Photoluminescence and Electrochemiluminescence Dual-Signaling Sensors for Selective Detection of Cysteine Based on Iridium(III) Complexes.
Kim, Taemin; Hong, Jong-In; ACS omega 4 (2019) 12616–12625; doi:10.1021/acsomega.9b01501

data_4516972
_publ_section_title
;
 Photoluminescence and Electrochemiluminescence Dual-Signaling Sensors for
 Selective Detection of Cysteine Based on Iridium(III) Complexes.
;
_journal_issue                   7
_journal_name_full               'ACS omega'
_journal_page_first              12616
_journal_page_last               12625
_journal_paper_doi               10.1021/acsomega.9b01501
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C33 H27 Ir N2 O6'
_chemical_formula_sum            'C33 H27 Ir N2 O6'
_chemical_formula_weight         739.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6397(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.88223(7)
_cell_length_b                   15.04355(10)
_cell_length_c                   15.39444(8)
_cell_measurement_reflns_used    21154
_cell_measurement_temperature    99.9(9)
_cell_measurement_theta_max      76.1370
_cell_measurement_theta_min      4.7330
_cell_volume                     2751.60(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2262
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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      1.00  32.00   1.00    6.34    --   41.49 -99.00-180.00   31
  2  \w    -35.00  74.00   1.00    6.34    --   41.49 -77.00-180.00  109
  3  \w     13.00  82.00   1.00    6.34    --   41.49 -99.00 -30.00   69
  4  \w     37.00  77.00   1.00    4.13    --  112.00 -77.00-120.00   40
  5  \w     41.00  73.00   1.00    4.13    --  112.00 -94.00-120.00   32
  6  \w    101.00 136.00   1.00    4.13    --  112.00 -77.00-120.00   35
  7  \w    100.00 129.00   1.00    4.13    --  112.00 111.00 150.00   29
  8  \w     29.00  83.00   1.00    4.13    --  112.00 -94.00 150.00   54
  9  \w     64.00 129.00   1.00    4.13    --  112.00 -45.00  90.00   65
 10  \w    131.00 157.00   1.00    4.13    --  112.00 111.00 150.00   26
 11  \w    141.00 166.00   1.00    4.13    --  112.00   0.00  30.00   25
 12  \w     81.00 108.00   1.00    4.13    --  112.00 -94.00-120.00   27
 13  \w    112.00 177.00   1.00    4.13    --  112.00  81.00 129.00   65
 14  \w    100.00 172.00   1.00    4.13    --  112.00 111.00-180.00   72
 15  \w     27.00 109.00   1.00    4.13    --  112.00   0.00  30.00   82
 16  \w   -118.00  33.00   1.00    6.34    --  -41.49   0.00  60.00  151
 17  \w    -43.00 -13.00   1.00    6.34    --  -41.49 -57.00 -60.00   30
 18  \w     24.00  89.00   1.00    6.34    --   41.49-125.00 120.00   65
 19  \w     17.00  67.00   1.00    6.34    --   41.49  38.00   0.00   50
 20  \w      6.00  34.00   1.00    6.34    --   42.00  87.00  50.73   28
 21  \w      5.00  32.00   1.00    6.34    --   42.00  89.00-176.89   27
 22  \w      6.00  34.00   1.00    6.34    --   42.00  87.00 -47.04   28
 23  \w     12.00  37.00   1.00    6.34    --   46.00  83.00  13.47   25
 24  \w     16.00  41.00   1.00    6.34    --   50.00  82.00-107.56   25
 25  \w     20.00  45.00   1.00    6.34    --   54.00  81.00  -1.79   25
 26  \w     20.00  45.00   1.00    6.34    --   54.00  81.00 170.67   25
 27  \w     28.00 134.00   1.00    6.34    --   58.00  77.00-158.31  106
 28  \w     33.00 113.00   1.00    6.34    --   62.00  75.00  37.47   80
 29  \w     29.00  69.00   1.00    6.34    --   62.00  77.00 104.56   40
 30  \w     34.00  76.00   1.00    6.34    --   66.00  76.00 -63.98   42
 31  \w     91.00 121.00   1.00    6.34    --   66.00  76.00-105.75   30
 32  \w     35.00  62.00   1.00    6.34    --   66.00  76.00-105.75   27
 33  \w     37.00  74.00   1.00    6.34    --   66.00  61.00  99.11   37
 34  \w     37.00  74.00   1.00    6.34    --   70.00  77.00 -90.28   37
 35  \w     38.00 102.00   1.00    6.34    --   70.00  76.00  -7.85   64
 36  \w     38.00  70.00   1.00    6.34    --   70.00  76.00 150.81   32
 37  \w    125.00 178.00   1.00    4.13    --  112.00  77.00-150.00   53
