# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NL_3_122_crown_0m
_database_code_depnum_ccdc_archive 'CCDC 2325807'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2024-01-15 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H82 I2 K O9 Si8 U, C4 H10 O'
_chemical_formula_sum            'C36 H92 I2 K O10 Si8 U'
_chemical_formula_weight         1440.74

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'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.4213(5)
_cell_length_b                   15.8641(6)
_cell_length_c                   16.3965(6)
_cell_angle_alpha                104.442(2)
_cell_angle_beta                 102.934(2)
_cell_angle_gamma                96.066(2)
_cell_volume                     3246.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9755
_cell_measurement_theta_min      2.3309
_cell_measurement_theta_max      33.0908

_exptl_crystal_description       block
_exptl_crystal_colour            green-blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_F_000             1434
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.702
_shelx_estimated_absorpt_T_min   0.483
_shelx_estimated_absorpt_T_max   0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_measurement_device_type  
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074

_diffrn_reflns_number            74723
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.294
_diffrn_reflns_theta_max         33.162
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             23927
_reflns_number_gt                19239
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex4 v2021.4-0 (Bruker, 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1275(Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Co-crystallized solvent diethyl ether was positionally disordered and refined 
as two separate ether molecules (O1E > C4E and O1EB > C4EB).  The 1,2 and 1,3 
bond distances were restrained to be similar to each other.  The Uij 
components of the anisotropic displacement parameters for the disordered 
atoms closer to each other than 2.0 Angstrom were restrained to be similar 
within a standard deviation of 0.01 Angstrom squared.
Subject to these conditions, the occupancy ratio of the positionally 
disordered moiety refined to 0.721(11) : 0.279(11).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+0.5905P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         23927
_refine_ls_number_parameters     591
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0595
_refine_ls_wR_factor_gt          0.0554
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.33060(2) 0.77062(2) 0.81481(2) 0.02406(2) Uani 1 1 d . . . . .
I1 I 0.23651(2) 0.87041(2) 0.96151(2) 0.04700(5) Uani 1 1 d . . . . .
Si1 Si 0.09497(4) 0.75723(4) 0.65922(4) 0.02841(12) Uani 1 1 d . . . . .
Si2 Si 0.23221(5) 0.86997(4) 0.68378(4) 0.02868(12) Uani 1 1 d . . . . .
Si3 Si 0.16995(6) 1.00368(5) 0.70623(5) 0.04059(15) Uani 1 1 d . . . . .
Si4 Si 0.27357(6) 0.84727(5) 0.54893(5) 0.04327(16) Uani 1 1 d . . . . .
O1 O 0.16171(10) 0.68648(9) 0.70300(9) 0.0253(3) Uani 1 1 d . . . . .
O2 O 0.48196(12) 0.90780(12) 0.86560(12) 0.0436(4) Uani 1 1 d . . . . .
C1 C -0.00255(18) 0.78151(18) 0.7243(2) 0.0462(6) Uani 1 1 d . . . . .
H1A H -0.046715 0.819900 0.700916 0.069 Uiso 1 1 calc R U . . .
H1B H 0.033752 0.811209 0.785395 0.069 Uiso 1 1 calc R U . . .
H1C H -0.045584 0.726077 0.720560 0.069 Uiso 1 1 calc R U . . .
C2 C 0.0167(2) 0.6968(2) 0.54589(18) 0.0538(7) Uani 1 1 d . . . . .
H2A H -0.016478 0.738363 0.518232 0.081 Uiso 1 1 calc R U . . .
H2B H -0.036700 0.650856 0.548147 0.081 Uiso 1 1 calc R U . . .
H2C H 0.062271 0.669412 0.511941 0.081 Uiso 1 1 calc R U . . .
C3 C 0.1573(3) 1.0455(2) 0.8201(2) 0.0622(8) Uani 1 1 d . . . . .
H3A H 0.139692 1.104985 0.828930 0.093 Uiso 1 1 calc R U . . .
H3B H 0.223152 1.047624 0.861681 0.093 Uiso 1 1 calc R U . . .
H3C H 0.102352 1.005908 0.829287 0.093 Uiso 1 1 calc R U . . .
C4 C 0.0384(3) 0.9986(3) 0.6347(3) 0.0893(14) Uani 1 1 d . . . . .
H4A H 0.034213 0.964498 0.574978 0.134 Uiso 1 1 calc R U . . .
H4B H 0.026594 1.058673 0.635290 0.134 Uiso 1 1 calc R U . . .
H4C H -0.014444 0.970133 0.656425 0.134 Uiso 1 1 calc R U . . .
C5 C 0.2624(4) 1.0900(2) 0.6885(4) 0.125(2) Uani 1 1 d . . . . .
H5A H 0.277192 1.067732 0.631885 0.188 Uiso 1 1 calc R U . . .
H5B H 0.327090 1.104229 0.734911 0.188 Uiso 1 1 calc R U . . .
H5C H 0.231380 1.143373 0.689505 0.188 Uiso 1 1 calc R U . . .
C6 C 0.1798(3) 0.8828(2) 0.4654(2) 0.0672(9) Uani 1 1 d . . . . .
H6A H 0.205366 0.877294 0.413147 0.101 Uiso 1 1 calc R U . . .
H6B H 0.173483 0.944486 0.489608 0.101 Uiso 1 1 calc R U . . .
H6C H 0.111753 0.845226 0.450014 0.101 Uiso 1 1 calc R U . . .
C7 C 0.4051(3) 0.9115(3) 0.5629(3) 0.0773(11) Uani 1 1 d . . . . .
H7A H 0.418788 0.905379 0.505634 0.116 Uiso 1 1 calc R U . . .
H7B H 0.458138 0.888677 0.598967 0.116 Uiso 1 1 calc R U . . .
H7C H 0.407025 0.974026 0.591420 0.116 Uiso 1 1 calc R U . . .
C8 C 0.2793(3) 0.7281(2) 0.4964(2) 0.0624(9) Uani 1 1 d . . . . .
H8A H 0.208682 0.695129 0.469348 0.094 Uiso 1 1 calc R U . . .
H8B H 0.314602 0.702240 0.540808 0.094 Uiso 1 1 calc R U . . .
H8C H 0.317608 0.725272 0.451668 0.094 Uiso 1 1 calc R U . . .
C9 C 0.5058(2) 0.9553(2) 0.8068(2) 0.0622(9) Uani 1 1 d . . . . .
H9A H 0.540368 0.919862 0.767160 0.093 Uiso 1 1 calc R U . . .
H9B H 0.551915 1.011285 0.840058 0.093 Uiso 1 1 calc R U . . .
H9C H 0.441596 0.967195 0.772903 0.093 Uiso 1 1 calc R U . . .
C10 C 0.57557(18) 0.8970(2) 0.9218(2) 0.0602(9) Uani 1 1 d . . . . .
H10A H 0.623900 0.954114 0.946661 0.072 Uiso 1 1 calc R U . . .
H10B H 0.610196 0.853806 0.888402 0.072 Uiso 1 1 calc R U . . .
I1' I 0.48091(2) 0.69839(2) 0.70535(2) 0.05202(5) Uani 1 1 d . . . . .
Si1' Si 0.15002(4) 0.57598(4) 0.69354(4) 0.02659(11) Uani 1 1 d . . . . .
Si2' Si 0.26084(5) 0.58024(4) 0.82584(4) 0.03066(12) Uani 1 1 d . . . . .
Si3' Si 0.32912(8) 0.44946(6) 0.80112(7) 0.0641(2) Uani 1 1 d . . . . .
Si4' Si 0.15010(6) 0.56228(5) 0.91471(5) 0.04310(16) Uani 1 1 d . . . . .
O2' O 0.47743(14) 0.78299(13) 0.95443(13) 0.0515(5) Uani 1 1 d . . . . .
C1' C 0.1945(2) 0.52728(16) 0.59405(16) 0.0404(5) Uani 1 1 d . . . . .
H1'A H 0.184848 0.462858 0.582054 0.061 Uiso 1 1 calc R U . . .
H1'B H 0.268080 0.550740 0.604082 0.061 Uiso 1 1 calc R U . . .
H1'C H 0.153735 0.542809 0.544049 0.061 Uiso 1 1 calc R U . . .
C2' C 0.00827(18) 0.52980(18) 0.66845(18) 0.0435(6) Uani 1 1 d . . . . .
H2'A H -0.028537 0.539361 0.613622 0.065 Uiso 1 1 calc R U . . .
H2'B H -0.020263 0.559621 0.715761 0.065 Uiso 1 1 calc R U . . .
H2'C H -0.000314 0.466332 0.662895 0.065 Uiso 1 1 calc R U . . .
C3' C 0.4488(3) 0.4613(3) 0.7607(4) 0.1097(18) Uani 1 1 d . . . . .
H3'A H 0.463566 0.402659 0.735526 0.164 Uiso 1 1 calc R U . . .
H3'B H 0.507679 0.494610 0.809416 0.164 Uiso 1 1 calc R U . . .
H3'C H 0.437545 0.492972 0.716030 0.164 Uiso 1 1 calc R U . . .
C4' C 0.3631(6) 0.4132(4) 0.9031(4) 0.156(3) Uani 1 1 d . . . . .
H4'A H 0.299441 0.394735 0.918393 0.234 Uiso 1 1 calc R U . . .
H4'B H 0.406865 0.462494 0.950836 0.234 Uiso 1 1 calc R U . . .
H4'C H 0.400888 0.363608 0.893166 0.234 Uiso 1 1 calc R U . . .
C5' C 0.2367(4) 0.3519(2) 0.7185(3) 0.0950(14) Uani 1 1 d . . . . .
H5'A H 0.216415 0.365341 0.662494 0.143 Uiso 1 1 calc R U . . .
H5'B H 0.174899 0.339884 0.738915 0.143 Uiso 1 1 calc R U . . .
H5'C H 0.270965 0.299972 0.711202 0.143 Uiso 1 1 calc R U . . .
C6' C 0.2298(3) 0.5853(2) 1.0306(2) 0.0690(10) Uani 1 1 d . . . . .
H6'A H 0.288133 0.552900 1.031605 0.104 Uiso 1 1 calc R U . . .
H6'B H 0.186421 0.566182 1.065585 0.104 Uiso 1 1 calc R U . . .
H6'C H 0.256379 0.648787 1.054755 0.104 Uiso 1 1 calc R U . . .
C7' C 0.0716(3) 0.4481(2) 0.8842(2) 0.0752(11) Uani 1 1 d . . . . .
H7'A H 0.027580 0.446181 0.924280 0.113 Uiso 1 1 calc R U . . .
H7'B H 0.118447 0.405090 0.888191 0.113 Uiso 1 1 calc R U . . .
H7'C H 0.027894 0.433726 0.824436 0.113 Uiso 1 1 calc R U . . .
C8' C 0.0547(2) 0.6403(2) 0.9191(2) 0.0553(7) Uani 1 1 d . . . . .
H8'A H 0.013656 0.634374 0.859833 0.083 Uiso 1 1 calc R U . . .
H8'B H 0.092057 0.701008 0.945526 0.083 Uiso 1 1 calc R U . . .
H8'C H 0.008489 0.626179 0.954176 0.083 Uiso 1 1 calc R U . . .
C9' C 0.4610(3) 0.7421(3) 1.0204(3) 0.0957(16) Uani 1 1 d . . . . .
H9'A H 0.414467 0.685213 0.992830 0.143 Uiso 1 1 calc R U . . .
H9'B H 0.429626 0.780653 1.060512 0.143 Uiso 1 1 calc R U . . .
H9'C H 0.527592 0.732690 1.052874 0.143 Uiso 1 1 calc R U . . .
C10' C 0.5474(2) 0.8651(2) 0.9926(2) 0.0593(9) Uani 1 1 d . . . . .
H10C H 0.610443 0.856918 1.032566 0.071 Uiso 1 1 calc R U . . .
H10D H 0.513953 0.908950 1.026638 0.071 Uiso 1 1 calc R U . . .
O1E O -0.2444(5) 0.1996(6) 0.7566(8) 0.0928(18) Uani 0.721(11) 1 d D U P A 1
C1E C -0.0612(7) 0.2133(8) 0.8024(7) 0.096(3) Uani 0.721(11) 1 d D U P A 1
H1EA H -0.065364 0.156918 0.759269 0.145 Uiso 0.721(11) 1 calc R U P A 1
H1EB H -0.065712 0.202647 0.857911 0.145 Uiso 0.721(11) 1 calc R U P A 1
H1EC H 0.004847 0.251376 0.810817 0.145 Uiso 0.721(11) 1 calc R U P A 1
C2E C -0.1509(5) 0.2587(4) 0.7699(6) 0.0838(18) Uani 0.721(11) 1 d D U P A 1
H2EA H -0.148829 0.315054 0.813618 0.101 Uiso 0.721(11) 1 calc R U P A 1
H2EB H -0.146237 0.271417 0.714635 0.101 Uiso 0.721(11) 1 calc R U P A 1
C3E C -0.3354(6) 0.2386(5) 0.7333(5) 0.094(2) Uani 0.721(11) 1 d D U P A 1
H3EA H -0.334610 0.256713 0.679803 0.113 Uiso 0.721(11) 1 calc R U P A 1
H3EB H -0.331819 0.292589 0.780596 0.113 Uiso 0.721(11) 1 calc R U P A 1
C4E C -0.4327(8) 0.1801(9) 0.7182(10) 0.146(4) Uani 0.721(11) 1 d D U P A 1
H4EA H -0.490229 0.213078 0.710884 0.219 Uiso 0.721(11) 1 calc R U P A 1
H4EB H -0.431018 0.156458 0.768260 0.219 Uiso 0.721(11) 1 calc R U P A 1
H4EC H -0.442377 0.131242 0.665442 0.219 Uiso 0.721(11) 1 calc R U P A 1
O1EB O -0.2344(12) 0.1831(17) 0.7437(19) 0.081(3) Uani 0.279(11) 1 d D U P A 2
C1EB C -0.0526(18) 0.217(2) 0.7724(19) 0.091(6) Uani 0.279(11) 1 d D U P A 2
H1E1 H -0.061027 0.152712 0.746718 0.137 Uiso 0.279(11) 1 calc R U P A 2
H1E2 H 0.011255 0.236650 0.819810 0.137 Uiso 0.279(11) 1 calc R U P A 2
H1E3 H -0.048443 0.246854 0.727604 0.137 Uiso 0.279(11) 1 calc R U P A 2
C2EB C -0.1458(13) 0.2382(13) 0.8085(13) 0.087(3) Uani 0.279(11) 1 d D U P A 2
H2EC H -0.139548 0.224506 0.864999 0.104 Uiso 0.279(11) 1 calc R U P A 2
H2ED H -0.151180 0.301383 0.817051 0.104 Uiso 0.279(11) 1 calc R U P A 2
C3EB C -0.3262(13) 0.2069(14) 0.7666(14) 0.094(3) Uani 0.279(11) 1 d D U P A 2
H3EC H -0.329547 0.269045 0.766968 0.113 Uiso 0.279(11) 1 calc R U P A 2
H3ED H -0.324219 0.201984 0.825917 0.113 Uiso 0.279(11) 1 calc R U P A 2
C4EB C -0.4180(14) 0.1495(16) 0.7047(19) 0.087(5) Uani 0.279(11) 1 d D U P A 2
H4ED H -0.420480 0.155157 0.646091 0.131 Uiso 0.279(11) 1 calc R U P A 2
H4EE H -0.480264 0.166710 0.721338 0.131 Uiso 0.279(11) 1 calc R U P A 2
H4EF H -0.415063 0.088131 0.704874 0.131 Uiso 0.279(11) 1 calc R U P A 2
K1 K 0.74477(4) 0.74380(3) 0.72603(3) 0.03394(10) Uani 1 1 d . . . . .
O1K O 0.71101(14) 0.56682(12) 0.71895(14) 0.0499(5) Uani 1 1 d . . . . .
O2K O 0.80972(14) 0.68988(12) 0.87520(12) 0.0454(4) Uani 1 1 d . . . . .
O3K O 0.82814(13) 0.86975(11) 0.88760(12) 0.0408(4) Uani 1 1 d . . . . .
O4K O 0.80086(14) 0.92127(13) 0.73301(14) 0.0484(5) Uani 1 1 d . . . . .
O5K O 0.68985(17) 0.79786(17) 0.57693(14) 0.0618(6) Uani 1 1 d . . . . .
O6K O 0.68905(15) 0.61512(15) 0.56443(13) 0.0582(6) Uani 1 1 d . . . . .
C1K C 0.7553(3) 0.5397(2) 0.7927(2) 0.0594(8) Uani 1 1 d . . . . .
H1KA H 0.828084 0.532550 0.794196 0.071 Uiso 1 1 calc R U . . .
H1KB H 0.715993 0.482261 0.790189 0.071 Uiso 1 1 calc R U . . .
C2K C 0.7516(3) 0.6089(2) 0.8723(2) 0.0618(8) Uani 1 1 d . . . . .
H2KA H 0.678783 0.615867 0.870567 0.074 Uiso 1 1 calc R U . . .
H2KB H 0.780907 0.591103 0.925209 0.074 Uiso 1 1 calc R U . . .
C3K C 0.8257(3) 0.7552(2) 0.95552(19) 0.0556(7) Uani 1 1 d . . . . .
H3KA H 0.862982 0.734010 1.003812 0.067 Uiso 1 1 calc R U . . .
H3KB H 0.758097 0.767294 0.965925 0.067 Uiso 1 1 calc R U . . .
C4K C 0.8872(2) 0.8364(2) 0.95264(18) 0.0525(7) Uani 1 1 d . . . . .
H4KA H 0.904303 0.881062 1.010202 0.063 Uiso 1 1 calc R U . . .
H4KB H 0.952969 0.823532 0.938494 0.063 Uiso 1 1 calc R U . . .
C5K C 0.8814(2) 0.95036(17) 0.8838(2) 0.0504(7) Uani 1 1 d . . . . .
H5KA H 0.947740 0.940983 0.869090 0.061 Uiso 1 1 calc R U . . .
H5KB H 0.897069 0.994963 0.941292 0.061 Uiso 1 1 calc R U . . .
C6K C 0.8156(2) 0.98219(18) 0.8168(2) 0.0542(8) Uani 1 1 d . . . . .
H6KA H 0.747563 0.987976 0.829596 0.065 Uiso 1 1 calc R U . . .
H6KB H 0.849156 1.041053 0.817325 0.065 Uiso 1 1 calc R U . . .
C7K C 0.7381(3) 0.9474(2) 0.6647(3) 0.0674(10) Uani 1 1 d . . . . .
H7KA H 0.767295 1.007907 0.666123 0.081 Uiso 1 1 calc R U . . .
H7KB H 0.667015 0.947643 0.672409 0.081 Uiso 1 1 calc R U . . .
C8K C 0.7346(3) 0.8842(3) 0.5792(2) 0.0745(11) Uani 1 1 d . . . . .
H8KA H 0.692792 0.902746 0.530969 0.089 Uiso 1 1 calc R U . . .
H8KB H 0.805746 0.883924 0.571598 0.089 Uiso 1 1 calc R U . . .
C9K C 0.6837(3) 0.7313(3) 0.4973(2) 0.0866(13) Uani 1 1 d . . . . .
H9KA H 0.754397 0.725025 0.490921 0.104 Uiso 1 1 calc R U . . .
H9KB H 0.645690 0.748824 0.446756 0.104 Uiso 1 1 calc R U . . .
C10K C 0.6289(3) 0.6461(3) 0.4998(2) 0.0783(11) Uani 1 1 d . . . . .
H10E H 0.561192 0.654186 0.512371 0.094 Uiso 1 1 calc R U . . .
H10F H 0.615665 0.601987 0.442277 0.094 Uiso 1 1 calc R U . . .
C11K C 0.6401(2) 0.5321(2) 0.5676(2) 0.0625(9) Uani 1 1 d . . . . .
H11A H 0.631015 0.487120 0.511213 0.075 Uiso 1 1 calc R U . . .
H11B H 0.570644 0.537250 0.577570 0.075 Uiso 1 1 calc R U . . .
C12K C 0.7045(2) 0.50412(19) 0.6390(2) 0.0613(9) Uani 1 1 d . . . . .
H12A H 0.672663 0.445032 0.639304 0.074 Uiso 1 1 calc R U . . .
H12B H 0.774777 0.500634 0.630292 0.074 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.5613(13) . ?
U1 O2' 2.6149(17) . ?
U1 O2 2.6384(16) . ?
U1 I1' 3.11253(19) . ?
U1 Si2 3.1149(6) . ?
