Frustrated N-heterocyclic carbene-silylium ion Lewis pairs.
Silva Valverde, Miguel F.; Theuergarten, Eileen; Bannenberg, Thomas; Freytag, Matthias; Jones, Peter G.; Tamm, Matthias; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9400–9408; doi:10.1039/c5dt01362c

data_7034867
_publ_section_title
;
 Frustrated N-heterocyclic carbene-silylium ion Lewis pairs.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9400
_journal_page_last               9408
_journal_paper_doi               10.1039/c5dt01362c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C35.5 H43 Au F3 N2 O3 P S'
_chemical_formula_weight         862.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.201(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2711(5)
_cell_length_b                   16.7779(8)
_cell_length_c                   22.7298(10)
_cell_measurement_reflns_used    8282
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.4730
_cell_measurement_theta_min      2.4240
_cell_volume                     3514.9(3)
_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 16.1419
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            93410
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.90
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91745
_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            colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
A badly resolved rigion of residual electron density around the inversion 
centre 0.5, 0.5, 0.5 was tentatively identified as half a disordered 
molecule of toluene but could not be refined satisfactorily. For this 
reason the program SQEEZE (part of the PLATON suite, A. Spek, University 
of Utrecht, Metherlands, 2009) was used to remove mathematically the 
effects of the solvent. Derived parameters such as the formular weight 
correspond two molecules of toluene per cell.
;
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         10522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0191P)^2^+0.3978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                8019
_reflns_number_total             10522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01362c3.cif
_cod_data_source_block           eileen62
_cod_depositor_comments
'Adding full bibliography for 7034861--7034869.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C35.50 H43 Au F3 N2 O3 P S'
_cod_database_code               7034867
_refine_instructions_details
;
CELL 0.71073   9.271150  16.777888  22.729799  90.0000  96.2013  90.0000
ZERR    4.00   0.000500   0.000800   0.001000   0.0000   0.0040   0.0000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    F    P    S    AU
UNIT  142  172  8  12  12  4  4  4
MERG   2
FMAP   2
 
