Cyclometalated Ir(iii) complexes bridged by µ-OH and µ-3,5-bis(4-methoxyphenyl)-pyrazole ligands
Mausami,; Trivedi, Harshita; Patra, Ranjan; Behere, Ravi Prakash; Kuila, Biplab; Singh Patel, Sandeep Kumar; Pandey, Mrituanjay D.; Maiti, Biswajit; Mahanti, Bani; RSC Advances 16 (2026) 13358–13368; doi:10.1039/D6RA00878J

data_7251787
_publ_section_title
;
 Cyclometalated Ir(iii) complexes bridged by &#x00B5;-OH and
 &#x00B5;-3,5-bis(4-methoxyphenyl)-pyrazole ligands
;
_journal_issue                   15
_journal_name_full               'RSC Advances'
_journal_page_first              13358
_journal_page_last               13368
_journal_paper_doi               10.1039/D6RA00878J
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         'C61 H47 Ir2 N6 O3, [+ solvents]'
_chemical_formula_sum            'C62.5 H50 Cl Ir2 N6 O6'
_chemical_formula_weight         1400.93
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2026-02-01 deposited with the CCDC.	2026-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                86.0060(10)
_cell_angle_beta                 89.7850(10)
_cell_angle_gamma                70.5140(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9421(2)
_cell_length_b                   15.4721(2)
_cell_length_c                   15.7074(2)
_cell_measurement_reflns_used    23961
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9180
_cell_measurement_theta_min      3.0240
_cell_volume                     2728.78(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  26.00   0.50    0.20    --  -40.83  36.00-154.00  134
  2  \w    -41.00  26.00   0.50    0.20    --  -40.83  36.00-154.00  134
  3  \w    -26.00  41.00   0.50    0.20    --   40.83 -36.00  49.00  134
  4  \w    -26.00  41.00   0.50    0.20    --   40.83 -36.00  49.00  134
  5  \w   -149.00 -68.00   0.50    0.55    --  -82.50 -36.00  49.00  162
  6  \w     81.00 163.00   0.50    0.55    --   96.04  36.00-154.00  164
  7  \w    -78.00   4.00   0.50    0.20    --  -40.83 104.00 -60.00  164
  8  \w   -107.00 -26.00   0.50    0.20    --  -40.83 -36.00  49.00  162
  9  \w    -78.00   4.00   0.50    0.20    --  -40.83 104.00 -60.00  164
 10  \w    -64.00  27.00   0.50    0.20    --  -40.83  65.00 -90.00  182
 11  \w    -64.00  27.00   0.50    0.20    --  -40.83  65.00 -90.00  182
 12  \w    -24.00  35.00   0.50    0.20    --  -40.83  11.00  30.00  118
 13  \w    -97.00 -19.00   0.50    0.20    --  -40.83 138.00  60.00  156
 14  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00   0.00  118
 15  \w   -107.00 -26.00   0.50    0.20    --  -40.83 -36.00  49.00  162
 16  \w    -68.00  28.00   0.50    0.20    --  -40.83  77.00  90.00  192
 17  \w    -28.00  31.00   0.50    0.20    --  -40.83  21.00 -60.00  118
 18  \w    -68.00  28.00   0.50    0.20    --  -40.83  77.00  90.00  192
 19  \w    -31.00  28.00   0.50    0.20    --   40.83 -21.00 -90.00  118
 20  \w     22.00 113.00   0.50    0.20    --   40.83  21.00 -60.00  182
 21  \w     41.00 100.00   0.50    0.20    --   40.83-138.00 -30.00  118
 22  \w    -31.00  28.00   0.50    0.20    --   40.83 -21.00 -60.00  118
 23  \w     22.00 113.00   0.50    0.20    --   40.83  21.00 -60.00  182
 24  \w    -35.00  24.00   0.50    0.20    --   40.83 -11.00 -30.00  118
 25  \w     26.00 108.00   0.50    0.20    --   40.83  36.00-154.00  164
 26  \w    -84.00 -18.00   0.50    0.55    --  -82.50 117.00  60.00  132
 27  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00  90.00   64
 28  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00 -90.00   64
 29  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00-120.00   64
 30  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00 -30.00   64
 31  \w    -47.00 -15.00   0.50    0.55    --  -82.50  42.00 150.00   64
 32  \w    -80.00  -9.00   0.50    0.55    --  -82.50  96.00   0.00  142
 33  \w   -146.00 -78.00   0.50    0.55    --  -82.50-117.00   0.00  136
 34  \w    -80.00  -9.00   0.50    0.55    --  -82.50  96.00   0.00  142
 35  \w     44.00 127.00   0.50    0.55    --   96.04-145.00  90.00  166
 36  \w     28.00  68.00   0.50    0.55    --   96.04 -59.00 150.00   80
 37  \w     27.00 105.00   0.50    0.55    --   96.04 -77.00-180.00  156
 38  \w     82.00 164.00   0.50    0.55    --   96.04  33.00 120.00  164
 39  \w     81.00 164.00   0.50    0.55    --   96.04 145.00  90.00  166
 40  \w     28.00  83.00   0.50    0.55    --   96.04 -68.00-150.00  110
 41  \w     81.00 166.00   0.50    0.55    --   96.04  25.00 -60.00  170
 42  \w     28.00  68.00   0.50    0.55    --   96.04 -59.00 -30.00   80
 43  \w     29.00  57.00   0.50    0.55    --   96.04 -50.00 120.00   56
 44  \w     27.00 105.00   0.50    0.55    --   96.04 -77.00 -60.00  156
