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_4026278
_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_compound_source        'local laboratory'
_chemical_formula_moiety         'C53 H31 Cu N4, 0.47(C H Cl3)'
_chemical_formula_sum            'C53.47 H31.47 Cl1.4 Cu N4'
_chemical_formula_weight         843.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
_cell_angle_beta                 130.67(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   35.073(13)
_cell_length_b                   18.943(9)
_cell_length_c                   23.102(11)
_cell_measurement_reflns_used    8858
_cell_measurement_temperature    110.0(5)
_cell_measurement_theta_max      23.534
_cell_measurement_theta_min      2.546
_cell_volume                     11642(10)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare  et al., 1999)'
_diffrn_ambient_temperature      110.0(5)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_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  0.3028
_diffrn_reflns_av_sigmaI/netI    0.3786
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73637
_diffrn_reflns_theta_full        23.58
_diffrn_reflns_theta_max         23.58
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       needle
_exptl_crystal_F_000             5197
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.3463
_refine_ls_R_factor_gt           0.1339
_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^)+(0.1270P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2609
_refine_ls_wR_factor_ref         0.3433
_reflns_number_gt                2676
_reflns_number_total             8643
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo200026u_si_002.cif
_cod_data_source_block           Compound3a
_cod_original_cell_volume        11642(9)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C53.47 H31.47 Cl1.40 Cu N4'
_cod_database_code               4026278