Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803026217/su6055sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803026217/su6055Isup2.hkl |
CCDC reference: 227755
Data collection: COLLECT (Bruker-Nonius, 2002); cell refinement: EVALCCD (Duisenberg, 1998); data reduction: EVALCCD; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).
[Ge2(C4H9)2(C12H10O2Si)3] | Z = 2 |
Mr = 902.31 | F(000) = 932 |
Triclinic, P1 | Dx = 1.359 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.789 (5) Å | Cell parameters from 226 reflections |
b = 11.212 (5) Å | θ = 6.0–20.0° |
c = 19.071 (5) Å | µ = 1.49 mm−1 |
α = 96.831 (5)° | T = 294 K |
β = 105.521 (5)° | Irregular, colorless |
γ = 90.594 (5)° | 0.22 × 0.18 × 0.12 mm |
V = 2204.9 (15) Å3 |
Nonius KappaCCD diffractometer | 11629 independent reflections |
Radiation source: fine-focus sealed tube | 6529 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.076 |
Detector resolution: 9 pixels mm-1 | θmax = 29.0°, θmin = 3.2° |
ω scans with 1.80 ° and 162 sec per frame | h = −14→14 |
Absorption correction: part of the refinement model (ΔF) (Parkin et al., 1995); cubic fit to sinθ/λ - 24 parameters | k = −15→15 |
Tmin = 0.735, Tmax = 0.841 | l = −26→26 |
49113 measured reflections |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0482P)2 + 0.7808P] where P = (Fo2 + 2Fc2)/3 |
11629 reflections | (Δ/σ)max = 0.001 |
496 parameters | Δρmax = 0.97 e Å−3 |
0 restraints | Δρmin = −0.45 e Å−3 |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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 | ||
Ge1 | 0.37436 (3) | 0.11003 (3) | 0.71595 (2) | 0.0330 (1) | |
Ge2 | 0.24455 (3) | 0.40448 (3) | 0.78813 (2) | 0.0318 (1) | |
Si1 | 0.34262 (9) | 0.35179 (8) | 0.64605 (5) | 0.0365 (3) | |
Si2 | 0.09988 (9) | 0.15303 (8) | 0.73909 (5) | 0.0389 (3) | |
Si3 | 0.47655 (8) | 0.26735 (8) | 0.87133 (5) | 0.0342 (3) | |
O1 | 0.2474 (2) | 0.39751 (19) | 0.69603 (11) | 0.0408 (7) | |
O2 | 0.4135 (2) | 0.23129 (18) | 0.67401 (11) | 0.0414 (8) | |
O3 | 0.2059 (2) | 0.09992 (19) | 0.69772 (12) | 0.0447 (8) | |
O4 | 0.1578 (2) | 0.27489 (18) | 0.79567 (11) | 0.0397 (7) | |
O5 | 0.4031 (2) | 0.38538 (18) | 0.84138 (11) | 0.0378 (7) | |
O6 | 0.4333 (2) | 0.14695 (18) | 0.81171 (11) | 0.0417 (7) | |
C1 | 0.2410 (3) | 0.3180 (3) | 0.54956 (18) | 0.0468 (11) | |
C2 | 0.2373 (5) | 0.2062 (4) | 0.5096 (2) | 0.0773 (18) | |
C3 | 0.1546 (6) | 0.1790 (5) | 0.4394 (2) | 0.097 (2) | |
C4 | 0.0783 (5) | 0.2635 (7) | 0.4077 (3) | 0.096 (2) | |
C5 | 0.0830 (5) | 0.3780 (6) | 0.4438 (3) | 0.103 (2) | |
C6 | 0.1640 (4) | 0.4045 (5) | 0.5150 (2) | 0.0778 (19) | |
C7 | 0.4714 (3) | 0.4688 (3) | 0.65583 (17) | 0.0387 (11) | |
C8 | 0.4899 (4) | 0.5247 (3) | 0.5980 (2) | 0.0547 (14) | |
C9 | 0.5931 (5) | 0.6064 (3) | 0.6082 (2) | 0.0689 (18) | |
C10 | 0.6777 (4) | 0.6350 (3) | 0.6753 (2) | 0.0608 (16) | |
C11 | 0.6606 (4) | 0.5838 (4) | 0.7334 (2) | 0.0664 (17) | |
C12 | 0.5585 (4) | 0.5028 (4) | 0.7235 (2) | 0.0603 (16) | |
C13 | 0.0613 (3) | 0.0412 (3) | 0.7966 (2) | 0.0440 (11) | |
C14 | 0.1471 (4) | 0.0281 (3) | 0.8657 (2) | 0.0606 (14) | |
C15 | 0.1186 (4) | −0.0496 (4) | 0.9109 (3) | 0.0723 (17) | |
C16 | 0.0050 (4) | −0.1165 (3) | 0.8891 (3) | 0.0663 (16) | |
C17 | −0.0799 (4) | −0.1069 (3) | 0.8229 (3) | 0.0651 (16) | |
