4,4,5,5-Tetramethyl-2-(4-pyridyl)imidazolidin-1-oxyl-3-oxide trichloroacetic acid solvate
Chen, Hong-Xian; Li, Zhong-Shu; Sun, Bai-Wang; Acta Crystallographica Section E 64 (2008) o1197–; doi:10.1107/S1600536808016085

data_2218802
_publ_section_title
;
 4,4,5,5-Tetramethyl-2-(4-pyridyl)imidazolidin-1-oxyl-3-oxide
 trichloroacetic acid solvate
;
_journal_coeditor_code           RZ2217
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1197
_journal_paper_doi               10.1107/S1600536808016085
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C12 H16 N3 O2 , C2 H Cl3 O2'
_chemical_formula_moiety         'C12 H16 N3 O2 , C2 H Cl3 O2'
_chemical_formula_sum            'C14 H17 Cl3 N3 O4'
_chemical_formula_weight         397.66
_chemical_name_systematic
;
4,4,5,5-Tetramethyl-2-(4-pyridyl)imidazolidin-1-oxyl-3-oxide
trichloroacetic acid solvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.003(2)
_cell_length_b                   21.036(4)
_cell_length_c                   9.2796(19)
_cell_measurement_reflns_used    12720
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      0.97
_cell_volume                     1764.9(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'thin-slice \w'
_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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14888
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.1663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                2041
_reflns_number_total             3100
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2217.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2218802
_cod_database_fobs_code          2218802