#------------------------------------------------------------------------------
#$Date: 2020-01-29 01:45:45 +0200 (Wed, 29 Jan 2020) $
#$Revision: 247299 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/40/4134065.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4134065
loop_
_publ_author_name
'Palumbo, Chad T.'
'Scopelliti, Rosario'
'Zivkovic, Ivica'
'Mazzanti, Marinella'
_publ_section_title
;
 C-H Bond Activation by an Isolated Dinuclear U(III)/U(IV) Nitride.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12804
_journal_year                    2020
_chemical_formula_sum            'C72 H171 N10 O2 Si16 U4'
_chemical_formula_weight         2610.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                92.605(2)
_cell_angle_beta                 92.492(3)
_cell_angle_gamma                109.741(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3775(4)
_cell_length_b                   15.2039(4)
_cell_length_c                   32.5115(10)
_cell_measurement_reflns_used    7282
_cell_measurement_temperature    140.2(6)
_cell_measurement_theta_max      72.4320
_cell_measurement_theta_min      3.0680
_cell_volume                     5741.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Mercury 4.2.0 (CCDC, 2019)'
_computing_publication_material  'CIFTab (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.2(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω   -113.00 -39.00   1.00    7.50    --  -40.91 -38.00-150.00   74
  2  ω    -64.00  29.00   1.00    7.50    --  -40.91  77.00 -60.00   93
  3  ω    -73.00  -6.00   1.00    7.50    --  -40.91 125.00 120.00   67
  4  ω    -48.00  27.00   1.00    7.50    --  -40.91  38.00  30.00   75
  5  ω    -87.00 -49.00   1.00    7.50    --  -40.91 125.00  30.00   38
  6  ω    -19.00  37.00   1.00    7.50    --   40.91 -77.00  90.00   56
  7  ω     53.00  80.00   1.00   30.00    --  105.15-111.00   0.00   27
  8  ω     29.00 131.00   1.00   30.00    --  105.15 -30.00 -30.00  102
  9  ω     76.00 109.00   1.00   30.00    --  105.15-111.00 -60.00   33
 10  ω     76.00 173.00   1.00   30.00    --  105.15  61.00 -30.00   97
 11  ω     48.00  91.00   1.00   30.00    --  105.15 -94.00  60.00   43
 12  ω     29.00 108.00   1.00   30.00    --  105.15-111.00 150.00   79
 13  ω    111.00 140.00   1.00   30.00    --  105.15 111.00 -90.00   29
 14  ω     54.00  79.00   1.00   30.00    --  105.15 -45.00  30.00   25
 15  ω    111.00 139.00   1.00   30.00    --  105.15  77.00 150.00   28
 16  ω     31.00 154.00   1.00   30.00    --  105.15 -15.00 150.00  123
 17  ω     36.00 129.00   1.00   30.00    --  105.15 -61.00-180.00   93
 18  ω     29.00 109.00   1.00   30.00    --  105.15-111.00  30.00   80
 19  ω     27.00 105.00   1.00   30.00    --  105.15 -94.00-180.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.1268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            43244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.858
_diffrn_reflns_theta_min         3.094
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.572
_exptl_absorpt_correction_T_max  0.417
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale orange'
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       plate
_exptl_crystal_F_000             2562
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.109
_refine_diff_density_max         3.235
_refine_diff_density_min         -2.268
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     988
_refine_ls_number_reflns         22238
_refine_ls_number_restraints     1137
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0493P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14040
_reflns_number_total             22238
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12804_si_007.cif
_cod_data_source_block           ctp613
_cod_original_cell_volume        5741.5(3)
_cod_database_code               4134065
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.105
_shelx_estimated_absorpt_t_max   0.250
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
U1 U 0.51034(4) 0.31300(3) 0.24022(2) 0.05595(14) Uani 1 1 d . . .
U2 U 0.35529(4) 0.46993(3) 0.26551(2) 0.04804(13) Uani 1 1 d . . .
Si1 Si 0.6135(4) 0.2931(3) 0.34319(15) 0.0614(11) Uani 1 1 d . . .
Si2 Si 0.6048(4) 0.1448(3) 0.2790(2) 0.0788(16) Uani 1 1 d . . .
Si3 Si 0.7638(5) 0.4140(4) 0.19402(18) 0.0805(14) Uani 1 1 d . . .
Si4 Si 0.5759(7) 0.2949(6) 0.1347(2) 0.111(3) Uani 1 1 d . . .
Si5 Si 0.3128(4) 0.4969(3) 0.37155(13) 0.0600(11) Uani 1 1 d . . .
Si6 Si 0.1267(4) 0.3493(3) 0.31748(15) 0.0582(10) Uani 1 1 d . . .
Si7 Si 0.5742(4) 0.6900(3) 0.25473(14) 0.0571(10) Uani 1 1 d . . .
Si8 Si 0.3270(4) 0.6770(3) 0.24982(16) 0.0629(11) Uani 1 1 d . . .
N1 N 0.5969(11) 0.2545(7) 0.2913(4) 0.059(3) Uani 1 1 d . . .
N2 N 0.6237(13) 0.3416(10) 0.1845(5) 0.071(3) Uani 1 1 d . . .
N3 N 0.5019(11) 0.4272(7) 0.2797(4) 0.060(3) Uani 1 1 d . . .
H3 H 0.553677 0.454365 0.299913 0.073 Uiso 1 1 calc R U .
N4 N 0.2585(11) 0.4362(7) 0.3252(4) 0.051(3) Uani 1 1 d . . .
N5 N 0.4316(11) 0.6284(7) 0.2627(4) 0.054(3) Uani 1 1 d . . .
C1 C 0.3254(15) 0.1842(11) 0.2424(7) 0.075(4) Uani 1 1 d . U .
C2 C 0.2449(16) 0.1114(12) 0.2440(7) 0.081(5) Uani 1 1 d . U .
C3 C 0.1512(17) 0.0304(12) 0.2468(7) 0.079(4) Uani 1 1 d . U .
C4 C 0.1582(18) -0.0602(12) 0.2399(7) 0.086(5) Uani 1 1 d . U .
H4 H 0.230598 -0.064586 0.233743 0.103 Uiso 1 1 calc R U .
C5 C 0.070(2) -0.1392(16) 0.2416(8) 0.106(5) Uani 1 1 d . U .
H5 H 0.078128 -0.198191 0.235087 0.127 Uiso 1 1 calc R U .
C6 C -0.036(2) -0.1327(16) 0.2536(8) 0.107(6) Uani 1 1 d . U .
H6 H -0.099102 -0.188010 0.257226 0.128 Uiso 1 1 calc R U .
C7 C -0.047(2) -0.0484(16) 0.2598(8) 0.105(5) Uani 1 1 d . U .
H7 H -0.119486 -0.044196 0.266605 0.126 Uiso 1 1 calc R U .
C8 C 0.0441(18) 0.0311(14) 0.2563(7) 0.088(5) Uani 1 1 d . U .
H8 H 0.033633 0.089779 0.260741 0.106 Uiso 1 1 calc R U .
C9 C 0.3734(15) 0.3861(11) 0.2007(5) 0.064(3) Uani 1 1 d . U .
C10 C 0.3098(16) 0.4399(11) 0.1952(6) 0.067(3) Uani 1 1 d . U .
