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#$Date: 2023-09-05 22:19:57 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286067 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/95/1569554.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1569554
loop_
_publ_author_name
'Deka, Hemanta'
'Ritacco, Ida'
'Fridman, Natalia'
'Caporaso, Lucia'
'Eisen, Moris S.'
_publ_section_title
;
 Catalytic regeneration of metal-hydrides from their corresponding
 metal-alkoxides via the hydroboration of carbonates to obtain
 methanol and diols.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              8369
_journal_page_last               8379
_journal_paper_doi               10.1039/d3sc01700a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C39 H80 N6 Si6 Th'
_chemical_formula_sum            'C39 H80 N6 Si6 Th'
_chemical_formula_weight         1033.67
_chemical_name_common            'Moris771b (Hemanta Deka)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-12-18 deposited with the CCDC.	2023-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.296(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6196(19)
_cell_length_b                   12.2443(10)
_cell_length_c                   19.8455(16)
_cell_measurement_reflns_used    9269
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.173
_cell_measurement_theta_min      1.918
_cell_volume                     5184.4(8)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEX2 (Bruker AXS)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45724
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.173
_diffrn_reflns_theta_max         25.173
_diffrn_reflns_theta_min         1.918
_exptl_absorpt_coefficient_mu    3.046
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9269
_refine_ls_number_restraints     445
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0304
_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/[σ²(Fo²)+(0.0209P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6797
_reflns_number_total             9269
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc01700a2.cif
_cod_data_source_block           Moris771b
_cod_depositor_comments
'Adding full bibliography for 1569554--1569556.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569554
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.658
_shelx_estimated_absorpt_t_max   0.711
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.25284(2) 0.56479(2) 0.58359(2) 0.02283(5) Uani 1 1 d . U . . .
Si1 Si 0.29332(6) 0.43469(11) 0.43007(6) 0.0355(3) Uani 1 1 d . U . . .
Si2 Si 0.16696(6) 0.53882(10) 0.42485(6) 0.0370(3) Uani 1 1 d . U . . .
Si3 Si 0.13732(6) 0.35707(11) 0.63148(7) 0.0439(4) Uani 1 1 d . U . . .
Si4 Si 0.16563(6) 0.55743(12) 0.71208(6) 0.0382(3) Uani 1 1 d . U . . .
Si5 Si 0.36055(6) 0.38892(10) 0.67615(6) 0.0360(3) Uani 1 1 d . U . . .
Si6 Si 0.40617(6) 0.61591(11) 0.69099(6) 0.0376(3) Uani 1 1 d . U . . .
N3 N 0.25179(14) 0.7415(3) 0.56011(14) 0.0234(8) Uani 1 1 d . U . . .
N1 N 0.29414(16) 0.8991(3) 0.51367(18) 0.0372(9) Uani 1 1 d . U . . .
N2 N 0.19255(15) 0.9003(3) 0.51807(16) 0.0304(8) Uani 1 1 d . U . . .
N4 N 0.23887(15) 0.5018(3) 0.47051(15) 0.0279(8) Uani 1 1 d . U . . .
N5 N 0.17892(14) 0.4780(3) 0.64407(16) 0.0294(8) Uani 1 1 d . U . . .
N6 N 0.34808(14) 0.5247(3) 0.65464(15) 0.0281(8) Uani 1 1 d . U . . .
C1 C 0.24709(18) 0.8366(3) 0.53385(19) 0.0256(9) Uani 1 1 d . U . . .
C2 C 0.2703(2) 0.9963(4) 0.4756(3) 0.0543(14) Uani 1 1 d . U . . .
H2A H 0.2674 0.9849 0.4258 0.065 Uiso 1 1 calc R U . . .
H2B H 0.2972 1.0606 0.4894 0.065 Uiso 1 1 calc R U . . .
C3 C 0.2066(2) 1.0096(3) 0.4954(2) 0.0427(12) Uani 1 1 d . U . . .
H3A H 0.2074 1.0636 0.5326 0.051 Uiso 1 1 calc R U . . .
H3B H 0.1754 1.0330 0.4558 0.051 Uiso 1 1 calc R U . . .
C4 C 0.35918(19) 0.8730(3) 0.5174(2) 0.0317(10) Uani 1 1 d . U . . .
C5 C 0.4017(2) 0.9286(4) 0.5661(2) 0.0356(10) Uani 1 1 d . U . . .
