Acta Crystallographica Section E Structure Reports
Online
ISSN 1600-5368
Diaquadihydroxohexakis(tri-tert-butoxysilane-thiolato)octalithium(I)±toluene (1/2)
Katarzyna Baranowska,a Jaroslaw Chojnacki,a* Wieslaw Wojnowskiaand Ingo Krossingb
aDepartment of Chemistry Technical University
of GdanÂsk 11/12, G. Narutowicz St., 80952-PL GdanÂsk, Poland, andbInstitut fuÈr Anorganische
Chemie der UniversitaÈt Karlsruhe TH, Engesserstraûe Geb. 30.45, D-76128 Karlsruhe, Germany
Correspondence e-mail: jarekch@chem.pg.gda.pl
Key indicators Single-crystal X-ray study
T= 200 K
Mean(C±C) = 0.003 AÊ Disorder in solvent or counterion
Rfactor = 0.036
wRfactor = 0.105
Data-to-parameter ratio = 17.5
For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
The title compound, [Li8(C12H27O3SSi)6(OH)2(H2O)2]2C7H8,
has been obtained by reaction of (tBuO)
3SiSH with metallic
lithium. The molecule is located on a centre of inversion. The asymmetric unit contains only half a molecule and one disordered toluene molecule.
Comment
Structural studies on thiolates, selenolates and tellurolates of
thes-block elements have recently been reviewed (Englich &
Ruhlandt-Senge, 2000). The number of lithium thiolates cited is about 40 and none of them contain an LiÐSÐSi fragment. We have attempted to introduce a new type of thiolate ligand, (tBuO)
3SiSÿ, which, as well as a coordinating S atom, shows
chelating properties using O atom(s) (Beckeret al., 1996). The
title compound, (I), was obtained according to the procedure
described in the Experimental section. The
diaquadihy-droxohexakis(tri-tert-butoxysilanethiolato)octalithium(I) core
is shown in Fig. 1. The molecule is centrosymmetric. Formally it can be regarded as an adduct of lithium thiolate and lithium hydroxide hydrate. Some similarities to the structure of
LiOHH2O (OjamaÈe et al., 1994; Hermansson & Thomas,
1982) may be found. Possible sources of H2O could have been
an oxide layer on the metal or traces of water in solvents.
Six Li atoms form two edge-sharing rectangles, to which two additional Li atoms are attached terminally. Hydroxyl O atoms lie in positions bridging four Li atoms. Water molecules
are bonded to Li atoms as 2 ligands. The two-coordinate
atom S1 is in a terminal position, while all the other S atoms
are four-coordinate and act as3ligands. Eight of the 18tert
-butoxy O atoms complete the coordination spheres of the Li atoms. Two disordered [s.o.f. 0.639 (7)/0.361 (7)] toluene molecules are associated with each complex molecule. A
disorder model was used for onetert-butyl group placed on
atom O3. The molecule is a rare example of a lithium thiolate
with Li Li short contacts of ca 2.5 AÊ, although similar
Received 9 September 2002 Accepted 18 September 2002 Online 27 September 2002
Experimental
The work was carried out using standard vacuum±nitrogen line and Schlenk techniques. The title compound was synthesized by direct reaction of a diethyl ether solution of (tBuO)
3SiSH (Piekos &
Wojnowski, 1962) (2 mmol) with lithium powder. The mixture was stirred magnetically for 2 d. The excess of metal was separated by twofold ®ltration and the solvent evaporated to dryness. Recrys-tallization from toluene afforded colourless crystals suitable for X-ray diffraction analysis.
Crystal data
[Li8(C12H27O3SSi)6(OH)2(H2O)2]
-2C7H8
Mr= 1986.7 Monoclinic,P21=n
a= 13.088 (3) AÊ b= 27.188 (5) AÊ c= 17.525 (4) AÊ
= 102.25 (3) V= 6094 (2) AÊ3
Z= 2
Dx= 1.083 Mg mÿ3 MoKradiation Cell parameters from 8000
re¯ections
= 4.1±26.1
= 0.23 mmÿ1
T= 200 (2) K Thick plate, colourless 0.60.30.2 mm
Data collection Stoe IPDS diffractometer
'scansi.e.u xetc
47490 measured re¯ections 11732 independent re¯ections 10031 re¯ections withI> 2(I)
Rint= 0.035
max= 25.9
h=ÿ16!16 k=ÿ33!33 l=ÿ21!21
Re®nement Re®nement onF2
R[F2> 2(F2)] = 0.036
wR(F2) = 0.105
S= 1.04 11732 re¯ections 669 parameters
H-atom parameters constrained
w= 1/[2(F
o2) + (0.0696P)2 + 0.8026P]
whereP= (Fo2+ 2Fc2)/3 (/)max= 0.03
max= 0.32 e AÊÿ3
min=ÿ0.24 e AÊÿ3
Table 1
Selected geometric parameters (AÊ,).
Li1ÐS1 2.449 (3)
Li1ÐS3 2.514 (3)
Li1ÐS2 2.541 (3)
Li1 Li3 3.070 (4)
S1ÐSi1 2.0546 (6)
Li2ÐO11 1.912 (3)
Li2ÐO10i 1.971 (3)
Li2ÐS2 2.579 (2)
Li2 Li4i 2.581 (3)
Li2 Li3 2.673 (3)
S2ÐSi2 2.0649 (7)
S2ÐLi3 2.433 (2)
Li3ÐO11 1.926 (2)
Li3ÐS3 2.647 (2)
Li3 Li4 2.680 (3)
S3ÐSi3 2.0644 (6)
S3ÐLi4 2.459 (2)
O11ÐLi4i 1.953 (2)
O11ÐLi4 1.959 (3)
Li4ÐO10 2.033 (3)
Li4 Li4i 2.451 (5)
Si1ÐS1ÐLi1 75.57 (6)
O11ÐLi2 Li4i 48.78 (8)
O11ÐLi2 Li3 46.09 (8) O10iÐLi2 Li3 130.04 (12)
S2ÐLi2 Li3 55.17 (7) Li4i Li2 Li3 91.48 (10)
Li2 Li3 Li4 81.90 (9) Li4i Li4 Li2i 88.37 (12)
Li4i Li4 Li3 94.23 (13)
Li2i Li4 Li3 164.31 (14)
Li4i Li4 Li2 47.33 (9)
Symmetry code: (i) 1ÿx;ÿy;2ÿz.
H atoms were located in a difference Fourier maps, then posi-tioned geometrically and allowed to ride on their respective parent atoms.
Data collection:IPDS(Stoe & Cie, 1999); cell re®nement:IPDS; data reduction:SHELXTL(Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to re®ne structure: SHELXL97 (Sheldrick, 1997); molecular graphics:
RESVIEW (Schwenk, 1998); software used to prepare material for publication:SHELXL97.
The authors thank Professor Hansgeorg SchnoÈckel for the opportunity to use the diffractometer for the X-ray diffraction measurement.
References
Becker, B., Radacki, K. & Wojnowski, W. (1996).J. Organomet. Chem.521, 39±49.
Bruker (1998).SHELXTL. Bruker AXS Inc., Madison, Wisconsin, USA. Englich, U. & Ruhlandt-Senge, K. (2000).Coord. Chem. Rev.210, 135±179. Hermansson, K. & Thomas, J. O. (1982).Acta Cryst.B38, 2555±2563. OjamaÈe, L., Hermansson, K., Pisani, C., CausaÁ, M. & Roetti, C. (1994).Acta
Cryst.B50, 268±279.
Piekos, R. & Wojnowski, W. (1962).Z. Anorg. Allg. Chem.318, 212±216. Schwenk, H. (1998).RESVIEW. Version 2.21. University of Munich, Germany. Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of
GoÈttingen, Germany.
