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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_NU-1306
_database_code_depnum_ccdc_archive 'CCDC 2203723'
loop_
_audit_author_name
_audit_author_address
'Sylvia L. Hanna'
;Northwestern University
United States of America
;
_audit_update_record             
;
2022-08-26 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_audit_creation_date             2022-06-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        NU-1306
_chemical_formula_moiety         'C87 H48 O32 U4'
_chemical_formula_sum            'C87 H48 O32 U4'
_chemical_formula_weight         2557.37
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           215
_space_group_name_H-M_alt        'P -4 3 m'
_space_group_name_Hall           'P -4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'-x, z, -y'
'x, -y, -z'
'-x, -z, y'
'-z, -y, x'
'-x, y, -z'
'z, -y, -x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'

_cell_length_a                   20.90200(10)
_cell_length_b                   20.90200(10)
_cell_length_c                   20.90200(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9131.95(13)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3351
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      72
_cell_measurement_theta_min      2.1
_shelx_estimated_absorpt_T_max   0.235
_shelx_estimated_absorpt_T_min   0.235
_exptl_absorpt_coefficient_mu    5.098
_exptl_absorpt_correction_T_max  0.19
_exptl_absorpt_correction_T_min  0.13
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.465
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1194
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.117
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33250
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.004
_diffrn_reflns_theta_min         2.114
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                3137
_reflns_number_total             3351
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 
;
 Flack x determined using 1325 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0668
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1453P)²+0.3780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1825
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 U1-O2 = U1-O1
 1.8 with sigma of 0.001
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.29977(3) 0.29977(3) 0.29977(3) 0.0953(4) Uani 1 6 d DS T P . .
O1 O 0.34949(5) 0.34949(5) 0.34949(5) 0.107(6) Uani 1 6 d DS T P . .
O2 O 0.25008(5) 0.25008(5) 0.25008(5) 0.127(9) Uani 1 6 d DS T P . .
O3 O 0.2149(4) 0.3800(4) 0.3069(4) 0.111(3) Uani 1 1 d . . . . .
C1 C 0.1917(7) 0.3592(6) 0.3592(6) 0.099(5) Uani 1 2 d S T P . .
C2 C 0.1414(6) 0.3916(6) 0.3916(6) 0.088(4) Uani 1 2 d S T P . .
C3 C 0.1187(5) 0.4506(5) 0.3711(5) 0.094(3) Uani 1 1 d . . . . .
H3 H 0.136464 0.469026 0.334669 0.113 Uiso 1 1 calc R U . . .
C4 C 0.0704(5) 0.4828(5) 0.4031(5) 0.091(3) Uani 1 1 d . . . . .
H4 H 0.053015 0.519671 0.385394 0.109 Uiso 1 1 calc R U . . .
C5 C 0.0480(5) 0.4608(5) 0.4608(5) 0.074(3) Uani 1 2 d S T P . .
C6 C 0.000000 0.500000 0.500000 0.073(5) Uani 1 8 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O1 1.7999(14) . ?
U1 O2 1.7991(14) . ?
U1 O3 2.445(6) 11 ?
U1 O3 2.445(6) 12 ?
U1 O3 2.445(6) 20 ?
U1 O3 2.445(6) . ?
U1 O3 2.445(6) 22 ?
U1 O3 2.445(6) 24 ?
U1 C1 2.861(14) 12 ?
U1 C1 2.861(14) . ?
U1 C1 2.861(14) 11 ?
O3 C1 1.273(10) . ?
C1 C2 1.422(18) . ?
C2 C3 1.389(11) 22 ?
C2 C3 1.389(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.386(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(11) . ?
C5 C6 1.533(12) . ?

