Synthesis and crystal structure of diiso-thio-cyanato-tetra-kis-(4-methyl-pyridine <i>N</i>-oxide)cobalt(II) and diiso-thio-cyanato-tris-(4-methyl-pyridine <i>N</i>-oxide)cobalt(II) showing two different metal coordination polyhedra.
Näther, Christian; Jess, Inke; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 174–179; doi:10.1107/S2056989024000471

data_2312401
_publ_section_title
;
 Synthesis and crystal structure of
 diiso-thio-cyanato-tetra-kis-(4-methyl-pyridine <i>N</i>-oxide)cobalt(II)
 and diiso-thio-cyanato-tris-(4-methyl-pyridine <i>N</i>-oxide)cobalt(II)
 showing two different metal coordination polyhedra.
;
_journal_coeditor_code           HB8092
_journal_issue                   'Pt 2'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              174
_journal_page_last               179
_journal_paper_doi               10.1107/S2056989024000471
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Co (N C S)2 (C6 H7 N1 O1)4]'
_chemical_formula_moiety         'C26 H28 Co N6 O4 S2'
_chemical_formula_sum            'C26 H28 Co N6 O4 S2'
_chemical_formula_weight         611.59
_chemical_name_systematic
;
Tetrakis(4-methylpyridine
<i>N</i>-oxide-\k<i>O</i>)bis(thiocyanato-\k<i>N</i>)cobalt(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90.609(3)
_cell_angle_beta                 96.346(3)
_cell_angle_gamma                108.090(4)
_cell_formula_units_Z            1
_cell_length_a                   7.0709(3)
_cell_length_b                   9.6651(5)
_cell_length_c                   11.0401(4)
_cell_measurement_reflns_used    5312
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      78.3470
_cell_measurement_theta_min      4.0340
_cell_volume                     711.99(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015a)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015b)
;
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7433
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.921
_diffrn_reflns_theta_min         4.033
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             317
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.475
_refine_ls_extinction_coef       0.0030(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015a)
;
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0431P)^2^+0.3098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                2935
_reflns_number_total             2950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8092.cif
_cod_data_source_block           1
_cod_original_cell_volume        712.00(6)
_cod_database_code               2312401
_shelx_hkl_checksum              74237
_shelx_res_checksum              34040