . . ? H53A C53 H53B 108.7 . . ? C54 C53 H53A 110.6 . . ? C54 C53 H53B 110.6 . . ? C53 C54 H54A 111.4 . . ? C53 C54 H54B 111.4 . . ? C53 C54 C55 101.7(13) . . ? H54A C54 H54B 109.3 . . ? C55 C54 H54A 111.4 . . ? C55 C54 H54B 111.4 . . ? C54 C55 H55A 110.9 . . ? C54 C55 H55B 110.9 . . ? H55A C55 H55B 108.9 . . ? C56 C55 C54 104.5(15) . . ? C56 C55 H55A 110.9 . . ? C56 C55 H55B 110.9 . . ? O2 C56 C55 104.5(13) . . ? O2 C56 H56A 110.9 . . ? O2 C56 H56B 110.9 . . ? C55 C56 H56A 110.9 . . ? C55 C56 H56B 110.9 . . ? H56A C56 H56B 108.9 . . ? N9 Th3 Cl3 97.5(3) . . ? N9 Th3 N12 70.6(4) . . ? N9 Th3 O3 172.7(4) . . ? N10 Th3 Cl3 108.1(3) . . ? N10 Th3 N9 101.1(5) . . ? N10 Th3 N11 123.8(4) . . ? N10 Th3 N12 67.7(4) . . ? N10 Th3 O3 85.0(4) . . ? N11 Th3 Cl3 121.6(3) . . ? N11 Th3 N9 97.0(4) . . ? N11 Th3 N12 69.4(4) . . ? N11 Th3 O3 82.5(4) . . ? N12 Th3 Cl3 165.5(3) . . ? O3 Th3 Cl3 76.8(2) . . ? O3 Th3 N12 115.8(3) . . ? Si7 N9 Th3 127.2(7) . . ? C63 N9 Th3 113.7(9) . . ? C63 N9 Si7 116.8(10) . . ? N9 Si7 C57 110.5(7) . . ? N9 Si7 C58 108.6(8) . . ? N9 Si7 C59 113.5(7) . . ? C57 Si7 C59 107.2(8) . . ? C58 Si7 C57 108.3(8) . . ? C58 Si7 C59 108.6(8) . . ? Si7 C57 H57A 109.5 . . ? Si7 C57 H57B 109.5 . . ? Si7 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Si7 C58 H58A 109.5 . . ? Si7 C58 H58B 109.5 . . ? Si7 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 Si7 112.1(11) . . ? C60 C59 C62 105.6(14) . . ? C61 C59 Si7 111.0(12) . . ? C61 C59 C60 108.3(15) . . ? C61 C59 C62 109.0(13) . . ? C62 C59 Si7 110.8(11) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61B 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N9 C63 H63A 109.7 . . ? N9 C63 H63B 109.7 . . ? N9 C63 C64 109.9(12) . . ? H63A C63 H63B 108.2 . . ? C64 C63 H63A 109.7 . . ? C64 C63 H63B 109.7 . . ? C63 C64 H64A 109.8 . . ? C63 C64 H64B 109.8 . . ? H64A C64 H64B 108.2 . . ? N12 C64 C63 109.5(12) . . ? N12 C64 H64A 109.8 . . ? N12 C64 H64B 109.8 . . ? Si8 N10 Th3 127.9(7) . . ? C71 N10 Th3 113.0(10) . . ? C71 N10 Si8 117.2(10) . . ? N10 Si8 C65 109.0(7) . . ? N10 Si8 C66 110.9(8) . . ? N10 Si8 C67 112.0(9) . . ? C65 Si8 C66 104.6(9) . . ? C65 Si8 C67 110.0(9) . . ? C66 Si8 C67 110.2(9) . . ? Si8 C65 H65A 109.5 . . ? Si8 C65 H65B 109.5 . . ? Si8 C65 H65C 109.5 . . ? H65A C65 H65B 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Si8 C66 H66A 109.5 . . ? Si8 C66 H66B 109.5 . . ? Si8 C66 H66C 109.5 . . ? H66A C66 H66B 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68 C67 Si8 110.6(13) . . ? C69 C67 Si8 110.4(16) . . ? C69 C67 C68 109.4(18) . . ? C70 C67 Si8 108.9(14) . . ? C70 C67 C68 106.8(17) . . ? C70 C67 C69 110.7(19) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68B 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69B 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70B 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N10 C71 H71A 109.9 . . ? N10 C71 H71B 109.9 . . ? N10 C71 C72 108.9(13) . . ? H71A C71 H71B 108.3 . . ? C72 C71 H71A 109.9 . . ? C72 C71 H71B 109.9 . . ? C71 C72 H72A 110.2 . . ? C71 C72 H72B 110.2 . . ? H72A C72 H72B 108.5 . . ? N12 C72 C71 107.7(12) . . ? N12 C72 H72A 110.2 . . ? N12 C72 H72B 110.2 . . ? Si9 N11 Th3 126.8(6) . . ? C79 N11 Th3 123.1(9) . . ? C79 N11 Si9 110.1(9) . . ? N11 Si9 C73 113.1(7) . . ? N11 Si9 C74 108.5(7) . . ? N11 Si9 C75 113.7(8) . . ? C73 Si9 C74 107.7(9) . . ? C73 Si9 C75 106.0(9) . . ? C74 Si9 C75 107.5(9) . . ? Si9 C73 H73A 109.5 . . ? Si9 C73 H73B 109.5 . . ? Si9 C73 H73C 109.5 . . ? H73A C73 H73B 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? Si9 C74 H74A 109.5 . . ? Si9 C74 H74B 109.5 . . ? Si9 C74 H74C 109.5 . . ? H74A C74 H74B 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 Si9 110.3(14) . . ? C77 C75 Si9 112.8(14) . . ? C77 C75 C76 109.2(17) . . ? C78 C75 Si9 109.6(15) . . ? C78 C75 C76 108.3(18) . . ? C78 C75 C77 106.5(16) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76B 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77B 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78B 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N11 C79 H79A 109.7 . . ? N11 C79 H79B 109.7 . . ? N11 C79 C80 109.9(12) . . ? H79A C79 H79B 108.2 . . ? C80 C79 H79A 109.7 . . ? C80 C79 H79B 109.7 . . ? C79 C80 H80A 109.0 . . ? C79 C80 H80B 109.0 . . ? H80A C80 H80B 107.8 . . ? N12 C80 C79 113.0(12) . . ? N12 C80 H80A 109.0 . . ? N12 C80 H80B 109.0 . . ? C64 N12 Th3 107.1(8) . . ? C64 N12 C72 111.4(12) . . ? C64 N12 C80 113.1(12) . . ? C72 N12 Th3 109.9(9) . . ? C72 N12 C80 109.6(12) . . ? C80 N12 Th3 105.6(8) . . ? C81 O3 Th3 129.5(16) . . ? C84 O3 Th3 119.1(8) . . ? C84 O3 C81 106(2) . . ? C84 O3 C81A 109.2(15) . . ? C81A O3 Th3 131.6(13) . . ? O3 C81 H81A 111.1 . . ? O3 C81 H81B 111.1 . . ? O3 C81 C82 103(3) . . ? H81A C81 H81B 109.1 . . ? C82 C81 H81A 111.1 . . ? C82 C81 H81B 111.1 . . ? C81 C82 H82A 110.9 . . ? C81 C82 H82B 110.9 . . ? H82A C82 H82B 108.9 . . ? C83 C82 C81 104(3) . . ? C83 C82 H82A 110.9 . . ? C83 C82 H82B 110.9 . . ? C82 C83 H83A 110.1 . . ? C82 C83 H83B 110.1 . . ? C82 C83 C84 108(2) . . ? H83A C83 H83B 108.4 . . ? H83C C83 H83D 109.2 . . ? C84 C83 H83A 110.1 . . ? C84 C83 H83B 110.1 . . ? C84 C83 H83C 111.4 . . ? C84 C83 H83D 111.4 . . ? C82A C83 H83C 111.4 . . ? C82A C83 H83D 111.4 . . ? C82A C83 C84 102(2) . . ? O3 C84 C83 106.2(13) . . ? O3 C84 H84A 110.5 . . ? O3 C84 H84B 110.5 . . ? C83 C84 H84A 110.5 . . ? C83 C84 H84B 110.5 . . ? H84A C84 H84B 108.7 . . ? O3 C81A H81C 111.7 . . ? O3 C81A H81D 111.7 . . ? O3 C81A C82A 100(2) . . ? H81C C81A H81D 109.5 . . ? C82A C81A H81C 111.7 . . ? C82A C81A H81D 111.7 . . ? C83 C82A C81A 102(2) . . ? C83 C82A H82C 111.4 . . ? C83 C82A H82D 111.4 . . ? C81A C82A H82C 111.4 . . ? C81A C82A H82D 111.4 . . ? H82C C82A H82D 109.2 . . ? 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 _geom_torsion_publ_flag Th1 N1 Si1 C1 -13.6(11) . . . . ? Th1 N1 Si1 C2 -131.7(9) . . . . ? Th1 N1 Si1 C3 107.6(10) . . . . ? Th1 N1 C7 C8 65.2(13) . . . . ? Th1 N2 Si2 C9 109.9(9) . . . . ? Th1 N2 Si2 C10 -11.9(10) . . . . ? Th1 N2 Si2 C11 -128.5(8) . . . . ? Th1 N2 C15 C16 32.7(16) . . . . ? Th1 N3 Si3 C17 -121.4(9) . . . . ? Th1 N3 Si3 C18 -5.0(11) . . . . ? Th1 N3 Si3 C19 116.3(9) . . . . ? Th1 N3 C23 C24 56.5(14) . . . . ? Th1 O1 C25 C26 -159.1(11) . . . . ? Th1 O1 C28 C27 -174.3(10) . . . . ? N1 Si1 C3 C4 63.6(15) . . . . ? N1 Si1 C3 C5 -58.5(14) . . . . ? N1 Si1 C3 C6 -175.9(13) . . . . ? N1 C7 C8 N4 -57.1(15) . . . . ? Si1 N1 C7 C8 -101.8(13) . . . . ? C1 Si1 C3 C4 -175.5(13) . . . . ? C1 Si1 C3 C5 62.4(13) . . . . ? C1 Si1 C3 C6 -55.0(16) . . . . ? C2 Si1 C3 C4 -59.6(15) . . . . ? C2 Si1 C3 C5 178.3(12) . . . . ? C2 Si1 C3 C6 60.9(16) . . . . ? C7 N1 Si1 C1 151.0(11) . . . . ? C7 N1 Si1 C2 32.9(14) . . . . ? C7 N1 Si1 C3 -87.8(13) . . . . ? C7 C8 N4 Th1 25.5(13) . . . . ? C7 C8 N4 C16 -96.3(14) . . . . ? C7 C8 N4 C24 143.7(12) . . . . ? N2 C15 C16 N4 -48.0(18) . . . . ? Si2 N2 C15 C16 -167.1(11) . . . . ? C15 N2 Si2 C9 -50.1(12) . . . . ? C15 N2 Si2 C10 -172.0(11) . . . . ? C15 N2 Si2 C11 71.4(12) . . . . ? C15 C16 N4 Th1 40.0(15) . . . . ? C15 C16 N4 C8 163.3(13) . . . . ? C15 C16 N4 C24 -76.4(16) . . . . ? N3 C23 C24 N4 -61.4(16) . . . . ? Si3 N3 C23 C24 -112.9(12) . . . . ? C23 N3 Si3 C17 46.2(12) . . . . ? C23 N3 Si3 C18 162.6(11) . . . . ? C23 N3 Si3 C19 -76.2(12) . . . . ? C23 C24 N4 Th1 35.8(13) . . . . ? C23 C24 N4 C8 -85.2(14) . . . . ? C23 C24 N4 C16 153.5(12) . . . . ? O1 C25 C26 C27 -29.6(18) . . . . ? C25 O1 C28 C27 14.3(17) . . . . ? C25 C26 C27 C28 37.4(19) . . . . ? C26 C27 C28 O1 -32.2(18) . . . . ? C28 O1 C25 C26 10.0(17) . . . . ? Th2 N5 Si4 C29 -122.6(10) . . . . ? Th2 N5 Si4 C30 -4.7(11) . . . . ? Th2 N5 Si4 C31 115.4(9) . . . . ? Th2 N5 C35 C36 56.9(17) . . . . ? Th2 N6 Si5 C37 -4.9(10) . . . . ? Th2 N6 Si5 C38 114.5(9) . . . . ? Th2 N6 Si5 C39 -123.4(9) . . . . ? Th2 N6 C43 C44 38.2(17) . . . . ? Th2 N7 Si6 C45 -132.5(10) . . . . ? Th2 N7 Si6 C46 -14.4(12) . . . . ? Th2 N7 Si6 C47 104.7(10) . . . . ? Th2 N7 C51 C52 64.2(14) . . . . ? Th2 O2 C53 C54 -174.2(10) . . . . ? Th2 O2 C56 C55 -159.6(12) . . . . ? N5 C35 C36 N8 -61.0(18) . . . . ? Si4 N5 C35 C36 -110.3(13) . . . . ? C35 N5 Si4 C29 42.3(14) . . . . ? C35 N5 Si4 C30 160.1(12) . . . . ? C35 N5 Si4 C31 -79.8(13) . . . . ? C35 C36 N8 Th2 34.8(15) . . . . ? C35 C36 N8 C44 150.9(14) . . . . ? C35 C36 N8 C52 -85.1(16) . . . . ? N6 Si5 C39 C40 62.4(15) . . . . ? N6 Si5 C39 C41 -55.6(15) . . . . ? N6 Si5 C39 C42 -174.7(12) . . . . ? N6 C43 C44 N8 -55.1(19) . . . . ? Si5 N6 C43 C44 -162.4(12) . . . . ? C37 Si5 C39 C40 -56.8(14) . . . . ? C37 Si5 C39 C41 -174.8(13) . . . . ? C37 Si5 C39 C42 66.1(15) . . . . ? C38 Si5 C39 C40 -173.9(13) . . . . ? C38 Si5 C39 C41 68.1(15) . . . . ? C38 Si5 C39 C42 -51.0(15) . . . . ? C43 N6 Si5 C37 -163.2(11) . . . . ? C43 N6 Si5 C38 -43.8(13) . . . . ? C43 N6 Si5 C39 78.3(13) . . . . ? C43 C44 N8 Th2 42.1(15) . . . . ? C43 C44 N8 C36 -74.4(18) . . . . ? C43 C44 N8 C52 163.0(15) . . . . ? N7 C51 C52 N8 -57.3(17) . . . . ? Si6 N7 C51 C52 -102.9(14) . . . . ? C51 N7 Si6 C45 32.8(14) . . . . ? C51 N7 Si6 C46 150.9(12) . . . . ? C51 N7 Si6 C47 -90.0(13) . . . . ? C51 C52 N8 Th2 28.0(15) . . . . ? C51 C52 N8 C36 145.8(13) . . . . ? C51 C52 N8 C44 -90.3(16) . . . . ? O2 C53 C54 C55 -33.2(19) . . . . ? C53 O2 C56 C55 6.7(19) . . . . ? C53 C54 C55 C56 37(2) . . . . ? C54 C55 C56 O2 -27(2) . . . . ? C56 O2 C53 C54 16.9(18) . . . . ? Th3 N9 Si7 C57 -117.2(9) . . . . ? Th3 N9 Si7 C58 1.5(10) . . . . ? Th3 N9 Si7 C59 122.3(8) . . . . ? Th3 N9 C63 C64 53.0(15) . . . . ? Th3 N10 Si8 C65 -6.4(12) . . . . ? Th3 N10 Si8 C66 -121.0(9) . . . . ? Th3 N10 Si8 C67 115.5(10) . . . . ? Th3 N10 C71 C72 63.4(15) . . . . ? Th3 N11 Si9 C73 -103.2(9) . . . . ? Th3 N11 Si9 C74 16.3(12) . . . . ? Th3 N11 Si9 C75 135.8(9) . . . . ? Th3 N11 C79 C80 23.0(16) . . . . ? Th3 O3 C81 C82 171(6) . . . . ? Th3 O3 C84 C83 -173.7(11) . . . . ? Th3 O3 C81A C82A -160(3) . . . . ? N9 Si7 C59 C60 58.2(14) . . . . ? N9 Si7 C59 C61 179.3(11) . . . . ? N9 Si7 C59 C62 -59.5(13) . . . . ? N9 C63 C64 N12 -61.3(16) . . . . ? Si7 N9 C63 C64 -110.8(12) . . . . ? C57 Si7 C59 C60 -64.1(14) . . . . ? C57 Si7 C59 C61 57.0(13) . . . . ? C57 Si7 C59 C62 178.2(12) . . . . ? C58 Si7 C59 C60 179.1(12) . . . . ? C58 Si7 C59 C61 -59.8(13) . . . . ? C58 Si7 C59 C62 61.4(14) . . . . ? C63 N9 Si7 C57 44.2(13) . . . . ? C63 N9 Si7 C58 162.8(11) . . . . ? C63 N9 Si7 C59 -76.3(12) . . . . ? C63 C64 N12 Th3 37.7(13) . . . . ? C63 C64 N12 C72 -82.4(14) . . . . ? C63 C64 N12 C80 153.7(12) . . . . ? N10 Si8 C67 C68 45.7(16) . . . . ? N10 Si8 C67 C69 166.9(14) . . . . ? N10 Si8 C67 C70 -71.3(16) . . . . ? N10 C71 C72 N12 -59.3(17) . . . . ? Si8 N10 C71 C72 -102.1(14) . . . . ? C65 Si8 C67 C68 167.1(13) . . . . ? C65 Si8 C67 C69 -71.7(17) . . . . ? C65 Si8 C67 C70 50.1(18) . . . . ? C66 Si8 C67 C68 -78.1(16) . . . . ? C66 Si8 C67 C69 43.1(18) . . . . ? C66 Si8 C67 C70 164.8(15) . . . . ? C71 N10 Si8 C65 156.6(12) . . . . ? C71 N10 Si8 C66 42.0(14) . . . . ? C71 N10 Si8 C67 -81.5(13) . . . . ? C71 C72 N12 Th3 29.4(14) . . . . ? C71 C72 N12 C64 147.9(13) . . . . ? C71 C72 N12 C80 -86.2(15) . . . . ? N11 C79 C80 N12 -47.1(17) . . . . ? Si9 N11 C79 C80 -153.2(10) . . . . ? C79 N11 Si9 C73 72.8(12) . . . . ? C79 N11 Si9 C74 -167.7(11) . . . . ? C79 N11 Si9 C75 -48.2(12) . . . . ? C79 C80 N12 Th3 45.6(14) . . . . ? C79 C80 N12 C64 -71.2(15) . . . . ? C79 C80 N12 C72 163.9(12) . . . . ? O3 C81 C82 C83 28(10) . . . . ? O3 C81A C82A C83 -41(5) . . . . ? C81 O3 C84 C83 30(3) . . . . ? C81 C82 C83 C84 -10(10) . . . . ? C82 C83 C84 O3 -12(7) . . . . ? C84 O3 C81 C82 -37(7) . . . . ? C84 O3 C81A C82A 22(5) . . . . ? C84 C83 C82A C81A 44(5) . . . . ? C81A O3 C84 C83 4(3) . . . . ? C82A C83 C84 O3 -30(3) . . . . ? _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' data_2 _nottingham_internal_coll_name THBGLI _nottingham_internal_coll_number 12008 _nottingham_internal_coll_client BMG/STL _nottingham_internal_coll_type sphere _nottingham_internal_coll_frame_method '\w and \f scans' _nottingham_internal_coll_frame_time '10 s' _nottingham_internal_coll_frame_width '0.3 and 0.5 degrees' _nottingham_internal_coll_user pczbg _nottingham_internal_coll_date 19/11/2012 _nottingham_internal_coll_location NOTTS _nottingham_internal_NCS_number ? _nottingham_internal_process_date 20/11/2012 _nottingham_internal_process_user pczbg _nottingham_internal_solution_date 20/11/2012 _nottingham_internal_solution_user BMG _nottingham_internal_refinement_date 13/10/2014 _nottingham_internal_refinement_user BMG _nottingham_internal_self_archive_date 13/10/2014 _nottingham_internal_self_validation_date 13/10/2014 _nottingham_internal_self_validation_user BMG _nottingham_internal_validation_date 21/11/2014 _nottingham_internal_validation_user pczwl _nottingham_internal_archive_date 21/11/2014 _refine_special_details ; Enhanced rigid bond and similarity restraints were applied to the thermal parameters of all atoms. ; _vrf_PLAT971_2 ; PROBLEM: Check Calcd Residual Density 0.81A From Th1 7.31 eA-3 RESPONSE: Large residual density features are adjacent to the heavy atoms (Th1 and I1) and are not chemically significant. ; _vrf_PLAT972_2 ; PROBLEM: Check Calcd Residual Density 1.26A From N3 -5.80 eA-3 RESPONSE: Large residual density features are adjacent to the heavy atoms (Th1 and I1) and are not chemically significant. ; _audit_creation_date 2014-11-21 _audit_creation_method ; Olex2 1.2 (compiled 2014.11.20 svn.r3092 for OlexSys, GUI svn.r4949) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C24 H57 I N4 Si3 Th' _chemical_formula_sum 'C24 H57 I N4 Si3 Th' _chemical_formula_weight 844.94 _chemical_melting_point ? 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Th' 'Th' -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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' _cell_length_a 9.7217(9) _cell_length_b 22.435(2) _cell_length_c 16.0507(15) _cell_angle_alpha 90 _cell_angle_beta 97.547(4) _cell_angle_gamma 90 _cell_volume 3470.4(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12828 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 27.58 _cell_measurement_theta_min 2.49 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 5.308 _exptl_absorpt_correction_T_max 0.4305 _exptl_absorpt_correction_T_min 0.2309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2007/2 (Bruker,2007) was used for absorption correction. wR2(int) was 0.1478 before and 0.0806 after correction. The Ratio of minimum to maximum transmission is 0.5364. The \l/2 correction factor is 0.0015. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1656 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_av_unetI/netI 0.0699 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 34380 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 1.569 _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.366 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4298 _reflns_number_total 6117 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _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 ? _refine_diff_density_max 6.879 _refine_diff_density_min -5.152 _refine_diff_density_rms 0.369 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 313 _refine_ls_number_reflns 6117 _refine_ls_number_restraints 486 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0785 _refine_ls_restrained_S_all 1.087 _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^)+(0.0722P)^2^+229.7088P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2000 _refine_ls_wR_factor_ref 0.2214 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 4.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,H24B) 4.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A, H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A, H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 0.28355(6) 0.70192(3) 0.52579(4) 0.0130(2) Uani 1 1 d . U . . . I1 I -0.00269(12) 0.70037(7) 0.40600(7) 0.0253(3) Uani 1 1 d . U . . . N1 N 0.3331(15) 0.7968(7) 0.5690(9) 0.0182(15) Uani 1 1 d . U . . . Si1 Si 0.3382(6) 0.8542(2) 0.4975(3) 0.0201(10) Uani 1 1 d . U . . . C1 C 0.318(2) 0.8167(9) 0.3919(11) 0.022(3) Uani 1 1 d . U . . . H1A H 0.3848 0.7840 0.3927 0.034 Uiso 1 1 calc GR . . . . H1B H 0.3350 0.8457 0.3488 0.034 Uiso 1 1 calc GR . . . . H1C H 0.2235 0.8010 0.3792 0.034 Uiso 1 1 calc GR . . . . C2 C 0.509(2) 0.8931(9) 0.5125(11) 0.022(3) Uani 1 1 d . U . . . H2A H 0.5239 0.9107 0.5689 0.034 Uiso 1 1 calc GR . . . . H2B H 0.5091 0.9246 0.4703 0.034 Uiso 1 1 calc GR . . . . H2C H 0.5828 0.8645 0.5064 0.034 Uiso 1 1 calc GR . . . . C3 C 0.198(2) 0.9126(9) 0.5000(11) 0.0249(18) Uani 1 1 d . U . . . C4 C 0.054(2) 0.8818(9) 0.4992(12) 0.026(3) Uani 1 1 d . U . . . H4A H 0.0350 0.8568 0.4489 0.040 Uiso 1 1 calc GR . . . . H4B H -0.0182 0.9123 0.4986 0.040 Uiso 1 1 calc GR . . . . H4C H 0.0551 0.8569 0.5495 0.040 Uiso 1 1 calc GR . . . . C5 C 0.190(2) 0.9543(10) 0.4227(12) 0.029(3) Uani 1 1 d . U . . . H5A H 0.2797 0.9738 0.4216 0.044 Uiso 1 1 calc GR . . . . H5B H 0.1182 0.9846 0.4263 0.044 Uiso 1 1 calc GR . . . . H5C H 0.1664 0.9309 0.3712 0.044 Uiso 1 1 calc GR . . . . C6 C 0.229(2) 0.9502(9) 0.5795(11) 0.027(3) Uani 1 1 d . U . . . H6A H 0.2356 0.9242 0.6290 0.040 Uiso 1 1 calc GR . . . . H6B H 0.1540 0.9792 0.5819 0.040 Uiso 1 1 calc GR . . . . H6C H 0.3169 0.9714 0.5787 0.040 Uiso 1 1 calc GR . . . . C7 C 0.4091(18) 0.8019(9) 0.6568(10) 0.0179(18) Uani 1 1 d . U . . . H7A H 0.3535 0.7833 0.6974 0.021 Uiso 1 1 calc R . . . . H7B H 0.4235 0.8444 0.6721 0.021 Uiso 1 1 calc R . . . . C8 C 0.5484(18) 0.7705(8) 0.6603(10) 0.0171(18) Uani 1 1 d . U . . . H8A H 0.6082 0.7918 0.6248 0.021 Uiso 1 1 calc R . . . . H8B H 0.5959 0.7700 0.7188 0.021 Uiso 1 1 calc R . . . . N2 N 0.2824(15) 0.6398(7) 0.6389(8) 0.0158(15) Uani 1 1 d . U . . . Si2 Si 0.1443(5) 0.6370(2) 0.6968(3) 0.0168(9) Uani 1 1 d . U . . . C9 C 0.0309(18) 0.7013(9) 0.6603(11) 0.020(3) Uani 1 1 d . U . . . H9A H 0.0849 0.7382 0.6674 0.031 Uiso 1 1 calc GR . . . . H9B H -0.0467 0.7034 0.6934 0.031 Uiso 1 1 calc GR . . . . H9C H -0.0050 0.6959 0.6008 0.031 Uiso 1 1 calc GR . . . . C10 C 0.2022(19) 0.6459(9) 0.8129(10) 0.020(3) Uani 1 1 d . U . . . H10A H 0.2677 0.6140 0.8322 0.030 Uiso 1 1 calc GR . . . . H10B H 0.1214 0.6436 0.8434 0.030 Uiso 1 1 calc GR . . . . H10C H 0.2475 0.6847 0.8234 0.030 Uiso 1 1 calc GR . . . . C11 C 0.0437(19) 0.5649(9) 0.6790(11) 0.0214(18) Uani 1 1 d . U . . . C12 C -0.023(2) 0.5613(10) 0.5857(11) 0.025(3) Uani 1 1 d . U . . . H12A H -0.0872 0.5948 0.5731 0.037 Uiso 1 1 calc GR . . . . H12B H -0.0747 0.5237 0.5764 0.037 Uiso 1 1 calc GR . . . . H12C H 0.0494 0.5629 0.5490 0.037 Uiso 1 1 calc GR . . . . C13 C -0.074(2) 0.5619(10) 0.7340(12) 0.026(3) Uani 1 1 d . U . . . H13A H -0.0356 0.5652 0.7934 0.039 Uiso 1 1 calc GR . . . . H13B H -0.1233 0.5238 0.7246 0.039 Uiso 1 1 calc GR . . . . H13C H -0.1394 0.5947 0.7191 0.039 Uiso 1 1 calc GR . . . . C14 C 0.139(2) 0.5120(9) 0.6982(12) 0.026(3) Uani 1 1 d . U . . . H14A H 0.2109 0.5126 0.6609 0.039 Uiso 1 1 calc GR . . . . H14B H 0.0849 0.4751 0.6893 0.039 Uiso 1 1 calc GR . . . . H14C H 0.1822 0.5141 0.7568 0.039 Uiso 1 1 calc GR . . . . C15 C 0.4195(17) 0.6161(8) 0.6754(10) 0.0162(18) Uani 1 1 d . U . . . H15A H 0.4601 0.5922 0.6328 0.019 Uiso 1 1 calc R . . . . H15B H 0.4090 0.5900 0.7239 0.019 Uiso 1 1 calc R . . . . C16 C 0.5130(18) 0.6675(8) 0.7031(10) 0.0164(18) Uani 1 1 d . U . . . H16A H 0.6062 0.6527 0.7260 0.020 Uiso 1 1 calc R . . . . H16B H 0.4749 0.6901 0.7479 0.020 Uiso 1 1 calc R . . . . N3 N 0.4689(15) 0.6737(7) 0.4601(9) 0.0157(15) Uani 1 1 d . U . . . Si3 Si 0.4621(5) 0.6080(2) 0.4042(3) 0.0163(9) Uani 1 1 d . U . . . C17 C 0.2914(18) 0.5738(9) 0.4175(11) 0.020(3) Uani 1 1 d . U . . . H17A H 0.2823 0.5713 0.4775 0.030 Uiso 1 1 calc GR . . . . H17B H 0.2860 0.5337 0.3930 0.030 Uiso 1 1 calc GR . . . . H17C H 0.2164 0.5985 0.3890 0.030 Uiso 1 1 calc GR . . . . C18 C 0.6059(18) 0.5569(9) 0.4487(10) 0.017(3) Uani 1 1 d . U . . . H18A H 0.6955 0.5754 0.4433 0.026 Uiso 1 1 calc GR . . . . H18B H 0.5981 0.5190 0.4179 0.026 Uiso 1 1 calc GR . . . . H18C H 0.5992 0.5494 0.5082 0.026 Uiso 1 1 calc GR . . . . C19 C 0.4725(18) 0.6190(9) 0.2862(10) 0.0175(17) Uani 1 1 d . U . . . C20 C 0.3526(18) 0.6584(9) 0.2494(11) 0.019(3) Uani 1 1 d . U . . . H20A H 0.2655 0.6361 0.2474 0.028 Uiso 1 1 calc GR . . . . H20B H 0.3663 0.6705 0.1925 0.028 Uiso 1 1 calc GR . . . . H20C H 0.3486 0.6938 0.2847 0.028 Uiso 1 1 calc GR . . . . C21 C 0.4608(19) 0.5585(9) 0.2426(11) 0.020(3) Uani 1 1 d . U . . . H21A H 0.5425 0.5344 0.2626 0.030 Uiso 1 1 calc GR . . . . H21B H 0.4554 0.5642 0.1817 0.030 Uiso 1 1 calc GR . . . . H21C H 0.3770 0.5381 0.2554 0.030 Uiso 1 1 calc GR . . . . C22 C 0.6116(18) 0.6473(9) 0.2756(11) 0.019(3) Uani 1 1 d . U . . . H22A H 0.6238 0.6839 0.3090 0.029 Uiso 1 1 calc GR . . . . H22B H 0.6140 0.6568 0.2162 0.029 Uiso 1 1 calc GR . . . . H22C H 0.6866 0.6193 0.2948 0.029 Uiso 1 1 calc GR . . . . C23 C 0.6023(17) 0.7018(9) 0.4909(10) 0.0163(18) Uani 1 1 d . U . . . H23A H 0.5961 0.7455 0.4820 0.020 Uiso 1 1 calc R . . . . H23B H 0.6759 0.6860 0.4598 0.020 Uiso 1 1 calc R . . . . C24 C 0.6371(18) 0.6883(8) 0.5838(10) 0.0166(18) Uani 1 1 d . U . . . H24A H 0.6526 0.6450 0.5919 0.020 Uiso 1 1 calc R . . . . H24B H 0.7236 0.7093 0.6065 0.020 Uiso 1 1 calc R . . . . N4 N 0.5236(14) 0.7076(7) 0.6290(8) 0.0156(15) Uani 1 1 d . U . . . 