#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:46:32 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233336 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/87/4348783.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_4348783
loop_
_publ_author_name
'Smiles, Danil E.'
'Wu, Guang'
'Hayton, Trevor W.'
_publ_section_title
;
 Synthesis, Electrochemistry, and Reactivity of the Actinide Trisulfides
 [K(18-crown-6)][An(η(3)-S3)(NR2)3] (An = U, Th; R = SiMe3).
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9150
_journal_page_last               9153
_journal_paper_doi               10.1021/acs.inorgchem.6b01618
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C34 H88 K N3 O7 S3 Si6 Th'
_chemical_formula_weight         1186.93
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.696(2)
_cell_angle_beta                 97.064(2)
_cell_angle_gamma                109.856(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2987(15)
_cell_length_b                   12.9526(18)
_cell_length_c                   20.985(3)
_cell_measurement_reflns_used    1369
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      11.81
_cell_volume                     2804.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22547
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    3.012
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         8.255
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         13635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0365P)²+5.7873P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                12255
_reflns_number_total             13635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01618_si_001.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4348783
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Th1 Th 0.592079(11) 0.741854(10) 0.240214(6) 0.00951(4) Uani 1 1 d .
K1 K 0.14567(7) 0.32448(6) 0.21757(4) 0.01444(14) Uani 1 1 d .
S2 S 0.47669(9) 0.53839(8) 0.28468(5) 0.01934(19) Uani 1 1 d .
S3 S 0.60966(9) 0.52858(7) 0.22658(5) 0.01902(18) Uani 1 1 d .
Si3 Si 0.88620(9) 0.76615(8) 0.18873(5) 0.01338(19) Uani 1 1 d .
Si4 Si 0.91916(9) 0.96427(8) 0.28784(5) 0.01170(18) Uani 1 1 d .
Si5 Si 0.43311(9) 0.87834(8) 0.34175(5) 0.01178(18) Uani 1 1 d .
Si6 Si 0.61707(9) 0.79254(8) 0.41006(5) 0.01377(19) Uani 1 1 d .
S1 S 0.33658(8) 0.57443(8) 0.23018(5) 0.01883(18) Uani 1 1 d .
Si2 Si 0.56222(10) 0.90791(8) 0.12752(5) 0.01514(19) Uani 1 1 d .
Si1 Si 0.40481(9) 0.66686(9) 0.07377(5) 0.0162(2) Uani 1 1 d .
O4 O 0.0549(2) 0.3732(2) 0.33526(12) 0.0165(5) Uani 1 1 d .
O7 O 0.1933(2) 0.6223(2) 0.53289(13) 0.0190(5) Uani 1 1 d .
O3 O 0.2758(2) 0.3192(2) 0.33867(13) 0.0171(5) Uani 1 1 d .
O2 O 0.3125(2) 0.2026(2) 0.22440(13) 0.0176(5) Uani 1 1 d .
O5 O -0.0744(2) 0.3792(2) 0.21304(13) 0.0206(6) Uani 1 1 d .
O1 O 0.1921(3) 0.2203(3) 0.10295(14) 0.0261(6) Uani 1 1 d .
O6 O -0.0361(3) 0.2624(3) 0.09942(14) 0.0285(7) Uani 1 1 d .
N1 N 0.5112(3) 0.7712(2) 0.13810(14) 0.0135(6) Uani 1 1 d .
N3 N 0.5508(3) 0.8208(2) 0.33907(14) 0.0108(5) Uani 1 1 d .
N2 N 0.8145(3) 0.8382(2) 0.23838(14) 0.0109(5) Uani 1 1 d .
C6 C 0.6210(3) 1.0097(3) 0.21130(19) 0.0179(7) Uani 1 1 d .
H6A H 0.5473 1.0176 0.2288 0.027 Uiso 1 1 calc R
H6B H 0.6776 1.0831 0.2062 0.027 Uiso 1 1 calc R
H6C H 0.6680 0.9803 0.2417 0.027 Uiso 1 1 calc R
C8 C 0.9545(3) 0.6777(3) 0.2332(2) 0.0218(8) Uani 1 1 d .
