A rare example of a compact heteroleptic cyclometalated iridium(iii) complex demonstrating well-separated dual emission.
Gitlina, Anastasia Yu; Ivonina, Maria V.; Sizov, Vladimir V.; Starova, Galina L.; Pushkarev, Anatoly P.; Volyniuk, Dmytro; Tunik, Sergey P.; Koshevoy, Igor O.; Grachova, Elena V.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7578–7586; doi:10.1039/c8dt01336e

data_7046210
_publ_section_title
;
 A rare example of a compact heteroleptic cyclometalated iridium(iii)
 complex demonstrating well-separated dual emission.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7578
_journal_page_last               7586
_journal_paper_doi               10.1039/c8dt01336e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C52 H36 Ir N4 O4, F6 P, 0.75(C H2 Cl2), 0.5(C4 H8 O2)'
_chemical_formula_sum            'C54.75 H41.5 Cl1.5 F6 Ir N4 O5 P'
_chemical_formula_weight         1225.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                110.0183(19)
_cell_angle_beta                 99.1822(17)
_cell_angle_gamma                100.8218(19)
_cell_formula_units_Z            2
_cell_length_a                   12.8631(3)
_cell_length_b                   14.9901(4)
_cell_length_c                   16.3368(3)
_cell_measurement_reflns_used    28117
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      75.8140
_cell_measurement_theta_min      3.5770
_cell_volume                     2820.28(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega    2.00   29.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287   38.0000  -90.0000 27

  2 omega  -70.00   34.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287   57.0000    0.0000 104

  3 omega  -49.00   36.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287   38.0000  150.0000 85

  4 omega    4.00   79.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       40.1287  -99.0000   60.0000 75

  5 omega   36.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  120.0000 79

  6 omega   88.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  150.0000 27

  7 omega   56.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  150.0000 27

  8 omega   51.00  134.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  120.0000 83

  9 omega  116.00  173.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  150.0000 57

 10 omega  141.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000   90.0000 37

 11 omega   89.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 26

 12 omega  108.00  143.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -90.0000 35

 13 omega  115.00  153.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -150.0000 38

 14 omega  138.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -180.0000 38

 15 omega   68.00  129.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       40.1287  178.0000  -90.0000 61

 16 omega   52.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000   90.0000 62

 17 omega   52.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  150.0000 57

 18 omega   40.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 50

 19 omega   47.00  104.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000   30.0000 57

 20 omega   55.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -90.0000 33

 21 omega   56.00  143.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -120.0000 87

 22 omega   75.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -120.0000 40

 23 omega   36.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 53

 24 omega   40.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 30

 25 omega   35.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 40

 26 omega   35.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 32

 27 omega   35.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 54

 28 omega -107.00  -22.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287  -57.0000 -150.0000 85

 29 omega -106.00  -46.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287  -57.0000   60.0000 60

 30 omega  -61.00  -14.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287  -38.0000 -120.0000 47

 31 omega  -40.00  -11.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287  -57.0000   60.0000 29

 32 omega  -43.00   34.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -      -40.1287   57.0000 -150.0000 77

 33 omega    7.00   32.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   87.0000  -35.8180 25

 34 omega   14.00   40.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   69.0000  -94.4091 26

 35 omega    8.00   33.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   85.0000   96.5586 25

 36 omega    9.00   44.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   81.0000   30.4025 35

 37 omega   17.00   42.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   81.0000  141.6626 25

 38 omega   18.00   43.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   79.0000  -77.2153 25

 39 omega   17.00   44.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   81.0000 -147.6330 27

 40 omega   17.00   44.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       52.0000   82.0000  -26.8406 27

 41 omega   22.00   47.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   78.0000 -172.7663 25

 42 omega   26.00   52.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   77.0000   58.1061 26

 43 omega   30.00   57.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000 -108.8749 27

 44 omega   34.00   65.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  -74.0314 31

 45 omega   35.00   67.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000   79.3500 32

 46 omega   35.00   62.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000    8.8411 27

 47 omega   34.00   60.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000 -165.2779 26

 48 omega   35.00   62.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000  162.3074 27

 49 omega   41.00   68.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   67.0000  -24.4637 27

 50 omega   43.00   71.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   74.0000  124.9182 28

 51 omega   44.00   99.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   72.0000 -115.7754 55

 52 omega  118.00  145.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   72.0000   38.9164 27

 53 omega   43.00   69.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   72.0000   38.9164 26