C18 | −0.0510 (4) | −0.0289 (3) | 0.7769 (2) | 0.0557 (12) | |
C19 | −0.0443 (3) | 0.1892 (3) | 0.6694 (2) | 0.0507 (12) | |
C20 | −0.1527 (4) | 0.2298 (4) | 0.6899 (3) | 0.0719 (17) | |
C21 | −0.2583 (5) | 0.2667 (5) | 0.6411 (4) | 0.100 (2) | |
C22 | −0.2554 (6) | 0.2666 (5) | 0.5690 (4) | 0.110 (3) | |
C23 | −0.1523 (6) | 0.2264 (6) | 0.5459 (3) | 0.117 (3) | |
C24 | −0.0467 (4) | 0.1860 (5) | 0.5965 (3) | 0.0831 (19) | |
C25 | 0.6537 (3) | 0.2945 (3) | 0.88946 (16) | 0.0394 (11) | |
C26 | 0.7120 (3) | 0.4096 (3) | 0.90358 (19) | 0.0485 (12) | |
C27 | 0.8446 (4) | 0.4259 (4) | 0.9187 (2) | 0.0630 (17) | |
C28 | 0.9210 (4) | 0.3278 (4) | 0.9208 (2) | 0.0642 (16) | |
C29 | 0.8669 (4) | 0.2160 (4) | 0.9084 (2) | 0.0614 (16) | |
C30 | 0.7344 (3) | 0.1984 (3) | 0.8926 (2) | 0.0518 (12) | |
C31 | 0.4385 (3) | 0.2380 (3) | 0.95807 (17) | 0.0382 (11) | |
C32 | 0.5123 (5) | 0.1662 (5) | 1.0041 (2) | 0.088 (2) | |
C33 | 0.4833 (5) | 0.1389 (5) | 1.0672 (3) | 0.106 (3) | |
C34 | 0.3782 (5) | 0.1843 (4) | 1.0848 (2) | 0.0769 (19) | |
C35 | 0.3047 (5) | 0.2567 (4) | 1.0420 (2) | 0.0839 (19) | |
C36 | 0.3353 (5) | 0.2848 (4) | 0.9795 (2) | 0.0744 (17) | |
C37 | 0.4449 (3) | −0.0382 (3) | 0.68243 (18) | 0.0446 (11) | |
C38 | 0.5889 (4) | −0.0296 (4) | 0.7163 (3) | 0.107 (2) | |
C39 | 0.4216 (7) | −0.0503 (5) | 0.6001 (3) | 0.131 (3) | |
C40 | 0.3851 (6) | −0.1411 (4) | 0.7061 (4) | 0.117 (3) | |
C41 | 0.1745 (3) | 0.5561 (3) | 0.81688 (18) | 0.0429 (11) | |
C42 | 0.0305 (4) | 0.5477 (4) | 0.7769 (3) | 0.0813 (19) | |
C43 | 0.1955 (5) | 0.5763 (3) | 0.8985 (2) | 0.0708 (18) | |
C44 | 0.2419 (5) | 0.6551 (3) | 0.7906 (3) | 0.093 (2) | |
H2 | 0.29130 | 0.14790 | 0.53000 | 0.0930* | |
H3 | 0.15170 | 0.10220 | 0.41430 | 0.1170* | |
H4 | 0.02220 | 0.24420 | 0.36110 | 0.1150* | |
H5 | 0.03310 | 0.43700 | 0.42120 | 0.1230* | |
H6 | 0.16650 | 0.48150 | 0.53980 | 0.0940* | |
H8 | 0.43240 | 0.50720 | 0.55180 | 0.0660* | |
H9 | 0.60440 | 0.64180 | 0.56850 | 0.0820* | |
H10 | 0.74670 | 0.68930 | 0.68150 | 0.0730* | |
H11 | 0.71760 | 0.60340 | 0.77970 | 0.0800* | |
H12 | 0.54750 | 0.46960 | 0.76400 | 0.0730* | |
H14 | 0.22470 | 0.07300 | 0.88100 | 0.0730* | |
H15 | 0.17640 | −0.05640 | 0.95610 | 0.0870* | |
H16 | −0.01440 | −0.16870 | 0.91950 | 0.0800* | |
H17 | −0.15710 | −0.15240 | 0.80840 | 0.0780* | |
H18 | −0.10940 | −0.02430 | 0.73160 | 0.0670* | |
H20 | −0.15320 | 0.23200 | 0.73870 | 0.0860* | |
H21 | −0.33030 | 0.29130 | 0.65610 | 0.1200* | |
H22 | −0.32520 | 0.29450 | 0.53570 | 0.1320* | |
H23 | −0.15210 | 0.22590 | 0.49710 | 0.1400* | |
H24 | 0.02290 | 0.15660 | 0.58070 | 0.1000* | |
H26 | 0.66130 | 0.47630 | 0.90290 | 0.0580* | |
H27 | 0.88210 | 0.50320 | 0.92740 | 0.0750* | |
H28 | 1.00990 | 0.33890 | 0.93080 | 0.0770* | |
H29 | 0.91860 | 0.15000 | 0.91040 | 0.0740* | |
H30 | 0.69870 | 0.12040 | 0.88400 | 0.0620* | |
H32 | 0.58490 | 0.13440 | 0.99280 | 0.1060* | |
H33 | 0.53590 | 0.08950 | 1.09720 | 0.1270* | |
H34 | 0.35740 | 0.16510 | 1.12650 | 0.0920* | |
H35 | 0.23270 | 0.28840 | 1.05410 | 0.1000* | |
H36 | 0.28410 | 0.33720 | 0.95120 | 0.0900* | |
H38A | 0.60670 | −0.02170 | 0.76870 | 0.1600* | |
H38B | 0.62510 | 0.03940 | 0.70220 | 0.1600* | |
H38C | 0.62630 | −0.10090 | 0.69940 | 0.1600* | |
