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_4324844
_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         'C58 H68 F2 Ir N5 O4,C H2 Cl2'
_chemical_formula_sum            'C59 H70 Cl2 F2 Ir N5 O4'
_chemical_formula_weight         1214.30
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.720(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.483(2)
_cell_length_b                   15.1691(11)
_cell_length_c                   27.432(2)
_cell_measurement_reflns_used    5767
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.41
_cell_volume                     11700.3(19)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART version 5.049 (Bruker, 1998)'
_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 8.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART CCD 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.012462
_diffrn_orient_matrix_UB_12      -0.057869
_diffrn_orient_matrix_UB_13      0.006279
_diffrn_orient_matrix_UB_21      0.011898
_diffrn_orient_matrix_UB_22      0.0132
_diffrn_orient_matrix_UB_23      0.038561
_diffrn_orient_matrix_UB_31      -0.031003
_diffrn_orient_matrix_UB_32      0.028168
_diffrn_orient_matrix_UB_33      -0.005131
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41258
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.428
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2006/1 (Bruker,2006) was used for absorption correction.
 R(int) was 0.0872 before and 0.0510 after correction. The Ratio of minimum 
 to maximum transmission is 0.5654. The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.474
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         10305
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+6.7972P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1326
_reflns_number_gt                7347
_reflns_number_total             10305
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic102153x_si_002_1.cif
_cod_data_source_block           18
_cod_original_cell_volume        11700.4(19)
_cod_database_code               4324844