Synthesis of the Epoxyquinol Dimer RKB-3564 D: Utilization of an Alkoxysilanol To Promote [4 + 4] Dimerization
Chaomin Li; John A. Porco; Journal of the American Chemical Society 126 (2004) 1310–1311; doi:10.1021/ja039543+

data_4112179
_publ_contact_author
;
    John A. Porco, Jr.
    Department of Chemistry
    Boston University
    Chemistry Dept.
    590 Commonwealth Ave.
    Boston MA 02215
;
_publ_contact_author_email       porco@chem.bu.edu
_publ_contact_author_phone       ' 617 353 2493'
_publ_section_title
;
 Synthesis of the Epoxyquinol Dimer RKB-3564 D: Utilization of an
 Alkoxysilanol To Promote [4 + 4] Dimerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1310
_journal_page_last               1311
_journal_paper_doi               10.1021/ja039543+
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C20 H20 O8'
_chemical_formula_weight         388.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.259(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.256(6)
_cell_length_b                   7.118(5)
_cell_length_c                   14.087(11)
_cell_measurement_temperature    125(2)
_cell_volume                     822.9(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      125(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker 1K CCD area detector'
_diffrn_measurement_method       '0.3 deg. 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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3254
_diffrn_reflns_theta_full        25.42
_diffrn_reflns_theta_max         25.42
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.9951
_exptl_absorpt_correction_T_min  0.9760
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      0
_exptl_crystal_description       rod
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.5(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         2285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.291
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                1719
_reflns_number_total             2285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0395432Bsi20031111_020608.cif
_cod_data_source_block           porco28
_cod_original_cell_volume        823.0(10)
_cod_database_code               4112179