Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806024019/hy2006sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806024019/hy2006IVsup2.hkl |
CCDC reference: 613733
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Li4(C40H28N4Si)(C4H8O)4(C4H10O)2]·C4H10O | F(000) = 2432 |
Mr = 1131.29 | Dx = 1.186 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 21125 reflections |
a = 27.561 (6) Å | θ = 4.0–27.5° |
b = 14.829 (3) Å | µ = 0.09 mm−1 |
c = 17.617 (4) Å | T = 173 K |
β = 118.38 (3)° | Block, yellow |
V = 6335 (3) Å3 | 0.12 × 0.09 × 0.08 mm |
Z = 4 |
Nonius KappaCCD area-detector diffractometer | 5558 independent reflections |
Radiation source: fine-focus sealed tube | 4207 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
φ and ω scans | θmax = 25.0°, θmin = 3.4° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | h = −32→32 |
Tmin = 0.992, Tmax = 0.995 | k = −17→17 |
21125 measured reflections | l = −20→20 |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0597P)2 + 4.7032P] where P = (Fo2 + 2Fc2)/3 |
5558 reflections | (Δ/σ)max < 0.001 |
408 parameters | Δρmax = 0.22 e Å−3 |
10 restraints | Δρmin = −0.25 e Å−3 |
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) | |
Si1 | 0.0000 | 0.75043 (4) | 0.2500 | 0.02881 (17) | |
N1 | 0.04134 (5) | 0.82548 (9) | 0.33046 (9) | 0.0316 (3) | |
N2 | 0.04190 (5) | 0.67491 (9) | 0.23257 (9) | 0.0315 (3) | |
Li1 | 0.0000 | 0.9285 (3) | 0.2500 | 0.0398 (10) | |
Li2 | 0.0000 | 0.5711 (3) | 0.2500 | 0.0386 (9) | |
Li3 | 0.10647 (13) | 0.7433 (3) | 0.3353 (2) | 0.0594 (10) | |
O1 | 0.03638 (6) | 1.01496 (10) | 0.20607 (9) | 0.0569 (4) | |
O2 | 0.03680 (6) | 0.48343 (9) | 0.34757 (9) | 0.0524 (4) | |
O3 | 0.18486 (5) | 0.74258 (13) | 0.38180 (10) | 0.0674 (5) | |
C1 | 0.07117 (7) | 0.80652 (12) | 0.41674 (11) | 0.0332 (4) | |
C2 | 0.07163 (8) | 0.72251 (13) | 0.45369 (12) | 0.0408 (4) | |
H2 | 0.0476 | 0.6766 | 0.4179 | 0.049* | |
C3 | 0.10594 (8) | 0.70337 (15) | 0.54117 (13) | 0.0489 (5) | |
H3 | 0.1047 | 0.6450 | 0.5624 | 0.059* | |
C4 | 0.14102 (9) | 0.76601 (15) | 0.59652 (13) | 0.0519 (5) | |
H4 | 0.1645 | 0.7511 | 0.6553 | 0.062* | |
C5 | 0.14222 (7) | 0.85367 (14) | 0.56564 (12) | 0.0433 (5) | |
C6 | 0.10794 (7) | 0.87457 (12) | 0.47665 (11) | 0.0355 (4) | |
C7 | 0.11090 (8) | 0.96203 (13) | 0.44824 (13) | 0.0439 (5) | |
H7 | 0.0884 | 0.9769 | 0.3892 | 0.053* | |
C8 | 0.14536 (9) | 1.02662 (15) | 0.50350 (15) | 0.0540 (5) | |
