#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:46:32 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233336 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/87/4348784.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_4348784
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 U'
_chemical_formula_weight         1394.88
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.370(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.095(3)
_cell_length_b                   23.499(4)
_cell_length_c                   19.344(4)
_cell_measurement_reflns_used    19633
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.00
_cell_measurement_theta_min      12.62
_cell_volume                     6178(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40590
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         8.790
_refine_diff_density_min         -2.385
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       0.00029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         13643
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0101P)²+198.2388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1950
_reflns_number_gt                10335
_reflns_number_total             13643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01618_si_001.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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      P2(1)/n
_cod_database_code               4348784
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.75555(3) 0.404431(17) 0.74910(2) 0.01305(12) Uani 1 1 d .
K1 K 1.0000 0.5000 0.5000 0.0228(8) Uani 1 2 d S
S1 S 0.9945(2) 0.42719(13) 0.69841(16) 0.0187(6) Uani 1 1 d .
K2 K 0.5000 0.5000 1.0000 0.0338(11) Uani 1 2 d S
S2 S 0.5252(2) 0.45033(14) 0.79980(17) 0.0240(7) Uani 1 1 d .
Si2 Si 0.7529(2) 0.29971(15) 0.61991(16) 0.0188(7) Uani 1 1 d .
Si3 Si 0.7663(3) 0.54342(15) 0.69304(19) 0.0245(8) Uani 1 1 d .
Si5 Si 0.7118(2) 0.29393(14) 0.85622(16) 0.0172(6) Uani 1 1 d .
Si6 Si 0.9142(3) 0.33906(17) 0.90202(17) 0.0241(7) Uani 1 1 d .
Si1 Si 0.5822(2) 0.37805(16) 0.58132(17) 0.0231(7) Uani 1 1 d .
Si4 Si 0.8087(4) 0.52831(17) 0.8520(2) 0.0380(10) Uani 1 1 d .
F4 F 0.4105(6) 0.3817(4) 0.7081(4) 0.0328(18) Uani 1 1 d .
F5 F 0.4403(6) 0.3542(4) 0.8178(4) 0.036(2) Uani 1 1 d .
F3 F 1.1630(5) 0.3822(3) 0.7003(4) 0.0335(18) Uani 1 1 d .
F1 F 1.0999(6) 0.3499(4) 0.7815(4) 0.0348(19) Uani 1 1 d .
F2 F 1.0421(5) 0.3226(3) 0.6716(4) 0.0326(18) Uani 1 1 d .
F6 F 0.3415(5) 0.4245(4) 0.7802(4) 0.039(2) Uani 1 1 d .
O7 O 1.1521(6) 0.5571(4) 0.5999(5) 0.029(2) Uani 1 1 d .
N2 N 0.7763(7) 0.4981(4) 0.7654(5) 0.0172(14) Uani 1 1 d .
O3 O 0.9782(6) 0.4386(4) 0.6242(5) 0.029(2) Uani 1 1 d .
O1 O 0.9085(5) 0.4013(4) 0.7165(4) 0.0188(17) Uani 1 1 d .
O2 O 1.0431(6) 0.4690(4) 0.7476(5) 0.030(2) Uani 1 1 d .
O9 O 1.0390(7) 0.3953(4) 0.4451(5) 0.029(2) Uani 1 1 d .
O8 O 1.1704(6) 0.4431(4) 0.5622(5) 0.027(2) Uani 1 1 d .
O6 O 0.5412(6) 0.4576(4) 0.8757(5) 0.027(2) Uani 1 1 d .
N1 N 0.6900(7) 0.3579(4) 0.6438(5) 0.016(2) Uani 1 1 d .
O4 O 0.6049(6) 0.4179(4) 0.7799(4) 0.0205(18) Uani 1 1 d .
O5 O 0.4921(7) 0.4980(4) 0.7550(5) 0.037(2) Uani 1 1 d .
N3 N 0.7982(7) 0.3418(4) 0.8393(5) 0.0172(14) Uani 1 1 d .
O12 O 0.3949(10) 0.4013(6) 1.0141(7) 0.060(4) Uani 1 1 d .