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 0.0085(3) 0.0257(4) 0.0047(3) -0.0006(3) 0.0004(2) 0.0002(3) I1 0.0173(6) 0.0442(8) 0.0136(6) 0.0033(6) -0.0014(5) -0.0003(6) N1 0.020(3) 0.028(3) 0.007(3) 0.000(2) 0.000(2) 0.000(2) Si1 0.026(2) 0.028(2) 0.0070(19) -0.0006(17) 0.0048(17) 0.0018(18) C1 0.029(6) 0.031(6) 0.008(4) 0.000(3) 0.004(4) 0.002(5) C2 0.029(4) 0.030(5) 0.009(5) 0.001(5) 0.004(4) 0.000(4) C3 0.032(3) 0.033(3) 0.011(3) 0.001(3) 0.005(3) 0.005(3) C4 0.032(4) 0.035(6) 0.013(6) 0.000(5) 0.006(4) 0.006(4) C5 0.037(6) 0.038(5) 0.014(4) 0.004(4) 0.006(4) 0.008(5) C6 0.035(6) 0.034(5) 0.012(4) 0.001(4) 0.006(4) 0.004(5) C7 0.018(3) 0.029(3) 0.006(3) -0.001(3) 0.001(3) -0.001(3) C8 0.016(3) 0.030(3) 0.005(3) -0.001(3) 0.000(3) -0.001(3) N2 0.013(3) 0.029(3) 0.005(3) -0.001(2) 0.001(2) 0.000(2) Si2 0.0138(19) 0.032(2) 0.0049(18) -0.0037(17) 0.0019(15) -0.0021(17) C9 0.017(5) 0.033(4) 0.010(5) -0.005(4) 0.000(4) 0.000(4) C10 0.016(6) 0.037(6) 0.006(3) -0.004(3) 0.002(3) -0.002(5) C11 0.020(3) 0.034(3) 0.011(3) -0.005(3) 0.004(3) -0.005(3) C12 0.025(6) 0.037(6) 0.012(4) -0.006(4) 0.003(4) -0.006(5) C13 0.023(5) 0.038(6) 0.017(5) -0.008(4) 0.008(4) -0.008(4) C14 0.024(5) 0.036(4) 0.018(6) -0.004(4) 0.005(4) -0.004(4) C15 0.014(3) 0.030(3) 0.004(3) -0.001(3) 0.001(3) 0.001(3) C16 0.014(3) 0.030(4) 0.005(3) -0.001(3) 0.000(2) 0.001(3) N3 0.011(3) 0.028(3) 0.007(3) -0.002(2) 0.000(2) 0.000(2) Si3 0.014(2) 0.027(2) 0.0072(18) -0.0014(16) 0.0009(15) 0.0009(17) C17 0.017(4) 0.031(6) 0.013(5) -0.003(4) 0.004(4) -0.001(4) C18 0.016(4) 0.030(5) 0.006(5) 0.000(4) 0.004(4) 0.002(4) C19 0.014(4) 0.030(4) 0.008(3) -0.001(2) 0.000(2) 0.000(3) C20 0.014(4) 0.031(5) 0.010(5) 0.000(4) 0.001(4) 0.000(4) C21 0.020(6) 0.031(4) 0.010(5) -0.002(3) 0.003(4) -0.001(4) C22 0.016(4) 0.032(6) 0.010(5) -0.001(4) 0.001(3) -0.001(4) C23 0.012(3) 0.030(4) 0.006(3) -0.002(3) 0.000(2) -0.001(3) C24 0.013(3) 0.031(4) 0.006(3) -0.002(3) -0.001(2) 0.000(3) N4 0.012(3) 0.029(3) 0.005(3) -0.001(2) -0.002(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 I1 3.1680(13) . ? Th1 N1 2.271(16) . ? Th1 N2 2.291(14) . ? Th1 N3 2.293(14) . ? Th1 N4 2.682(14) . ? N1 Si1 1.729(16) . ? N1 C7 1.51(2) . ? Si1 C1 1.878(18) . ? Si1 C2 1.86(2) . ? Si1 C3 1.90(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.56(3) . ? C3 C5 1.55(3) . ? C3 C6 1.53(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.52(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 N4 1.51(2) . ? N2 Si2 1.731(14) . ? N2 C15 1.48(2) . ? Si2 C9 1.86(2) . ? Si2 C10 1.884(17) . ? Si2 C11 1.89(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.56(2) . ? C11 C13 1.54(2) . ? C11 C14 1.51(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.50(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N4 1.50(2) . ? N3 Si3 1.723(16) . ? N3 C23 1.47(2) . ? Si3 C17 1.865(18) . ? Si3 C18 1.876(18) . ? Si3 C19 1.926(17) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.52(2) . ? C19 C21 1.53(3) . ? C19 C22 1.52(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.52(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 N4 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Th1 I1 109.2(4) . . ? N1 Th1 N2 110.6(5) . . ? N1 Th1 N3 104.5(5) . . ? N1 Th1 N4 68.6(5) . . ? N2 Th1 I1 112.3(4) . . ? N2 Th1 N3 106.4(5) . . ? N2 Th1 N4 68.5(5) . . ? N3 Th1 I1 113.5(4) . . ? N3 Th1 N4 67.9(5) . . ? N4 Th1 I1 177.8(3) . . ? Si1 N1 Th1 121.2(7) . . ? C7 N1 Th1 114.5(12) . . ? C7 N1 Si1 120.7(13) . . ? N1 Si1 C1 104.9(8) . . ? N1 Si1 C2 111.5(8) . . ? N1 Si1 C3 114.6(8) . . ? C1 Si1 C3 109.8(9) . . ? C2 Si1 C1 108.2(9) . . ? C2 Si1 C3 107.7(9) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Si1 109.9(14) . . ? C5 C3 Si1 111.2(13) . . ? C5 C3 C4 108.1(16) . . ? C6 C3 Si1 109.7(14) . . ? C6 C3 C4 109.3(16) . . ? C6 C3 C5 108.6(17) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 109.9 . . ? N1 C7 H7B 109.9 . . ? N1 C7 C8 108.9(14) . . ? H7A C7 H7B 108.3 . . ? C8 C7 H7A 109.9 . . ? C8 C7 H7B 109.9 . . ? C7 C8 H8A 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N4 C8 C7 108.6(14) . . ? N4 C8 H8A 110.0 . . ? N4 C8 H8B 110.0 . . ? Si2 N2 Th1 122.2(8) . . ? C15 N2 Th1 115.7(10) . . ? C15 N2 Si2 119.7(11) . . ? N2 Si2 C9 105.7(8) . . ? N2 Si2 C10 112.0(8) . . ? N2 Si2 C11 111.8(8) . . ? C9 Si2 C10 108.5(8) . . ? C9 Si2 C11 110.0(9) . . ? C10 Si2 C11 108.7(9) . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Si2 109.5(13) . . ? C13 C11 Si2 111.2(13) . . ? C13 C11 C12 107.4(15) . . ? C14 C11 Si2 110.5(13) . . ? C14 C11 C12 108.8(16) . . ? C14 C11 C13 109.4(16) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 110.0 . . ? N2 C15 H15B 110.0 . . ? N2 C15 C16 108.6(15) . . ? H15A C15 H15B 108.3 . . ? C16 C15 H15A 110.0 . . ? C16 C15 H15B 110.0 . . ? C15 C16 H16A 109.9 . . ? C15 C16 H16B 109.9 . . ? C15 C16 N4 109.0(13) . . ? H16A C16 H16B 108.3 . . ? N4 C16 H16A 109.9 . . ? N4 C16 H16B 109.9 . . ? Si3 N3 Th1 119.8(8) . . ? C23 N3 Th1 116.1(11) . . ? C23 N3 Si3 121.0(12) . . ? N3 Si3 C17 105.5(8) . . ? N3 Si3 C18 110.5(8) . . ? N3 Si3 C19 113.5(8) . . ? C17 Si3 C18 109.5(9) . . ? C17 Si3 C19 109.1(8) . . ? C18 Si3 C19 108.7(8) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Si3 108.7(12) . . ? C20 C19 C21 109.4(15) . . ? C20 C19 C22 111.3(16) . . ? C21 C19 Si3 109.1(12) . . ? C22 C19 Si3 109.0(12) . . ? C22 C19 C21 109.4(15) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 110.0 . . ? N3 C23 H23B 110.0 . . ? N3 C23 C24 108.6(14) . . ? H23A C23 H23B 108.4 . . ? C24 C23 H23A 110.0 . . ? C24 C23 H23B 110.0 . . ? C23 C24 H24A 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? N4 C24 C23 110.0(14) . . ? N4 C24 H24A 109.7 . . ? N4 C24 H24B 109.7 . . ? C8 N4 Th1 109.8(10) . . ? C16 N4 Th1 108.4(10) . . ? C16 N4 C8 108.6(13) . . ? C24 N4 Th1 109.4(9) . . ? C24 N4 C8 110.1(14) . . ? C24 N4 C16 110.5(14) . . ? 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 _geom_torsion_publ_flag Th1 N1 Si1 C1 -6.6(11) . . . . ? Th1 N1 Si1 C2 -123.5(9) . . . . ? Th1 N1 Si1 C3 113.9(10) . . . . ? Th1 N1 C7 C8 61.9(16) . . . . ? Th1 N2 Si2 C9 -10.5(11) . . . . ? Th1 N2 Si2 C10 -128.4(9) . . . . ? Th1 N2 Si2 C11 109.2(10) . . . . ? Th1 N2 C15 C16 59.2(15) . . . . ? Th1 N3 Si3 C17 -2.1(11) . . . . ? Th1 N3 Si3 C18 -120.4(9) . . . . ? Th1 N3 Si3 C19 117.3(9) . . . . ? Th1 N3 C23 C24 58.1(17) . . . . ? N1 Si1 C3 C4 -48.2(15) . . . . ? N1 Si1 C3 C5 -167.8(13) . . . . ? N1 Si1 C3 C6 72.0(16) . . . . ? N1 C7 C8 N4 -54.3(18) . . . . ? Si1 N1 C7 C8 -97.1(17) . . . . ? C1 Si1 C3 C4 69.6(14) . . . . ? C1 Si1 C3 C5 -50.1(17) . . . . ? C1 Si1 C3 C6 -170.2(13) . . . . ? C2 Si1 C3 C4 -172.8(12) . . . . ? C2 Si1 C3 C5 67.6(16) . . . . ? C2 Si1 C3 C6 -52.6(15) . . . . ? C7 N1 Si1 C1 151.0(13) . . . . ? C7 N1 Si1 C2 34.1(16) . . . . ? C7 N1 Si1 C3 -88.5(15) . . . . ? C7 C8 N4 Th1 25.2(14) . . . . ? C7 C8 N4 C16 -93.2(15) . . . . ? C7 C8 N4 C24 145.6(14) . . . . ? N2 Si2 C11 C12 -64.1(15) . . . . ? N2 Si2 C11 C13 177.4(13) . . . . ? N2 Si2 C11 C14 55.8(14) . . . . ? N2 C15 C16 N4 -57.7(17) . . . . ? Si2 N2 C15 C16 -103.5(15) . . . . ? C9 Si2 C11 C12 53.1(15) . . . . ? C9 Si2 C11 C13 -65.5(15) . . . . ? C9 Si2 C11 C14 172.9(12) . . . . ? C10 Si2 C11 C12 171.7(13) . . . . ? C10 Si2 C11 C13 53.1(16) . . . . ? C10 Si2 C11 C14 -68.5(14) . . . . ? C15 N2 Si2 C9 151.1(13) . . . . ? C15 N2 Si2 C10 33.1(16) . . . . ? C15 N2 Si2 C11 -89.2(14) . . . . ? C15 C16 N4 Th1 31.3(16) . . . . ? C15 C16 N4 C8 150.5(14) . . . . ? C15 C16 N4 C24 -88.6(17) . . . . ? N3 C23 C24 N4 -55(2) . . . . ? Si3 N3 C23 C24 -101.7(15) . . . . ? C23 N3 Si3 C17 157.0(13) . . . . ? C23 N3 Si3 C18 38.7(15) . . . . ? C23 N3 Si3 C19 -83.6(14) . . . . ? C23 C24 N4 Th1 28.9(17) . . . . ? C23 C24 N4 C8 -91.8(17) . . . . ? C23 C24 N4 C16 148.2(15) . . . . ? _shelx_hkl_checksum 9021 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' data_3 _nottingham_internal_coll_name THBGLr _nottingham_internal_coll_number 12061 _nottingham_internal_coll_client pczbg _nottingham_internal_coll_type 'hemisphere' _nottingham_internal_coll_frame_time '15' _nottingham_internal_coll_frame_width '0.3' _nottingham_internal_coll_frame_method '\w' _nottingham_internal_coll_user pczbg _nottingham_internal_coll_date 26/11/2012 _nottingham_internal_coll_location NOTTS _nottingham_internal_NCS_number ? _nottingham_internal_process_user pczbg _nottingham_internal_process_date 28/11/2012 _nottingham_internal_solution_user pczbg _nottingham_internal_solution_date 27/11/2012 _nottingham_internal_refinement_user pczbg _nottingham_internal_refinement_date 28/11/2012 _nottingham_internal_self_validation_user pczbg _nottingham_internal_self_validation_date 02/10/2014 _nottingham_internal_self_archive_date 02/10/2014 _nottingham_internal_validation_user pczwl _nottingham_internal_validation_date 10/11/2014 _nottingham_internal_archive_date 10/11/2014 _vrf_PLAT094_3 ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 4.67 Report RESPONSE: Large positive residual density peaks are adjacent to the Th atom, and are due to inadequate correction for absorption by the Th atom. ; _audit_creation_date 2014-10-02 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C28 H67 N5 Si3 Th' _chemical_formula_sum 'C28 H67 N5 Si3 Th' _chemical_formula_weight 790.17 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Th' 'Th' -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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' _cell_length_a 10.0050(4) _cell_length_b 23.2032(8) _cell_length_c 16.5776(6) _cell_angle_alpha 90 _cell_angle_beta 97.754(2) _cell_angle_gamma 90 _cell_volume 3813.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 17447 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 27.39 _cell_measurement_theta_min 2.149 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 4.027 _exptl_absorpt_correction_T_max 0.4305 _exptl_absorpt_correction_T_min 0.2815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2007/2 (Bruker,2007) was used for absorption correction. wR2(int) was 0.1134 before and 0.0505 after correction. The Ratio of minimum to maximum transmission is 0.6539. The \l/2 correction factor is 0.0015. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1608 _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.17 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_unetI/netI 0.0321 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 36814 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.438 _diffrn_reflns_theta_min 2.149 _diffrn_ambient_temperature 90(2) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7814 _reflns_number_total 8678 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)' _computing_data_collection 'Bruker SMART version 5.34 (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)' _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 ? _refine_diff_density_max 1.746 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.097 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 351 _refine_ls_number_reflns 8678 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0254 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+3.4221P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.0624 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A, H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A, H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C26(H26A,H26B, H26C), C28(H28A,H28B,H28C) ; _atom_sites_solution_hydrogens 'geom, Me from difmap' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.90438(2) 0.68513(2) 0.80901(2) 0.02159(4) Uani 1 1 d . . . . . N1 N 0.9097(2) 0.62322(10) 0.69893(15) 0.0274(5) Uani 1 1 d . . . . . Si1 Si 1.03557(8) 0.62331(3) 0.63741(5) 0.02609(16) Uani 1 1 d . . . . . C1 C 1.1504(4) 0.68529(12) 0.6726(2) 0.0340(7) Uani 1 1 d . . . . . H1A H 1.0996 0.7215 0.6658 0.051 Uiso 1 1 calc GR . . . . H1B H 1.2254 0.6866 0.6403 0.051 Uiso 1 1 calc GR . . . . H1C H 1.1859 0.6801 0.7302 0.051 Uiso 1 1 calc GR . . . . C2 C 0.9656(4) 0.63710(16) 0.5285(2) 0.0453(8) Uani 1 1 d . . . . . H2A H 0.9067 0.6051 0.5080 0.068 Uiso 1 1 calc GR . . . . H2B H 1.0399 0.6404 0.4959 0.068 Uiso 1 1 calc GR . . . . H2C H 0.9136 0.6730 0.5247 0.068 Uiso 1 1 calc GR . . . . C3 C 1.1391(3) 0.55412(12) 0.64291(18) 0.0282(6) Uani 1 1 d . . . . . C4 C 1.0445(4) 0.50170(13) 0.6302(2) 0.0420(8) Uani 1 1 d . . . . . H4A H 0.9864 0.5007 0.6733 0.063 Uiso 1 1 calc GR . . . . H4B H 1.0982 0.4663 0.6321 0.063 Uiso 1 1 calc GR . . . . H4C H 0.9885 0.5047 0.5771 0.063 Uiso 1 1 calc GR . . . . C5 C 1.2339(3) 0.55369(14) 0.5774(2) 0.0378(7) Uani 1 1 d . . . . . H5A H 1.1806 0.5558 0.5234 0.057 Uiso 1 1 calc GR . . . . H5B H 1.2870 0.5181 0.5818 0.057 Uiso 1 1 calc GR . . . . H5C H 1.2947 0.5869 0.5852 0.057 Uiso 1 1 calc GR . . . . C6 C 1.2238(3) 0.54778(14) 0.72672(19) 0.0367(7) Uani 1 1 d . . . . . H6A H 1.2848 0.5808 0.7367 0.055 Uiso 1 1 calc GR . . . . H6B H 1.2768 0.5122 0.7281 0.055 Uiso 1 1 calc GR . . . . H6C H 1.1640 0.5463 0.7689 0.055 Uiso 1 1 calc GR . . . . C7 C 0.7797(3) 0.59588(13) 0.6673(2) 0.0357(7) Uani 1 1 d . . . . . H7A H 0.7482 0.5717 0.7102 0.043 Uiso 1 1 calc R . . . . H7B H 0.7917 0.5707 0.6206 0.043 Uiso 1 1 calc R . . . . C8 C 0.6751(3) 0.64215(15) 0.6403(2) 0.0393(8) Uani 1 1 d . . . . . H8A H 0.7040 0.6648 0.5951 0.047 Uiso 1 1 calc R . . . . H8B H 0.5875 0.6238 0.6204 0.047 Uiso 1 1 calc R . . . . N2 N 0.7358(2) 0.65011(10) 0.87878(15) 0.0266(5) Uani 1 1 d . . . . . Si2 Si 0.74128(8) 0.59220(3) 0.94402(5) 0.02790(17) Uani 1 1 d . . . . . C9 C 0.8915(3) 0.54789(14) 0.9261(2) 0.0411(8) Uani 1 1 d . . . . . H9A H 0.8863 0.5390 0.8679 0.062 Uiso 1 1 calc GR . . . . H9B H 0.8923 0.5119 0.9571 0.062 Uiso 1 1 calc GR . . . . H9C H 0.9743 0.5696 0.9438 0.062 Uiso 1 1 calc GR . . . . C10 C 0.5864(3) 0.54582(13) 0.9203(2) 0.0373(7) Uani 1 1 d . . . . . H10A H 0.5080 0.5663 0.9357 0.056 Uiso 1 1 calc GR . . . . H10B H 0.5993 0.5097 0.9510 0.056 Uiso 1 1 calc GR . . . . H10C H 0.5714 0.5373 0.8619 0.056 Uiso 1 1 calc GR . . . . C11 C 0.7564(3) 0.61479(13) 1.05538(19) 0.0343(7) Uani 1 1 d . . . . . C12 C 0.8874(4) 0.6482(2) 1.0799(2) 0.0558(11) Uani 1 1 d . . . . . H12A H 0.9646 0.6228 1.0766 0.084 Uiso 1 1 calc GR . . . . H12B H 0.8900 0.6623 1.1358 0.084 Uiso 1 1 calc GR . . . . H12C H 0.8914 0.6810 1.0430 0.084 Uiso 1 1 calc GR . . . . C13 C 0.6389(4) 0.65424(17) 1.0676(2) 0.0522(9) Uani 1 1 d . . . . . H13A H 0.6422 0.6890 1.0342 0.078 Uiso 1 1 calc GR . . . . H13B H 0.6453 0.6652 1.1251 0.078 Uiso 1 1 calc GR . . . . H13C H 0.5536 0.6340 1.0513 0.078 Uiso 1 1 calc GR . . . . C14 C 0.7546(5) 0.56196(16) 1.1116(2) 0.0557(11) Uani 1 1 d . . . . . H14A H 0.6683 0.5418 1.0991 0.084 Uiso 1 1 calc GR . . . . H14B H 0.7661 0.5747 1.1685 0.084 Uiso 1 1 calc GR . . . . H14C H 0.8284 0.5358 1.1030 0.084 Uiso 1 1 calc GR . . . . C15 C 0.6018(3) 0.67470(13) 0.8493(2) 0.0322(7) Uani 1 1 d . . . . . H15A H 0.6051 0.7172 0.8547 0.039 Uiso 1 1 calc R . . . . H15B H 0.5345 0.6599 0.8828 0.039 Uiso 1 1 calc R . . . . C16 C 0.5597(3) 0.65840(15) 0.7604(2) 0.0380(7) Uani 1 1 d . . . . . H16A H 0.5539 0.6159 0.7552 0.046 Uiso 1 1 calc R . . . . H16B H 0.4696 0.6747 0.7412 0.046 Uiso 1 1 calc R . . . . N3 N 0.8290(3) 0.77681(10) 0.76906(15) 0.0307(5) Uani 1 1 d . . . . . Si3 Si 0.80543(10) 0.83408(3) 0.83220(5) 0.03203(19) Uani 1 1 d . . . . . C17 C 0.8410(4) 0.80734(13) 0.9403(2) 0.0344(7) Uani 1 1 d . . . . . H17A H 0.9357 0.7956 0.9520 0.052 Uiso 1 1 calc GR . . . . H17B H 0.7827 0.7743 0.9474 0.052 Uiso 1 1 calc GR . . . . H17C H 0.8230 0.8382 0.9777 0.052 Uiso 1 1 calc GR . . . . C18 C 0.6264(4) 0.86023(14) 0.8169(2) 0.0430(8) Uani 1 1 d . . . . . H18A H 0.5668 0.8295 0.8316 0.065 Uiso 1 1 calc GR . . . . H18B H 0.6006 0.8709 0.7597 0.065 Uiso 1 1 calc GR . . . . H18C H 0.6181 0.8939 0.8515 0.065 Uiso 1 1 calc GR . . . . C19 C 0.9184(4) 0.89858(13) 0.8185(2) 0.0460(10) Uani 1 1 d . . . . . C20 C 0.8896(6) 0.9210(2) 0.7312(3) 0.0814(16) Uani 1 1 d . . . . . H20A H 0.9081 0.8904 0.6933 0.122 Uiso 1 1 calc GR . . . . H20B H 0.9476 0.9542 0.7247 0.122 Uiso 1 1 calc GR . . . . H20C H 0.7948 0.9325 0.7195 0.122 Uiso 1 1 calc GR . . . . C21 C 1.0688(4) 0.88154(15) 0.8341(3) 0.0578(11) Uani 1 1 d . . . . . H21A H 1.0931 0.8711 0.8914 0.087 Uiso 1 1 calc GR . . . . H21B H 1.1243 0.9141 0.8209 0.087 Uiso 1 1 calc GR . . . . H21C H 1.0847 0.8485 0.7997 0.087 Uiso 1 1 calc GR . . . . C22 C 0.8957(5) 0.94693(15) 0.8794(3) 0.0653(13) Uani 1 1 d . . . . . H22A H 0.7995 0.9566 0.8738 0.098 Uiso 1 1 calc GR . . . . H22B H 0.9474 0.9812 0.8679 0.098 Uiso 1 1 calc GR . . . . H22C H 0.9257 0.9337 0.9350 0.098 Uiso 1 1 calc GR . . . . C23 C 0.7559(4) 0.77631(14) 0.68568(19) 0.0389(8) Uani 1 1 d . . . . . H23A H 0.8143 0.7596 0.6480 0.047 Uiso 1 1 calc R . . . . H23B H 0.7333 0.8163 0.6680 0.047 Uiso 1 1 calc R . . . . C24 C 0.6272(4) 0.74103(15) 0.6822(2) 0.0399(8) Uani 1 1 d . . . . . H24A H 0.5664 0.7590 0.7174 0.048 Uiso 1 1 calc R . . . . H24B H 0.5801 0.7405 0.6257 0.048 Uiso 1 1 calc R . . . . N4 N 0.6595(3) 0.68090(10) 0.70995(16) 0.0313(6) Uani 1 1 d . . . . . N5 N 1.1122(3) 0.68232(15) 0.88772(18) 0.0474(8) Uani 1 1 d . . . . . C25 C 1.1697(4) 0.73828(18) 0.9135(2) 0.0539(10) Uani 1 1 d . . . . . H25A H 1.1927 0.7377 0.9734 0.065 Uiso 1 1 calc R . . . . H25B H 1.0991 0.7679 0.9000 0.065 Uiso 1 1 calc R . . . . C26 C 1.2950(4) 0.7572(2) 0.8770(3) 0.0717(15) Uani 1 1 d . . . . . H26A H 1.2807 0.7507 0.8180 0.108 Uiso 1 1 calc GR . . . . H26B H 1.3731 0.7348 0.9015 0.108 Uiso 1 1 calc GR . . . . H26C H 1.3115 0.7983 0.8879 0.108 Uiso 1 1 calc GR . . . . C27 C 1.2040(4) 0.63461(17) 0.9087(2) 0.0484(9) Uani 1 1 d . . . . . H27A H 1.2854 0.6409 0.8819 0.058 Uiso 1 1 calc R . . . . H27B H 1.1601 0.5989 0.8857 0.058 Uiso 1 1 calc R . . . . C28 C 1.2483(4) 0.62515(19) 0.9982(3) 0.0558(10) Uani 1 1 d . . . . . H28A H 1.3003 0.5893 1.0060 0.084 Uiso 1 1 calc GR . . . . H28B H 1.1688 0.6224 1.0267 0.084 Uiso 1 1 calc GR . . . . H28C H 1.3046 0.6575 1.0203 0.084 Uiso 1 1 calc GR . . . . 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 0.01876(6) 0.02337(6) 0.02236(6) 0.00148(4) 0.00173(4) -0.00034(4) N1 0.0255(13) 0.0254(11) 0.0308(13) -0.0033(10) 0.0019(10) 0.0007(9) Si1 0.0310(4) 0.0227(3) 0.0246(4) 0.0002(3) 0.0037(3) 0.0011(3) C1 0.0385(19) 0.0264(14) 0.0380(17) 0.0005(12) 0.0091(14) -0.0047(12) C2 0.053(2) 0.052(2) 0.0295(17) 0.0006(15) 0.0008(15) 0.0129(17) C3 0.0332(16) 0.0228(12) 0.0297(14) -0.0006(11) 0.0082(12) 0.0006(12) C4 0.045(2) 0.0242(14) 0.059(2) -0.0087(14) 0.0169(17) -0.0031(13) C5 0.0386(18) 0.0397(16) 0.0378(17) 0.0037(14) 0.0145(14) 0.0065(14) C6 0.0415(19) 0.0332(15) 0.0354(16) 0.0047(13) 0.0051(14) 0.0093(14) C7 0.0290(17) 0.0341(15) 0.0432(18) -0.0100(14) 0.0015(14) -0.0032(13) C8 0.0278(17) 0.0499(19) 0.0372(17) -0.0111(15) -0.0069(13) 0.0009(14) N2 0.0218(12) 0.0256(11) 0.0327(13) 0.0039(10) 0.0042(10) 0.0000(9) Si2 0.0279(4) 0.0235(4) 0.0333(4) 0.0042(3) 0.0078(3) -0.0012(3) C9 0.0373(19) 0.0359(16) 0.051(2) 0.0092(15) 0.0080(15) 0.0086(14) C10 0.0402(19) 0.0303(15) 0.0428(18) -0.0052(13) 0.0111(15) -0.0101(13) C11 0.0340(18) 0.0359(16) 0.0338(16) 0.0061(13) 0.0068(13) -0.0105(13) C12 0.049(2) 0.080(3) 0.0361(19) 0.0032(19) -0.0023(16) -0.031(2) C13 0.056(2) 0.056(2) 0.044(2) -0.0187(18) 0.0052(18) 0.0003(19) C14 0.086(3) 0.045(2) 0.039(2) 0.0132(16) 0.019(2) -0.008(2) C15 0.0211(15) 0.0335(15) 0.0424(18) 0.0059(13) 0.0054(13) 0.0031(12) C16 0.0195(15) 0.0443(18) 0.049(2) 0.0014(15) -0.0010(13) 0.0015(13) N3 0.0431(15) 0.0233(11) 0.0284(13) 0.0041(10) 0.0142(11) 0.0038(10) Si3 0.0433(5) 0.0207(3) 0.0359(5) 0.0041(3) 0.0191(4) 0.0050(3) C17 0.0385(19) 0.0312(15) 0.0362(17) -0.0006(13) 0.0148(14) 0.0014(13) C18 0.051(2) 0.0336(16) 0.046(2) 0.0042(14) 0.0130(16) 0.0176(15) C19 0.065(3) 0.0192(14) 0.062(2) 0.0041(14) 0.035(2) -0.0015(14) C20 0.118(5) 0.059(3) 0.072(3) 0.034(2) 0.028(3) -0.015(3) C21 0.062(3) 0.0354(18) 0.085(3) -0.0093(19) 0.040(2) -0.0136(17) C22 0.069(3) 0.0287(17) 0.108(4) -0.016(2) 0.047(3) -0.0086(18) C23 0.053(2) 0.0324(15) 0.0323(16) 0.0083(13) 0.0102(15) 0.0151(15) C24 0.0406(19) 0.0461(19) 0.0312(16) 0.0054(14) -0.0020(14) 0.0204(15) N4 0.0245(14) 0.0354(13) 0.0324(14) -0.0010(10) -0.0023(11) 0.0078(10) N5 0.0228(15) 0.089(3) 0.0300(15) -0.0126(14) 0.0024(12) -0.0017(14) C25 0.050(2) 0.069(3) 0.044(2) -0.0041(19) 0.0088(17) 0.030(2) C26 0.028(2) 0.083(3) 0.103(4) -0.057(3) 0.005(2) -0.007(2) C27 0.0314(19) 0.067(2) 0.049(2) -0.0278(18) 0.0129(16) -0.0097(17) C28 0.037(2) 0.066(2) 0.065(3) -0.004(2) 0.0087(18) 0.0132(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 N1 2.329(2) . ? Th1 N2 2.317(2) . ? Th1 N3 2.323(2) . ? Th1 N4 2.761(3) . ? Th1 N5 2.302(3) . ? N1 Si1 1.724(2) . ? N1 C7 1.478(4) . ? Si1 C1 1.884(3) . ? Si1 C2 1.873(3) . ? Si1 C3 1.906(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.538(4) . ? C3 C5 1.536(4) . ? C3 C6 1.534(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.523(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 N4 1.488(4) . ? N2 Si2 1.721(2) . ? N2 C15 1.479(4) . ? Si2 C9 1.878(3) . ? Si2 C10 1.884(3) . ? Si2 C11 1.905(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.530(5) . ? C11 C13 1.525(5) . ? C11 C14 1.542(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.524(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N4 1.481(4) . ? N3 Si3 1.727(2) . ? N3 C23 1.474(4) . ? Si3 C17 1.884(3) . ? Si3 C18 1.876(4) . ? Si3 C19 1.907(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.528(6) . ? C19 C21 1.544(6) . ? C19 C22 1.546(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.520(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 N4 1.491(4) . ? N5 C25 1.461(5) . ? N5 C27 1.450(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.528(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.507(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Th1 N4 67.92(8) . . ? N2 Th1 N1 105.66(8) . . ? N2 Th1 N3 103.50(8) . . ? N2 Th1 N4 68.73(8) . . ? N3 Th1 N1 112.47(8) . . ? N3 Th1 N4 68.61(8) . . ? N5 Th1 N1 108.21(10) . . ? N5 Th1 N2 111.70(10) . . ? N5 Th1 N3 114.90(11) . . ? N5 Th1 N4 175.85(9) . . ? Si1 N1 Th1 123.95(12) . . ? C7 N1 Th1 115.53(18) . . ? C7 N1 Si1 117.9(2) . . ? N1 Si1 C1 106.33(13) . . ? N1 Si1 C2 111.23(15) . . ? N1 Si1 C3 113.97(12) . . ? C1 Si1 C3 108.89(14) . . ? C2 Si1 C1 107.53(17) . . ? C2 Si1 C3 108.66(14) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Si1 109.8(2) . . ? C5 C3 Si1 110.8(2) . . ? C5 C3 C4 109.0(2) . . ? C6 C3 Si1 110.76(19) . . ? C6 C3 C4 107.6(3) . . ? C6 C3 C5 108.7(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? N1 C7 C8 109.8(2) . . ? H7A C7 H7B 108.2 . . ? C8 C7 H7A 109.7 . . ? C8 C7 H7B 109.7 . . ? C7 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N4 C8 C7 109.7(3) . . ? N4 C8 H8A 109.7 . . ? N4 C8 H8B 109.7 . . ? Si2 N2 Th1 128.60(12) . . ? C15 N2 Th1 112.85(17) . . ? C15 N2 Si2 117.37(19) . . ? N2 Si2 C9 106.64(14) . . ? N2 Si2 C10 111.06(14) . . ? N2 Si2 C11 112.68(13) . . ? C9 Si2 C10 107.92(16) . . ? C9 Si2 C11 110.09(16) . . ? C10 Si2 C11 108.35(14) . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Si2 110.5(2) . . ? C12 C11 C14 108.8(3) . . ? C13 C11 Si2 109.4(2) . . ? C13 C11 C12 108.0(3) . . ? C13 C11 C14 109.0(3) . . ? C14 C11 Si2 111.2(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.6 . . ? N2 C15 H15B 109.6 . . ? N2 C15 C16 110.1(2) . . ? H15A C15 H15B 108.2 . . ? C16 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C15 C16 H16A 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? N4 C16 C15 109.8(3) . . ? N4 C16 H16A 109.7 . . ? N4 C16 H16B 109.7 . . ? Si3 N3 Th1 126.68(13) . . ? C23 N3 Th1 111.16(17) . . ? C23 N3 Si3 118.9(2) . . ? N3 Si3 C17 107.40(13) . . ? N3 Si3 C18 111.92(16) . . ? N3 Si3 C19 113.56(13) . . ? C17 Si3 C19 109.44(17) . . ? C18 Si3 C17 106.81(15) . . ? C18 Si3 C19 107.50(16) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Si3 109.9(3) . . ? C20 C19 C21 107.5(3) . . ? C20 C19 C22 110.3(3) . . ? C21 C19 Si3 111.0(2) . . ? C21 C19 C22 107.6(4) . . ? C22 C19 Si3 110.5(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? N3 C23 C24 110.5(3) . . ? H23A C23 H23B 108.1 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C23 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? N4 C24 C23 110.2(3) . . ? N4 C24 H24A 109.6 . . ? N4 C24 H24B 109.6 . . ? C8 N4 Th1 107.80(18) . . ? C8 N4 C24 111.5(3) . . ? C16 N4 Th1 106.76(18) . . ? C16 N4 C8 112.0(3) . . ? C16 N4 C24 111.7(3) . . ? C24 N4 Th1 106.76(19) . . ? C25 N5 Th1 115.5(2) . . ? C27 N5 Th1 130.7(2) . . ? C27 N5 C25 113.4(3) . . ? N5 C25 H25A 108.1 . . ? N5 C25 H25B 108.1 . . ? N5 C25 C26 116.9(3) . . ? H25A C25 H25B 107.3 . . ? C26 C25 H25A 108.1 . . ? C26 C25 H25B 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 H27A 108.3 . . ? N5 C27 H27B 108.3 . . ? N5 C27 C28 116.1(3) . . ? H27A C27 H27B 107.4 . . ? C28 C27 H27A 108.3 . . ? C28 C27 H27B 108.