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_2243930
_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          'C17 H24 N2 O5 S'
_chemical_formula_moiety         'C17 H24 N2 O5 S'
_chemical_formula_sum            'C17 H24 N2 O5 S'
_chemical_formula_weight         368.44
_chemical_name_systematic
'1-[<i>N</i>-(4-methylphenyl)-<i>N</i>-(methylsulfonyl)alanyl]piperidine-4-carboxylic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 100.546(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1013(2)
_cell_length_b                   12.3092(2)
_cell_length_c                   12.4348(3)
_cell_measurement_reflns_used    8359
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      31.5170
_cell_measurement_theta_min      2.7110
_cell_volume                     1820.97(6)
_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 0.934
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29518
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.736
_diffrn_reflns_theta_min         2.159
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.882
_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    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.770
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.294
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         6284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0593P)^2^+0.3685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                4779
_reflns_number_total             6284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2254sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243930
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.978
_shelx_hkl_checksum              89178
_shelx_res_checksum              31558
_cod_database_fobs_code 2243930