Tuning the electrochemiluminescent properties of iridium complexes of N-heterocyclic carbene ligands.
Quan, Linh M.; Stringer, Bradley D.; Haghighatbin, Mohammad A.; Agugiaro, Johnny; Barbante, Gregory J.; Wilson, David J. D.; Hogan, Conor F.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 653–663; doi:10.1039/c8dt04433c

data_7048307
_publ_section_title
;
 Tuning the electrochemiluminescent properties of iridium complexes of
 N-heterocyclic carbene ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              653
_journal_page_last               663
_journal_paper_doi               10.1039/c8dt04433c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H19 F6 Ir N4'
_chemical_formula_sum            'C32 H19 F6 Ir N4'
_chemical_formula_weight         765.71
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-19
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-23 deposited with the CCDC.
2018-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5122(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.84307(11)
_cell_length_b                   15.66542(16)
_cell_length_c                   15.57142(16)
_cell_measurement_reflns_used    11033
_cell_measurement_temperature    172.97(14)
_cell_measurement_theta_max      73.6878
_cell_measurement_theta_min      2.8382
_cell_volume                     2642.44(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      172.97(14)
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -55.00   34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0319   46.0000 -142.0000 89

  2 omega -116.00  -16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0319  -38.0000   60.0000 100

  3 omega -113.00  -67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0319 -138.0000 -154.0000 46

  4 omega   13.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0319  -99.0000  -90.0000 57

  5 omega   28.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0319 -138.0000   93.0000 69

  6 omega   30.00   79.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -30.0000 -180.0000 49

  7 omega  128.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  125.0000   30.0000 48

  8 omega   26.00   98.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -95.0000  -30.0000 72

  9 omega   96.00  122.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  125.0000   30.0000 26

 10 omega   35.00   81.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -30.0000   90.0000 46

 11 omega   30.00   63.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -30.0000   60.0000 33

 12 omega   53.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -30.0000  120.0000 38

 13 omega   60.00  114.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295 -125.0000  120.0000 54

 14 omega   29.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -30.0000  -60.0000 61

 15 omega   48.00   86.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -95.0000   30.0000 38

 16 omega   46.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295   15.0000    0.0000 128

 17 omega  123.00  155.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295   45.0000 -150.0000 32

 18 omega   96.00  122.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295 -125.0000  -60.0000 26

 19 omega   33.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -30.0000    0.0000 58

 20 omega   38.00  130.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.5295  -77.0000  120.0000 92
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0410470000
_diffrn_orient_matrix_UB_12      -0.0546224000
_diffrn_orient_matrix_UB_13      0.0759129000
_diffrn_orient_matrix_UB_21      0.0312450000
_diffrn_orient_matrix_UB_22      -0.0817481000
_diffrn_orient_matrix_UB_23      -0.0495597000
_diffrn_orient_matrix_UB_31      0.1325250000
_diffrn_orient_matrix_UB_32      0.0023402000
_diffrn_orient_matrix_UB_33      0.0398464000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17700
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.851
_diffrn_reflns_theta_min         4.005
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.740
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0205
_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^)+(0.0263P)^2^+1.8640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5141
_reflns_number_total             5281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04433c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7048306--7048309.cif.'
_cod_database_code               7048307
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H19 N5 F6 Ir'
_reflns_odcompleteness_completeness 99.98
_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:
 C9(H9), C31(H31), C15(H15), C13(H13), C18(H18), C3(H3), C26(H26), C5(H5),
 C21(H21), C30(H30), C32(H32), C24(H24), C20(H20), C8(H8), C19(H19), C29(H29)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              56637
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 27/06/2013
_olex2_submission_special_instructions 'No special instructions were received'