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_7719270
_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         'C21 H28 Mo N4 O5'
_chemical_formula_sum            'C21 H28 Mo N4 O5'
_chemical_formula_weight         512.41
_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             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                 100.1352(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.83307(4)
_cell_length_b                   24.99920(13)
_cell_length_c                   14.20530(8)
_cell_measurement_reflns_used    25217
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.9010
_cell_measurement_theta_min      3.5320
_cell_volume                     2388.70(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 0.997
_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    -35.00  24.00   0.50    0.20    --   40.83 -11.00-180.00  118
  2  \w    -35.00  24.00   0.50    0.20    --   40.83 -11.00-120.00  118
  3  \w    -25.00  48.00   0.50    0.20    --   40.83 -43.00 -30.00  146
  4  \w    -35.00  24.00   0.50    0.20    --   40.83 -11.00 -60.00  118
  5  \w     29.00  57.00   0.50    0.26    --   96.04 -50.00-180.00   56
  6  \w     29.00  57.00   0.50    0.26    --   96.04 -50.00-150.00   56
  7  \w     27.00 105.00   0.50    0.26    --   96.04 -77.00 -30.00  156
  8  \w     28.00  83.00   0.50    0.26    --   96.04 -68.00  30.00  110
  9  \w     27.00 105.00   0.50    0.26    --   96.04 -77.00 120.00  156
 10  \w     29.00  57.00   0.50    0.26    --   96.04 -50.00 150.00   56
 11  \w     23.00 106.00   0.50    0.26    --   96.04 -96.00  30.00  166
 12  \w     41.00 101.00   0.50    0.20    --   40.83-139.00 175.00  120
 13  \w     41.00 123.00   0.50    0.26    --   96.04-139.00 175.00  164
 14  \w     37.00 117.00   0.50    0.26    --   96.04-131.00  -9.00  160
 15  \w     44.00 127.00   0.50    0.26    --   96.04-145.00 -30.00  166
 16  \w     37.00  94.00   0.50    0.20    --   40.83-131.00  -9.00  114
 17  \w    -24.00  35.00   0.50    0.20    --  -40.83  11.00-180.00  118
 18  \w    -37.00  27.00   0.50    0.20    --  -40.83  32.00-120.00  128
 19  \w    -24.00  35.00   0.50    0.20    --  -40.83  11.00 -60.00  118
 20  \w    -47.00 -15.00   0.50    0.26    --  -82.50  42.00  30.00   64
 21  \w    -47.00 -15.00   0.50    0.26    --  -82.50  42.00  90.00   64
 22  \w    -47.00 -15.00   0.50    0.26    --  -82.50  42.00 120.00   64
 23  \w    -91.00 -15.00   0.50    0.20    --  -40.83 131.00  60.00  152
 24  \w    -91.00 -17.00   0.50    0.26    --  -82.50 131.00  60.00  148
 25  \w    -97.00 -20.00   0.50    0.26    --  -82.50 139.00-124.00  154
 26  \w    -97.00 -20.00   0.50    0.20    --  -40.83 139.00-124.00  154
 27  \w     81.00 166.00   0.50    0.26    --   96.04  25.00  60.00  170
 28  \w     69.00 165.00   0.50    0.26    --   96.04  77.00 120.00  192
 29  \w     72.00 164.00   0.50    0.26    --   96.04  68.00  90.00  184
 30  \w     72.00 164.00   0.50    0.26    --   96.04  68.00  60.00  184
 31  \w     72.00 164.00   0.50    0.26    --   96.04  68.00   0.00  184
 32  \w     18.00 109.00   0.50    0.20    --   40.83  65.00-120.00  182
 33  \w     74.00 163.00   0.50    0.26    --   96.04  59.00-180.00  178
 34  \w     81.00 166.00   0.50    0.26    --   96.04  25.00-120.00  170
 35  \w     77.00 163.00   0.50    0.26    --   96.04  50.00 -60.00  172
 36  \w     79.00 162.00   0.50    0.26    --   96.04  42.00 150.00  166
 37  \w     74.00 163.00   0.50    0.26    --   96.04  59.00 -30.00  178
 38  \w    105.00 170.00   0.50    0.26    --   96.04  96.00-150.00  130
