Synthesis of Polyphenylene Dendrimers Related to "Cubic Graphite"
Xianfeng Shen; Douglas M. Ho; Robert A. Pascal; Journal of the American Chemical Society 126 (2004) 5798–5805; doi:10.1021/ja030675c

data_4112542
_publ_section_title
;
 Synthesis of Polyphenylene Dendrimers Related to "Cubic Graphite"
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5798
_journal_page_last               5805
_journal_paper_doi               10.1021/ja030675c
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety         'C258 H174'
_chemical_formula_structural     'C258 H174 . 14(C H2 Cl2)'
_chemical_formula_sum            'C272 H202 Cl28'
_chemical_formula_weight         4462.94
_chemical_name_systematic
; 
 Hexakis(2',3',4',5',6'-pentaphenylbiphenyl-4-yl)benzene 
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   48.2928(11)
_cell_length_b                   48.2928(11)
_cell_length_c                   11.8656(11)
_cell_measurement_reflns_used    62392
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.84
_cell_measurement_theta_min      1.46
_cell_volume                     23965(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      298(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method
'omega scans; 1400 0.5 deg 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  0.104
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            62392
_diffrn_reflns_theta_max         18.84
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             6930
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -8.34(999)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.204
_refine_ls_hydrogen_treatment    'XYZ riding, U(H) = 1.2U(C)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         4402
_refine_ls_number_restraints     389
_refine_ls_restrained_S_all      1.009
_refine_ls_restrained_S_obs      1.145
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_obs          0.1321
_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^)+(0.2799P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3751
_refine_ls_wR_factor_obs         0.3431
_reflns_number_observed          2777
_reflns_number_total             4402
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja030675c.cif
_cod_data_source_block           rap118r3msqf
_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^)+(0.2799P)^2^+0.0000P] 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^)+(0.2799P)^2^+0.0000P] 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        23965.4(24)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4112542