Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806022161/cf2034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806022161/cf2034Isup2.hkl |
CCDC reference: 613629
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- Disorder in main residue
- R factor = 0.058
- wR factor = 0.148
- Data-to-parameter ratio = 15.6
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.65 Ratio PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C26 PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C26A
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.75 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C23 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C23A PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C9 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C27 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C27A PLAT301_ALERT_3_C Main Residue Disorder ......................... 23.00 Perc. PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 5 PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N4 - H4 ... ?
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Hooft, 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.
[Li6(C16H38N4Si)2Cl2(C4H8O)4] | F(000) = 2256 |
Mr = 1030.14 | Dx = 1.085 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 5541 reflections |
a = 19.405 (4) Å | θ = 3.5–27.5° |
b = 10.632 (2) Å | µ = 0.18 mm−1 |
c = 30.693 (6) Å | T = 173 K |
β = 95.40 (3)° | Plate, colourless |
V = 6304 (2) Å3 | 0.20 × 0.15 × 0.05 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 5541 independent reflections |
Radiation source: fine-focus sealed tube | 3720 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
φ and ω scans | θmax = 25.0°, θmin = 3.5° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | h = −23→23 |
Tmin = 0.964, Tmax = 0.991 | k = −12→12 |
10599 measured reflections | l = −36→36 |
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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.148 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0557P)2 + 10.6595P] where P = (Fo2 + 2Fc2)/3 |
5541 reflections | (Δ/σ)max = 0.008 |
355 parameters | Δρmax = 0.28 e Å−3 |
20 restraints | Δρmin = −0.28 e Å−3 |
Experimental. NMR (300 MHz, 298 K, d8-THF) 1H: 1.23, 1.13, 1.09 [s, 36H, C(CH3)3], 3.64, 1.78 [m, 16H, C4H8O]. 29Si: -60.3 [br s]. 7Li: 1.22 (s), 0.21 (s). |
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 | 0.56774 (4) | 0.27285 (7) | 0.38173 (2) | 0.0307 (2) | |
N1 | 0.53899 (11) | 0.1350 (2) | 0.35722 (7) | 0.0328 (5) | |
N2 | 0.54378 (12) | 0.3146 (2) | 0.43320 (7) | 0.0374 (6) | |
H2 | 0.5185 | 0.3834 | 0.4317 | 0.045* | |
