Luminescent iridium(III) complexes bearing boronic acid groups: potential sensors for carbohydrates.
Rahman, Rahad; Quazi, Nurul H.; White, Keith F.; Saker Neto, Nicolau; Hong, Yuning; Maeder, Marcel; Wilson, David J. D.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15609–15622; doi:10.1039/d5dt01291k

data_1575850
_publ_section_title
;
 Luminescent iridium(III) complexes bearing boronic acid groups: potential
 sensors for carbohydrates.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15609
_journal_page_last               15622
_journal_paper_doi               10.1039/d5dt01291k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C27 H24 B Ir N7 O2 Cl'
_chemical_formula_sum            'C27 H24 B Cl Ir N7 O2'
_chemical_formula_weight         716.99
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-07-27 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.87610(10)
_cell_length_b                   20.87610(10)
_cell_length_c                   12.9304(3)
_cell_measurement_reflns_used    19881
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.0700
_cell_measurement_theta_min      4.0060
_cell_volume                     5635.22(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 40.53 (release 29-04-2019))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -41.00  -1.00   0.50    1.00    --  -38.50 113.00-164.00   80
  2  \w    -71.00 -46.00   0.50    1.00    --  -38.50 113.00-164.00   50
  3  \w     36.00  74.00   0.50    4.00    --  100.00-113.00 103.00   76
  4  \w    114.00 140.00   0.50    4.00    --  100.00 113.00-164.00   52
  5  \w    -63.00 -25.00   0.50    1.00    --  -38.50 -43.00 -60.00   76
  6  \w    -13.00  23.00   0.50    1.00    --  -38.50  43.00 150.00   72
  7  \w    -69.00 -36.00   0.50    1.00    --  -38.50 -32.00-180.00   66
  8  \w    -53.00 -12.00   0.50    1.00    --  -38.50  54.00  60.00   82
  9  \w    -50.00   8.00   0.50    1.00    --  -38.50  43.00-180.00  116
 10  \w   -100.00 -70.00   0.50    1.00    --  -38.50 -54.00-150.00   60
 11  \w   -101.00 -67.00   0.50    1.00    --  -38.50 -43.00 -60.00   68
 12  \w   -103.00 -76.00   0.50    1.00    --  -38.50 -32.00-180.00   54
 13  \w    -49.00 -22.00   0.50    1.00    --  -38.50  21.00-180.00   54
 14  \w      5.00  30.00   0.50    1.00    --  -38.50  21.00-180.00   50
 15  \w    -52.00 -25.00   0.50    1.00    --  -38.50  43.00 150.00   54
 16  \w    -53.00 -27.00   0.50    1.00    --  -38.50 -54.00-150.00   52
 17  \w    -47.00 -22.00   0.50    1.00    --  -38.50  43.00  30.00   50
 18  \w    -13.00  24.00   0.50    1.00    --  -38.50  43.00  30.00   74
 19  \w     -7.00  24.00   0.50    1.00    --  -38.50  54.00  60.00   62
 20  \w    -38.00  29.00   0.50    1.00    --  -38.50  11.00 120.00  134
 21  \w     16.00  41.00   0.50    1.00    --   42.60-104.00 -90.00   50
 22  \w      8.00  76.00   0.50    1.00    --   42.60-104.00 -30.00  136
 23  \w    -17.00  48.00   0.50    1.00    --   42.60 -32.00 120.00  130
 24  \w     55.00  84.00   0.50    1.00    --   42.60-138.00-180.00   58
 25  \w     68.00  93.00   0.50    1.00    --   42.60-138.00  30.00   50
 26  \w     52.00  77.00   0.50    1.00    --   42.60-138.00 -90.00   50
 27  \w     19.00  78.00   0.50    1.00    --   42.60-113.00 103.00  118
 28  \w    -25.00  44.00   0.50    1.00    --   42.60 -21.00-150.00  138
 29  \w     66.00  92.00   0.50    4.00    --  100.00 -68.00-180.00   52
 30  \w     86.00 112.00   0.50    4.00    --  100.00 -59.00   0.00   52
 31  \w    100.00 126.00   0.50    4.00    --  100.00-145.00 -90.00   52
 32  \w     39.00  75.00   0.50    4.00    --  100.00 -59.00   0.00   72
 33  \w     78.00 124.00   0.50    4.00    --  100.00-145.00-180.00   92
 34  \w    104.00 163.00   0.50    4.00    --  100.00 117.00 -90.00  118
 35  \w    103.00 164.00   0.50    4.00    --  100.00  25.00 -90.00  122
 36  \w     79.00 125.00   0.50    4.00    --  100.00-145.00-120.00   92
 37  \w    105.00 165.00   0.50    4.00    --  100.00  77.00 120.00  120
 38  \w     95.00 167.00   0.50    4.00    --  100.00  25.00-120.00  144
 39  \w     36.00  77.00   0.50    4.00    --  100.00 -77.00   0.00   82
 40  \w     42.00  80.00   0.50    4.00    --  100.00 -42.00 120.00   76
 41  \w     35.00 109.00   0.50    4.00    --  100.00 -33.00 -30.00  148
 42  \w    102.00 127.00   0.50    4.00    --  100.00 -87.00 -90.00   50
 43  \w     37.00  62.00   0.50    4.00    --  100.00 -50.00  60.00   50
 44  \w     38.00 101.00   0.50    4.00    --  100.00-117.00 -30.00  126
 45  \w     83.00 109.00   0.50    4.00    --  100.00-117.00  60.00   52
 46  \w     50.00 100.00   0.50    4.00    --  100.00 -96.00-180.00  100
 47  \w     70.00 122.00   0.50    4.00    --  100.00 -68.00  90.00  104
 48  \w     45.00 108.00   0.50    4.00    --  100.00 -17.00   0.00  126
 49  \w    137.00 162.00   0.50    4.00    --  100.00  42.00-180.00   50
