Stereoselective synthesis of a set of two functionalized (E)-alkene dipeptide isosteres of L-amino acid-L-Glu and L-amino acid-D-Glu
Oishi, Shinya; Tamamura, Hirokazu; Yamashita, Masaki; Odagaki, Yoshihiko; Hamanaka, Nobuyuki; Otaka, Akira; Fujii, Nobutaka; Journal of the Chemical Society, Perkin Transactions 1  (2001) 2445–; doi:10.1039/b103833h

data_7216913
_publ_section_title
;
 Stereoselective synthesis of a set of two functionalized (E)-alkene
 dipeptide isosteres of L-amino acid-L-Glu and L-amino acid-D-Glu
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2445
_journal_paper_doi               10.1039/b103833h
_journal_year                    2001
_chemical_compound_source        synthesis
_chemical_formula_analytical
;Found: C, 63.88; H, 6.87; N, 2.65. 
C26H33NO6S requires C, 64.04; H, 6.82; N, 2.87%
;
_chemical_formula_moiety         'C26 H33 N O6 S '
_chemical_formula_sum            'C26 H33 N O6 S'
_chemical_formula_weight         487.61
_chemical_melting_point          372.0(10)
_chemical_name_common            Mts-L-Phe-Y[(E)-CH=CH]-D-Glu(OMe)-OMe
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Thu Jun  7 10:59:16 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.780(8)
_cell_length_b                   35.92(1)
_cell_length_c                   6.24(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.1
_cell_measurement_theta_min      8.3
_cell_volume                     2640(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.03523
_diffrn_orient_matrix_UB_12      0.02351
_diffrn_orient_matrix_UB_13      0.05433
_diffrn_orient_matrix_UB_21      -0.07103
_diffrn_orient_matrix_UB_22      0.01393
_diffrn_orient_matrix_UB_23      -0.03565
_diffrn_orient_matrix_UB_31      -0.03034
_diffrn_orient_matrix_UB_32      -0.00533
_diffrn_orient_matrix_UB_33      0.14655
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.198
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2628
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         65.22
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        9.20
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            colourlessprismatic
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1040.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.506
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     307
_refine_ls_number_reflns         869
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0957
_refine_ls_shift/esd_max         1.4690
_refine_ls_shift/esd_mean        0.1570
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.1005
_reflns_number_observed          869
_reflns_number_total             2628
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            b103833h.txt
_cod_data_source_block           Comp_22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '371-373K' was changed to '372.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2639(4)
_cod_original_sg_symbol_H-M      'P 21 21 21   '
_cod_original_formula_sum        'C26 H33 N O6 S '
_cod_database_code               7216913