C6 C 0.4653(2) 0.9112(3) 0.5660(2) 0.0396(12) Uani 1 1 d . U . . .
H6 H 0.4948 0.9477 0.5990 0.047 Uiso 1 1 calc R U . . .
C7 C 0.4871(2) 0.8431(4) 0.5200(2) 0.0385(11) Uani 1 1 d . U . . .
C8 C 0.4437(2) 0.7917(4) 0.4720(2) 0.0382(11) Uani 1 1 d . U . . .
H8 H 0.4581 0.7452 0.4395 0.046 Uiso 1 1 calc R U . . .
C9 C 0.3795(2) 0.8053(4) 0.4692(2) 0.0347(10) Uani 1 1 d . U . . .
C10 C 0.3811(2) 1.0076(4) 0.6165(2) 0.0518(14) Uani 1 1 d . U . . .
H10A H 0.3724 1.0789 0.5945 0.078 Uiso 1 1 calc R U . . .
H10B H 0.4145 1.0153 0.6559 0.078 Uiso 1 1 calc R U . . .
H10C H 0.3431 0.9799 0.6316 0.078 Uiso 1 1 calc R U . . .
C11 C 0.5568(2) 0.8255(4) 0.5240(3) 0.0611(15) Uani 1 1 d . U . . .
H11A H 0.5715 0.7734 0.5606 0.092 Uiso 1 1 calc R U . . .
H11B H 0.5787 0.8952 0.5336 0.092 Uiso 1 1 calc R U . . .
H11C H 0.5653 0.7965 0.4804 0.092 Uiso 1 1 calc R U . . .
C12 C 0.3333(2) 0.7544(4) 0.4136(2) 0.0525(14) Uani 1 1 d . U . . .
H12A H 0.3557 0.7094 0.3845 0.079 Uiso 1 1 calc R U . . .
H12B H 0.3100 0.8119 0.3860 0.079 Uiso 1 1 calc R U . . .
H12C H 0.3040 0.7085 0.4339 0.079 Uiso 1 1 calc R U . . .
C13 C 0.1409(2) 0.8912(3) 0.5546(2) 0.0322(10) Uani 1 1 d . U . . .
C14 C 0.0811(2) 0.8737(4) 0.5175(2) 0.0379(11) Uani 1 1 d . U . . .
C15 C 0.0299(2) 0.8706(4) 0.5525(3) 0.0566(14) Uani 1 1 d . U . . .
H15 H -0.0109 0.8583 0.5276 0.068 Uiso 1 1 calc R U . . .
C16 C 0.0372(3) 0.8853(5) 0.6226(3) 0.0658(17) Uani 1 1 d . U . . .
C17 C 0.0961(3) 0.9092(4) 0.6569(3) 0.0616(15) Uani 1 1 d . U . . .
H17 H 0.1011 0.9237 0.7045 0.074 Uiso 1 1 calc R U . . .
C18 C 0.1490(2) 0.9131(4) 0.6244(2) 0.0438(12) Uani 1 1 d . U . . .
C19 C 0.0701(2) 0.8631(4) 0.4411(2) 0.0494(13) Uani 1 1 d . U . . .
H19A H 0.0765 0.9342 0.4205 0.074 Uiso 1 1 calc R U . . .
H19B H 0.0270 0.8383 0.4254 0.074 Uiso 1 1 calc R U . . .
H19C H 0.0996 0.8099 0.4274 0.074 Uiso 1 1 calc R U . . .
C20 C -0.0186(3) 0.8768(5) 0.6595(3) 0.107(3) Uani 1 1 d . U . . .
H20A H -0.0573 0.8812 0.6263 0.160 Uiso 1 1 calc R U . . .
H20B H -0.0174 0.9369 0.6923 0.160 Uiso 1 1 calc R U . . .
H20C H -0.0171 0.8069 0.6837 0.160 Uiso 1 1 calc R U . . .
C21 C 0.2116(2) 0.9440(4) 0.6643(2) 0.0578(14) Uani 1 1 d . U . . .
H21A H 0.2255 1.0132 0.6469 0.087 Uiso 1 1 calc R U . . .
H21B H 0.2423 0.8867 0.6594 0.087 Uiso 1 1 calc R U . . .
H21C H 0.2080 0.9522 0.7126 0.087 Uiso 1 1 calc R U . . .
C22 C 0.37390(19) 0.4651(4) 0.4770(2) 0.0462(13) Uani 1 1 d . U . . .
