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_4114935
_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         'C60 H44 . 2 C60 H38 . C H2 Cl2'
_chemical_formula_structural     'C60 H44 . 2 C60 H38 . C H2 Cl2'
_chemical_formula_sum            'C181 H122 Cl2'
_chemical_formula_weight         2367.69
_chemical_name_systematic
; 
 1:2:1 2,3,5,6,7,8-hexaphenyl-1,4-di(o-tolyl)naphthalene : 1,2,3,8,9,10-
 hexaphenyldibenzo[fg,op]naphthacene : dichloromethane complex 
;
_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
_cell_angle_alpha                75.587(2)
_cell_angle_beta                 67.113(3)
_cell_angle_gamma                70.637(3)
_cell_formula_units_Z            1
_cell_length_a                   13.8946(6)
_cell_length_b                   15.1490(9)
_cell_length_c                   17.4672(10)
_cell_measurement_reflns_used    25504
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      1.71
_cell_volume                     3165.0(3)
_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      200(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method
'omega scans; 600 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  0.117
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25504
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_meas      ?
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1242
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.087
_refine_ls_goodness_of_fit_obs   1.210
_refine_ls_hydrogen_treatment    'XYZ riding, U(H) = 1.2U(C) or 1.5U(Cmethyl)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         8242
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.206
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_obs          0.0973
_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^)+(0.0836P)^2^+4.3570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2352
_refine_ls_wR_factor_obs         0.2081
_reflns_number_observed          5443
_reflns_number_total             8242
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0203723_1.cif
_cod_data_source_block           71ff
_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^)+(0.0836P)^2^+4.3570P] 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^)+(0.0836P)^2^+4.3570P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4114935