Organometallic Ir(III) complexes: post-synthetic modification, photophysical properties and binuclear complex construction.
Gitlina, Anastasia Yu; Khistiaeva, Viktoria; Melnikov, Alexey; Ivonina, Mariia; Sizov, Vladimir; Spiridonova, Dar'ya; Makarova, Anna; Vyalikh, Denis; Grachova, Elena; Dalton transactions (Cambridge, England : 2003) 52 (2023) 8986–8997; doi:10.1039/d3dt00901g

data_7713365
_publ_section_title
;
 Organometallic Ir(III) complexes: post-synthetic modification,
 photophysical properties and binuclear complex construction.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8986
_journal_page_last               8997
_journal_paper_doi               10.1039/d3dt00901g
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         '2(C46 H34 Ir N8), F6 P'
_chemical_formula_sum            'C92 H68 F6 Ir2 N16 P'
_chemical_formula_weight         1926.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.7680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.9654(2)
_cell_length_b                   33.9313(2)
_cell_length_c                   15.77980(10)
_cell_measurement_reflns_used    85090
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9040
_cell_measurement_theta_min      1.6730
_cell_volume                     22844.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_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    -43.00 -18.00   0.50    0.31    --  -38.82  28.00  20.00   50
  2  \w   -101.00 -63.00   0.50    0.31    --  -38.82 -28.00-141.00   76
  3  \w    -10.00  27.00   0.50    0.31    --  -38.82  28.00  20.00   74
  4  \w     66.00  91.00   0.50    0.31    --   38.82  28.00  20.00   50
  5  \w    100.00 125.00   0.50    1.23    --  107.00  28.00  20.00   50
  6  \w     41.00 119.00   0.50    1.23    --  107.00 -28.00-141.00  156
  7  \w   -104.00 -65.00   0.50    0.31    --  -38.82 -43.00  30.00   78
  8  \w   -101.00 -23.00   0.50    0.31    --  -38.82 -43.00 120.00  156
  9  \w    -58.00 -22.00   0.50    0.31    --  -38.82 -43.00  30.00   72
 10  \w     51.00 103.00   0.50    0.31    --   38.82  32.00-150.00  104
 11  \w     18.00  43.00   0.50    0.31    --   38.82  65.00 150.00   50
 12  \w    -14.00  59.00   0.50    0.31    --   38.82 -54.00  90.00  146
 13  \w     20.00 100.00   0.50    0.31    --   38.82  54.00 -30.00  160
 14  \w     26.00  51.00   0.50    0.31    --   38.82 -28.00-141.00   50
 15  \w     -7.00  60.00   0.50    0.31    --   38.82 -77.00  60.00  134
 16  \w     54.00  79.00   0.50    0.31    --   38.82  65.00 150.00   50
 17  \w    -27.00  17.00   0.50    0.31    --   38.82 -28.00-141.00   88
 18  \w     34.00  78.00   0.50    0.31    --   38.82  32.00 120.00   88
 19  \w     88.00 116.00   0.50    1.23    --  107.00 -61.00 120.00   56
 20  \w     42.00  75.00   0.50    1.23    --  107.00 -61.00 120.00   66
 21  \w     71.00  98.00   0.50    1.23    --  107.00-111.00 120.00   54
 22  \w     47.00 128.00   0.50    1.23    --  107.00 -77.00  30.00  162
 23  \w     38.00 111.00   0.50    1.23    --  107.00-111.00-120.00  146
 24  \w     93.00 139.00   0.50    1.23    --  107.00  30.00 -90.00   92
 25  \w     85.00 157.00   0.50    1.23    --  107.00  15.00  90.00  144
 26  \w    100.00 126.00   0.50    1.23    --  107.00 111.00  60.00   52
 27  \w     52.00 113.00   0.50    1.23    --  107.00 -86.00 120.00  122
 28  \w     39.00 103.00   0.50    1.23    --  107.00 -30.00  30.00  128
 29  \w     93.00 156.00   0.50    1.23    --  107.00  30.00  30.00  126
 30  \w     96.00 121.00   0.50    1.23    --  107.00  45.00-180.00   50
