# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_dkm246
_database_code_depnum_ccdc_archive 'CCDC 2039849'
loop_
_audit_author_name
_audit_author_address
'rosario scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2021-03-26 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-08-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H64 N3 Si6 U, C18 H36 K N2 O6'
_chemical_formula_sum            'C50 H100 K N5 O6 Si6 U'
_chemical_formula_weight         1313.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H100 K N5 O6 Si6 U'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.66789(14)
_cell_length_b                   17.47136(16)
_cell_length_c                   24.16489(19)
_cell_angle_alpha                90
_cell_angle_beta                 93.6596(8)
_cell_angle_gamma                90
_cell_volume                     6601.39(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20811
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5720
_cell_measurement_theta_min      3.1120
_shelx_estimated_absorpt_T_max   0.718
_shelx_estimated_absorpt_T_min   0.270
_exptl_absorpt_coefficient_mu    8.875
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.41.78a (Rigaku Oxford Diffraction, 2020)
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2712
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0654
0 0 -1 0.1319
0 -1 0 0.0847
-1 0 0 0.0180
1 0 0 0.0190
1 2 -2 0.1083
1 2 1 0.0739

_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
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
0.0004 -0.0001 0.9982 0.0478 -0.0196 0.0374
-0.0004 0.0001 -0.9982 -0.0478 0.0196 -0.0374
-0.0004 -0.9993 -0.0005 0.0569 0.0126 -0.0661
-0.9996 0.0003 0.0036 -0.0190 -0.0906 -0.0337
0.9996 -0.0003 -0.0036 0.0190 0.0906 0.0337
0.9997 1.9985 -1.9991 -0.1904 0.1047 0.0910
1.0008 1.9982 0.9957 -0.0470 0.0459 0.2032

