# Supplementary Information (SI) for CrystEngComm.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2432774'
loop_
_audit_author_name
_audit_author_address
'Lei Mei'
; Institute of High Energy Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2025-07-07 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_audit_creation_date             2025-07-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H11 N O5 U'
_chemical_formula_sum            'C14 H11 N O5 U'
_chemical_formula_weight         511.27
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n 21 a'
_space_group_name_Hall           'P -2ac -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   8.4393(4)
_cell_length_b                   9.9752(6)
_cell_length_c                   16.3986(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1380.49(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.22
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.778
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3785
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1214 before and 0.0618 after correction.
The Ratio of minimum to maximum transmission is 0.5076.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10189
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         3.397
_diffrn_ambient_temperature      296.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2829
_reflns_number_total             3019
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.888
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.288(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3019
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0186
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0106P)²+0.4597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0422
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.712(11)
 0.288(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Riding coordinates:
 O5(H5)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C6(H6), C7(H7), C4(H4), C14(H14), C11(H11), C9(H9), C12(H12),
 C13(H13)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.47236(2) -0.00176(6) 0.21155(2) 0.01661(7) Uani 1 1 d . . . . .
C2 C 0.8418(6) -0.0046(15) 0.0134(3) 0.0210(10) Uani 1 1 d . . . . .
C5 C 0.8740(8) 0.0092(15) -0.1561(3) 0.0257(16) Uani 1 1 d . . . . .
C8 C 0.8891(9) 0.0217(9) -0.2453(4) 0.031(2) Uani 1 1 d . . . . .
H8 H 0.957229 0.087992 -0.264365 0.038 Uiso 1 1 calc R U . . .
C3 C 0.9442(8) 0.0892(7) -0.0219(4) 0.0246(14) Uani 1 1 d . . . . .
H3 H 1.002575 0.147152 0.010862 0.030 Uiso 1 1 calc R U . . .
C6 C 0.7767(10) -0.0863(7) -0.1201(4) 0.0357(18) Uani 1 1 d . . . . .
H6 H 0.723825 -0.148133 -0.152678 0.043 Uiso 1 1 calc R U . . .
C7 C 0.7576(9) -0.0904(7) -0.0364(4) 0.0332(17) Uani 1 1 d . . . . .
H7 H 0.687466 -0.151626 -0.013409 0.040 Uiso 1 1 calc R U . . .
C4 C 0.9579(8) 0.0950(7) -0.1060(4) 0.0277(15) Uani 1 1 d . . . . .
H4 H 1.025158 0.158144 -0.129278 0.033 Uiso 1 1 calc R U . . .
C1 C 0.8118(6) -0.0045(14) 0.1029(3) 0.0215(11) Uani 1 1 d . . . . .
O5 O 0.2009(6) 0.0242(8) 0.2057(2) 0.030(2) Uani 1 1 d . . . . .
H5 H 0.162163 0.054918 0.154881 0.07(3) Uiso 1 1 d R . . . .
O2 O 0.9059(6) 0.0589(5) 0.1493(2) 0.0281(10) Uani 1 1 d . . . . .
C10 C 0.8367(8) -0.0354(6) -0.3897(4) 0.0230(18) Uani 1 1 d . . . . .
O3 O 0.4947(7) 0.1714(6) 0.1864(4) 0.0317(11) Uani 1 1 d . . . . .
C14 C 0.7819(8) -0.1343(7) -0.4428(4) 0.0281(14) Uani 1 1 d . . . . .
H14 H 0.729250 -0.209305 -0.422782 0.034 Uiso 1 1 calc R U . . .
O4 O 0.4465(7) -0.1739(5) 0.2316(4) 0.0361(13) Uani 1 1 d . . . . .
C11 C 0.9120(10) 0.0758(7) -0.4244(4) 0.0313(15) Uani 1 1 d . . . . .
H11 H 0.947584 0.145396 -0.391387 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8154(9) -0.0520(7) -0.3017(4) 0.0279(16) Uani 1 1 d . . . . .
H9 H 0.746021 -0.118250 -0.283943 0.033 Uiso 1 1 calc R U . . .
N1 N 0.8843(6) -0.0190(9) -0.5587(3) 0.0191(14) Uani 1 1 d . . . . .
C12 C 0.9331(9) 0.0817(7) -0.5077(4) 0.0264(14) Uani 1 1 d . . . . .
H12 H 0.982236 0.156591 -0.530074 0.032 Uiso 1 1 calc R U . . .
C13 C 0.8070(9) -0.1190(7) -0.5259(4) 0.0283(15) Uani 1 1 d . . . . .
H13 H 0.766267 -0.184278 -0.560565 0.034 Uiso 1 1 calc R U . . .
O1 O 0.6904(5) -0.0652(5) 0.1285(3) 0.0280(10) Uani 1 1 d . . . . .


_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 O5 2.308(5) . ?
U1 O5 2.373(4) 3 ?
U1 O2 2.426(4) 3_455 ?
U1 O3 1.785(6) . ?
U1 O4 1.762(5) . ?
U1 N1 2.620(4) 3_454 ?
U1 O1 2.375(4) . ?
C2 C3 1.399(13) . ?
C2 C7 1.379(12) . ?
C2 C1 1.490(6) . ?
C5 C8 1.474(8) . ?
C5 C6 1.389(13) . ?
C5 C4 1.382(12) . ?
C8 H8 0.9300 . ?
C8 C9 1.335(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.383(8) . ?
C7 H7 0.9300 . ?
C4 H4 0.9300 . ?
C1 O2 1.270(9) . ?
C1 O1 1.261(9) . ?
O5 H5 0.9457 . ?
C10 C14 1.395(9) . ?
C10 C11 1.399(9) . ?
C10 C9 1.463(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.388(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.380(9) . ?
C9 H9 0.9300 . ?
N1 C12 1.370(10) . ?
N1 C13 1.308(10) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?

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
O5 U1 O5 144.95(15) . 3 ?
O5 U1 O2 77.40(15) . 3_455 ?
O5 U1 O2 67.82(15) 3 3_455 ?
O5 U1 N1 71.68(15) . 3_454 ?
O5 U1 N1 141.73(15) 3 3_454 ?
O5 U1 O1 74.18(16) 3 . ?
O5 U1 O1 140.82(16) . . ?
O2 U1 N1 148.26(17) 3_455 3_454 ?
O3 U1 O5 89.2(3) . . ?
O3 U1 O5 86.6(3) . 3 ?
O3 U1 O2 90.0(2) . 3_455 ?
O3 U1 N1 82.7(3) . 3_454 ?
O3 U1 O1 92.5(2) . . ?
O4 U1 O5 95.8(3) . 3 ?
O4 U1 O5 89.7(3) . . ?
O4 U1 O2 92.2(2) . 3_455 ?
O4 U1 O3 177.2(3) . . ?
O4 U1 N1 94.6(3) . 3_454 ?
O4 U1 O1 86.8(2) . . ?
O1 U1 O2 141.69(16) . 3_455 ?
O1 U1 N1 69.75(16) . 3_454 ?
C3 C2 C1 120.8(10) . . ?
C7 C2 C3 119.3(5) . . ?
C7 C2 C1 119.7(9) . . ?
C6 C5 C8 122.1(8) . . ?
C4 C5 C8 119.6(8) . . ?
C4 C5 C6 118.3(5) . . ?
C5 C8 H8 116.5 . . ?
C9 C8 C5 126.9(8) . . ?
C9 C8 H8 116.5 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(6) . . ?
C4 C3 H3 120.3 . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.8(7) . . ?
C7 C6 H6 119.6 . . ?
C2 C7 C6 120.6(7) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C5 C4 C3 121.6(7) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
O2 C1 C2 119.0(8) . . ?
O1 C1 C2 117.8(7) . . ?
O1 C1 O2 123.2(5) . . ?
U1 O5 U1 140.4(2) . 3_455 ?
U1 O5 H5 114.6 . . ?
U1 O5 H5 105.0 3_455 . ?
C1 O2 U1 125.8(5) . 3 ?
C14 C10 C11 117.2(6) . . ?
C14 C10 C9 119.6(6) . . ?
C11 C10 C9 123.1(6) . . ?
C10 C14 H14 120.5 . . ?
C13 C14 C10 119.0(6) . . ?
C13 C14 H14 120.5 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.7(6) . . ?
C12 C11 H11 120.2 . . ?
C8 C9 C10 124.3(7) . . ?
C8 C9 H9 117.9 . . ?
C10 C9 H9 117.9 . . ?
C12 N1 U1 116.8(5) . 3_554 ?
C13 N1 U1 125.8(5) . 3_554 ?
C13 N1 C12 117.2(5) . . ?
C11 C12 H12 118.8 . . ?
N1 C12 C11 122.3(6) . . ?
N1 C12 H12 118.8 . . ?
C14 C13 H13 117.8 . . ?
N1 C13 C14 124.3(6) . . ?
N1 C13 H13 117.8 . . ?
C1 O1 U1 133.8(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 N1 C12 C11 -171.6(6) 3_554 . . . ?
U1 N1 C13 C14 170.3(5) 3_554 . . . ?
C2 C3 C4 C5 -0.7(12) . . . . ?
C2 C1 O2 U1 -148.3(8) . . . 3 ?
C2 C1 O1 U1 -125.9(9) . . . . ?
C5 C8 C9 C10 -179.4(8) . . . . ?
C5 C6 C7 C2 -3.7(14) . . . . ?
C8 C5 C6 C7 -176.1(8) . . . . ?
C8 C5 C4 C3 178.3(7) . . . . ?
C3 C2 C7 C6 1.5(13) . . . . ?
C3 C2 C1 O2 -16.4(15) . . . . ?
C3 C2 C1 O1 161.7(8) . . . . ?
C6 C5 C8 C9 0.3(14) . . . . ?
C6 C5 C4 C3 -1.3(13) . . . . ?
C7 C2 C3 C4 0.7(12) . . . . ?
C7 C2 C1 O2 169.1(8) . . . . ?
C7 C2 C1 O1 -12.8(16) . . . . ?
C4 C5 C8 C9 -179.3(9) . . . . ?
C4 C5 C6 C7 3.5(14) . . . . ?
C1 C2 C3 C4 -173.8(7) . . . . ?
C1 C2 C7 C6 176.0(9) . . . . ?
O2 C1 O1 U1 52.1(13) . . . . ?
C10 C14 C13 N1 2.3(12) . . . . ?
C10 C11 C12 N1 -0.7(12) . . . . ?
C14 C10 C11 C12 -1.9(11) . . . . ?
C14 C10 C9 C8 166.3(8) . . . . ?
C11 C10 C14 C13 1.2(11) . . . . ?
C11 C10 C9 C8 -13.0(11) . . . . ?
C9 C10 C14 C13 -178.1(6) . . . . ?
C9 C10 C11 C12 177.4(7) . . . . ?
C12 N1 C13 C14 -4.9(11) . . . . ?
C13 N1 C12 C11 4.1(11) . . . . ?
O1 C1 O2 U1 33.7(13) . . . 3 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.712(11)
2 0.288(11)

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2432775'
loop_
_audit_author_name
_audit_author_address
'Lei Mei'
; Institute of High Energy Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2025-07-07 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_audit_creation_date             2025-07-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C44 H28 N2 O22 U4, C28 H26 N2 O8 U'
_chemical_formula_sum            'C72 H54 N4 O30 U5'
_chemical_formula_weight         2645.34
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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                   10.7194(6)
_cell_length_b                   13.6309(8)
_cell_length_c                   14.1063(6)
_cell_angle_alpha                66.313(2)
_cell_angle_beta                 70.931(2)
_cell_angle_gamma                80.904(2)
_cell_volume                     1783.07(17)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    295.00
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.63
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.408
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5157
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0964 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.6917.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1214
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49576
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.578
_diffrn_reflns_theta_min         2.720
_diffrn_ambient_temperature      295.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5972
_reflns_number_total             8193
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0332
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0117P)²+9.8056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0642
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C19(H19), C18(H18), C27(H27), C20(H20), C8(H8), C35(H35), C36(H36),
 C7(H7), C28(H28), C14(H14), C3(H3), C33(H33), C13(H13), C25(H25), C9(H9),
 C29(H29), C15(H15), C4(H4), C10(H10), C30(H30), C32(H32), C12(H12), C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.63289(2) 0.02995(2) 1.22214(2) 0.01929(7) Uani 1 1 d . . . . .
U2 U 0.65065(2) -0.05502(2) 1.53556(2) 0.02063(7) Uani 1 1 d . . . . .
U3 U 0.500000 -0.500000 1.500000 0.02930(10) Uani 1 2 d S . P . .
O2 O 0.5822(5) -0.1020(4) 1.2583(4) 0.0288(12) Uani 1 1 d . . . . .
O5 O 0.5641(4) 0.0169(4) 1.3954(3) 0.0240(11) Uani 1 1 d . . . . .
O4 O 0.6162(5) -0.1861(4) 1.5533(4) 0.0368(13) Uani 1 1 d . . . . .
O1 O 0.6870(6) 0.1607(4) 1.1801(4) 0.0390(14) Uani 1 1 d . . . . .
O6 O 0.4062(5) 0.1027(4) 1.2502(4) 0.0277(12) Uani 1 1 d . . . . .
O3 O 0.6918(5) 0.0729(4) 1.5198(4) 0.0344(13) Uani 1 1 d . . . . .
O11 O 1.3926(5) -0.0815(5) 0.9581(4) 0.0375(14) Uani 1 1 d . . . . .
O15 O 0.4972(6) -0.2987(4) 1.4428(4) 0.0409(14) Uani 1 1 d . . . . .
H15A H 0.548475 -0.271003 1.378812 0.061 Uiso 1 1 d R U . . .
H15B H 0.530601 -0.282835 1.481935 0.061 Uiso 1 1 d R U . . .
O10 O 1.1967(5) -0.0203(5) 0.9403(4) 0.0375(14) Uani 1 1 d . . . . .
O8 O 0.8235(5) -0.0407(5) 1.2676(4) 0.0442(16) Uani 1 1 d . . . . .
O7 O 0.2095(5) 0.1398(5) 1.3426(4) 0.0386(14) Uani 1 1 d . . . . .
O9 O 0.8645(5) -0.0628(5) 1.4172(4) 0.0446(16) Uani 1 1 d . . . . .
O14 O 0.5278(6) -0.4292(4) 1.6234(4) 0.0462(16) Uani 1 1 d . . . . .
O13 O 0.5242(6) -0.6029(5) 1.6848(4) 0.0466(16) Uani 1 1 d . . . . .
N1 N -0.0195(7) 0.3571(6) 0.5292(5) 0.0390(17) Uani 1 1 d . . . . .
O12 O 0.3275(5) -0.4961(5) 1.5534(5) 0.0451(15) Uani 1 1 d . . . . .
C23 C 1.2736(7) -0.0578(6) 0.9983(5) 0.0242(16) Uani 1 1 d . . . . .
C22 C 1.0905(6) -0.0606(6) 1.1626(5) 0.0210(15) Uani 1 1 d . . . . .
H22 H 1.032198 -0.040732 1.121103 0.025 Uiso 1 1 calc R U . . .
C19 C 1.2653(7) -0.1196(6) 1.2864(5) 0.0261(16) Uani 1 1 d . . . . .
H19 H 1.323461 -0.139846 1.328075 0.031 Uiso 1 1 calc R U . . .
C37 C 0.5429(8) -0.5196(7) 1.6936(6) 0.0370(19) Uani 1 1 d . . . . .
C18 C 1.1322(7) -0.1015(6) 1.3320(5) 0.0260(16) Uani 1 1 d . . . . .
H18 H 1.101661 -0.107892 1.403894 0.031 Uiso 1 1 calc R U . . .
C27 C 0.7615(9) -0.6914(8) 2.3031(7) 0.050(2) Uani 1 1 d . . . . .
H27 H 0.699137 -0.740028 2.318196 0.060 Uiso 1 1 calc R U . . .
C1 C 0.2870(7) 0.1363(6) 1.2545(5) 0.0256(16) Uani 1 1 d . . . . .
C21 C 1.2237(6) -0.0769(6) 1.1169(5) 0.0217(15) Uani 1 1 d . . . . .
C20 C 1.3112(7) -0.1074(6) 1.1781(5) 0.0250(16) Uani 1 1 d . . . . .
H20 H 1.400155 -0.119576 1.146989 0.030 Uiso 1 1 calc R U . . .
N2 N 0.9073(8) -0.6335(6) 2.3623(6) 0.0465(19) Uani 1 1 d . . . . .
C8 C 0.1018(8) 0.1902(6) 1.1738(6) 0.0344(19) Uani 1 1 d . . . . .
H8 H 0.045283 0.184611 1.241600 0.041 Uiso 1 1 calc R U . . .
C35 C 0.5965(9) -0.6190(7) 1.8687(6) 0.042(2) Uani 1 1 d . . . . .
H35 H 0.568101 -0.681684 1.871971 0.050 Uiso 1 1 calc R U . . .
C17 C 1.0447(6) -0.0741(6) 1.2712(5) 0.0205(15) Uani 1 1 d . . . . .
C36 C 0.6449(9) -0.6197(8) 1.9500(7) 0.047(2) Uani 1 1 d . . . . .
H36 H 0.646583 -0.683355 2.008636 0.057 Uiso 1 1 calc R U . . .
C2 C 0.2348(7) 0.1700(6) 1.1603(5) 0.0246(15) Uani 1 1 d . . . . .
C7 C 0.0509(8) 0.2188(7) 1.0871(7) 0.042(2) Uani 1 1 d . . . . .
H7 H -0.039791 0.230025 1.098220 0.050 Uiso 1 1 calc R U . . .
C34 C 0.5918(8) -0.5230(6) 1.7833(6) 0.0322(18) Uani 1 1 d . . . . .
C16 C 0.9018(7) -0.0584(6) 1.3227(5) 0.0264(16) Uani 1 1 d . . . . .
C26 C 0.7975(9) -0.6091(7) 2.2028(7) 0.043(2) Uani 1 1 d . . . . .
