Application of Ring-Closing Metathesis to the Formal Total Synthesis of (+)-FR900482
Ingrid M. Fellows; David E. Kaelin; Stephen F. Martin; Journal of the American Chemical Society 122 (2000) 10781–10787; doi:10.1021/ja0013879

data_4116225
_publ_section_title
;
 Application of Ring-Closing Metathesis to the Formal Total Synthesis of
 (+)-FR900482
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10781
_journal_page_last               10787
_journal_paper_doi               10.1021/ja0013879
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C47.5 H47.5 Cl4.5 N2 O11 S'
_chemical_formula_weight         1013.96
_chemical_name_systematic
; 
 ? 
;
_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                110.15(2)
_cell_angle_beta                 97.598(19)
_cell_angle_gamma                89.51(2)
_cell_formula_units_Z            2
_cell_length_a                   11.018(4)
_cell_length_b                   14.145(4)
_cell_length_c                   17.790(6)
_cell_measurement_temperature    298(2)
_cell_volume                     2578.0(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scan
_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  0.1627
_diffrn_reflns_av_sigmaI/netI    0.2332
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9343
_diffrn_reflns_theta_full        22.41
_diffrn_reflns_theta_max         22.41
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.353
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plates
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .04
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.786
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         6008
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      1.762
_refine_ls_R_factor_all          0.3014
_refine_ls_R_factor_gt           0.1886
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2637
_refine_ls_wR_factor_ref         0.2924
_reflns_number_gt                2543
_reflns_number_total             6008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0013879_5.cif
_cod_data_source_block           43
_cod_original_cell_volume        2577.9(14)
_cod_original_formula_sum        'C47.50 H47.50 Cl4.50 N2 O11 S'
_cod_database_code               4116225