H8A H 1.0278 0.7265 0.2674 0.033 Uiso 1 1 calc R
H8B H 0.9827 0.6308 0.2020 0.033 Uiso 1 1 calc R
H8C H 0.8888 0.6297 0.2533 0.033 Uiso 1 1 calc R
C13 C 0.3353(3) 0.8558(3) 0.25808(18) 0.0178(7) Uani 1 1 d .
H13A H 0.3847 0.8431 0.2245 0.027 Uiso 1 1 calc R
H13B H 0.3142 0.9222 0.2543 0.027 Uiso 1 1 calc R
H13C H 0.2562 0.7902 0.2519 0.027 Uiso 1 1 calc R
C9 C 1.0200(3) 0.8583(3) 0.15391(19) 0.0209(8) Uani 1 1 d .
H9A H 0.9871 0.9022 0.1274 0.031 Uiso 1 1 calc R
H9B H 1.0542 0.8114 0.1264 0.031 Uiso 1 1 calc R
H9C H 1.0883 0.9092 0.1899 0.031 Uiso 1 1 calc R
C17 C 0.7574(3) 0.7519(3) 0.39421(19) 0.0183(7) Uani 1 1 d .
H17A H 0.7306 0.6915 0.3551 0.028 Uiso 1 1 calc R
H17B H 0.7883 0.7259 0.4321 0.028 Uiso 1 1 calc R
H17C H 0.8263 0.8171 0.3872 0.028 Uiso 1 1 calc R
C18 C 0.5056(4) 0.6772(3) 0.4428(2) 0.0222(8) Uani 1 1 d .
H18A H 0.4445 0.7040 0.4626 0.033 Uiso 1 1 calc R
H18B H 0.5552 0.6548 0.4760 0.033 Uiso 1 1 calc R
H18C H 0.4589 0.6125 0.4068 0.033 Uiso 1 1 calc R
C23 C 0.2235(4) 0.3389(4) 0.39550(19) 0.0229(8) Uani 1 1 d .
H23A H 0.2920 0.3674 0.4351 0.027 Uiso 1 1 calc R
H23B H 0.1588 0.2681 0.4006 0.027 Uiso 1 1 calc R
C12 C 0.8478(3) 1.0284(3) 0.35202(19) 0.0182(7) Uani 1 1 d .
H12A H 0.7632 0.9747 0.3535 0.027 Uiso 1 1 calc R
H12B H 0.8392 1.0967 0.3410 0.027 Uiso 1 1 calc R
H12C H 0.9038 1.0471 0.3949 0.027 Uiso 1 1 calc R
C1 C 0.4398(4) 0.6950(3) -0.00907(18) 0.0216(8) Uani 1 1 d .
H1A H 0.4330 0.7668 -0.0141 0.032 Uiso 1 1 calc R
H1B H 0.3779 0.6347 -0.0438 0.032 Uiso 1 1 calc R
H1C H 0.5267 0.6979 -0.0122 0.032 Uiso 1 1 calc R
C25 C -0.0167(4) 0.4446(3) 0.3281(2) 0.0214(8) Uani 1 1 d .
H25A H 0.0388 0.5171 0.3199 0.026 Uiso 1 1 calc R
H25B H -0.0497 0.4596 0.3687 0.026 Uiso 1 1 calc R
C21 C 0.4047(3) 0.2378(3) 0.28363(19) 0.0177(7) Uani 1 1 d .
H21A H 0.4676 0.3139 0.2858 0.021 Uiso 1 1 calc R
H21B H 0.4513 0.1857 0.2854 0.021 Uiso 1 1 calc R
C5 C 0.6984(4) 0.9439(4) 0.0820(2) 0.0255(9) Uani 1 1 d .
H5A H 0.7696 0.9282 0.1046 0.038 Uiso 1 1 calc R
H5B H 0.7266 1.0237 0.0803 0.038 Uiso 1 1 calc R
H5C H 0.6701 0.8987 0.0372 0.038 Uiso 1 1 calc R
C33 C 0.1494(4) 0.7135(3) 0.5379(2) 0.0221(8) Uani 1 1 d .
H33A H 0.2203 0.7835 0.5368 0.027 Uiso 1 1 calc R
H33B H 0.1194 0.7241 0.5799 0.027 Uiso 1 1 calc R
C20 C 0.3713(4) 0.2079(3) 0.1680(2) 0.0222(8) Uani 1 1 d .
