Chemoselective methoxycarbonylation of terminal alkynes catalyzed by Pd(II)-TROPP complexes.
Bettucci, Lorenzo; Bianchini, Claudio; Oberhauser, Werner; Vogt, Matthias; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 39 (2010) 6509–6517; doi:10.1039/c002976a

data_7025719
_publ_section_title
;
 Chemoselective methoxycarbonylation of terminal alkynes catalyzed by
 Pd(II)-TROPP complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6509
_journal_page_last               6517
_journal_paper_doi               10.1039/c002976a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C27 H24 Cl P Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C28.5 H25 Cl2 P Pd'
_chemical_formula_weight         575.76
_chemical_name_common            (PdClMe(trop))
_chemical_name_systematic        '[PdClMe(trop)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-04-20T15:12:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.175(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.907(5)
_cell_length_b                   19.718(5)
_cell_length_c                   15.161(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2660.8(19)
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (J. Appl. Cryst. 1999, 32, 115)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.125
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4654
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.48
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1759
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.2076
_reflns_number_gt                2463
_reflns_number_total             4654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002976a.txt
_cod_data_source_block           tropos
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C28.50 H25 Cl2 P Pd'
_cod_database_code               7025719