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_4114936
_publ_section_title
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 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 H40'
_chemical_formula_structural     'C60 H40 . 2 C H2 Cl2'
_chemical_formula_sum            'C62 H44 Cl4'
_chemical_formula_weight         930.77
_chemical_name_systematic
; 
 Octaphenylbiphenylene 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6482(5)
_cell_length_b                   24.2381(8)
_cell_length_c                   10.5573(3)
_cell_measurement_reflns_used    20081
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.38
_cell_volume                     4771.9(2)
_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; 500 0.5-degree frames; 360 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  0.063
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20081
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0021(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_hydrogen_treatment    'XYZ riding, U(H) = 1.2U(C)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4217
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_obs          0.0626
_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^)+(0.0823P)^2^+4.1516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1803
_refine_ls_wR_factor_obs         0.1531
_reflns_number_observed          2767
_reflns_number_total             4217
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0203723_2.cif
_cod_data_source_block           81new
_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^)+(0.0823P)^2^+4.1516P] 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^)+(0.0823P)^2^+4.1516P] 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               4114936