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_4022734
_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 H47 N4 O6'
_chemical_formula_sum            'C33 H47 N4 O6'
_chemical_formula_weight         595.76
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-10-22
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                90
_cell_angle_beta                 105.7235(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.998(3)
_cell_length_b                   34.477(3)
_cell_length_c                   11.1675(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    295
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3334.6(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_molecular_graphics    'teXsan for Windows v1.06 (MSC, 1997-99)'
_computing_publication_material  'teXsan for Windows v1.06 (MSC, 1997-99)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR92 (Altomare, et. al. 1994)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Quantum CCD'
_diffrn_measurement_method       Phi+Omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.185
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25733
_diffrn_reflns_theta_full        25.068
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         1.181
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.3827
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
HIGASHI, T. (1995). Abscor - Empirical Absorption Correction, 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1299
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         2659
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2757
_refine_ls_R_factor_gt           0.1210
_refine_ls_shift/su_max          0.000121
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 12.2 0.169 8.82 4.03 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1048
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0816
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              44
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2659
_reflns_number_total             7203
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            jo062266fsi20070108_061414.cif
_cod_data_source_block           11a_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4022734