Inherently dinuclear iridium(III) meso architectures accessed by cyclometalation of calix[4]arene-based bis(aryltriazoles)
Bezzubov, Stanislav; Ermolov, Kirill; Gorbunov, Alexander; Kalle, Paulina; Lentin, Ivan; Latyshev, Gennadij; Kovalev, Vladimir; Vatsouro, Ivan; Dalton Transactions  (2021) –; doi:10.1039/D1DT03579G

data_7708600
_publ_section_title
;
 Inherently dinuclear iridium(III) meso architectures accessed by
 cyclometalation of calix[4]arene-based bis(aryltriazoles)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03579G
_journal_year                    2021
_chemical_formula_moiety         'C164 H184 Ir2 N16 O8, 2(Cl), 2(C H2 Cl2)'
_chemical_formula_sum            'C166 H188 Cl6 Ir2 N16 O8'
_chemical_formula_weight         3132.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2021-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.424(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.9988(10)
_cell_length_b                   16.5267(8)
_cell_length_c                   29.1477(13)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    148.0
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.22
_cell_volume                     9553.0(8)
_computing_cell_refinement       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'PHOTON III area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            mixed-mode
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            44998
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.633
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0888 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.6649. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.116
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         16802
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0721P)^2^+55.2001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1673
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11655
_reflns_number_total             16802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03579g2.cif
_cod_data_source_block           v864_full
_cod_database_code               7708600
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.730
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C0 = C1AA-C0AA
 1.54 with sigma of 0.01
 C1AA-C022 \\sim C022-C0
 with sigma of 0.02
 C6-C02E \\sim C9-C02E \\sim C7-C02E \\sim C4-C02E \\sim C5-C02E \\sim C8-C02E
 with sigma of 0.02
 C21-C10B \\sim C22-C10B
 with sigma of 0.02
 C21-C10B \\sim C22-C10B \\sim C10-C10B
 with sigma of 0.02
 C13-C02C \\sim C16-C02C \\sim C14-C02C \\sim C11-C02C \\sim C12-C02C \\sim
C15-C02C
 with sigma of 0.02
 C1D-C1B \\sim C20-C18 \\sim C20-C17 \\sim C1D-C1A \\sim C1D-C1C \\sim C20-C19
 with sigma of 0.02
 C20-C021 \\sim C1D-C021
 with sigma of 0.02
 C1E-C10A \\sim C21-C10B \\sim C10B-C10 \\sim C10A-C1F \\sim C1G-C10A \\sim
C22-C10B
 with sigma of 0.02
 C10A-C017 \\sim C10B-C017
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C0) = Uanis(C1AA) = Uanis(C0AA) = Uanis(C3)
Uanis(C1AA) = Uanis(C0) = Uanis(C0AA) = Uanis(C3) = Uanis(C022)
Uanis(C8) = Uanis(C5) = Uanis(C4) = Uanis(C7) = Uanis(C9) = Uanis(C6)
Uanis(C15) = Uanis(C12) = Uanis(C11) = Uanis(C14) = Uanis(C16) = Uanis(C13)
Uanis(C1A) = Uanis(C17) = Uanis(C1B) = Uanis(C18) = Uanis(C1C) = Uanis(C19) =
Uanis(C1D) = Uanis(C20)
Uanis(C10B) = Uanis(C21) = Uanis(C22) = Uanis(C10) = Uanis(C1E) = Uanis(C10A) =
Uanis(C1F) = Uanis(C1G)
Uanis(Cl03) = Uanis(Cl00)
4. Others
 Fixed Sof: H02C(0.4) H02D(0.4) H02A(0.6) H02B(0.6) C20(0.63) C13(0.6)
 H13A(0.6) H13B(0.6) H13C(0.6) C10B(0.63) C0(0.4) H0A(0.4) H0B(0.4) C4(0.5)
 H4A(0.5) H4B(0.5) H4C(0.5) C0AA(0.6) H0AA(0.6) H0AB(0.6) H0AC(0.6) C12(0.6)
 H12A(0.6) H12B(0.6) H12C(0.6) C18(0.63) H18A(0.63) H18B(0.63) H18C(0.63)
 C17(0.63) H17A(0.63) H17B(0.63) H17C(0.63) C21(0.63) H21A(0.63) H21B(0.63)
 H21C(0.63) C11(0.4) H11A(0.4) H11B(0.4) H11C(0.4) C5(0.5) H5A(0.5) H5B(0.5)
 H5C(0.5) C22(0.63) H22A(0.63) H22B(0.63) H22C(0.63) C19(0.63) H19A(0.63)
 H19B(0.63) H19C(0.63) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C1AA(0.6) H1AA(0.6)
 H1AB(0.6) C3(0.4) H3A(0.4) H3B(0.4) H3C(0.4) C7(0.5) H7A(0.5) H7B(0.5)
 H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5)
 C10(0.63) H10A(0.63) H10B(0.63) H10C(0.63) C14(0.6) H14A(0.6) H14B(0.6)
 H14C(0.6) C15(0.4) H15A(0.4) H15B(0.4) H15C(0.4) C16(0.4) H16A(0.4) H16B(0.4)
 H16C(0.4) C1A(0.37) H1AC(0.37) H1AD(0.37) H1AE(0.37) C1B(0.37) H1BA(0.37)
 H1BB(0.37) H1BC(0.37) C1C(0.37) H1CA(0.37) H1CB(0.37) H1CC(0.37) C1D(0.37)
 C1E(0.37) H1EA(0.37) H1EB(0.37) H1EC(0.37) C10A(0.37) C1F(0.37) H1FA(0.37)
 H1FB(0.37) H1FC(0.37) C1G(0.37) H1GA(0.37) H1GB(0.37) H1GC(0.37)
5.a Secondary CH2 refined with riding coordinates:
 C00K(H00A,H00B), C00R(H00C,H00D), C00Y(H00E,H00F), C018(H01A,H01B), C01C(H01E,
 H01F), C01F(H01H,H01I), C01H(H01K,H01L), C01K(H01Q,H01R), C01S(H01T,H01U),
 C01U(H01W,H01X), C022(H02C,H02D), C022(H02A,H02B), C0(H0A,H0B), C02L(H02G,
 H02H), C1AA(H1AA,H1AB)
5.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00O(H00O), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00W(H00W), C00Z(H00Z), C010(H010), C011(H011), C01A(H01C), C01B(H01D),
 C01E(H01G), C01G(H01J), C01I(H01M), C01L(H01S), C01T(H01V), C01V(H01Y),
 C01W(H01Z), C01Z(H01), C020(H020), C023(H023), C025(H025), C026(H026),
 C02A(H02E), C02D(H02F)
5.c Idealised Me refined as rotating group:
 C01J(H01N,H01O,H01P), C13(H13A,H13B,H13C), C4(H4A,H4B,H4C), C0AA(H0AA,H0AB,
 H0AC), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C21(H21A,
 H21B,H21C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C),
 C19(H19A,H19B,H19C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C1A(H1AC,H1AD,H1AE), C1B(H1BA,H1BB,H1BC),
 C1C(H1CA,H1CB,H1CC), C1E(H1EA,H1EB,H1EC), C1F(H1FA,H1FB,H1FC), C1G(H1GA,H1GB,
 H1GC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86965
_shelx_fab_checksum              95957
_olex2_submission_special_instructions 'No special instructions were received'