U1 I1 3.12556(19) . ?
U1 Si2' 3.1276(6) . ?
Si1 O1 1.7041(15) . ?
Si1 C2 1.871(3) . ?
Si1 C1 1.878(2) . ?
Si1 Si2 2.3166(9) . ?
Si2 Si3 2.3358(9) . ?
Si2 Si4 2.3497(9) . ?
Si3 C4 1.869(4) . ?
Si3 C5 1.871(4) . ?
Si3 C3 1.872(3) . ?
Si4 C7 1.879(3) . ?
Si4 C6 1.882(3) . ?
Si4 C8 1.889(3) . ?
O1 Si1' 1.7078(15) . ?
O2 C9 1.432(4) . ?
O2 C10 1.436(3) . ?
C1 K1 3.388(2) 1_455 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C10' 1.483(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
I1' K1 3.4608(5) . ?
Si1' C1' 1.876(2) . ?
Si1' C2' 1.879(2) . ?
Si1' Si2' 2.3203(9) . ?
Si2' Si3' 2.3361(10) . ?
Si2' Si4' 2.3452(10) . ?
Si3' C4' 1.878(5) . ?
Si3' C3' 1.879(5) . ?
Si3' C5' 1.888(4) . ?
Si4' C8' 1.872(3) . ?
Si4' C6' 1.884(3) . ?
Si4' C7' 1.884(3) . ?
O2' C10' 1.429(3) . ?
O2' C9' 1.437(4) . ?
C1' H1'A 0.9800 . ?
C1' H1'B 0.9800 . ?
C1' H1'C 0.9800 . ?
C2' H2'A 0.9800 . ?
C2' H2'B 0.9800 . ?
C2' H2'C 0.9800 . ?
C3' H3'A 0.9800 . ?
C3' H3'B 0.9800 . ?
C3' H3'C 0.9800 . ?
C4' H4'A 0.9800 . ?
C4' H4'B 0.9800 . ?
C4' H4'C 0.9800 . ?
C5' H5'A 0.9800 . ?
C5' H5'B 0.9800 . ?
C5' H5'C 0.9800 . ?
C6' H6'A 0.9800 . ?
C6' H6'B 0.9800 . ?
C6' H6'C 0.9800 . ?
C7' H7'A 0.9800 . ?
C7' H7'B 0.9800 . ?
C7' H7'C 0.9800 . ?
C8' H8'A 0.9800 . ?
C8' H8'B 0.9800 . ?
C8' H8'C 0.9800 . ?
C9' H9'A 0.9800 . ?
C9' H9'B 0.9800 . ?
C9' H9'C 0.9800 . ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?
O1E C2E 1.424(9) . ?
O1E C3E 1.445(10) . ?
C1E C2E 1.529(10) . ?
C1E H1EA 0.9800 . ?
C1E H1EB 0.9800 . ?
C1E H1EC 0.9800 . ?
C2E H2EA 0.9900 . ?
C2E H2EB 0.9900 . ?
C3E C4E 1.454(10) . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
C4E H4EA 0.9800 . ?
C4E H4EB 0.9800 . ?
C4E H4EC 0.9800 . ?
O1EB C3EB 1.427(16) . ?
O1EB C2EB 1.435(16) . ?
C1EB C2EB 1.535(16) . ?
C1EB H1E1 0.9800 . ?
C1EB H1E2 0.9800 . ?
C1EB H1E3 0.9800 . ?
C2EB H2EC 0.9900 . ?
C2EB H2ED 0.9900 . ?
C3EB C4EB 1.455(16) . ?
C3EB H3EC 0.9900 . ?
C3EB H3ED 0.9900 . ?
C4EB H4ED 0.9800 . ?
C4EB H4EE 0.9800 . ?
C4EB H4EF 0.9800 . ?
K1 O5K 2.762(2) . ?
K1 O1K 2.765(2) . ?
K1 O2K 2.7785(19) . ?
K1 O3K 2.7969(18) . ?
K1 O6K 2.800(2) . ?
K1 O4K 2.803(2) . ?
O1K C1K 1.412(4) . ?
O1K C12K 1.413(3) . ?
O2K C3K 1.414(3) . ?
O2K C2K 1.414(4) . ?
O3K C5K 1.420(3) . ?
O3K C4K 1.427(3) . ?
O4K C7K 1.421(4) . ?
O4K C6K 1.427(4) . ?
O5K C8K 1.424(4) . ?
O5K C9K 1.439(4) . ?
O6K C10K 1.406(4) . ?
O6K C11K 1.427(4) . ?
C1K C2K 1.497(5) . ?
C1K H1KA 0.9900 . ?
C1K H1KB 0.9900 . ?
C2K H2KA 0.9900 . ?
C2K H2KB 0.9900 . ?
C3K C4K 1.473(4) . ?
C3K H3KA 0.9900 . ?
C3K H3KB 0.9900 . ?
C4K H4KA 0.9900 . ?
C4K H4KB 0.9900 . ?
C5K C6K 1.476(4) . ?
C5K H5KA 0.9900 . ?
C5K H5KB 0.9900 . ?
C6K H6KA 0.9900 . ?
C6K H6KB 0.9900 . ?
C7K C8K 1.495(5) . ?
C7K H7KA 0.9900 . ?
C7K H7KB 0.9900 . ?
C8K H8KA 0.9900 . ?
C8K H8KB 0.9900 . ?
C9K C10K 1.484(6) . ?
C9K H9KA 0.9900 . ?
C9K H9KB 0.9900 . ?
C10K H10E 0.9900 . ?
C10K H10F 0.9900 . ?
C11K C12K 1.484(5) . ?
C11K H11A 0.9900 . ?
C11K H11B 0.9900 . ?
C12K H12A 0.9900 . ?
C12K H12B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O2' 149.64(6) . . ?
O1 U1 O2 147.51(6) . . ?
O2' U1 O2 62.83(6) . . ?
O1 U1 I1' 96.82(3) . . ?
O2' U1 I1' 87.61(5) . . ?
O2 U1 I1' 79.16(4) . . ?
O1 U1 Si2 64.83(3) . . ?
O2' U1 Si2 145.13(5) . . ?
O2 U1 Si2 83.11(4) . . ?
I1' U1 Si2 93.423(12) . . ?
O1 U1 I1 98.86(3) . . ?
O2' U1 I1 78.78(5) . . ?
O2 U1 I1 87.63(4) . . ?
I1' U1 I1 164.321(6) . . ?
Si2 U1 I1 93.344(12) . . ?
O1 U1 Si2' 65.25(3) . . ?
O2' U1 Si2' 84.81(5) . . ?
O2 U1 Si2' 145.98(4) . . ?
I1' U1 Si2' 89.880(13) . . ?
Si2 U1 Si2' 130.014(16) . . ?
I1 U1 Si2' 96.548(13) . . ?
O1 Si1 C2 109.02(11) . . ?
O1 Si1 C1 104.56(10) . . ?
C2 Si1 C1 105.30(14) . . ?
O1 Si1 Si2 98.79(5) . . ?
C2 Si1 Si2 120.92(11) . . ?
C1 Si1 Si2 116.73(9) . . ?
Si1 Si2 Si3 108.25(3) . . ?
Si1 Si2 Si4 104.22(4) . . ?
Si3 Si2 Si4 105.37(3) . . ?
Si1 Si2 U1 79.87(2) . . ?
Si3 Si2 U1 131.17(3) . . ?
Si4 Si2 U1 119.43(3) . . ?
C4 Si3 C5 108.1(2) . . ?
C4 Si3 C3 104.82(17) . . ?
C5 Si3 C3 107.0(2) . . ?
C4 Si3 Si2 114.58(13) . . ?
C5 Si3 Si2 109.74(13) . . ?
C3 Si3 Si2 112.16(11) . . ?
C7 Si4 C6 106.58(18) . . ?
C7 Si4 C8 106.02(17) . . ?
C6 Si4 C8 106.04(16) . . ?
C7 Si4 Si2 110.43(12) . . ?
C6 Si4 Si2 113.75(11) . . ?
C8 Si4 Si2 113.48(10) . . ?
Si1 O1 Si1' 138.79(9) . . ?
Si1 O1 U1 110.56(7) . . ?
Si1' O1 U1 110.64(7) . . ?
C9 O2 C10 110.4(2) . . ?
C9 O2 U1 121.93(16) . . ?
C10 O2 U1 114.62(17) . . ?
Si1 C1 K1 145.89(14) . 1_455 ?
Si1 C1 H1A 109.5 . . ?
K1 C1 H1A 63.8 1_455 . ?
Si1 C1 H1B 109.5 . . ?
K1 C1 H1B 104.0 1_455 . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
K1 C1 H1C 51.1 1_455 . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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 . . ?
Si3 C3 H3A 109.5 . . ?
Si3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si4 C6 H6A 109.5 . . ?
Si4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C9 H9A 109.5 . . ?
O2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 C10' 108.0(2) . . ?
O2 C10 H10A 110.1 . . ?
C10' C10 H10A 110.1 . . ?
O2 C10 H10B 110.1 . . ?
C10' C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
U1 I1' K1 135.435(11) . . ?
O1 Si1' C1' 105.05(10) . . ?
O1 Si1' C2' 108.04(10) . . ?
C1' Si1' C2' 106.90(12) . . ?
O1 Si1' Si2' 99.69(5) . . ?
C1' Si1' Si2' 115.70(9) . . ?
C2' Si1' Si2' 119.98(9) . . ?
Si1' Si2' Si3' 105.87(4) . . ?
Si1' Si2' Si4' 104.39(3) . . ?
Si3' Si2' Si4' 104.46(4) . . ?
Si1' Si2' U1 79.66(2) . . ?
Si3' Si2' U1 134.14(4) . . ?
Si4' Si2' U1 118.40(3) . . ?
C4' Si3' C3' 108.2(3) . . ?
C4' Si3' C5' 104.5(3) . . ?
C3' Si3' C5' 106.2(2) . . ?
C4' Si3' Si2' 111.31(17) . . ?
C3' Si3' Si2' 111.96(14) . . ?
C5' Si3' Si2' 114.22(14) . . ?
C8' Si4' C6' 105.42(16) . . ?
C8' Si4' C7' 106.02(17) . . ?
C6' Si4' C7' 106.72(17) . . ?
C8' Si4' Si2' 114.31(10) . . ?
C6' Si4' Si2' 109.14(13) . . ?
C7' Si4' Si2' 114.59(12) . . ?
C10' O2' C9' 110.7(2) . . ?
C10' O2' U1 117.35(17) . . ?
C9' O2' U1 122.27(18) . . ?
Si1' C1' H1'A 109.5 . . ?
Si1' C1' H1'B 109.5 . . ?
H1'A C1' H1'B 109.5 . . ?
Si1' C1' H1'C 109.5 . . ?
H1'A C1' H1'C 109.5 . . ?
H1'B C1' H1'C 109.5 . . ?
Si1' C2' H2'A 109.5 . . ?
Si1' C2' H2'B 109.5 . . ?
H2'A C2' H2'B 109.5 . . ?
Si1' C2' H2'C 109.5 . . ?
H2'A C2' H2'C 109.5 . . ?
H2'B C2' H2'C 109.5 . . ?
Si3' C3' H3'A 109.5 . . ?
Si3' C3' H3'B 109.5 . . ?
H3'A C3' H3'B 109.5 . . ?
Si3' C3' H3'C 109.5 . . ?
H3'A C3' H3'C 109.5 . . ?
H3'B C3' H3'C 109.5 . . ?
Si3' C4' H4'A 109.5 . . ?
Si3' C4' H4'B 109.5 . . ?
H4'A C4' H4'B 109.5 . . ?
Si3' C4' H4'C 109.5 . . ?
H4'A C4' H4'C 109.5 . . ?
H4'B C4' H4'C 109.5 . . ?
Si3' C5' H5'A 109.5 . . ?
Si3' C5' H5'B 109.5 . . ?
H5'A C5' H5'B 109.5 . . ?
Si3' C5' H5'C 109.5 . . ?
H5'A C5' H5'C 109.5 . . ?
H5'B C5' H5'C 109.5 . . ?
Si4' C6' H6'A 109.5 . . ?
Si4' C6' H6'B 109.5 . . ?
H6'A C6' H6'B 109.5 . . ?
Si4' C6' H6'C 109.5 . . ?
H6'A C6' H6'C 109.5 . . ?
H6'B C6' H6'C 109.5 . . ?
Si4' C7' H7'A 109.5 . . ?
Si4' C7' H7'B 109.5 . . ?
H7'A C7' H7'B 109.5 . . ?
Si4' C7' H7'C 109.5 . . ?
H7'A C7' H7'C 109.5 . . ?
H7'B C7' H7'C 109.5 . . ?
Si4' C8' H8'A 109.5 . . ?
Si4' C8' H8'B 109.5 . . ?
H8'A C8' H8'B 109.5 . . ?
Si4' C8' H8'C 109.5 . . ?
H8'A C8' H8'C 109.5 . . ?
H8'B C8' H8'C 109.5 . . ?
O2' C9' H9'A 109.5 . . ?
O2' C9' H9'B 109.5 . . ?
H9'A C9' H9'B 109.5 . . ?
O2' C9' H9'C 109.5 . . ?
H9'A C9' H9'C 109.5 . . ?
H9'B C9' H9'C 109.5 . . ?
O2' C10' C10 108.6(2) . . ?
O2' C10' H10C 110.0 . . ?
C10 C10' H10C 110.0 . . ?
O2' C10' H10D 110.0 . . ?
C10 C10' H10D 110.0 . . ?
H10C C10' H10D 108.4 . . ?
C2E O1E C3E 112.1(9) . . ?
C2E C1E H1EA 109.5 . . ?
C2E C1E H1EB 109.5 . . ?
H1EA C1E H1EB 109.5 . . ?
C2E C1E H1EC 109.5 . . ?
H1EA C1E H1EC 109.5 . . ?
H1EB C1E H1EC 109.5 . . ?
O1E C2E C1E 106.9(7) . . ?
O1E C2E H2EA 110.3 . . ?
C1E C2E H2EA 110.3 . . ?
O1E C2E H2EB 110.3 . . ?
C1E C2E H2EB 110.3 . . ?
H2EA C2E H2EB 108.6 . . ?
O1E C3E C4E 113.8(9) . . ?
O1E C3E H3EA 108.8 . . ?
C4E C3E H3EA 108.8 . . ?
O1E C3E H3EB 108.8 . . ?
C4E C3E H3EB 108.8 . . ?
H3EA C3E H3EB 107.7 . . ?
C3E C4E H4EA 109.5 . . ?
C3E C4E H4EB 109.5 . . ?
H4EA C4E H4EB 109.5 . . ?
C3E C4E H4EC 109.5 . . ?
H4EA C4E H4EC 109.5 . . ?
H4EB C4E H4EC 109.5 . . ?
C3EB O1EB C2EB 108.7(16) . . ?
C2EB C1EB H1E1 109.5 . . ?
C2EB C1EB H1E2 109.5 . . ?
H1E1 C1EB H1E2 109.5 . . ?
C2EB C1EB H1E3 109.5 . . ?
H1E1 C1EB H1E3 109.5 . . ?
H1E2 C1EB H1E3 109.5 . . ?
O1EB C2EB C1EB 104.9(17) . . ?
O1EB C2EB H2EC 110.8 . . ?
C1EB C2EB H2EC 110.8 . . ?
O1EB C2EB H2ED 110.8 . . ?
C1EB C2EB H2ED 110.8 . . ?
H2EC C2EB H2ED 108.8 . . ?
O1EB C3EB C4EB 110.5(15) . . ?
O1EB C3EB H3EC 109.5 . . ?
C4EB C3EB H3EC 109.5 . . ?
O1EB C3EB H3ED 109.5 . . ?
C4EB C3EB H3ED 109.5 . . ?
H3EC C3EB H3ED 108.1 . . ?
C3EB C4EB H4ED 109.5 . . ?
C3EB C4EB H4EE 109.5 . . ?
H4ED C4EB H4EE 109.5 . . ?
C3EB C4EB H4EF 109.5 . . ?
H4ED C4EB H4EF 109.5 . . ?
H4EE C4EB H4EF 109.5 . . ?
O5K K1 O1K 120.90(7) . . ?
O5K K1 O2K 177.25(6) . . ?
O1K K1 O2K 59.51(6) . . ?
O5K K1 O3K 119.74(7) . . ?
O1K K1 O3K 119.31(6) . . ?
O2K K1 O3K 60.05(6) . . ?
O5K K1 O6K 61.73(8) . . ?
O1K K1 O6K 60.13(7) . . ?
O2K K1 O6K 118.06(7) . . ?
O3K K1 O6K 172.25(6) . . ?
O5K K1 O4K 60.15(7) . . ?
O1K K1 O4K 173.89(6) . . ?
O2K K1 O4K 119.12(6) . . ?
O3K K1 O4K 60.28(6) . . ?
O6K K1 O4K 119.33(7) . . ?
O5K K1 C1 89.73(7) . 1_655 ?
O1K K1 C1 102.92(6) . 1_655 ?
O2K K1 C1 87.54(6) . 1_655 ?
O3K K1 C1 79.40(6) . 1_655 ?
O6K K1 C1 93.12(7) . 1_655 ?
O4K K1 C1 70.97(6) . 1_655 ?
O5K K1 I1' 85.64(5) . . ?
O1K K1 I1' 76.73(4) . . ?
O2K K1 I1' 97.06(4) . . ?
O3K K1 I1' 105.81(4) . . ?
O6K K1 I1' 81.75(4) . . ?
O4K K1 I1' 109.35(4) . . ?
C1 K1 I1' 174.29(6) 1_655 . ?
C1K O1K C12K 113.4(2) . . ?
C1K O1K K1 119.59(16) . . ?
C12K O1K K1 117.92(19) . . ?
C3K O2K C2K 112.9(2) . . ?
C3K O2K K1 115.99(16) . . ?
C2K O2K K1 113.39(17) . . ?
C5K O3K C4K 111.7(2) . . ?
C5K O3K K1 114.81(15) . . ?
C4K O3K K1 114.14(15) . . ?
C7K O4K C6K 112.9(2) . . ?
C7K O4K K1 113.81(19) . . ?
C6K O4K K1 114.57(15) . . ?
C8K O5K C9K 114.0(3) . . ?
C8K O5K K1 118.13(19) . . ?
C9K O5K K1 114.5(2) . . ?
C10K O6K C11K 112.0(3) . . ?
C10K O6K K1 110.9(2) . . ?
C11K O6K K1 113.18(17) . . ?
O1K C1K C2K 108.0(2) . . ?
O1K C1K H1KA 110.1 . . ?
C2K C1K H1KA 110.1 . . ?
O1K C1K H1KB 110.1 . . ?
C2K C1K H1KB 110.1 . . ?
H1KA C1K H1KB 108.4 . . ?
O2K C2K C1K 109.1(3) . . ?
O2K C2K H2KA 109.9 . . ?
C1K C2K H2KA 109.9 . . ?
O2K C2K H2KB 109.9 . . ?
C1K C2K H2KB 109.9 . . ?
H2KA C2K H2KB 108.3 . . ?
O2K C3K C4K 109.0(2) . . ?
O2K C3K H3KA 109.9 . . ?
C4K C3K H3KA 109.9 . . ?
O2K C3K H3KB 109.9 . . ?
C4K C3K H3KB 109.9 . . ?
H3KA C3K H3KB 108.3 . . ?
O3K C4K C3K 108.8(2) . . ?
O3K C4K H4KA 109.9 . . ?
C3K C4K H4KA 109.9 . . ?
O3K C4K H4KB 109.9 . . ?
C3K C4K H4KB 109.9 . . ?
H4KA C4K H4KB 108.3 . . ?
O3K C5K C6K 109.1(2) . . ?
O3K C5K H5KA 109.9 . . ?
C6K C5K H5KA 109.9 . . ?
O3K C5K H5KB 109.9 . . ?
C6K C5K H5KB 109.9 . . ?
H5KA C5K H5KB 108.3 . . ?
O4K C6K C5K 109.5(2) . . ?
O4K C6K H6KA 109.8 . . ?
C5K C6K H6KA 109.8 . . ?
O4K C6K H6KB 109.8 . . ?
C5K C6K H6KB 109.8 . . ?
H6KA C6K H6KB 108.2 . . ?
O4K C7K C8K 109.1(3) . . ?
O4K C7K H7KA 109.9 . . ?
C8K C7K H7KA 109.9 . . ?
O4K C7K H7KB 109.9 . . ?
C8K C7K H7KB 109.9 . . ?
H7KA C7K H7KB 108.3 . . ?
O5K C8K C7K 109.4(3) . . ?
O5K C8K H8KA 109.8 . . ?
C7K C8K H8KA 109.8 . . ?
O5K C8K H8KB 109.8 . . ?
C7K C8K H8KB 109.8 . . ?
H8KA C8K H8KB 108.2 . . ?
O5K C9K C10K 109.0(3) . . ?
O5K C9K H9KA 109.9 . . ?
C10K C9K H9KA 109.9 . . ?
O5K C9K H9KB 109.9 . . ?
C10K C9K H9KB 109.9 . . ?
H9KA C9K H9KB 108.3 . . ?
O6K C10K C9K 110.2(3) . . ?
O6K C10K H10E 109.6 . . ?
C9K C10K H10E 109.6 . . ?
O6K C10K H10F 109.6 . . ?
C9K C10K H10F 109.6 . . ?
H10E C10K H10F 108.1 . . ?
O6K C11K C12K 109.8(2) . . ?
O6K C11K H11A 109.7 . . ?
C12K C11K H11A 109.7 . . ?
O6K C11K H11B 109.7 . . ?
C12K C11K H11B 109.7 . . ?
H11A C11K H11B 108.2 . . ?
O1K C12K C11K 108.4(2) . . ?
O1K C12K H12A 110.0 . . ?
C11K C12K H12A 110.0 . . ?
O1K C12K H12B 110.0 . . ?
C11K C12K H12B 110.0 . . ?
H12A C12K H12B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Si1 O1 Si1' -28.06(19) . . . . ?
C1 Si1 O1 Si1' 84.14(17) . . . . ?
Si2 Si1 O1 Si1' -155.18(12) . . . . ?
C2 Si1 O1 U1 151.02(12) . . . . ?
C1 Si1 O1 U1 -96.78(11) . . . . ?
Si2 Si1 O1 U1 23.91(7) . . . . ?
O1 Si1 C1 K1 -105.5(2) . . . 1_455 ?
C2 Si1 C1 K1 9.4(3) . . . 1_455 ?
Si2 Si1 C1 K1 146.62(17) . . . 1_455 ?
C9 O2 C10 C10' 168.2(2) . . . . ?
U1 O2 C10 C10' -49.5(3) . . . . ?
Si1 O1 Si1' C1' 80.47(16) . . . . ?
U1 O1 Si1' C1' -98.61(10) . . . . ?
Si1 O1 Si1' C2' -33.36(18) . . . . ?
U1 O1 Si1' C2' 147.56(10) . . . . ?
Si1 O1 Si1' Si2' -159.43(12) . . . . ?
U1 O1 Si1' Si2' 21.49(7) . . . . ?
C9' O2' C10' C10 170.6(3) . . . . ?
U1 O2' C10' C10 -42.5(3) . . . . ?
O2 C10 C10' O2' 59.5(3) . . . . ?
C3E O1E C2E C1E 174.7(7) . . . . ?
C2E O1E C3E C4E 179.4(9) . . . . ?
C3EB O1EB C2EB C1EB -173(3) . . . . ?
C2EB O1EB C3EB C4EB -177(2) . . . . ?
C12K O1K C1K C2K -176.5(2) . . . . ?
K1 O1K C1K C2K 37.1(3) . . . . ?
C3K O2K C2K C1K -169.6(2) . . . . ?
K1 O2K C2K C1K 55.9(3) . . . . ?
O1K C1K C2K O2K -60.7(3) . . . . ?
C2K O2K C3K C4K 179.6(2) . . . . ?
K1 O2K C3K C4K -47.1(3) . . . . ?
C5K O3K C4K C3K 177.6(2) . . . . ?
K1 O3K C4K C3K -50.1(3) . . . . ?
O2K C3K C4K O3K 64.5(3) . . . . ?
C4K O3K C5K C6K -178.9(2) . . . . ?
K1 O3K C5K C6K 49.1(2) . . . . ?
C7K O4K C6K C5K -180.0(2) . . . . ?
K1 O4K C6K C5K 47.5(2) . . . . ?
O3K C5K C6K O4K -64.6(3) . . . . ?
C6K O4K C7K C8K 175.1(2) . . . . ?
K1 O4K C7K C8K -52.0(3) . . . . ?
C9K O5K C8K C7K -179.4(3) . . . . ?
K1 O5K C8K C7K -40.7(3) . . . . ?
O4K C7K C8K O5K 61.1(3) . . . . ?
C8K O5K C9K C10K -175.8(3) . . . . ?
K1 O5K C9K C10K 43.9(4) . . . . ?
C11K O6K C10K C9K -178.6(3) . . . . ?
K1 O6K C10K C9K 53.9(3) . . . . ?
O5K C9K C10K O6K -67.1(4) . . . . ?
C10K O6K C11K C12K -177.7(3) . . . . ?
K1 O6K C11K C12K -51.5(3) . . . . ?
C1K O1K C12K C11K 169.8(2) . . . . ?
K1 O1K C12K C11K -43.3(3) . . . . ?
O6K C11K C12K O1K 62.7(3) . . . . ?

