meso-Aryl-Substituted Subporphyrins: Synthesis, Structures, and Large Substituent Effects on Their Electronic Properties
Yasuhide Inokuma; Zin Seok Yoon; Dongho Kim; Atsuhiro Osuka; Journal of the American Chemical Society 129 (2007) 4747–4761; doi:10.1021/ja069324z

data_4109308
_publ_section_title
;
 meso-Aryl-Substituted Subporphyrins: Synthesis, Structures, and Large
 Substituent Effects on Their Electronic Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4747
_journal_page_last               4761
_journal_paper_doi               10.1021/ja069324z
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '4(C34 H21 B N6 O7), 3(C H Cl3)'
_chemical_formula_sum            'C139 H87 B4 Cl9 N24 O28'
_chemical_formula_weight         2903.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                79.2060(10)
_cell_angle_beta                 81.2920(10)
_cell_angle_gamma                73.630(2)
_cell_formula_units_Z            1
_cell_length_a                   14.2905(11)
_cell_length_b                   14.3984(12)
_cell_length_c                   16.4038(13)
_cell_measurement_reflns_used    7569
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.37
_cell_volume                     3163.7(4)
_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 0.888
_diffrn_measured_fraction_theta_max 0.888
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20046
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.9054
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       prism
_exptl_crystal_F_000             1486
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1886
_refine_ls_number_reflns         16516
_refine_ls_number_restraints     1413
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+2.4886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                13756
_reflns_number_total             16516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069324zsi20061228_021904.cif
_cod_data_source_block           s4_no2n
_cod_database_code               4109308