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_1563847
_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 H64 Co N10 S2, 1.5(H2 O), Cl O4'
_chemical_formula_sum            'C36 H67 Cl Co N10 O5.5 S2'
_chemical_formula_weight         886.50
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.335(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   41.887(6)
_cell_length_b                   9.0663(11)
_cell_length_c                   25.397(3)
_cell_measurement_reflns_used    10823
_cell_measurement_temperature    125
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.20
_cell_volume                     9301(2)
_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 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0779
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            60145
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         2.161
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3784.00
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8502
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0829P)^2^+20.1381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5655
_reflns_number_total             8502
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            I.cif
_cod_data_source_block           I
_cod_database_code               1563847
_shelx_res_checksum              21684
_shelx_hkl_checksum              13665