Synthesis, characterization, photophysics and electrochemical study of luminescent iridium(iii) complexes with isocyanoborate ligands.
Chan, Kin-Cheung; Chu, Wing-Kin; Yiu, Shek-Man; Ko, Chi-Chiu; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15135–15144; doi:10.1039/c5dt00904a

data_7034909
_publ_section_title
;
 Synthesis, characterization, photophysics and electrochemical study of
 luminescent iridium(iii) complexes with isocyanoborate ligands.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15135
_journal_page_last               15144
_journal_paper_doi               10.1039/c5dt00904a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H16 B Cl F19 Ir N4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C48.5 H17 B Cl2 F19 Ir N4'
_chemical_formula_weight         1290.57
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Fri Jul 18 17:17:09 2014'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_audit_update_record
;
2015-02-23 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 112.2864(15)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   21.9289(3)
_cell_length_b                   13.81974(14)
_cell_length_c                   16.7040(2)
_cell_measurement_reflns_used    10938
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.6234
_cell_measurement_theta_min      3.8668
_cell_volume                     4684.03(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -2.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 56

  2 omega  -24.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 63

  3 omega   34.00   60.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   57.0000   60.0000 26

  4 omega   44.00  125.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000  -30.0000 81

  5 omega   98.00  124.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   57.0000   60.0000 26

  6 omega   -3.00   95.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000 -125.0000  -30.0000 98

  7 omega -131.00 -105.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000 -142.0000 -131.0000 26

  8 omega -108.00  -56.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  120.0000 52

  9 omega   38.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 33

 10 omega   43.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 29

 11 omega   37.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 34

 12 omega   48.00   74.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   83.0000 26

 13 omega   51.00  130.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000 -180.0000 79

 14 omega   40.00   67.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000    0.0000 27

 15 omega   39.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 33

 16 omega  128.00  176.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000  150.0000 48

 17 omega   38.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 32

 18 omega   39.00   65.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 26

 19 omega   39.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 33

 20 omega   72.00  125.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000    0.0000 53

 21 omega   80.00  146.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   83.0000 66

 22 omega   92.00  118.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   44.0000 26

 23 omega   46.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   44.0000 25

 24 omega  -21.00   69.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

 25 omega  -70.00  -39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -180.0000 31
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0624334000
_diffrn_orient_matrix_UB_12      0.0238011000
_diffrn_orient_matrix_UB_13      -0.0797577000
_diffrn_orient_matrix_UB_21      -0.0159090000
_diffrn_orient_matrix_UB_22      -0.1087468000
_diffrn_orient_matrix_UB_23      -0.0141168000
_diffrn_orient_matrix_UB_31      -0.0401320000
_diffrn_orient_matrix_UB_32      0.0061140000
_diffrn_orient_matrix_UB_33      0.0581232000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21237
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.87
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         8305
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+8.7274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                7382
_reflns_number_total             8305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00904a2.cif
_cod_data_source_block           071714a_cheung
_cod_depositor_comments
'Adding full bibliography for 7034908--7034910.cif.'
_cod_original_cell_volume        4684.04(10)
_cod_original_formula_sum        'C48.50 H17 B Cl2 F19 Ir N4'
_cod_database_code               7034909
_cell_oxdiff_angle_alpha         89.961(2)
_cell_oxdiff_angle_beta          112.304(3)
_cell_oxdiff_angle_gamma         90.010(2)
_cell_oxdiff_length_a            21.9364(6)
_cell_oxdiff_length_b            13.8180(4)
_cell_oxdiff_length_c            16.7025(5)
_cell_oxdiff_measurement_reflns_used 10644
_cell_oxdiff_volume              4684.0(2)
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13