An efficient and recyclable dendritic catalyst able to dramatically decrease palladium leaching in Suzuki couplings
Keller, Michel; Hameau, Aurélien; Spataro, Grégory; Ladeira, Sonia; Caminade, Anne-Marie; Majoral, Jean-Pierre; Ouali, Armelle; Green Chemistry 14 (2012) 2807–; doi:10.1039/c2gc35832h

data_7215078
_publ_section_title
;
 An efficient and recyclable dendritic catalyst able to dramatically
 decrease palladium leaching in Suzuki couplings
;
_journal_issue                   10
_journal_name_full               'Green Chemistry'
_journal_page_first              2807
_journal_paper_doi               10.1039/c2gc35832h
_journal_volume                  14
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H28 N3 O2 P S'
_chemical_formula_sum            'C27 H28 N3 O2 P S'
_chemical_formula_weight         489.55
_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
_cell_angle_alpha                90
_cell_angle_beta                 101.967(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7499(4)
_cell_length_b                   30.5632(13)
_cell_length_c                   8.5329(3)
_cell_measurement_reflns_used    7578
_cell_measurement_temperature    180
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.24
_cell_measurement_wavelength     0.71073
_cell_volume                     2487.44(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            33236
_diffrn_reflns_theta_full        28.8
_diffrn_reflns_theta_max         28.8
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.7676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                4844
_reflns_number_total             6476
_reflns_threshold_expression     >2/sigma(I)
_cod_data_source_file            c2gc35832h.txt
_cod_data_source_block           5-OH
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7215078