# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

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

data_dkm206_sq
_database_code_depnum_ccdc_archive 'CCDC 2181473'
loop_
_audit_author_name
_audit_author_address
'rosario scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_audit_creation_date             2020-06-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H114 N10 Si12 U2'
_chemical_formula_sum            'C44 H114 N10 Si12 U2'
_chemical_formula_weight         1596.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H130 N10 O2 Si12 U2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
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'

_cell_length_a                   24.4164(5)
_cell_length_b                   11.4199(2)
_cell_length_c                   29.7959(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.683(2)
_cell_angle_gamma                90
_cell_volume                     7958.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5760
_cell_measurement_theta_min      3.7770
_shelx_estimated_absorpt_T_max   0.338
_shelx_estimated_absorpt_T_min   0.131
_exptl_absorpt_coefficient_mu    13.339
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
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_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3200
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 -1 0.0286
0 7 -1 0.1007
-16 0 9 0.0723
-1 -7 2 0.1520
-15 0 0 0.0850
-3 0 -17 0.0513
0 0 18 0.0597
11 0 10 0.0469
-15 1 9 0.0693
-2 -6 -9 0.1235
-14 2 -2 0.0722
1 2 -18 0.0645
-8 -2 18 0.0787
3 -3 16 0.0799
0 6 12 0.0847
5 6 9 0.0825
-15 1 11 0.0697

_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.104
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
2.0001 0.0002 -0.9995 -0.0088 0.0011 -0.1269
0.2598 7.3942 -1.4093 -0.6083 -0.7937 0.0098
-15.5733 -0.0372 8.8917 0.0274 0.0339 0.9991
-0.7481 -7.3839 1.6861 0.6082 0.7935 0.0215
-15.1750 0.3759 0.0555 0.3311 -0.3125 0.8903
-2.7459 0.2812 -17.2703 0.7257 -0.6879 -0.0091
0.2280 -0.2330 18.4348 -0.7153 0.6783 0.1682
10.5423 -0.3863 10.1065 -0.6210 0.5878 -0.5186
-15.3104 1.4313 8.5319 -0.0954 -0.1227 0.9878
-2.4455 -6.2601 -8.6387 0.9584 0.2845 0.0244
-14.0934 1.7238 -2.3592 0.2808 -0.5145 0.8102
1.3576 2.4120 -17.9252 0.4630 -0.8520 -0.2444
-7.5154 -1.8547 18.2743 -0.3775 0.6958 0.6111
3.1216 -2.5662 15.9031 -0.4774 0.8779 -0.0385
-0.0538 5.8009 11.5446 -0.9723 -0.1810 0.1482
4.5445 5.7161 8.9358 -0.9725 -0.1807 -0.1471
-14.8002 1.4473 10.7279 -0.1962 -0.0376 0.9799

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9407
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.828
_diffrn_reflns_theta_min         4.143
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00 -38.00   1.00    4.00    --  -40.91 112.00   6.00   25
  2  ω     62.00  87.00   1.00    4.00    --   40.91-112.00 -86.00   25
  3  ω    104.00 167.00   1.00   16.00    --  105.15 112.00   6.00   63
  4  ω     69.00  96.00   1.00   16.00    --  105.15-112.00 -86.00   27
  5  ω   -115.00 -25.00   1.00    4.00    --  -40.91 -38.00 150.00   90
  6  ω     39.00  95.00   1.00    4.00    --   40.91-125.00-180.00   56
  7  ω    -32.00  59.00   1.00    4.00    --   40.91 -38.00 -30.00   91
  8  ω     35.00 109.00   1.00   16.00    --  105.15-111.00 120.00   74
  9  ω     44.00 109.00   1.00   16.00    --  105.15-111.00   0.00   65
 10  ω    109.00 168.00   1.00   16.00    --  105.15 111.00 -90.00   59
 11  ω     36.00  63.00   1.00   16.00    --  105.15-111.00 -30.00   27
 12  ω    104.00 164.00   1.00   16.00    --  105.15  77.00  90.00   60
 13  ω    105.00 170.00   1.00   16.00    --  105.15 111.00  30.00   65
 14  ω    121.00 147.00   1.00   16.00    --  105.15 111.00-150.00   26
 15  ω    127.00 170.00   1.00   16.00    --  105.15  30.00-180.00   43
 16  ω    107.00 169.00   1.00   16.00    --  105.15  77.00-120.00   62
;
_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      -0.0241706000
_diffrn_orient_matrix_UB_12      -0.0889642000
_diffrn_orient_matrix_UB_13      -0.0396281000
_diffrn_orient_matrix_UB_21      0.0182147000
_diffrn_orient_matrix_UB_22      -0.1012525000
_diffrn_orient_matrix_UB_23      0.0352872000
_diffrn_orient_matrix_UB_31      -0.0585035000
_diffrn_orient_matrix_UB_32      0.0052741000
_diffrn_orient_matrix_UB_33      0.0099141000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8306
_reflns_number_total             9407
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         9407
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0672P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0879
_refine_special_details          
;
 Refined as a 3-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4791(19)
 0.1442(11) 0.3767(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
3.b 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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.41098(2) 0.57013(2) 0.39507(2) 0.02373(7) Uani 1 1 d . . . . .
Si1 Si 0.35736(6) 0.83326(13) 0.33787(5) 0.0360(3) Uani 1 1 d . . . . .
Si2 Si 0.43197(6) 0.86358(13) 0.43488(5) 0.0350(3) Uani 1 1 d . . . . .
Si3 Si 0.26774(6) 0.56921(13) 0.40032(5) 0.0362(3) Uani 1 1 d . . . . .
Si4 Si 0.28973(6) 0.39790(14) 0.33382(6) 0.0415(3) Uani 1 1 d . . . . .
Si5 Si 0.48926(5) 0.35696(13) 0.36358(4) 0.0348(3) Uani 1 1 d . . . . .
Si6 Si 0.48661(6) 0.56585(14) 0.30507(5) 0.0369(3) Uani 1 1 d . . . . .
N1 N 0.51068(16) 0.5793(4) 0.45019(13) 0.0270(8) Uani 1 1 d . . . . .
N2 N 0.57675(15) 0.5261(4) 0.52735(13) 0.0284(8) Uani 1 1 d . . . . .
N3 N 0.39965(17) 0.7681(4) 0.38917(13) 0.0332(9) Uani 1 1 d . . . . .
N4 N 0.31755(15) 0.5080(4) 0.37457(14) 0.0303(8) Uani 1 1 d . . . . .
N5 N 0.46304(16) 0.4987(4) 0.34875(13) 0.0304(8) Uani 1 1 d . . . . .
C1 C 0.52193(19) 0.5267(4) 0.49477(15) 0.0261(8) Uani 1 1 d . . . . .
C2 C 0.55329(19) 0.6353(5) 0.44044(15) 0.0305(9) Uani 1 1 d . . . . .
H2 H 0.546722 0.670237 0.410415 0.037 Uiso 1 1 calc R U . . .
C3 C 0.60769(19) 0.6454(5) 0.47252(17) 0.0369(11) Uani 1 1 d . . . . .
H3 H 0.637210 0.689161 0.465404 0.044 Uiso 1 1 calc R U . . .
C4 C 0.61659(19) 0.5883(4) 0.51530(17) 0.0311(10) Uani 1 1 d . . . . .
H4 H 0.653362 0.593955 0.537316 0.037 Uiso 1 1 calc R U . . .
C5 C 0.3356(2) 0.7185(6) 0.29113(19) 0.0455(12) Uani 1 1 d . . . . .
H5A H 0.367555 0.664699 0.293535 0.068 Uiso 1 1 calc R U . . .
H5B H 0.324931 0.756013 0.260260 0.068 Uiso 1 1 calc R U . . .
H5C H 0.302781 0.674662 0.295177 0.068 Uiso 1 1 calc R U . . .
C6 C 0.2887(2) 0.9004(5) 0.3433(2) 0.0489(14) Uani 1 1 d . . . . .
H6A H 0.277645 0.862028 0.368820 0.073 Uiso 1 1 calc R U . . .
H6B H 0.258371 0.889787 0.313861 0.073 Uiso 1 1 calc R U . . .
H6C H 0.294547 0.984219 0.350092 0.073 Uiso 1 1 calc R U . . .
C7 C 0.3945(3) 0.9575(6) 0.3164(2) 0.0479(13) Uani 1 1 d . . . . .
H7A H 0.391915 1.028822 0.333981 0.072 Uiso 1 1 calc R U . . .
H7B H 0.376006 0.970644 0.282999 0.072 Uiso 1 1 calc R U . . .
H7C H 0.434763 0.937292 0.321196 0.072 Uiso 1 1 calc R U . . .
C8 C 0.4477(3) 0.7875(6) 0.49267(19) 0.0487(13) Uani 1 1 d . . . . .
H8A H 0.415262 0.797343 0.505571 0.073 Uiso 1 1 calc R U . . .
H8B H 0.482088 0.821306 0.514306 0.073 Uiso 1 1 calc R U . . .
H8C H 0.453836 0.703919 0.488457 0.073 Uiso 1 1 calc R U . . .
C9 C 0.3861(3) 0.9915(5) 0.4405(2) 0.0462(12) Uani 1 1 d . . . . .
H9A H 0.375445 1.035746 0.411059 0.069 Uiso 1 1 calc R U . . .
H9B H 0.407399 1.042448 0.466000 0.069 Uiso 1 1 calc R U . . .
H9C H 0.351447 0.963090 0.447300 0.069 Uiso 1 1 calc R U . . .
C10 C 0.5006(3) 0.9258(5) 0.4281(3) 0.0491(14) Uani 1 1 d . . . . .
H10A H 0.527186 0.861881 0.427736 0.074 Uiso 1 1 calc R U . . .
H10B H 0.517679 0.978276 0.454464 0.074 Uiso 1 1 calc R U . . .
H10C H 0.492543 0.969748 0.398703 0.074 Uiso 1 1 calc R U . . .
C11 C 0.3035(2) 0.6702(5) 0.4495(2) 0.0456(13) Uani 1 1 d . . . . .
H11A H 0.334661 0.628601 0.472007 0.068 Uiso 1 1 calc R U . . .
H11B H 0.275625 0.697004 0.465184 0.068 Uiso 1 1 calc R U . . .
H11C H 0.319097 0.737841 0.437001 0.068 Uiso 1 1 calc R U . . .
C12 C 0.2101(2) 0.6552(6) 0.3580(2) 0.0469(13) Uani 1 1 d . . . . .
H12A H 0.224838 0.687192 0.333266 0.070 Uiso 1 1 calc R U . . .
H12B H 0.197701 0.719449 0.374613 0.070 Uiso 1 1 calc R U . . .
H12C H 0.177481 0.603753 0.344039 0.070 Uiso 1 1 calc R U . . .
C13 C 0.2285(3) 0.4575(6) 0.4256(3) 0.0534(15) Uani 1 1 d . . . . .
H13A H 0.205953 0.407021 0.400419 0.080 Uiso 1 1 calc R U . . .
H13B H 0.203049 0.497377 0.440727 0.080 Uiso 1 1 calc R U . . .
H13C H 0.256145 0.409771 0.448715 0.080 Uiso 1 1 calc R U . . .
C14 C 0.2148(3) 0.4251(7) 0.2964(3) 0.067(2) Uani 1 1 d . . . . .
H14A H 0.188201 0.414043 0.315185 0.101 Uiso 1 1 calc R U . . .
H14B H 0.205462 0.369962 0.270095 0.101 Uiso 1 1 calc R U . . .
H14C H 0.211676 0.505436 0.284400 0.101 Uiso 1 1 calc R U . . .
C15 C 0.2875(3) 0.2530(6) 0.3629(3) 0.066(2) Uani 1 1 d . . . . .
H15A H 0.324782 0.237357 0.385445 0.098 Uiso 1 1 calc R U . . .
H15B H 0.278631 0.191032 0.339132 0.098 Uiso 1 1 calc R U . . .
H15C H 0.257989 0.254871 0.379259 0.098 Uiso 1 1 calc R U . . .
C16 C 0.3304(3) 0.3816(7) 0.2898(2) 0.0552(16) Uani 1 1 d . . . . .
H16A H 0.317306 0.440608 0.265181 0.083 Uiso 1 1 calc R U . . .
H16B H 0.323832 0.303192 0.275916 0.083 Uiso 1 1 calc R U . . .
H16C H 0.371260 0.392377 0.305249 0.083 Uiso 1 1 calc R U . . .
C17 C 0.4460(2) 0.2825(5) 0.39762(18) 0.0417(11) Uani 1 1 d . . . . .
H17A H 0.454167 0.317973 0.428797 0.063 Uiso 1 1 calc R U . . .
H17B H 0.455804 0.199102 0.400767 0.063 Uiso 1 1 calc R U . . .
H17C H 0.405221 0.291308 0.381169 0.063 Uiso 1 1 calc R U . . .
C18 C 0.5657(2) 0.3502(6) 0.4007(2) 0.0483(14) Uani 1 1 d . . . . .
H18A H 0.590151 0.388984 0.384275 0.072 Uiso 1 1 calc R U . . .
H18B H 0.577329 0.268173 0.406545 0.072 Uiso 1 1 calc R U . . .
H18C H 0.569385 0.389872 0.430565 0.072 Uiso 1 1 calc R U . . .
C19 C 0.4826(3) 0.2594(6) 0.3119(2) 0.0538(15) Uani 1 1 d . . . . .
H19A H 0.443561 0.263734 0.290875 0.081 Uiso 1 1 calc R U . . .
H19B H 0.491188 0.178483 0.322560 0.081 Uiso 1 1 calc R U . . .
H19C H 0.509634 0.284759 0.295025 0.081 Uiso 1 1 calc R U . . .
C20 C 0.4413(3) 0.5245(7) 0.24501(18) 0.0513(15) Uani 1 1 d . . . . .
H20A H 0.440151 0.439030 0.241938 0.077 Uiso 1 1 calc R U . . .
H20B H 0.457644 0.558397 0.221494 0.077 Uiso 1 1 calc R U . . .
H20C H 0.402426 0.554455 0.240187 0.077 Uiso 1 1 calc R U . . .
C21 C 0.4869(2) 0.7294(5) 0.3101(2) 0.0459(13) Uani 1 1 d . . . . .
H21A H 0.455781 0.762076 0.284703 0.069 Uiso 1 1 calc R U . . .
H21B H 0.523563 0.760021 0.307944 0.069 Uiso 1 1 calc R U . . .
H21C H 0.481579 0.751602 0.340355 0.069 Uiso 1 1 calc R U . . .
C22 C 0.5631(3) 0.5284(7) 0.3078(2) 0.0593(18) Uani 1 1 d . . . . .
H22A H 0.588391 0.548730 0.338736 0.089 Uiso 1 1 calc R U . . .
H22B H 0.574376 0.572732 0.283679 0.089 Uiso 1 1 calc R U . . .
H22C H 0.566049 0.444344 0.302230 0.089 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Si5 3.3896(13) . ?
U1 N1 2.518(4) . ?
U1 N2 2.499(4) 5_666 ?
U1 N3 2.278(5) . ?
U1 N4 2.298(4) . ?
U1 N5 2.279(4) . ?
Si1 N3 1.747(4) . ?
Si1 C5 1.875(6) . ?
Si1 C6 1.892(6) . ?
Si1 C7 1.890(6) . ?
Si2 N3 1.746(5) . ?
Si2 C8 1.868(6) . ?
Si2 C9 1.877(6) . ?
Si2 C10 1.883(6) . ?
Si3 N4 1.758(4) . ?
Si3 C11 1.872(6) . ?
Si3 C12 1.875(6) . ?
Si3 C13 1.877(6) . ?
Si4 N4 1.745(4) . ?
Si4 C14 1.874(7) . ?
Si4 C15 1.876(7) . ?
Si4 C16 1.867(6) . ?
Si5 N5 1.750(5) . ?
Si5 C17 1.867(5) . ?
Si5 C18 1.877(6) . ?
Si5 C19 1.871(6) . ?
Si6 N5 1.744(4) . ?
Si6 C20 1.874(6) . ?
Si6 C21 1.873(6) . ?
Si6 C22 1.895(6) . ?
N1 C1 1.411(6) . ?
N1 C2 1.323(6) . ?
N2 C1 1.410(6) . ?
N2 C4 1.334(6) . ?
C1 C1 1.344(9) 5_666 ?
C2 C3 1.401(7) . ?
C3 C4 1.392(7) . ?

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 Si5 72.18(9) . . ?
N2 U1 Si5 90.72(9) 5_666 . ?
N2 U1 N1 65.05(12) 5_666 . ?
N3 U1 Si5 139.20(9) . . ?
N3 U1 N1 94.72(14) . . ?
N3 U1 N2 119.18(14) . 5_666 ?
N3 U1 N4 101.33(14) . . ?
N3 U1 N5 112.65(14) . . ?
N4 U1 Si5 107.49(11) . . ?
N4 U1 N1 152.42(13) . . ?
N4 U1 N2 87.49(13) . 5_666 ?
N5 U1 Si5 28.16(11) . . ?
N5 U1 N1 78.87(13) . . ?
N5 U1 N2 117.59(13) . 5_666 ?
N5 U1 N4 114.36(14) . . ?
N3 Si1 C5 108.8(3) . . ?
N3 Si1 C6 114.4(3) . . ?
N3 Si1 C7 113.3(2) . . ?
C5 Si1 C6 106.1(3) . . ?
C5 Si1 C7 109.6(3) . . ?
C7 Si1 C6 104.3(3) . . ?
N3 Si2 C8 110.8(2) . . ?
N3 Si2 C9 114.1(2) . . ?
N3 Si2 C10 111.7(3) . . ?
C8 Si2 C9 104.5(3) . . ?
C8 Si2 C10 108.7(3) . . ?
C9 Si2 C10 106.7(3) . . ?
N4 Si3 C11 111.1(2) . . ?
N4 Si3 C12 113.2(2) . . ?
N4 Si3 C13 113.6(3) . . ?
C11 Si3 C12 107.2(3) . . ?
C11 Si3 C13 106.4(3) . . ?
C12 Si3 C13 104.7(3) . . ?
N4 Si4 C14 114.4(3) . . ?
N4 Si4 C15 111.8(3) . . ?
N4 Si4 C16 112.4(2) . . ?
C14 Si4 C15 105.6(4) . . ?
C16 Si4 C14 102.9(4) . . ?
C16 Si4 C15 109.1(4) . . ?
N5 Si5 U1 37.92(11) . . ?
N5 Si5 C17 109.6(2) . . ?
N5 Si5 C18 114.6(3) . . ?
N5 Si5 C19 113.8(2) . . ?
C17 Si5 U1 74.01(19) . . ?
C17 Si5 C18 106.5(2) . . ?
C17 Si5 C19 104.3(3) . . ?
C18 Si5 U1 114.2(2) . . ?
C19 Si5 U1 137.2(2) . . ?
C19 Si5 C18 107.3(3) . . ?
N5 Si6 C20 111.8(2) . . ?
N5 Si6 C21 111.9(2) . . ?
N5 Si6 C22 113.7(2) . . ?
C20 Si6 C22 106.7(3) . . ?
C21 Si6 C20 108.4(3) . . ?
C21 Si6 C22 103.9(3) . . ?
C1 N1 U1 119.1(3) . . ?
C2 N1 U1 123.4(3) . . ?
C2 N1 C1 117.4(4) . . ?
C1 N2 U1 118.5(3) . 5_666 ?
C4 N2 U1 125.4(3) . 5_666 ?
C4 N2 C1 115.7(4) . . ?
Si1 N3 U1 121.2(2) . . ?
Si2 N3 U1 122.8(2) . . ?
Si2 N3 Si1 116.0(3) . . ?
Si3 N4 U1 121.3(2) . . ?
Si4 N4 U1 124.5(2) . . ?
Si4 N4 Si3 114.2(2) . . ?
Si5 N5 U1 113.92(18) . . ?
Si6 N5 U1 130.9(2) . . ?
Si6 N5 Si5 114.8(2) . . ?
N2 C1 N1 122.7(4) . . ?
C1 C1 N1 117.3(5) 5_666 . ?
C1 C1 N2 120.0(5) 5_666 . ?
N1 C2 C3 122.8(4) . . ?
C4 C3 C2 117.1(4) . . ?
N2 C4 C3 124.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 Si5 N5 Si6 174.3(4) . . . . ?
U1 N1 C1 N2 178.9(3) . . . . ?
U1 N1 C1 C1 0.3(7) . . . 5_666 ?
U1 N1 C2 C3 176.2(4) . . . . ?
U1 N2 C1 N1 179.7(3) 5_666 . . . ?
U1 N2 C1 C1 -1.8(7) 5_666 . . 5_666 ?
U1 N2 C4 C3 -177.0(4) 5_666 . . . ?
N1 C2 C3 C4 3.1(8) . . . . ?
C1 N1 C2 C3 -1.0(7) . . . . ?
C1 N2 C4 C3 -3.9(7) . . . . ?
C2 N1 C1 N2 -3.8(7) . . . . ?
C2 N1 C1 C1 177.7(5) . . . 5_666 ?
C2 C3 C4 N2 -0.4(8) . . . . ?
C4 N2 C1 N1 6.1(7) . . . . ?
C4 N2 C1 C1 -175.4(5) . . . 5_666 ?
C5 Si1 N3 U1 -8.0(3) . . . . ?
C5 Si1 N3 Si2 172.1(2) . . . . ?
C6 Si1 N3 U1 110.5(3) . . . . ?
C6 Si1 N3 Si2 -69.4(3) . . . . ?
C7 Si1 N3 U1 -130.1(3) . . . . ?
C7 Si1 N3 Si2 50.0(3) . . . . ?
C8 Si2 N3 U1 -24.7(3) . . . . ?
C8 Si2 N3 Si1 155.2(3) . . . . ?
C9 Si2 N3 U1 -142.2(3) . . . . ?
C9 Si2 N3 Si1 37.6(3) . . . . ?
C10 Si2 N3 U1 96.7(3) . . . . ?
C10 Si2 N3 Si1 -83.4(3) . . . . ?
C11 Si3 N4 U1 -7.5(3) . . . . ?
C11 Si3 N4 Si4 171.7(3) . . . . ?
C12 Si3 N4 U1 113.2(3) . . . . ?
C12 Si3 N4 Si4 -67.6(3) . . . . ?
C13 Si3 N4 U1 -127.5(3) . . . . ?
C13 Si3 N4 Si4 51.8(4) . . . . ?
C14 Si4 N4 U1 -142.8(4) . . . . ?
C14 Si4 N4 Si3 38.0(4) . . . . ?
C15 Si4 N4 U1 97.3(3) . . . . ?
C15 Si4 N4 Si3 -81.9(3) . . . . ?
C16 Si4 N4 U1 -25.9(4) . . . . ?
C16 Si4 N4 Si3 154.9(3) . . . . ?
C17 Si5 N5 U1 21.1(3) . . . . ?
C17 Si5 N5 Si6 -164.6(3) . . . . ?
C18 Si5 N5 U1 -98.5(3) . . . . ?
C18 Si5 N5 Si6 75.8(3) . . . . ?
C19 Si5 N5 U1 137.5(3) . . . . ?
C19 Si5 N5 Si6 -48.2(4) . . . . ?
C20 Si6 N5 U1 -102.1(3) . . . . ?
C20 Si6 N5 Si5 84.9(3) . . . . ?
C21 Si6 N5 U1 19.7(4) . . . . ?
C21 Si6 N5 Si5 -153.3(3) . . . . ?
C22 Si6 N5 U1 137.1(4) . . . . ?
C22 Si6 N5 Si5 -36.0(4) . . . . ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.043 0.500 380 81 '2 THF'
2 0.750 -0.043 0.500 380 81 '2 THF'
3 0.250 0.457 0.000 380 81 '2 THF'
4 0.750 0.543 0.000 380 81 '2 THF'

