Cross-Bridging Reaction of 5,20-Diethynyl Substituted Hexaphyrins to Vinylene-Bridged Hexaphyrins
Masaaki Suzuki; Atsuhiro Osuka; Journal of the American Chemical Society 129 (2007) 464–465; doi:10.1021/ja067102v

data_4108988
_publ_section_title
;
 Cross-Bridging Reaction of 5,20-Diethynyl Substituted Hexaphyrins to
 Vinylene-Bridged Hexaphyrins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              464
_journal_page_last               465
_journal_paper_doi               10.1021/ja067102v
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C76 H58 F20 N6 Si2'
_chemical_formula_weight         1491.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.751(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.432(4)
_cell_length_b                   17.460(5)
_cell_length_c                   31.649(9)
_cell_measurement_reflns_used    21657
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      3.0
_cell_volume                     6726(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2723
_diffrn_reflns_av_sigmaI/netI    0.2353
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            52257
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         65821
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_correction_T_min  0.8967
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       prism
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         11814
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.2230
_refine_ls_R_factor_gt           0.0758
_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^)+(0.0799P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.2246
_reflns_number_gt                3967
_reflns_number_total             11814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067102vsi20061004_044022.cif
_cod_data_source_block           tips
_cod_database_code               4108988