H8 | 0.1466 | 1.0852 | 0.4826 | 0.065* | |
C9 | 0.17884 (8) | 1.00561 (16) | 0.59127 (15) | 0.0563 (6) | |
H9 | 0.2026 | 1.0501 | 0.6298 | 0.068* | |
C10 | 0.17717 (8) | 0.92215 (16) | 0.62083 (13) | 0.0520 (5) | |
H10 | 0.2000 | 0.9090 | 0.6802 | 0.062* | |
C11 | 0.07147 (7) | 0.69335 (12) | 0.18978 (11) | 0.0346 (4) | |
C12 | 0.10788 (7) | 0.62473 (13) | 0.18483 (12) | 0.0377 (4) | |
C13 | 0.14245 (8) | 0.64506 (15) | 0.14686 (13) | 0.0487 (5) | |
C14 | 0.14055 (9) | 0.73166 (16) | 0.11258 (15) | 0.0592 (6) | |
H14 | 0.1638 | 0.7461 | 0.0882 | 0.071* | |
C15 | 0.10509 (9) | 0.79472 (16) | 0.11463 (15) | 0.0541 (5) | |
H15 | 0.1033 | 0.8524 | 0.0900 | 0.065* | |
C16 | 0.07128 (8) | 0.77661 (13) | 0.15209 (13) | 0.0421 (5) | |
H16 | 0.0472 | 0.8226 | 0.1519 | 0.051* | |
C17 | 0.11044 (8) | 0.53766 (13) | 0.21780 (13) | 0.0434 (5) | |
H17 | 0.0877 | 0.5234 | 0.2431 | 0.052* | |
C18 | 0.14481 (8) | 0.47231 (15) | 0.21461 (15) | 0.0547 (6) | |
H18 | 0.1455 | 0.4139 | 0.2372 | 0.066* | |
C19 | 0.17892 (9) | 0.49229 (18) | 0.17781 (16) | 0.0619 (7) | |
H19 | 0.2029 | 0.4475 | 0.1757 | 0.074* | |
C20 | 0.17756 (9) | 0.57572 (18) | 0.14522 (16) | 0.0600 (6) | |
H20 | 0.2008 | 0.5882 | 0.1205 | 0.072* | |
C21 | 0.06770 (12) | 1.09288 (17) | 0.25051 (17) | 0.0726 (7) | |
H21A | 0.1076 | 1.0785 | 0.2810 | 0.087* | |
H21B | 0.0567 | 1.1139 | 0.2934 | 0.087* | |
C22 | 0.05618 (17) | 1.1630 (2) | 0.18486 (18) | 0.0998 (11) | |
H22A | 0.0909 | 1.1846 | 0.1874 | 0.120* | |
H22B | 0.0371 | 1.2149 | 0.1943 | 0.120* | |
C23 | 0.01952 (11) | 1.11893 (16) | 0.09809 (16) | 0.0648 (6) | |
H23A | −0.0197 | 1.1350 | 0.0766 | 0.078* | |
H23B | 0.0308 | 1.1364 | 0.0545 | 0.078* | |
C24 | 0.02920 (10) | 1.02049 (15) | 0.11919 (14) | 0.0536 (5) | |
H24A | −0.0028 | 0.9841 | 0.0786 | 0.064* | |
H24B | 0.0626 | 0.9993 | 0.1171 | 0.064* | |
C25 | 0.06727 (11) | 0.40443 (16) | 0.34822 (18) | 0.0685 (7) | |
H25A | 0.1071 | 0.4184 | 0.3749 | 0.082* | |
H25B | 0.0548 | 0.3831 | 0.2886 | 0.082* | |
C26 | 0.05719 (18) | 0.3353 (2) | 0.3981 (2) | 0.1059 (12) | |
H26A | 0.0924 | 0.3145 | 0.4467 | 0.127* | |
H26B | 0.0381 | 0.2829 | 0.3612 | 0.127* | |
C27 | 0.02103 (12) | 0.37965 (16) | 0.43177 (17) | 0.0689 (7) | |
H27A | −0.0182 | 0.3631 | 0.3961 | 0.083* | |
H27B | 0.0331 | 0.3628 | 0.4925 | 0.083* | |
C28 | 0.03017 (9) | 0.47799 (15) | 0.42365 (13) | 0.0521 (5) | |
H28A | −0.0019 | 0.5141 | 0.4168 | 0.063* | |
H28B | 0.0636 | 0.4998 | 0.4750 | 0.063* | |
