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_4071676
_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         'C68.50 H20 Cr1 N1 O2 S3'
_chemical_formula_sum            'C68.5 H20 Cr N O2 S3'
_chemical_formula_weight         1037.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-12-02T13:29:06-00:00
_cell_angle_alpha                80.38
_cell_angle_beta                 75.29
_cell_angle_gamma                66.89
_cell_formula_units_Z            2
_cell_length_a                   10.006
_cell_length_b                   11.455
_cell_length_c                   19.938
_cell_measurement_reflns_used    15828
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.84
_cell_measurement_wavelength     0.71073
_cell_volume                     2027.138
_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    SIR-2002
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6994
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.043(4)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         6994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1710P)^2^+2.1131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2253
_refine_ls_wR_factor_ref         0.2554
_reflns_number_gt                5219
_reflns_number_total             6994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800308n_si_005.cif
_cod_data_source_block           CrNOCS2
_cod_original_cell_volume        2027.1
_cod_original_formula_sum        'C68.50 H20 Cr N O2 S3'
_cod_database_code               4071676