#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:46:32 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233336 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/87/4348785.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_4348785
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            'C36 H88 F6 K N3 O13 S2 Si6 Th'
_chemical_formula_weight         1388.89
_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                102.032(5)
_cell_angle_beta                 109.232(5)
_cell_angle_gamma                96.868(5)
_cell_formula_units_Z            2
_cell_length_a                   13.365(5)
_cell_length_b                   14.225(5)
_cell_length_c                   18.947(6)
_cell_measurement_reflns_used    1971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      16.64
_cell_volume                     3257(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0924
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28627
_diffrn_reflns_theta_full        27.13
_diffrn_reflns_theta_max         27.13
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    2.594
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.6465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         12.366
_refine_diff_density_min         -4.581
_refine_diff_density_rms         0.343
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         14089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.1166
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0532P)²+233.9080P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2749
_refine_ls_wR_factor_ref         0.3035
_reflns_number_gt                10684
_reflns_number_total             14089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01618_si_001.cif
_cod_data_source_block           complex_4
_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_cell_volume        3256.5(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4348785
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 0.61108(5) 0.23562(4) 0.79939(3) 0.02365(18) Uani 1 1 d .
K2 K 1.0000 0.0000 1.0000 0.0223(9) Uani 1 2 d S
K1 K 0.5000 0.5000 0.5000 0.0236(10) Uani 1 2 d S
S2 S 0.6879(3) -0.0043(2) 0.8409(2) 0.0234(8) Uani 1 1 d .
S1 S 0.6301(4) 0.4633(3) 0.7207(2) 0.0267(8) Uani 1 1 d .
Si5 Si 0.6058(4) 0.2511(3) 0.9866(3) 0.0242(9) Uani 1 1 d .
Si4 Si 0.8666(4) 0.2181(3) 0.7821(3) 0.0245(9) Uani 1 1 d .
Si2 Si 0.3520(4) 0.0695(3) 0.6786(3) 0.0256(9) Uani 1 1 d .
Si3 Si 0.6791(4) 0.1689(3) 0.6322(3) 0.0261(9) Uani 1 1 d .
Si6 Si 0.7647(4) 0.4149(3) 0.9827(3) 0.0255(9) Uani 1 1 d .
Si1 Si 0.3476(4) 0.2775(3) 0.7447(3) 0.0274(10) Uani 1 1 d .
F1 F 0.6158(9) 0.6479(7) 0.7565(6) 0.038(2) Uani 1 1 d .
F2 F 0.4738(9) 0.5469(7) 0.7447(6) 0.036(2) Uani 1 1 d .
O1 O 0.6346(9) 0.0810(7) 0.8321(6) 0.0237(16) Uani 1 1 d .
O2 O 0.7809(11) 0.0164(8) 0.9096(7) 0.035(2) Uani 1 1 d .
F6 F 0.6193(9) -0.1707(7) 0.8638(7) 0.041(3) Uani 1 1 d .
O12 O 1.0849(9) 0.0223(8) 0.8878(6) 0.026(2) Uani 1 1 d .
O9 O 0.2797(10) 0.4154(8) 0.4589(7) 0.034(3) Uani 1 1 d .
F4 F 0.4942(9) -0.1132(8) 0.7947(7) 0.045(3) Uani 1 1 d .
F3 F 0.6190(9) 0.5741(7) 0.8465(6) 0.038(2) Uani 1 1 d .
F5 F 0.5650(10) -0.0485(7) 0.9182(7) 0.042(3) Uani 1 1 d .
O5 O 0.5650(11) 0.4458(8) 0.6405(7) 0.035(2) Uani 1 1 d .
O10 O 1.0334(10) 0.1660(8) 1.1254(7) 0.032(3) Uani 1 1 d .
O11 O 1.1487(10) 0.1686(8) 1.0256(7) 0.031(3) Uani 1 1 d .
O3 O 0.6993(11) -0.0554(8) 0.7711(7) 0.036(3) Uani 1 1 d .
