Carbopalladation of Maleate and Fumarate Esters and 1,1-Dimethylallene with Ortho-Substituted Aryl Palladium Complexes
Vicente, José; Abad, José Antonio; López-Sáez, María-José; Jones, Peter G.; Organometallics 29 (2010) 409–; doi:10.1021/om900957s

data_4063456
_publ_section_title
;
 Carbopalladation of Maleate and Fumarate Esters and 1,1-Dimethylallene
 with Ortho-Substituted Aryl Palladium Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              409
_journal_paper_doi               10.1021/om900957s
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C18 H29 F3 N2 O4 Pd S'
_chemical_formula_weight         532.89
_chemical_name_systematic
;

 ?

;
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.713(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4184(6)
_cell_length_b                   17.7346(11)
_cell_length_c                   15.4582(11)
_cell_measurement_reflns_used    7509
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.37
_cell_measurement_theta_min      2.30
_cell_volume                     2221.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43612
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.226
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment
'OH and allyl CH2 free, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         6758
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0567P)^2^+1.5373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                5321
_reflns_number_total             6758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900957s_si_002.cif
_cod_data_source_block           alley
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4063456