Cyclobutyl-Containing Rigid Analogues of Threonine: Synthesis and Physical Chemical Properties.
Feskov, Illia O.; Chernykh, Anton V.; Kondratov, Ivan S.; Klyachina, Mariya; Daniliuc, Constantin G.; Haufe, Günter; The Journal of organic chemistry 82 (2017) 12863–12868; doi:10.1021/acs.joc.7b02259

data_4033040
_publ_section_title
;
 Cyclobutyl-Containing Rigid Analogues of Threonine: Synthesis and
 Physical Chemical Properties.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12863
_journal_page_last               12868
_journal_paper_doi               10.1021/acs.joc.7b02259
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C10 H15 N O4'
_chemical_formula_weight         213.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                88.569(2)
_cell_angle_beta                 85.582(2)
_cell_angle_gamma                77.614(2)
_cell_formula_units_Z            2
_cell_length_a                   5.5617(2)
_cell_length_b                   9.7074(4)
_cell_length_c                   10.4167(3)
_cell_measurement_reflns_used    2445
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      66.6181
_cell_measurement_theta_min      4.2571
_cell_volume                     547.65(3)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_publication_material  'APEX2 v.2014.1-----1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'KappaCCD APEXII'
_diffrn_measurement_method       'phi / omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'CuK\a '
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3638
_diffrn_reflns_theta_full        65.07
_diffrn_reflns_theta_max         65.07
_diffrn_reflns_theta_min         4.26
_diffrn_source                   'fine--focus sealed tube'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison,
Wisconsin, USA.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0477P)^2^+0.1962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                1593
_reflns_number_total             1774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02259_si_001.cif
_cod_data_source_block           haf8553
_cod_depositor_comments
'Adding full bibliography for 4033040--4033042.cif.'
_cod_database_code               4033040
_shelx_res_checksum              23445
_shelx_hkl_checksum              23501