Unusually Fast Phosphorescence from Ir(III) Complexes via Dinuclear Molecular Design.
Shafikov, Marsel Z.; Daniels, Ruth; Kozhevnikov, Valery N.; The journal of physical chemistry letters  (2019) 7015–7024; doi:10.1021/acs.jpclett.9b03002

data_8000321
_publ_section_title
;
 Unusually Fast Phosphorescence from Ir(III) Complexes via Dinuclear
 Molecular Design.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              7015
_journal_page_last               7024
_journal_paper_doi               10.1021/acs.jpclett.9b03002
_journal_year                    2019
_chemical_formula_moiety         'C60 H56 Cl Ir N6'
_chemical_formula_sum            'C60 H56 Cl Ir N6'
_chemical_formula_weight         1088.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                75.089(2)
_cell_angle_beta                 68.707(3)
_cell_angle_gamma                78.676(2)
_cell_formula_units_Z            4
_cell_length_a                   15.7708(4)
_cell_length_b                   18.1452(5)
_cell_length_c                   20.4160(6)
_cell_measurement_reflns_used    31499
_cell_measurement_temperature    123.00(19)
_cell_measurement_theta_max      73.9750
_cell_measurement_theta_min      2.4510
_cell_volume                     5225.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.958
_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   -130.00 -34.00   1.00    7.50    --  -43.39 178.00 150.00   96
  2  \w    -26.00  69.00   1.00    7.50    --   43.39 -57.00   0.00   95
  3  \w     18.00 113.00   1.00    7.50    --   43.39  57.00 150.00   95
  4  \w     30.00 136.00   1.00   30.00    --  104.50 -77.00 -60.00  106
  5  \w     31.00  91.00   1.00   30.00    --  104.50 -30.00 -90.00   60
  6  \w     31.00  91.00   1.00   30.00    --  104.50 -30.00 120.00   60
  7  \w     31.00 121.00   1.00   30.00    --  104.50-125.00 -30.00   90
  8  \w     80.00 175.00   1.00   30.00    --  104.50  45.00 150.00   95
  9  \w     30.00 136.00   1.00   30.00    --  104.50 -77.00  90.00  106
 10  \w     34.00  98.00   1.00   30.00    --  104.50 -45.00-180.00   64
 11  \w     26.00 144.00   1.00   30.00    --  104.50 -15.00 -30.00  118
 12  \w     18.00 113.00   1.00    7.50    --   43.39  57.00  90.00   95
 13  \w     12.00 118.00   1.00    7.50    --   43.39  77.00 -30.00  106
 14  \w     18.00 113.00   1.00    7.50    --   43.39  57.00-120.00   95
 15  \w     78.00 174.00   1.00   30.00    --  104.50  61.00 -90.00   96
 16  \w     80.00 175.00   1.00   30.00    --  104.50  45.00 -30.00   95
 17  \w     78.00 145.00   1.00   30.00    --  104.50  61.00-150.00   67
 18  \w     78.00 178.00   1.00   30.00    --  104.50  30.00  60.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0503269000
_diffrn_orient_matrix_UB_12      -0.0161627000
_diffrn_orient_matrix_UB_13      -0.0460169000
_diffrn_orient_matrix_UB_21      -0.0763081000
_diffrn_orient_matrix_UB_22      -0.0314002000
_diffrn_orient_matrix_UB_23      0.0687323000
_diffrn_orient_matrix_UB_31      -0.0527394000
_diffrn_orient_matrix_UB_32      0.0810830000
_diffrn_orient_matrix_UB_33      -0.0009263000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56260
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.066
_diffrn_reflns_theta_min         2.372
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.749
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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    1.384
_exptl_crystal_description       prism
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.947
_refine_diff_density_min         -1.939
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         20352
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.2709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17799
_reflns_number_total             20352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b03002_si_003.cif
_cod_data_source_block           q047
_cod_database_code               8000321
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C60 H56 Cl Ir N6'
_chemical_oxdiff_usercomment     Yersin_Shafikov_RED-280
_reflns_odcompleteness_completeness 99.13
_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. Restrained distances
 C16-C17 \\sim C16-C18 \\sim C16-C19 \\sim C16-C17A \\sim C16-C18A \\sim
C16-C19A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C45 \\sim C46 \\sim C48 \\sim C47 \\sim C46A \\sim C47A \\sim C48A: within 1.7A
with sigma of 0.005 and sigma for terminal atoms of 0.005
C16 \\sim C18 \\sim C19A \\sim C17A \\sim C17 \\sim C19 \\sim C18A: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(1)
 Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C17A)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C17)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C19)=Sof(H19D)=Sof(H19E)=Sof(H19F)=FVAR(2)
5.a Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19A(H19A,H19B,H19C), C17A(H17A,H17B,H17C), C17(H17D,
 H17E,H17F), C19(H19D,H19E,H19F), C18A(H18D,H18E,H18F)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C42(H42), C75(H75), C68(H68), C8(H8), C44(H44), C27(H27), C30(H30),
 C72(H72), C28(H28), C4(H4), C74(H74), C57(H57), C65(H65), C32(H32), C24(H24),
 C60(H60), C5(H5), C21(H21), C20(H20), C29(H29), C80(H80), C64(H64), C101(H101),
  C50(H50), C15(H15), C103(H103), C14(H14), C36(H36), C92(H92), C114(H114),
 C35(H35), C81(H81), C54(H54), C59(H59), C111(H111), C113(H113), C90(H90),
 C58(H58), C87(H87), C34(H34), C116(H116), C84(H84), C93(H93), C53(H53),
 C33(H33), C112(H112), C52(H52), C96(H96), C51(H51), C89(H89), C118(H118),
 C88(H88), C120(H120), C94(H94), C95(H95), C117(H117), C119(H119)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C83(H83A,H83B,H83C), C82(H82A,H82B,H82C), C61(H61A,H61B,
 H61C), C77(H77A,H77B,H77C), C105(H10A,H10B,H10C), C46(H46A,H46B,H46C),
 C79(H79A,H79B,H79C), C107(H10D,H10E,H10F), C22(H22A,H22B,H22C), C106(H10G,H10H,
 H10I), C78(H78A,H78B,H78C), C48(H48A,H48B,H48C), C1(H1A,H1B,H1C), C47(H47A,
 H47B,H47C), C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F), C48A(H48D,H48E,H48F)
;
_olex2_date_sample_data_collection 2017-04-11
_olex2_date_sample_submission    2017-04-11
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a Lindemann tube oil'
_olex2_submission_original_sample_id RED-280
_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 2.958
_oxdiff_exptl_absorpt_empirical_full_min 0.574