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 _geom_torsion_publ_flag Th1 N1 Si1 C1 -4.58(19) . . . . ? Th1 N1 Si1 C2 -121.36(17) . . . . ? Th1 N1 Si1 C3 115.38(15) . . . . ? Th1 N1 C7 C8 59.0(3) . . . . ? Th1 N2 Si2 C9 -16.5(2) . . . . ? Th1 N2 Si2 C10 -133.88(16) . . . . ? Th1 N2 Si2 C11 104.34(18) . . . . ? Th1 N2 C15 C16 62.1(3) . . . . ? Th1 N3 Si3 C17 -3.7(2) . . . . ? Th1 N3 Si3 C18 -120.61(18) . . . . ? Th1 N3 Si3 C19 117.45(19) . . . . ? Th1 N3 C23 C24 65.1(3) . . . . ? Th1 N5 C25 C26 -111.8(3) . . . . ? Th1 N5 C27 C28 -125.9(3) . . . . ? N1 C7 C8 N4 -58.0(4) . . . . ? Si1 N1 C7 C8 -103.5(3) . . . . ? C7 N1 Si1 C1 156.3(2) . . . . ? C7 N1 Si1 C2 39.6(3) . . . . ? C7 N1 Si1 C3 -83.7(2) . . . . ? C7 C8 N4 Th1 30.5(3) . . . . ? C7 C8 N4 C16 -86.6(3) . . . . ? C7 C8 N4 C24 147.4(3) . . . . ? N2 C15 C16 N4 -59.8(3) . . . . ? Si2 N2 C15 C16 -106.5(3) . . . . ? C15 N2 Si2 C9 150.0(2) . . . . ? C15 N2 Si2 C10 32.7(3) . . . . ? C15 N2 Si2 C11 -89.1(2) . . . . ? C15 C16 N4 Th1 28.9(3) . . . . ? C15 C16 N4 C8 146.7(3) . . . . ? C15 C16 N4 C24 -87.5(3) . . . . ? N3 C23 C24 N4 -58.2(3) . . . . ? Si3 N3 C23 C24 -95.9(3) . . . . ? C23 N3 Si3 C17 154.0(2) . . . . ? C23 N3 Si3 C18 37.0(3) . . . . ? C23 N3 Si3 C19 -84.9(3) . . . . ? C23 C24 N4 Th1 24.1(3) . . . . ? C23 C24 N4 C8 -93.4(3) . . . . ? C23 C24 N4 C16 140.5(3) . . . . ? C25 N5 C27 C28 62.2(4) . . . . ? C27 N5 C25 C26 61.4(5) . . . . ? _shelx_SHELXL_version_number '2014/7' _olex2_submission_original_sample_id THBGLR _olex2_submission_special_instructions 'No special instructions were received' data_4 _nottingham_internal_coll_name THBGLS _nottingham_internal_coll_number 12096 _nottingham_internal_coll_client BMG/STL _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_time '15s, 60s' _nottingham_internal_coll_frame_width '1 degree' _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_user pczbg _nottingham_internal_coll_date 07/01/2013 _nottingham_internal_coll_location NOTTS _nottingham_internal_NCS_number ? _nottingham_internal_process_user pczbg _nottingham_internal_process_date 10/01/2013 _nottingham_internal_solution_user BMG _nottingham_internal_solution_date 10/01/2013 _nottingham_internal_refinement_user BMG _nottingham_internal_refinement_date 30/09/2014 _nottingham_internal_self_validation_user BMG _nottingham_internal_self_validation_date 30/09/2014 _nottingham_internal_self_archive_date 02/10/2014 _nottingham_internal_validation_user ? _nottingham_internal_validation_date ? _nottingham_internal_archive_date ? _refine_special_details ; The hydrogens for the two carbanion centres (C1 and C25) were initially located in the difference map, assigned a fixed C-H distance of 0.96 \%A and refined using a riding model. For H25A-D, due to disorder, the H-H distance within each disorder component was restrained to be approximately 1.6 \%A to give an H-C-H angle of approximately 120\%. Enhanced rigid bond and similarity restraints were applied to the thermal parameter of all atoms. Chemically equivalent Si-N, Si-C and C-C bonds of the disorderd fragments were restrained to be approximately equal. Some of the minor disorder components were refined isotropically. ; _audit_creation_date 2014-09-30 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C48 H112 N8 Si6 Th2' _chemical_formula_sum 'C48 H112 N8 Si6 Th2' _chemical_formula_weight 1434.07 _chemical_melting_point ? _chemical_oxdiff_formula 'C48 H112 N8 Si6 Th2' _chemical_oxdiff_usercomment 'THBGLS #12096 IN FOMBLIN FILM ON MICROMOUNT FOR BG/STL' 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' 'N' 'N' 0.0311 0.0180 '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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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' _cell_length_a 13.9997(3) _cell_length_b 21.9902(5) _cell_length_c 20.9322(5) _cell_angle_alpha 90 _cell_angle_beta 91.306(2) _cell_angle_gamma 90 _cell_volume 6442.4(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 29213 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 74.3500 _cell_measurement_theta_min 3.7950 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 16.118 _exptl_absorpt_correction_T_max 0.270 _exptl_absorpt_correction_T_min 0.041 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) (compiled Dec 19 2012,11:08:27) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2880 _exptl_crystal_size_max 0.3776 _exptl_crystal_size_mid 0.2201 _exptl_crystal_size_min 0.2145 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_unetI/netI 0.0259 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 48245 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 74.606 _diffrn_reflns_theta_min 3.744 _diffrn_ambient_temperature 120(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 10.3613 _diffrn_detector_type 'Agilent Diffraction Atlas detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -20.00 16.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -43.6627 57.0000 120.0000 36 #__ type_ start__ end____ width___ exp.time_ 2 omega 24.00 114.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 43.6627 38.0000 0.0000 90 #__ type_ start__ end____ width___ exp.time_ 3 omega 46.00 111.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 43.6627 38.0000 60.0000 65 #__ type_ start__ end____ width___ exp.time_ 4 omega -136.00 -106.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -60.0000 -95.0000 30.0000 30 #__ type_ start__ end____ width___ exp.time_ 5 omega 41.00 68.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 6 omega 40.00 77.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 -60.0000 37 #__ type_ start__ end____ width___ exp.time_ 7 omega 40.00 77.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 90.0000 37 #__ type_ start__ end____ width___ exp.time_ 8 omega 41.00 92.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -56.0000 -102.0000 51 #__ type_ start__ end____ width___ exp.time_ 9 omega 33.00 69.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 -120.0000 36 #__ type_ start__ end____ width___ exp.time_ 10 omega 129.00 158.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 30.0000 0.0000 29 #__ type_ start__ end____ width___ exp.time_ 11 omega 33.00 64.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 -90.0000 31 #__ type_ start__ end____ width___ exp.time_ 12 omega 41.00 69.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 -150.0000 28 #__ type_ start__ end____ width___ exp.time_ 13 omega 36.00 67.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 150.0000 31 #__ type_ start__ end____ width___ exp.time_ 14 omega 87.00 158.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 45.0000 -120.0000 71 #__ type_ start__ end____ width___ exp.time_ 15 omega 45.00 72.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 120.0000 27 #__ type_ start__ end____ width___ exp.time_ 16 omega 33.00 60.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 17 omega 94.00 158.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 45.0000 150.0000 64 #__ type_ start__ end____ width___ exp.time_ 18 omega 68.00 144.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 15.0000 150.0000 76 #__ type_ start__ end____ width___ exp.time_ 19 omega -115.00 -14.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -43.6627 -77.0000 -150.0000 101 #__ type_ start__ end____ width___ exp.time_ 20 omega -112.00 -19.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -43.6627 -57.0000 90.0000 93 #__ type_ start__ end____ width___ exp.time_ 21 omega 2.00 98.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 43.6627 -125.0000 120.0000 96 #__ type_ start__ end____ width___ exp.time_ 22 omega -28.00 74.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 43.6627 -77.0000 -90.0000 102 #__ type_ start__ end____ width___ exp.time_ 23 omega 36.00 122.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -125.0000 120.0000 86 #__ type_ start__ end____ width___ exp.time_ 24 omega 85.00 110.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 30.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 25 omega 33.00 69.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 -180.0000 36 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova-Duo, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0043852000 _diffrn_orient_matrix_UB_12 -0.0403465000 _diffrn_orient_matrix_UB_13 -0.0600144000 _diffrn_orient_matrix_UB_21 0.1014954000 _diffrn_orient_matrix_UB_22 0.0234828000 _diffrn_orient_matrix_UB_23 -0.0125448000 _diffrn_orient_matrix_UB_31 0.0422512000 _diffrn_orient_matrix_UB_32 -0.0522484000 _diffrn_orient_matrix_UB_33 0.0407861000 _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'microfocus sealed tube' _diffrn_source_target Cu _diffrn_source_type 'Agilent Diffraction microfocus tube' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 12453 _reflns_number_total 12869 _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 67.13 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) (compiled Dec 19 2012,11:08:27) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) (compiled Dec 19 2012,11:08:27) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) (compiled Dec 19 2012,11:08:27) ; _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 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 2.078 _refine_diff_density_min -1.699 _refine_diff_density_rms 0.170 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 807 _refine_ls_number_reflns 12869 _refine_ls_number_restraints 1609 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0514 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+94.6891P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1215 _refine_ls_wR_factor_ref 0.1221 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances H1B-H1A 1.6 with sigma of 0.02 H25C-H25D 1.6 with sigma of 0.02 H1AB-H1AA 1.6 with sigma of 0.02 H25A-H25B 1.6 with sigma of 0.02 C25A-H25D = C25-H25B = C25-H25A = C25A-H25C = C1-H1A = C1A-H1AA = C1-H1B = C1A-H1AB 0.96 with sigma of 0.001 Th1-H1AB = Th1-H1AA -3.45 with sigma of 0.02 C4A-C5A \\sim C5A-C6A \\sim C6A-C4A with sigma of 0.02 C6-C3 \\sim C5-C3 \\sim C4-C3 \\sim C6A-C3A \\sim C5A-C3A \\sim C4A-C3A with sigma of 0.02 C30A-C27A \\sim C29A-C27A \\sim C28A-C27A \\sim C30-C27 \\sim C29-C27 \\sim C28-C27 with sigma of 0.02 Si2-N2 \\sim Si2A-N2 with sigma of 0.02 Si2A-C11A \\sim Si2-C11 with sigma of 0.02 C13-C11 \\sim C12-C11 \\sim C14-C11 \\sim C13A-C11A \\sim C14A-C11A \\sim C12A-C11A with sigma of 0.02 Si2A-C9 \\sim Si2-C9A \\sim Si2A-C10A \\sim Si2-C10 with sigma of 0.02 Si1-C3 \\sim Si1A-C3A with sigma of 0.02 Si4-C26 \\sim Si4A-C26A with sigma of 0.02 Si4-C27 \\sim Si4A-C27A with sigma of 0.02 Si1A-C1 \\sim Si1-C1 with sigma of 0.02 Si1A-C1A \\sim Si1-C1 with sigma of 0.02 H1AA-H1AB \\sim H1B-H1A with sigma of 0.02 Si4-C25 \\sim Si4A-C25 with sigma of 0.02 Si4-C25 \\sim Si4A-C25A with sigma of 0.02 H25A-H25B \\sim H25C-H25D with sigma of 0.02 Th1-H1AB \\sim Th1-H1AA with sigma of 0.02 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(Si4A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(C28A)= Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)= Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C25A)=Sof(H25D)=Sof(H25C)=1-FVAR(1) Sof(Si4)=Sof(C25)=Sof(H25B)=Sof(H25A)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)= Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)= Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1) Sof(C1A)=Sof(H1AB)=Sof(H1AA)=Sof(Si1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)= Sof(C3A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)= Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(2) Sof(Si1)=Sof(C1)=Sof(H1B)=Sof(H1A)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)= Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)= Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(2) Sof(Si2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C14A)=Sof(H14A)= Sof(H14B)=Sof(H14C)=Sof(C11A)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)= Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C10A)=Sof(H10A)=Sof(H10B)= Sof(H10C)=1-FVAR(3) Sof(Si2)=Sof(C14)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C11)=Sof(C13)=Sof(H13A)= Sof(H13B)=Sof(H13C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C9)=Sof(H9A)= Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(3) 6.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,H24B), C31(H31A,H31B), C32(H32A,H32B), C39(H39A,H39B), C40(H40A,H40B), C47(H47A,H47B), C48(H48A,H48B) 6.b Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C2A(H2AA,H2AB,H2AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C17(H17A,H17B, H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A, H22B,H22C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C26A(H26D,H26E,H26F), C28A(H28D,H28E,H28F), C29A(H29D, H29E,H29F), C30A(H30D,H30E,H30F), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C41(H41A,H41B, H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A, H46B,H46C), C9A(H9AA,H9AB,H9AC), C14A(H14A,H14B,H14C), C14(H14D,H14E,H14F), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F), C13A(H13D,H13E, H13F), C9(H9A,H9B,H9C), C10A(H10A,H10B,H10C), C10(H10D,H10E,H10F) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -0.41316(2) -0.30022(2) -0.41190(2) 0.02691(8) Uani 1 1 d D . . . . N1 N -0.5369(5) -0.3671(3) -0.4305(4) 0.0363(14) Uani 1 1 d . . . . . Si1 Si -0.58860(19) -0.38590(13) -0.35837(13) 0.0331(7) Uani 0.873(6) 1 d . . P A 1 C1 C -0.5310(6) -0.3269(4) -0.3048(4) 0.0291(17) Uani 0.873(6) 1 d D . P A 1 H1B H -0.572(3) -0.2983(17) -0.285(2) 0.035 Uiso 0.873(6) 1 d DR . P A 1 H1A H -0.513(5) -0.3599(16) -0.2770(17) 0.035 Uiso 0.873(6) 1 d DR . P A 1 C1A C -0.549(2) -0.3071(12) -0.3083(12) 0.029(5) Uiso 0.127(6) 1 d D . P A 2 H1AB H -0.581(4) -0.2698(16) -0.298(2) 0.035 Uiso 0.127(6) 1 d DR . P A 2 H1AA H -0.528(3) -0.329(3) -0.2709(14) 0.035 Uiso 0.127(6) 1 d DR . P A 2 C2 C -0.5579(11) -0.4662(6) -0.3330(7) 0.044(2) Uani 0.873(6) 1 d . . P A 1 H2A H -0.591(11) -0.474(7) -0.298(8) 0.066 Uiso 0.873(6) 1 d R . P A 1 H2B H -0.566(12) -0.489(7) -0.366(7) 0.066 Uiso 0.873(6) 1 d R . P A 1 H2C H -0.493(11) -0.465(7) -0.322(7) 0.066 Uiso 0.873(6) 1 d R . P A 1 C3 C -0.7245(8) -0.3808(4) -0.3621(5) 0.0404(18) Uani 0.873(6) 1 d . . P A 1 C4 C -0.7547(9) -0.3217(6) -0.3953(6) 0.046(3) Uani 0.873(6) 1 d . . P A 1 H4A H -0.7278 -0.3204 -0.4381 0.070 Uiso 0.873(6) 1 calc GR . P A 1 H4B H -0.7312 -0.2870 -0.3703 0.070 Uiso 0.873(6) 1 calc GR . P A 1 H4C H -0.8246 -0.3200 -0.3989 0.070 Uiso 0.873(6) 1 calc GR . P A 1 C5 C -0.7659(9) -0.3823(6) -0.2947(5) 0.050(3) Uani 0.873(6) 1 d . . P A 1 H5A H -0.7396 -0.3485 -0.2694 0.075 Uiso 0.873(6) 1 calc GR . P A 1 H5B H -0.7488 -0.4209 -0.2739 0.075 Uiso 0.873(6) 1 calc GR . P A 1 H5C H -0.8356 -0.3786 -0.2977 0.075 Uiso 0.873(6) 1 calc GR . P A 1 C6 C -0.7667(9) -0.4343(6) -0.4007(7) 0.051(3) Uani 0.873(6) 1 d . . P A 1 H6A H -0.7433 -0.4727 -0.3824 0.077 Uiso 0.873(6) 1 calc GR . P A 1 H6B H -0.7470 -0.4313 -0.4452 0.077 Uiso 0.873(6) 1 calc GR . P A 1 H6C H -0.8365 -0.4332 -0.3991 0.077 Uiso 0.873(6) 1 calc GR . P A 1 Si1A Si -0.6206(12) -0.3495(9) -0.3736(8) 0.033(2) Uiso 0.127(6) 1 d . . P A 2 C2A C -0.730(6) -0.302(4) -0.405(4) 0.040(7) Uiso 0.127(6) 1 d . . P A 2 H2AA H -0.7516 -0.3175 -0.4467 0.059 Uiso 0.127(6) 1 calc GR . P A 2 H2AB H -0.7118 -0.2593 -0.4088 0.059 Uiso 0.127(6) 1 calc GR . P A 2 H2AC H -0.7825 -0.3056 -0.3746 0.059 Uiso 0.127(6) 1 calc GR . P A 2 C3A C -0.672(3) -0.4254(16) -0.348(2) 0.039(3) Uiso 0.127(6) 1 d . . P A 2 C4A C -0.601(6) -0.478(4) -0.340(4) 0.048(10) Uiso 0.127(6) 1 d . . P A 2 H4AA H -0.5508 -0.4669 -0.3082 0.072 Uiso 0.127(6) 1 calc GR . P A 2 H4AB H -0.5712 -0.4866 -0.3808 0.072 Uiso 0.127(6) 1 calc GR . P A 2 H4AC H -0.6344 -0.5143 -0.3251 0.072 Uiso 0.127(6) 1 calc GR . P A 2 C5A C -0.710(5) -0.417(4) -0.280(3) 0.043(7) Uiso 0.127(6) 1 d . . P A 2 H5AA H -0.7792 -0.4227 -0.2809 0.065 Uiso 0.127(6) 1 calc GR . P A 2 H5AB H -0.6946 -0.3757 -0.2649 0.065 Uiso 0.127(6) 1 calc GR . P A 2 H5AC H -0.6798 -0.4468 -0.2512 0.065 Uiso 0.127(6) 1 calc GR . P A 2 C6A C -0.757(5) -0.455(4) -0.384(4) 0.042(8) Uiso 0.127(6) 1 d . . P A 2 H6AA H -0.7865 -0.4850 -0.3563 0.063 Uiso 0.127(6) 1 calc GR . P A 2 H6AB H -0.7339 -0.4746 -0.4226 0.063 Uiso 0.127(6) 1 calc GR . P A 2 H6AC H -0.8034 -0.4233 -0.3956 0.063 Uiso 0.127(6) 1 calc GR . P A 2 C7 C -0.5613(7) -0.3986(5) -0.4895(4) 0.0424(19) Uani 1 1 d . . . . . H7A H -0.6160 -0.3781 -0.5112 0.051 Uiso 1 1 calc R . . . . H7B H -0.5799 -0.4410 -0.4801 0.051 Uiso 1 1 calc R . . . . C8 C -0.4759(7) -0.3982(4) -0.5324(4) 0.0398(17) Uani 1 1 d . . . . . H8A H -0.4291 -0.4291 -0.5175 0.048 Uiso 1 1 calc R . . . . H8B H -0.4965 -0.4086 -0.5766 0.048 Uiso 1 1 calc R . . . . N2 N -0.4210(6) -0.2212(4) -0.4857(4) 0.0386(14) Uani 1 1 d . . . . . Si2 Si -0.3453(5) -0.1667(3) -0.5216(3) 0.0430(13) Uani 0.608(10) 1 d . . P B 1 C15 C -0.5080(8) -0.2387(5) -0.5225(5) 0.048(2) Uani 1 1 d . . . . . H15A H -0.5311 -0.2035 -0.5479 0.057 Uiso 1 1 calc R . . . . H15B H -0.5587 -0.2502 -0.4925 0.057 Uiso 1 1 calc R . . . . C16 C -0.4888(8) -0.2919(5) -0.5671(5) 0.047(2) Uani 1 1 d . . . . . H16A H -0.5500 -0.3100 -0.5822 0.057 Uiso 1 1 calc R . . . . H16B H -0.4538 -0.2775 -0.6047 0.057 Uiso 1 1 calc R . . . . N3 N -0.2885(5) -0.3636(3) -0.4408(3) 0.0294(13) Uani 1 1 d . . . . . Si3 Si -0.24398(17) -0.41702(11) -0.38791(11) 0.0306(5) Uani 1 1 d . . . . . C17 C -0.2958(8) -0.4949(5) -0.4044(5) 0.047(2) Uani 1 1 d . . . . . H17A H -0.2760 -0.5088 -0.4465 0.070 Uiso 1 1 calc GR . . . . H17B H -0.3657 -0.4927 -0.4035 0.070 Uiso 1 1 calc GR . . . . H17C H -0.2726 -0.5234 -0.3716 0.070 Uiso 1 1 calc GR . . . . C18 C -0.2842(7) -0.3936(4) -0.3065(4) 0.0384(19) Uani 1 1 d . . . . . H18A H -0.3529 -0.3848 -0.3083 0.058 Uiso 1 1 calc GR . . . . H18B H -0.2492 -0.3571 -0.2927 0.058 Uiso 1 1 calc GR . . . . H18C H -0.2716 -0.4266 -0.2760 0.058 Uiso 1 1 calc GR . . . . C19 C -0.1081(7) -0.4231(4) -0.3866(4) 0.0388(17) Uani 1 1 d . . . . . C20 C -0.0737(8) -0.4623(5) -0.4428(5) 0.050(2) Uani 1 1 d . . . . . H20A H -0.0943 -0.4435 -0.4833 0.075 Uiso 1 1 calc GR . . . . H20B H -0.1012 -0.5031 -0.4397 0.075 Uiso 1 1 calc GR . . . . H20C H -0.0039 -0.4651 -0.4409 0.075 Uiso 1 1 calc GR . . . . C21 C -0.0728(8) -0.4531(5) -0.3243(5) 0.052(2) Uani 1 1 d . . . . . H21A H -0.1046 -0.4925 -0.3193 0.078 Uiso 1 1 calc GR . . . . H21B H -0.0876 -0.4268 -0.2881 0.078 Uiso 1 1 calc GR . . . . H21C H -0.0035 -0.4593 -0.3258 0.078 Uiso 1 1 calc GR . . . . C22 C -0.0642(8) -0.3593(5) -0.3930(5) 0.050(2) Uani 1 1 d . . . . . H22A H -0.0800 -0.3348 -0.3556 0.075 Uiso 1 1 calc GR . . . . H22B H -0.0899 -0.3397 -0.4317 0.075 Uiso 1 1 calc GR . . . . H22C H 0.0054 -0.3628 -0.3958 0.075 Uiso 1 1 calc GR . . . . C23 C -0.2673(7) -0.3757(5) -0.5087(4) 0.0379(17) Uani 1 1 d . . . . . H23A H -0.2754 -0.4197 -0.5174 0.045 Uiso 1 1 calc R . . . . H23B H -0.2000 -0.3650 -0.5166 0.045 Uiso 1 1 calc R . . . . C24 C -0.3320(7) -0.3398(5) -0.5538(4) 0.0389(17) Uani 1 1 d . . . . . H24A H -0.3075 -0.2977 -0.5573 0.047 Uiso 1 1 calc R . . . . H24B H -0.3310 -0.3585 -0.5968 0.047 Uiso 1 1 calc R . . . . N4 N -0.4310(6) -0.3382(4) -0.5316(4) 0.0391(14) Uani 1 1 d . . . . . Th2 Th -0.44334(2) -0.24610(2) -0.22298(2) 0.02778(8) Uani 1 1 d . . . . . N5 N -0.3036(5) -0.2001(4) -0.1907(4) 0.0416(15) Uani 1 1 d . . . . . Si4 Si -0.2506(2) -0.17586(15) -0.26264(16) 0.0322(8) Uani 0.735(6) 1 d . . P A 1 C25 C -0.3167(9) -0.2336(6) -0.3187(6) 0.031(2) Uani 0.735(6) 1 d D . P A 1 H25B H -0.320(8) -0.2068(19) -0.3549(15) 0.037 Uiso 0.735(6) 1 d DR . P A 1 H25A H -0.270(3) -0.2653(16) -0.324(4) 0.037 Uiso 0.735(6) 1 d DR . P A 1 C26 C -0.2723(11) -0.0935(6) -0.2811(7) 0.039(3) Uani 0.735(6) 1 d . . P A 1 H26A H -0.3409 -0.0866 -0.2881 0.059 Uiso 0.735(6) 1 calc GR . P A 1 H26B H -0.2382 -0.0823 -0.3197 0.059 Uiso 0.735(6) 1 calc GR . P A 1 H26C H -0.2491 -0.0686 -0.2452 0.059 Uiso 0.735(6) 1 calc GR . P A 1 C27 C -0.1162(8) -0.1898(5) -0.2609(5) 0.0354(18) Uani 0.735(6) 1 d . . P A 1 C28 C -0.0944(10) -0.2519(6) -0.2304(7) 0.039(3) Uani 0.735(6) 1 d . . P A 1 H28A H -0.1301 -0.2836 -0.2536 0.058 Uiso 0.735(6) 1 calc GR . P A 1 H28B H -0.1134 -0.2515 -0.1856 0.058 Uiso 0.735(6) 1 calc GR . P A 1 H28C H -0.0258 -0.2603 -0.2326 0.058 Uiso 0.735(6) 1 calc GR . P A 1 C29 C -0.0674(10) -0.1396(7) -0.2204(7) 0.039(3) Uani 0.735(6) 1 d . . P A 1 H29A H -0.0958 -0.1384 -0.1781 0.059 Uiso 0.735(6) 1 calc GR . P A 1 H29B H -0.0764 -0.1002 -0.2415 0.059 Uiso 0.735(6) 1 calc GR . P A 1 H29C H 0.0010 -0.1484 -0.2158 0.059 Uiso 0.735(6) 1 calc GR . P A 1 C30 C -0.0745(9) -0.1888(7) -0.3281(5) 0.040(3) Uani 0.735(6) 1 d . . P A 1 H30A H -0.0826 -0.1482 -0.3467 0.059 Uiso 0.735(6) 1 calc GR . P A 1 H30B H -0.1079 -0.2187 -0.3552 0.059 Uiso 0.735(6) 1 calc GR . P A 1 H30C H -0.0063 -0.1989 -0.3254 0.059 Uiso 0.735(6) 1 calc GR . P A 1 Si4A Si -0.2211(6) -0.2150(5) -0.2468(4) 0.0347(18) Uani 0.265(6) 1 d . . P A 2 C26A C -0.123(2) -0.2714(16) -0.229(2) 0.039(5) Uani 0.265(6) 1 d . . P A 2 H26D H -0.0693 -0.2637 -0.2571 0.059 Uiso 0.265(6) 1 calc GR . P A 2 H26E H -0.1472 -0.3127 -0.2364 0.059 Uiso 0.265(6) 1 calc GR . P A 2 H26F H -0.1016 -0.2672 -0.1844 0.059 Uiso 0.265(6) 1 calc GR . P A 2 C27A C -0.1643(18) -0.1379(10) -0.2635(12) 0.037(3) Uani 0.265(6) 1 d . . P A 2 C28A C -0.241(3) -0.0884(17) -0.269(2) 0.037(5) Uani 0.265(6) 1 d . . P A 2 H28D H -0.2833 -0.0911 -0.2320 0.056 Uiso 0.265(6) 1 calc GR . P A 2 H28E H -0.2790 -0.0941 -0.3083 0.056 Uiso 0.265(6) 1 calc GR . P A 2 H28F H -0.2108 -0.0483 -0.2692 0.056 Uiso 0.265(6) 1 calc GR . P A 2 C29A C -0.094(2) -0.1199(19) -0.2090(17) 0.036(5) Uani 0.265(6) 1 d . . P A 2 H29D H -0.0406 -0.1485 -0.2075 0.054 Uiso 0.265(6) 1 calc GR . P A 2 H29E H -0.1274 -0.1210 -0.1682 0.054 Uiso 0.265(6) 1 calc GR . P A 2 H29F H -0.0704 -0.0787 -0.2165 0.054 Uiso 0.265(6) 1 calc GR . P A 2 C30A C -0.110(3) -0.1406(19) -0.3259(14) 0.044(5) Uani 0.265(6) 1 d . . P A 2 H30D H -0.1556 -0.1422 -0.3621 0.066 Uiso 0.265(6) 1 calc GR . P A 2 H30E H -0.0697 -0.1771 -0.3261 0.066 Uiso 0.265(6) 1 calc GR . P A 2 H30F H -0.0697 -0.1044 -0.3296 0.066 Uiso 0.265(6) 1 calc GR . P A 2 C31 C -0.2835(8) -0.1714(6) -0.1294(5) 0.057(2) Uani 