_refine_diff_density_max         1.978
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.091




####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NL_3_99_UI3_t2_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2325809'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2024-01-15 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H58 I2 O3 Si8 U, C16 H40 K O8'
_chemical_formula_sum            'C36 H98 I2 K O11 Si8 U'
_chemical_formula_weight         1462.79

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'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   14.8717(5)
_cell_length_b                   15.8095(5)
_cell_length_c                   28.9025(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.785(2)
_cell_angle_gamma                90
_cell_volume                     6599.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9865
_cell_measurement_theta_min      2.6315
_cell_measurement_theta_max      27.4090

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             2924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.644
_shelx_estimated_absorpt_T_min   0.839
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5953
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.
(2015). J. Appl. Cryst. 48, 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_measurement_device_type  
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_reflns_number            127091
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.766
_diffrn_reflns_theta_max         33.247
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             25260
_reflns_number_gt                12924
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex4 v2021.4-0 (Bruker, 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1275(Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
There is one coordinating 1,2-dimethoxyethane (DME) molecule per
uranium center, each with the central C-C bond on a 2-fold axis
coincident with the uranium and silyl-ether oxygen atom 
(EQIV $1 2-x, +y, 3/2-z). 

The DME molecule with C9, C10, and O2 is disordered about the 2-fold axis
and their 1,2 and 1,3 bond distances were restrained to be similar to the 
well-resolved DME molecule of the potassium countercation C29, O11, C30, 
C31, O12, and C32. 

The DME molecule with C19, C20, and O4 is positionally disordered over 
two positions and the 1,2 and 1,3 bond distances of the disordered 
DME were restrained to be similar to half of another well-resolved 
DME molecule, O5 C22 C21.

In addition, the central C-C bond of each DME molecule (C10A-C10B,
C19-C19_$1, and C19b-C19b_$1) was restrained to 1.49 Angstrom (of a 
typical central C-C bond of a DME molecule) with an esd of 0.01 Angstrom, 
resulting in bond lengths of 1.481(8), 1.489(9), and 1.485(10) Angstrom, 
respectively.
 
The Uij components of the anisotropic displacement parameters for
disordered atoms closer to each other than 2.0 Angstrom were
restrained to be similar within a standard deviation of 0.01 Angstrom
squared.

Subject to these conditions, the occupancy ratio of the positionally
disordered moiety refined to 0.743(13) : 0.257(13).

