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Acta Crystallogr Sect E Struct Rep Online. 2010 December 1; 66(Pt 12): m1527.
Published online 2010 November 6. doi:  10.1107/S1600536810044685
PMCID: PMC3011566

μ2-Acetone-diacetone[μ3-tris­(trifluoro­meth­yl)methano­lato]bis­[μ2-tris­(trifluoro­meth­yl)methano­lato]trilithium

Abstract

The title compound, [Li3(C4F9O)3(C3H6O)3], features an open Li/O cube with an Li ion missing at one corner. Three of the four bridging O atoms of the cube carry a fluorinated tert-butyl residue, whereas the fourth is part of an acetone mol­ecule. Two of the Li atoms are further bonded to a non-bridging acetone mol­ecule. Two of the lithium ion coordination geometries are very distorted LiO4 tetra­hedra; the third could be described as a very distorted LiO3 T-shape with two distant F-atom neighbours. The Li(...)Li contact distances for the three-coordinate Li+ ion [2.608 (14) and 2.631 (12) Å] are much shorter that the contact distance [2.940 (13) Å] between the tetra­hedrally coordinated species.

Related literature

For background to weakly coordinating ligands, see: Kern et al. (2008 [triangle]); Reisinger et al. (2007 [triangle]); Lerner et al. (2002 [triangle], 2005 [triangle]). For a comparable cage structure with an Mg/O skeleton, see: Zechmann et al. (2001 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1527-scheme1.jpg

Experimental

Crystal data

  • [Li3(C4F9O)3(C3H6O)3]
  • M r = 900.17
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1527-efi1.jpg
  • a = 20.6939 (17) Å
  • b = 11.594 (1) Å
  • c = 15.2211 (13) Å
  • β = 102.246 (7)°
  • V = 3568.8 (5) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 0.21 mm−1
  • T = 173 K
  • 0.17 × 0.12 × 0.08 mm

Data collection

  • Stoe IPDS-II two-circle diffractometer
  • 26210 measured reflections
  • 6696 independent reflections
  • 3143 reflections with I > 2σ(I)
  • R int = 0.097

Refinement

  • R[F 2 > 2σ(F 2)] = 0.100
  • wR(F 2) = 0.313
  • S = 1.02
  • 6696 reflections
  • 520 parameters
  • H-atom parameters constrained
  • Δρmax = 0.65 e Å−3
  • Δρmin = −0.43 e Å−3

Data collection: X-AREA (Stoe & Cie, 2001 [triangle]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: XP (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Selected bond lengths (Å)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810044685/hb5716sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810044685/hb5716Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Comment

Weakly coordinating anions have gained prominence in wide areas of application in research laboratories and industry. One approach is to create such anions by tetrasubstitution of triele derivatives with perfluorinated alkoxides as [OC(CF3)3]- (Reisinger et al., 2007) or with siloxides [OSiR3]- (R = alkyl) (Kern et al., 2008; Lerner et al., 2005, 2002). In this paper we report the crystal structure of the adduct of Li[OC(CF3)3] with acetone, [Li(OC(CH3)2]3[OC(CF3)3]3, (I). According to a literature procedure (Reisinger et al., 2007), Li[OC(CF3)3] was easily accessible from the reaction of HOC(CF3)3 with LiH. Single crystals of (I) were obtained by recrystallization from acetone. Only one comparabel cage structure was found in the Cambridge Crystallographic Database, i.e.3-1,1-diphenylethoxo)-tris(µ2-1,1-diphenylethoxo)-bis(1,1-diphenylethoxy)-tri-magnesium toluene solvate (Zechmann et al., 2001). The title compound features an open Li—O cube with an Li ion missing at one corner. Three of the four bridging O atoms carry a tert.-butyl residue whereas the fourth is part of an acetone molecule. The two four-coordinated Li atoms are further bonded to an acetone molecule. This is the first example of such an Li—O sceleton and only one comparable structure was determined up to now containing Mg instead of Li as metal atoms.

Experimental

LiH (0.34 g, 43.7 mmol) and Et2O (100 ml) were combined under an N2 atmosphere. Li[OC(CF3)3] (6.1 ml, 43.8 mmol) was added dropwise at ambient temperature. After 1 h at ambient temperature, the solution was heated under reflux for 2 h. Colourless blocks of (I) were obtained by recrystallization from acetone Yield: 6.1 g (50%).

Refinement

H atoms were located in a difference map, but geometrically positioned and refined using a riding model with fixed individual displacement parameters [U(H) = 1.2 Ueq(C,N)] and with N—H = 0.88Å and C—H = 0.95 Å. The highest peak (2.75 e Å-3) in the final difference electron density map is at 1.36Å from Br1.

Figures

Fig. 1.
Perspective view of the title compound with displacement ellipsoids drawn at the 20% probability level; H atoms are omitted for clarity.

