"Click" Synthesis of Heteroleptic Tris-Cyclometalated Iridium(III) Complexes: Cu(I) Triazolide Intermediates as Transmetalating Reagents
Shuang Liu; Peter Müller; Michael K. Takase; Timothy M. Swager; Inorganic Chemistry 50 (2011) 7598–7609; doi:10.1021/ic2005985

data_4325875
_publ_contact_author_address
;Department of Chemisry
Massachusetts Institute of Technology
Cambridge, MA 02139
;
_publ_contact_author_email       tswager@MIT.EDU
_publ_contact_author_name        'Timothy M. Swager'
_publ_contact_author_phone       617-253-4423
_publ_section_title
;
 "Click" Synthesis of Heteroleptic Tris-Cyclometalated Iridium(III)
 Complexes: Cu(I) Triazolide Intermediates as Transmetalating Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7598
_journal_page_last               7609
_journal_paper_doi               10.1021/ic2005985
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C35 H30 F10 Ir N6 P'
_chemical_formula_weight         947.82
_chemical_name_systematic
; 
 ? 
;
_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                 92.2270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9605(2)
_cell_length_b                   14.0627(2)
_cell_length_c                   18.7948(3)
_cell_measurement_reflns_used    4433
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.23
_cell_measurement_theta_min      3.41
_cell_volume                     3422.95(9)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6186
_diffrn_reflns_theta_full        67.73
_diffrn_reflns_theta_max         67.73
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    8.819
_exptl_absorpt_correction_T_max  0.6668
_exptl_absorpt_correction_T_min  0.2715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6186
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0333P)^2^+6.1185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                5928
_reflns_number_total             6186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2005985_si_001_3.cif
_cod_data_source_block           6b_d10103_CCDC817544
_cod_database_code               4325875