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_4112505
_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 H38 F6 N4 P Rh'
_chemical_formula_weight         606.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 128.6360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5823(8)
_cell_length_b                   21.0284(10)
_cell_length_c                   10.3295(5)
_cell_measurement_reflns_used    43862
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.551
_cell_measurement_theta_min      3.284
_cell_volume                     2643.9(2)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36373
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.969921
_exptl_absorpt_correction_T_min  0.863648
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8052
_refine_ls_number_restraints     1815
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          2.262
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+2.1612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0547
_reflns_number_gt                7477
_reflns_number_total             8052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0495452Bsi20040126_120714.cif
_cod_data_source_block           nol148
_cod_database_code               4112505