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0445P)²+5.5493P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         25260
_refine_ls_number_parameters     611
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1275
_refine_ls_wR_factor_gt          0.1003
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.500000 0.79035(2) 0.250000 0.03246(6) Uani 1 2 d S T P . .
U2 U 1.000000 0.84928(2) 0.750000 0.03107(6) Uani 1 2 d S T P . .
I1 I 0.40327(3) 0.82589(3) 0.33215(2) 0.05697(11) Uani 1 1 d . . . . .
I2 I 0.91676(2) 0.87997(2) 0.83844(2) 0.04590(9) Uani 1 1 d . . . . .
K1 K 0.23843(7) 0.78379(7) 0.49260(4) 0.0415(2) Uani 1 1 d . . . . .
Si1 Si 0.60872(8) 0.58935(8) 0.27218(5) 0.0308(3) Uani 1 1 d . . . . .
Si2 Si 0.67295(8) 0.70508(8) 0.31668(5) 0.0329(3) Uani 1 1 d . . . . .
Si3 Si 0.66587(10) 0.67833(10) 0.39552(5) 0.0448(3) Uani 1 1 d . . . . .
Si4 Si 0.82949(9) 0.70350(9) 0.31642(5) 0.0422(3) Uani 1 1 d . . . . .
Si5 Si 0.89048(8) 0.64981(8) 0.72868(4) 0.0302(3) Uani 1 1 d . . . . .
Si6 Si 0.82423(8) 0.76514(9) 0.68359(4) 0.0331(3) Uani 1 1 d . . . . .
Si7 Si 0.66973(9) 0.76622(10) 0.68845(5) 0.0439(3) Uani 1 1 d . . . . .
Si8 Si 0.82032(10) 0.73057(10) 0.60419(5) 0.0418(3) Uani 1 1 d . . . . .
O1 O 0.500000 0.6267(3) 0.250000 0.0332(10) Uani 1 2 d S T P . .
O3 O 1.000000 0.6894(3) 0.750000 0.0281(9) Uani 1 2 d S T P B .
O5 O 0.4120(3) 0.8679(3) 0.50088(16) 0.0666(12) Uani 1 1 d D . . . .
O6 O 0.2878(3) 0.9264(3) 0.55436(15) 0.0613(11) Uani 1 1 d . . . . .
O7 O 0.2197(3) 0.6681(3) 0.41781(14) 0.0558(10) Uani 1 1 d . . . . .
O8 O 0.3738(3) 0.6497(3) 0.49407(16) 0.0613(11) Uani 1 1 d . . . . .
O9 O 0.1055(3) 0.6659(3) 0.51008(15) 0.0587(10) Uani 1 1 d . . . . .
O10 O 0.2644(3) 0.7068(3) 0.58018(13) 0.0623(11) Uani 1 1 d . . . . .
O11 O 0.1946(2) 0.9289(3) 0.43234(13) 0.0547(10) Uani 1 1 d D . . . .
O12 O 0.0538(3) 0.8520(2) 0.46477(15) 0.0578(10) Uani 1 1 d D . . . .
C1 C 0.6564(3) 0.5693(3) 0.21923(18) 0.0415(11) Uani 1 1 d . . . . .
H1A H 0.615878 0.529918 0.197672 0.062 Uiso 1 1 calc R U . . .
H1B H 0.718476 0.544669 0.229539 0.062 Uiso 1 1 calc R U . . .
H1C H 0.660105 0.622726 0.202584 0.062 Uiso 1 1 calc R U . . .
C2 C 0.6005(3) 0.4840(3) 0.30088(19) 0.0415(11) Uani 1 1 d . . . . .
H2A H 0.570283 0.443212 0.276553 0.062 Uiso 1 1 calc R U . . .
H2B H 0.564072 0.489829 0.324843 0.062 Uiso 1 1 calc R U . . .
H2C H 0.662790 0.463845 0.316205 0.062 Uiso 1 1 calc R U . . .
C3 C 0.5539(4) 0.6272(4) 0.4011(2) 0.0620(16) Uani 1 1 d . . . . .
H3A H 0.501400 0.660565 0.383347 0.093 Uiso 1 1 calc R U . . .
H3B H 0.552125 0.624974 0.434780 0.093 Uiso 1 1 calc R U . . .
H3C H 0.550245 0.569731 0.388162 0.093 Uiso 1 1 calc R U . . .
C4 C 0.6750(5) 0.7816(4) 0.4288(2) 0.0653(17) Uani 1 1 d . . . . .
H4A H 0.735408 0.807394 0.430016 0.098 Uiso 1 1 calc R U . . .
H4B H 0.668543 0.771222 0.461288 0.098 Uiso 1 1 calc R U . . .
H4C H 0.625756 0.819796 0.412422 0.098 Uiso 1 1 calc R U . . .
C5 C 0.7610(5) 0.6086(5) 0.4302(2) 0.085(2) Uani 1 1 d . . . . .
H5A H 0.764541 0.556880 0.412016 0.128 Uiso 1 1 calc R U . . .
H5B H 0.747844 0.593901 0.460823 0.128 Uiso 1 1 calc R U . . .
H5C H 0.820163 0.638825 0.435691 0.128 Uiso 1 1 calc R U . . .
C6 C 0.8900(4) 0.7915(4) 0.3555(2) 0.0644(17) Uani 1 1 d . . . . .
H6A H 0.953303 0.797282 0.351472 0.097 Uiso 1 1 calc R U . . .
H6B H 0.891881 0.778522 0.388867 0.097 Uiso 1 1 calc R U . . .
H6C H 0.856337 0.844597 0.346509 0.097 Uiso 1 1 calc R U . . .
C7 C 0.8931(4) 0.6032(4) 0.3372(2) 0.0586(16) Uani 1 1 d . . . . .
H7A H 0.864756 0.556386 0.316582 0.088 Uiso 1 1 calc R U . . .
H7B H 0.889941 0.591485 0.370057 0.088 Uiso 1 1 calc R U . . .
H7C H 0.958029 0.609139 0.335803 0.088 Uiso 1 1 calc R U . . .
C8 C 0.8479(4) 0.7226(4) 0.2553(2) 0.0644(17) Uani 1 1 d . . . . .
H8A H 0.829564 0.672197 0.235628 0.097 Uiso 1 1 calc R U . . .
H8B H 0.913507 0.734680 0.257669 0.097 Uiso 1 1 calc R U . . .
H8C H 0.810408 0.770947 0.240800 0.097 Uiso 1 1 calc R U . . .
C11 C 0.8978(3) 0.5445(3) 0.70045(18) 0.0428(12) Uani 1 1 d . . . . .
H11A H 0.835995 0.527197 0.682575 0.064 Uiso 1 1 calc R U . . .
H11B H 0.922137 0.502531 0.725241 0.064 Uiso 1 1 calc R U . . .
H11C H 0.939171 0.548450 0.678724 0.064 Uiso 1 1 calc R U . . .
C12 C 0.8449(3) 0.6309(3) 0.78316(18) 0.0420(11) Uani 1 1 d . . . . .
H12A H 0.782246 0.607369 0.773628 0.063 Uiso 1 1 calc R U . . .
H12B H 0.843302 0.684498 0.799954 0.063 Uiso 1 1 calc R U . . .
H12C H 0.885468 0.590901 0.804282 0.063 Uiso 1 1 calc R U . . .
C13 C 0.6574(4) 0.7946(5) 0.7501(2) 0.0702(19) Uani 1 1 d . . . . .
H13A H 0.683314 0.851026 0.758613 0.105 Uiso 1 1 calc R U . . .
H13B H 0.690868 0.753106 0.773059 0.105 Uiso 1 1 calc R U . . .
H13C H 0.591784 0.794275 0.750566 0.105 Uiso 1 1 calc R U . . .
C14 C 0.6049(4) 0.6646(4) 0.6738(3) 0.0724(19) Uani 1 1 d . . . . .
H14A H 0.541240 0.672042 0.677038 0.109 Uiso 1 1 calc R U . . .
H14B H 0.635418 0.620279 0.695599 0.109 Uiso 1 1 calc R U . . .
H14C H 0.603884 0.648360 0.640923 0.109 Uiso 1 1 calc R U . . .
C15 C 0.6042(4) 0.8490(4) 0.6469(2) 0.0632(17) Uani 1 1 d . . . . .
H15A H 0.607198 0.835846 0.614161 0.095 Uiso 1 1 calc R U . . .
H15B H 0.631927 0.904604 0.655905 0.095 Uiso 1 1 calc R U . . .
H15C H 0.539419 0.849487 0.649013 0.095 Uiso 1 1 calc R U . . .
C16 C 0.7223(5) 0.6578(5) 0.5753(2) 0.0691(19) Uani 1 1 d . . . . .
H16A H 0.724795 0.646907 0.542216 0.104 Uiso 1 1 calc R U . . .
H16B H 0.663014 0.684462 0.575759 0.104 Uiso 1 1 calc R U . . .
H16C H 0.728099 0.604235 0.592804 0.104 Uiso 1 1 calc R U . . .
C17 C 0.8065(5) 0.8291(4) 0.56711(19) 0.0632(17) Uani 1 1 d . . . . .
H17A H 0.807791 0.814578 0.534321 0.095 Uiso 1 1 calc R U . . .
H17B H 0.857173 0.868279 0.580301 0.095 Uiso 1 1 calc R U . . .
H17C H 0.747196 0.855996 0.567335 0.095 Uiso 1 1 calc R U . . .
C18 C 0.9301(4) 0.6775(4) 0.5967(2) 0.0631(16) Uani 1 1 d . . . . .
H18A H 0.932870 0.619701 0.609298 0.095 Uiso 1 1 calc R U . . .
H18B H 0.983915 0.709512 0.614221 0.095 Uiso 1 1 calc R U . . .
H18C H 0.930197 0.675724 0.562873 0.095 Uiso 1 1 calc R U . . .
C21 C 0.4886(4) 0.8276(5) 0.4895(3) 0.077(2) Uani 1 1 d D . . . .
H21A H 0.468016 0.796568 0.459428 0.115 Uiso 1 1 calc R U . . .
H21B H 0.516563 0.788006 0.514931 0.115 Uiso 1 1 calc R U . . .
H21C H 0.534494 0.870169 0.486055 0.115 Uiso 1 1 calc R U . . .
C22 C 0.4363(4) 0.9286(5) 0.5377(2) 0.0725(19) Uani 1 1 d D . . . .
H22A H 0.484566 0.966662 0.531029 0.087 Uiso 1 1 calc R U . . .
H22B H 0.462112 0.899637 0.568332 0.087 Uiso 1 1 calc R U . . .
C23 C 0.3555(5) 0.9784(5) 0.5414(3) 0.080(2) Uani 1 1 d . . . . .
H23A H 0.374760 1.023327 0.565568 0.096 Uiso 1 1 calc R U . . .
H23B H 0.328500 1.005886 0.510413 0.096 Uiso 1 1 calc R U . . .
C24 C 0.2093(5) 0.9709(5) 0.5599(3) 0.083(2) Uani 1 1 d . . . . .
H24A H 0.174669 0.991707 0.528772 0.125 Uiso 1 1 calc R U . . .
H24B H 0.228644 1.018911 0.581400 0.125 Uiso 1 1 calc R U . . .
H24C H 0.169746 0.933186 0.573281 0.125 Uiso 1 1 calc R U . . .
C25 C 0.4274(5) 0.6183(5) 0.5384(3) 0.088(2) Uani 1 1 d . . . . .
H25A H 0.391352 0.575951 0.551032 0.133 Uiso 1 1 calc R U . . .
H25B H 0.443368 0.665068 0.561144 0.133 Uiso 1 1 calc R U . . .
H25C H 0.484232 0.592234 0.533572 0.133 Uiso 1 1 calc R U . . .
C26 C 0.3431(5) 0.5853(4) 0.4613(3) 0.0719(19) Uani 1 1 d . . . . .
H26A H 0.298079 0.549366 0.472482 0.086 Uiso 1 1 calc R U . . .
H26B H 0.396191 0.549435 0.458584 0.086 Uiso 1 1 calc R U . . .
C27 C 0.2989(4) 0.6213(5) 0.4141(2) 0.0674(18) Uani 1 1 d . . . . .
H27A H 0.343074 0.658704 0.403132 0.081 Uiso 1 1 calc R U . . .
H27B H 0.280608 0.575243 0.390493 0.081 Uiso 1 1 calc R U . . .
C28 C 0.1681(5) 0.6951(5) 0.3728(2) 0.075(2) Uani 1 1 d . . . . .
H28A H 0.205724 0.733826 0.358731 0.112 Uiso 1 1 calc R U . . .
H28B H 0.112091 0.724321 0.376395 0.112 Uiso 1 1 calc R U . . .
H28C H 0.150770 0.645927 0.351923 0.112 Uiso 1 1 calc R U . . .
C29 C 0.2575(5) 0.9407(5) 0.4029(2) 0.075(2) Uani 1 1 d D . . . .
H29A H 0.246322 0.897706 0.377713 0.113 Uiso 1 1 calc R U . . .
H29B H 0.321137 0.935511 0.422105 0.113 Uiso 1 1 calc R U . . .
H29C H 0.248555 0.997103 0.388403 0.113 Uiso 1 1 calc R U . . .
C30 C 0.1018(4) 0.9332(4) 0.4056(2) 0.0565(15) Uani 1 1 d D . . . .
H30A H 0.088475 0.885440 0.382784 0.068 Uiso 1 1 calc R U . . .
H30B H 0.091359 0.986675 0.387273 0.068 Uiso 1 1 calc R U . . .
C31 C 0.0394(4) 0.9290(3) 0.4392(2) 0.0528(14) Uani 1 1 d D . . . .
H31A H 0.052376 0.977214 0.461649 0.063 Uiso 1 1 calc R U . . .
H31B H -0.026018 0.932928 0.421082 0.063 Uiso 1 1 calc R U . . .
C32 C -0.0098(4) 0.8425(4) 0.4950(2) 0.0651(17) Uani 1 1 d D . . . .
H32A H -0.073486 0.847114 0.475791 0.098 Uiso 1 1 calc R U . . .
H32B H 0.001656 0.887052 0.519334 0.098 Uiso 1 1 calc R U . . .
H32C H -0.000836 0.787046 0.510548 0.098 Uiso 1 1 calc R U . . .
C33 C 0.0498(5) 0.6228(5) 0.4694(3) 0.079(2) Uani 1 1 d . . . . .
H33A H 0.027892 0.663438 0.443572 0.118 Uiso 1 1 calc R U . . .
H33B H -0.003445 0.596430 0.478164 0.118 Uiso 1 1 calc R U . . .
H33C H 0.087009 0.579052 0.458721 0.118 Uiso 1 1 calc R U . . .
C34 C 0.1431(5) 0.6112(4) 0.5473(2) 0.0667(18) Uani 1 1 d . . . . .
H34A H 0.188409 0.573231 0.537719 0.080 Uiso 1 1 calc R U . . .
H34B H 0.093473 0.575945 0.554800 0.080 Uiso 1 1 calc R U . . .
C35 C 0.1901(5) 0.6605(4) 0.5904(2) 0.0663(18) Uani 1 1 d . . . . .
H35A H 0.145391 0.699766 0.599570 0.080 Uiso 1 1 calc R U . . .
H35B H 0.213638 0.621566 0.617396 0.080 Uiso 1 1 calc R U . . .
C36 C 0.3167(5) 0.7470(5) 0.6214(2) 0.079(2) Uani 1 1 d . . . . .
H36A H 0.365363 0.781375 0.613130 0.118 Uiso 1 1 calc R U . . .
H36B H 0.344945 0.704126 0.644924 0.118 Uiso 1 1 calc R U . . .
H36C H 0.276091 0.783386 0.634963 0.118 Uiso 1 1 calc R U . . .
C9A C 0.6616(11) 0.9461(10) 0.3151(6) 0.081(3) Uani 0.5 1 d D U P A -1
H9A H 0.706337 0.959837 0.296278 0.122 Uiso 0.5 1 calc R U P A -1
H9B H 0.683561 0.897054 0.335401 0.122 Uiso 0.5 1 calc R U P A -1
H9C H 0.654784 0.994625 0.335124 0.122 Uiso 0.5 1 calc R U P A -1
O2A O 0.5777(16) 0.9276(11) 0.2852(8) 0.056(3) Uani 0.5 1 d D U P A -1
C10A C 0.5201(13) 1.0011(9) 0.2837(5) 0.067(4) Uani 0.5 1 d D U P A -1
H10A H 0.558476 1.051436 0.295350 0.080 Uiso 0.5 1 calc R U P A -1
H10B H 0.475772 0.992601 0.303983 0.080 Uiso 0.5 1 calc R U P A -1
C10B C 0.4701(14) 1.0126(9) 0.2333(5) 0.068(4) Uani 0.5 1 d D U P A -1
H10C H 0.428879 1.062466 0.230327 0.082 Uiso 0.5 1 calc R U P A -1
H10D H 0.514985 1.022467 0.213489 0.082 Uiso 0.5 1 calc R U P A -1
O2B O 0.4160(17) 0.9379(12) 0.2169(9) 0.063(4) Uani 0.5 1 d D U P A -1
C9B C 0.3637(12) 0.9403(10) 0.1687(6) 0.081(3) Uani 0.5 1 d D U P A -1
H9D H 0.404154 0.956534 0.147929 0.122 Uiso 0.5 1 calc R U P A -1
H9E H 0.313624 0.981773 0.165614 0.122 Uiso 0.5 1 calc R U P A -1
H9F H 0.337286 0.884290 0.159419 0.122 Uiso 0.5 1 calc R U P A -1
O4 O 0.9050(7) 0.9897(6) 0.7295(3) 0.0574(19) Uani 0.743(13) 1 d D U P B 1
C19 C 0.9507(4) 1.0647(5) 0.7515(4) 0.071(3) Uani 0.743(13) 1 d D U P B 1
H19A H 0.947577 1.066739 0.785329 0.086 Uiso 0.743(13) 1 calc R U P B 1
H19B H 0.919004 1.115399 0.735286 0.086 Uiso 0.743(13) 1 calc R U P B 1
C20 C 0.8078(8) 0.9918(9) 0.7270(4) 0.070(3) Uani 0.743(13) 1 d D U P B 1
H20A H 0.780684 1.042631 0.709705 0.104 Uiso 0.743(13) 1 calc R U P B 1
H20B H 0.797817 0.992965 0.759287 0.104 Uiso 0.743(13) 1 calc R U P B 1
H20C H 0.778283 0.941440 0.710242 0.104 Uiso 0.743(13) 1 calc R U P B 1
O4B O 0.918(2) 0.9903(17) 0.7178(11) 0.063(4) Uani 0.257(13) 1 d D U P B 2
C19B C 0.9744(19) 1.0646(15) 0.7246(4) 0.065(4) Uani 0.257(13) 1 d D U P B 2
H19C H 0.935594 1.115983 0.717144 0.078 Uiso 0.257(13) 1 calc R U P B 2
H19D H 1.018226 1.063269 0.703606 0.078 Uiso 0.257(13) 1 calc R U P B 2
C20B C 0.825(2) 1.010(2) 0.7169(15) 0.070(6) Uani 0.257(13) 1 d D U P B 2
H20D H 0.796326 1.039334 0.687152 0.106 Uiso 0.257(13) 1 calc R U P B 2
H20E H 0.822670 1.046745 0.744012 0.106 Uiso 0.257(13) 1 calc R U P B 2
H20F H 0.790451 0.957790 0.719108 0.106 Uiso 0.257(13) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2A 2.553(18) . ?
U1 O1 2.587(4) . ?
U1 O2B 2.71(2) . ?
U1 I1 3.1064(4) 2_655 ?
U1 I1 3.1065(4) . ?
U1 Si2 3.1280(12) 2_655 ?
U1 Si2 3.1281(12) . ?
U2 O3 2.528(4) . ?
U2 O4B 2.61(3) . ?
U2 O4B 2.61(3) 2_756 ?
U2 O4 2.622(10) 2_756 ?
U2 O4 2.622(10) . ?
U2 I2 3.1319(3) . ?
U2 I2 3.1320(3) 2_756 ?
U2 Si6 3.1457(13) 2_756 ?
U2 Si6 3.1457(13) . ?
K1 O10 2.752(4) . ?