H39A | 0.46300 | 0.01680 | 0.58710 | 0.1970* | |
H39B | 0.33070 | −0.05160 | 0.57710 | 0.1970* | |
H39C | 0.45620 | −0.12360 | 0.58370 | 0.1970* | |
H40A | 0.40300 | −0.13060 | 0.75860 | 0.1750* | |
H40B | 0.42000 | −0.21460 | 0.69030 | 0.1750* | |
H40C | 0.29360 | −0.14420 | 0.68470 | 0.1750* | |
H42A | 0.01960 | 0.53600 | 0.72490 | 0.1220* | |
H42B | −0.00830 | 0.62060 | 0.79000 | 0.1220* | |
H42C | −0.00990 | 0.48100 | 0.79080 | 0.1220* | |
H43A | 0.15070 | 0.51350 | 0.91330 | 0.1060* | |
H43B | 0.16340 | 0.65260 | 0.91210 | 0.1060* | |
H43C | 0.28590 | 0.57560 | 0.92230 | 0.1060* | |
H44A | 0.22530 | 0.64060 | 0.73820 | 0.1390* | |
H44B | 0.33300 | 0.65530 | 0.81280 | 0.1390* | |
H44C | 0.21000 | 0.73150 | 0.80410 | 0.1390* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge1 | 0.0322 (2) | 0.0323 (2) | 0.0360 (2) | 0.0005 (1) | 0.0131 (1) | 0.0018 (1) |
Ge2 | 0.0335 (2) | 0.0311 (2) | 0.0344 (2) | 0.0021 (1) | 0.0149 (1) | 0.0058 (1) |
Si1 | 0.0398 (5) | 0.0414 (5) | 0.0332 (5) | 0.0035 (4) | 0.0165 (4) | 0.0087 (4) |
Si2 | 0.0327 (5) | 0.0367 (5) | 0.0497 (5) | −0.0035 (4) | 0.0179 (4) | 0.0002 (4) |
Si3 | 0.0351 (5) | 0.0358 (5) | 0.0321 (4) | 0.0003 (4) | 0.0093 (4) | 0.0051 (3) |
O1 | 0.0423 (13) | 0.0489 (13) | 0.0370 (12) | 0.0102 (10) | 0.0177 (10) | 0.0117 (10) |
O2 | 0.0426 (13) | 0.0433 (13) | 0.0458 (13) | 0.0053 (10) | 0.0225 (11) | 0.0113 (10) |
O3 | 0.0323 (12) | 0.0502 (13) | 0.0514 (14) | −0.0034 (10) | 0.0165 (10) | −0.0055 (10) |
O4 | 0.0395 (13) | 0.0385 (12) | 0.0448 (13) | −0.0062 (10) | 0.0201 (10) | 0.0011 (9) |
O5 | 0.0342 (12) | 0.0388 (12) | 0.0405 (12) | −0.0007 (9) | 0.0094 (10) | 0.0074 (9) |
O6 | 0.0466 (14) | 0.0392 (12) | 0.0381 (12) | −0.0005 (10) | 0.0100 (10) | 0.0038 (9) |
C1 | 0.044 (2) | 0.064 (2) | 0.0387 (19) | 0.0005 (17) | 0.0204 (16) | 0.0107 (17) |
C2 | 0.115 (4) | 0.067 (3) | 0.046 (2) | −0.011 (3) | 0.014 (2) | 0.011 (2) |
C3 | 0.144 (5) | 0.092 (4) | 0.042 (3) | −0.043 (4) | 0.008 (3) | −0.002 (2) |
C4 | 0.069 (3) | 0.164 (6) | 0.045 (3) | −0.021 (4) | 0.006 (2) | 0.000 (3) |
C5 | 0.072 (3) | 0.186 (6) | 0.049 (3) | 0.051 (4) | 0.009 (2) | 0.022 (3) |
C6 | 0.074 (3) | 0.108 (4) | 0.052 (3) | 0.036 (3) | 0.018 (2) | 0.007 (2) |
C7 | 0.043 (2) | 0.0364 (17) | 0.0437 (19) | 0.0047 (14) | 0.0223 (16) | 0.0078 (14) |
C8 | 0.070 (3) | 0.056 (2) | 0.043 (2) | −0.0057 (19) | 0.0231 (19) | 0.0085 (17) |
C9 | 0.104 (4) | 0.055 (2) | 0.062 (3) | −0.018 (2) | 0.047 (3) | 0.009 (2) |
C10 | 0.067 (3) | 0.049 (2) | 0.073 (3) | −0.0109 (19) | 0.036 (2) | −0.004 (2) |
C11 | 0.057 (3) | 0.079 (3) | 0.059 (3) | −0.019 (2) | 0.009 (2) | 0.010 (2) |
C12 | 0.060 (3) | 0.073 (3) | 0.051 (2) | −0.012 (2) | 0.014 (2) | 0.0242 (19) |
C13 | 0.041 (2) | 0.0315 (17) | 0.066 (2) | 0.0034 (14) | 0.0259 (18) | 0.0049 (15) |
C14 | 0.043 (2) | 0.062 (2) | 0.080 (3) | −0.0002 (18) | 0.013 (2) | 0.030 (2) |
C15 | 0.063 (3) | 0.072 (3) | 0.084 (3) | 0.008 (2) | 0.011 (2) | 0.039 (2) |
C16 | 0.072 (3) | 0.050 (2) | 0.091 (3) | 0.004 (2) | 0.037 (3) | 0.030 (2) |
C17 | 0.061 (3) | 0.049 (2) | 0.092 (3) | −0.0166 (19) | 0.034 (3) | 0.006 (2) |
C18 | 0.054 (2) | 0.052 (2) | 0.061 (2) | −0.0132 (18) | 0.0198 (19) | −0.0013 (18) |
C19 | 0.049 (2) | 0.042 (2) | 0.063 (2) | −0.0063 (16) | 0.0214 (19) | 0.0005 (17) |