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33861
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.677
_diffrn_reflns_theta_min         3.123
_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 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -112.00 -78.00   1.00    4.00    --  -40.91 -55.00 -59.00   34
  2  ω    -69.00  30.00   1.00    4.00    --  -40.91  55.00  83.00   99
  3  ω     50.00  96.00   1.00    4.00    --   40.91  55.00  83.00   46
  4  ω     -6.00  35.00   1.00    4.00    --   40.91 -55.00 -59.00   41
  5  ω     97.00 175.00   1.00   16.00    --  105.15  55.00  83.00   78
  6  ω     39.00 130.00   1.00   16.00    --  105.15 -55.00 -59.00   91
  7  ω    -20.00  73.00   1.00    4.00    --   40.91 -77.00-120.00   93
  8  ω     49.00  97.00   1.00    4.00    --   40.91-125.00-150.00   48
  9  ω    133.00 160.00   1.00   16.00    --  105.15  30.00-180.00   27
 10  ω     32.00 131.00   1.00   16.00    --  105.15 -45.00 150.00   99
 11  ω     25.00 154.00   1.00   16.00    --  105.15 -15.00 -90.00  129
 12  ω    135.00 162.00   1.00   16.00    --  105.15 111.00-120.00   27
 13  ω     98.00 129.00   1.00   16.00    --  105.15  30.00-180.00   31
 14  ω    119.00 172.00   1.00   16.00    --  105.15 111.00   0.00   53
;
_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      0.0191395000
_diffrn_orient_matrix_UB_12      -0.0569694000
_diffrn_orient_matrix_UB_13      0.0478599000
_diffrn_orient_matrix_UB_21      0.0905869000
_diffrn_orient_matrix_UB_22      -0.0125961000
_diffrn_orient_matrix_UB_23      -0.0196688000
_diffrn_orient_matrix_UB_31      0.0338716000
_diffrn_orient_matrix_UB_32      0.0660628000
_diffrn_orient_matrix_UB_33      0.0374433000
_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                11775
_reflns_number_total             12806
_reflns_odcompleteness_completeness 99.76
_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 1.171.41.78a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.78a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.78a (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, 2015)'
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12806
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0273
_refine_ls_restrained_S_all      1.051
_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)+(0.0284P)²+12.4631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0665
_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. Uiso/Uaniso restraints and constraints
K1 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim N4 \\sim N5
\\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\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
3.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
  C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_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 0.23252(2) 0.27931(2) 0.28902(2) 0.02127(4) Uani 1 1 d . . . . .
Si1 Si 0.08931(5) 0.32120(5) 0.39803(3) 0.02478(17) Uani 1 1 d . . . . .
Si2 Si 0.25123(6) 0.24269(6) 0.43018(4) 0.02976(19) Uani 1 1 d . . . . .
Si3 Si 0.36050(9) 0.43908(8) 0.30242(5) 0.0524(3) Uani 1 1 d . . . . .
Si4 Si 0.46686(7) 0.29825(9) 0.30104(5) 0.0508(3) Uani 1 1 d . . . . .
Si5 Si 0.26801(5) 0.18150(5) 0.17012(3) 0.02607(18) Uani 1 1 d . . . . .
Si6 Si 0.21441(6) 0.08033(5) 0.26158(4) 0.02901(19) Uani 1 1 d . . . . .
N1 N 0.18569(17) 0.28472(16) 0.37919(10) 0.0238(5) Uani 1 1 d . . . . .
N2 N 0.36624(19) 0.3411(2) 0.29854(12) 0.0394(7) Uani 1 1 d . . . . .
N3 N 0.24751(16) 0.16778(16) 0.23869(11) 0.0239(5) Uani 1 1 d . . . . .
C1 C 0.0959(2) 0.29700(18) 0.24539(12) 0.0236(6) Uani 1 1 d . . . . .
C2 C 0.1448(2) 0.35392(19) 0.22760(13) 0.0266(7) Uani 1 1 d . . . . .
C3 C 0.0048(2) 0.2789(2) 0.23045(13) 0.0283(7) Uani 1 1 d . . . . .
C4 C -0.0575(2) 0.3363(2) 0.22090(16) 0.0387(8) Uani 1 1 d . . . . .
H4 H -0.040912 0.388565 0.222065 0.046 Uiso 1 1 calc R U . . .
C5 C -0.1430(3) 0.3173(3) 0.20981(19) 0.0499(11) Uani 1 1 d . . . . .
H5 H -0.184247 0.356734 0.203712 0.060 Uiso 1 1 calc R U . . .
C6 C -0.1686(2) 0.2417(3) 0.20755(18) 0.0489(11) Uani 1 1 d . . . . .
H6 H -0.227129 0.229041 0.200116 0.059 Uiso 1 1 calc R U . . .
C7 C -0.1079(3) 0.1846(3) 0.21623(17) 0.0449(10) Uani 1 1 d . . . . .
H7 H -0.124698 0.132410 0.213986 0.054 Uiso 1 1 calc R U . . .
C8 C -0.0230(2) 0.2035(2) 0.22816(15) 0.0348(8) Uani 1 1 d . . . . .
H8 H 0.017488 0.163587 0.234994 0.042 Uiso 1 1 calc R U . . .
C9 C 0.1243(2) 0.4135(2) 0.18590(14) 0.0285(7) Uani 1 1 d . . . . .
C10 C 0.1022(3) 0.4877(2) 0.20133(16) 0.0401(9) Uani 1 1 d . . . . .
H10 H 0.100119 0.499724 0.239557 0.048 Uiso 1 1 calc R U . . .
C11 C 0.0831(3) 0.5439(2) 0.16216(18) 0.0460(10) Uani 1 1 d . . . . .
H11 H 0.068232 0.593831 0.173866 0.055 Uiso 1 1 calc R U . . .
C12 C 0.0855(3) 0.5284(2) 0.10628(17) 0.0453(10) Uani 1 1 d . . . . .
H12 H 0.072116 0.566966 0.079425 0.054 Uiso 1 1 calc R U . . .
C13 C 0.1077(3) 0.4557(2) 0.09021(16) 0.0433(9) Uani 1 1 d . . . . .
H13 H 0.109803 0.444300 0.051882 0.052 Uiso 1 1 calc R U . . .
C14 C 0.1269(2) 0.3991(2) 0.12903(14) 0.0336(8) Uani 1 1 d . . . . .
H14 H 0.142236 0.349508 0.116894 0.040 Uiso 1 1 calc R U . . .
C15 C 0.0458(3) 0.4047(2) 0.35634(15) 0.0406(9) Uani 1 1 d . . . . .
H15A H 0.083075 0.449210 0.363210 0.061 Uiso 1 1 calc R U . . .
H15B H -0.011878 0.416838 0.367232 0.061 Uiso 1 1 calc R U . . .
H15C H 0.043411 0.391772 0.316818 0.061 Uiso 1 1 calc R U . . .
C16 C 0.0051(2) 0.2450(2) 0.39486(18) 0.0421(9) Uani 1 1 d . . . . .
H16A H -0.013487 0.234826 0.356064 0.063 Uiso 1 1 calc R U . . .
H16B H -0.043905 0.262230 0.414854 0.063 Uiso 1 1 calc R U . . .
H16C H 0.028550 0.198041 0.412013 0.063 Uiso 1 1 calc R U . . .
C17 C 0.0964(2) 0.3621(3) 0.47022(14) 0.0395(9) Uani 1 1 d . . . . .
H17A H 0.105995 0.320555 0.497189 0.059 Uiso 1 1 calc R U . . .
H17B H 0.042935 0.388488 0.477014 0.059 Uiso 1 1 calc R U . . .
H17C H 0.144083 0.398405 0.474060 0.059 Uiso 1 1 calc R U . . .
C18 C 0.1958(3) 0.1759(3) 0.47760(16) 0.0449(10) Uani 1 1 d . . . . .
H18A H 0.152025 0.204133 0.496442 0.067 Uiso 1 1 calc R U . . .
H18B H 0.237731 0.154592 0.505224 0.067 Uiso 1 1 calc R U . . .
H18C H 0.168683 0.134174 0.455765 0.067 Uiso 1 1 calc R U . . .
C19 C 0.3136(3) 0.3133(3) 0.47559(17) 0.0469(10) Uani 1 1 d . . . . .
H19A H 0.342099 0.350019 0.452309 0.070 Uiso 1 1 calc R U . . .
H19B H 0.356504 0.285966 0.499319 0.070 Uiso 1 1 calc R U . . .
H19C H 0.274503 0.340638 0.498774 0.070 Uiso 1 1 calc R U . . .
C20 C 0.3348(3) 0.1817(3) 0.39904(17) 0.0442(9) Uani 1 1 d . . . . .
H20A H 0.306720 0.142894 0.374878 0.066 Uiso 1 1 calc R U . . .
H20B H 0.369757 0.156423 0.428736 0.066 Uiso 1 1 calc R U . . .
H20C H 0.371276 0.213972 0.377285 0.066 Uiso 1 1 calc R U . . .
C21 C 0.2585(3) 0.4690(3) 0.3330(2) 0.0559(12) Uani 1 1 d . . . . .
H21A H 0.209562 0.448941 0.310145 0.084 Uiso 1 1 calc R U . . .
H21B H 0.255338 0.524996 0.334057 0.084 Uiso 1 1 calc R U . . .
H21C H 0.257201 0.448672 0.370730 0.084 Uiso 1 1 calc R U . . .
C22 C 0.4463(4) 0.4862(4) 0.3489(3) 0.088(2) Uani 1 1 d . . . . .
H22A H 0.444772 0.465648 0.386511 0.132 Uiso 1 1 calc R U . . .
H22B H 0.436428 0.541583 0.349526 0.132 Uiso 1 1 calc R U . . .
H22C H 0.502421 0.475924 0.334682 0.132 Uiso 1 1 calc R U . . .
C23 C 0.3627(5) 0.4855(4) 0.2330(2) 0.085(2) Uani 1 1 d . . . . .
H23A H 0.416551 0.473037 0.216608 0.128 Uiso 1 1 calc R U . . .
H23B H 0.358070 0.541131 0.237213 0.128 Uiso 1 1 calc R U . . .
H23C H 0.314586 0.466789 0.208859 0.128 Uiso 1 1 calc R U . . .
C24 C 0.4652(3) 0.1959(3) 0.2789(2) 0.0564(12) Uani 1 1 d . . . . .
H24A H 0.417302 0.169587 0.294862 0.085 Uiso 1 1 calc R U . . .
H24B H 0.519028 0.171253 0.291874 0.085 Uiso 1 1 calc R U . . .
H24C H 0.458473 0.193064 0.238359 0.085 Uiso 1 1 calc R U . . .
C25 C 0.5410(4) 0.3453(4) 0.2533(3) 0.085(2) Uani 1 1 d . . . . .
H25A H 0.512883 0.348668 0.215942 0.128 Uiso 1 1 calc R U . . .
H25B H 0.593396 0.314944 0.252096 0.128 Uiso 1 1 calc R U . . .
H25C H 0.555252 0.396872 0.266885 0.128 Uiso 1 1 calc R U . . .
C26 C 0.5210(3) 0.3019(4) 0.3730(2) 0.0752(18) Uani 1 1 d . . . . .
H26A H 0.535789 0.355010 0.382496 0.113 Uiso 1 1 calc R U . . .
H26B H 0.573122 0.270813 0.374215 0.113 Uiso 1 1 calc R U . . .
H26C H 0.482131 0.281790 0.399715 0.113 Uiso 1 1 calc R U . . .
C27 C 0.3187(2) 0.2772(2) 0.15968(15) 0.0346(8) Uani 1 1 d . . . . .
H27A H 0.283057 0.317437 0.174518 0.052 Uiso 1 1 calc R U . . .
H27B H 0.324098 0.285924 0.119990 0.052 Uiso 1 1 calc R U . . .
H27C H 0.375603 0.278331 0.179087 0.052 Uiso 1 1 calc R U . . .
C28 C 0.1689(2) 0.1782(2) 0.12219(14) 0.0364(8) Uani 1 1 d . . . . .
H28A H 0.150594 0.124924 0.116942 0.055 Uiso 1 1 calc R U . . .
H28B H 0.181164 0.200384 0.086301 0.055 Uiso 1 1 calc R U . . .
H28C H 0.123369 0.207554 0.138319 0.055 Uiso 1 1 calc R U . . .
C29 C 0.3455(2) 0.1095(2) 0.14431(16) 0.0406(9) Uani 1 1 d . . . . .
H29A H 0.401464 0.116285 0.164172 0.061 Uiso 1 1 calc R U . . .
H29B H 0.350888 0.117091 0.104507 0.061 Uiso 1 1 calc R U . . .
H29C H 0.324379 0.057692 0.150815 0.061 Uiso 1 1 calc R U . . .
C30 C 0.3078(3) 0.0165(2) 0.28191(19) 0.0475(10) Uani 1 1 d . . . . .
H30A H 0.341593 0.007991 0.249712 0.071 Uiso 1 1 calc R U . . .
H30B H 0.286809 -0.032712 0.295018 0.071 Uiso 1 1 calc R U . . .
H30C H 0.343647 0.040880 0.311593 0.071 Uiso 1 1 calc R U . . .
C31 C 0.1482(2) 0.0915(2) 0.32310(15) 0.0360(8) Uani 1 1 d . . . . .
H31A H 0.185453 0.104288 0.355908 0.054 Uiso 1 1 calc R U . . .
H31B H 0.118127 0.043453 0.329596 0.054 Uiso 1 1 calc R U . . .
H31C H 0.106352 0.132597 0.315929 0.054 Uiso 1 1 calc R U . . .
C32 C 0.1448(3) 0.0255(2) 0.20968(17) 0.0433(9) Uani 1 1 d . . . . .
H32A H 0.092892 0.055085 0.199724 0.065 Uiso 1 1 calc R U . . .
H32B H 0.129011 -0.023617 0.225749 0.065 Uiso 1 1 calc R U . . .
H32C H 0.175919 0.016352 0.176412 0.065 Uiso 1 1 calc R U . . .
K1 K 0.72090(5) 0.24087(5) 0.49773(3) 0.03492(16) Uani 1 1 d . . . . .
O1 O 0.74190(19) 0.28043(16) 0.38870(11) 0.0427(6) Uani 1 1 d . U . . .
O2 O 0.7054(3) 0.1315(2) 0.41336(14) 0.0808(12) Uani 1 1 d . U . . .
O3 O 0.8346(2) 0.1475(3) 0.56083(14) 0.0731(10) Uani 1 1 d . U . . .
O4 O 0.88523(19) 0.2949(2) 0.52850(12) 0.0593(9) Uani 1 1 d . U . . .
O5 O 0.62160(16) 0.36341(18) 0.53702(13) 0.0456(7) Uani 1 1 d . U . . .
O6 O 0.5689(2) 0.2090(2) 0.55111(14) 0.0610(9) Uani 1 1 d . U . . .
N4 N 0.7654(2) 0.4021(2) 0.47017(16) 0.0479(8) Uani 1 1 d . U . . .
N5 N 0.6725(4) 0.0760(3) 0.52320(19) 0.0731(12) Uani 1 1 d . U . . .
C33 C 0.7454(3) 0.4129(3) 0.4104(2) 0.0552(11) Uani 1 1 d . U . . .
H33A H 0.770080 0.462257 0.399145 0.066 Uiso 1 1 calc R U . . .
H33B H 0.682504 0.416561 0.403618 0.066 Uiso 1 1 calc R U . . .
C34 C 0.7778(3) 0.3503(2) 0.37386(18) 0.0471(10) Uani 1 1 d . U . . .
H34A H 0.761600 0.361778 0.334456 0.056 Uiso 1 1 calc R U . . .
H34B H 0.840921 0.347424 0.378589 0.056 Uiso 1 1 calc R U . . .
C35 C 0.7645(3) 0.2187(3) 0.35450(17) 0.0477(10) Uani 1 1 d . U . . .
H35A H 0.824680 0.204011 0.364175 0.057 Uiso 1 1 calc R U . . .
H35B H 0.760292 0.235432 0.315279 0.057 Uiso 1 1 calc R U . . .
C36 C 0.7106(4) 0.1535(3) 0.3606(2) 0.0719(14) Uani 1 1 d . U . . .
H36A H 0.652417 0.165729 0.344595 0.086 Uiso 1 1 calc R U . . .
H36B H 0.732694 0.110347 0.339146 0.086 Uiso 1 1 calc R U . . .
C37 C 0.6468(5) 0.0679(3) 0.4209(2) 0.0845(17) Uani 1 1 d . U . . .
H37A H 0.647164 0.032155 0.389133 0.101 Uiso 1 1 calc R U . . .
H37B H 0.587772 0.087145 0.423699 0.101 Uiso 1 1 calc R U . . .
C38 C 0.6772(5) 0.0287(3) 0.4731(2) 0.0837(17) Uani 1 1 d . U . . .
H38A H 0.642597 -0.018091 0.477355 0.100 Uiso 1 1 calc R U . . .
H38B H 0.737290 0.012539 0.469911 0.100 Uiso 1 1 calc R U . . .
C39 C 0.7330(5) 0.0488(4) 0.5671(3) 0.0934(19) Uani 1 1 d . U . . .
H39A H 0.727001 -0.007392 0.570608 0.112 Uiso 1 1 calc R U . . .
H39B H 0.718553 0.072015 0.602713 0.112 Uiso 1 1 calc R U . . .
C40 C 0.8231(5) 0.0670(4) 0.5574(3) 0.0948(19) Uani 1 1 d . U . . .
H40A H 0.861848 0.041230 0.585506 0.114 Uiso 1 1 calc R U . . .
H40B H 0.836999 0.048614 0.520248 0.114 Uiso 1 1 calc R U . . .
C41 C 0.9208(4) 0.1679(5) 0.5587(2) 0.0823(17) Uani 1 1 d . U . . .
H41A H 0.940074 0.157665 0.521186 0.099 Uiso 1 1 calc R U . . .
H41B H 0.956274 0.137099 0.585718 0.099 Uiso 1 1 calc R U . . .
C42 C 0.9306(3) 0.2488(4) 0.57167(19) 0.0710(15) Uani 1 1 d . U . . .
H42A H 0.992007 0.262507 0.574195 0.085 Uiso 1 1 calc R U . . .
H42B H 0.907232 0.259646 0.607982 0.085 Uiso 1 1 calc R U . . .
C43 C 0.8884(3) 0.3732(4) 0.5379(2) 0.0654(14) Uani 1 1 d . U . . .
H43A H 0.947719 0.388820 0.549090 0.078 Uiso 1 1 calc R U . . .
H43B H 0.851535 0.386695 0.568217 0.078 Uiso 1 1 calc R U . . .
C44 C 0.8579(3) 0.4144(3) 0.4855(2) 0.0624(13) Uani 1 1 d . U . . .
H44A H 0.868520 0.469940 0.490457 0.075 Uiso 1 1 calc R U . . .
H44B H 0.891646 0.396605 0.454722 0.075 Uiso 1 1 calc R U . . .
C45 C 0.7145(3) 0.4558(3) 0.5012(2) 0.0614(13) Uani 1 1 d . U . . .
H45A H 0.715690 0.506616 0.483157 0.074 Uiso 1 1 calc R U . . .
H45B H 0.741274 0.461168 0.539204 0.074 Uiso 1 1 calc R U . . .
C46 C 0.6228(3) 0.4314(3) 0.5047(2) 0.0567(12) Uani 1 1 d . U . . .
H46A H 0.589988 0.472260 0.522216 0.068 Uiso 1 1 calc R U . . .
H46B H 0.596162 0.421753 0.467091 0.068 Uiso 1 1 calc R U . . .
C47 C 0.5367(3) 0.3413(3) 0.5465(2) 0.0562(12) Uani 1 1 d . U . . .
H47A H 0.504776 0.330222 0.510693 0.067 Uiso 1 1 calc R U . . .
H47B H 0.507225 0.383333 0.564953 0.067 Uiso 1 1 calc R U . . .
C48 C 0.5391(3) 0.2721(3) 0.5820(2) 0.0650(14) Uani 1 1 d . U . . .
H48A H 0.577842 0.280671 0.615406 0.078 Uiso 1 1 calc R U . . .
H48B H 0.481208 0.261034 0.594091 0.078 Uiso 1 1 calc R U . . .
C49 C 0.5671(5) 0.1389(4) 0.5810(3) 0.0842(17) Uani 1 1 d . U . . .
H49A H 0.510333 0.131708 0.595976 0.101 Uiso 1 1 calc R U . . .
H49B H 0.610889 0.139680 0.612374 0.101 Uiso 1 1 calc R U . . .
C50 C 0.5851(5) 0.0745(3) 0.5417(3) 0.0856(17) Uani 1 1 d . U . . .
H50A H 0.575679 0.025032 0.560426 0.103 Uiso 1 1 calc R U . . .
H50B H 0.544117 0.077542 0.508896 0.103 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 Si2 3.4644(9) . ?
U1 Si3 3.4401(11) . ?
U1 Si5 3.4189(8) . ?
U1 N1 2.345(2) . ?
U1 N2 2.355(3) . ?
U1 N3 2.317(3) . ?
U1 C1 2.345(3) . ?
U1 C2 2.352(3) . ?
Si1 N1 1.727(3) . ?
Si1 C15 1.877(4) . ?
Si1 C16 1.873(4) . ?
Si1 C17 1.881(4) . ?
Si2 N1 1.718(3) . ?
Si2 C18 1.886(4) . ?
Si2 C19 1.882(4) . ?
Si2 C20 1.882(4) . ?
Si3 N2 1.716(4) . ?
Si3 C21 1.878(5) . ?
Si3 C22 1.885(5) . ?
Si3 C23 1.865(5) . ?
Si4 N2 1.743(4) . ?
Si4 C24 1.867(5) . ?
Si4 C25 1.878(5) . ?
Si4 C26 1.887(5) . ?
Si5 N3 1.724(3) . ?
Si5 C27 1.876(4) . ?
Si5 C28 1.877(4) . ?
Si5 C29 1.881(4) . ?
Si6 N3 1.716(3) . ?
Si6 C30 1.880(4) . ?
Si6 C31 1.877(4) . ?
Si6 C32 1.873(4) . ?
C1 C2 1.342(5) . ?
C1 C3 1.485(5) . ?
C2 C9 1.470(5) . ?
C3 C4 1.407(5) . ?
C3 C8 1.388(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.380(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(5) . ?
C9 C14 1.400(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.384(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.380(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(5) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
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 . ?
K1 O1 2.764(3) . ?
K1 O2 2.794(3) . ?
K1 O3 2.795(4) . ?
K1 O4 2.798(3) . ?
K1 O5 2.845(3) . ?
K1 O6 2.836(3) . ?
K1 N4 2.987(4) . ?
K1 N5 3.051(4) . ?
O1 C34 1.401(5) . ?
O1 C35 1.418(5) . ?
O2 C36 1.340(7) . ?
O2 C37 1.460(7) . ?
O3 C40 1.419(8) . ?
O3 C41 1.401(7) . ?
O4 C42 1.465(6) . ?
O4 C43 1.387(7) . ?
O5 C46 1.422(6) . ?
O5 C47 1.417(5) . ?
O6 C48 1.426(6) . ?
O6 C49 1.421(7) . ?
N4 C33 1.472(6) . ?
N4 C44 1.488(6) . ?
N4 C45 1.467(5) . ?
N5 C38 1.473(7) . ?
N5 C39 1.457(8) . ?
N5 C50 1.468(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.513(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.431(7) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.487(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.481(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.454(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.507(8) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.507(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.481(8) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.511(8) . ?
C50 H50A 0.9900 . ?
C50 H50B 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
Si3 U1 Si2 92.58(3) . . ?
Si5 U1 Si2 136.64(2) . . ?
Si5 U1 Si3 111.07(3) . . ?
N1 U1 Si2 26.42(7) . . ?
N1 U1 Si3 95.45(7) . . ?
N1 U1 Si5 151.44(7) . . ?
N1 U1 N2 102.71(10) . . ?
N1 U1 C2 111.06(10) . . ?
N2 U1 Si2 88.26(8) . . ?
N2 U1 Si3 27.02(10) . . ?
N2 U1 Si5 96.89(8) . . ?
N3 U1 Si2 110.89(7) . . ?
N3 U1 Si3 130.83(7) . . ?
N3 U1 Si5 27.26(7) . . ?
N3 U1 N1 124.74(9) . . ?
N3 U1 N2 108.52(11) . . ?
N3 U1 C1 89.71(10) . . ?
N3 U1 C2 102.10(10) . . ?
C1 U1 Si2 118.98(8) . . ?
C1 U1 Si3 116.43(8) . . ?
C1 U1 Si5 83.15(7) . . ?
C1 U1 N1 94.70(10) . . ?
C1 U1 N2 139.82(12) . . ?
C1 U1 C2 33.22(11) . . ?
C2 U1 Si2 137.15(8) . . ?
C2 U1 Si3 85.60(9) . . ?
C2 U1 Si5 82.32(8) . . ?
C2 U1 N2 106.72(12) . . ?
N1 Si1 C15 116.07(15) . . ?
N1 Si1 C16 110.64(16) . . ?
N1 Si1 C17 112.55(15) . . ?
C15 Si1 C17 101.58(18) . . ?
C16 Si1 C15 107.4(2) . . ?
C16 Si1 C17 107.91(19) . . ?
N1 Si2 U1 37.41(9) . . ?
N1 Si2 C18 115.01(17) . . ?
N1 Si2 C19 113.72(18) . . ?
N1 Si2 C20 110.77(16) . . ?
C18 Si2 U1 134.35(14) . . ?
C19 Si2 U1 117.46(15) . . ?
C19 Si2 C18 107.1(2) . . ?
C20 Si2 U1 74.23(13) . . ?
C20 Si2 C18 104.6(2) . . ?
C20 Si2 C19 104.84(19) . . ?
N2 Si3 U1 38.57(10) . . ?
N2 Si3 C21 110.36(18) . . ?
N2 Si3 C22 115.5(3) . . ?
N2 Si3 C23 112.4(2) . . ?
C21 Si3 U1 75.94(14) . . ?
C21 Si3 C22 103.7(3) . . ?
C22 Si3 U1 143.1(2) . . ?
C23 Si3 U1 108.21(19) . . ?
C23 Si3 C21 107.3(3) . . ?
C23 Si3 C22 107.0(3) . . ?
N2 Si4 C24 113.96(18) . . ?
N2 Si4 C25 112.6(3) . . ?
N2 Si4 C26 111.7(2) . . ?
C24 Si4 C25 104.0(3) . . ?
C24 Si4 C26 107.1(3) . . ?
C25 Si4 C26 107.0(3) . . ?
N3 Si5 U1 37.98(9) . . ?
N3 Si5 C27 111.08(15) . . ?
N3 Si5 C28 113.03(15) . . ?
N3 Si5 C29 112.90(16) . . ?
C27 Si5 U1 76.14(11) . . ?
C27 Si5 C28 106.58(18) . . ?
C27 Si5 C29 105.28(18) . . ?
C28 Si5 U1 111.19(12) . . ?
C28 Si5 C29 107.47(18) . . ?
C29 Si5 U1 139.08(13) . . ?
N3 Si6 C30 111.48(17) . . ?
N3 Si6 C31 110.89(15) . . ?
N3 Si6 C32 114.50(16) . . ?
C31 Si6 C30 108.37(18) . . ?
C32 Si6 C30 106.4(2) . . ?
C32 Si6 C31 104.81(18) . . ?
Si1 N1 U1 126.20(14) . . ?
Si2 N1 U1 116.17(13) . . ?
Si2 N1 Si1 117.48(15) . . ?
Si3 N2 U1 114.40(17) . . ?
Si3 N2 Si4 118.50(18) . . ?
Si4 N2 U1 127.09(19) . . ?
Si5 N3 U1 114.76(14) . . ?
Si6 N3 U1 122.45(13) . . ?
Si6 N3 Si5 120.80(16) . . ?
C2 C1 U1 73.7(2) . . ?
C2 C1 C3 129.7(3) . . ?
C3 C1 U1 156.6(2) . . ?
C1 C2 U1 73.12(19) . . ?
C1 C2 C9 129.8(3) . . ?
C9 C2 U1 156.7(2) . . ?
C4 C3 C1 122.3(3) . . ?
C8 C3 C1 120.4(3) . . ?
C8 C3 C4 117.2(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.4 . . ?
C5 C6 C7 119.3(4) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.1(4) . . ?
C8 C7 H7 119.9 . . ?
C3 C8 H8 119.0 . . ?
C7 C8 C3 122.0(4) . . ?
C7 C8 H8 119.0 . . ?
C10 C9 C2 121.4(3) . . ?
C10 C9 C14 116.8(3) . . ?
C14 C9 C2 121.8(3) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 C9 121.5(4) . . ?
C11 C10 H10 119.3 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.7(4) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 120.7 . . ?
C13 C12 C11 118.7(4) . . ?
C13 C12 H12 120.7 . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C9 C14 H14 119.4 . . ?
C13 C14 C9 121.2(3) . . ?
C13 C14 H14 119.4 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18A 109.5 . . ?
Si2 C18 H18B 109.5 . . ?
Si2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si3 C23 H23A 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si4 C25 H25A 109.5 . . ?
Si4 C25 H25B 109.5 . . ?
Si4 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si4 C26 H26A 109.5 . . ?
Si4 C26 H26B 109.5 . . ?
Si4 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si5 C27 H27A 109.5 . . ?
Si5 C27 H27B 109.5 . . ?
Si5 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si5 C28 H28A 109.5 . . ?
Si5 C28 H28B 109.5 . . ?
Si5 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si5 C29 H29A 109.5 . . ?
Si5 C29 H29B 109.5 . . ?
Si5 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si6 C30 H30A 109.5 . . ?
Si6 C30 H30B 109.5 . . ?
Si6 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si6 C31 H31A 109.5 . . ?
Si6 C31 H31B 109.5 . . ?
Si6 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si6 C32 H32A 109.5 . . ?
Si6 C32 H32B 109.5 . . ?
Si6 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O1 K1 O2 59.03(10) . . ?
O1 K1 O3 123.76(10) . . ?
O1 K1 O4 90.31(9) . . ?
O1 K1 O5 103.35(9) . . ?
O1 K1 O6 129.60(10) . . ?
O1 K1 N4 60.52(9) . . ?
O1 K1 N5 118.34(11) . . ?
O2 K1 O3 91.23(13) . . ?
O2 K1 O4 117.40(13) . . ?
O2 K1 O5 137.27(12) . . ?
O2 K1 O6 99.28(12) . . ?
O2 K1 N4 119.54(11) . . ?
O2 K1 N5 59.36(11) . . ?
O3 K1 O4 60.56(13) . . ?
O3 K1 O5 126.88(11) . . ?
O3 K1 O6 99.29(12) . . ?
O3 K1 N4 121.49(12) . . ?
O3 K1 N5 59.78(14) . . ?
O4 K1 O5 99.85(10) . . ?
O4 K1 O6 136.96(10) . . ?
O4 K1 N4 61.13(11) . . ?
O4 K1 N5 120.06(14) . . ?
O5 K1 N4 60.35(9) . . ?
O5 K1 N5 119.66(11) . . ?
O6 K1 O5 60.20(9) . . ?
O6 K1 N4 120.11(10) . . ?
O6 K1 N5 59.73(12) . . ?
N4 K1 N5 178.57(13) . . ?
C34 O1 K1 122.4(2) . . ?
C34 O1 C35 113.2(3) . . ?
C35 O1 K1 114.5(2) . . ?
C36 O2 K1 119.4(3) . . ?
C36 O2 C37 114.4(4) . . ?
C37 O2 K1 117.1(3) . . ?
C40 O3 K1 118.2(4) . . ?
C41 O3 K1 114.4(3) . . ?
C41 O3 C40 111.6(5) . . ?
C42 O4 K1 113.6(3) . . ?
C43 O4 K1 113.5(3) . . ?
C43 O4 C42 114.5(4) . . ?
C46 O5 K1 114.8(2) . . ?
C47 O5 K1 112.8(3) . . ?
C47 O5 C46 111.2(4) . . ?
C48 O6 K1 113.5(3) . . ?
C49 O6 K1 116.4(3) . . ?
C49 O6 C48 112.5(4) . . ?
C33 N4 K1 107.6(2) . . ?
C33 N4 C44 111.7(4) . . ?
C44 N4 K1 108.6(3) . . ?
C45 N4 K1 110.3(3) . . ?
C45 N4 C33 109.3(4) . . ?
C45 N4 C44 109.4(4) . . ?
C38 N5 K1 109.8(3) . . ?
C39 N5 K1 107.3(4) . . ?
C39 N5 C38 110.6(5) . . ?
C39 N5 C50 110.4(5) . . ?
C50 N5 K1 109.1(3) . . ?
C50 N5 C38 109.7(5) . . ?
N4 C33 H33A 108.5 . . ?
N4 C33 H33B 108.5 . . ?
N4 C33 C34 114.9(4) . . ?
H33A C33 H33B 107.5 . . ?
C34 C33 H33A 108.5 . . ?
C34 C33 H33B 108.5 . . ?
O1 C34 C33 109.0(3) . . ?
O1 C34 H34A 109.9 . . ?
O1 C34 H34B 109.9 . . ?
C33 C34 H34A 109.9 . . ?
C33 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
O1 C35 H35A 109.2 . . ?
O1 C35 H35B 109.2 . . ?
O1 C35 C36 112.0(4) . . ?
H35A C35 H35B 107.9 . . ?
C36 C35 H35A 109.2 . . ?
C36 C35 H35B 109.2 . . ?
O2 C36 C35 113.5(5) . . ?
O2 C36 H36A 108.9 . . ?
O2 C36 H36B 108.9 . . ?
C35 C36 H36A 108.9 . . ?
C35 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
O2 C37 H37A 110.4 . . ?
O2 C37 H37B 110.4 . . ?
O2 C37 C38 106.6(5) . . ?
H37A C37 H37B 108.6 . . ?
C38 C37 H37A 110.4 . . ?
C38 C37 H37B 110.4 . . ?
N5 C38 C37 114.1(5) . . ?
N5 C38 H38A 108.7 . . ?
N5 C38 H38B 108.7 . . ?
C37 C38 H38A 108.7 . . ?
C37 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
N5 C39 H39A 108.9 . . ?
N5 C39 H39B 108.9 . . ?
N5 C39 C40 113.3(5) . . ?
H39A C39 H39B 107.7 . . ?
C40 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
O3 C40 C39 108.8(6) . . ?
O3 C40 H40A 109.9 . . ?
O3 C40 H40B 109.9 . . ?
C39 C40 H40A 109.9 . . ?
C39 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
O3 C41 H41A 109.8 . . ?
O3 C41 H41B 109.8 . . ?
O3 C41 C42 109.2(5) . . ?
H41A C41 H41B 108.3 . . ?
C42 C41 H41A 109.8 . . ?
C42 C41 H41B 109.8 . . ?
O4 C42 H42A 109.7 . . ?
O4 C42 H42B 109.7 . . ?
C41 C42 O4 109.9(4) . . ?
C41 C42 H42A 109.7 . . ?
C41 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
O4 C43 H43A 109.9 . . ?
O4 C43 H43B 109.9 . . ?
O4 C43 C44 109.2(4) . . ?
H43A C43 H43B 108.3 . . ?
C44 C43 H43A 109.9 . . ?
C44 C43 H43B 109.9 . . ?
N4 C44 C43 113.0(4) . . ?
N4 C44 H44A 109.0 . . ?
N4 C44 H44B 109.0 . . ?
C43 C44 H44A 109.0 . . ?
C43 C44 H44B 109.0 . . ?
H44A C44 H44B 107.8 . . ?
N4 C45 H45A 108.9 . . ?
N4 C45 H45B 108.9 . . ?
N4 C45 C46 113.6(4) . . ?
H45A C45 H45B 107.7 . . ?
C46 C45 H45A 108.9 . . ?
C46 C45 H45B 108.9 . . ?
O5 C46 C45 108.2(4) . . ?
O5 C46 H46A 110.1 . . ?
O5 C46 H46B 110.1 . . ?
C45 C46 H46A 110.1 . . ?
C45 C46 H46B 110.1 . . ?
H46A C46 H46B 108.4 . . ?
O5 C47 H47A 109.9 . . ?
O5 C47 H47B 109.9 . . ?
O5 C47 C48 109.1(4) . . ?
H47A C47 H47B 108.3 . . ?
C48 C47 H47A 109.9 . . ?
C48 C47 H47B 109.9 . . ?
O6 C48 C47 108.9(4) . . ?
O6 C48 H48A 109.9 . . ?
O6 C48 H48B 109.9 . . ?
C47 C48 H48A 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
O6 C49 H49A 110.1 . . ?
O6 C49 H49B 110.1 . . ?
O6 C49 C50 108.2(4) . . ?
H49A C49 H49B 108.4 . . ?
C50 C49 H49A 110.1 . . ?
C50 C49 H49B 110.1 . . ?
N5 C50 C49 113.1(5) . . ?
N5 C50 H50A 109.0 . . ?
N5 C50 H50B 109.0 . . ?
C49 C50 H50A 109.0 . . ?
C49 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?

