Double C-H Activation in a Rh-NHC Complex Leading to the Isolation of a 14-Electron Rh(III) Complex
Reto Dorta; Edwin D. Stevens; Steven P. Nolan; Journal of the American Chemical Society 126 (2004) 5054–5055; doi:10.1021/ja049545+

data_4112503
_publ_section_title
;
 Double C-H Activation in a Rh-NHC Complex Leading to the Isolation of a
 14-Electron Rh(III) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5054
_journal_page_last               5055
_journal_paper_doi               10.1021/ja049545+
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C22 H40 Cl N4 Rh'
_chemical_formula_weight         498.94
_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                65.2530(10)
_cell_angle_beta                 77.4040(10)
_cell_angle_gamma                73.0780(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4003(6)
_cell_length_b                   11.8460(8)
_cell_length_c                   12.6971(8)
_cell_measurement_reflns_used    7560
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.731
_cell_measurement_theta_min      2.479
_cell_volume                     1220.90(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9787
_diffrn_reflns_theta_full        29.73
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.862192
_exptl_absorpt_correction_T_min  0.660362
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.057
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0039(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                5304
_reflns_number_total             6179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0495452Bsi20040126_120630.cif
_cod_data_source_block           nol119m
_cod_database_code               4112503