ACTA 60
CONF
 
OMIT -1 2 8
 
TEMP -173
 
PLAN   10
L.S.   4
WGHT    0.019100    0.397800
FVAR      19.60560
AU    8    0.917743    0.521774    0.810612    11.00000    0.01251    0.01453 =
         0.01166    0.00116    0.00114    0.00161
P     6    0.851717    0.609728    0.736221    11.00000    0.01227    0.01444 =
         0.01057    0.00107    0.00220    0.00033
N1    3    0.881067    0.428069    0.923212    11.00000    0.01336    0.01891 =
         0.01623   -0.00144    0.00178    0.00105
N2    3    1.066681    0.383267    0.882272    11.00000    0.01093    0.01466 =
         0.01512    0.00159    0.00256    0.00069
C1    1    0.964533    0.441864    0.878996    11.00000    0.01293    0.01628 =
         0.00678   -0.00138    0.00024   -0.00273
C2    1    0.924629    0.356674    0.951356    11.00000    0.02043    0.02413 =
         0.02567    0.00934    0.00438    0.00205
C3    1    1.041272    0.329793    0.926792    11.00000    0.01766    0.01685 =
         0.02203    0.00657    0.00175   -0.00002
C4    1    0.760549    0.484318    0.938159    11.00000    0.01651    0.02519 =
         0.01722   -0.00329    0.00567    0.00262
C5    1    0.807477    0.570626    0.931680    11.00000    0.05607    0.02968 =
         0.03443    0.00400    0.02376    0.01798
AFIX 137
H5A   2    0.735110    0.606182    0.946069    11.00000   -1.50000
H5B   2    0.815927    0.582067    0.889911    11.00000   -1.50000
H5C   2    0.901575    0.579138    0.954892    11.00000   -1.50000
AFIX   0
C6    1    0.625641    0.465749    0.896886    11.00000    0.01711    0.08281 =
         0.05608   -0.03185   -0.00593    0.01288
AFIX 137
H6A   2    0.595211    0.410783    0.903321    11.00000   -1.50000
H6B   2    0.646578    0.472032    0.855792    11.00000   -1.50000
H6C   2    0.547731    0.502403    0.904803    11.00000   -1.50000
AFIX   0
C7    1    0.731256    0.476335    1.002800    11.00000    0.04656    0.03728 =
         0.02539    0.00479    0.02079    0.00659
AFIX 137
H7A   2    0.683794    0.425151    1.008524    11.00000   -1.50000
H7B   2    0.667953    0.519885    1.012918    11.00000   -1.50000
H7C   2    0.823241    0.478851    1.028398    11.00000   -1.50000
AFIX   0
C8    1    0.846228    0.314078    0.997118    11.00000    0.04581    0.03895 =
         0.06230    0.02809    0.03213    0.01119
AFIX 137
H8A   2    0.878415    0.258451    1.000152    11.00000   -1.50000
H8B   2    0.741443    0.315841    0.985303    11.00000   -1.50000
H8C   2    0.867992    0.340322    1.035571    11.00000   -1.50000
AFIX   0
C9    1    1.126305    0.256934    0.946211    11.00000    0.03645    0.02051 =
         0.04137    0.01451    0.01570    0.00704
AFIX 137
H9A   2    1.082206    0.231129    0.978565    11.00000   -1.50000
H9B   2    1.226417    0.272051    0.959919    11.00000   -1.50000
H9C   2    1.126028    0.219868    0.912878    11.00000   -1.50000
AFIX   0
C10   1    1.177466    0.377377    0.837669    11.00000    0.01326    0.01648 =
         0.01594    0.00038    0.00342    0.00378
C11   1    1.244567    0.458635    0.827983    11.00000    0.01418    0.02389 =
         0.02447    0.00397    0.00749    0.00014
AFIX 137
H11A  2    1.171756    0.493362    0.806605    11.00000   -1.50000
H11B  2    1.326926    0.452212    0.804758    11.00000   -1.50000
H11C  2    1.278158    0.482569    0.866358    11.00000   -1.50000
AFIX   0
C12   1    1.100149    0.343452    0.780444    11.00000    0.02443    0.02872 =
         0.02415   -0.00900    0.00499    0.00574
AFIX 137
H12A  2    1.064060    0.289879    0.787852    11.00000   -1.50000
H12B  2    1.168242    0.340649    0.750395    11.00000   -1.50000
H12C  2    1.018486    0.378040    0.766331    11.00000   -1.50000
AFIX   0
C13   1    1.303894    0.322377    0.859717    11.00000    0.01888    0.03020 =
         0.03498    0.00821    0.00731    0.00707
AFIX 137
H13A  2    1.342474    0.337964    0.899911    11.00000   -1.50000
H13B  2    1.380514    0.326849    0.833383    11.00000   -1.50000
H13C  2    1.269522    0.267154    0.859954    11.00000   -1.50000
AFIX   0
C14   1    0.656549    0.607882    0.716005    11.00000    0.01295    0.01058 =
         0.01341    0.00100   -0.00249    0.00228
C15   1    0.596217    0.588695    0.659175    11.00000    0.01490    0.02240 =
         0.01496   -0.00165    0.00444    0.00311
AFIX  43
