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_4088091
_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 H34 Ir N8, F6 P'
_chemical_formula_sum            'C44 H34 F6 Ir N8 P'
_chemical_formula_weight         1011.96
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-05T11:20:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.1940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1660(2)
_cell_length_b                   21.8245(2)
_cell_length_c                   20.9858(4)
_cell_measurement_reflns_used    11588
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3192
_cell_measurement_theta_min      1.7602
_cell_measurement_wavelength     0.71073
_cell_volume                     7849.89(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(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 -117.00  -48.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3079  178.0000  150.0000 69

  2 omega -111.00    9.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3079    0.0000   30.0000 120

  3 omega   56.00  112.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8548  178.0000 -180.0000 56

  4 omega  -89.00   -4.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3079  -57.0000  -30.0000 85

  5 omega   13.00   97.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8548   57.0000 -180.0000 84

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0031816
_diffrn_orient_matrix_UB_12      0.0207079
_diffrn_orient_matrix_UB_13      -0.0257689
_diffrn_orient_matrix_UB_21      -0.0048978
_diffrn_orient_matrix_UB_22      -0.0246279
_diffrn_orient_matrix_UB_23      -0.0219451
_diffrn_orient_matrix_UB_31      -0.0409418
_diffrn_orient_matrix_UB_32      0.0045994
_diffrn_orient_matrix_UB_33      -0.0013237
_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  0.0226
_diffrn_reflns_av_unetI/netI     0.026
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24093
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         1.76
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.516
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.494
_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    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.3477
_exptl_crystal_size_mid          0.1477
_exptl_crystal_size_min          0.0492
_refine_diff_density_max         1.579
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8143
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+44.2780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                7144
_reflns_number_total             8143
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00838_si_003.cif
_cod_data_source_block           at050
_cod_database_code               4088091