Crystal structure of (–)-(<i>R</i>,<i>E</i>)-3-(1,3-benzodioxol-5-yl)-5-[(4<i>S</i>,5<i>R</i>)-5-hydroxymethyl-2,2-dimethyl-1,3-dioxolan-4-yl]-<i>N</i>,<i>N</i>-dimethylpent-4-enamide
Oishi, Takeshi; Ishii, Koki; Ishibashi, Mizuki; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 74 (2018) 825–828; doi:10.1107/S2056989018007132

data_2242501
_publ_section_title
;
 Crystal structure of
 (--)-(<i>R</i>,<i>E</i>)-3-(1,3-benzodioxol-5-yl)-5-[(4<i>S</i>,5<i>R</i>)-5-hydroxymethyl-2,2-dimethyl-1,3-dioxolan-4-yl]-<i>N</i>,<i>N</i>-dimethylpent-4-enamide
;
_journal_coeditor_code           IS5496
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              825
_journal_page_last               828
_journal_paper_doi               10.1107/S2056989018007132
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C20 H27 N O6'
_chemical_formula_moiety         'C20 H27 N O6'
_chemical_formula_sum            'C20 H27 N O6'
_chemical_formula_weight         377.42
_chemical_melting_point_gt       409
_chemical_melting_point_lt       410
_chemical_name_systematic
(--)-(<i>R</i>,<i>E</i>)-3-(1,3-Benzodioxol-5-yl)-5-{(4<i>S</i>,5<i>R</i>)-5-hydroxymethyl-2,2-dimethyl-1,3-dioxolan-4-yl}-<i>N</i>,<i>N</i>-dimethylpent-4-enamide
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 91.475(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2538(6)
_cell_length_b                   6.0642(4)
_cell_length_c                   17.1441(10)
_cell_measurement_reflns_used    3257
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.8961
_cell_measurement_theta_min      2.4749
_cell_volume                     961.75(11)
_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</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0463
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8906
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2016)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2900
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0458
_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^)+1.1579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                2454
_reflns_number_total             2900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5496sup1.cif
_cod_data_source_block           I
_cod_database_code               2242501
_cod_database_fobs_code          2242501
_shelx_res_checksum              20335