C11 C 0.2676(16) 0.4586(12) 0.1544(6) 0.070(3) Uani 1 1 d . U .
C12 C 0.336(2) 0.5013(15) 0.1229(7) 0.089(4) Uani 1 1 d . U .
H12 H 0.416319 0.512356 0.126481 0.107 Uiso 1 1 calc R U .
C13 C 0.297(2) 0.5282(18) 0.0878(7) 0.102(5) Uani 1 1 d . U .
H13 H 0.351025 0.561976 0.069243 0.123 Uiso 1 1 calc R U .
C14 C 0.183(2) 0.5081(18) 0.0783(8) 0.107(5) Uani 1 1 d . U .
H14 H 0.154569 0.521900 0.052641 0.128 Uiso 1 1 calc R U .
C15 C 0.110(2) 0.4660(18) 0.1087(7) 0.103(5) Uani 1 1 d . U .
H15 H 0.029449 0.451842 0.104351 0.123 Uiso 1 1 calc R U .
C16 C 0.1534(19) 0.4456(16) 0.1439(7) 0.093(5) Uani 1 1 d . U .
H16 H 0.099960 0.419263 0.163872 0.111 Uiso 1 1 calc R U .
C17 C 0.4714(16) 0.2759(13) 0.3638(7) 0.083(5) Uani 1 1 d . . .
H17A H 0.423377 0.209762 0.359615 0.124 Uiso 1 1 calc R U .
H17B H 0.434135 0.314229 0.349347 0.124 Uiso 1 1 calc R U .
H17C H 0.481423 0.294653 0.393346 0.124 Uiso 1 1 calc R U .
C18 C 0.7062(14) 0.4203(10) 0.3533(5) 0.061(4) Uani 1 1 d . . .
H18A H 0.685113 0.457742 0.332764 0.091 Uiso 1 1 calc R U .
H18B H 0.787305 0.426594 0.351551 0.091 Uiso 1 1 calc R U .
H18C H 0.694310 0.442430 0.380991 0.091 Uiso 1 1 calc R U .
C19 C 0.6853(18) 0.2344(13) 0.3792(7) 0.092(6) Uani 1 1 d . . .
H19A H 0.763622 0.244106 0.371083 0.138 Uiso 1 1 calc R U .
H19B H 0.641551 0.167188 0.378007 0.138 Uiso 1 1 calc R U .
H19C H 0.688376 0.261213 0.407407 0.138 Uiso 1 1 calc R U .
C20 C 0.4974(18) 0.0502(10) 0.3055(8) 0.095(6) Uani 1 1 d . U .
H20A H 0.419513 0.045162 0.295512 0.142 Uiso 1 1 calc R U .
H20B H 0.507059 0.065450 0.335330 0.142 Uiso 1 1 calc R U .
H20C H 0.509277 -0.009457 0.299458 0.142 Uiso 1 1 calc R U .
C21 C 0.7535(17) 0.1360(13) 0.2892(8) 0.100(7) Uani 1 1 d . . .
H21A H 0.768981 0.134419 0.318916 0.150 Uiso 1 1 calc R U .
H21B H 0.811673 0.190373 0.278800 0.150 Uiso 1 1 calc R U .
H21C H 0.756458 0.078558 0.275049 0.150 Uiso 1 1 calc R U .
C22 C 0.5710(17) 0.1158(11) 0.2216(7) 0.093(5) Uani 1 1 d . . .
H22A H 0.617085 0.168538 0.206484 0.140 Uiso 1 1 calc R U .
H22B H 0.489085 0.104140 0.215032 0.140 Uiso 1 1 calc R U .
H22C H 0.589250 0.059794 0.213524 0.140 Uiso 1 1 calc R U .
C23 C 0.7791(19) 0.4749(15) 0.2457(7) 0.099(6) Uani 1 1 d . . .
H23A H 0.767580 0.429310 0.266833 0.148 Uiso 1 1 calc R U .
H23B H 0.721500 0.505851 0.247437 0.148 Uiso 1 1 calc R U .
H23C H 0.856274 0.521831 0.250033 0.148 Uiso 1 1 calc R U .
C24 C 0.866(2) 0.3471(18) 0.1964(10) 0.129(10) Uani 1 1 d . . .
H24A H 0.872748 0.322432 0.168596 0.193 Uiso 1 1 calc R U .
H24B H 0.837387 0.295105 0.214292 0.193 Uiso 1 1 calc R U .
H24C H 0.941921 0.388848 0.207538 0.193 Uiso 1 1 calc R U .
C25 C 0.820(2) 0.5083(18) 0.1561(8) 0.116(8) Uani 1 1 d . . .
H25A H 0.778398 0.552410 0.157868 0.174 Uiso 1 1 calc R U .
H25B H 0.809676 0.479106 0.127995 0.174 Uiso 1 1 calc R U .
H25C H 0.902541 0.541814 0.162829 0.174 Uiso 1 1 calc R U .
C26 C 0.440(2) 0.195(2) 0.1361(8) 0.143(10) Uani 1 1 d . . .
H26A H 0.386745 0.213441 0.152789 0.215 Uiso 1 1 calc R U .
H26B H 0.456529 0.142403 0.148264 0.215 Uiso 1 1 calc R U .
H26C H 0.406123 0.175536 0.107962 0.215 Uiso 1 1 calc R U .
C27 C 0.678(3) 0.244(2) 0.1079(8) 0.146(11) Uani 1 1 d . . .
H27A H 0.695926 0.199458 0.125506 0.218 Uiso 1 1 calc R U .
H27B H 0.749243 0.294794 0.103057 0.218 Uiso 1 1 calc R U .
H27C H 0.641466 0.211884 0.081529 0.218 Uiso 1 1 calc R U .
C28 C 0.548(3) 0.381(2) 0.0998(9) 0.153(10) Uani 1 1 d . U .
H28A H 0.620520 0.432186 0.096822 0.230 Uiso 1 1 calc R U .
H28B H 0.492507 0.405851 0.111714 0.230 Uiso 1 1 calc R U .
H28C H 0.517742 0.349312 0.072712 0.230 Uiso 1 1 calc R U .
C29 C 0.2598(19) 0.5977(14) 0.3805(7) 0.099(6) Uani 1 1 d . U .
H29A H 0.175548 0.574308 0.379714 0.148 Uiso 1 1 calc R U .
H29B H 0.285464 0.641693 0.358878 0.148 Uiso 1 1 calc R U .
H29C H 0.290589 0.629662 0.407494 0.148 Uiso 1 1 calc R U .
C30 C 0.275(2) 0.4246(15) 0.4170(7) 0.110(7) Uani 1 1 d . U .
H30A H 0.309627 0.375108 0.415299 0.165 Uiso 1 1 calc R U .
H30B H 0.191654 0.396187 0.417216 0.165 Uiso 1 1 calc R U .
H30C H 0.305370 0.464317 0.442375 0.165 Uiso 1 1 calc R U .
C31 C 0.4685(15) 0.5421(11) 0.3734(5) 0.068(4) Uani 1 1 d . . .
H31A H 0.493749 0.586152 0.351764 0.102 Uiso 1 1 calc R U .
H31B H 0.497597 0.490169 0.368906 0.102 Uiso 1 1 calc R U .
H31C H 0.498260 0.574377 0.400408 0.102 Uiso 1 1 calc R U .
