Enantioselective Total Syntheses of Citrinadins A and B. Stereochemical Revision of Their Assigned Structures.
Bian, Zhiguo; Marvin, Christopher C.; Pettersson, Martin; Martin, Stephen F.; Journal of the American Chemical Society 136 (2014) 14184–; doi:10.1021/ja5074646

data_4122695
_publ_section_title
;
 Enantioselective Total Syntheses of Citrinadins A and B. Stereochemical
 Revision of Their Assigned Structures.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14184
_journal_paper_doi               10.1021/ja5074646
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C35 H30 N O7 Si'
_chemical_formula_weight         604.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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-97
_cell_angle_alpha                74.475(5)
_cell_angle_beta                 89.769(5)
_cell_angle_gamma                80.187(5)
_cell_formula_units_Z            2
_cell_length_a                   9.149(5)
_cell_length_b                   12.298(5)
_cell_length_c                   19.169(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2045.7(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.820
_diffrn_measured_fraction_theta_max 0.820
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16645
_diffrn_reflns_theta_full        72.40
_diffrn_reflns_theta_max         72.40
_diffrn_reflns_theta_min         6.70
_exptl_absorpt_coefficient_mu    0.825
_exptl_crystal_density_diffrn    0.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             634
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6648
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+2.0146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                4782
_reflns_number_total             6648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5074646_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4122695--4122702.cif.'
_cod_database_code               4122695