#------------------------------------------------------------------------------
#$Date: 2022-08-06 14:40:09 +0300 (Sat, 06 Aug 2022) $
#$Revision: 277096 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/72/1567208.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_1567208
loop_
_publ_author_name
'Keener, Megan'
'Fadaei-Tirani, Farzaneh'
'Scopelliti, Rosario'
'Zivkovic, Ivica'
'Mazzanti, Marinella'
_publ_section_title
;
 Nitrogen activation and cleavage by a multimetallic uranium complex.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              8025
_journal_page_last               8035
_journal_paper_doi               10.1039/d2sc02997a
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C48 H126 N5 O8 Si10 U2, 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C84 H198 K2 N9 O20 Si10 U2'
_chemical_formula_weight         2489.66
_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_date             2022-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-24 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                106.635(2)
_cell_angle_beta                 103.811(2)
_cell_angle_gamma                95.243(2)
_cell_formula_units_Z            1
_cell_length_a                   13.8976(4)
_cell_length_b                   14.7410(4)
_cell_length_c                   18.5692(4)
_cell_measurement_reflns_used    22776
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      75.6210
_cell_measurement_theta_min      4.1460
_cell_volume                     3487.04(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_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 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -11.00   1.00    2.00    --  -40.91 -67.00 -61.00  103
  2  ω    -60.00  24.00   1.00    2.00    --  -40.91  67.00  72.00   84
  3  ω     38.00  63.00   1.00    2.00    --   40.91  67.00  72.00   25
  4  ω     98.00 125.00   1.00    8.00    --  112.00  67.00  72.00   27
  5  ω    103.00 140.00   1.00    8.00    --  112.00 -67.00 -61.00   37
  6  ω     50.00  91.00   1.00    8.00    --  112.00 -67.00 -61.00   41
  7  ω   -115.00 -18.00   1.00    2.00    --  -40.91 -38.00-180.00   97
  8  ω    -29.00   6.00   1.00    2.00    --   40.91 -57.00 150.00   35
  9  ω     -5.00  20.00   1.00    2.00    --   40.91 -67.00 -61.00   25
 10  ω     63.00  94.00   1.00    2.00    --   40.91-125.00-120.00   31
 11  ω     34.00  87.00   1.00    2.00    --   40.91-125.00-180.00   53
 12  ω     82.00 123.00   1.00    8.00    --  112.00 178.00-150.00   41
 13  ω     96.00 128.00   1.00    8.00    --  112.00  30.00-150.00   32
 14  ω    102.00 151.00   1.00    8.00    --  112.00  45.00   0.00   49
 15  ω     30.00  63.00   1.00    8.00    --  112.00 -94.00 -60.00   33
 16  ω     30.00 104.00   1.00    8.00    --  112.00 -94.00-150.00   74
 17  ω    129.00 178.00   1.00    8.00    --  112.00  30.00-150.00   49
 18  ω     84.00 111.00   1.00    8.00    --  112.00  61.00 150.00   27
 19  ω    113.00 178.00   1.00    8.00    --  112.00  61.00 150.00   65
 20  ω     50.00 109.00   1.00    8.00    --  112.00-111.00 120.00   59
 21  ω    104.00 177.00   1.00    8.00    --  112.00  77.00 -60.00   73
 22  ω     83.00 178.00   1.00    8.00    --  112.00  61.00  90.00   95
 23  ω     52.00  79.00   1.00    8.00    --  112.00 -94.00-180.00   27
 24  ω     76.00 109.00   1.00    8.00    --  112.00-111.00  60.00   33
 25  ω     29.00  71.00   1.00    8.00    --  112.00 -94.00-120.00   42
 26  ω     52.00 103.00   1.00    8.00    --  112.00-111.00  30.00   51
 27  ω     74.00 107.00   1.00    8.00    --  112.00-111.00  90.00   33
 28  ω     38.00 109.00   1.00    8.00    --  112.00-111.00 -30.00   71
 29  ω    105.00 175.00   1.00    8.00    --  112.00 111.00  30.00   70
 30  ω     63.00 109.00   1.00    8.00    --  112.00-111.00-150.00   46
 31  ω     47.00 107.00   1.00    8.00    --  112.00 -94.00 120.00   60
 32  ω     82.00 131.00   1.00    8.00    --  112.00 -45.00 -90.00   49
 33  ω    104.00 178.00   1.00    8.00    --  112.00  77.00-180.00   74
 34  ω    134.00 165.00   1.00    8.00    --  112.00  77.00  30.00   31
 35  ω     46.00 109.00   1.00    8.00    --  112.00-111.00   0.00   63
 36  ω    112.00 149.00   1.00    8.00    --  112.00  77.00  60.00   37
 37  ω     36.00 109.00   1.00    8.00    --  112.00-111.00 -90.00   73
 38  ω     78.00 109.00   1.00    8.00    --  112.00-111.00 -60.00   31
 39  ω    110.00 171.00   1.00    8.00    --  112.00 111.00 -90.00   61
 40  ω     46.00  71.00   1.00    8.00    --  112.00 -94.00 -90.00   25
 41  ω     61.00  86.00   1.00    8.00    --  112.00 -94.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0778982000
_diffrn_orient_matrix_UB_12      -0.0773405000
_diffrn_orient_matrix_UB_13      -0.0683794000
_diffrn_orient_matrix_UB_21      0.0791006000
_diffrn_orient_matrix_UB_22      -0.0664324000
_diffrn_orient_matrix_UB_23      -0.0061939000
_diffrn_orient_matrix_UB_31      -0.0331819000
_diffrn_orient_matrix_UB_32      -0.0431692000
_diffrn_orient_matrix_UB_33      0.0583897000
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41330
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.131
_diffrn_reflns_theta_min         3.176
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1287
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.296
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         14411
_refine_ls_number_restraints     922
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0592
_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)+(0.1043P)²+7.6578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13148
_reflns_number_total             14411
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-539
_cod_depositor_comments
'Adding full bibliography for 1567201--1567212.cif.'
_cod_original_cell_volume        3487.02(17)
_cod_database_code               1567208
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H60 N4 O20 Si8 K2 U2'
_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_max   0.264
_shelx_estimated_absorpt_t_min   0.119
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 K1-C47
 3.6 with sigma of 0.02
 K1-C45
 3.6 with sigma of 0.02
 C44-C43 \\sim C32-C31 \\sim C33-C34 \\sim C36-C35 \\sim C46-C45 \\sim C48-C47
\\sim C38-C37 \\sim C39-C40
 \\sim C41-C42
 with sigma of 0.02
 N4-C43 \\sim N4-C31 \\sim N4-C42 \\sim N5-C48 \\sim N5-C36 \\sim N5-C37
 with sigma of 0.02
 C43-C31 \\sim C31-C42
 with sigma of 0.02
 C48-C37 \\sim C37-C36
 with sigma of 0.02
 O6-C34 \\sim O6-C35 \\sim O5-C33 \\sim O5-C32 \\sim O7-C41 \\sim O7-C40 \\sim
O8-C39 \\sim O8-C38 \\sim O10-
 C47 \\sim O10-C46 \\sim O9-C45 \\sim O9-C44
 with sigma of 0.02
 C40-C41 \\sim C39-C38 \\sim C47-C46 \\sim C45-C44 \\sim C35-C34 \\sim C33-C32
 with sigma of 0.02
 C29-C28 \\sim C28-C30 \\sim C29-C30
 with sigma of 0.02
 Si5-C25 \\sim Si5-C26 \\sim Si5-C27 \\sim Si6-C29 \\sim Si6-C28 \\sim Si6-C30
 with sigma of 0.02
 C25-C27 \\sim C27-C26 \\sim C25-C26
 with sigma of 0.02
 C13-C14 \\sim C14-C15 \\sim C13-C15
 with sigma of 0.02
 C10-C12 \\sim C12-C11 \\sim C10-C11
 with sigma of 0.02
 C9-C10 \\sim C9-C13 \\sim C9-C12 \\sim C9-C15 \\sim C9-C11 \\sim C9-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C44) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C2) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: Si5(0.5) Si6(0.5) N1(0.5) H1(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C27(0.5) H27A(0.5) H27B(0.5)
 H27C(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 109 electrons were 
found in a volume of 800Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
1.35[C4H8O] per Asymmetric Unit 
which account for 108 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2022-01-14
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.587
_oxdiff_exptl_absorpt_empirical_full_min 0.484
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.44860(2) 0.42304(2) 0.38920(2) 0.03936(9) Uani 1 1 d . . . . .
