The title compound, [Na
4(C
12H
27O
3SSi)
4(CH
4O)
6], may be regarded as an assembly of short-contact ion triplets built of a dinuclear [Na
2(MeOH)
6]
2+ cation and two [Na{SSi(O
tBu)
3}
2]
− anions, related by a centre of symmetry. The presence of sulfur and oxygen bridges, as well as O—H
O and O—H
S hydrogen bonds, results in a tetranuclear complex with all Na atoms pentacoordinated. The complex sits on a centre of symmetry.
Supporting information
CCDC reference: 624017
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C)= 0.004 Å
- R factor = 0.037
- wR factor = 0.145
- Data-to-parameter ratio = 18.7
checkCIF/PLATON results
No syntax errors found
No errors found in this datablock
Data collection: KM-4 Software (Gałdecki et al., 1996); cell refinement: KM-4 Software; data reduction: KM-4 Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and
Mercury (Macrae et al., 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).
Tetrakis(µ
3-methanol)bis(methanol-
κO)(µ
2-tri-
tert-
butoxysilanethiolato-
κ3S;
S,
O)bis(tri-
tert-butoxysilanethiolato-
κ2S,
O)tetrasodium(I)
top
Crystal data top
[Na4(C12H27O3SSi)4(CH4O)6] | Z = 1 |
Mr = 1402.16 | F(000) = 764 |
Triclinic, P1 | Dx = 1.126 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.298 (2) Å | Cell parameters from 46 reflections |
b = 14.988 (3) Å | θ = 3.5–31° |
c = 17.932 (4) Å | µ = 0.25 mm−1 |
α = 101.90 (3)° | T = 150 K |
β = 99.64 (3)° | Plate, colourless |
γ = 103.38 (3)° | 0.5 × 0.4 × 0.2 mm |
V = 2068.1 (9) Å3 | |
Data collection top
Kuma KM-4 diffractometer | θmax = 25.6°, θmin = 1.2° |
Graphite monochromator | h = −10→9 |
ω/2θ scans | k = −17→17 |
7983 measured reflections | l = 0→21 |
7721 independent reflections | 3 standard reflections every 200 reflections |
5883 reflections with I > 2σ(I) | intensity decay: 0.7% |
Rint = 0.033 | |
Refinement top
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.145 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0991P)2 + 0.367P] where P = (Fo2 + 2Fc2)/3 |
7721 reflections | (Δ/σ)max = 0.005 |
412 parameters | Δρmax = 0.47 e Å−3 |
0 restraints | Δρmin = −0.39 e Å−3 |
Special details top
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 | x | y | z | Uiso*/Ueq | |
Si1 | 0.53647 (8) | 1.21023 (4) | 0.29777 (3) | 0.02378 (16) | |
Si2 | 0.27722 (7) | 0.76588 (4) | 0.19087 (3) | 0.02224 (15) | |
S1 | 0.35219 (7) | 1.14608 (4) | 0.34831 (3) | 0.03003 (16) | |
S2 | 0.50537 (7) | 0.83923 (4) | 0.26587 (3) | 0.02718 (15) | |
Na1 | 0.36575 (13) | 0.98569 (6) | 0.24666 (6) | 0.0367 (2) | |
Na2 | 0.43581 (12) | 0.89568 (7) | 0.41645 (5) | 0.0310 (2) | |
