Diastereoselective Formation of Chiral Tris-Cyclometalated Iridium (III) Complexes: Characterization and Photophysical Properties
Christine Schaffner-Hamann; Alexander von Zelewsky; Andrea Barbieri; Francesco Barigelletti; Gilles Muller; James P. Riehl; Antonia Neels; Journal of the American Chemical Society 126 (2004) 9339–9348; doi:10.1021/ja048655d

data_4112805
_publ_section_title
;
 Diastereoselective Formation of Chiral Tris-Cyclometalated Iridium (III)
 Complexes: Characterization and Photophysical Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9339
_journal_page_last               9348
_journal_paper_doi               10.1021/ja048655d
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration lamda
_chemical_formula_sum            'C309 H354 Ir4 N12 O27'
_chemical_formula_weight         5436.84
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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            1
_cell_length_a                   38.6193(10)
_cell_length_b                   15.8553(4)
_cell_length_c                   11.3176(4)
_cell_measurement_reflns_used    67476
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.28
_cell_volume                     6930.0(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            68522
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.981
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (PLATON03, Speck, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       rod
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.111
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         12226
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0781P)^2^+7.0419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                11453
_reflns_number_total             12226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048655dsi20040525_104126.cif
_cod_data_source_block           e:fac-lamda-IrL
_cod_database_code               4112805