X-ray structural characterization of charge delocalization onto the three equivalent benzenoid rings in hexamethoxytriptycene cation radical.
Chebny, Vincent J.; Navale, Tushar S.; Shukla, Ruchi; Lindeman, Sergey V.; Rathore, Rajendra; Organic letters 11 (2009) 2253–2256; doi:10.1021/ol900558s

data_1503891
_publ_section_title
;
 X-ray structural characterization of charge delocalization onto the three
 equivalent benzenoid rings in hexamethoxytriptycene cation radical.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2253
_journal_page_last               2256
_journal_paper_doi               10.1021/ol900558s
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C40.25 H44 Cl6 O6 Sb'
_chemical_formula_weight         958.20
_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                103.8740(10)
_cell_angle_beta                 93.9200(10)
_cell_angle_gamma                90.6470(10)
_cell_formula_units_Z            4
_cell_length_a                   12.5195(2)
_cell_length_b                   12.9701(2)
_cell_length_c                   26.6144(4)
_cell_measurement_reflns_used    8753
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      3
_cell_volume                     4184.02(11)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34690
_diffrn_reflns_theta_full        62.46
_diffrn_reflns_theta_max         62.46
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    9.122
_exptl_absorpt_correction_T_max  0.7408
_exptl_absorpt_correction_T_min  0.2388
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical (based on real shape of the crystal) absorption
 correction followed by:
 SADABS. Program for empirical absorption correction of
 area-detector data. University of Goetingen. Germany. 
 Sheldrick, G. M. 1996
;
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1946
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         12243
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0445P)^2^+6.0254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                9589
_reflns_number_total             12243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol900558s_si_003.cif
_cod_data_source_block           raj5za
_cod_database_code               1503891