O7 O 0.5867(11) 0.6860(8) 0.6029(7) 0.035(3) Uani 1 1 d .
O4 O 0.6016(9) 0.3849(7) 0.7555(6) 0.0237(16) Uani 1 1 d .
O8 O 0.3622(11) 0.6187(8) 0.5376(7) 0.037(3) Uani 1 1 d .
O6 O 0.7444(11) 0.4995(9) 0.7435(8) 0.038(3) Uani 1 1 d .
N3 N 0.6630(12) 0.3066(9) 0.9322(7) 0.026(3) Uani 1 1 d .
N1 N 0.4230(10) 0.1862(9) 0.7358(7) 0.022(3) Uani 1 1 d .
N2 N 0.7291(10) 0.2070(9) 0.7343(7) 0.023(3) Uani 1 1 d .
C32 C 1.0250(14) 0.1354(12) 1.1914(9) 0.030(4) Uani 1 1 d .
H32A H 1.0299 0.1932 1.2328 0.036 Uiso 1 1 calc R
H32B H 1.0846 0.1019 1.2121 0.036 Uiso 1 1 calc R
C29 C 1.1819(15) 0.1814(11) 0.9650(11) 0.030(4) Uani 1 1 d .
H29A H 1.2529 0.2273 0.9862 0.036 Uiso 1 1 calc R
H29B H 1.1289 0.2102 0.9301 0.036 Uiso 1 1 calc R
C15 C 0.6950(14) 0.1794(12) 1.0423(9) 0.029(4) Uani 1 1 d .
H15A H 0.7198 0.1353 1.0074 0.043 Uiso 1 1 calc R
H15B H 0.6544 0.1407 1.0649 0.043 Uiso 1 1 calc R
H15C H 0.7578 0.2246 1.0838 0.043 Uiso 1 1 calc R
C31 C 1.1332(17) 0.2366(11) 1.1469(10) 0.036(4) Uani 1 1 d .
H31A H 1.1960 0.2093 1.1725 0.044 Uiso 1 1 calc R
H31B H 1.1333 0.2976 1.1834 0.044 Uiso 1 1 calc R
C19 C 0.5803(14) 0.5623(11) 0.7693(10) 0.028(2) Uani 1 1 d .
C22 C 0.5173(16) 0.7509(11) 0.6089(10) 0.033(4) Uani 1 1 d .
H22A H 0.5027 0.7817 0.5653 0.039 Uiso 1 1 calc R
H22B H 0.5523 0.8035 0.6579 0.039 Uiso 1 1 calc R
C18 C 0.8387(16) 0.4541(13) 0.9198(11) 0.035(4) Uani 1 1 d .
H18A H 0.8855 0.4082 0.9117 0.052 Uiso 1 1 calc R
H18B H 0.8829 0.5203 0.9457 0.052 Uiso 1 1 calc R
H18C H 0.7858 0.4540 0.8696 0.052 Uiso 1 1 calc R
C30 C 1.1405(15) 0.2583(12) 1.0747(10) 0.033(4) Uani 1 1 d .
H30A H 1.0754 0.2816 1.0473 0.039 Uiso 1 1 calc R
H30B H 1.2050 0.3102 1.0878 0.039 Uiso 1 1 calc R
C6 C 0.4436(14) -0.0075(11) 0.6471(10) 0.030(4) Uani 1 1 d .
H6A H 0.4754 0.0239 0.6159 0.045 Uiso 1 1 calc R
H6B H 0.4014 -0.0731 0.6161 0.045 Uiso 1 1 calc R
H6C H 0.5014 -0.0132 0.6930 0.045 Uiso 1 1 calc R
C12 C 0.8961(14) 0.2249(14) 0.8868(11) 0.035(4) Uani 1 1 d .
H12A H 0.8341 0.2406 0.9002 0.052 Uiso 1 1 calc R
H12B H 0.9604 0.2761 0.9187 0.052 Uiso 1 1 calc R
H12C H 0.9091 0.1615 0.8962 0.052 Uiso 1 1 calc R
C23 C 0.4121(16) 0.6970(11) 0.6077(10) 0.034(4) Uani 1 1 d .
