Synthesis of Hexa(furan-2-yl)benzenes and Their π-Extended Derivatives
Koichi Mitsudo; Jyunji Harada; Yo Tanaka; Hiroki Mandai; Chie Nishioka; Hideo Tanaka; Atsushi Wakamiya; Yasujiro Murata; Seiji Suga; Journal of Organic Chemistry 78 (2013) 2763–2768; doi:10.1021/jo302652r

data_4028037
_publ_contact_author_address
;
Graduate School of Natural Science and Technology, Okayama University,
3-1-1 Tsushima-naka, Okayama 700-8530, Japan
;
_publ_contact_author_email       suga@cc.okayama-u.ac.jp
_publ_contact_author_fax         +81-86-251-8081
_publ_contact_author_name        'Seiji Suga'
_publ_contact_author_phone       +81-86-251-8081
_publ_section_title
;
 Synthesis of Hexa(furan-2-yl)benzenes and Their \p-Extended Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2763
_journal_page_last               2768
_journal_paper_doi               10.1021/jo302652r
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C66 H84 B6 O18, 2(C7 H8)'
_chemical_formula_sum            'C80 H100 B6 O18'
_chemical_formula_weight         1414.46
_chemical_name_common            Hexakis(5-Bpinfuran-2-yl)benzene
_chemical_name_systematic
;
 Hexakis[5-(4,4,5,5-tetramethyl-1,3,2-dioxaboryl)-2-furyl]benzene
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.951(2)
_cell_length_b                   25.304(3)
_cell_length_c                   19.179(3)
_cell_measurement_reflns_used    20526
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.08
_cell_volume                     8226.4(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            126649
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       Block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9419
_refine_ls_number_restraints     794
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1026P)^2^+3.9746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                8772
_reflns_number_total             9419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo302652r_si_002_5.cif
_cod_data_source_block           2c
_cod_original_cell_volume        8226.2(19)
_cod_database_code               4028037