#------------------------------------------------------------------------------
#$Date: 2022-09-01 01:13:14 +0300 (Thu, 01 Sep 2022) $
#$Revision: 277508 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/75/1567555.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_1567555
loop_
_publ_author_name
'Modder, dieuwertje'
'Batov, Mikhail'
'Rajeshkumar, Thayalan'
'Scopelliti, Rosario'
'Zivkovic, Ivica'
'Sienkiewicz, Andrzej'
'Maron, Laurent'
'Mazzanti, Marinella'
_publ_section_title
;
 Assembling Diuranium Complexes in Different States of Charge with a
 Bridging Redox-Active Ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03592H
_journal_year                    2022
_chemical_formula_moiety         'C44 H114 N10 Si12 U2, C18 H36 K N2 O6'
_chemical_formula_sum            'C62 H150 K N12 O6 Si12 U2'
_chemical_formula_weight         2012.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.332(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.9688(16)
_cell_length_b                   11.6805(5)
_cell_length_c                   32.306(3)
_cell_measurement_reflns_used    8607
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.1800
_cell_measurement_theta_min      3.0220
_cell_volume                     10221.3(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -117.00 -21.00   1.00   10.00    --  -42.38 -37.00   0.00   96
  2  ω    -39.00 -11.00   1.00   10.00    --  -42.38 125.00  60.00   28
  3  ω    -64.00  -6.00   1.00   10.00    --  -42.38 125.00-180.00   58
  4  ω   -117.00 -25.00   1.00   10.00    --  -42.38 -37.00 -90.00   92
  5  ω     15.00  64.00   1.00   10.00    --   42.38 -99.00 150.00   49
  6  ω     53.00  92.00   1.00   10.00    --   42.38-125.00 -30.00   39
  7  ω    105.00 152.00   1.00   40.00    --  103.80 111.00  30.00   47
  8  ω     76.00 108.00   1.00   40.00    --  103.80  61.00 120.00   32
  9  ω     78.00 172.00   1.00   40.00    --  103.80  45.00  90.00   94
 10  ω     35.00 108.00   1.00   40.00    --  103.80-111.00   0.00   73
 11  ω     69.00 105.00   1.00   40.00    --  103.80 -94.00  30.00   36
 12  ω    135.00 175.00   1.00   40.00    --  103.80  61.00 120.00   40
 13  ω     21.00  68.00   1.00   40.00    --  103.80 -94.00  30.00   47
 14  ω     31.00  64.00   1.00   40.00    --  103.80 -77.00  30.00   33
 15  ω     30.00 108.00   1.00   40.00    --  103.80-111.00 -90.00   78
 16  ω     32.00 106.00   1.00   40.00    --  103.80 -94.00-180.00   74
 17  ω    104.00 131.00   1.00   40.00    --  103.80 -77.00  30.00   27
 18  ω     37.00  77.00   1.00   40.00    --  103.80 -45.00 150.00   40
 19  ω     28.00  76.00   1.00   40.00    --  103.80 -94.00 -60.00   48
 20  ω     38.00 108.00   1.00   40.00    --  103.80-111.00 120.00   70
 21  ω     51.00 175.00   1.00   40.00    --  103.80  15.00-150.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0093896000
_diffrn_orient_matrix_UB_12      -0.0261679000
_diffrn_orient_matrix_UB_13      0.0423218000
_diffrn_orient_matrix_UB_21      -0.0241561000
_diffrn_orient_matrix_UB_22      0.1184439000
_diffrn_orient_matrix_UB_23      -0.0042705000
_diffrn_orient_matrix_UB_31      -0.0506287000
_diffrn_orient_matrix_UB_32      -0.0519344000
_diffrn_orient_matrix_UB_33      -0.0311773000
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            37255
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.679
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.903
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.143
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4100
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.054
_refine_diff_density_max         2.844
_refine_diff_density_min         -2.447
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         10025
_refine_ls_number_restraints     446
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0771
_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)+(0.1510P)²+66.7292P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2026
_refine_ls_wR_factor_ref         0.2502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6715
_reflns_number_total             10025
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc03592h2.cif
_cod_data_source_block           mb8
_cod_database_code               1567555
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C68 H164 N12 O6 Si12 K1 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   0.591
_shelx_estimated_absorpt_t_min   0.133
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29_$1-C29
 1.54 with sigma of 0.02
 O3-C29
 1.43 with sigma of 0.02
 O3-C29_$1 = O3_$1-C29
 2.4 with sigma of 0.02
 C31-C30 = C24-C23 = C26-C25 = C28-C27
 1.54 with sigma of 0.02
 O2-C26 = O1-C25 = O1-C24 = O3-C28 = O3-C29
 1.43 with sigma of 0.02
 N6_$1-C27_$1 = N6_$1-C23_$1 = N6_$1-C30_$1
 1.47 with sigma of 0.02
 C28_$1-C27_$1 \\sim C28-C27 \\sim C29_$1-C29
 with sigma of 0.02
 O3-C28 \\sim O3-C29 \\sim O3_$1-C29_$1 \\sim O3_$1-C28_$1
 with sigma of 0.02
 N6-C27 \\sim N6_$1-C27_$1
 with sigma of 0.02
 C30-C23 \\sim C23-C27
 with sigma of 0.02
 N6-C30 \\sim N6-C27 \\sim N6-C23
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Si2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C13) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
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.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), 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)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 200 electrons were 
found in a volume of 1392Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[C6H14] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2021-07-05
_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 3.298
_oxdiff_exptl_absorpt_empirical_full_min 0.543
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.36732(2) 0.31548(3) 0.32017(2) 0.06279(19) Uani 1 1 d . . . . .
