Thermal Carbosilylation of Endohedral Dimetallofullerene La2@Ih-C80 with Silirane
Michio Yamada; Mari Minowa; Satoru Sato; Masahiro Kako; Zdenek Slanina; Naomi Mizorogi; Takahiro Tsuchiya; Yutaka Maeda; Shigeru Nagase; Takeshi Akasaka; Journal of the American Chemical Society 132 (2010) 17953–17960; doi:10.1021/ja108671b

data_4103699
_publ_section_title
;
 Thermal Carbosilylation of Endohedral Dimetallofullerene La2@Ih-C80 with
 Silirane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17953
_journal_page_last               17960
_journal_paper_doi               10.1021/ja108671b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'La2 C112 H42 Si, C6 H14'
_chemical_formula_sum            'C118 H56 La2 Si'
_chemical_formula_weight         1779.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.415(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.097(6)
_cell_length_b                   14.762(7)
_cell_length_c                   34.122(14)
_cell_measurement_reflns_used    23876
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      45.02
_cell_measurement_theta_min      2.80
_cell_volume                     7101(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  IPDSC
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1679
_diffrn_reflns_av_sigmaI/netI    0.2519
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            56924
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.46
_diffrn_source                   synchrotron
_diffrn_source_type              'KEK-PF BL-8B'
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  0.9510
_exptl_absorpt_correction_T_min  0.9165
_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    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.517
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1154
_refine_ls_number_reflns         9775
_refine_ls_number_restraints     985
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.2287
_refine_ls_R_factor_gt           0.1214
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1927P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3428
_refine_ls_wR_factor_ref         0.3680
_reflns_number_gt                3318
_reflns_number_total             9775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108671b_si_002.cif
_cod_data_source_block           100706v3_final
_cod_original_cell_volume        7100(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4103699