Ir(iii) complex-based phosphorescence and electrochemiluminescence chemodosimetric probes for Hg(ii) ions with high selectivity and sensitivity.
Rhee, Hayoung; Kim, Taemin; Hong, Jong-In; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3803–3810; doi:10.1039/c8dt00309b

data_7045451
_publ_section_title
;
 Ir(iii) complex-based phosphorescence and electrochemiluminescence
 chemodosimetric probes for Hg(ii) ions with high selectivity and
 sensitivity.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3803
_journal_page_last               3810
_journal_paper_doi               10.1039/c8dt00309b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C26 H22 Ir N4'
_chemical_formula_sum            'C26 H22 Ir N4'
_chemical_formula_weight         582.67
_chemical_name_systematic        (ppy)2Ir(CH3CN)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-03 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.535(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9543(4)
_cell_length_b                   20.0441(5)
_cell_length_c                   9.0693(2)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    293.0(4)
_cell_measurement_theta_max      72.8070
_cell_measurement_theta_min      3.0120
_cell_volume                     2642.98(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2262
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_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    -64.00  15.00   1.00    4.21    --  -41.32  38.00 -90.00   79
  2  \w      2.00  29.00   1.00    4.21    --   41.32 -99.00-150.00   27
  3  \w     41.00  79.00   1.00    4.21    --   41.32-125.00 -60.00   38
  4  \w      9.00  76.00   1.00    4.21    --   41.32 -99.00  30.00   67
  5  \w     34.00  96.00   1.00    4.21    --   41.32-125.00 120.00   62
  6  \w    132.00 177.00   1.00   16.82    --  106.49  61.00-150.00   45
  7  \w     77.00 118.00   1.00   16.82    --  106.49  61.00-150.00   41
  8  \w     85.00 134.00   1.00   16.82    --  106.49  30.00 -90.00   49
  9  \w     33.00 116.00   1.00   16.82    --  106.49 -45.00  60.00   83
 10  \w    150.00 177.00   1.00   16.82    --  106.49  30.00 -90.00   27
 11  \w     33.00 121.00   1.00   16.82    --  106.49-125.00   0.00   88
 12  \w     98.00 131.00   1.00   16.82    --  106.49 125.00 150.00   33
 13  \w     79.00 137.00   1.00   16.82    --  106.49 -77.00 120.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0737312000
_diffrn_orient_matrix_UB_12      0.0209144000
_diffrn_orient_matrix_UB_13      -0.0845765000
_diffrn_orient_matrix_UB_21      -0.0393759000
_diffrn_orient_matrix_UB_22      -0.0504973000
_diffrn_orient_matrix_UB_23      -0.1266689000
_diffrn_orient_matrix_UB_31      -0.0650601000
_diffrn_orient_matrix_UB_32      0.0540641000
_diffrn_orient_matrix_UB_33      -0.0855815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10459
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.973
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_recrystallization_method 'slow vaporization.'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.890
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+4.5960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4646
_reflns_number_total             5203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00309b2.cif
_cod_data_source_block           exp_936
_cod_depositor_comments          'Adding full bibliography for 7045451.cif.'
_cod_database_code               7045451
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C27 H22Hg1Ir1 N202 '
_shelx_estimated_absorpt_t_max   0.637
_shelx_estimated_absorpt_t_min   0.437
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22)
2.b Fitted hexagon refined as free rotating group:
 C6(C7,C8,C9,C10,C11), C13(C14,C15,C16,C17,C12)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              25720
_shelx_fab_checksum              17803
_olex2_exptl_crystal_mounting_method 'nylon loop with Paratone oil '
_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 1.926
_oxdiff_exptl_absorpt_empirical_full_min 0.661