H22A H 0.3816 0.5439 0.4760 0.069 Uiso 1 1 calc R U . . .
H22B H 0.4050 0.4266 0.4550 0.069 Uiso 1 1 calc R U . . .
H22C H 0.3772 0.4407 0.5245 0.069 Uiso 1 1 calc R U . . .
C23 C 0.2939(2) 0.4752(4) 0.3389(2) 0.0522(14) Uani 1 1 d . U . . .
H23A H 0.2547 0.4519 0.3107 0.078 Uiso 1 1 calc R U . . .
H23B H 0.3293 0.4400 0.3224 0.078 Uiso 1 1 calc R U . . .
H23C H 0.2980 0.5547 0.3360 0.078 Uiso 1 1 calc R U . . .
C24 C 0.2785(2) 0.2842(3) 0.4247(2) 0.0492(13) Uani 1 1 d . U . . .
H24A H 0.2773 0.2552 0.4705 0.074 Uiso 1 1 calc R U . . .
H24B H 0.3121 0.2482 0.4054 0.074 Uiso 1 1 calc R U . . .
H24C H 0.2383 0.2702 0.3954 0.074 Uiso 1 1 calc R U . . .
C25 C 0.11537(19) 0.5853(4) 0.4869(2) 0.0423(12) Uani 1 1 d . U . . .
H25A H 0.1093 0.5250 0.5176 0.063 Uiso 1 1 calc R U . . .
H25B H 0.0747 0.6083 0.4618 0.063 Uiso 1 1 calc R U . . .
H25C H 0.1352 0.6468 0.5137 0.063 Uiso 1 1 calc R U . . .
C26 C 0.1261(2) 0.4270(4) 0.3709(2) 0.0598(14) Uani 1 1 d . U . . .
H26A H 0.1492 0.4103 0.3336 0.090 Uiso 1 1 calc R U . . .
H26B H 0.0835 0.4504 0.3520 0.090 Uiso 1 1 calc R U . . .
H26C H 0.1241 0.3616 0.3990 0.090 Uiso 1 1 calc R U . . .
C27 C 0.1713(2) 0.6569(4) 0.3665(2) 0.0479(13) Uani 1 1 d . U . . .
H27A H 0.1890 0.7202 0.3931 0.072 Uiso 1 1 calc R U . . .
H27B H 0.1292 0.6748 0.3429 0.072 Uiso 1 1 calc R U . . .
H27C H 0.1981 0.6379 0.3329 0.072 Uiso 1 1 calc R U . . .
C28 C 0.1672(3) 0.2472(4) 0.6946(3) 0.0722(17) Uani 1 1 d . U . . .
H28A H 0.2117 0.2337 0.6930 0.108 Uiso 1 1 calc R U . . .
H28B H 0.1433 0.1799 0.6830 0.108 Uiso 1 1 calc R U . . .
H28C H 0.1623 0.2707 0.7406 0.108 Uiso 1 1 calc R U . . .
C29 C 0.1377(2) 0.2979(4) 0.5448(2) 0.0554(14) Uani 1 1 d . U . . .
H29A H 0.1066 0.3357 0.5115 0.083 Uiso 1 1 calc R U . . .
H29B H 0.1274 0.2200 0.5453 0.083 Uiso 1 1 calc R U . . .
H29C H 0.1794 0.3070 0.5321 0.083 Uiso 1 1 calc R U . . .
C30 C 0.0522(2) 0.3736(5) 0.6383(3) 0.0804(19) Uani 1 1 d . U . . .
H30A H 0.0482 0.3932 0.6853 0.121 Uiso 1 1 calc R U . . .
H30B H 0.0301 0.3048 0.6260 0.121 Uiso 1 1 calc R U . . .
H30C H 0.0339 0.4314 0.6072 0.121 Uiso 1 1 calc R U . . .
C31 C 0.1715(2) 0.4837(4) 0.7956(2) 0.0610(15) Uani 1 1 d . U . . .
H31A H 0.1386 0.4280 0.7924 0.092 Uiso 1 1 calc R U . . .
H31B H 0.1663 0.5359 0.8317 0.092 Uiso 1 1 calc R U . . .
H31C H 0.2126 0.4487 0.8064 0.092 Uiso 1 1 calc R U . . .
C32 C 0.0891(2) 0.6313(4) 0.6983(3) 0.0628(15) Uani 1 1 d . U . . .