O1 | 0.7265 (2) | 1.25378 (11) | 0.35334 (9) | 0.0301 (4) | |
O2 | 0.5510 (2) | 1.12270 (11) | 0.22889 (9) | 0.0270 (3) | |
O3 | 0.4998 (2) | 1.29671 (11) | 0.26201 (10) | 0.0298 (4) | |
O4 | 0.21070 (19) | 0.84477 (10) | 0.15069 (9) | 0.0251 (3) | |
O5 | 0.12151 (19) | 0.72712 (10) | 0.23256 (9) | 0.0258 (3) | |
O6 | 0.2748 (2) | 0.67304 (11) | 0.12471 (9) | 0.0271 (3) | |
C1 | 0.0371 (4) | 0.9325 (2) | 0.36431 (17) | 0.0443 (7) | |
H1A | −0.0181 | 0.8951 | 0.3965 | 0.066* | |
H1B | −0.0456 | 0.9268 | 0.3164 | 0.066* | |
H1C | 0.0804 | 0.9992 | 0.3937 | 0.066* | |
C2 | 0.2417 (3) | 0.9401 (2) | 0.57091 (17) | 0.0432 (6) | |
H2A | 0.263 | 0.9652 | 0.6277 | 0.065* | |
H2B | 0.1683 | 0.8749 | 0.5558 | 0.065* | |
H2C | 0.1856 | 0.9796 | 0.5445 | 0.065* | |
C3 | 0.6683 (4) | 0.7390 (2) | 0.43424 (18) | 0.0545 (8) | |
H3A | 0.6524 | 0.7335 | 0.3779 | 0.082* | |
H3B | 0.622 | 0.6767 | 0.443 | 0.082* | |
H3C | 0.7899 | 0.7624 | 0.459 | 0.082* | |
C10 | 0.8116 (3) | 1.34418 (17) | 0.40831 (14) | 0.0339 (6) | |
C11 | 0.8734 (4) | 1.41576 (19) | 0.36342 (18) | 0.0481 (7) | |
H11A | 0.9469 | 1.3925 | 0.3312 | 0.072* | |
H11B | 0.9376 | 1.4765 | 0.4004 | 0.072* | |
H11C | 0.7755 | 1.4245 | 0.3297 | 0.072* | |
C12 | 0.6944 (4) | 1.3758 (2) | 0.45734 (18) | 0.0548 (8) | |
H12A | 0.5985 | 1.3866 | 0.4237 | 0.082* | |
H12B | 0.7568 | 1.4349 | 0.4969 | 0.082* | |
H12C | 0.6517 | 1.3266 | 0.4833 | 0.082* | |
C13 | 0.9633 (4) | 1.3279 (2) | 0.45815 (19) | 0.0586 (9) | |
H13A | 0.9236 | 1.2859 | 0.4906 | 0.088* | |
H13B | 1.0365 | 1.3887 | 0.4919 | 0.088* | |
H13C | 1.0278 | 1.2984 | 0.4242 | 0.088* | |
C20 | 0.6783 (3) | 1.11954 (17) | 0.18231 (14) | 0.0327 (5) | |
C21 | 0.7371 (4) | 1.21283 (19) | 0.16109 (16) | 0.0398 (6) | |
H21A | 0.6393 | 1.2271 | 0.1321 | 0.06* | |
H21B | 0.82 | 1.2079 | 0.1285 | 0.06* | |
H21C | 0.7901 | 1.2637 | 0.209 | 0.06* | |
C22 | 0.8263 (4) | 1.0954 (2) | 0.22854 (17) | 0.0439 (7) | |
H22A | 0.8775 | 1.1453 | 0.2772 | 0.066* | |
H22B | 0.9118 | 1.0909 | 0.1973 | 0.066* | |
H22C | 0.7852 | 1.0346 | 0.2408 | 0.066* | |
C23 | 0.5903 (4) | 1.0400 (2) | 0.10903 (17) | 0.0533 (8) | |
H23A | 0.5531 | 0.9803 | 0.1237 | 0.08* | |
H23B | 0.6698 | 1.0337 | 0.0748 | 0.08* | |
H23C | 0.4914 | 1.0546 | 0.0813 | 0.08* | |
C30 | 0.3505 (3) | 1.31012 (19) | 0.21777 (16) | 0.0370 (6) | |
C31 | 0.2484 (4) | 1.2192 (2) | 0.15716 (17) | 0.0473 (7) | |
H31A | 0.3206 | 1.1977 | 0.1234 | 0.071* | |
H31B | 0.1511 | 1.231 | 0.1254 | 0.071* | |
H31C | 0.2074 | 1.1703 | 0.1836 | 0.071* | |
C32 | 0.4155 (4) | 1.3880 (2) | 0.1783 (2) | 0.0584 (9) | |