Stoe & Cie (1997).IPDS.Version 2.86. Stoe & Cie, Darmstadt, Germany. Figure 1
supporting information
Acta Cryst. (2002). E58, m569–m570 [doi:10.1107/S1600536802016987]
Diaquadihydroxohexakis(tri-
tert
-butoxysilanethiolato)octalithium(I)
–
toluene
(1/2)
Katarzyna Baranowska, Jaroslaw Chojnacki, Wieslaw Wojnowski and Ingo Krossing
S1. Comment
Structural studies on thiolates, selenolates and tellurolates of the s-block elements have been recently reviewed (Englich
& Ruhland-Senge, 2000). The list of lithium thiolates cited is about 40 and none of them contain an Li–S–Si fragment.
Now we attempted to introduce a new type of thiolate ligand, (t-BuO)3SiS−, which apart from a coordinating S atom
shows chelating properties using O atom(s) (Becker et al., 1996). The title compound, (I), was obtained according to the
procedure described in the Experimental section. The diaquadihydroxohexakis(tri-tert-butoxysilanethiolato)octalithium(I)
core is presented in Fig. 1. The molecule is centrosymmetric. Formally it can be regarded as an adduct of lithium thiolate
and lithium hydroxide hydrate. Some similarities to the structure of LiOH H2O (Ojamaee et al., 1994; Hermansson &
Thomas, 1982) may be found. Possible sources of H2O could have been oxide layer on the metal or traces of water from
solvents.
Six Li atoms form two side-joined rectangles to which two additional Li atoms are attached terminally. Hydroxyl O
atoms lay in positions bridging four Li atoms. Water molecules are bonded to Li atoms as µ2 ligands. The two-bonded S1
atom is in a terminal position, while all the other S atoms are fourfold bonded to lithium as µ3 ligands. Eight of the 18
tert-butoxy O atoms fill the coordination sphere of the Li atoms. Two disordered [s.o.f. 0.639 (7)/0.361 (7)] toluene
molecules accompany each thiolate molecule. A disorder model was also applied for description of one tert-butyl group
placed on atom O3. The molecule is a rare example of lithium thiolate with Li···Li short contacts of ca 2.5 Å, although
similar distances can be found in LiOH H2O.
S2. Experimental
The work was carried out using standard vacuum–nitrogen line and Schlenk techniques. The title compound was
synthesized by direct reaction of a diethyl ether solution of (t-BuO)3SiSH (Piekos & Wojnowski, 1962) (2 mmol) with
lithium powder. The mixture was stirred magnetically for 2 d. The excess of metal was separated by twofold filtration and
the solvent evaporated to dryness. Recrystallization from toluene afforded colourless crystals suitable for X-ray
diffraction analysis.
S3. Refinement
H atoms were located in the difference Fourier maps, then positioned geometrically and allowed to ride on their
Figure 1
A view of the core of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 25% probability
level. All C and H atoms have been omitted.
Di(aqua)dihydroxohexakis(tri-tert-butoxysilanethiolato)octalithium(I) - toluene (1/2)
Crystal data
[Li8(C12H27O3SSi)6(OH)2(H2O)2]·2C7H8
Mr = 1986.7
Monoclinic, P21/n
Hall symbol: -P 2yn
a = 13.088 (3) Å
b = 27.188 (5) Å
c = 17.525 (4) Å
β = 102.25 (3)°
V = 6094 (2) Å3
Z = 2
F(000) = 2160
Dx = 1.083 Mg m−3
Mo Kα radiation, λ = 0.71073 Å
Cell parameters from 8000 reflections
θ = 4.1–26.1°
µ = 0.23 mm−1
T = 200 K
Thick plate, colourless 0.6 × 0.3 × 0.2 mm
Data collection Bruker IPDS
diffractometer
Radiation source: fine-focus sealed tube Graphite monochromator
area IPDS scans
47490 measured reflections 11732 independent reflections
10031 reflections with I > 2σ(I)
Rint = 0.035
θmax = 25.9°, θmin = 2.2°
h = −16→16
k = −33→33
Refinement
Refinement on F2
Least-squares matrix: full R[F2 > 2σ(F2)] = 0.036
wR(F2) = 0.105
S = 1.04
11732 reflections 669 parameters 31 restraints
Primary atom site location: structure-invariant direct methods
Secondary atom site location: difference Fourier map
Hydrogen site location: inferred from neighbouring sites
H-atom parameters constrained w = 1/[σ2(F
o2) + (0.0696P)2 + 0.8026P]
where P = (Fo2 + 2Fc2)/3
(Δ/σ)max = 0.030
Δρmax = 0.32 e Å−3
Δρmin = −0.24 e Å−3
Special details
Experimental. no
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2,
conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used
only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2
are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
x y z Uiso*/Ueq Occ. (<1)
Li1 0.3540 (2) 0.09614 (9) 0.85630 (15) 0.0426 (6)
S1 0.40258 (3) 0.116879 (14) 0.99526 (2) 0.03868 (10)