H23A H 0.4261 0.6697 0.6532 0.041 Uiso 1 1 calc R
H23B H 0.3628 0.7431 0.6105 0.041 Uiso 1 1 calc R
C3 C 0.3143(14) 0.3300(14) 0.6589(10) 0.035(4) Uani 1 1 d .
H3A H 0.3804 0.3491 0.6492 0.052 Uiso 1 1 calc R
H3B H 0.2829 0.3878 0.6693 0.052 Uiso 1 1 calc R
H3C H 0.2621 0.2806 0.6132 0.052 Uiso 1 1 calc R
C17 C 0.8699(16) 0.3983(12) 1.0695(9) 0.035(4) Uani 1 1 d .
H17A H 0.8411 0.3997 1.1109 0.052 Uiso 1 1 calc R
H17B H 0.9336 0.4514 1.0872 0.052 Uiso 1 1 calc R
H17C H 0.8906 0.3350 1.0562 0.052 Uiso 1 1 calc R
C7 C 0.5392(14) 0.1979(12) 0.5911(9) 0.029(4) Uani 1 1 d .
H7A H 0.4970 0.1832 0.6224 0.043 Uiso 1 1 calc R
H7B H 0.5021 0.1578 0.5375 0.043 Uiso 1 1 calc R
H7C H 0.5466 0.2676 0.5921 0.043 Uiso 1 1 calc R
C10 C 0.9475(15) 0.3328(13) 0.7778(12) 0.037(4) Uani 1 1 d .
H10A H 0.9621 0.3201 0.7296 0.056 Uiso 1 1 calc R
H10B H 1.0161 0.3528 0.8223 0.056 Uiso 1 1 calc R
H10C H 0.9064 0.3854 0.7792 0.056 Uiso 1 1 calc R
C9 C 0.6744(17) 0.0332(12) 0.5945(10) 0.036(4) Uani 1 1 d .
H9A H 0.7425 0.0247 0.5875 0.054 Uiso 1 1 calc R
H9B H 0.6141 0.0066 0.5446 0.054 Uiso 1 1 calc R
H9C H 0.6641 -0.0018 0.6318 0.054 Uiso 1 1 calc R
C16 C 0.7088(17) 0.5249(12) 1.0159(11) 0.039(4) Uani 1 1 d .
H16A H 0.6389 0.5232 0.9764 0.058 Uiso 1 1 calc R
H16B H 0.7596 0.5853 1.0239 0.058 Uiso 1 1 calc R
H16C H 0.6990 0.5231 1.0647 0.058 Uiso 1 1 calc R
C2 C 0.4223(15) 0.3796(12) 0.8361(10) 0.032(4) Uani 1 1 d .
H2A H 0.4034 0.3645 0.8788 0.048 Uiso 1 1 calc R
H2B H 0.4018 0.4415 0.8280 0.048 Uiso 1 1 calc R
H2C H 0.5005 0.3857 0.8489 0.048 Uiso 1 1 calc R
C21 C 0.6867(16) 0.7349(12) 0.6049(12) 0.038(4) Uani 1 1 d .
H21A H 0.7184 0.7924 0.6506 0.046 Uiso 1 1 calc R
H21B H 0.6757 0.7581 0.5576 0.046 Uiso 1 1 calc R
C25 C 0.2146(18) 0.4889(15) 0.4563(14) 0.052(6) Uani 1 1 d .
H25A H 0.1389 0.4589 0.4464 0.062 Uiso 1 1 calc R
H25B H 0.2151 0.5199 0.4142 0.062 Uiso 1 1 calc R
C26 C 0.2381(14) 0.3374(13) 0.3908(11) 0.036(4) Uani 1 1 d .
H26A H 0.2311 0.3635 0.3452 0.043 Uiso 1 1 calc R
H26B H 0.1653 0.3037 0.3846 0.043 Uiso 1 1 calc R
C11 C 0.9237(16) 0.1142(13) 0.7422(11) 0.038(4) Uani 1 1 d .