C20 | 0.052 (3) | 0.082 (3) | 0.073 (3) | 0.016 (2) | 0.006 (2) | −0.001 (2) |
C21 | 0.058 (3) | 0.104 (4) | 0.121 (5) | 0.029 (3) | 0.003 (3) | −0.005 (4) |
C22 | 0.062 (4) | 0.119 (5) | 0.128 (6) | 0.011 (3) | −0.024 (4) | 0.041 (4) |
C23 | 0.077 (4) | 0.183 (7) | 0.080 (4) | −0.009 (4) | −0.010 (3) | 0.050 (4) |
C24 | 0.049 (3) | 0.129 (4) | 0.070 (3) | −0.005 (3) | 0.010 (2) | 0.022 (3) |
C25 | 0.041 (2) | 0.050 (2) | 0.0273 (16) | −0.0005 (16) | 0.0090 (14) | 0.0062 (14) |
C26 | 0.045 (2) | 0.051 (2) | 0.050 (2) | 0.0011 (17) | 0.0139 (17) | 0.0060 (16) |
C27 | 0.049 (3) | 0.073 (3) | 0.063 (3) | −0.024 (2) | 0.008 (2) | 0.011 (2) |
C28 | 0.035 (2) | 0.098 (3) | 0.061 (3) | 0.003 (2) | 0.0161 (19) | 0.008 (2) |
C29 | 0.045 (2) | 0.078 (3) | 0.063 (3) | 0.017 (2) | 0.019 (2) | 0.005 (2) |
C30 | 0.045 (2) | 0.054 (2) | 0.056 (2) | 0.0056 (18) | 0.0149 (18) | 0.0017 (17) |
C31 | 0.042 (2) | 0.0350 (17) | 0.0387 (18) | 0.0018 (14) | 0.0121 (15) | 0.0059 (14) |
C32 | 0.075 (3) | 0.146 (5) | 0.065 (3) | 0.042 (3) | 0.037 (3) | 0.054 (3) |
C33 | 0.107 (4) | 0.159 (5) | 0.082 (4) | 0.058 (4) | 0.046 (3) | 0.079 (4) |
C34 | 0.109 (4) | 0.085 (3) | 0.053 (3) | 0.007 (3) | 0.043 (3) | 0.025 (2) |
C35 | 0.116 (4) | 0.088 (3) | 0.076 (3) | 0.039 (3) | 0.065 (3) | 0.030 (3) |
C36 | 0.089 (3) | 0.083 (3) | 0.073 (3) | 0.041 (3) | 0.046 (3) | 0.038 (2) |
C37 | 0.050 (2) | 0.0387 (19) | 0.047 (2) | 0.0055 (16) | 0.0180 (17) | 0.0016 (15) |
C38 | 0.059 (3) | 0.074 (3) | 0.177 (6) | 0.021 (2) | 0.029 (3) | −0.023 (3) |
C39 | 0.232 (8) | 0.096 (4) | 0.065 (3) | 0.083 (5) | 0.043 (4) | −0.005 (3) |
C40 | 0.144 (5) | 0.050 (3) | 0.196 (6) | 0.010 (3) | 0.110 (5) | 0.026 (3) |
C41 | 0.054 (2) | 0.0349 (18) | 0.045 (2) | 0.0099 (15) | 0.0207 (17) | 0.0081 (14) |
C42 | 0.069 (3) | 0.070 (3) | 0.098 (4) | 0.034 (2) | 0.012 (3) | 0.005 (2) |
C43 | 0.107 (4) | 0.053 (2) | 0.060 (3) | 0.021 (2) | 0.038 (2) | 0.0003 (19) |
C44 | 0.146 (5) | 0.037 (2) | 0.122 (4) | 0.007 (3) | 0.079 (4) | 0.017 (2) |
Ge1—O2 | 1.759 (2) | C35—C36 | 1.388 (6) |
Ge1—O3 | 1.756 (2) | C37—C38 | 1.512 (6) |
Ge1—O6 | 1.762 (2) | C37—C39 | 1.511 (6) |
Ge1—C37 | 1.945 (4) | C37—C40 | 1.488 (6) |
Ge2—O1 | 1.757 (2) | C41—C42 | 1.533 (6) |
Ge2—O4 | 1.761 (2) | C41—C43 | 1.501 (5) |
Ge2—O5 | 1.770 (2) | C41—C44 | 1.524 (6) |
Ge2—C41 | 1.946 (4) | C2—H2 | 0.9301 |
Si1—O1 | 1.626 (2) | C3—H3 | 0.9300 |
Si1—O2 | 1.634 (2) | C4—H4 | 0.9309 |
Si1—C1 | 1.865 (4) | C5—H5 | 0.9296 |
Si1—C7 | 1.858 (4) | C6—H6 | 0.9302 |
Si2—O3 | 1.634 (3) | C8—H8 | 0.9292 |
Si2—O4 | 1.641 (2) | C9—H9 | 0.9303 |
Si2—C13 | 1.873 (4) | C10—H10 | 0.9302 |
Si2—C19 | 1.840 (4) | C11—H11 | 0.9309 |
Si3—O5 | 1.632 (2) | C12—H12 | 0.9305 |
Si3—O6 | 1.634 (2) | C14—H14 | 0.9301 |
Si3—C25 | 1.864 (4) | C15—H15 | 0.9310 |
Si3—C31 | 1.872 (3) | C16—H16 | 0.9304 |
C1—C2 | 1.382 (5) | C17—H17 | 0.9300 |
C1—C6 | 1.393 (6) | C18—H18 | 0.9306 |
C2—C3 | 1.393 (6) | C20—H20 | 0.9295 |
C3—C4 | 1.352 (9) | C21—H21 | 0.9306 |
C4—C5 | 1.376 (10) | C22—H22 | 0.9298 |
C5—C6 | 1.400 (7) | C23—H23 | 0.9306 |
C7—C8 | 1.389 (5) | C24—H24 | 0.9306 |
C7—C12 | 1.386 (5) | C26—H26 | 0.9304 |
C8—C9 | 1.392 (6) | C27—H27 | 0.9300 |
C9—C10 | 1.358 (6) | C28—H28 | 0.9305 |
C10—C11 | 1.360 (5) | C29—H29 | 0.9295 |
C11—C12 | 1.379 (6) | C30—H30 | 0.9301 |