H32A | 0.481 | 1.446 | 0.2184 | 0.088* | |
H32B | 0.3187 | 1.4005 | 0.1468 | 0.088* | |
H32C | 0.4883 | 1.3674 | 0.1445 | 0.088* | |
C33 | 0.2441 (4) | 1.3424 (2) | 0.2732 (2) | 0.0534 (8) | |
H33A | 0.2082 | 1.2932 | 0.3002 | 0.08* | |
H33B | 0.1436 | 1.3536 | 0.2436 | 0.08* | |
H33C | 0.3118 | 1.4012 | 0.3118 | 0.08* | |
C40 | 0.0507 (3) | 0.83822 (17) | 0.09963 (14) | 0.0303 (5) | |
C41 | −0.0670 (3) | 0.8666 (2) | 0.15019 (17) | 0.0450 (7) | |
H41A | −0.099 | 0.8186 | 0.1788 | 0.067* | |
H41B | −0.1695 | 0.8717 | 0.117 | 0.067* | |
H41C | −0.0089 | 0.9281 | 0.1875 | 0.067* | |
C42 | −0.0298 (3) | 0.73908 (18) | 0.04606 (15) | 0.0374 (6) | |
H42A | 0.0469 | 0.7228 | 0.0127 | 0.056* | |
H42B | −0.1381 | 0.7372 | 0.0132 | 0.056* | |
H42C | −0.0498 | 0.6933 | 0.0777 | 0.056* | |
C43 | 0.0948 (4) | 0.9098 (2) | 0.05193 (17) | 0.0491 (7) | |
H43A | 0.1466 | 0.9732 | 0.0873 | 0.074* | |
H43B | −0.009 | 0.9099 | 0.0166 | 0.074* | |
H43C | 0.1751 | 0.8924 | 0.0212 | 0.074* | |
C50 | 0.0705 (3) | 0.64053 (16) | 0.25804 (14) | 0.0304 (5) | |
C51 | −0.0495 (4) | 0.6605 (2) | 0.31068 (18) | 0.0486 (7) | |
H51A | 0.0139 | 0.7102 | 0.358 | 0.073* | |
H51B | −0.1001 | 0.6026 | 0.3252 | 0.073* | |
H51C | −0.1397 | 0.6816 | 0.2828 | 0.073* | |
C52 | −0.0238 (4) | 0.55871 (18) | 0.18731 (16) | 0.0432 (7) | |
H52A | −0.1198 | 0.5747 | 0.1585 | 0.065* | |
H52B | −0.0661 | 0.5016 | 0.2047 | 0.065* | |
H52C | 0.0536 | 0.547 | 0.1531 | 0.065* | |
C53 | 0.2242 (4) | 0.6198 (2) | 0.30164 (17) | 0.0440 (7) | |
H53A | 0.3005 | 0.6093 | 0.2666 | 0.066* | |
H53B | 0.1876 | 0.563 | 0.3202 | 0.066* | |
H53C | 0.2843 | 0.6739 | 0.3465 | 0.066* | |
C60 | 0.3905 (3) | 0.65625 (17) | 0.07526 (14) | 0.0325 (5) | |
C61 | 0.5391 (3) | 0.63416 (19) | 0.12255 (17) | 0.0409 (6) | |
H61A | 0.5989 | 0.6888 | 0.1669 | 0.061* | |
H61B | 0.6174 | 0.6207 | 0.0893 | 0.061* | |
H61C | 0.4968 | 0.5788 | 0.142 | 0.061* | |
C62 | 0.4518 (4) | 0.7420 (2) | 0.04459 (16) | 0.0411 (6) | |
H62A | 0.3547 | 0.7535 | 0.0124 | 0.062* | |
H62B | 0.5336 | 0.7303 | 0.0128 | 0.062* | |
H62C | 0.5066 | 0.7977 | 0.0887 | 0.062* | |
C63 | 0.2891 (4) | 0.5709 (2) | 0.00865 (18) | 0.0552 (8) | |
H63A | 0.2459 | 0.5172 | 0.03 | 0.083* | |
H63B | 0.3626 | 0.5539 | −0.0262 | 0.083* | |
H63C | 0.1934 | 0.5864 | −0.0208 | 0.083* | |
O10 | 0.3990 (2) | 0.94111 (13) | 0.54874 (10) | 0.0346 (4) | |
O11 | 0.1739 (2) | 0.89821 (14) | 0.34444 (12) | 0.0436 (5) | |
O12 | 0.5828 (3) | 0.80317 (16) | 0.46715 (12) | 0.0486 (5) | |
H10D | 0.451 (5) | 0.917 (3) | 0.574 (2) | 0.072 (12)* | |
H11D | 0.137 (4) | 0.847 (2) | 0.3104 (19) | 0.049 (9)* | |