C28 C 0.8195(9) -0.7002(8) 2.3799(7) 0.050(2) Uani 1 1 d . . . . .
H28 H 0.795303 -0.755840 2.447089 0.060 Uiso 1 1 calc R U . . .
C31 C 0.6902(9) -0.5275(7) 1.9448(6) 0.042(2) Uani 1 1 d . . . . .
C14 C -0.1032(9) 0.3596(7) 0.6222(7) 0.042(2) Uani 1 1 d . . . . .
H14 H -0.191419 0.378719 0.626282 0.051 Uiso 1 1 calc R U . . .
C5 C 0.1325(9) 0.2308(7) 0.9845(6) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.3181(8) 0.1816(7) 1.0579(5) 0.036(2) Uani 1 1 d . . . . .
H3 H 0.408534 0.169072 1.047111 0.044 Uiso 1 1 calc R U . . .
C33 C 0.6317(9) -0.4314(7) 1.7793(7) 0.048(2) Uani 1 1 d . . . . .
H33 H 0.624991 -0.366938 1.722948 0.057 Uiso 1 1 calc R U . . .
C13 C 0.1054(9) 0.3318(7) 0.5238(6) 0.044(2) Uani 1 1 d . . . . .
H13 H 0.163239 0.330293 0.458823 0.052 Uiso 1 1 calc R U . . .
C25 C 0.8930(10) -0.5408(7) 2.1830(7) 0.053(3) Uani 1 1 d . . . . .
H25 H 0.921234 -0.486316 2.115426 0.063 Uiso 1 1 calc R U . . .
C9 C 0.0719(10) 0.2590(7) 0.8966(7) 0.051(2) Uani 1 1 d . . . . .
H9 H -0.019800 0.264795 0.915826 0.061 Uiso 1 1 calc R U . . .
C29 C 0.7351(10) -0.6017(8) 2.1211(7) 0.051(2) Uani 1 1 d . . . . .
H29 H 0.680789 -0.657330 2.139461 0.061 Uiso 1 1 calc R U . . .
C15 C -0.0613(9) 0.3342(7) 0.7129(6) 0.043(2) Uani 1 1 d . . . . .
H15 H -0.121533 0.335061 0.777273 0.052 Uiso 1 1 calc R U . . .
C4 C 0.2664(9) 0.2118(7) 0.9715(6) 0.043(2) Uani 1 1 d . . . . .
H4 H 0.323279 0.219524 0.903284 0.051 Uiso 1 1 calc R U . . .
C10 C 0.1313(10) 0.2764(8) 0.7967(7) 0.052(3) Uani 1 1 d . . . . .
H10 H 0.222852 0.268617 0.778196 0.063 Uiso 1 1 calc R U . . .
C30 C 0.7475(10) -0.5268(8) 2.0273(7) 0.052(2) Uani 1 1 d . . . . .
H30 H 0.795840 -0.467762 2.009747 0.063 Uiso 1 1 calc R U . . .
C11 C 0.0719(9) 0.3074(6) 0.7070(6) 0.037(2) Uani 1 1 d . . . . .
C32 C 0.6822(10) -0.4336(8) 1.8587(7) 0.057(3) Uani 1 1 d . . . . .
H32 H 0.711331 -0.370622 1.853934 0.068 Uiso 1 1 calc R U . . .
C12 C 0.1550(9) 0.3076(7) 0.6093(7) 0.045(2) Uani 1 1 d . . . . .
H12 H 0.244519 0.291257 0.601020 0.054 Uiso 1 1 calc R U . . .
C24 C 0.9466(11) -0.5540(8) 2.2649(7) 0.055(3) Uani 1 1 d . . . . .
H24 H 1.010126 -0.507444 2.252246 0.066 Uiso 1 1 calc R U . . .
H2 H 0.953(9) -0.637(7) 2.420(7) 0.07(3) Uiso 1 1 d . . . . .


_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 U2 3.8547(4) 2_658 ?
U1 O2 1.783(5) . ?
U1 O5 2.251(4) . ?
U1 O1 1.765(5) . ?
U1 O6 2.443(5) . ?
U1 O11 2.447(4) 2_757 ?
U1 O10 2.457(5) 2_757 ?
U1 O8 2.292(5) . ?
U1 C23 2.820(6) 2_757 ?
U2 U2 3.6145(5) 2_658 ?
U2 O5 2.255(4) . ?
U2 O5 2.254(4) 2_658 ?
U2 O4 1.784(6) . ?
U2 O6 2.696(4) 2_658 ?
U2 O3 1.776(5) . ?
U2 O7 2.465(5) 2_658 ?
U2 O9 2.370(5) . ?
U2 C1 2.977(6) 2_658 ?
U3 O15 2.529(5) . ?
U3 O15 2.529(5) 2_648 ?
U3 O14 2.415(5) 2_648 ?
U3 O14 2.415(5) . ?
U3 O13 2.494(5) 2_648 ?
U3 O13 2.494(5) . ?
U3 O12 1.755(6) . ?
U3 O12 1.755(6) 2_648 ?
U3 C37 2.817(7) . ?
U3 C37 2.817(7) 2_648 ?
O6 C1 1.278(8) . ?
O11 C23 1.264(8) . ?
O15 H15A 0.8531 . ?
O15 H15B 0.8536 . ?
O10 C23 1.257(8) . ?
O8 C16 1.256(8) . ?
O7 C1 1.263(8) . ?
O9 C16 1.240(8) . ?
O14 C37 1.260(9) . ?
O13 C37 1.243(9) . ?
N1 C14 1.335(10) . ?
N1 C13 1.314(10) . ?
C23 C21 1.505(9) . ?
C22 H22 0.9300 . ?
C22 C21 1.385(9) . ?
C22 C17 1.389(8) . ?
C19 H19 0.9300 . ?
C19 C18 1.388(9) . ?
C19 C20 1.391(9) . ?
C37 C34 1.503(10) . ?
C18 H18 0.9300 . ?
C18 C17 1.383(9) . ?
C27 H27 0.9300 . ?
C27 C26 1.383(12) . ?
C27 C28 1.373(11) . ?
C1 C2 1.485(9) . ?
C21 C20 1.384(9) . ?
C20 H20 0.9300 . ?
N2 C28 1.309(11) . ?
N2 C24 1.345(11) . ?
N2 H2 1.06(9) . ?
C8 H8 0.9300 . ?
C8 C2 1.373(10) . ?
C8 C7 1.390(10) . ?
C35 H35 0.9300 . ?
C35 C36 1.402(11) . ?
C35 C34 1.385(10) . ?
C17 C16 1.489(9) . ?
C36 H36 0.9300 . ?
C36 C31 1.384(12) . ?
C2 C3 1.389(9) . ?
C7 H7 0.9300 . ?
C7 C5 1.383(11) . ?
C34 C33 1.356(11) . ?
C26 C25 1.377(12) . ?
C26 C29 1.474(11) . ?
C28 H28 0.9300 . ?
C31 C30 1.487(11) . ?
C31 C32 1.380(12) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(10) . ?
C5 C9 1.474(10) . ?
C5 C4 1.382(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.387(10) . ?
C33 H33 0.9300 . ?
C33 C32 1.383(11) . ?
C13 H13 0.9300 . ?
C13 C12 1.374(11) . ?
C25 H25 0.9300 . ?
C25 C24 1.390(11) . ?
C9 H9 0.9300 . ?
C9 C10 1.280(12) . ?
C29 H29 0.9300 . ?
C29 C30 1.286(11) . ?
C15 H15 0.9300 . ?
C15 C11 1.401(12) . ?
C4 H4 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.482(10) . ?
C30 H30 0.9300 . ?
C11 C12 1.375(11) . ?
C32 H32 0.9300 . ?
C12 H12 0.9300 . ?
C24 H24 0.9300 . ?

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
O2 U1 U2 89.14(15) . 2_658 ?
O2 U1 O5 92.39(19) . . ?
O2 U1 O6 92.8(2) . . ?
O2 U1 O11 90.1(2) . 2_757 ?
O2 U1 O10 91.2(2) . 2_757 ?
O2 U1 O8 89.8(2) . . ?
O2 U1 C23 91.0(2) . 2_757 ?
O5 U1 U2 31.19(11) . 2_658 ?
O5 U1 O6 74.75(15) . . ?
O5 U1 O11 153.89(16) . 2_757 ?
O5 U1 O10 152.76(15) . 2_757 ?
O5 U1 O8 81.37(16) . . ?
O5 U1 C23 176.6(2) . 2_757 ?
O1 U1 U2 93.39(18) . 2_658 ?
O1 U1 O2 177.3(2) . . ?
O1 U1 O5 90.3(2) . . ?
O1 U1 O6 88.4(2) . . ?
O1 U1 O11 87.7(2) . 2_757 ?
O1 U1 O10 86.2(2) . 2_757 ?
O1 U1 O8 90.1(2) . . ?
O1 U1 C23 86.3(2) . 2_757 ?
O6 U1 U2 43.95(10) . 2_658 ?
O6 U1 O11 79.17(15) . 2_757 ?
O6 U1 O10 132.01(15) . 2_757 ?
O6 U1 C23 105.66(17) . 2_757 ?
O11 U1 U2 122.98(11) 2_757 2_658 ?
O11 U1 O10 53.01(16) 2_757 2_757 ?
O11 U1 C23 26.58(17) 2_757 2_757 ?
O10 U1 U2 175.97(11) 2_757 2_658 ?
O10 U1 C23 26.43(17) 2_757 2_757 ?
O8 U1 U2 112.37(12) . 2_658 ?
O8 U1 O6 156.07(16) . . ?
O8 U1 O11 124.64(17) . 2_757 ?
O8 U1 O10 71.65(16) . 2_757 ?
O8 U1 C23 98.08(18) . 2_757 ?
C23 U1 U2 149.55(14) 2_757 2_658 ?
U2 U2 U1 67.569(9) 2_658 2_658 ?
O5 U2 U1 31.13(10) 2_658 2_658 ?
O5 U2 U1 104.13(11) . 2_658 ?
O5 U2 U2 36.72(10) 2_658 2_658 ?
O5 U2 U2 36.71(11) . 2_658 ?
O5 U2 O5 73.42(16) 2_658 . ?
O5 U2 O6 143.08(15) . 2_658 ?
O5 U2 O6 69.74(14) 2_658 2_658 ?
O5 U2 O7 166.94(16) . 2_658 ?
O5 U2 O7 119.58(15) 2_658 2_658 ?
O5 U2 O9 91.15(17) . . ?
O5 U2 O9 164.00(17) 2_658 . ?
O5 U2 C1 168.43(18) . 2_658 ?
O5 U2 C1 95.15(17) 2_658 2_658 ?
O4 U2 U1 97.30(17) . 2_658 ?
O4 U2 U2 91.66(17) . 2_658 ?
O4 U2 O5 90.3(2) . . ?
O4 U2 O5 92.4(2) . 2_658 ?
O4 U2 O6 93.53(19) . 2_658 ?
O4 U2 O7 88.0(2) . 2_658 ?
O4 U2 O9 91.9(2) . . ?
O4 U2 C1 92.0(2) . 2_658 ?
O6 U2 U1 38.97(10) 2_658 2_658 ?
O6 U2 U2 106.43(10) 2_658 2_658 ?
O6 U2 C1 25.42(16) 2_658 2_658 ?
O3 U2 U1 83.64(16) . 2_658 ?
O3 U2 U2 91.08(17) . 2_658 ?
O3 U2 O5 89.7(2) . 2_658 ?
O3 U2 O5 92.0(2) . . ?
O3 U2 O4 177.3(2) . . ?
O3 U2 O6 85.59(19) . 2_658 ?
O3 U2 O7 89.4(2) . 2_658 ?
O3 U2 O9 86.5(2) . . ?
O3 U2 C1 86.1(2) . 2_658 ?
O7 U2 U1 88.94(11) 2_658 2_658 ?
O7 U2 U2 156.28(11) 2_658 2_658 ?
O7 U2 O6 49.98(15) 2_658 2_658 ?
O7 U2 C1 24.62(17) 2_658 2_658 ?
O9 U2 U1 162.05(12) . 2_658 ?
O9 U2 U2 127.73(12) . 2_658 ?
O9 U2 O6 125.34(15) . 2_658 ?
O9 U2 O7 75.97(17) . 2_658 ?
O9 U2 C1 100.09(19) . 2_658 ?
C1 U2 U1 64.34(14) 2_658 2_658 ?
C1 U2 U2 131.84(14) 2_658 2_658 ?
O15 U3 O15 180.0(3) . 2_648 ?
O15 U3 C37 88.4(2) . . ?
O15 U3 C37 88.4(2) 2_648 2_648 ?
O15 U3 C37 91.6(2) . 2_648 ?
O15 U3 C37 91.6(2) 2_648 . ?
O14 U3 O15 118.06(17) . 2_648 ?
O14 U3 O15 61.94(17) . . ?
O14 U3 O15 61.94(17) 2_648 2_648 ?
O14 U3 O15 118.06(17) 2_648 . ?
O14 U3 O14 180.00(11) 2_648 . ?
O14 U3 O13 52.50(19) . . ?
O14 U3 O13 52.50(19) 2_648 2_648 ?
O14 U3 O13 127.50(19) 2_648 . ?
O14 U3 O13 127.50(19) . 2_648 ?
O14 U3 C37 26.5(2) 2_648 2_648 ?
O14 U3 C37 153.5(2) 2_648 . ?
O14 U3 C37 153.5(2) . 2_648 ?
O14 U3 C37 26.5(2) . . ?
O13 U3 O15 65.59(18) . 2_648 ?
O13 U3 O15 114.41(18) . . ?
O13 U3 O15 65.59(18) 2_648 . ?
O13 U3 O15 114.41(18) 2_648 2_648 ?
O13 U3 O13 180.0 2_648 . ?
O13 U3 C37 26.2(2) 2_648 2_648 ?
O13 U3 C37 26.2(2) . . ?
O13 U3 C37 153.8(2) 2_648 . ?
O13 U3 C37 153.8(2) . 2_648 ?
O12 U3 O15 88.9(2) . . ?
O12 U3 O15 91.1(2) 2_648 . ?
O12 U3 O15 91.1(2) . 2_648 ?
O12 U3 O15 88.9(2) 2_648 2_648 ?
O12 U3 O14 88.4(2) . 2_648 ?
O12 U3 O14 91.6(2) 2_648 2_648 ?
O12 U3 O14 88.4(2) 2_648 . ?
O12 U3 O14 91.6(2) . . ?
O12 U3 O13 89.2(2) . 2_648 ?
O12 U3 O13 89.2(2) 2_648 . ?
O12 U3 O13 90.8(2) . . ?
O12 U3 O13 90.8(2) 2_648 2_648 ?
O12 U3 O12 180.0 . 2_648 ?
O12 U3 C37 86.7(2) . 2_648 ?
O12 U3 C37 93.3(2) . . ?
O12 U3 C37 86.7(2) 2_648 . ?
O12 U3 C37 93.3(3) 2_648 2_648 ?
C37 U3 C37 180.00(6) 2_648 . ?
U1 O5 U2 134.7(2) . . ?
U1 O5 U2 117.68(17) . 2_658 ?
U2 O5 U2 106.58(16) 2_658 . ?
U1 O6 U2 97.07(14) . 2_658 ?
C1 O6 U1 171.9(4) . . ?
C1 O6 U2 89.7(4) . 2_658 ?
C23 O11 U1 93.4(4) . 2_757 ?
U3 O15 H15A 109.8 . . ?
U3 O15 H15B 109.7 . . ?
H15A O15 H15B 104.4 . . ?
C23 O10 U1 93.1(4) . 2_757 ?
C16 O8 U1 153.3(5) . . ?
C1 O7 U2 101.0(4) . 2_658 ?
C16 O9 U2 131.6(5) . . ?
C37 O14 U3 94.9(5) . . ?
C37 O13 U3 91.6(5) . . ?
C13 N1 C14 118.8(7) . . ?
O11 C23 U1 60.0(3) . 2_757 ?
O11 C23 C21 119.4(6) . . ?
O10 C23 U1 60.5(3) . 2_757 ?
O10 C23 O11 120.5(6) . . ?
O10 C23 C21 120.0(6) . . ?
C21 C23 U1 178.0(5) . 2_757 ?
C21 C22 H22 120.3 . . ?
C21 C22 C17 119.3(6) . . ?
C17 C22 H22 120.3 . . ?
C18 C19 H19 120.2 . . ?
C18 C19 C20 119.6(6) . . ?
C20 C19 H19 120.2 . . ?
O14 C37 U3 58.7(4) . . ?
O14 C37 C34 117.8(8) . . ?
O13 C37 U3 62.2(4) . . ?
O13 C37 O14 120.4(7) . . ?
O13 C37 C34 121.7(7) . . ?
C34 C37 U3 169.0(6) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 C19 120.4(6) . . ?
C17 C18 H18 119.8 . . ?
C26 C27 H27 120.5 . . ?
C28 C27 H27 120.5 . . ?
C28 C27 C26 118.9(9) . . ?
O6 C1 U2 64.9(3) . 2_658 ?
O6 C1 C2 122.6(6) . . ?
O7 C1 U2 54.4(3) . 2_658 ?
O7 C1 O6 119.1(6) . . ?
O7 C1 C2 118.3(6) . . ?
C2 C1 U2 170.9(5) . 2_658 ?
C22 C21 C23 119.2(6) . . ?
C20 C21 C23 119.9(6) . . ?
C20 C21 C22 120.9(6) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.6(6) . . ?
C21 C20 H20 120.2 . . ?
C28 N2 C24 119.9(8) . . ?
C28 N2 H2 125(5) . . ?
C24 N2 H2 116(5) . . ?
C2 C8 H8 119.7 . . ?
C2 C8 C7 120.6(7) . . ?
C7 C8 H8 119.7 . . ?
C36 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
C34 C35 C36 118.5(8) . . ?
C22 C17 C16 120.5(6) . . ?
C18 C17 C22 120.1(6) . . ?
C18 C17 C16 119.5(6) . . ?
C35 C36 H36 119.4 . . ?
C31 C36 C35 121.3(8) . . ?
