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_4134358
_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 Y, C7 H8'
_chemical_formula_sum            'C46 H71 N3 Ni P3 Y'
_chemical_formula_weight         906.58
_chemical_name_common            17165-NiYL3
_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-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 95.0170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8967(5)
_cell_length_b                   14.0478(5)
_cell_length_c                   25.5457(9)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.90
_cell_measurement_theta_min      2.35
_cell_volume                     4610.4(3)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0860
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            78598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.576
_diffrn_reflns_theta_min         2.148
_diffrn_source                   'I\uS 3.0 Microfocus Tube'
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7465
_exptl_transmission_factor_min   0.6840
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         16776
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0269P)^2^+1.5086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10275
_reflns_number_total             16776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00905_si_001.cif
_cod_data_source_block           17165_Complex-7_NiY
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4134358
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              82425
_shelx_hkl_checksum              74065