Si1 Si 0.38866(17) 0.0948(4) 0.2618(2) 0.1029(15) Uani 1 1 d . . . . .
Si2 Si 0.44764(18) 0.2960(4) 0.2598(3) 0.1094(17) Uani 1 1 d . U . . .
Si3 Si 0.43838(16) 0.1502(4) 0.4221(2) 0.1077(16) Uani 1 1 d . . . . .
Si4 Si 0.3769(2) 0.3282(4) 0.43542(17) 0.0987(12) Uani 1 1 d . . . . .
Si5 Si 0.43097(14) 0.5746(4) 0.36260(19) 0.0961(14) Uani 1 1 d . . . . .
Si6 Si 0.32769(13) 0.6093(3) 0.29644(15) 0.0757(9) Uani 1 1 d . . . . .
N1 N 0.2995(3) 0.3192(8) 0.2410(4) 0.0629(17) Uani 1 1 d . . . . .
N2 N 0.2127(3) 0.2735(9) 0.1886(4) 0.0627(19) Uani 1 1 d . . . . .
N3 N 0.4078(4) 0.2321(11) 0.2794(5) 0.090(2) Uani 1 1 d . . . . .
N4 N 0.3963(4) 0.2624(11) 0.3979(4) 0.087(2) Uani 1 1 d . . . . .
N5 N 0.3748(4) 0.5167(9) 0.3253(4) 0.071(2) Uani 1 1 d . . . . .
C1 C 0.2529(4) 0.2729(9) 0.2318(4) 0.0547(19) Uani 1 1 d . . . . .
C2 C 0.2205(5) 0.3243(11) 0.1557(5) 0.073(3) Uani 1 1 d . . . . .
H2 H 0.193955 0.327970 0.126035 0.087 Uiso 1 1 calc R U . . .
C3 C 0.2652(5) 0.3726(14) 0.1620(5) 0.084(3) Uani 1 1 d . . . . .
H3 H 0.269171 0.408013 0.137321 0.101 Uiso 1 1 calc R U . . .
C4 C 0.3038(5) 0.3680(11) 0.2050(5) 0.070(2) Uani 1 1 d . . . . .
H4 H 0.334635 0.400311 0.209559 0.084 Uiso 1 1 calc R U . . .
C5 C 0.3639(4) 0.0419(11) 0.3075(6) 0.091(3) Uani 1 1 d . U . . .
H5A H 0.390445 0.048540 0.338496 0.136 Uiso 1 1 calc R U . . .
H5B H 0.353341 -0.038173 0.301340 0.136 Uiso 1 1 calc R U . . .
H5C H 0.335911 0.089512 0.304864 0.136 Uiso 1 1 calc R U . . .
C6 C 0.3410(8) 0.0839(17) 0.2019(8) 0.122(5) Uani 1 1 d . . . . .
H6A H 0.309375 0.111853 0.200027 0.184 Uiso 1 1 calc R U . . .
H6B H 0.337520 0.003786 0.191954 0.184 Uiso 1 1 calc R U . . .
H6C H 0.350928 0.130302 0.181943 0.184 Uiso 1 1 calc R U . . .
C7 C 0.4393(8) -0.0090(18) 0.2681(10) 0.136(6) Uani 1 1 d . U . . .
H7A H 0.458651 0.021724 0.252702 0.204 Uiso 1 1 calc R U . . .
H7B H 0.424763 -0.082511 0.254294 0.204 Uiso 1 1 calc R U . . .
H7C H 0.460893 -0.020223 0.300713 0.204 Uiso 1 1 calc R U . . .
C8 C 0.4366(8) 0.253(2) 0.2025(9) 0.128(5) Uani 1 1 d . . . . .
H8A H 0.440366 0.169568 0.201674 0.192 Uiso 1 1 calc R U . . .
H8B H 0.460508 0.290636 0.193775 0.192 Uiso 1 1 calc R U . . .
H8C H 0.403083 0.274642 0.181092 0.192 Uiso 1 1 calc R U . . .
