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_7719268
_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 O6'
_chemical_formula_sum            'C13 H12 Mo N4 O6'
_chemical_formula_weight         416.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.35850(10)
_cell_length_b                   11.70260(10)
_cell_length_c                   15.25080(10)
_cell_measurement_reflns_used    13525
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.9300
_cell_measurement_theta_min      2.9050
_cell_volume                     1491.78(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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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   0.00  192
  3  \w     21.00 108.00   0.50    0.20    --   40.83  54.00 -30.00  174
  4  \w     18.00 109.00   0.50    0.20    --   40.83  65.00-120.00  182
  5  \w     14.00 110.00   0.50    0.20    --   40.83  77.00 -90.00  192
  6  \w     16.00 114.00   0.50    0.20    --   40.83  18.00-106.00  196
  7  \w     69.00 103.00   0.50    0.58    --   96.04  77.00 -90.00   68
  8  \w     72.00 164.00   0.50    0.58    --   96.04  68.00-120.00  184
  9  \w     74.00 163.00   0.50    0.58    --   96.04  59.00 -30.00  178
 10  \w     74.00 163.00   0.50    0.58    --   96.04  59.00   0.00  178
 11  \w     74.00 163.00   0.50    0.58    --   96.04  59.00  30.00  178
 12  \w     74.00 163.00   0.50    0.58    --   96.04  59.00  60.00  178
 13  \w     72.00 164.00   0.50    0.58    --   96.04  68.00  90.00  184
 14  \w     72.00 164.00   0.50    0.58    --   96.04  68.00 120.00  184
 15  \w     72.00 164.00   0.50    0.58    --   96.04  68.00 150.00  184
 16  \w     79.00 162.00   0.50    0.58    --   96.04  42.00 -60.00  166
 17  \w     71.00 169.00   0.50    0.58    --   96.04  18.00-106.00  196
 18  \w     82.00 164.00   0.50    0.58    --   96.04  33.00-150.00  164
 19  \w    -32.00  26.00   0.50    0.20    --   40.83 -18.00  85.00  116
 20  \w    -25.00  48.00   0.50    0.20    --   40.83 -43.00 150.00  146
 21  \w    -31.00  28.00   0.50    0.20    --   40.83 -21.00-180.00  118
 22  \w     90.00 162.00   0.50    0.58    --   96.04 132.00 109.00  144
 23  \w    103.00 164.00   0.50    0.58    --   96.04 108.00  32.00  122
 24  \w     29.00  57.00   0.50    0.58    --   96.04 -50.00 -60.00   56
 25  \w     28.00  68.00   0.50    0.58    --   96.04 -59.00 -90.00   80
 26  \w     28.00  68.00   0.50    0.58    --   96.04 -59.00-180.00   80
 27  \w     29.00  57.00   0.50    0.58    --   96.04 -50.00-150.00   56
 28  \w     29.00  57.00   0.50    0.58    --   96.04 -50.00 -30.00   56
 29  \w     29.00  57.00   0.50    0.58    --   96.04 -50.00   0.00   56
 30  \w     28.00  68.00   0.50    0.58    --   96.04 -59.00  90.00   80
 31  \w     29.00  57.00   0.50    0.58    --   96.04 -50.00 150.00   56
 32  \w     38.00 117.00   0.50    0.58    --   96.04-132.00  39.00  158
 33  \w     32.00 110.00   0.50    0.58    --   96.04-117.00 120.00  156
 34  \w     28.00 109.00   0.50    0.58    --   96.04-108.00 -64.00  162
 35  \w     23.00 106.00   0.50    0.58    --   96.04 -96.00-180.00  166
 36  \w     21.00  79.00   0.50    0.20    --   40.83-108.00 -64.00  116
 37  \w    -83.00 -15.00   0.50    0.58    --  -82.50 108.00  32.00  136
 38  \w    -97.00 -19.00   0.50    0.20    --  -40.83 138.00 -74.00  156
 39  \w    -96.00 -19.00   0.50    0.58    --  -82.50 138.00 -74.00  154
 40  \w    -79.00   1.00   0.50    0.20    --  -40.83 108.00  32.00  160
 41  \w    -47.00 -15.00   0.50    0.58    --  -82.50  42.00   0.00   64
 42  \w    -26.00  32.00   0.50    0.20    --  -40.83  18.00-106.00  116
 43  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00  60.00  118
 44  \w   -114.00 -17.00   0.50    0.20    --  -40.83 -18.00  85.00  194
 45  \w   -108.00 -17.00   0.50    0.20    --  -40.83 -65.00  30.00  182
 46  \w   -109.00 -14.00   0.50    0.20    --  -40.83 -77.00 120.00  190
 47  \w   -155.00 -59.00   0.50    0.58    --  -82.50 -18.00  85.00  192
 48  \w   -150.00 -82.00   0.50    0.58    --  -82.50-108.00 -64.00  136
 49  \w   -150.00 -64.00   0.50    0.58    --  -82.50-138.00-136.00  172
 50  \w   -148.00 -68.00   0.50    0.58    --  -82.50-132.00  39.00  160
;
_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      -0.0428937000
_diffrn_orient_matrix_UB_12      0.1231265000
_diffrn_orient_matrix_UB_13      -0.0268887000
_diffrn_orient_matrix_UB_21      0.0077969000
_diffrn_orient_matrix_UB_22      -0.0348052000
_diffrn_orient_matrix_UB_23      -0.0973379000
_diffrn_orient_matrix_UB_31      -0.1790781000
_diffrn_orient_matrix_UB_32      -0.0310088000
_diffrn_orient_matrix_UB_33      0.0021656000
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20082
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.097
_diffrn_reflns_theta_min         4.763
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36402
_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 reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1062 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2700
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0229
_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/[\s^2^(Fo^2^)+(0.0383P)^2^+0.2664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                2623
_reflns_number_total             2700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01503k2.cif
_cod_data_source_block           OC
_cod_depositor_comments
'Adding full bibliography for 7719267--7719270.cif.'
_cod_database_code               7719268
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.463
_shelx_estimated_absorpt_t_min   0.299
_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,H) groups
2. Restrained distances
 O5-H5B = O5-H5A
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C10(H10), C11(H11), C12(H12)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              71508
_shelx_hkl_checksum              49306
_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 1.902
_oxdiff_exptl_absorpt_empirical_full_min 0.658