# Supplementary Information (SI) for Chemical Science.
# 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_nu-2003
_database_code_depnum_ccdc_archive 'CCDC 2347333'
loop_
_audit_author_name
_audit_author_address
'Haomiao Xie'
;Northwestern University
United States of America
;
_audit_update_record             
;
2024-04-10 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_audit_creation_date             2024-04-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 O5 V'
_chemical_formula_sum            'C7 H2.40 O6.20 V'
_chemical_formula_weight         236.63
_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'
V V 0.0687 2.1097 '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           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   16.342(3)
_cell_length_b                   6.8717(8)
_cell_length_c                   10.284(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1154.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1411
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      69.8770
_cell_measurement_theta_min      5.0570
_shelx_estimated_absorpt_T_max   0.931
_shelx_estimated_absorpt_T_min   0.868
_exptl_absorpt_coefficient_mu    7.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5436
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.441
_diffrn_reflns_theta_max         67.441
_diffrn_reflns_theta_min         5.081
_diffrn_ambient_temperature      111.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  11.00   0.50   10.00    --  -47.42  79.00  35.00  164
  2  ω    -21.00  54.00   0.50   10.00    --   47.42 -79.00 -89.00  150
  3  ω    -95.00 -69.00   0.50   20.00    -- -106.00  79.00  35.00   52
  4  ω   -174.00 -83.00   0.50   20.00    -- -106.00 -79.00 -89.00  182
  5  ω     72.00  98.00   0.50   20.00    --  113.25 -79.00 -89.00   52
  6  ω    140.00 166.00   0.50   20.00    --  113.25  79.00  35.00   52
  7  ω    -38.00  26.00   0.50   10.00    --  -47.42  37.00-180.00  128
  8  ω    -18.00  14.00   0.50   10.00    --  -47.42  19.00 -60.00   64
  9  ω   -108.00 -83.00   0.50   10.00    --  -47.42-125.00  60.00   50
 10  ω    -19.00  14.00   0.50   10.00    --  -47.42  19.00 -30.00   66
 11  ω   -117.00 -92.00   0.50   10.00    --  -47.42-125.00  30.00   50
 12  ω   -117.00 -85.00   0.50   10.00    --  -47.42   0.00-150.00   64
 13  ω     85.00 112.00   0.50   10.00    --   47.42 125.00-120.00   54
 14  ω    -23.00  36.00   0.50   10.00    --   47.42 -37.00 -30.00  118
 15  ω    -27.00  -2.00   0.50   10.00    --   47.42 -19.00  30.00   50
 16  ω    -64.00 -38.00   0.50   20.00    -- -106.00 125.00 150.00   52
 17  ω   -108.00 -70.00   0.50   20.00    -- -106.00 110.00 -15.66   76
 18  ω    -73.00 -47.00   0.50   20.00    -- -106.00  61.00-180.00   52
 19  ω   -177.00 -89.00   0.50   20.00    -- -106.00 -61.00 -30.00  176
 20  ω   -111.00 -80.00   0.50   20.00    -- -106.00 125.00 150.00   62