C9 C 0.5144(6) 0.259(2) 0.2978(9) 0.131(5) Uani 1 1 d . U . . .
H9A H 0.522766 0.284176 0.329226 0.196 Uiso 1 1 calc R U . . .
H9B H 0.535986 0.297704 0.286441 0.196 Uiso 1 1 calc R U . . .
H9C H 0.519065 0.176005 0.297514 0.196 Uiso 1 1 calc R U . . .
C10 C 0.4410(6) 0.4571(15) 0.2559(8) 0.107(5) Uani 1 1 d . . . . .
H10A H 0.433683 0.481991 0.224709 0.160 Uiso 1 1 calc R U . . .
H10B H 0.471775 0.492630 0.277499 0.160 Uiso 1 1 calc R U . . .
H10C H 0.413926 0.480219 0.263549 0.160 Uiso 1 1 calc R U . . .
C11 C 0.4067(7) 0.0101(15) 0.4238(7) 0.117(6) Uani 1 1 d . . . . .
H11A H 0.411957 -0.005922 0.455308 0.175 Uiso 1 1 calc R U . . .
H11B H 0.420603 -0.052328 0.412697 0.175 Uiso 1 1 calc R U . . .
H11C H 0.371220 0.016357 0.404176 0.175 Uiso 1 1 calc R U . . .
C12 C 0.4773(6) 0.1275(16) 0.3900(7) 0.115(4) Uani 1 1 d . . . . .
H12A H 0.458698 0.151291 0.358091 0.172 Uiso 1 1 calc R U . . .
H12B H 0.485866 0.046275 0.391085 0.172 Uiso 1 1 calc R U . . .
H12C H 0.507519 0.173129 0.404226 0.172 Uiso 1 1 calc R U . . .
C13 C 0.4855(8) 0.1714(16) 0.4827(8) 0.130(6) Uani 1 1 d . U . . .
H13A H 0.506486 0.236944 0.484189 0.195 Uiso 1 1 calc R U . . .
H13B H 0.505869 0.102408 0.493299 0.195 Uiso 1 1 calc R U . . .
H13C H 0.468624 0.185789 0.502388 0.195 Uiso 1 1 calc R U . . .
C14 C 0.3259(7) 0.4299(15) 0.4039(6) 0.097(4) Uani 1 1 d . . . . .
H14A H 0.335882 0.481946 0.385655 0.146 Uiso 1 1 calc R U . . .
H14B H 0.318282 0.474288 0.425877 0.146 Uiso 1 1 calc R U . . .
H14C H 0.296487 0.387082 0.383673 0.146 Uiso 1 1 calc R U . . .
C15 C 0.3520(10) 0.228(2) 0.4670(8) 0.129(6) Uani 1 1 d . . . . .
H15A H 0.322960 0.187721 0.444744 0.193 Uiso 1 1 calc R U . . .
H15B H 0.342586 0.272818 0.487698 0.193 Uiso 1 1 calc R U . . .
H15C H 0.377474 0.172572 0.484678 0.193 Uiso 1 1 calc R U . . .
C16 C 0.4249(9) 0.4145(19) 0.4826(7) 0.141(8) Uani 1 1 d . . . . .
H16A H 0.444672 0.363712 0.507999 0.211 Uiso 1 1 calc R U . . .
H16B H 0.408661 0.472325 0.493378 0.211 Uiso 1 1 calc R U . . .
H16C H 0.446451 0.452428 0.470985 0.211 Uiso 1 1 calc R U . . .
C17 C 0.4788(5) 0.4565(16) 0.3844(8) 0.118(5) Uani 1 1 d . . . . .
H17A H 0.469100 0.400901 0.401792 0.177 Uiso 1 1 calc R U . . .
H17B H 0.510951 0.489365 0.404280 0.177 Uiso 1 1 calc R U . . .
H17C H 0.480986 0.417973 0.358381 0.177 Uiso 1 1 calc R U . . .
C18 C 0.4545(7) 0.6898(15) 0.3371(9) 0.123(6) Uani 1 1 d . . . . .
H18A H 0.459906 0.658388 0.311437 0.184 Uiso 1 1 calc R U . . .
H18B H 0.485728 0.719603 0.360355 0.184 Uiso 1 1 calc R U . . .
H18C H 0.430241 0.751915 0.325963 0.184 Uiso 1 1 calc R U . . .
C19 C 0.4295(8) 0.6435(17) 0.4131(7) 0.122(5) Uani 1 1 d . . . . .
H19A H 0.418875 0.723219 0.405917 0.182 Uiso 1 1 calc R U . . .
H19B H 0.462581 0.641309 0.438559 0.182 Uiso 1 1 calc R U . . .
H19C H 0.406317 0.602578 0.421920 0.182 Uiso 1 1 calc R U . . .