C29 | 0.21301 (10) | 0.6572 (2) | 0.40506 (18) | 0.0808 (9) | |
H29A | 0.2520 | 0.6664 | 0.4489 | 0.097* | |
H29B | 0.2124 | 0.6290 | 0.3537 | 0.097* | |
C30 | 0.18507 (12) | 0.5965 (2) | 0.44069 (19) | 0.0881 (9) | |
H30A | 0.1850 | 0.6254 | 0.4907 | 0.132* | |
H30B | 0.2050 | 0.5391 | 0.4584 | 0.132* | |
H30C | 0.1470 | 0.5854 | 0.3962 | 0.132* | |
C31 | 0.20885 (10) | 0.8024 (2) | 0.34445 (19) | 0.0830 (9) | |
H31A | 0.2017 | 0.7793 | 0.2873 | 0.100* | |
H31B | 0.2493 | 0.8055 | 0.3820 | 0.100* | |
C32 | 0.18436 (11) | 0.8944 (2) | 0.3346 (2) | 0.0872 (9) | |
H32A | 0.1443 | 0.8910 | 0.2979 | 0.131* | |
H32B | 0.2002 | 0.9348 | 0.3081 | 0.131* | |
H32C | 0.1925 | 0.9178 | 0.3915 | 0.131* | |
O4 | 0.2316 (3) | 0.7582 (7) | 0.0110 (6) | 0.089 (2) | 0.30 |
C41 | 0.2798 (6) | 0.7038 (10) | 0.0732 (9) | 0.112 (4)* | 0.30 |
H41A | 0.3084 | 0.6953 | 0.0551 | 0.135* | 0.30 |
H41B | 0.2693 | 0.6453 | 0.0884 | 0.135* | 0.30 |
C40 | 0.2939 (7) | 0.7749 (11) | 0.1407 (10) | 0.111 (5)* | 0.30 |
H40A | 0.3264 | 0.7561 | 0.1939 | 0.167* | 0.30 |
H40B | 0.2627 | 0.7834 | 0.1522 | 0.167* | 0.30 |
H40C | 0.3017 | 0.8317 | 0.1203 | 0.167* | 0.30 |
C42 | 0.2229 (11) | 0.7094 (17) | −0.0681 (9) | 0.144 (5)* | 0.30 |
H42A | 0.2558 | 0.7138 | −0.0766 | 0.173* | 0.30 |
H42B | 0.2145 | 0.6449 | −0.0651 | 0.173* | 0.30 |
C43 | 0.1774 (6) | 0.7537 (11) | −0.1349 (12) | 0.097 (5)* | 0.30 |
H43A | 0.1679 | 0.7245 | −0.1901 | 0.146* | 0.30 |
H43B | 0.1868 | 0.8170 | −0.1372 | 0.146* | 0.30 |
H43C | 0.1458 | 0.7505 | −0.1239 | 0.146* | 0.30 |
O5 | 0.2594 (9) | 0.8068 (12) | −0.0137 (10) | 0.131 (6) | 0.20 |
C52 | 0.2749 (15) | 0.813 (2) | 0.0786 (12) | 0.144 (5)* | 0.20 |
H52A | 0.2411 | 0.8177 | 0.0846 | 0.173* | 0.20 |
H52B | 0.2971 | 0.8678 | 0.1033 | 0.173* | 0.20 |
C53 | 0.3072 (15) | 0.733 (2) | 0.128 (2) | 0.111 (5)* | 0.20 |
H53A | 0.3156 | 0.7381 | 0.1883 | 0.167* | 0.20 |
H53B | 0.3417 | 0.7292 | 0.1246 | 0.167* | 0.20 |
H53C | 0.2856 | 0.6777 | 0.1030 | 0.167* | 0.20 |
C51 | 0.2151 (13) | 0.748 (2) | −0.0602 (15) | 0.150 (12)* | 0.20 |
H51A | 0.1825 | 0.7629 | −0.0529 | 0.180* | 0.20 |
H51B | 0.2253 | 0.6842 | −0.0460 | 0.180* | 0.20 |
C50 | 0.2068 (10) | 0.7738 (19) | −0.1504 (15) | 0.114 (8)* | 0.20 |
H50A | 0.1756 | 0.7399 | −0.1944 | 0.172* | 0.20 |
H50B | 0.2403 | 0.7592 | −0.1542 | 0.172* | 0.20 |
H50C | 0.1993 | 0.8386 | −0.1599 | 0.172* | 0.20 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Si1 | 0.0280 (3) | 0.0325 (4) | 0.0266 (3) | 0.000 | 0.0135 (3) | 0.000 |
