A Triphenylene-Based Triptycene with Large Free Volume Synthesized by Zirconium-Mediated Biphenylation
Cameron L. Hilton; Christopher R. Jamison; Hannah K. Zane; Benjamin T. King; Journal of Organic Chemistry 74 (2009) 405–407; doi:10.1021/jo801643u

data_4024214
_publ_section_title
;
A Triphenylene-Based Triptycene with Large Free Volume Synthesized by
Zirconium-Mediated Biphenylation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              405
_journal_page_last               407
_journal_paper_doi               10.1021/jo801643u
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C20 H8 Br6'
_chemical_formula_weight         727.72
_chemical_name_systematic
; 
 2,3,6,7,12,13-hexabromotriptycene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 117.43
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4178(8)
_cell_length_b                   9.5733(5)
_cell_length_c                   15.4178(8)
_cell_measurement_temperature    100(2)
_cell_volume                     2019.72(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36025
_diffrn_reflns_theta_full        32.91
_diffrn_reflns_theta_max         32.91
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    11.929
_exptl_absorpt_correction_T_max  0.5156
_exptl_absorpt_correction_T_min  0.2840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+1.2947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                5234
_reflns_number_total             7285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo801643u_si_006.cif
_cod_data_source_block           ch226_0ma
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4024214