C32 C 0.0038(16) 0.3856(12) 0.3332(8) 0.091(6) Uani 1 1 d . . .
H32A H -0.002032 0.435494 0.316171 0.136 Uiso 1 1 calc R U .
H32B H 0.016731 0.408523 0.362299 0.136 Uiso 1 1 calc R U .
H32C H -0.067681 0.331745 0.329442 0.136 Uiso 1 1 calc R U .
C33 C 0.1182(16) 0.2413(10) 0.3442(6) 0.074(5) Uani 1 1 d . . .
H33A H 0.127201 0.255529 0.374093 0.110 Uiso 1 1 calc R U .
H33B H 0.179554 0.218708 0.335482 0.110 Uiso 1 1 calc R U .
H33C H 0.043321 0.192793 0.336980 0.110 Uiso 1 1 calc R U .
C34 C 0.1058(15) 0.3127(11) 0.2597(5) 0.073(5) Uani 1 1 d . . .
H34A H 0.158120 0.279051 0.252663 0.109 Uiso 1 1 calc R U .
H34B H 0.122459 0.368606 0.243861 0.109 Uiso 1 1 calc R U .
H34C H 0.026157 0.271838 0.253058 0.109 Uiso 1 1 calc R U .
C35 C 0.6113(17) 0.8205(11) 0.2541(7) 0.083(5) Uani 1 1 d . . .
H35A H 0.615522 0.847214 0.282403 0.124 Uiso 1 1 calc R U .
H35B H 0.551931 0.834490 0.237486 0.124 Uiso 1 1 calc R U .
H35C H 0.685830 0.847684 0.242203 0.124 Uiso 1 1 calc R U .
C36 C 0.6732(13) 0.6752(10) 0.2964(5) 0.059(4) Uani 1 1 d . . .
H36A H 0.656947 0.608338 0.299808 0.088 Uiso 1 1 calc R U .
H36B H 0.661950 0.705589 0.322309 0.088 Uiso 1 1 calc R U .
H36C H 0.752952 0.703896 0.289057 0.088 Uiso 1 1 calc R U .
C37 C 0.6132(17) 0.6477(12) 0.2045(6) 0.079(5) Uani 1 1 d . . .
H37A H 0.580263 0.672519 0.181717 0.119 Uiso 1 1 calc R U .
H37B H 0.582738 0.579081 0.201879 0.119 Uiso 1 1 calc R U .
H37C H 0.697115 0.669213 0.203544 0.119 Uiso 1 1 calc R U .
C38 C 0.3289(18) 0.7756(11) 0.2878(7) 0.085(6) Uani 1 1 d . . .
H38A H 0.405922 0.823189 0.290182 0.128 Uiso 1 1 calc R U .
H38B H 0.308993 0.750929 0.314818 0.128 Uiso 1 1 calc R U .
H38C H 0.272843 0.803796 0.278024 0.128 Uiso 1 1 calc R U .
C39 C 0.1819(14) 0.5838(10) 0.2530(6) 0.070(5) Uani 1 1 d . . .
H39A H 0.184009 0.546626 0.276703 0.105 Uiso 1 1 calc R U .
H39B H 0.162726 0.542955 0.227652 0.105 Uiso 1 1 calc R U .
H39C H 0.123483 0.613476 0.256430 0.105 Uiso 1 1 calc R U .
C40 C 0.3347(19) 0.7191(14) 0.1954(6) 0.093(6) Uani 1 1 d . . .
H40A H 0.329520 0.667100 0.175552 0.139 Uiso 1 1 calc R U .
H40B H 0.407848 0.769980 0.193189 0.139 Uiso 1 1 calc R U .
H40C H 0.270834 0.741821 0.189424 0.139 Uiso 1 1 calc R U .
U3 U 0.08135(4) 0.11101(3) 0.54123(2) 0.04261(12) Uani 1 1 d . . .
Si9 Si -0.0716(4) 0.2440(2) 0.49108(14) 0.0527(9) Uani 1 1 d . . .
Si10 Si 0.1100(3) 0.3369(2) 0.55885(13) 0.0498(9) Uani 1 1 d . . .
Si11 Si 0.3432(4) 0.1789(3) 0.49854(13) 0.0545(10) Uani 1 1 d . . .
Si12 Si 0.3371(4) 0.1003(2) 0.58344(13) 0.0529(9) Uani 1 1 d . . .
O1 O -0.0464(10) 0.0703(7) 0.5987(3) 0.062(3) Uani 1 1 d . . .
N6 N 0.0340(10) 0.2388(7) 0.5274(3) 0.046(2) Uani 1 1 d . . .
N7 N 0.2733(10) 0.1342(7) 0.5417(4) 0.047(2) Uani 1 1 d . . .
N8 N 0.000000 0.000000 0.500000 0.057(5) Uani 1 2 d S . P
C41 C -0.0818(17) 0.1645(11) 0.4446(5) 0.073(5) Uani 1 1 d . . .
H41A H -0.004554 0.173998 0.435444 0.110 Uiso 1 1 calc R U .
H41B H -0.128750 0.178455 0.422518 0.110 Uiso 1 1 calc R U .
H41C H -0.117468 0.099357 0.451539 0.110 Uiso 1 1 calc R U .
C42 C -0.0449(19) 0.3624(11) 0.4716(7) 0.091(7) Uani 1 1 d . . .
H42A H -0.041543 0.407123 0.494656 0.136 Uiso 1 1 calc R U .
H42B H -0.107425 0.360032 0.451499 0.136 Uiso 1 1 calc R U .
H42C H 0.028264 0.382220 0.458237 0.136 Uiso 1 1 calc R U .
C43 C -0.2152(15) 0.2091(14) 0.5128(6) 0.082(5) Uani 1 1 d . . .
H43A H -0.236809 0.144206 0.520659 0.123 Uiso 1 1 calc R U .
H43B H -0.272171 0.214132 0.491966 0.123 Uiso 1 1 calc R U .
H43C H -0.212446 0.250372 0.537109 0.123 Uiso 1 1 calc R U .
C44 C 0.2183(13) 0.4298(9) 0.5322(5) 0.060(4) Uani 1 1 d . . .
H44A H 0.251208 0.400639 0.510880 0.090 Uiso 1 1 calc R U .
H44B H 0.279679 0.467441 0.552292 0.090 Uiso 1 1 calc R U .
H44C H 0.181075 0.470157 0.519374 0.090 Uiso 1 1 calc R U .
C45 C 0.0150(14) 0.3909(11) 0.5853(6) 0.069(5) Uani 1 1 d . . .
H45A H -0.029456 0.411821 0.564620 0.103 Uiso 1 1 calc R U .
H45B H 0.062197 0.444753 0.603391 0.103 Uiso 1 1 calc R U .
H45C H -0.037618 0.344682 0.601734 0.103 Uiso 1 1 calc R U .
C46 C 0.1884(16) 0.2979(10) 0.6007(5) 0.065(4) Uani 1 1 d . . .
H46A H 0.132825 0.253009 0.616813 0.097 Uiso 1 1 calc R U .
H46B H 0.234261 0.352237 0.618801 0.097 Uiso 1 1 calc R U .
H46C H 0.239313 0.268033 0.588452 0.097 Uiso 1 1 calc R U .
C47 C 0.2321(13) 0.1925(11) 0.4611(5) 0.056(3) Uani 1 1 d . . .
