Synthesis, crystal structure and properties of the trigonal–bipyramidal complex tris(2-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II)
Näther, Christian; Jess, Inke; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024003050

data_2023083
_publ_section_title
;
 Synthesis, crystal structure and properties of the trigonal--bipyramidal
 complex tris(2-methylpyridine N-oxide-\kO)bis(thiocyanato-\kN)cobalt(II)
;
_journal_coeditor_code           JP2003
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024003050
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Co (N C S)2 (C6 H7 N O)3]'
_chemical_formula_moiety         'C20 H21 Co N5 O3 S2'
_chemical_formula_sum            'C20 H21 Co N5 O3 S2'
_chemical_formula_weight         502.47
_chemical_name_systematic
;
Tris(2-methylpyridine
<i>N</i>-oxide-\k<i>O</i>)bis(thiocyanato-\k<i>N</i>)cobalt(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.2990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9020(2)
_cell_length_b                   26.4007(2)
_cell_length_c                   7.19330(10)
_cell_measurement_reflns_used    17140
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.0130
_cell_measurement_theta_min      3.3500
_cell_volume                     2190.26(5)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999) and XP in SHELXTL-PC (Sheldrick,
2008)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/4</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24478
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.228
_diffrn_reflns_theta_min         3.348
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       needle
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.275
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1732 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4183
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+1.9394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                4137
_reflns_number_total             4183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp2003.cif
_cod_data_source_block           I
_cod_database_code               2023083
_shelx_hkl_checksum              40361
_shelx_res_checksum              19058