H12D | 0.595 (4) | 0.813 (3) | 0.514 (2) | 0.064 (11)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Si1 | 0.0292 (3) | 0.0205 (3) | 0.0205 (3) | 0.0040 (2) | 0.0038 (2) | 0.0075 (2) |
Si2 | 0.0258 (3) | 0.0205 (3) | 0.0201 (3) | 0.0051 (2) | 0.0045 (2) | 0.0067 (2) |
S1 | 0.0337 (3) | 0.0299 (3) | 0.0274 (3) | 0.0043 (2) | 0.0089 (2) | 0.0128 (2) |
S2 | 0.0282 (3) | 0.0282 (3) | 0.0221 (3) | 0.0057 (2) | 0.0022 (2) | 0.0050 (2) |
Na1 | 0.0438 (6) | 0.0219 (5) | 0.0378 (6) | 0.0040 (4) | −0.0009 (4) | 0.0068 (4) |
Na2 | 0.0361 (5) | 0.0336 (5) | 0.0238 (5) | 0.0099 (4) | 0.0058 (4) | 0.0085 (4) |
O1 | 0.0316 (9) | 0.0231 (8) | 0.0277 (8) | 0.0018 (7) | −0.0017 (7) | 0.0028 (7) |
O2 | 0.0304 (8) | 0.0247 (8) | 0.0248 (8) | 0.0051 (6) | 0.0066 (7) | 0.0063 (6) |
O3 | 0.0323 (8) | 0.0247 (8) | 0.0332 (9) | 0.0058 (7) | 0.0046 (7) | 0.0139 (7) |
O4 | 0.0259 (8) | 0.0243 (8) | 0.0241 (8) | 0.0035 (6) | 0.0029 (6) | 0.0103 (6) |
O5 | 0.0299 (8) | 0.0222 (8) | 0.0285 (8) | 0.0074 (6) | 0.0089 (7) | 0.0114 (6) |
O6 | 0.0304 (8) | 0.0236 (8) | 0.0256 (8) | 0.0065 (6) | 0.0067 (7) | 0.0033 (6) |
C1 | 0.0443 (15) | 0.0555 (17) | 0.0414 (15) | 0.0250 (13) | 0.0148 (13) | 0.0137 (13) |
C2 | 0.0405 (15) | 0.0498 (16) | 0.0410 (15) | 0.0091 (12) | 0.0124 (12) | 0.0165 (13) |
C3 | 0.064 (2) | 0.073 (2) | 0.0453 (17) | 0.0438 (18) | 0.0204 (15) | 0.0226 (16) |
C10 | 0.0367 (13) | 0.0267 (12) | 0.0273 (12) | −0.0027 (10) | −0.0015 (10) | 0.0027 (10) |
C11 | 0.0547 (17) | 0.0291 (13) | 0.0468 (16) | −0.0081 (12) | 0.0069 (14) | 0.0063 (12) |
C12 | 0.0584 (19) | 0.0447 (17) | 0.0458 (17) | −0.0016 (14) | 0.0167 (15) | −0.0085 (13) |
C13 | 0.0576 (19) | 0.0474 (17) | 0.0473 (17) | 0.0011 (14) | −0.0205 (15) | 0.0025 (14) |
C20 | 0.0390 (13) | 0.0307 (12) | 0.0274 (12) | 0.0060 (10) | 0.0135 (10) | 0.0046 (10) |
C21 | 0.0464 (15) | 0.0443 (15) | 0.0345 (14) | 0.0115 (12) | 0.0173 (12) | 0.0176 (12) |
C22 | 0.0441 (15) | 0.0490 (16) | 0.0496 (17) | 0.0216 (13) | 0.0189 (13) | 0.0200 (13) |
C23 | 0.0588 (19) | 0.0525 (18) | 0.0364 (15) | 0.0000 (15) | 0.0195 (14) | −0.0053 (13) |
C30 | 0.0380 (13) | 0.0406 (14) | 0.0412 (14) | 0.0167 (11) | 0.0080 (11) | 0.0238 (12) |
C31 | 0.0402 (15) | 0.0595 (18) | 0.0399 (15) | 0.0109 (13) | −0.0024 (12) | 0.0199 (14) |
C32 | 0.065 (2) | 0.0586 (19) | 0.069 (2) | 0.0222 (16) | 0.0151 (17) | 0.0465 (18) |
C33 | 0.0578 (19) | 0.0569 (19) | 0.062 (2) | 0.0327 (16) | 0.0196 (16) | 0.0271 (16) |
C40 | 0.0292 (12) | 0.0315 (12) | 0.0292 (12) | 0.0078 (10) | −0.0012 (10) | 0.0126 (10) |
C41 | 0.0356 (14) | 0.0508 (17) | 0.0481 (16) | 0.0190 (12) | 0.0027 (12) | 0.0094 (13) |
