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_4108989
_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            'C78 H30 Cl2 F20 N6 O6 Zn2'
_chemical_formula_weight         1728.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.290(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.0582(18)
_cell_length_b                   15.5874(17)
_cell_length_c                   14.5782(16)
_cell_measurement_reflns_used    8514
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      2.38
_cell_volume                     3835.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36674
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       prism
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.976
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         13526
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0912
_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^)+(0.1779P)^2^+11.4008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2555
_refine_ls_wR_factor_ref         0.2920
_reflns_number_gt                9598
_reflns_number_total             13526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067102vsi20061004_044043.cif
_cod_data_source_block           ph_zn21
_cod_database_code               4108989