# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_cxasap_sadabs_s_aa
_database_code_depnum_ccdc_archive 'CCDC 2353965'
loop_
_audit_author_name
_audit_author_address
'Yingjie Zhang'
;Australian Nuclear Science and Technology Organisation
Australia
;
_audit_update_record             
;
2024-05-08 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_audit_creation_date             2024-02-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'O11 U3, N O3, 2(H4 N)'
_chemical_formula_sum            'H8 N3 O14 U3'
_chemical_formula_weight         988.18
_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
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           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   12.387(3)
_cell_length_b                   7.4410(15)
_cell_length_c                   7.0020(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     645.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.989
_cell_measurement_theta_min      2.738
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    37.627
_exptl_absorpt_correction_T_max  0.4314
_exptl_absorpt_correction_T_min  0.2494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1137 before and 0.0667 after correction.
The Ratio of minimum to maximum transmission is 0.5781.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.085
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7396
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.989
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_min         2.738
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_type           
'silicon double crystal monochromated synchrotron'
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_measurement_device_type  'Eiger Detector'
_diffrn_measurement_method       'π  scans'
_diffrn_radiation_wavelength     0.71079
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                1165
_reflns_number_total             1191
_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       'BlueIce (McPhillips, et al., 2002)'
_computing_data_collection       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.382
_refine_diff_density_min         -2.982
_refine_diff_density_rms         0.432
_refine_ls_abs_structure_details 
;
 Flack x determined using 519 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1191
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0346
_refine_ls_restrained_S_all      1.006
_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)+(0.0577P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0873
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N2-H2A
 1.05 with sigma of 0.02
 N2-H2C
 1.05 with sigma of 0.02
 N2-H2B
 1.05 with sigma of 0.02
 N2-H2D
 1.05 with sigma of 0.02
 H2D-H2A
 1.85 with sigma of 0.02
 H2C-H2A
 1.85 with sigma of 0.02
 H2C-H2D
 1.85 with sigma of 0.02
 H2A-H2B
 1.85 with sigma of 0.02
 H2B-H2C
 1.85 with sigma of 0.02
 H2B-H2D
 1.85 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O6) = Uanis(O7)
Uiso(H2A) = Uiso(H2B) = Uiso(H2C) = Uiso(H2D)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.30860(6) 0.50660(8) 0.4111(2) 0.0137(3) Uani 1 1 d . . . . .
U2 U 0.500000 0.52377(11) 0.83861(11) 0.0146(3) Uani 1 2 d S T P . .
O1 O 0.2951(7) 0.7419(14) 0.355(2) 0.017(2) Uani 1 1 d . . . . .
O2 O 0.3239(9) 0.2693(16) 0.4636(18) 0.018(2) Uani 1 1 d . . . . .
O3 O 0.3327(9) 0.5752(16) 0.7238(17) 0.016(2) Uani 1 1 d . . . . .
O4 O 0.3753(10) 0.4440(15) 0.0862(18) 0.017(2) Uani 1 1 d . . . . .
O5 O 0.500000 0.578(2) 0.467(2) 0.016(3) Uani 1 2 d S T P . .
O6 O 0.500000 0.288(2) 0.773(2) 0.019(3) Uani 1 2 d S T P . .
O7 O 0.500000 0.761(2) 0.912(2) 0.019(3) Uani 1 2 d S T P . .
O8 O 0.4123(10) 0.0704(16) 0.135(2) 0.023(2) Uani 1 1 d . . . . .
O9 O 0.500000 -0.035(2) 0.381(3) 0.021(4) Uani 1 2 d S T P . .
N1 N 0.500000 0.035(3) 0.218(4) 0.016(4) Uani 1 2 d S T P . .
N2 N 0.3353(16) 0.9686(19) 0.727(3) 0.021(3) Uani 1 1 d D . . . .
H2A H 0.365(16) 1.019(18) 0.586(13) 0.04(4) Uiso 1 1 d D . . . .
H2B H 0.251(5) 1.016(17) 0.75(3) 0.04(4) Uiso 1 1 d D . . . .
H2C H 0.335(11) 0.818(4) 0.73(2) 0.04(4) Uiso 1 1 d D . . . .
H2D H 0.389(14) 1.016(16) 0.84(2) 0.04(4) Uiso 1 1 d 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 U1 3.7913(9) 2_564 ?
U1 U1 3.7913(9) 2_565 ?
U1 U2 3.8209(16) . ?
U1 U2 3.8628(12) 2_564 ?
U1 O1 1.802(10) . ?
U1 O2 1.814(12) . ?
U1 O3 2.268(12) . ?
U1 O3 2.270(11) 2_564 ?
U1 O4 2.613(12) 2_565 ?
U1 O4 2.465(13) . ?
U1 O5 2.462(5) . ?
U2 O3 2.255(11) . ?
U2 O3 2.255(11) 4_655 ?