C20 C 0.3292(7) 0.6642(15) 0.2424(6) 0.100(4) Uani 1 1 d . . . . .
H20A H 0.362700 0.689535 0.248946 0.149 Uiso 1 1 calc R U . . .
H20B H 0.306296 0.728725 0.230626 0.149 Uiso 1 1 calc R U . . .
H20C H 0.319312 0.602898 0.219510 0.149 Uiso 1 1 calc R U . . .
C21 C 0.2655(5) 0.5420(13) 0.2813(6) 0.089(4) Uani 1 1 d . . . . .
H21A H 0.259710 0.481766 0.258416 0.133 Uiso 1 1 calc R U . . .
H21B H 0.239764 0.600472 0.268725 0.133 Uiso 1 1 calc R U . . .
H21C H 0.264830 0.508634 0.308834 0.133 Uiso 1 1 calc R U . . .
C22 C 0.3265(6) 0.7414(13) 0.3303(6) 0.091(4) Uani 1 1 d . . . . .
H22A H 0.316317 0.719573 0.354282 0.137 Uiso 1 1 calc R U . . .
H22B H 0.302940 0.797008 0.309675 0.137 Uiso 1 1 calc R U . . .
H22C H 0.359457 0.775625 0.344297 0.137 Uiso 1 1 calc R U . . .
K1 K 0.250000 0.6610(8) 0.500000 0.127(2) Uani 1 2 d S T P . .
O1 O 0.2574(11) 0.740(3) 0.5811(8) 0.211(8) Uani 1 1 d D . . . .
O2 O 0.1697(11) 0.760(3) 0.5024(9) 0.208(7) Uani 1 1 d D U . . .
O3 O 0.2977(10) 0.424(2) 0.5362(8) 0.215(8) Uani 1 1 d D . . . .
N6 N 0.3416(12) 0.643(3) 0.5831(10) 0.228(8) Uani 1 1 d D . . . .
C23 C 0.3368(18) 0.669(4) 0.6251(11) 0.269(12) Uani 1 1 d D . . . .
H23A H 0.369530 0.682665 0.650773 0.323 Uiso 1 1 calc R U . . .
H23B H 0.320265 0.605531 0.633347 0.323 Uiso 1 1 calc R U . . .
C24 C 0.3047(13) 0.780(4) 0.6134(15) 0.278(14) Uani 1 1 d D . . . .
H24A H 0.302958 0.811600 0.641035 0.334 Uiso 1 1 calc R U . . .
H24B H 0.317968 0.838529 0.599679 0.334 Uiso 1 1 calc R U . . .
C25 C 0.2200(11) 0.824(3) 0.5731(11) 0.185(7) Uani 1 1 d D . . . .
H25A H 0.224431 0.887693 0.555130 0.221 Uiso 1 1 calc R U . . .
H25B H 0.223223 0.854763 0.602756 0.221 Uiso 1 1 calc R U . . .
C26 C 0.1683(12) 0.773(3) 0.5471(9) 0.180(7) Uani 1 1 d D . . . .
H26A H 0.164552 0.698651 0.560074 0.216 Uiso 1 1 calc R U . . .
H26B H 0.142041 0.826319 0.545748 0.216 Uiso 1 1 calc R U . . .
C27 C 0.3573(18) 0.526(3) 0.5839(16) 0.275(13) Uani 1 1 d D . . . .
H27A H 0.389023 0.517328 0.611354 0.330 Uiso 1 1 calc R U . . .
H27B H 0.364553 0.515659 0.556982 0.330 Uiso 1 1 calc R U . . .
C28 C 0.3247(17) 0.423(5) 0.5840(9) 0.268(16) Uani 1 1 d D . . . .
H28A H 0.343764 0.351952 0.595767 0.322 Uiso 1 1 calc R U . . .
H28B H 0.304070 0.439798 0.600420 0.322 Uiso 1 1 calc R U . . .
C29 C 0.2663(8) 0.328(3) 0.5262(3) 0.218(15) Uani 1 1 d D . . . .
H29A H 0.245301 0.333303 0.542907 0.261 Uiso 1 1 calc R U . . .
H29B H 0.285875 0.256803 0.535507 0.261 Uiso 1 1 calc R U . . .
C30 C 0.3769(16) 0.727(5) 0.5802(14) 0.279(14) Uani 1 1 d D . . . .
H30A H 0.410469 0.711768 0.604298 0.335 Uiso 1 1 calc R U . . .
H30B H 0.367262 0.805678 0.584474 0.335 Uiso 1 1 calc R U . . .
C31 C 0.3764(14) 0.715(6) 0.5323(14) 0.34(3) Uani 1 1 d D . . . .
H31A H 0.404442 0.758726 0.531442 0.409 Uiso 1 1 calc R U . . .