Crystal data

[Li3(C4F9O)3(C3H6O)3]F(000) = 1776
Mr = 900.17Dx = 1.675 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9264 reflections
a = 20.6939 (17) Åθ = 3.5–25.0°
b = 11.594 (1) ŵ = 0.21 mm1
c = 15.2211 (13) ÅT = 173 K
β = 102.246 (7)°Block, colourless
V = 3568.8 (5) Å30.17 × 0.12 × 0.08 mm
Z = 4

Data collection

Stoe IPDS-II two-circle diffractometer3143 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.097
graphiteθmax = 25.7°, θmin = 3.5°
ω scansh = −24→25
26210 measured reflectionsk = −14→14
6696 independent reflectionsl = −18→18

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.100Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.313H-atom parameters constrained
S = 1.02w = 1/[σ2(Fo2) + (0.1624P)2 + 1.3913P] where P = (Fo2 + 2Fc2)/3
6696 reflections(Δ/σ)max < 0.001
520 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = −0.43 e Å3

Special details

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)

xyzUiso*/Ueq
Li10.6834 (4)0.5080 (8)0.4511 (6)0.043 (2)
Li20.7494 (4)0.4245 (8)0.6049 (6)0.041 (2)
Li30.8063 (5)0.6077 (8)0.5565 (7)0.049 (2)
O10.71434 (17)0.5853 (3)0.5708 (3)0.0415 (9)
O20.83726 (17)0.4753 (4)0.6246 (3)0.0462 (10)
O30.69334 (17)0.3574 (3)0.5022 (2)0.0397 (9)
C10.6790 (3)0.6422 (6)0.6218 (5)0.0565 (17)
C20.8939 (3)0.4303 (7)0.6738 (5)0.0590 (18)
C30.6702 (3)0.2515 (5)0.4868 (4)0.0413 (13)
C110.7219 (5)0.6635 (11)0.7182 (7)0.103 (4)
C210.6158 (5)0.5731 (9)0.6284 (9)0.102 (4)
C310.6578 (5)0.7626 (9)0.5792 (8)0.093 (3)
C410.9234 (4)0.3436 (9)0.6161 (9)0.096 (3)
C510.8799 (4)0.3704 (9)0.7572 (6)0.087 (3)
C610.9451 (4)0.5287 (10)0.7049 (7)0.090 (3)
C710.6859 (6)0.1984 (8)0.4035 (7)0.100 (3)
C810.6918 (5)0.1737 (7)0.5691 (5)0.080 (3)
C910.5902 (4)0.2547 (8)0.4709 (7)0.081 (2)
O1A0.77526 (18)0.5481 (3)0.4267 (3)0.0426 (9)
C1A0.8023 (3)0.5270 (5)0.3646 (4)0.0457 (14)
C2A0.7665 (4)0.4695 (7)0.2816 (4)0.0616 (18)
H2A10.77990.38840.28230.092*
H2A20.77710.50790.22900.092*
H2A30.71880.47420.27840.092*
C3A0.8728 (4)0.5568 (10)0.3705 (6)0.091 (3)
H3A10.88970.59880.42660.136*
H3A20.87670.60550.31920.136*
H3A30.89850.48600.36960.136*
O1B0.6189 (2)0.5421 (4)0.3439 (3)0.0604 (12)
C1B0.5674 (3)0.5583 (6)0.2902 (4)0.0493 (15)
C2B0.5452 (4)0.4790 (7)0.2126 (5)0.0660 (19)
H2B10.57610.41410.21700.099*
H2B20.54420.52080.15640.099*
H2B30.50090.45000.21340.099*
C3B0.5244 (4)0.6581 (8)0.2999 (5)0.073 (2)
H3B10.49010.63350.33130.110*
H3B20.50370.68750.24020.110*
H3B30.55120.71900.33450.110*
O1C0.8575 (2)0.7423 (4)0.5414 (4)0.0727 (14)
C1C0.8808 (4)0.8329 (7)0.5301 (5)0.0657 (19)
C2C0.8563 (11)0.9436 (12)0.5431 (17)0.227 (11)
H2C10.81370.95500.50140.340*
H2C20.88781.00200.53180.340*
H2C30.85040.95060.60510.340*
C3C0.9489 (5)0.8424 (11)0.5096 (8)0.117 (4)
H3C10.96860.76540.51070.176*
H3C20.97680.89120.55500.176*
H3C30.94540.87680.45000.176*
F110.7411 (4)0.5655 (9)0.7591 (5)0.155 (3)
F120.7768 (3)0.7193 (6)0.7103 (5)0.133 (3)
F130.6917 (5)0.7303 (13)0.7659 (6)0.256 (7)
F210.5782 (2)0.5577 (6)0.5466 (6)0.140 (3)
F220.5812 (5)0.6268 (7)0.6783 (9)0.242 (7)
F230.6347 (5)0.4709 (6)0.6642 (5)0.149 (3)
F310.6204 (6)0.8171 (7)0.6263 (8)0.233 (6)
F320.7082 (4)0.8271 (5)0.5731 (5)0.128 (2)
F330.6231 (4)0.7495 (7)0.4977 (6)0.149 (3)
F410.9860 (3)0.3125 (6)0.6548 (6)0.138 (3)
F420.9217 (4)0.3780 (7)0.5360 (5)0.139 (3)
F430.8883 (3)0.2450 (6)0.6095 (6)0.141 (3)
F510.9265 (3)0.2930 (6)0.7959 (4)0.131 (2)
F520.8751 (3)0.4476 (7)0.8223 (4)0.135 (3)
F530.8223 (3)0.3172 (6)0.7409 (4)0.1077 (19)
F610.9188 (3)0.6205 (6)0.7306 (5)0.117 (2)
F620.9717 (2)0.5628 (6)0.6347 (5)0.118 (2)
F630.9970 (2)0.4962 (6)0.7679 (4)0.131 (3)
F710.7528 (3)0.2176 (5)0.4061 (4)0.116 (2)
F720.6800 (5)0.0836 (5)0.3979 (5)0.152 (3)
F730.6503 (3)0.2477 (5)0.3268 (3)0.1021 (18)
