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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016987/bt6192sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016987/bt6192Isup2.hkl
Contains datablock I

CCDC reference: 198311

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](C-C) = 0.003 Å
  • Disorder in solvent or counterion
  • R factor = 0.036
  • wR factor = 0.105
  • Data-to-parameter ratio = 17.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_213 Alert C Atom C20 has ADP max/min Ratio ........... 3.20 prolate PLAT_302 Alert C Anion/Solvent Disorder ....................... 50.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check

Comment top

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.

Experimental top

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.

Refinement top

H atoms were located in the difference Fourier maps, then positioned geometrically and allowed to ride on their respective parent atoms. [Please alter this added text as required]

Computing details top

Data collection: XSCANS (Bruker, 1999); cell refinement: XSCANS; data reduction: SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: RESVIEW (Schwenk, 1998); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 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) top
Crystal data top
[Li8(C12H27O3SSi)6(OH)2(H2O)2]·2C7H8F(000) = 2160
Mr = 1986.7Dx = 1.083 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8000 reflections
a = 13.088 (3) Åθ = 4.1–26.1°
b = 27.188 (5) ŵ = 0.23 mm1
c = 17.525 (4) ÅT = 200 K
β = 102.25 (3)°Thick plate, colourless
V = 6094 (2) Å30.6 × 0.3 × 0.2 mm
Z = 2
Data collection top
Bruker IPDS
diffractometer
10031 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.035
Graphite monochromatorθmax = 25.9°, θmin = 2.2°
area IPDS scansh = 1616
47490 measured reflectionsk = 3333
11732 independent reflectionsl = 2121
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0696P)2 + 0.8026P]
where P = (Fo2 + 2Fc2)/3
11732 reflections(Δ/σ)max = 0.030
669 parametersΔρmax = 0.32 e Å3
31 restraintsΔρmin = 0.24 e Å3
Crystal data top
[Li8(C12H27O3SSi)6(OH)2(H2O)2]·2C7H8V = 6094 (2) Å3
Mr = 1986.7Z = 2
Monoclinic, P21/nMo Kα radiation
a = 13.088 (3) ŵ = 0.23 mm1
b = 27.188 (5) ÅT = 200 K
c = 17.525 (4) Å0.6 × 0.3 × 0.2 mm
β = 102.25 (3)°
Data collection top
Bruker IPDS
diffractometer
10031 reflections with I > 2σ(I)
47490 measured reflectionsRint = 0.035
11732 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03631 restraints
wR(F2) = 0.105H-atom parameters constrained
S = 1.04Δρmax = 0.32 e Å3
11732 reflectionsΔρmin = 0.24 e Å3
669 parameters
Special details top