U2 O4 2.397(14) 4_656 ?
U2 O4 2.397(14) 1_556 ?
U2 O5 2.631(17) . ?
U2 O6 1.815(17) . ?
U2 O7 1.840(17) . ?
O8 N1 1.259(19) . ?
O9 N1 1.26(4) . ?
N2 H2A 1.11(3) . ?
N2 H2B 1.12(3) . ?
N2 H2C 1.12(3) . ?
N2 H2D 1.11(3) . ?

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
U1 U1 U1 134.86(4) 2_565 2_564 ?
U1 U1 U2 164.14(3) 2_564 . ?
U1 U1 U2 74.98(3) 2_565 2_564 ?
U1 U1 U2 60.99(3) 2_565 . ?
U1 U1 U2 59.88(3) 2_564 2_564 ?
U2 U1 U2 135.97(4) . 2_564 ?
O1 U1 U1 100.9(4) . 2_565 ?
O1 U1 U1 77.8(5) . 2_564 ?
O1 U1 U2 101.2(4) . . ?
O1 U1 U2 86.4(3) . 2_564 ?
O1 U1 O2 179.0(6) . . ?
O1 U1 O3 90.2(6) . . ?
O1 U1 O3 93.6(5) . 2_564 ?
O1 U1 O4 83.3(4) . 2_565 ?
O1 U1 O4 90.9(5) . . ?
O1 U1 O5 85.0(5) . . ?
O2 U1 U1 101.7(4) . 2_564 ?
O2 U1 U1 80.1(4) . 2_565 ?
O2 U1 U2 94.2(4) . 2_564 ?
O2 U1 U2 79.0(4) . . ?
O2 U1 O3 90.5(5) . . ?
O2 U1 O3 86.4(4) . 2_564 ?
O2 U1 O4 88.2(5) . . ?
O2 U1 O4 97.6(5) . 2_565 ?
O2 U1 O5 94.5(5) . . ?
O3 U1 U1 33.4(3) . 2_565 ?
O3 U1 U1 161.4(3) . 2_564 ?
O3 U1 U1 33.3(3) 2_564 2_564 ?
O3 U1 U1 103.4(3) 2_564 2_565 ?
O3 U1 U2 32.3(3) . . ?
O3 U1 U2 31.3(3) 2_564 2_564 ?
O3 U1 U2 160.1(3) 2_564 . ?
O3 U1 U2 105.7(3) . 2_564 ?
O3 U1 O3 136.0(3) . 2_564 ?
O3 U1 O4 152.8(4) . . ?
O3 U1 O4 68.7(4) 2_564 2_565 ?
O3 U1 O4 71.0(4) 2_564 . ?
O3 U1 O4 68.3(4) . 2_565 ?
O3 U1 O5 70.7(5) . . ?
O3 U1 O5 153.3(5) 2_564 . ?
O4 U1 U1 95.9(3) 2_565 2_564 ?
O4 U1 U1 167.4(3) . 2_565 ?
O4 U1 U1 43.2(3) . 2_564 ?
O4 U1 U1 40.2(3) 2_565 2_565 ?
O4 U1 U2 101.5(3) . 2_564 ?
O4 U1 U2 37.5(3) 2_565 2_564 ?
O4 U1 U2 99.7(3) 2_565 . ?
O4 U1 U2 121.4(3) . . ?
O4 U1 O4 138.8(4) . 2_565 ?
O5 U1 U1 103.1(4) . 2_565 ?
O5 U1 U1 121.5(4) . 2_564 ?
O5 U1 U2 170.6(4) . 2_564 ?
O5 U1 U2 43.1(4) . . ?
O5 U1 O4 82.3(5) . . ?
O5 U1 O4 137.2(5) . 2_565 ?
U1 U2 U1 76.71(4) 4_655 . ?
U1 U2 U1 135.64(4) . 3_565 ?
U1 U2 U1 59.129(16) . 2_565 ?
U1 U2 U1 163.47(5) 3_565 2_565 ?
U1 U2 U1 135.64(4) 4_655 2_565 ?
U1 U2 U1 59.130(16) 4_655 3_565 ?
O3 U2 U1 165.0(3) . 3_565 ?
O3 U2 U1 107.2(3) . 4_655 ?
O3 U2 U1 32.5(3) . . ?
O3 U2 U1 31.5(3) . 2_565 ?
O3 U2 U1 165.0(3) 4_655 2_565 ?
O3 U2 U1 32.5(3) 4_655 4_655 ?
O3 U2 U1 107.2(3) 4_655 . ?
O3 U2 U1 31.5(3) 4_655 3_565 ?
O3 U2 O3 133.5(6) 4_655 . ?
O3 U2 O4 153.1(4) 4_655 1_556 ?
O3 U2 O4 73.0(4) . 1_556 ?
O3 U2 O4 73.0(4) 4_655 4_656 ?
