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_4515459
_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         'C32 H26 Mn N2 O3 P'
_chemical_formula_sum            'C32 H26 Mn N2 O3 P'
_chemical_formula_weight         572.46
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.9510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.76630(10)
_cell_length_b                   16.9042(2)
_cell_length_c                   16.0896(2)
_cell_measurement_reflns_used    9394
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.0500
_cell_measurement_theta_min      5.2550
_cell_volume                     2630.72(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'micro-focus sealed X-ray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         4.571
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.962
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0365P)^2^+1.5568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4351
_reflns_number_total             4815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04585_si_002.cif
_cod_data_source_block           complex8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4515459
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.797
_shelx_estimated_absorpt_t_max   0.886
_shelx_res_checksum              29824
_shelx_hkl_checksum              18211