N3 | 0.65271 (11) | 0.2495 (2) | 0.37429 (8) | 0.0359 (6) | |
N4 | 0.53300 (12) | 0.3988 (2) | 0.34705 (7) | 0.0337 (6) | |
H4 | 0.5720 | 0.4301 | 0.3352 | 0.040* | |
Li1 | 0.4984 (3) | 0.2581 (5) | 0.30251 (16) | 0.0409 (12) | |
Cl1 | 0.59325 (4) | 0.26026 (8) | 0.25272 (2) | 0.0433 (2) | |
Li2 | 0.6211 (3) | 0.1535 (5) | 0.31762 (16) | 0.0430 (12) | |
Li3 | 0.6373 (3) | 0.0660 (5) | 0.38465 (18) | 0.0498 (14) | |
C1 | 0.47609 (14) | 0.0595 (3) | 0.36182 (9) | 0.0342 (7) | |
C2 | 0.48696 (17) | −0.0321 (3) | 0.40036 (10) | 0.0489 (8) | |
H2A | 0.5287 | −0.0822 | 0.3976 | 0.073* | |
H2B | 0.4468 | −0.0881 | 0.4003 | 0.073* | |
H2C | 0.4923 | 0.0153 | 0.4279 | 0.073* | |
C3 | 0.45934 (17) | −0.0203 (3) | 0.32067 (10) | 0.0475 (8) | |
H3A | 0.4508 | 0.0350 | 0.2952 | 0.071* | |
H3B | 0.4180 | −0.0711 | 0.3239 | 0.071* | |
H3C | 0.4985 | −0.0757 | 0.3165 | 0.071* | |
C4 | 0.41207 (15) | 0.1389 (3) | 0.36862 (11) | 0.0433 (8) | |
H4A | 0.4223 | 0.1945 | 0.3938 | 0.065* | |
H4B | 0.3735 | 0.0833 | 0.3740 | 0.065* | |
H4C | 0.3995 | 0.1896 | 0.3424 | 0.065* | |
C5 | 0.55391 (16) | 0.2674 (3) | 0.47813 (9) | 0.0411 (7) | |
C6 | 0.60378 (17) | 0.1563 (3) | 0.48113 (11) | 0.0517 (9) | |
H6A | 0.5836 | 0.0868 | 0.4632 | 0.078* | |
H6B | 0.6121 | 0.1290 | 0.5117 | 0.078* | |
H6C | 0.6477 | 0.1818 | 0.4704 | 0.078* | |
C7 | 0.48442 (17) | 0.2300 (3) | 0.49419 (10) | 0.0521 (9) | |
H7A | 0.4532 | 0.3026 | 0.4922 | 0.078* | |
H7B | 0.4917 | 0.2020 | 0.5247 | 0.078* | |
H7C | 0.4638 | 0.1615 | 0.4760 | 0.078* | |
C8 | 0.58530 (19) | 0.3718 (3) | 0.50848 (11) | 0.0570 (9) | |
H8A | 0.6302 | 0.3970 | 0.4991 | 0.086* | |
H8B | 0.5916 | 0.3404 | 0.5386 | 0.086* | |
H8C | 0.5541 | 0.4444 | 0.5070 | 0.086* | |
C9 | 0.71214 (15) | 0.3346 (3) | 0.38080 (11) | 0.0448 (8) | |
C10 | 0.7236 (2) | 0.3863 (4) | 0.42698 (13) | 0.0826 (13) | |
H10A | 0.6847 | 0.4408 | 0.4327 | 0.124* | |
H10B | 0.7667 | 0.4351 | 0.4301 | 0.124* | |
H10C | 0.7269 | 0.3166 | 0.4479 | 0.124* | |
C11 | 0.77723 (18) | 0.2617 (4) | 0.37175 (19) | 0.0923 (16) | |
H11A | 0.7827 | 0.1888 | 0.3913 | 0.139* | |
H11B | 0.8178 | 0.3166 | 0.3768 | 0.139* | |
H11C | 0.7729 | 0.2329 | 0.3413 | 0.139* | |
C12 | 0.7072 (2) | 0.4446 (4) | 0.34891 (14) | 0.0791 (13) | |
H12A | 0.6974 | 0.4130 | 0.3190 | 0.119* | |
H12B | 0.7512 | 0.4906 | 0.3513 | 0.119* | |
H12C | 0.6700 | 0.5012 | 0.3559 | 0.119* | |
C13 | 0.49105 (16) | 0.5139 (3) | 0.35245 (9) | 0.0389 (7) | |
C14 | 0.42099 (16) | 0.4794 (3) | 0.36693 (11) | 0.0510 (9) | |
H14A | 0.3972 | 0.4218 | 0.3456 | 0.076* | |
H14B | 0.3932 | 0.5558 | 0.3690 | 0.076* | |
H14C | 0.4272 | 0.4383 | 0.3956 | 0.076* | |
C15 | 0.4798 (2) | 0.5778 (3) | 0.30782 (11) | 0.0591 (10) | |
