Total synthesis and structural revision of (+)-muironolide a.
Xiao, Qing; Young, Kyle; Zakarian, Armen; Journal of the American Chemical Society 137 (2015) 5907–5910; doi:10.1021/jacs.5b03531

data_4123776
_publ_section_title
;
 Total synthesis and structural revision of (+)-muironolide a.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5907
_journal_page_last               5910
_journal_paper_doi               10.1021/jacs.5b03531
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C47 H80 Cl4 N O9'
_chemical_formula_weight         944.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_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                 90.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.08(4)
_cell_length_b                   7.555(9)
_cell_length_c                   17.70(2)
_cell_measurement_temperature    100(2)
_cell_volume                     4691(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_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  0.1493
_diffrn_reflns_av_sigmaI/netI    0.2493
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10326
_diffrn_reflns_theta_full        23.39
_diffrn_reflns_theta_max         23.39
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.308
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2036
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_coef       0.0038(11)
_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   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.2745
_refine_ls_R_factor_gt           0.1496
_refine_ls_shift/su_max          3.672
_refine_ls_shift/su_mean         0.075
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3445
_refine_ls_wR_factor_ref         0.4230
_reflns_number_gt                1983
_reflns_number_total             4662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b03531_si_003.cif
_cod_data_source_block           x07152014_0m_a
_cod_original_cell_volume        4690(9)
_cod_database_code               4123776