C‒H Oxidative Addition of Bisimidazolium Salts to Iridium and Rhodium Complexes, and N-Heterocyclic Carbene Generation. A Combined Experimental and Theoretical Study
Viciano, Mónica; Poyatos, Macarena; Sanaú, Mercedes; Peris, Eduardo; Rossin, Andrea; Ujaque, Gregori; Lledós, Agustí; Organometallics 25 (2006) 1120–1134; doi:10.1021/om051004l

data_4074919
_publ_section_title
;
 C--H Oxidative Addition of Bisimidazolium Salts to Iridium and
 Rhodium Complexes, and N-Heterocyclic Carbene Generation. A Combined
 Experimental and Theoretical Study
;
_journal_coden_ASTM              ORGND7
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1120
_journal_page_last               1134
_journal_paper_doi               10.1021/om051004l
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C25 H37 F6 Ir N4 P'
_chemical_formula_weight         730.76
_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                76.296(3)
_cell_angle_beta                 80.230(4)
_cell_angle_gamma                70.657(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7176(13)
_cell_length_b                   11.7660(18)
_cell_length_c                   17.981(3)
_cell_measurement_reflns_used    3356
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.80
_cell_measurement_theta_min      2.34
_cell_volume                     1682.3(5)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.1203
_diffrn_reflns_av_sigmaI/netI    0.1731
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13942
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    4.067
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             722
_refine_diff_density_max         1.806
_refine_diff_density_min         -2.277
_refine_diff_density_rms         0.262
_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     334
_refine_ls_number_reflns         9753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1728
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2300
_reflns_number_gt                4598
_reflns_number_total             9753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051004lsi20051122_052212.cif
_cod_data_source_block           p-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1682.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074919