Synthesis of [59]Fullerenones through Peroxide-Mediated Stepwise Cleavage of Fullerene Skeleton Bonds and X-ray Structures of Their Water-Encapsulated Open-Cage Complexes
Zuo Xiao; Jiayao Yao; Dazhi Yang; Fudong Wang; Shaohua Huang; Liangbing Gan; Zhenshan Jia; Zhongping Jiang; Xiaobing Yang; Bo Zheng; Gu Yuan; Shiwei Zhang; Zheming Wang; Journal of the American Chemical Society 129 (2007) 16149–16162; doi:10.1021/ja0763798

data_4110311
_publ_section_title
;
 Synthesis of [59]Fullerenones through Peroxide-Mediated Stepwise Cleavage
 of Fullerene Skeleton Bonds and X-ray Structures of Their
 Water-Encapsulated Open-Cage Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16149
_journal_page_last               16162
_journal_paper_doi               10.1021/ja0763798
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C72 H18 Br Cl2 N O8 S2'
_chemical_formula_weight         1239.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.253(2)
_cell_angle_beta                 85.787(2)
_cell_angle_gamma                88.3700(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6078(3)
_cell_length_b                   14.2697(4)
_cell_length_c                   14.6697(4)
_cell_measurement_reflns_used    19575
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2419.78(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0996
_diffrn_reflns_av_sigmaI/netI    0.1304
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33555
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.746
_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    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0028(4)
_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   0.914
_refine_ls_hydrogen_treatment    constraint
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         8508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0604P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                4313
_reflns_number_total             8508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0763798si20070823_053219.cif
_cod_data_source_block           07jun06a-200K
_cod_database_code               4110311