Phosphine-Free Pincer Cobalt Catalyst Precursors for the Selective Hydrogenation of Olefins
Puylaert, Pim; Dell'Acqua, Andrea; El Ouahabi, Fatima; Spannenberg, Anke; Roisnel, Thierry; Lefort, Laurent; Hinze, Sandra; Tin, Sergey; de Vries, Johannes G.; Catalysis Science & Technology  (2019) –; doi:10.1039/C8CY02218F

data_1550279
_publ_section_title
;
 Phosphine-Free Pincer Cobalt Catalyst Precursors for the Selective
 Hydrogenation of Olefins
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C8CY02218F
_journal_year                    2019
_chemical_formula_sum            'C20 H32 Cl4 Co2 N4 S2'
_chemical_formula_weight         652.27
_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
_audit_update_record
;
2018-08-27 deposited with the CCDC.
2018-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                72.8236(10)
_cell_angle_beta                 88.0499(11)
_cell_angle_gamma                70.2746(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6862(3)
_cell_length_b                   11.1085(4)
_cell_length_c                   17.7851(6)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.64
_cell_volume                     1362.03(9)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54839
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.780
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            blue-voilet
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0292P)^2^+0.5597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6112
_reflns_number_total             6586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy02218f2.cif
_cod_data_source_block           AX1392
_cod_database_code               1550279
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              65638
_shelx_hkl_checksum              97257