H32A H 0.0834 0.6679 0.6538 0.094 Uiso 1 1 calc R U . . .
H32B H 0.0887 0.6857 0.7344 0.094 Uiso 1 1 calc R U . . .
H32C H 0.0549 0.5790 0.6994 0.094 Uiso 1 1 calc R U . . .
C33 C 0.2284(2) 0.6647(4) 0.7254(2) 0.0510(14) Uani 1 1 d . U . . .
H33A H 0.2695 0.6295 0.7364 0.077 Uiso 1 1 calc R U . . .
H33B H 0.2217 0.7125 0.7632 0.077 Uiso 1 1 calc R U . . .
H33C H 0.2268 0.7080 0.6837 0.077 Uiso 1 1 calc R U . . .
C34 C 0.4412(2) 0.3377(4) 0.6720(3) 0.0609(15) Uani 1 1 d . U . . .
H34A H 0.4518 0.3534 0.6268 0.091 Uiso 1 1 calc R U . . .
H34B H 0.4428 0.2587 0.6800 0.091 Uiso 1 1 calc R U . . .
H34C H 0.4713 0.3741 0.7071 0.091 Uiso 1 1 calc R U . . .
C35 C 0.3080(2) 0.3038(4) 0.6125(2) 0.0475(12) Uani 1 1 d . U . . .
H35A H 0.2660 0.3364 0.6040 0.071 Uiso 1 1 calc R U . . .
H35B H 0.3054 0.2297 0.6305 0.071 Uiso 1 1 calc R U . . .
H35C H 0.3250 0.3009 0.5697 0.071 Uiso 1 1 calc R U . . .
C36 C 0.3419(2) 0.3530(4) 0.7621(2) 0.0598(15) Uani 1 1 d . U . . .
H36A H 0.3727 0.3871 0.7975 0.090 Uiso 1 1 calc R U . . .
H36B H 0.3435 0.2735 0.7679 0.090 Uiso 1 1 calc R U . . .
H36C H 0.2999 0.3795 0.7660 0.090 Uiso 1 1 calc R U . . .
C37 C 0.4720(2) 0.6226(4) 0.6402(3) 0.0656(16) Uani 1 1 d . U . . .
H37A H 0.4919 0.5507 0.6401 0.098 Uiso 1 1 calc R U . . .
H37B H 0.5030 0.6764 0.6607 0.098 Uiso 1 1 calc R U . . .
H37C H 0.4555 0.6441 0.5932 0.098 Uiso 1 1 calc R U . . .
C38 C 0.4405(2) 0.5785(4) 0.7809(2) 0.0594(15) Uani 1 1 d . U . . .
H38A H 0.4073 0.5777 0.8092 0.089 Uiso 1 1 calc R U . . .
H38B H 0.4724 0.6324 0.7991 0.089 Uiso 1 1 calc R U . . .
H38C H 0.4598 0.5060 0.7815 0.089 Uiso 1 1 calc R U . . .
C39 C 0.3757(2) 0.7571(4) 0.6975(2) 0.0491(13) Uani 1 1 d . U . . .
H39A H 0.3489 0.7767 0.6546 0.074 Uiso 1 1 calc R U . . .
H39B H 0.4109 0.8083 0.7064 0.074 Uiso 1 1 calc R U . . .
H39C H 0.3512 0.7606 0.7350 0.074 Uiso 1 1 calc R U . . .
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'
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
N3 Th1 N4 97.15(11) . . ?
N3 Th1 N6 107.98(11) . . ?
N4 Th1 N6 118.03(11) . . ?
N3 Th1 N5 123.66(11) . . ?
N4 Th1 N5 109.88(11) . . ?
N6 Th1 N5 101.37(11) . . ?
N4 Si1 C24 111.73(18) . . ?
N4 Si1 C22 108.77(17) . . ?
C24 Si1 C22 111.2(2) . . ?
N4 Si1 C23 115.55(18) . . ?
C24 Si1 C23 103.5(2) . . ?
C22 Si1 C23 106.0(2) . . ?
N4 Si2 C27 113.41(19) . . ?
N4 Si2 C26 114.2(2) . . ?
C27 Si2 C26 106.2(2) . . ?
N4 Si2 C25 108.34(17) . . ?
C27 Si2 C25 105.50(19) . . ?
C26 Si2 C25 108.7(2) . . ?