_platon_squeeze_void_probe_radius 1.20
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 9.626
_oxdiff_exptl_absorpt_empirical_full_min 0.391
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4791(19) 11223 6702 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.1442(11) 0 1998 nmt 0.9976 -0.0300 -0.0051 0.0259 0.9913 0.0526 0.0039
-0.3192 0.9931
3 0.3767(15) 0 5857 nmt 0.9966 -0.0273 -0.0067 0.0111 0.9990 0.0134 0.0099
-0.0761 1.0025

_twin_special_details            
;
Component 2 rotated by 7.6525° 
around [-0.90 -0.02 0.44] (reciprocal) or [-0.99 -0.10 0.10] (direct)
Component 3 rotated by 2.1621° 
around [-0.78 -0.09 0.62] (reciprocal) or [-0.83 -0.47 0.31] (direct)
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mb63
_database_code_depnum_ccdc_archive 'CCDC 2181476'
loop_
_audit_author_name
_audit_author_address
'rosario scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_audit_creation_date             2022-02-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H36 K N2 O6, 2(C8 H6 N4)'
_chemical_formula_sum            'C34 H48 K N10 O6'
_chemical_formula_weight         731.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H56 N10 O7 K1'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.3683(13)
_cell_length_b                   20.5260(10)
_cell_length_c                   14.6910(10)
_cell_angle_alpha                90
_cell_angle_beta                 116.777(9)
_cell_angle_gamma                90
_cell_volume                     4137.3(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4781
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      71.5460
_cell_measurement_theta_min      3.8180
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.785
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1556
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 2 1 0.0719
0 -2 1 0.0648
1 -2 -1 0.0684
1 -2 0 0.0692
-1 1 1 0.0661
2 -1 1 0.0733
2 -1 -1 0.0781
-2 1 -1 0.0617
-2 1 1 0.0571
0 0 1 0.0636
5 -2 -9 0.0639
2 5 7 0.0753
8 0 -8 0.0711
-8 -5 0 0.0624
-8 0 8 0.0550
-10 -3 4 0.0521
3 10 3 0.0829
-7 -9 4 0.0466
-2 6 8 0.0697
-1 13 0 0.0685
3 10 -6 0.0697
0 -13 0 0.0550
-4 -8 8 0.0579
-2 8 -6 0.0594
-6 10 1 0.0612

_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.124
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
-1.0009 2.0020 0.9995 0.1318 -0.0327 0.1371
0.0017 -2.0000 0.9991 -0.1727 0.0430 0.0682
1.0009 -2.0020 -0.9995 -0.1318 0.0327 -0.1371
1.0011 -2.0011 0.0002 -0.1834 -0.0085 -0.0401
-1.0001 1.0016 0.9993 0.0712 0.0094 0.1227
2.0000 -1.0000 1.0009 -0.2367 -0.1845 0.0601
1.9996 -1.0018 -0.9985 -0.1335 -0.1021 -0.1340
-2.0000 1.0000 -1.0009 0.2367 0.1845 -0.0601
-1.9996 1.0018 0.9985 0.1335 0.1021 0.1340
0.0002 0.0009 0.9997 -0.0516 -0.0412 0.0970
5.1604 -2.4399 -9.3400 0.0136 0.0090 -0.9999
1.8264 5.1309 6.9174 -0.1608 -0.6705 0.7242
8.3842 -0.1109 -8.2269 -0.1038 -0.4339 -0.8949
-8.4181 -4.6845 0.1575 0.2328 0.9716 0.0434
-8.4351 0.0551 8.1814 0.1059 0.4429 0.8903
-9.6262 -3.3880 3.5063 0.2134 0.8910 0.4007
3.2403 10.3394 3.2112 0.2576 -0.8685 0.4235
-7.3772 -8.9659 3.6369 -0.2707 0.9122 0.3077
-2.4945 6.3218 8.2561 0.1111 -0.3752 0.9203
-0.5373 13.2902 0.0314 0.8356 -0.5116 0.2002
3.0289 10.1825 -6.1621 0.7455 -0.4562 -0.4859
0.4695 -13.2910 0.0906 -0.8377 0.5129 -0.1876
-4.0785 -7.5443 7.8637 -0.6085 0.3723 0.7008
-1.5884 7.7838 -6.0935 0.8844 0.0702 -0.4613
-6.1191 10.3213 1.4292 0.9314 0.0736 0.3565

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16648
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.755
_diffrn_reflns_theta_min         3.875
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00   1.00   1.00   10.00    --  -43.01  45.00 113.00   51
  2  ω   -115.00 -17.00   1.00   10.00    --  -43.01 -45.00 -36.00   98
  3  ω     -5.00  20.00   1.00   10.00    --   43.01 -45.00 -36.00   25
  4  ω     28.00 101.00   1.00   10.00    --   43.01  45.00 113.00   73
  5  ω     34.00 112.00   1.00   40.00    --  103.80 -45.00 -36.00   78
  6  ω     79.00 150.00   1.00   40.00    --  103.80  45.00 113.00   71
  7  ω    -86.00  -9.00   1.00   10.00    --  -43.01 125.00 120.00   77
  8  ω    -86.00  -7.00   1.00   10.00    --  -43.01 125.00-150.00   79
  9  ω    103.00 177.00   1.00   40.00    --  103.80  77.00   0.00   74
 10  ω     82.00 107.00   1.00   40.00    --  103.80 -94.00 -60.00   25
 11  ω     67.00 126.00   1.00   40.00    --  103.80 178.00-120.00   59
 12  ω    106.00 153.00   1.00   40.00    --  103.80  77.00  30.00   47
 13  ω     28.00  55.00   1.00   40.00    --  103.80-111.00  60.00   27
 14  ω     22.00  86.00   1.00   40.00    --  103.80 -94.00 -30.00   64
 15  ω     68.00 104.00   1.00   40.00    --  103.80-111.00  60.00   36
 16  ω     62.00  92.00   1.00   40.00    --  103.80 178.00   0.00   30
 17  ω     97.00 146.00   1.00   40.00    --  103.80 178.00   0.00   49
 18  ω     57.00 108.00   1.00   40.00    --  103.80-111.00 120.00   51
 19  ω     90.00 166.00   1.00   40.00    --  103.80  61.00 -30.00   76
 20  ω    135.00 174.00   1.00   40.00    --  103.80 111.00 -30.00   39
 21  ω     30.00  65.00   1.00   40.00    --  103.80 -94.00 -60.00   35
 22  ω     82.00 107.00   1.00   40.00    --  103.80 -94.00-180.00   25
 23  ω     42.00  69.00   1.00   40.00    --  103.80 -94.00 150.00   27
 24  ω     71.00 106.00   1.00   40.00    --  103.80 -94.00 150.00   35
 25  ω     40.00  65.00   1.00   40.00    --  103.80 -94.00-180.00   25
;
_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      -0.0622724000
_diffrn_orient_matrix_UB_12      0.0604758000
_diffrn_orient_matrix_UB_13      -0.0516624000
_diffrn_orient_matrix_UB_21      -0.0927311000
_diffrn_orient_matrix_UB_22      -0.0421458000
_diffrn_orient_matrix_UB_23      -0.0411889000
_diffrn_orient_matrix_UB_31      -0.0113423000
_diffrn_orient_matrix_UB_32      0.0143775000
_diffrn_orient_matrix_UB_33      0.0970292000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3014
_reflns_number_total             4046
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (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)'
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4046
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0420
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0703P)²+0.4689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1259
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O3_$1-C9_$1 \\sim O3_$1-C10_$1
 with sigma of 0.02
 C9-C9_$1 \\sim C10-C10_$1
 with sigma of 0.02
3. Others
 Sof(C10)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
K1 K 0.500000 0.48804(3) 0.250000 0.04723(17) Uani 1 2 d S T P A .
O1 O 0.39110(11) 0.41714(7) 0.32598(9) 0.0519(3) Uani 1 1 d . . . . .
O2 O 0.59095(11) 0.43997(7) 0.45272(10) 0.0552(3) Uani 1 1 d . . . . .
O3 O 0.60042(17) 0.60821(8) 0.27397(18) 0.0890(6) Uani 1 1 d . . . . .
N1 N 0.71546(14) 0.49069(9) 0.36394(13) 0.0586(4) Uani 1 1 d . . . . .
C1 C 0.29050(17) 0.43178(12) 0.28717(17) 0.0623(6) Uani 1 1 d . . . . .
H1A H 0.282225 0.473348 0.316559 0.075 Uiso 1 1 calc R U . . .
H1B H 0.257519 0.396969 0.306659 0.075 Uiso 1 1 calc R U . . .
C2 C 0.43478(17) 0.40676(10) 0.43374(14) 0.0556(5) Uani 1 1 d . . . . .
H2A H 0.399373 0.371929 0.449899 0.067 Uiso 1 1 calc R U . . .
H2B H 0.430777 0.447167 0.468456 0.067 Uiso 1 1 calc R U . . .
C3 C 0.53820(18) 0.38778(10) 0.47038(15) 0.0573(5) Uani 1 1 d . . . . .
H3A H 0.567537 0.377753 0.544155 0.069 Uiso 1 1 calc R U . . .
H3B H 0.542217 0.348188 0.433976 0.069 Uiso 1 1 calc R U . . .
C4 C 0.69161(18) 0.42699(12) 0.49623(16) 0.0622(5) Uani 1 1 d . . . . .
H4A H 0.702906 0.385784 0.468152 0.075 Uiso 1 1 calc R U . . .
H4B H 0.717597 0.421810 0.570929 0.075 Uiso 1 1 calc R U . . .
C5 C 0.74428(19) 0.48214(13) 0.47355(16) 0.0678(6) Uani 1 1 d . . . . .
H5A H 0.731287 0.523167 0.500709 0.081 Uiso 1 1 calc R U . . .
H5B H 0.815294 0.473831 0.509727 0.081 Uiso 1 1 calc R U . . .
C6 C 0.75418(18) 0.43716(12) 0.32627(17) 0.0646(6) Uani 1 1 d . . . . .
H6A H 0.743780 0.395604 0.354179 0.078 Uiso 1 1 calc R U . . .
H6B H 0.825355 0.443277 0.352800 0.078 Uiso 1 1 calc R U . . .
C7 C 0.7513(2) 0.55367(13) 0.34779(19) 0.0732(7) Uani 1 1 d . . . . .
H7A H 0.750404 0.553209 0.279979 0.088 Uiso 1 1 calc R U . . .
H7B H 0.819968 0.558853 0.399589 0.088 Uiso 1 1 calc R U . . .
C8 C 0.6950(3) 0.61095(13) 0.3533(2) 0.0864(9) Uani 1 1 d . . . . .
H8A H 0.692757 0.611204 0.419650 0.104 Uiso 1 1 calc R U . . .
H8B H 0.727201 0.651547 0.348080 0.104 Uiso 1 1 calc R U . . .
C9 C 0.5297(9) 0.6616(4) 0.2214(8) 0.076(4) Uani 0.292(10) 1 d D . P A 1
H9A H 0.489343 0.651692 0.148294 0.091 Uiso 0.292(10) 1 calc R U P A 1
H9B H 0.563257 0.703768 0.228171 0.091 Uiso 0.292(10) 1 calc R U P A 1
C10 C 0.5502(3) 0.66335(14) 0.2925(3) 0.0722(15) Uani 0.708(10) 1 d D . P A 2
H10A H 0.583774 0.704685 0.293465 0.087 Uiso 0.708(10) 1 calc R U P A 2
H10B H 0.548543 0.658255 0.358706 0.087 Uiso 0.708(10) 1 calc R U P A 2
N2 N 0.80658(13) 0.68422(9) 0.59174(12) 0.0576(4) Uani 1 1 d . . . . .
N3 N 0.86215(12) 0.74560(9) 0.48696(11) 0.0538(4) Uani 1 1 d . . . . .
N4 N 0.68075(13) 0.75604(11) 0.07030(13) 0.0654(5) Uani 1 1 d . . . . .
N5 N 0.85144(13) 0.75649(9) 0.12612(12) 0.0564(4) Uani 1 1 d . . . . .
C11 C 0.79411(14) 0.73176(10) 0.52049(13) 0.0491(4) Uani 1 1 d . . . . .
C12 C 0.94053(16) 0.70864(12) 0.52160(15) 0.0604(5) Uani 1 1 d . . . . .
H12 H 0.988441 0.717380 0.499116 0.073 Uiso 1 1 calc R U . . .
C13 C 0.95675(18) 0.65758(14) 0.58926(18) 0.0712(6) Uani 1 1 d . . . . .
H13 H 1.012263 0.630095 0.611084 0.085 Uiso 1 1 calc R U . . .
C14 C 0.88616(17) 0.64943(13) 0.62288(17) 0.0653(6) Uani 1 1 d . . . . .
H14 H 0.896418 0.616315 0.671862 0.078 Uiso 1 1 calc R U . . .
C15 C 0.75867(14) 0.75315(9) 0.05452(13) 0.0461(4) Uani 1 1 d . . . . .
C16 C 0.86447(17) 0.76245(11) 0.22186(15) 0.0608(5) Uani 1 1 d . . . . .
H16 H 0.929189 0.765214 0.275028 0.073 Uiso 1 1 calc R U . . .
C17 C 0.78915(18) 0.76477(11) 0.24703(15) 0.0582(5) Uani 1 1 d . . . . .
H17 H 0.799694 0.768508 0.315693 0.070 Uiso 1 1 calc R U . . .
C18 C 0.69818(19) 0.76141(14) 0.16787(17) 0.0713(7) Uani 1 1 d . . . . .
H18 H 0.644012 0.762953 0.182557 0.086 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O1 2.8014(13) . ?
K1 O1 2.8015(13) 2_655 ?
K1 O2 2.8366(14) 2_655 ?
K1 O2 2.8366(14) . ?
K1 O3 2.8462(18) . ?
K1 O3 2.8462(18) 2_655 ?
K1 N1 2.962(2) 2_655 ?
K1 N1 2.962(2) . ?
O1 C1 1.418(3) . ?
O1 C2 1.430(2) . ?
O2 C3 1.436(2) . ?
O2 C4 1.408(3) . ?
O3 C8 1.396(4) . ?
O3 C9 1.490(10) . ?
O3 C10 1.463(4) . ?
N1 C5 1.476(3) . ?
N1 C6 1.471(3) . ?
N1 C7 1.466(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C6 1.493(3) 2_655 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.482(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.513(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.484(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C9 1.494(15) 2_655 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C10 1.484(9) 2_655 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
N2 C11 1.380(3) . ?
N2 C14 1.308(3) . ?
N3 C11 1.371(2) . ?
N3 C12 1.316(3) . ?
N4 C15 1.320(3) . ?
N4 C18 1.339(3) . ?
N5 C15 1.339(3) . ?
N5 C16 1.334(3) . ?
C11 C11 1.423(4) 7_666 ?
C12 H12 0.9500 . ?
C12 C13 1.388(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.390(3) . ?
C14 H14 0.9500 . ?
C15 C15 1.506(3) 7_665 ?
C16 H16 0.9500 . ?
C16 C17 1.365(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.359(3) . ?
C18 H18 0.9500 . ?

