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_4088088
_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         'C34 H24 N6'
_chemical_formula_sum            'C34 H24 N6'
_chemical_formula_weight         516.59
_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             2014-11-04T12:48:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.483(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.3182(2)
_cell_length_b                   9.8009(4)
_cell_length_c                   24.1848(8)
_cell_measurement_reflns_used    2918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.276
_cell_measurement_theta_min      3.642
_cell_measurement_wavelength     1.54184
_cell_volume                     1259.40(8)
_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 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -92.00  -45.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.2006  -57.0000   60.0000 47

  2 omega  -88.00  -13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.2006  -57.0000  -30.0000 75

  3 omega    7.00   96.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.2006 -125.0000 -180.0000 89

  4 omega   73.00  115.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  125.0000    0.0000 42

  5 omega   31.00   69.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000   60.0000 38

  6 omega   43.00   68.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -60.0000 25

  7 omega   60.00  122.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000   30.0000 62

  8 omega   85.00  146.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  125.0000  -60.0000 61

  9 omega   46.00   71.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000  -30.0000 25

 10 omega   52.00  108.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  120.0000 56

 11 omega   33.00   62.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -90.0000 29

 12 omega   31.00   67.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -180.0000 36

 13 omega   31.00   63.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -150.0000 32

 14 omega   57.00   82.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -120.0000 25

 15 omega   34.00   65.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -120.0000 31

 16 omega   17.00  114.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.2006   57.0000  -60.0000 97

 17 omega   26.00   95.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.2006   38.0000 -120.0000 69

 18 omega   30.00   60.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000   90.0000 30

 19 omega   30.00   55.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -60.0000 25

 20 omega   57.00   80.00   1.0000    5.5000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -77.0000  -60.0000 23

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0176503
_diffrn_orient_matrix_UB_12      -0.057058
_diffrn_orient_matrix_UB_13      -0.0590736
_diffrn_orient_matrix_UB_21      0.0473152
_diffrn_orient_matrix_UB_22      -0.1439118
_diffrn_orient_matrix_UB_23      0.0238945
_diffrn_orient_matrix_UB_31      -0.2854228
_diffrn_orient_matrix_UB_32      -0.0273328
_diffrn_orient_matrix_UB_33      -0.0024934
_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  0.0192
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5801
_diffrn_reflns_theta_full        67.5
_diffrn_reflns_theta_max         67.5
_diffrn_reflns_theta_min         3.66
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.87
_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    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.3914
_exptl_crystal_size_mid          0.2119
_exptl_crystal_size_min          0.0574
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.7099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                1992
_reflns_number_total             2276
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00838_si_007.cif
_cod_data_source_block           tp090
_cod_database_code               4088088