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_4113819
_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            'C30 H18 F9 Ir N6'
_chemical_formula_weight         825.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   17.5088(13)
_cell_length_b                   17.0833(12)
_cell_length_c                   40.472(3)
_cell_measurement_reflns_used    8739
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.25
_cell_volume                     12105.5(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            59022
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    4.499
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_meas      0
_exptl_crystal_description       cube
_exptl_crystal_F_000             6368
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.000000(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         10321
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          3.419
_refine_ls_shift/su_mean         0.051
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+71.8154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                7384
_reflns_number_total             10321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034537zsi20030403_065644.cif
_cod_data_source_block           irarnm
_cod_original_cell_volume        12105.4(15)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4113819