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_1505301
_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            'C52 H44'
_chemical_formula_weight         668.87
_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-97
_cell_angle_alpha                96.2450(10)
_cell_angle_beta                 103.0610(10)
_cell_angle_gamma                103.8060(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4794(6)
_cell_length_b                   12.9657(9)
_cell_length_c                   16.3977(11)
_cell_measurement_reflns_used    5090
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.25
_cell_volume                     1878.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13355
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0002(14)
_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_ref   1.011
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+0.0154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1903
_reflns_number_gt                4796
_reflns_number_total             8349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol063056ssi20061218_034204.cif
_cod_data_source_block           zh408ccd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P(-1)
_cod_database_code               1505301