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_7719491
_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 O2 S2'
_chemical_formula_sum            'C8 H7 N3 Ni O2 S2'
_chemical_formula_weight         300.00
_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
_audit_creation_date             2025-06-24
_audit_creation_method
;FinalCif V152 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-06-28 deposited with the CCDC.	2025-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                76.322(3)
_cell_angle_beta                 74.716(3)
_cell_angle_gamma                72.152(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7849(6)
_cell_length_b                   8.1304(6)
_cell_length_c                   9.7163(8)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      76.019
_cell_measurement_theta_min      4.787
_cell_volume                     556.51(8)
_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-III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_monochromator  'HELIOS Multi-layer'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18052
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.572
_diffrn_reflns_theta_min         4.787
_diffrn_source                   micro-focus
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_type              'Incoatec Diamond'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.948
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.6181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1371 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.8198.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       prism
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0273
_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/[\s^2^(Fo^2^)+(0.0447P)^2^+0.3421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2152
_reflns_number_total             2315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02188j2.cif
_cod_data_source_block           gr1_151
_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               7719491
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.438
_shelx_estimated_absorpt_t_max   0.602
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              59452