 39  \w    105.00 170.00   0.50    0.26    --   96.04  96.00-120.00  130
 40  \w     85.00 163.00   0.50    0.26    --   96.04 139.00-124.00  156
 41  \w     99.00 160.00   0.50    0.26    --   96.04 117.00 -90.00  122
 42  \w     91.00 162.00   0.50    0.26    --   96.04 131.00  60.00  142
 43  \w     99.00 160.00   0.50    0.26    --   96.04 117.00 -30.00  122
 44  \w      8.00  35.00   0.50    0.20    --   40.83  93.00-170.67   54
 45  \w     12.00  43.00   0.50    0.20    --   40.83  83.00 -85.95   62
 46  \w     13.00  43.00   0.50    0.20    --   40.83  81.00 -37.76   60
 47  \w     11.00  43.00   0.50    0.20    --   40.83  85.00  -1.07   64
 48  \w     13.00  43.00   0.50    0.20    --   40.83  82.00  59.79   60
 49  \w     13.00  43.00   0.50    0.20    --   40.83  81.00  98.08   60
 50  \w     13.00  43.00   0.50    0.20    --   40.83  81.00 152.68   60
 51  \w   -107.00 -24.00   0.50    0.20    --  -40.83 -43.00 150.00  166
 52  \w   -108.00 -17.00   0.50    0.20    --  -40.83 -65.00 120.00  182
 53  \w   -107.00 -24.00   0.50    0.20    --  -40.83 -43.00  30.00  166
 54  \w   -108.00 -21.00   0.50    0.20    --  -40.83 -54.00   0.00  174
 55  \w   -108.00 -21.00   0.50    0.20    --  -40.83 -54.00 -60.00  174
 56  \w   -151.00 -55.00   0.50    0.26    --  -82.50 -77.00 -60.00  192
 57  \w   -151.00 -55.00   0.50    0.26    --  -82.50 -77.00-120.00  192
 58  \w   -150.00 -69.00   0.50    0.26    --  -82.50 -33.00-120.00  162
 59  \w   -151.00 -56.00   0.50    0.26    --  -82.50 -74.00  18.99  190
 60  \w   -148.00 -69.00   0.50    0.26    --  -82.50-131.00  -9.00  158
 61  \w   -151.00 -63.00   0.50    0.26    --  -82.50-139.00 175.00  176
;
_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      -0.0948377000
_diffrn_orient_matrix_UB_12      -0.0556703000
_diffrn_orient_matrix_UB_13      -0.0200635000
_diffrn_orient_matrix_UB_21      0.1942787000
_diffrn_orient_matrix_UB_22      -0.0263238000
_diffrn_orient_matrix_UB_23      0.0503993000
_diffrn_orient_matrix_UB_31      -0.0756701000
_diffrn_orient_matrix_UB_32      0.0021863000
_diffrn_orient_matrix_UB_33      0.0958866000
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            36941
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.040
_diffrn_reflns_theta_min         3.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.809
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59570
_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 yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4338
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0401P)^2^+0.8029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4061
_reflns_number_total             4338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01503k2.cif
_cod_data_source_block           TC
_cod_depositor_comments
'Adding full bibliography for 7719267--7719270.cif.'
_cod_database_code               7719270
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.513
_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. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C21-H5
 1.873381 with sigma of 0.02
 Mo1-H5
 2.877017 with sigma of 0.02
3.a Me refined with riding coordinates:
 C21(H21a,H21b,H21c)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C10(H10), C12(H12)
3.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C18(H18a,H18b,
 H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c)
;
_shelx_res_checksum              80702
_shelx_hkl_checksum              44787
_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 1.321
_oxdiff_exptl_absorpt_empirical_full_min 0.820