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_2242310
_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_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          '[Zn (N C S)2 (C6 H6 N2 S)2]'
_chemical_formula_moiety         'C14 H12 N6 S4 Zn'
_chemical_formula_sum            'C14 H12 N6 S4 Zn'
_chemical_formula_weight         457.91
_chemical_name_systematic
;
Bis(pyridine-4-thioamide-\k<i>N</i>)bis(thiocyanato-\k<i>N</i>)zinc(II)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.965(3)
_cell_length_b                   41.216(7)
_cell_length_c                   5.1117(7)
_cell_measurement_reflns_used    6296
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.997
_cell_measurement_theta_min      1.976
_cell_volume                     3995.6(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0873
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6296
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.976
_exptl_absorpt_coefficient_mu    1.657
_exptl_absorpt_correction_T_max  0.8935
_exptl_absorpt_correction_T_min  0.7885
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(<i>X-RED32</i> and <i>X-SHAPE</i>; Stoe, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.360
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 638 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.014(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1919
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+3.6629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                1711
_reflns_number_total             1919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5430sup1.cif
_cod_data_source_block           2
_cod_database_code               2242310
_cod_database_fobs_code          2242310
_shelx_hkl_checksum              46283
_shelx_res_checksum              80785
_shelxl_version_number           2.014