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_7708599
_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         '2(C74 H87 Ir N8 O4), 2(F6 P)'
_chemical_formula_sum            'C148 H174 F12 Ir2 N16 O8 P2'
_chemical_formula_weight         2979.36
_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   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                105.9690(10)
_cell_angle_beta                 90.215(2)
_cell_angle_gamma                114.547(2)
_cell_formula_units_Z            2
_cell_length_a                   19.3154(12)
_cell_length_b                   22.6544(13)
_cell_length_c                   26.8007(15)
_cell_measurement_reflns_used    9595
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.18
_cell_volume                     10162.0(10)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Photon III'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Photon III area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            133799
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.488
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.378
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1099 before and 0.0489 after correction. The Ratio of minimum to maximum transmission is 0.7533. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_description       block
_exptl_crystal_F_000             3060
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.491
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1523
_refine_ls_number_reflns         35698
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+56.2772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26918
_reflns_number_total             35698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03579g2.cif
_cod_data_source_block           v873d_1
_cod_database_code               7708599
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.644
_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
 C47B-C31A
 2.5 with sigma of 0.02
 C31A-C1D
 2.5 with sigma of 0.02
 C47A-C9
 2.5 with sigma of 0.02
 C0AA-C26B
 2.5 with sigma of 0.02
 C0AA-C1J
 2.5 with sigma of 0.02
 C26A-C7
 2.5 with sigma of 0.02
 C1K-C7
 2.5 with sigma of 0.02
 C26A-C1K
 2.5 with sigma of 0.02
 C1H-C046 = C046-C4AA
 1.54 with sigma of 0.02
 C24B-C4AA = C5-C4AA = C1I-C1H = C25B-C4AA = C25A-C1H = C24A-C1H
 1.54 with sigma of 0.02
 C25A-C1I
 2.5 with sigma of 0.02
 C1I-C24A
 2.5 with sigma of 0.02
 C24A-C25A
 2.5 with sigma of 0.02
 C25B-C5
 2.5 with sigma of 0.02
 C24B-C25B
 2.5 with sigma of 0.02
 C24B-C5
 2.5 with sigma of 0.02
 C15-C14 = C16-C14
 1.54 with sigma of 0.02
 O00R-C15
 1.45 with sigma of 0.02
 O00R-C61A
 1.45 with sigma of 0.02
 C61A-C2AA
 1.5 with sigma of 0.02
 C2AA-C3AA
 1.5 with sigma of 0.01
 C1E-C1F = C5AA-C6AA
 1.54 with sigma of 0.02
 C1F-C1G = C6AA-C6
 1.54 with sigma of 0.02
 C044-C058
 1.54 with sigma of 0.02
 C61A-C3AA
 2.5 with sigma of 0.02
 C9-C05W \\sim C1D-C05W \\sim C31B-C05W \\sim C31A-C05W \\sim C47A-C05W \\sim
C47B-C05W
 with sigma of 0.02
 C04N-C04F \\sim C05Y-C04N \\sim C04O-C04N
 with sigma of 0.02
 C05R-C04V \\sim C05L-C04V \\sim C05I-C04V