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 Si2 N1 Si1 176.0(3) . . . . ?
U1 Si3 N2 Si4 179.2(3) . . . . ?
U1 Si5 N3 Si6 164.3(3) . . . . ?
U1 C1 C2 C9 175.1(4) . . . . ?
U1 C1 C3 C4 146.5(5) . . . . ?
U1 C1 C3 C8 -30.2(7) . . . . ?
U1 C2 C9 C10 -92.1(6) . . . . ?
U1 C2 C9 C14 87.2(7) . . . . ?
C1 C2 C9 C10 99.8(5) . . . . ?
C1 C2 C9 C14 -80.9(5) . . . . ?
C1 C3 C4 C5 -176.7(3) . . . . ?
C1 C3 C8 C7 177.8(3) . . . . ?
C2 C1 C3 C4 -37.1(5) . . . . ?
C2 C1 C3 C8 146.2(4) . . . . ?
C2 C9 C10 C11 179.8(4) . . . . ?
C2 C9 C14 C13 -179.9(4) . . . . ?
C3 C1 C2 U1 -178.5(4) . . . . ?
C3 C1 C2 C9 -3.4(6) . . . . ?
C3 C4 C5 C6 -0.4(6) . . . . ?
C4 C3 C8 C7 0.9(5) . . . . ?
C4 C5 C6 C7 -0.3(7) . . . . ?
C5 C6 C7 C8 1.3(6) . . . . ?
C6 C7 C8 C3 -1.7(6) . . . . ?
C8 C3 C4 C5 0.1(5) . . . . ?
C9 C10 C11 C12 0.0(7) . . . . ?
C10 C9 C14 C13 -0.6(6) . . . . ?
C10 C11 C12 C13 -0.3(7) . . . . ?
C11 C12 C13 C14 0.3(7) . . . . ?
C12 C13 C14 C9 0.2(6) . . . . ?
C14 C9 C10 C11 0.5(6) . . . . ?
C15 Si1 N1 U1 -33.8(2) . . . . ?
C15 Si1 N1 Si2 150.68(19) . . . . ?
C16 Si1 N1 U1 89.0(2) . . . . ?
C16 Si1 N1 Si2 -86.6(2) . . . . ?
C17 Si1 N1 U1 -150.20(19) . . . . ?
C17 Si1 N1 Si2 34.3(2) . . . . ?
C18 Si2 N1 U1 -131.29(18) . . . . ?
C18 Si2 N1 Si1 44.7(2) . . . . ?
C19 Si2 N1 U1 104.75(19) . . . . ?
C19 Si2 N1 Si1 -79.3(2) . . . . ?
C20 Si2 N1 U1 -13.0(2) . . . . ?
C20 Si2 N1 Si1 163.0(2) . . . . ?
C21 Si3 N2 U1 28.2(2) . . . . ?
C21 Si3 N2 Si4 -152.5(2) . . . . ?
C22 Si3 N2 U1 145.5(3) . . . . ?
C22 Si3 N2 Si4 -35.3(3) . . . . ?
C23 Si3 N2 U1 -91.5(3) . . . . ?
C23 Si3 N2 Si4 87.8(3) . . . . ?
C24 Si4 N2 U1 13.7(3) . . . . ?
C24 Si4 N2 Si3 -165.5(2) . . . . ?
C25 Si4 N2 U1 131.7(3) . . . . ?
C25 Si4 N2 Si3 -47.4(3) . . . . ?
C26 Si4 N2 U1 -107.8(3) . . . . ?
C26 Si4 N2 Si3 73.0(3) . . . . ?
C27 Si5 N3 U1 24.36(19) . . . . ?
C27 Si5 N3 Si6 -171.30(17) . . . . ?
C28 Si5 N3 U1 -95.38(18) . . . . ?
C28 Si5 N3 Si6 69.0(2) . . . . ?
C29 Si5 N3 U1 142.36(17) . . . . ?
C29 Si5 N3 Si6 -53.3(2) . . . . ?
C30 Si6 N3 U1 -110.0(2) . . . . ?
C30 Si6 N3 Si5 86.9(2) . . . . ?
C31 Si6 N3 U1 10.8(2) . . . . ?
C31 Si6 N3 Si5 -152.28(18) . . . . ?
C32 Si6 N3 U1 129.17(18) . . . . ?
C32 Si6 N3 Si5 -33.9(2) . . . . ?
K1 O1 C34 C33 -39.6(5) . . . . ?
K1 O1 C35 C36 48.5(5) . . . . ?
K1 O2 C36 C35 30.5(7) . . . . ?
K1 O2 C37 C38 -58.8(6) . . . . ?
K1 O3 C40 C39 -51.4(6) . . . . ?
K1 O3 C41 C42 51.9(5) . . . . ?
K1 O4 C42 C41 45.5(5) . . . . ?
K1 O4 C43 C44 -60.3(4) . . . . ?
K1 O5 C46 C45 -56.1(4) . . . . ?
K1 O5 C47 C48 51.6(4) . . . . ?
K1 O6 C48 C47 49.6(5) . . . . ?
K1 O6 C49 C50 -56.2(6) . . . . ?
K1 N4 C33 C34 -47.3(4) . . . . ?
K1 N4 C44 C43 -37.0(4) . . . . ?
K1 N4 C45 C46 -40.4(6) . . . . ?
K1 N5 C38 C37 -38.3(7) . . . . ?
K1 N5 C39 C40 -46.4(7) . . . . ?
K1 N5 C50 C49 -41.8(6) . . . . ?
O1 C35 C36 O2 -52.5(7) . . . . ?
O2 C37 C38 N5 64.5(7) . . . . ?
O3 C41 C42 O4 -65.4(5) . . . . ?
O4 C43 C44 N4 67.3(5) . . . . ?
O5 C47 C48 O6 -69.0(5) . . . . ?
O6 C49 C50 N5 66.9(8) . . . . ?
N4 C33 C34 O1 59.4(5) . . . . ?
N4 C45 C46 O5 66.1(6) . . . . ?
N5 C39 C40 O3 67.4(8) . . . . ?
C33 N4 C44 C43 -155.5(4) . . . . ?
C33 N4 C45 C46 77.7(5) . . . . ?
C34 O1 C35 C36 -164.6(4) . . . . ?
C35 O1 C34 C33 176.5(4) . . . . ?
C36 O2 C37 C38 154.3(5) . . . . ?
C37 O2 C36 C35 176.6(5) . . . . ?
C38 N5 C39 C40 73.2(7) . . . . ?
C38 N5 C50 C49 -162.1(5) . . . . ?
C39 N5 C38 C37 -156.5(6) . . . . ?
C39 N5 C50 C49 75.8(7) . . . . ?
C40 O3 C41 C42 -170.5(5) . . . . ?
C41 O3 C40 C39 172.8(5) . . . . ?
C42 O4 C43 C44 167.1(4) . . . . ?
C43 O4 C42 C41 178.1(4) . . . . ?
C44 N4 C33 C34 71.8(5) . . . . ?
C44 N4 C45 C46 -159.7(5) . . . . ?
C45 N4 C33 C34 -167.0(4) . . . . ?
C45 N4 C44 C43 83.4(5) . . . . ?
C46 O5 C47 C48 -177.9(4) . . . . ?
C47 O5 C46 C45 174.4(4) . . . . ?
C48 O6 C49 C50 170.5(5) . . . . ?
C49 O6 C48 C47 -175.7(5) . . . . ?
C50 N5 C38 C37 81.6(7) . . . . ?
C50 N5 C39 C40 -165.2(6) . . . . ?

_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 1.439
_oxdiff_exptl_absorpt_empirical_full_min 0.738
####################################################################### 
# 
# 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_dkm134
_database_code_depnum_ccdc_archive 'CCDC 2039850'
loop_
_audit_author_name
_audit_author_address
'rosario scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2021-03-26 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_audit_creation_date             2020-05-15
_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         'C30 H64 N5 Si6 U, 2(C9 H18 K0.5 N O3)'
_chemical_formula_sum            'C48 H100 K N7 O6 Si6 U'
_chemical_formula_weight         1317.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H100 N7 O6 Si6 K1 U1'
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                   22.6297(5)
_cell_length_b                   23.9733(5)
_cell_length_c                   23.9063(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.9909(18)
_cell_angle_gamma                90
_cell_volume                     12951.7(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8692
_cell_measurement_temperature    139.9(6)
_cell_measurement_theta_max      72.5570
_cell_measurement_theta_min      6.5910
_shelx_estimated_absorpt_T_max   0.691
_shelx_estimated_absorpt_T_min   0.357
_exptl_absorpt_coefficient_mu    9.057
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (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            'lustrous intense black'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5440
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 -10 -5 0.0526
0 16 -1 0.0179
3 12 -10 0.0265
13 -7 0 0.0486
1 -13 9 0.0286
8 2 12 0.0399
8 8 10 0.0323
-2 8 13 0.0361
3 -11 -11 0.0313
3 -15 -3 0.0256
-4 -15 2 0.0232

_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.044
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
-10.4604 -9.5758 -4.6408 -0.4191 -0.8794 0.2258
0.0623 15.5346 -0.6774 -0.0946 0.5137 -0.8528
3.1139 11.9439 -9.5489 0.3610 0.0682 -0.9301
13.1657 -6.8989 -0.3092 0.8420 0.1560 0.5165
1.1337 -12.8852 8.5526 -0.0740 -0.0149 0.9971
8.0364 1.6722 12.4374 0.1174 0.8921 0.4363
7.8751 8.0120 9.9301 0.1299 0.9915 0.0091
-2.3176 7.8678 13.2652 -0.5669 0.8238 0.0091
2.7922 -10.7858 -10.9120 0.5514 -0.8008 0.2337
3.2170 -14.9261 -2.8760 0.3837 -0.5562 0.7372
-4.1343 -14.7986 2.1154 -0.1927 -0.5480 0.8140

