Rare-Earth Supported Nickel Catalysts for Alkyne Semihydrogenation: Chemo- and Regioselectivity Impacted by the Lewis Acidity and Size of the Support.
Ramirez, Bianca L.; Lu, Connie C.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00905

data_4134360
_publ_section_title
;
 Rare-Earth Supported Nickel Catalysts for Alkyne Semihydrogenation:
 Chemo- and Regioselectivity Impacted by the Lewis Acidity and Size of the
 Support.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00905
_journal_year                    2020
_chemical_formula_moiety         'C39 H63 N3 Ni P3 La, C7 H8'
_chemical_formula_sum            'C42.5 H67 La N3 Ni P3'
_chemical_formula_weight         910.52
_chemical_name_common            19023-NiLa_monoclinic
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.336(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.2562(12)
_cell_length_b                   10.0180(6)
_cell_length_c                   39.979(2)
_cell_measurement_reflns_used    2934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.47
_cell_volume                     8513.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ShelXle Rev. 712 (Huebschle, 2011)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            127265
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.600
_diffrn_reflns_theta_min         2.165
_diffrn_source                   'I\uS 3.0 Microfocus Tube'
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6514
_refine_diff_density_max         0.474
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         13087
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0097P)^2^+14.7490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11429
_reflns_number_total             13087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00905_si_001.cif
_cod_data_source_block           19023_Complex-8'_NiLa_monoclinic
_cod_original_cell_volume        8513.2(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C42.50 H67 La N3 Ni P3'
_cod_database_code               4134360
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.821
_shelx_estimated_absorpt_t_max   0.884
_shelx_res_checksum              29021
_shelx_hkl_checksum              24426