H20A H 0.4323 0.1682 0.1697 0.027 Uiso 1 1 calc R
H20B H 0.4191 0.2871 0.1666 0.027 Uiso 1 1 calc R
C4 C 0.4330(4) 0.9487(4) 0.0855(2) 0.0271(9) Uani 1 1 d .
H4A H 0.3953 0.8990 0.0423 0.041 Uiso 1 1 calc R
H4B H 0.4699 1.0264 0.0802 0.041 Uiso 1 1 calc R
H4C H 0.3663 0.9420 0.1121 0.041 Uiso 1 1 calc R
C26 C -0.1255(4) 0.3865(3) 0.27158(19) 0.0203(8) Uani 1 1 d .
H26A H -0.1752 0.3104 0.2775 0.024 Uiso 1 1 calc R
H26B H -0.1833 0.4291 0.2689 0.024 Uiso 1 1 calc R
C24 C 0.1625(4) 0.4233(3) 0.3879(2) 0.0232(8) Uani 1 1 d .
H24A H 0.1345 0.4454 0.4290 0.028 Uiso 1 1 calc R
H24B H 0.2246 0.4912 0.3781 0.028 Uiso 1 1 calc R
C11 C 1.0623(3) 0.9483(3) 0.3356(2) 0.0200(8) Uani 1 1 d .
H11A H 1.0334 0.8840 0.3568 0.030 Uiso 1 1 calc R
H11B H 1.1094 1.0165 0.3691 0.030 Uiso 1 1 calc R
H11C H 1.1186 0.9360 0.3057 0.030 Uiso 1 1 calc R
C31 C 0.3397(4) 0.5433(3) 0.5748(2) 0.0289(9) Uani 1 1 d .
H31A H 0.2686 0.4794 0.5815 0.043 Uiso 1 1 calc R
H31B H 0.4158 0.5579 0.6079 0.043 Uiso 1 1 calc R
H31C H 0.3583 0.5260 0.5309 0.043 Uiso 1 1 calc R
C14 C 0.3154(4) 0.8171(3) 0.3943(2) 0.0213(8) Uani 1 1 d .
H14A H 0.2761 0.7356 0.3787 0.032 Uiso 1 1 calc R
H14B H 0.2487 0.8496 0.3918 0.032 Uiso 1 1 calc R
H14C H 0.3599 0.8342 0.4400 0.032 Uiso 1 1 calc R
C32 C 0.3035(3) 0.6453(3) 0.58114(19) 0.0197(8) Uani 1 1 d .
H32A H 0.2851 0.6637 0.6255 0.024 Uiso 1 1 calc R
H32B H 0.3750 0.7104 0.5747 0.024 Uiso 1 1 calc R
C2 C 0.4086(4) 0.5228(3) 0.0703(2) 0.0228(8) Uani 1 1 d .
H2A H 0.4952 0.5247 0.0675 0.034 Uiso 1 1 calc R
H2B H 0.3481 0.4713 0.0317 0.034 Uiso 1 1 calc R
H2C H 0.3845 0.4968 0.1101 0.034 Uiso 1 1 calc R
C22 C 0.3349(3) 0.2386(3) 0.34047(19) 0.0185(7) Uani 1 1 d .
H22A H 0.2692 0.1634 0.3371 0.022 Uiso 1 1 calc R
H22B H 0.3959 0.2581 0.3824 0.022 Uiso 1 1 calc R
C7 C 0.7707(4) 0.6714(3) 0.11313(19) 0.0213(8) Uani 1 1 d .
H7A H 0.7055 0.6099 0.1258 0.032 Uiso 1 1 calc R
H7B H 0.8172 0.6406 0.0839 0.032 Uiso 1 1 calc R
H7C H 0.7292 0.7144 0.0904 0.032 Uiso 1 1 calc R
C15 C 0.5050(4) 1.0337(3) 0.37631(19) 0.0181(7) Uani 1 1 d .
H15A H 0.5547 1.0476 0.4205 0.027 Uiso 1 1 calc R
H15B H 0.4365 1.0636 0.3784 0.027 Uiso 1 1 calc R
H15C H 0.5614 1.0707 0.3480 0.027 Uiso 1 1 calc R
C16 C 0.6797(4) 0.9156(4) 0.48170(19) 0.0250(8) Uani 1 1 d .