 with sigma of 0.02
 C26A-C04K \\sim C26B-C04K \\sim C04K-C7 \\sim C04K-C1J \\sim C04K-C0AA \\sim
C04K-C1K
 with sigma of 0.02
 C1AA-C1B \\sim C1B-C0 \\sim C12-C0 \\sim C12-C05Q
 with sigma of 0.02
 P005-F03C \\sim P005-F05E \\sim P005-F068 \\sim P005-F8 \\sim P005-F054 \\sim
P005-F04R
 with sigma of 0.02
 C1B-C0 \\sim C12-C1L
 with sigma of 0.02
 O00P-C0 \\sim O00P-C1L
 with sigma of 0.02
 O00W-C1E \\sim O00W-C5AA
 with sigma of 0.02
3. Restrained planarity
 F04R, F8, F05E, F03C
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C1D) = Uanis(C31B) = Uanis(C31A) = Uanis(C47A) = Uanis(C47B)
Uanis(C05W) = Uanis(C1D) = Uanis(C9) = Uanis(C47B) = Uanis(C47A) = Uanis(C31A)
= Uanis(C31B)
Uanis(C04O) = Uanis(C04N) = Uanis(C04F) = Uanis(C05Y)
Uanis(C05R) = Uanis(C04V) = Uanis(C05I) = Uanis(C05L)
Uanis(C04P) = Uanis(C04L) = Uanis(C05D)
Uiso(C26A) = Uiso(C1K) = Uiso(C7)
Uanis(C12) = Uanis(C0) = Uanis(C1B) = Uanis(C1AA) = Uanis(C05Q)
Uanis(C1J) = Uanis(C0AA) = Uanis(C26B)
Uanis(F068) = Uanis(F8) = Uanis(F054) = Uanis(F04R) = Uanis(F03C) = Uanis(F05E)
Uanis(C0) = Uanis(C1L) = Uanis(C1B) = Uanis(C1AA) = Uanis(C05Q) = Uanis(C12)
Uanis(C05H) = Uanis(C05G) = Uanis(C055) = Uanis(C04Y)
Uanis(C25A) = Uanis(C24A) = Uanis(C1H) = Uanis(C1I)
Uanis(C046) = Uanis(C1H) = Uanis(C25A) = Uanis(C1I) = Uanis(C24A)
Uiso(C24B) = Uiso(C4AA) = Uiso(C5) = Uiso(C25B)
Uanis(O00P) = Uanis(C1L) = Uanis(C0) = Uanis(C1B) = Uanis(C1AA) = Uanis(C05Q) =
Uanis(C12)
Uanis(C04F) = Uanis(C04N) = Uanis(C04O) = Uanis(C05Y) = Uanis(C02Y)
Uanis(C1J) = Uanis(C04K) = Uanis(C0AA) = Uanis(C26B)
Uanis(C04I) = Uanis(C03I) = Uanis(C040) = Uanis(C01Q) = Uanis(C3) = Uanis(C02F)
Uiso(C15) = Uiso(C14) = Uiso(C16)
Uanis(C61A) = Uanis(C2AA) = Uanis(C3AA)
Uanis(C6) = Uanis(C1G)
Uanis(C1E) = Uanis(C5AA)
Uanis(C1F) = Uanis(C6AA)
Uanis(C1E) = Uanis(C5AA) = Uanis(C1F) = Uanis(C6AA) = Uanis(C1G) = Uanis(C6)
5. Rigid body (RIGU) restrains
 C02S, C03V, C03M, C046, C03R, C04D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C0(0.4) H0A(0.4) H0B(0.4) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5)
 C4AA(0.5) C5AA(0.5) H5AA(0.5) H5AB(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C05Q(0.6)
 H05P(0.6) H05Q(0.6) H05R(0.6) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C24B(0.5)
 H24A(0.5) H24B(0.5) H24C(0.5) C25B(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
 C26B(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C31B(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5) C47B(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C9(0.5) H9A(0.5) H9B(0.5)
 H9C(0.5) C12(0.6) H12A(0.6) H12B(0.6) C1B(0.4) H1BA(0.4) H1BB(0.4) C1D(0.5)
 H1DA(0.5) H1DB(0.5) H1DC(0.5) C47A(0.5) H47D(0.5) H47E(0.5) H47F(0.5)
 C31A(0.5) H31D(0.5) H31E(0.5) H31F(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5) C1F(0.5)
 H1FA(0.5) H1FB(0.5) C1G(0.5) H1GA(0.5) H1GB(0.5) H1GC(0.5) C1AA(0.4) H1AA(0.4)
 H1AB(0.4) H1AC(0.4) C1H(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C1I(0.5)
 H1IA(0.5) H1IB(0.5) H1IC(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5) C1J(0.5)
 H1JA(0.5) H1JB(0.5) H1JC(0.5) C26A(0.5) H26D(0.5) H26E(0.5) H26F(0.5) C1K(0.5)
