TEMPO radicals showing magnetic interactions. II. 4-(Benzylideneamino)-TEMPO and related compounds
Iwasaki, Fujiko; Yoshikawa, Joseph H.; Yamamoto, Hajime; Takada, Kiwamu; Kan-nari, Eiji; Yasui, Masanori; Ishida, Takayuki; Nogami, Takashi; Acta Crystallographica Section B 55 (1999) 1057–1067; doi:10.1107/S0108768199007326

data_2105633
_publ_section_title
;
 TEMPO radicals showing magnetic interactions. II.
 4-(Benzylideneamino)-TEMPO and related compounds
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1057
_journal_page_last               1067
_journal_paper_doi               10.1107/S0108768199007326
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C17 H25 N2 O3 S '
_chemical_formula_sum            'C17 H25 N2 O3 S'
_chemical_formula_weight         337.46
_chemical_name_common            4-MeSO2-Ph-TEMPO
_chemical_name_systematic
4-(4-mesylphenylmethyleneamino)-2,2,6,6-tetramethylpiperidin-1-oxyl
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.539(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1835(18)
_cell_length_b                   15.487(2)
_cell_length_c                   11.5660(18)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    294
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      17.2
_cell_volume                     1822.3(5)
_computing_cell_refinement       'AFC (Rigaku Co., 1994)'
_computing_data_collection       'AFC (Rigaku Co., 1994)'
_computing_data_reduction        'teXsan (MSC, 1992)'
_computing_molecular_graphics    'ORTEP II (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0114
_diffrn_reflns_av_sigmaI/netI    .0247
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4390
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        2.06
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .193
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .976
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             724.00
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .25
_refine_diff_density_max         .218
_refine_diff_density_min         -.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          .0581
_refine_ls_R_factor_gt           .0409
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.4517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1235
_reflns_number_gt                3223
_reflns_number_total             4184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            oa0021.cif
_cod_data_source_block           14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.4517P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.4517P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1822.2(5)
_cod_original_sg_symbol_H-M      'P 21/c       '
_cod_original_formula_sum        'C17 H25 N2 O3 S '
_cod_database_code               2105633