A Brønsted acid-catalyzed generation of palladium complexes: efficient head-to-tail dimerization of alkynes
Chen, Tieqiao; Guo, Cancheng; Goto, Midori; Han, Li-Biao; Chemical Communications (Cambridge, United Kingdom) 49 (2013) 7498–7500; doi:10.1039/c3cc43131b

data_7109793
_publ_section_title
;
 A Br\/onsted acid-catalyzed generation of palladium complexes:
 efficient head-to-tail dimerization of alkynes
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   68
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              7498
_journal_page_last               7500
_journal_paper_doi               10.1039/c3cc43131b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C30 H46 O2 P2 Pd'
_chemical_formula_weight         607.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.6760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7501(14)
_cell_length_b                   14.1473(17)
_cell_length_c                   18.600(2)
_cell_measurement_reflns_used    8021
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.28
_cell_volume                     3027.9(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayerd confocal mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23648
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_correction_T_min  0.8965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+2.2121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                3772
_reflns_number_total             5280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hanchenPd.txt
_cod_data_source_block           hanchenpd
_cod_original_cell_volume        3028.0(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7109793