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_7064328
_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         'C18 H20 Mo N2 O7 S'
_chemical_formula_sum            'C18 H20 Mo N2 O7 S'
_chemical_formula_weight         504.36
_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   geom
_audit_creation_date             2025-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-04 deposited with the CCDC.	2025-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.9080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.57400(10)
_cell_length_b                   16.43340(10)
_cell_length_c                   14.39460(10)
_cell_measurement_reflns_used    19848
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.8450
_cell_measurement_theta_min      2.6540
_cell_volume                     2023.48(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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     32.00 110.00   0.50    0.41    --   96.04-117.00 120.00  156
  2  \w     44.00 127.00   0.50    0.41    --   96.04-145.00 -90.00  166
  3  \w    -31.00  28.00   0.50    0.20    --   40.83 -21.00 -30.00  118
  4  \w    -31.00  28.00   0.50    0.20    --   40.83 -21.00  90.00  118
  5  \w    105.00 166.00   0.50    0.41    --   96.04 104.00 161.00  122
  6  \w     32.00 110.00   0.50    0.41    --   96.04-117.00 -60.00  156
  7  \w     18.00  78.00   0.50    0.20    --   40.83-104.00  60.00  120
  8  \w     26.00 107.00   0.50    0.41    --   96.04-104.00  60.00  162
  9  \w     27.00 105.00   0.50    0.41    --   96.04 -77.00  60.00  156
 10  \w     28.00  83.00   0.50    0.41    --   96.04 -68.00  90.00  110
 11  \w     27.00 105.00   0.50    0.41    --   96.04 -77.00 120.00  156
 12  \w     28.00  68.00   0.50    0.41    --   96.04 -59.00 150.00   80
 13  \w     28.00  68.00   0.50    0.41    --   96.04 -59.00   0.00   80
 14  \w     29.00  57.00   0.50    0.41    --   96.04 -50.00 120.00   56
 15  \w     28.00  68.00   0.50    0.41    --   96.04 -59.00 -30.00   80
 16  \w     29.00  57.00   0.50    0.41    --   96.04 -50.00 -30.00   56
 17  \w     28.00  83.00   0.50    0.41    --   96.04 -68.00 -90.00  110
 18  \w     28.00  68.00   0.50    0.41    --   96.04 -59.00 -90.00   80
 19  \w     29.00  57.00   0.50    0.41    --   96.04 -50.00-120.00   56
 20  \w     29.00  57.00   0.50    0.41    --   96.04 -50.00-150.00   56
 21  \w     29.00  57.00   0.50    0.41    --   96.04 -50.00-180.00   56
 22  \w     28.00  68.00   0.50    0.41    --   96.04 -59.00-150.00   80
 23  \w     29.00  57.00   0.50    0.41    --   96.04 -50.00 -90.00   56
 24  \w     29.00  57.00   0.50    0.41    --   96.04 -50.00 -60.00   56
 25  \w     81.00 166.00   0.50    0.41    --   96.04  25.00  90.00  170
 26  \w     77.00 163.00   0.50    0.41    --   96.04  50.00 150.00  172
 27  \w     69.00 130.00   0.50    0.41    --   96.04  77.00 -30.00  122
 28  \w     79.00 162.00   0.50    0.41    --   96.04  42.00-150.00  166
 29  \w     74.00 163.00   0.50    0.41    --   96.04  59.00-120.00  178
 30  \w     74.00 163.00   0.50    0.41    --   96.04  59.00 -90.00  178
 31  \w     77.00 163.00   0.50    0.41    --   96.04  50.00 -60.00  172
 32  \w     81.00 166.00   0.50    0.41    --   96.04  25.00   0.00  170
 33  \w     77.00 163.00   0.50    0.41    --   96.04  50.00  30.00  172
 34  \w     79.00 162.00   0.50    0.41    --   96.04  42.00 120.00  166
 35  \w     21.00 108.00   0.50    0.20    --   40.83  54.00  60.00  174
 36  \w     14.00 110.00   0.50    0.20    --   40.83  77.00   0.00  192
 37  \w     14.00 110.00   0.50    0.20    --   40.83  77.00 -30.00  192
 38  \w     14.00 110.00   0.50    0.20    --   40.83  77.00  60.00  192
