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_1512804
_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         'C36 H35 N3 Ni O P2 S'
_chemical_formula_sum            'C36 H35 N3 Ni O P2 S'
_chemical_formula_weight         678.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.801(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0067(14)
_cell_length_b                   10.2385(14)
_cell_length_c                   27.191(4)
_cell_measurement_reflns_used    1777
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.6191
_cell_measurement_theta_min      5.0434
_cell_volume                     3283.4(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'SHELXLTL (Sheldrick, 2008)'
_computing_publication_material  SHELXLTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.1100
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            30228
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.74
_diffrn_reflns_theta_min         5.05
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.457
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         11040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0781P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                5537
_reflns_number_total             11040
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2013-394-605-615-4.cif
_cod_data_source_block           7
_cod_database_code               1512804