#------------------------------------------------------------------------------
#$Date: 2024-04-16 05:12:08 +0300 (Tue, 16 Apr 2024) $
#$Revision: 291226 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/30/2023083.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_2023083
loop_
_publ_author_name
'Näther, Christian'
'Jess, Inke'
_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
N-oxide-κO)bis(thiocyanato-κN)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
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/4 (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       '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  0.0355
_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 x determined using 1732 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  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/[σ²(Fo²)+(0.0636P)²+1.9394P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            jp2003.cif
_cod_data_source_block           I
_cod_database_code               2023083
_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.
;
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 0.63119(5) 0.86737(2) 0.79970(6) 0.01961(14) Uani d 1 . .
N N1 0.4719(3) 0.83113(11) 0.7698(4) 0.0235(6) Uani d 1 . .
C C1 0.3811(3) 0.82456(12) 0.7982(5) 0.0227(7) Uani d 1 . .
S S1 0.25390(8) 0.81632(4) 0.84239(13) 0.0304(2) Uani d 1 . .
N N2 0.7907(3) 0.90130(11) 0.8467(4) 0.0243(6) Uani d 1 . .
C C2 0.8812(3) 0.92031(13) 0.8804(5) 0.0233(7) Uani d 1 . .
S S2 1.00934(8) 0.94704(4) 0.92598(13) 0.0313(2) Uani d 1 . .
O O11 0.6887(2) 0.81252(9) 0.6570(4) 0.0277(6) Uani d 1 . .
N N11 0.6138(3) 0.77822(11) 0.5616(5) 0.0250(6) Uani d 1 . .
C C11 0.6035(3) 0.73262(14) 0.6406(6) 0.0260(7) Uani d 1 . .
C C12 0.5254(3) 0.69782(14) 0.5330(6) 0.0269(7) Uani d 1 . .
H H12 0.518236 0.665128 0.584075 0.032 Uiso calc 1 . .
C C13 0.4589(3) 0.71024(15) 0.3547(6) 0.0288(8) Uani d 1 . .
H H13 0.404785 0.686632 0.283627 0.035 Uiso calc 1 . .
C C14 0.4715(3) 0.75755(15) 0.2791(6) 0.0292(8) Uani d 1 . .
H H14 0.425779 0.766777 0.155868 0.035 Uiso calc 1 . .
C C15 0.5502(4) 0.79080(14) 0.3837(6) 0.0284(8) Uani d 1 . .
H H15 0.560585 0.823010 0.331396 0.034 Uiso calc 1 . .
O O21 0.5544(2) 0.92584(9) 0.6365(4) 0.0268(5) Uani d 1 . .
N N21 0.4395(3) 0.92595(11) 0.5586(4) 0.0237(6) Uani d 1 . .
C C21 0.3663(3) 0.94142(13) 0.6653(5) 0.0264(8) Uani d 1 . .
C C22 0.2489(4) 0.94383(14) 0.5780(6) 0.0292(8) Uani d 1 . .
H H22 0.196291 0.954631 0.649971 0.035 Uiso calc 1 . .
C C23 0.2074(4) 0.93070(15) 0.3871(6) 0.0323(8) Uani d 1 . .
H H23 0.126916 0.932915 0.327424 0.039 Uiso calc 1 . .
C C24 0.2845(4) 0.91433(15) 0.2842(6) 0.0308(8) Uani d 1 . .
H H24 0.257430 0.904713 0.153547 0.037 Uiso calc 1 . .
C C25 0.4001(4) 0.91215(14) 0.3729(6) 0.0284(8) Uani d 1 . .
H H25 0.453469 0.900781 0.303152 0.034 Uiso calc 1 . .
O O31 0.6345(2) 0.86796(9) 1.0842(4) 0.0246(5) Uani d 1 . .
N N31 0.7388(3) 0.87132(12) 1.2112(5) 0.0268(7) Uani d 1 . .
C C31 0.7804(4) 0.91637(15) 1.2867(6) 0.0302(8) Uani d 1 . .
C C32 0.8873(4) 0.91678(17) 1.4195(6) 0.0335(9) Uani d 1 . .
H H32 0.918314 0.948072 1.474374 0.040 Uiso calc 1 . .
C C33 0.9489(4) 0.87328(17) 1.4731(6) 0.0342(9) Uani d 1 . .
H H33 1.021778 0.874207 1.564265 0.041 Uiso calc 1 . .
C C34 0.9030(4) 0.82742(16) 1.3916(6) 0.0331(9) Uani d 1 . .
H H34 0.944526 0.796754 1.427124 0.040 Uiso calc 1 . .
C C35 0.7986(4) 0.82690(15) 1.2613(6) 0.0297(8) Uani d 1 . .
H H35 0.767106 0.795842 1.204877 0.036 Uiso calc 1 . .
C C36 0.7088(4) 0.96175(16) 1.2225(7) 0.0365(9) Uani d 1 . .
H H36A 0.637607 0.959791 1.267447 0.055 Uiso calc 1 . .
H H36B 0.688837 0.963430 1.082058 0.055 Uiso calc 1 . .
H H36C 0.752416 0.992135 1.275386 0.055 Uiso calc 1 . .
C C16 0.6740(4) 0.72348(16) 0.8382(6) 0.0325(8) Uani d 1 . .
H H16A 0.648259 0.746150 0.927280 0.049 Uiso calc 1 . .
H H16B 0.755859 0.730027 0.843848 0.049 Uiso calc 1 . .
H H16C 0.664650 0.688212 0.874079 0.049 Uiso calc 1 . .
C C26 0.4185(4) 0.95516(14) 0.8691(6) 0.0289(8) Uani d 1 . .
