Crystal structure of (+)-methyl (<i>E</i>)-3-[(2<i>S</i>,4<i>S</i>,5<i>R</i>)-2-amino-5-hydroxymethyl-2-trichloromethyl-1,3-dioxolan-4-yl]-2-methylprop-2-enoate
Oishi, Takeshi; Yasushima, Daichi; Yuasa, Kihiro; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 72 (2016) 343–346; doi:10.1107/S2056989016002474

data_2241563
_publ_section_title
;
 Crystal structure of (+)-methyl
 (<i>E</i>)-3-[(2<i>S</i>,4<i>S</i>,5<i>R</i>)-2-amino-5-hydroxymethyl-2-trichloromethyl-1,3-dioxolan-4-yl]-2-methylprop-2-enoate
;
_journal_coeditor_code           IS5442
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              343
_journal_page_last               346
_journal_paper_doi               10.1107/S2056989016002474
_journal_volume                  72
_journal_year                    2016
_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       366
_chemical_melting_point_lt       365
_chemical_name_systematic
;(+)-Methyl
(<i>E</i>)-3-[(2<i>S</i>,4<i>S</i>,5<i>R</i>)-2-amino-5-(hydroxymethyl)-2-trichloromethyl-1,3-dioxolan-4-yl]-2-methylprop-2-enoate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.847(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8821(9)
_cell_length_b                   5.5847(3)
_cell_length_c                   17.2971(14)
_cell_measurement_reflns_used    6489
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.45
_cell_volume                     1382.96(16)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2014)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2013</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0299
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11488
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.211
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 959 quotients
[(<i>I</i>^+^)--(<i>I</i>^--^)]/[(<i>I</i>^+^)+(<i>I</i>^--^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0137P)^2^+1.9510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                2272
_reflns_number_total             2420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5442sup1.cif
_cod_data_source_block           I
_cod_database_code               2241563
_shelx_res_checksum              27704
_cod_database_fobs_code 2241563