H11A H 0.8874 0.0525 0.7461 0.057 Uiso 1 1 calc R
H11B H 1.0015 0.1256 0.7720 0.057 Uiso 1 1 calc R
H11C H 0.9120 0.1103 0.6878 0.057 Uiso 1 1 calc R
C28 C 1.1907(15) 0.0864(13) 0.9207(11) 0.035(4) Uani 1 1 d .
H28A H 1.2431 0.0567 0.9553 0.042 Uiso 1 1 calc R
H28B H 1.2166 0.0960 0.8789 0.042 Uiso 1 1 calc R
C5 C 0.2818(15) 0.0006(15) 0.7311(12) 0.039(4) Uani 1 1 d .
H5A H 0.3328 0.0064 0.7834 0.059 Uiso 1 1 calc R
H5B H 0.2568 -0.0688 0.7023 0.059 Uiso 1 1 calc R
H5C H 0.2197 0.0289 0.7346 0.059 Uiso 1 1 calc R
C8 C 0.7646(15) 0.2352(15) 0.5898(11) 0.038(4) Uani 1 1 d .
H8A H 0.7614 0.3050 0.6014 0.057 Uiso 1 1 calc R
H8B H 0.7374 0.2074 0.5336 0.057 Uiso 1 1 calc R
H8C H 0.8397 0.2281 0.6124 0.057 Uiso 1 1 calc R
C14 C 0.5727(18) 0.3410(15) 1.0613(12) 0.043(5) Uani 1 1 d .
H14A H 0.6393 0.3867 1.0977 0.065 Uiso 1 1 calc R
H14B H 0.5402 0.3047 1.0897 0.065 Uiso 1 1 calc R
H14C H 0.5216 0.3778 1.0350 0.065 Uiso 1 1 calc R
C27 C 1.0838(14) -0.0655(13) 0.8352(11) 0.033(4) Uani 1 1 d .
H27A H 1.1427 -0.0971 0.8608 0.040 Uiso 1 1 calc R
H27B H 1.0962 -0.0500 0.7898 0.040 Uiso 1 1 calc R
C4 C 0.2465(16) 0.0745(14) 0.5873(11) 0.039(4) Uani 1 1 d .
H4A H 0.1883 0.1020 0.5991 0.059 Uiso 1 1 calc R
H4B H 0.2170 0.0081 0.5527 0.059 Uiso 1 1 calc R
H4C H 0.2787 0.1160 0.5619 0.059 Uiso 1 1 calc R
C13 C 0.4737(16) 0.1665(15) 0.9236(11) 0.041(4) Uani 1 1 d .
H13A H 0.4220 0.2044 0.8996 0.061 Uiso 1 1 calc R
H13B H 0.4453 0.1325 0.9552 0.061 Uiso 1 1 calc R
H13C H 0.4846 0.1181 0.8831 0.061 Uiso 1 1 calc R
C20 C 0.5864(14) -0.0881(11) 0.8563(10) 0.028(2) Uani 1 1 d .
C24 C 0.2617(17) 0.5640(16) 0.5329(15) 0.053(6) Uani 1 1 d .
H24A H 0.2113 0.6085 0.5375 0.063 Uiso 1 1 calc R
H24B H 0.2743 0.5314 0.5755 0.063 Uiso 1 1 calc R
C1 C 0.2182(16) 0.2373(15) 0.7570(14) 0.045(5) Uani 1 1 d .
