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_4088090
_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 H31 Br Ir N6, 2(F3 P0.5)'
_chemical_formula_sum            'C44 H31 Br F6 Ir N6 P'
_chemical_formula_weight         1060.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-13T12:53:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.771(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.2267(12)
_cell_length_b                   13.2492(3)
_cell_length_c                   26.6858(9)
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    99.94(17)
_cell_measurement_theta_max      21.238
_cell_measurement_theta_min      1.953
_cell_measurement_wavelength     0.71073
_cell_volume                     9650.2(6)
_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      99.94(17)
_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  -24.00   61.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -57.0000  -60.0000 85

  2 omega  -16.00   91.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   38.0000  150.0000 107

  3 omega  -37.00   51.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -38.0000 -150.0000 88

  4 omega   56.00   93.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   57.0000   30.0000 37

  5 omega   71.00  116.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767 -178.0000 -150.0000 45

  6 omega   79.00  118.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767 -178.0000   30.0000 39

  7 omega   80.00  105.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   77.0000  150.0000 25

  8 omega  -30.00   59.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -57.0000  150.0000 89

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0242294
_diffrn_orient_matrix_UB_12      0.0193927
_diffrn_orient_matrix_UB_13      0.0067385
_diffrn_orient_matrix_UB_21      -0.0066088
_diffrn_orient_matrix_UB_22      0.0341255
_diffrn_orient_matrix_UB_23      0.0175432
_diffrn_orient_matrix_UB_31      0.0067155
_diffrn_orient_matrix_UB_32      -0.0363669
_diffrn_orient_matrix_UB_33      0.0200636
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_unetI/netI     0.1323
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            38469
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.686
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.81514
_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    1.46
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.2357
_exptl_crystal_size_mid          0.0956
_exptl_crystal_size_min          0.0361
_refine_diff_density_max         2.87
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9489
_refine_ls_number_restraints     477
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.157
_refine_ls_wR_factor_ref         0.1735
_reflns_number_gt                5762
_reflns_number_total             9489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00838_si_005.cif
_cod_data_source_block           at148
_cod_database_code               4088090