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 K1 O1 117.40(6) . 2_655 ?
O1 K1 O2 60.08(4) . . ?
O1 K1 O2 97.90(4) . 2_655 ?
O1 K1 O2 97.89(4) 2_655 . ?
O1 K1 O2 60.08(4) 2_655 2_655 ?
O1 K1 O3 96.41(5) 2_655 . ?
O1 K1 O3 142.09(5) 2_655 2_655 ?
O1 K1 O3 96.41(5) . 2_655 ?
O1 K1 O3 142.08(5) . . ?
O1 K1 N1 61.21(4) . 2_655 ?
O1 K1 N1 61.21(4) 2_655 . ?
O1 K1 N1 120.05(5) . . ?
O1 K1 N1 120.05(5) 2_655 2_655 ?
O2 K1 O2 139.29(6) 2_655 . ?
O2 K1 O3 114.50(5) . 2_655 ?
O2 K1 O3 100.85(6) 2_655 2_655 ?
O2 K1 O3 100.85(6) . . ?
O2 K1 O3 114.49(5) 2_655 . ?
O2 K1 N1 119.76(4) . 2_655 ?
O2 K1 N1 61.08(4) . . ?
O2 K1 N1 61.08(5) 2_655 2_655 ?
O2 K1 N1 119.76(4) 2_655 . ?
O3 K1 O3 59.85(9) . 2_655 ?
O3 K1 N1 60.55(6) 2_655 2_655 ?
O3 K1 N1 117.37(6) . 2_655 ?
O3 K1 N1 117.37(6) 2_655 . ?
O3 K1 N1 60.55(6) . . ?
N1 K1 N1 177.89(8) 2_655 . ?
C1 O1 K1 117.94(11) . . ?
C1 O1 C2 111.08(14) . . ?
C2 O1 K1 116.86(11) . . ?
C3 O2 K1 113.45(12) . . ?
C4 O2 K1 117.61(11) . . ?
C4 O2 C3 111.79(16) . . ?
C8 O3 K1 116.15(15) . . ?
C8 O3 C9 130.2(5) . . ?
C8 O3 C10 104.6(2) . . ?
C9 O3 K1 110.2(4) . . ?
C10 O3 K1 113.0(2) . . ?
C5 N1 K1 108.91(13) . . ?
C6 N1 K1 108.20(13) . . ?
C6 N1 C5 110.37(19) . . ?
C7 N1 K1 109.32(16) . . ?
C7 N1 C5 109.37(17) . . ?
C7 N1 C6 110.64(18) . . ?
O1 C1 H1A 109.8 . . ?
O1 C1 H1B 109.8 . . ?
O1 C1 C6 109.52(16) . 2_655 ?
H1A C1 H1B 108.2 . . ?
C6 C1 H1A 109.8 2_655 . ?
C6 C1 H1B 109.8 2_655 . ?
O1 C2 H2A 109.8 . . ?
O1 C2 H2B 109.8 . . ?
O1 C2 C3 109.45(15) . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 H2A 109.8 . . ?
C3 C2 H2B 109.8 . . ?
O2 C3 C2 109.80(17) . . ?
O2 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
C2 C3 H3A 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
O2 C4 H4A 109.6 . . ?
O2 C4 H4B 109.6 . . ?
O2 C4 C5 110.22(19) . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 H4A 109.6 . . ?
C5 C4 H4B 109.6 . . ?
N1 C5 C4 113.70(18) . . ?
N1 C5 H5A 108.8 . . ?
N1 C5 H5B 108.8 . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N1 C6 C1 114.5(2) . 2_655 ?
N1 C6 H6A 108.6 . . ?
N1 C6 H6B 108.6 . . ?
C1 C6 H6A 108.6 2_655 . ?
C1 C6 H6B 108.6 2_655 . ?
H6A C6 H6B 107.6 . . ?
N1 C7 H7A 108.6 . . ?
N1 C7 H7B 108.6 . . ?
N1 C7 C8 114.7(2) . . ?
H7A C7 H7B 107.6 . . ?
C8 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
O3 C8 C7 109.6(2) . . ?
O3 C8 H8A 109.7 . . ?
O3 C8 H8B 109.7 . . ?
C7 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O3 C9 C9 101.4(7) . 2_655 ?
O3 C9 H9A 111.5 . . ?
O3 C9 H9B 111.5 . . ?
C9 C9 H9A 111.5 2_655 . ?
C9 C9 H9B 111.5 2_655 . ?
H9A C9 H9B 109.3 . . ?
O3 C10 C10 106.2(3) . 2_655 ?
O3 C10 H10A 110.5 . . ?
O3 C10 H10B 110.5 . . ?
C10 C10 H10A 110.5 2_655 . ?
C10 C10 H10B 110.5 2_655 . ?
H10A C10 H10B 108.7 . . ?
C14 N2 C11 116.10(18) . . ?
C12 N3 C11 117.05(18) . . ?
C15 N4 C18 115.60(19) . . ?
C16 N5 C15 115.72(18) . . ?
N2 C11 C11 118.2(2) . 7_666 ?
N3 C11 N2 123.45(19) . . ?
N3 C11 C11 118.3(2) . 7_666 ?
N3 C12 H12 118.3 . . ?
N3 C12 C13 123.4(2) . . ?
C13 C12 H12 118.3 . . ?
C12 C13 H13 122.3 . . ?
C12 C13 C14 115.4(2) . . ?
C14 C13 H13 122.3 . . ?
N2 C14 C13 124.5(2) . . ?
N2 C14 H14 117.7 . . ?
C13 C14 H14 117.7 . . ?
N4 C15 N5 126.10(17) . . ?
N4 C15 C15 116.8(2) . 7_665 ?
N5 C15 C15 117.1(2) . 7_665 ?
N5 C16 H16 118.5 . . ?
N5 C16 C17 123.1(2) . . ?
C17 C16 H16 118.5 . . ?
C16 C17 H17 122.0 . . ?
C18 C17 C16 115.93(18) . . ?
C18 C17 H17 122.0 . . ?
N4 C18 C17 123.6(2) . . ?
N4 C18 H18 118.2 . . ?
C17 C18 H18 118.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O1 C1 C6 45.6(2) . . . 2_655 ?
K1 O1 C2 C3 -44.06(19) . . . . ?
K1 O2 C3 C2 -50.58(17) . . . . ?
K1 O2 C4 C5 44.6(2) . . . . ?
K1 O3 C8 C7 49.9(2) . . . . ?
K1 O3 C9 C9 61.9(9) . . . 2_655 ?
K1 O3 C10 C10 -54.5(4) . . . 2_655 ?
K1 N1 C5 C4 46.9(2) . . . . ?
K1 N1 C6 C1 46.4(2) . . . 2_655 ?
K1 N1 C7 C8 43.3(2) . . . . ?
O1 C2 C3 O2 63.0(2) . . . . ?
O2 C4 C5 N1 -63.4(3) . . . . ?
N1 C7 C8 O3 -64.6(3) . . . . ?
C1 O1 C2 C3 176.66(17) . . . . ?
C2 O1 C1 C6 -175.62(17) . . . 2_655 ?
C3 O2 C4 C5 178.43(16) . . . . ?
C4 O2 C3 C2 173.57(16) . . . . ?
C5 N1 C6 C1 165.47(19) . . . 2_655 ?
C5 N1 C7 C8 -75.9(3) . . . . ?
C6 N1 C5 C4 -71.8(3) . . . . ?
C6 N1 C7 C8 162.3(2) . . . . ?
C7 N1 C5 C4 166.3(2) . . . . ?
C7 N1 C6 C1 -73.3(3) . . . 2_655 ?
C8 O3 C9 C9 -95.7(8) . . . 2_655 ?
C8 O3 C10 C10 178.3(3) . . . 2_655 ?
C9 O3 C8 C7 -153.6(4) . . . . ?
C10 O3 C8 C7 175.2(2) . . . . ?
N3 C12 C13 C14 -3.0(4) . . . . ?
N5 C16 C17 C18 -0.8(4) . . . . ?
C11 N2 C14 C13 0.1(4) . . . . ?
C11 N3 C12 C13 -0.2(3) . . . . ?
C12 N3 C11 N2 3.7(3) . . . . ?
C12 N3 C11 C11 -176.1(2) . . . 7_666 ?
C12 C13 C14 N2 3.0(4) . . . . ?
C14 N2 C11 N3 -3.7(3) . . . . ?
C14 N2 C11 C11 176.2(2) . . . 7_666 ?
C15 N4 C18 C17 1.0(4) . . . . ?
C15 N5 C16 C17 0.3(3) . . . . ?
C16 N5 C15 N4 0.9(3) . . . . ?
C16 N5 C15 C15 179.6(2) . . . 7_665 ?
C16 C17 C18 N4 0.1(4) . . . . ?
C18 N4 C15 N5 -1.5(3) . . . . ?
C18 N4 C15 C15 179.8(2) . . . 7_665 ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 158 electrons were 
found in a volume of 716Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O] per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
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 0.000 0.500 -0.051 357.7 79.3 '2 THF'
2 0.500 0.000 -0.080 357.7 79.3 '2 THF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2021-10-04
_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 1.557
_oxdiff_exptl_absorpt_empirical_full_min 0.641
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mb8
_database_code_depnum_ccdc_archive 'CCDC 2181474'
loop_
_audit_author_name
_audit_author_address
'rosario scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT234_mb8                 
;
PROBLEM: Large Hirshfeld Difference O2       --C31_b    .       0.33 Ang.  
RESPONSE: This is due to the disorder affecting the K(crypt) cation
;
_vrf_PLAT410_mb8                 
;
PROBLEM: Short Intra H...H Contact  H24B     ..H30B     .       1.79 Ang.  
RESPONSE: This is due to the disorder affecting the K(crypt) cation
;
_vrf_PLAT973_mb8                 
;
PROBLEM: Check Calcd Positive Resid. Density on        U1       3.97 eA-3  
RESPONSE: This is due to absorption artifacts
;
_vrf_PLAT241_mb8                 
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O2 Check 
RESPONSE: This is due to the disorder affecting the K(crypt) cation
;
_vrf_PLAT242_mb8                 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         K1 Check 
RESPONSE: This is due to the disorder affecting the K(crypt) cation
;
_vrf_PLAT342_mb8                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.04 Ang.  
RESPONSE: This is due to the disorder affecting the K(crypt) cation
;
# end Validation Reply Form

_audit_creation_date             2021-11-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_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
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C68 H164 N12 O6 Si12 K1 U2'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
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'

_cell_length_a                   29.9688(16)
_cell_length_b                   11.6805(5)
_cell_length_c                   32.306(3)
_cell_angle_alpha                90
_cell_angle_beta                 115.332(9)
_cell_angle_gamma                90
_cell_volume                     10221.3(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8607
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.1800
_cell_measurement_theta_min      3.0220
_shelx_estimated_absorpt_T_max   0.591
_shelx_estimated_absorpt_T_min   0.133
_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_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4100
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

_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.054
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

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6715
_reflns_number_total             10025
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         2.844
_refine_diff_density_min         -2.447
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       .
_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_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0771
_refine_ls_restrained_S_all      1.019
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 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_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_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 . . . ?

_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.
;
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'

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

data_dkm132
_database_code_depnum_ccdc_archive 'CCDC 2181478'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;EPFL
Switzerland
;
_audit_update_record             
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_audit_creation_date             2020-05-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C44 H114 N10 Si12 U2, 2(C18 H36 K N2 O6), 4(C4 H10 O)'
_chemical_formula_sum            'C96 H226 K2 N14 O16 Si12 U2'
_chemical_formula_weight         2724.23
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C96 H226 K2 N14 O16 Si12 U2'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.78160(13)
_cell_length_b                   16.73893(18)
_cell_length_c                   17.00630(17)
_cell_angle_alpha                63.8536(11)
_cell_angle_beta                 84.3138(8)
_cell_angle_gamma                74.6504(9)
_cell_volume                     3395.39(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    29165
_cell_measurement_temperature    139.9(9)
_cell_measurement_theta_max      75.8420
_cell_measurement_theta_min      4.3420
_shelx_estimated_absorpt_T_max   0.454
_shelx_estimated_absorpt_T_min   0.203
_exptl_absorpt_coefficient_mu    8.674
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
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)
Empirical absorption correction using spherical harmonics as
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1418
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 2 2 0.0460
0 0 1 0.0577
0 0 -1 0.0499
0 -1 1 0.0570
-1 -2 -1 0.0645
-2 1 2 0.1263
1 -1 -2 0.0469
-2 -2 -5 0.0619
0 1 -1 0.0665

_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.108
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
0.9994 1.9978 1.9993 -0.1446 0.0971 -0.1431
0.0000 -0.0008 0.9997 0.0257 0.0128 -0.0968
-0.0000 0.0008 -0.9997 -0.0257 -0.0128 0.0968
0.0005 -1.0007 0.9999 0.0858 -0.0635 -0.1387
-0.9994 -1.9986 -0.9996 0.1703 -0.0843 0.0463
-2.0014 0.9987 1.9988 0.1429 0.2645 -0.0848
1.0009 -0.9984 -1.9990 -0.0671 -0.1832 0.1182
-1.9999 -1.9951 -4.9986 0.1433 -0.0544 0.4668
-0.0005 1.0007 -0.9999 -0.0858 0.0635 0.1387

