Coordination polymers with iridium(III) metalloligands: the effect of pore size upon luminescent cation sensing.
Hong, Zhejun; Siripanich, Pattara; Stansfield, Oliver G.; Hall, Christopher R.; Connell, Timothy U.; Hua, Carol; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11656–11666; doi:10.1039/d5dt00813a

data_7718967
_publ_section_title
;
 Coordination polymers with iridium(III) metalloligands: the effect of
 pore size upon luminescent cation sensing.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11656
_journal_page_last               11666
_journal_paper_doi               10.1039/d5dt00813a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C68 H44 Cd Ir2 N8 O8, C3 H6 N O, 2[C3H7NO], 4[H2O]'
_chemical_formula_sum            'C77 H72 Cd Ir2 N11 O15'
_chemical_formula_weight         1888.25
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-19
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-19 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2290(3)
_cell_length_b                   13.0870(2)
_cell_length_c                   32.8383(5)
_cell_measurement_reflns_used    24562
_cell_measurement_temperature    270.00(12)
_cell_measurement_theta_max      79.0160
_cell_measurement_theta_min      2.6720
_cell_volume                     7404.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      270.00(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_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     28.00  77.00   0.50    1.60    --   47.51 -94.00 140.00   98
  2  \w   -162.00 -99.00   0.50    6.00    --  -91.75 -94.00 140.00  126
  3  \w   -140.00-100.00   0.50    6.00    --  -91.75-101.00-119.00   80
  4  \w     69.00  95.00   0.50    6.00    --  110.75-101.00-119.00   52
  5  \w    108.00 175.00   0.50    6.00    --  110.75 101.00 -14.00  134
  6  \w   -110.00 -40.00   0.50    1.60    --  -47.51 -57.00 150.00  140
  7  \w   -118.00 -44.00   0.50    1.60    --  -47.51 -38.00   0.00  148
  8  \w   -119.00 -88.00   0.50    1.60    --  -47.51 -77.00 -90.00   62
  9  \w    -60.00 -28.00   0.50    1.60    --  -47.51 -77.00 -90.00   64
 10  \w    -85.00 -26.00   0.50    1.60    --  -47.51 125.00 -60.00  118
 11  \w    -51.00 -26.00   0.50    6.00    --  -91.75  45.00-150.00   50
 12  \w    -57.00 -19.00   0.50    6.00    --  -91.75  61.00 120.00   76
 13  \w    -48.00 -23.00   0.50    6.00    --  -91.75  45.00 -30.00   50
 14  \w    -51.00 -26.00   0.50    6.00    --  -91.75  45.00 -90.00   50
 15  \w     39.00  70.00   0.50    6.00    --  110.75 -61.00 150.00   62
 16  \w     39.00  67.00   0.50    6.00    --  110.75 -61.00 -30.00   56
 17  \w     44.00  69.00   0.50    6.00    --  110.75 -61.00 -90.00   50
 18  \w    117.00 178.00   0.50    6.00    --  110.75  15.00  90.00  122
 19  \w     42.00  67.00   0.50    6.00    --  110.75-125.00   0.00   50
 20  \w     43.00  68.00   0.50    6.00    --  110.75 -61.00 -60.00   50
 21  \w     39.00  66.00   0.50    6.00    --  110.75 -61.00   0.00   54
 22  \w     60.00  93.00   0.50    6.00    --  110.75 -77.00 -90.00   66
 23  \w    101.00 147.00   0.50    6.00    --  110.75  30.00   0.00   92
 24  \w     63.00  89.00   0.50    6.00    --  110.75 -77.00 120.00   52
 25  \w     82.00 107.00   0.50    6.00    --  110.75-125.00   0.00   50
 26  \w     43.00  69.00   0.50    6.00    --  110.75 -61.00-120.00   52
 27  \w     44.00  70.00   0.50    6.00    --  110.75 -61.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0328503000
_diffrn_orient_matrix_UB_12      -0.0306576000
_diffrn_orient_matrix_UB_13      0.0418437000
_diffrn_orient_matrix_UB_21      0.0786535000
_diffrn_orient_matrix_UB_22      -0.0483300000
_diffrn_orient_matrix_UB_23      0.0113814000
_diffrn_orient_matrix_UB_31      0.0271369000
_diffrn_orient_matrix_UB_32      0.1028619000
_diffrn_orient_matrix_UB_33      0.0178536000
_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  0.0756
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            46402
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         2.691
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.710
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             3732
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.666
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.439(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         13477
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                12147
_reflns_number_total             13477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00813a2.cif
_cod_data_source_block           ch-1-1c1x
_cod_depositor_comments
'Adding full bibliography for 7718966--7718969.cif.'
_cod_database_code               7718967
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C74 H58 N10 O11 Cd Ir2'
_chemical_oxdiff_usercomment     'Orange block'
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.365
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56052
 0.43948
2. Rigid bond restraints
 C9, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C63(H63), C62(H62), C70(H70), C64(H64), C71(H71), C67(H67), C85(H85),
 C74(H74), C46(H46), C47(H47), C72(H72), C36(H36), C81(H81), C42(H42), C34(H34),
  C29(H29), C51(H51), C52(H52), C86(H86), C78(H78), C41(H41), C43(H43),
 C90(H90), C73(H73), C37(H37), C80(H80), C59(H59), C75(H75), C53(H53), C57(H57),
  C92(H92), C79(H79), C56(H56), C50(H50), C40(H40), C91(H91), C45(H45),
 C84(H84), C87(H87), C58(H58), C31(H31), C93(H93), C48(H48), C32(H32)
3.b Idealised Me refined as rotating group:
 C96(H96A,H96B,H96C), C97(H97A,H97B,H97C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 482 electrons were 
found in a volume of 1960\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C3H7NO], 4[H2O] per Formula Unit 
which account for 480 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70485
_shelx_hkl_checksum              16339
_shelx_fab_checksum              41999
_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 3.057
_oxdiff_exptl_absorpt_empirical_full_min 0.344