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) top
xyzUiso*/UeqOcc. (<1)
Li10.3540 (2)0.09614 (9)0.85630 (15)0.0426 (6)
S10.40258 (3)0.116879 (14)0.99526 (2)0.03868 (10)
Si10.32191 (3)0.177407 (13)0.94425 (2)0.03116 (9)
O10.22702 (9)0.19555 (4)0.98355 (7)0.0467 (3)
C10.0663 (2)0.20629 (16)1.0186 (2)0.1283 (14)
H1A0.03240.21140.96500.192*
H1B0.01680.19331.04670.192*
H1C0.09300.23711.04130.192*
C20.20943 (19)0.16138 (10)1.10654 (12)0.0758 (6)
H2A0.23140.19221.13150.114*
H2B0.16190.14541.13340.114*
H2C0.26940.14081.10800.114*
C30.15570 (15)0.17040 (9)1.02280 (13)0.0640 (5)
C40.1189 (2)0.12246 (12)0.98174 (17)0.0934 (9)
H4A0.08410.12910.92880.140*
H4B0.17810.10150.98200.140*
H4C0.07140.10641.00850.140*
O20.27772 (8)0.15869 (4)0.85295 (5)0.0370 (2)
C50.3049 (2)0.20371 (9)0.74205 (13)0.0817 (7)
H5A0.34590.22850.77360.123*
H5B0.34950.17710.73370.123*
H5C0.27170.21760.69260.123*
C60.22176 (15)0.18467 (6)0.78369 (9)0.0495 (4)
C70.1533 (2)0.14649 (9)0.73574 (14)0.0888 (9)
H7A0.10100.13580.76310.133*
H7B0.11990.16040.68640.133*
H7C0.19520.11890.72720.133*
C80.15867 (19)0.22711 (8)0.80483 (13)0.0739 (6)
H8A0.10640.21480.83100.111*
H8B0.20410.24930.83880.111*
H8C0.12540.24420.75820.111*
O30.38847 (9)0.22686 (4)0.93626 (6)0.0443 (3)
C90.5279 (5)0.2825 (2)0.9591 (3)0.103 (3)0.623 (8)
H9A0.58340.25910.96170.155*0.623 (8)
H9B0.49990.29100.90560.155*0.623 (8)
H9C0.55450.31150.98780.155*0.623 (8)
C9A0.5593 (5)0.2440 (4)1.0107 (8)0.127 (6)0.377 (8)
H9D0.58520.24130.96360.191*0.377 (8)
H9E0.56030.21211.03460.191*0.377 (8)
H9F0.60270.26611.04610.191*0.377 (8)
C100.44020 (16)0.26206 (6)0.99196 (11)0.0545 (4)
C110.3531 (6)0.30315 (18)0.9860 (3)0.0972 (18)0.623 (8)
H11A0.29020.29651.00410.146*0.623 (8)
H11B0.38840.33081.01400.146*0.623 (8)
H11C0.33580.31050.93120.146*0.623 (8)
C11A0.4273 (11)0.3123 (3)0.9692 (5)0.110 (5)0.377 (8)
H11D0.35800.32570.95640.165*0.377 (8)
H11E0.45640.31170.92330.165*0.377 (8)
H11F0.47030.33221.00850.165*0.377 (8)
C120.4697 (6)0.2422 (2)1.0705 (3)0.083 (2)0.623 (8)
H12A0.51710.21481.07820.124*0.623 (8)
H12B0.49830.26841.10520.124*0.623 (8)
H12C0.40380.23211.08110.124*0.623 (8)
C12A0.4148 (11)0.2567 (6)1.0751 (7)0.106 (5)0.377 (8)
H12D0.34380.26791.06780.080*0.377 (8)
H12E0.41990.22381.09580.080*0.377 (8)
H12F0.45950.27811.11100.080*0.377 (8)
Li20.61825 (19)0.05337 (9)0.91064 (13)0.0358 (5)
S20.49948 (3)0.083604 (13)0.78254 (2)0.03587 (9)
Si20.64987 (3)0.083239 (14)0.76353 (2)0.03103 (10)
O40.71906 (7)0.05744 (4)0.84372 (5)0.0335 (2)
C130.81269 (17)0.01748 (8)0.83322 (16)0.0751 (6)
H13A0.76650.03460.85990.113*
H13B0.88020.03290.84450.113*
H13C0.78470.01850.77800.113*
C140.86042 (15)0.03943 (10)0.94834 (11)0.0662 (6)
H14A0.81440.02100.97360.099*
H14B0.86030.07330.96370.099*
H14C0.93000.02650.96340.099*
C150.89667 (14)0.06402 (9)0.81966 (12)0.0640 (5)
H15A0.90180.09740.83780.096*
H15B0.86980.06350.76430.096*
H15C0.96470.04910.83130.096*
C160.82336 (12)0.03555 (7)0.86037 (9)0.0445 (4)
O50.66903 (9)0.04873 (4)0.69258 (6)0.0417 (2)
C170.6687 (3)0.00699 (11)0.57554 (15)0.1148 (12)
H17A0.73960.00310.59580.172*
H17B0.65660.00920.51970.172*
H17C0.62170.01670.58990.172*
C180.65093 (16)0.05613 (8)0.60875 (9)0.0566 (5)
C190.7305 (3)0.09155 (13)0.59065 (14)0.1177 (13)
H19A0.80090.07890.61180.177*
H19B0.72210.12350.61440.177*
H19C0.72050.09540.53390.177*
C200.5422 (3)0.07361 (19)0.57973 (13)0.1398 (17)
H20A0.53290.10450.60390.210*
H20B0.49410.04990.59250.210*
H20C0.52930.07780.52410.210*
O60.69754 (9)0.13643 (4)0.74817 (6)0.0450 (3)
C210.6068 (2)0.21254 (9)0.7494 (2)0.1012 (9)
H21A0.54870.19760.76600.152*
H21B0.59470.21190.69350.152*
H21C0.61420.24600.76730.152*
C220.7224 (2)0.18048 (9)0.87132 (13)0.0830 (7)
H22A0.66220.16570.88520.124*
H22B0.73320.21270.89400.124*
H22C0.78280.16050.89050.124*
C230.7989 (2)0.20821 (9)0.75963 (18)0.0921 (9)
H23A0.78630.21090.70380.138*
H23B0.85970.18820.77780.138*
H23C0.81020.24040.78250.138*
C240.70470 (17)0.18452 (7)0.78309 (11)0.0564 (4)
Li30.46363 (18)0.00101 (9)0.82350 (13)0.0331 (5)
S30.27493 (3)0.011720 (12)0.853421 (18)0.03073 (9)
Si30.27025 (3)0.050209 (13)0.784603 (19)0.02714 (9)
O70.18441 (8)0.05102 (4)0.70316 (5)0.0367 (2)
