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_4120357
_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
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 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            'C105 H102 B2 F30 Ir2 N4 O5'
_chemical_formula_weight         2475.93
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.0605(14)
_cell_length_b                   38.2428(12)
_cell_length_c                   10.7300(4)
_cell_measurement_reflns_used    14866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.3090
_cell_measurement_theta_min      3.6880
_cell_volume                     10283.5(8)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_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 0.994
_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  0.0896
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            116497
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.21
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    5.895
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       needle
_exptl_crystal_F_000             4936
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
 Five badly resolved regions of residual electron density at different
 positions were tentatively identified as more or less disordered acetone
 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 formular weight correspond to
 20 acetone molecules per cell.
;
_refine_diff_density_max         5.050
_refine_diff_density_min         -2.317
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         18619
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0567P)^2^+38.4061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                16751
_reflns_number_total             18619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406529c_si_002_12.cif
_cod_data_source_block           evg20
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4120357