Structural and electronic tuning of hybrid metal thiocyanate <i>N</i>-oxides.
Robertson, Grace M.; Jaffe, Adam; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14648–14653; doi:10.1039/d5dt02188j

data_7719493
_publ_section_title
;
 Structural and electronic tuning of hybrid metal thiocyanate
 <i>N</i>-oxides.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14648
_journal_page_last               14653
_journal_paper_doi               10.1039/d5dt02188j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C8 H7 Co N3 O S2'
_chemical_formula_sum            'C8 H7 Co N3 O S2'
_chemical_formula_weight         284.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2025-06-25
_audit_creation_method
;FinalCif V152 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-06-29 deposited with the CCDC.	2025-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.708(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6608(5)
_cell_length_b                   7.6617(5)
_cell_length_c                   18.9923(12)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      68.231
_cell_measurement_theta_min      6.237
_cell_volume                     1104.68(12)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2022)'
_computing_data_collection       'Bruker APEX (Bruker, 2022)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'FinalCIF (Kratzert, 2023)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON-II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_monochromator  'MONTEL Multi-layer'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32121
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.342
_diffrn_reflns_theta_min         6.237
_diffrn_source                   micro-focus
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_type              'Incoatec I\mS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.529
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1449 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.7405.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.899
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2018
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0672
_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/[\s^2^(Fo^2^)+(0.0514P)^2^+11.0429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1973
_reflns_number_total             2018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02188j2.cif
_cod_data_source_block           gr154-aj1
_cod_depositor_comments
'Adding full bibliography for 7719491--7719495.cif.'
_cod_database_code               7719493
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.257
_shelx_estimated_absorpt_t_max   0.717
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N007-C5A
 1.38 with sigma of 0.02
3. Restrained planarity
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma of 0.1
4. Rigid bond restraints
 C5, C4, C3, C2, C1, N007
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N007, C5A, C4A, C3A, C2A, C1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C3 \\sim C2 \\sim C1 \\sim N007: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N007 \\sim C5A \\sim C4A \\sim C3A \\sim C2A \\sim C1A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
6. Same fragment restrains
{C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.001, 1-3: 0.002
as in
{C1A, C2A, C3A, C4A, C5A, C6A}
7. Others
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
8.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A)
8.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_dffrn_source_type               Siemens
_shelx_res_checksum              42429