#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/02/4120282.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_4120282
loop_
_publ_author_name
'Clément Camp'
'Jacques Pécaut'
'Marinella Mazzanti'
_publ_section_title
;
 Tuning Uranium-Nitrogen Multiple Bond Formation with Ancillary Siloxide
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12101
_journal_page_last               12111
_journal_paper_doi               10.1021/ja405815b
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C71.5 H150.5 K N O22 Si4 U'
_chemical_formula_weight         1765.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.358(4)
_cell_angle_beta                 91.810(4)
_cell_angle_gamma                118.909(5)
_cell_formula_units_Z            2
_cell_length_a                   14.4543(8)
_cell_length_b                   14.5344(8)
_cell_length_c                   25.4464(12)
_cell_measurement_reflns_used    3690
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0035
_cell_measurement_theta_min      3.2585
_cell_volume                     4651.9(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -39.00   50.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613   57.0000  120.0000 89

  2 omega  -25.00   23.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613  -99.0000 -120.0000 48

  3 omega  -42.00   52.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613   37.0000 -120.0000 94

  4 omega  -87.00    3.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613  -57.0000  -30.0000 90

  5 omega  -95.00  -32.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613  179.0000 -120.0000 63

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_sigmaI/netI    0.2167
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35721
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    1.902
_exptl_absorpt_correction_T_max  0.9487
_exptl_absorpt_correction_T_min  0.8195
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'translucent light bronze'
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             1859
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     978
_refine_ls_number_reflns         18800
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0259P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                11498
_reflns_number_total             18800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_05.cif
_cod_data_source_block           5-Ad
_cod_original_cell_volume        4651.9(4)
_cod_original_formula_sum        'C71.50 H150.50 K N O22 Si4 U'
_cod_database_code               4120282
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.86855(3) 0.61958(3) 0.732342(12) 0.01717(9) Uani 1 1 d . . .
Si1 Si 0.95837(19) 0.73756(18) 0.60451(8) 0.0214(5) Uani 1 1 d . . .
O1 O 0.9083(4) 0.6652(4) 0.65074(17) 0.0219(13) Uani 1 1 d . . .
O2 O 1.0252(4) 0.8632(4) 0.62360(19) 0.0293(15) Uani 1 1 d . . .
O3 O 1.0465(5) 0.7200(5) 0.5736(2) 0.0377(17) Uani 1 1 d . . .
O4 O 0.8623(4) 0.7150(4) 0.56060(19) 0.0305(15) Uani 1 1 d . . .
C1 C 0.9995(7) 0.9351(7) 0.6529(3) 0.027(2) Uani 1 1 d . . .
C2 C 0.9355(9) 0.9671(8) 0.6177(4) 0.062(3) Uani 1 1 d . . .
H2A H 0.9773 1.0031 0.5889 0.093 Uiso 1 1 calc R . .
H2B H 0.9175 1.0149 0.6386 0.093 Uiso 1 1 calc R . .
H2C H 0.8702 0.9039 0.6031 0.093 Uiso 1 1 calc R . .
C3 C 0.9371(7) 0.8854(6) 0.7001(3) 0.038(2) Uani 1 1 d . . .
H3A H 0.8693 0.8235 0.6872 0.057 Uiso 1 1 calc R . .
H3B H 0.9240 0.9372 0.7206 0.057 Uiso 1 1 calc R . .
H3C H 0.9781 0.8638 0.7225 0.057 Uiso 1 1 calc R . .
C4 C 1.1044(7) 1.0305(7) 0.6726(3) 0.046(3) Uani 1 1 d . . .
H4A H 1.1447 1.0089 0.6956 0.069 Uiso 1 1 calc R . .
H4B H 1.0916 1.0830 0.6926 0.069 Uiso 1 1 calc R . .
H4C H 1.1450 1.0613 0.6424 0.069 Uiso 1 1 calc R . .
C5 C 1.0926(7) 0.6549(7) 0.5797(3) 0.027(2) Uani 1 1 d . . .
C6 C 1.0056(8) 0.5399(8) 0.5734(4) 0.059(3) Uani 1 1 d . . .
H6A H 0.9603 0.5268 0.6029 0.088 Uiso 1 1 calc R . .
H6B H 1.0377 0.4939 0.5733 0.088 Uiso 1 1 calc R . .
H6C H 0.9629 0.5250 0.5400 0.088 Uiso 1 1 calc R . .
C7 C 1.1702(7) 0.6779(7) 0.5371(3) 0.034(2) Uani 1 1 d . . .
H7A H 1.1315 0.6586 0.5022 0.051 Uiso 1 1 calc R . .
H7B H 1.2067 0.6365 0.5407 0.051 Uiso 1 1 calc R . .
H7C H 1.2224 0.7533 0.5411 0.051 Uiso 1 1 calc R . .
C8 C 1.1490(8) 0.6802(8) 0.6336(3) 0.052(3) Uani 1 1 d . . .
H8A H 1.1990 0.7561 0.6397 0.078 Uiso 1 1 calc R . .
H8B H 1.1878 0.6407 0.6361 0.078 Uiso 1 1 calc R . .
H8C H 1.0972 0.6603 0.6604 0.078 Uiso 1 1 calc R . .
C9 C 0.8573(7) 0.7255(8) 0.5053(3) 0.034(2) Uani 1 1 d . . .
C10 C 0.7628(9) 0.7420(9) 0.4945(3) 0.065(4) Uani 1 1 d . . .
H10A H 0.6986 0.6814 0.5045 0.097 Uiso 1 1 calc R . .
H10B H 0.7549 0.7485 0.4568 0.097 Uiso 1 1 calc R . .
H10C H 0.7740 0.8066 0.5153 0.097 Uiso 1 1 calc R . .
C11 C 0.8413(9) 0.6265(9) 0.4739(3) 0.067(4) Uani 1 1 d . . .
H11C H 0.9038 0.6180 0.4801 0.101 Uiso 1 1 calc R . .
H11D H 0.8307 0.6313 0.4362 0.101 Uiso 1 1 calc R . .
H11E H 0.7787 0.5655 0.4849 0.101 Uiso 1 1 calc R . .
C12 C 0.9580(8) 0.8216(9) 0.4915(4) 0.076(4) Uani 1 1 d . . .
H12A H 0.9661 0.8854 0.5118 0.114 Uiso 1 1 calc R . .
H12B H 0.9531 0.8284 0.4536 0.114 Uiso 1 1 calc R . .
H12C H 1.0196 0.8126 0.5002 0.114 Uiso 1 1 calc R . .
Si2 Si 0.8879(2) 0.3988(2) 0.78565(9) 0.0257(6) Uani 1 1 d . . .
O21 O 0.8508(4) 0.4703(4) 0.75691(18) 0.0265(14) Uani 1 1 d . . .
O22 O 0.9156(5) 0.4417(5) 0.8481(2) 0.0393(17) Uani 1 1 d . . .
O23 O 0.9949(5) 0.4030(4) 0.7646(2) 0.0334(15) Uani 1 1 d . . .
O24 O 0.8017(5) 0.2737(5) 0.7785(2) 0.0410(17) Uani 1 1 d . . .