C31 C36 H36 119.4 . . ?
C8 C2 C1 119.9(6) . . ?
C8 C2 C3 118.9(6) . . ?
C3 C2 C1 121.3(6) . . ?
C8 C7 H7 119.4 . . ?
C5 C7 C8 121.2(8) . . ?
C5 C7 H7 119.4 . . ?
C35 C34 C37 120.0(7) . . ?
C33 C34 C37 119.3(7) . . ?
C33 C34 C35 120.7(7) . . ?
O8 C16 C17 118.1(6) . . ?
O9 C16 O8 122.6(7) . . ?
O9 C16 C17 119.4(6) . . ?
C27 C26 C29 118.1(8) . . ?
C25 C26 C27 118.5(7) . . ?
C25 C26 C29 123.3(8) . . ?
C27 C28 H28 118.7 . . ?
N2 C28 C27 122.6(9) . . ?
N2 C28 H28 118.7 . . ?
C36 C31 C30 122.5(8) . . ?
C32 C31 C36 118.0(8) . . ?
C32 C31 C30 119.6(9) . . ?
N1 C14 H14 119.3 . . ?
N1 C14 C15 121.5(8) . . ?
C15 C14 H14 119.3 . . ?
C7 C5 C9 118.5(8) . . ?
C4 C5 C7 117.7(7) . . ?
C4 C5 C9 123.8(8) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(7) . . ?
C4 C3 H3 120.0 . . ?
C34 C33 H33 119.9 . . ?
C34 C33 C32 120.2(8) . . ?
C32 C33 H33 119.9 . . ?
N1 C13 H13 118.3 . . ?
N1 C13 C12 123.3(8) . . ?
C12 C13 H13 118.3 . . ?
C26 C25 H25 120.3 . . ?
C26 C25 C24 119.4(8) . . ?
C24 C25 H25 120.3 . . ?
C5 C9 H9 116.3 . . ?
C10 C9 C5 127.3(10) . . ?
C10 C9 H9 116.3 . . ?
C26 C29 H29 116.4 . . ?
C30 C29 C26 127.2(9) . . ?
C30 C29 H29 116.4 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C11 119.8(8) . . ?
C11 C15 H15 120.1 . . ?
C5 C4 C3 121.6(7) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C9 C10 H10 116.0 . . ?
C9 C10 C11 128.0(10) . . ?
C11 C10 H10 116.0 . . ?
C31 C30 H30 117.6 . . ?
C29 C30 C31 124.8(9) . . ?
C29 C30 H30 117.6 . . ?
C15 C11 C10 126.3(8) . . ?
C12 C11 C15 116.8(7) . . ?
C12 C11 C10 116.9(8) . . ?
C31 C32 C33 121.3(9) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 H32 119.4 . . ?
C13 C12 C11 119.9(8) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
N2 C24 C25 120.6(9) . . ?
N2 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?

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 O11 C23 O10 -1.1(8) 2_757 . . . ?
U1 O11 C23 C21 177.7(6) 2_757 . . . ?
U1 O10 C23 O11 1.0(8) 2_757 . . . ?
U1 O10 C23 C21 -177.7(6) 2_757 . . . ?
U1 O8 C16 O9 27.3(17) . . . . ?
U1 O8 C16 C17 -152.3(9) . . . . ?
U2 O6 C1 O7 4.9(7) 2_658 . . . ?
U2 O6 C1 C2 -174.0(7) 2_658 . . . ?
U2 O7 C1 O6 -5.5(8) 2_658 . . . ?
U2 O7 C1 C2 173.5(6) 2_658 . . . ?
U2 O9 C16 O8 5.1(12) . . . . ?
U2 O9 C16 C17 -175.2(5) . . . . ?
U3 O14 C37 O13 -8.3(9) . . . . ?
U3 O14 C37 C34 168.0(6) . . . . ?
U3 O13 C37 O14 8.0(9) . . . . ?
U3 O13 C37 C34 -168.2(7) . . . . ?
U3 C37 C34 C35 -119(3) . . . . ?
U3 C37 C34 C33 61(3) . . . . ?
O6 C1 C2 C8 170.3(7) . . . . ?
O6 C1 C2 C3 -9.6(12) . . . . ?
O11 C23 C21 C22 -173.8(7) . . . . ?
O11 C23 C21 C20 8.0(11) . . . . ?
O10 C23 C21 C22 5.0(11) . . . . ?
O10 C23 C21 C20 -173.2(7) . . . . ?
O7 C1 C2 C8 -8.6(11) . . . . ?
O7 C1 C2 C3 171.4(7) . . . . ?
O14 C37 C34 C35 173.0(8) . . . . ?
O14 C37 C34 C33 -7.3(12) . . . . ?
O13 C37 C34 C35 -10.7(13) . . . . ?
O13 C37 C34 C33 169.0(9) . . . . ?
N1 C14 C15 C11 1.3(13) . . . . ?
N1 C13 C12 C11 1.0(14) . . . . ?
C23 C21 C20 C19 176.8(7) . . . . ?
C22 C21 C20 C19 -1.4(11) . . . . ?
C22 C17 C16 O8 5.2(11) . . . . ?
C22 C17 C16 O9 -174.4(7) . . . . ?
C19 C18 C17 C22 -2.4(11) . . . . ?
C19 C18 C17 C16 178.1(7) . . . . ?
C37 C34 C33 C32 -177.3(9) . . . . ?
C18 C19 C20 C21 0.2(11) . . . . ?
C18 C17 C16 O8 -175.3(7) . . . . ?
C18 C17 C16 O9 5.0(11) . . . . ?
C27 C26 C25 C24 -2.3(15) . . . . ?
C27 C26 C29 C30 174.0(10) . . . . ?
C1 C2 C3 C4 179.2(8) . . . . ?
C21 C22 C17 C18 1.3(11) . . . . ?
C21 C22 C17 C16 -179.2(7) . . . . ?
C20 C19 C18 C17 1.7(11) . . . . ?
C8 C2 C3 C4 -0.7(12) . . . . ?
C8 C7 C5 C9 178.7(8) . . . . ?
C8 C7 C5 C4 1.0(13) . . . . ?
C35 C36 C31 C30 -177.3(9) . . . . ?
C35 C36 C31 C32 2.2(14) . . . . ?
C35 C34 C33 C32 2.4(14) . . . . ?
C17 C22 C21 C23 -177.6(7) . . . . ?
C17 C22 C21 C20 0.6(11) . . . . ?
C36 C35 C34 C37 178.9(8) . . . . ?
C36 C35 C34 C33 -0.8(13) . . . . ?
C36 C31 C30 C29 -16.0(16) . . . . ?
C36 C31 C32 C33 -0.6(15) . . . . ?
C2 C8 C7 C5 -1.9(13) . . . . ?
C2 C3 C4 C5 -0.2(13) . . . . ?
C7 C8 C2 C1 -178.2(7) . . . . ?
C7 C8 C2 C3 1.8(12) . . . . ?
C7 C5 C9 C10 177.8(10) . . . . ?
C7 C5 C4 C3 0.1(13) . . . . ?
C34 C35 C36 C31 -1.5(14) . . . . ?
C34 C33 C32 C31 -1.7(16) . . . . ?
C26 C27 C28 N2 0.3(15) . . . . ?
C26 C25 C24 N2 0.9(16) . . . . ?
C26 C29 C30 C31 175.1(9) . . . . ?
C28 C27 C26 C25 1.7(14) . . . . ?
C28 C27 C26 C29 179.4(9) . . . . ?
C28 N2 C24 C25 1.1(15) . . . . ?
C14 N1 C13 C12 0.1(14) . . . . ?
C14 C15 C11 C10 -178.6(8) . . . . ?
C14 C15 C11 C12 -0.2(12) . . . . ?
C5 C9 C10 C11 -178.3(8) . . . . ?
C13 N1 C14 C15 -1.2(13) . . . . ?
C25 C26 C29 C30 -8.4(17) . . . . ?
C9 C5 C4 C3 -177.5(8) . . . . ?
C9 C10 C11 C15 6.9(16) . . . . ?
C9 C10 C11 C12 -171.5(10) . . . . ?
C29 C26 C25 C24 -179.9(9) . . . . ?
C15 C11 C12 C13 -0.9(12) . . . . ?
C4 C5 C9 C10 -4.6(16) . . . . ?
C10 C11 C12 C13 177.7(8) . . . . ?
C30 C31 C32 C33 178.9(9) . . . . ?
C32 C31 C30 C29 164.5(10) . . . . ?
C24 N2 C28 C27 -1.7(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2432777'
loop_
_audit_author_name
_audit_author_address
'Lei Mei'
; Institute of High Energy Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2025-07-07 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_audit_creation_date             2025-04-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H13 N3 O10 U'
_chemical_formula_sum            'C15 H13 N3 O10 U'
_chemical_formula_weight         633.31
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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                   9.1929(14)
_cell_length_b                   9.9213(15)
_cell_length_c                   10.3415(14)
_cell_angle_alpha                78.599(6)
_cell_angle_beta                 83.835(6)
_cell_angle_gamma                82.331(7)
_cell_volume                     913.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.89
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.950
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0875 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.8384.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.303
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27400
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.181
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3675
_reflns_number_total             3957
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3957
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0260
_refine_ls_restrained_S_all      1.043
_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)+(0.0175P)²+3.6686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0620
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C9(H9), C6(H6), C12(H12), C14(H14), C7(H7), C13(H13),
 C4(H4), C3(H3)
1.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 1.24977(2) 0.26080(2) 0.13998(2) 0.02145(6) Uani 1 1 d . . . . .
O9 O 1.1986(3) 0.0931(3) 0.0058(3) 0.0278(7) Uani 1 1 d . . . . .
O8 O 1.4098(4) 0.1716(4) -0.0416(3) 0.0300(7) Uani 1 1 d . . . . .
O5 O 1.3515(4) 0.4256(4) 0.2476(3) 0.0289(7) Uani 1 1 d . . . . .
O3 O 1.0729(4) 0.3382(4) 0.3090(3) 0.0307(8) Uani 1 1 d . . . . .
O6 O 1.4981(4) 0.3427(4) 0.0991(3) 0.0306(8) Uani 1 1 d . . . . .
O2 O 1.3160(4) 0.1176(4) 0.2575(3) 0.0305(7) Uani 1 1 d . . . . .
O4 O 1.0041(4) 0.1949(4) 0.1960(4) 0.0308(8) Uani 1 1 d . . . . .
O10 O 1.3550(4) 0.0155(4) -0.1444(3) 0.0335(8) Uani 1 1 d . . . . .
O1 O 1.1795(4) 0.4042(4) 0.0243(3) 0.0296(7) Uani 1 1 d . . . . .
N3 N 1.3234(4) 0.0899(4) -0.0643(4) 0.0236(8) Uani 1 1 d . . . . .
N2 N 1.4774(4) 0.4245(4) 0.1817(4) 0.0250(8) Uani 1 1 d . . . . .
C8 C 0.4133(5) 0.2795(5) 0.5901(5) 0.0257(9) Uani 1 1 d . . . . .
H8 H 0.4032 0.3331 0.6578 0.031 Uiso 1 1 calc R U . . .
O7 O 1.5692(4) 0.4947(4) 0.1977(4) 0.0365(8) Uani 1 1 d . . . . .
C11 C 0.1221(5) 0.3298(5) 0.7408(5) 0.0262(9) Uani 1 1 d . . . . .
H11 H 0.1892 0.3943 0.7426 0.031 Uiso 1 1 calc R U . . .
N1 N -0.1044(4) 0.2424(4) 0.8192(4) 0.0280(9) Uani 1 1 d . . . . .
C5 C 0.5567(5) 0.2701(5) 0.5128(4) 0.0239(9) Uani 1 1 d . . . . .
C10 C 0.1563(5) 0.2318(5) 0.6571(4) 0.0226(9) Uani 1 1 d . . . . .
C9 C 0.2953(5) 0.2201(5) 0.5747(4) 0.0232(9) Uani 1 1 d . . . . .
H9 H 0.3023 0.1674 0.5065 0.028 Uiso 1 1 calc R U . . .
C6 C 0.5931(5) 0.1844(5) 0.4184(5) 0.0254(9) Uani 1 1 d . . . . .
H6 H 0.5246 0.1257 0.4051 0.031 Uiso 1 1 calc R U . . .
C12 C -0.0067(5) 0.3322(5) 0.8192(5) 0.0296(10) Uani 1 1 d . . . . .
H12 H -0.0282 0.3988 0.8751 0.035 Uiso 1 1 calc R U . . .
C14 C 0.0516(5) 0.1423(5) 0.6579(5) 0.0288(10) Uani 1 1 d . . . . .
H14 H 0.0690 0.0760 0.6015 0.035 Uiso 1 1 calc R U . . .
C7 C 0.7273(5) 0.1847(5) 0.3448(5) 0.0248(9) Uani 1 1 d . . . . .
H7 H 0.7498 0.1282 0.2794 0.030 Uiso 1 1 calc R U . . .
C13 C -0.0760(5) 0.1486(5) 0.7389(6) 0.0321(11) Uani 1 1 d . . . . .
H13 H -0.1455 0.0859 0.7386 0.039 Uiso 1 1 calc R U . . .
C4 C 0.6615(5) 0.3527(5) 0.5341(5) 0.0253(9) Uani 1 1 d . . . . .
H4 H 0.6389 0.4097 0.5990 0.030 Uiso 1 1 calc R U . . .
C1 C 0.9755(5) 0.2676(5) 0.2869(5) 0.0248(9) Uani 1 1 d . . . . .
C15 C -0.2388(6) 0.2460(6) 0.9098(7) 0.0464(15) Uani 1 1 d . . . . .
H15A H -0.2229 0.1780 0.9912 0.070 Uiso 1 1 calc R U . . .
H15B H -0.3205 0.2238 0.8673 0.070 Uiso 1 1 calc R U . . .
H15C H -0.2626 0.3387 0.9314 0.070 Uiso 1 1 calc R U . . .
C3 C 0.7972(5) 0.3521(5) 0.4617(5) 0.0255(9) Uani 1 1 d . . . . .
H3 H 0.8672 0.4084 0.4769 0.031 Uiso 1 1 calc R U . . .
C2 C 0.8308(5) 0.2683(5) 0.3663(4) 0.0232(9) Uani 1 1 d . . . . .


_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 O9 2.485(3) . ?
U1 O8 2.488(3) . ?
U1 O5 2.478(3) . ?
U1 O3 2.424(3) . ?
U1 O6 2.490(3) . ?
U1 O2 1.764(3) . ?
U1 O4 2.414(3) . ?
U1 O1 1.766(3) . ?
U1 N3 2.932(4) . ?
U1 N2 2.929(4) . ?
U1 C1 2.801(4) . ?
O9 N3 1.290(5) . ?
O8 N3 1.276(5) . ?
O5 N2 1.278(5) . ?
O3 C1 1.273(6) . ?
O6 N2 1.273(5) . ?
O4 C1 1.280(6) . ?
O10 N3 1.203(5) . ?
N2 O7 1.208(5) . ?
C8 H8 0.9500 . ?
C8 C5 1.467(6) . ?
C8 C9 1.340(7) . ?
C11 H11 0.9500 . ?
C11 C10 1.409(6) . ?
C11 C12 1.362(7) . ?
N1 C12 1.346(7) . ?
N1 C13 1.349(7) . ?
N1 C15 1.469(6) . ?
C5 C6 1.404(6) . ?
C5 C4 1.406(6) . ?
C10 C9 1.463(6) . ?
C10 C14 1.393(7) . ?
C9 H9 0.9500 . ?
C6 H6 0.9500 . ?
C6 C7 1.379(6) . ?
C12 H12 0.9500 . ?
C14 H14 0.9500 . ?
C14 C13 1.367(7) . ?
C7 H7 0.9500 . ?
C7 C2 1.404(6) . ?
C13 H13 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.384(6) . ?
C1 C2 1.485(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C2 1.397(6) . ?

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
O9 U1 O8 51.47(10) . . ?
O9 U1 O6 116.89(10) . . ?
O9 U1 N3 25.90(10) . . ?
O9 U1 N2 142.45(11) . . ?
O9 U1 C1 95.76(12) . . ?
O8 U1 O6 65.52(11) . . ?
O8 U1 N3 25.59(11) . . ?
O8 U1 N2 91.02(11) . . ?
O8 U1 C1 147.15(12) . . ?
O5 U1 O9 168.10(11) . . ?
O5 U1 O8 116.65(11) . . ?
O5 U1 O6 51.21(10) . . ?
O5 U1 N3 142.21(11) . . ?
O5 U1 N2 25.65(10) . . ?
O5 U1 C1 96.14(12) . . ?
O3 U1 O9 122.73(11) . . ?
O3 U1 O8 174.02(10) . . ?
O3 U1 O5 69.16(11) . . ?
O3 U1 O6 120.35(11) . . ?
O3 U1 N3 148.63(11) . . ?
O3 U1 N2 94.81(11) . . ?
O3 U1 C1 26.98(12) . . ?
O6 U1 N3 91.01(11) . . ?
O6 U1 N2 25.57(10) . . ?
O6 U1 C1 147.33(12) . . ?
O2 U1 O9 87.59(14) . . ?
O2 U1 O8 91.24(14) . . ?
O2 U1 O5 92.25(14) . . ?
O2 U1 O3 89.88(14) . . ?
O2 U1 O6 90.78(14) . . ?
O2 U1 O4 89.24(14) . . ?
O2 U1 O1 178.72(15) . . ?
O2 U1 N3 88.63(13) . . ?
O2 U1 N2 92.26(14) . . ?
O2 U1 C1 89.32(15) . . ?
O4 U1 O9 68.65(11) . . ?
O4 U1 O8 120.02(11) . . ?
O4 U1 O5 123.25(11) . . ?
O4 U1 O3 54.11(11) . . ?
O4 U1 O6 174.45(10) . . ?
O4 U1 N3 94.54(11) . . ?
O4 U1 N2 148.89(11) . . ?
O4 U1 C1 27.13(12) . . ?
O1 U1 O9 92.49(13) . . ?
