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_7048121
_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         'C21 H27 N2 Ni S, F6 P'
_chemical_formula_sum            'C21 H27 F6 N2 Ni P S'
_chemical_formula_weight         543.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 95.4090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2425(2)
_cell_length_b                   15.5464(4)
_cell_length_c                   16.5839(5)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.61
_cell_measurement_theta_min      3.91
_cell_volume                     2372.29(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23312
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.698
_diffrn_reflns_theta_min         3.905
_diffrn_source                   'Cu-ImuS microfocus tube'
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF / n-pentane'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+5.3540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3634
_reflns_number_total             4166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03882a2.cif
_cod_data_source_block           mcfu170809
_cod_depositor_comments
'Adding full bibliography for 7048120--7048123.cif.'
_cod_database_code               7048121
_shelx_estimated_absorpt_t_min   0.598
_shelx_estimated_absorpt_t_max   0.785
_shelxl_version_number           2013-4
_shelx_res_checksum              21511