Porphyrin synthesis in water provides new expanded porphyrins with direct bipyrrole linkages: isolation and characterization of two heptaphyrins.
Hiroto, Satoru; Shinokubo, Hiroshi; Osuka, Atsuhiro; Journal of the American Chemical Society 128 (2006) 6568–6569; doi:10.1021/ja061621g

data_4101297
_publ_section_title
;
 Porphyrin synthesis in water provides new expanded porphyrins with
 direct bipyrrole linkages: isolation and characterization of two
 heptaphyrins.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6568
_journal_page_last               6569
_journal_paper_doi               10.1021/ja061621g
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C99 H31 Cl3 F35 N8'
_chemical_formula_weight         2101.65
_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                101.478(13)
_cell_angle_beta                 95.064(15)
_cell_angle_gamma                107.334(15)
_cell_formula_units_Z            2
_cell_length_a                   11.921(5)
_cell_length_b                   13.300(5)
_cell_length_c                   29.176(10)
_cell_measurement_temperature    123(2)
_cell_volume                     4273(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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            41061
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.9928
_exptl_absorpt_correction_T_min  0.8890
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2090
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1296
_refine_ls_number_reflns         19112
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0802
_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^)+(0.0752P)^2^+9.6463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2393
_reflns_number_gt                11358
_reflns_number_total             19112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061621gsi20060417_033125.cif
_cod_data_source_block           shelxl
_cod_database_code               4101297