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.788
_diffrn_reflns_theta_min         3.688
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -15.00   1.00   13.50    --  -40.91 -46.00  27.00   99
  2  ω    -48.00  30.00   1.00   13.50    --  -40.91  46.00 177.00   78
  3  ω      9.00  48.00   1.00   13.50    --   40.91 -46.00  27.00   39
  4  ω     61.00 108.00   1.00   13.50    --   40.91  46.00 177.00   47
  5  ω     92.00 178.00   1.00   55.00    --  105.15  46.00 177.00   86
  6  ω     34.00 119.00   1.00   55.00    --  105.15 -46.00  27.00   85
  7  ω     28.00  95.00   1.00   13.50    --   40.91-125.00-120.00   67
  8  ω     55.00  97.00   1.00   13.50    --   40.91-125.00 -30.00   42
  9  ω     23.00 106.00   1.00   55.00    --  105.15 -94.00  30.00   83
 10  ω    151.00 177.00   1.00   55.00    --  105.15  77.00-180.00   26
 11  ω    124.00 173.00   1.00   55.00    --  105.15 111.00  60.00   49
 12  ω    104.00 165.00   1.00   55.00    --  105.15  77.00 120.00   61
 13  ω    104.00 164.00   1.00   55.00    --  105.15  77.00  90.00   60
 14  ω     47.00  99.00   1.00   55.00    --  105.15-111.00   0.00   52
;
_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      0.0593439000
_diffrn_orient_matrix_UB_12      -0.0075441000
_diffrn_orient_matrix_UB_13      -0.0278904000
_diffrn_orient_matrix_UB_21      0.0312782000
_diffrn_orient_matrix_UB_22      0.0349815000
_diffrn_orient_matrix_UB_23      0.0468162000
_diffrn_orient_matrix_UB_31      0.0120368000
_diffrn_orient_matrix_UB_32      -0.0534391000
_diffrn_orient_matrix_UB_33      0.0344833000
_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                7639
_reflns_number_total             14444
_reflns_special_details          
;
 _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 1.171.40.79a (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    'SHELXS (Sheldrick, 2008)'
_refine_diff_density_max         4.553
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         14444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0502
_refine_ls_restrained_S_all      0.841
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0859P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1328
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.808(2)
 0.192(2)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.58396(2) 0.50004(2) 0.24153(2) 0.03824(9) Uani 1 1 d . . . . .
Si1 Si 0.71668(11) 0.56894(11) 0.21582(10) 0.0510(6) Uani 1 1 d . . . . .
Si2 Si 0.72890(11) 0.47891(12) 0.30243(10) 0.0513(6) Uani 1 1 d . . . . .
Si3 Si 0.56536(13) 0.35316(11) 0.24517(11) 0.0558(6) Uani 1 1 d . . . . .
Si4 Si 0.47965(11) 0.41888(12) 0.30759(11) 0.0576(6) Uani 1 1 d . . . . .
Si5 Si 0.47255(11) 0.54060(12) 0.14382(10) 0.0503(6) Uani 1 1 d . . . . .
Si6 Si 0.50835(12) 0.63089(11) 0.22216(11) 0.0552(6) Uani 1 1 d . . . . .
N1 N 0.5958(3) 0.4689(3) 0.1686(3) 0.0547(18) Uani 1 1 d . . . . .
N2 N 0.5739(3) 0.5315(3) 0.3150(3) 0.0536(18) Uani 1 1 d . . . . .
N3 N 0.6870(3) 0.5169(3) 0.2533(3) 0.0490(18) Uani 1 1 d . . . . .
N4 N 0.5396(3) 0.4174(3) 0.2664(3) 0.0457(16) Uani 1 1 d . . . . .
N5 N 0.5149(3) 0.5634(3) 0.2015(3) 0.0474(16) Uani 1 1 d . . . . .
C1 C 0.6218(4) 0.4457(3) 0.1231(3) 0.0428(18) Uani 1 1 d . . . . .
C2 C 0.6835(4) 0.4407(4) 0.1218(4) 0.052(2) Uani 1 1 d . . . . .
H2 H 0.707754 0.455766 0.151684 0.063 Uiso 1 1 calc R U . . .
C3 C 0.7099(4) 0.4142(4) 0.0777(4) 0.058(2) Uani 1 1 d . . . . .
H3 H 0.751775 0.410893 0.077676 0.070 Uiso 1 1 calc R U . . .
C4 C 0.6746(5) 0.3928(4) 0.0340(4) 0.061(2) Uani 1 1 d . . . . .
H4 H 0.692400 0.374470 0.003892 0.074 Uiso 1 1 calc R U . . .
C5 C 0.6146(4) 0.3975(4) 0.0334(4) 0.056(2) Uani 1 1 d . . . . .
H5 H 0.590892 0.382663 0.003038 0.068 Uiso 1 1 calc R U . . .
C6 C 0.5883(4) 0.4239(4) 0.0771(4) 0.054(2) Uani 1 1 d . . . . .
H6 H 0.546397 0.427467 0.075929 0.065 Uiso 1 1 calc R U . . .
C7 C 0.5823(4) 0.5515(4) 0.3678(4) 0.050(2) Uani 1 1 d . . . . .
C8 C 0.5403(4) 0.5442(5) 0.4094(4) 0.063(3) Uani 1 1 d . . . . .
H8 H 0.504494 0.524750 0.400102 0.076 Uiso 1 1 calc R U . . .
C9 C 0.5505(5) 0.5647(5) 0.4630(4) 0.075(3) Uani 1 1 d . . . . .
H9 H 0.521757 0.558789 0.490031 0.091 Uiso 1 1 calc R U . . .
C10 C 0.6011(5) 0.5934(4) 0.4780(4) 0.068(3) Uani 1 1 d . . . . .
H10 H 0.607809 0.607012 0.515058 0.082 Uiso 1 1 calc R U . . .
C11 C 0.6422(5) 0.6021(5) 0.4383(4) 0.066(3) Uani 1 1 d . . . . .
H11 H 0.677245 0.622433 0.448045 0.079 Uiso 1 1 calc R U . . .
C12 C 0.6329(4) 0.5815(4) 0.3841(4) 0.060(2) Uani 1 1 d . . . . .
H12 H 0.661941 0.588076 0.357527 0.072 Uiso 1 1 calc R U . . .
C13 C 0.6645(4) 0.5905(4) 0.1574(4) 0.058(2) Uani 1 1 d . . . . .
H13A H 0.660910 0.560561 0.129565 0.087 Uiso 1 1 calc R U . . .
H13B H 0.679346 0.624329 0.139869 0.087 Uiso 1 1 calc R U . . .
H13C H 0.625576 0.598115 0.171949 0.087 Uiso 1 1 calc R U . . .
C14 C 0.7876(4) 0.5510(5) 0.1832(4) 0.066(3) Uani 1 1 d . . . . .
H14A H 0.817760 0.541731 0.212652 0.099 Uiso 1 1 calc R U . . .
H14B H 0.800904 0.582937 0.161621 0.099 Uiso 1 1 calc R U . . .
H14C H 0.781271 0.518843 0.158270 0.099 Uiso 1 1 calc R U . . .
C15 C 0.7344(5) 0.6329(4) 0.2591(4) 0.064(3) Uani 1 1 d . . . . .
H15A H 0.698592 0.645902 0.276370 0.096 Uiso 1 1 calc R U . . .
H15B H 0.749288 0.662278 0.235114 0.096 Uiso 1 1 calc R U . . .
H15C H 0.764709 0.623698 0.288525 0.096 Uiso 1 1 calc R U . . .
C16 C 0.7822(4) 0.4297(4) 0.2694(4) 0.063(3) Uani 1 1 d . . . . .
H16A H 0.760184 0.404759 0.243359 0.095 Uiso 1 1 calc R U . . .
H16B H 0.803048 0.407627 0.298685 0.095 Uiso 1 1 calc R U . . .
H16C H 0.810863 0.451281 0.248969 0.095 Uiso 1 1 calc R U . . .
C17 C 0.6807(4) 0.4361(4) 0.3470(4) 0.054(2) Uani 1 1 d . . . . .
H17A H 0.656374 0.460893 0.368941 0.081 Uiso 1 1 calc R U . . .
H17B H 0.705550 0.412872 0.372459 0.081 Uiso 1 1 calc R U . . .
H17C H 0.655016 0.412225 0.323073 0.081 Uiso 1 1 calc R U . . .
C18 C 0.7772(4) 0.5230(5) 0.3519(4) 0.062(3) Uani 1 1 d . . . . .
H18A H 0.805220 0.544322 0.330441 0.092 Uiso 1 1 calc R U . . .
H18B H 0.799078 0.498731 0.378690 0.092 Uiso 1 1 calc R U . . .
H18C H 0.752363 0.548723 0.372160 0.092 Uiso 1 1 calc R U . . .
C19 C 0.6451(5) 0.3544(5) 0.2226(5) 0.074(3) Uani 1 1 d . . . . .
H19A H 0.646066 0.342826 0.183361 0.110 Uiso 1 1 calc R U . . .
H19B H 0.669240 0.328790 0.246176 0.110 Uiso 1 1 calc R U . . .
H19C H 0.661027 0.392320 0.226737 0.110 Uiso 1 1 calc R U . . .
C20 C 0.5685(5) 0.3029(5) 0.3052(5) 0.077(3) Uani 1 1 d . . . . .
H20A H 0.596785 0.316452 0.334548 0.116 Uiso 1 1 calc R U . . .
H20B H 0.581241 0.266273 0.292148 0.116 Uiso 1 1 calc R U . . .
H20C H 0.529227 0.299684 0.320256 0.116 Uiso 1 1 calc R U . . .
C21 C 0.5210(5) 0.3221(5) 0.1851(5) 0.073(3) Uani 1 1 d . . . . .
H21A H 0.478904 0.323280 0.192754 0.109 Uiso 1 1 calc R U . . .
H21B H 0.533167 0.283302 0.179851 0.109 Uiso 1 1 calc R U . . .
H21C H 0.527614 0.343427 0.150970 0.109 Uiso 1 1 calc R U . . .
C22 C 0.5006(5) 0.4043(5) 0.3830(5) 0.077(3) Uani 1 1 d . . . . .
H22A H 0.508642 0.364419 0.387933 0.116 Uiso 1 1 calc R U . . .
H22B H 0.468058 0.415270 0.406151 0.116 Uiso 1 1 calc R U . . .
H22C H 0.536151 0.425719 0.394410 0.116 Uiso 1 1 calc R U . . .
C23 C 0.4209(5) 0.3650(5) 0.2874(5) 0.080(3) Uani 1 1 d . . . . .
H23A H 0.407102 0.370646 0.248240 0.120 Uiso 1 1 calc R U . . .
H23B H 0.387507 0.369090 0.311582 0.120 Uiso 1 1 calc R U . . .
H23C H 0.437696 0.327517 0.291873 0.120 Uiso 1 1 calc R U . . .
C24 C 0.4370(4) 0.4850(5) 0.3029(4) 0.071(3) Uani 1 1 d . . . . .
H24A H 0.464437 0.516564 0.302353 0.107 Uiso 1 1 calc R U . . .
H24B H 0.412599 0.488210 0.335450 0.107 Uiso 1 1 calc R U . . .
H24C H 0.411481 0.485001 0.268538 0.107 Uiso 1 1 calc R U . . .
C25 C 0.4521(5) 0.4646(4) 0.1482(4) 0.057(2) Uani 1 1 d . . . . .
H25A H 0.487752 0.442509 0.157063 0.086 Uiso 1 1 calc R U . . .
H25B H 0.433767 0.452449 0.112237 0.086 Uiso 1 1 calc R U . . .
H25C H 0.424044 0.459464 0.177690 0.086 Uiso 1 1 calc R U . . .
C26 C 0.5093(4) 0.5525(4) 0.0766(4) 0.057(2) Uani 1 1 d . . . . .
H26A H 0.517045 0.592390 0.072034 0.086 Uiso 1 1 calc R U . . .
H26B H 0.483364 0.539310 0.045188 0.086 Uiso 1 1 calc R U . . .
H26C H 0.546771 0.531913 0.077189 0.086 Uiso 1 1 calc R U . . .
C27 C 0.3982(4) 0.5768(5) 0.1338(5) 0.068(3) Uani 1 1 d . . . . .
H27A H 0.377737 0.575456 0.168920 0.102 Uiso 1 1 calc R U . . .
H27B H 0.374214 0.557809 0.104271 0.102 Uiso 1 1 calc R U . . .
H27C H 0.404270 0.615726 0.123099 0.102 Uiso 1 1 calc R U . . .
C28 C 0.4388(6) 0.6452(5) 0.2594(5) 0.082(3) Uani 1 1 d . . . . .
H28A H 0.404335 0.636194 0.234523 0.123 Uiso 1 1 calc R U . . .
H28B H 0.437562 0.684653 0.269828 0.123 Uiso 1 1 calc R U . . .
H28C H 0.438360 0.622082 0.293181 0.123 Uiso 1 1 calc R U . . .
C29 C 0.5692(6) 0.6568(5) 0.2711(6) 0.084(4) Uani 1 1 d . . . . .
H29A H 0.570764 0.634217 0.305372 0.126 Uiso 1 1 calc R U . . .
H29B H 0.561840 0.695838 0.280606 0.126 Uiso 1 1 calc R U . . .
H29C H 0.607032 0.653836 0.253138 0.126 Uiso 1 1 calc R U . . .
C30 C 0.5135(5) 0.6793(5) 0.1598(5) 0.071(3) Uani 1 1 d . . . . .
H30A H 0.548506 0.669661 0.139359 0.106 Uiso 1 1 calc R U . . .
H30B H 0.516731 0.717919 0.172961 0.106 Uiso 1 1 calc R U . . .
H30C H 0.477941 0.675192 0.134978 0.106 Uiso 1 1 calc R U . . .
K1 K 0.750000 0.32493(12) 0.500000 0.0584(7) Uani 1 2 d S T P . .
O1 O 0.7262(4) 0.2630(3) 0.5978(3) 0.081(2) Uani 1 1 d . . . . .
O2 O 0.6557(3) 0.2756(3) 0.4364(3) 0.071(2) Uani 1 1 d . . . . .
O3 O 0.6970(3) 0.4270(3) 0.5280(3) 0.0653(17) Uani 1 1 d . . . . .
N6 N 0.6267(4) 0.3247(4) 0.5446(4) 0.074(3) Uani 1 1 d . . . . .
C31 C 0.7761(6) 0.2499(5) 0.6337(5) 0.087(4) Uani 1 1 d . . . . .
H31A H 0.765946 0.219929 0.660014 0.104 Uiso 1 1 calc R U . . .
H31B H 0.788507 0.283199 0.655922 0.104 Uiso 1 1 calc R U . . .
C32 C 0.6770(6) 0.2813(6) 0.6286(6) 0.097(4) Uani 1 1 d . . . . .
H32A H 0.685454 0.318517 0.644988 0.116 Uiso 1 1 calc R U . . .
H32B H 0.670468 0.254890 0.659543 0.116 Uiso 1 1 calc R U . . .
C33 C 0.6226(6) 0.2840(6) 0.5897(5) 0.089(4) Uani 1 1 d . . . . .
H33A H 0.615351 0.246658 0.572978 0.107 Uiso 1 1 calc R U . . .
H33B H 0.588131 0.293450 0.611728 0.107 Uiso 1 1 calc R U . . .
C34 C 0.5860(6) 0.3115(6) 0.4974(6) 0.089(4) Uani 1 1 d . . . . .
H34A H 0.582329 0.344667 0.472846 0.107 Uiso 1 1 calc R U . . .
H34B H 0.546563 0.304113 0.511845 0.107 Uiso 1 1 calc R U . . .
C35 C 0.6025(6) 0.2640(6) 0.4637(6) 0.092(4) Uani 1 1 d . . . . .
H35A H 0.608355 0.230744 0.487904 0.111 Uiso 1 1 calc R U . . .
H35B H 0.570301 0.255727 0.435283 0.111 Uiso 1 1 calc R U . . .
C36 C 0.6735(6) 0.2309(4) 0.4018(5) 0.082(4) Uani 1 1 d . . . . .
H36A H 0.639578 0.218475 0.377109 0.099 Uiso 1 1 calc R U . . .
H36B H 0.686836 0.198912 0.425477 0.099 Uiso 1 1 calc R U . . .
C37 C 0.6146(5) 0.3813(6) 0.5659(5) 0.086(4) Uani 1 1 d . . . . .
H37A H 0.634183 0.385299 0.603718 0.103 Uiso 1 1 calc R U . . .
H37B H 0.571474 0.385263 0.569737 0.103 Uiso 1 1 calc R U . . .
C38 C 0.6352(6) 0.4277(5) 0.5295(5) 0.087(4) Uani 1 1 d . . . . .
H38A H 0.617317 0.423274 0.491107 0.104 Uiso 1 1 calc R U . . .
H38B H 0.622166 0.463929 0.544390 0.104 Uiso 1 1 calc R U . . .
C39 C 0.7170(6) 0.4737(5) 0.4991(4) 0.082(4) Uani 1 1 d . . . . .
H39A H 0.702630 0.508263 0.516635 0.098 Uiso 1 1 calc R U . . .
H39B H 0.701157 0.472678 0.459752 0.098 Uiso 1 1 calc R U . . .
K2 K 0.750000 0.69447(11) 0.000000 0.0504(6) Uani 1 2 d S T P . .
O4 O 0.7995(4) 0.7505(3) 0.0963(3) 0.079(2) Uani 1 1 d . . . . .
O5 O 0.6749(4) 0.7385(3) 0.0792(3) 0.078(2) Uani 1 1 d . . . . .
O6 O 0.6899(3) 0.5938(3) -0.0196(3) 0.0619(17) Uani 1 1 d . . . . .
N7 N 0.6167(4) 0.6960(4) -0.0241(4) 0.075(3) Uani 1 1 d . . . . .
C40 C 0.8582(6) 0.7351(6) 0.1155(6) 0.093(4) Uani 1 1 d . . . . .
H40A H 0.858337 0.696647 0.130582 0.112 Uiso 1 1 calc R U . . .
H40B H 0.872777 0.760641 0.145702 0.112 Uiso 1 1 calc R U . . .
C41 C 0.7603(7) 0.7502(6) 0.1387(5) 0.103(5) Uani 1 1 d . . . . .
H41A H 0.777038 0.772401 0.170637 0.123 Uiso 1 1 calc R U . . .
H41B H 0.755100 0.711433 0.151780 0.123 Uiso 1 1 calc R U . . .
C42 C 0.7020(7) 0.7734(6) 0.1202(6) 0.100(5) Uani 1 1 d . . . . .
H42A H 0.676585 0.776299 0.152534 0.120 Uiso 1 1 calc R U . . .
H42B H 0.707046 0.811251 0.104593 0.120 Uiso 1 1 calc R U . . .
C43 C 0.6181(5) 0.7572(6) 0.0596(7) 0.092(4) Uani 1 1 d . . . . .
H43A H 0.622024 0.790152 0.035087 0.111 Uiso 1 1 calc R U . . .
H43B H 0.594821 0.768308 0.091746 0.111 Uiso 1 1 calc R U . . .
C44 C 0.5871(6) 0.7112(6) 0.0276(6) 0.093(4) Uani 1 1 d . . . . .
H44A H 0.585289 0.677914 0.052005 0.111 Uiso 1 1 calc R U . . .
H44B H 0.545932 0.722903 0.017513 0.111 Uiso 1 1 calc R U . . .
C45 C 0.5987(5) 0.6417(5) -0.0423(5) 0.077(3) Uani 1 1 d . . . . .
H45A H 0.606253 0.637969 -0.082529 0.093 Uiso 1 1 calc R U . . .
H45B H 0.555505 0.638185 -0.038518 0.093 Uiso 1 1 calc R U . . .
C46 C 0.6293(5) 0.5945(5) -0.0107(5) 0.072(3) Uani 1 1 d . . . . .
H46A H 0.623482 0.598622 0.029829 0.086 Uiso 1 1 calc R U . . .
H46B H 0.611446 0.558562 -0.023186 0.086 Uiso 1 1 calc R U . . .
C47 C 0.7179(5) 0.5468(4) 0.0048(5) 0.076(3) Uani 1 1 d . . . . .
H47A H 0.699669 0.512546 -0.011375 0.091 Uiso 1 1 calc R U . . .
H47B H 0.712232 0.546740 0.045581 0.091 Uiso 1 1 calc R U . . .
C48 C 0.6021(6) 0.7386(6) -0.0663(7) 0.097(5) Uani 1 1 d . . . . .
H48A H 0.606134 0.775964 -0.048851 0.117 Uiso 1 1 calc R U . . .
H48B H 0.560317 0.733963 -0.080010 0.117 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 N1 1.929(8) . ?
U1 N2 1.935(8) . ?
U1 N3 2.370(7) . ?
U1 N4 2.314(7) . ?
U1 N5 2.347(7) . ?
Si1 N3 1.696(8) . ?
Si1 C13 1.855(9) . ?
Si1 C14 1.871(10) . ?
Si1 C15 1.881(10) . ?
Si2 N3 1.728(7) . ?
Si2 C16 1.888(9) . ?
Si2 C17 1.870(9) . ?
Si2 C18 1.891(9) . ?
Si3 N4 1.732(7) . ?
Si3 C19 1.911(11) . ?
Si3 C20 1.872(11) . ?
Si3 C21 1.865(11) . ?
Si4 N4 1.717(8) . ?
Si4 C22 1.873(11) . ?
Si4 C23 1.898(11) . ?
Si4 C24 1.855(11) . ?
Si5 N5 1.727(7) . ?
Si5 C25 1.883(10) . ?
Si5 C26 1.870(10) . ?
Si5 C27 1.897(9) . ?
Si6 N5 1.700(8) . ?
Si6 C28 1.879(11) . ?
Si6 C29 1.867(11) . ?
Si6 C30 1.896(11) . ?
N1 C1 1.380(11) . ?
N2 C7 1.356(11) . ?
C1 C2 1.402(12) . ?
C1 C6 1.405(12) . ?
C2 C3 1.393(12) . ?
C3 C4 1.381(13) . ?
C4 C5 1.361(13) . ?
C5 C6 1.383(12) . ?
C7 C8 1.422(13) . ?
C7 C12 1.390(13) . ?
C8 C9 1.382(14) . ?
C9 C10 1.367(15) . ?
C10 C11 1.379(15) . ?
C11 C12 1.392(13) . ?
K1 O1 2.845(8) . ?
K1 O1 2.845(8) 2_656 ?
K1 O2 2.816(7) 2_656 ?
K1 O2 2.816(7) . ?
K1 O3 2.822(7) . ?
K1 O3 2.822(7) 2_656 ?
K1 N6 3.038(9) 2_656 ?
K1 N6 3.038(9) . ?
O1 C31 1.419(13) . ?
O1 C32 1.433(17) . ?
O2 C35 1.424(15) . ?
O2 C36 1.425(14) . ?
O3 C38 1.401(14) . ?
O3 C39 1.403(13) . ?
N6 C33 1.461(14) . ?
N6 C34 1.453(14) . ?
N6 C37 1.480(16) . ?
C31 C36 1.526(19) 2_656 ?
C32 C33 1.506(17) . ?
C34 C35 1.456(19) . ?
C37 C38 1.500(18) . ?
C39 C39 1.49(3) 2_656 ?
K2 O4 2.844(7) 2_655 ?
K2 O4 2.844(7) . ?
K2 O5 2.814(8) . ?
K2 O5 2.814(8) 2_655 ?
K2 O6 2.798(7) . ?
K2 O6 2.798(7) 2_655 ?
K2 N7 3.041(9) . ?
K2 N7 3.041(9) 2_655 ?
O4 C40 1.432(14) . ?
O4 C41 1.382(17) . ?
O5 C42 1.404(14) . ?
O5 C43 1.418(14) . ?
O6 C46 1.398(12) . ?
O6 C47 1.405(12) . ?
N7 C44 1.483(16) . ?
N7 C45 1.425(14) . ?
N7 C48 1.461(15) . ?
C40 C48 1.52(2) 2_655 ?
C41 C42 1.478(19) . ?
C43 C44 1.496(17) . ?
C45 C46 1.510(16) . ?
C47 C47 1.48(2) 2_655 ?