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40729
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.054
_diffrn_reflns_theta_min         2.895
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.9(9)
_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 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  12.00   1.00    2.00    --  -40.91  21.00 110.00   31
  2  ω   -119.00  -3.00   1.00    2.00    --  -40.91 -21.00 -55.00  116
  3  ω     40.00 120.00   1.00    2.00    --   40.91  21.00 110.00   80
  4  ω    122.00 177.00   1.00    8.00    --  112.00  21.00 110.00   55
  5  ω     74.00 128.00   1.00    8.00    --  112.00 -21.00 -55.00   54
  6  ω     41.00  70.00   1.00    8.00    --  112.00 -21.00 -55.00   29
  7  ω    -85.00  -9.00   1.00    2.00    --  -40.91 125.00  90.00   76
  8  ω     43.00  78.00   1.00    2.00    --   40.91-125.00  90.00   35
  9  ω     -4.00  21.00   1.00    2.00    --   40.91 -21.00 -55.00   25
 10  ω    -17.00  64.00   1.00    2.00    --   40.91 -77.00-150.00   81
 11  ω      8.00  82.00   1.00    2.00    --   40.91 -99.00 -60.00   74
 12  ω     87.00 177.00   1.00    8.00    --  112.00  30.00   0.00   90
 13  ω     40.00 137.00   1.00    8.00    --  112.00 -45.00-180.00   97
 14  ω     30.00 100.00   1.00    8.00    --  112.00 -94.00   0.00   70
 15  ω     60.00  87.00   1.00    8.00    --  112.00-111.00 -90.00   27
 16  ω     84.00 171.00   1.00    8.00    --  112.00  61.00  30.00   87
 17  ω     30.00  92.00   1.00    8.00    --  112.00 -94.00 150.00   62
 18  ω     44.00  69.00   1.00    8.00    --  112.00-111.00  30.00   25
 19  ω     74.00 109.00   1.00    8.00    --  112.00-111.00 -60.00   35
 20  ω     37.00  84.00   1.00    8.00    --  112.00 -30.00  30.00   47
 21  ω    113.00 140.00   1.00    8.00    --  112.00 -61.00  60.00   27
 22  ω     35.00  62.00   1.00    8.00    --  112.00 -15.00 120.00   27
 23  ω     63.00 109.00   1.00    8.00    --  112.00-111.00  60.00   46
 24  ω     53.00 109.00   1.00    8.00    --  112.00-111.00 -30.00   56
 25  ω     71.00 155.00   1.00    8.00    --  112.00 -15.00 120.00   84
 26  ω     36.00 109.00   1.00    8.00    --  112.00-111.00-150.00   73
 27  ω     55.00 109.00   1.00    8.00    --  112.00-111.00   0.00   54
 28  ω     37.00  79.00   1.00    8.00    --  112.00-111.00 150.00   42
 29  ω     83.00 109.00   1.00    8.00    --  112.00-111.00 150.00   26
 30  ω     96.00 123.00   1.00    8.00    --  112.00 -61.00-180.00   27
 31  ω    107.00 138.00   1.00    8.00    --  112.00 -30.00  30.00   31
 32  ω     36.00 109.00   1.00    8.00    --  112.00-111.00  90.00   73
 33  ω     91.00 134.00   1.00    8.00    --  112.00  45.00 -60.00   43
 34  ω    138.00 166.00   1.00    8.00    --  112.00  45.00 -60.00   28
 35  ω     64.00 101.00   1.00    8.00    --  112.00 -94.00  90.00   37
 36  ω     55.00  84.00   1.00    8.00    --  112.00 -61.00-180.00   29
 37  ω     46.00  80.00   1.00    8.00    --  112.00 -61.00  60.00   34
 38  ω     41.00  66.00   1.00    8.00    --  112.00-111.00-180.00   25
 39  ω     74.00 109.00   1.00    8.00    --  112.00-111.00-120.00   35
 40  ω     43.00  70.00   1.00    8.00    --  112.00 -94.00 -30.00   27
 41  ω     37.00  70.00   1.00    8.00    --  112.00 -94.00-150.00   33
;
_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      -0.0757657000
_diffrn_orient_matrix_UB_12      -0.0601444000
_diffrn_orient_matrix_UB_13      0.0256578000
_diffrn_orient_matrix_UB_21      -0.0811711000
_diffrn_orient_matrix_UB_22      0.0763161000
_diffrn_orient_matrix_UB_23      0.0129046000
_diffrn_orient_matrix_UB_31      -0.0333700000
_diffrn_orient_matrix_UB_32      0.0419023000
_diffrn_orient_matrix_UB_33      -0.0967626000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13728
_reflns_number_total             14025
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         14025
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0221
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0245P)²+2.5506P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0536
_refine_special_details          ?
_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.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),
 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), C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
2.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), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.51395(2) 0.14411(2) 0.28339(2) 0.02155(3) Uani 1 1 d . . . . .
Si1 Si 0.53365(5) 0.36274(4) 0.27528(4) 0.02979(13) Uani 1 1 d . . . . .
Si2 Si 0.35457(5) 0.37992(4) 0.18250(4) 0.02871(13) Uani 1 1 d . . . . .
Si3 Si 0.71412(5) 0.19534(4) 0.13845(4) 0.02846(12) Uani 1 1 d . . . . .
Si4 Si 0.78380(5) 0.04121(4) 0.31188(4) 0.02641(12) Uani 1 1 d . . . . .
Si5 Si 0.45434(5) 0.04678(5) 0.13864(4) 0.02851(12) Uani 1 1 d . . . . .
Si6 Si 0.30853(5) 0.06764(5) 0.27180(4) 0.02920(13) Uani 1 1 d . . . . .
N1 N 0.47259(15) 0.12664(13) 0.43982(12) 0.0252(4) Uani 1 1 d . . . . .
N2 N 0.46579(15) 0.02071(13) 0.59775(12) 0.0253(4) Uani 1 1 d . . . . .
N3 N 0.46221(15) 0.31208(13) 0.24309(12) 0.0266(4) Uani 1 1 d . . . . .
N4 N 0.68721(16) 0.12244(13) 0.24224(13) 0.0268(4) Uani 1 1 d . . . . .
N5 N 0.41998(15) 0.08313(14) 0.21950(12) 0.0263(4) Uani 1 1 d . . . . .
C1 C 0.48480(17) 0.03671(15) 0.50910(14) 0.0232(4) Uani 1 1 d . . . . .
C2 C 0.43189(19) 0.09355(17) 0.61283(15) 0.0288(5) Uani 1 1 d . . . . .
H2 H 0.421338 0.084575 0.671900 0.035 Uiso 1 1 calc R U . . .
C3 C 0.4103(2) 0.18399(17) 0.54677(16) 0.0339(5) Uani 1 1 d . . . . .
H3 H 0.381697 0.235062 0.559587 0.041 Uiso 1 1 calc R U . . .
C4 C 0.4330(2) 0.19502(16) 0.46133(16) 0.0300(5) Uani 1 1 d . . . . .
H4 H 0.419097 0.255711 0.415697 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5887(2) 0.4519(2) 0.1828(2) 0.0452(7) Uani 1 1 d . . . . .
H5A H 0.611890 0.430844 0.137194 0.068 Uiso 1 1 calc R U . . .
H5B H 0.645692 0.461090 0.205251 0.068 Uiso 1 1 calc R U . . .
H5C H 0.537190 0.510000 0.158055 0.068 Uiso 1 1 calc R U . . .
C6 C 0.4650(2) 0.4283(2) 0.3394(2) 0.0420(6) Uani 1 1 d . . . . .
H6A H 0.404914 0.473373 0.306251 0.063 Uiso 1 1 calc R U . . .
H6B H 0.509576 0.460190 0.349205 0.063 Uiso 1 1 calc R U . . .
H6C H 0.445153 0.385352 0.395997 0.063 Uiso 1 1 calc R U . . .
C7 C 0.6435(2) 0.27583(19) 0.34703(18) 0.0366(5) Uani 1 1 d . . . . .
H7A H 0.619139 0.237654 0.403852 0.055 Uiso 1 1 calc R U . . .
H7B H 0.688862 0.307658 0.355758 0.055 Uiso 1 1 calc R U . . .
H7C H 0.679901 0.236860 0.318875 0.055 Uiso 1 1 calc R U . . .
C8 C 0.2464(2) 0.4026(2) 0.2532(2) 0.0418(6) Uani 1 1 d . . . . .
H8A H 0.244852 0.345420 0.305231 0.063 Uiso 1 1 calc R U . . .
H8B H 0.183046 0.425763 0.219821 0.063 Uiso 1 1 calc R U . . .
H8C H 0.255203 0.448389 0.271251 0.063 Uiso 1 1 calc R U . . .
C9 C 0.3135(2) 0.3284(2) 0.11691(19) 0.0419(6) Uani 1 1 d . . . . .
H9A H 0.352928 0.340573 0.063446 0.063 Uiso 1 1 calc R U . . .
H9B H 0.241940 0.355929 0.101219 0.063 Uiso 1 1 calc R U . . .
H9C H 0.324392 0.261965 0.151897 0.063 Uiso 1 1 calc R U . . .
C10 C 0.3621(3) 0.4977(2) 0.0972(2) 0.0477(7) Uani 1 1 d . . . . .
H10A H 0.370929 0.534578 0.126261 0.072 Uiso 1 1 calc R U . . .
H10B H 0.299913 0.527744 0.061659 0.072 Uiso 1 1 calc R U . . .
H10C H 0.419482 0.491881 0.059456 0.072 Uiso 1 1 calc R U . . .
C11 C 0.7814(2) 0.28107(19) 0.13568(18) 0.0378(6) Uani 1 1 d . . . . .
H11A H 0.751623 0.304863 0.178267 0.057 Uiso 1 1 calc R U . . .
H11B H 0.774795 0.331925 0.076843 0.057 Uiso 1 1 calc R U . . .
H11C H 0.852829 0.250975 0.150492 0.057 Uiso 1 1 calc R U . . .
C12 C 0.5941(2) 0.26333(19) 0.07306(17) 0.0386(6) Uani 1 1 d . . . . .
H12A H 0.555144 0.221317 0.074878 0.058 Uiso 1 1 calc R U . . .
H12B H 0.609775 0.299841 0.012183 0.058 Uiso 1 1 calc R U . . .
H12C H 0.554539 0.304353 0.097987 0.058 Uiso 1 1 calc R U . . .
C13 C 0.7962(2) 0.1373(2) 0.07366(19) 0.0409(6) Uani 1 1 d . . . . .
H13A H 0.858450 0.097821 0.107035 0.061 Uiso 1 1 calc R U . . .
H13B H 0.812548 0.183917 0.017772 0.061 Uiso 1 1 calc R U . . .
H13C H 0.760283 0.099877 0.062483 0.061 Uiso 1 1 calc R U . . .
C14 C 0.9079(2) 0.0737(2) 0.2923(2) 0.0399(6) Uani 1 1 d . . . . .
H14A H 0.930317 0.082784 0.233120 0.060 Uiso 1 1 calc R U . . .
H14B H 0.958080 0.024467 0.335368 0.060 Uiso 1 1 calc R U . . .
H14C H 0.899791 0.130703 0.298288 0.060 Uiso 1 1 calc R U . . .
C15 C 0.8120(2) -0.07124(17) 0.30363(18) 0.0342(5) Uani 1 1 d . . . . .
H15A H 0.756871 -0.101179 0.328970 0.051 Uiso 1 1 calc R U . . .
H15B H 0.874854 -0.111157 0.335694 0.051 Uiso 1 1 calc R U . . .
H15C H 0.818924 -0.059876 0.241919 0.051 Uiso 1 1 calc R U . . .
C16 C 0.7567(2) 0.0186(2) 0.42904(17) 0.0379(6) Uani 1 1 d . . . . .
H16A H 0.752115 0.074461 0.436269 0.057 Uiso 1 1 calc R U . . .
H16B H 0.811068 -0.030985 0.466919 0.057 Uiso 1 1 calc R U . . .
H16C H 0.692863 0.000648 0.445172 0.057 Uiso 1 1 calc R U . . .
C17 C 0.4045(2) 0.1394(2) 0.02771(17) 0.0425(6) Uani 1 1 d . . . . .
H17A H 0.330960 0.158732 0.029018 0.064 Uiso 1 1 calc R U . . .
H17B H 0.423735 0.115487 -0.016357 0.064 Uiso 1 1 calc R U . . .
H17C H 0.432840 0.192066 0.012763 0.064 Uiso 1 1 calc R U . . .
C18 C 0.5945(2) 0.0088(2) 0.13098(18) 0.0368(5) Uani 1 1 d . . . . .
H18A H 0.626733 0.048181 0.142669 0.055 Uiso 1 1 calc R U . . .
H18B H 0.611395 0.013328 0.072038 0.055 Uiso 1 1 calc R U . . .
H18C H 0.618541 -0.055058 0.174225 0.055 Uiso 1 1 calc R U . . .
C19 C 0.4085(3) -0.0557(2) 0.1530(2) 0.0495(7) Uani 1 1 d . . . . .
H19A H 0.434395 -0.107588 0.208833 0.074 Uiso 1 1 calc R U . . .
H19B H 0.432524 -0.072455 0.104792 0.074 Uiso 1 1 calc R U . . .
H19C H 0.334734 -0.040058 0.152765 0.074 Uiso 1 1 calc R U . . .
C20 C 0.2738(2) 0.1344(2) 0.33930(18) 0.0361(5) Uani 1 1 d . . . . .
H20A H 0.323052 0.108766 0.387400 0.054 Uiso 1 1 calc R U . . .
H20B H 0.206723 0.130360 0.363349 0.054 Uiso 1 1 calc R U . . .
H20C H 0.273545 0.198873 0.302332 0.054 Uiso 1 1 calc R U . . .
C21 C 0.1978(2) 0.1114(2) 0.1947(2) 0.0428(6) Uani 1 1 d . . . . .
H21A H 0.193627 0.175614 0.153472 0.064 Uiso 1 1 calc R U . . .
H21B H 0.135820 0.107242 0.228254 0.064 Uiso 1 1 calc R U . . .
H21C H 0.206288 0.074219 0.162117 0.064 Uiso 1 1 calc R U . . .
C22 C 0.3067(2) -0.0537(2) 0.3507(2) 0.0425(6) Uani 1 1 d . . . . .
H22A H 0.318064 -0.091867 0.318893 0.064 Uiso 1 1 calc R U . . .
H22B H 0.241116 -0.054271 0.378919 0.064 Uiso 1 1 calc R U . . .
H22C H 0.359821 -0.078183 0.395475 0.064 Uiso 1 1 calc R U . . .
K1 K 0.87169(4) 0.46407(3) 0.34881(3) 0.02814(9) Uani 1 1 d . . . . .
O1 O 0.92368(14) 0.36238(12) 0.24998(11) 0.0324(4) Uani 1 1 d . . . . .
O2 O 0.84313(15) 0.55188(13) 0.16467(12) 0.0358(4) Uani 1 1 d . . . . .
O3 O 0.67291(15) 0.51583(14) 0.40868(13) 0.0372(4) Uani 1 1 d . . . . .
O4 O 0.79720(14) 0.34086(13) 0.50420(12) 0.0358(4) Uani 1 1 d . . . . .
O5 O 1.06900(14) 0.42395(13) 0.40768(12) 0.0322(4) Uani 1 1 d . . . . .
O6 O 0.95432(14) 0.60527(12) 0.34846(11) 0.0316(4) Uani 1 1 d . . . . .
N6 N 0.98771(16) 0.26902(15) 0.43822(14) 0.0306(4) Uani 1 1 d . . . . .
N7 N 0.75538(17) 0.65990(15) 0.26296(15) 0.0334(4) Uani 1 1 d . . . . .
C23 C 0.9760(2) 0.22485(17) 0.38276(17) 0.0344(5) Uani 1 1 d . . . . .
H23A H 0.906236 0.218010 0.387334 0.041 Uiso 1 1 calc R U . . .
H23B H 1.021784 0.162522 0.405433 0.041 Uiso 1 1 calc R U . . .
C24 C 0.9981(2) 0.27746(18) 0.28703(17) 0.0338(5) Uani 1 1 d . . . . .
H24A H 1.065610 0.289445 0.281737 0.041 Uiso 1 1 calc R U . . .
H24B H 0.997703 0.240530 0.254928 0.041 Uiso 1 1 calc R U . . .
C25 C 0.9442(2) 0.41420(19) 0.16091(17) 0.0352(5) Uani 1 1 d . . . . .
H25A H 0.955858 0.375376 0.129029 0.042 Uiso 1 1 calc R U . . .
H25B H 1.005596 0.435784 0.157058 0.042 Uiso 1 1 calc R U . . .
C26 C 0.8559(2) 0.49509(19) 0.12044(17) 0.0360(5) Uani 1 1 d . . . . .
H26A H 0.867820 0.530454 0.057541 0.043 Uiso 1 1 calc R U . . .
H26B H 0.794307 0.473500 0.125325 0.043 Uiso 1 1 calc R U . . .
C27 C 0.7569(2) 0.62750(19) 0.13244(18) 0.0382(6) Uani 1 1 d . . . . .
H27A H 0.694766 0.605732 0.152286 0.046 Uiso 1 1 calc R U . . .
H27B H 0.755981 0.657067 0.067584 0.046 Uiso 1 1 calc R U . . .
C28 C 0.7616(2) 0.69579(18) 0.16681(17) 0.0364(5) Uani 1 1 d . . . . .
H28A H 0.825422 0.714876 0.148309 0.044 Uiso 1 1 calc R U . . .
H28B H 0.705602 0.751065 0.139867 0.044 Uiso 1 1 calc R U . . .
C29 C 0.6498(2) 0.6653(2) 0.2885(2) 0.0455(7) Uani 1 1 d . . . . .
H29A H 0.617817 0.642722 0.255330 0.055 Uiso 1 1 calc R U . . .
H29B H 0.614570 0.730469 0.271485 0.055 Uiso 1 1 calc R U . . .
C30 C 0.6354(2) 0.6109(2) 0.3852(2) 0.0483(7) Uani 1 1 d . . . . .
H30A H 0.671484 0.629269 0.419602 0.058 Uiso 1 1 calc R U . . .
H30B H 0.562978 0.624000 0.398737 0.058 Uiso 1 1 calc R U . . .
C31 C 0.6595(2) 0.4629(2) 0.49918(19) 0.0379(6) Uani 1 1 d . . . . .
H31A H 0.587818 0.478917 0.513736 0.045 Uiso 1 1 calc R U . . .
H31B H 0.699696 0.476765 0.534600 0.045 Uiso 1 1 calc R U . . .
C32 C 0.6923(2) 0.3627(2) 0.52050(18) 0.0373(6) Uani 1 1 d . . . . .
H32A H 0.679346 0.325572 0.582743 0.045 Uiso 1 1 calc R U . . .
H32B H 0.654270 0.348840 0.483604 0.045 Uiso 1 1 calc R U . . .
C33 C 0.8340(2) 0.24507(19) 0.52912(18) 0.0377(6) Uani 1 1 d . . . . .
H33A H 0.806536 0.227919 0.488750 0.045 Uiso 1 1 calc R U . . .
H33B H 0.812573 0.209905 0.589201 0.045 Uiso 1 1 calc R U . . .
C34 C 0.9471(2) 0.22288(19) 0.52565(17) 0.0369(6) Uani 1 1 d . . . . .
H34A H 0.972989 0.240189 0.566692 0.044 Uiso 1 1 calc R U . . .
H34B H 0.972893 0.155654 0.546437 0.044 Uiso 1 1 calc R U . . .
C35 C 1.0946(2) 0.26380(18) 0.44707(17) 0.0333(5) Uani 1 1 d . . . . .
H35A H 1.127526 0.272677 0.390405 0.040 Uiso 1 1 calc R U . . .
H35B H 1.127337 0.201648 0.491216 0.040 Uiso 1 1 calc R U . . .
C36 C 1.1109(2) 0.33429(19) 0.47402(17) 0.0345(5) Uani 1 1 d . . . . .
H36A H 1.077957 0.326559 0.530496 0.041 Uiso 1 1 calc R U . . .
H36B H 1.183751 0.325822 0.481623 0.041 Uiso 1 1 calc R U . . .
C37 C 1.1048(2) 0.49182(19) 0.41646(18) 0.0342(5) Uani 1 1 d . . . . .
H37A H 1.179236 0.477190 0.414308 0.041 Uiso 1 1 calc R U . . .
H37B H 1.084661 0.492921 0.473559 0.041 Uiso 1 1 calc R U . . .
C38 C 1.0612(2) 0.58395(19) 0.34312(18) 0.0357(5) Uani 1 1 d . . . . .
H38A H 1.087245 0.631608 0.347501 0.043 Uiso 1 1 calc R U . . .
H38B H 1.081285 0.582736 0.286045 0.043 Uiso 1 1 calc R U . . .
C39 C 0.9105(2) 0.69721(18) 0.28685(17) 0.0349(5) Uani 1 1 d . . . . .
H39A H 0.931971 0.705804 0.226927 0.042 Uiso 1 1 calc R U . . .
H39B H 0.933386 0.741136 0.300433 0.042 Uiso 1 1 calc R U . . .
C40 C 0.7969(2) 0.71504(18) 0.29179(18) 0.0370(6) Uani 1 1 d . . . . .
H40A H 0.777072 0.701754 0.353017 0.044 Uiso 1 1 calc R U . . .
H40B H 0.766990 0.780922 0.254982 0.044 Uiso 1 1 calc R U . . .
O7 O 0.2140(2) 0.75047(19) 0.25292(18) 0.0635(7) Uani 1 1 d . . . . .
C41 C 0.2778(4) 0.6839(3) 0.2281(3) 0.0713(11) Uani 1 1 d . . . . .
H41A H 0.243192 0.680410 0.181829 0.086 Uiso 1 1 calc R U . . .
H41B H 0.289321 0.623105 0.279298 0.086 Uiso 1 1 calc R U . . .
C42 C 0.3771(4) 0.7041(4) 0.1952(4) 0.0870(16) Uani 1 1 d . . . . .
H42A H 0.366812 0.761247 0.141033 0.130 Uiso 1 1 calc R U . . .
H42B H 0.419335 0.653542 0.183378 0.130 Uiso 1 1 calc R U . . .
H42C H 0.410494 0.710760 0.239438 0.130 Uiso 1 1 calc R U . . .
C43 C 0.1621(3) 0.8302(3) 0.1817(2) 0.0554(8) Uani 1 1 d . . . . .
H43A H 0.120473 0.813463 0.149909 0.067 Uiso 1 1 calc R U . . .
H43B H 0.210781 0.860993 0.140375 0.067 Uiso 1 1 calc R U . . .
C44 C 0.0964(3) 0.8934(3) 0.2172(2) 0.0574(8) Uani 1 1 d . . . . .
H44A H 0.061829 0.950198 0.168536 0.086 Uiso 1 1 calc R U . . .
H44B H 0.137977 0.907901 0.250221 0.086 Uiso 1 1 calc R U . . .
H44C H 0.046544 0.863401 0.255929 0.086 Uiso 1 1 calc R U . . .
O8 O 0.97650(17) 0.77115(15) 0.06130(13) 0.0433(4) Uani 1 1 d . . . . .
C45 C 0.9134(3) 0.8573(2) 0.0078(2) 0.0515(8) Uani 1 1 d . . . . .
H45A H 0.849209 0.848570 -0.004581 0.062 Uiso 1 1 calc R U . . .
H45B H 0.946319 0.885678 -0.048686 0.062 Uiso 1 1 calc R U . . .
C46 C 0.8929(4) 0.9185(3) 0.0519(3) 0.0778(13) Uani 1 1 d . . . . .
H46A H 0.849156 0.977905 0.014226 0.117 Uiso 1 1 calc R U . . .
H46B H 0.956458 0.927696 0.063444 0.117 Uiso 1 1 calc R U . . .
H46C H 0.859514 0.890658 0.107465 0.117 Uiso 1 1 calc R U . . .
C47 C 0.9978(3) 0.7105(2) 0.0214(2) 0.0486(7) Uani 1 1 d . . . . .
H47A H 1.027932 0.738919 -0.036569 0.058 Uiso 1 1 calc R U . . .
H47B H 0.934796 0.697394 0.012453 0.058 Uiso 1 1 calc R U . . .
C48 C 1.0694(3) 0.6233(2) 0.0789(3) 0.0557(8) Uani 1 1 d . . . . .
H48A H 1.084416 0.580792 0.051547 0.084 Uiso 1 1 calc R U . . .
H48B H 1.038861 0.595216 0.135983 0.084 Uiso 1 1 calc R U . . .
H48C H 1.131739 0.636607 0.087064 0.084 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Si6 3.4560(7) . ?
U1 N1 2.5670(19) . ?
U1 N2 2.5621(19) 2_656 ?
U1 N3 2.494(2) . ?
U1 N4 2.399(2) . ?
U1 N5 2.420(2) . ?
Si1 N3 1.716(2) . ?
Si1 C5 1.890(3) . ?
Si1 C6 1.895(3) . ?
Si1 C7 1.880(3) . ?
Si2 N3 1.712(2) . ?
Si2 C8 1.886(3) . ?
Si2 C9 1.881(3) . ?
Si2 C10 1.886(3) . ?
Si3 N4 1.719(2) . ?
Si3 C11 1.886(3) . ?
Si3 C12 1.877(3) . ?
Si3 C13 1.885(3) . ?
Si4 N4 1.720(2) . ?
Si4 C14 1.884(3) . ?
Si4 C15 1.884(3) . ?
Si4 C16 1.875(3) . ?
Si5 N5 1.715(2) . ?
Si5 C17 1.884(3) . ?
Si5 C18 1.878(3) . ?
Si5 C19 1.891(3) . ?
Si6 N5 1.719(2) . ?
Si6 C20 1.880(3) . ?
Si6 C21 1.883(3) . ?
Si6 C22 1.883(3) . ?
N1 C1 1.423(3) . ?
N1 C4 1.319(3) . ?
N2 C1 1.420(3) . ?
N2 C2 1.312(3) . ?
C1 C1 1.349(5) 2_656 ?
C2 H2 0.9500 . ?
C2 C3 1.404(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.396(3) . ?
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 2.8058(18) . ?
K1 O2 2.8291(19) . ?
K1 O3 2.874(2) . ?
K1 O4 2.8408(19) . ?
K1 O5 2.7978(18) . ?
K1 O6 2.8800(19) . ?
K1 N6 2.978(2) . ?
K1 N7 2.985(2) . ?
O1 C24 1.427(3) . ?
O1 C25 1.419(3) . ?
O2 C26 1.420(3) . ?
O2 C27 1.427(3) . ?
O3 C30 1.416(4) . ?
O3 C31 1.420(3) . ?
O4 C32 1.424(3) . ?
O4 C33 1.422(3) . ?
O5 C36 1.427(3) . ?
O5 C37 1.421(3) . ?
O6 C38 1.425(3) . ?
O6 C39 1.429(3) . ?
N6 C23 1.473(3) . ?
N6 C34 1.474(3) . ?
N6 C35 1.471(3) . ?
N7 C28 1.475(3) . ?
N7 C29 1.467(4) . ?
N7 C40 1.468(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.516(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.504(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.512(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.512(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.499(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.505(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.513(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.503(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.515(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
O7 C41 1.419(5) . ?
O7 C43 1.414(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.493(7) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.500(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O8 C45 1.414(4) . ?
O8 C47 1.410(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.476(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.494(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 U1 Si6 92.16(5) . . ?
N2 U1 Si6 71.28(5) 2_656 . ?
N2 U1 N1 63.98(6) 2_656 . ?
N3 U1 Si6 110.10(5) . . ?
N3 U1 N1 84.38(6) . . ?
N3 U1 N2 148.30(6) . 2_656 ?
N4 U1 Si6 137.55(5) . . ?
N4 U1 N1 118.23(6) . . ?
N4 U1 N2 94.96(6) . 2_656 ?
N4 U1 N3 102.23(7) . . ?
N4 U1 N5 111.85(7) . . ?
N5 U1 Si6 27.43(5) . . ?
N5 U1 N1 118.21(6) . . ?
N5 U1 N2 78.36(6) . 2_656 ?
N5 U1 N3 118.14(7) . . ?
N3 Si1 C5 115.02(13) . . ?
N3 Si1 C6 115.47(12) . . ?
N3 Si1 C7 111.69(11) . . ?
C5 Si1 C6 102.27(14) . . ?
C7 Si1 C5 105.81(14) . . ?
C7 Si1 C6 105.52(13) . . ?
N3 Si2 C8 112.02(12) . . ?
N3 Si2 C9 112.50(12) . . ?
N3 Si2 C10 116.02(13) . . ?
C9 Si2 C8 107.86(15) . . ?
C9 Si2 C10 103.16(15) . . ?
C10 Si2 C8 104.48(14) . . ?
N4 Si3 C11 113.90(11) . . ?
N4 Si3 C12 109.57(12) . . ?
N4 Si3 C13 115.08(12) . . ?
C12 Si3 C11 106.74(13) . . ?
C12 Si3 C13 106.53(14) . . ?
C13 Si3 C11 104.42(13) . . ?
N4 Si4 C14 114.80(12) . . ?
N4 Si4 C15 112.42(11) . . ?
N4 Si4 C16 111.96(11) . . ?
C15 Si4 C14 104.73(13) . . ?
C16 Si4 C14 103.89(13) . . ?
C16 Si4 C15 108.38(13) . . ?
N5 Si5 C17 111.85(12) . . ?
N5 Si5 C18 112.68(11) . . ?
N5 Si5 C19 114.93(12) . . ?
C17 Si5 C19 105.26(16) . . ?
C18 Si5 C17 107.63(14) . . ?
C18 Si5 C19 103.80(14) . . ?
N5 Si6 U1 40.44(7) . . ?
N5 Si6 C20 110.56(11) . . ?
N5 Si6 C21 113.61(12) . . ?
N5 Si6 C22 116.25(12) . . ?
C20 Si6 U1 71.75(9) . . ?
C20 Si6 C21 104.52(13) . . ?
C20 Si6 C22 104.73(13) . . ?
C21 Si6 U1 136.03(11) . . ?
C21 Si6 C22 106.16(14) . . ?
C22 Si6 U1 117.28(10) . . ?
C1 N1 U1 118.70(14) . . ?
C4 N1 U1 125.14(15) . . ?
C4 N1 C1 115.95(19) . . ?
C1 N2 U1 119.70(14) . 2_656 ?
C2 N2 U1 123.53(15) . 2_656 ?
C2 N2 C1 116.6(2) . . ?
Si1 N3 U1 120.86(10) . . ?
Si2 N3 U1 120.89(10) . . ?
Si2 N3 Si1 118.25(12) . . ?
Si3 N4 U1 117.07(10) . . ?
Si3 N4 Si4 119.47(12) . . ?
Si4 N4 U1 123.43(10) . . ?
Si5 N5 U1 129.11(11) . . ?
Si5 N5 Si6 118.54(12) . . ?
Si6 N5 U1 112.12(9) . . ?
N2 C1 N1 122.4(2) . . ?
C1 C1 N1 119.5(3) 2_656 . ?
C1 C1 N2 118.1(3) 2_656 . ?
N2 C2 H2 118.1 . . ?
N2 C2 C3 123.8(2) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 H3 121.7 . . ?
C4 C3 C2 116.6(2) . . ?
C4 C3 H3 121.7 . . ?
N1 C4 C3 124.2(2) . . ?
N1 C4 H4 117.9 . . ?
C3 C4 H4 117.9 . . ?
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 O2 59.41(5) . . ?
O1 K1 O3 125.02(6) . . ?
O1 K1 O4 102.25(6) . . ?
O1 K1 O6 130.04(6) . . ?
O1 K1 N6 61.97(6) . . ?
O1 K1 N7 119.31(6) . . ?
O2 K1 O3 102.20(6) . . ?
O2 K1 O4 141.78(6) . . ?
O2 K1 O6 92.65(5) . . ?
O2 K1 N6 120.63(6) . . ?
O2 K1 N7 60.64(6) . . ?
O3 K1 O6 99.43(6) . . ?
O3 K1 N6 118.33(6) . . ?
O3 K1 N7 61.08(6) . . ?
O4 K1 O3 58.72(6) . . ?
O4 K1 O6 121.43(6) . . ?
O4 K1 N6 60.20(6) . . ?
O4 K1 N7 119.04(6) . . ?
O5 K1 O1 94.23(6) . . ?
O5 K1 O2 115.22(6) . . ?
O5 K1 O3 136.34(6) . . ?
O5 K1 O4 98.28(6) . . ?
O5 K1 O6 58.93(5) . . ?
O5 K1 N6 60.48(6) . . ?
O5 K1 N7 119.02(6) . . ?
O6 K1 N6 118.75(6) . . ?
O6 K1 N7 60.58(6) . . ?
N6 K1 N7 178.72(6) . . ?
C24 O1 K1 117.00(14) . . ?
C25 O1 K1 114.46(15) . . ?
C25 O1 C24 110.7(2) . . ?
C26 O2 K1 117.52(15) . . ?
C26 O2 C27 111.8(2) . . ?
C27 O2 K1 115.51(16) . . ?
C30 O3 K1 115.22(17) . . ?
C30 O3 C31 111.0(2) . . ?
C31 O3 K1 113.97(15) . . ?
C32 O4 K1 118.32(16) . . ?
C33 O4 K1 118.10(15) . . ?
C33 O4 C32 110.6(2) . . ?
C36 O5 K1 118.23(15) . . ?
C37 O5 K1 120.31(15) . . ?
C37 O5 C36 111.55(19) . . ?
C38 O6 K1 112.10(14) . . ?
C38 O6 C39 111.0(2) . . ?
C39 O6 K1 116.39(14) . . ?
C23 N6 K1 106.37(14) . . ?
C23 N6 C34 109.8(2) . . ?
C34 N6 K1 110.53(15) . . ?
C35 N6 K1 110.44(15) . . ?
C35 N6 C23 110.3(2) . . ?
C35 N6 C34 109.4(2) . . ?
C28 N7 K1 110.44(15) . . ?
C29 N7 K1 108.68(16) . . ?
C29 N7 C28 109.5(2) . . ?
C29 N7 C40 109.8(2) . . ?
C40 N7 K1 109.34(15) . . ?
C40 N7 C28 109.1(2) . . ?
N6 C23 H23A 108.8 . . ?
N6 C23 H23B 108.8 . . ?
N6 C23 C24 113.8(2) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
O1 C24 C23 109.5(2) . . ?
O1 C24 H24A 109.8 . . ?
O1 C24 H24B 109.8 . . ?
C23 C24 H24A 109.8 . . ?
C23 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
O1 C25 H25A 109.9 . . ?
O1 C25 H25B 109.9 . . ?
O1 C25 C26 108.9(2) . . ?
H25A C25 H25B 108.3 . . ?
C26 C25 H25A 109.9 . . ?
C26 C25 H25B 109.9 . . ?
O2 C26 C25 109.0(2) . . ?
O2 C26 H26A 109.9 . . ?
O2 C26 H26B 109.9 . . ?
C25 C26 H26A 109.9 . . ?
C25 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
O2 C27 H27A 110.0 . . ?
O2 C27 H27B 110.0 . . ?
O2 C27 C28 108.6(2) . . ?
H27A C27 H27B 108.3 . . ?
C28 C27 H27A 110.0 . . ?
C28 C27 H27B 110.0 . . ?
N7 C28 C27 113.8(2) . . ?
N7 C28 H28A 108.8 . . ?
N7 C28 H28B 108.8 . . ?
C27 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
N7 C29 H29A 108.7 . . ?
N7 C29 H29B 108.7 . . ?
N7 C29 C30 114.3(2) . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
O3 C30 C29 109.7(3) . . ?
O3 C30 H30A 109.7 . . ?
O3 C30 H30B 109.7 . . ?
C29 C30 H30A 109.7 . . ?
C29 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
O3 C31 H31A 109.7 . . ?
O3 C31 H31B 109.7 . . ?
O3 C31 C32 109.8(2) . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
O4 C32 C31 108.2(2) . . ?
O4 C32 H32A 110.1 . . ?
O4 C32 H32B 110.1 . . ?
C31 C32 H32A 110.1 . . ?
C31 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
O4 C33 H33A 110.0 . . ?
O4 C33 H33B 110.0 . . ?
O4 C33 C34 108.7(2) . . ?
H33A C33 H33B 108.3 . . ?
C34 C33 H33A 110.0 . . ?
C34 C33 H33B 110.0 . . ?
N6 C34 C33 114.7(2) . . ?
N6 C34 H34A 108.6 . . ?
N6 C34 H34B 108.6 . . ?
C33 C34 H34A 108.6 . . ?
C33 C34 H34B 108.6 . . ?
H34A C34 H34B 107.6 . . ?
N6 C35 H35A 108.9 . . ?
N6 C35 H35B 108.9 . . ?
N6 C35 C36 113.4(2) . . ?
H35A C35 H35B 107.7 . . ?
C36 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
O5 C36 C35 108.9(2) . . ?
O5 C36 H36A 109.9 . . ?
O5 C36 H36B 109.9 . . ?
C35 C36 H36A 109.9 . . ?
C35 C36 H36B 109.9 . . ?
H36A C36 H36B 108.3 . . ?
O5 C37 H37A 109.9 . . ?
O5 C37 H37B 109.9 . . ?
O5 C37 C38 109.0(2) . . ?
H37A C37 H37B 108.3 . . ?
C38 C37 H37A 109.9 . . ?
C38 C37 H37B 109.9 . . ?
O6 C38 C37 109.3(2) . . ?
O6 C38 H38A 109.8 . . ?
O6 C38 H38B 109.8 . . ?
C37 C38 H38A 109.8 . . ?
C37 C38 H38B 109.8 . . ?
H38A C38 H38B 108.3 . . ?
O6 C39 H39A 109.9 . . ?
O6 C39 H39B 109.9 . . ?
O6 C39 C40 109.1(2) . . ?
H39A C39 H39B 108.3 . . ?
C40 C39 H39A 109.9 . . ?
C40 C39 H39B 109.9 . . ?
N7 C40 C39 113.6(2) . . ?
N7 C40 H40A 108.9 . . ?
N7 C40 H40B 108.9 . . ?
C39 C40 H40A 108.9 . . ?
C39 C40 H40B 108.9 . . ?
H40A C40 H40B 107.7 . . ?
C43 O7 C41 113.9(3) . . ?
O7 C41 H41A 108.9 . . ?
O7 C41 H41B 108.9 . . ?
O7 C41 C42 113.5(4) . . ?
H41A C41 H41B 107.7 . . ?
C42 C41 H41A 108.9 . . ?
C42 C41 H41B 108.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O7 C43 H43A 110.0 . . ?
O7 C43 H43B 110.0 . . ?
O7 C43 C44 108.3(3) . . ?
H43A C43 H43B 108.4 . . ?
C44 C43 H43A 110.0 . . ?
C44 C43 H43B 110.0 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C47 O8 C45 112.0(2) . . ?
O8 C45 H45A 109.6 . . ?
O8 C45 H45B 109.6 . . ?
O8 C45 C46 110.3(3) . . ?
H45A C45 H45B 108.1 . . ?
C46 C45 H45A 109.6 . . ?
C46 C45 H45B 109.6 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O8 C47 H47A 109.9 . . ?
O8 C47 H47B 109.9 . . ?
O8 C47 C48 109.1(3) . . ?
H47A C47 H47B 108.3 . . ?
C48 C47 H47A 109.9 . . ?
C48 C47 H47B 109.9 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 Si6 N5 Si5 174.99(19) . . . . ?
U1 N1 C1 N2 178.59(16) . . . . ?
U1 N1 C1 C1 -1.6(4) . . . 2_656 ?
U1 N1 C4 C3 179.4(2) . . . . ?
U1 N2 C1 N1 178.47(16) 2_656 . . . ?
U1 N2 C1 C1 -1.3(3) 2_656 . . 2_656 ?
U1 N2 C2 C3 -172.8(2) 2_656 . . . ?
N2 C2 C3 C4 -4.2(4) . . . . ?
C1 N1 C4 C3 4.8(4) . . . . ?
C1 N2 C2 C3 2.6(4) . . . . ?
C2 N2 C1 N1 2.8(3) . . . . ?
C2 N2 C1 C1 -177.0(3) . . . 2_656 ?
C2 C3 C4 N1 0.1(4) . . . . ?
C4 N1 C1 N2 -6.4(3) . . . . ?
C4 N1 C1 C1 173.4(3) . . . 2_656 ?
C5 Si1 N3 U1 116.82(14) . . . . ?
C5 Si1 N3 Si2 -63.12(17) . . . . ?
C6 Si1 N3 U1 -124.36(14) . . . . ?
C6 Si1 N3 Si2 55.71(17) . . . . ?
C7 Si1 N3 U1 -3.79(16) . . . . ?
C7 Si1 N3 Si2 176.27(13) . . . . ?
C8 Si2 N3 U1 99.39(14) . . . . ?
C8 Si2 N3 Si1 -80.67(16) . . . . ?
C9 Si2 N3 U1 -22.32(16) . . . . ?
C9 Si2 N3 Si1 157.62(14) . . . . ?
C10 Si2 N3 U1 -140.77(14) . . . . ?
C10 Si2 N3 Si1 39.16(19) . . . . ?
C11 Si3 N4 U1 109.01(13) . . . . ?
C11 Si3 N4 Si4 -68.99(17) . . . . ?
C12 Si3 N4 U1 -10.45(15) . . . . ?
C12 Si3 N4 Si4 171.55(14) . . . . ?
C13 Si3 N4 U1 -130.44(13) . . . . ?
C13 Si3 N4 Si4 51.56(18) . . . . ?
C14 Si4 N4 U1 -149.19(13) . . . . ?
C14 Si4 N4 Si3 28.67(18) . . . . ?
C15 Si4 N4 U1 91.23(14) . . . . ?
C15 Si4 N4 Si3 -90.91(15) . . . . ?
C16 Si4 N4 U1 -31.06(17) . . . . ?
C16 Si4 N4 Si3 146.80(14) . . . . ?
C17 Si5 N5 U1 -96.36(16) . . . . ?
C17 Si5 N5 Si6 89.62(17) . . . . ?
C18 Si5 N5 U1 25.05(18) . . . . ?
C18 Si5 N5 Si6 -148.97(14) . . . . ?
C19 Si5 N5 U1 143.69(16) . . . . ?
C19 Si5 N5 Si6 -30.3(2) . . . . ?
C20 Si6 N5 U1 17.12(14) . . . . ?
C20 Si6 N5 Si5 -167.88(13) . . . . ?
C21 Si6 N5 U1 134.27(13) . . . . ?
C21 Si6 N5 Si5 -50.74(18) . . . . ?
C22 Si6 N5 U1 -102.07(14) . . . . ?
C22 Si6 N5 Si5 72.92(17) . . . . ?
K1 O1 C24 C23 44.8(2) . . . . ?
K1 O1 C25 C26 -54.4(2) . . . . ?
K1 O2 C26 C25 -39.8(3) . . . . ?
K1 O2 C27 C28 55.0(3) . . . . ?
K1 O3 C30 C29 49.1(3) . . . . ?
K1 O3 C31 C32 -52.4(2) . . . . ?
K1 O4 C32 C31 -43.3(3) . . . . ?
K1 O4 C33 C34 48.9(3) . . . . ?
K1 O5 C36 C35 50.1(2) . . . . ?
K1 O5 C37 C38 -37.0(3) . . . . ?
K1 O6 C38 C37 -55.4(2) . . . . ?
K1 O6 C39 C40 47.3(2) . . . . ?
K1 N6 C23 C24 50.0(2) . . . . ?
K1 N6 C34 C33 42.1(3) . . . . ?
K1 N6 C35 C36 42.1(2) . . . . ?
K1 N7 C28 C27 39.1(3) . . . . ?
K1 N7 C29 C30 45.8(3) . . . . ?
K1 N7 C40 C39 47.9(3) . . . . ?
O1 C25 C26 O2 62.0(3) . . . . ?
O2 C27 C28 N7 -64.1(3) . . . . ?
O3 C31 C32 O4 63.1(3) . . . . ?
O4 C33 C34 N6 -61.7(3) . . . . ?
O5 C37 C38 O6 61.1(3) . . . . ?
O6 C39 C40 N7 -66.0(3) . . . . ?
N6 C23 C24 O1 -66.8(3) . . . . ?
N6 C35 C36 O5 -62.2(3) . . . . ?
N7 C29 C30 O3 -66.5(4) . . . . ?
C23 N6 C34 C33 -74.9(3) . . . . ?
C23 N6 C35 C36 159.4(2) . . . . ?
C24 O1 C25 C26 170.8(2) . . . . ?
C25 O1 C24 C23 178.4(2) . . . . ?
C26 O2 C27 C28 -167.1(2) . . . . ?
C27 O2 C26 C25 -176.8(2) . . . . ?
C28 N7 C29 C30 166.5(3) . . . . ?
C28 N7 C40 C39 -73.0(3) . . . . ?
C29 N7 C28 C27 -80.6(3) . . . . ?
C29 N7 C40 C39 167.0(2) . . . . ?
C30 O3 C31 C32 175.5(2) . . . . ?
C31 O3 C30 C29 -179.5(2) . . . . ?
C32 O4 C33 C34 -170.3(2) . . . . ?
C33 O4 C32 C31 176.0(2) . . . . ?
C34 N6 C23 C24 169.6(2) . . . . ?
C34 N6 C35 C36 -79.8(3) . . . . ?
C35 N6 C23 C24 -69.8(3) . . . . ?
C35 N6 C34 C33 163.9(2) . . . . ?
C36 O5 C37 C38 178.0(2) . . . . ?
C37 O5 C36 C35 -164.0(2) . . . . ?
C38 O6 C39 C40 177.2(2) . . . . ?
C39 O6 C38 C37 172.6(2) . . . . ?
C40 N7 C28 C27 159.3(2) . . . . ?
C40 N7 C29 C30 -73.8(3) . . . . ?
C41 O7 C43 C44 178.9(3) . . . . ?
C43 O7 C41 C42 81.0(5) . . . . ?
C45 O8 C47 C48 176.7(3) . . . . ?
C47 O8 C45 C46 179.9(3) . . . . ?