H H26A 0.480012 0.980250 0.875055 0.043 Uiso calc 1 . .
H H26B 0.451361 0.924805 0.940647 0.043 Uiso calc 1 . .
H H26C 0.358631 0.969462 0.925716 0.043 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'
S S 0.3331 0.5567 '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 . . 176.35(13) y
O11 Co1 N1 . . 91.87(12) y
O11 Co1 N2 . . 88.87(12) y
O11 Co1 O21 . . 114.88(12) y
O11 Co1 O31 . . 126.83(11) y
O21 Co1 N1 . . 91.23(11) y
O21 Co1 N2 . . 91.70(12) y
O21 Co1 O31 . . 118.20(11) y
O31 Co1 N1 . . 84.17(12) y
O31 Co1 N2 . . 92.52(12) y
C1 N1 Co1 . . 155.7(3) y
N1 C1 S1 . . 178.6(3) ?
C2 N2 Co1 . . 177.5(3) ?
N2 C2 S2 . . 179.4(4) ?
N11 O11 Co1 . . 119.1(2) ?
O11 N11 C11 . . 120.5(3) ?
O11 N11 C15 . . 117.7(3) ?
C11 N11 C15 . . 121.8(3) ?
N11 C11 C12 . . 118.1(3) ?
N11 C11 C16 . . 117.4(3) ?
C12 C11 C16 . . 124.5(4) ?
C11 C12 H12 . . 119.6 ?
C13 C12 C11 . . 120.8(4) ?
C13 C12 H12 . . 119.6 ?
C12 C13 H13 . . 120.3 ?
C12 C13 C14 . . 119.4(4) ?
C14 C13 H13 . . 120.3 ?
C13 C14 H14 . . 120.4 ?
C15 C14 C13 . . 119.3(4) ?
C15 C14 H14 . . 120.4 ?
N11 C15 C14 . . 120.6(3) ?
N11 C15 H15 . . 119.7 ?
C14 C15 H15 . . 119.7 ?
N21 O21 Co1 . . 120.8(2) ?
O21 N21 C21 . . 119.6(3) ?
O21 N21 C25 . . 118.7(3) ?
C25 N21 C21 . . 121.7(3) ?
N21 C21 C22 . . 118.3(3) ?
N21 C21 C26 . . 117.4(3) ?
C22 C21 C26 . . 124.4(4) ?
C21 C22 H22 . . 119.6 ?
C23 C22 C21 . . 120.8(4) ?
C23 C22 H22 . . 119.6 ?
C22 C23 H23 . . 120.4 ?
C24 C23 C22 . . 119.2(4) ?
C24 C23 H23 . . 120.4 ?
C23 C24 H24 . . 120.4 ?
C25 C24 C23 . . 119.2(4) ?
C25 C24 H24 . . 120.4 ?
N21 C25 C24 . . 120.8(4) ?
N21 C25 H25 . . 119.6 ?
C24 C25 H25 . . 119.6 ?
N31 O31 Co1 . . 117.8(2) ?
O31 N31 C35 . . 116.9(3) ?
C31 N31 O31 . . 121.0(3) ?
C31 N31 C35 . . 122.2(4) ?
N31 C31 C32 . . 117.8(4) ?
N31 C31 C36 . . 117.6(4) ?
C32 C31 C36 . . 124.6(4) ?
C31 C32 H32 . . 119.2 ?
C33 C32 C31 . . 121.6(4) ?
C33 C32 H32 . . 119.2 ?
C32 C33 H33 . . 120.5 ?
C32 C33 C34 . . 118.9(4) ?
C34 C33 H33 . . 120.5 ?
C33 C34 H34 . . 120.2 ?
C35 C34 C33 . . 119.6(4) ?
C35 C34 H34 . . 120.2 ?
N31 C35 H35 . . 120.0 ?
C34 C35 N31 . . 119.9(4) ?
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 . 2.086(3) y
Co1 N2 . 2.051(3) y
Co1 O11 . 1.992(3) y
Co1 O21 . 2.016(2) y
Co1 O31 . 2.037(3) y
N1 C1 . 1.162(5) ?
C1 S1 . 1.637(4) ?
N2 C2 . 1.158(5) ?
C2 S2 . 1.639(4) ?
O11 N11 . 1.335(4) ?
N11 C11 . 1.350(5) ?
N11 C15 . 1.358(5) ?
C11 C12 . 1.397(5) ?
C11 C16 . 1.481(5) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.370(6) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.385(6) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.367(6) ?
C15 H15 . 0.9500 ?
O21 N21 . 1.344(4) ?
N21 C21 . 1.358(5) ?
N21 C25 . 1.352(5) ?
C21 C22 . 1.384(6) ?
C21 C26 . 1.489(5) ?
C22 H22 . 0.9500 ?
C22 C23 . 1.384(6) ?
C23 H23 . 0.9500 ?
C23 C24 . 1.382(7) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.368(6) ?
C25 H25 . 0.9500 ?
O31 N31 . 1.351(4) ?
N31 C31 . 1.350(5) ?
N31 C35 . 1.373(5) ?
C31 C32 . 1.390(6) ?
C31 C36 . 1.477(6) ?
C32 H32 . 0.9500 ?
C32 C33 . 1.366(7) ?
C33 H33 . 0.9500 ?
C33 C34 . 1.396(6) ?
C34 H34 . 0.9500 ?
C34 C35 . 1.359(6) ?
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 S1 1_554 0.95 2.95 3.868(4) 162.9
C15 H15 O31 1_554 0.95 2.47 3.296(5) 144.9
C32 H32 S2 2_575 0.95 3.02 3.873(4) 149.5
C26 H26B O31 . 0.98 2.64 3.512(5) 148.7