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 N2 178.8(3) . . ?
N1 U1 N3 89.5(3) . . ?
N1 U1 N4 89.1(3) . . ?
N1 U1 N5 90.2(3) . . ?
N2 U1 N3 89.3(3) . . ?
N2 U1 N4 91.6(3) . . ?
N2 U1 N5 90.6(3) . . ?
N4 U1 N3 123.6(2) . . ?
N4 U1 N5 111.7(2) . . ?
N5 U1 N3 124.6(2) . . ?
N3 Si1 C13 110.5(4) . . ?
N3 Si1 C14 115.0(4) . . ?
N3 Si1 C15 112.8(4) . . ?
C13 Si1 C14 106.1(5) . . ?
C13 Si1 C15 107.3(5) . . ?
C14 Si1 C15 104.7(5) . . ?
N3 Si2 C16 112.6(4) . . ?
N3 Si2 C17 111.1(4) . . ?
N3 Si2 C18 114.1(4) . . ?
C16 Si2 C18 104.5(5) . . ?
C17 Si2 C16 107.4(5) . . ?
C17 Si2 C18 106.6(4) . . ?
N4 Si3 C19 114.0(4) . . ?
N4 Si3 C20 110.4(5) . . ?
N4 Si3 C21 113.8(4) . . ?
C20 Si3 C19 103.1(5) . . ?
C21 Si3 C19 105.5(6) . . ?
C21 Si3 C20 109.4(5) . . ?
N4 Si4 C22 112.4(4) . . ?
N4 Si4 C23 113.8(5) . . ?
N4 Si4 C24 114.0(4) . . ?
C22 Si4 C23 104.9(6) . . ?
C24 Si4 C22 108.8(5) . . ?
C24 Si4 C23 102.1(5) . . ?
N5 Si5 C25 112.9(4) . . ?
N5 Si5 C26 112.6(4) . . ?
N5 Si5 C27 114.1(4) . . ?
C25 Si5 C27 103.3(5) . . ?
C26 Si5 C25 108.5(4) . . ?
C26 Si5 C27 104.7(5) . . ?
N5 Si6 C28 113.5(5) . . ?
N5 Si6 C29 115.2(5) . . ?
N5 Si6 C30 110.1(4) . . ?
C28 Si6 C30 110.4(5) . . ?
C29 Si6 C28 104.5(6) . . ?
C29 Si6 C30 102.5(6) . . ?
C1 N1 U1 162.5(6) . . ?
C7 N2 U1 165.0(6) . . ?
Si1 N3 U1 118.5(3) . . ?
Si1 N3 Si2 121.9(5) . . ?
Si2 N3 U1 119.5(4) . . ?
Si3 N4 U1 121.9(4) . . ?
Si4 N4 U1 119.7(4) . . ?
Si4 N4 Si3 118.4(4) . . ?
Si5 N5 U1 116.8(4) . . ?
Si6 N5 U1 124.3(4) . . ?
Si6 N5 Si5 118.7(4) . . ?
N1 C1 C2 121.2(7) . . ?
N1 C1 C6 122.1(8) . . ?
C2 C1 C6 116.7(8) . . ?
C3 C2 C1 121.6(8) . . ?
C4 C3 C2 119.2(9) . . ?
C5 C4 C3 120.9(9) . . ?
C4 C5 C6 120.0(9) . . ?
C5 C6 C1 121.6(8) . . ?
N2 C7 C8 122.7(9) . . ?
N2 C7 C12 121.2(8) . . ?
C12 C7 C8 116.1(8) . . ?
C9 C8 C7 121.3(10) . . ?
C10 C9 C8 121.2(10) . . ?
C9 C10 C11 118.9(9) . . ?
C10 C11 C12 120.8(10) . . ?
C7 C12 C11 121.7(10) . . ?
O1 K1 O1 117.1(4) 2_656 . ?
O1 K1 N6 120.3(3) . 2_656 ?
O1 K1 N6 59.6(3) 2_656 2_656 ?
O1 K1 N6 120.3(3) 2_656 . ?
O1 K1 N6 59.6(3) . . ?
O2 K1 O1 60.5(3) 2_656 . ?
O2 K1 O1 93.1(2) . . ?
O2 K1 O1 93.1(2) 2_656 2_656 ?
O2 K1 O1 60.5(3) . 2_656 ?
O2 K1 O2 130.3(3) . 2_656 ?
O2 K1 O3 123.8(2) 2_656 . ?
O2 K1 O3 100.0(2) 2_656 2_656 ?
O2 K1 O3 123.8(2) . 2_656 ?
O2 K1 O3 100.0(2) . . ?
O2 K1 N6 119.6(2) 2_656 . ?
O2 K1 N6 60.3(3) . . ?
O2 K1 N6 60.3(2) 2_656 2_656 ?
O2 K1 N6 119.6(2) . 2_656 ?
O3 K1 O1 138.5(2) . 2_656 ?
O3 K1 O1 99.0(2) 2_656 2_656 ?
O3 K1 O1 99.0(2) . . ?
O3 K1 O1 138.5(2) 2_656 . ?
O3 K1 O3 59.7(3) . 2_656 ?
O3 K1 N6 60.6(3) 2_656 2_656 ?
O3 K1 N6 119.6(3) . 2_656 ?
O3 K1 N6 119.6(3) 2_656 . ?
O3 K1 N6 60.6(3) . . ?
N6 K1 N6 179.8(4) 2_656 . ?
C31 O1 K1 115.7(7) . . ?
C31 O1 C32 111.8(10) . . ?
C32 O1 K1 116.7(7) . . ?
C35 O2 K1 118.0(7) . . ?
C35 O2 C36 113.0(9) . . ?
C36 O2 K1 113.5(7) . . ?
C38 O3 K1 116.9(7) . . ?
C38 O3 C39 110.6(8) . . ?
C39 O3 K1 115.1(6) . . ?
C33 N6 K1 110.8(7) . . ?
C33 N6 C37 109.8(11) . . ?
C34 N6 K1 106.5(7) . . ?
C34 N6 C33 111.3(10) . . ?
C34 N6 C37 110.2(10) . . ?
C37 N6 K1 108.0(7) . . ?
O1 C31 C36 108.9(10) . 2_656 ?
O1 C32 C33 109.1(11) . . ?
N6 C33 C32 113.7(10) . . ?
N6 C34 C35 115.5(11) . . ?
O2 C35 C34 110.4(10) . . ?
O2 C36 C31 109.9(9) . 2_656 ?
N6 C37 C38 114.2(11) . . ?
O3 C38 C37 110.3(9) . . ?
O3 C39 C39 109.5(7) . 2_656 ?
O4 K2 O4 123.6(4) . 2_655 ?
O4 K2 N7 119.5(3) 2_655 2_655 ?
O4 K2 N7 59.8(3) . 2_655 ?
O4 K2 N7 59.8(3) 2_655 . ?
O4 K2 N7 119.5(3) . . ?
O5 K2 O4 98.1(3) . 2_655 ?
O5 K2 O4 60.3(2) . . ?
O5 K2 O4 60.3(2) 2_655 2_655 ?
O5 K2 O4 98.1(3) 2_655 . ?
O5 K2 O5 135.9(3) 2_655 . ?
O5 K2 N7 119.7(3) . 2_655 ?
O5 K2 N7 119.7(3) 2_655 . ?
O5 K2 N7 59.7(3) 2_655 2_655 ?
O5 K2 N7 59.7(3) . . ?
O6 K2 O4 135.3(2) 2_655 2_655 ?
O6 K2 O4 96.0(2) 2_655 . ?
O6 K2 O4 135.3(2) . . ?
O6 K2 O4 96.0(2) . 2_655 ?
O6 K2 O5 121.1(2) 2_655 . ?
O6 K2 O5 97.5(2) . . ?
O6 K2 O5 121.1(2) . 2_655 ?
O6 K2 O5 97.5(2) 2_655 2_655 ?
O6 K2 O6 60.8(3) . 2_655 ?
O6 K2 N7 120.7(2) 2_655 . ?
O6 K2 N7 120.7(2) . 2_655 ?
O6 K2 N7 60.6(2) . . ?
O6 K2 N7 60.6(2) 2_655 2_655 ?
N7 K2 N7 178.6(4) . 2_655 ?
C40 O4 K2 117.2(6) . . ?
C41 O4 K2 110.5(7) . . ?
C41 O4 C40 112.5(11) . . ?
C42 O5 K2 115.9(7) . . ?
C42 O5 C43 113.3(10) . . ?
C43 O5 K2 117.8(7) . . ?
C46 O6 K2 115.9(6) . . ?
C46 O6 C47 111.8(7) . . ?
C47 O6 K2 114.6(6) . . ?
C44 N7 K2 109.4(7) . . ?
C45 N7 K2 108.2(7) . . ?
C45 N7 C44 110.1(10) . . ?
C45 N7 C48 112.1(11) . . ?
C48 N7 K2 109.1(7) . . ?
C48 N7 C44 107.9(11) . . ?
O4 C40 C48 108.3(11) . 2_655 ?
O4 C41 C42 112.1(12) . . ?
O5 C42 C41 109.6(11) . . ?
O5 C43 C44 109.2(10) . . ?
N7 C44 C43 112.7(10) . . ?
N7 C45 C46 114.6(10) . . ?
O6 C46 C45 111.1(9) . . ?
O6 C47 C47 111.2(7) . 2_655 ?
N7 C48 C40 111.9(11) . 2_655 ?