H31B H 0.380180 0.633999 0.525962 0.409 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
1 2 -2 0.1576
-1 0 -1 0.0242
1 0 1 0.0301
2 1 -20 0.0301
0 0 19 0.0328
0 6 13 0.1148
0 -6 -13 0.1078
9 4 9 0.0809
-17 0 0 0.0330
17 0 1 0.0257
-10 0 21 0.0216
0 -7 7 0.1340
10 0 -21 0.0331
-2 -3 18 0.0644
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
N1 U1 Si1 73.1(2) . . ?
N1 U1 N2 64.7(3) . 7 ?
N2 U1 Si1 91.2(2) 7 . ?
N3 U1 Si1 27.5(3) . . ?
N3 U1 N1 79.8(4) . . ?
N3 U1 N2 117.5(4) . 7 ?
N3 U1 N4 116.3(5) . . ?
N3 U1 N5 113.3(4) . . ?
N4 U1 Si1 108.6(4) . . ?
N4 U1 N1 149.5(4) . . ?
N4 U1 N2 84.8(4) . 7 ?
N5 U1 Si1 139.1(3) . . ?
N5 U1 N1 93.8(3) . . ?
N5 U1 N2 118.5(3) . 7 ?
N5 U1 N4 101.9(4) . . ?
N3 Si1 U1 39.3(4) . . ?
N3 Si1 C5 102.7(7) . . ?
N3 Si1 C6 114.2(8) . . ?
N3 Si1 C7 115.2(9) . . ?
C5 Si1 U1 67.1(4) . . ?
C6 Si1 U1 112.7(6) . . ?
C6 Si1 C5 112.6(8) . . ?
C6 Si1 C7 107.1(11) . . ?
C7 Si1 U1 139.4(9) . . ?
C7 Si1 C5 104.8(9) . . ?
N3 Si2 C8 113.6(9) . . ?
N3 Si2 C9 111.3(8) . . ?
N3 Si2 C10 112.4(7) . . ?
C8 Si2 C9 106.2(11) . . ?
C8 Si2 C10 104.1(11) . . ?
C10 Si2 C9 108.8(10) . . ?
N4 Si3 C11 112.5(8) . . ?
N4 Si3 C12 111.0(7) . . ?
N4 Si3 C13 116.3(9) . . ?
C12 Si3 C11 109.2(10) . . ?
C12 Si3 C13 103.1(11) . . ?
C13 Si3 C11 104.1(9) . . ?
N4 Si4 C14 110.1(7) . . ?
N4 Si4 C15 115.4(9) . . ?
N4 Si4 C16 115.9(11) . . ?
C14 Si4 C15 105.4(11) . . ?
C14 Si4 C16 105.5(9) . . ?
C16 Si4 C15 103.6(12) . . ?
N5 Si5 C17 109.2(7) . . ?
N5 Si5 C18 114.3(8) . . ?
N5 Si5 C19 113.8(8) . . ?
C18 Si5 C17 108.7(9) . . ?
C19 Si5 C17 106.9(11) . . ?
C19 Si5 C18 103.6(10) . . ?
N5 Si6 C20 112.4(7) . . ?
N5 Si6 C21 111.9(6) . . ?
N5 Si6 C22 114.6(7) . . ?
C20 Si6 C21 108.4(9) . . ?
C20 Si6 C22 105.7(8) . . ?
C21 Si6 C22 103.2(7) . . ?
C1 N1 U1 120.7(8) . . ?
C4 N1 U1 123.7(8) . . ?
C4 N1 C1 115.5(10) . . ?
C1 N2 U1 118.8(7) . 7 ?
C2 N2 U1 125.7(9) . 7 ?
C2 N2 C1 115.5(10) . . ?
Si1 N3 U1 113.2(5) . . ?
Si1 N3 Si2 117.6(8) . . ?
Si2 N3 U1 128.7(7) . . ?
Si3 N4 U1 122.4(8) . . ?
Si4 N4 U1 123.2(6) . . ?
Si4 N4 Si3 114.3(8) . . ?
Si5 N5 U1 118.2(5) . . ?
Si6 N5 U1 124.1(5) . . ?
Si6 N5 Si5 117.6(6) . . ?
N2 C1 N1 124.3(10) . . ?
C1 C1 N1 116.6(13) 7 . ?
C1 C1 N2 119.2(11) 7 . ?
N2 C2 H2 118.1 . . ?
N2 C2 C3 123.9(14) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 H3 120.9 . . ?
C4 C3 C2 118.3(13) . . ?
C4 C3 H3 120.9 . . ?
N1 C4 C3 122.6(12) . . ?
N1 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si5 C17 H17A 109.5 . . ?
Si5 C17 H17B 109.5 . . ?
Si5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si5 C18 H18A 109.5 . . ?
Si5 C18 H18B 109.5 . . ?
Si5 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si5 C19 H19A 109.5 . . ?
