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_7719494
_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 N3 Ni O S2'
_chemical_formula_sum            'C8 H7 N3 Ni O S2'
_chemical_formula_weight         284.00
_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             2025-06-28
_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                 98.538(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5711(8)
_cell_length_b                   7.5734(8)
_cell_length_c                   18.995(2)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      25.288
_cell_measurement_theta_min      2.168
_cell_volume                     1077.1(2)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (G. Sheldrick)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON-III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_monochromator  'HELIOS Multi-layer'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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            54990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.360
_diffrn_reflns_theta_min         2.168
_diffrn_source                   micro-focus
_diffrn_source_type              'Incoatec IuS'
_exptl_absorpt_coefficient_mu    2.162
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7025
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0752 before and 0.0610 after correction.
The Ratio of minimum to maximum transmission is 0.8150.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         1971
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.311
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.1009
_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^)+40.6168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2279
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1932
_reflns_number_total             1971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02188j2.cif
_cod_data_source_block           gr1_121a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7719491--7719495.cif.
;
_cod_database_code               7719494
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.745
_olex2_refinement_description
;
1. Restrained planarity
 C3A, C4A, C5A, C6A, C7A, N3
 with sigma of 0.1
2. Rigid bond restraints
 C3, C4, C5, C6, C7, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1, S1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3A, C4A, C5A, C6A, C7A, N3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3A, O1, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim N3: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim S1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim N3A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
N3A \\sim O1 \\sim N3: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Others
 Sof(C7A)=Sof(H7A)=Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C3A)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C4A)=Sof(H4A)=Sof(N3A)=1-FVAR(1)
 Sof(C3)=Sof(N3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=
 Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C7A(H7A), C6A(H6A), C5A(H5A), C4A(H4A)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              18206
_olex2_submission_special_instructions 'No special instructions were received'