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_7041587
_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         'C8 H16 Cl Cu N4 S2'
_chemical_formula_sum            'C8 H16 Cl Cu N4 S2'
_chemical_formula_weight         331.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-03
_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                 105.936(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9744(16)
_cell_length_b                   7.6298(10)
_cell_length_c                   14.1661(16)
_cell_measurement_reflns_used    1311
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.8580
_cell_measurement_theta_min      4.6010
_cell_volume                     1348.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_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 0.994
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
  1 omega   10.00   94.00   1.0000    1.1350
omega____ theta____ kappa____ phi______ frames
    -       25.9925   37.0000  -30.0000 84

  2 omega    1.00   53.00   1.0000    1.1350
omega____ theta____ kappa____ phi______ frames
    -       25.9925   19.0000   90.0000 52

  3 omega  -24.00   18.00   1.0000    1.1350
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -99.0000 -120.0000 42

  4 omega   41.00   67.00   1.0000    1.1350
omega____ theta____ kappa____ phi______ frames
    -       25.9925 -178.0000 -150.0000 26

  5 omega  -43.00    9.00   1.0000    1.1350
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -37.0000  150.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0440118000
_diffrn_orient_matrix_UB_12      -0.0587657000
_diffrn_orient_matrix_UB_13      -0.0109301000
_diffrn_orient_matrix_UB_21      -0.0061994000
_diffrn_orient_matrix_UB_22      0.0123414000
_diffrn_orient_matrix_UB_23      -0.0508886000
_diffrn_orient_matrix_UB_31      0.0354826000
_diffrn_orient_matrix_UB_32      -0.0709622000
_diffrn_orient_matrix_UB_33      0.0004248000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4253
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.501
_diffrn_reflns_theta_min         3.130
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1824
_reflns_number_total             2223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04103e2.cif
_cod_data_source_block           jpl-131
_cod_depositor_comments
'Adding full bibliography for 7041581--7041593.cif.'
_cod_database_code               7041587
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C40 H38 N2 S P Cl Cu'
_chemical_oxdiff_usercomment     'Lobana's JPL-131'
_reflns_odcompleteness_completeness 99.82
_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:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              43111
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id 'JPL 131'
_olex2_submission_special_instructions 'No special instructions were received'