N5 Si3 C29 112.65(19) . . ?
N5 Si3 C30 113.0(2) . . ?
C29 Si3 C30 105.0(2) . . ?
N5 Si3 C28 113.7(2) . . ?
C29 Si3 C28 106.5(2) . . ?
C30 Si3 C28 105.3(2) . . ?
N5 Si4 C32 114.4(2) . . ?
N5 Si4 C31 115.1(2) . . ?
C32 Si4 C31 107.1(2) . . ?
N5 Si4 C33 107.29(17) . . ?
C32 Si4 C33 106.6(2) . . ?
C31 Si4 C33 105.6(2) . . ?
N6 Si5 C34 115.0(2) . . ?
N6 Si5 C36 113.86(19) . . ?
C34 Si5 C36 107.5(2) . . ?
N6 Si5 C35 108.38(18) . . ?
C34 Si5 C35 104.6(2) . . ?
C36 Si5 C35 106.8(2) . . ?
N6 Si6 C39 112.53(18) . . ?
N6 Si6 C37 111.3(2) . . ?
C39 Si6 C37 107.8(2) . . ?
N6 Si6 C38 112.63(19) . . ?
C39 Si6 C38 104.5(2) . . ?
C37 Si6 C38 107.7(2) . . ?
C1 N3 Th1 168.0(3) . . ?
C1 N1 C4 128.6(3) . . ?
C1 N1 C2 112.8(3) . . ?
C4 N1 C2 118.0(3) . . ?
C1 N2 C13 122.7(3) . . ?
C1 N2 C3 111.6(3) . . ?
C13 N2 C3 116.4(3) . . ?
Si2 N4 Si1 120.11(17) . . ?
Si2 N4 Th1 112.41(15) . . ?
Si1 N4 Th1 127.30(16) . . ?
Si4 N5 Si3 116.58(18) . . ?
Si4 N5 Th1 110.50(16) . . ?
Si3 N5 Th1 132.90(17) . . ?
Si5 N6 Si6 116.12(18) . . ?
Si5 N6 Th1 115.83(16) . . ?
Si6 N6 Th1 127.99(17) . . ?
N3 C1 N1 127.6(4) . . ?
N3 C1 N2 127.4(4) . . ?
N1 C1 N2 105.0(3) . . ?
N1 C2 C3 102.4(3) . . ?
N1 C2 H2A 111.3 . . ?
C3 C2 H2A 111.3 . . ?
N1 C2 H2B 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
N2 C3 C2 103.1(3) . . ?
N2 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
N2 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C9 C4 C5 121.4(4) . . ?
C9 C4 N1 121.0(4) . . ?
C5 C4 N1 117.2(4) . . ?
C6 C5 C4 117.6(4) . . ?
C6 C5 C10 119.8(4) . . ?
C4 C5 C10 122.6(4) . . ?
C7 C6 C5 122.6(4) . . ?
C7 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
C6 C7 C8 117.9(4) . . ?
C6 C7 C11 119.8(4) . . ?
C8 C7 C11 122.2(4) . . ?
C7 C8 C9 122.4(4) . . ?
C7 C8 H8 118.8 . . ?
C9 C8 H8 118.8 . . ?
C4 C9 C8 118.0(4) . . ?
C4 C9 C12 120.5(4) . . ?
C8 C9 C12 121.4(4) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 120.7(4) . . ?
C18 C13 N2 120.3(4) . . ?
C14 C13 N2 118.5(4) . . ?
C13 C14 C15 118.8(4) . . ?
C13 C14 C19 121.8(4) . . ?
C15 C14 C19 119.3(4) . . ?
C16 C15 C14 121.6(5) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C17 C16 C15 118.0(5) . . ?
C17 C16 C20 121.5(6) . . ?
C15 C16 C20 120.4(6) . . ?
C16 C17 C18 122.6(5) . . ?
C16 C17 H17 118.7 . . ?
C18 C17 H17 118.7 . . ?
C13 C18 C17 118.0(4) . . ?
C13 C18 C21 122.1(4) . . ?
C17 C18 C21 119.9(4) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si3 C28 H28A 109.5 . . ?
Si3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si3 C29 H29A 109.5 . . ?
Si3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si3 C30 H30A 109.5 . . ?
Si3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si4 C31 H31A 109.5 . . ?
Si4 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si4 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si4 C32 H32A 109.5 . . ?
