Amphidinolide B: Total Synthesis, Structural Investigation, and Biological Evaluation
Liang Lu; Wei Zhang; Sangkil Nam; David A. Horne; Richard Jove; Rich G. Carter; Journal of Organic Chemistry 78 (2013) 2213–2247; doi:10.1021/jo3026077

data_4028023
_publ_section_title
;
 Amphidinolide B: Total Synthesis, Structural Investigation, and
 Biological Evaluation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2213
_journal_page_last               2247
_journal_paper_doi               10.1021/jo3026077
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C54 H70 O8 Si4'
_chemical_formula_weight         959.46
_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                 107.571(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.506(3)
_cell_length_b                   22.806(5)
_cell_length_c                   12.710(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3179.6(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29953
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.9539
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         11186
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.354
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1168P)^2^+0.4626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1980
_reflns_number_gt                8142
_reflns_number_total             11186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo3026077_si_002.cif
_cod_data_source_block           rc34
_cod_original_cell_volume        3179.5(12)
_cod_database_code               4028023