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_4134363
_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         'C43 H71 N3 Ni O P3 Y'
_chemical_formula_sum            'C43 H71 N3 Ni O P3 Y'
_chemical_formula_weight         886.55
_chemical_name_common            17034_NiYL3THF
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                93.4220(10)
_cell_angle_beta                 92.5660(10)
_cell_angle_gamma                114.5710(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9384(4)
_cell_length_b                   12.4594(4)
_cell_length_c                   20.0961(7)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    126(2)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.32
_cell_volume                     2479.05(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'ShelXle Rev. 712 (Huebschle, 2011)'
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_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      126(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            91591
_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         26.731
_diffrn_reflns_theta_min         2.221
_diffrn_source                   normal
_exptl_absorpt_coefficient_mu    1.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6647
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         10522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0301P)^2^+0.4866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8380
_reflns_number_total             10522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00905_si_001.cif
_cod_data_source_block           17034_Complex-7-THF
_cod_database_code               4134363
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.825
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              76812
_shelx_hkl_checksum              2175
_shelx_fab_checksum              67407