 54 omega   47.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   72.0000   96.2854 31

 55 omega   49.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   67.0000   -7.8839 41

 56 omega   55.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   75.0000 -177.4576 26

 57 omega   57.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   65.0000  163.2056 27

 58 omega   55.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   72.0000   54.4080 31

 59 omega   64.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   52.0000  -31.9983 27

 60 omega   65.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   62.0000 -149.9823 34

 61 omega  145.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   77.0000   12.2210 33

 62 omega   66.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   77.0000   12.2210 29

 63 omega   67.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   75.0000   80.3353 47

 64 omega  133.00  160.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   75.0000   80.3353 27

 65 omega   69.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   65.0000  139.2064 26

 66 omega   76.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000  137.0763 40

 67 omega   78.00  104.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -85.6655 26

 68 omega   79.00  152.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -60.0000 73

 69 omega  116.00  163.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 47

 70 omega   79.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 26

 71 omega   84.00  111.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 27

 72 omega  144.00  171.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 27

 73 omega   79.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 33

 74 omega   84.00  121.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 37

 75 omega   79.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 27

 76 omega   83.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 30

 77 omega   79.00  146.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -30.0000 67

 78 omega   80.00  155.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -90.0000 75

 79 omega  127.00  154.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000    0.0000 27

 80 omega   82.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000    0.0000 27

 81 omega  114.00  166.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  150.0000 52

 82 omega   79.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  150.0000 34

 83 omega   79.00  111.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   30.0000 32

 84 omega   79.00  158.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -120.0000 79

 85 omega   79.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   90.0000 43

 86 omega   32.00   57.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   75.0000   -9.9039 25

 87 omega   39.00   66.00   1.0000    1.2000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   75.0000  -48.4233 27

 88 omega   47.00   74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   72.0000  139.3717 27

 89 omega   52.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   75.0000 -111.2038 31

 90 omega   56.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   69.0000  -44.6526 27

 91 omega   58.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   77.0000   74.6971 26

 92 omega   59.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   74.0000  166.2212 26

 93 omega   71.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0000   74.0000 -148.6023 26

 94 omega   81.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   70.0000  -69.6325 25

 95 omega   83.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000    0.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0826833000
_diffrn_orient_matrix_UB_12      -0.0892533000
_diffrn_orient_matrix_UB_13      -0.0761819000
_diffrn_orient_matrix_UB_21      -0.0891909000
_diffrn_orient_matrix_UB_22      0.0169231000
_diffrn_orient_matrix_UB_23      0.0519459000
_diffrn_orient_matrix_UB_31      -0.0317170000
_diffrn_orient_matrix_UB_32      0.0677356000
_diffrn_orient_matrix_UB_33      -0.0469102000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57831
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         4.078
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       tables
_exptl_crystal_F_000             1219
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.651
_refine_diff_density_min         -2.566
_refine_diff_density_rms         0.127
_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     698
_refine_ls_number_reflns         10598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0763P)^2^+6.7792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9733
_reflns_number_total             10598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01336e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7046210--7046212.cif.'
_cod_original_cell_volume        2820.27(11)
_cod_original_formula_sum        'C54.75 H41.50 Cl1.50 F6 Ir N4 O5 P'
_cod_database_code               7046210
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid body (RIGU) restrains
 F1, F6, F5, F4, F3, F2
 with sigma for 1-2 distances of 0.4 and sigma for 1-3 distances of 0.04
3. Others
 Fixed Sof: Cl2(0.75) Cl6(0.75) C53(0.75) H53A(0.75) H53B(0.75) O6(0.5)
 O5(0.5) C56(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57(0.5) C55(0.5) H55A(0.5)
 H55B(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C55(H55A,H55B)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C8(H8), C28(H28), C12(H12), C17(H), C4(H4), C22(H22), C42(H42),
 C7(H7), C6(H6), C47(H47), C21(H21), C26(H26), C5(H5), C13(H13), C16(H16),
 C43(H43), C44(H44), C14(H14), C20(H20), C24(H24), C18(H18), C19(H19), C27(HA),
 C15(H15), C23(H23), C49(H49), C50(H50), C48(H48)
4.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C57(H57A,H57B,H57), C54(H54A,H54B,
 H54C)
4.d :
 C25(H25)
;
_shelx_res_checksum              56452
_shelx_fab_checksum              93329
_olex2_submission_special_instructions 'No special instructions were received'