O1 U1 O8 89.81(14) . . ?
O1 U1 O5 87.94(14) . . ?
O1 U1 O3 89.00(14) . . ?
O1 U1 O6 90.32(14) . . ?
O1 U1 O4 89.60(14) . . ?
O1 U1 N3 92.00(13) . . ?
O1 U1 N2 88.46(13) . . ?
O1 U1 C1 89.40(15) . . ?
N2 U1 N3 116.56(11) . . ?
C1 U1 N3 121.65(12) . . ?
C1 U1 N2 121.79(12) . . ?
N3 O9 U1 96.8(2) . . ?
N3 O8 U1 97.0(2) . . ?
N2 O5 U1 97.3(2) . . ?
C1 O3 U1 93.2(3) . . ?
N2 O6 U1 96.8(2) . . ?
C1 O4 U1 93.5(3) . . ?
O9 N3 U1 57.3(2) . . ?
O8 N3 U1 57.4(2) . . ?
O8 N3 O9 114.6(3) . . ?
O10 N3 U1 177.5(3) . . ?
O10 N3 O9 122.3(4) . . ?
O10 N3 O8 123.1(4) . . ?
O5 N2 U1 57.0(2) . . ?
O6 N2 U1 57.6(2) . . ?
O6 N2 O5 114.6(4) . . ?
O7 N2 U1 178.5(3) . . ?
O7 N2 O5 122.4(4) . . ?
O7 N2 O6 123.0(4) . . ?
C5 C8 H8 116.7 . . ?
C9 C8 H8 116.7 . . ?
C9 C8 C5 126.6(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C12 C11 C10 120.2(5) . . ?
C12 N1 C13 119.8(4) . . ?
C12 N1 C15 119.2(5) . . ?
C13 N1 C15 121.0(5) . . ?
C6 C5 C8 123.3(4) . . ?
C6 C5 C4 118.8(4) . . ?
C4 C5 C8 117.9(4) . . ?
C11 C10 C9 122.8(4) . . ?
C14 C10 C11 116.7(4) . . ?
C14 C10 C9 120.4(4) . . ?
C8 C9 C10 123.6(4) . . ?
C8 C9 H9 118.2 . . ?
C10 C9 H9 118.2 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(4) . . ?
C7 C6 H6 119.7 . . ?
C11 C12 H12 119.2 . . ?
N1 C12 C11 121.6(5) . . ?
N1 C12 H12 119.2 . . ?
C10 C14 H14 119.6 . . ?
C13 C14 C10 120.9(5) . . ?
C13 C14 H14 119.6 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C2 120.1(4) . . ?
C2 C7 H7 119.9 . . ?
N1 C13 C14 120.9(4) . . ?
N1 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C5 C4 H4 119.5 . . ?
C3 C4 C5 120.9(4) . . ?
C3 C4 H4 119.5 . . ?
O3 C1 U1 59.8(2) . . ?
O3 C1 O4 119.1(4) . . ?
O3 C1 C2 120.6(4) . . ?
O4 C1 U1 59.4(2) . . ?
O4 C1 C2 120.3(4) . . ?
C2 C1 U1 178.8(3) . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 C3 H3 120.1 . . ?
C4 C3 C2 119.7(4) . . ?
C2 C3 H3 120.1 . . ?
C7 C2 C1 119.8(4) . . ?
C3 C2 C7 119.9(4) . . ?
C3 C2 C1 120.3(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O9 N3 O8 -2.8(4) . . . . ?
U1 O9 N3 O10 177.1(4) . . . . ?
U1 O8 N3 O9 2.8(4) . . . . ?
U1 O8 N3 O10 -177.1(4) . . . . ?
U1 O5 N2 O6 -2.2(4) . . . . ?
U1 O5 N2 O7 178.3(4) . . . . ?
U1 O3 C1 O4 -0.7(5) . . . . ?
U1 O3 C1 C2 178.7(4) . . . . ?
U1 O6 N2 O5 2.2(4) . . . . ?
U1 O6 N2 O7 -178.3(4) . . . . ?
U1 O4 C1 O3 0.7(5) . . . . ?
U1 O4 C1 C2 -178.7(4) . . . . ?
O3 C1 C2 C7 -177.0(4) . . . . ?
O3 C1 C2 C3 3.3(7) . . . . ?
O4 C1 C2 C7 2.4(7) . . . . ?
O4 C1 C2 C3 -177.3(4) . . . . ?
C8 C5 C6 C7 177.1(4) . . . . ?
C8 C5 C4 C3 -178.0(4) . . . . ?
C11 C10 C9 C8 14.1(7) . . . . ?
C11 C10 C14 C13 -1.5(7) . . . . ?
C5 C8 C9 C10 178.8(4) . . . . ?
C5 C6 C7 C2 1.7(7) . . . . ?
C5 C4 C3 C2 -0.1(7) . . . . ?
C10 C11 C12 N1 0.0(7) . . . . ?
C10 C14 C13 N1 0.6(8) . . . . ?
C9 C8 C5 C6 -6.3(8) . . . . ?
C9 C8 C5 C4 172.9(5) . . . . ?
C9 C10 C14 C13 177.2(4) . . . . ?
C6 C5 C4 C3 1.3(7) . . . . ?
C6 C7 C2 C1 179.8(4) . . . . ?
C6 C7 C2 C3 -0.5(7) . . . . ?
C12 C11 C10 C9 -177.4(4) . . . . ?
C12 C11 C10 C14 1.2(7) . . . . ?
C12 N1 C13 C14 0.6(7) . . . . ?
C14 C10 C9 C8 -164.4(5) . . . . ?
C13 N1 C12 C11 -0.9(7) . . . . ?
C4 C5 C6 C7 -2.1(7) . . . . ?
C4 C3 C2 C7 -0.4(7) . . . . ?
C4 C3 C2 C1 179.4(4) . . . . ?
C15 N1 C12 C11 177.5(5) . . . . ?
C15 N1 C13 C14 -177.7(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2432778'
loop_
_audit_author_name
_audit_author_address
'Lei Mei'
; Institute of High Energy Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2025-07-07 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_audit_creation_date             2025-04-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H30 N4 O18 U2, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H36 N6 O18 U2'
_chemical_formula_weight         1388.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.6995(14)
_cell_length_b                   9.0816(4)
_cell_length_c                   19.7705(10)
_cell_angle_alpha                90
_cell_angle_beta                 119.4020(10)
_cell_angle_gamma                90
_cell_volume                     4489.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5050
_cell_measurement_temperature    293.00
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.84
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.289
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6358
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0808 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.8527.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.479
_diffrn_ambient_temperature      293.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3612
_reflns_number_total             5159
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.778
_refine_diff_density_min         -1.778
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5159
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.045
_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)+47.9806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0906
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Restrained distances
 C17-C19
 1.39 with sigma of 0.01
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C4(H4), C3(H3), C11(H11), C9(H9), C18(H18), C6(H6), C13(H13),
 C19(H19), C14(H14), C12(H12)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.37341(2) 0.90158(3) 0.39898(2) 0.03944(10) Uani 1 1 d . . . . .
O6 O 0.4356(3) 0.7764(7) 0.3654(4) 0.0580(17) Uani 1 1 d . . . . .
O3 O 0.3284(2) 0.7689(6) 0.4590(3) 0.0520(15) Uani 1 1 d . . . . .
O4 O 0.3886(2) 0.6493(6) 0.4434(3) 0.0516(15) Uani 1 1 d . . . . .
O5 O 0.4214(2) 1.0117(6) 0.3391(4) 0.0523(15) Uani 1 1 d . . . . .
O1 O 0.3220(2) 0.8507(6) 0.3072(3) 0.0522(15) Uani 1 1 d . . . . .
O2 O 0.4232(2) 0.9582(6) 0.4908(3) 0.0521(15) Uani 1 1 d . . . . .
O8 O 0.3498(2) 1.1709(6) 0.3637(3) 0.0516(15) Uani 1 1 d . . . . .
O7 O 0.3034(2) 1.0568(6) 0.4066(4) 0.0557(16) Uani 1 1 d . . . . .
O9 O 0.2815(3) 1.2801(8) 0.3597(4) 0.0642(18) Uani 1 1 d . . . . .
N2 N 0.3107(3) 1.1722(9) 0.3766(4) 0.0474(17) Uani 1 1 d . . . . .
N1 N 0.3352(3) -0.3826(8) 0.7187(4) 0.0543(19) Uani 1 1 d . . . . .
C16 C 0.4426(3) 0.8929(10) 0.3355(5) 0.0440(19) Uani 1 1 d . . . . .
C1 C 0.3554(3) 0.6485(9) 0.4682(5) 0.043(2) Uani 1 1 d . . . . .
C2 C 0.3479(3) 0.5221(9) 0.5060(4) 0.0389(18) Uani 1 1 d . . . . .
C8 C 0.3274(3) 0.1333(8) 0.6097(4) 0.0394(19) Uani 1 1 d . . . . .
H8 H 0.3033 0.1388 0.6282 0.047 Uiso 1 1 calc R U . . .
C7 C 0.3838(3) 0.4053(10) 0.5260(5) 0.049(2) Uani 1 1 d . . . . .
H7 H 0.4121 0.4120 0.5157 0.059 Uiso 1 1 calc R U . . .
C4 C 0.3000(3) 0.3833(8) 0.5565(4) 0.0401(18) Uani 1 1 d . . . . .
H4 H 0.2718 0.3765 0.5667 0.048 Uiso 1 1 calc R U . . .
C5 C 0.3358(3) 0.2667(9) 0.5753(4) 0.0396(18) Uani 1 1 d . . . . .
C3 C 0.3066(3) 0.5090(9) 0.5226(5) 0.0410(18) Uani 1 1 d . . . . .
H3 H 0.2826 0.5866 0.5107 0.049 Uiso 1 1 calc R U . . .
C11 C 0.3025(3) -0.1507(9) 0.6662(5) 0.047(2) Uani 1 1 d . . . . .
H11 H 0.2770 -0.0773 0.6541 0.056 Uiso 1 1 calc R U . . .
C17 C 0.4735(3) 0.8870(9) 0.2944(5) 0.0436(19) Uani 1 1 d D . . . .
C10 C 0.3441(3) -0.1286(9) 0.6509(5) 0.043(2) Uani 1 1 d . . . . .
C9 C 0.3518(4) 0.0043(10) 0.6165(5) 0.049(2) Uani 1 1 d . . . . .
H9 H 0.3758 -0.0009 0.5976 0.059 Uiso 1 1 calc R U . . .
C18 C 0.4868(4) 1.0176(10) 0.2712(5) 0.052(2) Uani 1 1 d . . . . .
H18 H 0.4777 1.1069 0.2846 0.062 Uiso 1 1 calc R U . . .
C6 C 0.3782(3) 0.2808(10) 0.5605(5) 0.049(2) Uani 1 1 d . . . . .
H6 H 0.4030 0.2050 0.5742 0.059 Uiso 1 1 calc R U . . .
C13 C 0.3750(4) -0.3683(10) 0.7030(6) 0.063(3) Uani 1 1 d . . . . .
H13 H 0.3999 -0.4438 0.7162 0.076 Uiso 1 1 calc R U . . .
C19 C 0.4863(4) 0.7542(9) 0.2717(6) 0.058(3) Uani 1 1 d D . . . .
H19 H 0.4768 0.6654 0.2851 0.070 Uiso 1 1 calc R U . . .
C21 C 0.4958(4) 1.3569(13) 0.3880(8) 0.073(3) Uani 1 1 d . . . . .
C14 C 0.3800(4) -0.2455(10) 0.6681(5) 0.053(2) Uani 1 1 d . . . . .
H14 H 0.4072 -0.2390 0.6555 0.063 Uiso 1 1 calc R U . . .
C12 C 0.2984(4) -0.2788(11) 0.6989(5) 0.054(2) Uani 1 1 d . . . . .
H12 H 0.2696 -0.2933 0.7075 0.065 Uiso 1 1 calc R U . . .
C15 C 0.3308(5) -0.5198(10) 0.7579(6) 0.079(3) Uani 1 1 d . . . . .
H15A H 0.3408 -0.6038 0.7383 0.119 Uiso 1 1 calc R U . . .
H15B H 0.2946 -0.5311 0.7475 0.119 Uiso 1 1 calc R U . . .
H15C H 0.3543 -0.5120 0.8129 0.119 Uiso 1 1 calc R U . . .
C20 C 0.4746(5) 1.3295(16) 0.4378(9) 0.114(5) Uani 1 1 d . . . . .
H20A H 0.4563 1.4158 0.4406 0.171 Uiso 1 1 calc R U . . .
H20B H 0.5031 1.3056 0.4887 0.171 Uiso 1 1 calc R U . . .
H20C H 0.4500 1.2486 0.4179 0.171 Uiso 1 1 calc R U . . .
N3 N 0.5130(5) 1.3797(14) 0.3492(7) 0.114(4) Uani 1 1 d . . . . .


_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 O6 2.467(6) . ?
U1 O3 2.457(5) . ?
U1 O4 2.415(5) . ?
U1 O5 2.427(5) . ?
U1 O1 1.747(6) . ?
U1 O2 1.747(6) . ?
U1 O8 2.542(6) . ?
U1 O7 2.519(5) . ?
U1 N2 2.949(8) . ?
U1 C16 2.825(7) . ?
U1 C1 2.849(8) . ?
O6 C16 1.276(10) . ?
O3 C1 1.300(9) . ?
O4 C1 1.270(9) . ?
O5 C16 1.259(9) . ?
O8 N2 1.268(8) . ?
O7 N2 1.271(9) . ?
O9 N2 1.224(9) . ?
N1 C13 1.328(12) . ?
N1 C12 1.324(11) . ?
N1 C15 1.506(10) . ?
C16 C17 1.467(10) . ?
C1 C2 1.441(11) . ?
C2 C7 1.393(11) . ?
C2 C3 1.384(10) . ?
C8 H8 0.9300 . ?
C8 C5 1.466(10) . ?
C8 C9 1.337(11) . ?
C7 H7 0.9300 . ?
C7 C6 1.370(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.392(11) . ?
C4 C3 1.382(10) . ?
C5 C6 1.389(11) . ?
C3 H3 0.9300 . ?
C11 H11 0.9300 . ?
C11 C10 1.384(11) . ?
C11 C12 1.364(11) . ?
C17 C18 1.392(11) . ?
C17 C19 1.396(8) . ?
C10 C9 1.454(11) . ?
C10 C14 1.399(11) . ?
C9 H9 0.9300 . ?
C18 C18 1.377(15) 2_655 ?
C18 H18 0.9300 . ?
C6 H6 0.9300 . ?
C13 H13 0.9300 . ?
C13 C14 1.354(12) . ?
C19 C19 1.424(16) 2_655 ?
C19 H19 0.9300 . ?
C21 C20 1.409(17) . ?
C21 N3 1.118(15) . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

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
O6 U1 O8 120.01(18) . . ?
O6 U1 O7 168.0(2) . . ?
O6 U1 N2 144.4(2) . . ?
O6 U1 C16 26.8(2) . . ?
O6 U1 C1 94.8(2) . . ?
O3 U1 O6 121.72(19) . . ?
O3 U1 O8 118.16(18) . . ?
O3 U1 O7 67.77(19) . . ?
O3 U1 N2 93.1(2) . . ?
O3 U1 C16 148.5(2) . . ?
O3 U1 C1 27.1(2) . . ?
O4 U1 O6 68.59(18) . . ?
O4 U1 O3 53.37(18) . . ?
O4 U1 O5 121.54(19) . . ?
O4 U1 O8 171.31(17) . . ?
O4 U1 O7 121.10(19) . . ?
O4 U1 N2 146.43(19) . . ?
O4 U1 C16 95.4(2) . . ?
O4 U1 C1 26.3(2) . . ?
O5 U1 O6 53.14(18) . . ?
O5 U1 O3 174.85(19) . . ?
O5 U1 O8 66.96(18) . . ?
O5 U1 O7 117.28(19) . . ?
O5 U1 N2 92.0(2) . . ?
O5 U1 C16 26.4(2) . . ?
O5 U1 C1 147.8(2) . . ?
O1 U1 O6 87.2(2) . . ?
O1 U1 O3 89.8(2) . . ?
O1 U1 O4 92.1(2) . . ?
O1 U1 O5 89.6(2) . . ?
O1 U1 O8 89.7(2) . . ?
O1 U1 O7 85.3(2) . . ?
O1 U1 N2 85.6(2) . . ?
O1 U1 C16 87.1(2) . . ?
O1 U1 C1 91.5(2) . . ?
O2 U1 O6 94.8(2) . . ?
O2 U1 O3 89.9(2) . . ?
O2 U1 O4 89.5(2) . . ?
O2 U1 O5 90.9(2) . . ?
O2 U1 O1 177.7(3) . . ?
O2 U1 O8 88.5(2) . . ?
O2 U1 O7 92.5(2) . . ?
O2 U1 N2 92.2(2) . . ?
O2 U1 C16 94.3(3) . . ?
O2 U1 C1 89.3(2) . . ?
O8 U1 N2 25.34(17) . . ?
O8 U1 C16 93.2(2) . . ?
O8 U1 C1 145.2(2) . . ?
O7 U1 O8 50.57(17) . . ?
O7 U1 N2 25.34(17) . . ?
O7 U1 C16 142.9(2) . . ?
O7 U1 C1 94.8(2) . . ?
C16 U1 N2 117.9(2) . . ?
C16 U1 C1 121.6(2) . . ?
C1 U1 N2 120.2(2) . . ?
C16 O6 U1 92.4(5) . . ?
C1 O3 U1 93.5(5) . . ?
C1 O4 U1 96.3(5) . . ?
C16 O5 U1 94.7(5) . . ?
N2 O8 U1 95.6(5) . . ?
N2 O7 U1 96.6(4) . . ?
O8 N2 U1 59.1(4) . . ?
O8 N2 O7 116.8(7) . . ?
O7 N2 U1 58.1(4) . . ?
O9 N2 U1 173.5(6) . . ?
O9 N2 O8 120.5(8) . . ?
