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_7708605
_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
'C188 H200 Ir2 N16 O8, 2(Cl), 2(C H2 Cl2), C4 H10 O'
_chemical_formula_sum            'C194 H214 Cl6 Ir2 N16 O9'
_chemical_formula_weight         3510.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5551(9)
_cell_length_b                   21.0953(7)
_cell_length_c                   33.6113(9)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.28
_cell_volume                     19537.7(10)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'PHOTON III area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'mixed mode'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0528
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            94035
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         1.765
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0837 before and 0.0481 after correction. The Ratio of minimum to maximum transmission is 0.7545. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       plate
_exptl_crystal_F_000             7272
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, EtOEt'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.399
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.309(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2026
_refine_ls_number_reflns         34200
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0633P)^2^+35.5769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.963
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                27481
_reflns_number_total             34200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03579g2.cif
_cod_data_source_block           v872b
_cod_database_code               7708605
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.691(7)
 0.309(7)
2. 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
3. Restrained distances
 C16-C2AA
 2.6 with sigma of 0.02
 C12-C8B
 2.55 with sigma of 0.02
 C1AA-C12
 2.55 with sigma of 0.02
 C05A-C05X
 1.54 with sigma of 0.02
 C5AA-C05N \\sim C11-C05N \\sim C3A-C05N \\sim C3B-C05N \\sim C05N-C3AA \\sim
C9-C05N
 with sigma of 0.02
 C8B-C064 \\sim C5-C064 \\sim C1AA-C064
 with sigma of 0.02
 C043-C0 \\sim C043-C16 \\sim C043-C13 \\sim C043-C4AA \\sim C043-C14 \\sim
C043-C2AA
 with sigma of 0.02
 C12B-C05Q \\sim C12A-C05Q \\sim C05Q-C17 \\sim C05Q-C6 \\sim C05Q-C7 \\sim
C05Q-C18
 with sigma of 0.02
 C1AA-C064 \\sim C0AA-C064 \\sim C064-C12 \\sim C064-C5 \\sim C8B-C064 \\sim
C8A-C064
 with sigma of 0.02
 C06H-C06F \\sim C06I-C06C
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C3AA) = Uanis(C3B) = Uanis(C3A) = Uanis(C5AA) = Uanis(C11)
Uanis(C13) = Uanis(C4AA) = Uanis(C14) = Uanis(C2AA) = Uanis(C0) = Uanis(C16)
Uanis(C12A) = Uanis(C12B) = Uanis(C18) = Uanis(C7) = Uanis(C6) = Uanis(C17)
Uanis(C1AA) = Uanis(C0AA) = Uanis(C12) = Uanis(C5) = Uanis(C8B) = Uanis(C8A)
Uanis(C06I) = Uanis(C06C)
Uanis(C05Y) = Uanis(C04T) = Uanis(C06G)
Uanis(C04E) = Uanis(C04F) = Uanis(C02W)
Uanis(C05Q) = Uanis(C12B) = Uanis(C12A) = Uanis(C17) = Uanis(C6) = Uanis(C7) =
Uanis(C18)
Uanis(C064) = Uanis(C5) = Uanis(C12) = Uanis(C0AA) = Uanis(C1AA) = Uanis(C8A) =
Uanis(C8B)
5. Others
 Fixed Sof: C0(0.66) H0A(0.66) H0B(0.66) H0C(0.66) C3AA(0.5) H3AB(0.5)
 H3AC(0.5) H3AD(0.5) C4AA(0.34) H4AB(0.34) H4AC(0.34) H4AD(0.34) C5AA(0.5)
