Synthesis, structure and biological activity of nitroxide malonate methanofullerenes.
Gubskaya, Valentina P.; Berezhnaya, Lucia Sh; Gubaidullin, Aidar T.; Faingold, Irina I.; Kotelnikova, Raisa A.; Konovalova, Nina P.; Morozov, Vladimir I.; Litvinov, Igor A.; Nuretdinov, Ildus A.; Organic & biomolecular chemistry 5 (2007) 976–981; doi:10.1039/b617892h

data_7151093
_publ_section_title
;
 Synthesis, structure and biological activity of nitroxide malonate
 methanofullerenes.
;
_journal_issue                   6
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              976
_journal_page_last               981
_journal_paper_doi               10.1039/b617892h
_journal_volume                  5
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C81 H34 N2 O6, 2(C H Cl3)'
_chemical_formula_sum            'C75 H16 Cl6 N2 O6'
_chemical_formula_weight         1369.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 132.09(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.403(9)
_cell_length_b                   17.845(4)
_cell_length_c                   17.218(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5792(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2213
_diffrn_reflns_av_sigmaI/netI    0.5829
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9464
_diffrn_reflns_theta_full        74.26
_diffrn_reflns_theta_max         74.26
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.252
_exptl_absorpt_correction_T_max  0.6623
_exptl_absorpt_correction_T_min  0.6422
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_size_rad          0.1000
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.4209
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1923
_reflns_number_gt                984
_reflns_number_total             5631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b617892h.txt
_cod_data_source_block           gubs7
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7151093