H16A H 0.7374 0.9810 0.4685 0.038 Uiso 1 1 calc R
H16B H 0.7264 0.8971 0.5180 0.038 Uiso 1 1 calc R
H16C H 0.6077 0.9328 0.4959 0.038 Uiso 1 1 calc R
C27 C -0.1708(4) 0.3335(4) 0.1561(2) 0.0314(10) Uani 1 1 d .
H27A H -0.2258 0.3787 0.1540 0.038 Uiso 1 1 calc R
H27B H -0.2252 0.2557 0.1569 0.038 Uiso 1 1 calc R
C34 C 0.0416(4) 0.6885(4) 0.4814(2) 0.0287(9) Uani 1 1 d .
H34A H 0.0729 0.6810 0.4401 0.043 Uiso 1 1 calc R
H34B H 0.0091 0.7499 0.4851 0.043 Uiso 1 1 calc R
H34C H -0.0274 0.6184 0.4822 0.043 Uiso 1 1 calc R
C3 C 0.2349(4) 0.6552(4) 0.0775(2) 0.0239(8) Uani 1 1 d .
H3A H 0.2146 0.6373 0.1196 0.036 Uiso 1 1 calc R
H3B H 0.1760 0.5956 0.0416 0.036 Uiso 1 1 calc R
H3C H 0.2258 0.7267 0.0735 0.036 Uiso 1 1 calc R
C10 C 0.9817(4) 1.0792(3) 0.2416(2) 0.0190(7) Uani 1 1 d .
C19 C 0.2688(4) 0.1539(4) 0.1085(2) 0.0252(9) Uani 1 1 d .
H19A H 0.3076 0.1478 0.0690 0.030 Uiso 1 1 calc R
H19B H 0.2153 0.0775 0.1122 0.030 Uiso 1 1 calc R
C28 C -0.1064(5) 0.3346(5) 0.0975(2) 0.0374(12) Uani 1 1 d .
H28A H -0.1715 0.3087 0.0566 0.045 Uiso 1 1 calc R
H28B H -0.0480 0.4118 0.0983 0.045 Uiso 1 1 calc R
C30 C 0.0902(5) 0.1731(5) 0.0479(2) 0.0443(14) Uani 1 1 d .
H30A H 0.0305 0.1001 0.0533 0.053 Uiso 1 1 calc R
H30B H 0.1244 0.1604 0.0074 0.053 Uiso 1 1 calc R
C29 C 0.0211(6) 0.2530(6) 0.0429(2) 0.0505(16) Uani 1 1 d .
H29A H 0.0821 0.3275 0.0405 0.061 Uiso 1 1 calc R
H29B H -0.0457 0.2249 0.0027 0.061 Uiso 1 1 calc R
H10A H 1.047(5) 1.076(4) 0.220(2) 0.032(13) Uiso 1 1 d .
H10B H 1.009(5) 1.145(4) 0.272(2) 0.030(13) Uiso 1 1 d .
H10C H 0.920(5) 1.083(4) 0.211(3) 0.034(14) Uiso 1 1 d .
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
N3 Th1 N1 122.01(10) . .
N3 Th1 N2 107.36(10) . .
N1 Th1 N2 96.20(10) . .
N3 Th1 S3 118.81(7) . .
N1 Th1 S3 110.83(7) . .
N2 Th1 S3 94.55(7) . .
N3 Th1 S2 81.83(7) . .
N1 Th1 S2 122.17(7) . .
N2 Th1 S2 128.42(7) . .
S3 Th1 S2 42.78(3) . .
N3 Th1 S1 83.37(7) . .
N1 Th1 S1 85.92(7) . .
N2 Th1 S1 165.38(7) . .
S3 Th1 S1 71.28(3) . .
S2 Th1 S1 41.70(3) . .
O1 K1 O3 119.31(8) . .
O1 K1 O5 119.17(9) . .
O3 K1 O5 119.31(8) . .
O1 K1 O6 60.01(8) . .
O3 K1 O6 161.92(9) . .
O5 K1 O6 59.27(8) . .
