Metal derivatives of N1-substituted thiosemicarbazones: Synthesis, structures and spectroscopy of nickel(II) and cobalt(III) complexes
Tarlok S. Lobana; Poonam Kumari; Geeta Hundal; Ray J. Butcher; A. Castineiras; Takashiro Akitsu; Inorganica Chimica Acta 394 (2013) 605–615; doi:10.1016/j.ica.2012.09.021

data_1512806
_publ_section_title
;
 Metal derivatives of N1-substituted thiosemicarbazones: Synthesis,
 structures and spectroscopy of nickel(II) and cobalt(III) complexes
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              605
_journal_page_last               615
_journal_paper_doi               10.1016/j.ica.2012.09.021
_journal_volume                  394
_journal_year                    2013
_chemical_formula_moiety         'C21 H24 Co N9 S6, H2 O'
_chemical_formula_sum            'C21 H26 Co N9 O S6'
_chemical_formula_weight         671.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 114.963(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7381(12)
_cell_length_b                   29.112(3)
_cell_length_c                   9.9919(12)
_cell_measurement_reflns_used    7662
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.7005
_cell_measurement_theta_min      2.206
_cell_volume                     2831.7(6)
_computing_cell_refinement       'SMART Software (Bruker, 1997)'
_computing_data_collection       'SMART Software (Bruker, 1997)'
_computing_data_reduction        'SAINT Software (Bruker, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker CCD SMART1000 '
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33631
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.6900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+3.7547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                4865
_reflns_number_total             6068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-605-615-6.cif
_cod_data_source_block           9
_cod_original_cell_volume        2831.7(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512806