Si1 0.32191 (3) 0.177407 (13) 0.94425 (2) 0.03116 (9)
O1 0.22702 (9) 0.19555 (4) 0.98355 (7) 0.0467 (3)
C1 0.0663 (2) 0.20629 (16) 1.0186 (2) 0.1283 (14)
H1A 0.0324 0.2114 0.9650 0.192*
H1B 0.0168 0.1933 1.0467 0.192*
H1C 0.0930 0.2371 1.0413 0.192*
C2 0.20943 (19) 0.16138 (10) 1.10654 (12) 0.0758 (6)
H2A 0.2314 0.1922 1.1315 0.114*
H2B 0.1619 0.1454 1.1334 0.114*
H2C 0.2694 0.1408 1.1080 0.114*
C3 0.15570 (15) 0.17040 (9) 1.02280 (13) 0.0640 (5)
C4 0.1189 (2) 0.12246 (12) 0.98174 (17) 0.0934 (9)
H4A 0.0841 0.1291 0.9288 0.140*
H4B 0.1781 0.1015 0.9820 0.140*
H4C 0.0714 0.1064 1.0085 0.140*
O2 0.27772 (8) 0.15869 (4) 0.85295 (5) 0.0370 (2)
C5 0.3049 (2) 0.20371 (9) 0.74205 (13) 0.0817 (7)
H5A 0.3459 0.2285 0.7736 0.123*
H5B 0.3495 0.1771 0.7337 0.123*
H5C 0.2717 0.2176 0.6926 0.123*
C6 0.22176 (15) 0.18467 (6) 0.78369 (9) 0.0495 (4)
H7A 0.1010 0.1358 0.7631 0.133*
H7B 0.1199 0.1604 0.6864 0.133*
H7C 0.1952 0.1189 0.7272 0.133*
C8 0.15867 (19) 0.22711 (8) 0.80483 (13) 0.0739 (6)
H8A 0.1064 0.2148 0.8310 0.111*
H8B 0.2041 0.2493 0.8388 0.111*
H8C 0.1254 0.2442 0.7582 0.111*
O3 0.38847 (9) 0.22686 (4) 0.93626 (6) 0.0443 (3)
C9 0.5279 (5) 0.2825 (2) 0.9591 (3) 0.103 (3) 0.623 (8)
H9A 0.5834 0.2591 0.9617 0.155* 0.623 (8)
H9B 0.4999 0.2910 0.9056 0.155* 0.623 (8)
H9C 0.5545 0.3115 0.9878 0.155* 0.623 (8)
C9A 0.5593 (5) 0.2440 (4) 1.0107 (8) 0.127 (6) 0.377 (8)
H9D 0.5852 0.2413 0.9636 0.191* 0.377 (8)
H9E 0.5603 0.2121 1.0346 0.191* 0.377 (8)
H9F 0.6027 0.2661 1.0461 0.191* 0.377 (8)
C10 0.44020 (16) 0.26206 (6) 0.99196 (11) 0.0545 (4)
C11 0.3531 (6) 0.30315 (18) 0.9860 (3) 0.0972 (18) 0.623 (8)
H11A 0.2902 0.2965 1.0041 0.146* 0.623 (8)
H11B 0.3884 0.3308 1.0140 0.146* 0.623 (8)
H11C 0.3358 0.3105 0.9312 0.146* 0.623 (8)
C11A 0.4273 (11) 0.3123 (3) 0.9692 (5) 0.110 (5) 0.377 (8)
H11D 0.3580 0.3257 0.9564 0.165* 0.377 (8)
H11E 0.4564 0.3117 0.9233 0.165* 0.377 (8)
H11F 0.4703 0.3322 1.0085 0.165* 0.377 (8)
C12 0.4697 (6) 0.2422 (2) 1.0705 (3) 0.083 (2) 0.623 (8)
H12A 0.5171 0.2148 1.0782 0.124* 0.623 (8)
H12B 0.4983 0.2684 1.1052 0.124* 0.623 (8)
H12C 0.4038 0.2321 1.0811 0.124* 0.623 (8)
C12A 0.4148 (11) 0.2567 (6) 1.0751 (7) 0.106 (5) 0.377 (8)
H12D 0.3438 0.2679 1.0678 0.080* 0.377 (8)
H12E 0.4199 0.2238 1.0958 0.080* 0.377 (8)
H12F 0.4595 0.2781 1.1110 0.080* 0.377 (8)
Li2 0.61825 (19) 0.05337 (9) 0.91064 (13) 0.0358 (5)
S2 0.49948 (3) 0.083604 (13) 0.78254 (2) 0.03587 (9)
Si2 0.64987 (3) 0.083239 (14) 0.76353 (2) 0.03103 (10)
O4 0.71906 (7) 0.05744 (4) 0.84372 (5) 0.0335 (2)
C13 0.81269 (17) −0.01748 (8) 0.83322 (16) 0.0751 (6)
H13A 0.7665 −0.0346 0.8599 0.113*
H13B 0.8802 −0.0329 0.8445 0.113*
H13C 0.7847 −0.0185 0.7780 0.113*
C14 0.86042 (15) 0.03943 (10) 0.94834 (11) 0.0662 (6)
H14A 0.8144 0.0210 0.9736 0.099*
H14B 0.8603 0.0733 0.9637 0.099*
H14C 0.9300 0.0265 0.9634 0.099*
C15 0.89667 (14) 0.06402 (9) 0.81966 (12) 0.0640 (5)
H15A 0.9018 0.0974 0.8378 0.096*
H15C 0.9647 0.0491 0.8313 0.096*
C16 0.82336 (12) 0.03555 (7) 0.86037 (9) 0.0445 (4)
O5 0.66903 (9) 0.04873 (4) 0.69258 (6) 0.0417 (2)
C17 0.6687 (3) 0.00699 (11) 0.57554 (15) 0.1148 (12)
H17A 0.7396 −0.0031 0.5958 0.172*
H17B 0.6566 0.0092 0.5197 0.172*
H17C 0.6217 −0.0167 0.5899 0.172*
C18 0.65093 (16) 0.05613 (8) 0.60875 (9) 0.0566 (5)
C19 0.7305 (3) 0.09155 (13) 0.59065 (14) 0.1177 (13)
H19A 0.8009 0.0789 0.6118 0.177*
H19B 0.7221 0.1235 0.6144 0.177*
H19C 0.7205 0.0954 0.5339 0.177*
C20 0.5422 (3) 0.07361 (19) 0.57973 (13) 0.1398 (17)
H20A 0.5329 0.1045 0.6039 0.210*
H20B 0.4941 0.0499 0.5925 0.210*
H20C 0.5293 0.0778 0.5241 0.210*
O6 0.69754 (9) 0.13643 (4) 0.74817 (6) 0.0450 (3)
C21 0.6068 (2) 0.21254 (9) 0.7494 (2) 0.1012 (9)
H21A 0.5487 0.1976 0.7660 0.152*
H21B 0.5947 0.2119 0.6935 0.152*
H21C 0.6142 0.2460 0.7673 0.152*
C22 0.7224 (2) 0.18048 (9) 0.87132 (13) 0.0830 (7)
H22A 0.6622 0.1657 0.8852 0.124*
H22B 0.7332 0.2127 0.8940 0.124*
H22C 0.7828 0.1605 0.8905 0.124*
C23 0.7989 (2) 0.20821 (9) 0.75963 (18) 0.0921 (9)
H23A 0.7863 0.2109 0.7038 0.138*
H23B 0.8597 0.1882 0.7778 0.138*
H23C 0.8102 0.2404 0.7825 0.138*
C24 0.70470 (17) 0.18452 (7) 0.78309 (11) 0.0564 (4)
Li3 0.46363 (18) 0.00101 (9) 0.82350 (13) 0.0331 (5)
S3 0.27493 (3) 0.011720 (12) 0.853421 (18) 0.03073 (9)
Si3 0.27025 (3) −0.050209 (13) 0.784603 (19) 0.02714 (9)
O7 0.18441 (8) −0.05102 (4) 0.70316 (5) 0.0367 (2)
C25 0.23262 (18) 0.01956 (8) 0.63263 (11) 0.0650 (5)
