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_7708602
_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 H184 Ir2 N16 O8, 2(Cl), 3.7(H2 O), 5.4(C2 H6 O)'
_chemical_formula_sum            'C170.8 H223.8 Cl2 Ir2 N16 O17.1'
_chemical_formula_weight         3229.94
_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   mixed
_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                 102.2470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.3502(10)
_cell_length_b                   18.8077(8)
_cell_length_c                   20.2321(7)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.33
_cell_volume                     9054.9(6)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'PHOTON III area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'mixed mode'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '3-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  0.1474
_diffrn_reflns_av_unetI/netI     0.1404
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78627
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.040
_diffrn_reflns_theta_max         25.040
_diffrn_reflns_theta_min         2.025
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1101 before and 0.0693 after correction. The Ratio of minimum to maximum transmission is 0.7175. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             3371
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, C2H5OH, H2O'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.601
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         15966
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0937P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8695
_reflns_number_total             15966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03579g2.cif
_cod_data_source_block           v860de
_cod_original_formula_sum        'C170.80 H223.80 Cl2 Ir2 N16 O17.10'
_cod_database_code               7708602
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.835
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C1A-C19
 2.55 with sigma of 0.02
 C16-C17
 2.55 with sigma of 0.02
 C18-C1A
 2.55 with sigma of 0.02
 O02P-C02I
 1.46 with sigma of 0.02
 C3-C1AA
 1.54 with sigma of 0.02
 C02S-C02I
 1.54 with sigma of 0.02
 O3-C1AA
 1.46 with sigma of 0.02
 O3-C3
 2.5 with sigma of 0.02
 C1E-C6
 2.55 with sigma of 0.02
 O004-C5 \\sim O004-C0
 with sigma of 0.02
 N00D-C7 \\sim N00D-C4
 with sigma of 0.02
 C5-C4 \\sim C7-C0
 with sigma of 0.02
 O003-C8 \\sim O003-C12
 with sigma of 0.02
 C9-C10 \\sim C14-C13
 with sigma of 0.02
 C9-C12 \\sim C8-C13
 with sigma of 0.02
 C9-C14 \\sim C13-C10
 with sigma of 0.02
 C18-C01P \\sim C15-C01P \\sim C19-C01P \\sim C16-C01P \\sim C17-C01P \\sim
C1A-C01P
 with sigma of 0.02
 C22-C028 \\sim C1D-C028 \\sim C21-C028 \\sim C1C-C028 \\sim C1B-C028 \\sim
C20-C028
 with sigma of 0.02
 C24-C026 \\sim C6A-C026 \\sim C25-C026 \\sim C1E-C026 \\sim C23-C026 \\sim
C6-C026
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C10) = Uanis(C13) = Uanis(C9) = Uanis(C8) = Uanis(C12)
Uanis(C18) = Uanis(C15) = Uanis(C19) = Uanis(C16) = Uanis(C17) = Uanis(C1A)
Uanis(C1D) = Uanis(C22) = Uanis(C20) = Uanis(C1B) = Uanis(C1C) = Uanis(C21)
Uanis(O1) = Uanis(C0AA) = Uanis(C11)
Uanis(O3) = Uanis(C1AA) = Uanis(C3)
Uanis(C02S) = Uanis(C02I) = Uanis(O02P)
Uanis(C4) = Uanis(C7)
Uanis(C25) = Uanis(C1E) = Uanis(C23) = Uanis(C6) = Uanis(C24) = Uanis(C6A)
4. Others
 Fixed Sof: C0(0.75) H0A(0.75) H0B(0.75) O01Z(0.85) H01R(0.85) H01S(0.85)
 C4(0.25) H4A(0.25) H4B(0.25) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C10(0.65)
 H10A(0.65) H10B(0.65) H10C(0.65) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
 C8(0.65) H8A(0.65) H8B(0.65) C02I(0.85) H02S(0.85) H02T(0.85) C22(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) C9(0.35) H9A(0.35) H9B(0.35) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) O02P(0.85) H02U(0.85) C21(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C02S(0.85) H02V(0.85)
 H02W(0.85) H02X(0.85) O1(0.45) H1(0.45) C0AA(0.45) H0AA(0.45) H0AB(0.45)
 C11(0.45) H11A(0.45) H11B(0.45) H11C(0.45) C1AA(0.4) H1AD(0.4) H1AE(0.4)
 O3(0.4) H3(0.4) C3(0.4) H3A(0.4) H3B(0.4) H3C(0.4) C5(0.25) H5A(0.25)
 H5B(0.25) C7(0.75) H7A(0.75) H7B(0.75) C12(0.35) H12A(0.35) H12B(0.35)
 C13(0.65) H13A(0.65) H13B(0.65) C14(0.35) H14A(0.35) H14B(0.35) H14C(0.35)
 C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5)
 C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5)
 C1C(0.5) H1CA(0.5) H1CB(0.5) H1CC(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
 C6(0.6) H6A(0.6) H6B(0.6) H6C(0.6) C1E(0.6) H1EA(0.6) H1EB(0.6) H1EC(0.6)
 C6A(0.6) H6AA(0.6) H6AB(0.6) H6AC(0.6) C25(0.4) H25A(0.4) H25B(0.4) H25C(0.4)
 C24(0.4) H24A(0.4) H24B(0.4) H24C(0.4) C23(0.4) H23A(0.4) H23B(0.4) H23C(0.4)
5.a Riding coordinates:
 O00J(H00G,H00H), O012(H012), O01Z(H01R,H01S), O02P(H02U), O1(H1), O3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B), C00N(H00C,H00D), C00R(H00E,H00F), C019(H01A,H01B), C01A(H01C,
 H01D), C01R(H01H,H01L), C0(H0A,H0B), C4(H4A,H4B), C029(H02A,H02B), C02A(H02C,
 H02D), C02B(H02N,H02O), C8(H8A,H8B), C02I(H02S,H02T), C9(H9A,H9B), C0AA(H0AA,
 H0AB), C1AA(H1AD,H1AE), C5(H5A,H5B), C7(H7A,H7B), C12(H12A,H12B), C13(H13A,
 H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X), C010(H010), C011(H011),
 C013(H013), C015(H015), C017(H017), C01B(H01E), C01D(H01F), C01G(H01G),
 C01I(H01I), C01J(H01J), C01K(H01K), C01N(H01N), C01Q(H01Q), C01U(H01U),
 C01V(H01V), C01W(H01W), C020(H020), C021(H021), C023(H023), C024(H024),
 C025(H025), C027(H027)
5.d Idealised Me refined as rotating group:
 C01T(H01M,H01O,H01P), C17(H17A,H17B,H17C), C02D(H02E,H02F,H02G), C02E(H02H,
 H02I,H02J), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C),
 C02K(H02K,H02L,H02M), C02L(H02P,H02Q,H02R), C16(H16A,H16B,H16C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C02S(H02V,H02W,H02X), C11(H11A,H11B,H11C), C3(H3A,
 H3B,H3C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,
 H1DC), C6(H6A,H6B,H6C), C1E(H1EA,H1EB,H1EC), C6A(H6AA,H6AB,H6AC), C25(H25A,
 H25B,H25C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4802
_shelx_fab_checksum              39419
_olex2_submission_special_instructions 'No special instructions were received'