Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016987/bt6192sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016987/bt6192Isup2.hkl |
CCDC reference: 198311
Key indicators
- Single-crystal X-ray study
- T = 200 K
- Mean (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
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
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.
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]
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.
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. |
[Li8(C12H27O3SSi)6(OH)2(H2O)2]·2C7H8 | F(000) = 2160 |
Mr = 1986.7 | Dx = 1.083 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8000 reflections |
a = 13.088 (3) Å | θ = 4.1–26.1° |
b = 27.188 (5) Å | µ = 0.23 mm−1 |
c = 17.525 (4) Å | T = 200 K |
β = 102.25 (3)° | Thick plate, colourless |
V = 6094 (2) Å3 | 0.6 × 0.3 × 0.2 mm |
Z = 2 |
Bruker IPDS diffractometer | 10031 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.035 |
Graphite monochromator | θmax = 25.9°, θmin = 2.2° |
area IPDS scans | h = −16→16 |
47490 measured reflections | k = −33→33 |
11732 independent reflections | l = −21→21 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-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 parameters | Δρmax = 0.32 e Å−3 |
31 restraints | Δρmin = −0.24 e Å−3 |
[Li8(C12H27O3SSi)6(OH)2(H2O)2]·2C7H8 | V = 6094 (2) Å3 |
Mr = 1986.7 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.088 (3) Å | µ = 0.23 mm−1 |
b = 27.188 (5) Å | T = 200 K |
c = 17.525 (4) Å | 0.6 × 0.3 × 0.2 mm |
β = 102.25 (3)° |
Bruker IPDS diffractometer | 10031 reflections with I > 2σ(I) |
47490 measured reflections | Rint = 0.035 |
11732 independent reflections |
R[F2 > 2σ(F2)] = 0.036 | 31 restraints |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.32 e Å−3 |
11732 reflections | Δρmin = −0.24 e Å−3 |
669 parameters |
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. |
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) | |
C7 | 0.1533 (2) | 0.14649 (9) | 0.73574 (14) | 0.0888 (9) | |
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* | |
H15B | 0.8698 | 0.0635 | 0.7643 | 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* | |
O8 | 0.24940 (7) | −0.10048 (4) | 0.83109 (5) | 0.0326 (2) | |
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) |
H50C | 0.2893 | −0.4001 | 1.1991 | 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) |
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) |
C16 | 0.0351 (7) | 0.0546 (10) | 0.0427 (8) | 0.0049 (7) | 0.0057 (6) | −0.0010 (7) |
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) |
C60 | 0.176 (17) | 0.103 (12) | 0.121 (13) | 0.012 (11) | −0.092 (14) | 0.012 (9) |
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—H9E | 0.9600 | C30—H30A | 0.9599 |
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—H15A | 0.9600 | C62—C63 | 1.393 (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) |
H1A—C1—H1B | 109.5 | S3—Li3—Li2 | 116.96 (10) |
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 |
H8B—C8—H8C | 109.5 | O7—C27—C25 | 110.77 (14) |
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 |
C10—C11A—H11F | 108.9 | H34A—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—Li3 | 107.05 (6) | O11—Li4—Li2 | 24.67 (6) |
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) |
H17A—C17—H17C | 109.5 | C61—C62—H62A | 126.1 |
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 |
Symmetry code: (i) −x+1, −y, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Li8(C12H27O3SSi)6(OH)2(H2O)2]·2C7H8 |
Mr | 1986.7 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 200 |
a, b, c (Å) | 13.088 (3), 27.188 (5), 17.525 (4) |
β (°) | 102.25 (3) |
V (Å3) | 6094 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.23 |
Crystal size (mm) | 0.6 × 0.3 × 0.2 |
Data collection | |
Diffractometer | Bruker IPDS diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 47490, 11732, 10031 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.615 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.105, 1.04 |
No. of reflections | 11732 |
No. of parameters | 669 |
No. of restraints | 31 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.32, −0.24 |
Computer programs: XSCANS (Bruker, 1999), XSCANS, SHELXTL (Bruker, 1998), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), RESVIEW (Schwenk, 1998), SHELXL97.
Li1—S1 | 2.449 (3) | S2—Li3 | 2.433 (2) |
Li1—S3 | 2.514 (3) | Li3—O11 | 1.926 (2) |
Li1—S2 | 2.541 (3) | Li3—S3 | 2.647 (2) |
Li1—Li3 | 3.070 (4) | Li3—Li4 | 2.680 (3) |
S1—Si1 | 2.0546 (6) | S3—Si3 | 2.0644 (6) |
Li2—O11 | 1.912 (3) | S3—Li4 | 2.459 (2) |
Li2—O10i | 1.971 (3) | O11—Li4i | 1.953 (2) |
Li2—S2 | 2.579 (2) | O11—Li4 | 1.959 (3) |
Li2—Li4i | 2.581 (3) | Li4—O10 | 2.033 (3) |
Li2—Li3 | 2.673 (3) | Li4—Li4i | 2.451 (5) |
S2—Si2 | 2.0649 (7) | ||
Si1—S1—Li1 | 75.57 (6) | Li2—Li3—Li4 | 81.90 (9) |
O11—Li2—Li4i | 48.78 (8) | Li4i—Li4—Li2i | 88.37 (12) |
O11—Li2—Li3 | 46.09 (8) | Li4i—Li4—Li3 | 94.23 (13) |
O10i—Li2—Li3 | 130.04 (12) | Li2i—Li4—Li3 | 164.31 (14) |
S2—Li2—Li3 | 55.17 (7) | Li4i—Li4—Li2 | 47.33 (9) |
Li4i—Li2—Li3 | 91.48 (10) |
Symmetry code: (i) −x+1, −y, −z+2. |
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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.