C15 C 0.6521(10) 0.3196(6) 0.9262(6) 0.025(3) Uani 1 1 d .
H15A H 0.7005 0.3196 0.9731 0.037 Uiso 1 1 calc R
H15B H 0.5974 0.2943 0.9277 0.037 Uiso 1 1 calc R
H15C H 0.6272 0.3583 0.9144 0.037 Uiso 1 1 calc R
C13 C 0.6136(10) 0.2773(6) 0.7736(7) 0.027(3) Uani 1 1 d .
H13A H 0.5886 0.3128 0.7488 0.040 Uiso 1 1 calc R
H13B H 0.5599 0.2572 0.7865 0.040 Uiso 1 1 calc R
H13C H 0.6407 0.2533 0.7420 0.040 Uiso 1 1 calc R
C20 C 0.4235(9) 0.3985(6) 0.7749(7) 0.029(3) Uani 1 1 d .
C19 C 1.0791(8) 0.3673(6) 0.7141(6) 0.020(2) Uani 1 1 d .
O11 O 0.3160(7) 0.4781(5) 0.9106(5) 0.054(3) Uani 1 1 d D
O10 O 0.4052(8) 0.5903(6) 0.9136(6) 0.067(4) Uani 1 1 d D
C21 C 1.0483(12) 0.6347(6) 0.5950(8) 0.039(4) Uani 1 1 d .
H21A H 1.0836 0.6517 0.5621 0.047 Uiso 1 1 calc R
H21B H 1.0303 0.6655 0.6241 0.047 Uiso 1 1 calc R
C14 C 0.7646(11) 0.2226(6) 0.8877(7) 0.031(3) Uani 1 1 d .
H14A H 0.7872 0.2041 0.8495 0.046 Uiso 1 1 calc R
H14B H 0.7141 0.1990 0.8999 0.046 Uiso 1 1 calc R
H14C H 0.8203 0.2273 0.9301 0.046 Uiso 1 1 calc R
C17 C 0.9076(10) 0.3349(7) 0.9981(6) 0.034(2) Uani 1 1 d .
H17A H 0.8669 0.3661 1.0078 0.051 Uiso 1 1 calc R
H17B H 0.9740 0.3378 1.0303 0.051 Uiso 1 1 calc R
H17C H 0.8783 0.2984 1.0060 0.051 Uiso 1 1 calc R
C23 C 1.2239(10) 0.5187(7) 0.6439(7) 0.037(4) Uani 1 1 d .
H23A H 1.1945 0.4984 0.6780 0.045 Uiso 1 1 calc R
H23B H 1.2815 0.5406 0.6718 0.045 Uiso 1 1 calc R
C5 C 0.8242(11) 0.3222(7) 0.5547(7) 0.034(3) Uani 1 1 d .
H5A H 0.7790 0.3269 0.5069 0.050 Uiso 1 1 calc R
H5B H 0.8731 0.2929 0.5528 0.050 Uiso 1 1 calc R
H5C H 0.8577 0.3583 0.5704 0.050 Uiso 1 1 calc R
C6 C 0.8400(9) 0.2674(6) 0.6995(7) 0.027(3) Uani 1 1 d .
H6A H 0.8928 0.2945 0.7200 0.041 Uiso 1 1 calc R
H6B H 0.8683 0.2327 0.6851 0.041 Uiso 1 1 calc R
H6C H 0.8049 0.2579 0.7355 0.041 Uiso 1 1 calc R
C22 C 1.1090(12) 0.5927(7) 0.6408(8) 0.041(4) Uani 1 1 d .
H22A H 1.1610 0.6120 0.6780 0.049 Uiso 1 1 calc R
H22B H 1.0684 0.5699 0.6650 0.049 Uiso 1 1 calc R
C18 C 0.9878(10) 0.4050(7) 0.8986(7) 0.037(3) Uani 1 1 d .
H18A H 0.9786 0.4165 0.8486 0.056 Uiso 1 1 calc R
H18B H 1.0576 0.3973 0.9206 0.056 Uiso 1 1 calc R
H18C H 0.9655 0.4356 0.9250 0.056 Uiso 1 1 calc R
C32 C 0.3167(15) 0.3871(10) 0.9500(10) 0.070(5) Uani 1 1 d .
