Crystal structure of 1-hydroxy-2,2,6,6-tetramethylpiperidin-1-ium trifluoromethanesulfonate
Godemann, Christian; Spannenberg, Anke; Beweries, Torsten; Acta Crystallographica Section E 71 (2015) o921–; doi:10.1107/S2056989015020897

data_2241299
_publ_section_title
;
 Crystal structure of 1-hydroxy-2,2,6,6-tetramethylpiperidin-1-ium
 trifluoromethanesulfonate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o921
_journal_paper_doi               10.1107/S2056989015020897
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C9 H20 N O +, C F3 O3 S -'
_chemical_formula_moiety         'C9 H20 N O +, C F3 O3 S -'
_chemical_formula_sum            'C10 H20 F3 N O4 S'
_chemical_formula_weight         307.33
_chemical_name_systematic
;
1-Hydroxy-2,2,6,6-tetramethylpiperidin-1-ium trifluoromethanesulfonate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                79.5417(7)
_cell_angle_beta                 76.5159(7)
_cell_angle_gamma                75.5022(6)
_cell_formula_units_Z            2
_cell_length_a                   8.2824(2)
_cell_length_b                   8.7656(2)
_cell_length_c                   10.5703(3)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.90
_cell_measurement_theta_min      2.59
_cell_volume                     716.28(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.998
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.343
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0476P)^2^+0.2597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                3039
_reflns_number_total             3452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5176sup1.cif
_cod_data_source_block           I
_cod_database_code               2241299
_cod_database_fobs_code          2241299
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.913
_shelx_hkl_checksum              82866
_shelx_res_checksum              67217
_shelxl_version_number           2.014