# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_ks1070c
_database_code_depnum_ccdc_archive 'CCDC 2411215'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;EPFL
Switzerland
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C90 H146 N8 O4 U2, 3.6[C7H8]'
_chemical_formula_sum            'C115.20 H174.80 N8 O4 U2'
_chemical_formula_weight         2211.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C111 H170 N8 O4 U2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.8734(7)
_cell_length_b                   20.7159(8)
_cell_length_c                   26.4929(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.162(3)
_cell_angle_gamma                90
_cell_volume                     5387.5(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11851
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.4630
_cell_measurement_theta_min      2.6960
_shelx_estimated_absorpt_T_max   0.709
_shelx_estimated_absorpt_T_min   0.277
_exptl_absorpt_coefficient_mu    8.801
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.281
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
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 gold'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2276
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 1 0.0945
0 2 -1 0.0152
0 1 2 0.0417
0 -13 4 0.0245
1 0 2 0.0775
-1 -13 3 0.0343
0 0 1 0.0329
0 0 -1 0.0192
-5 0 13 0.0712
1 -2 -2 0.0757
0 13 -4 0.0133
1 -12 -7 0.0267
5 -1 -11 0.0796
0 -9 13 0.0324
-1 -10 -10 0.0403
-1 -8 14 0.0362
-2 1 0 0.0879
-3 2 -13 0.0530

_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.042
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.9995 1.0008 1.0006 0.3258 -0.0019 -0.0708
-0.0005 1.9994 -1.0007 -0.0171 -0.0175 -0.1577
-0.0005 0.9998 1.9991 0.0410 0.1246 -0.0448
0.1265 -13.1339 3.7186 0.0747 -0.0419 0.9963
0.9997 0.0005 2.0002 0.1919 0.0701 0.0210
-1.1642 -13.1255 2.5533 -0.1450 -0.0566 0.9878
-0.0001 0.0000 0.9998 0.0198 0.0533 0.0136
0.0001 -0.0000 -0.9998 -0.0198 -0.0533 -0.0136
-4.7532 0.0278 12.8499 -0.4690 0.8597 0.2024
1.0008 -1.9990 -1.9980 0.1100 -0.1790 0.1107
-0.4286 13.1145 -3.5825 -0.1180 0.0598 -0.9912
0.5543 -12.1167 -7.4553 -0.0804 -0.6352 0.7682
5.1950 -0.8491 -11.4690 0.5625 -0.8170 -0.1271
0.4246 -8.8526 12.7125 0.3045 0.5036 0.8085
-1.3116 -10.3124 -10.0333 -0.4132 -0.6720 0.6145
-0.7680 -8.0963 13.7293 0.1441 0.6151 0.7752
-2.0002 0.9987 -0.0017 -0.3033 0.0910 -0.0597
-3.4745 1.8721 -13.1727 -0.7878 -0.5417 -0.2929

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57981
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         2.714
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     67.00 108.00   0.50    1.50    --   63.87  18.00 169.00   82
  2  ω    -76.00 -50.00   0.50    1.50    --  -64.59 -18.00   1.00   52
  3  ω   -114.00 -77.00   0.50    1.50    --  -71.12 -18.00   1.00   74
  4  ω     96.00 122.00   0.50    1.50    --   75.73  18.00 169.00   52
  5  ω     45.00  75.00   0.50    1.50    --   76.61  18.00 169.00   60
  6  ω     30.00  55.00   0.50    1.50    --   63.87 -95.00 150.00   50
  7  ω     28.00 101.00   0.50    1.50    --   63.87   0.00 -60.00  146
  8  ω    -57.00 -27.00   0.50    1.50    --  -64.59   0.00  60.00   60
  9  ω    -91.00 -43.00   0.50    1.50    --  -64.59 125.00-150.00   96
 10  ω    -85.00 -32.00   0.50    1.50    --  -71.12 111.00 150.00  106
 11  ω    -71.00 -40.00   0.50    1.50    --  -71.12   0.00-180.00   62
 12  ω    -86.00 -31.00   0.50    1.50    --  -71.12 111.00-180.00  110
 13  ω    -78.00 -39.00   0.50    1.50    --  -71.12 111.00  30.00   78
 14  ω    -70.00 -37.00   0.50    1.50    --  -71.12   0.00-150.00   66
 15  ω     53.00  79.00   0.50    1.50    --   75.73-111.00-120.00   52
 16  ω     38.00  63.00   0.50    1.50    --   75.73 -95.00-180.00   50
 17  ω     68.00  93.00   0.50    1.50    --   75.73-111.00 120.00   50
 18  ω     66.00  92.00   0.50    1.50    --   75.73-111.00 -60.00   52
 19  ω     59.00  93.00   0.50    1.50    --   76.61-125.00-120.00   68
 20  ω     48.00 103.00   0.50    1.50    --   76.61-125.00 -90.00  110
 21  ω     78.00 103.00   0.50    1.50    --   76.61-125.00 -30.00   50
 22  ω     71.00 102.00   0.50    1.50    --   76.61-125.00 120.00   62
 23  ω     48.00  74.00   0.50    1.50    --   76.61 -95.00   0.00   52
 24  ω     54.00  80.00   0.50    1.50    --   76.61 -95.00 150.00   52
 25  ω     55.00  81.00   0.50    1.50    --   76.61 -95.00 120.00   52
 26  ω     51.00  87.00   0.50    1.50    --   76.61-125.00  90.00   72
 27  ω     60.00 103.00   0.50    1.50    --   76.61-125.00   0.00   86
 28  ω     42.00  80.00   0.50    1.50    --   76.61 -95.00 -60.00   76
 29  ω     71.00 116.00   0.50    1.50    --   79.75   1.00-145.30   90
 30  ω     65.00 126.00   0.50    1.50    --   79.75  21.00  48.01  122
 31  ω     98.00 124.00   0.50    1.50    --   79.75  19.00 -13.93   52
 32  ω     54.00  83.00   0.50    1.50    --   79.75  19.00 -13.93   58
 33  ω     40.00 101.00   0.50    1.50    --   79.75-115.00 -73.44  122
 34  ω     70.00  96.00   0.50    1.50    --   79.75  21.00 -94.17   52
 35  ω     42.00  82.00   0.50    1.50    --   79.75   0.00-160.30   80
 36  ω     66.00 107.00   0.50    1.50    --   79.75  23.00   2.58   82
 37  ω     58.00  84.00   0.50    1.50    --   79.75  17.00-165.59   52
 38  ω     53.00 103.00   0.50    1.50    --   79.75   5.00 137.30  100
 39  ω     63.00 106.00   0.50    1.50    --   79.75   6.00 -60.43   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1522960000
_diffrn_orient_matrix_UB_12      0.0013999000
_diffrn_orient_matrix_UB_13      0.0198372000
_diffrn_orient_matrix_UB_21      -0.0365991000
_diffrn_orient_matrix_UB_22      0.0179351000
_diffrn_orient_matrix_UB_23      0.0533287000
_diffrn_orient_matrix_UB_31      -0.0061650000
_diffrn_orient_matrix_UB_32      -0.0720615000
_diffrn_orient_matrix_UB_33      0.0136232000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7365
_reflns_number_total             9157
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.936
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         9157
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0412
_refine_ls_restrained_S_all      1.052
_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)+(0.0692P)²+0.9433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1092
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C38 \\sim C46-C38 \\sim C40-C38 \\sim C47-C38 \\sim C41-C38 \\sim C48-C38
 with sigma of 0.02
 C46-C48 \\sim C48-C47 \\sim C46-C47
 with sigma of 0.02
 C39-C41 \\sim C41-C40 \\sim C39-C40
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C39 \\sim C46 \\sim C38 \\sim C40 \\sim C47 \\sim C48 \\sim C41: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(1)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
5.b Me refined with riding coordinates:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C8(H8), C33(H33), C35(H35)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C27(H27A,
 H27B,H27C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C48(H48A,H48B,
 H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.51822(2) 0.43086(2) 0.43875(2) 0.03398(8) Uani 1 1 d . . . . .
O1 O 0.6965(4) 0.45295(18) 0.39671(16) 0.0399(9) Uani 1 1 d . . . . .
O2 O 0.5198(4) 0.33159(16) 0.46909(16) 0.0377(9) Uani 1 1 d . . . . .
N1 N 0.5346(4) 0.3463(2) 0.35152(19) 0.0369(10) Uani 1 1 d . . . . .
N2 N 0.3279(5) 0.4498(2) 0.3574(2) 0.0460(12) Uani 1 1 d . . . . .
N3 N 0.1940(4) 0.2968(2) 0.4284(2) 0.0416(11) Uani 1 1 d . . . . .
N4 N 0.2094(6) 0.2244(3) 0.3332(2) 0.0569(15) Uani 1 1 d . . . . .
C1 C 0.3962(6) 0.4613(3) 0.5176(2) 0.0398(13) Uani 1 1 d . . . . .
H1 H 0.327599 0.434053 0.528567 0.048 Uiso 1 1 calc R U . . .
C2 C 0.5350(6) 0.4502(3) 0.5362(2) 0.0375(12) Uani 1 1 d . . . . .
H2 H 0.557709 0.418068 0.561256 0.045 Uiso 1 1 calc R U . . .
C3 C 0.6415(6) 0.4880(3) 0.5168(2) 0.0401(13) Uani 1 1 d . . . . .
H3 H 0.734766 0.478864 0.527062 0.048 Uiso 1 1 calc R U . . .
C4 C 0.7562(5) 0.4523(3) 0.3544(2) 0.0357(12) Uani 1 1 d . . . . .
C5 C 0.8258(6) 0.5070(3) 0.3370(2) 0.0391(13) Uani 1 1 d . . . . .
C6 C 0.8779(6) 0.5024(3) 0.2901(2) 0.0421(14) Uani 1 1 d . . . . .
H6 H 0.922917 0.539160 0.278368 0.050 Uiso 1 1 calc R U . . .
C7 C 0.8682(6) 0.4474(3) 0.2592(3) 0.0414(14) Uani 1 1 d . . . . .
C8 C 0.8028(5) 0.3941(3) 0.2781(3) 0.0420(14) Uani 1 1 d . . . . .
H8 H 0.794923 0.355496 0.258679 0.050 Uiso 1 1 calc R U . . .
C9 C 0.7487(5) 0.3960(3) 0.3246(2) 0.0366(12) Uani 1 1 d . . . . .
C10 C 0.8415(6) 0.5690(3) 0.3685(3) 0.0448(14) Uani 1 1 d . . . . .
C11 C 0.6990(7) 0.5994(3) 0.3696(3) 0.0485(15) Uani 1 1 d . . . . .
H11A H 0.665640 0.614912 0.335626 0.073 Uiso 1 1 calc R U . . .
H11B H 0.704864 0.635593 0.393552 0.073 Uiso 1 1 calc R U . . .
H11C H 0.636053 0.566827 0.380431 0.073 Uiso 1 1 calc R U . . .
C12 C 0.9091(6) 0.5545(3) 0.4225(3) 0.0465(15) Uani 1 1 d . . . . .
H12A H 0.860305 0.519100 0.437179 0.070 Uiso 1 1 calc R U . . .
H12B H 0.905621 0.593068 0.443649 0.070 Uiso 1 1 calc R U . . .
H12C H 1.004207 0.541919 0.420855 0.070 Uiso 1 1 calc R U . . .
C13 C 0.9301(7) 0.6197(3) 0.3455(3) 0.0564(18) Uani 1 1 d . . . . .
H13A H 1.020198 0.601400 0.342078 0.085 Uiso 1 1 calc R U . . .
H13B H 0.940017 0.657612 0.367755 0.085 Uiso 1 1 calc R U . . .
H13C H 0.886797 0.632553 0.311996 0.085 Uiso 1 1 calc R U . . .
C14 C 0.9190(6) 0.4476(3) 0.2072(3) 0.0488(15) Uani 1 1 d . . . . .
C15 C 0.9146(9) 0.3842(4) 0.1818(4) 0.088(3) Uani 1 1 d . . . . .
H15A H 0.974617 0.353975 0.202034 0.133 Uiso 1 1 calc R U . . .
H15B H 0.945059 0.388731 0.148028 0.133 Uiso 1 1 calc R U . . .
H15C H 0.821054 0.367581 0.178624 0.133 Uiso 1 1 calc R U . . .
C16 C 0.8355(11) 0.4966(5) 0.1725(4) 0.106(4) Uani 1 1 d . . . . .
H16A H 0.740511 0.482290 0.166793 0.159 Uiso 1 1 calc R U . . .
H16B H 0.873574 0.499388 0.139878 0.159 Uiso 1 1 calc R U . . .
H16C H 0.839682 0.539104 0.188788 0.159 Uiso 1 1 calc R U . . .
C17 C 1.0641(8) 0.4712(5) 0.2106(4) 0.096(3) Uani 1 1 d . . . . .
H17A H 1.070603 0.513579 0.227167 0.144 Uiso 1 1 calc R U . . .
H17B H 1.092505 0.474827 0.176421 0.144 Uiso 1 1 calc R U . . .
H17C H 1.123642 0.440548 0.230556 0.144 Uiso 1 1 calc R U . . .
C18 C 0.6809(6) 0.3377(3) 0.3438(3) 0.0446(14) Uani 1 1 d . . . . .
H18A H 0.687981 0.301909 0.319386 0.053 Uiso 1 1 calc R U . . .
H18B H 0.731414 0.324533 0.376447 0.053 Uiso 1 1 calc R U . . .
C19 C 0.4574(6) 0.3744(3) 0.3059(3) 0.0471(15) Uani 1 1 d . . . . .
H19A H 0.377164 0.346828 0.295795 0.056 Uiso 1 1 calc R U . . .
H19B H 0.515699 0.373903 0.277751 0.056 Uiso 1 1 calc R U . . .
C20 C 0.4098(6) 0.4420(3) 0.3131(3) 0.0430(14) Uani 1 1 d . . . . .
H20A H 0.353584 0.455959 0.281759 0.052 Uiso 1 1 calc R U . . .
H20B H 0.490135 0.470813 0.317983 0.052 Uiso 1 1 calc R U . . .
C21 C 0.2749(6) 0.5160(3) 0.3546(3) 0.0470(15) Uani 1 1 d . . . . .
H21A H 0.215753 0.522681 0.381529 0.071 Uiso 1 1 calc R U . . .
H21B H 0.222506 0.522867 0.321445 0.071 Uiso 1 1 calc R U . . .
H21C H 0.350984 0.546546 0.358832 0.071 Uiso 1 1 calc R U . . .
C22 C 0.2132(6) 0.4046(3) 0.3523(3) 0.0498(16) Uani 1 1 d . . . . .
H22A H 0.248791 0.360223 0.349246 0.060 Uiso 1 1 calc R U . . .
H22B H 0.154107 0.414468 0.320701 0.060 Uiso 1 1 calc R U . . .
C23 C 0.1270(6) 0.4068(3) 0.3972(3) 0.0467(15) Uani 1 1 d . . . . .
H23A H 0.181862 0.424341 0.427546 0.056 Uiso 1 1 calc R U . . .
H23B H 0.047309 0.435359 0.388857 0.056 Uiso 1 1 calc R U . . .
C24 C 0.0789(5) 0.3383(3) 0.4081(3) 0.0454(15) Uani 1 1 d . . . . .
H24A H 0.010944 0.340354 0.432934 0.055 Uiso 1 1 calc R U . . .
H24B H 0.034041 0.319085 0.376365 0.055 Uiso 1 1 calc R U . . .
C25 C 0.1614(6) 0.2277(3) 0.4243(3) 0.0450(14) Uani 1 1 d . . . . .
H25A H 0.086986 0.218225 0.445405 0.054 Uiso 1 1 calc R U . . .
H25B H 0.242315 0.202702 0.438304 0.054 Uiso 1 1 calc R U . . .
C26 C 0.1185(6) 0.2045(3) 0.3703(3) 0.0518(16) Uani 1 1 d . . . . .
H26A H 0.113314 0.156779 0.370469 0.062 Uiso 1 1 calc R U . . .
H26B H 0.025973 0.221130 0.359383 0.062 Uiso 1 1 calc R U . . .
C27 C 0.1412(9) 0.2198(4) 0.2825(3) 0.087(3) Uani 1 1 d . . . . .
H27A H 0.122675 0.174400 0.274026 0.130 Uiso 1 1 calc R U . . .
H27B H 0.199478 0.238228 0.258443 0.130 Uiso 1 1 calc R U . . .
H27C H 0.055214 0.243747 0.280474 0.130 Uiso 1 1 calc R U . . .