 H1KA(0.5) H1KB(0.5) H1KC(0.5) C1L(0.6) H1LA(0.6) H1LB(0.6) C61A(0.45)
 H61A(0.45) H61B(0.45) C2AA(0.45) H2AA(0.45) H2AB(0.45) C16(0.55) H16A(0.55)
 H16B(0.55) H16C(0.55) C14(0.55) H14A(0.55) H14B(0.55) C15(0.55) H15A(0.55)
 H15B(0.55) C3AA(0.45) H3AA(0.45) H3AB(0.45) H3AC(0.45)
 Fixed U11: C61A(0.161779) C2AA(0.161779) C3AA(0.161779)
 Fixed U12: C61A(0.002921) C2AA(0.002921) C3AA(0.002921)
 Fixed U13: C61A(-0.031534) C2AA(-0.031534) C3AA(-0.031534)
 Fixed U22: C61A(0.021344) C2AA(0.021344) C3AA(0.021344)
 Fixed U23: C61A(0.007459) C2AA(0.007459) C3AA(0.007459)
 Fixed U33: C61A(0.21907) C2AA(0.21907) C3AA(0.21907)
 Fixed X: C5(1.09304) C31B(0.5977) C9(0.47512) C16(0.42421) C15(0.450809)
 Fixed Y: C5(0.707069) C31B(0.29183) C9(0.1715) C16(0.63083) C15(0.54317)
 Fixed Z: C5(0.035449) C31B(-0.012131) C9(-0.025731) C16(0.15415) C15(0.19277)
7.a Secondary CH2 refined with riding coordinates:
 C01H(H01A,H01B), C01M(H01C,H01D), C01U(H01E,H01F), C022(H02H,H02I), C029(H02J,
 H02K), C02D(H02N,H02O), C02I(H02A,H02C), C02K(H02D,H02E), C02L(H02F,H02G),
 C02W(H02P,H02Q), C034(H03E,H03F), C03D(H03A,H03B), C03H(H03J,H03K), C03Q(H03C,
 H03D), C0(H0A,H0B), C043(H04A,H04B), C044(H04C,H04D), C04B(H04O,H04P),
 C04G(H04E,H04F), C5AA(H5AA,H5AB), C6AA(H6AA,H6AB), C12(H12A,H12B), C1B(H1BA,
 H1BB), C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1L(H1LA,H1LB), C61A(H61A,H61B),
 C2AA(H2AA,H2AB), C14(H14A,H14B), C15(H15A,H15B)
7.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C05Q(H05P,H05Q,H05R), C05Y(H05,HF,HG), C24B(H24A,H24B,H24C),
 C25B(H25A,H25B,H25C), C31B(H31A,H31B,H31C), C47B(H47A,H47B,H47C), C9(H9A,H9B,
 H9C), C1D(H1DA,H1DB,H1DC), C47A(H47D,H47E,H47F), C31A(H31D,H31E,H31F),
 C1G(H1GA,H1GB,H1GC), C1AA(H1AA,H1AB,H1AC), C26A(H26D,H26E,H26F), C16(H16A,H16B,
 H16C)
7.c Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00X(H00X), C015(H015), C019(H019), C01I(H01I), C01P(H01P),
 C01Q(H01Q), C01S(H01S), C01T(H01T), C01Z(H01Z), C020(H020), C026(H026),
 C02A(H02L), C02B(H02B), C02C(H02M), C02T(H02T), C02U(H02U), C02X(H02X),
 C030(H030), C033(H033), C038(H038), C039(H039), C03E(H03G), C03F(H03H),
 C03I(H03I), C03K(H03L), C03L(H03N), C03M(H03M), C03N(H03O), C03O(H03P),
 C03P(H03Q), C03R(H03R), C03S(H03S), C03W(H03W), C040(H040), C042(H042),
 C049(H049), C04I(H04I), C04M(H04M), C04Q(H04Q), C04T(H04T), C04U(H04Z)
7.d Idealised Me refined as rotating group:
 C03Y(H03T,H03U,H03V), C04F(H04R,H04S,H04U), C04H(H04V,H04W,H04X), C04L(H04G,
 H04H,H04J), C04O(H04Y,H,HA), C04P(H04K,H04L,H04N), C0AA(H0AA,H0AB,H0AC),
 C055(H05A,H05B,H05C), C056(H05S,H05T,H05U), C058(H05D,H05E,H05F), C05D(H05G,
 H05H,H05I), C05G(H05J,H05K,H05L), C05H(H05M,H05N,H05O), C05I(H05V,H05W,H05X),
 C05L(H05Y,HB,HC), C6(H6A,H6B,H6C), C05R(H05Z,HD,HE), C7(H7A,H7B,H7C),
 C26B(H26A,H26B,H26C), C25A(H25D,H25E,H25F), C1I(H1IA,H1IB,H1IC), C24A(H24D,
 H24E,H24F), C1J(H1JA,H1JB,H1JC), C1K(H1KA,H1KB,H1KC), C3AA(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              13680
_shelx_fab_checksum              69771
_olex2_submission_special_instructions 'No special instructions were received'