#------------------------------------------------------------------------------
#$Date: 2024-03-05 22:26:20 +0200 (Tue, 05 Mar 2024) $
#$Revision: 290313 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/24/2312401.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_2312401
loop_
_publ_author_name
'Näther, Christian'
'Jess, Inke'
_publ_section_title
;
 Synthesis and crystal structure of
 diiso-thio-cyanato-tetra-kis-(4-methyl-pyridine N-oxide)cobalt(II)
 and diiso-thio-cyanato-tris-(4-methyl-pyridine N-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
N-oxide-κO)bis(thiocyanato-κN)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       '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  0.0171
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0431P)²+0.3098P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            hb8092.cif
_cod_data_source_block           1
_cod_original_cell_volume        712.00(6)
_cod_database_code               2312401
_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'
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 0.500000 0.000000 0.500000 0.01633(12) Uani d 1 . .
N N1 0.4838(2) -0.09719(16) 0.32743(12) 0.0207(3) Uani d 1 . .
C C1 0.4728(2) -0.17698(19) 0.24550(14) 0.0205(3) Uani d 1 . .
S S1 0.45856(6) -0.29171(5) 0.13159(4) 0.02849(13) Uani d 1 . .
O O11 0.29908(17) -0.18891(13) 0.55992(10) 0.0207(2) Uani d 1 . .
N N11 0.1767(2) -0.28091(15) 0.47249(12) 0.0177(3) Uani d 1 . .
C C11 0.2312(3) -0.39113(19) 0.42796(16) 0.0232(3) Uani d 1 . .
H H11 0.354482 -0.404151 0.460193 0.028 Uiso calc 1 . .
C C12 0.1101(3) -0.48501(19) 0.33621(16) 0.0252(4) Uani d 1 . .
H H12 0.149798 -0.562764 0.305869 0.030 Uiso calc 1 . .
C C13 -0.0708(3) -0.46695(19) 0.28735(15) 0.0231(3) Uani d 1 . .
C C14 -0.1231(2) -0.35312(19) 0.33727(15) 0.0216(3) Uani d 1 . .
H H14 -0.246404 -0.338563 0.307292 0.026 Uiso calc 1 . .
C C15 0.0012(2) -0.26130(18) 0.42952(15) 0.0193(3) Uani d 1 . .
H H15 -0.036625 -0.184181 0.462878 0.023 Uiso calc 1 . .
C C16 -0.2018(3) -0.5642(2) 0.18404(18) 0.0328(4) Uani d 1 . .
H H16A -0.130107 -0.552506 0.111847 0.049 Uiso calc 1 . .
H H16B -0.324611 -0.537857 0.165466 0.049 Uiso calc 1 . .
H H16C -0.236267 -0.665831 0.207245 0.049 Uiso calc 1 . .
O O21 0.24737(17) 0.07014(13) 0.44699(10) 0.0207(2) Uani d 1 . .
N N21 0.1883(2) 0.09747(15) 0.33301(12) 0.0186(3) Uani d 1 . .
C C21 -0.0100(2) 0.06152(18) 0.29449(15) 0.0202(3) Uani d 1 . .
H H21 -0.104965 0.014060 0.347311 0.024 Uiso calc 1 . .
C C22 -0.0750(2) 0.09351(19) 0.17864(15) 0.0217(3) Uani d 1 . .
H H22 -0.214644 0.067556 0.152642 0.026 Uiso calc 1 . .
C C23 0.0608(3) 0.16314(19) 0.09945(15) 0.0226(3) Uani d 1 . .
C C24 0.2635(3) 0.1974(2) 0.14277(16) 0.0258(4) Uani d 1 . .
H H24 0.360977 0.244184 0.091201 0.031 Uiso calc 1 . .
C C25 0.3255(2) 0.1652(2) 0.25860(16) 0.0236(4) Uani d 1 . .
H H25 0.464495 0.190292 0.286400 0.028 Uiso calc 1 . .
C C26 -0.0054(3) 0.2016(2) -0.02611(16) 0.0284(4) Uani d 1 . .
H H26A -0.131570 0.128174 -0.058861 0.043 Uiso calc 1 . .
H H26B 0.097434 0.204362 -0.079528 0.043 Uiso calc 1 . .
H H26C -0.025290 0.297392 -0.021875 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
N1 Co1 N1 . 2_656 180.00(8) n
N1 Co1 O11 2_656 2_656 92.39(5) y
N1 Co1 O11 . 2_656 87.61(5) y
N1 Co1 O11 2_656 . 87.61(5) ?