C28 C 0.3371(7) 0.1886(3) 0.3388(3) 0.0563(18) Uani 1 1 d . . . . .
H28A H 0.328388 0.149767 0.316857 0.068 Uiso 1 1 calc R U . . .
H28B H 0.357322 0.174126 0.374419 0.068 Uiso 1 1 calc R U . . .
C29 C 0.4554(7) 0.2311(3) 0.3240(3) 0.0574(19) Uani 1 1 d . . . . .
H29A H 0.539241 0.205051 0.323041 0.069 Uiso 1 1 calc R U . . .
H29B H 0.431554 0.250872 0.290175 0.069 Uiso 1 1 calc R U . . .
C30 C 0.4763(6) 0.2835(3) 0.3655(3) 0.0465(15) Uani 1 1 d . . . . .
H30A H 0.386885 0.292195 0.377826 0.056 Uiso 1 1 calc R U . . .
H30B H 0.536430 0.265475 0.394354 0.056 Uiso 1 1 calc R U . . .
C31 C 0.2353(5) 0.3150(3) 0.4813(2) 0.0412(13) Uani 1 1 d . . . . .
H31A H 0.154284 0.311215 0.500143 0.049 Uiso 1 1 calc R U . . .
H31B H 0.261430 0.361138 0.481769 0.049 Uiso 1 1 calc R U . . .
C32 C 0.3503(6) 0.2779(2) 0.5106(2) 0.0368(12) Uani 1 1 d . . . . .
C33 C 0.3178(6) 0.2366(3) 0.5483(3) 0.0439(14) Uani 1 1 d . . . . .
H33 H 0.224208 0.229300 0.551736 0.053 Uiso 1 1 calc R U . . .
C34 C 0.4149(6) 0.2050(3) 0.5816(3) 0.0529(16) Uani 1 1 d . . . . .
C35 C 0.5508(6) 0.2145(3) 0.5730(3) 0.0471(15) Uani 1 1 d . . . . .
H35 H 0.619600 0.192520 0.594241 0.057 Uiso 1 1 calc R U . . .
C36 C 0.5911(6) 0.2550(3) 0.5345(3) 0.0427(14) Uani 1 1 d . . . . .
C37 C 0.4878(5) 0.2891(3) 0.5043(2) 0.0406(13) Uani 1 1 d . . . . .
C38 C 0.3713(7) 0.1625(4) 0.6239(3) 0.070(2) Uani 1 1 d D U . . .
C39 C 0.2730(10) 0.1087(5) 0.6001(4) 0.088(3) Uani 0.837(8) 1 d D U P A 2
H39A H 0.191720 0.128724 0.582176 0.132 Uiso 0.837(8) 1 calc R U P A 2
H39B H 0.246055 0.080622 0.627115 0.132 Uiso 0.837(8) 1 calc R U P A 2
H39C H 0.319606 0.082969 0.576179 0.132 Uiso 0.837(8) 1 calc R U P A 2
C40 C 0.4879(9) 0.1246(4) 0.6518(4) 0.075(3) Uani 0.837(8) 1 d D U P A 2
H40A H 0.530556 0.097592 0.627616 0.112 Uiso 0.837(8) 1 calc R U P A 2
H40B H 0.452847 0.097177 0.677608 0.112 Uiso 0.837(8) 1 calc R U P A 2
H40C H 0.555514 0.154665 0.668259 0.112 Uiso 0.837(8) 1 calc R U P A 2
C41 C 0.2978(10) 0.1995(5) 0.6602(4) 0.083(3) Uani 0.837(8) 1 d D U P A 2
H41A H 0.356030 0.234497 0.674897 0.125 Uiso 0.837(8) 1 calc R U P A 2
H41B H 0.274402 0.170731 0.687378 0.125 Uiso 0.837(8) 1 calc R U P A 2
H41C H 0.214240 0.217657 0.642478 0.125 Uiso 0.837(8) 1 calc R U P A 2
C42 C 0.7437(6) 0.2594(3) 0.5278(3) 0.0466(15) Uani 1 1 d . . . . .
C43 C 0.8324(6) 0.2168(3) 0.5650(3) 0.063(2) Uani 1 1 d . . . . .
H43A H 0.829109 0.232940 0.599662 0.095 Uiso 1 1 calc R U . . .
H43B H 0.926619 0.217883 0.556606 0.095 Uiso 1 1 calc R U . . .
H43C H 0.798400 0.172381 0.562697 0.095 Uiso 1 1 calc R U . . .
C44 C 0.7961(6) 0.3287(3) 0.5356(3) 0.061(2) Uani 1 1 d . . . . .
H44A H 0.747046 0.357021 0.510232 0.091 Uiso 1 1 calc R U . . .
H44B H 0.893707 0.329998 0.531890 0.091 Uiso 1 1 calc R U . . .
H44C H 0.780943 0.343461 0.569714 0.091 Uiso 1 1 calc R U . . .
C45 C 0.7645(7) 0.2373(3) 0.4747(3) 0.0593(18) Uani 1 1 d . . . . .
H45A H 0.725835 0.193983 0.468920 0.089 Uiso 1 1 calc R U . . .
H45B H 0.862114 0.236160 0.470994 0.089 Uiso 1 1 calc R U . . .
H45C H 0.718858 0.267330 0.449858 0.089 Uiso 1 1 calc R U . . .
C47 C 0.444(4) 0.2022(17) 0.6685(12) 0.079(6) Uani 0.163(8) 1 d D U P A 1
H47A H 0.404925 0.245791 0.668049 0.118 Uiso 0.163(8) 1 calc R U P A 1
H47B H 0.430161 0.181094 0.700716 0.118 Uiso 0.163(8) 1 calc R U P A 1
H47C H 0.541158 0.204783 0.664978 0.118 Uiso 0.163(8) 1 calc R U P A 1
C46 C 0.425(4) 0.0951(11) 0.622(2) 0.082(6) Uani 0.163(8) 1 d D U P A 1
H46A H 0.393871 0.069871 0.649917 0.123 Uiso 0.163(8) 1 calc R U P A 1
H46B H 0.390754 0.075212 0.589542 0.123 Uiso 0.163(8) 1 calc R U P A 1
H46C H 0.524502 0.096037 0.625353 0.123 Uiso 0.163(8) 1 calc R U P A 1
C48 C 0.2167(19) 0.167(2) 0.625(2) 0.083(6) Uani 0.163(8) 1 d D U P A 1
H48A H 0.193362 0.207892 0.639821 0.124 Uiso 0.163(8) 1 calc R U P A 1
H48B H 0.186217 0.131074 0.645354 0.124 Uiso 0.163(8) 1 calc R U P A 1
H48C H 0.171594 0.163463 0.590196 0.124 Uiso 0.163(8) 1 calc R U P A 1


_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 O1 2.229(4) . ?
U1 O2 2.207(3) . ?
U1 N1 2.918(5) . ?
U1 N2 2.732(5) . ?
U1 C1 2.614(6) 3_666 ?
U1 C1 2.599(6) . ?
U1 C2 2.620(6) 3_666 ?
U1 C2 2.600(6) . ?
U1 C3 2.664(6) 3_666 ?
U1 C3 2.573(6) . ?
O1 C4 1.321(7) . ?
O2 C37 1.345(7) . ?
N1 C18 1.491(7) . ?
N1 C19 1.477(8) . ?
N1 C30 1.485(7) . ?
N2 C20 1.504(8) . ?
N2 C21 1.465(7) . ?
N2 C22 1.466(8) . ?
N3 C24 1.479(7) . ?
N3 C25 1.470(7) . ?
N3 C31 1.467(8) . ?
N4 C26 1.460(9) . ?
N4 C27 1.440(10) . ?
N4 C28 1.457(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.424(8) . ?
C1 C3 1.417(8) 3_666 ?
C2 H2 0.9500 . ?
C2 C3 1.448(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.426(8) . ?
C4 C9 1.407(8) . ?
C5 C6 1.398(8) . ?
C5 C10 1.532(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.401(8) . ?
C7 C8 1.398(8) . ?
C7 C14 1.516(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(8) . ?
C9 C18 1.497(8) . ?
C10 C11 1.544(8) . ?
C10 C12 1.540(10) . ?
C10 C13 1.535(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.475(10) . ?
C14 C16 1.546(11) . ?
C14 C17 1.508(9) . ?
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 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.496(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.534(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.534(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.524(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.546(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.545(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.514(8) . ?
C32 C33 1.378(8) . ?
C32 C37 1.405(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.395(9) . ?
C34 C35 1.399(9) . ?
C34 C38 1.523(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.411(9) . ?
C36 C37 1.415(8) . ?
C36 C42 1.538(8) . ?
C38 C39 1.566(10) . ?
C38 C40 1.518(9) . ?
C38 C41 1.480(10) . ?
C38 C47 1.549(17) . ?
C38 C46 1.495(16) . ?
C38 C48 1.532(16) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.527(9) . ?
C42 C44 1.532(8) . ?
C42 C45 1.515(10) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N1 67.27(14) . . ?
O1 U1 N2 95.12(16) . . ?
O1 U1 C1 79.07(16) . 3_666 ?
O1 U1 C1 144.20(17) . . ?
O1 U1 C2 119.66(17) . . ?
O1 U1 C2 97.14(16) . 3_666 ?
O1 U1 C3 88.66(17) . . ?
O1 U1 C3 128.88(15) . 3_666 ?
O2 U1 O1 113.45(14) . . ?
O2 U1 N1 74.35(14) . . ?
O2 U1 N2 113.51(14) . . ?
O2 U1 C1 130.25(18) . 3_666 ?
O2 U1 C1 85.34(16) . . ?
O2 U1 C2 77.58(16) . . ?
O2 U1 C2 141.06(17) . 3_666 ?
O2 U1 C3 98.70(17) . . ?
O2 U1 C3 114.13(16) . 3_666 ?
N2 U1 N1 63.47(14) . . ?
C1 U1 N1 148.43(15) . . ?
C1 U1 N1 145.13(16) 3_666 . ?
C1 U1 N2 112.83(17) 3_666 . ?
C1 U1 N2 105.11(17) . . ?
C1 U1 C1 66.0(2) . 3_666 ?
C1 U1 C2 31.80(18) . . ?
C1 U1 C2 56.32(17) . 3_666 ?
C1 U1 C2 31.58(17) 3_666 3_666 ?
C1 U1 C3 56.21(17) 3_666 3_666 ?
C1 U1 C3 31.20(18) . 3_666 ?
C2 U1 N1 151.13(15) . . ?
C2 U1 N1 142.65(16) 3_666 . ?
C2 U1 N2 136.59(17) . . ?
C2 U1 N2 85.69(16) 3_666 . ?
C2 U1 C1 56.37(18) . 3_666 ?
C2 U1 C2 66.2(2) . 3_666 ?
C2 U1 C3 31.79(17) 3_666 3_666 ?
C2 U1 C3 56.09(19) . 3_666 ?
C3 U1 N1 148.33(15) . . ?
C3 U1 N1 144.52(16) 3_666 . ?
C3 U1 N2 142.59(16) . . ?
C3 U1 N2 82.40(17) 3_666 . ?
C3 U1 C1 57.48(18) . . ?
C3 U1 C1 31.69(18) . 3_666 ?
C3 U1 C2 56.94(17) . 3_666 ?
C3 U1 C2 32.50(17) . . ?
C3 U1 C3 66.8(2) . 3_666 ?
C4 O1 U1 150.5(4) . . ?
C37 O2 U1 150.4(4) . . ?
C18 N1 U1 108.5(3) . . ?
C19 N1 U1 110.1(3) . . ?
C19 N1 C18 110.9(5) . . ?
C19 N1 C30 111.7(5) . . ?
C30 N1 U1 105.8(3) . . ?
C30 N1 C18 109.7(4) . . ?
C20 N2 U1 102.6(3) . . ?
C21 N2 U1 112.7(4) . . ?
C21 N2 C20 106.3(5) . . ?
C21 N2 C22 109.0(5) . . ?
C22 N2 U1 116.0(4) . . ?
C22 N2 C20 109.6(5) . . ?
C25 N3 C24 112.7(4) . . ?
C31 N3 C24 108.9(5) . . ?
C31 N3 C25 110.9(5) . . ?
C27 N4 C26 110.5(6) . . ?
C27 N4 C28 112.0(6) . . ?
C28 N4 C26 112.1(6) . . ?
U1 C1 U1 114.0(2) . 3_666 ?
U1 C1 H1 125.4 3_666 . ?
U1 C1 H1 120.6 . . ?
C2 C1 U1 74.4(3) . 3_666 ?
C2 C1 U1 74.1(3) . . ?
C2 C1 H1 119.4 . . ?
C3 C1 U1 76.9(4) 3_666 . ?
C3 C1 U1 72.6(3) 3_666 3_666 ?
C3 C1 H1 119.4 3_666 . ?
C3 C1 C2 121.3(5) 3_666 . ?
U1 C2 U1 113.8(2) . 3_666 ?
U1 C2 H2 124.8 . . ?
U1 C2 H2 121.4 3_666 . ?
C1 C2 U1 74.0(3) . 3_666 ?
C1 C2 U1 74.1(3) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0(5) . . ?
C3 C2 U1 75.8(3) . 3_666 ?
C3 C2 U1 72.7(4) . . ?
C3 C2 H2 120.0 . . ?
U1 C3 U1 113.2(2) . 3_666 ?
U1 C3 H3 126.9 3_666 . ?
U1 C3 H3 119.9 . . ?
C1 C3 U1 75.8(4) 3_666 . ?
C1 C3 U1 71.9(3) 3_666 3_666 ?
C1 C3 C2 118.6(5) 3_666 . ?
C1 C3 H3 120.7 3_666 . ?
C2 C3 U1 72.4(3) . 3_666 ?
C2 C3 U1 74.8(3) . . ?
C2 C3 H3 120.7 . . ?
O1 C4 C5 122.8(5) . . ?
O1 C4 C9 118.9(5) . . ?
C9 C4 C5 118.3(5) . . ?
C4 C5 C10 120.9(5) . . ?
C6 C5 C4 118.1(5) . . ?
C6 C5 C10 121.1(5) . . ?
C5 C6 H6 117.8 . . ?
C5 C6 C7 124.4(6) . . ?
C7 C6 H6 117.8 . . ?
C6 C7 C14 121.3(5) . . ?
C8 C7 C6 116.0(6) . . ?
C8 C7 C14 122.6(6) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 C7 122.0(6) . . ?
C9 C8 H8 119.0 . . ?
C4 C9 C18 118.5(5) . . ?
C8 C9 C4 121.1(5) . . ?
C8 C9 C18 120.3(5) . . ?
C5 C10 C11 108.2(5) . . ?
C5 C10 C12 110.5(5) . . ?
C5 C10 C13 112.7(6) . . ?
C12 C10 C11 111.5(5) . . ?
C13 C10 C11 106.8(5) . . ?
C13 C10 C12 107.1(5) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 C14 C16 109.6(6) . . ?
C15 C14 C7 114.5(6) . . ?
C15 C14 C16 109.0(8) . . ?
C15 C14 C17 107.3(6) . . ?
C17 C14 C7 110.6(6) . . ?
C17 C14 C16 105.4(7) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 C9 115.2(5) . . ?
N1 C18 H18A 108.5 . . ?
N1 C18 H18B 108.5 . . ?
C9 C18 H18A 108.5 . . ?
C9 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
N1 C19 H19A 108.7 . . ?
N1 C19 H19B 108.7 . . ?
N1 C19 C20 114.0(5) . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
N2 C20 H20A 108.8 . . ?
N2 C20 H20B 108.8 . . ?
C19 C20 N2 113.7(5) . . ?
C19 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 108.9 . . ?
N2 C22 H22B 108.9 . . ?
N2 C22 C23 113.4(5) . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C22 C23 H23A 109.9 . . ?
C22 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 C22 109.1(5) . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
N3 C24 C23 111.4(4) . . ?
N3 C24 H24A 109.4 . . ?
N3 C24 H24B 109.4 . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N3 C25 H25A 108.7 . . ?
N3 C25 H25B 108.7 . . ?
N3 C25 C26 114.4(5) . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
N4 C26 C25 114.4(5) . . ?
N4 C26 H26A 108.7 . . ?
N4 C26 H26B 108.7 . . ?
C25 C26 H26A 108.7 . . ?
C25 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
N4 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
N4 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
N4 C28 C29 110.7(5) . . ?
H28A C28 H28B 108.1 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C28 C29 H29A 110.7 . . ?
