Total Synthesis and Structural Revision of Vannusals A and B: Synthesis of the Originally Assigned Structure of Vannusal B
K. C. Nicolaou; Adrian Ortiz; Hongjun Zhang; Philippe Dagneau; Andreas Lanver; Michael P. Jennings; Stellios Arseniyadis; Raffaella Faraoni; Dimitrios E. Lizos; Journal of the American Chemical Society 132 (2010) 7138–7152; doi:10.1021/ja100740t

data_4102416
_publ_section_title
;
 Total Synthesis and Structural Revision of Vannusals A and B: Synthesis
 of the Originally Assigned Structure of Vannusal B
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7138
_journal_page_last               7152
_journal_paper_doi               10.1021/ja100740t
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C40 H51 Br N O6'
_chemical_formula_weight         721.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 130.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.042(8)
_cell_length_b                   11.144(2)
_cell_length_c                   26.725(5)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      10.48
_cell_measurement_theta_min      7.42
_cell_volume                     8568(5)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31595
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    1.000
_exptl_absorpt_correction_T_max  0.7954
_exptl_absorpt_correction_T_min  0.7672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block-shaped
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.048(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         14619
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.2194
_reflns_number_gt                8416
_reflns_number_total             14619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja100740t_si_003.cif
_cod_data_source_block           hzkc2
_cod_original_cell_volume        8568(3)
_cod_database_code               4102416