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_4305283
_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, C H2 Cl2'
_chemical_formula_sum            'C36 H30 Cl2 Ir N3'
_chemical_formula_weight         767.73
_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                 90.325(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9298(8)
_cell_length_b                   9.6998(5)
_cell_length_c                   20.7136(10)
_cell_measurement_reflns_used    163
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.44
_cell_measurement_theta_min      3.21
_cell_volume                     2999.6(3)
_computing_cell_refinement       Dirax
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, ABST'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70813
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    4.660
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.821
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+15.1030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                4464
_reflns_number_total             5581
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800169n-file001_1.cif
_cod_data_source_block           s3342a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4305283