Si1 Si 0.57188(14) 0.20951(13) 0.31509(11) 0.0471(4) Uani 1 1 d . . . . .
Si2 Si 0.5311(2) 0.5317(3) 0.2584(2) 0.0926(10) Uani 1 1 d . . . . .
Si3 Si 0.3571(3) 0.60047(17) 0.30894(14) 0.0745(7) Uani 1 1 d . . . . .
Si4 Si 0.22874(14) 0.26745(14) 0.25202(12) 0.0511(4) Uani 1 1 d . . . . .
Si5 Si 0.2223(3) 0.2920(3) 0.4125(3) 0.0525(8) Uani 0.5 1 d D . P A 1
Si6 Si 0.2556(3) 0.3584(4) 0.4323(3) 0.0593(10) Uani 0.5 1 d D . P A 2
O1 O 0.5306(4) 0.3002(3) 0.3582(3) 0.0524(10) Uani 1 1 d . . . . .
O2 O 0.4882(5) 0.1533(5) 0.2313(4) 0.0705(14) Uani 1 1 d . . . . .
O3 O 0.6755(4) 0.2333(4) 0.2920(4) 0.0591(11) Uani 1 1 d . . . . .
O4 O 0.5975(4) 0.1355(4) 0.3640(4) 0.0592(11) Uani 1 1 d . . . . .
N1 N 0.5737(10) 0.5165(9) 0.4850(7) 0.054(3) Uani 0.5 1 d . . P A 1
H1 H 0.631928 0.531519 0.476742 0.065 Uiso 0.5 1 calc R U P A 1
N2 N 0.4443(6) 0.5263(6) 0.3081(4) 0.0704(13) Uani 1 1 d . . . . .
N3 N 0.2867(4) 0.3266(5) 0.3481(4) 0.0525(11) Uani 1 1 d . . . . .
C1 C 0.4956(9) 0.0883(10) 0.1608(6) 0.093(2) Uani 1 1 d . . . . .
C2 C 0.3888(11) 0.0309(10) 0.1188(8) 0.112(3) Uani 1 1 d . U . . .
H2A H 0.366131 -0.001677 0.152467 0.168 Uiso 1 1 calc R U . . .
H2B H 0.389225 -0.016903 0.069797 0.168 Uiso 1 1 calc R U . . .
H2C H 0.342930 0.074850 0.107250 0.168 Uiso 1 1 calc R U . . .
C3 C 0.5289(13) 0.1411(13) 0.1123(8) 0.124(4) Uani 1 1 d . . . . .
H3A H 0.496337 0.197757 0.115532 0.186 Uiso 1 1 calc R U . . .
H3B H 0.510524 0.099205 0.057766 0.186 Uiso 1 1 calc R U . . .
H3C H 0.602074 0.161369 0.131199 0.186 Uiso 1 1 calc R U . . .
C4 C 0.5672(10) 0.0175(10) 0.1757(8) 0.109(3) Uani 1 1 d . . . . .
H4A H 0.631369 0.053456 0.212726 0.163 Uiso 1 1 calc R U . . .
H4B H 0.578900 -0.018671 0.126283 0.163 Uiso 1 1 calc R U . . .
H4C H 0.536893 -0.027096 0.197618 0.163 Uiso 1 1 calc R U . . .
C5 C 0.7766(7) 0.2645(7) 0.3393(6) 0.0702(17) Uani 1 1 d . . . . .
C6 C 0.8308(9) 0.3076(11) 0.2907(9) 0.103(3) Uani 1 1 d . . . . .
H6A H 0.828120 0.257529 0.242055 0.155 Uiso 1 1 calc R U . . .
H6B H 0.901096 0.333355 0.320680 0.155 Uiso 1 1 calc R U . . .
H6C H 0.797756 0.359413 0.278433 0.155 Uiso 1 1 calc R U . . .
C7 C 0.8233(8) 0.1776(9) 0.3512(8) 0.085(2) Uani 1 1 d . . . . .
H7A H 0.793586 0.152641 0.386082 0.128 Uiso 1 1 calc R U . . .
H7B H 0.896079 0.197298 0.374623 0.128 Uiso 1 1 calc R U . . .
H7C H 0.810052 0.127315 0.300601 0.128 Uiso 1 1 calc R U . . .
C8 C 0.7834(9) 0.3355(9) 0.4161(8) 0.097(3) Uani 1 1 d . . . . .
H8A H 0.742098 0.384159 0.408099 0.146 Uiso 1 1 calc R U . . .
H8B H 0.853573 0.366668 0.441826 0.146 Uiso 1 1 calc R U . . .
H8C H 0.759036 0.302706 0.448967 0.146 Uiso 1 1 calc R U . . .
C9 C 0.5418(6) 0.0911(6) 0.4051(5) 0.0690(17) Uani 1 1 d D . . . .