C42 | 0.0350 (13) | 0.0381 (14) | 0.0337 (13) | 0.0070 (11) | −0.0028 (11) | 0.0097 (11) |
C43 | 0.0524 (17) | 0.0465 (16) | 0.0450 (16) | 0.0047 (13) | −0.0060 (13) | 0.0285 (14) |
C50 | 0.0356 (12) | 0.0248 (11) | 0.0327 (13) | 0.0041 (10) | 0.0082 (10) | 0.0157 (10) |
C51 | 0.0591 (18) | 0.0469 (16) | 0.0526 (18) | 0.0136 (14) | 0.0296 (15) | 0.0280 (14) |
C52 | 0.0487 (16) | 0.0309 (13) | 0.0412 (15) | −0.0042 (12) | 0.0052 (12) | 0.0108 (12) |
C53 | 0.0460 (15) | 0.0385 (15) | 0.0487 (16) | 0.0083 (12) | 0.0014 (13) | 0.0248 (13) |
C60 | 0.0363 (13) | 0.0329 (13) | 0.0280 (12) | 0.0105 (10) | 0.0101 (10) | 0.0036 (10) |
C61 | 0.0405 (15) | 0.0383 (14) | 0.0494 (16) | 0.0183 (12) | 0.0132 (12) | 0.0127 (12) |
C62 | 0.0445 (15) | 0.0510 (16) | 0.0367 (14) | 0.0175 (13) | 0.0173 (12) | 0.0192 (12) |
C63 | 0.0538 (18) | 0.0517 (18) | 0.0447 (17) | 0.0078 (14) | 0.0130 (14) | −0.0152 (14) |
O10 | 0.0445 (10) | 0.0366 (10) | 0.0299 (9) | 0.0174 (8) | 0.0119 (8) | 0.0147 (8) |
O11 | 0.0351 (10) | 0.0404 (11) | 0.0487 (12) | 0.0146 (8) | 0.0044 (9) | −0.0040 (9) |
O12 | 0.0692 (14) | 0.0642 (14) | 0.0285 (10) | 0.0428 (11) | 0.0140 (10) | 0.0175 (9) |
Geometric parameters (Å, º) top
Si1—O1 | 1.6234 (18) | C21—H21C | 0.98 |
Si1—O3 | 1.6261 (17) | C22—H22A | 0.98 |
Si1—O2 | 1.6480 (17) | C22—H22B | 0.98 |
Si1—S1 | 2.0559 (10) | C22—H22C | 0.98 |
Si1—Na1 | 3.2029 (15) | C23—H23A | 0.98 |
Si2—O6 | 1.6254 (17) | C23—H23B | 0.98 |
Si2—O5 | 1.6496 (16) | C23—H23C | 0.98 |
Si2—O4 | 1.6559 (16) | C30—C33 | 1.515 (4) |
Si2—S2 | 2.0434 (13) | C30—C31 | 1.517 (4) |
Si2—Na1 | 3.1095 (14) | C30—C32 | 1.526 (4) |
S1—Na1 | 2.7386 (15) | C31—H31A | 0.98 |
S2—Na1 | 2.7632 (13) | C31—H31B | 0.98 |
S2—Na2 | 2.8542 (13) | C31—H31C | 0.98 |
Na1—O4 | 2.362 (2) | C32—H32A | 0.98 |
Na1—O2 | 2.3778 (19) | C32—H32B | 0.98 |
Na1—O11 | 2.871 (2) | C32—H32C | 0.98 |
Na1—Na2 | 3.5906 (16) | C33—H33A | 0.98 |
Na2—O12 | 2.273 (2) | C33—H33B | 0.98 |
Na2—O11 | 2.347 (2) | C33—H33C | 0.98 |
Na2—O10i | 2.405 (2) | C40—C41 | 1.513 (4) |
Na2—O10 | 2.420 (2) | C40—C42 | 1.521 (3) |
Na2—C2i | 3.129 (3) | C40—C43 | 1.522 (3) |
Na2—Na2i | 3.663 (2) | C41—H41A | 0.98 |
O1—C10 | 1.442 (3) | C41—H41B | 0.98 |
O2—C20 | 1.455 (3) | C41—H41C | 0.98 |
O3—C30 | 1.434 (3) | C42—H42A | 0.98 |
O4—C40 | 1.451 (3) | C42—H42B | 0.98 |
O5—C50 | 1.459 (3) | C42—H42C | 0.98 |
O6—C60 | 1.441 (3) | C43—H43A | 0.98 |
C1—O11 | 1.418 (3) | C43—H43B | 0.98 |
C1—H1A | 0.98 | C43—H43C | 0.98 |
C1—H1B | 0.98 | C50—C53 | 1.511 (4) |
C1—H1C | 0.98 | C50—C52 | 1.519 (4) |
C2—O10 | 1.424 (3) | C50—C51 | 1.519 (4) |
