Half-Sandwich Manganese Complexes Bearing Cp Tethered N-Heterocyclic Carbene Ligands: Synthesis and Mechanistic Insights into the Catalytic Ketone Hydrosilylation
Valyaev, Dmitry A.; Wei, Duo; Elangovan, Saravanakumar; Cavailles, Matthieu; Dorcet, Vincent; Sortais, Jean-Baptiste; Darcel, Christophe; Lugan, Noël; Organometallics 35 (2016) 4090–; doi:10.1021/acs.organomet.6b00785

data_4089171
_publ_section_title
;
 Half-Sandwich Manganese Complexes Bearing Cp Tethered N-Heterocyclic
 Carbene Ligands: Synthesis and Mechanistic Insights into the Catalytic
 Ketone Hydrosilylation
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              4090
_journal_paper_doi               10.1021/acs.organomet.6b00785
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C32 H33 Mn N2 O Si'
_chemical_formula_sum            'C32 H33 Mn N2 O Si'
_chemical_formula_weight         544.63
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-06-21T11:30:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.803(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8276(5)
_cell_length_b                   17.7797(7)
_cell_length_c                   28.1804(17)
_cell_measurement_reflns_used    23582
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.6430
_cell_measurement_theta_min      3.1789
_cell_measurement_wavelength     0.71073
_cell_volume                     5871.2(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            33051
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.169
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS, Sheldrick, Bruker, 2000'
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+12.5126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0
_reflns_number_gt                5681
_reflns_number_total             6002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00785_si_002.cif
_cod_data_source_block           8b
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4089171
_shelx_res_checksum              2482
_shelx_hkl_checksum              75526
_shelx_fab_checksum              77482