Synthesis of 2-acetylpyridine-N-substituted thiosemicarbazonates of copper(ii) with high antimicrobial activity against methicillin resistant S. aureus, K. pneumoniae 1 and C. albicans
Kaushal, Mani; Lobana, Tarlok S.; Nim, Lovedeep; Bala, Ritu; Arora, Daljit S.; Garcia-Santos, Isabel; Duff, Courtney E.; Jasinski, Jerry P.; New Journal of Chemistry 43 (2019) 11727–; doi:10.1039/C9NJ01459D

data_7058555
_publ_section_title
;
 Synthesis of 2-acetylpyridine-N-substituted thiosemicarbazonates of
 copper(ii) with high antimicrobial activity against methicillin resistant
 S. aureus, K. pneumoniae 1 and C. albicans
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11727
_journal_paper_doi               10.1039/C9NJ01459D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C10 H13 Cu I N4 S'
_chemical_formula_sum            'C10 H13 Cu I N4 S'
_chemical_formula_weight         411.74
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-02-05 deposited with the CCDC.    2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.277(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7000(3)
_cell_length_b                   8.8890(4)
_cell_length_c                   14.2638(4)
_cell_measurement_reflns_used    2278
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.3280
_cell_measurement_theta_min      4.1450
_cell_volume                     1354.44(8)
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro  (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015b)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0416
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -60.00 -10.00   1.00    2.10    --  -33.50  77.00   0.00   50
  2  \w    -94.00  -7.00   1.00    2.10    --  -33.50 -77.00-120.00   87
  3  \w    -82.00 -36.00   1.00    2.10    --  -33.50-178.00 -30.00   46
  4  \w     -1.00  58.00   1.00    2.10    --   35.36 -99.00  60.00   59
  5  \w     50.00 109.00   1.00    8.38    --  108.00 -94.00 -60.00   59
  6  \w     70.00 129.00   1.00    8.38    --  108.00 -30.00-150.00   59
  7  \w     40.00 103.00   1.00    8.38    --  108.00 -94.00   0.00   63
  8  \w     58.00  99.00   1.00    8.38    --  108.00 -94.00  90.00   41
  9  \w     42.00 119.00   1.00    8.38    --  108.00 -45.00 -30.00   77
 10  \w     70.00 176.00   1.00    8.38    --  108.00  15.00  60.00  106
 11  \w    131.00 157.00   1.00    8.38    --  108.00 111.00  90.00   26
 12  \w    112.00 157.00   1.00    8.38    --  108.00 111.00  30.00   45
 13  \w    102.00 127.00   1.00    8.38    --  108.00 111.00 -60.00   25
 14  \w    101.00 127.00   1.00    8.38    --  108.00 111.00  90.00   26
 15  \w    -69.00 -44.00   1.00    2.10    --  -33.50-178.00 150.00   25
 16  \w    -83.00 -37.00   1.00    2.10    --  -33.50-178.00  60.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku, Oxford diffraction'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0102782000
_diffrn_orient_matrix_UB_12      -0.1695625000
_diffrn_orient_matrix_UB_13      -0.0216621000
_diffrn_orient_matrix_UB_21      -0.1427416000
_diffrn_orient_matrix_UB_22      0.0162622000
_diffrn_orient_matrix_UB_23      -0.0176917000
_diffrn_orient_matrix_UB_31      0.0177216000
_diffrn_orient_matrix_UB_32      0.0323617000
_diffrn_orient_matrix_UB_33      -0.1044676000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.355
_diffrn_reflns_theta_min         5.032
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_description       prism
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.900
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0796P)^2^+0.0587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2302
_reflns_number_total             2581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01459d2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7058549--7058555.cif.'
_cod_database_code               7058555
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C14 H14 N5 S Cu I'
_chemical_oxdiff_usercomment     'Lobana's JPL-230-New'
_shelx_estimated_absorpt_t_max   0.359
_shelx_estimated_absorpt_t_min   0.055
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), C4(H4A), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              66168
_olex2_exptl_crystal_mounting_method 'POLYMER LOOP'
_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 4.116
_oxdiff_exptl_absorpt_empirical_full_min 0.541