H15A | 0.5248 | 0.5967 | 0.2972 | 0.089* | |
H15B | 0.4539 | 0.6561 | 0.3105 | 0.089* | |
H15C | 0.4536 | 0.5216 | 0.2871 | 0.089* | |
C16 | 0.52806 (19) | 0.6072 (3) | 0.38489 (11) | 0.0555 (9) | |
H16A | 0.5358 | 0.5678 | 0.4138 | 0.083* | |
H16B | 0.4993 | 0.6825 | 0.3868 | 0.083* | |
H16C | 0.5726 | 0.6310 | 0.3747 | 0.083* | |
O1 | 0.68789 (11) | −0.0603 (2) | 0.42025 (7) | 0.0533 (6) | 0.80 |
C20 | 0.6847 (3) | −0.1931 (4) | 0.41731 (19) | 0.0717 (15) | 0.80 |
H20A | 0.6676 | −0.2194 | 0.3873 | 0.086* | 0.80 |
H20B | 0.6533 | −0.2272 | 0.4380 | 0.086* | 0.80 |
C21 | 0.7576 (4) | −0.2401 (5) | 0.4288 (2) | 0.0761 (18) | 0.80 |
H21A | 0.7809 | −0.2570 | 0.4021 | 0.091* | 0.80 |
H21B | 0.7577 | −0.3179 | 0.4465 | 0.091* | 0.80 |
C22 | 0.7923 (3) | −0.1332 (5) | 0.4549 (2) | 0.0722 (15) | 0.80 |
H22A | 0.8090 | −0.1615 | 0.4848 | 0.087* | 0.80 |
H22B | 0.8321 | −0.1005 | 0.4404 | 0.087* | 0.80 |
C23 | 0.7387 (3) | −0.0358 (5) | 0.45658 (19) | 0.0825 (17) | 0.80 |
H23A | 0.7173 | −0.0406 | 0.4846 | 0.099* | 0.80 |
H23B | 0.7590 | 0.0490 | 0.4539 | 0.099* | 0.80 |
O2 | 0.6661 (7) | −0.0222 (11) | 0.3163 (6) | 0.0475 (19) | 0.65 |
C24 | 0.7396 (3) | −0.0414 (6) | 0.3150 (3) | 0.075 (2) | 0.65 |
H24A | 0.7645 | −0.0345 | 0.3445 | 0.090* | 0.65 |
H24B | 0.7592 | 0.0203 | 0.2954 | 0.090* | 0.65 |
C25 | 0.7439 (3) | −0.1737 (8) | 0.2972 (3) | 0.101 (2) | 0.65 |
H25A | 0.7864 | −0.1847 | 0.2821 | 0.121* | 0.65 |
H25B | 0.7440 | −0.2363 | 0.3211 | 0.121* | 0.65 |
C26 | 0.6828 (8) | −0.1870 (13) | 0.2669 (6) | 0.125 (4) | 0.65 |
H26A | 0.6714 | −0.2763 | 0.2606 | 0.150* | 0.65 |
H26B | 0.6870 | −0.1412 | 0.2392 | 0.150* | 0.65 |
C27 | 0.6312 (5) | −0.1255 (10) | 0.2942 (6) | 0.070 (3) | 0.65 |
H27A | 0.5904 | −0.0955 | 0.2753 | 0.084* | 0.65 |
H27B | 0.6154 | −0.1862 | 0.3157 | 0.084* | 0.65 |
O1A | 0.68789 (11) | −0.0603 (2) | 0.42025 (7) | 0.0533 (6) | 0.20 |
C20A | 0.6684 (12) | −0.1524 (18) | 0.4485 (8) | 0.0717 (15) | 0.20 |
H20C | 0.6201 | −0.1796 | 0.4403 | 0.086* | 0.20 |
H20D | 0.6721 | −0.1211 | 0.4790 | 0.086* | 0.20 |
C21A | 0.7160 (13) | −0.255 (2) | 0.4440 (9) | 0.0761 (18) | 0.20 |
H21C | 0.6973 | −0.3154 | 0.4214 | 0.091* | 0.20 |
H21D | 0.7264 | −0.3000 | 0.4721 | 0.091* | 0.20 |
C22A | 0.7818 (14) | −0.187 (3) | 0.4299 (12) | 0.0722 (15) | 0.20 |
H22C | 0.8182 | −0.1826 | 0.4547 | 0.087* | 0.20 |
H22D | 0.8005 | −0.2324 | 0.4055 | 0.087* | 0.20 |
C23A | 0.7618 (12) | −0.0679 (19) | 0.4168 (8) | 0.0825 (17) | 0.20 |
H23C | 0.7721 | −0.0528 | 0.3863 | 0.099* | 0.20 |
H23D | 0.7866 | −0.0042 | 0.4359 | 0.099* | 0.20 |
O2A | 0.6717 (14) | 0.004 (2) | 0.3154 (11) | 0.0475 (19) | 0.35 |