H1A H 0.1715 0.1840 0.7118 0.068 Uiso 1 1 calc R
H1B H 0.1816 0.2927 0.7618 0.068 Uiso 1 1 calc R
H1C H 0.2332 0.2138 0.8038 0.068 Uiso 1 1 calc R
O14 O 0.964(3) 0.756(2) 0.5184(18) 0.052(7) Uiso 0.50 1 d P
C41 C 0.946(3) 0.218(2) 0.3468(18) 0.026(6) Uiso 0.50 1 d P
C33 C 0.840(5) 0.270(5) 0.293(4) 0.074(15) Uiso 0.50 1 d P
C35 C 0.931(5) 0.526(4) 0.326(3) 0.067(14) Uiso 0.50 1 d P
O15 O 0.860(4) 0.345(3) 0.277(3) 0.085(12) Uiso 0.50 1 d P
C36 C 0.999(4) 0.705(4) 0.463(3) 0.053(11) Uiso 0.50 1 d P
C37 C 0.964(5) 0.608(5) 0.417(4) 0.076(16) Uiso 0.50 1 d P
C39 C 0.965(3) 0.911(3) 0.602(2) 0.031(7) Uiso 0.50 1 d P
C38 C 1.009(3) 0.854(3) 0.541(2) 0.037(8) Uiso 0.50 1 d P
C40 C 0.899(3) 0.438(2) 0.3416(18) 0.023(6) Uiso 0.50 1 d P
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'
F F 0.0171 0.0103 '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
N2 Th1 N3 125.2(5) . .
N2 Th1 N1 121.7(4) . .
N3 Th1 N1 113.0(5) . .
N2 Th1 O1 86.5(4) . .
N3 Th1 O1 86.7(4) . .
N1 Th1 O1 94.5(4) . .
N2 Th1 O4 85.8(4) . .
N3 Th1 O4 98.5(4) . .
N1 Th1 O4 88.7(4) . .
O1 Th1 O4 172.3(4) . .
N2 Th1 Si1 133.9(3) . .
N3 Th1 Si1 97.1(4) . .
N1 Th1 Si1 26.7(3) . .
O1 Th1 Si1 116.1(3) . .
O4 Th1 Si1 69.2(3) . .
O12 K2 O12 180.000(3) . 2_757
O12 K2 O11 119.9(3) . 2_757
O12 K2 O11 60.1(3) 2_757 2_757
O12 K2 O11 60.1(3) . .
O12 K2 O11 119.9(3) 2_757 .
O11 K2 O11 180.0(3) 2_757 .
O12 K2 O10 61.1(3) . 2_757
O12 K2 O10 118.9(3) 2_757 2_757
O11 K2 O10 59.9(4) 2_757 2_757
O11 K2 O10 120.1(4) . 2_757
O12 K2 O10 118.9(3) . .
O12 K2 O10 61.1(3) 2_757 .
O11 K2 O10 120.1(4) 2_757 .
O11 K2 O10 59.9(4) . .
O10 K2 O10 180.0(5) 2_757 .
O12 K2 O2 84.9(3) . 2_757
O12 K2 O2 95.1(3) 2_757 2_757
O11 K2 O2 110.8(3) 2_757 2_757
O11 K2 O2 69.2(3) . 2_757
O10 K2 O2 95.1(3) 2_757 2_757
O10 K2 O2 84.9(3) . 2_757
O12 K2 O2 95.1(3) . .
O12 K2 O2 84.9(3) 2_757 .
O11 K2 O2 69.2(3) 2_757 .
O11 K2 O2 110.8(3) . .
O10 K2 O2 84.9(3) 2_757 .
O10 K2 O2 95.1(3) . .
O2 K2 O2 179.999(2) 2_757 .
O7 K1 O7 179.999(2) 2_666 .
O7 K1 O8 119.9(4) 2_666 .
O7 K1 O8 60.1(4) . .
O7 K1 O8 60.1(4) 2_666 2_666
O7 K1 O8 119.9(4) . 2_666
O8 K1 O8 180.0(5) . 2_666
O7 K1 O5 80.8(3) 2_666 2_666
O7 K1 O5 99.2(3) . 2_666
O8 K1 O5 84.4(4) . 2_666
O8 K1 O5 95.6(4) 2_666 2_666
O7 K1 O5 99.2(3) 2_666 .
O7 K1 O5 80.8(3) . .
O8 K1 O5 95.6(4) . .
O8 K1 O5 84.4(4) 2_666 .
O5 K1 O5 180.0(8) 2_666 .
