Syntheses and crystal structures of the five- and sixfold coordinated complexes diiso-seleno-cyanato-tris-(2-methyl-pyridine <i>N</i>-oxide)cobalt(II) and diiso-seleno-cyanato-tetra-kis-(2-methyl-pyridine <i>N</i>-oxide)cobalt(II).
Näther, Christian; Jess, Inke; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 704–708; doi:10.1107/S2056989024005073

data_2023157
_publ_section_title
;
 Syntheses and crystal structures of the five- and sixfold coordinated
 complexes diiso-seleno-cyanato-tris-(2-methyl-pyridine
 <i>N</i>-oxide)cobalt(II) and
 diiso-seleno-cyanato-tetra-kis-(2-methyl-pyridine
 <i>N</i>-oxide)cobalt(II).
;
_journal_coeditor_code           HB8098
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              704
_journal_page_last               708
_journal_paper_doi               10.1107/S2056989024005073
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Co (N C Se)2 (C6 H7 N1 O1)3]'
_chemical_formula_moiety         'C20 H21 Co N5 O3 Se2'
_chemical_formula_sum            'C20 H21 Co N5 O3 Se2'
_chemical_formula_weight         596.27
_chemical_name_systematic
;
Diisoselenocyanatotris(2-methylpyridine <i>N</i>-oxide)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
_cell_angle_alpha                90
_cell_angle_beta                 104.2765(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.07686(6)
_cell_length_b                   26.47661(16)
_cell_length_c                   7.25623(4)
_cell_measurement_reflns_used    35276
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.4900
_cell_measurement_theta_min      3.3190
_cell_volume                     2248.56(2)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.87a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.87a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.87a (Rigaku OD, 2023)
;
_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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            49619
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.434
_diffrn_reflns_theta_min         3.338
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.960
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPr; Rigaku OD, 2023)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       needle
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.402
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2302 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.0305(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4828
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0195
_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^)+(0.0682P)^2^+0.5399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                4788
_reflns_number_total             4828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8098.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2023156--2023157.cif.'
_cod_database_code               2023157
_shelx_estimated_absorpt_t_min   0.267
_shelx_estimated_absorpt_t_max   0.691
_shelx_hkl_checksum              83928
_shelx_res_checksum              40524