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 N1 C1 C2 -9(3) . . . . ?
U1 N1 C1 C6 168.7(17) . . . . ?
U1 N2 C7 C8 -145(2) . . . . ?
U1 N2 C7 C12 36(3) . . . . ?
N1 C1 C2 C3 175.9(9) . . . . ?
N1 C1 C6 C5 -175.7(9) . . . . ?
N2 C7 C8 C9 179.4(10) . . . . ?
N2 C7 C12 C11 -179.7(9) . . . . ?
C1 C2 C3 C4 0.6(15) . . . . ?
C2 C1 C6 C5 1.8(13) . . . . ?
C2 C3 C4 C5 0.3(16) . . . . ?
C3 C4 C5 C6 -0.2(16) . . . . ?
C4 C5 C6 C1 -0.9(15) . . . . ?
C6 C1 C2 C3 -1.6(13) . . . . ?
C7 C8 C9 C10 0.7(18) . . . . ?
C8 C7 C12 C11 1.2(14) . . . . ?
C8 C9 C10 C11 0.6(18) . . . . ?
C9 C10 C11 C12 -0.9(17) . . . . ?
C10 C11 C12 C7 0.0(16) . . . . ?
C12 C7 C8 C9 -1.5(15) . . . . ?
C13 Si1 N3 U1 -15.7(5) . . . . ?
C13 Si1 N3 Si2 168.1(5) . . . . ?
C14 Si1 N3 U1 -135.7(4) . . . . ?
C14 Si1 N3 Si2 48.1(6) . . . . ?
C15 Si1 N3 U1 104.3(5) . . . . ?
C15 Si1 N3 Si2 -71.9(6) . . . . ?
C16 Si2 N3 U1 111.9(5) . . . . ?
C16 Si2 N3 Si1 -71.9(6) . . . . ?
C17 Si2 N3 U1 -8.7(5) . . . . ?
C17 Si2 N3 Si1 167.5(5) . . . . ?
C18 Si2 N3 U1 -129.2(4) . . . . ?
C18 Si2 N3 Si1 47.0(6) . . . . ?
C19 Si3 N4 U1 19.7(6) . . . . ?
C19 Si3 N4 Si4 -159.7(5) . . . . ?
C20 Si3 N4 U1 135.2(5) . . . . ?
C20 Si3 N4 Si4 -44.2(6) . . . . ?
C21 Si3 N4 U1 -101.4(5) . . . . ?
C21 Si3 N4 Si4 79.2(6) . . . . ?
C22 Si4 N4 U1 -99.1(5) . . . . ?
C22 Si4 N4 Si3 80.3(6) . . . . ?
C23 Si4 N4 U1 141.9(5) . . . . ?
C23 Si4 N4 Si3 -38.7(6) . . . . ?
C24 Si4 N4 U1 25.3(6) . . . . ?
C24 Si4 N4 Si3 -155.3(5) . . . . ?
C25 Si5 N5 U1 36.2(5) . . . . ?
C25 Si5 N5 Si6 -148.8(5) . . . . ?
C26 Si5 N5 U1 -87.2(5) . . . . ?
C26 Si5 N5 Si6 87.9(5) . . . . ?
C27 Si5 N5 U1 153.7(4) . . . . ?
C27 Si5 N5 Si6 -31.3(6) . . . . ?
C28 Si6 N5 U1 -109.7(6) . . . . ?
C28 Si6 N5 Si5 75.6(6) . . . . ?
C29 Si6 N5 U1 10.8(7) . . . . ?
C29 Si6 N5 Si5 -163.9(6) . . . . ?
C30 Si6 N5 U1 126.0(5) . . . . ?
C30 Si6 N5 Si5 -48.7(6) . . . . ?
K1 O1 C31 C36 -43.3(11) . . . 2_656 ?
K1 O1 C32 C33 54.3(12) . . . . ?
K1 O2 C35 C34 45.3(12) . . . . ?
K1 O2 C36 C31 -52.2(10) . . . 2_656 ?
K1 O3 C38 C37 52.1(12) . . . . ?
K1 O3 C39 C39 -47.9(10) . . . 2_656 ?
K1 N6 C33 C32 39.2(15) . . . . ?
K1 N6 C34 C35 47.7(12) . . . . ?
K1 N6 C37 C38 41.4(11) . . . . ?
O1 C32 C33 N6 -63.3(16) . . . . ?
N6 C34 C35 O2 -65.3(14) . . . . ?
N6 C37 C38 O3 -64.8(13) . . . . ?
C31 O1 C32 C33 -169.4(10) . . . . ?
C32 O1 C31 C36 179.9(10) . . . 2_656 ?
C33 N6 C34 C35 -73.3(15) . . . . ?
C33 N6 C37 C38 162.4(10) . . . . ?
C34 N6 C33 C32 157.6(13) . . . . ?
C34 N6 C37 C38 -74.6(12) . . . . ?
C35 O2 C36 C31 170.0(9) . . . 2_656 ?
C36 O2 C35 C34 -178.9(9) . . . . ?
C37 N6 C33 C32 -80.0(14) . . . . ?
C37 N6 C34 C35 164.6(11) . . . . ?
C38 O3 C39 C39 176.9(10) . . . 2_656 ?
C39 O3 C38 C37 -173.6(10) . . . . ?
K2 O4 C40 C48 52.0(12) . . . 2_655 ?
K2 O4 C41 C42 -54.5(13) . . . . ?
K2 O5 C42 C41 -40.3(15) . . . . ?
K2 O5 C43 C44 54.1(13) . . . . ?
K2 O6 C46 C45 52.2(11) . . . . ?
K2 O6 C47 C47 -45.4(12) . . . 2_655 ?
K2 N7 C44 C43 41.6(14) . . . . ?
K2 N7 C45 C46 40.4(12) . . . . ?
K2 N7 C48 C40 47.1(13) . . . 2_655 ?
O4 C41 C42 O5 65.5(16) . . . . ?
O5 C43 C44 N7 -64.7(16) . . . . ?
N7 C45 C46 O6 -64.9(14) . . . . ?
C40 O4 C41 C42 172.3(10) . . . . ?
C41 O4 C40 C48 -178.2(10) . . . 2_655 ?
C42 O5 C43 C44 -166.0(12) . . . . ?
C43 O5 C42 C41 179.0(12) . . . . ?
C44 N7 C45 C46 -79.2(13) . . . . ?
C44 N7 C48 C40 165.9(11) . . . 2_655 ?
C45 N7 C44 C43 160.4(12) . . . . ?
C45 N7 C48 C40 -72.7(14) . . . 2_655 ?
C46 O6 C47 C47 -179.8(11) . . . 2_655 ?
C47 O6 C46 C45 -174.0(9) . . . . ?
C48 N7 C44 C43 -77.0(14) . . . . ?
C48 N7 C45 C46 160.7(11) . . . . ?

_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 2.530
_oxdiff_exptl_absorpt_empirical_full_min 0.618
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
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 0.808(2) 19854 12431 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.192(2) 0 12431 nmt 0.9992 0.0285 -0.0031 -0.0347 0.9988 -0.0191 0.0039
0.0186 1.0001

_twin_special_details            
;
Component 2 rotated by 2.1669° 
 around [0.50 -0.10 -0.86] (reciprocal) or [0.52 -0.11 -0.84] (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_dkm297_sq
_database_code_depnum_ccdc_archive 'CCDC 2039851'
loop_
_audit_author_name
_audit_author_address
'rosario scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2021-03-26 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT342_dkm297_sq           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02267 Ang.  
RESPONSE: The crystals display twinning problems and this certainly
plays a role in the overall quality of the refinement and, particularly, 
in the average C-C bond precision.  
;
# end Validation Reply Form

_audit_creation_date             2020-10-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H64 N5 Si6 U, C18 H36 K N2 O6'
_chemical_formula_sum            'C48 H100 K N7 O6 Si6 U'
_chemical_formula_weight         1317.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H108 N7 O7 Si6 K1 U1'
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                   11.4770(3)
_cell_length_b                   16.6790(8)
_cell_length_c                   19.0067(8)
_cell_angle_alpha                103.478(4)
_cell_angle_beta                 101.463(3)
_cell_angle_gamma                90.908(3)
_cell_volume                     3460.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12607
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6540
_cell_measurement_theta_min      3.9160
_shelx_estimated_absorpt_T_max   0.450
_shelx_estimated_absorpt_T_min   0.202
_exptl_absorpt_coefficient_mu    8.476
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (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 brown'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -4 12 0.0559
0 4 -12 0.0559
7 -2 -2 0.1387
-7 2 2 0.1297
7 0 -7 0.1305
4 0 8 0.1148
0 11 0 0.0932
2 -10 5 0.0860
-2 -9 -3 0.0750
5 -9 0 0.0992
3 -7 -6 0.0950
-4 8 4 0.1214
-5 1 10 0.1103
-7 -4 3 0.1281
6 5 -6 0.1438
-3 -9 6 0.0872
5 8 -3 0.1280
-6 6 3 0.1176
-5 4 9 0.1084
1 -1 12 0.0574
-4 -6 10 0.0850
0 -11 4 0.0519

_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.112
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
-0.1266 -4.2551 11.9753 -0.4342 -0.3702 0.8212
0.1266 4.2551 -11.9753 0.4342 0.3702 -0.8212
7.3665 -1.7526 -2.3456 0.6178 0.5291 0.5816
-7.3449 1.9694 1.7207 -0.5941 -0.5089 -0.6230
6.8473 0.0775 -6.9332 0.7430 0.6356 0.2096
4.1717 0.0825 8.2996 -0.2750 0.3201 0.9066
0.1967 10.5325 -0.2301 -0.6348 0.7428 -0.2128
2.0396 -10.1776 4.6608 0.4691 -0.5497 0.6912
-1.6671 -9.0640 -2.7838 0.6433 -0.7521 -0.1431
4.6307 -8.5456 -0.1546 0.7771 -0.1867 0.6011
2.8332 -7.4508 -6.2714 0.9721 -0.2328 0.0290
-3.8378 8.3432 3.6325 -0.9258 0.2220 -0.3060
-4.6565 1.2017 10.3208 -0.9084 -0.3771 0.1806
-6.9423 -3.7675 3.3682 -0.3107 -0.8779 -0.3644
6.3701 5.1090 -5.6486 0.3301 0.9333 0.1411
-3.1839 -9.4426 6.0889 0.0763 -0.9585 0.2746
4.9183 7.9810 -2.9622 -0.0784 0.9905 0.1129
-6.1836 5.7195 3.0398 -0.8461 -0.1579 -0.5091
-4.5713 3.8048 8.8616 -0.9822 -0.1826 0.0442
0.7753 -1.4906 11.7029 -0.5456 -0.1005 0.8320
-3.5108 -6.4252 10.4824 -0.3833 -0.8036 0.4553
-0.4527 -10.7774 3.7191 0.4351 -0.8011 0.4110

