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_4107210
_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            'C35 H35 Br N4 O5 S'
_chemical_formula_weight         703.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                94.815(8)
_cell_angle_beta                 95.074(4)
_cell_angle_gamma                101.252(7)
_cell_formula_units_Z            2
_cell_length_a                   9.588(4)
_cell_length_b                   10.753(4)
_cell_length_c                   15.679(6)
_cell_measurement_reflns_used    2976
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.3328
_cell_measurement_theta_min      3.0975
_cell_volume                     1570.7(11)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10555
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.7636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       Block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+3.0824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                3953
_reflns_number_total             5421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja209945x_si_002_2.cif
_cod_data_source_block           7
_cod_original_cell_volume        1570.7(10)
_cod_database_code               4107210