C24A | 0.7307 (7) | 0.0096 (12) | 0.2924 (5) | 0.075 (2) | 0.35 |
H24C | 0.7727 | 0.0016 | 0.3131 | 0.090* | 0.35 |
H24D | 0.7325 | 0.0921 | 0.2775 | 0.090* | 0.35 |
C25A | 0.7298 (7) | −0.0878 (15) | 0.2609 (5) | 0.101 (2) | 0.35 |
H25C | 0.7767 | −0.1234 | 0.2595 | 0.121* | 0.35 |
H25D | 0.7122 | −0.0568 | 0.2315 | 0.121* | 0.35 |
C26A | 0.6818 (15) | −0.183 (2) | 0.2772 (12) | 0.125 (4) | 0.35 |
H26C | 0.7043 | −0.2351 | 0.3013 | 0.150* | 0.35 |
H26D | 0.6609 | −0.2385 | 0.2535 | 0.150* | 0.35 |
C27A | 0.6305 (10) | −0.091 (2) | 0.2928 (13) | 0.070 (3) | 0.35 |
H27C | 0.6014 | −0.0544 | 0.2677 | 0.084* | 0.35 |
H27D | 0.6001 | −0.1321 | 0.3127 | 0.084* | 0.35 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Si1 | 0.0283 (4) | 0.0299 (4) | 0.0335 (4) | −0.0008 (3) | −0.0002 (3) | −0.0032 (3) |
N1 | 0.0279 (12) | 0.0321 (13) | 0.0380 (13) | −0.0023 (10) | 0.0017 (10) | −0.0042 (10) |
N2 | 0.0424 (14) | 0.0337 (13) | 0.0353 (13) | 0.0092 (11) | −0.0005 (11) | −0.0009 (11) |
N3 | 0.0275 (12) | 0.0366 (14) | 0.0431 (14) | −0.0028 (11) | 0.0008 (10) | −0.0055 (11) |
N4 | 0.0339 (13) | 0.0297 (13) | 0.0375 (14) | −0.0002 (11) | 0.0033 (11) | −0.0026 (10) |
Li1 | 0.046 (3) | 0.036 (3) | 0.039 (3) | 0.000 (2) | −0.006 (2) | −0.003 (2) |
Cl1 | 0.0350 (4) | 0.0591 (5) | 0.0352 (4) | −0.0005 (4) | 0.0005 (3) | 0.0017 (4) |
Li2 | 0.042 (3) | 0.047 (3) | 0.040 (3) | 0.009 (2) | 0.003 (2) | −0.004 (2) |
Li3 | 0.044 (3) | 0.044 (3) | 0.059 (3) | 0.007 (3) | −0.008 (3) | 0.009 (3) |
C1 | 0.0301 (15) | 0.0312 (15) | 0.0409 (16) | −0.0041 (12) | 0.0010 (13) | −0.0016 (13) |
C2 | 0.051 (2) | 0.0394 (18) | 0.055 (2) | −0.0051 (16) | −0.0019 (16) | 0.0088 (15) |
C3 | 0.0458 (18) | 0.0415 (18) | 0.054 (2) | −0.0097 (15) | −0.0003 (16) | −0.0089 (15) |
C4 | 0.0310 (16) | 0.0429 (18) | 0.056 (2) | −0.0009 (14) | 0.0049 (14) | 0.0019 (15) |
C5 | 0.0475 (18) | 0.0424 (18) | 0.0319 (16) | 0.0080 (15) | −0.0042 (14) | −0.0022 (14) |
C6 | 0.055 (2) | 0.052 (2) | 0.0462 (19) | 0.0170 (17) | −0.0026 (16) | 0.0037 (16) |
C7 | 0.059 (2) | 0.057 (2) | 0.0405 (18) | 0.0097 (18) | 0.0064 (16) | 0.0058 (16) |
C8 | 0.063 (2) | 0.062 (2) | 0.0443 (19) | 0.0079 (19) | −0.0031 (17) | −0.0117 (17) |
C9 | 0.0294 (15) | 0.0467 (19) | 0.057 (2) | −0.0049 (15) | −0.0028 (14) | −0.0027 (16) |
C10 | 0.074 (3) | 0.097 (3) | 0.074 (3) | −0.039 (3) | −0.008 (2) | −0.022 (2) |
C11 | 0.0309 (19) | 0.070 (3) | 0.176 (5) | −0.0048 (19) | 0.010 (2) | −0.011 (3) |
C12 | 0.054 (2) | 0.080 (3) | 0.099 (3) | −0.036 (2) | −0.014 (2) | 0.022 (2) |
C13 | 0.0459 (18) | 0.0268 (15) | 0.0436 (18) | 0.0078 (14) | 0.0017 (14) | −0.0022 (13) |