C13—C14 | 1.418 (5) | C32—H32 | 0.9300 |
C13—C18 | 1.376 (5) | C33—H33 | 0.9297 |
C14—C15 | 1.383 (6) | C34—H34 | 0.9297 |
C15—C16 | 1.368 (6) | C35—H35 | 0.9301 |
C16—C17 | 1.364 (7) | C36—H36 | 0.9296 |
C17—C18 | 1.398 (6) | C38—H38A | 0.9588 |
C19—C20 | 1.393 (6) | C38—H38B | 0.9606 |
C19—C24 | 1.380 (7) | C38—H38C | 0.9596 |
C20—C21 | 1.367 (8) | C39—H39A | 0.9611 |
C21—C22 | 1.384 (10) | C39—H39B | 0.9604 |
C22—C23 | 1.364 (9) | C39—H39C | 0.9593 |
C23—C24 | 1.400 (8) | C40—H40A | 0.9600 |
C25—C26 | 1.394 (5) | C40—H40B | 0.9590 |
C25—C30 | 1.389 (5) | C40—H40C | 0.9605 |
C26—C27 | 1.387 (6) | C42—H42A | 0.9596 |
C27—C28 | 1.379 (6) | C42—H42B | 0.9593 |
C28—C29 | 1.345 (6) | C42—H42C | 0.9601 |
C29—C30 | 1.387 (6) | C43—H43A | 0.9604 |
C31—C32 | 1.364 (6) | C43—H43B | 0.9594 |
C31—C36 | 1.374 (6) | C43—H43C | 0.9599 |
C32—C33 | 1.388 (7) | C44—H44A | 0.9603 |
C33—C34 | 1.354 (8) | C44—H44B | 0.9604 |
C34—C35 | 1.334 (6) | C44—H44C | 0.9589 |
Ge1···Ge2 | 3.8473 (18) | C26···H12 | 2.9344 |
Ge2···Ge1 | 3.8473 (18) | C30···H32 | 2.9529 |
Ge2···H36 | 3.2059 | C31···H14 | 2.8903 |
Si1···Si2 | 4.276 (2) | C35···H26viii | 3.0369 |
Si1···Si3 | 4.372 (2) | C36···H14 | 2.8762 |
Si2···Si1 | 4.276 (2) | C39···H2 | 2.9099 |
Si2···Si3 | 4.261 (2) | C43···H36 | 3.0480 |
Si3···Si1 | 4.372 (2) | H2···O2 | 2.7533 |
Si3···Si2 | 4.261 (2) | H2···C39 | 2.9099 |
Si3···H12 | 3.4387 | H2···H39A | 2.4770 |
O1···Si2 | 3.445 (3) | H2···H39B | 2.5068 |
O1···O4 | 2.831 (3) | H8···C1 | 2.9337 |
O1···O5 | 2.851 (3) | H8···C6 | 2.9757 |
O1···C41 | 3.019 (4) | H10···C4iv | 2.9413 |
O1···C44 | 3.228 (5) | H12···Si3 | 3.4387 |
O2···O6 | 2.851 (3) | H12···O5 | 2.6510 |
O2···Si3 | 3.612 (3) | H12···C26 | 2.9344 |
O2···O3 | 2.832 (3) | H12···H26 | 2.5962 |
O2···C37 | 3.062 (4) | H14···C31 | 2.8903 |
O2···C39 | 3.313 (6) | H14···C36 | 2.8762 |
O3···O2 | 2.832 (3) | H18···C19 | 2.9525 |
O3···C40 | 3.333 (6) | H18···C20 | 3.0553 |
O3···O6 | 2.805 (3) | H21···C7vi | 2.9365 |
O3···Si1 | 3.532 (3) | H21···C12vi | 2.9789 |
O3···C37 | 3.084 (4) | H24···O3 | 2.6996 |
O4···Si3 | 3.361 (3) | H24···C2 | 3.0545 |
O4···O1 | 2.831 (3) | H26···O5 | 2.8431 |
O4···C41 | 3.128 (4) | H26···H12 | 2.5962 |
O4···C42 | 3.385 (5) | H26···C35viii | 3.0369 |
O4···O5 | 2.782 (3) | H28···H43Av | 2.5722 |
O5···Si1 | 3.578 (3) | H29···C14v | 3.0967 |
O5···O1 | 2.851 (3) | H30···O6 | 2.8620 |
O5···O4 | 2.782 (3) | H30···H38A | 2.5148 |
O5···C41 | 3.108 (4) | H32···C25 | 3.0420 |
O5···C43 | 3.411 (5) | H32···C30 | 2.9529 |
O6···Si2 | 3.496 (3) | H36···Ge2 | 3.2059 |
O6···O3 | 2.805 (3) | H36···O4 | 2.9098 |
O6···C38 | 3.301 (5) | H36···O5 | 2.8320 |
O6···O2 | 2.851 (3) | H36···C43 | 3.0480 |
O6···C37 | 3.059 (4) | H36···H43A | 2.5186 |
O1···H44A | 2.7797 | H38A···O6 | 2.8764 |
O2···H39A | 2.8927 | H38A···H30 | 2.5148 |
O2···H2 | 2.7533 | H38A···H40A | 2.4535 |
O3···H24 | 2.6996 | H38B···H39A | 2.3969 |
O3···H40C | 2.9097 | H38C···C10ii | 3.0222 |
O4···H36 | 2.9098 | H38C···H39C | 2.4477 |
O5···H26 | 2.8431 | H38C···H40B | 2.5082 |
O5···H36 | 2.8320 | H39A···O2 | 2.8927 |
O5···H12 | 2.6510 | H39A···H2 | 2.4770 |
O6···H30 | 2.8620 | H39A···H38B | 2.3969 |
O6···H38A | 2.8764 | H39B···H2 | 2.5068 |
C18···C20 | 3.551 (6) | H39B···H40C | 2.5272 |
C20···C18 | 3.551 (6) | H39B···C23vii | 3.0757 |
