# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_gcb_124_5_crys6_0m
_database_code_depnum_ccdc_archive 'CCDC 2528711'
loop_
_audit_author_name
_audit_author_address
'Grant C. Benthin'
;The University of Iowa
United States of America
;
_audit_update_record             
;
2026-02-04 deposited with the CCDC.	2026-04-08 downloaded from the CCDC.
;
_audit_creation_date             2025-12-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/1
loop_
_audit_author_email
''
_chemical_name_common            Studtite
_chemical_name_systematic        'Diaquaperoxo(dioxouranium(VI)) Dihydrate'
_chemical_formula_moiety         'H4 O6 U, 2(H2 O)'
_chemical_formula_sum            'H8 O8 U'
_chemical_formula_weight         374.09
_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'
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        C2/c
_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                   13.9991(13)
_cell_length_b                   6.7481(7)
_cell_length_c                   8.4848(9)
_cell_angle_alpha                90
_cell_angle_beta                 123.143(3)
_cell_angle_gamma                90
_cell_volume                     671.13(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1724
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      3.48
_shelx_estimated_absorpt_T_max   0.889
_shelx_estimated_absorpt_T_min   0.325
_exptl_absorpt_coefficient_mu    24.177
_exptl_absorpt_correction_T_max  0.4288
_exptl_absorpt_correction_T_min  0.2803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0892 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.6537.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.702
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.386
_diffrn_reflns_theta_min         3.476
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_oxdiff_ac3_digest_hkl    41454ae477728725998f2bddbc712ec285e04a
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                443
_reflns_number_total             619
_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         0.797
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       0.00045(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         619
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.220
_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)+14.5849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0478
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O4-H4A
 0.97 with sigma of 0.02
 O4-H4B
 0.97 with sigma of 0.02
 O3-H3A
 0.97 with sigma of 0.02
 O3-H3B
 0.97 with sigma of 0.02
 H3B-H3A
 1.534 with sigma of 0.04
 H4A-H4B
 1.534 with sigma of 0.04
;
_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 0.500000 0.500000 0.500000 0.00783(19) Uani 1 2 d S . P . .
O2 O 0.5639(5) 0.6137(9) 0.3081(8) 0.0087(13) Uani 1 1 d . . . . .
O4 O 0.1569(5) 0.4797(13) 0.4461(8) 0.0109(13) Uani 1 1 d D . . . .
O3 O 0.2954(5) 0.5425(8) 0.3234(8) 0.0101(16) Uani 1 1 d D . . . .
O1 O 0.4902(5) 0.2495(9) 0.4213(8) 0.0096(13) Uani 1 1 d . . . . .
H3A H 0.253(8) 0.50(2) 0.377(13) 0.06(4) Uiso 1 1 d D . . . .
H3B H 0.246(8) 0.51(3) 0.191(6) 0.09(5) Uiso 1 1 d D . . . .
H4A H 0.117(9) 0.358(9) 0.391(19) 0.07(5) Uiso 1 1 d D . . . .
H4B H 0.101(7) 0.582(11) 0.408(16) 0.04(4) Uiso 1 1 d D . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.0088(2) 0.0090(2) 0.0069(2) 0.0005(4) 0.00513(17) 0.0011(4)
O2 0.005(3) 0.013(3) 0.009(3) 0.002(2) 0.005(2) 0.001(2)
O4 0.013(3) 0.007(4) 0.013(3) 0.001(3) 0.007(2) 0.004(3)
O3 0.009(3) 0.014(5) 0.008(3) 0.002(2) 0.005(2) -0.001(2)
O1 0.014(3) 0.005(3) 0.011(3) -0.001(2) 0.009(3) -0.001(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 O2 2.373(6) . ?
U1 O2 2.373(6) 5_666 ?
U1 O2 2.380(6) 2_655 ?
U1 O2 2.380(6) 6_566 ?
U1 O3 2.417(6) 5_666 ?
U1 O3 2.417(6) . ?
U1 O1 1.795(6) 5_666 ?
U1 O1 1.795(6) . ?
O2 O2 1.498(11) 2_655 ?
O4 H4A 0.96(2) . ?
O4 H4B 0.96(2) . ?
O3 H3A 0.97(2) . ?
O3 H3B 0.97(2) . ?

