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_7058550
_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 Br Cu N4 S'
_chemical_formula_sum            'C10 H13 Br Cu N4 S'
_chemical_formula_weight         364.75
_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             2018-01-10
_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                 108.471(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7061(5)
_cell_length_b                   14.2341(4)
_cell_length_c                   14.1240(5)
_cell_measurement_reflns_used    3507
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.1200
_cell_measurement_theta_min      4.5150
_cell_volume                     2613.56(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.980
_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    -46.00  34.00   1.00    1.96    --  -33.50  77.00 -30.00   80
  2  \w    -45.00  32.00   1.00    1.96    --  -33.50  37.00-120.00   77
  3  \w    -46.00  -8.00   1.00    1.96    --  -33.50  77.00  30.00   38
  4  \w    -97.00 -70.00   1.00    1.96    --  -33.50 178.00 -30.00   27
  5  \w     39.00  76.00   1.00    7.84    --  108.00 -30.00  90.00   37
  6  \w     90.00 129.00   1.00    7.84    --  108.00 -30.00  90.00   39
  7  \w     88.00 140.00   1.00    7.84    --  108.00  77.00 120.00   52
  8  \w    151.00 176.00   1.00    7.84    --  108.00  77.00 120.00   25
  9  \w     91.00 177.00   1.00    7.84    --  108.00  30.00 -90.00   86
 10  \w    142.00 168.00   1.00    7.84    --  108.00  30.00-150.00   26
 11  \w     91.00 120.00   1.00    7.84    --  108.00  30.00-150.00   29
 12  \w     71.00 115.00   1.00    7.84    --  108.00 -30.00-180.00   44
 13  \w     84.00 128.00   1.00    7.84    --  108.00 -77.00 -90.00   44
 14  \w     48.00  74.00   1.00    1.96    --   35.23 -99.00 -90.00   26
 15  \w     41.00 121.00   1.00    7.84    --  108.00 -61.00-150.00   80
 16  \w     41.00 116.00   1.00    7.84    --  108.00-111.00  60.00   75
 17  \w   -102.00 -14.00   1.00    1.96    --  -33.50 -37.00  60.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  Rigaku-OxfordDiffracti0on
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1174542000
_diffrn_orient_matrix_UB_12      0.0126815000
_diffrn_orient_matrix_UB_13      0.0429049000
_diffrn_orient_matrix_UB_21      0.0077167000
_diffrn_orient_matrix_UB_22      -0.0022624000
_diffrn_orient_matrix_UB_23      -0.1064424000
_diffrn_orient_matrix_UB_31      -0.0137374000
_diffrn_orient_matrix_UB_32      0.1074897000
_diffrn_orient_matrix_UB_33      -0.0073401000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10315
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.377
_diffrn_reflns_theta_min         4.533
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27181
_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            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       needle
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.452
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0830P)^2^+0.9612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4113
_reflns_number_total             4977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01459d2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7058549--7058555.cif.'
_cod_original_cell_volume        2613.55(16)
_cod_database_code               7058550
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C10 H11 N4 S Br Cu'
_chemical_oxdiff_usercomment     'Lobana's JPL-249'
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.234
_reflns_odcompleteness_completeness 99.78
_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:
 C8A(H8AA,H8AB), C8B(H8BA,H8BB)
2.b Aromatic/amide H refined with riding coordinates:
 N4A(H4A), C4A(H4AA), C5A(H5A), C6A(H6A), C7A(H7A), N4B(H4B), C4B(H4BA),
 C5B(H5B), C6B(H6B), C7B(H7B)
2.c Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C9B(H9BA,H9BB,H9BC), C10B(H10D,
 H10E,H10F)
;
_shelx_res_checksum              30816
_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 3.420
_oxdiff_exptl_absorpt_empirical_full_min 0.648