F810.7605 (3)0.1430 (5)0.5695 (4)0.1074 (19)
F820.6600 (3)0.0768 (4)0.5725 (3)0.0832 (14)
F830.6956 (2)0.2306 (4)0.6451 (2)0.0793 (13)
F910.5672 (2)0.3351 (5)0.4146 (4)0.0982 (18)
F920.5740 (3)0.2663 (5)0.5522 (4)0.0981 (16)
F930.5642 (3)0.1539 (5)0.4341 (4)0.121 (2)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Li10.038 (5)0.045 (5)0.045 (5)0.002 (4)0.008 (4)0.005 (4)
Li20.037 (4)0.044 (5)0.041 (5)−0.004 (4)0.009 (4)−0.003 (4)
Li30.039 (5)0.041 (5)0.071 (6)−0.009 (4)0.023 (4)−0.016 (5)
O10.0337 (18)0.036 (2)0.059 (2)0.0016 (16)0.0205 (17)−0.0120 (17)
O20.0281 (18)0.058 (3)0.049 (2)0.0018 (18)−0.0005 (16)−0.0015 (19)
O30.0357 (18)0.031 (2)0.050 (2)−0.0061 (16)0.0046 (16)−0.0028 (16)
C10.048 (3)0.047 (4)0.083 (5)−0.001 (3)0.033 (3)−0.018 (3)
C20.034 (3)0.075 (5)0.063 (4)−0.002 (3)0.001 (3)0.011 (3)
C30.046 (3)0.034 (3)0.041 (3)−0.004 (2)0.003 (2)−0.005 (2)
C110.083 (6)0.133 (9)0.098 (7)0.018 (7)0.032 (5)−0.068 (7)
C210.094 (7)0.086 (7)0.154 (10)−0.017 (5)0.090 (7)−0.061 (7)
C310.076 (6)0.077 (6)0.137 (9)0.030 (5)0.047 (6)−0.022 (6)
C410.065 (5)0.085 (7)0.139 (9)0.029 (5)0.025 (5)0.016 (6)
C510.060 (5)0.104 (7)0.084 (6)−0.012 (5)−0.013 (4)0.030 (5)
C610.039 (4)0.098 (7)0.120 (7)−0.017 (4)−0.015 (4)0.022 (6)
C710.153 (10)0.068 (6)0.093 (7)−0.007 (6)0.059 (7)−0.008 (5)
C810.114 (7)0.057 (5)0.063 (5)−0.021 (5)0.002 (4)0.011 (4)
C910.055 (4)0.072 (5)0.110 (7)−0.019 (4)0.001 (4)−0.004 (5)
O1A0.0373 (19)0.042 (2)0.048 (2)−0.0021 (17)0.0095 (17)0.0005 (18)
C1A0.042 (3)0.046 (3)0.052 (3)0.007 (3)0.015 (3)0.005 (3)
C2A0.067 (4)0.070 (5)0.053 (4)−0.006 (4)0.023 (3)−0.013 (3)
C3A0.052 (4)0.138 (9)0.089 (6)−0.009 (5)0.034 (4)−0.018 (6)
O1B0.041 (2)0.067 (3)0.069 (3)0.007 (2)0.003 (2)0.028 (2)
C1B0.037 (3)0.053 (4)0.061 (4)0.003 (3)0.017 (3)0.027 (3)
C2B0.058 (4)0.068 (5)0.072 (5)0.001 (4)0.014 (3)0.016 (4)
C3B0.059 (4)0.096 (6)0.066 (4)0.030 (4)0.015 (3)0.019 (4)
O1C0.064 (3)0.051 (3)0.102 (4)−0.018 (2)0.015 (3)0.007 (3)
C1C0.089 (5)0.053 (4)0.059 (4)−0.008 (4)0.024 (4)−0.004 (3)
C2C0.27 (2)0.089 (10)0.40 (3)0.021 (12)0.23 (2)0.007 (14)
C3C0.094 (7)0.132 (10)0.125 (9)−0.039 (7)0.025 (6)0.014 (7)
F110.136 (6)0.219 (9)0.121 (5)0.050 (6)0.052 (4)0.078 (6)
F120.098 (4)0.109 (5)0.167 (6)0.001 (4)−0.024 (4)−0.076 (4)
F130.181 (8)0.435 (18)0.142 (6)0.133 (10)0.012 (6)−0.161 (9)
F210.051 (3)0.113 (5)0.246 (9)−0.016 (3)0.006 (4)−0.059 (5)
F220.220 (9)0.161 (7)0.438 (16)−0.106 (7)0.279 (11)−0.176 (9)
F230.260 (9)0.075 (4)0.150 (5)−0.073 (5)0.132 (6)−0.033 (4)
F310.352 (14)0.116 (6)0.310 (12)0.140 (8)0.244 (12)0.044 (7)
F320.170 (6)0.059 (3)0.166 (6)−0.030 (4)0.060 (5)−0.004 (3)
F330.122 (5)0.146 (6)0.162 (6)0.042 (5)−0.009 (5)0.050 (5)
F410.059 (3)0.135 (5)0.215 (7)0.045 (3)0.020 (4)0.038 (5)
F420.140 (6)0.174 (7)0.121 (5)0.076 (5)0.070 (4)0.008 (5)
F430.097 (4)0.081 (4)0.234 (8)0.025 (3)0.009 (5)−0.045 (5)
F510.094 (4)0.149 (6)0.133 (5)0.008 (4)−0.013 (3)0.075 (4)
F520.133 (5)0.202 (8)0.064 (3)−0.030 (5)0.008 (3)−0.013 (4)
F530.081 (3)0.130 (5)0.110 (4)−0.028 (3)0.014 (3)0.037 (3)
F610.078 (3)0.093 (4)0.161 (6)−0.029 (3)−0.017 (3)−0.035 (4)
F620.051 (3)0.131 (5)0.169 (6)−0.013 (3)0.014 (3)0.049 (4)
F630.060 (3)0.156 (6)0.146 (5)−0.031 (3)−0.051 (3)0.038 (4)
F710.132 (5)0.099 (4)0.144 (5)0.005 (4)0.093 (4)−0.020 (4)
F720.304 (10)0.055 (3)0.136 (5)−0.038 (4)0.133 (6)−0.041 (3)
F730.175 (5)0.089 (3)0.042 (2)−0.014 (4)0.021 (3)−0.002 (2)
F810.088 (3)0.087 (4)0.133 (4)0.037 (3)−0.007 (3)0.016 (3)
F820.115 (4)0.045 (2)0.086 (3)−0.022 (2)0.013 (3)0.019 (2)
F830.117 (4)0.073 (3)0.043 (2)0.010 (3)0.005 (2)0.004 (2)
F910.056 (2)0.097 (4)0.123 (4)−0.017 (2)−0.023 (3)0.048 (3)
F920.089 (3)0.119 (4)0.103 (4)−0.031 (3)0.058 (3)−0.017 (3)
F930.117 (4)0.086 (4)0.133 (5)−0.065 (3)−0.032 (4)0.009 (3)