O9 N2 O7 122.7(7) . . ?
C13 N1 C15 120.0(9) . . ?
C12 N1 C13 121.0(8) . . ?
C12 N1 C15 118.9(9) . . ?
O6 C16 U1 60.7(4) . . ?
O6 C16 C17 120.1(7) . . ?
O5 C16 U1 58.9(4) . . ?
O5 C16 O6 119.5(7) . . ?
O5 C16 C17 120.4(8) . . ?
C17 C16 U1 174.0(6) . . ?
O3 C1 U1 59.4(4) . . ?
O3 C1 C2 120.8(7) . . ?
O4 C1 U1 57.4(4) . . ?
O4 C1 O3 116.8(7) . . ?
O4 C1 C2 122.4(8) . . ?
C2 C1 U1 177.8(6) . . ?
C7 C2 C1 118.5(7) . . ?
C3 C2 C1 123.6(8) . . ?
C3 C2 C7 117.9(8) . . ?
C5 C8 H8 117.5 . . ?
C9 C8 H8 117.5 . . ?
C9 C8 C5 125.0(7) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 C2 121.3(7) . . ?
C6 C7 H7 119.4 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0(7) . . ?
C4 C5 C8 119.0(7) . . ?
C6 C5 C8 122.2(8) . . ?
C6 C5 C4 118.8(7) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.4(8) . . ?
C4 C3 H3 119.3 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C12 C11 C10 120.8(8) . . ?
C18 C17 C16 119.3(7) . . ?
C18 C17 C19 118.2(7) . . ?
C19 C17 C16 122.3(8) . . ?
C11 C10 C9 124.6(8) . . ?
C11 C10 C14 116.6(8) . . ?
C14 C10 C9 118.8(8) . . ?
C8 C9 C10 125.6(8) . . ?
C8 C9 H9 117.2 . . ?
C10 C9 H9 117.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C18 C17 121.5(4) 2_655 . ?
C18 C18 H18 119.2 2_655 . ?
C7 C6 C5 120.6(8) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
N1 C13 H13 119.5 . . ?
N1 C13 C14 121.1(9) . . ?
C14 C13 H13 119.5 . . ?
C17 C19 C19 120.3(5) . 2_655 ?
C17 C19 H19 119.9 . . ?
C19 C19 H19 119.9 2_655 . ?
N3 C21 C20 179.1(15) . . ?
C10 C14 H14 120.0 . . ?
C13 C14 C10 120.0(9) . . ?
C13 C14 H14 120.0 . . ?
N1 C12 C11 120.3(8) . . ?
N1 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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 O6 C16 O5 4.5(9) . . . . ?
U1 O6 C16 C17 -173.1(7) . . . . ?
U1 O3 C1 O4 -1.6(8) . . . . ?
U1 O3 C1 C2 177.5(7) . . . . ?
U1 O4 C1 O3 1.6(8) . . . . ?
U1 O4 C1 C2 -177.4(7) . . . . ?
U1 O5 C16 O6 -4.6(9) . . . . ?
U1 O5 C16 C17 173.0(7) . . . . ?
U1 O8 N2 O7 6.7(7) . . . . ?
U1 O8 N2 O9 -172.5(7) . . . . ?
U1 O7 N2 O8 -6.8(7) . . . . ?
U1 O7 N2 O9 172.4(7) . . . . ?
O6 C16 C17 C18 -171.5(8) . . . . ?
O6 C16 C17 C19 14.1(13) . . . . ?
O3 C1 C2 C7 -169.4(8) . . . . ?
O3 C1 C2 C3 11.6(12) . . . . ?
O4 C1 C2 C7 9.6(12) . . . . ?
O4 C1 C2 C3 -169.4(8) . . . . ?
O5 C16 C17 C18 10.9(13) . . . . ?
O5 C16 C17 C19 -163.4(9) . . . . ?
N1 C13 C14 C10 2.7(14) . . . . ?
C16 C17 C18 C18 -176.4(10) . . . 2_655 ?
C16 C17 C19 C19 176.5(11) . . . 2_655 ?
C1 C2 C7 C6 -178.6(8) . . . . ?
C1 C2 C3 C4 177.7(7) . . . . ?
C2 C7 C6 C5 1.1(13) . . . . ?
C8 C5 C6 C7 177.9(8) . . . . ?
C7 C2 C3 C4 -1.3(12) . . . . ?
C4 C5 C6 C7 -1.9(12) . . . . ?
C5 C8 C9 C10 179.6(8) . . . . ?
C5 C4 C3 C2 0.5(12) . . . . ?
C3 C2 C7 C6 0.5(12) . . . . ?
C3 C4 C5 C8 -178.7(7) . . . . ?
C3 C4 C5 C6 1.0(12) . . . . ?
C11 C10 C9 C8 14.7(14) . . . . ?
C11 C10 C14 C13 -4.5(13) . . . . ?
C10 C11 C12 N1 2.0(14) . . . . ?
C9 C8 C5 C4 166.3(8) . . . . ?
C9 C8 C5 C6 -13.5(13) . . . . ?
C9 C10 C14 C13 177.4(8) . . . . ?
C18 C17 C19 C19 2.1(17) . . . 2_655 ?
C13 N1 C12 C11 -4.0(14) . . . . ?
C19 C17 C18 C18 -1.8(16) . . . 2_655 ?
C14 C10 C9 C8 -167.3(8) . . . . ?
C12 N1 C13 C14 1.7(14) . . . . ?
C12 C11 C10 C9 -179.8(8) . . . . ?
C12 C11 C10 C14 2.2(13) . . . . ?
C15 N1 C13 C14 -179.7(9) . . . . ?
C15 N1 C12 C11 177.3(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2432776'
loop_
_audit_author_name
_audit_author_address
'Lei Mei'
; Institute of High Energy Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2025-07-07 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_audit_creation_date             2025-04-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H44 N4 O14 U2'
_chemical_formula_sum            'C56 H44 N4 O14 U2'
_chemical_formula_weight         1473.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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                   17.3390(9)
_cell_length_b                   7.1155(4)
_cell_length_c                   19.8403(12)
_cell_angle_alpha                90
_cell_angle_beta                 99.829(2)
_cell_angle_gamma                90
_cell_volume                     2411.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.89
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.783
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0875 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.8384.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            75510
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_min         2.571
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4678
_reflns_number_total             5579
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.055
_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)+(0.0138P)²+4.1558P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0508
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1.a Rotating group:
 O7(H7A,H7B)
1.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C14(H14), C27(H27), C22(H22), C13(H13), C8(H8), C11(H11),
 C28(H28), C23(H23), C21(H21), C5(H5), C4(H4), C3(H3), C9(H9), C12(H12),
 C19(H19), C17(H17), C7(H7), C18(H18)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.27878(2) 0.47603(2) 0.72943(2) 0.01726(4) Uani 1 1 d . . . . .
O4 O 0.37036(15) 0.4927(4) 0.84020(13) 0.0242(6) Uani 1 1 d . . . . .
O6 O 0.23039(14) 0.4555(4) 0.61329(13) 0.0218(6) Uani 1 1 d . . . . .
O1 O 0.27708(19) 0.7251(4) 0.72482(16) 0.0276(6) Uani 1 1 d . . . . .
O3 O 0.24415(15) 0.4870(4) 0.84130(13) 0.0270(6) Uani 1 1 d . . . . .
O2 O 0.28788(19) 0.2285(4) 0.73476(16) 0.0285(7) Uani 1 1 d . . . . .
O5 O 0.10016(16) 0.4412(4) 0.58907(15) 0.0312(7) Uani 1 1 d . . . . .
N2 N 0.58932(18) 0.5027(4) 0.31228(17) 0.0229(7) Uani 1 1 d . . . . .
O7 O 0.14262(16) 0.4625(5) 0.72132(15) 0.0382(8) Uani 1 1 d . . . . .
H7A H 0.1208 0.4645 0.6784 0.057 Uiso 1 1 d R U . . .
H7B H 0.1263 0.5648 0.7384 0.057 Uiso 1 1 d R U . . .
N1 N -0.0469(2) 0.5584(5) 1.19009(18) 0.0248(7) Uani 1 1 d . . . . .
C24 C 0.4520(2) 0.4920(5) 0.3702(2) 0.0216(8) Uani 1 1 d . . . . .
C26 C 0.5211(2) 0.5714(6) 0.2788(2) 0.0282(9) Uani 1 1 d . . . . .
H26 H 0.5203 0.6243 0.2347 0.034 Uiso 1 1 calc R U . . .
C25 C 0.4524(2) 0.5692(6) 0.3050(2) 0.0268(9) Uani 1 1 d . . . . .
H25 H 0.4058 0.6194 0.2793 0.032 Uiso 1 1 calc R U . . .
C10 C 0.0727(2) 0.5545(5) 1.1110(2) 0.0205(8) Uani 1 1 d . . . . .
C1 C 0.3141(2) 0.4890(5) 0.87340(19) 0.0204(8) Uani 1 1 d . . . . .
C14 C -0.0012(2) 0.6266(5) 1.0858(2) 0.0236(9) Uani 1 1 d . . . . .
H14 H -0.0122 0.6762 1.0407 0.028 Uiso 1 1 calc R U . . .
C27 C 0.5889(2) 0.4257(6) 0.3737(2) 0.0262(9) Uani 1 1 d . . . . .
H27 H 0.6362 0.3739 0.3977 0.031 Uiso 1 1 calc R U . . .
C22 C 0.3100(2) 0.5318(5) 0.37260(19) 0.0204(8) Uani 1 1 d . . . . .
H22 H 0.3036 0.5626 0.3254 0.024 Uiso 1 1 calc R U . . .
C16 C 0.1679(2) 0.5027(5) 0.49830(18) 0.0179(7) Uani 1 1 d . . . . .
C13 C -0.0588(2) 0.6259(5) 1.1266(2) 0.0244(9) Uani 1 1 d . . . . .
H13 H -0.1089 0.6757 1.1083 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2091(2) 0.5133(5) 1.09339(19) 0.0207(8) Uani 1 1 d . . . . .
H8 H 0.2221 0.4969 1.1415 0.025 Uiso 1 1 calc R U . . .
C11 C 0.0844(2) 0.4820(6) 1.1776(2) 0.0263(9) Uani 1 1 d . . . . .
H11 H 0.1337 0.4303 1.1973 0.032 Uiso 1 1 calc R U . . .
C15 C 0.1650(2) 0.4623(5) 0.57167(19) 0.0187(7) Uani 1 1 d . . . . .
C28 C 0.5225(2) 0.4183(6) 0.4038(2) 0.0260(9) Uani 1 1 d . . . . .
H28 H 0.5251 0.3625 0.4477 0.031 Uiso 1 1 calc R U . . .
C23 C 0.3821(2) 0.4889(5) 0.4030(2) 0.0234(8) Uani 1 1 d . . . . .
H23 H 0.3890 0.4532 0.4498 0.028 Uiso 1 1 calc R U . . .
C21 C 0.2373(2) 0.4890(5) 0.47192(19) 0.0183(7) Uani 1 1 d . . . . .
H21 H 0.2837 0.4468 0.5004 0.022 Uiso 1 1 calc R U . . .
C6 C 0.2741(2) 0.4954(5) 1.05507(19) 0.0194(8) Uani 1 1 d . . . . .
C5 C 0.3487(2) 0.4528(5) 1.0908(2) 0.0225(8) Uani 1 1 d . . . . .
H5 H 0.3565 0.4415 1.1392 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4116(2) 0.4269(6) 1.0570(2) 0.0252(9) Uani 1 1 d . . . . .
H4 H 0.4619 0.3982 1.0822 0.030 Uiso 1 1 calc R U . . .
C20 C 0.2391(2) 0.5372(5) 0.40357(19) 0.0186(7) Uani 1 1 d . . . . .
C3 C 0.4011(2) 0.4429(5) 0.9867(2) 0.0232(8) Uani 1 1 d . . . . .
H3 H 0.4442 0.4260 0.9636 0.028 Uiso 1 1 calc R U . . .
C2 C 0.3272(2) 0.4839(5) 0.94957(19) 0.0190(7) Uani 1 1 d . . . . .
C9 C 0.1346(2) 0.5495(5) 1.0690(2) 0.0222(8) Uani 1 1 d . . . . .
H9 H 0.1204 0.5737 1.0214 0.027 Uiso 1 1 calc R U . . .
C12 C 0.0235(2) 0.4866(6) 1.2143(2) 0.0274(9) Uani 1 1 d . . . . .
H12 H 0.0322 0.4359 1.2593 0.033 Uiso 1 1 calc R U . . .
C19 C 0.1703(2) 0.6001(5) 0.3627(2) 0.0226(8) Uani 1 1 d . . . . .
H19 H 0.1707 0.6337 0.3164 0.027 Uiso 1 1 calc R U . . .
C17 C 0.0997(2) 0.5647(5) 0.4557(2) 0.0201(8) Uani 1 1 d . . . . .
H17 H 0.0520 0.5728 0.4732 0.024 Uiso 1 1 calc R U . . .
C7 C 0.2643(2) 0.5112(5) 0.98362(18) 0.0177(7) Uani 1 1 d . . . . .
H7 H 0.2143 0.5407 0.9582 0.021 Uiso 1 1 calc R U . . .
C18 C 0.1012(2) 0.6140(5) 0.3889(2) 0.0252(9) Uani 1 1 d . . . . .
H18 H 0.0548 0.6577 0.3607 0.030 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O4 2.485(3) . ?
U1 O6 2.318(3) . ?
U1 O1 1.775(3) . ?
U1 O3 2.398(3) . ?
U1 O2 1.770(3) . ?
U1 N2 2.566(3) 3_666 ?
U1 O7 2.341(3) . ?
U1 C1 2.819(4) . ?
O4 C1 1.267(4) . ?
O6 C15 1.285(4) . ?
O3 C1 1.270(4) . ?
O5 C15 1.240(4) . ?
N2 U1 2.566(3) 3_666 ?
N2 C26 1.345(5) . ?
N2 C27 1.337(5) . ?
O7 H7A 0.8704 . ?
O7 H7B 0.8702 . ?
N1 C13 1.332(5) . ?
N1 C12 1.335(5) . ?
C24 C25 1.407(5) . ?
C24 C28 1.390(5) . ?
C24 C23 1.471(5) . ?
C26 H26 0.9500 . ?
C26 C25 1.379(5) . ?
C25 H25 0.9500 . ?
C10 C14 1.392(5) . ?
C10 C11 1.401(5) . ?
C10 C9 1.468(5) . ?
C1 C2 1.490(5) . ?
C14 H14 0.9500 . ?
C14 C13 1.389(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.327(5) . ?
C22 C20 1.465(5) . ?
C16 C15 1.493(5) . ?
C16 C21 1.395(5) . ?
C16 C17 1.402(5) . ?
C13 H13 0.9500 . ?
C8 H8 0.9500 . ?
C8 C6 1.468(5) . ?
C8 C9 1.325(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.382(5) . ?
C28 H28 0.9500 . ?
C23 H23 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.405(5) . ?
C6 C5 1.398(5) . ?
C6 C7 1.403(5) . ?
C5 H5 0.9500 . ?
C5 C4 1.387(5) . ?
C4 H4 0.9500 . ?
C4 C3 1.380(6) . ?
C20 C19 1.398(5) . ?
C3 H3 0.9500 . ?
C3 C2 1.395(5) . ?
C2 C7 1.391(5) . ?
C9 H9 0.9500 . ?
C12 H12 0.9500 . ?
C19 H19 0.9500 . ?
C19 C18 1.389(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.376(6) . ?
C7 H7 0.9500 . ?
C18 H18 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 U1 N2 79.18(9) . 3_666 ?
O4 U1 C1 26.71(9) . . ?
O6 U1 O4 161.87(8) . . ?
O6 U1 O3 144.77(9) . . ?
O6 U1 N2 82.79(10) . 3_666 ?
O6 U1 O7 74.89(9) . . ?
O6 U1 C1 171.26(10) . . ?
O1 U1 O4 90.02(12) . . ?
O1 U1 O6 90.66(12) . . ?
O1 U1 O3 90.61(13) . . ?
O1 U1 N2 86.12(13) . 3_666 ?
O1 U1 O7 91.71(14) . . ?
O1 U1 C1 91.05(13) . . ?
O3 U1 O4 53.33(8) . . ?
O3 U1 N2 132.41(10) . 3_666 ?
O3 U1 C1 26.64(9) . . ?
O2 U1 O4 87.58(12) . . ?
O2 U1 O6 90.59(12) . . ?
O2 U1 O1 175.90(13) . . ?
O2 U1 O3 90.62(13) . . ?
O2 U1 N2 90.15(13) . 3_666 ?
O2 U1 O7 92.38(14) . . ?
O2 U1 C1 88.30(13) . . ?
N2 U1 C1 105.88(11) 3_666 . ?
O7 U1 O4 123.20(9) . . ?
O7 U1 O3 69.87(9) . . ?
O7 U1 N2 157.56(10) . 3_666 ?
O7 U1 C1 96.49(10) . . ?
C1 O4 U1 91.5(2) . . ?
C15 O6 U1 140.0(2) . . ?
C1 O3 U1 95.5(2) . . ?
C26 N2 U1 125.2(3) . 3_666 ?
C27 N2 U1 117.5(2) . 3_666 ?
C27 N2 C26 117.3(3) . . ?
U1 O7 H7A 109.4 . . ?
U1 O7 H7B 109.2 . . ?
H7A O7 H7B 104.5 . . ?
C13 N1 C12 117.6(3) . . ?
C25 C24 C23 123.1(4) . . ?
C28 C24 C25 116.5(3) . . ?
C28 C24 C23 120.4(4) . . ?
N2 C26 H26 118.2 . . ?
N2 C26 C25 123.6(4) . . ?
C25 C26 H26 118.2 . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.5(4) . . ?
C26 C25 H25 120.3 . . ?
C14 C10 C11 116.9(4) . . ?
C14 C10 C9 121.5(4) . . ?
C11 C10 C9 121.6(4) . . ?
O4 C1 U1 61.79(19) . . ?
O4 C1 O3 119.6(3) . . ?