N1 | 0.0311 (7) | 0.0360 (8) | 0.0270 (8) | −0.0007 (6) | 0.0133 (6) | −0.0006 (6) |
N2 | 0.0309 (7) | 0.0362 (8) | 0.0299 (8) | −0.0005 (6) | 0.0164 (6) | −0.0016 (6) |
Li1 | 0.048 (2) | 0.037 (2) | 0.035 (2) | 0.000 | 0.019 (2) | 0.000 |
Li2 | 0.046 (2) | 0.034 (2) | 0.040 (2) | 0.000 | 0.024 (2) | 0.000 |
Li3 | 0.0338 (17) | 0.086 (3) | 0.053 (2) | −0.0017 (17) | 0.0165 (15) | −0.029 (2) |
O1 | 0.0746 (10) | 0.0478 (8) | 0.0480 (9) | −0.0172 (7) | 0.0289 (8) | 0.0019 (7) |
O2 | 0.0666 (9) | 0.0468 (8) | 0.0521 (9) | 0.0135 (7) | 0.0348 (8) | 0.0125 (7) |
O3 | 0.0306 (7) | 0.1061 (13) | 0.0603 (10) | 0.0004 (8) | 0.0173 (7) | −0.0296 (9) |
C1 | 0.0305 (9) | 0.0417 (10) | 0.0284 (9) | 0.0035 (7) | 0.0146 (7) | −0.0018 (7) |
C2 | 0.0430 (10) | 0.0429 (11) | 0.0327 (10) | 0.0016 (8) | 0.0148 (8) | 0.0016 (8) |
C3 | 0.0545 (12) | 0.0513 (12) | 0.0358 (11) | 0.0081 (10) | 0.0174 (9) | 0.0073 (9) |
C4 | 0.0500 (12) | 0.0659 (15) | 0.0298 (10) | 0.0132 (10) | 0.0107 (9) | 0.0027 (10) |
C5 | 0.0347 (10) | 0.0597 (13) | 0.0317 (10) | 0.0062 (9) | 0.0127 (8) | −0.0083 (9) |
C6 | 0.0305 (9) | 0.0444 (11) | 0.0322 (10) | 0.0032 (7) | 0.0155 (8) | −0.0065 (8) |
C7 | 0.0411 (10) | 0.0492 (12) | 0.0399 (11) | −0.0036 (9) | 0.0181 (9) | −0.0095 (9) |
C8 | 0.0527 (12) | 0.0513 (13) | 0.0559 (14) | −0.0093 (10) | 0.0241 (11) | −0.0152 (10) |
C9 | 0.0413 (11) | 0.0671 (16) | 0.0530 (14) | −0.0070 (10) | 0.0162 (10) | −0.0277 (12) |
C10 | 0.0380 (11) | 0.0703 (15) | 0.0369 (11) | 0.0049 (10) | 0.0090 (9) | −0.0167 (10) |
C11 | 0.0308 (9) | 0.0434 (11) | 0.0313 (9) | −0.0042 (7) | 0.0161 (7) | −0.0061 (8) |
C12 | 0.0313 (9) | 0.0468 (11) | 0.0356 (10) | −0.0050 (8) | 0.0164 (8) | −0.0116 (8) |
C13 | 0.0402 (10) | 0.0650 (14) | 0.0480 (12) | −0.0091 (9) | 0.0269 (9) | −0.0172 (10) |
C14 | 0.0592 (13) | 0.0734 (16) | 0.0673 (15) | −0.0146 (12) | 0.0483 (12) | −0.0099 (12) |
C15 | 0.0593 (13) | 0.0588 (13) | 0.0596 (14) | −0.0088 (11) | 0.0406 (12) | 0.0010 (11) |
C16 | 0.0437 (10) | 0.0451 (11) | 0.0458 (11) | −0.0034 (8) | 0.0280 (9) | 0.0002 (9) |
C17 | 0.0366 (10) | 0.0500 (12) | 0.0442 (11) | 0.0013 (8) | 0.0196 (9) | −0.0097 (9) |
C18 | 0.0470 (12) | 0.0519 (13) | 0.0615 (14) | 0.0055 (10) | 0.0229 (11) | −0.0143 (11) |
C19 | 0.0408 (12) | 0.0730 (17) | 0.0713 (16) | 0.0037 (11) | 0.0261 (11) | −0.0292 (13) |