C28 C29 H29B 110.7 . . ?
H29A C29 H29B 108.8 . . ?
C30 C29 C28 105.5(5) . . ?
C30 C29 H29A 110.7 . . ?
C30 C29 H29B 110.7 . . ?
N1 C30 C29 117.7(5) . . ?
N1 C30 H30A 107.9 . . ?
N1 C30 H30B 107.9 . . ?
C29 C30 H30A 107.9 . . ?
C29 C30 H30B 107.9 . . ?
H30A C30 H30B 107.2 . . ?
N3 C31 H31A 107.7 . . ?
N3 C31 H31B 107.7 . . ?
N3 C31 C32 118.5(5) . . ?
H31A C31 H31B 107.1 . . ?
C32 C31 H31A 107.7 . . ?
C32 C31 H31B 107.7 . . ?
C33 C32 C31 117.8(5) . . ?
C33 C32 C37 119.5(5) . . ?
C37 C32 C31 122.4(5) . . ?
C32 C33 H33 118.3 . . ?
C32 C33 C34 123.5(6) . . ?
C34 C33 H33 118.3 . . ?
C33 C34 C35 115.9(6) . . ?
C33 C34 C38 120.5(6) . . ?
C35 C34 C38 123.6(6) . . ?
C34 C35 H35 118.3 . . ?
C34 C35 C36 123.5(6) . . ?
C36 C35 H35 118.3 . . ?
C35 C36 C37 117.6(5) . . ?
C35 C36 C42 118.3(5) . . ?
C37 C36 C42 124.1(6) . . ?
O2 C37 C32 119.5(5) . . ?
O2 C37 C36 120.7(5) . . ?
C32 C37 C36 119.8(5) . . ?
C34 C38 C39 109.1(7) . . ?
C34 C38 C47 96.4(17) . . ?
C34 C38 C48 110(2) . . ?
C40 C38 C34 113.4(6) . . ?
C40 C38 C39 103.5(6) . . ?
C41 C38 C34 112.1(7) . . ?
C41 C38 C39 107.7(7) . . ?
C41 C38 C40 110.5(7) . . ?
C46 C38 C34 113(2) . . ?
C46 C38 C47 112.7(15) . . ?
C46 C38 C48 114.1(14) . . ?
C48 C38 C47 109.6(14) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C36 113.1(5) . . ?
C43 C42 C44 107.0(5) . . ?
C44 C42 C36 111.2(5) . . ?
C45 C42 C36 108.7(5) . . ?
C45 C42 C43 107.4(6) . . ?
C45 C42 C44 109.3(6) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C38 C47 H47A 109.5 . . ?
C38 C47 H47B 109.5 . . ?
C38 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C38 C46 H46A 109.5 . . ?
C38 C46 H46B 109.5 . . ?
C38 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C38 C48 H48A 109.5 . . ?
C38 C48 H48B 109.5 . . ?
C38 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C4 C5 133.9(6) . . . . ?
U1 O1 C4 C9 -44.7(10) . . . . ?
U1 O2 C37 C32 62.3(10) . . . . ?
U1 O2 C37 C36 -118.6(7) . . . . ?
U1 N1 C18 C9 -70.5(6) . . . . ?
U1 N1 C19 C20 9.1(6) . . . . ?
U1 N1 C30 C29 172.9(5) . . . . ?
U1 N2 C20 C19 68.9(5) . . . . ?
U1 N2 C22 C23 61.8(6) . . . . ?
U1 C1 C2 U1 121.22(16) . . . 3_666 ?
U1 C1 C2 U1 -121.22(16) 3_666 . . . ?
U1 C1 C2 C3 58.6(5) . . . . ?
U1 C1 C2 C3 -62.6(5) 3_666 . . . ?
U1 C2 C3 U1 120.96(16) . . . 3_666 ?
U1 C2 C3 U1 -120.96(16) 3_666 . . . ?
U1 C2 C3 C1 -57.0(5) 3_666 . . 3_666 ?
U1 C2 C3 C1 64.0(5) . . . 3_666 ?
O1 C4 C5 C6 -176.0(5) . . . . ?
O1 C4 C5 C10 3.3(8) . . . . ?
O1 C4 C9 C8 176.0(5) . . . . ?
O1 C4 C9 C18 -3.9(8) . . . . ?
N1 C19 C20 N2 -54.4(7) . . . . ?
N2 C22 C23 C24 -143.5(5) . . . . ?
N3 C25 C26 N4 49.3(8) . . . . ?
N3 C31 C32 C33 -108.6(6) . . . . ?
N3 C31 C32 C37 78.0(7) . . . . ?
N4 C28 C29 C30 68.3(8) . . . . ?
C1 C2 C3 U1 61.7(5) . . . 3_666 ?
C1 C2 C3 U1 -59.3(5) . . . . ?
C1 C2 C3 C1 4.7(9) . . . 3_666 ?
C3 C1 C2 U1 -63.4(5) 3_666 . . . ?
C3 C1 C2 U1 57.8(5) 3_666 . . 3_666 ?
C3 C1 C2 C3 -4.8(10) 3_666 . . . ?
C4 C5 C6 C7 -1.0(9) . . . . ?
C4 C5 C10 C11 -67.2(7) . . . . ?
C4 C5 C10 C12 55.2(7) . . . . ?
C4 C5 C10 C13 174.9(5) . . . . ?
C4 C9 C18 N1 60.9(7) . . . . ?
C5 C4 C9 C8 -2.6(8) . . . . ?
C5 C4 C9 C18 177.5(5) . . . . ?
C5 C6 C7 C8 -0.8(9) . . . . ?
C5 C6 C7 C14 175.9(6) . . . . ?
C6 C5 C10 C11 112.1(6) . . . . ?
C6 C5 C10 C12 -125.6(6) . . . . ?
C6 C5 C10 C13 -5.8(8) . . . . ?
C6 C7 C8 C9 0.9(8) . . . . ?
C6 C7 C14 C15 173.9(7) . . . . ?
C6 C7 C14 C16 -63.2(8) . . . . ?
C6 C7 C14 C17 52.5(9) . . . . ?
C7 C8 C9 C4 0.8(9) . . . . ?
C7 C8 C9 C18 -179.3(5) . . . . ?
C8 C7 C14 C15 -9.6(9) . . . . ?
C8 C7 C14 C16 113.2(8) . . . . ?
C8 C7 C14 C17 -131.0(7) . . . . ?
C8 C9 C18 N1 -119.0(6) . . . . ?
C9 C4 C5 C6 2.7(8) . . . . ?
C9 C4 C5 C10 -178.1(5) . . . . ?
C10 C5 C6 C7 179.7(6) . . . . ?
C14 C7 C8 C9 -175.8(6) . . . . ?
C18 N1 C19 C20 -111.1(5) . . . . ?
C18 N1 C30 C29 -70.3(7) . . . . ?
C19 N1 C18 C9 50.5(7) . . . . ?
C19 N1 C30 C29 53.1(7) . . . . ?
C20 N2 C22 C23 177.4(5) . . . . ?
C21 N2 C20 C19 -172.6(5) . . . . ?
C21 N2 C22 C23 -66.7(7) . . . . ?
C22 N2 C20 C19 -55.0(7) . . . . ?
C22 C23 C24 N3 68.5(7) . . . . ?
C24 N3 C25 C26 58.1(7) . . . . ?
C24 N3 C31 C32 178.7(5) . . . . ?
C25 N3 C24 C23 -161.9(5) . . . . ?
C25 N3 C31 C32 54.2(6) . . . . ?
C26 N4 C28 C29 -147.9(6) . . . . ?
C27 N4 C26 C25 -160.9(6) . . . . ?
C27 N4 C28 C29 87.2(7) . . . . ?
C28 N4 C26 C25 73.4(7) . . . . ?
C28 C29 C30 N1 -153.2(6) . . . . ?
C30 N1 C18 C9 174.3(5) . . . . ?
C30 N1 C19 C20 126.3(5) . . . . ?
C31 N3 C24 C23 74.6(6) . . . . ?
C31 N3 C25 C26 -179.5(5) . . . . ?
C31 C32 C33 C34 -172.9(6) . . . . ?
C31 C32 C37 O2 -3.8(9) . . . . ?
C31 C32 C37 C36 177.1(5) . . . . ?
C32 C33 C34 C35 -3.6(10) . . . . ?
C32 C33 C34 C38 177.1(6) . . . . ?
C33 C32 C37 O2 -177.1(5) . . . . ?
C33 C32 C37 C36 3.9(9) . . . . ?
C33 C34 C35 C36 2.1(10) . . . . ?
C33 C34 C38 C39 57.2(9) . . . . ?
C33 C34 C38 C40 172.0(7) . . . . ?
C33 C34 C38 C41 -62.0(10) . . . . ?
C33 C34 C38 C47 -118.3(16) . . . . ?
C33 C34 C38 C46 123.8(18) . . . . ?
C33 C34 C38 C48 -4.7(18) . . . . ?
C34 C35 C36 C37 2.1(10) . . . . ?
C34 C35 C36 C42 -177.9(6) . . . . ?
C35 C34 C38 C39 -122.1(8) . . . . ?
C35 C34 C38 C40 -7.3(11) . . . . ?
C35 C34 C38 C41 118.7(8) . . . . ?
C35 C34 C38 C47 62.4(16) . . . . ?
C35 C34 C38 C46 -55.5(18) . . . . ?
C35 C34 C38 C48 176.0(18) . . . . ?
C35 C36 C37 O2 175.8(5) . . . . ?
C35 C36 C37 C32 -5.1(9) . . . . ?
C35 C36 C42 C43 0.8(9) . . . . ?
C35 C36 C42 C44 -119.6(6) . . . . ?
C35 C36 C42 C45 119.9(7) . . . . ?
C37 C32 C33 C34 0.7(9) . . . . ?
C37 C36 C42 C43 -179.2(6) . . . . ?
C37 C36 C42 C44 60.4(8) . . . . ?
C37 C36 C42 C45 -60.0(7) . . . . ?
C38 C34 C35 C36 -178.6(7) . . . . ?
C42 C36 C37 O2 -4.2(9) . . . . ?
C42 C36 C37 C32 174.9(5) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 350 electrons were 
found in a volume of 1556Å³ in 1 void per unit cell. 
This is consistent with the presence of 
4[C7H8] per formula unit 
which account for 400 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.463 0.000 0.500 778.2 174.8 '3.6 C7H8'
2 -0.739 0.500 0.000 778.2 174.8 '3.6 C7H8'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.940
_oxdiff_exptl_absorpt_empirical_full_min 0.473
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               4
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 0.5072 47993 20468 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.1763 0 5052 nmt 0.9942 0.0075 -0.0152 -0.0474 1.0005 -0.0287 0.1071 0.0440
1.0033
3 0.0887 0 2016 nmt 0.0191 0.2846 0.3000 -0.6345 -0.7634 0.4239 2.5496 -0.4030
0.1805
4 0.2278 0 16577 nmt -1.0000 -0.0137 -0.0008 -0.0569 1.0006 -0.0020 0.0054
0.0000 -0.9998

_twin_special_details            
;
Component 2 rotated by 3.2647° 
around [0.33 -0.78 -0.54] (reciprocal) or [0.86 -0.48 -0.17] (direct)
Component 3 rotated by -141.4619° 
around [0.32 0.11 0.94] (reciprocal) or [0.93 0.06 0.37] (direct)
Component 4 rotated by -179.8860° 
around [-0.01 1.00 -0.00] (reciprocal) or [-0.03 1.00 -0.00] (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_ks820
_database_code_depnum_ccdc_archive 'CCDC 2411216'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;EPFL
Switzerland
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H97 N4 O6 Si U, 0.5(C6 H14)'
_chemical_formula_sum            'C57 H104 N4 O6 Si U'
_chemical_formula_weight         1207.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C57 H104 N4 O6 Si1 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'
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                   11.2069(3)
_cell_length_b                   14.7053(5)
_cell_length_c                   18.7776(6)
_cell_angle_alpha                84.700(3)
_cell_angle_beta                 80.165(2)
_cell_angle_gamma                82.473(2)
_cell_volume                     3015.04(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11609
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      69.7940
_cell_measurement_theta_min      3.6700
_shelx_estimated_absorpt_T_max   0.518
_shelx_estimated_absorpt_T_min   0.254
_exptl_absorpt_coefficient_mu    8.138
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.108a (Rigaku Oxford Diffraction, 2024)
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 red'
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 2 0.0251
-1 1 -2 0.0682
1 0 -2 0.1135
-1 0 2 0.1016
2 1 -1 0.1187
-1 -1 -2 0.0496
-2 -9 -2 0.0377
-1 -2 0 0.0530
0 -2 -1 0.0566
0 1 0 0.0733
1 9 -1 0.0509
1 2 1 0.0633
3 8 6 0.0623
4 8 2 0.0633
2 9 4 0.0558

_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.093
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0002 -0.9996 1.9999 -0.1805 0.1511 0.0435
-1.0002 0.9996 -1.9999 0.1805 -0.1511 -0.0435
1.0000 0.0002 -2.0000 0.0507 -0.0542 0.2228
-1.0000 -0.0002 2.0000 -0.0507 0.0542 -0.2228
1.9999 1.0004 -1.0000 0.1030 0.0986 0.2804
-0.9998 -1.0001 -1.9999 -0.0194 -0.2117 -0.0084
-2.2058 -9.3638 -2.4236 -0.8238 -0.5667 0.0091
-0.9997 -2.0000 0.0000 -0.1850 -0.1242 -0.0893
0.0004 -1.9997 -1.0000 -0.1672 -0.1195 0.0843
-0.0002 0.9999 -0.0000 0.1000 0.0303 -0.0176
1.2391 9.3268 -1.3133 0.9572 0.2840 0.0552
0.9997 2.0000 0.9999 0.1522 0.1831 0.0400
3.1646 8.4283 5.7128 0.6080 0.7931 -0.0354
4.2069 8.4408 1.6586 0.7267 0.6210 0.2936
2.3727 9.1731 3.7381 0.7592 0.6490 -0.0497

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13062
_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         72.371
_diffrn_reflns_theta_min         3.039
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_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    -62.00 -36.00   1.00    2.50    --  -43.01  72.00-175.00   26
  2  ω    119.00 162.00   1.00   10.00    --  103.18  72.00-175.00   43
  3  ω    106.00 133.00   1.00   10.00    --  103.18 -72.00  54.00   27
  4  ω     41.00  67.00   1.00   10.00    --  103.18 -72.00  54.00   26
  5  ω   -117.00 -19.00   1.00    2.50    --  -43.01 -37.00 150.00   98
  6  ω      6.00  31.00   1.00    2.50    --  -43.01  72.00-175.00   25
  7  ω    -84.00 -12.00   1.00    2.50    --  -43.01 125.00 -90.00   72
  8  ω    -30.00  -5.00   1.00    2.50    --   43.01 -37.00 -60.00   25
  9  ω     16.00 115.00   1.00    2.50    --   43.01  57.00 -90.00   99
 10  ω    -14.00  71.00   1.00    2.50    --   43.01 -72.00  54.00   85
 11  ω     39.00  66.00   1.00    2.50    --   43.01 -37.00 -60.00   27
 12  ω     77.00 109.00   1.00   10.00    --  103.18-111.00 -30.00   32
 13  ω     51.00 109.00   1.00   10.00    --  103.18-111.00-120.00   58
 14  ω     39.00 111.00   1.00   10.00    --  103.18 -61.00-150.00   72
 15  ω     31.00 128.00   1.00   10.00    --  103.18 -45.00 -90.00   97
 16  ω     68.00 106.00   1.00   10.00    --  103.18-111.00 150.00   38
 17  ω     32.00 126.00   1.00   10.00    --  103.18 -45.00  60.00   94
 18  ω    125.00 151.00   1.00   10.00    --  103.18 111.00  60.00   26
 19  ω     70.00  96.00   1.00   10.00    --  103.18-111.00  30.00   26
 20  ω     31.00 109.00   1.00   10.00    --  103.18-111.00  90.00   78
 21  ω    135.00 162.00   1.00   10.00    --  103.18  30.00  30.00   27
 22  ω    104.00 130.00   1.00   10.00    --  103.18  30.00  30.00   26
 23  ω     27.00 131.00   1.00   10.00    --  103.18 -30.00 150.00  104
 24  ω     51.00 178.00   1.00   10.00    --  103.18  15.00 150.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0149484000
_diffrn_orient_matrix_UB_12      0.0999960000
_diffrn_orient_matrix_UB_13      -0.0328127000
_diffrn_orient_matrix_UB_21      0.0636097000
_diffrn_orient_matrix_UB_22      0.0302969000
_diffrn_orient_matrix_UB_23      0.0588968000
_diffrn_orient_matrix_UB_31      0.1243677000
_diffrn_orient_matrix_UB_32      -0.0175312000
_diffrn_orient_matrix_UB_33      -0.0492292000
_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                10759
_reflns_number_total             13062
_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 1.171.43.108a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.108a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         3.762
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         13062
_refine_ls_number_restraints     190
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0434
_refine_ls_restrained_S_all      0.970
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0567P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1023
_refine_special_details          
;
 Refined as a 4-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.522(3)
 0.2115(18) 0.1421(17) 0.1245(17)
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
 C58-C59 = C59-C60 = C60-C61 = C61-C62 = C62-C63
 1.52 with sigma of 0.02
 C58-C60 = C61-C63
 2.53 with sigma of 0.04
 C59-C61 = C60-C62
 2.54 with sigma of 0.04
 C58-C59 \\sim C59-C60 \\sim C60-C61 \\sim C61-C62 \\sim C62-C63
 with sigma of 0.02
 C58-C60 \\sim C60-C62 \\sim C59-C61 \\sim C61-C63
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=1-FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
 Fixed Sof: C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5)
 H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C27(H27A,H27B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C29(H29), C31(H31)
7.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C63(H63A,H63B,H63C)
;
_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 0.36281(2) 0.62664(2) 0.72712(2) 0.02985(7) Uani 1 1 d . . . . .
