A facile synthesis of trinaphtho[3.3.3]propellane and its pi-extension and the formation of a two-dimensional honeycomb molecular assembly
Takashi Kubo; Shogo Miyazaki; Takuya Kodama; Mitsuya Aoba; Yasukazu Hirao; Hiroyuki Kurata; Chem.Commun. 51 (2015) 3801–; doi:10.1039/C4cc09883H

data_7116584
_publ_section_title
;
 A facile synthesis of trinaphtho[3.3.3]propellane and its pi-extension
 and the formation of a two-dimensional honeycomb molecular assembly
;
_journal_name_full               Chem.Commun.
_journal_page_first              3801
_journal_paper_doi               10.1039/C4cc09883H
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C50 H24, 1.5(C12 H4 N4), C6 H5 Cl'
_chemical_formula_sum            'C74 H35 Cl N6'
_chemical_formula_weight         1043.53
_chemical_name_systematic        FAP-TCNQ
_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
_audit_update_record
;
2014-12-04 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                109.2553(9)
_cell_angle_beta                 90.5719(11)
_cell_angle_gamma                109.4063(8)
_cell_formula_units_Z            2
_cell_length_a                   10.6327(3)
_cell_length_b                   14.0819(4)
_cell_length_c                   19.8579(8)
_cell_measurement_reflns_used    15975
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      54.96
_cell_measurement_theta_min      6.09
_cell_volume                     2623.52(15)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26103
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1076
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chlorobenzene'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         11925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0838P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                6932
_reflns_number_total             11925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc09883h2.cif
_cod_data_source_block           xsm3x28
_cod_database_code               7116584