C250.23262 (18)0.01956 (8)0.63263 (11)0.0650 (5)
H25A0.28740.00090.61770.097*
H25B0.25990.03650.68070.097*
H25C0.20550.04300.59250.097*
C260.10487 (19)0.04469 (9)0.56998 (10)0.0722 (6)
H26A0.05060.06640.57850.108*
H26B0.16100.06360.55740.108*
H26C0.07740.02290.52760.108*
C270.14567 (14)0.01485 (6)0.64379 (9)0.0476 (4)
C280.05776 (16)0.01324 (8)0.66865 (12)0.0651 (5)
H28A0.00440.00940.67610.098*
H28B0.02850.03660.62890.098*
H28C0.08480.03030.71670.098*
O80.24940 (7)0.10048 (4)0.83109 (5)0.0326 (2)
C290.18610 (16)0.16786 (7)0.89315 (11)0.0580 (5)
H29A0.20190.15100.94240.087*
H29B0.24640.18600.88620.087*
H29C0.12890.19010.89230.087*
C300.12976 (15)0.15707 (7)0.74931 (11)0.0552 (4)
H30A0.11000.13350.70810.083*
H30B0.07280.17940.74900.083*
H30C0.18980.17510.74160.083*
C310.15624 (12)0.13053 (6)0.82741 (9)0.0393 (3)
C320.06662 (13)0.09771 (8)0.83899 (11)0.0542 (4)
H32A0.04970.07480.79640.081*
H32B0.08710.08000.88720.081*
H32C0.00650.11760.84070.081*
O90.39054 (7)0.05571 (3)0.76993 (5)0.0309 (2)
C330.44418 (12)0.09355 (6)0.73312 (8)0.0377 (3)
C340.45868 (18)0.13913 (7)0.78346 (12)0.0625 (5)
H34A0.39170.15360.78320.094*
H34B0.49190.13050.83600.094*
H34C0.50160.16230.76320.094*
C350.3822 (2)0.10533 (11)0.65305 (12)0.0934 (10)
H35A0.37530.07630.62120.140*
H35B0.31400.11680.65680.140*
H35C0.41740.13040.63000.140*
C360.5494 (2)0.07117 (9)0.7327 (2)0.1045 (11)
H36A0.54040.04230.70030.157*
H36B0.59180.09460.71260.157*
H36C0.58320.06230.78500.157*
O110.54664 (7)0.00555 (3)0.92782 (5)0.0303 (2)
H11G0.58070.03500.93240.036*
Li40.41519 (19)0.01426 (10)0.96272 (13)0.0369 (5)
O100.37146 (8)0.08350 (4)0.98571 (5)0.0354 (2)
H10B0.42210.10140.98580.043*
H10A0.32460.09180.94370.043*
C560.2680 (8)0.3710 (4)1.0311 (4)0.107 (4)0.639 (7)
H56A0.32110.39371.02340.128*0.639 (7)
C520.1793 (7)0.3331 (3)1.1145 (5)0.112 (4)0.639 (7)
H52A0.17360.32311.16600.134*0.639 (7)
C550.1985 (7)0.3535 (3)0.9657 (3)0.130 (3)0.639 (7)
H55A0.20150.36550.91470.156*0.639 (7)
C510.2606 (3)0.36238 (14)1.1041 (2)0.0735 (14)0.639 (7)
C540.1203 (11)0.3204 (6)0.9762 (6)0.217 (10)0.639 (7)
H54A0.08370.30170.93230.261*0.639 (7)
C530.1151 (6)0.3095 (2)1.0533 (6)0.154 (4)0.639 (7)
H53A0.05550.29121.06120.185*0.639 (7)
C500.3302 (10)0.3822 (4)1.1690 (8)0.154 (5)0.639 (7)
H50A0.37990.40391.15350.185*0.639 (7)
H50B0.36660.35591.20010.185*0.639 (7)
H50C0.28930.40011.19910.185*0.639 (7)
C610.1943 (5)0.3371 (2)1.0309 (4)0.076 (2)0.361 (7)
C620.2022 (10)0.3247 (4)1.1085 (5)0.082 (4)0.361 (7)
H62A0.15770.30221.12850.099*0.361 (7)
C650.3262 (9)0.3986 (5)1.0674 (9)0.158 (6)0.361 (7)
H65A0.36830.42191.04640.189*0.361 (7)
C640.3325 (12)0.3882 (6)1.1460 (8)0.162 (11)0.361 (7)
H64A0.38690.40601.18040.194*0.361 (7)
C660.2529 (11)0.3753 (6)1.0108 (7)0.082 (4)0.361 (7)
H66A0.24640.37880.95550.098*0.361 (7)
C630.2631 (11)0.3538 (4)1.1661 (5)0.161 (9)0.361 (7)
H63A0.26890.35071.22140.193*0.361 (7)
C600.1290 (11)0.3143 (6)0.9750 (8)0.152 (11)0.361 (7)
H60A0.13060.32120.92150.182*0.361 (7)
H60B0.06270.32420.98500.182*0.361 (7)
H60C0.13870.27970.98460.182*0.361 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Li10.0554 (15)0.0323 (13)0.0399 (13)0.0066 (11)0.0095 (11)0.0004 (10)
S10.0467 (2)0.03331 (19)0.03350 (18)0.00866 (14)0.00288 (14)0.00498 (14)
Si10.0369 (2)0.02489 (19)0.03067 (18)0.00222 (14)0.00480 (14)0.00117 (14)
O10.0477 (6)0.0445 (6)0.0511 (6)0.0094 (5)0.0172 (5)0.0017 (5)
C10.0781 (18)0.184 (4)0.139 (3)0.059 (2)0.0608 (19)0.035 (3)
C20.0828 (15)0.0961 (17)0.0571 (12)0.0112 (13)0.0338 (11)0.0020 (11)
C30.0467 (10)0.0839 (15)0.0675 (12)0.0021 (9)0.0256 (9)0.0036 (11)
C40.0702 (14)0.119 (2)0.0908 (17)0.0498 (15)0.0165 (13)0.0055 (16)
O20.0488 (6)0.0268 (5)0.0310 (5)0.0068 (4)0.0012 (4)0.0020 (4)
C50.123 (2)0.0666 (14)0.0573 (12)0.0170 (14)0.0226 (13)0.0276 (11)
C60.0704 (11)0.0343 (8)0.0355 (8)0.0130 (7)0.0076 (7)0.0062 (6)
C70.115 (2)0.0562 (13)0.0671 (13)0.0044 (12)0.0431 (13)0.0010 (10)
C80.0909 (15)0.0583 (12)0.0607 (12)0.0364 (11)0.0105 (11)0.0055 (10)
O30.0576 (6)0.0346 (6)0.0383 (5)0.0104 (5)0.0047 (5)0.0018 (4)
C90.114 (4)0.097 (5)0.100 (3)0.071 (4)0.025 (3)0.020 (3)
C9A0.055 (4)0.118 (8)0.190 (12)0.010 (4)0.013 (5)0.069 (9)
