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_4116224
_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 H45 Cl6 I N2 O10 S'
_chemical_formula_weight         1169.51
_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                79.1540(10)
_cell_angle_beta                 72.9720(10)
_cell_angle_gamma                72.1280(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1029(2)
_cell_length_b                   14.0516(2)
_cell_length_c                   14.8296(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2470.16(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49695
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_correction_T_min  0.7657
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         13977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0226P)^2^+1.9425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                11608
_reflns_number_total             13977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0013879_4.cif
_cod_data_source_block           40
_cod_original_cell_volume        2470.17(7)
_cod_database_code               4116224