4,4'-{Diazenediylbis[(1,4-phenylene)bis(carbonyloxy)]}bis(2,2,6,6-tetramethylpiperidinyloxidanyl): the first crystal structure determination from powder data of a nitroxide radical
Bekö, Sándor L.; Thoms, Silke D.; Schmidt, Martin U.; Acta Crystallographica Section C 69 (2013) 1513–1515; doi:10.1107/S0108270113029211

data_2019320
_publ_section_title
;
 4,4'-{Diazenediylbis[(1,4-phenylene)bis(carbonyloxy)]}bis(2,2,6,6-tetramethylpiperidinyloxidanyl):
 the first crystal structure determination from powder data of a nitroxide
 radical
;
_journal_coeditor_code           SK3514
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1513
_journal_page_last               1515
_journal_paper_doi               10.1107/S0108270113029211
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C32 H42 N4 O6'
_chemical_formula_moiety         'C32 H42 N4 O6'
_chemical_formula_sum            'C32 H42 N4 O6'
_chemical_formula_weight         578.7
_chemical_melting_point          498.38
_chemical_name_common
;
Azobis(4-benzoyloxy-2,2,6,6-tetramethylpiperidinyloxidanyl)
;
_chemical_name_systematic
4,4'-{Diazenediylbis[(1,4-phenylene)bis(carbonyloxy)]}bis(2,2,6,6-tetramethylpiperidinyloxidanyl)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 109.2220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.3355(5)
_cell_length_b                   5.9277(2)
_cell_length_c                   14.5264(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1572.12(8)
_computing_cell_refinement       'TOPAS Academic (Coelho, 2007)'
_computing_data_collection       '<i>WinX^POW^</i> (Stoe & Cie, 2004)'
_computing_data_reduction        'DASH (David <i>et al.</i>, 2006)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_structure_refinement  'TOPAS Academic (Coelho, 2007)'
_computing_structure_solution    'DASH (David <i>et al.</i>, 2006)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Stoe Stadi-P'
_diffrn_radiation_monochromator  'primary focussing Ge 111'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.54056
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       powder
_exptl_crystal_F_000             620.0
_pd_char_particle_morphology     needles
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        79.99
_pd_meas_2theta_range_min        2.0
_pd_meas_number_of_points        7700
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        79.99
_pd_proc_2theta_range_min        2.0
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function
;
Chebyshev polynomials with 20 refinable coefficients
;
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function
;
Fundamental Parameters Line Profile Fitting Approach
(Cheary <i>et al.</i>, 2004)
;
_pd_proc_ls_prof_R_factor        9.336
_pd_proc_ls_prof_wR_expected     6.772
_pd_proc_ls_prof_wR_factor       8.997
_pd_proc_wavelength              1.54056
_pd_spec_mounting                '0.7 mm glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              30
_pd_spec_size_equat              0.7
_pd_spec_size_thick              0.7
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.153
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    67
_refine_ls_number_parameters     114
_refine_ls_number_restraints     59
_refine_ls_shift/su_max          0.001
_refine_ls_weighting_details     w=1/\s[Y\~obs\~]^2^
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            sk3514.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019320