Highly Efficient, Selective, and General Method for the Preparation of Meridional Homo- and Heteroleptic Tris-cyclometalated Iridium Complexes
Huo, Shouquan; Deaton, Joseph C.; Rajeswaran, Manju; Lenhart, William C.; Inorganic Chemistry 45 (2006) 3155–3157; doi:10.1021/ic060089v

data_4332183
_publ_contact_author
;
        Manju Rajeswaran
        Eastman Kodak Company
        Research & Development 
        Rochester, NY 14650-2106
        USA        
;
_publ_section_title
;
 Highly Efficient, Selective, and General Method for the Preparation of
 Meridional Homo- and Heteroleptic Tris-cyclometalated Iridium Complexes
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3155
_journal_page_last               3157
_journal_paper_doi               10.1021/ic060089v
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C42 H30 Cl Ir N3'
_chemical_formula_weight         804.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.8010(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7950(13)
_cell_length_b                   23.1360(6)
_cell_length_c                   10.5570(5)
_cell_measurement_reflns_used    52452
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      1.00
_cell_volume                     3509.3(4)
_computing_cell_refinement
;
 HKL Scalepack (Otwinowski & Minor 1997)
;
_computing_data_collection       'Collect (Nonius BV, 2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0825
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15259
_diffrn_reflns_theta_full        21.25
_diffrn_reflns_theta_max         21.25
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    3.914
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.918
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         3865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+28.6057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                3175
_reflns_number_total             3865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060089vsup1.cif
_cod_data_source_block           merIrpiq2ppy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332183