#------------------------------------------------------------------------------
#$Date: 2023-09-05 23:08:38 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286164 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/26/7062622.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7062622
loop_
_publ_author_name
'Lv, Wei'
'Chen, Lei'
'Chen, Xue-Tai'
'Yan, Hong'
'Wang, Zhenxing'
'Ouyang, Zhong-Wen'
'Xue, Zi-Ling'
_publ_section_title
;
 Structures and magnetic anisotropies of two seven-coordinate
 Co(ii)--nitrate complexes showing slow magnetic relaxation
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15553
_journal_page_last               15560
_journal_paper_doi               10.1039/D3NJ02160B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C11 H15 Co N5 O6 S2, C2 H3 N'
_chemical_formula_sum            'C13 H18 Co N6 O6 S2'
_chemical_formula_weight         477.38
_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
_audit_creation_date             2023-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-26 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                92.616(4)
_cell_angle_beta                 103.465(3)
_cell_angle_gamma                112.947(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7797(9)
_cell_length_b                   10.3740(11)
_cell_length_c                   10.8769(9)
_cell_measurement_reflns_used    5823
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      27.209
_cell_measurement_theta_min      2.350
_cell_volume                     976.72(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8631
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.239
_diffrn_reflns_theta_min         2.350
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1148 before and 0.0474 after correction.
The Ratio of minimum to maximum transmission is 0.6938.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4279
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0331
_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)+(0.0466P)²+0.2519P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3860
_reflns_number_total             4279
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj02160b2.cif
_cod_data_source_block           Cotmpdt(NO3)2
_cod_depositor_comments
'Adding full bibliography for 7062621--7062622.cif.'
_cod_database_code               7062622
_shelx_shelxl_version_number     2018/3
_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_max   0.876
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Rigid bond restraints
 Co1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Co1, O4
 with sigma for 1-2 distances of 0.0008 and sigma for 1-3 distances of 0.0016
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C5(H5)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.27894(2) 0.43338(2) 0.67160(2) 0.02074(9) Uani 1 1 d . U . . .
S1 S 0.05205(5) 0.35798(5) 0.48718(4) 0.02712(12) Uani 1 1 d . . . . .
S2 S 0.51324(5) 0.46199(5) 0.83204(4) 0.02612(12) Uani 1 1 d . . . . .
N2 N 0.32308(15) 0.28003(15) 0.57559(13) 0.0183(3) Uani 1 1 d . . . . .
O2 O 0.15207(15) 0.41998(15) 0.80884(13) 0.0312(3) Uani 1 1 d . U . . .
O4 O 0.33167(16) 0.65292(15) 0.71424(14) 0.0340(3) Uani 1 1 d . U . . .
O1 O 0.14629(16) 0.21511(16) 0.75697(13) 0.0346(3) Uani 1 1 d . . . . .
O3 O 0.04860(17) 0.24760(18) 0.90974(14) 0.0391(4) Uani 1 1 d . . . . .
O6 O 0.4814(2) 0.81949(16) 0.63042(16) 0.0445(4) Uani 1 1 d . . . . .
O5 O 0.4198(2) 0.59754(16) 0.56767(15) 0.0419(4) Uani 1 1 d . . . . .
N3 N 0.69236(16) 0.34784(17) 0.77249(14) 0.0244(3) Uani 1 1 d . . . . .
N1 N 0.03949(17) 0.20158(18) 0.28216(14) 0.0268(3) Uani 1 1 d . . . . .
N5 N 0.41344(18) 0.69412(17) 0.63714(15) 0.0283(3) Uani 1 1 d . . . . .
N4 N 0.11389(16) 0.29234(18) 0.82717(14) 0.0267(3) Uani 1 1 d . . . . .
C4 C 0.20557(18) 0.18752(19) 0.48058(16) 0.0200(3) Uani 1 1 d . . . . .
C8 C 0.42505(18) 0.23692(18) 0.64569(15) 0.0191(3) Uani 1 1 d . . . . .
C3 C 0.09867(19) 0.24509(19) 0.40661(16) 0.0217(3) Uani 1 1 d . . . . .
C9 C 0.55407(19) 0.34806(18) 0.74776(16) 0.0203(3) Uani 1 1 d . . . . .
C10 C 0.7449(2) 0.2750(2) 0.68759(18) 0.0296(4) Uani 1 1 d . . . . .
H10A H 0.761261 0.196944 0.726350 0.044 Uiso 1 1 calc R U . . .
H10B H 0.841931 0.341987 0.674640 0.044 Uiso 1 1 calc R U . . .
H10C H 0.666563 0.237436 0.604998 0.044 Uiso 1 1 calc R U . . .
C6 C 0.2735(2) -0.00141(19) 0.54348(17) 0.0254(4) Uani 1 1 d . . . . .