 45  \w     28.00  68.00   0.50    0.55    --   96.04 -59.00 120.00   80
 46  \w     27.00 105.00   0.50    0.55    --   96.04 -77.00 -60.00  156
 47  \w     32.00 110.00   0.50    0.55    --   96.04-117.00  90.00  156
 48  \w     28.00  68.00   0.50    0.55    --   96.04 -59.00   0.00   80
 49  \w     23.00 106.00   0.50    0.55    --   96.04 -96.00 120.00  166
 50  \w    105.00 170.00   0.50    0.55    --   96.04  96.00 120.00  130
 51  \w    105.00 170.00   0.50    0.55    --   96.04  96.00  90.00  130
 52  \w    105.00 170.00   0.50    0.55    --   96.04  96.00-150.00  130
 53  \w     23.00 106.00   0.50    0.55    --   96.04 -96.00  90.00  166
 54  \w     32.00 110.00   0.50    0.55    --   96.04-117.00 -60.00  156
 55  \w     29.00  57.00   0.50    0.55    --   96.04 -50.00 150.00   56
 56  \w     81.00 166.00   0.50    0.55    --   96.04  25.00-180.00  170
 57  \w     81.00 166.00   0.50    0.55    --   96.04  25.00-180.00  170
 58  \w     74.00 163.00   0.50    0.55    --   96.04  59.00 150.00  178
 59  \w     27.00 105.00   0.50    0.55    --   96.04 -77.00 120.00  156
 60  \w     44.00 127.00   0.50    0.55    --   96.04-145.00 -60.00  166
 61  \w     99.00 160.00   0.50    0.55    --   96.04 117.00  30.00  122
 62  \w     44.00 127.00   0.50    0.55    --   96.04-145.00 -60.00  166
 63  \w     29.00  57.00   0.50    0.55    --   96.04 -50.00   0.00   56
 64  \w     29.00  57.00   0.50    0.55    --   96.04 -50.00-120.00   56
 65  \w    105.00 170.00   0.50    0.55    --   96.04  96.00   0.00  130
 66  \w     44.00 127.00   0.50    0.55    --   96.04-145.00  90.00  166
 67  \w     44.00 127.00   0.50    0.55    --   96.04-145.00-150.00  166
 68  \w     44.00 127.00   0.50    0.55    --   96.04-145.00-150.00  166
 69  \w     81.00 166.00   0.50    0.55    --   96.04  25.00 -90.00  170
 70  \w     29.00  57.00   0.50    0.55    --   96.04 -50.00-180.00   56
 71  \w     32.00 110.00   0.50    0.55    --   96.04-117.00 -30.00  156
 72  \w   -108.00 -17.00   0.50    0.20    --  -40.83 -65.00 -60.00  182
 73  \w   -108.00 -17.00   0.50    0.20    --  -40.83 -65.00   0.00  182
 74  \w     12.00  43.00   0.50    0.20    --   40.83  84.00-159.46   62
 75  \w     13.00  43.00   0.50    0.20    --   40.83  80.00 110.40   60
 76  \w     14.00 110.00   0.50    0.20    --   40.83  77.00-120.00  192
 77  \w     11.00  43.00   0.50    0.20    --   40.83  86.00 -63.21   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1299850000
_diffrn_orient_matrix_UB_12      -0.0188160000
_diffrn_orient_matrix_UB_13      0.0279812000
_diffrn_orient_matrix_UB_21      -0.0086982000
_diffrn_orient_matrix_UB_22      0.0974566000
_diffrn_orient_matrix_UB_23      -0.0354417000
_diffrn_orient_matrix_UB_31      -0.0419716000
_diffrn_orient_matrix_UB_32      0.0369159000
_diffrn_orient_matrix_UB_33      0.0873581000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17624
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.100
_diffrn_reflns_theta_min         2.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.272
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         17624
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0615
_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^)+(0.1313P)^2^+2.4702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15532
_reflns_number_total             17624
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9285\% 
around [-0.00 0.00 1.00] (reciprocal) or [0.03 -0.08 1.00] (direct)
;
_cod_data_source_file            d6ra00878j2.cif
_cod_data_source_block           ht20b_twin1_hklf4
_cod_original_formula_sum        'C62.50 H50 Cl Ir2 N6 O6'
_cod_database_code               7251787
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Ir'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(4)
 0.22(1) 0.24(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N3-N4
 2.8 with sigma of 0.04
4.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C56(H56), C26(H26), C43(H43), C36(H36), C37(H37), C19(H19),
 C13(H13), C57(H57), C1(H1), C10(H10), C7(H7), C2(H2), C46(H46), C60(H60),
 C49(H49), C15(H15), C14(H14), C22(H22), C4(H4), C24(H24), C34(H34), C40(H40),
 C32(H32), C3(H3), C53(H53), C16(H16), C52(H52), C50(H50), C59(H59), C29(H29),
 C35(H35), C21(H21), C30(H30), C42(H42), C25(H25), C41(H41), C9(H9), C31(H31),
 C8(H8), C20(H20)
4.b Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C54(H54A,H54B,H54C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66052
_shelx_fab_checksum              35006
_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 2.247
_oxdiff_exptl_absorpt_empirical_full_min 0.615
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2