Rational Synthesis of A(2)B-type meso-Triarylsubporphyrins.
Tanaka, Takayuki; Kitano, Masaaki; Hayashi, Shin-Ya; Aratani, Naoki; Osuka, Atsuhiro; Organic letters 14 (2012) 2694–2697; doi:10.1021/ol300865s

data_1507693
_publ_section_title
;
 Rational Synthesis of A(2)B-type meso-Triarylsubporphyrins.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2694
_journal_page_last               2697
_journal_paper_doi               10.1021/ol300865s
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C32 H22 B N3 O S'
_chemical_formula_sum            'C32 H22 B N3 O S'
_chemical_formula_weight         507.40
_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                 110.5139(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4058(4)
_cell_length_b                   13.7067(4)
_cell_length_c                   14.2504(4)
_cell_measurement_reflns_used    14530
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      3.23
_cell_volume                     2452.45(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21533
_diffrn_reflns_theta_full        66.00
_diffrn_reflns_theta_max         66.00
_diffrn_reflns_theta_min         4.78
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.8708
_exptl_absorpt_correction_T_min  0.7639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Higashi, T. (1995). 
 Program for Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         4262
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.173
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1583P)^2^+0.1101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.2857
_reflns_number_gt                2465
_reflns_number_total             4262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol300865s_si_004.cif
_cod_data_source_block           20212ta2
_cod_original_cell_volume        2452.45(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1507693