Stereoselective Syntheses of Rolliniastatin 1, Rollimembrin, and Membranacin
Gyochang Keum; Cheol Hee Hwang; Soon Bang Kang; Youseung Kim; Eun Lee; Journal of the American Chemical Society 127 (2005) 10396–10399; doi:10.1021/ja0526867

data_4111823
_publ_contact_author             ' Gyochang Keum; Eun Lee* '
_publ_contact_author_email       ' gkeum@kist.re.kr //  eunlee@snu.ac.kr '
_publ_section_title
;
 Stereoselective Syntheses of Rolliniastatin 1, Rollimembrin, and
 Membranacin
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10396
_journal_page_last               10399
_journal_paper_doi               10.1021/ja0526867
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C22 H26 O4 S'
_chemical_formula_weight         386.49
_chemical_melting_point          435.0(5)
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 90.86(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   9.601(2)
_cell_length_b                   21.070(2)
_cell_length_c                   9.898(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2002.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.829
_diffrn_measured_fraction_theta_max 0.829
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3247
_diffrn_reflns_theta_full        25.16
_diffrn_reflns_theta_max         25.16
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.9550
_exptl_absorpt_correction_T_min  0.9327
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         3064
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0689P)^2^+0.2767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                3007
_reflns_number_total             3064
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0526867si20050505_062334.cif
_cod_data_source_block           k
_cod_database_code               4111823