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_4103682
_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
;
(C48 H22 O8) (C7 H8)1.45 (C H2 Cl2)0.55
;
_chemical_formula_sum            'C58.7 H34.7 Cl1.1 O8'
_chemical_formula_weight         906.96
_chemical_name_systematic
;
2K-8-100-dp
;
_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                71.370(6)
_cell_angle_beta                 81.391(8)
_cell_angle_gamma                87.499(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8671(16)
_cell_length_b                   14.0629(18)
_cell_length_c                   14.0671(17)
_cell_measurement_reflns_used    1488
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.50
_cell_volume                     2199.5(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1158
_diffrn_reflns_av_sigmaI/netI    0.1468
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16258
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             939
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9680
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2100
_refine_ls_wR_factor_ref         0.2528
_reflns_number_gt                4404
_reflns_number_total             9680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1088309_si_001.cif
_cod_data_source_block           dh0601m
_cod_original_formula_sum        'C58.70 H34.70 Cl1.10 O8'
_cod_database_code               4103682