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_4025749
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C9 H13 N1 O5'
_chemical_formula_sum            'C9 H13 N O5'
_chemical_formula_weight         215.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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             2010-03-08
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 117.8070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6573(2)
_cell_length_b                   9.6225(2)
_cell_length_c                   11.3219(2)
_cell_measurement_reflns_used    8050
_cell_measurement_temperature    293
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     1026.98(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.989
_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      -0.962806E-1
_diffrn_orient_matrix_UB_12      -0.376089E-1
_diffrn_orient_matrix_UB_13      -0.02348
_diffrn_orient_matrix_UB_21      -0.277704E-1
_diffrn_orient_matrix_UB_22      0.95066E-2
_diffrn_orient_matrix_UB_23      -0.97055E-1
_diffrn_orient_matrix_UB_31      0.348195E-1
_diffrn_orient_matrix_UB_32      -0.964116E-1
_diffrn_orient_matrix_UB_33      -0.4108E-3
_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  0.057
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13017
_diffrn_reflns_theta_full        26.109
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.034
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9718
_exptl_absorpt_correction_T_min  0.9305
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.63
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.16
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0615
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.05
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.0002568
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[\s^2^(F) + ( 0.00P)^2^ + 0.02P]
 ,where P=(max(Fo,0) + 2Fc)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0637
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                1953
_reflns_number_total             2333
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            jo101159a_si_001.cif
_cod_data_source_block           publish
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_original_formula_sum        'C9 H13 N1 O5'
_cod_database_code               4025749