C21 C 0.9616(8) 0.4149(7) 0.8916(3) 0.033(2) Uani 1 1 d . . .
C22 C 0.8823(8) 0.3839(9) 0.9334(4) 0.069(4) Uani 1 1 d . . .
H22A H 0.8651 0.4406 0.9416 0.104 Uiso 1 1 calc R . .
H22B H 0.9128 0.3721 0.9654 0.104 Uiso 1 1 calc R . .
H22C H 0.8176 0.3188 0.9201 0.104 Uiso 1 1 calc R . .
C23 C 0.9872(10) 0.3299(8) 0.8774(4) 0.073(4) Uani 1 1 d . . .
H23A H 0.9229 0.2661 0.8624 0.109 Uiso 1 1 calc R . .
H23B H 1.0155 0.3146 0.9091 0.109 Uiso 1 1 calc R . .
H23C H 1.0404 0.3525 0.8513 0.109 Uiso 1 1 calc R . .
C24 C 1.0592(9) 0.5145(8) 0.9125(4) 0.063(3) Uani 1 1 d . . .
H24A H 1.1078 0.5399 0.8844 0.095 Uiso 1 1 calc R . .
H24B H 1.0939 0.5007 0.9422 0.095 Uiso 1 1 calc R . .
H24C H 1.0400 0.5682 0.9245 0.095 Uiso 1 1 calc R . .
C25 C 1.0129(8) 0.3519(8) 0.7178(4) 0.041(3) Uani 1 1 d . . .
C26 C 1.1273(9) 0.4265(9) 0.7061(4) 0.075(4) Uani 1 1 d . . .
H26A H 1.1323 0.4914 0.6944 0.112 Uiso 1 1 calc R . .
H26B H 1.1485 0.3919 0.6782 0.112 Uiso 1 1 calc R . .
H26C H 1.1743 0.4441 0.7382 0.112 Uiso 1 1 calc R . .
C27 C 0.9995(10) 0.2457(8) 0.7309(4) 0.076(4) Uani 1 1 d . . .
H27A H 1.0460 0.2565 0.7623 0.114 Uiso 1 1 calc R . .
H27B H 1.0182 0.2131 0.7009 0.114 Uiso 1 1 calc R . .
H27C H 0.9256 0.1992 0.7378 0.114 Uiso 1 1 calc R . .
C28 C 0.9355(9) 0.3357(9) 0.6721(3) 0.065(4) Uani 1 1 d . . .
H28A H 0.8630 0.2890 0.6811 0.098 Uiso 1 1 calc R . .
H28B H 0.9505 0.3035 0.6406 0.098 Uiso 1 1 calc R . .
H28C H 0.9426 0.4040 0.6650 0.098 Uiso 1 1 calc R . .
C29 C 0.6897(8) 0.2156(7) 0.7849(4) 0.037(2) Uani 1 1 d . . .
C30 C 0.6750(10) 0.1270(10) 0.8157(6) 0.118(6) Uani 1 1 d U . .
H30A H 0.6872 0.0762 0.7936 0.177 Uiso 1 1 calc R . .
H30B H 0.6025 0.0917 0.8267 0.177 Uiso 1 1 calc R . .
H30C H 0.7255 0.1548 0.8470 0.177 Uiso 1 1 calc R . .
C31 C 0.6326(10) 0.1744(10) 0.7312(4) 0.100(5) Uani 1 1 d . . .
H31A H 0.6480 0.2338 0.7106 0.150 Uiso 1 1 calc R . .
H31B H 0.5561 0.1343 0.7347 0.150 Uiso 1 1 calc R . .
H31C H 0.6561 0.1282 0.7132 0.150 Uiso 1 1 calc R . .
C32 C 0.6502(8) 0.2836(9) 0.8131(4) 0.067(4) Uani 1 1 d . . .
H32A H 0.6907 0.3145 0.8474 0.101 Uiso 1 1 calc R . .
H32B H 0.5749 0.2401 0.8186 0.101 Uiso 1 1 calc R . .
H32C H 0.6592 0.3402 0.7917 0.101 Uiso 1 1 calc R . .
Si3 Si 0.8407(2) 0.7903(2) 0.84023(10) 0.0307(6) Uani 1 1 d . . .
O41 O 0.8268(4) 0.7094(4) 0.79143(19) 0.0260(14) Uani 1 1 d . . .
O42 O 0.9386(5) 0.9049(5) 0.8344(2) 0.0397(17) Uani 1 1 d . . .
O43 O 0.8818(6) 0.7639(6) 0.8974(2) 0.061(2) Uani 1 1 d . . .
O44 O 0.7374(6) 0.7906(5) 0.8564(3) 0.063(2) Uani 1 1 d . . .
C41 C 0.9845(8) 1.0035(8) 0.8669(4) 0.047(3) Uani 1 1 d . . .
C42 C 1.0536(11) 1.0849(9) 0.8326(4) 0.105(5) Uani 1 1 d . . .
H42A H 1.1032 1.0646 0.8173 0.158 Uiso 1 1 calc R . .
H42B H 1.0934 1.1535 0.8539 0.158 Uiso 1 1 calc R . .
H42C H 1.0095 1.0901 0.8042 0.158 Uiso 1 1 calc R . .
C43 C 1.0551(11) 1.0033(9) 0.9116(4) 0.098(5) Uani 1 1 d U . .
H43A H 1.0133 0.9459 0.9330 0.148 Uiso 1 1 calc R . .
H43B H 1.0861 1.0711 0.9337 0.148 Uiso 1 1 calc R . .
H43C H 1.1119 0.9930 0.8972 0.148 Uiso 1 1 calc R . .
C44 C 0.9053(10) 1.0288(11) 0.8882(7) 0.176(8) Uani 1 1 d U . .
H44A H 0.8568 1.0247 0.8592 0.264 Uiso 1 1 calc R . .
H44B H 0.9411 1.1004 0.9066 0.264 Uiso 1 1 calc R . .
H44C H 0.8650 0.9782 0.9131 0.264 Uiso 1 1 calc R . .
C45 C 0.8234(11) 0.6790(8) 0.9275(4) 0.064(4) Uani 1 1 d U . .
C46 C 0.9153(10) 0.6875(10) 0.9670(5) 0.093(5) Uani 1 1 d . . .
H46A H 0.9676 0.6787 0.9468 0.139 Uiso 1 1 calc R . .
H46B H 0.8851 0.6322 0.9909 0.139 Uiso 1 1 calc R . .
H46C H 0.9499 0.7570 0.9877 0.139 Uiso 1 1 calc R . .
C47 C 0.7525(9) 0.7028(9) 0.9632(4) 0.073(4) Uani 1 1 d . . .
H47A H 0.7912 0.7767 0.9785 0.109 Uiso 1 1 calc R . .
H47B H 0.7321 0.6563 0.9916 0.109 Uiso 1 1 calc R . .
H47C H 0.6887 0.6904 0.9423 0.109 Uiso 1 1 calc R . .
C48 C 0.7642(13) 0.5746(9) 0.8960(4) 0.126(7) Uani 1 1 d . . .
H48A H 0.7013 0.5693 0.8771 0.189 Uiso 1 1 calc R . .
H48B H 0.7423 0.5185 0.9195 0.189 Uiso 1 1 calc R . .
