Synthesis and Derivatization of Iridium(I) and Iridium(III) Pentamethyl[60]fullerene Complexes
Matsuo, Yutaka; Iwashita, Akihiko; Nakamura, Eiichi; Organometallics 24 (2005) 89–95; doi:10.1021/om049333l

data_4075760
_publ_contact_author             'Matsuo, Yutaka'
_publ_section_title
;
Synthesis and Derivatization of Iridium(I) and Iridium(III) 
Pentamethyl[60]fullerene Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              89
_journal_page_last               95
_journal_paper_doi               10.1021/om049333l
_journal_volume                  24
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C65 H15 I2 Ir1'
_chemical_formula_structural     'C65 H15 I2 Ir1'
_chemical_formula_sum            'C72 H21 I2 Ir O'
_chemical_formula_weight         1347.89
_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             2003-09-19T22:17:19-00:00
_cell_angle_alpha                73.171(5)
_cell_angle_beta                 87.823(6)
_cell_angle_gamma                79.239(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9950(8)
_cell_length_b                   13.5060(13)
_cell_length_c                   17.1450(16)
_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                     2176.1(3)
_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 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7686
_diffrn_reflns_theta_full        25.8
_diffrn_reflns_theta_max         25.8
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    4.543
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.823
_refine_diff_density_min         -3.337
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.0054(9)
_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   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         7686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0821
_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^)+(0.1899P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2646
_reflns_number_gt                5748
_reflns_number_total             7686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049333lsi20040826_055445.cif
_cod_data_source_block           IrC60Me5I2CO
_cod_database_code               4075760