Coordination Complexes of Pentamethylcyclopentadienyl Iridium(III) Diiodide with Tin(II) Phthalocyanine and Pentamethylcyclopentadienyl Iridium(II) Halide with Fullerene C60‒Anions
Konarev, Dmitri V.; Troyanov, Sergey I.; Kuzmin, Alexey V.; Nakano, Yoshiaki; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Saito, Gunzi; Lyubovskaya, Rimma N.; Organometallics 34 (2015) 879–; doi:10.1021/om501210s

data_4085567
_publ_section_title
;
 Coordination Complexes of Pentamethylcyclopentadienyl Iridium(III)
 Diiodide with Tin(II) Phthalocyanine and Pentamethylcyclopentadienyl
 Iridium(II) Halide with Fullerene C60--Anions
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              879
_journal_paper_doi               10.1021/om501210s
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'(C70 H15 I Ir), (C16 H36 N), 0.188(C6 H14), 1.315(C6 H4 CL2)'
_chemical_formula_sum            'C95 H58.88 Cl2.63 I Ir N'
_chemical_formula_weight         1626.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.1347(11)
_cell_length_b                   15.0786(5)
_cell_length_c                   27.3801(10)
_cell_measurement_reflns_used    52345
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.565
_cell_measurement_theta_min      2.346
_cell_volume                     12854.1(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            134071
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         4.018
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_T_max  0.5349
_exptl_absorpt_correction_T_min  0.3698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 - Bruker AXS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             6484
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         2.698
_refine_diff_density_min         -2.920
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.337(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1677
_refine_ls_number_reflns         26159
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+65.0364P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                24968
_reflns_number_total             26159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501210s_si_005.cif
_cod_data_source_block           TBA_PMCpIrIC60_C6H4Cl2
_cod_depositor_comments
'Adding full bibliography for 4085565--4085568.cif.'
_cod_database_code               4085567
_shelx_estimated_absorpt_t_min   0.432
_shelx_estimated_absorpt_t_max   0.549
_shelxl_version_number           2013-2
_shelx_res_checksum              35460
_shelx_hkl_checksum              65911