H32A H 0.3460 0.3731 0.9120 0.084 Uiso 1 1 calc R
H32B H 0.2748 0.3566 0.9613 0.084 Uiso 1 1 calc R
C12 C 0.7345(16) 0.5912(7) 0.8576(9) 0.057(4) Uani 1 1 d .
H12A H 0.7479 0.6211 0.8262 0.086 Uiso 1 1 calc R
H12B H 0.7512 0.6051 0.9072 0.086 Uiso 1 1 calc R
H12C H 0.6645 0.5812 0.8426 0.086 Uiso 1 1 calc R
C26 C 1.1001(11) 0.3609(6) 0.5007(7) 0.033(3) Uani 1 1 d .
H26A H 1.1138 0.3239 0.4808 0.040 Uiso 1 1 calc R
H26B H 1.0663 0.3535 0.5386 0.040 Uiso 1 1 calc R
C4 C 0.6699(11) 0.2413(6) 0.5773(7) 0.033(3) Uani 1 1 d .
H4A H 0.6294 0.2297 0.6089 0.050 Uiso 1 1 calc R
H4B H 0.7091 0.2089 0.5689 0.050 Uiso 1 1 calc R
H4C H 0.6272 0.2545 0.5314 0.050 Uiso 1 1 calc R
C9 C 0.8718(10) 0.5928(6) 0.7088(8) 0.036(2) Uani 1 1 d .
H9A H 0.8659 0.6215 0.7442 0.053 Uiso 1 1 calc R
H9B H 0.8724 0.6117 0.6637 0.053 Uiso 1 1 calc R
H9C H 0.9332 0.5715 0.7268 0.053 Uiso 1 1 calc R
C8 C 0.6490(10) 0.5848(6) 0.6733(9) 0.036(2) Uani 1 1 d .
H8A H 0.5978 0.5620 0.6858 0.053 Uiso 1 1 calc R
H8B H 0.6285 0.5943 0.6221 0.053 Uiso 1 1 calc R
H8C H 0.6593 0.6200 0.7016 0.053 Uiso 1 1 calc R
C24 C 1.2551(9) 0.4777(7) 0.5968(7) 0.034(3) Uani 1 1 d .
H24A H 1.2798 0.4980 0.5602 0.041 Uiso 1 1 calc R
H24B H 1.3086 0.4533 0.6252 0.041 Uiso 1 1 calc R
C25 C 1.1947(11) 0.3925(6) 0.5314(7) 0.035(4) Uani 1 1 d .
H25A H 1.2402 0.3691 0.5683 0.042 Uiso 1 1 calc R
H25B H 1.2271 0.4016 0.4932 0.042 Uiso 1 1 calc R
C7 C 0.7673(10) 0.4999(6) 0.6101(7) 0.029(3) Uani 1 1 d .
H7A H 0.8311 0.5044 0.5993 0.044 Uiso 1 1 calc R
H7B H 0.7148 0.5132 0.5693 0.044 Uiso 1 1 calc R
H7C H 0.7567 0.4596 0.6191 0.044 Uiso 1 1 calc R
C3 C 0.5988(11) 0.3837(7) 0.4884(7) 0.037(3) Uani 1 1 d .
H3A H 0.6580 0.4060 0.4898 0.056 Uiso 1 1 calc R
H3B H 0.5413 0.4025 0.4570 0.056 Uiso 1 1 calc R
H3C H 0.6057 0.3455 0.4700 0.056 Uiso 1 1 calc R
C2 C 0.5388(10) 0.4486(6) 0.6027(8) 0.031(3) Uani 1 1 d .
H2A H 0.5102 0.4451 0.6434 0.047 Uiso 1 1 calc R
H2B H 0.4889 0.4630 0.5609 0.047 Uiso 1 1 calc R
H2C H 0.5944 0.4752 0.6149 0.047 Uiso 1 1 calc R
C16 C 0.9904(10) 0.2779(7) 0.8864(7) 0.034(2) Uani 1 1 d .
