Hydrazone-based dioxidomolybdenum(VI) complexes: catalytic oxidation of omeprazole sulfide.
Nafisa, ?; Mahiya, Kuldeep; Rana, Lata; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12919–12932; doi:10.1039/d5dt01503k

data_7719267
_publ_section_title
;
 Hydrazone-based dioxidomolybdenum(VI) complexes: catalytic oxidation of
 omeprazole sulfide.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12919
_journal_page_last               12932
_journal_paper_doi               10.1039/d5dt01503k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C12 H10 Mo N4 O5, H2 O'
_chemical_formula_sum            'C12 H12 Mo N4 O6'
_chemical_formula_weight         404.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-21 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.4080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.15770(10)
_cell_length_b                   10.32150(10)
_cell_length_c                   12.28650(10)
_cell_measurement_reflns_used    22691
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.9420
_cell_measurement_theta_min      3.8370
_cell_volume                     1435.40(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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     10.00  43.00   0.50    0.20    --   40.83  89.00 163.10   66
  2  \w      8.00  35.00   0.50    0.20    --   40.83  93.00 116.76   54
  3  \w      8.00  35.00   0.50    0.20    --   40.83  94.00  19.36   54
  4  \w     12.00  43.00   0.50    0.20    --   40.83  83.00 113.80   62
  5  \w      9.00  42.00   0.50    0.20    --   40.83  91.00   9.33   66
  6  \w     12.00  43.00   0.50    0.20    --   40.83  84.00 -53.14   62
  7  \w     11.00  43.00   0.50    0.20    --   40.83  87.00-115.77   64
  8  \w     13.00  43.00   0.50    0.20    --   40.83  81.00-179.00   60
  9  \w     12.00  43.00   0.50    0.20    --   40.83  83.00-150.81   62
 10  \w     13.00  43.00   0.50    0.20    --   40.83  80.00-119.45   60
 11  \w     21.00 108.00   0.50    0.20    --   40.83  54.00-120.00  174
 12  \w     24.00 108.00   0.50    0.20    --   40.83  43.00-180.00  168
 13  \w    -34.00 118.00   0.50    0.20    --   40.83   1.00-150.00  304
 14  \w     21.00 108.00   0.50    0.20    --   40.83  54.00 -60.00  174
 15  \w     14.00  43.00   0.50    0.20    --   40.83  79.00  -0.33   58
 16  \w     69.00 165.00   0.50    0.20    --   96.04  77.00 150.00  192
 17  \w     69.00 165.00   0.50    0.20    --   96.04  77.00  90.00  192
 18  \w     69.00 165.00   0.50    0.20    --   96.04  77.00  60.00  192
 19  \w     72.00 164.00   0.50    0.20    --   96.04  68.00 120.00  184
 20  \w     69.00 165.00   0.50    0.20    --   96.04  77.00 -60.00  192
 21  \w     72.00 164.00   0.50    0.20    --   96.04  68.00  30.00  184
 22  \w     69.00 165.00   0.50    0.20    --   96.04  77.00 -90.00  192
 23  \w     77.00 163.00   0.50    0.20    --   96.04  50.00   0.00  172
 24  \w     72.00 164.00   0.50    0.20    --   96.04  68.00-120.00  184
 25  \w     69.00 165.00   0.50    0.20    --   96.04  77.00-180.00  192
 26  \w     72.00 164.00   0.50    0.20    --   96.04  68.00-150.00  184
 27  \w     21.00 173.00   0.50    0.20    --   96.04   1.00-150.00  304
 28  \w    105.00 170.00   0.50    0.20    --   96.04  96.00-120.00  130
 29  \w     99.00 160.00   0.50    0.20    --   96.04 117.00-150.00  122
 30  \w     99.00 160.00   0.50    0.20    --   96.04 117.00 -30.00  122
 31  \w    105.00 170.00   0.50    0.20    --   96.04  96.00  90.00  130
 32  \w     18.00 170.00   0.50    0.20    --   96.04  -1.00  30.00  304
 33  \w     28.00  68.00   0.50    0.20    --   96.04 -59.00 -30.00   80
 34  \w     29.00  57.00   0.50    0.20    --   96.04 -50.00 -90.00   56
 35  \w     29.00  57.00   0.50    0.20    --   96.04 -50.00-180.00   56
 36  \w     28.00  83.00   0.50    0.20    --   96.04 -68.00-180.00  110
 37  \w     27.00 105.00   0.50    0.20    --   96.04 -77.00-180.00  156
 38  \w    -27.00  28.00   0.50    0.20    --   40.83 -32.00-120.00  110