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 O2 180.0(3) . 5_666 ?
O2 U1 O2 36.7(3) 5_666 6_566 ?
O2 U1 O2 143.3(3) . 6_566 ?
O2 U1 O2 143.3(3) 5_666 2_655 ?
O2 U1 O2 36.7(3) . 2_655 ?
O2 U1 O2 180.0 6_566 2_655 ?
O2 U1 O3 107.46(19) . . ?
O2 U1 O3 71.01(19) 2_655 . ?
O2 U1 O3 108.99(19) 6_566 . ?
O2 U1 O3 107.46(19) 5_666 5_666 ?
O2 U1 O3 72.54(19) 5_666 . ?
O2 U1 O3 72.54(19) . 5_666 ?
O2 U1 O3 108.99(19) 2_655 5_666 ?
O2 U1 O3 71.01(19) 6_566 5_666 ?
O3 U1 O3 180.0 . 5_666 ?
O1 U1 O2 88.3(2) . 5_666 ?
O1 U1 O2 88.3(2) 5_666 . ?
O1 U1 O2 91.7(2) 5_666 5_666 ?
O1 U1 O2 91.7(2) . . ?
O1 U1 O2 90.7(2) . 6_566 ?
O1 U1 O2 89.3(2) . 2_655 ?
O1 U1 O2 90.7(2) 5_666 2_655 ?
O1 U1 O2 89.3(2) 5_666 6_566 ?
O1 U1 O3 93.3(2) . . ?
O1 U1 O3 86.7(2) . 5_666 ?
O1 U1 O3 93.3(2) 5_666 5_666 ?
O1 U1 O3 86.7(2) 5_666 . ?
O1 U1 O1 180.0(4) . 5_666 ?
U1 O2 U1 126.4(2) . 2_655 ?
O2 O2 U1 71.4(4) 2_655 2_655 ?
O2 O2 U1 71.9(4) 2_655 . ?
H4A O4 H4B 107(4) . . ?
U1 O3 H3A 120(7) . . ?
U1 O3 H3B 124(8) . . ?
H3A O3 H3B 104(4) . . ?

_shelx_res_file                  
;
TITL gcb_124_5_crys6_0m_a.res in C2/c
    gcb_124_5_crys6_0m.res
    created by SHELXL-2019/1 at 15:14:41 on 30-Dec-2025
REM Old TITL gcb_124_5_crys6_0m_c.res in C2/c
REM SHELXT solution in C2/c: R1 0.056, Rweak 0.001, Alpha 0.019
REM <I/s> 0.757 for 56 systematic absences, Orientation as input
REM Formula found by SHELXT: O8 U
CELL 0.71073 13.9991 6.7481 8.4848 90 123.143 90
ZERR 4 0.0013 0.0007 0.0009 0 0.003 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC H O U
UNIT 32 32 4
DFIX 0.97 O4 H4a
DFIX 0.97 O4 H4b
DFIX 0.97 O3 H3a
DFIX 0.97 O3 H3b
DANG 1.534 H3b H3a
DANG 1.534 H4a H4b

L.S. 50
PLAN  5
SIZE 0.005 0.005 0.06
TEMP -173.15
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\GCB_124_5_crys6_0m.hkl">
REM </olex2.extras>