1 1 d . . . . . H31A H -0.2885 -0.1267 -0.1339 0.069 Uiso 1 1 calc R . . . . H31B H -0.2176 -0.1813 -0.1148 0.069 Uiso 1 1 calc R . . . . C32 C -0.3548(7) -0.1938(6) -0.0801(5) 0.051(2) Uani 1 1 d . . . . . H32A H -0.3372 -0.2353 -0.0660 0.062 Uiso 1 1 calc R . . . . H32B H -0.3525 -0.1668 -0.0423 0.062 Uiso 1 1 calc R . . . . N6 N -0.5515(6) -0.1661(4) -0.2224(3) 0.0370(15) Uani 1 1 d . . . . . Si5 Si -0.60817(19) -0.13292(12) -0.28895(12) 0.0380(5) Uani 1 1 d . . . . . C33 C -0.5715(7) -0.1773(5) -0.3606(4) 0.041(2) Uani 1 1 d . . . . . H33A H -0.6089 -0.2149 -0.3634 0.061 Uiso 1 1 calc GR . . . . H33B H -0.5034 -0.1872 -0.3567 0.061 Uiso 1 1 calc GR . . . . H33C H -0.5831 -0.1530 -0.3992 0.061 Uiso 1 1 calc GR . . . . C34 C -0.5694(9) -0.0520(5) -0.3014(5) 0.053(2) Uani 1 1 d . . . . . H34A H -0.5001 -0.0507 -0.3069 0.080 Uiso 1 1 calc GR . . . . H34B H -0.5863 -0.0275 -0.2642 0.080 Uiso 1 1 calc GR . . . . H34C H -0.6017 -0.0356 -0.3398 0.080 Uiso 1 1 calc GR . . . . C35 C -0.7442(7) -0.1350(5) -0.2849(5) 0.0458(19) Uani 1 1 d . . . . . C36 C -0.7755(7) -0.1955(5) -0.2553(5) 0.049(2) Uani 1 1 d . . . . . H36A H -0.7539 -0.1971 -0.2105 0.074 Uiso 1 1 calc GR . . . . H36B H -0.7474 -0.2293 -0.2789 0.074 Uiso 1 1 calc GR . . . . H36C H -0.8454 -0.1985 -0.2577 0.074 Uiso 1 1 calc GR . . . . C37 C -0.7837(9) -0.0826(6) -0.2449(6) 0.059(3) Uani 1 1 d . . . . . H37A H -0.7652 -0.0437 -0.2638 0.089 Uiso 1 1 calc GR . . . . H37B H -0.7577 -0.0853 -0.2012 0.089 Uiso 1 1 calc GR . . . . H37C H -0.8536 -0.0854 -0.2443 0.089 Uiso 1 1 calc GR . . . . C38 C -0.7874(9) -0.1299(6) -0.3535(5) 0.060(3) Uani 1 1 d . . . . . H38A H -0.7670 -0.1648 -0.3788 0.090 Uiso 1 1 calc GR . . . . H38B H -0.7652 -0.0923 -0.3733 0.090 Uiso 1 1 calc GR . . . . H38C H -0.8573 -0.1294 -0.3516 0.090 Uiso 1 1 calc GR . . . . C39 C -0.5744(8) -0.1336(5) -0.1632(4) 0.0456(19) Uani 1 1 d . . . . . H39A H -0.6286 -0.1541 -0.1425 0.055 Uiso 1 1 calc R . . . . H39B H -0.5945 -0.0916 -0.1738 0.055 Uiso 1 1 calc R . . . . C40 C -0.4908(8) -0.1316(5) -0.1174(5) 0.0465(19) Uani 1 1 d . . . . . H40A H -0.4406 -0.1048 -0.1344 0.056 Uiso 1 1 calc R . . . . H40B H -0.5109 -0.1149 -0.0759 0.056 Uiso 1 1 calc R . . . . N7 N -0.4569(6) -0.3154(4) -0.1407(3) 0.0388(15) Uani 1 1 d . . . . . Si6 Si -0.3956(2) -0.37214(15) -0.09907(13) 0.0520(7) Uani 1 1 d . . . . . C41 C -0.3992(11) -0.3609(7) -0.0097(5) 0.075(4) Uani 1 1 d . . . . . H41A H -0.3690 -0.3220 0.0017 0.113 Uiso 1 1 calc GR . . . . H41B H -0.3647 -0.3941 0.0118 0.113 Uiso 1 1 calc GR . . . . H41C H -0.4658 -0.3606 0.0038 0.113 Uiso 1 1 calc GR . . . . C42 C -0.2681(9) -0.3702(7) -0.1243(6) 0.067(3) Uani 1 1 d . . . . . H42A H -0.2361 -0.4079 -0.1110 0.100 Uiso 1 1 calc GR . . . . H42B H -0.2356 -0.3354 -0.1042 0.100 Uiso 1 1 calc GR . . . . H42C H -0.2660 -0.3663 -0.1709 0.100 Uiso 1 1 calc GR . . . . C43 C -0.4480(10) -0.4505(6) -0.1150(5) 0.061(2) Uani 1 1 d . . . . . C44 C -0.5560(10) -0.4500(6) -0.1059(7) 0.073(3) Uani 1 1 d . . . . . H44A H -0.5853 -0.4190 -0.1338 0.109 Uiso 1 1 calc GR . . . . H44B H -0.5696 -0.4406 -0.0613 0.109 Uiso 1 1 calc GR . . . . H44C H -0.5825 -0.4900 -0.1170 0.109 Uiso 1 1 calc GR . . . . C45 C -0.4007(12) -0.4986(7) -0.0730(6) 0.083(4) Uani 1 1 d . . . . . H45A H -0.4091 -0.4882 -0.0280 0.124 Uiso 1 1 calc GR . . . . H45B H -0.3324 -0.5005 -0.0820 0.124 Uiso 1 1 calc GR . . . . H45C H -0.4300 -0.5383 -0.0820 0.124 Uiso 1 1 calc GR . . . . C46 C -0.4327(11) -0.4677(6) -0.1846(6) 0.069(3) Uani 1 1 d . . . . . H46A H -0.3647 -0.4755 -0.1911 0.103 Uiso 1 1 calc GR . . . . H46B H -0.4541 -0.4342 -0.2124 0.103 Uiso 1 1 calc GR . . . . H46C H -0.4696 -0.5044 -0.1951 0.103 Uiso 1 1 calc GR . . . . C47 C -0.5429(7) -0.2900(5) -0.1119(4) 0.0400(18) Uani 1 1 d . . . . . H47A H -0.5727 -0.3210 -0.0845 0.048 Uiso 1 1 calc R . . . . H47B H -0.5896 -0.2785 -0.1460 0.048 Uiso 1 1 calc R . . . . C48 C -0.5165(7) -0.2334(5) -0.0713(4) 0.0423(18) Uani 1 1 d . . . . . H48A H -0.5751 -0.2107 -0.0606 0.051 Uiso 1 1 calc R . . . . H48B H -0.4841 -0.2461 -0.0309 0.051 Uiso 1 1 calc R . . . . N8 N -0.4525(6) -0.1942(4) -0.1083(4) 0.0422(15) Uani 1 1 d . . . . . Si2A Si -0.3593(7) -0.1562(4) -0.4988(5) 0.0390(17) Uani 0.392(10) 1 d . . P B 2 C9A C -0.2254(17) -0.1868(16) -0.4866(19) 0.041(5) Uani 0.392(10) 1 d . . P B 2 H9AA H -0.2178 -0.2249 -0.5103 0.061 Uiso 0.392(10) 1 calc GR . P B 2 H9AB H -0.2123 -0.1942 -0.4410 0.061 Uiso 0.392(10) 1 calc GR . P B 2 H9AC H -0.1805 -0.1564 -0.5023 0.061 Uiso 0.392(10) 1 calc GR . P B 2 C14A C -0.337(3) -0.1778(16) -0.6300(14) 0.056(5) Uani 0.392(10) 1 d . . P B 2 H14A H -0.3731 -0.2151 -0.6222 0.084 Uiso 0.392(10) 1 calc GR . P B 2 H14B H -0.2685 -0.1859 -0.6228 0.084 Uiso 0.392(10) 1 calc GR . P B 2 H14C H -0.3480 -0.1645 -0.6742 0.084 Uiso 0.392(10) 1 calc GR . P B 2 C14 C -0.3798(17) -0.0683(11) -0.4367(8) 0.061(4) Uani 0.608(10) 1 d . . P B 1 H14D H -0.3125 -0.0680 -0.4227 0.091 Uiso 0.608(10) 1 calc GR . P B 1 H14E H -0.4149 -0.0980 -0.4115 0.091 Uiso 0.608(10) 1 calc GR . P B 1 H14F H -0.4073 -0.0278 -0.4307 0.091 Uiso 0.608(10) 1 calc GR . P B 1 C11 C -0.3871(11) -0.0857(7) -0.5080(7) 0.050(2) Uani 0.608(10) 1 d . . P B 1 C13 C -0.3265(16) -0.0392(9) -0.5449(10) 0.063(4) Uani 0.608(10) 1 d . . P B 1 H13A H -0.3446 -0.0405 -0.5904 0.095 Uiso 0.608(10) 1 calc GR . P B 1 H13B H -0.2586 -0.0494 -0.5396 0.095 Uiso 0.608(10) 1 calc GR . P B 1 H13C H -0.3378 0.0017 -0.5282 0.095 Uiso 0.608(10) 1 calc GR . P B 1 C12 C -0.4924(13) -0.0790(10) -0.5289(11) 0.066(4) Uani 0.608(10) 1 d . . P B 1 H12A H -0.5304 -0.1105 -0.5083 0.100 Uiso 0.608(10) 1 calc GR . P B 1 H12B H -0.4984 -0.0834 -0.5755 0.100 Uiso 0.608(10) 1 calc GR . P B 1 H12C H -0.5157 -0.0388 -0.5165 0.100 Uiso 0.608(10) 1 calc GR . P B 1 C11A C -0.3691(15) -0.1276(10) -0.5839(9) 0.047(3) Uani 0.392(10) 1 d . . P B 2 C12A C -0.309(2) -0.0692(12) -0.5858(15) 0.057(5) Uani 0.392(10) 1 d . . P B 2 H12D H -0.2542 -0.0730 -0.5559 0.085 Uiso 0.392(10) 1 calc GR . P B 2 H12E H -0.3479 -0.0344 -0.5737 0.085 Uiso 0.392(10) 1 calc GR . P B 2 H12F H -0.2854 -0.0631 -0.6291 0.085 Uiso 0.392(10) 1 calc GR . P B 2 C13A C -0.4710(17) -0.1111(15) -0.6067(15) 0.058(5) Uani 0.392(10) 1 d . . P B 2 H13D H -0.4993 -0.0829 -0.5762 0.088 Uiso 0.392(10) 1 calc GR . P B 2 H13E H -0.5098 -0.1481 -0.6097 0.088 Uiso 0.392(10) 1 calc GR . P B 2 H13F H -0.4687 -0.0917 -0.6489 0.088 Uiso 0.392(10) 1 calc GR . P B 2 C9 C -0.2295(11) -0.1682(10) -0.4784(10) 0.036(4) Uani 0.608(10) 1 d . . P B 1 H9A H -0.1952 -0.2056 -0.4891 0.055 Uiso 0.608(10) 1 calc GR . P B 1 H9B H -0.2400 -0.1670 -0.4323 0.055 Uiso 0.608(10) 1 calc GR . P B 1 H9C H -0.1915 -0.1329 -0.4907 0.055 Uiso 0.608(10) 1 calc GR . P B 1 C10A C -0.397(2) -0.0903(11) -0.4483(14) 0.050(5) Uani 0.392(10) 1 d . . P B 2 H10A H -0.4034 -0.1038 -0.4040 0.074 Uiso 0.392(10) 1 calc GR . P B 2 H10B H -0.4582 -0.0746 -0.4645 0.074 Uiso 0.392(10) 1 calc GR . P B 2 H10C H -0.3484 -0.0582 -0.4501 0.074 Uiso 0.392(10) 1 calc GR . P B 2 C10 C -0.3260(17) -0.1735(11) -0.6099(7) 0.053(4) Uani 0.608(10) 1 d . . P B 1 H10D H -0.3875 -0.1707 -0.6330 0.080 Uiso 0.608(10) 1 calc GR . P B 1 H10E H -0.2962 -0.2128 -0.6191 0.080 Uiso 0.608(10) 1 calc GR . P B 1 H10F H -0.2841 -0.1406 -0.6238 0.080 Uiso 0.608(10) 1 calc GR . P B 1 C25A C -0.315(2) -0.2177(11) -0.3202(12) 0.028(3) Uani 0.265(6) 1 d D . P A 2 H25D H -0.316(19) -0.1774(13) -0.338(3) 0.033 Uiso 0.265(6) 1 d DR . P A 2 H25C H -0.300(9) -0.2481(19) -0.351(2) 0.033 Uiso 0.265(6) 1 d DR . 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 Th1 0.02474(14) 0.03446(15) 0.02147(13) -0.00285(10) -0.00065(10) -0.00236(10) N1 0.034(3) 0.040(3) 0.035(3) -0.009(2) 0.000(2) -0.012(3) Si1 0.0300(13) 0.0361(14) 0.0334(13) -0.0068(11) 0.0023(10) -0.0066(11) C1 0.027(3) 0.034(3) 0.026(3) 0.001(3) 0.002(3) -0.001(3) C2 0.047(6) 0.040(4) 0.047(6) -0.006(4) 0.010(5) -0.005(4) C3 0.034(3) 0.045(3) 0.042(3) -0.004(3) 0.002(3) -0.007(3) C4 0.038(6) 0.055(5) 0.046(6) -0.003(4) 0.001(5) 0.000(4) C5 0.041(5) 0.057(6) 0.051(5) -0.006(4) 0.008(4) -0.009(5) C6 0.040(5) 0.056(5) 0.057(6) -0.012(5) 0.002(5) -0.014(5) C7 0.042(4) 0.051(4) 0.034(4) -0.012(3) -0.001(3) -0.011(3) C8 0.043(4) 0.046(4) 0.030(4) -0.008(3) -0.003(3) -0.003(3) N2 0.043(3) 0.043(3) 0.030(3) 0.004(2) -0.007(2) 0.001(2) Si2 0.052(3) 0.049(3) 0.027(3) 0.011(2) -0.007(2) -0.009(2) C15 0.048(4) 0.048(4) 0.045(4) 0.006(3) -0.016(3) 0.001(3) C16 0.050(4) 0.050(4) 0.041(4) 0.003(3) -0.013(3) -0.001(3) N3 0.033(3) 0.038(3) 0.018(3) 0.003(2) 0.005(2) 0.005(2) Si3 0.0328(11) 0.0343(11) 0.0248(10) 0.0029(9) 0.0036(9) 0.0004(9) C17 0.054(5) 0.040(4) 0.046(5) 0.000(4) 0.002(4) -0.001(4) C18 0.042(5) 0.046(5) 0.027(4) 0.005(3) 0.009(3) -0.002(4) C19 0.034(3) 0.046(4) 0.036(4) 0.002(3) 0.004(3) 0.006(3) C20 0.046(5) 0.053(5) 0.050(5) -0.003(4) 0.007(4) 0.011(4) C21 0.046(5) 0.065(6) 0.045(5) 0.009(4) -0.007(4) 0.008(5) C22 0.043(5) 0.053(5) 0.053(6) 0.002(4) 0.000(4) -0.001(4) C23 0.040(4) 0.050(4) 0.024(3) -0.001(3) 0.006(3) 0.003(3) C24 0.046(4) 0.051(4) 0.020(3) 0.000(3) -0.001(3) -0.003(3) N4 0.040(3) 0.046(3) 0.031(3) -0.001(2) -0.004(2) -0.001(3) Th2 0.02525(14) 0.03774(16) 0.02031(13) -0.00362(11) -0.00003(10) -0.00353(11) N5 0.031(3) 0.061(4) 0.033(3) -0.011(3) -0.004(2) -0.014(3) Si4 0.0258(14) 0.0367(17) 0.0338(16) -0.0001(13) -0.0055(12) -0.0085(12) C25 0.026(4) 0.040(5) 0.027(4) -0.008(4) 0.004(3) -0.008(4) C26 0.038(6) 0.041(5) 0.039(6) -0.007(4) -0.008(5) -0.008(4) C27 0.027(3) 0.044(4) 0.034(4) 0.000(3) -0.004(3) -0.007(3) C28 0.028(5) 0.047(5) 0.041(6) 0.001(5) 0.001(5) -0.003(4) C29 0.031(6) 0.049(6) 0.038(6) -0.004(5) -0.002(5) -0.010(4) C30 0.032(5) 0.054(7) 0.033(5) 0.001(4) -0.003(4) -0.004(5) Si4A 0.029(3) 0.043(4) 0.031(3) -0.003(3) -0.008(3) -0.005(3) C26A 0.028(8) 0.046(8) 0.042(10) -0.001(8) -0.007(8) -0.007(7) C27A 0.031(5) 0.044(4) 0.035(5) -0.002(4) -0.005(4) -0.007(4) C28A 0.030(8) 0.042(7) 0.038(10) 0.001(7) -0.007(7) -0.009(7) C29A 0.027(8) 0.045(9) 0.036(8) -0.005(7) -0.002(7) -0.003(7) C30A 0.039(8) 0.052(9) 0.040(7) -0.002(6) 0.001(6) -0.009(7) C31 0.046(4) 0.083(5) 0.042(4) -0.018(4) -0.004(3) -0.016(4) C32 0.045(4) 0.074(5) 0.035(4) -0.012(4) -0.007(3) -0.006(4) N6 0.042(3) 0.041(3) 0.029(3) -0.007(2) 0.008(2) 0.008(3) Si5 0.0413(13) 0.0413(13) 0.0315(12) -0.0014(10) 0.0027(10) 0.0048(10) C33 0.043(5) 0.050(5) 0.030(4) -0.002(3) -0.001(3) 0.004(4) C34 0.067(6) 0.043(4) 0.050(6) 0.001(4) -0.002(5) 0.004(4) C35 0.042(4) 0.055(4) 0.040(4) 0.002(3) 0.002(3) 0.009(3) C36 0.041(5) 0.061(5) 0.046(5) 0.000(4) 0.006(4) 0.005(4) C37 0.058(6) 0.063(6) 0.057(6) -0.006(5) 0.013(5) 0.013(5) C38 0.052(6) 0.078(7) 0.051(5) 0.003(5) -0.004(4) 0.015(5) C39 0.058(4) 0.049(4) 0.030(3) -0.008(3) 0.008(3) 0.009(4) C40 0.058(4) 0.051(4) 0.031(4) -0.009(3) 0.005(3) -0.002(3) N7 0.043(3) 0.053(3) 0.021(3) 0.005(3) 0.004(2) 0.002(3) Si6 0.0655(18) 0.0649(17) 0.0259(12) 0.0117(12) 0.0039(12) 0.0167(14) C41 0.100(9) 0.093(8) 0.034(4) 0.010(5) -0.001(5) 0.025(7) C42 0.062(5) 0.087(8) 0.051(6) 0.004(6) -0.003(4) 0.020(5) C43 0.084(5) 0.062(4) 0.039(4) 0.015(3) 0.015(4) 0.011(4) C44 0.092(6) 0.058(7) 0.070(7) 0.010(6) 0.024(5) 0.006(5) C45 0.119(9) 0.076(7) 0.053(6) 0.020(5) 0.013(6) 0.027(6) C46 0.100(8) 0.061(6) 0.045(5) 0.015(4) 0.012(5) 0.007(6) C47 0.043(4) 0.054(4) 0.024(3) 0.001(3) 0.008(3) -0.004(3) C48 0.046(4) 0.056(4) 0.026(3) -0.003(3) 0.006(3) -0.001(3) N8 0.043(3) 0.054(3) 0.030(3) -0.004(3) -0.001(2) -0.005(3) Si2A 0.041(3) 0.044(3) 0.032(4) 0.002(3) -0.002(3) -0.003(3) C9A 0.045(6) 0.048(11) 0.028(10) 0.004(9) -0.002(6) -0.004(6) C14A 0.067(10) 0.064(8) 0.037(9) 0.007(7) -0.002(8) -0.002(8) C14 0.071(9) 0.062(9) 0.049(6) 0.006(6) 0.005(6) -0.017(7) C11 0.055(5) 0.052(4) 0.042(5) 0.008(4) -0.001(4) -0.008(4) C13 0.076(8) 0.064(8) 0.050(8) 0.016(6) 0.000(7) -0.016(7) C12 0.065(6) 0.059(8) 0.075(9) 0.010(7) -0.007(6) -0.004(6) C11A 0.052(5) 0.054(5) 0.034(5) 0.010(4) -0.001(4) -0.006(4) C12A 0.059(9) 0.060(8) 0.052(10) 0.014(7) 0.000(8) -0.010(7) C13A 0.057(7) 0.063(10) 0.055(10) 0.019(8) -0.004(6) -0.005(6) C9 0.044(5) 0.048(9) 0.017(6) -0.004(6) 0.005(4) 0.003(5) C10A 0.061(9) 0.048(8) 0.040(8) -0.002(6) 0.005(7) -0.008(7) C10 0.064(8) 0.064(8) 0.031(6) 0.006(5) -0.009(6) -0.005(7) C25A 0.024(5) 0.033(6) 0.026(5) -0.004(4) 0.000(4) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 N1 2.299(7) . ? Th1 C1 2.875(9) . ? Th1 C1A 2.92(3) . ? Th1 N2 2.325(8) . ? Th1 N3 2.325(7) . ? Th1 N4 2.648(7) . ? Th1 C25 2.767(10) . ? Th1 C25A 2.955(18) . ? Th1 H25C 2.31(11) . ? N1 Si1 1.739(8) . ? N1 Si1A 1.73(2) . ? N1 C7 1.449(11) . ? Si1 C1 1.884(9) . ? Si1 C2 1.890(13) . ? Si1 C3 1.906(11) . ? C1 H1B 0.9600(10) . ? C1 H1A 0.9600(10) . ? C1 Th2 2.739(9) . ? C1A H1AB 0.9600(10) . ? C1A H1AA 0.9600(10) . ? C1A Si1A 1.920(19) . ? C1A Th2 2.656(19) . ? C2 H2A 0.89(15) . ? C2 H2B 0.86(16) . ? C2 H2C 0.93(15) . ? C3 C4 1.527(12) . ? C3 C5 1.539(12) . ? C3 C6 1.539(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Si1A C2A 1.96(9) . ? Si1A C3A 1.90(2) . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C3A C4A 1.534(18) . ? C3A C5A 1.536(18) . ? C3A C6A 1.536(18) . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? C5A H5AA 0.9800 . ? C5A H5AB 0.9800 . ? C5A H5AC 0.9800 . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.511(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 N4 1.461(12) . ? N2 Si2 1.779(10) . ? N2 C15 1.477(12) . ? N2 Si2A 1.696(12) . ? Si2 C11 1.899(17) . ? Si2 C9 1.840(17) . ? Si2 C10 1.881(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.524(15) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N4 1.489(12) . ? N3 Si3 1.722(7) . ? N3 C23 1.481(10) . ? Si3 C17 1.888(10) . ? Si3 C18 1.879(9) . ? Si3 C19 1.906(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.544(13) . ? C19 C21 1.533(13) . ? C19 C22 1.539(14) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.515(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 N4 1.472(12) . ? Th2 H1B 2.48(6) . ? Th2 H1AB 2.51(7) . ? Th2 H1AA 2.38(7) . ? Th2 N5 2.290(7) . ? Th2 C25 2.720(14) . ? Th2 N6 2.321(7) . ? Th2 N7 2.311(7) . ? Th2 N8 2.663(8) . ? Th2 C25A 2.81(4) . ? N5 Si4 1.776(9) . ? N5 Si4A 1.698(12) . ? N5 C31 1.452(12) . ? Si4 C25 1.948(10) . ? Si4 C26 1.875(14) . ? Si4 C27 1.907(12) . ? C25 H25B 0.9600(10) . ? C25 H25A 0.9600(11) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.536(13) . ? C27 C29 1.541(12) . ? C27 C30 1.536(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? Si4A C26A 1.88(2) . ? Si4A C27A 1.91(2) . ? Si4A C25A 2.002(17) . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C27A C28A 1.535(17) . ? C27A C29A 1.538(17) . ? C27A C30A 1.528(17) . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.533(15) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 N8 1.477(12) . ? N6 Si5 1.747(8) . ? N6 C39 1.473(11) . ? Si5 C33 1.871(9) . ? Si5 C34 1.880(11) . ? Si5 C35 1.909(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.535(15) . ? C35 C37 1.534(15) . ? C35 C38 1.549(14) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.497(14) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 N8 1.489(13) . ? N7 Si6 1.737(8) . ? N7 C47 1.469(12) . ? Si6 C41 1.889(12) . ? Si6 C42 1.873(13) . ? Si6 C43 1.900(14) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.528(19) . ? C43 C45 1.518(17) . ? C43 C46 1.526(16) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.547(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C48 N8 1.476(12) . ? Si2A C9A 2.00(2) . ? Si2A C11A 1.892(19) . ? Si2A C10A 1.876(17) . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C14A C11A 1.542(18) . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C14 C11 1.541(16) . ? C11 C13 1.547(15) . ? C11 C12 1.536(16) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11A C12A 1.539(17) . ? C11A C13A 1.537(17) . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C25A H25D 0.9600(10) . ? C25A H25C 0.9600(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Th1 C1 63.7(3) . . ? N1 Th1 C1A 65.9(4) . . ? N1 Th1 N2 109.9(3) . . ? N1 Th1 N3 98.0(3) . . ? N1 Th1 N4 65.4(3) . . ? N1 Th1 C25 144.3(3) . . ? N1 Th1 C25A 147.0(7) . . ? N1 Th1 H25C 156.2(15) . . ? C1A Th1 C25A 81.3(8) . . ? C1A Th1 H25C 94(2) . . ? N2 Th1 C1 130.7(3) . . ? N2 Th1 C1A 120.7(6) . . ? N2 Th1 N4 66.7(3) . . ? N2 Th1 C25 95.0(3) . . ? N2 Th1 C25A 89.3(5) . . ? N2 Th1 H25C 90.9(13) . . ? N3 Th1 C1 121.9(3) . . ? N3 Th1 C1A 131.9(6) . . ? N3 Th1 N2 107.4(3) . . ? N3 Th1 N4 67.6(2) . . ? N3 Th1 C25 98.3(3) . . ? N3 Th1 C25A 101.4(7) . . ? N3 Th1 H25C 86(2) . . ? N4 Th1 C1 129.1(2) . . ? N4 Th1 C1A 129.6(4) . . ? N4 Th1 C25 150.2(3) . . ? N4 Th1 C25A 147.2(7) . . ? N4 Th1 H25C 136.4(19) . . ? C25 Th1 C1 80.7(3) . . ? C25A Th1 H25C 15.6(19) . . ? Si1 N1 Th1 109.4(3) . . ? Si1A N1 Th1 105.1(6) . . ? C7 N1 Th1 127.7(6) . . ? C7 N1 Si1 122.2(6) . . ? C7 N1 Si1A 122.9(8) . . ? N1 Si1 C1 99.9(4) . . ? N1 Si1 C2 111.7(5) . . ? N1 Si1 C3 112.6(4) . . ? C1 Si1 C2 112.6(6) . . ? C1 Si1 C3 113.4(4) . . ? C2 Si1 C3 106.7(6) . . ? Th1 C1 H1B 125(3) . . ? Th1 C1 H1A 119(4) . . ? Si1 C1 Th1 85.5(3) . . ? Si1 C1 H1B 117(3) . . ? Si1 C1 H1A 87(3) . . ? Si1 C1 Th2 177.0(5) . . ? H1B C1 H1A 112.6(17) . . ? Th2 C1 Th1 95.6(3) . . ? Th2 C1 H1B 64(3) . . ? Th2 C1 H1A 90(3) . . ? Th1 C1A H1AB 116(3) . . ? Th1 C1A H1AA 116(3) . . ? H1AB C1A H1AA 112.7(17) . . ? Si1A C1A Th1 80.4(10) . . ? Si1A C1A H1AB 110(5) . . ? Si1A C1A H1AA 119(5) . . ? Si1A C1A Th2 176.7(19) . . ? Th2 C1A Th1 96.4(10) . . ? Th2 C1A H1AB 71(4) . . ? Th2 C1A H1AA 63(4) . . ? Si1 C2 H2A 107(9) . . ? Si1 C2 H2B 106(10) . . ? Si1 C2 H2C 105(9) . . ? H2A C2 H2B 120(10) . . ? H2A C2 H2C 108(10) . . ? H2B C2 H2C 110(10) . . ? C4 C3 Si1 109.6(7) . . ? C4 C3 C5 109.3(9) . . ? C4 C3 C6 108.3(10) . . ? C5 C3 Si1 110.9(7) . . ? C6 C3 Si1 110.3(8) . . ? C6 C3 C5 108.4(9) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 Si1A C1A 104.4(13) . . ? N1 Si1A C2A 115(3) . . ? N1 Si1A C3A 105.4(18) . . ? C1A Si1A C2A 112(3) . . ? C3A Si1A C1A 115(2) . . ? C3A Si1A C2A 105(3) . . ? Si1A C2A H2AA 109.5 . . ? Si1A C2A H2AB 109.5 . . ? Si1A C2A H2AC 109.5 . . ? H2AA C2A H2AB 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? C4A C3A Si1A 117(5) . . ? C4A C3A C5A 103(3) . . ? C4A C3A C6A 103(3) . . ? C5A C3A Si1A 107(4) . . ? C5A C3A C6A 103(3) . . ? C6A C3A Si1A 121(5) . . ? C3A C4A H4AA 109.5 . . ? C3A C4A H4AB 109.5 . . ? C3A C4A H4AC 109.5 . . ? H4AA C4A H4AB 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? C3A C5A H5AA 109.5 . . ? C3A C5A H5AB 109.5 . . ? C3A C5A H5AC 109.5 . . ? H5AA C5A H5AB 109.5 . . ? H5AA C5A H5AC 109.5 . . ? H5AB C5A H5AC 109.5 . . ? C3A C6A H6AA 109.5 . . ? C3A C6A H6AB 109.5 . . ? C3A C6A H6AC 109.5 . . ? H6AA C6A H6AB 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? N1 C7 H7A 109.8 . . ? N1 C7 H7B 109.8 . . ? N1 C7 C8 109.3(7) . . ? H7A C7 H7B 108.3 . . ? C8 C7 H7A 109.8 . . ? C8 C7 H7B 109.8 . . ? C7 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N4 C8 C7 110.2(8) . . ? N4 C8 H8A 109.6 . . ? N4 C8 H8B 109.6 . . ? Si2 N2 Th1 139.9(5) . . ? C15 N2 Th1 100.2(6) . . ? C15 N2 Si2 116.6(6) . . ? C15 N2 Si2A 123.5(7) . . ? Si2A N2 Th1 136.1(5) . . ? N2 Si2 C11 112.4(6) . . ? N2 Si2 C9 107.9(8) . . ? N2 Si2 C10 117.6(9) . . ? C9 Si2 C11 102.3(8) . . ? C9 Si2 C10 109.7(11) . . ? C10 Si2 C11 105.9(9) . . ? N2 C15 H15A 109.4 . . ? N2 C15 H15B 109.4 . . ? N2 C15 C16 111.4(9) . . ? H15A C15 H15B 108.0 . . ? C16 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C15 C16 H16A 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? N4 C16 C15 108.7(8) . . ? N4 C16 H16A 109.9 . . ? N4 C16 H16B 109.9 . . ? Si3 N3 Th1 120.3(3) . . ? C23 N3 Th1 121.7(5) . . ? C23 N3 Si3 114.6(6) . . ? N3 Si3 C17 111.7(4) . . ? N3 Si3 C18 106.6(4) . . ? N3 Si3 C19 113.8(4) . . ? C17 Si3 C19 108.6(5) . . ? C18 Si3 C17 107.0(5) . . ? C18 Si3 C19 109.0(4) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Si3 110.9(7) . . ? C21 C19 Si3 110.2(7) . . ? C21 C19 C20 107.8(8) . . ? C21 C19 C22 110.2(9) . . ? C22 C19 Si3 109.6(7) . . ? C22 C19 C20 108.1(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 109.2 . . ? N3 C23 H23B 109.2 . . ? N3 C23 C24 112.0(7) . . ? H23A C23 H23B 107.9 . . ? C24 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C23 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? N4 C24 C23 111.7(7) . . ? N4 C24 H24A 109.3 . . ? N4 C24 H24B 109.3 . . ? C8 N4 Th1 109.0(5) . . ? C8 N4 C16 112.5(8) . . ? C8 N4 C24 112.5(8) . . ? C16 N4 Th1 107.1(6) . . ? C24 N4 Th1 103.7(5) . . ? C24 N4 C16 111.4(8) . . ? C1 Th2 H1B 20.43(15) . . ? C1A Th2 H1AB 21.17(16) . . ? C1A Th2 H1AA 21.1(3) . . ? C1A Th2 N8 141.7(7) . . ? C1A Th2 C25A 88.9(8) . . ? H1AB Th2 H1AA 38.0(7) . . ? N5 Th2 C1 147.0(3) . . ? N5 Th2 H1B 165.0(8) . . ? N5 Th2 C1A 151.7(8) . . ? N5 Th2 H1AB 156.0(7) . . ? N5 Th2 H1AA 151.0(9) . . ? N5 Th2 C25 66.8(3) . . ? N5 Th2 N6 102.5(3) . . ? N5 Th2 N7 98.9(3) . . ? N5 Th2 N8 66.6(3) . . ? N5 Th2 C25A 64.0(4) . . ? C25 Th2 C1 84.0(3) . . ? C25 Th2 H1B 98.2(9) . . ? N6 Th2 C1 102.2(3) . . ? N6 Th2 H1B 83.4(5) . . ? N6 Th2 C1A 91.9(6) . . ? N6 Th2 H1AB 70.7(6) . . ? N6 Th2 H1AA 105.3(9) . . ? N6 Th2 C25 111.3(3) . . ? N6 Th2 N8 68.0(3) . . ? N6 Th2 C25A 105.2(5) . . ? N7 Th2 C1 89.7(3) . . ? N7 Th2 H1B 90.6(11) . . ? N7 Th2 C1A 96.5(7) . . ? N7 Th2 H1AB 104.8(7) . . ? N7 Th2 H1AA 76.2(5) . . ? N7 Th2 C25 133.0(3) . . ? N7 Th2 N6 115.6(3) . . ? N7 Th2 N8 66.7(3) . . ? N7 Th2 C25A 138.6(5) . . ? N8 Th2 C1 144.2(3) . . ? N8 Th2 H1B 128.2(7) . . ? N8 Th2 H1AB 126.9(4) . . ? N8 Th2 H1AA 132.4(5) . . ? N8 Th2 C25 131.8(3) . . ? N8 Th2 C25A 127.0(4) . . ? C25A Th2 H1AB 94.9(6) . . ? C25A Th2 H1AA 100.6(6) . . ? Si4 N5 Th2 104.6(3) . . ? Si4A N5 Th2 107.5(4) . . ? C31 N5 Th2 126.8(6) . . ? C31 N5 Si4 122.9(7) . . ? C31 N5 Si4A 125.1(7) . . ? N5 Si4 C25 96.5(5) . . ? N5 Si4 C26 113.3(6) . . ? N5 Si4 C27 111.5(4) . . ? C26 Si4 C25 115.6(6) . . ? C26 Si4 C27 108.3(6) . . ? C27 Si4 C25 111.2(5) . . ? Th1 C25 H25B 76(5) . . ? Th1 C25 H25A 82(4) . . ? Th2 C25 Th1 98.6(4) . . ? Th2 C25 H25B 128(6) . . ? Th2 C25 H25A 118(4) . . ? Si4 C25 Th1 170.9(6) . . ? Si4 C25 Th2 86.0(5) . . ? Si4 C25 H25B 95(4) . . ? Si4 C25 H25A 103(4) . . ? H25B C25 H25A 112.4(18) . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Si4 109.7(8) . . ? C28 C27 C29 109.1(10) . . ? C29 C27 Si4 108.7(8) . . ? C30 C27 Si4 112.1(8) . . ? C30 C27 C28 108.5(10) . . ? C30 C27 C29 108.7(10) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 Si4A C26A 119.7(15) . . ? N5 Si4A C27A 104.4(10) . . ? N5 Si4A C25A 95.2(12) . . ? C26A Si4A C27A 108.5(15) . . ? C26A Si4A C25A 126.6(16) . . ? C27A Si4A C25A 99.0(12) . . ? Si4A C26A H26D 109.5 . . ? Si4A C26A H26E 109.5 . . ? Si4A C26A H26F 109.5 . . ? H26D C26A H26E 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C28A C27A Si4A 110(2) . . ? C28A C27A C29A 108(3) . . ? C29A C27A Si4A 111(2) . . ? C30A C27A Si4A 110(2) . . ? C30A C27A C28A 109(3) . . ? C30A C27A C29A 109(3) . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28E 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29D 109.5 . . ? C27A C29A H29E 109.5 . . ? C27A C29A H29F 109.5 . . ? H29D C29A H29E 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C27A C30A H30D 109.5 . . ? C27A C30A H30E 109.5 . . ? C27A C30A H30F 109.5 . . ? H30D C30A H30E 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? N5 C31 H31A 109.7 . . ? N5 C31 H31B 109.7 . . ? N5 C31 C32 109.8(9) . . ? H31A C31 H31B 108.2 . . ? C32 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? C31 C32 H32A 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.2 . . ? N8 C32 C31 110.1(8) . . ? N8 C32 H32A 109.6 . . ? N8 C32 H32B 109.6 . . ? Si5 N6 Th2 126.6(4) . . ? C39 N6 Th2 121.8(6) . . ? C39 N6 Si5 111.4(6) . . ? N6 Si5 C33 107.1(4) . . ? N6 Si5 C34 112.3(5) . . ? N6 Si5 C35 113.0(4) . . ? C33 Si5 C34 107.3(5) . . ? C33 Si5 C35 108.4(5) . . ? C34 Si5 C35 108.7(5) . . ? Si5 C33 H33A 109.5 . . ? Si5 C33 H33B 109.5 . . ? Si5 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si5 C34 H34A 109.5 . . ? Si5 C34 H34B 109.5 . . ? Si5 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 Si5 109.5(7) . . ? C36 C35 C38 109.1(10) . . ? C37 C35 Si5 112.3(8) . . ? C37 C35 C36 108.7(9) . . ? C37 C35 C38 108.2(9) . . ? C38 C35 Si5 109.0(7) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N6 C39 H39A 109.3 . . ? N6 C39 H39B 109.3 . . ? N6 C39 C40 111.8(8) . . ? H39A C39 H39B 107.9 . . ? C40 C39 H39A 109.3 . . ? C40 C39 H39B 109.3 . . ? C39 C40 H40A 109.8 . . ? C39 C40 H40B 109.8 . . ? H40A C40 H40B 108.3 . . ? N8 C40 C39 109.2(8) . . ? N8 C40 H40A 109.8 . . ? N8 C40 H40B 109.8 . . ? Si6 N7 Th2 143.1(4) . . ? C47 N7 Th2 97.9(5) . . ? C47 N7 Si6 117.8(6) . . ? N7 Si6 C41 112.3(5) . . ? N7 Si6 C42 107.8(5) . . ? N7 Si6 C43 112.3(5) . . ? C41 Si6 C43 105.9(6) . . ? C42 Si6 C41 108.9(6) . . ? C42 Si6 C43 109.8(6) . . ? Si6 C41 H41A 109.5 . . ? Si6 C41 H41B 109.5 . . ? Si6 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si6 C42 H42A 109.5 . . ? Si6 C42 H42B 109.5 . . ? Si6 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 Si6 110.6(9) . . ? C45 C43 Si6 111.7(10) . . ? C45 C43 C44 110.7(11) . . ? C45 C43 C46 108.1(11) . . ? C46 C43 Si6 109.2(8) . . ? C46 C43 C44 106.3(12) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Th2 C47 H47A 155.4 . . ? Th2 C47 H47B 70.1 . . ? N7 C47 Th2 52.0(4) . . ? N7 C47 H47A 109.6 . . ? N7 C47 H47B 109.6 . . ? N7 C47 C48 110.1(8) . . ? H47A C47 H47B 108.1 . . ? C48 C47 Th2 93.4(5) . . ? C48 C47 H47A 109.6 . . ? C48 C47 H47B 109.6 . . ? C47 C48 H48A 109.9 . . ? C47 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? N8 C48 C47 108.7(7) . . ? N8 C48 H48A 109.9 . . ? N8 C48 H48B 109.9 . . ? C32 N8 Th2 107.4(6) . . ? C32 N8 C40 111.9(8) . . ? C40 N8 Th2 107.8(5) . . ? C48 N8 Th2 105.4(5) . . ? C48 N8 C32 111.2(8) . . ? C48 N8 C40 112.7(8) . . ? N2 Si2A C9A 100.1(12) . . ? N2 Si2A C11A 114.0(8) . . ? N2 Si2A C10A 114.2(11) . . ? C11A Si2A C9A 106.3(15) . . ? C10A Si2A C9A 117.4(16) . . ? C10A Si2A C11A 105.0(13) . . ? Si2A C9A H9AA 109.5 . . ? Si2A C9A H9AB 109.5 . . ? Si2A C9A H9AC 109.5 . . ? H9AA C9A H9AB 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? H14A C14A H14B 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C11A C14A H14A 109.5 . . ? C11A C14A H14B 109.5 . . ? C11A C14A H14C 109.5 . . ? H14D C14 H14E 109.5 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C11 C14 H14D 109.5 . . ? C11 C14 H14E 109.5 . . ? C11 C14 H14F 109.5 . . ? C14 C11 Si2 111.4(13) . . ? C14 C11 C13 107.1(15) . . ? C13 C11 Si2 111.8(13) . . ? C12 C11 Si2 110.1(12) . . ? C12 C11 C14 107.1(16) . . ? C12 C11 C13 109.1(15) . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14A C11A Si2A 109.5(18) . . ? C12A C11A Si2A 105.9(16) . . ? C12A C11A C14A 114(2) . . ? C13A C11A Si2A 114.8(17) . . ? C13A C11A C14A 105(2) . . ? C13A C11A C12A 108(2) . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12E 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C11A C13A H13D 109.5 . . ? C11A C13A H13E 109.5 . . ? C11A C13A H13F 109.5 . . ? H13D C13A H13E 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2A C10A H10A 109.5 . . ? Si2A C10A H10B 109.5 . . ? Si2A C10A H10C 109.5 . . ? H10A C10A H10B 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? Si2 C10 H10D 109.5 . . ? Si2 C10 H10E 109.5 . . ? Si2 C10 H10F 109.5 . . ? H10D C10 H10E 109.5 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? Th1 C25A H25D 109(10) . . ? Th1 C25A H25C 40(8) . . ? Th2 C25A Th1 92.3(9) . . ? Th2 C25A H25D 119(10) . . ? Th2 C25A H25C 120(6) . . ? Si4A C25A Th1 143.6(11) . . ? Si4A C25A Th2 82.6(10) . . ? Si4A C25A H25D 106(10) . . ? Si4A C25A H25C 113(7) . . ? H25D C25A H25C 112.6(18) . . ? 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 _geom_torsion_publ_flag Th1 N1 Si1 C1 11.9(5) . . . . ? Th1 N1 Si1 C2 -107.3(6) . . . . ? Th1 N1 Si1 C3 132.6(4) . . . . ? Th1 N1 Si1A C1A -20.7(13) . . . . ? Th1 N1 Si1A C2A 102(3) . . . . ? Th1 N1 Si1A C3A -141.8(17) . . . . ? Th1 N1 C7 C8 18.7(12) . . . . ? Th1 N2 Si2 C11 -122.5(8) . . . . ? Th1 N2 Si2 C9 -10.4(11) . . . . ? Th1 N2 Si2 C10 114.2(10) . . . . ? Th1 N2 C15 C16 -75.0(8) . . . . ? Th1 N2 Si2A C9A 43.9(15) . . . . ? Th1 N2 Si2A C11A 156.9(9) . . . . ? Th1 N2 Si2A C10A -82.5(15) . . . . ? Th1 N3 Si3 C17 98.4(5) . . . . ? Th1 N3 Si3 C18 -18.1(5) . . . . ? Th1 N3 Si3 C19 -138.3(4) . . . . ? Th1 N3 C23 C24 3.1(10) . . . . ? N1 Si1 C1 Th1 -9.0(4) . . . . ? N1 Si1A C3A C4A 40(3) . . . . ? N1 Si1A C3A C5A 155(3) . . . . ? N1 Si1A C3A C6A -87(4) . . . . ? N1 C7 C8 N4 -43.2(11) . . . . ? Si1 N1 C7 C8 -150.0(7) . . . . ? C1A Si1A C3A C4A -74(4) . . . . ? C1A Si1A C3A C5A 41(4) . . . . ? C1A Si1A C3A C6A 159(3) . . . . ? C2 Si1 C1 Th1 109.6(5) . . . . ? C3 Si1 C1 Th1 -129.1(4) . . . . ? Si1A N1 C7 C8 171.5(10) . . . . ? C2A Si1A C3A C4A 163(4) . . . . ? C2A Si1A C3A C5A -82(4) . . . . ? C2A Si1A C3A C6A 35(5) . . . . ? C7 N1 Si1 C1 -177.6(8) . . . . ? C7 N1 Si1 C2 63.1(10) . . . . ? C7 N1 Si1 C3 -56.9(9) . . . . ? C7 N1 Si1A C1A -178.6(12) . . . . ? C7 N1 Si1A C2A -56(3) . . . . ? C7 N1 Si1A C3A 60(2) . . . . ? C7 C8 N4 Th1 46.2(9) . . . . ? C7 C8 N4 C16 -72.5(10) . . . . ? C7 C8 N4 C24 160.7(7) . . . . ? N2 Si2 C11 C14 65.7(13) . . . . ? N2 Si2 C11 C13 -174.5(11) . . . . ? N2 Si2 C11 C12 -53.0(13) . . . . ? N2 C15 C16 N4 44.3(12) . . . . ? N2 Si2A C11A C14A -56(2) . . . . ? N2 Si2A C11A C12A -179.8(16) . . . . ? N2 Si2A C11A C13A 62(2) . . . . ? Si2 N2 C15 C16 88.6(9) . . . . ? C15 N2 Si2 C11 83.0(9) . . . . ? C15 N2 Si2 C9 -164.9(9) . . . . ? C15 N2 Si2 C10 -40.3(12) . . . . ? C15 N2 Si2A C9A -141.3(14) . . . . ? C15 N2 Si2A C11A -28.4(13) . . . . ? C15 N2 Si2A C10A 92.3(15) . . . . ? C15 C16 N4 Th1 4.6(10) . . . . ? C15 C16 N4 C8 124.4(9) . . . . ? C15 C16 N4 C24 -108.2(9) . . . . ? N3 C23 C24 N4 -40.6(11) . . . . ? Si3 N3 C23 C24 162.3(6) . . . . ? C23 N3 Si3 C17 -61.1(7) . . . . ? C23 N3 Si3 C18 -177.6(6) . . . . ? C23 N3 Si3 C19 62.2(7) . . . . ? C23 C24 N4 Th1 52.1(8) . . . . ? C23 C24 N4 C8 -65.6(10) . . . . ? C23 C24 N4 C16 167.0(8) . . . . ? Th2 N5 Si4 C25 -23.0(5) . . . . ? Th2 N5 Si4 C26 98.6(6) . . . . ? Th2 N5 Si4 C27 -138.9(4) . . . . ? Th2 N5 Si4A C26A -106.3(15) . . . . ? Th2 N5 Si4A C27A 132.2(9) . . . . ? Th2 N5 Si4A C25A 31.5(9) . . . . ? Th2 N5 C31 C32 19.1(14) . . . . ? Th2 N6 Si5 C33 3.6(6) . . . . ? Th2 N6 Si5 C34 -113.8(6) . . . . ? Th2 N6 Si5 C35 122.9(5) . . . . ? Th2 N6 C39 C40 31.8(11) . . . . ? Th2 N7 Si6 C41 129.5(8) . . . . ? Th2 N7 Si6 C42 9.6(9) . . . . ? Th2 N7 Si6 C43 -111.4(8) . . . . ? Th2 N7 C47 C48 -78.1(7) . . . . ? Th2 C47 C48 N8 -4.6(8) . . . . ? N5 C31 C32 N8 -44.4(14) . . . . ? Si4 N5 C31 C32 168.5(8) . . . . ? Si4A N5 C31 C32 -150.8(9) . . . . ? C31 N5 Si4 C25 -178.1(9) . . . . ? C31 N5 Si4 C26 -56.5(10) . . . . ? C31 N5 Si4 C27 66.0(10) . . . . ? C31 N5 Si4A C26A 65.3(18) . . . . ? C31 N5 Si4A C27A -56.2(14) . . . . ? C31 N5 Si4A C25A -156.9(12) . . . . ? C31 C32 N8 Th2 46.5(10) . . . . ? C31 C32 N8 C40 -71.7(11) . . . . ? C31 C32 N8 C48 161.3(9) . . . . ? N6 C39 C40 N8 -51.3(11) . . . . ? Si5 N6 C39 C40 -143.7(8) . . . . ? C39 N6 Si5 C33 179.0(7) . . . . ? C39 N6 Si5 C34 61.5(8) . . . . ? C39 N6 Si5 C35 -61.8(8) . . . . ? C39 C40 N8 Th2 44.8(9) . . . . ? C39 C40 N8 C32 162.8(8) . . . . ? C39 C40 N8 C48 -71.1(10) . . . . ? N7 Si6 C43 C44 -50.1(9) . . . . ? N7 Si6 C43 C45 -173.9(8) . . . . ? N7 Si6 C43 C46 66.5(10) . . . . ? N7 C47 C48 N8 46.1(10) . . . . ? Si6 N7 C47 Th2 170.4(8) . . . . ? Si6 N7 C47 C48 92.2(9) . . . . ? C41 Si6 C43 C44 72.7(10) . . . . ? C41 Si6 C43 C45 -51.1(11) . . . . ? C41 Si6 C43 C46 -170.7(9) . . . . ? C42 Si6 C43 C44 -170.0(8) . . . . ? C42 Si6 C43 C45 66.3(10) . . . . ? C42 Si6 C43 C46 -53.3(10) . . . . ? C47 N7 Si6 C41 -34.5(10) . . . . ? C47 N7 Si6 C42 -154.4(8) . . . . ? C47 N7 Si6 C43 84.6(8) . . . . ? C47 C48 N8 Th2 5.2(9) . . . . ? C47 C48 N8 C32 -111.0(9) . . . . ? C47 C48 N8 C40 122.5(9) . . . . ? Si2A N2 C15 C16 108.7(10) . . . . ? C9A Si2A C11A C14A 53(2) . . . . ? C9A Si2A C11A C12A -71(2) . . . . ? C9A Si2A C11A C13A 171(2) . . . . ? C9 Si2 C11 C14 -49.7(14) . . . . ? C9 Si2 C11 C13 70.1(14) . . . . ? C9 Si2 C11 C12 -168.4(13) . . . . ? C10A Si2A C11A C14A 178(2) . . . . ? C10A Si2A C11A C12A 55(2) . . . . ? C10A Si2A C11A C13A -64(2) . . . . ? C10 Si2 C11 C14 -164.6(14) . . . . ? C10 Si2 C11 C13 -44.8(15) . . . . ? C10 Si2 C11 C12 76.7(14) . . . . ? _shelx_SHELXL_version_number '2014/7' 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 3 12 5 0.1135 3.0197 12.0203 5.0136 -0.7726 0.5259 -0.2960 4 -10 8 0.1623 3.9674 -9.9589 7.9973 -0.0607 0.0685 1.0141 -5 -10 -7 0.1115 -5.0116 -10.0347 -7.0140 0.8038 -0.6563 0.0265 -5 5 -10 0.1833 -4.9760 4.9518 -10.0028 0.3787 -0.2633 -0.8769 -8 -1 8 0.1068 -8.0003 -1.0145 7.9969 -0.4741 -0.9361 0.0411 5 5 10 0.1235 4.9982 5.0441 10.0110 -0.7824 0.5002 0.3559 -3 12 -5 0.1357 -2.9664 11.9698 -4.9939 -0.1962 0.0427 -0.9544 -2 -14 2 0.0951 -2.0306 -13.9979 1.9879 0.4366 -0.5597 0.7267 8 -1 -7 0.0955 7.9951 -0.9822 -6.9982 0.4947 0.8762 0.1037 3 13 -2 0.1331 3.0274 13.0027 -1.9881 -0.3920 0.6375 -0.6325 7 10 2 0.1291 7.0135 10.0310 2.0135 -0.4948 0.9221 -0.1457 -4 12 2 0.1368 -3.9708 11.9827 2.0080 -0.6214 -0.1468 -0.7120 -3 -10 -8 0.0904 -3.0129 -10.0285 -8.0131 0.8723 -0.4408 0.0699 7 -6 5 0.1557 6.9756 -5.9550 5.0015 -0.0293 0.5054 0.8099 -5 1 11 0.1376 -5.0013 1.0050 11.0016 -0.7227 -0.6220 0.1849 3 -13 -2 0.1137 2.9696 -12.9866 -2.0094 0.6576 0.0217 0.7220 _olex2_submission_original_sample_id THBGLS _olex2_submission_special_instructions 'No special instructions were received' data_5 _nottingham_internal_coll_name UBMGMW _nottingham_internal_coll_number 11948 _nottingham_internal_coll_client BMG/STL _nottingham_internal_coll_type hemisphere _nottingham_internal_coll_frame_method \w _nottingham_internal_coll_frame_time 60 _nottingham_internal_coll_frame_width 0.3 _nottingham_internal_coll_user BMG _nottingham_internal_coll_date 26/10/2012 _nottingham_internal_coll_location NOTTS _nottingham_internal_NCS_number ? _nottingham_internal_process_date 26/10/2012 _nottingham_internal_process_user BMG/WL _nottingham_internal_solution_date 26/10/2012 _nottingham_internal_solution_user BMG/WL _nottingham_internal_refinement_date 10/11/2014 _nottingham_internal_refinement_user BMG/WL _nottingham_internal_validation_date 14/11/2014 _nottingham_internal_validation_user pczwl _nottingham_internal_archive_date 14/11/2014 _refine_special_details ; Disordered lattice solvent molecules could not be refined as sensible chemical entites, and so were removed with PLATON SQUEEZE. The removed electron density equated to 8 toluene molecules per unit cell (the solvent used for crystallisation), or one molecule of toluene per moiety. These toluene molecules were included in the formula, and in the calculation of dervied parameters (Mr, F000 etc). T-butyl group C19-C22 is disordered over two orientaions. The occupancies of the two components were refined competitvely, converging at a ratio of 0.838:0.162. Chemically equivalent 1,2- C-C and C-Si distances of the disordered atoms were restrained to be approximately equal. Anti-bumping restraints were applied to the hydrogen atoms of C18 and minor component atom C21, to prevent to poorly located minor component hydrogen atoms approaching too close to those of C18. Enhanced rigid bond restraints were applied to the whole structure. ; _vrf_CHEMW03_5 ; PROBLEM: WARNING: The ratio of given/expected molecular weight as RESPONSE: PLATON SQUEEZE has been employed; the removed solvent has been included in the formula, and calculation of derived parameters. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.912 0.250 373 95 '2(C7 H8)' 2 1.000 0.412 0.250 373 95 '2(C7 H8)' 3 0.500 0.087 0.750 373 96 '2(C7 H8)' 4 1.000 0.587 0.750 373 96 '2(C7 H8)' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ? _audit_creation_date 2014-11-14 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C28 H63 N6 Si3 U, C24 H20 B, C7 H8' _chemical_formula_sum 'C59 H91 B N6 Si3 U' _chemical_formula_weight 1217.48 _chemical_melting_point ? 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.557(8) _cell_length_b 25.947(8) _cell_length_c 21.479(6) _cell_angle_alpha 90 _cell_angle_beta 128.242(5) _cell_angle_gamma 90 _cell_volume 12062(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7063 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 27.43 _cell_measurement_theta_min 2.16 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.792 _exptl_absorpt_correction_T_max 0.4305 _exptl_absorpt_correction_T_min 0.3526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2007/2 (Bruker,2007) was used for absorption correction. wR2(int) was 0.0702 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.8190. The \l/2 correction factor is 0.0015. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 5008 _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_unetI/netI 0.0800 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 37344 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.548 _diffrn_reflns_theta_min 1.980 _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 8.366 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_standards_number . _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 10555 _reflns_number_total 13761 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _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 ? _refine_diff_density_max 2.052 _refine_diff_density_min -1.302 _refine_diff_density_rms 0.133 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 625 _refine_ls_number_reflns 13761 _refine_ls_number_restraints 602 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0753 _refine_ls_restrained_S_all 1.163 _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^)+(0.0555P)^2^+46.6730P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1567 _refine_ls_wR_factor_ref 0.1675 _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 H21A-H18B -2 with sigma of 0.02 H21B-H18B -2 with sigma of 0.02 Si3-C19A \\sim Si3-C19 with sigma of 0.02 C19-C21 \\sim C19-C21A \\sim C20-C19 \\sim C20A-C19 \\sim C19-C22 \\sim C19-C22A with sigma of 0.02 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(C19A)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=Sof(H21D)= Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1) Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)= Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,H24B) 5.b Aromatic/amide H refined with riding coordinates: C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52) 5.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A, H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A, H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F), C21(H21A,H21B,H21C), C21A(H21D,H21E, H21F), C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 U1 U 0.26022(2) 0.34150(2) 0.29641(2) 0.03649(10) Uani 1 1 d . . . . . N1 N 0.2857(3) 0.2596(2) 0.3057(4) 0.0397(14) Uani 1 1 d . . . . . Si1 Si 0.35151(12) 0.22706(9) 0.38175(14) 0.0434(5) Uani 1 1 d . . . . . C1 C 0.3942(4) 0.2706(4) 0.4696(5) 0.056(2) Uani 1 1 d . . . . . H1A H 0.3969 0.3051 0.4533 0.085 Uiso 1 1 calc GR . . . . H1B H 0.4359 0.2571 0.5096 0.085 Uiso 1 1 calc GR . . . . H1C H 0.3722 0.2725 0.4919 0.085 Uiso 1 1 calc GR . . . . C2 C 0.3305(5) 0.1674(3) 0.4101(6) 0.064(3) Uani 1 1 d . . . . . H2A H 0.3110 0.1773 0.4340 0.096 Uiso 1 1 calc GR . . . . H2B H 0.3679 0.1474 0.4483 0.096 Uiso 1 1 calc GR . . . . H2C H 0.3016 0.1465 0.3627 0.096 Uiso 1 1 calc GR . . . . C3 C 0.4040(4) 0.2089(3) 0.3566(5) 0.0464(18) Uani 1 1 d . . . . . C4 C 0.4273(4) 0.2582(3) 0.3431(5) 0.052(2) Uani 1 1 d . . . . . H4A H 0.3922 0.2771 0.2978 0.078 Uiso 1 1 calc GR . . . . H4B H 0.4560 0.2490 0.3325 0.078 Uiso 1 1 calc GR . . . . H4C H 0.4486 0.2799 0.3906 0.078 Uiso 1 1 calc GR . . . . C5 C 0.4613(5) 0.1794(4) 0.4267(6) 0.065(3) Uani 1 1 d . . . . . H5A H 0.4826 0.2006 0.4748 0.098 Uiso 1 1 calc GR . . . . H5B H 0.4894 0.1721 0.4145 0.098 Uiso 1 1 calc GR . . . . H5C H 0.4480 0.1470 0.4353 0.098 Uiso 1 1 calc GR . . . . C6 C 0.3710(5) 0.1758(4) 0.2827(6) 0.057(2) Uani 1 1 d . . . . . H6A H 0.3533 0.1455 0.2894 0.086 Uiso 1 1 calc GR . . . . H6B H 0.4004 0.1646 0.2742 0.086 Uiso 1 1 calc GR . . . . H6C H 0.3378 0.1958 0.2369 0.086 Uiso 1 1 calc GR . . . . C7 C 0.2335(4) 0.2278(3) 0.2415(5) 0.0466(19) Uani 1 1 d . . . . . H7A H 0.2474 0.1920 0.2449 0.056 Uiso 1 1 calc R . . . . H7B H 0.2172 0.2421 0.1891 0.056 Uiso 1 1 calc R . . . . C8 C 0.1842(4) 0.2285(3) 0.2513(5) 0.0488(19) Uani 1 1 d . . . . . H8A H 0.1469 0.2105 0.2063 0.059 Uiso 1 1 calc R . . . . H8B H 0.1990 0.2105 0.3008 0.059 Uiso 1 1 calc R . . . . N2 N 0.2521(3) 0.3440(2) 0.3935(4) 0.0416(15) Uani 1 1 d . . . . . Si2 Si 0.26262(12) 0.39690(9) 0.44999(13) 0.0443(5) Uani 1 1 d . . . . . C9 C 0.2810(4) 0.4540(3) 0.4150(5) 0.048(2) Uani 1 1 d . . . . . H9A H 0.3226 0.4502 0.4306 0.072 Uiso 1 1 calc GR . . . . H9B H 0.2792 0.4854 0.4390 0.072 Uiso 1 1 calc GR . . . . H9C H 0.2509 0.4565 0.3572 0.072 Uiso 1 1 calc GR . . . . C10 C 0.1902(5) 0.4122(4) 0.4355(6) 0.059(2) Uani 1 1 d . . . . . H10A H 0.1565 0.4174 0.3789 0.089 Uiso 1 1 calc GR . . . . H10B H 0.1962 0.4437 0.4647 0.089 Uiso 1 1 calc GR . . . . H10C H 0.1800 0.3836 0.4553 0.089 Uiso 1 1 calc GR . . . . C11 C 0.3286(4) 0.3885(3) 0.5606(5) 0.0481(19) Uani 1 1 d . . . . . C12 C 0.3270(6) 0.4315(4) 0.6077(6) 0.073(3) Uani 1 1 d . . . . . H12A H 0.3324 0.4649 0.5912 0.109 Uiso 1 1 calc GR . . . . H12B H 0.3605 0.4264 0.6644 0.109 Uiso 1 1 calc GR . . . . H12C H 0.2872 0.4310 0.5978 0.109 Uiso 1 1 calc GR . . . . C13 C 0.3234(5) 0.3365(3) 0.5898(5) 0.054(2) Uani 1 1 d . . . . . H13A H 0.2824 0.3335 0.5764 0.081 Uiso 1 1 calc GR . . . . H13B H 0.3552 0.3342 0.6474 0.081 Uiso 1 1 calc GR . . . . H13C H 0.3292 0.3086 0.5643 0.081 Uiso 1 1 calc GR . . . . C14 C 0.3910(4) 0.3913(3) 0.5766(5) 0.057(2) Uani 1 1 d . . . . . H14A H 0.3917 0.3661 0.5431 0.085 Uiso 1 1 calc GR . . . . H14B H 0.4242 0.3835 0.6325 0.085 Uiso 1 1 calc GR . . . . H14C H 0.3969 0.4260 0.5644 0.085 Uiso 1 1 calc GR . . . . C15 C 0.2199(4) 0.2986(3) 0.3956(4) 0.047(2) Uani 1 1 d . . . . . H15A H 0.2125 0.3046 0.4347 0.056 Uiso 1 1 calc R . . . . H15B H 0.2459 0.2675 0.4118 0.056 Uiso 1 1 calc R . . . . C16 C 0.1586(4) 0.2906(3) 0.3137(5) 0.0460(19) Uani 1 1 d . . . . . H16A H 0.1373 0.2601 0.3143 0.055 Uiso 1 1 calc R . . . . H16B H 0.1318 0.3211 0.2989 0.055 Uiso 1 1 calc R . . . . N3 N 0.1721(3) 0.3800(3) 0.2008(4) 0.0471(16) Uani 1 1 d . . . . . Si3 Si 0.16751(15) 0.43642(10) 0.15438(15) 0.0584(7) Uani 1 1 d . . . . . C17 C 0.2480(5) 0.4592(3) 0.2075(6) 0.071(3) Uani 1 1 d . . . . . H17A H 0.2638 0.4728 0.2594 0.106 Uiso 1 1 calc GR . . . . H17B H 0.2489 0.4863 0.1765 0.106 Uiso 1 1 calc GR . . . . H17C H 0.2740 0.4303 0.2146 0.106 Uiso 1 1 calc GR . . . . C18 C 0.1346(5) 0.4211(4) 0.0478(5) 0.066(3) Uani 1 1 d . . . . . H18A H 0.1643 0.4003 0.0480 0.099 Uiso 1 1 calc GR . . . . H18B H 0.1266 0.4533 0.0190 0.099 Uiso 1 1 calc DGR . . . . H18C H 0.0959 0.4019 0.0217 0.099 Uiso 1 1 calc GR . . . . C19 C 0.1156(8) 0.4869(8) 0.1495(9) 0.086(9) Uani 0.16(2) 1 d . . P A 1 C19A C 0.1184(7) 0.4889(5) 0.1522(8) 0.086(4) Uani 0.84(2) 1 d . . P A 2 C20 C 0.128(5) 0.482(4) 0.231(3) 0.085(14) Uani 0.16(2) 1 d . . P A 1 H20A H 0.0955 0.5004 0.2279 0.127 Uiso 0.16(2) 1 calc GR . P A 1 H20B H 0.1682 0.4970 0.2726 0.127 Uiso 0.16(2) 1 calc GR . P A 1 H20C H 0.1275 0.4455 0.2422 0.127 Uiso 0.16(2) 1 calc GR . P A 1 C20A C 0.1420(10) 0.5046(6) 0.2340(8) 0.099(6) Uani 0.84(2) 1 d . . P A 2 H20D H 0.1363 0.4762 0.2588 0.148 Uiso 0.84(2) 1 calc GR . P A 2 H20E H 0.1192 0.5349 0.2304 0.148 Uiso 0.84(2) 1 calc GR . P A 2 H20F H 0.1861 0.5131 0.2660 0.148 Uiso 0.84(2) 1 calc GR . P A 2 C21 C 0.061(3) 0.483(3) 0.0588(19) 0.092(14) Uani 0.16(2) 1 d . . P A 1 H21A H 0.0509 0.4467 0.0437 0.138 Uiso 0.16(2) 1 calc DGR . P A 1 H21B H 0.0733 0.4990 0.0290 0.138 Uiso 0.16(2) 1 calc DGR . P A 1 H21C H 0.0249 0.5010 0.0469 0.138 Uiso 0.16(2) 1 calc GR . P A 1 C21A C 0.0471(6) 0.4705(5) 0.1003(8) 0.081(4) Uani 0.84(2) 1 d . . P A 2 H21D H 0.0335 0.4570 0.0492 0.122 Uiso 0.84(2) 1 calc GR . P A 2 H21E H 0.0211 0.4999 0.0914 0.122 Uiso 0.84(2) 1 calc GR . P A 2 H21F H 0.0433 0.4434 0.1290 0.122 Uiso 0.84(2) 1 calc GR . P A 2 C22 C 0.153(4) 0.534(2) 0.156(6) 0.095(12) Uani 0.16(2) 1 d . . P A 1 H22A H 0.1947 0.5337 0.2075 0.143 Uiso 0.16(2) 1 calc GR . P A 1 H22B H 0.1321 0.5661 0.1511 0.143 Uiso 0.16(2) 1 calc GR . P A 1 H22C H 0.1571 0.5328 0.1135 0.143 Uiso 0.16(2) 1 calc GR . P A 1 C22A C 0.1194(10) 0.5364(5) 0.1123(10) 0.101(5) Uani 0.84(2) 1 d . . P A 2 H22D H 0.1615 0.5503 0.1440 0.152 Uiso 0.84(2) 1 calc GR . P A 2 H22E H 0.0915 0.5625 0.1075 0.152 Uiso 0.84(2) 1 calc GR . P A 2 H22F H 0.1059 0.5273 0.0594 0.152 Uiso 0.84(2) 1 calc GR . P A 2 C23 C 0.1111(4) 0.3578(4) 0.1688(6) 0.059(2) Uani 1 1 d . . . . . H23A H 0.0799 0.3685 0.1129 0.071 Uiso 1 1 calc R . . . . H23B H 0.0979 0.3708 0.1996 0.071 Uiso 1 1 calc R . . . . C24 C 0.1154(4) 0.2987(4) 0.1738(5) 0.054(2) Uani 1 1 d . . . . . H24A H 0.0771 0.2842 0.1615 0.065 Uiso 1 1 calc R . . . . H24B H 0.1198 0.2852 0.1345 0.065 Uiso 1 1 calc R . . . . N4 N 0.1691(3) 0.2829(3) 0.2543(4) 0.0449(15) Uani 1 1 d . . . . . N5 N 0.3627(3) 0.3892(2) 0.3717(4) 0.0413(15) Uani 1 1 d . . . . . C25 C 0.4035(4) 0.4167(3) 0.4086(4) 0.0361(16) Uani 1 1 d . . . . . C26 C 0.4535(3) 0.4522(3) 0.4565(4) 0.0362(17) Uani 1 1 d . . . . . H26A H 0.4709 0.4612 0.4296 0.054 Uiso 1 1 calc GR . . . . H26B H 0.4855 0.4363 0.5078 0.054 Uiso 1 1 calc GR . . . . H26C H 0.4382 0.4834 0.4648 0.054 Uiso 1 1 calc GR . . . . N6 N 0.2749(3) 0.3336(3) 0.1863(4) 0.0448(16) Uani 1 1 d . . . . . C27 