Synthesis of (3-nitro-2-oxo-benzaldehyde thiosemicarbazonato)-zinc(II) complexes: the position of nitro group in phenyl ring alters antimicrobial activity against <i>K. pneumoniae</i> 1, <i>S. typhimurium</i> 2, MRSA and <i>C. albicans</i>.
Lobana, Tarlok S.; Indoria, Shikha; Sood, Henna; Arora, Daljit S.; Kaur, Manpreet; Jasinski, Jerry P.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6823–6833; doi:10.1039/d1dt00657f

data_7707145
_publ_section_title
;
 Synthesis of (3-nitro-2-oxo-benzaldehyde thiosemicarbazonato)-zinc(II)
 complexes: the position of nitro group in phenyl ring alters
 antimicrobial activity against <i>K. pneumoniae</i> 1, <i>S.
 typhimurium</i> 2, MRSA and <i>C. albicans</i>.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6823
_journal_page_last               6833
_journal_paper_doi               10.1039/d1dt00657f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C22 H18 N6 O3 S Zn, 1.5(H2 O)'
_chemical_formula_sum            'C22 H21 N6 O4.5 S Zn'
_chemical_formula_weight         538.87
_chemical_name_systematic        JPL-176
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2021-03-24 deposited with the CCDC.	2021-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                109.265(6)
_cell_angle_beta                 94.725(5)
_cell_angle_gamma                113.463(7)
_cell_formula_units_Z            4
_cell_length_a                   12.1163(8)
_cell_length_b                   13.7570(10)
_cell_length_c                   17.8138(9)
_cell_measurement_reflns_used    8041
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.5420
_cell_measurement_theta_min      3.4230
_cell_volume                     2491.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0416
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_details
;
  1 omega  -30.00    2.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -      -23.9612  -19.0000   30.0000 32

  2 omega  -40.00   10.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -77.0000    0.0000 50

  3 omega  -43.00   -5.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -19.0000  -60.0000 38

  4 omega    6.00   35.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -57.0000 -150.0000 29

  5 omega    1.00   71.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -       25.9925   77.0000  -60.0000 70

  6 omega    4.00   81.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -       25.9925   77.0000   30.0000 77

  7 omega   -1.00   92.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -       25.9925   77.0000 -150.0000 93

  8 omega  -24.00   65.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -99.0000  120.0000 89

  9 omega  -93.00  -37.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -      -23.9612  -19.0000   30.0000 56

 10 omega  -89.00  -64.00   1.0000   15.0750
omega____ theta____ kappa____ phi______ frames
    -      -23.9612  -21.0000  -53.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0657882000
_diffrn_orient_matrix_UB_12      -0.0253338000
_diffrn_orient_matrix_UB_13      -0.0105153000
_diffrn_orient_matrix_UB_21      -0.0028598000
_diffrn_orient_matrix_UB_22      -0.0546561000
_diffrn_orient_matrix_UB_23      -0.0060520000
_diffrn_orient_matrix_UB_31      -0.0000456000
_diffrn_orient_matrix_UB_32      0.0110181000
_diffrn_orient_matrix_UB_33      0.0418034000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34122
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.750
_diffrn_reflns_theta_min         3.029
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         16383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0868P)^2^+0.5585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9944
_reflns_number_total             16383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00657f2.cif
_cod_data_source_block           jpl-176
_cod_depositor_comments
;
Adding full bibliography for 7707144--7707147.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H42 N12 O9 S2 Zn2'
_cod_original_formula_weight         1077.75
_cod_original_formula_moiety         '2(C22 H18 N6 O3 S Zn), 3(H2 O)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2491.7(3)
_cod_database_code               7707145
_chemical_oxdiff_formula         'C22 H24 N6 S O3 Zn'
_chemical_oxdiff_usercomment     'Lobana's JPL-176'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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, All O(H,H) groups
2.a Free rotating group:
 O1SA(H1SA,H1SB), O1SB(H1SC,H1SD), O1SC(H1SE,H1SF)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C9A(H9AA,H9AB)
2.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C3(H3A), C4(H4), C5(H5), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), N3A(H3AA), C1A(H1A),
 C3A(H3AB), C4A(H4A), C5A(H5A), C13A(H13A), C14A(H14A), C15A(H15A), C17A(H17A),
 C18A(H18A), C20A(H20A), C21A(H21A), C22A(H22A)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              79601
_shelx_hkl_checksum              89896
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id JPL-176
_olex2_submission_special_instructions 'No special instructions were received'