Highly Regioselective Addition and Dehydrogenative Cross-Coupling of H-Heteroatoms with Alkynes Using An Unconventional Palladacycle Catalyst
Qing Xu.; Ruwei Shen.; Yutaka Ono.; Ritsuko Nagahata; Shigeru Shimada; Midori Goto; Li-Biao Han; Chem.Commun. 47 (2011) 2333–; doi:10.1039/c0cc03436c

data_7105987
_publ_section_title
;
 Highly Regioselective Addition and Dehydrogenative Cross-Coupling of
 H-Heteroatoms with Alkynes Using An Unconventional Palladacycle Catalyst
;
_journal_name_full               Chem.Commun.
_journal_page_first              2333
_journal_paper_doi               10.1039/c0cc03436c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C72 H54 O12 P6 Pd6'
_chemical_formula_sum            'C72 H54 O12 P6 Pd6'
_chemical_formula_weight         1935.45
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-11-10
_audit_creation_method           'by CrystalStructure 4.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   20.7526(17)
_cell_length_b                   17.8092(14)
_cell_length_c                   18.6170(15)
_cell_measurement_reflns_used    5330
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.19
_cell_volume                     6880.6(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean '8.366 [pixels/mm]'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45474
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.738
_exptl_absorpt_correction_T_max  0.8736
_exptl_absorpt_correction_T_min  0.8187
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3792.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.130
_refine_diff_density_min         -1.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     24
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0250P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                5818
_reflns_number_total             8562
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            C0CC03436C.TXT
_cod_data_source_block           General
_cod_database_code               7105987