Iridium(I) Complexes with Anionic N-Heterocyclic Carbene Ligands as Catalysts for the Hydrogenation of Alkenes in Nonpolar Media
Eugene L. Kolychev; Sabrina Kronig; Kai Brandhorst; Matthias Freytag; Peter G. Jones; Matthias Tamm; Journal of the American Chemical Society 135 (2013) 12448–12459; doi:10.1021/ja406529c

data_4120351
_publ_contact_author
;
        Peter G. Jones (for X-ray details)
        Institut f\"ur Anorganische und Analytische Chemie
        Technische Universit\"at Braunschweig
        Postfach 3329
        38023 Braunschweig
        Germany
;
_publ_contact_author_email       p.jones@tu-bs.de
_publ_contact_author_fax         '049 531 391-5387'
_publ_contact_author_phone       '049 531 391-5382'
_publ_section_title
;
 Iridium(I) Complexes with Anionic N-Heterocyclic Carbene Ligands as
 Catalysts for the Hydrogenation of Alkenes in Nonpolar Media
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12448
_journal_page_last               12459
_journal_paper_doi               10.1021/ja406529c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C55 H51 B F15 Li N2 O4'
_chemical_formula_weight         1106.73
_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                82.280(4)
_cell_angle_beta                 84.241(4)
_cell_angle_gamma                84.873(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6075(6)
_cell_length_b                   12.9170(6)
_cell_length_c                   15.9241(8)
_cell_measurement_reflns_used    45500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.7560
_cell_measurement_theta_min      3.4603
_cell_volume                     2549.2(2)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) x-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72219
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         75.94
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
 A badly resolved region of electron density around the inversion centre
 -0.5 0 0.5 was tentatively identified as a disordered THF molecule but
 could not be refined satisfactorily. For this reason the program SQUEEZE
 (part of the PLATON suite; A. Spek, University of Utrecht, Netherlands,
 2009) was used to remove mathematically the effects of the solvent. Derived
 parameters such as the formular weight correspond tho two THF molecules
 per cell.
;
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         10565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.8966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                9853
_reflns_number_total             10565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406529c_si_002_06.cif
_cod_data_source_block           evg15
_cod_database_code               4120351