C14 | 0.0426 (18) | 0.046 (2) | 0.063 (2) | 0.0145 (16) | 0.0015 (17) | −0.0028 (17) |
C15 | 0.081 (3) | 0.0414 (19) | 0.054 (2) | 0.0178 (19) | 0.0012 (19) | 0.0047 (16) |
C16 | 0.071 (2) | 0.0357 (19) | 0.059 (2) | 0.0009 (17) | 0.0034 (19) | −0.0095 (16) |
O1 | 0.0499 (13) | 0.0482 (14) | 0.0588 (15) | 0.0115 (11) | −0.0106 (11) | 0.0027 (11) |
C20 | 0.082 (4) | 0.041 (3) | 0.086 (4) | −0.005 (3) | −0.023 (3) | 0.004 (3) |
C21 | 0.079 (5) | 0.051 (3) | 0.096 (4) | 0.024 (3) | 0.001 (4) | −0.005 (3) |
C22 | 0.049 (3) | 0.077 (4) | 0.089 (4) | 0.014 (3) | −0.004 (3) | −0.002 (3) |
C23 | 0.089 (4) | 0.059 (3) | 0.090 (4) | 0.021 (3) | −0.044 (3) | −0.015 (3) |
O2 | 0.038 (2) | 0.037 (6) | 0.0669 (17) | 0.008 (3) | 0.0023 (16) | −0.007 (4) |
C24 | 0.046 (3) | 0.076 (5) | 0.106 (6) | 0.017 (3) | 0.020 (4) | 0.001 (4) |
C25 | 0.063 (4) | 0.126 (7) | 0.117 (6) | 0.036 (4) | 0.022 (4) | −0.027 (5) |
C26 | 0.108 (4) | 0.135 (5) | 0.129 (9) | 0.039 (4) | −0.003 (5) | −0.084 (5) |
C27 | 0.069 (3) | 0.045 (7) | 0.095 (3) | 0.018 (4) | 0.007 (2) | −0.025 (6) |
O1A | 0.0499 (13) | 0.0482 (14) | 0.0588 (15) | 0.0115 (11) | −0.0106 (11) | 0.0027 (11) |
C20A | 0.082 (4) | 0.041 (3) | 0.086 (4) | −0.005 (3) | −0.023 (3) | 0.004 (3) |
C21A | 0.079 (5) | 0.051 (3) | 0.096 (4) | 0.024 (3) | 0.001 (4) | −0.005 (3) |
C22A | 0.049 (3) | 0.077 (4) | 0.089 (4) | 0.014 (3) | −0.004 (3) | −0.002 (3) |
C23A | 0.089 (4) | 0.059 (3) | 0.090 (4) | 0.021 (3) | −0.044 (3) | −0.015 (3) |
O2A | 0.038 (2) | 0.037 (6) | 0.0669 (17) | 0.008 (3) | 0.0023 (16) | −0.007 (4) |
C24A | 0.046 (3) | 0.076 (5) | 0.106 (6) | 0.017 (3) | 0.020 (4) | 0.001 (4) |
C25A | 0.063 (4) | 0.126 (7) | 0.117 (6) | 0.036 (4) | 0.022 (4) | −0.027 (5) |
C26A | 0.108 (4) | 0.135 (5) | 0.129 (9) | 0.039 (4) | −0.003 (5) | −0.084 (5) |
C27A | 0.069 (3) | 0.045 (7) | 0.095 (3) | 0.018 (4) | 0.007 (2) | −0.025 (6) |
Si1—N3 | 1.704 (2) | C13—C15 | 1.526 (4) |
Si1—N1 | 1.716 (2) | C13—C16 | 1.535 (4) |
Si1—N2 | 1.745 (2) | C14—H14A | 0.980 |
Si1—N4 | 1.802 (2) | C14—H14B | 0.980 |
N1—C1 | 1.479 (3) | C14—H14C | 0.980 |
N1—Li2 | 2.102 (5) | C15—H15A | 0.980 |
N1—Li3 | 2.141 (6) | C15—H15B | 0.980 |
N1—Li1 | 2.215 (5) | C15—H15C | 0.980 |
N2—C5 | 1.463 (3) | C16—H16A | 0.980 |
N2—H2 | 0.880 | C16—H16B | 0.980 |
N3—C9 | 1.465 (4) | C16—H16C | 0.980 |
N3—Li3 | 2.004 (6) | O1—C20 | 1.416 (5) |
N3—Li2 | 2.060 (5) | O1—C23 | 1.441 (5) |
N4—C13 | 1.487 (3) | C20—C21 | 1.509 (8) |
N4—Li1 | 2.094 (5) | C20—H20A | 0.990 |
N4—H4 | 0.930 | C20—H20B | 0.990 |
Li1—Cl1i | 2.339 (5) | C21—C22 | 1.513 (8) |
Li1—Cl1 | 2.500 (5) | C21—H21A | 0.990 |
Cl1—Li2 | 2.312 (5) | C21—H21B | 0.990 |
Cl1—Li1i | 2.339 (5) | C22—C23 | 1.472 (7) |