H48C H 0.8098 0.5668 0.8703 0.189 Uiso 1 1 calc R . .
C49 C 0.6428(9) 0.7777(9) 0.8203(5) 0.064(3) Uani 1 1 d U . .
C50 C 0.6783(12) 0.8367(10) 0.7764(5) 0.135(7) Uani 1 1 d U . .
H50A H 0.7482 0.8984 0.7861 0.202 Uiso 1 1 calc R . .
H50B H 0.6280 0.8602 0.7658 0.202 Uiso 1 1 calc R . .
H50C H 0.6834 0.7924 0.7469 0.202 Uiso 1 1 calc R . .
C51 C 0.5742(8) 0.6592(8) 0.8066(4) 0.067(4) Uani 1 1 d . . .
H51A H 0.5101 0.6445 0.7852 0.101 Uiso 1 1 calc R . .
H51B H 0.5543 0.6248 0.8392 0.101 Uiso 1 1 calc R . .
H51C H 0.6140 0.6317 0.7865 0.101 Uiso 1 1 calc R . .
C52 C 0.5900(8) 0.8209(8) 0.8565(3) 0.062(3) Uani 1 1 d . . .
H52A H 0.6364 0.8971 0.8652 0.093 Uiso 1 1 calc R . .
H52B H 0.5762 0.7858 0.8890 0.093 Uiso 1 1 calc R . .
H52C H 0.5228 0.8080 0.8390 0.093 Uiso 1 1 calc R . .
Si4 Si 0.5875(2) 0.4557(2) 0.67318(9) 0.0292(6) Uani 1 1 d . . .
O61 O 0.7034(4) 0.5324(4) 0.70063(19) 0.0273(14) Uani 1 1 d . A .
O62B O 0.5244(14) 0.5325(14) 0.6666(8) 0.029(6) Uani 0.337(16) 1 d PU A 2
O62 O 0.5444(7) 0.5010(7) 0.6297(4) 0.032(3) Uani 0.663(16) 1 d PU A 1
O63 O 0.5125(5) 0.3984(5) 0.7182(2) 0.0420(17) Uani 1 1 d . A .
O64B O 0.5741(16) 0.4014(18) 0.6176(8) 0.040(7) Uani 0.337(16) 1 d PU A 2
O64 O 0.5842(8) 0.3472(8) 0.6394(4) 0.036(4) Uani 0.663(16) 1 d PU A 1
C61 C 0.5349(7) 0.5979(7) 0.6259(4) 0.035(2) Uani 1 1 d . . .
C62 C 0.6460(7) 0.6893(7) 0.6322(3) 0.043(3) Uani 1 1 d . A .
H62A H 0.6720 0.7050 0.6696 0.064 Uiso 1 1 calc R . .
H62B H 0.6464 0.7514 0.6194 0.064 Uiso 1 1 calc R . .
H62C H 0.6921 0.6710 0.6116 0.064 Uiso 1 1 calc R . .
C63 C 0.4613(9) 0.6166(10) 0.6591(5) 0.118(6) Uani 1 1 d . A .
H63A H 0.3885 0.5596 0.6499 0.178 Uiso 1 1 calc R . .
H63B H 0.4662 0.6844 0.6528 0.178 Uiso 1 1 calc R . .
H63C H 0.4808 0.6180 0.6965 0.178 Uiso 1 1 calc R . .
C64 C 0.4914(11) 0.5709(12) 0.5700(4) 0.120(6) Uani 1 1 d . A .
H64A H 0.5416 0.5625 0.5479 0.180 Uiso 1 1 calc R . .
H64B H 0.4798 0.6277 0.5585 0.180 Uiso 1 1 calc R . .
H64C H 0.4238 0.5047 0.5667 0.180 Uiso 1 1 calc R . .
C65 C 0.4017(7) 0.3250(7) 0.7191(3) 0.032(2) Uani 1 1 d . . .
C66 C 0.3601(8) 0.3765(9) 0.7586(3) 0.059(3) Uani 1 1 d . A .
H66A H 0.4025 0.3957 0.7925 0.088 Uiso 1 1 calc R . .
H66B H 0.2859 0.3268 0.7636 0.088 Uiso 1 1 calc R . .
H66C H 0.3649 0.4401 0.7455 0.088 Uiso 1 1 calc R . .
C67 C 0.3394(7) 0.3016(7) 0.6653(3) 0.043(3) Uani 1 1 d . A .
H67A H 0.3483 0.3678 0.6534 0.064 Uiso 1 1 calc R . .
H67B H 0.2641 0.2536 0.6687 0.064 Uiso 1 1 calc R . .
H67C H 0.3661 0.2685 0.6394 0.064 Uiso 1 1 calc R . .
C68 C 0.3913(8) 0.2237(8) 0.7384(4) 0.064(3) Uani 1 1 d . A .
H68A H 0.4179 0.1907 0.7125 0.095 Uiso 1 1 calc R . .
H68B H 0.3166 0.1748 0.7427 0.095 Uiso 1 1 calc R . .
H68C H 0.4327 0.2406 0.7724 0.095 Uiso 1 1 calc R . .
C69 C 0.6203(9) 0.3402(8) 0.5905(4) 0.043(3) Uani 1 1 d . . .
C70 C 0.7060(11) 0.4384(10) 0.5714(5) 0.139(7) Uani 1 1 d U A .
H70A H 0.6801 0.4887 0.5672 0.208 Uiso 1 1 calc R . .
H70B H 0.7261 0.4204 0.5373 0.208 Uiso 1 1 calc R . .
H70C H 0.7678 0.4702 0.5972 0.208 Uiso 1 1 calc R . .
C71 C 0.6671(17) 0.2739(17) 0.6001(7) 0.249(14) Uani 1 1 d . A .
H71A H 0.7363 0.3165 0.6200 0.373 Uiso 1 1 calc R . .
H71B H 0.6761 0.2434 0.5663 0.373 Uiso 1 1 calc R . .
H71C H 0.6204 0.2170 0.6206 0.373 Uiso 1 1 calc R . .
C72 C 0.5346(12) 0.2857(12) 0.5480(4) 0.136(7) Uani 1 1 d . A .
H72A H 0.4804 0.2184 0.5588 0.204 Uiso 1 1 calc R . .
H72B H 0.5636 0.2723 0.5158 0.204 Uiso 1 1 calc R . .
H72C H 0.5026 0.3301 0.5410 0.204 Uiso 1 1 calc R . .
N1 N 1.0167(5) 0.6974(5) 0.7582(2) 0.0227(17) Uani 1 1 d . . .
C81 C 1.1233(7) 0.7581(7) 0.7845(3) 0.025(2) Uani 1 1 d . . .
C82 C 1.1202(7) 0.7900(7) 0.8423(3) 0.037(2) Uani 1 1 d . . .
H82A H 1.0796 0.7260 0.8606 0.045 Uiso 1 1 calc R . .
H82B H 1.0840 0.8330 0.8453 0.045 Uiso 1 1 calc R . .
C83 C 1.2337(8) 0.8543(8) 0.8689(3) 0.044(3) Uani 1 1 d . . .
H83 H 1.2309 0.8760 0.9068 0.052 Uiso 1 1 calc R . .