H25A 0.2874 0.0009 0.6177 0.097*
H25B 0.2599 0.0365 0.6807 0.097*
H25C 0.2055 0.0430 0.5925 0.097*
C26 0.10487 (19) −0.04469 (9) 0.56998 (10) 0.0722 (6)
H26A 0.0506 −0.0664 0.5785 0.108*
H26B 0.1610 −0.0636 0.5574 0.108*
H26C 0.0774 −0.0229 0.5276 0.108*
C27 0.14567 (14) −0.01485 (6) 0.64379 (9) 0.0476 (4)
C28 0.05776 (16) 0.01324 (8) 0.66865 (12) 0.0651 (5)
H28A 0.0044 −0.0094 0.6761 0.098*
H28B 0.0285 0.0366 0.6289 0.098*
H28C 0.0848 0.0303 0.7167 0.098*
C29 0.18610 (16) −0.16786 (7) 0.89315 (11) 0.0580 (5)
H29A 0.2019 −0.1510 0.9424 0.087*
H29B 0.2464 −0.1860 0.8862 0.087*
H29C 0.1289 −0.1901 0.8923 0.087*
C30 0.12976 (15) −0.15707 (7) 0.74931 (11) 0.0552 (4)
H30A 0.1100 −0.1335 0.7081 0.083*
H30B 0.0728 −0.1794 0.7490 0.083*
H30C 0.1898 −0.1751 0.7416 0.083*
C31 0.15624 (12) −0.13053 (6) 0.82741 (9) 0.0393 (3)
C32 0.06662 (13) −0.09771 (8) 0.83899 (11) 0.0542 (4)
H32A 0.0497 −0.0748 0.7964 0.081*
H32B 0.0871 −0.0800 0.8872 0.081*
H32C 0.0065 −0.1176 0.8407 0.081*
O9 0.39054 (7) −0.05571 (3) 0.76993 (5) 0.0309 (2)
C33 0.44418 (12) −0.09355 (6) 0.73312 (8) 0.0377 (3)
C34 0.45868 (18) −0.13913 (7) 0.78346 (12) 0.0625 (5)
H34A 0.3917 −0.1536 0.7832 0.094*
H34B 0.4919 −0.1305 0.8360 0.094*
H34C 0.5016 −0.1623 0.7632 0.094*
C35 0.3822 (2) −0.10533 (11) 0.65305 (12) 0.0934 (10)
H35A 0.3753 −0.0763 0.6212 0.140*
H35B 0.3140 −0.1168 0.6568 0.140*
H35C 0.4174 −0.1304 0.6300 0.140*
C36 0.5494 (2) −0.07117 (9) 0.7327 (2) 0.1045 (11)
H36A 0.5404 −0.0423 0.7003 0.157*
H36B 0.5918 −0.0946 0.7126 0.157*
H36C 0.5832 −0.0623 0.7850 0.157*
O11 0.54664 (7) −0.00555 (3) 0.92782 (5) 0.0303 (2)
H11G 0.5807 −0.0350 0.9324 0.036*
Li4 0.41519 (19) −0.01426 (10) 0.96272 (13) 0.0369 (5)
O10 0.37146 (8) −0.08350 (4) 0.98571 (5) 0.0354 (2)
H10B 0.4221 −0.1014 0.9858 0.043*
H10A 0.3246 −0.0918 0.9437 0.043*
C56 0.2680 (8) −0.3710 (4) 1.0311 (4) 0.107 (4) 0.639 (7)
H56A 0.3211 −0.3937 1.0234 0.128* 0.639 (7)
C52 0.1793 (7) −0.3331 (3) 1.1145 (5) 0.112 (4) 0.639 (7)
H52A 0.1736 −0.3231 1.1660 0.134* 0.639 (7)
C55 0.1985 (7) −0.3535 (3) 0.9657 (3) 0.130 (3) 0.639 (7)
H55A 0.2015 −0.3655 0.9147 0.156* 0.639 (7)
C51 0.2606 (3) −0.36238 (14) 1.1041 (2) 0.0735 (14) 0.639 (7)
C54 0.1203 (11) −0.3204 (6) 0.9762 (6) 0.217 (10) 0.639 (7)
H54A 0.0837 −0.3017 0.9323 0.261* 0.639 (7)
C53 0.1151 (6) −0.3095 (2) 1.0533 (6) 0.154 (4) 0.639 (7)
H53A 0.0555 −0.2912 1.0612 0.185* 0.639 (7)
C50 0.3302 (10) −0.3822 (4) 1.1690 (8) 0.154 (5) 0.639 (7)
H50A 0.3799 −0.4039 1.1535 0.185* 0.639 (7)
H50B 0.3666 −0.3559 1.2001 0.185* 0.639 (7)
C61 0.1943 (5) −0.3371 (2) 1.0309 (4) 0.076 (2) 0.361 (7)
C62 0.2022 (10) −0.3247 (4) 1.1085 (5) 0.082 (4) 0.361 (7)
H62A 0.1577 −0.3022 1.1285 0.099* 0.361 (7)
C65 0.3262 (9) −0.3986 (5) 1.0674 (9) 0.158 (6) 0.361 (7)
H65A 0.3683 −0.4219 1.0464 0.189* 0.361 (7)
C64 0.3325 (12) −0.3882 (6) 1.1460 (8) 0.162 (11) 0.361 (7)
H64A 0.3869 −0.4060 1.1804 0.194* 0.361 (7)
C66 0.2529 (11) −0.3753 (6) 1.0108 (7) 0.082 (4) 0.361 (7)
H66A 0.2464 −0.3788 0.9555 0.098* 0.361 (7)
C63 0.2631 (11) −0.3538 (4) 1.1661 (5) 0.161 (9) 0.361 (7)
H63A 0.2689 −0.3507 1.2214 0.193* 0.361 (7)
C60 0.1290 (11) −0.3143 (6) 0.9750 (8) 0.152 (11) 0.361 (7)
H60A 0.1306 −0.3212 0.9215 0.182* 0.361 (7)
H60B 0.0627 −0.3242 0.9850 0.182* 0.361 (7)
H60C 0.1387 −0.2797 0.9846 0.182* 0.361 (7)
Atomic displacement parameters (Å2)
U11 U22 U33 U12 U13 U23
Li1 0.0554 (15) 0.0323 (13) 0.0399 (13) 0.0066 (11) 0.0095 (11) 0.0004 (10)
S1 0.0467 (2) 0.03331 (19) 0.03350 (18) 0.00866 (14) 0.00288 (14) 0.00498 (14)
Si1 0.0369 (2) 0.02489 (19) 0.03067 (18) 0.00222 (14) 0.00480 (14) 0.00117 (14)
O1 0.0477 (6) 0.0445 (6) 0.0511 (6) 0.0094 (5) 0.0172 (5) 0.0017 (5)
C1 0.0781 (18) 0.184 (4) 0.139 (3) 0.059 (2) 0.0608 (19) 0.035 (3)
C2 0.0828 (15) 0.0961 (17) 0.0571 (12) −0.0112 (13) 0.0338 (11) 0.0020 (11)
C3 0.0467 (10) 0.0839 (15) 0.0675 (12) 0.0021 (9) 0.0256 (9) 0.0036 (11)
C4 0.0702 (14) 0.119 (2) 0.0908 (17) −0.0498 (15) 0.0165 (13) −0.0055 (16)
O2 0.0488 (6) 0.0268 (5) 0.0310 (5) 0.0068 (4) −0.0012 (4) 0.0020 (4)
C5 0.123 (2) 0.0666 (14) 0.0573 (12) 0.0170 (14) 0.0226 (13) 0.0276 (11)
C6 0.0704 (11) 0.0343 (8) 0.0355 (8) 0.0130 (7) −0.0076 (7) 0.0062 (6)
C7 0.115 (2) 0.0562 (13) 0.0671 (13) 0.0044 (12) −0.0431 (13) −0.0010 (10)
C8 0.0909 (15) 0.0583 (12) 0.0607 (12) 0.0364 (11) −0.0105 (11) 0.0055 (10)
O3 0.0576 (6) 0.0346 (6) 0.0383 (5) −0.0104 (5) 0.0047 (5) 0.0018 (4)