WGHT    0.000000   14.584900
EXTI    0.000452
FVAR       0.27934
U1    3    0.500000    0.500000    0.500000    10.50000    0.00881    0.00905 =
         0.00691    0.00055    0.00513    0.00107
O2    2    0.563908    0.613675    0.308107    11.00000    0.00527    0.01288 =
         0.00927    0.00184    0.00476    0.00090
O4    2    0.156940    0.479651    0.446088    11.00000    0.01290    0.00673 =
         0.01292    0.00147    0.00692    0.00408
O3    2    0.295353    0.542462    0.323421    11.00000    0.00926    0.01364 =
         0.00824    0.00165    0.00530   -0.00051
O1    2    0.490179    0.249505    0.421256    11.00000    0.01444    0.00527 =
         0.01140   -0.00071    0.00858   -0.00102
H3A   1    0.253167    0.500763    0.377424    11.00000    0.06100
H3B   1    0.245586    0.511597    0.191166    11.00000    0.08700
H4A   1    0.116705    0.357511    0.390899    11.00000    0.07303
H4B   1    0.100984    0.581695    0.407806    11.00000    0.03822
HKLF 4




REM  gcb_124_5_crys6_0m_a.res in C2/c
REM wR2 = 0.0478, GooF = S = 1.226, Restrained GooF = 1.220 for all data
REM R1 = 0.0281 for 443 Fo > 4sig(Fo) and 0.0493 for all 619 data
REM 60 parameters refined using 6 restraints

END

WGHT      0.0000     14.5754

REM Highest difference peak  0.797,  deepest hole -0.901,  1-sigma level  0.197
Q1    1   0.6008  0.5140  0.5818  11.00000  0.05    0.80
Q2    1   0.4298  0.5732  0.4382  11.00000  0.05    0.78
Q3    1   0.2439  0.4488  0.2380  11.00000  0.05    0.70
Q4    1   0.2135  0.3585  0.5212  11.00000  0.05    0.62
Q5    1   0.5138  0.4823  0.3337  11.00000  0.05    0.61
;
_shelx_res_checksum              82218
_olex2_date_sample_completion    2024-09-13
_olex2_date_sample_data_collection 2024-07-08
_olex2_date_sample_submission    2024-07-08
_olex2_submission_original_sample_id GCB-124-5-crys6
_olex2_submission_special_instructions 'No special instructions were received'
_special_details                 
;
Validation Responses to checkCIF Alerts:

PLAT041_ALERT_1_C
PROBLEM: Calc. and Reported SumFormula   Strings Differ
Response: The difference arises because the uranium atom lies on a 
special position in space group C2/c, reducing the number of independent 
atoms in the asymmetric unit. checkCIF interprets this as Z = 2, but 
the correct value is Z = 4, as stated in the CIF and confirmed by the 
UNIT line (H32 O32 U4). The reported formula (H8 O8 U) represents one 
asymmetric unit, while the full unit cell contains four formula units. 
No structural issues are present; the difference is due to the handling 
of special positions and asymmetric unit representation.

PLAT042_ALERT_1_C
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ 
RESPONSE: See response to PLAT041. The reported and calculated moiety 
formulas differ because checkCIF interprets this structure as Z = 2, 
while the correct value is Z = 4. All relevant values differ by the same 
factor, so this alert can be safely ignored.

PLAT906_ALERT_3_C (multiple)
PROBLEM: Large K Value in the Analysis of Variance
RESPONSE: These alerts indicate large K values in the analysis of 
variance (K = 31.109 and K = 3.380). These high K values likely result 
from the presence of heavy atoms (U) and the standard weighting scheme 
used. The refinement is stable (shift/su max = 0.000), with good R-values 
(R1 = 0.0281, wR2 = 0.0478)and no signs of modeling issues. The alerts 
are not considered significant for this structure type.

PLAT975_ALERT_2_C (multiple)
PROBLEM: Check Calcd Resid. Dens.
RESPONSE: The positive residuals near O2 and O3 are likely due to nearby 
hydrogen atoms restrained using DFIX and DANG restraints and the presence 
of heavy uranium atoms. These residuals are typical and not indicative 
of modeling issues.

PLAT976_ALERT_2_C (multiple)
PROBLEM: Check Calcd Resid. Dens.
RESPONSE: The negative residuals near O2 and O3 are common in structures 
with heavy atoms like uranium. They likely result from scattering 
contrast and idealized hydrogen placement. No signs of disorder or 
instability were found.

