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_4120356
_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            'C63 H55 B F15 Ir N2'
_chemical_formula_weight         1328.10
_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                88.192(3)
_cell_angle_beta                 81.336(3)
_cell_angle_gamma                78.973(3)
_cell_formula_units_Z            4
_cell_length_a                   10.7273(3)
_cell_length_b                   21.9190(5)
_cell_length_c                   25.9304(6)
_cell_measurement_reflns_used    120693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.9940
_cell_measurement_theta_min      3.4454
_cell_volume                     5916.2(3)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) 
(compiled Oct 27 2011,15:02:11) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) 
(compiled Oct 27 2011,15:02:11) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) 
(compiled Oct 27 2011,15:02:11) 
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            206840
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.19
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    5.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) 
(compiled Oct 27 2011,15:02:11) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
 Four badly resolved regions of residual electron density were tentativly
 identified as as disordered benzene molecules 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 formula weight correspond to four molecules of benzene.
;
_refine_diff_density_max         1.978
_refine_diff_density_min         -2.281
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         24579
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+11.8416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                23389
_reflns_number_total             24579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406529c_si_002_11.cif
_cod_data_source_block           evg6
_cod_database_code               4120356