C84 C 1.2889(8) 0.7873(8) 0.8657(3) 0.045(3) Uani 1 1 d . . .
H84A H 1.3617 0.8282 0.8830 0.054 Uiso 1 1 calc R . .
H84B H 1.2494 0.7233 0.8841 0.054 Uiso 1 1 calc R . .
C85 C 1.2929(7) 0.7560(7) 0.8080(3) 0.034(2) Uani 1 1 d . . .
H85 H 1.3285 0.7117 0.8058 0.040 Uiso 1 1 calc R . .
C86 C 1.1802(7) 0.6909(7) 0.7814(3) 0.030(2) Uani 1 1 d . . .
H86A H 1.1402 0.6264 0.7993 0.035 Uiso 1 1 calc R . .
H86B H 1.1831 0.6690 0.7439 0.035 Uiso 1 1 calc R . .
C87 C 1.1883(7) 0.8593(7) 0.7574(3) 0.035(2) Uani 1 1 d . . .
H87A H 1.1901 0.8400 0.7194 0.042 Uiso 1 1 calc R . .
H87B H 1.1539 0.9039 0.7601 0.042 Uiso 1 1 calc R . .
C88 C 1.2965(8) 0.9526(8) 0.8406(4) 0.055(3) Uani 1 1 d . . .
H88A H 1.2623 0.9973 0.8431 0.066 Uiso 1 1 calc R . .
H88B H 1.3692 0.9942 0.8579 0.066 Uiso 1 1 calc R . .
C89 C 1.3560(7) 0.8533(8) 0.7796(3) 0.041(3) Uani 1 1 d . . .
H89A H 1.3591 0.8321 0.7421 0.050 Uiso 1 1 calc R . .
H89B H 1.4294 0.8941 0.7962 0.050 Uiso 1 1 calc R . .
C90 C 1.3017(7) 0.9218(7) 0.7832(4) 0.043(3) Uani 1 1 d . . .
H90 H 1.3429 0.9868 0.7651 0.052 Uiso 1 1 calc R . .
K1 K 0.5000 0.0000 0.5000 0.0415(8) Uani 1 2 d S . .
O91 O 0.3277(6) 0.0168(6) 0.4581(3) 0.062(2) Uani 1 1 d . . .
O92 O 0.4805(6) 0.0169(6) 0.3919(3) 0.065(2) Uani 1 1 d . . .
O93 O 0.6657(6) 0.0377(6) 0.4392(3) 0.065(2) Uani 1 1 d . . .
C91 C 0.3149(10) 0.0029(10) 0.4022(4) 0.075(4) Uani 1 1 d . . .
H91A H 0.2686 0.0310 0.3899 0.091 Uiso 1 1 calc R . .
H91B H 0.2799 -0.0734 0.3899 0.091 Uiso 1 1 calc R . .
C92 C 0.4153(9) 0.0564(10) 0.3798(4) 0.069(4) Uani 1 1 d . . .
H92A H 0.4030 0.0501 0.3409 0.083 Uiso 1 1 calc R . .
H92B H 0.4506 0.1324 0.3929 0.083 Uiso 1 1 calc R . .
C93 C 0.5781(9) 0.0609(9) 0.3670(4) 0.065(4) Uani 1 1 d . . .
H93A H 0.6155 0.1388 0.3746 0.078 Uiso 1 1 calc R . .
H93B H 0.5631 0.0435 0.3282 0.078 Uiso 1 1 calc R . .
C94 C 0.6479(10) 0.0183(10) 0.3866(5) 0.079(4) Uani 1 1 d . . .
H94A H 0.6132 -0.0588 0.3764 0.095 Uiso 1 1 calc R . .
H94B H 0.7162 0.0520 0.3702 0.095 Uiso 1 1 calc R . .
C95 C 0.7457(7) 0.0127(8) 0.4591(4) 0.050(3) Uani 1 1 d U . .
H95A H 0.7238 -0.0624 0.4484 0.060 Uiso 1 1 calc R . .
H95B H 0.8143 0.0573 0.4445 0.060 Uiso 1 1 calc R . .
C96 C 0.7558(10) 0.0325(10) 0.5152(5) 0.083(5) Uani 1 1 d . . .
H96A H 0.8105 0.0157 0.5286 0.099 Uiso 1 1 calc R . .
H96B H 0.7840 0.1093 0.5241 0.099 Uiso 1 1 calc R . .
K2 K 0.5000 0.5000 1.0000 0.0485(9) Uani 1 2 d S . .
O101 O 0.5079(5) 0.6883(5) 1.0396(3) 0.0475(19) Uani 1 1 d . . .
O102 O 0.3521(5) 0.5541(6) 0.9600(2) 0.0509(19) Uani 1 1 d . . .
O103 O 0.3750(5) 0.3894(6) 0.9079(2) 0.0496(19) Uani 1 1 d . . .
C101 C 0.4140(9) 0.6914(8) 1.0315(4) 0.053(3) Uani 1 1 d . . .
H10J H 0.4259 0.7635 1.0421 0.064 Uiso 1 1 calc R . .
H10K H 0.3596 0.6419 1.0532 0.064 Uiso 1 1 calc R . .
C102 C 0.3767(9) 0.6604(8) 0.9739(4) 0.063(3) Uani 1 1 d . . .
H10F H 0.3131 0.6679 0.9668 0.075 Uiso 1 1 calc R . .
H10G H 0.4329 0.7077 0.9523 0.075 Uiso 1 1 calc R . .
C103 C 0.3248(9) 0.5231(10) 0.9055(4) 0.067(4) Uani 1 1 d . . .
H10D H 0.3870 0.5635 0.8853 0.080 Uiso 1 1 calc R . .
H10E H 0.2675 0.5376 0.8938 0.080 Uiso 1 1 calc R . .
C104 C 0.2883(9) 0.4076(10) 0.8955(4) 0.065(4) Uani 1 1 d . . .
H10N H 0.2295 0.3678 0.9176 0.077 Uiso 1 1 calc R . .
H10O H 0.2621 0.3828 0.8579 0.077 Uiso 1 1 calc R . .
C105 C 0.3508(9) 0.2837(9) 0.9002(4) 0.062(3) Uani 1 1 d . . .
H10L H 0.3154 0.2530 0.8643 0.074 Uiso 1 1 calc R . .
H10M H 0.3014 0.2432 0.9262 0.074 Uiso 1 1 calc R . .
C106 C 0.4484(9) 0.2755(9) 0.9061(4) 0.060(3) Uani 1 1 d . . .
H10H H 0.4319 0.2012 0.8975 0.072 Uiso 1 1 calc R . .
H10I H 0.5002 0.3196 0.8818 0.072 Uiso 1 1 calc R . .
C111 C 0.5344(14) -0.0068(17) 0.9986(8) 0.055(6) Uani 0.50 1 d PDU . .
H11F H 0.5027 -0.0742 0.9753 0.066 Uiso 0.50 1 calc PR . .
H11G H 0.5403 -0.0271 1.0343 0.066 Uiso 0.50 1 calc PR . .
C112 C 0.6340(15) 0.0370(15) 0.9867(7) 0.053(6) Uani 0.50 1 d PDU . .