C20 | 0.0452 (12) | 0.0787 (17) | 0.0683 (15) | −0.0076 (11) | 0.0370 (11) | −0.0278 (13) |
C21 | 0.0883 (18) | 0.0601 (15) | 0.0608 (15) | −0.0277 (13) | 0.0285 (14) | −0.0021 (12) |
C22 | 0.168 (3) | 0.0685 (18) | 0.0626 (18) | −0.043 (2) | 0.055 (2) | −0.0031 (14) |
C23 | 0.0844 (17) | 0.0617 (15) | 0.0556 (14) | −0.0054 (13) | 0.0393 (13) | 0.0079 (12) |
C24 | 0.0630 (14) | 0.0565 (13) | 0.0520 (13) | −0.0055 (10) | 0.0361 (11) | −0.0026 (10) |
C25 | 0.0840 (17) | 0.0555 (14) | 0.0796 (17) | 0.0248 (12) | 0.0500 (15) | 0.0188 (13) |
C26 | 0.186 (4) | 0.0680 (19) | 0.120 (3) | 0.047 (2) | 0.119 (3) | 0.0392 (18) |
C27 | 0.0985 (19) | 0.0582 (15) | 0.0638 (16) | 0.0070 (13) | 0.0498 (15) | 0.0143 (12) |
C28 | 0.0601 (13) | 0.0542 (13) | 0.0393 (11) | 0.0056 (10) | 0.0215 (10) | 0.0013 (10) |
C29 | 0.0376 (12) | 0.123 (2) | 0.0655 (17) | 0.0158 (14) | 0.0114 (12) | −0.0328 (16) |
C30 | 0.0631 (16) | 0.110 (2) | 0.0699 (18) | 0.0145 (16) | 0.0144 (14) | −0.0241 (17) |
C31 | 0.0433 (13) | 0.131 (3) | 0.0793 (19) | −0.0164 (15) | 0.0326 (13) | −0.0436 (18) |
C32 | 0.0622 (16) | 0.116 (3) | 0.089 (2) | −0.0187 (16) | 0.0411 (15) | −0.0313 (18) |
O4 | 0.066 (5) | 0.097 (6) | 0.075 (5) | −0.014 (4) | 0.011 (4) | 0.001 (5) |
O5 | 0.174 (16) | 0.144 (15) | 0.086 (10) | −0.011 (14) | 0.071 (11) | 0.012 (11) |
Si1—N1 | 1.7352 (15) | C21—C22 | 1.473 (4) |
Si1—N1i | 1.7352 (15) | C21—H21A | 0.9900 |
Si1—N2 | 1.7375 (14) | C21—H21B | 0.9900 |
Si1—N2i | 1.7375 (14) | C22—C23 | 1.522 (4) |
N1—C1 | 1.370 (2) | C22—H22A | 0.9900 |
N1—Li1 | 2.026 (4) | C22—H22B | 0.9900 |
N1—Li3 | 2.138 (4) | C23—C24 | 1.499 (3) |
N2—C11 | 1.375 (2) | C23—H23A | 0.9900 |
N2—Li2 | 2.033 (3) | C23—H23B | 0.9900 |
N2—Li3 | 2.100 (4) | C24—H24A | 0.9900 |
Li1—O1i | 1.997 (3) | C24—H24B | 0.9900 |
Li1—O1 | 1.997 (3) | C25—C26 | 1.460 (4) |
Li1—N1i | 2.026 (4) | C25—H25A | 0.9900 |
Li2—O2i | 2.004 (3) | C25—H25B | 0.9900 |
Li2—O2 | 2.004 (3) | C26—C27 | 1.529 (4) |
Li2—N2i | 2.033 (3) | C26—H26A | 0.9900 |
Li3—O3 | 1.912 (4) | C26—H26B | 0.9900 |
Li3—C1 | 2.282 (4) | C27—C28 | 1.498 (3) |
Li3—C11 | 2.388 (4) | C27—H27A | 0.9900 |
Li3—C2 | 2.696 (4) | C27—H27B | 0.9900 |
O1—C21 | 1.432 (3) | C28—H28A | 0.9900 |
O1—C24 | 1.449 (3) | C28—H28B | 0.9900 |
O2—C25 | 1.438 (3) | C29—C30 | 1.502 (4) |
O2—C28 | 1.438 (2) | C29—H29A | 0.9900 |
O3—C29 | 1.439 (3) | C29—H29B | 0.9900 |
O3—C31 | 1.439 (3) | C30—H30A | 0.9800 |
C1—C2 | 1.403 (3) | C30—H30B | 0.9800 |