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14136
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.725
_diffrn_reflns_theta_min         3.938
_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 0.972
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -13.00   1.00    4.00    --  -40.91 -57.00 -65.00  100
  2  ω    -55.00  31.00   1.00    4.00    --  -40.91  57.00  76.00   86
  3  ω     -5.00  20.00   1.00    4.00    --   40.91 -57.00 -65.00   25
  4  ω     73.00 100.00   1.00    4.00    --   40.91  57.00  76.00   27
  5  ω     32.00 129.00   1.00   16.00    --  105.15 -57.00 -65.00   97
  6  ω     87.00 177.00   1.00   16.00    --  105.15  57.00  76.00   90
  7  ω    -65.00  33.00   1.00    4.00    --  -40.91  38.00-120.00   98
  8  ω    -80.00  -9.00   1.00    4.00    --  -40.91 125.00  90.00   71
  9  ω     59.00  90.00   1.00    4.00    --   40.91-125.00-120.00   31
 10  ω     34.00 107.00   1.00   16.00    --  105.15-111.00 -90.00   73
 11  ω    109.00 136.00   1.00   16.00    --  105.15 -15.00  60.00   27
 12  ω     31.00 108.00   1.00   16.00    --  105.15-111.00 120.00   77
 13  ω     60.00  90.00   1.00   16.00    --  105.15 -15.00  60.00   30
 14  ω    104.00 132.00   1.00   16.00    --  105.15 111.00 120.00   28
 15  ω     79.00 178.00   1.00   16.00    --  105.15  45.00  30.00   99
 16  ω     79.00 106.00   1.00   16.00    --  105.15 -94.00   0.00   27
 17  ω    104.00 171.00   1.00   16.00    --  105.15  77.00 -60.00   67
 18  ω    104.00 132.00   1.00   16.00    --  105.15 -77.00  90.00   28
 19  ω    105.00 147.00   1.00   16.00    --  105.15  45.00 -90.00   42
 20  ω     24.00  75.00   1.00   16.00    --  105.15 -94.00 -60.00   51
 21  ω     24.00  58.00   1.00   16.00    --  105.15 -15.00  60.00   34
 22  ω     70.00 109.00   1.00   16.00    --  105.15-111.00   0.00   39
 23  ω    117.00 178.00   1.00   16.00    --  105.15  77.00 -30.00   61
 24  ω     29.00 106.00   1.00   16.00    --  105.15 -94.00 150.00   77
;
_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      0.0505621000
_diffrn_orient_matrix_UB_12      -0.0624842000
_diffrn_orient_matrix_UB_13      -0.0579272000
_diffrn_orient_matrix_UB_21      0.0864268000
_diffrn_orient_matrix_UB_22      0.0687856000
_diffrn_orient_matrix_UB_23      -0.0055550000
_diffrn_orient_matrix_UB_31      0.0938757000
_diffrn_orient_matrix_UB_32      -0.0205962000
_diffrn_orient_matrix_UB_33      0.0622523000
_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                13270
_reflns_number_total             14136
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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         5.937
_refine_diff_density_min         -5.122
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         14136
_refine_ls_number_restraints     934
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.1069
_refine_ls_restrained_S_all      1.114
_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)+(0.1197P)²+86.4352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2799
_refine_ls_wR_factor_ref         0.2818
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.658(3)
 0.342(3)
2. 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
3. Restrained distances
 C31-C32 \\sim C34-C33 \\sim C36-C35 \\sim C48-C47 \\sim C46-C45 \\sim C44-C43
\\sim C37-C38 \\sim C40-C39
 \\sim C42-C41
 with sigma of 0.02
 Si6-C28 \\sim Si6-C29 \\sim Si6-C30 \\sim Si5-C26 \\sim Si5-C25 \\sim Si5-C27
\\sim Si3-C20 \\sim Si3-C21
 \\sim Si3-C19 \\sim Si4-C24 \\sim Si4-C22 \\sim Si4-C23 \\sim Si2-C16 \\sim
Si2-C18 \\sim Si2-C17 \\sim Si1-
 C14 \\sim Si1-C15 \\sim Si1-C13
 with sigma of 0.02
 O3-C39 \\sim O3-C38 \\sim O4-C40 \\sim O4-C41 \\sim O2-C34 \\sim O2-C35 \\sim
O6-C47 \\sim O6-C46 \\sim O5-
 C45 \\sim O5-C44 \\sim O1-C32 \\sim O1-C33
 with sigma of 0.02
 N1-C1 \\sim N2-C7
 with sigma of 0.02
 N7-C42 \\sim N7-C36 \\sim N7-C48 \\sim N6-C31 \\sim N6-C37 \\sim N6-C43
 with sigma of 0.02
 Si4-N4 \\sim Si3-N4 \\sim Si1-N3 \\sim Si2-N3 \\sim Si5-N5 \\sim Si6-N5
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C12(H12), C11(H11), C10(H10), C9(H9),
 C8(H8)
5.c Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C7(C12,C11,C10,C9,C8)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_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 0.53361(5) 0.66691(3) 0.74237(3) 0.02999(18) Uani 1 1 d . . . . .
Si1 Si 0.4634(4) 0.8452(3) 0.6721(3) 0.0380(10) Uani 1 1 d D . . . .
Si2 Si 0.2833(4) 0.7065(3) 0.6110(3) 0.0422(11) Uani 1 1 d D . . . .
Si3 Si 0.4364(5) 0.4635(3) 0.6759(3) 0.0512(13) Uani 1 1 d D . . . .
Si4 Si 0.4135(4) 0.5215(3) 0.8332(3) 0.0413(11) Uani 1 1 d D . . . .
Si5 Si 0.7793(4) 0.6613(3) 0.6494(3) 0.0423(11) Uani 1 1 d D . . . .
Si6 Si 0.8179(5) 0.5834(4) 0.7750(3) 0.0499(13) Uani 1 1 d D . . . .
N1 N 0.4799(12) 0.7451(8) 0.8443(8) 0.036(3) Uani 1 1 d D . . . .
N2 N 0.6029(11) 0.7634(8) 0.8461(7) 0.034(3) Uani 1 1 d D . . . .
N3 N 0.4192(10) 0.7430(7) 0.6680(8) 0.036(3) Uani 1 1 d D . . . .
N4 N 0.4568(12) 0.5436(8) 0.7564(6) 0.038(3) Uani 1 1 d D . . . .
N5 N 0.7248(10) 0.6347(9) 0.7195(7) 0.037(3) Uani 1 1 d D . . . .
C1 C 0.4036(8) 0.8092(5) 0.8595(7) 0.034(3) Uani 1 1 d DG . . . .
C6 C 0.4485(7) 0.8900(6) 0.8928(7) 0.038(3) Uani 1 1 d G . . . .
H6 H 0.531978 0.903192 0.903804 0.046 Uiso 1 1 calc R U . . .
C5 C 0.3712(9) 0.9515(5) 0.9100(7) 0.043(4) Uani 1 1 d G . . . .
H5 H 0.401903 1.006674 0.932733 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2491(9) 0.9322(6) 0.8939(7) 0.049(4) Uani 1 1 d G . . . .
H4 H 0.196264 0.974167 0.905633 0.058 Uiso 1 1 calc R U . . .
C3 C 0.2042(6) 0.8514(7) 0.8606(7) 0.045(4) Uani 1 1 d G . . . .
H3 H 0.120698 0.838176 0.849603 0.054 Uiso 1 1 calc R U . . .
C2 C 0.2814(8) 0.7899(5) 0.8434(7) 0.043(4) Uani 1 1 d G . . . .
H2 H 0.250771 0.734692 0.820674 0.051 Uiso 1 1 calc R U . . .
C7 C 0.6834(9) 0.7880(7) 0.9131(5) 0.040(3) Uani 1 1 d DG . . . .
C12 C 0.6516(8) 0.8074(8) 0.9817(6) 0.045(4) Uani 1 1 d G . . . .
H12 H 0.570567 0.800796 0.984866 0.054 Uiso 1 1 calc R U . . .
C11 C 0.7383(12) 0.8365(10) 1.0456(5) 0.061(5) Uani 1 1 d G . . . .
H11 H 0.716617 0.849796 1.092474 0.073 Uiso 1 1 calc R U . . .
C10 C 0.8569(10) 0.8462(10) 1.0410(6) 0.066(5) Uani 1 1 d G . . . .
H10 H 0.916167 0.866107 1.084659 0.080 Uiso 1 1 calc R U . . .
C9 C 0.8887(8) 0.8268(9) 0.9724(8) 0.061(5) Uani 1 1 d G . . . .
H9 H 0.969668 0.833417 0.969237 0.073 Uiso 1 1 calc R U . . .
C8 C 0.8019(10) 0.7977(8) 0.9085(6) 0.045(4) Uani 1 1 d G . . . .
H8 H 0.823619 0.784416 0.861628 0.054 Uiso 1 1 calc R U . . .
C13 C 0.6190(12) 0.8745(11) 0.7252(11) 0.046(4) Uani 1 1 d D . . . .
H13A H 0.628596 0.859627 0.772892 0.069 Uiso 1 1 calc R U . . .
H13B H 0.635448 0.934212 0.733692 0.069 Uiso 1 1 calc R U . . .
H13C H 0.674745 0.845095 0.697064 0.069 Uiso 1 1 calc R U . . .
C14 C 0.3705(13) 0.9247(10) 0.7156(8) 0.039(4) Uani 1 1 d D . . . .
H14A H 0.303916 0.933954 0.677825 0.059 Uiso 1 1 calc R U . . .
H14B H 0.419180 0.976549 0.738297 0.059 Uiso 1 1 calc R U . . .
H14C H 0.339349 0.905562 0.753706 0.059 Uiso 1 1 calc R U . . .
C15 C 0.4609(19) 0.8654(14) 0.5786(9) 0.052(5) Uani 1 1 d D . . . .
H15A H 0.507129 0.824846 0.551512 0.079 Uiso 1 1 calc R U . . .
H15B H 0.495910 0.921162 0.584643 0.079 Uiso 1 1 calc R U . . .
H15C H 0.378439 0.860592 0.550841 0.079 Uiso 1 1 calc R U . . .
C16 C 0.1709(17) 0.7863(14) 0.6038(14) 0.063(6) Uani 1 1 d D . . . .
H16A H 0.167091 0.818181 0.653496 0.095 Uiso 1 1 calc R U . . .
H16B H 0.092528 0.758815 0.578858 0.095 Uiso 1 1 calc R U . . .
H16C H 0.194489 0.823435 0.575300 0.095 Uiso 1 1 calc R U . . .
C17 C 0.2966(19) 0.6569(15) 0.5136(8) 0.059(5) Uani 1 1 d D . . . .
H17A H 0.350792 0.691592 0.497628 0.088 Uiso 1 1 calc R U . . .
H17B H 0.217904 0.650887 0.480728 0.088 Uiso 1 1 calc R U . . .
H17C H 0.328011 0.602318 0.511814 0.088 Uiso 1 1 calc R U . . .
C18 C 0.2121(15) 0.6295(14) 0.6500(13) 0.059(6) Uani 1 1 d D . . . .
H18A H 0.274114 0.604258 0.679580 0.089 Uiso 1 1 calc R U . . .
H18B H 0.165489 0.586558 0.609487 0.089 Uiso 1 1 calc R U . . .
H18C H 0.159549 0.657554 0.681422 0.089 Uiso 1 1 calc R U . . .
C19 C 0.2808(15) 0.4158(16) 0.6406(14) 0.068(6) Uani 1 1 d D . . . .
H19A H 0.224675 0.459488 0.640701 0.102 Uiso 1 1 calc R U . . .
H19B H 0.262955 0.380904 0.672589 0.102 Uiso 1 1 calc R U . . .
H19C H 0.273208 0.382044 0.590075 0.102 Uiso 1 1 calc R U . . .
C20 C 0.482(2) 0.5084(14) 0.6031(10) 0.057(5) Uani 1 1 d D . . . .
H20A H 0.424330 0.547170 0.588785 0.086 Uiso 1 1 calc R U . . .
H20B H 0.485749 0.463865 0.559690 0.086 Uiso 1 1 calc R U . . .
H20C H 0.561169 0.537548 0.622664 0.086 Uiso 1 1 calc R U . . .
C21 C 0.530(2) 0.3747(12) 0.6783(18) 0.083(8) Uani 1 1 d D . . . .
H21A H 0.546688 0.352268 0.628989 0.124 Uiso 1 1 calc R U . . .
H21B H 0.488798 0.331884 0.693311 0.124 Uiso 1 1 calc R U . . .
H21C H 0.605850 0.393064 0.713791 0.124 Uiso 1 1 calc R U . . .
C22 C 0.2506(12) 0.5321(13) 0.8280(12) 0.047(4) Uani 1 1 d D . . . .
H22A H 0.234907 0.590780 0.839963 0.070 Uiso 1 1 calc R U . . .
H22B H 0.224491 0.505286 0.863502 0.070 Uiso 1 1 calc R U . . .
H22C H 0.206756 0.505736 0.777929 0.070 Uiso 1 1 calc R U . . .
C23 C 0.4898(18) 0.5903(14) 0.9244(9) 0.057(5) Uani 1 1 d D . . . .
H23A H 0.576069 0.592996 0.927320 0.085 Uiso 1 1 calc R U . . .
H23B H 0.472166 0.567890 0.964683 0.085 Uiso 1 1 calc R U . . .
H23C H 0.461070 0.645894 0.928726 0.085 Uiso 1 1 calc R U . . .
C24 C 0.4443(19) 0.4149(10) 0.8456(11) 0.050(4) Uani 1 1 d D . . . .
H24A H 0.411427 0.374137 0.799325 0.075 Uiso 1 1 calc R U . . .
H24B H 0.407126 0.404445 0.885041 0.075 Uiso 1 1 calc R U . . .
H24C H 0.530577 0.410560 0.858982 0.075 Uiso 1 1 calc R U . . .
C25 C 0.8902(16) 0.7531(11) 0.6840(13) 0.055(5) Uani 1 1 d D . . . .
H25A H 0.862206 0.794586 0.721562 0.083 Uiso 1 1 calc R U . . .
H25B H 0.898810 0.776998 0.642655 0.083 Uiso 1 1 calc R U . . .
H25C H 0.967436 0.735610 0.705713 0.083 Uiso 1 1 calc R U . . .
C26 C 0.6553(14) 0.6829(12) 0.5772(9) 0.046(4) Uani 1 1 d D . . . .
H26A H 0.596804 0.635358 0.559631 0.068 Uiso 1 1 calc R U . . .
H26B H 0.687539 0.692544 0.535672 0.068 Uiso 1 1 calc R U . . .
H26C H 0.616655 0.731952 0.598587 0.068 Uiso 1 1 calc R U . . .
C27 C 0.854(2) 0.5776(13) 0.5945(13) 0.062(5) Uani 1 1 d D . . . .
H27A H 0.919744 0.559580 0.627709 0.093 Uiso 1 1 calc R U . . .
H27B H 0.885654 0.598551 0.557503 0.093 Uiso 1 1 calc R U . . .
H27C H 0.796469 0.530705 0.569668 0.093 Uiso 1 1 calc R U . . .
C28 C 0.7560(18) 0.5751(12) 0.8568(9) 0.047(4) Uani 1 1 d D . . . .
H28A H 0.718308 0.626030 0.874606 0.071 Uiso 1 1 calc R U . . .
H28B H 0.820582 0.566668 0.896183 0.071 Uiso 1 1 calc R U . . .
H28C H 0.696721 0.528146 0.842616 0.071 Uiso 1 1 calc R U . . .
C29 C 0.9694(13) 0.6381(15) 0.8113(14) 0.069(6) Uani 1 1 d D . . . .
H29A H 1.004072 0.645159 0.769809 0.103 Uiso 1 1 calc R U . . .
H29B H 1.020856 0.605375 0.839805 0.103 Uiso 1 1 calc R U . . .
H29C H 0.962648 0.692403 0.843305 0.103 Uiso 1 1 calc R U . . .
C30 C 0.847(3) 0.4777(12) 0.7243(16) 0.082(8) Uani 1 1 d D . . . .
H30A H 0.841751 0.438498 0.754862 0.124 Uiso 1 1 calc R U . . .
H30B H 0.927369 0.478710 0.713601 0.124 Uiso 1 1 calc R U . . .
H30C H 0.788260 0.460556 0.677753 0.124 Uiso 1 1 calc R U . . .
K1 K 0.8639(4) 1.1848(2) 0.8116(2) 0.0451(9) Uani 1 1 d . . . . .
O1 O 0.6227(13) 1.1832(11) 0.7426(8) 0.064(4) Uani 1 1 d D . . . .
O2 O 0.8070(14) 1.1742(11) 0.6570(8) 0.072(4) Uani 1 1 d D . . . .
O3 O 0.8683(12) 1.2983(8) 0.9489(8) 0.051(3) Uani 1 1 d D . . . .
O4 O 1.0282(15) 1.3239(10) 0.8602(9) 0.067(4) Uani 1 1 d D . . . .
O5 O 0.8234(11) 1.0365(8) 0.8477(8) 0.048(3) Uani 1 1 d D . . . .
O6 O 1.0150(11) 1.0555(8) 0.7813(7) 0.046(3) Uani 1 1 d D . . . .
N6 N 0.6690(12) 1.1673(9) 0.8959(8) 0.049(3) Uani 1 1 d D . . . .
N7 N 1.0596(17) 1.2000(10) 0.7257(9) 0.062(4) Uani 1 1 d D . . . .
C31 C 0.5600(17) 1.1969(17) 0.8601(12) 0.068(6) Uani 1 1 d D . . . .
H31A H 0.568041 1.257864 0.869339 0.082 Uiso 1 1 calc R U . . .
H31B H 0.492614 1.181949 0.880913 0.082 Uiso 1 1 calc R U . . .
C32 C 0.5357(19) 1.159(2) 0.7786(12) 0.082(7) Uani 1 1 d D . . . .
H32A H 0.531365 1.098442 0.770182 0.098 Uiso 1 1 calc R U . . .
H32B H 0.457077 1.175414 0.755815 0.098 Uiso 1 1 calc R U . . .
C33 C 0.603(2) 1.149(2) 0.6655(10) 0.095(8) Uani 1 1 d D . . . .
H33A H 0.519604 1.155006 0.642132 0.113 Uiso 1 1 calc R U . . .
H33B H 0.616015 1.088752 0.656037 0.113 Uiso 1 1 calc R U . . .
C34 C 0.6865(19) 1.191(2) 0.6329(15) 0.101(9) Uani 1 1 d D . . . .
H34A H 0.664449 1.172877 0.578265 0.121 Uiso 1 1 calc R U . . .
H34B H 0.678697 1.251450 0.647040 0.121 Uiso 1 1 calc R U . . .
C35 C 0.889(2) 1.2172(18) 0.6302(15) 0.087(7) Uani 1 1 d D . . . .
H35A H 0.892287 1.276921 0.653910 0.105 Uiso 1 1 calc R U . . .
H35B H 0.862014 1.209758 0.576115 0.105 Uiso 1 1 calc R U . . .
C36 C 1.009(2) 1.1850(18) 0.6469(11) 0.076(6) Uani 1 1 d D . . . .
H36A H 1.003116 1.124781 0.624723 0.092 Uiso 1 1 calc R U . . .
H36B H 1.063390 1.211304 0.623259 0.092 Uiso 1 1 calc R U . . .
C37 C 0.7074(18) 1.2197(12) 0.9707(10) 0.057(4) Uani 1 1 d D . . . .
H37A H 0.766704 1.190790 0.999475 0.069 Uiso 1 1 calc R U . . .
H37B H 0.637793 1.226413 0.994559 0.069 Uiso 1 1 calc R U . . .
C38 C 0.7607(17) 1.3035(13) 0.9750(13) 0.062(5) Uani 1 1 d D . . . .
H38A H 0.703278 1.332492 0.945123 0.074 Uiso 1 1 calc R U . . .
H38B H 0.776561 1.336228 1.026997 0.074 Uiso 1 1 calc R U . . .
C39 C 0.9278(19) 1.3761(11) 0.9581(14) 0.062(5) Uani 1 1 d D . . . .
H39A H 0.939998 1.407485 1.010412 0.075 Uiso 1 1 calc R U . . .
H39B H 0.879352 1.408445 0.926890 0.075 Uiso 1 1 calc R U . . .
C40 C 1.0451(19) 1.3624(14) 0.9363(11) 0.064(5) Uani 1 1 d D . . . .
H40A H 1.091247 1.416044 0.946887 0.077 Uiso 1 1 calc R U . . .
H40B H 1.091061 1.327182 0.965628 0.077 Uiso 1 1 calc R U . . .
C41 C 1.1390(19) 1.3149(17) 0.8383(13) 0.077(6) Uani 1 1 d D . . . .
H41A H 1.185179 1.274918 0.861787 0.092 Uiso 1 1 calc R U . . .
H41B H 1.186060 1.368582 0.853398 0.092 Uiso 1 1 calc R U . . .
C42 C 1.114(3) 1.2842(14) 0.7559(12) 0.078(7) Uani 1 1 d D . . . .
H42A H 1.059867 1.322159 0.734387 0.094 Uiso 1 1 calc R U . . .
H42B H 1.189239 1.287582 0.738978 0.094 Uiso 1 1 calc R U . . .
C43 C 0.6561(15) 1.0818(11) 0.9000(12) 0.051(4) Uani 1 1 d D . . . .
H43A H 0.602173 1.050282 0.854148 0.061 Uiso 1 1 calc R U . . .
H43B H 0.617837 1.079775 0.941933 0.061 Uiso 1 1 calc R U . . .
C44 C 0.7713(15) 1.0401(13) 0.9097(10) 0.049(4) Uani 1 1 d D . . . .
H44A H 0.826589 1.071282 0.955111 0.059 Uiso 1 1 calc R U . . .
H44B H 0.756227 0.983515 0.915214 0.059 Uiso 1 1 calc R U . . .
C45 C 0.9101(16) 0.9772(12) 0.8409(10) 0.049(4) Uani 1 1 d D . . . .
H45A H 0.873319 0.921708 0.836702 0.059 Uiso 1 1 calc R U . . .
H45B H 0.975062 0.990529 0.885465 0.059 Uiso 1 1 calc R U . . .
C46 C 0.9599(17) 0.9768(10) 0.7737(10) 0.047(4) Uani 1 1 d D . . . .
H46A H 1.018831 0.934256 0.768218 0.056 Uiso 1 1 calc R U . . .
H46B H 0.895113 0.963253 0.728978 0.056 Uiso 1 1 calc R U . . .
C47 C 1.0866(19) 1.0519(12) 0.7284(12) 0.056(5) Uani 1 1 d D . . . .
H47A H 1.037091 1.032434 0.677915 0.067 Uiso 1 1 calc R U . . .
H47B H 1.149083 1.012593 0.735282 0.067 Uiso 1 1 calc R U . . .
C48 C 1.143(2) 1.1365(11) 0.7374(13) 0.062(5) Uani 1 1 d D . . . .
H48A H 1.192852 1.154503 0.787915 0.074 Uiso 1 1 calc R U . . .
H48B H 1.196907 1.132699 0.702086 0.074 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 Si3 3.417(5) . ?
U1 N1 2.271(14) . ?
U1 N2 2.229(13) . ?
U1 N3 2.342(13) . ?
U1 N4 2.318(13) . ?
U1 N5 2.366(12) . ?
Si1 N3 1.752(11) . ?
Si1 C13 1.863(13) . ?
Si1 C14 1.862(13) . ?
Si1 C15 1.879(13) . ?
Si2 N3 1.722(11) . ?
Si2 C16 1.876(13) . ?
Si2 C17 1.880(13) . ?
Si2 C18 1.876(13) . ?
Si3 N4 1.754(11) . ?
Si3 C19 1.872(13) . ?
Si3 C20 1.876(13) . ?
Si3 C21 1.849(14) . ?
Si4 N4 1.745(11) . ?
Si4 C22 1.866(12) . ?
Si4 C23 1.878(13) . ?
Si4 C24 1.878(13) . ?
Si5 N5 1.722(11) . ?
Si5 C25 1.881(13) . ?
Si5 C26 1.872(13) . ?
Si5 C27 1.868(13) . ?
Si6 N5 1.728(11) . ?
Si6 C28 1.864(13) . ?
Si6 C29 1.875(14) . ?
Si6 C30 1.873(14) . ?
N1 N2 1.431(19) . ?
N1 C1 1.407(13) . ?
N2 C7 1.385(14) . ?
C1 C6 1.3900 . ?
C1 C2 1.3900 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C4 C3 1.3900 . ?
C3 C2 1.3900 . ?
C7 C12 1.3900 . ?
C7 C8 1.3900 . ?
C12 C11 1.3900 . ?
C11 C10 1.3900 . ?
C10 C9 1.3900 . ?
C9 C8 1.3900 . ?
K1 O1 2.815(16) . ?
K1 O2 2.842(16) . ?
K1 O3 2.836(14) . ?
K1 O4 2.822(16) . ?
K1 O5 2.772(13) . ?
K1 O6 2.814(13) . ?
K1 N6 3.046(16) . ?
K1 N7 3.066(18) . ?
O1 C32 1.417(15) . ?
O1 C33 1.415(15) . ?
O2 C34 1.422(15) . ?
O2 C35 1.411(16) . ?
O3 C38 1.416(15) . ?
O3 C39 1.414(15) . ?
O4 C40 1.412(15) . ?
O4 C41 1.414(15) . ?
O5 C44 1.413(14) . ?
O5 C45 1.417(14) . ?
O6 C46 1.413(14) . ?
O6 C47 1.412(14) . ?
N6 C31 1.453(15) . ?
N6 C37 1.463(16) . ?
N6 C43 1.453(16) . ?
N7 C36 1.457(16) . ?
N7 C42 1.463(16) . ?
N7 C48 1.465(16) . ?
C31 C32 1.497(18) . ?
C33 C34 1.493(19) . ?
C35 C36 1.490(18) . ?
C37 C38 1.496(17) . ?
C39 C40 1.491(17) . ?
C41 C42 1.496(18) . ?
C43 C44 1.502(16) . ?
C45 C46 1.497(16) . ?
C47 C48 1.502(17) . ?