Si5 C19 H19B 109.5 . . ?
Si5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si6 C20 H20A 109.5 . . ?
Si6 C20 H20B 109.5 . . ?
Si6 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si6 C21 H21A 109.5 . . ?
Si6 C21 H21B 109.5 . . ?
Si6 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si6 C22 H22A 109.5 . . ?
Si6 C22 H22B 109.5 . . ?
Si6 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 K1 O1 139.8(14) 2_556 . ?
O1 K1 O3 120.3(8) 2_556 . ?
O1 K1 O3 120.3(8) . 2_556 ?
O1 K1 O3 96.2(8) 2_556 2_556 ?
O1 K1 O3 96.2(8) . . ?
O1 K1 N6 58.4(9) . . ?
O1 K1 N6 58.4(9) 2_556 2_556 ?
O1 K1 N6 125.0(9) . 2_556 ?
O1 K1 N6 125.0(9) 2_556 . ?
O1 K1 C25 23.0(6) 2_556 2_556 ?
O1 K1 C25 122.7(9) . 2_556 ?
O2 K1 O1 100.2(9) 2_556 . ?
O2 K1 O1 100.2(9) . 2_556 ?
O2 K1 O1 61.9(8) . . ?
O2 K1 O1 61.9(8) 2_556 2_556 ?
O2 K1 O2 129.4(14) 2_556 . ?
O2 K1 O3 96.9(8) 2_556 . ?
O2 K1 O3 130.0(9) 2_556 2_556 ?
O2 K1 O3 96.9(9) . 2_556 ?
O2 K1 O3 130.0(9) . . ?
O2 K1 N6 63.7(8) . 2_556 ?
O2 K1 N6 63.7(8) 2_556 . ?
O2 K1 N6 120.3(9) . . ?
O2 K1 N6 120.3(9) 2_556 2_556 ?
O2 K1 C25 106.4(8) . 2_556 ?
O2 K1 C25 41.0(7) 2_556 2_556 ?
O3 K1 O3 53.8(9) 2_556 . ?
O3 K1 C25 122.5(7) . 2_556 ?
O3 K1 C25 116.6(7) 2_556 2_556 ?
N6 K1 O3 112.6(8) 2_556 . ?
N6 K1 O3 112.6(8) . 2_556 ?
N6 K1 O3 59.3(8) 2_556 2_556 ?
N6 K1 O3 59.3(8) . . ?
N6 K1 N6 171.9(13) 2_556 . ?
N6 K1 C25 104.6(8) . 2_556 ?
N6 K1 C25 80.0(8) 2_556 2_556 ?
C24 O1 K1 117(3) . . ?
C25 O1 K1 109.1(19) . . ?
C25 O1 C24 112(3) . . ?
C26 O2 K1 118(2) . . ?
C26 O2 C31 112(3) . 2_556 ?
C31 O2 K1 113(2) 2_556 . ?
C28 O3 K1 112(3) . . ?
C28 O3 C29 105(3) . . ?
C29 O3 K1 118(2) . . ?
C23 N6 K1 115(2) . . ?
C23 N6 C30 107(2) . . ?
C27 N6 K1 105(3) . . ?
C27 N6 C23 110(2) . . ?
C27 N6 C30 113(4) . . ?
C30 N6 K1 108(2) . . ?
N6 C23 H23A 111.0 . . ?
N6 C23 H23B 111.0 . . ?
N6 C23 C24 104(3) . . ?
H23A C23 H23B 109.0 . . ?
C24 C23 H23A 111.0 . . ?
C24 C23 H23B 111.0 . . ?
O1 C24 C23 103(3) . . ?
O1 C24 H24A 111.1 . . ?
O1 C24 H24B 111.1 . . ?
C23 C24 H24A 111.1 . . ?
C23 C24 H24B 111.1 . . ?
H24A C24 H24B 109.1 . . ?
O1 C25 H25A 109.3 . . ?
O1 C25 H25B 109.3 . . ?
O1 C25 C26 112(3) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
O2 C26 C25 98(2) . . ?
O2 C26 H26A 112.3 . . ?
O2 C26 H26B 112.3 . . ?
C25 C26 H26A 112.3 . . ?
C25 C26 H26B 112.3 . . ?
H26A C26 H26B 109.9 . . ?
N6 C27 H27A 106.8 . . ?
N6 C27 H27B 106.8 . . ?
N6 C27 C28 122(4) . . ?
H27A C27 H27B 106.6 . . ?
C28 C27 H27A 106.8 . . ?
C28 C27 H27B 106.8 . . ?
O3 C28 C27 94(3) . . ?
O3 C28 H28A 113.0 . . ?
O3 C28 H28B 113.0 . . ?
C27 C28 H28A 113.0 . . ?
C27 C28 H28B 113.0 . . ?
H28A C28 H28B 110.4 . . ?