H6 H 0.252027 -0.099407 0.536911 0.031 Uiso 1 1 calc R U . . .
C7 C 0.4026(2) 0.09607(19) 0.63394(17) 0.0233(4) Uani 1 1 d . . . . .
H7 H 0.474057 0.066984 0.686711 0.028 Uiso 1 1 calc R U . . .
C5 C 0.17617(19) 0.04483(19) 0.46282(17) 0.0236(4) Uani 1 1 d . . . . .
H5 H 0.090953 -0.019693 0.396625 0.028 Uiso 1 1 calc R U . . .
C1 C 0.0992(3) 0.1286(2) 0.20317(18) 0.0361(5) Uani 1 1 d . . . . .
H1A H 0.201359 0.137827 0.251637 0.054 Uiso 1 1 calc R U . . .
H1B H 0.107413 0.171402 0.125219 0.054 Uiso 1 1 calc R U . . .
H1C H 0.028666 0.028143 0.180119 0.054 Uiso 1 1 calc R U . . .
C2 C -0.0846(2) 0.2374(3) 0.21196(19) 0.0384(5) Uani 1 1 d . . . . .
H2A H -0.177003 0.190220 0.241166 0.058 Uiso 1 1 calc R U . . .
H2B H -0.107890 0.205876 0.120243 0.058 Uiso 1 1 calc R U . . .
H2C H -0.051986 0.340209 0.227436 0.058 Uiso 1 1 calc R U . . .
N6 N 0.6576(3) 0.0687(3) 0.9072(2) 0.0611(6) Uani 1 1 d . . . . .
C11 C 0.8119(2) 0.4371(3) 0.8867(2) 0.0387(5) Uani 1 1 d . . . . .
H11A H 0.838172 0.537019 0.878396 0.058 Uiso 1 1 calc R U . . .
H11B H 0.903979 0.417935 0.895965 0.058 Uiso 1 1 calc R U . . .
H11C H 0.773467 0.416103 0.962292 0.058 Uiso 1 1 calc R U . . .
C13 C 0.6308(3) -0.0366(3) 0.9416(2) 0.0431(5) Uani 1 1 d . . . . .
C12 C 0.5973(3) -0.1706(3) 0.9885(3) 0.0552(7) Uani 1 1 d . . . . .
H12A H 0.621572 -0.232645 0.934841 0.083 Uiso 1 1 calc R U . . .
H12B H 0.487717 -0.215272 0.985527 0.083 Uiso 1 1 calc R U . . .
H12C H 0.660079 -0.154706 1.076914 0.083 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Co1 O1 88.75(4) . . ?
S2 Co1 S1 166.427(19) . . ?
S2 Co1 O1 86.70(4) . . ?
N2 Co1 S1 83.11(4) . . ?
N2 Co1 S2 83.40(4) . . ?
N2 Co1 O2 131.66(6) . . ?
N2 Co1 O4 146.45(6) . . ?
N2 Co1 O1 76.65(5) . . ?
N2 Co1 O5 89.02(6) . . ?
O2 Co1 S1 94.39(4) . . ?
O2 Co1 S2 93.46(4) . . ?
O2 Co1 O4 81.53(6) . . ?
O2 Co1 O1 55.01(5) . . ?
O2 Co1 O5 139.31(6) . . ?
O4 Co1 S1 101.31(4) . . ?
O4 Co1 S2 90.79(4) . . ?
O4 Co1 O1 136.15(5) . . ?
O4 Co1 O5 57.94(6) . . ?
O5 Co1 S1 90.54(5) . . ?
O5 Co1 S2 90.71(5) . . ?
O5 Co1 O1 165.64(5) . . ?
C3 S1 Co1 95.69(6) . . ?
C9 S2 Co1 95.69(6) . . ?
C4 N2 Co1 116.60(11) . . ?
C8 N2 Co1 116.12(10) . . ?
C8 N2 C4 119.05(15) . . ?
N4 O2 Co1 102.04(11) . . ?
N5 O4 Co1 96.24(11) . . ?
N4 O1 Co1 85.87(11) . . ?
N5 O5 Co1 90.08(11) . . ?
C9 N3 C10 125.28(14) . . ?
C9 N3 C11 119.52(16) . . ?
C11 N3 C10 114.91(15) . . ?
C3 N1 C1 124.48(17) . . ?
C3 N1 C2 119.78(17) . . ?
C2 N1 C1 115.49(15) . . ?
O6 N5 O4 122.27(17) . . ?
O6 N5 O5 122.19(18) . . ?
O5 N5 O4 115.54(16) . . ?
O1 N4 O2 116.77(15) . . ?
O3 N4 O2 121.03(17) . . ?
O3 N4 O1 122.20(18) . . ?
N2 C4 C3 115.41(15) . . ?
N2 C4 C5 121.71(16) . . ?