K1 O7 2.794(4) . ?
K1 O9 2.848(4) . ?
K1 O11 2.860(4) . ?
K1 O6 2.861(4) . ?
K1 O5 2.862(4) . ?
K1 O12 2.880(4) . ?
K1 O8 2.917(4) . ?
Si1 O1 1.6971(19) . ?
Si1 C1 1.861(5) . ?
Si1 C2 1.878(5) . ?
Si1 Si2 2.3084(18) . ?
Si2 Si4 2.3299(18) . ?
Si2 Si3 2.3445(19) . ?
Si3 C5 1.882(6) . ?
Si3 C4 1.883(6) . ?
Si3 C3 1.892(6) . ?
Si4 C7 1.871(6) . ?
Si4 C8 1.875(6) . ?
Si4 C6 1.881(6) . ?
Si5 O3 1.7163(19) . ?
Si5 C11 1.869(5) . ?
Si5 C12 1.880(5) . ?
Si5 Si6 2.3197(18) . ?
Si6 Si7 2.3352(18) . ?
Si6 Si8 2.3463(18) . ?
Si7 C14 1.870(7) . ?
Si7 C15 1.883(6) . ?
Si7 C13 1.887(6) . ?
Si8 C17 1.874(6) . ?
Si8 C16 1.889(6) . ?
Si8 C18 1.892(6) . ?
O5 C21 1.412(7) . ?
O5 C22 1.414(7) . ?
O6 C24 1.405(7) . ?
O6 C23 1.417(7) . ?
O7 C28 1.410(7) . ?
O7 C27 1.417(7) . ?
O8 C26 1.391(8) . ?
O8 C25 1.428(8) . ?
O9 C34 1.390(7) . ?
O9 C33 1.439(8) . ?
O10 C36 1.410(8) . ?
O10 C35 1.414(7) . ?
O11 C30 1.414(6) . ?
O11 C29 1.421(7) . ?
O12 C31 1.414(6) . ?
O12 C32 1.441(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.462(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
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 C27 1.481(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
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 C31 1.496(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
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 C35 1.494(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C9A O2A 1.370(17) . ?
C9A H9A 0.9800 . ?
C9A H9B 0.9800 . ?
C9A H9C 0.9800 . ?
O2A C10A 1.437(16) . ?
C10A C10B 1.481(8) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C10B O2B 1.444(15) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
O2B C9B 1.424(18) . ?
C9B H9D 0.9800 . ?
C9B H9E 0.9800 . ?
C9B H9F 0.9800 . ?
O4 C20 1.431(10) . ?
O4 C19 1.438(9) . ?
C19 C19 1.489(9) 2_756 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
O4B C20B 1.414(16) . ?
O4B C19B 1.433(16) . ?
C19B C19B 1.485(10) 2_756 ?
C19B H19C 0.9900 . ?
C19B H19D 0.9900 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A U1 O1 148.2(4) . . ?
O2A U1 O2B 62.3(2) . . ?
O1 U1 O2B 149.4(4) . . ?
O2A U1 I1 84.4(7) . 2_655 ?
O1 U1 I1 100.422(10) . 2_655 ?
O2B U1 I1 80.4(7) . 2_655 ?
O2A U1 I1 77.9(7) . . ?
O1 U1 I1 100.421(10) . . ?
O2B U1 I1 81.7(7) . . ?
I1 U1 I1 159.157(19) 2_655 . ?
O2A U1 Si2 147.1(4) . 2_655 ?
O1 U1 Si2 64.47(2) . 2_655 ?
O2B U1 Si2 84.9(4) . 2_655 ?
I1 U1 Si2 93.99(3) 2_655 2_655 ?
I1 U1 Si2 94.95(3) . 2_655 ?
O2A U1 Si2 83.9(4) . . ?
O1 U1 Si2 64.47(2) . . ?
O2B U1 Si2 146.1(4) . . ?
I1 U1 Si2 94.95(3) 2_655 . ?
I1 U1 Si2 93.99(3) . . ?
Si2 U1 Si2 128.94(5) 2_655 . ?
O3 U2 O4B 148.8(7) . . ?
O3 U2 O4B 148.8(7) . 2_756 ?
O4B U2 O4B 62.4(13) . 2_756 ?
O3 U2 O4 147.8(2) . 2_756 ?
O3 U2 O4 147.8(2) . . ?
O4 U2 O4 64.3(4) 2_756 . ?
O3 U2 I2 98.911(8) . . ?
O4B U2 I2 85.2(6) . . ?
O4B U2 I2 79.6(6) 2_756 . ?
O4 U2 I2 88.88(19) 2_756 . ?
O4 U2 I2 75.95(19) . . ?
O3 U2 I2 98.912(8) . 2_756 ?
O4 U2 I2 75.95(19) 2_756 2_756 ?
O4 U2 I2 88.88(19) . 2_756 ?
I2 U2 I2 162.177(16) . 2_756 ?
O3 U2 Si6 64.98(2) . 2_756 ?
O4 U2 Si6 84.0(2) 2_756 2_756 ?
O4 U2 Si6 145.2(2) . 2_756 ?
I2 U2 Si6 90.01(2) . 2_756 ?
I2 U2 Si6 97.52(2) 2_756 2_756 ?
O3 U2 Si6 64.98(2) . . ?
O4B U2 Si6 83.8(7) . . ?
O4B U2 Si6 146.2(6) 2_756 . ?
O4 U2 Si6 145.2(2) 2_756 . ?
O4 U2 Si6 84.0(2) . . ?
I2 U2 Si6 97.52(2) . . ?
I2 U2 Si6 90.01(2) 2_756 . ?
Si6 U2 Si6 129.96(5) 2_756 . ?
O10 K1 O7 112.86(14) . . ?
O10 K1 O9 59.90(13) . . ?
O7 K1 O9 76.32(12) . . ?
O10 K1 O11 151.23(13) . . ?
O7 K1 O11 95.02(12) . . ?
O9 K1 O11 124.43(12) . . ?
O10 K1 O6 79.38(13) . . ?
O7 K1 O6 164.15(12) . . ?
O9 K1 O6 119.39(12) . . ?
O11 K1 O6 74.65(12) . . ?
O10 K1 O5 101.68(14) . . ?
O7 K1 O5 106.88(12) . . ?
O9 K1 O5 159.92(13) . . ?
O11 K1 O5 75.46(12) . . ?
O6 K1 O5 59.30(12) . . ?
O10 K1 O12 109.74(12) . . ?
O7 K1 O12 96.67(12) . . ?
O9 K1 O12 68.82(12) . . ?
O11 K1 O12 57.70(11) . . ?
O6 K1 O12 88.00(12) . . ?
O5 K1 O12 129.06(12) . . ?
O10 K1 O8 73.75(12) . . ?
O7 K1 O8 58.46(12) . . ?
O9 K1 O8 91.59(13) . . ?
O11 K1 O8 130.42(12) . . ?
O6 K1 O8 119.34(13) . . ?
O5 K1 O8 74.38(12) . . ?
O12 K1 O8 152.23(13) . . ?
O1 Si1 C1 105.33(17) . . ?
O1 Si1 C2 108.6(2) . . ?
C1 Si1 C2 106.8(2) . . ?
O1 Si1 Si2 99.51(14) . . ?
C1 Si1 Si2 113.89(17) . . ?
C2 Si1 Si2 121.26(18) . . ?
Si1 Si2 Si4 105.71(7) . . ?
Si1 Si2 Si3 106.87(7) . . ?
Si4 Si2 Si3 106.11(7) . . ?
Si1 Si2 U1 80.09(5) . . ?
Si4 Si2 U1 132.70(6) . . ?
Si3 Si2 U1 117.12(6) . . ?
C5 Si3 C4 106.4(3) . . ?
C5 Si3 C3 105.7(3) . . ?
C4 Si3 C3 106.5(3) . . ?
C5 Si3 Si2 114.9(2) . . ?
C4 Si3 Si2 109.0(2) . . ?
C3 Si3 Si2 113.9(2) . . ?
C7 Si4 C8 105.2(3) . . ?
C7 Si4 C6 107.5(3) . . ?
C8 Si4 C6 106.8(3) . . ?
C7 Si4 Si2 115.9(2) . . ?
C8 Si4 Si2 111.83(19) . . ?
C6 Si4 Si2 109.0(2) . . ?
O3 Si5 C11 109.4(2) . . ?
O3 Si5 C12 104.94(16) . . ?
C11 Si5 C12 107.1(2) . . ?
O3 Si5 Si6 98.91(13) . . ?
C11 Si5 Si6 121.08(18) . . ?
C12 Si5 Si6 113.95(17) . . ?
Si5 Si6 Si7 105.32(7) . . ?
Si5 Si6 Si8 105.94(7) . . ?
Si7 Si6 Si8 105.37(7) . . ?
Si5 Si6 U2 79.03(4) . . ?
Si7 Si6 U2 130.29(6) . . ?
Si8 Si6 U2 121.24(6) . . ?
C14 Si7 C15 106.9(3) . . ?
C14 Si7 C13 104.9(3) . . ?
C15 Si7 C13 106.6(3) . . ?
C14 Si7 Si6 116.2(2) . . ?
C15 Si7 Si6 109.5(2) . . ?
C13 Si7 Si6 112.1(2) . . ?
C17 Si8 C16 106.6(3) . . ?
C17 Si8 C18 106.5(3) . . ?
C16 Si8 C18 106.0(3) . . ?
C17 Si8 Si6 109.8(2) . . ?
C16 Si8 Si6 114.3(2) . . ?
C18 Si8 Si6 113.2(2) . . ?
Si1 O1 Si1 139.3(3) . 2_655 ?
Si1 O1 U1 110.36(15) . . ?
Si1 O1 U1 110.36(15) 2_655 . ?
Si5 O3 Si5 137.3(3) 2_756 . ?
Si5 O3 U2 111.37(13) 2_756 . ?
Si5 O3 U2 111.37(13) . . ?
C21 O5 C22 114.0(5) . . ?
C21 O5 K1 122.2(4) . . ?
C22 O5 K1 116.2(3) . . ?
C24 O6 C23 113.7(5) . . ?
C24 O6 K1 111.6(4) . . ?
C23 O6 K1 112.6(3) . . ?
C28 O7 C27 111.5(5) . . ?
C28 O7 K1 116.6(4) . . ?
C27 O7 K1 118.0(3) . . ?
C26 O8 C25 112.3(5) . . ?
C26 O8 K1 114.1(4) . . ?
C25 O8 K1 120.1(4) . . ?
C34 O9 C33 112.6(5) . . ?
C34 O9 K1 112.1(4) . . ?
C33 O9 K1 117.0(4) . . ?
C36 O10 C35 110.9(5) . . ?
C36 O10 K1 120.5(4) . . ?
C35 O10 K1 118.4(3) . . ?
C30 O11 C29 111.2(4) . . ?
C30 O11 K1 115.0(3) . . ?
C29 O11 K1 112.6(4) . . ?
C31 O12 C32 111.5(4) . . ?
C31 O12 K1 119.0(3) . . ?
C32 O12 K1 120.8(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 . . ?
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 . . ?
Si3 C3 H3A 109.5 . . ?
Si3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si4 C6 H6A 109.5 . . ?
Si4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si5 C11 H11A 109.5 . . ?
Si5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si5 C12 H12A 109.5 . . ?
Si5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si7 C13 H13A 109.5 . . ?
Si7 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si7 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si7 C14 H14A 109.5 . . ?
Si7 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si7 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si7 C15 H15A 109.5 . . ?
Si7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si8 C16 H16A 109.5 . . ?
Si8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si8 C17 H17A 109.5 . . ?
Si8 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si8 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si8 C18 H18A 109.5 . . ?
Si8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O5 C21 H21A 109.5 . . ?
O5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C23 110.7(5) . . ?
O5 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
O5 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
O6 C23 C22 110.8(6) . . ?
O6 C23 H23A 109.5 . . ?
C22 C23 H23A 109.5 . . ?
O6 C23 H23B 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
O6 C24 H24A 109.5 . . ?
O6 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O6 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O8 C25 H25A 109.5 . . ?
O8 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O8 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O8 C26 C27 110.4(6) . . ?
O8 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
O8 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
O7 C27 C26 109.0(5) . . ?
O7 C27 H27A 109.9 . . ?
C26 C27 H27A 109.9 . . ?
O7 C27 H27B 109.9 . . ?
C26 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
O7 C28 H28A 109.5 . . ?
O7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O11 C29 H29A 109.5 . . ?
O11 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O11 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O11 C30 C31 108.6(4) . . ?
O11 C30 H30A 110.0 . . ?
C31 C30 H30A 110.0 . . ?
O11 C30 H30B 110.0 . . ?
C31 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
O12 C31 C30 109.7(4) . . ?
O12 C31 H31A 109.7 . . ?
C30 C31 H31A 109.7 . . ?
O12 C31 H31B 109.7 . . ?
C30 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
O12 C32 H32A 109.5 . . ?
O12 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O12 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O9 C33 H33A 109.5 . . ?
O9 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O9 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O9 C34 C35 110.1(5) . . ?
O9 C34 H34A 109.6 . . ?
C35 C34 H34A 109.6 . . ?
O9 C34 H34B 109.6 . . ?
C35 C34 H34B 109.6 . . ?
H34A C34 H34B 108.2 . . ?
O10 C35 C34 109.2(5) . . ?
O10 C35 H35A 109.8 . . ?
C34 C35 H35A 109.8 . . ?
O10 C35 H35B 109.8 . . ?
C34 C35 H35B 109.8 . . ?
H35A C35 H35B 108.3 . . ?
O10 C36 H36A 109.5 . . ?
O10 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O10 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O2A C9A H9A 109.5 . . ?
O2A C9A H9B 109.5 . . ?
H9A C9A H9B 109.5 . . ?
O2A C9A H9C 109.5 . . ?
H9A C9A H9C 109.5 . . ?
H9B C9A H9C 109.5 . . ?
C9A O2A C10A 107.0(14) . . ?
C9A O2A U1 133.6(12) . . ?
C10A O2A U1 117.8(11) . . ?
O2A C10A C10B 106.5(14) . . ?
O2A C10A H10A 110.4 . . ?
C10B C10A H10A 110.4 . . ?
O2A C10A H10B 110.4 . . ?
C10B C10A H10B 110.4 . . ?
H10A C10A H10B 108.6 . . ?
O2B C10B C10A 109.5(14) . . ?
O2B C10B H10C 109.8 . . ?
C10A C10B H10C 109.8 . . ?
O2B C10B H10D 109.8 . . ?
C10A C10B H10D 109.8 . . ?
H10C C10B H10D 108.2 . . ?
C9B O2B C10B 115.6(17) . . ?
C9B O2B U1 117.8(14) . . ?
C10B O2B U1 114.5(11) . . ?
O2B C9B H9D 109.5 . . ?
O2B C9B H9E 109.5 . . ?
H9D C9B H9E 109.5 . . ?
O2B C9B H9F 109.5 . . ?
H9D C9B H9F 109.5 . . ?
H9E C9B H9F 109.5 . . ?
C20 O4 C19 111.6(8) . . ?
C20 O4 U2 121.0(6) . . ?
C19 O4 U2 115.2(6) . . ?
O4 C19 C19 110.0(7) . 2_756 ?
O4 C19 H19A 109.7 . . ?
C19 C19 H19A 109.7 2_756 . ?
O4 C19 H19B 109.7 . . ?
C19 C19 H19B 109.7 2_756 . ?
H19A C19 H19B 108.2 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C20B O4B C19B 111(2) . . ?
C20B O4B U2 124.7(19) . . ?
C19B O4B U2 116.2(18) . . ?
O4B C19B H19C 110.5 . . ?
C19B C19B H19C 110.5 2_756 . ?
O4B C19B H19D 110.5 . . ?
C19B C19B H19D 110.5 2_756 . ?
H19C C19B H19D 108.6 . . ?
O4B C20B H20D 109.5 . . ?
O4B C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
O4B C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Si1 O1 Si1 85.02(18) . . . 2_655 ?
C2 Si1 O1 Si1 -29.13(18) . . . 2_655 ?
Si2 Si1 O1 Si1 -156.83(6) . . . 2_655 ?
C1 Si1 O1 U1 -94.98(18) . . . . ?
C2 Si1 O1 U1 150.87(18) . . . . ?
Si2 Si1 O1 U1 23.17(6) . . . . ?
C11 Si5 O3 Si5 -28.77(18) . . . 2_756 ?
C12 Si5 O3 Si5 85.84(18) . . . 2_756 ?
Si6 Si5 O3 Si5 -156.30(6) . . . 2_756 ?
C11 Si5 O3 U2 151.23(18) . . . . ?
C12 Si5 O3 U2 -94.16(18) . . . . ?
Si6 Si5 O3 U2 23.70(6) . . . . ?
C21 O5 C22 C23 169.4(6) . . . . ?
K1 O5 C22 C23 -40.2(7) . . . . ?
C24 O6 C23 C22 178.3(6) . . . . ?
K1 O6 C23 C22 -53.5(7) . . . . ?
O5 C22 C23 O6 63.5(8) . . . . ?
C25 O8 C26 C27 -172.5(5) . . . . ?
K1 O8 C26 C27 46.5(6) . . . . ?
C28 O7 C27 C26 -172.6(6) . . . . ?
K1 O7 C27 C26 48.4(6) . . . . ?
O8 C26 C27 O7 -62.9(7) . . . . ?
C29 O11 C30 C31 -174.4(5) . . . . ?
K1 O11 C30 C31 56.2(5) . . . . ?
C32 O12 C31 C30 -175.7(5) . . . . ?
K1 O12 C31 C30 36.4(6) . . . . ?
O11 C30 C31 O12 -60.3(6) . . . . ?
C33 O9 C34 C35 -172.9(5) . . . . ?
K1 O9 C34 C35 52.6(6) . . . . ?
C36 O10 C35 C34 -173.6(5) . . . . ?
K1 O10 C35 C34 40.9(6) . . . . ?
O9 C34 C35 O10 -62.8(7) . . . . ?
C9A O2A C10A C10B 138.0(18) . . . . ?
U1 O2A C10A C10B -54.4(19) . . . . ?
O2A C10A C10B O2B 59.0(13) . . . . ?
C10A C10B O2B C9B 179.7(19) . . . . ?
C10A C10B O2B U1 -38(2) . . . . ?
C20 O4 C19 C19 -173.6(10) . . . 2_756 ?
U2 O4 C19 C19 43.5(12) . . . 2_756 ?
C20B O4B C19B C19B 102(3) . . . 2_756 ?
U2 O4B C19B C19B -49(3) . . . 2_756 ?

