Synthetic Study of Pactamycin: Enantioselective Construction of the Pactamycin Core with Five Contiguous Stereocenters.
Yamaguchi, Mami; Hayashi, Minami; Hamada, Yasumasa; Nemoto, Tetsuhiro; Organic letters 18 (2016) 2347–2350; doi:10.1021/acs.orglett.6b00761

data_1543819
_publ_section_title
;
 Synthetic Study of Pactamycin: Enantioselective Construction of the
 Pactamycin Core with Five Contiguous Stereocenters.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2347
_journal_page_last               2350
_journal_paper_doi               10.1021/acs.orglett.6b00761
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C30 H39 N3 O10 S'
_chemical_formula_sum            'C30 H39 N3 O10 S'
_chemical_formula_weight         633.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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
_cell_angle_alpha                95.4973(11)
_cell_angle_beta                 105.1594(11)
_cell_angle_gamma                113.2588(11)
_cell_formula_units_Z            2
_cell_length_a                   12.1373(3)
_cell_length_b                   12.1458(3)
_cell_length_c                   12.5058(3)
_cell_measurement_reflns_used    11686
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.76
_cell_volume                     1593.08(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17254
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672.00
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.640
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0598P)^2^+1.2491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                3242
_reflns_number_total             5695
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol6b00761_si_002.cif
_cod_data_source_block           160212nemoto32
_cod_original_cell_volume        1593.07(6)
_cod_database_code               1543819