 H5AB(0.5) H5AC(0.5) H5AD(0.5) C2AA(0.34) H2AB(0.34) H2AC(0.34) H2AD(0.34)
 C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5) C12B(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C3B(0.5)
 H3BA(0.5) H3BB(0.5) H3BC(0.5) C8B(0.5) H8BA(0.5) H8BB(0.5) H8BC(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) H9C(0.5) C3A(0.5) H3AE(0.5) H3AF(0.5) H3AG(0.5) C11(0.5)
 H11A(0.5) H11B(0.5) H11C(0.5) C1AA(0.5) H1AB(0.5) H1AC(0.5) H1AD(0.5)
 C13(0.66) H13A(0.66) H13B(0.66) H13C(0.66) C14(0.66) H14A(0.66) H14B(0.66)
 H14C(0.66) C16(0.34) H16A(0.34) H16B(0.34) H16C(0.34) C12A(0.5) H12D(0.5)
 H12E(0.5) H12F(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C0AA(0.5) H0AB(0.5) H0AC(0.5) H0AD(0.5) C8A(0.5) H8AB(0.5)
 H8AC(0.5) H8AD(0.5) C12(0.5) H12G(0.5) H12H(0.5) H12I(0.5)
 Fixed X: Ir1(0.21197)
 Fixed Y: Ir1(0.29994)
 Fixed Z: Ir1(0.55842)
6.a Secondary CH2 refined with riding coordinates:
 C013(H01A,H01B), C016(H01C,H01D), C017(H01E,H01F), C01B(H01G,H01H), C01X(H01R,
 H01S), C029(H02A,H02B), C02R(H02G,H02H), C035(H03A,H03B), C038(H03C,H03D),
 C03D(H03F,H03G), C03K(H03I,H03K), C03R(H03L,H03O), C03T(H03P,H03Q), C041(H04A,
 H04B), C04J(H04M,H04N), C04K(H04O,H04P), C04N(H04T,H04U), C04Q(H04X,H04Y),
 C04U(H0AA,HB), C050(H05A,H05B), C05G(H05N,H05O), C05M(H05T,H05U), C05T(H05,HC),
  C05V(H9AA,HD), C05X(H6AA,HE), C069(H06U,H06V), C06H(H06Q,H06R), C06I(H06S,
 H06T)
6.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C1AA(H1AB,H1AC,H1AD), C12A(H12D,H12E,H12F), C0AA(H0AB,H0AC,
 H0AD)
6.c Aromatic/amide H refined with riding coordinates:
 C012(H012), C01C(H01I), C01D(H01J), C01F(H01K), C01I(H01L), C01M(H01M),
 C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01U(H01U), C023(H023),
 C024(H024), C028(H028), C02A(H02C), C02C(H02D), C02D(H02E), C02F(H02F),
 C02L(H02L), C02M(H02M), C02N(H02N), C02O(H02O), C02P(H02P), C02S(H02S),
 C02Z(H02Z), C030(H030), C031(H031), C033(H033), C036(H036), C03A(H03E),
 C03G(H03H), C03J(H03J), C03M(H03M), C03N(H03N), C03S(H03S), C03U(H03U),
 C03W(H03W), C03X(H03X), C03Y(H03Y), C044(H044), C046(H046), C047(H047),
 C048(H048), C049(H049), C04B(H04C), C04D(H04D), C04H(H04K), C04I(H04L),
 C04O(H04V), C04P(H04W), C04R(H04Z), C04W(H1AA), C04X(H2AA), C04Y(H3AA),
 C04Z(H4AA), C052(H052), C054(H054), C055(H055), C056(H056), C057(H057),
 C05D(H05L), C05E(H05M), C05K(H05S), C05P(H05Y), C05S(H05Z), C05W(H5AA),
 C05Z(H8AA), C06B(H06G)
6.d Idealised Me refined as rotating group:
 C02T(H02I,H02J,H02K), C02V(H02Q,H02R,H02T), C02W(H02U,H02V,H02W), C04E(H04E,
 H04F,H04G), C04F(H04H,H04I,H04J), C04L(H04Q,H04R,H04S), C04T(H04,H,HA),
 C059(H05C,H05D,H05E), C05A(H05F,H05G,H05H), C05C(H05I,H05J,H05K), C05H(H05P,
 H05Q,H05R), C05O(H05V,H05W,H05X), C0(H0A,H0B,H0C), C05Y(H7AA,HF,HG), C061(H06A,
 H06B,H06C), C3AA(H3AB,H3AC,H3AD), C063(H06D,H06E,H06F), C4AA(H4AB,H4AC,H4AD),
 C5AA(H5AB,H5AC,H5AD), C06C(H06K,H06L,H06M), C06F(H06N,H06O,H06P), C06G(H06H,
 H06I,H06J), C2AA(H2AB,H2AC,H2AD), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12B(H12A,
 H12B,H12C), C3B(H3BA,H3BB,H3BC), C8B(H8BA,H8BB,H8BC), C9(H9A,H9B,H9C),
 C3A(H3AE,H3AF,H3AG), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C8A(H8AB,
 H8AC,H8AD), C12(H12G,H12H,H12I)
;
_shelx_res_checksum              99322
_shelx_fab_checksum              5026
_olex2_submission_special_instructions 'No special instructions were received'