C5 C4 C3 122.47(15) . . ?
N2 C8 C9 115.34(15) . . ?
N2 C8 C7 121.95(15) . . ?
C7 C8 C9 122.32(16) . . ?
N1 C3 S1 122.56(15) . . ?
N1 C3 C4 118.99(16) . . ?
C4 C3 S1 118.39(12) . . ?
N3 C9 S2 122.69(13) . . ?
N3 C9 C8 118.84(15) . . ?
C8 C9 S2 118.37(13) . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.58(17) . . ?
C8 C7 C6 118.49(17) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
C4 C5 H5 120.7 . . ?
C6 C5 C4 118.61(15) . . ?
C6 C5 H5 120.7 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C13 C12 178.9(3) . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 S1 2.4474(5) . ?
Co1 S2 2.4380(5) . ?
Co1 N2 2.0979(15) . ?
Co1 O2 2.1294(14) . ?
Co1 O4 2.1318(15) . ?
Co1 O1 2.4768(16) . ?
Co1 O5 2.2688(15) . ?
S1 C3 1.6901(18) . ?
S2 C9 1.6841(18) . ?
N2 C4 1.344(2) . ?
N2 C8 1.342(2) . ?
O2 N4 1.267(2) . ?
O4 N5 1.266(2) . ?
O1 N4 1.257(2) . ?
O3 N4 1.226(2) . ?
O6 N5 1.223(2) . ?
O5 N5 1.257(2) . ?
N3 C9 1.317(2) . ?
N3 C10 1.465(2) . ?
N3 C11 1.464(2) . ?
N1 C3 1.322(2) . ?
N1 C1 1.474(2) . ?
N1 C2 1.463(3) . ?
C4 C3 1.495(3) . ?
C4 C5 1.388(3) . ?
C8 C9 1.500(2) . ?
C8 C7 1.385(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C6 H6 0.9500 . ?
C6 C7 1.386(2) . ?
C6 C5 1.383(3) . ?
C7 H7 0.9500 . ?
C5 H5 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N6 C13 1.123(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 C12 1.445(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 S1 C3 N1 -160.29(14) . . . . ?
Co1 S1 C3 C4 22.55(13) . . . . ?
Co1 S2 C9 N3 161.13(15) . . . . ?
Co1 S2 C9 C8 -22.64(14) . . . . ?
Co1 N2 C4 C3 33.37(18) . . . . ?
Co1 N2 C4 C5 -139.42(14) . . . . ?
Co1 N2 C8 C9 -33.78(18) . . . . ?
Co1 N2 C8 C7 139.20(14) . . . . ?
Co1 O2 N4 O1 -5.98(17) . . . . ?
Co1 O2 N4 O3 173.98(13) . . . . ?
Co1 O4 N5 O6 -175.64(16) . . . . ?
Co1 O4 N5 O5 4.57(18) . . . . ?
Co1 O1 N4 O2 5.04(14) . . . . ?
Co1 O1 N4 O3 -174.92(15) . . . . ?
Co1 O5 N5 O4 -4.26(16) . . . . ?
Co1 O5 N5 O6 175.94(17) . . . . ?
N2 C4 C3 S1 -39.3(2) . . . . ?
N2 C4 C3 N1 143.43(16) . . . . ?
N2 C4 C5 C6 -1.7(3) . . . . ?
N2 C8 C9 S2 39.8(2) . . . . ?
N2 C8 C9 N3 -143.84(17) . . . . ?
N2 C8 C7 C6 2.4(3) . . . . ?
C4 N2 C8 C9 178.78(13) . . . . ?
C4 N2 C8 C7 -8.2(2) . . . . ?
C8 N2 C4 C3 -179.35(14) . . . . ?
C8 N2 C4 C5 7.9(2) . . . . ?
C3 C4 C5 C6 -174.01(16) . . . . ?
C9 C8 C7 C6 174.94(16) . . . . ?
C10 N3 C9 S2 -165.72(16) . . . . ?
C10 N3 C9 C8 18.1(3) . . . . ?
C7 C8 C9 S2 -133.17(16) . . . . ?
C7 C8 C9 N3 43.2(2) . . . . ?
C7 C6 C5 C4 -4.1(3) . . . . ?
C5 C4 C3 S1 133.43(15) . . . . ?
C5 C4 C3 N1 -43.8(2) . . . . ?
C5 C6 C7 C8 3.8(3) . . . . ?
C1 N1 C3 S1 166.49(16) . . . . ?
C1 N1 C3 C4 -16.4(3) . . . . ?
C2 N1 C3 S1 -7.5(2) . . . . ?
C2 N1 C3 C4 169.68(17) . . . . ?
C11 N3 C9 S2 7.8(3) . . . . ?
C11 N3 C9 C8 -168.43(18) . . . . ?