C9 0.114 (4) 0.097 (5) 0.100 (3) −0.071 (4) 0.025 (3) −0.020 (3)
C9A 0.055 (4) 0.118 (8) 0.190 (12) −0.010 (4) −0.013 (5) −0.069 (9)
C10 0.0749 (12) 0.0345 (9) 0.0514 (9) −0.0173 (8) 0.0076 (8) −0.0056 (7)
C11 0.138 (5) 0.039 (2) 0.106 (4) 0.009 (3) 0.008 (3) −0.028 (2)
C11A 0.178 (13) 0.038 (3) 0.084 (5) −0.021 (5) −0.040 (7) 0.006 (3)
C12 0.124 (5) 0.058 (3) 0.049 (3) −0.035 (3) −0.023 (3) 0.003 (2)
C12A 0.148 (11) 0.119 (11) 0.050 (4) −0.067 (8) 0.019 (7) −0.030 (6)
Li2 0.0423 (12) 0.0407 (13) 0.0249 (10) −0.0063 (10) 0.0083 (9) 0.0025 (9)
S2 0.03889 (18) 0.0361 (2) 0.03430 (18) 0.00290 (14) 0.01155 (14) 0.00878 (13)
Si2 0.0395 (2) 0.0319 (2) 0.02289 (17) −0.00335 (14) 0.00937 (14) 0.00161 (13)
O4 0.0338 (5) 0.0408 (5) 0.0265 (4) 0.0010 (4) 0.0074 (4) 0.0028 (4)
C13 0.0572 (11) 0.0561 (12) 0.1077 (18) 0.0179 (9) 0.0077 (11) −0.0129 (12)
C14 0.0496 (10) 0.0977 (17) 0.0458 (10) 0.0152 (10) −0.0023 (8) 0.0112 (10)
C15 0.0399 (9) 0.0935 (16) 0.0617 (11) −0.0046 (9) 0.0175 (8) −0.0007 (11)
O5 0.0534 (6) 0.0485 (6) 0.0254 (5) −0.0020 (5) 0.0132 (4) −0.0036 (4)
C17 0.205 (4) 0.097 (2) 0.0536 (13) −0.010 (2) 0.0549 (18) −0.0322 (13)
C18 0.0717 (12) 0.0769 (13) 0.0236 (7) −0.0062 (10) 0.0160 (7) −0.0056 (7)
C19 0.185 (3) 0.136 (3) 0.0477 (12) −0.068 (2) 0.0595 (17) −0.0106 (14)
C20 0.110 (2) 0.272 (5) 0.0300 (11) 0.064 (3) −0.0017 (12) 0.0087 (18)
O6 0.0615 (7) 0.0385 (6) 0.0381 (5) −0.0130 (5) 0.0177 (5) 0.0027 (4)
C21 0.111 (2) 0.0484 (13) 0.141 (3) 0.0088 (13) 0.0205 (19) 0.0104 (15)
C22 0.138 (2) 0.0557 (13) 0.0602 (13) −0.0218 (14) 0.0329 (13) −0.0199 (10)
C23 0.117 (2) 0.0616 (14) 0.110 (2) −0.0461 (14) 0.0507 (17) −0.0121 (13)
C24 0.0793 (12) 0.0356 (9) 0.0576 (10) −0.0151 (8) 0.0222 (9) 0.0000 (7)
Li3 0.0401 (12) 0.0319 (12) 0.0273 (10) −0.0046 (9) 0.0070 (9) 0.0001 (9)
S3 0.03661 (17) 0.02851 (17) 0.02649 (16) 0.00068 (12) 0.00538 (12) −0.00316 (12)
Si3 0.03171 (18) 0.02737 (19) 0.02110 (16) −0.00053 (13) 0.00282 (13) −0.00070 (13)
O7 0.0421 (5) 0.0377 (6) 0.0257 (5) 0.0010 (4) −0.0030 (4) −0.0007 (4)
C25 0.0942 (15) 0.0581 (12) 0.0446 (9) 0.0119 (10) 0.0190 (10) 0.0216 (8)
C26 0.0889 (15) 0.0843 (15) 0.0301 (8) 0.0292 (12) −0.0174 (9) −0.0087 (9)
C27 0.0586 (10) 0.0513 (10) 0.0267 (7) 0.0171 (8) −0.0046 (6) 0.0017 (6)
C28 0.0608 (11) 0.0719 (13) 0.0556 (11) 0.0279 (10) −0.0035 (9) −0.0065 (9)
O8 0.0352 (5) 0.0305 (5) 0.0306 (5) −0.0060 (4) 0.0036 (4) 0.0017 (4)
C29 0.0662 (11) 0.0489 (10) 0.0597 (11) −0.0181 (9) 0.0149 (9) 0.0119 (8)
C30 0.0658 (11) 0.0455 (10) 0.0528 (10) −0.0198 (8) 0.0092 (8) −0.0152 (8)
C31 0.0400 (7) 0.0371 (8) 0.0412 (8) −0.0125 (6) 0.0094 (6) −0.0025 (6)
C32 0.0433 (9) 0.0667 (12) 0.0557 (10) −0.0061 (8) 0.0175 (7) −0.0050 (9)
O9 0.0363 (5) 0.0285 (5) 0.0288 (4) −0.0004 (4) 0.0086 (4) −0.0038 (4)
C33 0.0430 (8) 0.0365 (8) 0.0356 (7) 0.0052 (6) 0.0123 (6) −0.0064 (6)
C34 0.0822 (13) 0.0476 (11) 0.0596 (11) 0.0225 (9) 0.0194 (10) 0.0018 (8)
C35 0.1144 (19) 0.118 (2) 0.0381 (10) 0.0651 (17) −0.0055 (11) −0.0299 (12)
C36 0.0867 (17) 0.0652 (14) 0.192 (3) −0.0145 (13) 0.097 (2) −0.0397 (18)
O11 0.0356 (5) 0.0299 (5) 0.0247 (4) −0.0003 (4) 0.0046 (4) 0.0049 (3)
Li4 0.0403 (12) 0.0463 (14) 0.0227 (10) −0.0090 (10) 0.0032 (9) 0.0044 (9)
O10 0.0374 (5) 0.0398 (6) 0.0272 (5) −0.0013 (4) 0.0027 (4) 0.0003 (4)
C56 0.139 (8) 0.112 (6) 0.080 (4) −0.045 (5) 0.044 (5) −0.030 (4)
C52 0.129 (6) 0.060 (4) 0.161 (8) −0.047 (4) 0.066 (5) −0.025 (4)
C55 0.181 (7) 0.134 (6) 0.069 (3) −0.037 (5) 0.012 (4) −0.005 (4)
C51 0.073 (3) 0.061 (2) 0.080 (3) −0.0234 (19) 0.0021 (18) 0.0036 (18)
C54 0.247 (19) 0.147 (14) 0.25 (2) −0.072 (12) 0.037 (14) −0.017 (12)
C53 0.141 (6) 0.073 (4) 0.232 (11) 0.029 (4) 0.002 (6) 0.005 (5)
C50 0.163 (11) 0.134 (10) 0.141 (7) −0.051 (7) −0.019 (6) 0.058 (6)
C61 0.084 (5) 0.050 (4) 0.089 (5) −0.003 (3) 0.006 (4) 0.006 (3)
C62 0.106 (8) 0.048 (5) 0.102 (8) −0.027 (6) 0.043 (6) −0.031 (5)
C65 0.116 (9) 0.124 (11) 0.217 (18) 0.028 (8) −0.001 (10) 0.026 (12)
C64 0.078 (9) 0.106 (11) 0.27 (3) −0.006 (7) −0.043 (12) −0.028 (15)
C66 0.079 (6) 0.094 (8) 0.067 (7) 0.007 (5) 0.003 (5) −0.041 (6)
C63 0.25 (2) 0.158 (14) 0.058 (6) −0.133 (15) −0.011 (8) 0.002 (7)
Geometric parameters (Å, º)
Li1—O2 1.967 (3) C20—H20A 0.9600
Li1—S1 2.449 (3) C20—H20B 0.9600
Li1—S3 2.514 (3) C20—H20C 0.9599
Li1—S2 2.541 (3) O6—C24 1.438 (2)
Li1—Si1 2.777 (3) C21—C24 1.500 (4)
Li1—Li3 3.070 (4) C21—H21A 0.9600
Li1—Li4 3.535 (4) C21—H21B 0.9602