Geometric parameters (Å, °)

Li1—O31.905 (10)C51—F521.354 (12)
Li1—O1B1.918 (9)C51—F511.356 (10)
Li1—O12.009 (10)C61—F611.293 (12)
Li1—O1A2.066 (10)C61—F631.333 (9)
Li1—Li22.631 (12)C61—F621.361 (12)
Li1—Li32.940 (13)C71—F721.337 (11)
Li2—Li32.608 (14)C71—F731.367 (12)
Li2—O21.874 (9)C71—F711.395 (13)
Li2—O31.904 (9)C81—F821.309 (9)
Li2—O12.027 (10)C81—F831.319 (9)
Li2—F532.606 (10)C81—F811.464 (11)
Li2—F832.639 (10)C91—F911.287 (10)
Li3—O21.885 (12)C91—F921.355 (11)
Li3—O1C1.928 (11)C91—F931.356 (9)
Li3—O11.977 (10)O1A—C1A1.221 (7)
Li3—O1A2.063 (11)C1A—C2A1.482 (9)
O1—C11.347 (7)C1A—C3A1.483 (9)
O2—C21.355 (7)C2A—H2A10.9800
O3—C31.321 (7)C2A—H2A20.9800
C1—C211.555 (11)C2A—H2A30.9800
C1—C311.563 (13)C3A—H3A10.9800
C1—C111.565 (13)C3A—H3A20.9800
C2—C511.528 (12)C3A—H3A30.9800
C2—C411.542 (13)O1B—C1B1.212 (7)
C2—C611.560 (11)C1B—C3B1.485 (10)
C3—C711.505 (11)C1B—C2B1.490 (10)
C3—C811.531 (9)C2B—H2B10.9800
C3—C911.622 (10)C2B—H2B20.9800
C11—F131.308 (10)C2B—H2B30.9800
C11—F111.315 (14)C3B—H3B10.9800
C11—F121.334 (13)C3B—H3B20.9800
C21—F221.307 (9)C3B—H3B30.9800
C21—F231.329 (14)O1C—C1C1.184 (8)
C21—F211.332 (13)C1C—C2C1.409 (16)
C31—F321.302 (11)C1C—C3C1.509 (13)
C31—F331.303 (12)C2C—H2C10.9800
C31—F311.322 (10)C2C—H2C20.9800
C41—F421.276 (13)C2C—H2C30.9800
C41—F431.346 (12)C3C—H3C10.9800
C41—F411.354 (10)C3C—H3C20.9800
C51—F531.318 (9)C3C—H3C30.9800
O3—Li1—O1B122.1 (5)F32—C31—F31109.5 (10)
O3—Li1—O193.0 (4)F33—C31—F31107.7 (10)
O1B—Li1—O1135.2 (6)F32—C31—C1112.6 (7)
O3—Li1—O1A104.8 (4)F33—C31—C1109.9 (8)
O1B—Li1—O1A107.6 (5)F31—C31—C1110.3 (9)
O1—Li1—O1A86.2 (4)F42—C41—F43106.8 (11)
O3—Li1—Li246.3 (3)F42—C41—F41109.2 (9)
O1B—Li1—Li2165.7 (5)F43—C41—F41104.8 (8)
O1—Li1—Li249.6 (3)F42—C41—C2114.0 (8)
O1A—Li1—Li285.3 (4)F43—C41—C2108.9 (8)
O3—Li1—Li397.6 (4)F41—C41—C2112.5 (9)
O1B—Li1—Li3138.5 (5)F53—C51—F52104.1 (9)
O1—Li1—Li342.1 (3)F53—C51—F51107.6 (8)
O1A—Li1—Li344.6 (3)F52—C51—F51106.0 (7)
Li2—Li1—Li355.5 (3)F53—C51—C2112.3 (6)
O2—Li2—O3131.4 (5)F52—C51—C2111.4 (8)
O2—Li2—O192.0 (4)F51—C51—C2114.8 (8)
O3—Li2—O192.5 (4)F61—C61—F63110.0 (9)
O2—Li2—F5369.2 (3)F61—C61—F62105.4 (8)
O3—Li2—F53127.3 (5)F63—C61—F62104.3 (7)
O1—Li2—F53139.3 (5)F61—C61—C2113.1 (7)
O2—Li2—Li346.3 (3)F63—C61—C2113.8 (8)
O3—Li2—Li3109.5 (5)F62—C61—C2109.6 (8)
O1—Li2—Li348.5 (3)F72—C71—F73109.7 (9)
F53—Li2—Li3113.2 (4)F72—C71—F71103.7 (9)