O7 K1 O9 119.8(4) 2_666 2_666
O7 K1 O9 60.2(4) . 2_666
O8 K1 O9 119.0(3) . 2_666
O8 K1 O9 61.0(3) 2_666 2_666
O5 K1 O9 93.6(4) 2_666 2_666
O5 K1 O9 86.4(4) . 2_666
O7 K1 O9 60.2(4) 2_666 .
O7 K1 O9 119.8(4) . .
O8 K1 O9 61.0(3) . .
O8 K1 O9 119.0(3) 2_666 .
O5 K1 O9 86.4(4) 2_666 .
O5 K1 O9 93.6(4) . .
O9 K1 O9 179.999(1) 2_666 .
O2 S2 O3 115.9(8) . .
O2 S2 O1 113.6(6) . .
O3 S2 O1 113.3(7) . .
O2 S2 C20 104.8(8) . .
O3 S2 C20 105.8(8) . .
O1 S2 C20 101.7(7) . .
O6 S1 O5 117.3(8) . .
O6 S1 O4 114.7(7) . .
O5 S1 O4 113.3(7) . .
O6 S1 C19 105.5(8) . .
O5 S1 C19 103.7(8) . .
O4 S1 C19 99.6(7) . .
N3 Si5 C13 111.0(8) . .
N3 Si5 C15 112.9(7) . .
C13 Si5 C15 108.1(9) . .
N3 Si5 C14 113.8(8) . .
C13 Si5 C14 104.9(10) . .
C15 Si5 C14 105.6(9) . .
N2 Si4 C11 114.2(8) . .
N2 Si4 C10 111.9(8) . .
C11 Si4 C10 105.9(9) . .
N2 Si4 C12 109.9(7) . .
C11 Si4 C12 107.4(8) . .
C10 Si4 C12 107.2(9) . .
N1 Si2 C4 111.7(8) . .
N1 Si2 C6 111.7(7) . .
C4 Si2 C6 105.3(8) . .
N1 Si2 C5 112.0(8) . .
C4 Si2 C5 107.5(9) . .
C6 Si2 C5 108.3(8) . .
N2 Si3 C8 112.6(8) . .
N2 Si3 C9 112.0(7) . .
C8 Si3 C9 106.0(9) . .
N2 Si3 C7 110.2(7) . .
C8 Si3 C7 105.4(8) . .
C9 Si3 C7 110.4(8) . .
N3 Si6 C17 112.0(7) . .
N3 Si6 C16 113.1(8) . .
C17 Si6 C16 107.5(8) . .
N3 Si6 C18 112.3(8) . .
C17 Si6 C18 106.4(9) . .
C16 Si6 C18 105.0(8) . .
N1 Si1 C1 114.9(8) . .
N1 Si1 C3 111.5(8) . .
C1 Si1 C3 107.3(9) . .
N1 Si1 C2 111.1(7) . .
C1 Si1 C2 102.2(9) . .
C3 Si1 C2 109.4(8) . .
N1 Si1 Th1 37.0(4) . .
C1 Si1 Th1 139.3(6) . .
C3 Si1 Th1 111.2(6) . .
C2 Si1 Th1 77.2(6) . .
S2 O1 Th1 155.4(7) . .
S2 O2 K2 153.9(8) . .
C27 O12 C28 111.3(13) . .
C27 O12 K2 116.4(9) . .
C28 O12 K2 112.1(10) . .
C26 O9 C25 112.3(14) . .
C26 O9 K1 113.8(11) . .
C25 O9 K1 111.2(11) . .
S1 O5 K1 152.4(7) . .
C32 O10 C31 111.2(12) . .
C32 O10 K2 110.7(9) . .
C31 O10 K2 114.3(10) . .
C29 O11 C30 115.0(13) . .
C29 O11 K2 118.1(10) . .
C30 O11 K2 117.1(10) . .
C21 O7 C22 111.6(13) . .
C21 O7 K1 116.6(10) . .
C22 O7 K1 118.6(10) . .
S1 O4 Th1 158.0(7) . .
C24 O8 C23 112.7(15) . .
