Synthesis of (-)-Sordarin
Shunsuke Chiba; Mitsuru Kitamura; Koichi Narasaka; Journal of the American Chemical Society 128 (2006) 6931–6937; doi:10.1021/ja060408h

data_4110604
_publ_contact_author
;
Dr Koichi Narasaka
Department of Chemistry
Graduate School of Science
The University of Tokyo
7-3-1 Hongo
Bunkyo-ku
Tokyo, Japan 113-0033
;
_publ_contact_author_email       narasaka@chem.s.u-tokyp.ac.jp
_publ_contact_author_fax         '+81 3 5800 6891'
_publ_contact_author_phone       '+81 3 5841 4343'
_publ_section_title
;
 Synthesis of (-)-Sordarin
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6931
_journal_page_last               6937
_journal_paper_doi               10.1021/ja060408h
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C21 H28 O3'
_chemical_formula_weight         328.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(2)
_cell_angle_beta                 105.577(3)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   14.286(7)
_cell_length_b                   7.151(3)
_cell_length_c                   18.100(9)
_cell_measurement_temperature    120(2)
_cell_volume                     1781.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.729
_diffrn_measured_fraction_theta_max 0.729
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKYa
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9709
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.9611
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0430
_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/[Ys^2^(Fo^2^)+(0.0485P)^2^+0.6702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                2685
_reflns_number_total             2985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060408hsi20060127_023916.cif
_cod_data_source_block           chib0129
_cod_original_cell_volume        1781.1(15)
_cod_database_code               4110604