 39  \w    -25.00  48.00   0.50    0.20    --   40.83 -43.00  90.00  146
 40  \w     29.00  57.00   0.50    0.20    --   96.04 -50.00 120.00   56
 41  \w     28.00  68.00   0.50    0.20    --   96.04 -59.00 -90.00   80
 42  \w     26.00 127.00   0.50    0.20    --   96.04 -87.00 -90.00  202
 43  \w     32.00 110.00   0.50    0.20    --   96.04-117.00-150.00  156
 44  \w     44.00 127.00   0.50    0.20    --   96.04-145.00-150.00  166
 45  \w     32.00 110.00   0.50    0.20    --   96.04-117.00 -90.00  156
 46  \w     26.00 127.00   0.50    0.20    --   96.04 -87.00  90.00  202
 47  \w     44.00 127.00   0.50    0.20    --   96.04-145.00  90.00  166
 48  \w     32.00 110.00   0.50    0.20    --   96.04-117.00  90.00  156
 49  \w     18.00  78.00   0.50    0.20    --   40.83-104.00  30.00  120
 50  \w     41.00 100.00   0.50    0.20    --   40.83-138.00-150.00  118
 51  \w     18.00  78.00   0.50    0.20    --   40.83-104.00-180.00  120
 52  \w   -116.00  36.00   0.50    0.20    --  -40.83   1.00-150.00  304
 53  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00 -90.00  118
 54  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00   0.00  118
 55  \w    -48.00  26.00   0.50    0.20    --  -40.83  43.00  60.00  148
 56  \w   -105.00 -14.00   0.50    0.20    --  -82.50  77.00  30.00  182
 57  \w    -57.00 -16.00   0.50    0.20    --  -82.50  50.00 -60.00   82
 58  \w    -47.00 -15.00   0.50    0.20    --  -82.50  42.00 -90.00   64
 59  \w   -158.00  -6.00   0.50    0.20    --  -82.50   1.00-150.00  304
 60  \w    -47.00 -15.00   0.50    0.20    --  -82.50  42.00-150.00   64
 61  \w    -57.00 -16.00   0.50    0.20    --  -82.50  50.00-180.00   82
 62  \w   -108.00 -17.00   0.50    0.20    --  -40.83 -65.00 -60.00  182
 63  \w   -109.00 -14.00   0.50    0.20    --  -40.83 -77.00 -90.00  190
 64  \w   -109.00 -14.00   0.50    0.20    --  -40.83 -77.00  30.00  190
 65  \w   -109.00 -14.00   0.50    0.20    --  -40.83 -77.00  90.00  190
 66  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00  60.00  192
 67  \w   -152.00 -56.00   0.50    0.20    --  -82.50 -75.00  95.19  192
 68  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00 150.00  192
 69  \w   -151.00 -55.00   0.50    0.20    --  -82.50 -77.00  20.83  192
 70  \w   -151.00 -56.00   0.50    0.20    --  -82.50 -76.00 -14.02  190
 71  \w   -151.00 -56.00   0.50    0.20    --  -82.50 -74.00 -49.88  190
 72  \w   -150.00 -58.00   0.50    0.20    --  -82.50 -68.00 -90.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1092179000
_diffrn_orient_matrix_UB_12      0.0012104000
_diffrn_orient_matrix_UB_13      -0.1142834000
_diffrn_orient_matrix_UB_21      -0.0812390000
_diffrn_orient_matrix_UB_22      -0.0017929000
_diffrn_orient_matrix_UB_23      0.0712521000
_diffrn_orient_matrix_UB_31      -0.0000794000
_diffrn_orient_matrix_UB_32      0.1492232000
_diffrn_orient_matrix_UB_33      0.0017376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28088
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.024
_diffrn_reflns_theta_min         4.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.870
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.00152(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2613
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0285P)^2^+1.4934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2579
_reflns_number_total             2613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01503k2.cif
_cod_data_source_block           SP
_cod_depositor_comments
'Adding full bibliography for 7719267--7719270.cif.'
_cod_database_code               7719267
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.507
_shelx_estimated_absorpt_t_min   0.332
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
 O6-H6A = O6-H6B
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              15727
_shelx_hkl_checksum              93639
_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 1.528
_oxdiff_exptl_absorpt_empirical_full_min 0.706