A non-innocent, π-extended N-heterobicyclic carbene-thiolate ligand.
Marquardt, Michael; Vendier, Laure; Sournia-Saquet, Alix; Maurel, Vincent; Mouesca, Jean-Marie; Bastin, Stéphanie; Castillo, Ivan; César, Vincent; Chemical communications (Cambridge, England) 61 (2025) 11437–11440; doi:10.1039/d5cc02841h

data_7134757
_publ_section_title
;
 A non-innocent, &#x3c0;-extended N-heterobicyclic carbene-thiolate
 ligand.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11437
_journal_page_last               11440
_journal_paper_doi               10.1039/d5cc02841h
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C32 H30 N4 Ni S2'
_chemical_formula_sum            'C32 H30 N4 Ni S2'
_chemical_formula_weight         593.46
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2025-05-09 deposited with the CCDC.	2025-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                94.9271(6)
_cell_angle_beta                 109.9393(6)
_cell_angle_gamma                107.1058(6)
_cell_formula_units_Z            2
_cell_length_a                   11.23947(7)
_cell_length_b                   11.63264(9)
_cell_length_c                   12.08649(7)
_cell_measurement_reflns_used    32865
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.65
_cell_measurement_theta_min      3.96
_cell_volume                     1388.979(19)
_computing_cell_refinement
; 
 CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
;
_computing_data_collection
'CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)'
_computing_data_reduction
; 
 CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_unetI/netI     0.033
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48416
_diffrn_reflns_theta_full        74.788
_diffrn_reflns_theta_max         80.417
_diffrn_reflns_theta_min         3.977
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9968
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5946
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.0004629
_refine_ls_shift/su_mean         0.0000230
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 2.09P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1069
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1069
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5655
_reflns_number_total             5946
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.54
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0394
_oxford_refine_ls_scale          3.83(5)
_oxford_reflns_number_all        5946
_cod_data_source_file            d5cc02841h2.cif
_cod_data_source_block           20231208EqA
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

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

 Adding full bibliography for 7134755--7134757.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7134757
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0394
_oxford_refine_ls_wr_factor_all  0.1069