A highly active manganese precatalyst for the hydrosilylation of ketones and esters.
Mukhopadhyay, Tufan K.; Flores, Marco; Groy, Thomas L.; Trovitch, Ryan J.; Journal of the American Chemical Society 136 (2014) 882–885; doi:10.1021/ja4116346

data_4120531
_publ_section_title
;
 A highly active manganese precatalyst for the hydrosilylation of ketones
 and esters.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              882
_journal_page_last               885
_journal_paper_doi               10.1021/ja4116346
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C39 H41 Mn N3 P2'
_chemical_formula_sum            'C39 H41 Mn N3 P2'
_chemical_formula_weight         668.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.103(3)
_cell_angle_beta                 90.505(3)
_cell_angle_gamma                115.432(2)
_cell_formula_units_Z            2
_cell_length_a                   10.773(2)
_cell_length_b                   12.341(2)
_cell_length_c                   14.004(3)
_cell_measurement_reflns_used    4603
_cell_measurement_temperature    123.(2)
_cell_measurement_theta_max      26.2468
_cell_measurement_theta_min      2.2273
_cell_volume                     1672.5(5)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection
'Bruker Instrument Service v2010, 9, 0, 0 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2010.9-1 (Bruker AXS, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart APEX'
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14656
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         1.84
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.528
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.5642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                5273
_reflns_number_total             6766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4116346_si_001.cif
_cod_data_source_block           Ph2PPrPDIMn
_cod_database_code               4120531