_refine_diff_density_max         1.699
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.136




####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NLguest3_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2325811'
loop_
_audit_author_name
_audit_author_address
'Matthias Zeller'
;Purdue University
United States of America
;
_audit_update_record             
;
2024-01-15 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;

_vrf_PLAT910_NLguest3_0m_a       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 11 Note

RESPONSE: Data were collected with a sealed tube molybdenum wavelength
instrument with 0.6 mm beam size and the smallest suitable beam stop. The
crystal to beam stop distance is not adjustable. For large unit cell sizes
such as is the case here some reflections are obstructed by the beam stop (11
out of a total of 20794 independent reflections, or 0.05%).
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H88 I2 K O9 Si8 U, C4 H10 O'
_chemical_formula_sum            'C40 H98 I2 K O10 Si8 U'
_chemical_formula_weight         1494.83

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'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   49.049(13)
_cell_length_b                   13.108(5)
_cell_length_c                   21.124(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.054(19)
_cell_angle_gamma                90
_cell_volume                     13581(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9729
_cell_measurement_theta_min      2.2121
_cell_measurement_theta_max      29.4964

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             5976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.542
_shelx_estimated_absorpt_T_min   0.484
_shelx_estimated_absorpt_T_max   0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5664
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_measurement_device_type  
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean 7.4074


_diffrn_reflns_number            179769
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.491
_diffrn_reflns_theta_max         30.599
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             20794
_reflns_number_gt                13797
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex4 v2021.4-0 (Bruker, 2021)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
;  
SHELXL-2019/3 (Sheldrick, 2015, 2019), 
SHELXLE Rev1275(Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Six reflections were obstructed by the beamstop and were omitted from 
refinement.

#---

Atoms (within the same PART) were restrained to be 0.02 Angstrom from 
each other.

#---

THF molecule disorder:

One of the two THF molecules on the uranium center were found to be 
disordered (O2). The 1,2 and 1,3 positions for disordered moieties were 
restrained to have similar geometries to each other. The position and 
Uij of the anisotropic displacement parameters (ADPs) were constrained 
to be the same for atoms O2 and O2B.

THF molecules containing O3 was initially modelled as disordered. However,
the second disordered moiety was found to be < 5% and thus was omitted 
from further disorder modelling (FVAR 3 = 0.96824) and was refined 
using FVAR 1 during the final refinement process.

The Uij components of ADPs for disordered atoms closer to each 
other than 2.0 Angstrom were restrained to be similar with an esd of 
0.01 Angstrom squared. 

Under these conditions, the THF O2/O2B was found to have an occupancy ratio of
0.613(11) : 0.387(11).

#---

Diethyl ether molecule disorder:

There is an outersphere diethyl ether molecule that was found to be disordered
into two positions over an inversion center, defining four different positions 
for one ether molecule. The 1,2 and 1,3 positions for disordered ether 
molecules were restrained to have similar geometries to a well-defined ether 
molecule (which has O10 on an inversion center).

The Uij components of ADPs for disordered atoms closer to each other than 2.0 
Angstrom were restrained to be similar with an esd of 0.01 Angstrom squared. 

Under these conditions, the diethyl ether molecule O11/O11B was found to have 
an occupancy ratio of 0.291(13) : 0.209(13).
Thus, a PART ratio of 0.582(26) : 0.418(26).