H16A H 0.9624 0.2423 0.8985 0.051 Uiso 1 1 calc R
H16B H 1.0579 0.2822 0.9165 0.051 Uiso 1 1 calc R
H16C H 0.9909 0.2772 0.8358 0.051 Uiso 1 1 calc R
O13 O 0.2794(15) 0.6939(9) 0.7550(11) 0.108(6) Uiso 1 1 d .
C1 C 0.4777(9) 0.3275(7) 0.5756(7) 0.036(4) Uani 1 1 d .
H1A H 0.4896 0.2924 0.5520 0.054 Uiso 1 1 calc R
H1B H 0.4163 0.3450 0.5478 0.054 Uiso 1 1 calc R
H1C H 0.4725 0.3188 0.6240 0.054 Uiso 1 1 calc R
C10 C 0.9416(15) 0.5513(7) 0.8822(9) 0.057(4) Uani 1 1 d .
H10A H 0.9809 0.5281 0.8581 0.086 Uiso 1 1 calc R
H10B H 0.9660 0.5463 0.9342 0.086 Uiso 1 1 calc R
H10C H 0.9468 0.5915 0.8700 0.086 Uiso 1 1 calc R
C28 C 0.4686(15) 0.6270(9) 0.8914(13) 0.067(6) Uani 1 1 d .
H28A H 0.4324 0.6608 0.8674 0.080 Uiso 1 1 calc R
H28B H 0.4995 0.6076 0.8575 0.080 Uiso 1 1 calc R
C31 C 0.2583(15) 0.4364(10) 0.9252(10) 0.070(5) Uani 1 1 d .
H31A H 0.2058 0.4270 0.8815 0.084 Uiso 1 1 calc R
H31B H 0.2267 0.4496 0.9624 0.084 Uiso 1 1 calc R
C27 C 0.544(2) 0.6440(11) 0.9564(15) 0.095(10) Uani 1 1 d .
H27A H 0.5838 0.6753 0.9446 0.114 Uiso 1 1 calc R
H27B H 0.5109 0.6584 0.9923 0.114 Uiso 1 1 calc R
C36 C 0.172(3) 0.7189(17) 0.820(2) 0.151(14) Uiso 1 1 d .
H36A H 0.1370 0.6826 0.8127 0.227 Uiso 1 1 calc R
H36B H 0.1275 0.7495 0.8246 0.227 Uiso 1 1 calc R
H36C H 0.2270 0.7169 0.8634 0.227 Uiso 1 1 calc R
C34 C 0.333(2) 0.7057(13) 0.6975(17) 0.109(9) Uiso 1 1 d .
H34A H 0.3675 0.7426 0.7068 0.131 Uiso 1 1 calc R
H34B H 0.2848 0.7074 0.6497 0.131 Uiso 1 1 calc R
C11 C 0.7838(10) 0.4766(6) 0.9192(7) 0.028(3) Uani 1 1 d .
H11A H 0.7189 0.4844 0.9267 0.043 Uiso 1 1 calc R
H11B H 0.8343 0.4806 0.9647 0.043 Uiso 1 1 calc R
H11C H 0.7850 0.4377 0.9012 0.043 Uiso 1 1 calc R
C33 C 0.406(2) 0.6576(13) 0.6994(17) 0.116(10) Uiso 1 1 d .
H33A H 0.4700 0.6680 0.7316 0.174 Uiso 1 1 calc R
H33B H 0.4136 0.6512 0.6510 0.174 Uiso 1 1 calc R
H33C H 0.3822 0.6227 0.7168 0.174 Uiso 1 1 calc R
C35 C 0.214(3) 0.7310(18) 0.754(2) 0.162(16) Uiso 1 1 d .
