Crystal structures of tetrakis(pyridine-4-thioamide-κ<i>N</i>)bis(thiocyanato-κ<i>N</i>)cobalt(II) monohydrate and bis(pyridine-4-thioamide-κ<i>N</i>)bis(thiocyanato-κ<i>N</i>)zinc(II)
Neumann, Tristan; Jess, Inke; Näther, Christian; Acta Crystallographica Section E 74 (2018) 141–146; doi:10.1107/S205698901800021X

data_2242309
_publ_section_title
;
 Crystal structures of
 tetrakis(pyridine-4-thioamide-\k<i>N</i>)bis(thiocyanato-\k<i>N</i>)cobalt(II)
 monohydrate and
 bis(pyridine-4-thioamide-\k<i>N</i>)bis(thiocyanato-\k<i>N</i>)zinc(II)
;
_journal_coeditor_code           WM5430
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              141
_journal_page_last               146
_journal_paper_doi               10.1107/S205698901800021X
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Co (N C S)2 (C6 H6 N2 S)4], H2 O'
_chemical_formula_moiety         'C26 H24 Co N10 S6, H2 O'
_chemical_formula_sum            'C26 H26 Co N10 O S6'
_chemical_formula_weight         745.89
_chemical_name_systematic
;
Tetrakis(pyridine-4-thioamide-\k<i>N</i>)bis(thiocyanato-\k<i>N</i>)cobalt(II)
monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 100.763(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9256(2)
_cell_length_b                   12.9595(6)
_cell_length_c                   24.1116(6)
_cell_measurement_reflns_used    7301
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      54.0
_cell_measurement_theta_min      3.1
_cell_volume                     3353.91(19)
_computing_cell_refinement
;
<i>X-AREA</i> (Stoe, 2008)
;
_computing_data_collection
;
<i>X-AREA</i> (Stoe, 2008)
;
_computing_data_reduction
;
<i>X-AREA</i> (Stoe, 2008)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1990)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.719
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.8864
_exptl_absorpt_correction_T_min  0.7873
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(<i>X-RED32</i> and <i>X-SHAPE</i>; Stoe, 2008)
;
_exptl_crystal_colour            'light red'
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+1.8302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                6291
_reflns_number_total             7301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5430sup1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C26 H26 Co1 N10 O1 S6'
_cod_database_code               2242309
_cod_database_fobs_code          2242309
_shelx_hkl_checksum              57365
_shelx_res_checksum              69365
_shelxl_version_number           2.014