C10 C 0.4316(10) 0.0644(14) 0.3561(11) 0.077(4) Uani 0.499(14) 1 d D . P B 1
H10A H 0.390330 0.040198 0.384914 0.116 Uiso 0.499(14) 1 calc R U P B 1
H10B H 0.425510 0.014495 0.306492 0.116 Uiso 0.499(14) 1 calc R U P B 1
H10C H 0.408495 0.121383 0.345619 0.116 Uiso 0.499(14) 1 calc R U P B 1
C11 C 0.5582(13) 0.1542(12) 0.4858(9) 0.074(4) Uani 0.499(14) 1 d D . P B 1
H11A H 0.579349 0.220876 0.489082 0.111 Uiso 0.499(14) 1 calc R U P B 1
H11B H 0.610682 0.134897 0.521190 0.111 Uiso 0.499(14) 1 calc R U P B 1
H11C H 0.495567 0.148907 0.500971 0.111 Uiso 0.499(14) 1 calc R U P B 1
C12 C 0.5826(14) -0.0040(11) 0.4020(12) 0.080(5) Uani 0.499(14) 1 d D . P B 1
H12A H 0.542970 -0.042417 0.423494 0.120 Uiso 0.499(14) 1 calc R U P B 1
H12B H 0.653179 0.010595 0.432992 0.120 Uiso 0.499(14) 1 calc R U P B 1
H12C H 0.577472 -0.040268 0.347624 0.120 Uiso 0.499(14) 1 calc R U P B 1
C13 C 0.4787(16) -0.0017(12) 0.3572(13) 0.101(6) Uani 0.501(14) 1 d D . P B 2
H13A H 0.448565 -0.029827 0.390271 0.151 Uiso 0.501(14) 1 calc R U P B 2
H13B H 0.519939 -0.044995 0.333259 0.151 Uiso 0.501(14) 1 calc R U P B 2
H13C H 0.425308 0.007644 0.316120 0.151 Uiso 0.501(14) 1 calc R U P B 2
C14 C 0.4752(13) 0.1620(13) 0.4415(12) 0.081(5) Uani 0.501(14) 1 d D . P B 2
H14A H 0.429871 0.178712 0.399900 0.122 Uiso 0.501(14) 1 calc R U P B 2
H14B H 0.518791 0.220429 0.479563 0.122 Uiso 0.501(14) 1 calc R U P B 2
H14C H 0.435590 0.130899 0.467745 0.122 Uiso 0.501(14) 1 calc R U P B 2
C15 C 0.6223(12) 0.0841(13) 0.4756(10) 0.076(4) Uani 0.501(14) 1 d D . P B 2
H15A H 0.650679 0.148730 0.512454 0.113 Uiso 0.501(14) 1 calc R U P B 2
H15B H 0.675926 0.054021 0.457395 0.113 Uiso 0.501(14) 1 calc R U P B 2
H15C H 0.591598 0.045208 0.501704 0.113 Uiso 0.501(14) 1 calc R U P B 2
C16 C 0.6094(15) 0.4506(15) 0.2684(12) 0.144(4) Uani 1 1 d . U . . .
H16A H 0.602731 0.428145 0.312053 0.216 Uiso 1 1 calc R U . . .
H16B H 0.679045 0.481299 0.278721 0.216 Uiso 1 1 calc R U . . .
H16C H 0.591264 0.395833 0.220052 0.216 Uiso 1 1 calc R U . . .
C17 C 0.6332(15) 0.6361(16) 0.3033(12) 0.155(5) Uani 1 1 d . U . . .
H17A H 0.634277 0.672156 0.266549 0.233 Uiso 1 1 calc R U . . .
H17B H 0.697693 0.614097 0.316203 0.233 Uiso 1 1 calc R U . . .
H17C H 0.622100 0.677677 0.351177 0.233 Uiso 1 1 calc R U . . .
C18 C 0.4804(12) 0.5320(14) 0.1556(8) 0.122(5) Uani 1 1 d . . . . .
H18A H 0.427850 0.475569 0.126549 0.183 Uiso 1 1 calc R U . . .
H18B H 0.534889 0.529966 0.130311 0.183 Uiso 1 1 calc R U . . .
H18C H 0.452013 0.590527 0.156191 0.183 Uiso 1 1 calc R U . . .
C19 C 0.2531(9) 0.5660(9) 0.2159(6) 0.084(3) Uani 1 1 d . . . . .
H19A H 0.276514 0.587954 0.176981 0.126 Uiso 1 1 calc R U . . .
H19B H 0.195491 0.596100 0.225969 0.126 Uiso 1 1 calc R U . . .
H19C H 0.232741 0.496002 0.196091 0.126 Uiso 1 1 calc R U . . .
C20 C 0.4076(14) 0.7312(9) 0.3250(9) 0.114(4) Uani 1 1 d . U . . .
H20A H 0.475350 0.749453 0.361233 0.170 Uiso 1 1 calc R U . . .
H20B H 0.363220 0.772243 0.347036 0.170 Uiso 1 1 calc R U . . .
H20C H 0.410161 0.739344 0.274842 0.170 Uiso 1 1 calc R U . . .
C21 C 0.2930(14) 0.5964(9) 0.3870(8) 0.108(4) Uani 1 1 d . U . . .
H21A H 0.254475 0.531931 0.373568 0.162 Uiso 1 1 calc R U . . .
H21B H 0.247489 0.643503 0.390479 0.162 Uiso 1 1 calc R U . . .
H21C H 0.343772 0.611714 0.437403 0.162 Uiso 1 1 calc R U . . .
C22 C 0.1040(7) 0.3041(8) 0.2166(6) 0.078(2) Uani 1 1 d . . . . .
H22A H 0.055608 0.281280 0.240922 0.118 Uiso 1 1 calc R U . . .
H22B H 0.079032 0.275762 0.159619 0.118 Uiso 1 1 calc R U . . .
H22C H 0.112701 0.374298 0.230937 0.118 Uiso 1 1 calc R U . . .
C23 C 0.3071(8) 0.2925(8) 0.1887(5) 0.073(2) Uani 1 1 d . . . . .
H23A H 0.318648 0.361690 0.196406 0.110 Uiso 1 1 calc R U . . .
H23B H 0.271999 0.257741 0.133675 0.110 Uiso 1 1 calc R U . . .
H23C H 0.371855 0.271361 0.202685 0.110 Uiso 1 1 calc R U . . .
C24 C 0.2075(9) 0.1335(7) 0.2292(9) 0.106(4) Uani 1 1 d . . . . .
H24A H 0.272302 0.112137 0.242240 0.159 Uiso 1 1 calc R U . . .
H24B H 0.173679 0.102769 0.173356 0.159 Uiso 1 1 calc R U . . .
H24C H 0.165332 0.115511 0.260063 0.159 Uiso 1 1 calc R U . . .
C25 C 0.1154(12) 0.1848(12) 0.3690(12) 0.078(5) Uani 0.5 1 d D . P A 1
H25A H 0.060279 0.199249 0.332292 0.118 Uiso 0.5 1 calc R U P A 1
H25B H 0.091154 0.171695 0.411064 0.118 Uiso 0.5 1 calc R U P A 1
H25C H 0.139660 0.128329 0.341338 0.118 Uiso 0.5 1 calc R U P A 1
C26 C 0.1632(16) 0.3940(13) 0.4588(12) 0.082(6) Uani 0.5 1 d D . P A 1
H26A H 0.215492 0.450398 0.488820 0.124 Uiso 0.5 1 calc R U P A 1
H26B H 0.128389 0.375603 0.493940 0.124 Uiso 0.5 1 calc R U P A 1
H26C H 0.114849 0.409413 0.418073 0.124 Uiso 0.5 1 calc R U P A 1
C27 C 0.3086(12) 0.2632(14) 0.4953(10) 0.079(5) Uani 0.5 1 d D . P A 1
H27A H 0.322284 0.197811 0.476204 0.118 Uiso 0.5 1 calc R U P A 1
H27B H 0.276334 0.267833 0.537432 0.118 Uiso 0.5 1 calc R U P A 1
H27C H 0.371954 0.308967 0.515229 0.118 Uiso 0.5 1 calc R U P A 1
C28 C 0.1407(10) 0.4170(13) 0.4330(13) 0.071(4) Uani 0.5 1 d D . P A 2
H28A H 0.137052 0.442879 0.486924 0.107 Uiso 0.5 1 calc R U P A 2
H28B H 0.080312 0.369252 0.401886 0.107 Uiso 0.5 1 calc R U P A 2
H28C H 0.144871 0.469314 0.410483 0.107 Uiso 0.5 1 calc R U P A 2
C29 C 0.2333(16) 0.2414(11) 0.4542(13) 0.087(5) Uani 0.5 1 d D . P A 2
H29A H 0.183955 0.194095 0.409204 0.130 Uiso 0.5 1 calc R U P A 2
H29B H 0.207644 0.252768 0.500277 0.130 Uiso 0.5 1 calc R U P A 2
H29C H 0.296689 0.216941 0.464558 0.130 Uiso 0.5 1 calc R U P A 2
C30 C 0.3728(10) 0.4387(11) 0.5003(8) 0.059(3) Uani 0.5 1 d D . P A 2
H30A H 0.408561 0.411873 0.540209 0.071 Uiso 0.5 1 calc R U P A 2
H30B H 0.362918 0.504935 0.525049 0.071 Uiso 0.5 1 calc R U P A 2
K1 K -0.06420(13) -0.25816(13) 0.21158(12) 0.0679(5) Uani 1 1 d D . . . .
