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_4088092
_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         'C44 H28 F4 Ir N8, F6 P, C H2 Cl2'
_chemical_formula_sum            'C45 H30 Cl2 F10 Ir N8 P'
_chemical_formula_weight         1166.84
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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             2014-11-04T13:47:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.080(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4848(6)
_cell_length_b                   9.4724(2)
_cell_length_c                   20.0655(7)
_cell_measurement_reflns_used    10483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.679
_cell_measurement_theta_min      2.028
_cell_measurement_wavelength     0.71073
_cell_volume                     4262.8(2)
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
  1 omega   91.00  117.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000  120.0000 26

  2 omega    2.00   53.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -38.0000 -120.0000 51

  3 omega  -52.00   92.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   19.0000  -60.0000 144

  4 omega   73.00  114.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000 -120.0000 41

  5 omega   41.00  111.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000  150.0000 70

  6 omega   53.00   81.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000 -150.0000 28

  7 omega   40.00   80.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000   90.0000 40

  8 omega  -38.00    1.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -57.0000  120.0000 39

  9 omega   15.00   41.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -57.0000  120.0000 26

 10 omega   15.00   68.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  -99.0000 -120.0000 53

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.021051
_diffrn_orient_matrix_UB_12      -0.014799
_diffrn_orient_matrix_UB_13      0.0237445
_diffrn_orient_matrix_UB_21      0.0234671
_diffrn_orient_matrix_UB_22      -0.0056583
_diffrn_orient_matrix_UB_23      0.0254383
_diffrn_orient_matrix_UB_31      -0.0024798
_diffrn_orient_matrix_UB_32      0.0731818
_diffrn_orient_matrix_UB_33      0.0067462
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Mo) X-ray micro-source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31975
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         1.82
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.385
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1202
_exptl_crystal_size_min          0.0405
_refine_diff_density_max         0.832
_refine_diff_density_min         -2.569
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+5.2151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                7707
_reflns_number_total             8825
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00838_si_006.cif
_cod_data_source_block           a2014020_at227
_cod_database_code               4088092