 38  \w     80.00 128.00   1.00    4.13    --  112.00  77.00-120.00   48
 39  \w     79.00 122.00   1.00    4.13    --  112.00  77.00-150.00   43
 40  \w    117.00 163.00   1.00    4.13    --  112.00  61.00  30.00   46
 41  \w     85.00 112.00   1.00    4.13    --  112.00  61.00-150.00   27
 42  \w     86.00 118.00   1.00    4.13    --  112.00  61.00 120.00   32
 43  \w    150.00 178.00   1.00    4.13    --  112.00  77.00-120.00   28
 44  \w     84.00 114.00   1.00    4.13    --  112.00  61.00  30.00   30
 45  \w     79.00 176.00   1.00    4.13    --  112.00  77.00  90.00   97
 46  \w     83.00 115.00   1.00    4.13    --  112.00  61.00 -60.00   32
 47  \w     80.00 160.00   1.00    4.13    --  112.00  77.00 -30.00   80
 48  \w     84.00 111.00   1.00    4.13    --  112.00  61.00 -90.00   27
 49  \w    143.00 169.00   1.00    4.13    --  112.00  61.00-180.00   26
 50  \w     83.00 119.00   1.00    4.13    --  112.00  61.00-180.00   36
 51  \w    139.00 172.00   1.00    4.13    --  112.00  77.00   0.00   33
 52  \w     59.00 115.00   1.00    4.13    --  112.00-111.00 120.00   56
 53  \w     79.00 110.00   1.00    4.13    --  112.00  77.00-180.00   31
 54  \w     79.00 110.00   1.00    4.13    --  112.00  77.00 -90.00   31
 55  \w    131.00 170.00   1.00    4.13    --  112.00  77.00 120.00   39
 56  \w     79.00 108.00   1.00    4.13    --  112.00  77.00  30.00   29
 57  \w     79.00 119.00   1.00    4.13    --  112.00  77.00   0.00   40
 58  \w     79.00 130.00   1.00    4.13    --  112.00  77.00 150.00   51
 59  \w     79.00 124.00   1.00    4.13    --  112.00  77.00 120.00   45
 60  \w     79.00 120.00   1.00    4.13    --  112.00  77.00 -60.00   41
 61  \w    134.00 168.00   1.00    4.13    --  112.00  77.00 -60.00   34
 62  \w     79.00 158.00   1.00    4.13    --  112.00  77.00  60.00   79
 63  \w     67.00 110.00   1.00    4.13    --  112.00-111.00-120.00   43
 64  \w     37.00  80.00   1.00    4.13    --  112.00-111.00 -60.00   43
 65  \w     83.00 116.00   1.00    4.13    --  112.00-111.00 -60.00   33
 66  \w     83.00 141.00   1.00    4.13    --  112.00  61.00   0.00   58
 67  \w     83.00 112.00   1.00    4.13    --  112.00  61.00 150.00   29
 68  \w     84.00 131.00   1.00    4.13    --  112.00  61.00  60.00   47
 69  \w     29.00 100.00   1.00    4.13    --  112.00 -94.00  30.00   71
 70  \w     91.00 116.00   1.00    4.13    --  112.00-111.00 -30.00   25
 71  \w     83.00 109.00   1.00    4.13    --  112.00  61.00 -30.00   26
 72  \w     38.00  79.00   1.00    4.13    --  112.00-111.00 -30.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0414208000
_diffrn_orient_matrix_UB_12      -0.0423136000
_diffrn_orient_matrix_UB_13      -0.0857201000
_diffrn_orient_matrix_UB_21      -0.1038406000
_diffrn_orient_matrix_UB_22      0.0613509000
_diffrn_orient_matrix_UB_23      0.0000560000
_diffrn_orient_matrix_UB_31      0.0656588000
_diffrn_orient_matrix_UB_32      0.0702223000
_diffrn_orient_matrix_UB_33      -0.0516804000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27302
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.579
_diffrn_reflns_theta_min         4.743
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.820
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.44a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0150
_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^)+(0.0209P)^2^+5.7056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2844
_reflns_number_total             2877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01501_si_002.cif
_cod_data_source_block           ir(appy)2acac
_cod_database_code               4516972
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C33H27IrN2O6
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1BA(H1BA)
2.b X=CH2 refined with riding coordinates:
 C6(H6A,H6B)
;
_shelx_res_checksum              15474
_shelx_hkl_checksum              35575
_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 1.758
_oxdiff_exptl_absorpt_empirical_full_min 0.690