O5 O -0.0950(11) -0.4637(7) 0.1587(7) 0.139(3) Uani 1 1 d D . . . .
O6 O -0.0104(9) -0.3613(9) 0.3167(6) 0.131(3) Uani 1 1 d D . . . .
O7 O 0.0634(11) -0.2223(8) 0.1216(7) 0.134(3) Uani 1 1 d D . . . .
O8 O 0.1044(8) -0.1104(8) 0.2763(7) 0.124(3) Uani 1 1 d D . . . .
O9 O -0.2493(11) -0.2281(13) 0.1341(10) 0.178(4) Uani 1 1 d D U . . .
O10 O -0.1891(11) -0.1565(12) 0.2904(11) 0.175(4) Uani 1 1 d D . . . .
N4 N -0.1300(12) -0.3638(12) 0.0395(9) 0.156(3) Uani 1 1 d D U . . .
N5 N 0.0060(12) -0.1636(12) 0.3865(10) 0.157(3) Uani 1 1 d D . . . .
C31 C -0.1387(16) -0.4663(14) 0.0280(12) 0.170(5) Uani 1 1 d D U . . .
H31A H -0.123637 -0.496327 -0.022119 0.204 Uiso 1 1 calc R U . . .
H31B H -0.210328 -0.490889 0.020585 0.204 Uiso 1 1 calc R U . . .
C32 C -0.0786(19) -0.5039(16) 0.0866(9) 0.170(5) Uani 1 1 d D U . . .
H32A H -0.097709 -0.574709 0.069835 0.204 Uiso 1 1 calc R U . . .
H32B H -0.006339 -0.488373 0.090578 0.204 Uiso 1 1 calc R U . . .
C33 C -0.0463(14) -0.5037(11) 0.2125(8) 0.133(4) Uani 1 1 d D . . . .
H33A H 0.025690 -0.498844 0.213878 0.159 Uiso 1 1 calc R U . . .
H33B H -0.075436 -0.572736 0.196280 0.159 Uiso 1 1 calc R U . . .
C34 C -0.0551(11) -0.4559(9) 0.2901(8) 0.117(3) Uani 1 1 d D . . . .
H34A H -0.127069 -0.460161 0.288576 0.140 Uiso 1 1 calc R U . . .
H34B H -0.023007 -0.488899 0.326629 0.140 Uiso 1 1 calc R U . . .
C35 C -0.010(2) -0.3203(15) 0.3944(10) 0.197(8) Uani 1 1 d D . . . .
H35A H 0.014390 -0.361613 0.426129 0.236 Uiso 1 1 calc R U . . .
H35B H -0.078144 -0.309537 0.398327 0.236 Uiso 1 1 calc R U . . .
C36 C 0.060(2) -0.2279(14) 0.4201(14) 0.191(6) Uani 1 1 d D . . . .
H36A H 0.081576 -0.201039 0.477868 0.229 Uiso 1 1 calc R U . . .
H36B H 0.120676 -0.237392 0.401373 0.229 Uiso 1 1 calc R U . . .
C37 C 0.0735(14) -0.0737(14) 0.4004(12) 0.169(5) Uani 1 1 d D . . . .
H37A H 0.033196 -0.026434 0.385724 0.203 Uiso 1 1 calc R U . . .
H37B H 0.109379 -0.046475 0.456845 0.203 Uiso 1 1 calc R U . . .
C38 C 0.1462(14) -0.0894(15) 0.3557(8) 0.150(5) Uani 1 1 d D . . . .
H38A H 0.198399 -0.031124 0.374659 0.180 Uiso 1 1 calc R U . . .
H38B H 0.179572 -0.143118 0.365122 0.180 Uiso 1 1 calc R U . . .
C39 C 0.1783(11) -0.1181(11) 0.2386(8) 0.122(4) Uani 1 1 d D . . . .
H39A H 0.214006 -0.171273 0.245951 0.146 Uiso 1 1 calc R U . . .
H39B H 0.227791 -0.057621 0.258986 0.146 Uiso 1 1 calc R U . . .
C40 C 0.1270(13) -0.1373(11) 0.1556(9) 0.137(5) Uani 1 1 d D . . . .
H40A H 0.088674 -0.084994 0.150418 0.165 Uiso 1 1 calc R U . . .
H40B H 0.178345 -0.135953 0.126800 0.165 Uiso 1 1 calc R U . . .
C41 C 0.0218(16) -0.2424(13) 0.0435(8) 0.146(6) Uani 1 1 d D . . . .
H41A H 0.075419 -0.250684 0.016566 0.176 Uiso 1 1 calc R U . . .
H41B H -0.008948 -0.187363 0.034109 0.176 Uiso 1 1 calc R U . . .
C42 C -0.0555(17) -0.3300(15) 0.0097(13) 0.176(5) Uani 1 1 d D U . . .
H42A H -0.092684 -0.326787 -0.041865 0.212 Uiso 1 1 calc R U . . .
H42B H -0.017383 -0.383389 -0.001686 0.212 Uiso 1 1 calc R U . . .
C43 C -0.2255(17) -0.3388(19) 0.0103(14) 0.205(6) Uani 1 1 d D . . . .
H43A H -0.268139 -0.397269 -0.030047 0.246 Uiso 1 1 calc R U . . .
H43B H -0.214161 -0.291585 -0.016815 0.246 Uiso 1 1 calc R U . . .
C44 C -0.2851(19) -0.2988(17) 0.0644(12) 0.182(5) Uani 1 1 d D U . . .
H44A H -0.340749 -0.276294 0.033580 0.218 Uiso 1 1 calc R U . . .
H44B H -0.316512 -0.354208 0.075806 0.218 Uiso 1 1 calc R U . . .
C45 C -0.3109(14) -0.1996(17) 0.1764(12) 0.202(7) Uani 1 1 d D . . . .
H45A H -0.342713 -0.256162 0.186077 0.242 Uiso 1 1 calc R U . . .
H45B H -0.364928 -0.175713 0.145291 0.242 Uiso 1 1 calc R U . . .
C46 C -0.2664(18) -0.1247(19) 0.2519(14) 0.224(11) Uani 1 1 d D . . . .
H46A H -0.242448 -0.063831 0.244047 0.268 Uiso 1 1 calc R U . . .
H46B H -0.316698 -0.113119 0.281832 0.268 Uiso 1 1 calc R U . . .
C47 C -0.1376(17) -0.0905(18) 0.3612(11) 0.206(8) Uani 1 1 d D . . . .
H47A H -0.185102 -0.056702 0.386527 0.247 Uiso 1 1 calc R U . . .