H35A H 0.1603 0.7284 0.7094 0.194 Uiso 1 1 calc R
H35B H 0.2422 0.7697 0.7580 0.194 Uiso 1 1 calc R
C29 C 0.2627(9) 0.5261(6) 0.8766(10) 0.078(5) Uani 1 1 d D
H29A H 0.2277 0.5434 0.9095 0.093 Uiso 1 1 calc R
H29B H 0.2126 0.5133 0.8331 0.093 Uiso 1 1 calc R
C30 C 0.3281(11) 0.5713(6) 0.8553(7) 0.078(5) Uani 1 1 d D
H30A H 0.3569 0.5553 0.8180 0.093 Uiso 1 1 calc R
H30B H 0.2869 0.6043 0.8341 0.093 Uiso 1 1 calc R
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'
U U -9.6767 9.6646 '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'
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 U1 N3 122.7(3) . .
N2 U1 N1 127.3(3) . .
N3 U1 N1 110.0(4) . .
N2 U1 O4 85.7(3) . .
N3 U1 O4 88.0(3) . .
N1 U1 O4 96.3(3) . .
N2 U1 O1 88.5(3) . .
N3 U1 O1 96.4(3) . .
N1 U1 O1 86.0(3) . .
O4 U1 O1 174.0(3) . .
O8 K1 O8 179.999(1) 3_766 .
O8 K1 O9 59.8(3) 3_766 3_766
O8 K1 O9 120.2(3) . 3_766
O8 K1 O9 120.2(3) 3_766 .
O8 K1 O9 59.8(3) . .
O9 K1 O9 179.999(1) 3_766 .
O8 K1 O7 60.7(3) 3_766 3_766
O8 K1 O7 119.3(3) . 3_766
O9 K1 O7 119.4(3) 3_766 3_766
O9 K1 O7 60.7(3) . 3_766
O8 K1 O7 119.3(3) 3_766 .
O8 K1 O7 60.7(3) . .
O9 K1 O7 60.6(3) 3_766 .
O9 K1 O7 119.4(3) . .
O7 K1 O7 180.0(3) 3_766 .
O8 K1 O3 109.6(2) 3_766 .
O8 K1 O3 70.4(2) . .
O9 K1 O3 92.8(3) 3_766 .
O9 K1 O3 87.2(3) . .
O7 K1 O3 95.9(3) 3_766 .
O7 K1 O3 84.1(3) . .
O8 K1 O3 70.4(2) 3_766 3_766
O8 K1 O3 109.6(2) . 3_766
O9 K1 O3 87.2(3) 3_766 3_766
O9 K1 O3 92.8(3) . 3_766
O7 K1 O3 84.1(3) 3_766 3_766
O7 K1 O3 95.9(3) . 3_766
O3 K1 O3 179.999(1) . 3_766
O8 K1 C22 79.0(3) 3_766 3_766
O8 K1 C22 101.0(3) . 3_766
O9 K1 C22 138.8(3) 3_766 3_766
O9 K1 C22 41.2(3) . 3_766
O7 K1 C22 22.2(3) 3_766 3_766
O7 K1 C22 157.8(3) . 3_766
O3 K1 C22 102.4(3) . 3_766
O3 K1 C22 77.6(3) 3_766 3_766
O8 K1 C22 101.0(3) 3_766 .
O8 K1 C22 79.0(3) . .
O9 K1 C22 41.2(3) 3_766 .
O9 K1 C22 138.8(3) . .
O7 K1 C22 157.8(3) 3_766 .
O7 K1 C22 22.2(3) . .
O3 K1 C22 77.6(3) . .
O3 K1 C22 102.4(3) 3_766 .
C22 K1 C22 179.999(1) 3_766 .
O2 S1 O3 118.0(6) . .
O2 S1 O1 114.1(5) . .
O3 S1 O1 113.2(5) . .
O2 S1 C19 104.3(6) . .
O3 S1 C19 103.8(5) . .
O1 S1 C19 100.7(5) . .
O11 K2 O11 180.0(7) . 3_667
O11 K2 O6 76.7(3) . .
O11 K2 O6 103.3(3) 3_667 .
O11 K2 O6 103.3(3) . 3_667
O11 K2 O6 76.7(3) 3_667 3_667
O6 K2 O6 179.999(2) . 3_667
O11 K2 O12 58.2(4) . .
O11 K2 O12 121.8(4) 3_667 .
O6 K2 O12 91.4(3) . .
O6 K2 O12 88.6(3) 3_667 .