_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.459
_oxdiff_exptl_absorpt_empirical_full_min 0.665
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dkm478
_database_code_depnum_ccdc_archive 'CCDC 2181475'
loop_
_audit_author_name
_audit_author_address
'rosario scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2022-06-23 deposited with the CCDC.	2022-08-31 downloaded from the CCDC.
;
_audit_creation_date             2021-11-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C22 H57 N5 Si6 U), C24 H20 B, C3 H7'
_chemical_formula_sum            'C71 H141 B N10 Si12 U2'
_chemical_formula_weight         1958.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C83 H169 B1 N10 Si12 U2'
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'
B B 0.0090 0.0039 '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'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.1222(2)
_cell_length_b                   15.2178(2)
_cell_length_c                   23.8147(4)
_cell_angle_alpha                98.8987(12)
_cell_angle_beta                 91.1267(12)
_cell_angle_gamma                92.6498(13)
_cell_volume                     5406.63(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    32124
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      76.3760
_cell_measurement_theta_min      3.3670
_shelx_estimated_absorpt_T_max   0.411
_shelx_estimated_absorpt_T_min   0.108
_exptl_absorpt_coefficient_mu    9.910
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1988
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -2 0.0886
0 -1 2 0.0656
-1 2 0 0.1723
0 1 -1 0.0788
0 -1 1 0.0685
1 2 -2 0.0647
-1 -2 2 0.0730
2 2 -1 0.0445
-2 -2 1 0.0677
0 -2 -1 0.1220
2 1 1 0.0462
-2 -1 -1 0.0628
8 -2 9 0.0496
0 -6 -11 0.1237

_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.109
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
0.0008 0.9986 -2.0016 -0.0490 0.1452 -0.0023
-0.0008 -0.9986 2.0016 0.0490 -0.1452 0.0023
-0.9992 1.9985 -0.0014 -0.0239 0.1035 -0.1976
0.0006 0.9990 -1.0010 -0.0525 0.0915 -0.0397
-0.0006 -0.9990 1.0010 0.0525 -0.0915 0.0397
1.0012 1.9981 -2.0016 -0.1930 0.1552 -0.0361
-1.0012 -1.9981 2.0016 0.1930 -0.1552 0.0361
2.0010 1.9987 -1.0006 -0.2845 0.0735 -0.0302
-2.0010 -1.9987 1.0006 0.2845 -0.0735 0.0302
-0.0006 -1.9990 -0.9997 0.1154 -0.0219 0.1917
2.0002 1.0000 1.0010 -0.2355 -0.0717 -0.0278
-2.0002 -1.0000 -1.0010 0.2355 0.0717 0.0278
7.7242 -1.9596 9.2410 -0.6023 -0.7856 0.1413
-0.0243 -5.7073 -11.0589 0.3598 0.3787 0.8527