H47A H 0.173863 0.131054 0.453538 0.084 Uiso 1 1 calc R U .
H47B H 0.268655 0.219536 0.436274 0.084 Uiso 1 1 calc R U .
H47C H 0.195372 0.233980 0.473741 0.084 Uiso 1 1 calc R U .
C48 C 0.4106(19) 0.1020(15) 0.4736(6) 0.090(6) Uani 1 1 d . . .
H48A H 0.478221 0.102899 0.490702 0.135 Uiso 1 1 calc R U .
H48B H 0.434254 0.124004 0.446447 0.135 Uiso 1 1 calc R U .
H48C H 0.355493 0.037961 0.470326 0.135 Uiso 1 1 calc R U .
C49 C 0.4556(14) 0.2983(12) 0.5095(6) 0.076(5) Uani 1 1 d . . .
H49A H 0.422413 0.339036 0.524745 0.114 Uiso 1 1 calc R U .
H49B H 0.482268 0.325269 0.483447 0.114 Uiso 1 1 calc R U .
H49C H 0.520746 0.292580 0.526091 0.114 Uiso 1 1 calc R U .
C50 C 0.3931(18) 0.0051(12) 0.5694(7) 0.086(6) Uani 1 1 d . . .
H50A H 0.331613 -0.047255 0.554915 0.130 Uiso 1 1 calc R U .
H50B H 0.420499 -0.016290 0.594510 0.130 Uiso 1 1 calc R U .
H50C H 0.456825 0.028418 0.551427 0.130 Uiso 1 1 calc R U .
C51 C 0.4575(15) 0.1989(11) 0.6095(6) 0.070(5) Uani 1 1 d . . .
H51A H 0.527203 0.208335 0.594478 0.106 Uiso 1 1 calc R U .
H51B H 0.471281 0.184365 0.637846 0.106 Uiso 1 1 calc R U .
H51C H 0.437678 0.256112 0.609755 0.106 Uiso 1 1 calc R U .
C52 C 0.2256(14) 0.0563(10) 0.6221(4) 0.057(3) Uani 1 1 d . . .
H52A H 0.194797 0.105645 0.630029 0.086 Uiso 1 1 calc R U .
H52B H 0.260879 0.038873 0.646567 0.086 Uiso 1 1 calc R U .
H52C H 0.163172 0.001388 0.609827 0.086 Uiso 1 1 calc R U .
C65 C -0.109(2) 0.1306(15) 0.6155(8) 0.111(6) Uani 1 1 d . U .
H65A H -0.058464 0.179056 0.635829 0.134 Uiso 1 1 calc R U .
H65B H -0.134765 0.162089 0.593016 0.134 Uiso 1 1 calc R U .
C66 C -0.208(2) 0.0696(13) 0.6352(8) 0.100(5) Uani 1 1 d . U .
H66A H -0.279982 0.065417 0.619559 0.120 Uiso 1 1 calc R U .
H66B H -0.209954 0.094946 0.663666 0.120 Uiso 1 1 calc R U .
C67 C -0.1968(17) -0.0239(12) 0.6361(6) 0.080(4) Uani 1 1 d . U .
H67A H -0.253830 -0.069249 0.616302 0.096 Uiso 1 1 calc R U .
H67B H -0.207872 -0.047467 0.664086 0.096 Uiso 1 1 calc R U .
C68 C -0.0777(16) -0.0091(12) 0.6242(6) 0.072(4) Uani 1 1 d . U .
H68A H -0.024240 0.003729 0.648995 0.086 Uiso 1 1 calc R U .
H68B H -0.074384 -0.065501 0.608540 0.086 Uiso 1 1 calc R U .
U4 U 0.96284(5) 0.94226(4) 0.05487(2) 0.05919(15) Uani 1 1 d . . .
Si13 Si 1.1244(5) 0.8176(5) 0.0930(2) 0.098(2) Uani 1 1 d . . .
Si14 Si 0.9767(6) 0.7297(4) 0.0160(2) 0.0864(16) Uani 1 1 d . . .
Si15 Si 0.7234(5) 0.8327(4) 0.10122(17) 0.0777(14) Uani 1 1 d . . .
Si16 Si 0.6687(4) 0.9140(3) 0.02382(16) 0.0666(12) Uani 1 1 d . . .
O2 O 1.0085(13) 1.0823(10) 0.1014(4) 0.099(4) Uani 1 1 d D . .
N9 N 1.0216(13) 0.8177(10) 0.0543(5) 0.074(3) Uani 1 1 d . . .
N10 N 0.7707(12) 0.8946(9) 0.0571(4) 0.065(3) Uani 1 1 d . . .
N11 N 1.000000 1.000000 0.000000 0.058(4) Uani 1 2 d S . P
C53 C 1.1680(18) 0.9368(15) 0.1242(7) 0.102(6) Uani 1 1 d . . .
H53A H 1.098752 0.950058 0.131364 0.153 Uiso 1 1 calc R U .
H53B H 1.214761 0.986136 0.107627 0.153 Uiso 1 1 calc R U .
H53C H 1.212745 0.934551 0.149557 0.153 Uiso 1 1 calc R U .
C54 C 1.068(2) 0.7252(16) 0.1301(8) 0.110(7) Uani 1 1 d . U .
H54A H 1.049146 0.663258 0.115786 0.165 Uiso 1 1 calc R U .
H54B H 0.998748 0.731153 0.141604 0.165 Uiso 1 1 calc R U .
H54C H 1.126657 0.732545 0.152539 0.165 Uiso 1 1 calc R U .
C55 C 1.260(2) 0.8085(19) 0.0740(9) 0.130(9) Uani 1 1 d . . .
H55A H 1.324136 0.840270 0.094252 0.196 Uiso 1 1 calc R U .
H55B H 1.275285 0.838098 0.047685 0.196 Uiso 1 1 calc R U .
H55C H 1.252786 0.742391 0.070001 0.196 Uiso 1 1 calc R U .
C56 C 0.932(3) 0.6096(16) 0.0346(10) 0.165(13) Uani 1 1 d . . .
H56A H 0.848891 0.579268 0.029415 0.247 Uiso 1 1 calc R U .
H56B H 0.952093 0.613213 0.064318 0.247 Uiso 1 1 calc R U .
H56C H 0.972028 0.573009 0.020024 0.247 Uiso 1 1 calc R U .
C57 C 1.090(3) 0.745(2) -0.0216(10) 0.163(11) Uani 1 1 d . U .
H57A H 1.156562 0.733992 -0.008221 0.245 Uiso 1 1 calc R U .
H57B H 1.113185 0.808242 -0.030982 0.245 Uiso 1 1 calc R U .
H57C H 1.059449 0.699282 -0.045257 0.245 Uiso 1 1 calc R U .
C58 C 0.8494(18) 0.7426(12) -0.0130(6) 0.086(5) Uani 1 1 d . . .
H58A H 0.875126 0.796822 -0.029913 0.129 Uiso 1 1 calc R U .
H58B H 0.795654 0.751863 0.006551 0.129 Uiso 1 1 calc R U .
H58C H 0.810931 0.685968 -0.030925 0.129 Uiso 1 1 calc R U .
C59 C 0.620(2) 0.8709(18) 0.1290(7) 0.109(7) Uani 1 1 d . . .
H59A H 0.557640 0.872148 0.109518 0.164 Uiso 1 1 calc R U .