Si1 Si 0.11029(15) 0.73619(11) 0.86775(9) 0.0317(3) Uani 1 1 d . . . . .
O1 O 0.2919(4) 0.4847(3) 0.7515(2) 0.0352(9) Uani 1 1 d . . . . .
O2 O 0.2709(4) 0.6809(3) 0.6316(3) 0.0440(11) Uani 1 1 d . . . . .
O3 O 0.2060(4) 0.6898(3) 0.8054(2) 0.0354(9) Uani 1 1 d . . . . .
O4 O 0.0820(4) 0.8477(3) 0.8561(2) 0.0394(10) Uani 1 1 d . . . . .
O5 O -0.0231(4) 0.6997(3) 0.8816(2) 0.0378(10) Uani 1 1 d . . . . .
O6 O 0.1746(4) 0.7182(3) 0.9408(2) 0.0391(10) Uani 1 1 d . . . . .
N1 N 0.4999(5) 0.5309(4) 0.8294(3) 0.0404(13) Uani 1 1 d . . . . .
N2 N 0.5587(6) 0.5159(5) 0.6402(4) 0.0554(16) Uani 1 1 d . . . . .
N3 N 0.5314(5) 0.7233(5) 0.6166(3) 0.0469(14) Uani 1 1 d . . . . .
N4 N 0.4740(5) 0.7454(4) 0.7962(3) 0.0439(13) Uani 1 1 d . . . . .
C1 C 0.6042(6) 0.4577(5) 0.8134(5) 0.0528(19) Uani 1 1 d . . . . .
H1A H 0.571786 0.397797 0.816319 0.063 Uiso 1 1 calc R U . . .
H1B H 0.656357 0.454666 0.851348 0.063 Uiso 1 1 calc R U . . .
C2 C 0.6838(7) 0.4720(6) 0.7388(5) 0.062(2) Uani 1 1 d . . . . .
H2A H 0.695548 0.537866 0.729582 0.074 Uiso 1 1 calc R U . . .
H2B H 0.765001 0.436563 0.739782 0.074 Uiso 1 1 calc R U . . .
C3 C 0.6311(9) 0.4434(6) 0.6782(6) 0.069(2) Uani 1 1 d . . . . .
H3A H 0.698749 0.416217 0.642507 0.083 Uiso 1 1 calc R U . . .
H3B H 0.579075 0.394440 0.697516 0.083 Uiso 1 1 calc R U . . .
C4 C 0.6383(7) 0.5699(7) 0.5872(5) 0.060(2) Uani 1 1 d . . . . .
H4A H 0.672075 0.532780 0.545429 0.072 Uiso 1 1 calc R U . . .
H4B H 0.707500 0.582762 0.609673 0.072 Uiso 1 1 calc R U . . .
C5 C 0.5747(7) 0.6589(6) 0.5603(5) 0.059(2) Uani 1 1 d . . . . .
H5A H 0.631247 0.688301 0.521338 0.071 Uiso 1 1 calc R U . . .
H5B H 0.504188 0.646061 0.539047 0.071 Uiso 1 1 calc R U . . .
C6 C 0.6382(7) 0.7604(7) 0.6326(5) 0.062(2) Uani 1 1 d . . . . .
H6A H 0.672119 0.797534 0.588932 0.074 Uiso 1 1 calc R U . . .
H6B H 0.700634 0.708020 0.640690 0.074 Uiso 1 1 calc R U . . .
C7 C 0.6202(7) 0.8192(5) 0.6966(5) 0.055(2) Uani 1 1 d . . . . .
H7A H 0.693042 0.851768 0.693789 0.066 Uiso 1 1 calc R U . . .
H7B H 0.549313 0.866305 0.693204 0.066 Uiso 1 1 calc R U . . .
C8 C 0.5998(6) 0.7654(5) 0.7690(4) 0.0497(17) Uani 1 1 d . . . . .
H8A H 0.653289 0.706318 0.765623 0.060 Uiso 1 1 calc R U . . .
H8B H 0.626103 0.799977 0.805233 0.060 Uiso 1 1 calc R U . . .
C9 C 0.4684(7) 0.6943(5) 0.8677(4) 0.0490(17) Uani 1 1 d . . . . .
H9A H 0.382278 0.685968 0.886821 0.059 Uiso 1 1 calc R U . . .
H9B H 0.496828 0.731762 0.901190 0.059 Uiso 1 1 calc R U . . .
C10 C 0.5437(7) 0.6006(5) 0.8673(4) 0.0485(18) Uani 1 1 d . . . . .
H10A H 0.628389 0.608693 0.844368 0.058 Uiso 1 1 calc R U . . .
H10B H 0.546077 0.576649 0.918127 0.058 Uiso 1 1 calc R U . . .
C11 C 0.3937(6) 0.4923(4) 0.8779(4) 0.0385(14) Uani 1 1 d . . . . .
H11A H 0.321765 0.539425 0.879973 0.046 Uiso 1 1 calc R U . . .
H11B H 0.413645 0.480103 0.927504 0.046 Uiso 1 1 calc R U . . .
C12 C 0.3603(5) 0.4049(4) 0.8541(3) 0.0316(12) Uani 1 1 d . . . . .
C13 C 0.3844(6) 0.3236(4) 0.8958(3) 0.0379(14) Uani 1 1 d . . . . .
H13 H 0.425193 0.324706 0.936013 0.045 Uiso 1 1 calc R U . . .
C14 C 0.3508(6) 0.2408(4) 0.8807(4) 0.0382(14) Uani 1 1 d . . . . .
C15 C 0.2872(6) 0.2446(4) 0.8231(3) 0.0352(13) Uani 1 1 d . . . . .
H15 H 0.261465 0.189097 0.812437 0.042 Uiso 1 1 calc R U . . .
C16 C 0.2581(6) 0.3244(4) 0.7795(3) 0.0340(13) Uani 1 1 d . . . . .
C17 C 0.3011(5) 0.4072(4) 0.7932(3) 0.0311(12) Uani 1 1 d . . . . .
C18 C 0.3860(7) 0.1503(5) 0.9246(4) 0.0441(16) Uani 1 1 d . . . . .
C19 C 0.3425(11) 0.1611(6) 1.0043(5) 0.074(3) Uani 1 1 d . . . . .
H19A H 0.379652 0.211320 1.019539 0.111 Uiso 1 1 calc R U . . .
H19B H 0.366137 0.103781 1.032105 0.111 Uiso 1 1 calc R U . . .
H19C H 0.253555 0.175218 1.013047 0.111 Uiso 1 1 calc R U . . .
C20 C 0.5221(9) 0.1295(7) 0.9138(7) 0.083(3) Uani 1 1 d . . . . .
H20A H 0.552951 0.121382 0.862436 0.124 Uiso 1 1 calc R U . . .
H20B H 0.544856 0.073000 0.942756 0.124 Uiso 1 1 calc R U . . .
H20C H 0.557433 0.180613 0.929071 0.124 Uiso 1 1 calc R U . . .
C21 C 0.3311(11) 0.0705(5) 0.9045(6) 0.080(3) Uani 1 1 d . . . . .
H21A H 0.242109 0.084430 0.911333 0.121 Uiso 1 1 calc R U . . .
H21B H 0.353379 0.015539 0.935332 0.121 Uiso 1 1 calc R U . . .
H21C H 0.361899 0.059253 0.853608 0.121 Uiso 1 1 calc R U . . .
C22 C 0.1744(6) 0.3209(4) 0.7226(4) 0.0361(13) Uani 1 1 d . . . . .
C23 C 0.1292(8) 0.2264(5) 0.7245(5) 0.057(2) Uani 1 1 d . . . . .
H23A H 0.072201 0.228833 0.689950 0.086 Uiso 1 1 calc R U . . .
H23B H 0.087688 0.210084 0.773381 0.086 Uiso 1 1 calc R U . . .
H23C H 0.198802 0.180102 0.711250 0.086 Uiso 1 1 calc R U . . .
C24 C 0.2410(7) 0.3414(5) 0.6456(4) 0.0480(17) Uani 1 1 d . . . . .
H24A H 0.315725 0.298598 0.636639 0.072 Uiso 1 1 calc R U . . .
H24B H 0.261778 0.404650 0.640327 0.072 Uiso 1 1 calc R U . . .
H24C H 0.187911 0.334183 0.610569 0.072 Uiso 1 1 calc R U . . .
C25 C 0.0626(6) 0.3927(5) 0.7376(4) 0.0466(16) Uani 1 1 d . . . . .
H25A H 0.010329 0.391919 0.700829 0.070 Uiso 1 1 calc R U . . .
H25B H 0.089226 0.453845 0.735770 0.070 Uiso 1 1 calc R U . . .
H25C H 0.016742 0.378166 0.785690 0.070 Uiso 1 1 calc R U . . .
C26 C 0.4845(9) 0.4691(7) 0.6025(6) 0.077(3) Uani 1 1 d . . . . .
H26A H 0.427915 0.435874 0.637889 0.116 Uiso 1 1 calc R U . . .
H26B H 0.537299 0.425531 0.571071 0.116 Uiso 1 1 calc R U . . .
H26C H 0.438086 0.514437 0.572958 0.116 Uiso 1 1 calc R U . . .
C27 C 0.4465(7) 0.8017(5) 0.5905(4) 0.0524(19) Uani 1 1 d . . . . .
H27A H 0.495979 0.849878 0.565619 0.063 Uiso 1 1 calc R U . . .
H27B H 0.394280 0.828223 0.633346 0.063 Uiso 1 1 calc R U . . .
C28 C 0.3645(7) 0.7802(5) 0.5398(4) 0.0485(17) Uani 1 1 d . . . . .
C29 C 0.3771(7) 0.8197(5) 0.4697(5) 0.0543(19) Uani 1 1 d . . . . .
H29 H 0.440978 0.856931 0.453477 0.065 Uiso 1 1 calc R U . . .
C30 C 0.2992(7) 0.8069(5) 0.4223(4) 0.0496(17) Uani 1 1 d . . . . .
C31 C 0.2052(7) 0.7545(4) 0.4490(4) 0.0427(15) Uani 1 1 d . . . . .
H31 H 0.149592 0.746203 0.417834 0.051 Uiso 1 1 calc R U . . .
C32 C 0.1876(6) 0.7128(4) 0.5202(3) 0.0371(14) Uani 1 1 d . . . . .
C33 C 0.2728(6) 0.7234(5) 0.5653(4) 0.0402(14) Uani 1 1 d . . . . .
C34 C 0.3188(8) 0.8500(6) 0.3432(4) 0.056(2) Uani 1 1 d . . . . .
C35 C 0.2956(15) 0.9524(7) 0.3440(6) 0.104(4) Uani 1 1 d . . . . .
H35A H 0.211100 0.970148 0.366361 0.155 Uiso 1 1 calc R U . . .
H35B H 0.309160 0.980126 0.294223 0.155 Uiso 1 1 calc R U . . .
H35C H 0.351216 0.974021 0.371967 0.155 Uiso 1 1 calc R U . . .
C36 C 0.2308(13) 0.8202(8) 0.2986(5) 0.093(4) Uani 1 1 d . . . . .
H36A H 0.243633 0.753135 0.296937 0.139 Uiso 1 1 calc R U . . .
H36B H 0.245667 0.849056 0.249216 0.139 Uiso 1 1 calc R U . . .
H36C H 0.146742 0.839159 0.320962 0.139 Uiso 1 1 calc R U . . .
C37 C 0.4470(10) 0.8214(9) 0.3080(6) 0.090(3) Uani 1 1 d . . . . .
H37A H 0.504073 0.843889 0.334495 0.135 Uiso 1 1 calc R U . . .
H37B H 0.459165 0.847444 0.257726 0.135 Uiso 1 1 calc R U . . .
H37C H 0.461466 0.754159 0.308886 0.135 Uiso 1 1 calc R U . . .
C38 C 0.0762(6) 0.6609(5) 0.5484(4) 0.0433(15) Uani 1 1 d . . . . .
C39 C -0.0063(8) 0.6599(7) 0.4913(4) 0.060(2) Uani 1 1 d . . . . .
H39A H -0.029357 0.723100 0.472652 0.089 Uiso 1 1 calc R U . . .
H39B H -0.079843 0.632003 0.513381 0.089 Uiso 1 1 calc R U . . .
H39C H 0.037578 0.624078 0.451412 0.089 Uiso 1 1 calc R U . . .
C40 C 0.1158(7) 0.5613(5) 0.5723(5) 0.0529(18) Uani 1 1 d . . . . .
H40A H 0.165440 0.530593 0.531205 0.079 Uiso 1 1 calc R U . . .
H40B H 0.043578 0.529523 0.589677 0.079 Uiso 1 1 calc R U . . .
H40C H 0.163964 0.559591 0.611453 0.079 Uiso 1 1 calc R U . . .
C41 C 0.0012(7) 0.7087(6) 0.6129(4) 0.0530(18) Uani 1 1 d . . . . .
H41A H 0.051229 0.707781 0.651004 0.079 Uiso 1 1 calc R U . . .
H41B H -0.070261 0.676622 0.631564 0.079 Uiso 1 1 calc R U . . .
H41C H -0.025529 0.772591 0.597504 0.079 Uiso 1 1 calc R U . . .
C42 C 0.3952(7) 0.8334(5) 0.8064(5) 0.059(2) Uani 1 1 d . . . . .
H42A H 0.383763 0.863952 0.758995 0.089 Uiso 1 1 calc R U . . .
H42B H 0.433799 0.873041 0.832600 0.089 Uiso 1 1 calc R U . . .
H42C H 0.315879 0.821645 0.834338 0.089 Uiso 1 1 calc R U . . .
C43 C 0.0154(7) 0.9077(5) 0.8086(4) 0.0444(15) Uani 1 1 d . U . . .
