Total Synthesis of Phorboxazole A via de Novo Oxazole Formation: Convergent Total Synthesis
Bo Wang; T. Matthew Hansen; Lynn Weyer; Dimao Wu; Ting Wang; Mathias Christmann; Yingtao Lu; Lu Ying; Mary M. Engler; Russell D. Cink; Chi-Sing Lee; Feryan Ahmed; Craig J. Forsyth; Journal of the American Chemical Society 133 (2011) 1506–1516; doi:10.1021/ja1089099

data_4105586
_publ_section_title
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 Total Synthesis of Phorboxazole A via de Novo Oxazole Formation:
 Convergent Total Synthesis
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1506
_journal_page_last               1516
_journal_paper_doi               10.1021/ja1089099
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        'R. Cink / Prof. C. Forsyth'
_chemical_formula_sum            'C55 H74 N2 O10 Si'
_chemical_formula_weight         951.25
_chemical_name_common            97329b
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_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            8
_cell_length_a                   21.3411(2)
_cell_length_b                   21.3411(2)
_cell_length_c                   27.0738(3)
_cell_measurement_temperature    173(2)
_cell_volume                     12330.6(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23893
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(24)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.210
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         10086
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.006
_refine_ls_restrained_S_obs      1.201
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_obs          0.0712
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1939
_refine_ls_wR_factor_obs         0.1711
_reflns_number_observed          5683
_reflns_number_total             10086
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja1089099_si_002.cif
_cod_data_source_block           97329b
_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^)+(0.1039P)^2^+0.0000P] 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^)+(0.1039P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4105586