C100.0749 (12)0.0345 (9)0.0514 (9)0.0173 (8)0.0076 (8)0.0056 (7)
C110.138 (5)0.039 (2)0.106 (4)0.009 (3)0.008 (3)0.028 (2)
C11A0.178 (13)0.038 (3)0.084 (5)0.021 (5)0.040 (7)0.006 (3)
C120.124 (5)0.058 (3)0.049 (3)0.035 (3)0.023 (3)0.003 (2)
C12A0.148 (11)0.119 (11)0.050 (4)0.067 (8)0.019 (7)0.030 (6)
Li20.0423 (12)0.0407 (13)0.0249 (10)0.0063 (10)0.0083 (9)0.0025 (9)
S20.03889 (18)0.0361 (2)0.03430 (18)0.00290 (14)0.01155 (14)0.00878 (13)
Si20.0395 (2)0.0319 (2)0.02289 (17)0.00335 (14)0.00937 (14)0.00161 (13)
O40.0338 (5)0.0408 (5)0.0265 (4)0.0010 (4)0.0074 (4)0.0028 (4)
C130.0572 (11)0.0561 (12)0.1077 (18)0.0179 (9)0.0077 (11)0.0129 (12)
C140.0496 (10)0.0977 (17)0.0458 (10)0.0152 (10)0.0023 (8)0.0112 (10)
C150.0399 (9)0.0935 (16)0.0617 (11)0.0046 (9)0.0175 (8)0.0007 (11)
C160.0351 (7)0.0546 (10)0.0427 (8)0.0049 (7)0.0057 (6)0.0010 (7)
O50.0534 (6)0.0485 (6)0.0254 (5)0.0020 (5)0.0132 (4)0.0036 (4)
C170.205 (4)0.097 (2)0.0536 (13)0.010 (2)0.0549 (18)0.0322 (13)
C180.0717 (12)0.0769 (13)0.0236 (7)0.0062 (10)0.0160 (7)0.0056 (7)
C190.185 (3)0.136 (3)0.0477 (12)0.068 (2)0.0595 (17)0.0106 (14)
C200.110 (2)0.272 (5)0.0300 (11)0.064 (3)0.0017 (12)0.0087 (18)
O60.0615 (7)0.0385 (6)0.0381 (5)0.0130 (5)0.0177 (5)0.0027 (4)
C210.111 (2)0.0484 (13)0.141 (3)0.0088 (13)0.0205 (19)0.0104 (15)
C220.138 (2)0.0557 (13)0.0602 (13)0.0218 (14)0.0329 (13)0.0199 (10)
C230.117 (2)0.0616 (14)0.110 (2)0.0461 (14)0.0507 (17)0.0121 (13)
C240.0793 (12)0.0356 (9)0.0576 (10)0.0151 (8)0.0222 (9)0.0000 (7)
Li30.0401 (12)0.0319 (12)0.0273 (10)0.0046 (9)0.0070 (9)0.0001 (9)
S30.03661 (17)0.02851 (17)0.02649 (16)0.00068 (12)0.00538 (12)0.00316 (12)
Si30.03171 (18)0.02737 (19)0.02110 (16)0.00053 (13)0.00282 (13)0.00070 (13)
O70.0421 (5)0.0377 (6)0.0257 (5)0.0010 (4)0.0030 (4)0.0007 (4)
C250.0942 (15)0.0581 (12)0.0446 (9)0.0119 (10)0.0190 (10)0.0216 (8)
C260.0889 (15)0.0843 (15)0.0301 (8)0.0292 (12)0.0174 (9)0.0087 (9)
C270.0586 (10)0.0513 (10)0.0267 (7)0.0171 (8)0.0046 (6)0.0017 (6)
C280.0608 (11)0.0719 (13)0.0556 (11)0.0279 (10)0.0035 (9)0.0065 (9)
O80.0352 (5)0.0305 (5)0.0306 (5)0.0060 (4)0.0036 (4)0.0017 (4)
C290.0662 (11)0.0489 (10)0.0597 (11)0.0181 (9)0.0149 (9)0.0119 (8)
C300.0658 (11)0.0455 (10)0.0528 (10)0.0198 (8)0.0092 (8)0.0152 (8)
C310.0400 (7)0.0371 (8)0.0412 (8)0.0125 (6)0.0094 (6)0.0025 (6)
C320.0433 (9)0.0667 (12)0.0557 (10)0.0061 (8)0.0175 (7)0.0050 (9)
O90.0363 (5)0.0285 (5)0.0288 (4)0.0004 (4)0.0086 (4)0.0038 (4)
C330.0430 (8)0.0365 (8)0.0356 (7)0.0052 (6)0.0123 (6)0.0064 (6)
C340.0822 (13)0.0476 (11)0.0596 (11)0.0225 (9)0.0194 (10)0.0018 (8)
C350.1144 (19)0.118 (2)0.0381 (10)0.0651 (17)0.0055 (11)0.0299 (12)
C360.0867 (17)0.0652 (14)0.192 (3)0.0145 (13)0.097 (2)0.0397 (18)
O110.0356 (5)0.0299 (5)0.0247 (4)0.0003 (4)0.0046 (4)0.0049 (3)
Li40.0403 (12)0.0463 (14)0.0227 (10)0.0090 (10)0.0032 (9)0.0044 (9)
O100.0374 (5)0.0398 (6)0.0272 (5)0.0013 (4)0.0027 (4)0.0003 (4)
C560.139 (8)0.112 (6)0.080 (4)0.045 (5)0.044 (5)0.030 (4)
C520.129 (6)0.060 (4)0.161 (8)0.047 (4)0.066 (5)0.025 (4)
C550.181 (7)0.134 (6)0.069 (3)0.037 (5)0.012 (4)0.005 (4)
C510.073 (3)0.061 (2)0.080 (3)0.0234 (19)0.0021 (18)0.0036 (18)
C540.247 (19)0.147 (14)0.25 (2)0.072 (12)0.037 (14)0.017 (12)
C530.141 (6)0.073 (4)0.232 (11)0.029 (4)0.002 (6)0.005 (5)
C500.163 (11)0.134 (10)0.141 (7)0.051 (7)0.019 (6)0.058 (6)
C610.084 (5)0.050 (4)0.089 (5)0.003 (3)0.006 (4)0.006 (3)
C620.106 (8)0.048 (5)0.102 (8)0.027 (6)0.043 (6)0.031 (5)
C650.116 (9)0.124 (11)0.217 (18)0.028 (8)0.001 (10)0.026 (12)
C640.078 (9)0.106 (11)0.27 (3)0.006 (7)0.043 (12)0.028 (15)
C660.079 (6)0.094 (8)0.067 (7)0.007 (5)0.003 (5)0.041 (6)
C630.25 (2)0.158 (14)0.058 (6)0.133 (15)0.011 (8)0.002 (7)
C600.176 (17)0.103 (12)0.121 (13)0.012 (11)0.092 (14)0.012 (9)
Geometric parameters (Å, º) top
Li1—O21.967 (3)C20—H20A0.9600
Li1—S12.449 (3)C20—H20B0.9600
Li1—S32.514 (3)C20—H20C0.9599
Li1—S22.541 (3)O6—C241.438 (2)
Li1—Si12.777 (3)C21—C241.500 (4)
Li1—Li33.070 (4)C21—H21A0.9600
Li1—Li43.535 (4)C21—H21B0.9602
S1—Si12.0546 (6)C21—H21C0.9602
Si1—O11.6196 (12)C22—C241.518 (3)
Si1—O31.6242 (11)C22—H22A0.9599