H11A H 0.6665 0.1078 1.0068 0.064 Uiso 0.50 1 calc PR . .
H11B H 0.6294 0.0498 0.9492 0.064 Uiso 0.50 1 calc PR . .
C113 C 0.7108(14) 0.0123(17) 0.9889(7) 0.070(7) Uani 0.50 1 d PDU . .
H11H H 0.7792 0.0769 0.9967 0.105 Uiso 0.50 1 calc PR . .
H11I H 0.7108 -0.0240 0.9548 0.105 Uiso 0.50 1 calc PR . .
H11J H 0.6993 -0.0343 1.0167 0.105 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 1 1 0.0403 0.0000 1.0000 1.0000 0.0260 -0.0574 0.0168
0 -1 -1 0.0320 -0.0000 -1.0000 -1.0000 -0.0260 0.0574 -0.0168
-1 1 1 0.0505 -1.0000 1.0000 1.0000 0.0132 -0.0221 0.0586
1 -1 -1 0.0335 1.0000 -1.0000 -1.0000 -0.0132 0.0221 -0.0586
-1 -1 0 0.0264 -1.0000 -1.0000 0.0000 -0.0548 0.0718 0.0348
1 1 0 0.0524 1.0000 1.0000 -0.0000 0.0548 -0.0718 -0.0348
0 0 1 0.0010 0.0000 -0.0000 1.0000 -0.0159 -0.0209 0.0098
0 0 -1 0.0270 -0.0000 0.0000 -1.0000 0.0159 0.0209 -0.0098
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
N1 U1 O61 178.1(2) . .
N1 U1 O21 92.5(2) . .
O61 U1 O21 88.0(2) . .
N1 U1 O41 91.8(2) . .
O61 U1 O41 89.63(19) . .
O21 U1 O41 114.34(17) . .
N1 U1 O1 91.5(2) . .
O61 U1 O1 86.71(18) . .
O21 U1 O1 121.93(17) . .
O41 U1 O1 123.39(17) . .
O1 Si1 O2 114.5(3) . .
O1 Si1 O3 115.8(3) . .
O2 Si1 O3 100.9(3) . .
O1 Si1 O4 108.4(3) . .
O2 Si1 O4 109.3(3) . .
O3 Si1 O4 107.6(3) . .
Si1 O1 U1 159.6(3) . .
C1 O2 Si1 133.2(5) . .
C5 O3 Si1 133.8(5) . .
C9 O4 Si1 133.9(5) . .
O2 C1 C4 105.9(7) . .
O2 C1 C2 110.7(7) . .
C4 C1 C2 110.3(8) . .
O2 C1 C3 110.8(6) . .
C4 C1 C3 109.5(7) . .
C2 C1 C3 109.5(8) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O3 C5 C8 110.0(6) . .
O3 C5 C7 106.4(7) . .
C8 C5 C7 110.7(8) . .
O3 C5 C6 109.0(8) . .
C8 C5 C6 108.9(8) . .
C7 C5 C6 111.7(6) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O4 C9 C11 109.9(7) . .
O4 C9 C10 106.0(6) . .
C11 C9 C10 110.1(9) . .
O4 C9 C12 110.4(8) . .
C11 C9 C12 110.9(8) . .
C10 C9 C12 109.5(8) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11C 109.5 . .
C9 C11 H11D 109.5 . .
H11C C11 H11D 109.5 . .
C9 C11 H11E 109.5 . .
H11C C11 H11E 109.5 . .
H11D C11 H11E 109.5 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O21 Si2 O24 114.0(3) . .
O21 Si2 O22 108.6(3) . .
O24 Si2 O22 110.0(3) . .
O21 Si2 O23 114.2(3) . .
O24 Si2 O23 103.8(3) . .
O22 Si2 O23 105.9(3) . .
Si2 O21 U1 155.0(4) . .
C21 O22 Si2 133.1(5) . .
C25 O23 Si2 131.9(6) . .
C29 O24 Si2 133.1(5) . .
O22 C21 C23 114.4(7) . .
O22 C21 C24 106.0(7) . .
C23 C21 C24 110.5(9) . .
O22 C21 C22 106.1(8) . .
C23 C21 C22 110.8(9) . .
C24 C21 C22 108.7(8) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C21 C24 H24A 109.5 . .
C21 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C21 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
O23 C25 C28 110.7(7) . .
O23 C25 C27 108.2(7) . .
C28 C25 C27 110.1(9) . .
O23 C25 C26 105.1(8) . .
C28 C25 C26 111.4(9) . .
C27 C25 C26 111.1(9) . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C25 C27 H27A 109.5 . .
C25 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C25 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C25 C28 H28A 109.5 . .
C25 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C25 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
O24 C29 C30 105.5(8) . .
O24 C29 C31 108.1(8) . .
C30 C29 C31 110.7(11) . .
O24 C29 C32 112.2(8) . .
C30 C29 C32 111.1(9) . .
C31 C29 C32 109.2(8) . .
C29 C30 H30A 109.5 . .
C29 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C29 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C29 C31 H31A 109.5 . .
C29 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C29 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C29 C32 H32A 109.5 . .
C29 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C29 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
O44 Si3 O41 116.1(4) . .
O44 Si3 O42 114.7(3) . .
O41 Si3 O42 110.6(3) . .
O44 Si3 O43 100.8(4) . .
O41 Si3 O43 113.0(3) . .
O42 Si3 O43 100.2(4) . .
Si3 O41 U1 159.2(3) . .
C41 O42 Si3 133.0(6) . .
C45 O43 Si3 127.8(8) . .
C49 O44 Si3 128.5(5) . .
O42 C41 C44 113.2(9) . .
O42 C41 C42 105.7(8) . .
C44 C41 C42 110.7(11) . .
O42 C41 C43 110.0(8) . .
C44 C41 C43 109.7(10) . .
C42 C41 C43 107.3(10) . .
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 . .
C41 C43 H43A 109.5 . .
C41 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C41 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C41 C44 H44A 109.5 . .
C41 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C41 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
O43 C45 C48 114.3(8) . .
O43 C45 C47 111.1(8) . .
C48 C45 C47 112.2(12) . .
O43 C45 C46 100.8(10) . .
C48 C45 C46 113.0(10) . .
C47 C45 C46 104.4(8) . .
C45 C46 H46A 109.5 . .
C45 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
C45 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C45 C47 H47A 109.5 . .
C45 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
C45 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C45 C48 H48A 109.5 . .
C45 C48 H48B 109.5 . .
H48A C48 H48B 109.5 . .
C45 C48 H48C 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
C50 C49 C52 111.4(10) . .
C50 C49 C51 115.1(10) . .
C52 C49 C51 111.2(9) . .
C50 C49 O44 111.1(10) . .
C52 C49 O44 102.4(8) . .
C51 C49 O44 104.8(9) . .
C49 C50 H50A 109.5 . .
C49 C50 H50B 109.5 . .
H50A C50 H50B 109.5 . .
C49 C50 H50C 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
C49 C51 H51A 109.5 . .
C49 C51 H51B 109.5 . .
H51A C51 H51B 109.5 . .
C49 C51 H51C 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
C49 C52 H52A 109.5 . .
