#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:08:44 +0300 (Wed, 07 Aug 2024) $
#$Revision: 294011 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023157.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023157
loop_
_publ_author_name
'Näther, Christian'
'Jess, Inke'
_publ_section_title
;
 Syntheses and crystal structures of the five- and sixfold coordinated
 complexes diiso-seleno-cyanato-tris-(2-methyl-pyridine
 N-oxide)cobalt(II) and
 diiso-seleno-cyanato-tetra-kis-(2-methyl-pyridine
 N-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 N-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
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/4 (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       'ω 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 x determined using 2302 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  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/[σ²(Fo²)+(0.0682P)²+0.5399P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.267
_shelx_estimated_absorpt_t_max   0.691
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.63215(4) 0.86731(2) 0.79899(6) 0.01397(11) Uani d 1 . .
N N1 0.4748(2) 0.83139(10) 0.7711(4) 0.0180(5) Uani d 1 . .
C C1 0.3847(3) 0.82543(12) 0.7960(4) 0.0173(6) Uani d 1 . .
Se Se1 0.24577(3) 0.81838(2) 0.84143(4) 0.02001(9) Uani d 1 . .
N N2 0.7899(2) 0.90028(10) 0.8433(4) 0.0184(5) Uani d 1 . .
C C2 0.8794(3) 0.91870(12) 0.8762(4) 0.0172(6) Uani d 1 . .
Se Se2 1.01804(3) 0.94751(2) 0.92765(4) 0.02230(10) Uani d 1 . .
O O11 0.6860(2) 0.81331(8) 0.6514(4) 0.0209(5) Uani d 1 . .
N N11 0.6102(2) 0.77961(10) 0.5563(4) 0.0169(5) Uani d 1 . .
C C11 0.5986(3) 0.73433(12) 0.6337(4) 0.0173(6) Uani d 1 . .
C C12 0.5201(3) 0.70021(12) 0.5273(4) 0.0185(6) Uani d 1 . .
H H12 0.512002 0.667709 0.577882 0.022 Uiso calc 1 . .
C C13 0.4543(3) 0.71294(13) 0.3504(5) 0.0210(6) Uani d 1 . .
H H13 0.399759 0.689803 0.280355 0.025 Uiso calc 1 . .
C C14 0.4686(3) 0.76001(13) 0.2754(5) 0.0218(6) Uani d 1 . .
H H14 0.423837 0.769563 0.153540 0.026 Uiso calc 1 . .
C C15 0.5483(3) 0.79260(12) 0.3801(5) 0.0204(6) Uani d 1 . .
H H15 0.560187 0.824548 0.328556 0.024 Uiso calc 1 . .
O O21 0.55635(18) 0.92647(9) 0.6444(3) 0.0199(4) Uani d 1 . .
N N21 0.4429(2) 0.92698(10) 0.5685(4) 0.0178(5) Uani d 1 . .
C C21 0.3714(3) 0.94192(11) 0.6761(5) 0.0194(6) Uani d 1 . .
C C22 0.2550(3) 0.94443(12) 0.5905(5) 0.0220(6) Uani d 1 . .
H H22 0.203471 0.955060 0.662840 0.026 Uiso calc 1 . .
C C23 0.2133(3) 0.93161(15) 0.4009(5) 0.0247(7) Uani d 1 . .
H H23 0.133828 0.933923 0.342723 0.030 Uiso calc 1 . .
C C24 0.2889(3) 0.91531(13) 0.2967(5) 0.0236(7) Uani d 1 . .
H H24 0.261750 0.905660 0.167347 0.028 Uiso calc 1 . .
C C25 0.4040(3) 0.91336(12) 0.3842(5) 0.0219(6) Uani d 1 . .
H H25 0.456510 0.902355 0.314261 0.026 Uiso calc 1 . .
O O31 0.6368(2) 0.86742(9) 1.0809(3) 0.0189(4) Uani d 1 . .
N N31 0.7399(2) 0.87014(10) 1.2061(4) 0.0183(5) Uani d 1 . .
C C31 0.7818(3) 0.91535(13) 1.2802(4) 0.0204(6) Uani d 1 . .