H59B H 0.658559 0.933726 0.142058 0.164 Uiso 1 1 calc R U .
H59C H 0.587702 0.827187 0.150139 0.164 Uiso 1 1 calc R U .
C60 C 0.851(2) 0.8565(15) 0.1389(6) 0.098(6) Uani 1 1 d . . .
H60A H 0.904257 0.920564 0.136652 0.147 Uiso 1 1 calc R U .
H60B H 0.891225 0.812109 0.132611 0.147 Uiso 1 1 calc R U .
H60C H 0.825668 0.849358 0.167002 0.147 Uiso 1 1 calc R U .
C61 C 0.659(2) 0.7035(13) 0.0899(7) 0.102(7) Uani 1 1 d . . .
H61A H 0.719530 0.678924 0.081620 0.153 Uiso 1 1 calc R U .
H61B H 0.599530 0.689864 0.067424 0.153 Uiso 1 1 calc R U .
H61C H 0.625605 0.673720 0.114595 0.153 Uiso 1 1 calc R U .
C62 C 0.621(2) 1.0111(13) 0.0458(7) 0.094(6) Uani 1 1 d . . .
H62A H 0.688488 1.067716 0.051877 0.141 Uiso 1 1 calc R U .
H62B H 0.582410 0.991989 0.071213 0.141 Uiso 1 1 calc R U .
H62C H 0.567994 1.023904 0.025664 0.141 Uiso 1 1 calc R U .
C63 C 0.5399(16) 0.8067(12) 0.0128(7) 0.086(6) Uani 1 1 d . . .
H63A H 0.509612 0.781898 0.038842 0.128 Uiso 1 1 calc R U .
H63B H 0.561592 0.759392 -0.002966 0.128 Uiso 1 1 calc R U .
H63C H 0.480743 0.822254 -0.003275 0.128 Uiso 1 1 calc R U .
C64 C 0.7254(17) 0.9473(12) -0.0266(5) 0.077(5) Uani 1 1 d . . .
H64A H 0.746604 0.896342 -0.039447 0.115 Uiso 1 1 calc R U .
H64B H 0.793518 1.004094 -0.022884 0.115 Uiso 1 1 calc R U .
H64C H 0.666514 0.959184 -0.044361 0.115 Uiso 1 1 calc R U .
C69 C 1.119(2) 1.151(2) 0.1193(9) 0.164(10) Uani 1 1 d D U .
H69A H 1.176850 1.120378 0.123306 0.197 Uiso 1 1 calc R U .
H69B H 1.148522 1.202330 0.100547 0.197 Uiso 1 1 calc R U .
C70 C 1.098(2) 1.188(2) 0.1576(9) 0.169(9) Uani 1 1 d D U .
H70A H 1.127840 1.257400 0.158951 0.203 Uiso 1 1 calc R U .
H70B H 1.135967 1.166575 0.180564 0.203 Uiso 1 1 calc R U .
C71 C 0.976(2) 1.154(2) 0.1605(9) 0.163(9) Uani 1 1 d D U .
H71A H 0.949502 1.206443 0.169791 0.196 Uiso 1 1 calc R U .
H71B H 0.953897 1.105790 0.180826 0.196 Uiso 1 1 calc R U .
C72 C 0.922(2) 1.116(2) 0.1206(9) 0.157(9) Uani 1 1 d D U .
H72A H 0.906602 1.164176 0.104403 0.188 Uiso 1 1 calc R U .
H72B H 0.849534 1.063533 0.123029 0.188 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0935
1 2 2 0.0717
1 -1 1 0.0738
1 0 1 0.0664
1 -2 1 0.0766
-2 -1 -2 0.0719
1 1 1 0.0706
2 -1 2 0.0649
2 -2 -1 0.0835
1 0 0 0.0689
2 2 1 0.0717
0 2 1 0.0655
2 -1 -1 0.0760
-2 1 1 0.0685
0 -2 -1 0.0792
0 1 -1 0.0619
-1 0 -2 0.0630
-1 2 -2 0.0339
-2 1 -2 0.0438
-7 7 2 0.0438
-4 9 8 0.0594
-6 6 12 0.0699
6 0 13 0.0666
5 -6 14 0.0758
7 -2 -11 0.0900
7 2 -7 0.0777
0 3 -20 0.0869
1 5 -17 0.0744
-6 3 -14 0.0529
-4 -6 -5 0.0742
-3 8 12 0.0602
5 0 15 0.0659
4 -4 17 0.0724
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_3
N3 U1 N2 120.2(5) .
N3 U1 N1 93.7(5) .
N2 U1 N1 109.2(5) .
N3 U1 C1 107.1(6) .
N2 U1 C1 125.2(6) .
N1 U1 C1 92.6(5) .
N3 U1 C9 73.4(5) .
N2 U1 C9 88.0(5) .
N1 U1 C9 162.3(5) .
C1 U1 C9 80.2(6) .
N3 U1 Si2 120.6(4) .
N2 U1 Si2 96.8(4) .
N1 U1 Si2 27.4(3) .
C1 U1 Si2 80.0(4) .
C9 U1 Si2 158.6(3) .
N3 U1 Si3 102.0(4) .
N2 U1 Si3 26.5(4) .
N1 U1 Si3 93.2(3) .
C1 U1 Si3 149.9(5) .
C9 U1 Si3 101.1(4) .
Si2 U1 Si3 92.00(14) .
N3 U1 U2 33.0(3) .
N2 U1 U2 118.7(4) .
N1 U1 U2 121.0(3) .
C1 U1 U2 86.7(4) .
C9 U1 U2 43.0(3) .
Si2 U1 U2 143.02(11) .
Si3 U1 U2 114.98(11) .
N3 U2 N5 104.4(4) .
N3 U2 N4 101.1(5) .
N5 U2 N4 108.9(4) .
N3 U2 C10 107.3(6) .
N5 U2 C10 95.2(5) .
N4 U2 C10 136.6(5) .
N3 U2 C9 76.8(5) .
N5 U2 C9 112.2(5) .
N4 U2 C9 138.0(5) .
C10 U2 C9 31.9(6) .
N3 U2 Si8 133.3(3) .
N5 U2 Si8 28.9(3) .
N4 U2 Si8 99.4(3) .
C10 U2 Si8 84.5(4) .
C9 U2 Si8 112.5(4) .
N3 U2 Si6 111.3(4) .
N5 U2 Si6 127.0(4) .
N4 U2 Si6 27.8(3) .
C10 U2 Si6 109.5(5) .
C9 U2 Si6 113.2(4) .
Si8 U2 Si6 106.33(12) .
N3 U2 U1 32.7(3) .
N5 U2 U1 123.4(3) .
N4 U2 U1 113.4(3) .
C10 U2 U1 78.8(5) .
C9 U2 U1 46.8(4) .
Si8 U2 U1 145.70(10) .
Si6 U2 U1 107.43(7) .
N1 Si1 C17 110.1(8) .
N1 Si1 C19 117.0(9) .
C17 Si1 C19 104.9(10) .
N1 Si1 C18 113.7(7) .
C17 Si1 C18 108.6(8) .
C19 Si1 C18 101.7(8) .
N1 Si2 C20 112.4(8) .
N1 Si2 C22 109.0(8) .
C20 Si2 C22 106.6(10) .
