Crystal structure of (–)-methyl (<i>R</i>,<i>E</i>)-4-[(2<i>R</i>,4<i>R</i>)-2-amino-2-trichloromethyl-1,3-dioxolan-4-yl]-4-hydroxy-2-methylbut-2-enoate
Oishi, Takeshi; Kidena, Mayu; Sugai, Tomoya; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 73 (2017) 983–986; doi:10.1107/S2056989017008283

data_2242131
_publ_section_title
;
 Crystal structure of (--)-methyl
 (<i>R</i>,<i>E</i>)-4-[(2<i>R</i>,4<i>R</i>)-2-amino-2-trichloromethyl-1,3-dioxolan-4-yl]-4-hydroxy-2-methylbut-2-enoate
;
_journal_coeditor_code           SU5377
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              983
_journal_page_last               986
_journal_paper_doi               10.1107/S2056989017008283
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C10 H14 Cl3 N O5'
_chemical_formula_moiety         'C10 H14 Cl3 N O5'
_chemical_formula_sum            'C10 H14 Cl3 N O5'
_chemical_formula_weight         334.57
_chemical_melting_point_gt       358
_chemical_melting_point_lt       359
_chemical_name_systematic
'(-)-Methyl (<i>R</i>,<i>E</i>)-4-[(2<i>R</i>,4<i>R</i>)-2-amino-2-trichloromethyl-1,3-dioxolan-4-yl]-4-hydroxy-2-methylbut-2-enoate'
_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_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.763(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.8494(4)
_cell_length_b                   12.6458(8)
_cell_length_c                   9.5658(6)
_cell_measurement_reflns_used    8568
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.73
_cell_volume                     684.23(8)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>publCif</i> (Westrip, 2010) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayered confocal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10686
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2016)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.293
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 993 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2376
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0300
_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^)+0.7994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                2268
_reflns_number_total             2376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5377sup1.cif
_cod_data_source_block           I
_cod_database_code               2242131
_cod_database_fobs_code          2242131
_shelx_res_checksum              76497