O2—Li2—Li1109.3 (5)F73—C71—F71108.0 (8)
O3—Li2—Li146.3 (3)F72—C71—C3115.4 (8)
O1—Li2—Li149.0 (3)F73—C71—C3112.0 (8)
F53—Li2—Li1170.6 (5)F71—C71—C3107.5 (8)
Li3—Li2—Li168.3 (4)F82—C81—F83109.3 (7)
O2—Li2—F83132.4 (5)F82—C81—F81106.7 (7)
O3—Li2—F8368.2 (3)F83—C81—F81103.9 (6)
O1—Li2—F83134.2 (4)F82—C81—C3118.4 (6)
F53—Li2—F8367.1 (3)F83—C81—C3112.1 (6)
Li3—Li2—F83175.8 (5)F81—C81—C3105.2 (6)
Li1—Li2—F83110.8 (4)F91—C91—F92114.0 (8)
O2—Li3—O1C126.4 (5)F91—C91—F93107.0 (7)
O2—Li3—O193.2 (5)F92—C91—F93108.0 (7)
O1C—Li3—O1133.3 (6)F91—C91—C3109.7 (7)
O2—Li3—O1A104.7 (5)F92—C91—C3107.9 (6)
O1C—Li3—O1A103.0 (5)F93—C91—C3110.2 (7)
O1—Li3—O1A87.1 (4)C1A—O1A—Li3135.1 (4)
O2—Li3—Li245.9 (3)C1A—O1A—Li1133.2 (5)
O1C—Li3—Li2170.2 (6)Li3—O1A—Li190.8 (4)
O1—Li3—Li250.2 (3)O1A—C1A—C2A121.5 (5)
O1A—Li3—Li286.0 (4)O1A—C1A—C3A120.9 (6)
O2—Li3—Li197.7 (4)C2A—C1A—C3A117.6 (6)
O1C—Li3—Li1133.4 (6)C1A—C2A—H2A1109.5
O1—Li3—Li142.9 (3)C1A—C2A—H2A2109.5
O1A—Li3—Li144.6 (3)H2A1—C2A—H2A2109.5
Li2—Li3—Li156.2 (3)C1A—C2A—H2A3109.5
C1—O1—Li3130.7 (5)H2A1—C2A—H2A3109.5
C1—O1—Li1129.3 (4)H2A2—C2A—H2A3109.5
Li3—O1—Li195.0 (4)C1A—C3A—H3A1109.5
C1—O1—Li2120.8 (5)C1A—C3A—H3A2109.5
Li3—O1—Li281.3 (4)H3A1—C3A—H3A2109.5
Li1—O1—Li281.4 (4)C1A—C3A—H3A3109.5
C2—O2—Li2131.6 (5)H3A1—C3A—H3A3109.5
C2—O2—Li3140.4 (5)H3A2—C3A—H3A3109.5
Li2—O2—Li387.9 (4)C1B—O1B—Li1163.7 (5)
C3—O3—Li2131.4 (4)O1B—C1B—C3B120.9 (7)
C3—O3—Li1140.9 (4)O1B—C1B—C2B121.2 (6)
Li2—O3—Li187.4 (4)C3B—C1B—C2B118.0 (6)
O1—C1—C21110.6 (5)C1B—C2B—H2B1109.5
O1—C1—C31109.7 (6)C1B—C2B—H2B2109.5
C21—C1—C31108.7 (7)H2B1—C2B—H2B2109.5
O1—C1—C11110.3 (6)C1B—C2B—H2B3109.5
C21—C1—C11109.8 (8)H2B1—C2B—H2B3109.5
C31—C1—C11107.6 (8)H2B2—C2B—H2B3109.5
O2—C2—C51109.9 (6)C1B—C3B—H3B1109.5
O2—C2—C41109.7 (6)C1B—C3B—H3B2109.5
C51—C2—C41110.1 (8)H3B1—C3B—H3B2109.5
O2—C2—C61109.8 (6)C1B—C3B—H3B3109.5
C51—C2—C61108.4 (7)H3B1—C3B—H3B3109.5
C41—C2—C61109.0 (7)H3B2—C3B—H3B3109.5
O3—C3—C71113.3 (6)C1C—O1C—Li3170.9 (7)
O3—C3—C81111.7 (5)O1C—C1C—C2C128.1 (10)
C71—C3—C81111.7 (7)O1C—C1C—C3C121.5 (8)
O3—C3—C91109.0 (5)C2C—C1C—C3C110.0 (10)
C71—C3—C91106.3 (7)C1C—C2C—H2C1109.5
C81—C3—C91104.3 (6)C1C—C2C—H2C2109.5
F13—C11—F11112.3 (12)H2C1—C2C—H2C2109.5
F13—C11—F12106.2 (11)C1C—C2C—H2C3109.5
F11—C11—F12106.6 (9)H2C1—C2C—H2C3109.5
F13—C11—C1111.7 (8)H2C2—C2C—H2C3109.5
F11—C11—C1111.2 (9)C1C—C3C—H3C1109.5
F12—C11—C1108.4 (9)C1C—C3C—H3C2109.5
