Synthesis, characterization, and biological applications of zinc(ii) complexes of the methylthiosalicylate ligand
Pratap, Rajesh; Kumari, Soni; Chaturvedi, Nishtha; Mishra, Rajnikant; Bhattacharya, Subrato; New Journal of Chemistry 48 (2024) 19763–19778; doi:10.1039/D4NJ03927K

data_7063522
_publ_section_title
;
 Synthesis, characterization, and biological applications of zinc(ii)
 complexes of the methylthiosalicylate ligand
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19763
_journal_page_last               19778
_journal_paper_doi               10.1039/D4NJ03927K
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C28 H22 N2 O4 S2 Zn'
_chemical_formula_sum            'C28 H22 N2 O4 S2 Zn'
_chemical_formula_weight         579.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-11-04 deposited with the CCDC.	2024-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.315(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2575(4)
_cell_length_b                   29.5010(8)
_cell_length_c                   10.2104(4)
_cell_measurement_reflns_used    24586
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.6110
_cell_measurement_theta_min      2.3710
_cell_volume                     2579.69(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.83a (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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_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     18.00  61.00   0.50   21.85    --   11.77-132.00  42.00   86
  2  \w     18.00  69.00   0.50   21.85    --   11.77-137.00-134.00  102
  3  \w    -74.00 -33.00   0.50   21.85    --  -11.14 -38.00-180.00   82
  4  \w    -26.00  23.00   0.50   21.85    --  -11.14 -99.00 120.00   98
  5  \w    -78.00 -28.00   0.50   21.85    --  -11.14 -57.00 -60.00  100
  6  \w    -30.00  -1.00   0.50   21.85    --  -11.14 -38.00-180.00   58
  7  \w    -23.00   8.00   0.50   21.85    --  -11.14 -99.00 -30.00   62
  8  \w    -22.00   9.00   0.50   21.85    --  -11.14 -57.00 -60.00   62
  9  \w     -6.00  53.00   0.50   21.85    --  -11.14  38.00-120.00  118
 10  \w    -25.00  50.00   0.50   21.85    --  -11.14  38.00-150.00  150
 11  \w    -25.00  21.00   0.50   21.85    --  -11.14  38.00  30.00   92
 12  \w    -74.00 -40.00   0.50   21.85    --  -11.14 -38.00  60.00   68
 13  \w    -24.00  22.00   0.50   21.85    --  -11.14 -99.00 -60.00   92
 14  \w    -21.00   4.00   0.50   21.85    --  -11.14 -38.00  60.00   50
 15  \w    -18.00  13.00   0.50   21.85    --  -11.14 -99.00   0.00   62
 16  \w    -20.00  22.00   0.50   21.85    --  -11.14 -99.00-180.00   84
 17  \w    -26.00  15.00   0.50   21.85    --  -11.14 -99.00-120.00   82
 18  \w    -23.00   3.00   0.50   21.85    --  -11.14 -99.00  90.00   52
 19  \w     40.00  76.00   0.50   21.85    --   11.77  57.00 -90.00   72
 20  \w     -5.00  32.00   0.50   21.85    --   11.77  57.00 -90.00   74
 21  \w    -14.00  42.00   0.50   21.85    --   11.77  77.00  90.00  112
 22  \w    -39.00  28.00   0.50   21.85    --   11.77 -57.00-180.00  134
 23  \w      2.00  67.00   0.50   21.85    --   11.77  57.00 -60.00  130
 24  \w     11.00  38.00   0.50   21.85    --   11.77-125.00 -60.00   54
 25  \w    -22.00  29.00   0.50   21.85    --   11.77 -99.00 -60.00  102
 26  \w     19.00  44.00   0.50   21.85    --   11.77-125.00  90.00   50
 27  \w    -54.00  16.00   0.50   21.85    --   11.77 -38.00 -90.00  140
 28  \w    -61.00  -2.00   0.50   21.85    --   11.77 -19.00 120.00  118
 29  \w    -52.00  14.00   0.50   21.85    --   11.77 -38.00  90.00  132
 30  \w    -20.00   5.00   0.50   21.85    --   11.77 -19.00 150.00   50
 31  \w    -46.00  -4.00   0.50   21.85    --   11.77 -19.00-150.00   84
 32  \w    -41.00 -15.00   0.50   21.85    --   11.77 -57.00  60.00   52
 33  \w     51.00  79.00   0.50   21.85    --   11.77  57.00  30.00   56
 34  \w     -4.00  21.00   0.50   21.85    --   11.77 -38.00-150.00   50
 35  \w      5.00  30.00   0.50   21.85    --   11.77 -57.00  60.00   50
 36  \w     -3.00  22.00   0.50   21.85    --   11.77 -38.00 -30.00   50
 37  \w    -58.00 -33.00   0.50   21.85    --   11.77 -19.00 150.00   50
 38  \w    -35.00  -7.00   0.50   21.85    --   11.77 -19.00  90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0278309000
_diffrn_orient_matrix_UB_12      -0.0053531000
_diffrn_orient_matrix_UB_13      -0.0731477000
_diffrn_orient_matrix_UB_21      0.0050302000
_diffrn_orient_matrix_UB_22      -0.0234393000
_diffrn_orient_matrix_UB_23      0.0166524000
_diffrn_orient_matrix_UB_31      -0.0778368000
_diffrn_orient_matrix_UB_32      0.0003943000
_diffrn_orient_matrix_UB_33      -0.0030829000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0860
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            61670
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.081
_diffrn_reflns_theta_min         2.378
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.59(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         10870
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0763P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1508
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                6179
_reflns_number_total             10870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03927k2.cif
_cod_data_source_block           zn-5_auto
_cod_depositor_comments
'Adding full bibliography for 7063519--7063522.cif.'
_cod_original_cell_volume        2579.68(19)
_cod_database_code               7063522
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'Zn C H O N S'
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.41(2)
 0.59(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed U11: C25(0.041525) C26(0.041781) C21(0.039098) C22(0.058273)
 C24(0.061049) C23(0.060387)
 Fixed U12: C25(0.007771) C26(0.006343) C21(0.00427) C22(-0.006446)
 C24(0.010095) C23(0.015552)
 Fixed U13: C25(0.00322) C26(-0.000613) C21(-0.002393) C22(-0.003622)
 C24(0.009988) C23(-0.00589)
 Fixed U22: C25(0.07155) C26(0.058) C21(0.06725) C22(0.06464) C24(0.07646)
 C23(0.05569)
 Fixed U23: C25(0.00822) C26(0.0068) C21(0.0084) C22(0.01689) C24(0.00411)
 C23(-0.0075)
 Fixed U33: C25(0.06624) C26(0.04566) C21(0.05674) C22(0.09879) C24(0.0719)
 C23(0.11838)
4.a Riding coordinates:
 C30(H30)
4.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C5(H5), C29(H29), C25(H25), C3(H3), C45(H45), C1(H1), C6(H6),
 C8(H8), C22(H22), C34(H34), C44(H44), C10(H10), C9(H9), C43(H43), C24(H24),
 C23(H23), C50(H50), C37(H37), C36(H36), C38(H38), C33(H33), C14(H14), C51(H51),
  C2(H2), C15(H15), C17(H17), C16(H16), C52(H52), C53(H53)
4.c Idealised Me refined as rotating group:
 C48(H48a,H48b,H48c), C28(H28a,H28b,H28c), C56(H56a,H56b,H56c), C20(H20a,H20b,
 H20c)
;
_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 1.195
_oxdiff_exptl_absorpt_empirical_full_min 0.813