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_1507691
_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
'C38 H31 B N3 O, 0.24(C6 H14), 1.53(C H2 Cl2)'
_chemical_formula_sum            'C40.94 H38.35 B Cl3.06 N3 O'
_chemical_formula_weight         707.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                99.827(2)
_cell_angle_beta                 96.5051(19)
_cell_angle_gamma                93.876(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8047(3)
_cell_length_b                   11.0075(4)
_cell_length_c                   16.8098(5)
_cell_measurement_reflns_used    37632
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      3.32
_cell_volume                     1769.06(10)
_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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16524
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         4.48
_exptl_absorpt_coefficient_mu    2.676
_exptl_absorpt_correction_T_max  0.7757
_exptl_absorpt_correction_T_min  0.5007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Higashi, T. (1995). 
 Program for Absorption Correction.
 Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         5778
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                3411
_reflns_number_total             5778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol300865s_si_002.cif
_cod_data_source_block           20128ta
_cod_database_code               1507691