Limits of Activity: Weakly Coordinating Ligands in Arylphosphinesulfonato Palladium(II) Polymerization Catalysts
Neuwald, Boris; Ölscher, Franz; Göttker-Schnetmann, Inigo; Mecking, Stefan; Organometallics 31 (2012) 3128–; doi:10.1021/om3000339

data_4078013
_publ_section_title
;
 Limits of Activity: Weakly Coordinating Ligands in Arylphosphinesulfonato
 Palladium(II) Polymerization Catalysts
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3128
_journal_paper_doi               10.1021/om3000339
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C22 H25 O6 P Pd S, C H4 O'
_chemical_formula_sum            'C23 H29 O7 P Pd S'
_chemical_formula_weight         586.89
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.681(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4001(6)
_cell_length_b                   14.0634(6)
_cell_length_c                   15.5159(9)
_cell_measurement_reflns_used    38099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      1.96
_cell_volume                     2482.4(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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43129
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  0.8529
_exptl_absorpt_correction_T_min  0.7059
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED 32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+2.8492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                5598
_reflns_number_total             6310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3000339_si_002.cif
_cod_data_source_block           gs09_01
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4078013