O11 K2 O12 121.8(4) . 3_667
O11 K2 O12 58.2(4) 3_667 3_667
O6 K2 O12 88.6(3) . 3_667
O6 K2 O12 91.4(3) 3_667 3_667
O12 K2 O12 180.0(3) . 3_667
O11 K2 O10 63.1(3) . .
O11 K2 O10 116.9(3) 3_667 .
O6 K2 O10 86.1(3) . .
O6 K2 O10 93.9(3) 3_667 .
O12 K2 O10 120.2(4) . .
O12 K2 O10 59.8(4) 3_667 .
O11 K2 O10 116.9(3) . 3_667
O11 K2 O10 63.1(3) 3_667 3_667
O6 K2 O10 93.9(3) . 3_667
O6 K2 O10 86.1(3) 3_667 3_667
O12 K2 O10 59.8(4) . 3_667
O12 K2 O10 120.2(4) 3_667 3_667
O10 K2 O10 180.000(3) . 3_667
O5 S2 O6 117.9(6) . .
O5 S2 O4 113.2(5) . .
O6 S2 O4 113.6(5) . .
O5 S2 C20 104.8(6) . .
O6 S2 C20 104.2(6) . .
O4 S2 C20 100.5(5) . .
N1 Si2 C4 113.0(6) . .
N1 Si2 C6 111.6(5) . .
C4 Si2 C6 105.5(7) . .
N1 Si2 C5 110.7(6) . .
C4 Si2 C5 107.2(7) . .
C6 Si2 C5 108.5(6) . .
N2 Si3 C9 111.3(6) . .
N2 Si3 C8 111.3(6) . .
C9 Si3 C8 109.6(6) . .
N2 Si3 C7 109.4(5) . .
C9 Si3 C7 106.9(6) . .
C8 Si3 C7 108.2(7) . .
N3 Si5 C13 111.8(5) . .
N3 Si5 C14 113.6(6) . .
C13 Si5 C14 103.5(6) . .
N3 Si5 C15 113.3(5) . .
C13 Si5 C15 108.3(6) . .
C14 Si5 C15 105.7(6) . .
N3 Si6 C16 112.7(6) . .
N3 Si6 C18 111.6(6) . .
C16 Si6 C18 106.5(7) . .
N3 Si6 C17 113.6(5) . .
C16 Si6 C17 107.5(6) . .
C18 Si6 C17 104.5(6) . .
N1 Si1 C2 111.6(6) . .
N1 Si1 C1 113.4(6) . .
C2 Si1 C1 106.3(6) . .
N1 Si1 C3 112.2(6) . .
C2 Si1 C3 106.4(7) . .
C1 Si1 C3 106.5(7) . .
N2 Si4 C12 111.9(7) . .
N2 Si4 C11 110.3(5) . .
C12 Si4 C11 105.5(7) . .
N2 Si4 C10 113.3(6) . .
C12 Si4 C10 106.6(9) . .
C11 Si4 C10 108.9(7) . .
C22 O7 C23 112.4(11) . .
C22 O7 K1 108.0(8) . .
C23 O7 K1 113.1(8) . .
Si3 N2 Si4 117.7(6) . .
Si3 N2 U1 120.8(5) . .
Si4 N2 U1 121.4(5) . .
S1 O3 K1 155.8(6) . .
S1 O1 U1 154.0(5) . .
C26 O9 C21 112.5(11) . 3_766
C26 O9 K1 110.6(7) . .
C21 O9 K1 114.0(8) 3_766 .
C25 O8 C24 113.7(10) . .
C25 O8 K1 120.6(8) . .
C24 O8 K1 116.7(8) . .
S2 O6 K2 155.2(5) . .
Si1 N1 Si2 116.0(5) . .
Si1 N1 U1 124.3(5) . .
Si2 N1 U1 119.6(5) . .
S2 O4 U1 156.8(5) . .
Si5 N3 Si6 114.4(5) . .
Si5 N3 U1 120.8(5) . .
Si6 N3 U1 124.7(5) . .
C27 O12 C32 114.8(17) 3_667 .
C27 O12 K2 112.6(12) 3_667 .
C32 O12 K2 113.8(12) . .