C24 O8 K1 113.5(10) . .
C23 O8 K1 115.3(11) . .
Si5 N3 Si6 117.0(7) . .
Si5 N3 Th1 120.0(7) . .
Si6 N3 Th1 122.9(7) . .
Si2 N1 Si1 117.2(7) . .
Si2 N1 Th1 126.5(7) . .
Si1 N1 Th1 116.3(6) . .
Si4 N2 Si3 117.3(8) . .
Si4 N2 Th1 122.7(7) . .
Si3 N2 Th1 120.1(6) . .
O10 C32 C27 107.9(13) . 2_757
O10 C32 H32A 110.1 . .
C27 C32 H32A 110.1 2_757 .
O10 C32 H32B 110.1 . .
C27 C32 H32B 110.1 2_757 .
H32A C32 H32B 108.4 . .
O11 C29 C28 110.3(13) . .
O11 C29 H29A 109.6 . .
C28 C29 H29A 109.6 . .
O11 C29 H29B 109.6 . .
C28 C29 H29B 109.6 . .
H29A C29 H29B 108.1 . .
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 . .
O10 C31 C30 108.0(14) . .
O10 C31 H31A 110.1 . .
C30 C31 H31A 110.1 . .
O10 C31 H31B 110.1 . .
C30 C31 H31B 110.1 . .
H31A C31 H31B 108.4 . .
F2 C19 F1 107.7(13) . .
F2 C19 F3 108.6(14) . .
F1 C19 F3 107.2(13) . .
F2 C19 S1 112.9(11) . .
F1 C19 S1 109.7(12) . .
F3 C19 S1 110.6(11) . .
O7 C22 C23 110.3(13) . .
O7 C22 H22A 109.6 . .
C23 C22 H22A 109.6 . .
O7 C22 H22B 109.6 . .
C23 C22 H22B 109.6 . .
H22A C22 H22B 108.1 . .
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 . .
O11 C30 C31 108.2(13) . .
O11 C30 H30A 110.1 . .
C31 C30 H30A 110.1 . .
O11 C30 H30B 110.1 . .
C31 C30 H30B 110.1 . .
H30A C30 H30B 108.4 . .
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 . .
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 . .
O8 C23 C22 109.9(15) . .
O8 C23 H23A 109.7 . .
C22 C23 H23A 109.7 . .
O8 C23 H23B 109.7 . .
C22 C23 H23B 109.7 . .
H23A C23 H23B 108.2 . .
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 . .
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 . .
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 . .
Si4 C10 H10A 109.5 . .
Si4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 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 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 . .
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 . .
O7 C21 C26 107.9(13) . 2_666
O7 C21 H21A 110.1 . .
C26 C21 H21A 110.1 2_666 .
O7 C21 H21B 110.1 . .
C26 C21 H21B 110.1 2_666 .
H21A C21 H21B 108.4 . .
O9 C25 C24 107.6(17) . .
O9 C25 H25A 110.2 . .
C24 C25 H25A 110.2 . .
O9 C25 H25B 110.2 . .
C24 C25 H25B 110.2 . .
H25A C25 H25B 108.5 . .
O9 C26 C21 109.8(14) . 2_666
O9 C26 H26A 109.7 . .
C21 C26 H26A 109.7 2_666 .
O9 C26 H26B 109.7 . .
C21 C26 H26B 109.7 2_666 .
H26A C26 H26B 108.2 . .
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 . .
C29 C28 O12 108.3(15) . .
C29 C28 H28A 110.0 . .
O12 C28 H28A 110.0 . .
C29 C28 H28B 110.0 . .
O12 C28 H28B 110.0 . .
H28A C28 H28B 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 . .
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 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 . .
O12 C27 C32 109.6(14) . 2_757
O12 C27 H27A 109.7 . .
C32 C27 H27A 109.7 2_757 .
O12 C27 H27B 109.7 . .
C32 C27 H27B 109.7 2_757 .
H27A C27 H27B 108.2 . .
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 . .
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 . .
F6 C20 F4 106.1(13) . .