N1 Si2 C21 114.4(7) .
C20 Si2 C21 109.0(10) .
C22 Si2 C21 104.8(10) .
N1 Si2 U1 37.8(5) .
C20 Si2 U1 116.4(7) .
C22 Si2 U1 72.2(6) .
C21 Si2 U1 133.5(7) .
N2 Si3 C23 108.9(9) .
N2 Si3 C24 112.1(10) .
C23 Si3 C24 105.4(13) .
N2 Si3 C25 116.1(11) .
C23 Si3 C25 106.8(11) .
C24 Si3 C25 106.8(13) .
N2 Si3 U1 36.8(5) .
C23 Si3 U1 73.0(7) .
C24 Si3 U1 114.9(9) .
C25 Si3 U1 136.8(9) .
N2 Si4 C26 109.4(11) .
N2 Si4 C28 113.5(11) .
C26 Si4 C28 107.9(15) .
N2 Si4 C27 113.9(10) .
C26 Si4 C27 104.7(13) .
C28 Si4 C27 106.9(15) .
N4 Si5 C31 110.4(7) .
N4 Si5 C30 113.9(8) .
C31 Si5 C30 105.5(11) .
N4 Si5 C29 111.6(9) .
C31 Si5 C29 108.5(8) .
C30 Si5 C29 106.6(12) .
N4 Si6 C33 113.3(7) .
N4 Si6 C32 114.1(7) .
C33 Si6 C32 107.5(10) .
N4 Si6 C34 106.7(7) .
C33 Si6 C34 105.7(8) .
C32 Si6 C34 109.1(10) .
N4 Si6 U2 38.9(4) .
C33 Si6 U2 123.2(7) .
C32 Si6 U2 128.4(7) .
C34 Si6 U2 67.8(5) .
N5 Si7 C36 111.8(7) .
N5 Si7 C37 109.7(7) .
C36 Si7 C37 108.3(9) .
N5 Si7 C35 115.1(8) .
C36 Si7 C35 104.0(8) .
C37 Si7 C35 107.7(9) .
N5 Si8 C39 107.9(6) .
N5 Si8 C38 112.7(8) .
C39 Si8 C38 105.4(9) .
N5 Si8 C40 113.4(9) .
C39 Si8 C40 107.6(9) .
C38 Si8 C40 109.4(10) .
N5 Si8 U2 39.3(4) .
C39 Si8 U2 69.3(5) .
C38 Si8 U2 130.6(7) .
C40 Si8 U2 119.2(7) .
Si2 N1 Si1 117.7(8) .
Si2 N1 U1 114.8(7) .
Si1 N1 U1 124.6(6) .
Si3 N2 Si4 119.2(9) .
Si3 N2 U1 116.7(7) .
Si4 N2 U1 124.1(8) .
U1 N3 U2 114.3(5) .
Si5 N4 Si6 124.5(8) .
Si5 N4 U2 122.2(6) .
Si6 N4 U2 113.3(6) .
Si7 N5 Si8 119.2(7) .
Si7 N5 U2 125.0(6) .
Si8 N5 U2 111.8(6) .
C2 C1 U1 169.4(16) .
C1 C2 C3 178(3) .
C8 C3 C2 123(2) .
C8 C3 C4 114.5(18) .
C2 C3 C4 122(2) .
C5 C4 C3 124(2) .
C4 C5 C6 118(2) .
C7 C6 C5 120(2) .
C6 C7 C8 120(3) .
C7 C8 C3 123(2) .
C10 C9 U2 67.6(10) .
C10 C9 U1 157.6(12) .
U2 C9 U1 90.1(5) .
C9 C10 C11 124.2(16) .
C9 C10 U2 80.4(11) .
C11 C10 U2 154.3(12) .
C16 C11 C12 110(2) .
C16 C11 C10 124(2) .
C12 C11 C10 125.9(18) .
C13 C12 C11 125(2) .
C12 C13 C14 122(3) .
C13 C14 C15 116(2) .
C16 C15 C14 120(2) .
C15 C16 C11 127(2) .
N8 U3 N6 111.9(3) .
N8 U3 N7 107.1(2) .
N6 U3 N7 114.6(4) .
N8 U3 O1 100.1(2) .
N6 U3 O1 93.7(4) .
N7 U3 O1 128.3(4) .
N8 U3 Si10 139.99(7) .
N6 U3 Si10 28.3(3) .
N7 U3 Si10 96.1(3) .
O1 U3 Si10 89.8(2) .
N8 U3 Si11 97.05(6) .
N6 U3 Si11 97.6(3) .
N7 U3 Si11 26.6(3) .
O1 U3 Si11 154.3(3) .
Si10 U3 Si11 89.28(10) .
N8 U3 Si12 112.13(6) .
N6 U3 Si12 129.0(3) .
N7 U3 Si12 26.1(3) .
O1 U3 Si12 102.7(3) .
Si10 U3 Si12 103.06(9) .
Si11 U3 Si12 52.64(11) .
N8 U3 U3 0.0 2_556
N6 U3 U3 111.9(3) 2_556
N7 U3 U3 107.1(2) 2_556
O1 U3 U3 100.1(2) 2_556
Si10 U3 U3 139.99(7) 2_556
Si11 U3 U3 97.05(6) 2_556
Si12 U3 U3 112.13(6) 2_556
N6 Si9 C43 111.4(8) .
N6 Si9 C41 111.1(7) .
C43 Si9 C41 107.8(9) .
N6 Si9 C42 114.0(7) .
C43 Si9 C42 106.5(10) .
C41 Si9 C42 105.7(9) .
N6 Si10 C45 112.8(7) .
N6 Si10 C44 114.3(6) .
C45 Si10 C44 108.3(8) .
N6 Si10 C46 107.2(6) .
C45 Si10 C46 106.0(8) .
C44 Si10 C46 107.8(8) .
N6 Si10 U3 38.5(4) .
C45 Si10 U3 130.1(5) .
C44 Si10 U3 120.6(5) .
C46 Si10 U3 69.3(4) .
N7 Si11 C48 113.3(8) .
N7 Si11 C47 106.8(7) .
C48 Si11 C47 108.2(8) .
N7 Si11 C49 112.9(7) .
C48 Si11 C49 108.4(10) .
C47 Si11 C49 107.1(8) .
N7 Si11 U3 36.3(4) .
C48 Si11 U3 126.6(8) .
C47 Si11 U3 70.5(5) .
C49 Si11 U3 123.3(6) .
N7 Si12 C50 112.7(8) .
N7 Si12 C51 112.4(7) .
C50 Si12 C51 107.8(9) .
N7 Si12 C52 108.1(7) .
C50 Si12 C52 108.0(8) .
C51 Si12 C52 107.5(8) .
N7 Si12 U3 35.5(4) .
C50 Si12 U3 123.2(7) .
C51 Si12 U3 126.5(6) .
C52 Si12 U3 72.7(5) .
C68 O1 C65 103.9(13) .
C68 O1 U3 132.1(10) .
C65 O1 U3 124.0(10) .
Si10 N6 Si9 119.9(6) .
Si10 N6 U3 113.3(6) .
Si9 N6 U3 126.8(5) .
Si11 N7 Si12 124.4(7) .
Si11 N7 U3 117.1(6) .
Si12 N7 U3 118.4(6) .
U3 N8 U3 180.0 2_556
C66 C65 O1 107.0(16) .
