Synthesis and Catalytic Applications of a Triptycene-Based Monophosphine Ligand for Palladium-Mediated Organic Transformations.
Leung, Franco King-Chi; Ishiwari, Fumitaka; Shoji, Yoshiaki; Nishikawa, Tsuyoshi; Takeda, Ryohei; Nagata, Yuuya; Suginome, Michinori; Uozumi, Yasuhiro; Yamada, Yoichi M. A.; Fukushima, Takanori; ACS omega 2 (2017) 1930–1937; doi:10.1021/acsomega.7b00200

data_4516863
_publ_section_title
;
 Synthesis and Catalytic Applications of a Triptycene-Based Monophosphine
 Ligand for Palladium-Mediated Organic Transformations.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              1930
_journal_page_last               1937
_journal_paper_doi               10.1021/acsomega.7b00200
_journal_volume                  2
_journal_year                    2017
_chemical_formula_sum            'C71 H62 Br4 Cl2 O3 P2 Pd2'
_chemical_formula_weight         1628.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 97.6850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3561(9)
_cell_length_b                   21.5867(16)
_cell_length_c                   25.9119(19)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.34
_cell_volume                     6849.3(9)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHELL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            65548
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.974
_diffrn_reflns_theta_min         1.232
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_T_max  0.569
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.210
_refine_diff_density_max         1.409
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         12025
_refine_ls_number_restraints     1176
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+28.0917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10646
_reflns_number_total             12025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00200_si_002.cif
_cod_data_source_block           PdBr2-1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4516863
_shelx_estimated_absorpt_t_min   0.363
_shelx_estimated_absorpt_t_max   0.569
_shelxl_version_number           2014/6
_shelx_res_checksum              73094
_shelx_hkl_checksum              96078