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_4071674
_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         'C82 H31 Br Mo O3'
_chemical_formula_structural     'C82 H31 Br Mo O3'
_chemical_formula_sum            'C82 H31 Br Mo O3'
_chemical_formula_weight         1239.92
_chemical_name_systematic
;
 MoC60Me5BrCO3
;
_space_group_IT_number           14
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-05-17T17:05:19-00:00
_cell_angle_alpha                90
_cell_angle_beta                 96.709(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6970(17)
_cell_length_b                   19.0670(15)
_cell_length_c                   22.379(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     4956.9(11)
_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 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14797
_diffrn_reflns_theta_full        25.59
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.85
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0000(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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         8839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          2.1
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [0.00000+1.00000exp(0.09(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0756+13.5293*P+(0.0787P)^2^+0.0671sin\q/\l]
 where P = 0.01372Fo^2^ + 0.98628Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                5727
_reflns_number_total             8839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800308n_si_003.cif
_cod_data_source_block           MoBrCO3
_cod_original_cell_volume        4956.9(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071674