C65 C66 C67 108.0(18) .
C66 C67 C68 104.3(15) .
O1 C68 C67 106.9(16) .
N11 U4 N10 106.5(4) .
N11 U4 N9 106.8(4) .
N10 U4 N9 109.7(5) .
N11 U4 O2 100.9(4) .
N10 U4 O2 97.7(5) .
N9 U4 O2 132.8(6) .
N11 U4 Si15 135.68(11) .
N10 U4 Si15 29.4(4) .
N9 U4 Si15 93.3(4) .
O2 U4 Si15 92.6(4) .
N11 U4 Si13 118.71(12) .
N10 U4 Si13 122.8(4) .
N9 U4 Si13 27.1(4) .
O2 U4 Si13 105.7(4) .
Si15 U4 Si13 97.16(15) .
N11 U4 U4 0.0 2_775
N10 U4 U4 106.5(4) 2_775
N9 U4 U4 106.8(4) 2_775
O2 U4 U4 100.9(4) 2_775
Si15 U4 U4 135.67(10) 2_775
Si13 U4 U4 118.71(12) 2_775
N9 Si13 C55 114.9(11) .
N9 Si13 C54 113.2(9) .
C55 Si13 C54 108.4(13) .
N9 Si13 C53 107.1(9) .
C55 Si13 C53 105.8(12) .
C54 Si13 C53 106.9(11) .
N9 Si13 U4 35.8(5) .
C55 Si13 U4 128.3(9) .
C54 Si13 U4 122.0(9) .
C53 Si13 U4 71.4(6) .
N9 Si14 C56 114.4(12) .
N9 Si14 C57 110.2(12) .
C56 Si14 C57 110.2(16) .
N9 Si14 C58 107.4(8) .
C56 Si14 C58 107.8(13) .
C57 Si14 C58 106.5(13) .
N10 Si15 C59 113.9(10) .
N10 Si15 C61 113.2(8) .
C59 Si15 C61 108.0(12) .
N10 Si15 C60 107.9(9) .
C59 Si15 C60 105.4(11) .
C61 Si15 C60 108.0(11) .
N10 Si15 U4 38.7(5) .
C59 Si15 U4 134.6(9) .
C61 Si15 U4 116.4(8) .
C60 Si15 U4 70.6(7) .
N10 Si16 C64 111.6(9) .
N10 Si16 C63 112.0(8) .
C64 Si16 C63 105.5(9) .
N10 Si16 C62 110.9(9) .
C64 Si16 C62 107.8(10) .
C63 Si16 C62 108.9(10) .
C72 O2 C69 102.2(17) .
C72 O2 U4 124.8(12) .
C69 O2 U4 132.9(14) .
Si14 N9 Si13 120.5(9) .
Si14 N9 U4 122.2(8) .
Si13 N9 U4 117.1(8) .
Si16 N10 Si15 118.2(9) .
Si16 N10 U4 129.7(8) .
Si15 N10 U4 112.0(7) .
U4 N11 U4 179.998(13) 2_775
C70 C69 O2 108.1(19) .
C69 C70 C71 106(2) .
C70 C71 C72 108(2) .
C71 C72 O2 103.8(19) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N3 2.146(11) .
U1 N2 2.306(15) .
U1 N1 2.307(14) .
U1 C1 2.466(16) .
U1 C9 2.641(18) .
U1 Si2 3.419(5) .
U1 Si3 3.438(6) .
U1 U2 3.6201(7) .
U2 N3 2.163(13) .
U2 N5 2.279(11) .
U2 N4 2.310(13) .
U2 C10 2.317(17) .
U2 C9 2.470(16) .
U2 Si8 3.342(4) .
U2 Si6 3.379(4) .
Si1 N1 1.741(15) .
Si1 C17 1.85(2) .
Si1 C19 1.870(19) .
Si1 C18 1.890(14) .
Si2 N1 1.733(12) .
Si2 C20 1.87(2) .
Si2 C22 1.90(2) .
Si2 C21 1.91(2) .
Si3 N2 1.717(16) .
Si3 C23 1.85(2) .
Si3 C24 1.87(2) .
Si3 C25 1.90(2) .
Si4 N2 1.733(15) .
Si4 C26 1.85(3) .
Si4 C28 1.87(3) .
Si4 C27 1.91(2) .
Si5 N4 1.716(12) .
Si5 C31 1.811(18) .
Si5 C30 1.86(2) .
Si5 C29 1.876(19) .
Si6 N4 1.717(12) .
Si6 C33 1.867(17) .
Si6 C32 1.867(19) .
Si6 C34 1.916(17) .
Si7 N5 1.733(13) .
Si7 C36 1.860(15) .
Si7 C37 1.871(19) .
Si7 C35 1.879(16) .
Si8 N5 1.740(13) .
Si8 C39 1.886(16) .
Si8 C38 1.891(17) .
Si8 C40 1.90(2) .
C1 C2 1.22(2) .
C2 C3 1.39(3) .
C3 C8 1.38(3) .
C3 C4 1.42(3) .
C4 C5 1.33(3) .
C5 C6 1.42(4) .
C6 C7 1.34(3) .
C7 C8 1.36(3) .
C9 C10 1.33(2) .
C10 C11 1.48(3) .
C11 C16 1.39(3) .
C11 C12 1.40(3) .
C12 C13 1.35(3) .
C13 C14 1.36(3) .
C14 C15 1.39(3) .
C15 C16 1.34(3) .
U3 N8 2.0464(4) .
U3 N6 2.269(11) .
U3 N7 2.281(12) .
U3 O1 2.465(10) .
U3 Si10 3.351(3) .
U3 Si11 3.428(4) .
U3 Si12 3.453(4) .
U3 U3 4.0929(8) 2_556
Si9 N6 1.747(12) .
Si9 C43 1.855(19) .
Si9 C41 1.863(16) .
Si9 C42 1.863(16) .
Si10 N6 1.728(9) .
Si10 C45 1.863(15) .
Si10 C44 1.865(14) .
Si10 C46 1.869(17) .
Si11 N7 1.724(13) .
Si11 C48 1.831(18) .
Si11 C47 1.867(15) .
Si11 C49 1.885(15) .
Si12 N7 1.725(12) .
Si12 C50 1.851(18) .
Si12 C51 1.858(15) .
Si12 C52 1.880(17) .
O1 C68 1.448(19) .
O1 C65 1.49(2) .
C65 C66 1.46(3) .
C66 C67 1.48(3) .
C67 C68 1.49(3) .
U4 N11 2.0261(6) .
U4 N10 2.246(14) .
U4 N9 2.246(15) .
U4 O2 2.441(13) .
U4 Si15 3.334(5) .
U4 Si13 3.419(7) .
U4 U4 4.0523(11) 2_775
Si13 N9 1.751(16) .
Si13 C55 1.86(3) .
Si13 C54 1.87(2) .
Si13 C53 1.93(2) .
Si14 N9 1.716(16) .
Si14 C56 1.86(3) .
Si14 C57 1.86(3) .
Si14 C58 1.87(2) .
Si15 N10 1.763(15) .
Si15 C59 1.83(2) .
Si15 C61 1.866(19) .
Si15 C60 1.88(2) .
Si16 N10 1.736(15) .
Si16 C64 1.836(18) .
Si16 C63 1.864(16) .
