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_4108990
_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 H56 F20 N6 Si2'
_chemical_formula_weight         1489.45
_chemical_name_systematic
; 
 ? 
;
_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_method           SHELXL-97
_cell_angle_alpha                95.39(2)
_cell_angle_beta                 103.75(2)
_cell_angle_gamma                96.10(2)
_cell_formula_units_Z            1
_cell_length_a                   8.390(5)
_cell_length_b                   13.865(9)
_cell_length_c                   15.169(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1691.3(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16131
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         7727
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       prism
_exptl_crystal_F_000             762
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+0.6226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2220
_reflns_number_gt                4904
_reflns_number_total             7507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067102vsi20061213_025143.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1691.2(17)
_cod_database_code               4108990