 21  ω    -68.00 -43.00   0.50   20.00    -- -106.00 107.00 -88.49   50
 22  ω    -73.00 -34.00   0.50   20.00    -- -106.00  61.00  30.00   78
 23  ω   -173.00 -98.00   0.50   20.00    -- -106.00 -61.00-120.00  150
 24  ω    -65.00 -38.00   0.50   20.00    -- -106.00  61.00-120.00   54
 25  ω   -106.00 -77.00   0.50   20.00    -- -106.00 107.00 -88.49   58
 26  ω   -176.00-107.00   0.50   20.00    -- -106.00 -61.00   0.00  138
 27  ω    -72.00 -43.00   0.50   20.00    -- -106.00  61.00-150.00   58
 28  ω    -66.00 -39.00   0.50   20.00    -- -106.00 110.00 -15.66   54
 29  ω    142.00 177.00   0.50   20.00    --  113.25  77.00 -60.00   70
 30  ω     95.00 130.00   0.50   20.00    --  113.25  77.00 -60.00   70
 31  ω     68.00 106.00   0.50   20.00    --  113.25 -94.00  90.00   76
 32  ω     44.00  71.00   0.50   20.00    --  113.25 -61.00  30.00   54
 33  ω     42.00  71.00   0.50   20.00    --  113.25 -61.00  60.00   58
 34  ω     43.00 106.00   0.50   20.00    --  113.25 -94.00-150.00  126
 35  ω     82.00 111.00   0.50   20.00    --  113.25-125.00  90.00   58
 36  ω     42.00  76.00   0.50   20.00    --  113.25-125.00  90.00   68
 37  ω     57.00  91.00   0.50   20.00    --  113.25 -94.00 -90.00   68
 38  ω     42.00  92.00   0.50   20.00    --  113.25 -94.00 120.00  100
 39  ω    123.00 177.00   0.50   20.00    --  113.25   0.00-180.00  108
 40  ω    102.00 178.00   0.50   20.00    --  113.25  77.00  60.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                493
_reflns_number_total             594
_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       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.594
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         594
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.1448
_refine_ls_restrained_S_all      1.591
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3655
_refine_ls_wR_factor_ref         0.3719
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Restrained distances
 C3-C2 \\sim C3-C2_$3
 with sigma of 0.01
 C3-C2 \\sim C4_$1-C2
 with sigma of 0.01
 C4-C3 \\sim C4_$1-C3
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C4 \\sim C4 \\sim C3 \\sim C4 \\sim C3 \\sim C4: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: C4(0.5) C3(0.25)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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
V1 V 0.500000 0.500000 0.500000 0.0642(12) Uani 1 4 d S T P . .
O1 O 0.500000 0.250000 0.4091(9) 0.080(3) Uani 1 4 d S T P . .
O2 O 0.4134(4) 0.5898(8) 0.3783(8) 0.117(3) Uani 1 1 d . . . . .
C1 C 0.3821(8) 0.750000 0.3478(17) 0.099(5) Uani 1 2 d S T P A .
C2 C 0.3043(9) 0.750000 0.288(2) 0.151(9) Uani 1 2 d DS T P . .
C4 C 0.2320(16) 0.596(4) 0.295(3) 0.144(12) Uani 0.5 1 d D U P A -1
C3 C 0.2187(17) 0.750000 0.361(3) 0.166(14) Uani 0.5 2 d DS TU P A .


