Selective N-Formylation of Amines with H2 and CO2 Catalyzed by Cobalt Pincer Complexes
Daw, Prosenjit; Chakraborty, Subrata; Leitus, Gregory; Diskin-Posner, Yael; Ben-David, Yehoshoa; Milstein, David; ACS Catalysis 7 (2017) 2500–; doi:10.1021/acscatal.7b00116

data_4514101
_publ_section_title
;
 Selective N-Formylation of Amines with H2 and CO2 Catalyzed by Cobalt
 Pincer Complexes
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              2500
_journal_paper_doi               10.1021/acscatal.7b00116
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C21 H39 Cl2 Co N P2'
_chemical_formula_sum            'C21 H39 Cl2 Co N P2'
_chemical_formula_weight         497.30
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                98.190(6)
_cell_angle_beta                 90.641(3)
_cell_angle_gamma                110.333(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2698(7)
_cell_length_b                   10.9458(9)
_cell_length_c                   14.8705(15)
_cell_measurement_reflns_used    23411
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.78
_cell_volume                     1246.6(2)
_computing_cell_refinement       'Software Bruker KappaApex CCD'
_computing_data_collection       'Software Bruker KappaApex CCD'
_computing_data_reduction        'Software Bruker KappaApex CCD'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker KappaApex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18323
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.613
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker KappaApex CCD'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       plate
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+0.3353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4126
_reflns_number_total             5087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b00116_si_002.cif
_cod_data_source_block           complex1
_cod_database_code               4514101
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              68104
_shelx_hkl_checksum              61912