# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2169103'
loop_
_audit_author_name
_audit_author_address
'Christopher L. Cahill'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-04-27 deposited with the CCDC.	2022-06-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H8 Cl6 N2 O6 U2, 2(C4 H5 N2), 2(H2 O)'
_chemical_formula_sum            'C12 H22 Cl6 N6 O8 U2'
_chemical_formula_weight         1067.11

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3929(3)
_cell_length_b                   8.7830(5)
_cell_length_c                   12.2365(6)
_cell_angle_alpha                70.837(2)
_cell_angle_beta                 73.478(2)
_cell_angle_gamma                69.922(3)
_cell_volume                     691.57(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9669
_cell_measurement_theta_min      5.100
_cell_measurement_theta_max      54.241

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_F_000             486
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    12.319
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3556
_exptl_absorpt_correction_T_max  0.5242
_exptl_absorpt_process_details   'SADABS-2016/2, G. Sheldrick'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27388
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.554
_diffrn_reflns_theta_max         27.161
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3069
_reflns_number_gt                3012
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'APEX-3, Bruker-AXS'
_computing_cell_refinement       'SAINT v. 8.38A, Bruker-AXS'
_computing_data_reduction        'SAINT v. 8.38A, Bruker-AXS'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'WinGX, L. Farraguia'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0083P)²+0.7417P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3069
_refine_ls_number_parameters     160
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0110
_refine_ls_R_factor_gt           0.0106
_refine_ls_wR_factor_ref         0.0256
_refine_ls_wR_factor_gt          0.0254
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.18723(2) 0.68052(2) 0.24511(2) 0.01529(3) Uani 1 1 d . . . . .
Cl1 Cl 0.53686(8) 0.46021(7) 0.17338(5) 0.02687(12) Uani 1 1 d . . . . .
Cl2 Cl -0.14912(8) 0.88088(7) 0.17500(4) 0.02300(11) Uani 1 1 d . . . . .
Cl3 Cl 0.00647(8) 0.82974(6) 0.42478(4) 0.01991(10) Uani 1 1 d . . . . .
O1 O 0.3094(2) 0.83868(19) 0.17576(13) 0.0200(3) Uani 1 1 d . . . . .
O2 O 0.0802(2) 0.51366(19) 0.31922(14) 0.0221(3) Uani 1 1 d . . . . .
O5 O 0.1891(2) 0.6429(2) 0.05596(14) 0.0287(4) Uani 1 1 d . . . . .
H5A H 0.095027 0.688041 0.016010 0.043 Uiso 1 1 d R U . . .
H5B H 0.287977 0.593921 0.009040 0.043 Uiso 1 1 d R U . . .
N1 N 0.3966(3) 0.5595(2) 0.40830(16) 0.0192(4) Uani 1 1 d . . . . .
C1 C 0.5499(3) 0.6127(3) 0.4020(2) 0.0222(4) Uani 1 1 d . . . . .
H1 H 0.589486 0.692828 0.333143 0.027 Uiso 1 1 calc R U . . .
C2 C 0.3486(3) 0.4457(3) 0.5072(2) 0.0216(4) Uani 1 1 d . . . . .
H2 H 0.241387 0.404245 0.514949 0.026 Uiso 1 1 calc R U . . .
N3 N 0.3631(3) 0.1399(2) 0.22045(16) 0.0237(4) Uani 1 1 d . . . . .
H3 H 0.449998 0.102771 0.266308 0.028 Uiso 1 1 d R U . . .
N4 N 0.0951(3) 0.2486(2) 0.07975(16) 0.0246(4) Uani 1 1 d . . . . .
C5 C 0.4256(4) 0.1593(3) 0.10427(19) 0.0236(5) Uani 1 1 d . . . . .
H5 H 0.561763 0.135882 0.070681 0.028 Uiso 1 1 calc R U . . .
C6 C 0.2875(4) 0.2139(3) 0.03478(19) 0.0230(5) Uani 1 1 d . . . . .
H6 H 0.330096 0.227565 -0.047914 0.028 Uiso 1 1 calc R U . . .
C7 C 0.0397(4) 0.2282(3) 0.1957(2) 0.0279(5) Uani 1 1 d . . . . .
H7 H -0.096465 0.252181 0.229351 0.033 Uiso 1 1 calc R U . . .
C8 C 0.1734(4) 0.1733(3) 0.26873(19) 0.0258(5) Uani 1 1 d . . . . .
H8 H 0.130860 0.159617 0.351426 0.031 Uiso 1 1 calc R U . . .
O7 O 0.5811(2) 0.0682(3) 0.38301(16) 0.0331(4) Uani 1 1 d D . . . .
H7B H 0.689(3) 0.004(3) 0.379(3) 0.050 Uiso 1 1 d D U . . .
H7A H 0.588(5) 0.161(2) 0.353(3) 0.050 Uiso 1 1 d D 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 O2 1.7640(15) . ?
U1 O1 1.7654(14) . ?
U1 O5 2.4385(15) . ?
U1 N1 2.5979(19) . ?
U1 Cl2 2.6895(6) . ?
U1 Cl3 2.7121(5) . ?
U1 Cl1 2.7543(5) . ?
O5 H5A 0.8699 . ?
O5 H5B 0.8699 . ?
N1 C2 1.340(3) . ?
N1 C1 1.342(3) . ?
C1 C2 1.377(3) 2_666 ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
N3 C8 1.328(3) . ?
N3 C5 1.336(3) . ?
N3 H3 0.8801 . ?
N4 C7 1.329(3) . ?
N4 C6 1.337(3) . ?
C5 C6 1.373(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.378(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
O7 H7B 0.804(17) . ?
O7 H7A 0.791(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 U1 O1 175.82(7) . . ?
O2 U1 O5 90.05(7) . . ?
O1 U1 O5 91.84(6) . . ?
O2 U1 N1 85.91(7) . . ?
O1 U1 N1 90.24(6) . . ?
O5 U1 N1 139.95(6) . . ?
O2 U1 Cl2 91.55(6) . . ?
O1 U1 Cl2 92.59(5) . . ?
O5 U1 Cl2 71.79(4) . . ?
N1 U1 Cl2 148.04(4) . . ?
O2 U1 Cl3 90.72(5) . . ?
O1 U1 Cl3 89.50(5) . . ?
O5 U1 Cl3 150.01(4) . . ?
N1 U1 Cl3 69.97(4) . . ?
Cl2 U1 Cl3 78.219(16) . . ?
O2 U1 Cl1 90.83(5) . . ?
O1 U1 Cl1 86.31(5) . . ?
O5 U1 Cl1 70.30(4) . . ?
N1 U1 Cl1 69.94(4) . . ?
Cl2 U1 Cl1 142.010(17) . . ?
Cl3 U1 Cl1 139.657(17) . . ?
U1 O5 H5A 127.1 . . ?
U1 O5 H5B 127.9 . . ?
H5A O5 H5B 104.5 . . ?
C2 N1 C1 116.4(2) . . ?
C2 N1 U1 120.79(14) . . ?
C1 N1 U1 122.68(15) . . ?
N1 C1 C2 121.7(2) . 2_666 ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 2_666 . ?
N1 C2 C1 121.9(2) . 2_666 ?
N1 C2 H2 119.1 . . ?
C1 C2 H2 119.1 2_666 . ?
C8 N3 C5 121.7(2) . . ?
C8 N3 H3 119.1 . . ?
C5 N3 H3 119.2 . . ?
C7 N4 C6 117.7(2) . . ?
N3 C5 C6 118.1(2) . . ?
N3 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
N4 C6 C5 122.1(2) . . ?
N4 C6 H6 118.9 . . ?
C5 C6 H6 118.9 . . ?
N4 C7 C8 122.1(2) . . ?
N4 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
N3 C8 C7 118.3(2) . . ?
N3 C8 H8 120.9 . . ?
C7 C8 H8 120.9 . . ?
H7B O7 H7A 110(3) . . ?

