The Structure of Hexabenzotriphenylene and the Problem of Overcrowded "D3h" Polycyclic Aromatic Compounds
Lisa Barnett; Douglas M. Ho; Kim K. Baldridge; Robert A. Pascal; Journal of the American Chemical Society 121 (1999) 727–733; doi:10.1021/ja983471i

data_4116293
_publ_section_title
;
 The Structure of Hexabenzotriphenylene and the Problem of Overcrowded
 "D3h" Polycyclic Aromatic Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              727
_journal_page_last               733
_journal_paper_doi               10.1021/ja983471i
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C42 H24'
_chemical_formula_structural     'C42 H24'
_chemical_formula_sum            'C42 H24'
_chemical_formula_weight         528.61
_chemical_melting_point_gt       623
_chemical_name_common            Hexabenzotriphenylene
_chemical_name_systematic
; 
 Dibenzo[f,j]phenanthro[9,10-s]picene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.013(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9721(5)
_cell_length_b                   7.0005(1)
_cell_length_c                   19.5456(5)
_cell_measurement_reflns_used    45305
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.10
_cell_volume                     2651.44(10)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method
'oscillations; 651 deg data in 1 deg increments'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45305
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.013
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    'xyz refined, isotropic'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6016
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_obs          0.0512
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.4023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1327
_refine_ls_wR_factor_obs         0.1091
_reflns_number_observed          3652
_reflns_number_total             6016
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja983471i_1.cif
_cod_data_source_block           rap002f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.4023P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.4023P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2651.4(1)
_cod_database_code               4116293