 39  \w     14.00 110.00   0.50    0.20    --   40.83  77.00 -60.00  192
 40  \w     14.00 110.00   0.50    0.20    --   40.83  77.00-120.00  192
 41  \w     14.00 110.00   0.50    0.20    --   40.83  77.00-150.00  192
 42  \w     14.00 110.00   0.50    0.20    --   40.83  77.00-180.00  192
 43  \w     18.00 109.00   0.50    0.20    --   40.83  65.00 120.00  182
 44  \w     18.00 109.00   0.50    0.20    --   40.83  65.00 150.00  182
 45  \w    -78.00   4.00   0.50    0.20    --  -40.83 104.00 161.00  164
 46  \w    -82.00 -12.00   0.50    0.41    --  -82.50 104.00 161.00  140
 47  \w    -78.00   4.00   0.50    0.20    --  -40.83 104.00 -60.00  164
 48  \w    -24.00  35.00   0.50    0.20    --  -40.83  11.00 -60.00  118
 49  \w    -37.00  27.00   0.50    0.20    --  -40.83  32.00-180.00  128
 50  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00 -30.00  118
 51  \w    -24.00  35.00   0.50    0.20    --  -40.83  11.00 120.00  118
 52  \w    -57.00 -16.00   0.50    0.41    --  -82.50  50.00 120.00   82
 53  \w    -47.00 -15.00   0.50    0.41    --  -82.50  42.00 150.00   64
 54  \w    -47.00 -15.00   0.50    0.41    --  -82.50  42.00 -30.00   64
 55  \w    -47.00 -15.00   0.50    0.41    --  -82.50  42.00-180.00   64
 56  \w   -109.00 -28.00   0.50    0.20    --  -40.83 -32.00-120.00  162
 57  \w   -150.00 -69.00   0.50    0.41    --  -82.50 -33.00-120.00  162
 58  \w   -153.00 -83.00   0.50    0.41    --  -82.50-104.00  60.00  140
;
_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      -0.1153993000
_diffrn_orient_matrix_UB_12      -0.0325276000
_diffrn_orient_matrix_UB_13      -0.0779745000
_diffrn_orient_matrix_UB_21      0.0016358000
_diffrn_orient_matrix_UB_22      0.0833035000
_diffrn_orient_matrix_UB_23      -0.0490212000
_diffrn_orient_matrix_UB_31      0.1382529000
_diffrn_orient_matrix_UB_32      -0.0281543000
_diffrn_orient_matrix_UB_33      -0.0549767000
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28038
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.089
_diffrn_reflns_theta_min         4.088
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57930
_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    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.00051(6)
_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   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3692
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0301P)^2^+0.9151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3447
_reflns_number_total             3692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj04083c2.cif
_cod_data_source_block           sac_auto
_cod_database_code               7064328
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.416
_shelx_estimated_absorpt_t_min   0.240
_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
 S1-O5 \\sim S1A-O5
 with sigma of 0.02
 S1-C17 \\sim S1A-C18A
 with sigma of 0.02
 S1-C18 \\sim S1A-C17A
 with sigma of 0.02
 O5-C17 \\sim O5-C18A
 with sigma of 0.04
 O5-C18 \\sim O5-C17A
 with sigma of 0.04
 C17-C18 \\sim C18A-C17A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1A \\sim C17 \\sim C17A \\sim C18 \\sim C18A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C17A) = Uanis(C17)
Uanis(S1) = Uanis(S1A)
4. Rigid body (RIGU) restrains
 S1, S1A, C17, C17A, C18, C18A
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.005
5. Others
 Sof(S1A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(S1)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F),
 C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              59071
_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 1.423
_oxdiff_exptl_absorpt_empirical_full_min 0.801