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_4116221
_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            'C31 H32 F3 N O10'
_chemical_formula_weight         635.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9851(12)
_cell_length_b                   37.016(4)
_cell_length_c                   8.274(2)
_cell_measurement_temperature    188(2)
_cell_volume                     3058.1(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.1641
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6336
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.115
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_F_000             1328
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.34(193)
_refine_ls_extinction_coef       0.0155(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.261
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6033
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.287
_refine_ls_R_factor_all          0.2322
_refine_ls_R_factor_obs          0.0787
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.6716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1869
_refine_ls_wR_factor_obs         0.1299
_reflns_number_observed          2223
_reflns_number_total             6034
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0013879_1.cif
_cod_data_source_block           16-Mosher_ester
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.6716P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.6716P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116221