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_7223317
_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 N6 Ni S2'
_chemical_formula_sum            'C22 H26 N6 Ni S2'
_chemical_formula_weight         497.32
_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             2015-07-09
_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                   13.2007(7)
_cell_length_b                   17.5298(9)
_cell_length_c                   20.1722(11)
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.2340
_cell_measurement_theta_min      4.1050
_cell_volume                     4668.0(4)
_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 0.979
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -4.00   47.00   1.0000   34.8800
omega____ theta____ kappa____ phi______ frames
    -       10.0590  -99.0000   60.0000 51

  2 omega   32.00   77.00   1.0000   34.8800
omega____ theta____ kappa____ phi______ frames
    -       10.0590   57.0000  -30.0000 45

  3 omega  -54.00   14.00   1.0000   34.8800
omega____ theta____ kappa____ phi______ frames
    -       10.0590  -77.0000 -120.0000 68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0471558000
_diffrn_orient_matrix_UB_12      -0.0059411000
_diffrn_orient_matrix_UB_13      -0.0160728000
_diffrn_orient_matrix_UB_21      0.0197314000
_diffrn_orient_matrix_UB_22      -0.0331607000
_diffrn_orient_matrix_UB_23      -0.0154622000
_diffrn_orient_matrix_UB_31      -0.0167039000
_diffrn_orient_matrix_UB_32      -0.0224136000
_diffrn_orient_matrix_UB_33      0.0271442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_laue_measured_fraction_full 0.979
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16086
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         3.445
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55541
_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    1.415
_exptl_crystal_description       plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0630P)^2^+0.2310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3247
_reflns_number_total             4122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra18568h2.cif
_cod_data_source_block           nil1
_cod_database_code               7223317
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Ni1 S2 N6 C22 H20'
_reflns_odcompleteness_completeness 99.57
_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:
 C2(H2A,H2B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              54685
_olex2_submission_special_instructions 'No special instructions were received'