F6 C20 F5 109.2(13) . .
F4 C20 F5 108.4(15) . .
F6 C20 S2 110.4(12) . .
F4 C20 S2 110.4(11) . .
F5 C20 S2 112.2(11) . .
O8 C24 C25 107.9(18) . .
O8 C24 H24A 110.1 . .
C25 C24 H24A 110.1 . .
O8 C24 H24B 110.1 . .
C25 C24 H24B 110.1 . .
H24A C24 H24B 108.4 . .
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 . .
C38 O14 C36 111(3) . .
O15 C33 C41 121(5) . .
C33 O15 C40 117(5) . .
C37 C36 O14 130(5) . .
O14 C38 C39 110(3) . .
C35 C40 O15 119(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Th1 N2 2.324(14) .
Th1 N3 2.335(12) .
Th1 N1 2.344(13) .
Th1 O1 2.434(10) .
Th1 O4 2.439(10) .
Th1 Si1 3.491(5) .
K2 O12 2.774(12) .
K2 O12 2.774(12) 2_757
K2 O11 2.771(12) 2_757
K2 O11 2.771(12) .
K2 O10 2.852(12) 2_757
K2 O10 2.852(12) .
K2 O2 2.931(13) 2_757
K2 O2 2.931(13) .
K1 O7 2.788(12) 2_666
K1 O7 2.789(12) .
K1 O8 2.803(13) .
K1 O8 2.803(13) 2_666
K1 O5 2.815(11) 2_666
K1 O5 2.815(11) .
K1 O9 2.824(13) 2_666
K1 O9 2.824(13) .
S2 O2 1.418(13) .
S2 O3 1.435(12) .
S2 O1 1.490(10) .
S2 C20 1.834(17) .
S1 O6 1.438(14) .
S1 O5 1.431(12) .
S1 O4 1.482(11) .
S1 C19 1.834(17) .
Si5 N3 1.727(15) .
Si5 C13 1.87(2) .
Si5 C15 1.867(17) .
Si5 C14 1.905(19) .
Si4 N2 1.731(13) .
Si4 C11 1.876(19) .
Si4 C10 1.878(19) .
Si4 C12 1.870(19) .
Si2 N1 1.740(13) .
Si2 C4 1.859(18) .
Si2 C6 1.893(18) .
Si2 C5 1.904(19) .
Si3 N2 1.762(13) .
Si3 C8 1.871(19) .
Si3 C9 1.900(16) .
Si3 C7 1.905(17) .
Si6 N3 1.779(15) .
Si6 C17 1.860(17) .
Si6 C16 1.892(18) .
Si6 C18 1.905(17) .
Si1 N1 1.750(14) .
Si1 C1 1.86(2) .
Si1 C3 1.874(18) .
Si1 C2 1.889(18) .
F1 C19 1.352(17) .
F2 C19 1.32(2) .
F6 C20 1.323(17) .
O12 C27 1.42(2) .
O12 C28 1.45(2) .
O9 C26 1.41(2) .
O9 C25 1.44(2) .
F4 C20 1.33(2) .
F3 C19 1.346(19) .
F5 C20 1.33(2) .
O10 C32 1.44(2) .
O10 C31 1.45(2) .
O11 C29 1.40(2) .
O11 C30 1.45(2) .
O7 C21 1.42(2) .
O7 C22 1.40(2) .
O8 C24 1.43(3) .
O8 C23 1.44(2) .
C32 C27 1.52(2) 2_757
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C29 C28 1.47(2) .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C31 C30 1.49(3) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C22 C23 1.51(3) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C21 C26 1.52(3) 2_666
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C25 C24 1.49(3) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 C21 1.52(3) 2_666
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C27 C32 1.52(2) 2_757
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
O14 C38 1.38(5) .
O14 C36 1.39(5) .
C41 C33 1.80(7) .
C33 O15 1.19(7) .
C35 C40 1.39(6) .
O15 C40 1.51(5) .
C36 C37 1.40(8) .
C39 C38 1.59(5) .
