Development of a Convergent Entry to the Diazofluorene Antitumor Antibiotics: Enantioselective Synthesis of Kinamycin F
Christina M. Woo; Liang Lu; Shivajirao L. Gholap; Devin R. Smith; Seth B. Herzon; Journal of the American Chemical Society 132 (2010) 2540–2541; doi:10.1021/ja910769j

data_4101980
_publ_section_title
;
 Development of a Convergent Entry to the Diazofluorene Antitumor
 Antibiotics: Enantioselective Synthesis of Kinamycin F
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2540
_journal_page_last               2541
_journal_paper_doi               10.1021/ja910769j
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C23 H23 Br O7 '
_chemical_formula_sum            'C23 H23 Br O7'
_chemical_formula_weight         491.33
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.362(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   5.4308(9)
_cell_length_b                   15.240(3)
_cell_length_c                   12.964(2)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    223.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     1061.6(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 6.85
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11030
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_exptl_absorpt_coefficient_mu    1.985
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             504.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2285 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.006(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4781
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.9230
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                3671
_reflns_number_total             4781
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja910769j_si_002.cif
_cod_data_source_block           '_Herzon_CW01'
_cod_original_cell_volume        1061.5(3)
_cod_original_formula_sum        'C23 H23 Br O7 '
_cod_database_code               4101980