Silica-Supported Triptycene-Type Phosphine. Synthesis, Characterization, and Application to Pd-Catalyzed Suzuki‒Miyaura Cross-Coupling of Chloroarenes
Iwai, Tomohiro; Konishi, Shota; Miyazaki, Tatsuya; Kawamorita, Soichiro; Yokokawa, Natsumi; Ohmiya, Hirohisa; Sawamura, Masaya; ACS Catalysis 5 (2015) 7254–; doi:10.1021/acscatal.5b00904

data_4516661
_publ_section_title
;
 Silica-Supported Triptycene-Type Phosphine. Synthesis, Characterization,
 and Application to Pd-Catalyzed Suzuki--Miyaura Cross-Coupling of
 Chloroarenes
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              7254
_journal_paper_doi               10.1021/acscatal.5b00904
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C55 H40 Cl3 O3 P3 Si3'
_chemical_formula_sum            'C55 H40 Cl3 O3 P3 Si3'
_chemical_formula_weight         1032.46
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            4
_cell_length_a                   15.5297(5)
_cell_length_b                   15.5297(5)
_cell_length_c                   24.1564(11)
_cell_measurement_reflns_used    12145
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     5045.3(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 1.028
_diffrn_measured_fraction_theta_max 1.028
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39823
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3860
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0398P)^2^+2.8552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                3339
_reflns_number_total             3860
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            cs5b00904_si_001.cif
_cod_data_source_block           silanol_3
_cod_original_cell_volume        5045.3(4)
_cod_database_code               4516661