H47B H -0.089835 -0.042265 0.353677 0.247 Uiso 1 1 calc R U . . .
C48 C -0.0825(16) -0.142(2) 0.4108(17) 0.210(7) Uani 1 1 d D . . . .
H48A H -0.063101 -0.101317 0.466345 0.252 Uiso 1 1 calc R U . . .
H48B H -0.125829 -0.202013 0.405249 0.252 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'
K K 0.3868 1.0657 '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 0.1589
0 -1 -2 0.1262
0 -2 1 0.1196
3 -8 -4 0.1235
-5 4 8 0.1088
0 9 -5 0.2729
-6 -5 -2 0.0945
0 3 -12 0.1927
-2 0 -10 0.1447
-4 -2 -7 0.1140
5 3 6 0.1198
2 0 10 0.1096
4 6 -11 0.2262
2 -3 -10 0.1530
-1 -7 -4 0.1035
-1 4 9 0.0999
0 6 6 0.1411
-7 4 7 0.0978
4 -9 3 0.1131
5 -8 1 0.1217
-9 2 3 0.0918
-8 4 0 0.1526
6 -6 6 0.1156
8 -4 0 0.2021
-8 -2 -1 0.0895
-6 1 -6 0.1103
5 -1 8 0.1080
6 0 6 0.1231
3 4 7 0.1089
-3 -6 -3 0.0928
-2 -4 -8 0.1120
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 U1 111.86(14) . 2_666 ?
O1 U1 Si6 110.68(16) . . ?
O1 U1 N1 121.8(4) . 2_666 ?
O1 U1 N2 114.6(3) . . ?
O1 U1 N3 95.5(2) . . ?
O1 U1 C30 95.7(3) . 2_666 ?
O1 U1 C30 117.8(4) . . ?
N1 U1 U1 29.0(3) 2_666 2_666 ?
N1 U1 U1 31.5(3) . 2_666 ?
N1 U1 O1 95.8(4) . . ?
N1 U1 N1 60.5(6) . 2_666 ?
N1 U1 N2 119.5(4) 2_666 . ?
N1 U1 N2 94.9(4) . . ?
N1 U1 N3 88.6(3) 2_666 . ?
N1 U1 N3 148.5(4) . . ?
N1 U1 C30 9.3(5) . 2_666 ?
N1 U1 C30 68.3(4) 2_666 2_666 ?
N2 U1 U1 110.05(19) . 2_666 ?
N2 U1 Si6 120.5(2) . . ?
N2 U1 C30 86.5(4) . 2_666 ?
N2 U1 C30 127.6(4) . . ?
N3 U1 U1 117.43(15) . 2_666 ?
N3 U1 Si6 31.88(16) . . ?
N3 U1 N2 106.9(2) . . ?
N3 U1 C30 157.0(3) . 2_666 ?
N3 U1 C30 68.4(3) . . ?
C30 U1 Si6 36.6(3) . . ?
C30 U1 Si6 125.1(3) 2_666 . ?
C30 U1 C30 88.6(4) . 2_666 ?
O1 Si1 O2 107.8(3) . . ?
O1 Si1 O3 115.4(3) . . ?
O1 Si1 O4 114.8(3) . . ?
O3 Si1 O2 104.8(3) . . ?
O4 Si1 O2 109.8(4) . . ?
O4 Si1 O3 103.8(3) . . ?
N2 Si2 C16 111.0(7) . . ?
N2 Si2 C17 115.5(7) . . ?
N2 Si2 C18 115.3(6) . . ?
C16 Si2 C17 93.9(11) . . ?
C16 Si2 C18 114.6(9) . . ?
C17 Si2 C18 104.5(9) . . ?
N2 Si3 C19 114.2(5) . . ?
N2 Si3 C20 115.3(7) . . ?
N2 Si3 C21 109.8(5) . . ?
C19 Si3 C20 103.5(6) . . ?
C19 Si3 C21 105.1(7) . . ?
C21 Si3 C20 108.2(7) . . ?
N3 Si4 C22 112.9(4) . . ?
N3 Si4 C23 111.1(4) . . ?
N3 Si4 C24 112.6(6) . . ?
C23 Si4 C22 106.0(5) . . ?
C23 Si4 C24 105.5(6) . . ?
C24 Si4 C22 108.1(5) . . ?
N3 Si5 C25 118.6(7) . . ?
N3 Si5 C26 109.2(8) . . ?
N3 Si5 C27 113.5(6) . . ?
C26 Si5 C25 104.3(7) . . ?
C26 Si5 C27 106.4(8) . . ?
C27 Si5 C25 103.9(7) . . ?
N3 Si6 U1 48.7(2) . . ?
N3 Si6 C28 116.9(8) . . ?
N3 Si6 C29 104.3(7) . . ?
N3 Si6 C30 101.7(6) . . ?
C28 Si6 U1 128.5(7) . . ?
C28 Si6 C29 108.8(7) . . ?
C29 Si6 U1 122.5(6) . . ?
C30 Si6 U1 53.2(5) . . ?
C30 Si6 C28 112.8(7) . . ?
C30 Si6 C29 112.0(7) . . ?
Si1 O1 U1 165.8(4) . . ?
C1 O2 Si1 132.0(6) . . ?
C5 O3 Si1 130.6(6) . . ?
C9 O4 Si1 132.7(5) . . ?
U1 N1 U1 119.5(6) . 2_666 ?
U1 N1 H1 120.3 . . ?
U1 N1 H1 120.3 2_666 . ?
Si2 N2 U1 121.2(5) . . ?
Si2 N2 Si3 121.0(4) . . ?
Si3 N2 U1 117.6(4) . . ?
Si4 N3 U1 121.5(3) . . ?
Si4 N3 Si5 112.8(4) . . ?
Si5 N3 U1 124.9(3) . . ?
Si6 N3 U1 99.4(3) . . ?
Si6 N3 Si4 137.8(4) . . ?
O2 C1 C2 105.5(9) . . ?
O2 C1 C3 110.4(11) . . ?
O2 C1 C4 112.2(10) . . ?
C2 C1 C4 108.7(12) . . ?
C3 C1 C2 110.1(12) . . ?
C3 C1 C4 109.9(11) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C5 C6 104.6(9) . . ?
O3 C5 C7 109.7(8) . . ?
O3 C5 C8 111.7(8) . . ?
C6 C5 C7 108.4(9) . . ?
C8 C5 C6 112.0(11) . . ?
C8 C5 C7 110.2(10) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O4 C9 C10 107.3(9) . . ?
O4 C9 C11 110.7(9) . . ?
O4 C9 C12 104.3(9) . . ?
O4 C9 C13 114.5(12) . . ?
O4 C9 C14 109.5(9) . . ?
O4 C9 C15 104.7(9) . . ?
C10 C9 C12 107.4(9) . . ?
C11 C9 C10 114.4(9) . . ?
C11 C9 C12 112.2(9) . . ?
C13 C9 C14 109.7(10) . . ?
C13 C9 C15 112.8(10) . . ?
C15 C9 C14 105.2(9) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C15 H15A 109.5 . . ?
C9 C15 H15B 109.5 . . ?
C9 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si2 C16 H16A 109.5 . . ?
Si2 C16 H16B 109.5 . . ?
Si2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si3 C19 H19A 109.5 . . ?
Si3 C19 H19B 109.5 . . ?
Si3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si4 C22 H22A 109.5 . . ?
Si4 C22 H22B 109.5 . . ?
