Total Synthesis, Stereochemical Reassignment, and Absolute Configuration of Chlorofusin
Sang Yeul Lee; Ryan C. Clark; Dale L. Boger; Journal of the American Chemical Society 129 (2007) 9860–9861; doi:10.1021/ja073264v

data_4109776
_publ_section_title
;
 Total Synthesis, Stereochemical Reassignment, and Absolute Configuration
 of Chlorofusin
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9860
_journal_page_last               9861
_journal_paper_doi               10.1021/ja073264v
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C22 H22 Cl N O6'
_chemical_formula_weight         431.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.9229(16)
_cell_length_b                   20.997(4)
_cell_length_c                   25.787(5)
_cell_measurement_reflns_used    8122
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.59
_cell_volume                     4265.4(15)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31261
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADBAS (Sheldrick, 1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      0
_exptl_crystal_description       Parallelpiped
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         7517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+2.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                5447
_reflns_number_total             7517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073264vrom20070508_124826.cif
_cod_data_source_block           sang
_cod_original_cell_volume        4265.3(15)
_cod_database_code               4109776