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_4075759
_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         'C67 H15 Ir1 O2'
_chemical_formula_structural     'C67 H15 Ir1 O2'
_chemical_formula_sum            'C67 H15 Ir O2'
_chemical_formula_weight         1043.99
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-09-19T22:40:04-00:00
_cell_angle_alpha                90.003(5)
_cell_angle_beta                 93.525(4)
_cell_angle_gamma                90.001(5)
_cell_formula_units_Z            4
_cell_length_a                   9.9750(10)
_cell_length_b                   23.1470(16)
_cell_length_c                   16.0130(15)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     3690.3(6)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.1053
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12852
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    3.679
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         5.636
_refine_diff_density_min         -3.426
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       0.0002(3)
_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   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         7012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1989P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2306
_refine_ls_wR_factor_ref         0.2921
_reflns_number_gt                3562
_reflns_number_total             7012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049333lsi20040826_055423.cif
_cod_data_source_block           IrC60Me5CO2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075759