A Facile One-Pot Synthesis of meso-Aryl-Substituted [14]Triphyrin(2.1.1)
Zhao-Li Xue; Zhen Shen; John Mack; Daiki Kuzuhara; Hiroko Yamada; Tetsuo Okujima; Noboru Ono; Xiao-Zeng You; Nagao Kobayashi; Journal of the American Chemical Society 130 (2008) 16478–16479; doi:10.1021/ja8068769

data_4108796
_publ_section_title
;
 A Facile One-Pot Synthesis of meso-Aryl-Substituted [14]Triphyrin(2.1.1)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16478
_journal_page_last               16479
_journal_paper_doi               10.1021/ja8068769
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '2(C52 H33 N3), H2 O'
_chemical_formula_sum            'C104 H68 N6 O'
_chemical_formula_weight         1417.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                76.727(2)
_cell_angle_beta                 83.313(4)
_cell_angle_gamma                76.375(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5097(7)
_cell_length_b                   13.7167(9)
_cell_length_c                   27.347(2)
_cell_measurement_reflns_used    7500
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      3.04
_cell_volume                     3720.9(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29152
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         14144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.06P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                10653
_reflns_number_total             14144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8068769_si_001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4108796