Regioselective β-Metalation of meso-Phosphanylporphyrins. Structure and Optical Properties of Porphyrin Dimers Linked by Peripherally Fused Phosphametallacycles
Yoshihiro Matano; Kazuaki Matsumoto; Yoshihide Nakao; Hidemitsu Uno; Shigeyoshi Sakaki; Hiroshi Imahori; Journal of the American Chemical Society 130 (2008) 4588–4589; doi:10.1021/ja710542e

data_4107658
_publ_contact_author_email       uno@dpc.ehime-u.ac.jp
_publ_contact_author_fax         +81-89-927-9670
_publ_contact_author_name        'Prof Hidemitsu Uno'
_publ_contact_author_phone       +81-89-927-9660
_publ_section_title
;
 Regioselective \b-Metalation of meso-Phosphanylporphyrins. Structure and
 Optical Properties of Porphyrin Dimers Linked by Peripherally Fused
 Phosphametallacycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4588
_journal_page_last               4589
_journal_paper_doi               10.1021/ja710542e
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety
;
C120 H108 N8 O2 P2 Pd Zn2, 3(C6 H6), 2(C H4 O)
;
_chemical_formula_sum            'C140 H134 N8 O4 P2 Pd Zn2'
_chemical_formula_weight         2291.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-10-22
_audit_creation_method           'by CrystalStructure 3.8.2'
_cell_angle_alpha                97.695(8)
_cell_angle_beta                 91.885(8)
_cell_angle_gamma                98.247(9)
_cell_formula_units_Z            1
_cell_length_a                   11.030(5)
_cell_length_b                   16.207(8)
_cell_length_c                   16.613(8)
_cell_measurement_reflns_used    7439
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2909(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Mercury-8 CCD (2x2 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0840
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35979
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1198
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.638
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         13199
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1971
_reflns_number_gt                8931
_reflns_number_total             13199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710542e-file005.cif
_cod_data_source_block           '__Matsu_Pd'
_cod_original_formula_sum        'C140 H134 N8 O4 P2 Pd Zn2 '
_cod_database_code               4107658