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_7708603
_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
'C148 H184 Cl2 Ir2 N12 O16, 7.9(C H2 Cl2), 9.7(C H4 O)'
_chemical_formula_sum            'C165.6 H238.6 Cl17.8 Ir2 N12 O25.7'
_chemical_formula_weight         3824.08
_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   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                103.234(2)
_cell_angle_beta                 106.527(2)
_cell_angle_gamma                96.082(2)
_cell_formula_units_Z            1
_cell_length_a                   13.0463(7)
_cell_length_b                   20.2747(12)
_cell_length_c                   20.6481(11)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      2.24
_cell_volume                     5010.6(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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'PHOTON III area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'mixed mode'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83251
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.791
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  0.6482
_exptl_absorpt_correction_T_min  0.5245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1422 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.8092. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       prism
_exptl_crystal_F_000             1978
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, CH3OH'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.402
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         29156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0665P)^2^+11.3535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25258
_reflns_number_total             29156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03579g2.cif
_cod_data_source_block           v854
_cod_original_formula_sum        'C165.60 H238.60 Cl17.80 Ir2 N12 O25.70'
_cod_database_code               7708603
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.737
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C033) = Uanis(C02Y) = Uanis(C02M)
Uanis(C02T) = Uanis(C02Z) = Uanis(C034) = Uanis(C02X)
Uanis(C02I) = Uanis(C02M) = Uanis(C033) = Uanis(C02Y)
3. Others
 Fixed Sof: Cl06(0.85) Cl07(0.85) Cl0A(0.85) Cl(0.85) Cl3(0.75) Cl2(0.75)
 Cl5(0.5) Cl6(0.5) O02L(0.85) H9AA(0.85) C02P(0.85) H4BA(0.85) HH(0.85)
 C02V(0.85) H3BA(0.85) HM(0.85) C035(0.75) H03V(0.75) H03W(0.75) C7(0.5)
 H7A(0.5) H7B(0.5) C9(0.85) H9A(0.85) H9B(0.85) H9C(0.85)
4.a Riding coordinates:
 O02A(H7AA), O02J(H8AA), O02L(H9AA), O02Q(H0BA), O02R(H1BA)
4.b Secondary CH2 refined with riding coordinates:
 C00V(H00A,H00B), C011(H01A,H01B), C01C(H01D,H01E), C01F(H01F,H01G), C01G(H01H,
 H01I), C01H(H01J,H01K), C01O(H01L,H01M), C01Q(H01O,H01Q), C020(H02A,H02B),
 C026(H02F,H02G), C028(H02H,H02I), C02K(H02Z,HB), C02N(H2BA,HE), C02P(H4BA,HH),
 C02V(H3BA,HM), C035(H03V,H03W), C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00X(H00X), C00Y(H00Y), C010(H010), C012(H012), C016(H016),
 C01A(H01C), C01N(H01N), C01P(H01P), C01R(H01R), C01U(H01U), C01W(H01W),
 C023(H023), C024(H024)
4.d Idealised Me refined as rotating group:
 C021(H02C,H02D,H02E), C029(H02J,H02K,H02L), C02C(H02M,H02N,H02O), C02D(H02P,
 H02Q,H02R), C02E(H02S,H02T,H02U), C02F(H02V,H02W,H02X), C02H(H02Y,H,HA),
 C02M(H02,HC,HD), C02O(H0AA,HF,HG), C02S(H1AA,HI,HJ), C02U(H2AA,HK,HL),
 C02W(H3AA,HN,HO), C02X(H4AA,HP,HQ), C02Y(H5AA,HR,HS), C02Z(H6AA,HT,HU),
 C030(H03A,H03B,H03C), C032(H03M,H03N,H03O), C033(H03D,H03E,H03F), C034(H03G,
 H03H,H03I), C036(H03P,H03Q,H03R), C037(H03S,H03T,H03U), C038(H03J,H03K,H03L),
 C9(H9A,H9B,H9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19033
_shelx_fab_checksum              6612
_olex2_submission_special_instructions 'No special instructions were received'