Synthesis of Fullerene Oxides Containing Both 6,6-Closed Epoxide and 5,6-Open Ether Moieties through Thermolysis of Fullerene Peroxides
Jiayao Yao; Dazhi Yang; Zuo Xiao; Liangbing Gan; Zheming Wang; Journal of Organic Chemistry 74 (2009) 3528–3531; doi:10.1021/jo9000977

data_4024489
_publ_section_title
;
Synthesis of Fullerene Oxides Containing Both 6,6-Closed Epoxide and
5,6-Open Ether Moieties through Thermolysis of Fullerene Peroxides
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3528
_journal_page_last               3531
_journal_paper_doi               10.1021/jo9000977
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C79 H49 Cl9 D3 N O16'
_chemical_formula_weight         1593.27
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 117.0560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9150(2)
_cell_length_b                   25.7935(4)
_cell_length_c                   22.4441(4)
_cell_measurement_reflns_used    86487
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      3.41
_cell_volume                     7174.0(2)
_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(2)
_diffrn_detector_area_resol_mean 9
_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  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86487
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.41
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.699
_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    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.265
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         12699
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.260
_refine_ls_R_factor_all          0.1854
_refine_ls_R_factor_obs          0.1066
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2392P)^2^+2.0006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3733
_refine_ls_wR_factor_obs         0.3136
_reflns_number_observed          6517
_reflns_number_total             12699
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jo9000977_si_003.cif
_cod_data_source_block           07jun08a
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2392P)^2^+2.0006P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2392P)^2^+2.0006P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

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_sg_symbol_H-M      'P 2(1)/c'
_cod_original_formula_sum        'C79 H49 D3 Cl9 N O16'
_cod_database_code               4024489