Carbene Complexes of Rhodium and Iridium from Tripodal N-Heterocyclic Carbene Ligands: Synthesis and Catalytic Properties
Elena Mas-Marzá; Macarena Poyatos; Mercedes Sanaú; Eduardo Peris; Inorganic Chemistry 43 (2004) 2213–2219; doi:10.1021/ic035317p

data_4310749
_publ_section_title
;
 Carbene Complexes of Rhodium and Iridium from Tripodal N-Heterocyclic
 Carbene Ligands: Synthesis and Catalytic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2213
_journal_page_last               2219
_journal_paper_doi               10.1021/ic035317p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C34 H55 F12 N6 P2 Rh'
_chemical_formula_weight         940.69
_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                 120.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.544(7)
_cell_length_b                   10.027(2)
_cell_length_c                   28.873(6)
_cell_measurement_temperature    293(2)
_cell_volume                     8393(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.2324
_diffrn_reflns_av_sigmaI/netI    0.1915
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29035
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.569
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3872
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         15998
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1946
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.797
_refine_ls_shift/su_mean         0.189
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1776P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2248
_refine_ls_wR_factor_ref         0.3230
_reflns_number_gt                6979
_reflns_number_total             15998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035317psi20040116_055819.cif
_cod_data_source_block           compound_8-Rh
_cod_original_cell_volume        8393(3)
_cod_database_code               4310749