Si1—O21.6616 (11)C22—H22B0.9600
O1—C31.444 (2)C22—H22C0.9600
C1—C31.514 (3)C23—C241.523 (3)
C1—H1A0.9599C23—H23A0.9599
C1—H1B0.9600C23—H23B0.9600
C1—H1C0.9601C23—H23C0.9601
C2—C31.507 (3)Li3—O111.926 (2)
C2—H2A0.9600Li3—O91.948 (2)
C2—H2B0.9600Li3—S32.647 (2)
C2—H2C0.9599Li3—Li42.680 (3)
C3—C41.517 (4)Li3—Si32.842 (2)
C4—H4A0.9599S3—Si32.0644 (6)
C4—H4B0.9601S3—Li42.459 (2)
C4—H4C0.9600Si3—O71.6185 (11)
O2—C61.4600 (17)Si3—O81.6433 (10)
C5—C61.523 (3)Si3—O91.6549 (10)
C5—H5A0.9598O7—C271.4431 (18)
C5—H5B0.9601C25—C271.518 (3)
C5—H5C0.9599C25—H25A0.9600
C6—C71.506 (3)C25—H25B0.9602
C6—C81.510 (3)C25—H25C0.9600
C7—H7A0.9600C26—C271.524 (2)
C7—H7B0.9600C26—H26A0.9601
C7—H7C0.9598C26—H26B0.9601
C8—H8A0.9599C26—H26C0.9599
C8—H8B0.9599C27—C281.520 (2)
C8—H8C0.9600C28—H28A0.9600
O3—C101.431 (2)C28—H28B0.9600
C9—C101.495 (5)C28—H28C0.9600
C9—H9A0.9600O8—C311.4578 (16)
C9—H9B0.9600C29—C311.523 (2)
C9—H9C0.9600C29—H29A0.9601
C9A—C101.601 (8)C29—H29B0.9601
C9A—H9A1.0594C29—H29C0.9600
C9A—H9D0.9599C30—C311.521 (2)
C9A—H9E0.9600C30—H30A0.9599
C9A—H9F0.9600C30—H30B0.9599
C10—C11A1.422 (7)C30—H30C0.9599
C10—C121.452 (6)C31—C321.521 (2)
C10—C12A1.569 (11)C32—H32A0.9599
C10—C111.584 (5)C32—H32B0.9599
C11—H11A0.9600C32—H32C0.9601
C11—H11B0.9601O9—C331.4696 (16)
C11—H11C0.9600C33—C351.499 (2)
C11—H11D0.8151C33—C361.507 (3)
C11A—H11B1.1386C33—C341.510 (2)
C11A—H11C1.2418C34—H34A0.9601
C11A—H11D0.9600C34—H34B0.9601
C11A—H11E0.9599C34—H34C0.9600
C11A—H11F0.9601C35—H35A0.9600
C12—H12A0.9601C35—H35B0.9600
C12—H12B0.9598C35—H35C0.9600
C12—H12C0.9600C36—H36A0.9600
C12—H12E0.9962C36—H36B0.9598
C12—H12F1.2312C36—H36C0.9600
C12A—H12B1.1524O11—Li4i1.953 (2)
C12A—H12C0.6951O11—Li41.959 (3)
C12A—H12D0.9599O11—H11G0.9126
C12A—H12E0.9601Li4—O11i1.953 (2)
C12A—H12F0.9598Li4—O102.033 (3)
Li2—O111.912 (3)Li4—Li4i2.451 (5)
Li2—O41.945 (3)Li4—Li2i2.581 (3)
Li2—O10i1.971 (3)O10—Li2i1.971 (3)
Li2—S22.579 (2)O10—H10B0.8210
Li2—Li4i2.581 (3)O10—H10A0.8821
Li2—Li32.673 (3)C56—C511.324 (7)
Li2—Si22.816 (2)C56—C551.387 (7)
Li2—Li43.508 (3)C56—H56A0.9600
S2—Si22.0649 (7)C52—C531.372 (7)
S2—Li32.433 (2)C52—C511.372 (7)
Si2—O51.6191 (11)C52—H52A0.9601
Si2—O61.6201 (11)C55—C541.406 (8)
Si2—O41.6574 (11)C55—H55A0.9599
O4—C161.4608 (18)C51—C501.405 (10)
C13—C161.515 (3)C54—C531.399 (8)
C13—H13A0.9600C54—H54A0.9601
C13—H13B0.9599C53—H53A0.9600
C13—H13C0.9600C50—H50A0.9599
C14—C161.519 (2)C50—H50B0.9600
C14—H14A0.9600C50—H50C0.9601
C14—H14B0.9603C61—C601.311 (11)
C14—H14C0.9599C61—C661.381 (8)
C15—C161.523 (3)C61—C621.383 (8)
C15—H15A0.9600C62—C631.393 (8)
C15—H15B0.9599C62—H62A0.9599
C15—H15C0.9600C65—C661.379 (8)
O5—C181.4517 (18)C65—C641.392 (8)
C17—C181.495 (3)C65—H65A0.9601
C17—H17A0.9599C64—C631.399 (8)
C17—H17B0.9600C64—H64A0.9599
C17—H17C0.9600C66—H56A1.0062
C18—C201.484 (4)C66—H66A0.9600
C18—C191.501 (3)C63—H63A0.9600
C19—H19A0.9800C60—H60A0.9601
C19—H19B0.9800C60—H60B0.9600
C19—H19C0.9800C60—H60C0.9600
O2—Li1—S181.57 (9)C24—O6—Si2137.17 (10)
O2—Li1—S3125.76 (14)C24—C21—H21A109.4
S1—Li1—S3104.42 (10)C24—C21—H21B109.6
O2—Li1—S2122.10 (12)H21A—C21—H21B109.5
S1—Li1—S2118.20 (11)C24—C21—H21C109.5
S3—Li1—S2102.54 (9)H21A—C21—H21C109.5
O2—Li1—Si136.17 (5)H21B—C21—H21C109.4
S1—Li1—Si145.77 (5)C24—C22—H22A109.4
S3—Li1—Si1128.86 (11)C24—C22—H22B109.5
S2—Li1—Si1127.39 (11)H22A—C22—H22B109.5
O2—Li1—Li3167.76 (13)C24—C22—H22C109.5
S1—Li1—Li3110.32 (10)H22A—C22—H22C109.5
S3—Li1—Li355.53 (7)H22B—C22—H22C109.5
S2—Li1—Li350.32 (6)C24—C23—H23A109.5
Si1—Li1—Li3154.96 (11)C24—C23—H23B109.4
O2—Li1—Li4143.77 (12)H23A—C23—H23B109.5
S1—Li1—Li471.87 (7)C24—C23—H23C109.5
S3—Li1—Li444.07 (6)H23A—C23—H23C109.5
S2—Li1—Li492.54 (8)H23B—C23—H23C109.5
Si1—Li1—Li4115.26 (9)O6—C24—C21108.74 (19)
Li3—Li1—Li447.23 (7)O6—C24—C22110.46 (15)
Si1—S1—Li175.57 (6)C21—C24—C22111.7 (2)
O1—Si1—O3104.97 (6)O6—C24—C23104.65 (17)
O1—Si1—O2111.17 (6)C21—C24—C23110.6 (2)
O3—Si1—O2104.71 (6)C22—C24—C23110.4 (2)
O1—Si1—S1115.38 (5)O11—Li3—O9120.30 (13)
O3—Si1—S1117.71 (5)O11—Li3—S2105.08 (10)
O2—Si1—S1102.44 (4)O9—Li3—S2133.96 (11)
O1—Si1—Li1134.31 (8)O11—Li3—S3100.61 (9)
O3—Si1—Li1117.62 (7)O9—Li3—S378.42 (8)
S1—Si1—Li158.65 (6)S2—Li3—S3101.73 (9)
