4-Amino-2,2,6,6-tetramethylpiperidin-1-oxyl radical (ATEMPO)
Legros, Jean-Pierre; De Caro, Dominique; Casellas, Hélène; Acta Crystallographica Section E 63 (2007) o3414–o3414; doi:10.1107/S1600536807032898

data_2214568
_publ_section_title
;
 4-Amino-2,2,6,6-tetramethylpiperidin-1-oxyl radical (ATEMPO)
;
_journal_coeditor_code           CF2110
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3414
_journal_page_last               o3414
_journal_paper_doi               10.1107/S1600536807032898
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C9 H19 N2 O'
_chemical_formula_moiety         'C9 H19 N2 O'
_chemical_formula_sum            'C9 H19 N2 O'
_chemical_formula_weight         171.26
_chemical_name_common
;
 ATEMPO
;
_chemical_name_systematic
;
 4-amino-2,2,6,6-tetramethylpiperidine 1-oxyl
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.61(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.721(2)
_cell_length_b                   12.919(3)
_cell_length_c                   13.955(4)
_cell_measurement_reflns_used    943
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      3.10
_cell_volume                     1024.6(5)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996),
CAMERON (Pearce & Watkin, 1993)
and ORTEP3 (Farrugia, 1997)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe IPDS imaging plate'
_diffrn_measurement_method       '\f scans with 1.5\% steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7824
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                1618
_reflns_number_total             1989
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf2110.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2214568
_cod_database_fobs_code          2214568