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
C2 N1 C1 C2 -0.4(3) . . . 2_666 ?
U1 N1 C1 C2 175.93(16) . . . 2_666 ?
C1 N1 C2 C1 0.4(3) . . . 2_666 ?
U1 N1 C2 C1 -176.00(16) . . . 2_666 ?
C8 N3 C5 C6 -0.5(3) . . . . ?
C7 N4 C6 C5 -0.1(3) . . . . ?
N3 C5 C6 N4 0.4(3) . . . . ?
C6 N4 C7 C8 0.0(3) . . . . ?
C5 N3 C8 C7 0.4(3) . . . . ?
N4 C7 C8 N3 -0.1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O5 H5A N4 0.87 1.91 2.766(3) 170.0 2_565 yes
O5 H5B Cl1 0.87 2.35 3.1585(16) 155.0 2_665 yes
C1 H1 Cl2 0.95 2.86 3.742(2) 155.0 1_655 yes
N3 H3 O7 0.88 1.84 2.693(3) 164.1 . yes
C5 H5 Cl2 0.95 2.76 3.390(3) 124.8 1_645 yes
C6 H6 Cl2 0.95 2.85 3.437(2) 120.6 2_565 yes
C6 H6 O1 0.95 2.66 3.347(3) 130.1 2_665 yes
C7 H7 Cl1 0.95 2.83 3.613(3) 140.8 1_455 yes
C8 H8 Cl3 0.95 2.66 3.600(2) 171.6 2_566 yes
O7 H7B Cl2 0.804(17) 2.84(3) 3.2821(18) 117(3) 1_645 yes
O7 H7B Cl3 0.804(17) 2.422(19) 3.1980(19) 162(3) 1_645 yes
O7 H7A Cl1 0.791(17) 2.81(2) 3.528(2) 153(3) . yes

_refine_diff_density_max         0.458
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.075



# start Validation Reply Form
_vrf_PLAT417_shelx               
;
PROBLEM: Short Inter D-H..H-D       H3       ..H7A      .       1.94 Ang.  
RESPONSE: H3 on the lattice pyrazinium cation is involved in a short 
hydrogen bond to O7. H7A is attached to O7 thus both H3 and H7a are 
close to one another. 



;
