Synthetic Routes to 5,10,15-Triaryl-tetrabenzocorroles
Giuseppe Pomarico; Sara Nardis; Roberto Paolesse; Owendi C. Ongayi; Brandy H. Courtney; Frank R. Fronczek; Maria Graça H. Vicente; Journal of Organic Chemistry 76 (2011) 3765–3773; doi:10.1021/jo200026u

data_4026279
_publ_section_title
;
 Synthetic Routes to 5,10,15-Triaryl-tetrabenzocorroles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3765
_journal_page_last               3773
_journal_paper_doi               10.1021/jo200026u
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C57 H29 Cu N7'
_chemical_formula_sum            'C57 H29 Cu N7'
_chemical_formula_weight         875.42
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.471(4)
_cell_angle_beta                 68.114(4)
_cell_angle_gamma                75.445(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9578(7)
_cell_length_b                   13.0892(6)
_cell_length_c                   15.4144(8)
_cell_measurement_reflns_used    2657
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      51.30
_cell_measurement_theta_min      3.24
_cell_volume                     2064.1(2)
_computing_cell_refinement       'Bruker (2006) Apex-II '
_computing_data_collection       'Bruker (2006) Apex-II'
_computing_data_reduction        'Bruker (2006) Apex-II '
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20113
_diffrn_reflns_theta_full        57.02
_diffrn_reflns_theta_max         57.0
_diffrn_reflns_theta_min         3.2
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Contribution from 46 electrons per cell were removed from the
observed structure factors for refinement.
;
_refine_diff_density_max         0.992
_refine_diff_density_min         -1.811
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         5503
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0937
_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^)+(0.1788P)^2^+4.2914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2665
_refine_ls_wR_factor_ref         0.2895
_reflns_number_gt                3852
_reflns_number_total             5503
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo200026u_si_003.cif
_cod_data_source_block           Compound4
_cod_original_cell_volume        2064.15(19)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4026279