O4 C1 C2 122.0(3) . . ?
O3 C1 U1 57.85(18) . . ?
O3 C1 C2 118.4(3) . . ?
C2 C1 U1 175.1(3) . . ?
C10 C14 H14 120.0 . . ?
C13 C14 C10 120.0(4) . . ?
C13 C14 H14 120.0 . . ?
N2 C27 H27 118.6 . . ?
N2 C27 C28 122.8(4) . . ?
C28 C27 H27 118.6 . . ?
C23 C22 H22 116.3 . . ?
C23 C22 C20 127.4(4) . . ?
C20 C22 H22 116.3 . . ?
C21 C16 C15 121.8(3) . . ?
C21 C16 C17 119.3(3) . . ?
C17 C16 C15 118.8(3) . . ?
N1 C13 C14 122.8(4) . . ?
N1 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C6 C8 H8 116.1 . . ?
C9 C8 H8 116.1 . . ?
C9 C8 C6 127.9(4) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 H11 120.4 . . ?
O6 C15 C16 117.4(3) . . ?
O5 C15 O6 124.0(3) . . ?
O5 C15 C16 118.5(3) . . ?
C24 C28 H28 119.8 . . ?
C27 C28 C24 120.4(4) . . ?
C27 C28 H28 119.8 . . ?
C24 C23 H23 117.3 . . ?
C22 C23 C24 125.4(4) . . ?
C22 C23 H23 117.3 . . ?
C16 C21 H21 119.7 . . ?
C16 C21 C20 120.6(3) . . ?
C20 C21 H21 119.7 . . ?
C5 C6 C8 118.8(3) . . ?
C5 C6 C7 118.1(3) . . ?
C7 C6 C8 123.1(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.3 . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.1 . . ?
C21 C20 C22 123.9(3) . . ?
C19 C20 C22 117.4(3) . . ?
C19 C20 C21 118.7(3) . . ?
C4 C3 H3 119.9 . . ?
C4 C3 C2 120.2(4) . . ?
C2 C3 H3 119.9 . . ?
C3 C2 C1 120.6(3) . . ?
C7 C2 C1 119.5(3) . . ?
C7 C2 C3 119.8(3) . . ?
C10 C9 H9 118.0 . . ?
C8 C9 C10 124.0(4) . . ?
C8 C9 H9 118.0 . . ?
N1 C12 C11 123.7(4) . . ?
N1 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
C20 C19 H19 119.6 . . ?
C18 C19 C20 120.8(4) . . ?
C18 C19 H19 119.6 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17 119.7 . . ?
C6 C7 H7 119.6 . . ?
C2 C7 C6 120.7(3) . . ?
C2 C7 H7 119.6 . . ?
C19 C18 H18 119.9 . . ?
C17 C18 C19 120.1(4) . . ?
C17 C18 H18 119.9 . . ?

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 O4 C1 O3 -2.7(4) . . . . ?
U1 O4 C1 C2 176.3(3) . . . . ?
U1 O6 C15 O5 -18.1(6) . . . . ?
U1 O6 C15 C16 160.4(3) . . . . ?
U1 O3 C1 O4 2.8(4) . . . . ?
U1 O3 C1 C2 -176.3(3) . . . . ?
U1 N2 C26 C25 -175.2(3) 3_666 . . . ?
U1 N2 C27 C28 175.4(3) 3_666 . . . ?
O4 C1 C2 C3 -13.7(5) . . . . ?
O4 C1 C2 C7 169.5(3) . . . . ?
O3 C1 C2 C3 165.3(4) . . . . ?
O3 C1 C2 C7 -11.5(5) . . . . ?
N2 C26 C25 C24 0.1(7) . . . . ?
N2 C27 C28 C24 0.2(6) . . . . ?
C26 N2 C27 C28 -1.4(6) . . . . ?
C25 C24 C28 C27 1.1(6) . . . . ?
C25 C24 C23 C22 10.1(6) . . . . ?
C10 C14 C13 N1 0.0(6) . . . . ?
C10 C11 C12 N1 -0.5(6) . . . . ?
C1 C2 C7 C6 176.0(3) . . . . ?
C14 C10 C11 C12 -0.4(6) . . . . ?
C14 C10 C9 C8 167.9(4) . . . . ?
C27 N2 C26 C25 1.2(6) . . . . ?
C22 C20 C19 C18 -178.3(4) . . . . ?
C16 C21 C20 C22 178.2(3) . . . . ?
C16 C21 C20 C19 0.4(5) . . . . ?
C16 C17 C18 C19 0.9(6) . . . . ?
C13 N1 C12 C11 1.2(6) . . . . ?
C8 C6 C5 C4 177.4(4) . . . . ?
C8 C6 C7 C2 -176.8(3) . . . . ?
C11 C10 C14 C13 0.7(6) . . . . ?
C11 C10 C9 C8 -14.0(6) . . . . ?
C15 C16 C21 C20 -176.7(3) . . . . ?
C15 C16 C17 C18 176.1(3) . . . . ?
C28 C24 C25 C26 -1.2(6) . . . . ?
C28 C24 C23 C22 -170.6(4) . . . . ?
C23 C24 C25 C26 178.1(4) . . . . ?
C23 C24 C28 C27 -178.3(4) . . . . ?
C23 C22 C20 C21 -2.5(6) . . . . ?
C23 C22 C20 C19 175.4(4) . . . . ?
C21 C16 C15 O6 15.2(5) . . . . ?
C21 C16 C15 O5 -166.2(4) . . . . ?
C21 C16 C17 C18 -0.8(5) . . . . ?
C21 C20 C19 C18 -0.3(6) . . . . ?
C6 C8 C9 C10 176.5(4) . . . . ?
C6 C5 C4 C3 -0.1(6) . . . . ?
C5 C6 C7 C2 0.4(5) . . . . ?
C5 C4 C3 C2 -0.4(6) . . . . ?
C4 C3 C2 C1 -175.9(4) . . . . ?
C4 C3 C2 C7 0.9(6) . . . . ?
C20 C22 C23 C24 -177.7(4) . . . . ?
C20 C19 C18 C17 -0.4(6) . . . . ?
C3 C2 C7 C6 -0.8(5) . . . . ?
C9 C10 C14 C13 178.8(4) . . . . ?
C9 C10 C11 C12 -178.5(4) . . . . ?
C9 C8 C6 C5 -178.8(4) . . . . ?
C9 C8 C6 C7 -1.6(6) . . . . ?
C12 N1 C13 C14 -0.9(6) . . . . ?
C17 C16 C15 O6 -161.7(3) . . . . ?
C17 C16 C15 O5 16.9(5) . . . . ?
C17 C16 C21 C20 0.2(5) . . . . ?
C7 C6 C5 C4 0.1(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2432779'
loop_
_audit_author_name
_audit_author_address
'Lei Mei'
; Institute of High Energy Physics, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2025-07-07 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_audit_creation_date             2025-04-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_shelx_SHELXL_version_number     2019/3
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H34 N2 O22 U4'
_chemical_formula_sum            'C46 H34 N2 O22 U4'
_chemical_formula_weight         1918.87
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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                   12.9936(13)
_cell_length_b                   14.0664(17)
_cell_length_c                   14.0763(16)
_cell_angle_alpha                100.371(4)
_cell_angle_beta                 96.142(4)
_cell_angle_gamma                95.899(4)
_cell_volume                     2496.5(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.534
_cell_measurement_theta_min      2.995
_shelx_estimated_absorpt_T_max   0.356
_shelx_estimated_absorpt_T_min   0.282
_exptl_absorpt_coefficient_mu    13.018
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.7491.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.553
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            84209
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         2.967
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11137
_reflns_number_total             11491
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         11491
_refine_ls_number_restraints     483
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.032
_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)+6.1676P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0445
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.73094
 0.26906
2. Uiso/Uaniso restraints and constraints
C1 \\sim N1A \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8
\\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim N1A
\\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A
\\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Same fragment restrains
{C1, N1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A,
C15A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C1, N1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15}
4. Others
 Sof(N1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(N1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C18(H18), C19(H19), C21(H21), C22(H22), C26(H26), C27(H27), C29(H29),
  C30(H30), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
 C42(H42), C43(H43), C44(H44), C45(H45), C3A(H3A), C4A(H4A), C6A(H6A), C7A(H7A),
  C8A(H8A), C9A(H9A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C46(H46A,H46B,H46C), C15A(H15D,H15E,H15F)
;
_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 0.29219(2) 0.18337(2) 0.44702(2) 0.01834(4) Uani 1 1 d . . . . .
U2 U 0.25612(2) 0.29180(2) 0.71032(2) 0.01642(4) Uani 1 1 d . . . . .
U3 U 0.24691(2) 0.46752(2) 0.55405(2) 0.01574(4) Uani 1 1 d . . . . .
U4 U 0.18670(2) 0.56989(2) 0.81267(2) 0.01814(4) Uani 1 1 d . . . . .
O1 O 0.3704(3) 0.0345(3) 0.3875(3) 0.0315(9) Uani 1 1 d . . . . .
O2 O 0.3079(4) 0.1120(3) 0.2757(3) 0.0353(10) Uani 1 1 d . . . . .
O3 O 0.1737(3) 0.1089(3) 0.4450(3) 0.0276(8) Uani 1 1 d . . . . .
O4 O 0.4136(3) 0.2526(3) 0.4481(3) 0.0301(8) Uani 1 1 d . . . . .
O5 O 0.2492(3) 0.3072(2) 0.5533(2) 0.0195(7) Uani 1 1 d . . . . .
O6 O 0.1224(3) 0.2383(3) 0.6843(3) 0.0294(8) Uani 1 1 d . . . . .
O7 O 0.3913(3) 0.3359(3) 0.7433(3) 0.0255(8) Uani 1 1 d . . . . .
O8 O 0.2238(3) 0.4442(2) 0.7049(2) 0.0194(7) Uani 1 1 d . . . . .
O9 O 0.1097(3) 0.4693(3) 0.5324(3) 0.0253(8) Uani 1 1 d . . . . .
O10 O 0.3856(3) 0.4776(3) 0.5675(3) 0.0247(8) Uani 1 1 d . . . . .
O11 O 0.0656(3) 0.5707(3) 0.7431(3) 0.0262(8) Uani 1 1 d . . . . .
O12 O 0.3081(3) 0.5730(3) 0.8853(3) 0.0311(9) Uani 1 1 d . . . . .
O13 O 0.2298(4) 0.3296(3) 0.8736(3) 0.0359(10) Uani 1 1 d . . . . .
O14 O 0.1189(3) 0.4413(3) 0.8842(2) 0.0258(8) Uani 1 1 d . . . . .
O15 O 0.2016(3) 0.2684(3) 1.3422(2) 0.0280(8) Uani 1 1 d . . . . .
O16 O 0.2328(3) 0.4303(3) 1.3811(2) 0.0302(9) Uani 1 1 d . . . . .
O17 O 0.2765(3) 0.6366(2) 0.5279(2) 0.0246(8) Uani 1 1 d . . . . .
O18 O 0.2696(3) 0.6355(2) 0.6831(2) 0.0237(7) Uani 1 1 d . . . . .
O19 O 0.2951(3) 1.1387(3) 0.7551(3) 0.0291(8) Uani 1 1 d . . . . .
O20 O 0.3344(3) 1.1414(2) 0.6069(2) 0.0232(7) Uani 1 1 d . . . . .
O21 O 0.1819(4) 0.7466(3) 0.8774(3) 0.0383(10) Uani 1 1 d . . . . .
O22 O 0.1203(3) 0.6425(3) 0.9624(3) 0.0305(9) Uani 1 1 d . . . . .
N2 N -0.0661(3) 1.2661(3) 1.5284(3) 0.0271(9) Uani 1 1 d . . . . .
C1 C 0.3536(4) 0.0426(4) 0.2991(3) 0.0263(10) Uani 1 1 d D U . . .
N1 N 0.5725(11) -0.4924(7) -0.2752(6) 0.020(2) Uani 0.513(7) 1 d D . P A 1
C2 C 0.391(3) -0.033(2) 0.2245(17) 0.026(2) Uani 0.513(7) 1 d D U P A 1
C3 C 0.4192(16) -0.1171(14) 0.2489(13) 0.027(2) Uani 0.513(7) 1 d D U P A 1
H3 H 0.413486 -0.128963 0.312583 0.032 Uiso 0.513(7) 1 calc R U P A 1
C4 C 0.4560(16) -0.1852(11) 0.1816(9) 0.028(2) Uani 0.513(7) 1 d D U P A 1
H4 H 0.480485 -0.241096 0.200809 0.034 Uiso 0.513(7) 1 calc R U P A 1
C5 C 0.4574(13) -0.1727(9) 0.0860(7) 0.028(2) Uani 0.513(7) 1 d D U P A 1
C6 C 0.4266(11) -0.0888(10) 0.0599(10) 0.029(2) Uani 0.513(7) 1 d D U P A 1
H6 H 0.428005 -0.079721 -0.005279 0.035 Uiso 0.513(7) 1 calc R U P A 1
C7 C 0.3930(13) -0.0163(15) 0.1290(15) 0.029(2) Uani 0.513(7) 1 d D U P A 1
H7 H 0.372523 0.041690 0.111313 0.035 Uiso 0.513(7) 1 calc R U P A 1
C8 C 0.4940(9) -0.2487(8) 0.0152(6) 0.031(2) Uani 0.513(7) 1 d D U P A 1
H8 H 0.513776 -0.303751 0.039616 0.037 Uiso 0.513(7) 1 calc R U P A 1
C9 C 0.5027(9) -0.2500(8) -0.0779(7) 0.035(2) Uani 0.513(7) 1 d D U P A 1
H9 H 0.489378 -0.193965 -0.103840 0.042 Uiso 0.513(7) 1 calc R U P A 1
C10 C 0.5321(9) -0.3342(7) -0.1431(7) 0.032(2) Uani 0.513(7) 1 d D U P A 1
C11 C 0.5586(9) -0.4187(8) -0.1117(8) 0.032(2) Uani 0.513(7) 1 d D U P A 1
H11 H 0.563294 -0.422050 -0.044594 0.038 Uiso 0.513(7) 1 calc R U P A 1
C12 C 0.5779(10) -0.4968(8) -0.1787(8) 0.031(2) Uani 0.513(7) 1 d D U P A 1
H12 H 0.595162 -0.554298 -0.157652 0.037 Uiso 0.513(7) 1 calc R U P A 1
C13 C 0.5530(10) -0.4116(8) -0.3066(8) 0.027(2) Uani 0.513(7) 1 d D U P A 1
H13 H 0.553252 -0.408964 -0.373575 0.032 Uiso 0.513(7) 1 calc R U P A 1
C14 C 0.5324(9) -0.3313(8) -0.2420(7) 0.030(2) Uani 0.513(7) 1 d D U P A 1
H14 H 0.518433 -0.273877 -0.265003 0.037 Uiso 0.513(7) 1 calc R U P A 1
C15 C 0.590(3) -0.5779(17) -0.3479(15) 0.028(4) Uani 0.513(7) 1 d D U P A 1
H15A H 0.662384 -0.591590 -0.335234 0.042 Uiso 0.513(7) 1 calc R U P A 1
H15B H 0.577858 -0.563706 -0.413568 0.042 Uiso 0.513(7) 1 calc R U P A 1
H15C H 0.542281 -0.634766 -0.342978 0.042 Uiso 0.513(7) 1 calc R U P A 1
C16 C 0.1685(4) 0.3809(4) 0.9189(3) 0.0235(10) Uani 1 1 d . . . . .
C17 C 0.1634(4) 0.3685(4) 1.0209(3) 0.0200(10) Uani 1 1 d . . . . .
C18 C 0.1387(4) 0.4453(4) 1.0885(3) 0.0207(10) Uani 1 1 d . . . . .
H18 H 0.113229 0.500268 1.068062 0.025 Uiso 1 1 calc R U . . .
C19 C 0.1521(4) 0.4396(4) 1.1865(3) 0.0219(9) Uani 1 1 d . . . . .
H19 H 0.139980 0.492910 1.234155 0.026 Uiso 1 1 calc R U . . .
C20 C 0.1834(4) 0.3561(4) 1.2154(3) 0.0190(10) Uani 1 1 d . . . . .
C21 C 0.1999(4) 0.2764(4) 1.1463(3) 0.0226(10) Uani 1 1 d . . . . .
H21 H 0.216558 0.217935 1.165679 0.027 Uiso 1 1 calc R U . . .
C22 C 0.1917(4) 0.2840(4) 1.0489(3) 0.0243(10) Uani 1 1 d . . . . .
H22 H 0.205421 0.231411 1.001269 0.029 Uiso 1 1 calc R U . . .
C23 C 0.2072(4) 0.3515(4) 1.3203(3) 0.0225(10) Uani 1 1 d . . . . .
C24 C 0.2858(4) 0.6818(3) 0.6152(4) 0.0207(10) Uani 1 1 d . . . . .
C25 C 0.3141(4) 0.7891(3) 0.6368(4) 0.0190(9) Uani 1 1 d . . . . .
C26 C 0.3429(4) 0.8363(4) 0.5632(4) 0.0245(11) Uani 1 1 d . . . . .
H26 H 0.355582 0.799305 0.503094 0.029 Uiso 1 1 calc R U . . .
C27 C 0.3530(4) 0.9362(4) 0.5772(4) 0.0250(11) Uani 1 1 d . . . . .
H27 H 0.374006 0.968440 0.527291 0.030 Uiso 1 1 calc R U . . .
C28 C 0.3322(4) 0.9904(3) 0.6651(4) 0.0207(10) Uani 1 1 d . . . . .
C29 C 0.3099(4) 0.9430(4) 0.7408(4) 0.0241(11) Uani 1 1 d . . . . .
H29 H 0.300059 0.980012 0.801915 0.029 Uiso 1 1 calc R U . . .
C30 C 0.3021(4) 0.8432(4) 0.7277(4) 0.0239(10) Uani 1 1 d . . . . .
H30 H 0.288579 0.811218 0.779867 0.029 Uiso 1 1 calc R U . . .