C49 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
C49 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
O64B Si4 O62 66.5(8) . .
O64B Si4 O63 122.6(9) . .
O62 Si4 O63 118.1(5) . .
O64B Si4 O61 119.8(8) . .
O62 Si4 O61 117.1(4) . .
O63 Si4 O61 107.8(3) . .
O64B Si4 O64 37.7(7) . .
O62 Si4 O64 103.3(5) . .
O63 Si4 O64 98.7(4) . .
O61 Si4 O64 109.9(4) . .
O64B Si4 O62B 103.8(9) . .
O62 Si4 O62B 38.6(5) . .
O63 Si4 O62B 89.9(7) . .
O61 Si4 O62B 107.2(7) . .
O64 Si4 O62B 137.1(7) . .
Si4 O61 U1 171.0(3) . .
C61 O62B Si4 126.9(14) . .
C61 O62 Si4 136.2(8) . .
C65 O63 Si4 134.4(6) . .
C69 O64B Si4 134.9(16) . .
C69 O64 Si4 127.9(9) . .
O62B C61 C64 131.0(12) . .
O62B C61 O62 45.2(7) . .
C64 C61 O62 95.6(9) . .
O62B C61 C63 79.5(11) . .
C64 C61 C63 109.4(10) . .
O62 C61 C63 119.8(9) . .
O62B C61 C62 107.8(10) . .
C64 C61 C62 111.8(9) . .
O62 C61 C62 106.3(8) . .
C63 C61 C62 112.8(8) . .
C61 C62 H62A 109.5 . .
C61 C62 H62B 109.5 . .
H62A C62 H62B 109.5 . .
C61 C62 H62C 109.5 . .
H62A C62 H62C 109.5 . .
H62B C62 H62C 109.5 . .
C61 C63 H63A 109.5 . .
C61 C63 H63B 109.5 . .
H63A C63 H63B 109.5 . .
C61 C63 H63C 109.5 . .
H63A C63 H63C 109.5 . .
H63B C63 H63C 109.5 . .
C61 C64 H64A 109.5 . .
C61 C64 H64B 109.5 . .
H64A C64 H64B 109.5 . .
C61 C64 H64C 109.5 . .
H64A C64 H64C 109.5 . .
H64B C64 H64C 109.5 . .
O63 C65 C66 105.7(7) . .
O63 C65 C68 107.9(8) . .
C66 C65 C68 110.0(8) . .
O63 C65 C67 113.3(7) . .
C66 C65 C67 109.0(7) . .
C68 C65 C67 110.9(8) . .
C65 C66 H66A 109.5 . .
C65 C66 H66B 109.5 . .
H66A C66 H66B 109.5 . .
C65 C66 H66C 109.5 . .
H66A C66 H66C 109.5 . .
H66B C66 H66C 109.5 . .
C65 C67 H67A 109.5 . .
C65 C67 H67B 109.5 . .
H67A C67 H67B 109.5 . .
C65 C67 H67C 109.5 . .
H67A C67 H67C 109.5 . .
H67B C67 H67C 109.5 . .
C65 C68 H68A 109.5 . .
C65 C68 H68B 109.5 . .
H68A C68 H68B 109.5 . .
C65 C68 H68C 109.5 . .
H68A C68 H68C 109.5 . .
H68B C68 H68C 109.5 . .
O64 C69 C71 100.2(11) . .
O64 C69 C72 113.4(10) . .
C71 C69 C72 108.8(13) . .
O64 C69 O64B 43.2(7) . .
C71 C69 O64B 142.7(14) . .
C72 C69 O64B 95.9(12) . .
O64 C69 C70 118.9(10) . .
C71 C69 C70 106.2(12) . .
C72 C69 C70 108.5(11) . .
O64B C69 C70 91.2(12) . .
C69 C70 H70A 109.5 . .
C69 C70 H70B 109.5 . .
H70A C70 H70B 109.5 . .
C69 C70 H70C 109.5 . .
H70A C70 H70C 109.5 . .
H70B C70 H70C 109.5 . .
C69 C71 H71A 109.5 . .
C69 C71 H71B 109.5 . .
H71A C71 H71B 109.5 . .
C69 C71 H71C 109.5 . .
H71A C71 H71C 109.5 . .
H71B C71 H71C 109.5 . .
C69 C72 H72A 109.5 . .
C69 C72 H72B 109.5 . .
H72A C72 H72B 109.5 . .
C69 C72 H72C 109.5 . .
H72A C72 H72C 109.5 . .
H72B C72 H72C 109.5 . .
C81 N1 U1 172.3(5) . .
N1 C81 C82 111.3(6) . .
N1 C81 C87 110.0(6) . .
C82 C81 C87 108.5(7) . .
N1 C81 C86 109.8(7) . .
C82 C81 C86 108.3(7) . .
C87 C81 C86 108.9(6) . .
C81 C82 C83 110.0(7) . .
C81 C82 H82A 109.7 . .
C83 C82 H82A 109.7 . .
C81 C82 H82B 109.7 . .
C83 C82 H82B 109.7 . .
H82A C82 H82B 108.2 . .
C88 C83 C84 108.9(8) . .
C88 C83 C82 109.7(8) . .
C84 C83 C82 109.8(8) . .
C88 C83 H83 109.4 . .
C84 C83 H83 109.4 . .
C82 C83 H83 109.4 . .
C85 C84 C83 108.5(7) . .
C85 C84 H84A 110.0 . .
C83 C84 H84A 110.0 . .
C85 C84 H84B 110.0 . .
C83 C84 H84B 110.0 . .
H84A C84 H84B 108.4 . .
C84 C85 C89 110.6(8) . .
C84 C85 C86 110.0(7) . .
C89 C85 C86 110.2(7) . .
C84 C85 H85 108.7 . .
C89 C85 H85 108.7 . .
C86 C85 H85 108.7 . .
C85 C86 C81 109.5(7) . .
C85 C86 H86A 109.8 . .
C81 C86 H86A 109.8 . .
C85 C86 H86B 109.8 . .
C81 C86 H86B 109.8 . .
H86A C86 H86B 108.2 . .
C90 C87 C81 110.6(7) . .
C90 C87 H87A 109.5 . .
C81 C87 H87A 109.5 . .
C90 C87 H87B 109.5 . .
C81 C87 H87B 109.5 . .
H87A C87 H87B 108.1 . .
C90 C88 C83 110.4(8) . .
C90 C88 H88A 109.6 . .
C83 C88 H88A 109.6 . .
C90 C88 H88B 109.6 . .
C83 C88 H88B 109.6 . .
H88A C88 H88B 108.1 . .
C85 C89 C90 108.7(7) . .
C85 C89 H89A 110.0 . .
C90 C89 H89A 110.0 . .
C85 C89 H89B 110.0 . .
C90 C89 H89B 110.0 . .
H89A C89 H89B 108.3 . .
C88 C90 C87 108.3(7) . .
C88 C90 C89 109.3(7) . .
C87 C90 C89 110.2(8) . .
C88 C90 H90 109.7 . .
C87 C90 H90 109.7 . .
C89 C90 H90 109.7 . .
O93 K1 O93 180.000(1) . 2_656
O93 K1 O92 59.9(2) . .
O93 K1 O92 120.1(2) 2_656 .