S1—Si1 2.0546 (6) C21—H21C 0.9602
Si1—O1 1.6196 (12) C22—C24 1.518 (3)
Si1—O3 1.6242 (11) C22—H22A 0.9599
Si1—O2 1.6616 (11) C22—H22B 0.9600
O1—C3 1.444 (2) C22—H22C 0.9600
C1—C3 1.514 (3) C23—C24 1.523 (3)
C1—H1A 0.9599 C23—H23A 0.9599
C1—H1B 0.9600 C23—H23B 0.9600
C1—H1C 0.9601 C23—H23C 0.9601
C2—C3 1.507 (3) Li3—O11 1.926 (2)
C2—H2A 0.9600 Li3—O9 1.948 (2)
C2—H2B 0.9600 Li3—S3 2.647 (2)
C2—H2C 0.9599 Li3—Li4 2.680 (3)
C3—C4 1.517 (4) Li3—Si3 2.842 (2)
C4—H4A 0.9599 S3—Si3 2.0644 (6)
C4—H4B 0.9601 S3—Li4 2.459 (2)
C4—H4C 0.9600 Si3—O7 1.6185 (11)
O2—C6 1.4600 (17) Si3—O8 1.6433 (10)
C5—C6 1.523 (3) Si3—O9 1.6549 (10)
C5—H5A 0.9598 O7—C27 1.4431 (18)
C5—H5B 0.9601 C25—C27 1.518 (3)
C5—H5C 0.9599 C25—H25A 0.9600
C6—C7 1.506 (3) C25—H25B 0.9602
C6—C8 1.510 (3) C25—H25C 0.9600
C7—H7A 0.9600 C26—C27 1.524 (2)
C7—H7B 0.9600 C26—H26A 0.9601
C7—H7C 0.9598 C26—H26B 0.9601
C8—H8A 0.9599 C26—H26C 0.9599
C8—H8B 0.9599 C27—C28 1.520 (2)
C8—H8C 0.9600 C28—H28A 0.9600
O3—C10 1.431 (2) C28—H28B 0.9600
C9—C10 1.495 (5) C28—H28C 0.9600
C9—H9A 0.9600 O8—C31 1.4578 (16)
C9—H9B 0.9600 C29—C31 1.523 (2)
C9—H9C 0.9600 C29—H29A 0.9601
C9A—C10 1.601 (8) C29—H29B 0.9601
C9A—H9A 1.0594 C29—H29C 0.9600
C9A—H9D 0.9599 C30—C31 1.521 (2)
C9A—H9F 0.9600 C30—H30B 0.9599
C10—C11A 1.422 (7) C30—H30C 0.9599
C10—C12 1.452 (6) C31—C32 1.521 (2)
C10—C12A 1.569 (11) C32—H32A 0.9599
C10—C11 1.584 (5) C32—H32B 0.9599
C11—H11A 0.9600 C32—H32C 0.9601
C11—H11B 0.9601 O9—C33 1.4696 (16)
C11—H11C 0.9600 C33—C35 1.499 (2)
C11—H11D 0.8151 C33—C36 1.507 (3)
C11A—H11B 1.1386 C33—C34 1.510 (2)
C11A—H11C 1.2418 C34—H34A 0.9601
C11A—H11D 0.9600 C34—H34B 0.9601
C11A—H11E 0.9599 C34—H34C 0.9600
C11A—H11F 0.9601 C35—H35A 0.9600
C12—H12A 0.9601 C35—H35B 0.9600
C12—H12B 0.9598 C35—H35C 0.9600
C12—H12C 0.9600 C36—H36A 0.9600
C12—H12E 0.9962 C36—H36B 0.9598
C12—H12F 1.2312 C36—H36C 0.9600
C12A—H12B 1.1524 O11—Li4i 1.953 (2)
C12A—H12C 0.6951 O11—Li4 1.959 (3)
C12A—H12D 0.9599 O11—H11G 0.9126
C12A—H12E 0.9601 Li4—O11i 1.953 (2)
C12A—H12F 0.9598 Li4—O10 2.033 (3)
Li2—O11 1.912 (3) Li4—Li4i 2.451 (5)
Li2—O4 1.945 (3) Li4—Li2i 2.581 (3)
Li2—O10i 1.971 (3) O10—Li2i 1.971 (3)
Li2—S2 2.579 (2) O10—H10B 0.8210
Li2—Li4i 2.581 (3) O10—H10A 0.8821
Li2—Li3 2.673 (3) C56—C51 1.324 (7)
Li2—Si2 2.816 (2) C56—C55 1.387 (7)
Li2—Li4 3.508 (3) C56—H56A 0.9600
S2—Si2 2.0649 (7) C52—C53 1.372 (7)
S2—Li3 2.433 (2) C52—C51 1.372 (7)
Si2—O5 1.6191 (11) C52—H52A 0.9601
Si2—O6 1.6201 (11) C55—C54 1.406 (8)
Si2—O4 1.6574 (11) C55—H55A 0.9599
O4—C16 1.4608 (18) C51—C50 1.405 (10)
C13—C16 1.515 (3) C54—C53 1.399 (8)
C13—H13A 0.9600 C54—H54A 0.9601
C13—H13B 0.9599 C53—H53A 0.9600
C13—H13C 0.9600 C50—H50A 0.9599
C14—C16 1.519 (2) C50—H50B 0.9600
C14—H14A 0.9600 C50—H50C 0.9601
C14—H14B 0.9603 C61—C60 1.311 (11)
C14—H14C 0.9599 C61—C66 1.381 (8)
C15—C16 1.523 (3) C61—C62 1.383 (8)
C15—H15B 0.9599 C62—H62A 0.9599
C15—H15C 0.9600 C65—C66 1.379 (8)
O5—C18 1.4517 (18) C65—C64 1.392 (8)
C17—C18 1.495 (3) C65—H65A 0.9601
C17—H17A 0.9599 C64—C63 1.399 (8)
C17—H17B 0.9600 C64—H64A 0.9599
C17—H17C 0.9600 C66—H56A 1.0062
C18—C20 1.484 (4) C66—H66A 0.9600
C18—C19 1.501 (3) C63—H63A 0.9600
C19—H19A 0.9800 C60—H60A 0.9601
C19—H19B 0.9800 C60—H60B 0.9600
C19—H19C 0.9800 C60—H60C 0.9600
O2—Li1—S1 81.57 (9) C24—O6—Si2 137.17 (10)
O2—Li1—S3 125.76 (14) C24—C21—H21A 109.4
S1—Li1—S3 104.42 (10) C24—C21—H21B 109.6
O2—Li1—S2 122.10 (12) H21A—C21—H21B 109.5
S1—Li1—S2 118.20 (11) C24—C21—H21C 109.5
S3—Li1—S2 102.54 (9) H21A—C21—H21C 109.5
O2—Li1—Si1 36.17 (5) H21B—C21—H21C 109.4
S1—Li1—Si1 45.77 (5) C24—C22—H22A 109.4
S3—Li1—Si1 128.86 (11) C24—C22—H22B 109.5
S2—Li1—Si1 127.39 (11) H22A—C22—H22B 109.5
O2—Li1—Li3 167.76 (13) C24—C22—H22C 109.5
S1—Li1—Li3 110.32 (10) H22A—C22—H22C 109.5
S3—Li1—Li3 55.53 (7) H22B—C22—H22C 109.5
S2—Li1—Li3 50.32 (6) C24—C23—H23A 109.5
Si1—Li1—Li3 154.96 (11) C24—C23—H23B 109.4
O2—Li1—Li4 143.77 (12) H23A—C23—H23B 109.5
S1—Li1—Li4 71.87 (7) C24—C23—H23C 109.5
S3—Li1—Li4 44.07 (6) H23A—C23—H23C 109.5
S2—Li1—Li4 92.54 (8) H23B—C23—H23C 109.5
Si1—Li1—Li4 115.26 (9) O6—C24—C21 108.74 (19)
Li3—Li1—Li4 47.23 (7) O6—C24—C22 110.46 (15)
Si1—S1—Li1 75.57 (6) C21—C24—C22 111.7 (2)
O1—Si1—O3 104.97 (6) O6—C24—C23 104.65 (17)
O1—Si1—O2 111.17 (6) C21—C24—C23 110.6 (2)
O3—Si1—O2 104.71 (6) C22—C24—C23 110.4 (2)
O1—Si1—S1 115.38 (5) O11—Li3—O9 120.30 (13)
O3—Si1—S1 117.71 (5) O11—Li3—S2 105.08 (10)
O2—Si1—S1 102.44 (4) O9—Li3—S2 133.96 (11)
