Dehydrogenative Cross-Coupling of Primary Alcohols To Form Cross-Esters Catalyzed by a Manganese Pincer Complex
Das, Uttam Kumar; Ben-David, Yehoshoa; Leitus, Gregory; Diskin-Posner, Yael; Milstein, David; ACS Catalysis 9 (2018) 479–; doi:10.1021/acscatal.8b04585

data_4515458
_publ_section_title
;
 Dehydrogenative Cross-Coupling of Primary Alcohols To Form Cross-Esters
 Catalyzed by a Manganese Pincer Complex
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              479
_journal_paper_doi               10.1021/acscatal.8b04585
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C25 H19 Br Mn N2 O2 P'
_chemical_formula_sum            'C25 H19 Br Mn N2 O2 P'
_chemical_formula_weight         545.24
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.057(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9669(4)
_cell_length_b                   13.8740(4)
_cell_length_c                   12.3572(4)
_cell_measurement_reflns_used    24591
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.3410
_cell_measurement_theta_min      3.7710
_cell_volume                     2219.93(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.4c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.4c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.4c (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44170
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.473
_exptl_absorpt_coefficient_mu    2.493
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.212
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.4c (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0188
_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^)+(0.0117P)^2^+1.9534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4187
_reflns_number_total             4358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04585_si_002.cif
_cod_data_source_block           complex6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4515458
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.550
_shelx_estimated_absorpt_t_max   0.803
_shelx_res_checksum              31631
_shelx_hkl_checksum              2804