Synthesis of Metal Fullerene Complexes by the Use of Fullerene Halides
Matsuo, Yutaka; Kuninobu, Yoichiro; Muramatsu, Ayako; Sawamura, Masaya; Nakamura, Eiichi; Organometallics 27 (2008) 3403–; doi:10.1021/om8001262

data_4071364
_publ_contact_author             'Matsuo, Y.'
_publ_section_title
;
 Synthesis of Metal Fullerene Complexes by the Use of Fullerene Halides
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3403
_journal_paper_doi               10.1021/om8001262
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C69 H15 O3 Re1 S2'
_chemical_formula_structural     'C69 H15 O3 RE1 S2'
_chemical_formula_sum            'C69 H15 O3 Re S2'
_chemical_formula_weight         1142.13
_chemical_name_systematic
;
 ReC60Me5CO3CS2
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 122.842(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.9090(10)
_cell_length_b                   14.7480(7)
_cell_length_c                   19.4810(6)
_cell_measurement_reflns_used    6790
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.23
_cell_measurement_wavelength     0.71073
_cell_volume                     7943.8(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.2108
_diffrn_measured_fraction_theta_max 0.7384
_diffrn_measurement_device_type  'Imaging Plate'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6790
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        NA
_diffrn_standards_interval_count NA
_diffrn_standards_number         NA
_exptl_absorpt_coefficient_mu    3.229
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.91
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.826
_refine_diff_density_min         -3.711
_refine_diff_density_rms         0.292
_refine_ls_extinction_coef       0.0023(2)
_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   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         6790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1515P)^2^+348.9638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2523
_refine_ls_wR_factor_ref         0.2565
_reflns_number_gt                6251
_reflns_number_total             6790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8001262-file001.cif
_cod_data_source_block           ReC60CO3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4071364