Synthetic studies on the pederin family of antitumour agents. Syntheses of mycalamide B, theopederin D and pederin
Kocienski, Philip; Narquizian, Robert; Raubo, Piotr; Smith, Christopher; Farrugia, Louis J.; Muir, Kenneth; Boyle, F. Thomas; Journal of the Chemical Society, Perkin Transactions 1  (2000) 2357–; doi:10.1039/a909898d

data_7213251
_publ_section_title
;
 Synthetic studies on the pederin family of antitumour agents. Syntheses
 of mycalamide B, theopederin D and pederin
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2357
_journal_paper_doi               10.1039/a909898d
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H39 N O7 Se'
_chemical_formula_structural     'C29 H39 N O7 Se'
_chemical_formula_sum            'C29 H39 N O7 Se'
_chemical_formula_weight         592.57
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1998-09-10T08:40:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.768(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5035(5)
_cell_length_b                   10.0704(9)
_cell_length_c                   17.6777(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      20.09
_cell_measurement_theta_min      13.18
_cell_measurement_wavelength     0.71073
_cell_volume                     1470.31(17)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.36162E-1
_diffrn_orient_matrix_UB_12      0.7662E-2
_diffrn_orient_matrix_UB_13      -0.57953E-1
_diffrn_orient_matrix_UB_21      -0.10945
_diffrn_orient_matrix_UB_22      0.29504E-1
_diffrn_orient_matrix_UB_23      0.4901E-2
_diffrn_orient_matrix_UB_31      0.37063E-1
_diffrn_orient_matrix_UB_32      0.09457
_diffrn_orient_matrix_UB_33      0.00319
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4104
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.34
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  0.8306
_exptl_absorpt_correction_T_min  0.6815
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   7
        Theta correction was applied.
        Averaged transmission function was used.
        Fourier smoothing - Window value   4
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         3402
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                2097
_reflns_number_total             3402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909898dsup1.cif
_cod_data_source_block           pk3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7213251
_exptl_absorpt_factor_mur        0.183
_exptl_absorpt_correction_t_ave  0.7745
_diffrn_standards_decay_corr_max 1.024
_diffrn_standards_decay_corr_min 0.976