C44 C 0.0123(15) 0.8650(9) 0.7394(7) 0.065(4) Uani 0.665(13) 1 d . U P A 1
H44A H -0.045452 0.903231 0.712228 0.098 Uiso 0.665(13) 1 calc R U P A 1
H44B H -0.013352 0.803362 0.750643 0.098 Uiso 0.665(13) 1 calc R U P A 1
H44C H 0.093858 0.860430 0.710100 0.098 Uiso 0.665(13) 1 calc R U P A 1
C45 C 0.0651(17) 0.9977(9) 0.7981(10) 0.077(4) Uani 0.665(13) 1 d . U P A 1
H45A H 0.149302 0.989768 0.772556 0.116 Uiso 0.665(13) 1 calc R U P A 1
H45B H 0.063635 1.021339 0.845420 0.116 Uiso 0.665(13) 1 calc R U P A 1
H45C H 0.015252 1.041482 0.769446 0.116 Uiso 0.665(13) 1 calc R U P A 1
C46 C -0.1190(12) 0.9233(10) 0.8510(8) 0.071(4) Uani 0.665(13) 1 d . U P A 1
H46A H -0.170418 0.963257 0.820819 0.107 Uiso 0.665(13) 1 calc R U P A 1
H46B H -0.118796 0.952407 0.895906 0.107 Uiso 0.665(13) 1 calc R U P A 1
H46C H -0.151302 0.863987 0.862784 0.107 Uiso 0.665(13) 1 calc R U P A 1
C47 C -0.088(2) 0.8688(17) 0.7877(15) 0.059(6) Uani 0.335(13) 1 d . U P A 2
H47A H -0.128099 0.913645 0.754916 0.088 Uiso 0.335(13) 1 calc R U P A 2
H47B H -0.146090 0.854673 0.831178 0.088 Uiso 0.335(13) 1 calc R U P A 2
H47C H -0.057208 0.812402 0.763129 0.088 Uiso 0.335(13) 1 calc R U P A 2
C48 C 0.111(3) 0.921(2) 0.7424(16) 0.087(9) Uani 0.335(13) 1 d . U P A 2
H48A H 0.153389 0.861057 0.728420 0.131 Uiso 0.335(13) 1 calc R U P A 2
H48B H 0.170552 0.958916 0.753614 0.131 Uiso 0.335(13) 1 calc R U P A 2
H48C H 0.072336 0.951838 0.702314 0.131 Uiso 0.335(13) 1 calc R U P A 2
C49 C -0.016(3) 0.9910(17) 0.8410(19) 0.074(7) Uani 0.335(13) 1 d . U P A 2
H49A H 0.020739 1.039924 0.809029 0.111 Uiso 0.335(13) 1 calc R U P A 2
H49B H 0.013983 0.986007 0.887379 0.111 Uiso 0.335(13) 1 calc R U P A 2
H49C H -0.104971 1.005644 0.849224 0.111 Uiso 0.335(13) 1 calc R U P A 2
C50 C -0.0585(6) 0.6096(4) 0.8817(4) 0.0369(14) Uani 1 1 d . . . . .
C51 C -0.0881(7) 0.6006(5) 0.8070(4) 0.0473(16) Uani 1 1 d . . . . .
H51A H -0.014089 0.603465 0.770941 0.071 Uiso 1 1 calc R U . . .
H51B H -0.149961 0.650921 0.795660 0.071 Uiso 1 1 calc R U . . .
H51C H -0.119399 0.541591 0.806120 0.071 Uiso 1 1 calc R U . . .
C52 C 0.0425(6) 0.5349(5) 0.8993(4) 0.0403(14) Uani 1 1 d . . . . .
H52A H 0.012348 0.474650 0.904163 0.060 Uiso 1 1 calc R U . . .
H52B H 0.067410 0.546379 0.944947 0.060 Uiso 1 1 calc R U . . .
H52C H 0.112646 0.535721 0.860244 0.060 Uiso 1 1 calc R U . . .
C53 C -0.1721(7) 0.6056(5) 0.9386(4) 0.0506(18) Uani 1 1 d . . . . .
H53A H -0.233714 0.656581 0.928096 0.076 Uiso 1 1 calc R U . . .
H53B H -0.151318 0.610596 0.986568 0.076 Uiso 1 1 calc R U . . .
H53C H -0.204672 0.547072 0.937778 0.076 Uiso 1 1 calc R U . . .
C54 C 0.1453(7) 0.7587(5) 1.0097(4) 0.0435(15) Uani 1 1 d . . . . .
C55 C 0.1947(9) 0.8505(5) 1.0021(5) 0.064(2) Uani 1 1 d . . . . .
H55A H 0.151464 0.893109 0.969168 0.096 Uiso 1 1 calc R U . . .
H55B H 0.281963 0.842357 0.982372 0.096 Uiso 1 1 calc R U . . .
H55C H 0.182871 0.875577 1.049664 0.096 Uiso 1 1 calc R U . . .
C56 C 0.0098(8) 0.7696(7) 1.0361(5) 0.066(2) Uani 1 1 d . . . . .
H56A H -0.007050 0.795577 1.083448 0.099 Uiso 1 1 calc R U . . .
H56B H -0.020365 0.709339 1.040483 0.099 Uiso 1 1 calc R U . . .
H56C H -0.031328 0.810822 1.001405 0.099 Uiso 1 1 calc R U . . .
C57 C 0.2122(9) 0.6916(6) 1.0606(5) 0.063(2) Uani 1 1 d . . . . .
H57A H 0.299753 0.684749 1.041772 0.094 Uiso 1 1 calc R U . . .
H57B H 0.181541 0.631631 1.063923 0.094 Uiso 1 1 calc R U . . .
H57C H 0.198233 0.715196 1.108814 0.094 Uiso 1 1 calc R U . . .
C58 C -0.183(4) 0.970(3) 0.421(3) 0.202(16) Uani 0.5 1 d D U P B -1
H58A H -0.236192 1.025106 0.435750 0.303 Uiso 0.5 1 calc R U P B -1
H58B H -0.231766 0.919010 0.421463 0.303 Uiso 0.5 1 calc R U P B -1
H58C H -0.137831 0.981160 0.372254 0.303 Uiso 0.5 1 calc R U P B -1
C59 C -0.093(3) 0.944(2) 0.474(2) 0.133(9) Uani 0.5 1 d D U P B -1
H59A H -0.138018 0.925198 0.521937 0.160 Uiso 0.5 1 calc R U P B -1
H59B H -0.035558 0.889908 0.456947 0.160 Uiso 0.5 1 calc R U P B -1
C60 C -0.021(2) 1.0206(18) 0.4815(17) 0.108(7) Uani 0.5 1 d D U P B -1
H60A H -0.078400 1.072250 0.502226 0.130 Uiso 0.5 1 calc R U P B -1
H60B H 0.017496 1.042653 0.432670 0.130 Uiso 0.5 1 calc R U P B -1
C61 C 0.076(3) 0.9949(19) 0.5285(18) 0.114(7) Uani 0.5 1 d D U P B -1
H61A H 0.130582 0.940639 0.509873 0.137 Uiso 0.5 1 calc R U P B -1
H61B H 0.037389 0.977431 0.578405 0.137 Uiso 0.5 1 calc R U P B -1
C62 C 0.152(3) 1.072(2) 0.530(2) 0.150(10) Uani 0.5 1 d D U P B -1
H62A H 0.100140 1.120688 0.558682 0.180 Uiso 0.5 1 calc R U P B -1
H62B H 0.172893 1.099223 0.480195 0.180 Uiso 0.5 1 calc R U P B -1
C63 C 0.268(3) 1.047(3) 0.562(3) 0.189(15) Uani 0.5 1 d D U P B -1
H63A H 0.250778 1.013399 0.609281 0.283 Uiso 0.5 1 calc R U P B -1
H63B H 0.302818 1.103618 0.567919 0.283 Uiso 0.5 1 calc R U P B -1
H63C H 0.327301 1.008898 0.529257 0.283 Uiso 0.5 1 calc R U P B -1


_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 O1 2.309(4) . ?
U1 O2 2.251(4) . ?
U1 O3 2.248(4) . ?
U1 N1 2.824(5) . ?
U1 N2 2.909(6) . ?
U1 N3 2.953(6) . ?
U1 N4 2.797(6) . ?
Si1 O3 1.586(5) . ?
Si1 O4 1.631(5) . ?
Si1 O5 1.625(5) . ?
Si1 O6 1.641(5) . ?
O1 C17 1.324(7) . ?
O2 C33 1.338(8) . ?
O4 C43 1.428(8) . ?
O5 C50 1.433(7) . ?
O6 C54 1.443(8) . ?
N1 C1 1.491(9) . ?
N1 C10 1.479(8) . ?
N1 C11 1.509(9) . ?
N2 C3 1.461(12) . ?
N2 C4 1.467(11) . ?
N2 C26 1.453(11) . ?
N3 C5 1.461(11) . ?
N3 C6 1.465(9) . ?
N3 C27 1.498(10) . ?
N4 C8 1.473(9) . ?
N4 C9 1.472(10) . ?
N4 C42 1.476(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.540(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.483(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.494(13) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.515(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.506(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.518(11) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.511(8) . ?
C12 C13 1.390(9) . ?
C12 C17 1.412(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(9) . ?
C14 C15 1.385(9) . ?
C14 C18 1.542(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.403(9) . ?
C16 C17 1.427(8) . ?
C16 C22 1.545(8) . ?
C18 C19 1.508(12) . ?
C18 C20 1.498(12) . ?
C18 C21 1.501(10) . ?
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 C23 1.535(9) . ?
C22 C24 1.532(10) . ?
C22 C25 1.533(10) . ?
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 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.510(10) . ?
C28 C29 1.380(11) . ?
C28 C33 1.402(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.390(11) . ?
C30 C31 1.384(11) . ?
C30 C34 1.552(10) . ?
C31 H31 0.9500 . ?
C31 C32 1.413(9) . ?
C32 C33 1.411(9) . ?
C32 C38 1.540(10) . ?
C34 C35 1.495(13) . ?
C34 C36 1.526(14) . ?
C34 C37 1.498(14) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.532(10) . ?
C38 C40 1.524(10) . ?
C38 C41 1.524(10) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.501(15) . ?
C43 C45 1.488(15) . ?
C43 C46 1.578(15) . ?
C43 C47 1.48(2) . ?
C43 C48 1.51(3) . ?
C43 C49 1.40(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.516(9) . ?
C50 C52 1.528(9) . ?
C50 C53 1.520(10) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.511(11) . ?
C54 C56 1.507(11) . ?
C54 C57 1.525(11) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C58 C59 1.519(14) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.501(13) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.509(13) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.510(14) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.518(14) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N1 74.39(15) . . ?
O1 U1 N2 80.45(18) . . ?
O1 U1 N3 139.62(17) . . ?
O1 U1 N4 138.25(16) . . ?
O2 U1 O1 100.27(16) . . ?
O2 U1 N1 168.74(17) . . ?
O2 U1 N2 93.68(19) . . ?
O2 U1 N3 69.62(16) . . ?
O2 U1 N4 119.77(18) . . ?
O3 U1 O1 90.74(16) . . ?
O3 U1 O2 91.82(17) . . ?
O3 U1 N1 98.09(16) . . ?
O3 U1 N2 170.33(18) . . ?
O3 U1 N3 127.45(17) . . ?
O3 U1 N4 77.50(16) . . ?
N1 U1 N2 75.78(19) . . ?
N1 U1 N3 107.80(16) . . ?
N2 U1 N3 62.09(19) . . ?
N4 U1 N1 68.02(16) . . ?
N4 U1 N2 106.46(18) . . ?
N4 U1 N3 71.50(17) . . ?
O3 Si1 O4 114.8(2) . . ?
O3 Si1 O5 115.2(2) . . ?
O3 Si1 O6 105.7(2) . . ?
O4 Si1 O6 104.9(2) . . ?
O5 Si1 O4 104.6(2) . . ?
O5 Si1 O6 111.3(2) . . ?
C17 O1 U1 143.2(4) . . ?
C33 O2 U1 151.4(4) . . ?
Si1 O3 U1 171.4(3) . . ?
C43 O4 Si1 133.5(4) . . ?
C50 O5 Si1 131.5(4) . . ?
C54 O6 Si1 131.6(4) . . ?
C1 N1 U1 125.7(5) . . ?
C1 N1 C11 111.0(5) . . ?
C10 N1 U1 107.1(4) . . ?
C10 N1 C1 106.8(5) . . ?
C10 N1 C11 109.2(6) . . ?
C11 N1 U1 96.1(3) . . ?
C3 N2 U1 117.6(5) . . ?
C3 N2 C4 110.5(7) . . ?
C4 N2 U1 114.0(5) . . ?
C26 N2 U1 98.2(5) . . ?
C26 N2 C3 105.8(8) . . ?
C26 N2 C4 109.3(7) . . ?
C5 N3 U1 105.4(5) . . ?
C5 N3 C6 107.4(6) . . ?
C5 N3 C27 110.9(6) . . ?
C6 N3 U1 123.4(5) . . ?
C6 N3 C27 108.2(6) . . ?
C27 N3 U1 101.2(4) . . ?
C8 N4 U1 121.2(4) . . ?
C8 N4 C42 108.4(6) . . ?
C9 N4 U1 98.5(4) . . ?
C9 N4 C8 109.8(6) . . ?
C9 N4 C42 107.2(6) . . ?
C42 N4 U1 110.6(4) . . ?
N1 C1 H1A 108.6 . . ?
N1 C1 H1B 108.6 . . ?
N1 C1 C2 114.5(6) . . ?
H1A C1 H1B 107.6 . . ?
C2 C1 H1A 108.6 . . ?
C2 C1 H1B 108.6 . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C3 C2 C1 113.6(7) . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
N2 C3 C2 116.0(7) . . ?
N2 C3 H3A 108.3 . . ?
N2 C3 H3B 108.3 . . ?
C2 C3 H3A 108.3 . . ?
C2 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
N2 C4 H4A 108.9 . . ?
N2 C4 H4B 108.9 . . ?
N2 C4 C5 113.4(7) . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
N3 C5 C4 113.7(7) . . ?
N3 C5 H5A 108.8 . . ?
N3 C5 H5B 108.8 . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N3 C6 H6A 107.9 . . ?
N3 C6 H6B 107.9 . . ?
N3 C6 C7 117.8(7) . . ?
H6A C6 H6B 107.2 . . ?
C7 C6 H6A 107.9 . . ?
C7 C6 H6B 107.9 . . ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 C6 113.7(7) . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
N4 C8 C7 116.3(6) . . ?
N4 C8 H8A 108.2 . . ?
N4 C8 H8B 108.2 . . ?
C7 C8 H8A 108.2 . . ?
C7 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
N4 C9 H9A 108.7 . . ?
N4 C9 H9B 108.7 . . ?
N4 C9 C10 114.4(6) . . ?
H9A C9 H9B 107.6 . . ?
C10 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
N1 C10 C9 115.5(5) . . ?
N1 C10 H10A 108.4 . . ?
N1 C10 H10B 108.4 . . ?
C9 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
N1 C11 H11A 108.6 . . ?
N1 C11 H11B 108.6 . . ?
N1 C11 C12 114.5(6) . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C13 C12 C11 118.0(5) . . ?
C13 C12 C17 121.4(5) . . ?
C17 C12 C11 120.5(5) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 C12 122.2(6) . . ?
C14 C13 H13 118.9 . . ?
C13 C14 C18 121.3(6) . . ?
C15 C14 C13 115.9(6) . . ?
C15 C14 C18 122.8(6) . . ?
C14 C15 H15 117.5 . . ?
C14 C15 C16 124.9(6) . . ?
C16 C15 H15 117.5 . . ?
C15 C16 C17 117.8(5) . . ?
C15 C16 C22 119.2(5) . . ?
C17 C16 C22 122.8(5) . . ?
O1 C17 C12 118.3(5) . . ?
O1 C17 C16 124.2(5) . . ?
C12 C17 C16 117.4(5) . . ?
C19 C18 C14 109.7(6) . . ?
C20 C18 C14 109.2(6) . . ?
C20 C18 C19 107.6(8) . . ?
C20 C18 C21 109.7(8) . . ?
C21 C18 C14 112.8(6) . . ?
C21 C18 C19 107.6(7) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C16 112.5(5) . . ?
C24 C22 C16 111.3(5) . . ?
C24 C22 C23 107.0(6) . . ?
C24 C22 C25 108.8(6) . . ?
C25 C22 C16 109.2(5) . . ?
C25 C22 C23 108.0(6) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 H26A 109.5 . . ?
N2 C26 H26B 109.5 . . ?
N2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C27 H27A 108.1 . . ?
N3 C27 H27B 108.1 . . ?
N3 C27 C28 116.8(6) . . ?
H27A C27 H27B 107.3 . . ?
C28 C27 H27A 108.1 . . ?
C28 C27 H27B 108.1 . . ?
C29 C28 C27 119.7(7) . . ?
C29 C28 C33 120.6(7) . . ?
C33 C28 C27 119.6(7) . . ?
C28 C29 H29 119.0 . . ?
C28 C29 C30 122.1(7) . . ?
C30 C29 H29 119.0 . . ?
C29 C30 C34 120.5(7) . . ?
C31 C30 C29 117.0(7) . . ?
C31 C30 C34 122.5(7) . . ?
C30 C31 H31 118.3 . . ?
C30 C31 C32 123.3(7) . . ?
C32 C31 H31 118.3 . . ?
C31 C32 C38 120.8(6) . . ?
C33 C32 C31 117.8(6) . . ?
C33 C32 C38 121.4(6) . . ?
O2 C33 C28 118.1(6) . . ?
O2 C33 C32 122.9(6) . . ?
C28 C33 C32 119.0(6) . . ?
C35 C34 C30 109.1(8) . . ?
