Synthesis, characterization, and catalytic application in aldehyde hydrosilylation of half-sandwich nickel complexes bearing (κ<sup>1</sup>-C)- and hemilabile (κ<sup>2</sup>-C,S)-thioether-functionalised NHC ligands.
Ulm, Franck; Poblador-Bahamonde, Amalia I; Choppin, Sabine; Bellemin-Laponnaz, Stéphane; Chetcuti, Michael J.; Achard, Thierry; Ritleng, Vincent; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17134–17145; doi:10.1039/c8dt03882a

data_7048122
_publ_section_title
;
 Synthesis, characterization, and catalytic application in aldehyde
 hydrosilylation of half-sandwich nickel complexes bearing
 (\k<sup>1</sup>-C)- and hemilabile
 (\k<sup>2</sup>-C,S)-thioether-functionalised NHC ligands.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17134
_journal_page_last               17145
_journal_paper_doi               10.1039/c8dt03882a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C23 H31 N2 Ni S, F6 P'
_chemical_formula_sum            'C23 H31 F6 N2 Ni P S'
_chemical_formula_weight         571.24
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-09-13 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2564(3)
_cell_length_b                   15.4610(4)
_cell_length_c                   27.1428(7)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.60
_cell_volume                     5143.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            50260
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/n-pentane'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+4.6493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5579
_reflns_number_total             7498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03882a2.cif
_cod_data_source_block           mcfu170413
_cod_depositor_comments
'Adding full bibliography for 7048120--7048123.cif.'
_cod_database_code               7048122
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.847
_shelxl_version_number           2013-4
_shelx_res_checksum              44467