O3 U2 O4 153.1(4) . 4_656 ?
O3 U2 O5 67.8(3) 4_655 . ?
O3 U2 O5 67.8(3) . . ?
O4 U2 U1 41.7(3) 4_656 3_565 ?
O4 U2 U1 41.7(3) 1_556 2_565 ?
O4 U2 U1 99.1(3) 1_556 . ?
O4 U2 U1 121.9(3) 4_656 2_565 ?
O4 U2 U1 163.4(3) 4_656 . ?
O4 U2 U1 99.1(3) 4_656 4_655 ?
O4 U2 U1 163.4(3) 1_556 4_655 ?
O4 U2 U1 121.9(3) 1_556 3_565 ?
O4 U2 O4 80.2(5) 4_656 1_556 ?
O4 U2 O5 138.9(3) 4_656 . ?
O4 U2 O5 138.9(3) 1_556 . ?
O5 U2 U1 39.74(9) . 4_655 ?
O5 U2 U1 97.98(3) . 3_565 ?
O5 U2 U1 97.98(3) . 2_565 ?
O5 U2 U1 39.74(10) . . ?
O6 U2 U1 88.67(9) . 3_565 ?
O6 U2 U1 76.6(4) . 4_655 ?
O6 U2 U1 88.67(9) . 2_565 ?
O6 U2 U1 76.6(4) . . ?
O6 U2 O3 94.2(4) . 4_655 ?
O6 U2 O3 94.2(4) . . ?
O6 U2 O4 86.8(5) . 1_556 ?
O6 U2 O4 86.8(5) . 4_656 ?
O6 U2 O5 84.2(7) . . ?
O6 U2 O7 178.4(7) . . ?
O7 U2 U1 104.6(4) . . ?
O7 U2 U1 91.11(8) . 2_565 ?
O7 U2 U1 104.6(4) . 4_655 ?
O7 U2 U1 91.11(8) . 3_565 ?
O7 U2 O3 86.4(4) . 4_655 ?
O7 U2 O3 86.4(4) . . ?
O7 U2 O4 92.0(5) . 4_656 ?
O7 U2 O4 92.0(5) . 1_556 ?
O7 U2 O5 97.4(7) . . ?
U1 O3 U1 113.3(5) . 2_565 ?
U2 O3 U1 117.2(5) . 2_565 ?
U2 O3 U1 115.3(5) . . ?
U1 O4 U1 96.6(4) . 2_564 ?
U2 O4 U1 100.8(4) 1_554 2_564 ?
U2 O4 U1 146.8(5) 1_554 . ?
U1 O5 U1 148.7(8) 4_655 . ?
U1 O5 U2 97.2(4) 4_655 . ?
U1 O5 U2 97.2(4) . . ?
O8 N1 O8 119(2) 4_655 . ?
O9 N1 O8 120.4(12) . 4_655 ?
O9 N1 O8 120.4(12) . . ?
H2A N2 H2B 110(3) . . ?
H2A N2 H2C 109(3) . . ?
H2A N2 H2D 110(3) . . ?
H2B N2 H2C 108(3) . . ?
H2B N2 H2D 110(3) . . ?
H2C N2 H2D 109(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT971_cxasap_sadabs_s_aa  
;
PROBLEM: Check Calcd Resid. Dens.  0.94Ang From U2              4.39 eA-3  
RESPONSE: The alert arises due to the strong X-ray absorption for U oxides. 
;
_vrf_PLAT973_cxasap_sadabs_s_aa  
;
PROBLEM: Check Calcd Positive Resid. Density on        U2       2.77 eA-3  
RESPONSE: The alert arises due to the strong X-ray absorption for U oxides.
;
_vrf_PLAT090_cxasap_sadabs_s_aa  
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.97 Note  
RESPONSE: The alert arises due to only one-circle data possible.
;
_vrf_PLAT353_cxasap_sadabs_s_aa  
;
PROBLEM: Long   N-H (N0.87,N1.01A)  N2       - H2A      .       1.12 Ang.  
RESPONSE: Possibly due to the hydrogen bonding.
;
_vrf_PLAT430_cxasap_sadabs_s_aa  
;
PROBLEM: Short Inter D...A Contact  O4       ..O8       .       2.84 Ang.  
RESPONSE: Due to the intramolecular interactions.
;
_vrf_PLAT972_cxasap_sadabs_s_aa  
;
PROBLEM: Check Calcd Resid. Dens.  0.85Ang From U1             -3.00 eA-3  
RESPONSE: The alert arises due to the strong X-ray absorption for U oxides.
;
_vrf_PLAT976_cxasap_sadabs_s_aa  
;
PROBLEM: Check Calcd Resid. Dens.  0.92Ang From O5      .      -1.53 eA-3  
RESPONSE: The a;ert arises possibly due to the oxygen atom disorder.
;
# end Validation Reply Form
