Hydroamination of Aromatic Alkynes to Imines Catalyzed by Pd(II)-Anthraphos Complexes.
Erken, Christina; Hindemith, Carsten; Weyhermüller, Thomas; Hölscher, Markus; Werlé, Christophe; Leitner, Walter; ACS omega 5 (2020) 8912–8918; doi:10.1021/acsomega.0c00562

data_4517542
_publ_section_title
;
 Hydroamination of Aromatic Alkynes to Imines Catalyzed by
 Pd(II)-Anthraphos Complexes.
;
_journal_issue                   15
_journal_name_full               'ACS omega'
_journal_page_first              8912
_journal_page_last               8918
_journal_paper_doi               10.1021/acsomega.0c00562
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C46 H43 Cl P2 Pd, C4 H8 O'
_chemical_formula_sum            'C50 H51 Cl O P2 Pd'
_chemical_formula_weight         871.70
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                WLG-ECH-236
_audit_creation_date             2018-01-25
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                85.293(3)
_cell_angle_beta                 74.338(3)
_cell_angle_gamma                84.999(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4317(15)
_cell_length_b                   12.324(2)
_cell_length_c                   15.915(2)
_cell_measurement_reflns_used    8538
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9111
_cell_measurement_theta_min      2.6632
_cell_volume                     2146.7(5)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (G. M. Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         1\mS
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63768
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.095
_diffrn_reflns_theta_min         2.573
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.98840
_exptl_absorpt_correction_T_min  0.95891
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.871
_refine_diff_density_min         -1.647
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         13682
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.9696P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10235
_reflns_number_total             13682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c00562_si_003.cif
_cod_data_source_block           11329
_cod_depositor_comments
'Adding full bibliography for 4517542--4517544.cif.'
_cod_database_code               4517542
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.984
_shelxl_version_number           2013-2
_shelx_res_checksum              35449
_shelx_hkl_checksum              38651