Si4 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si4 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si4 C33 H33A 109.5 . . ?
Si4 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si4 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si5 C34 H34A 109.5 . . ?
Si5 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
Si5 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si5 C35 H35A 109.5 . . ?
Si5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
Si5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si5 C36 H36A 109.5 . . ?
Si5 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
Si5 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si6 C37 H37A 109.5 . . ?
Si6 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
Si6 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si6 C38 H38A 109.5 . . ?
Si6 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
Si6 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si6 C39 H39A 109.5 . . ?
Si6 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
Si6 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
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 N3 2.212(3) . ?
Th1 N4 2.346(3) . ?
Th1 N6 2.352(3) . ?
Th1 N5 2.397(3) . ?
Si1 N4 1.735(3) . ?
Si1 C24 1.871(4) . ?
Si1 C22 1.875(4) . ?
Si1 C23 1.879(4) . ?
Si2 N4 1.729(3) . ?
Si2 C27 1.864(4) . ?
Si2 C26 1.870(5) . ?
Si2 C25 1.879(4) . ?
Si3 N5 1.729(3) . ?
Si3 C29 1.868(4) . ?
Si3 C30 1.877(5) . ?
Si3 C28 1.880(5) . ?
Si4 N5 1.725(3) . ?
Si4 C32 1.867(4) . ?
Si4 C31 1.874(4) . ?
Si4 C33 1.876(4) . ?
Si5 N6 1.727(3) . ?
Si5 C34 1.867(4) . ?
Si5 C36 1.868(4) . ?
Si5 C35 1.873(4) . ?
Si6 N6 1.747(3) . ?
Si6 C39 1.862(5) . ?
Si6 C37 1.874(4) . ?
Si6 C38 1.876(4) . ?
N3 C1 1.274(5) . ?
N1 C1 1.383(5) . ?
N1 C4 1.432(5) . ?
N1 C2 1.458(5) . ?
N2 C1 1.406(5) . ?
N2 C13 1.431(5) . ?
N2 C3 1.460(5) . ?
C2 C3 1.502(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.389(5) . ?
C4 C5 1.398(6) . ?
C5 C6 1.393(5) . ?
C5 C10 1.509(6) . ?
C6 C7 1.373(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.378(6) . ?
C7 C11 1.511(6) . ?
C8 C9 1.390(5) . ?
C8 H8 0.9500 . ?
C9 C12 1.501(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.394(6) . ?
C13 C14 1.397(6) . ?
C14 C15 1.399(6) . ?
C14 C19 1.502(6) . ?
C15 C16 1.387(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.375(7) . ?
C16 C20 1.511(6) . ?
C17 C18 1.402(6) . ?
C17 H17 0.9500 . ?
C18 C21 1.501(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 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 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
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 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
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 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
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 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C27 Si2 N4 Si1 -73.5(3) . . . . ?
C26 Si2 N4 Si1 48.4(3) . . . . ?
C25 Si2 N4 Si1 169.7(2) . . . . ?
C27 Si2 N4 Th1 102.0(2) . . . . ?
C26 Si2 N4 Th1 -136.1(2) . . . . ?
C25 Si2 N4 Th1 -14.8(2) . . . . ?
C24 Si1 N4 Si2 -83.6(3) . . . . ?
C22 Si1 N4 Si2 153.3(2) . . . . ?
C23 Si1 N4 Si2 34.3(3) . . . . ?
C24 Si1 N4 Th1 101.6(2) . . . . ?
C22 Si1 N4 Th1 -21.5(3) . . . . ?
C23 Si1 N4 Th1 -140.5(2) . . . . ?
C32 Si4 N5 Si3 -74.3(3) . . . . ?
C31 Si4 N5 Si3 50.5(3) . . . . ?
C33 Si4 N5 Si3 167.6(2) . . . . ?
C32 Si4 N5 Th1 104.5(2) . . . . ?
C31 Si4 N5 Th1 -130.7(2) . . . . ?
C33 Si4 N5 Th1 -13.5(2) . . . . ?
C29 Si3 N5 Si4 163.9(2) . . . . ?
C30 Si3 N5 Si4 45.1(3) . . . . ?
C28 Si3 N5 Si4 -74.8(3) . . . . ?
C29 Si3 N5 Th1 -14.6(3) . . . . ?
C30 Si3 N5 Th1 -133.4(3) . . . . ?
C28 Si3 N5 Th1 106.7(3) . . . . ?
