Synthesis and structure of a twisted, colossal quinone
Watson, Jr, James A.; Pascal, Jr, Robert A.; Ho, Douglas M.; Kilway, Kathleen V.; Tetrahedron Letters 41 (2000) 5005–5008; doi:10.1016/S0040-4039(00)00773-5

data_5000395
_publ_section_title
;
 Synthesis and structure of a twisted, colossal quinone
;
_journal_issue                   26
_journal_name_full               'Tetrahedron Letters'
_journal_page_first              5005
_journal_page_last               5008
_journal_paper_doi               10.1016/S0040-4039(00)00773-5
_journal_volume                  41
_journal_year                    2000
_chemical_formula_moiety         'C86 H88 O2, 2(C4 H8 O2)'
_chemical_formula_structural     'C86 H88 O2 . 2(C4 H8 O2)'
_chemical_formula_sum            'C94 H104 O6'
_chemical_formula_weight         1329.77
_chemical_name_systematic
;\
2,5,8,12,15,18,21,25-Octa(t-butyl)diacenaphtho[1,2-l:1',2'-l']-\
benzo[1,2-j:4,5-j']difluoranthene-10,23-dione Ethyl Acetate Solvate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.5203(2)
_cell_length_b                   16.5203(2)
_cell_length_c                   25.6779(4)
_cell_volume                     6069.12(14)
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans; 800 1.0\% rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69816
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(263)
_refine_ls_extinction_coef       0.0027(6)
_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_all   1.023
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_obs          0.0516
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+1.0012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1424
_refine_ls_wR_factor_obs         0.1294
_reflns_number_observed          4272
_reflns_number_total             5302
_reflns_observed_criterion       I>2\s(I)
_cod_database_code               5000395