C2—H2A | 0.98 | C51—H51A | 0.98 |
C2—H2B | 0.98 | C51—H51B | 0.98 |
C2—H2C | 0.98 | C51—H51C | 0.98 |
C3—O12 | 1.414 (3) | C52—H52A | 0.98 |
C3—H3A | 0.98 | C52—H52B | 0.98 |
C3—H3B | 0.98 | C52—H52C | 0.98 |
C3—H3C | 0.98 | C53—H53A | 0.98 |
C10—C12 | 1.507 (4) | C53—H53B | 0.98 |
C10—C13 | 1.516 (4) | C53—H53C | 0.98 |
C10—C11 | 1.517 (4) | C60—C62 | 1.515 (4) |
C11—H11A | 0.98 | C60—C61 | 1.518 (4) |
C11—H11B | 0.98 | C60—C63 | 1.519 (4) |
C11—H11C | 0.98 | C61—H61A | 0.98 |
C12—H12A | 0.98 | C61—H61B | 0.98 |
C12—H12B | 0.98 | C61—H61C | 0.98 |
C12—H12C | 0.98 | C62—H62A | 0.98 |
C13—H13A | 0.98 | C62—H62B | 0.98 |
C13—H13B | 0.98 | C62—H62C | 0.98 |
C13—H13C | 0.98 | C63—H63A | 0.98 |
C20—C21 | 1.518 (3) | C63—H63B | 0.98 |
C20—C23 | 1.520 (4) | C63—H63C | 0.98 |
C20—C22 | 1.522 (4) | O10—H10D | 0.78 (4) |
C21—H21A | 0.98 | O11—H11D | 0.83 (3) |
C21—H21B | 0.98 | O12—H12D | 0.81 (4) |
| | | |
O1—Si1—O3 | 104.47 (9) | C21—C20—C23 | 110.5 (2) |
O1—Si1—O2 | 105.05 (9) | O2—C20—C22 | 108.29 (19) |
O3—Si1—O2 | 111.15 (9) | C21—C20—C22 | 111.2 (2) |
O1—Si1—S1 | 116.00 (7) | C23—C20—C22 | 110.2 (2) |
O3—Si1—S1 | 115.87 (7) | C20—C21—H21A | 109.5 |
O2—Si1—S1 | 103.90 (7) | C20—C21—H21B | 109.5 |
O1—Si1—Na1 | 120.12 (7) | H21A—C21—H21B | 109.5 |
O3—Si1—Na1 | 133.03 (7) | C20—C21—H21C | 109.5 |
O2—Si1—Na1 | 46.10 (6) | H21A—C21—H21C | 109.5 |
S1—Si1—Na1 | 57.97 (4) | H21B—C21—H21C | 109.5 |
O6—Si2—O5 | 104.09 (9) | C20—C22—H22A | 109.5 |
O6—Si2—O4 | 111.37 (8) | C20—C22—H22B | 109.5 |
O5—Si2—O4 | 102.44 (8) | H22A—C22—H22B | 109.5 |
O6—Si2—S2 | 117.11 (7) | C20—C22—H22C | 109.5 |
O5—Si2—S2 | 115.49 (7) | H22A—C22—H22C | 109.5 |
O4—Si2—S2 | 105.49 (7) | H22B—C22—H22C | 109.5 |
O6—Si2—Na1 | 148.12 (7) | C20—C23—H23A | 109.5 |
O5—Si2—Na1 | 104.62 (7) | C20—C23—H23B | 109.5 |
O4—Si2—Na1 | 48.45 (6) | H23A—C23—H23B | 109.5 |
S2—Si2—Na1 | 60.75 (4) | C20—C23—H23C | 109.5 |
Si1—S1—Na1 | 82.51 (4) | H23A—C23—H23C | 109.5 |
Si2—S2—Na1 | 79.07 (4) | H23B—C23—H23C | 109.5 |
Si2—S2—Na2 | 106.66 (4) | O3—C30—C33 | 109.0 (2) |
Na1—S2—Na2 | 79.44 (4) | O3—C30—C31 | 110.8 (2) |
O4—Na1—O2 | 127.76 (7) | C33—C30—C31 | 110.5 (2) |
O4—Na1—S1 | 146.61 (6) | O3—C30—C32 | 105.4 (2) |
O2—Na1—S1 | 69.40 (5) | C33—C30—C32 | 110.3 (2) |
O4—Na1—S2 | 69.88 (5) | C31—C30—C32 | 110.7 (2) |
O2—Na1—S2 | 116.42 (6) | C30—C31—H31A | 109.5 |
S1—Na1—S2 | 133.13 (4) | C30—C31—H31B | 109.5 |
O4—Na1—O11 | 82.81 (7) | H31A—C31—H31B | 109.5 |
O2—Na1—O11 | 148.80 (7) | C30—C31—H31C | 109.5 |
S1—Na1—O11 | 81.10 (5) | H31A—C31—H31C | 109.5 |
S2—Na1—O11 | 76.74 (5) | H31B—C31—H31C | 109.5 |
