Crystal structures of two alanylpiperidine analogues
Mambourg, Kalina; Tumanov, Nikolay; Henon, Gilles; Lanners, Steve; Garcia-Ladona, Javier; Wouters, Johan; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021010392

data_2243929
_publ_section_title
;
 Crystal structures of two alanylpiperidine analogues
;
_journal_coeditor_code           VM2254
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021010392
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C19 H28 N2 O5 S'
_chemical_formula_moiety         'C19 H28 N2 O5 S'
_chemical_formula_sum            'C19 H28 N2 O5 S'
_chemical_formula_weight         396.49
_chemical_name_systematic
'Ethyl 1-[<i>N</i>-(4-methylphenyl)-<i>N</i>-(methylsulfonyl)alanyl]piperidine-4-carboxylate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                75.947(6)
_cell_angle_beta                 79.302(6)
_cell_angle_gamma                74.554(5)
_cell_formula_units_Z            2
_cell_length_a                   8.5368(6)
_cell_length_b                   9.6594(6)
_cell_length_c                   13.5173(12)
_cell_measurement_reflns_used    3246
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.4
_cell_volume                     1033.47(14)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3712
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur, Gemini Ultra R
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_unetI/netI     0.045
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13200
_diffrn_reflns_theta_full        25.2
_diffrn_reflns_theta_max         32.8
_diffrn_reflns_theta_min         2.234
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlisPro (Rigaku OD, 2018), based on expressions derived by Clark &
Reid (1995)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.790
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.375
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.093
_refine_ls_R_factor_gt           0.054
_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^)+(0.0633P)^2^+0.1206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.130
_refine_ls_wR_factor_ref         0.158
_reflns_number_gt                4304
_reflns_number_total             6870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2254sup1.cif
_cod_data_source_block           I
_cod_database_code               2243929
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.991
_shelx_hkl_checksum              78714
_shelx_res_checksum              36550
_cod_database_fobs_code 2243929