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 O2 180.00(5) . . ?
O1 U1 O3 89.3(3) . 22 ?
O1 U1 O3 89.3(3) . 12 ?
O1 U1 O3 89.3(3) . 24 ?
O1 U1 O3 89.3(3) . 20 ?
O1 U1 O3 89.3(3) . . ?
O1 U1 O3 89.3(3) . 11 ?
O1 U1 C1 87.4(4) . . ?
O1 U1 C1 87.4(4) . 11 ?
O1 U1 C1 87.4(4) . 12 ?
O2 U1 O3 90.7(3) . 11 ?
O2 U1 O3 90.7(3) . 24 ?
O2 U1 O3 90.7(3) . 22 ?
O2 U1 O3 90.7(3) . . ?
O2 U1 O3 90.7(3) . 12 ?
O2 U1 O3 90.7(3) . 20 ?
O2 U1 C1 92.6(4) . . ?
O2 U1 C1 92.6(4) . 11 ?
O2 U1 C1 92.6(4) . 12 ?
O3 U1 O3 172.3(3) 22 12 ?
O3 U1 O3 119.984(11) 24 22 ?
O3 U1 O3 172.3(3) 24 11 ?
O3 U1 O3 172.3(3) . 20 ?
O3 U1 O3 119.983(11) . 11 ?
O3 U1 O3 52.5(3) . 22 ?
O3 U1 O3 119.986(11) . 12 ?
O3 U1 O3 67.5(3) 22 11 ?
O3 U1 O3 52.5(3) 11 20 ?
O3 U1 O3 119.984(11) 24 20 ?
O3 U1 O3 119.984(11) 22 20 ?
O3 U1 O3 52.5(3) 24 12 ?
O3 U1 O3 67.5(3) 12 20 ?
O3 U1 O3 119.984(11) 11 12 ?
O3 U1 O3 67.5(3) . 24 ?
O3 U1 C1 26.29(15) 12 12 ?
O3 U1 C1 146.08(15) 20 . ?
O3 U1 C1 93.73(14) . 12 ?
O3 U1 C1 146.08(16) 24 11 ?
O3 U1 C1 93.73(14) 11 . ?
O3 U1 C1 26.29(15) 11 11 ?
O3 U1 C1 26.29(15) 24 12 ?
O3 U1 C1 146.08(16) 11 12 ?
O3 U1 C1 26.29(15) 22 . ?
O3 U1 C1 93.73(14) 22 11 ?
O3 U1 C1 146.08(15) 12 . ?
O3 U1 C1 93.73(14) 12 11 ?
O3 U1 C1 26.29(15) 20 11 ?
O3 U1 C1 93.73(14) 20 12 ?
O3 U1 C1 146.08(15) . 11 ?
O3 U1 C1 26.29(15) . . ?
O3 U1 C1 146.08(15) 22 12 ?
O3 U1 C1 93.73(14) 24 . ?
C1 U1 C1 119.79(6) 12 11 ?
C1 U1 C1 119.79(6) 11 . ?
C1 U1 C1 119.79(6) 12 . ?
C1 O3 U1 95.4(6) . . ?
O3 C1 U1 58.3(6) . . ?
O3 C1 U1 58.3(6) 22 . ?
O3 C1 O3 116.2(12) . 22 ?
O3 C1 C2 121.9(6) . . ?
O3 C1 C2 121.9(6) 22 . ?
C2 C1 U1 175.6(14) . . ?
C3 C2 C1 121.9(5) 22 . ?
C3 C2 C1 121.9(5) . . ?
C3 C2 C3 115.6(12) . 22 ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 122.0(8) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(8) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C4 118.1(11) 22 . ?
C4 C5 C6 120.9(5) 22 . ?
C4 C5 C6 120.9(5) . . ?
C5 C6 C5 115.4(6) 6_566 5_556 ?
C5 C6 C5 98.2(11) 5_556 3_565 ?
C5 C6 C5 115.4(6) 5_556 . ?
C5 C6 C5 115.4(6) 3_565 . ?
C5 C6 C5 98.2(11) 6_566 . ?
C5 C6 C5 115.4(6) 6_566 3_565 ?

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 O3 C1 O3 -7.0(19) . . . 22 ?
U1 O3 C1 C2 174.8(16) . . . . ?
O3 C1 C2 C3 -176.1(16) . . . 22 ?
O3 C1 C2 C3 6(3) 22 . . 22 ?
O3 C1 C2 C3 176.1(16) 22 . . . ?
O3 C1 C2 C3 -6(3) . . . . ?
C1 C2 C3 C4 -178.9(15) . . . . ?
C2 C3 C4 C5 7(2) . . . . ?
C3 C2 C3 C4 -8(2) 22 . . . ?
C3 C4 C5 C4 -6(2) . . . 22 ?
C3 C4 C5 C6 173.2(11) . . . . ?
C4 C5 C6 C5 89.5(12) 22 . . 6_566 ?
C4 C5 C6 C5 -89.5(12) . . . 6_566 ?
C4 C5 C6 C5 -33.7(10) 22 . . 5_556 ?
C4 C5 C6 C5 147.3(14) . . . 5_556 ?
C4 C5 C6 C5 33.7(10) . . . 3_565 ?
C4 C5 C6 C5 -147.3(14) 22 . . 3_565 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.038 0.280 -0.332 2155.1 241.6 '1 DMF'

_smtbx_masks_void_probe_radius   5.0
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
