Catalytic oxidation of tetralin by dioxomolybdenum complexes: design, synthesis, characterization and DFT investigations
Nafisa,; Rana, Lata; Mahiya, Kuldeep; New Journal of Chemistry 50 (2026) 798–809; doi:10.1039/D5NJ04083C

data_7064327
_publ_section_title
;
 Catalytic oxidation of tetralin by dioxomolybdenum complexes: design,
 synthesis, characterization and DFT investigations
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              798
_journal_page_last               809
_journal_paper_doi               10.1039/D5NJ04083C
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C19 H22 Mo N2 O8 S'
_chemical_formula_sum            'C19 H22 Mo N2 O8 S'
_chemical_formula_weight         534.38
_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     dual
_audit_creation_date             2025-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-10-12 deposited with the CCDC.	2025-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.21100(10)
_cell_length_b                   8.01890(10)
_cell_length_c                   29.0172(2)
_cell_measurement_reflns_used    14904
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.9300
_cell_measurement_theta_min      3.0360
_cell_volume                     2139.74(4)
_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    -68.00  28.00   0.50    0.20    --  -40.83  77.00-120.00  192
  2  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00 -30.00  118
  3  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00  60.00  118
  4  \w    -37.00  27.00   0.50    0.20    --  -40.83  32.00  90.00  128
  5  \w    -37.00  27.00   0.50    0.20    --  -40.83  32.00 150.00  128
  6  \w     71.00 169.00   0.50    0.50    --   96.04  17.00 120.00  196
  7  \w     95.00 160.00   0.50    0.50    --   96.04 124.00 121.00  130
  8  \w     81.00 164.00   0.50    0.50    --   96.04 145.00  90.00  166
  9  \w    105.00 170.00   0.50    0.50    --   96.04  96.00  90.00  130
 10  \w     99.00 160.00   0.50    0.50    --   96.04 117.00 -30.00  122
 11  \w     79.00 164.00   0.50    0.50    --   96.04 147.00 -72.00  170
 12  \w     99.00 160.00   0.50    0.50    --   96.04 117.00-150.00  122
 13  \w     14.00 110.00   0.50    0.20    --   40.83  77.00 -90.00  192
 14  \w     21.00 108.00   0.50    0.20    --   40.83  54.00-120.00  174
 15  \w     21.00 108.00   0.50    0.20    --   40.83  54.00-180.00  174
 16  \w     14.00 110.00   0.50    0.20    --   40.83  77.00   0.00  192
 17  \w     14.00 110.00   0.50    0.20    --   40.83  77.00  90.00  192
 18  \w    -35.00  24.00   0.50    0.20    --   40.83 -11.00  90.00  118
 19  \w     28.00  83.00   0.50    0.50    --   96.04 -68.00  90.00  110
 20  \w     29.00  57.00   0.50    0.50    --   96.04 -50.00  30.00   56
 21  \w    -35.00  24.00   0.50    0.20    --   40.83 -11.00 -90.00  118
 22  \w     29.00  57.00   0.50    0.50    --   96.04 -50.00-180.00   56
 23  \w     29.00  57.00   0.50    0.50    --   96.04 -50.00-150.00   56
 24  \w     27.00 105.00   0.50    0.50    --   96.04 -77.00-150.00  156
 25  \w     45.00 106.00   0.50    0.20    --   40.83-147.00-121.00  122
 26  \w     23.00 106.00   0.50    0.50    --   96.04 -96.00-180.00  166
 27  \w     45.00 128.00   0.50    0.50    --   96.04-147.00-121.00  166
 28  \w     23.00 106.00   0.50    0.50    --   96.04 -96.00  60.00  166
 29  \w     32.00 110.00   0.50    0.50    --   96.04-117.00  90.00  156
 30  \w     33.00 111.00   0.50    0.50    --   96.04-124.00  43.00  156
 31  \w     33.00  89.00   0.50    0.20    --   40.83-124.00  43.00  112
 32  \w   -108.00 -17.00   0.50    0.20    --  -40.83 -65.00  90.00  182
 33  \w   -108.00 -21.00   0.50    0.20    --  -40.83 -54.00 -90.00  174
 34  \w   -108.00 -21.00   0.50    0.20    --  -40.83 -54.00 -30.00  174
 35  \w   -107.00 -24.00   0.50    0.20    --  -40.83 -43.00   0.00  166
 36  \w   -156.00 -83.00   0.50    0.50    --  -82.50 -96.00  90.00  146
 37  \w   -108.00 -57.00   0.50    0.20    --  -40.83-147.00-121.00  102
 38  \w   -151.00 -57.00   0.50    0.50    --  -82.50-147.00-121.00  188
 39  \w   -147.00 -73.00   0.50    0.50    --  -82.50-124.00  43.00  148
 40  \w    -47.00 -15.00   0.50    0.50    --  -82.50  42.00 -30.00   64
 41  \w   -103.00 -24.00   0.50    0.20    --  -40.83 147.00 -72.00  158
 42  \w    -86.00 -11.00   0.50    0.20    --  -40.83 124.00 121.00  150
 43  \w    -85.00 -18.00   0.50    0.50    --  -82.50 124.00 121.00  134
;
_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      0.1533479000
_diffrn_orient_matrix_UB_12      0.0238408000
_diffrn_orient_matrix_UB_13      -0.0175723000
_diffrn_orient_matrix_UB_21      -0.0138051000
_diffrn_orient_matrix_UB_22      0.1900161000
_diffrn_orient_matrix_UB_23      0.0062591000
_diffrn_orient_matrix_UB_31      0.0660776000
_diffrn_orient_matrix_UB_32      -0.0154600000
_diffrn_orient_matrix_UB_33      0.0497887000
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21524
_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         68.070
_diffrn_reflns_theta_min         3.051
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.369
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49005
_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 pinkish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.00054(5)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0311P)^2^+1.0146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3441
_reflns_number_total             3882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04083c2.cif
_cod_data_source_block           oval-3dm_auto
_cod_database_code               7064327
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.429
_shelx_estimated_absorpt_t_min   0.269
_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.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C10(H10), C14(H14), C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              59515
_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 1.458
_oxdiff_exptl_absorpt_empirical_full_min 0.744