Li2—O2A | 1.87 (3) | C22—H22A | 0.990 |
Li2—O2 | 2.065 (14) | C22—H22B | 0.990 |
Li3—O1 | 1.939 (5) | C23—H23A | 0.990 |
Li3—O2A | 2.38 (2) | C23—H23B | 0.990 |
Li3—O2 | 2.410 (13) | O2—C27 | 1.428 (9) |
C1—C3 | 1.531 (4) | O2—C24 | 1.445 (12) |
C1—C2 | 1.532 (4) | C24—C25 | 1.513 (9) |
C1—C4 | 1.532 (4) | C24—H24A | 0.990 |
C2—H2A | 0.980 | C24—H24B | 0.990 |
C2—H2B | 0.980 | C25—C26 | 1.444 (15) |
C2—H2C | 0.980 | C25—H25A | 0.990 |
C3—H3A | 0.980 | C25—H25B | 0.990 |
C3—H3B | 0.980 | C26—C27 | 1.514 (11) |
C3—H3C | 0.980 | C26—H26A | 0.990 |
C4—H4A | 0.980 | C26—H26B | 0.990 |
C4—H4B | 0.980 | C27—H27A | 0.990 |
C4—H4C | 0.980 | C27—H27B | 0.990 |
C5—C6 | 1.524 (4) | C20A—C21A | 1.44 (3) |
C5—C7 | 1.531 (5) | C20A—H20C | 0.990 |
C5—C8 | 1.538 (4) | C20A—H20D | 0.990 |
C6—H6A | 0.980 | C21A—C22A | 1.57 (4) |
C6—H6B | 0.980 | C21A—H21C | 0.990 |
C6—H6C | 0.980 | C21A—H21D | 0.990 |
C7—H7A | 0.980 | C22A—C23A | 1.37 (3) |
C7—H7B | 0.980 | C22A—H22C | 0.990 |
C7—H7C | 0.980 | C22A—H22D | 0.990 |
C8—H8A | 0.980 | C23A—H23C | 0.990 |
C8—H8B | 0.980 | C23A—H23D | 0.990 |
C8—H8C | 0.980 | O2A—C24A | 1.401 (16) |
C9—C10 | 1.517 (5) | O2A—C27A | 1.426 (17) |
C9—C12 | 1.523 (5) | C24A—C25A | 1.415 (14) |
C9—C11 | 1.529 (5) | C24A—H24C | 0.990 |
C10—H10A | 0.980 | C24A—H24D | 0.990 |
C10—H10B | 0.980 | C25A—C26A | 1.496 (18) |
C10—H10C | 0.980 | C25A—H25C | 0.990 |
C11—H11A | 0.980 | C25A—H25D | 0.990 |
C11—H11B | 0.980 | C26A—C27A | 1.510 (18) |
C11—H11C | 0.980 | C26A—H26C | 0.990 |
C12—H12A | 0.980 | C26A—H26D | 0.990 |
C12—H12B | 0.980 | C27A—H27C | 0.990 |
C12—H12C | 0.980 | C27A—H27D | 0.990 |
C13—C14 | 1.515 (4) | ||
N3—Si1—N1 | 95.48 (11) | N4—C13—C14 | 110.5 (2) |
N3—Si1—N2 | 120.12 (12) | N4—C13—C15 | 107.4 (2) |
N1—Si1—N2 | 120.69 (12) | C14—C13—C15 | 108.3 (3) |
N3—Si1—N4 | 110.02 (12) | N4—C13—C16 | 112.1 (2) |
N1—Si1—N4 | 106.71 (11) | C14—C13—C16 | 110.1 (3) |
N2—Si1—N4 | 103.24 (11) | C15—C13—C16 | 108.2 (3) |
C1—N1—Si1 | 131.22 (18) | C13—C14—H14A | 109.5 |
C1—N1—Li2 | 141.6 (2) | C13—C14—H14B | 109.5 |
Si1—N1—Li2 | 86.61 (17) | H14A—C14—H14B | 109.5 |
C1—N1—Li3 | 119.3 (2) | C13—C14—H14C | 109.5 |
Si1—N1—Li3 | 83.08 (18) | H14A—C14—H14C | 109.5 |
Li2—N1—Li3 | 64.1 (2) | H14B—C14—H14C | 109.5 |
C1—N1—Li1 | 98.9 (2) | C13—C15—H15A | 109.5 |
Si1—N1—Li1 | 84.58 (16) | C13—C15—H15B | 109.5 |
Li2—N1—Li1 | 75.0 (2) | H15A—C15—H15B | 109.5 |
Li3—N1—Li1 | 137.8 (2) | C13—C15—H15C | 109.5 |
C5—N2—Si1 | 137.9 (2) | H15A—C15—H15C | 109.5 |
C5—N2—H2 | 111.0 | H15B—C15—H15C | 109.5 |
Si1—N2—H2 | 111.0 | C13—C16—H16A | 109.5 |
C9—N3—Si1 | 130.6 (2) | C13—C16—H16B | 109.5 |
C9—N3—Li3 | 135.0 (2) | H16A—C16—H16B | 109.5 |