H15   2    0.656984    0.579455    0.628790    11.00000   -1.20000
AFIX   0
C16   1    0.447156    0.583124    0.647097    11.00000    0.01938    0.02402 =
         0.01714   -0.00362   -0.00499    0.00319
AFIX  43
H16   2    0.405768    0.569278    0.608385    11.00000   -1.20000
AFIX   0
C17   1    0.358021    0.597486    0.690738    11.00000    0.01224    0.01937 =
         0.02589   -0.00257   -0.00280   -0.00166
AFIX  43
H17   2    0.255717    0.593869    0.681896    11.00000   -1.20000
AFIX   0
C18   1    0.417128    0.617115    0.747263    11.00000    0.01343    0.01990 =
         0.02186    0.00221    0.00771    0.00069
AFIX  43
H18   2    0.355420    0.627621    0.777111    11.00000   -1.20000
AFIX   0
C19   1    0.565819    0.621482    0.760431    11.00000    0.01470    0.01818 =
         0.01485   -0.00048    0.00287    0.00040
AFIX  43
H19   2    0.606539    0.633688    0.799548    11.00000   -1.20000
AFIX   0
C20   1    0.898642    0.711087    0.758119    11.00000    0.01758    0.01528 =
         0.00977   -0.00175    0.00314   -0.00356
C21   1    0.814861    0.776070    0.738346    11.00000    0.01871    0.02014 =
         0.01790   -0.00333    0.00648   -0.00011
AFIX  43
H21   2    0.727551    0.767981    0.713104    11.00000   -1.20000
AFIX   0
C22   1    0.856995    0.852577    0.754968    11.00000    0.02722    0.01783 =
         0.02808    0.00005    0.00977    0.00157
AFIX  43
H22   2    0.798909    0.896678    0.740902    11.00000   -1.20000
AFIX   0
C23   1    0.983179    0.865144    0.791935    11.00000    0.03550    0.02142 =
         0.03125   -0.00741    0.01098   -0.00782
AFIX  43
H23   2    1.011886    0.917746    0.803387    11.00000   -1.20000
AFIX   0
C24   1    1.067905    0.800522    0.812289    11.00000    0.02057    0.03169 =
         0.02698   -0.00732    0.00160   -0.00917
AFIX  43
H24   2    1.155154    0.808931    0.837503    11.00000   -1.20000
AFIX   0
C25   1    1.025671    0.724284    0.795987    11.00000    0.01772    0.02401 =
         0.01469   -0.00046    0.00264    0.00030
AFIX  43
H25   2    1.083269    0.680257    0.810575    11.00000   -1.20000
AFIX   0
C26   1    0.933615    0.592606    0.668273    11.00000    0.01389    0.01305 =
         0.01095    0.00170    0.00251   -0.00292
C27   1    0.948975    0.654612    0.628581    11.00000    0.02279    0.01871 =
         0.01384    0.00046    0.00442   -0.00267
AFIX  43
H27   2    0.916228    0.706666    0.636840    11.00000   -1.20000
AFIX   0
C28   1    1.011890    0.640211    0.577233    11.00000    0.02896    0.03300 =
         0.01629    0.00212    0.00353   -0.00961
AFIX  43
H28   2    1.021906    0.682494    0.550174    11.00000   -1.20000
AFIX   0
C29   1    1.060071    0.565246    0.564996    11.00000    0.02073    0.03308 =
         0.01530   -0.00742    0.00657   -0.01137
AFIX  43
H29   2    1.103984    0.556201    0.529713    11.00000   -1.20000
AFIX   0
C30   1    1.045191    0.502703    0.603659    11.00000    0.01838    0.02458 =
         0.02357   -0.00731    0.00704   -0.00240
AFIX  43
H30   2    1.078162    0.450825    0.595027    11.00000   -1.20000
AFIX   0
C31   1    0.981327    0.516880    0.655288    11.00000    0.01612    0.01569 =
         0.01599   -0.00029    0.00361   -0.00249
AFIX  43
H31   2    0.970254    0.474260    0.681947    11.00000   -1.20000
AFIX   0
S     7    0.464640    0.727318    0.923864    11.00000    0.02289    0.02421 =
         0.01574   -0.00037    0.00686    0.00186
O1    4    0.528277    0.700034    0.981064    11.00000    0.03185    0.02723 =
         0.01915    0.00512    0.00416    0.00196
O2    4    0.432158    0.665685    0.881115    11.00000    0.05611    0.04431 =
         0.02539   -0.01360    0.01283   -0.02283
O3    4    0.356493    0.788686    0.925743    11.00000    0.02831    0.04835 =
         0.03931    0.01572    0.01537    0.01745
C32   1    0.612365    0.782551    0.895761    11.00000    0.02462    0.02091 =
         0.02339    0.00368    0.00600    0.00369
F1    5    0.727608    0.737609    0.889114    11.00000    0.02936    0.03156 =
         0.05114    0.01244    0.02239    0.00937
F2    5    0.656914    0.841750    0.932641    11.00000    0.04994    0.02526 =
         0.04352   -0.00330    0.00210   -0.00967
F3    5    0.569791    0.815741    0.843336    11.00000    0.04307    0.04249 =
         0.02785    0.01931    0.01101    0.00673
 
HKLF    4
;