PLAT977_ALERT_2_C
PROBLEM: Check Negative Difference Density on H4B
RESPONSE: The small negative difference density near H4B (-0.31 eA-3) 
is typical for hydrogen atoms refined with idealized positions and 
isotropic displacement parameters, especially in the presence of heavy 
atoms like uranium. This does not indicate a modeling issue or disorder.
;
####################################################################### 
# 
# 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_gcb_135_4_cr3_dry1_ds2_vfinal
_database_code_depnum_ccdc_archive 'CCDC 2528712'
loop_
_audit_author_name
_audit_author_address
'Grant C. Benthin'
;The University of Iowa
United States of America
;
_audit_update_record             
;
2026-02-04 deposited with the CCDC.	2026-04-08 downloaded from the CCDC.
;
_audit_creation_date             2025-12-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_shelx_SHELXL_version_number     2019/1
loop_
_audit_author_email
''
_publ_section_validation_response 
;
PLAT088_ALERT_3_B
PROBLEM: Poor Data/Parameter Ratio
RESPONSE: The low data-to-parameter ratio of 6.22 arises from the reality 
that the crystal is highly symmetric and only contains a few atoms. 
After merging symmetry-equivalent reflections, only 143 unique 
reflections remain, while 23 parameters were refined. This ratio is 
typical for small, highly symmetric structures with heavy atoms. Despite 
the limited ratio, the refinement is of reasonable quality (R1 = 0.035, 
wR2 = 0.084, GOF = 1.20) and is chemically sensible. Given the nature 
of the compound and symmetry constraints, the ratio is unavoidable and 
does not compromise the validity of the structural model.

PLAT094_ALERT_2_B
PROBLEM: Ratio of Maximum / Minimum Residual Density
RESPONSE: The relatively high ratio of maximum to minimum residual 
density (5.3) is likely due to the presence of uranium in a small unit 
cell with only a few light atoms. The significant positive peaks and 
negative holes are located near the uranium atom and are likely the result 
of Fourier truncation effects around U center. These features are common 
in actinide structures, especially those with limited data resolution, and 
do not indicate missing atoms or disorder.

PLAT971_ALERT_2_B
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From U1
RESPONSE: The relatively large residual peak of 3.31 eA-3 at about 1.1 A 
from U1 is typical for structures with heavy atoms like uranium. The peak 
does not correspond to any chemically reasonable additional atom or 
ligand. Attempts to model extra sites, split positions, twinning, or 
alternative unit cells/space groups did not lead to improvement in 
R-values. Given these factors, the residual peak is considered acceptable 
and does not affect the validity of the model.

PLAT215_ALERT_3_C
PROBLEM: Disordered O1 has ADP max/min Ratio
RESPONSE: O1 lies on a special position in space group Immm and was 
refined anisotropically with partial occupancy (0.5). The elevated ADP 
ratio of 3.9 may reflect residual anisotropy due to symmetry constraints 
and limited data rather than true physical disorder. Attempts to model 
alternative disorder or split positions did not improve refinement or 
R-values. The current model is chemically reasonable and consistent with 
expected U-O bonding.

PLAT975_ALERT_2_C (multiple)
PROBLEM: Check Calcd Resid. Dens.
RESPONSE: The positive residuals near the oxygen atoms are likely due to 
nearby hydrogen atoms restrained using DFIX and DANG restraints and the 
presence of a heavy uranium atom. These residuals are considered typical 
and are not indicative of modeling issues.

