Organopnictogen(III) bis(arylthiolates) containing NCN-aryl pincer ligands: from synthesis and characterization to reactivity
Duneș, Gabriel; Soran, Albert; Silvestru, Cristian; Dalton Transactions  (2022) –; doi:10.1039/D2DT01436J

data_7710560
_publ_section_title
;
 Organopnictogen(III) bis(arylthiolates) containing NCN-aryl pincer
 ligands: from synthesis and characterization to reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01436J
_journal_year                    2022
_chemical_formula_moiety         'C16 H23 Bi I2 N2 O2, 0.5(I2)'
_chemical_formula_sum            'C16 H23 Bi I3 N2 O2'
_chemical_formula_weight         865.04
_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
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2022-02-17 deposited with the CCDC.	2022-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.5660(10)
_cell_angle_beta                 94.0610(10)
_cell_angle_gamma                109.3520(10)
_cell_formula_units_Z            2
_cell_length_a                   9.1472(2)
_cell_length_b                   9.8243(2)
_cell_length_c                   13.1662(3)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    295.(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.37
_cell_volume                     1112.83(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker APEX4 2021.10-0'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1328)'
_computing_publication_material  'Bruker APEX4 2021.10-0'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295.(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39183
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'Incoatec Mo--I\mS 3.0 microfocus source'
_exptl_absorpt_coefficient_mu    12.094
_exptl_absorpt_correction_T_max  0.55
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.557
_refine_ls_extinction_coef       0.00153(13)
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0266P)^2^+3.8493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5187
_reflns_number_total             5515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01436j2.cif
_cod_data_source_block           0166alb
_cod_database_code               7710560
_shelx_res_checksum              38044
_shelx_hkl_checksum              36968