C3—O1—Si1133.63 (12)O11—Li3—Li245.64 (8)
C3—C1—H1A109.4O9—Li3—Li2158.76 (14)
C3—C1—H1B109.6S2—Li3—Li260.46 (7)
H1A—C1—H1B109.5S3—Li3—Li2116.96 (10)
C3—C1—H1C109.4O11—Li3—Li446.88 (7)
H1A—C1—H1C109.5O9—Li3—Li497.43 (10)
H1B—C1—H1C109.5S2—Li3—Li4120.61 (11)
C3—C2—H2A109.6S3—Li3—Li454.97 (7)
C3—C2—H2B109.5Li2—Li3—Li481.90 (9)
H2A—C2—H2B109.5O11—Li3—Si3118.46 (10)
C3—C2—H2C109.3O9—Li3—Si334.43 (5)
H2A—C2—H2C109.5S2—Li3—Si3126.80 (9)
H2B—C2—H2C109.5S3—Li3—Si344.00 (4)
O1—C3—C2109.01 (16)Li2—Li3—Si3157.80 (10)
O1—C3—C1104.0 (2)Li4—Li3—Si376.81 (8)
C2—C3—C1110.4 (2)O11—Li3—Li195.28 (10)
O1—C3—C4110.67 (17)O9—Li3—Li1123.78 (12)
C2—C3—C4111.0 (2)S2—Li3—Li153.47 (7)
C1—C3—C4111.5 (2)S3—Li3—Li151.52 (7)
C3—C4—H4A109.5Li2—Li3—Li176.79 (10)
C3—C4—H4B109.4Li4—Li3—Li175.52 (10)
H4A—C4—H4B109.5Si3—Li3—Li191.72 (9)
C3—C4—H4C109.5Si3—S3—Li498.36 (6)
H4A—C4—H4C109.5Si3—S3—Li1135.83 (6)
H4B—C4—H4C109.5Li4—S3—Li190.60 (9)
C6—O2—Si1131.54 (10)Si3—S3—Li373.01 (5)
C6—O2—Li1127.24 (12)Li4—S3—Li363.19 (8)
Si1—O2—Li199.51 (9)Li1—S3—Li372.95 (8)
C6—C5—H5A109.4O7—Si3—O8105.59 (5)
C6—C5—H5B109.6O7—Si3—O9111.53 (6)
H5A—C5—H5B109.5O8—Si3—O9105.39 (5)
C6—C5—H5C109.4O7—Si3—S3117.08 (4)
H5A—C5—H5C109.5O8—Si3—S3112.09 (4)
H5B—C5—H5C109.5O9—Si3—S3104.67 (4)
O2—C6—C7105.34 (14)O7—Si3—Li3129.38 (6)
O2—C6—C8111.69 (14)O8—Si3—Li3121.44 (6)
C7—C6—C8111.84 (19)O9—Si3—Li341.71 (6)
O2—C6—C5106.22 (15)S3—Si3—Li362.99 (5)
C7—C6—C5111.6 (2)C27—O7—Si3134.31 (10)
C8—C6—C5109.96 (18)C27—C25—H25A109.5
C6—C7—H7A109.4C27—C25—H25B109.5
C6—C7—H7B109.5H25A—C25—H25B109.5
H7A—C7—H7B109.5C27—C25—H25C109.5
C6—C7—H7C109.5H25A—C25—H25C109.5
H7A—C7—H7C109.5H25B—C25—H25C109.5
H7B—C7—H7C109.5C27—C26—H26A109.5
C6—C8—H8A109.5C27—C26—H26B109.4
C6—C8—H8B109.5H26A—C26—H26B109.5
H8A—C8—H8B109.5C27—C26—H26C109.5
C6—C8—H8C109.5H26A—C26—H26C109.5
H8A—C8—H8C109.5H26B—C26—H26C109.5
H8B—C8—H8C109.5O7—C27—C25110.77 (14)
C10—O3—Si1132.82 (10)O7—C27—C28107.89 (14)
C10—C9—H9A111.7C25—C27—C28111.16 (17)
C10—C9—H9B107.5O7—C27—C26104.80 (14)
H9A—C9—H9B109.5C25—C27—C26110.86 (17)
C10—C9—H9C109.1C28—C27—C26111.13 (16)
H9A—C9—H9C109.5C27—C28—H28A109.5
H9B—C9—H9C109.5C27—C28—H28B109.5
C10—C9—H9D97.7H28A—C28—H28B109.5
C10—C9—H11E83.1C27—C28—H28C109.5
C10—C9A—H9A99.1H28A—C28—H28C109.5
C10—C9A—H9D110.7H28B—C28—H28C109.5
C10—C9A—H9E106.8C31—O8—Si3132.02 (9)
C10—C9A—H9F110.9C31—C29—H29A109.5
H9D—C9A—H9F109.5C31—C29—H29B109.4
H9E—C9A—H9F109.5H29A—C29—H29B109.5
C11A—C10—O3116.1 (3)C31—C29—H29C109.5
C11A—C10—C12127.9 (4)H29A—C29—H29C109.5
O3—C10—C12112.9 (3)H29B—C29—H29C109.5
C11A—C10—C965.8 (6)C31—C30—H30A109.5
O3—C10—C9106.1 (2)C31—C30—H30B109.5
C12—C10—C9115.6 (4)H30A—C30—H30B109.5
C11A—C10—C12A108.3 (7)C31—C30—H30C109.4
O3—C10—C12A114.1 (5)H30A—C30—H30C109.5
C9—C10—C12A136.3 (5)H30B—C30—H30C109.5
O3—C10—C11101.4 (2)O8—C31—C30109.55 (12)
C12—C10—C11111.6 (4)O8—C31—C32109.07 (13)
C9—C10—C11108.2 (4)C30—C31—C32111.32 (14)
C12A—C10—C1180.5 (6)O8—C31—C29105.19 (12)
C11A—C10—C9A113.9 (7)C30—C31—C29109.72 (15)
O3—C10—C9A103.5 (3)C32—C31—C29111.80 (14)
C12—C10—C9A68.9 (6)C31—C32—H32A109.5
C9—C10—C9A53.1 (5)C31—C32—H32B109.4
C12A—C10—C9A99.7 (7)H32A—C32—H32B109.5
C11—C10—C9A152.4 (4)C31—C32—H32C109.5
C10—C11—H11A120.0H32A—C32—H32C109.5
C10—C11—H11B104.8H32B—C32—H32C109.5
H11A—C11—H11B109.5C33—O9—Si3133.66 (9)
C10—C11—H11C103.1C33—O9—Li3122.30 (11)
H11A—C11—H11C109.5Si3—O9—Li3103.86 (8)
H11B—C11—H11C109.5O9—C33—C35110.25 (13)
C10—C11—H11D114.9O9—C33—C36103.99 (13)
C10—C11A—H11B106.0C35—C33—C36113.3 (2)
C10—C11A—H11C99.1O9—C33—C34109.31 (12)
H11B—C11A—H11C82.3C35—C33—C34110.35 (18)
C10—C11A—H11D118.8C36—C33—C34109.43 (19)
C10—C11A—H11E100.1C33—C34—H34A109.4
H11D—C11A—H11E109.5C33—C34—H34B109.5
C10—C11A—H11F108.9H34A—C34—H34B109.5
H11D—C11A—H11F109.5C33—C34—H34C109.5
H11E—C11A—H11F109.5H34A—C34—H34C109.5
C10—C12—H12A117.1H34B—C34—H34C109.5
C10—C12—H12B108.3C33—C35—H35A109.5
H12A—C12—H12B109.5C33—C35—H35B109.4
C10—C12—H12C102.7H35A—C35—H35B109.5
H12A—C12—H12C109.5C33—C35—H35C109.5
H12B—C12—H12C109.5H35A—C35—H35C109.5
C10—C12—H12E122.7H35B—C35—H35C109.5
C10—C12—H12F102.2C33—C36—H36A109.6
C10—C12A—H12B91.8C33—C36—H36B109.5
C10—C12A—H12C108.7H36A—C36—H36B109.5