O4—Na1—Si2 | 31.64 (4) | C30—C32—H32A | 109.5 |
O2—Na1—Si2 | 139.58 (6) | C30—C32—H32B | 109.5 |
S1—Na1—Si2 | 150.31 (4) | H32A—C32—H32B | 109.5 |
S2—Na1—Si2 | 40.18 (3) | C30—C32—H32C | 109.5 |
O11—Na1—Si2 | 69.21 (5) | H32A—C32—H32C | 109.5 |
O4—Na1—Si1 | 150.96 (6) | H32B—C32—H32C | 109.5 |
O2—Na1—Si1 | 29.96 (4) | C30—C33—H33A | 109.5 |
S1—Na1—Si1 | 39.52 (3) | C30—C33—H33B | 109.5 |
S2—Na1—Si1 | 130.07 (4) | H33A—C33—H33B | 109.5 |
O11—Na1—Si1 | 119.52 (6) | C30—C33—H33C | 109.5 |
Si2—Na1—Si1 | 167.56 (4) | H33A—C33—H33C | 109.5 |
O4—Na1—Na2 | 100.77 (5) | H33B—C33—H33C | 109.5 |
O2—Na1—Na2 | 124.00 (6) | O4—C40—C41 | 108.17 (19) |
S1—Na1—Na2 | 85.56 (4) | O4—C40—C42 | 111.91 (19) |
S2—Na1—Na2 | 51.39 (3) | C41—C40—C42 | 110.8 (2) |
O11—Na1—Na2 | 40.72 (5) | O4—C40—C43 | 105.25 (19) |
Si2—Na1—Na2 | 72.02 (4) | C41—C40—C43 | 110.1 (2) |
Si1—Na1—Na2 | 108.27 (4) | C42—C40—C43 | 110.5 (2) |
O12—Na2—O11 | 144.91 (9) | C40—C41—H41A | 109.5 |
O12—Na2—O10i | 111.68 (9) | C40—C41—H41B | 109.5 |
O11—Na2—O10i | 103.36 (8) | H41A—C41—H41B | 109.5 |
O12—Na2—O10 | 83.08 (8) | C40—C41—H41C | 109.5 |
O11—Na2—O10 | 100.85 (8) | H41A—C41—H41C | 109.5 |
O10i—Na2—O10 | 81.23 (8) | H41B—C41—H41C | 109.5 |
O12—Na2—S2 | 92.68 (6) | C40—C42—H42A | 109.5 |
O11—Na2—S2 | 83.93 (6) | C40—C42—H42B | 109.5 |
O10i—Na2—S2 | 98.31 (6) | H42A—C42—H42B | 109.5 |
O10—Na2—S2 | 175.19 (6) | C40—C42—H42C | 109.5 |
O12—Na2—C2i | 95.08 (9) | H42A—C42—H42C | 109.5 |
O11—Na2—C2i | 118.33 (9) | H42B—C42—H42C | 109.5 |
O10i—Na2—C2i | 25.84 (7) | C40—C43—H43A | 109.5 |
O10—Na2—C2i | 98.65 (8) | C40—C43—H43B | 109.5 |
S2—Na2—C2i | 79.39 (7) | H43A—C43—H43B | 109.5 |
O12—Na2—Na1 | 140.83 (7) | C40—C43—H43C | 109.5 |
O11—Na2—Na1 | 52.94 (6) | H43A—C43—H43C | 109.5 |
O10i—Na2—Na1 | 72.30 (6) | H43B—C43—H43C | 109.5 |
O10—Na2—Na1 | 134.56 (6) | O5—C50—C53 | 110.39 (19) |
S2—Na2—Na1 | 49.16 (3) | O5—C50—C52 | 109.36 (18) |
C2i—Na2—Na1 | 72.17 (7) | C53—C50—C52 | 110.8 (2) |
O12—Na2—Na2i | 99.38 (7) | O5—C50—C51 | 104.70 (19) |
O11—Na2—Na2i | 106.02 (7) | C53—C50—C51 | 111.6 (2) |
O10i—Na2—Na2i | 40.77 (5) | C52—C50—C51 | 109.9 (2) |
O10—Na2—Na2i | 40.46 (5) | C50—C51—H51A | 109.5 |
S2—Na2—Na2i | 138.87 (5) | C50—C51—H51B | 109.5 |
C2i—Na2—Na2i | 60.56 (7) | H51A—C51—H51B | 109.5 |
Na1—Na2—Na2i | 105.30 (4) | C50—C51—H51C | 109.5 |
C10—O1—Si1 | 132.77 (16) | H51A—C51—H51C | 109.5 |
C20—O2—Si1 | 129.96 (14) | H51B—C51—H51C | 109.5 |
C20—O2—Na1 | 123.89 (13) | C50—C52—H52A | 109.5 |
Si1—O2—Na1 | 103.95 (8) | C50—C52—H52B | 109.5 |
C30—O3—Si1 | 133.23 (15) | H52A—C52—H52B | 109.5 |
