Modulating the catalytic properties of decavanadate hybrids using a mixed counterion strategy for selective oxidation of thiophene-based sulfides and detoxification of mustard gas simulant.
Routh, Kousik; Kar, Aranya; Pradeep, Chullikkattil P.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6195–6210; doi:10.1039/d5dt00102a

data_7718343
_publ_section_title
;
 Modulating the catalytic properties of decavanadate hybrids using a mixed
 counterion strategy for selective oxidation of thiophene-based sulfides
 and detoxification of mustard gas simulant.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6195
_journal_page_last               6210
_journal_paper_doi               10.1039/d5dt00102a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'H2 O28 V10, 2(C8 H11 O S), 2(C9 H11 O S)'
_chemical_formula_sum            'C34 H46 O32 S4 V10'
_chemical_formula_weight         1604.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-03-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2025-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.642(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0870(2)
_cell_length_b                   12.6637(3)
_cell_length_c                   21.3134(4)
_cell_measurement_reflns_used    6177
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0770
_cell_measurement_theta_min      2.5030
_cell_volume                     2691.64(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00 120.00   1.00   17.97    --   26.84 178.00-120.00   85
  2  \w    -55.00  80.00   1.00   17.97    --   26.84 -37.00 -60.00  135
  3  \w    -59.00 100.00   1.00   17.97    --   26.84   0.00-180.00  159
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0236910000
_diffrn_orient_matrix_UB_12      -0.0432338000
_diffrn_orient_matrix_UB_13      -0.0162993000
_diffrn_orient_matrix_UB_21      -0.0528555000
_diffrn_orient_matrix_UB_22      0.0077906000
_diffrn_orient_matrix_UB_23      -0.0255438000
_diffrn_orient_matrix_UB_31      0.0412516000
_diffrn_orient_matrix_UB_32      0.0347764000
_diffrn_orient_matrix_UB_33      -0.0146519000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15260
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         1.876
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.335
_exptl_crystal_size_min          0.153
_refine_diff_density_max         2.129
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+3.9858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4896
_reflns_number_total             5998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00102a2.cif
_cod_data_source_block           krp_oh_dmf_rt_mo
_cod_depositor_comments          'Adding full bibliography for 7718343.cif.'
_cod_original_cell_volume        2691.66(10)
_cod_database_code               7718343
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C68  H92  O64  S8  V20  '
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C7(H7), C2(H2), C3(H3), C14(H14), C12(H12), C6(H6), C15(H15), C5(H5)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C8(H8A,H8B,H8C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              24810
_shelx_hkl_checksum              59410
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.509
_oxdiff_exptl_absorpt_empirical_full_min 0.718