H12B—C12A—H12C113.8C33—C36—H36C109.4
C10—C12A—H12D103.6H36A—C36—H36C109.5
C10—C12A—H12E115.2H36B—C36—H36C109.5
H12D—C12A—H12E109.5Li2—O11—Li388.26 (10)
C10—C12A—H12F109.4Li2—O11—Li4i83.78 (10)
H12D—C12A—H12F109.5Li3—O11—Li4i151.88 (12)
H12E—C12A—H12F109.5Li2—O11—Li4130.01 (12)
O11—Li2—O4124.08 (14)Li3—O11—Li487.23 (10)
O11—Li2—O10i98.23 (10)Li4i—O11—Li477.59 (11)
O4—Li2—O10i127.55 (13)Li2—O11—H11G120.2
O11—Li2—S2100.31 (10)Li3—O11—H11G109.3
O4—Li2—S279.50 (8)Li4i—O11—H11G97.9
O10i—Li2—S2125.48 (12)Li4—O11—H11G108.2
O11—Li2—Li4i48.78 (8)O11i—Li4—O11102.41 (11)
O4—Li2—Li4i143.35 (14)O11i—Li4—O1094.87 (10)
O10i—Li2—Li4i50.92 (8)O11—Li4—O10118.48 (14)
S2—Li2—Li4i134.35 (11)O11i—Li4—Li4i51.31 (9)
O11—Li2—Li346.09 (8)O11—Li4—Li4i51.09 (9)
O4—Li2—Li3102.36 (11)O10—Li4—Li4i116.66 (16)
O10i—Li2—Li3130.04 (12)O11i—Li4—S3132.78 (13)
S2—Li2—Li355.17 (7)O11—Li4—S3106.38 (10)
Li4i—Li2—Li391.48 (10)O10—Li4—S3103.03 (10)
O11—Li2—Si2123.91 (11)Li4i—Li4—S3140.04 (16)
O4—Li2—Si235.07 (5)O11i—Li4—Li2i47.43 (8)
O10i—Li2—Si2136.83 (12)O11—Li4—Li2i129.71 (13)
S2—Li2—Si244.74 (4)O10—Li4—Li2i48.83 (8)
Li4i—Li2—Si2172.23 (12)Li4i—Li4—Li2i88.37 (12)
Li3—Li2—Si282.59 (8)S3—Li4—Li2i123.61 (11)
O11—Li2—Li425.32 (7)O11i—Li4—Li3142.27 (13)
O4—Li2—Li4146.59 (12)O11—Li4—Li345.89 (8)
O10i—Li2—Li483.42 (9)O10—Li4—Li3117.05 (12)
S2—Li2—Li492.49 (8)Li4i—Li4—Li394.23 (13)
Li4i—Li2—Li444.29 (9)S3—Li4—Li361.84 (7)
Li3—Li2—Li449.14 (7)Li2i—Li4—Li3164.31 (14)
Si2—Li2—Li4130.99 (9)O11i—Li4—Li293.49 (9)
Si2—S2—Li3107.05 (6)O11—Li4—Li224.67 (6)
Si2—S2—Li1157.74 (7)O10—Li4—Li2142.91 (12)
Li3—S2—Li176.20 (8)Li4i—Li4—Li247.33 (9)
Si2—S2—Li273.72 (6)S3—Li4—Li297.37 (8)
Li3—S2—Li264.37 (8)Li2i—Li4—Li2135.71 (9)
Li1—S2—Li288.75 (8)Li3—Li4—Li248.96 (7)
O5—Si2—O6105.18 (6)O11i—Li4—Li1105.44 (11)
O5—Si2—O4105.08 (6)O11—Li4—Li181.26 (9)
O6—Si2—O4111.00 (6)O10—Li4—Li1148.13 (11)
O5—Si2—S2115.78 (5)Li4i—Li4—Li195.20 (13)
O6—Si2—S2115.88 (5)S3—Li4—Li145.33 (6)
O4—Si2—S2103.49 (4)Li2i—Li4—Li1137.98 (12)
O5—Si2—Li2127.79 (7)Li3—Li4—Li157.25 (8)
O6—Si2—Li2123.10 (7)Li2—Li4—Li161.11 (7)
O4—Si2—Li242.41 (6)Li2i—O10—Li480.25 (10)
S2—Si2—Li261.54 (6)Li2i—O10—H10B110.3
C16—O4—Si2131.38 (9)Li4—O10—H10B106.7
C16—O4—Li2125.52 (11)Li2i—O10—H10A140.8
Si2—O4—Li2102.52 (9)Li4—O10—H10A104.2
C16—C13—H13A109.5H10B—O10—H10A105.6
C16—C13—H13B109.4C51—C56—C55124.6 (6)
H13A—C13—H13B109.5C51—C56—H56A116.9
C16—C13—H13C109.5C55—C56—H56A118.1
H13A—C13—H13C109.5C53—C52—C51122.1 (6)
H13B—C13—H13C109.5C53—C52—H52A116.5
C16—C14—H14A109.6C51—C52—H52A120.4
C16—C14—H14B109.4C56—C55—C54118.6 (6)
H14A—C14—H14B109.5C56—C55—H55A120.3
C16—C14—H14C109.5C54—C55—H55A120.9
H14A—C14—H14C109.5C56—C51—C52116.7 (6)
H14B—C14—H14C109.5C56—C51—C50123.1 (8)
C16—C15—H15A109.4C52—C51—C50120.2 (8)
C16—C15—H15B109.5C53—C54—C55116.6 (6)
H15A—C15—H15B109.5C53—C54—H54A122.9
C16—C15—H15C109.5C55—C54—H54A119.2
H15A—C15—H15C109.5C52—C53—C54120.6 (6)
H15B—C15—H15C109.5C52—C53—H53A120.8
O4—C16—C13107.76 (14)C54—C53—H53A117.2
O4—C16—C14104.96 (13)C51—C50—H50A111.6
C13—C16—C14111.91 (18)C51—C50—H50B109.5
O4—C16—C15110.75 (15)H50A—C50—H50B109.5
C13—C16—C15111.21 (17)C51—C50—H50C107.3
C14—C16—C15110.06 (16)H50A—C50—H50C109.5
C18—O5—Si2132.72 (12)H50B—C50—H50C109.5
C18—C17—H17A109.2C60—C61—C66118.2 (10)
C18—C17—H17B109.6C60—C61—C62121.4 (10)
H17A—C17—H17B109.5C66—C61—C62120.3 (6)
C18—C17—H17C109.6C61—C62—C63119.1 (6)
H17A—C17—H17C109.5C61—C62—H62A126.1
H17B—C17—H17C109.5C63—C62—H62A113.3
O5—C18—C20109.26 (16)C66—C65—C64120.2 (7)
O5—C18—C17105.35 (18)C66—C65—H65A113.3
C20—C18—C17111.7 (3)C64—C65—H65A126.4
O5—C18—C19109.34 (17)C65—C64—C63118.7 (7)
C20—C18—C19112.3 (3)C65—C64—H64A113.5
C17—C18—C19108.6 (2)C63—C64—H64A127.8
C18—C19—H19A109.5C65—C66—C61120.2 (7)
C18—C19—H19B109.5C65—C66—H66A125.4
H19A—C19—H19B109.5C61—C66—H66A113.4
C18—C19—H19C109.5C62—C63—C64120.0 (7)
H19A—C19—H19C109.5C62—C63—H63A126.2
H19B—C19—H19C109.5C64—C63—H63A113.4
C18—C20—H20A109.4C61—C60—H60A119.5
C18—C20—H20B109.5C61—C60—H60B101.6
H20A—C20—H20B109.5H60A—C60—H60B109.5
C18—C20—H20C109.6C61—C60—H60C106.8
H20A—C20—H20C109.5H60A—C60—H60C109.5
H20B—C20—H20C109.5H60B—C60—H60C109.5
Symmetry code: (i) x+1, y, z+2.

