Controlled Acrylate Insertion Regioselectivity in Diazaphospholidine-Sulfonato Palladium(II) Complexes
Wucher, Philipp; Roesle, Philipp; Falivene, Laura; Cavallo, Luigi; Caporaso, Lucia; Göttker-Schnetmann, Inigo; Mecking, Stefan; Organometallics 31 (2012) 8505–; doi:10.1021/om300755j

data_4079458
_publ_section_title
;
 Controlled Acrylate Insertion Regioselectivity in
 Diazaphospholidine-Sulfonato Palladium(II) Complexes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              8505
_journal_paper_doi               10.1021/om300755j
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C38 H50 N3 O3 P Pd S'
_chemical_formula_sum            'C38 H50 N3 O3 P Pd S'
_chemical_formula_weight         766.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.484(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9735(7)
_cell_length_b                   11.2607(3)
_cell_length_c                   18.2288(7)
_cell_measurement_reflns_used    69967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.13
_cell_volume                     3678.1(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation  method'
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60659
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.8898
_exptl_absorpt_correction_T_min  0.8280
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.917
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0461
_reflns_number_gt                7758
_reflns_number_total             8802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300755j_si_002.cif
_cod_data_source_block           g:\x_ray\gs08_011
_cod_original_sg_symbol_Hall     'P 2yn'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4079458