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_4113821
_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           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                 103.030(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.5923(10)
_cell_length_b                   33.878(3)
_cell_length_c                   15.5667(14)
_cell_measurement_temperature    296(2)
_cell_volume                     5956.0(9)
_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_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30328
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    4.572
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_F_000             3184
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.000000(14)
_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   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         10165
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          3.469
_refine_ls_shift/su_mean         0.073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+34.9216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                8242
_reflns_number_total             10165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034537zsi20030403_065733.cif
_cod_data_source_block           arnlm
_cod_database_code               4113821