Versatile Synthetic Route to and DSC Analysis of Dehydrobenzoannulenes: Crystal Structure of a Heretofore Inaccessible [20]Annulene Derivative
Michael M. Haley; Michael L. Bell; Jamieson J. English; Charles A. Johnson; Timothy J. R. Weakley; Journal of the American Chemical Society 119 (1997) 2956–2957; doi:10.1021/ja964048h

data_4116944
_publ_section_title
;
 Versatile Synthetic Route to and DSC Analysis of Dehydrobenzoannulenes:
 Crystal Structure of a Heretofore Inaccessible [20]Annulene Derivative
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2956
_journal_page_last               2957
_journal_paper_doi               10.1021/ja964048h
_journal_volume                  119
_journal_year                    1997
_chemical_formula_moiety         'C36 H16 '
_chemical_formula_sum            'C36 H16'
_chemical_formula_weight         448.52
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Sat Nov 16 15:20:11 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90.16(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.223(4)
_cell_length_b                   12.601(3)
_cell_length_c                   24.378(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      22.0
_cell_volume                     4983(2)
_computing_cell_refinement       'Enraf-Nonius software v.5 '
_computing_data_collection       'Enraf-Nonius software v.5 '
_computing_data_reduction        'MSC TEXSAN suite v.5.0 (1989) '
_computing_publication_material  'MSC TEXSAN suite v.5.0 (1989) '
_computing_structure_refinement  'MSC TEXSAN suite v.5.0 (1989) '
_computing_structure_solution    'MSC TEXSAN suite v.5.0 (1989) '
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_orient_matrix_UB_11      -0.01633
_diffrn_orient_matrix_UB_12      -0.06981
_diffrn_orient_matrix_UB_13      0.01613
_diffrn_orient_matrix_UB_21      0.04918
_diffrn_orient_matrix_UB_22      -0.03411
_diffrn_orient_matrix_UB_23      -0.01721
_diffrn_orient_matrix_UB_31      0.03333
_diffrn_orient_matrix_UB_32      0.01602
_diffrn_orient_matrix_UB_33      0.03354
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  1.62
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            3802
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        -2.60
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         -0.20
_refine_diff_density_min         0.19
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.625
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         2651
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0605
_refine_ls_shift/esd_max         0.0284
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0411
_reflns_number_observed          2651
_reflns_number_total             3802
_reflns_observed_criterion       1.00
_cod_data_source_file            ja964048h.cif
_cod_data_source_block           C36H16
_cod_original_cell_volume        4983(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C36 H16 '
_cod_database_code               4116944