Easy preparation of cobalt corrole and hexaphyrin and isolation of new oligopyrroles in the solvent-free condensation of pyrrole with pentafluorobenzaldehyde.
Simkhovich, Liliya; Goldberg, Israel; Gross, Zeev; Organic letters 5 (2003) 1241–1244; doi:10.1021/ol0341142

data_1507272
_publ_section_title
;
 Easy preparation of cobalt corrole and hexaphyrin and isolation of new
 oligopyrroles in the solvent-free condensation of pyrrole with
 pentafluorobenzaldehyde.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1241
_journal_page_last               1244
_journal_paper_doi               10.1021/ol0341142
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C44 H10 F20 N4 O2'
_chemical_formula_weight         1006.56
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.4620(16)
_cell_angle_beta                 98.3280(17)
_cell_angle_gamma                105.560(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3440(3)
_cell_length_b                   13.6840(4)
_cell_length_c                   15.2040(5)
_cell_measurement_reflns_used    4751
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      1.60
_cell_volume                     1986.61(11)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '0.8 deg. Phi & 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7299
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'parallelpiped rods'
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         7299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+6.5939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                4751
_reflns_number_total             7299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0341142si20030316_054640.cif
_cod_data_source_block           Compound-10
_cod_original_cell_volume        1986.61(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1507272