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_7063521
_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         '2(C22 H30 N2 O4 S2 Zn), H2 O'
_chemical_formula_sum            'C44 H62 N4 O9 S4 Zn2'
_chemical_formula_weight         1049.95
_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     dual
_audit_creation_date             2023-08-03
_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                 90.253(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7007(3)
_cell_length_b                   16.6815(5)
_cell_length_c                   17.3948(6)
_cell_measurement_reflns_used    18016
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.6920
_cell_measurement_theta_min      2.4970
_cell_volume                     2524.67(14)
_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    '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 0.982
_diffrn_measured_fraction_theta_max 0.937
_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    -65.00  -1.00   0.50    3.60    --  -11.38 -72.00  11.00  128
  2  \w     37.00  66.00   0.50    3.60    --   11.61-133.00 133.00   58
  3  \w      0.00  26.00   0.50    3.60    --   11.61 -48.00-175.00   52
  4  \w     23.00  68.00   0.50    3.60    --   11.61-137.00 -43.00   90
  5  \w    -56.00 -12.00   0.50    3.60    --   11.61 -48.00-175.00   88
  6  \w    -23.00   6.00   0.50    3.60    --  -11.38 -99.00-180.00   58
  7  \w    -28.00  -3.00   0.50    3.60    --  -11.38 -48.00-175.00   50
  8  \w    -65.00 -40.00   0.50    3.60    --  -11.38 -48.00-175.00   50
  9  \w    -22.00  20.00   0.50    3.60    --  -11.38 -99.00 150.00   84
 10  \w    -23.00  22.00   0.50    3.60    --  -11.38 -99.00 -90.00   90
 11  \w    -17.00   8.00   0.50    3.60    --  -11.38 -99.00-150.00   50
 12  \w    -23.00  22.00   0.50    3.60    --  -11.38 -99.00 -30.00   90
 13  \w      0.00  64.00   0.50    3.60    --   11.61  38.00 150.00  128
 14  \w      2.00  28.00   0.50    3.60    --   11.61  38.00-150.00   52
 15  \w    -13.00  12.00   0.50    3.60    --   11.61 -38.00  30.00   50
 16  \w    -48.00 -22.00   0.50    3.60    --   11.61 -38.00  30.00   52
 17  \w    -40.00  14.00   0.50    3.60    --   11.61 -38.00 120.00  108
 18  \w     49.00  74.00   0.50    3.60    --   11.61  38.00-150.00   50
 19  \w    -60.00   5.00   0.50    3.60    --   11.61 -19.00 -90.00  130
 20  \w     16.00  43.00   0.50    3.60    --   11.61-125.00   0.00   54
 21  \w    -61.00 -48.50   0.50    3.60    --   11.61 -19.00 -30.00   25
;
_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      0.0148067000
_diffrn_orient_matrix_UB_12      0.0049809000
_diffrn_orient_matrix_UB_13      0.0398554000
_diffrn_orient_matrix_UB_21      0.0637243000
_diffrn_orient_matrix_UB_22      0.0248320000
_diffrn_orient_matrix_UB_23      -0.0086395000
_diffrn_orient_matrix_UB_31      -0.0486477000
_diffrn_orient_matrix_UB_32      0.0341423000
_diffrn_orient_matrix_UB_33      0.0005146000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29608
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.105
_diffrn_reflns_theta_min         2.613
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.83a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2359 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9744
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1038P)^2^+0.0739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.890
_reflns_Friedel_fraction_max     0.808
_reflns_number_gt                6889
_reflns_number_total             9744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03927k2.cif
_cod_data_source_block           zn-2again_auto
_cod_depositor_comments
'Adding full bibliography for 7063519--7063522.cif.'
_cod_database_code               7063521
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H O N S Zn'
_olex2_refinement_description
;
1. 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, All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B)
2.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C17(H17A,H17B), C39(H39A,H39B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C27(H27), C34(H34), C5(H5), C25(H25), C2(H2), C4(H4), C35(H35),
 C13(H13), C26(H26), C24(H24), C32(H32), C12(H12), C3(H3), C11(H11), C33(H33)
2.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C8(H8A,H8B,H8C), C19(H19A,H19B,
 H19C), C38(H38A,H38B,H38C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C44(H44A,
 H44B,H44C), C41(H41A,H41B,H41C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C),
 C21(H21A,H21B,H21C)
;
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.761