Photochemical Addition of C60 with Siliranes: Synthesis and Characterization of Carbosilylated and Hydrosilylated C60 Derivatives
Junko Nagatsuka; Sachie Sugitani; Masahiro Kako; Tsukasa Nakahodo; Naomi Mizorogi; Midori O. Ishitsuka; Yutaka Maeda; Takahiro Tsuchiya; Takeshi Akasaka; Xingfa Gao; Shigeru Nagase; Journal of the American Chemical Society 132 (2010) 12106–12120; doi:10.1021/ja1049719

data_4102966
_publ_contact_author_address
;Center for Tsukuba Advanced Research Alliance
University of Tsukuba
Tsukuba, Ibaraki 305-8577, Japan
;
_publ_contact_author_email       akasaka@tara.tsukuba.ac.jp
_publ_contact_author_fax         +81-298-53-6409
_publ_contact_author_name        'Takeshi AKASAKA'
_publ_contact_author_phone       +81-298-53-6409
_publ_section_title
;
 Photochemical Addition of C60 with Siliranes: Synthesis and
 Characterization of Carbosilylated and Hydrosilylated C60 Derivatives
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12106
_journal_page_last               12120
_journal_paper_doi               10.1021/ja1049719
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C106 H58 Si '
_chemical_formula_sum            'C106 H58 Si'
_chemical_formula_weight         1359.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.091(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.694(4)
_cell_length_b                   13.366(2)
_cell_length_c                   24.195(4)
_cell_measurement_reflns_used    52224
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6368.8(19)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      100.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61116
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2832.00
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.14
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     965
_refine_ls_number_reflns         14522
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1026P)^2^+9.3504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1833
_reflns_number_gt                12708
_reflns_number_total             14522
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja1049719_si_004.cif
_cod_data_source_block           '_Compound_4b'
_cod_original_cell_volume        6369.0(18)
_cod_original_formula_sum        'C106 H58 Si '
_cod_database_code               4102966