C35 C34 C36 107.3(9) . . ?
C35 C34 C37 110.4(9) . . ?
C36 C34 C30 111.9(7) . . ?
C37 C34 C30 109.2(7) . . ?
C37 C34 C36 108.9(9) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C32 112.8(6) . . ?
C40 C38 C32 110.9(6) . . ?
C40 C38 C39 107.5(6) . . ?
C41 C38 C32 108.3(6) . . ?
C41 C38 C39 108.1(6) . . ?
C41 C38 C40 109.2(6) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O4 C43 C44 112.1(7) . . ?
O4 C43 C45 108.5(8) . . ?
O4 C43 C46 105.2(7) . . ?
O4 C43 C47 114.4(10) . . ?
O4 C43 C48 102.3(12) . . ?
C44 C43 C46 108.5(10) . . ?
C45 C43 C44 114.3(10) . . ?
C45 C43 C46 107.8(11) . . ?
C47 C43 C48 110(2) . . ?
C49 C43 O4 106.4(12) . . ?
C49 C43 C47 114.8(18) . . ?
C49 C43 C48 109(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47A 109.5 . . ?
C43 C47 H47B 109.5 . . ?
C43 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C43 C49 H49A 109.5 . . ?
C43 C49 H49B 109.5 . . ?
C43 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O5 C50 C51 107.1(5) . . ?
O5 C50 C52 111.5(5) . . ?
O5 C50 C53 106.1(5) . . ?
C51 C50 C52 110.7(6) . . ?
C51 C50 C53 110.5(6) . . ?
C53 C50 C52 110.8(6) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O6 C54 C55 108.9(6) . . ?
O6 C54 C56 111.4(6) . . ?
O6 C54 C57 104.5(6) . . ?
C55 C54 C57 110.0(6) . . ?
C56 C54 C55 110.8(7) . . ?
C56 C54 C57 111.1(7) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C59 C58 H58A 109.5 . . ?
C59 C58 H58B 109.5 . . ?
C59 C58 H58C 109.5 . . ?
C58 C59 H59A 109.0 . . ?
C58 C59 H59B 109.0 . . ?
H59A C59 H59B 107.8 . . ?
C60 C59 C58 112.9(19) . . ?
C60 C59 H59A 109.0 . . ?
C60 C59 H59B 109.0 . . ?
C59 C60 H60A 108.7 . . ?
C59 C60 H60B 108.7 . . ?
C59 C60 C61 114.3(17) . . ?
H60A C60 H60B 107.6 . . ?
C61 C60 H60A 108.7 . . ?
C61 C60 H60B 108.7 . . ?
C60 C61 H61A 109.1 . . ?
C60 C61 H61B 109.1 . . ?
C60 C61 C62 112.5(18) . . ?
H61A C61 H61B 107.8 . . ?
C62 C61 H61A 109.1 . . ?
C62 C61 H61B 109.1 . . ?
C61 C62 H62A 108.2 . . ?
C61 C62 H62B 108.2 . . ?
C61 C62 C63 116(2) . . ?
H62A C62 H62B 107.3 . . ?
C63 C62 H62A 108.2 . . ?
C63 C62 H62B 108.2 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C17 C12 12.9(10) . . . . ?
U1 O1 C17 C16 -165.2(5) . . . . ?
U1 O2 C33 C28 -20.8(13) . . . . ?
U1 O2 C33 C32 158.5(7) . . . . ?
U1 N1 C1 C2 34.6(8) . . . . ?
U1 N1 C10 C9 24.4(7) . . . . ?
U1 N1 C11 C12 83.9(5) . . . . ?
U1 N2 C3 C2 -52.4(9) . . . . ?
U1 N2 C4 C5 -29.9(9) . . . . ?
U1 N3 C5 C4 -59.2(7) . . . . ?
U1 N3 C6 C7 -49.1(10) . . . . ?
U1 N3 C27 C28 -76.7(7) . . . . ?
U1 N4 C8 C7 67.3(8) . . . . ?
U1 N4 C9 C10 64.7(5) . . . . ?
Si1 O4 C43 C44 -27.4(11) . . . . ?
Si1 O4 C43 C45 -154.5(9) . . . . ?
Si1 O4 C43 C46 90.3(9) . . . . ?
Si1 O4 C43 C47 30.0(16) . . . . ?
Si1 O4 C43 C48 -88.3(18) . . . . ?
Si1 O4 C43 C49 157.8(17) . . . . ?
Si1 O5 C50 C51 -95.9(6) . . . . ?
Si1 O5 C50 C52 25.4(8) . . . . ?
Si1 O5 C50 C53 146.1(5) . . . . ?
Si1 O6 C54 C55 -80.4(8) . . . . ?
Si1 O6 C54 C56 42.1(9) . . . . ?
Si1 O6 C54 C57 162.1(5) . . . . ?
O3 Si1 O4 C43 73.1(7) . . . . ?
O3 Si1 O5 C50 39.4(6) . . . . ?
O3 Si1 O6 C54 165.3(5) . . . . ?
O4 Si1 O5 C50 166.4(5) . . . . ?
O4 Si1 O6 C54 43.7(6) . . . . ?
O5 Si1 O4 C43 -54.1(7) . . . . ?
O5 Si1 O6 C54 -68.9(6) . . . . ?
O6 Si1 O4 C43 -171.4(6) . . . . ?
O6 Si1 O5 C50 -80.9(6) . . . . ?
N1 C1 C2 C3 -80.1(9) . . . . ?
N1 C11 C12 C13 109.8(7) . . . . ?
N1 C11 C12 C17 -73.2(8) . . . . ?
N2 C4 C5 N3 64.3(9) . . . . ?
N3 C6 C7 C8 72.5(10) . . . . ?
N3 C27 C28 C29 -116.0(8) . . . . ?
N3 C27 C28 C33 66.8(10) . . . . ?
N4 C9 C10 N1 -68.1(8) . . . . ?
C1 N1 C10 C9 161.3(7) . . . . ?
C1 N1 C11 C12 -48.1(7) . . . . ?
C1 C2 C3 N2 94.4(9) . . . . ?
C3 N2 C4 C5 -165.0(8) . . . . ?
C4 N2 C3 C2 80.9(10) . . . . ?
C5 N3 C6 C7 -171.8(8) . . . . ?
C5 N3 C27 C28 34.8(9) . . . . ?
C6 N3 C5 C4 74.0(8) . . . . ?
C6 N3 C27 C28 152.4(7) . . . . ?
C6 C7 C8 N4 -83.5(9) . . . . ?
C8 N4 C9 C10 -63.0(7) . . . . ?
C9 N4 C8 C7 -178.9(6) . . . . ?
C10 N1 C1 C2 -91.9(8) . . . . ?
C10 N1 C11 C12 -165.6(5) . . . . ?
C11 N1 C1 C2 149.2(6) . . . . ?
C11 N1 C10 C9 -78.6(7) . . . . ?
C11 C12 C13 C14 176.3(6) . . . . ?
C11 C12 C17 O1 9.8(9) . . . . ?
C11 C12 C17 C16 -172.0(6) . . . . ?
C12 C13 C14 C15 -2.5(10) . . . . ?
C12 C13 C14 C18 175.9(7) . . . . ?
C13 C12 C17 O1 -173.3(6) . . . . ?
C13 C12 C17 C16 4.9(9) . . . . ?
C13 C14 C15 C16 1.5(10) . . . . ?
C13 C14 C18 C19 54.6(10) . . . . ?
C13 C14 C18 C20 -63.1(10) . . . . ?
C13 C14 C18 C21 174.6(8) . . . . ?
C14 C15 C16 C17 2.7(10) . . . . ?
C14 C15 C16 C22 -173.2(6) . . . . ?
C15 C14 C18 C19 -127.1(8) . . . . ?
C15 C14 C18 C20 115.2(9) . . . . ?
C15 C14 C18 C21 -7.1(11) . . . . ?
C15 C16 C17 O1 172.3(6) . . . . ?
C15 C16 C17 C12 -5.7(9) . . . . ?
C15 C16 C22 C23 2.3(9) . . . . ?
C15 C16 C22 C24 -117.7(7) . . . . ?
C15 C16 C22 C25 122.2(7) . . . . ?
C17 C12 C13 C14 -0.7(11) . . . . ?
C17 C16 C22 C23 -173.4(7) . . . . ?
C17 C16 C22 C24 66.6(8) . . . . ?
C17 C16 C22 C25 -53.5(8) . . . . ?
C18 C14 C15 C16 -176.9(7) . . . . ?
C22 C16 C17 O1 -11.9(10) . . . . ?
C22 C16 C17 C12 170.0(6) . . . . ?
C26 N2 C3 C2 -160.9(8) . . . . ?
C26 N2 C4 C5 78.9(9) . . . . ?
C27 N3 C5 C4 -168.0(6) . . . . ?
C27 N3 C6 C7 68.4(9) . . . . ?
C27 C28 C29 C30 -175.9(8) . . . . ?
C27 C28 C33 O2 -8.2(11) . . . . ?
C27 C28 C33 C32 172.4(7) . . . . ?
C28 C29 C30 C31 2.0(12) . . . . ?
C28 C29 C30 C34 -178.1(8) . . . . ?
C29 C28 C33 O2 174.6(7) . . . . ?
C29 C28 C33 C32 -4.8(11) . . . . ?
C29 C30 C31 C32 -1.7(11) . . . . ?
C29 C30 C34 C35 -66.7(11) . . . . ?
C29 C30 C34 C36 174.7(9) . . . . ?
C29 C30 C34 C37 54.0(11) . . . . ?
C30 C31 C32 C33 -1.8(10) . . . . ?
C30 C31 C32 C38 175.8(7) . . . . ?
C31 C30 C34 C35 113.3(10) . . . . ?
C31 C30 C34 C36 -5.3(12) . . . . ?
C31 C30 C34 C37 -126.0(9) . . . . ?
C31 C32 C33 O2 -174.4(6) . . . . ?
C31 C32 C33 C28 4.9(10) . . . . ?
C31 C32 C38 C39 0.8(9) . . . . ?
C31 C32 C38 C40 121.5(7) . . . . ?
C31 C32 C38 C41 -118.7(7) . . . . ?
C33 C28 C29 C30 1.2(13) . . . . ?
C33 C32 C38 C39 178.3(7) . . . . ?
C33 C32 C38 C40 -61.0(8) . . . . ?
C33 C32 C38 C41 58.8(8) . . . . ?
C34 C30 C31 C32 178.4(7) . . . . ?
C38 C32 C33 O2 8.0(10) . . . . ?
C38 C32 C33 C28 -172.6(7) . . . . ?
C42 N4 C8 C7 -62.1(9) . . . . ?
C42 N4 C9 C10 179.4(5) . . . . ?
C58 C59 C60 C61 -175(3) . . . . ?
C59 C60 C61 C62 176(4) . . . . ?
C60 C61 C62 C63 -167(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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.617
_oxdiff_exptl_absorpt_empirical_full_min 0.710
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               4
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 0.522(3) 21788 4296 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2115(18) 0 1856 nmt 1.0014 0.0245 -0.0234 -0.0524 0.9935 0.0665 0.0824
-0.1060 0.9951
3 0.1421(17) 0 1648 nmt 1.0003 -0.1809 0.0106 0.3319 0.9433 -0.0802 0.0198
0.0789 0.9901
4 0.1245(17) 0 1573 nmt -0.3602 0.1677 -0.5238 -0.2606 1.0014 0.0474 1.4337
0.2788 -0.6119

_twin_special_details            
;
Component 2 rotated by 5.8258° 
around [-0.66 -0.49 -0.57] (reciprocal) or [-0.92 -0.33 -0.20] (direct)
Component 3 rotated by 14.8060° 
around [0.24 0.06 0.97] (reciprocal) or [0.41 -0.05 0.91] (direct)
Component 4 rotated by -119.0580° 
around [0.04 0.98 0.21] (reciprocal) or [-0.12 0.99 0.07] (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_lm5
_database_code_depnum_ccdc_archive 'CCDC 2411217'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;EPFL
Switzerland
;
_audit_update_record             
;
2024-12-18 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_audit_creation_date             2024-11-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H70 N4 O2 U, 2[C4H8O]'
_chemical_formula_sum            'C50 H86 N4 O4 U'
_chemical_formula_weight         1045.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H86 N4 O4 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'
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'
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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.1897(4)
_cell_length_b                   15.6587(6)
_cell_length_c                   19.7929(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.971(3)
_cell_angle_gamma                90
_cell_volume                     4980.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6090
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6540
_cell_measurement_theta_min      3.3210
_shelx_estimated_absorpt_T_max   0.560
_shelx_estimated_absorpt_T_min   0.128
_exptl_absorpt_coefficient_mu    9.514
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.206
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense gold'
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2152
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 1 0.0240
-2 0 -1 0.0463
0 -1 0 0.1619
0 1 0 0.2037
-1 0 1 0.0231
2 6 10 0.1139
0 -1 -2 0.1193
-9 -1 -4 0.0349
6 2 9 0.0420
-9 3 -5 0.0901
3 -3 11 0.0505
-1 0 2 0.0235
9 -3 4 0.0706
1 0 -2 0.0535
6 -8 4 0.1245
-6 8 -2 0.1497
8 0 -10 0.0439
-8 -6 5 0.0847
-1 -2 2 0.0992
-8 -6 2 0.0802
1 0 2 0.0253
-1 0 -1 0.0514
8 -2 7 0.0460

_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.069
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.0013 0.0004 1.0002 0.1918 0.0673 0.0728
-2.0013 -0.0004 -1.0002 -0.1918 -0.0673 -0.0728
-0.0007 -1.0009 0.0002 -0.0353 0.0916 0.0081
0.0007 1.0009 -0.0002 0.0353 -0.0916 -0.0081
-1.0005 -0.0016 0.9987 -0.0169 0.0038 -0.1149
1.7416 6.2699 9.5453 0.8456 -0.2994 -0.4419
-0.0010 -0.9990 -1.9982 -0.1407 0.0417 0.1127
-9.4324 -1.3969 -3.9378 -0.9124 -0.1700 -0.3724
6.2360 1.9179 9.0487 0.9783 0.1818 -0.0995
-8.5073 3.4781 -4.8231 -0.7230 -0.6186 -0.3077
3.3315 -2.8803 11.0509 0.7130 0.6092 -0.3472
-1.0003 -0.0025 1.9979 0.0358 0.0287 -0.1672
8.9767 -3.4404 3.7034 0.6978 0.5972 0.3954
1.0003 0.0025 -1.9979 -0.0358 -0.0287 0.1672
5.5948 -7.7114 3.9626 0.3260 0.9229 0.2049
-6.4512 7.5403 -2.4886 -0.3138 -0.8887 -0.3343
7.9712 -0.0849 -9.5002 0.0496 -0.0597 0.9970
-7.5563 -6.2143 5.3443 -0.4621 0.5416 -0.7023
-1.0018 -2.0043 1.9982 -0.0348 0.2119 -0.1511
-8.4401 -6.0243 2.0231 -0.6920 0.4228 -0.5851
1.0009 -0.0012 1.9989 0.1750 0.0711 -0.0421
-1.0007 0.0002 -0.9997 -0.1223 -0.0461 -0.0102
7.6770 -2.4550 7.0071 0.8166 0.5617 0.1330

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.1270
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27066
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.642
_diffrn_reflns_theta_min         3.335
_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 0.965
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00 -13.00   1.00   12.50    --  -40.66 124.00 -29.00   72
  2  ω   -112.00 -87.00   1.00   12.50    --  -40.66-147.00  86.00   25
  3  ω     50.00  75.00   1.00   12.50    --   40.66-147.00  86.00   25
  4  ω     42.00  79.00   1.00   12.50    --   40.66-124.00-107.00   37
  5  ω     65.00 108.00   1.00   50.00    --  106.09-124.00-107.00   43
  6  ω    103.00 128.00   1.00   50.00    --  106.09 147.00 136.00   25
  7  ω    113.00 138.00   1.00   50.00    --  106.09 124.00 -29.00   25
  8  ω    102.00 128.00   1.00   50.00    --  106.09-147.00  86.00   26
  9  ω   -112.00 -14.00   1.00   12.50    --  -40.66 -57.00  60.00   98
 10  ω    -31.00  -4.00   1.00   12.50    --   40.66 -38.00-180.00   27
 11  ω     18.00 114.00   1.00   12.50    --   40.66  38.00-180.00   96
 12  ω     19.00  46.00   1.00   12.50    --   40.66 -38.00-150.00   27
 13  ω     79.00 107.00   1.00   50.00    --  106.09 -94.00-120.00   28
 14  ω    104.00 178.00   1.00   50.00    --  106.09  77.00 -30.00   74
 15  ω     94.00 121.00   1.00   50.00    --  106.09 -77.00  60.00   27
 16  ω    143.00 170.00   1.00   50.00    --  106.09  77.00-120.00   27
 17  ω     97.00 176.00   1.00   50.00    --  106.09 125.00 150.00   79
 18  ω     24.00 105.00   1.00   50.00    --  106.09 -94.00 -90.00   81
 19  ω     37.00  88.00   1.00   50.00    --  106.09 -77.00  60.00   51
 20  ω    103.00 164.00   1.00   50.00    --  106.09  77.00-150.00   61
 21  ω    106.00 175.00   1.00   50.00    --  106.09  77.00  60.00   69
;
_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      0.0694789000
_diffrn_orient_matrix_UB_12      0.0352463000
_diffrn_orient_matrix_UB_13      0.0527618000
_diffrn_orient_matrix_UB_21      0.0211918000
_diffrn_orient_matrix_UB_22      -0.0915196000
_diffrn_orient_matrix_UB_23      0.0248813000
_diffrn_orient_matrix_UB_31      0.0625526000
_diffrn_orient_matrix_UB_32      -0.0081029000
_diffrn_orient_matrix_UB_33      -0.0523859000
_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                6059
_reflns_number_total             9714
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.946
_refine_diff_density_min         -2.135
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9714
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0633
_refine_ls_restrained_S_all      0.996
_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)+(0.0500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1589
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C46 \\sim C46-C45 \\sim C44-C45
 with sigma of 0.02
 C20-C19 \\sim C21-C19 \\sim C22-C19 \\sim C44-C43 \\sim C45-C43 \\sim C46-C43
 with sigma of 0.02
 C19-C15 \\sim C43-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C43 \\sim C44 \\sim C45 \\sim C46:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
4. Others
 Sof(C43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=1-FVAR(1)
 Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C34(H34A,H34B)
5.b Me refined with riding coordinates:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C30(H30), C32(H32)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.67812(2) 0.21751(2) 0.80264(2) 0.04532(12) Uani 1 1 d . . . . .
