Unusual Dinuclear and Mononuclear Cyclometalated Iridium Complexes of 2,5-Diaryl-1,3,4-oxadiazole Derivatives
Yonghao Zheng; Andrei S. Batsanov; Martin R. Bryce; Inorganic Chemistry 50 (2011) 3354–3362; doi:10.1021/ic102153x

data_4324846
_publ_contact_author             'Andrei S.Batsanov'
_publ_contact_author_email       a.s.batsanov@durham.ac.uk
_publ_section_title
;
 Unusual Dinuclear and Mononuclear Cyclometalated Iridium Complexes of
 2,5-Diaryl-1,3,4-oxadiazole Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3354
_journal_page_last               3362
_journal_paper_doi               10.1021/ic102153x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C92 H104 Cl2 F4 Ir2 N8 O4,2(C H2 Cl2)'
_chemical_formula_sum            'C94 H108 Cl6 F4 Ir2 N8 O4'
_chemical_formula_weight         2086.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.029(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2350(5)
_cell_length_b                   15.2472(5)
_cell_length_c                   21.7641(8)
_cell_measurement_reflns_used    8235
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.949
_cell_measurement_theta_min      2.297
_cell_volume                     4651.6(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
A short history of SHELX (Sheldrick, 2008)/Bruker
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART CCD 6000'
_diffrn_measurement_method       '\W scans'
_diffrn_orient_matrix_UB_11      -0.053633
_diffrn_orient_matrix_UB_12      -0.041981
_diffrn_orient_matrix_UB_13      -0.013342
_diffrn_orient_matrix_UB_21      0.007164
_diffrn_orient_matrix_UB_22      0.008175
_diffrn_orient_matrix_UB_23      -0.044532
_diffrn_orient_matrix_UB_31      0.046469
_diffrn_orient_matrix_UB_32      -0.049723
_diffrn_orient_matrix_UB_33      0.003938
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            97915
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         1.59
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.092
_exptl_absorpt_correction_T_max  0.6764
_exptl_absorpt_correction_T_min  0.3287
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
"'XPREP 6.14 (Bruker, 2003), R(int)=0.101 before correction"
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       tabular
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.808
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         16837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+8.7864P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                13995
_reflns_number_total             16837
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic102153x_si_002_3.cif
_cod_data_source_block           13
_cod_database_code               4324846