Octaphenylbiphenylene and Dodecaphenyltriptycene
Jun Lu; Jiajia Zhang; Xianfeng Shen; Douglas M. Ho; Robert A. Pascal; Journal of the American Chemical Society 124 (2002) 8035–8041; doi:10.1021/ja0203723

data_4114937
_publ_section_title
;
 Octaphenylbiphenylene and Dodecaphenyltriptycene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8035
_journal_page_last               8041
_journal_paper_doi               10.1021/ja0203723
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C92 H62'
_chemical_formula_structural     'C92 H62 . C H2 Cl2'
_chemical_formula_sum            'C93 H64 Cl2'
_chemical_formula_weight         1252.34
_chemical_name_systematic
; 
 1,2,3,4,5,6,7,8,13,14,15,16-Dodecaphenyltriptycene 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 125.4847(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2738(4)
_cell_length_b                   28.5548(5)
_cell_length_c                   32.3310(5)
_cell_measurement_reflns_used    82861
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      1.27
_cell_volume                     14488.9(5)
_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  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method
'omega scans; 800 0.5-degree frames; 480 sec/deg'
_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  0.071
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            82861
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.794
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.172
_refine_ls_hydrogen_treatment    'XYZ riding, U(H) = 1.2U(C)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1730
_refine_ls_number_reflns         18933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.172
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_obs          0.0753
_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^)+(0.1364P)^2^+7.6582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2266
_refine_ls_wR_factor_obs         0.2071
_reflns_number_observed          12780
_reflns_number_total             18933
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0203723_3.cif
_cod_data_source_block           84sq2tf
_cod_depositor_comments
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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^)+(0.1364P)^2^+7.6582P] 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^)+(0.1364P)^2^+7.6582P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4114937