Si4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si4 C23 H23A 109.5 . . ?
Si4 C23 H23B 109.5 . . ?
Si4 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si5 C25 H25A 109.5 . . ?
Si5 C25 H25B 109.5 . . ?
Si5 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si5 C26 H26A 109.5 . . ?
Si5 C26 H26B 109.5 . . ?
Si5 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si5 C27 H27A 109.5 . . ?
Si5 C27 H27B 109.5 . . ?
Si5 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si6 C28 H28A 109.5 . . ?
Si6 C28 H28B 109.5 . . ?
Si6 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si6 C29 H29A 109.5 . . ?
Si6 C29 H29B 109.5 . . ?
Si6 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
U1 C30 H30A 113.6 . . ?
U1 C30 H30B 113.6 . . ?
Si6 C30 U1 90.2(6) . . ?
Si6 C30 H30A 113.6 . . ?
Si6 C30 H30B 113.6 . . ?
H30A C30 H30B 110.9 . . ?
O5 K1 N4 60.8(4) . . ?
O5 K1 N5 115.6(4) . . ?
O5 K1 C44 81.9(5) . . ?
O6 K1 O5 58.8(3) . . ?
O6 K1 O7 121.0(4) . . ?
O6 K1 O8 97.5(4) . . ?
O6 K1 N4 119.2(4) . . ?
O6 K1 N5 57.2(4) . . ?
O6 K1 C44 128.4(5) . . ?
O7 K1 O5 99.0(4) . . ?
O7 K1 N4 62.4(4) . . ?
O7 K1 N5 118.4(4) . . ?
O7 K1 C44 95.2(5) . . ?
O8 K1 O5 135.3(4) . . ?
O8 K1 O7 58.7(3) . . ?
O8 K1 N4 120.6(4) . . ?
O8 K1 N5 60.8(4) . . ?
O8 K1 C44 133.7(5) . . ?
O9 K1 O5 100.1(5) . . ?
O9 K1 O6 132.0(4) . . ?
O9 K1 O7 103.7(5) . . ?
O9 K1 O8 121.6(4) . . ?
O9 K1 O10 57.4(5) . . ?
O9 K1 N4 65.7(5) . . ?
O9 K1 N5 116.9(5) . . ?
O9 K1 C44 21.7(4) . . ?
O10 K1 O5 121.8(5) . . ?
O10 K1 O6 95.2(5) . . ?
O10 K1 O7 136.2(4) . . ?
O10 K1 O8 95.6(4) . . ?
O10 K1 N4 122.7(5) . . ?
O10 K1 N5 59.6(5) . . ?
O10 K1 C44 77.4(5) . . ?
N4 K1 N5 176.3(5) . . ?
N4 K1 C44 45.4(4) . . ?
N5 K1 C44 136.7(5) . . ?
C32 O5 K1 114.5(11) . . ?
C33 O5 K1 114.7(9) . . ?
C33 O5 C32 110.9(12) . . ?
C34 O6 K1 115.2(8) . . ?
C34 O6 C35 109.9(11) . . ?
C35 O6 K1 118.9(13) . . ?
C40 O7 K1 113.5(10) . . ?
C40 O7 C41 113.8(11) . . ?
C41 O7 K1 117.6(11) . . ?
C38 O8 K1 114.5(10) . . ?
C39 O8 K1 116.4(8) . . ?
C39 O8 C38 110.1(11) . . ?
C44 O9 K1 109.0(14) . . ?
C45 O9 K1 117.0(12) . . ?
C45 O9 C44 119.4(15) . . ?
C46 O10 K1 120.9(15) . . ?
C46 O10 C47 112.6(14) . . ?
C47 O10 K1 113.3(11) . . ?
C31 N4 K1 108.6(12) . . ?
C42 N4 K1 105.4(13) . . ?
C42 N4 C31 112.7(15) . . ?
C42 N4 C43 112.5(19) . . ?
C43 N4 K1 106.0(14) . . ?
C43 N4 C31 111.2(14) . . ?
C36 N5 K1 107.7(13) . . ?
C36 N5 C37 110.6(14) . . ?
C37 N5 K1 106.3(12) . . ?
C48 N5 K1 106.2(16) . . ?
C48 N5 C36 116(2) . . ?
C48 N5 C37 109.6(14) . . ?
N4 C31 H31A 107.0 . . ?
N4 C31 H31B 107.0 . . ?
N4 C31 C32 121.5(18) . . ?
H31A C31 H31B 106.7 . . ?
C32 C31 H31A 107.0 . . ?
C32 C31 H31B 107.0 . . ?
O5 C32 C31 110.1(18) . . ?
O5 C32 H32A 109.6 . . ?
O5 C32 H32B 109.6 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.2 . . ?
O5 C33 H33A 109.4 . . ?
O5 C33 H33B 109.4 . . ?
O5 C33 C34 111.4(13) . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
O6 C34 C33 111.3(13) . . ?
O6 C34 H34A 109.4 . . ?
O6 C34 H34B 109.4 . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
O6 C35 H35A 111.1 . . ?
O6 C35 H35B 111.1 . . ?
O6 C35 C36 103.4(18) . . ?
H35A C35 H35B 109.0 . . ?
C36 C35 H35A 111.1 . . ?
C36 C35 H35B 111.1 . . ?
N5 C36 C35 107(2) . . ?
N5 C36 H36A 110.4 . . ?
N5 C36 H36B 110.4 . . ?
C35 C36 H36A 110.4 . . ?
C35 C36 H36B 110.4 . . ?
H36A C36 H36B 108.6 . . ?
N5 C37 H37A 109.3 . . ?
N5 C37 H37B 109.3 . . ?
H37A C37 H37B 108.0 . . ?
C38 C37 N5 111.4(15) . . ?
C38 C37 H37A 109.3 . . ?
C38 C37 H37B 109.3 . . ?
O8 C38 C37 113.4(16) . . ?
O8 C38 H38A 108.9 . . ?
O8 C38 H38B 108.9 . . ?
C37 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
O8 C39 H39A 110.6 . . ?
O8 C39 H39B 110.6 . . ?
O8 C39 C40 105.9(14) . . ?
H39A C39 H39B 108.7 . . ?
C40 C39 H39A 110.6 . . ?
C40 C39 H39B 110.6 . . ?
O7 C40 C39 114.3(14) . . ?
O7 C40 H40A 108.7 . . ?
O7 C40 H40B 108.7 . . ?
C39 C40 H40A 108.7 . . ?
C39 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
O7 C41 H41A 109.1 . . ?
O7 C41 H41B 109.1 . . ?
O7 C41 C42 112.6(16) . . ?
H41A C41 H41B 107.8 . . ?
C42 C41 H41A 109.1 . . ?
C42 C41 H41B 109.1 . . ?
N4 C42 C41 130(2) . . ?
N4 C42 H42A 104.7 . . ?
N4 C42 H42B 104.7 . . ?
C41 C42 H42A 104.7 . . ?
C41 C42 H42B 104.7 . . ?
H42A C42 H42B 105.7 . . ?
N4 C43 H43A 107.3 . . ?
N4 C43 H43B 107.3 . . ?
N4 C43 C44 120(2) . . ?
H43A C43 H43B 106.9 . . ?
C44 C43 H43A 107.3 . . ?
C44 C43 H43B 107.3 . . ?
K1 C44 H44A 152.1 . . ?