O1 K1 O2 60.19(8) . .
O3 K1 O2 59.24(7) . .
O5 K1 O2 161.96(8) . .
O6 K1 O2 115.78(8) . .
O1 K1 O4 164.96(9) . .
O3 K1 O4 59.58(7) . .
O5 K1 O4 59.72(8) . .
O6 K1 O4 115.77(8) . .
O2 K1 O4 115.62(8) . .
O1 K1 S1 100.54(7) . .
O3 K1 S1 89.40(6) . .
O5 K1 S1 94.88(6) . .
O6 K1 S1 108.62(7) . .
O2 K1 S1 103.00(6) . .
O4 K1 S1 94.47(6) . .
O1 K1 C10 88.83(10) . 1_445
O3 K1 C10 77.03(9) . 1_445
O5 K1 C10 89.35(10) . 1_445
O6 K1 C10 84.90(10) . 1_445
O2 K1 C10 72.69(9) . 1_445
O4 K1 C10 76.25(9) . 1_445
S1 K1 C10 166.12(8) . 1_445
O1 K1 S2 99.02(7) . .
O3 K1 S2 60.88(6) . .
O5 K1 S2 122.55(6) . .
O6 K1 S2 136.58(7) . .
O2 K1 S2 73.74(6) . .
O4 K1 S2 93.07(6) . .
S1 K1 S2 33.25(2) . .
C10 K1 S2 135.49(8) 1_445 .
S1 S2 S3 107.89(6) . .
S1 S2 Th1 70.57(4) . .
S3 S2 Th1 67.14(3) . .
S1 S2 K1 57.53(4) . .
S3 S2 K1 113.74(5) . .
Th1 S2 K1 125.90(3) . .
S2 S3 Th1 70.08(4) . .
N2 Si3 C8 112.26(17) . .
N2 Si3 C7 112.18(15) . .
C8 Si3 C7 107.62(18) . .
N2 Si3 C9 114.72(16) . .
C8 Si3 C9 106.49(17) . .
C7 Si3 C9 102.89(18) . .
N2 Si4 C12 114.57(15) . .
N2 Si4 C10 113.94(16) . .
C12 Si4 C10 103.48(18) . .
N2 Si4 C11 112.13(16) . .
C12 Si4 C11 104.56(18) . .
C10 Si4 C11 107.29(18) . .
N3 Si5 C14 113.34(16) . .
N3 Si5 C13 111.98(15) . .
C14 Si5 C13 105.87(18) . .
N3 Si5 C15 111.17(16) . .
C14 Si5 C15 106.26(18) . .
C13 Si5 C15 107.84(17) . .
N3 Si6 C18 115.33(16) . .
N3 Si6 C17 108.93(15) . .
C18 Si6 C17 107.50(17) . .
N3 Si6 C16 113.99(17) . .
C18 Si6 C16 103.93(19) . .
C17 Si6 C16 106.62(18) . .
S2 S1 Th1 67.73(3) . .
S2 S1 K1 89.22(4) . .
Th1 S1 K1 152.21(4) . .
N1 Si2 C5 113.54(17) . .
N1 Si2 C4 114.42(18) . .
C5 Si2 C4 107.65(19) . .
N1 Si2 C6 110.08(15) . .
C5 Si2 C6 106.58(18) . .
C4 Si2 C6 103.87(18) . .
N1 Si1 C2 115.91(16) . .
N1 Si1 C3 110.28(17) . .
C2 Si1 C3 106.75(19) . .
N1 Si1 C1 112.06(17) . .
C2 Si1 C1 102.50(18) . .
C3 Si1 C1 108.86(18) . .
C24 O4 C25 111.8(3) . .
C24 O4 K1 108.3(2) . .
C25 O4 K1 110.6(2) . .
C32 O7 C33 111.8(3) . .
C22 O3 C23 113.1(3) . .
C22 O3 K1 118.1(2) . .
C23 O3 K1 118.3(2) . .
C21 O2 C20 111.9(3) . .
C21 O2 K1 114.3(2) . .
C20 O2 K1 108.2(2) . .
C27 O5 C26 112.5(3) . .
C27 O5 K1 118.8(2) . .
C26 O5 K1 117.5(2) . .
