Synthesis of Cyclododeciptycene Quinones
Kaiyan Lou; Allan M. Prior; Bernard Wiredu; John Desper; Duy H. Hua; Journal of the American Chemical Society 132 (2010) 17635–17641; doi:10.1021/ja1088309

data_4103683
_publ_section_title
;
 Synthesis of Cyclododeciptycene Quinones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17635
_journal_page_last               17641
_journal_paper_doi               10.1021/ja1088309
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
;
(C88 H48 O12) (C2 H5 O)
;
_chemical_formula_sum            'C90 H53 O13'
_chemical_formula_weight         1342.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           230
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I a -3 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   33.0333(17)
_cell_length_b                   33.0333(17)
_cell_length_c                   33.0333(17)
_cell_measurement_reflns_used    3743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.90
_cell_measurement_theta_min      2.47
_cell_volume                     36046(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1821
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            91091
_diffrn_reflns_theta_full        20.80
_diffrn_reflns_theta_max         20.80
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    0.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Triangular
_exptl_crystal_F_000             11152
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.768
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         1580
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.738
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.1065
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2727
_refine_ls_wR_factor_ref         0.2986
_reflns_number_gt                924
_reflns_number_total             1580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1088309_si_002.cif
_cod_data_source_block           dh0608a
_cod_database_code               4103683