Interaction of a Bulky N-Heterocyclic Carbene Ligand with Rh(I) and Ir(I). Double C-H Activation and Isolation of Bare 14-Electron Rh(III) and Ir(III) Complexes
Natalie M. Scott; Reto Dorta; Edwin D. Stevens; Andrea Correa; Luigi Cavallo; Steven P. Nolan; Journal of the American Chemical Society 127 (2005) 3516–3526; doi:10.1021/ja043249f

data_4111509
_publ_section_title
;
 Interaction of a Bulky N-Heterocyclic Carbene Ligand with Rh(I) and
 Ir(I). Double C-H Activation and Isolation of Bare 14-Electron Rh(III)
 and Ir(III) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3516
_journal_page_last               3526
_journal_paper_doi               10.1021/ja043249f
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C24 H38 F6 Ir N4 O2 P'
_chemical_formula_weight         751.75
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
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_cell_angle_beta                 101.576(2)
_cell_angle_gamma                103.503(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2547(11)
_cell_length_b                   11.7363(12)
_cell_length_c                   13.3823(14)
_cell_measurement_reflns_used    10823
_cell_measurement_temperature    396(2)
_cell_measurement_theta_max      28.485
_cell_measurement_theta_min      2.295
_cell_volume                     1435.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      396(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0517
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_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
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_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    4.773
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.471895
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.5
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_refine_diff_density_max         1.077
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     353
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_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                2471
_reflns_number_total             2679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043249fsi20041109_040115.cif
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c:\docume~1\owner\mydocu~1\natsdo~1\neworl~1\natalie\irco2\nol173m
_cod_database_code               4111509