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66393
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.884
_diffrn_reflns_theta_min         2.926
_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 0.994
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  17.00   1.00    2.50    --  -42.76  75.00 -29.00   70
  2  ω     -8.00  17.00   1.00    2.50    --   42.76 -75.00-157.00   25
  3  ω     41.00  68.00   1.00   10.00    --  112.00 -75.00-157.00   27
  4  ω    112.00 143.00   1.00   10.00    --  112.00  75.00 -29.00   31
  5  ω    -62.00  32.00   1.00    2.50    --  -42.76  37.00-150.00   94
  6  ω   -116.00 -27.00   1.00    2.50    --  -42.76 -37.00-120.00   89
  7  ω   -115.00 -26.00   1.00    2.50    --  -42.76 -57.00  60.00   89
  8  ω     30.00  99.00   1.00    2.50    --   42.76-125.00  90.00   69
  9  ω     35.00  74.00   1.00    2.50    --   42.76 -77.00-180.00   39
 10  ω      1.00  28.00   1.00    2.50    --   42.76 -77.00-180.00   27
 11  ω     68.00 108.00   1.00   10.00    --  112.00-111.00   0.00   40
 12  ω     78.00 176.00   1.00   10.00    --  112.00  15.00  30.00   98
 13  ω     62.00 131.00   1.00   10.00    --  112.00 178.00 120.00   69
 14  ω     42.00  93.00   1.00   10.00    --  112.00 -45.00-120.00   51
 15  ω    106.00 133.00   1.00   10.00    --  112.00 -45.00-120.00   27
 16  ω     72.00 109.00   1.00   10.00    --  112.00-111.00 -90.00   37
 17  ω    109.00 141.00   1.00   10.00    --  112.00 111.00  60.00   32
 18  ω     36.00 109.00   1.00   10.00    --  112.00-111.00-150.00   73
 19  ω    104.00 174.00   1.00   10.00    --  112.00  77.00  90.00   70
 20  ω     57.00 111.00   1.00   10.00    --  112.00 -45.00  60.00   54
 21  ω    104.00 177.00   1.00   10.00    --  112.00  77.00-150.00   73
 22  ω     44.00 109.00   1.00   10.00    --  112.00-111.00 120.00   65
 23  ω     72.00 109.00   1.00   10.00    --  112.00-111.00 -30.00   37
 24  ω     45.00  75.00   1.00   10.00    --  112.00 -94.00  60.00   30
 25  ω     37.00  85.00   1.00   10.00    --  112.00 -77.00-120.00   48
 26  ω    116.00 144.00   1.00   10.00    --  112.00 -77.00-120.00   28
 27  ω    153.00 178.00   1.00   10.00    --  112.00  77.00 150.00   25
 28  ω     36.00  97.00   1.00   10.00    --  112.00-111.00-120.00   61
 29  ω     60.00 116.00   1.00   10.00    --  112.00  15.00-150.00   56
 30  ω    120.00 147.00   1.00   10.00    --  112.00  15.00-150.00   27
 31  ω     36.00  63.00   1.00   10.00    --  112.00 -94.00   0.00   27
 32  ω     45.00 109.00   1.00   10.00    --  112.00-111.00 150.00   64
 33  ω    143.00 170.00   1.00   10.00    --  112.00 111.00  60.00   27
 34  ω     82.00 108.00   1.00   10.00    --  112.00-111.00  30.00   26
 35  ω     81.00 108.00   1.00   10.00    --  112.00-111.00  60.00   27
 36  ω     39.00 109.00   1.00   10.00    --  112.00-111.00  90.00   70
 37  ω    109.00 155.00   1.00   10.00    --  112.00 111.00   0.00   46
 38  ω     37.00  85.00   1.00   10.00    --  112.00-111.00-180.00   48
 39  ω     89.00 171.00   1.00   10.00    --  112.00  45.00 -90.00   82
 40  ω    104.00 140.00   1.00   10.00    --  112.00 111.00-150.00   36
;
_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      -0.0880325000
_diffrn_orient_matrix_UB_12      -0.0559593000
_diffrn_orient_matrix_UB_13      -0.0034631000
_diffrn_orient_matrix_UB_21      -0.0278693000
_diffrn_orient_matrix_UB_22      0.0378159000
_diffrn_orient_matrix_UB_23      -0.0537028000
_diffrn_orient_matrix_UB_31      0.0433800000
_diffrn_orient_matrix_UB_32      -0.0772293000
_diffrn_orient_matrix_UB_33      -0.0373433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17947
_reflns_number_total             22270
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (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)'
_refine_diff_density_max         1.842
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     990
_refine_ls_number_reflns         22270
_refine_ls_number_restraints     385
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.013
_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)+(0.0325P)²+25.8647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1041
_refine_special_details          ?
_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
 Si11-N10 \\sim Si12-N10 \\sim Si13-N11 \\sim Si14-N11
 with sigma of 0.02
 U2-N10 \\sim U2-N11
 with sigma of 0.02
 Si13-C45 \\sim Si11-C41 \\sim Si11-C39 \\sim Si11-C40 \\sim Si13-C46 \\sim
Si13-C47 \\sim Si12-C42 ~
 Si14-C48 \\sim Si12-C44 \\sim Si14-C50 \\sim Si14-C49 \\sim Si12-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si11 \\sim Si12 \\sim Si13 \\sim Si14 \\sim N10 \\sim N11 \\sim C39 \\sim C40
\\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48
\\sim C49 \\sim C50: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
4. Rigid body (RIGU) restrains
 Si11, Si12, Si13, Si14, N10, N11, C39, C40, C41, C42, C43, C44, C45, C46, C47,
  C48, C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Si13)=Sof(Si14)=Sof(N11)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=
 Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(H50C)=1-FVAR(1)
 Sof(Si11)=Sof(Si12)=Sof(N10)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=
 Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C76(H76A,H76B), C77(H77A,H77B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C24(H24), C25(H25), C26(H26), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71),
 C72(H72), C73(H73), C74(H74)
6.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), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C75(H75A,H75B,H75C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.53264(2) 0.13881(2) 0.40185(2) 0.02899(5) Uani 1 1 d . . . . .
Si1 Si 0.73456(10) 0.17768(11) 0.46773(7) 0.0340(3) Uani 1 1 d . . . . .
Si2 Si 0.66042(11) 0.34840(10) 0.45315(7) 0.0338(3) Uani 1 1 d . . . . .
Si3 Si 0.64959(18) 0.07391(12) 0.27449(8) 0.0542(5) Uani 1 1 d . . . . .
Si4 Si 0.46113(18) 0.00758(13) 0.27305(9) 0.0591(6) Uani 1 1 d . . . . .
Si5 Si 0.39024(13) 0.27524(12) 0.34776(8) 0.0439(4) Uani 1 1 d . . . . .
Si6 Si 0.31360(11) 0.20625(12) 0.44633(8) 0.0422(4) Uani 1 1 d . . . . .
N1 N 0.5117(3) 0.1200(3) 0.5055(2) 0.0293(9) Uani 1 1 d . . . . .
N2 N 0.4751(3) 0.0229(3) 0.57479(19) 0.0296(9) Uani 1 1 d . . . . .
N3 N 0.6451(3) 0.2311(3) 0.44177(19) 0.0300(9) Uani 1 1 d . . . . .
N4 N 0.5490(4) 0.0692(3) 0.3117(2) 0.0447(13) Uani 1 1 d . . . . .
N5 N 0.4045(3) 0.2088(3) 0.4013(2) 0.0361(10) Uani 1 1 d . . . . .
C1 C 0.4961(4) 0.0369(3) 0.5214(2) 0.0279(10) Uani 1 1 d . . . . .
C2 C 0.4575(4) 0.0949(4) 0.6119(2) 0.0316(11) Uani 1 1 d . . . . .
H2 H 0.436121 0.087151 0.648151 0.038 Uiso 1 1 calc R U . . .
C3 C 0.4694(4) 0.1805(4) 0.5992(2) 0.0325(11) Uani 1 1 d . . . . .
H3 H 0.457052 0.231071 0.626126 0.039 Uiso 1 1 calc R U . . .
C4 C 0.5000(4) 0.1894(4) 0.5461(2) 0.0310(11) Uani 1 1 d . . . . .
H4 H 0.513334 0.247668 0.537908 0.037 Uiso 1 1 calc R U . . .
C5 C 0.7307(5) 0.0596(4) 0.4315(3) 0.0432(14) Uani 1 1 d . . . . .
H5A H 0.684719 0.025076 0.448253 0.065 Uiso 1 1 calc R U . . .
H5B H 0.788280 0.034207 0.436394 0.065 Uiso 1 1 calc R U . . .
H5C H 0.717213 0.057401 0.390897 0.065 Uiso 1 1 calc R U . . .
C6 C 0.8471(4) 0.2243(5) 0.4524(3) 0.0498(16) Uani 1 1 d . . . . .
H6A H 0.849705 0.229915 0.411978 0.075 Uiso 1 1 calc R U . . .
H6B H 0.892287 0.184328 0.461660 0.075 Uiso 1 1 calc R U . . .
H6C H 0.858090 0.283114 0.475456 0.075 Uiso 1 1 calc R U . . .
C7 C 0.7315(5) 0.1731(6) 0.5454(3) 0.0546(18) Uani 1 1 d . . . . .
H7A H 0.731556 0.233793 0.566439 0.082 Uiso 1 1 calc R U . . .
H7B H 0.783636 0.143723 0.556937 0.082 Uiso 1 1 calc R U . . .
H7C H 0.677694 0.139534 0.553555 0.082 Uiso 1 1 calc R U . . .
C8 C 0.7256(5) 0.3913(4) 0.3967(3) 0.0434(15) Uani 1 1 d . . . . .
H8A H 0.780553 0.359733 0.391429 0.065 Uiso 1 1 calc R U . . .
H8B H 0.739779 0.455180 0.408044 0.065 Uiso 1 1 calc R U . . .
H8C H 0.690702 0.381658 0.360987 0.065 Uiso 1 1 calc R U . . .
C9 C 0.7167(5) 0.3932(4) 0.5233(3) 0.0472(16) Uani 1 1 d . . . . .
H9A H 0.682963 0.372841 0.554019 0.071 Uiso 1 1 calc R U . . .
H9B H 0.719642 0.458459 0.528626 0.071 Uiso 1 1 calc R U . . .
H9C H 0.776726 0.371784 0.523976 0.071 Uiso 1 1 calc R U . . .
C10 C 0.5521(5) 0.4021(5) 0.4566(3) 0.0493(16) Uani 1 1 d . . . . .
H10A H 0.528490 0.402099 0.418010 0.074 Uiso 1 1 calc R U . . .
H10B H 0.560322 0.463565 0.476250 0.074 Uiso 1 1 calc R U . . .
H10C H 0.510343 0.368893 0.477491 0.074 Uiso 1 1 calc R U . . .
C11 C 0.7227(6) 0.1732(4) 0.3058(3) 0.0505(17) Uani 1 1 d . . . . .
H11A H 0.692847 0.227900 0.302112 0.076 Uiso 1 1 calc R U . . .
H11B H 0.778573 0.172615 0.285632 0.076 Uiso 1 1 calc R U . . .
H11C H 0.734912 0.170975 0.346156 0.076 Uiso 1 1 calc R U . . .
C12 C 0.7131(7) -0.0281(5) 0.2755(4) 0.069(2) Uani 1 1 d . . . . .
H12A H 0.721280 -0.038478 0.314808 0.103 Uiso 1 1 calc R U . . .
H12B H 0.771076 -0.019983 0.258805 0.103 Uiso 1 1 calc R U . . .
H12C H 0.680310 -0.079430 0.253346 0.103 Uiso 1 1 calc R U . . .
C13 C 0.6343(8) 0.0846(6) 0.1972(3) 0.076(3) Uani 1 1 d . . . . .
H13A H 0.603523 0.030415 0.176912 0.114 Uiso 1 1 calc R U . . .
H13B H 0.692279 0.092749 0.180553 0.114 Uiso 1 1 calc R U . . .
H13C H 0.599030 0.136036 0.193806 0.114 Uiso 1 1 calc R U . . .
C14 C 0.4175(8) 0.0591(6) 0.2120(3) 0.082(3) Uani 1 1 d . . . . .
H14A H 0.425586 0.124082 0.220974 0.122 Uiso 1 1 calc R U . . .
H14B H 0.354359 0.042359 0.205540 0.122 Uiso 1 1 calc R U . . .
H14C H 0.449821 0.037802 0.177698 0.122 Uiso 1 1 calc R U . . .
C15 C 0.4899(8) -0.1075(5) 0.2396(4) 0.082(3) Uani 1 1 d . . . . .
H15A H 0.540477 -0.103323 0.214926 0.122 Uiso 1 1 calc R U . . .
H15B H 0.438931 -0.136947 0.217080 0.122 Uiso 1 1 calc R U . . .
H15C H 0.505248 -0.142237 0.269519 0.122 Uiso 1 1 calc R U . . .
C16 C 0.3669(6) -0.0081(5) 0.3211(4) 0.066(2) Uani 1 1 d . . . . .
H16A H 0.382127 -0.051199 0.345894 0.099 Uiso 1 1 calc R U . . .
H16B H 0.313708 -0.030361 0.298121 0.099 Uiso 1 1 calc R U . . .
H16C H 0.355525 0.048989 0.344357 0.099 Uiso 1 1 calc R U . . .
C17 C 0.3492(5) 0.3889(5) 0.3737(4) 0.0575(19) Uani 1 1 d . . . . .
H17A H 0.285628 0.383855 0.380443 0.086 Uiso 1 1 calc R U . . .
H17B H 0.359887 0.427544 0.344920 0.086 Uiso 1 1 calc R U . . .
H17C H 0.380866 0.414589 0.409175 0.086 Uiso 1 1 calc R U . . .
C18 C 0.4993(5) 0.2889(5) 0.3133(3) 0.0550(18) Uani 1 1 d . . . . .
H18A H 0.547111 0.295967 0.342248 0.083 Uiso 1 1 calc R U . . .
H18B H 0.499584 0.341699 0.294359 0.083 Uiso 1 1 calc R U . . .
H18C H 0.508366 0.236076 0.285111 0.083 Uiso 1 1 calc R U . . .
C19 C 0.3080(6) 0.2254(6) 0.2907(4) 0.070(2) Uani 1 1 d . . . . .
H19A H 0.330705 0.233722 0.253489 0.105 Uiso 1 1 calc R U . . .
H19B H 0.251881 0.254715 0.296647 0.105 Uiso 1 1 calc R U . . .
H19C H 0.298406 0.161615 0.291960 0.105 Uiso 1 1 calc R U . . .
C20 C 0.3202(5) 0.3038(5) 0.5057(3) 0.0532(18) Uani 1 1 d . . . . .
H20A H 0.373635 0.301295 0.529215 0.080 Uiso 1 1 calc R U . . .
H20B H 0.267822 0.301614 0.529159 0.080 Uiso 1 1 calc R U . . .
H20C H 0.322466 0.359416 0.489654 0.080 Uiso 1 1 calc R U . . .
C21 C 0.3048(5) 0.1000(5) 0.4764(3) 0.0493(16) Uani 1 1 d . . . . .
H21A H 0.329091 0.052144 0.449679 0.074 Uiso 1 1 calc R U . . .
H21B H 0.242434 0.084812 0.482655 0.074 Uiso 1 1 calc R U . . .
H21C H 0.338191 0.107189 0.512634 0.074 Uiso 1 1 calc R U . . .
C22 C 0.2033(5) 0.2083(6) 0.4092(4) 0.064(2) Uani 1 1 d . . . . .
H22A H 0.198206 0.265766 0.395948 0.096 Uiso 1 1 calc R U . . .
H22B H 0.155950 0.199961 0.435621 0.096 Uiso 1 1 calc R U . . .
H22C H 0.198281 0.160277 0.376561 0.096 Uiso 1 1 calc R U . . .
U2 U 0.17003(2) 0.58037(2) 0.09281(2) 0.03444(6) Uani 1 1 d D . . . .
Si7 Si 0.33839(11) 0.73341(12) 0.08244(8) 0.0425(4) Uani 1 1 d . . . . .
Si8 Si 0.24118(12) 0.68450(13) -0.02713(8) 0.0421(4) Uani 1 1 d . . . . .
Si9 Si 0.35154(11) 0.42747(13) 0.09783(7) 0.0405(4) Uani 1 1 d . . . . .
Si10 Si 0.16810(12) 0.36517(15) 0.11264(8) 0.0471(4) Uani 1 1 d . . . . .
Si11 Si 0.0925(5) 0.7801(5) 0.1678(4) 0.0496(14) Uani 0.64(2) 1 d D U P A 1
Si12 Si 0.1400(5) 0.6458(7) 0.2409(3) 0.0530(16) Uani 0.64(2) 1 d D U P A 1
Si13 Si 0.0894(9) 0.7602(11) 0.1839(6) 0.056(2) Uani 0.36(2) 1 d D U P A 2
Si14 Si 0.1408(10) 0.6154(11) 0.2452(6) 0.055(2) Uani 0.36(2) 1 d D U P A 2
N6 N 0.1186(3) 0.4841(3) -0.00077(19) 0.0308(10) Uani 1 1 d . . . . .
N7 N -0.0015(3) 0.4352(4) -0.0707(2) 0.0365(11) Uani 1 1 d . . . . .
N8 N 0.2509(3) 0.6694(3) 0.0446(2) 0.0361(10) Uani 1 1 d . . . . .
N9 N 0.2401(3) 0.4555(4) 0.1013(2) 0.0379(11) Uani 1 1 d . . . . .
N10 N 0.1328(10) 0.6735(8) 0.1718(4) 0.0454(17) Uani 0.64(2) 1 d D U P A 1
N11 N 0.1309(19) 0.6525(14) 0.1786(6) 0.051(2) Uani 0.36(2) 1 d D U P A 2
C23 C 0.0298(4) 0.4774(4) -0.0188(2) 0.0297(11) Uani 1 1 d . . . . .
C24 C 0.0586(4) 0.4044(5) -0.1080(3) 0.0405(14) Uani 1 1 d . . . . .
H24 H 0.039457 0.378928 -0.145421 0.049 Uiso 1 1 calc R U . . .
C25 C 0.1493(4) 0.4085(4) -0.0937(2) 0.0365(13) Uani 1 1 d . . . . .
H25 H 0.191583 0.386532 -0.120712 0.044 Uiso 1 1 calc R U . . .
C26 C 0.1746(4) 0.4459(4) -0.0385(3) 0.0351(12) Uani 1 1 d . . . . .
H26 H 0.234987 0.444312 -0.027078 0.042 Uiso 1 1 calc R U . . .
C27 C 0.4452(4) 0.7309(5) 0.0446(3) 0.0506(16) Uani 1 1 d . . . . .
H27A H 0.459884 0.668964 0.032308 0.076 Uiso 1 1 calc R U . . .
H27B H 0.492241 0.761451 0.070213 0.076 Uiso 1 1 calc R U . . .
H27C H 0.439514 0.761034 0.011238 0.076 Uiso 1 1 calc R U . . .
C28 C 0.3545(5) 0.6904(5) 0.1520(3) 0.0488(16) Uani 1 1 d . . . . .
H28A H 0.309500 0.713732 0.178609 0.073 Uiso 1 1 calc R U . . .
H28B H 0.413573 0.709891 0.168206 0.073 Uiso 1 1 calc R U . . .
H28C H 0.348888 0.625145 0.145380 0.073 Uiso 1 1 calc R U . . .
C29 C 0.3181(6) 0.8562(5) 0.0994(4) 0.063(2) Uani 1 1 d . . . . .
H29A H 0.327666 0.884103 0.065487 0.094 Uiso 1 1 calc R U . . .
H29B H 0.359081 0.884225 0.130064 0.094 Uiso 1 1 calc R U . . .
H29C H 0.256992 0.863792 0.111541 0.094 Uiso 1 1 calc R U . . .
C30 C 0.2672(6) 0.8018(5) -0.0393(4) 0.062(2) Uani 1 1 d . . . . .
H30A H 0.227694 0.842018 -0.016999 0.093 Uiso 1 1 calc R U . . .
H30B H 0.258760 0.805453 -0.079794 0.093 Uiso 1 1 calc R U . . .
H30C H 0.328843 0.819176 -0.027568 0.093 Uiso 1 1 calc R U . . .
C31 C 0.3172(5) 0.6125(5) -0.0723(3) 0.0481(16) Uani 1 1 d . . . . .
H31A H 0.361877 0.650103 -0.087951 0.072 Uiso 1 1 calc R U . . .
H31B H 0.283141 0.575847 -0.103564 0.072 Uiso 1 1 calc R U . . .
H31C H 0.346645 0.573895 -0.049263 0.072 Uiso 1 1 calc R U . . .
C32 C 0.1233(4) 0.6623(5) -0.0539(3) 0.0496(16) Uani 1 1 d . . . . .
H32A H 0.116162 0.601909 -0.075317 0.074 Uiso 1 1 calc R U . . .
H32B H 0.108512 0.705505 -0.078704 0.074 Uiso 1 1 calc R U . . .
H32C H 0.083700 0.667908 -0.021562 0.074 Uiso 1 1 calc R U . . .
C33 C 0.4153(5) 0.4997(5) 0.0552(3) 0.0503(17) Uani 1 1 d . . . . .
H33A H 0.389689 0.492092 0.016546 0.076 Uiso 1 1 calc R U . . .
H33B H 0.477109 0.483121 0.053792 0.076 Uiso 1 1 calc R U . . .
H33C H 0.412584 0.562125 0.072885 0.076 Uiso 1 1 calc R U . . .
C34 C 0.4079(4) 0.4377(6) 0.1695(3) 0.0510(17) Uani 1 1 d . . . . .
H34A H 0.418272 0.500859 0.185271 0.076 Uiso 1 1 calc R U . . .
H34B H 0.464655 0.409087 0.165745 0.076 Uiso 1 1 calc R U . . .
H34C H 0.370242 0.408664 0.194930 0.076 Uiso 1 1 calc R U . . .
C35 C 0.3655(5) 0.3118(5) 0.0599(3) 0.0571(19) Uani 1 1 d . . . . .
H35A H 0.327732 0.269613 0.077035 0.086 Uiso 1 1 calc R U . . .
H35B H 0.427534 0.296871 0.063263 0.086 Uiso 1 1 calc R U . . .
H35C H 0.348537 0.308441 0.019710 0.086 Uiso 1 1 calc R U . . .
C36 C 0.2105(5) 0.2987(7) 0.1671(4) 0.067(2) Uani 1 1 d . . . . .
H36A H 0.266930 0.273904 0.154895 0.100 Uiso 1 1 calc R U . . .
H36B H 0.167293 0.250078 0.170865 0.100 Uiso 1 1 calc R U . . .
H36C H 0.219332 0.337496 0.203827 0.100 Uiso 1 1 calc R U . . .
C37 C 0.0630(5) 0.4104(6) 0.1428(3) 0.0577(19) Uani 1 1 d . . . . .
H37A H 0.076440 0.450107 0.178761 0.086 Uiso 1 1 calc R U . . .
H37B H 0.022786 0.361010 0.149720 0.086 Uiso 1 1 calc R U . . .
H37C H 0.034813 0.443601 0.115862 0.086 Uiso 1 1 calc R U . . .
C38 C 0.1369(6) 0.2845(6) 0.0470(4) 0.062(2) Uani 1 1 d . . . . .
H38A H 0.091924 0.309654 0.024853 0.093 Uiso 1 1 calc R U . . .
H38B H 0.113038 0.228593 0.057708 0.093 Uiso 1 1 calc R U . . .
H38C H 0.189400 0.272848 0.024049 0.093 Uiso 1 1 calc R U . . .
C39 C 0.1705(11) 0.8750(11) 0.2002(7) 0.061(4) Uani 0.64(2) 1 d D U P A 1
H39A H 0.161535 0.887947 0.241220 0.091 Uiso 0.64(2) 1 calc R U P A 1
H39B H 0.158864 0.927893 0.182905 0.091 Uiso 0.64(2) 1 calc R U P A 1
H39C H 0.231678 0.858649 0.193283 0.091 Uiso 0.64(2) 1 calc R U P A 1
C40 C 0.0696(11) 0.7908(12) 0.0919(6) 0.054(3) Uani 0.64(2) 1 d D U P A 1
H40A H 0.123831 0.781228 0.070391 0.082 Uiso 0.64(2) 1 calc R U P A 1
H40B H 0.049703 0.850576 0.089685 0.082 Uiso 0.64(2) 1 calc R U P A 1
H40C H 0.023400 0.746267 0.075858 0.082 Uiso 0.64(2) 1 calc R U P A 1
C41 C -0.0133(8) 0.8022(12) 0.2050(7) 0.061(3) Uani 0.64(2) 1 d D U P A 1
H41A H -0.058819 0.756747 0.189178 0.091 Uiso 0.64(2) 1 calc R U P A 1
H41B H -0.032401 0.861155 0.199745 0.091 Uiso 0.64(2) 1 calc R U P A 1
H41C H -0.004300 0.800447 0.245674 0.091 Uiso 0.64(2) 1 calc R U P A 1
C42 C 0.1838(12) 0.7398(12) 0.2959(6) 0.066(4) Uani 0.64(2) 1 d D U P A 1
H42A H 0.238192 0.766406 0.282466 0.100 Uiso 0.64(2) 1 calc R U P A 1
H42B H 0.196808 0.717312 0.331374 0.100 Uiso 0.64(2) 1 calc R U P A 1
H42C H 0.139507 0.784998 0.302547 0.100 Uiso 0.64(2) 1 calc R U P A 1
C43 C 0.2157(11) 0.5530(12) 0.2446(8) 0.051(3) Uani 0.64(2) 1 d D U P A 1
H43A H 0.199868 0.503751 0.213940 0.077 Uiso 0.64(2) 1 calc R U P A 1
H43B H 0.209946 0.532291 0.281399 0.077 Uiso 0.64(2) 1 calc R U P A 1
H43C H 0.277000 0.574418 0.240475 0.077 Uiso 0.64(2) 1 calc R U P A 1
C44 C 0.0290(8) 0.6090(14) 0.2657(6) 0.063(3) Uani 0.64(2) 1 d D U P A 1
H44A H -0.012158 0.656859 0.265445 0.094 Uiso 0.64(2) 1 calc R U P A 1
H44B H 0.035408 0.595267 0.304388 0.094 Uiso 0.64(2) 1 calc R U P A 1
H44C H 0.005919 0.555790 0.240195 0.094 Uiso 0.64(2) 1 calc R U P A 1
C45 C 0.1676(17) 0.8520(19) 0.2195(11) 0.057(5) Uani 0.36(2) 1 d D U P A 2
H45A H 0.163356 0.856430 0.260853 0.086 Uiso 0.36(2) 1 calc R U P A 2
H45B H 0.151986 0.908414 0.207858 0.086 Uiso 0.36(2) 1 calc R U P A 2
H45C H 0.228246 0.839041 0.208437 0.086 Uiso 0.36(2) 1 calc R U P A 2
C46 C 0.064(2) 0.785(2) 0.1106(9) 0.056(4) Uani 0.36(2) 1 d D U P A 2
H46A H 0.117758 0.779414 0.088133 0.084 Uiso 0.36(2) 1 calc R U P A 2
H46B H 0.043568 0.845192 0.113141 0.084 Uiso 0.36(2) 1 calc R U P A 2
H46C H 0.017836 0.741961 0.092235 0.084 Uiso 0.36(2) 1 calc R U P A 2
C47 C -0.0148(14) 0.776(2) 0.2247(12) 0.059(4) Uani 0.36(2) 1 d D U P A 2