PLAT976_ALERT_2_C
PROBLEM: Check Calcd Resid. Dens.
RESPONSE: The small negative residual feature near O1 is generally 
considered acceptable given the presence of a heavy atom (uranium).
Attempts to model alternative disorder/occupancy for O1 did not improve 
R-values or reduce the feature. The refinement is otherwise robust (R1 = 
0.035, wR2 = 0.084, GOF = 1.20), and the model provides chemically 
sensible geometry for U-O(peroxo) and U-O(water) bonding. Overall, the 
feature is considered acceptable and not indicative of a model deficiency.
;
_chemical_name_common            Metastudtite
_chemical_name_systematic        Diaquaperoxo(dioxouranium(VI))
_chemical_formula_moiety         'H4 O6 U'
_chemical_formula_sum            'H4 O6 U'
_chemical_formula_weight         338.06
_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'
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           71
_space_group_name_H-M_alt        Immm
_space_group_name_Hall           '-I 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   4.1946(5)
_cell_length_b                   6.5143(9)
_cell_length_c                   8.7339(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     238.65(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3658
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.328
_cell_measurement_theta_min      3.902
_shelx_estimated_absorpt_T_max   0.849
_shelx_estimated_absorpt_T_min   0.106
_exptl_absorpt_coefficient_mu    33.938
_exptl_absorpt_correction_T_max  0.0613
_exptl_absorpt_correction_T_min  0.0263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1335 before and 0.0979 after correction.
The Ratio of minimum to maximum transmission is 0.4290.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.704
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             288
_exptl_crystal_preparation       
'Dehydration of a single crystal of studtite at ambient temperature and pressure'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3334
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.328
_diffrn_reflns_theta_min         3.902
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_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                143
_reflns_number_total             143
_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         3.482
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.413
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         143
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0350
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0602P)²+6.5168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0843
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O3-H3
 0.97 with sigma of 0.02
 H3-U1
 3.114 with sigma of 0.04
2. Others
 Fixed Sof: O2(0.25) O1(0.25)
;
_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 0.500000 0.500000 0.500000 0.0303(5) Uani 1 8 d DS T P . .
O3 O 0.500000 0.500000 0.777(2) 0.038(4) Uani 1 4 d DS T P . .
O2 O 0.000000 0.621(4) 0.584(2) 0.033(5) Uani 0.5 2 d S T P . .
O1 O 0.633(6) 0.236(3) 0.500000 0.038(5) Uani 0.5 2 d S T P . .
H3 H 0.500000 0.385(9) 0.847(6) 0.05(6) Uiso 1 2 d DS . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.0190(7) 0.0294(8) 0.0426(8) 0.000 0.000 0.000
O3 0.031(9) 0.038(9) 0.045(9) 0.000 0.000 0.000
O2 0.035(11) 0.036(13) 0.026(10) -0.004(10) 0.000 0.000
O1 0.027(10) 0.019(9) 0.068(14) 0.000 0.000 0.018(9)

_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 2.358(10) 9_566 ?
U1 O2 2.358(10) 9_666 ?
U1 O2 2.358(10) 10_656 ?
U1 O2 2.358(10) 2_565 ?
U1 O2 2.358(10) 10_556 ?
U1 O2 2.358(10) . ?
U1 O2 2.358(10) 1_655 ?
U1 O2 2.358(10) 2_665 ?
U1 O1 1.80(2) . ?
U1 O1 1.80(2) 11_565 ?
U1 O1 1.80(2) 3_656 ?
U1 O1 1.80(2) 9_666 ?
O3 H3 0.97(2) . ?
O2 O2 1.47(4) 10_556 ?
O2 O2 1.58(5) 2_565 ?
O1 O1 1.11(5) 3_656 ?

