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_4514102
_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 Cl Co N P2'
_chemical_formula_sum            'C21 H39 Cl Co N P2'
_chemical_formula_weight         461.85
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.477(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2619(7)
_cell_length_b                   8.3444(4)
_cell_length_c                   19.9331(11)
_cell_measurement_reflns_used    17209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.65
_cell_volume                     2357.0(2)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17209
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.445
_diffrn_reflns_theta_min         2.649
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_correction_T_min  0.6497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX 2'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0297P)^2^+0.6775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3966
_reflns_number_total             4818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b00116_si_002.cif
_cod_data_source_block           comlex1_Cl
_cod_database_code               4514102
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.650
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              99744
_shelx_hkl_checksum              50021