O1—Si1—Li1 134.31 (8) O11—Li3—S3 100.61 (9)
O3—Si1—Li1 117.62 (7) O9—Li3—S3 78.42 (8)
S1—Si1—Li1 58.65 (6) S2—Li3—S3 101.73 (9)
C3—O1—Si1 133.63 (12) O11—Li3—Li2 45.64 (8)
C3—C1—H1A 109.4 O9—Li3—Li2 158.76 (14)
C3—C1—H1B 109.6 S2—Li3—Li2 60.46 (7)
C3—C1—H1C 109.4 O11—Li3—Li4 46.88 (7)
H1A—C1—H1C 109.5 O9—Li3—Li4 97.43 (10)
H1B—C1—H1C 109.5 S2—Li3—Li4 120.61 (11)
C3—C2—H2A 109.6 S3—Li3—Li4 54.97 (7)
C3—C2—H2B 109.5 Li2—Li3—Li4 81.90 (9)
H2A—C2—H2B 109.5 O11—Li3—Si3 118.46 (10)
C3—C2—H2C 109.3 O9—Li3—Si3 34.43 (5)
H2A—C2—H2C 109.5 S2—Li3—Si3 126.80 (9)
H2B—C2—H2C 109.5 S3—Li3—Si3 44.00 (4)
O1—C3—C2 109.01 (16) Li2—Li3—Si3 157.80 (10)
O1—C3—C1 104.0 (2) Li4—Li3—Si3 76.81 (8)
C2—C3—C1 110.4 (2) O11—Li3—Li1 95.28 (10)
O1—C3—C4 110.67 (17) O9—Li3—Li1 123.78 (12)
C2—C3—C4 111.0 (2) S2—Li3—Li1 53.47 (7)
C1—C3—C4 111.5 (2) S3—Li3—Li1 51.52 (7)
C3—C4—H4A 109.5 Li2—Li3—Li1 76.79 (10)
C3—C4—H4B 109.4 Li4—Li3—Li1 75.52 (10)
H4A—C4—H4B 109.5 Si3—Li3—Li1 91.72 (9)
C3—C4—H4C 109.5 Si3—S3—Li4 98.36 (6)
H4A—C4—H4C 109.5 Si3—S3—Li1 135.83 (6)
H4B—C4—H4C 109.5 Li4—S3—Li1 90.60 (9)
C6—O2—Si1 131.54 (10) Si3—S3—Li3 73.01 (5)
C6—O2—Li1 127.24 (12) Li4—S3—Li3 63.19 (8)
Si1—O2—Li1 99.51 (9) Li1—S3—Li3 72.95 (8)
C6—C5—H5A 109.4 O7—Si3—O8 105.59 (5)
C6—C5—H5B 109.6 O7—Si3—O9 111.53 (6)
H5A—C5—H5B 109.5 O8—Si3—O9 105.39 (5)
C6—C5—H5C 109.4 O7—Si3—S3 117.08 (4)
H5A—C5—H5C 109.5 O8—Si3—S3 112.09 (4)
H5B—C5—H5C 109.5 O9—Si3—S3 104.67 (4)
O2—C6—C7 105.34 (14) O7—Si3—Li3 129.38 (6)
O2—C6—C8 111.69 (14) O8—Si3—Li3 121.44 (6)
C7—C6—C8 111.84 (19) O9—Si3—Li3 41.71 (6)
O2—C6—C5 106.22 (15) S3—Si3—Li3 62.99 (5)
C7—C6—C5 111.6 (2) C27—O7—Si3 134.31 (10)
C8—C6—C5 109.96 (18) C27—C25—H25A 109.5
C6—C7—H7A 109.4 C27—C25—H25B 109.5
C6—C7—H7B 109.5 H25A—C25—H25B 109.5
H7A—C7—H7B 109.5 C27—C25—H25C 109.5
C6—C7—H7C 109.5 H25A—C25—H25C 109.5
H7A—C7—H7C 109.5 H25B—C25—H25C 109.5
H7B—C7—H7C 109.5 C27—C26—H26A 109.5
C6—C8—H8A 109.5 C27—C26—H26B 109.4
C6—C8—H8B 109.5 H26A—C26—H26B 109.5
H8A—C8—H8B 109.5 C27—C26—H26C 109.5
C6—C8—H8C 109.5 H26A—C26—H26C 109.5
H8A—C8—H8C 109.5 H26B—C26—H26C 109.5
C10—O3—Si1 132.82 (10) O7—C27—C28 107.89 (14)
C10—C9—H9A 111.7 C25—C27—C28 111.16 (17)
C10—C9—H9B 107.5 O7—C27—C26 104.80 (14)
H9A—C9—H9B 109.5 C25—C27—C26 110.86 (17)
C10—C9—H9C 109.1 C28—C27—C26 111.13 (16)
H9A—C9—H9C 109.5 C27—C28—H28A 109.5
H9B—C9—H9C 109.5 C27—C28—H28B 109.5
C10—C9—H9D 97.7 H28A—C28—H28B 109.5
C10—C9—H11E 83.1 C27—C28—H28C 109.5
C10—C9A—H9A 99.1 H28A—C28—H28C 109.5
C10—C9A—H9D 110.7 H28B—C28—H28C 109.5
C10—C9A—H9E 106.8 C31—O8—Si3 132.02 (9)
C10—C9A—H9F 110.9 C31—C29—H29A 109.5
H9D—C9A—H9F 109.5 C31—C29—H29B 109.4
H9E—C9A—H9F 109.5 H29A—C29—H29B 109.5
C11A—C10—O3 116.1 (3) C31—C29—H29C 109.5
C11A—C10—C12 127.9 (4) H29A—C29—H29C 109.5
O3—C10—C12 112.9 (3) H29B—C29—H29C 109.5
C11A—C10—C9 65.8 (6) C31—C30—H30A 109.5
O3—C10—C9 106.1 (2) C31—C30—H30B 109.5
C12—C10—C9 115.6 (4) H30A—C30—H30B 109.5
C11A—C10—C12A 108.3 (7) C31—C30—H30C 109.4
O3—C10—C12A 114.1 (5) H30A—C30—H30C 109.5
C9—C10—C12A 136.3 (5) H30B—C30—H30C 109.5
O3—C10—C11 101.4 (2) O8—C31—C30 109.55 (12)
C12—C10—C11 111.6 (4) O8—C31—C32 109.07 (13)
C9—C10—C11 108.2 (4) C30—C31—C32 111.32 (14)
C12A—C10—C11 80.5 (6) O8—C31—C29 105.19 (12)
C11A—C10—C9A 113.9 (7) C30—C31—C29 109.72 (15)
O3—C10—C9A 103.5 (3) C32—C31—C29 111.80 (14)
C12—C10—C9A 68.9 (6) C31—C32—H32A 109.5
C9—C10—C9A 53.1 (5) C31—C32—H32B 109.4
C12A—C10—C9A 99.7 (7) H32A—C32—H32B 109.5
C11—C10—C9A 152.4 (4) C31—C32—H32C 109.5
C10—C11—H11A 120.0 H32A—C32—H32C 109.5
C10—C11—H11B 104.8 H32B—C32—H32C 109.5
H11A—C11—H11B 109.5 C33—O9—Si3 133.66 (9)
C10—C11—H11C 103.1 C33—O9—Li3 122.30 (11)
H11A—C11—H11C 109.5 Si3—O9—Li3 103.86 (8)
H11B—C11—H11C 109.5 O9—C33—C35 110.25 (13)
C10—C11—H11D 114.9 O9—C33—C36 103.99 (13)
C10—C11A—H11B 106.0 C35—C33—C36 113.3 (2)
C10—C11A—H11C 99.1 O9—C33—C34 109.31 (12)
H11B—C11A—H11C 82.3 C35—C33—C34 110.35 (18)
C10—C11A—H11D 118.8 C36—C33—C34 109.43 (19)
C10—C11A—H11E 100.1 C33—C34—H34A 109.4
H11D—C11A—H11E 109.5 C33—C34—H34B 109.5
H11D—C11A—H11F 109.5 C33—C34—H34C 109.5
H11E—C11A—H11F 109.5 H34A—C34—H34C 109.5
C10—C12—H12A 117.1 H34B—C34—H34C 109.5
C10—C12—H12B 108.3 C33—C35—H35A 109.5
H12A—C12—H12B 109.5 C33—C35—H35B 109.4
C10—C12—H12C 102.7 H35A—C35—H35B 109.5
H12A—C12—H12C 109.5 C33—C35—H35C 109.5
H12B—C12—H12C 109.5 H35A—C35—H35C 109.5
C10—C12—H12E 122.7 H35B—C35—H35C 109.5
C10—C12—H12F 102.2 C33—C36—H36A 109.6
