Organic and Organometallic Derivatives of Dihydrogen-Encapsulated [60]Fullerene
Yutaka Matsuo; Hiroyuki Isobe; Takatsugu Tanaka; Yasujiro Murata; Michihisa Murata; Koichi Komatsu; Eiichi Nakamura; Journal of the American Chemical Society 127 (2005) 17148–17149; doi:10.1021/ja056077a

data_4112101
_publ_contact_author             'NAKAMURA, Eiichi'
_publ_contact_author_email       nakamura@chem.s.u-tokyo.ac.jp
_publ_section_title
;
 Organic and Organometallic Derivatives of Dihydrogen-Encapsulated
 [60]Fullerene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17148
_journal_page_last               17149
_journal_paper_doi               10.1021/ja056077a
_journal_volume                  127
_journal_year                    2005
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C96 H31.60 Fe1 S2'
_chemical_formula_sum            'C96 H31.6 Fe S2'
_chemical_formula_weight         1304.68
_chemical_name_systematic
;
 H2FeC60Ph5Cp
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-02-10T11:07:18-00:00
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1670(14)
_cell_length_b                   17.3660(15)
_cell_length_c                   20.5530(8)
_cell_measurement_reflns_used    37937
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.3
_cell_measurement_wavelength     0.71073
_cell_volume                     5413.5(7)
_computing_cell_refinement       Scalepack(HKL)
_computing_data_collection       Xpress(MacScience)
_computing_data_reduction        'Denzo and Scalepack(HKL)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5162
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         2.3
_exptl_absorpt_coefficient_mu    0.42
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       prism
_exptl_crystal_F_000             2662
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.37(3)
_refine_ls_extinction_coef       0.0210(17)
_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   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         5162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1359P)^2^+2.8096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                4529
_reflns_number_total             5162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056077asi20051019_073700.cif
_cod_data_source_block           H2FeC60Ph5
_cod_original_formula_sum        'C96 H31.60 Fe S2'
_cod_database_code               4112101