Activation and Deactivation of Neutral Palladium(II) Phosphinesulfonato Polymerization Catalysts
R Thomas; Tritschler, Ulrich; Roesle, Philipp; Göttker-Schnetmann, Inigo; Müller, Heiko M.; Caporaso, Lucia; Poater, Albert; Cavallo, Luigi; Mecking, Stefan; Organometallics 31 (2012) 8388–; doi:10.1021/om300969d

data_4079702
_publ_section_title
;
 Activation and Deactivation of Neutral Palladium(II) Phosphinesulfonato
 Polymerization Catalysts
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8388
_journal_paper_doi               10.1021/om300969d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C34 H32 O9 P2 Pd S2'
_chemical_formula_sum            'C34 H32 O9 P2 Pd S2'
_chemical_formula_weight         817.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.902(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1796(11)
_cell_length_b                   15.5480(9)
_cell_length_c                   21.1054(19)
_cell_measurement_reflns_used    31980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      1.70
_cell_volume                     3532.1(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38911
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.8389
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
;
_refine_diff_density_max         1.401
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0443P)^2^+11.3547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                5489
_reflns_number_total             6667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300969d_si_002.cif
_cod_data_source_block           f:\\gs12_005
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4079702