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_7041583
_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         'C14 H28 Cu I N4 S2'
_chemical_formula_sum            'C14 H28 Cu I N4 S2'
_chemical_formula_weight         506.96
_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     direct
_audit_creation_date             2014-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-09-29 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                102.429(4)
_cell_angle_beta                 100.467(5)
_cell_angle_gamma                100.840(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4901(4)
_cell_length_b                   10.3906(4)
_cell_length_c                   14.1896(8)
_cell_measurement_reflns_used    3390
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.4260
_cell_measurement_theta_min      3.3920
_cell_volume                     1030.40(10)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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 0.992
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_details
;
  1 omega  -40.00   40.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -      -23.8050   57.0000   30.0000 80

  2 omega   11.00   43.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -      -23.8050   77.0000  -30.0000 32

  3 omega   -1.00   94.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -       25.9925   77.0000 -120.0000 95

  4 omega   41.00   68.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -       25.9925  178.0000  -60.0000 27

  5 omega  -39.00    3.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -      -23.8050  -77.0000   30.0000 42

  6 omega  -14.00   65.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -99.0000  -30.0000 79

  7 omega  -41.00   53.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -       25.9925  -77.0000  120.0000 94

  8 omega  -72.00  -47.00   1.0000    9.9550
omega____ theta____ kappa____ phi______ frames
    -      -23.8050  -77.0000   30.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Aglient, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0337988000
_diffrn_orient_matrix_UB_12      0.0694850000
_diffrn_orient_matrix_UB_13      0.0257840000
_diffrn_orient_matrix_UB_21      0.0851271000
_diffrn_orient_matrix_UB_22      0.0005214000
_diffrn_orient_matrix_UB_23      -0.0152891000
_diffrn_orient_matrix_UB_31      -0.0378775000
_diffrn_orient_matrix_UB_32      0.0186407000
_diffrn_orient_matrix_UB_33      -0.0432440000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12340
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.734
_diffrn_reflns_theta_min         3.190
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43213
_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    1.634
_exptl_crystal_description       plank
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         6759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0362P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4756
_reflns_number_total             6759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04103e2.cif
_cod_data_source_block           jpl-113
_cod_depositor_comments
'Adding full bibliography for 7041581--7041593.cif.'
_cod_original_cell_volume        1030.40(9)
_cod_database_code               7041583
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C14 H24 N4 S2 I Cu'
_chemical_oxdiff_usercomment     'Lobana's JPL-113'
_reflns_odcompleteness_completeness 99.87
_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:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              30636
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id JPL-113
_olex2_submission_special_instructions 'No special instructions were received'