4-Ethynyl-2,2,6,6-tetramethyl-1,2,5,6-tetrahydropyridine <i>N</i>-oxide
Bats, Jan W.; Frolow, Olga; Engels, Joachim W.; Acta Crystallographica Section E 65 (2009) o529–; doi:10.1107/S1600536809004681

data_2221197
_publ_section_title
;
 4-Ethynyl-2,2,6,6-tetramethyl-1,2,5,6-tetrahydropyridine
 <i>N</i>-oxide
;
_journal_coeditor_code           SU2096
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o529
_journal_paper_doi               10.1107/S1600536809004681
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C11 H16 N O'
_chemical_formula_moiety         'C11 H16 N O'
_chemical_formula_sum            'C11 H16 N O'
_chemical_formula_weight         178.25
_chemical_name_common
;
4-ethynyl-2,2,6,6-tetramethyl-1-oxyl-3,4-dehydropiperidine
;
_chemical_name_systematic
;
4-Ethynyl-2,2,6,6-tetramethyl-1,2,5,6-tetrahydropyridine <i>N</i>-oxide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.434(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0996(9)
_cell_length_b                   20.800(3)
_cell_length_c                   8.3662(13)
_cell_measurement_reflns_used    212
_cell_measurement_temperature    167(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     1052.5(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      167(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Siemens SMART 1K CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18416
_diffrn_reflns_theta_full        31.0
_diffrn_reflns_theta_max         32.23
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  1200
_diffrn_standards_number         322
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.166
_refine_ls_extinction_coef       0.074(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+0.2P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                3143
_reflns_number_total             3580
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2096.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2221197
_cod_database_fobs_code          2221197