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_4111508
_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            'C48 H76 F12 N8 O4 P2 Rh2'
_chemical_formula_weight         1324.93
_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                106.3800(10)
_cell_angle_beta                 102.2210(10)
_cell_angle_gamma                103.3720(10)
_cell_formula_units_Z            1
_cell_length_a                   10.2573(5)
_cell_length_b                   11.7090(6)
_cell_length_c                   13.3613(7)
_cell_measurement_reflns_used    11164
_cell_measurement_temperature    396(2)
_cell_measurement_theta_max      30.433
_cell_measurement_theta_min      2.382
_cell_volume                     1430.43(13)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9710
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.932585
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+5.3020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                2437
_reflns_number_total             2671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043249fsi20041109_040055.cif
_cod_data_source_block           nol176m
_cod_database_code               4111508