C31 C 0.3214(4) 1.0959(3) 0.6776(4) 0.0211(10) Uani 1 1 d . . . . .
C32 C 0.1388(4) 0.7299(4) 0.9497(4) 0.0267(11) Uani 1 1 d . . . . .
C33 C 0.1075(4) 0.8107(4) 1.0207(4) 0.0261(11) Uani 1 1 d . . . . .
C34 C 0.0564(5) 0.7893(4) 1.0977(4) 0.0293(12) Uani 1 1 d . . . . .
H34 H 0.042694 0.723462 1.104935 0.035 Uiso 1 1 calc R U . . .
C35 C 0.0252(5) 0.8630(4) 1.1643(4) 0.0324(13) Uani 1 1 d . . . . .
H35 H -0.011095 0.847318 1.215601 0.039 Uiso 1 1 calc R U . . .
C36 C 0.0475(4) 0.9611(4) 1.1555(4) 0.0292(12) Uani 1 1 d . . . . .
C37 C 0.0979(5) 0.9810(4) 1.0783(4) 0.0366(14) Uani 1 1 d . . . . .
H37 H 0.112407 1.046557 1.070670 0.044 Uiso 1 1 calc R U . . .
C38 C 0.1277(5) 0.9064(4) 1.0114(4) 0.0370(14) Uani 1 1 d . . . . .
H38 H 0.162372 0.921760 0.959003 0.044 Uiso 1 1 calc R U . . .
C39 C 0.0191(5) 1.0413(4) 1.2262(4) 0.0320(13) Uani 1 1 d . . . . .
H39 H 0.043451 1.105462 1.219545 0.038 Uiso 1 1 calc R U . . .
C40 C -0.0373(4) 1.0334(4) 1.2987(4) 0.0282(11) Uani 1 1 d . . . . .
H40 H -0.069903 0.970567 1.301760 0.034 Uiso 1 1 calc R U . . .
C41 C -0.0521(4) 1.1156(4) 1.3741(4) 0.0250(10) Uani 1 1 d . . . . .
C42 C -0.0388(4) 1.2132(4) 1.3646(4) 0.0268(11) Uani 1 1 d . . . . .
H42 H -0.024773 1.229054 1.304124 0.032 Uiso 1 1 calc R U . . .
C43 C -0.0458(4) 1.2862(4) 1.4417(4) 0.0263(11) Uani 1 1 d . . . . .
H43 H -0.036140 1.352067 1.433884 0.032 Uiso 1 1 calc R U . . .
C44 C -0.0847(4) 1.1723(4) 1.5389(4) 0.0282(11) Uani 1 1 d . . . . .
H44 H -0.101872 1.158632 1.599364 0.034 Uiso 1 1 calc R U . . .
C45 C -0.0793(4) 1.0967(4) 1.4636(4) 0.0283(11) Uani 1 1 d . . . . .
H45 H -0.094000 1.031397 1.472057 0.034 Uiso 1 1 calc R U . . .
C46 C -0.0705(5) 1.3455(4) 1.6120(4) 0.0336(13) Uani 1 1 d . . . . .
H46A H -0.056697 1.408555 1.592525 0.050 Uiso 1 1 calc R U . . .
H46B H -0.017861 1.341055 1.665841 0.050 Uiso 1 1 calc R U . . .
H46C H -0.139954 1.339379 1.633173 0.050 Uiso 1 1 calc R U . . .
N1A N 0.5802(14) -0.5135(8) -0.2531(7) 0.034(3) Uani 0.487(7) 1 d D U P A 2
C2A C 0.385(3) -0.028(3) 0.2159(18) 0.026(3) Uani 0.487(7) 1 d D U P A 2
C3A C 0.3696(14) -0.0130(15) 0.1222(14) 0.027(2) Uani 0.487(7) 1 d D U P A 2
H3A H 0.336587 0.041166 0.108774 0.032 Uiso 0.487(7) 1 calc R U P A 2
C4A C 0.4011(12) -0.0765(11) 0.0467(11) 0.029(2) Uani 0.487(7) 1 d D U P A 2
H4A H 0.390705 -0.064553 -0.017771 0.034 Uiso 0.487(7) 1 calc R U P A 2
C5A C 0.4477(13) -0.1573(10) 0.0642(7) 0.027(2) Uani 0.487(7) 1 d D U P A 2
C6A C 0.4608(17) -0.1745(12) 0.1580(9) 0.029(3) Uani 0.487(7) 1 d D U P A 2
H6A H 0.488375 -0.231780 0.169977 0.035 Uiso 0.487(7) 1 calc R U P A 2
C7A C 0.4337(18) -0.1080(15) 0.2365(14) 0.029(3) Uani 0.487(7) 1 d D U P A 2
H7A H 0.447752 -0.117367 0.301601 0.035 Uiso 0.487(7) 1 calc R U P A 2
C8A C 0.4752(10) -0.2277(8) -0.0183(7) 0.033(2) Uani 0.487(7) 1 d D U P A 2
H8A H 0.450484 -0.218996 -0.081783 0.039 Uiso 0.487(7) 1 calc R U P A 2
C9A C 0.5305(9) -0.3014(8) -0.0133(7) 0.033(2) Uani 0.487(7) 1 d D U P A 2
H9A H 0.559971 -0.309124 0.049125 0.040 Uiso 0.487(7) 1 calc R U P A 2
C10A C 0.5487(9) -0.3718(8) -0.0986(7) 0.032(2) Uani 0.487(7) 1 d D U P A 2
C11A C 0.5329(9) -0.3564(8) -0.1947(8) 0.033(2) Uani 0.487(7) 1 d D U P A 2
H11A H 0.512034 -0.296687 -0.207440 0.040 Uiso 0.487(7) 1 calc R U P A 2
C12A C 0.5479(12) -0.4286(10) -0.2704(8) 0.035(2) Uani 0.487(7) 1 d D U P A 2
H12A H 0.535483 -0.418938 -0.335529 0.041 Uiso 0.487(7) 1 calc R U P A 2
C13A C 0.5974(11) -0.5299(9) -0.1628(9) 0.035(2) Uani 0.487(7) 1 d D U P A 2
H13A H 0.618612 -0.590227 -0.152305 0.042 Uiso 0.487(7) 1 calc R U P A 2
C14A C 0.5847(9) -0.4595(8) -0.0843(8) 0.033(2) Uani 0.487(7) 1 d D U P A 2
H14A H 0.600390 -0.470528 -0.020031 0.039 Uiso 0.487(7) 1 calc R U P A 2
C15A C 0.596(3) -0.5927(18) -0.3340(16) 0.035(6) Uani 0.487(7) 1 d D U P A 2
H15D H 0.549076 -0.589522 -0.392556 0.053 Uiso 0.487(7) 1 calc R U P A 2
H15E H 0.579747 -0.655957 -0.315399 0.053 Uiso 0.487(7) 1 calc R U P A 2
H15F H 0.668231 -0.584695 -0.347163 0.053 Uiso 0.487(7) 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 U2 3.8426(5) . ?
U1 O1 2.472(4) . ?
U1 O2 2.478(4) . ?
U1 O3 1.765(4) . ?
U1 O4 1.763(4) . ?
U1 O5 2.242(3) . ?
U1 O15 2.355(3) 1_554 ?
U1 O20 2.449(3) 1_545 ?
U2 U3 3.5951(4) . ?
U2 O5 2.252(3) . ?
U2 O6 1.793(4) . ?
U2 O7 1.784(4) . ?
U2 O8 2.239(3) . ?
U2 O13 2.334(3) . ?
U2 O19 2.436(4) 1_545 ?
U2 O20 2.698(3) 1_545 ?
U3 U4 3.8589(5) . ?
U3 O5 2.257(3) . ?
U3 O8 2.253(3) . ?
U3 O9 1.780(4) . ?
U3 O10 1.781(4) . ?
U3 O16 2.379(3) 1_554 ?
U3 O17 2.469(3) . ?
U3 O18 2.677(3) . ?
U4 O8 2.241(3) . ?
U4 O11 1.765(4) . ?
U4 O12 1.778(4) . ?
U4 O14 2.363(3) . ?
U4 O18 2.482(3) . ?
U4 O21 2.498(4) . ?
U4 O22 2.455(4) . ?
O1 C1 1.268(6) . ?
O2 C1 1.267(6) . ?
O13 C16 1.274(7) . ?
O14 C16 1.253(6) . ?
O15 C23 1.258(6) . ?
O16 C23 1.263(6) . ?
O17 C24 1.265(6) . ?
O18 C24 1.274(6) . ?
O19 C31 1.248(6) . ?
O20 C31 1.292(6) . ?
O21 C32 1.258(6) . ?
O22 C32 1.276(6) . ?
N2 C43 1.347(7) . ?
N2 C44 1.354(7) . ?
N2 C46 1.480(6) . ?
C1 C2 1.506(8) . ?
C1 C2A 1.513(8) . ?
N1 C12 1.365(12) . ?
N1 C13 1.330(13) . ?
N1 C15 1.487(8) . ?
C2 C3 1.37(3) . ?
C2 C7 1.41(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(19) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(12) . ?
C5 C6 1.382(14) . ?
C5 C8 1.478(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.415(19) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.324(11) . ?
C9 H9 0.9500 . ?
C9 C10 1.472(11) . ?
C10 C11 1.403(12) . ?
C10 C14 1.401(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.375(13) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.385(13) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.485(6) . ?
C17 C18 1.394(7) . ?
C17 C22 1.389(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.390(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.394(7) . ?
C20 C21 1.396(7) . ?
C20 C23 1.490(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.389(7) . ?
C22 H22 0.9500 . ?
C24 C25 1.484(6) . ?
C25 C26 1.391(7) . ?
C25 C30 1.399(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.375(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.400(7) . ?
C28 C29 1.396(7) . ?
C28 C31 1.486(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.375(7) . ?
C30 H30 0.9500 . ?
C32 C33 1.493(7) . ?
C33 C34 1.392(7) . ?
C33 C38 1.377(8) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.410(8) . ?
C36 C37 1.383(8) . ?
C36 C39 1.470(7) . ?
C37 H37 0.9500 . ?
C37 C38 1.393(7) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C39 C40 1.332(8) . ?
C40 H40 0.9500 . ?
C40 C41 1.465(7) . ?
C41 C42 1.398(8) . ?
C41 C45 1.407(8) . ?
C42 H42 0.9500 . ?
C42 C43 1.371(7) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.372(7) . ?
C45 H45 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
N1A C12A 1.360(13) . ?
N1A C13A 1.331(13) . ?
N1A C15A 1.488(9) . ?
C2A C3A 1.37(3) . ?
C2A C7A 1.41(3) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.386(19) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.390(12) . ?
C5A C6A 1.381(14) . ?
C5A C8A 1.484(9) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.413(19) . ?
C7A H7A 0.9500 . ?
C8A H8A 0.9500 . ?
C8A C9A 1.329(11) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.469(11) . ?
C10A C11A 1.405(13) . ?
C10A C14A 1.403(12) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.378(13) . ?
C12A H12A 0.9500 . ?
C13A H13A 0.9500 . ?
C13A C14A 1.381(13) . ?
C14A H14A 0.9500 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 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 U2 128.05(8) . . ?
O1 U1 O2 52.84(12) . . ?
O2 U1 U2 177.76(11) . . ?
O3 U1 U2 85.56(12) . . ?
O3 U1 O1 88.32(16) . . ?
O3 U1 O2 92.46(16) . . ?
O3 U1 O5 93.71(15) . . ?
O3 U1 O15 88.01(16) . 1_554 ?
O3 U1 O20 83.78(15) . 1_545 ?
O4 U1 U2 95.75(12) . . ?
O4 U1 O1 88.95(16) . . ?
O4 U1 O2 86.27(16) . . ?
O4 U1 O3 177.22(17) . . ?
O4 U1 O5 88.66(15) . . ?
O4 U1 O15 93.89(16) . 1_554 ?
O4 U1 O20 95.43(15) . 1_545 ?
O5 U1 U2 31.31(8) . . ?
O5 U1 O1 158.55(12) . . ?
O5 U1 O2 148.10(12) . . ?
O5 U1 O15 78.51(12) . 1_554 ?
O5 U1 O20 75.20(11) . 1_545 ?
O15 U1 U2 108.37(9) 1_554 . ?
O15 U1 O1 122.92(12) 1_554 . ?
O15 U1 O2 70.46(12) 1_554 . ?
O15 U1 O20 151.82(12) 1_554 1_545 ?
O20 U1 U2 44.23(8) 1_545 . ?
O20 U1 O1 83.82(12) 1_545 . ?
O20 U1 O2 136.64(12) 1_545 . ?
U3 U2 U1 67.453(9) . . ?
O5 U2 U1 31.14(8) . . ?
O5 U2 U3 37.17(8) . . ?
O5 U2 O13 157.53(12) . . ?
O5 U2 O19 119.38(12) . 1_545 ?
O5 U2 O20 70.11(10) . 1_545 ?
O6 U2 U1 88.49(12) . . ?
O6 U2 U3 98.60(12) . . ?
O6 U2 O5 88.10(15) . . ?
O6 U2 O8 95.79(15) . . ?
O6 U2 O13 87.50(17) . . ?
O6 U2 O19 86.78(16) . 1_545 ?
O6 U2 O20 96.05(15) . 1_545 ?
O7 U2 U1 93.19(12) . . ?
O7 U2 U3 87.09(12) . . ?
O7 U2 O5 96.17(15) . . ?
O7 U2 O6 174.28(17) . . ?
O7 U2 O8 89.10(14) . . ?
O7 U2 O13 89.95(17) . . ?
O7 U2 O19 87.81(15) . 1_545 ?
O7 U2 O20 81.90(14) . 1_545 ?
O8 U2 U1 104.17(8) . . ?
O8 U2 U3 36.97(8) . . ?
O8 U2 O5 73.24(10) . . ?
O8 U2 O13 85.30(12) . . ?
O8 U2 O19 167.27(12) . 1_545 ?
O8 U2 O20 140.94(11) . 1_545 ?
O13 U2 U1 170.04(10) . . ?
O13 U2 U3 122.19(10) . . ?
O13 U2 O19 82.35(13) . 1_545 ?
O13 U2 O20 132.28(12) . 1_545 ?
O19 U2 U1 88.33(9) 1_545 . ?
O19 U2 U3 154.90(9) 1_545 . ?
O19 U2 O20 50.58(11) 1_545 1_545 ?
O20 U2 U1 39.29(7) 1_545 . ?
O20 U2 U3 104.34(7) 1_545 . ?
U2 U3 U4 67.425(9) . . ?
O5 U3 U2 37.08(8) . . ?
O5 U3 U4 103.45(8) . . ?
O5 U3 O16 88.10(12) . 1_554 ?
O5 U3 O17 166.13(12) . . ?
O5 U3 O18 138.73(11) . . ?
O8 U3 U2 36.71(8) . . ?
O8 U3 U4 30.75(8) . . ?
O8 U3 O5 72.90(11) . . ?
O8 U3 O16 157.33(13) . 1_554 ?
O8 U3 O17 118.11(11) . . ?
O8 U3 O18 67.86(11) . . ?
O9 U3 U2 100.06(12) . . ?
O9 U3 U4 78.91(11) . . ?
O9 U3 O5 99.23(15) . . ?
O9 U3 O8 87.28(14) . . ?
O9 U3 O10 172.93(17) . . ?
O9 U3 O16 83.61(15) . 1_554 ?
O9 U3 O17 90.09(15) . . ?
O9 U3 O18 91.32(14) . . ?
O10 U3 U2 86.98(12) . . ?
O10 U3 U4 103.47(12) . . ?
O10 U3 O5 86.76(14) . . ?
O10 U3 O8 98.14(15) . . ?
O10 U3 O16 92.89(15) . 1_554 ?
O10 U3 O17 83.36(15) . . ?
O10 U3 O18 86.57(14) . . ?
O16 U3 U2 125.15(9) 1_554 . ?
O16 U3 U4 160.34(10) 1_554 . ?
O16 U3 O17 82.70(12) 1_554 . ?
O16 U3 O18 132.89(12) 1_554 . ?
O17 U3 U2 151.01(8) . . ?
O17 U3 U4 88.35(8) . . ?
O17 U3 O18 50.39(10) . . ?
O18 U3 U2 101.89(7) . . ?
O18 U3 U4 39.69(7) . . ?
O8 U4 U3 30.92(8) . . ?
O8 U4 O14 81.24(12) . . ?
O8 U4 O18 71.72(11) . . ?
O8 U4 O21 153.94(12) . . ?
O8 U4 O22 153.51(12) . . ?
O11 U4 U3 78.94(11) . . ?
O11 U4 O8 91.35(14) . . ?
O11 U4 O12 178.01(17) . . ?
O11 U4 O14 92.13(15) . . ?
O11 U4 O18 87.10(15) . . ?
O11 U4 O21 87.16(17) . . ?
O11 U4 O22 91.16(15) . . ?
O12 U4 U3 102.63(12) . . ?
O12 U4 O8 90.62(15) . . ?
O12 U4 O14 88.49(16) . . ?
O12 U4 O18 93.22(16) . . ?
O12 U4 O21 90.94(17) . . ?
O12 U4 O22 87.22(16) . . ?
O14 U4 U3 109.80(8) . . ?
O14 U4 O18 152.92(11) . . ?
O14 U4 O21 124.81(12) . . ?
O14 U4 O22 72.32(12) . . ?
O18 U4 U3 43.53(8) . . ?
O18 U4 O21 82.21(12) . . ?
O21 U4 U3 124.01(9) . . ?
O22 U4 U3 169.88(10) . . ?
O22 U4 O18 134.75(12) . . ?
O22 U4 O21 52.55(12) . . ?
C1 O1 U1 93.4(3) . . ?
C1 O2 U1 93.1(3) . . ?
U1 O5 U2 117.55(14) . . ?
U1 O5 U3 133.61(15) . . ?
U2 O5 U3 105.75(12) . . ?
U2 O8 U3 106.32(12) . . ?
U2 O8 U4 135.22(14) . . ?
U4 O8 U3 118.33(14) . . ?