N1 Co1 O11 . . 92.39(5) ?
N1 Co1 O21 . 2_656 87.56(5) y
N1 Co1 O21 2_656 2_656 92.44(5) y
N1 Co1 O21 2_656 . 87.56(5) ?
N1 Co1 O21 . . 92.44(5) ?
O11 Co1 O11 . 2_656 180.00(5) n
O11 Co1 O21 2_656 2_656 87.15(5) y
O11 Co1 O21 . . 87.15(5) ?
O11 Co1 O21 2_656 . 92.85(5) y
O11 Co1 O21 . 2_656 92.85(5) ?
O21 Co1 O21 2_656 . 180.0 n
Co1 N1 C1 . . 165.56(14) y
N1 C1 S1 . . 178.94(16) ?
N11 O11 Co1 . . 115.97(9) ?
O11 N11 C11 . . 119.50(14) ?
O11 N11 C15 . . 119.60(14) ?
C11 N11 C15 . . 120.90(14) ?
N11 C11 H11 . . 119.7 ?
N11 C11 C12 . . 120.53(16) ?
C12 C11 H11 . . 119.7 ?
C11 C12 H12 . . 119.8 ?
C11 C12 C13 . . 120.48(16) ?
C13 C12 H12 . . 119.8 ?
C12 C13 C16 . . 121.54(17) ?
C14 C13 C12 . . 117.17(16) ?
C14 C13 C16 . . 121.28(16) ?
C13 C14 H14 . . 119.5 ?
C15 C14 C13 . . 120.93(16) ?
C15 C14 H14 . . 119.5 ?
N11 C15 C14 . . 119.97(15) ?
N11 C15 H15 . . 120.0 ?
C14 C15 H15 . . 120.0 ?
C13 C16 H16A . . 109.5 ?
C13 C16 H16B . . 109.5 ?
C13 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N21 O21 Co1 . . 125.03(9) ?
O21 N21 C21 . . 119.16(13) ?
O21 N21 C25 . . 120.30(13) ?
C21 N21 C25 . . 120.50(14) ?
N21 C21 H21 . . 119.9 ?
N21 C21 C22 . . 120.29(15) ?
C22 C21 H21 . . 119.9 ?
C21 C22 H22 . . 119.5 ?
C21 C22 C23 . . 121.07(15) ?
C23 C22 H22 . . 119.5 ?
C22 C23 C24 . . 116.66(15) ?
C22 C23 C26 . . 122.24(16) ?
C24 C23 C26 . . 121.09(16) ?
C23 C24 H24 . . 119.3 ?
C25 C24 C23 . . 121.49(16) ?
C25 C24 H24 . . 119.3 ?
N21 C25 C24 . . 119.99(15) ?
N21 C25 H25 . . 120.0 ?
C24 C25 H25 . . 120.0 ?
C23 C26 H26A . . 109.5 ?
C23 C26 H26B . . 109.5 ?
C23 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 . 2.0910(14) y
Co1 N1 2_656 2.0910(14) ?
Co1 O11 . 2.1005(12) y
Co1 O11 2_656 2.1005(12) ?
Co1 O21 2_656 2.1266(11) ?
Co1 O21 . 2.1266(11) y
N1 C1 . 1.163(2) ?
C1 S1 . 1.6414(18) ?
O11 N11 . 1.3381(17) ?
N11 C11 . 1.346(2) ?
N11 C15 . 1.348(2) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.374(3) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.394(3) ?
C13 C14 . 1.392(3) ?
C13 C16 . 1.498(2) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.377(2) ?
C15 H15 . 0.9500 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
O21 N21 . 1.3369(17) ?
N21 C21 . 1.352(2) ?
N21 C25 . 1.356(2) ?
C21 H21 . 0.9500 ?
C21 C22 . 1.382(2) ?
C22 H22 . 0.9500 ?
C22 C23 . 1.391(2) ?
C23 C24 . 1.393(2) ?
C23 C26 . 1.501(2) ?
C24 H24 . 0.9500 ?
C24 C25 . 1.376(2) ?
C25 H25 . 0.9500 ?
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_455 0.95 2.83 3.7271(17) 157
C15 H15 O21 2_556 0.95 2.40 3.295(2) 157
C21 H21 O21 2_556 0.95 2.62 3.520(2) 158
C24 H24 S1 2_655 0.95 2.87 3.7591(18) 156
C25 H25 O11 2_656 0.95 2.25 3.090(2) 147