 31  \w     43.00 125.00   0.50    1.23    --  107.00 -45.00 -90.00  164
 32  \w     42.00 127.00   0.50    1.23    --  107.00 -69.00 -90.00  170
 33  \w     83.00 109.00   0.50    0.31    --   38.82  28.00  20.00   52
 34  \w    -57.00   0.00   0.50    0.31    --  -38.82  21.00-180.00  114
 35  \w     12.00  41.00   0.50    0.31    --   38.82  77.00-180.00   58
 36  \w     52.00  78.00   0.50    0.31    --   38.82  77.00  90.00   52
 37  \w     34.00  59.00   0.50    0.31    --   38.82 -54.00-150.00   50
 38  \w    -25.00  12.00   0.50    0.31    --   38.82 -32.00 150.00   74
 39  \w     17.00  43.00   0.50    0.31    --   38.82  77.00  90.00   52
 40  \w      5.00  47.00   0.50    0.31    --   38.82 -32.00  90.00   84
 41  \w     19.00  47.00   0.50    0.31    --   38.82  77.00 150.00   56
 42  \w     83.00 108.00   0.50    0.31    --   38.82  32.00 -90.00   50
 43  \w     18.00  65.00   0.50    0.31    --   38.82  77.00 120.00   94
 44  \w    -25.00   1.00   0.50    0.31    --   38.82 -54.00-150.00   52
 45  \w     32.00  58.00   0.50    0.31    --   38.82  32.00 -90.00   52
 46  \w     25.00  51.00   0.50    0.31    --   38.82 -32.00 150.00   52
 47  \w     18.00  52.00   0.50    0.31    --   38.82  65.00  90.00   68
 48  \w     38.00  64.00   0.50    0.31    --   38.82  65.00-120.00   52
 49  \w     47.00  96.00   0.50    1.23    --  107.00 -61.00-150.00   98
 50  \w    120.00 146.00   0.50    1.23    --  107.00  80.00 100.54   52
 51  \w    126.00 152.00   0.50    1.23    --  107.00  77.00  60.00   52
 52  \w     80.00 105.00   0.50    1.23    --  107.00  80.00 100.54   50
 53  \w     85.00 115.00   0.50    1.23    --  107.00  61.00  90.00   60
 54  \w     81.00 117.00   0.50    1.23    --  107.00  77.00  60.00   72
 55  \w     80.00 106.00   0.50    1.23    --  107.00  77.00-180.00   52
 56  \w     92.00 118.00   0.50    1.23    --  107.00  45.00 120.00   52
 57  \w     88.00 146.00   0.50    1.23    --  107.00  53.00 150.00  116
 58  \w     81.00 107.00   0.50    1.23    --  107.00  77.00  90.00   52
 59  \w     80.00 105.00   0.50    1.23    --  107.00  77.00  30.00   50
 60  \w     80.00 106.00   0.50    1.23    --  107.00  79.00  85.01   52
 61  \w     80.00 105.00   0.50    1.23    --  107.00  77.00 150.00   50
 62  \w     83.00 149.00   0.50    1.23    --  107.00  69.00 120.00  132
 63  \w     85.00 111.00   0.50    1.23    --  107.00  69.00  60.00   52
 64  \w    121.00 147.00   0.50    1.23    --  107.00  53.00  60.00   52
 65  \w     90.00 125.00   0.50    1.23    --  107.00  45.00  60.00   70
 66  \w     87.00 112.00   0.50    1.23    --  107.00  53.00  60.00   50
 67  \w     83.00 109.00   0.50    1.23    --  107.00  69.00 150.00   52
 68  \w     87.00 128.00   0.50    1.23    --  107.00  53.00-180.00   82
 69  \w    132.00 157.00   0.50    1.23    --  107.00  53.00  90.00   50
 70  \w    122.00 150.00   0.50    1.23    --  107.00  69.00-150.00   56
 71  \w     87.00 112.00   0.50    1.23    --  107.00  53.00  90.00   50
 72  \w    129.00 157.00   0.50    1.23    --  107.00  37.00   0.00   56
 73  \w     87.00 113.00   0.50    1.23    --  107.00  61.00 150.00   52
 74  \w     85.00 124.00   0.50    1.23    --  107.00  62.00-177.09   78
 75  \w     84.00 110.00   0.50    1.23    --  107.00  69.00-180.00   52
 76  \w     86.00 112.00   0.50    1.23    --  107.00  61.00-180.00   52
 77  \w     75.00 121.00   0.50    1.23    --  107.00 -37.00  90.00   92
 78  \w     80.00 106.00   0.50    1.23    --  107.00  77.00 120.00   52
 79  \w    132.00 157.00   0.50    1.23    --  107.00  30.00 -90.00   50
 80  \w    127.00 153.00   0.50    1.23    --  107.00  77.00-180.00   52
