Cyclometalated Iridium Complexes of Bis(Aryl) Phosphine Ligands: Catalytic C-H/C-D Exchanges and C-C Coupling Reactions
Jesús Campos; María F. Espada; Joaquín López-Serrano; Ernesto Carmona; Inorganic Chemistry 52 (2013) 6694–6704; doi:10.1021/ic400759r

data_4335123
_publ_section_title
;
 Cyclometalated Iridium Complexes of Bis(Aryl) Phosphine Ligands:
 Catalytic C-H/C-D Exchanges and C-C Coupling Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6694
_journal_page_last               6704
_journal_paper_doi               10.1021/ic400759r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C32 H12 B F24, C29 H37 Ir O P'
_chemical_formula_sum            'C61 H49 B F24 Ir O P'
_chemical_formula_weight         1487.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.912(5)
_cell_angle_beta                 81.439(5)
_cell_angle_gamma                84.605(5)
_cell_formula_units_Z            2
_cell_length_a                   12.228(5)
_cell_length_b                   12.879(5)
_cell_length_c                   19.160(5)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      2.54
_cell_volume                     2962.0(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18540
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    2.398
_exptl_absorpt_correction_T_max  0.7618
_exptl_absorpt_correction_T_min  0.3802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 APEX2 Software Suite; Bruker 2005.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.233
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         10140
_refine_ls_number_restraints     580
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+30.7492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                9007
_reflns_number_total             10140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400759r_si_002.cif
_cod_data_source_block           mo_mfe0313b_0m
_cod_database_code               4335123