F22—C21—F23109.7 (11)H3C1—C3C—H3C2109.5
F22—C21—F21108.9 (11)C1C—C3C—H3C3109.5
F23—C21—F21109.1 (8)H3C1—C3C—H3C3109.5
F22—C21—C1111.3 (7)H3C2—C3C—H3C3109.5
F23—C21—C1107.8 (9)C51—F53—Li2105.9 (5)
F21—C21—C1110.0 (9)C81—F83—Li299.9 (5)
F32—C31—F33106.7 (10)
O3—Li1—Li2—O2129.5 (6)Li3—O1—C1—C3174.5 (9)
O1B—Li1—Li2—O2169 (2)Li1—O1—C1—C31−74.1 (8)
O1—Li1—Li2—O2−75.2 (5)Li2—O1—C1—C31−179.3 (6)
O1A—Li1—Li2—O213.8 (5)Li3—O1—C1—C11−43.9 (10)
Li3—Li1—Li2—O2−22.0 (4)Li1—O1—C1—C11167.5 (7)
O1B—Li1—Li2—O339 (2)Li2—O1—C1—C1162.3 (8)
O1—Li1—Li2—O3155.3 (5)Li2—O2—C2—C51−33.8 (10)
O1A—Li1—Li2—O3−115.7 (5)Li3—O2—C2—C51140.4 (8)
Li3—Li1—Li2—O3−151.4 (5)Li2—O2—C2—C4187.4 (8)
O3—Li1—Li2—O1−155.3 (5)Li3—O2—C2—C41−98.4 (9)
O1B—Li1—Li2—O1−116 (2)Li2—O2—C2—C61−152.9 (7)
O1A—Li1—Li2—O189.0 (4)Li3—O2—C2—C6121.3 (11)
Li3—Li1—Li2—O153.3 (3)Li2—O3—C3—C71−124.9 (7)
O3—Li1—Li2—Li3151.4 (5)Li1—O3—C3—C7164.3 (10)
O1—Li1—Li2—Li3−53.3 (3)Li2—O3—C3—C812.4 (9)
O1A—Li1—Li2—Li335.8 (3)Li1—O3—C3—C81−168.5 (7)
O3—Li1—Li2—F83−24.2 (4)Li2—O3—C3—C91117.1 (7)
O1—Li1—Li2—F83131.1 (5)Li1—O3—C3—C91−53.8 (9)
O1A—Li1—Li2—F83−139.9 (4)O1—C1—C11—F13172.4 (11)
Li3—Li1—Li2—F83−175.6 (5)C21—C1—C11—F13−65.4 (14)
O3—Li2—Li3—O2−129.2 (6)C31—C1—C11—F1352.8 (14)
O1—Li2—Li3—O2155.4 (6)O1—C1—C11—F11−61.2 (10)
F53—Li2—Li3—O219.2 (4)C21—C1—C11—F1161.0 (9)
Li1—Li2—Li3—O2−150.8 (5)C31—C1—C11—F11179.2 (8)
O2—Li2—Li3—O1−155.4 (6)O1—C1—C11—F1255.7 (10)
O3—Li2—Li3—O175.4 (5)C21—C1—C11—F12177.9 (7)
F53—Li2—Li3—O1−136.2 (5)C31—C1—C11—F12−63.9 (9)
Li1—Li2—Li3—O153.9 (3)O1—C1—C21—F22179.5 (11)
O2—Li2—Li3—O1A115.0 (5)C31—C1—C21—F22−60.0 (14)
O3—Li2—Li3—O1A−14.2 (5)C11—C1—C21—F2257.5 (14)
O1—Li2—Li3—O1A−89.6 (4)O1—C1—C21—F2359.1 (10)
F53—Li2—Li3—O1A134.2 (4)C31—C1—C21—F23179.6 (7)
Li1—Li2—Li3—O1A−35.8 (3)C11—C1—C21—F23−62.9 (9)
O2—Li2—Li3—Li1150.8 (5)O1—C1—C21—F21−59.7 (10)
O3—Li2—Li3—Li121.5 (4)C31—C1—C21—F2160.8 (9)
O1—Li2—Li3—Li1−53.9 (3)C11—C1—C21—F21178.3 (7)
F53—Li2—Li3—Li1169.9 (5)O1—C1—C31—F32−60.3 (10)
O3—Li1—Li3—O20.3 (5)C21—C1—C31—F32178.6 (8)
O1B—Li1—Li3—O2−163.3 (7)C11—C1—C31—F3259.7 (10)
O1—Li1—Li3—O286.4 (5)O1—C1—C31—F3358.4 (9)
O1A—Li1—Li3—O2−103.2 (5)C21—C1—C31—F33−62.6 (9)
Li2—Li1—Li3—O220.7 (4)C11—C1—C31—F33178.5 (8)
O3—Li1—Li3—O1C162.3 (6)O1—C1—C31—F31177.0 (9)
O1B—Li1—Li3—O1C−1.3 (12)C21—C1—C31—F3156.0 (12)
O1—Li1—Li3—O1C−111.6 (8)C11—C1—C31—F31−62.9 (11)