C10—C12A—H12B 91.8 C33—C36—H36B 109.5
C10—C12A—H12C 108.7 H36A—C36—H36B 109.5
H12B—C12A—H12C 113.8 C33—C36—H36C 109.4
C10—C12A—H12D 103.6 H36A—C36—H36C 109.5
C10—C12A—H12E 115.2 H36B—C36—H36C 109.5
H12D—C12A—H12E 109.5 Li2—O11—Li3 88.26 (10)
C10—C12A—H12F 109.4 Li2—O11—Li4i 83.78 (10)
H12D—C12A—H12F 109.5 Li3—O11—Li4i 151.88 (12)
H12E—C12A—H12F 109.5 Li2—O11—Li4 130.01 (12)
O11—Li2—O4 124.08 (14) Li3—O11—Li4 87.23 (10)
O11—Li2—O10i 98.23 (10) Li4i—O11—Li4 77.59 (11)
O4—Li2—O10i 127.55 (13) Li2—O11—H11G 120.2
O11—Li2—S2 100.31 (10) Li3—O11—H11G 109.3
O4—Li2—S2 79.50 (8) Li4i—O11—H11G 97.9
O10i—Li2—S2 125.48 (12) Li4—O11—H11G 108.2
O11—Li2—Li4i 48.78 (8) O11i—Li4—O11 102.41 (11)
O4—Li2—Li4i 143.35 (14) O11i—Li4—O10 94.87 (10)
O10i—Li2—Li4i 50.92 (8) O11—Li4—O10 118.48 (14)
S2—Li2—Li4i 134.35 (11) O11i—Li4—Li4i 51.31 (9)
O11—Li2—Li3 46.09 (8) O11—Li4—Li4i 51.09 (9)
O4—Li2—Li3 102.36 (11) O10—Li4—Li4i 116.66 (16)
O10i—Li2—Li3 130.04 (12) O11i—Li4—S3 132.78 (13)
S2—Li2—Li3 55.17 (7) O11—Li4—S3 106.38 (10)
Li4i—Li2—Li3 91.48 (10) O10—Li4—S3 103.03 (10)
O11—Li2—Si2 123.91 (11) Li4i—Li4—S3 140.04 (16)
O4—Li2—Si2 35.07 (5) O11i—Li4—Li2i 47.43 (8)
O10i—Li2—Si2 136.83 (12) O11—Li4—Li2i 129.71 (13)
S2—Li2—Si2 44.74 (4) O10—Li4—Li2i 48.83 (8)
Li4i—Li2—Si2 172.23 (12) Li4i—Li4—Li2i 88.37 (12)
Li3—Li2—Si2 82.59 (8) S3—Li4—Li2i 123.61 (11)
O11—Li2—Li4 25.32 (7) O11i—Li4—Li3 142.27 (13)
O4—Li2—Li4 146.59 (12) O11—Li4—Li3 45.89 (8)
O10i—Li2—Li4 83.42 (9) O10—Li4—Li3 117.05 (12)
S2—Li2—Li4 92.49 (8) Li4i—Li4—Li3 94.23 (13)
Li4i—Li2—Li4 44.29 (9) S3—Li4—Li3 61.84 (7)
Li3—Li2—Li4 49.14 (7) Li2i—Li4—Li3 164.31 (14)
Si2—Li2—Li4 130.99 (9) O11i—Li4—Li2 93.49 (9)
Si2—S2—Li1 157.74 (7) O10—Li4—Li2 142.91 (12)
Li3—S2—Li1 76.20 (8) Li4i—Li4—Li2 47.33 (9)
Si2—S2—Li2 73.72 (6) S3—Li4—Li2 97.37 (8)
Li3—S2—Li2 64.37 (8) Li2i—Li4—Li2 135.71 (9)
Li1—S2—Li2 88.75 (8) Li3—Li4—Li2 48.96 (7)
O5—Si2—O6 105.18 (6) O11i—Li4—Li1 105.44 (11)
O5—Si2—O4 105.08 (6) O11—Li4—Li1 81.26 (9)
O6—Si2—O4 111.00 (6) O10—Li4—Li1 148.13 (11)
O5—Si2—S2 115.78 (5) Li4i—Li4—Li1 95.20 (13)
O6—Si2—S2 115.88 (5) S3—Li4—Li1 45.33 (6)
O4—Si2—S2 103.49 (4) Li2i—Li4—Li1 137.98 (12)
O5—Si2—Li2 127.79 (7) Li3—Li4—Li1 57.25 (8)
O6—Si2—Li2 123.10 (7) Li2—Li4—Li1 61.11 (7)
O4—Si2—Li2 42.41 (6) Li2i—O10—Li4 80.25 (10)
S2—Si2—Li2 61.54 (6) Li2i—O10—H10B 110.3
C16—O4—Si2 131.38 (9) Li4—O10—H10B 106.7
C16—O4—Li2 125.52 (11) Li2i—O10—H10A 140.8
Si2—O4—Li2 102.52 (9) Li4—O10—H10A 104.2
C16—C13—H13A 109.5 H10B—O10—H10A 105.6
C16—C13—H13B 109.4 C51—C56—C55 124.6 (6)
H13A—C13—H13B 109.5 C51—C56—H56A 116.9
C16—C13—H13C 109.5 C55—C56—H56A 118.1
H13A—C13—H13C 109.5 C53—C52—C51 122.1 (6)
H13B—C13—H13C 109.5 C53—C52—H52A 116.5
C16—C14—H14A 109.6 C51—C52—H52A 120.4
C16—C14—H14B 109.4 C56—C55—C54 118.6 (6)
H14A—C14—H14B 109.5 C56—C55—H55A 120.3
C16—C14—H14C 109.5 C54—C55—H55A 120.9
H14A—C14—H14C 109.5 C56—C51—C52 116.7 (6)
H14B—C14—H14C 109.5 C56—C51—C50 123.1 (8)
C16—C15—H15A 109.4 C52—C51—C50 120.2 (8)
C16—C15—H15B 109.5 C53—C54—C55 116.6 (6)
H15A—C15—H15B 109.5 C53—C54—H54A 122.9
C16—C15—H15C 109.5 C55—C54—H54A 119.2
H15A—C15—H15C 109.5 C52—C53—C54 120.6 (6)
H15B—C15—H15C 109.5 C52—C53—H53A 120.8
O4—C16—C13 107.76 (14) C54—C53—H53A 117.2
O4—C16—C14 104.96 (13) C51—C50—H50A 111.6
C13—C16—C14 111.91 (18) C51—C50—H50B 109.5
O4—C16—C15 110.75 (15) H50A—C50—H50B 109.5
C13—C16—C15 111.21 (17) C51—C50—H50C 107.3
C14—C16—C15 110.06 (16) H50A—C50—H50C 109.5
C18—O5—Si2 132.72 (12) H50B—C50—H50C 109.5
C18—C17—H17A 109.2 C60—C61—C66 118.2 (10)
C18—C17—H17B 109.6 C60—C61—C62 121.4 (10)
H17A—C17—H17B 109.5 C66—C61—C62 120.3 (6)
C18—C17—H17C 109.6 C61—C62—C63 119.1 (6)
H17B—C17—H17C 109.5 C63—C62—H62A 113.3
O5—C18—C20 109.26 (16) C66—C65—C64 120.2 (7)
O5—C18—C17 105.35 (18) C66—C65—H65A 113.3
C20—C18—C17 111.7 (3) C64—C65—H65A 126.4
O5—C18—C19 109.34 (17) C65—C64—C63 118.7 (7)
C20—C18—C19 112.3 (3) C65—C64—H64A 113.5
C17—C18—C19 108.6 (2) C63—C64—H64A 127.8
C18—C19—H19A 109.5 C65—C66—C61 120.2 (7)
C18—C19—H19B 109.5 C65—C66—H66A 125.4
H19A—C19—H19B 109.5 C61—C66—H66A 113.4
C18—C19—H19C 109.5 C62—C63—C64 120.0 (7)
H19A—C19—H19C 109.5 C62—C63—H63A 126.2
H19B—C19—H19C 109.5 C64—C63—H63A 113.4
C18—C20—H20A 109.4 C61—C60—H60A 119.5
C18—C20—H20B 109.5 C61—C60—H60B 101.6
H20A—C20—H20B 109.5 H60A—C60—H60B 109.5
C18—C20—H20C 109.6 C61—C60—H60C 106.8
H20A—C20—H20C 109.5 H60A—C60—H60C 109.5
H20B—C20—H20C 109.5 H60B—C60—H60C 109.5