Si1—N3—Li3 | 87.71 (19) | C13—C16—H16C | 109.5 |
C9—N3—Li2 | 126.1 (2) | H16A—C16—H16C | 109.5 |
Si1—N3—Li2 | 88.30 (17) | H16B—C16—H16C | 109.5 |
Li3—N3—Li2 | 67.3 (2) | C20—O1—C23 | 104.6 (3) |
C13—N4—Si1 | 136.37 (19) | C20—O1—Li3 | 129.7 (3) |
C13—N4—Li1 | 121.0 (2) | C23—O1—Li3 | 125.7 (3) |
Si1—N4—Li1 | 86.20 (16) | O1—C20—C21 | 106.4 (4) |
C13—N4—H4 | 102.9 | O1—C20—H20A | 110.5 |
Si1—N4—H4 | 102.9 | C21—C20—H20A | 110.5 |
Li1—N4—H4 | 102.9 | O1—C20—H20B | 110.5 |
N4—Li1—N1 | 81.83 (19) | C21—C20—H20B | 110.5 |
N4—Li1—Cl1i | 129.9 (2) | H20A—C20—H20B | 108.6 |
N1—Li1—Cl1i | 138.4 (2) | C20—C21—C22 | 103.7 (4) |
N4—Li1—Cl1 | 100.6 (2) | C20—C21—H21A | 111.0 |
N1—Li1—Cl1 | 103.8 (2) | C22—C21—H21A | 111.0 |
Cl1i—Li1—Cl1 | 96.33 (17) | C20—C21—H21B | 111.0 |
Li2—Cl1—Li1i | 136.04 (18) | C22—C21—H21B | 111.0 |
Li2—Cl1—Li1 | 66.10 (17) | H21A—C21—H21B | 109.0 |
Li1i—Cl1—Li1 | 83.66 (17) | C23—C22—C21 | 105.3 (4) |
O2A—Li2—N3 | 109.6 (11) | C23—C22—H22A | 110.7 |
N3—Li2—O2 | 111.8 (6) | C21—C22—H22A | 110.7 |
O2A—Li2—N1 | 111.8 (8) | C23—C22—H22B | 110.7 |
N3—Li2—N1 | 74.91 (18) | C21—C22—H22B | 110.7 |
O2—Li2—N1 | 105.8 (4) | H22A—C22—H22B | 108.8 |
O2A—Li2—Cl1 | 117.7 (11) | O1—C23—C22 | 106.3 (4) |
N3—Li2—Cl1 | 120.8 (3) | O1—C23—H23A | 110.5 |
O2—Li2—Cl1 | 119.5 (5) | C22—C23—H23A | 110.5 |
N1—Li2—Cl1 | 114.6 (2) | O1—C23—H23B | 110.5 |
Li3—Li2—Cl1 | 172.2 (3) | C22—C23—H23B | 110.5 |
O1—Li3—N3 | 133.5 (3) | H23A—C23—H23B | 108.7 |
O1—Li3—N1 | 147.6 (3) | C27—O2—C24 | 107.6 (6) |
N3—Li3—N1 | 75.2 (2) | C27—O2—Li2 | 121.5 (11) |
O1—Li3—O2A | 98.2 (9) | C24—O2—Li2 | 123.3 (7) |
N3—Li3—O2A | 93.9 (7) | C27—O2—Li3 | 125.0 (8) |
N1—Li3—O2A | 93.3 (9) | C24—O2—Li3 | 113.0 (10) |
O1—Li3—O2 | 94.2 (5) | Li2—O2—Li3 | 59.9 (3) |
N3—Li3—O2 | 101.0 (4) | O2—C24—C25 | 103.3 (6) |
N1—Li3—O2 | 93.6 (5) | O2—C24—H24A | 111.1 |
N1—C1—C3 | 109.6 (2) | C25—C24—H24A | 111.1 |
N1—C1—C2 | 111.4 (2) | O2—C24—H24B | 111.1 |
C3—C1—C2 | 106.7 (2) | C25—C24—H24B | 111.1 |
N1—C1—C4 | 113.6 (2) | H24A—C24—H24B | 109.1 |
C3—C1—C4 | 107.8 (2) | C26—C25—C24 | 104.7 (7) |
C2—C1—C4 | 107.4 (2) | C26—C25—H25A | 110.8 |
C1—C2—H2A | 109.5 | C24—C25—H25A | 110.8 |
C1—C2—H2B | 109.5 | C26—C25—H25B | 110.8 |
H2A—C2—H2B | 109.5 | C24—C25—H25B | 110.8 |
C1—C2—H2C | 109.5 | H25A—C25—H25B | 108.9 |
H2A—C2—H2C | 109.5 | C25—C26—C27 | 98.4 (9) |
H2B—C2—H2C | 109.5 | C25—C26—H26A | 112.1 |
C1—C3—H3A | 109.5 | C27—C26—H26A | 112.1 |
C1—C3—H3B | 109.5 | C25—C26—H26B | 112.1 |
H3A—C3—H3B | 109.5 | C27—C26—H26B | 112.1 |
C1—C3—H3C | 109.5 | H26A—C26—H26B | 109.7 |
H3A—C3—H3C | 109.5 | O2—C27—C26 | 106.7 (7) |
H3B—C3—H3C | 109.5 | O2—C27—H27A | 110.4 |