 50  \w     58.00 126.00   0.50    4.00    --  100.00-145.00 -30.00  136
 51  \w     91.00 116.00   0.50    4.00    --  100.00 -87.00   0.00   50
 52  \w     88.00 126.00   0.50    4.00    --  100.00  42.00-180.00   76
 53  \w     79.00 113.00   0.50    4.00    --  100.00 -42.00 150.00   68
 54  \w     96.00 121.00   0.50    4.00    --  100.00 -77.00   0.00   50
 55  \w     34.00  74.00   0.50    4.00    --  100.00 -87.00 -90.00   80
 56  \w    100.00 126.00   0.50    4.00    --  100.00-145.00 120.00   52
 57  \w     35.00 109.00   0.50    4.00    --  100.00-117.00   0.00  148
 58  \w     42.00  88.00   0.50    4.00    --  100.00-145.00 -90.00   92
 59  \w     83.00 108.00   0.50    4.00    --  100.00-107.00-108.11   50
 60  \w     63.00 100.00   0.50    4.00    --  100.00 -33.00 150.00   74
 61  \w     54.00 105.00   0.50    4.00    --  100.00 -91.00 -18.74  102
 62  \w     70.00  96.00   0.50    4.00    --  100.00 -42.00-150.00   52
 63  \w    108.00 134.00   0.50    4.00    --  100.00 145.00-150.00   52
 64  \w     74.00 102.00   0.50    4.00    --  100.00-117.00  90.00   56
 65  \w     87.00 162.00   0.50    4.00    --  100.00  42.00 -60.00  150
 66  \w    106.00 164.00   0.50    4.00    --  100.00  96.00   0.00  116
 67  \w     49.00  74.00   0.50    4.00    --  100.00 -42.00 150.00   50
 68  \w    140.00 165.00   0.50    4.00    --  100.00  77.00  60.00   50
 69  \w    139.00 164.00   0.50    4.00    --  100.00 145.00-120.00   50
 70  \w    105.00 131.00   0.50    4.00    --  100.00  77.00  30.00   52
 71  \w    105.00 155.00   0.50    4.00    --  100.00  77.00 -30.00  100
 72  \w    115.00 140.00   0.50    4.00    --  100.00  77.00 -90.00   50
 73  \w     68.00  98.00   0.50    4.00    --  100.00 -33.00 -90.00   60
 74  \w     62.00 100.00   0.50    4.00    --  100.00-117.00  30.00   76
 75  \w     54.00  87.00   0.50    4.00    --  100.00 -59.00-150.00   66
 76  \w     70.00 103.00   0.50    4.00    --  100.00 -42.00-120.00   66
 77  \w     95.00 124.00   0.50    4.00    --  100.00 145.00-120.00   58
 78  \w    108.00 133.00   0.50    4.00    --  100.00 145.00 150.00   50
 79  \w    121.00 146.00   0.50    4.00    --  100.00  25.00 150.00   50
 80  \w     66.00  91.00   0.50    4.00    --  100.00 -59.00-120.00   50
 81  \w    113.00 158.00   0.50    4.00    --  100.00  17.00-180.00   90
 82  \w     75.00 117.00   0.50    4.00    --  100.00 -85.00 139.23   84
 83  \w     69.00  97.00   0.50    4.00    --  100.00 -50.00  60.00   56
 84  \w     35.00  61.00   0.50    4.00    --  100.00 -87.00 120.00   52
 85  \w    101.00 126.00   0.50    4.00    --  100.00 -87.00 120.00   50
 86  \w     50.00  75.00   0.50    4.00    --  100.00 -33.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0626458000
_diffrn_orient_matrix_UB_12      0.0334838000
_diffrn_orient_matrix_UB_13      -0.0321658000
_diffrn_orient_matrix_UB_21      0.0366659000
_diffrn_orient_matrix_UB_22      0.0380776000
_diffrn_orient_matrix_UB_23      -0.0832470000
_diffrn_orient_matrix_UB_31      -0.0130909000
_diffrn_orient_matrix_UB_32      -0.0535832000
_diffrn_orient_matrix_UB_33      -0.0790828000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37497
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.168
_diffrn_reflns_theta_min         5.846
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.355
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       needle
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1007 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0381
_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^)+30.4045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2620
_reflns_number_total             2733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01291k2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 1575847--1575850.cif.'
_cod_database_code               1575850
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H22 N7 O2 B Cl Ir'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(N1B)=Sof(N2B)=Sof(C1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=
 Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=
 Sof(C9B)=Sof(H9B)=1-FVAR(1)
 Sof(N1A)=Sof(N2A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=
 Sof(C9A)=Sof(H9A)=FVAR(1)
 Fixed Sof: Ir1(0.5) N3(0.5) N4(0.5) N5(0.5) C10(0.5) H10(0.5) C11(0.5)
 H11(0.5) C12(0.5) C13(0.5) H13(0.5) C14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16(0.5) C17(0.5) H17(0.5) Cl1(0.5) O1(0.5) O2(0.5) H2(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) B1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C4A(H4A), C4B(H4B), C5A(H5A),
 C5B(H5B), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B), C9A(H9A), C9B(H9B), C10(H10),
  C11(H11), C13(H13), C15(H15), C16(H16), C17(H17)
3.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.101
_oxdiff_exptl_absorpt_empirical_full_min 0.569