Near Infrared Phosphorescent Dinuclear Ir(III) Complex Exhibiting Unusually Slow Intersystem Crossing and Dual Emissive Behavior.
Shafikov, Marsel Z.; Zaytsev, Andrey V.; Suleymanova, Alfiya F.; Brandl, Fabian; Kowalczyk, Aleksandra; Gapińska, Magdalena; Kowalski, Konrad; Kozhevnikov, Valery N.; Czerwieniec, Rafał; The journal of physical chemistry letters  (2020) 5849–5855; doi:10.1021/acs.jpclett.0c01276

data_8000439
_publ_section_title
;
 Near Infrared Phosphorescent Dinuclear Ir(III) Complex Exhibiting
 Unusually Slow Intersystem Crossing and Dual Emissive Behavior.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              5849
_journal_page_last               5855
_journal_paper_doi               10.1021/acs.jpclett.0c01276
_journal_year                    2020
_chemical_formula_moiety         'C78 H80 Cl2 F10 Ir2 N6 O2 S2, 2.5(C H2 Cl2)'
_chemical_formula_sum            'C80.5 H85 Cl7 F10 Ir2 N6 O2 S2'
_chemical_formula_weight         2055.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-28
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.08060(10)
_cell_length_b                   15.66330(10)
_cell_length_c                   23.8140(2)
_cell_measurement_reflns_used    42658
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.1230
_cell_measurement_theta_min      3.6950
_cell_volume                     4106.70(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -97.00  -2.00   1.00    2.00    --  -41.42 125.00 120.00   95
  2  \w    -66.00  33.00   1.00    2.00    --  -41.42  37.00 150.00   99
  3  \w     13.00 115.00   1.00    2.00    --   41.42  57.00   0.00  102
  4  \w     17.00 116.00   1.00    2.00    --   41.42  37.00 120.00   99
  5  \w     36.00 116.00   1.00   10.00    --  112.00-111.00 -90.00   80
  6  \w     36.00 116.00   1.00   10.00    --  112.00-114.00  36.00   80
  7  \w     39.00  77.00   1.00   10.00    --  112.00 -45.00 -60.00   38
  8  \w     39.00  77.00   1.00   10.00    --  112.00 -45.00   0.00   38
  9  \w     36.00  69.00   1.00   10.00    --  112.00 -30.00 150.00   33
 10  \w     36.00 116.00   1.00   10.00    --  112.00-111.00  90.00   80
 11  \w     36.00 145.00   1.00   10.00    --  112.00 -77.00 -90.00  109
 12  \w     40.00 141.00   1.00   10.00    --  112.00 -61.00  60.00  101
 13  \w     36.00  69.00   1.00   10.00    --  112.00 -30.00-180.00   33
 14  \w     36.00 116.00   1.00   10.00    --  112.00-111.00-180.00   80
 15  \w     30.00 158.00   1.00   10.00    --  112.00 -15.00 -90.00  128
 16  \w     40.00  93.00   1.00   10.00    --  112.00 -56.00 -90.00   53
 17  \w     29.00 109.00   1.00   10.00    --  112.00 -94.00-150.00   80
 18  \w     29.00 109.00   1.00   10.00    --  112.00 -94.00  90.00   80
 19  \w     30.00 158.00   1.00   10.00    --  112.00 -15.00  30.00  128
 20  \w     36.00  69.00   1.00   10.00    --  112.00 -30.00-120.00   33
 21  \w     36.00  69.00   1.00   10.00    --  112.00 -30.00-150.00   33
 22  \w   -126.00 -40.00   1.00    2.00    --  -41.42-173.00-104.00   86
 23  \w     13.00 115.00   1.00    2.00    --   41.42  57.00-150.00  102
 24  \w    -33.00  66.00   1.00    2.00    --   41.42 -37.00-150.00   99
 25  \w      9.00 118.00   1.00    2.00    --   41.42  77.00 -90.00  109
 26  \w      9.00 118.00   1.00    2.00    --   41.42  77.00 120.00  109
 27  \w     84.00 158.00   1.00   10.00    --  112.00  30.00-180.00   74
 28  \w     86.00 158.00   1.00   10.00    --  112.00  45.00 120.00   72
 29  \w     59.00 158.00   1.00   10.00    --  112.00  15.00 120.00   99
 30  \w     86.00 158.00   1.00   10.00    --  112.00  45.00 -30.00   72
 31  \w     83.00 158.00   1.00   10.00    --  112.00  61.00-150.00   75
 32  \w     83.00 158.00   1.00   10.00    --  112.00  61.00   0.00   75
 33  \w     83.00 158.00   1.00   10.00    --  112.00  61.00-120.00   75
 34  \w     83.00 158.00   1.00   10.00    --  112.00  61.00  30.00   75
 35  \w     83.00 158.00   1.00   10.00    --  112.00  61.00-180.00   75
 36  \w     79.00 105.00   1.00   10.00    --  112.00  77.00  60.00   26
 37  \w     84.00 158.00   1.00   10.00    --  112.00  30.00 -60.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67621
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.387
_diffrn_reflns_theta_min         3.384
_exptl_absorpt_coefficient_mu    9.367
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
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    1.662
_exptl_crystal_description       needle
_exptl_crystal_F_000             2042
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         8564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0468P)^2^+10.3780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8035
_reflns_number_total             8564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz0c01276_si_002.cif
_cod_data_source_block           s124
_cod_depositor_comments          'Adding full bibliography for 8000439.cif.'
_cod_original_formula_sum        'C80.50 H85 Cl7 F10 Ir2 N6 O2 S2'
_cod_database_code               8000439
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C1A(0.25) H1AA(0.25) H1AB(0.25) Cl5(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C40(H40A,H40B), C1A(H1AA,H1AB)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C21(H21A,H21B,
 H21C)
;
_shelx_res_checksum              34343
_shelx_hkl_checksum              13204
_olex2_date_sample_data_collection 2019-10-21
_olex2_date_sample_submission    2019-10-16
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_original_sample_id AV-VK2-31-6
_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
- B-factor correction
;