Si16 C62 1.886(18) .
O2 C72 1.48(2) .
O2 C69 1.49(2) .
C69 C70 1.41(2) .
C70 C71 1.43(2) .
C71 C72 1.43(2) .
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
C20 Si2 N1 Si1 57.0(12)
C22 Si2 N1 Si1 175.0(9)
C21 Si2 N1 Si1 -68.1(13)
U1 Si2 N1 Si1 161.6(13)
C20 Si2 N1 U1 -104.6(10)
C22 Si2 N1 U1 13.5(10)
C21 Si2 N1 U1 130.4(11)
C17 Si1 N1 Si2 -99.9(10)
C19 Si1 N1 Si2 19.8(12)
C18 Si1 N1 Si2 137.9(8)
C17 Si1 N1 U1 59.7(10)
C19 Si1 N1 U1 179.4(8)
C18 Si1 N1 U1 -62.5(10)
C23 Si3 N2 Si4 166.1(11)
C24 Si3 N2 Si4 -77.6(15)
C25 Si3 N2 Si4 45.6(14)
U1 Si3 N2 Si4 180.0(15)
C23 Si3 N2 U1 -13.8(12)
C24 Si3 N2 U1 102.4(12)
C25 Si3 N2 U1 -134.4(10)
C26 Si4 N2 Si3 163.2(13)
C28 Si4 N2 Si3 -76.2(16)
C27 Si4 N2 Si3 46.4(16)
C26 Si4 N2 U1 -16.9(15)
C28 Si4 N2 U1 103.8(15)
C27 Si4 N2 U1 -133.7(13)
C31 Si5 N4 Si6 155.0(9)
C30 Si5 N4 Si6 36.4(14)
C29 Si5 N4 Si6 -84.3(11)
C31 Si5 N4 U2 -27.9(10)
C30 Si5 N4 U2 -146.5(11)
C29 Si5 N4 U2 92.8(10)
C33 Si6 N4 Si5 -68.1(11)
C32 Si6 N4 Si5 55.3(13)
C34 Si6 N4 Si5 175.9(9)
U2 Si6 N4 Si5 177.3(13)
C33 Si6 N4 U2 114.6(8)
C32 Si6 N4 U2 -121.9(10)
C34 Si6 N4 U2 -1.4(9)
C36 Si7 N5 Si8 142.8(8)
C37 Si7 N5 Si8 -97.0(10)
C35 Si7 N5 Si8 24.5(12)
C36 Si7 N5 U2 -61.5(10)
C37 Si7 N5 U2 58.6(11)
C35 Si7 N5 U2 -179.8(9)
C39 Si8 N5 Si7 169.8(9)
C38 Si8 N5 Si7 -74.3(11)
C40 Si8 N5 Si7 50.7(11)
U2 Si8 N5 Si7 158.7(13)
C39 Si8 N5 U2 11.1(10)
C38 Si8 N5 U2 127.0(8)
C40 Si8 N5 U2 -108.0(9)
C8 C3 C4 C5 1(3)
C2 C3 C4 C5 -179(2)
C3 C4 C5 C6 -4(4)
C4 C5 C6 C7 5(4)
C5 C6 C7 C8 -3(4)
C6 C7 C8 C3 0(4)
C2 C3 C8 C7 -179(2)
C4 C3 C8 C7 1(3)
U2 C9 C10 C11 171.9(19)
U1 C9 C10 C11 166(3)
U1 C9 C10 U2 -6(4)
C9 C10 C11 C16 127(2)
U2 C10 C11 C16 -71(4)
C9 C10 C11 C12 -60(3)
U2 C10 C11 C12 101(3)
C16 C11 C12 C13 2(3)
C10 C11 C12 C13 -172(2)
C11 C12 C13 C14 -6(4)
C12 C13 C14 C15 6(4)
C13 C14 C15 C16 -2(4)
C14 C15 C16 C11 -2(4)
C12 C11 C16 C15 3(3)
C10 C11 C16 C15 176(2)
C45 Si10 N6 Si9 50.9(11)
C44 Si10 N6 Si9 -73.4(10)
C46 Si10 N6 Si9 167.2(8)
U3 Si10 N6 Si9 177.3(12)
C45 Si10 N6 U3 -126.4(8)
C44 Si10 N6 U3 109.3(8)
C46 Si10 N6 U3 -10.1(9)
C43 Si9 N6 Si10 -91.6(10)
C41 Si9 N6 Si10 148.3(9)
C42 Si9 N6 Si10 29.0(12)
C43 Si9 N6 U3 85.3(10)
C41 Si9 N6 U3 -34.8(11)
C42 Si9 N6 U3 -154.1(10)
C48 Si11 N7 Si12 55.5(11)
C47 Si11 N7 Si12 174.5(7)
C49 Si11 N7 Si12 -68.1(10)
U3 Si11 N7 Si12 176.2(10)
C48 Si11 N7 U3 -120.7(9)
C47 Si11 N7 U3 -1.8(7)
C49 Si11 N7 U3 115.6(8)
C50 Si12 N7 Si11 -60.4(10)
C51 Si12 N7 Si11 61.7(10)
C52 Si12 N7 Si11 -179.8(7)
U3 Si12 N7 Si11 -176.2(10)
C50 Si12 N7 U3 115.8(8)
C51 Si12 N7 U3 -122.1(8)
C52 Si12 N7 U3 -3.6(7)
C68 O1 C65 C66 -25(3)
U3 O1 C65 C66 156.3(16)
O1 C65 C66 C67 8(3)
C65 C66 C67 C68 11(3)
C65 O1 C68 C67 32(2)
U3 O1 C68 C67 -149.2(12)
C66 C67 C68 O1 -27(2)
C56 Si14 N9 Si13 50.2(17)
C57 Si14 N9 Si13 -74.6(16)
C58 Si14 N9 Si13 169.8(10)
C56 Si14 N9 U4 -134.4(15)
C57 Si14 N9 U4 100.7(15)
C58 Si14 N9 U4 -14.9(12)
C55 Si13 N9 Si14 54.0(15)
C54 Si13 N9 Si14 -71.4(15)
C53 Si13 N9 Si14 171.1(11)
U4 Si13 N9 Si14 175.6(16)
C55 Si13 N9 U4 -121.6(12)
C54 Si13 N9 U4 113.0(12)
C53 Si13 N9 U4 -4.5(12)
C64 Si16 N10 Si15 -163.3(9)
C63 Si16 N10 Si15 -45.3(12)
C62 Si16 N10 Si15 76.6(11)
C64 Si16 N10 U4 19.7(12)
C63 Si16 N10 U4 137.7(10)
C62 Si16 N10 U4 -100.4(11)
C59 Si15 N10 Si16 -45.1(13)
C61 Si15 N10 Si16 78.7(13)
C60 Si15 N10 Si16 -161.8(10)
U4 Si15 N10 Si16 -177.5(13)
C59 Si15 N10 U4 132.4(10)
C61 Si15 N10 U4 -103.8(11)
C60 Si15 N10 U4 15.8(11)
C72 O2 C69 C70 26(4)
U4 O2 C69 C70 -151(2)
O2 C69 C70 C71 -9(5)
C69 C70 C71 C72 -13(5)
C70 C71 C72 O2 29(4)
C69 O2 C72 C71 -33(4)
U4 O2 C72 C71 145(2)
