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_4517543
_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         'C40 H30 N P2 Pd, F6 Sb, 2(C4 H8 O)'
_chemical_formula_sum            'C48 H46 F6 N O2 P2 Pd Sb'
_chemical_formula_weight         1072.95
_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-CE-501-04
_audit_creation_date             2019-09-26
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                86.933(4)
_cell_angle_beta                 70.832(4)
_cell_angle_gamma                68.328(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1515(6)
_cell_length_b                   12.2420(7)
_cell_length_c                   16.8588(5)
_cell_measurement_reflns_used    132698
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.9991
_cell_measurement_theta_min      2.6307
_cell_volume                     2194.8(2)
_computing_cell_refinement       'REVALCCD V. 1.6, 2008'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'REVALCCD V. 1.6, 2008'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            129182
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.058
_diffrn_reflns_theta_min         3.016
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  0.84242
_exptl_absorpt_correction_T_min  0.80281
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran, acetonitrile, pentane '
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_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.939
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_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         23949
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0332P)^2^+1.0531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19400
_reflns_number_total             23949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c00562_si_004.cif
_cod_data_source_block           12658
_cod_depositor_comments
'Adding full bibliography for 4517542--4517544.cif.'
_cod_original_cell_volume        2194.84(19)
_cod_database_code               4517543
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              64268
_shelx_hkl_checksum              71116