O93 K1 O92 120.1(2) . 2_656
O93 K1 O92 59.9(2) 2_656 2_656
O92 K1 O92 180.00(4) . 2_656
O93 K1 O91 119.4(2) . .
O93 K1 O91 60.6(2) 2_656 .
O92 K1 O91 60.4(2) . .
O92 K1 O91 119.6(2) 2_656 .
O93 K1 O91 60.6(2) . 2_656
O93 K1 O91 119.4(2) 2_656 2_656
O92 K1 O91 119.6(2) . 2_656
O92 K1 O91 60.4(2) 2_656 2_656
O91 K1 O91 180.0(3) . 2_656
O93 K1 C96 138.4(3) . 2_656
O93 K1 C96 41.6(3) 2_656 2_656
O92 K1 C96 78.5(3) . 2_656
O92 K1 C96 101.5(3) 2_656 2_656
O91 K1 C96 20.5(2) . 2_656
O91 K1 C96 159.5(2) 2_656 2_656
O93 K1 C96 41.6(3) . .
O93 K1 C96 138.4(3) 2_656 .
O92 K1 C96 101.5(3) . .
O92 K1 C96 78.5(3) 2_656 .
O91 K1 C96 159.5(2) . .
O91 K1 C96 20.5(2) 2_656 .
C96 K1 C96 180.000(1) 2_656 .
C96 O91 C91 118.9(11) 2_656 .
C96 O91 K1 111.2(7) 2_656 .
C91 O91 K1 113.8(6) . .
C92 O92 C93 115.4(9) . .
C92 O92 K1 113.0(6) . .
C93 O92 K1 114.8(6) . .
C94 O93 C95 112.1(8) . .
C94 O93 K1 119.5(7) . .
C95 O93 K1 117.7(6) . .
O91 C91 C92 111.2(10) . .
O91 C91 H91A 109.4 . .
C92 C91 H91A 109.4 . .
O91 C91 H91B 109.4 . .
C92 C91 H91B 109.4 . .
H91A C91 H91B 108.0 . .
O92 C92 C91 112.8(11) . .
O92 C92 H92A 109.0 . .
C91 C92 H92A 109.0 . .
O92 C92 H92B 109.0 . .
C91 C92 H92B 109.0 . .
H92A C92 H92B 107.8 . .
O92 C93 C94 110.9(9) . .
O92 C93 H93A 109.5 . .
C94 C93 H93A 109.5 . .
O92 C93 H93B 109.5 . .
C94 C93 H93B 109.5 . .
H93A C93 H93B 108.1 . .
O93 C94 C93 110.2(10) . .
O93 C94 H94A 109.6 . .
C93 C94 H94A 109.6 . .
O93 C94 H94B 109.6 . .
C93 C94 H94B 109.6 . .
H94A C94 H94B 108.1 . .
C96 C95 O93 107.6(8) . .
C96 C95 H95A 110.2 . .
O93 C95 H95A 110.2 . .
C96 C95 H95B 110.2 . .
O93 C95 H95B 110.2 . .
H95A C95 H95B 108.5 . .
O91 C96 C95 119.5(12) 2_656 .
O91 C96 K1 48.3(6) 2_656 .
C95 C96 K1 84.7(7) . .
O91 C96 H96A 107.5 2_656 .
C95 C96 H96A 107.5 . .
K1 C96 H96A 154.9 . .
O91 C96 H96B 107.5 2_656 .
C95 C96 H96B 107.5 . .
K1 C96 H96B 89.3 . .
H96A C96 H96B 107.0 . .
O103 K2 O103 180.000(2) . 2_667
O103 K2 O101 119.5(2) . .
O103 K2 O101 60.5(2) 2_667 .
O103 K2 O101 60.5(2) . 2_667
O103 K2 O101 119.5(2) 2_667 2_667
O101 K2 O101 180.000(2) . 2_667
O103 K2 O102 60.6(2) . .
O103 K2 O102 119.4(2) 2_667 .
O101 K2 O102 60.1(2) . .
O101 K2 O102 119.9(2) 2_667 .
O103 K2 O102 119.4(2) . 2_667
O103 K2 O102 60.6(2) 2_667 2_667
O101 K2 O102 119.9(2) . 2_667
O101 K2 O102 60.1(2) 2_667 2_667
O102 K2 O102 180.000(4) . 2_667
C101 O101 C106 111.0(7) . 2_667
C101 O101 K2 115.0(6) . .
C106 O101 K2 114.7(5) 2_667 .
C103 O102 C102 112.4(8) . .
C103 O102 K2 112.8(5) . .
C102 O102 K2 115.2(6) . .
C105 O103 C104 114.7(9) . .
C105 O103 K2 114.6(6) . .
C104 O103 K2 116.0(5) . .
O101 C101 C102 108.5(8) . .
O101 C101 H10J 110.0 . .
C102 C101 H10J 110.0 . .
O101 C101 H10K 110.0 . .
C102 C101 H10K 110.0 . .
H10J C101 H10K 108.4 . .
O102 C102 C101 109.7(8) . .
O102 C102 H10F 109.7 . .
C101 C102 H10F 109.7 . .
O102 C102 H10G 109.7 . .
C101 C102 H10G 109.7 . .
H10F C102 H10G 108.2 . .
O102 C103 C104 108.6(9) . .
O102 C103 H10D 110.0 . .
C104 C103 H10D 110.0 . .
O102 C103 H10E 110.0 . .
C104 C103 H10E 110.0 . .
H10D C103 H10E 108.3 . .
O103 C104 C103 109.2(9) . .
O103 C104 H10N 109.8 . .
C103 C104 H10N 109.8 . .
O103 C104 H10O 109.8 . .
C103 C104 H10O 109.8 . .
H10N C104 H10O 108.3 . .
O103 C105 C106 110.3(9) . .
O103 C105 H10L 109.6 . .
C106 C105 H10L 109.6 . .
O103 C105 H10M 109.6 . .
C106 C105 H10M 109.6 . .
H10L C105 H10M 108.1 . .
O101 C106 C105 107.8(8) 2_667 .
O101 C106 H10H 110.1 2_667 .
C105 C106 H10H 110.1 . .
O101 C106 H10I 110.1 2_667 .
C105 C106 H10I 110.1 . .
H10H C106 H10I 108.5 . .
C111 C111 C112 143(3) 2_657 .
C111 C111 H11F 101.1 2_657 .
C112 C111 H11F 101.1 . .
C111 C111 H11G 101.1 2_657 .
C112 C111 H11G 101.1 . .
H11F C111 H11G 104.5 . .
C111 C112 C113 136(2) . .
C111 C112 H11A 103.1 . .
C113 C112 H11A 103.1 . .
C111 C112 H11B 103.1 . .
C113 C112 H11B 103.1 . .
H11A C112 H11B 105.1 . .
C112 C113 H11H 109.5 . .
C112 C113 H11I 109.5 . .
H11H C113 H11I 109.5 . .
C112 C113 H11J 109.5 . .
H11H C113 H11J 109.5 . .
H11I C113 H11J 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 1.937(7) .
U1 O61 2.180(6) .
U1 O21 2.200(5) .
U1 O41 2.201(4) .
