Stereogenic motif consisting of rigid ring and intraannular chains: isolation and structures of stereoisomers of 9-alkyl-1,8-anthrylene-butadiynylene cyclic dimers.
Toyota, Shinji; Onishi, Hiroyuki; Kawai, Yoshihiro; Morimoto, Takaaki; Miyahara, Hiroaki; Iwanaga, Tetsuo; Wakamatsu, Kan; Organic letters 11 (2009) 321–324; doi:10.1021/ol802488z

data_1503736
_publ_section_title
;
 Stereogenic motif consisting of rigid ring and intraannular chains:
 isolation and structures of stereoisomers of
 9-alkyl-1,8-anthrylene-butadiynylene cyclic dimers.
;
_journal_issue                   2
_journal_name_full               'Organic letters'
_journal_page_first              321
_journal_page_last               324
_journal_paper_doi               10.1021/ol802488z
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C44 H32'
_chemical_formula_sum            'C44 H32'
_chemical_formula_weight         560.70
_chemical_melting_point_gt       451
_chemical_melting_point_lt       453
_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                72.870(12)
_cell_angle_beta                 72.915(14)
_cell_angle_gamma                68.027(9)
_cell_formula_units_Z            2
_cell_length_a                   11.1772(7)
_cell_length_b                   11.9076(14)
_cell_length_c                   13.265(3)
_cell_measurement_temperature    113(2)
_cell_volume                     1530.7(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.1168
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14634
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9925
_exptl_absorpt_correction_T_min  0.9737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         6933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                3873
_reflns_number_total             6933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol802488z_si_002.cif
_cod_data_source_block           syn3cBu
_cod_original_cell_volume        1530.6(4)
_cod_database_code               1503736