O1A—Li1—Li3—O1C58.8 (7)O2—C2—C41—F4243.0 (11)
Li2—Li1—Li3—O1C−177.3 (8)C51—C2—C41—F42164.0 (8)
O3—Li1—Li3—O1−86.1 (5)C61—C2—C41—F42−77.2 (10)
O1B—Li1—Li3—O1110.3 (9)O2—C2—C41—F43−76.2 (9)
O1A—Li1—Li3—O1170.4 (6)C51—C2—C41—F4344.8 (9)
Li2—Li1—Li3—O1−65.7 (4)C61—C2—C41—F43163.6 (8)
O3—Li1—Li3—O1A103.5 (5)O2—C2—C41—F41168.0 (8)
O1B—Li1—Li3—O1A−60.1 (7)C51—C2—C41—F41−71.0 (10)
O1—Li1—Li3—O1A−170.4 (6)C61—C2—C41—F4147.8 (11)
Li2—Li1—Li3—O1A123.9 (5)O2—C2—C51—F5337.0 (11)
O3—Li1—Li3—Li2−20.4 (4)C41—C2—C51—F53−83.9 (10)
O1B—Li1—Li3—Li2176.0 (9)C61—C2—C51—F53157.0 (8)
O1—Li1—Li3—Li265.7 (4)O2—C2—C51—F52−79.3 (8)
O1A—Li1—Li3—Li2−123.9 (5)C41—C2—C51—F52159.8 (7)
O2—Li3—O1—C1106.0 (6)C61—C2—C51—F5240.7 (9)
O1C—Li3—O1—C1−44.3 (11)O2—C2—C51—F51160.3 (7)
O1A—Li3—O1—C1−149.4 (6)C41—C2—C51—F5139.4 (10)
Li2—Li3—O1—C1123.4 (7)C61—C2—C51—F51−79.7 (10)
Li1—Li3—O1—C1−156.1 (7)O2—C2—C61—F6141.1 (11)
O2—Li3—O1—Li1−97.9 (4)C51—C2—C61—F61−78.9 (10)
O1C—Li3—O1—Li1111.9 (8)C41—C2—C61—F61161.2 (8)
O1A—Li3—O1—Li16.7 (4)O2—C2—C61—F63167.5 (8)
Li2—Li3—O1—Li1−80.4 (4)C51—C2—C61—F6347.5 (12)
O2—Li3—O1—Li2−17.4 (4)C41—C2—C61—F63−72.4 (11)
O1C—Li3—O1—Li2−167.7 (8)O2—C2—C61—F62−76.2 (9)
O1A—Li3—O1—Li287.2 (4)C51—C2—C61—F62163.8 (7)
Li1—Li3—O1—Li280.4 (4)C41—C2—C61—F6244.0 (9)
O3—Li1—O1—C1−105.4 (6)O3—C3—C71—F72162.5 (9)
O1B—Li1—O1—C138.6 (11)C81—C3—C71—F7235.3 (13)
O1A—Li1—O1—C1149.9 (5)C91—C3—C71—F72−77.9 (11)
Li2—Li1—O1—C1−123.0 (6)O3—C3—C71—F73−71.1 (10)
Li3—Li1—O1—C1156.6 (7)C81—C3—C71—F73161.6 (7)
O3—Li1—O1—Li398.0 (5)C91—C3—C71—F7348.5 (9)
O1B—Li1—O1—Li3−118.0 (8)O3—C3—C71—F7147.4 (9)
O1A—Li1—O1—Li3−6.7 (4)C81—C3—C71—F71−79.8 (8)
Li2—Li1—O1—Li380.3 (4)C91—C3—C71—F71167.0 (7)
O3—Li1—O1—Li217.6 (4)O3—C3—C81—F82163.0 (7)
O1B—Li1—O1—Li2161.6 (8)C71—C3—C81—F82−68.9 (11)
O1A—Li1—O1—Li2−87.1 (4)C91—C3—C81—F8245.4 (10)
Li3—Li1—O1—Li2−80.3 (4)O3—C3—C81—F8334.3 (9)
O2—Li2—O1—C1−115.0 (5)C71—C3—C81—F83162.3 (8)
O3—Li2—O1—C1113.3 (5)C91—C3—C81—F83−83.3 (8)
F53—Li2—O1—C1−55.4 (8)O3—C3—C81—F81−78.0 (7)
Li3—Li2—O1—C1−132.5 (5)C71—C3—C81—F8150.1 (8)
Li1—Li2—O1—C1130.9 (5)C91—C3—C81—F81164.4 (6)
F83—Li2—O1—C151.8 (8)O3—C3—C91—F9147.9 (8)
O2—Li2—O1—Li317.5 (4)C71—C3—C91—F91−74.4 (8)
O3—Li2—O1—Li3−114.1 (5)C81—C3—C91—F91167.4 (7)
F53—Li2—O1—Li377.2 (7)O3—C3—C91—F92−76.8 (7)
Li1—Li2—O1—Li3−96.5 (4)C71—C3—C91—F92160.8 (7)
F83—Li2—O1—Li3−175.6 (6)C81—C3—C91—F9242.6 (8)