K1 C44 H44B 94.4 . . ?
O9 C44 K1 49.3(11) . . ?
O9 C44 C43 126(2) . . ?
O9 C44 H44A 105.9 . . ?
O9 C44 H44B 105.9 . . ?
C43 C44 K1 85.6(15) . . ?
C43 C44 H44A 105.9 . . ?
C43 C44 H44B 105.9 . . ?
H44A C44 H44B 106.2 . . ?
O9 C45 H45A 108.2 . . ?
O9 C45 H45B 108.2 . . ?
O9 C45 C46 116(2) . . ?
H45A C45 H45B 107.4 . . ?
C46 C45 H45A 108.2 . . ?
C46 C45 H45B 108.2 . . ?
O10 C46 C45 106.7(19) . . ?
O10 C46 H46A 110.4 . . ?
O10 C46 H46B 110.4 . . ?
C45 C46 H46A 110.4 . . ?
C45 C46 H46B 110.4 . . ?
H46A C46 H46B 108.6 . . ?
O10 C47 H47A 110.0 . . ?
O10 C47 H47B 110.0 . . ?
O10 C47 C48 108(2) . . ?
H47A C47 H47B 108.4 . . ?
C48 C47 H47A 110.0 . . ?
C48 C47 H47B 110.0 . . ?
N5 C48 C47 108.6(18) . . ?
N5 C48 H48A 110.0 . . ?
N5 C48 H48B 110.0 . . ?
C47 C48 H48A 110.0 . . ?
C47 C48 H48B 110.0 . . ?
H48A C48 H48B 108.4 . . ?
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 U1 3.9213(4) 2_666 ?
U1 Si6 3.119(4) . ?
U1 O1 2.237(5) . ?
U1 N1 2.184(11) . ?
U1 N1 2.355(12) 2_666 ?
U1 N2 2.424(7) . ?
U1 N3 2.375(6) . ?
U1 C30 2.497(16) . ?
U1 C30 2.962(12) 2_666 ?
Si1 O1 1.582(5) . ?
Si1 O2 1.638(6) . ?
Si1 O3 1.634(5) . ?
Si1 O4 1.620(6) . ?
Si2 N2 1.694(9) . ?
Si2 C16 1.707(18) . ?
Si2 C17 1.838(17) . ?
Si2 C18 1.871(14) . ?
Si3 N2 1.705(10) . ?
Si3 C19 1.871(11) . ?
Si3 C20 1.903(13) . ?
Si3 C21 1.884(13) . ?
Si4 N3 1.698(6) . ?
Si4 C22 1.886(9) . ?
Si4 C23 1.870(10) . ?
Si4 C24 1.877(10) . ?
Si5 N3 1.808(7) . ?
Si5 C25 1.904(13) . ?
Si5 C26 1.871(13) . ?
Si5 C27 1.890(13) . ?
Si6 N3 1.670(7) . ?
Si6 C28 1.886(12) . ?
Si6 C29 1.898(13) . ?
Si6 C30 1.859(12) . ?
O2 C1 1.417(11) . ?
O3 C5 1.421(11) . ?
O4 C9 1.444(10) . ?
N1 H1 0.8800 . ?
C1 C2 1.538(18) . ?
C1 C3 1.47(2) . ?
C1 C4 1.542(17) . ?
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 C6 1.533(14) . ?
C5 C7 1.536(14) . ?
C5 C8 1.483(15) . ?
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 C10 1.532(13) . ?
C9 C11 1.472(14) . ?
C9 C12 1.551(13) . ?
C9 C13 1.463(14) . ?
C9 C14 1.573(13) . ?
C9 C15 1.541(14) . ?
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 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
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 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
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 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
K1 O5 2.861(10) . ?
K1 O6 2.810(11) . ?
K1 O7 2.823(12) . ?
K1 O8 2.811(10) . ?
K1 O9 2.773(15) . ?
K1 O10 2.799(14) . ?
K1 N4 2.994(17) . ?
K1 N5 3.015(17) . ?
K1 C44 3.46(2) . ?
O5 C32 1.384(13) . ?
O5 C33 1.375(12) . ?
O6 C34 1.369(12) . ?
O6 C35 1.394(13) . ?
O7 C40 1.352(12) . ?
O7 C41 1.359(12) . ?
O8 C38 1.380(13) . ?
O8 C39 1.371(12) . ?
O9 C44 1.355(14) . ?
O9 C45 1.312(13) . ?
O10 C46 1.343(14) . ?
O10 C47 1.370(14) . ?
N4 C31 1.454(15) . ?
N4 C42 1.401(15) . ?
N4 C43 1.433(15) . ?
N5 C36 1.448(15) . ?
N5 C37 1.472(15) . ?
N5 C48 1.439(16) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.477(15) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.451(14) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.483(16) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.448(15) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.467(15) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.475(15) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.480(16) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.462(16) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.475(16) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
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
U1 Si6 N3 Si4 -166.7(9) . . . . ?
Si1 O2 C1 C2 157.0(9) . . . . ?
Si1 O2 C1 C3 -84.1(14) . . . . ?
Si1 O2 C1 C4 38.8(17) . . . . ?
Si1 O3 C5 C6 -160.4(8) . . . . ?
Si1 O3 C5 C7 83.5(10) . . . . ?
Si1 O3 C5 C8 -39.0(13) . . . . ?
Si1 O4 C9 C10 39.0(11) . . . . ?
Si1 O4 C9 C11 -86.4(11) . . . . ?
Si1 O4 C9 C12 152.7(9) . . . . ?
Si1 O4 C9 C13 90.3(12) . . . . ?
Si1 O4 C9 C14 -33.3(12) . . . . ?
Si1 O4 C9 C15 -145.7(9) . . . . ?
O1 Si1 O2 C1 158.1(11) . . . . ?
O1 Si1 O3 C5 74.9(8) . . . . ?
O1 Si1 O4 C9 48.9(8) . . . . ?
O2 Si1 O1 U1 -20.6(13) . . . . ?
O2 Si1 O3 C5 -166.8(7) . . . . ?
O2 Si1 O4 C9 -72.7(8) . . . . ?
O3 Si1 O1 U1 96.1(12) . . . . ?
O3 Si1 O2 C1 34.7(12) . . . . ?
O3 Si1 O4 C9 175.7(7) . . . . ?
O4 Si1 O1 U1 -143.3(12) . . . . ?
O4 Si1 O2 C1 -76.1(11) . . . . ?
O4 Si1 O3 C5 -51.7(8) . . . . ?
N3 Si6 C30 U1 4.1(6) . . . . ?
C16 Si2 N2 U1 4.7(10) . . . . ?
C16 Si2 N2 Si3 179.4(9) . . . . ?
C17 Si2 N2 U1 -100.7(9) . . . . ?
C17 Si2 N2 Si3 74.0(10) . . . . ?
C18 Si2 N2 U1 137.1(7) . . . . ?
C18 Si2 N2 Si3 -48.2(9) . . . . ?
C19 Si3 N2 U1 -109.8(5) . . . . ?
C19 Si3 N2 Si2 75.3(7) . . . . ?
C20 Si3 N2 U1 130.5(6) . . . . ?
C20 Si3 N2 Si2 -44.3(8) . . . . ?
C21 Si3 N2 U1 8.0(7) . . . . ?
C21 Si3 N2 Si2 -166.9(7) . . . . ?
C22 Si4 N3 U1 -120.6(5) . . . . ?
