Total Synthesis, Assignment of Absolute Stereochemistry, and Structural Revision of Chlorofusin
Wen-Jian Qian; Wan-Guo Wei; Yong-Xia Zhang; Zhu-Jun Yao; Journal of the American Chemical Society 129 (2007) 6400–6401; doi:10.1021/ja072225g

data_4109440
_publ_section_title
;
 Total Synthesis, Assignment of Absolute Stereochemistry, and Structural
 Revision of Chlorofusin
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6400
_journal_page_last               6401
_journal_paper_doi               10.1021/ja072225g
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C18 H22 Cl N O6'
_chemical_formula_weight         383.82
_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                 101.878(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3212(12)
_cell_length_b                   7.5076(7)
_cell_length_c                   18.8449(17)
_cell_measurement_reflns_used    1246
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.461
_cell_measurement_theta_min      4.417
_cell_volume                     1844.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10512
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57656
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2196
_reflns_number_gt                1918
_reflns_number_total             4023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072225gsi20070330_043318.cif
_cod_data_source_block           cd24195
_cod_original_formula_sum        'C18 H22 N O6  Cl'
_cod_database_code               4109440