Dinuclear iridium complexes ligated by lithium-ion endohedral fullerene Li<sup>+</sup>@C<sub>60</sub>.
Fukushi, Chinari; Komuro, Takashi; Hashimoto, Hisako; Chemical communications (Cambridge, England) 61 (2025) 2273–2276; doi:10.1039/d4cc05485g

data_7134110
_publ_section_title
;
 Dinuclear iridium complexes ligated by lithium-ion endohedral fullerene
 Li<sup>+</sup>@C<sub>60</sub>.
;
_journal_issue                   11
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2273
_journal_page_last               2276
_journal_paper_doi               10.1039/d4cc05485g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C76 H24 I2 Ir2 Li, C2 F6 N O4 S2, C2 H2 Cl4'
_chemical_formula_sum            'C80 H26 Cl4 F6 I2 Ir2 Li N O4 S2'
_chemical_formula_weight         2030.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-10-04
_audit_creation_method
;
Olex2 1.5-ac7-002
(compiled 2024.05.10 svn.r6303ca7c for Rigaku Oxford Diffraction, GUI svn.r6967)
;
_audit_update_record
;
2024-10-10 deposited with the CCDC.	2024-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                115.704(2)
_cell_angle_beta                 97.1726(18)
_cell_angle_gamma                93.7882(18)
_cell_formula_units_Z            2
_cell_length_a                   13.6521(3)
_cell_length_b                   14.7289(3)
_cell_length_c                   16.0559(3)
_cell_measurement_reflns_used    18403
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.2810
_cell_measurement_theta_min      2.0670
_cell_volume                     2860.07(12)
_computing_cell_refinement
;
'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
;
_computing_data_collection
;
'CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)'
;
_computing_data_reduction
;
'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
;
_computing_molecular_graphics    'Olex2 1.5-ac7-002 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-002 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38933
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         2.158
_exptl_absorpt_coefficient_mu    6.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.357
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,1,2,2-tetrachloroethane/diethyl ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.445
_refine_diff_density_min         -3.933
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         10156
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+29.4811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8590
_reflns_number_total             10156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05485g2.cif
_cod_data_source_block           IrI_complex_3
_cod_depositor_comments
'Adding full bibliography for 7134108--7134110.cif.'
_cod_original_cell_volume        2860.07(11)
_cod_database_code               7134110
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.463
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S1A-N1A = S2A-N1A
 1.56 with sigma of 0.01
 S1B-N1B = S2B-N1B
 1.56 with sigma of 0.01
 C77A-F1A = C77A-F2A = C77A-F3A
 1.32 with sigma of 0.01
 C78A-F4A = C78A-F5A = C78A-F6A
 1.32 with sigma of 0.01
 C77B-F1B = C77B-F2B = C77B-F3B
 1.32 with sigma of 0.01
 C78B-F4B = C78B-F5B = C78B-F6B
 1.32 with sigma of 0.01
 S1A-C77A = S2A-C78A
 1.83 with sigma of 0.01
 S1A-O1A = S1A-O2A = S2A-O3A = S2A-O4A
 1.43 with sigma of 0.01
 S1B-C77B = S2B-C78B
 1.83 with sigma of 0.01
 S1B-O1B = S1B-O2B = S2B-O3B = S2B-O4B
 1.43 with sigma of 0.01
 S1A-S2A = S1B-S2B
 2.8 with sigma of 0.01
 O2B-N1B = O4B-N1B
 2.44 with sigma of 0.01
 F1B-F2B = F1B-F3B = F2B-F3B
 2.14 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Li1A \\sim Li1B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
S1B \\sim S2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Cl1A \\sim Cl2A \\sim Cl3A \\sim Cl4A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
Cl1B \\sim Cl2B \\sim Cl3B \\sim Cl4B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
Cl1A \\sim C79A \\sim Cl2A \\sim H79A \\sim C80A \\sim Cl3A \\sim Cl4A \\sim
H80A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
Uanis(Li1A) \\sim Ueq, Uanis(Li1B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C77B) \\sim Ueq, Uanis(C78B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(S1B) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C79B) \\sim Ueq, Uanis(C80B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C77A) = Uanis(C78A)
Uanis(C77B) = Uanis(C78B)
Uanis(N1A) = Uanis(N1B)
Uanis(O1A) = Uanis(O2A) = Uanis(O3A) = Uanis(O4A) = Uanis(O1B) = Uanis(O2B) =
Uanis(O3B) = Uanis(O4B)
Uanis(F1B) = Uanis(F2B) = Uanis(F3B) = Uanis(F4B) = Uanis(F5B) = Uanis(F6B)
Uanis(C79B) = Uanis(C80B)
4. Rigid body (RIGU) restrains
 S1B, S2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1A, Cl2A, Cl3A, Cl4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1B, Cl2B, Cl3B, Cl4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73, C72, C71, C76, C75, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Li1B)=1-FVAR(1)
 Sof(Li1A)=FVAR(1)
 Sof(N1B)=Sof(S1B)=Sof(S2B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(C77B)=
 Sof(C78B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(Cl1A)=
 Sof(Cl2A)=Sof(Cl3A)=Sof(Cl4A)=Sof(C79A)=Sof(H79A)=Sof(C80A)=Sof(H80A)=1-FVAR(2)
 Sof(N1A)=Sof(S1A)=Sof(S2A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(C77A)=
 Sof(C78A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(Cl1B)=
 Sof(Cl2B)=Sof(Cl3B)=Sof(Cl4B)=Sof(C79B)=Sof(H79B)=Sof(C80B)=Sof(H80B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C79A(H79A), C79B(H79B), C80A(H80A), C80B(H80B)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
;
_shelx_res_checksum              63703
_shelx_hkl_checksum              26432
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;