Nickel(II) and copper(II) complexes constructed with N2S2 hybrid benzamidine-thiosemicarbazone ligand: Synthesis, X-ray crystal structure, DFT, kinetico-catalytic and in vitro biological applications
Paranthaman, Vijayan; Viswanathamurthi, Periasamy; Krishnaswamy, Velmurugan; Raju, Nandhakumar; Manickam Dakshinamoorthi, Bala Kumaran; PT, kalaichelvan; Malecki, Jan; RSC Adv.  (2015) –; doi:10.1039/C5RA18568H

data_7223318
_publ_section_title
;
 Nickel(II) and copper(II) complexes constructed with N2S2 hybrid
 benzamidine-thiosemicarbazone ligand: Synthesis, X-ray crystal structure,
 DFT, kinetico-catalytic and in vitro biological applications
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA18568H
_journal_year                    2015
_chemical_formula_moiety         'C22 H26 Cu N6 S2'
_chemical_formula_sum            'C22 H26 Cu N6 S2'
_chemical_formula_weight         502.15
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-14 deposited with the CCDC.
2015-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3637(4)
_cell_length_b                   17.6802(7)
_cell_length_c                   19.9696(6)
_cell_measurement_reflns_used    4768
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.6960
_cell_measurement_theta_min      4.2850
_cell_volume                     4718.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -11.00   84.00   1.0000   19.7600
omega____ theta____ kappa____ phi______ frames
    -       10.3715   38.0000  120.0000 95

  2 omega  -40.00   -1.00   1.0000   19.7600
omega____ theta____ kappa____ phi______ frames
    -      -11.3090  -19.0000  -60.0000 39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0468983000
_diffrn_orient_matrix_UB_12      -0.0132987000
_diffrn_orient_matrix_UB_13      0.0117668000
_diffrn_orient_matrix_UB_21      0.0175987000
_diffrn_orient_matrix_UB_22      0.0377716000
_diffrn_orient_matrix_UB_23      0.0020682000
_diffrn_orient_matrix_UB_31      -0.0175415000
_diffrn_orient_matrix_UB_32      0.0023416000
_diffrn_orient_matrix_UB_33      0.0334566000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_laue_measured_fraction_full 0.975
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13366
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_min         3.608
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0460P)^2^+1.8410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3346
_reflns_number_total             4158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra18568h2.cif
_cod_data_source_block           cul1
_cod_database_code               7223318
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Cu1 S2 N6 C23 H27'
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C19(H19A,H19B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), C4(H4), C5(H5), C6(H6A), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
  C14(H14)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              48121
_olex2_submission_special_instructions 'No special instructions were received'