Preparation of Azafullerene Derivatives from Fullerene-Mixed Peroxides and Single Crystal X-ray Structures of Azafulleroid and Azafullerene
Gaihong Zhang; Shaohua Huang; Zuo Xiao; Quan Chen; Liangbing Gan; Zheming Wang; Journal of the American Chemical Society 130 (2008) 12614–12615; doi:10.1021/ja805072h

data_4108375
_publ_section_title
;
 Preparation of Azafullerene Derivatives from Fullerene-Mixed Peroxides
 and Single Crystal X-ray Structures of Azafulleroid and Azafullerene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12614
_journal_page_last               12615
_journal_paper_doi               10.1021/ja805072h
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C79.5 H41 N O10 S3'
_chemical_formula_weight         1266.31
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.5385(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0042(3)
_cell_length_b                   19.4639(3)
_cell_length_c                   17.5579(2)
_cell_measurement_reflns_used    45426
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.395
_cell_volume                     5640.88(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1377
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70097
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  1.001
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2612
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         9855
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1600
_refine_ls_R_factor_gt           0.0834
_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^)+(0.1119P)^2^+8.7922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2070
_refine_ls_wR_factor_ref         0.2391
_reflns_number_gt                5299
_reflns_number_total             9855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805072h_si_002.cif
_cod_data_source_block           07may16a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constr.' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        5640.88(14)
_cod_original_formula_sum        'C79.50 H41 N O10 S3'
_cod_database_code               4108375