Single-wing Extended Tribenzotriquinacenes via Bowl-shaped Dehydrobenzene and Isobenzofuran Tribenzotriquinacene Derivatives
Wen-Xue Niu; Er-Qun Yang; Zi-Fa Shi; Xiao-Ping Cao; Dietmar Kuck; Journal of Organic Chemistry 77 (2012) 1422–1434; doi:10.1021/jo2022668

data_4026926
_publ_section_title
;
 Single-wing Extended Tribenzotriquinacenes via Bowl-shaped Dehydrobenzene
 and Isobenzofuran Tribenzotriquinacene Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1422
_journal_page_last               1434
_journal_paper_doi               10.1021/jo2022668
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C50 H44 O2'
_chemical_formula_weight         676.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                106.815(13)
_cell_angle_beta                 100.455(13)
_cell_angle_gamma                97.499(12)
_cell_formula_units_Z            2
_cell_length_a                   11.063(3)
_cell_length_b                   11.841(3)
_cell_length_c                   15.632(4)
_cell_measurement_reflns_used    2028
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.07
_cell_measurement_theta_min      2.37
_cell_volume                     1890.9(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9404
_diffrn_reflns_theta_full        24.60
_diffrn_reflns_theta_max         24.60
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9895
_exptl_absorpt_correction_T_min  0.9833
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0043(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6252
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0629
_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^)+(0.1000P)^2^+0.8738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.2039
_reflns_number_gt                3702
_reflns_number_total             6252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2022668_si_003.cif
_cod_data_source_block           niuwenxuehuang_0m
_cod_original_cell_volume        1890.8(8)
_cod_database_code               4026926