O3 C29 C29 107.3(13) . 2_556 ?
O3 C29 H29A 110.3 . . ?
O3 C29 H29B 110.3 . . ?
C29 C29 H29A 110.3 2_556 . ?
C29 C29 H29B 110.3 2_556 . ?
H29A C29 H29B 108.5 . . ?
N6 C30 H30A 110.1 . . ?
N6 C30 H30B 110.1 . . ?
N6 C30 C31 108(3) . . ?
H30A C30 H30B 108.4 . . ?
C31 C30 H30A 110.1 . . ?
C31 C30 H30B 110.1 . . ?
O2 C31 C30 110(4) 2_556 . ?
O2 C31 H31A 109.7 2_556 . ?
O2 C31 H31B 109.7 2_556 . ?
C30 C31 H31A 109.7 . . ?
C30 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
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 Si1 3.412(5) . ?
U1 N1 2.494(11) . ?
U1 N2 2.516(9) 7 ?
U1 N3 2.350(13) . ?
U1 N4 2.361(13) . ?
U1 N5 2.360(10) . ?
Si1 N3 1.717(14) . ?
Si1 C5 2.011(16) . ?
Si1 C6 1.85(2) . ?
Si1 C7 1.884(17) . ?
Si2 N3 1.742(12) . ?
Si2 C8 1.81(2) . ?
Si2 C9 1.897(19) . ?
Si2 C10 1.891(18) . ?
Si3 N4 1.755(13) . ?
Si3 C11 1.905(17) . ?
Si3 C12 1.88(2) . ?
Si3 C13 1.878(19) . ?
Si4 N4 1.732(17) . ?
Si4 C14 1.858(17) . ?
Si4 C15 1.90(2) . ?
Si4 C16 1.879(19) . ?
Si5 N5 1.734(10) . ?
Si5 C17 1.895(17) . ?
Si5 C18 1.867(18) . ?
Si5 C19 1.84(2) . ?
Si6 N5 1.706(11) . ?
Si6 C20 1.877(18) . ?
Si6 C21 1.883(14) . ?
Si6 C22 1.900(17) . ?
N1 C1 1.406(13) . ?
N1 C4 1.349(17) . ?
N2 C1 1.401(15) . ?
N2 C2 1.321(17) . ?
C1 C1 1.37(2) 7 ?
C2 H2 0.9500 . ?
C2 C3 1.39(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.38(2) . ?
C4 H4 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
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 . ?
K1 O1 2.70(2) . ?
K1 O1 2.70(2) 2_556 ?
K1 O2 2.70(3) 2_556 ?
K1 O2 2.70(3) . ?
K1 O3 3.11(3) 2_556 ?
K1 O3 3.11(3) . ?
K1 N6 2.91(3) 2_556 ?
K1 N6 2.91(3) . ?
K1 C25 3.44(3) 2_556 ?
O1 C24 1.428(19) . ?
O1 C25 1.421(18) . ?
O2 C26 1.473(18) . ?
O2 C31 1.45(6) 2_556 ?
O3 C28 1.404(14) . ?
O3 C29 1.405(12) . ?
N6 C23 1.453(14) . ?
N6 C27 1.450(14) . ?
N6 C30 1.475(14) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.557(19) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.530(19) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.544(16) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C29 1.550(15) 2_556 ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.546(19) . ?
C31 H31A 0.9900 . ?
C31 H31B 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 Si1 N3 Si2 -172.6(13) . . . . ?
U1 N1 C1 N2 178.7(8) . . . . ?
U1 N1 C1 C1 0.4(16) . . . 7 ?
U1 N1 C4 C3 -177.5(11) . . . . ?
U1 N2 C1 N1 179.7(8) 7 . . . ?
U1 N2 C1 C1 -2.0(16) 7 . . 7 ?
U1 N2 C2 C3 179.8(11) 7 . . . ?
N2 C2 C3 C4 0(2) . . . . ?
C1 N1 C4 C3 0.2(18) . . . . ?
C1 N2 C2 C3 1(2) . . . . ?
C2 N2 C1 N1 -1.6(16) . . . . ?
C2 N2 C1 C1 176.7(13) . . . 7 ?
C2 C3 C4 N1 -1(2) . . . . ?
C4 N1 C1 N2 0.9(16) . . . . ?
C4 N1 C1 C1 -177.4(12) . . . 7 ?
C5 Si1 N3 U1 -25.3(8) . . . . ?
C5 Si1 N3 Si2 162.1(8) . . . . ?
C6 Si1 N3 U1 96.9(10) . . . . ?
C6 Si1 N3 Si2 -75.7(11) . . . . ?
C7 Si1 N3 U1 -138.6(10) . . . . ?
C7 Si1 N3 Si2 48.9(14) . . . . ?
C8 Si2 N3 U1 -137.5(11) . . . . ?
