Synthesis, characterization and antimicrobial activities of Co(III) and Ni(II) complexes with 5-methyl-3-formylpyrazole-N(4)-dihexylthiosemicarbazone (HMPzNHex2): X-ray crystallography and DFT calculations of [Co(MPzNHex2)2]ClO4·1.5H2O (I) and [Ni(HMPzNHex2)2]Cl2·2H2O (II)
Saha, Manan; Biswas, Jayanta Kumar; Mondal, Monojit; Ghosh, Debarati; Mandal, Susmita; Cordes, David B.; Slawin, Alexandra M.Z.; Mandal, Tarun Kanti; Saha, Nitis Chandra; Inorganica Chimica Acta 483 (2018) 271–283; doi:10.1016/j.ica.2018.08.024

data_1563848
_publ_section_title
;
 Synthesis, characterization and antimicrobial activities of Co(III) and
 Ni(II) complexes with
 5-methyl-3-formylpyrazole-N(4)-dihexylthiosemicarbazone (HMPzNHex2):
 X-ray crystallography and DFT calculations of
 [Co(MPzNHex2)2]ClO4&#x00B7;1.5H2O (I) and [Ni(HMPzNHex2)2]Cl2&#x00B7;2H2O
 (II)
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              271
_journal_page_last               283
_journal_paper_doi               10.1016/j.ica.2018.08.024
_journal_volume                  483
_journal_year                    2018
_chemical_formula_moiety         'C36 H66 N10 Ni S2, 2(H2 O), 2(Cl)'
_chemical_formula_sum            'C36 H70 Cl2 N10 Ni O2 S2'
_chemical_formula_weight         868.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                77.16(2)
_cell_angle_beta                 74.464(19)
_cell_angle_gamma                86.80(2)
_cell_formula_units_Z            2
_cell_length_a                   10.867(4)
_cell_length_b                   13.428(5)
_cell_length_c                   17.055(5)
_cell_measurement_reflns_used    4164
_cell_measurement_temperature    125
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      1.90
_cell_volume                     2337.8(14)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2002
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30168
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.429
_diffrn_reflns_theta_min         1.945
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             932.00
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.53
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8492
_refine_ls_number_restraints     423
_refine_ls_R_factor_all          0.2851
_refine_ls_R_factor_gt           0.1707
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1641P)^2^+30.4522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4093
_refine_ls_wR_factor_ref         0.4666
_reflns_number_gt                3783
_reflns_number_total             8492
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            II.cif
_cod_data_source_block           II
_cod_database_code               1563848
_shelx_res_checksum              26635
_shelx_hkl_checksum              8984