C1—C4—H4A | 109.5 | C26—C27—H27A | 110.4 |
C1—C4—H4B | 109.5 | O2—C27—H27B | 110.4 |
H4A—C4—H4B | 109.5 | C26—C27—H27B | 110.4 |
C1—C4—H4C | 109.5 | H27A—C27—H27B | 108.6 |
H4A—C4—H4C | 109.5 | C21A—C20A—H20C | 110.8 |
H4B—C4—H4C | 109.5 | C21A—C20A—H20D | 110.8 |
N2—C5—C6 | 110.5 (2) | H20C—C20A—H20D | 108.8 |
N2—C5—C7 | 110.4 (2) | C20A—C21A—C22A | 103 (2) |
C6—C5—C7 | 110.7 (3) | C20A—C21A—H21C | 111.2 |
N2—C5—C8 | 109.5 (3) | C22A—C21A—H21C | 111.2 |
C6—C5—C8 | 108.0 (3) | C20A—C21A—H21D | 111.2 |
C7—C5—C8 | 107.6 (3) | C22A—C21A—H21D | 111.2 |
C5—C6—H6A | 109.5 | H21C—C21A—H21D | 109.1 |
C5—C6—H6B | 109.5 | C23A—C22A—C21A | 107 (2) |
H6A—C6—H6B | 109.5 | C23A—C22A—H22C | 110.3 |
C5—C6—H6C | 109.5 | C21A—C22A—H22C | 110.3 |
H6A—C6—H6C | 109.5 | C23A—C22A—H22D | 110.3 |
H6B—C6—H6C | 109.5 | C21A—C22A—H22D | 110.3 |
C5—C7—H7A | 109.5 | H22C—C22A—H22D | 108.6 |
C5—C7—H7B | 109.5 | C22A—C23A—H23C | 110.4 |
H7A—C7—H7B | 109.5 | C22A—C23A—H23D | 110.4 |
C5—C7—H7C | 109.5 | H23C—C23A—H23D | 108.6 |
H7A—C7—H7C | 109.5 | C24A—O2A—C27A | 103.4 (12) |
H7B—C7—H7C | 109.5 | C24A—O2A—Li2 | 116.1 (19) |
C5—C8—H8A | 109.5 | C27A—O2A—Li2 | 110 (2) |
C5—C8—H8B | 109.5 | C24A—O2A—Li3 | 138.6 (19) |
H8A—C8—H8B | 109.5 | C27A—O2A—Li3 | 116.0 (17) |
C5—C8—H8C | 109.5 | Li2—O2A—Li3 | 62.6 (5) |
H8A—C8—H8C | 109.5 | O2A—C24A—C25A | 110.8 (10) |
H8B—C8—H8C | 109.5 | C25A—C24A—Li2 | 129.1 (9) |
N3—C9—C10 | 113.3 (3) | O2A—C24A—H24C | 109.5 |
N3—C9—C12 | 112.7 (3) | C25A—C24A—H24C | 109.5 |
C10—C9—C12 | 108.4 (3) | O2A—C24A—H24D | 109.5 |
N3—C9—C11 | 108.4 (3) | C25A—C24A—H24D | 109.5 |
C10—C9—C11 | 107.6 (3) | H24C—C24A—H24D | 108.1 |
C12—C9—C11 | 106.0 (3) | C24A—C25A—C26A | 103.8 (10) |
C9—C10—H10A | 109.5 | C24A—C25A—H25C | 111.0 |
C9—C10—H10B | 109.5 | C26A—C25A—H25C | 111.0 |
H10A—C10—H10B | 109.5 | C24A—C25A—H25D | 111.0 |
C9—C10—H10C | 109.5 | C26A—C25A—H25D | 111.0 |
H10A—C10—H10C | 109.5 | H25C—C25A—H25D | 109.0 |
H10B—C10—H10C | 109.5 | C25A—C26A—C27A | 96.4 (13) |
C9—C11—H11A | 109.5 | C25A—C26A—H26C | 112.5 |
C9—C11—H11B | 109.5 | C27A—C26A—H26C | 112.5 |
H11A—C11—H11B | 109.5 | C25A—C26A—H26D | 112.5 |
C9—C11—H11C | 109.5 | C27A—C26A—H26D | 112.5 |
H11A—C11—H11C | 109.5 | H26C—C26A—H26D | 110.0 |
H11B—C11—H11C | 109.5 | O2A—C27A—C26A | 105.0 (13) |
C9—C12—H12A | 109.5 | C26A—C27A—Li2 | 140.9 (11) |
C9—C12—H12B | 109.5 | O2A—C27A—H27C | 110.7 |
H12A—C12—H12B | 109.5 | C26A—C27A—H27C | 110.7 |
C9—C12—H12C | 109.5 | O2A—C27A—H27D | 110.7 |
H12A—C12—H12C | 109.5 | C26A—C27A—H27D | 110.7 |
H12B—C12—H12C | 109.5 | H27C—C27A—H27D | 108.8 |
Symmetry code: (i) −x+1, y, −z+1/2. |
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