3-Ethynyl-2,2,5,5-tetramethyl-1-oxyl-3-pyrroline
Frolow, Olga; Bats, Jan W.; Engels, Joachim W.; Acta Crystallographica Section E 65 (2009) o1848–; doi:10.1107/S1600536809026725

data_2222810
_publ_section_title
;
 3-Ethynyl-2,2,5,5-tetramethyl-1-oxyl-3-pyrroline
;
_journal_coeditor_code           NC2152
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1848
_journal_paper_doi               10.1107/S1600536809026725
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C10 H14 N O'
_chemical_formula_moiety         'C10 H14 N O'
_chemical_formula_sum            'C10 H14 N O'
_chemical_formula_weight         164.22
_chemical_name_systematic
;
3-Ethynyl-2,2,5,5-tetramethyl-1-oxyl-3-pyrroline
;
_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                 104.333(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9326(15)
_cell_length_b                   19.058(4)
_cell_length_c                   6.5989(11)
_cell_measurement_reflns_used    130
_cell_measurement_temperature    167(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     966.6(3)
_computing_cell_refinement       'SMART (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 0.992
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16848
_diffrn_reflns_theta_full        31.65
_diffrn_reflns_theta_max         32.35
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  1200
_diffrn_standards_number         182
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+0.35P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                2214
_reflns_number_total             3301
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nc2152.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2222810
_cod_database_fobs_code          2222810