Nitroxide-Substituted Nitronyl Nitroxide and Iminonitroxide
Shuichi Suzuki; Takanori Furui; Masato Kuratsu; Masatoshi Kozaki; Daisuke Shiomi; Kazunobu Sato; Takeji Takui; Keiji Okada; Journal of the American Chemical Society 132 (2010) 15908–15910; doi:10.1021/ja107769z

data_4103523
_publ_contact_author_address
;
Department of Chemistry, Graduate 
School of Science, Osaka City University, Sugimoto, Sumiyoshi-ku, Osaka
558-8585, Japan
;
_publ_contact_author_email       okadak@sci.osaka-cu.ac.jp
_publ_contact_author_fax         +81-6-6605-2568
_publ_contact_author_name        'Keiji Okada'
_publ_contact_author_phone       +81-6-6690-2709
_publ_section_title
;
 Nitroxide-Substituted Nitronyl Nitroxide and Iminonitroxide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15908
_journal_page_last               15910
_journal_paper_doi               10.1021/ja107769z
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C11 H21 N3 O3'
_chemical_formula_sum            'C11 H21 N3 O3'
_chemical_formula_weight         243.31
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_date             2009-04-24
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   34.674(2)
_cell_length_b                   34.674(2)
_cell_length_c                   6.0958(4)
_cell_measurement_reflns_used    4845
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0754
_cell_volume                     6347.0(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;

scan:

    Number of images: 600

               Slice: -80.0000 - 100.0000

         Image width: 0.3000

            Exp time: 10.0000

       Rotation axis: Phi

               Omega: 0.0000

                 Chi: 0.0000

                 Phi: 0.0000

                 XTD: 55.0419

              2theta: 24.7829

scan:

    Number of images: 200

               Slice: -15.0000 - 45.0000

         Image width: 0.3000

            Exp time: 10.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 0.0000

                 XTD: 55.0419

              2theta: 24.7829

scan:

    Number of images: 200

               Slice: -15.0000 - 45.0000

         Image width: 0.3000

            Exp time: 10.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 90.0000

                 XTD: 55.0419

              2theta: 24.7829

scan:

    Number of images: 200

               Slice: -15.0000 - 45.0000

         Image width: 0.3000

            Exp time: 10.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 180.0000

                 XTD: 55.0419

              2theta: 24.7829

scan:

    Number of images: 200

               Slice: -15.0000 - 45.0000

         Image width: 0.3000

            Exp time: 10.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 90.0000

                 Phi: 270.0000

                 XTD: 55.0419

              2theta: 24.7829

;
_diffrn_measurement_device_details
;

AFC7: Eulerian 3-circle

;
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ' \w or \f '
_diffrn_radiation_detector       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            16313
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.07
_diffrn_source_current           250.0000
_diffrn_source_power             15.0000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2376
_exptl_crystal_preparation
'mounted on a glass fiber with epoxy resin and placed in N2 stream at 170(2) K'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0602P)^2^+23.2811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                3043
_reflns_number_total             3183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107769z_si_002.cif
_cod_data_source_block           tBuNO-NN
_cod_original_cell_volume        6347.2(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4103523