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_4101296
_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_moiety
'2(C70 H20 F30 N7), 4(C2 H F3 O2), 6(C2 F3 O2), C Cl3, 5(O)'
_chemical_formula_sum            'C161 H44 Cl3 F90 N14 O25'
_chemical_formula_weight         4390.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.439(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.120(4)
_cell_length_b                   31.455(7)
_cell_length_c                   39.222(6)
_cell_measurement_reflns_used    9291
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.23
_cell_volume                     21642(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            180422
_diffrn_reflns_theta_full        23.23
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.9824
_exptl_absorpt_correction_T_min  0.9322
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8676
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.591
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.085
_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     2434
_refine_ls_number_reflns         30875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1645P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2326
_refine_ls_wR_factor_ref         0.2565
_reflns_number_gt                18479
_reflns_number_total             30875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061621gsi20060308_092947.cif
_cod_data_source_block           p21c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4101296