C32···C33i | 3.533 (8) | H39C···H38C | 2.4477 |
C33···C32i | 3.533 (8) | H39C···H40B | 2.4973 |
C37···O3 | 3.084 (4) | H40A···H38A | 2.4535 |
C37···O2 | 3.062 (4) | H40B···H38C | 2.5082 |
C37···O6 | 3.059 (4) | H40B···H39C | 2.4973 |
C40···C44ii | 3.513 (8) | H40C···O3 | 2.9097 |
C41···O4 | 3.128 (4) | H40C···H39B | 2.5272 |
C41···O1 | 3.019 (4) | H42A···H44A | 2.4370 |
C41···O5 | 3.108 (4) | H42B···H43B | 2.5420 |
C44···C40iii | 3.513 (8) | H42B···H44C | 2.5858 |
C1···H8 | 2.9337 | H42C···H43A | 2.4922 |
C2···H24 | 3.0545 | H43A···H28vi | 2.5722 |
C4···H10iv | 2.9413 | H43A···H36 | 2.5186 |
C6···H8 | 2.9757 | H43A···H42C | 2.4922 |
C7···H21v | 2.9365 | H43B···H42B | 2.5420 |
C10···H38Ciii | 3.0222 | H43B···H44C | 2.5012 |
C12···H21v | 2.9789 | H43C···H44B | 2.5338 |
C14···H29vi | 3.0967 | H44A···O1 | 2.7797 |
C19···H18 | 2.9525 | H44A···H42A | 2.4370 |
C20···H18 | 3.0553 | H44B···H43C | 2.5338 |
C23···H39Bvii | 3.0757 | H44C···H42B | 2.5858 |
C25···H32 | 3.0420 | H44C···H43B | 2.5012 |
O2—Ge1—O3 | 107.36 (10) | C1—C2—H2 | 119.29 |
O2—Ge1—O6 | 108.17 (10) | C3—C2—H2 | 119.30 |
O2—Ge1—C37 | 111.42 (12) | C2—C3—H3 | 119.78 |
O3—Ge1—O6 | 105.75 (10) | C4—C3—H3 | 119.88 |
O3—Ge1—C37 | 112.73 (12) | C3—C4—H4 | 119.81 |
O6—Ge1—C37 | 111.11 (12) | C5—C4—H4 | 119.72 |
O1—Ge2—O4 | 107.13 (10) | C4—C5—H5 | 120.46 |
O1—Ge2—O5 | 107.83 (10) | C6—C5—H5 | 120.41 |
O1—Ge2—C41 | 109.11 (12) | C1—C6—H6 | 119.26 |
O4—Ge2—O5 | 103.97 (10) | C5—C6—H6 | 119.33 |
O4—Ge2—C41 | 114.96 (12) | C7—C8—H8 | 119.39 |
O5—Ge2—C41 | 113.41 (12) | C9—C8—H8 | 119.58 |
O1—Si1—O2 | 110.17 (12) | C8—C9—H9 | 119.56 |
O1—Si1—C1 | 107.09 (14) | C10—C9—H9 | 119.53 |
O1—Si1—C7 | 110.00 (14) | C9—C10—H10 | 120.27 |
O2—Si1—C1 | 110.34 (14) | C11—C10—H10 | 120.25 |
O2—Si1—C7 | 107.07 (14) | C10—C11—H11 | 120.12 |
C1—Si1—C7 | 112.19 (15) | C12—C11—H11 | 120.10 |
O3—Si2—O4 | 110.89 (12) | C7—C12—H12 | 118.55 |
O3—Si2—C13 | 109.98 (14) | C11—C12—H12 | 118.61 |
O3—Si2—C19 | 108.70 (14) | C13—C14—H14 | 119.06 |
O4—Si2—C13 | 106.18 (14) | C15—C14—H14 | 119.12 |
O4—Si2—C19 | 109.29 (14) | C14—C15—H15 | 120.19 |
C13—Si2—C19 | 111.80 (16) | C16—C15—H15 | 119.98 |
O5—Si3—O6 | 111.95 (11) | C15—C16—H16 | 119.93 |
O5—Si3—C25 | 109.21 (14) | C17—C16—H16 | 119.90 |
O5—Si3—C31 | 110.03 (14) | C16—C17—H17 | 119.84 |
O6—Si3—C25 | 108.10 (13) | C18—C17—H17 | 120.04 |
O6—Si3—C31 | 108.09 (13) | C13—C18—H18 | 119.02 |
C25—Si3—C31 | 109.41 (14) | C17—C18—H18 | 119.04 |
Ge2—O1—Si1 | 137.92 (14) | C19—C20—H20 | 118.70 |
Ge1—O2—Si1 | 135.70 (14) | C21—C20—H20 | 118.69 |
Ge1—O3—Si2 | 135.85 (14) | C20—C21—H21 | 120.71 |
Ge2—O4—Si2 | 133.33 (13) | C22—C21—H21 | 120.90 |
Ge2—O5—Si3 | 132.23 (13) | C21—C22—H22 | 119.25 |
Ge1—O6—Si3 | 138.32 (13) | C23—C22—H22 | 119.45 |
Si1—C1—C2 | 121.7 (3) | C22—C23—H23 | 120.39 |
Si1—C1—C6 | 121.2 (3) | C24—C23—H23 | 120.40 |
C2—C1—C6 | 117.1 (3) | C19—C24—H24 | 119.54 |
C1—C2—C3 | 121.4 (4) | C23—C24—H24 | 119.47 |
C2—C3—C4 | 120.3 (5) | C25—C26—H26 | 119.55 |
C3—C4—C5 | 120.5 (5) | C27—C26—H26 | 119.62 |
C4—C5—C6 | 119.1 (6) | C26—C27—H27 | 119.91 |
C1—C6—C5 | 121.4 (5) | C28—C27—H27 | 119.89 |
Si1—C7—C8 | 123.9 (3) | C27—C28—H28 | 120.08 |
Si1—C7—C12 | 120.1 (3) | C29—C28—H28 | 119.98 |
C8—C7—C12 | 115.9 (3) | C28—C29—H29 | 119.84 |
