Crystal structure of (2<i>S</i>,4<i>R</i>)-ethyl 4-nitromethyl-1-[(<i>S</i>)-1-phenylethyl]-6-sulfanylidenepiperidine-2-carboxylate
Zárate, Araceli; Aparicio, David; Palillero, Angel; Mendoza, Angel; Acta Crystallographica Section E 71 (2015) o41–o42; doi:10.1107/S2056989014026711

data_2240272
_publ_section_title
;
 Crystal structure of (2<i>S</i>,4<i>R</i>)-ethyl
 4-nitromethyl-1-[(<i>S</i>)-1-phenylethyl]-6-sulfanylidenepiperidine-2-carboxylate
;
_journal_coeditor_code           SU5036
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o41
_journal_page_last               o42
_journal_paper_doi               10.1107/S2056989014026711
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C17 H22 N2 O4 S'
_chemical_formula_moiety         'C17 H22 N2 O4 S'
_chemical_formula_sum            'C17 H22 N2 O4 S'
_chemical_formula_weight         350.42
_chemical_name_systematic
4-Nitromethyl-1-[(<i>S</i>)-1-phenylethyl]-6-sulfanylidenepiperidine-2-carboxylate
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7999(2)
_cell_length_b                   10.0103(6)
_cell_length_c                   30.4050(18)
_cell_measurement_reflns_used    2144
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.402
_cell_measurement_theta_min      3.556
_cell_volume                     1765.28(16)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5564
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Agilent Xcalibur Atlas Gemini'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            8486
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26.052
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.2019
_exptl_crystal_size_mid          0.0902
_exptl_crystal_size_min          0.0524
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.178
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 705 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.16(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.056
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                2306
_reflns_number_total             3373
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5036sup1.cf
_cod_data_source_block           I
_cod_database_code               2240272
_cod_database_fobs_code          2240272