Azobenzene Derivatives Carrying a Nitroxide Radical
Shin'ichi Nakatsuji; Masahiro Fujino; Satoko Hasegawa; Hiroki Akutsu; Jun-ichi Yamada; Vladimir S. Gurman; Andrey Kh.Vorobiev; Journal of Organic Chemistry 72 (2007) 2021–2029; doi:10.1021/jo062266f

data_4022732
_publ_contact_author_address
; 
University of Hyogo, Graduate School of Material Science
3-2-1 Kouto, Kamigori, Hyogo 678-1297, Japan
;
_publ_contact_author_email       nakatuji@sci.u-hyogo.ac.jp
_publ_contact_author_fax         +81-791-58-0164
_publ_contact_author_name        'Shin'ichi Nakatsuji'
_publ_contact_author_phone       +81-791-58-0163
_publ_section_title
;
 Azobenzene Derivatives Carrying a Nitroxide Radical
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2021
_journal_page_last               2029
_journal_paper_doi               10.1021/jo062266f
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C33 H48 N3 O4 '
_chemical_formula_sum            'C33 H48 N3 O4'
_chemical_formula_weight         550.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2004-05-27
_audit_creation_method           'by teXsan for Windows v1.06'
_cell_angle_alpha                90
_cell_angle_beta                 100.52(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.973(6)
_cell_length_b                   42.691(9)
_cell_length_c                   12.856(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    303.2
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      10.7
_cell_volume                     3223(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows v1.06 (MSC, 1997-99)'
_computing_publication_material  'teXsan for Windows v1.06 (MSC, 1997-99)'
_computing_structure_refinement  'teXsan for Windows v1.06 (MSC, 1997-99)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      303.2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.10997
_diffrn_orient_matrix_UB_12      0.01786
_diffrn_orient_matrix_UB_13      0.01225
_diffrn_orient_matrix_UB_21      0.09950
_diffrn_orient_matrix_UB_22      -0.01230
_diffrn_orient_matrix_UB_23      0.05656
_diffrn_orient_matrix_UB_31      0.08371
_diffrn_orient_matrix_UB_32      -0.00884
_diffrn_orient_matrix_UB_33      -0.05395
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K'a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.10032
_diffrn_reflns_av_sigmaI/netI    0.372
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6455
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        24.907
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        -0.37
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North,Phillips & Matthews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.957
_refine_ls_goodness_of_fit_ref   1.960
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     361
_refine_ls_number_reflns         994
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/['s^2^(Fo) + 0.00021|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0560
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                994
_reflns_number_total             6205
_reflns_threshold_expression     I>3.00's(I)
_cod_data_source_file            jo062266fsi20070108_061337.cif
_cod_data_source_block           '_7a'
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C33 H48 N3 O4 '
_cod_database_code               4022732