Studies on cyclization reactions of 3-amino-2,4-dihydroxybutanoic acid derivatives.
Esgulian, Mathieu; Belot, Vincent; Guillot, Régis; Deloisy, Sandrine; Aitken, David J.; Organic & biomolecular chemistry 15 (2017) 1453–1462; doi:10.1039/c6ob02759h

data_7155448
_publ_section_title
;
 Studies on cyclization reactions of 3-amino-2,4-dihydroxybutanoic acid
 derivatives.
;
_journal_issue                   6
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1453
_journal_page_last               1462
_journal_paper_doi               10.1039/c6ob02759h
_journal_volume                  15
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C10 H13 N O7'
_chemical_formula_sum            'C10 H13 N O7'
_chemical_formula_weight         259.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.033(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0454(6)
_cell_length_b                   14.0347(14)
_cell_length_c                   7.1416(8)
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      2.90
_cell_volume                     594.73(11)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_unetI/netI     0.0943
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20042
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.409
_diffrn_reflns_theta_min         2.903
_exptl_absorpt_coefficient_mu    0.124
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       plate
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 755 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1675
_refine_ls_R_factor_gt           0.1101
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1462P)^2^+1.0323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2694
_refine_ls_wR_factor_ref         0.3029
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                2242
_reflns_number_total             3515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob02759h2.cif
_cod_data_source_block           15a
_cod_depositor_comments
'Adding full bibliography for 7155448--7155450.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7155448
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              90778