C 0.2743(3) 0.3192(3) 0.1355(5) 0.0388(17) Uani 1 1 d . . . . . C28 C 0.2725(4) 0.2986(3) 0.0718(5) 0.049(2) Uani 1 1 d . . . . . H28A H 0.2518 0.3231 0.0276 0.073 Uiso 1 1 calc GR . . . . H28B H 0.2498 0.2659 0.0538 0.073 Uiso 1 1 calc GR . . . . H28C H 0.3148 0.2926 0.0906 0.073 Uiso 1 1 calc GR . . . . B1 B 0.3984(4) 0.6268(3) 0.5277(5) 0.0311(15) Uani 1 1 d . . . . . C29 C 0.4037(3) 0.6222(3) 0.4561(4) 0.0308(14) Uani 1 1 d . . . . . C30 C 0.3722(4) 0.5849(3) 0.3960(4) 0.0373(16) Uani 1 1 d . . . . . H30 H 0.3432 0.5632 0.3934 0.045 Uiso 1 1 calc R . . . . C31 C 0.3819(4) 0.5784(3) 0.3399(4) 0.0407(17) Uani 1 1 d . . . . . H31 H 0.3600 0.5524 0.3005 0.049 Uiso 1 1 calc R . . . . C32 C 0.4234(4) 0.6098(3) 0.3412(4) 0.0371(16) Uani 1 1 d . . . . . H32 H 0.4298 0.6058 0.3028 0.045 Uiso 1 1 calc R . . . . C33 C 0.4549(3) 0.6467(3) 0.3993(4) 0.0359(16) Uani 1 1 d . . . . . H33 H 0.4833 0.6687 0.4010 0.043 Uiso 1 1 calc R . . . . C34 C 0.4456(3) 0.6520(3) 0.4556(4) 0.0336(15) Uani 1 1 d . . . . . H34 H 0.4689 0.6773 0.4958 0.040 Uiso 1 1 calc R . . . . C35 C 0.4028(3) 0.6875(3) 0.5553(4) 0.0344(15) Uani 1 1 d . . . . . C36 C 0.3812(4) 0.7277(3) 0.5015(5) 0.0445(19) Uani 1 1 d . . . . . H36 H 0.3664 0.7199 0.4492 0.053 Uiso 1 1 calc R . . . . C37 C 0.3801(4) 0.7785(3) 0.5199(6) 0.056(2) Uani 1 1 d . . . . . H37 H 0.3653 0.8048 0.4814 0.067 Uiso 1 1 calc R . . . . C38 C 0.4008(4) 0.7900(4) 0.5956(6) 0.059(2) Uani 1 1 d . . . . . H38 H 0.4000 0.8247 0.6091 0.070 Uiso 1 1 calc R . . . . C39 C 0.4225(4) 0.7522(3) 0.6511(5) 0.051(2) Uani 1 1 d . . . . . H39 H 0.4370 0.7603 0.7032 0.062 Uiso 1 1 calc R . . . . C40 C 0.4230(4) 0.7015(3) 0.6303(5) 0.0451(19) Uani 1 1 d . . . . . H40 H 0.4379 0.6754 0.6692 0.054 Uiso 1 1 calc R . . . . C41 C 0.4557(3) 0.5925(3) 0.6004(4) 0.0332(15) Uani 1 1 d . . . . . C42 C 0.5145(3) 0.6130(3) 0.6591(4) 0.0361(16) Uani 1 1 d . . . . . H42 H 0.5204 0.6491 0.6591 0.043 Uiso 1 1 calc R . . . . C43 C 0.5642(3) 0.5833(3) 0.7169(4) 0.0358(16) Uani 1 1 d . . . . . H43 H 0.6031 0.5992 0.7554 0.043 Uiso 1 1 calc R . . . . C44 C 0.5577(4) 0.5307(3) 0.7191(4) 0.0370(16) Uani 1 1 d . . . . . H44 H 0.5918 0.5103 0.7592 0.044 Uiso 1 1 calc R . . . . C45 C 0.5016(4) 0.5083(3) 0.6627(4) 0.0373(16) Uani 1 1 d . . . . . H45 H 0.4968 0.4721 0.6632 0.045 Uiso 1 1 calc R . . . . C46 C 0.4516(3) 0.5386(3) 0.6044(4) 0.0339(15) Uani 1 1 d . . . . . H46 H 0.4131 0.5223 0.5659 0.041 Uiso 1 1 calc R . . . . C47 C 0.3317(3) 0.6064(3) 0.5019(4) 0.0352(15) Uani 1 1 d . . . . . C48 C 0.2767(3) 0.6178(3) 0.4270(4) 0.0383(17) Uani 1 1 d . . . . . H48 H 0.2785 0.6357 0.3900 0.046 Uiso 1 1 calc R . . . . C49 C 0.2197(4) 0.6036(3) 0.4052(5) 0.0456(19) Uani 1 1 d . . . . . H49 H 0.1834 0.6112 0.3532 0.055 Uiso 1 1 calc R . . . . C50 C 0.2147(4) 0.5787(3) 0.4577(5) 0.0463(19) Uani 1 1 d . . . . . H50 H 0.1754 0.5690 0.4424 0.056 Uiso 1 1 calc R . . . . C51 C 0.2680(4) 0.5682(3) 0.5331(5) 0.0435(18) Uani 1 1 d . . . . . H51 H 0.2657 0.5517 0.5707 0.052 Uiso 1 1 calc R . . . . C52 C 0.3250(4) 0.5820(3) 0.5536(4) 0.0371(16) Uani 1 1 d . . . . . H52 H 0.3611 0.5742 0.6056 0.045 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.04113(17) 0.03428(15) 0.03414(15) -0.00564(12) 0.02333(13) -0.01042(13) N1 0.040(3) 0.036(3) 0.040(3) -0.010(2) 0.024(3) -0.016(2) Si1 0.0488(14) 0.0391(12) 0.0457(12) 0.0015(10) 0.0310(11) -0.0037(10) C1 0.055(6) 0.062(5) 0.044(4) -0.004(4) 0.027(4) 0.002(4) C2 0.067(6) 0.048(5) 0.079(6) 0.022(4) 0.046(6) 0.006(4) C3 0.047(4) 0.045(4) 0.050(4) -0.002(3) 0.032(4) -0.005(3) C4 0.049(5) 0.058(5) 0.053(5) -0.004(4) 0.034(4) -0.011(4) C5 0.056(5) 0.066(6) 0.076(6) 0.011(5) 0.041(5) 0.006(4) C6 0.057(6) 0.057(5) 0.066(5) -0.008(4) 0.042(5) -0.006(4) C7 0.048(4) 0.035(4) 0.051(4) -0.012(3) 0.028(4) -0.015(3) C8 0.046(4) 0.054(4) 0.040(4) -0.015(3) 0.023(4) -0.022(3) N2 0.045(4) 0.044(3) 0.035(3) -0.004(3) 0.024(3) -0.011(3) Si2 0.0526(15) 0.0465(13) 0.0358(11) -0.0034(9) 0.0284(11) -0.0091(10) C9 0.055(5) 0.045(4) 0.041(4) -0.008(3) 0.028(4) -0.003(4) C10 0.061(5) 0.059(6) 0.056(5) -0.002(4) 0.035(5) -0.001(4) C11 0.057(5) 0.040(4) 0.039(4) -0.008(3) 0.025(3) -0.012(3) C12 0.115(9) 0.049(5) 0.051(5) -0.003(4) 0.050(6) 0.001(5) C13 0.064(6) 0.050(4) 0.045(4) 0.002(4) 0.032(4) -0.013(4) C14 0.056(5) 0.051(5) 0.046(5) 0.003(4) 0.023(4) -0.015(4) C15 0.052(5) 0.052(4) 0.033(4) -0.006(3) 0.025(3) -0.017(4) C16 0.046(4) 0.054(5) 0.039(4) -0.004(3) 0.027(3) -0.009(3) N3 0.051(4) 0.052(4) 0.045(3) 0.001(3) 0.033(3) -0.002(3) Si3 0.078(2) 0.0455(14) 0.0428(13) 0.0043(11) 0.0329(14) 0.0040(12) C17 0.098(6) 0.026(4) 0.079(6) 0.003(4) 0.051(5) -0.004(4) C18 0.097(8) 0.051(5) 0.050(4) 0.003(4) 0.045(5) -0.005(5) C19 0.103(14) 0.067(13) 0.073(15) 0.002(10) 0.047(12) 0.019(11) C19A 0.109(8) 0.058(6) 0.060(6) 0.000(5) 0.038(6) 0.026(5) C20 0.09(3) 0.08(3) 0.071(17) -0.001(15) 0.041(19) 0.02(2) C20A 0.118(12) 0.075(10) 0.062(6) -0.009(6) 0.034(7) 0.051(9) C21 0.106(16) 0.06(2) 0.078(15) 0.006(12) 0.043(13) 0.023(15) C21A 0.097(7) 0.081(8) 0.051(7) 0.000(6) 0.039(6) 0.035(6) C22 0.11(2) 0.070(14) 0.09(2) 0.002(13) 0.053(19) 0.016(14) C22A 0.131(13) 0.059(7) 0.085(9) 0.004(6) 0.052(9) 0.032(7) C23 0.047(5) 0.078(5) 0.049(5) 0.006(4) 0.027(4) 0.004(4) C24 0.040(4) 0.075(5) 0.043(4) -0.004(3) 0.023(3) -0.010(3) N4 0.040(3) 0.054(3) 0.039(3) -0.008(3) 0.024(3) -0.017(3) N5 0.044(4) 0.043(3) 0.038(3) -0.008(3) 0.026(3) -0.010(3) C25 0.038(4) 0.037(4) 0.030(3) -0.002(3) 0.020(3) -0.004(3) C26 0.034(4) 0.035(4) 0.033(4) -0.004(3) 0.017(3) -0.006(3) N6 0.043(4) 0.050(4) 0.039(3) -0.007(3) 0.025(3) -0.008(3) C27 0.030(4) 0.048(4) 0.037(3) -0.001(3) 0.020(3) -0.003(3) C28 0.047(5) 0.060(5) 0.047(4) -0.011(4) 0.033(4) -0.005(4) B1 0.029(3) 0.033(3) 0.027(3) 0.000(3) 0.015(3) 0.001(3) C29 0.026(3) 0.031(3) 0.026(3) 0.006(2) 0.011(3) 0.009(2) C30 0.043(4) 0.035(4) 0.033(3) 0.002(3) 0.023(3) 0.002(3) C31 0.044(4) 0.041(4) 0.037(4) 0.001(3) 0.025(3) 0.004(3) C32 0.036(4) 0.041(4) 0.034(3) 0.007(3) 0.022(3) 0.012(3) C33 0.032(4) 0.040(4) 0.033(3) 0.012(3) 0.019(3) 0.010(3) C34 0.032(4) 0.032(3) 0.033(3) 0.006(3) 0.017(3) 0.006(3) C35 0.024(4) 0.040(3) 0.037(3) -0.004(3) 0.018(3) 0.002(3) C36 0.045(5) 0.043(4) 0.042(4) 0.003(3) 0.026(4) 0.011(3) C37 0.047(5) 0.042(4) 0.064(5) -0.001(3) 0.028(4) 0.012(3) C38 0.045(5) 0.051(5) 0.069(5) -0.012(4) 0.030(4) 0.005(4) C39 0.034(4) 0.058(4) 0.055(4) -0.023(3) 0.024(4) -0.003(3) C40 0.044(5) 0.051(4) 0.039(4) -0.007(3) 0.025(4) 0.002(3) C41 0.030(3) 0.041(3) 0.029(3) -0.001(2) 0.018(3) 0.006(2) C42 0.031(3) 0.045(4) 0.029(3) 0.000(3) 0.016(3) -0.001(3) C43 0.030(4) 0.044(4) 0.028(3) -0.003(3) 0.015(3) -0.001(3) C44 0.038(4) 0.039(4) 0.030(3) 0.004(3) 0.019(3) 0.005(3) C45 0.040(4) 0.032(3) 0.038(3) 0.007(3) 0.023(3) 0.003(3) C46 0.028(3) 0.039(3) 0.033(3) -0.001(3) 0.018(3) 0.000(3) C47 0.029(3) 0.040(4) 0.034(3) 0.001(3) 0.018(3) 0.002(3) C48 0.031(3) 0.046(4) 0.036(3) 0.002(3) 0.019(3) 0.004(3) C49 0.032(4) 0.058(5) 0.039(4) 0.003(3) 0.018(3) 0.002(3) C50 0.034(4) 0.052(5) 0.049(4) -0.001(3) 0.024(3) -0.003(3) C51 0.045(4) 0.045(4) 0.045(4) 0.001(3) 0.030(3) 0.000(3) C52 0.035(4) 0.041(4) 0.036(3) 0.003(3) 0.022(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N1 2.209(6) . ? U1 N2 2.232(7) . ? U1 N3 2.222(7) . ? U1 N4 2.573(6) . ? U1 N5 2.544(7) . ? U1 N6 2.644(7) . ? N1 Si1 1.732(7) . ? N1 C7 1.482(9) . ? Si1 C1 1.863(9) . ? Si1 C2 1.880(9) . ? Si1 C3 1.891(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.536(11) . ? C3 C5 1.550(13) . ? C3 C6 1.516(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.496(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 N4 1.485(11) . ? N2 Si2 1.733(7) . ? N2 C15 1.491(10) . ? Si2 C9 1.868(9) . ? Si2 C10 1.861(10) . ? Si2 C11 1.910(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.526(12) . ? C11 C13 1.533(11) . ? C11 C14 1.530(13) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.520(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N4 1.485(10) . ? N3 Si3 1.731(7) . ? N3 C23 1.485(11) . ? Si3 C17 1.855(11) . ? Si3 C18 1.910(9) . ? Si3 C19 1.89(2) . ? Si3 C19A 1.899(12) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.562(19) . ? C19 C21 1.562(18) . ? C19 C22 1.559(19) . ? C19A C20A 1.503(17) . ? C19A C21A 1.62(2) . ? C19A C22A 1.51(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.537(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 N4 1.477(10) . ? N5 C25 1.139(9) . ? C25 C26 1.432(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N6 C27 1.142(10) . ? C27 C28 1.443(11) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? B1 C29 1.637(11) . ? B1 C35 1.659(11) . ? B1 C41 1.635(10) . ? B1 C47 1.643(11) . ? C29 C30 1.403(10) . ? C29 C34 1.395(10) . ? C30 H30 0.9500 . ? C30 C31 1.399(11) . ? C31 H31 0.9500 . ? C31 C32 1.387(11) . ? C32 H32 0.9500 . ? C32 C33 1.373(10) . ? C33 H33 0.9500 . ? C33 C34 1.392(10) . ? C34 H34 0.9500 . ? C35 C36 1.387(10) . ? C35 C40 1.390(10) . ? C36 H36 0.9500 . ? C36 C37 1.382(11) . ? C37 H37 0.9500 . ? C37 C38 1.380(13) . ? C38 H38 0.9500 . ? C38 C39 1.364(13) . ? C39 H39 0.9500 . ? C39 C40 1.391(11) . ? C40 H40 0.9500 . ? C41 C42 1.404(10) . ? C41 C46 1.409(10) . ? C42 H42 0.9500 . ? C42 C43 1.380(10) . ? C43 H43 0.9500 . ? C43 C44 1.382(10) . ? C44 H44 0.9500 . ? C44 C45 1.369(10) . ? C45 H45 0.9500 . ? C45 C46 1.397(10) . ? C46 H46 0.9500 . ? C47 C48 1.397(10) . ? C47 C52 1.387(10) . ? C48 H48 0.9500 . ? C48 C49 1.382(11) . ? C49 H49 0.9500 . ? C49 C50 1.379(11) . ? C50 H50 0.9500 . ? C50 C51 1.382(11) . ? C51 H51 0.9500 . ? C51 C52 1.389(11) . ? C52 H52 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U1 N2 98.8(2) . . ? N1 U1 N3 128.4(2) . . ? N1 U1 N4 69.5(2) . . ? N1 U1 N5 104.2(2) . . ? N1 U1 N6 77.9(2) . . ? N2 U1 N4 72.8(2) . . ? N2 U1 N5 96.1(2) . . ? N2 U1 N6 176.3(2) . . ? N3 U1 N2 99.6(3) . . ? N3 U1 N4 70.8(2) . . ? N3 U1 N5 121.1(2) . . ? N3 U1 N6 83.9(2) . . ? N4 U1 N6 107.2(2) . . ? N5 U1 N4 165.6(2) . . ? N5 U1 N6 83.2(2) . . ? Si1 N1 U1 130.0(3) . . ? C7 N1 U1 112.3(5) . . ? C7 N1 Si1 117.0(5) . . ? N1 Si1 C1 107.2(4) . . ? N1 Si1 C2 110.7(4) . . ? N1 Si1 C3 113.0(4) . . ? C1 Si1 C2 107.4(5) . . ? C1 Si1 C3 109.0(4) . . ? C2 Si1 C3 109.4(4) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Si1 109.2(6) . . ? C4 C3 C5 107.6(7) . . ? C5 C3 Si1 110.1(6) . . ? C6 C3 Si1 111.7(6) . . ? C6 C3 C4 109.0(7) . . ? C6 C3 C5 109.1(8) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 110.2 . . ? N1 C7 H7B 110.2 . . ? N1 C7 C8 107.7(7) . . ? H7A C7 H7B 108.5 . . ? C8 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? C7 C8 H8A 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N4 C8 C7 108.7(7) . . ? N4 C8 H8A 109.9 . . ? N4 C8 H8B 109.9 . . ? Si2 N2 U1 127.3(3) . . ? C15 N2 U1 114.2(5) . . ? C15 N2 Si2 116.7(5) . . ? N2 Si2 C9 108.5(3) . . ? N2 Si2 C10 110.7(4) . . ? N2 Si2 C11 113.5(4) . . ? C9 Si2 C11 107.7(4) . . ? C10 Si2 C9 107.0(4) . . ? C10 Si2 C11 109.2(4) . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Si2 110.2(7) . . ? C12 C11 C13 108.9(8) . . ? C12 C11 C14 107.8(8) . . ? C13 C11 Si2 110.5(6) . . ? C14 C11 Si2 110.3(6) . . ? C14 C11 C13 109.1(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.8 . . ? N2 C15 H15B 109.8 . . ? N2 C15 C16 109.2(6) . . ? H15A C15 H15B 108.3 . . ? C16 C15 H15A 109.8 . . ? C16 C15 H15B 109.8 . . ? C15 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N4 C16 C15 110.2(7) . . ? N4 C16 H16A 109.6 . . ? N4 C16 H16B 109.6 . . ? Si3 N3 U1 124.2(4) . . ? C23 N3 U1 122.0(5) . . ? C23 N3 Si3 113.8(6) . . ? N3 Si3 C17 106.4(4) . . ? N3 Si3 C18 109.0(4) . . ? N3 Si3 C19 113.6(6) . . ? N3 Si3 C19A 114.7(6) . . ? C17 Si3 C18 107.7(5) . . ? C17 Si3 C19 112.9(6) . . ? C17 Si3 C19A 110.5(6) . . ? C19 Si3 C18 107.1(6) . . ? C19A Si3 C18 108.5(5) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Si3 104(4) . . ? C21 C19 Si3 98(3) . . ? C21 C19 C20 140(6) . . ? C22 C19 Si3 96(4) . . ? C22 C19 C20 107(5) . . ? C22 C19 C21 104(5) . . ? C20A C19A Si3 112.3(10) . . ? C20A C19A C21A 110.3(14) . . ? C20A C19A C22A 107.1(12) . . ? C21A C19A Si3 110.4(8) . . ? C22A C19A Si3 109.6(12) . . ? C22A C19A C21A 106.9(11) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19A C20A H20D 109.5 . . ? C19A C20A H20E 109.5 . . ? C19A C20A H20F 109.5 . . ? H20D C20A H20E 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19A C21A H21D 109.5 . . ? C19A C21A H21E 109.5 . . ? C19A C21A H21F 109.5 . . ? H21D C21A H21E 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19A C22A H22D 109.5 . . ? C19A C22A H22E 109.5 . . ? C19A C22A H22F 109.5 . . ? H22D C22A H22E 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? N3 C23 H23A 109.7 . . ? N3 C23 H23B 109.7 . . ? N3 C23 C24 109.8(7) . . ? H23A C23 H23B 108.2 . . ? C24 C23 H23A 109.7 . . ? C24 C23 H23B 109.7 . . ? C23 C24 H24A 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? N4 C24 C23 109.7(7) . . ? N4 C24 H24A 109.7 . . ? N4 C24 H24B 109.7 . . ? C8 N4 U1 109.8(5) . . ? C8 N4 C16 112.0(7) . . ? C16 N4 U1 106.6(4) . . ? C24 N4 U1 107.5(5) . . ? C24 N4 C8 108.5(6) . . ? C24 N4 C16 112.4(7) . . ? C25 N5 U1 167.6(7) . . ? N5 C25 C26 177.3(9) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 N6 U1 163.6(6) . . ? N6 C27 C28 177.1(9) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 B1 C35 112.0(6) . . ? C29 B1 C47 113.0(6) . . ? C41 B1 C29 105.2(6) . . ? C41 B1 C35 111.2(6) . . ? C41 B1 C47 111.4(6) . . ? C47 B1 C35 104.3(6) . . ? C30 C29 B1 123.4(7) . . ? C34 C29 B1 121.5(6) . . ? C34 C29 C30 114.7(7) . . ? C29 C30 H30 118.8 . . ? C31 C30 C29 122.4(8) . . ? C31 C30 H30 118.8 . . ? C30 C31 H31 119.8 . . ? C32 C31 C30 120.4(7) . . ? C32 C31 H31 119.8 . . ? C31 C32 H32 120.7 . . ? C33 C32 C31 118.6(7) . . ? C33 C32 H32 120.7 . . ? C32 C33 H33 119.9 . . ? C32 C33 C34 120.3(7) . . ? C34 C33 H33 119.9 . . ? C29 C34 H34 118.3 . . ? C33 C34 C29 123.5(7) . . ? C33 C34 H34 118.3 . . ? C36 C35 B1 121.2(6) . . ? C36 C35 C40 115.1(7) . . ? C40 C35 B1 123.5(7) . . ? C35 C36 H36 118.2 . . ? C37 C36 C35 123.6(8) . . ? C37 C36 H36 118.2 . . ? C36 C37 H37 120.7 . . ? C38 C37 C36 118.5(9) . . ? C38 C37 H37 120.7 . . ? C37 C38 H38 119.6 . . ? C39 C38 C37 120.7(8) . . ? C39 C38 H38 119.6 . . ? C38 C39 H39 120.5 . . ? C38 C39 C40 119.0(8) . . ? C40 C39 H39 120.5 . . ? C35 C40 C39 123.0(8) . . ? C35 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? C42 C41 B1 123.2(7) . . ? C42 C41 C46 114.4(6) . . ? C46 C41 B1 122.1(6) . . ? C41 C42 H42 118.4 . . ? C43 C42 C41 123.2(7) . . ? C43 C42 H42 118.4 . . ? C42 C43 H43 119.9 . . ? C42 C43 C44 120.3(7) . . ? C44 C43 H43 119.9 . . ? C43 C44 H44 120.4 . . ? C45 C44 C43 119.2(7) . . ? C45 C44 H44 120.4 . . ? C44 C45 H45 119.9 . . ? C44 C45 C46 120.1(7) . . ? C46 C45 H45 119.9 . . ? C41 C46 H46 118.6 . . ? C45 C46 C41 122.7(7) . . ? C45 C46 H46 118.6 . . ? C48 C47 B1 120.7(7) . . ? C52 C47 B1 123.5(6) . . ? C52 C47 C48 115.5(7) . . ? C47 C48 H48 119.0 . . ? C49 C48 C47 122.0(8) . . ? C49 C48 H48 119.0 . . ? C48 C49 H49 119.5 . . ? C50 C49 C48 121.0(8) . . ? C50 C49 H49 119.5 . . ? C49 C50 H50 120.7 . . ? C49 C50 C51 118.6(8) . . ? C51 C50 H50 120.7 . . ? C50 C51 H51 120.2 . . ? C50 C51 C52 119.6(8) . . ? C52 C51 H51 120.2 . . ? C47 C52 C51 123.3(7) . . ? C47 C52 H52 118.4 . . ? C51 C52 H52 118.4 . . ? 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 _geom_torsion_publ_flag U1 N1 Si1 C1 12.1(6) . . . . ? U1 N1 Si1 C2 128.9(5) . . . . ? U1 N1 Si1 C3 -108.1(5) . . . . ? U1 N1 C7 C8 -64.5(7) . . . . ? U1 N2 Si2 C9 1.1(6) . . . . ? U1 N2 Si2 C10 118.3(5) . . . . ? U1 N2 Si2 C11 -118.5(5) . . . . ? U1 N2 C15 C16 -51.3(8) . . . . ? U1 N3 Si3 C17 -5.8(6) . . . . ? U1 N3 Si3 C18 110.0(5) . . . . ? U1 N3 Si3 C19 -130.6(6) . . . . ? U1 N3 Si3 C19A -128.2(6) . . . . ? U1 N3 C23 C24 -30.6(10) . . . . ? N1 Si1 C3 C4 62.9(6) . . . . ? N1 Si1 C3 C5 -179.2(6) . . . . ? N1 Si1 C3 C6 -57.8(7) . . . . ? N1 C7 C8 N4 54.0(9) . . . . ? Si1 N1 C7 C8 106.9(7) . . . . ? C1 Si1 C3 C4 -56.2(7) . . . . ? C1 Si1 C3 C5 61.7(7) . . . . ? C1 Si1 C3 C6 -176.9(6) . . . . ? C2 Si1 C3 C4 -173.3(6) . . . . ? C2 Si1 C3 C5 -55.4(7) . . . . ? C2 Si1 C3 C6 66.0(7) . . . . ? C7 N1 Si1 C1 -157.5(6) . . . . ? C7 N1 Si1 C2 -40.6(7) . . . . ? C7 N1 Si1 C3 82.4(7) . . . . ? C7 C8 N4 U1 -22.4(7) . . . . ? C7 C8 N4 C16 -140.5(7) . . . . ? C7 C8 N4 C24 94.8(8) . . . . ? N2 C15 C16 N4 58.2(9) . . . . ? Si2 N2 C15 C16 114.9(7) . . . . ? C15 N2 Si2 C9 -163.0(6) . . . . ? C15 N2 Si2 C10 -45.9(7) . . . . ? C15 N2 Si2 C11 77.3(7) . . . . ? C15 C16 N4 U1 -36.0(7) . . . . ? C15 C16 N4 C8 84.1(8) . . . . ? C15 C16 N4 C24 -153.4(7) . . . . ? N3 Si3 C19 C20 38(4) . . . . ? N3 Si3 C19 C21 -108(4) . . . . ? N3 Si3 C19 C22 147(4) . . . . ? N3 Si3 C19A C20A 59.5(15) . . . . ? N3 Si3 C19A C21A -64.0(10) . . . . ? N3 Si3 C19A C22A 178.5(10) . . . . ? N3 C23 C24 N4 49.4(10) . . . . ? Si3 N3 C23 C24 147.1(6) . . . . ? C17 Si3 C19 C20 -83(4) . . . . ? C17 Si3 C19 C21 131(4) . . . . ? C17 Si3 C19 C22 26(4) . . . . ? C17 Si3 C19A C20A -60.6(15) . . . . ? C17 Si3 C19A C21A 175.9(9) . . . . ? C17 Si3 C19A C22A 58.3(12) . . . . ? C18 Si3 C19 C20 158(4) . . . . ? C18 Si3 C19 C21 12(4) . . . . ? C18 Si3 C19 C22 -92(4) . . . . ? C18 Si3 C19A C20A -178.4(13) . . . . ? C18 Si3 C19A C21A 58.1(11) . . . . ? C18 Si3 C19A C22A -59.4(12) . . . . ? C23 N3 Si3 C17 176.6(7) . . . . ? C23 N3 Si3 C18 -67.6(7) . . . . ? C23 N3 Si3 C19 51.8(8) . . . . ? C23 N3 Si3 C19A 54.2(8) . . . . ? C23 C24 N4 U1 -43.6(8) . . . . ? C23 C24 N4 C8 -162.3(7) . . . . ? C23 C24 N4 C16 73.3(9) . . . . ? B1 C29 C30 C31 -173.7(7) . . . . ? B1 C29 C34 C33 175.0(6) . . . . ? B1 C35 C36 C37 175.6(8) . . . . ? B1 C35 C40 C39 -175.3(8) . . . . ? B1 C41 C42 C43 -174.8(7) . . . . ? B1 C41 C46 C45 174.9(7) . . . . ? B1 C47 C48 C49 -176.3(7) . . . . ? B1 C47 C52 C51 175.1(7) . . . . ? C29 B1 C35 C36 31.1(10) . . . . ? C29 B1 C35 C40 -154.5(7) . . . . ? C29 B1 C41 C42 90.3(8) . . . . ? C29 B1 C41 C46 -83.2(8) . . . . ? C29 B1 C47 C48 -40.6(9) . . . . ? C29 B1 C47 C52 146.1(7) . . . . ? C29 C30 C31 C32 -0.8(12) . . . . ? C30 C29 C34 C33 1.6(10) . . . . ? C30 C31 C32 C33 0.7(11) . . . . ? C31 C32 C33 C34 0.4(11) . . . . ? C32 C33 C34 C29 -1.7(11) . . . . ? C34 C29 C30 C31 -0.4(10) . . . . ? C35 B1 C29 C30 -146.3(7) . . . . ? C35 B1 C29 C34 40.9(9) . . . . ? C35 B1 C41 C42 -31.1(10) . . . . ? C35 B1 C41 C46 155.4(7) . . . . ? C35 B1 C47 C48 81.2(8) . . . . ? C35 B1 C47 C52 -92.1(8) . . . . ? C35 C36 C37 C38 -0.7(14) . . . . ? C36 C35 C40 C39 -0.7(12) . . . . ? C36 C37 C38 C39 0.5(15) . . . . ? C37 C38 C39 C40 -0.4(14) . . . . ? C38 C39 C40 C35 0.5(13) . . . . ? C40 C35 C36 C37 0.8(13) . . . . ? C41 B1 C29 C30 92.8(8) . . . . ? C41 B1 C29 C34 -80.0(8) . . . . ? C41 B1 C35 C36 148.5(7) . . . . ? C41 B1 C35 C40 -37.1(10) . . . . ? C41 B1 C47 C48 -158.8(7) . . . . ? C41 B1 C47 C52 27.9(10) . . . . ? C41 C42 C43 C44 0.1(12) . . . . ? C42 C41 C46 C45 0.9(11) . . . . ? C42 C43 C44 C45 0.8(12) . . . . ? C43 C44 C45 C46 -0.7(12) . . . . ? C44 C45 C46 C41 -0.1(12) . . . . ? C46 C41 C42 C43 -0.8(11) . . . . ? C47 B1 C29 C30 -28.9(9) . . . . ? C47 B1 C29 C34 158.3(6) . . . . ? C47 B1 C35 C36 -91.3(8) . . . . ? C47 B1 C35 C40 83.0(8) . . . . ? C47 B1 C41 C42 -147.0(7) . . . . ? C47 B1 C41 C46 39.5(9) . . . . ? C47 C48 C49 C50 1.8(13) . . . . ? C48 C47 C52 C51 1.4(11) . . . . ? C48 C49 C50 C51 0.2(13) . . . . ? C49 C50 C51 C52 -1.3(12) . . . . ? C50 C51 C52 C47 0.5(12) . . . . ? C52 C47 C48 C49 -2.5(11) . . . . ? _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' data_6 _nottingham_internal_coll_name THBGLP _nottingham_internal_coll_number 12008 _nottingham_internal_coll_client BMG/STL _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_time '10s, 40s' _nottingham_internal_coll_frame_width '1 degree' _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_user pczbg _nottingham_internal_coll_date 19/11/2012 _nottingham_internal_coll_location NOTTS _nottingham_internal_NCS_number ? _nottingham_internal_process_user pczbg _nottingham_internal_process_date 20/11/2012 _nottingham_internal_solution_user BMG _nottingham_internal_solution_date 20/11/2012 _nottingham_internal_refinement_user BMG _nottingham_internal_refinement_date 01/10/2014 _nottingham_internal_self_validation_user BMG _nottingham_internal_self_validation_date 01/10/2014 _nottingham_internal_self_archive_date 02/10/2014 _nottingham_internal_validation_user pczwl _nottingham_internal_validation_date 10/11/2014 _nottingham_internal_archive_date 10/11/2014 _refine_special_details ; Global enhanced rigid bond and similarity restraints were applied to the thermal parameters of all atoms. The silyl group Si2 (and the attached alkyl groups) is disordered over two positions. The occupancies of the two components were refined competitively, converging at a ratio of 0.515:0.485. The ligand arm beginning with N6 is disordered over two positions. The occupancies of the two components were refined competitively, converging at a ratio of 0.662:0.338. Chemically equivalent Si-N, Si-C and C-C bonds within disordered fragments were restrained to be approximately equal. ; _audit_creation_date 2014-10-01 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C48 H112 N8 O2 Si6 Th2' _chemical_formula_sum 'C48 H112 N8 O2 Si6 Th2' _chemical_formula_weight 1466.07 _chemical_melting_point ? _chemical_oxdiff_formula 'C48 H112 N8 Si6 Th2' _chemical_oxdiff_usercomment 'THBGLP #12008 IN FOMBLIN FILM ON MICROMOUNT FOR BG/STL' 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' '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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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' _cell_length_a 14.3210(3) _cell_length_b 22.3137(4) _cell_length_c 20.5302(4) _cell_angle_alpha 90 _cell_angle_beta 94.3624(17) _cell_angle_gamma 90 _cell_volume 6541.5(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 32027 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 74.5472 _cell_measurement_theta_min 3.6338 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 15.911 _exptl_absorpt_correction_T_max 0.458 _exptl_absorpt_correction_T_min 0.185 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2944 _exptl_crystal_size_max 0.1685 _exptl_crystal_size_mid 0.1117 _exptl_crystal_size_min 0.0796 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 87133 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 74.720 _diffrn_reflns_theta_min 3.637 _diffrn_ambient_temperature 120(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 10.3613 _diffrn_detector_type 'Agilent Diffraction Atlas detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -100.00 -55.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -43.9127 -153.0000 67.0000 45 #__ type_ start__ end____ width___ exp.time_ 2 omega -70.00 -12.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -43.9127 77.0000 150.0000 58 #__ type_ start__ end____ width___ exp.time_ 3 omega 26.00 111.