Mechanistic Investigation of Bis(imino)pyridine Manganese Catalyzed Carbonyl and Carboxylate Hydrosilylation.
Mukhopadhyay, Tufan K.; Rock, Christopher L.; Hong, Mannkyu; Ashley, Daniel C.; Groy, Thomas L.; Baik, Mu-Hyun; Trovitch, Ryan J.; Journal of the American Chemical Society 139 (2017) 4901–4915; doi:10.1021/jacs.7b00879

data_4131232
_publ_section_title
;
 Mechanistic Investigation of Bis(imino)pyridine Manganese Catalyzed
 Carbonyl and Carboxylate Hydrosilylation.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4901
_journal_page_last               4915
_journal_paper_doi               10.1021/jacs.7b00879
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C94 H92 F6 Mn2 N6 O2 P4, 6(C4 H8 O)'
_chemical_formula_sum            'C118 H140 F6 Mn2 N6 O8 P4'
_chemical_formula_weight         2118.11
_chemical_name_common            2Ph2PPrPDIMnOCPhCF3
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                92.0219(9)
_cell_angle_beta                 115.4329(8)
_cell_angle_gamma                109.4571(9)
_cell_formula_units_Z            1
_cell_length_a                   14.5008(8)
_cell_length_b                   14.7881(9)
_cell_length_c                   15.1141(9)
_cell_measurement_reflns_used    4214
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      24.6409
_cell_measurement_theta_min      2.3483
_cell_volume                     2698.6(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2014)'
_computing_data_collection       'Bruker Instrument Service v2015.5.1.3'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL XT-2014/4'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22407
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.507
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9794
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0674P)^2^+2.1838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                7072
_reflns_number_total             9794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00879_si_002.cif
_cod_data_source_block           2Ph2PPrPDIMnOCPhCF3
_cod_database_code               4131232
_shelx_res_checksum              73671
_shelx_hkl_checksum              11007