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_7708601
_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         'C160 H188 Ir2 N16 O8, 2(Cl)'
_chemical_formula_sum            'C160 H188 Cl2 Ir2 N16 O8'
_chemical_formula_weight         2918.55
_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                 106.4790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.2215(6)
_cell_length_b                   20.0567(6)
_cell_length_c                   20.2899(7)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.34
_cell_volume                     9452.0(5)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.40A (?, 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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'PHOTON III area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            mixed-mode
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0543
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45618
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.848
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1576 before and 0.0460 after correction. The Ratio of minimum to maximum transmission is 0.7976. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       plate
_exptl_crystal_F_000             3024
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, MeOH'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         16665
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1021P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11113
_reflns_number_total             16665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03579g2.cif
_cod_data_source_block           v865c1
_cod_database_code               7708601
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.736
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-C6
 2.55 with sigma of 0.02
 C3-C0AA
 2.55 with sigma of 0.02
 C6-C8
 2.55 with sigma of 0.02
 C5-C8
 2.55 with sigma of 0.02
 C0-C0AA
 2.55 with sigma of 0.02
 C0-C3
 2.55 with sigma of 0.02
 C18-C17 = C02C-C028
 1.54 with sigma of 0.01
 C1AA-C0AA \\sim C3-C1AA \\sim C1AA-C0
 with sigma of 0.02
 C7-C6 \\sim C8-C7 \\sim C7-C5
 with sigma of 0.02
 C1AA-C01A \\sim C7-C01A
 with sigma of 0.02
 C4B-C023 \\sim C4A-C023 \\sim C10-C023 \\sim C11-C023 \\sim C12-C023 \\sim
C4-C023
 with sigma of 0.02
 N4-C1C \\sim N4-C9
 with sigma of 0.02
 C9A-C1C \\sim C9B-C9
 with sigma of 0.02
 C19-C01V \\sim C1A-C01V
 with sigma of 0.02
 C9B-C1B \\sim C9A-C20
 with sigma of 0.02
 C02C_$1-C028_$1 \\sim C02K_$1-C02C_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1AA) = Uanis(C3) = Uanis(C0) = Uanis(C0AA) = Uanis(C5) = Uanis(C6) =
Uanis(C7) = Uanis(C8)
Uanis(C017) = Uanis(C01A) = Uanis(C01E) = Uanis(C1AA) = Uanis(C3) = Uanis(C0) =
Uanis(C0AA) = Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(C8)
Uanis(C023) = Uanis(C4) = Uanis(C10) = Uanis(C4B) = Uanis(C11) = Uanis(C4A) =
Uanis(C12)
Uanis(C1A) = Uanis(C1B) = Uanis(C9B) = Uanis(C9) = Uanis(C19) = Uanis(C20) =
Uanis(C9A) = Uanis(C1C)
Uanis(C022) = Uanis(C02F) = Uanis(C025)
Uanis(C01Z) = Uanis(C022) = Uanis(C02F) = Uanis(C025)
Uanis(C13) = Uanis(C17) = Uanis(C18)
Uanis(C028) = Uanis(C02C)
Uanis(O003) = Uanis(C13) = Uanis(C17) = Uanis(C18)
Uanis(O006) = Uanis(C028) = Uanis(C02C) = Uanis(C02K)
4. Others
 Fixed Sof: H01V(0.5) H01A(0.5) C1A(0.5) H1A(0.5) C1B(0.5) H1B(0.5) C9B(0.5)
 H9B(0.5) C9(0.5) H9(0.5) C1AA(0.45) C19(0.5) H19(0.5) C20(0.5) H20(0.5)
 C3(0.45) H3A(0.45) H3B(0.45) H3C(0.45) C4(0.45) H4A(0.45) H4B(0.45) H4C(0.45)
 C0(0.45) H0A(0.45) H0B(0.45) H0C(0.45) C0AA(0.45) H0AA(0.45) H0AB(0.45)
 H0AC(0.45) C10(0.45) H10A(0.45) H10B(0.45) H10C(0.45) C4B(0.45) H4BA(0.45)
 H4BB(0.45) H4BC(0.45) C5(0.55) H5A(0.55) H5B(0.55) H5C(0.55) C6(0.55)
 H6A(0.55) H6B(0.55) H6C(0.55) C7(0.55) C8(0.55) H8A(0.55) H8B(0.55) H8C(0.55)
 C11(0.55) H11A(0.55) H11B(0.55) H11C(0.55) C4A(0.55) H4AA(0.55) H4AB(0.55)
 H4AC(0.55) C12(0.55) H12A(0.55) H12B(0.55) H12C(0.55) C9A(0.5) H9A(0.5)
 C1C(0.5) H1C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00M(H00C,H00D), C00R(H00E,H00F), C00X(H00G,H00H), C00Y(H00J,
 H00L), C014(H01B,H01C), C01F(H01D,H01F), C01H(H01G,H01H), C13(H13A,H13B),
 C028(H02M,H02N), C02C(H02R,H02S), C17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C01V(H01V), C01V(H01A), C1A(H1A), C1B(H1B), C9B(H9B), C9(H9), C00I(H00I),
 C00K(H00K), C00P(H00P), C00Q(H00Q), C00T(H00T), C00U(H00U), C012(H012),
 C013(H013), C017(H017), C01E(H01E), C01I(H01I), C01J(H01J), C01K(H01K),
 C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01R(H01R),
 C01U(H01U), C01Y(H01Y), C021(H021), C024(H024), C19(H19), C20(H20), C9A(H9A),
 C1C(H1C)
5.c Fitted hexagon refined as free rotating group:
 N4(C01V,C1A,C1B,C9B,C9)
5.d Idealised Me refined as rotating group:
 C022(H02A,H02B,H02C), C025(H02D,H02E,H02F), C026(H02G,H02H,H02I), C027(H02J,
 H02K,H02L), C02B(H02O,H02P,H02Q), C02F(H02T,H02U,H02V), C3(H3A,H3B,H3C),
 C4(H4A,H4B,H4C), C0(H0A,H0B,H0C), C02K(H02W,H02X,H02Y), C0AA(H0AA,H0AB,H0AC),
 C10(H10A,H10B,H10C), C4B(H4BA,H4BB,H4BC), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C4A(H4AA,H4AB,H4AC), C12(H12A,H12B,H12C),
  C18(H18A,H18B,H18C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57243
_shelx_fab_checksum              97811
_olex2_submission_special_instructions 'No special instructions were received'