C16 O13 U2 133.6(3) . . ?
C16 O14 U4 127.2(3) . . ?
C23 O15 U1 139.4(4) . 1_556 ?
C23 O16 U3 132.2(3) . 1_556 ?
C24 O17 U3 99.6(3) . . ?
U4 O18 U3 96.78(11) . . ?
C24 O18 U3 89.6(3) . . ?
C24 O18 U4 161.9(3) . . ?
C31 O19 U2 100.8(3) . 1_565 ?
U1 O20 U2 96.48(11) 1_565 1_565 ?
C31 O20 U1 156.2(3) . 1_565 ?
C31 O20 U2 87.4(3) . 1_565 ?
C32 O21 U4 93.0(3) . . ?
C32 O22 U4 94.5(3) . . ?
C43 N2 C44 119.8(4) . . ?
C43 N2 C46 120.8(5) . . ?
C44 N2 C46 119.4(5) . . ?
O1 C1 C2 117.3(14) . . ?
O1 C1 C2A 123.4(14) . . ?
O2 C1 O1 120.7(4) . . ?
O2 C1 C2 122.1(14) . . ?
O2 C1 C2A 115.9(14) . . ?
C12 N1 C15 120.6(12) . . ?
C13 N1 C12 121.2(8) . . ?
C13 N1 C15 118.1(12) . . ?
C3 C2 C1 120(2) . . ?
C3 C2 C7 120.5(6) . . ?
C7 C2 C1 119(2) . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.5(13) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 119.7 . . ?
C3 C4 C5 120.6(12) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C8 119.1(9) . . ?
C6 C5 C4 119.3(6) . . ?
C6 C5 C8 121.6(9) . . ?
C5 C6 H6 119.6 . . ?
C5 C6 C7 120.8(12) . . ?
C7 C6 H6 119.6 . . ?
C2 C7 C6 118.2(13) . . ?
C2 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
C5 C8 H8 115.8 . . ?
C9 C8 C5 128.4(9) . . ?
C9 C8 H8 115.8 . . ?
C8 C9 H9 118.5 . . ?
C8 C9 C10 123.1(9) . . ?
C10 C9 H9 118.5 . . ?
C11 C10 C9 123.4(8) . . ?
C14 C10 C9 118.9(9) . . ?
C14 C10 C11 117.6(8) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(9) . . ?
C12 C11 H11 120.2 . . ?
N1 C12 C11 120.7(10) . . ?
N1 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
N1 C13 H13 119.9 . . ?
N1 C13 C14 120.2(9) . . ?
C14 C13 H13 119.9 . . ?
C10 C14 H14 119.7 . . ?
C13 C14 C10 120.5(10) . . ?
C13 C14 H14 119.7 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O13 C16 C17 114.8(5) . . ?
O14 C16 O13 124.3(4) . . ?
O14 C16 C17 120.8(5) . . ?
C18 C17 C16 119.1(4) . . ?
C22 C17 C16 119.4(4) . . ?
C22 C17 C18 121.3(4) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 C17 118.5(4) . . ?
C19 C18 H18 120.8 . . ?
C18 C19 H19 119.8 . . ?
C18 C19 C20 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C21 120.6(4) . . ?
C19 C20 C23 121.4(4) . . ?
C21 C20 C23 117.9(4) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 C20 119.0(5) . . ?
C22 C21 H21 120.5 . . ?
C17 C22 H22 120.0 . . ?
C21 C22 C17 120.0(4) . . ?
C21 C22 H22 120.0 . . ?
O15 C23 O16 124.2(5) . . ?
O15 C23 C20 117.3(4) . . ?
O16 C23 C20 118.5(5) . . ?
O17 C24 O18 120.0(4) . . ?
O17 C24 C25 119.2(4) . . ?
O18 C24 C25 120.8(4) . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 C30 120.1(4) . . ?
C30 C25 C24 120.1(4) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.2(5) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.8(5) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 C31 122.2(4) . . ?
C29 C28 C27 119.6(4) . . ?
C29 C28 C31 117.9(4) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.8 . . ?
C25 C30 H30 120.3 . . ?
C29 C30 C25 119.4(5) . . ?
C29 C30 H30 120.3 . . ?
O19 C31 U2 54.5(2) . 1_565 ?
O19 C31 O20 120.6(4) . . ?
O19 C31 C28 119.3(4) . . ?
O20 C31 U2 66.5(2) . 1_565 ?
O20 C31 C28 120.1(4) . . ?
C28 C31 U2 168.1(4) . 1_565 ?
O21 C32 O22 119.9(5) . . ?
O21 C32 C33 121.1(5) . . ?
O22 C32 C33 119.1(5) . . ?
C34 C33 C32 119.6(5) . . ?
C38 C33 C32 121.4(5) . . ?
C38 C33 C34 119.1(5) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 C33 120.8(5) . . ?
C35 C34 H34 119.6 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.0(5) . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C39 121.7(5) . . ?
C37 C36 C35 118.4(5) . . ?
C37 C36 C39 120.0(5) . . ?
C36 C37 H37 119.4 . . ?
C36 C37 C38 121.1(6) . . ?
C38 C37 H37 119.4 . . ?
C33 C38 C37 120.6(6) . . ?
C33 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C36 C39 H39 116.6 . . ?
C40 C39 C36 126.8(6) . . ?
C40 C39 H39 116.6 . . ?
C39 C40 H40 118.0 . . ?
C39 C40 C41 124.1(5) . . ?
C41 C40 H40 118.0 . . ?
C42 C41 C40 124.6(5) . . ?
C42 C41 C45 116.7(5) . . ?
C45 C41 C40 118.7(5) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 C41 120.7(5) . . ?
C43 C42 H42 119.6 . . ?
N2 C43 C42 121.1(5) . . ?
N2 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
N2 C44 H44 119.4 . . ?
N2 C44 C45 121.1(5) . . ?
C45 C44 H44 119.4 . . ?
C41 C45 H45 119.9 . . ?
C44 C45 C41 120.3(5) . . ?
C44 C45 H45 119.9 . . ?
N2 C46 H46A 109.5 . . ?
N2 C46 H46B 109.5 . . ?
N2 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C12A N1A C15A 121.5(13) . . ?
C13A N1A C12A 121.2(8) . . ?
C13A N1A C15A 117.3(13) . . ?
C3A C2A C1 121(2) . . ?
C3A C2A C7A 120.0(6) . . ?
C7A C2A C1 119(2) . . ?
C2A C3A H3A 119.6 . . ?
C2A C3A C4A 120.8(13) . . ?
C4A C3A H3A 119.6 . . ?
C3A C4A H4A 119.6 . . ?
C3A C4A C5A 120.7(12) . . ?
C5A C4A H4A 119.6 . . ?
C4A C5A C8A 120.0(9) . . ?
C6A C5A C4A 118.9(6) . . ?
C6A C5A C8A 120.9(9) . . ?
C5A C6A H6A 119.5 . . ?
C5A C6A C7A 121.0(12) . . ?
C7A C6A H6A 119.5 . . ?
C2A C7A C6A 118.4(14) . . ?
C2A C7A H7A 120.8 . . ?
C6A C7A H7A 120.8 . . ?
C5A C8A H8A 116.3 . . ?
C9A C8A C5A 127.3(9) . . ?
C9A C8A H8A 116.3 . . ?
C8A C9A H9A 118.0 . . ?
C8A C9A C10A 124.0(9) . . ?
C10A C9A H9A 118.0 . . ?
C11A C10A C9A 123.8(8) . . ?
C14A C10A C9A 118.8(9) . . ?
C14A C10A C11A 117.4(8) . . ?
C10A C11A H11A 120.2 . . ?
C12A C11A C10A 119.5(10) . . ?
C12A C11A H11A 120.2 . . ?
N1A C12A C11A 120.8(10) . . ?
N1A C12A H12A 119.6 . . ?
C11A C12A H12A 119.6 . . ?
N1A C13A H13A 119.9 . . ?
N1A C13A C14A 120.3(10) . . ?
C14A C13A H13A 119.9 . . ?
C10A C14A H14A 119.7 . . ?
C13A C14A C10A 120.6(10) . . ?
C13A C14A H14A 119.7 . . ?
N1A C15A H15D 109.5 . . ?
N1A C15A H15E 109.5 . . ?
N1A C15A H15F 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 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 C1 O2 -1.3(6) . . . . ?
U1 O1 C1 C2 178.2(18) . . . . ?
U1 O1 C1 C2A 179(2) . . . . ?
U1 O2 C1 O1 1.3(6) . . . . ?
U1 O2 C1 C2 -178.1(19) . . . . ?
U1 O2 C1 C2A -178.7(19) . . . . ?
U1 O15 C23 O16 -39.5(8) 1_556 . . . ?
U1 O15 C23 C20 139.5(4) 1_556 . . . ?
U1 O20 C31 U2 -100.2(8) 1_565 . . 1_565 ?
U1 O20 C31 O19 -108.0(8) 1_565 . . . ?
U1 O20 C31 C28 68.8(10) 1_565 . . . ?
U2 O13 C16 O14 -15.1(9) . . . . ?
U2 O13 C16 C17 168.0(4) . . . . ?
U2 O19 C31 O20 8.9(5) 1_565 . . . ?
U2 O19 C31 C28 -168.0(4) 1_565 . . . ?
U2 O20 C31 O19 -7.9(5) 1_565 . . . ?
U2 O20 C31 C28 169.0(4) 1_565 . . . ?
U3 O16 C23 O15 -14.3(8) 1_556 . . . ?
U3 O16 C23 C20 166.6(3) 1_556 . . . ?
U3 O17 C24 O18 -6.1(5) . . . . ?
U3 O17 C24 C25 174.9(4) . . . . ?
U3 O18 C24 O17 5.5(5) . . . . ?
U3 O18 C24 C25 -175.5(4) . . . . ?
U4 O14 C16 O13 -52.5(7) . . . . ?
U4 O14 C16 C17 124.2(4) . . . . ?
U4 O18 C24 O17 -105.5(10) . . . . ?
U4 O18 C24 C25 73.5(12) . . . . ?
U4 O21 C32 O22 2.3(6) . . . . ?
U4 O21 C32 C33 -177.0(5) . . . . ?
U4 O22 C32 O21 -2.3(6) . . . . ?
U4 O22 C32 C33 177.0(4) . . . . ?
O1 C1 C2 C3 15(4) . . . . ?
O1 C1 C2 C7 -167(2) . . . . ?
O1 C1 C2A C3A -177(2) . . . . ?
O1 C1 C2A C7A 2(4) . . . . ?
O2 C1 C2 C3 -166(2) . . . . ?
O2 C1 C2 C7 12(4) . . . . ?
O2 C1 C2A C3A 3(4) . . . . ?
O2 C1 C2A C7A -178(2) . . . . ?
O13 C16 C17 C18 152.4(5) . . . . ?
O13 C16 C17 C22 -22.3(7) . . . . ?
O14 C16 C17 C18 -24.5(8) . . . . ?
O14 C16 C17 C22 160.8(5) . . . . ?
O17 C24 C25 C26 -8.2(7) . . . . ?
O17 C24 C25 C30 165.5(5) . . . . ?
O18 C24 C25 C26 172.8(5) . . . . ?
O18 C24 C25 C30 -13.5(7) . . . . ?
O21 C32 C33 C34 177.6(6) . . . . ?
O21 C32 C33 C38 -2.1(9) . . . . ?
O22 C32 C33 C34 -1.7(8) . . . . ?
O22 C32 C33 C38 178.6(6) . . . . ?
N2 C44 C45 C41 1.2(8) . . . . ?
C1 C2 C3 C4 -178(2) . . . . ?
C1 C2 C7 C6 -179(2) . . . . ?
C1 C2A C3A C4A 179(2) . . . . ?
C1 C2A C7A C6A 178(2) . . . . ?
N1 C13 C14 C10 0.1(18) . . . . ?
C2 C3 C4 C5 -5(3) . . . . ?
C3 C2 C7 C6 -1(4) . . . . ?
C3 C4 C5 C6 3(3) . . . . ?
C3 C4 C5 C8 -178.0(16) . . . . ?
C4 C5 C6 C7 0(2) . . . . ?
C4 C5 C8 C9 -178.9(16) . . . . ?
C5 C6 C7 C2 -1(3) . . . . ?
C5 C8 C9 C10 -174.7(13) . . . . ?
C6 C5 C8 C9 0(2) . . . . ?
C7 C2 C3 C4 4(4) . . . . ?
C8 C5 C6 C7 -179.2(14) . . . . ?
C8 C9 C10 C11 -3.3(19) . . . . ?
C8 C9 C10 C14 175.7(12) . . . . ?
C9 C10 C11 C12 175.4(12) . . . . ?
C9 C10 C14 C13 -175.8(11) . . . . ?
C10 C11 C12 N1 0.7(19) . . . . ?
C11 C10 C14 C13 3.3(17) . . . . ?
C12 N1 C13 C14 -3(2) . . . . ?
C13 N1 C12 C11 3(2) . . . . ?
C14 C10 C11 C12 -3.7(18) . . . . ?
C15 N1 C12 C11 -178(2) . . . . ?
C15 N1 C13 C14 178(2) . . . . ?
C16 C17 C18 C19 -168.7(5) . . . . ?
C16 C17 C22 C21 171.9(5) . . . . ?
C17 C18 C19 C20 -4.0(8) . . . . ?
C18 C17 C22 C21 -2.7(8) . . . . ?
C18 C19 C20 C21 -1.1(8) . . . . ?
C18 C19 C20 C23 174.7(5) . . . . ?
C19 C20 C21 C22 4.3(8) . . . . ?
C19 C20 C23 O15 157.5(5) . . . . ?
C19 C20 C23 O16 -23.4(7) . . . . ?
C20 C21 C22 C17 -2.5(8) . . . . ?
C21 C20 C23 O15 -26.6(7) . . . . ?
C21 C20 C23 O16 152.5(5) . . . . ?
C22 C17 C18 C19 5.9(8) . . . . ?
C23 C20 C21 C22 -171.6(5) . . . . ?
C24 C25 C26 C27 169.5(5) . . . . ?
C24 C25 C30 C29 -168.0(5) . . . . ?
C25 C26 C27 C28 -1.3(8) . . . . ?
C26 C25 C30 C29 5.7(8) . . . . ?
C26 C27 C28 C29 5.3(8) . . . . ?
C26 C27 C28 C31 -167.7(5) . . . . ?
C27 C28 C29 C30 -3.9(8) . . . . ?
C27 C28 C31 U2 119.0(16) . . . 1_565 ?
C27 C28 C31 O19 174.6(5) . . . . ?
C27 C28 C31 O20 -2.3(8) . . . . ?
C28 C29 C30 C25 -1.6(8) . . . . ?
C29 C28 C31 U2 -54.1(18) . . . 1_565 ?
C29 C28 C31 O19 1.5(7) . . . . ?
C29 C28 C31 O20 -175.4(5) . . . . ?
C30 C25 C26 C27 -4.2(8) . . . . ?
C31 C28 C29 C30 169.4(5) . . . . ?
C32 C33 C34 C35 -179.2(5) . . . . ?
C32 C33 C38 C37 179.9(6) . . . . ?
C33 C34 C35 C36 -1.5(9) . . . . ?
C34 C33 C38 C37 0.2(10) . . . . ?
C34 C35 C36 C37 1.8(9) . . . . ?
C34 C35 C36 C39 -177.8(6) . . . . ?
C35 C36 C37 C38 -1.1(10) . . . . ?
C35 C36 C39 C40 -6.8(10) . . . . ?
C36 C37 C38 C33 0.1(11) . . . . ?
C36 C39 C40 C41 172.1(5) . . . . ?
C37 C36 C39 C40 173.6(6) . . . . ?
C38 C33 C34 C35 0.5(9) . . . . ?
C39 C36 C37 C38 178.6(6) . . . . ?
C39 C40 C41 C42 21.0(9) . . . . ?
C39 C40 C41 C45 -157.4(6) . . . . ?
C40 C41 C42 C43 -174.5(5) . . . . ?
C40 C41 C45 C44 174.2(5) . . . . ?
C41 C42 C43 N2 -0.3(8) . . . . ?
C42 C41 C45 C44 -4.4(8) . . . . ?
C43 N2 C44 C45 2.6(8) . . . . ?
C44 N2 C43 C42 -3.1(8) . . . . ?
C45 C41 C42 C43 4.0(8) . . . . ?
C46 N2 C43 C42 178.3(5) . . . . ?
C46 N2 C44 C45 -178.7(5) . . . . ?
N1A C13A C14A C10A 3(2) . . . . ?
C2A C3A C4A C5A 1(3) . . . . ?
C3A C2A C7A C6A -3(5) . . . . ?
C3A C4A C5A C6A 1(3) . . . . ?
C3A C4A C5A C8A 176.4(15) . . . . ?
C4A C5A C6A C7A -4(3) . . . . ?
C4A C5A C8A C9A 171.4(16) . . . . ?
C5A C6A C7A C2A 5(3) . . . . ?
C5A C8A C9A C10A 175.9(14) . . . . ?
C6A C5A C8A C9A -13(3) . . . . ?
C7A C2A C3A C4A 0(4) . . . . ?
C8A C5A C6A C7A -179.4(17) . . . . ?
C8A C9A C10A C11A 16(2) . . . . ?
C8A C9A C10A C14A -164.1(13) . . . . ?
C9A C10A C11A C12A -177.2(12) . . . . ?
C9A C10A C14A C13A 176.5(12) . . . . ?
C10A C11A C12A N1A -2(2) . . . . ?
C11A C10A C14A C13A -4.0(18) . . . . ?
C12A N1A C13A C14A -1(2) . . . . ?
C13A N1A C12A C11A 1(3) . . . . ?
C14A C10A C11A C12A 3.2(19) . . . . ?
C15A N1A C12A C11A 179(2) . . . . ?
C15A N1A C13A C14A 180(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.73094
2 0.26906

# start Validation Reply Form
_vrf_PLAT910_6                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note
RESPONSE: The missing FCF reflections below theta(min) were caused
by the high beamstop theta(min) limit set.
;