U1 O1 2.236(4) .
Si1 O1 1.587(5) .
Si1 O2 1.623(6) .
Si1 O3 1.628(5) .
Si1 O4 1.640(6) .
O2 C1 1.434(8) .
O3 C5 1.412(9) .
O4 C9 1.430(8) .
C1 C4 1.512(12) .
C1 C2 1.516(11) .
C1 C3 1.533(10) .
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 C8 1.499(11) .
C5 C7 1.521(9) .
C5 C6 1.521(12) .
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 C11 1.502(12) .
C9 C10 1.516(11) .
C9 C12 1.528(12) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11C 0.9800 .
C11 H11D 0.9800 .
C11 H11E 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
Si2 O21 1.592(5) .
Si2 O24 1.624(7) .
Si2 O22 1.626(6) .
Si2 O23 1.627(6) .
O22 C21 1.445(9) .
O23 C25 1.454(9) .
O24 C29 1.440(10) .
C21 C23 1.477(11) .
C21 C24 1.493(13) .
C21 C22 1.515(11) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C25 C28 1.510(12) .
C25 C27 1.525(12) .
C25 C26 1.532(13) .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 C30 1.489(12) .
C29 C31 1.494(13) .
C29 C32 1.512(11) .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
Si3 O44 1.563(7) .
Si3 O41 1.582(5) .
Si3 O42 1.603(6) .
Si3 O43 1.694(7) .
O42 C41 1.431(10) .
O43 C45 1.413(10) .
O44 C49 1.549(12) .
C41 C44 1.469(13) .
C41 C42 1.493(13) .
C41 C43 1.504(14) .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 C48 1.483(14) .
C45 C47 1.533(12) .
C45 C46 1.590(15) .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
C49 C50 1.413(14) .
C49 C52 1.498(11) .
C49 C51 1.520(13) .
C50 H50A 0.9800 .
C50 H50B 0.9800 .
C50 H50C 0.9800 .
C51 H51A 0.9800 .
C51 H51B 0.9800 .
C51 H51C 0.9800 .
C52 H52A 0.9800 .
C52 H52B 0.9800 .
C52 H52C 0.9800 .
Si4 O64B 1.525(18) .
Si4 O62 1.584(8) .
Si4 O63 1.592(6) .
Si4 O61 1.593(6) .
Si4 O64 1.716(10) .
Si4 O62B 1.763(17) .
O62B C61 1.421(18) .
O62 C61 1.489(12) .
O63 C65 1.434(10) .
O64B C69 1.491(19) .
O64 C69 1.380(11) .
C61 C64 1.481(12) .
C61 C63 1.489(12) .
C61 C62 1.502(11) .
C62 H62A 0.9800 .
C62 H62B 0.9800 .
C62 H62C 0.9800 .
C63 H63A 0.9800 .
C63 H63B 0.9800 .
C63 H63C 0.9800 .
C64 H64A 0.9800 .
C64 H64B 0.9800 .
C64 H64C 0.9800 .
C65 C66 1.515(11) .
C65 C68 1.528(12) .
C65 C67 1.535(11) .
C66 H66A 0.9800 .
C66 H66B 0.9800 .
C66 H66C 0.9800 .
C67 H67A 0.9800 .
C67 H67B 0.9800 .
C67 H67C 0.9800 .
C68 H68A 0.9800 .
C68 H68B 0.9800 .
C68 H68C 0.9800 .
C69 C71 1.450(15) .
C69 C72 1.473(15) .
C69 C70 1.497(14) .
C70 H70A 0.9800 .
C70 H70B 0.9800 .
C70 H70C 0.9800 .
C71 H71A 0.9800 .
C71 H71B 0.9800 .
C71 H71C 0.9800 .
C72 H72A 0.9800 .
C72 H72B 0.9800 .
C72 H72C 0.9800 .
N1 C81 1.461(10) .
C81 C82 1.517(10) .
C81 C87 1.543(11) .
C81 C86 1.551(10) .
C82 C83 1.541(12) .
C82 H82A 0.9900 .
C82 H82B 0.9900 .
C83 C88 1.525(12) .
C83 C84 1.529(11) .
C83 H83 1.0000 .
C84 C85 1.515(10) .
C84 H84A 0.9900 .
C84 H84B 0.9900 .
C85 C89 1.518(11) .
C85 C86 1.534(11) .
C85 H85 1.0000 .
C86 H86A 0.9900 .
C86 H86B 0.9900 .
C87 C90 1.532(11) .
C87 H87A 0.9900 .
C87 H87B 0.9900 .
C88 C90 1.509(11) .
C88 H88A 0.9900 .
C88 H88B 0.9900 .
C89 C90 1.536(11) .
C89 H89A 0.9900 .
C89 H89B 0.9900 .
C90 H90 1.0000 .
K1 O93 2.743(6) .
K1 O93 2.743(6) 2_656
K1 O92 2.799(7) .
K1 O92 2.799(7) 2_656
K1 O91 2.803(7) .
K1 O91 2.803(7) 2_656
K1 C96 3.499(12) 2_656
K1 C96 3.499(12) .
O91 C96 1.312(11) 2_656
O91 C91 1.415(11) .
O92 C92 1.357(11) .
O92 C93 1.430(10) .
O93 C94 1.336(11) .
O93 C95 1.457(10) .
C91 C92 1.437(13) .
C91 H91A 0.9900 .
C91 H91B 0.9900 .
C92 H92A 0.9900 .
C92 H92B 0.9900 .
C93 C94 1.507(13) .
C93 H93A 0.9900 .
C93 H93B 0.9900 .
C94 H94A 0.9900 .
C94 H94B 0.9900 .
C95 C96 1.424(13) .
C95 H95A 0.9900 .
C95 H95B 0.9900 .
C96 O91 1.312(11) 2_656
C96 H96A 0.9900 .
C96 H96B 0.9900 .
K2 O103 2.773(6) .
K2 O103 2.773(6) 2_667
K2 O101 2.791(6) .
K2 O101 2.791(6) 2_667
K2 O102 2.799(6) .
K2 O102 2.799(6) 2_667
O101 C101 1.390(10) .
O101 C106 1.449(11) 2_667
O102 C103 1.407(11) .
O102 C102 1.420(10) .
O103 C105 1.397(11) .
O103 C104 1.430(10) .
C101 C102 1.502(13) .
C101 H10J 0.9900 .
C101 H10K 0.9900 .
C102 H10F 0.9900 .
C102 H10G 0.9900 .
C103 C104 1.494(14) .
C103 H10D 0.9900 .
C103 H10E 0.9900 .
C104 H10N 0.9900 .
C104 H10O 0.9900 .
C105 C106 1.477(13) .
C105 H10L 0.9900 .
C105 H10M 0.9900 .
C106 O101 1.449(11) 2_667
C106 H10H 0.9900 .
C106 H10I 0.9900 .
C111 C111 1.11(3) 2_657
C111 C112 1.319(15) .
C111 H11F 0.9900 .
C111 H11G 0.9900 .
C112 C113 1.323(15) .
C112 H11A 0.9900 .
C112 H11B 0.9900 .
C113 H11H 0.9800 .
C113 H11I 0.9800 .
C113 H11J 0.9800 .
