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_4116222
_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            'C40 H45 N O7'
_chemical_formula_weight         651.77
_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
_cell_angle_alpha                106.540(10)
_cell_angle_beta                 113.170(10)
_cell_angle_gamma                96.981(8)
_cell_formula_units_Z            2
_cell_length_a                   12.5460(10)
_cell_length_b                   12.6620(10)
_cell_length_c                   12.9950(10)
_cell_measurement_temperature    188(2)
_cell_volume                     1754.3(3)
_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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8964
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.084
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_F_000             696
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0258(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   1.090
_refine_ls_goodness_of_fit_obs   1.182
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         7853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_restrained_S_obs      1.182
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_obs          0.0512
_refine_ls_shift/esd_max         0.062
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.3097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1133
_refine_ls_wR_factor_obs         0.0967
_reflns_number_observed          5149
_reflns_number_total             7855
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0013879_2.cif
_cod_data_source_block           32
_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^)+(0.0375P)^2^+0.3097P] 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^)+(0.0375P)^2^+0.3097P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1754.3(2)
_cod_database_code               4116222