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_7025718
_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         'C31 H28 O P Pd,(P F6), 0.5 (C6 H6)'
_chemical_formula_sum            'C34 H31 F6 O P2 Pd'
_chemical_formula_weight         737.93
_chemical_name_common            (Pd(CH2CH2COCH3)(trop))(PF6)
_chemical_name_systematic        '[Pd(CH2CH2COCH3)(trop)](PF6)'
_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             2010-04-19T18:43:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.763(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9962(5)
_cell_length_b                   8.9054(2)
_cell_length_c                   21.4435(5)
_cell_measurement_temperature    180.2(2)
_cell_volume                     3213.42(15)
_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      180.2(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Xcalibur 3, Oxford diffraction'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10409
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         32.48
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.576
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         10409
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.089
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+0.1666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                6560
_reflns_number_total             10409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002976a.txt
_cod_data_source_block           trop180k
_cod_original_cell_volume        3213.42(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7025718