C1—C6 | 1.464 (2) | C30—H30C | 0.9800 |
C2—C3 | 1.402 (3) | C31—C32 | 1.495 (4) |
C2—H2 | 0.9500 | C31—H31A | 0.9900 |
C3—C4 | 1.361 (3) | C31—H31B | 0.9900 |
C3—H3 | 0.9500 | C32—H32A | 0.9800 |
C4—C5 | 1.416 (3) | C32—H32B | 0.9800 |
C4—H4 | 0.9500 | C32—H32C | 0.9800 |
C5—C10 | 1.419 (3) | O4—C42 | 1.486 (17) |
C5—C6 | 1.428 (3) | O4—C41 | 1.493 (14) |
C6—C7 | 1.406 (3) | C41—C40 | 1.496 (15) |
C7—C8 | 1.374 (3) | C41—H41A | 0.9900 |
C7—H7 | 0.9500 | C41—H41B | 0.9900 |
C8—C9 | 1.408 (3) | C40—H40A | 0.9800 |
C8—H8 | 0.9500 | C40—H40B | 0.9800 |
C9—C10 | 1.352 (3) | C40—H40C | 0.9800 |
C9—H9 | 0.9500 | C42—C43 | 1.410 (16) |
C10—H10 | 0.9500 | C42—H42A | 0.9900 |
C11—C16 | 1.401 (3) | C42—H42B | 0.9900 |
C11—C12 | 1.461 (2) | C43—H43A | 0.9800 |
C12—C17 | 1.404 (3) | C43—H43B | 0.9800 |
C12—C13 | 1.433 (3) | C43—H43C | 0.9800 |
C13—C14 | 1.409 (3) | O5—C51 | 1.401 (17) |
C13—C20 | 1.422 (3) | O5—C52 | 1.473 (17) |
C14—C15 | 1.365 (3) | C52—C53 | 1.491 (19) |
C14—H14 | 0.9500 | C52—H52A | 0.9900 |
C15—C16 | 1.400 (3) | C52—H52B | 0.9900 |
C15—H15 | 0.9500 | C53—H53A | 0.9800 |
C16—H16 | 0.9500 | C53—H53B | 0.9800 |
C17—C18 | 1.375 (3) | C53—H53C | 0.9800 |
C17—H17 | 0.9500 | C51—C50 | 1.541 (19) |
C18—C19 | 1.404 (3) | C51—H51A | 0.9900 |
C18—H18 | 0.9500 | C51—H51B | 0.9900 |
C19—C20 | 1.357 (4) | C50—H50A | 0.9800 |
C19—H19 | 0.9500 | C50—H50B | 0.9800 |
C20—H20 | 0.9500 | C50—H50C | 0.9800 |
N1—Si1—N1i | 100.20 (10) | O1—C21—C22 | 106.9 (2) |
N1—Si1—N2 | 108.92 (7) | O1—C21—H21A | 110.3 |
N1i—Si1—N2 | 120.17 (7) | C22—C21—H21A | 110.3 |
N1—Si1—N2i | 120.17 (7) | O1—C21—H21B | 110.3 |
N1i—Si1—N2i | 108.92 (7) | C22—C21—H21B | 110.3 |
N2—Si1—N2i | 99.75 (10) | H21A—C21—H21B | 108.6 |
C1—N1—Si1 | 126.11 (12) | C21—C22—C23 | 106.1 (2) |
C1—N1—Li1 | 140.56 (14) | C21—C22—H22A | 110.5 |
Si1—N1—Li1 | 88.83 (10) | C23—C22—H22A | 110.5 |
C1—N1—Li3 | 77.80 (14) | C21—C22—H22B | 110.5 |
Si1—N1—Li3 | 83.09 (11) | C23—C22—H22B | 110.5 |
Li1—N1—Li3 | 129.81 (14) | H22A—C22—H22B | 108.7 |
C11—N2—Si1 | 125.84 (12) | C24—C23—C22 | 102.4 (2) |
C11—N2—Li2 | 139.50 (14) | C24—C23—H23A | 111.3 |
Si1—N2—Li2 | 89.33 (10) | C22—C23—H23A | 111.3 |
C11—N2—Li3 | 84.06 (14) | C24—C23—H23B | 111.3 |
Si1—N2—Li3 | 84.18 (11) | C22—C23—H23B | 111.3 |
Li2—N2—Li3 | 123.00 (14) | H23A—C23—H23B | 109.2 |
O1i—Li1—O1 | 100.1 (2) | O1—C24—C23 | 103.65 (17) |
O1i—Li1—N1i | 122.44 (7) | O1—C24—H24A | 111.0 |
O1—Li1—N1i | 115.59 (6) | C23—C24—H24A | 111.0 |
