Structurally characterized intermediates in the stepwise insertion of CO-ethylene or CO-methyl acrylate into the metal-carbon bond of Pd(II) complexes stabilized by (phosphinomethyl)oxazoline ligands.
Agostinho, Magno; Braunstein, Pierre; Chemical communications (Cambridge, England)  (2007) 58–60; doi:10.1039/b613865a

data_7101622
_publ_section_title
;
 Structurally characterized intermediates in the stepwise insertion of
 CO-ethylene or CO-methyl acrylate into the metal-carbon bond of Pd(II)
 complexes stabilized by (phosphinomethyl)oxazoline ligands.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              58
_journal_page_last               60
_journal_paper_doi               10.1039/b613865a
_journal_year                    2007
_chemical_formula_moiety         'C19 H23 N O P Pd, C F3 S O3'
_chemical_formula_sum            'C20 H23 F3 N O4 P Pd S'
_chemical_formula_weight         567.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             22-1-05
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.55(5)
_cell_angle_beta                 100.18(5)
_cell_angle_gamma                98.93(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3330(10)
_cell_length_b                   9.827(2)
_cell_length_c                   14.261(3)
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1132.4(4)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8568
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0175P)^2^+0.5690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                5724
_reflns_number_total             6592
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b613865a.txt
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101622