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 O2 180.0 9_566 1_655 ?
O2 U1 O2 143.6(10) 10_556 9_666 ?
O2 U1 O2 140.9(11) 10_656 . ?
O2 U1 O2 54.4(10) 1_655 9_666 ?
O2 U1 O2 54.4(10) 9_566 . ?
O2 U1 O2 143.6(10) 2_665 . ?
O2 U1 O2 125.6(10) 9_566 9_666 ?
O2 U1 O2 39.1(11) 9_566 10_556 ?
O2 U1 O2 39.1(11) 10_656 9_666 ?
O2 U1 O2 140.9(11) 2_565 9_666 ?
O2 U1 O2 36.4(10) 10_556 . ?
O2 U1 O2 140.9(11) 1_655 10_556 ?
O2 U1 O2 125.6(10) 2_665 2_565 ?
O2 U1 O2 180.0 10_656 2_565 ?
O2 U1 O2 36.4(10) 1_655 10_656 ?
O2 U1 O2 140.9(11) 9_566 2_665 ?
O2 U1 O2 125.6(10) 10_556 10_656 ?
O2 U1 O2 36.4(10) 2_665 9_666 ?
O2 U1 O2 180.0 9_666 . ?
O2 U1 O2 39.1(11) 1_655 2_665 ?
O2 U1 O2 36.4(10) 9_566 2_565 ?
O2 U1 O2 125.6(10) 1_655 . ?
O2 U1 O2 143.6(10) 1_655 2_565 ?
O2 U1 O2 180.0 10_556 2_665 ?
O2 U1 O2 54.4(10) 10_556 2_565 ?
O2 U1 O2 39.1(11) 2_565 . ?
O2 U1 O2 143.6(10) 9_566 10_656 ?
O2 U1 O2 54.4(10) 2_665 10_656 ?
O1 U1 O2 92.5(10) 11_565 2_665 ?
O1 U1 O2 53.7(9) 3_656 9_566 ?
O1 U1 O2 126.3(10) 9_666 9_666 ?
O1 U1 O2 126.3(9) 11_565 2_565 ?
O1 U1 O2 92.5(10) 11_565 9_666 ?
O1 U1 O2 126.3(9) 3_656 1_655 ?
O1 U1 O2 126.3(10) . 10_556 ?
O1 U1 O2 87.5(10) 11_565 10_556 ?
O1 U1 O2 92.5(10) 9_666 9_566 ?
O1 U1 O2 87.5(10) 11_565 . ?
O1 U1 O2 87.5(10) 3_656 9_666 ?
O1 U1 O2 53.7(9) 3_656 2_565 ?
O1 U1 O2 53.7(9) . 9_666 ?
O1 U1 O2 92.5(10) . 10_656 ?
O1 U1 O2 53.7(9) . 2_665 ?
O1 U1 O2 92.5(10) 9_666 2_565 ?
O1 U1 O2 53.7(9) 11_565 1_655 ?
O1 U1 O2 87.5(10) . 2_565 ?
O1 U1 O2 92.5(10) 3_656 . ?
O1 U1 O2 53.7(10) 9_666 . ?
O1 U1 O2 126.3(10) . . ?
O1 U1 O2 92.5(10) 3_656 10_556 ?
O1 U1 O2 53.7(9) 11_565 10_656 ?
O1 U1 O2 126.3(9) 3_656 10_656 ?
O1 U1 O2 87.5(10) 9_666 10_656 ?
O1 U1 O2 53.7(9) 9_666 10_556 ?
O1 U1 O2 87.5(10) 9_666 1_655 ?
O1 U1 O2 92.5(10) . 1_655 ?
O1 U1 O2 87.5(10) 3_656 2_665 ?
O1 U1 O2 126.3(9) 11_565 9_566 ?
O1 U1 O2 126.3(10) 9_666 2_665 ?
O1 U1 O2 87.5(10) . 9_566 ?
O1 U1 O1 144.0(17) 3_656 9_666 ?
O1 U1 O1 36.0(17) 11_565 9_666 ?
O1 U1 O1 144.0(17) 11_565 . ?
O1 U1 O1 180.0 11_565 3_656 ?
O1 U1 O1 36.0(17) 3_656 . ?
O1 U1 O1 180.0(16) 9_666 . ?
U1 O3 H3 129(5) . . ?
U1 O2 U1 125.6(10) 1_455 . ?
O2 O2 U1 71.8(5) 10_556 1_455 ?
O2 O2 U1 71.8(5) 10_556 . ?
O2 O2 U1 70.5(5) 2_565 . ?
O2 O2 U1 70.5(5) 2_565 1_455 ?
O2 O2 O2 90.000(1) 10_556 2_565 ?
O1 O1 U1 72.0(8) 3_656 . ?

