Azobenzene-Appended Bis-Cyclometalated Iridium(III) Bipyridyl Complexes
Telleria, Ainara; Pérez-Miqueo, Jorge; Altube, Ainhoa; García-Lecina, Eva; de Cózar, Abel; Freixa, Zoraida; Organometallics 34 (2015) 5513–; doi:10.1021/acs.organomet.5b00838

data_4088089
_publ_section_title
;
 Azobenzene-Appended Bis-Cyclometalated Iridium(III) Bipyridyl Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5513
_journal_paper_doi               10.1021/acs.organomet.5b00838
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C56 H38 Br2 Ir N8, F6 P'
_chemical_formula_sum            'C56 H38 Br2 F6 Ir N8 P'
_chemical_formula_weight         1319.93
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-13T11:07:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                85.8675(15)
_cell_angle_beta                 83.4417(17)
_cell_angle_gamma                81.9153(15)
_cell_formula_units_Z            4
_cell_length_a                   15.2882(3)
_cell_length_b                   19.3171(3)
_cell_length_c                   20.0260(4)
_cell_measurement_reflns_used    18557
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.7
_cell_measurement_theta_min      2.901
_cell_measurement_wavelength     1.54184
_cell_volume                     5807.62(19)
_computing_cell_refinement
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_collection
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_reduction
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'OLEX2 (Dolomanov et al, 2009)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
  1 omega -113.00  -68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756 -144.0000   43.0000 45

  2 omega   14.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   38.0000   30.0000 93

  3 omega  -32.00   66.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756  -38.0000 -150.0000 98

  4 omega   11.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000  120.0000 87

  5 omega -129.00  -65.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -61.0000  120.0000 64

  6 omega  -77.00  -36.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   77.0000  -90.0000 41

  7 omega   24.00  109.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000   60.0000 85

  8 omega  100.00  158.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  125.0000 -120.0000 58

  9 omega   77.00  151.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   77.0000 -150.0000 74

 10 omega   67.00  108.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -180.0000 41

 11 omega   25.00   59.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -180.0000 34

 12 omega   34.00   64.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  -30.0000 30

 13 omega   25.00   52.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  150.0000 27

 14 omega   53.00   87.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  150.0000 34

 15 omega   94.00  121.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000    0.0000 27

 16 omega   39.00   73.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000   30.0000 34

 17 omega   87.00  134.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  125.0000   30.0000 47

 18 omega   38.00  135.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -77.0000 -120.0000 97

 19 omega   25.00   52.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000    0.0000 27

 20 omega   70.00   95.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000    0.0000 25

 21 omega   33.00   78.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000 -120.0000 45

 22 omega   96.00  121.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000 -120.0000 25

 23 omega   30.00   63.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -120.0000 33

 24 omega   39.00   72.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000    0.0000 33

 25 omega   34.00  139.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609    0.0000   60.0000 105

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0730805
_diffrn_orient_matrix_UB_12      0.0345325
_diffrn_orient_matrix_UB_13      0.0265827
_diffrn_orient_matrix_UB_21      -0.0422181
_diffrn_orient_matrix_UB_22      -0.012589
_diffrn_orient_matrix_UB_23      0.072691
_diffrn_orient_matrix_UB_31      0.0578997
_diffrn_orient_matrix_UB_32      -0.0718241
_diffrn_orient_matrix_UB_33      0.0050004
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray micro-source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45282
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.84
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.65592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.51
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.1687
_exptl_crystal_size_mid          0.1378
_exptl_crystal_size_min          0.0411
_refine_diff_density_max         1.948
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         20928
_refine_ls_number_restraints     1061
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+13.8458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                16277
_reflns_number_total             20928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00838_si_004.cif
_cod_data_source_block           at146
_cod_database_code               4088089