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_4071673
_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         'C68 H15 Mo1 N1 O3 S2'
_chemical_formula_sum            'C68 H15 Mo N O3 S2'
_chemical_formula_weight         1053.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-07-17T11:07:14-00:00
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.280(4)
_cell_length_b                   14.9930(10)
_cell_length_c                   19.193(3)
_cell_measurement_reflns_used    51451
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.24
_cell_measurement_wavelength     0.71073
_cell_volume                     7850.1(18)
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6548
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.324
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.378
_refine_ls_extinction_coef       0.073(7)
_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   1.769
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         6548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.769
_refine_ls_R_factor_all          0.1773
_refine_ls_R_factor_gt           0.1567
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4176
_refine_ls_wR_factor_ref         0.4396
_reflns_number_gt                4733
_reflns_number_total             6548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800308n_si_002.cif
_cod_data_source_block           MoNoCO2
_cod_database_code               4071673