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_4033042
_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            'C6 H14 Cl N O4'
_chemical_formula_weight         199.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.2719(3)
_cell_length_b                   10.6899(3)
_cell_length_c                   16.9891(5)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    102.(2)
_cell_measurement_theta_max      72.2296
_cell_measurement_theta_min      5.2070
_cell_volume                     1865.50(9)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection
;

APEX3 v2016.1-0 (Bruker AXS Inc., 2016)
;
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      102.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14261
_diffrn_reflns_theta_full        72.22
_diffrn_reflns_theta_max         72.22
_diffrn_reflns_theta_min         5.21
_diffrn_source                   'Cu ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    3.507
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0334P)^2^+1.4682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                1797
_reflns_number_total             1836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02259_si_001.cif
_cod_data_source_block           haf8801
_cod_depositor_comments
'Adding full bibliography for 4033040--4033042.cif.'
_cod_database_code               4033042
_shelx_res_checksum              52673
_shelx_hkl_checksum              89990