O2—Li2—O1—Li1114.0 (4)O3—C3—C91—F93165.4 (6)
O3—Li2—O1—Li1−17.6 (4)C71—C3—C91—F9343.0 (9)
F53—Li2—O1—Li1173.7 (7)C81—C3—C91—F93−75.1 (8)
Li3—Li2—O1—Li196.5 (4)O2—Li3—O1A—C1A−83.6 (7)
F83—Li2—O1—Li1−79.1 (6)O1C—Li3—O1A—C1A50.0 (8)
O3—Li2—O2—C2−106.8 (8)O1—Li3—O1A—C1A−176.2 (6)
O1—Li2—O2—C2158.1 (6)Li2—Li3—O1A—C1A−125.9 (6)
F53—Li2—O2—C215.2 (7)Li1—Li3—O1A—C1A−169.7 (7)
Li3—Li2—O2—C2176.3 (7)O2—Li3—O1A—Li186.0 (5)
Li1—Li2—O2—C2−154.9 (6)O1C—Li3—O1A—Li1−140.4 (5)
F83—Li2—O2—C2−9.1 (10)O1—Li3—O1A—Li1−6.5 (4)
O3—Li2—O2—Li376.9 (7)Li2—Li3—O1A—Li143.8 (4)
O1—Li2—O2—Li3−18.2 (4)O3—Li1—O1A—C1A84.3 (7)
F53—Li2—O2—Li3−161.1 (4)O1B—Li1—O1A—C1A−47.1 (8)
Li1—Li2—O2—Li328.7 (5)O1—Li1—O1A—C1A176.4 (5)
F83—Li2—O2—Li3174.6 (6)Li2—Li1—O1A—C1A126.7 (6)
O1C—Li3—O2—C2−3.6 (12)Li3—Li1—O1A—C1A170.0 (7)
O1—Li3—O2—C2−157.0 (7)O3—Li1—O1A—Li3−85.7 (5)
O1A—Li3—O2—C2115.1 (8)O1B—Li1—O1A—Li3142.9 (5)
Li2—Li3—O2—C2−175.7 (9)O1—Li1—O1A—Li36.4 (4)
Li1—Li3—O2—C2160.1 (7)Li2—Li1—O1A—Li3−43.3 (4)
O1C—Li3—O2—Li2172.0 (7)Li3—O1A—C1A—C2A171.8 (6)
O1—Li3—O2—Li218.7 (4)Li1—O1A—C1A—C2A6.1 (10)
O1A—Li3—O2—Li2−69.2 (5)Li3—O1A—C1A—C3A−7.4 (11)
Li1—Li3—O2—Li2−24.2 (4)Li1—O1A—C1A—C3A−173.1 (7)
O2—Li2—O3—C3109.3 (8)O3—Li1—O1B—C1B68 (2)
O1—Li2—O3—C3−155.8 (5)O1—Li1—O1B—C1B−68 (2)
F53—Li2—O3—C314.9 (9)O1A—Li1—O1B—C1B−171.0 (18)
Li3—Li2—O3—C3157.6 (5)Li2—Li1—O1B—C1B35 (4)
Li1—Li2—O3—C3−174.2 (7)Li3—Li1—O1B—C1B−131.3 (18)
F83—Li2—O3—C3−18.6 (6)Li1—O1B—C1B—C3B67 (2)
O2—Li2—O3—Li1−76.4 (7)Li1—O1B—C1B—C2B−113 (2)
O1—Li2—O3—Li118.4 (4)F52—C51—F53—Li294.9 (6)
F53—Li2—O3—Li1−170.8 (6)F51—C51—F53—Li2−153.0 (7)
Li3—Li2—O3—Li1−28.1 (5)C2—C51—F53—Li2−25.7 (10)
F83—Li2—O3—Li1155.6 (4)O2—Li2—F53—C519.0 (7)
O1B—Li1—O3—C33.8 (11)O3—Li2—F53—C51135.9 (8)
O1—Li1—O3—C3154.6 (6)O1—Li2—F53—C51−58.3 (10)
O1A—Li1—O3—C3−118.5 (7)Li3—Li2—F53—C51−5.7 (8)
Li2—Li1—O3—C3173.1 (8)F83—Li2—F53—C51169.7 (7)
Li3—Li1—O3—C3−163.4 (6)F82—C81—F83—Li2−174.1 (6)
O1B—Li1—O3—Li2−169.3 (6)F81—C81—F83—Li272.3 (5)
O1—Li1—O3—Li2−18.6 (4)C3—C81—F83—Li2−40.7 (7)
O1A—Li1—O3—Li268.3 (5)O2—Li2—F83—C81−94.5 (8)
Li3—Li1—O3—Li223.4 (4)O3—Li2—F83—C8132.4 (5)
Li3—O1—C1—C21−165.6 (8)O1—Li2—F83—C81103.4 (7)
Li1—O1—C1—C2145.8 (10)F53—Li2—F83—C81−119.1 (5)
Li2—O1—C1—C21−59.4 (9)Li1—Li2—F83—C8151.0 (6)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB5716).

References

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