C40—O4—Si2 | 131.46 (14) | C50—C52—H52C | 109.5 |
C40—O4—Na1 | 121.66 (13) | H52A—C52—H52C | 109.5 |
Si2—O4—Na1 | 99.92 (8) | H52B—C52—H52C | 109.5 |
C50—O5—Si2 | 131.83 (15) | C50—C53—H53A | 109.5 |
C60—O6—Si2 | 131.83 (14) | C50—C53—H53B | 109.5 |
O11—C1—H1A | 109.5 | H53A—C53—H53B | 109.5 |
O11—C1—H1B | 109.5 | C50—C53—H53C | 109.5 |
H1A—C1—H1B | 109.5 | H53A—C53—H53C | 109.5 |
O11—C1—H1C | 109.5 | H53B—C53—H53C | 109.5 |
H1A—C1—H1C | 109.5 | O6—C60—C62 | 110.6 (2) |
H1B—C1—H1C | 109.5 | O6—C60—C61 | 108.4 (2) |
O10—C2—H2A | 109.5 | C62—C60—C61 | 110.7 (2) |
O10—C2—H2B | 109.5 | O6—C60—C63 | 105.3 (2) |
H2A—C2—H2B | 109.5 | C62—C60—C63 | 110.8 (2) |
O10—C2—H2C | 109.5 | C61—C60—C63 | 110.8 (2) |
H2A—C2—H2C | 109.5 | C60—C61—H61A | 109.5 |
H2B—C2—H2C | 109.5 | C60—C61—H61B | 109.5 |
O12—C3—H3A | 109.5 | H61A—C61—H61B | 109.5 |
O12—C3—H3B | 109.5 | C60—C61—H61C | 109.5 |
H3A—C3—H3B | 109.5 | H61A—C61—H61C | 109.5 |
O12—C3—H3C | 109.5 | H61B—C61—H61C | 109.5 |
H3A—C3—H3C | 109.5 | C60—C62—H62A | 109.5 |
H3B—C3—H3C | 109.5 | C60—C62—H62B | 109.5 |
O1—C10—C12 | 110.6 (2) | H62A—C62—H62B | 109.5 |
O1—C10—C13 | 105.1 (2) | C60—C62—H62C | 109.5 |
C12—C10—C13 | 111.3 (3) | H62A—C62—H62C | 109.5 |
O1—C10—C11 | 108.8 (2) | H62B—C62—H62C | 109.5 |
C12—C10—C11 | 111.4 (2) | C60—C63—H63A | 109.5 |
C13—C10—C11 | 109.4 (2) | C60—C63—H63B | 109.5 |
C10—C11—H11A | 109.5 | H63A—C63—H63B | 109.5 |
C10—C11—H11B | 109.5 | C60—C63—H63C | 109.5 |
H11A—C11—H11B | 109.5 | H63A—C63—H63C | 109.5 |
C10—C11—H11C | 109.5 | H63B—C63—H63C | 109.5 |
H11A—C11—H11C | 109.5 | C2—O10—Na2i | 106.76 (16) |
H11B—C11—H11C | 109.5 | C2—O10—Na2 | 126.00 (16) |
C10—C12—H12A | 109.5 | Na2i—O10—Na2 | 98.77 (8) |
C10—C12—H12B | 109.5 | C2—O10—H10D | 110 (3) |
H12A—C12—H12B | 109.5 | Na2i—O10—H10D | 105 (3) |
C10—C12—H12C | 109.5 | Na2—O10—H10D | 108 (3) |
H12A—C12—H12C | 109.5 | C1—O11—Na2 | 134.03 (17) |
H12B—C12—H12C | 109.5 | C1—O11—Na1 | 118.50 (17) |
C10—C13—H13A | 109.5 | Na2—O11—Na1 | 86.34 (7) |
C10—C13—H13B | 109.5 | C1—O11—H11D | 110 (2) |
H13A—C13—H13B | 109.5 | Na2—O11—H11D | 106 (2) |
C10—C13—H13C | 109.5 | Na1—O11—H11D | 92 (2) |
H13A—C13—H13C | 109.5 | C3—O12—Na2 | 132.85 (18) |
H13B—C13—H13C | 109.5 | C3—O12—H12D | 115 (3) |
O2—C20—C21 | 111.3 (2) | Na2—O12—H12D | 112 (3) |
O2—C20—C23 | 105.2 (2) | | |
Symmetry code: (i) −x+1, −y+2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O10—H10D···S1i | 0.78 (4) | 2.44 (4) | 3.216 (2) | 172 (4) |
O11—H11D···O5 | 0.83 (3) | 1.99 (3) | 2.803 (3) | 163 (3) |
O12—H12D···S1i | 0.81 (4) | 2.35 (4) | 3.161 (2) | 175 (4) |
Symmetry code: (i) −x+1, −y+2, −z+1. |