Total Synthesis of (+)-SCH 351448
Eun Joo Kang; Eun Jin Cho; Young Eun Lee; Mi Kyung Ji; Dong Mok Shin; Young Keun Chung; Eun Lee; Journal of the American Chemical Society 126 (2004) 2680–2681; doi:10.1021/ja0315309

data_4112272
_publ_section_title
;
 Total Synthesis of (+)-SCH 351448
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2680
_journal_page_last               2681
_journal_paper_doi               10.1021/ja0315309
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C64 H95 Na O16'
_chemical_formula_weight         1143.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 112.676(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.848(1)
_cell_length_b                   22.329(1)
_cell_length_c                   13.845(1)
_cell_measurement_reflns_used    10181
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     3950.1(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP32
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.1644
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20168
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.9857
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            WHITE
_exptl_crystal_density_diffrn    0.961
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -3.2(7)
_refine_ls_extinction_coef       0.026(2)
_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_ref   0.838
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         13040
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.2039
_refine_ls_R_factor_gt           0.1041
_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^)+(0.1630P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2452
_refine_ls_wR_factor_ref         0.2833
_reflns_number_gt                4416
_reflns_number_total             13040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0315309si20040203_012556.cif
_cod_data_source_block           na
_cod_database_code               4112272