Group 6 Metal Complexes of the η5-Pentamethyl[60]fullerene
Matsuo, Yutaka; Iwashita, Akihiko; Nakamura, Eiichi; Organometallics 27 (2008) 4611–; doi:10.1021/om800308n

data_4071675
_publ_contact_author             'Matsuo, Y.'
_publ_section_title
;
 Group 6 Metal Complexes of the \h5-Pentamethyl[60]fullerene
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4611
_journal_paper_doi               10.1021/om800308n
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C65 H15 Br1 Mo1 O2'
_chemical_formula_structural     'C65 H15 BR1 O2 MO1'
_chemical_formula_sum            'C65 H15 Br Mo O2'
_chemical_formula_weight         1003.62
_chemical_name_systematic
;
 MoC60Me5O2Br
;
_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
_audit_creation_date             2003-04-05T21:54:51-00:00
_cell_angle_alpha                90
_cell_angle_beta                 112.160(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.595(3)
_cell_length_b                   9.9180(8)
_cell_length_c                   21.1440(14)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     7301.6(10)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6718
_diffrn_reflns_theta_full        25.81
_diffrn_reflns_theta_max         25.81
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.514
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.8
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.00052(12)
_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   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         6718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0686
_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^)+(0.1290P)^2^+15.5051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                4879
_reflns_number_total             6718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800308n_si_004.cif
_cod_data_source_block           MoO2Br
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4071675