H47A H -0.062509 0.736257 0.205253 0.089 Uiso 0.36(2) 1 calc R U P A 2
H47B H -0.031461 0.838007 0.226978 0.089 Uiso 0.36(2) 1 calc R U P A 2
H47C H -0.005105 0.762323 0.263105 0.089 Uiso 0.36(2) 1 calc R U P A 2
C48 C 0.1767(19) 0.703(2) 0.3066(10) 0.060(5) Uani 0.36(2) 1 d D U P A 2
H48A H 0.221075 0.744422 0.294062 0.089 Uiso 0.36(2) 1 calc R U P A 2
H48B H 0.202506 0.674959 0.337016 0.089 Uiso 0.36(2) 1 calc R U P A 2
H48C H 0.125430 0.735974 0.320885 0.089 Uiso 0.36(2) 1 calc R U P A 2
C49 C 0.228(2) 0.532(2) 0.2423(15) 0.055(4) Uani 0.36(2) 1 d D U P A 2
H49A H 0.200840 0.471932 0.230368 0.082 Uiso 0.36(2) 1 calc R U P A 2
H49B H 0.256150 0.535229 0.280046 0.082 Uiso 0.36(2) 1 calc R U P A 2
H49C H 0.272622 0.544482 0.214997 0.082 Uiso 0.36(2) 1 calc R U P A 2
C50 C 0.0337(13) 0.564(2) 0.2660(12) 0.058(4) Uani 0.36(2) 1 d D U P A 2
H50A H -0.003074 0.610906 0.284439 0.087 Uiso 0.36(2) 1 calc R U P A 2
H50B H 0.045761 0.522372 0.292348 0.087 Uiso 0.36(2) 1 calc R U P A 2
H50C H 0.002361 0.532029 0.231911 0.087 Uiso 0.36(2) 1 calc R U P A 2
C51 C 0.3058(4) 0.3352(4) 0.7897(2) 0.0307(11) Uani 1 1 d . . . . .
C52 C 0.2574(4) 0.2578(4) 0.7959(2) 0.0351(12) Uani 1 1 d . . . . .
H52 H 0.219972 0.229838 0.765192 0.042 Uiso 1 1 calc R U . . .
C53 C 0.2613(5) 0.2191(4) 0.8454(3) 0.0439(14) Uani 1 1 d . . . . .
H53 H 0.227618 0.165493 0.847314 0.053 Uiso 1 1 calc R U . . .
C54 C 0.3141(5) 0.2585(5) 0.8918(3) 0.0477(16) Uani 1 1 d . . . . .
H54 H 0.318347 0.231675 0.925174 0.057 Uiso 1 1 calc R U . . .
C55 C 0.3604(4) 0.3382(5) 0.8880(3) 0.0420(14) Uani 1 1 d . . . . .
H55 H 0.395629 0.367163 0.919463 0.050 Uiso 1 1 calc R U . . .
C56 C 0.3557(4) 0.3758(4) 0.8389(3) 0.0358(12) Uani 1 1 d . . . . .
H56 H 0.387203 0.430985 0.837990 0.043 Uiso 1 1 calc R U . . .
C57 C 0.2416(4) 0.3321(4) 0.6815(2) 0.0332(12) Uani 1 1 d . . . . .
C58 C 0.1766(4) 0.3733(5) 0.6536(3) 0.0398(13) Uani 1 1 d . . . . .
H58 H 0.169263 0.435165 0.664718 0.048 Uiso 1 1 calc R U . . .
C59 C 0.1221(5) 0.3261(6) 0.6099(3) 0.0544(19) Uani 1 1 d . . . . .
H59 H 0.078816 0.356287 0.591822 0.065 Uiso 1 1 calc R U . . .
C60 C 0.1309(5) 0.2362(6) 0.5929(3) 0.057(2) Uani 1 1 d . . . . .
H60 H 0.092485 0.203760 0.564146 0.069 Uiso 1 1 calc R U . . .
C61 C 0.1961(5) 0.1941(5) 0.6180(3) 0.0492(16) Uani 1 1 d . . . . .
H61 H 0.204222 0.132604 0.605838 0.059 Uiso 1 1 calc R U . . .
C62 C 0.2496(4) 0.2415(4) 0.6610(3) 0.0405(13) Uani 1 1 d . . . . .
H62 H 0.294249 0.210947 0.677614 0.049 Uiso 1 1 calc R U . . .
C63 C 0.4089(4) 0.3779(4) 0.7066(2) 0.0303(11) Uani 1 1 d . . . . .
C64 C 0.4796(4) 0.3389(4) 0.7305(2) 0.0318(11) Uani 1 1 d . . . . .
H64 H 0.470106 0.313264 0.763950 0.038 Uiso 1 1 calc R U . . .
C65 C 0.5631(4) 0.3361(4) 0.7073(2) 0.0369(13) Uani 1 1 d . . . . .
H65 H 0.608849 0.307620 0.724346 0.044 Uiso 1 1 calc R U . . .
C66 C 0.5801(4) 0.3747(4) 0.6592(3) 0.0367(13) Uani 1 1 d . . . . .
H66 H 0.637900 0.375285 0.644188 0.044 Uiso 1 1 calc R U . . .
C67 C 0.5116(4) 0.4121(4) 0.6334(2) 0.0341(12) Uani 1 1 d . . . . .
H67 H 0.521635 0.436949 0.599728 0.041 Uiso 1 1 calc R U . . .
C68 C 0.4280(4) 0.4135(4) 0.6569(2) 0.0332(12) Uani 1 1 d . . . . .
H68 H 0.381883 0.439516 0.638491 0.040 Uiso 1 1 calc R U . . .
C69 C 0.2851(4) 0.4869(4) 0.7535(2) 0.0313(11) Uani 1 1 d . . . . .
C70 C 0.1991(4) 0.5067(4) 0.7715(3) 0.0392(13) Uani 1 1 d . . . . .
H70 H 0.155919 0.459210 0.770901 0.047 Uiso 1 1 calc R U . . .
C71 C 0.1750(5) 0.5935(5) 0.7902(3) 0.0457(15) Uani 1 1 d . . . . .
H71 H 0.116063 0.604630 0.801299 0.055 Uiso 1 1 calc R U . . .
C72 C 0.2372(5) 0.6630(4) 0.7926(3) 0.0449(15) Uani 1 1 d . . . . .
H72 H 0.220935 0.722336 0.804742 0.054 Uiso 1 1 calc R U . . .
C73 C 0.3239(5) 0.6467(4) 0.7772(3) 0.0414(14) Uani 1 1 d . . . . .
H73 H 0.367592 0.694156 0.779995 0.050 Uiso 1 1 calc R U . . .
C74 C 0.3454(4) 0.5592(4) 0.7575(2) 0.0368(12) Uani 1 1 d . . . . .
H74 H 0.404444 0.548654 0.746315 0.044 Uiso 1 1 calc R U . . .
B1 B 0.3092(4) 0.3824(4) 0.7328(3) 0.0302(12) Uani 1 1 d . . . . .
C75 C 0.0618(10) -0.0427(10) 0.3716(6) 0.126(5) Uani 1 1 d . . . . .
H75A H 0.058798 -0.009362 0.339658 0.189 Uiso 1 1 calc R U . . .
H75B H 0.038360 -0.103960 0.359345 0.189 Uiso 1 1 calc R U . . .
H75C H 0.123478 -0.043411 0.384844 0.189 Uiso 1 1 calc R U . . .
C76 C 0.0087(8) 0.0001(8) 0.4183(5) 0.086(3) Uani 1 1 d . . . . .
H76A H -0.054442 -0.017012 0.408911 0.103 Uiso 1 1 calc R U . . .
H76B H 0.016067 0.065422 0.419628 0.103 Uiso 1 1 calc R U . . .
C77 C 0.0289(6) -0.0202(6) 0.4762(5) 0.075(3) Uani 1 1 d . . . . .
H77A H 0.091119 -0.000121 0.486416 0.090 Uiso 1 1 calc R U . . .
H77B H 0.024647 -0.085742 0.474401 0.090 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 Si1 3.3901(16) . ?
U1 Si5 3.4262(18) . ?
U1 N1 2.553(5) . ?
U1 N2 2.604(5) 2_656 ?
U1 N3 2.253(5) . ?
U1 N4 2.266(5) . ?
U1 N5 2.255(5) . ?
Si1 N3 1.760(5) . ?
Si1 C5 1.867(6) . ?
Si1 C6 1.878(7) . ?
Si1 C7 1.862(8) . ?
Si2 N3 1.766(5) . ?
Si2 C8 1.862(7) . ?
Si2 C9 1.876(7) . ?
Si2 C10 1.862(7) . ?
Si3 N4 1.779(7) . ?
Si3 C11 1.878(8) . ?
Si3 C12 1.866(8) . ?
Si3 C13 1.884(8) . ?
Si4 N4 1.750(6) . ?
Si4 C14 1.877(8) . ?
Si4 C15 1.882(8) . ?
Si4 C16 1.875(10) . ?
Si5 N5 1.762(5) . ?
Si5 C17 1.882(8) . ?
Si5 C18 1.875(8) . ?
Si5 C19 1.870(8) . ?
Si6 N5 1.762(5) . ?
Si6 C20 1.883(8) . ?
Si6 C21 1.868(7) . ?
Si6 C22 1.876(7) . ?
N1 C1 1.386(7) . ?
N1 C4 1.338(7) . ?
N2 C1 1.363(7) . ?
N2 C2 1.337(7) . ?
C1 C1 1.405(10) 2_656 ?
C2 H2 0.9500 . ?
C2 C3 1.386(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(8) . ?
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 . ?
U2 Si7 3.4090(19) . ?
U2 Si10 3.379(2) . ?
U2 N6 2.557(4) . ?
U2 N7 2.585(5) 2_565 ?
U2 N8 2.242(5) . ?
U2 N9 2.252(5) . ?
U2 N10 2.270(8) . ?
U2 N11 2.267(12) . ?
Si7 N8 1.753(5) . ?
Si7 C27 1.864(7) . ?
Si7 C28 1.890(7) . ?
Si7 C29 1.890(7) . ?
Si8 N8 1.764(5) . ?
Si8 C30 1.878(8) . ?
Si8 C31 1.866(7) . ?
Si8 C32 1.879(6) . ?
Si9 N9 1.758(5) . ?
Si9 C33 1.858(7) . ?
Si9 C34 1.874(7) . ?
Si9 C35 1.873(8) . ?
Si10 N9 1.770(6) . ?
Si10 C36 1.884(8) . ?
Si10 C37 1.873(8) . ?
Si10 C38 1.870(8) . ?
Si11 N10 1.775(9) . ?
Si11 C39 1.880(10) . ?
Si11 C40 1.867(11) . ?
Si11 C41 1.862(9) . ?
Si12 N10 1.764(8) . ?
Si12 C42 1.871(10) . ?
Si12 C43 1.870(11) . ?
Si12 C44 1.880(10) . ?
Si13 N11 1.769(12) . ?
Si13 C45 1.873(13) . ?
Si13 C46 1.876(13) . ?
Si13 C47 1.873(13) . ?
Si14 N11 1.771(12) . ?
Si14 C48 1.875(13) . ?
Si14 C49 1.869(13) . ?
Si14 C50 1.873(13) . ?
N6 C23 1.395(7) . ?
N6 C26 1.334(7) . ?
N7 C23 1.367(7) . ?
N7 C24 1.333(7) . ?
C23 C23 1.409(10) 2_565 ?
C24 H24 0.9500 . ?
C24 C25 1.402(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.389(8) . ?
C26 H26 0.9500 . ?
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 0.9800 . ?
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 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
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 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
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 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.386(9) . ?
C51 C56 1.423(8) . ?
C51 B1 1.629(9) . ?
C52 H52 0.9500 . ?
C52 C53 1.397(9) . ?
C53 H53 0.9500 . ?
C53 C54 1.391(10) . ?
C54 H54 0.9500 . ?
C54 C55 1.388(11) . ?
C55 H55 0.9500 . ?
C55 C56 1.379(9) . ?
C56 H56 0.9500 . ?
C57 C58 1.401(9) . ?
C57 C62 1.401(9) . ?
C57 B1 1.647(8) . ?
C58 H58 0.9500 . ?
C58 C59 1.399(9) . ?
C59 H59 0.9500 . ?
C59 C60 1.379(12) . ?
C60 H60 0.9500 . ?
C60 C61 1.377(11) . ?
C61 H61 0.9500 . ?
C61 C62 1.382(9) . ?
C62 H62 0.9500 . ?
C63 C64 1.400(8) . ?
C63 C68 1.407(8) . ?
C63 B1 1.642(8) . ?
C64 H64 0.9500 . ?
C64 C65 1.389(8) . ?
C65 H65 0.9500 . ?
C65 C66 1.389(9) . ?
C66 H66 0.9500 . ?
C66 C67 1.383(9) . ?
C67 H67 0.9500 . ?
C67 C68 1.393(8) . ?
C68 H68 0.9500 . ?
C69 C70 1.409(8) . ?
C69 C74 1.386(9) . ?
C69 B1 1.649(8) . ?
C70 H70 0.9500 . ?
C70 C71 1.394(9) . ?
C71 H71 0.9500 . ?
C71 C72 1.376(11) . ?
C72 H72 0.9500 . ?
C72 C73 1.390(10) . ?
C73 H73 0.9500 . ?
C73 C74 1.398(8) . ?
C74 H74 0.9500 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C75 C76 1.471(15) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C76 C77 1.488(15) . ?
C77 C77 1.517(19) 2_556 ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Si1 U1 Si5 132.48(4) . . ?
N1 U1 Si1 73.26(11) . . ?
N1 U1 Si5 116.08(11) . . ?
N1 U1 N2 62.69(14) . 2_656 ?
N2 U1 Si1 90.47(11) 2_656 . ?
N2 U1 Si5 136.37(11) 2_656 . ?
N3 U1 Si1 28.12(12) . . ?
N3 U1 Si5 104.53(13) . . ?
N3 U1 N1 81.21(15) . . ?
N3 U1 N2 117.43(16) . 2_656 ?
N3 U1 N4 117.4(2) . . ?
N3 U1 N5 111.79(17) . . ?
N4 U1 Si1 109.16(17) . . ?
N4 U1 Si5 87.80(15) . . ?
N4 U1 N1 146.15(17) . . ?
N4 U1 N2 83.46(17) . 2_656 ?
N5 U1 Si1 137.10(13) . . ?
N5 U1 Si5 27.39(14) . . ?
N5 U1 N1 90.46(17) . . ?
N5 U1 N2 117.30(17) . 2_656 ?
N5 U1 N4 106.1(2) . . ?
N3 Si1 U1 37.12(15) . . ?
N3 Si1 C5 108.6(3) . . ?
N3 Si1 C6 114.9(3) . . ?
N3 Si1 C7 113.9(3) . . ?
C5 Si1 U1 73.8(2) . . ?
C5 Si1 C6 104.8(3) . . ?
C6 Si1 U1 137.9(3) . . ?
C7 Si1 U1 113.0(2) . . ?
C7 Si1 C5 106.1(3) . . ?
C7 Si1 C6 107.7(4) . . ?
N3 Si2 C8 113.0(3) . . ?
N3 Si2 C9 112.9(3) . . ?
N3 Si2 C10 111.0(3) . . ?
C8 Si2 C9 107.6(3) . . ?
C10 Si2 C8 107.9(3) . . ?
C10 Si2 C9 104.0(3) . . ?
N4 Si3 C11 111.3(3) . . ?
N4 Si3 C12 111.9(4) . . ?
N4 Si3 C13 114.2(4) . . ?
C11 Si3 C13 105.1(4) . . ?
C12 Si3 C11 108.2(4) . . ?
C12 Si3 C13 105.7(4) . . ?
N4 Si4 C14 114.2(4) . . ?
N4 Si4 C15 113.8(4) . . ?
N4 Si4 C16 110.1(3) . . ?
C14 Si4 C15 104.2(4) . . ?
C16 Si4 C14 107.9(5) . . ?
C16 Si4 C15 106.0(5) . . ?
N5 Si5 U1 36.07(17) . . ?
N5 Si5 C17 114.4(3) . . ?
N5 Si5 C18 108.3(3) . . ?
N5 Si5 C19 113.5(3) . . ?
C17 Si5 U1 134.5(3) . . ?
C18 Si5 U1 72.9(2) . . ?
C18 Si5 C17 108.6(4) . . ?
C19 Si5 U1 118.9(3) . . ?
C19 Si5 C17 104.3(4) . . ?
C19 Si5 C18 107.4(4) . . ?
N5 Si6 C20 111.4(3) . . ?
N5 Si6 C21 111.5(3) . . ?
N5 Si6 C22 114.0(3) . . ?
C21 Si6 C20 109.9(4) . . ?
C21 Si6 C22 103.0(3) . . ?
C22 Si6 C20 106.6(4) . . ?
C1 N1 U1 121.7(3) . . ?
C4 N1 U1 121.9(4) . . ?
C4 N1 C1 115.4(5) . . ?
C1 N2 U1 119.3(3) . 2_656 ?
C2 N2 U1 124.1(4) . 2_656 ?
C2 N2 C1 116.6(5) . . ?
Si1 N3 U1 114.8(2) . . ?
Si1 N3 Si2 113.1(3) . . ?
Si2 N3 U1 132.1(3) . . ?
Si3 N4 U1 123.5(3) . . ?
Si4 N4 U1 121.5(3) . . ?
Si4 N4 Si3 115.0(3) . . ?
Si5 N5 U1 116.5(3) . . ?
Si5 N5 Si6 113.8(3) . . ?
Si6 N5 U1 129.7(3) . . ?
N1 C1 C1 116.3(6) . 2_656 ?
N2 C1 N1 124.6(5) . . ?
N2 C1 C1 119.1(6) . 2_656 ?
N2 C2 H2 118.9 . . ?
N2 C2 C3 122.2(5) . . ?
C3 C2 H2 118.9 . . ?
C2 C3 H3 121.3 . . ?
C4 C3 C2 117.4(5) . . ?
C4 C3 H3 121.3 . . ?
N1 C4 C3 123.2(5) . . ?
N1 C4 H4 118.4 . . ?
C3 C4 H4 118.4 . . ?
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 . . ?
Si10 U2 Si7 132.27(4) . . ?
N6 U2 Si7 115.36(12) . . ?
N6 U2 Si10 72.25(12) . . ?
N6 U2 N7 62.98(14) . 2_565 ?
N7 U2 Si7 136.70(13) 2_565 . ?
N7 U2 Si10 90.07(13) 2_565 . ?
N8 U2 Si7 27.38(13) . . ?
N8 U2 Si10 136.74(13) . . ?
N8 U2 N6 90.06(17) . . ?
N8 U2 N7 117.06(18) . 2_565 ?
N8 U2 N9 111.26(19) . . ?
N8 U2 N10 103.3(4) . . ?
N8 U2 N11 111.9(7) . . ?
N9 U2 Si7 103.71(14) . . ?
N9 U2 Si10 28.65(14) . . ?
N9 U2 N6 80.48(16) . . ?
N9 U2 N7 117.58(18) . 2_565 ?
N9 U2 N10 120.0(3) . . ?
N9 U2 N11 111.6(5) . . ?
N10 U2 Si7 85.7(4) . . ?
N10 U2 Si10 112.7(3) . . ?
N10 U2 N6 147.5(4) . . ?
N10 U2 N7 84.7(4) . 2_565 ?
N11 U2 Si7 92.4(7) . . ?
N11 U2 Si10 103.1(5) . . ?
N11 U2 N6 146.9(8) . . ?
N8 Si7 U2 36.02(18) . . ?
N8 Si7 C27 114.5(3) . . ?
N8 Si7 C28 107.6(3) . . ?
N8 Si7 C29 114.1(3) . . ?
C27 Si7 U2 134.5(3) . . ?
C27 Si7 C28 109.2(3) . . ?
C27 Si7 C29 103.6(4) . . ?
C28 Si7 U2 72.2(2) . . ?
C28 Si7 C29 107.7(4) . . ?
C29 Si7 U2 119.6(3) . . ?
N8 Si8 C30 114.1(3) . . ?
N8 Si8 C31 111.1(3) . . ?
N8 Si8 C32 110.5(3) . . ?
C30 Si8 C32 103.3(4) . . ?
C31 Si8 C30 106.6(4) . . ?
C31 Si8 C32 111.0(3) . . ?
N9 Si9 C33 110.7(3) . . ?
N9 Si9 C34 113.1(3) . . ?
N9 Si9 C35 112.7(3) . . ?
C33 Si9 C34 107.9(4) . . ?
C33 Si9 C35 104.2(4) . . ?
C35 Si9 C34 107.8(4) . . ?
N9 Si10 U2 37.60(17) . . ?
N9 Si10 C36 114.3(3) . . ?
N9 Si10 C37 108.7(3) . . ?
N9 Si10 C38 114.6(3) . . ?
C36 Si10 U2 138.0(3) . . ?
C37 Si10 U2 73.7(3) . . ?
C37 Si10 C36 104.3(4) . . ?
C38 Si10 U2 113.6(3) . . ?
C38 Si10 C36 107.2(4) . . ?
C38 Si10 C37 107.2(4) . . ?
N10 Si11 C39 113.7(7) . . ?
N10 Si11 C40 109.5(6) . . ?
N10 Si11 C41 114.2(7) . . ?
C40 Si11 C39 108.6(8) . . ?
C41 Si11 C39 104.3(7) . . ?
C41 Si11 C40 106.0(7) . . ?
N10 Si12 C42 113.7(7) . . ?
N10 Si12 C43 111.8(7) . . ?
N10 Si12 C44 111.8(7) . . ?
C42 Si12 C44 106.4(8) . . ?
C43 Si12 C42 105.6(7) . . ?
C43 Si12 C44 107.1(8) . . ?
N11 Si13 C45 114.4(13) . . ?
N11 Si13 C46 109.0(11) . . ?
N11 Si13 C47 115.0(13) . . ?
C45 Si13 C46 107.1(13) . . ?
C47 Si13 C45 104.0(12) . . ?
C47 Si13 C46 106.7(12) . . ?
N11 Si14 C48 115.5(12) . . ?
N11 Si14 C49 109.7(13) . . ?
N11 Si14 C50 111.8(13) . . ?
C49 Si14 C48 104.3(14) . . ?
C49 Si14 C50 109.2(14) . . ?
C50 Si14 C48 106.0(12) . . ?
C23 N6 U2 121.4(3) . . ?
C26 N6 U2 122.9(4) . . ?
C26 N6 C23 115.3(5) . . ?
C23 N7 U2 120.0(3) . 2_565 ?
C24 N7 U2 123.3(4) . 2_565 ?
C24 N7 C23 116.7(5) . . ?
Si7 N8 U2 116.6(3) . . ?
Si7 N8 Si8 113.7(3) . . ?
Si8 N8 U2 129.7(3) . . ?
Si9 N9 U2 133.6(3) . . ?
Si9 N9 Si10 112.6(3) . . ?
Si10 N9 U2 113.7(3) . . ?
Si11 N10 U2 121.7(5) . . ?
Si12 N10 U2 123.2(5) . . ?
Si12 N10 Si11 115.0(4) . . ?
Si13 N11 U2 119.8(8) . . ?
Si13 N11 Si14 112.9(8) . . ?
Si14 N11 U2 127.3(9) . . ?
N6 C23 C23 116.3(6) . 2_565 ?
N7 C23 N6 124.9(5) . . ?
N7 C23 C23 118.7(6) . 2_565 ?
N7 C24 H24 118.9 . . ?
N7 C24 C25 122.2(5) . . ?
C25 C24 H24 118.9 . . ?
C24 C25 H25 121.4 . . ?
C26 C25 C24 117.1(5) . . ?
C26 C25 H25 121.4 . . ?
N6 C26 C25 123.4(5) . . ?
N6 C26 H26 118.3 . . ?
C25 C26 H26 118.3 . . ?
Si7 C27 H27A 109.5 . . ?
Si7 C27 H27B 109.5 . . ?
Si7 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si7 C28 H28A 109.5 . . ?
Si7 C28 H28B 109.5 . . ?
Si7 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si7 C29 H29A 109.5 . . ?
Si7 C29 H29B 109.5 . . ?
Si7 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si8 C31 H31A 109.5 . . ?
Si8 C31 H31B 109.5 . . ?
Si8 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si8 C32 H32A 109.5 . . ?
Si8 C32 H32B 109.5 . . ?
Si8 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si9 C33 H33A 109.5 . . ?
Si9 C33 H33B 109.5 . . ?
Si9 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si9 C34 H34A 109.5 . . ?
Si9 C34 H34B 109.5 . . ?
Si9 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si9 C35 H35A 109.5 . . ?
Si9 C35 H35B 109.5 . . ?
Si9 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si10 C36 H36A 109.5 . . ?
Si10 C36 H36B 109.5 . . ?
Si10 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si10 C37 H37A 109.5 . . ?
Si10 C37 H37B 109.5 . . ?
Si10 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si10 C38 H38A 109.5 . . ?
Si10 C38 H38B 109.5 . . ?
Si10 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si11 C39 H39A 109.5 . . ?
Si11 C39 H39B 109.5 . . ?
Si11 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
Si11 C40 H40A 109.5 . . ?
Si11 C40 H40B 109.5 . . ?
Si11 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Si11 C41 H41A 109.5 . . ?
Si11 C41 H41B 109.5 . . ?
Si11 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
Si12 C42 H42A 109.5 . . ?
Si12 C42 H42B 109.5 . . ?
Si12 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si12 C43 H43A 109.5 . . ?
Si12 C43 H43B 109.5 . . ?
Si12 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si12 C44 H44A 109.5 . . ?
Si12 C44 H44B 109.5 . . ?
Si12 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si13 C45 H45A 109.5 . . ?
Si13 C45 H45B 109.5 . . ?
Si13 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Si13 C46 H46A 109.5 . . ?
Si13 C46 H46B 109.5 . . ?
Si13 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Si13 C47 H47A 109.5 . . ?
Si13 C47 H47B 109.5 . . ?
Si13 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
Si14 C48 H48A 109.5 . . ?
Si14 C48 H48B 109.5 . . ?
Si14 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si14 C49 H49A 109.5 . . ?
Si14 C49 H49B 109.5 . . ?
Si14 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Si14 C50 H50A 109.5 . . ?
Si14 C50 H50B 109.5 . . ?
Si14 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 C56 114.8(6) . . ?
C52 C51 B1 126.5(5) . . ?
C56 C51 B1 118.7(5) . . ?
C51 C52 H52 118.5 . . ?
C51 C52 C53 122.9(6) . . ?
C53 C52 H52 118.5 . . ?
C52 C53 H53 119.7 . . ?
C54 C53 C52 120.6(6) . . ?
C54 C53 H53 119.7 . . ?
C53 C54 H54 121.0 . . ?
C55 C54 C53 118.0(6) . . ?
C55 C54 H54 121.0 . . ?
C54 C55 H55 119.6 . . ?
C56 C55 C54 120.8(6) . . ?
C56 C55 H55 119.6 . . ?
C51 C56 H56 118.7 . . ?
C55 C56 C51 122.7(6) . . ?
C55 C56 H56 118.7 . . ?
C58 C57 C62 114.9(6) . . ?
C58 C57 B1 125.3(5) . . ?
C62 C57 B1 119.7(5) . . ?
C57 C58 H58 119.0 . . ?
C59 C58 C57 122.0(7) . . ?
C59 C58 H58 119.0 . . ?
C58 C59 H59 119.8 . . ?
C60 C59 C58 120.4(7) . . ?
C60 C59 H59 119.8 . . ?
C59 C60 H60 120.4 . . ?
C61 C60 C59 119.1(7) . . ?
C61 C60 H60 120.4 . . ?
C60 C61 H61 120.1 . . ?
C60 C61 C62 119.8(7) . . ?
C62 C61 H61 120.1 . . ?
C57 C62 H62 118.2 . . ?
C61 C62 C57 123.6(7) . . ?
C61 C62 H62 118.2 . . ?
C64 C63 C68 115.2(5) . . ?
C64 C63 B1 124.1(5) . . ?
C68 C63 B1 120.7(5) . . ?
C63 C64 H64 118.7 . . ?
C65 C64 C63 122.7(6) . . ?
C65 C64 H64 118.7 . . ?
C64 C65 H65 119.8 . . ?
C66 C65 C64 120.3(6) . . ?
C66 C65 H65 119.8 . . ?
C65 C66 H66 120.5 . . ?
C67 C66 C65 118.9(5) . . ?
C67 C66 H66 120.6 . . ?
C66 C67 H67 120.0 . . ?
C66 C67 C68 120.0(6) . . ?
C68 C67 H67 120.0 . . ?
C63 C68 H68 118.6 . . ?
C67 C68 C63 122.8(6) . . ?
C67 C68 H68 118.6 . . ?
C70 C69 B1 119.7(5) . . ?
C74 C69 C70 115.6(5) . . ?
C74 C69 B1 124.6(5) . . ?
C69 C70 H70 118.8 . . ?
C71 C70 C69 122.4(6) . . ?
C71 C70 H70 118.8 . . ?
C70 C71 H71 120.2 . . ?
C72 C71 C70 119.6(6) . . ?
C72 C71 H71 120.2 . . ?
C71 C72 H72 119.9 . . ?
C71 C72 C73 120.3(6) . . ?
C73 C72 H72 119.9 . . ?
C72 C73 H73 120.6 . . ?
C72 C73 C74 118.8(6) . . ?
C74 C73 H73 120.6 . . ?
C69 C74 C73 123.4(6) . . ?
C69 C74 H74 118.3 . . ?
C73 C74 H74 118.3 . . ?
C51 B1 C57 112.7(5) . . ?
C51 B1 C63 110.1(5) . . ?
C51 B1 C69 105.9(4) . . ?
C57 B1 C69 112.2(5) . . ?
C63 B1 C57 105.8(4) . . ?
C63 B1 C69 110.3(5) . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C76 C75 H75A 109.5 . . ?
C76 C75 H75B 109.5 . . ?
C76 C75 H75C 109.5 . . ?
C75 C76 H76A 108.1 . . ?
C75 C76 H76B 108.1 . . ?
C75 C76 C77 117.0(11) . . ?
H76A C76 H76B 107.3 . . ?
C77 C76 H76A 108.1 . . ?
C77 C76 H76B 108.1 . . ?
C76 C77 C77 117.0(11) . 2_556 ?
C76 C77 H77A 108.1 . . ?
C76 C77 H77B 108.1 . . ?
C77 C77 H77A 108.1 2_556 . ?
C77 C77 H77B 108.1 2_556 . ?
H77A C77 H77B 107.3 . . ?