C30 O1 C19 112.3(3) . .
C30 O1 K1 118.1(2) . .
C19 O1 K1 117.9(2) . .
C28 O6 C29 112.2(3) . .
C28 O6 K1 112.0(3) . .
C29 O6 K1 111.9(3) . .
Si2 N1 Si1 118.18(17) . .
Si2 N1 Th1 116.39(15) . .
Si1 N1 Th1 125.43(15) . .
Si6 N3 Si5 119.28(16) . .
Si6 N3 Th1 116.82(14) . .
Si5 N3 Th1 122.45(15) . .
Si4 N2 Si3 114.79(15) . .
Si4 N2 Th1 128.04(14) . .
Si3 N2 Th1 116.66(14) . .
Si2 C6 H6A 109.5 . .
Si2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si3 C8 H8A 109.5 . .
Si3 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si3 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Si5 C13 H13A 109.5 . .
Si5 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
Si5 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Si3 C9 H9A 109.5 . .
Si3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
Si3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
Si6 C17 H17A 109.5 . .
Si6 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
Si6 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
Si6 C18 H18A 109.5 . .
Si6 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
Si6 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
O3 C23 C24 108.5(3) . .
O3 C23 H23A 110.0 . .
C24 C23 H23A 110.0 . .
O3 C23 H23B 110.0 . .
C24 C23 H23B 110.0 . .
H23A C23 H23B 108.4 . .
Si4 C12 H12A 109.5 . .
Si4 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
Si4 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O4 C25 C26 108.0(3) . .
O4 C25 H25A 110.1 . .
C26 C25 H25A 110.1 . .
O4 C25 H25B 110.1 . .
C26 C25 H25B 110.1 . .
H25A C25 H25B 108.4 . .
O2 C21 C22 108.1(3) . .
O2 C21 H21A 110.1 . .
C22 C21 H21A 110.1 . .
O2 C21 H21B 110.1 . .
C22 C21 H21B 110.1 . .
H21A C21 H21B 108.4 . .
Si2 C5 H5A 109.5 . .
Si2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
O7 C33 C34 108.9(3) . .
O7 C33 H33A 109.9 . .
C34 C33 H33A 109.9 . .
O7 C33 H33B 109.9 . .
C34 C33 H33B 109.9 . .
H33A C33 H33B 108.3 . .
O2 C20 C19 108.3(3) . .
O2 C20 H20A 110.0 . .
C19 C20 H20A 110.0 . .
O2 C20 H20B 110.0 . .
C19 C20 H20B 110.0 . .
H20A C20 H20B 108.4 . .
Si2 C4 H4A 109.5 . .
Si2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O5 C26 C25 108.4(3) . .
O5 C26 H26A 110.0 . .
C25 C26 H26A 110.0 . .
O5 C26 H26B 110.0 . .
C25 C26 H26B 110.0 . .
H26A C26 H26B 108.4 . .
O4 C24 C23 107.8(3) . .
O4 C24 H24A 110.1 . .
C23 C24 H24A 110.1 . .
O4 C24 H24B 110.1 . .
C23 C24 H24B 110.1 . .
H24A C24 H24B 108.5 . .
Si4 C11 H11A 109.5 . .
Si4 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
Si4 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C32 C31 H31A 109.5 . .
C32 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C32 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
Si5 C14 H14A 109.5 . .
Si5 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
Si5 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O7 C32 C31 108.5(3) . .
O7 C32 H32A 110.0 . .
C31 C32 H32A 110.0 . .
O7 C32 H32B 110.0 . .
C31 C32 H32B 110.0 . .
H32A C32 H32B 108.4 . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O3 C22 C21 108.5(3) . .
O3 C22 H22A 110.0 . .
C21 C22 H22A 110.0 . .
O3 C22 H22B 110.0 . .
C21 C22 H22B 110.0 . .
H22A C22 H22B 108.4 . .
Si3 C7 H7A 109.5 . .
Si3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si3 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si5 C15 H15A 109.5 . .
Si5 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
Si5 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
Si6 C16 H16A 109.5 . .
Si6 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
Si6 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O5 C27 C28 107.9(4) . .
O5 C27 H27A 110.1 . .
C28 C27 H27A 110.1 . .