C C32 0.8872(3) 0.91558(14) 1.4123(5) 0.0237(7) Uani d 1 . .
H H32 0.918537 0.946696 1.466300 0.028 Uiso calc 1 . .
C C33 0.9469(3) 0.87135(15) 1.4660(5) 0.0250(7) Uani d 1 . .
H H33 1.018835 0.871934 1.556260 0.030 Uiso calc 1 . .
C C34 0.9007(3) 0.82600(14) 1.3865(5) 0.0237(7) Uani d 1 . .
H H34 0.940708 0.795231 1.421995 0.028 Uiso calc 1 . .
C C35 0.7968(3) 0.82592(13) 1.2565(5) 0.0207(6) Uani d 1 . .
H H35 0.764512 0.795027 1.201666 0.025 Uiso calc 1 . .
C C36 0.7123(3) 0.96119(14) 1.2166(5) 0.0272(7) Uani d 1 . .
H H36A 0.641642 0.959482 1.259800 0.041 Uiso calc 1 . .
H H36B 0.693531 0.963154 1.077488 0.041 Uiso calc 1 . .
H H36C 0.755827 0.991225 1.270547 0.041 Uiso calc 1 . .
C C16 0.6698(3) 0.72386(14) 0.8287(5) 0.0254(7) Uani d 1 . .
H H16A 0.648341 0.747113 0.919137 0.038 Uiso calc 1 . .
H H16B 0.750650 0.728605 0.831326 0.038 Uiso calc 1 . .
H H16C 0.657240 0.688988 0.864016 0.038 Uiso calc 1 . .
C C26 0.4234(3) 0.95514(13) 0.8779(5) 0.0240(7) Uani d 1 . .
H H26A 0.481990 0.981121 0.883718 0.036 Uiso calc 1 . .
H H26B 0.458476 0.924982 0.946474 0.036 Uiso calc 1 . .
H H26C 0.364160 0.968028 0.936542 0.036 Uiso calc 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Co1 N1 . . 176.24(11) y
O11 Co1 N1 . . 91.77(10) y
O11 Co1 N2 . . 88.63(10) y
O11 Co1 O21 . . 115.08(11) y
O11 Co1 O31 . . 127.68(10) y
O21 Co1 N1 . . 91.29(10) y
O21 Co1 N2 . . 91.92(10) y
O21 Co1 O31 . . 117.13(10) y
O31 Co1 N1 . . 84.07(10) y
O31 Co1 N2 . . 92.72(10) y
C1 N1 Co1 . . 156.2(3) y
N1 C1 Se1 . . 177.6(3) ?
C2 N2 Co1 . . 177.2(2) y
N2 C2 Se2 . . 179.8(3) ?
N11 O11 Co1 . . 118.91(18) y
O11 N11 C11 . . 120.4(3) ?
O11 N11 C15 . . 117.6(3) ?
C11 N11 C15 . . 121.9(3) ?
N11 C11 C12 . . 118.2(3) ?
N11 C11 C16 . . 117.8(3) ?
C12 C11 C16 . . 124.0(3) ?
C11 C12 H12 . . 119.5 ?
C13 C12 C11 . . 121.0(3) ?
C13 C12 H12 . . 119.5 ?
C12 C13 H13 . . 120.4 ?
C12 C13 C14 . . 119.2(3) ?
C14 C13 H13 . . 120.4 ?
C13 C14 H14 . . 120.5 ?
C15 C14 C13 . . 119.0(3) ?
C15 C14 H14 . . 120.5 ?
N11 C15 C14 . . 120.7(3) ?
N11 C15 H15 . . 119.7 ?
C14 C15 H15 . . 119.7 ?
N21 O21 Co1 . . 120.92(18) y
O21 N21 C21 . . 119.7(3) ?
O21 N21 C25 . . 118.2(3) ?
C21 N21 C25 . . 122.1(3) ?
N21 C21 C22 . . 118.2(3) ?
N21 C21 C26 . . 117.5(3) ?
C22 C21 C26 . . 124.3(3) ?
C21 C22 H22 . . 119.6 ?
