Solution State Conformational Preferences of Dipeptides Derived from N-Aminoazetidinecarboxylic Acid: An Assessment of the Hydrazino Turn
Amandine Altmayer-Henzien; Valérie Declerck; Denis Merlet; Jean-Pierre Baltaze; Jonathan Farjon; Régis Guillot; David J. Aitken; Journal of Organic Chemistry 78 (2013) 6031–6039; doi:10.1021/jo400736t

data_4028345
_publ_contact_author_address
;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay
UMR CNRS 8182
B\^at. 420 
Universit\'e Paris 11
91405 ORSAY Cedex,
France.
;
_publ_contact_author_email       david.aitken@u-psud.fr
_publ_contact_author_name        'David J. AITKEN'
_publ_section_title
;
 Solution State Conformational Preferences of Dipeptides Derived from
 N-Aminoazetidinecarboxylic Acid: An Assessment of the Hydrazino Turn
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6031
_journal_page_last               6039
_journal_paper_doi               10.1021/jo400736t
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C13 H23 N3 O3'
_chemical_formula_sum            'C13 H23 N3 O3'
_chemical_formula_weight         269.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.3150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6775(2)
_cell_length_b                   25.0538(8)
_cell_length_c                   10.3034(3)
_cell_measurement_reflns_used    8458
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      33.57
_cell_measurement_theta_min      2.19
_cell_volume                     1426.19(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40293
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         34.53
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9982
_exptl_absorpt_correction_T_min  0.9796
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       needle
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.3952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                4429
_reflns_number_total             6022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400736t_si_002.cif
_cod_data_source_block           933GuillotICMMO
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4028345