Probing the mer- to fac- Isomerization of Tris-Cyclometallated Homo- and Heteroleptic (C,N)3 Iridium(III) Complexes
Aidan R. McDonald; Martin Lutz; Lars S. von Chrzanowski; Gerard P. M. van Klink; Anthony L. Spek; Gerard van Koten; Inorganic Chemistry 47 (2008) 6681–6691; doi:10.1021/ic800169n

data_4305285
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
Probing the mer- to fac- Isomerization of Tris-Cyclometallated Homo- and
Heteroleptic (C,N)3 Iridium(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6681
_journal_page_last               6691
_journal_paper_doi               10.1021/ic800169n
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C35 H28 Ir N3'
_chemical_formula_sum            'C35 H28 Ir N3'
_chemical_formula_weight         682.80
_space_group_IT_number           167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   20.02588(1)
_cell_length_b                   20.02588(1)
_cell_length_c                   36.14264(2)
_cell_measurement_reflns_used    26096
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.63
_cell_volume                     12552.601(11)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            51277
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    4.815
_exptl_absorpt_correction_T_max  0.3658
_exptl_absorpt_correction_T_min  0.0712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.619
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0206P)^2^+42.2655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                2783
_reflns_number_total             3176
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800169n-file001_3.cif
_cod_data_source_block           s3833a
_cod_original_cell_volume        12552.593(11)
_cod_original_sg_symbol_Hall     '-R 3 2"C'
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4305285