Synthesis of Dragmacidin D via Direct C-H Couplings
Debashis Mandal; Atsushi D. Yamaguchi; Junichiro Yamaguchi; Kenichiro Itami; Journal of the American Chemical Society 133 (2011) 19660–19663; doi:10.1021/ja209945x

data_4107209
_publ_section_title
;
 Synthesis of Dragmacidin D via Direct C-H Couplings
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19660
_journal_page_last               19663
_journal_paper_doi               10.1021/ja209945x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C20 H17 N3 O3 S'
_chemical_formula_weight         379.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.854(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.239(3)
_cell_length_b                   8.1646(17)
_cell_length_c                   15.033(3)
_cell_measurement_reflns_used    3772
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.1501
_cell_volume                     1745.5(6)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11262
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_correction_T_min  0.9688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       Chip
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0567P)^2^+0.6497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                2613
_reflns_number_total             3061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja209945x_si_002_1.cif
_cod_data_source_block           S1
_cod_original_cell_volume        1745.6(6)
_cod_database_code               4107209