Structural studies on thiosalicylate complexes of Zn(II) & Hg(II). First insight into Zn(II)-thiosalicylate complex as potential antibacterial, antibiofilm and anti-tumour agent
Nayak, Mousumi; Kumar Singh, Ashish; Prakash, Pradyot; Kant, Rajni; Bhattacharya, Subrato; Inorganica Chimica Acta 501 (2020) 119263–; doi:10.1016/j.ica.2019.119263

data_1565615
_publ_section_title
;
 Structural studies on thiosalicylate complexes of Zn(II) & Hg(II). First
 insight into Zn(II)-thiosalicylate complex as potential antibacterial,
 antibiofilm and anti-tumour agent
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119263
_journal_paper_doi               10.1016/j.ica.2019.119263
_journal_volume                  501
_journal_year                    2020
_chemical_formula_moiety         'C14 H8 Hg O4 S2, C6 H18 N2'
_chemical_formula_sum            'C20 H26 Hg N2 O4 S2'
_chemical_formula_weight         623.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   12.1384(5)
_cell_length_b                   65.810(2)
_cell_length_c                   11.2189(5)
_cell_measurement_reflns_used    8100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.9830
_cell_measurement_theta_min      5.3600
_cell_volume                     8962.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4622
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_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   -129.00 -34.50   0.75    4.00    --  -38.45 178.00 -90.00  126
  2  \w    -53.00 130.00   0.75    4.00    --   38.45   0.00   0.00  244
  3  \w     57.00 130.50   0.75    4.00    --   38.45 178.00-120.00   98
  4  \w     28.00 115.00   0.75   16.00    --  109.73-111.00 -30.00  116
  5  \w     23.00 108.50   0.75   16.00    --  109.73 -94.00-120.00  114
  6  \w    100.00 178.00   0.75   16.00    --  109.73 111.00 150.00  104
  7  \w    100.00 178.00   0.75   16.00    --  109.73 111.00 -60.00  104
  8  \w     28.00 115.00   0.75   16.00    --  109.73-111.00   0.00  116
  9  \w     74.00 177.50   0.75   16.00    --  109.73  77.00  30.00  138
 10  \w     79.00 178.00   0.75   16.00    --  109.73  45.00 150.00  132
 11  \w   -116.00  -6.50   0.75    4.00    --  -38.45 -57.00-180.00  146
 12  \w   -122.00  -2.00   0.75    4.00    --  -38.45 -77.00 120.00  160
 13  \w      2.00 122.00   0.75    4.00    --   38.45  77.00   0.00  160
 14  \w     77.00 177.50   0.75   16.00    --  109.73  61.00  90.00  134
 15  \w     72.00 177.00   0.75   16.00    --  109.73  30.00 -30.00  140
 16  \w     74.00 177.50   0.75   16.00    --  109.73  77.00-180.00  138
 17  \w     28.00  55.00   0.75   16.00    --  109.73-111.00 150.00   36
 18  \w     77.00 177.50   0.75   16.00    --  109.73  61.00   0.00  134
 19  \w     77.00 177.50   0.75   16.00    --  109.73  61.00-120.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0971540000
_diffrn_orient_matrix_UB_12      0.0191900000
_diffrn_orient_matrix_UB_13      0.0161440000
_diffrn_orient_matrix_UB_21      0.0362757500
_diffrn_orient_matrix_UB_22      -0.1079723000
_diffrn_orient_matrix_UB_23      0.0106572500
_diffrn_orient_matrix_UB_31      0.0900475500
_diffrn_orient_matrix_UB_32      0.0640099000
_diffrn_orient_matrix_UB_33      0.0131574500
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1307
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       77
_diffrn_reflns_limit_k_min       -77
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17295
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.018
_diffrn_reflns_theta_max         67.018
_diffrn_reflns_theta_min         5.377
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.303
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.050
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       rod
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.096
_refine_diff_density_max         3.504
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.215
_refine_ls_abs_structure_details
;
 Flack x determined using 1561 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3817
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1071P)^2^+570.1819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2227
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                3721
_reflns_number_total             3817
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.3271\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [-0.11 -0.08 0.99] (direct)
;
_cod_data_source_file            ICA-2020-501-119263.cif
_cod_data_source_block           mn2_cu_twin1_hklf4
_cod_database_code               1565615
_chemical_oxdiff_formula         'Hg1 C20 N2 O4 S2 H24'
_diffrn_oxdiff_ac3_digest_frames
;
01e943237e09bfb9a969509682db5591cd0247426be
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N005(H005), N006(H006)
2.b Secondary CH2 refined with riding coordinates:
 C00E(H00D,H00E), C00S(H00V,H00W)
2.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K), C00T(H00T), C00O(H00O), C00Q(H00Q), C00P(H00P),
 C00M(H00M), C008(H008)
2.d Fitted hexagon refined as free rotating group:
 C00C(C00I,C00K,C00T,C00O,C00J), C00D(C00Q,C00P,C00M,C008,C00N)
2.e Idealised Me refined as rotating group:
 C009(H00A,H00B,H00C), C00G(H00F,H00G,H00H), C00L(H00J,H00L,H00N), C00R(H00R,
 H00S,H00U)
;
_shelx_res_checksum              80455
_shelx_hkl_checksum              44167
_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 2.222
_oxdiff_exptl_absorpt_empirical_full_min 0.392
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2