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 . .
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 . .
F5 C20 F4 109.6(12) . .
F5 C20 F6 109.2(10) . .
F4 C20 F6 108.3(10) . .
F5 C20 S2 111.2(9) . .
F4 C20 S2 110.6(9) . .
F6 C20 S2 107.9(10) . .
F1 C19 F3 107.7(9) . .
F1 C19 F2 108.0(11) . .
F3 C19 F2 107.6(9) . .
F1 C19 S1 111.7(8) . .
F3 C19 S1 110.0(9) . .
F2 C19 S1 111.7(8) . .
C31 O11 C29 113.5(14) . .
C31 O11 K2 121.5(12) . .
C29 O11 K2 115.9(8) . .
C28 O10 C30 111.7(14) . .
C28 O10 K2 114.2(11) . .
C30 O10 K2 112.3(9) . .
C22 C21 O9 106.0(12) . 3_766
C22 C21 H21A 110.5 . .
O9 C21 H21A 110.5 3_766 .
C22 C21 H21B 110.5 . .
O9 C21 H21B 110.5 3_766 .
H21A C21 H21B 108.7 . .
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 . .
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 . .
O7 C23 C24 108.7(11) . .
O7 C23 H23A 110.0 . .
C24 C23 H23A 110.0 . .
O7 C23 H23B 110.0 . .
C24 C23 H23B 110.0 . .
H23A C23 H23B 108.3 . .
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 . .
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 . .
O7 C22 C21 109.8(12) . .
O7 C22 K1 49.8(7) . .
C21 C22 K1 83.3(9) . .
O7 C22 H22A 109.7 . .
C21 C22 H22A 109.7 . .
K1 C22 H22A 159.4 . .
O7 C22 H22B 109.7 . .
C21 C22 H22B 109.7 . .
K1 C22 H22B 80.9 . .
H22A C22 H22B 108.2 . .
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 . .
C31 C32 O12 109.8(16) . .
C31 C32 H32A 109.7 . .
O12 C32 H32A 109.7 . .
C31 C32 H32B 109.7 . .
O12 C32 H32B 109.7 . .
H32A C32 H32B 108.2 . .
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 . .
O9 C26 C25 108.0(11) . .
O9 C26 H26A 110.1 . .
C25 C26 H26A 110.1 . .
O9 C26 H26B 110.1 . .
C25 C26 H26B 110.1 . .
H26A C26 H26B 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 . .
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 . .
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 . .
O8 C24 C23 107.9(10) . .
O8 C24 H24A 110.1 . .
C23 C24 H24A 110.1 . .
O8 C24 H24B 110.1 . .
C23 C24 H24B 110.1 . .
H24A C24 H24B 108.4 . .
O8 C25 C26 107.1(10) . .
O8 C25 H25A 110.3 . .
C26 C25 H25A 110.3 . .
O8 C25 H25B 110.3 . .
C26 C25 H25B 110.3 . .
H25A C25 H25B 108.5 . .
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 . .
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 . .
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 . .
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 . .
C35 O13 C34 112(3) . .
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 . .
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 . .
O10 C28 C27 106.3(17) . .
O10 C28 H28A 110.5 . .
C27 C28 H28A 110.5 . .
O10 C28 H28B 110.5 . .
C27 C28 H28B 110.5 . .
H28A C28 H28B 108.7 . .
O11 C31 C32 109.4(17) . .
O11 C31 H31A 109.8 . .
C32 C31 H31A 109.8 . .
O11 C31 H31B 109.8 . .
C32 C31 H31B 109.8 . .
H31A C31 H31B 108.2 . .
O12 C27 C28 111.8(18) 3_667 .
O12 C27 H27A 109.3 3_667 .
C28 C27 H27A 109.3 . .
O12 C27 H27B 109.3 3_667 .
C28 C27 H27B 109.3 . .
H27A C27 H27B 107.9 . .
C35 C36 H36A 109.5 . .
C35 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C35 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
O13 C34 C33 108(2) . .
O13 C34 H34A 110.1 . .
C33 C34 H34A 110.1 . .
O13 C34 H34B 110.1 . .