C23 C22 C21 . . 120.8(3) ?
C23 C22 H22 . . 119.6 ?
C22 C23 H23 . . 120.4 ?
C22 C23 C24 . . 119.3(3) ?
C24 C23 H23 . . 120.4 ?
C23 C24 H24 . . 120.5 ?
C25 C24 C23 . . 119.0(3) ?
C25 C24 H24 . . 120.5 ?
N21 C25 C24 . . 120.6(3) ?
N21 C25 H25 . . 119.7 ?
C24 C25 H25 . . 119.7 ?
N31 O31 Co1 . . 118.01(18) y
O31 N31 C31 . . 120.3(3) ?
O31 N31 C35 . . 117.1(3) ?
C31 N31 C35 . . 122.5(3) ?
N31 C31 C32 . . 117.7(3) ?
N31 C31 C36 . . 118.1(3) ?
C32 C31 C36 . . 124.2(3) ?
C31 C32 H32 . . 119.5 ?
C33 C32 C31 . . 121.1(3) ?
C33 C32 H32 . . 119.5 ?
C32 C33 H33 . . 120.4 ?
C32 C33 C34 . . 119.2(3) ?
C34 C33 H33 . . 120.4 ?
C33 C34 H34 . . 120.2 ?
C35 C34 C33 . . 119.6(3) ?
C35 C34 H34 . . 120.2 ?
N31 C35 C34 . . 119.9(3) ?
N31 C35 H35 . . 120.0 ?
C34 C35 H35 . . 120.0 ?
C31 C36 H36A . . 109.5 ?
C31 C36 H36B . . 109.5 ?
C31 C36 H36C . . 109.5 ?
H36A C36 H36B . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
C11 C16 H16A . . 109.5 ?
C11 C16 H16B . . 109.5 ?
C11 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C21 C26 H26A . . 109.5 ?
C21 C26 H26B . . 109.5 ?
C21 C26 H26C . . 109.5 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N1 . 2.090(3) y
Co1 N2 . 2.047(3) y
Co1 O11 . 1.989(2) y
Co1 O21 . 2.011(2) y
Co1 O31 . 2.032(2) y
N1 C1 . 1.157(4) ?
C1 Se1 . 1.797(3) ?
N2 C2 . 1.156(4) ?
C2 Se2 . 1.794(3) ?
O11 N11 . 1.341(3) ?
N11 C11 . 1.346(4) ?
N11 C15 . 1.357(4) ?
C11 C12 . 1.397(4) ?
C11 C16 . 1.490(4) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.374(5) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.387(5) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.374(5) ?
C15 H15 . 0.9500 ?
O21 N21 . 1.345(3) ?
N21 C21 . 1.358(4) ?
N21 C25 . 1.353(4) ?
C21 C22 . 1.392(5) ?
C21 C26 . 1.485(4) ?
C22 H22 . 0.9500 ?
C22 C23 . 1.385(5) ?
C23 H23 . 0.9500 ?
C23 C24 . 1.390(5) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.379(5) ?
C25 H25 . 0.9500 ?
O31 N31 . 1.350(4) ?
N31 C31 . 1.358(4) ?
N31 C35 . 1.361(4) ?
C31 C32 . 1.392(5) ?
C31 C36 . 1.483(5) ?
C32 H32 . 0.9500 ?
C32 C33 . 1.380(5) ?
C33 H33 . 0.9500 ?
C33 C34 . 1.388(5) ?
C34 H34 . 0.9500 ?
C34 C35 . 1.371(5) ?
C35 H35 . 0.9500 ?
C36 H36A . 0.9800 ?
C36 H36B . 0.9800 ?
C36 H36C . 0.9800 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
C26 H26A . 0.9800 ?
C26 H26B . 0.9800 ?
C26 H26C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C14 H14 Se1 1_554 0.95 3.00 3.920(3) 163
C15 H15 O31 1_554 0.95 2.49 3.305(4) 144
C32 H32 Se2 2_575 0.95 3.09 3.945(4) 151
C26 H26B O31 . 0.98 2.62 3.511(4) 151
