Donors and Acceptors Based on Triangular Dehydrobenzo[12]annulenes: Formation of a Triple-Layered Rosette Structure by a Charge-Transfer Complex
Kazukuni Tahara; Takumi Fujita; Motohiro Sonoda; Motoo Shiro; Yoshito Tobe; Journal of the American Chemical Society 130 (2008) 14339–14345; doi:10.1021/ja804604y

data_4108545
_publ_section_title
;
 Donors and Acceptors Based on Triangular Dehydrobenzo[12]annulenes:
 Formation of a Triple-Layered Rosette Structure by a Charge-Transfer
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14339
_journal_page_last               14345
_journal_paper_doi               10.1021/ja804604y
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         '3(C30 H27 N3), 3(C24 F12), 2(C H Cl3)'
_chemical_formula_sum            'C164 H83 Cl6 F36 N9'
_chemical_formula_weight         3076.18
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 119.7139(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   19.6903(4)
_cell_length_b                   19.7776(5)
_cell_length_c                   19.8704(5)
_cell_measurement_reflns_used    21522
_cell_measurement_temperature    110.1
_cell_measurement_theta_max      68.1
_cell_measurement_theta_min      4.5
_cell_volume                     6720.6(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla, 2005)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            95957
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_exptl_absorpt_coefficient_mu    2.135
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.784
_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    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             3112.00
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.78
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  11116 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.012(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1950
_refine_ls_number_reflns         23651
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0957P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                15879
_reflns_number_total             23651
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja804604y_si_004.cif
_cod_data_source_block           '_DBAcocrystal'
_cod_original_formula_sum        'C164 H83 Cl6 F36 N9 '
_cod_database_code               4108545