C22 Si4 N3 Si5 69.0(6) . . . . ?
C22 Si4 N3 Si6 43.9(9) . . . . ?
C23 Si4 N3 U1 -1.6(6) . . . . ?
C23 Si4 N3 Si5 -172.0(4) . . . . ?
C23 Si4 N3 Si6 162.9(7) . . . . ?
C24 Si4 N3 U1 116.6(6) . . . . ?
C24 Si4 N3 Si5 -53.8(6) . . . . ?
C24 Si4 N3 Si6 -78.9(9) . . . . ?
C25 Si5 N3 U1 -160.7(7) . . . . ?
C25 Si5 N3 Si4 9.4(8) . . . . ?
C26 Si5 N3 U1 80.1(8) . . . . ?
C26 Si5 N3 Si4 -109.8(8) . . . . ?
C27 Si5 N3 U1 -38.3(8) . . . . ?
C27 Si5 N3 Si4 131.7(8) . . . . ?
C28 Si6 N3 U1 118.9(7) . . . . ?
C28 Si6 N3 Si4 -47.7(10) . . . . ?
C28 Si6 C30 U1 -122.0(9) . . . . ?
C29 Si6 N3 U1 -120.9(7) . . . . ?
C29 Si6 N3 Si4 72.4(10) . . . . ?
C29 Si6 C30 U1 114.9(8) . . . . ?
C30 Si6 N3 U1 -4.3(6) . . . . ?
C30 Si6 N3 Si4 -171.0(8) . . . . ?
K1 O5 C32 C31 -53(2) . . . . ?
K1 O5 C33 C34 43.0(17) . . . . ?
K1 O6 C34 C33 49.1(15) . . . . ?
K1 O6 C35 C36 -57(2) . . . . ?
K1 O7 C40 C39 46.4(19) . . . . ?
K1 O7 C41 C42 -37(2) . . . . ?
K1 O8 C38 C37 -51(2) . . . . ?
K1 O8 C39 C40 49.3(15) . . . . ?
K1 O9 C44 C43 -42(3) . . . . ?
K1 O9 C45 C46 44(3) . . . . ?
K1 O10 C46 C45 39(3) . . . . ?
K1 O10 C47 C48 -60(2) . . . . ?
K1 N4 C31 C32 -27(2) . . . . ?
K1 N4 C42 C41 -18(3) . . . . ?
K1 N4 C43 C44 -19(3) . . . . ?
K1 N5 C36 C35 -57(2) . . . . ?
K1 N5 C37 C38 -47.6(18) . . . . ?
K1 N5 C48 C47 -51(2) . . . . ?
O5 C33 C34 O6 -62.6(18) . . . . ?
O6 C35 C36 N5 76(3) . . . . ?
O7 C41 C42 N4 40(4) . . . . ?
O8 C39 C40 O7 -65(2) . . . . ?
O9 C45 C46 O10 -54(4) . . . . ?
O10 C47 C48 N5 78(3) . . . . ?
N4 C31 C32 O5 56(3) . . . . ?
N4 C43 C44 K1 16(2) . . . . ?
N4 C43 C44 O9 46(4) . . . . ?
N5 C37 C38 O8 70(2) . . . . ?
C31 N4 C42 C41 -137(3) . . . . ?
C31 N4 C43 C44 99(3) . . . . ?
C32 O5 C33 C34 174.6(16) . . . . ?
C33 O5 C32 C31 175.0(17) . . . . ?
C34 O6 C35 C36 167.2(18) . . . . ?
C35 O6 C34 C33 -173.3(18) . . . . ?
C36 N5 C37 C38 69(2) . . . . ?
C36 N5 C48 C47 -170.1(18) . . . . ?
C37 N5 C36 C35 -172.9(16) . . . . ?
C37 N5 C48 C47 64(3) . . . . ?
C38 O8 C39 C40 -178.3(14) . . . . ?
C39 O8 C38 C37 176.0(16) . . . . ?
C40 O7 C41 C42 -174(2) . . . . ?
C41 O7 C40 C39 -175.5(17) . . . . ?
C42 N4 C31 C32 89(3) . . . . ?
C42 N4 C43 C44 -134(2) . . . . ?
C43 N4 C31 C32 -143(2) . . . . ?
C43 N4 C42 C41 97(3) . . . . ?
C44 O9 C45 C46 178(2) . . . . ?
C45 O9 C44 K1 -138(3) . . . . ?
C45 O9 C44 C43 -180(2) . . . . ?
C46 O10 C47 C48 159(2) . . . . ?
C47 O10 C46 C45 177(2) . . . . ?
C48 N5 C36 C35 62(3) . . . . ?
C48 N5 C37 C38 -162(2) . . . . ?
loop_
_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
-0.0013 -0.0014 -0.9984 0.0685 0.0062 -0.0582
-0.0072 -1.0029 -1.9923 0.2143 0.0784 -0.0728
-0.0077 -1.9986 1.0076 0.0863 0.1259 0.1454
3.2720 -7.6850 -3.9310 0.6083 0.7937 -0.0063
-4.6390 4.4037 8.2598 -0.5440 -0.7107 0.4461
0.3216 9.4667 -4.6165 -0.4415 -0.5749 -0.6889
-5.6664 -4.6417 -2.3254 0.9594 -0.1255 0.2526
0.2310 2.5470 -11.7596 0.5891 -0.0781 -0.8043
-2.2172 -0.0176 -9.9531 0.8547 -0.1126 -0.5068
-4.0124 -2.1848 -7.1875 0.9730 -0.1277 -0.1922
4.6194 3.0042 5.8165 -0.9899 0.1298 0.0567
2.4214 0.2496 9.7112 -0.8720 0.1148 0.4759
3.8663 5.9079 -10.5457 -0.0370 -0.0213 -0.9991
1.7924 -3.2707 -9.6181 0.7710 0.4186 -0.4799
-0.5337 -7.4267 -3.7470 0.8722 0.4744 0.1195
-1.3638 4.2403 8.6966 -0.8164 -0.4434 0.3700
-0.2758 6.2705 6.0185 -0.8750 -0.4757 0.0899
-7.1329 3.5800 7.0460 -0.2030 -0.8457 0.4936
3.8786 -8.9680 2.6277 0.2118 0.8863 0.4119
4.8954 -8.4417 0.6697 0.2258 0.9439 0.2411
-8.9728 1.6138 3.3217 0.3470 -0.8375 0.4220
-8.4289 3.8324 -0.3095 0.3814 -0.9194 0.0962
5.7243 -6.3404 5.7444 -0.3483 0.8384 0.4192
8.4210 -3.8478 0.3374 -0.3815 0.9196 -0.0936
-7.9372 -1.9016 -0.6814 0.8120 -0.4973 0.3057
-6.2733 0.8205 -6.0516 0.8390 -0.5132 -0.1806
4.5521 -1.3009 8.4110 -0.8291 0.3944 0.3962
5.9976 0.1776 6.0306 -0.8933 0.4253 0.1455
2.9173 4.0393 6.5920 -0.9904 -0.0784 0.1137
-3.2872 -6.3103 -3.2255 0.9647 0.1792 0.1932
-1.5519 -3.7839 -7.8884 0.9529 0.1775 -0.2458
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.586 -0.939 0.000 778.9 108.6 '2.7 THF'
2 0.000 0.500 0.500 21.0 0.0 ?