O1 O 0.6161(4) 0.0949(4) 0.8213(4) 0.0446(16) Uani 1 1 d . . . . .
O2 O 0.5567(4) 0.2792(5) 0.7929(4) 0.0514(18) Uani 1 1 d . . . . .
N1 N 0.7421(5) 0.1827(7) 0.9293(5) 0.055(2) Uani 1 1 d . . . . .
N2 N 0.6966(5) 0.3784(6) 0.8617(5) 0.058(3) Uani 1 1 d . . . . .
N3 N 0.7299(6) 0.3285(7) 0.7197(5) 0.060(3) Uani 1 1 d . . . . .
N4 N 0.8134(4) 0.1782(6) 0.8076(4) 0.048(2) Uani 1 1 d . . . . .
C1 C 0.8053(7) 0.2397(9) 0.9657(7) 0.072(4) Uani 1 1 d . . . . .
H1A H 0.853800 0.241982 0.939799 0.087 Uiso 1 1 calc R U . . .
H1B H 0.824340 0.214014 1.010645 0.087 Uiso 1 1 calc R U . . .
C2 C 0.7769(7) 0.3301(9) 0.9769(7) 0.067(4) Uani 1 1 d . . . . .
H2A H 0.816519 0.356532 1.012987 0.080 Uiso 1 1 calc R U . . .
H2B H 0.721984 0.327707 0.994021 0.080 Uiso 1 1 calc R U . . .
C3 C 0.7696(5) 0.3886(8) 0.9140(7) 0.060(3) Uani 1 1 d . . . . .
H3A H 0.770158 0.448392 0.930226 0.072 Uiso 1 1 calc R U . . .
H3B H 0.820227 0.380392 0.891310 0.072 Uiso 1 1 calc R U . . .
C4 C 0.7037(6) 0.4363(7) 0.8047(6) 0.057(3) Uani 1 1 d . . . . .
H4A H 0.722549 0.492711 0.823164 0.069 Uiso 1 1 calc R U . . .
H4B H 0.647762 0.444049 0.779149 0.069 Uiso 1 1 calc R U . . .
C5 C 0.7613(7) 0.4079(8) 0.7565(7) 0.063(3) Uani 1 1 d . . . . .
H5A H 0.816817 0.396744 0.781763 0.076 Uiso 1 1 calc R U . . .
H5B H 0.767212 0.453833 0.723085 0.076 Uiso 1 1 calc R U . . .
C6 C 0.7961(7) 0.2941(9) 0.6807(6) 0.068(4) Uani 1 1 d . . . . .
H6A H 0.810488 0.339336 0.649205 0.081 Uiso 1 1 calc R U . . .
H6B H 0.771899 0.246039 0.652445 0.081 Uiso 1 1 calc R U . . .
C7 C 0.8753(7) 0.2634(9) 0.7202(7) 0.071(4) Uani 1 1 d . . . . .
H7A H 0.894599 0.307517 0.754370 0.085 Uiso 1 1 calc R U . . .
H7B H 0.917932 0.258714 0.688526 0.085 Uiso 1 1 calc R U . . .
C8 C 0.8711(7) 0.1794(8) 0.7565(7) 0.064(3) Uani 1 1 d . . . . .
H8A H 0.854476 0.134454 0.722373 0.077 Uiso 1 1 calc R U . . .
H8B H 0.927436 0.165000 0.778851 0.077 Uiso 1 1 calc R U . . .
C9 C 0.8469(8) 0.1166(8) 0.8591(7) 0.070(4) Uani 1 1 d . . . . .
H9A H 0.900945 0.137648 0.881664 0.084 Uiso 1 1 calc R U . . .
H9B H 0.856916 0.061715 0.836644 0.084 Uiso 1 1 calc R U . . .
C10 C 0.7877(6) 0.1013(8) 0.9133(7) 0.064(3) Uani 1 1 d . . . . .
H10A H 0.746483 0.057059 0.896772 0.077 Uiso 1 1 calc R U . . .
H10B H 0.820130 0.079820 0.955499 0.077 Uiso 1 1 calc R U . . .
C11 C 0.6799(7) 0.1600(10) 0.9760(6) 0.071(4) Uani 1 1 d . . . . .
H11A H 0.650066 0.211530 0.987311 0.107 Uiso 1 1 calc R U . . .
H11B H 0.708531 0.134916 1.017821 0.107 Uiso 1 1 calc R U . . .
H11C H 0.640181 0.118590 0.953669 0.107 Uiso 1 1 calc R U . . .
C12 C 0.6186(6) 0.3955(8) 0.8943(7) 0.065(4) Uani 1 1 d . . . . .
H12A H 0.608451 0.345938 0.923249 0.078 Uiso 1 1 calc R U . . .
H12B H 0.628641 0.445719 0.924561 0.078 Uiso 1 1 calc R U . . .
C13 C 0.5409(6) 0.4116(8) 0.8461(7) 0.060(3) Uani 1 1 d . . . . .
C14 C 0.4974(6) 0.4885(8) 0.8529(7) 0.064(4) Uani 1 1 d . . . . .
H14 H 0.520053 0.530667 0.884367 0.077 Uiso 1 1 calc R U . . .
C15 C 0.4219(7) 0.5029(9) 0.8139(8) 0.069(4) Uani 1 1 d D . . . .
C16 C 0.3921(6) 0.4406(8) 0.7668(7) 0.064(3) Uani 1 1 d . . . . .
H16 H 0.341805 0.451585 0.738118 0.076 Uiso 1 1 calc R U . . .
C17 C 0.4331(6) 0.3616(8) 0.7595(6) 0.059(3) Uani 1 1 d . . . . .
C18 C 0.5108(6) 0.3495(8) 0.7994(6) 0.056(3) Uani 1 1 d . . . . .
C19 C 0.3723(7) 0.5857(8) 0.8230(7) 0.064(4) Uani 0.857(13) 1 d D U P A 1
C20 C 0.4151(8) 0.6454(10) 0.8773(9) 0.075(5) Uani 0.857(13) 1 d D U P A 1
H20A H 0.428035 0.614041 0.920106 0.113 Uiso 0.857(13) 1 calc R U P A 1
H20B H 0.377994 0.693263 0.884177 0.113 Uiso 0.857(13) 1 calc R U P A 1
H20C H 0.466650 0.667251 0.862438 0.113 Uiso 0.857(13) 1 calc R U P A 1
C21 C 0.2888(7) 0.5602(10) 0.8444(8) 0.063(4) Uani 0.857(13) 1 d D U P A 1
H21A H 0.256694 0.528714 0.807357 0.094 Uiso 0.857(13) 1 calc R U P A 1
H21B H 0.258141 0.611613 0.854774 0.094 Uiso 0.857(13) 1 calc R U P A 1
H21C H 0.297751 0.523931 0.884998 0.094 Uiso 0.857(13) 1 calc R U P A 1
C22 C 0.3596(10) 0.6311(11) 0.7553(9) 0.086(5) Uani 0.857(13) 1 d D U P A 1
H22A H 0.412493 0.655756 0.745480 0.128 Uiso 0.857(13) 1 calc R U P A 1
H22B H 0.318484 0.676784 0.757001 0.128 Uiso 0.857(13) 1 calc R U P A 1
H22C H 0.339545 0.590344 0.719489 0.128 Uiso 0.857(13) 1 calc R U P A 1
C23 C 0.3935(7) 0.2908(9) 0.7109(7) 0.066(3) Uani 1 1 d . . . . .
C24 C 0.3863(7) 0.2105(9) 0.7528(8) 0.082(4) Uani 1 1 d . . . . .
H24A H 0.441102 0.195585 0.776479 0.122 Uiso 1 1 calc R U . . .
H24B H 0.365627 0.163480 0.722757 0.122 Uiso 1 1 calc R U . . .
H24C H 0.347486 0.220670 0.786327 0.122 Uiso 1 1 calc R U . . .
C25 C 0.4478(7) 0.2725(9) 0.6557(7) 0.075(4) Uani 1 1 d . . . . .
H25A H 0.457115 0.325430 0.631353 0.113 Uiso 1 1 calc R U . . .
H25B H 0.420182 0.230644 0.623812 0.113 Uiso 1 1 calc R U . . .
H25C H 0.501336 0.249536 0.676281 0.113 Uiso 1 1 calc R U . . .
C26 C 0.3057(7) 0.3175(9) 0.6773(7) 0.076(4) Uani 1 1 d . . . . .
H26A H 0.268964 0.325615 0.712611 0.114 Uiso 1 1 calc R U . . .
H26B H 0.283048 0.272714 0.645782 0.114 Uiso 1 1 calc R U . . .
H26C H 0.309781 0.371045 0.652263 0.114 Uiso 1 1 calc R U . . .
C27 C 0.6599(7) 0.3550(9) 0.6686(7) 0.066(3) Uani 1 1 d . . . . .
H27A H 0.630762 0.304231 0.649002 0.099 Uiso 1 1 calc R U . . .
H27B H 0.681604 0.387715 0.632341 0.099 Uiso 1 1 calc R U . . .
H27C H 0.621176 0.390601 0.690569 0.099 Uiso 1 1 calc R U . . .
C28 C 0.5701(6) 0.0495(7) 0.7724(5) 0.041(2) Uani 1 1 d . . . . .
C29 C 0.5077(6) -0.0090(7) 0.7857(6) 0.048(3) Uani 1 1 d . . . . .
C30 C 0.4644(6) -0.0527(7) 0.7321(5) 0.044(2) Uani 1 1 d . . . . .
H30 H 0.424112 -0.093500 0.741909 0.053 Uiso 1 1 calc R U . . .
C31 C 0.4767(6) -0.0401(7) 0.6646(6) 0.048(3) Uani 1 1 d . . . . .
C32 C 0.5390(6) 0.0198(7) 0.6535(5) 0.049(3) Uani 1 1 d . . . . .
H32 H 0.549753 0.029685 0.607975 0.059 Uiso 1 1 calc R U . . .
C33 C 0.5860(6) 0.0655(6) 0.7059(5) 0.039(2) Uani 1 1 d . . . . .
C34 C 0.6512(6) 0.1310(7) 0.6957(6) 0.053(3) Uani 1 1 d . . . . .
H34A H 0.631467 0.168466 0.656805 0.064 Uiso 1 1 calc R U . . .
H34B H 0.703012 0.102496 0.685985 0.064 Uiso 1 1 calc R U . . .
C35 C 0.4873(7) -0.0234(8) 0.8587(6) 0.056(3) Uani 1 1 d . . . . .
C36 C 0.4184(7) -0.0895(9) 0.8643(6) 0.071(4) Uani 1 1 d . . . . .
H36A H 0.366245 -0.069280 0.839026 0.106 Uiso 1 1 calc R U . . .
H36B H 0.410767 -0.097505 0.912235 0.106 Uiso 1 1 calc R U . . .
H36C H 0.434177 -0.144006 0.845113 0.106 Uiso 1 1 calc R U . . .
C37 C 0.5639(7) -0.0518(9) 0.9048(6) 0.067(4) Uani 1 1 d . . . . .
H37A H 0.577123 -0.111004 0.894251 0.101 Uiso 1 1 calc R U . . .
H37B H 0.553235 -0.047810 0.952391 0.101 Uiso 1 1 calc R U . . .
H37C H 0.610931 -0.014873 0.897588 0.101 Uiso 1 1 calc R U . . .
C38 C 0.4563(7) 0.0614(8) 0.8877(5) 0.054(3) Uani 1 1 d . . . . .
H38A H 0.499213 0.105403 0.886811 0.081 Uiso 1 1 calc R U . . .
H38B H 0.444968 0.052370 0.934692 0.081 Uiso 1 1 calc R U . . .
H38C H 0.405243 0.079914 0.859881 0.081 Uiso 1 1 calc R U . . .
C39 C 0.4306(6) -0.0903(8) 0.6061(5) 0.051(3) Uani 1 1 d . . . . .
C40 C 0.3630(7) -0.1499(9) 0.6294(6) 0.063(3) Uani 1 1 d . . . . .
H40A H 0.388125 -0.186827 0.666303 0.095 Uiso 1 1 calc R U . . .
H40B H 0.339225 -0.185170 0.591026 0.095 Uiso 1 1 calc R U . . .
H40C H 0.319011 -0.115322 0.645715 0.095 Uiso 1 1 calc R U . . .
C41 C 0.4916(6) -0.1468(9) 0.5726(7) 0.065(3) Uani 1 1 d . . . . .
H41A H 0.530292 -0.110665 0.551095 0.098 Uiso 1 1 calc R U . . .
H41B H 0.460516 -0.183182 0.538118 0.098 Uiso 1 1 calc R U . . .
H41C H 0.522855 -0.182745 0.607358 0.098 Uiso 1 1 calc R U . . .
C42 C 0.3893(6) -0.0289(8) 0.5531(6) 0.063(3) Uani 1 1 d . . . . .
H42A H 0.356738 0.013186 0.575276 0.094 Uiso 1 1 calc R U . . .
H42B H 0.352398 -0.060730 0.519120 0.094 Uiso 1 1 calc R U . . .
H42C H 0.432013 0.000479 0.530778 0.094 Uiso 1 1 calc R U . . .
C43 C 0.367(3) 0.583(2) 0.798(3) 0.066(8) Uani 0.143(13) 1 d D U P A 2
C44 C 0.418(4) 0.663(4) 0.791(4) 0.072(11) Uani 0.143(13) 1 d D U P A 2
H44A H 0.443675 0.660418 0.748577 0.108 Uiso 0.143(13) 1 calc R U P A 2
H44B H 0.380941 0.713367 0.789129 0.108 Uiso 0.143(13) 1 calc R U P A 2
H44C H 0.460749 0.668256 0.829687 0.108 Uiso 0.143(13) 1 calc R U P A 2
C45 C 0.329(5) 0.593(6) 0.864(4) 0.067(11) Uani 0.143(13) 1 d D U P A 2
H45A H 0.295241 0.542233 0.870873 0.101 Uiso 0.143(13) 1 calc R U P A 2
H45B H 0.373262 0.598600 0.901770 0.101 Uiso 0.143(13) 1 calc R U P A 2
H45C H 0.293454 0.643711 0.861212 0.101 Uiso 0.143(13) 1 calc R U P A 2
C46 C 0.295(4) 0.587(6) 0.741(3) 0.077(12) Uani 0.143(13) 1 d D U P A 2
H46A H 0.259556 0.536382 0.743352 0.115 Uiso 0.143(13) 1 calc R U P A 2
H46B H 0.261615 0.638480 0.746777 0.115 Uiso 0.143(13) 1 calc R U P A 2
H46C H 0.316161 0.588949 0.697051 0.115 Uiso 0.143(13) 1 calc R U P A 2


_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 O1 2.219(6) . ?