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
O2 U1 O1 O1 -18.2(5) 9_566 . . 3_656 ?
O2 U1 O1 O1 -22.8(6) 10_556 . . 3_656 ?
O2 U1 O1 O1 157.2(6) 2_665 . . 3_656 ?
O2 U1 O1 O1 -161.8(5) 10_656 . . 3_656 ?
O2 U1 O1 O1 22.8(6) . . . 3_656 ?
O2 U1 O1 O1 -157.2(6) 9_666 . . 3_656 ?
O2 U1 O1 O1 161.8(5) 1_655 . . 3_656 ?
O2 U1 O1 O1 18.2(5) 2_565 . . 3_656 ?
O1 U1 O1 O1 180.0 11_565 . . 3_656 ?

_shelx_res_file                  
;
TITL gcb_135_4_cr3_dry1_ds2_vfinal_a.res in Immm
    gcb_135_4_cr3_dry1_ds2_vfinal.res
    created by SHELXL-2019/1 at 10:17:47 on 31-Dec-2025
REM Old TITL GCB_135_4_cr3_dry1_ds2_vFinal in Immm
REM SHELXT solution in Immm: R1 0.109, Rweak 0.526, Alpha 0.012
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: O2 U
CELL 0.71073 4.1946 6.5143 8.7339 90 90 90
ZERR 2 0.0005 0.0009 0.0013 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SFAC H O U
UNIT 8 12 2
DFIX 0.97 O3 H3
DANG 3.114 H3 U1

L.S. 1
PLAN  5
SIZE 0.12 0.015 0.005
TEMP -173.15
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\GCB_135_4_cr3_dry1_ds2_vFinal.hkl">
REM </olex2.extras>

WGHT    0.060200    6.516800
FVAR       0.54686
U1    3    0.500000    0.500000    0.500000    10.12500    0.01900    0.02940 =
         0.04262    0.00000    0.00000    0.00000
O3    2    0.500000    0.500000    0.777132    10.25000    0.03055    0.03753 =
         0.04509    0.00000    0.00000    0.00000
O2    2    0.000000    0.621022    0.584263    10.25000    0.03488    0.03640 =
         0.02641   -0.00395    0.00000    0.00000
O1    2    0.632796    0.236447    0.500000    10.25000    0.02740    0.01888 =
         0.06845    0.00000    0.00000    0.01773
H3    1    0.500000    0.384902    0.846811    10.50000    0.04743
HKLF 4




REM  gcb_135_4_cr3_dry1_ds2_vfinal_a.res in Immm
REM wR2 = 0.0843, GooF = S = 1.198, Restrained GooF = 1.188 for all data
REM R1 = 0.0350 for 143 Fo > 4sig(Fo) and 0.0350 for all 143 data
REM 23 parameters refined using 2 restraints

END

WGHT      0.0656      0.0000

REM Highest difference peak  3.482,  deepest hole -0.657,  1-sigma level  0.413
Q1    1   0.5000  0.5000  0.6102  10.25000  0.05    3.48
Q2    1   0.6927  0.5000  0.5000  10.25000  0.05    1.04
Q3    1   0.5000  0.5000  1.0000  10.12500  0.05    0.67
Q4    1   0.5000  0.3594  0.7020  10.50000  0.05    0.62
Q5    1   0.7514  0.1372  0.5000  10.50000  0.05    0.61
;
_shelx_res_checksum              68314
_olex2_date_sample_completion    2025-01-06
_olex2_date_sample_data_collection 2025-01-03
_olex2_date_sample_submission    2025-01-03
_olex2_submission_original_sample_id GCB_135_4_cr3_dry1
_olex2_submission_special_instructions 'No special instructions were received'