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 43.9127 57.0000 -30.0000 85 #__ type_ start__ end____ width___ exp.time_ 4 omega -101.00 -75.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -60.0000 -125.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 5 omega 29.00 88.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -95.0000 120.0000 59 #__ type_ start__ end____ width___ exp.time_ 6 omega 115.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 45.0000 150.0000 43 #__ type_ start__ end____ width___ exp.time_ 7 omega 34.00 67.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 -90.0000 33 #__ type_ start__ end____ width___ exp.time_ 8 omega 47.00 74.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 120.0000 27 #__ type_ start__ end____ width___ exp.time_ 9 omega 36.00 109.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -121.0000 51.0000 73 #__ type_ start__ end____ width___ exp.time_ 10 omega 27.00 97.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -95.0000 60.0000 70 #__ type_ start__ end____ width___ exp.time_ 11 omega 72.00 101.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -125.0000 -150.0000 29 #__ type_ start__ end____ width___ exp.time_ 12 omega 79.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 77.0000 -150.0000 79 #__ type_ start__ end____ width___ exp.time_ 13 omega 40.00 68.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 30.0000 28 #__ type_ start__ end____ width___ exp.time_ 14 omega 90.00 120.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -125.0000 -90.0000 30 #__ type_ start__ end____ width___ exp.time_ 15 omega 41.00 70.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 150.0000 29 #__ type_ start__ end____ width___ exp.time_ 16 omega 45.00 71.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 -120.0000 26 #__ type_ start__ end____ width___ exp.time_ 17 omega -24.00 69.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 43.9127 -57.0000 -120.0000 93 #__ type_ start__ end____ width___ exp.time_ 18 omega 14.00 115.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 43.9127 77.0000 -150.0000 101 #__ type_ start__ end____ width___ exp.time_ 19 omega 19.00 112.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 43.9127 57.0000 120.0000 93 #__ type_ start__ end____ width___ exp.time_ 20 omega -131.00 -30.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -60.0000 -77.0000 30.0000 101 #__ type_ start__ end____ width___ exp.time_ 21 omega 76.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 77.0000 -120.0000 82 #__ type_ start__ end____ width___ exp.time_ 22 omega 36.00 77.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -45.0000 -150.0000 41 #__ type_ start__ end____ width___ exp.time_ 23 omega 85.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 30.0000 120.0000 73 #__ type_ start__ end____ width___ exp.time_ 24 omega 27.00 110.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -95.0000 -120.0000 83 #__ type_ start__ end____ width___ exp.time_ 25 omega 83.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 45.0000 -60.0000 75 #__ type_ start__ end____ width___ exp.time_ 26 omega 33.00 69.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 -30.0000 90.0000 36 #__ type_ start__ end____ width___ exp.time_ 27 omega 76.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 77.0000 -180.0000 82 #__ type_ start__ end____ width___ exp.time_ 28 omega 66.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 15.0000 60.0000 92 #__ type_ start__ end____ width___ exp.time_ 29 omega -112.00 -19.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -43.9127 -57.0000 90.0000 93 #__ type_ start__ end____ width___ exp.time_ 30 omega -113.00 -55.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -43.9127 -153.0000 -108.0000 58 #__ type_ start__ end____ width___ exp.time_ 31 omega 14.00 115.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 43.9127 77.0000 -60.0000 101 #__ type_ start__ end____ width___ exp.time_ 32 omega 80.00 105.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 61.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 33 omega 76.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 77.0000 120.0000 82 #__ type_ start__ end____ width___ exp.time_ 34 omega 80.00 158.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 105.8472 61.0000 -30.0000 78 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova-Duo, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1034965000 _diffrn_orient_matrix_UB_12 0.0029634000 _diffrn_orient_matrix_UB_13 0.0263995000 _diffrn_orient_matrix_UB_21 0.0009707000 _diffrn_orient_matrix_UB_22 -0.0685425000 _diffrn_orient_matrix_UB_23 0.0091809000 _diffrn_orient_matrix_UB_31 0.0304759000 _diffrn_orient_matrix_UB_32 -0.0079441000 _diffrn_orient_matrix_UB_33 -0.0698364000 _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'microfocus sealed tube' _diffrn_source_target Cu _diffrn_source_type 'Agilent Diffraction microfocus tube' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 11326 _reflns_number_total 13232 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 67.13 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _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 ? _refine_diff_density_max 4.319 _refine_diff_density_min -2.033 _refine_diff_density_rms 0.130 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 770 _refine_ls_number_reflns 13232 _refine_ls_number_restraints 1264 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0455 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+31.9469P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1128 _refine_ls_wR_factor_ref 0.1184 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C12A-C11A \\sim C13A-C11A \\sim C14A-C11A \\sim C12-C11 \\sim C13-C11 \\sim C14-C11 with sigma of 0.02 C37-C35 \\sim C37A-C35A \\sim C38-C35 \\sim C38A-C35A \\sim C36A-C35A \\sim C36-C35 with sigma of 0.02 Si5A-N6A \\sim Si5-N6 with sigma of 0.02 Si5-C35 \\sim Si5A-C35A with sigma of 0.02 Si5-C33 \\sim Si5A-C33A \\sim Si5A-C34A \\sim Si5-C34 with sigma of 0.02 Si2A-N2 \\sim Si2-N2 with sigma of 0.02 Si2A-C11A \\sim Si2-C11 with sigma of 0.02 Si2-C10 \\sim Si2-C9 \\sim Si2A-C10A \\sim Si2A-C9A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 4. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(Si2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)= Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)= Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)= Sof(H14F)=1-FVAR(1) Sof(Si2)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)= Sof(H10C)=Sof(C11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)= Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1) Sof(N6A)=Sof(Si5A)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)= Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(C36A)=Sof(H36D)=Sof(H36E)= Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38D)= Sof(H38E)=Sof(H38F)=Sof(H39C)=Sof(H39D)=1-FVAR(2) Sof(N6)=Sof(Si5)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)= Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)= Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(H39A)= Sof(H39B)=FVAR(2) 6.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C31(H31A,H31B), C32(H32A,H32B), C39(H39C,H39D), C39(H39A,H39B), C40(H40A,H40B), C47(H47A,H47B), C48(H48A,H48B) 6.b Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A, H9B,H9C), C9A(H9AA,H9AB,H9AC), C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F), C13(H13A,H13B,H13C), C13A(H13D,H13E, H13F), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B, H22C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A, H30B,H30C), C33(H33A,H33B,H33C), C33A(H33D,H33E,H33F), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F), C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F), C37(H37A,H37B, H37C), C37A(H37D,H37E,H37F), C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B, H45C), C46(H46A,H46B,H46C) ; _atom_sites_solution_hydrogens 'geom, Me from difmap' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.53551(2) 0.29336(2) 0.56303(2) 0.03648(7) Uani 1 1 d . . . . . O1 O 0.4732(4) 0.2900(2) 0.6695(2) 0.0468(11) Uani 1 1 d . . . . . N1 N 0.4314(5) 0.3752(3) 0.5684(3) 0.0515(14) Uani 1 1 d . . . . . Si1 Si 0.38100(17) 0.39619(9) 0.63787(10) 0.0540(5) Uani 1 1 d . . . . . C1 C 0.3992(5) 0.3276(3) 0.6920(3) 0.0485(15) Uani 1 1 d . . . . . H1A H 0.4161 0.3404 0.7376 0.058 Uiso 1 1 calc R . . . . H1B H 0.3402 0.3044 0.6914 0.058 Uiso 1 1 calc R . . . . C2 C 0.4390(8) 0.4642(4) 0.6781(5) 0.075(3) Uani 1 1 d . . . . . H2A H 0.5004 0.4530 0.6988 0.113 Uiso 1 1 calc GR . . . . H2B H 0.3997 0.4799 0.7112 0.113 Uiso 1 1 calc GR . . . . H2C H 0.4469 0.4951 0.6450 0.113 Uiso 1 1 calc GR . . . . C3 C 0.2493(7) 0.4112(4) 0.6281(4) 0.0667(19) Uani 1 1 d . . . . . C4 C 0.2127(7) 0.4127(5) 0.6967(5) 0.077(2) Uani 1 1 d . . . . . H4A H 0.2184 0.3728 0.7165 0.115 Uiso 1 1 calc GR . . . . H4B H 0.1468 0.4250 0.6933 0.115 Uiso 1 1 calc GR . . . . H4C H 0.2496 0.4415 0.7241 0.115 Uiso 1 1 calc GR . . . . C5 C 0.2262(8) 0.4730(5) 0.5964(5) 0.087(3) Uani 1 1 d . . . . . H5A H 0.2677 0.5035 0.6171 0.131 Uiso 1 1 calc GR . . . . H5B H 0.1609 0.4834 0.6023 0.131 Uiso 1 1 calc GR . . . . H5C H 0.2354 0.4711 0.5496 0.131 Uiso 1 1 calc GR . . . . C6 C 0.2009(7) 0.3608(5) 0.5872(5) 0.077(2) Uani 1 1 d . . . . . H6A H 0.2256 0.3597 0.5440 0.116 Uiso 1 1 calc GR . . . . H6B H 0.1333 0.3682 0.5824 0.116 Uiso 1 1 calc GR . . . . H6C H 0.2130 0.3223 0.6093 0.116 Uiso 1 1 calc GR . . . . C7 C 0.4143(8) 0.4161(4) 0.5128(4) 0.072(2) Uani 1 1 d . . . . . H7A H 0.3532 0.4060 0.4897 0.086 Uiso 1 1 calc R . . . . H7B H 0.4099 0.4575 0.5296 0.086 Uiso 1 1 calc R . . . . C8 C 0.4861(7) 0.4142(4) 0.4664(4) 0.066(2) Uani 1 1 d . . . . . H8A H 0.4622 0.4343 0.4255 0.080 Uiso 1 1 calc R . . . . H8B H 0.5416 0.4367 0.4846 0.080 Uiso 1 1 calc R . . . . N2 N 0.4833(4) 0.2329(2) 0.4744(3) 0.0428(11) Uani 1 1 d . . . . . Si2 Si 0.4768(3) 0.15890(15) 0.44982(17) 0.0407(11) Uani 0.515(6) 1 d . . P A 1 Si2A Si 0.5345(3) 0.17694(18) 0.42659(18) 0.0455(12) Uani 0.485(6) 1 d . . P A 2 C9 C 0.3558(10) 0.1315(8) 0.4208(9) 0.059(4) Uani 0.515(6) 1 d . . P A 1 H9A H 0.3097 0.1486 0.4485 0.089 Uiso 0.515(6) 1 calc GR . P A 1 H9B H 0.3539 0.0877 0.4234 0.089 Uiso 0.515(6) 1 calc GR . P A 1 H9C H 0.3410 0.1441 0.3754 0.089 Uiso 0.515(6) 1 calc GR . P A 1 C9A C 0.6665(9) 0.1741(9) 0.4430(8) 0.055(4) Uani 0.485(6) 1 d . . P A 2 H9AA H 0.6952 0.2048 0.4169 0.083 Uiso 0.485(6) 1 calc GR . P A 2 H9AB H 0.6893 0.1345 0.4311 0.083 Uiso 0.485(6) 1 calc GR . P A 2 H9AC H 0.6831 0.1815 0.4895 0.083 Uiso 0.485(6) 1 calc GR . P A 2 C10 C 0.5192(14) 0.1090(7) 0.5200(8) 0.060(4) Uani 0.515(6) 1 d . . P A 1 H10A H 0.5877 0.1109 0.5261 0.090 Uiso 0.515(6) 1 calc GR . P A 1 H10B H 0.4997 0.0676 0.5105 0.090 Uiso 0.515(6) 1 calc GR . P A 1 H10C H 0.4922 0.1225 0.5599 0.090 Uiso 0.515(6) 1 calc GR . P A 1 C10A C 0.5126(18) 0.1926(9) 0.3358(6) 0.056(4) Uani 0.485(6) 1 d . . P A 2 H10D H 0.4471 0.1837 0.3218 0.084 Uiso 0.485(6) 1 calc GR . P A 2 H10E H 0.5538 0.1674 0.3115 0.084 Uiso 0.485(6) 1 calc GR . P A 2 H10F H 0.5255 0.2349 0.3273 0.084 Uiso 0.485(6) 1 calc GR . P A 2 C11 C 0.5533(11) 0.1433(6) 0.3804(7) 0.068(3) Uani 0.515(6) 1 d . . P A 1 C11A C 0.4850(10) 0.1002(6) 0.4420(6) 0.055(3) Uani 0.485(6) 1 d . . P A 2 C12 C 0.5497(18) 0.0770(7) 0.3610(12) 0.089(5) Uani 0.515(6) 1 d . . P A 1 H12A H 0.5748 0.0525 0.3979 0.134 Uiso 0.515(6) 1 calc GR . P A 1 H12B H 0.5874 0.0706 0.3237 0.134 Uiso 0.515(6) 1 calc GR . P A 1 H12C H 0.4847 0.0654 0.3489 0.134 Uiso 0.515(6) 1 calc GR . P A 1 C12A C 0.5175(16) 0.0775(9) 0.5104(8) 0.066(4) Uani 0.485(6) 1 d . . P A 2 H12D H 0.5858 0.0733 0.5140 0.099 Uiso 0.485(6) 1 calc GR . P A 2 H12E H 0.4886 0.0385 0.5177 0.099 Uiso 0.485(6) 1 calc GR . P A 2 H12F H 0.4988 0.1062 0.5431 0.099 Uiso 0.485(6) 1 calc GR . P A 2 C13 C 0.521(2) 0.1763(11) 0.3179(9) 0.085(6) Uani 0.515(6) 1 d . . P A 1 H13A H 0.4522 0.1802 0.3151 0.127 Uiso 0.515(6) 1 calc GR . P A 1 H13B H 0.5394 0.1537 0.2801 0.127 Uiso 0.515(6) 1 calc GR . P A 1 H13C H 0.5491 0.2163 0.3181 0.127 Uiso 0.515(6) 1 calc GR . P A 1 C13A C 0.3776(11) 0.1018(8) 0.4358(10) 0.062(4) Uani 0.485(6) 1 d . . P A 2 H13D H 0.3554 0.1308 0.4669 0.093 Uiso 0.485(6) 1 calc GR . P A 2 H13E H 0.3532 0.0619 0.4452 0.093 Uiso 0.485(6) 1 calc GR . P A 2 H13F H 0.3556 0.1136 0.3913 0.093 Uiso 0.485(6) 1 calc GR . P A 2 C14 C 0.6533(13) 0.1615(11) 0.4027(12) 0.091(5) Uani 0.515(6) 1 d . . P A 1 H14A H 0.6522 0.1983 0.4286 0.136 Uiso 0.515(6) 1 calc GR . P A 1 H14B H 0.6887 0.1685 0.3644 0.136 Uiso 0.515(6) 1 calc GR . P A 1 H14C H 0.6831 0.1294 0.4294 0.136 Uiso 0.515(6) 1 calc GR . P A 1 C14A C 0.5172(16) 0.0543(7) 0.3917(9) 0.068(4) Uani 0.485(6) 1 d . . P A 2 H14D H 0.4944 0.0668 0.3476 0.101 Uiso 0.485(6) 1 calc GR . P A 2 H14E H 0.4918 0.0147 0.4010 0.101 Uiso 0.485(6) 1 calc GR . P A 2 H14F H 0.5858 0.0524 0.3948 0.101 Uiso 0.485(6) 1 calc GR . P A 2 C15 C 0.4063(6) 0.2687(3) 0.4428(4) 0.0580(17) Uani 1 1 d . . . . . H15A H 0.3653 0.2830 0.4763 0.070 Uiso 1 1 calc R . . . . H15B H 0.3683 0.2433 0.4114 0.070 Uiso 1 1 calc R . . . . C16 C 0.4437(7) 0.3217(4) 0.4074(4) 0.065(2) Uani 1 1 d . . . . . H16A H 0.4726 0.3079 0.3678 0.078 Uiso 1 1 calc R . . . . H16B H 0.3917 0.3493 0.3937 0.078 Uiso 1 1 calc R . . . . N3 N 0.6710(5) 0.3451(3) 0.5388(3) 0.0539(15) Uani 1 1 d . . . . . Si3 Si 0.73494(16) 0.38592(11) 0.59879(10) 0.0578(5) Uani 1 1 d . . . . . C17 C 0.7131(7) 0.4682(4) 0.5988(4) 0.072(2) Uani 1 1 d . . . . . H17A H 0.7128 0.4836 0.5541 0.107 Uiso 1 1 calc GR . . . . H17B H 0.7627 0.4882 0.6264 0.107 Uiso 1 1 calc GR . . . . H17C H 0.6524 0.4762 0.6161 0.107 Uiso 1 1 calc GR . . . . C18 C 0.7011(7) 0.3535(5) 0.6773(4) 0.078(3) Uani 1 1 d . . . . . H18A H 0.6327 0.3503 0.6762 0.118 Uiso 1 1 calc GR . . . . H18B H 0.7238 0.3795 0.7135 0.118 Uiso 1 1 calc GR . . . . H18C H 0.7289 0.3136 0.6834 0.118 Uiso 1 1 calc GR . . . . C19 C 0.8656(7) 0.3771(4) 0.5948(5) 0.071(2) Uani 1 1 d . . . . . C20 C 0.9155(7) 0.3925(6) 0.6632(5) 0.093(3) Uani 1 1 d . . . . . H20A H 0.9024 0.4343 0.6742 0.140 Uiso 1 1 calc GR . . . . H20B H 0.9832 0.3869 0.6619 0.140 Uiso 1 1 calc GR . . . . H20C H 0.8921 0.3660 0.6964 0.140 Uiso 1 1 calc GR . . . . C21 C 0.8891(7) 0.3098(5) 0.5750(5) 0.073(2) Uani 1 1 d . . . . . H21A H 0.8590 0.2819 0.6037 0.110 Uiso 1 1 calc GR . . . . H21B H 0.9571 0.3037 0.5796 0.110 Uiso 1 1 calc GR . . . . H21C H 0.8658 0.3026 0.5295 0.110 Uiso 1 1 calc GR . . . . C22 C 0.9014(6) 0.4248(4) 0.5461(4) 0.070(2) Uani 1 1 d . . . . . H22A H 0.8668 0.4202 0.5033 0.106 Uiso 1 1 calc GR . . . . H22B H 0.9684 0.4187 0.5417 0.106 Uiso 1 1 calc GR . . . . H22C H 0.8912 0.4652 0.5629 0.106 Uiso 1 1 calc GR . . . . C23 C 0.6840(6) 0.3662(5) 0.4712(4) 0.068(2) Uani 1 1 d . . . . . H23A H 0.7424 0.3487 0.4564 0.082 Uiso 1 1 calc R . . . . H23B H 0.6908 0.4103 0.4715 0.082 Uiso 1 1 calc R . . . . C24 C 0.6037(7) 0.3491(4) 0.4243(4) 0.068(2) Uani 1 1 d . . . . . H24A H 0.6036 0.3753 0.3854 0.081 Uiso 1 1 calc R . . . . H24B H 0.6127 0.3073 0.4098 0.081 Uiso 1 1 calc R . . . . N4 N 0.5145(5) 0.3536(3) 0.4513(3) 0.0488(12) Uani 1 1 d . . . . . Th2 Th 0.51123(2) 0.20388(2) 0.73369(2) 0.04472(8) Uani 1 1 d . . . . . O2 O 0.5945(3) 0.2172(2) 0.6367(2) 0.0443(10) Uani 1 1 d . . . . . N5 N 0.6559(5) 0.1552(4) 0.7548(3) 0.0629(17) Uani 1 1 d . . . . . Si4 Si 0.74265(15) 0.15507(12) 0.70158(10) 0.0611(6) Uani 1 1 d . . . . . C25 C 0.6801(5) 0.1867(4) 0.6239(3) 0.0572(18) Uani 1 1 d . . . . . H25A H 0.7222 0.2151 0.6034 0.069 Uiso 1 1 calc R . . . . H25B H 0.6655 0.1536 0.5926 0.069 Uiso 1 1 calc R . . . . C26 C 0.8467(7) 0.2006(5) 0.7294(5) 0.088(3) Uani 1 1 d . . . . . H26A H 0.8262 0.2378 0.7495 0.131 Uiso 1 1 calc GR . . . . H26B H 0.8824 0.2103 0.6920 0.131 Uiso 1 1 calc GR . . . . H26C H 0.8863 0.1778 0.7616 0.131 Uiso 1 1 calc GR . . . . C27 C 0.7903(8) 0.0794(5) 0.6813(5) 0.088(3) Uani 1 1 d . . . . . C28 C 0.8418(8) 0.0852(6) 0.6182(5) 0.100(3) Uani 1 1 d . . . . . H28A H 0.7982 0.1002 0.5828 0.150 Uiso 1 1 calc GR . . . . H28B H 0.8657 0.0459 0.6062 0.150 Uiso 1 1 calc GR . . . . H28C H 0.8942 0.1133 0.6256 0.150 Uiso 1 1 calc GR . . . . C29 C 0.7060(10) 0.0348(6) 0.6713(6) 0.110(4) Uani 1 1 d . . . . . H29A H 0.6869 0.0219 0.7139 0.165 Uiso 1 1 calc GR . . . . H29B H 0.7249 -0.0002 0.6467 0.165 Uiso 1 1 calc GR . . . . H29C H 0.6534 0.0549 0.6469 0.165 Uiso 1 1 calc GR . . . . C30 C 0.8624(9) 0.0544(6) 0.7351(6) 0.109(4) Uani 1 1 d . . . . . H30A H 0.9223 0.0753 0.7329 0.164 Uiso 1 1 calc GR . . . . H30B H 0.8714 0.0114 0.7280 0.164 Uiso 1 1 calc GR . . . . H30C H 0.8389 0.0608 0.7781 0.164 Uiso 1 1 calc GR . . . . C31 C 0.6753(7) 0.1267(6) 0.8190(4) 0.086(3) Uani 1 1 d . . . . . H31A H 0.7335 0.1028 0.8188 0.103 Uiso 1 1 calc R . . . . H31B H 0.6854 0.1582 0.8529 0.103 Uiso 1 1 calc R . . . . C32 C 0.6002(8) 0.0887(6) 0.8352(6) 0.104(3) Uani 1 1 d . . . . . H32A H 0.6125 0.0748 0.8809 0.125 Uiso 1 1 calc R . . . . H32B H 0.5987 0.0529 0.8066 0.125 Uiso 1 1 calc R . . . . N6 N 0.492(3) 0.2559(18) 0.839(2) 0.066(4) Uani 0.34(3) 1 d . . P B 1 N6A N 0.4874(16) 0.2420(9) 0.8345(10) 0.065(3) Uani 0.66(3) 1 d . . P B 2 Si5 Si 0.5436(14) 0.3183(12) 0.8778(9) 0.075(3) Uani 0.34(3) 1 d . . P B 1 Si5A Si 0.5503(7) 0.2957(6) 0.8807(4) 0.069(2) Uani 0.66(3) 1 d . . P B 2 C33 C 0.619(3) 0.294(2) 0.9499(15) 0.080(7) Uani 0.34(3) 1 d . . P B 1 H33A H 0.6743 0.2730 0.9355 0.121 Uiso 0.34(3) 1 calc GR . P B 1 H33B H 0.5843 0.2670 0.9767 0.121 Uiso 0.34(3) 1 calc GR . P B 1 H33C H 0.6399 0.3292 0.9758 0.121 Uiso 0.34(3) 1 calc GR . P B 1 C33A C 0.6196(16) 0.2622(13) 0.9517(9) 0.096(6) Uani 0.66(3) 1 d . . P B 2 H33D H 0.5777 0.2402 0.9787 0.144 Uiso 0.66(3) 1 calc GR . P B 2 H33E H 0.6513 0.2941 0.9777 0.144 Uiso 0.66(3) 1 calc GR . P B 2 H33F H 0.6663 0.2347 0.9361 0.144 Uiso 0.66(3) 1 calc GR . P B 2 C34 C 0.616(3) 0.354(2) 0.8188(19) 0.083(8) Uani 0.34(3) 1 d . . P B 1 H34A H 0.6150 0.3980 0.8249 0.124 Uiso 0.34(3) 1 calc GR . P B 1 H34B H 0.5914 0.3446 0.7743 0.124 Uiso 0.34(3) 1 calc GR . P B 1 H34C H 0.6808 0.3399 0.8258 0.124 Uiso 0.34(3) 1 calc GR . P B 1 C34A C 0.6289(18) 0.3250(14) 0.8216(11) 0.101(7) Uani 0.66(3) 1 d . . P B 2 H34D H 0.6278 0.2983 0.7837 0.151 Uiso 0.66(3) 1 calc GR . P B 2 H34E H 0.6929 0.3273 0.8422 0.151 Uiso 0.66(3) 1 calc GR . P B 2 H34F H 0.6081 0.3651 0.8074 0.151 Uiso 0.66(3) 1 calc GR . P B 2 C35 C 0.456(2) 0.3751(16) 0.9073(15) 0.087(5) Uani 0.34(3) 1 d . . P B 1 C35A C 0.4779(13) 0.3589(9) 0.9142(8) 0.089(4) Uani 0.66(3) 1 d . . P B 2 C36 C 0.374(3) 0.386(2) 0.8550(18) 0.085(7) Uani 0.34(3) 1 d . . P B 1 H36A H 0.3980 0.4034 0.8157 0.127 Uiso 0.34(3) 1 calc GR . P B 1 H36B H 0.3289 0.4141 0.8722 0.127 Uiso 0.34(3) 1 calc GR . P B 1 H36C H 0.3424 0.3481 0.8439 0.127 Uiso 0.34(3) 1 calc GR . P B 1 C36A C 0.4112(18) 0.3915(11) 0.8632(10) 0.097(5) Uani 0.66(3) 1 d . . P B 2 H36D H 0.4478 0.4100 0.8301 0.145 Uiso 0.66(3) 1 calc GR . P B 2 H36E H 0.3765 0.4226 0.8849 0.145 Uiso 0.66(3) 1 calc GR . P B 2 H36F H 0.3671 0.3626 0.8422 0.145 Uiso 0.66(3) 1 calc GR . P B 2 C37 C 0.517(3) 0.431(2) 0.925(2) 0.101(8) Uani 0.34(3) 1 d . . P B 1 H37A H 0.5783 0.4188 0.9452 0.151 Uiso 0.34(3) 1 calc GR . P B 1 H37B H 0.4859 0.4571 0.9549 0.151 Uiso 0.34(3) 1 calc GR . P B 1 H37C H 0.5269 0.4540 0.8847 0.151 Uiso 0.34(3) 1 calc GR . P B 1 C37A C 0.5469(17) 0.4065(12) 0.9471(10) 0.107(6) Uani 0.66(3) 1 d . . P B 2 H37D H 0.5981 0.3859 0.9724 0.160 Uiso 0.66(3) 1 calc GR . P B 2 H37E H 0.5132 0.4321 0.9761 0.160 Uiso 0.66(3) 1 calc GR . P B 2 H37F H 0.5727 0.4311 0.9132 0.160 Uiso 0.66(3) 1 calc GR . P B 2 C38 C 0.415(3) 0.362(2) 0.9741(17) 0.094(7) Uani 0.34(3) 1 d . . P B 1 H38A H 0.3719 0.3282 0.9693 0.141 Uiso 0.34(3) 1 calc GR . P B 1 H38B H 0.3814 0.3977 0.9879 0.141 Uiso 0.34(3) 1 calc GR . P B 1 H38C H 0.4662 0.3528 1.0069 0.141 Uiso 0.34(3) 1 calc GR . P B 1 C38A C 0.4144(17) 0.3345(11) 0.9668(10) 0.096(5) Uani 0.66(3) 1 d . . P B 2 H38D H 0.3733 0.3030 0.9475 0.144 Uiso 0.66(3) 1 calc GR . P B 2 H38E H 0.3762 0.3672 0.9824 0.144 Uiso 0.66(3) 1 calc GR . P B 2 H38F H 0.4538 0.3179 1.0036 0.144 Uiso 0.66(3) 1 calc GR . P B 2 C39 C 0.4324(7) 0.2026(5) 0.8758(5) 0.083(2) Uani 1 1 d . . . . . H39C H 0.4203 0.2232 0.9170 0.100 Uiso 0.66(3) 1 calc R . P B 2 H39D H 0.3716 0.1921 0.8524 0.100 Uiso 0.66(3) 1 calc R . P B 2 H39A H 0.4117 0.2186 0.9173 0.100 Uiso 0.34(3) 1 calc R . P B 1 H39B H 0.3758 0.1919 0.8475 0.100 Uiso 0.34(3) 1 calc R . P B 1 C40 C 0.4889(9) 0.1481(6) 0.8895(6) 0.102(3) Uani 1 1 d . . . . . H40A H 0.5490 0.1590 0.9137 0.123 Uiso 1 1 calc R . . . . H40B H 0.4550 0.1204 0.9171 0.123 Uiso 1 1 calc R . . . . N7 N 0.3981(5) 0.1307(3) 0.7049(4) 0.0630(16) Uani 1 1 d . . . . . Si6 Si 0.30049(15) 0.13529(9) 0.65142(10) 0.0521(4) Uani 1 1 d . . . . . C41 C 0.3195(6) 0.1983(3) 0.5942(4) 0.0541(17) Uani 1 1 d . . . . . H41A H 0.3310 0.2353 0.6192 0.081 Uiso 1 1 calc GR . . . . H41B H 0.2637 0.2032 0.5639 0.081 Uiso 1 1 calc GR . . . . H41C H 0.3737 0.1894 0.5694 0.081 Uiso 1 1 calc GR . . . . C42 C 0.2826(7) 0.0656(4) 0.6006(5) 0.078(3) Uani 1 1 d . . . . . H42A H 0.3409 0.0555 0.5811 0.118 Uiso 1 1 calc GR . . . . H42B H 0.2329 0.0726 0.5659 0.118 Uiso 1 1 calc GR . . . . H42C H 0.2646 0.0325 0.6283 0.118 Uiso 1 1 calc GR . . . . C43 C 0.1879(6) 0.1497(4) 0.6919(4) 0.0642(19) Uani 1 1 d . . . . . C44 C 0.1062(7) 0.1593(6) 0.6390(5) 0.090(3) Uani 1 1 d . . . . . H44A H 0.1189 0.1947 0.6128 0.134 Uiso 1 1 calc GR . . . . H44B H 0.0478 0.1652 0.6601 0.134 Uiso 1 1 calc GR . . . . H44C H 0.1003 0.1240 0.6106 0.134 Uiso 1 1 calc GR . . . . C45 C 0.1648(8) 0.0967(5) 0.7347(6) 0.092(3) Uani 1 1 d . . . . . H45A H 0.1499 0.0616 0.7071 0.138 Uiso 1 1 calc GR . . . . H45B H 0.1108 0.1067 0.7592 0.138 Uiso 1 1 calc GR . . . . H45C H 0.2188 0.0877 0.7653 0.138 Uiso 1 1 calc GR . . . . C46 C 0.1968(8) 0.2062(5) 0.7351(5) 0.083(3) Uani 1 1 d . . . . . H46A H 0.2474 0.2005 0.7695 0.124 Uiso 1 1 calc GR . . . . H46B H 0.1377 0.2131 0.7551 0.124 Uiso 1 1 calc GR . . . . H46C H 0.2110 0.2409 0.7083 0.124 Uiso 1 1 calc GR . . . . C47 C 0.4176(8) 0.0712(5) 0.7345(6) 0.092(3) Uani 1 1 d . . . . . H47A H 0.4734 0.0536 0.7161 0.110 Uiso 1 1 calc R . . . . H47B H 0.3638 0.0442 0.7236 0.110 Uiso 1 1 calc R . . . . C48 C 0.4347(8) 0.0764(5) 0.8078(6) 0.098(3) Uani 1 1 d . . . . . H48A H 0.3757 0.0886 0.8262 0.118 Uiso 1 1 calc R . . . . H48B H 0.4524 0.0365 0.8259 0.118 Uiso 1 1 calc R . . . . N8 N 0.5069(6) 0.1187(4) 0.8282(4) 0.086(2) Uani 1 1 d . . . . . 