C7—C8—C9 | 121.0 (3) | C30—C29—H29 | 119.71 |
C8—C9—C10 | 120.9 (4) | C25—C30—H30 | 119.20 |
C9—C10—C11 | 119.5 (4) | C29—C30—H30 | 119.23 |
C10—C11—C12 | 119.8 (4) | C31—C32—H32 | 118.72 |
C7—C12—C11 | 122.8 (4) | C33—C32—H32 | 118.75 |
Si2—C13—C14 | 120.5 (3) | C32—C33—H33 | 120.02 |
Si2—C13—C18 | 123.4 (3) | C34—C33—H33 | 120.19 |
C14—C13—C18 | 116.1 (3) | C33—C34—H34 | 120.16 |
C13—C14—C15 | 121.8 (4) | C35—C34—H34 | 120.20 |
C14—C15—C16 | 119.8 (5) | C34—C35—H35 | 119.84 |
C15—C16—C17 | 120.2 (4) | C36—C35—H35 | 119.95 |
C16—C17—C18 | 120.1 (4) | C31—C36—H36 | 118.91 |
C13—C18—C17 | 121.9 (4) | C35—C36—H36 | 118.76 |
Si2—C19—C20 | 120.4 (3) | C37—C38—H38A | 109.50 |
Si2—C19—C24 | 122.0 (3) | C37—C38—H38B | 109.42 |
C20—C19—C24 | 117.4 (4) | C37—C38—H38C | 109.47 |
C19—C20—C21 | 122.6 (5) | H38A—C38—H38B | 109.46 |
C20—C21—C22 | 118.4 (5) | H38A—C38—H38C | 109.50 |
C21—C22—C23 | 121.3 (6) | H38B—C38—H38C | 109.48 |
C22—C23—C24 | 119.2 (5) | C37—C39—H39A | 109.51 |
C19—C24—C23 | 121.0 (4) | C37—C39—H39B | 109.50 |
Si3—C25—C26 | 122.6 (3) | C37—C39—H39C | 109.52 |
Si3—C25—C30 | 120.3 (3) | H39A—C39—H39B | 109.39 |
C26—C25—C30 | 117.0 (3) | H39A—C39—H39C | 109.46 |
C25—C26—C27 | 120.8 (3) | H39B—C39—H39C | 109.46 |
C26—C27—C28 | 120.2 (4) | C37—C40—H40A | 109.43 |
C27—C28—C29 | 119.9 (4) | C37—C40—H40B | 109.49 |
C28—C29—C30 | 120.5 (4) | C37—C40—H40C | 109.42 |
C25—C30—C29 | 121.6 (3) | H40A—C40—H40B | 109.53 |
Si3—C31—C32 | 121.3 (3) | H40A—C40—H40C | 109.42 |
Si3—C31—C36 | 123.2 (3) | H40B—C40—H40C | 109.54 |
C32—C31—C36 | 115.5 (3) | C41—C42—H42A | 109.44 |
C31—C32—C33 | 122.5 (5) | C41—C42—H42B | 109.51 |
C32—C33—C34 | 119.8 (5) | C41—C42—H42C | 109.42 |
C33—C34—C35 | 119.6 (4) | H42A—C42—H42B | 109.56 |
C34—C35—C36 | 120.2 (5) | H42A—C42—H42C | 109.43 |
C31—C36—C35 | 122.3 (4) | H42B—C42—H42C | 109.46 |
Ge1—C37—C38 | 107.9 (3) | C41—C43—H43A | 109.46 |
Ge1—C37—C39 | 109.7 (3) | C41—C43—H43B | 109.52 |
Ge1—C37—C40 | 108.8 (3) | C41—C43—H43C | 109.42 |
C38—C37—C39 | 107.6 (4) | H43A—C43—H43B | 109.48 |
C38—C37—C40 | 110.7 (4) | H43A—C43—H43C | 109.48 |
C39—C37—C40 | 112.0 (4) | H43B—C43—H43C | 109.47 |
Ge2—C41—C42 | 106.7 (3) | C41—C44—H44A | 109.40 |
Ge2—C41—C43 | 110.4 (2) | C41—C44—H44B | 109.45 |
Ge2—C41—C44 | 107.2 (3) | C41—C44—H44C | 109.58 |
C42—C41—C43 | 111.0 (4) | H44A—C44—H44B | 109.39 |
C42—C41—C44 | 110.0 (3) | H44A—C44—H44C | 109.46 |
C43—C41—C44 | 111.4 (3) | H44B—C44—H44C | 109.54 |
O3—Ge1—C37—C40 | −46.6 (4) | C19—Si2—C13—C14 | −161.0 (3) |
O6—Ge1—C37—C40 | 71.9 (4) | O4—Si2—C19—C20 | −62.5 (3) |
C37—Ge1—O6—Si3 | 143.6 (2) | C13—Si2—C19—C24 | −130.1 (4) |
O2—Ge1—C37—C40 | −167.4 (3) | C25—Si3—C31—C32 | −42.5 (4) |
O2—Ge1—C37—C38 | 72.4 (3) | C25—Si3—O5—Ge2 | 156.70 (17) |
O2—Ge1—O3—Si2 | −92.4 (2) | O6—Si3—C31—C32 | 75.0 (4) |
O3—Ge1—O2—Si1 | 21.7 (2) | O6—Si3—O5—Ge2 | 37.0 (2) |
O6—Ge1—O2—Si1 | −92.01 (19) | O5—Si3—C25—C30 | −159.5 (3) |
C37—Ge1—O2—Si1 | 145.58 (19) | C31—Si3—O5—Ge2 | −83.2 (2) |
O3—Ge1—O6—Si3 | −93.8 (2) | O5—Si3—C31—C36 | 18.4 (4) |
O6—Ge1—C37—C39 | −165.2 (3) | C25—Si3—C31—C36 | 138.4 (3) |
C37—Ge1—O3—Si2 | 144.5 (2) | C31—Si3—C25—C26 | −97.0 (3) |
O2—Ge1—O6—Si3 | 21.0 (2) | O5—Si3—O6—Ge1 | 26.9 (3) |
O6—Ge1—O3—Si2 | 22.9 (2) | C25—Si3—O6—Ge1 | −93.4 (2) |
