Total Synthesis of Marinomycins A-C and of Their Monomeric Counterparts Monomarinomycin A and iso-Monomarinomycin A
K. C. Nicolaou; Andrea L. Nold; Robert R. Milburn; Corinna S. Schindler; Kevin P. Cole; Junichiro Yamaguchi; Journal of the American Chemical Society 129 (2007) 1760–1768; doi:10.1021/ja068053p

data_4109081
_publ_section_title
;
 Total Synthesis of Marinomycins A-C and of Their Monomeric Counterparts
 Monomarinomycin A and iso-Monomarinomycin A
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1760
_journal_page_last               1768
_journal_paper_doi               10.1021/ja068053p
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C30 H38 O7'
_chemical_formula_weight         510.60
_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                 117.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.257(7)
_cell_length_b                   8.2518(17)
_cell_length_c                   21.011(4)
_cell_measurement_temperature    158(2)
_cell_volume                     5586(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.1181
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20793
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.085
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             2192
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(13)
_refine_ls_extinction_coef       0.00091(14)
_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   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         9730
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.235
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                6342
_reflns_number_total             9730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068053prom20061110_013313.cif
_cod_data_source_block           nold
_cod_database_code               4109081