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_7719269
_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         'C13 H12 Mo N4 O5'
_chemical_formula_sum            'C13 H12 Mo N4 O5'
_chemical_formula_weight         400.21
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-17
_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                 90.897(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5485(2)
_cell_length_b                   10.80420(10)
_cell_length_c                   17.3072(3)
_cell_measurement_reflns_used    13383
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.9410
_cell_measurement_theta_min      2.5410
_cell_volume                     1411.32(5)
_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     14.00 110.00   0.50    0.20    --   40.83  77.00  60.00  192
  2  \w     14.00 110.00   0.50    0.20    --   40.83  77.00  30.00  192
  3  \w     14.00 110.00   0.50    0.20    --   40.83  77.00 -30.00  192
  4  \w     14.00 110.00   0.50    0.20    --   40.83  77.00 -90.00  192
  5  \w     18.00 109.00   0.50    0.20    --   40.83  65.00-120.00  182
  6  \w     18.00 109.00   0.50    0.20    --   40.83  65.00-180.00  182
  7  \w     14.00 110.00   0.50    0.20    --   40.83  77.00-150.00  192
  8  \w     18.00 109.00   0.50    0.20    --   40.83  65.00 150.00  182
  9  \w     21.00 108.00   0.50    0.20    --   40.83  54.00 120.00  174
 10  \w     21.00 108.00   0.50    0.20    --   40.83  54.00 -30.00  174
 11  \w    105.00 170.00   0.50    0.42    --   96.04  96.00-150.00  130
 12  \w     99.00 160.00   0.50    0.42    --   96.04 117.00-150.00  122
 13  \w     96.00 160.00   0.50    0.42    --   96.04 123.00-179.00  128
 14  \w    105.00 170.00   0.50    0.42    --   96.04  96.00 -60.00  130
 15  \w     79.00 162.00   0.50    0.42    --   96.04  42.00 -30.00  166
 16  \w     69.00 165.00   0.50    0.42    --   96.04  77.00 150.00  192
 17  \w     69.00 165.00   0.50    0.42    --   96.04  77.00 120.00  192
 18  \w     72.00 164.00   0.50    0.42    --   96.04  68.00  60.00  184
 19  \w     72.00 164.00   0.50    0.42    --   96.04  68.00-120.00  184
 20  \w     69.00 165.00   0.50    0.42    --   96.04  77.00-150.00  192
 21  \w     69.00 165.00   0.50    0.42    --   96.04  77.00-180.00  192
 22  \w     72.00 164.00   0.50    0.42    --   96.04  68.00 -90.00  184
 23  \w     74.00 163.00   0.50    0.42    --   96.04  59.00   0.00  178
 24  \w     74.00 163.00   0.50    0.42    --   96.04  59.00  30.00  178
 25  \w     74.00 163.00   0.50    0.42    --   96.04  59.00  90.00  178
 26  \w     77.00 163.00   0.50    0.42    --   96.04  50.00 120.00  172
 27  \w     27.00 105.00   0.50    0.42    --   96.04 -77.00 -30.00  156
 28  \w     29.00  57.00   0.50    0.42    --   96.04 -50.00  90.00   56
 29  \w     29.00  57.00   0.50    0.42    --   96.04 -50.00 150.00   56
 30  \w     29.00  57.00   0.50    0.42    --   96.04 -50.00 120.00   56
 31  \w     27.00 105.00   0.50    0.42    --   96.04 -77.00  90.00  156
 32  \w     29.00  57.00   0.50    0.42    --   96.04 -50.00   0.00   56
 33  \w    -27.00  37.00   0.50    0.20    --   40.83 -32.00  90.00  128
 34  \w    -35.00  24.00   0.50    0.20    --   40.83 -11.00 -30.00  118
 35  \w     29.00  57.00   0.50    0.42    --   96.04 -50.00-180.00   56
 36  \w     28.00  68.00   0.50    0.42    --   96.04 -59.00 -90.00   80
 37  \w     29.00  57.00   0.50    0.42    --   96.04 -50.00 -30.00   56
 38  \w     23.00 106.00   0.50    0.42    --   96.04 -96.00 -30.00  166
 39  \w     44.00 127.00   0.50    0.42    --   96.04-145.00-150.00  166
 40  \w     32.00 110.00   0.50    0.42    --   96.04-117.00 -60.00  156
 41  \w     46.00 130.00   0.50    0.42    --   96.04-149.00 -62.00  168
 42  \w     32.00 110.00   0.50    0.42    --   96.04-123.00 100.00  156
 43  \w     32.00  88.00   0.50    0.20    --   40.83-123.00 100.00  112
 44  \w     46.00 106.00   0.50    0.20    --   40.83-149.00 -62.00  120
 45  \w     41.00 100.00   0.50    0.20    --   40.83-138.00-180.00  118
 46  \w    -61.00  26.00   0.50    0.20    --  -40.83  54.00-150.00  174
 47  \w    -85.00 -11.00   0.50    0.20    --  -40.83 123.00-179.00  148
 48  \w   -104.00 -25.00   0.50    0.20    --  -40.83 149.00 -16.00  158
 49  \w    -24.00  35.00   0.50    0.20    --  -40.83  11.00 -30.00  118
 50  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00 -60.00  118
 51  \w   -151.00 -55.00   0.50    0.42    --  -82.50 -77.00 -60.00  192
 52  \w   -151.00 -55.00   0.50    0.42    --  -82.50 -77.00 -30.00  192
 53  \w   -151.00 -55.00   0.50    0.42    --  -82.50 -77.00  60.00  192
 54  \w   -147.00 -74.00   0.50    0.42    --  -82.50-123.00 100.00  146
 55  \w   -109.00 -56.00   0.50    0.20    --  -40.83-149.00 -62.00  106
 56  \w   -150.00 -56.00   0.50    0.42    --  -82.50-149.00 -62.00  188
 57  \w   -153.00 -78.00   0.50    0.42    --  -82.50 -87.00-120.00  150
 58  \w   -153.00 -78.00   0.50    0.42    --  -82.50 -87.00-180.00  150
;
_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      0.0836742000
_diffrn_orient_matrix_UB_12      0.1098645000
_diffrn_orient_matrix_UB_13      -0.0428456000
_diffrn_orient_matrix_UB_21      0.0779604000
_diffrn_orient_matrix_UB_22      -0.0899598000
_diffrn_orient_matrix_UB_23      -0.0595969000
_diffrn_orient_matrix_UB_31      -0.1690878000
_diffrn_orient_matrix_UB_32      0.0129435000
_diffrn_orient_matrix_UB_33      -0.0503657000
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22019
_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         68.041
_diffrn_reflns_theta_min         4.825
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49401
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2558
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0542P)^2^+1.4092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2288
_reflns_number_total             2558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01503k2.cif
_cod_data_source_block           HC
_cod_depositor_comments
'Adding full bibliography for 7719267--7719270.cif.'
_cod_database_code               7719269
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.504
_shelx_estimated_absorpt_t_min   0.329
_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
2. Restrained distances
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C12(H12)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              89187
_shelx_hkl_checksum              85162
_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 1.677
_oxdiff_exptl_absorpt_empirical_full_min 0.733