O3—Ge1—C37—C39 | 76.3 (4) | C31—Si3—O6—Ge1 | 148.2 (2) |
O6—Ge1—C37—C38 | −48.3 (3) | O5—Si3—C31—C32 | −162.5 (3) |
O2—Ge1—C37—C39 | −44.5 (4) | O6—Si3—C31—C36 | −104.1 (3) |
O3—Ge1—C37—C38 | −166.8 (3) | O6—Si3—C25—C26 | 145.5 (3) |
O1—Ge2—C41—C43 | −168.4 (3) | O5—Si3—C25—C26 | 23.4 (3) |
O4—Ge2—C41—C44 | −167.3 (3) | C31—Si3—C25—C30 | 80.0 (3) |
O5—Ge2—C41—C42 | −168.9 (2) | O6—Si3—C25—C30 | −37.4 (3) |
O4—Ge2—C41—C42 | −49.5 (3) | Si1—C1—C2—C3 | 175.5 (4) |
O5—Ge2—O4—Si2 | −106.06 (19) | Si1—C1—C6—C5 | −177.0 (4) |
O1—Ge2—C41—C44 | −47.0 (3) | C2—C1—C6—C5 | 2.2 (6) |
O5—Ge2—C41—C44 | 73.2 (3) | C6—C1—C2—C3 | −3.7 (7) |
O4—Ge2—O5—Si3 | 18.19 (19) | C1—C2—C3—C4 | 2.1 (8) |
C41—Ge2—O1—Si1 | 140.2 (2) | C2—C3—C4—C5 | 1.2 (9) |
C41—Ge2—O4—Si2 | 129.38 (19) | C3—C4—C5—C6 | −2.6 (9) |
O1—Ge2—C41—C42 | 70.8 (3) | C4—C5—C6—C1 | 0.9 (8) |
C41—Ge2—O5—Si3 | 143.75 (18) | C12—C7—C8—C9 | 2.2 (6) |
O1—Ge2—O4—Si2 | 8.0 (2) | Si1—C7—C8—C9 | −176.0 (3) |
O1—Ge2—O5—Si3 | −95.31 (18) | Si1—C7—C12—C11 | 176.1 (3) |
O4—Ge2—O1—Si1 | −94.7 (2) | C8—C7—C12—C11 | −2.2 (6) |
O4—Ge2—C41—C43 | 71.2 (3) | C7—C8—C9—C10 | −0.9 (6) |
O5—Ge2—O1—Si1 | 16.6 (2) | C8—C9—C10—C11 | −0.6 (6) |
O5—Ge2—C41—C43 | −48.2 (3) | C9—C10—C11—C12 | 0.6 (6) |
O2—Si1—C7—C12 | −57.0 (3) | C10—C11—C12—C7 | 0.9 (7) |
O2—Si1—C1—C2 | −3.4 (4) | Si2—C13—C18—C17 | −176.5 (3) |
O1—Si1—C7—C12 | 62.7 (3) | Si2—C13—C14—C15 | 177.0 (3) |
O1—Si1—C1—C2 | −123.4 (3) | C18—C13—C14—C15 | −0.7 (6) |
O2—Si1—C7—C8 | 121.2 (3) | C14—C13—C18—C17 | 1.1 (6) |
C7—Si1—C1—C2 | 115.9 (4) | C13—C14—C15—C16 | 0.1 (7) |
C1—Si1—C7—C8 | 0.0 (4) | C14—C15—C16—C17 | 0.1 (7) |
C1—Si1—O2—Ge1 | −88.1 (2) | C15—C16—C17—C18 | 0.2 (7) |
C7—Si1—C1—C6 | −65.0 (4) | C16—C17—C18—C13 | −0.9 (6) |
O2—Si1—O1—Ge2 | 35.9 (2) | C24—C19—C20—C21 | −0.6 (7) |
C1—Si1—O1—Ge2 | 155.9 (2) | Si2—C19—C20—C21 | 174.8 (4) |
C7—Si1—O1—Ge2 | −81.9 (2) | Si2—C19—C24—C23 | −173.0 (4) |
C7—Si1—O2—Ge1 | 149.51 (18) | C20—C19—C24—C23 | 2.4 (7) |
O2—Si1—C1—C6 | 175.7 (3) | C19—C20—C21—C22 | −1.8 (8) |
O1—Si1—C7—C8 | −119.1 (3) | C20—C21—C22—C23 | 2.6 (9) |
O1—Si1—O2—Ge1 | 29.9 (2) | C21—C22—C23—C24 | −0.9 (9) |
C1—Si1—C7—C12 | −178.2 (3) | C22—C23—C24—C19 | −1.7 (9) |
O1—Si1—C1—C6 | 55.8 (3) | Si3—C25—C26—C27 | 178.3 (3) |
O4—Si2—O3—Ge1 | 23.3 (2) | C30—C25—C26—C27 | 1.1 (5) |
O4—Si2—C13—C14 | −41.9 (3) | C26—C25—C30—C29 | −0.6 (5) |
C13—Si2—O3—Ge1 | −93.8 (2) | Si3—C25—C30—C29 | −177.8 (3) |
C19—Si2—O3—Ge1 | 143.5 (2) | C25—C26—C27—C28 | −0.8 (5) |
O3—Si2—C13—C14 | 78.1 (3) | C26—C27—C28—C29 | −0.2 (6) |
O3—Si2—C19—C20 | 176.3 (3) | C27—C28—C29—C30 | 0.8 (6) |
O3—Si2—O4—Ge2 | 45.1 (2) | C28—C29—C30—C25 | −0.4 (6) |
C13—Si2—O4—Ge2 | 164.59 (18) | Si3—C31—C32—C33 | −177.3 (4) |
O4—Si2—C19—C24 | 112.6 (4) | C32—C31—C36—C35 | −2.8 (6) |
C13—Si2—C19—C20 | 54.7 (4) | C36—C31—C32—C33 | 1.9 (7) |
C19—Si2—C13—C18 | 16.5 (4) | Si3—C31—C36—C35 | 176.4 (3) |
O4—Si2—C13—C18 | 135.6 (3) | C31—C32—C33—C34 | 0.0 (8) |
C19—Si2—O4—Ge2 | −74.7 (2) | C32—C33—C34—C35 | −1.2 (8) |
O3—Si2—C19—C24 | −8.5 (4) | C33—C34—C35—C36 | 0.4 (7) |
O3—Si2—C13—C18 | −104.4 (3) | C34—C35—C36—C31 | 1.7 (7) |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) x, y−1, z; (iii) x, y+1, z; (iv) −x+1, −y+1, −z+1; (v) x+1, y, z; (vi) x−1, y, z; (vii) −x, −y, −z+1; (viii) −x+1, −y+1, −z+2. |