Experimental details

Crystal data
Chemical formula[Li8(C12H27O3SSi)6(OH)2(H2O)2]·2C7H8
Mr1986.7
Crystal system, space groupMonoclinic, P21/n
Temperature (K)200
a, b, c (Å)13.088 (3), 27.188 (5), 17.525 (4)
β (°) 102.25 (3)
V3)6094 (2)
Z2
Radiation typeMo Kα
µ (mm1)0.23
Crystal size (mm)0.6 × 0.3 × 0.2
Data collection
DiffractometerBruker IPDS
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
47490, 11732, 10031
Rint0.035
(sin θ/λ)max1)0.615
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.105, 1.04
No. of reflections11732
No. of parameters669
No. of restraints31
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.32, 0.24

Computer programs: XSCANS (Bruker, 1999), XSCANS, SHELXTL (Bruker, 1998), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), RESVIEW (Schwenk, 1998), SHELXL97.

Selected geometric parameters (Å, º) top
Li1—S12.449 (3)S2—Li32.433 (2)
Li1—S32.514 (3)Li3—O111.926 (2)
Li1—S22.541 (3)Li3—S32.647 (2)
Li1—Li33.070 (4)Li3—Li42.680 (3)
S1—Si12.0546 (6)S3—Si32.0644 (6)
Li2—O111.912 (3)S3—Li42.459 (2)
Li2—O10i1.971 (3)O11—Li4i1.953 (2)
Li2—S22.579 (2)O11—Li41.959 (3)
Li2—Li4i2.581 (3)Li4—O102.033 (3)
Li2—Li32.673 (3)Li4—Li4i2.451 (5)
S2—Si22.0649 (7)
Si1—S1—Li175.57 (6)Li2—Li3—Li481.90 (9)
O11—Li2—Li4i48.78 (8)Li4i—Li4—Li2i88.37 (12)
O11—Li2—Li346.09 (8)Li4i—Li4—Li394.23 (13)
O10i—Li2—Li3130.04 (12)Li2i—Li4—Li3164.31 (14)
S2—Li2—Li355.17 (7)Li4i—Li4—Li247.33 (9)
Li4i—Li2—Li391.48 (10)
Symmetry code: (i) x+1, y, z+2.
 

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