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²+40.3862P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20794
_refine_ls_number_parameters     687
_refine_ls_number_restraints     300
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1152
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.62748(2) 0.12493(2) 0.31874(2) 0.03219(5) Uani 1 1 d . . . . .
I1 I 0.62049(2) -0.09729(3) 0.36748(2) 0.06008(10) Uani 1 1 d . . . . .
I2 I 0.62764(2) 0.32441(3) 0.24129(2) 0.06152(11) Uani 1 1 d . . . . .
K1 K 0.61526(2) 0.51780(8) 0.61964(5) 0.0398(2) Uani 1 1 d . . . . .
Si1 Si 0.57522(2) 0.19563(10) 0.39537(6) 0.0373(3) Uani 1 1 d . . . . .
Si2 Si 0.60903(2) 0.21807(10) 0.47046(5) 0.0365(3) Uani 1 1 d . . . . .
Si3 Si 0.67004(2) 0.25835(11) 0.42688(6) 0.0419(3) Uani 1 1 d . . . . .
Si4 Si 0.68946(2) 0.15649(11) 0.35004(6) 0.0384(3) Uani 1 1 d . . . . .
Si5 Si 0.55561(3) 0.35744(13) 0.38112(8) 0.0546(4) Uani 1 1 d . . . . .
Si6 Si 0.54154(3) 0.10454(12) 0.44921(7) 0.0493(3) Uani 1 1 d . . . . .
Si7 Si 0.72475(3) 0.25543(14) 0.30798(7) 0.0561(4) Uani 1 1 d . . . . .
Si8 Si 0.71100(3) 0.02757(14) 0.40752(7) 0.0568(4) Uani 1 1 d . . . . .
O1 O 0.63729(6) 0.2141(2) 0.42375(13) 0.0353(6) Uani 1 1 d . . . . .
O4 O 0.64203(9) 0.3642(3) 0.69402(19) 0.0588(10) Uani 1 1 d . . . . .
O5 O 0.67082(7) 0.5112(3) 0.62759(17) 0.0574(9) Uani 1 1 d . . . . .
O6 O 0.64631(8) 0.6393(3) 0.53900(19) 0.0635(10) Uani 1 1 d . . . . .
O7 O 0.58935(8) 0.6667(3) 0.5495(2) 0.0695(11) Uani 1 1 d . . . . .
O8 O 0.55874(7) 0.5083(3) 0.60286(19) 0.0631(10) Uani 1 1 d . . . . .
O9 O 0.58445(9) 0.3882(3) 0.6942(2) 0.0637(10) Uani 1 1 d . . . . .
C1 C 0.61352(12) 0.1099(5) 0.5278(2) 0.0588(15) Uani 1 1 d . . . . .
H1A H 0.612379 0.044881 0.504963 0.088 Uiso 1 1 calc R U . . .
H1B H 0.599145 0.112760 0.559898 0.088 Uiso 1 1 calc R U . . .
H1C H 0.631375 0.115459 0.548314 0.088 Uiso 1 1 calc R U . . .
C2 C 0.61032(11) 0.3363(5) 0.5193(3) 0.0601(15) Uani 1 1 d . . . . .
H2A H 0.625921 0.332867 0.548213 0.090 Uiso 1 1 calc R U . . .
H2B H 0.593448 0.342454 0.543817 0.090 Uiso 1 1 calc R U . . .
H2C H 0.612255 0.395728 0.491517 0.090 Uiso 1 1 calc R U . . .
C3 C 0.66805(12) 0.3978(4) 0.4074(3) 0.0662(17) Uani 1 1 d . . . . .
H3A H 0.660984 0.406343 0.364357 0.099 Uiso 1 1 calc R U . . .
H3B H 0.686276 0.428035 0.410340 0.099 Uiso 1 1 calc R U . . .
H3C H 0.655841 0.431777 0.437476 0.099 Uiso 1 1 calc R U . . .
C4 C 0.68205(11) 0.2491(6) 0.5111(3) 0.0661(17) Uani 1 1 d . . . . .
H4A H 0.681457 0.177758 0.524868 0.099 Uiso 1 1 calc R U . . .
H4B H 0.670175 0.290250 0.538272 0.099 Uiso 1 1 calc R U . . .
H4C H 0.700802 0.274517 0.514117 0.099 Uiso 1 1 calc R U . . .
C5 C 0.53258(11) 0.4006(5) 0.4482(3) 0.0658(16) Uani 1 1 d . . . . .
H5A H 0.524494 0.466807 0.437494 0.099 Uiso 1 1 calc R U . . .
H5B H 0.543301 0.407116 0.487138 0.099 Uiso 1 1 calc R U . . .
H5C H 0.518068 0.350288 0.454474 0.099 Uiso 1 1 calc R U . . .
C6 C 0.58119(14) 0.4621(5) 0.3697(4) 0.085(2) Uani 1 1 d . . . . .
H6A H 0.594489 0.441500 0.337572 0.127 Uiso 1 1 calc R U . . .
H6B H 0.590615 0.475310 0.409803 0.127 Uiso 1 1 calc R U . . .
H6C H 0.571823 0.524238 0.355783 0.127 Uiso 1 1 calc R U . . .
C7 C 0.53376(18) 0.3561(7) 0.3080(4) 0.098(3) Uani 1 1 d . . . . .
H7A H 0.544922 0.337339 0.271317 0.147 Uiso 1 1 calc R U . . .
H7B H 0.525914 0.423980 0.301288 0.147 Uiso 1 1 calc R U . . .
H7C H 0.519053 0.306177 0.313183 0.147 Uiso 1 1 calc R U . . .
C8 C 0.53347(13) 0.1511(5) 0.5316(3) 0.0665(16) Uani 1 1 d . . . . .
H8A H 0.526959 0.221727 0.529510 0.100 Uiso 1 1 calc R U . . .
H8B H 0.549949 0.147985 0.557768 0.100 Uiso 1 1 calc R U . . .
H8C H 0.519303 0.107857 0.550241 0.100 Uiso 1 1 calc R U . . .
C9 C 0.55035(13) -0.0338(5) 0.4579(3) 0.0689(17) Uani 1 1 d . . . . .
H9A H 0.553054 -0.063973 0.415974 0.103 Uiso 1 1 calc R U . . .
H9B H 0.535456 -0.069234 0.479646 0.103 Uiso 1 1 calc R U . . .
H9C H 0.567139 -0.040501 0.482773 0.103 Uiso 1 1 calc R U . . .
C10 C 0.50869(12) 0.1103(6) 0.4026(3) 0.081(2) Uani 1 1 d . . . . .
H10A H 0.512121 0.089262 0.358823 0.122 Uiso 1 1 calc R U . . .
H10B H 0.501620 0.180178 0.403096 0.122 Uiso 1 1 calc R U . . .
H10C H 0.495272 0.064280 0.421783 0.122 Uiso 1 1 calc R U . . .
C11 C 0.74684(14) 0.3204(7) 0.3678(4) 0.097(3) Uani 1 1 d . . . . .
H11A H 0.761114 0.359162 0.346046 0.145 Uiso 1 1 calc R U . . .
H11B H 0.755266 0.269119 0.395360 0.145 Uiso 1 1 calc R U . . .
H11C H 0.735733 0.366855 0.393354 0.145 Uiso 1 1 calc R U . . .
C12 C 0.74836(13) 0.1753(7) 0.2594(3) 0.087(2) Uani 1 1 d . . . . .
H12A H 0.738444 0.147297 0.223036 0.131 Uiso 1 1 calc R U . . .
H12B H 0.755453 0.119293 0.285345 0.131 Uiso 1 1 calc R U . . .
H12C H 0.763548 0.217361 0.244340 0.131 Uiso 1 1 calc R U . . .
C13 C 0.71133(13) 0.3578(6) 0.2549(4) 0.087(3) Uani 1 1 d . . . . .
H13A H 0.726569 0.391335 0.233271 0.131 Uiso 1 1 calc R U . . .
H13B H 0.701350 0.408195 0.280132 0.131 Uiso 1 1 calc R U . . .
H13C H 0.699048 0.327683 0.223426 0.131 Uiso 1 1 calc R U . . .
C14 C 0.68833(12) -0.0327(5) 0.4693(3) 0.0691(17) Uani 1 1 d . . . . .
H14A H 0.669972 -0.041879 0.451876 0.104 Uiso 1 1 calc R U . . .
H14B H 0.687443 0.011741 0.506564 0.104 Uiso 1 1 calc R U . . .
H14C H 0.695815 -0.099138 0.481532 0.104 Uiso 1 1 calc R U . . .
C15 C 0.7205(2) -0.0755(6) 0.3514(4) 0.105(3) Uani 1 1 d . . . . .
H15A H 0.729229 -0.045621 0.313956 0.157 Uiso 1 1 calc R U . . .
H15B H 0.704133 -0.112860 0.338457 0.157 Uiso 1 1 calc R U . . .
H15C H 0.733278 -0.122542 0.372041 0.157 Uiso 1 1 calc R U . . .
C16 C 0.74318(12) 0.0680(7) 0.4490(3) 0.089(2) Uani 1 1 d . . . . .
H16A H 0.755741 0.098328 0.418254 0.134 Uiso 1 1 calc R U . . .
H16B H 0.751783 0.008372 0.468634 0.134 Uiso 1 1 calc R U . . .
H16C H 0.738784 0.118331 0.481740 0.134 Uiso 1 1 calc R U . . .
C25 C 0.66784(12) 0.3989(5) 0.7144(3) 0.0628(15) Uani 1 1 d . . . . .
H25A H 0.677426 0.343880 0.737494 0.075 Uiso 1 1 calc R U . . .
H25B H 0.665609 0.457649 0.743401 0.075 Uiso 1 1 calc R U . . .
C26 C 0.68414(11) 0.4303(5) 0.6578(3) 0.0638(16) Uani 1 1 d . . . . .
H26A H 0.702613 0.451862 0.671192 0.077 Uiso 1 1 calc R U . . .
H26B H 0.686008 0.372060 0.628322 0.077 Uiso 1 1 calc R U . . .
C27 C 0.68615(11) 0.5582(5) 0.5793(3) 0.0663(16) Uani 1 1 d . . . . .
H27A H 0.686786 0.513668 0.541534 0.080 Uiso 1 1 calc R U . . .
H27B H 0.705055 0.570153 0.594025 0.080 Uiso 1 1 calc R U . . .
C28 C 0.67302(12) 0.6563(6) 0.5633(3) 0.0711(18) Uani 1 1 d . . . . .
H28A H 0.671969 0.699616 0.601600 0.085 Uiso 1 1 calc R U . . .
H28B H 0.684122 0.692580 0.531314 0.085 Uiso 1 1 calc R U . . .
C29 C 0.63289(14) 0.7336(6) 0.5232(4) 0.080(2) Uani 1 1 d . . . . .
H29A H 0.643285 0.769958 0.489984 0.095 Uiso 1 1 calc R U . . .
H29B H 0.631853 0.778045 0.561003 0.095 Uiso 1 1 calc R U . . .
C30 C 0.60486(14) 0.7097(6) 0.4999(3) 0.083(2) Uani 1 1 d . . . . .
H30A H 0.595957 0.772866 0.484558 0.099 Uiso 1 1 calc R U . . .
H30B H 0.605915 0.661075 0.464090 0.099 Uiso 1 1 calc R U . . .
C31 C 0.56177(13) 0.6470(6) 0.5317(4) 0.085(2) Uani 1 1 d . . . . .
H31A H 0.561330 0.598973 0.495526 0.102 Uiso 1 1 calc R U . . .
H31B H 0.552849 0.711250 0.518429 0.102 Uiso 1 1 calc R U . . .
C32 C 0.54689(13) 0.6023(6) 0.5863(4) 0.086(2) Uani 1 1 d . . . . .
H32A H 0.547715 0.649572 0.622752 0.103 Uiso 1 1 calc R U . . .
H32B H 0.527503 0.592013 0.574876 0.103 Uiso 1 1 calc R U . . .
C33 C 0.54422(13) 0.4611(6) 0.6525(4) 0.081(2) Uani 1 1 d . . . . .
H33A H 0.525336 0.446303 0.638682 0.098 Uiso 1 1 calc R U . . .
H33B H 0.543395 0.507344 0.689507 0.098 Uiso 1 1 calc R U . . .
C34 C 0.55841(14) 0.3637(6) 0.6704(4) 0.079(2) Uani 1 1 d . . . . .
H34A H 0.547731 0.327119 0.703029 0.095 Uiso 1 1 calc R U . . .
H34B H 0.560123 0.318931 0.632885 0.095 Uiso 1 1 calc R U . . .
C35 C 0.59820(15) 0.3045(5) 0.7213(4) 0.080(2) Uani 1 1 d . . . . .
H35A H 0.600861 0.250570 0.689105 0.096 Uiso 1 1 calc R U . . .
H35B H 0.587187 0.275719 0.756290 0.096 Uiso 1 1 calc R U . . .
C36 C 0.62504(16) 0.3388(6) 0.7459(3) 0.081(2) Uani 1 1 d . . . . .
H36A H 0.622611 0.399067 0.773561 0.097 Uiso 1 1 calc R U . . .
H36B H 0.633547 0.283723 0.771179 0.097 Uiso 1 1 calc R U . . .
O2 O 0.59133(7) 0.0692(4) 0.23707(16) 0.0643(10) Uani 0.613(11) 1 d D U P A 1
C17 C 0.5672(2) 0.0097(17) 0.2534(7) 0.072(2) Uani 0.613(11) 1 d D U P A 1
H17A H 0.563412 0.012661 0.299415 0.086 Uiso 0.613(11) 1 calc R U P A 1
H17B H 0.569172 -0.062415 0.240364 0.086 Uiso 0.613(11) 1 calc R U P A 1
C18 C 0.5454(2) 0.0619(11) 0.2163(5) 0.079(2) Uani 0.613(11) 1 d D U P A 1
H18A H 0.535402 0.111475 0.243081 0.095 Uiso 0.613(11) 1 calc R U P A 1
H18B H 0.532228 0.011845 0.199041 0.095 Uiso 0.613(11) 1 calc R U P A 1
C19 C 0.5603(2) 0.1154(12) 0.1640(6) 0.087(3) Uani 0.613(11) 1 d D U P A 1
H19A H 0.558481 0.190310 0.168433 0.104 Uiso 0.613(11) 1 calc R U P A 1
H19B H 0.552825 0.095067 0.122297 0.104 Uiso 0.613(11) 1 calc R U P A 1
C20 C 0.5905(2) 0.0837(11) 0.1693(4) 0.072(2) Uani 0.613(11) 1 d D U P A 1
H20A H 0.594429 0.019977 0.145871 0.087 Uiso 0.613(11) 1 calc R U P A 1
H20B H 0.603018 0.138402 0.155110 0.087 Uiso 0.613(11) 1 calc R U P A 1
O2B O 0.59133(7) 0.0692(4) 0.23707(16) 0.0643(10) Uani 0.387(11) 1 d D U P A 2
C17B C 0.5646(4) 0.027(3) 0.2535(9) 0.072(3) Uani 0.387(11) 1 d D U P A 2
H17C H 0.552849 0.079852 0.273306 0.087 Uiso 0.387(11) 1 calc R U P A 2
H17D H 0.566347 -0.031274 0.282787 0.087 Uiso 0.387(11) 1 calc R U P A 2
C18B C 0.5533(4) -0.0057(17) 0.1911(8) 0.082(3) Uani 0.387(11) 1 d D U P A 2
H18C H 0.559478 -0.075411 0.180296 0.098 Uiso 0.387(11) 1 calc R U P A 2
H18D H 0.533090 -0.004530 0.191555 0.098 Uiso 0.387(11) 1 calc R U P A 2
C19B C 0.5642(4) 0.0703(17) 0.1451(7) 0.076(3) Uani 0.387(11) 1 d D U P A 2
H19C H 0.549664 0.118409 0.132165 0.091 Uiso 0.387(11) 1 calc R U P A 2
H19D H 0.571165 0.035345 0.106885 0.091 Uiso 0.387(11) 1 calc R U P A 2
C20B C 0.5871(4) 0.1272(16) 0.1784(7) 0.076(3) Uani 0.387(11) 1 d D U P A 2
H20C H 0.603881 0.127569 0.152217 0.091 Uiso 0.387(11) 1 calc R U P A 2
H20D H 0.581807 0.198483 0.187655 0.091 Uiso 0.387(11) 1 calc R U P A 2
O3 O 0.64929(7) 0.0436(3) 0.21991(16) 0.0535(9) Uani 1 1 d . . . B 1
C21 C 0.67076(14) 0.0875(5) 0.1823(3) 0.0705(17) Uani 1 1 d . . . B 1
H21A H 0.679474 0.145252 0.204710 0.085 Uiso 1 1 calc R U . B 1
H21B H 0.663646 0.111959 0.141104 0.085 Uiso 1 1 calc R U . B 1
C22 C 0.6907(2) 0.0011(7) 0.1730(5) 0.113(3) Uani 1 1 d . . . B 1
H22A H 0.699111 0.005088 0.130536 0.135 Uiso 1 1 calc R U . B 1
H22B H 0.705267 0.004033 0.205344 0.135 Uiso 1 1 calc R U . B 1
C23 C 0.6745(2) -0.0955(7) 0.1796(5) 0.114(3) Uani 1 1 d . . . B 1
H23A H 0.673370 -0.131973 0.138670 0.137 Uiso 1 1 calc R U . B 1
H23B H 0.682877 -0.141231 0.211464 0.137 Uiso 1 1 calc R U . B 1
C24 C 0.6477(2) -0.0619(6) 0.2001(4) 0.111(3) Uani 1 1 d . . . B 1
H24A H 0.634545 -0.068818 0.164818 0.133 Uiso 1 1 calc R U . B 1
H24B H 0.641382 -0.104840 0.235677 0.133 Uiso 1 1 calc R U . B 1
O10 O 0.500000 0.2655(5) 0.750000 0.0769(18) Uani 1 2 d DS T P . .
C37 C 0.4876(2) 0.2106(7) 0.7012(5) 0.113(3) Uani 1 1 d D . . . .
H37A H 0.473303 0.166114 0.719495 0.135 Uiso 1 1 calc R U . . .
H37B H 0.501358 0.166132 0.681000 0.135 Uiso 1 1 calc R U . . .
C38 C 0.4752(2) 0.2757(8) 0.6526(4) 0.112(3) Uani 1 1 d D . . . .
H38A H 0.489516 0.313553 0.630404 0.168 Uiso 1 1 calc R U . . .
H38B H 0.462603 0.323905 0.672687 0.168 Uiso 1 1 calc R U . . .
H38C H 0.465190 0.233232 0.622318 0.168 Uiso 1 1 calc R U . . .
O11 O 0.7294(6) 0.7267(17) 0.4785(10) 0.079(4) Uani 0.291(13) 1 d D U P C -1
C39 C 0.7358(5) 0.674(2) 0.4235(12) 0.094(6) Uani 0.291(13) 1 d D U P C -1
H39A H 0.747675 0.615826 0.434332 0.113 Uiso 0.291(13) 1 calc R U P C -1
H39B H 0.746298 0.720180 0.395298 0.113 Uiso 0.291(13) 1 calc R U P C -1
C40 C 0.7119(7) 0.637(2) 0.3890(14) 0.118(9) Uani 0.291(13) 1 d D U P C -1
H40A H 0.714433 0.648147 0.343567 0.177 Uiso 0.291(13) 1 calc R U P C -1
H40B H 0.695618 0.672866 0.403489 0.177 Uiso 0.291(13) 1 calc R U P C -1
H40C H 0.709756 0.563347 0.396967 0.177 Uiso 0.291(13) 1 calc R U P C -1
C41 C 0.7507(6) 0.770(3) 0.5146(14) 0.075(4) Uani 0.291(13) 1 d D U P C -1
H41A H 0.759150 0.825307 0.489673 0.090 Uiso 0.291(13) 1 calc R U P C -1
H41B H 0.764751 0.717025 0.521824 0.090 Uiso 0.291(13) 1 calc R U P C -1
C42 C 0.7424(6) 0.811(2) 0.5754(12) 0.075(5) Uani 0.291(13) 1 d D U P C -1
H42A H 0.730481 0.869837 0.568791 0.113 Uiso 0.291(13) 1 calc R U P C -1
H42B H 0.758552 0.831672 0.599350 0.113 Uiso 0.291(13) 1 calc R U P C -1
H42C H 0.732488 0.758235 0.599154 0.113 Uiso 0.291(13) 1 calc R U P C -1
O11B O 0.7518(5) 0.829(2) 0.5641(14) 0.076(5) Uani 0.209(13) 1 d D U P C -2
C39B C 0.7731(6) 0.889(2) 0.5896(16) 0.083(6) Uani 0.209(13) 1 d D U P C -2
H39C H 0.766619 0.920652 0.629456 0.099 Uiso 0.209(13) 1 calc R U P C -2
H39D H 0.777120 0.945233 0.559559 0.099 Uiso 0.209(13) 1 calc R U P C -2
C40B C 0.7982(6) 0.835(3) 0.6026(17) 0.099(9) Uani 0.209(13) 1 d D U P C -2
H40D H 0.804306 0.799402 0.564151 0.149 Uiso 0.209(13) 1 calc R U P C -2
H40E H 0.795082 0.784359 0.636199 0.149 Uiso 0.209(13) 1 calc R U P C -2
H40F H 0.812311 0.882892 0.616225 0.149 Uiso 0.209(13) 1 calc R U P C -2
C41B C 0.7573(12) 0.778(5) 0.508(2) 0.076(5) Uani 0.209(13) 1 d D U P C -2
H41C H 0.773913 0.735781 0.514140 0.091 Uiso 0.209(13) 1 calc R U P C -2
H41D H 0.761550 0.828960 0.474887 0.091 Uiso 0.209(13) 1 calc R U P C -2
C42B C 0.7358(13) 0.712(5) 0.484(3) 0.078(6) Uani 0.209(13) 1 d D U P C -2
H42D H 0.722719 0.752446 0.459761 0.118 Uiso 0.209(13) 1 calc R U P C -2
H42E H 0.726451 0.679337 0.519822 0.118 Uiso 0.209(13) 1 calc R U P C -2
H42F H 0.743719 0.659134 0.456814 0.118 Uiso 0.209(13) 1 calc R U P C -2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 2.553(3) . ?
U1 O3 2.578(3) . ?
U1 O2B 2.579(3) . ?
U1 O2 2.579(3) . ?
U1 I2 3.0845(10) . ?
U1 I1 3.1086(11) . ?
U1 Si4 3.1377(15) . ?
U1 Si1 3.1713(14) . ?
I2 K1 3.3535(13) 6_565 ?
K1 O5 2.731(4) . ?
K1 O7 2.760(4) . ?
K1 O9 2.767(4) . ?
K1 O6 2.786(4) . ?
K1 O8 2.797(4) . ?
K1 O4 2.871(4) . ?
Si1 Si2 2.3123(18) . ?
Si1 Si6 2.3348(18) . ?
Si1 Si5 2.348(2) . ?
