Synthesis, structures, antimicrobial activity and biosafety evaluation of pyridine-2-formaldehyde-N-susbtituted-thiosemicarbazonates of copper(ii)
Kaushal, Mani; Lobana, Tarlok S.; Nim, Lovedeep; Kaur, Jaskamal; Bala, Ritu; Hundal, Geeta; Arora, Daljit S.; Garcia-Santos, Isabel; Duff, Courtney E.; Jasinski, Jerry P.; New Journal of Chemistry 42 (2018) 15879–; doi:10.1039/C8NJ03619E

data_7057665
_publ_section_title
;
 Synthesis, structures, antimicrobial activity and biosafety evaluation of
 pyridine-2-formaldehyde-N-susbtituted-thiosemicarbazonates of copper(ii)
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15879
_journal_paper_doi               10.1039/C8NJ03619E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C9 H11 Cl Cu N4 S, C2 H3 N'
_chemical_formula_sum            'C11 H14 Cl Cu N5 S'
_chemical_formula_weight         347.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-11-29 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                96.619(6)
_cell_angle_beta                 98.510(6)
_cell_angle_gamma                102.123(7)
_cell_formula_units_Z            2
_cell_length_a                   8.5331(7)
_cell_length_b                   9.4698(7)
_cell_length_c                   9.5110(7)
_cell_measurement_reflns_used    1957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.2950
_cell_measurement_theta_min      5.3530
_cell_volume                     734.58(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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 16.0416
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.974
_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     23.00  83.00   1.00    1.00    --   35.17  57.00 -30.00   60
  2  \w     40.00 112.00   1.00    1.02    --  108.00 -45.00  30.00   72
  3  \w    101.00 127.00   1.00    1.02    --  108.00 -30.00  30.00   26
  4  \w     93.00 176.00   1.00    1.02    --  108.00  45.00 120.00   83
  5  \w    115.00 177.00   1.00    1.02    --  108.00 111.00 150.00   62
  6  \w    101.00 176.00   1.00    1.02    --  108.00 111.00  60.00   75
  7  \w     92.00 162.00   1.00    1.02    --  108.00  45.00  60.00   70
  8  \w     88.00 116.00   1.00    1.02    --  108.00 -30.00-120.00   28
  9  \w     72.00  97.00   1.00    1.02    --  108.00 -94.00-120.00   25
 10  \w     76.00 109.00   1.00    1.02    --  108.00 -94.00-180.00   33
 11  \w     60.00  85.00   1.00    1.02    --  108.00 -30.00-120.00   25
 12  \w     87.00 158.00   1.00    1.02    --  108.00  30.00-150.00   71
 13  \w    118.00 143.00   1.00    1.02    --  108.00 111.00-150.00   25
 14  \w     74.00 105.00   1.00    1.00    --   35.17 178.00-180.00   31
 15  \w    -41.00  32.00   1.00    1.00    --  -33.50  77.00 150.00   73
 16  \w    -96.00 -22.00   1.00    1.00    --  -33.50 -57.00   0.00   74
 17  \w     30.00  74.00   1.00    1.00    --   35.17 -99.00  30.00   44
 18  \w     65.00 116.00   1.00    1.02    --  108.00-111.00  90.00   51
 19  \w     61.00  91.00   1.00    1.02    --  108.00 -94.00 120.00   30
 20  \w     45.00 123.00   1.00    1.02    --  108.00 -45.00 150.00   78
 21  \w     41.00  70.00   1.00    1.02    --  108.00 -94.00   0.00   29
 22  \w     80.00 112.00   1.00    1.02    --  108.00-111.00 -30.00   32
 23  \w     37.00  62.00   1.00    1.00    --   35.17 -99.00-180.00   25
 24  \w      0.00  25.00   1.00    1.00    --   35.17 -57.00-180.00   25
 25  \w    -98.00  -9.00   1.00    1.00    --  -33.50 -77.00-120.00   89
 26  \w     44.00  80.00   1.00    1.02    --  108.00 -77.00 150.00   36
 27  \w   -100.00 -49.00   1.00    1.00    --  -33.50 -57.00  90.00   51
;
_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      -0.1544120000
_diffrn_orient_matrix_UB_12      0.0561890000
_diffrn_orient_matrix_UB_13      -0.0433210000
_diffrn_orient_matrix_UB_21      0.0985667000
_diffrn_orient_matrix_UB_22      0.1584281000
_diffrn_orient_matrix_UB_23      0.0505292000
_diffrn_orient_matrix_UB_31      0.0405820000
_diffrn_orient_matrix_UB_32      0.0088958000
_diffrn_orient_matrix_UB_33      -0.1517335000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4611
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.373
_diffrn_reflns_theta_min         4.756
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03189
_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    1.570
_exptl_crystal_description       irregular
_exptl_crystal_F_000             354
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.100
_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     174
_refine_ls_number_reflns         2792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2373
_reflns_number_total             2792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03619e2.cif
_cod_data_source_block           jpl-231
_cod_depositor_comments
'Adding full bibliography for 7057663--7057667.cif.'
_cod_database_code               7057665
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C9 H11 N4 S Cl Cu'
_chemical_oxdiff_usercomment     'Lobana's JPL-231'
_reflns_odcompleteness_completeness 99.70
_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:
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C3(H3), C4(H4A), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              53189
_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 18.556
_oxdiff_exptl_absorpt_empirical_full_min 0.485