Absolute configurations of Emycin D, E and F; mimicry of centrosymmetric space groups by mixtures of chiral stereoisomers
Walker, Martina; Pohl, Ehmke; Herbst-Irmer, Regine; Gerlitz, Martin; Rohr, Jürgen; Sheldrick, George M.; Acta Crystallographica Section B 55 (1999) 607–616; doi:10.1107/S0108768199003948

data_2003002
_publ_section_title
;
 Absolute configurations of Emycin D, E and F; mimicry of
 centrosymmetric space groups by mixtures of chiral stereoisomers
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              607
_journal_page_last               616
_journal_paper_doi               10.1107/S0108768199003948
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C26 H19 Br O5'
_chemical_formula_weight         491.32
_chemical_name_common            O-brominebenzoyl-Emycin_D
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.32(2)
_cell_angle_beta                 110.25(2)
_cell_angle_gamma                92.76(2)
_cell_formula_units_Z            2
_cell_length_a                   8.279(2)
_cell_length_b                   11.539(3)
_cell_length_c                   11.962(3)
_cell_measurement_reflns_used    43
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1042.9(5)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device_type  'Stoe-Siemens AED2 four-circle)'
_diffrn_measurement_method       'profile data from 2theta/omega'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6304
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.01
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_T_max  0.426
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SHELXTL 5.1 (Sheldrick, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         .411
_refine_diff_density_min         -.409
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.290
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0300P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                5946
_reflns_number_total             6304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jz0006.cif
_cod_data_source_block           salbei
_cod_original_sg_symbol_H-M      P1
_cod_database_code               2003002