C33 C34 H34B 110.1 . .
H34A C34 H34B 108.4 . .
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 . .
C34 C33 H33A 109.5 . .
C34 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C34 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
O13 C35 C36 107(3) . .
O13 C35 H35A 110.2 . .
C36 C35 H35A 110.2 . .
O13 C35 H35B 110.2 . .
C36 C35 H35B 110.2 . .
H35A C35 H35B 108.5 . .
O11 C29 C30 113.2(8) . .
O11 C29 H29A 108.9 . .
C30 C29 H29A 108.9 . .
O11 C29 H29B 108.9 . .
C30 C29 H29B 108.9 . .
H29A C29 H29B 107.8 . .
O10 C30 C29 113.1(9) . .
O10 C30 H30A 109.0 . .
C29 C30 H30A 109.0 . .
O10 C30 H30B 109.0 . .
C29 C30 H30B 109.0 . .
H30A C30 H30B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N2 2.232(10) .
U1 N3 2.240(10) .
U1 N1 2.280(9) .
U1 O4 2.374(7) .
U1 O1 2.402(7) .
K1 O8 2.733(8) 3_766
K1 O8 2.733(8) .
K1 O9 2.792(9) 3_766
K1 O9 2.792(9) .
K1 O7 2.817(9) 3_766
K1 O7 2.817(9) .
K1 O3 2.887(8) .
K1 O3 2.887(8) 3_766
K1 C22 3.508(16) 3_766
K1 C22 3.508(16) .
S1 O2 1.413(10) .
S1 O3 1.419(9) .
S1 O1 1.480(8) .
S1 C19 1.817(13) .
K2 O11 2.758(10) .
K2 O11 2.758(10) 3_667
K2 O6 2.802(8) .
K2 O6 2.802(8) 3_667
K2 O12 2.804(13) .
K2 O12 2.804(13) 3_667
K2 O10 2.809(14) .
K2 O10 2.809(14) 3_667
S2 O5 1.418(10) .
S2 O6 1.435(9) .
S2 O4 1.489(8) .
S2 C20 1.844(15) .
Si2 N1 1.758(10) .
Si2 C4 1.850(14) .
Si2 C6 1.858(13) .
Si2 C5 1.885(14) .
Si3 N2 1.734(10) .
Si3 C9 1.847(14) .
Si3 C8 1.868(14) .
Si3 C7 1.906(13) .
Si5 N3 1.751(10) .
Si5 C13 1.856(13) .
Si5 C14 1.870(13) .
Si5 C15 1.872(12) .
Si6 N3 1.761(10) .
Si6 C16 1.865(15) .
Si6 C18 1.875(15) .
Si6 C17 1.888(12) .
Si1 N1 1.737(10) .
Si1 C2 1.852(14) .
Si1 C1 1.872(14) .
Si1 C3 1.878(13) .
Si4 N2 1.766(9) .
Si4 C12 1.832(19) .
Si4 C11 1.880(13) .
Si4 C10 1.89(2) .
F4 C20 1.318(14) .
F5 C20 1.314(15) .
F3 C19 1.327(13) .
F1 C19 1.323(13) .
F2 C19 1.351(14) .
F6 C20 1.335(14) .
O7 C22 1.395(16) .
O7 C23 1.452(18) .
O9 C26 1.435(16) .
O9 C21 1.453(18) 3_766
O8 C25 1.412(16) .
O8 C24 1.452(16) .
O12 C27 1.39(3) 3_667
O12 C32 1.46(2) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
O11 C31 1.35(2) .
O11 C29 1.417(9) .
O10 C28 1.39(2) .
O10 C30 1.416(9) .
C21 C22 1.45(2) .
C21 O9 1.453(18) 3_766
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C23 C24 1.47(2) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C32 C31 1.43(3) .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C26 C25 1.50(2) .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
O13 C35 1.27(4) .
O13 C34 1.52(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C28 C27 1.47(3) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C27 O12 1.39(3) 3_667
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C36 C35 1.55(5) .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C34 C33 1.53(4) .
C34 H34A 0.9900 .
C34 H34B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C29 C30 1.534(9) .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
