Synthesis and structures of diindeno-fused 1,12-diphenylbenzo[c]phenanthrene and 1,14-diphenyl[5]helicene bearing severe helical twists.
Zhang, Yanzhong; Petersen, Jeffrey L.; Wang, Kung K.; Organic letters 9 (2007) 1025–1028; doi:10.1021/ol063056s

data_1505302
_publ_section_title
;
 Synthesis and structures of diindeno-fused
 1,12-diphenylbenzo[c]phenanthrene and 1,14-diphenyl[5]helicene bearing
 severe helical twists.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1025
_journal_page_last               1028
_journal_paper_doi               10.1021/ol063056s
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C56 H46'
_chemical_formula_weight         718.93
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5363(13)
_cell_length_b                   15.7011(11)
_cell_length_c                   13.4032(9)
_cell_measurement_reflns_used    5958
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.20
_cell_volume                     3893.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13355
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+1.4447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                3016
_reflns_number_total             4389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol063056ssi20061218_034230.cif
_cod_data_source_block           zh5ccd
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1505302