_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
V1 O1 1.956(5) 9_666 ?
V1 O1 1.956(5) . ?
V1 O2 1.988(6) 9_666 ?
V1 O2 1.988(6) . ?
V1 O2 1.988(6) 4_566 ?
V1 O2 1.988(6) 12_655 ?
O2 C1 1.254(8) . ?
C1 C2 1.412(19) . ?
C2 C2 1.94(3) 7_545 ?
C2 C4 1.59(2) . ?
C2 C4 1.59(2) 11_575 ?
C2 C3 1.58(2) 13_565 ?
C2 C3 1.59(2) 11_575 ?
C2 C3 1.59(2) . ?
C3 C3 0.00(10) 11_575 ?

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 V1 O1 180.0 9_666 . ?
O1 V1 O2 91.6(3) 9_666 12_655 ?
O1 V1 O2 88.4(3) 9_666 9_666 ?
O1 V1 O2 91.6(3) . 9_666 ?
O1 V1 O2 88.4(3) . . ?
O1 V1 O2 88.4(3) . 12_655 ?
O1 V1 O2 88.4(3) 9_666 4_566 ?
O1 V1 O2 91.6(3) 9_666 . ?
O1 V1 O2 91.6(3) . 4_566 ?
O2 V1 O2 89.2(5) 9_666 12_655 ?
O2 V1 O2 89.2(5) . 4_566 ?
O2 V1 O2 90.8(5) . 12_655 ?
O2 V1 O2 180.0(3) 12_655 4_566 ?
O2 V1 O2 90.8(5) 9_666 4_566 ?
O2 V1 O2 180.0 . 9_666 ?
V1 O1 V1 122.9(5) . 2_655 ?
C1 O2 V1 136.1(6) . . ?
O2 C1 O2 122.9(10) 11_575 . ?
O2 C1 C2 118.4(5) . . ?
O2 C1 C2 118.4(5) 11_575 . ?
C1 C2 C2 178(3) . 7_545 ?
C1 C2 C4 130.6(15) . . ?
C1 C2 C4 130.6(15) . 11_575 ?
C1 C2 C3 129(2) . 13_565 ?
C1 C2 C3 126(3) . . ?
C1 C2 C3 126(3) . 11_575 ?
C4 C2 C2 48.5(12) . 7_545 ?
C4 C2 C2 48.5(12) 11_575 7_545 ?
C4 C2 C4 83(2) . 11_575 ?
C4 C2 C3 47.3(13) 11_575 11_575 ?
C4 C2 C3 47.3(13) . . ?
C4 C2 C3 47.3(13) . 11_575 ?
C4 C2 C3 47.3(13) 11_575 . ?
C3 C2 C2 52.2(8) . 7_545 ?
C3 C2 C2 52.4(8) 13_565 7_545 ?
C3 C2 C2 52.2(8) 11_575 7_545 ?
C3 C2 C4 82.4(13) 13_565 . ?
C3 C2 C4 82.4(13) 13_565 11_575 ?
C3 C2 C3 104.6(16) 13_565 11_575 ?
C3 C2 C3 104.6(16) 13_565 . ?
C3 C2 C3 0.0(10) 11_575 . ?
C2 C3 C2 75.4(16) 7_545 . ?
C4 C3 C2 61.5(18) 11_575 7_545 ?
C4 C3 C2 66.3(8) 11_575 . ?
C3 C3 C2 0(10) 11_575 . ?
C3 C3 C2 0(10) 11_575 7_545 ?
C3 C3 C4 0(10) 11_575 11_575 ?

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
V1 O2 C1 O2 14(3) . . . 11_575 ?
V1 O2 C1 C2 -159.7(13) . . . . ?
O2 C1 C2 C4 -148(2) 11_575 . . . ?
O2 C1 C2 C4 26(4) . . . . ?
O2 C1 C2 C4 -26(4) 11_575 . . 11_575 ?
O2 C1 C2 C4 148(2) . . . 11_575 ?
O2 C1 C2 C3 -93.1(16) . . . 13_565 ?
O2 C1 C2 C3 86.9(16) . . . . ?
O2 C1 C2 C3 86.9(16) . . . 11_575 ?
O2 C1 C2 C3 -86.9(16) 11_575 . . . ?
O2 C1 C2 C3 -86.9(16) 11_575 . . 11_575 ?
O2 C1 C2 C3 93.1(16) 11_575 . . 13_565 ?
C1 C2 C3 C2 180.000(3) . . . 7_545 ?
C1 C2 C3 C4 115.1(17) . . . 11_575 ?
C1 C2 C3 C3 0(100) . . . 11_575 ?
C2 C2 C3 C4 -64.9(17) 7_545 . . 11_575 ?
C2 C2 C3 C3 0.0(15) 7_545 . . 11_575 ?
C4 C2 C3 C2 64.9(17) 11_575 . . 7_545 ?
C4 C2 C3 C2 -64.9(17) . . . 7_545 ?
C4 C2 C3 C4 -130(3) . . . 11_575 ?
C4 C2 C3 C3 0(3) . . . 11_575 ?
C4 C2 C3 C3 0.0(5) 11_575 . . 11_575 ?
C3 C2 C3 C2 0(100) 11_575 . . 7_545 ?
C3 C2 C3 C2 0.000(1) 13_565 . . 7_545 ?
C3 C2 C3 C4 0(100) 11_575 . . 11_575 ?
C3 C2 C3 C4 -64.9(17) 13_565 . . 11_575 ?
C3 C2 C3 C3 0.0(15) 13_565 . . 11_575 ?

_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 0.000 -0.803 0.500 213.3 24.2 '2.4 H2O'
2 0.500 -0.636 0.000 213.3 24.2 '2.4 H2O'

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