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 179.1(4) . . . . ?
U1 Si5 N5 Si6 -179.0(5) . . . . ?
U1 N1 C1 N2 -172.7(4) . . . . ?
U1 N1 C1 C1 8.0(8) . . . 2_656 ?
U1 N1 C4 C3 165.3(4) . . . . ?
U1 N2 C1 N1 -172.6(4) 2_656 . . . ?
U1 N2 C1 C1 6.7(8) 2_656 . . 2_656 ?
U1 N2 C2 C3 174.6(4) 2_656 . . . ?
N2 C2 C3 C4 0.4(9) . . . . ?
C1 N1 C4 C3 -3.7(8) . . . . ?
C1 N2 C2 C3 -7.0(8) . . . . ?
C2 N2 C1 N1 8.9(8) . . . . ?
C2 N2 C1 C1 -171.8(6) . . . 2_656 ?
C2 C3 C4 N1 5.3(9) . . . . ?
C4 N1 C1 N2 -3.7(8) . . . . ?
C4 N1 C1 C1 177.0(6) . . . 2_656 ?
C5 Si1 N3 U1 21.0(3) . . . . ?
C5 Si1 N3 Si2 -159.9(3) . . . . ?
C6 Si1 N3 U1 138.0(3) . . . . ?
C6 Si1 N3 Si2 -42.9(4) . . . . ?
C7 Si1 N3 U1 -97.0(3) . . . . ?
C7 Si1 N3 Si2 82.1(4) . . . . ?
C8 Si2 N3 U1 -96.5(4) . . . . ?
C8 Si2 N3 Si1 84.6(4) . . . . ?
C9 Si2 N3 U1 141.1(3) . . . . ?
C9 Si2 N3 Si1 -37.8(4) . . . . ?
C10 Si2 N3 U1 24.8(4) . . . . ?
C10 Si2 N3 Si1 -154.1(3) . . . . ?
C11 Si3 N4 U1 -21.4(5) . . . . ?
C11 Si3 N4 Si4 157.6(3) . . . . ?
C12 Si3 N4 U1 99.8(4) . . . . ?
C12 Si3 N4 Si4 -81.2(5) . . . . ?
C13 Si3 N4 U1 -140.3(4) . . . . ?
C13 Si3 N4 Si4 38.7(5) . . . . ?
C14 Si4 N4 U1 110.8(5) . . . . ?
C14 Si4 N4 Si3 -68.2(5) . . . . ?
C15 Si4 N4 U1 -129.6(4) . . . . ?
C15 Si4 N4 Si3 51.3(5) . . . . ?
C16 Si4 N4 U1 -10.8(5) . . . . ?
C16 Si4 N4 Si3 170.2(4) . . . . ?
C17 Si5 N5 U1 -133.1(3) . . . . ?
C17 Si5 N5 Si6 47.8(4) . . . . ?
C18 Si5 N5 U1 -11.8(4) . . . . ?
C18 Si5 N5 Si6 169.1(3) . . . . ?
C19 Si5 N5 U1 107.3(4) . . . . ?
C19 Si5 N5 Si6 -71.7(5) . . . . ?
C20 Si6 N5 U1 96.3(4) . . . . ?
C20 Si6 N5 Si5 -84.8(4) . . . . ?
C21 Si6 N5 U1 -26.9(5) . . . . ?
C21 Si6 N5 Si5 152.0(3) . . . . ?
C22 Si6 N5 U1 -143.0(4) . . . . ?
C22 Si6 N5 Si5 35.9(5) . . . . ?
U2 Si7 N8 Si8 -179.2(5) . . . . ?
U2 Si10 N9 Si9 -178.9(4) . . . . ?
U2 N6 C23 N7 172.8(5) . . . . ?
U2 N6 C23 C23 -3.3(9) . . . 2_565 ?
U2 N6 C26 C25 -166.9(5) . . . . ?
U2 N7 C23 N6 175.2(4) 2_565 . . . ?
U2 N7 C23 C23 -8.8(9) 2_565 . . 2_565 ?
U2 N7 C24 C25 -175.7(5) 2_565 . . . ?
N7 C24 C25 C26 0.2(11) . . . . ?
C23 N6 C26 C25 5.3(9) . . . . ?
C23 N7 C24 C25 4.9(10) . . . . ?
C24 N7 C23 N6 -5.4(10) . . . . ?
C24 N7 C23 C23 170.6(7) . . . 2_565 ?
C24 C25 C26 N6 -5.7(10) . . . . ?
C26 N6 C23 N7 0.4(9) . . . . ?
C26 N6 C23 C23 -175.6(7) . . . 2_565 ?
C27 Si7 N8 U2 133.1(3) . . . . ?
C27 Si7 N8 Si8 -46.1(4) . . . . ?
C28 Si7 N8 U2 11.6(4) . . . . ?
C28 Si7 N8 Si8 -167.6(3) . . . . ?
C29 Si7 N8 U2 -107.8(4) . . . . ?
C29 Si7 N8 Si8 73.0(5) . . . . ?
C30 Si8 N8 U2 144.3(4) . . . . ?
C30 Si8 N8 Si7 -36.6(4) . . . . ?
C31 Si8 N8 U2 -95.2(4) . . . . ?
C31 Si8 N8 Si7 83.9(4) . . . . ?
C32 Si8 N8 U2 28.5(5) . . . . ?
C32 Si8 N8 Si7 -152.5(3) . . . . ?
C33 Si9 N9 U2 -24.4(5) . . . . ?
C33 Si9 N9 Si10 154.2(3) . . . . ?
C34 Si9 N9 U2 96.8(4) . . . . ?
C34 Si9 N9 Si10 -84.5(4) . . . . ?
C35 Si9 N9 U2 -140.6(4) . . . . ?
C35 Si9 N9 Si10 38.0(4) . . . . ?
C36 Si10 N9 U2 -138.5(4) . . . . ?
C36 Si10 N9 Si9 42.6(5) . . . . ?
C37 Si10 N9 U2 -22.5(4) . . . . ?
C37 Si10 N9 Si9 158.6(3) . . . . ?
C38 Si10 N9 U2 97.3(4) . . . . ?
C38 Si10 N9 Si9 -81.6(4) . . . . ?
C39 Si11 N10 U2 -112.3(9) . . . . ?
C39 Si11 N10 Si12 68.4(10) . . . . ?
C40 Si11 N10 U2 9.4(11) . . . . ?
C40 Si11 N10 Si12 -169.9(8) . . . . ?
C41 Si11 N10 U2 128.1(8) . . . . ?
C41 Si11 N10 Si12 -51.2(10) . . . . ?
C42 Si12 N10 U2 139.2(9) . . . . ?
C42 Si12 N10 Si11 -41.6(11) . . . . ?
C43 Si12 N10 U2 19.7(12) . . . . ?
C43 Si12 N10 Si11 -161.1(9) . . . . ?
C44 Si12 N10 U2 -100.3(9) . . . . ?
C44 Si12 N10 Si11 78.9(10) . . . . ?
C45 Si13 N11 U2 -108.2(16) . . . . ?
C45 Si13 N11 Si14 69.4(18) . . . . ?
C46 Si13 N11 U2 12(2) . . . . ?
C46 Si13 N11 Si14 -170.7(15) . . . . ?
C47 Si13 N11 U2 131.4(15) . . . . ?
C47 Si13 N11 Si14 -51.0(19) . . . . ?
C48 Si14 N11 U2 140.5(17) . . . . ?
C48 Si14 N11 Si13 -37(2) . . . . ?
C49 Si14 N11 U2 23(2) . . . . ?
C49 Si14 N11 Si13 -154.4(17) . . . . ?
C50 Si14 N11 U2 -98.2(19) . . . . ?
C50 Si14 N11 Si13 84.4(17) . . . . ?
C51 C52 C53 C54 1.1(9) . . . . ?
C52 C51 C56 C55 4.0(8) . . . . ?
C52 C51 B1 C57 4.1(8) . . . . ?
C52 C51 B1 C63 -113.8(6) . . . . ?
C52 C51 B1 C69 127.0(6) . . . . ?
C52 C53 C54 C55 1.8(10) . . . . ?
C53 C54 C55 C56 -1.6(10) . . . . ?
C54 C55 C56 C51 -1.4(9) . . . . ?
C56 C51 C52 C53 -3.8(8) . . . . ?
C56 C51 B1 C57 -175.2(5) . . . . ?
C56 C51 B1 C63 66.9(6) . . . . ?
C56 C51 B1 C69 -52.3(6) . . . . ?
C57 C58 C59 C60 0.2(11) . . . . ?
C58 C57 C62 C61 -2.3(9) . . . . ?
C58 C57 B1 C51 125.7(6) . . . . ?
C58 C57 B1 C63 -114.0(6) . . . . ?
C58 C57 B1 C69 6.3(8) . . . . ?
C58 C59 C60 C61 -2.3(12) . . . . ?
C59 C60 C61 C62 2.1(11) . . . . ?
C60 C61 C62 C57 0.2(11) . . . . ?
C62 C57 C58 C59 2.1(9) . . . . ?
C62 C57 B1 C51 -57.2(7) . . . . ?
C62 C57 B1 C63 63.2(7) . . . . ?
C62 C57 B1 C69 -176.5(5) . . . . ?
C63 C64 C65 C66 1.5(9) . . . . ?
C64 C63 C68 C67 -1.4(8) . . . . ?
C64 C63 B1 C51 -0.1(7) . . . . ?
C64 C63 B1 C57 -122.2(6) . . . . ?
C64 C63 B1 C69 116.3(6) . . . . ?
C64 C65 C66 C67 -2.9(9) . . . . ?
C65 C66 C67 C68 2.2(9) . . . . ?
C66 C67 C68 C63 0.0(9) . . . . ?
C68 C63 C64 C65 0.6(8) . . . . ?
C68 C63 B1 C51 179.2(5) . . . . ?
C68 C63 B1 C57 57.1(6) . . . . ?
C68 C63 B1 C69 -64.4(6) . . . . ?
C69 C70 C71 C72 -1.4(10) . . . . ?
C70 C69 C74 C73 -0.9(9) . . . . ?
C70 C69 B1 C51 -67.9(6) . . . . ?
C70 C69 B1 C57 55.3(7) . . . . ?
C70 C69 B1 C63 173.0(5) . . . . ?
C70 C71 C72 C73 -1.0(10) . . . . ?
C71 C72 C73 C74 2.2(10) . . . . ?
C72 C73 C74 C69 -1.3(10) . . . . ?
C74 C69 C70 C71 2.2(9) . . . . ?
C74 C69 B1 C51 108.6(6) . . . . ?
C74 C69 B1 C57 -128.2(6) . . . . ?
C74 C69 B1 C63 -10.5(8) . . . . ?
B1 C51 C52 C53 176.9(5) . . . . ?
B1 C51 C56 C55 -176.6(5) . . . . ?
B1 C57 C58 C59 179.3(6) . . . . ?
B1 C57 C62 C61 -179.7(6) . . . . ?
B1 C63 C64 C65 180.0(5) . . . . ?
B1 C63 C68 C67 179.2(5) . . . . ?
B1 C69 C70 C71 179.1(6) . . . . ?
B1 C69 C74 C73 -177.5(6) . . . . ?
C75 C76 C77 C77 -177.0(12) . . . 2_556 ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 211 electrons were 
found in a volume of 1336Å³ in 1 void per unit cell. 
This is consistent with the presence of 
2[C6H14] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
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 -0.052 -0.941 -0.941 1335.5 210.9 '4 C6H14'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2021-03-19
_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 1.700
_oxdiff_exptl_absorpt_empirical_full_min 0.642