U1 O2 2.177(6) . ?
U1 N1 2.651(10) . ?
U1 N2 2.779(9) . ?
U1 N3 2.599(9) . ?
U1 N4 2.265(6) . ?
U1 C34 2.505(11) . ?
O1 C28 1.349(12) . ?
O2 C18 1.343(13) . ?
N1 C1 1.477(15) . ?
N1 C10 1.526(14) . ?
N1 C11 1.490(13) . ?
N2 C3 1.481(14) . ?
N2 C4 1.463(15) . ?
N2 C12 1.510(12) . ?
N3 C5 1.499(15) . ?
N3 C6 1.494(13) . ?
N3 C27 1.484(15) . ?
N4 C8 1.459(12) . ?
N4 C9 1.459(15) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.514(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.538(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.479(15) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.497(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.505(17) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.541(15) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.505(16) . ?
C13 C14 1.411(15) . ?
C13 C18 1.388(17) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(18) . ?
C15 C16 1.393(19) . ?
C15 C19 1.548(17) . ?
C15 C43 1.55(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.419(16) . ?
C17 C18 1.415(14) . ?
C17 C23 1.555(18) . ?
C19 C20 1.524(14) . ?
C19 C21 1.518(12) . ?
C19 C22 1.509(14) . ?
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 C24 1.519(17) . ?
C23 C25 1.510(17) . ?
C23 C26 1.551(16) . ?
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 C29 1.412(13) . ?
C28 C33 1.393(13) . ?
C29 C30 1.380(15) . ?
C29 C35 1.537(15) . ?
C30 H30 0.9500 . ?
C30 C31 1.388(14) . ?
C31 C32 1.415(15) . ?
C31 C39 1.519(15) . ?
C32 H32 0.9500 . ?
C32 C33 1.406(14) . ?
C33 C34 1.503(14) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.535(15) . ?
C35 C37 1.515(17) . ?
C35 C38 1.554(15) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.550(14) . ?
C39 C41 1.534(14) . ?
C39 C42 1.517(15) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.517(18) . ?
C43 C45 1.518(18) . ?
C43 C46 1.519(18) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U1 N1 78.3(3) . . ?
O1 U1 N2 137.9(3) . . ?
O1 U1 N3 150.6(3) . . ?
O1 U1 N4 102.3(3) . . ?
O1 U1 C34 68.7(3) . . ?
O2 U1 O1 88.7(3) . . ?
O2 U1 N1 114.8(3) . . ?
O2 U1 N2 71.6(3) . . ?
O2 U1 N3 90.2(3) . . ?
O2 U1 N4 169.0(3) . . ?
O2 U1 C34 95.9(3) . . ?
N1 U1 N2 77.2(3) . . ?
N3 U1 N1 128.0(3) . . ?
N3 U1 N2 68.5(3) . . ?
N4 U1 N1 68.8(3) . . ?
N4 U1 N2 100.0(3) . . ?
N4 U1 N3 79.9(3) . . ?
N4 U1 C34 87.6(3) . . ?
C34 U1 N1 134.1(4) . . ?
C34 U1 N2 147.6(4) . . ?
C34 U1 N3 82.2(3) . . ?
C28 O1 U1 123.9(6) . . ?
C18 O2 U1 149.3(7) . . ?
C1 N1 U1 120.4(8) . . ?
C1 N1 C10 106.3(9) . . ?
C1 N1 C11 108.7(9) . . ?
C10 N1 U1 96.8(7) . . ?
C11 N1 U1 114.8(7) . . ?
C11 N1 C10 108.1(10) . . ?
C3 N2 U1 115.3(7) . . ?
C3 N2 C12 108.7(9) . . ?
C4 N2 U1 104.5(7) . . ?
C4 N2 C3 110.0(9) . . ?
C4 N2 C12 111.6(10) . . ?
C12 N2 U1 106.7(6) . . ?
C5 N3 U1 111.3(7) . . ?
C6 N3 U1 113.1(7) . . ?
C6 N3 C5 109.2(9) . . ?
C27 N3 U1 109.9(6) . . ?
C27 N3 C5 106.5(10) . . ?
C27 N3 C6 106.6(10) . . ?
C8 N4 U1 131.6(7) . . ?
C8 N4 C9 106.1(8) . . ?
C9 N4 U1 119.0(6) . . ?
N1 C1 H1A 108.4 . . ?
N1 C1 H1B 108.4 . . ?
N1 C1 C2 115.6(10) . . ?
H1A C1 H1B 107.4 . . ?
C2 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
C1 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C1 C2 C3 115.7(11) . . ?
H2A C2 H2B 107.4 . . ?
C3 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
N2 C3 C2 118.6(9) . . ?
N2 C3 H3A 107.7 . . ?
N2 C3 H3B 107.7 . . ?
C2 C3 H3A 107.7 . . ?
C2 C3 H3B 107.7 . . ?
H3A C3 H3B 107.1 . . ?
N2 C4 H4A 108.5 . . ?
N2 C4 H4B 108.5 . . ?
N2 C4 C5 115.2(10) . . ?
H4A C4 H4B 107.5 . . ?
C5 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
N3 C5 H5A 109.4 . . ?
N3 C5 H5B 109.4 . . ?
C4 C5 N3 111.1(8) . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N3 C6 H6A 107.8 . . ?
N3 C6 H6B 107.8 . . ?
N3 C6 C7 117.9(11) . . ?
H6A C6 H6B 107.2 . . ?
C7 C6 H6A 107.8 . . ?
C7 C6 H6B 107.8 . . ?
C6 C7 H7A 108.2 . . ?
C6 C7 H7B 108.2 . . ?
C6 C7 C8 116.4(10) . . ?
H7A C7 H7B 107.3 . . ?
C8 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
N4 C8 C7 114.3(9) . . ?
N4 C8 H8A 108.7 . . ?
N4 C8 H8B 108.7 . . ?
C7 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
N4 C9 H9A 109.1 . . ?
N4 C9 H9B 109.1 . . ?
N4 C9 C10 112.3(9) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
N1 C10 C9 111.9(10) . . ?
N1 C10 H10A 109.2 . . ?
N1 C10 H10B 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 108.3 . . ?
N2 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C13 C12 N2 115.9(11) . . ?
C13 C12 H12A 108.3 . . ?
C13 C12 H12B 108.3 . . ?
C14 C13 C12 118.1(12) . . ?
C18 C13 C12 120.3(10) . . ?
C18 C13 C14 121.5(11) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(13) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 118.0(12) . . ?
C14 C15 C19 120.4(13) . . ?
C14 C15 C43 134(3) . . ?
C16 C15 C19 121.6(12) . . ?
C16 C15 C43 107(3) . . ?
C15 C16 H16 118.3 . . ?
C15 C16 C17 123.3(11) . . ?
C17 C16 H16 118.3 . . ?
C16 C17 C23 121.4(10) . . ?
C18 C17 C16 117.1(12) . . ?
C18 C17 C23 121.4(11) . . ?
O2 C18 C13 118.9(10) . . ?
O2 C18 C17 121.4(11) . . ?
C13 C18 C17 119.6(11) . . ?
C20 C19 C15 113.5(11) . . ?
C21 C19 C15 107.7(10) . . ?
C21 C19 C20 108.0(12) . . ?
C22 C19 C15 107.9(11) . . ?
C22 C19 C20 109.8(13) . . ?
C22 C19 C21 110.0(12) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C17 107.8(11) . . ?
C24 C23 C26 109.3(10) . . ?
C25 C23 C17 110.5(9) . . ?
C25 C23 C24 109.1(12) . . ?
C25 C23 C26 108.9(11) . . ?
C26 C23 C17 111.2(11) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C27 H27A 109.5 . . ?
N3 C27 H27B 109.5 . . ?
N3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 C29 123.5(9) . . ?
O1 C28 C33 115.7(9) . . ?
C33 C28 C29 120.7(10) . . ?
C28 C29 C35 120.8(10) . . ?
C30 C29 C28 119.1(9) . . ?
C30 C29 C35 120.2(9) . . ?
C29 C30 H30 118.3 . . ?
C29 C30 C31 123.4(9) . . ?
C31 C30 H30 118.3 . . ?
C30 C31 C32 115.6(10) . . ?
C30 C31 C39 123.1(10) . . ?
C32 C31 C39 121.1(9) . . ?
C31 C32 H32 118.2 . . ?
C33 C32 C31 123.6(9) . . ?
C33 C32 H32 118.2 . . ?
C28 C33 C32 117.5(9) . . ?
C28 C33 C34 117.5(9) . . ?
C32 C33 C34 125.0(9) . . ?
U1 C34 H34A 110.1 . . ?
U1 C34 H34B 110.1 . . ?
C33 C34 U1 108.0(6) . . ?
C33 C34 H34A 110.1 . . ?
C33 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
C29 C35 C38 109.7(10) . . ?
C36 C35 C29 114.0(10) . . ?
C36 C35 C38 106.3(9) . . ?
C37 C35 C29 110.8(8) . . ?
C37 C35 C36 107.9(11) . . ?
C37 C35 C38 107.8(10) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C31 C39 C40 112.5(9) . . ?
C31 C39 C41 110.2(8) . . ?
C41 C39 C40 107.2(10) . . ?
C42 C39 C31 109.5(10) . . ?
C42 C39 C40 108.6(9) . . ?
C42 C39 C41 108.7(9) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C15 113(5) . . ?
C44 C43 C45 106(3) . . ?
C44 C43 C46 106(2) . . ?
C45 C43 C15 101(4) . . ?
C45 C43 C46 106(3) . . ?
C46 C43 C15 124(5) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O1 C28 C29 -156.2(7) . . . . ?
U1 O1 C28 C33 22.0(11) . . . . ?
U1 O2 C18 C13 -25(2) . . . . ?
U1 O2 C18 C17 154.2(10) . . . . ?
U1 N1 C1 C2 62.2(13) . . . . ?
U1 N1 C10 C9 54.9(10) . . . . ?
U1 N2 C3 C2 -59.0(11) . . . . ?
U1 N2 C4 C5 -46.2(11) . . . . ?
U1 N2 C12 C13 -71.1(12) . . . . ?
U1 N3 C5 C4 -45.1(12) . . . . ?
U1 N3 C6 C7 -60.0(13) . . . . ?
U1 N4 C8 C7 50.6(15) . . . . ?
U1 N4 C9 C10 -12.2(14) . . . . ?
O1 C28 C29 C30 -179.6(9) . . . . ?
O1 C28 C29 C35 1.1(15) . . . . ?
O1 C28 C33 C32 -179.7(8) . . . . ?
O1 C28 C33 C34 -0.5(13) . . . . ?
N1 C1 C2 C3 -75.5(13) . . . . ?
N2 C4 C5 N3 65.8(14) . . . . ?
N2 C12 C13 C14 -123.7(11) . . . . ?
N2 C12 C13 C18 60.4(16) . . . . ?
N3 C6 C7 C8 74.1(16) . . . . ?
N4 C9 C10 N1 -35.7(15) . . . . ?
C1 N1 C10 C9 -69.6(13) . . . . ?
C1 C2 C3 N2 76.9(12) . . . . ?
C3 N2 C4 C5 78.2(13) . . . . ?
C3 N2 C12 C13 164.0(11) . . . . ?
C4 N2 C3 C2 -176.9(9) . . . . ?
C4 N2 C12 C13 42.6(14) . . . . ?
C5 N3 C6 C7 64.5(15) . . . . ?
C6 N3 C5 C4 -170.6(10) . . . . ?
C6 C7 C8 N4 -60.9(16) . . . . ?
C8 N4 C9 C10 -174.2(10) . . . . ?
C9 N4 C8 C7 -150.6(12) . . . . ?
C10 N1 C1 C2 170.6(10) . . . . ?
C11 N1 C1 C2 -73.3(14) . . . . ?
C11 N1 C10 C9 173.8(10) . . . . ?
C12 N2 C3 C2 60.7(13) . . . . ?
C12 N2 C4 C5 -161.1(10) . . . . ?
C12 C13 C14 C15 -174.2(11) . . . . ?
C12 C13 C18 O2 -7.3(17) . . . . ?
C12 C13 C18 C17 173.2(11) . . . . ?
C13 C14 C15 C16 -2.0(18) . . . . ?
C13 C14 C15 C19 177.7(11) . . . . ?
C13 C14 C15 C43 -166(3) . . . . ?
C14 C13 C18 O2 176.9(10) . . . . ?
C14 C13 C18 C17 -2.6(17) . . . . ?
C14 C15 C16 C17 3.5(19) . . . . ?
C14 C15 C19 C20 0.0(17) . . . . ?
C14 C15 C19 C21 -119.5(13) . . . . ?
C14 C15 C19 C22 121.8(14) . . . . ?
C14 C15 C43 C44 37(5) . . . . ?
C14 C15 C43 C45 -76(4) . . . . ?
C14 C15 C43 C46 166(3) . . . . ?
C15 C16 C17 C18 -4.4(18) . . . . ?
C15 C16 C17 C23 174.4(11) . . . . ?
C16 C15 C19 C20 179.6(12) . . . . ?
C16 C15 C19 C21 60.2(17) . . . . ?
C16 C15 C19 C22 -58.5(16) . . . . ?
C16 C15 C43 C44 -129(3) . . . . ?
C16 C15 C43 C45 118(3) . . . . ?
C16 C15 C43 C46 1(4) . . . . ?
C16 C17 C18 O2 -175.7(10) . . . . ?
C16 C17 C18 C13 3.8(17) . . . . ?
C16 C17 C23 C24 -122.7(12) . . . . ?
C16 C17 C23 C25 118.2(12) . . . . ?
C16 C17 C23 C26 -2.9(16) . . . . ?
C18 C13 C14 C15 1.6(18) . . . . ?
C18 C17 C23 C24 56.0(14) . . . . ?
C18 C17 C23 C25 -63.1(15) . . . . ?
C18 C17 C23 C26 175.8(11) . . . . ?
C19 C15 C16 C17 -176.2(11) . . . . ?
C23 C17 C18 O2 5.6(17) . . . . ?
C23 C17 C18 C13 -175.0(11) . . . . ?
C27 N3 C5 C4 74.7(12) . . . . ?
C27 N3 C6 C7 179.2(11) . . . . ?
C28 C29 C30 C31 -2.4(16) . . . . ?
C28 C29 C35 C36 -179.6(10) . . . . ?
C28 C29 C35 C37 -57.5(15) . . . . ?
C28 C29 C35 C38 61.4(13) . . . . ?
C28 C33 C34 U1 -16.2(11) . . . . ?
C29 C28 C33 C32 -1.4(14) . . . . ?
C29 C28 C33 C34 177.7(9) . . . . ?
C29 C30 C31 C32 1.6(15) . . . . ?
C29 C30 C31 C39 178.2(10) . . . . ?
C30 C29 C35 C36 1.1(16) . . . . ?
C30 C29 C35 C37 123.1(12) . . . . ?
C30 C29 C35 C38 -118.0(11) . . . . ?
C30 C31 C32 C33 -0.7(15) . . . . ?
C30 C31 C39 C40 5.6(15) . . . . ?
C30 C31 C39 C41 -114.0(11) . . . . ?
C30 C31 C39 C42 126.5(11) . . . . ?
C31 C32 C33 C28 0.6(15) . . . . ?
C31 C32 C33 C34 -178.5(10) . . . . ?
C32 C31 C39 C40 -178.0(10) . . . . ?
C32 C31 C39 C41 62.4(14) . . . . ?
C32 C31 C39 C42 -57.1(12) . . . . ?
C32 C33 C34 U1 163.0(8) . . . . ?
C33 C28 C29 C30 2.3(15) . . . . ?
C33 C28 C29 C35 -177.1(10) . . . . ?
C35 C29 C30 C31 177.0(10) . . . . ?
C39 C31 C32 C33 -177.4(9) . . . . ?
C43 C15 C16 C17 172(2) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 296 electrons were 
found in a volume of 1320Å³ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H8O] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.945 -0.945 0.000 659.8 148.0 '4 THF'
2 -0.586 0.586 0.500 659.8 148.0 '4 THF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2023-05-23
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.536
_oxdiff_exptl_absorpt_empirical_full_min 0.457