O1i—Li1—N1 | 115.59 (6) | O1—C24—H24B | 111.0 |
O1—Li1—N1 | 122.44 (7) | C23—C24—H24B | 111.0 |
N1i—Li1—N1 | 82.14 (18) | H24A—C24—H24B | 109.0 |
O2i—Li2—O2 | 99.1 (2) | O2—C25—C26 | 107.4 (2) |
O2i—Li2—N2i | 121.90 (7) | O2—C25—H25A | 110.2 |
O2—Li2—N2i | 116.99 (6) | C26—C25—H25A | 110.2 |
O2i—Li2—N2 | 116.99 (6) | O2—C25—H25B | 110.2 |
O2—Li2—N2 | 121.90 (7) | C26—C25—H25B | 110.2 |
N2i—Li2—N2 | 81.60 (17) | H25A—C25—H25B | 108.5 |
O3—Li3—N2 | 133.52 (19) | C25—C26—C27 | 106.1 (2) |
O3—Li3—N1 | 140.9 (2) | C25—C26—H26A | 110.5 |
N2—Li3—N1 | 83.65 (13) | C27—C26—H26A | 110.5 |
O3—Li3—C1 | 117.74 (17) | C25—C26—H26B | 110.5 |
N2—Li3—C1 | 107.48 (15) | C27—C26—H26B | 110.5 |
N1—Li3—C1 | 35.92 (8) | H26A—C26—H26B | 108.7 |
O3—Li3—C11 | 104.81 (16) | C28—C27—C26 | 102.2 (2) |
N2—Li3—C11 | 34.95 (8) | C28—C27—H27A | 111.3 |
N1—Li3—C11 | 103.35 (16) | C26—C27—H27A | 111.3 |
C1—Li3—C11 | 136.62 (16) | C28—C27—H27B | 111.3 |
O3—Li3—C2 | 114.43 (18) | C26—C27—H27B | 111.3 |
N2—Li3—C2 | 98.29 (15) | H27A—C27—H27B | 109.2 |
N1—Li3—C2 | 59.68 (10) | O2—C28—C27 | 104.19 (17) |
C1—Li3—C2 | 31.35 (8) | O2—C28—H28A | 110.9 |
C11—Li3—C2 | 133.20 (16) | C27—C28—H28A | 110.9 |
C21—O1—C24 | 106.02 (16) | O2—C28—H28B | 110.9 |
C21—O1—Li1 | 126.13 (16) | C27—C28—H28B | 110.9 |
C24—O1—Li1 | 127.16 (13) | H28A—C28—H28B | 108.9 |
C25—O2—C28 | 106.21 (16) | O3—C29—C30 | 109.4 (2) |
C25—O2—Li2 | 126.21 (15) | O3—C29—H29A | 109.8 |
C28—O2—Li2 | 126.80 (13) | C30—C29—H29A | 109.8 |
C29—O3—C31 | 111.7 (2) | O3—C29—H29B | 109.8 |
C29—O3—Li3 | 118.2 (2) | C30—C29—H29B | 109.8 |
C31—O3—Li3 | 118.2 (2) | H29A—C29—H29B | 108.2 |
N1—C1—C2 | 124.42 (16) | C29—C30—H30A | 109.5 |
N1—C1—C6 | 120.20 (16) | C29—C30—H30B | 109.5 |
C2—C1—C6 | 115.29 (16) | H30A—C30—H30B | 109.5 |
N1—C1—Li3 | 66.27 (13) | C29—C30—H30C | 109.5 |
C2—C1—Li3 | 90.81 (16) | H30A—C30—H30C | 109.5 |
C6—C1—Li3 | 112.37 (14) | H30B—C30—H30C | 109.5 |
C3—C2—C1 | 122.86 (18) | O3—C31—C32 | 109.6 (2) |
C3—C2—Li3 | 124.85 (15) | O3—C31—H31A | 109.8 |
C1—C2—Li3 | 57.84 (13) | C32—C31—H31A | 109.8 |
C3—C2—H2 | 118.6 | O3—C31—H31B | 109.8 |
C1—C2—H2 | 118.6 | C32—C31—H31B | 109.8 |
Li3—C2—H2 | 87.7 | H31A—C31—H31B | 108.2 |
C4—C3—C2 | 121.9 (2) | C31—C32—H32A | 109.5 |
C4—C3—H3 | 119.1 | C31—C32—H32B | 109.5 |
C2—C3—H3 | 119.1 | H32A—C32—H32B | 109.5 |
C3—C4—C5 | 119.34 (18) | C31—C32—H32C | 109.5 |
C3—C4—H4 | 120.3 | H32A—C32—H32C | 109.5 |
C5—C4—H4 | 120.3 | H32B—C32—H32C | 109.5 |
