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_7708604
_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
'C140 H168 Cl2 Ir2 N12 O8, 6.5(C2 H4 Cl2), 2(C H2 Cl2)'
_chemical_formula_sum            'C155 H198 Cl19 Ir2 N12 O8'
_chemical_formula_weight         3415.19
_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                 103.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6360(13)
_cell_length_b                   13.1399(6)
_cell_length_c                   34.199(2)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.38
_cell_volume                     8587.1(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'PHOTON II area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0952
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            97984
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.200
_diffrn_reflns_theta_max         25.200
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1375 before and 0.0685 after correction. The Ratio of minimum to maximum transmission is 0.8167. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       needle
_exptl_crystal_F_000             3506
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, C2H4Cl2'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.815
_refine_diff_density_min         -2.568
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         15109
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0741
_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^)+(0.0758P)^2^+102.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11175
_reflns_number_total             15109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03579g2.cif
_cod_data_source_block           v839e
_cod_original_cell_volume        8587.0(9)
_cod_database_code               7708604
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.556
_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, All C(H,H,H,H,H,
  H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C028 = C02Z-C028 = C032-C02Z = C21-C20
 1.54 with sigma of 0.02
 Cl00-C02M \\sim Cl8-C02M \\sim Cl-C02I \\sim Cl7-C02I \\sim Cl10-C02I \\sim
Cl6-C02I
 with sigma of 0.01
 C0AA-C02A \\sim C3-C02A \\sim C18B-C02A
 with sigma of 0.01
 C02Z-C028 \\sim C21-C028 \\sim C21-C20 \\sim C032-C02Z
 with sigma of 0.01
 C0AA-C02A \\sim C4-C02A \\sim C5-C02A \\sim C3-C02A \\sim C18A-C02A \\sim
C18B-C02A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl) = Uanis(Cl7) = Uanis(Cl10) = Uanis(Cl6)
Uanis(C02M) = Uanis(Cl00) = Uanis(Cl8) = Uanis(C02I) = Uanis(Cl6) = Uanis(Cl7)
= Uanis(Cl10) = Uanis(Cl)
Uanis(C12) = Uanis(C1AA) = Uanis(C0) = Uanis(C13) = Uanis(C9) = Uanis(C7)
Uanis(C028) = Uanis(C21) = Uanis(C20) = Uanis(C032) = Uanis(C02Z)
Uanis(C4) = Uanis(C0AA) = Uanis(C18B) = Uanis(C18A) = Uanis(C3) = Uanis(C5)
Uanis(C02G) = Uanis(C02F)
Uanis(C02N) = Uanis(Cl03)
Uanis(C011) = Uanis(C00O) = Uanis(N2) = Uanis(N00E) = Uanis(N00M)
Uanis(C2) = Uanis(C00N) = Uanis(C00P)
Uanis(C018) = Uanis(C01M) = Uanis(C013)
Uanis(C02A) = Uanis(C4) = Uanis(C0AA) = Uanis(C18B) = Uanis(C18A) = Uanis(C3) =
Uanis(C5)
4. Others
 Fixed Sof: Cl00(0.75) Cl(0.25) H02K(0.5) H02L(0.5) H02I(0.5) H02J(0.5)
 HB(0.25) H2AA(0.25) HC(0.25) HD(0.25) HE(0.25) HF(0.25) HG(0.25) HH(0.25)
 C12(0.75) H12A(0.75) H12B(0.75) H12C(0.75) H3AA(0.75) HI(0.75) HJ(0.25)
 HK(0.25) C1AA(0.75) H1AA(0.75) H1AB(0.75) H1AC(0.75) C0(0.75) H0A(0.75)
 H0B(0.75) H0C(0.75) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C02Z(0.5) H02(0.5)
 HO(0.5) C032(0.5) H03A(0.5) H03B(0.5) H03C(0.5) Cl8(0.25) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C21(0.5) H21A(0.5) H21B(0.5) C18B(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) Cl6(0.25) Cl7(0.25) Cl10(0.25)
 C13(0.25) H13A(0.25) H13B(0.25) H13C(0.25) C9(0.25) H9A(0.25) H9B(0.25)
 H9C(0.25) C7(0.25) H7A(0.25) H7B(0.25) H7C(0.25) C4(0.5) H4A(0.5) H4B(0.5)
 H4C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C18A(0.5) H18D(0.5) H18E(0.5)
 H18F(0.5) Cl0A(0.75) Cl2(0.75) C6(0.75) H6A(0.75) H6B(0.75) C8(0.75) H8A(0.75)
 H8B(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00B), C00Y(H00C,H00D), C010(H01A,H01B), C017(H01C,H01D), C018(H01E,
 H01F), C01T(H01S,H01T), C01X(H01U,H01W), C01Z(H01X,H01Y), C020(H02A,H02B),
 C028(H02K,H02L), C028(H02I,H02J), C02C(H02M,H02N), C02D(H02O,H02P), C02F(H4AA,
 H), C02G(H5AA,HA), C02I(HB,H2AA), C02I(HC,HD), C02I(HE,HF), C02I(HG,HH),
 C02M(H3AA,HI), C02M(HJ,HK), C02N(H6AA,HL), C02Z(H02,HO), C21(H21A,H21B),
 C6(H6A,H6B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00R(H00R), C00S(H00S), C00W(H00W), C011(H011), C014(H014),
 C016(H016), C01A(H01G), C01B(H01H), C01D(H01I), C01G(H01J), C01I(H01K),
 C01J(H01L), C01L(H01M), C01P(H01Q), C01R(H01R), C01V(H01V), C025(H025)
5.c Idealised Me refined as rotating group:
 C01O(H01N,H01O,H01P), C021(H02C,H02D,H02E), C024(H02F,H02G,H02H), C02E(H02Q,
 H02R,H02S), C02K(H02T,H02U,H02V), C12(H12A,H12B,H12C), C02O(H02W,H02X,H02Y),
 C1AA(H1AA,H1AB,H1AC), C0(H0A,H0B,H0C), C02U(H02Z,HM,HN), C0AA(H0AA,H0AB,H0AC),
 C032(H03A,H03B,H03C), C20(H20A,H20B,H20C), C18B(H18A,H18B,H18C), C3(H3A,H3B,
 H3C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C18A(H18D,H18E,H18F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63410
_shelx_fab_checksum              7760
_olex2_submission_special_instructions 'No special instructions were received'