Si2 O1 1.703(3) . ?
Si2 C2 1.862(6) . ?
Si2 C1 1.877(6) . ?
Si3 O1 1.709(3) . ?
Si3 C3 1.876(6) . ?
Si3 C4 1.877(5) . ?
Si3 Si4 2.3080(19) . ?
Si4 Si8 2.333(2) . ?
Si4 Si7 2.339(2) . ?
Si5 C6 1.875(7) . ?
Si5 C7 1.880(7) . ?
Si5 C5 1.899(6) . ?
Si6 C9 1.873(7) . ?
Si6 C8 1.886(6) . ?
Si6 C10 1.889(6) . ?
Si7 C13 1.869(6) . ?
Si7 C11 1.869(7) . ?
Si7 C12 1.871(7) . ?
Si8 C15 1.859(8) . ?
Si8 C16 1.881(7) . ?
Si8 C14 1.888(6) . ?
O4 C25 1.412(7) . ?
O4 C36 1.417(8) . ?
O5 C26 1.400(7) . ?
O5 C27 1.409(7) . ?
O6 C28 1.424(7) . ?
O6 C29 1.439(8) . ?
O7 C30 1.413(7) . ?
O7 C31 1.427(7) . ?
O8 C32 1.407(8) . ?
O8 C33 1.411(7) . ?
O9 C34 1.409(8) . ?
O9 C35 1.409(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C25 C26 1.496(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.476(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.493(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.485(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.502(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.485(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
O2 C20 1.445(9) . ?
O2 C17 1.460(10) . ?
C17 C18 1.491(16) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.502(13) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.542(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O2B C17B 1.465(14) . ?
O2B C20B 1.469(13) . ?
C17B C18B 1.49(2) . ?
C17B H17C 0.9900 . ?
C17B H17D 0.9900 . ?
C18B C19B 1.490(17) . ?
C18B H18C 0.9900 . ?
C18B H18D 0.9900 . ?
C19B C20B 1.522(16) . ?
C19B H19C 0.9900 . ?
C19B H19D 0.9900 . ?
C20B H20C 0.9900 . ?
C20B H20D 0.9900 . ?
O3 C21 1.441(7) . ?
O3 C24 1.447(8) . ?
C21 C22 1.508(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.500(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.451(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
O10 C37 1.396(9) . ?
O10 C37 1.396(9) 2_656 ?
C37 C38 1.466(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O11 C39 1.386(17) . ?
O11 C41 1.409(18) . ?
C39 C40 1.465(19) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.450(18) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O11B C41B 1.392(19) . ?
O11B C39B 1.417(18) . ?
C39B C40B 1.453(19) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C41B C42B 1.45(2) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 O3 144.61(10) . . ?
O1 U1 O2B 147.15(11) . . ?
O1 U1 O2 147.15(11) . . ?
O3 U1 O2 68.06(12) . . ?
O1 U1 I2 94.13(7) . . ?
O3 U1 I2 85.41(9) . . ?
O2B U1 I2 83.53(10) . . ?
O2 U1 I2 83.53(10) . . ?
O1 U1 I1 99.34(7) . . ?
O3 U1 I1 85.78(9) . . ?
O2B U1 I1 83.11(10) . . ?
O2 U1 I1 83.11(10) . . ?
I2 U1 I1 166.017(13) . . ?
O1 U1 Si4 64.83(7) . . ?
O3 U1 Si4 79.78(9) . . ?
O2B U1 Si4 147.54(9) . . ?
O2 U1 Si4 147.54(9) . . ?
I2 U1 Si4 89.83(3) . . ?
I1 U1 Si4 99.25(3) . . ?
O1 U1 Si1 64.82(7) . . ?
O3 U1 Si1 150.52(8) . . ?
O2B U1 Si1 82.46(10) . . ?
O2 U1 Si1 82.46(10) . . ?
I2 U1 Si1 91.46(3) . . ?
I1 U1 Si1 90.88(3) . . ?
Si4 U1 Si1 129.59(4) . . ?
U1 I2 K1 158.24(2) . 6_565 ?
O5 K1 O7 120.95(13) . . ?
O5 K1 O9 119.42(13) . . ?
O7 K1 O9 119.22(13) . . ?
O5 K1 O6 60.65(12) . . ?
O7 K1 O6 61.26(13) . . ?
O9 K1 O6 176.57(13) . . ?
O5 K1 O8 174.24(13) . . ?
O7 K1 O8 60.50(13) . . ?
O9 K1 O8 60.19(13) . . ?
O6 K1 O8 119.35(13) . . ?
O5 K1 O4 59.25(12) . . ?
O7 K1 O4 179.29(14) . . ?
O9 K1 O4 60.50(13) . . ?
O6 K1 O4 119.06(13) . . ?
O8 K1 O4 119.38(13) . . ?
O5 K1 I2 78.02(8) . 6_566 ?
O7 K1 I2 93.33(11) . 6_566 ?
O9 K1 I2 92.37(10) . 6_566 ?
O6 K1 I2 90.98(9) . 6_566 ?
O8 K1 I2 107.65(9) . 6_566 ?
O4 K1 I2 86.05(9) . 6_566 ?
Si2 Si1 Si6 103.78(7) . . ?
Si2 Si1 Si5 105.45(8) . . ?
Si6 Si1 Si5 103.56(8) . . ?
Si2 Si1 U1 78.92(5) . . ?
Si6 Si1 U1 132.20(7) . . ?
Si5 Si1 U1 121.98(6) . . ?
O1 Si2 C2 108.6(2) . . ?
O1 Si2 C1 104.8(2) . . ?
C2 Si2 C1 105.5(3) . . ?
O1 Si2 Si1 100.51(11) . . ?
C2 Si2 Si1 120.64(19) . . ?
C1 Si2 Si1 115.45(19) . . ?
O1 Si3 C3 105.8(2) . . ?
O1 Si3 C4 108.0(2) . . ?
C3 Si3 C4 106.6(3) . . ?
O1 Si3 Si4 99.50(12) . . ?
C3 Si3 Si4 115.5(2) . . ?
C4 Si3 Si4 120.0(2) . . ?
Si3 Si4 Si8 103.89(7) . . ?
Si3 Si4 Si7 104.61(8) . . ?
Si8 Si4 Si7 105.32(8) . . ?
Si3 Si4 U1 79.88(5) . . ?
Si8 Si4 U1 116.90(7) . . ?
Si7 Si4 U1 135.26(6) . . ?
C6 Si5 C7 106.4(4) . . ?
C6 Si5 C5 106.0(3) . . ?
C7 Si5 C5 106.1(3) . . ?
C6 Si5 Si1 113.8(2) . . ?
C7 Si5 Si1 109.3(3) . . ?
C5 Si5 Si1 114.7(2) . . ?
C9 Si6 C8 105.7(3) . . ?
C9 Si6 C10 106.6(3) . . ?
C8 Si6 C10 106.7(3) . . ?
C9 Si6 Si1 112.33(19) . . ?
C8 Si6 Si1 115.7(2) . . ?
C10 Si6 Si1 109.2(2) . . ?
C13 Si7 C11 106.4(4) . . ?
C13 Si7 C12 107.0(3) . . ?
C11 Si7 C12 105.5(4) . . ?
C13 Si7 Si4 111.5(2) . . ?
C11 Si7 Si4 115.1(2) . . ?
C12 Si7 Si4 110.8(3) . . ?
C15 Si8 C16 106.9(4) . . ?
C15 Si8 C14 106.6(4) . . ?
C16 Si8 C14 106.9(3) . . ?
C15 Si8 Si4 108.0(2) . . ?
C16 Si8 Si4 114.7(3) . . ?
C14 Si8 Si4 113.32(19) . . ?
Si2 O1 Si3 137.14(18) . . ?
Si2 O1 U1 111.36(14) . . ?
Si3 O1 U1 111.43(14) . . ?
C25 O4 C36 111.6(5) . . ?
C25 O4 K1 110.5(3) . . ?
C36 O4 K1 108.6(4) . . ?
C26 O5 C27 114.3(4) . . ?
C26 O5 K1 121.1(3) . . ?
C27 O5 K1 118.3(3) . . ?
C28 O6 C29 111.7(5) . . ?
C28 O6 K1 111.8(3) . . ?
C29 O6 K1 112.5(4) . . ?
C30 O7 C31 112.8(5) . . ?
C30 O7 K1 115.6(4) . . ?
C31 O7 K1 116.7(4) . . ?
C32 O8 C33 111.1(5) . . ?
C32 O8 K1 113.7(4) . . ?
C33 O8 K1 115.2(4) . . ?
C34 O9 C35 113.7(5) . . ?
C34 O9 K1 115.6(4) . . ?
C35 O9 K1 116.6(4) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si3 C3 H3A 109.5 . . ?
Si3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si5 C5 H5A 109.5 . . ?
Si5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si5 C6 H6A 109.5 . . ?
Si5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si5 C7 H7A 109.5 . . ?
Si5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si6 C8 H8A 109.5 . . ?
Si6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si6 C9 H9A 109.5 . . ?
Si6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si6 C10 H10A 109.5 . . ?
Si6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si7 C11 H11A 109.5 . . ?
Si7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si7 C12 H12A 109.5 . . ?
Si7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si7 C13 H13A 109.5 . . ?
Si7 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si7 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si8 C14 H14A 109.5 . . ?
Si8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si8 C15 H15A 109.5 . . ?
Si8 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si8 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si8 C16 H16A 109.5 . . ?
Si8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C25 C26 109.0(5) . . ?
O4 C25 H25A 109.9 . . ?
C26 C25 H25A 109.9 . . ?
O4 C25 H25B 109.9 . . ?
C26 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
O5 C26 C25 108.8(5) . . ?
O5 C26 H26A 109.9 . . ?
C25 C26 H26A 109.9 . . ?
O5 C26 H26B 109.9 . . ?
C25 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
O5 C27 C28 108.3(5) . . ?
O5 C27 H27A 110.0 . . ?
C28 C27 H27A 110.0 . . ?
O5 C27 H27B 110.0 . . ?
C28 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
O6 C28 C27 110.4(6) . . ?
O6 C28 H28A 109.6 . . ?
C27 C28 H28A 109.6 . . ?
O6 C28 H28B 109.6 . . ?
C27 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
O6 C29 C30 108.5(6) . . ?
O6 C29 H29A 110.0 . . ?
C30 C29 H29A 110.0 . . ?
O6 C29 H29B 110.0 . . ?
C30 C29 H29B 110.0 . . ?
H29A C29 H29B 108.4 . . ?
O7 C30 C29 109.6(5) . . ?
O7 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 . . ?
O7 C30 H30B 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
O7 C31 C32 109.5(6) . . ?
O7 C31 H31A 109.8 . . ?
C32 C31 H31A 109.8 . . ?
O7 C31 H31B 109.8 . . ?
C32 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
O8 C32 C31 109.6(6) . . ?
O8 C32 H32A 109.7 . . ?
C31 C32 H32A 109.7 . . ?
O8 C32 H32B 109.7 . . ?
C31 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
O8 C33 C34 109.0(5) . . ?
O8 C33 H33A 109.9 . . ?
C34 C33 H33A 109.9 . . ?
O8 C33 H33B 109.9 . . ?
C34 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
O9 C34 C33 108.4(6) . . ?
O9 C34 H34A 110.0 . . ?
C33 C34 H34A 110.0 . . ?
O9 C34 H34B 110.0 . . ?
C33 C34 H34B 110.0 . . ?
H34A C34 H34B 108.4 . . ?
O9 C35 C36 109.3(6) . . ?
O9 C35 H35A 109.8 . . ?
C36 C35 H35A 109.8 . . ?
O9 C35 H35B 109.8 . . ?
C36 C35 H35B 109.8 . . ?
H35A C35 H35B 108.3 . . ?
O4 C36 C35 108.8(6) . . ?
O4 C36 H36A 109.9 . . ?
C35 C36 H36A 109.9 . . ?
O4 C36 H36B 109.9 . . ?
C35 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
C20 O2 C17 106.4(7) . . ?
C20 O2 U1 130.1(5) . . ?
C17 O2 U1 123.4(5) . . ?
O2 C17 C18 102.3(9) . . ?
O2 C17 H17A 111.3 . . ?
C18 C17 H17A 111.3 . . ?
O2 C17 H17B 111.3 . . ?
C18 C17 H17B 111.3 . . ?
H17A C17 H17B 109.2 . . ?
C17 C18 C19 104.5(8) . . ?
C17 C18 H18A 110.8 . . ?
C19 C18 H18A 110.8 . . ?
C17 C18 H18B 110.8 . . ?
C19 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
C18 C19 C20 106.8(9) . . ?
C18 C19 H19A 110.4 . . ?
C20 C19 H19A 110.4 . . ?
C18 C19 H19B 110.4 . . ?
C20 C19 H19B 110.4 . . ?
H19A C19 H19B 108.6 . . ?
O2 C20 C19 97.7(8) . . ?
O2 C20 H20A 112.2 . . ?
C19 C20 H20A 112.2 . . ?
O2 C20 H20B 112.2 . . ?
C19 C20 H20B 112.2 . . ?
H20A C20 H20B 109.8 . . ?
C17B O2B C20B 105.6(11) . . ?
C17B O2B U1 124.3(8) . . ?
C20B O2B U1 120.9(6) . . ?
O2B C17B C18B 103.4(13) . . ?
O2B C17B H17C 111.1 . . ?
C18B C17B H17C 111.1 . . ?
O2B C17B H17D 111.1 . . ?
C18B C17B H17D 111.1 . . ?
H17C C17B H17D 109.1 . . ?
C19B C18B C17B 104.4(12) . . ?
C19B C18B H18C 110.9 . . ?
C17B C18B H18C 110.9 . . ?
C19B C18B H18D 110.9 . . ?
C17B C18B H18D 110.9 . . ?
H18C C18B H18D 108.9 . . ?
C18B C19B C20B 107.1(11) . . ?
C18B C19B H19C 110.3 . . ?
C20B C19B H19C 110.3 . . ?
C18B C19B H19D 110.3 . . ?
C20B C19B H19D 110.3 . . ?
H19C C19B H19D 108.6 . . ?
O2B C20B C19B 103.8(11) . . ?
O2B C20B H20C 111.0 . . ?
C19B C20B H20C 111.0 . . ?
O2B C20B H20D 111.0 . . ?
C19B C20B H20D 111.0 . . ?
H20C C20B H20D 109.0 . . ?
C21 O3 C24 105.1(5) . . ?
C21 O3 U1 125.9(3) . . ?
C24 O3 U1 127.5(4) . . ?
O3 C21 C22 104.2(6) . . ?
O3 C21 H21A 110.9 . . ?
C22 C21 H21A 110.9 . . ?
O3 C21 H21B 110.9 . . ?
C22 C21 H21B 110.9 . . ?
H21A C21 H21B 108.9 . . ?
C23 C22 C21 106.2(7) . . ?
C23 C22 H22A 110.5 . . ?
C21 C22 H22A 110.5 . . ?
C23 C22 H22B 110.5 . . ?
C21 C22 H22B 110.5 . . ?
H22A C22 H22B 108.7 . . ?
C24 C23 C22 104.5(7) . . ?
C24 C23 H23A 110.9 . . ?
C22 C23 H23A 110.9 . . ?
C24 C23 H23B 110.9 . . ?
C22 C23 H23B 110.9 . . ?
H23A C23 H23B 108.9 . . ?
O3 C24 C23 109.2(7) . . ?
O3 C24 H24A 109.8 . . ?
C23 C24 H24A 109.8 . . ?
O3 C24 H24B 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.3 . . ?
C37 O10 C37 118.0(10) . 2_656 ?
O10 C37 C38 113.4(7) . . ?
O10 C37 H37A 108.9 . . ?
C38 C37 H37A 108.9 . . ?
O10 C37 H37B 108.9 . . ?
C38 C37 H37B 108.9 . . ?
H37A C37 H37B 107.7 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 O11 C41 119.0(18) . . ?
O11 C39 C40 113.8(17) . . ?
O11 C39 H39A 108.8 . . ?
C40 C39 H39A 108.8 . . ?
O11 C39 H39B 108.8 . . ?
C40 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O11 C41 C42 114.8(16) . . ?
O11 C41 H41A 108.6 . . ?
C42 C41 H41A 108.6 . . ?
O11 C41 H41B 108.6 . . ?
C42 C41 H41B 108.6 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41B O11B C39B 116.7(19) . . ?
O11B C39B C40B 115.0(17) . . ?
O11B C39B H39C 108.5 . . ?
C40B C39B H39C 108.5 . . ?
O11B C39B H39D 108.5 . . ?
C40B C39B H39D 108.5 . . ?
H39C C39B H39D 107.5 . . ?
C39B C40B H40D 109.5 . . ?
C39B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C39B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
O11B C41B C42B 116.0(17) . . ?
O11B C41B H41C 108.3 . . ?
C42B C41B H41C 108.3 . . ?
O11B C41B H41D 108.3 . . ?
C42B C41B H41D 108.3 . . ?
H41C C41B H41D 107.4 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Si2 O1 Si3 28.1(4) . . . . ?
C1 Si2 O1 Si3 -84.3(3) . . . . ?
Si1 Si2 O1 Si3 155.7(3) . . . . ?
C2 Si2 O1 U1 -148.5(2) . . . . ?
C1 Si2 O1 U1 99.1(2) . . . . ?
Si1 Si2 O1 U1 -20.94(15) . . . . ?
C3 Si3 O1 Si2 -77.2(4) . . . . ?
C4 Si3 O1 Si2 36.7(4) . . . . ?
Si4 Si3 O1 Si2 162.7(3) . . . . ?
C3 Si3 O1 U1 99.4(3) . . . . ?
C4 Si3 O1 U1 -146.7(2) . . . . ?
Si4 Si3 O1 U1 -20.71(15) . . . . ?
C36 O4 C25 C26 -176.6(5) . . . . ?
K1 O4 C25 C26 -55.7(5) . . . . ?
C27 O5 C26 C25 170.7(5) . . . . ?
K1 O5 C26 C25 -37.4(5) . . . . ?
O4 C25 C26 O5 62.2(6) . . . . ?
C26 O5 C27 C28 -165.7(5) . . . . ?
K1 O5 C27 C28 41.6(6) . . . . ?
C29 O6 C28 C27 179.7(5) . . . . ?
K1 O6 C28 C27 52.6(6) . . . . ?
O5 C27 C28 O6 -62.7(7) . . . . ?
C28 O6 C29 C30 -178.5(6) . . . . ?
K1 O6 C29 C30 -51.7(6) . . . . ?
C31 O7 C30 C29 176.8(6) . . . . ?
K1 O7 C30 C29 -45.4(8) . . . . ?
O6 C29 C30 O7 65.2(8) . . . . ?
C30 O7 C31 C32 -179.9(7) . . . . ?
K1 O7 C31 C32 42.7(8) . . . . ?
C33 O8 C32 C31 -176.9(6) . . . . ?
K1 O8 C32 C31 51.1(7) . . . . ?
O7 C31 C32 O8 -62.5(8) . . . . ?
C32 O8 C33 C34 -177.4(6) . . . . ?
K1 O8 C33 C34 -46.2(7) . . . . ?
C35 O9 C34 C33 171.1(6) . . . . ?
K1 O9 C34 C33 -50.1(7) . . . . ?
O8 C33 C34 O9 63.8(8) . . . . ?
C34 O9 C35 C36 -178.9(6) . . . . ?
K1 O9 C35 C36 42.7(7) . . . . ?
C25 O4 C36 C35 179.1(5) . . . . ?
K1 O4 C36 C35 57.2(6) . . . . ?
O9 C35 C36 O4 -68.8(8) . . . . ?
C20 O2 C17 C18 -45.2(17) . . . . ?
U1 O2 C17 C18 137.0(9) . . . . ?
O2 C17 C18 C19 22.5(17) . . . . ?
C17 C18 C19 C20 5.0(16) . . . . ?
C17 O2 C20 C19 46.3(15) . . . . ?
U1 O2 C20 C19 -136.1(8) . . . . ?
C18 C19 C20 O2 -30.5(14) . . . . ?
C20B O2B C17B C18B 41(3) . . . . ?
U1 O2B C17B C18B -172.4(13) . . . . ?
O2B C17B C18B C19B -34(3) . . . . ?
C17B C18B C19B C20B 15(3) . . . . ?
C17B O2B C20B C19B -31(3) . . . . ?
U1 O2B C20B C19B -179.2(13) . . . . ?
C18B C19B C20B O2B 10(2) . . . . ?
C24 O3 C21 C22 -33.0(8) . . . . ?
U1 O3 C21 C22 133.5(6) . . . . ?
O3 C21 C22 C23 25.0(9) . . . . ?
C21 C22 C23 C24 -7.2(11) . . . . ?
C21 O3 C24 C23 29.8(10) . . . . ?
U1 O3 C24 C23 -136.4(6) . . . . ?
C22 C23 C24 O3 -13.5(11) . . . . ?
C37 O10 C37 C38 180.0(10) 2_656 . . . ?
C41 O11 C39 C40 -178(3) . . . . ?
C39 O11 C41 C42 -172(3) . . . . ?
C41B O11B C39B C40B -58(5) . . . . ?
C39B O11B C41B C42B 177(4) . . . . ?

_refine_diff_density_max         1.543
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.122