C4—C5—C10 | 121.75 (19) | C42—O4—C41 | 96.6 (10) |
C4—C5—C6 | 119.81 (18) | O4—C41—C40 | 90.3 (10) |
C10—C5—C6 | 118.4 (2) | O4—C41—H41A | 113.6 |
C7—C6—C5 | 118.10 (17) | C40—C41—H41A | 113.6 |
C7—C6—C1 | 121.10 (16) | O4—C41—H41B | 113.6 |
C5—C6—C1 | 120.80 (17) | C40—C41—H41B | 113.6 |
C8—C7—C6 | 121.9 (2) | H41A—C41—H41B | 110.9 |
C8—C7—H7 | 119.1 | C41—C40—H40A | 109.5 |
C6—C7—H7 | 119.1 | C41—C40—H40B | 109.5 |
C7—C8—C9 | 119.7 (2) | H40A—C40—H40B | 109.5 |
C7—C8—H8 | 120.2 | C41—C40—H40C | 109.5 |
C9—C8—H8 | 120.2 | H40A—C40—H40C | 109.5 |
C10—C9—C8 | 120.1 (2) | H40B—C40—H40C | 109.5 |
C10—C9—H9 | 120.0 | C43—C42—O4 | 103.8 (16) |
C8—C9—H9 | 120.0 | C43—C42—H42A | 111.0 |
C9—C10—C5 | 121.8 (2) | O4—C42—H42A | 111.0 |
C9—C10—H10 | 119.1 | C43—C42—H42B | 111.0 |
C5—C10—H10 | 119.1 | O4—C42—H42B | 111.0 |
N2—C11—C16 | 124.44 (16) | H42A—C42—H42B | 109.0 |
N2—C11—C12 | 119.81 (16) | C42—C43—H43A | 109.5 |
C16—C11—C12 | 115.70 (16) | C42—C43—H43B | 109.5 |
N2—C11—Li3 | 61.00 (13) | H43A—C43—H43B | 109.5 |
C16—C11—Li3 | 98.31 (16) | C42—C43—H43C | 109.5 |
C12—C11—Li3 | 109.98 (15) | H43A—C43—H43C | 109.5 |
C17—C12—C13 | 118.23 (17) | H43B—C43—H43C | 109.5 |
C17—C12—C11 | 121.13 (16) | C51—O5—C52 | 113.4 (16) |
C13—C12—C11 | 120.64 (18) | O5—C52—C53 | 112 (3) |
C14—C13—C20 | 122.50 (19) | O5—C52—H52A | 109.2 |
C14—C13—C12 | 119.63 (18) | C53—C52—H52A | 109.2 |
C20—C13—C12 | 117.9 (2) | O5—C52—H52B | 109.2 |
C15—C14—C13 | 119.60 (18) | C53—C52—H52B | 109.2 |
C15—C14—H14 | 120.2 | H52A—C52—H52B | 107.9 |
C13—C14—H14 | 120.2 | C52—C53—H53A | 109.5 |
C14—C15—C16 | 121.7 (2) | C52—C53—H53B | 109.5 |
C14—C15—H15 | 119.1 | H53A—C53—H53B | 109.5 |
C16—C15—H15 | 119.1 | C52—C53—H53C | 109.5 |
C15—C16—C11 | 122.63 (18) | H53A—C53—H53C | 109.5 |
C15—C16—H16 | 118.7 | H53B—C53—H53C | 109.5 |
C11—C16—H16 | 118.7 | O5—C51—C50 | 96 (2) |
C18—C17—C12 | 122.11 (19) | O5—C51—H51A | 112.5 |
C18—C17—H17 | 118.9 | C50—C51—H51A | 112.5 |
C12—C17—H17 | 118.9 | O5—C51—H51B | 112.5 |
C17—C18—C19 | 119.7 (2) | C50—C51—H51B | 112.5 |
C17—C18—H18 | 120.1 | H51A—C51—H51B | 110.0 |
C19—C18—H18 | 120.1 | C51—C50—H50A | 109.5 |
C20—C19—C18 | 119.9 (2) | C51—C50—H50B | 109.5 |
C20—C19—H19 | 120.1 | H50A—C50—H50B | 109.5 |
C18—C19—H19 | 120.1 | C51—C50—H50C | 109.5 |
C19—C20—C13 | 122.2 (2) | H50A—C50—H50C | 109.5 |
C19—C20—H20 | 118.9 | H50B—C50—H50C | 109.5 |
C13—C20—H20 | 118.9 |
Symmetry code: (i) −x, y, −z+1/2. |