Inner C-arylation of a doubly N-confused porphyrin‒Pd complex in toluene—the possibility of a Pd3+ intermediate
Furuta, Hiroyuki; Maeda, Hiromitsu; Osuka, Atsuhiro; Yasutake, Mikio; Shinmyozu, Teruo; Ishikawa, Yuichi; Chemical Communications  (2000) 1143–; doi:10.1039/b003022h

data_7110974
_publ_section_title
;
 Inner C-arylation of a doubly N-confused porphyrin--Pd complex in
 toluene---the possibility of a Pd3+ intermediate
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1143
_journal_paper_doi               10.1039/b003022h
_journal_year                    2000
_chemical_formula_sum            'C56 H25.6 F20 N4 O1.3 Pd'
_chemical_formula_weight         1261.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 118.743(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.780(1)
_cell_length_b                   22.179(2)
_cell_length_c                   15.618(1)
_cell_measurement_reflns_used    15405
_cell_measurement_temperature    93.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     4792.6(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ?w
_diffrn_radiation_type           'Mo K??'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.230
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37233
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.85
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^?l^3^/sin(2?q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     752
_refine_ls_number_reflns         3178
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          -0.0710
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[?s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2475
_reflns_number_gt                3178
_reflns_number_total             17002
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b003022hsup1.cif
_cod_data_source_block           yasu40
_cod_original_cell_volume        4792.5(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C56 H25.6 F20 N4 O1.30 Pd '
_cod_database_code               7110974