#------------------------------------------------------------------------------
#$Date: 2025-11-29 21:46:04 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303777 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/94/7719491.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_7719491
loop_
_publ_author_name
'Robertson, Grace M.'
'Jaffe, Adam'
_publ_section_title
;
 Structural and electronic tuning of hybrid metal thiocyanate
 N-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 ω and φ-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 λ/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/[σ²(Fo²)+(0.0447P)²+0.3421P] where P=(Fo²+2Fc²)/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 > 2σ(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_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_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'
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
Ni1 Ni 0.88161(4) 0.36567(4) 0.48631(3) 0.01564(11) Uani 1 1 d . . . . .
S1 S 0.82694(6) -0.21562(5) 0.67368(4) 0.01794(12) Uani 1 1 d . . . . .
S2 S 0.26431(6) 0.63666(6) 0.70974(5) 0.02065(12) Uani 1 1 d . . . . .
O1 O 0.97160(18) 0.58712(15) 0.38363(13) 0.0175(3) Uani 1 1 d . . . . .
O2 O 0.6955(2) 1.08001(18) -0.04398(14) 0.0270(3) Uani 1 1 d . . . . .
N1 N 0.8501(2) 0.13468(19) 0.60395(16) 0.0201(3) Uani 1 1 d . . . . .
N2 N 0.6416(2) 0.5020(2) 0.59722(16) 0.0188(3) Uani 1 1 d . . . . .
N3 N 0.8963(2) 0.71071(19) 0.28006(16) 0.0164(3) Uani 1 1 d . . . . .
C1 C 0.8404(2) -0.0094(2) 0.63495(18) 0.0178(3) Uani 1 1 d . . . . .
C2 C 0.4874(3) 0.5573(2) 0.64415(18) 0.0180(4) Uani 1 1 d . . . . .
C3 C 0.7446(3) 0.8378(2) 0.3176(2) 0.0200(4) Uani 1 1 d . . . . .
H3 H 0.688504 0.839260 0.416943 0.024 Uiso 1 1 calc R U . . .
C4 C 0.6695(3) 0.9663(2) 0.21307(19) 0.0203(4) Uani 1 1 d . . . . .
H4 H 0.562262 1.056541 0.239759 0.024 Uiso 1 1 calc R U . . .
C5 C 0.7529(3) 0.9621(2) 0.0680(2) 0.0208(4) Uani 1 1 d . . . . .
C6 C 0.9083(3) 0.8249(3) 0.0325(2) 0.0248(4) Uani 1 1 d . . . . .
H6 H 0.965019 0.817634 -0.066047 0.030 Uiso 1 1 calc R U . . .
C7 C 0.9779(3) 0.7014(2) 0.1404(2) 0.0212(4) Uani 1 1 d . . . . .
H7 H 1.084125 0.608883 0.116867 0.025 Uiso 1 1 calc R U . . .
C8 C 0.5529(3) 1.2364(3) -0.0125(2) 0.0316(5) Uani 1 1 d . . . . .
H8A H 0.528548 1.313249 -0.103358 0.047 Uiso 1 1 calc R U . . .
H8B H 0.593422 1.297951 0.043398 0.047 Uiso 1 1 calc R U . . .
H8C H 0.439998 1.204231 0.043814 0.047 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 0.0181 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Ni1 S1 83.548(17) 2_666 2_756 ?
O1 Ni1 S1 82.58(4) . 2_756 ?
O1 Ni1 S1 92.39(4) 2_766 2_756 ?
O1 Ni1 S2 166.59(4) 2_766 2_666 ?
O1 Ni1 S2 94.72(4) . 2_666 ?
O1 Ni1 O1 72.05(5) . 2_766 ?
N1 Ni1 S1 91.26(5) . 2_756 ?
N1 Ni1 S2 96.81(5) . 2_666 ?
N1 Ni1 O1 166.24(6) . . ?
N1 Ni1 O1 96.05(6) . 2_766 ?
N1 Ni1 N2 92.98(6) . . ?
N2 Ni1 S1 174.49(5) . 2_756 ?
N2 Ni1 S2 92.46(4) . 2_666 ?
N2 Ni1 O1 94.01(6) . . ?
N2 Ni1 O1 90.66(6) . 2_766 ?
C1 S1 Ni1 102.00(6) . 2_756 ?
C2 S2 Ni1 102.95(6) . 2_666 ?
Ni1 O1 Ni1 107.95(5) . 2_766 ?
N3 O1 Ni1 123.72(10) . 2_766 ?
N3 O1 Ni1 124.71(10) . . ?
C5 O2 C8 117.89(15) . . ?
C1 N1 Ni1 161.45(14) . . ?
C2 N2 Ni1 162.96(14) . . ?
C3 N3 O1 120.09(14) . . ?
C3 N3 C7 121.70(15) . . ?
C7 N3 O1 118.21(14) . . ?
N1 C1 S1 178.14(16) . . ?
N2 C2 S2 179.21(16) . . ?
N3 C3 H3 119.8 . . ?
N3 C3 C4 120.48(17) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.10(17) . . ?
C5 C4 H4 120.4 . . ?
O2 C5 C4 125.13(17) . . ?
O2 C5 C6 115.98(17) . . ?
C4 C5 C6 118.89(17) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 C5 119.61(17) . . ?
C7 C6 H6 120.2 . . ?
N3 C7 C6 120.18(17) . . ?
N3 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 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
Ni1 S1 2.5286(5) 2_756 ?
Ni1 S2 2.4679(5) 2_666 ?
Ni1 O1 2.0695(12) . ?
Ni1 O1 2.0759(12) 2_766 ?
Ni1 N1 2.0033(16) . ?
Ni1 N2 2.0286(16) . ?
S1 C1 1.6591(18) . ?
S2 C2 1.6621(19) . ?
O1 N3 1.3557(18) . ?
O2 C5 1.343(2) . ?
O2 C8 1.443(3) . ?
N1 C1 1.159(2) . ?
N2 C2 1.153(3) . ?
N3 C3 1.341(2) . ?
N3 C7 1.347(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(3) . ?
C5 C6 1.401(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.367(3) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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
Ni1 O1 N3 C3 82.32(17) . . . . ?
Ni1 O1 N3 C3 -73.63(18) 2_766 . . . ?
Ni1 O1 N3 C7 -97.67(16) . . . . ?
Ni1 O1 N3 C7 106.37(15) 2_766 . . . ?
O1 N3 C3 C4 178.52(16) . . . . ?
O1 N3 C7 C6 -178.99(17) . . . . ?
O2 C5 C6 C7 178.62(18) . . . . ?
N3 C3 C4 C5 0.2(3) . . . . ?
C3 N3 C7 C6 1.0(3) . . . . ?
C3 C4 C5 O2 -179.13(18) . . . . ?
C3 C4 C5 C6 1.5(3) . . . . ?
C4 C5 C6 C7 -1.9(3) . . . . ?
C5 C6 C7 N3 0.7(3) . . . . ?
C7 N3 C3 C4 -1.5(3) . . . . ?
C8 O2 C5 C4 9.2(3) . . . . ?
C8 O2 C5 C6 -171.37(18) . . . . ?
