Radical Hydrodehalogenation of Aryl Halides with H2 Catalyzed by a Phenanthroline-Based PNNP Cobalt(I) Complex
Jheng, Nai-Yuan; Ishizaka, Yusuke; Naganawa, Yuki; Minami, Yasunori; Sekiguchi, Akira; Iizuka, Kosuke; Nakajima, Yumiko; ACS Catalysis 12 (2022) 2320–2329; doi:10.1021/acscatal.1c04797

data_4519343
_publ_section_title
;
 Radical Hydrodehalogenation of Aryl Halides with H2 Catalyzed by a
 Phenanthroline-Based PNNP Cobalt(I) Complex
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              2320
_journal_page_last               2329
_journal_paper_doi               10.1021/acscatal.1c04797
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C55 H52 Br Co N2 P2'
_chemical_formula_weight         941.76
_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                 103.191(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.276(2)
_cell_length_b                   26.264(5)
_cell_length_c                   17.399(4)
_cell_measurement_reflns_used    730
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4571.9(16)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'ORTEP3 for windows'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1834
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57744
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Rigaku NUMABS'
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.880
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.401
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.309
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         10155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.309
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0725
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7070
_reflns_number_total             10155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04797_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4519343
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.381
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              92358
_shelx_hkl_checksum              79496