C34 Si5 N6 Si6 -45.8(3) . . . . ?
C36 Si5 N6 Si6 78.9(3) . . . . ?
C35 Si5 N6 Si6 -162.5(2) . . . . ?
C34 Si5 N6 Th1 136.6(2) . . . . ?
C36 Si5 N6 Th1 -98.6(2) . . . . ?
C35 Si5 N6 Th1 20.0(2) . . . . ?
C39 Si6 N6 Si5 -154.9(2) . . . . ?
C37 Si6 N6 Si5 84.0(3) . . . . ?
C38 Si6 N6 Si5 -37.0(3) . . . . ?
C39 Si6 N6 Th1 22.3(3) . . . . ?
C37 Si6 N6 Th1 -98.8(2) . . . . ?
C38 Si6 N6 Th1 140.1(2) . . . . ?
Th1 N3 C1 N1 -97.5(14) . . . . ?
Th1 N3 C1 N2 81.4(14) . . . . ?
C4 N1 C1 N3 -0.2(7) . . . . ?
C2 N1 C1 N3 170.6(4) . . . . ?
C4 N1 C1 N2 -179.3(4) . . . . ?
C2 N1 C1 N2 -8.5(5) . . . . ?
C13 N2 C1 N3 28.4(6) . . . . ?
C3 N2 C1 N3 173.9(4) . . . . ?
C13 N2 C1 N1 -152.5(4) . . . . ?
C3 N2 C1 N1 -7.0(4) . . . . ?
C1 N1 C2 C3 19.6(5) . . . . ?
C4 N1 C2 C3 -168.5(4) . . . . ?
C1 N2 C3 C2 18.7(5) . . . . ?
C13 N2 C3 C2 166.5(4) . . . . ?
N1 C2 C3 N2 -21.7(5) . . . . ?
C1 N1 C4 C9 79.5(6) . . . . ?
C2 N1 C4 C9 -91.0(5) . . . . ?
C1 N1 C4 C5 -108.1(5) . . . . ?
C2 N1 C4 C5 81.4(5) . . . . ?
C9 C4 C5 C6 -2.0(6) . . . . ?
N1 C4 C5 C6 -174.3(4) . . . . ?
C9 C4 C5 C10 176.4(4) . . . . ?
N1 C4 C5 C10 4.0(6) . . . . ?
C4 C5 C6 C7 0.6(6) . . . . ?
C10 C5 C6 C7 -177.8(4) . . . . ?
C5 C6 C7 C8 0.7(6) . . . . ?
C5 C6 C7 C11 -178.4(4) . . . . ?
C6 C7 C8 C9 -0.9(6) . . . . ?
C11 C7 C8 C9 178.2(4) . . . . ?
C5 C4 C9 C8 1.9(6) . . . . ?
N1 C4 C9 C8 174.0(4) . . . . ?
C5 C4 C9 C12 -174.5(4) . . . . ?
N1 C4 C9 C12 -2.4(6) . . . . ?
C7 C8 C9 C4 -0.4(6) . . . . ?
C7 C8 C9 C12 175.9(4) . . . . ?
C1 N2 C13 C18 60.8(5) . . . . ?
C3 N2 C13 C18 -83.1(5) . . . . ?
C1 N2 C13 C14 -127.1(4) . . . . ?
C3 N2 C13 C14 89.0(5) . . . . ?
C18 C13 C14 C15 -4.5(6) . . . . ?
N2 C13 C14 C15 -176.6(4) . . . . ?
C18 C13 C14 C19 172.7(4) . . . . ?
N2 C13 C14 C19 0.6(6) . . . . ?
C13 C14 C15 C16 0.4(7) . . . . ?
C19 C14 C15 C16 -176.9(5) . . . . ?
C14 C15 C16 C17 3.7(8) . . . . ?
C14 C15 C16 C20 -177.4(5) . . . . ?
C15 C16 C17 C18 -3.8(8) . . . . ?
C20 C16 C17 C18 177.3(5) . . . . ?
C14 C13 C18 C17 4.4(7) . . . . ?
N2 C13 C18 C17 176.3(4) . . . . ?
C14 C13 C18 C21 -173.4(4) . . . . ?
N2 C13 C18 C21 -1.4(6) . . . . ?
C16 C17 C18 C13 -0.2(7) . . . . ?
C16 C17 C18 C21 177.6(5) . . . . ?