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 0.04739(13) 0.04107(12) 0.02048(11) 0.00079(7) -0.00071(8) -0.00295(8) O1 0.057(3) 0.056(3) 0.028(2) 0.0065(18) 0.0049(19) 0.008(2) N1 0.075(4) 0.043(3) 0.036(3) 0.003(2) 0.005(2) 0.008(3) Si1 0.0775(14) 0.0451(10) 0.0398(10) -0.0028(8) 0.0063(9) 0.0008(9) C1 0.060(4) 0.053(3) 0.033(3) 0.003(3) 0.005(3) 0.005(3) C2 0.109(7) 0.055(4) 0.062(5) -0.016(4) 0.012(5) -0.017(4) C3 0.080(4) 0.061(4) 0.060(4) 0.004(3) 0.006(3) 0.015(3) C4 0.083(6) 0.080(6) 0.070(5) 0.008(4) 0.018(4) 0.015(5) C5 0.112(8) 0.075(5) 0.079(6) 0.016(4) 0.032(5) 0.034(5) C6 0.068(5) 0.085(5) 0.078(6) -0.008(4) 0.000(4) 0.014(4) C7 0.113(6) 0.055(4) 0.048(4) 0.013(3) 0.014(4) 0.015(4) C8 0.111(6) 0.052(3) 0.037(3) 0.004(3) 0.009(4) 0.002(3) N2 0.054(3) 0.044(2) 0.029(2) -0.0019(19) -0.003(2) -0.004(2) Si2 0.048(2) 0.0400(17) 0.0334(18) -0.0042(13) 0.0020(15) -0.0036(14) Si2A 0.050(2) 0.053(2) 0.0342(19) -0.0036(15) 0.0047(16) 0.0016(17) C9 0.061(6) 0.054(8) 0.060(9) -0.008(7) -0.003(6) -0.010(6) C9A 0.048(6) 0.076(10) 0.042(8) -0.003(7) 0.008(5) 0.009(5) C10 0.072(9) 0.054(7) 0.053(7) 0.002(6) -0.003(6) 0.004(7) C10A 0.077(10) 0.060(9) 0.033(6) -0.003(5) 0.011(6) 0.013(8) C11 0.081(7) 0.066(6) 0.060(6) -0.005(5) 0.030(5) 0.006(5) C11A 0.069(6) 0.051(5) 0.045(6) -0.004(4) 0.008(5) 0.001(4) C12 0.113(12) 0.073(7) 0.088(11) -0.015(7) 0.050(9) 0.005(7) C12A 0.086(10) 0.066(9) 0.048(6) -0.002(6) 0.007(6) 0.001(8) C13 0.115(13) 0.079(11) 0.062(8) -0.004(7) 0.025(8) 0.004(10) C13A 0.068(7) 0.056(9) 0.064(10) -0.006(7) 0.009(6) -0.005(5) C14 0.082(7) 0.098(11) 0.097(11) -0.013(9) 0.033(7) 0.004(7) C14A 0.099(11) 0.050(7) 0.055(8) -0.003(6) 0.017(7) 0.006(7) C15 0.059(4) 0.054(3) 0.059(4) -0.004(3) -0.015(3) 0.000(3) C16 0.092(5) 0.056(4) 0.044(4) 0.001(3) -0.022(3) -0.004(3) N3 0.064(3) 0.070(4) 0.028(2) 0.002(2) 0.000(2) -0.021(3) Si3 0.0668(13) 0.0598(12) 0.0458(11) -0.0067(9) -0.0016(9) 0.0010(10) C17 0.093(6) 0.052(4) 0.069(6) -0.015(4) 0.000(5) 0.002(4) C18 0.088(6) 0.109(7) 0.037(4) -0.002(4) -0.004(4) -0.035(5) C19 0.068(4) 0.083(5) 0.061(4) -0.011(4) -0.006(3) -0.004(3) C20 0.073(6) 0.140(9) 0.064(5) -0.006(5) -0.012(4) -0.015(6) C21 0.059(5) 0.095(5) 0.066(5) -0.007(4) 0.002(4) 0.010(4) C22 0.059(5) 0.093(6) 0.060(5) -0.011(4) 0.002(4) -0.010(4) C23 0.077(5) 0.095(6) 0.033(3) 0.001(3) 0.003(3) -0.021(4) C24 0.085(4) 0.082(5) 0.035(3) 0.006(3) 0.002(3) -0.008(4) N4 0.071(3) 0.047(3) 0.027(2) 0.000(2) -0.002(2) -0.005(2) Th2 0.04082(13) 0.06333(16) 0.02977(12) 0.01516(9) 0.00116(9) -0.00033(10) O2 0.046(2) 0.058(3) 0.028(2) 0.0065(18) -0.0011(17) 0.0052(19) N5 0.054(3) 0.096(5) 0.038(3) 0.023(3) -0.001(2) 0.014(3) Si4 0.0516(11) 0.0914(16) 0.0391(10) 0.0146(10) -0.0047(9) 0.0089(10) C25 0.055(4) 0.083(5) 0.033(3) 0.009(3) -0.003(3) 0.018(3) C26 0.062(5) 0.143(8) 0.055(5) 0.020(5) -0.016(4) -0.019(5) C27 0.094(6) 0.105(5) 0.063(5) 0.019(4) -0.003(4) 0.036(4) C28 0.101(7) 0.128(8) 0.071(5) 0.015(5) 0.009(5) 0.050(6) C29 0.131(8) 0.103(7) 0.095(8) 0.004(6) 0.001(6) 0.015(6) C30 0.116(8) 0.134(9) 0.075(6) 0.028(6) -0.006(5) 0.057(7) C31 0.066(4) 0.138(7) 0.053(4) 0.046(5) 0.002(3) 0.025(4) C32 0.079(5) 0.146(7) 0.087(6) 0.063(5) 0.004(4) 0.014(4) N6 0.055(7) 0.115(7) 0.029(6) 0.002(5) 0.003(5) -0.008(6) N6A 0.058(5) 0.109(7) 0.028(4) 0.006(4) 0.002(4) -0.005(5) Si5 0.063(5) 0.125(8) 0.038(5) -0.010(6) 0.003(4) -0.016(6) Si5A 0.066(3) 0.113(5) 0.0271(19) 0.006(3) 0.0098(17) -0.018(4) C33 0.065(11) 0.131(17) 0.044(9) 0.000(10) 0.002(8) -0.027(12) C33A 0.087(9) 0.148(15) 0.051(7) 0.006(9) -0.014(6) -0.014(10) C34 0.073(13) 0.126(17) 0.051(11) -0.006(12) 0.013(9) -0.017(13) C34A 0.099(11) 0.144(16) 0.061(8) 0.002(10) 0.022(8) -0.034(11) C35 0.082(9) 0.132(10) 0.046(8) -0.017(7) 0.002(7) -0.008(8) C35A 0.097(7) 0.129(8) 0.041(5) -0.013(5) 0.003(5) -0.008(6) C36 0.079(11) 0.128(16) 0.047(10) -0.015(10) 0.008(9) -0.009(11) C36A 0.110(11) 0.123(10) 0.055(7) -0.018(7) -0.004(8) -0.005(9) C37 0.091(14) 0.137(12) 0.074(15) -0.023(10) 0.000(11) -0.014(11) C37A 0.127(11) 0.137(11) 0.055(9) -0.013(8) 0.000(8) -0.023(9) C38 0.087(13) 0.142(17) 0.052(9) -0.019(10) 0.004(8) -0.013(13) C38A 0.111(10) 0.123(12) 0.055(7) -0.017(8) 0.021(7) 0.002(9) C39 0.070(5) 0.135(6) 0.046(4) 0.008(4) 0.014(4) -0.012(4) C40 0.098(6) 0.138(6) 0.073(5) 0.042(4) 0.020(5) -0.007(5) N7 0.057(3) 0.056(3) 0.074(4) 0.018(3) -0.001(3) -0.003(3) Si6 0.0518(11) 0.0544(11) 0.0512(11) -0.0003(9) 0.0113(9) -0.0039(8) C41 0.058(4) 0.061(4) 0.044(4) -0.004(3) 0.012(3) -0.011(3) C42 0.074(6) 0.071(5) 0.093(6) -0.014(4) 0.025(5) -0.013(4) C43 0.052(4) 0.088(5) 0.056(4) 0.004(3) 0.019(3) -0.002(3) C44 0.056(5) 0.136(9) 0.078(6) 0.006(5) 0.014(4) 0.003(5) C45 0.091(7) 0.102(6) 0.088(7) 0.013(5) 0.042(5) -0.007(5) C46 0.079(6) 0.100(6) 0.072(6) -0.008(4) 0.030(5) 0.007(5) C47 0.095(6) 0.073(5) 0.106(6) 0.037(4) 0.002(5) -0.005(4) C48 0.096(6) 0.105(6) 0.094(5) 0.055(5) 0.008(4) -0.004(5) N8 0.072(4) 0.117(5) 0.071(4) 0.049(4) 0.013(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 O1 2.425(5) . ? Th1 N1 2.366(6) . ? Th1 N2 2.341(5) . ? Th1 N3 2.343(6) . ? Th1 N4 2.656(5) . ? Th1 O2 2.387(4) . ? O1 C1 1.454(8) . ? O1 Th2 2.369(4) . ? N1 Si1 1.711(6) . ? N1 C7 1.467(9) . ? Si1 C1 1.898(7) . ? Si1 C2 1.890(8) . ? Si1 C3 1.911(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.540(13) . ? C3 C5 1.550(12) . ? C3 C6 1.536(13) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.456(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 N4 1.452(10) . ? N2 Si2 1.727(6) . ? N2 Si2A 1.781(7) . ? N2 C15 1.471(9) . ? Si2 C9 1.891(12) . ? Si2 C10 1.885(12) . ? Si2 C11 1.894(14) . ? Si2A C9A 1.895(12) . ? Si2A C10A 1.898(13) . ? Si2A C11A 1.889(14) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11 C12 1.534(14) . ? C11 C13 1.523(15) . ? C11 C14 1.524(15) . ? C11A C12A 1.530(14) . ? C11A C13A 1.533(14) . ? C11A C14A 1.550(14) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.507(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N4 1.485(9) . ? N3 Si3 1.736(6) . ? N3 C23 1.490(9) . ? Si3 C17 1.863(9) . ? Si3 C18 1.864(9) . ? Si3 C19 1.889(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.565(12) . ? C19 C21 1.598(13) . ? C19 C22 1.574(13) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.493(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 N4 1.434(11) . ? Th2 O2 2.415(5) . ? Th2 N5 2.350(6) . ? Th2 N6 2.49(4) . ? Th2 N6A 2.288(19) . ? Th2 N7 2.344(7) . ? O2 C25 1.444(9) . ? N5 Si4 1.716(7) . ? N5 C31 1.470(9) . ? Si4 C25 1.905(7) . ? Si4 C26 1.857(10) . ? Si4 C27 1.881(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.543(15) . ? C27 C29 1.565(17) . ? C27 C30 1.556(13) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.429(15) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 N8 1.492(13) . ? N6 Si5 1.741(17) . ? N6 C39 1.67(4) . ? N6A Si5A 1.736(12) . ? N6A C39 1.49(2) . ? Si5 C33 1.850(16) . ? Si5 C34 1.841(16) . ? Si5 C35 1.91(2) . ? Si5A C33A 1.857(13) . ? Si5A C34A 1.837(12) . ? Si5A C35A 1.910(16) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C35 C36 1.553(17) . ? C35 C37 1.560(17) . ? C35 C38 1.557(16) . ? C35A C36A 1.544(15) . ? C35A C37A 1.567(14) . ? C35A C38A 1.563(14) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C37A H37D 0.9800 . ? C37A H37E 0.9800 . ? C37A H37F 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39 H39C 0.9900 . ? C39 H39D 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.475(16) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 N8 1.461(15) . ? N7 Si6 1.714(7) . ? N7 C47 1.478(11) . ? Si6 C41 1.865(8) . ? Si6 C42 1.879(9) . ? Si6 C43 1.897(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.549(13) . ? C43 C45 1.526(13) . ? C43 C46 1.541(13) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.511(16) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C48 N8 1.438(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Th1 N4 140.29(18) . . ? N1 Th1 O1 72.86(18) . . ? N1 Th1 N4 67.6(2) . . ? N1 Th1 O2 135.56(18) . . ? N2 Th1 O1 124.41(19) . . ? N2 Th1 N1 108.4(2) . . ? N2 Th1 N3 109.8(2) . . ? N2 Th1 N4 67.15(18) . . ? N2 Th1 O2 99.14(18) . . ? N3 Th1 O1 125.04(18) . . ? N3 Th1 N1 99.5(2) . . ? N3 Th1 N4 67.0(2) . . ? N3 Th1 O2 103.1(2) . . ? O2 Th1 O1 62.80(16) . . ? O2 Th1 N4 156.81(18) . . ? C1 O1 Th1 126.5(4) . . ? C1 O1 Th2 115.7(4) . . ? Th2 O1 Th1 116.21(19) . . ? Si1 N1 Th1 123.9(3) . . ? C7 N1 Th1 120.8(5) . . ? C7 N1 Si1 115.0(5) . . ? N1 Si1 C1 102.7(3) . . ? N1 Si1 C2 112.6(4) . . ? N1 Si1 C3 115.9(4) . . ? C1 Si1 C3 107.0(4) . . ? C2 Si1 C1 110.8(4) . . ? C2 Si1 C3 107.6(4) . . ? O1 C1 Si1 110.5(4) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Si1 108.1(6) . . ? C4 C3 C5 106.7(7) . . ? C5 C3 Si1 112.1(7) . . ? C6 C3 Si1 109.3(6) . . ? C6 C3 C4 110.2(8) . . ? C6 C3 C5 110.4(8) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 108.7 . . ? N1 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C8 C7 N1 114.0(8) . . ? C8 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C7 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N4 C8 C7 113.0(7) . . ? N4 C8 H8A 109.0 . . ? N4 C8 H8B 109.0 . . ? Si2 N2 Th1 141.7(3) . . ? Si2A N2 Th1 135.4(3) . . ? C15 N2 Th1 102.4(4) . . ? C15 N2 Si2 111.6(4) . . ? C15 N2 Si2A 117.6(5) . . ? N2 Si2 C9 115.4(6) . . ? N2 Si2 C10 109.5(6) . . ? N2 Si2 C11 112.0(5) . . ? C9 Si2 C11 105.8(8) . . ? C10 Si2 C9 106.5(9) . . ? C10 Si2 C11 107.2(8) . . ? N2 Si2A C9A 111.8(6) . . ? N2 Si2A C10A 111.6(6) . . ? N2 Si2A C11A 111.6(5) . . ? C9A Si2A C10A 105.6(10) . . ? C11A Si2A C9A 108.8(7) . . ? C11A Si2A C10A 107.2(8) . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2A C9A H9AA 109.5 . . ? Si2A C9A H9AB 109.5 . . ? Si2A C9A H9AC 109.5 . . ? H9AA C9A H9AB 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2A C10A H10D 109.5 . . ? Si2A C10A H10E 109.5 . . ? Si2A C10A H10F 109.5 . . ? H10D C10A H10E 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C12 C11 Si2 111.3(11) . . ? C13 C11 Si2 112.8(13) . . ? C13 C11 C12 104.2(17) . . ? C13 C11 C14 110.3(19) . . ? C14 C11 Si2 108.0(11) . . ? C14 C11 C12 110.3(17) . . ? C12A C11A Si2A 111.2(11) . . ? C12A C11A C13A 108.5(15) . . ? C12A C11A C14A 107.9(14) . . ? C13A C11A Si2A 110.6(10) . . ? C13A C11A C14A 107.9(14) . . ? C14A C11A Si2A 110.7(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12E 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11A C13A H13D 109.5 . . ? C11A C13A H13E 109.5 . . ? C11A C13A H13F 109.5 . . ? H13D C13A H13E 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11A C14A H14D 109.5 . . ? C11A C14A H14E 109.5 . . ? C11A C14A H14F 109.5 . . ? H14D C14A H14E 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? Th1 C15 H15A 74.5 . . ? Th1 C15 H15B 155.4 . . ? N2 C15 Th1 49.2(3) . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? N2 C15 C16 110.9(7) . . ? H15A C15 H15B 108.0 . . ? C16 C15 Th1 91.9(4) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C15 C16 H16A 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? N4 C16 C15 109.6(6) . . ? N4 C16 H16A 109.8 . . ? N4 C16 H16B 109.8 . . ? Si3 N3 Th1 120.6(3) . . ? C23 N3 Th1 121.2(5) . . ? C23 N3 Si3 113.5(5) . . ? N3 Si3 C17 116.0(4) . . ? N3 Si3 C18 104.6(4) . . ? N3 Si3 C19 112.6(4) . . ? C17 Si3 C18 109.1(5) . . ? C17 Si3 C19 105.7(5) . . ? C18 Si3 C19 108.7(5) . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 Si3 108.9(7) . . ? C20 C19 C21 110.1(9) . . ? C20 C19 C22 105.8(8) . . ? C21 C19 Si3 109.8(6) . . ? C22 C19 Si3 109.2(6) . . ? C22 C19 C21 112.9(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 109.2 . . ? N3 C23 H23B 109.2 . . ? N3 C23 C24 112.0(7) . . ? H23A C23 H23B 107.9 . . ? C24 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C23 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? N4 C24 C23 113.5(7) . . ? N4 C24 H24A 108.9 . . ? N4 C24 H24B 108.9 . . ? C8 N4 Th1 107.5(4) . . ? C8 N4 C16 112.7(7) . . ? C16 N4 Th1 108.0(4) . . ? C24 N4 Th1 104.6(5) . . ? C24 N4 C8 114.8(7) . . ? C24 N4 C16 108.6(6) . . ? O1 Th2 O2 63.20(16) . . ? O1 Th2 N6 94.0(12) . . ? O2 Th2 N6 139.0(9) . . ? N5 Th2 O1 129.8(2) . . ? N5 Th2 O2 74.08(19) . . ? N5 Th2 N6 102.2(12) . . ? N6A Th2 O1 99.1(6) . . ? N6A Th2 O2 144.8(5) . . ? N6A Th2 N5 101.2(7) . . ? N6A Th2 N7 109.8(5) . . ? N7 Th2 O1 107.4(2) . . ? N7 Th2 O2 104.7(2) . . ? N7 Th2 N5 107.9(3) . . ? N7 Th2 N6 115.0(9) . . ? Th1 O2 Th2 115.91(19) . . ? C25 O2 Th1 119.0(4) . . ? C25 O2 Th2 124.9(4) . . ? Si4 N5 Th2 123.6(3) . . ? C31 N5 Th2 118.0(5) . . ? C31 N5 Si4 118.3(6) . . ? N5 Si4 C25 102.5(3) . . ? N5 Si4 C26 113.9(5) . . ? N5 Si4 C27 115.8(5) . . ? C26 Si4 C25 111.7(4) . . ? C26 Si4 C27 105.3(6) . . ? C27 Si4 C25 107.6(4) . . ? O2 C25 Si4 111.9(5) . . ? O2 C25 H25A 109.2 . . ? O2 C25 H25B 109.2 . . ? Si4 C25 H25A 109.2 . . ? Si4 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Si4 108.3(8) . . ? C28 C27 C29 110.9(11) . . ? C28 C27 C30 107.0(9) . . ? C29 C27 Si4 108.1(8) . . ? C30 C27 Si4 113.4(8) . . ? C30 C27 C29 109.2(10) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 H31A 109.3 . . ? N5 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C32 C31 N5 111.7(8) . . ? C32 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? C31 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C31 C32 N8 113.3(10) . . ? H32A C32 H32B 107.7 . . ? N8 C32 H32A 108.9 . . ? N8 C32 H32B 108.9 . . ? Si5 N6 Th2 134(2) . . ? C39 N6 Th2 98.9(13) . . ? C39 N6 Si5 125(3) . . ? Si5A N6A Th2 130.0(12) . . ? C39 N6A Th2 114.7(9) . . ? C39 N6A Si5A 111.9(12) . . ? N6 Si5 C33 110(2) . . ? N6 Si5 C34 107(2) . . ? N6 Si5 C35 114(2) . . ? C33 Si5 C35 107.4(17) . . ? C34 Si5 C33 109(2) . . ? C34 Si5 C35 109.6(18) . . ? N6A Si5A C33A 112.0(11) . . ? N6A Si5A C34A 101.8(11) . . ? N6A Si5A C35A 115.7(10) . . ? C33A Si5A C35A 106.6(9) . . ? C34A Si5A C33A 110.1(12) . . ? C34A Si5A C35A 110.6(10) . . ? Si5 C33 H33A 109.5 . . ? Si5 C33 H33B 109.5 . . ? Si5 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si5A C33A H33D 109.5 . . ? Si5A C33A H33E 109.5 . . ? Si5A C33A H33F 109.5 . . ? H33D C33A H33E 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? Si5 C34 H34A 109.5 . . ? Si5 C34 H34B 109.5 . . ? Si5 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si5A C34A H34D 109.5 . . ? Si5A C34A H34E 109.5 . . ? Si5A C34A H34F 109.5 . . ? H34D C34A H34E 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C36 C35 Si5 111(2) . . ? C36 C35 C37 115(3) . . ? C36 C35 C38 109(3) . . ? C37 C35 Si5 104(2) . . ? C38 C35 Si5 117(3) . . ? C38 C35 C37 101(3) . . ? C36A C35A Si5A 115.3(12) . . ? C36A C35A C37A 108.1(15) . . ? C36A C35A C38A 105.7(17) . . ? C37A C35A Si5A 108.3(13) . . ? C38A C35A Si5A 110.6(13) . . ? C38A C35A C37A 108.7(15) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35A C36A H36D 109.5 . . ? C35A C36A H36E 109.5 . . ? C35A C36A H36F 109.5 . . ? H36D C36A H36E 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35A C37A H37D 109.5 . . ? C35A C37A H37E 109.5 . . ? C35A C37A H37F 109.5 . . ? H37D C37A H37E 109.5 . . ? H37D C37A H37F 109.5 . . ? H37E C37A H37F 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35A C38A H38D 109.5 . . ? C35A C38A H38E 109.5 . . ? C35A C38A H38F 109.5 . . ? H38D C38A H38E 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? N6 C39 H39A 109.1 . . ? N6 C39 H39B 109.1 . . ? N6A C39 H39C 110.4 . . ? N6A C39 H39D 110.4 . . ? H39C C39 H39D 108.6 . . ? H39A C39 H39B 107.8 . . ? C40 C39 N6 112(2) . . ? C40 C39 N6A 106.8(12) . . ? C40 C39 H39C 110.4 . . ? C40 C39 H39D 110.4 . . ? C40 C39 H39A 109.1 . . ? C40 C39 H39B 109.1 . . ? C39 C40 H40A 109.7 . . ? C39 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? N8 C40 C39 109.6(9) . . ? N8 C40 H40A 109.7 . . ? N8 C40 H40B 109.7 . . ? Si6 N7 Th2 129.4(3) . . ? C47 N7 Th2 114.6(6) . . ? C47 N7 Si6 115.9(6) . . ? N7 Si6 C41 107.3(4) . . ? N7 Si6 C42 112.2(4) . . ? N7 Si6 C43 114.1(4) . . ? C41 Si6 C42 107.1(4) . . ? C41 Si6 C43 108.5(4) . . ? C42 Si6 C43 107.4(4) . . ? Si6 C41 H41A 109.5 . . ? Si6 C41 H41B 109.5 . . ? Si6 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si6 C42 H42A 109.5 . . ? Si6 C42 H42B 109.5 . . ? Si6 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 Si6 109.8(6) . . ? C45 C43 Si6 110.4(7) . . ? C45 C43 C44 109.0(8) . . ? C45 C43 C46 108.3(8) . . ? C46 C43 Si6 110.8(6) . . ? C46 C43 C44 108.5(9) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N7 C47 H47A 109.5 . . ? N7 C47 H47B 109.5 . . ? N7 C47 C48 110.6(10) . . ? H47A C47 H47B 108.1 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? C47 C48 H48A 108.9 . . ? C47 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? N8 C48 C47 113.5(9) . . ? N8 C48 H48A 108.9 . . ? N8 C48 H48B 108.9 . . ? C32 N8 Th2 108.3(5) . . ? C40 N8 Th2 108.4(7) . . ? C40 N8 C32 109.5(9) . . ? C48 N8 Th2 107.8(6) . . ? C48 N8 C32 110.6(10) . . ? C48 N8 C40 112.1(9) . . ? 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 _geom_torsion_publ_flag Th1 O1 C1 Si1 -17.3(7) . . . . ? Th1 N1 Si1 C1 -16.5(5) . . . . ? Th1 N1 Si1 C2 102.7(5) . . . . ? Th1 N1 Si1 C3 -132.8(4) . . . . ? Th1 N1 C7 C8 -19.2(11) . . . . ? Th1 N2 Si2 C9 125.6(8) . . . . ? Th1 N2 Si2 C10 5.4(9) . . . . ? Th1 N2 Si2 C11 -113.3(7) . . . . ? Th1 N2 Si2A C9A -11.3(8) . . . . ? Th1 N2 Si2A C10A -129.3(9) . . . . ? Th1 N2 Si2A C11A 110.8(6) . . . . ? Th1 N2 C15 C16 73.6(7) . . . . ? Th1 C15 C16 N4 -2.1(7) . . . . ? Th1 N3 Si3 C17 -99.0(5) . . . . ? Th1 N3 Si3 C18 21.3(6) . . . . ? Th1 N3 Si3 C19 139.1(4) . . . . ? Th1 N3 C23 C24 -1.3(11) . . . . ? Th1 O2 C25 Si4 154.9(3) . . . . ? N1 Si1 C1 O1 19.2(6) . . . . ? N1 C7 C8 N4 44.1(11) . . . . ? Si1 N1 C7 C8 154.2(7) . . . . ? C2 Si1 C1 O1 -101.3(6) . . . . ? C3 Si1 C1 O1 141.6(5) . . . . ? C7 N1 Si1 C1 170.3(6) . . . . ? C7 N1 Si1 C2 -70.4(7) . . . . ? C7 N1 Si1 C3 54.0(7) . . . . ? C7 C8 N4 Th1 -44.2(9) . . . . ? C7 C8 N4 C16 74.7(9) . . . . ? C7 C8 N4 C24 -160.1(8) . . . . ? N2 Si2 C11 C12 177.8(14) . . . . ? N2 Si2 C11 C13 -65.6(16) . . . . ? N2 Si2 C11 C14 56.5(14) . . . . ? N2 Si2A C11A C12A -69.9(12) . . . . ? N2 Si2A C11A C13A 50.7(12) . . . . ? N2 Si2A C11A C14A 170.2(11) . . . . ? N2 C15 C16 N4 -48.7(9) . . . . ? Si2 N2 C15 Th1 162.0(5) . . . . ? Si2 N2 C15 C16 -124.4(6) . . . . ? Si2A N2 C15 Th1 -159.6(6) . . . . ? Si2A N2 C15 C16 -86.0(7) . . . . ? C9 Si2 C11 C12 -55.7(16) . . . . ? C9 Si2 C11 C13 60.9(16) . . . . ? C9 Si2 C11 C14 -177.0(13) . . . . ? C9A Si2A C11A C12A 53.9(14) . . . . ? C9A Si2A C11A C13A 174.5(11) . . . . ? C9A Si2A C11A C14A -66.0(13) . . . . ? C10 Si2 C11 C12 57.7(16) . . . . ? C10 Si2 C11 C13 174.3(15) . . . . ? C10 Si2 C11 C14 -63.6(14) . . . . ? C10A Si2A C11A C12A 167.6(13) . . . . ? C10A Si2A C11A C13A -71.7(13) . . . . ? C10A Si2A C11A C14A 47.7(14) . . . . ? C15 N2 Si2 C9 -25.3(9) . . . . ? C15 N2 Si2 C10 -145.5(8) . . . . ? C15 N2 Si2 C11 95.8(7) . . . . ? C15 N2 Si2A C9A 139.7(8) . . . . ? C15 N2 Si2A C10A 21.7(11) . . . . ? C15 N2 Si2A C11A -98.2(7) . . . . ? C15 C16 N4 Th1 2.5(8) . . . . ? C15 C16 N4 C8 -116.1(8) . . . . ? C15 C16 N4 C24 115.4(8) . . . . ? N3 Si3 C19 C20 -157.7(7) . . . . ? N3 Si3 C19 C21 -37.0(8) . . . . ? N3 Si3 C19 C22 87.2(6) . . . . ? N3 C23 C24 N4 38.6(11) . . . . ? Si3 N3 C23 C24 -156.8(7) . . . . ? C17 Si3 C19 C20 74.7(8) . . . . ? C17 Si3 C19 C21 -164.6(6) . . . . ? C17 Si3 C19 C22 -40.4(7) . . . . ? C18 Si3 C19 C20 -42.3(9) . . . . ? C18 Si3 C19 C21 78.4(7) . . . . ? C18 Si3 C19 C22 -157.4(6) . . . . ? C23 N3 Si3 C17 56.7(8) . . . . ? C23 N3 Si3 C18 176.9(7) . . . . ? C23 N3 Si3 C19 -65.2(7) . . . . ? C23 C24 N4 Th1 -50.9(8) . . . . ? C23 C24 N4 C8 66.7(9) . . . . ? C23 C24 N4 C16 -166.0(7) . . . . ? Th2 O1 C1 Si1 177.5(3) . . . . ? Th2 O2 C25 Si4 -19.1(8) . . . . ? Th2 N5 Si4 C25 -11.3(6) . . . . ? Th2 N5 Si4 C26 109.5(5) . . . . ? Th2 N5 Si4 C27 -128.2(5) . . . . ? Th2 N5 C31 C32 50.2(13) . . . . ? Th2 N6 Si5 C33 -110(4) . . . . ? Th2 N6 Si5 C34 8(4) . . . . ? Th2 N6 Si5 C35 130(3) . . . . ? Th2 N6 C39 C40 65.9(19) . . . . ? Th2 N6A Si5A C33A -107.4(16) . . . . ? Th2 N6A Si5A C34A 10.2(19) . . . . ? Th2 N6A Si5A C35A 130.1(14) . . . . ? Th2 N6A C39 C40 64.7(15) . . . . ? Th2 N7 Si6 C41 21.5(6) . . . . ? Th2 N7 Si6 C42 138.9(5) . . . . ? Th2 N7 Si6 C43 -98.7(6) . . . . ? Th2 N7 C47 C48 53.4(11) . . . . ? N5 Si4 C27 C28 161.9(7) . . . . ? N5 Si4 C27 C29 41.7(8) . . . . ? N5 Si4 C27 C30 -79.5(10) . . . . ? N5 C31 C32 N8 -51.3(15) . . . . ? Si4 N5 C31 C32 -133.8(9) . . . . ? C25 Si4 C27 C28 48.0(9) . . . . ? C25 Si4 C27 C29 -72.1(8) . . . . ? C25 Si4 C27 C30 166.6(9) . . . . ? C26 Si4 C27 C28 -71.3(9) . . . . ? C26 Si4 C27 C29 168.5(7) . . . . ? C26 Si4 C27 C30 47.3(10) . . . . ? C31 N5 Si4 C25 172.9(8) . . . . ? C31 N5 Si4 C26 -66.2(9) . . . . ? C31 N5 Si4 C27 56.1(9) . . . . ? C31 C32 N8 Th2 28.9(13) . . . . ? C31 C32 N8 C40 -89.1(12) . . . . ? C31 C32 N8 C48 146.8(10) . . . . ? N6 C39 C40 N8 -68.1(17) . . . . ? N6A C39 C40 N8 -59.5(13) . . . . ? Si5 N6 C39 C40 -101(3) . . . . ? Si5A N6A C39 C40 -96.6(15) . . . . ? C39 N6 Si5 C33 52(4) . . . . ? C39 N6 Si5 C34 170(3) . . . . ? C39 N6 Si5 C35 -68(4) . . . . ? C39 N6A Si5A C33A 50.2(19) . . . . ? C39 N6A Si5A C34A 167.8(16) . . . . ? C39 N6A Si5A C35A -72.2(17) . . . . ? C39 C40 N8 Th2 29.7(11) . . . . ? C39 C40 N8 C32 147.7(9) . . . . ? C39 C40 N8 C48 -89.1(11) . . . . ? N7 Si6 C43 C44 174.4(7) . . . . ? N7 Si6 C43 C45 -65.4(8) . . . . ? N7 Si6 C43 C46 54.6(8) . . . . ? N7 C47 C48 N8 -54.3(13) . . . . ? Si6 N7 C47 C48 -130.2(8) . . . . ? C41 Si6 C43 C44 54.8(8) . . . . ? C41 Si6 C43 C45 175.1(7) . . . . ? C41 Si6 C43 C46 -64.9(7) . . . . ? C42 Si6 C43 C44 -60.6(8) . . . . ? C42 Si6 C43 C45 59.6(8) . . . . ? C42 Si6 C43 C46 179.6(7) . . . . ? C47 N7 Si6 C41 -154.2(7) . . . . ? C47 N7 Si6 C42 -36.9(9) . . . . ? C47 N7 Si6 C43 85.5(8) . . . . ? C47 C48 N8 Th2 28.4(12) . . . . ? C47 C48 N8 C32 -89.8(11) . . . . ? C47 C48 N8 C40 147.6(10) . . . . ? _shelx_SHELXL_version_number '2014/7' 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 0 4 0.0476 9.0010 -0.0132 4.0155 1.0375 0.0465 -0.0060 7 -2 -9 0.0689 6.9985 -2.0184 -8.9942 0.4809 0.0626 0.8574 0 -1 -13 0.0664 -0.0018 -1.0078 -13.0078 -0.3466 -0.0504 0.9164 -6 0 -9 0.0572 -6.0013 0.0054 -9.0146 -0.8591 -0.0890 0.4466 -8 2 8 0.0761 -7.9987 2.0196 7.9921 -0.6109 -0.0728 -0.8179 1 14 -2 0.0197 1.0076 14.0099 -2.0138 0.0926 -0.9778 0.0600 -1 14 4 0.0374 -0.9919 14.0165 3.9874 0.0441 -0.9251 -0.4200 0 -14 0 0.0512 -0.0077 -14.0126 0.0139 -0.0420 0.9606 0.1101 3 1 12 0.0673 3.0019 1.0021 12.0114 0.6307 0.0445 -0.7553 -8 0 -6 0.0566 -8.0011 0.0104 -6.0154 -0.9869 -0.0637 0.1762 6 10 2 0.0312 6.0061 9.9999 2.0000 0.7040 -0.6612 -0.0361 -7 9 -4 0.0492 -6.9959 9.0179 -4.0215 -0.8035 -0.6618 -0.0040 7 -9 2 0.0529 6.9957 -9.0190 2.0202 0.7506 0.6435 0.1438 3 -6 11 0.0617 2.9979 -6.0047 11.0176 0.5833 0.5156 -0.6304 -2 -12 -7 0.0602 -2.0074 -12.0111 -6.9957 -0.4280 0.7571 0.5228 -4 -13 0 0.0640 -4.0075 -13.0049 0.0072 -0.4531 0.8876 -0.0193 _olex2_submission_original_sample_id THBGLP _olex2_submission_special_instructions 'No special instructions were received' _vrf_PLAT971_6 ; PROBLEM: Check Calcd Residual Density 1.18A From Si3 4.83 eA-3 RESPONSE: Arises from anomalous absorption. ;