Green Synthesis of α,β- and β,β-Dipeptides under Solvent-Free Conditions
José G. Hernández; Eusebio Juaristi; Journal of Organic Chemistry 75 (2010) 7107–7111; doi:10.1021/jo101159a

data_4025750
_publ_contact_author_address
;
Departamento de Quimica
Cinvestav, Mexico
A.P. 14-740; CP 07360
Mexico DF, Mexico
;
_publ_contact_author_email       ejuarist@cinvestav.mx
_publ_contact_author_fax         52(55)57473389
_publ_contact_author_name        'Eusebio Juaristi'
_publ_contact_author_phone       52(55)57473722
_publ_section_title
;
 Green Synthesis of \a,\b- and \b,\b-Dipeptides under Solvent-Free
 Conditions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7107
_journal_page_last               7111
_journal_paper_doi               10.1021/jo101159a
_journal_volume                  75
_journal_year                    2010
_chemical_absolute_configuration syn
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H17 N1 O5'
_chemical_formula_sum            'C15 H17 N O5'
_chemical_formula_weight         291.3
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-05-31
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.759(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.7030(10)
_cell_length_b                   12.3865(17)
_cell_length_c                   9.1015(13)
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.814
_cell_measurement_wavelength     0.71073
_cell_volume                     748.75(19)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.76848E-1
_diffrn_orient_matrix_UB_12      -0.2727E-3
_diffrn_orient_matrix_UB_13      -0.102123
_diffrn_orient_matrix_UB_21      0.128042
_diffrn_orient_matrix_UB_22      0.118265E-1
_diffrn_orient_matrix_UB_23      -0.427896E-1
_diffrn_orient_matrix_UB_31      0.192237E-1
_diffrn_orient_matrix_UB_32      -0.798617E-1
_diffrn_orient_matrix_UB_33      -0.59879E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.109
_diffrn_reflns_av_unetI/netI     0.1095
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4165
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         27.439
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9951
_exptl_absorpt_correction_T_min  0.9807
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.19
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -2(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0376
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1265
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.000069
_refine_ls_shift/su_mean         0.0075641
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 0.42P]
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2625
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                1498
_reflns_number_total             2374
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            jo101159a_si_002.cif
_cod_data_source_block           publish
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C15 H17 N1 O5'
_cod_database_code               4025750