C8 Si2 N3 Si1 33.7(13) . . . . ?
C9 Si2 N3 U1 102.6(12) . . . . ?
C9 Si2 N3 Si1 -86.1(13) . . . . ?
C10 Si2 N3 U1 -19.7(13) . . . . ?
C10 Si2 N3 Si1 151.6(10) . . . . ?
C11 Si3 N4 U1 -96.6(10) . . . . ?
C11 Si3 N4 Si4 82.0(11) . . . . ?
C12 Si3 N4 U1 26.0(10) . . . . ?
C12 Si3 N4 Si4 -155.3(8) . . . . ?
C13 Si3 N4 U1 143.4(11) . . . . ?
C13 Si3 N4 Si4 -37.9(13) . . . . ?
C14 Si4 N4 U1 7.1(10) . . . . ?
C14 Si4 N4 Si3 -171.6(8) . . . . ?
C15 Si4 N4 U1 126.2(10) . . . . ?
C15 Si4 N4 Si3 -52.4(11) . . . . ?
C16 Si4 N4 U1 -112.5(10) . . . . ?
C16 Si4 N4 Si3 68.9(11) . . . . ?
C17 Si5 N5 U1 9.8(11) . . . . ?
C17 Si5 N5 Si6 -173.0(10) . . . . ?
C18 Si5 N5 U1 131.8(9) . . . . ?
C18 Si5 N5 Si6 -51.1(12) . . . . ?
C19 Si5 N5 U1 -109.5(9) . . . . ?
C19 Si5 N5 Si6 67.7(11) . . . . ?
C20 Si6 N5 U1 -97.6(9) . . . . ?
C20 Si6 N5 Si5 85.5(10) . . . . ?
C21 Si6 N5 U1 24.6(10) . . . . ?
C21 Si6 N5 Si5 -152.3(8) . . . . ?
C22 Si6 N5 U1 141.7(8) . . . . ?
C22 Si6 N5 Si5 -35.3(10) . . . . ?
K1 O1 C24 C23 -65(4) . . . . ?
K1 O1 C25 C26 61(3) . . . . ?
K1 O2 C26 C25 48(3) . . . . ?
K1 O3 C28 C27 -55(3) . . . . ?
K1 O3 C29 C29 52(3) . . . 2_556 ?
K1 N6 C23 C24 -45(3) . . . . ?
K1 N6 C27 C28 -59(4) . . . . ?
K1 N6 C30 C31 -47(5) . . . . ?
O1 C25 C26 O2 -71(3) . . . . ?
N6 C23 C24 O1 69(4) . . . . ?
N6 C27 C28 O3 84(5) . . . . ?
N6 C30 C31 O2 71(6) . . . 2_556 ?
C23 N6 C27 C28 65(5) . . . . ?
C23 N6 C30 C31 -171(4) . . . . ?
C24 O1 C25 C26 -168(3) . . . . ?
C25 O1 C24 C23 168(3) . . . . ?
C27 N6 C23 C24 -163(4) . . . . ?
C27 N6 C30 C31 68(6) . . . . ?
C28 O3 C29 C29 177(3) . . . 2_556 ?
C29 O3 C28 C27 175(3) . . . . ?
C30 N6 C23 C24 75(5) . . . . ?
C30 N6 C27 C28 -176(3) . . . . ?
C31 O2 C26 C25 -178(3) 2_556 . . . ?
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
1.0035 1.9982 -2.0004 -0.1464 0.2210 -0.0922
-0.9989 0.0009 -1.0009 -0.0330 0.0285 0.0817
0.9989 -0.0009 1.0009 0.0330 -0.0285 -0.0817
1.9346 0.6448 -19.6926 -0.8685 0.1137 0.4825
0.2659 -0.1491 18.8334 0.7985 -0.1045 -0.5929
-0.1697 5.7071 12.5413 0.3830 0.6265 -0.6788
0.2064 -5.7095 -12.5510 -0.3837 -0.6276 0.6774
8.9862 4.3946 8.5545 0.1627 0.2669 -0.9499
-17.4051 -0.0716 -0.4332 0.1470 0.4138 0.8984
17.0332 -0.0835 1.2958 -0.1029 -0.4269 -0.8984
-9.9278 0.2497 20.8788 0.9703 0.1802 -0.1613
0.1888 -7.0559 6.8457 0.4726 -0.8695 0.1435
10.2666 -0.1854 -20.8400 -0.9735 -0.1810 0.1396
-2.4228 -3.3504 17.9669 0.8708 -0.4150 -0.2635
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 0.250 0.074 0.500 347.6 49.8 '1 hexane'
2 -0.250 -0.074 0.500 347.6 50.1 '1 hexane'
3 0.250 0.426 1.000 347.6 50.1 '1 hexane'
4 -0.250 0.574 0.000 347.6 49.8 '1 hexane'