 81  \w     88.00 120.00   0.50    1.23    --  107.00  53.00 120.00   64
 82  \w     87.00 113.00   0.50    1.23    --  107.00  52.00 146.33   52
 83  \w     89.00 115.00   0.50    1.23    --  107.00  61.00  60.00   52
 84  \w     88.00 122.00   0.50    1.23    --  107.00  61.00 120.00   68
 85  \w    130.00 155.00   0.50    1.23    --  107.00  69.00  90.00   50
 86  \w     83.00 108.00   0.50    1.23    --  107.00  69.00  90.00   50
 87  \w    127.00 144.00   0.50    1.23    --  107.00 101.00-149.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0517337000
_diffrn_orient_matrix_UB_12      -0.0086481000
_diffrn_orient_matrix_UB_13      0.0319539000
_diffrn_orient_matrix_UB_21      0.0816923000
_diffrn_orient_matrix_UB_22      0.0146628000
_diffrn_orient_matrix_UB_23      -0.0127262000
_diffrn_orient_matrix_UB_31      -0.0177646000
_diffrn_orient_matrix_UB_32      0.0420839000
_diffrn_orient_matrix_UB_33      0.0110064000
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            119978
_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         70.000
_diffrn_reflns_theta_min         2.071
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
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    1.121
_exptl_crystal_description       prism
_exptl_crystal_F_000             7640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
The unit cell of C92H68F6Ir2N16P contains disordered molecules of solvent have been treated as a diffuse contribution to the overall scattering without specific atom positions by PLATON/SQUEEZE.                         

N: Total Potential Solvent Accessible Void Vol  (SOLV-Map Value) ...  9726 Ang^3
N: Electron Count Voids / Cell =   2913

2913e approximately correspond to 6 C3H6O + 4.1 C5H12 per f.u.
;
_refine_diff_density_max         1.695
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         21648
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+62.8045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20542
_reflns_number_total             21648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00901g3.cif
_cod_data_source_block           12309_vk281_sq
_cod_database_code               7713365
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C92 H68 F6 Ir2 N16 P'
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.435
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P1-F9
 1.5 with sigma of 0.02
 P1-F10
 1.7 with sigma of 0.02
 P1-F11
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F10) = Uanis(F3)
Uanis(F8) = Uanis(F5)
4. Others
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25'(H25C,H25D)
5.b Aromatic/amide H refined with riding coordinates:
 C4'(H4'), C4(H4), C5(H5), C5'(H5'), C6'(H6'), C6(H6), C7'(H7'), C7(H7),
 C10'(H10'), C10(H10), C11(H11), C11'(H11'), C13'(H13'), C13(H13), C15(H15),
 C15'(H15'), C16(H16), C16'(H16'), C18(H18), C18'(H18'), C19'(H19'), C19(H19),
 C24'(H24'), C24(H24), C27(H27), C27'(H27'), C28(H28), C28'(H28'), C29'(H29'),
 C29(H29), C30'(H30'), C30(H30), C33'(H33'), C33(H33), C34'(H34'), C34(H34),
 C35(H35), C35'(H35'), C36'(H36'), C36(H36), C39'(H39'), C39(H39), C40'(H40'),
 C40(H40), C41'(H41'), C41(H41), C42(H42), C42'(H42'), C45'(H45'), C45(H45),
 C46(H46), C46'(H46'), C47'(H47'), C47(H47), C48(H48), C48'(H48'), C51(H51),
 C51'(H51'), C52(H52), C52'(H52'), C53(H53), C53'(H53'), C54(H54), C54'(H54')
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_void_probe_radius 1.20
_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 2.690
_oxdiff_exptl_absorpt_empirical_full_min 0.627