Iridium Cyclometalated Complexes with Axial Symmetry. Synthesis and Photophysical Properties of a trans-Biscyclometalated Complex Containing the Terdentate Ligand 2,6-Diphenylpyridine
Matthew Polson; Sandro Fracasso; Valerio Bertolasi; Marcella Ravaglia; Franco Scandola; Inorganic Chemistry 43 (2004) 1950–1956; doi:10.1021/ic0351848

data_4310730
_publ_section_title
;
 Iridium Cyclometalated Complexes with Axial Symmetry. Synthesis and
 Photophysical Properties of a trans-Biscyclometalated Complex Containing
 the Terdentate Ligand 2,6-Diphenylpyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1950
_journal_page_last               1956
_journal_paper_doi               10.1021/ic0351848
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '(C45 H31 Br Ir N4)+, (N O3)-,2(H2 O) '
_chemical_formula_sum            'C45 H35 Br Ir N5 O5'
_chemical_formula_weight         997.89
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.496(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4308(4)
_cell_length_b                   9.0312(2)
_cell_length_c                   26.7601(7)
_cell_measurement_reflns_used    36873
_cell_measurement_temperature    295
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4.13
_cell_volume                     4078.50(17)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36873
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    4.306
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         7964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+13.8881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                6044
_reflns_number_total             7964
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0351848si20031014_062942.cif
_cod_data_source_block           ir
_cod_original_cell_volume        4078.5(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4310730