O5 C27 H27B 110.1 . .
C28 C27 H27B 110.1 . .
H27A C27 H27B 108.4 . .
C33 C34 H34A 109.5 . .
C33 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C33 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
Si1 C3 H3A 109.5 . .
Si1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si4 C10 K1 158.4(2) . 1_665
Si4 C10 H10A 116(3) . .
K1 C10 H10A 69(3) 1_665 .
Si4 C10 H10B 106(3) . .
K1 C10 H10B 54(3) 1_665 .
H10A C10 H10B 110(4) . .
Si4 C10 H10C 113(3) . .
K1 C10 H10C 83(3) 1_665 .
H10A C10 H10C 105(4) . .
H10B C10 H10C 106(4) . .
O1 C19 C20 108.8(3) . .
O1 C19 H19A 109.9 . .
C20 C19 H19A 109.9 . .
O1 C19 H19B 109.9 . .
C20 C19 H19B 109.9 . .
H19A C19 H19B 108.3 . .
O6 C28 C27 108.8(4) . .
O6 C28 H28A 109.9 . .
C27 C28 H28A 109.9 . .
O6 C28 H28B 109.9 . .
C27 C28 H28B 109.9 . .
H28A C28 H28B 108.3 . .
O1 C30 C29 108.5(4) . .
O1 C30 H30A 110.0 . .
C29 C30 H30A 110.0 . .
O1 C30 H30B 110.0 . .
C29 C30 H30B 110.0 . .
H30A C30 H30B 108.4 . .
O6 C29 C30 108.7(4) . .
O6 C29 H29A 109.9 . .
C30 C29 H29A 109.9 . .
O6 C29 H29B 109.9 . .
C30 C29 H29B 109.9 . .
H29A C29 H29B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th1 N3 2.343(3) .
Th1 N1 2.361(3) .
Th1 N2 2.405(3) .
Th1 S3 2.8108(10) .
Th1 S2 2.8679(9) .
Th1 S1 2.9224(9) .
K1 O1 2.773(3) .
K1 O3 2.798(3) .
K1 O5 2.802(3) .
K1 O6 2.834(3) .
K1 O2 2.844(3) .
K1 O4 2.854(3) .
K1 S1 3.1719(12) .
K1 C10 3.240(4) 1_445
K1 S2 3.7595(12) .
S2 S1 2.0616(14) .
S2 S3 2.0720(13) .
Si3 N2 1.744(3) .
Si3 C8 1.878(4) .
Si3 C7 1.882(4) .
Si3 C9 1.885(4) .
Si4 N2 1.737(3) .
Si4 C12 1.881(4) .
Si4 C10 1.883(4) .
Si4 C11 1.886(4) .
Si5 N3 1.734(3) .
Si5 C14 1.877(4) .
Si5 C13 1.881(4) .
Si5 C15 1.881(4) .
Si6 N3 1.729(3) .
Si6 C18 1.880(4) .
Si6 C17 1.883(4) .
Si6 C16 1.884(4) .
Si2 N1 1.725(3) .
Si2 C5 1.873(4) .
Si2 C4 1.881(4) .
Si2 C6 1.920(4) .
Si1 N1 1.743(3) .
Si1 C2 1.872(4) .
Si1 C3 1.886(4) .
Si1 C1 1.890(4) .
O4 C24 1.428(5) .
O4 C25 1.433(4) .
O7 C32 1.418(5) .
O7 C33 1.423(4) .
O3 C22 1.419(4) .
O3 C23 1.422(4) .
O2 C21 1.423(5) .
O2 C20 1.426(4) .
O5 C27 1.412(5) .
O5 C26 1.424(4) .
O1 C30 1.419(6) .
O1 C19 1.420(5) .
O6 C28 1.420(5) .
O6 C29 1.427(5) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C23 C24 1.494(6) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C25 C26 1.492(6) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C21 C22 1.510(5) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C33 C34 1.501(6) .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C20 C19 1.490(6) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C31 C32 1.503(6) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C27 C28 1.503(6) .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C10 K1 3.240(4) 1_665
C10 H10A 0.92(5) .
C10 H10B 0.91(5) .
C10 H10C 0.92(5) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C30 C29 1.500(7) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
