Synthesis and Characterization of Facial and Meridional Tris-cyclometalated Iridium(III) Complexes
Arnold B. Tamayo; Bert D. Alleyne; Peter I. Djurovich; Sergey Lamansky; Irina Tsyba; Nam N. Ho; Robert Bau; Mark E. Thompson; Journal of the American Chemical Society 125 (2003) 7377–7387; doi:10.1021/ja034537z

data_4113823
_publ_section_title
;
 Synthesis and Characterization of Facial and Meridional
 Tris-cyclometalated Iridium(III) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7377
_journal_page_last               7387
_journal_paper_doi               10.1021/ja034537z
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C37 H32 Cl2 Ir N3'
_chemical_formula_weight         781.76
_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                 91.383(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.113(2)
_cell_length_b                   9.9696(15)
_cell_length_c                   21.093(3)
_cell_measurement_temperature    223(2)
_cell_volume                     3177.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24547
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    4.401
_exptl_absorpt_correction_T_max  0.5581
_exptl_absorpt_correction_T_min  0.4058
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         5422
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+18.5285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                4312
_reflns_number_total             5422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034537zsi20030403_065817.cif
_cod_data_source_block           mt11s
_cod_database_code               4113823