Variable coordination and C-S bond cleavage activity of N-substituted imidazolidine-2-thiones towards copper: synthesis, spectroscopy, structures, ESI-mass and antimicrobial studies.
Aulakh, Jaspreet K.; Lobana, Tarlok S.; Sood, Henna; Arora, Daljit S.; Garcia-Santos, Isabel; Hundal, Geeta; Kaur, Manpreet; Smolenski, Victoria A.; Jasinski, Jerry P.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1324–1339; doi:10.1039/c6dt04103e

data_7041586
_publ_section_title
;
 Variable coordination and C-S bond cleavage activity of N-substituted
 imidazolidine-2-thiones towards copper: synthesis, spectroscopy,
 structures, ESI-mass and antimicrobial studies.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1324
_journal_page_last               1339
_journal_paper_doi               10.1039/c6dt04103e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C18 H20 Cl Cu N4 S2'
_chemical_formula_sum            'C18 H20 Cl Cu N4 S2'
_chemical_formula_weight         455.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_space_group_name_Hall  '-I 2yc'
_symmetry_space_group_name_H-M   'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-29 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.378(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5161(5)
_cell_length_b                   10.4367(5)
_cell_length_c                   28.1083(14)
_cell_measurement_reflns_used    3750
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.6670
_cell_measurement_theta_min      3.8550
_cell_volume                     3961.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_details
;
  1 omega   19.00   45.00   1.0000    3.6800
omega____ theta____ kappa____ phi______ frames
    -      -23.6487    0.0000  -30.0000 26

  2 omega  -27.00   29.00   1.0000    3.6800
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -57.0000   90.0000 56

  3 omega   15.00   62.00   1.0000    3.6800
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -99.0000   60.0000 47

  4 omega  -43.00  -11.00   1.0000    3.6800
omega____ theta____ kappa____ phi______ frames
    -      -23.6487   37.0000 -120.0000 32

  5 omega  -73.00   -7.00   1.0000    3.6800
omega____ theta____ kappa____ phi______ frames
    -      -23.6487  -57.0000 -150.0000 66

  6 omega   42.00   75.00   1.0000    3.6800
omega____ theta____ kappa____ phi______ frames
    -       25.9925  178.0000    0.0000 33

  7 omega   35.00   97.00   1.0000    3.6800
omega____ theta____ kappa____ phi______ frames
    -       25.9925  178.0000   60.0000 62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0353537000
_diffrn_orient_matrix_UB_12      -0.0502060000
_diffrn_orient_matrix_UB_13      -0.0004085000
_diffrn_orient_matrix_UB_21      -0.0371314000
_diffrn_orient_matrix_UB_22      -0.0423634000
_diffrn_orient_matrix_UB_23      -0.0091368000
_diffrn_orient_matrix_UB_31      0.0114777000
_diffrn_orient_matrix_UB_32      0.0173556000
_diffrn_orient_matrix_UB_33      -0.0235400000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            15929
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.910
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         6586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0487P)^2^+0.8870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4400
_reflns_number_total             6586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04103e2.cif
_cod_data_source_block           tsl-442
_cod_depositor_comments
'Adding full bibliography for 7041581--7041593.cif.'
_cod_database_code               7041586
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C18 H36 N4 S2 Cl Cu'
_chemical_oxdiff_usercomment     'Lobana's TSL-442'
_reflns_odcompleteness_completeness 99.75
_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
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              77438