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_7041581
_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         'C12 H24 Cl Cu N4 S2'
_chemical_formula_sum            'C12 H24 Cl Cu N4 S2'
_chemical_formula_weight         387.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-29 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.984(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0097(4)
_cell_length_b                   14.0814(3)
_cell_length_c                   18.9263(6)
_cell_measurement_reflns_used    6891
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.4910
_cell_measurement_theta_min      3.4430
_cell_volume                     3530.63(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      173(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 0.907
_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    -33.00  -6.00   1.00   10.00    --  -23.80 -77.00 -60.00   27
  2  \w     23.00  65.00   1.00   10.00    --   25.99 -99.00 -60.00   42
  3  \w    -22.00   4.00   1.00   10.00    --   25.99 -99.00 -60.00   26
  4  \w    -49.00   3.00   1.00   10.00    --  -23.80 -19.00-180.00   52
  5  \w     29.00  89.00   1.00   10.00    --   25.99  57.00 150.00   60
  6  \w     -1.00  74.00   1.00   10.00    --   25.99  77.00  60.00   75
  7  \w     35.00  79.00   1.00   10.00    --   25.99 178.00 -90.00   44
;
_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      -0.0007980000
_diffrn_orient_matrix_UB_12      -0.0470870000
_diffrn_orient_matrix_UB_13      0.0131146000
_diffrn_orient_matrix_UB_21      0.0049900000
_diffrn_orient_matrix_UB_22      0.0177724000
_diffrn_orient_matrix_UB_23      0.0361327000
_diffrn_orient_matrix_UB_31      -0.0532504000
_diffrn_orient_matrix_UB_32      0.0023276000
_diffrn_orient_matrix_UB_33      -0.0097720000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29554
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.761
_diffrn_reflns_theta_min         3.109
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.621
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.458
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         11848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0420P)^2^+1.8716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8285
_reflns_number_total             11848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04103e2.cif
_cod_data_source_block           jpl-201
_cod_depositor_comments
'Adding full bibliography for 7041581--7041593.cif.'
_cod_original_cell_volume        3530.66(18)
_cod_database_code               7041581
_chemical_oxdiff_formula         'C44 H44 N4 S2 Cu'
_chemical_oxdiff_usercomment     'Lobana's JPL-201'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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:
 C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C8A(H8AA,
 H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C11A(H11A,H11B), C2B(H2BA,H2BB),
 C3B(H3BA,H3BB), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C8B(H8BA,H8BB), C9B(H9BA,H9BB),
  C10B(H10C,H10D), C11B(H11C,H11D)
2.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N3A(H3A), N1B(H1B), N3B(H3B)
2.c Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C12A(H12A,H12B,H12C), C6B(H6BA,H6BB,H6BC), C12B(H12D,
 H12E,H12F)
;
_shelx_res_checksum              5930
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'nylon loop'
_olex2_submission_original_sample_id JPL-201
_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 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.761