Influence of Halogen Atoms on a Homologous Series of Bis-Cyclometalated Iridium(III) Complexes
Etienne Baranoff; Basile F. E. Curchod; Filippo Monti; Frédéric Steimer; Gianluca Accorsi; Ivano Tavernelli; Ursula Rothlisberger; Rosario Scopelliti; Michael Grätzel; Md. Khaja Nazeeruddin; Inorganic Chemistry 51 (2012) 799–811; doi:10.1021/ic2011474

data_4327947
_publ_section_title
;
 Influence of Halogen Atoms on a Homologous Series of Bis-Cyclometalated
 Iridium(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              799
_journal_page_last               811
_journal_paper_doi               10.1021/ic2011474
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C28 H16 Br4 Ir N3 O2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C28.5 H17 Br4 Cl Ir N3 O2'
_chemical_formula_weight         980.74
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 90.412(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   30.6777(6)
_cell_length_b                   11.2485(2)
_cell_length_c                   35.0954(7)
_cell_measurement_reflns_used    19659
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.5028
_cell_measurement_theta_min      2.6293
_cell_volume                     12110.3(4)
_computing_cell_refinement
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
;
_computing_data_collection
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
;
_computing_data_reduction
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
;
_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      140(2)
_diffrn_detector_area_resol_mean 8.2812
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction, KM4/Sapphire CCD'
_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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            44681
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    9.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50519
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             7344
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.301
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10690
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+176.4050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                7997
_reflns_number_total             10690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2011474_si_004.cif
_cod_data_source_block           eb55
_cod_original_formula_sum        'C28.50 H17 Br4 Cl Ir N3 O2'
_cod_database_code               4327947