TEMPO radicals showing magnetic interactions. I. 4-(4-Halobenzylideneamino)TEMPO and related compounds
Iwasaki, Fujiko; Yoshikawa, Joseph H.; Yamamoto, Hajime; Kan-nari, Eiji; Takada, Kiwamu; Yasui, Masanori; Ishida, Takayuki; Nogami, Takashi; Acta Crystallographica, Section B: Structural Science 55 (1999) 231–245; doi:10.1107/S0108768198012786

data_2003060
_publ_section_title
;
 TEMPO radicals showing magnetic interactions. I.
 4-(4-Halobenzylideneamino)TEMPO and related compounds
;
_journal_coden_ASTM              ASBSDK
_journal_issue                   2
_journal_name_full
;
 Acta Crystallographica, Section B: Structural Science
;
_journal_page_first              231
_journal_page_last               245
_journal_paper_doi               10.1107/S0108768198012786
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C15 H22 N3 O'
_chemical_formula_weight         260.36
_chemical_name_common            4-Py-TEMPO
_chemical_name_systematic
;
 4-(4-pyridyl)methyleneamino-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
_cell_angle_beta                 125.95(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.977(6)
_cell_length_b                   20.158(7)
_cell_length_c                   11.383(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      17.3
_cell_measurement_theta_min      14.3
_cell_volume                     1482(2)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'ORTEP II'
_computing_publication_material  teXsan
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3631
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        -0.08
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             564.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.2298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                2464
_reflns_number_total             3400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            oa0019.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.2298P] 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^)+(0.0537P)^2^+0.2298P] 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        1481.0(10)
_cod_original_sg_symbol_H-M      'P 21/c       '
_cod_original_formula_sum        'C15 H22 N3 O '
_cod_database_code               2003060
_cod_database_fobs_code          2003060