Crystal structure and Hirshfeld surface analysis of 1-[(benzyldimethylsilyl)methyl]-1-ethylpiperidin-1-ium ethanesulfonate
Kirchhoff, Jan-Lukas; Koller, Stephan G.; Louven, Kathrin; Strohmann, Carsten; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S205698902101361X

data_2244000
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 1-[(benzyldimethylsilyl)methyl]-1-ethylpiperidin-1-ium ethanesulfonate
;
_journal_coeditor_code           HB8003
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205698902101361X
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C17 H30 N Si +, C2 H5 O4 S -'
_chemical_formula_moiety         'C17 H30 N Si +, C2 H5 O4 S -'
_chemical_formula_sum            'C19 H35 N O4 S Si'
_chemical_formula_weight         401.63
_chemical_name_systematic
;
1-[(Benzyldimethylsilyl)methyl]-1-ethylpiperidin-1-ium ethanesulfonate
;
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.033(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4627(8)
_cell_length_b                   12.8187(11)
_cell_length_c                   10.3926(9)
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      2.98
_cell_volume                     1077.95(17)
_computing_cell_refinement
;
SAINT (Bruker, 2021)
;
_computing_data_collection
;
APEX4 (Bruker, 2021)
;
_computing_data_reduction
;
SAINT (Bruker, 2021)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
<i>CrystalExplorer21</i> (Spackman
<i>et al.</i>,  2021; Turner <i>et al.</i>,  2017),
<i>publCIF</i> (Westrip, 2010), <i>Mercury</i>
(Macrae <i>et al.</i>,  2020),
<i>GaussView 6.016</i> (Frisch <i>et al.</i>,  2016), <i>Gaussian 09
Revision A.02</i>
(Frisch <i>et al.</i>,  2016), <i>SCHAKAL99</i> (Keller, 1999),
<i>Molekel 4.3</i> (Fl\"ukiger <i>et al.</i>,  2000)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            68418
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.993
_diffrn_reflns_theta_min         2.517
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.816
_exptl_crystal_size_mid          0.439
_exptl_crystal_size_min          0.384
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.590
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3811 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         8122
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0390P)^2^+0.1456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                7987
_reflns_number_total             8122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8003sup1.cif
_cod_data_source_block           I
_cod_database_code               2244000
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.917
_shelx_hkl_checksum              54127
_shelx_res_checksum              48508
_cod_database_fobs_code 2244000