Synthesis of Cyclic Imides by Acceptorless Dehydrogenative Coupling of Diols and Amines Catalyzed by a Manganese Pincer Complex.
Espinosa-Jalapa, Noel Angel; Kumar, Amit; Leitus, Gregory; Diskin-Posner, Yael; Milstein, David; Journal of the American Chemical Society 139 (2017) 11722–11725; doi:10.1021/jacs.7b08341

data_4131662
_publ_section_title
;
 Synthesis of Cyclic Imides by Acceptorless Dehydrogenative Coupling of
 Diols and Amines Catalyzed by a Manganese Pincer Complex.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11722
_journal_page_last               11725
_journal_paper_doi               10.1021/jacs.7b08341
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C21 H35 Br Mn N2 O2 P'
_chemical_formula_sum            'C21 H35 Br Mn N2 O2 P'
_chemical_formula_weight         513.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.111(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6861(15)
_cell_length_b                   14.7681(18)
_cell_length_c                   13.3305(15)
_cell_measurement_reflns_used    19395
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.18
_cell_volume                     2373.7(5)
_computing_cell_refinement       APEX2
_computing_data_collection       'Collect package Bruker APEX2'
_computing_data_reduction        APEX2
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX - II KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19386
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.139
_diffrn_reflns_theta_min         2.181
_exptl_absorpt_coefficient_mu    2.325
_exptl_absorpt_correction_T_max  0.7758
_exptl_absorpt_correction_T_min  0.4123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+1.2840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4318
_reflns_number_total             5189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08341_si_002.cif
_cod_data_source_block           complex5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4131662
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.412
_shelx_estimated_absorpt_t_max   0.776
_shelx_res_checksum              97842
_shelx_hkl_checksum              70774