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 Si3 121.1(4) . . ?
N1 U1 N3 90.5(5) . . ?
N1 U1 N4 94.4(4) . . ?
N1 U1 N5 130.2(5) . . ?
N2 U1 Si3 143.2(4) . . ?
N2 U1 N1 37.1(5) . . ?
N2 U1 N3 102.0(5) . . ?
N2 U1 N4 116.3(4) . . ?
N2 U1 N5 94.4(5) . . ?
N3 U1 Si3 108.1(3) . . ?
N3 U1 N5 117.4(4) . . ?
N4 U1 Si3 28.1(3) . . ?
N4 U1 N3 120.9(4) . . ?
N4 U1 N5 103.2(5) . . ?
N5 U1 Si3 90.1(4) . . ?
N3 Si1 C13 112.1(7) . . ?
N3 Si1 C14 115.1(7) . . ?
N3 Si1 C15 113.2(9) . . ?
C13 Si1 C15 105.4(10) . . ?
C14 Si1 C13 105.7(8) . . ?
C14 Si1 C15 104.5(8) . . ?
N3 Si2 C16 115.1(9) . . ?
N3 Si2 C17 112.5(9) . . ?
N3 Si2 C18 108.9(8) . . ?
C16 Si2 C17 106.3(11) . . ?
C16 Si2 C18 104.3(10) . . ?
C18 Si2 C17 109.5(12) . . ?
N4 Si3 U1 38.5(4) . . ?
N4 Si3 C19 115.2(9) . . ?
N4 Si3 C20 106.6(9) . . ?
N4 Si3 C21 117.4(12) . . ?
C19 Si3 U1 129.5(9) . . ?
C19 Si3 C20 109.0(12) . . ?
C20 Si3 U1 68.1(7) . . ?
C21 Si3 U1 125.5(9) . . ?
C21 Si3 C19 104.6(13) . . ?
C21 Si3 C20 103.2(11) . . ?
N4 Si4 C22 111.2(9) . . ?
N4 Si4 C23 114.6(8) . . ?
N4 Si4 C24 114.5(8) . . ?
C22 Si4 C23 105.9(10) . . ?
C22 Si4 C24 106.7(9) . . ?
C24 Si4 C23 103.3(11) . . ?
N5 Si5 C25 112.5(9) . . ?
N5 Si5 C26 111.0(7) . . ?
N5 Si5 C27 114.8(10) . . ?
C26 Si5 C25 109.4(10) . . ?
C27 Si5 C25 106.3(10) . . ?
C27 Si5 C26 102.4(10) . . ?
N5 Si6 C28 111.0(8) . . ?
N5 Si6 C29 112.0(10) . . ?
N5 Si6 C30 113.0(11) . . ?
C28 Si6 C29 107.0(11) . . ?
C28 Si6 C30 109.2(12) . . ?
C30 Si6 C29 104.3(13) . . ?
N2 N1 U1 69.9(7) . . ?
C1 N1 U1 136.7(11) . . ?
C1 N1 N2 120.5(12) . . ?
N1 N2 U1 73.0(7) . . ?
C7 N2 U1 149.0(10) . . ?
C7 N2 N1 120.4(12) . . ?
Si1 N3 U1 121.0(5) . . ?
Si2 N3 U1 123.5(6) . . ?
Si2 N3 Si1 115.3(7) . . ?
Si3 N4 U1 113.4(5) . . ?
Si4 N4 U1 129.4(6) . . ?
Si4 N4 Si3 117.2(8) . . ?
Si5 N5 U1 122.9(6) . . ?
Si5 N5 Si6 116.8(7) . . ?
Si6 N5 U1 120.3(6) . . ?
C6 C1 N1 121.2(9) . . ?
C6 C1 C2 120.0 . . ?
C2 C1 N1 118.7(9) . . ?
C5 C6 C1 120.0 . . ?
C6 C5 C4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C2 C3 C4 120.0 . . ?
C3 C2 C1 120.0 . . ?
N2 C7 C12 124.3(9) . . ?
N2 C7 C8 115.6(9) . . ?
C12 C7 C8 120.0 . . ?
C11 C12 C7 120.0 . . ?
C12 C11 C10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C10 C9 C8 120.0 . . ?
C9 C8 C7 120.0 . . ?
O1 K1 O2 61.7(4) . . ?
O1 K1 O3 100.7(4) . . ?
O1 K1 O4 126.1(5) . . ?
O1 K1 N6 59.9(4) . . ?
O1 K1 N7 120.0(5) . . ?
O2 K1 N6 120.8(5) . . ?
O2 K1 N7 58.9(5) . . ?
O3 K1 O2 140.8(5) . . ?
O3 K1 N6 60.9(4) . . ?
O3 K1 N7 119.8(4) . . ?
O4 K1 O2 100.6(5) . . ?
O4 K1 O3 59.7(4) . . ?
O4 K1 N6 120.1(4) . . ?
O4 K1 N7 60.6(4) . . ?
O5 K1 O1 91.1(5) . . ?
O5 K1 O2 113.6(5) . . ?
O5 K1 O3 100.7(4) . . ?
O5 K1 O4 138.9(5) . . ?
O5 K1 O6 60.0(3) . . ?
O5 K1 N6 60.2(4) . . ?
O5 K1 N7 119.2(4) . . ?
O6 K1 O1 125.6(5) . . ?
O6 K1 O2 87.4(4) . . ?
O6 K1 O3 127.6(4) . . ?
O6 K1 O4 101.5(4) . . ?
O6 K1 N6 120.0(4) . . ?
O6 K1 N7 59.4(4) . . ?
N6 K1 N7 179.3(5) . . ?
C32 O1 K1 117.8(12) . . ?
C33 O1 K1 111.9(13) . . ?
C33 O1 C32 115.4(19) . . ?
C34 O2 K1 111.9(14) . . ?
C35 O2 K1 115.4(14) . . ?
C35 O2 C34 113.3(19) . . ?
C38 O3 K1 116.6(12) . . ?
C39 O3 K1 115.2(12) . . ?
C39 O3 C38 113.4(15) . . ?
C40 O4 K1 114.8(11) . . ?
C40 O4 C41 110.6(17) . . ?
C41 O4 K1 116.8(13) . . ?
C44 O5 K1 116.9(11) . . ?
C44 O5 C45 113.4(13) . . ?
C45 O5 K1 118.3(10) . . ?
C46 O6 K1 113.1(10) . . ?
C47 O6 K1 121.7(11) . . ?
C47 O6 C46 110.3(13) . . ?
C31 N6 K1 109.0(12) . . ?
C31 N6 C37 108.8(16) . . ?
C37 N6 K1 107.4(10) . . ?
C43 N6 K1 109.0(10) . . ?
C43 N6 C31 113.3(17) . . ?
C43 N6 C37 109.1(15) . . ?
C36 N7 K1 110.4(14) . . ?
C36 N7 C42 111.5(19) . . ?
C36 N7 C48 108.5(17) . . ?
C42 N7 K1 105.6(13) . . ?
C42 N7 C48 113.2(19) . . ?
C48 N7 K1 107.6(11) . . ?
N6 C31 C32 109.9(18) . . ?
O1 C32 C31 113.8(19) . . ?
O1 C33 C34 109(2) . . ?
O2 C34 C33 112(2) . . ?
O2 C35 C36 109.5(19) . . ?
N7 C36 C35 113.5(19) . . ?
N6 C37 C38 115.2(17) . . ?
O3 C38 C37 111.3(16) . . ?
O3 C39 C40 108.5(16) . . ?
O4 C40 C39 110.3(18) . . ?
O4 C41 C42 107(2) . . ?
N7 C42 C41 116.6(18) . . ?
N6 C43 C44 114.2(15) . . ?
O5 C44 C43 109.9(14) . . ?
O5 C45 C46 109.9(14) . . ?
O6 C46 C45 109.1(15) . . ?
O6 C47 C48 109.1(15) . . ?
N7 C48 C47 115.1(18) . . ?

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 Si3 N4 Si4 178.1(14) . . . . ?
U1 N1 N2 C7 -149.3(13) . . . . ?
U1 N1 C1 C6 -107.4(13) . . . . ?
U1 N1 C1 C2 75.2(16) . . . . ?
U1 N2 C7 C12 -117.5(17) . . . . ?
U1 N2 C7 C8 66(2) . . . . ?
N1 N2 C7 C12 -9.0(18) . . . . ?
N1 N2 C7 C8 174.9(11) . . . . ?
N1 C1 C6 C5 -177.3(13) . . . . ?
N1 C1 C2 C3 177.4(13) . . . . ?
N2 N1 C1 C6 -14.9(18) . . . . ?
N2 N1 C1 C2 167.7(11) . . . . ?
N2 C7 C12 C11 -175.9(13) . . . . ?
N2 C7 C8 C9 176.3(12) . . . . ?
C1 N1 N2 U1 -133.1(14) . . . . ?
C1 N1 N2 C7 77.6(18) . . . . ?
C1 C6 C5 C4 0.0 . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C4 C3 C2 C1 0.0 . . . . ?
C2 C1 C6 C5 0.0 . . . . ?
C7 C12 C11 C10 0.0 . . . . ?
C12 C7 C8 C9 0.0 . . . . ?
C12 C11 C10 C9 0.0 . . . . ?
C11 C10 C9 C8 0.0 . . . . ?
C10 C9 C8 C7 0.0 . . . . ?
C8 C7 C12 C11 0.0 . . . . ?
C13 Si1 N3 U1 11.5(12) . . . . ?
C13 Si1 N3 Si2 -172.7(9) . . . . ?
C14 Si1 N3 U1 -109.3(8) . . . . ?
C14 Si1 N3 Si2 66.6(11) . . . . ?
C15 Si1 N3 U1 130.6(9) . . . . ?
C15 Si1 N3 Si2 -53.6(11) . . . . ?
C16 Si2 N3 U1 143.9(10) . . . . ?
C16 Si2 N3 Si1 -31.9(13) . . . . ?
C17 Si2 N3 U1 -94.2(12) . . . . ?
C17 Si2 N3 Si1 90.1(12) . . . . ?
C18 Si2 N3 U1 27.3(13) . . . . ?
C18 Si2 N3 Si1 -148.4(11) . . . . ?
C19 Si3 N4 U1 -122.5(11) . . . . ?
C19 Si3 N4 Si4 55.6(14) . . . . ?
C20 Si3 N4 U1 -1.4(11) . . . . ?
C20 Si3 N4 Si4 176.7(10) . . . . ?
C21 Si3 N4 U1 113.6(10) . . . . ?
C21 Si3 N4 Si4 -68.3(12) . . . . ?
C22 Si4 N4 U1 94.3(11) . . . . ?
C22 Si4 N4 Si3 -83.4(11) . . . . ?
C23 Si4 N4 U1 -25.7(14) . . . . ?
C23 Si4 N4 Si3 156.6(11) . . . . ?
C24 Si4 N4 U1 -144.7(10) . . . . ?
C24 Si4 N4 Si3 37.6(13) . . . . ?
C25 Si5 N5 U1 103.0(11) . . . . ?
C25 Si5 N5 Si6 -76.2(12) . . . . ?
C26 Si5 N5 U1 -19.8(12) . . . . ?
C26 Si5 N5 Si6 161.0(9) . . . . ?
C27 Si5 N5 U1 -135.3(11) . . . . ?
C27 Si5 N5 Si6 45.5(13) . . . . ?
C28 Si6 N5 U1 -8.7(12) . . . . ?
C28 Si6 N5 Si5 170.5(9) . . . . ?
C29 Si6 N5 U1 -128.3(11) . . . . ?
C29 Si6 N5 Si5 51.0(13) . . . . ?
C30 Si6 N5 U1 114.3(13) . . . . ?
C30 Si6 N5 Si5 -66.4(14) . . . . ?
K1 O1 C32 C31 44(3) . . . . ?
K1 O1 C33 C34 -53(2) . . . . ?
K1 O2 C34 C33 -44(3) . . . . ?
K1 O2 C35 C36 59(3) . . . . ?
K1 O3 C38 C37 48(2) . . . . ?
K1 O3 C39 C40 -48(2) . . . . ?
K1 O4 C40 C39 -48(2) . . . . ?
K1 O4 C41 C42 54(2) . . . . ?
K1 O5 C44 C43 55.6(19) . . . . ?
K1 O5 C45 C46 -38(2) . . . . ?
K1 O6 C46 C45 -53.8(16) . . . . ?
K1 O6 C47 C48 43(2) . . . . ?
K1 N6 C31 C32 49(2) . . . . ?
K1 N6 C37 C38 43.6(18) . . . . ?
K1 N6 C43 C44 36.9(19) . . . . ?
K1 N7 C36 C35 36(3) . . . . ?
K1 N7 C42 C41 44(3) . . . . ?
K1 N7 C48 C47 47(2) . . . . ?
O1 C33 C34 O2 68(3) . . . . ?
O2 C35 C36 N7 -65(3) . . . . ?
O3 C39 C40 O4 65(3) . . . . ?
O4 C41 C42 N7 -68(3) . . . . ?
O5 C45 C46 O6 61(2) . . . . ?
O6 C47 C48 N7 -62(2) . . . . ?
N6 C31 C32 O1 -65(3) . . . . ?
N6 C37 C38 O3 -65(2) . . . . ?
N6 C43 C44 O5 -63(2) . . . . ?
C31 N6 C37 C38 -74(2) . . . . ?
C31 N6 C43 C44 158.4(17) . . . . ?
C32 O1 C33 C34 169(2) . . . . ?
C33 O1 C32 C31 180(2) . . . . ?
C34 O2 C35 C36 -170(2) . . . . ?
C35 O2 C34 C33 -177(2) . . . . ?
C36 N7 C42 C41 164(2) . . . . ?
C36 N7 C48 C47 -73(2) . . . . ?
C37 N6 C31 C32 165.5(18) . . . . ?
C37 N6 C43 C44 -80(2) . . . . ?
C38 O3 C39 C40 174.0(19) . . . . ?
C39 O3 C38 C37 -174.6(19) . . . . ?
C40 O4 C41 C42 -172.7(19) . . . . ?
C41 O4 C40 C39 176.8(19) . . . . ?
C42 N7 C36 C35 -81(3) . . . . ?
C42 N7 C48 C47 162.8(17) . . . . ?
C43 N6 C31 C32 -73(2) . . . . ?
C43 N6 C37 C38 161.7(16) . . . . ?
C44 O5 C45 C46 179.5(16) . . . . ?
C45 O5 C44 C43 -161.4(17) . . . . ?
C46 O6 C47 C48 179.6(17) . . . . ?
C47 O6 C46 C45 166.1(16) . . . . ?
C48 N7 C36 C35 154(2) . . . . ?
C48 N7 C42 C41 -73(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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.403
_oxdiff_exptl_absorpt_empirical_full_min 0.486
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
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 0.658(3) 19215 7457 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.342(3) 0 7457 nmt 1.0005 0.0024 0.0024 -0.0162 -0.9754 0.0792 -0.6598
-0.0987 -1.0185

_twin_special_details            
;
Component 2 rotated by -175.1076° 
around [0.95 -0.02 -0.31] (reciprocal) or [1.00 0.00 0.00] (direct)
;
